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_4341437
_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         'C5 H18 N2 O21 Se6 V3'
_chemical_formula_sum            'C5 H18 N2 O21 Se6 V3'
_chemical_formula_weight         1068.78
_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   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                93.9196(18)
_cell_angle_beta                 108.7243(16)
_cell_angle_gamma                103.2235(17)
_cell_formula_units_Z            1
_cell_length_a                   8.0016(12)
_cell_length_b                   8.9089(14)
_cell_length_c                   9.1270(14)
_cell_measurement_reflns_used    4622
_cell_measurement_temperature    100
_cell_measurement_theta_max      31
_cell_measurement_theta_min      2
_cell_volume                     592.71(16)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13266
_diffrn_reflns_theta_full        25.292
_diffrn_reflns_theta_max         31.615
_diffrn_reflns_theta_min         2.377
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.469
_exptl_absorpt_correction_T_max  0.04
_exptl_absorpt_correction_T_min  0.03
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.994
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             503
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.68
_refine_diff_density_min         -1.87
_refine_ls_abs_structure_details 'Flack (1983), 3273 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.034(8)
_refine_ls_extinction_coef       37.7(14)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.8764
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         6465
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0234
_refine_ls_shift/su_max          0.0009315
_refine_ls_shift/su_mean         0.0000596
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 55.4 81.2 57.3 23.0 8.78 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0587
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0577
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              13
_reflns_limit_l_min              -13
_reflns_number_gt                6661
_reflns_number_total             6923
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0227
_oxford_refine_ls_scale          0.5938(8)
_oxford_reflns_number_all        6907
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ic501736r_si_002.cif
_cod_data_source_block           '[(S)-C5H14N2][(VO)3(SeO3)2(HSeO3)4]-3b'
_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.

'_atom_sites_solution_primary' value 'Direct' changed to
'direct' 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_sg_symbol_H-M      'P 1 '
_cod_database_code               4341437