The crystal structure of 2-chloro-1,3-bis(2,4,6-trimethylphenyl)-4,4-dimethyl-1,3,2λ3,4-diazaphosphasiletidine
Breuers, Verena; Frank, Walter; Zeitschrift für Kristallographie - New Crystal Structures 231 (2016) 529–532; doi:10.1515/ncrs-2015-0176

data_8106930
_publ_section_title
;
 The crystal structure of
 2-chloro-1,3-bis(2,4,6-trimethylphenyl)-4,4-dimethyl-1,3,2\l3,4-diazaphosphasiletidine
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              529
_journal_page_last               532
_journal_paper_doi               10.1515/ncrs-2015-0176
_journal_volume                  231
_journal_year                    2016
_chemical_formula_moiety         'C19.88 H27.64 Cl1.12 N2 P Si'
_chemical_formula_sum            'C19.88 H27.64 Cl1.12 N2 P Si'
_chemical_formula_weight         393.36
_chemical_name_systematic
;
2-chloro-1,3-bis(2,4,6-trimethylphenyl)-4,4-dimethyl-1,3,2\l^3^,4-\
diazaphosphasiletidine
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.811(3)
_cell_length_b                   14.357(3)
_cell_length_c                   17.523(3)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      2.2
_cell_volume                     4229.3(14)
_computing_cell_refinement       'CELL (Stoe & Cie, 1996)'
_computing_data_collection       'EXPOSE (Stoe & Cie, 1996)'
_computing_data_reduction        'INTEGRATE (Stoe & Cie, 1996)'
_computing_molecular_graphics    'Diamond ver. 3.0a'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       \f-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            52947
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         2.198
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.334
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       plate
_exptl_crystal_F_000             1671
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3691
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0591P)^2^+2.6586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1089
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3344
_reflns_number_total             3691
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2015-0176_suppl.cif
_cod_data_source_block           1055
_cod_database_code               8106930