#------------------------------------------------------------------------------
#$Date: 2023-07-05 11:58:15 +0300 (Wed, 05 Jul 2023) $
#$Revision: 284853 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/17/7131709.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7131709
loop_
_publ_author_name
'Ma, Liulei'
'Zheng, Qixuan'
'Unruh, Daniel K.'
'Hutchins, Kristin M.'
_publ_section_title
;
 Reversible interconversion of pharmaceutical salt polymorphs facilitated
 by mechanical methods.
;
_journal_issue                   50
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7779
_journal_page_last               7782
_journal_paper_doi               10.1039/d3cc02188b
_journal_volume                  59
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C14 H19 N4 O3, C3 H5 O3'
_chemical_formula_sum            'C17 H24 N4 O6'
_chemical_formula_weight         380.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-15
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2023-02-10 deposited with the CCDC.	2023-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.2640(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.09750(10)
_cell_length_b                   36.4142(5)
_cell_length_c                   10.00430(10)
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.2290
_cell_measurement_theta_min      4.5810
_cell_volume                     1849.18(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -76.00  25.00   0.50    6.91    --  -47.76  90.00 -15.00  202
  2  ω    -20.00  77.00   0.50    6.91    --   47.76 -90.00-130.00  194
  3  ω   -163.00 -79.00   0.50   25.00    --  -91.75 -90.00-130.00  168
  4  ω    -79.00 -19.00   0.50   25.00    --  -91.75  90.00 -15.00  120
  5  ω     35.00 105.00   0.50   25.00    --  107.31 -90.00-130.00  140
  6  ω    101.00 178.00   0.50   25.00    --  107.31  90.00 -15.00  154
  7  ω   -120.00 -73.00   0.50    6.91    --  -47.76-125.00   0.00   94
  8  ω   -120.00 -73.00   0.50    6.91    --  -47.76-125.00  30.00   94
  9  ω   -120.00 -73.00   0.50    6.91    --  -47.76-125.00 -30.00   94
 10  ω    -25.00  28.00   0.50    6.91    --  -47.76  19.00 -90.00  106
 11  ω    -85.00 -19.00   0.50   25.00    --  -91.75 125.00   0.00  132
 12  ω    -64.00 -19.00   0.50   25.00    --  -91.75  57.00 -30.00   90
 13  ω    -64.00 -19.00   0.50   25.00    --  -91.75  57.00 -60.00   90
 14  ω    -64.00 -19.00   0.50   25.00    --  -91.75  57.00   0.00   90
 15  ω    -64.00 -19.00   0.50   25.00    --  -91.75  57.00-180.00   90
 16  ω    -82.00 -37.00   0.50   25.00    --  -91.75 125.00 120.00   90
 17  ω     96.00 167.00   0.50   25.00    --  107.31  19.00 -90.00  142
 18  ω     35.00  62.00   0.50   25.00    --  107.31 -57.00 120.00   54
 19  ω     82.00 107.00   0.50   25.00    --  107.31 -77.00  30.00   50
 20  ω     37.00  67.00   0.50   25.00    --  107.31 -57.00  30.00   60
 21  ω     37.00 107.00   0.50   25.00    --  107.31 -77.00-120.00  140
 22  ω    100.00 169.00   0.50   25.00    --  107.31 125.00  60.00  138
 23  ω     35.00  68.00   0.50   25.00    --  107.31 -57.00  60.00   66
 24  ω     36.00  66.00   0.50   25.00    --  107.31 -57.00  90.00   60
 25  ω     36.00  68.00   0.50   25.00    --  107.31 -77.00  30.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0354371000
_diffrn_orient_matrix_UB_12      -0.0108238000
_diffrn_orient_matrix_UB_13      -0.1461196000
_diffrn_orient_matrix_UB_21      -0.1199596000
_diffrn_orient_matrix_UB_22      0.0369927000
_diffrn_orient_matrix_UB_23      -0.0489027000
_diffrn_orient_matrix_UB_31      0.2765179000
_diffrn_orient_matrix_UB_32      0.0174453000
_diffrn_orient_matrix_UB_33      0.0130164000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18312
_diffrn_reflns_point_group_measured_fraction_full 0.836
_diffrn_reflns_point_group_measured_fraction_max 0.775
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.207
_diffrn_reflns_theta_min         2.427
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.878
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.725
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       needle
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.161
_exptl_crystal_size_mid          0.033
_exptl_crystal_size_min          0.021
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.1(2)
_refine_ls_extinction_coef       0.0018(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         6107
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0580P)²+0.1770P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.0945
_reflns_Friedel_coverage         0.602
_reflns_Friedel_fraction_full    0.667
_reflns_Friedel_fraction_max     0.592
_reflns_number_gt                5538
_reflns_number_total             6107
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3cc02188b2.cif
_cod_data_source_block           TMP_DLA_a
_cod_depositor_comments
'Adding full bibliography for 7131709--7131712.cif.'
