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#$Date: 2023-07-18 00:54:53 +0300 (Tue, 18 Jul 2023) $
#$Revision: 285249 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/18/7131896.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_7131896
loop_
_publ_author_name
'Wei, Shuxia'
'Ma, Chengfeng'
'Liu, Xinge'
'Liu, Naiyun'
'Yuan, MingJun'
'Xiao, Kang'
'Yan, Weibo'
'Xin, Hao'
_publ_section_title
;
 A facial synthesis of a copper (I) thiourea sulphate complex and its
 application for highly efficient chalcopyrite solar cells
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC02417B
_journal_year                    2023
_chemical_formula_moiety         '2Cu, 6[CH4N2S], SO4, H2O'
_chemical_formula_sum            'C6 H26 Cu2 N12 O5 S7'
_chemical_formula_weight         697.89
_chemical_name_systematic
'bis(μ-thiourea)-tetrakis(thiourea)-di-copper-(Cu-Cu) sulfate hydrate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc2bg7pr
_audit_creation_method           SHELXL-2019/2
_audit_update_record
;
2023-05-18 deposited with the CCDC.	2023-07-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.2009(11)
_cell_length_b                   12.3001(7)
_cell_length_c                   21.4316(13)
_cell_measurement_reflns_used    9871
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      30.82
_cell_measurement_theta_min      2.69
_cell_volume                     5061.6(5)
_computing_cell_refinement       'APEX III'
_computing_data_collection       'APEX III; Bruker AXS'
_computing_data_reduction        'SAINT; Bruker AXS'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker AXS area detector; Photon 100'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            53895
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.687
_diffrn_reflns_theta_min         2.691
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.302
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.5672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016; Bruker; Krause, L.,et al., J. Appl. Cryst. 48 (2015) 3-10'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       0.00064(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         8539
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0276P)²+3.1237P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0753
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5826
_reflns_number_total             8539
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3cc02417b13.cif
_cod_data_source_block           CuTua_a
_cod_database_code               7131896
_shelx_shelxl_version_number     2019/2
_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   0.545
_shelx_estimated_absorpt_t_max   0.724
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, 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
Cu1 Cu 0.62430(2) 0.26540(2) 0.32197(2) 0.02985(7) Uani 1 1 d . . . . .
O1 O 0.71603(9) -0.02399(13) 0.55095(8) 0.0359(4) Uani 1 1 d . . . . .
C1 C 0.71626(10) 0.37180(17) 0.20383(10) 0.0228(4) Uani 1 1 d . . . . .
S1 S 0.64124(3) 0.35339(4) 0.42013(2) 0.02498(11) Uani 1 1 d . . . . .
H1O H 0.5732(18) 0.0177(18) 0.5921(16) 0.081(12) Uiso 1 1 d D . . . .
N1 N 0.73461(10) 0.35646(15) 0.14553(8) 0.0323(4) Uani 1 1 d . . . . .
H1A H 0.732690 0.409420 0.119394 0.039 Uiso 1 1 calc R U . . .
H1B H 0.748552 0.293436 0.133455 0.039 Uiso 1 1 calc R U . . .
Cu2 Cu 0.55865(2) 0.45544(2) 0.36678(2) 0.02985(8) Uani 1 1 d . . . . .
O2 O 0.70965(9) -0.21612(13) 0.53218(7) 0.0373(4) Uani 1 1 d . . . . .
C2 C 0.64405(11) 0.67378(17) 0.40010(10) 0.0261(4) Uani 1 1 d . . . . .
S2 S 0.53585(3) 0.36021(4) 0.26672(2) 0.02256(11) Uani 1 1 d . . . . .
H2O H 0.554(2) 0.097(4) 0.6487(9) 0.112(16) Uiso 1 1 d D . . . .
N2 N 0.69502(11) 0.46891(16) 0.22152(9) 0.0372(5) Uani 1 1 d . . . . .
