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#$Date: 2016-03-25 15:46:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179935 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/30/7023005.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_7023005
loop_
_publ_author_name
'Friedrich, Dirk'
'Kluge, Oliver'
'Kischel, Marcus'
'Krautscheid, Harald'
_publ_section_title
;
 Tetranuclear organometallic complexes based on 1,2-ethanedithiolate
 ligands as potential precursors for CuMS2 (M = Ga, In).
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9613
_journal_page_last               9620
_journal_paper_doi               10.1039/c3dt50461a
_journal_volume                  42
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C38 H86 Cu2 In2 P2 S4'
_chemical_formula_sum            'C38 H86 Cu2 In2 P2 S4'
_chemical_formula_weight         1089.97
_chemical_name_common
;
bis(mu!3$-1,2-dithiolatoethane-S,S,S',S')-tetra(butan-1-ido) -
bis(triisopropylphosphine)-dicopper(+1)-diindium(+3)
;
_chemical_name_systematic
;
bis(μ₃-1,2-dithiolatoethane-S,S,S',S')-tetra(butan-1-ido)
-bis(triisopropylphosphine)-dicopper(+1)-diindium(+3)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_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_date             2012-10-12T13:08:47-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                118.253(5)
_cell_angle_beta                 98.990(5)
_cell_angle_gamma                90.370(5)
_cell_formula_units_Z            1
_cell_length_a                   10.988(5)
_cell_length_b                   11.495(5)
_cell_length_c                   11.649(5)
_cell_measurement_reflns_used    16732
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      25.82
_cell_measurement_theta_min      2.5
_cell_measurement_wavelength     0.71073
_cell_volume                     1274.7(10)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-AREA, STOE X-RED'
_computing_molecular_graphics    'DIAMOND 3.2'
_computing_publication_material
;
'WinGX publication routines'
Farrugia, L. J. (1999) WinGX, J. Appl. Cryst. 32, 837-838
;
_computing_structure_refinement
;
'SHELXL-97'
Sheldrick, G.M. (2008) Acta Cryst. A64, 112
;
_computing_structure_solution
;
'SIR-92'
Altomare, A., Cascarano, G.,
Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350.
;
_diffrn_ambient_temperature      213(2)
_diffrn_detector                 'image plate (34 cm diameter / schwenk)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.928
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS-2T'
_diffrn_measurement_method       'ω 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  0.0569
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14887
_diffrn_reflns_theta_full        25.77
_diffrn_reflns_theta_max         25.77
_diffrn_reflns_theta_min         2.5
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.97
_exptl_absorpt_correction_T_max  0.4985
_exptl_absorpt_correction_T_min  0.2653
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Busing, W. R. & Levy, H. A. (1957) Acta Cryst. 10, 180-182.
and
Coppens, P., Leiserowitz, L. & Rabinovich, D. (1965)
Acta Cryst. 1965, 1035-1038.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.42
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.88
_exptl_crystal_size_mid          0.68
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.607
_refine_diff_density_min         -1.193
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4542
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0895P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1227
_reflns_number_gt                3815
_reflns_number_total             4542
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50461a.txt
_cod_data_source_block           ip1_1157b
_cod_database_code               7023005
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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3344(5) 0.3309(5) 0.2788(5) 0.0615(12) Uani 1 1 d . . .
H1A H 0.3846 0.275 0.2142 0.074 Uiso 1 1 calc R . .
H1B H 0.2498 0.3197 0.231 0.074 Uiso 1 1 calc R . .
C2 C 0.6169(4) 0.5303(5) 0.6636(4) 0.0555(11) Uani 1 1 d . . .
H2A H 0.5286 0.5213 0.6272 0.067 Uiso 1 1 calc R . .
H2B H 0.625 0.5052 0.7338 0.067 Uiso 1 1 calc R . .
