#------------------------------------------------------------------------------
#$Date: 2023-12-04 18:33:55 +0200 (Mon, 04 Dec 2023) $
#$Revision: 288011 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/10/68/7106809.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_7106809
loop_
_publ_author_name
'Yao, Xiao-Qiang'
'Pan, Zhao-Rui'
'Hu, Jin-Song'
'Li, Yi-Zhi'
'Guo, Zi-Jian'
'Zheng, He-Gen'
_publ_section_title
;
 The rational synthesis of (10,3)-type MOFs based on tetranuclear [W(Mo)OS3Cu3]+
 secondary building units
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   36
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              10049
_journal_page_last               10051
_journal_paper_doi               10.1039/c1cc12691a
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety
'C27 H21.60 Br Cu3 N7 O1.30 S3 W, C3 H7 N O, 0.7(H2 O)'
_chemical_formula_sum            'C30 H30 Br Cu3 N8 O3 S3 W'
_chemical_formula_weight         1101.18
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 128.195(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   37.3848(11)
_cell_length_b                   9.3228(13)
_cell_length_c                   30.230(2)
_cell_measurement_reflns_used    5811
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      25.173
_cell_measurement_theta_min      2.179
_cell_volume                     8280.4(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_sigmaI/netI    0.0792
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21700
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    5.445
_exptl_absorpt_correction_T_max  0.34
_exptl_absorpt_correction_T_min  0.25
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             4272
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.025
_refine_diff_density_min         -1.059
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         8113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.05P)²+1.99P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1113
_reflns_number_gt                5543
_reflns_number_total             8113
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc12691a.txt
_cod_data_source_block           cluster2
_cod_original_cell_volume        8280.3(13)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7106809
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.1832(2) 1.1904(7) 0.7163(3) 0.0291(14) Uani 1 1 d . . .
C2 C -0.1253(2) 1.0159(8) 0.7763(3) 0.0397(17) Uani 1 1 d . . .
H2 H -0.1153 0.9358 0.7995 0.048 Uiso 1 1 calc R . .
C3 C -0.1674(2) 1.0748(8) 0.7525(3) 0.0404(17) Uani 1 1 d . . .
H3 H -0.1854 1.0363 0.7610 0.049 Uiso 1 1 calc R . .
C4 C -0.15454(19) 1.2547(7) 0.7071(3) 0.0353(16) Uani 1 1 d . . .
H4 H -0.1633 1.3387 0.6861 0.042 Uiso 1 1 calc R . .
C5 C -0.0984(2) 1.0782(7) 0.7649(3) 0.0362(16) Uani 1 1 d . . .
C6 C -0.1136(2) 1.1931(7) 0.7291(3) 0.0399(17) Uani 1 1 d . . .
H6 H -0.0959 1.2293 0.7199 0.048 Uiso 1 1 calc R . .
C7 C -0.0447(2) 0.8766(7) 0.7940(3) 0.0353(15) Uani 1 1 d . . .
H7 H -0.0648 0.8036 0.7863 0.042 Uiso 1 1 calc R . .
C8 C 0.0141(2) 0.9869(8) 0.8151(3) 0.0429(18) Uani 1 1 d . . .
H8 H 0.0424 1.0049 0.8242 0.051 Uiso 1 1 calc R . .
C9 C 0.1641(2) 1.1402(7) 0.4672(3) 0.0342(15) Uani 1 1 d . . .
H9 H 0.1719 1.2108 0.4935 0.041 Uiso 1 1 calc R . .
C10 C 0.1368(2) 1.0355(7) 0.3891(3) 0.0411(17) Uani 1 1 d . . .
H10 H 0.1221 1.0202 0.3510 0.049 Uiso 1 1 calc R . .
C11 C 0.1555(3) 0.9319(7) 0.4286(3) 0.0395(16) Uani 1 1 d . . .
H11 H 0.1561 0.8343 0.4228 0.047 Uiso 1 1 calc R . .
C12 C 0.1974(2) 0.9317(6) 0.5330(3) 0.0327(14) Uani 1 1 d . . .
C13 C 0.2233(3) 0.8135(8) 0.5448(3) 0.0427(18) Uani 1 1 d . . .
H13 H 0.2264 0.7791 0.5184 0.051 Uiso 1 1 calc R . .
C14 C 0.1961(2) 0.9920(6) 0.5745(3) 0.0281(14) Uani 1 1 d . . .
H14 H 0.1781 1.0718 0.5667 0.034 Uiso 1 1 calc R . .
C15 C 0.2226(2) 0.9293(6) 0.6281(3) 0.0338(15) Uani 1 1 d . . .
H15 H 0.2232 0.9715 0.6564 0.041 Uiso 1 1 calc R . .
