#------------------------------------------------------------------------------
#$Date: 2016-02-16 20:30:59 +0000 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/82/4308255.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_4308255
loop_
_publ_author_name
'Rachel Shaw'
'Rebecca H. Laye'
'Leigh F. Jones'
'David M. Low'
'Caytie Talbot-Eeckelaers'
'Qiang Wei'
'Constantinos J. Milios'
'Simon Teat'
'Madeleine Helliwell'
'James Raftery'
'Marco Evangelisti'
'Marco Affronte'
'David Collison'
'Euan K. Brechin'
'Eric J. L. McInnes'
_publ_section_title
;
1,2,3-Triazolate-Bridged Tetradecametallic Transition Metal Clusters
[M14(L)6O6(OMe)18X6] (M = FeIII, CrIII and VIII/IV) and Related Compounds:
Ground-State Spins Ranging from S=0 to S=25 and Spin-Enhanced
Magnetocaloric Effect
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4968
_journal_page_last               4978
_journal_paper_doi               10.1021/ic070320k
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C67.3 H107.2 Cl2.1 N18 O29.2 V14'
_chemical_formula_weight         2423.32
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                66.155(2)
_cell_angle_beta                 75.976(2)
_cell_angle_gamma                76.399(2)
_cell_formula_units_Z            1
_cell_length_a                   13.3000(19)
_cell_length_b                   14.938(2)
_cell_length_c                   15.264(2)
_cell_measurement_reflns_used    13284
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.42
_cell_measurement_theta_min      2.28
_cell_volume                     2658.7(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6888
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26114
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.65
_diffrn_reflns_theta_min         1.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.293
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.124
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     630
_refine_ls_number_reflns         14135
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1495P)^2^+0.4276P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1945
_refine_ls_wR_factor_ref         0.2099
_reflns_number_gt                11021
_reflns_number_total             14135
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic070320k-file006.cif
_cod_data_source_block           rl3
_cod_original_formula_sum        'C67.30 H107.20 Cl2.10 N18 O29.20 V14'
_cod_database_code               4308255
loop_
_publ_contact_author
'Dr Eric J. L. McInnes'
'Dr Euan K. Brechin'
loop_
_publ_contact_author_email
eric.mcinnes@manchester.ac.uk
ebrechin@staff.ed.ac.uk
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.47088(4) 0.44855(4) 0.63695(3) 0.03355(13) Uani 1 1 d . A .
V2 V 0.70791(4) 0.42109(4) 0.70377(4) 0.03992(14) Uani 1 1 d . . .
V3 V 0.38363(4) 0.23166(4) 0.68757(4) 0.04337(14) Uani 1 1 d . . .
V4 V 0.28346(4) 0.63088(4) 0.68512(4) 0.04438(15) Uani 1 1 d . . .
V5 V 0.33187(4) 0.40070(4) 0.49225(4) 0.03695(13) Uani 1 1 d . . .
V6 V 0.27824(4) 0.60868(4) 0.49230(4) 0.03595(13) Uani 1 1 d . . .
V7 V 0.44746(4) 0.70780(4) 0.49942(4) 0.03768(13) Uani 1 1 d . . .
O1 O 0.61743(16) 0.46582(15) 0.58756(15) 0.0345(4) Uani 1 1 d . . .
O2 O 0.44165(16) 0.36226(15) 0.57905(15) 0.0352(4) Uani 1 1 d . . .
O3 O 0.38627(15) 0.57960(15) 0.57832(14) 0.0343(4) Uani 1 1 d . A .
O4 O 0.49171(19) 0.17309(18) 0.60170(17) 0.0452(5) Uani 1 1 d . . .
C4 C 0.5056(6) 0.0735(4) 0.6097(5) 0.0947(18) Uani 1 1 d . . .
O5 O 0.28248(19) 0.27616(18) 0.59553(17) 0.0471(5) Uani 1 1 d . B .
C5 C 0.2067(5) 0.2216(5) 0.6013(4) 0.0914(18) Uani 1 1 d . . .
O6 O 0.24788(18) 0.44762(17) 0.38533(17) 0.0433(5) Uani 1 1 d . . .
C6 C 0.1729(5) 0.4078(4) 0.3679(4) 0.0825(15) Uani 1 1 d . . .
O7 O 0.23081(16) 0.47998(16) 0.55910(15) 0.0386(4) Uani 1 1 d . B .
C7 C 0.1209(3) 0.4703(3) 0.5881(3) 0.0520(8) Uani 1 1 d . . .
O8 O 0.19649(18) 0.64259(17) 0.38642(16) 0.0420(5) Uani 1 1 d . . .
C8 C 0.0928(3) 0.6896(4) 0.3729(3) 0.0673(11) Uani 1 1 d . B .
O9 O 0.18591(19) 0.65698(18) 0.59532(16) 0.0450(5) Uani 1 1 d . C .
C9 C 0.0821(4) 0.7087(5) 0.6013(4) 0.0840(16) Uani 1 1 d . . .
O10 O 0.33486(16) 0.73312(15) 0.42714(15) 0.0371(4) Uani 1 1 d . . .
C10 C 0.2680(3) 0.8283(3) 0.3981(3) 0.0517(8) Uani 1 1 d . B .
O11 O 0.34623(19) 0.75233(18) 0.60158(16) 0.0451(5) Uani 1 1 d . C .
C11 C 0.3166(6) 0.8441(4) 0.6122(4) 0.0943(18) Uani 1 1 d . . .
