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_4301460
_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
;
_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
'(C72 H92 Cl10 N4 O4 V4), (C6 H8 N2), 5.5 (C4 H10 O)'
_chemical_formula_sum            'C100 H155 Cl10 N6 O9.5 V4'
_chemical_formula_weight         2151.56
_chemical_name_systematic
; 
 ? 
;
_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                113.412(3)
_cell_angle_beta                 96.194(2)
_cell_angle_gamma                103.904(3)
_cell_formula_units_Z            2
_cell_length_a                   15.0798(9)
_cell_length_b                   20.4731(13)
_cell_length_c                   22.2124(14)
_cell_measurement_temperature    100(2)
_cell_volume                     5947.3(7)
_computing_cell_refinement       'Bruker SAINT 7.34A'
_computing_data_collection       'Bruker SAINT 7.34A'
_computing_data_reduction        'Bruker SAINT 7.34A'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX2'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source
'rotating anode, 50 kV, 40 mA, Multi-Layer Optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1654
_diffrn_reflns_av_sigmaI/netI    0.1282
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            97715
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    0.580
_exptl_absorpt_correction_T_max  0.9348
_exptl_absorpt_correction_T_min  0.8552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2007/4'
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2270
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.363
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1245
_refine_ls_number_reflns         20900
_refine_ls_number_restraints     226
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1307
_refine_ls_R_factor_gt           0.0693
_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^)+(0.1062P)^2^+3.4534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1719
_refine_ls_wR_factor_ref         0.2101
_reflns_number_gt                12421
_reflns_number_total             20900
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8018327_si_001_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' 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_cell_volume        5947.3(6)
_cod_original_formula_sum        'C100 H155 Cl10 N6 O9.50 V4'
_cod_database_code               4301460