Nickel(II) Complexes Containing Bidentate Amido Phosphine Ligands Derived from α-Iminophosphorus Ylides: Synthesis and Structural Characterization
Pei-Ying Lee; Lan-Chang Liang; Inorganic Chemistry 47 (2008) 749–758; doi:10.1021/ic701836j

data_4304351
_publ_section_title
;
Nickel(II) Complexes Containing Bidentate Amido Phosphine Ligands Derived
from \a-Iminophosphorus Ylides: Synthesis and Structural Characterization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              749
_journal_page_last               758
_journal_paper_doi               10.1021/ic701836j
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C50 H60 Br2 N2 O P2'
_chemical_formula_weight         926.76
_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                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.127(4)
_cell_length_b                   13.562(3)
_cell_length_c                   37.528(7)
_cell_measurement_temperature    293(2)
_cell_volume                     9735(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0721
_diffrn_reflns_av_sigmaI/netI    0.0695
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            53108
_diffrn_reflns_theta_full        26.07
_diffrn_reflns_theta_max         26.07
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    1.767
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3856
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.980
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.872
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         9585
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.872
_refine_ls_R_factor_all          0.1220
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          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^)+(0.0936P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1438
_refine_ls_wR_factor_ref         0.1676
_reflns_number_gt                4361
_reflns_number_total             9585
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701836j-file003_3.cif
_cod_data_source_block           h1
_cod_database_code               4304351