O12 O 0.56095(18) 0.67501(16) 0.57270(16) 0.0395(4) Uani 1 1 d . . .
C12 C 0.5835(3) 0.7425(3) 0.6076(3) 0.0594(9) Uani 1 1 d . B .
N21 N 0.6268(2) 0.29911(19) 0.76295(17) 0.0372(5) Uani 1 1 d . A .
N22 N 0.5371(2) 0.31116(18) 0.73372(18) 0.0372(5) Uani 1 1 d . . .
N23 N 0.5013(2) 0.22596(19) 0.76259(18) 0.0385(5) Uani 1 1 d . A .
C21 C 0.6515(2) 0.2007(2) 0.8150(2) 0.0371(6) Uani 1 1 d . . .
C22 C 0.7373(3) 0.1465(2) 0.8622(2) 0.0414(6) Uani 1 1 d . A .
H22A H 0.7921 0.1782 0.8608 0.050 Uiso 1 1 calc R . .
C23 C 0.7396(3) 0.0467(3) 0.9103(3) 0.0473(7) Uani 1 1 d . . .
C24 C 0.6557(3) -0.0007(3) 0.9133(3) 0.0491(7) Uani 1 1 d . A .
C25 C 0.5732(3) 0.0522(2) 0.8662(2) 0.0439(7) Uani 1 1 d . . .
H25A H 0.5185 0.0205 0.8674 0.053 Uiso 1 1 calc R A .
C26 C 0.5712(2) 0.1539(2) 0.8162(2) 0.0376(6) Uani 1 1 d . A .
C27 C 0.8301(4) -0.0135(3) 0.9632(4) 0.0673(12) Uani 1 1 d . A .
H27A H 0.8850 0.0273 0.9458 0.101 Uiso 1 1 calc R . .
H27B H 0.8586 -0.0713 0.9447 0.101 Uiso 1 1 calc R . .
H27C H 0.8054 -0.0357 1.0334 0.101 Uiso 1 1 calc R . .
C28 C 0.6598(3) -0.1101(3) 0.9707(3) 0.0636(10) Uani 1 1 d . . .
H28A H 0.5934 -0.1300 0.9740 0.095 Uiso 1 1 calc R A .
H28B H 0.6713 -0.1250 1.0365 0.095 Uiso 1 1 calc R . .
H28C H 0.7175 -0.1467 0.9388 0.095 Uiso 1 1 calc R . .
N31 N 0.2927(2) 0.3298(2) 0.75668(18) 0.0408(5) Uani 1 1 d . A .
N32 N 0.3255(2) 0.41569(19) 0.72827(18) 0.0396(5) Uani 1 1 d . . .
N33 N 0.2544(2) 0.4818(2) 0.75637(18) 0.0412(5) Uani 1 1 d . A .
C31 C 0.1943(2) 0.3381(2) 0.8086(2) 0.0426(7) Uani 1 1 d . . .
C32 C 0.1225(3) 0.2722(3) 0.8554(2) 0.0484(7) Uani 1 1 d . A .
H32A H 0.1391 0.2068 0.8553 0.058 Uiso 1 1 calc R . .
C33 C 0.0273(3) 0.3038(3) 0.9016(3) 0.0535(8) Uani 1 1 d . . .
C34 C 0.0024(3) 0.4026(3) 0.9018(3) 0.0555(9) Uani 1 1 d . A .
C35 C 0.0729(3) 0.4684(3) 0.8556(2) 0.0496(8) Uani 1 1 d . . .
H35A H 0.0563 0.5339 0.8554 0.060 Uiso 1 1 calc R A .
C36 C 0.1704(2) 0.4349(3) 0.8088(2) 0.0431(7) Uani 1 1 d . A .
C37 C -0.0529(3) 0.2339(4) 0.9529(4) 0.0709(12) Uani 1 1 d . A .
H37A H -0.0256 0.1711 0.9433 0.106 Uiso 1 1 calc R . .
H37B H -0.1181 0.2638 0.9260 0.106 Uiso 1 1 calc R . .
H37C H -0.0670 0.2218 1.0225 0.106 Uiso 1 1 calc R . .
C38 C -0.1037(3) 0.4358(4) 0.9517(4) 0.0733(12) Uani 1 1 d . . .
H38A H -0.1587 0.4259 0.9254 0.110 Uiso 1 1 calc R A .
H38B H -0.1106 0.5062 0.9406 0.110 Uiso 1 1 calc R . .
H38C H -0.1108 0.3969 1.0216 0.110 Uiso 1 1 calc R . .
N41 N 0.4120(2) 0.5757(2) 0.76152(18) 0.0395(5) Uani 1 1 d . A .
N42 N 0.4860(2) 0.51223(19) 0.73297(18) 0.0379(5) Uani 1 1 d . . .
N43 N 0.5735(2) 0.49459(19) 0.76933(18) 0.0386(5) Uani 1 1 d . A .
C41 C 0.4512(3) 0.5994(2) 0.8227(2) 0.0401(6) Uani 1 1 d . . .
C42 C 0.4073(3) 0.6613(3) 0.8753(2) 0.0442(7) Uani 1 1 d . A .
H42A H 0.3382 0.6968 0.8712 0.053 Uiso 1 1 calc R . .
C43 C 0.4667(3) 0.6690(3) 0.9326(2) 0.0458(7) Uani 1 1 d . . .
