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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_I _audit_update_record '2014-06-10 # Formatted by IUCr publCIF' _audit_creation_method 'Jana2006 Version : 14/01/2014' _journal_date_recd_electronic 2014-01-29 _journal_date_from_coeditor 2014-04-07 _journal_date_accepted 2014-04-07 _journal_date_printers_first 2014-04-25 _journal_date_proofs_out 2014-06-11 _journal_date_proofs_in 2014-06-20 _journal_coeditor_code DK5025 _journal_paper_doi https://doi.org/10.1107/S2052520614007707 _journal_techeditor_code B140770 _iucr_compatibility_tag ACTA95 _journal_paper_category FA _journal_coden_ASTM ASBSDK _journal_name_full 'Acta Crystallographica, Section B' _journal_year 2014 _journal_volume 70 _journal_issue 04 _journal_page_first 652 _journal_page_last 659 _publ_requested_journal 'Acta Crystallographica Section B' _publ_section_title ;N-H...O and C-H...F hydrogen bonds in the incommensurately modulated crystal structure of adamantan-1-ammonium 4-fluorobenzoate ; _publ_contact_author_name 'Schonleber, Andreas' _publ_contact_author_address ;Laboratory of Crystallography University of Bayreuth 95440 Bayreuth Germany ; _publ_contact_author_email andreas.schoenleber@uni-bayreuth.de loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Schonleber, Andreas' '? # footnote' ;Laboratory of Crystallography University of Bayreuth 95440 Bayreuth Germany ; 'van Smaalen, Sander' '? # footnote' ;Laboratory of Crystallography University of Bayreuth 95440 Bayreuth Germany ; 'Weiss, Hans-Christoph' '? # footnote' ;Currenta GmbH & Co OHG 51368 Leverkeusen Germany ; 'Kesel, Andreas J.' '? # footnote' ;Chammunsterstr. 47 81827 Munchen Germany ; _database_code_depnum_ccdc_archive 'CCDC 995840' _chemical_formula_sum 'C17 H22 F1 N1 O2' _chemical_formula_weight 291.4 _chemical_absolute_configuration ? _space_group_crystal_system monoclinic _space_group_ssg_name P21/n(\a0\g)00 loop_ _space_group_symop_ssg_id _space_group_symop_ssg_operation_algebraic 1 x1,x2,x3,x4 2 -x1+1/2,x2+1/2,-x3+1/2,-x4 3 -x1,-x2,-x3,-x4 4 x1+1/2,-x2+1/2,x3+1/2,x4 _cell_length_a 10.84980(10) _cell_length_b 6.52470(10) _cell_length_c 21.3826(3) _cell_angle_alpha 90 _cell_angle_beta 98.2460(10) _cell_angle_gamma 90 _cell_volume 1498.06(3) _cell_modulation_dimension 1 loop_ _cell_wave_vector_seq_id _cell_wave_vector_x _cell_wave_vector_y _cell_wave_vector_z 1 0.423700 0.000000 0.428400 _cell_formula_units_Z 4 _cell_measurement_temperature 97.0(1) _exptl_crystal_type_of_structure mod _exptl_crystal_density_diffrn 1.2914 _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 0.753 _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.015 _exptl_absorpt_correction_type empirical _diffrn_ambient_temperature 293 _diffrn_radiation_type 'Cu K\a' _diffrn_source 'X-ray tube' _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-cycle diffractometer' _diffrn_measurement_device_type 'Oxford Diffraction CCD' _diffrn_reflns_number 29463 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 65.68 _diffrn_reflns_theta_full 33.24 _diffrn_measured_fraction_theta_max 0.87 _diffrn_measured_fraction_theta_full 0.96 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_unetI/netI 0.0304 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 3 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _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 x-ray _reflns_number_total 11225 _reflns_number_gt 6001 _reflns_threshold_expression I>3\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_gt 0.0618 _refine_ls_R_factor_all 0.0953 _refine_ls_wR_factor_ref 0.0713 _refine_ls_goodness_of_fit_ref 1.76 _refine_ls_goodness_of_fit_gt 2.17 _refine_ls_number_reflns 11225 _refine_ls_number_parameters 991 _refine_ls_number_restraints 6 _refine_ls_number_constraints 307 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/(\s^2^(F)+0.000121F^2^) _refine_ls_hydrogen_treatment mixed _refine_ls_shift/su_max 0.0026 _refine_ls_shift/su_mean 0.0001 _refine_diff_density_max 0.26 _refine_diff_density_min -0.27 _refine_ls_extinction_method none loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0181 0.0091 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' F 0.0727 0.0534 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' N 0.0311 0.0180 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0492 