#------------------------------------------------------------------------------
#$Date: 2019-11-17 08:28:53 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228859 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/97/1549730.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_1549730
loop_
_publ_author_name
'Yu, Fei'
'Kurmoo, Mohamedally'
'Zhuang, Gui-Lin'
'Zuo, Jing-Lin'
_publ_section_title
;
 Hierarchical tandem assembly of planar [3× 3] building units into
 {3× [3× 3]} oligomers: mixed-valency, electrical conductivity
 and magnetism.
;
_journal_issue                   38
_journal_name_full               'Chemical science'
_journal_page_first              7498
_journal_page_last               7504
_journal_paper_doi               10.1039/c8sc02851f
_journal_volume                  9
_journal_year                    2018
_chemical_formula_sum            'C98 H60 Cu9 N36 O6 S'
_chemical_formula_weight         2441.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-05-21 deposited with the CCDC.
2018-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.970(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.700(18)
_cell_length_b                   10.890(6)
_cell_length_c                   30.813(17)
_cell_measurement_reflns_used    6095
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.03
_cell_measurement_theta_min      2.29
_cell_volume                     9947(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker D8 ADVANCE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0694
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            33019
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.540
_diffrn_reflns_theta_min         1.374
_exptl_absorpt_coefficient_mu    1.979
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_description       block
_exptl_crystal_F_000             4900
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_refine_diff_density_max         1.181
_refine_diff_density_min         -1.073
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         11089
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1236
_refine_ls_R_factor_gt           0.0696
_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)+(0.1032P)²+51.1929P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1833
_refine_ls_wR_factor_ref         0.2138
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6476
_reflns_number_total             11089
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8sc02851f2.cif
_cod_data_source_block           Cu9
_cod_depositor_comments
'Adding full bibliography for 1549730--1549731.cif.'
_cod_original_cell_volume        9947(9)
_cod_database_code               1549730
_shelx_shelxl_version_number     2018/3
_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_min   0.693
_shelx_estimated_absorpt_t_max   0.742
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cu1 Cu 0.37192(2) 0.66046(7) 0.20798(3) 0.0386(2) Uani 1 1 d . . .
Cu2 Cu 0.500000 0.80522(13) 0.250000 0.0545(3) Uani 1 2 d S T P
Cu3 Cu 0.62100(2) 0.94726(7) 0.26247(3) 0.0419(2) Uani 1 1 d . . .
Cu4 Cu 0.500000 1.09105(11) 0.250000 0.0506(3) Uani 1 2 d S T P
Cu5 Cu 0.75108(3) 0.80388(8) 0.30470(3) 0.0513(2) Uani 1 1 d . . .
Cu6 Cu 0.500000 0.51268(12) 0.250000 0.0518(3) Uani 1 2 d S T P
N1 N 0.32451(16) 0.6498(5) 0.13958(19) 0.0425(12) Uani 1 1 d . . .
N2 N 0.40712(15) 0.7212(4) 0.17587(17) 0.0362(11) Uani 1 1 d . . .
N3 N 0.44957(15) 0.7569(4) 0.18962(17) 0.0343(11) Uani 1 1 d . . .
N4 N 0.52637(15) 0.8518(5) 0.20616(17) 0.0370(11) Uani 1 1 d . . .
N5 N 0.56750(15) 0.8883(4) 0.21087(18) 0.0371(11) Uani 1 1 d . . .
N6 N 0.64137(16) 0.9575(4) 0.20914(19) 0.0381(11) Uani 1 1 d . . .
N7 N 0.48659(19) 1.1549(5) 0.3058(2) 0.0554(15) Uani 1 1 d . . .
N8 N 0.55798(17) 1.0637(5) 0.3018(2) 0.0455(13) Uani 1 1 d . . .
N9 N 0.59839(16) 1.0269(5) 0.3054(2) 0.0423(12) Uani 1 1 d . . .
N10 N 0.67639(16) 0.9516(5) 0.32022(19) 0.0415(12) Uani 1 1 d . . .
N11 N 0.71955(16) 0.9168(4) 0.33240(19) 0.0404(12) Uani 1 1 d . . .
N12 N 0.80133(17) 0.8247(5) 0.3717(2) 0.0480(13) Uani 1 1 d . . .
N13 N 0.22763(17) 0.7956(4) 0.2489(2) 0.0459(13) Uani 1 1 d . . .
N14 N 0.29652(16) 0.6918(4) 0.24049(19) 0.0385(11) Uani 1 1 d . . .
N15 N 0.33810(15) 0.6544(4) 0.24658(18) 0.0355(11) Uani 1 1 d . . .
N16 N 0.41727(17) 0.5806(5) 0.26548(19) 0.0435(12) Uani 1 1 d . . .
N17 N 0.46030(17) 0.5425(5) 0.28028(19) 0.0436(12) Uani 1 1 d . . .
N18 N 0.54091(19) 0.4532(5) 0.3178(2) 0.0532(15) Uani 1 1 d . . .
C1 C 0.2826(2) 0.6101(7) 0.1253(3) 0.0590(19) Uani 1 1 d . . .
H1 H 0.271984 0.587822 0.148557 0.071 Uiso 1 1 calc R U .
C2 C 0.2542(3) 0.6003(9) 0.0774(3) 0.078(3) Uani 1 1 d . . .
