Crystal structure of 1,3-di-<i>tert</i>-butyl-2-chloro-1,3,2-diazaphosphorinane {-} a saturated six-membered phosphorus nitrogen heterocycle with a partially flattened chair conformation and a long P^III^—Cl bond
Mecke, Erik; Frank, Walter; Acta Crystallographica Section E 75 (2019) 552–556; doi:10.1107/S2056989019004195

data_2242889
_publ_section_title
;
 Crystal structure of
 1,3-di-<i>tert</i>-butyl-2-chloro-1,3,2-diazaphosphorinane {-} a
 saturated six-membered phosphorus nitrogen heterocycle with a partially
 flattened chair conformation and a long P^III^---Cl bond
;
_journal_coeditor_code           PK2615
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              552
_journal_page_last               556
_journal_paper_doi               10.1107/S2056989019004195
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          'C11 H24 Cl N2 P'
_chemical_formula_moiety         'C11 H24 Cl N2 P'
_chemical_formula_sum            'C11 H24 Cl N2 P'
_chemical_formula_weight         250.74
_chemical_name_common
;
1,3-Di-<i>tert</i>-butyl-2-chloro-1,3,2-diazaphosphorinane
;
_chemical_name_systematic
;
1,3-Di-<i>tert</i>-butyl-2-chloro-1,3,2-diazaphosphinane
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 101.547(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5954(5)
_cell_length_b                   9.1549(3)
_cell_length_c                   12.9614(6)
_cell_measurement_reflns_used    20870
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      59.22
_cell_measurement_theta_min      4.45
_cell_volume                     1464.33(10)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2002)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2002)
;
_computing_data_reduction
;
X-AREA (Stoe & Cie, 2002)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2015)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a4)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16291
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.163
_diffrn_reflns_theta_min         2.743
_exptl_absorpt_coefficient_mu    0.347
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(XPREP; Bruker, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         3943
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0327P)^2^+0.8644P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1089
_reflns_number_gt                3547
_reflns_number_total             3943
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk2615sup1.cif
_cod_data_source_block           I
_cod_database_code               2242889
_cod_database_fobs_code          2242889
_shelx_estimated_absorpt_t_min   0.843
_shelx_estimated_absorpt_t_max   0.940
_shelx_hkl_checksum              35414
_shelx_res_checksum              74665