Synthesis and Structural Characterization of Novel Terminal and Bridging Re(V)-Sulfido Complexes
Josemon Jacob; Ilia A. Guzei; James H. Espenson; Inorganic Chemistry 38 (1999) 3266–3267; doi:10.1021/ic990354v

data_4322145
_publ_contact_author_address
;
   Department of Chemistry
   Iowa State University of Science and Technology
   Ames, Iowa, 50011
   USA
;
_publ_contact_author_email       iguzei@iastate.edu
_publ_contact_author_fax         +515-294-5717
_publ_contact_author_name
;
Ilia A. Guzei
;
_publ_contact_author_phone       +515-294-6419
_publ_section_title
;
 Synthesis and Structural Characterization of Novel Terminal and Bridging
 Re(V)-Sulfido Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3266
_journal_page_last               3267
_journal_paper_doi               10.1021/ic990354v
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C29 H27 P Re S3'
_chemical_formula_weight         688.86
_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                 91.2370(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2936(5)
_cell_length_b                   22.2088(12)
_cell_length_c                   13.0576(7)
_cell_measurement_temperature    173(2)
_cell_volume                     2694.5(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0491
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5496
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    4.818
_exptl_absorpt_correction_T_max  0.6992
_exptl_absorpt_correction_T_min  0.2204
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         5496
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0080P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0416
_refine_ls_wR_factor_ref         0.0436
_reflns_number_gt                4280
_reflns_number_total             5496
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990354v_1.cif
_cod_data_source_block           esp06
_cod_database_code               4322145