Tris[bis(diphenylphosphino)methane-κ^2^<i>P,P</i>']rhenium(I) perrhenate
Kenton H. Whitmire; Daniel R. Derringer; Kimberly R. Kongkasuwan; Acta Crystallographica Section E 58 (2002) m363–m365; doi:10.1107/S1600536802010838

data_2201429
_publ_section_title
;
 Tris[bis(diphenylphosphino)methane-\k^2^<i>P,P</i>']rhenium(I)
 perrhenate
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m363
_journal_page_last               m365
_journal_paper_doi               10.1107/S1600536802010838
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Re (C25 H22 P2)3] [Re O4]'
_chemical_formula_moiety         'C75 H66 P6 Re1 1+, O4 Re1 1-'
_chemical_formula_sum            'C75 H66 O4 P6 Re2'
_chemical_formula_weight         1589.50
_chemical_name_systematic
;
tris[bis(diphenylphosphino)methane]rhenium(I) perrhenate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.805(4)
_cell_length_b                   37.831(14)
_cell_length_c                   19.3318(18)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      5.9
_cell_measurement_theta_min      3.5
_cell_volume                     13022(6)
_computing_cell_refinement       TEXSAN
_computing_data_collection
;
TEXSAN (Molecular Structure Corporation, 1990)
;
_computing_data_reduction        TEXSAN
_computing_molecular_graphics    'SHELXTL-Plus (Siemens, 1993)'
_computing_publication_material  'SHELXTL93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Rigaku AFC-5S'
_diffrn_measurement_method       2\q-\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0657
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5937
_diffrn_reflns_theta_full        20.00
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         2.24
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.913
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular cut block'
_exptl_crystal_F_000             6304
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.962
_refine_diff_density_min         -0.957
_refine_ls_extinction_coef       constr
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         5937
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0455
_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^) + 156.3064P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1148
_reflns_number_gt                4208
_reflns_number_total             5937
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv6110.cif
_cod_data_source_block           I
_cod_database_code               2201429
_cod_database_fobs_code          2201429