#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:37:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179386 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/83/4328307.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_4328307
loop_
_publ_author_name
'Roberto Fernández de Luis'
'José L. Mesa'
'M. Karmele Urtiaga'
'Edurne S. Larrea'
'Teófilo Rojo'
'María I. Arriortua'
_publ_contact_author
;
   Dra. Miren Karmele Urtiaga Greaves
   Facultad de Ciencia y Tecnología
   Dpto. de Mineralogía y Petrología 
   Universidad del País Vasco
   Apartado 644
   48080 Bilbao
   Spain
;
_publ_contact_author_email       karmele.urtiaga@ehu.es
_publ_contact_author_fax         '34 4 4648500'
_publ_contact_author_phone       '34 4 601000 ext 5372'
_publ_section_title
;
 Flexible and Dynamic Thermal Behavior of Self-Catenated
 [{Ni3(H2O)3(Bpa)4}(V6O18)].8H2O Constructed from 10-c Heterometallic
 Inorganic-Organic Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2130
_journal_page_last               2139
_journal_paper_doi               10.1021/ic201951e
_journal_volume                  51
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C48 H54 N8 Ni3 O21 V6'
_chemical_formula_sum            'C48 H54 N8 Ni3 O29 V6'
_chemical_formula_weight         1688.76
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2010-03-12T12:04:22-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 112.3880(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5536(2)
_cell_length_b                   19.0463(2)
_cell_length_c                   27.7435(3)
_cell_measurement_reflns_used    20529
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.8607
_cell_measurement_theta_min      2.8851
_cell_volume                     6622.05(15)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
        (compiled Jan 27 2009,14:17:37)
;
_computing_data_collection
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
        (compiled Jan 27 2009,14:17:37)
;
_computing_data_reduction
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
        (compiled Jan 27 2009,14:17:37)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.264
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Goniometer Xcalibur, detector: Onyx (Nova)'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0589482398
_diffrn_orient_matrix_UB_12      -0.028522269
_diffrn_orient_matrix_UB_13      -0.0501598447
_diffrn_orient_matrix_UB_21      0.0920176443
_diffrn_orient_matrix_UB_22      -0.0416466136
_diffrn_orient_matrix_UB_23      -0.012177554
_diffrn_orient_matrix_UB_31      -0.0339007723
_diffrn_orient_matrix_UB_32      -0.0631307749
_diffrn_orient_matrix_UB_33      0.0306844312
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            50933
_diffrn_reflns_theta_full        74.02
_diffrn_reflns_theta_max         74.02
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    8.446
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.50677
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
X-RED (Stoe & Cie, March 2001 Revision 1.22) and
X-SHAPE (Stoe & Cie, October 1999, Revision 1.06)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_F_000             3408
_exptl_crystal_size_max          0.1207
_exptl_crystal_size_mid          0.0533
_exptl_crystal_size_min          0.0269
_refine_diff_density_max         1.176
_refine_diff_density_min         -1.09
_refine_diff_density_rms         0.12
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     862
_refine_ls_number_reflns         13347
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1011P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1446
_reflns_number_gt                10278
_reflns_number_total             13347
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201951e_si_002.cif
_cod_data_source_block           '[{Ni3(H2O)3(Bpa)4}(V6O18)]_8H2O'
