#------------------------------------------------------------------------------
#$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $
#$Revision: 14 $
#$URL: svn://www.crystallography.net/cod/cif/5/5000309.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_5000309
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_formula_moiety          ?
_chemical_formula_structural      ?
_chemical_formula_analytical      ?
_chemical_formula_sum             'C43 H55 Cl5 N4 O20 V4'
_chemical_formula_weight          1328.92
_chemical_melting_point           ?
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device        ?
_diffrn_measurement_method        ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             12313
_diffrn_reflns_av_R_equivalents   0.0400
_diffrn_reflns_av_sigmaI/netI     0.0701
_diffrn_reflns_limit_h_min        -14
_diffrn_reflns_limit_h_max        7
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_k_max        14
_diffrn_reflns_limit_l_min        -17
_diffrn_reflns_limit_l_max        17
_diffrn_reflns_theta_min          3.07
_diffrn_reflns_theta_max          22.50
_reflns_number_total              7256
_reflns_number_observed           5730
_reflns_observed_criterion        >2sigma(I)
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme
; calc
 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0400P)^2^+0.0000sin\q/\l]
 where P = 1.00000Fo^2^ + 0.00000Fc^2^
;
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     ?
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.0012(6)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns          7249
_refine_ls_number_parameters      906
_refine_ls_number_restraints      456
_refine_ls_R_factor_all           0.0905
_refine_ls_R_factor_obs           0.0716
_refine_ls_wR_factor_all          0.1719
_refine_ls_wR_factor_obs          0.1649
_refine_ls_goodness_of_fit_all    1.858
_refine_ls_goodness_of_fit_obs    2.059
_refine_ls_restrained_S_all       1.827
_refine_ls_restrained_S_obs       1.989
_refine_ls_shift/esd_max          -0.957
_refine_ls_shift/esd_mean         0.046
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_thermal_displace_type
 _atom_site_occupancy
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_group
V1 V 0.41758(9) 0.30533(8) 0.69063(7) 0.0125(3) Uani 1 d U .
V2 V 0.58057(9) 0.29032(8) 0.83016(7) 0.0127(3) Uani 1 d U .
V3 V 0.34478(9) 0.21497(8) 0.86994(7) 0.0127(3) Uani 1 d U .
V4 V 0.65218(9) 0.19676(8) 0.65458(7) 0.0133(3) Uani 1 d U .
O5 O 0.4310(3) 0.2864(3) 0.8124(3) 0.0108(11) Uani 1 d U .
O6 O 0.5660(3) 0.2780(3) 0.7089(3) 0.0116(11) Uani 1 d U .
O7 O 0.4435(3) 0.4558(3) 0.6990(3) 0.0134(11) Uani 1 d U .
O8 O 0.5579(4) 0.4426(3) 0.8158(3) 0.0153(11) Uani 1 d U .
C9 C 0.5014(6) 0.4941(5) 0.7564(4) 0.016(2) Uani 1 d U .
C10 C 0.5090(7) 0.6054(6) 0.7582(5) 0.022(2) Uani 1 d U .
C11 C 0.4318(7) 0.6692(6) 0.6963(5) 0.025(2) Uani 1 d U .
O12 O 0.2693(4) 0.3419(3) 0.6762(3) 0.0148(11) Uani 1 d U .
O13 O 0.2177(4) 0.2583(3) 0.7875(3) 0.0179(11) Uani 1 d U .
C14 C 0.2011(6) 0.3090(5) 0.7170(4) 0.015(2) Uani 1 d U .
C15 C 0.0921(7) 0.3269(6) 0.6774(6) 0.027(2) Uani 1 d U .
C16 C 0.0512(10) 0.2347(10) 0.6415(8) 0.053(3) Uani 1 d U .
O17 O 0.3826(3) 0.1547(3) 0.6815(3) 0.0142(11) Uani 1 d U .
O18 O 0.3594(4) 0.0880(3) 0.8101(3) 0.0169(11) Uani 1 d U .
C19 C 0.3669(5) 0.0816(5) 0.7305(4) 0.015(2) Uani 1 d U .
C20 C 0.3557(7) -0.0197(6) 0.6965(5) 0.019(2) Uani 1 d U .
C21 C 0.3874(7) -0.0323(6) 0.6089(5) 0.020(2) Uani 1 d U .
O22 O 0.4267(4) 0.2985(3) 0.5661(3) 0.0150(11) Uani 1 d U .
O23 O 0.5405(4) 0.1694(3) 0.5598(3) 0.0160(11) Uani 1 d U .
C24 C 0.4614(6) 0.2214(5) 0.5309(4) 0.014(2) Uani 1 d U .
C25 C 0.4032(6) 0.1912(6) 0.4498(5) 0.021(2) Uani 1 d U .
