#------------------------------------------------------------------------------
#$Date: 2022-02-04 00:56:22 +0200 (Fri, 04 Feb 2022) $
#$Revision: 272499 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/96/7129657.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_7129657
loop_
_publ_author_name
'Fong, Angela'
'Cambell, Cameron'
'Huynh, Silvia'
'McCormick McPherson, Laura J.'
'Teat, Simon'
'Bebbington, Magnus W. P.'
'Dalgarno, Scott'
_publ_section_title
;
 Facile Synthetic Routes to Bridge-Functionalised Calix[4]arenes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06889J
_journal_year                    2022
_chemical_formula_moiety         '2(C68 H80 O12), 1.25(C8 H12 N4)'
_chemical_formula_sum            'C146 H175 N5 O24'
_chemical_formula_weight         2383.90
_space_group_crystal_system      tetragonal
_space_group_IT_number           100
_space_group_name_Hall           'P 4 -2ab'
_space_group_name_H-M_alt        'P 4 b m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2022-01-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-01-24 deposited with the CCDC.	2022-02-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   25.0238(7)
_cell_length_b                   25.0238(7)
_cell_length_c                   10.8155(6)
_cell_measurement_reflns_used    10082
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      26.7100
_cell_measurement_theta_min      3.4610
_cell_volume                     6772.6(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -88.00  19.00   1.00   10.00    --   -9.43 -19.00-120.00  107
  2  ω    -18.00  30.00   1.00   10.00    --   -9.43 -99.00 150.00   48
  3  ω    -44.00  -7.00   1.00   10.00    --   -9.43 100.00 177.14   37
  4  ω      5.00  56.00   1.00   10.00    --   10.84-127.00 127.00   51
  5  ω    -14.00  13.00   1.00   10.00    --   10.84  57.00  90.00   27
  6  ω     -1.00  25.00   1.00   10.00    --   10.84-122.00  11.80   26
  7  ω     48.00  75.00   1.00   10.00    --   10.84  19.00-120.00   27
  8  ω    -38.00 -11.00   1.00   10.00    --   10.84 -77.00  90.00   27
  9  ω     12.00  37.00   1.00   10.00    --   10.84 -57.00  90.00   25
 10  ω    -62.00 -25.00   1.00   10.00    --   10.84 -77.00   0.00   37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0011987000
_diffrn_orient_matrix_UB_12      -0.0273592000
_diffrn_orient_matrix_UB_13      -0.0169601000
_diffrn_orient_matrix_UB_21      0.0020463000
_diffrn_orient_matrix_UB_22      0.0072151000
_diffrn_orient_matrix_UB_23      -0.0632291000
_diffrn_orient_matrix_UB_31      0.0282488000
_diffrn_orient_matrix_UB_32      -0.0016622000
_diffrn_orient_matrix_UB_33      0.0038552000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0831
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            73696
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.996
_diffrn_reflns_theta_min         2.935
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.519
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_description       block
_exptl_crystal_F_000             2556
_exptl_crystal_size_max          0.383
_exptl_crystal_size_mid          0.295
_exptl_crystal_size_min          0.161
_refine_diff_density_max         0.217
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Flack x determined using 2423 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.1(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         7480
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0328P)²+2.6835P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1046
_reflns_Friedel_coverage         0.860
_reflns_Friedel_fraction_full    0.966
_reflns_Friedel_fraction_max     0.956
_reflns_number_gt                6635
_reflns_number_total             7480
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1cc06889j2.cif
_cod_data_source_block           2
_cod_database_code               7129657
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C68 H80 O12'
_chemical_oxdiff_usercomment     '@ 120 K AF148'
_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.
;
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Sof: C32(0.5) H32A(0.5) H32B(0.5) H32C(0.5) C33(0.5) H33A(0.5)
 H33B(0.5) H33C(0.5) C34(0.5) H34A(0.5) H34B(0.5) H34C(0.5) H35A(0.5) H35B(0.5)
 H35C(0.5) H36A(0.5) H36B(0.5) H36C(0.5) C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5)
 C29(0.5) H29A(0.5) H29B(0.5) H29C(0.5) C30(0.5) H30A(0.5) H30B(0.5) H30C(0.5)
 H42A(0.25) H42B(0.25) H42C(0.25) H44A(0.5) H44B(0.5) H44C(0.5) N3(0.5)
 C46(0.5) H46A(0.5) H46B(0.5) H46C(0.5) C47(0.5)
2.a Everything fixed:
 H42A, H42B, H42C
2.b Ternary CH refined with riding coordinates:
 C7(H7), C22(H22)
2.c Me refined with riding coordinates:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
2.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C14(H14), C15(H15), C19(H19), C24(H24), C38(H38), C39(H39)
2.e Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C17(H17A,H17B,H17C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C41(H41A,
 H41B,H41C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C44(H44A,H44B,H44C), C46(H46A,H46B,H46C)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.312
_oxdiff_exptl_absorpt_empirical_full_min 0.797
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+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 0.49885(8) 0.41493(8) 0.6746(2) 0.0208(4) Uani 1 1 d . . . . .
