#------------------------------------------------------------------------------
#$Date: 2021-03-05 03:56:25 +0200 (Fri, 05 Mar 2021) $
#$Revision: 262610 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/63/7706343.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_7706343
loop_
_publ_author_name
'Hu, Chen'
'Zhao, Yingnan'
'Han, Xiao'
'Song, Jiaqi'
'Ding, Jie'
'Hou, Hongwei'
_publ_section_title
;
 Facilely controllable synthesis of copper-benzothiadiazole complexes
 via solvothermal reactions: exploring the customized synthetic
 approach by experiments.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1816
_journal_page_last               1823
_journal_paper_doi               10.1039/d0dt03817b
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         '0.5(C64 H40 Br6 Cu6 N24 S4)'
_chemical_formula_sum            'C32 H20 Br3 Cu3 N12 S2'
_chemical_formula_weight         1067.07
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc2667nb
_audit_creation_date             2020-12-19
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-31 deposited with the CCDC.	2021-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.907(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.745(5)
_cell_length_b                   11.282(4)
_cell_length_c                   21.686(7)
_cell_measurement_reflns_used    9425
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.33
_cell_volume                     3433(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298.01
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            18021
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.495
_diffrn_reflns_theta_min         2.336
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.502
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0605 before and 0.0440 after correction.
The Ratio of minimum to maximum transmission is 0.7948.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            \^A
_exptl_crystal_colour_primary    \^A
_exptl_crystal_density_diffrn    2.065
_exptl_crystal_description       plate
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         3911
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0232
_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)+(0.0234P)²+4.0353P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0518
_refine_ls_wR_factor_ref         0.0544
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3342
_reflns_number_total             3911
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt03817b2.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 7706342--7706346.cif.'
_cod_original_cell_volume        3432.8(19)
_cod_database_code               7706343
_shelx_shelxl_version_number     2016/6
_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   0.438
_shelx_estimated_absorpt_t_min   0.391
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C11(H11), C13(H13), C14(H14), C15(H15),
 C16(H16)
;
_olex2_submission_special_instructions 'No special instructions were received'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.56775(2) 0.24618(2) 0.34350(2) 0.03364(7) Uani 1 1 d . . . . .
Br2 Br 0.500000 0.58199(3) 0.250000 0.03689(9) Uani 1 2 d S T P . .
Cu1 Cu 0.62335(2) 0.45304(3) 0.36790(2) 0.03559(8) Uani 1 1 d . . . . .
Cu2 Cu 0.500000 0.37209(4) 0.250000 0.03921(11) Uani 1 2 d S T P . .
S1 S 0.90702(5) 0.54196(6) 0.55919(3) 0.04232(15) Uani 1 1 d . . . . .
N1 N 0.80496(14) 0.51264(17) 0.50584(10) 0.0352(4) Uani 1 1 d . . . . .
N2 N 0.87658(14) 0.64435(17) 0.60175(10) 0.0367(5) Uani 1 1 d . . . . .
N3 N 0.58213(13) 0.53817(16) 0.43347(8) 0.0285(4) Uani 1 1 d . . . . .
N4 N 0.49675(12) 0.66205(15) 0.47618(8) 0.0264(4) Uani 1 1 d . . . . .
N5 N 0.77661(15) 0.81821(17) 0.64888(10) 0.0335(4) Uani 1 1 d . . . . .
H5 H 0.8315(19) 0.823(2) 0.6525(12) 0.034(7) Uiso 1 1 d . . . . .
N6 N 0.77058(13) 1.02104(15) 0.67059(8) 0.0277(4) Uani 1 1 d . . . . .
C1 C 0.41609(16) 0.7187(2) 0.48061(11) 0.0324(5) Uani 1 1 d . . . . .
H1 H 0.419718 0.772538 0.513749 0.039 Uiso 1 1 calc R . . . .
C2 C 0.33128(17) 0.6942(2) 0.43556(11) 0.0383(5) Uani 1 1 d . . . . .
H2 H 0.276314 0.732513 0.437364 0.046 Uiso 1 1 calc R . . . .
C3 C 0.32598(17) 0.6107(2) 0.38588(11) 0.0377(5) Uani 1 1 d . . . . .
H3 H 0.267193 0.593862 0.355813 0.045 Uiso 1 1 calc R . . . .