C26 C 0.3060(8) 0.2525(8) 0.4215(7) 0.041(3) Uani 1 d U .
O27 O 0.5711(3) 0.2821(3) 0.9561(3) 0.0142(11) Uani 1 d U .
O28 O 0.4552(4) 0.1690(3) 0.9669(3) 0.0165(11) Uani 1 d U .
C29 C 0.5352(6) 0.2096(5) 0.9940(4) 0.014(2) Uani 1 d U .
C30 C 0.5887(6) 0.1728(6) 1.0801(5) 0.020(2) Uani 1 d U .
C31 C 0.6862(7) 0.2211(7) 1.1074(6) 0.029(2) Uani 1 d U .
O32 O 0.7296(4) 0.3070(3) 0.8436(3) 0.0175(11) Uani 1 d U .
O33 O 0.7783(3) 0.2182(3) 0.7363(3) 0.0155(11) Uani 1 d U .
C34 C 0.7963(6) 0.2620(5) 0.8048(5) 0.018(2) Uani 1 d U .
C35 C 0.9049(7) 0.2574(8) 0.8444(6) 0.032(2) Uani 1 d U .
C36 C 0.9198(8) 0.2931(7) 0.9346(6) 0.037(2) Uani 1 d U .
O37 O 0.6131(3) 0.1369(3) 0.8467(3) 0.0145(11) Uani 1 d U .
O38 O 0.6328(4) 0.0702(3) 0.7215(3) 0.0179(12) Uani 1 d U .
C39 C 0.6215(5) 0.0637(5) 0.8008(4) 0.016(2) Uani 1 d U .
C40 C 0.6186(7) -0.0400(5) 0.8418(5) 0.020(2) Uani 1 d U .
C41 C 0.6418(7) -0.1273(6) 0.7879(5) 0.021(2) Uani 1 d U .
N42 N 0.3056(4) 0.3256(4) 0.9554(3) 0.0139(13) Uani 1 d U .
C43 C 0.3456(6) 0.4148(5) 0.9583(5) 0.018(2) Uani 1 d U .
C44 C 0.3289(6) 0.4839(6) 1.0178(5) 0.017(2) Uani 1 d U .
C45 C 0.2635(6) 0.4581(5) 1.0785(5) 0.022(2) Uani 1 d U .
C46 C 0.2229(6) 0.3673(5) 1.0749(5) 0.019(2) Uani 1 d U .
C47 C 0.2442(6) 0.3001(5) 1.0142(4) 0.017(2) Uani 1 d U .
C48 C 0.2057(5) 0.1987(5) 1.0075(4) 0.013(2) Uani 1 d U .
C49 C 0.1417(6) 0.1568(5) 1.0615(5) 0.019(2) Uani 1 d U .
C50 C 0.1123(6) 0.0608(6) 1.0502(5) 0.024(2) Uani 1 d U .
C51 C 0.1438(6) 0.0067(6) 0.9851(5) 0.022(2) Uani 1 d U .
C52 C 0.2071(6) 0.0517(5) 0.9334(5) 0.018(2) Uani 1 d U .
N53 N 0.2388(4) 0.1436(4) 0.9441(3) 0.0143(14) Uani 1 d U .
N54 N 0.7584(4) 0.1165(4) 0.5846(3) 0.0143(14) Uani 1 d U .
C55 C 0.7878(6) 0.0187(6) 0.5976(5) 0.019(2) Uani 1 d U .
C56 C 0.8489(6) -0.0326(6) 0.5450(5) 0.022(2) Uani 1 d U .
C57 C 0.8788(6) 0.0202(6) 0.4775(5) 0.023(2) Uani 1 d U .
C58 C 0.8523(6) 0.1212(6) 0.4659(5) 0.021(2) Uani 1 d U .
C59 C 0.7911(6) 0.1699(5) 0.5197(4) 0.017(2) Uani 1 d U .
C60 C 0.7583(5) 0.2772(5) 0.5115(4) 0.015(2) Uani 1 d U .
C61 C 0.7880(6) 0.3451(6) 0.4515(5) 0.022(2) Uani 1 d U .
C62 C 0.7472(6) 0.4434(6) 0.4459(5) 0.026(2) Uani 1 d U .
C63 C 0.6785(6) 0.4737(6) 0.5007(5) 0.020(2) Uani 1 d U .
C64 C 0.6543(6) 0.4022(5) 0.5593(5) 0.019(2) Uani 1 d U .
N65 N 0.6915(4) 0.3073(4) 0.5663(3) 0.0138(13) Uani 1 d U .
Cl66 Cl 0.9792(2) 0.14925(14) 0.25133(11) 0.0249(5) Uani 1 d U .