O2 O 0.35866(9) 0.31369(8) 0.5167(2) 0.0298(5) Uani 1 1 d . . . . .
O3 O 0.36662(9) 0.33328(9) 0.8063(2) 0.0335(6) Uani 1 1 d . . . . .
C1 C 0.54738(11) 0.37941(10) 0.5014(3) 0.0170(6) Uani 1 1 d . . . . .
C2 C 0.54652(11) 0.35710(11) 0.3841(3) 0.0196(6) Uani 1 1 d . . . . .
H2 H 0.5788 0.3480 0.3470 0.024 Uiso 1 1 calc R U . . .
C3 C 0.49932(12) 0.34777(11) 0.3195(3) 0.0183(6) Uani 1 1 d . . . . .
C4 C 0.45153(11) 0.36082(11) 0.3796(3) 0.0189(6) Uani 1 1 d . . . . .
H4 H 0.4194 0.3555 0.3382 0.023 Uiso 1 1 calc R U . . .
C5 C 0.45033(11) 0.38159(10) 0.4995(3) 0.0175(6) Uani 1 1 d . . . . .
C6 C 0.49877(12) 0.39044(11) 0.5603(3) 0.0174(6) Uani 1 1 d . . . . .
C7 C 0.39857(11) 0.39997(11) 0.5598(3) 0.0184(6) Uani 1 1 d . . . . .
H7 H 0.4070 0.4078 0.6464 0.022 Uiso 1 1 calc R U . . .
C8 C 0.50071(12) 0.32481(12) 0.1876(3) 0.0234(7) Uani 1 1 d . . . . .
C9 C 0.54387(14) 0.35291(15) 0.1109(3) 0.0349(8) Uani 1 1 d . . . . .
H9A H 0.5375 0.3907 0.1111 0.052 Uiso 1 1 calc R U . . .
H9B H 0.5428 0.3398 0.0275 0.052 Uiso 1 1 calc R U . . .
H9C H 0.5784 0.3458 0.1461 0.052 Uiso 1 1 calc R U . . .
C10 C 0.44752(14) 0.33280(15) 0.1198(3) 0.0340(8) Uani 1 1 d . . . . .
H10A H 0.4198 0.3137 0.1624 0.051 Uiso 1 1 calc R U . . .
H10B H 0.4506 0.3195 0.0368 0.051 Uiso 1 1 calc R U . . .
H10C H 0.4389 0.3702 0.1176 0.051 Uiso 1 1 calc R U . . .
C11 C 0.51413(15) 0.26523(13) 0.1935(3) 0.0355(9) Uani 1 1 d . . . . .
H11A H 0.5475 0.2604 0.2359 0.053 Uiso 1 1 calc R U . . .
H11B H 0.5170 0.2512 0.1111 0.053 Uiso 1 1 calc R U . . .
H11C H 0.4864 0.2467 0.2371 0.053 Uiso 1 1 calc R U . . .
C12 C 0.50037(14) 0.37971(14) 0.7786(3) 0.0305(8) Uani 1 1 d . . . . .
H12A H 0.5307 0.3564 0.7716 0.046 Uiso 1 1 calc R U . . .
H12B H 0.4682 0.3589 0.7809 0.046 Uiso 1 1 calc R U . . .
H12C H 0.5033 0.4003 0.8533 0.046 Uiso 1 1 calc R U . . .
C13 C 0.35428(12) 0.35805(12) 0.5607(3) 0.0233(7) Uani 1 1 d . . . . .
C14 C 0.30191(12) 0.37615(12) 0.6148(4) 0.0291(8) Uani 1 1 d . . . . .
H14 H 0.2782 0.3933 0.5619 0.035 Uiso 1 1 calc R U . . .
C15 C 0.28656(13) 0.36976(12) 0.7314(4) 0.0305(8) Uani 1 1 d . . . . .
H15 H 0.2526 0.3815 0.7534 0.037 Uiso 1 1 calc R U . . .
C16 C 0.32007(14) 0.34517(12) 0.8278(4) 0.0294(8) Uani 1 1 d . . . . .
C17 C 0.29514(17) 0.33584(17) 0.9517(4) 0.0476(10) Uani 1 1 d . . . . .
H17A H 0.2693 0.3076 0.9455 0.071 Uiso 1 1 calc R U . . .
H17B H 0.2778 0.3679 0.9790 0.071 Uiso 1 1 calc R U . . .
H17C H 0.3223 0.3260 1.0101 0.071 Uiso 1 1 calc R U . . .
