The Rhenium Tris(dithiolene) Electron Transfer Series: Calibrating Covalency
Stephen Sproules; Thomas Weyhermüller; Richard Goddard; Karl Wieghardt; Inorganic Chemistry 50 (2011) 12623–12631; doi:10.1021/ic2016534

data_4327119
_publ_section_title
;
 The Rhenium Tris(dithiolene) Electron Transfer Series: Calibrating
 Covalency
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12623
_journal_page_last               12631
_journal_paper_doi               10.1021/ic2016534
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         '(C24 H20 P)+, (C42 H30 Re S6)-, (C4 H9 N O)'
_chemical_formula_sum            'C70 H59 N O P Re S6'
_chemical_formula_weight         1339.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.539(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.1730(10)
_cell_length_b                   31.364(3)
_cell_length_c                   14.7187(12)
_cell_measurement_temperature    100(2)
_cell_volume                     5853.4(9)
_computing_cell_refinement       'Nonius Collect Software'
_computing_data_collection       'Nonius Collect Software'
_computing_data_reduction        'Nonius Collect Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
'3634 images at 0.5 deg. stepwise rotation in omega and phi, 5 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0151
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            304224
_diffrn_reflns_theta_full        32.50
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    2.364
_exptl_absorpt_correction_T_max  0.9114
_exptl_absorpt_correction_T_min  0.8712
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS 2008/1, Bruker AXS (2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_description       'opaque parallelepiped'
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.634
_refine_diff_density_min         -6.382
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.325
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     745
_refine_ls_number_reflns         21162
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.327
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.054
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+34.1882P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1116
_reflns_number_gt                19747
_reflns_number_total             21162
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2016534_si_002_2.cif
_cod_data_source_block           6321
_cod_original_cell_volume        5853.4(8)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4327119