Crystal structure of 2-chloro-1,3-bis(2,6-diisopropylphenyl)-1,3,2-diazaphospholidine 2-oxide
Veinot, Alex J.; Hendsbee, Arthur D.; Masuda, Jason D.; Acta Crystallographica Section E 73 (2017) 735–737; doi:10.1107/S2056989017005825

data_2242203
_publ_section_title
;
 Crystal structure of
 2-chloro-1,3-bis(2,6-diisopropylphenyl)-1,3,2-diazaphospholidine 2-oxide
;
_journal_coeditor_code           HB7671
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              735
_journal_page_last               737
_journal_paper_doi               10.1107/S2056989017005825
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C26 H38 Cl N2 O P'
_chemical_formula_moiety         'C26 H38 Cl N2 O P'
_chemical_formula_sum            'C26 H38 Cl N2 O P'
_chemical_formula_weight         461.00
_chemical_name_systematic
;
2-Chloro-1,3-bis(2,6-diisopropylphenyl)-1,3,2-diazaphospholidine 2-oxide
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2016/4
_cell_angle_alpha                90
_cell_angle_beta                 106.818(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.984(3)
_cell_length_b                   6.6328(11)
_cell_length_c                   20.140(3)
_cell_measurement_reflns_used    4093
_cell_measurement_temperature    104(2)
_cell_measurement_theta_max      24.50
_cell_measurement_theta_min      2.53
_cell_volume                     2555.4(7)
_computing_cell_refinement
;
SAINT (Bruker, 2008)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and PLATON (Spek, 2009)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2016</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      104(2)
_diffrn_detector_area_resol_mean 66
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Siemens/Bruker APEXII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0732
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30194
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.394
_diffrn_reflns_theta_min         2.113
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.232
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_description       Block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.326
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         6307
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0435P)^2^+0.5837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1086
_reflns_number_gt                4640
_reflns_number_total             6307
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7671sup1.cif
_cod_data_source_block           I
_cod_database_code               2242203
_cod_database_fobs_code          2242203
_shelx_estimated_absorpt_t_min   0.944
_shelx_estimated_absorpt_t_max   0.962
_shelx_hkl_checksum              59638
_shelx_res_checksum              73495