_cod_database_code               7131709
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C35  H35  N35  O35  '
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.872
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.1(2)
 -0.1(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3. Rigid body (RIGU) restrains
 O10A, O11A, O12A, C32A, C33A, C34A, O10B, O11B, O12B, C32B, C33B, C34B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Fixed Sof: O10A(0.5) O11A(0.5) O12A(0.5) H12A(0.5) C32A(0.5) C33A(0.5)
 H33A(0.5) C34A(0.5) H34A(0.5) H34B(0.5) H34C(0.5) O10B(0.5) O11B(0.5)
 O12B(0.5) H12B(0.5) C32B(0.5) C33B(0.5) H33B(0.5) C34B(0.5) H34D(0.5)
 H34E(0.5) H34F(0.5)
5.a Ternary CH refined with riding coordinates:
 C30(H30), C33A(H33A), C33B(H33B)
5.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C24(H24A,H24B)
5.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C4(H4), C6(H6), C12(H12), N5(H5), C18(H18), C20(H20), C26(H26)
5.d X=CH2 refined with riding coordinates:
 N2(H2A,H2B), N4(H4A,H4B), N6(H6A,H6B), N8(H8D,H8E)
5.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C21(H21A,H21B,H21C),
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C31(H31A,H31B,H31C), C34A(H34A,H34B,
 H34C), C34B(H34D,H34E,H34F)
5.f Idealised tetrahedral OH refined as rotating group:
 O9(H9), O12A(H12A), O12B(H12B)
;
_olex2_exptl_crystal_mounting_method 'Hampton Research 20 micron nylon CryoLoop'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.653
_oxdiff_exptl_absorpt_empirical_full_min 0.735
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O -0.3817(4) 0.69841(7) 0.3166(2) 0.0281(5) Uani 1 1 d . . . . .
O2 O -0.0267(4) 0.74467(6) 0.4369(2) 0.0265(5) Uani 1 1 d . . . . .
O3 O 0.3271(4) 0.72193(7) 0.6340(2) 0.0282(5) Uani 1 1 d . . . . .
N1 N 0.4143(5) 0.55484(7) 0.3648(2) 0.0210(5) Uani 1 1 d . . . . .
H1 H 0.450546 0.558553 0.281517 0.025 Uiso 1 1 calc R U . . .
N2 N 0.7227(5) 0.50897(7) 0.3836(2) 0.0218(5) Uani 1 1 d . . . . .
H2A H 0.808935 0.491399 0.429281 0.026 Uiso 1 1 calc R U . . .
H2B H 0.760147 0.514175 0.301596 0.026 Uiso 1 1 calc R U . . .
N3 N 0.4775(5) 0.51991(7) 0.5634(2) 0.0213(5) Uani 1 1 d . . . . .
N4 N 0.2368(5) 0.53234(8) 0.7389(3) 0.0274(6) Uani 1 1 d . . . . .
H4A H 0.317192 0.513854 0.781962 0.033 Uiso 1 1 calc R U . . .
H4B H 0.118403 0.545199 0.777340 0.033 Uiso 1 1 calc R U . . .
C1 C -0.2126(6) 0.68386(9) 0.4163(3) 0.0223(6) Uani 1 1 d . . . . .
C2 C -0.0306(6) 0.70859(9) 0.4792(3) 0.0230(6) Uani 1 1 d . . . . .
C3 C 0.1552(6) 0.69605(9) 0.5807(3) 0.0235(6) Uani 1 1 d . . . . .
C4 C 0.1523(6) 0.65947(9) 0.6221(3) 0.0222(6) Uani 1 1 d . . . . .
H4 H 0.276325 0.651149 0.692271 0.027 Uiso 1 1 calc R U . . .
C5 C -0.0317(5) 0.63523(9) 0.5609(3) 0.0210(6) Uani 1 1 d . . . . .
C6 C -0.2138(6) 0.64724(9) 0.4569(3) 0.0216(6) Uani 1 1 d . . . . .
H6 H -0.337641 0.630522 0.414229 0.026 Uiso 1 1 calc R U . . .
C7 C -0.5815(6) 0.67492(10) 0.2558(3) 0.0283(7) Uani 1 1 d . . . . .
H7A H -0.685584 0.688237 0.184192 0.042 Uiso 1 1 calc R U . . .
H7B H -0.696622 0.666957 0.323525 0.042 Uiso 1 1 calc R U . . .
H7C H -0.499842 0.653398 0.217901 0.042 Uiso 1 1 calc R U . . .
C8 C -0.1365(7) 0.76926(10) 0.5297(4) 0.0320(7) Uani 1 1 d . . . . .
H8A H -0.107421 0.794702 0.502806 0.048 Uiso 1 1 calc R U . . .
H8B H -0.050719 0.765120 0.620204 0.048 Uiso 1 1 calc R U . . .
