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_4087191
_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         'C23 H36 N, C18 H15 Cl3 Ni P'
_chemical_formula_sum            'C41 H51 Cl3 N Ni P'
_chemical_formula_weight         753.85
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                87.564(2)
_cell_angle_beta                 75.702(2)
_cell_angle_gamma                77.918(2)
_cell_formula_units_Z            2
_cell_length_a                   11.7585(10)
_cell_length_b                   12.4165(10)
_cell_length_c                   15.0414(12)
_cell_measurement_reflns_used    9883
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.93
_cell_measurement_theta_min      2.38
_cell_volume                     2080.8(3)
_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-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  triumph
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34754
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.077
_diffrn_reflns_theta_min         1.397
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.724
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6337
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_description       prism
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.200
_platon_squeeze_details
;
The residual electron density was assigned to half a molecule of 
the dichloromethane solvent [41/2= 21 e per asymmetric unit; half
a molecule of C1H2Cl2 would give 21 e]. 
;
_refine_diff_density_max         0.987
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         12191
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+0.2575P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1191
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9138
_reflns_number_total             12191
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00906_si_002.cif
_cod_data_source_block           mcmh140424
_cod_database_code               4087191
_shelx_estimated_absorpt_t_min   0.812
_shelx_estimated_absorpt_t_max   0.869
_shelxl_version_number           2013-4
_shelx_res_checksum              33855
_shelx_hkl_checksum              4402