Incommensurately modulated structure of morpholinium tetrafluoroborate and configurational versus chemical entropies at the incommensurate and lock-in phase transitions
Authors:Noohinejad, Leila ; van Smaalen, Sander ; Petricek, Vaclav ; Schoeleber, Andreas
Journal:Acta Crystallographica Section B 73 836-843 (2017)
DOI:https://doi.org/10.1107/S2052520617009398
B-IncStrDB ID: 13272ESbhTu Entry date: 2021-10-20 Last revision: 2022-02-12
I
Chemical data
Structural Formula Sum: C4 H10 B1 F4 N1 O1 [ Help ]
Formula weight: 174.93 Da [ Help ]
Absolute configuration: . [ Help ]
Crystallographic data and experimental details
Crystal system: orthorhombic [ Help ]
Superspace group name: Pnam(α00)00s [ Help ]
Symmetry operations of the superspace group: (Show/hide table) [ Help ]
| Operation code | Operation in algebraic form |
|---|---|
| 1 | x1,x2,x3,x4 |
| 2 | -x1,-x2,x3+1/2,-x4+1/2 |
| 3 | -x1+1/2,x2+1/2,-x3,-x4 |
| 4 | x1+1/2,-x2+1/2,-x3+1/2,x4+1/2 |
| 5 | -x1,-x2,-x3,-x4 |
| 6 | x1,x2,-x3+1/2,x4+1/2 |
| 7 | x1+1/2,-x2+1/2,x3,x4 |
| 8 | -x1+1/2,x2+1/2,x3+1/2,-x4+1/2 |
a: 8.09423(9) Å [ Help ]
b: 9.40452(16) Å [ Help ]
c: 9.54481(18) Å [ Help ]
α: 90 ° [ Help ]
β: 90 ° [ Help ]
γ: 90 ° [ Help ]
Volume: 726.57(2) Å3 [ Help ]
Modulation dimension: 1 [ Help ]
Measured independent wave vectors: (Show/hide table) [ Help ]
| Wave vector id | q_x | q_y | q_z |
|---|---|---|---|
| 1 | 0.421930 | 0.000000 | 0.000000 |
Z: 4 [ Help ]
Cell determination reflection Nb.: 25395 [ Help ]
θ(min) for cell determination: 2.13 ° [ Help ]
θ(max) for cell determination: 42.62 ° [ Help ]
Cell measurement temperature: 130 K [ Help ]
μ: 0.174 mm-1 [ Help ]
Absorption correction type: empirical [ Help ]
Absorption correction remarks: SADABS; Sheldrick,2008 [ Help ]
Minimum transmission factor: 0.4553 [ Help ]
Maximum transmission factor: 0.7486 [ Help ]
Refinement details
Total nb. of reflections: 6389 [ Help ]
Nb. of observed reflections: 2802 [ Help ]
Intense reflections threshold: I>3σ(I) [ Help ]
Refinement based on: F [ Help ]
R(obs): 0.0586 [ Help ]
wR(obs): 0.0682 [ Help ]
R(all): 0.1651 [ Help ]
wR(all): 0.0733 [ Help ]
S(all): 2.73 [ Help ]
S(obs): 3.90 [ Help ]
Nb. of reflections: 6389 [ Help ]
Nb. of parameters: 185 [ Help ]
Number of restraints: 0 [ Help ]
Number of constraints: 51 [ Help ]
Weighting scheme: sigma [ Help ]
Weighting scheme remarks: w=1/(σ2(F)+0.0001F2) [ Help ]
Refinement of hydrogen atoms: constr [ Help ]
Δ/σ(max): 0.0006 [ Help ]
Δ/σ(mean): 0.0001 [ Help ]
Δρ(max): 0.62 e_Å-3 [ Help ]
Δρ(min): -0.54 e_Å-3 [ Help ]