H8C H -0.325974 0.764681 0.529353 0.048 Uiso 1 1 calc R U . . .
C9 C 0.5018(6) 0.71120(10) 0.7468(3) 0.0319(8) Uani 1 1 d . . . . .
H9A H 0.609511 0.690435 0.721856 0.048 Uiso 1 1 calc R U . . .
H9B H 0.399303 0.703914 0.820685 0.048 Uiso 1 1 calc R U . . .
H9C H 0.616674 0.731867 0.775414 0.048 Uiso 1 1 calc R U . . .
C10 C -0.0308(5) 0.59563(8) 0.6082(3) 0.0210(6) Uani 1 1 d . . . . .
H10A H -0.208972 0.585171 0.586739 0.025 Uiso 1 1 calc R U . . .
H10B H 0.007576 0.595181 0.706979 0.025 Uiso 1 1 calc R U . . .
C11 C 0.1680(5) 0.57147(8) 0.5459(3) 0.0203(6) Uani 1 1 d . . . . .
C12 C 0.2359(5) 0.57644(9) 0.4192(3) 0.0209(6) Uani 1 1 d . . . . .
H12 H 0.155226 0.595801 0.366652 0.025 Uiso 1 1 calc R U . . .
C13 C 0.5373(5) 0.52751(9) 0.4381(3) 0.0200(6) Uani 1 1 d . . . . .
C14 C 0.2942(6) 0.54082(9) 0.6159(3) 0.0216(6) Uani 1 1 d . . . . .
O4 O 1.3795(4) 0.30111(7) 1.1836(2) 0.0319(5) Uani 1 1 d . . . . .
O5 O 1.0237(4) 0.25557(6) 1.0618(2) 0.0284(5) Uani 1 1 d . . . . .
O6 O 0.6734(4) 0.27842(6) 0.8658(2) 0.0282(5) Uani 1 1 d . . . . .
N5 N 0.5769(6) 0.44554(7) 1.1298(2) 0.0277(6) Uani 1 1 d . . . . .
H5 H 0.532524 0.441773 1.211619 0.033 Uiso 1 1 calc R U . . .
N6 N 0.2802(5) 0.49304(8) 1.1077(3) 0.0271(6) Uani 1 1 d . . . . .
H6A H 0.202233 0.511264 1.061909 0.033 Uiso 1 1 calc R U . . .
H6B H 0.235984 0.487821 1.188539 0.033 Uiso 1 1 calc R U . . .
N7 N 0.5340(5) 0.48092(7) 0.9325(2) 0.0193(5) Uani 1 1 d . . . . .
N8 N 0.7795(5) 0.46785(8) 0.7587(3) 0.0256(6) Uani 1 1 d . . . . .
H8D H 0.704437 0.486687 0.715367 0.031 Uiso 1 1 calc R U . . .
H8E H 0.896915 0.454572 0.721163 0.031 Uiso 1 1 calc R U . . .
C15 C 1.2114(6) 0.31593(9) 1.0833(3) 0.0256(7) Uani 1 1 d . . . . .
C16 C 1.0287(6) 0.29157(8) 1.0211(3) 0.0231(6) Uani 1 1 d . . . . .
C17 C 0.8447(6) 0.30414(8) 0.9190(3) 0.0241(6) Uani 1 1 d . . . . .
C18 C 0.8470(6) 0.34056(9) 0.8789(4) 0.0287(7) Uani 1 1 d . . . . .
H18 H 0.722468 0.348995 0.809188 0.034 Uiso 1 1 calc R U . . .
C19 C 1.0325(6) 0.36498(9) 0.9411(4) 0.0309(8) Uani 1 1 d . . . . .
C20 C 1.2126(6) 0.35260(9) 1.0433(4) 0.0295(7) Uani 1 1 d . . . . .
H20 H 1.337407 0.369157 1.086280 0.035 Uiso 1 1 calc R U . . .
C21 C 1.5807(7) 0.32440(11) 1.2460(3) 0.0336(8) Uani 1 1 d . . . . .
H21A H 1.692621 0.333282 1.178299 0.050 Uiso 1 1 calc R U . . .
H21B H 1.688051 0.310527 1.314919 0.050 Uiso 1 1 calc R U . . .
H21C H 1.499288 0.345364 1.287720 0.050 Uiso 1 1 calc R U . . .
C22 C 1.1380(7) 0.23112(9) 0.9697(4) 0.0313(7) Uani 1 1 d . . . . .
H22A H 1.048839 0.234385 0.879492 0.047 Uiso 1 1 calc R U . . .
H22B H 1.116965 0.205665 0.998721 0.047 Uiso 1 1 calc R U . . .
H22C H 1.325807 0.236692 0.968399 0.047 Uiso 1 1 calc R U . . .
C23 C 0.4971(6) 0.28913(10) 0.7534(4) 0.0324(8) Uani 1 1 d . . . . .