H2 H 0.224304 0.570472 0.067771 0.094 Uiso 1 1 calc R U .
C3 C 0.2688(3) 0.6334(9) 0.0440(3) 0.076(2) Uani 1 1 d . . .
H3 H 0.248909 0.629967 0.010912 0.091 Uiso 1 1 calc R U .
C45 C 0.5473(2) 0.4527(6) 0.3974(3) 0.0580(19) Uani 1 1 d . . .
H45 H 0.534115 0.467265 0.419165 0.070 Uiso 1 1 calc R U .
C4 C 0.3131(2) 0.6723(7) 0.0582(3) 0.0599(19) Uani 1 1 d . . .
H4 H 0.324459 0.691820 0.035372 0.072 Uiso 1 1 calc R U .
C5 C 0.33999(19) 0.6818(5) 0.1068(2) 0.0415(14) Uani 1 1 d . . .
C6 C 0.3867(2) 0.7213(5) 0.1280(2) 0.0367(13) Uani 1 1 d . . .
C7 C 0.4174(2) 0.7606(6) 0.1105(2) 0.0418(14) Uani 1 1 d . . .
H7 H 0.412328 0.770211 0.077964 0.050 Uiso 1 1 calc R U .
C8 C 0.45622(19) 0.7823(5) 0.1502(2) 0.0333(12) Uani 1 1 d . . .
C9 C 0.50107(19) 0.8273(5) 0.1602(2) 0.0345(13) Uani 1 1 d . . .
C10 C 0.5259(2) 0.8523(6) 0.1337(2) 0.0402(14) Uani 1 1 d . . .
H10 H 0.516376 0.845147 0.100135 0.048 Uiso 1 1 calc R U .
C11 C 0.56704(19) 0.8892(5) 0.1672(2) 0.0362(13) Uani 1 1 d . . .
C12 C 0.60904(19) 0.9282(5) 0.1660(2) 0.0357(13) Uani 1 1 d . . .
C13 C 0.6169(2) 0.9353(6) 0.1256(3) 0.0531(17) Uani 1 1 d . . .
H13 H 0.593769 0.915677 0.095034 0.064 Uiso 1 1 calc R U .
C14 C 0.6592(3) 0.9713(8) 0.1300(3) 0.069(2) Uani 1 1 d . . .
H14 H 0.665619 0.975001 0.102736 0.083 Uiso 1 1 calc R U .
C15 C 0.6912(2) 1.0012(7) 0.1739(3) 0.061(2) Uani 1 1 d . . .
H15 H 0.720098 1.027949 0.177423 0.073 Uiso 1 1 calc R U .
C16 C 0.6818(2) 0.9928(6) 0.2129(3) 0.0484(16) Uani 1 1 d . . .
H16 H 0.704706 1.012587 0.243587 0.058 Uiso 1 1 calc R U .
C17 C 0.4475(3) 1.1974(7) 0.3040(4) 0.067(2) Uani 1 1 d . . .
H17 H 0.423213 1.211517 0.273684 0.081 Uiso 1 1 calc R U .
C19 C 0.4767(3) 1.2002(8) 0.3883(4) 0.085(3) Uani 1 1 d . . .
H19 H 0.472752 1.215269 0.416633 0.102 Uiso 1 1 calc R U .
C20 C 0.5179(3) 1.1575(7) 0.3914(3) 0.067(2) Uani 1 1 d . . .
H20 H 0.542596 1.142916 0.421447 0.080 Uiso 1 1 calc R U .
C21 C 0.5214(2) 1.1374(5) 0.3487(3) 0.0493(17) Uani 1 1 d . . .
C22 C 0.5626(2) 1.0929(5) 0.3459(2) 0.0414(15) Uani 1 1 d . . .
C23 C 0.6063(2) 1.0744(5) 0.3785(2) 0.0440(15) Uani 1 1 d . . .
H23 H 0.618813 1.086944 0.412192 0.053 Uiso 1 1 calc R U .
C24 C 0.6281(2) 1.0335(5) 0.3514(2) 0.0399(14) Uani 1 1 d . . .
C25 C 0.6733(2) 0.9924(5) 0.3603(2) 0.0395(14) Uani 1 1 d . . .
C26 C 0.7142(2) 0.9857(6) 0.3982(2) 0.0440(15) Uani 1 1 d . . .
H26 H 0.721980 1.009327 0.430415 0.053 Uiso 1 1 calc R U .
C27 C 0.74235(19) 0.9356(5) 0.3787(2) 0.0395(14) Uani 1 1 d . . .
C28 C 0.7894(2) 0.8989(6) 0.3998(3) 0.0493(16) Uani 1 1 d . . .
C29 C 0.8204(3) 0.9373(9) 0.4439(3) 0.080(3) Uani 1 1 d . . .
H29 H 0.811580 0.989210 0.463284 0.097 Uiso 1 1 calc R U .
C30 C 0.8646(3) 0.8987(12) 0.4595(4) 0.111(4) Uani 1 1 d . . .
H30 H 0.886436 0.923192 0.490123 0.133 Uiso 1 1 calc R U .
C31 C 0.8769(3) 0.8270(11) 0.4316(4) 0.111(4) Uani 1 1 d . . .
H31 H 0.907159 0.800091 0.441983 0.134 Uiso 1 1 calc R U .