_cod_original_cell_volume        6622.05(14)
_cod_database_code               4328307
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1A N 0.8953(6) 0.2266(5) -0.0542(4) 0.0344(12) Uani 0.590(10) 1 d PD A 1
C1A C 0.8054(7) 0.1974(4) -0.0535(4) 0.0344(12) Uani 0.590(10) 1 d PD A 1
H1A H 0.7642 0.2228 -0.0394 0.041 Uiso 0.590(10) 1 calc PR A 1
C2A C 0.7725(7) 0.1312(4) -0.0730(4) 0.0344(12) Uani 0.590(10) 1 d PD A 1
H2A H 0.71 0.1126 -0.0719 0.041 Uiso 0.590(10) 1 calc PR A 1
C3A C 0.8326(7) 0.0920(4) -0.0945(3) 0.0344(12) Uani 0.590(10) 1 d PD A 1
C4A C 0.9279(7) 0.1219(4) -0.0949(3) 0.0344(12) Uani 0.590(10) 1 d PD A 1
H4A H 0.9708 0.0972 -0.1083 0.041 Uiso 0.590(10) 1 calc PR A 1
C5A C 0.9562(8) 0.1896(4) -0.0745(4) 0.0344(12) Uani 0.590(10) 1 d PD A 1
H5A H 1.0183 0.2098 -0.075 0.041 Uiso 0.590(10) 1 calc PR A 1
N1B N 0.8713(9) 0.2298(6) -0.0500(5) 0.0273(15) Uani 0.410(10) 1 d PD A 2
C1B C 0.7792(9) 0.2078(6) -0.0452(4) 0.0273(15) Uani 0.410(10) 1 d PD A 2
H1B H 0.75 0.236 -0.0267 0.033 Uiso 0.410(10) 1 calc PR A 2
C2B C 0.7275(9) 0.1461(5) -0.0662(4) 0.0273(15) Uani 0.410(10) 1 d PD A 2
H2B H 0.6652 0.1337 -0.0617 0.033 Uiso 0.410(10) 1 calc PR A 2
C3B C 0.7689(9) 0.1027(5) -0.0942(4) 0.0273(15) Uani 0.410(10) 1 d PD A 2
C4B C 0.8646(9) 0.1245(5) -0.0986(4) 0.0273(15) Uani 0.410(10) 1 d PD A 2
H4B H 0.8953 0.0969 -0.1167 0.033 Uiso 0.410(10) 1 calc PR A 2
C5B C 0.9131(10) 0.1871(5) -0.0759(4) 0.0273(15) Uani 0.410(10) 1 d PD A 2
H5B H 0.9769 0.1999 -0.0788 0.033 Uiso 0.410(10) 1 calc PR A 2
C6A C 0.7954(8) 0.0211(5) -0.1205(5) 0.061(3) Uani 0.590(10) 1 d PD A 1
H6A1 H 0.847 0.0046 -0.1344 0.073 Uiso 0.590(10) 1 calc PR A 1
H6A2 H 0.795 -0.0122 -0.0941 0.073 Uiso 0.590(10) 1 calc PR A 1
C6B C 0.7204(13) 0.0304(7) -0.1114(6) 0.060(5) Uani 0.410(10) 1 d PD A 2
H6B1 H 0.773 -0.0052 -0.0938 0.072 Uiso 0.410(10) 1 calc PR A 2
H6B2 H 0.6602 0.0243 -0.1011 0.072 Uiso 0.410(10) 1 calc PR A 2
C7 C 0.6874(4) 0.0208(3) -0.1635(3) 0.0483(14) Uani 1 1 d D . .
H7A H 0.684 0.0563 -0.1892 0.058 Uiso 1 1 calc R A 1
H7B H 0.6332 0.0314 -0.1497 0.058 Uiso 1 1 calc R A 1
C8 C 0.6302(3) -0.1733(2) -0.18841(16) 0.0242(8) Uiso 1 1 d . A .
H8 H 0.6127 -0.2113 -0.1721 0.029 Uiso 1 1 calc R . .
C9 C 0.6431(4) -0.1085(2) -0.16465(18) 0.0337(10) Uani 1 1 d . . .
H9 H 0.6352 -0.1035 -0.133 0.04 Uiso 1 1 calc R A .
C10 C 0.6680(4) -0.0507(2) -0.18838(19) 0.0343(10) Uani 1 1 d . A .
C11 C 0.6798(4) -0.0624(2) -0.23585(17) 0.0299(9) Uani 1 1 d . . .
H11 H 0.6972 -0.0254 -0.253 0.036 Uiso 1 1 calc R A .
C12 C 0.6656(3) -0.12925(19) -0.25718(16) 0.0217(7) Uani 1 1 d . A .
H12 H 0.6731 -0.136 -0.2888 0.026 Uiso 1 1 calc R . .
C13 C 0.3976(3) 0.7548(2) -0.30452(16) 0.0260(8) Uani 1 1 d . . .
H13 H 0.4184 0.7835 -0.3261 0.031 Uiso 1 1 calc R . .
C14 C 0.2912(3) 0.7559(3) -0.30955(17) 0.0340(10) Uani 1 1 d . . .
H14 H 0.2422 0.7845 -0.3344 0.041 Uiso 1 1 calc R . .
C15 C 0.2589(3) 0.7141(2) -0.27716(16) 0.0263(8) Uani 1 1 d . . .
C16 C 0.3359(3) 0.6751(2) -0.24034(19) 0.0305(9) Uani 1 1 d . . .
H16 H 0.3185 0.6485 -0.2166 0.037 Uiso 1 1 calc R . .
C17 C 0.4395(3) 0.6751(2) -0.23829(17) 0.0226(8) Uani 1 1 d . . .
H17 H 0.4896 0.6467 -0.2138 0.027 Uiso 1 1 calc R . .
C18 C 0.1432(3) 0.7099(3) -0.28388(17) 0.0306(9) Uani 1 1 d . . .
H18A H 0.1207 0.6612 -0.289 0.037 Uiso 1 1 calc R . .
H18B H 0.1005 0.7355 -0.3151 0.037 Uiso 1 1 calc R . .
C19 C 0.1213(3) 0.7391(3) -0.23791(17) 0.0322(10) Uani 1 1 d . . .
H19A H 0.1657 0.7145 -0.2065 0.039 Uiso 1 1 calc R . .
H19B H 0.1414 0.7883 -0.2335 0.039 Uiso 1 1 calc R . .
C20 C -0.1315(3) 0.7431(2) -0.20993(14) 0.0189(7) Uani 1 1 d . . .
H20 H -0.1507 0.7543 -0.182 0.023 Uiso 1 1 calc R . .
C21 C -0.0255(3) 0.7491(2) -0.20326(15) 0.0228(8) Uani 1 1 d . . .
H21 H 0.0248 0.7643 -0.1716 0.027 Uiso 1 1 calc R . .
