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#\#CIF_1.0 ################################################################################ # # # This CIF is a part of the B-IncStrDB # # (Bilbao Incommensurate Structures Database) # # http://www.cryst.ehu.eus/bincstrdb/ # # # # Please note that the structure of the CIF file may differ from the one # # deposited, as it may have been modified to comply with the standard. The # # file has been validated against official dictionaries as well as local # # dictionaries including non-standard data names used by SHELXL (Sheldrick, # # G. M. (2008). Acta Cryst. A 64, 112-122) and JANA (Petricek, V., Dusek, M. # # and Palatinus, L. (2014), Z. Kristallogr. 229, 345-352). # # # # For comments and/or criticisms, please e-mail to administrador-bcs@ehu.es # # # ################################################################################ data_global _audit_creation_method 'Jana2006 Version : 09/12/2016' _journal_date_recd_electronic 2018-07-20 _journal_date_accepted 2018-10-23 _journal_coeditor_code LT5013SUP1 _journal_techeditor_code M181502 _iucr_compatibility_tag ACTA95 _journal_paper_category FA _publ_contact_author_name 'Dr. L. Canadillas-Delgado' _publ_contact_author_address ;Institut Laue-Langevin, 71 Avenue des Martyrs, CS 20156, 38042 Grenoble Cedex 9, France ; _publ_contact_author_email lcd@ill.fr _journal_name_full 'IUCrJ' _journal_volume 6 _journal_year 2019 _journal_page_first 105 _journal_page_last 115 _journal_paper_doi https://doi.org/10.1107/S2052252518015026 _publ_section_title 'Incommensurate structures of the [CH~3~NH~3~][Co(COOH)~3~] compound' loop_ _publ_author_name _publ_author_address _publ_author_footnote _publ_author_email 'Canadillas-Delgado, Laura' ;Diffraction Group, Institut Laue Langevin, 71, avenue des Martyrs, Grenoble 38042, France and Centro Universitario de la Defensa de Zaragoza, Crtra. Huesca s/n, Zaragoza 50090, Spain ; ? lcd@ill.fr 'Mazzuca, Lidia' ;Diffraction Group, Institut Laue Langevin, 71, avenue des Martyrs, Grenoble 38042, France ; ? ? 'Fabelo, Oscar' ;Diffraction Group, Institut Laue Langevin, 71, avenue des Martyrs, Grenoble 38042, France ; ? Edward.Tiekink@gmail.com 'Rodriguez-Velamazan, J. Alberto' ;Diffraction Group, Institut Laue Langevin, 71, avenue des Martyrs, Grenoble 38042, France ; ? ? 'Rodriguez-Carvajal, Juan' ;Diffraction Group, Institut Laue Langevin, 71, avenue des Martyrs, Grenoble 38042, France ; ? ? _publ_section_references ; Petricek, V., Dusek, M. & Palatinus L. (2014). Z. Kristallogr. 229(5), 345-352. Palatinus L. & Chapuis G. (2007). J. Appl. Cryst. 40, 786-790. Brandenburg, K. (2017). DIAMOND Version 4. Crystal Impact GbR, Bonn, Germany. ; data_I _chemical_formula_sum 'C4 H9 Co1 N1 O6' _chemical_formula_weight 226 _chemical_absolute_configuration ? _space_group_crystal_system orthorhombic _space_group_ssg_name Pnma(00\g)0s0 loop_ _space_group_symop_ssg_id _space_group_symop_ssg_operation_algebraic 1 x1,x2,x3,x4 2 -x1+1/2,-x2,x3+1/2,x4+1/2 3 -x1,x2+1/2,-x3,-x4+1/2 4 x1+1/2,-x2+1/2,-x3+1/2,-x4 5 -x1,-x2,-x3,-x4 6 x1+1/2,x2,-x3+1/2,-x4+1/2 7 x1,-x2+1/2,x3,x4+1/2 8 -x1+1/2,x2+1/2,x3+1/2,x4 _cell_length_a 8.2674(2) _cell_length_b 11.6600(4) _cell_length_c 8.1483(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 785.48(4) _cell_modulation_dimension 1 loop_ _cell_wave_vector_seq_id _cell_wave_vector_x _cell_wave_vector_y _cell_wave_vector_z 1 0.000000 0.000000 0.143000 _cell_formula_units_Z 4 _cell_measurement_reflns_used 725 _cell_measurement_theta_min 5.12 _cell_measurement_theta_max 61.15 _cell_measurement_temperature 122 _exptl_crystal_type_of_structure mod _exptl_crystal_density_diffrn 1.9115 _exptl_crystal_F_000 158.404 _exptl_absorpt_coefficient_mu 0.2417 _exptl_crystal_description prism _exptl_crystal_size_max 5 _exptl_crystal_size_mid 4 _exptl_crystal_size_min 4 _exptl_crystal_size_rad 4 _exptl_crystal_colour red _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'absorption corretion done through d19face, d19abs and d19abscan programs from ILL' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist ? ? ? ? _diffrn_ambient_temperature 122 _diffrn_source_power 55000 _diffrn_radiation_type neutron _diffrn_source 'neutron source' _diffrn_source_type 'ILL High Flux Reactor, beam H11' _diffrn_radiation_monochromator 'copper 331' _diffrn_measurement_device_type 'D19 position-sensitive detector diffractometer' _diffrn_measurement_method 'omega step-scans' _diffrn_detector_area_resol_mean 210 _diffrn_radiation_wavelength 1.4569 _diffrn_reflns_number 22671 _diffrn_reflns_theta_min 5.12 _diffrn_reflns_theta_max 61.15 _diffrn_reflns_theta_full 61.15 _diffrn_measured_fraction_theta_max 0.98 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_av_R_equivalents 0.1145 _diffrn_reflns_av_unetI/netI 0.0117 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_index_m_1_min -2 _diffrn_reflns_limit_index_m_1_max 2 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_radiation_probe neutron _reflns_number_total 3543 _reflns_number_gt 1880 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0880 _refine_ls_wR_factor_gt 0.1048 _refine_ls_R_factor_all 0.1189 _refine_ls_wR_factor_ref 0.1067 _refine_ls_goodness_of_fit_ref 4.66 _refine_ls_goodness_of_fit_gt 6.60 _refine_ls_number_reflns 3543 _refine_ls_number_parameters 333 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/(\s^2^(F)+0.0001F^2^) _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max 0.0041 _refine_ls_shift/su_mean 0.0006 _refine_ls_extinction_method none loop_ _atom_type_symbol _atom_type_scat_length_neutron _atom_type_scat_source C 6.646 International_Tables_Vol_C H -3.739 International_Tables_Vol_C Co 2.490 International_Tables_Vol_C N 9.360 International_Tables_Vol_C O 5.803 International_Tables_Vol_C loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.5 0 0 Uani 0.0232(10) 4 1 d ? ? ? O1 O 0.59584(13) -0.07056(10) -0.21411(13) Uani 0.0276(4) 8 1 d ? ? ? O2 O 0.77272(13) -0.05976(10) -0.41827(13) Uani 0.0277(4) 8 1 d ? ? ? O3 O 0.47437(14) 0.15518(10) -0.12770(12) Uani 0.0273(4) 8 1 d ? ? ? N1 N 0.91481(12) 0.25 -0.03036(14) Uani 0.0307(4) 4 1 d ? ? ? C1 C 0.71991(12) -0.02969(9) -0.27949(12) Uani 0.0266(3) 8 1 d ? ? ? C3 C 1.08563(18) 0.25 0.0242(2) Uani 0.0354(6) 4 1 d ? ? ? C2 C 0.49044(17) 0.25 -0.05698(16) Uani 0.0268(4) 4 1 d ? ? ? H1 H 0.7886(3) 0.0336(3) -0.2118(3) Uani 0.0569(9) 8 1 d ? ? ? H2 H 0.5200(5) 0.25 0.0756(4) Uani 0.0483(11) 4 1 d ? ? ? H1n H 0.9118(4) 0.25 -0.1549(4) Uani 0.0562(14) 4 1 d ? ? ? H3a H 1.0897(5) 0.25 0.1551(5) Uani 0.0722(17) 4 1 d ? ? ? H2n H 0.8544(3) 0.1784(2) 0.0129(3) Uani 0.0428(7) 8 1 d ? ? ? H3b H 1.1454(4) 0.3250(3) -0.0197(4) Uani 0.0710(11) 8 1 d ? ? ? loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co1 Co 0.0245(17) 0.026(2) 0.0187(15) 0.0004(12) 0.0007(12) -0.0006(12) O1 O 0.0272(7) 0.0277(7) 0.0280(6) -0.0043(4) 0.0027(4) -0.0020(4) O2 O 0.0265(6) 0.0305(7) 0.0262(6) -0.0037(4) 0.0022(4) -0.0007(4) O3 O 0.0329(7) 0.0222(7) 0.0268(6) -0.0009(4) -0.0018(4) -0.0010(4) N1 N 0.0315(7) 0.0294(7) 0.0311(7) 0 0.0028(4) 0 C1 C 0.0260(6) 0.0264(6) 0.0273(6) -0.0030(4) 0.0029(4) -0.0002(4) C3 C 0.0291(9) 0.0373(11) 0.0397(10) 0 0.0008(6) 0 C2 C 0.0297(7) 0.0252(8) 0.0256(8) 0 -0.0028(5) 0 H1 H 0.0542(16) 0.0659(17) 0.0506(15) -0.0279(13) 0.0142(12) -0.0258(12) H2 H 0.070(2) 0.0386(18) 0.0364(17) 0 -0.0106(14) 0 H1n H 0.0433(19) 0.086(3) 0.039(2) 0 0.0018(13) 0 H3a H 0.051(2) 0.115(4) 0.050(3) 0 -0.0058(16) 0 H2n H 0.0463(13) 0.0360(13) 0.0461(11) -0.0088(10) 0.0050(9) 0.0029(10) H3b H 0.0522(16) 0.0687(19) 0.092(2) -0.0187(15) -0.0042(14) 0.0233(17) loop_ _atom_site_Fourier_wave_vector_seq_id _jana_atom_site_Fourier_wave_vector_q1_coeff 1 1 2 2 loop_ _atom_site_displace_Fourier_id _atom_site_displace_Fourier_atom_site_label _atom_site_displace_Fourier_axis _atom_site_displace_Fourier_wave_vector_seq_id Co1x1 Co1 x 1 Co1y1 Co1 y 1 Co1z1 Co1 z 1 O1x1 O1 x 1 O1y1 O1 y 1 O1z1 O1 z 1 O1x2 O1 x 2 O1y2 O1 y 2 O1z2 O1 z 2 O2x1 O2 x 1 O2y1 O2 y 1 O2z1 O2 z 1 O3x1 O3 x 1 O3y1 O3 y 1 O3z1 O3 z 1 O3x2 O3 x 2 O3y2 O3 y 2 O3z2 O3 z 2 N1x1 N1 x 1 N1y1 N1 y 1 N1z1 N1 z 1 N1x2 N1 x 2 N1y2 N1 y 2 N1z2 N1 z 2 C1x1 C1 x 1 C1y1 C1 y 1 C1z1 C1 z 1 C1x2 C1 x 2 C1y2 C1 y 2 C1z2 C1 z 2 C3x1 C3 x 1 C3y1 C3 y 1 C3z1 C3 z 1 C3x2 C3 x 2 C3y2 C3 y 2 C3z2 C3 z 2 C2x1 C2 x 1 C2y1 C2 y 1 C2z1 C2 z 1 H1x1 H1 x 1 H1y1 H1 y 1 H1z1 H1 z 1 H1x2 H1 x 2 H1y2 H1 y 2 H1z2 H1 z 2 H2x1 H2 x 1 H2y1 H2 y 1 H2z1 H2 z 1 H2x2 H2 x 2 H2y2 H2 y 2 H2z2 H2 z 2 H1nx1 H1n x 1 H1ny1 H1n y 1 H1nz1 H1n z 1 H1nx2 H1n x 2 H1ny2 H1n y 2 H1nz2 H1n z 2 H3ax1 H3a x 1 H3ay1 H3a y 1 H3az1 H3a z 1 H3ax2 H3a x 2 H3ay2 H3a y 2 H3az2 H3a z 2 H2nx1 H2n x 1 H2ny1 H2n y 1 H2nz1 H2n z 1 H2nx2 H2n x 2 H2ny2 H2n y 2 H2nz2 H2n z 2 H3bx1 H3b x 1 H3by1 H3b y 1 H3bz1 H3b z 1 H3bx2 H3b x 2 H3by2 H3b y 2 H3bz2 H3b z 2 loop_ _atom_site_displace_Fourier_param_id _atom_site_displace_Fourier_param_cos _atom_site_displace_Fourier_param_sin Co1x1 0 -0.0011(5) Co1y1 0 0.0134(4) Co1z1 0 -0.0004(5) O1x1 -0.00139(18) -0.00133(17) O1y1 0.00210(12) 0.01322(12) O1z1 0.00026(16) 0.00035(17) O1x2 -0.0004(4) 0.0009(5) O1y2 0.0002(2) 0.0000(2) O1z2 0.0005(4) -0.0004(4) O2x1 0.00049(18) -0.00138(17) O2y1 0.00081(12) 0.01335(12) O2z1 0.00183(16) -0.00024(17) O3x1 -0.00188(18) -0.00075(16) O3y1 0.00131(12) 0.01344(12) O3z1 -0.00022(16) 0.00036(16) O3x2 -0.0008(5) -0.0002(5) O3y2 0.00004(19) 0.00000(18) O3z2 0.0002(4) -0.0003(4) N1x1 0 0 N1y1 0.00339(13) 0.01261(13) N1z1 0 0 N1x2 -0.0009(4) -0.0004(4) N1y2 0 0 N1z2 -0.0009(4) 0.0005(4) C1x1 0.00023(16) -0.00122(15) C1y1 0.00080(10) 0.01314(11) C1z1 0.00067(15) -0.00030(15) C1x2 0.0000(4) 0.0007(4) C1y2 -0.00004(16) -0.00010(19) C1z2 -0.0003(4) -0.0001(4) C3x1 0 0 C3y1 0.00067(19) 0.01261(19) C3z1 0 0 C3x2 -0.0004(6) 0.0000(6) C3y2 0 0 C3z2 -0.0005(6) 0.0004(6) C2x1 0 0 C2y1 0.00038(15) 0.01381(15) C2z1 0 0 H1x1 0.0016(4) -0.0011(4) H1y1 -0.0007(3) 0.0140(3) H1z1 0.0014(4) 0.0002(4) H1x2 0.0001(10) 0.0008(11) H1y2 -0.0003(4) 0.0002(5) H1z2 0.0010(10) 0.0001(9) H2x1 0 0 H2y1 -0.0014(3) 0.0133(3) H2z1 0 0 H2x2 -0.0006(15) -0.0001(15) H2y2 0 0 H2z2 0.0003(11) 0.0003(11) H1nx1 0 0 H1ny1 0.0095(4) 0.0123(4) H1nz1 0 0 H1nx2 0.0046(14) -0.0031(15) H1ny2 0 0 H1nz2 0.0024(13) -0.0026(13) H3ax1 0 0 H3ay1 -0.0050(5) 0.0130(5) H3az1 0 0 H3ax2 0.0000(17) -0.0055(17) H3ay2 0 0 H3az2 0.0002(16) -0.0035(16) H2nx1 -0.0005(3) -0.0002(3) H2ny1 0.0028(2) 0.0133(2) H2nz1 -0.0036(3) 0.0003(3) H2nx2 0.0009(9) 0.0000(8) H2ny2 -0.0002(4) 0.0000(4) H2nz2 0.0013(8) 0.0001(8) H3bx1 0.0002(4) 0.0003(4) H3by1 0.0027(3) 0.0125(3) H3bz1 0.0042(5) 0.0003(5) H3bx2 0.0010(11) -0.0011(12) H3by2 0.0006(6) -0.0003(6) H3bz2 0.0011(13) 0.0001(13) loop_ _atom_site_U_Fourier_id _atom_site_U_Fourier_atom_site_label _atom_site_U_Fourier_tens_elem _atom_site_U_Fourier_wave_vector_seq_id Co1U111 Co1 U11 1 Co1U221 Co1 U22 1 Co1U331 Co1 U33 1 Co1U121 Co1 U12 1 Co1U131 Co1 U13 1 Co1U231 Co1 U23 1 O1U111 O1 U11 1 O1U221 O1 U22 1 O1U331 O1 U33 1 O1U121 O1 U12 1 O1U131 O1 U13 1 O1U231 O1 U23 1 O2U111 O2 U11 1 O2U221 O2 U22 1 O2U331 O2 U33 1 O2U121 O2 U12 1 O2U131 O2 U13 1 O2U231 O2 U23 1 O3U111 O3 U11 1 O3U221 O3 U22 1 O3U331 O3 U33 1 O3U121 O3 U12 1 O3U131 O3 U13 1 O3U231 O3 U23 1 N1U111 N1 U11 1 N1U221 N1 U22 1 N1U331 N1 U33 1 N1U121 N1 U12 1 N1U131 N1 U13 1 N1U231 N1 U23 1 C1U111 C1 U11 1 C1U221 C1 U22 1 C1U331 C1 U33 1 C1U121 C1 U12 1 C1U131 C1 U13 1 C1U231 C1 U23 1 C3U111 C3 U11 1 C3U221 C3 U22 1 C3U331 C3 U33 1 C3U121 C3 U12 1 C3U131 C3 U13 1 C3U231 C3 U23 1 C2U111 C2 U11 1 C2U221 C2 U22 1 C2U331 C2 U33 1 C2U121 C2 U12 1 C2U131 C2 U13 1 C2U231 C2 U23 1 H1U111 H1 U11 1 H1U221 H1 U22 1 H1U331 H1 U33 1 H1U121 H1 U12 1 H1U131 H1 U13 1 H1U231 H1 U23 1 H2U111 H2 U11 1 H2U221 H2 U22 1 H2U331 H2 U33 1 H2U121 H2 U12 1 H2U131 H2 U13 1 H2U231 H2 U23 1 H1nU111 H1n U11 1 H1nU221 H1n U22 1 H1nU331 H1n U33 1 H1nU121 H1n U12 1 H1nU131 H1n U13 1 H1nU231 H1n U23 1 H3aU111 H3a U11 1 H3aU221 H3a U22 1 H3aU331 H3a U33 1 H3aU121 H3a U12 1 H3aU131 H3a U13 1 H3aU231 H3a U23 1 H2nU111 H2n U11 1 H2nU221 H2n U22 1 H2nU331 H2n U33 1 H2nU121 H2n U12 1 H2nU131 H2n U13 1 H2nU231 H2n U23 1 H3bU111 H3b U11 1 H3bU221 H3b U22 1 H3bU331 H3b U33 1 H3bU121 H3b U12 1 H3bU131 H3b U13 1 H3bU231 H3b U23 1 loop_ _atom_site_U_Fourier_param_id _atom_site_U_Fourier_param_cos _atom_site_U_Fourier_param_sin Co1U111 0.006(2) 0 Co1U221 -0.006(3) 0 Co1U331 0.003(2) 0 Co1U121 -0.0015(17) 0 Co1U131 -0.0001(18) 0 Co1U231 -0.0016(16) 0 O1U111 -0.0009(7) 0.0028(7) O1U221 0.0001(8) -0.0014(8) O1U331 0.0004(7) 0.0014(7) O1U121 -0.0005(6) 0.0002(6) O1U131 0.0010(6) 0.0006(6) O1U231 -0.0012(6) -0.0014(6) O2U111 0.0008(7) -0.0024(7) O2U221 0.0000(8) -0.0006(8) O2U331 0.0007(7) 0.0009(7) O2U121 0.0001(6) 0.0013(6) O2U131 0.0000(6) 0.0002(6) O2U231 -0.0002(5) 0.0008(6) O3U111 -0.0009(8) 0.0019(8) O3U221 0.0004(8) -0.0026(8) O3U331 -0.0007(7) 0.0009(7) O3U121 0.0008(6) 0.0000(6) O3U131 -0.0010(6) -0.0011(6) O3U231 -0.0009(6) -0.0013(6) N1U111 0 0 N1U221 0 0 N1U331 0 0 N1U121 0.0015(7) 0.0008(7) N1U131 0 0 N1U231 -0.0017(6) -0.0012(6) C1U111 0.0013(6) -0.0014(6) C1U221 -0.0004(7) 0.0011(7) C1U331 0.0004(6) -0.0013(6) C1U121 0.0002(6) -0.0005(6) C1U131 0.0006(5) -0.0002(6) C1U231 -0.0007(5) 0.0001(5) C3U111 0 0 C3U221 0 0 C3U331 0 0 C3U121 0.0007(10) 0.0035(10) C3U131 0 0 C3U231 0.0011(9) -0.0012(9) C2U111 0 0 C2U221 0 0 C2U331 0 0 C2U121 0.0006(7) -0.0003(7) C2U131 0 0 C2U231 -0.0006(7) 0.0009(7) H1U111 -0.0009(18) 0.0033(18) H1U221 0.002(2) 0.005(2) H1U331 0.0013(18) 0.0019(17) H1U121 0.0008(17) -0.0032(16) H1U131 -0.0008(14) -0.0007(15) H1U231 -0.0010(15) -0.0050(16) H2U111 0 0 H2U221 0 0 H2U331 0 0 H2U121 -0.001(2) -0.002(2) H2U131 0 0 H2U231 0.0019(16) -0.0019(16) H1nU111 0 0 H1nU221 0 0 H1nU331 0 0 H1nU121 0.003(2) 0.003(2) H1nU131 0 0 H1nU231 0.002(2) 0.005(2) H3aU111 0 0 H3aU221 0 0 H3aU331 0 0 H3aU121 0.003(3) 0.003(3) H3aU131 0 0 H3aU231 0.008(3) 0.004(3) H2nU111 -0.0033(16) -0.0020(14) H2nU221 0.0036(16) 0.0030(16) H2nU331 -0.0020(15) -0.0027(15) H2nU121 0.0015(14) 0.0027(14) H2nU131 0.0016(12) -0.0061(12) H2nU231 -0.0012(13) 0.0003(12) H3bU111 -0.001(2) -0.0019(18) H3bU221 -0.001(2) 0.000(2) H3bU331 0.003(3) 0.001(3) H3bU121 -0.0011(19) -0.0005(19) H3bU131 -0.0007(18) 0.0023(17) H3bU231 -0.002(2) -0.001(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_ssg_symmetry_1 _geom_bond_site_ssg_symmetry_2 _geom_bond_distance_av _geom_bond_distance_min _geom_bond_distance_max _geom_bond_publ_flag Co1 O1 ? ? 2.084(5) 2.075(6) 2.100(6) ? Co1 O1 ? 5_6555 2.084(5) 2.075(6) 2.100(6) ? Co1 O2 ? 2_6555 2.112(3) 2.107(4) 2.117(4) ? Co1 O2 ? 6_4545 2.112(3) 2.107(4) 2.117(4) ? Co1 O3 ? ? 2.098(5) 2.095(6) 2.101(6) ? Co1 O3 ? 5_6555 2.098(5) 2.095(6) 2.101(6) ? O1 C1 ? ? 1.251(7) 1.244(7) 1.255(7) ? O2 C1 ? ? 1.262(5) 1.255(5) 1.268(5) ? O3 C2 ? ? 1.254(4) 1.252(4) 1.258(4) ? N1 C3 ? ? 1.481(6) 1.474(7) 1.486(7) ? C3 H3a ? ? 1.068(15) 1.037(15) 1.099(15) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_ssg_symmetry_1 _geom_angle_site_ssg_symmetry_2 _geom_angle_site_ssg_symmetry_3 _geom_angle_av _geom_angle_min _geom_angle_max _geom_angle_publ_flag O1 Co1 O1 ? ? 5_6555 179.8(3) 179.6(2) 180.0(5) ? O1 Co1 O2 ? ? 2_6555 93.23(18) 92.8(2) 93.41(15) ? O1 Co1 O2 ? ? 6_4545 86.77(17) 86.48(16) 87.0(2) ? O1 Co1 O3 ? ? ? 87.94(19) 87.6(2) 88.22(18) ? O1 Co1 O3 ? ? 