#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:47:07 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179128 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/90/4309004.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4309004
loop_
_publ_author_name
'Taisei Kurata'
'Akira Uehara'
'Yoshihito Hayashi'
'Kiyoshi Isobe'
_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       ω
_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/[σ²(Fo²) + (0.0458P)²+0.4778P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni(1) Ni -0.03168(3) -0.07550(3) -0.09543(2) 0.01025(9) Uani 1.00 d . . .
Ni(2) Ni 0.12829(3) 0.12021(3) -0.05223(2) 0.01123(9) Uani 1.00 d . . .
V(1) V -0.19895(4) -0.19354(4) -0.29028(3) 0.0126(1) Uani 1.00 d . . .
V(2) V 0.02685(4) -0.23873(4) -0.25823(3) 0.0119(1) Uani 1.00 d . . .
V(3) V 0.02270(4) -0.26111(3) -0.07377(3) 0.0106(1) Uani 1.00 d . . .
V(4) V 0.27439(4) -0.11548(3) 0.06901(3) 0.0117(1) Uani 1.00 d . . .
V(5) V 0.11569(4) -0.03111(4) 0.21837(3) 0.0117(1) Uani 1.00 d . . .
P(1) P -0.38165(7) 0.41533(6) 0.22557(5) 0.0158(2) Uani 1.00 d . . .
P(2) P -0.22472(8) 0.19955(6) -0.39305(5) 0.0195(2) Uani 1.00 d . . .
O(1) O -0.1673(2) -0.0848(2) -0.3051(1) 0.0170(4) Uani 1.00 d . . .
O(2) O -0.3273(2) -0.2575(2) -0.3444(1) 0.0191(5) Uani 1.00 d . . .
O(3) O -0.1889(2) -0.1654(1) -0.1798(1) 0.0145(4) Uani 1.00 d . . .
O(4) O -0.1046(2) -0.2631(2) -0.3308(1) 0.0168(4) Uani 1.00 d . . .
O(5) O 0.0685(2) -0.1243(2) -0.1865(1) 0.0143(4) Uani 1.00 d . . .
O(6) O 0.1197(2) -0.2606(2) -0.3201(1) 0.0181(5) Uani 1.00 d . . .
O(7) O 0.0155(2) -0.3082(2) -0.1922(1) 0.0162(4) Uani 1.00 d . . .
O(8) O -0.0359(2) -0.1729(1) -0.0430(1) 0.0125(4) Uani 1.00 d . . .
O(9) O -0.0503(2) -0.3401(2) -0.0439(1) 0.0155(4) Uani 1.00 d . . .
O(10) O 0.1666(2) -0.2201(2) -0.0142(1) 0.0173(4) Uani 1.00 d . . .
O(11) O 0.3007(2) -0.0321(2) 0.0333(1) 0.0179(5) Uani 1.00 d . . .
O(12) O 0.3928(2) -0.1414(2) 0.0838(1) 0.0170(4) Uani 1.00 d . . .
O(13) O 0.2267(2) -0.0756(2) 0.1738(1) 0.0177(5) Uani 1.00 d . . .
O(14) O 0.0241(2) -0.0315(1) 0.1359(1) 0.0130(4) Uani 1.00 d . . .
O(15) O 0.0429(2) -0.1038(2) 0.2549(1) 0.0184(5) Uani 1.00 d . . .
O(16) O 0.1091(2) 0.0214(1) -0.0057(1) 0.0108(4) Uani 1.00 d . . .
O(17) O 0.2121(2) 0.0525(2) -0.1496(1) 0.0168(4) Uani 1.00 d . . .
O(18) O 0.2759(2) 0.2064(2) 0.0422(1) 0.0164(4) Uani 1.00 d . . .
O(19) O 0.1297(2) 0.2217(2) -0.1007(1) 0.0181(5) Uani 1.00 d . . .
O(20) O 0.4074(2) 0.0959(2) -0.0298(1) 0.0184(5) Uani 1.00 d . . .