C3A C 0.5459(14) 0.1967(18) 0.6274(14) 0.041(3) Uani 0.499(16) 1 d PD A 1
H3A1 H 0.5208 0.2815 0.691 0.049 Uiso 0.499(16) 1 calc PR A 1
H3A2 H 0.4806 0.1281 0.6079 0.049 Uiso 0.499(16) 1 calc PR A 1
C4A C 0.6595(13) 0.170(3) 0.6944(14) 0.144(11) Uani 0.499(16) 1 d PD A 1
H4A1 H 0.6906 0.256 0.7717 0.173 Uiso 0.499(16) 1 calc PR A 1
H4A2 H 0.6301 0.115 0.7297 0.173 Uiso 0.499(16) 1 calc PR A 1
C5A C 0.7629(14) 0.116(3) 0.6467(18) 0.143(10) Uani 0.499(16) 1 d PD A 1
H5A1 H 0.7971 0.1727 0.6162 0.171 Uiso 0.499(16) 1 calc PR A 1
H5A2 H 0.7336 0.0306 0.5673 0.171 Uiso 0.499(16) 1 calc PR A 1
C6A C 0.8698(14) 0.089(3) 0.724(2) 0.076(5) Uani 0.499(16) 1 d PD A 1
H6A1 H 0.9367 0.1578 0.7549 0.114 Uiso 0.499(16) 1 calc PR A 1
H6A2 H 0.8977 0.0035 0.6681 0.114 Uiso 0.499(16) 1 calc PR A 1
H6A3 H 0.8444 0.0873 0.7996 0.114 Uiso 0.499(16) 1 calc PR A 1
C3B C 0.5715(14) 0.1702(19) 0.6039(18) 0.057(5) Uani 0.501(16) 1 d PD A 2
H3B1 H 0.5492 0.2469 0.6805 0.069 Uiso 0.501(16) 1 calc PR A 2
H3B2 H 0.5165 0.0927 0.583 0.069 Uiso 0.501(16) 1 calc PR A 2
C4B C 0.7039(11) 0.1462(15) 0.6370(14) 0.075(4) Uani 0.501(16) 1 d PD A 2
H4B1 H 0.7264 0.0753 0.5563 0.09 Uiso 0.501(16) 1 calc PR A 2
H4B2 H 0.7563 0.2267 0.6616 0.09 Uiso 0.501(16) 1 calc PR A 2
C5B C 0.7340(12) 0.1111(14) 0.7410(15) 0.094(5) Uani 0.501(16) 1 d PD A 2
H5B1 H 0.6828 0.0297 0.7159 0.112 Uiso 0.501(16) 1 calc PR A 2
H5B2 H 0.7108 0.1814 0.8217 0.112 Uiso 0.501(16) 1 calc PR A 2
C6B C 0.8662(17) 0.090(4) 0.773(3) 0.119(10) Uani 0.501(16) 1 d PD A 2
H6B1 H 0.8702 0.0093 0.7806 0.179 Uiso 0.501(16) 1 calc PR A 2
H6B2 H 0.9053 0.1646 0.8564 0.179 Uiso 0.501(16) 1 calc PR A 2
H6B3 H 0.909 0.0815 0.7031 0.179 Uiso 0.501(16) 1 calc PR A 2
C7 C 0.5835(5) 0.0637(6) 0.2477(6) 0.0798(18) Uani 1 1 d D A .
H7A H 0.5695 -0.0254 0.2373 0.096 Uiso 1 1 calc R . .
H7B H 0.521 0.0703 0.1816 0.096 Uiso 1 1 calc R . .
C8 C 0.7069(5) 0.0747(6) 0.2147(6) 0.0743(15) Uani 1 1 d D . .
H8A H 0.7701 0.0643 0.2778 0.089 Uiso 1 1 calc R . .
H8B H 0.7228 0.164 0.2264 0.089 Uiso 1 1 calc R . .
C9 C 0.7210(6) -0.0251(7) 0.0762(6) 0.092(2) Uani 1 1 d D . .