O4 O 0.07545(8) 0.42455(8) 0.6421(3) 0.0176(6) Uani 1 2 d S T P . .
O5 O 0.04758(8) 0.54758(8) 0.6058(3) 0.0185(6) Uani 1 2 d S T P . .
O6 O 0.21900(8) 0.44882(9) 0.4670(2) 0.0292(5) Uani 1 1 d . . . . .
O7 O 0.19711(10) 0.47999(10) 0.7780(2) 0.0369(6) Uani 1 1 d . . . . .
C18 C 0.12547(10) 0.55702(10) 0.4786(3) 0.0141(6) Uani 1 1 d . . . . .
C19 C 0.15310(11) 0.58565(11) 0.3893(3) 0.0167(6) Uani 1 1 d . . . . .
H19 H 0.1850 0.5719 0.3588 0.020 Uiso 1 1 calc R U . . .
C20 C 0.13461(11) 0.63461(11) 0.3436(4) 0.0171(9) Uani 1 2 d S T P D .
C21 C 0.07783(10) 0.57783(10) 0.5249(4) 0.0163(9) Uani 1 2 d S T P . .
C22 C 0.14162(10) 0.50081(11) 0.5189(3) 0.0170(6) Uani 1 1 d . . . . .
H22 H 0.1316 0.4976 0.6062 0.020 Uiso 1 1 calc R U . . .
C23 C 0.10862(10) 0.45954(10) 0.4494(3) 0.0151(6) Uani 1 1 d . . . . .
C24 C 0.10957(11) 0.45752(11) 0.3214(3) 0.0190(6) Uani 1 1 d . . . . .
H24 H 0.1323 0.4805 0.2788 0.023 Uiso 1 1 calc R U . . .
C25 C 0.07773(11) 0.42227(11) 0.2542(4) 0.0209(9) Uani 1 2 d S T P A .
C26 C 0.07520(10) 0.42480(10) 0.5132(4) 0.0148(8) Uani 1 2 d S T P . .
C27 C 0.16460(12) 0.66460(12) 0.2419(4) 0.0221(9) Uani 1 2 d S T P . .
C31 C 0.08197(14) 0.41803(14) 0.1133(5) 0.0290(11) Uani 1 2 d S T P . .
C32 C 0.0227(6) 0.4154(6) 0.0558(14) 0.063(4) Uani 0.5 1 d . . P A -1
H32A H 0.0060 0.4498 0.0628 0.094 Uiso 0.5 1 calc R U P A -1
H32B H 0.0248 0.4054 -0.0298 0.094 Uiso 0.5 1 calc R U P A -1
H32C H 0.0020 0.3893 0.0999 0.094 Uiso 0.5 1 calc R U P A -1
C33 C 0.0387(5) 0.3900(5) 0.0540(12) 0.042(3) Uani 0.5 1 d . . P A -1
H33A H 0.0446 0.3893 -0.0337 0.062 Uiso 0.5 1 calc R U P A -1
H33B H 0.0370 0.3541 0.0849 0.062 Uiso 0.5 1 calc R U P A -1
H33C H 0.0056 0.4080 0.0712 0.062 Uiso 0.5 1 calc R U P A -1
C34 C 0.1071(4) 0.3619(3) 0.0824(8) 0.060(3) Uani 0.5 1 d . . P A -1
H34A H 0.1435 0.3610 0.1103 0.091 Uiso 0.5 1 calc R U P A -1
H34B H 0.0871 0.3344 0.1235 0.091 Uiso 0.5 1 calc R U P A -1
H34C H 0.1060 0.3561 -0.0053 0.091 Uiso 0.5 1 calc R U P A -1
C35 C 0.05748(14) 0.55748(14) 0.7337(4) 0.0293(11) Uani 1 2 d S T P . .
H35A H 0.0635 0.5950 0.7461 0.044 Uiso 0.5 1 calc R U P B -1
H35B H 0.0885 0.5378 0.7595 0.044 Uiso 0.5 1 calc R U P B -1
H35C H 0.0271 0.5463 0.7814 0.044 Uiso 0.5 1 calc R U P B -1
C36 C 0.11353(12) 0.38647(12) 0.6897(4) 0.0236(10) Uani 1 2 d S T P . .
H36A H 0.1100 0.3533 0.6459 0.035 Uiso 0.5 1 calc R U P C -1
H36B H 0.1069 0.3807 0.7761 0.035 Uiso 0.5 1 calc R U P C -1
H36C H 0.1491 0.4001 0.6789 0.035 Uiso 0.5 1 calc R U P C -1
C37 C 0.20164(11) 0.48950(11) 0.5123(3) 0.0204(6) Uani 1 1 d . . . . .
