Crystal structure of <i>O</i>-isopropyl [bis(trimethylsilyl)amino](<i>tert</i>-butylamino)phosphinothioate
Kovalenko, Oleksandr O.; Kinzhybalo, Vasyl; Brusylovets, Oleksii A.; Lis, Tadeusz; Acta Crystallographica Section E 71 (2015) o37–o38; doi:10.1107/S205698901402622X

data_2240292
_publ_section_title
;
 Crystal structure of <i>O</i>-isopropyl
 [bis(trimethylsilyl)amino](<i>tert</i>-butylamino)phosphinothioate
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o37
_journal_page_last               o38
_journal_paper_doi               10.1107/S205698901402622X
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C13 H35 N2 O P S Si2'
_chemical_formula_moiety         'C13 H35 N2 O P S Si2'
_chemical_formula_sum            'C13 H35 N2 O P S Si2'
_chemical_formula_weight         354.64
_chemical_name_systematic
;
<i>O</i>-Isopropyl
[bis(trimethylsilyl)amino](<i>tert</i>-butylamino)phosphinothioate
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 100.52(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.942(3)
_cell_length_b                   11.907(3)
_cell_length_c                   17.726(5)
_cell_measurement_reflns_used    25646
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.6
_cell_measurement_theta_min      4
_cell_volume                     2063.1(10)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2003)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2003)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2003)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS2014 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type
;
Oxford Xcalibur PX \k-geometry diffractometer with a CCD area detector
;
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            36939
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.579
_diffrn_reflns_theta_min         4.718
_exptl_absorpt_coefficient_mu    0.35
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.84
_refine_diff_density_min         -0.34
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         7436
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.071P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1154
_reflns_number_gt                5938
_reflns_number_total             7436
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            xu5831sup1.cif
_cod_data_source_block           I
_cod_database_code               2240292
_cod_database_fobs_code          2240292
_shelx_estimated_absorpt_t_min   0.902
_shelx_estimated_absorpt_t_max   0.933
_shelx_hkl_checksum              18524
_shelx_res_checksum              35729