H23A H 0.598045 0.299358 0.683335 0.049 Uiso 1 1 calc R U . . .
H23B H 0.374667 0.307737 0.781581 0.049 Uiso 1 1 calc R U . . .
H23C H 0.397682 0.267661 0.718048 0.049 Uiso 1 1 calc R U . . .
C24 C 1.0317(6) 0.40422(9) 0.8933(4) 0.0343(8) Uani 1 1 d . . . . .
H24A H 0.993942 0.404469 0.794422 0.041 Uiso 1 1 calc R U . . .
H24B H 1.209886 0.414676 0.914643 0.041 Uiso 1 1 calc R U . . .
C25 C 0.8333(6) 0.42861(9) 0.9542(3) 0.0251(7) Uani 1 1 d . . . . .
C26 C 0.7593(6) 0.42334(9) 1.0778(3) 0.0298(7) Uani 1 1 d . . . . .
H26 H 0.835117 0.403727 1.130742 0.036 Uiso 1 1 calc R U . . .
C27 C 0.4653(6) 0.47334(8) 1.0545(3) 0.0212(6) Uani 1 1 d . . . . .
C28 C 0.7153(6) 0.45943(8) 0.8811(3) 0.0206(6) Uani 1 1 d . . . . .
O7 O 0.8837(4) 0.54921(7) 0.1575(2) 0.0296(5) Uani 1 1 d . . . . .
O8 O 0.4912(4) 0.57680(7) 0.1199(2) 0.0272(5) Uani 1 1 d . . . . .
O9 O 1.0620(4) 0.57639(8) -0.0634(2) 0.0368(6) Uani 1 1 d . . . . .
H9 H 1.168696 0.580561 0.003940 0.055 Uiso 1 1 calc R U . . .
C29 C 0.7239(6) 0.56932(8) 0.0911(3) 0.0209(6) Uani 1 1 d . . . . .
C30 C 0.8067(5) 0.58741(8) -0.0360(3) 0.0246(6) Uani 1 1 d . . . . .
H30 H 0.680864 0.579166 -0.112678 0.029 Uiso 1 1 calc R U . . .
C31 C 0.7888(10) 0.62883(11) -0.0278(5) 0.0570(12) Uani 1 1 d . . . . .
H31A H 0.896280 0.637509 0.052222 0.086 Uiso 1 1 calc R U . . .
H31B H 0.604901 0.636063 -0.022260 0.086 Uiso 1 1 calc R U . . .
H31C H 0.853565 0.639748 -0.108054 0.086 Uiso 1 1 calc R U . . .
O10A O 0.4976(9) 0.42019(14) 0.3645(4) 0.0217(9) Uani 0.5 1 d . . P A 1
O11A O 0.132(3) 0.4539(5) 0.3444(13) 0.0239(16) Uani 0.5 1 d . . P A 1
O12A O -0.0688(8) 0.41868(14) 0.5517(4) 0.0263(9) Uani 0.5 1 d . . P A 1
H12A H -0.186698 0.425145 0.492103 0.039 Uiso 0.5 1 calc R U P A 1
C32A C 0.2656(11) 0.42849(17) 0.3930(6) 0.0175(9) Uani 0.5 1 d . . P A 1
C33A C 0.1406(10) 0.40164(15) 0.4904(5) 0.0212(10) Uani 0.5 1 d . . P A 1
H33A H 0.065875 0.380333 0.436565 0.025 Uiso 0.5 1 calc R U P A 1
C34A C 0.3348(10) 0.38678(16) 0.6008(5) 0.0264(11) Uani 0.5 1 d . . P A 1
H34A H 0.400593 0.406970 0.659419 0.040 Uiso 0.5 1 calc R U P A 1
H34B H 0.482606 0.375172 0.560971 0.040 Uiso 0.5 1 calc R U P A 1
H34C H 0.246972 0.368594 0.653500 0.040 Uiso 0.5 1 calc R U P A 1
O10B O 0.189(3) 0.4545(5) 0.3285(15) 0.029(2) Uani 0.5 1 d . . P B 2
O11B O -0.0024(6) 0.44758(10) 0.5192(3) 0.0216(7) Uani 0.5 1 d . . P B 2
O12B O 0.5789(8) 0.40747(14) 0.4038(4) 0.0269(9) Uani 0.5 1 d . . P B 2
H12B H 0.715746 0.418242 0.436419 0.040 Uiso 0.5 1 calc R U P B 2
C32B C 0.1750(10) 0.44044(14) 0.4422(5) 0.0184(8) Uani 0.5 1 d . . P B 2
C33B C 0.3773(10) 0.41159(14) 0.4913(5) 0.0223(9) Uani 0.5 1 d . . P B 2
H33B H 0.459398 0.418955 0.581958 0.027 Uiso 0.5 1 calc R U P B 2
C34B C 0.2380(13) 0.37458(19) 0.5035(7) 0.0322(13) Uani 0.5 1 d . . P B 2
H34D H 0.155144 0.367215 0.415284 0.048 Uiso 0.5 1 calc R U P B 2
H34E H 0.102744 0.376914 0.566573 0.048 Uiso 0.5 1 calc R U P B 2
H34F H 0.366895 0.355960 0.536391 0.048 Uiso 0.5 1 calc R U P B 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 23 2 0.0125
3 1 -1 0.0653
-3 -13 0 0.0667
0 1 -2 0.0112
0 -1 2 0.0093
2 10 -4 0.0384
0 -24 1 0.0142
-2 -18 0 0.0494
0 -17 -5 0.0118
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 C7 117.3(3) . . ?
