#------------------------------------------------------------------------------
#$Date: 2019-11-23 00:07:54 +0200 (Sat, 23 Nov 2019) $
#$Revision: 231622 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/61/4346129.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_4346129
loop_
_publ_author_name
'Knorr, Michael'
'Bonnot, Antoine'
'Lapprand, Antony'
'Khatyr, Abderrahim'
'Strohmann, Carsten'
'Kubicki, Marek M.'
'Rousselin, Yoann'
'Harvey, Pierre D.'
_publ_section_title
;
 Reactivity of CuI and CuBr toward dialkyl sulfides RSR: from discrete
 molecular Cu4I4S4 and Cu8I8S6 clusters to luminescent copper(I)
 coordination polymers.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4076
_journal_page_last               4093
_journal_paper_doi               10.1021/acs.inorgchem.5b00327
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C12 H30 Br3 Cu3 S3'
_chemical_formula_sum            'C12 H30 Br3 Cu3 S3'
_chemical_formula_weight         700.89
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.617(4)
_cell_angle_beta                 83.668(5)
_cell_angle_gamma                69.142(4)
_cell_formula_units_Z            2
_cell_length_a                   8.6040(10)
_cell_length_b                   11.9434(13)
_cell_length_c                   12.1004(15)
_cell_measurement_reflns_used    9786
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      2.34
_cell_volume                     1144.6(2)
_computing_cell_refinement       'SAINT (Bruker, 2012)'
_computing_data_collection       'APEX2 (Bruker, 2012)'
_computing_data_reduction        'SAINT (Bruker, 2012)'
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXD, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      115(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius Kappa Apex II'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            43734
_diffrn_reflns_theta_full        27.60
_diffrn_reflns_theta_max         27.60
_diffrn_reflns_theta_min         2.67
_exptl_absorpt_coefficient_mu    8.264
_exptl_absorpt_correction_T_max  0.4003
_exptl_absorpt_correction_T_min  0.2149
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1250 before and 0.0464 after correction.
The Ratio of minimum to maximum transmission is 0.5369.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    2.034
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         5284
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0182
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0124P)²+0.6332P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0354
_refine_ls_wR_factor_ref         0.0367
_reflns_number_gt                4786
_reflns_number_total             5284
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00327_si_003.cif
_cod_data_source_block           13mkcubrmespr_compound_10
_cod_database_code               4346129
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Br1 Br -0.13363(2) 1.433681(15) 0.119864(15) 0.01495(4) Uani 1 1 d .
Br2 Br 0.73118(2) 1.064210(16) 0.216526(16) 0.01784(5) Uani 1 1 d .
Br3 Br 0.35110(2) 0.974034(16) 0.123258(15) 0.01458(4) Uani 1 1 d .
Cu1 Cu 0.11280(3) 1.378080(19) -0.009937(19) 0.01384(5) Uani 1 1 d .
Cu2 Cu 0.42829(3) 1.13087(2) 0.21303(2) 0.01690(5) Uani 1 1 d .
Cu3 Cu 0.64807(3) 0.96016(2) 0.08531(2) 0.01799(6) Uani 1 1 d .
S1 S 0.34007(5) 1.31224(4) 0.10121(4) 0.01110(9) Uani 1 1 d .
S2 S 0.86234(5) 0.77585(4) 0.10515(4) 0.01236(9) Uani 1 1 d .
S3 S 0.29502(6) 1.12909(4) 0.38502(4) 0.01743(10) Uani 1 1 d .
C1 C 0.2958(2) 1.43693(15) 0.18108(15) 0.0138(4) Uani 1 1 d .
H1A H 0.2826 1.5116 0.1278 0.017 Uiso 1 1 calc R
H1B H 0.1879 1.4477 0.2242 0.017 Uiso 1 1 calc R
C2 C 0.4256(2) 1.42336(17) 0.26176(16) 0.0175(4) Uani 1 1 d .
H2A H 0.5354 1.4091 0.2204 0.021 Uiso 1 1 calc R
H2B H 0.4343 1.3524 0.3192 0.021 Uiso 1 1 calc R
C3 C 0.3805(3) 1.53629(19) 0.31928(18) 0.0251(5) Uani 1 1 d .
H3A H 0.3769 1.6059 0.2628 0.038 Uiso 1 1 calc R
H3B H 0.4646 1.5244 0.3727 0.038 Uiso 1 1 calc R
H3C H 0.2712 1.5511 0.3593 0.038 Uiso 1 1 calc R
C4 C 0.5142(2) 1.32657(17) 0.00992(16) 0.0168(4) Uani 1 1 d .
