Cyclic Polyvanadates Incorporating Template Transition Metal Cationic Species: Synthesis and Structures of Hexavanadate [PdV6O18]4-, Octavanadate [Cu2V8O24]4-, and Decavanadate [Ni4V10O30(OH)2(H2O)6]4-
Taisei Kurata; Akira Uehara; Yoshihito Hayashi; Kiyoshi Isobe; Inorganic Chemistry 44 (2005) 2524–2530; doi:10.1021/ic048751f

data_4309004
_publ_contact_author_address
;
Department of Chemistry, Faculty of Science, Kanazawa University
Kakuma, Kanazawa, 920-1192, JAPAN
;
_publ_contact_author_email       hayashi@cacheibm.s.kanazawa-u.ac.jp
_publ_contact_author_fax         ' +81-76-264-5742 '
_publ_contact_author_name        'Yoshihito HAYASHI'
_publ_contact_author_phone       ' +81-76-264-5695 '
_publ_section_title
;
Cyclic Polyvanadates Incorporating Template Transition Metal Cationic
Species: Synthesis and Structures of Hexavanadate [PdV6O18]4-,
Octavanadate [Cu2V8O24]4-, and Decavanadate [Ni4V10O30(OH)2(H2O)6]4-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2524
_journal_page_last               2530
_journal_paper_doi               10.1021/ic048751f
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety
'(C24 H20 P1 1+)4, (H14 Ni4 O38 V10 4+), (C2 H3 N1)2, (H2 O1)2'
_chemical_formula_sum            'C100 H104 N2 Ni4 O40 P4 V10'
_chemical_formula_weight         2841.89
_chemical_melting_point          ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Thu Aug 19 19:51:27 2004'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                112.438(3)
_cell_angle_beta                 94.735(3)
_cell_angle_gamma                104.749(3)
_cell_formula_units_Z            1
_cell_length_a                   12.333(2)
_cell_length_b                   16.208(4)
_cell_length_c                   16.516(3)
_cell_measurement_reflns_used    11483
_cell_measurement_temperature    123.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.3
_cell_volume                     2890.7(10)
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_collection       CRYSTALCLEAR
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_molecular_graphics    'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  SHELXL93
_computing_structure_solution    SHELXS86
_diffrn_detector_area_resol_mean 14.62
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            340
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.31
_exptl_absorpt_coefficient_mu    1.537
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). ABSCOR - Program for Absorption Correction, Rigaku
Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       Prism
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.86
_refine_diff_density_min         -0.59
_refine_ls_extinction_coef       0.0000
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     721
_refine_ls_number_reflns         10394
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.0800
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.0458P)^2^+0.4778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1038
_reflns_number_gt                10394
_reflns_number_total             12795
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ic048751fsi20040922_034703_1.cif
_cod_data_source_block           '_kura13'
_cod_depositor_comments
;
The following automatic conversions were performed:
_chemical_melting_point value 'not measured' changed to '?' - value
is undefined or not given.
Automatic conversion script
Id: cif_fix_values 1391 2010-09-07 12:51:13Z saulius 

The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2890(1)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4309004