5_6555 92.1(2) 91.79(17) 92.3(2) ? O1 Co1 O2 5_6555 ? 2_6555 86.77(17) 86.48(16) 87.0(2) ? O1 Co1 O2 5_6555 ? 6_4545 93.23(18) 92.8(2) 93.41(15) ? O1 Co1 O3 5_6555 ? ? 92.1(2) 91.79(17) 92.3(2) ? O1 Co1 O3 5_6555 ? 5_6555 87.94(19) 87.6(2) 88.22(18) ? O2 Co1 O2 2_6555 ? 6_4545 179.8(3) 179.6(2) 180.0(5) ? O2 Co1 O3 2_6555 ? ? 87.79(18) 87.51(16) 88.20(15) ? O2 Co1 O3 2_6555 ? 5_6555 92.21(18) 91.71(16) 92.5(2) ? O2 Co1 O3 6_4545 ? ? 92.21(18) 91.71(16) 92.5(2) ? O2 Co1 O3 6_4545 ? 5_6555 87.79(18) 87.51(16) 88.20(15) ? O3 Co1 O3 ? ? 5_6555 179.8(3) 179.6(3) 180.0(5) ? Co1 O1 C1 ? ? ? 121.2(3) 120.8(4) 121.8(3) ? Co1 O2 C1 2_6545 ? ? 120.0(2) 119.5(2) 120.4(2) ? Co1 O3 C2 ? ? ? 121.4(3) 121.1(3) 122.1(3) ? O1 C1 O2 ? ? ? 124.1(4) 123.5(4) 124.5(4) ? N1 C3 H3a ? ? ? 109.2(9) 106.8(9) 111.3(9) ? O3 C2 O3 ? ? 7_5555 123.7(3) 123.5(3) 123.9(3) ? data_II _chemical_formula_sum 'C4 H9 Co1 N1 O6' _chemical_formula_weight 226 _chemical_absolute_configuration ? _space_group_crystal_system orthorhombic _space_group_ssg_name Pnma(00\g)0s0 loop_ _space_group_symop_ssg_id _space_group_symop_ssg_operation_algebraic 1 x1,x2,x3,x4 2 -x1+1/2,-x2,x3+1/2,x4+1/2 3 -x1,x2+1/2,-x3,-x4+1/2 4 x1+1/2,-x2+1/2,-x3+1/2,-x4 5 -x1,-x2,-x3,-x4 6 x1+1/2,x2,-x3+1/2,-x4+1/2 7 x1,-x2+1/2,x3,x4+1/2 8 -x1+1/2,x2+1/2,x3+1/2,x4 _cell_length_a 8.2556(2) _cell_length_b 11.6519(3) _cell_length_c 8.1508(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 784.05(4) _cell_modulation_dimension 1 loop_ _cell_wave_vector_seq_id _cell_wave_vector_x _cell_wave_vector_y _cell_wave_vector_z 1 0.000000 0.000000 0.143000 _cell_formula_units_Z 4 _cell_measurement_reflns_used 1445 _cell_measurement_theta_min 5.13 _cell_measurement_theta_max 61.25 _cell_measurement_temperature 106 _exptl_crystal_type_of_structure mod _exptl_crystal_density_diffrn 1.915 _exptl_crystal_F_000 158.404 _exptl_absorpt_coefficient_mu 0.2417 _exptl_crystal_description prism _exptl_crystal_size_max 5 _exptl_crystal_size_mid 4 _exptl_crystal_size_min 4 _exptl_crystal_size_rad 4 _exptl_crystal_colour red _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'absorption corretion done through d19face, d19abs and d19abscan programs from ILL' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist ? ? ? ? _diffrn_ambient_temperature 106 _diffrn_source_power 55000 _diffrn_radiation_type neutron _diffrn_source 'neutron source' _diffrn_source_type 'ILL High Flux Reactor, beam H11' _diffrn_radiation_monochromator 'copper 331' _diffrn_measurement_device_type 'D19 position-sensitive detector diffractometer' _diffrn_measurement_method 'omega step-scans' _diffrn_detector_area_resol_mean 210 _diffrn_radiation_wavelength 1.4569 _diffrn_reflns_number 22676 _diffrn_reflns_theta_min 5.13 _diffrn_reflns_theta_max 61.25 _diffrn_reflns_theta_full 61.25 _diffrn_measured_fraction_theta_max 0.98 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_av_R_equivalents 0.1122 _diffrn_reflns_av_unetI/netI 0.0121 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_index_m_1_min -2 _diffrn_reflns_limit_index_m_1_max 2 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_radiation_probe neutron _reflns_number_total 3544 _reflns_number_gt 2370 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0836 _refine_ls_wR_factor_gt 0.0965 _refine_ls_R_factor_all 0.1012 _refine_ls_wR_factor_ref 0.0982 _refine_ls_goodness_of_fit_ref 4.79 _refine_ls_goodness_of_fit_gt 5.91 _refine_ls_number_reflns 3544 _refine_ls_number_parameters 333 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/(\s^2^(F)+0.0001F^2^) _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max 0.0044 _refine_ls_shift/su_mean 0.0007 _refine_ls_extinction_method none loop_ _atom_type_symbol _atom_type_scat_length_neutron _atom_type_scat_source C 6.646 International_Tables_Vol_C H -3.739 International_Tables_Vol_C Co 2.490 International_Tables_Vol_C N 9.360 International_Tables_Vol_C O 5.803 International_Tables_Vol_C loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.5 0 0 Uani 0.0259(10) 4 1 d ? ? ? O1 O 0.59580(13) -0.07083(9) -0.21413(13) Uani 0.0280(4) 8 1 d ? ? ? O2 O 0.77265(13) -0.05973(9) -0.41846(12) Uani 0.0272(3) 8 1 d ? ? ? O3 O 0.47451(14) 0.15486(9) -0.12793(12) Uani 0.0274(3) 8 1 d ? ? ? N1 N 0.91509(12) 0.25 -0.03026(13) Uani 0.0303(4) 4 1 d ? ? ? C1 C 0.71984(12) -0.02973(9) -0.27964(12) Uani 0.0272(3) 8 1 d ? ? ? C3 C 1.08639(17) 0.25 0.0242(2) Uani 0.0345(5) 4 1 d ? ? ? C2 C 0.49064(17) 0.25 -0.05694(17) Uani 0.0274(4) 4 1 d ? ? ? H1 H 0.7884(3) 0.0342(2) -0.2126(3) Uani 0.0560(9) 8 1 d ? ? ? H2 H 0.5192(5) 0.25 0.0748(4) Uani 0.0468(11) 4 1 d ? ? ? H1n H 0.9124(4) 0.25 -0.1553(4) Uani 0.0530(12) 4 1 d ? ? ? H3a H 1.0895(4) 0.25 0.1559(5) Uani 0.0669(15) 4 1 d ? ? ? H2n H 0.8547(3) 0.17859(19) 0.0128(3) Uani 0.0426(7) 8 1 d ? ? ? H3b H 1.1454(4) 0.3244(3) -0.0196(4) Uani 0.0673(10) 8 1 d ? ? ? loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co1 Co 0.0255(17) 0.027(2) 0.0250(17) -0.0008(12) 0.0017(13) 0.0013(13) O1 O 0.0280(6) 0.0288(7) 0.0273(6) -0.0043(4) 0.0031(4) -0.0019(4) O2 O 0.0260(6) 0.0302(6) 0.0255(6) -0.0019(4) 0.0029(4) -0.0003(4) O3 O 0.0332(6) 0.0228(6) 0.0261(5) -0.0018(4) -0.0021(4) -0.0011(4) N1 N 0.0312(6) 0.0294(7) 0.0304(7) 0 0.0026(4) 0 C1 C 0.0256(6) 0.0280(6) 0.0279(6) -0.0028(4) 0.0012(4) -0.0004(4) C3 C 0.0290(9) 0.0361(10) 0.0383(10) 0 0.0002(6) 0 C2 C 0.0297(7) 0.0243(8) 0.0282(8) 0 -0.0027(5) 0 H1 H 0.0549(15) 0.0609(16) 0.0521(15) -0.0250(12) 0.0171(11) -0.0239(12) H2 H 0.068(2) 0.0373(17) 0.0347(16) 0 -0.0108(13) 0 H1n H 0.0450(18) 0.076(2) 0.038(2) 0 0.0005(12) 0 H3a H 0.051(2) 0.102(3) 0.048(2) 0 -0.0046(15) 0 H2n H 0.0457(12) 0.0360(13) 0.0460(11) -0.0065(10) 0.0027(9) 0.0023(9) H3b H 0.0496(15) 0.0658(18) 0.0867(18) -0.0172(14) -0.0035(13) 0.0179(15) loop_ _jana_atom_site_ADP_C_label _jana_atom_site_ADP_C_type_symbol _jana_atom_site_ADP_C_111 _jana_atom_site_ADP_C_112 _jana_atom_site_ADP_C_113 _jana_atom_site_ADP_C_122 _jana_atom_site_ADP_C_123 _jana_atom_site_ADP_C_133 _jana_atom_site_ADP_C_222 _jana_atom_site_ADP_C_223 _jana_atom_site_ADP_C_233 _jana_atom_site_ADP_C_333 Co1 Co 0 0 0 0 0 0 0 0 0 0 O2 O -0.0014(13) -0.0008(4) -0.0002(7) 0.0002(3) 0.0002(2) -0.0011(6) 0.0001(4) 0.0002(3) 0.0005(3) 0.0016(10) O1 O 0.0045(9) -0.0003(3) -0.0011(5) 0.0010(3) -0.0006(2) 0.0012(6) -0.0001(4) -0.0006(3) -0.0001(4) -0.0039(13) O3 O 0.0011(9) 0.0008(3) 0.0006(5) 0.0000(3) 0.0006(2) 0.0007(5) 0.0002(5) 0.0003(3) 0.0003(4) 0.0004(10) N2 N 0.0030(12) 0 0.0004(8) 0.0009(4) 0 0.0017(10) 0 0.0005(4) 0 0.0006(17) loop_ _atom_site_Fourier_wave_vector_seq_id _jana_atom_site_Fourier_wave_vector_q1_coeff 1 1 2 2 loop_ _atom_site_displace_Fourier_id _atom_site_displace_Fourier_atom_site_label _atom_site_displace_Fourier_axis _atom_site_displace_Fourier_wave_vector_seq_id Co1x1 Co1 x 1 Co1y1 Co1 y 1 Co1z1 Co1 z 1 O1x1 O1 x 1 O1y1 O1 y 1 O1z1 O1 z 1 O1x2 O1 x 2 O1y2 O1 y 2 O1z2 O1 z 2 O2x1 O2 x 1 O2y1 O2 y 1 O2z1 O2 z 1 O3x1 O3 x 1 O3y1 O3 y 1 O3z1 O3 z 1 O3x2 O3 x 2 O3y2 O3 y 2 O3z2 O3 z 2 N1x1 N1 x 1 N1y1 N1 y 1 N1z1 N1 z 1 N1x2 N1 x 2 N1y2 N1 y 2 N1z2 N1 z 2 C1x1 C1 x 1 C1y1 C1 y 1 C1z1 C1 z 1 C1x2 C1 x 2 C1y2 C1 y 2 C1z2 C1 z 2 C3x1 C3 x 1 C3y1 C3 y 1 C3z1 C3 z 1 C3x2 C3 x 2 C3y2 C3 y 2 C3z2 C3 z 2 C2x1 C2 x 1 C2y1 C2 y 1 C2z1 C2 z 1 H1x1 H1 x 1 H1y1 H1 y 1 H1z1 H1 z 1 H1x2 H1 x 2 H1y2 H1 y 2 H1z2 H1 z 2 H2x1 H2 x 1 H2y1 H2 y 1 H2z1 H2 z 1 H2x2 H2 x 2 H2y2 H2 y 2 H2z2 H2 z 2 H1nx1 H1n x 1 H1ny1 H1n y 1 H1nz1 H1n z 1 H1nx2 H1n x 2 H1ny2 H1n y 2 H1nz2 H1n z 2 H3ax1 H3a x 1 H3ay1 H3a y 1 H3az1 H3a z 1 H3ax2 H3a x 2 H3ay2 H3a y 2 H3az2 H3a z 2 H2nx1 H2n x 1 H2ny1 H2n y 1 H2nz1 H2n z 1 H2nx2 H2n x 2 H2ny2 H2n y 2 H2nz2 H2n z 2 