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_7050904
_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            'C60 H62 F24 N24 Ni4 O P4 S4'
_chemical_formula_weight         2078.30
_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                 100.376(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.563(6)
_cell_length_b                   40.993(16)
_cell_length_c                   15.378(6)
_cell_measurement_reflns_used    3278
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.36
_cell_measurement_theta_min      2.32
_cell_volume                     9030(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  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1307
_diffrn_reflns_av_sigmaI/netI    0.3124
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            37088
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    1.086
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.6108
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4200
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1291
_refine_ls_number_reflns         11779
_refine_ls_number_restraints     579
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1842
_refine_ls_R_factor_gt           0.0775
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
[0.00000+1.00000exp(5.00(sin\q/\l)^2^)]/
[\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0000P)^2^+0.0000sin\q/\l]
where P = 0.33333Fo^2^ + 0.66667Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1572
_reflns_number_gt                3569
_reflns_number_total             11779
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b203819f.txt
_cod_data_source_block           complex_1
_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      'P2(1)/n  '
_cod_database_code               7050904