0.0322 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' loop_ _restr_distance_atom_site_label_1 _restr_distance_atom_site_label_2 _restr_distance_target _restr_distance_target_weight_param N11 H11a 0.87 0.05 N11 H11b 0.87 0.05 N11 H11c 0.87 0.05 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 C01 C -0.06259(9) 0.38058(15) -0.15316(6) Uani 0.0306(3) 4 1 d ? ? ? C02 C 0.02518(9) 0.29051(15) -0.09876(5) Uani 0.0310(3) 4 1 d ? ? ? C03 C 0.09126(11) 0.41989(16) -0.05531(6) Uani 0.0390(4) 4 1 d ? ? ? C04 C 0.17229(11) 0.34689(17) -0.00443(6) Uani 0.0428(4) 4 1 d ? ? ? C05 C 0.18623(11) 0.14257(17) 0.00211(6) Uani 0.0420(4) 4 1 d ? ? ? C06 C 0.12363(16) 0.00717(19) -0.03990(8) Uani 0.0523(5) 4 1 d ? ? ? C07 C 0.04147(13) 0.08249(17) -0.09034(6) Uani 0.0423(4) 4 1 d ? ? ? F08 F 0.26562(8) 0.06883(11) 0.05162(4) Uani 0.0608(3) 4 1 d ? ? ? O09 O -0.12359(7) 0.26017(11) -0.19206(4) Uani 0.0375(3) 4 1 d ? ? ? O10 O -0.06978(8) 0.57222(12) -0.15579(4) Uani 0.0418(3) 4 1 d ? ? ? N11 N 0.14166(8) 0.13244(13) 0.24462(4) Uani 0.0317(3) 4 1 d ? ? ? C12 C 0.05548(9) 0.13331(13) 0.29297(5) Uani 0.0285(3) 4 1 d ? ? ? C13 C 0.09251(10) -0.03906(13) 0.34078(5) Uani 0.0331(3) 4 1 d ? ? ? C14 C 0.00475(11) -0.03839(14) 0.39012(6) Uani 0.0372(4) 4 1 d ? ? ? C15 C 0.01334(10) 0.16851(14) 0.42492(6) Uani 0.0355(3) 4 1 d ? ? ? C16 C -0.02291(9) 0.34135(13) 0.37675(5) Uani 0.0322(3) 4 1 d ? ? ? C17 C 0.06498(9) 0.34024(13) 0.32721(5) Uani 0.0307(3) 4 1 d ? ? ? C18 C -0.07819(9) 0.09895(13) 0.26048(5) Uani 0.0307(3) 4 1 d ? ? ? C19 C -0.16604(9) 0.10039(14) 0.30998(6) Uani 0.0349(3) 4 1 d ? ? ? C20 C -0.15685(10) 0.30724(14) 0.34471(6) Uani 0.0351(3) 4 1 d ? ? ? C21 C -0.12916(11) -0.07209(14) 0.35808(6) Uani 0.0385(4) 4 1 d ? ? ? H03 H 0.080475 0.563804 -0.060677 Uiso 0.0468 4 1 d ? ? ? H04 H 0.217471 0.43786 0.025433 Uiso 0.0514 4 1 d ? ? ? H06 H 0.136534 -0.136056 -0.034428 Uiso 0.0627 4 1 d ? ? ? H07 H -0.004502 -0.009952 -0.119586 Uiso 0.0507 4 1 d ? ? ? H11a H 0.2175(10) 0.1501(13) 0.2626(6) Uiso 0.0476 4 1 d ? ? ? H11b H 0.1354(10) 0.0108(15) 0.2242(5) Uiso 0.0476 4 1 d ? ? ? H11c H 0.1202(11) 0.2339(14) 0.2166(5) Uiso 0.0476 4 1 d ? ? ? H13a H 0.08697 -0.168485 0.319235 Uiso 0.0398 4 1 d ? ? ? H13b H 0.176266 -0.017357 0.361068 Uiso 0.0398 4 1 d ? ? ? H14 H 0.028077 -0.146646 0.419828 Uiso 0.0446 4 1 d ? ? ? H15a H -0.042676 0.168648 0.455798 Uiso 0.0425 4 1 d ? ? ? H15b H 0.097066 0.18964 0.445341 Uiso 0.0425 4 1 d ? ? ? H16 H -0.016901 0.471243 0.398035 Uiso 0.0387 4 1 d ? ? ? H17a H 0.148861 0.360879 0.347481 Uiso 0.0368 4 1 d ? ? ? H17b H 0.042131 0.44794 0.297245 Uiso 0.0368 4 1 d ? ? ? H18a H -0.101038 0.206473 0.23045 Uiso 0.0369 4 1 d ? ? ? H18b H -0.083604 -0.030917 0.239188 Uiso 0.0369 4 1 d ? ? ? H19 H -0.249823 0.079757 0.289558 Uiso 0.0419 4 1 d ? ? ? H20a H -0.180233 0.415363 0.314982 Uiso 0.0421 4 1 d ? ? ? H20b H -0.211836 0.307131 0.37607 Uiso 0.0421 4 1 d ? ? ? H21a H -0.184235 -0.07108 0.389397 Uiso 0.0462 4 1 d ? ? ? H21b H -0.135038 -0.201758 0.336676 Uiso 0.0462 4 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 C01 C 0.0232(5) 0.0433(6) 0.0247(7) 0.0005(3) 0.0019(4) 0.0020(4) C02 C 0.0230(5) 0.0467(6) 0.0234(7) -0.0027(4) 0.0032(4) 0.0014(4) C03 C 0.0354(6) 0.0436(6) 0.0348(8) 0.0074(4) -0.0057(5) -0.0057(4) C04 C 0.0354(6) 0.0522(6) 0.0364(8) 0.0020(4) -0.0101(5) -0.0082(5) C05 C 0.0367(6) 0.0543(6) 0.0314(8) -0.0051(5) -0.0080(5) 0.0120(5) C06 C 0.0618(11) 0.0448(6) 0.0443(9) -0.0158(7) -0.0125(8) 0.0165(6) C07 C 0.0453(8) 0.0439(6) 0.0338(8) -0.0171(6) -0.0077(6) 0.0076(5) F08 F 0.0613(5) 0.0646(4) 0.0465(5) -0.0057(3) -0.0260(4) 0.0175(3) O09 O 0.0274(4) 0.0536(4) 0.0284(5) 0.0009(3) -0.0064(3) -0.0047(3) O10 O 0.0420(4) 0.0496(5) 0.0302(5) 0.0002(3) -0.0074(3) 0.0048(3) N11 N 0.0233(4) 0.0460(5) 0.0238(5) 0.0006(3) -0.0038(3) 0.0024(4) C12 C 0.0251(5) 0.0360(5) 0.0229(6) 0.0030(3) -0.0012(4) 0.0020(4) C13 C 0.0328(5) 0.0378(5) 0.0274(7) 0.0083(4) -0.0009(4) 0.0020(4) C14 C 0.0441(6) 0.0351(5) 0.0318(7) 0.0075(4) 0.0039(5) 0.0087(4) C15 C 0.0372(6) 0.0447(5) 0.0241(6) 0.0063(4) 0.0029(4) 0.0021(4) C16 C 0.0344(5) 0.0337(4) 0.0273(6) 0.0039(3) -0.0002(4) -0.0014(4) C17 C 0.0275(5) 0.0348(5) 0.0273(6) 0.0003(3) -0.0040(4) 0.0023(4) C18 C 0.0252(5) 0.0369(5) 0.0280(6) 0.0010(3) -0.0031(4) 0.0003(4) C19 