C16 C 0.2446(2) 0.7457(6) 0.5951(3) 0.0328(15) Uani 1 1 d . . .
H16 H 0.2576 0.6561 0.5999 0.039 Uiso 1 1 calc R . .
C17 C 0.2479(2) 0.8060(7) 0.6401(3) 0.0333(15) Uani 1 1 d . . .
C18 C 0.2589(2) 0.7520(7) 0.7270(3) 0.0339(15) Uani 1 1 d . . .
C19 C 0.2225(3) 0.7859(8) 0.9053(4) 0.051(2) Uani 1 1 d . . .
H19 H 0.2315 0.8154 0.9402 0.061 Uiso 1 1 calc R . .
C20 C 0.18556(19) 0.6829(6) 0.8240(3) 0.0281(14) Uani 1 1 d . . .
H20 H 0.1644 0.6282 0.7924 0.034 Uiso 1 1 calc R . .
C21 C 0.2437(3) 0.8201(9) 0.8826(3) 0.0453(19) Uani 1 1 d . . .
H21 H 0.2694 0.8774 0.8992 0.054 Uiso 1 1 calc R . .
C22 C 0.2320(2) 0.7551(6) 0.7947(3) 0.0281(14) Uani 1 1 d . . .
C23 C 0.2026(2) 0.7098(8) 0.7397(3) 0.0388(17) Uani 1 1 d . . .
H23 H 0.1738 0.6775 0.7255 0.047 Uiso 1 1 calc R . .
C24 C 0.2753(3) 0.7987(8) 0.8161(3) 0.0453(18) Uani 1 1 d . . .
H24 H 0.2959 0.8267 0.8535 0.054 Uiso 1 1 calc R . .
C28 C 0.2879(3) 0.8006(8) 0.7819(4) 0.0454(19) Uani 1 1 d . . .
H28 H 0.3165 0.8353 0.7960 0.054 Uiso 1 1 calc R . .
C29 C 0.2151(2) 0.7112(7) 0.7042(3) 0.0400(17) Uani 1 1 d . . .
H29 H 0.1945 0.6853 0.6665 0.048 Uiso 1 1 calc R . .
C30 C -0.0165(2) 1.0865(8) 0.8018(3) 0.0423(18) Uani 1 1 d . . .
H30 H -0.0130 1.1854 0.8021 0.051 Uiso 1 1 calc R . .
C31 C 0.0880(2) 0.5082(8) 0.6755(3) 0.0355(16) Uani 1 1 d . . .
H31 H 0.0961 0.4264 0.6974 0.043 Uiso 1 1 calc R . .
C32 C 0.0535(3) 0.3334(8) 0.5974(4) 0.058(2) Uani 1 1 d . . .
H32A H 0.0792 0.2732 0.6234 0.087 Uiso 1 1 calc R . .
H32B H 0.0476 0.3322 0.5616 0.087 Uiso 1 1 calc R . .
H32C H 0.0273 0.2983 0.5929 0.087 Uiso 1 1 calc R . .
C33 C 0.0589(2) 0.6019(7) 0.5813(3) 0.0347(15) Uani 1 1 d . . .
H33A H 0.0341 0.6639 0.5705 0.052 Uiso 1 1 calc R . .
H33B H 0.0530 0.5607 0.5483 0.052 Uiso 1 1 calc R . .
H33C H 0.0866 0.6563 0.6014 0.052 Uiso 1 1 calc R . .
N1 N 0.1423(2) 1.1668(6) 0.4132(2) 0.0373(14) Uani 1 1 d . . .
N2 N 0.17404(19) 0.9987(5) 0.4804(2) 0.0304(12) Uani 1 1 d . . .
N3 N 0.27305(17) 0.7448(6) 0.6924(2) 0.0349(13) Uani 1 1 d . . .
N4 N 0.18450(19) 0.6976(6) 0.8663(2) 0.0367(14) Uani 1 1 d . . .
N5 N 0.22012(17) 0.7542(6) 0.8305(2) 0.0328(12) Uani 1 1 d . . .
N6 N -0.00175(18) 0.8569(6) 0.8134(3) 0.0363(13) Uani 1 1 d . . .
N7 N -0.05427(19) 1.0139(6) 0.7877(2) 0.0321(12) Uani 1 1 d . . .
N8 N 0.0635(2) 0.4819(7) 0.6192(3) 0.0425(14) Uani 1 1 d . . .
O1 O 0.06705(16) 0.2740(5) 0.8300(2) 0.0451(13) Uani 1 1 d . . .
O2 O 0.10108(16) 0.6200(5) 0.7019(2) 0.0449(13) Uani 1 1 d . . .
O3 O 0.0692(4) 0.9533(14) 0.5061(5) 0.062(4) Uani 0.40 1 d P . .
