Branched tetrasilane substituted phosphines ‒ synthesis and characterisation of PhSi(SiiPr2)3P and {PhSi(SiMe2)3}2P14
Michael Feierabend; Carsten von Hanisch; Chem.Commun. 50 (2014) 4416–; doi:10.1039/C4CC00165F

data_7112251
_publ_section_title
;
 Branched tetrasilane substituted phosphines -- synthesis and
 characterisation of PhSi(SiiPr2)3P and {PhSi(SiMe2)3}2P14
;
_journal_name_full               Chem.Commun.
_journal_page_first              4416
_journal_paper_doi               10.1039/C4CC00165F
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C69 H116 P28 Si16'
_chemical_formula_sum            'C69 H116 P28 Si16'
_chemical_formula_weight         2262.22
_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-97
_cell_angle_alpha                88.880(19)
_cell_angle_beta                 87.593(19)
_cell_angle_gamma                77.702(18)
_cell_formula_units_Z            1
_cell_length_a                   9.310(2)
_cell_length_b                   16.566(4)
_cell_length_c                   18.804(4)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.00
_cell_measurement_theta_min      1.26
_cell_volume                     2830.9(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.918
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method'
_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  0.1002
_diffrn_reflns_av_sigmaI/netI    0.2485
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12809
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    0.611
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1174
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.742
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         8177
_refine_ls_number_restraints     228
_refine_ls_restrained_S_all      0.741
_refine_ls_R_factor_all          0.1656
_refine_ls_R_factor_gt           0.0716
_refine_ls_shift/su_max          0.951
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0812P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1586
_refine_ls_wR_factor_ref         0.1803
_reflns_number_gt                3183
_reflns_number_total             8177
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc00165f2.cif
_cod_data_source_block           d_test_p14
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7112251