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_4341434
_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_sum            'C5 H18 N2 O21 Se6 V3'
_chemical_formula_weight         1068.79
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_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                93.563(3)
_cell_angle_beta                 108.910(2)
_cell_angle_gamma                103.594(3)
_cell_formula_units_Z            1
_cell_length_a                   8.0532(17)
_cell_length_b                   8.9284(19)
_cell_length_c                   9.111(2)
_cell_measurement_reflns_used    1542
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.2251
_cell_measurement_theta_min      2.9660
_cell_volume                     595.5(2)
_computing_cell_refinement       'SAINT V8.30C (Bruker, 2012)'
_computing_data_collection       'Apex2 v2013.4-1 (Bruker, 2012)'
_computing_data_reduction        'SAINT V8.30C (Bruker, 2012)'
_computing_molecular_graphics    'Shelxtl (Bruker, 2003)'
_computing_publication_material  'Shelxtl (Bruker, 2003)'
_computing_structure_refinement
;  
SHELXL-2013 (Sheldrick, 2013), 
SHELXLE Rev609 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9243
_diffrn_reflns_point_group_measured_fraction_full 0.927
_diffrn_reflns_point_group_measured_fraction_max 0.811
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         31.531
_diffrn_reflns_theta_min         2.777
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    10.419
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.3544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 v2013.4-1 (Bruker, 2012)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.980
_exptl_crystal_description       prism
_exptl_crystal_F_000             503
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.181(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         6461
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+0.0277P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0596
_reflns_Friedel_coverage         0.817
_reflns_Friedel_fraction_full    0.864
_reflns_Friedel_fraction_max     0.729
_reflns_number_gt                6037
_reflns_number_total             6461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic501736r_si_002.cif
_cod_data_source_block           '[C5H14N2][(VO)3(SeO3)2(HSeO3)4]-1b'
_cod_database_code               4341434
_shelx_estimated_absorpt_t_min   0.106
_shelx_estimated_absorpt_t_max   0.394