Formation Principles for Vanadium Selenites: The Role of pH on Product Composition
Olshansky, Jacob H.; Wiener, Karina J.; Smith, Matthew D.; Nourmahnad, Anahita; Charles, Max J.; Zeller, Matthias; Schrier, Joshua; Norquist, Alexander J.; Inorganic Chemistry  (2014) 141103102403006–; doi:10.1021/ic501736r

data_4341433
_publ_section_title
;
 Formation Principles for Vanadium Selenites: The Role of pH on Product
 Composition
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              141103102403006
_journal_paper_doi               10.1021/ic501736r
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'H4 O21 Se6 V3, C5 H14 N2'
_chemical_formula_sum            'C5 H18 N2 O21 Se6 V3'
_chemical_formula_weight         1068.79
_space_group_IT_number           1
_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
_cell_angle_alpha                93.598(4)
_cell_angle_beta                 108.804(4)
_cell_angle_gamma                103.521(4)
_cell_formula_units_Z            1
_cell_length_a                   8.031(3)
_cell_length_b                   8.923(3)
_cell_length_c                   9.111(3)
_cell_measurement_reflns_used    1564
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.56
_cell_measurement_theta_min      2.78
_cell_volume                     594.1(4)
_computing_cell_refinement       'Apex2 v2011.2-0'
_computing_data_collection       'Apex2 v2011.2-0 (Bruker, 2011)'
_computing_data_reduction        'Apex2 v2011.2-0'
_computing_molecular_graphics    'SHELXTL 6.14'
_computing_publication_material  'SHELXTL 6.14'
_computing_structure_refinement
;  
SHELXTL 6.14, Shelxle (H\"ubschle et al., 2011)
;
_computing_structure_solution
'SHELXTL 6.14 (Bruker, 2003; Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       '\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  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13896
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         31.82
_diffrn_reflns_theta_min         2.37
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.444
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.4946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2  v2011.2-0 (Bruker, 2011)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.987
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             503
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.817
_refine_diff_density_rms         0.165
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 3363 Friedel pairs'
_refine_ls_abs_structure_Flack   0.050(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         7087
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0561P)^2^+1.1105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0979
_reflns_number_gt                6422
_reflns_number_total             7087
_reflns_threshold_expression     I>2\s(I)
_oxford_refine_ls_scale          0.5552(3)
_cod_data_source_file            ic501736r_si_002.cif
_cod_data_source_block           '[C5H14N2][(VO)3(SeO3)2(HSeO3)4]-1a'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 
;
_cod_original_cell_volume        594.1(3)
_cod_original_sg_symbol_H-M      P1
_cod_database_code               4341433