H9A H 0.7024 -0.1141 0.0641 0.111 Uiso 1 1 calc R . .
H9B H 0.6588 -0.013 0.0136 0.111 Uiso 1 1 calc R . .
C10 C 0.8412(9) -0.0195(10) 0.0416(10) 0.141(4) Uani 1 1 d D . .
H10A H 0.8334 0.006 -0.0274 0.211 Uiso 1 1 calc R . .
H10B H 0.8726 -0.106 0.0099 0.211 Uiso 1 1 calc R . .
H10C H 0.898 0.0453 0.1192 0.211 Uiso 1 1 calc R . .
C11 C 0.9665(4) 0.3640(5) 0.3020(5) 0.0571(11) Uani 1 1 d . . .
H11A H 1.0157 0.2901 0.2619 0.086 Uiso 1 1 calc R . .
H11B H 0.9037 0.3396 0.3388 0.086 Uiso 1 1 calc R . .
H11C H 1.0196 0.4401 0.372 0.086 Uiso 1 1 calc R . .
C12 C 0.9047(4) 0.3986(5) 0.1978(5) 0.0522(10) Uani 1 1 d . . .
H12 H 0.8539 0.3172 0.1277 0.063 Uiso 1 1 calc R . .
C13 C 1.0029(5) 0.4288(7) 0.1316(6) 0.0773(16) Uani 1 1 d . . .
H13A H 1.0604 0.5029 0.1983 0.116 Uiso 1 1 calc R . .
H13B H 0.9624 0.4512 0.0654 0.116 Uiso 1 1 calc R . .
H13C H 1.0476 0.3514 0.0896 0.116 Uiso 1 1 calc R . .
C14 C 0.9746(5) 0.7308(5) 0.4291(6) 0.0699(14) Uani 1 1 d . . .
H14A H 1.0111 0.8193 0.4571 0.105 Uiso 1 1 calc R . .
H14B H 1.0384 0.6697 0.4096 0.105 Uiso 1 1 calc R . .
H14C H 0.9371 0.7314 0.4994 0.105 Uiso 1 1 calc R . .
C15 C 0.8764(4) 0.6869(5) 0.3058(5) 0.0592(11) Uani 1 1 d . . .
H15 H 0.9172 0.6745 0.2313 0.071 Uiso 1 1 calc R . .
C16 C 0.7853(6) 0.7926(6) 0.3281(7) 0.0828(17) Uani 1 1 d . . .
H16A H 0.7404 0.8008 0.3966 0.124 Uiso 1 1 calc R . .
H16B H 0.7273 0.767 0.2464 0.124 Uiso 1 1 calc R . .
H16C H 0.8304 0.8771 0.3555 0.124 Uiso 1 1 calc R . .
C17 C 0.7148(6) 0.4987(9) 0.0049(6) 0.094(2) Uani 1 1 d . . .
H17A H 0.7722 0.4324 -0.0311 0.142 Uiso 1 1 calc R . .
H17B H 0.756 0.5862 0.0372 0.142 Uiso 1 1 calc R . .
H17C H 0.6443 0.4828 -0.0638 0.142 Uiso 1 1 calc R . .
C18 C 0.6705(4) 0.4904(6) 0.1195(5) 0.0653(13) Uani 1 1 d . . .
H18 H 0.6117 0.5587 0.1522 0.078 Uiso 1 1 calc R . .
C19 C 0.5985(5) 0.3565(7) 0.0738(6) 0.0802(17) Uani 1 1 d . . .
H19A H 0.5292 0.3412 0.004 0.12 Uiso 1 1 calc R . .
H19B H 0.568 0.3574 0.1481 0.12 Uiso 1 1 calc R . .
H19C H 0.6528 0.2861 0.0406 0.12 Uiso 1 1 calc R . .