C2 O2 C8 112.1(2) . . ?
C3 O3 C9 116.9(3) . . ?
C12 N1 H1 119.9 . . ?
C12 N1 C13 120.2(2) . . ?
C13 N1 H1 119.9 . . ?
H2A N2 H2B 120.0 . . ?
C13 N2 H2A 120.0 . . ?
C13 N2 H2B 120.0 . . ?
C13 N3 C14 118.1(2) . . ?
H4A N4 H4B 120.0 . . ?
C14 N4 H4A 120.0 . . ?
C14 N4 H4B 120.0 . . ?
O1 C1 C2 115.3(3) . . ?
O1 C1 C6 124.4(3) . . ?
C6 C1 C2 120.3(3) . . ?
O2 C2 C1 120.1(3) . . ?
O2 C2 C3 120.3(3) . . ?
C3 C2 C1 119.5(3) . . ?
O3 C3 C2 115.2(3) . . ?
O3 C3 C4 124.6(3) . . ?
C4 C3 C2 120.1(3) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 C3 120.0(3) . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 120.3(3) . . ?
C4 C5 C10 118.9(3) . . ?
C6 C5 C10 120.8(3) . . ?
C1 C6 C5 119.7(3) . . ?
C1 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
O1 C7 H7A 109.5 . . ?
O1 C7 H7B 109.5 . . ?
O1 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O2 C8 H8A 109.5 . . ?
O2 C8 H8B 109.5 . . ?
O2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O3 C9 H9A 109.5 . . ?
O3 C9 H9B 109.5 . . ?
O3 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C5 C10 H10A 108.8 . . ?
C5 C10 H10B 108.8 . . ?
C5 C10 C11 113.9(2) . . ?
H10A C10 H10B 107.7 . . ?
C11 C10 H10A 108.8 . . ?
C11 C10 H10B 108.8 . . ?
C12 C11 C10 122.9(3) . . ?
C12 C11 C14 114.7(3) . . ?
C14 C11 C10 122.4(2) . . ?
N1 C12 C11 122.4(3) . . ?
N1 C12 H12 118.8 . . ?
C11 C12 H12 118.8 . . ?
N2 C13 N1 117.7(2) . . ?
N2 C13 N3 120.8(3) . . ?
N3 C13 N1 121.5(3) . . ?
N3 C14 C11 122.9(2) . . ?
N4 C14 N3 116.7(3) . . ?
N4 C14 C11 120.4(3) . . ?
C15 O4 C21 117.5(3) . . ?
C16 O5 C22 112.4(2) . . ?
C17 O6 C23 117.2(3) . . ?
C26 N5 H5 120.2 . . ?
C27 N5 H5 120.2 . . ?
C27 N5 C26 119.7(3) . . ?
H6A N6 H6B 120.0 . . ?
C27 N6 H6A 120.0 . . ?
C27 N6 H6B 120.0 . . ?
C27 N7 C28 118.5(2) . . ?
H8D N8 H8E 120.0 . . ?
C28 N8 H8D 120.0 . . ?
C28 N8 H8E 120.0 . . ?
O4 C15 C16 115.1(3) . . ?
O4 C15 C20 124.7(3) . . ?
C16 C15 C20 120.2(3) . . ?
O5 C16 C15 120.4(3) . . ?
O5 C16 C17 120.0(3) . . ?
C15 C16 C17 119.6(3) . . ?
O6 C17 C16 115.1(3) . . ?
O6 C17 C18 124.7(3) . . ?
C18 C17 C16 120.1(3) . . ?
C17 C18 H18 119.9 . . ?
C17 C18 C19 120.1(3) . . ?
C19 C18 H18 119.9 . . ?
C18 C19 C24 118.6(3) . . ?
C20 C19 C18 119.7(3) . . ?
C20 C19 C24 121.7(3) . . ?
C15 C20 H20 119.9 . . ?
C19 C20 C15 120.2(3) . . ?
C19 C20 H20 119.9 . . ?
O4 C21 H21A 109.5 . . ?
O4 C21 H21B 109.5 . . ?
O4 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O5 C22 H22A 109.5 . . ?
O5 C22 H22B 109.5 . . ?
O5 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O6 C23 H23A 109.5 . . ?