H3A H 0.0630 1.0195 0.4829 0.075 Uiso 0.40 1 d PR . .
H3C H 0.0620 0.8725 0.4895 0.075 Uiso 0.40 1 d PR . .
O4 O 0.1071(7) 0.951(2) 0.6057(8) 0.067(6) Uani 0.30 1 d P . .
H4A H 0.1351 0.9326 0.6231 0.080 Uiso 0.30 1 d PR . .
H4B H 0.1044 1.0308 0.6168 0.080 Uiso 0.30 1 d PR . .
O5 O 0.0821(5) 0.2361(16) 0.9634(6) 0.032(3) Uani 0.30 1 d P . .
H5D H 0.0876 0.1974 0.9925 0.039 Uiso 0.30 1 d PR . .
H5C H 0.0909 0.1807 0.9495 0.039 Uiso 0.30 1 d PR . .
Cu1 Cu 0.10688(3) 0.51506(9) 0.95871(4) 0.0443(2) Uani 1 1 d . . .
Cu2 Cu 0.13791(3) 0.64116(9) 0.87414(4) 0.0432(2) Uani 1 1 d . . .
Cu3 Cu 0.02557(3) 0.67188(9) 0.82316(4) 0.0438(2) Uani 1 1 d . . .
S1 S 0.15182(6) 0.46222(19) 0.93488(9) 0.0450(5) Uani 1 1 d . . .
S2 S 0.06565(6) 0.60498(19) 0.79339(9) 0.0448(5) Uani 1 1 d . . .
S3 S 0.03387(6) 0.49792(19) 0.88162(9) 0.0446(5) Uani 1 1 d . . .
W1 W 0.078283(10) 0.44275(3) 0.857176(15) 0.04338(11) Uani 1 1 d . . .
Br1 Br 0.12970(2) 0.57563(7) 1.04511(3) 0.04504(19) 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 0.0033 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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C3 C1 C4 119.2(6) . . ?
C3 C1 N3 118.5(6) . 3_455 ?
C4 C1 N3 122.2(6) . 3_455 ?
C3 C2 C5 118.5(6) . . ?
C3 C2 H2 120.7 . . ?
C5 C2 H2 120.7 . . ?
C2 C3 C1 121.0(6) . . ?
C2 C3 H3 119.5 . . ?
C1 C3 H3 119.5 . . ?
C6 C4 C1 119.2(6) . . ?
C6 C4 H4 120.4 . . ?
C1 C4 H4 120.4 . . ?
C6 C5 C2 120.9(6) . . ?
C6 C5 N7 119.4(6) . . ?
C2 C5 N7 119.6(6) . . ?
C4 C6 C5 120.7(7) . . ?
C4 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
N7 C7 N6 110.1(6) . . ?
N7 C7 H7 125.0 . . ?
N6 C7 H7 125.0 . . ?
C30 C8 N6 110.2(6) . . ?
C30 C8 H8 124.9 . . ?
N6 C8 H8 124.9 . . ?
N1 C9 N2 113.0(6) . . ?
N1 C9 H9 123.5 . . ?
N2 C9 H9 123.5 . . ?
C11 C10 N1 110.1(6) . . ?
C11 C10 H10 125.0 . . ?
N1 C10 H10 125.0 . . ?
C10 C11 N2 107.4(6) . . ?
C10 C11 H11 126.3 . . ?
N2 C11 H11 126.3 . . ?
C13 C12 N2 120.1(6) . . ?
C13 C12 C14 120.1(6) . . ?
N2 C12 C14 119.7(5) . . ?
C16 C13 C12 120.0(6) . . ?
C16 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C15 C14 C12 118.4(5) . . ?
C15 C14 H14 120.8 . . ?
C12 C14 H14 120.8 . . ?
C17 C15 C14 121.9(6) . . ?
C17 C15 H15 119.0 . . ?
C14 C15 H15 119.0 . . ?
C13 C16 C17 122.4(6) . . ?
C13 C16 H16 118.8 . . ?
C17 C16 H16 118.8 . . ?
N3 C17 C15 121.2(6) . . ?
N3 C17 C16 122.6(6) . . ?
C15 C17 C16 116.1(6) . . ?
C29 C18 C28 119.9(6) . . ?
C29 C18 N3 118.7(7) . . ?
C28 C18 N3 121.5(6) . . ?
C21 C19 N4 108.1(7) . . ?
C21 C19 H19 126.0 . . ?
N4 C19 H19 126.0 . . ?
N4 C20 N5 114.2(6) . . ?
N4 C20 H20 122.9 . . ?
N5 C20 H20 122.9 . . ?
C19 C21 N5 107.9(6) . . ?
C19 C21 H21 126.0 . . ?
