4-(2,4-Dichlorophenyl)-5,5-dimethyl-2-(3-silatranylpropylmino)-1,3,2-dioxaphosphorinane 2-oxide
Liu, Zhe-Rong; Tan, Xiao-Jing; Wang, De-Jian; Wang, Yan; Acta Crystallographica Section E 67 (2011) o3279–; doi:10.1107/S1600536811044928

data_2232929
_publ_section_title
;
 4-(2,4-Dichlorophenyl)-5,5-dimethyl-2-(3-silatranylpropylmino)-1,3,2-dioxaphosphorinane
 2-oxide
;
_journal_coeditor_code           RZ2656
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3279
_journal_paper_doi               10.1107/S1600536811044928
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C20 H31 Cl2 N2 O6 P Si'
_chemical_formula_moiety         'C20 H31 Cl2 N2 O6 P Si'
_chemical_formula_sum            'C20 H31 Cl2 N2 O6 P Si'
_chemical_formula_weight         525.43
_chemical_melting_point_gt       522
_chemical_melting_point_lt       523
_chemical_name_systematic
;
4-(2,4-Dichlorophenyl)-5,5-dimethyl-2-(3-silatranylpropylmino)-
1,3,2-dioxaphosphorinane 2-oxide
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                111.135(2)
_cell_angle_beta                 95.926(2)
_cell_angle_gamma                90.424(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7738(12)
_cell_length_b                   10.9320(13)
_cell_length_c                   11.2807(13)
_cell_measurement_reflns_used    1174
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      19.34
_cell_measurement_theta_min      2.23
_cell_volume                     1231.2(2)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0816
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6745
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.416
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_meas      1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.345
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         4720
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1037
_refine_ls_R_factor_gt           0.0654
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0969P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1634
_refine_ls_wR_factor_ref         0.1937
_reflns_number_gt                2997
_reflns_number_total             4720
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rz2656.cif
_cod_data_source_block           I
_cod_database_code               2232929
_cod_database_fobs_code          2232929