O67 O 1.0872(4) 0.1596(4) 0.2628(3) 0.0354(14) Uani 1 d U .
O68 O 0.9295(4) 0.2306(4) 0.2920(3) 0.0329(14) Uani 1 d U .
O69 O 0.9449(4) 0.1562(4) 0.1615(3) 0.0338(14) Uani 1 d U .
O70 O 0.9566(5) 0.0547(4) 0.2871(4) 0.045(2) Uani 1 d U .
Cl71 Cl 1.0584(2) 0.4178(2) 0.43015(14) 0.0466(6) Uani 1 d U .
Cl72 Cl 1.1684(2) 0.4900(2) 0.29319(14) 0.0477(7) Uani 1 d U .
C73 C 1.0777(7) 0.4077(7) 0.3217(5) 0.035(2) Uani 1 d U .
Cl74 Cl 0.2069(2) 0.54065(15) 0.78603(12) 0.0307(5) Uani 1 d U .
Cl75 Cl 0.0439(2) 0.5189(2) 0.89190(14) 0.0453(6) Uani 1 d U .
C76 C 0.1391(7) 0.5964(6) 0.8637(5) 0.028(2) Uani 1 d U .
H77 H 0.5088(45) 0.6262(41) 0.8099(42) 0.002(16) Uiso 1 d . .
H78 H 0.5763(68) 0.6133(55) 0.7419(52) 0.040(25) Uiso 1 d . .
H79 H 0.4410(51) 0.7426(52) 0.6971(42) 0.017(18) Uiso 1 d . .
H80 H 0.3615(74) 0.6526(60) 0.7049(56) 0.050(28) Uiso 1 d . .
H81 H 0.4363(52) 0.6564(47) 0.6377(48) 0.019(19) Uiso 1 d . .
H82 H 0.0895(54) 0.3863(53) 0.6446(47) 0.023(20) Uiso 1 d . .
H83 H 0.0560(58) 0.3448(51) 0.7173(49) 0.024(22) Uiso 1 d . .
H84 H 0.0550(58) 0.1745(58) 0.6679(48) 0.022(23) Uiso 1 d . .
H85 H -0.0190(79) 0.2559(62) 0.6238(59) 0.055(29) Uiso 1 d . .
H86 H 0.0846(72) 0.2176(65) 0.5977(62) 0.052(31) Uiso 1 d . .
H87 H 0.3816(67) -0.0656(61) 0.7318(57) 0.047(28) Uiso 1 d . .
H88 H 0.2755(60) -0.0339(49) 0.6976(45) 0.028(20) Uiso 1 d . .
H89 H 0.3404(51) 0.0257(46) 0.5639(42) 0.015(17) Uiso 1 d . .
H90 H 0.3836(54) -0.1015(55) 0.5911(45) 0.027(21) Uiso 1 d . .
H91 H 0.4561(67) -0.0144(55) 0.6110(50) 0.037(25) Uiso 1 d . .
H92 H 0.3918(43) 0.1152(42) 0.4566(35) 0.000(15) Uiso 1 d . .
H93 H 0.4580(62) 0.1893(53) 0.4068(50) 0.039(23) Uiso 1 d . .
H94 H 0.3149(77) 0.3148(77) 0.4024(66) 0.055(36) Uiso 1 d . .
H95 H 0.2726(54) 0.2161(49) 0.3803(47) 0.020(19) Uiso 1 d . .
H96 H 0.2633(72) 0.2468(63) 0.4646(63) 0.054(31) Uiso 1 d . .
H97 H 0.5992(49) 0.1068(50) 1.0729(41) 0.013(18) Uiso 1 d . .
H98 H 0.5336(55) 0.1846(46) 1.1174(44) 0.019(19) Uiso 1 d . .
H99 H 0.6804(57) 0.2938(60) 1.1100(48) 0.029(22) Uiso 1 d . .
H100 H 0.7198(64) 0.1751(59) 1.1550(56) 0.044(25) Uiso 1 d . .
H101 H 0.7239(90) 0.2204(83) 1.0713(78) 0.089(46) Uiso 1 d . .
H102 H 0.9482(51) 0.1949(47) 0.8355(39) 0.012(17) Uiso 1 d . .
H103 H 0.9152(56) 0.2971(51) 0.8203(47) 0.003(23) Uiso 1 d . .
H104 H 0.8894(76) 0.3714(72) 0.9514(62) 0.076(32) Uiso 1 d . .
H105 H 0.8925(130) 0.2098(124) 0.9742(107) 0.190(69) Uiso 1 d . .
H106 H 0.9964(83) 0.2878(67) 0.9481(62) 0.073(32) Uiso 1 d . .
H107 H 0.6608(56) -0.0373(48) 0.8820(47) 0.016(21) Uiso 1 d . .