C38 C 0.23912(12) 0.53129(13) 0.5594(3) 0.0267(8) Uani 1 1 d . . . . .
H38 H 0.2607 0.5478 0.5006 0.032 Uiso 1 1 calc R U . . .
C39 C 0.24522(12) 0.54745(13) 0.6747(4) 0.0308(8) Uani 1 1 d . . . . .
H39 H 0.2698 0.5745 0.6903 0.037 Uiso 1 1 calc R U . . .
C40 C 0.21509(13) 0.52501(13) 0.7808(3) 0.0291(8) Uani 1 1 d . . . . .
C41 C 0.20747(16) 0.56102(15) 0.8893(4) 0.0435(9) Uani 1 1 d . . . . .
H41A H 0.1929 0.5410 0.9570 0.065 Uiso 1 1 calc R U . . .
H41B H 0.1833 0.5893 0.8675 0.065 Uiso 1 1 calc R U . . .
H41C H 0.2413 0.5759 0.9131 0.065 Uiso 1 1 calc R U . . .
C28 C 0.1405(3) 0.7186(3) 0.2083(7) 0.0297(16) Uani 0.5 1 d . . P D -1
H28A H 0.1047 0.7136 0.1786 0.045 Uiso 0.5 1 calc R U P D -1
H28B H 0.1617 0.7352 0.1450 0.045 Uiso 0.5 1 calc R U P D -1
H28C H 0.1398 0.7411 0.2802 0.045 Uiso 0.5 1 calc R U P D -1
C29 C 0.1649(3) 0.6285(3) 0.1257(6) 0.0336(16) Uani 0.5 1 d . . P D -1
H29A H 0.1813 0.5949 0.1453 0.050 Uiso 0.5 1 calc R U P D -1
H29B H 0.1846 0.6458 0.0609 0.050 Uiso 0.5 1 calc R U P D -1
H29C H 0.1288 0.6225 0.0988 0.050 Uiso 0.5 1 calc R U P D -1
C30 C 0.2233(3) 0.6743(3) 0.2821(8) 0.0363(18) Uani 0.5 1 d . . P D -1
H30A H 0.2240 0.6985 0.3510 0.054 Uiso 0.5 1 calc R U P D -1
H30B H 0.2430 0.6895 0.2144 0.054 Uiso 0.5 1 calc R U P D -1
H30C H 0.2393 0.6410 0.3057 0.054 Uiso 0.5 1 calc R U P D -1
N1 N 0.5000 0.5000 0.0769(9) 0.079(3) Uani 1 4 d S T P . .
C42 C 0.5000 0.5000 0.3152(7) 0.0327(16) Uani 1 4 d S T P . .
C43 C 0.5000 0.5000 0.1830(9) 0.0398(18) Uani 1 4 d S T P . .
H42A H 0.4906 0.5349 0.3448 0.060 Uiso 0.25 1 d . U P E -1
H42B H 0.4745 0.4744 0.3448 0.060 Uiso 0.25 1 d . U P F -1
H42C H 0.5349 0.4907 0.3448 0.060 Uiso 0.25 1 d . U P G -1
N2 N 0.79120(16) 0.29120(16) 0.8441(5) 0.0560(14) Uani 1 2 d S T P . .
C44 C 0.80604(17) 0.30604(17) 0.6105(6) 0.0441(14) Uani 1 2 d S T P . .
H44A H 0.8082 0.2721 0.5693 0.066 Uiso 0.5 1 calc R U P H -1
H44B H 0.8387 0.3254 0.5982 0.066 Uiso 0.5 1 calc R U P H -1
H44C H 0.7768 0.3262 0.5771 0.066 Uiso 0.5 1 calc R U P H -1
C45 C 0.79762(14) 0.29762(14) 0.7416(6) 0.0346(12) Uani 1 2 d S T P . .
N3 N 0.2696(4) 0.3393(3) 0.2708(9) 0.069(2) Uani 0.5 1 d . . P I -1
C46 C 0.1844(15) 0.3224(15) 0.3965(8) 0.054(6) Uani 0.5 1 d . . P I -1
H46A H 0.1595 0.3006 0.3515 0.082 Uiso 0.5 1 calc R U P I -1
H46B H 0.1682 0.3562 0.4150 0.082 Uiso 0.5 1 calc R U P I -1
H46C H 0.1940 0.3047 0.4722 0.082 Uiso 0.5 1 calc R U P I -1
C47 C 0.2311(4) 0.3306(3) 0.3235(9) 0.046(2) Uani 0.5 1 d . . P I -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
33 13 2 0.1701
2 -35 -2 0.0742
1 35 2 0.0755
35 -1 -2 0.2032
32 -5 6 0.2084
1 -8 15 0.1336
-35 2 0 0.1707
0 8 -15 0.1414
2 6 15 0.1382
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
C6 O1 C12 115.6(2) . . ?
