Redetermined structure of diphenylphosphonimidotriphenylphosphorane: location of the hydrogen atoms and analysis of the intermolecular interactions
Betz, Richard; Gerber, Thomas; Hosten, Eric; Schalekamp, Henk; Acta Crystallographica Section E 67 (2011) o1028–o1029; doi:10.1107/S1600536811011500

data_2229995
_publ_section_title
;
 Redetermined structure of diphenylphosphonimidotriphenylphosphorane:
 location of the hydrogen atoms and analysis of the intermolecular
 interactions
;
_journal_coeditor_code           HB5826
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1028
_journal_page_last               o1029
_journal_paper_doi               10.1107/S1600536811011500
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C30 H25 N O P2'
_chemical_formula_moiety         'C30 H25 N O P2'
_chemical_formula_sum            'C30 H25 N O P2'
_chemical_formula_weight         477.45
_chemical_melting_point_gt       442
_chemical_melting_point_lt       445
_chemical_name_common
;
Diphenylphosphonimidotriphenylphosphorane
;
_chemical_name_systematic
;
Diphenylphosphonimidotriphenylphosphorane
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.6607(12)
_cell_length_b                   15.1593(10)
_cell_length_c                   8.9192(6)
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.67
_cell_volume                     2387.9(3)
_computing_cell_refinement       'SAINT (Bruker, 2010)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2010)'
_computing_molecular_graphics
'ORTEPIII (Farrugia, 1997) and MERCURY (Macrae et al., 2006)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_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  0.0209
_diffrn_reflns_av_sigmaI/netI    0.0149
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            12511
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    0.206
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.88
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.254
_refine_ls_abs_structure_details 'Flack (1983), 1332 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.03(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         4498
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0452P)^2^+0.5077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0763
_reflns_number_gt                4348
_reflns_number_total             4498
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb5826.cif
_cod_data_source_block           I
_cod_database_code               2229995
_cod_database_fobs_code          2229995