# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1440 ############################################################################## # IUMSC CIF Archive file # ############################################################################## data_MSC95138 _audit_creation_method 'minor manual editing of SDT2CIF v. 1.1 BETA output' _chemical_formula_sum 'C26 H55 Cl1 N3 O17 V5' _chemical_formula_moiety ? _chemical_formula_weight 971.893 _cell_length_a 16.111(2) _cell_length_b 14.9003(19) _cell_length_c 33.674(5) _cell_angle_alpha 90 _cell_angle_beta 91.390(7) _cell_angle_gamma 90 _cell_volume 8081.5(19) _cell_formula_units_Z 8 _cell_measurement_reflns_used 120 _cell_measurement_theta_min 12.73 _cell_measurement_theta_max 16.86 _cell_measurement_temperature ? _exptl_crystal_colour ? _exptl_crystal_description ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4000 _exptl_absorpt_coefficient_mu 1.2493 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details Tompa _exptl_absorpt_correction_T_min 0.468 _exptl_absorpt_correction_T_max 0.746 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2+x,1/2+y,z -x,y,1/2-z 1/2-x,1/2+y,1/2-z x,-y,1/2+z 1/2+x,1/2-y,1/2+z -x,-y,-z 1/2-x,1/2-y,-z _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature ? _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7969 _diffrn_reflns_av_R_equivalents 0.024 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max ? _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min ? _diffrn_reflns_limit_h_max ? _diffrn_reflns_limit_k_min ? _diffrn_reflns_limit_k_max ? _diffrn_reflns_limit_l_min ? _diffrn_reflns_limit_l_max ? _diffrn_standards_number 4 _diffrn_standards_decay_% -3.8 _diffrn_standards_interval_count 300 _reflns_number_total 7133 _reflns_number_gt 5837 _reflns_threshold_expression F^2^>2.33\s(F^2^) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source V V 0.267 0.53 'International Tables Vol. IV (1974) Table 2.2B' CL Cl 0.132 0.159 'International Tables Vol. IV (1974) Table 2.2B' O O 0.008 0.006 'International Tables Vol. IV (1974) Table 2.2B' N N 0.004 0.003 'International Tables Vol. IV (1974) Table 2.2B' C C 0.002 0.002 'International Tables Vol. IV (1974) Table 2.2B' H H 0 0 'International Tables Vol. IV (1974) Table 2.2B' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_number_reflns ? _refine_ls_number_parameters ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_coef 0.4152E-7 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_expression ; Larson, A. C. (1967). Acta Cryst. 23, p. 664. Eq. (3) ; _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack ? _refine_ls_weighting_scheme calc _refine_ls_weighting_details w^-1^=\s^2^(F)+(.07F)^2^ _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0411 _refine_ls_goodness_of_fit_ref 1.3432 _refine_ls_shift/su_max 0.1347 _refine_diff_density_max ? _refine_diff_density_min ? _computing_data_collection 'NPS, local program' _computing_cell_refinement 'XTEL, local package' _computing_data_reduction 'XTEL, local package' _computing_structure_solution MULTAN78 _computing_structure_refinement 'XTEL, local package' _computing_molecular_graphics 'XTEL, local package' _computing_publication_material 'XTEL, local package' 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_disorder_group _atom_site_disorder_assembly V1 V 0.61931(3) 0.21372(3) 0.157497(10) 0.01408(12) Uani 1 0 . V2 V 0.77291(3) 0.06367(3) 0.130446(10) 0.01365(12) Uani 1 0 . V3 V 0.89959(3) 0.24511(3) 0.108096(10) 0.01427(12) Uani 1 0 . V4 V 0.74740(3) 0.39357(3) 0.138109(10) 0.01503(12) Uani 1 0 . V5 V 0.79553(3) 0.22628(3) 0.176781(10) 0.01460(12) Uani 1 0 . CL6 CL 0.72222(4) 0.23349(4) 0.08763(2) 0.01539(17) Uani 1 0 . O7 O 0.71536(10) 0.13598(10) 0.16950(10) 0.0144(6) Uani 1 0 . O8 O 0.85908(10) 0.15199(10) 0.14400(10) 0.0147(6) Uani 1 0 . O9 O 0.84600(10) 0.31904(10) 0.14831(10) 0.0154(6) Uani 1 0 . O10 O 0.70276(10) 0.30328(10) 0.17412(10) 0.0160(6) Uani 1 0 . O11 O 0.56112(10) 0.20073(10) 0.19472(10) 0.0212(6) Uani 1 0 . O12 O 0.80149(10) 0.97339(10) 0.15249(10) 0.0204(6) Uani 1 0 . O13 O 0.99655(10) 0.25477(10) 0.11838(10) 0.0228(6) Uani 1 0 . O14 O 0.76204(10) 0.48179(10) 0.16425(10) 0.0243(6) Uani 1 0 . O15 O 0.83462(10) 0.22352(10) 0.22121(10) 0.0193(6) Uani 1 0 . O16 O 0.56736(10) 0.12527(10) 0.11891(10) 0.0182(6) Uani 1 0 . C17 C 0.5923(2) 0.0549(2) 0.10216(10) 0.0181(6) Uani 1 0 . O18 O 0.66510(10) 0.02351(10) 0.10479(10) 0.0190(6) Uani 1 0 . C19 C 0.5310(2) 0.0044(2) 0.07665(10) 0.0248(12) Uani 1 0 . O20 O 0.81878(10) 0.04360(10) 0.07611(10) 0.0190(6) Uani 1 0 . C21 C 0.8684(2) 0.0851(2) 0.05430(10) 0.0194(8) Uani 1 0 . O22 O 0.90399(10) 0.15815(10) 0.06227(10) 0.0190(6) Uani 1 0 . C23 C 0.8859(2) 0.0435(2) 0.01471(10) 0.0284(12) Uani 1 0 . O24 O 0.88627(10) 0.33952(10) 0.06557(10) 0.0183(6) Uani 1 0 . C25 C 0.8387(2) 0.4059(2) 0.06052(10) 0.0179(6) Uani 1 0 . O26 O 0.78792(10) 0.43582(10) 0.08498(10) 0.0197(6) Uani 1 0 . C27 C 0.8424(2) 0.4528(2) 0.02078(10) 0.0303(12) Uani 1 0 . O28 O 0.63345(10) 0.42404(10) 0.11599(10) 0.0207(6) Uani 1 0 . C29 C 0.5639(2) 0.3858(2) 0.11627(10) 0.0200(6) Uani 1 0 . O30 O 0.54982(10) 0.30714(10) 0.12844(10) 0.0204(6) Uani 1 0 . C31 C 0.4903(2) 0.4378(2) 0.09998(10) 0.0294(10) Uani 1 0 . N32 N 0.73835(10) -0.27380(10) 0.11133(10) 0.0174(6) Uani 1 0 . C33 C 0.7043(2) 0.8112(2) 0.09202(10) 0.0251(10) Uani 1 0 . C34 C 0.7453(3) -0.1622(2) 0.05420(10) 0.0412(14) Uani 1 0 . C35 C 0.6880(2) 0.7045(2) 0.14757(10) 0.0211(10) Uani 1 0 . C36 C 0.6943(2) 0.7739(3) 0.18009(10) 0.0424(12) Uani 1 0 . C37 C 0.8293(2) 0.7408(2) 0.12291(10) 0.0288(10) Uani 1 0 . C38 C 0.8675(2) 0.6680(3) 0.14850(10) 0.0545(16) Uani 1 0 . C39 C 0.7311(2) 0.6468(2) 0.08331(10) 0.0310(10) Uani 1 0 . C40 C 0.6463(3) -0.3679(2) 0.06463(10) 0.0426(14) Uani 1 0 . N41 N 0.5 0.4715(2) 0.25 0.0167(12) Uani 1 0 . C42 C 0.5707(2) 0.4134(2) 0.23518(10) 0.0219(8) Uani 1 0 . C43 C 0.6058(2) 0.3461(2) 0.26479(10) 0.0272(12) Uani 1 0 . C44 C 0.5328(2) 0.5294(2) 0.28416(10) 0.0226(10) Uani 1 0 . C45 C 0.4716(2) 0.5965(2) 0.29998(10) 0.0372(12) Uani 1 0 . N46 N 1 0.4607(2) 0.25 0.0321(14) Uani 1 0 . C47 C 1.0004(2) 0.3991(2) 0.28591(10) 0.0281(12) Uani 1 0 . C48 C 0.9944(2) 0.4469(2) 0.32541(10) 0.0396(12) Uani 1 0 . C49 C 0.9232(3) 0.5210(3) 0.24910(10) 0.0595(16) Uani 1 0 . C50 C 0.8410(3) 0.4752(3) 0.25384(10) 0.0623(16) Uani 1 0 . C51 C 0.9498(2) 0.2591(3) -0.02417(10) 0.0362(12) Uani 1 0 . C52 C 1.0340(2) 0.2917(2) -0.02093(10) 0.0327(12) Uani 1 0 . N53 N 0.0989(2) 0.3174(3) 0.98059(10) 0.0682(16) Uani 1 0 . H1 H 0.4788 0.0342 0.077 0.0374 Uiso 1 0 . H2 H 0.55 0.0019 0.0503 0.0374 Uiso 1 0 . H3 H 0.525 -0.0547 0.0868 0.0374 Uiso 1 0 . H4 H 0.8764 0.9807 0.0159 0.0414 Uiso 1 0 . H5 H 0.8504 0.0692 -0.0052 0.0414 Uiso 1 0 . H6 H 0.9422 0.0542 0.0082 0.0414 Uiso 1 0 . H7 H 0.8986 0.4634 0.0145 0.043 Uiso 1 0 . H8 H 0.817 0.4158 0.001 0.043 Uiso 1 0 . H9 H 0.8135 0.5081 0.0222 0.043 Uiso 1 0 . H10 H 0.5091 0.4921 0.0884 0.0416 Uiso 1 0 . H11 H 0.462 0.4029 0.0804 0.0416 Uiso 1 0 . H12 H 0.4539 0.4512 0.1209 0.0416 Uiso 1 0 . H13 H 0.6468 0.8023 0.0863 0.0374 Uiso 1 0 . H14 H 0.7109 -0.141 0.1105 0.0374 Uiso 1 0 . H15 H 0.8027 -0.1523 0.0594 0.0537 Uiso 1 0 . H16 H 0.7384 -0.2088 0.0352 0.0537 Uiso 1 0 . H17 H 0.7204 0.8913 0.0442 