N5 C21 H21 126.0 . . ?
C23 C22 C24 119.0(6) . . ?
C23 C22 N5 122.3(6) . . ?
C24 C22 N5 118.7(6) . . ?
C22 C23 C29 121.6(6) . . ?
C22 C23 H23 119.2 . . ?
C29 C23 H23 119.2 . . ?
C28 C24 C22 119.9(7) . . ?
C28 C24 H24 120.1 . . ?
C22 C24 H24 120.1 . . ?
C24 C28 C18 121.3(7) . . ?
C24 C28 H28 119.3 . . ?
C18 C28 H28 119.3 . . ?
C18 C29 C23 118.1(6) . . ?
C18 C29 H29 120.9 . . ?
C23 C29 H29 120.9 . . ?
C8 C30 N7 106.0(6) . . ?
C8 C30 H30 127.0 . . ?
N7 C30 H30 127.0 . . ?
O2 C31 N8 131.2(7) . . ?
O2 C31 H31 114.4 . . ?
N8 C31 H31 114.4 . . ?
N8 C32 H32A 109.5 . . ?
N8 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N8 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N8 C33 H33A 109.5 . . ?
N8 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N8 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C9 N1 C10 105.3(6) . . ?
C9 N1 Cu2 129.1(5) . 6_575 ?
C10 N1 Cu2 122.0(5) . 6_575 ?
C9 N2 C12 129.0(6) . . ?
C9 N2 C11 104.2(6) . . ?
C12 N2 C11 126.8(5) . . ?
C17 N3 C1 119.5(5) . 3_545 ?
C17 N3 C18 121.6(5) . . ?
C1 N3 C18 118.4(5) 3_545 . ?
C20 N4 C19 104.6(6) . . ?
C20 N4 Cu2 130.7(5) . . ?
C19 N4 Cu2 124.1(5) . . ?
C20 N5 C21 105.2(6) . . ?
C20 N5 C22 128.4(6) . . ?
C21 N5 C22 126.3(5) . . ?
C8 N6 C7 106.0(6) . . ?
C8 N6 Cu3 128.6(4) . . ?
C7 N6 Cu3 124.6(5) . . ?
C7 N7 C30 107.5(6) . . ?
C7 N7 C5 126.5(6) . . ?
C30 N7 C5 125.8(6) . . ?
C31 N8 C32 121.0(7) . . ?
C31 N8 C33 118.6(6) . . ?
C32 N8 C33 117.9(6) . . ?
H3A O3 H3C 109.5 . . ?
H4A O4 H4B 109.5 . . ?
H5D O5 H5C 109.5 . . ?
S3 Cu1 S1 108.71(8) . . ?
S3 Cu1 Br1 124.40(7) . . ?
S1 Cu1 Br1 126.89(7) . . ?
S3 Cu1 W1 54.28(6) . . ?
S1 Cu1 W1 54.43(6) . . ?
Br1 Cu1 W1 178.60(4) . . ?
N4 Cu2 N1 94.1(2) . 6_576 ?
N4 Cu2 S2 117.44(19) . . ?
N1 Cu2 S2 110.95(17) 6_576 . ?
N4 Cu2 S1 120.80(18) . . ?
N1 Cu2 S1 105.74(17) 6_576 . ?
S2 Cu2 S1 106.35(8) . . ?
N4 Cu2 W1 148.33(17) . . ?
N1 Cu2 W1 117.55(17) 6_576 . ?
S2 Cu2 W1 53.25(5) . . ?
S1 Cu2 W1 53.32(5) . . ?
N6 Cu3 S2 127.09(19) . . ?
N6 Cu3 S3 124.1(2) . . ?
S2 Cu3 S3 107.88(8) . . ?
N6 Cu3 W1 167.62(19) . . ?
S2 Cu3 W1 54.14(5) . . ?
S3 Cu3 W1 53.92(5) . . ?
Cu1 S1 W1 71.47(6) . . ?
Cu1 S1 Cu2 104.62(8) . . ?
W1 S1 Cu2 72.45(7) . . ?
W1 S2 Cu3 71.65(7) . . ?
W1 S2 Cu2 72.65(7) . . ?
Cu3 S2 Cu2 99.85(9) . . ?
Cu1 S3 W1 71.79(6) . . ?
Cu1 S3 Cu3 104.48(8) . . ?
W1 S3 Cu3 71.48(7) . . ?
O1 W1 S3 110.92(18) . . ?
O1 W1 S2 110.33(19) . . ?
S3 W1 S2 108.62(7) . . ?
O1 W1 S1 110.73(17) . . ?
S3 W1 S1 108.03(8) . . ?
S2 W1 S1 108.12(7) . . ?
O1 W1 Cu1 126.82(19) . . ?
