Mild Synthesis and Structural Characterization of a Novel Vanadyl Selenite-Hydrogen Selenite Phase, Na[VO(SeO3)(HSeO3)].1,5H2O
Stefano Canossa; Giovanni Predieri; Claudia Graiff; Crystals 8 (2018) 215–; doi:10.3390/cryst8050215

data_1549470
_publ_section_title
;
 Mild Synthesis and Structural Characterization of a Novel Vanadyl
 Selenite-Hydrogen Selenite Phase, Na[VO(SeO3)(HSeO3)].1,5H2O
;
_journal_name_full               Crystals
_journal_page_first              215
_journal_paper_doi               10.3390/cryst8050215
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'H3 Na O8 Se2 V'
_chemical_formula_sum            'H3 Na O8 Se2 V'
_chemical_formula_weight         362.87
_chemical_name_systematic        'Sodium vanadyl selenite hydrogenselenite '
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 111.6120(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.5779(16)
_cell_length_b                   7.5662(7)
_cell_length_c                   12.5844(11)
_cell_measurement_reflns_used    859
_cell_measurement_temperature    298
_cell_measurement_theta_max      26
_cell_measurement_theta_min      4
_cell_volume                     1644.6(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX2'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9710
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.358
_exptl_absorpt_coefficient_mu    10.117
_exptl_absorpt_correction_T_max  0.692
_exptl_absorpt_correction_T_min  0.620
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.931
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_preparation       metathesis
_exptl_crystal_recrystallization_method 'slow solvent evaporation'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.548
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.171
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         1697
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0488P)^2^+11.4303P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1365
_reflns_number_total             1697
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Crystals-2018-8-215.cif
_cod_data_source_block           NaSeHSeVO
_cod_database_code               1549470
_shelx_estimated_absorpt_t_max   0.151
_shelx_estimated_absorpt_t_min   0.081