N(1) N 0.3928(6) 0.2714(5) -0.2946(5) 0.107(2) Uani 1.00 d . . .
C(1) C -0.5119(3) 0.4416(2) 0.2488(2) 0.0212(7) Uani 1.00 d . . .
C(2) C -0.5939(3) 0.4304(3) 0.1794(2) 0.0280(8) Uani 1.00 d . . .
C(3) C -0.7028(4) 0.4344(3) 0.1951(3) 0.041(1) Uani 1.00 d . . .
C(4) C -0.7279(3) 0.4494(3) 0.2792(3) 0.040(1) Uani 1.00 d . . .
C(5) C -0.6460(3) 0.4613(3) 0.3481(3) 0.0338(9) Uani 1.00 d . . .
C(6) C -0.5386(3) 0.4573(3) 0.3337(2) 0.0253(7) Uani 1.00 d . . .
C(7) C -0.3424(3) 0.4373(2) 0.1317(2) 0.0219(7) Uani 1.00 d . . .
C(8) C -0.3021(4) 0.5298(3) 0.1424(3) 0.0354(9) Uani 1.00 d . . .
C(9) C -0.2694(5) 0.5489(3) 0.0714(3) 0.051(1) Uani 1.00 d . . .
C(10) C -0.2747(5) 0.4761(4) -0.0090(3) 0.049(1) Uani 1.00 d . . .
C(11) C -0.3142(4) 0.3853(3) -0.0200(3) 0.042(1) Uani 1.00 d . . .
C(12) C -0.3497(4) 0.3642(3) 0.0504(2) 0.0306(8) Uani 1.00 d . . .
C(13) C -0.2674(3) 0.4886(2) 0.3218(2) 0.0187(7) Uani 1.00 d . . .
C(14) C -0.2693(3) 0.5786(3) 0.3780(2) 0.0298(8) Uani 1.00 d . . .
C(15) C -0.1816(4) 0.6342(3) 0.4517(3) 0.0352(9) Uani 1.00 d . . .
C(16) C -0.0912(3) 0.6029(3) 0.4689(2) 0.0309(9) Uani 1.00 d . . .
C(17) C -0.0873(3) 0.5169(3) 0.4116(2) 0.0290(8) Uani 1.00 d . . .
C(18) C -0.1765(3) 0.4581(2) 0.3380(2) 0.0224(7) Uani 1.00 d . . .
C(19) C -0.4061(3) 0.2937(2) 0.2012(2) 0.0141(6) Uani 1.00 d . . .
C(20) C -0.5080(3) 0.2429(2) 0.2145(2) 0.0170(6) Uani 1.00 d . . .
C(21) C -0.5258(3) 0.1510(2) 0.2006(2) 0.0194(7) Uani 1.00 d . . .
C(22) C -0.4428(3) 0.1082(2) 0.1737(2) 0.0186(6) Uani 1.00 d . . .
C(23) C -0.3424(3) 0.1572(2) 0.1592(2) 0.0181(6) Uani 1.00 d . . .
C(24) C -0.3238(3) 0.2495(2) 0.1722(2) 0.0176(6) Uani 1.00 d . . .
C(25) C -0.3024(3) 0.2429(2) -0.4565(2) 0.0195(7) Uani 1.00 d . . .
C(26) C -0.4006(3) 0.2633(3) -0.4326(2) 0.0310(9) Uani 1.00 d . . .
C(27) C -0.4604(3) 0.2981(3) -0.4796(3) 0.0328(9) Uani 1.00 d . . .
C(28) C -0.4225(3) 0.3122(3) -0.5512(2) 0.0252(7) Uani 1.00 d . . .
C(29) C -0.3235(3) 0.2941(3) -0.5737(2) 0.0286(8) Uani 1.00 d . . .
C(30) C -0.2618(3) 0.2600(3) -0.5264(2) 0.0270(8) Uani 1.00 d . . .
C(31) C -0.3195(4) 0.1059(3) -0.3763(2) 0.0292(8) Uani 1.00 d . . .