C32 C 0.8448(3) 0.7940(8) 0.3882(3) 0.077(3) Uani 1 1 d . . .
H32 H 0.853821 0.745542 0.368113 0.092 Uiso 1 1 calc R U .
C33 C 0.1895(2) 0.8417(7) 0.2490(3) 0.062(2) Uani 1 1 d . . .
H33 H 0.169036 0.884406 0.221528 0.074 Uiso 1 1 calc R U .
C34 C 0.1792(3) 0.8289(7) 0.2878(4) 0.077(3) Uani 1 1 d . . .
H34 H 0.152524 0.864740 0.287198 0.092 Uiso 1 1 calc R U .
C35 C 0.2067(3) 0.7663(7) 0.3260(3) 0.070(2) Uani 1 1 d . . .
H35 H 0.199609 0.756346 0.352657 0.084 Uiso 1 1 calc R U .
C36 C 0.2464(2) 0.7149(6) 0.3267(3) 0.0541(18) Uani 1 1 d . . .
H36 H 0.266569 0.670168 0.353729 0.065 Uiso 1 1 calc R U .
C37 C 0.25538(19) 0.7307(5) 0.2875(2) 0.0394(14) Uani 1 1 d . . .
C38 C 0.2953(2) 0.6820(5) 0.2836(2) 0.0378(14) Uani 1 1 d . . .
C39 C 0.3356(2) 0.6370(5) 0.3173(2) 0.0389(14) Uani 1 1 d . . .
H39 H 0.343490 0.620580 0.350164 0.047 Uiso 1 1 calc R U .
C40 C 0.36185(19) 0.6211(5) 0.2926(2) 0.0350(13) Uani 1 1 d . . .
C41 C 0.40741(19) 0.5782(5) 0.3037(2) 0.0367(13) Uani 1 1 d . . .
C42 C 0.4440(2) 0.5383(5) 0.3439(2) 0.0408(14) Uani 1 1 d . . .
H42 H 0.446254 0.527421 0.375371 0.049 Uiso 1 1 calc R U .
C43 C 0.4769(2) 0.5179(5) 0.3273(2) 0.0409(14) Uani 1 1 d . . .
C44 C 0.5236(2) 0.4727(5) 0.3495(2) 0.0416(15) Uani 1 1 d . . .
C18 C 0.4414(3) 1.2209(7) 0.3441(4) 0.081(3) Uani 1 1 d . . .
H18 H 0.413353 1.251064 0.341786 0.098 Uiso 1 1 calc R U .
C46 C 0.5907(3) 0.4109(7) 0.4132(3) 0.071(2) Uani 1 1 d . . .
H46 H 0.607823 0.395269 0.446325 0.085 Uiso 1 1 calc R U .
C47 C 0.6095(3) 0.3914(7) 0.3820(4) 0.067(2) Uani 1 1 d . . .
H47 H 0.639757 0.363797 0.392884 0.081 Uiso 1 1 calc R U .
C48 C 0.5837(2) 0.4125(7) 0.3351(3) 0.063(2) Uani 1 1 d . . .
H48 H 0.596542 0.397824 0.313074 0.076 Uiso 1 1 calc R U .
S1 S 0.4951(3) 0.5782(9) 0.4920(3) 0.132(2) Uani 0.5 1 d D U P
O1 O 0.5167(7) 0.681(2) 0.4803(10) 0.199(6) Uani 0.5 1 d D U P
O2 O 0.4517(6) 0.621(2) 0.4899(10) 0.207(6) Uani 0.5 1 d D U P
O3 O 0.5201(5) 0.5323(14) 0.5389(5) 0.214(5) Uani 1 1 d . U .
O4 O 0.7038(6) 1.2083(15) 0.5150(6) 0.242(6) Uani 1 1 d D U .
C49 C 0.7266(8) 1.272(3) 0.4910(10) 0.276(11) Uani 1 1 d D U .
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'
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'
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
N2 Cu1 N15 161.4(2) . .
N2 Cu1 N16 103.1(2) . .
N15 Cu1 N16 80.8(2) . .
N2 Cu1 N1 81.1(2) . .
N15 Cu1 N1 104.6(2) . .
N16 Cu1 N1 150.0(2) . .
N4 Cu2 N4 149.9(3) 2_655 .
N4 Cu2 N3 106.58(19) 2_655 .
N4 Cu2 N3 81.58(19) . .
N4 Cu2 N3 81.58(19) 2_655 2_655
N4 Cu2 N3 106.58(19) . 2_655
N3 Cu2 N3 149.0(3) . 2_655
N5 Cu3 N10 161.4(2) . .
N5 Cu3 N9 103.6(2) . .
N10 Cu3 N9 80.9(2) . .
N5 Cu3 N6 80.9(2) . .
N10 Cu3 N6 104.2(2) . .
N9 Cu3 N6 150.3(2) . .
N8 Cu4 N8 162.2(3) . 2_655
N8 Cu4 N7 105.2(2) . 2_655
N8 Cu4 N7 80.9(2) 2_655 2_655
N8 Cu4 N7 80.9(2) . .
N8 Cu4 N7 105.2(2) 2_655 .
N7 Cu4 N7 140.6(3) 2_655 .
N14 Cu5 N11 106.3(2) 2_655 .