H108 H 0.5460(67) -0.0404(55) 0.8601(51) 0.044(25) Uiso 1 d . .
H109 H 0.6340(48) -0.1942(47) 0.8175(41) 0.010(17) Uiso 1 d . .
H110 H 0.7114(58) -0.1318(46) 0.7738(43) 0.016(19) Uiso 1 d . .
H111 H 0.6058(59) -0.1256(52) 0.7308(53) 0.033(22) Uiso 1 d . .
H112 H 0.3857(48) 0.4265(43) 0.9248(40) 0.000(17) Uiso 1 d . .
H113 H 0.3547(46) 0.5396(44) 1.0191(37) 0.000(16) Uiso 1 d . .
H114 H 0.2539(51) 0.5176(48) 1.1224(44) 0.024(19) Uiso 1 d . .
H115 H 0.1796(49) 0.3450(42) 1.1119(40) 0.004(16) Uiso 1 d . .
H116 H 0.1249(45) 0.1990(41) 1.1040(39) 0.001(15) Uiso 1 d . .
H117 H 0.0781(51) 0.0284(46) 1.0824(42) 0.009(18) Uiso 1 d . .
H118 H 0.1280(50) -0.0512(49) 0.9743(42) 0.012(19) Uiso 1 d . .
H119 H 0.2307(53) 0.0173(47) 0.8885(46) 0.019(19) Uiso 1 d . .
H120 H 0.7698(46) -0.0177(42) 0.6361(40) 0.000(16) Uiso 1 d . .
H121 H 0.8665(44) -0.1042(43) 0.5549(36) 0.000(15) Uiso 1 d . .
H122 H 0.9244(68) -0.0160(61) 0.4417(57) 0.058(28) Uiso 1 d . .
H123 H 0.8612(53) 0.1622(49) 0.4316(45) 0.014(21) Uiso 1 d . .
H124 H 0.8348(60) 0.3239(52) 0.4214(48) 0.028(22) Uiso 1 d . .
H125 H 0.7616(69) 0.4992(65) 0.4166(58) 0.059(30) Uiso 1 d . .
H126 H 0.6466(51) 0.5391(49) 0.5022(41) 0.015(18) Uiso 1 d . .
H127 H 0.6025(47) 0.4133(41) 0.6024(39) 0.007(16) Uiso 1 d . .
H128 H 1.0996(60) 0.3395(58) 0.3188(48) 0.034(22) Uiso 1 d . .
H129 H 0.9992(71) 0.4342(61) 0.2881(56) 0.058(27) Uiso 1 d . .
H130 H 0.1136(61) 0.6648(59) 0.8447(50) 0.037(23) Uiso 1 d . .
H131 H 0.1843(69) 0.6167(60) 0.9107(58) 0.053(27) Uiso 1 d . .
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 0.0102(8) 0.0232(6) 0.0044(6) -0.0012(5) 0.0033(5) 0.0010(5)
V2 0.0097(7) 0.0237(7) 0.0052(6) -0.0003(5) 0.0035(5) -0.0013(5)
V3 0.0110(8) 0.0235(7) 0.0046(6) -0.0019(5) 0.0046(5) -0.0023(5)
V4 0.0104(8) 0.0240(7) 0.0062(6) 0.0005(5) 0.0045(5) 0.0005(5)
O5 0.010(3) 0.019(2) 0.005(2) -0.001(2) 0.004(2) -0.001(2)
O6 0.009(3) 0.021(2) 0.006(2) 0.000(2) 0.007(2) 0.000(2)
O7 0.010(3) 0.023(2) 0.007(2) -0.001(2) 0.001(2) 0.001(2)
O8 0.014(3) 0.022(2) 0.011(2) -0.003(2) 0.003(2) -0.001(2)
C9 0.013(4) 0.025(3) 0.010(3) 0.000(3) 0.009(3) 0.003(3)
C10 0.021(4) 0.027(3) 0.019(4) -0.001(3) 0.001(3) -0.003(3)
C11 0.026(5) 0.028(4) 0.020(4) -0.001(3) -0.001(4) 0.000(4)
O12 0.010(3) 0.026(2) 0.009(2) 0.001(2) 0.003(2) 0.001(2)
O13 0.014(3) 0.031(2) 0.010(2) 0.000(2) 0.004(2) -0.001(2)
C14 0.015(4) 0.021(3) 0.012(3) -0.002(3) 0.005(3) -0.001(3)
C15 0.021(4) 0.034(4) 0.024(4) 0.005(3) 0.003(3) 0.003(3)
C16 0.034(6) 0.069(7) 0.051(6) -0.006(5) -0.012(5) -0.006(5)