O6 C23 H23B 109.5 . . ?
O6 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C19 C24 H24A 108.7 . . ?
C19 C24 H24B 108.7 . . ?
C19 C24 C25 114.2(3) . . ?
H24A C24 H24B 107.6 . . ?
C25 C24 H24A 108.7 . . ?
C25 C24 H24B 108.7 . . ?
C26 C25 C24 122.8(3) . . ?
C26 C25 C28 116.1(3) . . ?
C28 C25 C24 121.0(3) . . ?
N5 C26 H26 119.2 . . ?
C25 C26 N5 121.6(3) . . ?
C25 C26 H26 119.2 . . ?
N6 C27 N5 117.2(3) . . ?
N7 C27 N5 122.2(3) . . ?
N7 C27 N6 120.7(3) . . ?
N7 C28 C25 121.9(3) . . ?
N8 C28 N7 116.8(3) . . ?
N8 C28 C25 121.3(3) . . ?
C30 O9 H9 109.5 . . ?
O7 C29 O8 125.7(3) . . ?
O7 C29 C30 118.8(2) . . ?
O8 C29 C30 115.5(2) . . ?
O9 C30 C29 111.7(2) . . ?
O9 C30 H30 107.6 . . ?
O9 C30 C31 110.8(3) . . ?
C29 C30 H30 107.6 . . ?
C31 C30 C29 111.3(2) . . ?
C31 C30 H30 107.6 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33A O12A H12A 109.5 . . ?
O10A C32A C33A 115.5(5) . . ?
O11A C32A O10A 125.6(7) . . ?
O11A C32A C33A 118.7(7) . . ?
O12A C33A C32A 111.2(5) . . ?
O12A C33A H33A 107.9 . . ?
O12A C33A C34A 108.0(4) . . ?
C32A C33A H33A 107.9 . . ?
C34A C33A C32A 113.8(4) . . ?
C34A C33A H33A 107.9 . . ?
C33A C34A H34A 109.5 . . ?
C33A C34A H34B 109.5 . . ?
C33A C34A H34C 109.5 . . ?
H34A C34A H34B 109.5 . . ?
H34A C34A H34C 109.5 . . ?
H34B C34A H34C 109.5 . . ?
C33B O12B H12B 109.5 . . ?
O10B C32B O11B 124.8(7) . . ?
O10B C32B C33B 118.7(6) . . ?
O11B C32B C33B 116.5(4) . . ?
O12B C33B C32B 112.4(4) . . ?
O12B C33B H33B 108.8 . . ?
O12B C33B C34B 108.9(4) . . ?
C32B C33B H33B 108.8 . . ?
C32B C33B C34B 109.1(4) . . ?
C34B C33B H33B 108.8 . . ?
C33B C34B H34D 109.5 . . ?
C33B C34B H34E 109.5 . . ?
C33B C34B H34F 109.5 . . ?
H34D C34B H34E 109.5 . . ?
H34D C34B H34F 109.5 . . ?
H34E C34B H34F 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.364(4) . ?
O1 C7 1.423(4) . ?
O2 C2 1.381(4) . ?
O2 C8 1.439(4) . ?
O3 C3 1.362(4) . ?
O3 C9 1.427(4) . ?
N1 H1 0.8800 . ?
N1 C12 1.354(4) . ?
N1 C13 1.356(4) . ?
N2 H2A 0.8800 . ?
N2 H2B 0.8800 . ?
N2 C13 1.320(4) . ?
N3 C13 1.345(4) . ?
N3 C14 1.349(4) . ?
N4 H4A 0.8800 . ?
N4 H4B 0.8800 . ?
N4 C14 1.327(4) . ?
C1 C2 1.400(4) . ?
C1 C6 1.394(5) . ?
C2 C3 1.400(4) . ?
C3 C4 1.395(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.389(4) . ?
C5 C6 1.399(4) . ?
C5 C10 1.517(4) . ?
C6 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.518(4) . ?
C11 C12 1.357(4) . ?
C11 C14 1.438(4) . ?
C12 H12 0.9500 . ?
O4 C15 1.369(4) . ?
O4 C21 1.430(4) . ?
O5 C16 1.374(4) . ?
O5 C22 1.442(4) . ?
O6 C17 1.356(4) . ?
O6 C23 1.428(4) . ?
N5 H5 0.8800 . ?
N5 C26 1.370(5) . ?
N5 C27 1.355(4) . ?
N6 H6A 0.8800 . ?
N6 H6B 0.8800 . ?
N6 C27 1.334(4) . ?
N7 C27 1.330(4) . ?
N7 C28 1.348(4) . ?
N8 H8D 0.8800 . ?
N8 H8E 0.8800 . ?
N8 C28 1.332(4) . ?
C15 C16 1.391(4) . ?
C15 C20 1.394(5) . ?
C16 C17 1.399(4) . ?
C17 C18 1.386(5) . ?