C22 C 0.0055(3) 0.7325(2) -0.24414(16) 0.0245(8) Uani 1 1 d . . .
C23 C -0.0743(3) 0.7111(2) -0.29087(16) 0.0256(8) Uani 1 1 d . . .
H23 H -0.0575 0.7001 -0.3195 0.031 Uiso 1 1 calc R . .
C24 C -0.1785(3) 0.7066(2) -0.29425(15) 0.0204(7) Uani 1 1 d . . .
H24 H -0.2307 0.6922 -0.3257 0.024 Uiso 1 1 calc R . .
C25 C 1.1361(3) 0.5821(2) 0.11709(17) 0.0258(8) Uani 1 1 d . . .
H25 H 1.1852 0.5684 0.1029 0.031 Uiso 1 1 calc R . .
C26 C 1.1428(3) 0.5523(2) 0.16341(16) 0.0259(8) Uani 1 1 d . . .
H26 H 1.1952 0.519 0.1796 0.031 Uiso 1 1 calc R . .
C27 C 1.0712(3) 0.5718(2) 0.18628(15) 0.0243(8) Uani 1 1 d . . .
C28 C 0.9935(3) 0.6207(2) 0.15876(17) 0.0285(9) Uani 1 1 d . . .
H28 H 0.9429 0.6348 0.1718 0.034 Uiso 1 1 calc R . .
C29 C 0.9911(3) 0.6481(2) 0.11239(17) 0.0283(9) Uani 1 1 d . . .
H29 H 0.9381 0.6805 0.0949 0.034 Uiso 1 1 calc R . .
C30 C 1.0738(3) 0.5383(2) 0.23583(16) 0.0281(9) Uani 1 1 d . . .
H30A H 1.0272 0.564 0.2488 0.034 Uiso 1 1 calc R . .
H30B H 1.1457 0.5407 0.262 0.034 Uiso 1 1 calc R . .
C31 C 1.0378(3) 0.4606(2) 0.22700(16) 0.0267(8) Uani 1 1 d . . .
H31A H 1.0893 0.4335 0.2182 0.032 Uiso 1 1 calc R . .
H31B H 1.0351 0.4414 0.2589 0.032 Uiso 1 1 calc R . .
C32 C 0.7384(3) 0.4674(2) 0.15095(15) 0.0249(8) Uani 1 1 d . . .
H32 H 0.6772 0.4763 0.1575 0.03 Uiso 1 1 calc R . .
C33 C 0.8366(3) 0.4686(3) 0.19217(15) 0.0298(9) Uani 1 1 d . . .
H33 H 0.8403 0.4788 0.2256 0.036 Uiso 1 1 calc R . .
C34 C 0.9299(3) 0.4545(2) 0.18382(15) 0.0223(7) Uani 1 1 d . . .
C35 C 0.9187(3) 0.4400(2) 0.13301(16) 0.0237(8) Uani 1 1 d . . .
H35 H 0.9784 0.43 0.1255 0.028 Uiso 1 1 calc R . .
C36 C 0.8180(3) 0.4405(2) 0.09343(15) 0.0207(7) Uani 1 1 d . . .
H36 H 0.8124 0.4313 0.0596 0.025 Uiso 1 1 calc R . .
C37 C 0.6612(3) 0.2950(2) 0.06161(15) 0.0205(7) Uani 1 1 d . . .
H37 H 0.7166 0.3144 0.054 0.025 Uiso 1 1 calc R . .
C38 C 0.6672(3) 0.2245(2) 0.07534(16) 0.0259(8) Uani 1 1 d . . .
H38 H 0.7259 0.1977 0.0771 0.031 Uiso 1 1 calc R . .
C39 C 0.5851(3) 0.1943(2) 0.08635(16) 0.0232(8) Uani 1 1 d . . .
C40 C 0.5011(3) 0.2374(2) 0.08398(16) 0.0228(8) Uani 1 1 d . . .
H40 H 0.4451 0.2195 0.0918 0.027 Uiso 1 1 calc R . .
C41 C 0.5003(3) 0.30685(19) 0.07004(14) 0.0188(7) Uani 1 1 d . . .
H41 H 0.4425 0.3346 0.0683 0.023 Uiso 1 1 calc R . .
C42 C 0.5850(4) 0.1172(2) 0.09971(18) 0.0312(9) Uani 1 1 d . . .
H42A H 0.5129 0.099 0.0838 0.037 Uiso 1 1 calc R . .
H42B H 0.6292 0.0915 0.0853 0.037 Uiso 1 1 calc R . .
C43 C 0.6260(3) 0.1050(2) 0.15767(17) 0.0279(8) Uani 1 1 d . . .
H43A H 0.5869 0.1351 0.1724 0.033 Uiso 1 1 calc R . .
H43B H 0.7004 0.1188 0.1728 0.033 Uiso 1 1 calc R . .
C44 C 0.6098(4) -0.0945(2) 0.15832(16) 0.0241(8) Uani 1 1 d . . .
H44 H 0.6046 -0.1316 0.1357 0.029 Uiso 1 1 calc R . .