Extinction method: none [ Help ]
Structural Information
Average Structure: (Show/hide table) [ Help ]
| Atom site label | Atom symbol | x | y | z | ADP type | Uiso/equiv | Symmetry multiplicity | Occupancy | Coords from (d)iffraction or (c)alculated | Coords restraints or constraints | Disordered cluster | Disordered group |
|---|---|---|---|---|---|---|---|---|---|---|---|---|
| O1 | O | 0.03326(8) | 0.76034(6) | 0.25 | Uani | 0.03003(19) | 4 | 1 | d | . | . | . |
| N1 | N | 0.26956(7) | 0.53856(5) | 0.25 | Uani | 0.0238(2) | 4 | 1 | d | . | . | . |
| C1 | C | 0.12672(7) | 0.72981(6) | 0.37320(6) | Uani | 0.03110(19) | 8 | 1 | d | . | . | . |
| C2 | C | 0.17310(7) | 0.57458(6) | 0.37769(5) | Uani | 0.02729(17) | 8 | 1 | d | . | . | . |
| H1c | H | 0.293506 | 0.443102 | 0.25 | Uiso | 0.0356 | 4 | 1 | d | . | . | . |
| H2b | H | 0.239028 | 0.556542 | 0.459063 | Uiso | 0.0327 | 8 | 1 | d | . | . | . |
| H2a | H | 0.074813 | 0.517806 | 0.380692 | Uiso | 0.0327 | 8 | 1 | d | . | . | . |
| H1d | H | 0.366956 | 0.588698 | 0.25 | Uiso | 0.0356 | 4 | 1 | d | . | . | . |
| H1b | H | 0.062524 | 0.75312 | 0.454268 | Uiso | 0.0373 | 8 | 1 | d | . | . | . |
| H1a | H | 0.225014 | 0.78668 | 0.373974 | Uiso | 0.0373 | 8 | 1 | d | . | . | . |
| B1a | B | 0.1760(9) | 0.1454(7) | 0.2623(5) | Uani | 0.0262(17) | 8 | 0.1834 | d | . | . | . |
| F1a | F | 0.2321(13) | 0.2578(10) | 0.3422(9) | Uani | 0.039(3) | 8 | 0.1834 | d | . | . | . |
| F2a | F | 0.3049(11) | 0.0576(10) | 0.2264(8) | Uani | 0.042(3) | 8 | 0.1834 | d | . | . | . |
| F3a | F | 0.0601(12) | 0.0705(10) | 0.3387(11) | Uani | 0.040(3) | 8 | 0.1834 | d | . | . | . |
| F4a | F | 0.0999(13) | 0.1976(12) | 0.1440(7) | Uani | 0.061(3) | 8 | 0.1834 | d | . | . | . |
| B1b | B | 0.1542(4) | 0.1250(2) | 0.2631(4) | Uani | 0.0220(6) | 8 | 0.3166 | d | . | . | . |
| F1b | F | 0.298(3) | 0.047(4) | 0.2510(12) | Uani | 0.0351(15) | 8 | 0.3166 | d | . | . | . |
| F2b | F | 0.0646(19) | 0.118(3) | 0.1411(10) | Uani | 0.0432(15) | 8 | 0.3166 | d | . | . | . |
| F3b | F | 0.062(3) | 0.071(3) | 0.3728(11) | Uani | 0.0257(15) | 8 | 0.3166 | d | . | . | . |
| F4b | F | 0.194(5) | 0.2638(19) | 0.2943(12) | Uani | 0.0498(16) | 8 | 0.3166 | d | . | . | . |
ADP components: (Show/hide table) [ Help ]
| Atom site label | Atom site symbol | U11 | U22 | U33 | U12 | U13 | U23 |
|---|---|---|---|---|---|---|---|
| O1 | O | 0.0273(3) | 0.0225(3) | 0.0403(4) | 0.0070(2) | 0 | 0 |
| N1 | N | 0.0228(4) | 0.0139(3) | 0.0346(4) | 0.0002(2) | 0 | 0 |
| C1 | C | 0.0326(4) | 0.0250(3) | 0.0358(3) | 0.0039(2) | -0.0019(3) | -0.0079(2) |