0.0537 Uiso 1 0 . H18 H 0.6313 -0.3007 0.1394 0.0333 Uiso 1 0 . H19 H 0.7068 -0.3514 0.158 0.0333 Uiso 1 0 . H20 H 0.7505 0.7786 0.1892 0.0546 Uiso 1 0 . H21 H 0.676 -0.1698 0.1701 0.0546 Uiso 1 0 . H22 H 0.6607 0.7562 0.2015 0.0546 Uiso 1 0 . H23 H 0.86 -0.2553 0.0992 0.0416 Uiso 1 0 . H24 H 0.8337 -0.2042 0.137 0.0416 Uiso 1 0 . H25 H 0.8379 -0.3366 0.1725 0.0667 Uiso 1 0 . H26 H 0.8646 0.6125 0.1347 0.0667 Uiso 1 0 . H27 H 0.9238 -0.3176 0.1544 0.0667 Uiso 1 0 . H28 H 0.769 -0.3446 0.0625 0.0433 Uiso 1 0 . H29 H 0.7457 0.5942 0.0978 0.0433 Uiso 1 0 . H30 H 0.6305 -0.3164 0.0496 0.0545 Uiso 1 0 . H31 H 0.6476 0.5813 0.0476 0.0545 Uiso 1 0 . H32 H 0.6072 -0.3778 0.0848 0.0545 Uiso 1 0 . H33 H 0.5508 0.3811 0.2126 0.0344 Uiso 1 0 . H34 H 0.6145 0.452 0.2277 0.0344 Uiso 1 0 . H35 H 0.5633 0.3062 0.2725 0.0399 Uiso 1 0 . H36 H 0.6492 0.3131 0.2529 0.0399 Uiso 1 0 . H37 H 0.6273 0.377 0.2875 0.0399 Uiso 1 0 . H38 H 0.5492 0.4909 0.3053 0.0354 Uiso 1 0 . H39 H 0.5796 0.5616 0.2752 0.0354 Uiso 1 0 . H40 H 0.4974 0.63 0.3209 0.05 Uiso 1 0 . H41 H 0.4545 0.6361 0.2792 0.05 Uiso 1 0 . H42 H 0.4247 0.5657 0.3097 0.05 Uiso 1 0 . H43 H 0.9547 0.3592 0.2832 0.0408 Uiso 1 0 . H44 H 1.0508 0.3658 0.2862 0.0408 Uiso 1 0 . H45 H 1.04 0.4866 0.3289 0.0519 Uiso 1 0 . H46 H 0.944 0.48 0.3259 0.0519 Uiso 1 0 . H47 H 0.995 0.4039 0.3463 0.0519 Uiso 1 0 . H48 H 0.9296 0.5635 0.27 0.0708 Uiso 1 0 . H49 H 0.9215 0.5514 0.2243 0.0708 Uiso 1 0 . H50 H 0.7981 0.5188 0.2532 0.0736 Uiso 1 0 . H51 H 0.8324 0.4336 0.2328 0.0736 Uiso 1 0 . H52 H 0.841 0.4445 0.2785 0.0736 Uiso 1 0 . H53 H 0.9279 0.253 0.0016 0.0488 Uiso 1 0 . H54 H 0.917 0.3006 0.9609 0.0488 Uiso 1 0 . H55 H 0.9491 0.2026 0.9629 0.0488 Uiso 1 0 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 V1 0.0113(2) 0.0133(2) 0.0178(2) 0.0011(2) 0.0030(2) 0.0010(2) V2 0.0131(2) 0.0106(2) 0.0172(2) 0.0013(2) 0.0000(2) -0.0005(2) V3 0.0095(2) 0.0161(2) 0.0172(2) 0.0000(2) -0.0005(2) 0.0003(2) V4 0.0152(2) 0.0103(2) 0.0195(2) 0.0005(2) 0.0011(2) 0.0008(2) V5 0.0149(2) 0.0139(2) 0.0149(2) 0.0010(2) -0.0014(2) -0.0005(2) CL6 0.0135(3) 0.0165(3) 0.0161(3) -0.0007(2) -0.0003(2) 0.0005(2) O7 0.0149(10) 0.0134(10) 0.0149(10) 0.0005(10) 0.0016(10) 0.0018(10) O8 0.0131(10) 0.0132(10) 0.0178(10) 0.0021(10) -0.0003(10) 0.0000(10) O9 0.0133(10) 0.0141(10) 0.0189(10) -0.0011(10) -0.0008(10) -0.0008(10) O10 0.0176(10) 0.0126(10) 0.0178(10) 0.0001(10) 0.0025(10) -0.0013(10) O11 0.0179(10) 0.0192(10) 0.0270(10) 0.0034(10) 0.0077(10) 0.0028(10) O12 0.0225(10) 0.0146(10) 0.0241(10) 0.0015(10) -0.0003(10) 0.0008(10) O13 0.0118(10) 0.0283(10) 0.0281(10) 0.0001(10) -0.0014(10) 0.0010(10) O14 0.0313(10) 0.0157(10) 0.0258(10) 0.0013(10) 0.0000(10) -0.0023(10) O15 0.0218(10) 0.0199(10) 0.0161(10) 0.0024(10) -0.0044(10) 0.0005(10) O16 0.0143(10) 0.0178(10) 0.0224(10) -0.0024(10) -0.0019(10) 0.0023(10) C17 0.0181(10) 0.0173(10) 0.0189(10) -0.0039(10) 0.0025(10) 0.0051(10) O18 0.0187(10) 0.0164(10) 0.0218(10) -0.0018(10) -0.0008(10) -0.0015(10) C19 0.025(2) 0.024(2) 0.025(2) -0.0066(10) -0.0036(10) 0.0015(10) O20 0.0201(10) 0.0174(10) 0.0195(10) 0.0018(10) 0.0022(10) -0.0041(10) C21 0.0156(10) 0.0201(10) 0.022(2) 0.0069(10) 0.0005(10) -0.0003(10) O22 0.0171(10) 0.0211(10) 0.0189(10) 0.0017(10) 0.0033(10) 0.0000(10) C23 0.033(2) 0.029(2) 0.024(2) 0.0035(10) 0.0033(10) -0.0061(10) O24 0.0137(10) 0.0211(10) 0.0201(10) -0.0004(10) 0.0027(10) 0.0033(10) C25 0.0145(10) 0.0172(10) 0.0218(10) -0.0045(10) -0.0033(10) 0.0015(10) O26 0.0197(10) 0.0154(10) 0.0241(10) -0.0021(10) 0.0019(10) 0.0043(10) C27 0.029(2) 0.034(2) 0.028(2) 0.0013(10) 0.0027(10) 0.0104(10) O28 0.0151(10) 0.0165(10) 0.0304(10) 0.0035(10) 0.0030(10) 0.0053(10) C29 0.0184(10) 0.0217(10) 0.0201(10) 0.0058(10) 0.0047(10) 0.0010(10) O30 0.0152(10) 0.0195(10) 0.0264(10) 0.0044(10) 0.0000(10) 0.0051(10) C31 0.0183(10) 0.028(2) 0.042(2) 0.0058(10) 0.0019(10) 0.0094(10) N32 0.0185(10) 0.0124(10) 0.0212(10) 0.0009(10) 0.0014(10) 0.0008(10) C33 0.036(2) 0.0115(10) 0.028(2) 0.0029(10) -0.0074(10) 0.0020(10) C34 0.075(3) 0.022(2) 0.026(2) -0.012(2) -0.007(2) 0.0046(10) C35 0.0131(10) 0.026(2) 0.025(2) -0.0022(10) 0.0016(10) 0.0043(10) C36 0.044(2) 0.058(2) 0.025(2) -0.025(2) 0.010(2) -0.009(2) C37 0.0176(10) 0.026(2) 0.043(2) -0.0009(10) 0.0080(10) 0.0071(10) C38 0.014(2) 0.047(2) 0.102(4) -0.000(2) -0.002(2) 0.036(2) C39 0.043(2) 0.0165(10) 0.034(2) -0.0013(10) 0.0124(10) -0.0053(10) C40 0.074(3) 0.024(2) 0.030(2) -0.014(2) -0.006(2) -0.0091(10) N41 0.015(2) 0.018(2) 0.017(2) 0 0.0003(10) 0 C42 0.0193(10) 0.025(2) 0.0218(10) 0.0028(10) 0.0008(10) -0.0025(10) C43 0.029(2) 0.027(2) 0.025(2) 0.0097(10) -0.0036(10) -0.0043(10) C44 0.0184(10) 0.023(2) 0.026(2) 0.0009(10) -0.0049(10) -0.0048(10) C45 0.027(2) 0.037(2) 0.047(2) 0.0069(10) -0.011(2) -0.023(2) N46 0.067(3) 0.017(2) 0.013(2) 0 0.000(2) 0 C47 0.045(2) 0.020(2) 0.020(2) 0.0051(10) 0.0036(10) 0.0030(10) C48 0.064(2) 0.036(2) 0.019(2) 0.015(2) 0.001(2) 0.0025(10) C49 0.126(4) 0.028(2) 0.024(2) 0.037(2) 0.005(2) 0.007(2) C50 0.082(3) 0.069(3) 0.036(2) 0.048(3) -0.012(2) -0.007(2) C51 0.038(2) 0.051(2) 0.020(2) -0.010(2) 0.0016(10) 0.0008(10) C52 0.029(2) 0.036(2) 0.034(2) 0.0045(10) 0.0052(10) 0.0089(10) N53 0.034(2) 0.087(3) 0.083(3) -0.008(2) 0.006(2) 0.021(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 V5 2.9031(7) . . no N53 C52 1.114(5) . 1_456 no V1 CL6 2.9260(8) . . no C17 C19 1.496(4) . . no V1 O7 1.9672(18) . . no C21 C23 1.503(4) . . no V1 O10 1.9661(19) . . no C25 C27 1.512(4) . . no V1 O11 1.5953(19) . . no C29 C31 1.509(4) . . no V1 O16 2.0182(19) . . no C33 C34 1.502(5) . 1_565 no V1 O30 2.0236(19) . . no C35 C36 1.507(5) . . no V2 V5 2.9001(7) . . no C37 C38 1.508(5) . . no V2 CL6 3.0153(8) . . no C39 C40 1.505(5) . 1_565 no V2 O7 1.9517(18) . . no C42 C43 1.514(4) . . no V2 O8 1.9588(18) . . no C44 C45 1.510(4) . . no V2 O12 1.5986(19) . 1_545 no C47 C48 1.514(4) . . no V2 O18 2.0121(19) . . no C49 C50 1.502(7) . . no V2 O20 2.0123(19) . . no C51 C52 1.443(5) . . no V3 V5 2.9030(7) . . no V3 CL6 2.9284(8) . . no V3 O8 1.9624(18) . . no V3 O9 1.9620(19) . . no V3 O13 1.5984(19) . . no V3 O22 2.018(2) . . no V3 O24 2.0152(19) . . no V4 V5 2.9089(7) . . no V4 CL6 2.9513(8) . . no V4 O9 1.9616(18) . . no V4 O10 1.9596(19) . . no V4 O14 1.596(2) . . no V4 O26 2.020(2) . . no V4 O28 2.0162(19) . . no V5 O7 1.8770(18) . . no V5 O8 1.8834(18) . . no V5 O9 1.8785(18) . . no V5 O10 1.8845(18) . . no V5 O15 1.6098(19) . . no O16 C17 1.261(3) . . no O18 C17 1.264(3) . . no O20 C21 1.261(3) . . no O22 C21 1.256(3) . . no O24 C25 1.260(3) . . no O26 C25 1.257(3) . . no O28 C29 1.257(3) . . no O30 C29 1.264(3) . . no N32 C33 1.520(3) . 1_545 no N32 C35 1.517(3) . 1_545 no N32 C37 1.523(4) . 1_545 no N32 C39 1.517(4) . 1_545 no N41 C42 1.525(3) . . no N41 C42 1.525(3) . 3_655 no N41 C44 1.522(3) . . no N41 C44 1.522(3) . 3_655 no N46 C47 1.517(4) . . no N46 C47 1.517(4) . 3_755 no N46 C49 1.528(5) . . no N46 C49 1.528(5) . 3_755 no C19 H1 0.951(3) . . no C50 H51 0.948(4) . . no C19 H2 0.946(3) . . no C50 H52 0.949(4) . . no C19 H3 0.951(3) . . no C51 H53 0.950(3) . . no C23 H4 0.950(3) . 1_545 no C51 H54 0.950(4) . 1_554 no C23 H5 0.951(3) . . no C51 H55 0.950(4) . 