C(32) C -0.3962(4) 0.1239(3) -0.3207(3) 0.044(1) Uani 1.00 d . . .
C(33) C -0.4723(5) 0.0485(4) -0.3123(3) 0.057(1) Uani 1.00 d . . .
C(34) C -0.4693(5) -0.0407(3) -0.3551(3) 0.051(1) Uani 1.00 d . . .
C(35) C -0.3877(5) -0.0565(3) -0.4052(4) 0.057(1) Uani 1.00 d . . .
C(36) C -0.3129(4) 0.0162(3) -0.4167(3) 0.041(1) Uani 1.00 d . . .
C(37) C -0.1536(3) 0.2953(2) -0.2879(2) 0.0193(7) Uani 1.00 d . . .
C(38) C -0.1386(3) 0.2815(3) -0.2096(2) 0.0251(8) Uani 1.00 d . . .
C(39) C -0.0757(4) 0.3578(3) -0.1304(2) 0.0352(9) Uani 1.00 d . . .
C(40) C -0.0282(4) 0.4445(3) -0.1303(2) 0.038(1) Uani 1.00 d . . .
C(41) C -0.0424(4) 0.4581(3) -0.2080(3) 0.0330(9) Uani 1.00 d . . .
C(42) C -0.1055(3) 0.3831(3) -0.2869(2) 0.0264(8) Uani 1.00 d . . .
C(43) C -0.1198(4) 0.1576(3) -0.4515(2) 0.0293(8) Uani 1.00 d . . .
C(44) C -0.0095(4) 0.1805(3) -0.4057(3) 0.0350(9) Uani 1.00 d . . .
C(45) C 0.0707(5) 0.1442(4) -0.4500(4) 0.053(1) Uani 1.00 d . . .
C(46) C 0.0374(6) 0.0848(4) -0.5403(4) 0.066(2) Uani 1.00 d . . .
C(47) C -0.0692(6) 0.0622(4) -0.5868(3) 0.066(2) Uani 1.00 d . . .
C(48) C -0.1502(5) 0.0972(4) -0.5433(3) 0.054(1) Uani 1.00 d . . .
C(50) C 0.3964(5) 0.2584(4) -0.2311(5) 0.065(2) Uani 1.00 d . . .
C(51) C 0.4012(5) 0.2439(5) -0.1494(5) 0.074(2) Uani 1.00 d . . .
H(1) H -0.5761 0.4202 0.1214 0.0344 Uiso 1.00 calc . . .
H(2) H -0.7601 0.4276 0.1483 0.0493 Uiso 1.00 calc . . .
H(3) H -0.8031 0.4507 0.2886 0.0468 Uiso 1.00 calc . . .
H(4) H -0.6641 0.4719 0.4058 0.0405 Uiso 1.00 calc . . .
H(5) H -0.4810 0.4658 0.3817 0.0308 Uiso 1.00 calc . . .
H(6) H -0.2973 0.5804 0.1986 0.0420 Uiso 1.00 calc . . .
H(7) H -0.2430 0.6126 0.0787 0.0609 Uiso 1.00 calc . . .
H(8) H -0.2509 0.4898 -0.0575 0.0589 Uiso 1.00 calc . . .
H(9) H -0.3178 0.3351 -0.0760 0.0502 Uiso 1.00 calc . . .
H(10) H -0.3778 0.3008 0.0431 0.0373 Uiso 1.00 calc . . .
H(11) H -0.3305 0.6007 0.3655 0.0358 Uiso 1.00 calc . . .
H(12) H -0.1827 0.6956 0.4909 0.0412 Uiso 1.00 calc . . .
H(13) H -0.0317 0.6415 0.5210 0.0374 Uiso 1.00 calc . . .
H(14) H -0.0224 0.4968 0.4222 0.0348 Uiso 1.00 calc . . .
H(15) H -0.1745 0.3969 0.2988 0.0276 Uiso 1.00 calc . . .
H(16) H -0.5652 0.2725 0.2331 0.0203 Uiso 1.00 calc . . .