H4A H 0.6057 1.3196 0.0552 0.025 Uiso 1 1 calc R
H4B H 0.4802 1.4055 -0.0368 0.025 Uiso 1 1 calc R
H4C H 0.5514 1.2623 -0.0383 0.025 Uiso 1 1 calc R
C5 C 0.0745(2) 1.19052(19) 0.35856(17) 0.0227(4) Uani 1 1 d .
H5A H 0.0514 1.2694 0.3104 0.027 Uiso 1 1 calc R
H5B H 0.0487 1.1355 0.3164 0.027 Uiso 1 1 calc R
C6 C -0.0401(3) 1.2080(2) 0.46315(18) 0.0258(5) Uani 1 1 d .
H6A H -0.0071 1.2552 0.5104 0.031 Uiso 1 1 calc R
H6B H -0.0294 1.1283 0.5069 0.031 Uiso 1 1 calc R
C7 C -0.2198(3) 1.27383(19) 0.43354(19) 0.0267(5) Uani 1 1 d .
H7A H -0.2521 1.2276 0.3861 0.040 Uiso 1 1 calc R
H7B H -0.2313 1.3541 0.3930 0.040 Uiso 1 1 calc R
H7C H -0.2920 1.2823 0.5024 0.040 Uiso 1 1 calc R
C8 C 0.3223(3) 0.97386(18) 0.43716(18) 0.0267(5) Uani 1 1 d .
H8A H 0.2767 0.9402 0.3852 0.040 Uiso 1 1 calc R
H8B H 0.2638 0.9693 0.5111 0.040 Uiso 1 1 calc R
H8C H 0.4413 0.9275 0.4436 0.040 Uiso 1 1 calc R
C9 C 0.8759(2) 0.72173(17) 0.25406(15) 0.0171(4) Uani 1 1 d .
H9A H 0.9749 0.6476 0.2664 0.021 Uiso 1 1 calc R
H9B H 0.8886 0.7838 0.2939 0.021 Uiso 1 1 calc R
C10 C 0.7202(3) 0.69446(19) 0.30060(17) 0.0239(4) Uani 1 1 d .
H10A H 0.6239 0.7710 0.2989 0.029 Uiso 1 1 calc R
H10B H 0.6977 0.6429 0.2527 0.029 Uiso 1 1 calc R
C11 C 0.7389(3) 0.6308(2) 0.41990(19) 0.0354(6) Uani 1 1 d .
H11A H 0.8351 0.5556 0.4220 0.053 Uiso 1 1 calc R
H11B H 0.6380 0.6121 0.4467 0.053 Uiso 1 1 calc R
H11C H 0.7556 0.6834 0.4682 0.053 Uiso 1 1 calc R
C12 C 1.0476(2) 0.81578(18) 0.07583(18) 0.0217(4) Uani 1 1 d .
H12A H 1.1452 0.7452 0.0980 0.033 Uiso 1 1 calc R
H12B H 1.0388 0.8813 0.1182 0.033 Uiso 1 1 calc R
H12C H 1.0595 0.8425 -0.0046 0.033 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'
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
Cu1 Br1 Cu1 72.154(11) . 2_585
Cu2 Br2 Cu3 69.081(10) . .
Cu3 Br3 Cu3 80.299(11) . 2_675
Cu3 Br3 Cu2 65.995(10) . .
Cu3 Br3 Cu2 106.676(12) 2_675 .
S2 Cu1 S1 106.581(18) 2_675 .
S2 Cu1 Br1 114.921(16) 2_675 .
S1 Cu1 Br1 105.611(17) . .
S2 Cu1 Br1 117.561(17) 2_675 2_585
S1 Cu1 Br1 102.965(15) . 2_585
Br1 Cu1 Br1 107.846(11) . 2_585
S2 Cu1 Cu1 138.659(18) 2_675 2_585
S1 Cu1 Cu1 114.759(16) . 2_585
Br1 Cu1 Cu1 54.276(9) . 2_585
Br1 Cu1 Cu1 53.571(11) 2_585 2_585
S3 Cu2 S1 114.420(19) . .
S3 Cu2 Br2 114.084(17) . .
S1 Cu2 Br2 108.173(15) . .
S3 Cu2 Br3 103.050(16) . .
S1 Cu2 Br3 108.278(17) . .
Br2 Cu2 Br3 108.465(11) . .
S3 Cu2 Cu3 136.593(17) . .