| C2 | C | 0.0319(3) | 0.0243(3) | 0.0256(3) | 0.0005(2) | -0.0023(2) | -0.0003(2) |
| B1a | B | 0.012(3) | 0.035(3) | 0.031(3) | 0.0059(16) | -0.0047(18) | -0.0092(17) |
| F1a | F | 0.055(7) | 0.020(4) | 0.041(6) | -0.016(4) | -0.002(4) | 0.004(4) |
| F2a | F | 0.034(4) | 0.041(5) | 0.050(7) | 0.022(4) | 0.015(4) | 0.011(4) |
| F3a | F | 0.021(5) | 0.042(6) | 0.057(6) | -0.017(4) | 0.007(4) | -0.029(4) |
| F4a | F | 0.074(6) | 0.072(7) | 0.038(4) | 0.050(5) | -0.019(4) | -0.014(4) |
| B1b | B | 0.0256(10) | 0.0141(10) | 0.0263(13) | -0.0017(6) | -0.0011(7) | 0.0008(8) |
| F1b | F | 0.0259(18) | 0.028(3) | 0.051(3) | 0.0027(19) | -0.001(2) | -0.005(2) |
| F2b | F | 0.039(2) | 0.071(3) | 0.020(2) | 0.011(2) | -0.0007(19) | 0.0016(19) |
| F3b | F | 0.033(3) | 0.022(3) | 0.022(2) | -0.002(2) | -0.002(2) | 0.003(2) |
| F4b | F | 0.049(3) | 0.0148(19) | 0.086(3) | -0.0101(18) | 0.013(3) | -0.005(2) |
Fourier Wave Vectors (explicit: q_x,q_y,q_z or coefficients: q_1,q_2,...): (Show/hide table) [ Help ]
| Wave vector code | q_1 |
|---|---|
| 1 | 1 |
Table: (Show/hide table) [ Help ]
| _jana_atom_site_occ_Fourier_absolute_site_label | _jana_atom_site_occ_Fourier_absolute |
|---|---|
| B1a | 0.1834 |
| F1a | 0.1834 |
| F2a | 0.1834 |
| F3a | 0.1834 |
| F4a | 0.1834 |
| B1b | 0.3166 |
| F1b | 0.3166 |
| F2b | 0.3166 |
| F3b | 0.3166 |
| F4b | 0.3166 |
Definition of the occupation Fourier series: (Show/hide table) [ Help ]
| Modulation code | Atom site label | Wave vector code |
|---|---|---|
| B1ao1 | B1a | 1 |
| F1ao1 | F1a | 1 |
| F2ao1 | F2a | 1 |
| F3ao1 | F3a | 1 |
| F4ao1 | F4a | 1 |
| B1bo1 | B1b | 1 |
| F1bo1 | F1b | 1 |
| F2bo1 | F2b | 1 |
| F3bo1 | F3b | 1 |
| F4bo1 | F4b | 1 |
Occupation Fourier coefficients: (Show/hide table) [ Help ]
| Modulation code | Cosine coefficient | Sine coefficient |
|---|---|---|
| B1ao1 | 0.1482 | -0.1243 |
| F1ao1 | 0.165 | -0.101 |
| F2ao1 | 0.1813 | -0.0675 |
| F3ao1 | 0.1036 | -0.1634 |
| F4ao1 | 0.1203 | -0.1515 |
| B1bo1 | 0.1462 | -0.1437 |
| F1bo1 | 0.1892 | -0.079 |
| F2bo1 | 0.1083 | -0.174 |
| F3bo1 | 0.1072 | -0.1747 |
| F4bo1 | 0.1604 | -0.1276 |
Definition of the displacive (translational) Fourier series: (Show/hide table) [ Help ]
| Modulation code | Atom site label | Displacement axis | Wave vector code |
|---|---|---|---|
| O1x1 | O1 | x | 1 |
| O1y1 | O1 | y | 1 |
| O1z1 | O1 | z | 1 |
| N1x1 | N1 | x | 1 |
| N1y1 | N1 | y | 1 |
| N1z1 | N1 | z | 1 |
| C1x1 | C1 | x | 1 |
| C1y1 | C1 | y | 1 |
| C1z1 | C1 | z | 1 |
| C2x1 | C2 | x | 1 |
