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_4326192
_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            'C55 H64 F12 N14 Ni3 O P2'
_chemical_formula_weight         1403.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.5530(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.6917(18)
_cell_length_b                   15.6090(15)
_cell_length_c                   22.973(2)
_cell_measurement_temperature    298(2)
_cell_volume                     6542.4(11)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0869
_diffrn_reflns_av_sigmaI/netI    0.1223
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            32538
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.986
_exptl_absorpt_correction_T_max  0.7118
_exptl_absorpt_correction_T_min  0.6765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       block
_exptl_crystal_F_000             2888
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.37
_refine_diff_density_max         3.452
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     868
_refine_ls_number_reflns         11532
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.2275
_refine_ls_R_factor_gt           0.1214
_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^)+(0.1719P)^2^+90.7385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3083
_refine_ls_wR_factor_ref         0.4136
_reflns_number_gt                5371
_reflns_number_total             11532
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2012233_si_002_2.cif
_cod_data_source_block           2
_cod_database_code               4326192