C2 C1 C6 118.8(3) . . ?
C2 C1 C7 121.0(3) . 3_655 ?
C6 C1 C7 119.7(3) . 3_655 ?
C1 C2 H2 118.7 . . ?
C1 C2 C3 122.7(3) . . ?
C3 C2 H2 118.7 . . ?
C2 C3 C4 117.0(3) . . ?
C2 C3 C8 120.6(3) . . ?
C4 C3 C8 122.5(3) . . ?
C3 C4 H4 118.8 . . ?
C5 C4 C3 122.4(3) . . ?
C5 C4 H4 118.8 . . ?
C4 C5 C7 121.9(3) . . ?
C6 C5 C4 118.5(3) . . ?
C6 C5 C7 119.3(3) . . ?
O1 C6 C1 119.6(3) . . ?
O1 C6 C5 119.6(3) . . ?
C5 C6 C1 120.6(3) . . ?
C1 C7 H7 106.7 4_565 . ?
C5 C7 C1 110.4(2) . 4_565 ?
C5 C7 H7 106.7 . . ?
C5 C7 C13 114.4(2) . . ?
C13 C7 C1 111.4(2) . 4_565 ?
C13 C7 H7 106.7 . . ?
C9 C8 C3 110.3(3) . . ?
C9 C8 C10 107.0(3) . . ?
C10 C8 C3 112.1(3) . . ?
C11 C8 C3 109.3(3) . . ?
C11 C8 C9 108.4(3) . . ?
C11 C8 C10 109.7(3) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O1 C12 H12A 109.5 . . ?
O1 C12 H12B 109.5 . . ?
O1 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O2 C13 C7 124.1(3) . . ?
O2 C13 C14 120.4(3) . . ?
C14 C13 C7 115.3(3) . . ?
C13 C14 H14 117.1 . . ?
C15 C14 C13 125.8(3) . . ?
C15 C14 H14 117.1 . . ?
C14 C15 H15 118.0 . . ?
C14 C15 C16 123.9(3) . . ?
C16 C15 H15 118.0 . . ?
O3 C16 C15 120.5(3) . . ?
O3 C16 C17 122.0(3) . . ?
C15 C16 C17 117.5(3) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C26 O4 C36 111.3(3) . . ?
C21 O5 C35 115.0(3) . . ?
C19 C18 C21 118.9(3) . . ?
C19 C18 C22 122.9(2) . . ?
C21 C18 C22 117.9(2) . . ?
C18 C19 H19 118.9 . . ?
C18 C19 C20 122.2(3) . . ?
C20 C19 H19 118.9 . . ?
C19 C20 C19 117.0(4) . 8_455 ?
C19 C20 C27 121.43(19) 8_455 . ?
C19 C20 C27 121.43(19) . . ?
C19 C20 C27 121.43(19) . 8_455 ?
C19 C20 C27 121.43(19) 8_455 8_455 ?
C27 C20 C27 0.0(3) . 8_455 ?
O5 C21 C18 119.41(18) . . ?
O5 C21 C18 119.41(18) . 8_455 ?
C18 C21 C18 120.7(4) . 8_455 ?
C18 C22 H22 106.4 . . ?
C18 C22 C37 114.6(2) . . ?
C23 C22 C18 109.9(2) . . ?
C23 C22 H22 106.4 . . ?
C23 C22 C37 112.6(2) . . ?
C37 C22 H22 106.4 . . ?
C24 C23 C22 120.6(3) . . ?
C24 C23 C26 118.9(3) . . ?
C26 C23 C22 120.4(3) . . ?
C23 C24 H24 118.8 . . ?
C23 C24 C25 122.3(3) . . ?
C25 C24 H24 118.8 . . ?
C24 C25 C24 116.9(4) . 7 ?
C24 C25 C31 121.6(2) . . ?
C24 C25 C31 121.6(2) 7 . ?
C23 C26 O4 119.76(19) . . ?
C23 C26 O4 119.76(19) 7 . ?
C23 C26 C23 120.5(4) . 7 ?
C20 C27 C29 107.5(4) . . ?
C20 C27 C29 107.5(4) . 8_455 ?
C20 C27 C30 109.9(4) . . ?
C20 C27 C30 109.9(4) . 8_455 ?
C27 C27 C20 0(10) 8_455 . ?
C27 C27 C28 0(10) 8_455 . ?
C27 C27 C28 0(10) 8_455 8_455 ?
C27 C27 C29 0(10) 8_455 . ?
C27 C27 C29 0(10) 8_455 8_455 ?
C27 C27 C30 0(10) 8_455 . ?
C27 C27 C30 0(10) 8_455 8_455 ?
C28 C27 C20 114.3(3) 8_455 . ?
