# Copyright The Royal Society of Chemistry, 1999
# CCDC Number: 186/1492

data_VO(Hm)(L)
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C21 H27 N O10 V' 
_chemical_formula_weight          504.37 
_chemical_melting_point           ? 
_chemical_compound_source         ? 
 
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' 
 'V'  'V'   0.3005   0.5294 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M    p2(1)  
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z' 
 
_cell_length_a                    9.789(3) 
_cell_length_b                    18.534(5) 
_cell_length_c                    13.689(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  91.64(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      2483(1) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        parallopiped 
_exptl_crystal_colour             dark 
_exptl_crystal_size_max           0.4 
_exptl_crystal_size_mid           0.4 
_exptl_crystal_size_min           0.3 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.349 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1052 
_exptl_absorpt_coefficient_mu     0.452 
_exptl_absorpt_correction_type    semi-empirical 
_exptl_absorpt_correction_T_min   0.703 
_exptl_absorpt_correction_T_max   0.769 
 
_exptl_special_details 
; 
 ? 
; 
 
_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             4381 
_diffrn_reflns_av_R_equivalents   0.0365 
_diffrn_reflns_av_sigmaI/netI     0.0723 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        21 
_diffrn_reflns_limit_l_min        -15 
_diffrn_reflns_limit_l_max        15 
_diffrn_reflns_theta_min          1.85 
_diffrn_reflns_theta_max          24.05 
_reflns_number_total              4060 
_reflns_number_observed           2828 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 1 with very negative 
F^2^ 
 or flagged by the user for potential systematic errors.  Weighted R-
factors 
 wR and all goodnesses of fit S are based on F^2^, conventional R-
factors R 
 are based on F, with F set to zero for negative F^2^. The observed 
criterion 
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. 
and is 
 not relevant to the choice of reflections for refinement.  R-factors 
based 
 on F^2^ are statistically about twice as large as those based on F, and 
R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
 'calc w=1/[\s^2^(Fo^2^)+(0.0678P)^2^+2.7983P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     ? 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.00 
_refine_ls_number_reflns          4059 
_refine_ls_number_parameters      449 
_refine_ls_number_restraints      1 
_refine_ls_R_factor_all           0.1034 
_refine_ls_R_factor_obs           0.0649 
_refine_ls_wR_factor_all          0.1637 
_refine_ls_wR_factor_obs          0.1396 
_refine_ls_goodness_of_fit_all    1.030 
_refine_ls_goodness_of_fit_obs    1.082 
_refine_ls_restrained_S_all       1.035 
_refine_ls_restrained_S_obs       1.081 
_refine_ls_shift/esd_max          0.000 
_refine_ls_shift/esd_mean         0.000 
 
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 -1.1702(2) 0.11869(8) -1.09473(12) 0.0456(4) Uani 1 d . . 
O1 O -0.9782(7) -0.0900(5) -1.1882(5) 0.070(2) Uani 1 d . . 
O2 O -1.1573(9) -0.1585(4) -1.1296(7) 0.085(3) Uani 1 d . . 
O3 O -1.1019(6) 0.0288(3) -1.0839(4) 0.045(2) Uani 1 d . . 
O4 O -1.2974(7) 0.0505(4) -1.2117(5) 0.047(2) Uani 1 d . . 
H4B H -1.3694(78) 0.0441(46) -1.2113(56) 0.016(24) Uiso 1 d . . 
O5 O -1.1948(8) -0.0260(4) -1.3907(5) 0.071(2) Uani 1 d . . 
O6 O -0.8474(14) -0.0160(11) -1.3370(12) 0.168(7) Uani 1 d . . 
O7 O -1.0866(7) 0.1603(4) -1.0128(6) 0.065(2) Uani 1 d . . 
O8 O -1.3248(7) 0.0913(3) -1.0136(5) 0.047(2) Uani 1 d . . 
O9 O -1.5264(7) 0.1186(4) -0.9523(5) 0.063(2) Uani 1 d . . 
O10 O -1.0809(7) 0.1518(4) -1.2040(6) 0.065(2) Uani 1 d . . 
N1 N -1.3181(8) 0.1938(4) -1.1351(6) 0.050(2) Uani 1 d . . 
C1 C -1.0760(10) -0.0970(6) -1.1157(8) 0.054(3) Uiso 1 d . . 