C 0.0243(5) 0.0434(5) 0.0357(7) -0.0003(3) -0.0002(4) -0.0016(4) C20 C 0.0303(5) 0.0381(5) 0.0363(7) 0.0064(3) 0.0023(4) 0.0011(4) C21 C 0.0412(6) 0.0353(5) 0.0408(8) -0.0026(4) 0.0119(5) 0.0013(4) 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 C01x1 C01 x 1 C01y1 C01 y 1 C01z1 C01 z 1 C01x2 C01 x 2 C01y2 C01 y 2 C01z2 C01 z 2 C02x1 C02 x 1 C02y1 C02 y 1 C02z1 C02 z 1 C02x2 C02 x 2 C02y2 C02 y 2 C02z2 C02 z 2 C03x1 C03 x 1 C03y1 C03 y 1 C03z1 C03 z 1 C03x2 C03 x 2 C03y2 C03 y 2 C03z2 C03 z 2 C04x1 C04 x 1 C04y1 C04 y 1 C04z1 C04 z 1 C04x2 C04 x 2 C04y2 C04 y 2 C04z2 C04 z 2 C05x1 C05 x 1 C05y1 C05 y 1 C05z1 C05 z 1 C05x2 C05 x 2 C05y2 C05 y 2 C05z2 C05 z 2 C06x1 C06 x 1 C06y1 C06 y 1 C06z1 C06 z 1 C06x2 C06 x 2 C06y2 C06 y 2 C06z2 C06 z 2 C07x1 C07 x 1 C07y1 C07 y 1 C07z1 C07 z 1 C07x2 C07 x 2 C07y2 C07 y 2 C07z2 C07 z 2 F08x1 F08 x 1 F08y1 F08 y 1 F08z1 F08 z 1 F08x2 F08 x 2 F08y2 F08 y 2 F08z2 F08 z 2 O09x1 O09 x 1 O09y1 O09 y 1 O09z1 O09 z 1 O09x2 O09 x 2 O09y2 O09 y 2 O09z2 O09 z 2 O10x1 O10 x 1 O10y1 O10 y 1 O10z1 O10 z 1 O10x2 O10 x 2 O10y2 O10 y 2 O10z2 O10 z 2 N11x1 N11 x 1 N11y1 N11 y 1 N11z1 N11 z 1 N11x2 N11 x 2 N11y2 N11 y 2 N11z2 N11 z 2 C12x1 C12 x 1 C12y1 C12 y 1 C12z1 C12 z 1 C12x2 C12 x 2 C12y2 C12 y 2 C12z2 C12 z 2 C13x1 C13 x 1 C13y1 C13 y 1 C13z1 C13 z 1 C13x2 C13 x 2 C13y2 C13 y 2 C13z2 C13 z 2 C14x1 C14 x 1 C14y1 C14 y 1 C14z1 C14 z 1 C14x2 C14 x 2 C14y2 C14 y 2 C14z2 C14 z 2 C15x1 C15 x 1 C15y1 C15 y 1 C15z1 C15 z 1 C15x2 C15 x 2 C15y2 C15 y 2 C15z2 C15 z 2 C16x1 C16 x 1 C16y1 C16 y 1 C16z1 C16 z 1 C16x2 C16 x 2 C16y2 C16 y 2 C16z2 C16 z 2 C17x1 C17 x 1 C17y1 C17 y 1 C17z1 C17 z 1 C17x2 C17 x 2 C17y2 C17 y 2 C17z2 C17 z 2 C18x1 C18 x 1 C18y1 C18 y 1 C18z1 C18 z 1 C18x2 C18 x 2 C18y2 C18 y 2 C18z2 C18 z 2 C19x1 C19 x 1 C19y1 C19 y 1 C19z1 C19 z 1 C19x2 C19 x 2 C19y2 C19 y 2 C19z2 C19 z 2 C20x1 C20 x 1 C20y1 C20 y 1 C20z1 C20 z 1 C20x2 C20 x 2 C20y2 C20 y 2 C20z2 C20 z 2 C21x1 C21 x 1 C21y1 C21 y 1 C21z1 C21 z 1 C21x2 C21 x 2 C21y2 C21 y 2 C21z2 C21 z 2 H03x1 H03 x 1 H03y1 H03 y 1 H03z1 H03 z 1 H03x2 H03 x 2 H03y2 H03 y 2 H03z2 H03 z 2 H04x1 H04 x 1 H04y1 H04 y 1 H04z1 H04 z 1 H04x2 H04 x 2 H04y2 H04 y 2 H04z2 H04 z 2 H06x1 H06 x 1 H06y1 H06 y 1 H06z1 H06 z 1 H06x2 H06 x 2 H06y2 H06 y 2 H06z2 H06 z 2 H07x1 H07 x 1 H07y1 H07 y 1 H07z1 H07 z 1 H07x2 H07 x 2 H07y2 H07 y 2 H07z2 H07 z 2 H11ax1 H11a x 1 H11ay1 H11a y 1 H11az1 H11a z 1 H11ax2 H11a x 2 H11ay2 H11a y 2 H11az2 H11a z 2 H11bx1 H11b x 1 H11by1 H11b y 1 H11bz1 H11b z 1 H11bx2 H11b x 2 H11by2 H11b y 2 H11bz2 H11b z 2 H11cx1 H11c x 1 H11cy1 H11c y 1 H11cz1 H11c z 1 H11cx2 H11c x 2 H11cy2 H11c y 2 H11cz2 H11c z 2 H13ax1 H13a x 1 H13ay1 H13a y 1 H13az1 H13a z 1 H13ax2 H13a x 2 H13ay2 H13a y 2 H13az2 H13a z 2 H13bx1 H13b x 1 H13by1 H13b y 1 H13bz1 H13b z 1 H13bx2 H13b x 2 H13by2 H13b y 2 H13bz2 H13b z 2 H14x1 H14 x 1 H14y1 H14 y 1 H14z1 H14 z 1 H14x2 H14 x 2 H14y2 H14 y 2 H14z2 H14 z 2 H15ax1 H15a x 1 H15ay1 H15a y 1 H15az1 H15a z 1 H15ax2 H15a x 2 H15ay2 H15a y 2 H15az2 H15a z 2 H15bx1 H15b x 1 H15by1 H15b y 1 H15bz1 H15b z 1 H15bx2 H15b x 2 H15by2 H15b y 2 H15bz2 H15b z 2 H16x1 H16 x 1 H16y1 H16 y 1 H16z1 H16 z 1 H16x2 H16 x 2 H16y2 H16 y 2 H16z2 H16 z 2 H17ax1 H17a x 1 H17ay1 H17a y 1 H17az1 H17a z 1 H17ax2 H17a x 2 H17ay2 H17a y 2 H17az2 H17a z 2 H17bx1 H17b x 1 H17by1 H17b y 1 H17bz1 H17b z 1 H17bx2 H17b x 2 H17by2 H17b y 2 H17bz2 H17b z 2 H18ax1 H18a x 1 H18ay1 H18a y 1 H18az1 H18a z 1 H18ax2 H18a x 2 H18ay2 H18a y 2 H18az2 H18a z 2 H18bx1 H18b x 1 H18by1 H18b y 1 H18bz1 H18b z 1 H18bx2 H18b x 2 H18by2 H18b y 2 H18bz2 H18b z 2 H19x1 H19 x 1 H19y1 H19 y 1 H19z1 H19 z 1 H19x2 H19 x 2 H19y2 H19 y 2 H19z2 H19 z 2 H20ax1 H20a x 1 H20ay1 H20a y 1 H20az1 H20a z 1 H20ax2 H20a x 2 H20ay2 H20a y 2 H20az2 H20a z 2 H20bx1 H20b x 1 H20by1 H20b y 1 H20bz1 H20b z 1 H20bx2 H20b x 2 H20by2 H20b y 2 H20bz2 H20b z 2 H21ax1 H21a x 1 H21ay1 H21a y 1 H21az1 H21a z 1 H21ax2 H21a x 2 H21ay2 H21a y 2 H21az2 H21a z 2 H21bx1 H21b x 1 H21by1 H21b y 1 H21bz1 H21b z 1 H21bx2 H21b x 2 H21by2 H21b y 2 H21bz2 H21b z 2 loop_ _atom_site_displace_Fourier_param_id _atom_site_displace_Fourier_param_cos _atom_site_displace_Fourier_param_sin C01x1 -0.00102(14) -0.00335(14) C01y1 0.0353(2) 0.0286(2) C01z1 0.00111(8) -0.00031(8) C01x2 0.0005(2) 0.0002(2) C01y2 -0.0001(3) 0.0097(3) C01z2 -0.00050(11) -0.00009(11) C02x1 0.00045(14) -0.00532(13) C02y1 0.0206(2) 0.03567(19) C02z1 0.00092(8) 0.00043(8) C02x2 0.0000(2) -0.00143(19) C02y2 -0.0045(3) 0.0048(3) C02z2 -0.00054(11) -0.00042(11) C03x1 0.00231(17) 0.00957(14) C03y1 0.0092(2) 0.03819(19) C03z1 0.00071(10) -0.00418(8) C03x2 -0.0026(2) 0.0015(2) C03y2 -0.0051(3) 0.0018(3) C03z2 0.00080(12) -0.00053(12) C04x1 0.00080(17) 0.00614(16) C04y1 -0.0040(2) 0.0369(2) C04z1 0.00144(9) -0.00274(8) C04x2 -0.0023(2) -0.0006(2) C04y2 -0.0029(3) -0.0007(3) C04z2 0.00122(12) -0.00031(12) C05x1 0.00842(18) -0.01138(16) C05y1 -0.0059(3) 0.0364(2) C05z1 -0.00116(9) 0.00298(9) C05x2 0.0007(2) -0.0010(2) C05y2 -0.0026(3) -0.0005(3) C05z2 0.00026(13) 0.00086(12) C06x1 0.0059(2) -0.02798(17) C06y1 0.0055(3) 0.0383(2) C06z1 -0.00042(11) 0.00799(9) C06x2 0.0047(3) -0.0041(3) C06y2 -0.0069(3) 0.0013(3) C06z2 -0.00105(14) 0.00070(14) C07x1 -0.0039(2) -0.02240(16) C07y1 0.0195(3) 0.0376(2) C07z1 0.00228(9) 0.00603(8) C07x2 0.0016(2) -0.0049(2) C07y2 -0.0054(3) 0.0056(3) C07z2 -0.00044(12) 0.00076(12) F08x1 0.01589(12) -0.01124(12) F08y1 -0.01589(15) 0.03007(15) F08z1 -0.00343(6) 0.00356(6) F08x2 0.00172(17) 0.00051(17) F08y2 -0.00163(19) -0.00103(19) F08z2 -0.00041(8) 0.00031(8) O09x1 -0.00204(10) -0.00198(10) O09y1 0.04161(14) 0.01936(16) O09z1 0.00082(6) -0.00108(6) O09x2 -0.00072(15) -0.00042(15) O09y2 0.0042(2) 0.0067(2) O09z2 -0.00069(8) -0.00035(8) O10x1 0.00012(11) -0.00234(12) O10y1 0.03513(15) 0.02750(16) O10z1 0.00121(6) 0.00020(6) O10x2 0.00018(16) 0.00081(17) O10y2 0.0005(2) 0.0080(2) O10z2 -0.00060(8) 0.00006(8) N11x1 -0.00136(11) -0.00082(12) N11y1 -0.04428(17) 0.0109(2) N11z1 -0.00119(6) -0.00065(7) N11x2 0.00088(16) 0.00008(17) N11y2 -0.0048(2) 0.0041(3) N11z2 0.00023(9) 0.00014(9) C12x1 -0.00266(13) 0.00076(13) C12y1 -0.03732(17) 0.00767(20) C12z1 -0.00186(7) 0.00046(8) C12x2 0.00045(15) 0.00001(14) C12y2 -0.0024(2) 0.0038(2) C12z2 0.00045(9) 0.00030(9) C13x1 -0.00844(14) 0.00337(15) C13y1 -0.03795(17) -0.0029(2) C13z1 -0.00129(7) -0.00116(8) C13x2 0.00002(15) 0.00033(15) C13y2 -0.0024(2) 0.0023(2) C13z2 0.00048(8) 0.00037(9) C14x1 -0.01028(15) 0.00552(16) C14y1 -0.03040(18) -0.0063(2) C14z1 -0.00219(8) -0.00033(8) C14x2 -0.00041(17) 0.00050(17) C14y2 -0.0003(2) 0.0016(2) C14z2 0.00031(9) 0.00020(9) C15x1 -0.00838(14) 0.00336(16) C15y1 -0.02819(19) -0.0120(2) C15z1 -0.00312(8) 0.00072(8) C15x2 0.00024(17) 0.00009(16) C15y2 0.0006(2) 0.0017(2) C15z2 0.00046(10) 0.00044(9) C16x1 -0.00254(14) 0.00095(14) C16y1 -0.03055(18) -0.0028(2) C16z1 -0.00380(7) 0.00258(8) C16x2 0.00024(16) -0.00037(16) C16y2 0.0001(2) 0.0017(2) C16z2 0.00001(9) 0.00024(8) C17x1 -0.00066(13) -0.00083(13) C17y1 -0.03771(17) 0.0012(2) C17z1 -0.00282(7) 0.00128(7) C17x2 0.00022(14) -0.00037(14) C17y2 -0.0017(2) 0.0026(2) C17z2 0.00004(8) 0.00014(8) C18x1 -0.00198(13) 0.00164(13) C18y1 -0.02772(19) 0.01771(19) C18z1 -0.00246(8) 0.00261(8) C18x2 0.00020(16) 0.00010(16) C18y2 0.0013(2) 0.0031(2) C18z2 0.00022(9) -0.00004(9) C19x1 -0.00254(13) 0.00454(14) C19y1 -0.02400(19) 0.01076(19) C19z1 -0.00227(8) 0.00413(8) C19x2 0.00010(16) 0.00007(16) C19y2 0.0009(2) 0.0015(2) C19z2 0.00011(9) 0.00023(9) C20x1 -0.00165(14) 0.00164(14) C20y1 -0.02610(19) 0.00448(19) C20z1 -0.00301(8) 0.00543(8) C20x2 0.00033(17) -0.00109(17) C20y2 0.0012(2) 0.0003(2) C20z2 0.00044(10) -0.00021(10) C21x1 -0.00658(16) 0.00933(16) C21y1 -0.02681(19) 0.0020(2) C21z1 -0.00283(8) 0.00199(9) C21x2 0.0000(2) 0.0007(2) C21y2 0.0000(2) 0.0013(2) C21z2 0.00034(9) 0.00007(9) H03x1 0.003 0.0225 H03y1 0.0106 0.0381 H03z1 0.0005 -0.0085 H03x2 -0.0053 0.0032 H03y2 -0.0039 0.0024 H03z2 0.0014 -0.0008 H04x1 -0.0058 0.0152 H04y1 -0.0115 0.0343 H04z1 0.0038 -0.0054 H04x2 -0.0041 -0.0014 H04y2 -0.0014 0.0006 H04z2 0.0019 -0.0002 H06x1 0.0095 -0.0414 H06y1 0.0044 0.0377 H06z1 -0.0016 0.0123 H06x2 0.0091 -0.0056 H06y2 -0.0079 -0.0001 H06z2 -0.0021 0.0012 H07x1 -0.0129 -0.0285 H07y1 0.0276 0.0345 H07z1 0.0049 0.0078 H07x2 0.0001 -0.0071 H07y2 -0.0038 0.0083 H07z2 -0.0001 0.0015 H11ax1 -0.0014(14) -0.0024(14) H11ay1 -0.0460(19) 0.002(2) H11az1 0.0005(8) -0.0006(8) H11ax2 0.0010(16) 0.0003(16) H11ay2 -0.007(2) 0.004(3) H11az2 0.0009(11) 0.0000(10) H11bx1 0.0006(14) 0.0013(15) H11by1 -0.043(2) 0.016(2) H11bz1 -0.0025(7) -0.0004(7) H11bx2 0.003(2) 0.000(2) H11by2 -0.002(2) 0.004(2) H11bz2 -0.0024(9) 0.0022(9) H11cx1 0.0000(15) -0.0020(15) H11cy1 -0.042(2) 0.015(2) H11cz1 -0.0003(7) -0.0001(7) H11cx2 -0.002(2) -0.001(2) H11cy2 0.002(2) 0.000(2) H11cz2 0.0017(9) -0.0015(9) H13ax1 -0.0104 0.005 H13ay1 -0.0386 0.0012 H13az1 -0.0011 -0.0018 H13ax2 0.0001 0.0006 H13ay2 -0.0024 0.0027 H13az2 0.0008 0.0002 H13bx1 -0.0091 0.001 H13by1 -0.0405 -0.0127 H13bz1 -0.0002 -0.0016 H13bx2 -0.0003 0.0002 H13by2 -0.0029 0.001 H13bz2 0.0003 0.0006 H14x1 -0.0142 0.0055 H14y1 -0.0283 -0.0119 H14z1 -0.0014 -0.0013 H14x2 -0.0012 0.0005 H14y2 -0.0004 0.0013 H14z2 0.0004 0.0003 H15ax1 -0.0099 0.0049 H15ay1 -0.0239 -0.0143 H15az1 -0.0039 0.0014 H15ax2 0 -0.0001 H15ay2 0.0017 0.0011 H15az2 0.0004 0.0003 H15bx1 -0.0093 0.0011 H15by1 -0.0276 -0.0192 H15bz1 -0.0022 -0.0004 H15bx2 0.0003 0.0003 H15by2 -0.0007 0.0019 H15bz2 0 0.0004 H16x1 -0.001 -0.0003 H16y1 -0.0295 -0.0062 H16z1 -0.0044 0.003 H16x2 0.0005 -0.0005 H16y2 0.0004 0.0015 H16z2 -0.0004 0.0003 H17ax1 -0.0007 -0.0009 H17ay1 -0.0399 -0.0085 H17az1 -0.0022 0.0002 H17ax2 0.0003 -0.0002 H17ay2 -0.0026 0.0021 H17az2 0 0.0001 H17bx1 0.0021 -0.0035 H17by1 -0.0374 0.0077 H17bz1 -0.0031 0.0024 H17bx2 0 -0.001 H17by2 -0.0017 0.0029 H17bz2 -0.0002 0.0001 H18ax1 -0.0007 -0.0018 H18ay1 -0.0242 0.0225 H18az1 -0.0019 0.0038 H18ax2 0.0001 -0.0005 H18ay2 0.0024 0.0026 H18az2 0.0003 0 H18bx1 -0.0023 0.0034 H18by1 -0.0266 0.0211 H18bz1 -0.0021 0.0019 H18bx2 0.0005 0.0006 H18by2 0.0018 0.0029 H18bz2 0.0001 -0.0001 H19x1 -0.0013 0.0048 H19y1 -0.019 0.0138 H19z1 -0.001 0.0054 H19x2 0.0002 -0.0001 H19y2 0.0007 0.0003 H19z2 0.0002 0.0004 H20ax1 -0.0005 -0.0023 H20ay1 -0.0247 0.0096 H20az1 -0.0022 0.0069 H20ax2 -0.0003 -0.001 H20ay2 0.0015 -0.0005 H20az2 0.0004 -0.0005 H20bx1 -0.0022 0.0036 H20by1 -0.0242 -0.0008 H20bz1 -0.003 0.0065 H20bx2 0.0003 -0.0013 H20by2 0.0009 -0.0003 H20bz2 0.0005 -0.0003 H21ax1 -0.0067 0.0114 H21ay1 -0.0248 -0.0028 H21az1 -0.0031 0.003 H21ax2 0 0.0009 H21ay2 0.0006 0.0005 H21az2 0.0004 0.0001 H21bx1 -0.0065 0.0116 H21by1 -0.0265 0.0058 H21bz1 -0.0027 0.0012 H21bx2 0.0004 0.0007 H21by2 0 0.0015 H21bz2 0.0004 -0.0001 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 C01U111 C01 U11 1 C01U221 C01 U22 1 C01U331 C01 U33 1 C01U121 C01 U12 1 C01U131 C01 U13 1 C01U231 C01 U23 1 C01U112 C01 U11 2 C01U222 C01 U22 2 C01U332 C01 U33 2 C01U122 C01 U12 2 C01U132 C01 U13 2 C01U232 C01 U23 2 C02U111 C02 U11 1 C02U221 C02 U22 1 C02U331 C02 U33 1 C02U121 C02 U12 1 C02U131 C02 U13 1 C02U231 C02 U23 1 C02U112 C02 U11 2 C02U222 C02 U22 2 C02U332 C02 U33 2 C02U122 C02 U12 2 C02U132 C02 U13 2 C02U232 C02 U23 2 C03U111 C03 U11 1 C03U221 C03 U22 1 C03U331 C03 U33 1 C03U121 C03 U12 1 C03U131 C03 U13 1 C03U231 C03 U23 1 C03U112 C03 U11 2 C03U222 C03 U22 2 C03U332 C03 U33 2 C03U122 C03 U12 2 C03U132 C03 U13 2 C03U232 C03 U23 2 C04U111 C04 U11 1 C04U221 C04 U22 1 C04U331 C04 U33 1 C04U121 C04 U12 1 C04U131 C04 U13 1 C04U231 C04 U23 1 C04U112 C04 U11 2 C04U222 C04 U22 2 C04U332 C04 U33 2 C04U122 C04 U12 2 C04U132 C04 U13 2 C04U232 C04 U23 2 C05U111 C05 U11 1 C05U221 C05 U22 1 C05U331 C05 U33 1 C05U121 C05 U12 1 C05U131 C05 U13 1 C05U231 C05 U23 1 C05U112 C05 U11 2 C05U222 C05 U22 2 C05U332 C05 U33 2 C05U122 C05 U12 2 C05U132 C05 U13 2 C05U232 C05 U23 2 C06U111 C06 U11 1 C06U221 C06 U22 1 C06U331 C06 U33 1 C06U121 C06 U12 1 C06U131 C06 U13 1 C06U231 C06 U23 1 C06U112 C06 U11 2 C06U222 C06 U22 2 C06U332 C06 U33 2 C06U122 C06 U12 2 C06U132 C06 U13 2 C06U232 C06 U23 2 C07U111 C07 U11 1 C07U221 C07 U22 1 C07U331 C07 U33 1 C07U121 C07 U12 1 C07U131 C07 U13 1 C07U231 C07 U23 1 C07U112 C07 U11 2 C07U222 C07 U22 2 C07U332 C07 U33 2 C07U122 C07 U12 2 C07U132 C07 U13 2 C07U232 C07 U23 2 F08U111 F08 U11 1 F08U221 F08 U22 1 F08U331 F08 U33 1 F08U121 F08 U12 1 F08U131 F08 U13 1 F08U231 F08 U23 1 F08U112 F08 U11 2 F08U222 F08 U22 2 F08U332 F08 U33 2 F08U122 F08 U12 2 F08U132 F08 U13 2 F08U232 F08 U23 2 O09U111 O09 U11 1 O09U221 O09 U22 1 O09U331 O09 U33 1 O09U121 O09 U12 1 O09U131 O09 U13 1 O09U231 O09 U23 1 O09U112 O09 U11 2 O09U222 O09 U22 2 O09U332 O09 U33 2 O09U122 O09 U12 2 O09U132 O09 U13 2 O09U232 O09 U23 2 O10U111 O10 U11 1 O10U221 O10 U22 1 O10U331 O10 U33 1 O10U121 O10 U12 1 O10U131 O10 U13 1 O10U231 O10 U23 1 O10U112 O10 U11 2 O10U222 O10 U22 2 O10U332 O10 U33 2 O10U122 O10 U12 2 O10U132 O10 U13 2 O10U232 O10 U23 2 