O17 0.011(3) 0.021(2) 0.011(2) -0.001(2) 0.002(2) 0.000(2)
O18 0.016(3) 0.025(2) 0.010(2) -0.006(2) 0.003(2) 0.000(2)
C19 0.008(3) 0.024(3) 0.012(3) -0.003(3) -0.001(3) 0.003(3)
C20 0.022(4) 0.021(3) 0.015(3) -0.004(3) 0.002(3) -0.001(3)
C21 0.020(5) 0.024(4) 0.016(4) -0.006(3) 0.007(3) 0.000(4)
O22 0.015(3) 0.023(2) 0.007(2) 0.000(2) 0.003(2) 0.000(2)
O23 0.009(3) 0.031(2) 0.009(2) -0.001(2) 0.005(2) -0.003(2)
C24 0.015(4) 0.019(3) 0.011(3) 0.001(3) 0.008(3) -0.004(3)
C25 0.017(4) 0.025(3) 0.021(3) -0.005(3) 0.004(3) 0.001(3)
C26 0.035(6) 0.051(6) 0.033(5) -0.017(5) -0.014(5) 0.009(5)
O27 0.013(3) 0.021(2) 0.009(2) -0.001(2) 0.004(2) -0.002(2)
O28 0.014(3) 0.024(2) 0.011(2) -0.005(2) 0.000(2) 0.005(2)
C29 0.013(4) 0.013(3) 0.015(3) 0.000(3) 0.005(3) 0.005(3)
C30 0.018(4) 0.023(3) 0.019(3) 0.003(3) 0.003(3) -0.002(3)
C31 0.021(5) 0.042(5) 0.023(5) 0.011(4) -0.001(4) -0.006(4)
O32 0.010(3) 0.027(2) 0.015(2) -0.002(2) 0.002(2) 0.000(2)
O33 0.009(3) 0.030(2) 0.008(2) 0.000(2) 0.004(2) -0.001(2)
C34 0.015(4) 0.022(3) 0.018(3) 0.002(3) 0.002(3) -0.002(3)
C35 0.024(4) 0.043(4) 0.028(4) 0.002(4) 0.002(3) -0.001(4)
C36 0.026(5) 0.051(5) 0.032(5) -0.012(4) -0.007(4) -0.003(4)
O37 0.012(3) 0.020(2) 0.012(2) -0.005(2) 0.003(2) -0.001(2)
O38 0.021(3) 0.025(2) 0.009(2) 0.000(2) 0.005(2) 0.002(2)
C39 0.007(3) 0.026(3) 0.015(3) -0.002(3) 0.003(3) -0.003(3)
C40 0.016(4) 0.028(3) 0.016(3) 0.001(3) 0.001(3) -0.002(3)
C41 0.025(5) 0.027(4) 0.012(4) -0.002(3) -0.001(4) 0.000(4)
N42 0.012(3) 0.020(3) 0.008(3) 0.000(2) 0.000(2) 0.004(2)
C43 0.018(4) 0.025(3) 0.012(3) 0.004(3) 0.003(3) 0.000(3)
C44 0.017(4) 0.018(3) 0.015(3) -0.002(3) -0.002(3) -0.001(3)
C45 0.023(4) 0.026(3) 0.016(3) -0.003(3) 0.000(3) 0.001(3)
C46 0.014(4) 0.029(3) 0.014(3) 0.001(3) 0.005(3) 0.001(3)
C47 0.013(4) 0.024(3) 0.014(3) 0.004(3) 0.002(3) 0.001(3)
C48 0.013(4) 0.021(3) 0.006(3) 0.002(3) 0.001(3) 0.001(3)
C49 0.015(4) 0.027(3) 0.016(3) -0.005(3) 0.003(3) 0.004(3)
C50 0.021(4) 0.030(4) 0.023(4) 0.003(3) 0.008(3) -0.007(3)
C51 0.024(4) 0.024(3) 0.021(4) -0.003(3) 0.005(3) -0.005(3)
C52 0.015(4) 0.027(3) 0.013(3) -0.006(3) 0.007(3) 0.000(3)
N53 0.010(3) 0.024(3) 0.009(3) -0.003(2) 0.003(2) 0.001(2)
N54 0.011(3) 0.023(3) 0.008(3) 0.003(2) 0.003(2) 0.000(2)
C55 0.018(4) 0.030(4) 0.011(3) 0.001(3) 0.005(3) -0.001(3)
C56 0.020(4) 0.026(3) 0.020(3) -0.002(3) 0.004(3) 0.003(3)
C57 0.019(4) 0.030(3) 0.017(3) 0.001(3) 0.002(3) 0.005(3)
C58 0.018(4) 0.030(4) 0.015(3) 0.000(3) 0.006(3) -0.003(3)
C59 0.014(4) 0.029(3) 0.007(3) 0.000(3) 0.004(3) -0.003(3)
