New sulfate-bridged dinuclear oxidovanadium complexes
Evgenia S. Bazhinaa; Marina E. Nikiforova; Grigory G. Aleksandrov; Nikolay N. Efimov; Helena A. Ugolkova; Oleg M. Nikitin; Tatiana V. Magdesieva; Artem S. Bogomyakov; Vadim V. Minin; Aleksei A. Sidorov; Vladimir M. Novotortsev; Igor L. Eremenko; Inorganica Chimica Acta 392 (2012) 192–198; doi:10.1016/j.ica.2012.06.001

data_1512481
_publ_section_title
;
 New sulfate-bridged dinuclear oxidovanadium complexes
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              192
_journal_page_last               198
_journal_paper_doi               10.1016/j.ica.2012.06.001
_journal_volume                  392
_journal_year                    2012
_chemical_formula_moiety         'C38 H56 N4 O12 S2 V2, 4(C H4 O)'
_chemical_formula_sum            'C42 H72 N4 O16 S2 V2'
_chemical_formula_weight         1055.04
_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                93.5630(10)
_cell_angle_beta                 103.7080(10)
_cell_angle_gamma                116.3860(10)
_cell_formula_units_Z            1
_cell_length_a                   10.9943(7)
_cell_length_b                   11.2068(7)
_cell_length_c                   11.9861(8)
_cell_measurement_reflns_used    4739
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.95
_cell_measurement_theta_min      2.16
_cell_volume                     1261.26(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0369
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12684
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         2.07
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.523
_exptl_absorpt_correction_T_max  0.9496
_exptl_absorpt_correction_T_min  0.8893
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS v2004/1, Sheldrick, G.M., (2004)'
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             558
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         6288
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0890P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1254
_reflns_number_gt                5259
_reflns_number_total             6288
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2012-392-192-198-1.cif
_cod_data_source_block           v
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1512481