β-Oxo-δ-diimine Nickel Complexes: A Comparison of Tautomeric Active Species in Ethylene Polymerization Catalysis
Chiu, Hsin-Chun; Pearce, Adam J.; Dunn, Peter L.; Cramer, Christopher J.; Tonks, Ian A.; Organometallics 35 (2016) 2076–; doi:10.1021/acs.organomet.6b00256

data_4086533
_publ_section_title
;
 \b-Oxo-\d-diimine Nickel Complexes: A Comparison of Tautomeric Active
 Species in Ethylene Polymerization Catalysis
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2076
_journal_paper_doi               10.1021/acs.organomet.6b00256
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C86 H108 K2 N4 Ni2 O2, C7 H8'
_chemical_formula_sum            'C50 H62 K N3 Ni O'
_chemical_formula_weight         818.83
_chemical_name_common            LNiK
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 102.4000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.0019(5)
_cell_length_b                   13.3076(3)
_cell_length_c                   29.0717(6)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      74.44
_cell_measurement_theta_min      3.11
_cell_volume                     9069.1(3)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker SMART Platform CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            43651
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.580
_diffrn_reflns_theta_min         3.113
_diffrn_source                   normal
_exptl_absorpt_coefficient_mu    1.722
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.6189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_description       Block
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.269
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         9058
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0562
_refine_ls_shift/su_max          0.056
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0687P)^2^+28.3163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1452
_refine_ls_wR_factor_ref         0.1533
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7675
_reflns_number_total             9058
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00256_si_003.cif
_cod_data_source_block           15227_0m
_cod_depositor_comments
'Adding full bibliography for 4086532--4086539.cif.'
_cod_database_code               4086533
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.6189
_shelx_estimated_absorpt_t_max   0.7538
_shelx_res_checksum              29405
_shelx_hkl_checksum              85436