C60 0.011(3) 0.025(3) 0.009(3) 0.001(3) -0.003(3) -0.005(3)
C61 0.019(4) 0.032(4) 0.017(3) -0.001(3) 0.005(3) -0.001(3)
C62 0.028(4) 0.030(4) 0.020(3) 0.003(3) -0.002(3) -0.011(3)
C63 0.019(4) 0.025(3) 0.016(3) 0.002(3) -0.003(3) -0.002(3)
C64 0.018(4) 0.026(3) 0.012(3) 0.001(3) -0.003(3) -0.004(3)
N65 0.012(3) 0.023(3) 0.008(3) -0.001(2) 0.005(2) -0.003(2)
Cl66 0.0256(13) 0.0346(11) 0.0156(10) 0.0009(8) 0.0098(9) 0.0030(9)
O67 0.019(3) 0.061(4) 0.025(3) 0.002(3) 0.001(3) 0.005(3)
O68 0.047(4) 0.033(3) 0.020(3) -0.001(2) 0.016(3) 0.003(3)
O69 0.026(4) 0.057(3) 0.017(3) -0.011(3) -0.001(2) 0.007(3)
O70 0.055(4) 0.039(3) 0.042(4) 0.005(3) 0.018(3) 0.001(3)
Cl71 0.0340(15) 0.084(2) 0.0234(12) -0.0074(11) 0.0079(10) -0.0035(12)
Cl72 0.041(2) 0.070(2) 0.0311(13) 0.0064(11) -0.0038(11) -0.0201(12)
C73 0.036(4) 0.043(4) 0.028(4) -0.004(3) 0.007(3) -0.005(3)
Cl74 0.0310(14) 0.0425(12) 0.0196(11) -0.0043(9) 0.0079(9) 0.0009(9)
Cl75 0.035(2) 0.076(2) 0.0275(12) 0.0023(11) 0.0080(10) -0.0230(12)
C76 0.027(4) 0.032(4) 0.025(4) -0.002(3) 0.003(3) -0.003(3)
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 O5 1.928(4) . ?
V1 O6 1.972(5) . ?
V1 O12 1.988(5) . ?
V1 O22 2.004(4) . ?
V1 O7 2.053(4) . ?
V1 O17 2.085(4) . ?
V1 V2 2.909(2) . ?
V2 O6 1.931(4) . ?
V2 O5 1.981(5) . ?
V2 O32 1.995(5) . ?
V2 O27 2.019(5) . ?
V2 O8 2.024(4) . ?
V2 O37 2.055(4) . ?
V3 O5 1.830(4) . ?
V3 O18 1.981(4) . ?
V3 O28 2.049(5) . ?
V3 O13 2.053(5) . ?
V3 N42 2.126(5) . ?
V3 N53 2.173(6) . ?
V4 O6 1.841(4) . ?
V4 O38 1.993(5) . ?
V4 O33 2.042(5) . ?
V4 O23 2.050(5) . ?
V4 N65 2.116(6) . ?
V4 N54 2.159(6) . ?
O7 C9 1.267(8) . ?
O8 C9 1.283(8) . ?
C9 C10 1.487(10) . ?
C10 C11 1.528(11) . ?
O12 C14 1.263(8) . ?
O13 C14 1.273(8) . ?
C14 C15 1.513(11) . ?
C15 C16 1.478(14) . ?
O17 C19 1.259(8) . ?
O18 C19 1.288(8) . ?
C19 C20 1.480(9) . ?
C20 C21 1.516(10) . ?
O22 C24 1.276(8) . ?
O23 C24 1.253(8) . ?
C24 C25 1.508(10) . ?
C25 C26 1.500(12) . ?
O27 C29 1.260(8) . ?
O28 C29 1.261(8) . ?
C29 C30 1.515(10) . ?
C30 C31 1.507(12) . ?
O32 C34 1.274(8) . ?
O33 C34 1.262(8) . ?
C34 C35 1.504(11) . ?
C35 C36 1.526(12) . ?
O37 C39 1.247(8) . ?
O38 C39 1.288(8) . ?
C39 C40 1.501(10) . ?
C40 C41 1.509(11) . ?
N42 C43 1.326(9) . ?
N42 C47 1.356(9) . ?
C43 C44 1.373(10) . ?
C44 C45 1.418(11) . ?
C45 C46 1.348(10) . ?
C46 C47 1.384(10) . ?
C47 C48 1.470(9) . ?
C48 N53 1.368(8) . ?
C48 C49 1.399(10) . ?
C49 C50 1.366(10) . ?
C50 C51 1.376(11) . ?
C51 C52 1.385(11) . ?
C52 N53 1.325(9) . ?
N54 C55 1.333(9) . ?