N14 Cu5 N12 146.0(2) 2_655 .
N11 Cu5 N12 80.8(2) . .
N14 Cu5 N13 80.9(2) 2_655 2_655
N11 Cu5 N13 141.2(2) . 2_655
N12 Cu5 N13 114.7(2) . 2_655
N17 Cu6 N17 160.5(3) . 2_655
N17 Cu6 N18 105.3(2) . 2_655
N17 Cu6 N18 81.0(2) 2_655 2_655
N17 Cu6 N18 81.0(2) . .
N17 Cu6 N18 105.3(2) 2_655 .
N18 Cu6 N18 143.2(3) 2_655 .
C1 N1 C5 119.9(6) . .
C1 N1 Cu1 126.5(5) . .
C5 N1 Cu1 113.5(4) . .
N3 N2 C6 108.7(4) . .
N3 N2 Cu1 135.1(4) . .
C6 N2 Cu1 116.0(4) . .
N2 N3 C8 108.5(5) . .
N2 N3 Cu2 136.6(4) . .
C8 N3 Cu2 114.1(4) . .
C9 N4 N5 108.5(4) . .
C9 N4 Cu2 115.2(4) . .
N5 N4 Cu2 135.5(4) . .
C11 N5 N4 107.8(5) . .
C11 N5 Cu3 116.8(4) . .
N4 N5 Cu3 135.1(4) . .
C16 N6 C12 119.5(5) . .
C16 N6 Cu3 126.9(5) . .
C12 N6 Cu3 113.6(3) . .
C17 N7 C21 119.0(7) . .
C17 N7 Cu4 128.1(6) . .
C21 N7 Cu4 112.5(4) . .
N9 N8 C22 107.6(5) . .
N9 N8 Cu4 135.2(4) . .
C22 N8 Cu4 117.0(4) . .
N8 N9 C24 108.6(5) . .
N8 N9 Cu3 135.5(4) . .
C24 N9 Cu3 115.1(4) . .
C25 N10 N11 108.0(5) . .
C25 N10 Cu3 116.5(4) . .
N11 N10 Cu3 135.4(4) . .
C27 N11 N10 107.7(5) . .
C27 N11 Cu5 113.4(4) . .
N10 N11 Cu5 135.7(4) . .
C32 N12 C28 116.9(6) . .
C32 N12 Cu5 129.2(5) . .
C28 N12 Cu5 112.8(4) . .
C33 N13 C37 118.1(6) . .
C33 N13 Cu5 128.1(5) . 2_655
C37 N13 Cu5 113.7(4) . 2_655
N15 N14 C38 106.5(5) . .
N15 N14 Cu5 135.9(4) . 2_655
C38 N14 Cu5 113.2(4) . 2_655
N14 N15 C40 109.0(4) . .
N14 N15 Cu1 134.8(4) . .
C40 N15 Cu1 115.5(4) . .
C41 N16 N17 107.4(5) . .
C41 N16 Cu1 115.4(4) . .
N17 N16 Cu1 136.2(4) . .
C43 N17 N16 108.4(5) . .
C43 N17 Cu6 116.3(4) . .
N16 N17 Cu6 135.3(4) . .
C44 N18 C48 117.0(7) . .
C44 N18 Cu6 113.4(4) . .
C48 N18 Cu6 129.0(5) . .
N1 C1 C2 121.2(7) . .
N1 C1 H1 119.4 . .
C2 C1 H1 119.4 . .
C3 C2 C1 119.9(7) . .
C3 C2 H2 120.0 . .
C1 C2 H2 120.0 . .
C2 C3 C4 119.7(8) . .
C2 C3 H3 120.1 . .
C4 C3 H3 120.1 . .
C44 C45 C46 117.9(8) . .
C44 C45 H45 121.1 . .
C46 C45 H45 121.1 . .
C5 C4 C3 117.9(7) . .
C5 C4 H4 121.0 . .
C3 C4 H4 121.0 . .
N1 C5 C4 121.4(6) . .
N1 C5 C6 113.3(6) . .
C4 C5 C6 125.3(6) . .
N2 C6 C7 108.7(5) . .
N2 C6 C5 115.9(5) . .
C7 C6 C5 135.3(6) . .
C8 C7 C6 104.9(5) . .
C8 C7 H7 127.6 . .
C6 C7 H7 127.6 . .
N3 C8 C7 109.2(5) . .
N3 C8 C9 114.1(5) . .
C7 C8 C9 136.6(5) . .
N4 C9 C10 109.1(5) . .
N4 C9 C8 114.5(5) . .
C10 C9 C8 136.4(6) . .
C11 C10 C9 104.2(5) . .
C11 C10 H10 127.9 . .
C9 C10 H10 127.9 . .
N5 C11 C10 110.3(5) . .
N5 C11 C12 114.7(5) . .
C10 C11 C12 135.0(5) . .
N6 C12 C13 120.8(5) . .
N6 C12 C11 113.8(5) . .
C13 C12 C11 125.4(6) . .
C12 C13 C14 119.0(7) . .
C12 C13 H13 120.5 . .
C14 C13 H13 120.5 . .
C15 C14 C13 119.1(7) . .
C15 C14 H14 120.5 . .
C13 C14 H14 120.5 . .
C14 C15 C16 119.8(6) . .