H3bx1 H3b x 1 H3by1 H3b y 1 H3bz1 H3b z 1 H3bx2 H3b x 2 H3by2 H3b y 2 H3bz2 H3b z 2 loop_ _atom_site_displace_Fourier_param_id _atom_site_displace_Fourier_param_cos _atom_site_displace_Fourier_param_sin Co1x1 0 -0.0022(5) Co1y1 0 0.0229(4) Co1z1 0 0.0004(5) O1x1 -0.00242(16) -0.00208(15) O1y1 0.00359(12) 0.02258(13) O1z1 0.00021(16) 0.00026(16) O1x2 0.0000(3) 0.0003(3) O1y2 0.00046(15) 0.00006(15) O1z2 0.0002(2) 0.0001(3) O2x1 0.00064(16) -0.00222(15) O2y1 0.00128(12) 0.02271(12) O2z1 0.00287(15) -0.00030(16) O3x1 -0.00358(16) -0.00162(15) O3y1 0.00228(12) 0.02286(13) O3z1 -0.00049(14) 0.00031(15) O3x2 0.0004(3) 0.0000(3) O3y2 -0.00009(14) 0.00005(14) O3z2 0.0001(2) -0.0004(2) N1x1 0 0 N1y1 0.00602(13) 0.02153(13) N1z1 0 0 N1x2 -0.0001(3) -0.0003(3) N1y2 0 0 N1z2 -0.0003(2) 0.0005(3) C1x1 0.00040(14) -0.00191(13) C1y1 0.00127(10) 0.02244(11) C1z1 0.00130(14) 0.00008(14) C1x2 0.0001(3) 0.0004(3) C1y2 0.00023(12) -0.00021(13) C1z2 -0.0002(2) -0.0001(2) C3x1 0 0 C3y1 0.00151(18) 0.02164(19) C3z1 0 0 C3x2 0.0008(4) 0.0008(4) C3y2 0 0 C3z2 -0.0007(4) 0.0003(4) C2x1 0 0 C2y1 0.00093(15) 0.02321(15) C2z1 0 0 H1x1 0.0025(4) -0.0017(3) H1y1 -0.0011(3) 0.0228(3) H1z1 0.0022(3) 0.0002(4) H1x2 0.0005(7) 0.0019(7) H1y2 -0.0011(3) -0.0003(3) H1z2 0.0012(6) 0.0007(6) H2x1 0 0 H2y1 -0.0031(3) 0.0224(3) H2z1 0 0 H2x2 -0.0005(9) 0.0005(9) H2y2 0 0 H2z2 0.0004(7) -0.0012(7) H1nx1 0 0 H1ny1 0.0148(4) 0.0205(4) H1nz1 0 0 H1nx2 0.0013(9) 0.0007(9) H1ny2 0 0 H1nz2 -0.0016(8) -0.0015(8) H3ax1 0 0 H3ay1 -0.0082(5) 0.0223(5) H3az1 0 0 H3ax2 -0.0023(11) -0.0012(11) H3ay2 0 0 H3az2 -0.0004(9) -0.0001(9) H2nx1 -0.0008(3) -0.0002(3) H2ny1 0.0038(2) 0.0220(3) H2nz1 -0.0055(3) 0.0003(3) H2nx2 0.0004(6) -0.0004(6) H2ny2 0.0003(3) 0.0001(3) H2nz2 0.0001(5) -0.0002(5) H3bx1 0.0005(4) 0.0002(4) H3by1 0.0044(3) 0.0211(3) H3bz1 0.0077(4) -0.0003(4) H3bx2 0.0020(7) -0.0001(7) H3by2 -0.0004(4) -0.0003(4) H3bz2 -0.0003(7) -0.0016(8) loop_ _atom_site_U_Fourier_id _atom_site_U_Fourier_atom_site_label _atom_site_U_Fourier_tens_elem _atom_site_U_Fourier_wave_vector_seq_id Co1U111 Co1 U11 1 Co1U221 Co1 U22 1 Co1U331 Co1 U33 1 Co1U121 Co1 U12 1 Co1U131 Co1 U13 1 Co1U231 Co1 U23 1 O1U111 O1 U11 1 O1U221 O1 U22 1 O1U331 O1 U33 1 O1U121 O1 U12 1 O1U131 O1 U13 1 O1U231 O1 U23 1 O2U111 O2 U11 1 O2U221 O2 U22 1 O2U331 O2 U33 1 O2U121 O2 U12 1 O2U131 O2 U13 1 O2U231 O2 U23 1 O3U111 O3 U11 1 O3U221 O3 U22 1 O3U331 O3 U33 1 O3U121 O3 U12 1 O3U131 O3 U13 1 O3U231 O3 U23 1 N1U111 N1 U11 1 N1U221 N1 U22 1 N1U331 N1 U33 1 N1U121 N1 U12 1 N1U131 N1 U13 1 N1U231 N1 U23 1 C1U111 C1 U11 1 C1U221 C1 U22 1 C1U331 C1 U33 1 C1U121 C1 U12 1 C1U131 C1 U13 1 C1U231 C1 U23 1 C3U111 C3 U11 1 C3U221 C3 U22 1 C3U331 C3 U33 1 C3U121 C3 U12 1 C3U131 C3 U13 1 C3U231 C3 U23 1 C2U111 C2 U11 1 C2U221 C2 U22 1 C2U331 C2 U33 1 C2U121 C2 U12 1 C2U131 C2 U13 1 C2U231 C2 U23 1 H1U111 H1 U11 1 H1U221 H1 U22 1 H1U331 H1 U33 1 H1U121 H1 U12 1 H1U131 H1 U13 1 H1U231 H1 U23 1 H2U111 H2 U11 1 H2U221 H2 U22 1 H2U331 H2 U33 1 H2U121 H2 U12 1 H2U131 H2 U13 1 H2U231 H2 U23 1 H1nU111 H1n U11 1 H1nU221 H1n U22 1 H1nU331 H1n U33 1 H1nU121 H1n U12 1 H1nU131 H1n U13 1 H1nU231 H1n U23 1 H3aU111 H3a U11 1 H3aU221 H3a U22 1 H3aU331 H3a U33 1 H3aU121 H3a U12 1 H3aU131 H3a U13 1 H3aU231 H3a U23 1 H2nU111 H2n U11 1 H2nU221 H2n U22 1 H2nU331 H2n U33 1 H2nU121 H2n U12 1 H2nU131 H2n U13 1 H2nU231 H2n U23 1 H3bU111 H3b U11 1 H3bU221 H3b U22 1 H3bU331 H3b U33 1 H3bU121 H3b U12 1 H3bU131 H3b U13 1 H3bU231 H3b U23 1 loop_ _atom_site_U_Fourier_param_id _atom_site_U_Fourier_param_cos _atom_site_U_Fourier_param_sin Co1U111 0.002(2) 0 Co1U221 -0.001(3) 0 Co1U331 -0.001(2) 0 Co1U121 -0.0015(17) 0 Co1U131 -0.0004(17) 0 Co1U231 -0.0018(17) 0 O1U111 -0.0004(6) 0.0019(7) O1U221 0.0001(8) -0.0002(8) O1U331 0.0004(6) -0.0002(7) O1U121 -0.0003(6) 0.0005(6) O1U131 0.0002(5) 0.0002(5) O1U231 -0.0004(5) -0.0016(6) O2U111 -0.0001(6) -0.0005(6) O2U221 0.0000(8) -0.0007(8) O2U331 0.0002(7) 0.0000(6) O2U121 -0.0004(6) 0.0007(6) O2U131 0.0005(5) -0.0004(5) O2U231 -0.0007(5) 0.0006(6) O3U111 -0.0004(7) 0.0012(7) O3U221 0.0013(8) -0.0015(8) O3U331 -0.0004(6) 0.0004(6) O3U121 -0.0009(6) 0.0008(6) O3U131 -0.0010(5) -0.0008(5) O3U231 -0.0001(5) -0.0007(5) N1U111 0 0 N1U221 0 0 N1U331 0 0 N1U121 -0.0003(7) 0.0004(6) N1U131 0 0 N1U231 -0.0006(6) -0.0010(6) C1U111 -0.0001(5) -0.0010(6) C1U221 0.0002(7) 0.0011(7) C1U331 0.0000(6) 0.0004(6) C1U121 0.0003(5) -0.0005(5) C1U131 0.0004(5) -0.0002(5) C1U231 0.0001(5) 0.0006(5) C3U111 0 0 C3U221 0 0 C3U331 0 0 C3U121 -0.0008(9) 0.0036(9) C3U131 0 0 C3U231 0.0010(9) -0.0005(9) C2U111 0 0 C2U221 0 0 C2U331 0 0 C2U121 0.0000(7) -0.0001(7) C2U131 0 0 C2U231 -0.0003(7) 0.0016(7) H1U111 -0.0012(16) 0.0016(16) H1U221 0.0001(19) 0.002(2) H1U331 0.0028(16) -0.0006(16) H1U121 0.0018(16) -0.0009(15) H1U131 -0.0021(13) -0.0015(14) H1U231 -0.0025(14) -0.0021(14) H2U111 0 0 H2U221 0 0 H2U331 0 0 H2U121 -0.0010(19) -0.0049(19) H2U131 0 0 H2U231 0.0014(14) -0.0013(15) H1nU111 0 0 H1nU221 0 0 H1nU331 0 0 H1nU121 0.003(2) -0.001(2) H1nU131 0 0 H1nU231 0.0017(19) 0.0016(19) H3aU111 0 0 H3aU221 0 0 H3aU331 0 0 H3aU121 0.001(2) 0.002(3) H3aU131 0 0 H3aU231 0.009(2) 0.003(2) H2nU111 -0.0012(13) -0.0002(14) H2nU221 0.0019(15) 0.0016(15) H2nU331 -0.0002(13) 0.0000(14) H2nU121 -0.0002(13) 0.0003(13) H2nU131 0.0010(11) -0.0042(11) H2nU231 0.0011(12) 0.0006(12) H3bU111 -0.0012(16) -0.0027(16) H3bU221 -0.002(2) -0.001(2) H3bU331 0.003(2) 0.006(2) H3bU121 -0.0025(17) 0.0012(18) H3bU131 -0.0018(15) 0.0036(15) H3bU231 -0.0005(19) -0.0022(19) loop_ _jana_atom_site_ADP_C_Fourier_atom_site_label _jana_atom_site_ADP_C_Fourier_tens_elem _jana_atom_site_ADP_C_Fourier_wave_vector_seq_id _jana_atom_site_ADP_C_Fourier_param_cos _jana_atom_site_ADP_C_Fourier_param_sin Co1 C111 1 0 -0.008(4) Co1 C112 1 0 0.0031(15) Co1 C113 1 0 0.0012(19) Co1 C122 1 0 -0.0018(11) Co1 C123 1 0 0.0009(9) Co1 C133 1 0 0.0004(19) Co1 C222 1 0 0.0013(17) Co1 C223 1 0 -0.0002(11) Co1 C233 1 0 0.0027(13) Co1 C333 1 0 0.005(3) O2 C111 1 -0.0016(13) 0.0020(14) O2 C112 1 -0.0001(5) 0.0003(5) O2 C113 1 0.0021(8) 0.0017(7) O2 C122 1 -0.0002(4) 0.0001(3) O2 C123 1 0.0004(3) 0.0003(4) O2 C133 1 0.0008(7) 0.0005(6) O2 C222 1 0.0001(5) 0.0007(5) O2 C223 1 -0.0003(3) 0.0003(3) O2 C233 1 0.0007(4) 0.0002(5) O2 C333 1 0.0011(12) 0.0010(12) O1 C111 1 0.0013(11) 0.0003(11) O1 C112 1 0.0001(4) 0.0015(4) O1 C113 1 -0.0004(7) -0.0019(7) O1 C122 1 0.0004(3) 0.0003(3) O1 C123 1 -0.0005(3) -0.0006(3) O1 C133 1 0.0004(7) 0.0009(7) O1 C222 1 0.0004(5) 0.0016(5) O1 C223 1 0.0000(3) 0.0004(3) O1 C233 1 -0.0001(5) 0.0009(5) O1 C333 1 0.0008(16) -0.0007(17) O3 C111 1 0.0028(11) -0.0026(10) O3 C112 1 0.0000(4) 0.0009(4) O3 C113 1 0.0006(6) -0.0005(6) O3 C122 1 0.0005(4) -0.0001(4) O3 C123 1 0.0002(3) 0.0000(3) O3 C133 1 0.0007(6) -0.0010(6) O3 C222 1 -0.0006(7) 0.0018(7) O3 C223 1 0.0001(4) -0.0003(4) O3 C233 1 0.0002(5) 0.0005(6) O3 C333 1 -0.0006(11) 0.0012(11) N2 C111 1 0 0 N2 C112 1 0.0002(7) 0.0004(8) N2 C113 1 0 0 N2 C122 1 0 0 N2 C123 1 -0.0005(5) 0.0000(5) N2 C133 1 0 0 N2 C222 1 -0.0012(8) 0.0014(8) N2 C223 1 0 0 N2 C233 1 -0.0016(9) 0.0004(9) N2 C333 1 0 0 C1 C111 1 0.0010(13) -0.0017(14) C1 C112 1 0.0007(5) 0.0017(5) C1 C113 1 -0.0019(7) -0.0013(8) C1 C122 1 0.0002(4) 0.0005(4) C1 C123 1 -0.0003(3) 0.0002(4) C1 C133 1 -0.0005(9) 0.0001(9) C1 C222 1 -0.0008(6) 0.0014(6) C1 C223 1 -0.0004(4) -0.0001(4) C1 C233 1 0.0003(6) -0.0001(6) C1 C333 1 -0.0022(16) 0.0029(16) C3 C111 1 0 0 C3 C112 1 0.0007(9) -0.0012(9) C3 C113 1 0 0 C3 C122 1 0 0 C3 C123 1 0.0006(6) 0.0012(6) C3 C133 1 0 0 C3 C222 1 0.0013(12) 0.0020(12) C3 C223 1 0 0 C3 C233 1 0.0008(12) 0.0017(12) C3 C333 1 0 0 C2 C111 1 0 0 C2 C112 1 