N54 C59 1.354(9) . ?
C55 C56 1.402(10) . ?
C56 C57 1.366(11) . ?
C57 C58 1.365(11) . ?
C58 C59 1.400(10) . ?
C59 C60 1.460(10) . ?
C60 N65 1.371(9) . ?
C60 C61 1.389(10) . ?
C61 C62 1.377(11) . ?
C62 C63 1.390(11) . ?
C63 C64 1.378(10) . ?
C64 N65 1.321(9) . ?
Cl66 O70 1.417(6) . ?
Cl66 O67 1.443(6) . ?
Cl66 O69 1.445(5) . ?
Cl66 O68 1.447(5) . ?
Cl71 C73 1.782(9) . ?
Cl72 C73 1.758(9) . ?
Cl74 C76 1.775(8) . ?
Cl75 C76 1.762(9) . ?
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
O5 V1 O6 82.6(2) . . ?
O5 V1 O12 95.9(2) . . ?
O6 V1 O12 176.0(2) . . ?
O5 V1 O22 167.1(2) . . ?
O6 V1 O22 87.6(2) . . ?
O12 V1 O22 94.4(2) . . ?
O5 V1 O7 91.1(2) . . ?
O6 V1 O7 87.1(2) . . ?
O12 V1 O7 89.2(2) . . ?
O22 V1 O7 96.8(2) . . ?
O5 V1 O17 89.1(2) . . ?
O6 V1 O17 96.0(2) . . ?
O12 V1 O17 87.7(2) . . ?
O22 V1 O17 83.6(2) . . ?
O7 V1 O17 176.8(2) . . ?
O5 V1 V2 42.60(14) . . ?
O6 V1 V2 41.27(12) . . ?
O12 V1 V2 136.37(13) . . ?
O22 V1 V2 128.80(15) . . ?
O7 V1 V2 80.70(13) . . ?
O17 V1 V2 101.54(13) . . ?
O6 V2 O5 82.3(2) . . ?
O6 V2 O32 96.3(2) . . ?
O5 V2 O32 174.8(2) . . ?
O6 V2 O27 167.4(2) . . ?
O5 V2 O27 87.8(2) . . ?
O32 V2 O27 94.2(2) . . ?
O6 V2 O8 91.3(2) . . ?
O5 V2 O8 86.6(2) . . ?
O32 V2 O8 88.5(2) . . ?
O27 V2 O8 95.7(2) . . ?
O6 V2 O37 89.6(2) . . ?
O5 V2 O37 97.0(2) . . ?
O32 V2 O37 87.9(2) . . ?
O27 V2 O37 84.0(2) . . ?
O8 V2 O37 176.4(2) . . ?
O6 V2 V1 42.36(14) . . ?
O5 V2 V1 41.22(12) . . ?
O32 V2 V1 136.21(15) . . ?
O27 V2 V1 128.82(14) . . ?
O8 V2 V1 80.51(14) . . ?
O37 V2 V1 102.46(13) . . ?
O5 V3 O18 96.8(2) . . ?
O5 V3 O28 93.5(2) . . ?
O18 V3 O28 93.8(2) . . ?
O5 V3 O13 95.1(2) . . ?
O18 V3 O13 89.5(2) . . ?
O28 V3 O13 170.5(2) . . ?
O5 V3 N42 99.2(2) . . ?
O18 V3 N42 163.9(2) . . ?
O28 V3 N42 83.4(2) . . ?
O13 V3 N42 91.0(2) . . ?
O5 V3 N53 174.4(2) . . ?
O18 V3 N53 88.7(2) . . ?
O28 V3 N53 86.7(2) . . ?
O13 V3 N53 84.3(2) . . ?
N42 V3 N53 75.3(2) . . ?
O6 V4 O38 95.4(2) . . ?
O6 V4 O33 95.0(2) . . ?
O38 V4 O33 89.2(2) . . ?
O6 V4 O23 93.0(2) . . ?
O38 V4 O23 93.2(2) . . ?
O33 V4 O23 171.4(2) . . ?
O6 V4 N65 98.0(2) . . ?
O38 V4 N65 166.4(2) . . ?
O33 V4 N65 91.6(2) . . ?
O23 V4 N65 84.1(2) . . ?
O6 V4 N54 173.7(2) . . ?
O38 V4 N54 90.8(2) . . ?
O33 V4 N54 83.9(2) . . ?
O23 V4 N54 87.8(2) . . ?
N65 V4 N54 75.8(2) . . ?
V3 O5 V1 123.8(2) . . ?
V3 O5 V2 130.8(2) . . ?
V1 O5 V2 96.2(2) . . ?
V4 O6 V2 123.4(2) . . ?
V4 O6 V1 131.6(2) . . ?