H1A H -1.0287(10) -0.1003(6) -1.0518(8) 0.064 Uiso 1 calc R . 
C2 C -1.1738(10) -0.0334(5) -1.1147(7) 0.046(2) Uiso 1 d . . 
C3 C -1.2358(10) -0.0195(6) -1.2160(7) 0.043(2) Uiso 1 d . . 
C4 C -1.1332(10) -0.0196(6) -1.2967(7) 0.048(2) Uiso 1 d . . 
H4A H -1.0795(10) 0.0250(6) -1.2932(7) 0.058 Uiso 1 calc R . 
C5 C -1.0374(12) -0.0843(8) -1.2863(9) 0.075(3) Uiso 1 d . . 
H5A H -1.0893(12) -0.1283(8) -1.3011(9) 0.090 Uiso 1 calc R . 
C6 C -0.9191(20) -0.0808(14) -1.3511(14) 0.141(8) Uani 1 d . . 
H6A H -0.8586(20) -0.1212(14) -1.3373(14) 0.170 Uiso 1 calc R . 
H6B H -0.9508(20) -0.0844(14) -1.4187(14) 0.170 Uiso 1 calc R . 
C7 C -1.0842(19) -0.2242(7) -1.1208(13) 0.128(7) Uani 1 d . . 
H7A H -1.1458(19) -0.2640(7) -1.1311(13) 0.191 Uiso 1 calc R . 
H7B H -1.0426(19) -0.2276(7) -1.0566(13) 0.191 Uiso 1 calc R . 
H7C H -1.0145(19) -0.2257(7) -1.1687(13) 0.191 Uiso 1 calc R . 
C8 C -1.2383(15) 0.0379(8) -1.4357(9) 0.093(4) Uani 1 d . . 
H8A H -1.2784(15) 0.0272(8) -1.4988(9) 0.140 Uiso 1 calc R . 
H8B H -1.1615(15) 0.0695(8) -1.4430(9) 0.140 Uiso 1 calc R . 
H8C H -1.3049(15) 0.0610(8) -1.3961(9) 0.140 Uiso 1 calc R . 
C9 C -0.7255(18) -0.0113(20) -1.3842(14) 0.241(18) Uani 1 d . . 
H9A H -0.6839(18) 0.0347(20) -1.3705(14) 0.361 Uiso 1 calc R . 
H9B H -0.7421(18) -0.0160(20) -1.4534(14) 0.361 Uiso 1 calc R . 
H9C H -0.6656(18) -0.0491(20) -1.3618(14) 0.361 Uiso 1 calc R . 
C10 C -1.4293(10) 0.1327(5) -1.0039(7) 0.049(3) Uiso 1 d . . 
C11 C -1.4244(11) 0.2009(6) -1.0625(8) 0.062(3) Uiso 1 d . . 
H11A H -1.5123(11) 0.2094(6) -1.0951(8) 0.074 Uiso 1 calc R . 
H11B H -1.4041(11) 0.2415(6) -1.0198(8) 0.074 Uiso 1 calc R . 
C12 C -1.3313(11) 0.2260(6) -1.2163(8) 0.059(3) Uiso 1 d . . 
H12A H -1.4094(11) 0.2540(6) -1.2258(8) 0.071 Uiso 1 calc R . 
C13 C -1.2391(11) 0.2237(6) -1.2942(8) 0.058(3) Uiso 1 d . . 
C14 C -1.2687(13) 0.2601(7) -1.3827(9) 0.079(4) Uiso 1 d . . 
H14A H -1.3510(13) 0.2849(7) -1.3901(9) 0.094 Uiso 1 calc R . 
C15 C -1.1814(14) 0.2599(8) -1.4567(11) 0.092(4) Uiso 1 d . . 
H15A H -1.2043(14) 0.2834(8) -1.5149(11) 0.110 Uiso 1 calc R . 
C16 C -1.0562(15) 0.2245(8) -1.4457(11) 0.098(4) Uiso 1 d . . 
H16A H -0.9958(15) 0.2251(8) -1.4969(11) 0.118 Uiso 1 calc R . 
C17 C -1.0199(13) 0.1885(7) -1.3609(9) 0.075(4) Uiso 1 d . . 
H17A H -0.9356(13) 0.1656(7) -1.3535(9) 0.090 Uiso 1 calc R . 