| C2y1 | C2 | y | 1 |
| C2z1 | C2 | z | 1 |
| H1cx1 | H1c | x | 1 |
| H1cy1 | H1c | y | 1 |
| H1cz1 | H1c | z | 1 |
| H2bx1 | H2b | x | 1 |
| H2by1 | H2b | y | 1 |
| H2bz1 | H2b | z | 1 |
| H2ax1 | H2a | x | 1 |
| H2ay1 | H2a | y | 1 |
| H2az1 | H2a | z | 1 |
| H1dx1 | H1d | x | 1 |
| H1dy1 | H1d | y | 1 |
| H1dz1 | H1d | z | 1 |
| H1bx1 | H1b | x | 1 |
| H1by1 | H1b | y | 1 |
| H1bz1 | H1b | z | 1 |
| H1ax1 | H1a | x | 1 |
| H1ay1 | H1a | y | 1 |
| H1az1 | H1a | z | 1 |
| B1ax1 | B1a | x | 1 |
| B1ay1 | B1a | y | 1 |
| B1az1 | B1a | z | 1 |
| F1ax1 | F1a | x | 1 |
| F1ay1 | F1a | y | 1 |
| F1az1 | F1a | z | 1 |
| F2ax1 | F2a | x | 1 |
| F2ay1 | F2a | y | 1 |
| F2az1 | F2a | z | 1 |
| F3ax1 | F3a | x | 1 |
| F3ay1 | F3a | y | 1 |
| F3az1 | F3a | z | 1 |
| F4ax1 | F4a | x | 1 |
| F4ay1 | F4a | y | 1 |
| F4az1 | F4a | z | 1 |
| B1bx1 | B1b | x | 1 |
| B1by1 | B1b | y | 1 |
| B1bz1 | B1b | z | 1 |
| F1bx1 | F1b | x | 1 |
| F1by1 | F1b | y | 1 |
| F1bz1 | F1b | z | 1 |
| F2bx1 | F2b | x | 1 |
| F2by1 | F2b | y | 1 |
| F2bz1 | F2b | z | 1 |
| F3bx1 | F3b | x | 1 |
| F3by1 | F3b | y | 1 |
| F3bz1 | F3b | z | 1 |
| F4bx1 | F4b | x | 1 |
| F4by1 | F4b | y | 1 |
| F4bz1 | F4b | z | 1 |
Displacive (translational) Fourier coefficients: (Show/hide table) [ Help ]
| Modulation code | Cosine coefficient | Sine coefficient |
|---|---|---|
| O1x1 | 0 | 0 |
| O1y1 | 0 | 0 |
| O1z1 | -0.01460(8) | 0.01918(9) |
| N1x1 | 0 | 0 |
| N1y1 | 0 | 0 |
| N1z1 | -0.00039(8) | 0.01582(8) |
| C1x1 | -0.00769(7) | -0.00815(7) |
| C1y1 | 0.00799(7) | -0.00623(7) |
| C1z1 | -0.01218(8) | 0.01779(8) |
| C2x1 | -0.00769(7) | -0.00942(7) |
| C2y1 | 0.00899(7) | -0.00588(7) |
| C2z1 | -0.00257(7) | 0.01197(6) |
| H1cx1 | 0 | 0 |
| H1cy1 | 0 | 0 |
| H1cz1 | 0.0066 | 0.0152 |
| H2bx1 | -0.0099 | -0.0173 |
| H2by1 | 0.0154 | -0.0069 |
| H2bz1 | -0.0011 | 0.0147 |
| H2ax1 | -0.0104 | -0.0073 |
| H2ay1 | 0.0077 | -0.0082 |
| H2az1 | -0.0019 | 0.0048 |
| H1dx1 | 0 | 0 |
| H1dy1 | 0 | 0 |
| H1dz1 | -0.0074 | 0.022 |
| H1bx1 | -0.0152 | -0.0111 |
| H1by1 | 0.011 | -0.0124 |
| H1bz1 | -0.0137 | 0.0185 |
| H1ax1 | -0.0051 | -0.0098 |
| H1ay1 | 0.009 | -0.0041 |
| H1az1 | -0.0176 | 0.0214 |
| B1ax1 | -0.0053(8) | 0.0003(8) |
| B1ay1 | -0.0023(7) | 0.0005(6) |
| B1az1 | 0.0011(6) | 0.0087(5) |
| F1ax1 | -0.0038(14) | -0.0119(13) |
| F1ay1 | -0.0004(10) | 0.0008(9) |
| F1az1 | -0.0036(10) | 0.0137(9) |
| F2ax1 | -0.0076(11) | 0.0065(11) |
| F2ay1 | -0.0055(11) | 0.0089(10) |
| F2az1 | -0.0007(11) | 0.0076(10) |
| F3ax1 | -0.0023(12) | 0.0059(11) |