C45 C 0.6125(4) -0.0270(2) 0.14103(17) 0.0335(10) Uani 1 1 d . . .
H45 H 0.6116 -0.0195 0.1077 0.04 Uiso 1 1 calc R . .
C46 C 0.6165(4) 0.0301(2) 0.17310(16) 0.0264(8) Uani 1 1 d . . .
C47 C 0.6123(3) 0.0149(2) 0.22101(15) 0.0234(8) Uani 1 1 d . . .
H47 H 0.6091 0.051 0.2429 0.028 Uiso 1 1 calc R . .
C48 C 0.6129(3) -0.05421(19) 0.23632(14) 0.0189(7) Uani 1 1 d . . .
H48 H 0.6122 -0.063 0.2692 0.023 Uiso 1 1 calc R . .
N2 N 0.6415(2) -0.18443(15) -0.23397(12) 0.0174(6) Uani 1 1 d . . .
N3 N 0.4706(2) 0.71408(15) -0.26997(11) 0.0144(5) Uani 1 1 d . . .
N4 N -0.2082(2) 0.72184(15) -0.25472(12) 0.0157(6) Uani 1 1 d . . .
N5 N 1.0617(3) 0.63012(18) 0.09126(13) 0.0247(7) Uani 1 1 d . . .
N6 N 0.7286(2) 0.45366(15) 0.10166(12) 0.0171(6) Uani 1 1 d . . .
N7 N 0.5789(2) 0.33633(15) 0.05885(12) 0.0159(6) Uani 1 1 d . . .
N8 N 0.6144(2) -0.10911(15) 0.20661(11) 0.0133(5) Uani 1 1 d . . .
O1 O 0.41360(19) 0.25391(12) -0.16176(9) 0.0151(5) Uani 1 1 d . . .
O2 O 0.67928(19) 0.67212(12) -0.19033(10) 0.0158(5) Uani 1 1 d . . .
O3 O 0.3873(2) 0.36356(15) -0.10634(11) 0.0274(6) Uani 1 1 d . . .
O4 O 0.3972(3) 0.22799(18) -0.06558(13) 0.0410(8) Uani 1 1 d . . .
O5 O 0.8667(2) 0.63150(14) -0.11675(11) 0.0205(5) Uani 1 1 d . . .
O6 O 0.6802(2) 0.57789(17) -0.11008(11) 0.0300(7) Uani 1 1 d . . .
O7 O 0.4879(2) 0.52711(14) -0.18549(10) 0.0223(5) Uani 1 1 d . . .
O8 O 0.6219(2) 0.42916(16) -0.11529(10) 0.0246(6) Uani 1 1 d . . .
O9 O 0.6387(2) 0.42078(14) -0.01158(10) 0.0214(5) Uani 1 1 d . . .
O10 O 0.4967(2) 0.46547(13) 0.08709(10) 0.0172(5) Uani 1 1 d . . .
O11 O 0.5855(2) 0.29647(15) -0.07181(11) 0.0278(6) Uani 1 1 d . . .
O12 O 0.7865(2) 0.35787(16) -0.03879(11) 0.0274(6) Uani 1 1 d . A .
O13 O 0.9057(3) 0.70357(17) 0.00273(13) 0.0364(7) Uani 1 1 d . . .
O15 O 0.7337(3) 0.7824(3) 0.00340(15) 0.0575(12) Uani 1 1 d . . .
O16 O 0.7346(2) 0.72665(17) -0.09189(11) 0.0301(7) Uani 1 1 d . . .
O17 O 0.2147(3) 0.14354(19) -0.09635(13) 0.0424(8) Uani 1 1 d . . .
O18 O 0.3876(3) 0.10212(19) -0.01666(17) 0.0479(9) Uani 1 1 d . . .
O1W O 0.9445(2) 0.29567(15) 0.05234(11) 0.0271(6) Uani 1 1 d D A .
O2W O 0.9949(4) 0.42230(18) 0.01656(13) 0.0533(12) Uani 1 1 d D A .
O3W O 0.5745(2) 0.55184(13) 0.02230(10) 0.0205(5) Uani 1 1 d D . .
V1A V 0.81686(5) 0.76456(4) -0.02995(3) 0.0162(2) Uani 0.898(3) 1 d PU B 1
O14A O 0.8748(3) 0.8359(2) -0.03719(16) 0.0398(9) Uani 0.898(3) 1 d P B 1
V1B V 0.7793(5) 0.7025(3) -0.0163(2) 0.0178(17) Uiso 0.102(3) 1 d PU B 2
O14B O 0.7318(19) 0.6387(13) 0.0028(10) 0.0178(17) Uiso 0.102(3) 1 d P B 2
V2 V 0.74227(4) 0.65092(3) -0.12856(2) 0.01447(13) Uani 1 1 d . B .
V3 V 0.56826(5) 0.51760(3) -0.12549(2) 0.01672(14) Uani 1 1 d . . .
V4 V 0.65895(5) 0.37677(3) -0.05806(2) 0.01877(14) Uani 1 1 d . . .
