#------------------------------------------------------------------------------
#$Date: 2024-05-05 05:18:51 +0300 (Sun, 05 May 2024) $
#$Revision: 291597 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/82/7248226.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_7248226
loop_
_publ_author_name
'Cheret, Yohan'
'Avarvari, Narcis'
'Zigon, Nicolas'
_publ_section_title
;
 Metal--organic polyhedron from a flexible
 tetrakis(thiobenzyl-carboxylate)-tetrathiafulvalene
;
_journal_issue                   15
_journal_name_full               CrystEngComm
_journal_page_first              2072
_journal_page_last               2077
_journal_paper_doi               10.1039/D3CE01251D
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety
'C152 H96 Cu8 O40 S32, 0.25(C6 H14 N2 O2), 0.66(C3 N O)'
_chemical_formula_sum            'C155.9 H101.1 Cu8 N1.3 O41.3 S32'
_chemical_formula_weight         4187.51
_chemical_name_systematic
'[tetrakis(μ₂-4,4',4'',4'''-(([2,2'-bi(1,3-dithiolylidene)]-4,4',5,5'-tetrayltetrakis(sulfanediyl))tetrakis(methylene))tetrabenzoate-O,O')-bis(water)-di-copper(ii)]4, dimethylformamide solvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2024-01-19
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2024-01-24 deposited with the CCDC.	2024-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.324(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.081(3)
_cell_length_b                   31.525(6)
_cell_length_c                   20.060(2)
_cell_measurement_reflns_used    3080
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      60.0850
_cell_measurement_theta_min      3.1880
_cell_volume                     11692(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 42.102a (release 15-09-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -69.00  -9.00   1.00  100.00    --    0.00 -57.00 150.00   60
  2  ω    -31.00  25.00   1.00  100.00    --    0.00  77.00-120.00   56
  3  ω     99.00 147.00   1.00  400.00    --   80.52  61.00  60.00   48
  4  ω      9.00  42.00   1.00  400.00    --   80.52 -45.00  90.00   33
  5  ω      7.00  33.00   1.00  400.00    --   80.52 -30.00-180.00   26
  6  ω      6.00  35.00   1.00  400.00    --   80.52 -30.00 -30.00   29
  7  ω      9.00  34.00   1.00  400.00    --   80.52 -30.00  60.00   25
  8  ω    114.00 145.00   1.00  400.00    --   80.52  77.00  90.00   31
  9  ω      6.00  32.00   1.00  400.00    --   80.52 -30.00 150.00   26
 10  ω     10.00  68.00   1.00  400.00    --   80.52 -61.00-120.00   58
 11  ω     11.00  43.00   1.00  400.00    --   80.52 -45.00 120.00   32
 12  ω     43.00  70.00   1.00  400.00    --   80.52 -61.00 -60.00   27
 13  ω     10.00  37.00   1.00  400.00    --   80.52 -45.00-180.00   27
 14  ω     18.00  62.00   1.00  400.00    --   80.52 -61.00 -90.00   44
 15  ω      7.00  29.00   1.00  400.00    --   80.52 -30.00 -60.00   22
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0615464000
_diffrn_orient_matrix_UB_12      0.0152584000
_diffrn_orient_matrix_UB_13      -0.0313806000
_diffrn_orient_matrix_UB_21      0.0479905000
_diffrn_orient_matrix_UB_22      -0.0367693000
_diffrn_orient_matrix_UB_23      0.0359257000
_diffrn_orient_matrix_UB_31      -0.0290833000
_diffrn_orient_matrix_UB_32      -0.0283633000
_diffrn_orient_matrix_UB_33      -0.0632841000
_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  0.0962
_diffrn_reflns_av_unetI/netI     0.1165
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11535
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        33.411
_diffrn_reflns_theta_max         33.411
_diffrn_reflns_theta_min         2.771
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.929
_exptl_absorpt_correction_T_max  0.812
_exptl_absorpt_correction_T_min  0.229
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_description       needle
_exptl_crystal_F_000             4240
_exptl_crystal_recrystallization_method 'solvothermal in DMF'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.865
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.430
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         4566
_refine_ls_number_restraints     287
_refine_ls_restrained_S_all      1.395
_refine_ls_R_factor_all          0.1717
_refine_ls_R_factor_gt           0.1460
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3817
_refine_ls_wR_factor_ref         0.4082
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3178
_reflns_number_total             4566
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3ce01251d2.cif
_cod_data_source_block           cy082_dmf_cuaco-131023
_cod_depositor_comments
'Adding full bibliography for 7248225--7248227.cif.'
_cod_original_formula_sum        'C155.90 H101.10 Cu8 N1.30 O41.30 S32'
_cod_database_code               7248226
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C152 H96 Cu8 O40 S32'
_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   0.828
_shelx_estimated_absorpt_t_min   0.366
_diffrn_oxdiff_digest_frames
;
018597a471a5eda839fadd18bfe423f91d00566791d
;
_diffrn_oxdiff_digest_hkl
;
01af7c84ed74cdb470a7db8cbd540f7c405f49
;
_reflns_odcompleteness_completeness 97.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     44.45
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1A-C3A = N1B-C3B
 1.33 with sigma of 0.02
 N1A-C2A = N1A-C1A = N1B-C2B = N1B-C1B
 1.44 with sigma of 0.02