C44 C 0.5703(3) 0.6158(2) 0.9395(2) 0.0440(7) Uani 1 1 d . A .
C45 C 0.6136(3) 0.5557(2) 0.8872(2) 0.0418(6) Uani 1 1 d . . .
H45A H 0.6828 0.5202 0.8912 0.050 Uiso 1 1 calc R A .
C46 C 0.5532(3) 0.5483(2) 0.8280(2) 0.0384(6) Uani 1 1 d . A .
C47 C 0.4189(4) 0.7326(3) 0.9926(3) 0.0626(10) Uani 1 1 d . A .
H47A H 0.3493 0.7666 0.9767 0.094 Uiso 1 1 calc R . .
H47B H 0.4640 0.7818 0.9782 0.094 Uiso 1 1 calc R . .
H47C H 0.4123 0.6908 1.0617 0.094 Uiso 1 1 calc R . .
C48 C 0.6332(3) 0.6231(3) 1.0060(3) 0.0542(8) Uani 1 1 d . . .
H48A H 0.6993 0.5771 1.0067 0.081 Uiso 1 1 calc R A .
H48B H 0.5928 0.6061 1.0720 0.081 Uiso 1 1 calc R . .
H48C H 0.6481 0.6909 0.9826 0.081 Uiso 1 1 calc R . .
O2V O 0.7737(3) 0.3871(3) 0.7918(3) 0.0488(8) Uani 0.85 1 d P A 1
Cl2 Cl 0.8156(6) 0.3861(6) 0.7988(6) 0.0486(15) Uani 0.15 1 d P A 2
O3V O 0.3375(4) 0.1335(4) 0.7734(4) 0.0552(12) Uani 0.60 1 d P B 1
Cl3 Cl 0.3251(2) 0.0900(2) 0.7914(2) 0.0551(6) Uani 0.40 1 d P B 2
Cl4 Cl 0.17309(19) 0.69631(19) 0.78935(16) 0.0536(5) Uani 0.50 1 d P C 1
O4V O 0.2022(5) 0.6638(5) 0.7734(5) 0.0535(15) Uani 0.50 1 d P C 2
O1S O 0.8971(16) -0.1637(15) 0.7989(14) 0.106(5) Uiso 0.25 1 d P . .
C1S C 0.9109(16) -0.2562(16) 0.8471(15) 0.074(5) Uiso 0.25 1 d P . .
C2S C 0.745(2) -0.111(2) 0.671(2) 0.146(8) Uiso 0.40 1 d P . .
O2S O 0.826(2) -0.159(2) 0.6307(19) 0.116(7) Uiso 0.20 1 d P D 1
O2S' O 0.668(2) -0.150(2) 0.736(2) 0.118(7) Uiso 0.20 1 d P D 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0332(2) 0.0343(3) 0.0327(2) -0.01069(18) -0.00831(17) -0.00458(18)
V2 0.0356(3) 0.0389(3) 0.0489(3) -0.0171(2) -0.0146(2) -0.0028(2)
V3 0.0387(3) 0.0371(3) 0.0551(3) -0.0143(2) -0.0135(2) -0.0062(2)
V4 0.0398(3) 0.0416(3) 0.0549(3) -0.0216(2) -0.0147(2) 0.0019(2)
V5 0.0337(2) 0.0363(3) 0.0423(3) -0.0121(2) -0.01200(19) -0.00659(19)
V6 0.0310(2) 0.0375(3) 0.0395(3) -0.0136(2) -0.00961(18) -0.00267(19)
V7 0.0384(3) 0.0341(3) 0.0416(3) -0.0139(2) -0.0102(2) -0.0040(2)
O1 0.0328(9) 0.0332(10) 0.0377(9) -0.0117(8) -0.0099(7) -0.0038(7)
O2 0.0326(9) 0.0349(10) 0.0379(10) -0.0110(8) -0.0098(7) -0.0051(8)
O3 0.0321(9) 0.0354(10) 0.0358(9) -0.0128(8) -0.0083(7) -0.0031(8)
O4 0.0434(12) 0.0473(13) 0.0454(12) -0.0148(10) -0.0113(9) -0.0079(10)
C4 0.120(5) 0.057(3) 0.101(4) -0.032(3) 0.008(3) -0.023(3)
O5 0.0461(12) 0.0446(12) 0.0470(12) -0.0118(10) -0.0142(10) -0.0031(10)
C5 0.086(4) 0.092(4) 0.094(4) -0.004(3) -0.034(3) -0.046(3)
O6 0.0410(11) 0.0431(12) 0.0470(12) -0.0152(9) -0.0137(9) -0.0049(9)
C6 0.093(4) 0.086(3) 0.081(3) -0.014(3) -0.039(3) -0.043(3)
O7 0.0291(9) 0.0419(11) 0.0423(11) -0.0117(9) -0.0067(8) -0.0069(8)
C7 0.0331(15) 0.064(2) 0.0563(19) -0.0175(16) -0.0091(13) -0.0102(14)
O8 0.0412(11) 0.0421(12) 0.0449(11) -0.0165(9) -0.0120(9) -0.0043(9)
C8 0.045(2) 0.085(3) 0.074(3) -0.035(2) -0.0187(18) 0.0050(19)
O9 0.0453(12) 0.0473(13) 0.0408(11) -0.0144(9) -0.0100(9) -0.0045(10)
C9 0.048(2) 0.120(4) 0.083(3) -0.047(3) -0.017(2) 0.015(2)
O10 0.0358(10) 0.0355(10) 0.0388(10) -0.0119(8) -0.0121(8) -0.0007(8)
C10 0.0503(19) 0.0436(18) 0.057(2) -0.0170(15) -0.0166(15) 0.0051(14)
O11 0.0439(12) 0.0481(13) 0.0426(11) -0.0150(10) -0.0122(9) -0.0040(10)