C18 C -1.1164(11) 0.1877(6) -1.2852(8) 0.056(3) Uiso 1 d . . 
C19 C -0.4674(22) -0.6986(12) -0.8065(15) 0.136(7) Uiso 1 d . . 
H19A H -0.4941(22) -0.6558(12) -0.8370(15) 0.163 Uiso 1 calc R . 
C20 C -0.5575(28) -0.7413(16) -0.7797(18) 0.182(9) Uiso 1 d . . 
H20A H -0.6490(28) -0.7285(16) -0.7876(18) 0.218 Uiso 1 calc R . 
C21 C -0.5214(27) -0.8116(15) -0.7356(18) 0.181(9) Uiso 1 d . . 
H21A H -0.5862(27) -0.8454(15) -0.7176(18) 0.217 Uiso 1 calc R . 
C22 C -0.3778(24) -0.8229(14) -0.7234(17) 0.163(8) Uiso 1 d . . 
H22A H -0.3480(24) -0.8654(14) -0.6935(17) 0.195 Uiso 1 calc R . 
C23 C -0.2879(22) -0.7780(11) -0.7510(14) 0.133(6) Uiso 1 d . . 
H23A H -0.1952(22) -0.7884(11) -0.7438(14) 0.160 Uiso 1 calc R . 
C24 C -0.3326(24) -0.7122(13) -0.7930(15) 0.151(7) Uiso 1 d . . 
H24A H -0.2688(24) -0.6780(13) -0.8114(15) 0.181 Uiso 1 calc R . 
V51 V -1.6762(2) -0.08269(9) -0.94152(12) 0.0446(4) Uani 1 d . . 
O51 O -1.3172(7) -0.1786(4) -0.7635(6) 0.060(2) Uani 1 d . . 
O52 O -1.1640(6) -0.1322(4) -0.8749(5) 0.057(2) Uani 1 d . . 
O53 O -1.5262(6) -0.1358(3) -0.9106(5) 0.043(2) Uani 1 d . . 
O54 O -1.5361(6) -0.0034(4) -0.8533(5) 0.045(2) Uani 1 d . . 
H54B H -1.5196(100) 0.0421(61) -0.8679(73) 0.060(33) Uiso 1 d . . 
O55 O -1.4163(8) -0.0074(5) -0.6540(5) 0.073(2) Uani 1 d . . 
O56 O -1.4201(11) -0.1769(7) -0.5695(7) 0.128(4) Uani 1 d . . 
O57 O -1.7652(7) -0.1422(4) -0.9964(5) 0.059(2) Uani 1 d . . 
O58 O -1.5772(6) -0.0428(3) -1.0531(5) 0.047(2) Uani 1 d . . 
O59 O -1.5646(6) 0.0383(4) -1.1716(5) 0.059(2) Uani 1 d . . 
O60 O -1.7697(6) -0.0819(4) -0.8249(5) 0.056(2) Uani 1 d . . 
N51 N -1.7887(7) 0.0081(5) -0.9778(6) 0.046(2) Uani 1 d . . 
C51 C -1.2949(10) -0.1593(6) -0.8616(7) 0.051(3) Uiso 1 d . . 
H51A H -1.3076(10) -0.2023(6) -0.9026(7) 0.062 Uiso 1 calc R . 
C52 C -1.3950(9) -0.1015(5) -0.8968(7) 0.042(2) Uiso 1 d . . 
C53 C -1.4114(10) -0.0399(5) -0.8242(7) 0.045(2) Uiso 1 d . . 
C54 C -1.4231(10) -0.0667(5) -0.7194(7) 0.050(3) Uiso 1 d . . 
H54A H -1.5100(10) -0.0921(5) -0.7124(7) 0.060 Uiso 1 calc R . 
C55 C -1.3068(11) -0.1169(6) -0.6960(8) 0.055(3) Uiso 1 d . . 
H55A H -1.2214(11) -0.0913(6) -0.7084(8) 0.066 Uiso 1 calc R . 
C56 C -1.2978(12) -0.1461(8) -0.5940(9) 0.080(4) Uani 1 d . . 
H56B H -1.2258(12) -0.1820(8) -0.5892(9) 0.096 Uiso 1 calc R . 