1_554 no C23 H6 0.951(3) . . no C27 H7 0.948(3) . . no C27 H8 0.950(3) . . no C27 H9 0.949(3) . . no C31 H10 0.950(3) . . no C31 H11 0.950(3) . . no C31 H12 0.948(3) . . no C33 H13 0.951(3) . . no C33 H14 0.951(3) . 1_565 no C34 H15 0.949(4) . . no C34 H16 0.949(3) . . no C34 H17 0.950(4) . 1_545 no C35 H18 0.950(3) . 1_565 no C35 H19 0.951(3) . 1_565 no C36 H20 0.952(4) . . no C36 H21 0.948(4) . 1_565 no C36 H22 0.950(3) . . no C37 H23 0.950(3) . 1_565 no C37 H24 0.950(3) . 1_565 no C38 H25 0.950(5) . 1_565 no C38 H26 0.949(5) . . no C38 H27 0.948(3) . 1_565 no C39 H28 0.949(3) . 1_565 no C39 H29 0.950(3) . . no C40 H30 0.950(4) . . no C40 H31 0.950(3) . 1_545 no C40 H32 0.951(4) . . no C42 H33 0.950(3) . . no C42 H34 0.949(3) . . no C43 H35 0.948(3) . . no C43 H36 0.951(3) . . no C43 H37 0.950(3) . . no C44 H38 0.949(3) . . no C44 H39 0.950(3) . . no C45 H40 0.949(3) . . no C45 H41 0.950(4) . . no C45 H42 0.949(4) . . no C47 H43 0.949(3) . . no C47 H44 0.951(3) . . no C48 H45 0.949(4) . . no C48 H46 0.950(4) . . no C48 H47 0.951(3) . . no C49 H48 0.950(4) . . no C49 H49 0.950(4) . . no C50 H50 0.949(4) . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag V5 V1 CL6 66.62(2) . . . no V5 V1 O7 39.81(5) . . . no V5 V1 O10 40.02(5) . . . no V5 V1 O11 114.98(8) . . . no V5 V1 O16 125.04(6) . . . no V5 V1 O30 126.18(6) . . . no CL6 V1 O7 76.47(5) . . . no CL6 V1 O10 76.33(6) . . . no CL6 V1 O11 178.03(8) . . . no CL6 V1 O16 77.42(6) . . . no CL6 V1 O30 81.93(6) . . . no O7 V1 O10 79.16(8) . . . no O7 V1 O11 103.97(9) . . . no O7 V1 O16 93.42(8) . . . no O7 V1 O30 158.07(8) . . . no O10 V1 O11 105.64(9) . . . no O10 V1 O16 153.71(8) . . . no O10 V1 O30 92.14(8) . . . no O11 V1 O16 100.62(9) . . . no O11 V1 O30 97.74(9) . . . no O16 V1 O30 85.53(8) . . . no V5 V2 CL6 65.49(2) . . . no V5 V2 O7 39.81(5) . . . no V5 V2 O8 40.03(5) . . . no V5 V2 O12 114.97(7) . . 1_545 no V5 V2 O18 125.12(6) . . . no V5 V2 O20 124.69(6) . . . no CL6 V2 O7 74.41(5) . . . no CL6 V2 O8 74.32(5) . . . no CL6 V2 O12 178.71(8) . . 1_545 no CL6 V2 O18 79.82(6) . . . no CL6 V2 O20 77.94(6) . . . no O7 V2 O8 79.50(7) . . . no O7 V2 O12 106.74(9) . . 1_545 no O7 V2 O18 91.96(8) . . . no O7 V2 O20 152.33(8) . . . no O8 V2 O12 105.23(9) . . 1_545 no O8 V2 O18 154.07(8) . . . no O8 V2 O20 92.16(8) . . . no O12 V2 O18 100.67(9) 1_545 . . no O12 V2 O20 100.90(9) 1_545 . . no O18 V2 O20 84.12(8) . . . no V5 V3 CL6 66.59(2) . . . no V5 V3 O8 39.98(5) . . . no V5 V3 O9 39.83(5) . . . no V5 V3 O13 114.61(8) . . . no V5 V3 O22 125.38(6) . . . no V5 V3 O24 125.46(6) . . . no CL6 V3 O8 76.46(5) . . . no CL6 V3 O9 75.66(5) . . . no CL6 V3 O13 177.93(8) . . . no CL6 V3 O22 80.45(5) . . . no CL6 V3 O24 77.73(5) . . . no O8 V3 O9 79.24(8) . . . no O8 V3 O13 105.55(9) . . . no O8 V3 O22 92.03(8) . . . no O8 V3 O24 154.17(8) . . . no O9 V3 O13 104.13(9) . . . no O9 V3 O22 155.88(8) . . . no O9 V3 O24 93.30(8) . . . no O13 V3 O22 99.86(9) . . . no O13 V3 O24 100.24(9) . . . no O22 V3 O24 84.82(8) . . . no V5 V4 CL6 66.22(2) . . . no V5 V4 O9 39.70(5) . . . no V5 V4 O10 39.87(5) . . . no V5 V4 O14 115.12(8) . . . no V5 V4 O26 125.12(6) . . . no V5 V4 O28 126.07(6) . . . no CL6 V4 O9 75.09(5) . . . no CL6 V4 O10 75.77(6) . . . no CL6 V4 O14 178.23(8) . . . no CL6 V4 O26 77.56(6) . . . no CL6 V4 O28 81.84(6) . . . no O9 V4 O10 79.09(8) . . . no O9 V4 O14 105.15(9) . . . no O9 V4 O26 93.08(8) . . . no O9 V4 O28 156.69(8) . . . no O10 V4 O14 106.00(9) . . . no O10 V4 O26 153.31(8) . . . no O10 V4 O28 92.21(8) . . . no O14 V4 O26 100.67(9) . . . no O14 V4 O28 98.01(9) . . . no O26 V4 O28 85.04(8) . . . no V1 V5 V2 73.524(16) . . . no V1 V5 V3 114.12(2) . . . no V1 V5 V4 72.933(17) . . . no V1 V5 O7 42.14(5) . . . no V1 V5 O8 111.94(6) . . . no V1 V5 O9 111.49(6) . . . no V1 V5 O10 42.14(6) . . . no V1 V5 O15 124.39(7) . . . no V2 V5 V3 73.715(17) . . . no V2 V5 V4 116.52(2) . . . no V2 V5 O7 41.73(5) . . . no V2 V5 O8 41.98(5) . . . no V2 V5 O9 112.98(6) . . . no V2 V5 O10 113.20(6) . . . no V2 V5 O15 121.32(7) . . . no V3 V5 V4 73.339(17) . . . no V3 V5 O7 111.97(6) . . . no V3 V5 O8 42.02(6) . . . no V3 V5 O9 41.99(6) . . . no V3 V5 O10 112.08(6) . . . no V3 V5 O15 121.50(7) . . . no V4 V5 O7 112.38(6) . . . no V4 V5 O8 112.58(6) . . . no V4 V5 O9 41.84(5) . . . no V4 V5 O10 41.80(6) . . . no V4 V5 O15 122.14(7) . . . no O7 V5 O8 83.35(8) . . . no O7 V5 O9 139.97(8) . . . no O7 V5 O10 83.56(8) . . . no O7 V5 O15 110.83(9) . . . no O8 V5 O9 83.40(8) . . . no O8 V5 O10 140.51(8) . . . no O8 V5 O15 108.89(9) . . . no O9 V5 O10 83.13(8) . . . no O9 V5 O15 109.19(9) . . . no O10 V5 O15 110.60(9) . . . no V1 CL6 V2 71.528(19) . . . no V1 CL6 V3 112.67(3) . . . no V1 CL6 V4 71.99(2) . . . no V2 CL6 V3 71.680(19) . . . no V2 CL6 V4 111.78(3) . . . no V3 CL6 V4 72.357(19) . . . no V1 O7 V2 124.81(9) . . . no V1 O7 V5 98.05(8) . . . no V2 O7 V5 98.46(8) . . . no V2 O8 V3 125.17(9) . . . no V2 O8 V5 98.00(8) . . . no V3 O8 V5 98.00(8) . . . no V3 O9 V4 124.41(9) . . . no V3 O9 V5 98.19(8) . . . no V4 O9 V5 98.47(8) . . . no V1 O10 V4 123.27(10) . . . no V1 O10 V5 97.84(8) . . . no V4 O10 V5 98.33(8) . . . no V1 O16 C17 134.36(18) . . . no V2 O18 C17 135.22(18) . . . no V2 O20 C21 135.16(18) . . . no V3 O22 C21 134.08(18) . . . no V3 O24 C25 134.23(18) . . . no V4 O26 C25 134.37(18) . . . no V4 O28 C29 134.35(18) . . . no V1 O30 C29 133.86(18) . . . no C33 N32 C35 109.1(2) 1_545 . 1_545 no C33 N32 C37 109.0(2) 1_545 . 1_545 no C33 N32 C39 111.2(2) 1_545 . 1_545 no C35 N32 C37 110.8(2) 1_545 . 1_545 no C35 N32 C39 107.4(2) 1_545 . 1_545 no C37 N32 C39 109.3(2) 1_545 . 1_545 no C42 N41 C42 110.8(3) . . 3_655 no C42 N41 C42 110.8(3) 3_655 . . no C42 N41 C44 108.71(15) . . . no C42 N41 C44 108.71(15) . . 3_655 no C42 N41 C44 108.71(15) 3_655 . . no C42 N41 C44 108.71(15) 3_655 . 3_655 no C42 N41 C44 108.85(16) . . . no C42 N41 C44 108.85(16) . . 3_655 no C42 N41 C44 108.85(16) 3_655 . . no C42 N41 C44 108.85(16) 3_655 . 3_655 no C44 N41 C44 110.9(3) . . 3_655 no C44 N41 C44 110.9(3) 3_655 . . no C47 N46 C47 105.7(3) . . 3_755 no C47 N46 C47 105.7(3) 3_755 . . no C47 N46 C49 110.6(2) . . 3_755 no C47 N46 C49 110.6(2) 3_755 . . no C47 N46 C49 111.02(19) . . . no C47 N46 C49 111.02(19) 3_755 . 3_755 no C49 N46 C49 108.0(4) . . 3_755 no C49 N46 C49 108.0(4) 3_755 . . no O16 C17 O18 125.6(3) . . . no O16 C17 C19 117.5(3) . . . no O18 C17 C19 116.9(3) . . . no O20 C21 O22 126.4(3) . . . no O20 C21 C23 116.7(3) . . . no O22 C21 C23 116.9(3) . . . no O24 C25 O26 126.4(3) . . . no O24 C25 C27 116.4(3) . . . no O26 C25 C27 117.1(3) . . . no O28 C29 O30 126.1(3) . . . no O28 C29 C31 117.2(3) . . . no O30 C29 C31 116.6(3) . . . no N32 C33 C34 114.9(3) 1_565 . 1_565 no N32 C35 C36 114.2(2) 1_565 . . no N32 C37 C38 114.9(3) 1_565 . . no N32 C39 C40 115.4(3) 1_565 . 1_565 no N41 C42 C43 115.5(2) . . . no N41 C42 C43 115.5(2) 3_655 . . no N41 C44 C45 115.1(2) . . . no N41 C44 C45 115.1(2) 3_655 . . no N46 C47 C48 114.7(3) . . . no N46 C47 C48 114.7(3) 3_755 . . no N46 C49 C50 116.5(3) . . . no N46 C49 C50 116.5(3) 3_755 . . no N53 C52 C51 178.2(4) 1_654 . . no C17 C19 H1 109.2(3) . . . no C17 C19 H2 109.5(3) . . . no C17 C19 H3 109.4(3) . . . no H1 C19 H2 109.7(3) . . . no H1 C19 H3 109.3(3) . . . no H2 C19 H3 109.7(3) . . . no C21 C23 H4 109.5(3) . . 