H2A H 0.693321 0.521255 0.194963 0.045 Uiso 1 1 calc R U . . .
H2B H 0.682859 0.479932 0.259619 0.045 Uiso 1 1 calc R U . . .
S3 S 0.72046(3) 0.26393(5) 0.25484(3) 0.02887(12) Uani 1 1 d . . . . .
N3 N 0.69176(10) 0.75088(16) 0.39717(10) 0.0372(5) Uani 1 1 d . . . . .
H3A H 0.704984 0.783459 0.430644 0.045 Uiso 1 1 calc R U . . .
H3B H 0.709623 0.768532 0.361796 0.045 Uiso 1 1 calc R U . . .
O3 O 0.60514(8) -0.11512(15) 0.55414(8) 0.0418(4) Uani 1 1 d . . . . .
C3 C 0.41026(12) 0.56970(18) 0.36570(11) 0.0286(5) Uani 1 1 d . . . . .
N4 N 0.61833(13) 0.64961(19) 0.45489(10) 0.0512(6) Uani 1 1 d . . . . .
H4A H 0.632575 0.683599 0.487548 0.061 Uiso 1 1 calc R U . . .
H4B H 0.587168 0.599725 0.458246 0.061 Uiso 1 1 calc R U . . .
O4 O 0.68915(8) -0.14731(12) 0.63494(7) 0.0280(3) Uani 1 1 d . . . . .
C4 C 0.45491(11) 0.30484(17) 0.28298(10) 0.0247(4) Uani 1 1 d . . . . .
S4 S 0.60167(4) 0.07960(5) 0.32902(3) 0.03743(15) Uani 1 1 d . . . . .
N5 N 0.44203(12) 0.63000(19) 0.32414(11) 0.0473(6) Uani 1 1 d . . . . .
H5A H 0.418274 0.671908 0.300088 0.057 Uiso 1 1 calc R U . . .
H5B H 0.486650 0.627675 0.320908 0.057 Uiso 1 1 calc R U . . .
O5 O 0.55668(10) 0.08724(18) 0.60412(10) 0.0486(5) Uani 1 1 d D . . . .
C5 C 0.62819(13) 0.03139(17) 0.40060(11) 0.0308(5) Uani 1 1 d . . . . .
S5 S 0.61860(3) 0.60889(5) 0.33334(3) 0.02877(12) Uani 1 1 d . . . . .
N6 N 0.34186(11) 0.57661(19) 0.36853(12) 0.0486(6) Uani 1 1 d . . . . .
H6A H 0.319888 0.619473 0.343687 0.058 Uiso 1 1 calc R U . . .
H6B H 0.319188 0.538243 0.395232 0.058 Uiso 1 1 calc R U . . .
C6 C 0.60106(12) 0.27314(17) 0.47559(10) 0.0270(4) Uani 1 1 d . . . . .
S6 S 0.45452(3) 0.48640(5) 0.41573(3) 0.03394(14) Uani 1 1 d . . . . .
N7 N 0.39901(10) 0.35230(17) 0.26097(10) 0.0383(5) Uani 1 1 d . . . . .
H7A H 0.358535 0.325671 0.268838 0.046 Uiso 1 1 calc R U . . .
H7B H 0.402772 0.410098 0.238637 0.046 Uiso 1 1 calc R U . . .
S7 S 0.67985(3) -0.12571(4) 0.56781(2) 0.02225(11) Uani 1 1 d . . . . .
N8 N 0.44855(11) 0.21675(17) 0.31698(10) 0.0374(5) Uani 1 1 d . . . . .
H8A H 0.407912 0.190583 0.324658 0.045 Uiso 1 1 calc R U . . .
H8B H 0.485025 0.185145 0.331591 0.045 Uiso 1 1 calc R U . . .
N9 N 0.58466(12) -0.0257(2) 0.43405(11) 0.0501(6) Uani 1 1 d . . . . .