V5 V 0.44210(5) 0.28634(3) -0.10271(2) 0.01589(13) Uani 1 1 d . . .
V6 V 0.31526(6) 0.17011(4) -0.04580(3) 0.02742(17) Uani 1 1 d . . .
Ni1 Ni 0.93950(6) 0.32556(3) -0.02140(3) 0.02322(16) Uani 1 1 d . . .
Ni2 Ni 0.57942(5) 0.44251(3) 0.04277(2) 0.01463(13) Uani 1 1 d . . .
Ni3 Ni 0.63010(4) 0.71402(3) -0.26420(2) 0.01084(13) Uani 1 1 d . . .
O4W O 1.0224(4) 0.8390(2) -0.08480(19) 0.0583(11) Uani 1 1 d . . .
O5W O 0.7610(4) 0.5800(3) 0.0010(2) 0.0743(14) Uiso 1 1 d . . .
O6W O 0.9140(6) 0.9686(4) 0.0261(3) 0.0449(17) Uiso 0.5 1 d P . .
O7W O 0.9118(8) 0.9738(5) -0.0089(4) 0.065(2) Uiso 0.5 1 d P . .
O8W O 0.8383(6) 0.5332(4) -0.0145(3) 0.0484(18) Uiso 0.5 1 d P B .
O9W O 0.7419(8) 0.6271(5) 0.0412(4) 0.065(2) Uiso 0.5 1 d P B .
O10W O 0.9495(10) -0.0553(7) -0.1789(5) 0.088(3) Uiso 0.5 1 d P . .
O11W O 0.4223(7) -0.1287(4) 0.0316(3) 0.0506(18) Uiso 0.5 1 d P . .
O12W O 0.2829(7) -0.0234(5) -0.0214(4) 0.055(2) Uiso 0.5 1 d P . .
O13W O 0.1498(8) -0.0781(5) -0.1195(4) 0.064(2) Uiso 0.5 1 d P . .
O14W O 0.1827(6) -0.0580(4) -0.0432(3) 0.0451(17) Uiso 0.5 1 d P . .
O15W O 0.4027(5) -0.0396(4) 0.0104(3) 0.0366(14) Uiso 0.5 1 d P . .
O16W O 0.1448(7) 0.0068(5) -0.1360(4) 0.054(2) Uiso 0.5 1 d P . .
O17W O 0.0521(7) 0.0533(4) -0.1362(3) 0.0505(18) Uiso 0.5 1 d P . .
H3WA H 0.583(5) 0.578(3) 0.0519(18) 0.070(9) Uiso 1 1 d D . .
H3WB H 0.628(4) 0.574(3) 0.016(3) 0.070(9) Uiso 1 1 d D . .
H1WA H 0.999(4) 0.314(3) 0.0809(18) 0.070(9) Uiso 1 1 d D . .
H1WB H 0.947(5) 0.2519(16) 0.065(2) 0.070(9) Uiso 1 1 d D . .
H2WA H 1.049(4) 0.423(4) 0.0486(14) 0.070(9) Uiso 1 1 d D . .
H2WB H 0.956(4) 0.457(3) 0.021(3) 0.070(9) Uiso 1 1 d D . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables 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_3
C1A N1A C5A 119.2(7) . .
C1A N1A Ni1 118.6(6) . .
C5A N1A Ni1 122.1(6) . .
N1A C1A C2A 122.1(9) . .
C1A C2A C3A 120.3(8) . .
C2A C3A C4A 118.0(7) . .
C2A C3A C6A 122.4(8) . .
C4A C3A C6A 119.4(8) . .
C5A C4A C3A 118.6(8) . .
N1A C5A C4A 121.8(9) . .
C5B N1B C1B 116.9(10) . .
C5B N1B Ni1 121.4(8) . .
C1B N1B Ni1 121.6(7) . .
N1B C1B C2B 123.7(10) . .
C1B C2B C3B 119.6(10) . .
C2B C3B C4B 116.9(9) . .
C2B C3B C6B 119.7(10) . .
C4B C3B C6B 122.7(10) . .
C5B C4B C3B 120.4(10) . .
N1B C5B C4B 122.4(11) . .
C7 C6A C3A 115.3(7) . .
C7 C6B C3B 112.7(11) . .
C6B C7 C6A 47.3(9) . .
C6B C7 C10 122.8(7) . .
C6A C7 C10 108.4(5) . .
N2 C8 C9 123.4(4) . .
C8 C9 C10 119.5(4) . .
C9 C10 C11 117.0(4) . .
C9 C10 C7 122.1(5) . .
C11 C10 C7 120.7(5) . .
C12 C11 C10 119.9(4) . .
N2 C12 C11 122.4(4) . .
N3 C13 C14 122.5(4) . .
C15 C14 C13 119.6(4) . .
C16 C15 C14 117.1(4) . .
C16 C15 C18 121.6(4) . .
C14 C15 C18 121.2(4) . .
C15 C16 C17 120.3(4) . .
N3 C17 C16 122.9(4) . .
C15 C18 C19 113.7(4) . .
C22 C19 C18 113.4(4) . .
