Comparison of Two Phosphinidenes Binding to Silicon(IV)dichloride as well as to Silylene.
Kundu, Subrata; Sinhababu, Soumen; Siddiqui, Mujahuddin M.; Luebben, Anna V.; Dittrich, Birger; Yang, Tao; Frenking, Gernot; Roesky, Herbert W.; Journal of the American Chemical Society 140 (2018) 9409–9412; doi:10.1021/jacs.8b06230

data_4132773
_publ_section_title
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 Comparison of Two Phosphinidenes Binding to Silicon(IV)dichloride as well
 as to Silylene.
;
_journal_issue                   30
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9409
_journal_page_last               9412
_journal_paper_doi               10.1021/jacs.8b06230
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         '2(C60 H93 N3 P2 Si), C6 H14'
_chemical_formula_sum            'C126 H200 N6 P4 Si2'
_chemical_formula_weight         1978.97
_chemical_name_common            (cAAC)Si{P(cAAC)}2
_chemical_name_systematic        bisphosphinidenesilylene
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
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2018-06-12 # Formatted by publCIF

;
_cell_angle_alpha                97.348(2)
_cell_angle_beta                 101.539(2)
_cell_angle_gamma                105.097(2)
_cell_formula_units_Z            2
_cell_length_a                   13.3897(6)
_cell_length_b                   16.8613(7)
_cell_length_c                   28.7050(12)
_cell_measurement_reflns_used    9065
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.2355
_cell_measurement_theta_min      2.1835
_cell_volume                     6018.5(5)
_computing_cell_refinement       'SAINT V8.34A'
_computing_data_collection       'APEX2 v2012.2'
_computing_data_reduction        'SAINT V8.34A'
_computing_molecular_graphics    'XP Version 5.1'
_computing_publication_material  'XP Version 5.1'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0810
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            146696
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.814
_diffrn_reflns_theta_min         1.345
_diffrn_source                   'INCOATEC Microsource'
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_description       block
_exptl_crystal_F_000             2172
_exptl_crystal_size_max          0.291
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.112
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1408
_refine_ls_number_reflns         23097
_refine_ls_number_restraints     439
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+4.1893P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1195
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17607
_reflns_number_total             23097
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b06230_si_003.cif
_cod_data_source_block           avl_skr334
_cod_database_code               4132773
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.963
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              28967
_shelx_hkl_checksum              48221
_publcif_funding_html
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