 C3A-O1A = C3B-O1B
 1.22 with sigma of 0.02
 C30-C30_$1
 1.2 with sigma of 0.02
 C11_$1-C11
 1.25 with sigma of 0.02
 C1A-C3A = C2A-C3A = C2A-C1A = C2B-C3B = C1B-C3B = C1B-C2B
 2.45 with sigma of 0.04
 N1A-O1A = N1B-O1B
 2.25 with sigma of 0.04
 O5-C57 \\sim O6-C57 \\sim O4-C19 \\sim O3-C19 \\sim O1-C1 \\sim O2-C1 \\sim
O11-C76 \\sim O12-C76 \\sim O10-
 C20 \\sim O9-C20 \\sim O18-C68 \\sim O17-C68 \\sim O19-C39 \\sim O20-C39 \\sim
O16-C38 \\sim O15-C38
 with sigma of 0.02
3. Restrained planarity
 S14, C49, S11, C58, S15, S10
 with sigma of 0.1
 O1B, C3B, C1B, C2B, N1B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C58)
\\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C59) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.025
Uanis(C30) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(S6)
\\sim Ueq, Uanis(S7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.025
Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(S3) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(S2) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms
of 0.1
5. Rigid body (RIGU) restrains
 C30, C28, C29, S6, S7
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C9, C10, S3, C11, S2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Fixed Sof: C1A(0.25) H1AA(0.25) H1AB(0.25) H1AC(0.25) N1A(0.25) C2A(0.25)
 H2AA(0.25) H2AB(0.25) H2AC(0.25) C3A(0.25) H3A(0.25) O1A(0.25) C2B(0.33)
 C3B(0.33) N1B(0.33) O1B(0.33) C1B(0.33)
7.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C8(H8A,H8B), C50(H50A,H50B), C46(H46A,H46B), C27(H27A,H27B),
 C69(H69A,H69B), C61(H61A,H61B), C12(H12A,H12B)
7.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C26(H26), C22(H22), C23(H23), C72(H72), C71(H71), C75(H75),
 C74(H74), C4(H4), C3(H3), C7(H7), C6(H6), C36(H36), C37(H37), C33(H33),
 C34(H34), C42(H42), C41(H41), C45(H45), C44(H44), C17(H17), C18(H18), C14(H14),
  C15(H15), C55(H55), C56(H56), C52(H52), C53(H53), C64(H64), C66(H66),
 C67(H67), C63(H63), C3A(H3A)
7.c Fitted hexagon refined as free rotating group:
 C24(C25,C26,C21,C22,C23), C73(C72,C71,C70,C75,C74), C35(C36,C37,C32,C33,C34),
 C43(C42,C41,C40,C45,C44), C16(C17,C18,C13,C14,C15), C55(C56,C51,C52,C53,C54),
 C64(C65,C66,C67,C62,C63)
7.d Idealised Me refined with riding coordinates:
 C1A(H1AA,H1AB,H1AC), C2A(H2AA,H2AB,H2AC)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_ins_header
;
TITL CY082_DMF_CuAcO-131023 in P2(1)/m 
REM P2(1)/m (#11 in standard setting)
CELL 1.54184  19.080747  31.525297  20.060428  90.0000 104.3237  90.0000
ZERR    3.00   0.003253   0.006107   0.002468   0.0000   0.0150   0.0000
LATT  1
SYMM -x, y+1/2,-z 
SFAC C H O S Cu
UNIT 456.00 288.00 120.00 96.00 24.00
REM  CrysAlisPro recorded range (K): Min=180.0; max=180.0; aver:180.0
TEMP -93
SIZE 0.05 0.06 0.32
TREF
HKLF 4
END
;
_olex2_exptl_crystal_mounting_method 'paraffin oil'
_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 1.451
_oxdiff_exptl_absorpt_empirical_full_min 0.681
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-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
Cu5 Cu 0.7481(2) 0.62552(17) 0.6283(2) 0.100(2) Uani 1 1 d . . . . .
C59 C 0.455(3) 0.5348(13) 0.199(2) 0.137(15) Uani 1 1 d . U . . .
S10 S 0.5365(6) 0.5266(4) 0.2371(5) 0.134(4) Uani 1 1 d . . . . .
C58 C 0.5675(19) 0.5220(7) 0.1612(15) 0.063(10) Uani 1 1 d . U . . .
S15 S 0.4925(6) 0.5264(3) 0.0870(4) 0.116(4) Uani 1 1 d . . . . .
C60 C 0.418(2) 0.5384(12) 0.126(2) 0.126(14) Uani 1 1 d . U . . .
C38 C 0.7018(18) 0.5957(8) 0.7358(16) 0.100(12) Uiso 1 1 d D . . . .
O15 O 0.7040(11) 0.6295(7) 0.7034(10) 0.101(7) Uiso 1 1 d D . . . .
Cu3 Cu 0.8561(4) 0.750000 0.3454(3) 0.124(3) Uani 1 2 d S T P . .
S16 S 0.3370(7) 0.5393(6) 0.0791(5) 0.195(7) Uani 1 1 d . . . . .
O16 O 0.7185(11) 0.5578(7) 0.7277(10) 0.103(7) Uiso 1 1 d D . . . .
Cu2 Cu 0.3300(4) 0.750000 0.3911(4) 0.136(3) Uani 1 2 d S T P . .
O8 O 1.079(3) 0.750000 0.286(3) 0.24(2) Uiso 1 2 d S T P . .
Cu4 Cu 0.9857(4) 0.750000 0.3146(3) 0.136(3) Uani 1 2 d S T P . .
O7 O 0.757(3) 0.750000 0.379(2) 0.23(2) Uiso 1 2 d S T P . .
Cu6 Cu 0.7628(3) 0.54356(18) 0.6545(2) 0.113(2) Uani 1 1 d . . . . .
Cu1 Cu 0.4716(4) 0.750000 0.4038(5) 0.149(4) Uani 1 2 d S T P . .
O2 O 0.8537(11) 0.9414(7) 0.7135(10) 0.097(7) Uiso 1 1 d D . . . .
O22 O 0.7406(12) 0.6895(7) 0.6042(11) 0.115(8) Uiso 1 1 d . . . . .
C24 C 0.4376(17) 0.6196(8) 0.6702(11) 0.136(14) Uiso 1 1 d . . . . .
C25 C 0.4980(12) 0.6309(8) 0.6472(12) 0.115(13) Uiso 1 1 d G . . . .
H25 H 0.544957 0.622874 0.672938 0.138 Uiso 1 1 calc R . . . .
C26 C 0.4898(13) 0.6538(7) 0.5866(12) 0.095(11) Uiso 1 1 d G . . . .
H26 H 0.531112 0.661486 0.570878 0.114 Uiso 1 1 calc R . . . .
C21 C 0.4211(16) 0.6655(7) 0.5490(10) 0.135(14) Uiso 1 1 d G . . . .
C22 C 0.3607(12) 0.6542(9) 0.5720(14) 0.172(18) Uiso 1 1 d G . . . .
H22 H 0.313790 0.662205 0.546297 0.206 Uiso 1 1 calc R . . . .
C23 C 0.3689(13) 0.6313(9) 0.6326(15) 0.153(16) Uiso 1 1 d G . . . .
H23 H 0.327634 0.623593 0.648356 0.183 Uiso 1 1 calc R . . . .
O1 O 0.8394(12) 0.8703(7) 0.6894(10) 0.102(7) Uiso 1 1 d D . . . .
O21 O 0.7761(12) 0.4759(7) 0.6811(10) 0.115(8) Uiso 1 1 d . . . . .
S5 S 0.4703(7) 0.6094(4) 0.9471(5) 0.142(4) Uani 1 1 d . . . . .
S13 S 0.8043(7) 0.5111(5) 0.0626(5) 0.169(6) Uani 1 1 d . . . . .
S4 S 1.1918(7) 0.8976(4) 0.7075(6) 0.169(5) Uani 1 1 d . . . . .
S1 S 1.2276(6) 0.8906(5) 0.8776(6) 0.158(5) Uani 1 1 d . . . . .