H(17) H -0.5956 0.1164 0.2096 0.0231 Uiso 1.00 calc . . .
H(18) H -0.4553 0.0444 0.1649 0.0224 Uiso 1.00 calc . . .
H(19) H -0.2858 0.1271 0.1399 0.0216 Uiso 1.00 calc . . .
H(20) H -0.2549 0.2835 0.1616 0.0208 Uiso 1.00 calc . . .
H(21) H -0.4278 0.2528 -0.3836 0.0373 Uiso 1.00 calc . . .
H(22) H -0.5281 0.3126 -0.4622 0.0391 Uiso 1.00 calc . . .
H(23) H -0.4654 0.3342 -0.5851 0.0304 Uiso 1.00 calc . . .
H(24) H -0.2968 0.3046 -0.6230 0.0344 Uiso 1.00 calc . . .
H(25) H -0.1917 0.2490 -0.5415 0.0329 Uiso 1.00 calc . . .
H(26) H -0.3955 0.1872 -0.2876 0.0511 Uiso 1.00 calc . . .
H(27) H -0.5270 0.0606 -0.2747 0.0678 Uiso 1.00 calc . . .
H(28) H -0.5236 -0.0920 -0.3507 0.0623 Uiso 1.00 calc . . .
H(29) H -0.3821 -0.1192 -0.4333 0.0660 Uiso 1.00 calc . . .
H(30) H -0.2563 0.0045 -0.4527 0.0511 Uiso 1.00 calc . . .
H(31) H -0.1708 0.2204 -0.2107 0.0306 Uiso 1.00 calc . . .
H(32) H -0.0655 0.3501 -0.0759 0.0418 Uiso 1.00 calc . . .
H(33) H 0.0158 0.4964 -0.0756 0.0458 Uiso 1.00 calc . . .
H(34) H -0.0086 0.5188 -0.2073 0.0401 Uiso 1.00 calc . . .
H(35) H -0.1161 0.3919 -0.3408 0.0315 Uiso 1.00 calc . . .
H(36) H 0.0117 0.2220 -0.3429 0.0421 Uiso 1.00 calc . . .
H(37) H 0.1479 0.1602 -0.4187 0.0665 Uiso 1.00 calc . . .
H(38) H 0.0920 0.0586 -0.5710 0.0773 Uiso 1.00 calc . . .
H(39) H -0.0887 0.0226 -0.6494 0.0770 Uiso 1.00 calc . . .
H(40) H -0.2269 0.0801 -0.5757 0.0652 Uiso 1.00 calc . . .
H(41) H 0.3754 0.2879 -0.1056 0.0842 Uiso 1.00 calc . . .
H(42) H 0.3545 0.1816 -0.1614 0.0842 Uiso 1.00 calc . . .
H(43) H 0.4784 0.2503 -0.1261 0.0842 Uiso 1.00 calc . . .
H(44) H 0.2630 0.1983 0.0863 0.0101 Uiso 1.00 calc . . .
H(45) H 0.3430 0.1875 0.0318 0.0101 Uiso 1.00 calc . . .
H(46) H 0.0964 0.2596 -0.0588 0.0101 Uiso 1.00 calc . . .
H(47) H 0.0764 0.1974 -0.1490 0.0101 Uiso 1.00 calc . . .
H(48) H 0.1586 -0.0075 -0.1692 0.0101 Uiso 1.00 calc . . .
H(49) H 0.2562 0.0568 -0.1205 0.0101 Uiso 1.00 calc . . .
H(50) H 0.1640 0.0011 0.0082 0.0101 Uiso 1.00 calc . . .
H(51) H 0.4762 0.1155 -0.0338 0.0101 Uiso 1.00 calc . . .
H(52) H 0.3962 0.0504 -0.0077 0.0101 Uiso 1.00 calc . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
V V 0.300 0.529
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ni Ni 0.339 1.112
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
P P 0.102 0.094
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
? ? ? ? ? ? ? ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
? ? ? ? ? ?
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?
