Syntheses, Structures, and Magnetic Properties of Heterobimetallic Clusters with Tricyanometalate and π-Conjugated Ligands Containing 1,3-Dithiol-2-ylidene
Yan-Hong Peng; Yi-Fei Meng; Liang Hu; Quan-Xiu Li; Yi-Zhi Li; Jing-Lin Zuo; Xiao-Zeng You; Inorganic Chemistry 49 (2010) 1905–1912; doi:10.1021/ic9023713

data_4314917
_publ_section_title
;
 Syntheses, Structures, and Magnetic Properties of Heterobimetallic
 Clusters with Tricyanometalate and \p-Conjugated Ligands Containing
 1,3-Dithiol-2-ylidene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1905
_journal_page_last               1912
_journal_paper_doi               10.1021/ic9023713
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C112 H80 B2 Cl2 Fe2 N34 Ni2 O14 S16'
_chemical_formula_weight         2960.70
_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                99.914(2)
_cell_angle_beta                 91.470(3)
_cell_angle_gamma                101.981(2)
_cell_formula_units_Z            1
_cell_length_a                   14.668(2)
_cell_length_b                   14.929(2)
_cell_length_c                   18.808(3)
_cell_measurement_reflns_used    1855
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      24.5
_cell_measurement_theta_min      1.9
_cell_volume                     3960.6(10)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0756
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21475
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.719
_exptl_absorpt_correction_T_max  0.8579
_exptl_absorpt_correction_T_min  0.8241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             1510
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     883
_refine_ls_number_reflns         15169
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0588
_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^)+(0.0400P)^2^+1.2200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1077
_reflns_number_gt                10686
_reflns_number_total             15169
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9023713_si_002_1.cif
_cod_data_source_block           1
_cod_original_cell_volume        3960.7(10)
_cod_database_code               4314917