C11 0.125(5) 0.075(3) 0.081(3) -0.040(3) 0.007(3) -0.019(3)
O12 0.0414(11) 0.0376(11) 0.0439(11) -0.0156(9) -0.0146(9) -0.0054(8)
C12 0.066(2) 0.054(2) 0.070(2) -0.0291(18) -0.0187(19) -0.0121(18)
N21 0.0393(12) 0.0369(12) 0.0341(11) -0.0105(9) -0.0116(9) -0.0024(10)
N22 0.0398(12) 0.0343(12) 0.0368(11) -0.0098(9) -0.0120(9) -0.0049(10)
N23 0.0398(12) 0.0343(12) 0.0368(12) -0.0075(9) -0.0085(9) -0.0053(10)
C21 0.0416(15) 0.0350(14) 0.0330(12) -0.0117(11) -0.0087(11) -0.0017(11)
C22 0.0429(15) 0.0404(16) 0.0394(14) -0.0129(12) -0.0127(12) -0.0008(12)
C23 0.0450(17) 0.0410(17) 0.0494(17) -0.0096(13) -0.0165(13) 0.0014(13)
C24 0.0522(19) 0.0368(16) 0.0498(17) -0.0083(13) -0.0109(14) -0.0023(13)
C25 0.0431(16) 0.0397(16) 0.0432(15) -0.0091(12) -0.0071(12) -0.0071(12)
C26 0.0371(14) 0.0373(15) 0.0348(13) -0.0126(11) -0.0051(10) -0.0015(11)
C27 0.064(2) 0.045(2) 0.085(3) -0.0049(19) -0.041(2) 0.0021(17)
C28 0.061(2) 0.0360(18) 0.080(3) -0.0035(17) -0.023(2) -0.0031(16)
N31 0.0370(12) 0.0417(14) 0.0379(12) -0.0078(10) -0.0081(9) -0.0060(10)
N32 0.0384(12) 0.0384(13) 0.0390(12) -0.0124(10) -0.0063(10) -0.0037(10)
N33 0.0373(12) 0.0469(15) 0.0351(12) -0.0125(10) -0.0045(9) -0.0046(10)
C31 0.0367(14) 0.0456(17) 0.0371(14) -0.0063(12) -0.0088(11) -0.0046(12)
C32 0.0426(16) 0.0473(18) 0.0451(16) -0.0043(13) -0.0101(13) -0.0087(13)
C33 0.0413(17) 0.061(2) 0.0480(17) -0.0071(15) -0.0075(13) -0.0130(15)
C34 0.0397(17) 0.073(2) 0.0496(18) -0.0198(17) -0.0045(14) -0.0082(16)
C35 0.0421(16) 0.061(2) 0.0432(16) -0.0199(15) -0.0039(13) -0.0060(15)
C36 0.0372(14) 0.0503(18) 0.0368(14) -0.0116(12) -0.0063(11) -0.0052(13)
C37 0.047(2) 0.075(3) 0.074(3) -0.011(2) -0.0011(18) -0.0192(19)
C38 0.045(2) 0.092(3) 0.080(3) -0.036(3) 0.0065(19) -0.016(2)
N41 0.0421(13) 0.0416(14) 0.0354(11) -0.0160(10) -0.0088(10) -0.0019(10)
N42 0.0405(12) 0.0394(13) 0.0355(11) -0.0151(10) -0.0128(9) -0.0002(10)
N43 0.0420(13) 0.0395(13) 0.0366(12) -0.0144(10) -0.0145(10) -0.0020(10)
C41 0.0466(16) 0.0385(15) 0.0347(13) -0.0121(11) -0.0079(11) -0.0068(12)
C42 0.0492(17) 0.0440(17) 0.0388(14) -0.0178(13) -0.0036(12) -0.0054(13)
C43 0.0576(19) 0.0440(17) 0.0396(15) -0.0188(13) -0.0037(13) -0.0128(14)
C44 0.0570(19) 0.0417(16) 0.0368(14) -0.0137(12) -0.0086(13) -0.0145(14)
C45 0.0506(17) 0.0377(15) 0.0386(14) -0.0116(12) -0.0138(12) -0.0076(13)
C46 0.0464(16) 0.0346(14) 0.0347(13) -0.0107(11) -0.0108(11) -0.0069(12)
C47 0.069(3) 0.069(3) 0.065(2) -0.043(2) -0.0057(19) -0.011(2)
C48 0.066(2) 0.057(2) 0.0519(19) -0.0265(16) -0.0141(16) -0.0173(18)
O2V 0.049(2) 0.0515(18) 0.0473(17) -0.0163(13) -0.0157(17) -0.0065(18)
Cl2 0.055(4) 0.046(3) 0.049(3) -0.016(2) -0.022(3) -0.003(3)
O3V 0.054(3) 0.050(3) 0.059(3) -0.012(3) -0.008(2) -0.020(3)
Cl3 0.0523(13) 0.0496(15) 0.0567(13) -0.0074(12) -0.0099(10) -0.0169(12)
Cl4 0.0541(12) 0.0578(13) 0.0456(9) -0.0227(9) -0.0008(8) -0.0038(9)
O4V 0.048(3) 0.058(4) 0.050(3) -0.027(3) -0.002(2) 0.005(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 '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
_geom_angle_publ_flag
O1 V1 O2 106.32(9) . . ?