1_545 no C21 C23 H5 109.6(3) . . . no C21 C23 H6 109.6(3) . . . no H4 C23 H5 109.4(3) 1_545 . . no H4 C23 H6 109.4(3) 1_545 . . no H5 C23 H6 109.3(3) . . . no C25 C27 H7 109.5(3) . . . no C25 C27 H8 109.1(3) . . . no C25 C27 H9 109.2(3) . . . no H7 C27 H8 109.7(3) . . . no H7 C27 H9 109.8(3) . . . no H8 C27 H9 109.6(3) . . . no C29 C31 H10 109.3(3) . . . no C29 C31 H11 109.4(3) . . . no C29 C31 H12 109.4(3) . . . no H10 C31 H11 109.5(3) . . . no H10 C31 H12 109.6(3) . . . no H11 C31 H12 109.6(3) . . . no N32 C33 H13 108.1(3) 1_565 . . no N32 C33 H14 108.1(3) 1_565 . 1_565 no C34 C33 H13 108.2(3) 1_565 . . no C34 C33 H14 108.2(3) 1_565 . 1_565 no H13 C33 H14 109.4(3) . . 1_565 no C33 C34 H15 109.4(3) 1_545 . . no C33 C34 H16 109.4(3) 1_545 . . no C33 C34 H17 109.4(4) 1_545 . 1_545 no H15 C34 H16 109.6(4) . . . no H15 C34 H17 109.5(3) . . 1_545 no H16 C34 H17 109.5(3) . . 1_545 no N32 C35 H18 108.3(3) 1_565 . 1_565 no N32 C35 H19 108.2(2) 1_565 . 1_565 no C36 C35 H18 108.3(3) . . 1_565 no C36 C35 H19 108.4(3) . . 1_565 no H18 C35 H19 109.4(3) 1_565 . 1_565 no C35 C36 H20 109.4(3) . . . no C35 C36 H21 109.6(3) . . 1_565 no C35 C36 H22 109.5(3) . . . no H20 C36 H21 109.5(3) . . 1_565 no H20 C36 H22 109.3(4) . . . no H21 C36 H22 109.6(4) 1_565 . . no N32 C37 H23 108.2(3) 1_565 . 1_565 no N32 C37 H24 108.2(3) 1_565 . 1_565 no C38 C37 H23 108.0(3) . . 1_565 no C38 C37 H24 108.1(3) . . 1_565 no H23 C37 H24 109.5(3) 1_565 . 1_565 no C37 C38 H25 109.3(3) . . 1_565 no C37 C38 H26 109.3(4) . . . no C37 C38 H27 109.4(3) . . 1_565 no H25 C38 H26 109.5(4) 1_565 . . no H25 C38 H27 109.6(5) 1_565 . 1_565 no H26 C38 H27 109.7(4) . . 1_565 no N32 C39 H28 108.1(3) 1_565 . 1_565 no N32 C39 H29 108.0(3) 1_565 . . no C40 C39 H28 107.8(3) 1_565 . 1_565 no C40 C39 H29 107.8(3) 1_565 . . no H28 C39 H29 109.6(3) 1_565 . . no C39 C40 H30 109.5(3) 1_545 . . no C39 C40 H31 109.5(4) 1_545 . 1_545 no C39 C40 H32 109.5(3) 1_545 . . no H30 C40 H31 109.5(3) . . 1_545 no H30 C40 H32 109.4(4) . . . no H31 C40 H32 109.4(3) 1_545 . . no N41 C42 H33 107.9(2) . . . no N41 C42 H33 107.9(2) 3_655 . . no N41 C42 H34 108.0(3) . . . no N41 C42 H34 108.0(3) 3_655 . . no C43 C42 H33 107.8(3) . . . no C43 C42 H34 107.9(3) . . . no H33 C42 H34 109.5(3) . . . no C42 C43 H35 109.5(3) . . . no C42 C43 H36 109.4(3) . . . no C42 C43 H37 109.4(3) . . . no H35 C43 H36 109.6(3) . . . no H35 C43 H37 109.6(3) . . . no H36 C43 H37 109.4(3) . . . no N41 C44 H38 108.1(3) . . . no N41 C44 H38 108.1(3) 3_655 . . no N41 C44 H39 108.0(2) . . . no N41 C44 H39 108.0(2) 3_655 . . no C45 C44 H38 108.0(3) . . . no C45 C44 H39 107.9(3) . . . no H38 C44 H39 109.6(3) . . . no C44 C45 H40 109.4(3) . . . no C44 C45 H41 109.4(3) . . . no C44 C45 H42 109.4(3) . . . no H40 C45 H41 109.5(3) . . . no H40 C45 H42 109.6(4) . . . no H41 C45 H42 109.5(3) . . . no N46 C47 H43 108.2(3) . . . no N46 C47 H43 108.2(3) 3_755 . . no N46 C47 H44 108.1(3) . . . no N46 C47 H44 108.1(3) 3_755 . . no C48 C47 H43 108.3(3) . . . no C48 C47 H44 108.1(3) . . . no H43 C47 H44 109.4(3) . . . no C47 C48 H45 109.6(3) . . . no C47 C48 H46 109.4(3) . . . no C47 C48 H47 109.4(3) . . . no H45 C48 H46 109.6(3) . . . no H45 C48 H47 109.5(4) . . . no H46 C48 H47 109.4(4) . . . no N46 C49 H48 107.7(4) . . . no N46 C49 H48 107.7(4) 3_755 . . no N46 C49 H49 107.7(4) . . . no N46 C49 H49 107.7(4) 3_755 . . no C50 C49 H48 107.7(4) . . . no C50 C49 H49 107.6(5) . . . no H48 C49 H49 109.4(4) . . . no C49 C50 H50 109.2(5) . . . no C49 C50 H51 109.3(4) . . . no C49 C50 H52 109.2(4) . . . no H50 C50 H51 109.7(4) . . . no H50 C50 H52 109.7(4) . . . no H51 C50 H52 109.7(5) . . . no C52 C51 H53 109.4(3) . . . no C52 C51 H54 109.4(3) . . 1_554 no C52 C51 H55 109.5(3) . . 1_554 no H53 C51 H54 109.5(4) . . 1_554 no H53 C51 H55 109.5(3) . . 1_554 no H54 C51 H55 109.5(3) 1_554 . 1_554 no # The following lines may be used to test the character set of files sent by # network email or other means. They are not part of the CIF data archive. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ #===END ############################################################################## # IUMSC CIF Archive file # ############################################################################## data_MSC95206 _audit_creation_method 'minor manual editing of SDT2CIF v. 1.1 BETA output' _chemical_formula_sum 'C38 H81 N5 O29 V9' _chemical_formula_moiety ? _chemical_formula_weight 1530.55 _cell_length_a 13.3031(10) _cell_length_b 23.0313(18) _cell_length_c 10.8035(9) _cell_angle_alpha 90.813(5) _cell_angle_beta 111.914(4) _cell_angle_gamma 94.151(5) _cell_volume 3059.8(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 102 _cell_measurement_theta_min 9.68 _cell_measurement_theta_max 12.52 _cell_measurement_temperature ? _exptl_crystal_colour ? _exptl_crystal_description ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_diffrn 1.661 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1566 _exptl_absorpt_coefficient_mu 1.3933 _exptl_absorpt_correction_type none _exptl_absorpt_process_details none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature ? _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max ? _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min ? _diffrn_reflns_limit_h_max ? _diffrn_reflns_limit_k_min ? _diffrn_reflns_limit_k_max ? _diffrn_reflns_limit_l_min ? _diffrn_reflns_limit_l_max ? _diffrn_standards_number ? _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _reflns_number_total ? _reflns_number_gt ? _reflns_threshold_expression F^2^>2.33\s(F^2^) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source V V 0.267 0.53 'International Tables Vol. IV (1974) Table 2.2B' O O 0.008 0.006 'International Tables Vol. IV (1974) Table 2.2B' N N 0.004 0.003 'International Tables Vol. IV (1974) Table 2.2B' C C 0.002 0.002 'International Tables Vol. IV (1974) Table 2.2B' H H 0 0 'International Tables Vol. IV (1974) Table 2.2B' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_number_reflns ? _refine_ls_number_parameters ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_coef 0.5741E-7 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_expression ; Larson, A. C. (1967). Acta Cryst. 23, p. 664. Eq. (3) ; _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack ? _refine_ls_weighting_scheme calc _refine_ls_weighting_details w^-1^=\s^2^(F)+(.04F)^2^ _refine_ls_R_factor_gt ? _refine_ls_wR_factor_ref ? _refine_ls_goodness_of_fit_ref ? _refine_ls_shift/su_max ? _refine_diff_density_max ? _refine_diff_density_min ? _computing_data_collection 'NPS, local program' _computing_cell_refinement 'XTEL, local package' _computing_data_reduction 'XTEL, local package' _computing_structure_solution MULTAN78 _computing_structure_refinement 'XTEL, local package' _computing_molecular_graphics 'XTEL, local package' _computing_publication_material 'XTEL, local package' 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_disorder_group _atom_site_disorder_assembly V1 V 0.65791(10) 0.21795(10) 0.19805(10) 0.0106(7) Uani 1 0 . V2 V 0.62340(10) 0.25385(10) 0.49351(10) 0.0112(7) Uani 1 0 . V3 V 0.53461(10) 0.14865(10) 0.32435(10) 0.0110(7) Uani 1 0 . V4 V 0.39267(10) 0.15658(10) 0.04666(10) 0.0109(7) Uani 1 0 . V5 V 0.34246(10) 0.19194(10) 0.34892(10) 0.0103(7) Uani 1 0 . V6 V 0.41440(10) 0.34485(10) 