Synthesis, Structure, and Reactions of a Three-Coordinate Nickel-Carbene Complex, {1,2-Bis(di-tert-butylphosphino)ethane}NiCPh2
Daniel J. Mindiola; Gregory L. Hillhouse; Journal of the American Chemical Society 124 (2002) 9976–9977; doi:10.1021/ja0269183

data_4115073
_publ_section_title
;
 Synthesis, Structure, and Reactions of a Three-Coordinate Nickel-Carbene
 Complex, {1,2-Bis(di-tert-butylphosphino)ethane}NiCPh2
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9976
_journal_page_last               9977
_journal_paper_doi               10.1021/ja0269183
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C22 H46 N2 Ni O2 P2'
_chemical_formula_weight         491.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            18
_cell_length_a                   26.4905(12)
_cell_length_b                   26.4905(12)
_cell_length_c                   20.5306(13)
_cell_measurement_reflns_used    3405
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.99
_cell_measurement_theta_min      1.33
_cell_volume                     12477.1(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      373(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0733
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16290
_diffrn_reflns_theta_full        21.99
_diffrn_reflns_theta_max         21.99
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    0.833
_exptl_absorpt_correction_T_max  0.9517
_exptl_absorpt_correction_T_min  0.8511
_exptl_absorpt_correction_type   'semi-empirical from psi scans '
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_density_meas      1.177
_exptl_crystal_F_000             4788
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.143
_refine_diff_density_min         -1.295
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       0.00015(5)
_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   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3405
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0914
_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^)+(0.0926P)^2^+327.8298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2178
_refine_ls_wR_factor_ref         0.2219
_reflns_number_gt                3085
_reflns_number_total             3405
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0269183_s2_2.cif
_cod_data_source_block           danm50m
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4115073