New Crown-Shaped Polyoxovanadium(V) Cluster Cation with a μ6-Sulfato Anion and Zwitterionic μ-(β-Alanine): Crystal Structure of [V6O12(OH)3(O2CCH2CH2NH3)3(SO4)][Na][SO4].13H2O
Chew Hee Ng; Chai Wei Lim; Siang Guan Teoh; Hoong-Kun Fun; Anwar Usman; Seik Weng Ng; Inorganic Chemistry 41 (2002) 2–3; doi:10.1021/ic015574z

data_4317414
_publ_contact_author
;
     Assoc. Prof. Seik Weng Ng
     Institute of Postgraduate Studies
     University of Malaya
     50603 Kuala Lumpur
     Malaysia
;
_publ_contact_author_email       h1nswen@umcsd.um.edu.my
_publ_contact_author_fax         '03 7967 4606'
_publ_contact_author_phone       '03 7967 4414'
_publ_section_title
;
 New Crown-Shaped Polyoxovanadium(V) Cluster Cation with a \m6-Sulfato
 Anion and Zwitterionic \m-(\b-Alanine): Crystal Structure of
 [V6O12(OH)3(O2CCH2CH2NH3)3(SO4)][Na][SO4].13H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2
_journal_page_last               3
_journal_paper_doi               10.1021/ic015574z
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C9 H50 N3 Na O42 S2 V6'
_chemical_formula_weight         1265.27
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.011(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5192(4)
_cell_length_b                   20.1185(9)
_cell_length_c                   22.6174(9)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.61
_cell_measurement_theta_min      1.36
_cell_volume                     4299.1(3)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'ORTEP-II (Johnson, 1976)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.896
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device_type  'Siemens CCD area-detector diffractometer'
_diffrn_measurement_method       '\w scan'
_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  0.1089
_diffrn_reflns_av_sigmaI/netI    0.1219
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29940
_diffrn_reflns_theta_full        29.61
_diffrn_reflns_theta_max         29.61
_diffrn_reflns_theta_min         1.36
_diffrn_standards_decay_%        <0.1
_exptl_absorpt_coefficient_mu    1.483
_exptl_absorpt_correction_T_max  0.8906
_exptl_absorpt_correction_T_min  0.5747
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.226
_refine_diff_density_min         -1.177
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         10843
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0593
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0721P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1518
_refine_ls_wR_factor_ref         0.1634
_reflns_number_gt                7324
_reflns_number_total             10843
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic015574z_si.cif
_cod_data_source_block           w30m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4317414