Hydrogen-Atom Abstraction from Ni(I) Phosphido and Amido Complexes Gives Phosphinidene and Imide Ligands
Vlad M. Iluc; Gregory L. Hillhouse; Journal of the American Chemical Society 132 (2010) 15148–15150; doi:10.1021/ja107115q

data_4103415
_publ_section_title
;
 Hydrogen-Atom Abstraction from Ni(I) Phosphido and Amido Complexes Gives
 Phosphinidene and Imide Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15148
_journal_page_last               15150
_journal_paper_doi               10.1021/ja107115q
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C42 H65 N Ni P2'
_chemical_formula_weight         704.60
_chemical_name_systematic
;

 

 ?

 

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.214(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.803(2)
_cell_length_b                   20.155(4)
_cell_length_c                   18.138(4)
_cell_measurement_reflns_used    59
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.1
_cell_measurement_theta_min      2.18
_cell_volume                     3943.1(14)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_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  0.0700
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25060
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.21
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    0.602
_exptl_absorpt_correction_T_max  0.3084
_exptl_absorpt_correction_T_min  0.1938
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.080
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         9265
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0554P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1080
_reflns_number_gt                7908
_reflns_number_total             9265
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja107115q_si_002_2.cif
_cod_data_source_block           vlad816m
_cod_original_cell_volume        3942.9(14)
_cod_database_code               4103415