Synthesis and Chemistry of Bis(borylphosphino)silanes and -germanes
Tuqiang Chen; Eileen N. Duesler; Robert T. Paine; Heinrich Nöth; Inorganic Chemistry 38 (1999) 4993–4999; doi:10.1021/ic990507e

data_4322354
_publ_section_title
;
 Synthesis and Chemistry of Bis(borylphosphino)silanes and -germanes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4993
_journal_page_last               4999
_journal_paper_doi               10.1021/ic990507e
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C44 H86 B2 Ge Li2 N4 O4 P2'
_chemical_formula_weight         905.20
_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-97
_cell_angle_alpha                91.170(1)
_cell_angle_beta                 101.43(1)
_cell_angle_gamma                110.05(1)
_cell_formula_units_Z            2
_cell_length_a                   11.083(1)
_cell_length_b                   14.978(1)
_cell_length_c                   18.134(2)
_cell_measurement_reflns_used    42
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.76
_cell_measurement_theta_min      2.00
_cell_volume                     2758.9(5)
_computing_cell_refinement       'XSCANS V2.2 (Siemens, 1994)'
_computing_data_collection       'XSCANS V2.2 (Siemens, 1994)'
_computing_data_reduction        'XSCANS V2.2 (Siemens, 1994)'
_computing_molecular_graphics    'SHELXTL V5.0 (Siemens, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full .998
_diffrn_measured_fraction_theta_max .998
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       'profile data from \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  0.0579
_diffrn_reflns_av_sigmaI/netI    0.1422
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14351
_diffrn_reflns_theta_full        22.51
_diffrn_reflns_theta_max         22.51
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        5.2%
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.651
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8077
_exptl_absorpt_correction_type   'psi-scan corrections'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular plate'
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.667
_exptl_crystal_size_mid          0.322
_exptl_crystal_size_min          0.115
_refine_diff_density_max         .352
_refine_diff_density_min         -.312
_refine_diff_density_rms         .043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         7202
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
 [0.00000+1.00000exp(5.00(sin\q/\l)^2^)]/
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0300P)^2^+0.0000sin\q/\l]
 where P = 0.33333Fo^2^ + 0.66667Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0918
_reflns_number_gt                3832
_reflns_number_total             7202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990507e_2.cif
_cod_data_source_block           rtp945/13
_cod_original_cell_volume        2758.9(4)
_cod_database_code               4322354