S8 S 0.3847(8) 0.6021(4) 0.7842(6) 0.162(5) Uani 1 1 d . . . . .
S12 S 0.8574(6) 0.5037(4) 0.2346(5) 0.150(5) Uani 1 1 d . . . . .
S11 S 0.7038(6) 0.5073(4) 0.2340(5) 0.130(4) Uani 1 1 d . . . . .
C47 C 0.7605(19) 0.5060(11) 0.188(2) 0.096(12) Uani 1 1 d . U . . .
C48 C 0.7429(15) 0.5107(8) 0.1193(15) 0.055(9) Uani 1 1 d . U . . .
S14 S 0.6511(6) 0.5062(4) 0.0835(4) 0.125(4) Uani 1 1 d . . . . .
C49 C 0.6261(15) 0.5132(3) 0.1611(11) 0.028(8) Uani 1 1 d . U . . .
C76 C 0.3774(16) 0.6954(13) 0.299(2) 0.144(16) Uiso 1 1 d D . . . .
O6 O 0.8352(13) 0.7027(7) 0.2702(11) 0.111(8) Uiso 1 1 d D . . . .
O19 O 0.7920(11) 0.6150(7) 0.5540(10) 0.092(7) Uiso 1 1 d D . . . .
O3 O 0.8944(13) 0.7931(7) 0.4167(11) 0.117(8) Uiso 1 1 d D . . . .
O18 O 0.6584(13) 0.6105(8) 0.5648(11) 0.125(8) Uiso 1 1 d D . . . .
O12 O 0.3243(16) 0.7069(9) 0.3225(13) 0.150(10) Uiso 1 1 d D . . . .
O4 O 1.0094(13) 0.7932(7) 0.3881(11) 0.116(8) Uiso 1 1 d D . . . .
O17 O 0.6712(11) 0.5389(7) 0.5904(10) 0.100(7) Uiso 1 1 d D . . . .
O5 O 0.9495(15) 0.7044(8) 0.2464(13) 0.148(10) Uiso 1 1 d D . . . .
C31 C 0.5653(17) 0.6135(11) 0.9691(15) 0.097(11) Uiso 1 1 d . . . . .
H31A H 0.578704 0.640881 0.992987 0.117 Uiso 1 1 calc R . . . .
H31B H 0.585021 0.590685 1.002382 0.117 Uiso 1 1 calc R . . . .
C73 C 0.376(2) 0.6699(8) 0.2394(12) 0.142(15) Uiso 1 1 d . . . . .
C72 C 0.4279(14) 0.6580(10) 0.2055(18) 0.19(2) Uiso 1 1 d G . . . .
H72 H 0.476909 0.666089 0.223380 0.231 Uiso 1 1 calc R . . . .
C71 C 0.408(2) 0.6342(10) 0.1454(17) 0.174(18) Uiso 1 1 d G . . . .
H71 H 0.444084 0.626090 0.122167 0.209 Uiso 1 1 calc R . . . .
C70 C 0.337(2) 0.6224(10) 0.1192(13) 0.181(19) Uiso 1 1 d G . . . .
C75 C 0.2845(15) 0.6343(11) 0.1531(18) 0.30(3) Uiso 1 1 d G . . . .
H75 H 0.235469 0.626196 0.135174 0.359 Uiso 1 1 calc R . . . .
C74 C 0.3040(17) 0.6581(10) 0.2132(17) 0.149(15) Uiso 1 1 d G . . . .
H74 H 0.268293 0.666195 0.236388 0.179 Uiso 1 1 calc R . . . .
C5 C 1.069(2) 0.8925(16) 0.8589(17) 0.111(12) Uiso 1 1 d . . . . .
C4 C 1.042(2) 0.8539(15) 0.8383(19) 0.133(14) Uiso 1 1 d . . . . .
H4 H 1.064882 0.828085 0.856048 0.159 Uiso 1 1 calc R . . . .
C3 C 0.9745(18) 0.8559(12) 0.7864(16) 0.100(11) Uiso 1 1 d . . . . .
H3 H 0.946396 0.833042 0.762846 0.121 Uiso 1 1 calc R . . . .
C2 C 0.9598(18) 0.9006(13) 0.7787(16) 0.100(11) Uiso 1 1 d . . . . .
C7 C 0.9858(19) 0.9413(13) 0.8028(17) 0.110(12) Uiso 1 1 d . . . . .
H7 H 0.965008 0.968556 0.791376 0.132 Uiso 1 1 calc R . . . .
C6 C 1.050(2) 0.9299(16) 0.848(2) 0.136(15) Uiso 1 1 d . . . . .
H6 H 1.080686 0.951629 0.870856 0.163 Uiso 1 1 calc R . . . .
O14 O 0.569(4) 0.750000 0.405(3) 0.28(3) Uiso 1 2 d S T P . .
O11 O 0.4423(15) 0.7039(8) 0.3304(13) 0.136(9) Uiso 1 1 d D . . . .
O9 O 0.4749(13) 0.7075(7) 0.4745(11) 0.111(8) Uiso 1 1 d D . . . .
O13 O 0.214(3) 0.750000 0.400(2) 0.208(19) Uiso 1 2 d S T P . .
C39 C 0.8120(16) 0.5779(8) 0.5447(14) 0.078(10) Uiso 1 1 d D . . . .
O20 O 0.7988(13) 0.5436(8) 0.5725(12) 0.139(9) Uiso 1 1 d D . . . .
O10 O 0.3583(18) 0.7041(10) 0.4612(15) 0.173(11) Uiso 1 1 d D . . . .
C35 C 0.6664(11) 0.6013(8) 0.7977(9) 0.083(10) Uiso 1 1 d . . . . .
C36 C 0.6466(12) 0.6413(7) 0.8155(11) 0.119(13) Uiso 1 1 d G . . . .
H36 H 0.654398 0.665506 0.790002 0.143 Uiso 1 1 calc R . . . .
C37 C 0.6154(12) 0.6460(6) 0.8708(12) 0.116(13) Uiso 1 1 d G . . . .
H37 H 0.601828 0.673411 0.883012 0.139 Uiso 1 1 calc R . . . .
C32 C 0.6039(10) 0.6107(8) 0.9082(9) 0.078(10) Uiso 1 1 d G . . . .
C33 C 0.6237(11) 0.5707(7) 0.8903(10) 0.089(11) Uiso 1 1 d G . . . .
H33 H 0.615919 0.546493 0.915811 0.107 Uiso 1 1 calc R . . . .
C34 C 0.6550(12) 0.5660(6) 0.8350(12) 0.126(13) Uiso 1 1 d G . . . .
