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_7117318
_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         'C51 H101 N2 P5 Re6 Se8, 2(C7 H7 O3 S)'
_chemical_formula_sum            'C65 H115 N2 O6 P5 Re6 S2 Se8'
_chemical_formula_weight         2988.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-04-10 deposited with the CCDC.
2015-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.4338(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.8853(18)
_cell_length_b                   12.9302(18)
_cell_length_c                   25.069(4)
_cell_measurement_reflns_used    9511
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.22
_cell_volume                     4173.0(11)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF-2008 (Beurskens et al., 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w 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  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            33854
_diffrn_reflns_theta_full        26.52
_diffrn_reflns_theta_max         26.52
_diffrn_reflns_theta_min         0.81
_exptl_absorpt_coefficient_mu    12.348
_exptl_absorpt_correction_T_max  0.5606
_exptl_absorpt_correction_T_min  0.0628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.378
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2792
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone/diethylether'
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         6.488
_refine_diff_density_min         -2.262
_refine_diff_density_rms         0.350
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.394(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     856
_refine_ls_number_reflns         17244
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0897P)^2^+20.3890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1345
_refine_ls_wR_factor_ref         0.1441
_reflns_number_gt                14538
_reflns_number_total             17244
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c5cc03215f2.cif
_cod_data_source_block           isu1201
_cod_original_cell_volume        4173.0(10)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7117318