| F3ay1 | -0.0044(12) | -0.0090(11) |
| F3az1 | 0.0043(10) | 0.0026(9) |
| F4ax1 | -0.0071(13) | 0.0000(12) |
| F4ay1 | -0.0050(12) | 0.0015(11) |
| F4az1 | 0.0024(8) | 0.0092(7) |
| B1bx1 | 0.0007(4) | -0.0003(3) |
| B1by1 | 0.0039(3) | -0.0012(2) |
| B1bz1 | 0.0008(3) | 0.0021(3) |
| F1bx1 | -0.0019(5) | 0.0014(5) |
| F1by1 | 0.0025(5) | 0.0022(5) |
| F1bz1 | -0.0126(6) | 0.0025(5) |
| F2bx1 | -0.0018(5) | 0.0020(5) |
| F2by1 | 0.0175(6) | -0.0134(6) |
| F2bz1 | 0.0017(5) | 0.0012(4) |
| F3bx1 | 0.0018(5) | -0.0006(5) |
| F3by1 | -0.0072(6) | 0.0040(5) |
| F3bz1 | -0.0032(5) | 0.0046(5) |
| F4bx1 | 0.0048(6) | -0.0040(5) |
| F4by1 | -0.0006(5) | 0.0010(4) |
| F4bz1 | 0.0169(6) | -0.0022(6) |
Definition of the ADP Fourier series: (Show/hide table) [ Help ]
| Modulation code | Atom site label | Tensor element | Wave vector code |
|---|---|---|---|
| B1aU111 | B1a | U11 | 1 |
| B1aU221 | B1a | U22 | 1 |
| B1aU331 | B1a | U33 | 1 |
| B1aU121 | B1a | U12 | 1 |
| B1aU131 | B1a | U13 | 1 |
| B1aU231 | B1a | U23 | 1 |
| F1aU111 | F1a | U11 | 1 |
| F1aU221 | F1a | U22 | 1 |
| F1aU331 | F1a | U33 | 1 |
| F1aU121 | F1a | U12 | 1 |
| F1aU131 | F1a | U13 | 1 |
| F1aU231 | F1a | U23 | 1 |
| F2aU111 | F2a | U11 | 1 |
| F2aU221 | F2a | U22 | 1 |
| F2aU331 | F2a | U33 | 1 |
| F2aU121 | F2a | U12 | 1 |
| F2aU131 | F2a | U13 | 1 |
| F2aU231 | F2a | U23 | 1 |
| F3aU111 | F3a | U11 | 1 |
| F3aU221 | F3a | U22 | 1 |
| F3aU331 | F3a | U33 | 1 |
| F3aU121 | F3a | U12 | 1 |
| F3aU131 | F3a | U13 | 1 |
| F3aU231 | F3a | U23 | 1 |
| F4aU111 | F4a | U11 | 1 |
| F4aU221 | F4a | U22 | 1 |
| F4aU331 | F4a | U33 | 1 |
| F4aU121 | F4a | U12 | 1 |
| F4aU131 | F4a | U13 | 1 |
| F4aU231 | F4a | U23 | 1 |
| B1bU111 | B1b | U11 | 1 |
| B1bU221 | B1b | U22 | 1 |
| B1bU331 | B1b | U33 | 1 |
| B1bU121 | B1b | U12 | 1 |
| B1bU131 | B1b | U13 | 1 |
| B1bU231 | B1b | U23 | 1 |
| F1bU111 | F1b | U11 | 1 |
| F1bU221 | F1b | U22 | 1 |
| F1bU331 | F1b | U33 | 1 |
| F1bU121 | F1b | U12 | 1 |
| F1bU131 | F1b | U13 | 1 |
| F1bU231 | F1b | U23 | 1 |
| F2bU111 | F2b | U11 | 1 |
| F2bU221 | F2b | U22 | 1 |
| F2bU331 | F2b | U33 | 1 |
| F2bU121 | F2b | U12 | 1 |
| F2bU131 | F2b | U13 | 1 |
| F2bU231 | F2b | U23 | 1 |
| F3bU111 | F3b | U11 | 1 |
| F3bU221 | F3b | U22 | 1 |
| F3bU331 | F3b | U33 | 1 |
| F3bU121 | F3b | U12 | 1 |
| F3bU131 | F3b | U13 | 1 |
| F3bU231 | F3b | U23 | 1 |
| F4bU111 | F4b | U11 | 1 |
| F4bU221 | F4b | U22 | 1 |
| F4bU331 | F4b | U33 | 1 |
| F4bU121 | F4b | U12 | 1 |
| F4bU131 | F4b | U13 | 1 |
| F4bU231 | F4b | U23 | 1 |