O1 V1 O3 106.40(9) . . ?
O1 V1 N22 83.01(9) . . ?
O1 V1 N32 164.11(10) . . ?
O1 V1 N42 83.04(10) . . ?
O2 V1 O3 105.37(9) . . ?
O2 V1 N22 82.42(9) . . ?
O2 V1 N32 82.95(10) . . ?
O2 V1 N42 164.89(10) . . ?
O3 V1 N22 165.02(10) . . ?
O3 V1 N32 82.81(9) . . ?
O3 V1 N42 82.62(9) . . ?
N22 V1 N32 85.55(10) . . ?
N22 V1 N42 87.10(10) . . ?
N32 V1 N42 85.42(10) . . ?
O1 V2 O6 77.83(8) . 2_666 ?
O1 V2 O8 78.02(9) . 2_666 ?
O1 V2 N21 82.77(8) . . ?
O1 V2 N43 84.06(9) . . ?
O1 V2 O2V 179.05(16) . . ?
O1 V2 Cl2 170.9(3) . . ?
O6 V2 O8 89.64(10) 2_666 2_666 ?
O6 V2 N21 160.49(9) 2_666 . ?
O6 V2 N43 90.14(10) 2_666 . ?
O6 V2 O2V 102.89(16) 2_666 . ?
O6 V2 Cl2 95.4(2) 2_666 . ?
O8 V2 N21 88.39(10) 2_666 . ?
O8 V2 N43 161.71(9) 2_666 . ?
O8 V2 O2V 102.57(16) 2_666 . ?
O8 V2 Cl2 96.1(2) 2_666 . ?
N21 V2 N43 85.74(10) . . ?
N21 V2 O2V 96.49(16) . . ?
N21 V2 Cl2 104.2(2) . . ?
N43 V2 O2V 95.30(16) . . ?
N43 V2 Cl2 102.1(2) . . ?
O2V V2 Cl2 10.0(3) . . ?
O2 V3 O4 79.18(9) . . ?
O2 V3 O5 79.05(9) . . ?
O2 V3 N23 85.05(9) . . ?
O2 V3 N31 84.68(9) . . ?
O2 V3 O3V 178.0(2) . . ?
O2 V3 Cl3 175.29(10) . . ?
O4 V3 O5 91.30(10) . . ?
O4 V3 N23 89.80(10) . . ?
O4 V3 N31 163.20(10) . . ?
O4 V3 O3V 102.7(2) . . ?
O4 V3 Cl3 96.92(11) . . ?
O5 V3 N23 163.55(10) . . ?
O5 V3 N31 90.20(10) . . ?
O5 V3 O3V 101.5(2) . . ?
O5 V3 Cl3 98.50(11) . . ?
N23 V3 N31 84.13(10) . . ?
N23 V3 O3V 94.3(2) . . ?
N23 V3 Cl3 97.66(10) . . ?
N31 V3 O3V 93.4(2) . . ?
N31 V3 Cl3 99.40(11) . . ?
O3V V3 Cl3 6.6(2) . . ?
V6 V4 V7 57.982(19) . . ?
V6 V4 O3 40.51(5) . . ?
V6 V4 O9 39.29(7) . . ?
V6 V4 O11 85.94(7) . . ?
V6 V4 N33 86.61(7) . . ?
V6 V4 N41 125.33(7) . . ?
V6 V4 Cl4 137.34(6) . . ?
V6 V4 O4V 140.1(2) . . ?
V7 V4 O3 40.80(6) . . ?
V7 V4 O9 85.93(7) . . ?
V7 V4 O11 39.55(7) . . ?
V7 V4 N33 125.40(8) . . ?
V7 V4 N41 86.14(7) . . ?
V7 V4 Cl4 135.65(7) . . ?
V7 V4 O4V 142.6(2) . . ?
O3 V4 O9 79.80(9) . . ?
O3 V4 O11 80.34(9) . . ?
O3 V4 N33 84.93(9) . . ?
O3 V4 N41 85.07(9) . . ?
O3 V4 Cl4 175.76(9) . . ?
O3 V4 O4V 176.4(2) . . ?
O9 V4 O11 92.74(10) . . ?
O9 V4 N33 90.30(10) . . ?
O9 V4 N41 163.93(10) . . ?
O9 V4 Cl4 98.14(10) . . ?
O9 V4 O4V 100.9(2) . . ?
O11 V4 N33 164.18(10) . . ?
O11 V4 N41 90.01(10) . . ?
O11 V4 Cl4 96.11(10) . . ?
O11 V4 O4V 103.1(3) . . ?
N33 V4 N41 82.95(10) . . ?
N33 V4 Cl4 98.82(10) . . ?
N33 V4 O4V 91.6(3) . . ?
N41 V4 Cl4 97.31(9) . . ?
N41 V4 O4V 93.9(2) . . ?
Cl4 V4 O4V 7.7(3) . . ?
V6 V5 V7 120.26(2) . 2_666 ?
V6 V5 O1 42.53(6) . 2_666 ?
V6 V5 O2 92.11(6) . . ?