N11U111 N11 U11 1 N11U221 N11 U22 1 N11U331 N11 U33 1 N11U121 N11 U12 1 N11U131 N11 U13 1 N11U231 N11 U23 1 N11U112 N11 U11 2 N11U222 N11 U22 2 N11U332 N11 U33 2 N11U122 N11 U12 2 N11U132 N11 U13 2 N11U232 N11 U23 2 C12U111 C12 U11 1 C12U221 C12 U22 1 C12U331 C12 U33 1 C12U121 C12 U12 1 C12U131 C12 U13 1 C12U231 C12 U23 1 C12U112 C12 U11 2 C12U222 C12 U22 2 C12U332 C12 U33 2 C12U122 C12 U12 2 C12U132 C12 U13 2 C12U232 C12 U23 2 C13U111 C13 U11 1 C13U221 C13 U22 1 C13U331 C13 U33 1 C13U121 C13 U12 1 C13U131 C13 U13 1 C13U231 C13 U23 1 C13U112 C13 U11 2 C13U222 C13 U22 2 C13U332 C13 U33 2 C13U122 C13 U12 2 C13U132 C13 U13 2 C13U232 C13 U23 2 C14U111 C14 U11 1 C14U221 C14 U22 1 C14U331 C14 U33 1 C14U121 C14 U12 1 C14U131 C14 U13 1 C14U231 C14 U23 1 C14U112 C14 U11 2 C14U222 C14 U22 2 C14U332 C14 U33 2 C14U122 C14 U12 2 C14U132 C14 U13 2 C14U232 C14 U23 2 C15U111 C15 U11 1 C15U221 C15 U22 1 C15U331 C15 U33 1 C15U121 C15 U12 1 C15U131 C15 U13 1 C15U231 C15 U23 1 C15U112 C15 U11 2 C15U222 C15 U22 2 C15U332 C15 U33 2 C15U122 C15 U12 2 C15U132 C15 U13 2 C15U232 C15 U23 2 C16U111 C16 U11 1 C16U221 C16 U22 1 C16U331 C16 U33 1 C16U121 C16 U12 1 C16U131 C16 U13 1 C16U231 C16 U23 1 C16U112 C16 U11 2 C16U222 C16 U22 2 C16U332 C16 U33 2 C16U122 C16 U12 2 C16U132 C16 U13 2 C16U232 C16 U23 2 C17U111 C17 U11 1 C17U221 C17 U22 1 C17U331 C17 U33 1 C17U121 C17 U12 1 C17U131 C17 U13 1 C17U231 C17 U23 1 C17U112 C17 U11 2 C17U222 C17 U22 2 C17U332 C17 U33 2 C17U122 C17 U12 2 C17U132 C17 U13 2 C17U232 C17 U23 2 C18U111 C18 U11 1 C18U221 C18 U22 1 C18U331 C18 U33 1 C18U121 C18 U12 1 C18U131 C18 U13 1 C18U231 C18 U23 1 C18U112 C18 U11 2 C18U222 C18 U22 2 C18U332 C18 U33 2 C18U122 C18 U12 2 C18U132 C18 U13 2 C18U232 C18 U23 2 C19U111 C19 U11 1 C19U221 C19 U22 1 C19U331 C19 U33 1 C19U121 C19 U12 1 C19U131 C19 U13 1 C19U231 C19 U23 1 C19U112 C19 U11 2 C19U222 C19 U22 2 C19U332 C19 U33 2 C19U122 C19 U12 2 C19U132 C19 U13 2 C19U232 C19 U23 2 C20U111 C20 U11 1 C20U221 C20 U22 1 C20U331 C20 U33 1 C20U121 C20 U12 1 C20U131 C20 U13 1 C20U231 C20 U23 1 C20U112 C20 U11 2 C20U222 C20 U22 2 C20U332 C20 U33 2 C20U122 C20 U12 2 C20U132 C20 U13 2 C20U232 C20 U23 2 C21U111 C21 U11 1 C21U221 C21 U22 1 C21U331 C21 U33 1 C21U121 C21 U12 1 C21U131 C21 U13 1 C21U231 C21 U23 1 C21U112 C21 U11 2 C21U222 C21 U22 2 C21U332 C21 U33 2 C21U122 C21 U12 2 C21U132 C21 U13 2 C21U232 C21 U23 2 loop_ _atom_site_U_Fourier_param_id _atom_site_U_Fourier_param_cos _atom_site_U_Fourier_param_sin C01U111 -0.0007(7) 0.0007(7) C01U221 0.0044(8) 0.0001(8) C01U331 -0.0006(9) -0.0006(10) C01U121 -0.0012(5) 0.0002(5) C01U131 -0.0005(6) 0.0006(6) C01U231 -0.0008(6) 0.0000(6) C01U112 -0.0028(10) 0.0025(10) C01U222 -0.0002(10) -0.0174(10) C01U332 0.0035(13) -0.0030(13) C01U122 -0.0004(7) -0.0014(7) C01U132 -0.0013(9) -0.0033(8) C01U232 -0.0018(7) -0.0033(8) C02U111 -0.0009(7) 0.0014(7) C02U221 0.0021(8) -0.0002(6) C02U331 0.0001(10) 0.0004(9) C02U121 0.0010(6) 0.0018(5) C02U131 0.0006(6) 0.0019(6) C02U231 0.0007(6) -0.0020(5) C02U112 0.0006(10) 0.0017(10) C02U222 0.0202(10) -0.0204(10) C02U332 -0.0052(12) 0.0025(13) C02U122 -0.0030(7) 0.0040(7) C02U132 0.0010(8) -0.0018(9) C02U232 -0.0011(7) 0.0001(7) C03U111 -0.0021(9) 0.0020(7) C03U221 -0.0001(8) 0.0002(6) C03U331 -0.0009(12) 0.0003(10) C03U121 -0.0006(7) 0.0011(5) C03U131 0.0011(8) -0.0013(6) C03U231 -0.0003(7) -0.0019(5) C03U112 0.0077(12) -0.0011(12) C03U222 0.0203(10) -0.0025(9) C03U332 0.0060(14) 0.0018(14) C03U122 0.0097(8) -0.0018(7) C03U132 -0.0073(10) -0.0022(10) C03U232 -0.0102(8) -0.0022(8) C04U111 -0.0003(9) -0.0003(8) C04U221 -0.0007(9) -0.0001(8) C04U331 -0.0009(12) 0.0019(10) C04U121 -0.0003(7) 0.0026(6) C04U131 0.0016(8) 0.0000(7) C04U231 0.0009(7) -0.0022(6) C04U112 0.0001(12) -0.0014(13) C04U222 0.0117(11) 0.0133(11) C04U332 0.0097(15) 0.0025(15) C04U122 0.0053(8) 0.0021(8) C04U132 -0.0050(10) -0.0042(10) C04U232 -0.0074(9) -0.0064(9) C05U111 -0.0010(10) 0.0024(8) C05U221 0.0021(9) 0.0044(8) C05U331 0.0008(11) -0.0027(10) C05U121 0.0002(7) 0.0034(6) C05U131 0.0005(8) 0.0016(7) C05U231 0.0008(7) -0.0029(6) C05U112 0.0064(13) 0.0075(13) C05U222 0.0148(11) 0.0120(11) C05U332 -0.0018(14) 0.0014(14) C05U122 -0.0085(9) -0.0094(9) C05U132 -0.0032(10) -0.0093(10) C05U232 0.0060(9) 0.0034(9) C06U111 -0.0074(17) 0.0071(9) C06U221 -0.0043(9) -0.0001(6) C06U331 