Sequential Insertion Reactions of Carbon Monoxide and Ethylene into the Ni−C Bond of a Cationic Nickel(II) Alkyl Complex
Curley, John J.; Kitiachvili, Kristina D.; Waterman, Rory; Hillhouse, Gregory L.; Organometallics 28 (2009) 2568–; doi:10.1021/om900023y

data_4069097
_publ_section_title
;
 Sequential Insertion Reactions of Carbon Monoxide and Ethylene into the
 Ni&#x2212;C Bond of a Cationic Nickel(II) Alkyl Complex
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2568
_journal_paper_doi               10.1021/om900023y
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C56 H120 F12 Ni2 O3 P6'
_chemical_formula_weight         1372.76
_chemical_name_common            '[(dtbpe)Ni(CH2CH2C{O}CH2(C(CH3)3))][PF6]'
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 92.7520(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9208(10)
_cell_length_b                   37.697(2)
_cell_length_c                   12.2582(8)
_cell_measurement_temperature    100(2)
_cell_volume                     6886.9(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.949
_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  0.0550
_diffrn_reflns_av_sigmaI/netI    0.1340
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            42380
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_T_max  0.0092
_exptl_absorpt_correction_T_min  0.0074
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'semi-empirical based on psi scans'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2936
_exptl_crystal_size_max          0.35000
_exptl_crystal_size_mid          0.27000
_exptl_crystal_size_min          0.10000
_refine_diff_density_max         1.549
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.859
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         16282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.859
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1167
_reflns_number_gt                8837
_reflns_number_total             16282
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900023y_si_002.cif
_cod_data_source_block           metallacycle
_cod_original_cell_volume        6887.0(8)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4069097