C14 C15 H15 120.1 . .
C16 C15 H15 120.1 . .
N6 C16 C15 121.7(7) . .
N6 C16 H16 119.1 . .
C15 C16 H16 119.1 . .
N7 C17 C18 122.2(9) . .
N7 C17 H17 118.9 . .
C18 C17 H17 118.9 . .
C18 C19 C20 120.3(8) . .
C18 C19 H19 119.9 . .
C20 C19 H19 119.9 . .
C21 C20 C19 116.9(9) . .
C21 C20 H20 121.6 . .
C19 C20 H20 121.6 . .
N7 C21 C20 122.6(6) . .
N7 C21 C22 113.8(6) . .
C20 C21 C22 123.6(7) . .
N8 C22 C23 110.1(5) . .
N8 C22 C21 115.2(6) . .
C23 C22 C21 134.7(6) . .
C22 C23 C24 104.3(6) . .
C22 C23 H23 127.8 . .
C24 C23 H23 127.8 . .
N9 C24 C23 109.3(5) . .
N9 C24 C25 114.1(5) . .
C23 C24 C25 136.6(6) . .
N10 C25 C26 110.0(5) . .
N10 C25 C24 112.9(6) . .
C26 C25 C24 137.1(6) . .
C25 C26 C27 103.8(6) . .
C25 C26 H26 128.1 . .
C27 C26 H26 128.1 . .
N11 C27 C26 110.5(5) . .
N11 C27 C28 116.7(5) . .
C26 C27 C28 132.7(6) . .
N12 C28 C29 121.6(6) . .
N12 C28 C27 114.5(6) . .
C29 C28 C27 123.9(6) . .
C28 C29 C30 118.5(8) . .
C28 C29 H29 120.8 . .
C30 C29 H29 120.8 . .
C31 C30 C29 120.4(9) . .
C31 C30 H30 119.8 . .
C29 C30 H30 119.8 . .
C30 C31 C32 118.1(8) . .
C30 C31 H31 121.0 . .
C32 C31 H31 121.0 . .
N12 C32 C31 124.5(8) . .
N12 C32 H32 117.8 . .
C31 C32 H32 117.8 . .
N13 C33 C34 122.0(8) . .
N13 C33 H33 119.0 . .
C34 C33 H33 119.0 . .
C35 C34 C33 119.9(7) . .
C35 C34 H34 120.0 . .
C33 C34 H34 120.0 . .
C34 C35 C36 119.5(7) . .
C34 C35 H35 120.2 . .
C36 C35 H35 120.2 . .
C37 C36 C35 118.5(7) . .
C37 C36 H36 120.7 . .
C35 C36 H36 120.7 . .
N13 C37 C36 121.9(5) . .
N13 C37 C38 114.0(5) . .
C36 C37 C38 124.1(6) . .
N14 C38 C39 110.8(5) . .
N14 C38 C37 116.9(6) . .
C39 C38 C37 132.0(6) . .
C40 C39 C38 104.4(5) . .
C40 C39 H39 127.8 . .
C38 C39 H39 127.8 . .
N15 C40 C39 109.4(5) . .
N15 C40 C41 114.2(5) . .
C39 C40 C41 136.4(6) . .
N16 C41 C42 110.7(5) . .
N16 C41 C40 112.8(5) . .
C42 C41 C40 136.6(5) . .
C41 C42 C43 103.6(5) . .
C41 C42 H42 128.2 . .
C43 C42 H42 128.2 . .
N17 C43 C42 110.0(5) . .
N17 C43 C44 115.9(5) . .
C42 C43 C44 134.0(6) . .
N18 C44 C45 122.8(6) . .
N18 C44 C43 112.9(6) . .
C45 C44 C43 124.2(6) . .
C17 C18 C19 119.0(7) . .
C17 C18 H18 120.5 . .
C19 C18 H18 120.5 . .
C47 C46 C45 120.8(9) . .
C47 C46 H46 119.6 . .
C45 C46 H46 119.6 . .
C48 C47 C46 117.8(7) . .
C48 C47 H47 121.1 . .
C46 C47 H47 121.1 . .
N18 C48 C47 123.7(7) . .
N18 C48 H48 118.1 . .
C47 C48 H48 118.1 . .
O3 S1 O1 113.1(14) . .
O3 S1 O3 105.1(10) . 5_666
O1 S1 O3 122.2(13) . 5_666
O3 S1 O2 106.9(13) . .
O1 S1 O2 108.1(13) . .
O3 S1 O2 99.9(13) 5_666 .
O3 S1 S1 54.3(7) . 5_666
O1 S1 S1 139.8(12) . 5_666
O3 S1 S1 50.8(7) 5_666 5_666
O2 S1 S1 112.1(12) . 5_666
S1 O3 S1 74.9(10) . 5_666
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N2 1.924(4) .
Cu1 N15 1.937(4) .
Cu1 N16 1.969(5) .
Cu1 N1 2.025(5) .
Cu2 N4 1.952(4) 2_655
Cu2 N4 1.952(4) .
Cu2 N3 1.967(5) .
Cu2 N3 1.967(5) 2_655
Cu3 N5 1.911(5) .
Cu3 N10 1.931(5) .
Cu3 N9 1.968(5) .
Cu3 N6 2.020(5) .
Cu4 N8 1.917(5) .