S3 W1 Cu1 53.93(5) . . ?
S2 W1 Cu1 122.85(5) . . ?
S1 W1 Cu1 54.10(6) . . ?
O1 W1 Cu3 131.01(17) . . ?
S3 W1 Cu3 54.60(5) . . ?
S2 W1 Cu3 54.20(5) . . ?
S1 W1 Cu3 118.26(5) . . ?
Cu1 W1 Cu3 85.09(3) . . ?
O1 W1 Cu2 130.92(17) . . ?
S3 W1 Cu2 118.15(5) . . ?
S2 W1 Cu2 54.10(5) . . ?
S1 W1 Cu2 54.24(5) . . ?
Cu1 W1 Cu2 84.87(3) . . ?
Cu3 W1 Cu2 81.32(3) . . ?
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
C1 C3 1.382(9) . ?
C1 C4 1.397(8) . ?
C1 N3 1.413(7) 3_455 ?
C2 C3 1.376(10) . ?
C2 C5 1.380(9) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 C6 1.361(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.369(9) . ?
C5 N7 1.465(8) . ?
C6 H6 0.9300 . ?
C7 N7 1.311(8) . ?
C7 N6 1.338(8) . ?
C7 H7 0.9300 . ?
C8 C30 1.328(10) . ?
C8 N6 1.336(9) . ?
C8 H8 0.9300 . ?
C9 N1 1.322(9) . ?
C9 N2 1.362(8) . ?
C9 H9 0.9300 . ?
C10 C11 1.347(10) . ?
C10 N1 1.373(9) . ?
C10 H10 0.9300 . ?
C11 N2 1.405(8) . ?
C11 H11 0.9300 . ?
C12 C13 1.361(9) . ?
C12 N2 1.402(8) . ?
C12 C14 1.404(9) . ?
C13 C16 1.359(10) . ?
C13 H13 0.9300 . ?
C14 C15 1.401(9) . ?
C14 H14 0.9300 . ?
C15 C17 1.387(8) . ?
C15 H15 0.9300 . ?
C16 C17 1.407(10) . ?
C16 H16 0.9300 . ?
C17 N3 1.367(8) . ?
C18 C29 1.381(9) . ?
C18 C28 1.381(11) . ?
C18 N3 1.435(8) . ?
C19 C21 1.370(11) . ?
C19 N4 1.420(9) . ?
C19 H19 0.9300 . ?
C20 N4 1.310(8) . ?
C20 N5 1.356(8) . ?
C20 H20 0.9300 . ?
C21 N5 1.384(9) . ?
C21 H21 0.9300 . ?
C22 C23 1.376(9) . ?
C22 C24 1.382(10) . ?
C22 N5 1.401(8) . ?
C23 C29 1.411(10) . ?
C23 H23 0.9300 . ?
C24 C28 1.376(10) . ?
C24 H24 0.9300 . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 N7 1.375(8) . ?
C30 H30 0.9300 . ?
C31 O2 1.217(9) . ?
C31 N8 1.365(10) . ?
C31 H31 0.9300 . ?
C32 N8 1.480(9) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 N8 1.534(9) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
N1 Cu2 2.094(5) 6_575 ?
N3 C1 1.413(7) 3_545 ?
N4 Cu2 1.969(6) . ?
N6 Cu3 1.932(5) . ?
O1 W1 1.703(5) . ?
O3 H3A 0.8499 . ?
O3 H3C 0.8500 . ?
O4 H4A 0.8502 . ?
O4 H4B 0.8499 . ?
O5 H5D 0.8501 . ?
O5 H5C 0.8499 . ?
Cu1 S3 2.245(2) . ?
Cu1 S1 2.254(2) . ?
Cu1 Br1 2.2613(13) . ?
Cu1 W1 2.6381(11) . ?
Cu2 N1 2.094(5) 6_576 ?
Cu2 S2 2.284(2) . ?
Cu2 S1 2.290(2) . ?
Cu2 W1 2.6907(9) . ?
Cu3 S2 2.260(2) . ?
Cu3 S3 2.274(2) . ?
Cu3 W1 2.6453(9) . ?
S1 W1 2.2632(19) . ?
S2 W1 2.259(2) . ?
S3 W1 2.255(2) . ?
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
C5 C2 C3 C1 2.5(12) . . . . ?
C4 C1 C3 C2 -4.9(11) . . . . ?
N3 C1 C3 C2 178.9(7) 3_455 . . . ?
C3 C1 C4 C6 7.0(11) . . . . ?
N3 C1 C4 C6 -176.9(7) 3_455 . . . ?
C3 C2 C5 C6 -2.3(12) . . . . ?
C3 C2 C5 N7 -177.4(7) . . . . ?
C1 C4 C6 C5 -6.9(12) . . . . ?
