<i>N</i>,<i>N</i>'-Bis(5,5-dimethyl-2-thioxo-1,3,2-dioxaphosphinan-2-yl)ethane-1,2-diamine
Hai-Bing Li; Ya Li; De-Jun Xiong; De-Mei Tian; Acta Crystallographica Section E 63 (2007) o606–o607; doi:10.1107/S1600536807000694

data_2212406
_publ_section_title
<i>N</i>,<i>N</i>'-Bis(5,5-dimethyl-2-thioxo-1,3,2-dioxaphosphinan-2-yl)ethane-1,2-diamine
_journal_coeditor_code           WN2104
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o606
_journal_page_last               o607
_journal_paper_doi               10.1107/S1600536807000694
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C12 H26 N2 O4 P2 S2'
_chemical_formula_moiety         'C12 H26 N2 O4 P2 S2'
_chemical_formula_sum            'C12 H26 N2 O4 P2 S2'
_chemical_formula_weight         388.41
_chemical_name_systematic
;
N,N'-Bis(5,5-dimethyl-2-thioxo-1,3,2-dioxaphosphinan-2-yl)ethane-1,2-diamine
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.560(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.545(2)
_cell_length_b                   11.2714(16)
_cell_length_c                   12.1561(18)
_cell_measurement_reflns_used    2386
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.00
_cell_measurement_theta_min      2.30
_cell_volume                     1970.7(5)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w'
_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  0.0579
_diffrn_reflns_av_sigmaI/netI    0.0639
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14414
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.30
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.448
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.310
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         4296
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0697P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1490
_reflns_number_gt                2741
_reflns_number_total             4296
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wn2104.cif
_cod_data_source_block           I
_cod_original_cell_volume        1970.8(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2212406
_cod_database_fobs_code          2212406