H34 H 0.668489 0.538588 0.822802 0.151 Uiso 1 1 calc R . . . .
C1 C 0.8709(15) 0.9025(8) 0.7197(14) 0.070(9) Uiso 1 1 d D . . . .
C19 C 0.9609(14) 0.7992(10) 0.4209(15) 0.092(11) Uiso 1 1 d D . . . .
C43 C 0.8604(12) 0.5563(9) 0.3455(9) 0.096(11) Uiso 1 1 d . . . . .
C42 C 0.8535(11) 0.5979(8) 0.3660(11) 0.109(12) Uiso 1 1 d G . . . .
H42 H 0.861503 0.620813 0.338076 0.131 Uiso 1 1 calc R . . . .
C41 C 0.8347(12) 0.6060(7) 0.4275(12) 0.116(13) Uiso 1 1 d G . . . .
H41 H 0.829926 0.634360 0.441580 0.140 Uiso 1 1 calc R . . . .
C40 C 0.8229(11) 0.5724(9) 0.4684(9) 0.090(11) Uiso 1 1 d G . . . .
C45 C 0.8299(13) 0.5309(8) 0.4479(12) 0.140(14) Uiso 1 1 d G . . . .
H45 H 0.821861 0.507963 0.475853 0.167 Uiso 1 1 calc R . . . .
C44 C 0.8487(14) 0.5228(6) 0.3864(14) 0.180(18) Uiso 1 1 d G . . . .
H44 H 0.853438 0.494415 0.372349 0.216 Uiso 1 1 calc R . . . .
C10 C 1.2031(15) 0.8482(13) 0.753(2) 0.097(11) Uani 1 1 d . U . . .
C9 C 1.213(2) 0.8502(14) 0.819(3) 0.134(14) Uani 1 1 d . U . . .
S2 S 1.2307(7) 0.8004(5) 0.8606(6) 0.169(5) Uani 1 1 d . U . . .
C11 C 1.2181(16) 0.7695(3) 0.7855(12) 0.099(10) Uani 1 1 d D U . . .
S3 S 1.1943(7) 0.8029(5) 0.7084(6) 0.167(5) Uani 1 1 d . U . . .
C16 C 0.9945(17) 0.8266(8) 0.4895(12) 0.116(13) Uiso 1 1 d . . . . .
C17 C 0.9621(12) 0.8358(8) 0.5427(16) 0.166(17) Uiso 1 1 d G . . . .
H17 H 0.914234 0.826340 0.540306 0.199 Uiso 1 1 calc R . . . .
C18 C 0.9996(17) 0.8588(9) 0.5995(12) 0.128(13) Uiso 1 1 d G . . . .
H18 H 0.977481 0.865066 0.635845 0.153 Uiso 1 1 calc R . . . .
C13 C 1.0696(17) 0.8726(9) 0.6030(13) 0.153(16) Uiso 1 1 d G . . . .
C14 C 1.1021(12) 0.8635(10) 0.5498(18) 0.22(2) Uiso 1 1 d G . . . .
H14 H 1.149909 0.872925 0.552261 0.261 Uiso 1 1 calc R . . . .
C15 C 1.0645(17) 0.8405(9) 0.4931(13) 0.154(16) Uiso 1 1 d G . . . .
H15 H 1.086662 0.834199 0.456722 0.185 Uiso 1 1 calc R . . . .
C8 C 1.1522(18) 0.8827(12) 0.9172(17) 0.116(13) Uiso 1 1 d . . . . .
H8A H 1.153107 0.853197 0.934184 0.139 Uiso 1 1 calc R . . . .
H8B H 1.157854 0.901974 0.957138 0.139 Uiso 1 1 calc R . . . .
C20 C 0.4214(17) 0.6936(15) 0.494(2) 0.180(19) Uiso 1 1 d D . . . .
C50 C 0.792(3) 0.5656(14) 0.033(2) 0.167(17) Uiso 1 1 d . . . . .
H50A H 0.822260 0.570376 -0.000070 0.201 Uiso 1 1 calc R . . . .
H50B H 0.741103 0.569595 0.007970 0.201 Uiso 1 1 calc R . . . .
C46 C 0.880(2) 0.5541(12) 0.2747(18) 0.130(14) Uiso 1 1 d . . . . .
H46A H 0.932137 0.559331 0.281321 0.156 Uiso 1 1 calc R . . . .
H46B H 0.853156 0.576549 0.244265 0.156 Uiso 1 1 calc R . . . .
C27 C 0.450(2) 0.5904(12) 0.7375(18) 0.132(14) Uiso 1 1 d . . . . .
H27A H 0.499245 0.595363 0.767070 0.158 Uiso 1 1 calc R . . . .
H27B H 0.446429 0.560123 0.723818 0.158 Uiso 1 1 calc R . . . .
C28 C 0.4160(15) 0.6482(9) 0.8281(15) 0.062(7) Uani 1 1 d . U . . .
S7 S 0.3914(7) 0.6961(4) 0.7838(5) 0.141(4) Uani 1 1 d . U . . .
C30 C 0.4329(11) 0.7318(3) 0.8560(10) 0.040(6) Uani 1 1 d D U . . .
S6 S 0.4602(6) 0.7011(4) 0.9324(5) 0.132(4) Uani 1 1 d . U . . .
C29 C 0.4469(15) 0.6517(10) 0.8984(15) 0.063(7) Uani 1 1 d . U . . .
C57 C 0.8842(15) 0.6939(10) 0.2392(15) 0.084(10) Uiso 1 1 d D . . . .
C55 C 0.9056(11) 0.6445(7) 0.1547(12) 0.065(9) Uiso 1 1 d . . . . .
H55 H 0.954584 0.653663 0.165999 0.078 Uiso 1 1 calc R . . . .
C56 C 0.8833(15) 0.6128(7) 0.1059(11) 0.136(14) Uiso 1 1 d G . . . .
H56 H 0.916936 0.600307 0.083847 0.163 Uiso 1 1 calc R . . . .
C51 C 0.8117(17) 0.5993(8) 0.0893(12) 0.149(15) Uiso 1 1 d G . . . .
C52 C 0.7624(11) 0.6176(10) 0.1215(16) 0.23(2) Uiso 1 1 d G . . . .
H52 H 0.713489 0.608415 0.110151 0.270 Uiso 1 1 calc R . . . .
C53 C 0.7848(14) 0.6493(9) 0.1703(14) 0.148(15) Uiso 1 1 d G . . . .
H53 H 0.751135 0.661772 0.192303 0.178 Uiso 1 1 calc R . . . .
C54 C 0.8564(16) 0.6627(7) 0.1869(10) 0.117(13) Uiso 1 1 d G . . . .