H56A H -1.2751(12) -0.1074(8) -0.5487(9) 0.096 Uiso 1 calc R . 
C57 C -1.0613(10) -0.1849(7) -0.8500(11) 0.079(4) Uani 1 d . . 
H57C H -0.9724(10) -0.1647(7) -0.8599(11) 0.119 Uiso 1 calc R . 
H57B H -1.0739(10) -0.2266(7) -0.8907(11) 0.119 Uiso 1 calc R . 
H57A H -1.0689(10) -0.1985(7) -0.7827(11) 0.119 Uiso 1 calc R . 
C58 C -1.5364(16) 0.0081(11) -0.6061(12) 0.137(7) Uani 1 d . . 
H58C H -1.5217(16) 0.0488(11) -0.5637(12) 0.205 Uiso 1 calc R . 
H58B H -1.5626(16) -0.0329(11) -0.5682(12) 0.205 Uiso 1 calc R . 
H58A H -1.6076(16) 0.0192(11) -0.6534(12) 0.205 Uiso 1 calc R . 
C59 C -1.4171(24) -0.1999(16) -0.4681(13) 0.223(15) Uani 1 d . . 
H59C H -1.5034(24) -0.2211(16) -0.4529(13) 0.334 Uiso 1 calc R . 
H59B H -1.4002(24) -0.1589(16) -0.4265(13) 0.334 Uiso 1 calc R . 
H59A H -1.3457(24) -0.2348(16) -0.4578(13) 0.334 Uiso 1 calc R . 
C60 C -1.6244(10) 0.0112(6) -1.1056(8) 0.049(3) Uiso 1 d . . 
C61 C -1.7641(9) 0.0357(6) -1.0768(7) 0.049(2) Uiso 1 d . . 
H61B H -1.7688(9) 0.0880(6) -1.0772(7) 0.059 Uiso 1 calc R . 
H61A H -1.8329(9) 0.0173(6) -1.1227(7) 0.059 Uiso 1 calc R . 
C62 C -1.8660(10) 0.0437(6) -0.9233(7) 0.053(3) Uiso 1 d . . 
H62A H -1.9045(10) 0.0856(6) -0.9492(7) 0.064 Uiso 1 calc R . 
C63 C -1.9001(10) 0.0252(6) -0.8243(8) 0.055(3) Uiso 1 d . . 
C64 C -1.9936(13) 0.0698(8) -0.7752(10) 0.082(4) Uiso 1 d . . 
H64A H -2.0306(13) 0.1105(8) -0.8057(10) 0.098 Uiso 1 calc R . 
C65 C -2.0298(15) 0.0514(9) -0.6787(10) 0.095(4) Uiso 1 d . . 
H65A H -2.0891(15) 0.0807(9) -0.6447(10) 0.114 Uiso 1 calc R . 
C66 C -1.9787(13) -0.0083(7) -0.6366(10) 0.082(4) Uiso 1 d . . 
H66A H -2.0024(13) -0.0195(7) -0.5730(10) 0.098 Uiso 1 calc R . 
C67 C -1.8913(11) -0.0538(6) -0.6853(8) 0.065(3) Uiso 1 d . . 
H67A H -1.8593(11) -0.0957(6) -0.6552(8) 0.078 Uiso 1 calc R . 
C68 C -1.8516(9) -0.0368(5) -0.7787(7) 0.045(2) Uiso 1 d . . 
H52A H -1.3588(81) -0.0773(51) -0.9551(62) 0.049(24) Uiso 1 d . . 
H2A H -1.2629(88) -0.0496(47) -1.0750(62) 0.048(25) Uiso 1 d . . 
H53A H -1.3395(71) -0.0038(39) -0.8304(49) 0.020(19) Uiso 1 d . . 
