A Magneto-Structural Study of a Hexanuclear (VIV=O)6-Complex and a Tetranuclear Mixed-Valent [VIII2VIV2] Species
Biplab Biswas; Thomas Weyhermüller; Eckhard Bill; Phalguni Chaudhuri; Inorganic Chemistry 48 (2009) 1524–1532; doi:10.1021/ic8018327

data_4301459
_publ_section_title
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A Magneto-Structural Study of a Hexanuclear (VIV=O)6-Complex and a
Tetranuclear Mixed-Valent [VIII2VIV2] Species
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1524
_journal_page_last               1532
_journal_paper_doi               10.1021/ic8018327
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         '[C30 H66 N6 Na O18 V6]+, (Cl O4)-, 2 (C H4 O)'
_chemical_formula_sum            'C32 H74 Cl N6 Na O24 V6'
_chemical_formula_weight         1291.05
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 91.623(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.5049(12)
_cell_length_b                   23.205(2)
_cell_length_c                   33.414(3)
_cell_measurement_temperature    100(2)
_cell_volume                     10467.1(16)
_computing_cell_refinement       'Bruker AXS Collect Software'
_computing_data_collection       'Bruker AXS Collect Software'
_computing_data_reduction        'Bruker AXS Collect Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
'1685 images at 0.4 deg. stepwise rotation in omega and phi, 32 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode, 50 kV, 80 mA'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0972
_diffrn_reflns_av_sigmaI/netI    0.1120
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            39291
_diffrn_reflns_theta_full        23.50
_diffrn_reflns_theta_max         23.50
_diffrn_reflns_theta_min         6.59
_exptl_absorpt_coefficient_mu    1.170
_exptl_absorpt_correction_T_max  0.9770
_exptl_absorpt_correction_T_min  0.8821
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent parallelepiped'
_exptl_crystal_F_000             5328
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.51(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1282
_refine_ls_number_reflns         14982
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0771
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1220P)^2^+15.4925P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1869
_refine_ls_wR_factor_ref         0.2032
_reflns_number_gt                11815
_reflns_number_total             14982
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8018327_si_001_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Gaussian' changed to 'gaussian'
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      'C c'
_cod_database_code               4301459