0.0001(5) 0.0012(6) C2 C113 1 0 0 C2 C122 1 0 0 C2 C123 1 0.0001(4) 0.0006(4) C2 C133 1 0 0 C2 C222 1 0.0001(10) 0.0023(11) C2 C223 1 0 0 C2 C233 1 -0.0007(10) 0.0024(10) C2 C333 1 0 0 H1c1 C111 1 0.004(3) 0.005(3) H1c1 C112 1 0.0020(13) -0.0015(14) H1c1 C113 1 -0.0031(18) -0.0050(18) H1c1 C122 1 -0.0003(10) 0.0015(10) H1c1 C123 1 -0.0009(8) 0.0019(9) H1c1 C133 1 0.0029(18) -0.0004(16) H1c1 C222 1 -0.0010(13) -0.0008(13) H1c1 C223 1 -0.0001(10) 0.0007(10) H1c1 C233 1 -0.0015(12) -0.0016(13) H1c1 C333 1 -0.002(3) -0.001(3) H1c2 C111 1 0 0 H1c2 C112 1 -0.0004(16) 0.0014(16) H1c2 C113 1 0 0 H1c2 C122 1 0 0 H1c2 C123 1 0.0006(9) 0.0000(10) H1c2 C133 1 0 0 H1c2 C222 1 0.0000(14) -0.0010(14) H1c2 C223 1 0 0 H1c2 C233 1 0.0018(15) 0.0024(17) H1c2 C333 1 0 0 H1n C111 1 0 0 H1n C112 1 -0.0004(15) 0.0010(15) H1n C113 1 0 0 H1n C122 1 0 0 H1n C123 1 -0.0004(13) -0.0008(12) H1n C133 1 0 0 H1n C222 1 0.004(2) 0.003(2) H1n C223 1 0 0 H1n C233 1 -0.002(3) 0.001(4) H1n C333 1 0 0 H1c C111 1 0 0 H1c C112 1 -0.0015(18) 0.0008(19) H1c C113 1 0 0 H1c C122 1 0 0 H1c C123 1 0.0004(14) -0.0014(13) H1c C133 1 0 0 H1c C222 1 -0.004(3) 0.002(3) H1c C223 1 0 0 H1c C233 1 0.002(3) 0.002(3) H1c C333 1 0 0 H2n C111 1 -0.003(2) -0.001(3) H2n C112 1 0.0015(11) -0.0019(12) H2n C113 1 0.0008(15) 0.0042(14) H2n C122 1 -0.0012(8) 0.0001(8) H2n C123 1 0.0009(8) 0.0009(8) H2n C133 1 0.0023(14) -0.0018(14) H2n C222 1 0.0007(13) 0.0003(12) H2n C223 1 -0.0012(8) 0.0005(9) H2n C233 1 -0.0010(11) 0.0008(11) H2n C333 1 0.000(3) 0.003(3) H2c C111 1 -0.003(3) 0.002(3) H2c C112 1 0.0025(16) -0.0012(17) H2c C113 1 0.001(2) 0.002(2) H2c C122 1 -0.0005(13) 0.0011(13) H2c C123 1 -0.0005(12) 0.0010(12) H2c C133 1 0.000(2) -0.002(2) H2c C222 1 0.003(2) 0.003(2) H2c C223 1 -0.0004(14) 0.0007(14) H2c C233 1 -0.0016(19) -0.0012(19) H2c C333 1 -0.001(4) -0.003(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_ssg_symmetry_1 _geom_bond_site_ssg_symmetry_2 _geom_bond_distance_av _geom_bond_distance_min _geom_bond_distance_max _geom_bond_publ_flag Co1 O1 ? ? 2.086(4) 2.080(5) 2.091(5) ? Co1 O1 ? 5_6555 2.086(4) 2.080(5) 2.091(5) ? Co1 O2 ? 2_6555 2.110(3) 2.102(4) 2.117(4) ? Co1 O2 ? 6_4545 2.110(3) 2.102(4) 2.117(4) ? Co1 O3 ? ? 2.095(4) 2.092(5) 2.099(5) ? Co1 O3 ? 5_6555 2.095(4) 2.092(5) 2.099(5) ? O1 C1 ? ? 1.251(5) 1.248(5) 1.253(5) ? O2 C1 ? ? 1.262(4) 1.258(4) 1.266(4) ? O3 C2 ? ? 1.258(4) 1.252(4) 1.266(4) ? N1 C3 ? ? 1.483(4) 1.473(4) 1.492(4) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_ssg_symmetry_1 _geom_angle_site_ssg_symmetry_2 _geom_angle_site_ssg_symmetry_3 _geom_angle_av _geom_angle_min _geom_angle_max _geom_angle_publ_flag O1 Co1 O1 ? ? 5_6555 179.9(3) 179.74(17) 180.0(5) ? O1 Co1 O2 ? ? 2_6555 93.28(14) 92.91(13) 93.52(13) ? O1 Co1 O2 ? ? 6_4545 86.72(14) 86.49(13) 87.10(13) ? O1 Co1 O3 ? ? ? 87.86(16) 87.39(13) 88.20(14) ? O1 Co1 O3 ? ? 5_6555 92.14(17) 91.87(15) 92.61(13) ? O1 Co1 O2 5_6555 ? 2_6555 86.72(14) 86.49(13) 87.10(13) ? O1 Co1 O2 5_6555 ? 6_4545 93.28(14) 92.91(13) 93.52(13) ? O1 Co1 O3 5_6555 ? ? 92.14(17) 91.87(15) 92.61(13) ? O1 Co1 O3 5_6555 ? 5_6555 87.86(16) 87.39(13) 88.20(14) ? O2 Co1 O2 2_6555 ? 6_4545 179.9(3) 179.8(2) 180.0(5) ? O2 Co1 O3 2_6555 ? ? 87.79(15) 87.41(11) 88.10(13) ? O2 Co1 O3 2_6555 ? 5_6555 92.21(15) 91.82(13) 92.59(11) ? O2 Co1 O3 6_4545 ? ? 92.21(15) 91.82(13) 92.59(11) ? O2 Co1 O3 6_4545 ? 5_6555 87.79(15) 87.41(11) 88.10(13) ? O3 Co1 O3 ? ? 5_6555 179.9(3) 179.82(15) 180.0(5) ? Co1 O1 C1 ? ? ? 121.1(3) 120.6(3) 121.9(3) ? Co1 O2 C1 2_6545 ? ? 119.9(2) 119.33(19) 120.27(19) ? Co1 O3 C2 ? ? ? 121.2(2) 120.6(2) 122.1(2) ? O1 C1 O2 ? ? ? 124.1(3) 123.9(3) 124.3(3) ? O3 C2 O3 ? ? 7_5555 123.7(2) 123.3(2) 124.0(2) ? data_III _chemical_formula_sum 'C4 H9 Co1 N1 O6' _chemical_formula_weight 226 _chemical_absolute_configuration ? _space_group_crystal_system orthorhombic _space_group_ssg_name Pnma(00\g)0s0 loop_ _space_group_symop_ssg_id _space_group_symop_ssg_operation_algebraic 1 x1,x2,x3,x4 2 -x1+1/2,-x2,x3+1/2,x4+1/2 3 -x1,x2+1/2,-x3,-x4+1/2 4 x1+1/2,-x2+1/2,-x3+1/2,-x4 5 -x1,-x2,-x3,-x4 6 x1+1/2,x2,-x3+1/2,-x4+1/2 7 x1,-x2+1/2,x3,x4+1/2 8 -x1+1/2,x2+1/2,x3+1/2,x4 _cell_length_a 8.2702(3) _cell_length_b 11.6766(4) _cell_length_c 8.1631(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 788.29(7) _cell_modulation_dimension 1 loop_ _cell_wave_vector_seq_id _cell_wave_vector_x _cell_wave_vector_y _cell_wave_vector_z 1 0.000000 0.000000 0.124700 _cell_formula_units_Z 4 _cell_measurement_reflns_used 1077 _cell_measurement_theta_min 4.8 _cell_measurement_theta_max 61.37 _cell_measurement_temperature 90 _exptl_crystal_type_of_structure mod _exptl_crystal_density_diffrn 1.9047 _exptl_crystal_F_000 158.404 _exptl_absorpt_coefficient_mu 0.2417 _exptl_crystal_description prism _exptl_crystal_size_max 5 _exptl_crystal_size_mid 4 _exptl_crystal_size_min 4 _exptl_crystal_size_rad 4 _exptl_crystal_colour red _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'absorption corretion done through d19face, d19abs and d19abscan programs from ILL' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist ? ? ? ? _diffrn_ambient_temperature 90 _diffrn_source_power 55000 _diffrn_radiation_type neutron _diffrn_source 'neutron source' _diffrn_source_type 'ILL High Flux Reactor, beam H11' _diffrn_radiation_monochromator 'copper 331' _diffrn_measurement_device_type 'D19 position-sensitive detector diffractometer' _diffrn_measurement_method 'omega step-scans' _diffrn_detector_area_resol_mean 210 _diffrn_radiation_wavelength 1.4569 _diffrn_reflns_number 24351 _diffrn_reflns_theta_min 4.8 _diffrn_reflns_theta_max 61.37 _diffrn_reflns_theta_full 34.37 _diffrn_measured_fraction_theta_max 0.92 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_av_R_equivalents 0.1439 _diffrn_reflns_av_unetI/netI 0.0185 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_index_m_1_min -3 _diffrn_reflns_limit_index_m_1_max 3 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_radiation_probe neutron _reflns_number_total 4617 _reflns_number_gt 2408 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.1030 _refine_ls_wR_factor_gt 0.1293 _refine_ls_R_factor_all 0.1449 _refine_ls_wR_factor_ref 0.1326 _refine_ls_goodness_of_fit_ref 5.06 _refine_ls_goodness_of_fit_gt 7.08 _refine_ls_number_reflns 4617 _refine_ls_number_parameters 333 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/(\s^2^(F)+0.0001F^2^) _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max 0.0053 _refine_ls_shift/su_mean 0.0006 _refine_diff_density_max 0.18 _refine_diff_density_min -0.67 _refine_ls_extinction_method none loop_ _atom_type_symbol _atom_type_scat_length_neutron _atom_type_scat_source C 6.646 International_Tables_Vol_C H -3.739 International_Tables_Vol_C Co 2.490 International_Tables_Vol_C N 9.360 International_Tables_Vol_C O 5.803 International_Tables_Vol_C loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.5 0 0 Uani 0.0242(16) 4 1 d ? ? ? O1 O 0.59560(17) -0.07082(12) -0.2141(3) Uani 0.0266(6) 8 1 d ? ? ? O2 O 0.77267(17) -0.05990(12) -0.4184(3) Uani 0.0264(5) 8 1 d ? ? ? O3 O 0.47468(18) 0.15492(12) -0.1285(3) Uani 0.0280(6) 8 1 d ? ? ? N1 N 0.91491(18) 0.25 -0.0300(3) Uani 0.0280(6) 4 1 d ? ? ? C1 C 0.71992(15) -0.02981(11) -0.2799(2) Uani 0.0253(5) 8 1 d ? ? ? C3 C 1.0871(2) 0.25 0.0231(5) Uani 0.0345(9) 4 1 d ? ? ? C2 C 0.4904(2) 0.25 -0.0576(4) Uani 0.0247(8) 4 1 d ? ? ? H1 H 0.7873(4) 0.0352(3) -0.2144(5) Uani 0.0522(13) 8 1 d ? ? ? H2 H 0.5206(7) 0.25 0.0770(9) Uani 0.0505(18) 4 1 d ? ? ? H1n H 0.9122(6) 0.25 -0.1563(10) Uani 0.056(2) 4 1 d ? ? ? H3a H 1.0899(6) 0.25 0.1590(11) Uani 0.063(2) 4 1 d ? ? ? H2n H 0.8545(4) 0.1784(2) 0.0132(5) Uani 