C69 C 0.334(3) 0.5938(17) 0.054(2) 0.20(2) Uiso 1 1 d . . . . .
H69A H 0.376035 0.600337 0.035104 0.236 Uiso 1 1 calc R . . . .
H69B H 0.289345 0.599506 0.018428 0.236 Uiso 1 1 calc R . . . .
C61 C 0.409(2) 0.5143(14) 0.312(2) 0.164(17) Uiso 1 1 d . . . . .
H61A H 0.423623 0.487008 0.295137 0.197 Uiso 1 1 calc R . . . .
H61B H 0.366779 0.508719 0.331221 0.197 Uiso 1 1 calc R . . . .
C64 C 0.5356(14) 0.5838(6) 0.4583(13) 0.117(13) Uiso 1 1 d . . . . .
H64 H 0.539770 0.612053 0.475133 0.141 Uiso 1 1 calc R . . . .
C65 C 0.5824(11) 0.5526(9) 0.4926(9) 0.095(11) Uiso 1 1 d G . . . .
C66 C 0.5763(11) 0.5112(7) 0.4680(12) 0.112(12) Uiso 1 1 d G . . . .
H66 H 0.608266 0.489926 0.491441 0.135 Uiso 1 1 calc R . . . .
C67 C 0.5234(13) 0.5010(6) 0.4090(12) 0.115(12) Uiso 1 1 d G . . . .
H67 H 0.519228 0.472703 0.392126 0.138 Uiso 1 1 calc R . . . .
C62 C 0.4766(11) 0.5321(9) 0.3746(9) 0.093(11) Uiso 1 1 d G . . . .
C63 C 0.4827(12) 0.5735(7) 0.3993(12) 0.129(14) Uiso 1 1 d G . . . .
H63 H 0.450731 0.594829 0.375817 0.155 Uiso 1 1 calc R . . . .
C68 C 0.6432(15) 0.5716(8) 0.5579(14) 0.072(10) Uiso 1 1 d D . . . .
C1A C 0.617(5) 0.750000 0.592(4) 0.17(5) Uiso 0.5 2 d DS T P . .
H1AA H 0.660826 0.736312 0.585338 0.250 Uiso 0.25 1 calc R . . A -1
H1AB H 0.614761 0.779288 0.575335 0.250 Uiso 0.25 1 calc R . . A -1
H1AC H 0.574342 0.734400 0.566558 0.250 Uiso 0.25 1 calc R . . A -1
N1A N 0.619(3) 0.750000 0.664(3) 0.24(6) Uiso 0.5 2 d DS T P . .
C2A C 0.689(3) 0.750000 0.711(5) 0.37(13) Uiso 0.5 2 d DS T P . .
H2AA H 0.684725 0.742195 0.757341 0.551 Uiso 0.25 1 calc R . . B -1
H2AB H 0.710589 0.778368 0.712787 0.551 Uiso 0.25 1 calc R . . B -1
H2AC H 0.720407 0.729438 0.695875 0.551 Uiso 0.25 1 calc R . . B -1
C3A C 0.559(3) 0.750000 0.687(3) 0.014(18) Uiso 0.5 2 d DS T P . .
H3A H 0.512858 0.750000 0.654956 0.016 Uiso 0.5 2 calc RS T P . .
O1A O 0.562(3) 0.750000 0.748(3) 0.15(3) Uiso 0.5 2 d DS T P . .
C2B C 0.655(3) 0.6210(15) 0.336(3) 0.02(2) Uiso 0.33 1 d D . . . .
C3B C 0.685(3) 0.6678(18) 0.435(2) 0.04(2) Uiso 0.33 1 d D . . . .
N1B N 0.668(2) 0.6623(13) 0.367(2) 0.031(17) Uiso 0.33 1 d D . . . .
O1B O 0.695(5) 0.702(3) 0.464(5) 0.47(13) Uiso 0.33 1 d D . . . .
C1B C 0.659(6) 0.6974(18) 0.320(3) 0.15(5) Uiso 0.33 1 d D . . . .
C12 C 1.092(2) 0.8978(16) 0.670(2) 0.185(19) Uiso 1 1 d . . . . .
H12A H 1.067774 0.885807 0.703519 0.222 Uiso 1 1 calc R . . . .
H12B H 1.075676 0.927511 0.660572 0.222 Uiso 1 1 calc R . . . .
S9 S 0.3847(7) 0.5478(5) 0.2464(6) 0.178(6) Uani 1 1 d . . . . .
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'
Cu Cu -1.9646 0.5888 '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'
S S 0.3331 0.5567 '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
1 -5 -1 0.1373
-1 5 1 0.1414
4 0 5 0.0202
-4 0 -5 0.0256
2 -1 -5 0.0188
-2 0 5 0.0338
3 5 1 0.0988
-5 -2 3 0.0475
-4 1 5 0.0323
5 1 -3 0.0342
-5 0 3 0.0269
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
O15 Cu5 Cu6 87.3(7) . . ?
O15 Cu5 O22 95.9(9) . . ?
O15 Cu5 O19 173.7(10) . . ?
O15 Cu5 O18 92.6(9) . . ?
O22 Cu5 Cu6 176.8(6) . . ?
O1 Cu5 O15 90.0(9) 4_575 . ?
O1 Cu5 Cu6 84.4(7) 4_575 . ?
O1 Cu5 O22 94.8(9) 4_575 . ?
O1 Cu5 O19 90.4(8) 4_575 . ?
O1 Cu5 O18 169.6(11) 4_575 . ?
O19 Cu5 Cu6 86.6(7) . . ?
O19 Cu5 O22 90.3(9) . . ?
O19 Cu5 O18 86.0(9) . . ?
O18 Cu5 Cu6 85.6(8) . . ?
O18 Cu5 O22 95.0(10) . . ?
S10 C59 S9 122(3) . . ?
C60 C59 S10 133(3) . . ?
C60 C59 S9 105(3) . . ?
C59 S10 C58 95(2) . . ?
S10 C58 S15 109.8(19) . . ?
C49 C58 S10 124(3) . . ?
C49 C58 S15 126(3) . . ?
C60 S15 C58 102.1(17) . . ?
C59 C60 S15 100(3) . . ?
C59 C60 S16 138(3) . . ?
S16 C60 S15 120(3) . . ?
O15 C38 O16 134(3) . . ?
O15 C38 C35 113(2) . . ?
O16 C38 C35 112(2) . . ?
C38 O15 Cu5 116(2) . . ?
O7 Cu3 Cu4 175.1(14) . . ?
O6 Cu3 Cu4 81.8(7) 4_575 . ?
O6 Cu3 Cu4 81.8(7) . . ?
O6 Cu3 O7 101.6(12) 4_575 . ?
