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_4319019
_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            'C22 H52 N4 P2 Si2'
_chemical_formula_weight         490.80
_chemical_name_systematic        PhetPhos
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 114.147(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.5368(16)
_cell_length_b                   10.4604(17)
_cell_length_c                   12.6864(14)
_cell_measurement_reflns_used    53
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      12.77
_cell_measurement_theta_min      4.31
_cell_volume                     1518.1(4)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_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      292(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w 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  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3400
_diffrn_reflns_theta_full        25.29
_diffrn_reflns_theta_max         25.29
_diffrn_reflns_theta_min         1.78
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.238
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.074
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.48
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2656
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.038
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+0.4708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1264
_reflns_number_gt                2310
_reflns_number_total             2656
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020524v_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4319019