0.0427(11) 8 1 d ? ? ? H3b H 1.1455(4) 0.3249(3) -0.0195(6) Uani 0.0624(15) 8 1 d ? ? ? loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co1 Co 0.026(2) 0.028(2) 0.019(4) -0.0003(15) 0.000(2) 0.0010(18) O1 O 0.0261(8) 0.0321(8) 0.0217(12) -0.0036(5) 0.0029(7) -0.0009(6) O2 O 0.0261(8) 0.0309(8) 0.0221(12) -0.0016(5) 0.0021(7) -0.0010(6) O3 O 0.0323(8) 0.0245(8) 0.0271(14) -0.0010(5) -0.0002(7) -0.0012(7) N1 N 0.0293(8) 0.0311(9) 0.0236(13) 0 0.0022(9) 0 C1 C 0.0263(7) 0.0312(8) 0.0182(11) -0.0018(5) 0.0028(6) 0.0000(5) C3 C 0.0275(11) 0.0391(13) 0.037(2) 0 0.0010(12) 0 C2 C 0.0279(9) 0.0281(11) 0.0183(18) 0 -0.0023(9) 0 H1 H 0.0546(19) 0.062(2) 0.040(3) -0.0239(14) 0.0155(17) -0.0201(16) H2 H 0.074(3) 0.039(2) 0.038(4) 0 -0.016(3) 0 H1n H 0.045(3) 0.064(3) 0.058(5) 0 -0.003(3) 0 H3a H 0.049(3) 0.096(4) 0.043(5) 0 -0.006(3) 0 H2n H 0.0424(16) 0.0411(17) 0.045(3) -0.0066(12) 0.0074(15) 0.0022(13) H3b H 0.0435(18) 0.063(2) 0.081(4) -0.0133(15) -0.0025(18) 0.0111(19) loop_ _atom_site_Fourier_wave_vector_seq_id _jana_atom_site_Fourier_wave_vector_q1_coeff 1 1 2 2 loop_ _atom_site_displace_Fourier_id _atom_site_displace_Fourier_atom_site_label _atom_site_displace_Fourier_axis _atom_site_displace_Fourier_wave_vector_seq_id Co1x1 Co1 x 1 Co1y1 Co1 y 1 Co1z1 Co1 z 1 O1x1 O1 x 1 O1y1 O1 y 1 O1z1 O1 z 1 O1x2 O1 x 2 O1y2 O1 y 2 O1z2 O1 z 2 O2x1 O2 x 1 O2y1 O2 y 1 O2z1 O2 z 1 O3x1 O3 x 1 O3y1 O3 y 1 O3z1 O3 z 1 O3x2 O3 x 2 O3y2 O3 y 2 O3z2 O3 z 2 N1x1 N1 x 1 N1y1 N1 y 1 N1z1 N1 z 1 N1x2 N1 x 2 N1y2 N1 y 2 N1z2 N1 z 2 C1x1 C1 x 1 C1y1 C1 y 1 C1z1 C1 z 1 C1x2 C1 x 2 C1y2 C1 y 2 C1z2 C1 z 2 C3x1 C3 x 1 C3y1 C3 y 1 C3z1 C3 z 1 C3x2 C3 x 2 C3y2 C3 y 2 C3z2 C3 z 2 C2x1 C2 x 1 C2y1 C2 y 1 C2z1 C2 z 1 H1x1 H1 x 1 H1y1 H1 y 1 H1z1 H1 z 1 H1x2 H1 x 2 H1y2 H1 y 2 H1z2 H1 z 2 H2x1 H2 x 1 H2y1 H2 y 1 H2z1 H2 z 1 H2x2 H2 x 2 H2y2 H2 y 2 H2z2 H2 z 2 H1nx1 H1n x 1 H1ny1 H1n y 1 H1nz1 H1n z 1 H1nx2 H1n x 2 H1ny2 H1n y 2 H1nz2 H1n z 2 H3ax1 H3a x 1 H3ay1 H3a y 1 H3az1 H3a z 1 H3ax2 H3a x 2 H3ay2 H3a y 2 H3az2 H3a z 2 H2nx1 H2n x 1 H2ny1 H2n y 1 H2nz1 H2n z 1 H2nx2 H2n x 2 H2ny2 H2n y 2 H2nz2 H2n z 2 H3bx1 H3b x 1 H3by1 H3b y 1 H3bz1 H3b z 1 H3bx2 H3b x 2 H3by2 H3b y 2 H3bz2 H3b z 2 loop_ _atom_site_displace_Fourier_param_id _atom_site_displace_Fourier_param_cos _atom_site_displace_Fourier_param_sin Co1x1 0 -0.0027(7) Co1y1 0 0.0306(6) Co1z1 0 0.0016(8) O1x1 -0.0031(2) -0.0026(2) O1y1 0.00439(15) 0.03072(17) O1z1 -0.0002(2) 0.0016(2) O1x2 0.0002(3) -0.0001(3) O1y2 0.00031(16) 0.00024(16) O1z2 -0.0005(3) -0.0006(3) O2x1 0.0009(2) -0.0026(2) O2y1 0.00157(15) 0.03060(17) O2z1 0.0035(2) -0.0012(2) O3x1 -0.0042(2) -0.0020(2) O3y1 0.00289(15) 0.03065(16) O3z1 -0.0008(2) 0.0015(3) O3x2 -0.0002(3) 0.0000(3) O3y2 0.00026(16) 0.00005(17) O3z2 -0.0006(3) -0.0014(3) N1x1 0 0 N1y1 0.00763(16) 0.02946(18) N1z1 0 0 N1x2 0.0000(3) -0.0007(3) N1y2 0 0 N1z2 -0.0008(3) -0.0006(3) C1x1 0.00017(18) -0.00227(18) C1y1 0.00151(13) 0.03029(16) C1z1 0.00258(18) -0.0003(2) C1x2 -0.0002(3) 0.0002(3) C1y2 -0.00004(14) -0.00008(15) C1z2 -0.0002(3) -0.0009(3) C3x1 0 0 C3y1 0.0019(2) 0.0297(3) C3z1 0 0 C3x2 0.0002(4) -0.0001(4) C3y2 0 0 C3z2 -0.0009(4) 0.0002(4) C2x1 0 0 C2y1 0.00124(18) 0.0309(2) C2z1 0 0 H1x1 0.0031(5) -0.0024(5) H1y1 -0.0011(3) 0.0307(4) H1z1 0.0025(4) 0.0000(5) H1x2 0.0007(7) 0.0014(7) H1y2 -0.0001(4) 0.0002(4) H1z2 0.0000(6) -0.0008(6) H2x1 0 0 H2y1 -0.0038(4) 0.0313(5) H2z1 0 0 H2x2 0.0005(10) -0.0010(10) H2y2 0 0 H2z2 -0.0007(9) 0.0006(8) H1nx1 0 0 H1ny1 0.0185(5) 0.0278(6) H1nz1 0 0 H1nx2 0.0017(10) -0.0004(10) H1ny2 0 0 H1nz2 0.0002(10) 0.0003(11) H3ax1 0 0 H3ay1 -0.0094(6) 0.0298(7) H3az1 0 0 H3ax2 0.0010(11) -0.0015(11) H3ay2 0 0 H3az2 -0.0007(10) 0.0015(10) H2nx1 -0.0015(4) -0.0007(4) H2ny1 0.0051(3) 0.0300(3) H2nz1 -0.0056(4) -0.0004(5) H2nx2 0.0022(6) 0.0001(6) H2ny2 -0.0003(3) -0.0003(3) H2nz2 -0.0003(6) 0.0011(6) H3bx1 0.0002(5) 0.0008(5) H3by1 0.0053(4) 0.0292(4) H3bz1 0.0090(6) -0.0009(6) H3bx2 0.0005(7) -0.0011(7) H3by2 0.0002(4) 0.0001(4) H3bz2 0.0010(8) -0.0013(8) loop_ _atom_site_U_Fourier_id _atom_site_U_Fourier_atom_site_label _atom_site_U_Fourier_tens_elem _atom_site_U_Fourier_wave_vector_seq_id Co1U111 Co1 U11 1 Co1U221 Co1 U22 1 Co1U331 Co1 U33 1 Co1U121 Co1 U12 1 Co1U131 Co1 U13 1 Co1U231 Co1 U23 1 O1U111 O1 U11 1 O1U221 O1 U22 1 O1U331 O1 U33 1 O1U121 O1 U12 1 O1U131 O1 U13 1 O1U231 O1 U23 1 O2U111 O2 U11 1 O2U221 O2 U22 1 O2U331 O2 U33 1 O2U121 O2 U12 1 O2U131 O2 U13 1 O2U231 O2 U23 1 O3U111 O3 U11 1 O3U221 O3 U22 1 O3U331 O3 U33 1 O3U121 O3 U12 1 O3U131 O3 U13 1 O3U231 O3 U23 1 N1U111 N1 U11 1 N1U221 N1 U22 1 N1U331 N1 U33 1 N1U121 N1 U12 1 N1U131 N1 U13 1 N1U231 N1 U23 1 C1U111 C1 U11 1 C1U221 C1 U22 1 C1U331 C1 U33 1 C1U121 C1 U12 1 C1U131 C1 U13 1 C1U231 C1 U23 1 C3U111 C3 U11 1 C3U221 C3 U22 1 C3U331 C3 U33 1 C3U121 C3 U12 1 C3U131 C3 U13 1 C3U231 C3 U23 1 C2U111 C2 U11 1 C2U221 C2 U22 1 C2U331 C2 U33 1 C2U121 C2 U12 1 C2U131 C2 U13 1 C2U231 C2 U23 1 H1U111 H1 U11 1 H1U221 H1 U22 1 H1U331 H1 U33 1 H1U121 H1 U12 1 H1U131 H1 U13 1 H1U231 H1 U23 1 H2U111 H2 U11 1 H2U221 H2 U22 1 H2U331 H2 U33 1 H2U121 H2 U12 1 H2U131 H2 U13 1 H2U231 H2 U23 1 H1nU111 H1n U11 1 H1nU221 H1n U22 1 H1nU331 H1n U33 1 H1nU121 H1n U12 1 H1nU131 H1n U13 1 H1nU231 H1n U23 1 H3aU111 H3a U11 1 H3aU221 H3a U22 1 H3aU331 H3a U33 1 H3aU121 H3a U12 1 H3aU131 H3a U13 1 H3aU231 H3a U23 1 H2nU111 H2n U11 1 H2nU221 H2n U22 1 H2nU331 H2n U33 1 H2nU121 H2n U12 1 H2nU131 H2n U13 1 H2nU231 H2n U23 1 H3bU111 H3b U11 1 H3bU221 H3b U22 1 H3bU331 H3b U33 1 H3bU121 H3b U12 1 H3bU131 H3b U13 1 H3bU231 H3b U23 1 loop_ _atom_site_U_Fourier_param_id _atom_site_U_Fourier_param_cos _atom_site_U_Fourier_param_sin Co1U111 -0.001(3) 0 Co1U221 0.006(3) 0 Co1U331 -0.005(3) 0 Co1U121 -0.006(2) 0 Co1U131 0.002(2) 0 Co1U231 -0.001(2) 0 O1U111 0.0006(8) -0.0002(9) O1U221 0.0015(10) -0.0002(10) O1U331 -0.0022(8) 0.0005(10) O1U121 -0.0003(7) 0.0004(8) O1U131 -0.0009(7) 0.0005(8) O1U231 -0.0017(7) -0.0007(10) O2U111 -0.0011(8) 0.0004(8) O2U221 -0.0004(10) -0.0002(10) O2U331 0.0021(9) -0.0001(10) O2U121 -0.0017(7) 0.0001(7) O2U131 0.0019(7) 0.0019(8) O2U231 -0.0009(7) 0.0025(10) O3U111 -0.0002(9) 0.0018(9) O3U221 0.0023(10) -0.0027(11) O3U331 -0.0086(9) -0.0016(11) O3U121 -0.0003(7) -0.0010(7) O3U131 0.0011(7) -0.0026(8) O3U231 -0.0004(7) -0.0015(10) N1U111 0 0 N1U221 0 0 N1U331 0 0 N1U121 -0.0019(8) -0.0006(8) N1U131 0 0 N1U231 -0.0023(8) 0.0000(12) C1U111 -0.0010(7) -0.0016(8) C1U221 -0.0008(8) -0.0003(9) C1U331 0.0027(7) 0.0040(8) C1U121 -0.0003(6) 0.0002(7) C1U131 -0.0001(6) -0.0003(7) C1U231 -0.0004(6) -0.0002(8) C3U111 0 0 C3U221 0 0 C3U331 0 0 C3U121 0.0010(12) 0.0013(12) C3U131 0 0 C3U231 0.0021(11) 0.0033(17) C2U111 0 0 C2U221 0 0 C2U331 0 0 C2U121 0.0004(8) 0.0013(9) C2U131 0 0 C2U231 -0.0030(8) 0.0070(14) H1U111 -0.003(2) 0.000(2) H1U221 -0.001(2) 0.000(3) H1U331 0.006(2) 0.003(2) H1U121 0.0003(19) -0.002(2) H1U131 0.0008(16) -0.0003(19) H1U231 -0.0041(17) 0.000(2) H2U111 0 0 H2U221 0 0 H2U331 0 0 H2U121 -0.005(2) -0.005(3) H2U131 0 0 H2U231 0.004(2) -0.002(3) H1nU111 0 0 H1nU221 0 0 H1nU331 0 0 H1nU121 0.008(3) 0.004(3) H1nU131 0 0 H1nU231 0.007(3) 0.000(4) H3aU111 0 0 H3aU221 0 0 H3aU331 0 0 H3aU121 0.004(3) 0.001(3) H3aU131 0 0 H3aU231 0.012(3) -0.008(4) H2nU111 0.0014(18) 0.0003(19) H2nU221 -0.0037(19) -0.005(2) H2nU331 0.016(2) 0.010(2) H2nU121 0.0010(16) 0.0000(17) H2nU131 0.0033(15) -0.0078(16) H2nU231 0.0041(15) 0.0002(19) H3bU111 -0.002(2) -0.001(2) H3bU221 -0.003(3) 0.005(3) H3bU331 0.006(3) -0.001(4) H3bU121 -0.001(2) -0.001(2) H3bU131 -0.004(2) 0.000(2) H3bU231 -0.001(2) 0.002(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_ssg_symmetry_1 _geom_bond_site_ssg_symmetry_2 _geom_bond_distance_av _geom_bond_distance_min _geom_bond_distance_max _geom_bond_publ_flag Co1 O1 ? ? 