C4 C 0.40543(17) 0.5544(2) 0.38130(11) 0.0332(5) Uani 1 1 d . . . . .
H4 H 0.401139 0.499691 0.348440 0.040 Uiso 1 1 calc R . . . .
C5 C 0.49434(16) 0.58038(19) 0.42716(10) 0.0275(4) Uani 1 1 d . . . . .
C6 C 0.59051(15) 0.67164(18) 0.51507(10) 0.0258(4) Uani 1 1 d . . . . .
C7 C 0.64133(15) 0.59347(18) 0.48810(10) 0.0265(4) Uani 1 1 d . . . . .
C8 C 0.74100(16) 0.58423(18) 0.51976(11) 0.0275(4) Uani 1 1 d . . . . .
C9 C 0.78235(15) 0.65935(18) 0.57530(11) 0.0282(4) Uani 1 1 d . . . . .
C10 C 0.72652(16) 0.74432(18) 0.59879(10) 0.0276(4) Uani 1 1 d . . . . .
C11 C 0.62997(16) 0.74671(18) 0.56894(10) 0.0281(4) Uani 1 1 d . . . . .
H11 H 0.591119 0.796760 0.583820 0.034 Uiso 1 1 calc R . . . .
C12 C 0.73496(15) 0.91200(19) 0.67311(10) 0.0287(5) Uani 1 1 d . . . . .
C13 C 0.66220(18) 0.8913(2) 0.70016(12) 0.0411(6) Uani 1 1 d . . . . .
H13 H 0.639380 0.814878 0.701834 0.049 Uiso 1 1 calc R . . . .
C14 C 0.6247(2) 0.9850(3) 0.72428(14) 0.0524(7) Uani 1 1 d . . . . .
H14 H 0.575404 0.972875 0.741963 0.063 Uiso 1 1 calc R . . . .
C15 C 0.6604(2) 1.0977(3) 0.72222(14) 0.0520(7) Uani 1 1 d . . . . .
H15 H 0.635587 1.162489 0.738116 0.062 Uiso 1 1 calc R . . . .
C16 C 0.73378(18) 1.1114(2) 0.69600(12) 0.0390(6) Uani 1 1 d . . . . .
H16 H 0.759262 1.186786 0.695775 0.047 Uiso 1 1 calc R . . . .
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'
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
_geom_angle_publ_flag
Cu2 Br1 Cu1 69.56(2) . . ?
Br1 Cu1 Cu2 54.360(12) . . ?
N3 Cu1 Br1 117.42(5) . . ?
N3 Cu1 Cu2 124.30(6) . . ?
N3 Cu1 N6 133.22(7) . 7_666 ?
N6 Cu1 Br1 107.30(5) 7_666 . ?
N6 Cu1 Cu2 92.19(6) 7_666 . ?
Br1 Cu2 Br1 108.29(3) 2_655 . ?
Br1 Cu2 Cu1 56.08(2) 2_655 2_655 ?
Br1 Cu2 Cu1 160.160(17) 2_655 . ?
Br1 Cu2 Cu1 56.08(2) . . ?
Br1 Cu2 Cu1 160.161(17) . 2_655 ?
Br2 Cu2 Br1 125.858(15) . 2_655 ?
Br2 Cu2 Br1 125.857(15) . . ?
Br2 Cu2 Cu1 70.937(13) . 2_655 ?
Br2 Cu2 Cu1 70.937(13) . . ?
Cu1 Cu2 Cu1 141.87(3) 2_655 . ?
N1 S1 N2 101.06(10) . . ?
C8 N1 S1 106.12(16) . . ?
C9 N2 S1 106.11(16) . . ?
C5 N3 Cu1 127.03(15) . . ?
C5 N3 C7 105.13(17) . . ?
C7 N3 Cu1 125.91(14) . . ?
C1 N4 C5 122.49(18) . . ?
C1 N4 C6 129.96(19) . . ?
C6 N4 C5 107.55(17) . . ?
C10 N5 H5 113.7(18) . . ?
C10 N5 C12 123.8(2) . . ?
C12 N5 H5 117.5(18) . . ?
C12 N6 Cu1 120.92(14) . 7_666 ?
C12 N6 C16 117.61(19) . . ?
C16 N6 Cu1 121.46(15) . 7_666 ?
N4 C1 H1 120.7 . . ?
C2 C1 N4 118.6(2) . . ?