P1 P 0.79472(9) 0.52705(12) 0.26416(11) 0.0455(2) Uani 1 1 d . . .
S1 S 0.33285(10) 0.27338(10) 0.39941(11) 0.0505(3) Uani 1 1 d . . .
S2 S 0.69787(9) 0.41422(10) 0.53002(10) 0.0444(2) Uani 1 1 d . A .
Cu1 Cu 0.71810(4) 0.54004(5) 0.43280(5) 0.04254(15) Uani 1 1 d . . .
In1 In 0.54972(3) 0.20513(3) 0.44188(3) 0.04953(14) 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.31 '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
C2 C1 S1 114.1(3) 2_666 .
C1 C2 S2 113.0(3) 2_666 .
C4A C3A In1 119.2(10) . .
C5A C4A C3A 130.2(12) . .
C4A C5A C6A 124.7(13) . .
C4B C3B In1 109.8(11) . .
C5B C4B C3B 117.4(13) . .
C4B C5B C6B 116.3(14) . .
C8 C7 In1 118.2(4) . .
C7 C8 C9 114.7(5) . .
C10 C9 C8 116.2(6) . .
C11 C12 C13 110.2(4) . .
C11 C12 P1 111.5(3) . .
C13 C12 P1 115.9(4) . .
C14 C15 C16 110.3(5) . .
C14 C15 P1 109.3(4) . .
C16 C15 P1 110.7(4) . .
C17 C18 C19 112.2(5) . .
C17 C18 P1 114.8(4) . .
C19 C18 P1 109.4(4) . .
C15 P1 C12 106.6(2) . .
C15 P1 C18 105.0(3) . .
C12 P1 C18 105.2(2) . .
C15 P1 Cu1 111.28(18) . .
C12 P1 Cu1 116.24(16) . .
C18 P1 Cu1 111.71(17) . .
C1 S1 Cu1 99.08(17) . 2_666
C1 S1 In1 106.71(17) . .
Cu1 S1 In1 116.06(5) 2_666 .
C2 S2 Cu1 98.03(17) . .
C2 S2 In1 98.24(15) . .
Cu1 S2 In1 127.35(5) . .
P1 Cu1 S2 138.00(5) . .
P1 Cu1 S1 126.23(5) . 2_666
S2 Cu1 S1 94.63(6) . 2_666
C3B In1 C7 124.0(5) . .
C3B In1 C3A 11.2(4) . .
C7 In1 C3A 133.9(5) . .
C3B In1 S1 110.8(4) . .
C7 In1 S1 104.87(18) . .
C3A In1 S1 100.9(3) . .
C3B In1 S2 101.9(5) . .
C7 In1 S2 108.22(16) . .
C3A In1 S2 100.5(5) . .
S1 In1 S2 105.76(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.465(7) 2_666
C1 S1 1.816(6) .
C2 C1 1.465(7) 2_666
C2 S2 1.864(5) .
C3A C4A 1.479(13) .
C3A In1 2.215(16) .
C4A C5A 1.367(13) .
C5A C6A 1.492(14) .
C3B C4B 1.506(14) .
C3B In1 2.09(2) .
C4B C5B 1.442(13) .
C5B C6B 1.494(16) .
C7 C8 1.486(7) .
C7 In1 2.165(5) .
C8 C9 1.507(7) .
C9 C10 1.449(10) .
C11 C12 1.515(7) .
C12 C13 1.546(6) .
C12 P1 1.863(5) .
C14 C15 1.518(7) .
C15 C16 1.531(8) .
C15 P1 1.848(5) .
C17 C18 1.533(8) .
C18 C19 1.535(9) .
C18 P1 1.866(5) .
P1 Cu1 2.1979(14) .
S1 Cu1 2.2633(13) 2_666
S1 In1 2.5616(15) .
S2 Cu1 2.2470(14) .
S2 In1 2.5635(13) .
Cu1 S1 2.2633(13) 2_666