0.46676(10) 0.0131(7) Uani 1 0 . V7 V 0.20664(10) 0.28969(10) 0.29187(10) 0.0135(7) Uani 1 0 . V8 V 0.18192(10) 0.24623(10) 0.02571(10) 0.0130(7) Uani 1 0 . V9 V 0.24570(10) 0.38954(10) 0.15309(10) 0.0137(7) Uani 1 0 . O10 O 0.7639(4) 0.1884(2) 0.2006(5) 0.017(2) Uani 1 0 . O11 O 0.6585(4) 0.2018(2) 0.3767(5) 0.010(2) Uani 1 0 . O12 O 0.5462(4) 0.1515(2) 0.1581(5) 0.012(2) Uani 1 0 . O13 O 0.6976(4) 0.2407(2) 0.6426(5) 0.016(2) Uani 1 0 . O14 O 0.5011(4) 0.1945(2) 0.4460(5) 0.013(2) Uani 1 0 . O15 O 0.5379(4) 0.3090(2) 0.5028(5) 0.014(2) Uani 1 0 . O16 O 0.5673(4) 0.0868(2) 0.3860(5) 0.017(2) Uani 1 0 . O17 O 0.3848(4) 0.1460(2) 0.2227(5) 0.012(2) Uani 1 0 . O18 O 0.3467(4) 0.0949(2) -0.0305(5) 0.017(2) Uani 1 0 . O19 O 0.2766(4) 0.2011(2) 0.0021(5) 0.016(2) Uani 1 0 . O20 O 0.2905(4) 0.1443(2) 0.4187(5) 0.013(2) Uani 1 0 . O21 O 0.3328(4) 0.2681(2) 0.4273(5) 0.011(2) Uani 1 0 . O22 O 0.2163(4) 0.2196(2) 0.2065(5) 0.013(2) Uani 1 0 . O23 O 0.4159(4) 0.3667(2) 0.6082(5) 0.019(2) Uani 1 0 . O24 O 0.2761(4) 0.3647(2) 0.3360(5) 0.015(2) Uani 1 0 . O25 O 0.1077(4) 0.2842(2) 0.3419(5) 0.020(2) Uani 1 0 . O26 O 0.1573(4) 0.3151(2) 0.1153(5) 0.012(2) Uani 1 0 . O27 O 0.0645(4) 0.2141(2) -0.0557(5) 0.017(2) Uani 1 0 . O28 O 0.1592(4) 0.4356(2) 0.1373(5) 0.018(2) Uani 1 0 . O29 O 0.7275(4) 0.3002(2) 0.2544(5) 0.017(2) Uani 1 0 . O30 O 0.7193(4) 0.3164(2) 0.4563(5) 0.018(2) Uani 1 0 . C31 C 0.7501(6) 0.3300(3) 0.3618(8) 0.017(3) Uani 1 0 . C32 C 0.8222(8) 0.3847(4) 0.3820(9) 0.029(4) Uani 1 0 . O33 O 0.6066(4) 0.2414(2) 0.0057(5) 0.016(2) Uani 1 0 . O34 O 0.4399(4) 0.1965(2) -0.0875(5) 0.014(2) Uani 1 0 . C35 C 0.5187(7) 0.2280(3) -0.0932(8) 0.016(3) Uani 1 0 . C36 C 0.5080(6) 0.2532(4) -0.2227(8) 0.021(3) Uani 1 0 . O37 O 0.4848(4) 0.4153(2) 0.4151(5) 0.019(2) Uani 1 0 . O38 O 0.3820(4) 0.4442(2) 0.2122(5) 0.015(2) Uani 1 0 . C39 C 0.4667(6) 0.4479(3) 0.3167(8) 0.016(3) Uani 1 0 . C40 C 0.5536(7) 0.4953(4) 0.3261(9) 0.029(4) Uani 1 0 . O41 O 0.2468(4) 0.3908(2) -0.0323(5) 0.019(2) Uani 1 0 . O42 O 0.1961(4) 0.2983(2) -0.1154(5) 0.017(2) Uani 1 0 . C43 C 0.2201(6) 0.3518(4) -0.1258(8) 0.016(3) Uani 1 0 . C44 C 0.2165(7) 0.3711(4) -0.2577(8) 0.025(4) Uani 1 0 . O45 O 0.5034(4) 0.2619(2) 0.1962(5) 0.015(2) Uani 1 0 . O46 O 0.3735(4) 0.3184(2) 0.1836(5) 0.018(2) Uani 1 0 . C47 C 0.4560(7) 0.3067(4) 0.1587(8) 0.020(3) Uani 1 0 . C48 C 0.4940(7) 0.3497(4) 0.0779(10) 0.030(4) Uani 1 0 . N49 N 0.6588(5) 0.0706(3) 0.8380(6) 0.012(3) Uani 1 0 . C50 C 0.6477(6) 0.0060(3) 0.7971(8) 0.019(3) Uani 1 0 . C51 C 0.6599(7) -0.0076(4) 0.6674(8) 0.023(3) Uani 1 0 . C52 C 0.7749(7) 0.0952(4) 0.8616(9) 0.026(3) Uani 1 0 . C53 C 0.8040(7) 0.1575(4) 0.9133(8) 0.023(3) Uani 1 0 . C54 C 0.6345(6) 0.0782(3) 0.9632(8) 0.019(3) Uani 1 0 . C55 C 0.7105(7) 0.0522(4) 1.0874(8) 0.025(3) Uani 1 0 . C56 C 0.5807(7) 0.1036(4) 0.7286(9) 0.030(4) Uani 1 0 . C57 C 0.4620(7) 0.0814(4) 0.6855(9) 0.032(4) Uani 1 0 . N58 N 0.8215(5) 0.3836(3) 0.9033(6) 0.019(3) Uani 1 0 . C59 C 0.8359(7) 0.4367(4) 0.9958(8) 0.024(3) Uani 1 0 . C60 C 0.7403(8) 0.4490(4) 1.0274(9) 0.036(4) Uani 1 0 . C61 C 0.9238(6) 0.3830(4) 0.8734(8) 0.027(4) Uani 1 0 . C62 C 0.9237(7) 0.3337(5) 0.7800(9) 0.032(4) Uani 1 0 . C63 C 0.7214(6) 0.3861(4) 0.7755(8) 0.021(3) Uani 1 0 . C64 C 0.7259(7) 0.4351(4) 0.6879(8) 0.024(3) Uani 1 0 . C65 C 0.8037(6) 0.3276(4) 0.9686(8) 0.020(3) Uani 1 0 . C66 C 0.8975(7) 0.3127(4) 1.0913(9) 0.023(3) Uani 1 0 . N67 N 0.0332(5) 0.1487(3) 0.5716(7) 0.022(3) Uani 1 0 . C68 C -0.0498(14) 0.1250(8) 0.6180(17) 0.022(7) Uani 0.485 0 . C69 C 0.0840(13) 0.0999(8) 0.5151(19) 0.026(9) Uani 0.485 0 . C70 C -0.0094(13) 0.1877(8) 0.4519(15) 0.020(8) Uani 0.485 0 . C71 C 0.1235(14) 0.1792(7) 0.6837(16) 0.021(7) Uani 0.485 0 . C68 C -0.0599(12) 0.1161(7) 0.4647(17) 0 Uiso 0.515 0 . C69 C 0.0766(15) 0.1130(9) 0.700(2) 0 Uiso 0.515 0 . C70 C -0.0151(14) 0.2024(8) 0.6274(18) 0 Uiso 0.515 0 . C71 C 0.1143(13) 0.1704(7) 0.5245(18) 0 Uiso 0.515 0 . C72 C -0.1564(7) 0.0946(5) 0.5018(10) 0.039(4) Uani 1 0 . C73 C 0.1344(10) 0.0577(5) 0.6420(17) 0.094(7) Uani 1 0 . C74 C -0.0547(8) 0.2442(5) 0.5064(13) 0.057(5) Uani 1 0 . C75 C 0.2165(7) 0.2054(4) 0.6435(9) 0.030(4) Uani 1 0 . N76 N 0.9769(6) 0.5162(4) 0.3182(8) 0.033(3) Uani 1 0 . C77 C 1.0376(7) 0.4828(4) 0.3637(8) 0.021(3) Uani 1 0 . C78 C 1.1164(8) 0.4415(4) 0.4225(10) 0.035(4) Uani 1 0 . N79 N 0.0312(8) 0.0049(5) 0.1945(11) 0.067(5) Uani 1 0 . C80 C 0.0622(8) 0.0442(5) 0.1518(12) 0.046(5) Uani 1 0 . C81 C 0.1031(9) 0.0916(4) 0.0925(12) 0.054(5) Uani 1 0 . H1 H 0.8775 0.3863 0.4692 0.0432 Uiso 1 0 . H2 H 0.8555 0.3853 0.3177 0.0432 Uiso 1 0 . H3 H 0.7811 0.4175 0.3724 0.0432 Uiso 1 0 . H4 H 0.578 0.2608 -0.2271 0.0324 Uiso 1 0 . H5 H 0.4647 0.227 -0.2945 0.0324 Uiso 1 0 . H6 H 0.4744 0.289 -0.2312 0.0324 Uiso 1 0 . H7 H 0.6186 0.4884 0.3982 0.0407 Uiso 1 0 . H8 H 0.5664 0.4946 0.245 0.0407 Uiso 1 0 . H9 H 0.5307 0.5319 0.3397 0.0407 Uiso 1 0 . H10 H 0.2892 0.3785 -0.2538 0.0379 Uiso 1 0 . H11 H 0.1794 0.3416 -0.324 0.0379 Uiso 1 0 . H12 H 0.1807 0.4058 -0.2775 0.0379 Uiso 1 0 . H13 H 0.5706 0.3503 0.1055 0.0411 Uiso 1 0 . H14 H 0.4614 0.3372 -0.0147 0.0411 Uiso 1 0 . H15 H 0.4733 0.3869 0.0895 0.0411 Uiso 1 0 . H16 H 0.703 -0.0123 0.867 0.0304 Uiso 1 0 . H17 H 0.5787 -0.0101 0.7924 0.0304 Uiso 1 0 . H18 H 0.6524 -0.0485 0.6496 0.0359 Uiso 1 0 . H19 H 0.6056 0.01 0.5967 0.0359 Uiso 1 0 . H20 H 0.7299 0.0076 0.6713 0.0359 Uiso 1 0 . H21 H 0.8231 0.0713 0.9244 0.0384 Uiso 1 0 . H22 H 0.7842 0.0916 0.7789 0.0384 Uiso 1 0 . H23 H 0.8772 0.1686 0.9251 0.037 Uiso 1 0 . H24 H 0.7572 0.182 0.8511 0.037 Uiso 1 0 . H25 H 0.7955 0.1617 0.9966 0.037 Uiso 1 0 . H26 H 0.6364 0.1184 0.9818 0.0316 Uiso 1 0 . H27 H 0.5636 0.0602 0.9452 0.0316 Uiso 1 0 . H28 H 0.7089 0.0112 1.0726 0.0369 Uiso 1 0 . H29 H 0.7825 0.0692 1.1082 0.0369 Uiso 1 0 . H30 H 0.6885 0.0596 1.1597 0.0369 Uiso 1 0 . H31 H 0.5889 0.1429 0.758 0.0407 Uiso 1 0 . H32 H 0.6006 0.1005 0.6524 0.0407 Uiso 1 0 . H33 H 0.4408 0.0832 0.7613 0.0433 Uiso 1 0 . H34 H 0.4181 0.104 0.618 0.0433 Uiso 1 0 . H35 H 0.452 0.0415 0.6541 0.0433 Uiso 1 0 . H36 H 0.8949 0.4314 1.0766 0.0361 Uiso 1 0 . H37 H 0.8543 0.4699 0.9539 0.0361 Uiso 1 0 . H38 H 0.7583 0.4829 1.0863 0.049 Uiso 1 0 . H39 H 0.681 0.4553 0.9488 0.049 Uiso 1 0 . H40 H 0.7217 0.4169 1.0716 0.049 Uiso 1 0 . H41 H 0.9325 0.4186 0.8333 0.0397 Uiso 1 0 . H42 H 0.983 0.3807 0.9553 0.0397 Uiso 1 0 . H43 H 0.9162 0.2968 0.8179 0.0446 Uiso 1 0 . H44 H 0.8661 0.3348 0.696 0.0446 Uiso 1 0 . H45 H 0.9914 0.3358 0.7668 0.0446 Uiso 1 0 . H46 H 0.7129 0.3505 0.7252 0.0336 Uiso 1 0 . H47 H 0.6605 0.3892 0.7993 0.0336 Uiso 1 0 . H48 H 0.7341 0.4713 0.7351 0.0361 Uiso 1 0 . H49 H 0.786 0.4324 0.6606 0.0361 Uiso 1 0 . H50 H 0.6606 0.433 0.6105 0.0361 Uiso 1 0 . H51 H 0.7418 0.3302 0.9916 0.03 Uiso 1 0 . H52 H 0.7884 0.296 0.9032 0.03 Uiso 1 0 . H53 H 0.8795 0.2776 1.1253 0.0351 Uiso 1 0 . H54 H 0.9599 0.3087 1.0692 0.0351 Uiso 1 0 . H55 H 0.9142 0.3436 1.1575 0.0351 Uiso 1 0 . H56 H -0.0196 0.0961 0.6802 0.0423 Uiso 0.485 0 . H57 H -0.0711 0.1552 0.6597 0.0423 Uiso 0.485 0 . H58 H 0.0303 0.0782 0.4421 0.0418 Uiso 0.485 0 . H59 H 0.1403 0.116 0.489 0.0418 Uiso 0.485 0 . H60 H 0.0477 0.2003 0.4216 0.0408 Uiso 0.485 0 . H61 H -0.0667 0.1672 0.3784 0.0408 Uiso 0.485 0 . H62 H 0.0957 