S1 Cu2 Cu3 108.357(17) . .
Br2 Cu2 Cu3 55.943(9) . .
Br3 Cu2 Cu3 54.953(10) . .
S2 Cu3 Br2 99.685(16) . .
S2 Cu3 Br3 121.186(16) . .
Br2 Cu3 Br3 111.458(12) . .
S2 Cu3 Br3 103.812(16) . 2_675
Br2 Cu3 Br3 122.340(13) . 2_675
Br3 Cu3 Br3 99.701(11) . 2_675
S2 Cu3 Cu2 140.895(17) . .
Br2 Cu3 Cu2 54.976(11) . .
Br3 Cu3 Cu2 59.052(10) . .
Br3 Cu3 Cu2 114.862(13) 2_675 .
C4 S1 C1 101.43(8) . .
C4 S1 Cu2 108.12(6) . .
C1 S1 Cu2 111.29(6) . .
C4 S1 Cu1 106.26(7) . .
C1 S1 Cu1 102.11(6) . .
Cu2 S1 Cu1 125.08(2) . .
C12 S2 C9 100.91(10) . .
C12 S2 Cu1 109.01(7) . 2_675
C9 S2 Cu1 109.65(6) . 2_675
C12 S2 Cu3 103.65(7) . .
C9 S2 Cu3 107.38(6) . .
Cu1 S2 Cu3 123.78(2) 2_675 .
C8 S3 C5 101.68(10) . .
C8 S3 Cu2 106.87(7) . .
C5 S3 Cu2 104.97(7) . .
C2 C1 S1 115.54(12) . .
C2 C1 H1A 108.4 . .
S1 C1 H1A 108.4 . .
C2 C1 H1B 108.4 . .
S1 C1 H1B 108.4 . .
H1A C1 H1B 107.5 . .
C1 C2 C3 110.99(15) . .
C1 C2 H2A 109.4 . .
C3 C2 H2A 109.4 . .
C1 C2 H2B 109.4 . .
C3 C2 H2B 109.4 . .
H2A C2 H2B 108.0 . .
C2 C3 H3A 109.5 . .
C2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
S1 C4 H4A 109.5 . .
S1 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
S1 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C6 C5 S3 114.30(14) . .
C6 C5 H5A 108.7 . .
S3 C5 H5A 108.7 . .
C6 C5 H5B 108.7 . .
S3 C5 H5B 108.7 . .
H5A C5 H5B 107.6 . .
C5 C6 C7 110.89(18) . .
C5 C6 H6A 109.5 . .
C7 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
C7 C6 H6B 109.5 . .
H6A C6 H6B 108.0 . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
S3 C8 H8A 109.5 . .
S3 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
S3 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C10 C9 S2 110.20(13) . .
C10 C9 H9A 109.6 . .
S2 C9 H9A 109.6 . .
C10 C9 H9B 109.6 . .
S2 C9 H9B 109.6 . .
H9A C9 H9B 108.1 . .
C11 C10 C9 111.45(18) . .
C11 C10 H10A 109.3 . .
C9 C10 H10A 109.3 . .
C11 C10 H10B 109.3 . .
C9 C10 H10B 109.3 . .
H10A C10 H10B 108.0 . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
S2 C12 H12A 109.5 . .
S2 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
S2 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 Cu1 2.4508(4) .
Br1 Cu1 2.4729(4) 2_585
Br2 Cu2 2.4420(4) .
Br2 Cu3 2.4705(3) .
Br3 Cu3 2.4963(4) .
Br3 Cu3 2.5180(4) 2_675
Br3 Cu2 2.6150(4) .
Cu1 S2 2.2604(5) 2_675
Cu1 S1 2.3219(5) .
Cu1 Br1 2.4729(4) 2_585
Cu1 Cu1 2.8995(5) 2_585
Cu2 S3 2.2634(6) .
Cu2 S1 2.2802(5) .
Cu2 Cu3 2.7854(4) .
Cu3 S2 2.3103(5) .
Cu3 Br3 2.5180(4) 2_675
S1 C4 1.8028(18) .
S1 C1 1.8114(17) .
S2 C12 1.8045(19) .
S2 C9 1.8141(19) .
S2 Cu1 2.2604(5) 2_675
S3 C8 1.798(2) .
S3 C5 1.818(2) .
C1 C2 1.512(2) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 C3 1.526(3) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 C6 1.511(3) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 C7 1.517(3) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 C10 1.517(3) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 C11 1.515(3) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