H9A H 0.597548 -0.051626 0.469480 0.060 Uiso 1 1 calc R U . . .
H9B H 0.543109 -0.037332 0.420648 0.060 Uiso 1 1 calc R U . . .
N10 N 0.69097(12) 0.04814(19) 0.42176(11) 0.0499(6) Uani 1 1 d . . . . .
H10A H 0.703187 0.021728 0.457267 0.060 Uiso 1 1 calc R U . . .
H10B H 0.720156 0.085586 0.400202 0.060 Uiso 1 1 calc R U . . .
N11 N 0.63784(12) 0.23859(17) 0.52296(9) 0.0427(5) Uani 1 1 d . . . . .
H11A H 0.618688 0.198976 0.551220 0.051 Uiso 1 1 calc R U . . .
H11B H 0.681186 0.255484 0.525847 0.051 Uiso 1 1 calc R U . . .
N12 N 0.53481(11) 0.24683(17) 0.47162(11) 0.0434(5) Uani 1 1 d . . . . .
H12A H 0.515995 0.207184 0.500057 0.052 Uiso 1 1 calc R U . . .
H12B H 0.510306 0.269265 0.440599 0.052 Uiso 1 1 calc R 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
_geom_angle_publ_flag
S4 Cu1 S3 100.33(2) . . ?
S4 Cu1 S2 112.35(2) . . ?
S3 Cu1 S2 105.15(2) . . ?
S4 Cu1 S1 114.36(2) . . ?
S3 Cu1 S1 115.94(2) . . ?
S2 Cu1 S1 108.29(2) . . ?
S4 Cu1 Cu2 134.92(2) . . ?
S3 Cu1 Cu2 124.576(18) . . ?
S2 Cu1 Cu2 56.236(15) . . ?
S1 Cu1 Cu2 52.126(15) . . ?
N1 C1 N2 119.17(19) . . ?
N1 C1 S3 118.78(16) . . ?
N2 C1 S3 122.05(16) . . ?
C6 S1 Cu2 110.03(8) . . ?
C6 S1 Cu1 106.64(8) . . ?
Cu2 S1 Cu1 73.643(18) . . ?
C1 N1 H1A 120.0 . . ?
C1 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
S6 Cu2 S1 117.41(2) . . ?
S6 Cu2 S5 116.02(2) . . ?
S1 Cu2 S5 104.62(2) . . ?
S6 Cu2 S2 108.68(2) . . ?
S1 Cu2 S2 106.89(2) . . ?
S5 Cu2 S2 101.78(2) . . ?
S6 Cu2 Cu1 133.10(2) . . ?
S1 Cu2 Cu1 54.232(16) . . ?
S5 Cu2 Cu1 110.260(19) . . ?
S2 Cu2 Cu1 52.728(14) . . ?
N4 C2 N3 117.9(2) . . ?
N4 C2 S5 122.49(17) . . ?
N3 C2 S5 119.61(17) . . ?
C4 S2 Cu1 110.36(8) . . ?
C4 S2 Cu2 99.78(7) . . ?
Cu1 S2 Cu2 71.036(17) . . ?
C1 N2 H2A 120.0 . . ?
C1 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
C1 S3 Cu1 110.33(7) . . ?
C2 N3 H3A 120.0 . . ?
C2 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
N5 C3 N6 117.3(2) . . ?
N5 C3 S6 122.30(18) . . ?
N6 C3 S6 120.4(2) . . ?
C2 N4 H4A 120.0 . . ?
C2 N4 H4B 120.0 . . ?
H4A N4 H4B 120.0 . . ?
N7 C4 N8 119.5(2) . . ?
N7 C4 S2 119.17(17) . . ?
N8 C4 S2 121.35(17) . . ?
C5 S4 Cu1 109.89(8) . . ?
C3 N5 H5A 120.0 . . ?
C3 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
H1O O5 H2O 113(3) . . ?
N10 C5 N9 119.1(2) . . ?