N4 C20 C21 123.2(3) . .
C20 C21 C22 119.6(4) . .
C21 C22 C23 117.2(3) . .
C21 C22 C19 120.6(4) . .
C23 C22 C19 122.1(4) . .
C24 C23 C22 119.4(4) . .
N4 C24 C23 123.4(4) . .
N5 C25 C26 123.1(4) . .
C25 C26 C27 120.3(4) . .
C28 C27 C26 116.1(4) . .
C28 C27 C30 122.3(4) . .
C26 C27 C30 121.6(4) . .
C29 C28 C27 120.6(4) . .
N5 C29 C28 122.9(4) . .
C27 C30 C31 111.4(3) . .
C34 C31 C30 110.6(3) . .
N6 C32 C33 122.2(4) . .
C32 C33 C34 120.4(4) . .
C35 C34 C33 116.8(4) . .
C35 C34 C31 121.5(4) . .
C33 C34 C31 121.5(4) . .
C34 C35 C36 119.8(4) . .
N6 C36 C35 123.2(3) . .
N7 C37 C38 122.8(4) . .
C39 C38 C37 119.6(4) . .
C38 C39 C40 117.3(4) . .
C38 C39 C42 122.1(4) . .
C40 C39 C42 120.6(4) . .
C41 C40 C39 120.1(4) . .
N7 C41 C40 123.0(4) . .
C43 C42 C39 112.1(4) . .
C42 C43 C46 114.3(4) . .
N8 C44 C45 122.8(4) . .
C44 C45 C46 120.4(4) . .
C47 C46 C45 116.4(4) . .
C47 C46 C43 120.7(4) . .
C45 C46 C43 123.0(4) . .
C48 C47 C46 119.9(4) . .
N8 C48 C47 123.7(3) . .
C12 N2 C8 117.7(3) . .
C12 N2 Ni3 121.9(3) . 1_545
C8 N2 Ni3 120.3(3) . 1_545
C13 N3 C17 117.6(3) . .
C13 N3 Ni3 120.9(2) . .
C17 N3 Ni3 121.5(2) . .
C24 N4 C20 117.1(3) . .
C24 N4 Ni3 120.4(2) . 1_455
C20 N4 Ni3 122.5(2) . 1_455
C29 N5 C25 117.0(4) . .
C29 N5 Ni1 122.8(3) . 3_765
C25 N5 Ni1 120.2(3) . 3_765
C36 N6 C32 117.6(3) . .
C36 N6 Ni2 121.4(3) . .
C32 N6 Ni2 120.6(2) . .
C41 N7 C37 117.2(3) . .
C41 N7 Ni2 121.8(2) . .
C37 N7 Ni2 120.8(2) . .
C48 N8 C44 116.5(3) . .
C48 N8 Ni3 121.4(2) . 4_566
C44 N8 Ni3 122.0(2) . 4_566
V5 O1 Ni3 177.01(15) . 2_644
V2 O2 Ni3 166.72(15) . .
V5 O4 V6 162.3(3) . .
V2 O6 V3 149.34(17) . .
V4 O8 V3 128.37(16) . .
V4 O9 Ni2 158.28(16) . .
V3 O10 Ni2 177.74(17) 3_665 .
V4 O11 V5 127.09(17) . .
V4 O12 Ni1 173.3(2) . .
V1B O13 V1A 50.6(2) . .
V1B O13 Ni1 163.0(3) . 3_765
V1A O13 Ni1 141.9(2) . 3_765
V1A O15 V6 156.9(3) . 3_665
V1A O15 V1B 46.3(2) . .
V6 O15 V1B 151.2(4) 3_665 .
V2 O16 V1A 135.62(16) . .
V2 O16 V1B 110.5(2) . .
Ni2 O3W Ni2 100.96(11) . 3_665
O14A V1A O13 111.5(2) . .
O14A V1A O15 110.2(2) . .
O13 V1A O15 109.0(2) . .
O14A V1A O16 111.74(19) . .
O13 V1A O16 107.15(15) . .
O15 V1A O16 107.08(16) . .
O14B V1B O13 115.5(10) . .
O14B V1B O15 108.8(10) . .
O13 V1B O15 109.8(4) . .
O14B V1B O16 122.4(10) . .
O13 V1B O16 101.6(3) . .
O15 V1B O16 97.0(3) . .
O14B V1B O9W 20.9(10) . .
O13 V1B O9W 105.5(4) . .
O15 V1B O9W 97.1(4) . .
O16 V1B O9W 142.9(4) . .
O14B V1B O5W 24.8(9) . .
O13 V1B O5W 97.2(3) . .
O15 V1B O5W 133.1(4) . .
O16 V1B O5W 114.7(3) . .
O9W V1B O5W 37.4(3) . .
O14B V1B V2 99.4(10) . .
O13 V1B V2 94.5(3) . .
O15 V1B V2 128.7(3) . .
O16 V1B V2 32.53(13) . .
O9W V1B V2 119.5(3) . .
O5W V1B V2 84.5(2) . .
O9W O14B O5W 85.7(19) . .
O9W O14B V1B 127(2) . .
