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_4309006
_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_compound_source        synthetic
_chemical_formula_moiety         '(C8 H20 N1 1+)4, (Cu2 V8 O24 4+), 2(H2 O1)'
_chemical_formula_sum            'C32 H84 Cu2 N4 O26 V8'
_chemical_formula_weight         1475.65
_chemical_melting_point          ?
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 94.058(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7401(11)
_cell_length_b                   22.488(2)
_cell_length_c                   18.5046(15)
_cell_measurement_reflns_used    15840
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      3.644
_cell_volume                     5703.4(8)
_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  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.8447
_diffrn_measured_fraction_theta_max 0.8447
_diffrn_measurement_device       'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       dtintegrate.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1809
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14677
_diffrn_reflns_theta_full        30.49
_diffrn_reflns_theta_max         30.48
_diffrn_reflns_theta_min         3.65
_exptl_absorpt_coefficient_mu    2.055
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.875
_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            Green
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.833
_refine_ls_goodness_of_fit_ref   0.874
_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_parameters     703
_refine_ls_number_reflns         14677
_refine_ls_number_restraints     200
_refine_ls_restrained_S_all      0.829
_refine_ls_restrained_S_obs      0.864
_refine_ls_R_factor_all          0.1395
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0001P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1074
_refine_ls_wR_factor_ref         0.0723
_reflns_number_gt                6356
_reflns_number_total             14677
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048751fsi20040922_034703_3.cif
_cod_data_source_block           shelxl
_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:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0001P)^2^] where P=(Fo^2^+2Fc^2^)/3' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.0001P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5703.3(8)
_cod_database_code               4309006