Organometallic rhenium(III) chalcogenide clusters: coordination of N-heterocyclic carbenes
Jessica L. Durham; Wade B. Wilson; Daniel N. Huh; Robert McDonald; Lisa F. Szczepura; Chem.Commun. 51 (2015) 10536–; doi:10.1039/C5cc03215F

data_7117319
_publ_section_title
;
 Organometallic rhenium(III) chalcogenide clusters: coordination of
 N-heterocyclic carbenes
;
_journal_name_full               Chem.Commun.
_journal_page_first              10536
_journal_paper_doi               10.1039/C5cc03215F
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C54 H78 Cl2 N4 P2 Re6 S8, C H2 Cl2'
_chemical_formula_sum            'C55 H80 Cl4 N4 P2 Re6 S8'
_chemical_formula_weight         2374.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-04-09 deposited with the CCDC.
2015-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.1776(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6282(11)
_cell_length_b                   16.7446(11)
_cell_length_c                   25.1262(17)
_cell_measurement_reflns_used    9532
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.34
_cell_volume                     6990.9(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'DIRDIF-2008 (Beurskens et al., 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            248189
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.312
_diffrn_reflns_theta_min         1.462
_exptl_absorpt_coefficient_mu    10.823
_exptl_absorpt_correction_T_max  0.1085
_exptl_absorpt_correction_T_min  0.0433
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.256
_exptl_crystal_description       prism
_exptl_crystal_F_000             4456
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/diethylether'
_exptl_crystal_size_max          0.344
_exptl_crystal_size_mid          0.322
_exptl_crystal_size_min          0.186
_refine_diff_density_max         2.571
_refine_diff_density_min         -2.745
_refine_diff_density_rms         0.241
_refine_ls_extinction_coef       0.000110(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     708
_refine_ls_number_reflns         33649
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0492
_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/[\s^2^(Fo^2^)+(0.0583P)^2^+240.3996P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1472
_refine_ls_wR_factor_ref         0.1555
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                28321
_reflns_number_total             33649
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc03215f2.cif
_cod_data_source_block           isu1403
_cod_database_code               7117319
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.118
_shelx_estimated_absorpt_t_max   0.238
_shelx_res_checksum              25252