V2 O6 V1 96.4(2) . . ?
C9 O7 V1 126.1(4) . . ?
C9 O8 V2 127.4(4) . . ?
O7 C9 O8 124.3(6) . . ?
O7 C9 C10 120.9(6) . . ?
O8 C9 C10 114.7(6) . . ?
C9 C10 C11 115.8(7) . . ?
C14 O12 V1 129.5(4) . . ?
C14 O13 V3 134.7(5) . . ?
O12 C14 O13 124.6(7) . . ?
O12 C14 C15 117.8(7) . . ?
O13 C14 C15 117.6(7) . . ?
C16 C15 C14 112.2(8) . . ?
C19 O17 V1 137.9(4) . . ?
C19 O18 V3 125.7(4) . . ?
O17 C19 O18 124.6(6) . . ?
O17 C19 C20 119.5(6) . . ?
O18 C19 C20 116.0(6) . . ?
C19 C20 C21 115.6(7) . . ?
C24 O22 V1 124.6(4) . . ?
C24 O23 V4 130.6(4) . . ?
O23 C24 O22 123.9(6) . . ?
O23 C24 C25 118.3(6) . . ?
O22 C24 C25 117.8(6) . . ?
C26 C25 C24 115.6(7) . . ?
C29 O27 V2 123.9(4) . . ?
C29 O28 V3 130.3(4) . . ?
O28 C29 O27 124.3(6) . . ?
O28 C29 C30 118.0(6) . . ?
O27 C29 C30 117.7(6) . . ?
C31 C30 C29 115.5(7) . . ?
C34 O32 V2 127.5(4) . . ?
C34 O33 V4 135.7(5) . . ?
O33 C34 O32 125.1(7) . . ?
O33 C34 C35 116.8(7) . . ?
O32 C34 C35 118.1(7) . . ?
C34 C35 C36 114.5(8) . . ?
C39 O37 V2 137.2(4) . . ?
C39 O38 V4 125.8(4) . . ?
O37 C39 O38 125.2(6) . . ?
O37 C39 C40 117.1(6) . . ?
O38 C39 C40 117.7(6) . . ?
C39 C40 C41 116.0(7) . . ?
C43 N42 C47 118.7(6) . . ?
C43 N42 V3 122.7(5) . . ?
C47 N42 V3 118.3(4) . . ?
N42 C43 C44 124.0(8) . . ?
C43 C44 C45 117.4(7) . . ?
C46 C45 C44 118.2(7) . . ?
C45 C46 C47 121.6(8) . . ?
N42 C47 C46 120.0(6) . . ?
N42 C47 C48 114.9(6) . . ?
C46 C47 C48 125.1(7) . . ?
N53 C48 C49 120.0(6) . . ?
N53 C48 C47 115.4(6) . . ?
C49 C48 C47 124.6(6) . . ?
C50 C49 C48 119.5(7) . . ?
C49 C50 C51 120.3(8) . . ?
C50 C51 C52 118.0(7) . . ?
N53 C52 C51 123.1(7) . . ?
C52 N53 C48 119.2(6) . . ?
C52 N53 V3 124.9(5) . . ?
C48 N53 V3 116.0(4) . . ?
C55 N54 C59 119.1(6) . . ?
C55 N54 V4 124.8(5) . . ?
C59 N54 V4 115.9(4) . . ?
N54 C55 C56 122.7(7) . . ?
C57 C56 C55 118.3(7) . . ?
C58 C57 C56 119.2(8) . . ?
C57 C58 C59 120.9(8) . . ?
N54 C59 C58 119.7(7) . . ?
N54 C59 C60 115.8(6) . . ?
C58 C59 C60 124.5(7) . . ?
N65 C60 C61 121.0(6) . . ?
N65 C60 C59 114.8(6) . . ?
C61 C60 C59 124.1(7) . . ?
C62 C61 C60 119.2(8) . . ?
C61 C62 C63 119.8(8) . . ?
C64 C63 C62 117.4(7) . . ?
N65 C64 C63 124.4(7) . . ?
C64 N65 C60 118.1(6) . . ?
C64 N65 V4 124.5(5) . . ?
C60 N65 V4 117.4(4) . . ?
O70 Cl66 O67 110.0(4) . . ?
O70 Cl66 O69 110.0(4) . . ?
O67 Cl66 O69 108.4(3) . . ?
O70 Cl66 O68 110.0(3) . . ?
O67 Cl66 O68 109.0(3) . . ?
O69 Cl66 O68 109.4(3) . . ?
Cl72 C73 Cl71 111.1(5) . . ?
Cl75 C76 Cl74 111.0(4) . . ?
_refine_diff_density_max    1.465
_refine_diff_density_min   -0.810
_refine_diff_density_rms    0.145