C2 C1 H1 120.7 . . ?
C1 C2 H2 119.8 . . ?
C1 C2 C3 120.4(2) . . ?
C3 C2 H2 119.8 . . ?
C2 C3 H3 119.4 . . ?
C4 C3 C2 121.2(2) . . ?
C4 C3 H3 119.4 . . ?
C3 C4 H4 120.5 . . ?
C3 C4 C5 119.0(2) . . ?
C5 C4 H4 120.5 . . ?
N3 C5 N4 110.90(18) . . ?
N3 C5 C4 130.8(2) . . ?
N4 C5 C4 118.26(19) . . ?
N4 C6 C7 105.02(18) . . ?
N4 C6 C11 129.02(19) . . ?
C7 C6 C11 125.9(2) . . ?
N3 C7 C6 111.38(19) . . ?
N3 C7 C8 131.75(19) . . ?
C6 C7 C8 116.87(19) . . ?
N1 C8 C7 128.9(2) . . ?
N1 C8 C9 113.2(2) . . ?
C7 C8 C9 117.90(19) . . ?
N2 C9 C8 113.49(19) . . ?
N2 C9 C10 123.9(2) . . ?
C8 C9 C10 122.6(2) . . ?
N5 C10 C9 116.6(2) . . ?
C11 C10 N5 125.7(2) . . ?
C11 C10 C9 117.72(19) . . ?
C6 C11 H11 120.6 . . ?
C10 C11 C6 118.79(19) . . ?
C10 C11 H11 120.6 . . ?
N6 C12 N5 116.92(19) . . ?
N6 C12 C13 122.1(2) . . ?
C13 C12 N5 120.9(2) . . ?
C12 C13 H13 120.5 . . ?
C14 C13 C12 119.0(2) . . ?
C14 C13 H13 120.5 . . ?
C13 C14 H14 120.2 . . ?
C13 C14 C15 119.7(2) . . ?
C15 C14 H14 120.2 . . ?
C14 C15 H15 120.9 . . ?
C16 C15 C14 118.2(2) . . ?
C16 C15 H15 120.9 . . ?
N6 C16 C15 123.3(2) . . ?
N6 C16 H16 118.4 . . ?
C15 C16 H16 118.4 . . ?
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
Br1 Cu1 2.4764(8) . ?
Br1 Cu2 2.4253(6) . ?
Br2 Cu2 2.3682(9) . ?
Cu1 Cu2 2.7964(8) . ?
Cu1 N3 1.9609(18) . ?
Cu1 N6 2.0078(18) 7_666 ?
S1 N1 1.625(2) . ?
S1 N2 1.626(2) . ?
N1 C8 1.345(3) . ?
N2 C9 1.341(3) . ?
N3 C5 1.346(3) . ?
N3 C7 1.385(3) . ?
N4 C1 1.379(3) . ?
N4 C5 1.399(3) . ?
N4 C6 1.385(3) . ?
N5 H5 0.79(3) . ?
N5 C10 1.388(3) . ?
N5 C12 1.404(3) . ?
N6 C12 1.345(3) . ?
N6 C16 1.350(3) . ?
C1 H1 0.9300 . ?
C1 C2 1.358(3) . ?
C2 H2 0.9300 . ?
C2 C3 1.415(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.363(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.411(3) . ?
C6 C7 1.397(3) . ?
C6 C11 1.415(3) . ?
C7 C8 1.422(3) . ?
C8 C9 1.445(3) . ?
C9 C10 1.454(3) . ?
C10 C11 1.371(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.392(3) . ?
C13 H13 0.9300 . ?
C13 C14 1.370(4) . ?
C14 H14 0.9300 . ?
C14 C15 1.382(4) . ?
C15 H15 0.9300 . ?
C15 C16 1.377(3) . ?
C16 H16 0.9300 . ?
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
N5 H5 Br2 0.79(3) 2.93(3) 3.533(2) 136(2) 7_666
C1 H1 Br1 0.93 3.05 3.769(3) 135.2 5_666
C2 H2 Br1 0.93 3.13 3.829(3) 133.7 3_455
C4 H4 Br2 0.93 3.08 3.548(2) 113.3 .
C13 H13 Br1 0.93 2.99 3.581(3) 123.1 5_666
C16 H16 Br1 0.93 3.02 3.663(3) 127.4 7_666