Cu4 N8 1.917(5) 2_655
Cu4 N7 2.066(6) 2_655
Cu4 N7 2.066(6) .
Cu5 N14 2.006(5) 2_655
Cu5 N11 2.011(5) .
Cu5 N12 2.036(6) .
Cu5 N13 2.047(5) 2_655
Cu6 N17 1.919(5) .
Cu6 N17 1.919(5) 2_655
Cu6 N18 2.053(6) 2_655
Cu6 N18 2.053(6) .
N1 C1 1.322(8) .
N1 C5 1.353(8) .
N2 N3 1.327(6) .
N2 C6 1.338(8) .
N3 C8 1.350(7) .
N4 C9 1.330(8) .
N4 N5 1.350(6) .
N5 C11 1.339(7) .
N6 C16 1.335(7) .
N6 C12 1.341(8) .
N7 C17 1.338(8) .
N7 C21 1.345(9) .
N8 N9 1.340(6) .
N8 C22 1.342(8) .
N9 C24 1.340(8) .
N10 C25 1.356(8) .
N10 N11 1.352(6) .
N11 C27 1.318(8) .
N12 C32 1.334(9) .
N12 C28 1.356(8) .
N13 C33 1.346(8) .
N13 C37 1.353(8) .
N14 N15 1.354(6) .
N14 C38 1.349(7) .
N15 C40 1.348(8) .
N16 C41 1.347(7) .
N16 N17 1.348(7) .
N17 C43 1.342(8) .
N18 C44 1.338(8) .
N18 C48 1.345(9) .
C1 C2 1.378(12) .
C1 H1 0.9500 .
C2 C3 1.355(12) .
C2 H2 0.9500 .
C3 C4 1.389(10) .
C3 H3 0.9500 .
C45 C44 1.365(10) .
C45 C46 1.369(10) .
C45 H45 0.9500 .
C4 C5 1.382(10) .
C4 H4 0.9500 .
C5 C6 1.449(8) .
C6 C7 1.393(8) .
C7 C8 1.361(8) .
C7 H7 0.9500 .
C8 C9 1.450(8) .
C9 C10 1.401(7) .
C10 C11 1.364(8) .
C10 H10 0.9500 .
C11 C12 1.453(7) .
C12 C13 1.378(8) .
C13 C14 1.386(9) .
C13 H13 0.9500 .
C14 C15 1.353(11) .
C14 H14 0.9500 .
C15 C16 1.364(10) .
C15 H15 0.9500 .
C16 H16 0.9500 .
C17 C18 1.353(13) .
C17 H17 0.9500 .
C19 C18 1.382(14) .
C19 C20 1.390(11) .
C19 H19 0.9500 .
C20 C21 1.383(10) .
C20 H20 0.9500 .
C21 C22 1.468(8) .
C22 C23 1.373(9) .
C23 C24 1.381(8) .
C23 H23 0.9500 .
C24 C25 1.456(8) .
C25 C26 1.356(9) .
C26 C27 1.405(8) .
C26 H26 0.9500 .
C27 C28 1.452(8) .
C28 C29 1.373(10) .
C29 C30 1.383(11) .
C29 H29 0.9500 .
C30 C31 1.342(13) .
C30 H30 0.9500 .
C31 C32 1.354(13) .
C31 H31 0.9500 .
C32 H32 0.9500 .
C33 C34 1.378(11) .
C33 H33 0.9500 .
C34 C35 1.329(12) .
C34 H34 0.9500 .
C35 C36 1.406(9) .
C35 H35 0.9500 .
C36 C37 1.367(9) .
C36 H36 0.9500 .
C37 C38 1.461(7) .
C38 C39 1.379(8) .
C39 C40 1.376(7) .
C39 H39 0.9500 .
C40 C41 1.458(8) .
C41 C42 1.379(9) .
C42 C43 1.389(8) .
C42 H42 0.9500 .
C43 C44 1.469(8) .
C18 H18 0.9500 .
C46 C47 1.358(11) .
C46 H46 0.9500 .
C47 C48 1.352(12) .
C47 H47 0.9500 .
C48 H48 0.9500 .
S1 O3 1.416(13) .
S1 O1 1.447(15) .
S1 O3 1.484(15) 5_666
S1 O2 1.467(15) .
S1 S1 1.764(19) 5_666
O4 C49 1.432(10) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C45 H45 O3 0.95 2.60 3.520(17) 163.5 5_666 yes
C31 H31 O1 0.95 2.63 3.39(3) 137.2 7_666 yes
C42 H42 O3 0.95 2.48 3.383(15) 158.3 5_666 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C6 N2 N3 C8 1.1(6) . .
Cu1 N2 N3 C8 175.5(4) . .
C6 N2 N3 Cu2 169.2(4) . .
Cu1 N2 N3 Cu2 -16.4(9) . .
C9 N4 N5 C11 1.6(6) . .
Cu2 N4 N5 C11 170.5(4) . .
C9 N4 N5 Cu3 175.9(4) . .
Cu2 N4 N5 Cu3 -15.2(9) . .
C22 N8 N9 C24 -0.3(7) . .
Cu4 N8 N9 C24 175.4(5) . .
C22 N8 N9 Cu3 169.4(5) . .
Cu4 N8 N9 Cu3 -14.9(9) . .