2.089(6) 2.084(7) 2.095(7) ? Co1 O1 ? 5_6555 2.089(6) 2.084(7) 2.095(7) ? Co1 O2 ? 2_6555 2.115(4) 2.104(6) 2.125(6) ? Co1 O2 ? 6_4545 2.115(4) 2.104(6) 2.125(6) ? Co1 O3 ? ? 2.102(5) 2.093(7) 2.115(7) ? Co1 O3 ? 5_6555 2.102(5) 2.093(7) 2.115(7) ? O1 C1 ? ? 1.255(6) 1.243(6) 1.268(6) ? O2 C1 ? ? 1.262(5) 1.250(5) 1.271(5) ? O3 C2 ? ? 1.260(5) 1.247(5) 1.268(5) ? N1 C3 ? ? 1.489(5) 1.483(5) 1.495(5) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_ssg_symmetry_1 _geom_angle_site_ssg_symmetry_2 _geom_angle_site_ssg_symmetry_3 _geom_angle_av _geom_angle_min _geom_angle_max _geom_angle_publ_flag O1 Co1 O1 ? ? 5_6555 179.8(4) 179.5(2) 180.0(5) ? O1 Co1 O2 ? ? 2_6555 93.36(19) 92.91(14) 93.66(14) ? O1 Co1 O2 ? ? 6_4545 86.64(19) 86.30(16) 87.09(14) ? O1 Co1 O3 ? ? ? 87.8(2) 87.23(19) 88.44(19) ? O1 Co1 O3 ? ? 5_6555 92.2(2) 92.03(19) 92.60(19) ? O1 Co1 O2 5_6555 ? 2_6555 86.64(19) 86.30(16) 87.09(14) ? O1 Co1 O2 5_6555 ? 6_4545 93.36(19) 92.91(14) 93.66(14) ? O1 Co1 O3 5_6555 ? ? 92.2(2) 92.03(19) 92.60(19) ? O1 Co1 O3 5_6555 ? 5_6555 87.8(2) 87.23(19) 88.44(19) ? O2 Co1 O2 2_6555 ? 6_4545 179.9(3) 179.9(3) 180.0(5) ? O2 Co1 O3 2_6555 ? ? 87.74(19) 87.35(16) 88.26(16) ? O2 Co1 O3 2_6555 ? 5_6555 92.26(19) 91.69(16) 92.62(14) ? O2 Co1 O3 6_4545 ? ? 92.26(19) 91.69(16) 92.62(14) ? O2 Co1 O3 6_4545 ? 5_6555 87.74(19) 87.35(16) 88.26(16) ? O3 Co1 O3 ? ? 5_6555 179.7(3) 179.5(2) 180.0(5) ? Co1 O1 C1 ? ? ? 121.1(3) 120.3(4) 122.0(4) ? Co1 O2 C1 2_6545 ? ? 119.9(3) 119.2(2) 120.6(2) ? Co1 O3 C2 ? ? ? 121.2(3) 119.9(3) 122.9(3) ? O1 C1 O2 ? ? ? 124.1(4) 123.2(4) 124.7(4) ? O3 C2 O3 ? ? 7_5555 123.8(4) 122.7(4) 124.7(4) ? data_IV _chemical_formula_sum 'C4 H9 Co1 N1 O6' _chemical_formula_weight 226 _chemical_absolute_configuration ? _space_group_crystal_system orthorhombic _space_group_ssg_name Pnma(00\g)0s0 loop_ _space_group_symop_ssg_id _space_group_symop_ssg_operation_algebraic 1 x1,x2,x3,x4 2 -x1+1/2,-x2,x3+1/2,x4+1/2 3 -x1,x2+1/2,-x3,-x4+1/2 4 x1+1/2,-x2+1/2,-x3+1/2,-x4 5 -x1,-x2,-x3,-x4 6 x1+1/2,x2,-x3+1/2,-x4+1/2 7 x1,-x2+1/2,x3,x4+1/2 8 -x1+1/2,x2+1/2,x3+1/2,x4 _cell_length_a 8.2548(3) _cell_length_b 11.6547(6) _cell_length_c 8.1521(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 784.29(6) _cell_modulation_dimension 1 loop_ _cell_wave_vector_seq_id _cell_wave_vector_x _cell_wave_vector_y _cell_wave_vector_z 1 0.000000 0.000000 0.124700 _cell_formula_units_Z 4 _cell_measurement_reflns_used 1024 _cell_measurement_theta_min 4.81 _cell_measurement_theta_max 61.7 _cell_measurement_temperature 86 _exptl_crystal_type_of_structure mod _exptl_crystal_density_diffrn 1.9144 _exptl_crystal_F_000 158.404 _exptl_absorpt_coefficient_mu 0.2417 _exptl_crystal_description prism _exptl_crystal_size_max 5 _exptl_crystal_size_mid 4 _exptl_crystal_size_min 4 _exptl_crystal_size_rad 4 _exptl_crystal_colour red _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'absorption corretion done through d19face, d19abs and d19abscan programs from ILL' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist ? ? ? ? _diffrn_ambient_temperature 86 _diffrn_source_power 55000 _diffrn_radiation_type neutron _diffrn_source 'neutron source' _diffrn_source_type 'ILL High Flux Reactor, beam H11' _diffrn_radiation_monochromator 'copper 331' _diffrn_measurement_device_type 'D19 position-sensitive detector diffractometer' _diffrn_measurement_method 'omega step-scans' _diffrn_detector_area_resol_mean 210 _diffrn_radiation_wavelength 1.4569 _diffrn_reflns_number 31762 _diffrn_reflns_theta_min 4.81 _diffrn_reflns_theta_max 61.7 _diffrn_reflns_theta_full 61.7 _diffrn_measured_fraction_theta_max 0.98 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_av_R_equivalents 0.1462 _diffrn_reflns_av_unetI/netI 0.014 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_index_m_1_min -3 _diffrn_reflns_limit_index_m_1_max 3 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_radiation_probe neutron _reflns_number_total 4920 _reflns_number_gt 2637 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.1099 _refine_ls_wR_factor_gt 0.1297 _refine_ls_R_factor_all 0.1469 _refine_ls_wR_factor_ref 0.1326 _refine_ls_goodness_of_fit_ref 5.59 _refine_ls_goodness_of_fit_gt 7.70 _refine_ls_number_reflns 4920 _refine_ls_number_parameters 333 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/(\s^2^(F)+0.0001F^2^) _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max 0.0034 _refine_ls_shift/su_mean 0.0005 _refine_ls_extinction_method none loop_ _atom_type_symbol _atom_type_scat_length_neutron _atom_type_scat_source C 6.646 International_Tables_Vol_C H -3.739 International_Tables_Vol_C Co 2.490 International_Tables_Vol_C N 9.360 International_Tables_Vol_C O 5.803 International_Tables_Vol_C loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.5 0 0 Uani 0.0274(13) 4 1 d ? ? ? O1 O 0.59576(16) -0.07098(12) -0.21405(15) Uani 0.0300(5) 8 1 d ? ? ? O2 O 0.77279(16) -0.06000(12) -0.41842(15) Uani 0.0294(4) 8 1 d ? ? ? O3 O 0.47473(17) 0.15470(12) -0.12798(15) Uani 0.0293(4) 8 1 d ? ? ? N1 N 0.91541(15) 0.25 -0.02973(16) Uani 0.0318(5) 4 1 d ? ? ? C1 C 0.71957(15) -0.02973(11) -0.27930(14) Uani 0.0296(4) 8 1 d ? ? ? C3 C 1.0869(2) 0.25 0.0245(2) Uani 0.0360(7) 4 1 d ? ? ? C2 C 0.4902(2) 0.25 -0.0567(2) Uani 0.0291(5) 4 1 d ? ? ? H1 H 0.7886(4) 0.0348(3) -0.2131(3) Uani 0.0539(10) 8 1 d ? ? ? H2 H 0.5181(6) 0.25 0.0760(5) Uani 0.0501(13) 4 1 d ? ? ? H1n H 0.9117(5) 0.25 -0.1552(5) Uani 0.0512(14) 4 1 d ? ? ? H3a H 1.0894(5) 0.25 0.1553(5) Uani 0.0631(17) 4 1 d ? ? ? H2n H 0.8548(4) 0.1787(3) 0.0127(3) Uani 0.0446(9) 8 1 d ? ? ? H3b H 1.1452(4) 0.3242(3) -0.0197(4) Uani 0.0626(11) 8 1 d ? ? ? loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co1 Co 0.031(2) 0.031(3) 0.020(2) -0.0008(17) -0.0016(15) 0.0007(15) O1 O 0.0271(8) 0.0350(9) 0.0280(7) -0.0043(5) 0.0033(5) -0.0023(5) O2 O 0.0291(8) 0.0340(8) 0.0252(7) -0.0015(5) 0.0024(5) -0.0010(5) O3 O 0.0335(8) 0.0283(8) 0.0262(7) -0.0010(5) -0.0012(5) -0.0020(5) N1 N 0.0316(8) 0.0348(9) 0.0291(8) 0 0.0010(5) 0 C1 C 0.0300(7) 0.0332(8) 0.0256(7) -0.0026(5) 0.0015(5) 0.0000(5) C3 C 0.0299(10) 0.0448(13) 0.0332(11) 0 -0.0002(7) 0 C2 C 0.0301(9) 0.0320(10) 0.0251(9) 0 -0.0018(6) 0 H1 H 0.0529(18) 0.0624(19) 0.0464(17) -0.0249(14) 0.0133(13) -0.0208(13) H2 H 0.074(3) 0.042(2) 0.035(2) 0 -0.0143(17) 0 H1n H 0.048(2) 0.065(3) 0.041(2) 0 0.0027(16) 0 H3a H 0.053(3) 0.095(4) 0.042(3) 0 -0.0003(17) 0 H2n H 0.0473(16) 0.0447(17) 0.0419(13) -0.0072(13) 0.0029(11) 0.0025(11) H3b H 0.0444(17) 0.066(2) 0.078(2) -0.0120(15) -0.0056(15) 0.0098(16) loop_ _atom_site_Fourier_wave_vector_seq_id _jana_atom_site_Fourier_wave_vector_q1_coeff 1 1 2 2 loop_ _atom_site_displace_Fourier_id _atom_site_displace_Fourier_atom_site_label _atom_site_displace_Fourier_axis _atom_site_displace_Fourier_wave_vector_seq_id Co1x1 Co1 x 1 Co1y1 Co1 y 1 Co1z1 Co1 z 1 O1x1 O1 x 1 O1y1 O1 y 1 O1z1 O1 z 1 O1x2 O1 x 2 O1y2 O1 y 2 O1z2 O1 z 2 O2x1 O2 x 1 O2y1 O2 y 1 O2z1 O2 z 1 O3x1 O3 x 1 O3y1 O3 y 1 O3z1 O3 z 1 O3x2 O3 x 2 O3y2 O3 y 2 O3z2 O3 z 2 N1x1 N1 x 1 N1y1 N1 y 1 N1z1 N1 z 1 N1x2 N1 x 2 N1y2 N1 y 2 N1z2 N1 z 2 C1x1 C1 x 1 C1y1 C1 y 1 C1z1 C1 z 1 C1x2 C1 x 2 C1y2 C1 y 2 C1z2 C1 z 2 C3x1 C3 x 1 C3y1 C3 y 1 C3z1 C3 z 1 C3x2 C3 x 2 C3y2 C3 y 2 C3z2 C3 z 2 C2x1 C2 x 1 C2y1 C2 y 1 C2z1 C2 z 1 H1x1 H1 x 1 H1y1 H1 y 1 H1z1 H1 z 1 H1x2 H1 x 2 H1y2 H1 y 2 H1z2 H1 z 2 H2x1 H2 x 1 H2y1 H2 y 1 H2z1 H2 z 1 H2x2 H2 x 2 H2y2 H2 y 2 H2z2 H2 z 2 H1nx1 H1n x 1 H1ny1 H1n y 1 H1nz1 H1n z 1 H1nx2 H1n x 2 H1ny2 H1n y 2 H1nz2 H1n z 2 H3ax1 H3a x 1 H3ay1 H3a y 1 H3az1 H3a z 1 H3ax2 