Noninnocent Behavior of Ancillary Ligands: Apparent Trans Coupling of a Saturated N-Heterocyclic Carbene Unit with an Ethyl Ligand Mediated by Nickel
Tobias Steinke; Bryan K. Shaw; Howard Jong; Brian O. Patrick; Michael D. Fryzuk; Jennifer C. Green; Journal of the American Chemical Society 131 (2009) 10461–10466; doi:10.1021/ja901346g

data_4104748
_publ_section_title
;
 Noninnocent Behavior of Ancillary Ligands: Apparent Trans Coupling of a
 Saturated N-Heterocyclic Carbene Unit with an Ethyl Ligand Mediated by
 Nickel
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10461
_journal_page_last               10466
_journal_paper_doi               10.1021/ja901346g
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C29 H45 F6 N2 Ni P3'
_chemical_formula_weight         687.29
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 101.810(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   40.4970(10)
_cell_length_b                   17.8762(6)
_cell_length_c                   18.4624(7)
_cell_measurement_reflns_used    6162
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.98
_cell_measurement_theta_min      2.48
_cell_volume                     13082.6(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker X8 APEX'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_sigmaI/netI    0.0512
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            65454
_diffrn_reflns_theta_full        27.93
_diffrn_reflns_theta_max         27.93
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.796
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_correction_T_min  0.570
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_description       irregular
_exptl_crystal_F_000             5760
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         15616
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+22.3598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.1050
_reflns_number_gt                10858
_reflns_number_total             15616
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja901346g_si_002.cif
_cod_data_source_block           mf673
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4104748