C2 C5 C6 C4 4.6(12) . . . . ?
N7 C5 C6 C4 179.7(7) . . . . ?
N1 C10 C11 N2 -0.1(8) . . . . ?
N2 C12 C13 C16 -177.7(6) . . . . ?
C14 C12 C13 C16 6.1(11) . . . . ?
C13 C12 C14 C15 1.1(9) . . . . ?
N2 C12 C14 C15 -175.1(6) . . . . ?
C12 C14 C15 C17 -3.4(10) . . . . ?
C12 C13 C16 C17 -11.4(11) . . . . ?
C14 C15 C17 N3 -179.0(6) . . . . ?
C14 C15 C17 C16 -1.4(9) . . . . ?
C13 C16 C17 N3 -173.5(7) . . . . ?
C13 C16 C17 C15 8.9(10) . . . . ?
N4 C19 C21 N5 -0.6(9) . . . . ?
C24 C22 C23 C29 -2.0(10) . . . . ?
N5 C22 C23 C29 -179.9(6) . . . . ?
C23 C22 C24 C28 2.0(10) . . . . ?
N5 C22 C24 C28 180.0(6) . . . . ?
C22 C24 C28 C18 -3.7(11) . . . . ?
C29 C18 C28 C24 5.2(11) . . . . ?
N3 C18 C28 C24 -175.8(6) . . . . ?
C28 C18 C29 C23 -5.0(10) . . . . ?
N3 C18 C29 C23 175.9(6) . . . . ?
C22 C23 C29 C18 3.5(11) . . . . ?
N6 C8 C30 N7 -4.0(9) . . . . ?
N2 C9 N1 C10 1.1(8) . . . . ?
N2 C9 N1 Cu2 -157.3(5) . . . 6_575 ?
C11 C10 N1 C9 -0.6(8) . . . . ?
C11 C10 N1 Cu2 159.7(5) . . . 6_575 ?
N1 C9 N2 C12 178.7(6) . . . . ?
N1 C9 N2 C11 -1.1(8) . . . . ?
C13 C12 N2 C9 -147.4(7) . . . . ?
C14 C12 N2 C9 28.8(10) . . . . ?
C13 C12 N2 C11 32.4(10) . . . . ?
C14 C12 N2 C11 -151.4(6) . . . . ?
C10 C11 N2 C9 0.7(8) . . . . ?
C10 C11 N2 C12 -179.1(6) . . . . ?
C15 C17 N3 C1 -139.2(7) . . . 3_545 ?
C16 C17 N3 C1 43.3(10) . . . 3_545 ?
C15 C17 N3 C18 32.0(10) . . . . ?
C16 C17 N3 C18 -145.4(7) . . . . ?
C29 C18 N3 C17 51.1(9) . . . . ?
C28 C18 N3 C17 -127.9(7) . . . . ?
C29 C18 N3 C1 -137.6(7) . . . 3_545 ?
C28 C18 N3 C1 43.4(9) . . . 3_545 ?
N5 C20 N4 C19 -0.9(7) . . . . ?
N5 C20 N4 Cu2 170.4(4) . . . . ?
C21 C19 N4 C20 0.9(8) . . . . ?
C21 C19 N4 Cu2 -171.2(5) . . . . ?
N4 C20 N5 C21 0.6(8) . . . . ?
N4 C20 N5 C22 176.7(6) . . . . ?
C19 C21 N5 C20 0.0(8) . . . . ?
C19 C21 N5 C22 -176.2(6) . . . . ?
C23 C22 N5 C20 16.9(10) . . . . ?
C24 C22 N5 C20 -161.0(6) . . . . ?
C23 C22 N5 C21 -167.8(7) . . . . ?
C24 C22 N5 C21 14.3(10) . . . . ?
C30 C8 N6 C7 5.1(9) . . . . ?
C30 C8 N6 Cu3 175.0(6) . . . . ?
N7 C7 N6 C8 -4.2(9) . . . . ?
N7 C7 N6 Cu3 -174.6(5) . . . . ?
N6 C7 N7 C30 1.8(8) . . . . ?
N6 C7 N7 C5 176.8(6) . . . . ?
C8 C30 N7 C7 1.3(9) . . . . ?
C8 C30 N7 C5 -173.7(7) . . . . ?
C6 C5 N7 C7 -139.2(8) . . . . ?
C2 C5 N7 C7 36.0(11) . . . . ?
C6 C5 N7 C30 34.9(11) . . . . ?
C2 C5 N7 C30 -149.9(7) . . . . ?
O2 C31 N8 C32 177.0(7) . . . . ?
O2 C31 N8 C33 15.6(10) . . . . ?
C20 N4 Cu2 N1 -137.0(6) . . . 6_576 ?
