Synthesis and crystal structure of 1,3-di-<i>tert</i>-butyl-2-chloro-4,4-diphenyl-1,3,2λ^3^,4-diazaphosphasiletidine
Mo, Dennis; Frank, Walter; Acta Crystallographica Section E 75 (2019) 405–409; doi:10.1107/S2056989019002627

data_2242860
_publ_section_title
;
 Synthesis and crystal structure of
 1,3-di-<i>tert</i>-butyl-2-chloro-4,4-diphenyl-1,3,2\l^3^,4-diazaphosphasiletidine
;
_journal_coeditor_code           PK2614
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              405
_journal_page_last               409
_journal_paper_doi               10.1107/S2056989019002627
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          'C20 H28 Cl N2 P Si'
_chemical_formula_moiety         'C20 H28 Cl N2 P Si'
_chemical_formula_sum            'C20 H28 Cl N2 P Si'
_chemical_formula_weight         390.95
_chemical_melting_point          393.5
_chemical_name_systematic
;
1,3-Di-<i>tert</i>-butyl-2-chloro-4,4-diphenyl-1,3,2\l^3^,4-\
diazaphosphasiletidine
;
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 95.739(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4004(7)
_cell_length_b                   15.6272(6)
_cell_length_c                   10.3817(5)
_cell_measurement_reflns_used    12536
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.645
_cell_measurement_theta_min      2.605
_cell_volume                     2163.14(18)
_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 (Brandenburg, 2016)
;
_computing_publication_material
;
<i>SHELXL2014/7</i> (Sheldrick, 2015b) and publCIF (Westrip,
2010)
;
_computing_structure_refinement
;
<i>SHELXL2014/7</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0643
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.097
_diffrn_reflns_theta_min         2.607
_diffrn_source                   'sealed tube'
_diffrn_standards_number         11994
_exptl_absorpt_coefficient_mu    0.312
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_correction_T_min  0.688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SHELXTL; Sheldrick, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.269
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1837 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.08(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.495
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         5765
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.501
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0080P)^2^+1.4244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1038
_reflns_number_gt                4920
_reflns_number_total             5765
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk2614sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2242860
_cod_database_fobs_code          2242860
_shelx_estimated_absorpt_t_min   0.875
_shelx_estimated_absorpt_t_max   0.937
_shelx_hkl_checksum              22070
_shelx_res_checksum              87833