C28 C27 C20 114.3(3) . . ?
C28 C27 C28 130.3(6) 8_455 . ?
C28 C27 C29 109.0(5) . . ?
C28 C27 C29 64.6(4) 8_455 . ?
C28 C27 C29 64.6(4) . 8_455 ?
C28 C27 C29 109.0(5) 8_455 8_455 ?
C28 C27 C30 44.7(4) . 8_455 ?
C28 C27 C30 44.7(4) 8_455 . ?
C28 C27 C30 107.7(5) . . ?
C28 C27 C30 107.7(5) 8_455 8_455 ?
C29 C27 C29 49.1(6) . 8_455 ?
C29 C27 C30 141.2(5) . 8_455 ?
C29 C27 C30 141.2(5) 8_455 . ?
C29 C27 C30 108.3(5) . . ?
C29 C27 C30 108.3(5) 8_455 8_455 ?
C30 C27 C30 68.0(6) 8_455 . ?
C25 C31 C32 108.9(6) . . ?
C25 C31 C34 107.5(4) . 7 ?
C25 C31 C34 107.5(4) . . ?
C33 C31 C25 115.1(5) . . ?
C33 C31 C32 27.7(6) . . ?
C33 C31 C34 112.5(6) . 7 ?
C33 C31 C34 76.8(6) . . ?
C34 C31 C32 136.3(7) 7 . ?
C34 C31 C32 104.4(7) . . ?
C34 C31 C34 40.7(7) . 7 ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O5 C35 H35A 109.5 . . ?
O5 C35 H35B 109.5 . . ?
O5 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
O4 C36 H36A 109.5 . . ?
O4 C36 H36B 109.5 . . ?
O4 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O6 C37 C22 121.8(3) . . ?
O6 C37 C38 120.1(3) . . ?
C38 C37 C22 118.1(3) . . ?
C37 C38 H38 116.2 . . ?
C39 C38 C37 127.5(3) . . ?
C39 C38 H38 116.2 . . ?
C38 C39 H39 118.1 . . ?
C38 C39 C40 123.8(3) . . ?
C40 C39 H39 118.1 . . ?
O7 C40 C39 121.4(3) . . ?
O7 C40 C41 122.2(3) . . ?
C39 C40 C41 116.4(3) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C27 C28 C27 0.0(3) 8_455 . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28A 109.5 8_455 . ?
C27 C28 H28B 109.5 8_455 . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 8_455 . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C43 C42 H42A 109.4 . . ?
C43 C42 H42B 109.4 . . ?
C43 C42 H42C 109.4 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N1 C43 C42 180.0 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C45 C44 H44A 109.5 . . ?
C45 C44 H44B 109.5 . . ?
C45 C44 H44C 109.5 . . ?
N2 C45 C44 179.7(8) . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C47 C46 H46A 109.5 . . ?
C47 C46 H46B 109.5 . . ?
C47 C46 H46C 109.5 . . ?
N3 C47 C46 175.7(18) . . ?
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 C6 1.380(4) . ?
O1 C12 1.429(4) . ?
O2 C13 1.213(4) . ?
O3 C16 1.225(4) . ?
C1 C2 1.386(5) . ?
C1 C6 1.401(4) . ?
C1 C7 1.538(4) 3_655 ?
C2 H2 0.9300 . ?
C2 C3 1.392(4) . ?
C3 C4 1.400(4) . ?
C3 C8 1.539(5) . ?
C4 H4 0.9300 . ?
C4 C5 1.398(5) . ?
C5 C6 1.396(4) . ?
C5 C7 1.521(4) . ?
C7 C1 1.538(4) 4_565 ?
C7 H7 0.9800 . ?
C7 C13 1.526(4) . ?
C8 C9 1.533(5) . ?
C8 C10 1.533(4) . ?
C8 C11 1.529(4) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.505(5) . ?
C14 H14 0.9300 . ?
C14 C15 1.328(5) . ?
C15 H15 0.9300 . ?
C15 C16 1.473(5) . ?
C16 C17 1.496(5) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
O4 C26 1.394(5) . ?
O4 C36 1.443(5) . ?
O5 C21 1.382(5) . ?
O5 C35 1.427(6) . ?
O6 C37 1.210(4) . ?
O7 C40 1.213(4) . ?
C18 C19 1.387(4) . ?
C18 C21 1.394(3) . ?
C18 C22 1.527(4) . ?
C19 H19 0.9300 . ?
C19 C20 1.400(3) . ?
C20 C19 1.400(4) 8_455 ?
C20 C27 1.529(6) 8_455 ?
C20 C27 1.529(6) . ?
C21 C18 1.394(3) 8_455 ?
C22 H22 0.9800 . ?
C22 C23 1.521(4) . ?
C22 C37 1.530(4) . ?