H3A H -1.2985(85) -0.0532(47) -1.2406(60) 0.046(25) 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 0.0411(9) 0.0411(9) 0.0542(10) 0.0007(9) -0.0069(8) -0.0015(8) 
O1 0.070(5) 0.078(5) 0.063(5) -0.001(4) -0.007(4) 0.036(5) 
O2 0.094(6) 0.041(4) 0.118(7) 0.001(5) -0.027(6) 0.009(5) 
O3 0.038(4) 0.046(4) 0.052(4) -0.005(3) -0.006(3) -0.004(3) 
O4 0.028(4) 0.050(5) 0.061(5) 0.000(3) -0.001(3) 0.003(4) 
O5 0.093(6) 0.069(5) 0.050(5) -0.014(4) -0.021(4) 0.004(5) 
O6 0.109(10) 0.229(18) 0.172(13) 0.058(14) 0.086(10) 0.043(11) 
O7 0.066(5) 0.051(5) 0.077(5) -0.009(4) -0.017(4) -0.003(4) 
O8 0.056(4) 0.037(4) 0.048(4) 0.001(3) 0.004(3) 0.012(3) 
O9 0.071(5) 0.043(4) 0.076(5) 0.012(4) 0.021(4) 0.012(4) 
O10 0.042(4) 0.068(5) 0.084(6) 0.007(4) 0.010(4) -0.006(4) 
N1 0.059(5) 0.035(5) 0.057(5) 0.002(4) 0.006(4) 0.002(4) 
C6 0.122(16) 0.201(23) 0.104(12) 0.030(17) 0.045(12) 0.087(17) 
C7 0.156(15) 0.046(8) 0.180(18) 0.012(10) -0.019(13) 0.032(9) 
C8 0.126(11) 0.087(10) 0.064(8) -0.008(8) -0.044(8) 0.018(9) 
C9 0.090(13) 0.505(57) 0.130(17) -0.030(26) 0.031(12) -0.025(23) 
V51 0.0353(8) 0.0426(9) 0.0556(10) 0.0036(9) -0.0032(7) 0.0005(8) 
O51 0.043(4) 0.056(5) 0.081(5) 0.018(4) -0.004(4) -0.001(3) 
O52 0.030(3) 0.056(4) 0.084(5) 0.008(4) -0.002(3) -0.002(3) 
O53 0.032(3) 0.042(4) 0.054(4) 0.004(3) -0.009(3) -0.002(3) 
O54 0.037(4) 0.037(4) 0.059(5) 0.005(3) -0.006(3) 0.002(3) 
O55 0.067(5) 0.097(6) 0.054(5) -0.012(4) -0.003(4) 0.001(5) 
O56 0.104(8) 0.190(12) 0.089(7) 0.081(8) -0.004(6) -0.018(8) 
O57 0.039(4) 0.063(5) 0.074(5) -0.004(4) -0.011(3) -0.010(3) 
O58 0.042(4) 0.049(4) 0.050(4) 0.002(3) -0.004(3) 0.003(3) 
O59 0.038(4) 0.083(5) 0.056(4) 0.020(4) 0.007(3) 0.008(4) 
O60 0.048(4) 0.060(4) 0.059(4) 0.015(4) 0.007(3) 0.003(4) 
N51 0.026(4) 0.060(5) 0.051(5) 0.013(4) 0.000(4) 0.000(4) 
C56 0.063(8) 0.114(11) 0.062(8) 0.014(7) -0.016(6) -0.007(8) 
C57 0.034(6) 0.075(9) 0.130(12) 0.008(8) 0.005(7) 0.007(6) 
C58 0.096(12) 0.186(20) 0.129(14) -0.069(14) 0.006(11) 0.019(12) 
C59 0.213(23) 0.351(41) 0.104(15) 0.108(21) -0.019(15) -0.090(27) 
 
_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 O7 1.571(7) . ? 
V1 O3 1.799(7) . ? 
V1 O10 1.858(7) . ? 
V1 O8 1.970(7) . ? 
V1 N1 2.072(8) . ? 
V1 O4 2.366(7) . ? 
O1 C1 1.404(12) . ? 
O1 C5 1.452(13) . ? 
O2 C1 1.400(13) . ? 
O2 C7 1.416(15) . ? 
O3 C2 1.409(11) . ? 
O4 C3 1.433(12) . ? 
O5 C8 1.395(14) . ? 
O5 C4 1.410(11) . ? 
O6 C9 1.38(2) . ? 
O6 C6 1.40(3) . ? 
O8 C10 1.289(11) . ? 
O9 C10 1.228(11) . ? 
O10 C18 1.333(13) . ? 
N1 C12 1.265(13) . ? 
N1 C11 1.465(13) . ? 
C1 C2 1.518(14) . ? 
C2 C3 1.520(13) . ? 
C3 C4 1.514(13) . ? 
C4 C5 1.53(2) . ? 