H3a x 2 H3ay2 H3a y 2 H3az2 H3a z 2 H2nx1 H2n x 1 H2ny1 H2n y 1 H2nz1 H2n z 1 H2nx2 H2n x 2 H2ny2 H2n y 2 H2nz2 H2n z 2 H3bx1 H3b x 1 H3by1 H3b y 1 H3bz1 H3b z 1 H3bx2 H3b x 2 H3by2 H3b y 2 H3bz2 H3b z 2 loop_ _atom_site_displace_Fourier_param_id _atom_site_displace_Fourier_param_cos _atom_site_displace_Fourier_param_sin Co1x1 0 -0.0034(7) Co1y1 0 0.0322(5) Co1z1 0 0.0001(6) O1x1 -0.0033(2) -0.0025(2) O1y1 0.00449(16) 0.03227(17) O1z1 0.0002(2) 0.0006(2) O1x2 -0.0008(3) -0.0007(3) O1y2 0.00027(17) 0.00015(17) O1z2 -0.0004(3) -0.0005(3) O2x1 0.0006(2) -0.0027(2) O2y1 0.00136(16) 0.03259(16) O2z1 0.00313(20) -0.0005(2) O3x1 -0.0041(2) -0.0014(2) O3y1 0.00291(16) 0.03239(17) O3z1 -0.00019(19) 0.00049(19) O3x2 -0.0004(3) -0.0004(3) O3y2 0.00029(17) 0.00023(17) O3z2 -0.0003(3) -0.0008(3) N1x1 0 0 N1y1 0.00749(17) 0.03091(18) N1z1 0 0 N1x2 0.0004(3) -0.0006(3) N1y2 0 0 N1z2 0.0001(2) -0.0002(2) C1x1 -0.00004(18) -0.00201(18) C1y1 0.00140(14) 0.03202(15) C1z1 0.00207(17) 0.00073(18) C1x2 0.0002(3) 0.0001(3) C1y2 -0.00002(15) -0.00003(16) C1z2 0.0003(2) -0.0007(2) C3x1 0 0 C3y1 0.0015(3) 0.0311(3) C3z1 0 0 C3x2 0.0000(4) 0.0003(4) C3y2 0 0 C3z2 0.0000(4) 0.0009(4) C2x1 0 0 C2y1 0.0011(2) 0.0329(2) C2z1 0 0 H1x1 0.0025(4) -0.0027(4) H1y1 -0.0010(3) 0.0322(4) H1z1 0.0020(4) 0.0000(4) H1x2 0.0012(6) 0.0001(7) H1y2 -0.0001(4) -0.0001(4) H1z2 -0.0001(5) -0.0007(5) H2x1 0 0 H2y1 -0.0039(4) 0.0318(4) H2z1 0 0 H2x2 0.0009(9) 0.0005(9) H2y2 0 0 H2z2 -0.0003(7) -0.0015(7) H1nx1 0 0 H1ny1 0.0181(5) 0.0290(5) H1nz1 0 0 H1nx2 0.0008(9) 0.0020(9) H1ny2 0 0 H1nz2 -0.0007(8) -0.0009(8) H3ax1 0 0 H3ay1 -0.0102(6) 0.0303(6) H3az1 0 0 H3ax2 0.0000(10) -0.0010(10) H3ay2 0 0 H3az2 0.0001(8) -0.0003(8) H2nx1 -0.0002(4) -0.0013(4) H2ny1 0.0046(3) 0.0320(3) H2nz1 -0.0070(4) 0.0000(4) H2nx2 0.0010(6) 0.0000(6) H2ny2 -0.0007(3) -0.0001(3) H2nz2 -0.0012(5) 0.0007(5) H3bx1 0.0002(5) 0.0008(5) H3by1 0.0052(4) 0.0312(4) H3bz1 0.0094(5) -0.0016(5) H3bx2 -0.0002(7) 0.0002(7) H3by2 -0.0002(4) -0.0002(4) H3bz2 -0.0011(7) -0.0019(7) loop_ _atom_site_U_Fourier_id _atom_site_U_Fourier_atom_site_label _atom_site_U_Fourier_tens_elem _atom_site_U_Fourier_wave_vector_seq_id Co1U111 Co1 U11 1 Co1U221 Co1 U22 1 Co1U331 Co1 U33 1 Co1U121 Co1 U12 1 Co1U131 Co1 U13 1 Co1U231 Co1 U23 1 O1U111 O1 U11 1 O1U221 O1 U22 1 O1U331 O1 U33 1 O1U121 O1 U12 1 O1U131 O1 U13 1 O1U231 O1 U23 1 O2U111 O2 U11 1 O2U221 O2 U22 1 O2U331 O2 U33 1 O2U121 O2 U12 1 O2U131 O2 U13 1 O2U231 O2 U23 1 O3U111 O3 U11 1 O3U221 O3 U22 1 O3U331 O3 U33 1 O3U121 O3 U12 1 O3U131 O3 U13 1 O3U231 O3 U23 1 N1U111 N1 U11 1 N1U221 N1 U22 1 N1U331 N1 U33 1 N1U121 N1 U12 1 N1U131 N1 U13 1 N1U231 N1 U23 1 C1U111 C1 U11 1 C1U221 C1 U22 1 C1U331 C1 U33 1 C1U121 C1 U12 1 C1U131 C1 U13 1 C1U231 C1 U23 1 C3U111 C3 U11 1 C3U221 C3 U22 1 C3U331 C3 U33 1 C3U121 C3 U12 1 C3U131 C3 U13 1 C3U231 C3 U23 1 C2U111 C2 U11 1 C2U221 C2 U22 1 C2U331 C2 U33 1 C2U121 C2 U12 1 C2U131 C2 U13 1 C2U231 C2 U23 1 H1U111 H1 U11 1 H1U221 H1 U22 1 H1U331 H1 U33 1 H1U121 H1 U12 1 H1U131 H1 U13 1 H1U231 H1 U23 1 H2U111 H2 U11 1 H2U221 H2 U22 1 H2U331 H2 U33 1 H2U121 H2 U12 1 H2U131 H2 U13 1 H2U231 H2 U23 1 H1nU111 H1n U11 1 H1nU221 H1n U22 1 H1nU331 H1n U33 1 H1nU121 H1n U12 1 H1nU131 H1n U13 1 H1nU231 H1n U23 1 H3aU111 H3a U11 1 H3aU221 H3a U22 1 H3aU331 H3a U33 1 H3aU121 H3a U12 1 H3aU131 H3a U13 1 H3aU231 H3a U23 1 H2nU111 H2n U11 1 H2nU221 H2n U22 1 H2nU331 H2n U33 1 H2nU121 H2n U12 1 H2nU131 H2n U13 1 H2nU231 H2n U23 1 H3bU111 H3b U11 1 H3bU221 H3b U22 1 H3bU331 H3b U33 1 H3bU121 H3b U12 1 H3bU131 H3b U13 1 H3bU231 H3b U23 1 loop_ _atom_site_U_Fourier_param_id _atom_site_U_Fourier_param_cos _atom_site_U_Fourier_param_sin Co1U111 0.000(3) 0 Co1U221 -0.001(3) 0 Co1U331 0.003(3) 0 Co1U121 -0.006(2) 0 Co1U131 -0.002(2) 0 Co1U231 0.003(2) 0 O1U111 -0.0009(8) 0.0011(9) O1U221 0.0003(11) -0.0017(11) O1U331 0.0021(8) 0.0002(9) O1U121 -0.0006(8) 0.0013(8) O1U131 0.0006(7) -0.0003(7) O1U231 0.0026(7) -0.0013(7) O2U111 0.0005(9) -0.0005(9) O2U221 0.0004(11) 0.0010(11) O2U331 -0.0009(9) -0.0008(8) O2U121 -0.0020(8) -0.0001(8) O2U131 0.0019(7) 0.0005(7) O2U231 0.0030(7) 0.0001(7) O3U111 -0.0024(9) -0.0019(9) O3U221 -0.0004(11) 0.0003(11) O3U331 0.0019(8) -0.0002(8) O3U121 0.0002(8) 0.0010(8) O3U131 0.0007(7) -0.0029(7) O3U231 0.0023(7) -0.0009(8) N1U111 0 0 N1U221 0 0 N1U331 0 0 N1U121 -0.0017(9) -0.0011(9) N1U131 0 0 N1U231 0.0016(8) -0.0013(8) C1U111 0.0005(8) -0.0013(8) C1U221 -0.0005(9) -0.0013(10) C1U331 -0.0013(7) 0.0012(7) C1U121 -0.0006(7) -0.0007(7) C1U131 0.0002(6) 0.0004(7) C1U231 0.0041(7) 0.0000(7) C3U111 0 0 C3U221 0 0 C3U331 0 0 C3U121 0.0006(13) 0.0023(13) C3U131 0 0 C3U231 0.0039(11) 0.0000(11) C2U111 0 0 C2U221 0 0 C2U331 0 0 C2U121 0.0007(9) 0.0030(9) C2U131 0 0 C2U231 0.0038(9) 0.0036(10) H1U111 -0.0004(19) 0.000(2) H1U221 0.002(2) 0.004(3) H1U331 -0.0038(19) -0.0021(19) H1U121 0.0008(19) 0.0024(19) H1U131 -0.0040(16) -0.0019(17) H1U231 0.0030(17) -0.0020(17) H2U111 0 0 H2U221 0 0 H2U331 0 0 H2U121 -0.005(2) -0.003(2) H2U131 0 0 H2U231 0.0013(19) -0.003(2) H1nU111 0 0 H1nU221 0 0 H1nU331 0 0 H1nU121 0.006(2) 0.002(3) H1nU131 0 0 H1nU231 -0.003(2) 0.002(2) H3aU111 0 0 H3aU221 0 0 H3aU331 0 0 H3aU121 0.003(3) -0.001(3) H3aU131 0 0 H3aU231 0.011(3) 0.003(3) H2nU111 0.0044(19) 0.0018(19) H2nU221 0.001(2) -0.002(2) H2nU331 -0.0012(17) -0.0001(17) H2nU121 -0.0010(18) 0.0001(18) H2nU131 -0.0010(14) -0.0037(14) H2nU231 0.0053(15) -0.0010(15) H3bU111 -0.001(2) -0.004(2) H3bU221 -0.006(3) 0.006(3) H3bU331 0.005(3) 0.002(3) H3bU121 0.000(2) -0.003(2) H3bU131 -0.0012(18) 0.0026(19) H3bU231 0.000(2) 0.000(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_ssg_symmetry_1 _geom_bond_site_ssg_symmetry_2 _geom_bond_distance_av _geom_bond_distance_min _geom_bond_distance_max _geom_bond_publ_flag Co1 O1 ? ? 2.086(5) 2.081(6) 2.093(6) ? Co1 O1 ? 5_6555 2.086(5) 2.081(6) 2.093(6) ? Co1 O2 ? 2_6555 2.110(4) 2.099(5) 2.121(5) ? Co1 O2 ? 6_4545 2.110(4) 2.099(5) 2.121(5) ? Co1 O3 ? ? 2.094(5) 2.087(7) 2.102(7) ? Co1 O3 ? 5_6555 2.094(5) 2.087(7) 2.102(7) ? O1 C1 ? ? 1.249(6) 1.240(6) 1.259(6) ? O2 C1 ? ? 1.268(4) 1.255(4) 1.276(4) ? O3 C2 ? ? 1.261(5) 1.255(5) 1.267(5) ? N1 C3 ? ? 1.484(5) 1.474(5) 1.492(5) ? C3 H3b ? ? 1.055(11) 1.042(11) 1.065(11) ? C3 H3b ? 7_5555 1.055(11) 1.042(11) 1.065(11) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_ssg_symmetry_1 _geom_angle_site_ssg_symmetry_2 _geom_angle_site_ssg_symmetry_3 _geom_angle_av _geom_angle_min _geom_angle_max _geom_angle_publ_flag O1 Co1 O1 ? ? 5_6555 179.7(3) 179.4(2) 180.0(5) ? O1 Co1 O2 ? ? 2_6555 93.40(18) 92.74(15) 93.92(13) ? O1 Co1 O2 ? ? 6_4545 86.60(17) 86.08(13) 87.33(15) ? O1 Co1 O3 ? ? ? 87.88(19) 87.28(17) 88.45(17) ? O1 Co1 O3 ? ? 5_6555 92.1(2) 91.72(18) 92.68(16) ? O1 Co1 O2 5_6555 ? 2_6555 86.60(17) 86.08(13) 87.33(15) ? O1 Co1 O2 5_6555 ? 6_4545 93.40(18) 92.74(15) 93.92(13) ? O1 Co1 O3 5_6555 ? ? 92.1(2) 91.72(18) 92.68(16) ? O1 Co1 O3 5_6555 ? 5_6555 87.88(19) 87.28(17) 88.45(17) ? O2 Co1 O2 2_6555 ? 6_4545 179.9(3) 179.9(3) 180.0(5) ? O2 Co1 O3 2_6555 ? ? 87.69(18) 87.3(2) 88.39(16) ? O2 Co1 O3 2_6555 ? 5_6555 92.31(18) 91.58(15) 92.8(2) ? O2 Co1 O3 6_4545 ? ? 92.31(18) 91.58(15) 92.8(2) ? O2 Co1 O3 6_4545 ? 5_6555 87.69(18) 87.3(2) 88.39(16) ? O3 Co1 O3 ? ? 5_6555 179.6(3) 179.2(3) 180.0(5) ? Co1 O1 C1 ? ? ? 120.9(3) 120.2(3) 121.5(4) ? Co1 O2 C1 2_6545 ? ? 119.9(2) 119.4(2) 120.3(2) ? Co1 O3 C2 ? ? ? 121.2(3) 120.4(3) 122.4(3) ? O1 C1 O2 ? ? ? 123.9(4) 123.6(4) 124.3(4) ? N1 C3 H3b ? ? ? 109.4(6) 108.4(6) 110.3(6) ? N1 C3 H3b ? ? 7_5555 109.4(6) 108.4(6) 110.3(6) ? H3b C3 H3b ? ? 7_5555 110.5(9) 109.1(9) 111.7(9) ? O3 C2 O3 ? ? 7_5555 123.6(3) 122.9(3) 124.3(3) ?