Crystal structure of 2-chloro-1,3-di-tert-pentyl-4,4-diphenyl-1,3,2λ 3,4-diazaphosphasiletidine, C22H32ClN2PSi
Mo, Dennis; Serio, Marcel; Frank, Walter; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 139–142; doi:10.1515/ncrs-2017-0226

data_8106076
_publ_section_title
;
 Crystal structure of 2-chloro-1,3-di-tert-pentyl-4,4-diphenyl-1,3,2\l
 3,4-diazaphosphasiletidine, C22H32ClN2PSi
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              139
_journal_page_last               142
_journal_paper_doi               10.1515/ncrs-2017-0226
_journal_volume                  233
_journal_year                    2018
_chemical_formula_moiety         'C22 H32 Cl N2 P Si'
_chemical_formula_sum            'C22 H32 Cl N2 P Si'
_chemical_formula_weight         419.01
_chemical_name_systematic
;
2-chloro-1,3-di-<i>tert</i>-pentyl-4,4-diphenyl-1,3,2\l^3^,4-
diazaphosphasiletidine
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                77.694(2)
_cell_angle_beta                 84.144(2)
_cell_angle_gamma                89.029(2)
_cell_formula_units_Z            4
_cell_length_a                   11.8482(3)
_cell_length_b                   12.8044(3)
_cell_length_c                   15.6562(4)
_cell_measurement_reflns_used    75943
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.71
_cell_measurement_theta_min      2.07
_cell_volume                     2308.48(10)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2009)'
_computing_data_collection       'X-Area (Stoe & Cie, 2009)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2009)'
_computing_molecular_graphics    'Diamond ver. 3.0a [2]'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)[1]'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)[1]'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)[1]'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            62121
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.271
_diffrn_reflns_theta_min         2.076
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SHELXTL
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       isometric
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.49
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         12461
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0255P)^2^+1.5111P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1148
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11305
_reflns_number_total             12461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2017-0226_suppl.cif
_cod_data_source_block           Pro_573
_cod_database_code               8106076
_shelx_estimated_absorpt_t_min   0.866
_shelx_estimated_absorpt_t_max   0.866
_shelx_res_checksum              35258
_shelx_hkl_checksum              69028