Reactivity of CuI and CuBr toward dialkyl sulfides RSR: from discrete molecular Cu4I4S4 and Cu8I8S6 clusters to luminescent copper(I) coordination polymers.
Knorr, Michael; Bonnot, Antoine; Lapprand, Antony; Khatyr, Abderrahim; Strohmann, Carsten; Kubicki, Marek M.; Rousselin, Yoann; Harvey, Pierre D.; Inorganic chemistry 54 (2015) 4076–4093; doi:10.1021/acs.inorgchem.5b00327

data_4346128
_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         'C36 H84 Cu8 I8 S6'
_chemical_formula_sum            'C36 H84 Cu8 I8 S6'
_chemical_formula_weight         2232.91
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        '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                88.548(16)
_cell_angle_beta                 79.375(17)
_cell_angle_gamma                63.600(16)
_cell_formula_units_Z            1
_cell_length_a                   11.0096(19)
_cell_length_b                   11.6305(17)
_cell_length_c                   14.205(3)
_cell_measurement_reflns_used    33352
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.7470
_cell_measurement_theta_min      2.5550
_cell_volume                     1598.0(6)
_computing_cell_refinement       'CrysAlis CCD, Oxford Diffraction Ltd.2012'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.2012'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.2012'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.0560
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega    3.00   90.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1462   57.0000    0.0000 87

  2 omega  -48.00   38.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1462  -57.0000 -150.0000 86

  3 omega  -48.00   40.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1462  -57.0000   30.0000 88

  4 omega    8.00   94.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1462   38.0000  -60.0000 86

  5 omega    2.00   91.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1462   38.0000  120.0000 89

  6 omega  -25.00   63.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1462  -99.0000  150.0000 88

  7 omega   -4.00   81.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1462   38.0000 -150.0000 85

  8 omega  -24.00   63.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1462  -99.0000  -30.0000 87

  9 omega  -25.00   20.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.0837  -99.0000 -150.0000 45

 10 omega    1.00   82.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1462 -131.0000  -41.0000 81

 11 omega   34.00   97.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1462  179.0000 -120.0000 63

 12 omega  -51.00   47.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1462  -38.0000  -90.0000 98

 13 omega  -92.00    8.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.0837  -77.0000   90.0000 100

 14 omega  -91.00   -1.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.0837  -57.0000 -150.0000 90

 15 omega  -25.00   20.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.0837  -99.0000   60.0000 45

 16 omega  -25.00   20.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.0837  -99.0000 -120.0000 45

 17 omega  -52.00   94.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1462    0.0000 -180.0000 146

 18 omega    0.00   90.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1462   57.0000  -60.0000 90

 19 omega    7.00   88.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1462 -140.0000  144.0000 81

 20 omega  -48.00   43.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1462  -57.0000  150.0000 91

 21 omega   34.00   97.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1462  179.0000   90.0000 63

 22 omega  -25.00   20.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.0837  -99.0000    0.0000 45

 23 omega  -91.00   -1.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.0837  -57.0000  150.0000 90

 24 omega  -52.00   94.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1462    0.0000 -120.0000 146

 25 omega  -52.00   94.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1462    0.0000  -90.0000 146

 26 omega  -52.00   94.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1462    0.0000 -150.0000 146
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            79854
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.32
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.692
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         7735
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0221
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+1.1172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0597
_refine_ls_wR_factor_ref         0.0608
_reflns_number_gt                7248
_reflns_number_total             7735
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00327_si_003.cif
_cod_data_source_block           shelx_compound_8a
_cod_original_cell_volume        1597.9(5)
_cod_database_code               4346128
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.038) H2A(0.058) H2B(0.058) H2C(0.058) H3A(0.069) H3B(0.069)
 H3C(0.069) H4(0.042) H5A(0.071) H5B(0.071) H5C(0.071) H6A(0.073) H6B(0.073)
 H6C(0.073) H7A(0.06) H7B(0.06) H7C(0.06) H8(0.039) H9A(0.069) H9B(0.069)
 H9C(0.069) H10(0.041) H11A(0.063) H11B(0.063) H11C(0.063) H12A(0.062)
 H12B(0.062) H12C(0.062) H13(0.052) H14A(0.086) H14B(0.086) H14C(0.086)
 H15A(0.112) H15B(0.112) H15C(0.112) H16(0.041) H17A(0.064) H17B(0.064)
 H17C(0.064) H18A(0.075) H18B(0.075) H18C(0.075)
 Fixed X: H1(0.2707) H2A(0.3347) H2B(0.4356) H2C(0.3983) H3A(0.1762)
 H3B(0.0584) H3C(0.092) H4(-0.0439) H5A(0.0132) H5B(-0.0752) H5C(-0.1327) H6A(-
 0.013) H6B(0.1024) H6C(0.1391) H7A(1.0113) H7B(0.8514) H7C(0.9232) H8(0.985)
 H9A(1.1035) H9B(1.1364) H9C(1.1855) H10(0.9835) H11A(0.8183) H11B(0.7864)
 H11C(0.6986) H12A(0.8288) H12B(0.9856) H12C(0.948) H13(0.7375) H14A(0.6363)
 H14B(0.6876) H14C(0.7964) H15A(0.8111) H15B(0.7071) H15C(0.6531) H16(0.4722)
 H17A(0.2977) H17B(0.2559) H17C(0.3147) H18A(0.5739) H18B(0.6629) H18C(0.5451)
 Fixed Y: H1(1.3411) H2A(1.2345) H2B(1.1865) H2C(1.3237) H3A(1.5062)
 H3B(1.4943) H3C(1.4348) H4(1.3778) H5A(1.133) H5B(1.1904) H5C(1.2583)
 H6A(1.3682) H6B(1.3939) H6C(1.2534) H7A(0.8241) H7B(0.8742) H7C(0.9673)
 H8(0.7406) H9A(0.9153) H9B(0.7928) H9C(0.7733) H10(0.8857) H11A(0.951)
 H11B(1.0634) H11C(0.9833) H12A(0.7412) H12B(0.6875) H12C(0.7228) H13(0.438)
 H14A(0.3232) H14B(0.2678) H14C(0.2672) H15A(0.4639) H15B(0.5993) H15C(0.5332)
 H16(0.373) H17A(0.4741) H17B(0.5568) H17C(0.6036) H18A(0.4872) H18B(0.3535)
 H18C(0.3661)
 Fixed Z: H1(0.2737) H2A(0.0807) H2B(0.1564) H2C(0.1127) H3A(0.1666)
 H3B(0.245) H3C(0.1376) H4(0.3214) H5A(0.3969) H5B(0.3146) H5C(0.4207)
 H6A(0.4842) H6B(0.4136) H6C(0.4509) H7A(0.3841) H7B(0.3804) H7C(0.3549)
 H8(0.2417) H9A(0.198) H9B(0.1305) H9C(0.2315) H10(0.0406) H11A(-0.06)
 H11B(0.0174) H11C(0.0329) H12A(0.0645) H12B(0.078) H12C(-0.0259) H13(0.2159)
 H14A(0.0935) H14B(0.1907) H14C(0.0986) H15A(0.0515) H15B(0.1083) H15C(0.0393)
 H16(0.2879) H17A(0.4211) H17B(0.3303) H17C(0.4086) H18A(0.4093) H18B(0.3469)
 H18C(0.4366)
;