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_7045567
_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_sum            'C25 H24 F12 N6 P2 Pd'
_chemical_formula_weight         804.84
_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                99.532(2)
_cell_angle_beta                 91.502(2)
_cell_angle_gamma                104.897(2)
_cell_formula_units_Z            2
_cell_length_a                   10.9687(9)
_cell_length_b                   11.3949(9)
_cell_length_c                   12.2882(9)
_cell_measurement_reflns_used    3903
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.49
_cell_measurement_theta_min      2.29
_cell_volume                     1459.9(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 0.995
_diffrn_measured_fraction_theta_max 0.994
_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  0.0535
_diffrn_reflns_av_unetI/netI     0.0903
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13143
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.435
_diffrn_reflns_theta_min         2.290
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.852
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.831
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.873
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         6621
_refine_ls_number_restraints     2364
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_gt           0.0578
_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^)+(0.0494P)^2^+0.9658P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1231
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4649
_reflns_number_total             6621
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04666a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7045565--7045570.cif.'
_cod_database_code               7045567
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.790
_shelx_estimated_absorpt_t_max   0.897
_shelx_res_checksum              69710