Phosphorus and Olefin Substituent Effects on the Insertion Chemistry of Nickel(II) Hydride Complexes Containing Amido Diphosphine Ligands
Liang, Lan-Chang; Chien, Pin-Shu; Lee, Pei-Ying; Organometallics 27 (2008) 3082–; doi:10.1021/om701294a

data_4071143
_publ_section_title
;
 Phosphorus and Olefin Substituent Effects on the Insertion Chemistry of
 Nickel(II) Hydride Complexes Containing Amido Diphosphine Ligands
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3082
_journal_paper_doi               10.1021/om701294a
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C36 H53 N Ni P2'
_chemical_formula_sum            'C36 H53 N Ni P2'
_chemical_formula_weight         620.44
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.5360(10)
_cell_angle_beta                 99.2740(10)
_cell_angle_gamma                106.409(2)
_cell_formula_units_Z            4
_cell_length_a                   14.2470(4)
_cell_length_b                   16.2118(4)
_cell_length_c                   18.4856(6)
_cell_measurement_reflns_used    111886
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.037
_cell_volume                     3838.8(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 19'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.1104
_diffrn_reflns_av_sigmaI/netI    0.1066
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            46192
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.610
_exptl_absorpt_correction_T_max  0.9
_exptl_absorpt_correction_T_min  0.7724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.074
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.2
_platon_squeeze_details          ' ?'
_refine_diff_density_max         1.966
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.175
_refine_ls_extinction_coef       0.0142(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.850
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         13428
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.850
_refine_ls_R_factor_all          0.1305
_refine_ls_R_factor_gt           0.0814
_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^)+(0.1683P)^2^+4.1689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2152
_refine_ls_wR_factor_ref         0.2467
_reflns_number_gt                7837
_reflns_number_total             13428
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om701294a-file003.cif
_cod_data_source_block           2c
_cod_original_cell_volume        3838.80(19)
_cod_database_code               4071143