C25 N10 N11 C27 0.0(6) . .
Cu3 N10 N11 C27 -175.9(5) . .
C25 N10 N11 Cu5 157.6(5) . .
Cu3 N10 N11 Cu5 -18.3(9) . .
C38 N14 N15 C40 0.6(6) . .
Cu5 N14 N15 C40 154.6(5) 2_655 .
C38 N14 N15 Cu1 -169.1(4) . .
Cu5 N14 N15 Cu1 -15.0(9) 2_655 .
C41 N16 N17 C43 -0.5(7) . .
Cu1 N16 N17 C43 167.1(5) . .
C41 N16 N17 Cu6 177.2(5) . .
Cu1 N16 N17 Cu6 -15.2(10) . .
C5 N1 C1 C2 0.1(11) . .
Cu1 N1 C1 C2 -176.2(6) . .
N1 C1 C2 C3 -0.9(14) . .
C1 C2 C3 C4 2.6(15) . .
C2 C3 C4 C5 -3.3(13) . .
C1 N1 C5 C4 -0.9(10) . .
Cu1 N1 C5 C4 175.8(5) . .
C1 N1 C5 C6 -179.0(6) . .
Cu1 N1 C5 C6 -2.3(6) . .
C3 C4 C5 N1 2.5(11) . .
C3 C4 C5 C6 -179.7(7) . .
N3 N2 C6 C7 -0.9(7) . .
Cu1 N2 C6 C7 -176.5(4) . .
N3 N2 C6 C5 178.7(5) . .
Cu1 N2 C6 C5 3.1(7) . .
N1 C5 C6 N2 -0.4(8) . .
C4 C5 C6 N2 -178.4(6) . .
N1 C5 C6 C7 179.0(6) . .
C4 C5 C6 C7 1.1(11) . .
N2 C6 C7 C8 0.3(7) . .
C5 C6 C7 C8 -179.2(6) . .
N2 N3 C8 C7 -0.9(7) . .
Cu2 N3 C8 C7 -172.0(4) . .
N2 N3 C8 C9 177.7(5) . .
Cu2 N3 C8 C9 6.6(6) . .
C6 C7 C8 N3 0.3(7) . .
C6 C7 C8 C9 -177.8(6) . .
N5 N4 C9 C10 -1.9(6) . .
Cu2 N4 C9 C10 -173.4(4) . .
N5 N4 C9 C8 177.8(5) . .
Cu2 N4 C9 C8 6.3(6) . .
N3 C8 C9 N4 -8.5(7) . .
C7 C8 C9 N4 169.6(7) . .
N3 C8 C9 C10 171.1(6) . .
C7 C8 C9 C10 -10.8(12) . .
N4 C9 C10 C11 1.5(7) . .
C8 C9 C10 C11 -178.1(6) . .
N4 N5 C11 C10 -0.6(7) . .
Cu3 N5 C11 C10 -176.1(4) . .
N4 N5 C11 C12 179.3(5) . .
Cu3 N5 C11 C12 3.7(6) . .
C9 C10 C11 N5 -0.5(7) . .
C9 C10 C11 C12 179.6(6) . .
C16 N6 C12 C13 -0.7(9) . .
Cu3 N6 C12 C13 177.5(5) . .
C16 N6 C12 C11 178.8(5) . .
Cu3 N6 C12 C11 -3.1(6) . .
N5 C11 C12 N6 -0.3(7) . .
C10 C11 C12 N6 179.6(6) . .
N5 C11 C12 C13 179.2(6) . .
C10 C11 C12 C13 -1.0(11) . .
N6 C12 C13 C14 1.0(10) . .
C11 C12 C13 C14 -178.4(7) . .
C12 C13 C14 C15 -1.4(12) . .
C13 C14 C15 C16 1.5(12) . .
C12 N6 C16 C15 0.7(9) . .
Cu3 N6 C16 C15 -177.1(5) . .
C14 C15 C16 N6 -1.1(11) . .
C21 N7 C17 C18 -1.4(11) . .
Cu4 N7 C17 C18 170.7(6) . .
C18 C19 C20 C21 -0.1(12) . .
C17 N7 C21 C20 2.2(10) . .
Cu4 N7 C21 C20 -171.1(5) . .
C17 N7 C21 C22 -178.9(6) . .
Cu4 N7 C21 C22 7.8(7) . .
C19 C20 C21 N7 -1.5(11) . .
C19 C20 C21 C22 179.8(7) . .
N9 N8 C22 C23 -0.2(7) . .
Cu4 N8 C22 C23 -176.8(4) . .
N9 N8 C22 C21 179.1(5) . .
Cu4 N8 C22 C21 2.6(7) . .
N7 C21 C22 N8 -7.0(8) . .
C20 C21 C22 N8 171.8(6) . .
N7 C21 C22 C23 172.1(7) . .
C20 C21 C22 C23 -9.1(11) . .
N8 C22 C23 C24 0.6(7) . .
C21 C22 C23 C24 -178.6(7) . .
N8 N9 C24 C23 0.7(7) . .
Cu3 N9 C24 C23 -171.3(4) . .
N8 N9 C24 C25 178.4(5) . .
Cu3 N9 C24 C25 6.4(6) . .
C22 C23 C24 N9 -0.8(7) . .