O5W O14B V1B 122.0(19) . .
O5 V2 O2 110.51(13) . .
O5 V2 O16 110.32(13) . .
O2 V2 O16 105.93(13) . .
O5 V2 O6 109.11(14) . .
O2 V2 O6 111.88(13) . .
O16 V2 O6 109.05(16) . .
O5 V2 V1B 96.33(15) . .
O2 V2 V1B 141.65(14) . .
O16 V2 V1B 36.97(15) . .
O6 V2 V1B 82.74(15) . .
O7 V3 O10 109.05(14) . 3_665
O7 V3 O8 109.75(14) . .
O10 V3 O8 111.16(12) 3_665 .
O7 V3 O6 110.26(13) . .
O10 V3 O6 109.08(14) 3_665 .
O8 V3 O6 107.52(14) . .
O12 V4 O9 108.99(15) . .
O12 V4 O8 108.54(14) . .
O9 V4 O8 109.81(13) . .
O12 V4 O11 108.30(15) . .
O9 V4 O11 110.96(14) . .
O8 V4 O11 110.18(14) . .
O3 V5 O1 110.26(14) . .
O3 V5 O4 110.57(17) . .
O1 V5 O4 109.83(14) . .
O3 V5 O11 108.31(14) . .
O1 V5 O11 108.21(13) . .
O4 V5 O11 109.60(17) . .
O17 V6 O18 109.2(2) . .
O17 V6 O4 110.01(18) . .
O18 V6 O4 108.20(19) . .
O17 V6 O15 108.95(19) . 3_665
O18 V6 O15 112.0(2) . 3_665
O4 V6 O15 108.47(19) . 3_665
O13 Ni1 O12 178.04(13) 3_765 .
O13 Ni1 N1B 97.1(3) 3_765 .
O12 Ni1 N1B 84.8(3) . .
O13 Ni1 N1A 87.8(2) 3_765 .
O12 Ni1 N1A 94.2(2) . .
N1B Ni1 N1A 10.8(3) . .
O13 Ni1 O1W 91.74(13) 3_765 .
O12 Ni1 O1W 87.98(12) . .
N1B Ni1 O1W 88.8(3) . .
N1A Ni1 O1W 94.4(3) . .
O13 Ni1 N5 89.40(14) 3_765 3_765
O12 Ni1 N5 90.61(13) . 3_765
N1B Ni1 N5 98.9(4) . 3_765
N1A Ni1 N5 93.5(3) . 3_765
O1W Ni1 N5 172.03(13) . 3_765
O13 Ni1 O2W 88.54(16) 3_765 .
O12 Ni1 O2W 89.50(16) . .
N1B Ni1 O2W 170.1(3) . .
N1A Ni1 O2W 175.4(3) . .
O1W Ni1 O2W 82.96(14) . .
N5 Ni1 O2W 89.19(15) 3_765 .
O10 Ni2 O9 170.45(11) . .
O10 Ni2 N6 95.73(11) . .
O9 Ni2 N6 93.66(12) . .
O10 Ni2 N7 91.84(11) . .
O9 Ni2 N7 89.76(11) . .
N6 Ni2 N7 90.73(12) . .
O10 Ni2 O3W 88.98(10) . .
O9 Ni2 O3W 88.99(11) . .
N6 Ni2 O3W 91.82(11) . .
N7 Ni2 O3W 177.22(12) . .
O10 Ni2 O3W 85.12(11) . 3_665
O9 Ni2 O3W 85.33(11) . 3_665
N6 Ni2 O3W 170.82(11) . 3_665
N7 Ni2 O3W 98.38(11) . 3_665
O3W Ni2 O3W 79.04(11) . 3_665
O1 Ni3 O2 177.63(10) 2_654 .
O1 Ni3 N2 90.47(11) 2_654 1_565
O2 Ni3 N2 90.73(11) . 1_565
O1 Ni3 N3 91.55(11) 2_654 .
O2 Ni3 N3 90.55(11) . .
N2 Ni3 N3 86.94(12) 1_565 .
O1 Ni3 N4 89.35(11) 2_654 1_655
O2 Ni3 N4 88.64(11) . 1_655
N2 Ni3 N4 88.30(12) 1_565 1_655
N3 Ni3 N4 175.16(12) . 1_655
O1 Ni3 N8 91.02(10) 2_654 4_565
O2 Ni3 N8 87.85(10) . 4_565
N2 Ni3 N8 177.63(12) 1_565 4_565
N3 Ni3 N8 91.17(11) . 4_565
N4 Ni3 N8 93.57(11) 1_655 4_565
O14B O5W O8W 144.8(13) . .
O9W O5W O8W 149.0(7) . .
O9W O5W V1B 68.7(5) . .
O8W O5W V1B 111.6(4) . .
O14B O9W O5W 51.2(14) . .
O5W O9W V1B 73.9(5) . .
O14W O12W O15W 140.4(8) . .
O12W O15W O11W 111.6(6) . .
O17W O16W O13W 120.4(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1A C1A 1.345(10) .
N1A C5A 1.361(10) .
