Nickel(II) Complexes of Highly σ-Donating Cyclic (Alkyl)(Amino)- and Malonate-Carbenes: Syntheses and Catalytic Studies
Henrion, Mickaël; de P. Cardoso, Bernardo; César, Vincent; Chetcuti, Michael J.; Ritleng, Vincent; Organometallics 36 (2017) 1113–; doi:10.1021/acs.organomet.6b00906

data_4087192
_publ_section_title
;
 Nickel(II) Complexes of Highly \s-Donating Cyclic (Alkyl)(Amino)- and
 Malonate-Carbenes: Syntheses and Catalytic Studies
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1113
_journal_paper_doi               10.1021/acs.organomet.6b00906
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C33 H38 N4 Ni O2'
_chemical_formula_sum            'C33 H38 N4 Ni O2'
_chemical_formula_weight         581.38
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.6645(11)
_cell_length_b                   16.9683(11)
_cell_length_c                   20.0404(14)
_cell_measurement_reflns_used    5311
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.79
_cell_measurement_theta_min      2.37
_cell_volume                     5666.8(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_unetI/netI     0.0612
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            36320
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         1.992
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.722
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_description       plate
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6837
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+0.7997P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.1006
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4237
_reflns_number_total             6837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00906_si_002.cif
_cod_data_source_block           mcbc161006
_cod_database_code               4087192
_shelx_estimated_absorpt_t_min   0.786
_shelx_estimated_absorpt_t_max   0.918
_shelxl_version_number           2013-4
_shelx_res_checksum              84575
_shelx_hkl_checksum              9903