2,4,8,10,13-Pentamethyl-6-phenyl-13,14-dihydro-12<i>H</i>-6λ^5^-dibenzo[<i>d</i>,<i>i</i>][1,3,7,2]dioxazaphosphecin-6-thione
Krishnaiah, M.; Babu, V.H.H. Surendra; Sankar, A. Uma Ravi; Raju, C. Naga; Kant, Rajni; Acta Crystallographica Section E 66 (2010) o120–; doi:10.1107/S1600536809052180

data_2224732
_publ_section_title
2,4,8,10,13-Pentamethyl-6-phenyl-13,14-dihydro-12<i>H</i>-6\l^5^-dibenzo[<i>d</i>,<i>i</i>][1,3,7,2]dioxazaphosphecin-6-thione
_journal_coeditor_code           PB2015
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o120
_journal_paper_doi               10.1107/S1600536809052180
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C25 H28 N O2 P S'
_chemical_formula_moiety         'C25 H28 N O2 P S'
_chemical_formula_sum            'C25 H28 N O2 P S'
_chemical_formula_weight         437.52
_chemical_name_systematic
;
2,4,8,10,13-Pentamethyl-6-phenyl-13,14-dihydro-12<i>H</i>-6\l^5^-
dibenzo[<i>d</i>,<i>i</i>][1,3,7,2]dioxazaphosphecin-6-thione
;
_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                 99.525(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7117(9)
_cell_length_b                   16.3225(16)
_cell_length_c                   16.9021(16)
_cell_measurement_reflns_used    7063
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.2
_cell_measurement_theta_min      3.1
_cell_volume                     2370.3(4)
_computing_cell_refinement       'CryAlis PRO (Oxford Diffraction, 2007)'
_computing_data_collection       'CryAlis PRO (Oxford Diffraction, 2007)'
_computing_data_reduction        'CryAlis RED (Oxford Diffraction, 2007)'
_computing_molecular_graphics    'ZORTEPII (Zsolnai, 1997)'
_computing_publication_material  'PARST (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'X-ray diffractometer with CCD camera'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur'
_diffrn_measurement_method       \w-2\q
_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  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0653
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21854
_diffrn_reflns_theta_full        30.24
_diffrn_reflns_theta_max         30.24
_diffrn_reflns_theta_min         3.10
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.225
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_meas      1.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.287
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         7063
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1027
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0805P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1399
_refine_ls_wR_factor_ref         0.1614
_reflns_number_gt                3672
_reflns_number_total             7063
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pb2015.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_hbond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_geom_hbond_publ_flag' value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2224732
_cod_database_fobs_code          2224732