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_4329422
_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            'C92 H66 N20 O6 S Zn4'
_chemical_formula_weight         1841.19
_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                85.68(3)
_cell_angle_beta                 85.54(3)
_cell_angle_gamma                83.82(3)
_cell_formula_units_Z            2
_cell_length_a                   14.802(3)
_cell_length_b                   15.162(3)
_cell_length_c                   18.087(4)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      3.01
_cell_volume                     4014.2(15)
_computing_cell_refinement
;
'Rgaku R-AXIS RAPID diffractometer Control Software' 
;
_computing_data_collection
;      
'Rgaku R-AXIS RAPID diffractometer Control Software' 
;
_computing_data_reduction
;
'Rgaku R-AXIS RAPID diffractometer Control Software'
;
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  SHELXP-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       '\w 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  0.1565
_diffrn_reflns_av_sigmaI/netI    0.2058
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30894
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.278
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Higashi,T(1995)Program for Absorption Correction
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       block
_exptl_crystal_F_000             1884
_exptl_crystal_size_max          0.302
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1108
_refine_ls_number_reflns         13631
_refine_ls_number_restraints     2070
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.2164
_refine_ls_R_factor_gt           0.0950
_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^)+(0.1037P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1923
_refine_ls_wR_factor_ref         0.2369
_reflns_number_gt                6016
_reflns_number_total             13631
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202678s_1-5_3.cif
_cod_data_source_block           3
_cod_original_cell_volume        4014.3(14)
_cod_database_code               4329422