ADP Fourier coefficients: (Show/hide table) [ Help ]
| Modulation code | Cosine coefficient | Sine coefficient |
|---|---|---|
| B1aU111 | 0.016015 | -0.012835 |
| B1aU221 | -0.003849 | 0.005525 |
| B1aU331 | -0.011091 | 0.001865 |
| B1aU121 | 0.000081 | 0.003694 |
| B1aU131 | 0.00108 | -0.001996 |
| B1aU231 | 0.004893 | -0.005798 |
| F1aU111 | 0.006456 | 0.001026 |
| F1aU221 | -0.00172 | 0.00092 |
| F1aU331 | 0.001477 | -0.011583 |
| F1aU121 | 0.00628 | -0.001279 |
| F1aU131 | -0.001285 | -0.001705 |
| F1aU231 | -0.002341 | 0.003442 |
| F2aU111 | 0.014553 | -0.003281 |
| F2aU221 | -0.002061 | 0.004056 |
| F2aU331 | -0.007728 | -0.002976 |
| F2aU121 | -0.003089 | 0.00581 |
| F2aU131 | -0.008373 | 0.003424 |
| F2aU231 | -0.007537 | 0.002839 |
| F3aU111 | 0.009868 | -0.020394 |
| F3aU221 | 0.006784 | -0.004408 |
| F3aU331 | -0.011096 | -0.000274 |
| F3aU121 | -0.001529 | 0.007598 |
| F3aU131 | -0.004153 | -0.002535 |
| F3aU231 | 0.007884 | -0.012197 |
| F4aU111 | 0.00925 | -0.017765 |
| F4aU221 | 0.001007 | -0.00478 |
| F4aU331 | -0.009649 | 0.00311 |
| F4aU121 | -0.001919 | -0.000026 |
| F4aU131 | 0.001577 | -0.00267 |
| F4aU231 | 0.006723 | -0.009449 |
| B1bU111 | -0.003223 | 0.004295 |
| B1bU221 | 0.000432 | -0.001473 |
| B1bU331 | 0.003133 | -0.002956 |
| B1bU121 | 0 | -0.00001 |
| B1bU131 | -0.000366 | -0.001762 |
| B1bU231 | 0.003154 | -0.000969 |
| F1bU111 | -0.002205 | 0.002859 |
| F1bU221 | 0.007085 | 0.000497 |
| F1bU331 | 0.001347 | -0.012175 |
| F1bU121 | 0.00385 | 0.000667 |
| F1bU131 | -0.000067 | -0.005339 |
| F1bU231 | 0.0031 | -0.003718 |
| F2bU111 | -0.001371 | -0.003935 |
| F2bU221 | -0.021431 | 0.009195 |
| F2bU331 | 0.002731 | -0.006723 |
| F2bU121 | 0.00226 | 0.004226 |
| F2bU131 | -0.001362 | 0.00366 |
| F2bU231 | 0.002612 | -0.004911 |
| F3bU111 | 0.000391 | 0.001353 |
| F3bU221 | -0.007423 | 0.001272 |
| F3bU331 | 0.00008 | -0.004629 |
| F3bU121 | -0.002514 | 0.000206 |
| F3bU131 | -0.000235 | -0.004071 |
| F3bU231 | -0.002597 | -0.000185 |
| F4bU111 | 0.003905 | 0.001027 |
| F4bU221 | -0.000986 | -0.001162 |
| F4bU331 | -0.020621 | -0.000054 |
| F4bU121 | -0.000259 | 0.000087 |
| F4bU131 | -0.007136 | 0.0009 |
| F4bU231 | 0.010409 | -0.001875 |
mfb_n160
Chemical data
Formula moiety: B1 F4, C4 H10 N1 O1 [ Help ]
Structural Formula Sum: C4 H10 B1 F4 N1 O1 [ Help ]
Formula weight: 174.9 Da [ Help ]
Absolute configuration: . [ Help ]
Crystallographic data and experimental details
Crystal system: orthorhombic [ Help ]
Space group name (H-M): P n a m [ Help ]
Space group name (Hall): -P -2xabc;-2yab;-2zc [ Help ]