C18 H18 0.9500 . ?
C18 C19 1.401(4) . ?
C19 C20 1.386(5) . ?
C19 C24 1.507(5) . ?
C20 H20 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.515(4) . ?
C25 C26 1.340(5) . ?
C25 C28 1.441(4) . ?
C26 H26 0.9500 . ?
O7 C29 1.241(4) . ?
O8 C29 1.275(4) . ?
O9 H9 0.8400 . ?
O9 C30 1.413(3) . ?
C29 C30 1.525(4) . ?
C30 H30 1.0000 . ?
C30 C31 1.514(5) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
O10A C32A 1.278(8) . ?
O11A C32A 1.223(13) . ?
O12A H12A 0.8400 . ?
O12A C33A 1.421(7) . ?
C32A C33A 1.557(8) . ?
C33A H33A 1.0000 . ?
C33A C34A 1.514(7) . ?
C34A H34A 0.9800 . ?
C34A H34B 0.9800 . ?
C34A H34C 0.9800 . ?
O10B C32B 1.256(11) . ?
O11B C32B 1.267(7) . ?
O12B H12B 0.8400 . ?
O12B C33B 1.418(6) . ?
C32B C33B 1.522(7) . ?
C33B H33B 1.0000 . ?
C33B C34B 1.533(8) . ?
C34B H34D 0.9800 . ?
C34B H34E 0.9800 . ?
C34B H34F 0.9800 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1 O7 0.88 2.65 3.314(3) 132.8 . yes
N1 H1 O8 0.88 1.78 2.640(3) 166.0 . yes
N2 H2A O11A 0.88 2.36 2.947(12) 124.5 1_655 yes
N2 H2A O10B 0.88 2.63 3.183(11) 121.5 1_655 yes
N2 H2A O11B 0.88 2.03 2.907(4) 174.4 1_655 yes
N2 H2B O7 0.88 2.07 2.878(3) 152.8 . yes
N4 H4A N7 0.88 2.15 3.002(4) 163.0 . yes
N4 H4B O9 0.88 2.00 2.758(4) 143.7 1_456 yes
N5 H5 O10A 0.88 1.74 2.590(5) 160.5 1_556 yes
N5 H5 O11A 0.88 2.57 3.276(9) 137.5 1_556 yes
N5 H5 O10B 0.88 2.24 2.947(9) 137.1 1_556 yes
N5 H5 O12B 0.88 2.29 3.071(5) 148.4 1_556 yes
N6 H6A O7 0.88 2.40 2.950(3) 121.1 1_456 yes
N6 H6B O11A 0.88 2.09 2.921(9) 156.2 1_556 yes
N6 H6B O10B 0.88 1.88 2.693(10) 152.0 1_556 yes
N8 H8D N3 0.88 2.19 3.038(4) 162.0 . yes
N8 H8E O12A 0.88 2.16 2.896(5) 140.7 1_655 yes
N8 H8E O11B 0.88 2.15 2.831(4) 134.3 1_655 yes
O9 H9 O8 0.84 1.93 2.723(3) 157.4 1_655 yes
O12A H12A O10A 0.84 1.97 2.763(7) 157.4 1_455 yes
O12B H12B O11B 0.84 1.92 2.751(5) 172.5 1_655 yes
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 O2 -1.6(4) . . . . ?
O1 C1 C2 C3 -178.5(2) . . . . ?
O1 C1 C6 C5 -179.8(3) . . . . ?
O2 C2 C3 O3 1.8(4) . . . . ?
O2 C2 C3 C4 -179.3(3) . . . . ?
O3 C3 C4 C5 -180.0(3) . . . . ?
C1 C2 C3 O3 178.7(3) . . . . ?
C1 C2 C3 C4 -2.4(4) . . . . ?
C2 C1 C6 C5 -0.1(4) . . . . ?
C2 C3 C4 C5 1.3(4) . . . . ?
C3 C4 C5 C6 0.4(4) . . . . ?
C3 C4 C5 C10 -179.9(3) . . . . ?
C4 C5 C6 C1 -1.0(4) . . . . ?
C4 C5 C10 C11 -83.1(3) . . . . ?
C5 C10 C11 C12 -32.8(4) . . . . ?
C5 C10 C11 C14 148.9(3) . . . . ?
C6 C1 C2 O2 178.7(3) . . . . ?
C6 C1 C2 C3 1.8(4) . . . . ?
C6 C5 C10 C11 96.6(3) . . . . ?
C7 O1 C1 C2 -175.9(3) . . . . ?
C7 O1 C1 C6 3.8(4) . . . . ?
C8 O2 C2 C1 105.9(3) . . . . ?
C8 O2 C2 C3 -77.2(3) . . . . ?
C9 O3 C3 C2 173.8(3) . . . . ?
C9 O3 C3 C4 -5.1(4) . . . . ?
C10 C5 C6 C1 179.3(3) . . . . ?