C5 C6 1.48(2) . ? 
C10 C11 1.499(15) . ? 
C12 C13 1.418(14) . ? 
C13 C18 1.377(14) . ? 
C13 C14 1.41(2) . ? 
C14 C15 1.34(2) . ? 
C15 C16 1.40(2) . ? 
C16 C17 1.38(2) . ? 
C17 C18 1.42(2) . ? 
C19 C20 1.25(3) . ? 
C19 C24 1.35(2) . ? 
C20 C21 1.47(3) . ? 
C21 C22 1.43(3) . ? 
C22 C23 1.28(2) . ? 
C23 C24 1.41(3) . ? 
V51 O57 1.583(7) . ? 
V51 O53 1.809(6) . ? 
V51 O60 1.863(7) . ? 
V51 O58 1.976(6) . ? 
V51 N51 2.063(8) . ? 
V51 O54 2.325(7) . ? 
O51 C51 1.412(12) . ? 
O51 C55 1.472(12) . ? 
O52 C51 1.394(11) . ? 
O52 C57 1.436(12) . ? 
O53 C52 1.441(11) . ? 
O54 C53 1.442(11) . ? 
O55 C58 1.393(15) . ? 
O55 C54 1.417(12) . ? 
O56 C56 1.376(14) . ? 
O56 C59 1.45(2) . ? 
O58 C60 1.309(12) . ? 
O59 C60 1.201(11) . ? 
O60 C68 1.330(11) . ? 
N51 C62 1.264(12) . ? 
N51 C61 1.475(11) . ? 
C51 C52 1.522(13) . ? 
C52 C53 1.526(13) . ? 
C53 C54 1.525(13) . ? 
C54 C55 1.497(14) . ? 
C55 C56 1.50(2) . ? 
C60 C61 1.504(13) . ? 
C62 C63 1.446(14) . ? 
C63 C68 1.385(14) . ? 
C63 C64 1.42(2) . ? 
C64 C65 1.42(2) . ? 
C65 C66 1.34(2) . ? 
C66 C67 1.39(2) . ? 
C67 C68 1.384(14) . ? 
 
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 
O7 V1 O3 102.2(3) . . ? 
O7 V1 O10 99.5(4) . . ? 
O3 V1 O10 101.0(3) . . ? 
O7 V1 O8 96.7(4) . . ? 
O3 V1 O8 90.2(3) . . ? 
O10 V1 O8 157.8(3) . . ? 
O7 V1 N1 101.9(4) . . ? 
O3 V1 N1 154.0(3) . . ? 
O10 V1 N1 84.5(3) . . ? 
O8 V1 N1 77.4(3) . . ? 
O7 V1 O4 176.7(3) . . ? 
O3 V1 O4 75.4(3) . . ? 
O10 V1 O4 83.2(3) . . ? 
O8 V1 O4 81.2(3) . . ? 
N1 V1 O4 80.1(3) . . ? 
C1 O1 C5 113.5(8) . . ? 
C1 O2 C7 113.9(10) . . ? 
C2 O3 V1 123.5(5) . . ? 
C3 O4 V1 107.3(6) . . ? 
C8 O5 C4 116.7(8) . . ? 
C9 O6 C6 115.2(21) . . ? 
C10 O8 V1 122.0(6) . . ? 
C18 O10 V1 136.0(7) . . ? 
C12 N1 C11 119.7(9) . . ? 
C12 N1 V1 127.2(8) . . ? 
C11 N1 V1 112.6(6) . . ? 
O2 C1 O1 112.0(9) . . ? 
O2 C1 C2 106.1(8) . . ? 
O1 C1 C2 112.2(8) . . ? 
O3 C2 C1 109.2(8) . . ? 
O3 C2 C3 108.5(8) . . ? 
C1 C2 C3 111.0(8) . . ? 
O4 C3 C4 108.6(8) . . ? 
O4 C3 C2 105.8(8) . . ? 
C4 C3 C2 114.2(8) . . ? 
O5 C4 C3 112.9(8) . . ? 
O5 C4 C5 105.4(8) . . ? 
C3 C4 C5 110.6(9) . . ? 
O1 C5 C6 105.0(11) . . ? 
O1 C5 C4 111.8(10) . . ? 
C6 C5 C4 113.6(12) . . ? 