Space group nb.: 62 [ Help ]
Symmetry operations of the space group: (Show/hide table) [ Help ]
| Operation code | Operation in algebraic form |
|---|---|
| 1 | x,y,z |
| 2 | -x,-y,z+1/2 |
| 3 | -x+1/2,y+1/2,-z |
| 4 | x+1/2,-y+1/2,-z+1/2 |
| 5 | -x,-y,-z |
| 6 | x,y,-z+1/2 |
| 7 | x+1/2,-y+1/2,z |
| 8 | -x+1/2,y+1/2,z+1/2 |
a: 8.13100(12) Å [ Help ]
b: 9.40719(22) Å [ Help ]
c: 9.58445(29) Å [ Help ]
α: 90 ° [ Help ]
β: 90 ° [ Help ]
γ: 90 ° [ Help ]
Volume: 733.11(3) Å3 [ Help ]
Z: 4 [ Help ]
Cell determination reflection Nb.: 2015 [ Help ]
θ(min) for cell determination: 2.12 ° [ Help ]
θ(max) for cell determination: 37.61 ° [ Help ]
Cell measurement temperature: 160 K [ Help ]
μ: 0.173 mm-1 [ Help ]
Absorption correction type: empirical [ Help ]
Absorption correction remarks: SADABS; Sheldrick,2008 [ Help ]
Minimum transmission factor: 0.4473 [ Help ]
Maximum transmission factor: 0.7477 [ Help ]
Refinement details
Total nb. of reflections: 1797 [ Help ]
Nb. of observed reflections: 997 [ Help ]
Intense reflections threshold: I>3σ(I) [ Help ]
Refinement based on: F [ Help ]
R(obs): 0.0495 [ Help ]
wR(obs): 0.0649 [ Help ]
R(all): 0.0976 [ Help ]
wR(all): 0.0690 [ Help ]
S(all): 2.44 [ Help ]
S(obs): 3.14 [ Help ]
Nb. of reflections: 1797 [ Help ]
Nb. of parameters: 93 [ Help ]
Number of restraints: 0 [ Help ]
Number of constraints: 22 [ Help ]
Weighting scheme: sigma [ Help ]
Weighting scheme remarks: w=1/(σ2(F)+0.0001F2) [ Help ]
Refinement of hydrogen atoms: constr [ Help ]
Δ/σ(max): 0.0001 [ Help ]
Δ/σ(mean): 0.0000 [ Help ]
Δρ(max): 0.26 e_Å-3 [ Help ]
Δρ(min): -0.30 e_Å-3 [ Help ]
Extinction method: none [ Help ]
Structural Information
Average Structure: (Show/hide table) [ Help ]
| Atom site label | Atom symbol | x | y | z | ADP type | Uiso/equiv | Symmetry multiplicity | Occupancy | Coords from (d)iffraction or (c)alculated | Coords restraints or constraints | Disordered cluster | Disordered group |
|---|---|---|---|---|---|---|---|---|---|---|---|---|
| O1 | O | 0.02967(14) | 0.76002(11) | 0.25 | Uani | 0.0369(4) | 4 | 1 | d | . | . | . |
| N1 | N | 0.26669(14) | 0.53944(11) | 0.25 | Uani | 0.0278(4) | 4 | 1 | d | . | . | . |
| C1 | C | 0.12308(14) | 0.73029(12) | 0.37276(13) | Uani | 0.0373(4) | 8 | 1 | d | . | . | . |
| C2 | C | 0.17054(14) | 0.57537(11) | 0.37765(12) | Uani | 0.0326(3) | 8 | 1 | d | . | . | . |
| H1c | H | 0.290812 | 0.443886 | 0.25 | Uiso | 0.0417 | 4 | 1 | d | . | . | . |
| H2b | H | 0.236621 | 0.557948 | 0.458878 | Uiso | 0.0391 | 8 | 1 | d | . | . | . |
