Synthesis, structural characterization and NMR studies of group 10 metal complexes with macrocyclic amine N-heterocyclic carbene ligands.
Lu, Taotao; Liu, Zhiming; Steren, Carlos A.; Fei, Fan; Cook, Tabitha M.; Chen, Xue-Tai; Xue, Zi-Ling; Dalton transactions (Cambridge, England : 2003) 47 (2018) 4282–4292; doi:10.1039/c7dt04666a

data_7045569
_publ_section_title
;
 Synthesis, structural characterization and NMR studies of group 10 metal
 complexes with macrocyclic amine N-heterocyclic carbene ligands.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4282
_journal_page_last               4292
_journal_paper_doi               10.1039/c7dt04666a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C22 H26 N6 Ni, 2(F6 P)'
_chemical_formula_sum            'C22 H26 F12 N6 Ni P2'
_chemical_formula_weight         723.14
_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   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-01-19 deposited with the CCDC.
2018-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                87.532(5)
_cell_angle_beta                 64.664(4)
_cell_angle_gamma                74.006(5)
_cell_formula_units_Z            1
_cell_length_a                   8.8606(18)
_cell_length_b                   8.999(2)
_cell_length_c                   9.611(2)
_cell_measurement_reflns_used    3042
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.58
_cell_measurement_theta_min      2.35
_cell_volume                     663.3(2)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_unetI/netI     0.1445
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5223
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.584
_diffrn_reflns_theta_min         2.353
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.964
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_description       block
_exptl_crystal_F_000             366
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.040
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3042
_refine_ls_number_restraints     155
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1503
_refine_ls_R_factor_gt           0.0916
_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^)+(0.0613P)^2^+2.7219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1660
_refine_ls_wR_factor_ref         0.1870
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1904
_reflns_number_total             3042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04666a2.cif
_cod_data_source_block           4a
_cod_depositor_comments
'Adding full bibliography for 7045565--7045570.cif.'
_cod_database_code               7045569
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.761
_shelx_estimated_absorpt_t_max   0.910
_shelx_res_checksum              29720