V6 V5 O5 128.19(8) . . ?
V6 V5 O6 87.42(7) . . ?
V6 V5 O7 39.31(6) . . ?
V6 V5 O12 138.34(7) . 2_666 ?
V7 V5 O1 92.18(6) 2_666 2_666 ?
V7 V5 O2 42.37(6) 2_666 . ?
V7 V5 O5 87.86(7) 2_666 . ?
V7 V5 O6 129.28(7) 2_666 . ?
V7 V5 O7 137.51(6) 2_666 . ?
V7 V5 O12 39.47(6) 2_666 2_666 ?
O1 V5 O2 90.61(8) 2_666 . ?
O1 V5 O5 167.73(9) 2_666 . ?
O1 V5 O6 81.24(9) 2_666 . ?
O1 V5 O7 81.76(9) 2_666 . ?
O1 V5 O12 96.10(9) 2_666 2_666 ?
O2 V5 O5 81.16(9) . . ?
O2 V5 O6 168.46(9) . . ?
O2 V5 O7 95.42(9) . . ?
O2 V5 O12 81.73(9) . 2_666 ?
O5 V5 O6 108.12(10) . . ?
O5 V5 O7 89.93(10) . . ?
O5 V5 O12 91.72(10) . 2_666 ?
O6 V5 O7 91.52(9) . . ?
O6 V5 O12 90.97(9) . 2_666 ?
O7 V5 O12 176.44(9) . 2_666 ?
V4 V6 V5 116.32(2) . . ?
V4 V6 V7 60.973(17) . . ?
V4 V6 O1 132.28(6) . 2_666 ?
V4 V6 O3 42.95(6) . . ?
V4 V6 O7 93.25(7) . . ?
V4 V6 O8 146.19(7) . . ?
V4 V6 O9 38.37(7) . . ?
V4 V6 O10 85.95(6) . . ?
V5 V6 V7 119.69(2) . . ?
V5 V6 O1 42.44(6) . 2_666 ?
V5 V6 O3 91.60(6) . . ?
V5 V6 O7 39.35(7) . . ?
V5 V6 O8 87.32(7) . . ?
V5 V6 O9 128.65(7) . . ?
V5 V6 O10 138.25(7) . . ?
V7 V6 O1 91.58(6) . 2_666 ?
V7 V6 O3 42.44(6) . . ?
V7 V6 O7 137.37(6) . . ?
V7 V6 O8 129.66(7) . . ?
V7 V6 O9 87.85(7) . . ?
V7 V6 O10 39.38(6) . . ?
O1 V6 O3 90.01(8) 2_666 . ?
O1 V6 O7 81.71(9) 2_666 . ?
O1 V6 O8 81.52(9) 2_666 . ?
O1 V6 O9 167.74(9) 2_666 . ?
O1 V6 O10 96.13(9) 2_666 . ?
O3 V6 O7 95.24(9) . . ?
O3 V6 O8 168.58(9) . . ?
O3 V6 O9 81.31(9) . . ?
O3 V6 O10 81.69(8) . . ?
O7 V6 O8 91.12(9) . . ?
O7 V6 O9 90.43(10) . . ?
O7 V6 O10 176.27(9) . . ?
O8 V6 O9 108.16(10) . . ?
O8 V6 O10 91.56(9) . . ?
O9 V6 O10 91.20(9) . . ?
V4 V7 V5 116.09(2) . 2_666 ?
V4 V7 V6 61.046(19) . . ?
V4 V7 O2 132.46(6) . 2_666 ?
V4 V7 O3 43.03(6) . . ?
V4 V7 O4 145.99(7) . 2_666 ?
V4 V7 O10 86.06(7) . . ?
V4 V7 O11 38.70(7) . . ?
V4 V7 O12 93.32(7) . . ?
V5 V7 V6 120.04(2) 2_666 . ?
V5 V7 O2 42.42(6) 2_666 2_666 ?
V5 V7 O3 91.86(6) 2_666 . ?
V5 V7 O4 87.69(7) 2_666 2_666 ?
V5 V7 O10 138.75(7) 2_666 . ?
V5 V7 O11 128.46(7) 2_666 . ?
V5 V7 O12 39.23(7) 2_666 . ?
V6 V7 O2 92.08(6) . 2_666 ?
V6 V7 O3 42.21(6) . . ?
V6 V7 O4 129.31(7) . 2_666 ?
V6 V7 O10 39.46(6) . . ?
V6 V7 O11 87.98(7) . . ?
V6 V7 O12 137.89(7) . . ?
O2 V7 O3 90.25(8) 2_666 . ?
O2 V7 O4 81.53(9) 2_666 2_666 ?
O2 V7 O10 96.66(9) 2_666 . ?
O2 V7 O11 167.97(9) 2_666 . ?
O2 V7 O12 81.53(9) 2_666 . ?
O3 V7 O4 168.30(9) . 2_666 ?
O3 V7 O10 81.53(9) . . ?
O3 V7 O11 81.72(9) . . ?
O3 V7 O12 95.97(9) . . ?
O4 V7 O10 91.11(9) 2_666 . ?
O4 V7 O11 107.64(10) 2_666 . ?
O4 V7 O12 91.07(9) 2_666 . ?
O10 V7 O11 91.03(9) . . ?
O10 V7 O12 176.93(9) . . ?
O11 V7 O12 90.37(9) . . ?
V1 O1 V2 112.28(10) . . ?