| H2a | H | 0.073017 | 0.517953 | 0.381035 | Uiso | 0.0391 | 8 | 1 | d | . | . | . |
| H1d | H | 0.363752 | 0.589697 | 0.25 | Uiso | 0.0417 | 4 | 1 | d | . | . | . |
| H1b | H | 0.059043 | 0.753493 | 0.453771 | Uiso | 0.0448 | 8 | 1 | d | . | . | . |
| H1a | H | 0.220588 | 0.78783 | 0.373311 | Uiso | 0.0448 | 8 | 1 | d | . | . | . |
| B1a | B | 0.1760(14) | 0.1503(14) | 0.2613(11) | Uani | 0.027(2) | 8 | 0.188(13) | d | . | . | . |
| F1a | F | 0.233(2) | 0.261(2) | 0.341(2) | Uani | 0.053(6) | 8 | 0.188(13) | d | . | . | . |
| F2a | F | 0.300(2) | 0.056(2) | 0.2297(17) | Uani | 0.051(6) | 8 | 0.188(13) | d | . | . | . |
| F3a | F | 0.053(2) | 0.080(2) | 0.333(2) | Uani | 0.061(6) | 8 | 0.188(13) | d | . | . | . |
| F4a | F | 0.117(3) | 0.203(2) | 0.1374(14) | Uani | 0.080(6) | 8 | 0.188(13) | d | . | . | . |
| B1b | B | 0.1539(9) | 0.1233(6) | 0.2354(8) | Uani | 0.0251(13) | 8 | 0.312(13) | d | . | . | . |
| F1b | F | 0.295(3) | 0.046(3) | 0.254(2) | Uani | 0.044(3) | 8 | 0.312(13) | d | . | . | . |
| F2b | F | 0.060(3) | 0.068(3) | 0.1289(19) | Uani | 0.032(4) | 8 | 0.312(13) | d | . | . | . |
| F3b | F | 0.064(3) | 0.122(3) | 0.357(2) | Uani | 0.057(4) | 8 | 0.312(13) | d | . | . | . |
| F4b | F | 0.195(4) | 0.260(2) | 0.199(2) | Uani | 0.065(4) | 8 | 0.312(13) | d | . | . | . |
ADP components: (Show/hide table) [ Help ]
| Atom site label | Atom site symbol | U11 | U22 | U33 | U12 | U13 | U23 |
|---|---|---|---|---|---|---|---|
| O1 | O | 0.0284(6) | 0.0262(5) | 0.0560(8) | 0.0082(4) | 0 | 0 |
| N1 | N | 0.0239(7) | 0.0155(5) | 0.0439(7) | -0.0005(4) | 0 | 0 |
| C1 | C | 0.0360(7) | 0.0310(6) | 0.0449(7) | 0.0035(4) | -0.0010(5) | -0.0112(5) |
| C2 | C | 0.0387(7) | 0.0292(5) | 0.0299(5) | 0.0007(4) | -0.0024(5) | 0.0002(4) |
| B1a | B | 0.030(4) | 0.017(3) | 0.034(4) | 0.001(2) | -0.004(3) | -0.001(2) |
| F1a | F | 0.077(11) | 0.024(8) | 0.058(10) | -0.026(8) | -0.009(9) | -0.001(7) |
| F2a | F | 0.040(8) | 0.056(10) | 0.056(12) | 0.022(7) | 0.006(8) | 0.001(9) |
| F3a | F | 0.037(8) | 0.055(12) | 0.090(10) | -0.027(8) | 0.021(7) | -0.023(9) |
| F4a | F | 0.099(12) | 0.103(13) | 0.038(5) | 0.058(10) | -0.022(6) | -0.005(6) |
| B1b | B | 0.0262(19) | 0.015(2) | 0.034(2) | -0.0026(11) | 0.0002(10) | -0.0010(16) |
| F1b | F | 0.032(4) | 0.031(7) | 0.070(7) | 0.006(4) | -0.008(4) | -0.007(5) |
| F2b | F | 0.036(5) | 0.032(7) | 0.028(6) | -0.007(5) | 0.000(4) | -0.001(5) |
| F3b | F | 0.049(7) | 0.091(7) | 0.032(6) | 0.003(5) | 0.006(5) | -0.016(4) |
| F4b | F | 0.057(7) | 0.018(6) | 0.122(7) | -0.015(4) | -0.015(5) | 0.012(5) |