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_4322860
_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            'C44 H47 Cl N O3 P2 Re S2 Si2'
_chemical_formula_weight         1041.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                89.1080(10)
_cell_angle_beta                 83.6340(10)
_cell_angle_gamma                70.9010(10)
_cell_formula_units_Z            2
_cell_length_a                   10.1616(2)
_cell_length_b                   14.7095(3)
_cell_length_c                   17.0744(3)
_cell_measurement_temperature    150(1)
_cell_volume                     2396.21(8)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(1)
_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  0.0546
_diffrn_reflns_av_sigmaI/netI    0.0546
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10397
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    2.832
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       Rod
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          .125
_exptl_crystal_size_mid          .08
_exptl_crystal_size_min          .08
_refine_diff_density_max         7.247
_refine_diff_density_min         -3.360
_refine_diff_density_rms         0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.111
_refine_ls_goodness_of_fit_obs   1.132
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         6175
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_restrained_S_obs      1.132
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_obs          0.0837
_refine_ls_shift/esd_max         1.206
_refine_ls_shift/esd_mean        0.029
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0817P)^2^+69.0161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2085
_refine_ls_wR_factor_obs         0.2021
_reflns_number_observed          5624
_reflns_number_total             6175
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9715299_3.cif
_cod_data_source_block           kevm121
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0817P)^2^+69.0161P] 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^)+(0.0817P)^2^+69.0161P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C44 H47 N O3 Si2 P2 S2 Cl Re'
_cod_database_code               4322860