C22 C23 C24 C25 -177.7(7) . .
N11 N10 C25 C26 0.7(7) . .
Cu3 N10 C25 C26 177.5(4) . .
N11 N10 C25 C24 179.6(5) . .
Cu3 N10 C25 C24 -3.7(6) . .
N9 C24 C25 N10 -1.8(7) . .
C23 C24 C25 N10 175.0(7) . .
N9 C24 C25 C26 176.5(7) . .
C23 C24 C25 C26 -6.6(13) . .
N10 C25 C26 C27 -1.1(7) . .
C24 C25 C26 C27 -179.5(7) . .
N10 N11 C27 C26 -0.8(7) . .
Cu5 N11 C27 C26 -163.8(4) . .
N10 N11 C27 C28 177.3(5) . .
Cu5 N11 C27 C28 14.2(7) . .
C25 C26 C27 N11 1.2(7) . .
C25 C26 C27 C28 -176.5(7) . .
C32 N12 C28 C29 -2.1(11) . .
Cu5 N12 C28 C29 -171.3(7) . .
C32 N12 C28 C27 176.3(7) . .
Cu5 N12 C28 C27 7.0(7) . .
N11 C27 C28 N12 -14.4(9) . .
C26 C27 C28 N12 163.2(7) . .
N11 C27 C28 C29 163.9(8) . .
C26 C27 C28 C29 -18.5(12) . .
N12 C28 C29 C30 0.1(14) . .
C27 C28 C29 C30 -178.1(9) . .
C28 C29 C30 C31 1.0(19) . .
C29 C30 C31 C32 0(2) . .
C28 N12 C32 C31 3.2(14) . .
Cu5 N12 C32 C31 170.4(9) . .
C30 C31 C32 N12 -2.2(19) . .
C37 N13 C33 C34 2.8(11) . .
Cu5 N13 C33 C34 179.7(6) 2_655 .
N13 C33 C34 C35 -2.0(13) . .
C33 C34 C35 C36 0.8(13) . .
C34 C35 C36 C37 -0.3(12) . .
C33 N13 C37 C36 -2.3(9) . .
Cu5 N13 C37 C36 -179.7(5) 2_655 .
C33 N13 C37 C38 178.6(6) . .
Cu5 N13 C37 C38 1.3(6) 2_655 .
C35 C36 C37 N13 1.1(10) . .
C35 C36 C37 C38 -179.9(6) . .
N15 N14 C38 C39 -0.8(6) . .
Cu5 N14 C38 C39 -161.5(4) 2_655 .
N15 N14 C38 C37 173.1(5) . .
Cu5 N14 C38 C37 12.5(6) 2_655 .
N13 C37 C38 N14 -9.2(8) . .
C36 C37 C38 N14 171.8(6) . .
N13 C37 C38 C39 163.2(6) . .
C36 C37 C38 C39 -15.8(10) . .
N14 C38 C39 C40 0.7(7) . .
C37 C38 C39 C40 -172.0(6) . .
N14 N15 C40 C39 -0.1(6) . .
Cu1 N15 C40 C39 171.8(4) . .
N14 N15 C40 C41 179.7(5) . .
Cu1 N15 C40 C41 -8.4(6) . .
C38 C39 C40 N15 -0.4(6) . .
C38 C39 C40 C41 179.9(6) . .
N17 N16 C41 C42 0.0(7) . .
Cu1 N16 C41 C42 -170.6(4) . .
N17 N16 C41 C40 178.3(5) . .
Cu1 N16 C41 C40 7.8(6) . .
N15 C40 C41 N16 0.3(7) . .
C39 C40 C41 N16 -179.9(6) . .
N15 C40 C41 C42 178.1(6) . .
C39 C40 C41 C42 -2.2(12) . .
N16 C41 C42 C43 0.5(7) . .
C40 C41 C42 C43 -177.2(6) . .
N16 N17 C43 C42 0.9(7) . .
Cu6 N17 C43 C42 -177.3(4) . .
N16 N17 C43 C44 179.0(5) . .
Cu6 N17 C43 C44 0.8(7) . .
C41 C42 C43 N17 -0.9(7) . .
C41 C42 C43 C44 -178.4(6) . .
C48 N18 C44 C45 -0.3(9) . .
Cu6 N18 C44 C45 -172.5(5) . .
C48 N18 C44 C43 179.5(6) . .
Cu6 N18 C44 C43 7.3(6) . .
C46 C45 C44 N18 0.1(10) . .
C46 C45 C44 C43 -179.7(6) . .
N17 C43 C44 N18 -5.5(8) . .
C42 C43 C44 N18 172.0(6) . .
N17 C43 C44 C45 174.3(6) . .
C42 C43 C44 C45 -8.2(11) . .
N7 C17 C18 C19 -0.1(12) . .
C20 C19 C18 C17 0.9(13) . .
C44 C45 C46 C47 0.7(12) . .
C45 C46 C47 C48 -1.2(12) . .
C44 N18 C48 C47 -0.2(11) . .
Cu6 N18 C48 C47 170.6(6) . .
C46 C47 C48 N18 0.9(12) . .
O1 S1 O3 S1 -135.6(13) . 5_666
O3 S1 O3 S1 -0.001(1) 5_666 5_666
O2 S1 O3 S1 105.5(13) . 5_666
