Dinuclear fluoro-peroxovanadium(v) complexes with symmetric and asymmetric peroxo bridges: syntheses, structures and DFT studies
Chrappová, Jana; Schwendt, Peter; Sivák, Michal; Repiský, Michal; Malkin, Vladimir G.; Marek, Jaromír; Dalton Transactions  (2009) 465–473; doi:10.1039/b813228c

data_7000321
_publ_section_title
;
 Dinuclear fluoro-peroxovanadium(v) complexes with symmetric and
 asymmetric peroxo bridges: syntheses, structures and DFT studies
;
_journal_issue                   3
_journal_name_full               'Dalton Transactions'
_journal_page_first              465
_journal_page_last               473
_journal_paper_doi               10.1039/b813228c
_journal_year                    2009
_chemical_formula_moiety         'F O10 V2, H2 O, 3(Cs)'
_chemical_formula_sum            'Cs3 F H2 O11 V2'
_chemical_formula_weight         697.63
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.8867(7)
_cell_length_b                   12.6332(8)
_cell_length_c                   15.1797(9)
_cell_measurement_reflns_used    3399
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.4955
_cell_measurement_theta_min      2.697
_cell_volume                     2471.3(3)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction)'
_computing_molecular_graphics    'ORTEP-III (Johnson & Burnett, 1996)'
_computing_publication_material
;
SHELXL-97 (Sheldrick, 1997), PARST (Nardelli, 1995)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16.3
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Kuma KM4 + CCD'
_diffrn_measurement_method       'rotation method, \w--scan'
_diffrn_radiation_monochromator  'Enhance (Oxford Diffraction)'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10341
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.278
_exptl_absorpt_correction_T_max  0.39009
_exptl_absorpt_correction_T_min  0.07214
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'CrysAlis RED (Oxford Diffraction)'
_exptl_crystal_colour            'orange ?'
_exptl_crystal_density_diffrn    3.750
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       0.00161(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2096
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0213
_refine_ls_R_factor_gt           0.0194
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0150P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0421
_refine_ls_wR_factor_ref         0.0429
_reflns_number_gt                2010
_reflns_number_total             2096
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b813228c.txt
_cod_data_source_block           fp_2_4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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_Hall     '-P 2ac 2ab '
_cod_database_code               7000321