0.2096 0.7196 0.0375 Uiso 0.485 0 . H63 H 0.1526 0.1521 0.752 0.0375 Uiso 0.485 0 . H64 H -0.1885 0.1225 0.4383 0.0526 Uiso 0.485 0 . H65 H -0.1375 0.0632 0.46 0.0526 Uiso 0.485 0 . H66 H -0.2071 0.0804 0.5401 0.0526 Uiso 0.485 0 . H67 H 0.0781 0.0417 0.6681 0.1089 Uiso 0.485 0 . H68 H 0.1669 0.0262 0.6152 0.1089 Uiso 0.485 0 . H69 H 0.1883 0.0793 0.7144 0.1089 Uiso 0.485 0 . H70 H 0.0035 0.2643 0.5783 0.0721 Uiso 0.485 0 . H71 H -0.0824 0.2705 0.4361 0.0721 Uiso 0.485 0 . H72 H -0.1107 0.2311 0.5358 0.0721 Uiso 0.485 0 . H73 H 0.2456 0.176 0.6093 0.0441 Uiso 0.485 0 . H74 H 0.1886 0.2334 0.5767 0.0441 Uiso 0.485 0 . H75 H 0.2723 0.2251 0.7193 0.0441 Uiso 0.485 0 . H76 H -0.0868 0.1421 0.3919 0.0315 Uiso 0.515 0 . H77 H -0.0343 0.0839 0.434 0.0315 Uiso 0.515 0 . H78 H 0.1308 0.136 0.7708 0.0572 Uiso 0.515 0 . H79 H 0.0208 0.0983 0.7262 0.0572 Uiso 0.515 0 . H80 H -0.0731 0.1881 0.6517 0.0415 Uiso 0.515 0 . H81 H 0.0412 0.2217 0.7029 0.0415 Uiso 0.515 0 . H82 H 0.1393 0.1373 0.491 0.0312 Uiso 0.515 0 . H83 H 0.0823 0.1944 0.4518 0.0312 Uiso 0.515 0 . H84 H -0.1864 0.1269 0.5275 0.0526 Uiso 0.515 0 . H85 H -0.2108 0.0736 0.4282 0.0526 Uiso 0.515 0 . H86 H -0.1316 0.0698 0.5752 0.0526 Uiso 0.515 0 . H87 H 0.0803 0.0369 0.5666 0.1089 Uiso 0.515 0 . H88 H 0.1916 0.0736 0.6167 0.1089 Uiso 0.515 0 . H89 H 0.1631 0.0309 0.7108 0.1089 Uiso 0.515 0 . H90 H 0.0056 0.2589 0.4851 0.0721 Uiso 0.515 0 . H91 H -0.1072 0.2237 0.4304 0.0721 Uiso 0.515 0 . H92 H -0.0862 0.2762 0.5308 0.0721 Uiso 0.515 0 . H93 H 0.2469 0.1813 0.7155 0.0441 Uiso 0.515 0 . H94 H 0.2705 0.2189 0.6099 0.0441 Uiso 0.515 0 . H95 H 0.1912 0.2387 0.674 0.0441 Uiso 0.515 0 . H96 H 1.0861 0.4034 0.3895 0.0481 Uiso 1 0 . H97 H 1.1791 0.4506 0.402 0.0481 Uiso 1 0 . H98 H 1.1369 0.4438 0.5173 0.0481 Uiso 1 0 . H99 H 0.1802 0.0964 0.1353 0.0652 Uiso 1 0 . H100 H 0.0843 0.082 0.0001 0.0652 Uiso 1 0 . H101 H 0.0729 0.1262 0.1029 0.0652 Uiso 1 0 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 V1 0.0073(10) 0.0133(10) 0.0112(10) -0.0013(10) 0.0041(10) -0.0010(10) V2 0.0102(10) 0.0139(10) 0.0088(10) -0.0011(10) 0.0033(10) -0.0009(10) V3 0.0097(10) 0.0120(10) 0.0109(10) -0.0006(10) 0.0032(10) 0.0015(10) V4 0.0093(10) 0.0125(10) 0.0104(10) -0.0026(10) 0.0034(10) -0.0006(10) V5 0.0092(10) 0.0104(10) 0.0109(10) 0.0001(10) 0.0031(10) 0.0022(10) V6 0.0131(10) 0.0112(10) 0.0131(10) -0.0006(10) 0.0032(10) -0.0009(10) V7 0.0107(10) 0.0147(10) 0.0157(10) 0.0013(10) 0.0056(10) 0.0016(10) V8 0.0119(10) 0.0131(10) 0.0129(10) -0.0006(10) 0.0034(10) 0.0015(10) V9 0.0123(10) 0.0117(10) 0.0149(10) -0.0003(10) 0.0023(10) 0.0020(10) O10 0.020(3) 0.019(3) 0.014(3) 0.001(2) 0.009(3) 0.002(2) O11 0.002(3) 0.016(3) 0.009(3) 0.003(2) -0.003(2) 0.002(2) O12 0.007(3) 0.011(3) 0.017(3) 0.001(2) 0.004(2) -0.003(2) O13 0.016(3) 0.017(3) 0.012(3) -0.000(2) 0.002(2) 0.002(2) O14 0.007(3) 0.021(3) 0.012(3) -0.004(2) 0.005(2) 0.005(2) O15 0.013(3) 0.011(3) 0.011(3) -0.006(2) -0.002(2) -0.003(2) O16 0.013(3) 0.021(3) 0.015(3) -0.000(2) 0.001(2) 0.006(2) O17 0.012(3) 0.019(3) 0.007(3) -0.001(2) 0.006(2) 0.001(2) O18 0.022(3) 0.011(3) 0.016(3) -0.006(2) 0.008(3) -0.008(2) O19 0.015(3) 0.023(3) 0.010(3) 0.001(2) 0.003(2) 0.003(2) O20 0.013(3) 0.013(3) 0.016(3) 0.000(2) 0.010(2) 0.001(2) O21 0.011(3) 0.009(3) 0.011(3) -0.001(2) 0.003(2) -0.000(2) O22 0.008(3) 0.015(3) 0.012(3) 0.002(2) -0.001(2) 0.006(2) O23 0.016(3) 0.023(3) 0.017(3) 0.002(2) 0.005(3) -0.004(3) O24 0.019(3) 0.008(3) 0.018(3) 0.002(2) 0.008(3) 0.002(2) O25 0.018(3) 0.028(3) 0.018(3) 0.007(3) 0.011(3) 0.004(3) O26 0.010(3) 0.012(3) 0.013(3) 0.001(2) 0.002(2) -0.002(2) O27 0.014(3) 0.015(3) 0.018(3) -0.002(2) 0.003(2) 0.004(2) O28 0.014(3) 0.013(3) 0.023(3) 0.000(2) 0.000(3) 0.002(2) O29 0.016(3) 0.017(3) 0.017(3) -0.004(2) 0.006(3) -0.002(3) O30 0.014(3) 0.025(3) 0.013(3) -0.009(2) 0.007(3) -0.006(3) C31 0.007(4) 0.011(4) 0.026(5) -0.001(3) -0.001(4) -0.003(4) C32 0.051(6) 0.017(5) 0.030(5) -0.012(4) 0.028(5) -0.005(4) O33 0.014(3) 0.021(3) 0.011(3) -0.003(2) 0.004(3) -0.003(2) O34 0.011(3) 0.019(3) 0.013(3) -0.003(2) 0.007(2) 0.002(2) C35 0.023(5) 0.006(4) 0.021(5) 0.003(4) 0.011(4) 0.000(4) C36 0.015(5) 0.028(5) 0.021(5) -0.002(4) 0.007(4) 0.005(4) O37 0.021(3) 0.017(3) 0.013(3) -0.004(2) -0.000(3) 0.003(3) O38 0.009(3) 0.016(3) 0.013(3) -0.003(2) -0.004(3) 0.002(2) C39 0.019(5) 0.009(4) 0.021(5) 0.001(3) 0.010(4) -0.002(4) C40 0.026(5) 0.025(5) 0.031(6) -0.008(4) 0.007(4) -0.004(4) O41 0.022(3) 0.019(3) 0.017(3) 0.001(3) 0.006(3) 0.005(3) O42 0.021(3) 0.009(3) 0.021(3) -0.000(2) 0.008(3) 0.003(2) C43 0.012(4) 0.021(5) 0.016(5) 0.010(4) 0.006(4) -0.001(4) C44 0.044(6) 0.020(5) 0.020(5) 0.003(4) 0.019(4) 0.006(4) O45 0.020(3) 0.008(3) 0.020(3) 0.006(3) 0.010(3) 0.006(2) O46 0.016(3) 0.017(3) 0.025(3) 0.005(2) 0.011(3) 0.009(3) C47 0.016(5) 0.022(5) 0.020(5) -0.003(4) 0.006(4) -0.004(4) C48 0.037(6) 0.019(5) 0.049(6) 0.012(4) 0.032(5) 0.012(4) N49 0.017(4) 0.009(4) 0.014(4) 0.002(3) 0.008(3) 0.001(3) C50 0.017(5) 0.014(5) 0.025(5) -0.004(4) 0.009(4) 0.002(4) C51 0.027(5) 0.020(5) 0.021(5) 0.001(4) 0.006(4) 0.003(4) C52 0.024(5) 0.024(5) 0.033(5) 0.000(4) 0.015(4) 0.004(4) C53 0.026(5) 0.018(5) 0.025(5) -0.002(4) 0.009(4) 0.000(4) C54 0.021(5) 0.018(5) 0.016(5) 0.004(4) 0.007(4) -0.004(4) C55 0.028(5) 0.017(5) 0.024(5) 0.001(4) 0.004(4) -0.001(4) C56 0.031(5) 0.034(6) 0.019(5) 0.007(4) 0.002(4) 0.003(4) C57 0.032(6) 0.032(6) 0.022(5) 0.010(4) -0.000(4) -0.001(4) N58 0.014(4) 0.018(4) 0.016(4) -0.009(3) -0.002(3) -0.000(3) C59 0.031(5) 0.015(5) 0.020(5) -0.008(4) 0.003(4) -0.001(4) C60 0.049(6) 0.022(5) 0.030(6) -0.001(5) 0.008(5) -0.007(4) C61 0.011(5) 0.043(6) 0.021(5) -0.012(4) -0.000(4) 0.002(4) C62 0.011(5) 0.067(7) 0.025(5) 0.005(5) 0.013(4) 0.012(5) C63 0.011(4) 0.026(5) 0.018(5) 0.002(4) -0.003(4) 0.001(4) C64 0.023(5) 0.019(5) 0.025(5) -0.001(4) 0.002(4) 0.001(4) C65 0.019(5) 0.019(5) 0.022(5) -0.000(4) 0.006(4) 0.005(4) C66 0.018(5) 0.026(5) 0.030(5) -0.001(4) 0.011(4) 0.014(4) N67 0.009(4) 0.027(4) 0.026(4) -0.004(3) 0.003(3) -0.002(3) C68 0.027(9) 0.026(10) 0.020(10) 0.012(7) 0.016(8) 0.003(8) C69 0.006(11) 0.024(15) 0.042(13) -0.006(10) 0.004(10) 0.001(11) C70 0.019(11) 0.030(13) 0.004(11) -0.008(9) -0.005(9) 0.008(9) C71 0.026(9) 0.018(10) 0.016(11) 0.002(7) 0.005(9) -0.004(8) C72 0.022(5) 0.051(7) 0.044(6) -0.009(5) 0.015(5) 0.001(5) C73 0.046(8) 0.022(7) 0.161(15) -0.007(6) -0.029(8) 0.040(8) C74 0.026(6) 0.035(7) 0.095(10) 0.013(5) 0.002(6) 0.008(6) C75 0.023(5) 0.033(6) 0.034(6) -0.004(4) 0.010(4) 0.002(5) N76 0.026(5) 0.036(5) 0.033(5) -0.003(4) 0.008(4) 0.001(4) C77 0.023(5) 0.021(5) 0.020(5) -0.001(4) 0.009(4) 0.001(4) C78 0.035(6) 0.035(6) 0.041(6) 0.002(5) 0.020(5) 0.001(5) N79 0.057(7) 0.058(7) 0.080(8) -0.018(6) 0.016(6) 0.020(6) C80 0.026(6) 0.037(7) 0.065(8) 0.005(5) 0.003(6) 0.010(6) C81 0.043(7) 0.024(6) 0.075(9) -0.012(5) -0.000(6) 0.008(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 V2 3.4866(18) . . no V6 O23 1.595(5) . . no V1 V3 2.9075(18) . . no V6 O24 1.947(5) . . no V1 V4 3.4682(18) . . no V6 O37 2.005(5) . . no V1 O10 1.602(5) . . no V6 O45 4.044(5) . . no V1 O11 1.968(5) . . no V6 O46 2.946(6) . . no V1 O12 1.978(5) . . no V7 V8 2.9229(19) . . no V1 O29 2.027(5) . . no V7 V9 2.8832(19) . . no V1 O33 2.025(5) . . no