Inorganic Heterocyclic Bis(phosphines): Syntheses and Structures of a 1,2-Bis(diazasilaphosphetidino)ethane and Its Nickel, Molybdenum, and Rhodium Complexes
Ingo Schranz; Graham R. Lief; Steven J. Midstokke; Lothar Stahl; Inorganic Chemistry 41 (2002) 6919–6927; doi:10.1021/ic020524v

data_4319018
_publ_contact_author_address
;  Department of Chemistry
    University of North Dakota
    Grand Forks, ND 585620
    USA
;
_publ_contact_author_email       lstahl@chem.und.edu
_publ_contact_author_fax         '(701) 777-2331'
_publ_contact_author_name        'Lothar Stahl'
_publ_contact_author_phone       '(701) 777-2242'
_publ_section_title
;
 Inorganic Heterocyclic Bis(phosphines): Syntheses and Structures of a
 1,2-Bis(diazasilaphosphetidino)ethane and Its Nickel, Molybdenum, and
 Rhodium Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6919
_journal_page_last               6927
_journal_paper_doi               10.1021/ic020524v
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C30 H64 B F4 N4 P2 Rh Si2'
_chemical_formula_weight         788.69
_chemical_name_common            PhetPhosRh
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.064(2)
_cell_length_b                   18.3790(10)
_cell_length_c                   10.068(3)
_cell_measurement_temperature    293(2)
_cell_volume                     3897.7(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            4567
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.627
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          1.6
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.41(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         4060
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.639
_refine_ls_shift/su_mean         0.019
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0672P)^2^+1.9171P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1062
_reflns_number_gt                3567
_reflns_number_total             4060
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020524v_1.cif
_cod_data_source_block           5
_cod_original_formula_sum        C30H64BF4N4P2RhSi2
_cod_database_code               4319018