Synthesis and structural characterization of metal complexes with macrocyclic tetracarbene ligands
Fei, Fan; Lu, Taotao; Chen, Xue-tai; Xue, Ziling Ben; New J. Chem. 41 (2017) 13442–13453; doi:10.1039/C7NJ02485A

data_7056645
_publ_section_title
;
 Synthesis and structural characterization of metal complexes with
 macrocyclic tetracarbene ligands
;
_journal_issue                   22
_journal_name_full               'New J. Chem.'
_journal_page_first              13442
_journal_page_last               13453
_journal_paper_doi               10.1039/C7NJ02485A
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C42 H44 N8 Pd, 2(F6 P)'
_chemical_formula_sum            'C42 H44 F12 N8 P2 Pd'
_chemical_formula_weight         1057.19
_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-2014/7
_audit_update_record
;
2017-09-05 deposited with the CCDC.
2017-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90.046(4)
_cell_angle_beta                 96.534(4)
_cell_angle_gamma                102.324(4)
_cell_formula_units_Z            2
_cell_length_a                   11.4236(19)
_cell_length_b                   13.822(2)
_cell_length_c                   15.218(2)
_cell_measurement_reflns_used    2965
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.63
_cell_measurement_theta_min      2.40
_cell_volume                     2331.5(6)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_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, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'PHOTON 100 CMOS detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1429
_diffrn_reflns_av_unetI/netI     0.2607
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19191
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.515
_diffrn_reflns_theta_min         2.049
_diffrn_source                   'microfocus rotating (TXS)'
_exptl_absorpt_coefficient_mu    0.555
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.751
_refine_diff_density_min         -1.161
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         10610
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.2014
_refine_ls_R_factor_gt           0.1164
_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^)+(0.0846P)^2^+3.9950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2096
_refine_ls_wR_factor_ref         0.2419
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5843
_reflns_number_total             10610
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj02485a2.cif
_cod_data_source_block           10
_cod_database_code               7056645
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.912
_shelx_estimated_absorpt_t_max   0.936
_shelx_res_checksum              42821
_shelx_fab_checksum              45849