Neutral Mononuclear, Dinuclear, Tetranuclear d7/d10 Metal Complexes Containing bis-Pyrazole/Pyridine Ligands Supported by 2,6-bis(3-Pyrazolyl)Pyridine: Synthesis, Structure, Spectra, and Catalytic Activity
Lijuan Wan; Caishun Zhang; Yongheng Xing; Zhen Li; Na Xing; Liying Wan; Hui Shan; Inorganic Chemistry 51 (2012) 6517–6528; doi:10.1021/ic202678s

data_4329421
_publ_section_title
;
 Neutral Mononuclear, Dinuclear, Tetranuclear d7/d10 Metal Complexes
 Containing bis-Pyrazole/Pyridine Ligands Supported by
 2,6-bis(3-Pyrazolyl)Pyridine: Synthesis, Structure, Spectra, and
 Catalytic Activity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6517
_journal_page_last               6528
_journal_paper_doi               10.1021/ic202678s
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C98 H90 Co4 N22 O16 S2'
_chemical_formula_weight         2131.76
_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                74.7940(10)
_cell_angle_beta                 66.3760(10)
_cell_angle_gamma                67.9580(10)
_cell_formula_units_Z            2
_cell_length_a                   16.6277(11)
_cell_length_b                   17.5615(12)
_cell_length_c                   20.0031(13)
_cell_measurement_reflns_used    1498
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.12
_cell_volume                     4917.1(6)
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0720
_diffrn_reflns_av_sigmaI/netI    0.1492
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28524
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.12
_exptl_absorpt_coefficient_mu    0.783
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            deepred
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_description       block
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.469
_exptl_crystal_size_mid          0.241
_exptl_crystal_size_min          0.069
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1279
_refine_ls_number_reflns         17304
_refine_ls_number_restraints     170
_refine_ls_restrained_S_all      1.412
_refine_ls_R_factor_all          0.1874
_refine_ls_R_factor_gt           0.0861
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1442P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2431
_refine_ls_wR_factor_ref         0.2893
_reflns_number_gt                7439
_reflns_number_total             17304
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202678s_1-5_2.cif
_cod_data_source_block           2
_cod_database_code               4329421