V7 O21 1.874(5) . . no V1 O45 2.349(5) . . no V7 O22 1.883(5) . . no V2 V3 2.9076(18) . . no V7 O24 1.867(5) . . no V2 V5 3.6399(18) . . no V7 O25 1.597(5) . . no V2 V6 3.5309(18) . . no V7 O26 1.889(5) . . no V2 O11 1.930(5) . . no V7 O46 2.912(5) . . no V2 O13 1.591(5) . . no V8 V9 3.4788(19) . . no V2 O14 1.953(5) . . no V8 O19 1.776(5) . . no V2 O15 1.791(5) . . no V8 O22 1.952(5) . . no V2 O30 1.999(5) . . no V8 O26 1.957(5) . . no V2 O45 3.022(5) . . no V8 O27 1.596(5) . . no V2 O46 4.125(5) . . no V8 O42 2.008(5) . . no V3 V4 2.9045(18) . . no V8 O45 3.961(5) . . no V3 V5 2.9098(18) . . no V8 O46 2.869(6) . . no V3 O11 1.878(5) . . no V9 O24 1.965(5) . . no V3 O12 1.861(5) . . no V9 O26 1.954(5) . . no V3 O14 1.873(5) . . no V9 O28 1.586(5) . . no V3 O16 1.600(5) . . no V9 O38 2.016(5) . . no V3 O17 1.878(5) . . no V9 O41 2.009(5) . . no V3 O45 2.952(5) . . no V9 O46 2.384(5) . . no V4 V5 3.6612(18) . . no O29 C31 1.263(9) . . no V4 V8 3.5428(19) . . no O30 C31 1.269(10) . . no V4 O12 1.959(5) . . no O33 C35 1.270(9) . . no V4 O17 1.961(5) . . no O34 C35 1.251(9) . . no V4 O18 1.596(5) . . no O37 C39 1.267(9) . . no V4 O19 1.831(5) . . no O38 C39 1.259(9) . . no V4 O34 1.994(5) . . no O41 C43 1.270(9) . . no V4 O45 2.873(5) . . no O42 C43 1.267(9) . . no V4 O46 4.051(5) . . no O45 C47 1.242(9) . . no V5 V6 3.6626(19) . . no O46 C47 1.268(9) . . no V5 V7 2.9170(18) . . no N49 C50 1.527(10) . . no V5 V8 3.6415(18) . . no N49 C52 1.532(10) . . no V5 O14 1.971(5) . . no N49 C54 1.515(10) . . no V5 O17 1.980(5) . . no N49 C56 1.509(10) . . no V5 O20 1.598(5) . . no N58 C59 1.522(10) . . no V5 O21 1.970(5) . . no N58 C61 1.512(10) . . no V5 O22 1.961(5) . . no N58 C63 1.524(10) . . no V5 O45 3.480(5) . . no N58 C65 1.526(10) . . no V5 O46 3.517(5) . . no N67 C68 1.450(18) . . no V6 V7 2.8894(18) . . no N67 C69 1.578(19) . . no V6 V9 3.5123(19) . . no N67 C70 1.536(16) . . no V6 O15 1.806(5) . . no N67 C71 1.474(18) . . no V6 O21 1.960(5) . . no N67 C69 1.560(19) . . no N76 C77 1.136(11) . . no N79 C80 1.142(13) . . no C31 C32 1.489(11) . . no C35 C36 1.485(11) . . no C39 C40 1.505(11) . . no C43 C44 1.484(11) . . no C47 C48 1.511(12) . . no C50 C51 1.501(11) . . no C52 C53 1.502(12) . . no C54 C55 1.509(11) . . no C56 C57 1.517(13) . . no C59 C60 1.480(13) . . no C61 C62 1.508(13) . . no C63 C64 1.494(12) . . no C65 C66 1.508(11) . . no C68 C72 1.61(2) . . no C69 C73 1.65(2) . . no C70 C74 1.66(2) . . no C71 C75 1.543(19) . . no C77 C78 1.439(13) . . no C80 C81 1.447(15) . . no C32 H1 0.953(9) . . no C65 H51 0.950(8) . . no C32 H2 0.953(8) . . no C65 H52 0.961(8) . . no C32 H3 0.948(9) . . no C66 H53 0.943(8) . . no C36 H4 0.953(8) . . no C66 H54 0.955(8) . . no C36 H5 0.951(8) . . no C66 H55 0.956(9) . . no C36 H6 0.955(8) . . no C68 H56 0.953(17) . . no C40 H7 0.949(9) . . no C68 H57 0.940(16) . . no C40 H8 0.954(9) . . no C69 H58 0.949(17) . . no C40 H9 0.945(9) . . no C69 H59 0.948(17) . . no C44 H10 0.956(9) . . no C70 H60 0.961(16) . . no C44 H11 0.945(9) . . no C70 H61 0.958(16) . . no C44 H12 0.946(9) . . no C71 H62 0.955(16) . . no C48 H13 0.948(9) . . no C71 H63 0.958(17) . . no C48 H14 0.960(10) . . no C48 H15 0.939(8) . . no C50 H16 0.963(8) . . no C50 H17 0.947(8) . . no C51 H18 0.949(8) . . no C51 H19 0.954(8) . . no C51 H20 0.956(8) . . no C52 H21 0.954(9) . . no C52 H22 0.951(9) . . no C72 H64 0.949(10) . . no C53 H23 0.948(8) . . no C72 H65 0.945(10) . . no C53 H24 0.951(8) . . no C72 H66 0.954(9) . . no C53 H25 0.953(8) . . no C72 H84 0.955(10) . . no C54 H26 0.943(8) . . no C72 H85 0.947(10) . . no C54 H27 0.950(8) . . no C72 H86 0.953(10) . . no C55 H28 0.952(8) . . no C73 H67 0.948(15) . . no C55 H29 0.952(9) . . no C73 H68 0.963(16) . . no C55 H30 0.948(9) . . no C73 H69 0.945(13) . . no C56 H31 0.940(9) . . no C73 H87 0.955(13) . . no C56 H32 0.958(9) . . no C73 H88 0.952(15) . . no C57 H33 0.962(9) . . no C73 H89 0.956(12) . . no C57 H34 0.938(9) . . no C74 H70 0.953(11) . . no C57 H35 0.957(9) . . no C74 H71 0.956(11) . . no C59 H36 0.948(8) . . no C74 H72 0.945(12) . . no C59 H37 0.957(8) . . no C74 H90 0.955(12) . . no C60 H38 0.958(9) . . no C74 H91 0.947(12) . . no C60 H39 0.940(10) . . no C74 H92 0.954(11) . . no C60 H40 0.954(10) . . no C75 H73 0.939(9) . . no C61 H41 0.953(9) . . no C75 H74 0.961(9) . . no C61 H42 0.945(8) . . no C75 H75 0.957(9) . . no C62 H43 0.963(10) . . no C75 H93 0.940(9) . . no C62 H44 0.947(9) . . no C75 H94 0.955(9) . . no C62 H45 0.961(8) . . no C75 H95 0.962(9) . . no C63 H46 0.953(8) . . no C78 H96 0.945(10) . . no C63 H47 0.944(8) . . no C78 H97 0.950(9) . . no C64 H48 0.949(8) . . no C78 H98 0.956(10) . . no C64 H49 0.955(9) . . no C81 H99 0.952(10) . . no C64 H50 0.952(8) . . no C81 H100 0.953(12) . . no C81 H101 0.941(11) . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 V1 O11 101.7(2) . . . no O10 V1 O12 103.5(2) . . . no O10 V1 O29 97.8(2) . . . no O10 V1 O33 97.0(2) . . . no O10 V1 O45 179.5(2) . . . no O11 V1 O12 78.2(2) . . . no O11 V1 O29 93.1(2) . . . no O11 V1 O33 160.8(2) . . . no O11 V1 O45 77.93(18) . . . no O12 V1 O29 158.1(2) . . . no O12 V1 O33 93.4(2) . . . no O12 V1 O45 76.82(19) . . . no O29 V1 O33 88.5(2) . . . no O29 V1 O45 81.80(19) . . . no O33 V1 O45 83.33(19) . . . no O11 V2 O13 107.2(2) . . . no O11 V2 O14 79.0(2) . . . no O11 V2 O15 145.5(2) . . . no O11 V2 O30 88.1(2) . . . no O13 V2 O14 104.2(2) . . . no O13 V2 O15 107.2(3) . . . no O13 V2 O30 100.0(2) . . . no O14 V2 O15 90.7(2) . . . no O14 V2 O30 155.0(2) . . . no O15 V2 O30 88.0(2) . . . no O11 V3 O12 83.4(2) . . . no O11 V3 O14 82.3(2) . . . no O11 V3 O16 109.9(2) . . . no O11 V3 O17 139.5(2) . . . no O12 V3 O14 141.3(2) . . . no O12 V3 O16 109.4(3) . . . no O12 V3 O17 83.4(2) . . . no O14 V3 O16 109.3(3) . . . no O14 V3 O17 84.4(2) . . . no O16 V3 O17 110.7(2) . . . no O12 V4 O17 78.8(2) . . . no O12 V4 O18 107.6(2) . . . no O12 V4 O19 146.0(2) . . . no O12 V4 O34 88.5(2) . . . no O17 V4 O18 104.1(2) . . . no O17 V4 O19 89.6(2) . . . no O17 V4 O34 155.6(2) . . . no O18 V4 O19 106.1(3) . . . no O18 V4 O34 99.6(2) . . . no O19 V4 O34 89.5(2) . . . no O14 V5 O17 79.3(2) . . . no O14 V5 O20 106.0(2) . . . no O14 V5 O21 92.8(2) . . . no O14 V5 O22 150.0(2) . . . no O17 V5 O20 104.3(2) . . . no O17 V5 O21 149.6(2) . . . no O17 V5 O22 93.2(2) . . . no O20 V5 O21 106.1(2) . . . no O20 V5 O22 104.0(2) . . . no O21 V5 O22 79.0(2) . . . no O15 V6 O21 88.7(2) . . . no O15 V6 O23 105.6(3) . . . no O15 V6 O24 148.6(2) . . . no O15 V6 O37 89.4(2) . . . no O21 V6 O23 105.9(3) . . . no O21 V6 O24 79.5(2) . . . no O21 V6 O37 152.4(2) . . . no O23 V6 O24 105.7(3) . . . no O23 V6 O37 101.1(3) . . . no O24 V6 O37 87.9(2) . . . no O21 V7 O22 83.4(2) . . . no O21 V7 O24 83.8(2) . . . no O21 V7 O25 109.5(3) . . . no O21 V7 O26 141.0(2) . . . no O22 V7 O24 139.9(2) . . . no O22 V7 O25 111.1(3) . . . no O22 V7 O26 82.3(2) . . . no O24 V7 O25 109.0(3) . . . no O24 V7 O26 84.2(2) . . . no O25 V7 O26 109.4(3) . . . no O19 V8 O22 90.7(2) . . . no O19 V8 O26 147.9(2) . . . no O19 V8 O27 105.9(3) . . . no O19 V8 O42 90.0(2) . . . no O22 V8 O26 78.8(2) . . . no O22 V8 O27 103.4(2) . . . no O22 V8 O42 156.1(2) . . . no O26 V8 O27 106.1(3) . . . no O26 V8 O42 88.0(2) . . . no O27 V8 O42 99.4(2) . . . no O24 V9 O26 