O6 Cu3 O7 101.6(12) . . ?
O6 Cu3 O6 91.2(12) . 4_575 ?
O3 Cu3 Cu4 88.3(8) 4_575 . ?
O3 Cu3 Cu4 88.3(8) . . ?
O3 Cu3 O7 88.2(12) 4_575 . ?
O3 Cu3 O7 88.2(12) . . ?
O3 Cu3 O6 169.7(11) . . ?
O3 Cu3 O6 169.7(11) 4_575 4_575 ?
O3 Cu3 O6 90.1(8) . 4_575 ?
O3 Cu3 O6 90.1(8) 4_575 . ?
O3 Cu3 O3 86.8(13) . 4_575 ?
C60 S16 C69 98(2) . . ?
C38 O16 Cu6 120(2) . . ?
O12 Cu2 Cu1 86.8(9) . . ?
O12 Cu2 Cu1 86.8(9) 4_575 . ?
O12 Cu2 O12 90.2(16) 4_575 . ?
O12 Cu2 O13 100.0(12) 4_575 . ?
O12 Cu2 O13 100.0(12) . . ?
O12 Cu2 O10 167.5(14) 4_575 . ?
O12 Cu2 O10 167.5(14) . 4_575 ?
O12 Cu2 O10 87.1(11) . . ?
O12 Cu2 O10 87.1(11) 4_575 4_575 ?
O13 Cu2 Cu1 170.2(12) . . ?
O10 Cu2 Cu1 80.9(10) . . ?
O10 Cu2 Cu1 80.9(10) 4_575 . ?
O10 Cu2 O13 92.5(12) 4_575 . ?
O10 Cu2 O13 92.4(12) . . ?
O10 Cu2 O10 92.8(17) . 4_575 ?
O8 Cu4 Cu3 176.8(15) . . ?
O4 Cu4 Cu3 83.2(7) 4_575 . ?
O4 Cu4 Cu3 83.2(7) . . ?
O4 Cu4 O8 99.1(13) 4_575 . ?
O4 Cu4 O8 99.1(13) . . ?
O4 Cu4 O4 87.2(13) . 4_575 ?
O4 Cu4 O5 171.4(11) 4_575 4_575 ?
O4 Cu4 O5 89.5(10) 4_575 . ?
O4 Cu4 O5 89.5(10) . 4_575 ?
O4 Cu4 O5 171.4(11) . . ?
O5 Cu4 Cu3 88.6(8) 4_575 . ?
O5 Cu4 Cu3 88.6(8) . . ?
O5 Cu4 O8 89.2(13) . . ?
O5 Cu4 O8 89.2(13) 4_575 . ?
O5 Cu4 O5 92.7(15) 4_575 . ?
O16 Cu6 Cu5 83.0(7) . . ?
O16 Cu6 O21 95.0(9) . . ?
O16 Cu6 O20 165.3(11) . . ?
O2 Cu6 Cu5 85.1(7) 4_575 . ?
O2 Cu6 O16 88.4(8) 4_575 . ?
O2 Cu6 O21 93.3(9) 4_575 . ?
O2 Cu6 O20 93.9(9) 4_575 . ?
O21 Cu6 Cu5 177.5(6) . . ?
O17 Cu6 Cu5 84.7(7) . . ?
O17 Cu6 O16 91.8(9) . . ?
O17 Cu6 O2 169.7(10) . 4_575 ?
O17 Cu6 O21 96.9(9) . . ?
O17 Cu6 O20 83.5(10) . . ?
O20 Cu6 Cu5 82.7(8) . . ?
O20 Cu6 O21 99.4(10) . . ?
O14 Cu1 Cu2 175.4(19) . . ?
O14 Cu1 O11 95.9(15) . . ?
O14 Cu1 O11 95.9(15) . 4_575 ?
O14 Cu1 O9 98.0(15) . 4_575 ?
O14 Cu1 O9 98.0(15) . . ?
O11 Cu1 Cu2 80.8(8) . . ?
O11 Cu1 Cu2 80.8(8) 4_575 . ?
O11 Cu1 O11 90.6(14) . 4_575 ?
O9 Cu1 Cu2 85.4(8) 4_575 . ?
O9 Cu1 Cu2 85.4(8) . . ?
O9 Cu1 O11 89.4(9) . . ?
O9 Cu1 O11 166.0(11) 4_575 . ?
O9 Cu1 O11 89.4(9) 4_575 4_575 ?
O9 Cu1 O11 166.0(11) . 4_575 ?
O9 Cu1 O9 87.4(13) 4_575 . ?
C1 O2 Cu6 118(2) . 4_575 ?
C25 C24 C23 120.0 . . ?
C25 C24 C27 118(2) . . ?
C23 C24 C27 122(2) . . ?
C24 C25 C26 120.0 . . ?
C21 C26 C25 120.0 . . ?
C26 C21 C22 120.0 . . ?
C26 C21 C20 114(3) . . ?
C22 C21 C20 126(3) . . ?
C21 C22 C23 120.0 . . ?
C22 C23 C24 120.0 . . ?
C1 O1 Cu5 121(2) . 4_575 ?
C29 S5 C31 101.5(15) . . ?
C50 S13 C48 99.3(18) . . ?
C10 S4 C12 101.1(19) . . ?
C9 S1 C8 100(2) . . ?
C28 S8 C27 104.1(17) . . ?
C46 S12 C47 106.9(17) . . ?
C47 S11 C49 94.1(15) . . ?
S11 C47 S12 116(2) . . ?
C48 C47 S12 119(3) . . ?
C48 C47 S11 124(3) . . ?
C47 C48 S13 127(3) . . ?
C47 C48 S14 113(2) . . ?
S14 C48 S13 118.9(17) . . ?
C48 S14 C49 95.2(13) . . ?
C58 C49 S11 128(2) . . ?
C58 C49 S14 121(2) . . ?
S14 C49 S11 110.8(16) . . ?
O12 C76 C73 128(3) . . ?
O12 C76 O11 122(4) . . ?
O11 C76 C73 110(3) . . ?
C57 O6 Cu3 118(2) . . ?
C39 O19 Cu5 119(2) . . ?
C19 O3 Cu3 110(2) . . ?
C68 O18 Cu5 117(2) . . ?
C76 O12 Cu2 124(3) . . ?
C19 O4 Cu4 115(2) . . ?
C68 O17 Cu6 119(2) . . ?
C57 O5 Cu4 116(2) . . ?
C32 C31 S5 116.8(19) . . ?
C72 C73 C76 134(3) . . ?
C72 C73 C74 120.0 . . ?
C74 C73 C76 106(3) . . ?
C73 C72 C71 120.0 . . ?
