Self-assembly of a novel mixed-valence tetranuclear molecular square [FeII3FeIIIL2(HL)2]3+ and [M(HL)]44+ squares (M=Ni, Zn and Cd){H2L=bis(2-acetylpyridine) thiocarbazone}
Han Gang; Guo Dong; Duan Chun-Ying; Mo Hong; Meng Qing-jin; New J. Chem. 26 (2002) 1371–1377; doi:10.1039/b203819f

data_7050906
_publ_section_title
;
 Self-assembly of a novel mixed-valence tetranuclear molecular square
 [FeII3FeIIIL2(HL)2]3+ and [M(HL)]44+ squares (M=Ni, Zn and
 Cd){H2L=bis(2-acetylpyridine) thiocarbazone}
;
_journal_issue                   10
_journal_name_full               'New J. Chem.'
_journal_page_first              1371
_journal_page_last               1377
_journal_paper_doi               10.1039/b203819f
_journal_volume                  26
_journal_year                    2002
_chemical_formula_sum            'C69 H69 Cl12 Fe7 N24 O S4'
_chemical_formula_weight         2195.09
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 102.6440(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.6186(17)
_cell_length_b                   20.4906(11)
_cell_length_c                   29.7552(17)
_cell_measurement_reflns_used    5576
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.77
_cell_measurement_theta_min      2.38
_cell_volume                     18810.4(18)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0679
_diffrn_reflns_av_sigmaI/netI    0.0915
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            38734
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    1.532
_exptl_absorpt_correction_T_max  0.6922
_exptl_absorpt_correction_T_min  0.8311
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            dark-black
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8872
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.118
_refine_diff_density_min         -0.833
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.918
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1067
_refine_ls_number_reflns         12282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.918
_refine_ls_R_factor_all          0.1156
_refine_ls_R_factor_gt           0.0679
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1150P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1769
_refine_ls_wR_factor_ref         0.1945
_reflns_number_gt                6894
_reflns_number_total             12282
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b203819f.txt
_cod_data_source_block           complex_4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'C2/c  '
_cod_database_code               7050906