0.0001(14) -0.0042(11) C06U121 0.0071(9) 0.0008(5) C06U131 0.0041(11) 0.0016(7) C06U231 -0.0022(8) -0.0022(6) C06U112 0.0362(18) 0.0125(17) C06U222 0.0202(10) 0.0042(10) C06U332 0.0101(16) 0.0070(17) C06U122 -0.0261(10) -0.0078(9) C06U132 -0.0225(13) -0.0139(13) C06U232 0.0155(9) 0.0046(9) C07U111 -0.0026(13) 0.0046(8) C07U221 -0.0015(9) 0.0029(7) C07U331 0.0024(12) -0.0005(10) C07U121 0.0022(8) -0.0023(5) C07U131 0.0017(9) 0.0004(6) C07U231 0.0001(7) -0.0005(6) C07U112 0.0220(15) -0.0073(13) C07U222 0.0146(10) -0.0125(10) C07U332 0.0066(15) 0.0036(14) C07U122 -0.0187(9) 0.0115(9) C07U132 -0.0121(11) 0.0039(10) C07U232 0.0109(8) -0.0066(8) F08U111 -0.0001(8) 0.0042(8) F08U221 -0.0006(5) 0.0021(5) F08U331 0.0030(7) -0.0027(8) F08U121 0.0005(5) 0.0033(5) F08U131 -0.0032(6) 0.0019(6) F08U231 0.0004(4) -0.0014(4) F08U112 -0.0015(10) 0.0180(10) F08U222 0.0004(7) 0.0176(7) F08U332 -0.0023(10) -0.0001(10) F08U122 -0.0003(6) -0.0162(6) F08U132 0.0032(8) -0.0124(8) F08U232 -0.0010(6) 0.0089(6) O09U111 -0.0016(5) -0.0005(6) O09U221 0.0022(5) 0.0014(6) O09U331 0.0008(7) -0.0005(7) O09U121 -0.0008(4) -0.0004(4) O09U131 -0.0010(4) 0.0007(5) O09U231 0.0006(4) -0.0006(5) O09U112 0.0030(8) 0.0018(8) O09U222 -0.0168(7) -0.0268(7) O09U332 0.0005(9) 0.0002(9) O09U122 0.0004(5) 0.0023(5) O09U132 0.0027(6) -0.0002(6) O09U232 -0.0008(6) 0.0026(6) O10U111 0.0022(6) 0.0002(6) O10U221 -0.0011(6) 0.0003(6) O10U331 0.0025(7) -0.0002(7) O10U121 0.0005(4) -0.0008(4) O10U131 -0.0010(5) 0.0008(5) O10U231 -0.0006(4) -0.0007(4) O10U112 0.0007(10) 0.0053(9) O10U222 -0.0033(8) -0.0342(8) O10U332 0.0008(10) 0.0002(10) O10U122 -0.0001(6) 0.0016(6) O10U132 -0.0025(7) 0.0012(7) O10U232 -0.0020(6) -0.0006(6) N11U111 0.0004(6) -0.0006(6) N11U221 0.0025(5) -0.0005(7) N11U331 0.0008(7) 0.0005(8) N11U121 0.0010(4) -0.0002(5) N11U131 0.0005(5) -0.0001(5) N11U231 -0.0006(5) 0.0000(5) N11U112 0.0052(8) -0.0008(9) N11U222 -0.0235(8) 0.0156(8) N11U332 0.0023(10) 0.0015(10) N11U122 -0.0001(6) -0.0011(6) N11U132 0.0002(7) -0.0002(7) N11U232 -0.0022(7) 0.0008(7) C12U111 -0.0007(7) -0.0006(7) C12U221 0.0015(6) -0.0004(7) C12U331 0.0003(8) 0.0009(9) C12U121 0.0010(4) -0.0007(5) C12U131 0.0006(6) 0.0005(6) C12U231 0.0004(5) 0.0005(5) C12U112 0.0019(10) 0.0006(10) C12U222 -0.0116(8) 0.0143(8) C12U332 -0.0029(12) -0.0020(11) C12U122 -0.0032(6) 0.0026(6) C12U132 -0.0010(8) -0.0010(8) C12U232 -0.0038(7) 0.0014(7) C13U111 0.0028(7) -0.0003(8) C13U221 0.0008(6) -0.0006(7) C13U331 -0.0003(9) 0.0007(10) C13U121 0.0000(4) 0.0005(6) C13U131 0.0004(6) 0.0000(7) C13U231 -0.0012(5) 0.0005(6) C13U112 -0.0024(11) 0.0048(11) C13U222 -0.0192(8) 0.0026(8) C13U332 0.0006(12) 0.0026(12) C13U122 -0.0067(7) 0.0013(7) C13U132 0.0001(9) 0.0013(9) C13U232 -0.0011(7) -0.0005(7) C14U111 0.0036(9) -0.0024(9) C14U221 -0.0015(6) -0.0009(7) C14U331 -0.0004(10) 0.0009(11) C14U121 -0.0014(5) 0.0021(6) C14U131 -0.0007(7) 0.0003(7) C14U231 -0.0013(5) 0.0015(6) C14U112 0.0007(12) 0.0077(12) C14U222 -0.0136(8) 0.0034(8) C14U332 -0.0020(13) -0.0034(13) C14U122 -0.0070(7) 0.0036(7) C14U132 -0.0022(10) -0.0033(10) C14U232 -0.0054(7) -0.0003(7) C15U111 -0.0013(8) 0.0004(9) C15U221 -0.0029(6) -0.0027(8) C15U331 0.0027(9) -0.0001(10) C15U121 -0.0012(5) 0.0012(6) C15U131 0.0003(6) -0.0001(7) C15U231 -0.0007(5) 0.0021(6) C15U112 -0.0015(12) 0.0035(12) C15U222 -0.0130(9) -0.0010(9) C15U332 -0.0024(12) 0.0029(12) C15U122 -0.0043(7) 0.0008(7) C15U132 -0.0016(9) 0.0003(9) C15U232 -0.0044(7) 0.0002(7) C16U111 -0.0023(8) 0.0010(8) C16U221 -0.0003(6) -0.0010(6) C16U331 0.0018(9) -0.0007(9) C16U121 -0.0017(5) 0.0001(5) C16U131 0.0002(6) -0.0008(6) C16U231 -0.0005(5) 0.0014(5) C16U112 0.0029(11) -0.0009(11) C16U222 -0.0098(8) 0.0082(8) C16U332 -0.0011(12) -0.0016(12) C16U122 -0.0018(6) 0.0026(6) C16U132 -0.0009(8) 0.0010(9) C16U232 -0.0032(7) 0.0031(6) C17U111 -0.0035(7) -0.0003(7) C17U221 0.0031(5) -0.0007(7) C17U331 0.0012(9) -0.0019(9) C17U121 -0.0011(4) 0.0001(5) C17U131 0.0010(6) 0.0010(6) C17U231 0.0011(5) -0.0004(5) C17U112 0.0053(10) -0.0008(10) C17U222 -0.0148(8) 0.0073(8) C17U332 0.0007(12) 0.0019(12) C17U122 0.0001(6) 0.0003(6) C17U132 0.0022(8) 0.0013(8) C17U232 -0.0035(7) 0.0032(7) C18U111 -0.0003(7) 0.0004(7) C18U221 0.0012(6) -0.0016(6) C18U331 -0.0001(9) -0.0022(9) C18U121 -0.0001(5) 0.0007(5) C18U131 0.0003(6) 0.0004(6) C18U231 -0.0006(5) 0.0011(5) C18U112 -0.0001(10) -0.0033(10) C18U222 -0.0011(8) 0.0148(8) C18U332 0.0022(12) 0.0016(12) C18U122 -0.0002(6) 0.0023(6) C18U132 0.0017(8) 0.0000(8) C18U232 -0.0011(6) 0.0039(7) C19U111 -0.0005(7) 0.0013(7) C19U221 -0.0013(7) -0.0047(7) C19U331 0.0002(10) -0.0002(10) C19U121 -0.0003(5) 0.0018(5) C19U131 -0.0004(6) 0.0004(6) C19U231 -0.0001(6) 0.0017(6) C19U112 -0.0024(10) -0.0009(10) C19U222 0.0015(8) 0.0094(8) C19U332 -0.0003(14) 0.0026(13) C19U122 0.0009(6) 0.0018(6) C19U132 -0.0007(9) -0.0005(9) C19U232 -0.0002(7) 0.0063(7) C20U111 -0.0020(8) 0.0014(8) C20U221 -0.0016(7) -0.0032(7) C20U331 0.0024(10) -0.0019(10) C20U121 -0.0006(5) 0.0008(5) C20U131 0.0010(7) -0.0003(7) C20U231 0.0022(6) 0.0019(6) C20U112 0.0000(11) 0.0003(11) C20U222 0.0011(8) 0.0102(8) C20U332 -0.0008(14) 0.0023(13) C20U122 -0.0009(6) 0.0011(6) C20U132 0.0030(9) 0.0004(9) C20U232 0.0006(7) 0.0057(7) C21U111 -0.0001(9) -0.0008(9) C21U221 -0.0021(6) -0.0025(7) C21U331 0.0021(11) 0.0004(11) C21U121 -0.0017(5) 0.0032(5) C21U131 -0.0019(7) 0.0001(8) C21U231 -0.0009(6) 0.0038(6) C21U112 0.0029(13) 0.0016(12) C21U222 -0.0021(8) 0.0079(8) C21U332 -0.0048(14) 0.0034(15) C21U122 0.0000(7) 0.0018(7) C21U132 -0.0036(10) 0.0043(10) C21U232 -0.0022(7) 0.0025(7) 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 C01 C02 ? ? 1.513(5) 1.498(5) 1.528(5) ? C01 O09 ? ? 1.261(4) 1.239(5) 1.280(4) ? C01 O10 ? ? 1.254(4) 1.236(4) 1.268(4) ? C02 C03 ? ? 1.386(5) 1.365(5) 1.405(5) ? C02 C07 ? ? 1.388(5) 1.368(5) 1.406(5) ? C03 C04 ? ? 1.382(6) 1.371(6) 1.393(6) ? C04 C05 ? ? 1.360(5) 1.344(5) 1.380(5) ? C05 C06 ? ? 1.378(6) 1.356(6) 1.402(6) ? C05 F08 ? ? 1.355(5) 1.346(5) 1.365(5) ? C06 C07 ? ? 1.388(6) 1.380(7) 1.397(6) ? N11 C12 ? ? 1.491(5) 1.479(5) 1.499(5) ? C12 C13 ? ? 1.535(4) 1.528(4) 1.540(4) ? C12 C17 ? ? 1.533(4) 1.520(4) 1.548(4) ? C12 C18 ? ? 1.533(4) 1.526(4) 1.542(4) ? C13 C14 ? ? 1.520(5) 1.513(5) 1.527(5) ? C14 C15 ? ? 1.538(4) 1.527(4) 1.551(4) ? C14 C21 ? ? 1.531(5) 1.524(5) 1.535(5) ? C15 C16 ? ? 1.541(5) 1.535(5) 1.547(4) ? C16 C17 ? ? 1.525(5) 1.518(5) 1.531(5) ? C16 C20 ? ? 1.532(5) 1.521(5) 1.544(5) ? C18 C19 ? ? 1.524(5) 1.515(5) 1.532(5) ? C19 C20 ? ? 1.537(4) 1.516(4) 1.558(4) ? C19 C21 ? ? 1.539(5) 1.530(5) 1.548(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 C02 C01 O09 ? ? ? 118.6(3) 117.0(3) 119.7(3) ? C02 C01 O10 ? ? ? 116.8(3) 116.0(3) 117.7(3) ? O09 C01 O10 ? ? ? 124.7(3) 123.9(3) 125.5(4) ? C01 C02 C03 ? ? ? 119.1(3) 118.1(3) 119.7(3) ? C01 C02 C07 ? ? ? 122.4(3) 121.7(3) 123.1(3) ? C03 C02 C07 ? ? ? 118.5(3) 117.8(4) 119.4(3) ? C02 C03 C04 ? ? ? 121.6(3) 120.9(3) 122.3(3) ? C03 C04 C05 ? ? ? 118.1(4) 117.4(4) 118.9(4) ? C04 C05 C06 ? ? ? 122.6(4) 121.4(4) 124.1(4) ? C04 C05 F08 ? ? ? 118.9(4) 118.1(4) 119.4(4) ? C06 C05 F08 ? ? ? 118.5(3) 117.6(4) 119.4(3) ? C05 C06 C07 ? ? ? 118.5(4) 117.5(4) 119.7(3) ? C02 C07 C06 ? ? ? 120.5(4) 120.1(4) 120.8(4) ? N11 C12 C13 ? ? ? 109.2(3) 108.8(3) 109.5(3) ? N11 C12 C17 ? ? ? 109.2(3) 108.9(3) 109.5(3) ? N11 C12 C18 ? ? ? 109.4(3) 108.5(3) 110.2(3) ? C13 C12 C17 ? ? ? 109.6(3) 109.1(3) 110.2(3) ? C13 C12 C18 ? ? ? 109.6(2) 109.1(3) 110.0(2) ? C17 C12 C18 ? ? ? 109.9(2) 109.4(2) 110.4(3) ? C12 C13 C14 ? ? ? 109.3(3) 109.1(3) 109.6(3) ? C13 C14 C15 ? ? ? 109.8(3) 109.6(3) 110.0(3) ? C13 C14 C21 ? ? ? 109.8(3) 109.4(3) 110.1(3) ? C15 C14 C21 ? ? ? 109.3(3) 108.6(3) 109.7(3) ? C14 C15 C16 ? ? ? 109.1(3) 108.4(3) 109.9(3) ? C15 C16 C17 ? ? ? 109.6(3) 109.4(3) 109.9(3) ? C15 C16 C20 ? ? ? 109.1(3) 108.8(3) 109.3(3) ? C17 C16 C20 ? ? ? 109.7(3) 109.5(3) 110.0(3) ? C12 C17 C16 ? ? ? 109.3(3) 109.0(3) 109.7(3) ? C12 C18 C19 ? ? ? 109.3(3) 108.8(3) 109.7(3) ? C18 C19 C20 ? ? ? 109.7(3) 109.5(3) 110.1(3) ? C18 C19 C21 ? ? ? 109.4(3) 109.0(3) 109.6(3) ? C20 C19 C21 ? ? ? 109.1(3) 108.4(3) 109.7(3) ? C16 C20 C19 ? ? ? 109.6(3) 109.0(3) 110.0(3) ? C14 C21 C19 ? ? ? 109.5(3) 109.1(3) 109.9(3) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_ssg_symmetry_1 _geom_torsion_site_ssg_symmetry_2 _geom_torsion_site_ssg_symmetry_3 _geom_torsion_site_ssg_symmetry_4 _geom_torsion_av _geom_torsion_min _geom_torsion_max O10 C01 C02 C04 ? ? ? ? 0.8(3) -9.8(3) 9.0(3) O09 C01 C02 C06 ? ? ? ? 0.6(4) -15.6(4) 15.1(4) O09 C01 C02 C04 ? ? ? ? -46.8(3) -180.00(6) 179.6(3) O10 C01 C02 C06 ? ? ? ? -8.8(3) -179.9(3) 179.4(3)