C70 C71 C72 120.0 . . ?
C71 C70 C69 107(4) . . ?
C75 C70 C71 120.0 . . ?
C75 C70 C69 133(4) . . ?
C70 C75 C74 120.0 . . ?
C75 C74 C73 120.0 . . ?
C4 C5 C8 105(4) . . ?
C6 C5 C4 137(5) . . ?
C6 C5 C8 118(4) . . ?
C5 C4 C3 113(4) . . ?
C2 C3 C4 104(3) . . ?
C3 C2 C1 103(3) . . ?
C7 C2 C3 144(4) . . ?
C7 C2 C1 113(3) . . ?
C6 C7 C2 99(4) . . ?
C5 C6 C7 123(5) . . ?
C76 O11 Cu1 124(3) . . ?
C20 O9 Cu1 126(3) . . ?
O19 C39 O20 129(3) . . ?
O19 C39 C40 111(2) . . ?
O20 C39 C40 115(3) . . ?
C39 O20 Cu6 122(2) . . ?
C20 O10 Cu2 128(3) . . ?
C36 C35 C38 120(2) . . ?
C36 C35 C34 120.0 . . ?
C34 C35 C38 120(2) . . ?
C37 C36 C35 120.0 . . ?
C32 C37 C36 120.0 . . ?
C37 C32 C31 123(2) . . ?
C37 C32 C33 120.0 . . ?
C33 C32 C31 117(2) . . ?
C32 C33 C34 120.0 . . ?
C33 C34 C35 120.0 . . ?
O2 C1 C2 106(2) . . ?
O1 C1 O2 131(3) . . ?
O1 C1 C2 123(2) . . ?
O3 C19 O4 142(3) . . ?
O3 C19 C16 108(3) . . ?
O4 C19 C16 109(3) . . ?
C42 C43 C44 120.0 . . ?
C42 C43 C46 112(2) . . ?
C44 C43 C46 128(2) . . ?
C43 C42 C41 120.0 . . ?
C40 C41 C42 120.0 . . ?
C41 C40 C39 124(2) . . ?
C41 C40 C45 120.0 . . ?
C45 C40 C39 115(2) . . ?
C44 C45 C40 120.0 . . ?
C45 C44 C43 120.0 . . ?
C9 C10 S4 117(4) . . ?
C9 C10 S3 124(4) . . ?
S3 C10 S4 119(2) . . ?
S1 C9 S2 111(3) . . ?
C10 C9 S1 134(4) . . ?
C10 C9 S2 113(4) . . ?
C11 S2 C9 97.0(17) . . ?
S2 C11 S3 110.9(8) . . ?
C11 C11 S2 123.6(7) 4_575 . ?
C11 C11 S3 125.1(7) 4_575 . ?
C10 S3 C11 93.8(16) . . ?
C17 C16 C19 127(2) . . ?
C17 C16 C15 120.0 . . ?
C15 C16 C19 113(2) . . ?
C18 C17 C16 120.0 . . ?
C17 C18 C13 120.0 . . ?
C18 C13 C14 120.0 . . ?
C18 C13 C12 106(3) . . ?
C14 C13 C12 134(3) . . ?
C15 C14 C13 120.0 . . ?
C14 C15 C16 120.0 . . ?
C5 C8 S1 112(2) . . ?
O9 C20 C21 128(4) . . ?
O9 C20 O10 119(4) . . ?
O10 C20 C21 113(3) . . ?
C51 C50 S13 116(3) . . ?
C43 C46 S12 112(2) . . ?
C24 C27 S8 110(2) . . ?
S8 C28 S7 116.7(17) . . ?
C29 C28 S8 126(2) . . ?
C29 C28 S7 116(2) . . ?
C28 S7 C30 96.8(11) . . ?
C30 C30 S7 127.5(5) 4_575 . ?
C30 C30 S6 123.0(5) 4_575 . ?
S6 C30 S7 108.6(7) . . ?
C29 S6 C30 99.9(12) . . ?
S5 C29 S6 121.0(18) . . ?
C28 C29 S5 121(2) . . ?
C28 C29 S6 118(2) . . ?
O6 C57 C54 109(3) . . ?
O5 C57 O6 135(3) . . ?
O5 C57 C54 116(3) . . ?
C56 C55 C54 120.0 . . ?
C51 C56 C55 120.0 . . ?
C56 C51 C50 116(3) . . ?
C56 C51 C52 120.0 . . ?
C52 C51 C50 124(3) . . ?
C51 C52 C53 120.0 . . ?
C54 C53 C52 120.0 . . ?
C55 C54 C57 117(2) . . ?
C53 C54 C57 123(2) . . ?
C53 C54 C55 120.0 . . ?
C70 C69 S16 109(3) . . ?
S9 C61 C62 113(3) . . ?
C65 C64 C63 120.0 . . ?
C64 C65 C68 112(2) . . ?
C66 C65 C64 120.0 . . ?
C66 C65 C68 128(2) . . ?
C67 C66 C65 120.0 . . ?
C62 C67 C66 120.0 . . ?
C67 C62 C61 115(2) . . ?
C63 C62 C61 125(2) . . ?
C63 C62 C67 120.0 . . ?
C62 C63 C64 120.0 . . ?
O18 C68 O17 133(3) . . ?
O18 C68 C65 123(2) . . ?
O17 C68 C65 104(2) . . ?
C1A N1A C2A 116(3) . . ?
C3A N1A C1A 123(3) . . ?
C3A N1A C2A 121(3) . . ?
O1A C3A N1A 122(4) . . ?
O1B C3B N1B 125(5) . . ?
C3B N1B C2B 122(3) . . ?
C3B N1B C1B 122(3) . . ?
C1B N1B C2B 115(3) . . ?
C13 C12 S4 113(3) . . ?
C61 S9 C59 100(2) . . ?
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
Cu5 O15 1.90(2) . ?
Cu5 Cu6 2.638(8) . ?
Cu5 O22 2.07(2) . ?
Cu5 O1 1.87(2) 4_575 ?
Cu5 O19 1.91(2) . ?
Cu5 O18 1.92(2) . ?
C59 S10 1.57(5) . ?
C59 C60 1.47(5) . ?
C59 S9 1.88(4) . ?
S10 C58 1.77(3) . ?
C58 S15 1.80(3) . ?
C58 C49 1.15(3) . ?
S15 C60 1.82(4) . ?
C60 S16 1.60(4) . ?
C38 O15 1.251(15) . ?
C38 O16 1.258(15) . ?
C38 C35 1.56(3) . ?
Cu3 Cu4 2.693(10) . ?
Cu3 O7 2.16(5) . ?
Cu3 O6 2.09(2) . ?
Cu3 O6 2.09(2) 4_575 ?