O6 C6 C5 110.6(17) . . ? 
O9 C10 O8 124.1(9) . . ? 
O9 C10 C11 121.6(9) . . ? 
O8 C10 C11 114.2(9) . . ? 
N1 C11 C10 108.7(9) . . ? 
N1 C12 C13 126.6(11) . . ? 
C18 C13 C14 117.9(10) . . ? 
C18 C13 C12 121.3(10) . . ? 
C14 C13 C12 120.8(11) . . ? 
C15 C14 C13 121.8(13) . . ? 
C14 C15 C16 119.7(14) . . ? 
C17 C16 C15 121.6(14) . . ? 
C16 C17 C18 117.3(12) . . ? 
O10 C18 C13 121.5(10) . . ? 
O10 C18 C17 116.8(10) . . ? 
C13 C18 C17 121.7(11) . . ? 
C20 C19 C24 122.5(25) . . ? 
C19 C20 C21 121.2(26) . . ? 
C22 C21 C20 113.7(26) . . ? 
C23 C22 C21 123.7(26) . . ? 
C22 C23 C24 118.4(23) . . ? 
C19 C24 C23 120.4(23) . . ? 
O57 V51 O53 99.4(3) . . ? 
O57 V51 O60 97.8(4) . . ? 
O53 V51 O60 102.6(3) . . ? 
O57 V51 O58 99.7(3) . . ? 
O53 V51 O58 88.4(3) . . ? 
O60 V51 O58 157.4(3) . . ? 
O57 V51 N51 99.9(3) . . ? 
O53 V51 N51 157.6(3) . . ? 
O60 V51 N51 85.9(3) . . ? 
O58 V51 N51 77.2(3) . . ? 
O57 V51 O54 175.0(3) . . ? 
O53 V51 O54 76.1(3) . . ? 
O60 V51 O54 81.2(3) . . ? 
O58 V51 O54 82.5(3) . . ? 
N51 V51 O54 85.0(3) . . ? 
C51 O51 C55 113.0(8) . . ? 
C51 O52 C57 111.3(8) . . ? 
C52 O53 V51 120.3(5) . . ? 
C53 O54 V51 109.2(5) . . ? 
C58 O55 C54 115.6(10) . . ? 
C56 O56 C59 111.2(12) . . ? 
C60 O58 V51 122.5(6) . . ? 
C68 O60 V51 136.9(6) . . ? 
C62 N51 C61 118.6(8) . . ? 
C62 N51 V51 127.4(7) . . ? 
C61 N51 V51 113.8(6) . . ? 
O52 C51 O51 112.6(8) . . ? 
O52 C51 C52 106.9(8) . . ? 
O51 C51 C52 111.3(8) . . ? 
O53 C52 C51 107.1(8) . . ? 
O53 C52 C53 107.8(8) . . ? 
C51 C52 C53 113.5(8) . . ? 
O54 C53 C54 109.1(8) . . ? 
O54 C53 C52 106.0(7) . . ? 
C54 C53 C52 112.4(8) . . ? 
O55 C54 C55 108.9(8) . . ? 
O55 C54 C53 109.8(8) . . ? 
C55 C54 C53 109.1(8) . . ? 
O51 C55 C56 107.8(9) . . ? 
O51 C55 C54 108.0(8) . . ? 
C56 C55 C54 116.7(10) . . ? 
O56 C56 C55 110.4(9) . . ? 
O59 C60 O58 124.1(10) . . ? 
O59 C60 C61 122.5(9) . . ? 
O58 C60 C61 113.4(9) . . ? 
N51 C61 C60 108.1(8) . . ? 
N51 C62 C63 126.0(10) . . ? 
C68 C63 C64 119.3(10) . . ? 
C68 C63 C62 122.2(10) . . ? 
C64 C63 C62 118.4(10) . . ? 
C63 C64 C65 118.8(13) . . ? 
C66 C65 C64 120.0(14) . . ? 
C65 C66 C67 121.6(14) . . ? 
C68 C67 C66 120.0(12) . . ? 
O60 C68 C67 119.1(9) . . ? 
O60 C68 C63 120.7(9) . . ? 
C67 C68 C63 120.2(10) . . ? 
 
_refine_diff_density_max    0.457 
_refine_diff_density_min   -0.288 
_refine_diff_density_rms    0.067 

#=END