C19 N4 Cu2 N1 32.9(6) . . . 6_576 ?
C20 N4 Cu2 S2 -20.8(6) . . . . ?
C19 N4 Cu2 S2 149.1(5) . . . . ?
C20 N4 Cu2 S1 111.9(6) . . . . ?
C19 N4 Cu2 S1 -78.2(6) . . . . ?
C20 N4 Cu2 W1 42.9(8) . . . . ?
C19 N4 Cu2 W1 -147.2(5) . . . . ?
C8 N6 Cu3 S2 -37.0(8) . . . . ?
C7 N6 Cu3 S2 131.2(5) . . . . ?
C8 N6 Cu3 S3 130.8(6) . . . . ?
C7 N6 Cu3 S3 -61.0(7) . . . . ?
C8 N6 Cu3 W1 54.1(13) . . . . ?
C7 N6 Cu3 W1 -137.7(7) . . . . ?
S3 Cu1 S1 W1 -0.52(7) . . . . ?
Br1 Cu1 S1 W1 179.43(6) . . . . ?
S3 Cu1 S1 Cu2 64.88(9) . . . . ?
Br1 Cu1 S1 Cu2 -115.17(8) . . . . ?
W1 Cu1 S1 Cu2 65.40(7) . . . . ?
N4 Cu2 S1 Cu1 153.0(2) . . . . ?
N1 Cu2 S1 Cu1 48.20(19) 6_576 . . . ?
S2 Cu2 S1 Cu1 -69.83(10) . . . . ?
W1 Cu2 S1 Cu1 -64.72(6) . . . . ?
N4 Cu2 S1 W1 -142.3(2) . . . . ?
N1 Cu2 S1 W1 112.91(17) 6_576 . . . ?
S2 Cu2 S1 W1 -5.11(8) . . . . ?
N6 Cu3 S2 W1 164.7(2) . . . . ?
S3 Cu3 S2 W1 -4.70(7) . . . . ?
N6 Cu3 S2 Cu2 96.8(2) . . . . ?
S3 Cu3 S2 Cu2 -72.59(9) . . . . ?
W1 Cu3 S2 Cu2 -67.88(6) . . . . ?
N4 Cu2 S2 W1 144.01(18) . . . . ?
N1 Cu2 S2 W1 -109.40(18) 6_576 . . . ?
S1 Cu2 S2 W1 5.12(8) . . . . ?
N4 Cu2 S2 Cu3 -148.88(19) . . . . ?
N1 Cu2 S2 Cu3 -42.29(19) 6_576 . . . ?
S1 Cu2 S2 Cu3 72.23(9) . . . . ?
W1 Cu2 S2 Cu3 67.11(6) . . . . ?
S1 Cu1 S3 W1 0.52(7) . . . . ?
Br1 Cu1 S3 W1 -179.43(5) . . . . ?
S1 Cu1 S3 Cu3 -63.99(9) . . . . ?
Br1 Cu1 S3 Cu3 116.06(8) . . . . ?
W1 Cu1 S3 Cu3 -64.51(7) . . . . ?
N6 Cu3 S3 Cu1 -100.3(2) . . . . ?
S2 Cu3 S3 Cu1 69.44(10) . . . . ?
W1 Cu3 S3 Cu1 64.73(6) . . . . ?
N6 Cu3 S3 W1 -165.0(2) . . . . ?
S2 Cu3 S3 W1 4.72(7) . . . . ?
Cu1 S3 W1 O1 121.01(19) . . . . ?
Cu3 S3 W1 O1 -126.16(19) . . . . ?
Cu1 S3 W1 S2 -117.56(7) . . . . ?
Cu3 S3 W1 S2 -4.74(7) . . . . ?
Cu1 S3 W1 S1 -0.52(7) . . . . ?
Cu3 S3 W1 S1 112.31(6) . . . . ?
Cu3 S3 W1 Cu1 112.82(6) . . . . ?
Cu1 S3 W1 Cu3 -112.82(6) . . . . ?
Cu1 S3 W1 Cu2 -58.99(7) . . . . ?
Cu3 S3 W1 Cu2 53.83(7) . . . . ?
Cu3 S2 W1 O1 126.55(18) . . . . ?
Cu2 S2 W1 O1 -126.45(17) . . . . ?
Cu3 S2 W1 S3 4.77(7) . . . . ?
Cu2 S2 W1 S3 111.77(7) . . . . ?
Cu3 S2 W1 S1 -112.23(7) . . . . ?
Cu2 S2 W1 S1 -5.23(8) . . . . ?
Cu3 S2 W1 Cu1 -53.77(6) . . . . ?
Cu2 S2 W1 Cu1 53.23(7) . . . . ?