N1A Ni1 2.080(9) .
C1A C2A 1.378(10) .
C2A C3A 1.394(11) .
C3A C4A 1.416(11) .
C3A C6A 1.524(10) .
C4A C5A 1.400(9) .
N1B C5B 1.346(12) .
N1B C1B 1.370(13) .
N1B Ni1 2.063(11) .
C1B C2B 1.377(12) .
C2B C3B 1.391(13) .
C3B C4B 1.410(14) .
C3B C6B 1.523(13) .
C4B C5B 1.389(12) .
C6A C7 1.495(11) .
C6B C7 1.352(15) .
C7 C10 1.505(7) .
C8 N2 1.347(5) .
C8 C9 1.378(6) .
C9 C10 1.388(7) .
C10 C11 1.404(7) .
C11 C12 1.386(6) .
C12 N2 1.337(5) .
C13 N3 1.333(5) .
C13 C14 1.396(5) .
C14 C15 1.391(6) .
C15 C16 1.368(6) .
C15 C18 1.509(5) .
C16 C17 1.383(5) .
C17 N3 1.336(5) .
C18 C19 1.521(6) .
C19 C22 1.517(5) .
C20 N4 1.344(5) .
C20 C21 1.382(5) .
C21 C22 1.388(6) .
C22 C23 1.395(6) .
C23 C24 1.383(5) .
C24 N4 1.336(5) .
C25 N5 1.348(5) .
C25 C26 1.376(6) .
C26 C27 1.396(6) .
C27 C28 1.394(6) .
C27 C30 1.505(6) .
C28 C29 1.377(6) .
C29 N5 1.343(6) .
C30 C31 1.548(6) .
C31 C34 1.501(5) .
C32 N6 1.348(5) .
C32 C33 1.385(5) .
C33 C34 1.396(6) .
C34 C35 1.387(6) .
C35 C36 1.388(5) .
C36 N6 1.339(5) .
C37 N7 1.344(5) .
C37 C38 1.390(5) .
C38 C39 1.385(6) .
C39 C40 1.386(6) .
C39 C42 1.516(5) .
C40 C41 1.376(5) .
C41 N7 1.341(5) .
C42 C43 1.506(6) .
C43 C46 1.509(6) .
C44 N8 1.346(5) .
C44 C45 1.378(6) .
C45 C46 1.393(6) .
C46 C47 1.383(6) .
C47 C48 1.381(5) .
C48 N8 1.336(5) .
N2 Ni3 2.090(3) 1_545
N3 Ni3 2.106(3) .
N4 Ni3 2.110(3) 1_455
N5 Ni1 2.108(4) 3_765
N6 Ni2 2.071(3) .
N7 Ni2 2.072(3) .
N8 Ni3 2.136(3) 4_566
O1 V5 1.653(2) .
O1 Ni3 2.054(2) 2_644
O2 V2 1.648(2) .
O2 Ni3 2.059(3) .
O3 V5 1.633(3) .
O4 V5 1.773(3) .
O4 V6 1.793(3) .
O5 V2 1.634(3) .
O6 V2 1.799(3) .
O6 V3 1.819(3) .
O7 V3 1.615(3) .
O8 V4 1.778(3) .
O8 V3 1.813(3) .
O9 V4 1.646(3) .
O9 Ni2 2.003(3) .
O10 V3 1.652(3) 3_665
O10 Ni2 2.002(3) .
O11 V4 1.785(3) .
O11 V5 1.811(3) .
O12 V4 1.643(3) .
O12 Ni1 2.037(3) .
O13 V1B 1.590(7) .
O13 V1A 1.670(3) .
O13 Ni1 2.037(3) 3_765
O15 V1A 1.742(4) .
O15 V6 1.799(4) 3_665
O15 V1B 1.804(7) .
O16 V2 1.791(3) .
O16 V1A 1.805(3) .
O16 V1B 2.003(7) .
O17 V6 1.620(4) .
O18 V6 1.640(4) .
O1W Ni1 2.100(3) .
O2W Ni1 2.113(3) .
O3W Ni2 2.153(3) .
O3W Ni2 2.180(3) 3_665
V1A O14A 1.620(4) .
V1B O14B 1.56(3) .
V1B O9W 2.340(12) .
V1B O5W 2.413(8) .
V1B V2 3.119(6) .
O14B O9W 1.05(3) .
O14B O5W 1.19(2) .
V3 O10 1.652(3) 3_665
V6 O15 1.799(4) 3_665
Ni1 O13 2.037(3) 3_765
Ni1 N5 2.108(4) 3_765
Ni2 O3W 2.180(3) 3_665
Ni3 O1 2.054(2) 2_654
Ni3 N2 2.090(3) 1_565
Ni3 N4 2.110(3) 1_655
Ni3 N8 2.136(3) 4_565
O5W O9W 1.528(11) .
O5W O8W 1.555(10) .
O6W O7W 0.967(12) .
O11W O15W 1.782(10) .
O12W O14W 1.421(11) .
O12W O15W 1.555(11) .
O13W O16W 1.676(13) .
O16W O17W 1.535(12) .