C23 C24 1.386(4) . ?
C23 C26 1.389(3) . ?
C24 H24 0.9300 . ?
C24 C25 1.393(4) . ?
C25 C24 1.393(4) 7 ?
C25 C31 1.531(7) . ?
C26 C23 1.389(3) 7 ?
C27 C27 0.000(12) 8_455 ?
C27 C28 1.524(6) . ?
C27 C28 1.524(6) 8_455 ?
C27 C29 1.547(8) . ?
C27 C29 1.547(8) 8_455 ?
C27 C30 1.552(8) . ?
C27 C30 1.552(8) 8_455 ?
C31 C32 1.609(14) . ?
C31 C33 1.441(13) . ?
C31 C34 1.574(9) . ?
C31 C34 1.574(9) 7 ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 C38 1.494(4) . ?
C38 H38 0.9300 . ?
C38 C39 1.320(5) . ?
C39 H39 0.9300 . ?
C39 C40 1.484(5) . ?
C40 C41 1.491(5) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C28 C27 1.524(6) 8_455 ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
N1 C43 1.147(12) . ?
C42 C43 1.430(13) . ?
C42 H42A 0.9597 . ?
C42 H42B 0.9597 . ?
C42 H42C 0.9598 . ?
N2 C45 1.132(7) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C44 C45 1.449(9) . ?
N3 C47 1.141(11) . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C46 C47 1.43(4) . ?
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
O2 C13 C14 C15 89.3(4) . . . . ?
C1 C2 C3 C4 -1.5(4) . . . . ?
C1 C2 C3 C8 177.7(3) . . . . ?
C1 C7 C13 O2 125.4(3) 4_565 . . . ?
C1 C7 C13 C14 -51.3(4) 4_565 . . . ?
C2 C1 C6 O1 -177.0(2) . . . . ?
C2 C1 C6 C5 -3.1(4) . . . . ?
C2 C3 C4 C5 -0.9(4) . . . . ?
C2 C3 C8 C9 -44.1(4) . . . . ?
C2 C3 C8 C10 -163.2(3) . . . . ?
C2 C3 C8 C11 74.9(3) . . . . ?
C3 C4 C5 C6 1.1(4) . . . . ?
C3 C4 C5 C7 174.8(3) . . . . ?
C4 C3 C8 C9 135.1(3) . . . . ?
C4 C3 C8 C10 16.0(4) . . . . ?
C4 C3 C8 C11 -105.9(3) . . . . ?
C4 C5 C6 O1 174.8(2) . . . . ?
C4 C5 C6 C1 0.9(4) . . . . ?
C4 C5 C7 C1 -72.5(3) . . . 4_565 ?
C4 C5 C7 C13 54.2(4) . . . . ?
C5 C7 C13 O2 -0.7(5) . . . . ?
C5 C7 C13 C14 -177.4(3) . . . . ?
C6 C1 C2 C3 3.5(4) . . . . ?
C6 C5 C7 C1 101.1(3) . . . 4_565 ?
C6 C5 C7 C13 -132.3(3) . . . . ?
C7 C1 C2 C3 -168.7(3) 3_655 . . . ?
C7 C1 C6 O1 -4.8(4) 3_655 . . . ?
C7 C1 C6 C5 169.1(2) 3_655 . . . ?
C7 C5 C6 O1 1.0(4) . . . . ?
C7 C5 C6 C1 -172.9(2) . . . . ?
C7 C13 C14 C15 -93.8(4) . . . . ?
C8 C3 C4 C5 179.9(3) . . . . ?
C12 O1 C6 C1 -90.0(3) . . . . ?
C12 O1 C6 C5 96.1(3) . . . . ?
C13 C14 C15 C16 2.3(5) . . . . ?
C14 C15 C16 O3 6.3(5) . . . . ?
C14 C15 C16 C17 -174.0(3) . . . . ?
O6 C37 C38 C39 -115.3(4) . . . . ?
C18 C19 C20 C19 -1.9(6) . . . 8_455 ?
C18 C19 C20 C27 -177.8(3) . . . . ?
C18 C19 C20 C27 -177.8(3) . . . 8_455 ?
C18 C22 C23 C24 58.7(3) . . . . ?
C18 C22 C23 C26 -118.4(3) . . . . ?
C18 C22 C37 O6 -133.8(3) . . . . ?
C18 C22 C37 C38 44.0(4) . . . . ?
C19 C18 C21 O5 174.4(3) . . . . ?
C19 C18 C21 C18 2.7(5) . . . 8_455 ?
C19 C18 C22 C23 -96.7(3) . . . . ?
C19 C18 C22 C37 31.3(4) . . . . ?
C19 C20 C27 C27 0(100) . . . 8_455 ?
C19 C20 C27 C27 0(100) 8_455 . . 8_455 ?
