1,1'-(Diselanediylbis{[<i>P</i>,<i>P</i>-diphenyl-<i>N</i>-(trimethylsilyl)phosphorimidoyl]methanylylidene})bis[1,1-diphenyl-<i>N</i>-(trimethylsilyl)-λ^5^-phosphanamine] pentane disolvate
Thirumoorthi, Ramalingam; Chivers, Tristram; Laitinen, Risto S.; Acta Crystallographica Section E 70 (2014) o20–o21; doi:10.1107/S1600536813032674

data_2239116
_publ_section_title
;
 1,1'-(Diselanediylbis{[<i>P</i>,<i>P</i>-diphenyl-<i>N</i>-(trimethylsilyl)phosphorimidoyl]methanylylidene})bis[1,1-diphenyl-<i>N</i>-(trimethylsilyl)-\l^5^-phosphanamine]
 pentane disolvate
;
_journal_coeditor_code           SU2665
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o20
_journal_page_last               o21
_journal_paper_doi               10.1107/S1600536813032674
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C62 H78 N4 P4 Se2 Si4, 2C5 H12'
_chemical_formula_moiety         'C62 H78 N4 P4 Se2 Si4, 2(C5 H12)'
_chemical_formula_sum            'C72 H102 N4 P4 Se2 Si4'
_chemical_formula_weight         1417.74
_chemical_name_systematic
'1,1'-(Diselanediylbis{[<i>P</i>,<i>P</i>-diphenyl-<i>N</i>-(trimethylsilyl)phosphorimidoyl]methanylylidene})bis[1,1-diphenyl-<i>N</i>-(trimethylsilyl)-\l^5^-phosphanamine] pentane disolvate'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                65.6110(10)
_cell_angle_beta                 85.5250(10)
_cell_angle_gamma                76.730(2)
_cell_formula_units_Z            1
_cell_length_a                   10.2500(3)
_cell_length_b                   13.4420(3)
_cell_length_c                   14.6670(4)
_cell_measurement_reflns_used    6257
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.70
_cell_volume                     1791.03(8)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'DIAMOND (Putz & Brandenburg, 2013)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius KappaCCD FR540C'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11811
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    1.232
_exptl_absorpt_correction_T_max  0.8972
_exptl_absorpt_correction_T_min  0.7732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             746
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
The Platon SQUEEZE procedure (Spek, 2003, 2009) was applied to recover
85 electrons per unit cell in one void (total volume 249.4 \%A^3^);
that is 85 electrons per formula unit. Lattice solvent pentane
molecules (42 electrons/pentane) were present, and the electrons
recovered by SQUEEZE have been assigned as 2 pentane molecules per
formula unit. These pentane molecules have been included in the
formula for the calculation of crystal properties.
;
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.713
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         6257
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0683
_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^)+(0.0591P)^2^+10.1653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1573
_refine_ls_wR_factor_ref         0.1695
_reflns_number_gt                4902
_reflns_number_total             6257
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            su2665sup1.cf
_cod_data_source_block           I
_cod_database_code               2239116
_cod_database_fobs_code          2239116