Metallated triphenylphosphinimine complexes
Wei, Pingrong; Chan, Katie T. K.; Stephan, Douglas W.; Dalton Transactions  (2003) 3804–; doi:10.1039/b305877h

data_7013262
_publ_section_title
;
 Metallated triphenylphosphinimine complexes
;
_journal_issue                   19
_journal_name_full               'Dalton Transactions'
_journal_page_first              3804
_journal_paper_doi               10.1039/b305877h
_journal_year                    2003
_chemical_formula_sum            'C83 H71 Br N Ni1.5 P4'
_chemical_formula_weight         1374.26
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/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                 90.364(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.719(10)
_cell_length_b                   13.700(8)
_cell_length_c                   35.49(2)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     7643(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0618
_diffrn_reflns_av_sigmaI/netI    0.1212
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            31772
_diffrn_reflns_theta_full        23.22
_diffrn_reflns_theta_max         23.22
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    1.021
_exptl_absorpt_correction_T_max  0.256595
_exptl_absorpt_correction_T_min  0.176673
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2852
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.818
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     801
_refine_ls_number_reflns         10835
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.818
_refine_ls_R_factor_all          0.1126
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1215
_reflns_number_gt                5538
_reflns_number_total             10835
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b305877h.txt
_cod_data_source_block
'[(Ph3P)3NiBr].0.5[Ni(o-C6H4PPh2N3,5-C6H3Me2)2].0.5C6H6'
_cod_original_sg_symbol_H-M      P2/c
_cod_original_formula_sum        'C83 H71 Br N Ni1.50 P4'
_cod_database_code               7013262