Synthesis and Characterization of Rhenium Phosphinothiolate Complexes. Crystal and Molecular Structures of [HNEt3][Re{P(C6H4S)3}2], [ReOCl{OP(C6H5)2(C6H4S)}{(P(C6H5)2(C6H4S)}], [Re2O5{P(C6H5)2(C6H4S)}2], and [ReOCl{OP(C6H5)2(2-SC6H3-3-SiMe3)}2]
Paulo Perez-Lourido; J. Romero; J. Garcia-Vazquez; Antonio Sousa; Kevin P. Maresca; David J. Rose; Jon Zubieta; Inorganic Chemistry 37 (1998) 3331–3336; doi:10.1021/ic9715299

data_4322859
_publ_section_title
;
 Synthesis and Characterization of Rhenium Phosphinothiolate Complexes.
 Crystal and Molecular Structures of [HNEt3][Re{P(C6H4S)3}2],
 [ReOCl{OP(C6H5)2(C6H4S)}{(P(C6H5)2(C6H4S)}], [Re2O5{P(C6H5)2(C6H4S)}2],
 and [ReOCl{OP(C6H5)2(2-SC6H3-3-SiMe3)}2]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3331
_journal_page_last               3336
_journal_paper_doi               10.1021/ic9715299
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C36 H28 O5 P2 Re2 S2'
_chemical_formula_weight         1039.04
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 93.65
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6714(1)
_cell_length_b                   24.0076(2)
_cell_length_c                   13.363(1)
_cell_measurement_temperature    293(2)
_cell_volume                     3416.6(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21876
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    7.338
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    2.020
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          .125
_exptl_crystal_size_mid          .115
_exptl_crystal_size_min          .06
_refine_diff_density_max         2.700
_refine_diff_density_min         -2.827
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.125
_refine_ls_goodness_of_fit_obs   1.141
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         8073
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_restrained_S_obs      1.141
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_obs          0.0469
_refine_ls_shift/esd_max         0.065
_refine_ls_shift/esd_mean        0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+29.2187P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1219
_refine_ls_wR_factor_obs         0.1181
_reflns_number_observed          7392
_reflns_number_total             8073
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9715299_2.cif
_cod_data_source_block           dave163
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'Monclinic' was replaced with
'monoclinic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+29.2187P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+29.2187P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3416.51(4)
_cod_original_formula_sum        'C36 H28 O5 P2 S2 Re2'
_cod_database_code               4322859