<i>N</i>,<i>N</i>',<i>N</i>'',<i>N</i>'''-Tetrakis(2-methylphenyl)oxybis(phosphonic diamide): a redetermination at 150K with Mo <i>K</i>α radiation
Pourayoubi, Mehrdad; Padělková, Zdeňka; Rostami Chaijan, Mahnaz; R°užička, Aleš; Acta Crystallographica Section E 67 (2011) o450–o451; doi:10.1107/S1600536811002091

data_2229235
_publ_section_title
;
 <i>N</i>,<i>N</i>',<i>N</i>'',<i>N</i>'''-Tetrakis(2-methylphenyl)oxybis(phosphonic
 diamide): a redetermination at 150K with Mo <i>K</i>\a radiation
;
_journal_coeditor_code           SJ5092
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o450
_journal_page_last               o451
_journal_paper_doi               10.1107/S1600536811002091
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C28 H32 N4 O3 P2'
_chemical_formula_moiety         'C28 H32 N4 O3 P2'
_chemical_formula_sum            'C28 H32 N4 O3 P2'
_chemical_formula_weight         534.52
_chemical_name_common
;
<i>N</i>,<i>N</i>',<i>N</i>'',<i>N</i>'''-Tetrakis(2-
methylphenyl)oxybis(phosphonic diamide)
;
_chemical_name_systematic
;
<i>N</i>-{[bis(2-methylanilino)phosphoryloxy](2-
methylanilino)phosphoryl]}-2-methylaniline
;
_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
_cell_angle_beta                 118.915(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2621(6)
_cell_length_b                   15.7029(11)
_cell_length_c                   13.8401(8)
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     2713.2(3)
_computing_cell_refinement
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and Mercury (Macrae <i>et al.</i>, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1994)'
_diffrn_ambient_temperature      150.0(10)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker--Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_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  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19090
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens & Hamilton, 1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.505
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         6133
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0535
_refine_ls_shift/su_max_lt       0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+3.5968P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1211
_reflns_number_gt                4719
_reflns_number_total             6133
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj5092.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2229235
_cod_database_fobs_code          2229235