Bis(aqua)bis(eta5-cyclopentadienyl)vanadium(IV) bis(trifluoromethanesulfonate) tetrahydrofuran solvate: Synthesis and characterization
Theocharis C. Stamatatos; Spyros P. Perlepes; Catherine P. Raptopoulou; Aris Terzis; Nikolaos Klouras; Inorganica Chimica Acta 394 (2013) 747–751; doi:10.1016/j.ica.2012.09.038

data_1512832
_publ_section_title
;
 Bis(aqua)bis(eta5-cyclopentadienyl)vanadium(IV)
 bis(trifluoromethanesulfonate) tetrahydrofuran solvate: Synthesis and
 characterization
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              747
_journal_page_last               751
_journal_paper_doi               10.1016/j.ica.2012.09.038
_journal_volume                  394
_journal_year                    2013
_chemical_formula_sum            'C16 H22 F6 O9 S2 V'
_chemical_formula_weight         587.40
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.936(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.1577(1)
_cell_length_b                   21.0261(3)
_cell_length_c                   13.4999(2)
_cell_measurement_reflns_used    15615
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      71.96
_cell_measurement_theta_min      6.56
_cell_volume                     2315.26(6)
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       '\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16123
_diffrn_reflns_theta_full        65.00
_diffrn_reflns_theta_max         65.00
_diffrn_reflns_theta_min         6.64
_exptl_absorpt_coefficient_mu    6.153
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.350
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         3803
_refine_ls_number_restraints     160
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0541P)^2^+0.8718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1044
_reflns_number_gt                3402
_reflns_number_total             3803
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-394-747-751.cif
_cod_data_source_block           nkv118
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               1512832