1,2,4,5-Tetramethyl-3,6-diphenyl-1,2,4,5-tetraaza-3,6-diphosphinane
Kriel, Frederik H.; Caddy, Judy; Fernandes, Manuel A.; Acta Crystallographica Section E 64 (2008) o708–; doi:10.1107/S160053680800665X

data_2218018
_publ_section_title
;
 1,2,4,5-Tetramethyl-3,6-diphenyl-1,2,4,5-tetraaza-3,6-diphosphinane
;
_journal_coeditor_code           TK2250
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o708
_journal_paper_doi               10.1107/S160053680800665X
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C16 H22 N4 P2'
_chemical_formula_moiety         'C16 H22 N4 P2'
_chemical_formula_sum            'C16 H22 N4 P2'
_chemical_formula_weight         332.32
_chemical_name_common
;
Bis(phenylphosphino)cyclo-tetramethyldihydrazine
;
_chemical_name_systematic
;
1,2,4,5-Tetramethyl-3,6-diphenyl-1,2,4,5-tetraaza-3,6-diphosphinane
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2879(16)
_cell_length_b                   7.5426(9)
_cell_length_c                   17.125(2)
_cell_measurement_reflns_used    899
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.2
_cell_measurement_theta_min      3.0
_cell_volume                     1716.4(4)
_computing_cell_refinement       'SAINT-Plus (Bruker, 1999)'
_computing_data_collection       'SMART-NT (Bruker, 1998)'
_computing_data_reduction        'SAINT-Plus (Bruker, 1999)'
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, 1997) and Mercury (Macrae <i>et al.</i>,
2006)
;
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_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  0.031
_diffrn_reflns_av_sigmaI/netI    0.020
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10040
_diffrn_reflns_theta_full        27.0
_diffrn_reflns_theta_max         27.0
_diffrn_reflns_theta_min         2.4
_exptl_absorpt_coefficient_mu    0.255
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.32
_refine_diff_density_min         -0.25
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.08
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.08
_refine_ls_R_factor_all          0.037
_refine_ls_R_factor_gt           0.030
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+0.5379P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.089
_refine_ls_wR_factor_ref         0.094
_reflns_number_gt                1591
_reflns_number_total             1873
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk2250.cif
_cod_data_source_block           I
_cod_database_code               2218018
_cod_database_fobs_code          2218018