V1 O1 V5 124.67(10) . 2_666 ?
V1 O1 V6 125.02(10) . 2_666 ?
V2 O1 V5 96.84(8) . 2_666 ?
V2 O1 V6 96.56(8) . 2_666 ?
V5 O1 V6 95.03(9) 2_666 2_666 ?
V1 O2 V3 112.18(10) . . ?
V1 O2 V5 125.00(11) . . ?
V1 O2 V7 124.46(10) . 2_666 ?
V3 O2 V5 96.97(8) . . ?
V3 O2 V7 96.66(9) . 2_666 ?
V5 O2 V7 95.21(9) . 2_666 ?
V1 O3 V4 112.39(9) . . ?
V1 O3 V6 125.44(10) . . ?
V1 O3 V7 124.32(10) . . ?
V4 O3 V6 96.54(8) . . ?
V4 O3 V7 96.17(9) . . ?
V6 O3 V7 95.35(8) . . ?
V3 O4 V7 102.56(11) . 2_666 ?
V3 O4 C4 124.5(3) . . ?
V7 O4 C4 132.5(3) 2_666 . ?
V3 O5 V5 102.81(11) . . ?
V3 O5 C5 124.7(3) . . ?
V5 O5 C5 132.0(3) . . ?
V2 O6 V5 104.05(10) 2_666 . ?
V2 O6 C6 122.9(3) 2_666 . ?
V5 O6 C6 133.0(3) . . ?
V5 O7 V6 101.34(10) . . ?
V5 O7 C7 122.9(2) . . ?
V6 O7 C7 122.2(2) . . ?
V2 O8 V6 103.81(10) 2_666 . ?
V2 O8 C8 122.5(2) 2_666 . ?
V6 O8 C8 133.3(2) . . ?
V4 O9 V6 102.34(11) . . ?
V4 O9 C9 125.4(3) . . ?
V6 O9 C9 131.8(3) . . ?
V6 O10 V7 101.16(9) . . ?
V6 O10 C10 122.2(2) . . ?
V7 O10 C10 121.5(2) . . ?
V4 O11 V7 101.75(11) . . ?
V4 O11 C11 125.7(3) . . ?
V7 O11 C11 132.4(3) . . ?
V5 O12 V7 101.30(10) 2_666 . ?
V5 O12 C12 123.2(2) 2_666 . ?
V7 O12 C12 122.7(2) . . ?
V2 N21 N22 117.23(18) . . ?
V2 N21 C21 134.7(2) . . ?
N22 N21 C21 107.0(2) . . ?
V1 N22 N21 122.62(19) . . ?
V1 N22 N23 124.72(19) . . ?
N21 N22 N23 112.2(2) . . ?
V3 N23 N22 114.29(18) . . ?
V3 N23 C26 136.6(2) . . ?
N22 N23 C26 106.6(2) . . ?
N21 C21 C22 131.7(3) . . ?
N21 C21 C26 107.3(3) . . ?
C22 C21 C26 121.1(3) . . ?
C21 C22 C23 118.0(3) . . ?
C22 C23 C24 120.8(3) . . ?
C22 C23 C27 119.3(3) . . ?
C24 C23 C27 119.9(3) . . ?
C23 C24 C25 120.9(3) . . ?
C23 C24 C28 118.7(3) . . ?
C25 C24 C28 120.4(3) . . ?
C24 C25 C26 118.4(3) . . ?
N23 C26 C21 106.8(3) . . ?
N23 C26 C25 132.4(3) . . ?
C21 C26 C25 120.8(3) . . ?
V3 N31 N32 115.5(2) . . ?
V3 N31 C31 135.6(2) . . ?
N32 N31 C31 107.0(3) . . ?
V1 N32 N31 123.6(2) . . ?
V1 N32 N33 123.4(2) . . ?
N31 N32 N33 112.8(3) . . ?
V4 N33 N32 115.23(19) . . ?
V4 N33 C36 136.7(2) . . ?
N32 N33 C36 106.1(3) . . ?
N31 C31 C32 132.4(3) . . ?
N31 C31 C36 106.5(3) . . ?
C32 C31 C36 121.1(3) . . ?
C31 C32 C33 118.4(4) . . ?
C32 C33 C34 120.8(3) . . ?
C32 C33 C37 119.7(4) . . ?
C34 C33 C37 119.5(4) . . ?
C33 C34 C35 121.2(3) . . ?
C33 C34 C38 119.5(4) . . ?
C35 C34 C38 119.2(4) . . ?
C34 C35 C36 117.4(4) . . ?
N33 C36 C31 107.6(3) . . ?
N33 C36 C35 131.3(3) . . ?
C31 C36 C35 121.1(3) . . ?
V4 N41 N42 114.95(18) . . ?
V4 N41 C41 137.2(2) . . ?
N42 N41 C41 106.6(3) . . ?
V1 N42 N41 124.24(19) . . ?
V1 N42 N43 123.2(2) . . ?
N41 N42 N43 112.6(2) . . ?
V2 N43 N42 115.55(19) . . ?
V2 N43 C46 136.8(2) . . ?
N42 N43 C46 106.2(2) . . ?
N41 C41 C42 131.7(3) . . ?
N41 C41 C46 107.6(3) . . ?
C42 C41 C46 120.7(3) . . ?
C41 C42 C43 118.1(3) . . ?
C42 C43 C44 121.5(3) . . ?
C42 C43 C47 118.6(3) . . ?