C10 C11 C12 N1 179.7(3) . . . . ?
C10 C11 C14 N3 -177.7(3) . . . . ?
C10 C11 C14 N4 0.8(4) . . . . ?
C12 N1 C13 N2 -175.3(3) . . . . ?
C12 N1 C13 N3 3.2(4) . . . . ?
C12 C11 C14 N3 3.8(4) . . . . ?
C12 C11 C14 N4 -177.6(3) . . . . ?
C13 N1 C12 C11 -1.5(4) . . . . ?
C13 N3 C14 N4 179.1(3) . . . . ?
C13 N3 C14 C11 -2.3(4) . . . . ?
C14 N3 C13 N1 -1.3(4) . . . . ?
C14 N3 C13 N2 177.2(3) . . . . ?
C14 C11 C12 N1 -1.9(4) . . . . ?
O4 C15 C16 O5 0.5(4) . . . . ?
O4 C15 C16 C17 178.8(3) . . . . ?
O4 C15 C20 C19 -179.5(3) . . . . ?
O5 C16 C17 O6 -1.0(4) . . . . ?
O5 C16 C17 C18 179.1(3) . . . . ?
O6 C17 C18 C19 179.8(3) . . . . ?
C15 C16 C17 O6 -179.3(3) . . . . ?
C15 C16 C17 C18 0.8(5) . . . . ?
C16 C15 C20 C19 -0.2(5) . . . . ?
C16 C17 C18 C19 -0.4(5) . . . . ?
C17 C18 C19 C20 -0.4(5) . . . . ?
C17 C18 C19 C24 179.0(3) . . . . ?
C18 C19 C20 C15 0.7(5) . . . . ?
C18 C19 C24 C25 83.2(4) . . . . ?
C19 C24 C25 C26 30.7(4) . . . . ?
C19 C24 C25 C28 -150.1(3) . . . . ?
C20 C15 C16 O5 -178.8(3) . . . . ?
C20 C15 C16 C17 -0.5(5) . . . . ?
C20 C19 C24 C25 -97.4(4) . . . . ?
C21 O4 C15 C16 176.7(3) . . . . ?
C21 O4 C15 C20 -4.0(4) . . . . ?
C22 O5 C16 C15 -104.1(3) . . . . ?
C22 O5 C16 C17 77.6(3) . . . . ?
C23 O6 C17 C16 -174.6(3) . . . . ?
C23 O6 C17 C18 5.3(5) . . . . ?
C24 C19 C20 C15 -178.7(3) . . . . ?
C24 C25 C26 N5 -179.2(3) . . . . ?
C24 C25 C28 N7 178.5(3) . . . . ?
C24 C25 C28 N8 -1.1(4) . . . . ?
C26 N5 C27 N6 177.0(3) . . . . ?
C26 N5 C27 N7 -2.7(4) . . . . ?
C26 C25 C28 N7 -2.2(4) . . . . ?
C26 C25 C28 N8 178.2(3) . . . . ?
C27 N5 C26 C25 0.8(5) . . . . ?
C27 N7 C28 N8 -179.9(3) . . . . ?
C27 N7 C28 C25 0.5(4) . . . . ?
C28 N7 C27 N5 2.0(4) . . . . ?
C28 N7 C27 N6 -177.7(3) . . . . ?
C28 C25 C26 N5 1.5(5) . . . . ?
O7 C29 C30 O9 3.1(4) . . . . ?
O7 C29 C30 C31 -121.2(3) . . . . ?
O8 C29 C30 O9 -177.4(3) . . . . ?
O8 C29 C30 C31 58.2(4) . . . . ?
O10A C32A C33A O12A 160.0(5) . . . . ?
O10A C32A C33A C34A 37.8(7) . . . . ?
O11A C32A C33A O12A -24.3(12) . . . . ?
O11A C32A C33A C34A -146.5(12) . . . . ?
O10B C32B C33B O12B 6.8(13) . . . . ?
O10B C32B C33B C34B -114.1(13) . . . . ?
O11B C32B C33B O12B -175.5(4) . . . . ?
O11B C32B C33B C34B 63.6(6) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 1.1(2)
2 -0.1(2)
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.1317 22.6510 1.8062 -0.5044 0.7338 0.4551
3.3058 0.5298 -0.8270 0.2323 -0.3365 0.9126
-2.6884 -13.4082 -0.3822 0.1057 -0.1548 -0.9823
-0.0013 1.0148 -1.9977 0.2809 0.1354 -0.0087
0.0013 -1.0148 1.9977 -0.2809 -0.1354 0.0087
2.1831 10.2160 -4.3658 0.6047 0.3295 0.7251
0.0614 -23.5260 0.6011 0.1690 -0.9071 -0.3856
-2.1556 -17.9236 0.2667 0.0786 -0.4175 -0.9053
0.1552 -16.6460 -4.6093 0.8592 -0.4090 -0.3075