Cu3 O3 1.98(2) . ?
Cu3 O3 1.98(2) 4_575 ?
S16 C69 1.78(5) . ?
O16 Cu6 1.92(2) . ?
Cu2 Cu1 2.649(11) . ?
Cu2 O12 1.92(3) . ?
Cu2 O12 1.92(3) 4_575 ?
Cu2 O13 2.27(5) . ?
Cu2 O10 2.00(3) . ?
Cu2 O10 2.00(3) 4_575 ?
O8 Cu4 2.00(6) . ?
Cu4 O4 1.98(2) 4_575 ?
Cu4 O4 1.98(2) . ?
Cu4 O5 1.99(3) 4_575 ?
Cu4 O5 1.99(3) . ?
Cu6 O2 1.90(2) 4_575 ?
Cu6 O21 2.20(2) . ?
Cu6 O17 1.90(2) . ?
Cu6 O20 1.93(3) . ?
Cu1 O14 1.86(7) . ?
Cu1 O11 2.05(3) 4_575 ?
Cu1 O11 2.05(3) . ?
Cu1 O9 1.94(2) . ?
Cu1 O9 1.94(2) 4_575 ?
O2 C1 1.267(14) . ?
C24 C25 1.3900 . ?
C24 C23 1.3900 . ?
C24 C27 1.60(4) . ?
C25 C26 1.3900 . ?
C26 C21 1.3900 . ?
C21 C22 1.3900 . ?
C21 C20 1.41(4) . ?
C22 C23 1.3900 . ?
O1 C1 1.257(15) . ?
S5 C31 1.76(3) . ?
S5 C29 1.65(3) . ?
S13 C48 1.82(3) . ?
S13 C50 1.81(5) . ?
S4 C10 1.79(4) . ?
S4 C12 1.86(5) . ?
S1 C9 1.70(5) . ?
S1 C8 1.82(3) . ?
S8 C27 1.78(4) . ?
S8 C28 1.73(3) . ?
S12 C47 1.86(4) . ?
S12 C46 1.78(4) . ?
S11 C47 1.59(4) . ?
S11 C49 1.81(3) . ?
C47 C48 1.34(3) . ?
C48 S14 1.73(3) . ?
S14 C49 1.75(3) . ?
C76 O12 1.269(16) . ?
C76 C73 1.44(4) . ?
C76 O11 1.271(16) . ?
O6 C57 1.275(15) . ?
O19 C39 1.259(15) . ?
O3 C19 1.266(15) . ?
O18 C68 1.260(15) . ?
O4 C19 1.274(15) . ?
O17 C68 1.267(15) . ?
O5 C57 1.263(15) . ?
C31 C32 1.58(3) . ?
C73 C72 1.3900 . ?
C73 C74 1.3900 . ?
C72 C71 1.3900 . ?
C71 C70 1.3900 . ?
C70 C75 1.3900 . ?
C70 C69 1.57(5) . ?
C75 C74 1.3900 . ?
C5 C4 1.35(4) . ?
C5 C6 1.24(5) . ?
C5 C8 1.76(5) . ?
C4 C3 1.44(4) . ?
C3 C2 1.44(4) . ?
C2 C7 1.42(4) . ?
C2 C1 1.81(4) . ?
C7 C6 1.37(4) . ?
O9 C20 1.262(16) . ?
C39 O20 1.270(15) . ?
C39 C40 1.60(3) . ?
O10 C20 1.267(16) . ?
C35 C36 1.3900 . ?
C35 C34 1.3900 . ?
C36 C37 1.3900 . ?
C37 C32 1.3900 . ?
C32 C33 1.3900 . ?
C33 C34 1.3900 . ?
C19 C16 1.62(3) . ?
C43 C42 1.3900 . ?
C43 C44 1.3900 . ?
C43 C46 1.55(3) . ?
C42 C41 1.3900 . ?
C41 C40 1.3900 . ?
C40 C45 1.3900 . ?
C45 C44 1.3900 . ?
C10 C9 1.29(4) . ?
C10 S3 1.67(4) . ?
C9 S2 1.77(5) . ?
S2 C11 1.76(2) . ?
C11 C11 1.23(2) 4_575 ?
C11 S3 1.83(2) . ?
C16 C17 1.3900 . ?
C16 C15 1.3900 . ?
C17 C18 1.3900 . ?
C18 C13 1.3900 . ?
C13 C14 1.3900 . ?
C13 C12 1.52(5) . ?
C14 C15 1.3900 . ?
C50 C51 1.53(4) . ?
C28 S7 1.76(3) . ?
C28 C29 1.39(3) . ?
S7 C30 1.85(2) . ?
C30 C30 1.145(19) 4_575 ?
C30 S6 1.78(2) . ?
S6 C29 1.69(3) . ?
C57 C54 1.44(3) . ?
C55 C56 1.3900 . ?
C55 C54 1.3900 . ?
C56 C51 1.3900 . ?
C51 C52 1.3900 . ?
C52 C53 1.3900 . ?
C53 C54 1.3900 . ?
C61 C62 1.66(4) . ?
C61 S9 1.66(4) . ?
C64 C65 1.3900 . ?
C64 C63 1.3900 . ?
C65 C66 1.3900 . ?
C65 C68 1.63(3) . ?
C66 C67 1.3900 . ?
C67 C62 1.3900 . ?
C62 C63 1.3900 . ?
C1A N1A 1.43(2) . ?
N1A C2A 1.45(2) . ?
N1A C3A 1.334(19) . ?
C3A O1A 1.22(2) . ?
C2B N1B 1.441(19) . ?
C3B N1B 1.331(19) . ?
C3B O1B 1.21(2) . ?
N1B C1B 1.437(19) . ?
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
0.9862 -4.9980 -0.9987 0.0158 0.1952 0.1763
-0.9862 4.9980 0.9987 -0.0158 -0.1952 -0.1763
4.0087 0.0194 5.0072 0.0899 0.3715 -0.4340
-4.0087 -0.0194 -5.0072 -0.0899 -0.3715 0.4340
2.0045 -1.0141 -4.9936 0.2646 -0.0459 0.2865
-2.0079 0.0150 4.9934 -0.2800 0.0825 -0.2580
3.0249 5.0009 1.0079 0.2308 -0.0025 -0.2936
-5.0221 -1.9920 2.9867 -0.4332 -0.0605 0.0135
-4.0101 1.0126 4.9890 -0.3879 -0.0504 -0.2278
5.0187 0.9929 -2.9870 0.4178 0.0970 0.0149
-5.0153 0.0062 2.9873 -0.4023 -0.1336 -0.0434
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.552 -0.832 -0.032 3950.9 928.6 ?