N10 C5 S4 121.92(19) . . ?
N9 C5 S4 119.01(19) . . ?
C2 S5 Cu2 105.23(8) . . ?
C3 N6 H6A 120.0 . . ?
C3 N6 H6B 120.0 . . ?
H6A N6 H6B 120.0 . . ?
N11 C6 N12 119.5(2) . . ?
N11 C6 S1 118.61(18) . . ?
N12 C6 S1 121.89(18) . . ?
C3 S6 Cu2 104.27(8) . . ?
C4 N7 H7A 120.0 . . ?
C4 N7 H7B 120.0 . . ?
H7A N7 H7B 120.0 . . ?
O2 S7 O3 110.15(11) . . ?
O2 S7 O4 108.93(10) . . ?
O3 S7 O4 109.20(9) . . ?
O2 S7 O1 109.38(10) . . ?
O3 S7 O1 109.60(10) . . ?
O4 S7 O1 109.56(9) . . ?
C4 N8 H8A 120.0 . . ?
C4 N8 H8B 120.0 . . ?
H8A N8 H8B 120.0 . . ?
C5 N9 H9A 120.0 . . ?
C5 N9 H9B 120.0 . . ?
H9A N9 H9B 120.0 . . ?
C5 N10 H10A 120.0 . . ?
C5 N10 H10B 120.0 . . ?
H10A N10 H10B 120.0 . . ?
C6 N11 H11A 120.0 . . ?
C6 N11 H11B 120.0 . . ?
H11A N11 H11B 120.0 . . ?
C6 N12 H12A 120.0 . . ?
C6 N12 H12B 120.0 . . ?
H12A N12 H12B 120.0 . . ?
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
Cu1 S4 2.3312(7) . ?
Cu1 S3 2.3407(6) . ?
Cu1 S2 2.3763(6) . ?
Cu1 S1 2.3881(6) . ?
Cu1 Cu2 2.8241(4) . ?
O1 S7 1.4760(16) . ?
C1 N1 1.312(3) . ?
C1 N2 1.318(3) . ?
C1 S3 1.721(2) . ?
S1 C6 1.727(2) . ?
S1 Cu2 2.3233(6) . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
Cu2 S6 2.2897(6) . ?
Cu2 S5 2.3240(6) . ?
Cu2 S2 2.4825(6) . ?
O2 S7 1.4654(17) . ?
C2 N4 1.308(3) . ?
C2 N3 1.320(3) . ?
C2 S5 1.710(2) . ?
S2 C4 1.732(2) . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?
N3 H3A 0.8600 . ?
N3 H3B 0.8600 . ?
O3 S7 1.4698(17) . ?
C3 N5 1.310(3) . ?
C3 N6 1.317(3) . ?
C3 S6 1.709(2) . ?
N4 H4A 0.8600 . ?
N4 H4B 0.8600 . ?
O4 S7 1.4739(15) . ?
C4 N7 1.310(3) . ?
C4 N8 1.311(3) . ?
S4 C5 1.722(2) . ?
N5 H5A 0.8600 . ?
N5 H5B 0.8600 . ?
O5 H1O 0.948(18) . ?
O5 H2O 0.964(18) . ?
C5 N10 1.304(3) . ?
C5 N9 1.306(3) . ?
N6 H6A 0.8600 . ?
N6 H6B 0.8600 . ?
C6 N11 1.308(3) . ?
C6 N12 1.315(3) . ?
N7 H7A 0.8600 . ?
N7 H7B 0.8600 . ?
N8 H8A 0.8600 . ?
N8 H8B 0.8600 . ?
N9 H9A 0.8600 . ?
N9 H9B 0.8600 . ?
N10 H10A 0.8600 . ?
N10 H10B 0.8600 . ?
N11 H11A 0.8600 . ?
N11 H11B 0.8600 . ?
N12 H12A 0.8600 . ?
N12 H12B 0.8600 . ?
