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_7000320
_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         'F3 O8 V2, 2(F H), H2 O, 3(Cs) '
_chemical_formula_sum            'Cs3 F5 H4 O9 V2'
_chemical_formula_weight         743.64
_chemical_name_systematic
;
tricaesium mu-fluoro-mu-peroxo-bis(fluorooxodiperoxovanadate(V))
hydrogenfluoride disolvate monohydrate
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 113.041(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.695(2)
_cell_length_b                   8.7388(9)
_cell_length_c                   13.9833(10)
_cell_measurement_reflns_used    5816
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      31.487
_cell_measurement_theta_min      2.9080
_cell_volume                     1427.5(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.3611
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'KUMA KM4 + CCD'
_diffrn_measurement_method       'rotation method, \w--scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0156
_diffrn_reflns_av_sigmaI/netI    0.0086
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5943
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    8.936
_exptl_absorpt_correction_T_max  0.2096
_exptl_absorpt_correction_T_min  0.0504
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.6 (release 21-05-2007 CrysAlis171 .NET)
(compiled May 21 2007,16:32:00)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    3.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.045
_refine_diff_density_min         -1.134
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.355
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         1360
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.353
_refine_ls_R_factor_all          0.0215
_refine_ls_R_factor_gt           0.0212
_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^)+(0.0190P)^2^+15.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0535
_refine_ls_wR_factor_ref         0.0537
_reflns_number_gt                1350
_reflns_number_total             1360
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b813228c.txt
_cod_data_source_block           fp2
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7000320