Synthesis and Characterization of Nickel Inverse 9-Metallacrown-3, Palladium-Silver, and Dinuclear Platinum Complexes Containing Pyrazole-Functionalized NHC Ligands
Chao Chen; Huayu Qiu; Wanzhi Chen; Inorganic Chemistry 50 (2011) 8671–8678; doi:10.1021/ic2012233

data_4326194
_publ_section_title
;
 Synthesis and Characterization of Nickel Inverse 9-Metallacrown-3,
 Palladium-Silver, and Dinuclear Platinum Complexes Containing
 Pyrazole-Functionalized NHC Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8671
_journal_page_last               8678
_journal_paper_doi               10.1021/ic2012233
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C72 H82 F12 N18 Ni3 P2'
_chemical_formula_weight         1665.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                117.780(2)
_cell_angle_beta                 92.2230(10)
_cell_angle_gamma                108.868(2)
_cell_formula_units_Z            2
_cell_length_a                   13.2851(14)
_cell_length_b                   19.085(2)
_cell_length_c                   19.144(2)
_cell_measurement_reflns_used    5336
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.199
_cell_measurement_theta_min      2.206
_cell_volume                     3958.2(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0627
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20735
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_T_max  0.7605
_exptl_absorpt_correction_T_min  0.7278
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             1724
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.128
_refine_diff_density_min         -1.084
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     964
_refine_ls_number_reflns         13765
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.0638
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1127P)^2^+6.6472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1727
_refine_ls_wR_factor_ref         0.2238
_reflns_number_gt                8377
_reflns_number_total             13765
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2012233_si_002_4.cif
_cod_data_source_block           4
_cod_database_code               4326194