Role of Hydrogen-Bonding in the Formation of Polar Achiral and Nonpolar Chiral Vanadium Selenite Frameworks
Jacob H. Olshansky; Thanh Thao Tran; Kristen J. Hernandez; Matthias Zeller; P. Shiv Halasyamani; Joshua Schrier; Alexander J. Norquist; Inorganic Chemistry 51 (2012) 11040–11048; doi:10.1021/ic3015496

data_4330710
_publ_contact_author_address
; 
Department of Chemistry
Haverford College
370 Lancaster Avenue
Haverford PA, 19041 
;
_publ_contact_author_email       anorquis@haverford.edu
_publ_contact_author_fax         '610 896 4963'
_publ_contact_author_name        'Alexander J Norquist'
_publ_contact_author_phone       '610 896 2949'
_publ_section_title
;
 Role of Hydrogen-Bonding in the Formation of Polar Achiral and Nonpolar
 Chiral Vanadium Selenite Frameworks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11040
_journal_page_last               11048
_journal_paper_doi               10.1021/ic3015496
_journal_volume                  51
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C5 H20 N2 O16 Se4 V2'
_chemical_formula_sum            'C5 H20 N2 O16 Se4 V2'
_chemical_formula_weight         781.94
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.523(5)
_cell_length_b                   14.382(5)
_cell_length_c                   12.667(5)
_cell_measurement_reflns_used    7918
_cell_measurement_temperature    100
_cell_measurement_theta_max      32
_cell_measurement_theta_min      2
_cell_volume                     1917.0(14)
_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 0.986
_diffrn_measured_fraction_theta_max 0.931
_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  0.024
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14715
_diffrn_reflns_theta_full        25.104
_diffrn_reflns_theta_max         31.778
_diffrn_reflns_theta_min         1.416
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.653
_exptl_absorpt_correction_T_max  0.19
_exptl_absorpt_correction_T_min  0.05
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            aquamarine
_exptl_crystal_density_diffrn    2.709
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.56
_refine_diff_density_min         -0.51
_refine_ls_abs_structure_details 'Flack (1983), 2632 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.199(11)
_refine_ls_extinction_coef       11.0(17)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9769
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         5284
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0202
_refine_ls_shift/su_max          0.0009343
_refine_ls_shift/su_mean         0.0000412
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 3.05P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0467
_refine_ls_wR_factor_gt          0.0455
_refine_ls_wR_factor_ref         0.0447
_reflns_limit_h_max              15
_reflns_limit_h_min              0
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              -18
_reflns_number_gt                5469
_reflns_number_total             5812
_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   0.0192
_oxford_refine_ls_scale          0.26196(11)
_oxford_reflns_number_all        5799
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ic3015496_si_001_4.cif
_cod_data_source_block
'[C~5~H~14~N~2~][VO(SeO~3~)(HSeO~3~)]~2~.2H~2~O_Cmp-3'
_cod_original_sg_symbol_H-M      'P c a 21 '
_cod_database_code               4330710