C19 C20 C27 C28 -176.9(5) . . . . ?
C19 C20 C27 C28 7.5(6) 8_455 . . . ?
C19 C20 C27 C28 -7.5(6) . . . 8_455 ?
C19 C20 C27 C28 176.9(5) 8_455 . . 8_455 ?
C19 C20 C27 C29 -62.0(5) 8_455 . . 8_455 ?
C19 C20 C27 C29 62.0(5) . . . . ?
C19 C20 C27 C29 113.7(4) . . . 8_455 ?
C19 C20 C27 C29 -113.7(4) 8_455 . . . ?
C19 C20 C27 C30 -128.6(4) . . . 8_455 ?
C19 C20 C27 C30 55.7(5) 8_455 . . 8_455 ?
C19 C20 C27 C30 -55.7(5) . . . . ?
C19 C20 C27 C30 128.6(4) 8_455 . . . ?
C20 C27 C28 C27 0(100) . . . 8_455 ?
C21 C18 C19 C20 -0.4(5) . . . . ?
C21 C18 C22 C23 76.6(3) . . . . ?
C21 C18 C22 C37 -155.4(3) . . . . ?
C22 C18 C19 C20 172.9(3) . . . . ?
C22 C18 C21 O5 0.8(5) . . . . ?
C22 C18 C21 C18 -170.9(2) . . . 8_455 ?
C22 C23 C24 C25 -176.4(3) . . . . ?
C22 C23 C26 O4 -5.7(5) . . . . ?
C22 C23 C26 C23 172.5(2) . . . 7 ?
C22 C37 C38 C39 66.9(4) . . . . ?
C23 C22 C37 O6 -7.2(4) . . . . ?
C23 C22 C37 C38 170.6(3) . . . . ?
C23 C24 C25 C24 3.0(6) . . . 7 ?
C23 C24 C25 C31 -175.9(3) . . . . ?
C24 C23 C26 O4 177.1(3) . . . . ?
C24 C23 C26 C23 -4.7(5) . . . 7 ?
C24 C25 C31 C32 44.5(7) 7 . . . ?
C24 C25 C31 C32 -136.6(6) . . . . ?
C24 C25 C31 C33 15.3(7) 7 . . . ?
C24 C25 C31 C33 -165.8(6) . . . . ?
C24 C25 C31 C34 110.9(5) . . . . ?
C24 C25 C31 C34 -110.9(5) 7 . . 7 ?
C24 C25 C31 C34 68.1(5) . . . 7 ?
C24 C25 C31 C34 -68.1(5) 7 . . . ?
C26 C23 C24 C25 0.7(5) . . . . ?
C27 C20 C27 C28 0(100) 8_455 . . . ?
C27 C20 C27 C28 0(100) 8_455 . . 8_455 ?
C27 C20 C27 C29 0(100) 8_455 . . . ?
C27 C20 C27 C29 0(100) 8_455 . . 8_455 ?
C27 C20 C27 C30 0(100) 8_455 . . 8_455 ?
C27 C20 C27 C30 0(100) 8_455 . . . ?
C35 O5 C21 C18 -94.1(3) . . . 8_455 ?
C35 O5 C21 C18 94.1(3) . . . . ?
C36 O4 C26 C23 90.9(3) . . . 7 ?
C36 O4 C26 C23 -90.9(3) . . . . ?
C37 C22 C23 C24 -70.4(3) . . . . ?
C37 C22 C23 C26 112.4(3) . . . . ?
C37 C38 C39 C40 1.1(5) . . . . ?
C38 C39 C40 O7 25.5(5) . . . . ?
C38 C39 C40 C41 -153.5(3) . . . . ?
C28 C27 C28 C27 0(100) 8_455 . . 8_455 ?
C29 C27 C28 C27 0(100) . . . 8_455 ?
C29 C27 C28 C27 0(100) 8_455 . . 8_455 ?
C30 C27 C28 C27 0(100) 8_455 . . 8_455 ?
C30 C27 C28 C27 0(100) . . . 8_455 ?
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
32.7141 12.6258 1.6247 -0.4122 0.0553 0.9094
1.7980 -34.9614 -1.8900 0.9864 -0.1291 0.1016
0.5670 34.9812 1.9579 -0.9909 0.1298 -0.0346
35.0698 -0.7398 -1.6142 0.0056 0.1685 0.9857
32.2254 -4.7706 5.8565 -0.0074 -0.3388 0.9408
1.0807 -8.3081 14.8157 -0.0253 -0.9945 0.1015
-35.2316 1.7438 -0.1736 -0.0025 -0.0485 -0.9988
-0.0434 8.2661 -14.8274 0.0254 0.9971 -0.0721
2.0186 6.0198 15.0032 -0.4216 -0.9011 0.1049