Cu2 S2 W1 Cu3 107.00(7) . . . . ?
Cu3 S2 W1 Cu2 -107.00(7) . . . . ?
Cu1 S1 W1 O1 -121.1(2) . . . . ?
Cu2 S1 W1 O1 126.2(2) . . . . ?
Cu1 S1 W1 S3 0.52(7) . . . . ?
Cu2 S1 W1 S3 -112.15(7) . . . . ?
Cu1 S1 W1 S2 117.89(7) . . . . ?
Cu2 S1 W1 S2 5.22(8) . . . . ?
Cu2 S1 W1 Cu1 -112.67(6) . . . . ?
Cu1 S1 W1 Cu3 59.41(7) . . . . ?
Cu2 S1 W1 Cu3 -53.26(7) . . . . ?
Cu1 S1 W1 Cu2 112.67(7) . . . . ?
S3 Cu1 W1 O1 -90.4(2) . . . . ?
S1 Cu1 W1 O1 90.2(2) . . . . ?
Br1 Cu1 W1 O1 -70.7(19) . . . . ?
S1 Cu1 W1 S3 -179.39(9) . . . . ?
Br1 Cu1 W1 S3 19.7(19) . . . . ?
S3 Cu1 W1 S2 89.99(8) . . . . ?
S1 Cu1 W1 S2 -89.40(8) . . . . ?
Br1 Cu1 W1 S2 109.7(19) . . . . ?
S3 Cu1 W1 S1 179.39(9) . . . . ?
Br1 Cu1 W1 S1 -160.9(19) . . . . ?
S3 Cu1 W1 Cu3 48.94(6) . . . . ?
S1 Cu1 W1 Cu3 -130.45(6) . . . . ?
Br1 Cu1 W1 Cu3 68.6(19) . . . . ?
S3 Cu1 W1 Cu2 130.65(6) . . . . ?
S1 Cu1 W1 Cu2 -48.75(6) . . . . ?
Br1 Cu1 W1 Cu2 150.3(19) . . . . ?
N6 Cu3 W1 O1 173.1(9) . . . . ?
S2 Cu3 W1 O1 -86.6(2) . . . . ?
S3 Cu3 W1 O1 87.9(3) . . . . ?
N6 Cu3 W1 S3 85.3(9) . . . . ?
S2 Cu3 W1 S3 -174.46(9) . . . . ?
N6 Cu3 W1 S2 -100.3(9) . . . . ?
S3 Cu3 W1 S2 174.46(9) . . . . ?
N6 Cu3 W1 S1 -7.5(9) . . . . ?
S2 Cu3 W1 S1 92.73(9) . . . . ?
S3 Cu3 W1 S1 -92.82(9) . . . . ?
N6 Cu3 W1 Cu1 36.9(9) . . . . ?
S2 Cu3 W1 Cu1 137.15(6) . . . . ?
S3 Cu3 W1 Cu1 -48.40(6) . . . . ?
N6 Cu3 W1 Cu2 -48.7(9) . . . . ?
S2 Cu3 W1 Cu2 51.60(6) . . . . ?
S3 Cu3 W1 Cu2 -133.95(6) . . . . ?
N4 Cu2 W1 O1 3.2(4) . . . . ?
N1 Cu2 W1 O1 -176.9(3) 6_576 . . . ?
S2 Cu2 W1 O1 86.6(2) . . . . ?
S1 Cu2 W1 O1 -87.3(2) . . . . ?
N4 Cu2 W1 S3 -176.8(3) . . . . ?
N1 Cu2 W1 S3 3.12(19) 6_576 . . . ?
S2 Cu2 W1 S3 -93.42(9) . . . . ?
S1 Cu2 W1 S3 92.71(9) . . . . ?
N4 Cu2 W1 S2 -83.4(3) . . . . ?
N1 Cu2 W1 S2 96.53(19) 6_576 . . . ?
S1 Cu2 W1 S2 -173.87(9) . . . . ?
N4 Cu2 W1 S1 90.5(3) . . . . ?
N1 Cu2 W1 S1 -89.59(19) 6_576 . . . ?
S2 Cu2 W1 S1 173.87(9) . . . . ?
N4 Cu2 W1 Cu1 139.1(3) . . . . ?
N1 Cu2 W1 Cu1 -40.96(18) 6_576 . . . ?
S2 Cu2 W1 Cu1 -137.49(7) . . . . ?
S1 Cu2 W1 Cu1 48.64(7) . . . . ?
N4 Cu2 W1 Cu3 -135.1(3) . . . . ?
N1 Cu2 W1 Cu3 44.85(18) 6_576 . . . ?
S2 Cu2 W1 Cu3 -51.69(7) . . . . ?
S1 Cu2 W1 Cu3 134.44(7) . . . . ?