C44 C43 C47 119.9(3) . . ?
C43 C44 C45 120.4(3) . . ?
C43 C44 C48 120.4(3) . . ?
C45 C44 C48 119.2(3) . . ?
C44 C45 C46 118.2(3) . . ?
N43 C46 C41 107.0(3) . . ?
N43 C46 C45 131.8(3) . . ?
C41 C46 C45 121.2(3) . . ?
O2S C2S O2S' 126(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.950(2) . ?
V1 O2 1.979(2) . ?
V1 O3 1.984(2) . ?
V1 N22 2.121(2) . ?
V1 N32 2.124(3) . ?
V1 N42 2.110(2) . ?
V2 O1 2.177(2) . ?
V2 O6 2.010(2) 2_666 ?
V2 O8 2.015(2) 2_666 ?
V2 N21 2.103(3) . ?
V2 N43 2.122(3) . ?
V2 O2V 1.625(4) . ?
V2 Cl2 2.115(7) . ?
V3 O2 2.150(2) . ?
V3 O4 1.993(3) . ?
V3 O5 1.991(2) . ?
V3 N23 2.120(3) . ?
V3 N31 2.127(3) . ?
V3 O3V 1.651(5) . ?
V3 Cl3 2.250(3) . ?
V4 V6 3.1106(8) . ?
V4 V7 3.1084(8) . ?
V4 O3 2.133(2) . ?
V4 O9 1.976(2) . ?
V4 O11 1.985(2) . ?
V4 N33 2.129(3) . ?
V4 N41 2.118(3) . ?
V4 Cl4 2.256(2) . ?
V4 O4V 1.676(6) . ?
V5 V6 3.0201(8) . ?
V5 V7 3.0056(8) 2_666 ?
V5 O1 2.046(2) 2_666 ?
V5 O2 2.036(2) . ?
V5 O5 2.020(2) . ?
V5 O6 1.998(2) . ?
V5 O7 1.953(2) . ?
V5 O12 1.938(2) 2_666 ?
V6 V7 3.0142(8) . ?
V6 O1 2.050(2) 2_666 ?
V6 O3 2.034(2) . ?
V6 O7 1.951(2) . ?
V6 O8 1.995(2) . ?
V6 O9 2.016(2) . ?
V6 O10 1.952(2) . ?
V7 V5 3.0056(8) 2_666 ?
V7 O2 2.034(2) 2_666 ?
V7 O3 2.043(2) . ?
V7 O4 2.013(2) 2_666 ?
V7 O10 1.949(2) . ?
V7 O11 2.022(2) . ?
V7 O12 1.949(2) . ?
O1 V5 2.046(2) 2_666 ?
O1 V6 2.050(2) 2_666 ?
O2 V7 2.034(2) 2_666 ?
O4 V7 2.013(2) 2_666 ?
O4 C4 1.414(6) . ?
O5 C5 1.404(5) . ?
O6 V2 2.010(2) 2_666 ?
O6 C6 1.398(5) . ?
O7 C7 1.445(4) . ?
O8 V2 2.014(2) 2_666 ?
O8 C8 1.415(4) . ?
O9 C9 1.416(5) . ?
O10 C10 1.448(4) . ?
O11 C11 1.398(6) . ?
O12 V5 1.938(2) 2_666 ?
O12 C12 1.429(4) . ?
N21 N22 1.321(3) . ?
N21 C21 1.362(4) . ?
N22 N23 1.331(4) . ?
N23 C26 1.370(4) . ?
C21 C22 1.403(4) . ?
C21 C26 1.400(4) . ?
C22 C23 1.365(5) . ?
C23 C24 1.440(5) . ?
C23 C27 1.512(5) . ?
C24 C25 1.363(5) . ?
C24 C28 1.505(5) . ?
C25 C26 1.395(4) . ?
N31 N32 1.321(4) . ?
N31 C31 1.363(4) . ?
N32 N33 1.327(4) . ?
N33 C36 1.365(4) . ?
C31 C32 1.391(5) . ?
C31 C36 1.406(5) . ?
C32 C33 1.371(5) . ?
C33 C34 1.435(6) . ?
C33 C37 1.517(5) . ?
C34 C35 1.377(5) . ?
C34 C38 1.508(5) . ?
C35 C36 1.406(5) . ?
N41 N42 1.320(4) . ?
N41 C41 1.363(4) . ?
N42 N43 1.335(3) . ?
N43 C46 1.372(4) . ?
C41 C42 1.400(4) . ?
C41 C46 1.395(4) . ?
C42 C43 1.364(5) . ?
C43 C44 1.425(5) . ?
C43 C47 1.511(5) . ?
C44 C45 1.374(5) . ?
C44 C48 1.512(5) . ?
C45 C46 1.395(4) . ?
O1S C1S 1.27(3) . ?
C2S O2S 1.32(3) . ?
C2S O2S' 1.31(3) . ?
#BEGIN Loops that were not found in dictionaries:
loop_
_publ_author
'Eric J. L. McInnes'
'Euan K. Brechin'
'Rachel S. Shaw'
'Rebecca H. Laye'
'Leigh F. Jones'
'David M. Low'
'Caytie Talbot-Eeckelaers'
'Qiang Wei'
'Constantinos J. Milios'
'Simon Teat'
'Marco Evangelisti'
'Marco Affronte'
'David Collison'
'Madeilene Helliwell'
'James Raftery'
#END Loops that were not found in dictionaries