79.9(2) . . . no O24 V9 O28 102.0(3) . . . no O24 V9 O38 92.2(2) . . . no O24 V9 O41 159.3(2) . . . no O24 V9 O46 75.93(19) . . . no O26 V9 O28 103.0(2) . . . no O26 V9 O38 157.6(2) . . . no O26 V9 O41 92.5(2) . . . no O26 V9 O46 75.77(19) . . . no O28 V9 O38 99.2(2) . . . no O28 V9 O41 98.5(3) . . . no O28 V9 O46 177.7(2) . . . no O38 V9 O41 87.7(2) . . . no O38 V9 O46 82.0(2) . . . no O41 V9 O46 83.5(2) . . . no V1 O11 V2 126.9(3) . . . no V1 O11 V3 98.2(2) . . . no V2 O11 V3 99.5(2) . . . no V1 O12 V3 98.4(2) . . . no V1 O12 V4 123.5(3) . . . no V3 O12 V4 98.9(2) . . . no V2 O14 V3 98.9(2) . . . no V2 O14 V5 136.2(3) . . . no V3 O14 V5 98.3(2) . . . no V2 O15 V6 158.1(3) . . . no V3 O17 V4 98.3(2) . . . no V3 O17 V5 97.9(2) . . . no V4 O17 V5 136.6(3) . . . no V4 O19 V8 158.3(3) . . . no V5 O21 V6 137.5(3) . . . no V5 O21 V7 98.7(2) . . . no V6 O21 V7 97.8(2) . . . no V5 O22 V7 98.7(2) . . . no V5 O22 V8 137.1(3) . . . no V7 O22 V8 99.3(2) . . . no V6 O24 V7 98.5(2) . . . no V6 O24 V9 127.7(3) . . . no V7 O24 V9 97.6(2) . . . no V7 O26 V8 98.9(2) . . . no V7 O26 V9 97.2(2) . . . no V8 O26 V9 125.6(3) . . . no V1 O29 C31 131.3(5) . . . no V2 O30 C31 137.9(5) . . . no V1 O33 C35 131.4(5) . . . no V4 O34 C35 139.8(5) . . . no V6 O37 C39 138.9(5) . . . no V9 O38 C39 132.1(5) . . . no V9 O41 C43 132.1(5) . . . no V8 O42 C43 137.7(5) . . . no V1 O45 C47 140.1(5) . . . no V9 O46 C47 142.9(5) . . . no C50 N49 C52 108.3(6) . . . no C50 N49 C54 110.0(6) . . . no C50 N49 C56 110.8(6) . . . no C52 N49 C54 110.7(6) . . . no C52 N49 C56 108.4(6) . . . no C54 N49 C56 108.6(6) . . . no C59 N58 C61 107.2(6) . . . no C59 N58 C63 111.0(6) . . . no C59 N58 C65 111.1(6) . . . no C61 N58 C63 111.2(6) . . . no C61 N58 C65 110.2(6) . . . no C63 N58 C65 106.3(6) . . . no C68 N67 C69 112.5(10) . . . no C68 N67 C69 112.5(10) . . . no C68 N67 C70 114.0(10) . . . no C68 N67 C71 109.7(11) . . . no C69 N67 C70 102.1(11) . . . no C69 N67 C70 102.1(11) . . . no C69 N67 C71 106.5(10) . . . no C69 N67 C71 106.5(10) . . . no C70 N67 C71 111.6(10) . . . no C68 N67 C69 111.5(11) . . . no C68 N67 C69 111.5(11) . . . no O29 C31 O30 125.5(7) . . . no O29 C31 C32 117.5(7) . . . no O30 C31 C32 116.9(7) . . . no O33 C35 O34 124.5(7) . . . no O33 C35 C36 117.2(7) . . . no O34 C35 C36 118.3(7) . . . no O37 C39 O38 125.7(7) . . . no O37 C39 C40 117.2(7) . . . no O38 C39 C40 117.1(7) . . . no O41 C43 O42 125.4(7) . . . no O41 C43 C44 116.7(7) . . . no O42 C43 C44 118.0(7) . . . no O45 C47 O46 122.7(7) . . . no O45 C47 C48 120.5(7) . . . no O46 C47 C48 116.7(7) . . . no N49 C50 C51 115.6(6) . . . no N49 C52 C53 116.1(7) . . . no N49 C54 C55 116.4(6) . . . no N49 C56 C57 115.0(7) . . . no N58 C59 C60 116.2(7) . . . no N58 C61 C62 114.9(7) . . . no N58 C63 C64 115.6(7) . . . no N58 C65 C66 116.0(6) . . . no N67 C68 C72 114.1(11) . . . no N67 C69 C73 104.1(13) . . . no N67 C69 C73 104.1(13) . . . no N67 C70 C74 105.7(11) . . . no N67 C71 C75 113.2(11) . . . no N76 C77 C78 178.8(10) . . . no N79 C80 C81 176.6(14) . . . no C31 C32 H1 109.5(8) . . . no C31 C32 H2 109.6(8) . . . no C31 C32 H3 110.0(8) . . . no H1 C32 H2 109.0(9) . . . no H1 C32 H3 109.4(8) . . . no H2 C32 H3 109.4(9) . . . no C35 C36 H4 110.1(7) . . . no C35 C36 H5 110.1(7) . . . no C35 C36 H6 109.7(7) . . . no H4 C36 H5 109.1(8) . . . no H4 C36 H6 108.8(8) . . . no H5 C36 H6 109.0(8) . . . no C39 C40 H7 109.3(8) . . . no C39 C40 H8 108.9(8) . . . no C39 C40 H9 109.9(8) . . . no H7 C40 H8 109.2(9) . . . no H7 C40 H9 110.0(9) . . . no H8 C40 H9 109.6(9) . . . no C43 C44 H10 108.8(8) . . . no C43 C44 H11 109.7(8) . . . no C43 C44 H12 109.3(7) . . . no H10 C44 H11 109.5(8) . . . no H10 C44 H12 109.3(8) . . . no H11 C44 H12 110.3(9) . . . no C47 C48 H13 109.1(8) . . . no C47 C48 H14 108.9(8) . . . no C47 C48 H15 109.9(8) . . . no H13 C48 H14 108.8(8) . . . no H13 C48 H15 110.6(9) . . . no H14 C48 H15 109.5(9) . . . no N49 C50 H16 107.2(7) . . . no N49 C50 H17 108.1(7) . . . no C51 C50 H16 108.2(7) . . . no C51 C50 H17 109.0(7) . . . no H16 C50 H17 108.5(8) . . . no C50 C51 H18 110.4(7) . . . no C50 C51 H19 109.5(8) . . . no C50 C51 H20 110.0(7) . . . no H18 C51 H19 109.3(8) . . . no H18 C51 H20 109.1(8) . . . no H19 C51 H20 108.6(8) . . . no N49 C52 H21 107.2(7) . . . no N49 C52 H22 107.2(7) . . . no C53 C52 H21 108.5(8) . . . no C53 C52 H22 108.7(7) . . . no H21 C52 H22 109.0(8) . . . no C52 C53 H23 109.7(8) . . . no C52 C53 H24 109.5(8) . . . no C52 C53 H25 109.6(7) . . . no H23 C53 H24 109.5(8) . . . no H23 C53 H25 109.4(8) . . . no H24 C53 H25 109.1(8) . . . no N49 C54 H26 107.9(7) . . . no N49 C54 H27 107.5(7) . . . no C55 C54 H26 107.7(7) . . . no C55 C54 H27 107.2(7) . . . no H26 C54 H27 110.1(8) . . . no C54 C55 H28 109.7(8) . . . no C54 C55 H29 109.4(8) . . . no C54 C55 H30 109.5(8) . . . no H28 C55 H29 109.2(8) . . . no H28 C55 H30 109.5(8) . . . no H29 C55 H30 109.5(8) . . . no N49 C56 H31 108.3(7) . . . no N49 C56 H32 107.2(8) . . . no C57 C56 H31 108.9(8) . . . no C57 C56 H32 107.7(8) . . . no H31 C56 H32 109.6(9) . . . no C56 C57 H33 109.1(8) . . . no C56 C57 H34 110.6(9) . . . no C56 C57 H35 110.1(8) . . . no H33 C57 H34 109.4(9) . . . no H33 C57 H35 107.8(9) . . . no H34 C57 H35 109.8(9) . . . no N58 C59 H36 107.6(7) . . . no N58 C59 H37 107.4(7) . . . no C60 C59 H36 108.8(8) . . . no C60 C59 H37 107.7(8) . . . no H36 C59 H37 109.0(8) . . . no C59 C60 H38 109.2(9) . . . no C59 C60 H39 110.4(9) . . . no C59 C60 H40 109.2(8) . . . no H38 C60 H39 109.6(9) . . . no H38 C60 H40 108.5(9) . . . no H39 C60 H40 110.0(10) . . . no N58 C61 H41 107.8(8) . . . no N58 C61 H42 107.9(7) . . . no C62 C61 H41 107.7(8) . . . no C62 C61 H42 108.8(8) . . . no H41 C61 H42 109.6(8) . . . no C61 C62 H43 110.1(8) . . . no C61 C62 H44 111.4(8) . . . no C61 C62 H45 110.2(8) . . . no H43 C62 H44 108.7(9) . . . no H43 C62 H45 107.5(9) . . . no H44 C62 H45 108.8(8) . . . no N58 C63 H46 107.3(7) . . . no N58 C63 H47 108.2(7) . . . no C64 C63 H46 107.8(7) . . . no C64 C63 H47 108.1(7) . . . no H46 C63 H47 109.7(8) . . . no C63 C64 H48 109.9(8) . . . no C63 C64 H49 109.9(8) . . . no C63 C64 H50 109.7(7) . . . no H48 C64 H49 109.1(8) . . . no H48 C64 H50 109.3(8) . . . no H49 C64 H50 108.8(8) . . . no N58 C65 H51 108.5(7) . . . no N58 C65 H52 107.5(7) . . . no C66 C65 H51 108.4(7) . . . no C66 C65 H52 107.7(7) . . . no H51 C65 H52 108.5(8) . . . no C65 C66 H53 110.4(8) . . . no C65 C66 H54 109.5(8) . . . no C65 C66 H55 109.0(7) . . . no H53 C66 H54 109.6(8) . . . no H53 C66 H55 109.6(8) . . . no H54 C66 H55 108.6(8) . . . no N67 C68 H56 108.2(14) . . . no N67 C68 H57 108.9(15) . . . no C72 C68 H56 107.3(15) . . . no C72 C68 H57 108.2(14) . . . no H56 C68 H57 110.1(16) . . . no N67 C69 H58 111.5(14) . . . no N67 C69 H58 111.5(14) . . . no N67 C69 H59 111.3(14) . . . no N67 C69 H59 111.3(14) . . . no C73 C69 H58 110.1(15) . . . no C73 C69 H59 110.0(14) . . . no H58 C69 H59 109.7(19) . . . no N67 C70 H60 110.7(14) . . . no N67 C70 H61 111.1(13) . . . no C74 C70 H60 110.8(14) . . . no C74 C70 H61 110.7(14) . . . no H60 C70 H61 107.8(16) . . . no N67 C71 H62 108.7(14) . . . no N67 C71 H63 108.7(14) . . . no C75 C71 H62 109.4(14) . . . no C75 C71 H63 108.4(14) . . . no H62 C71 H63 108.4(16) . . . no C68 C72 H64 109.2(10) . . . no C68 C72 H65 109.9(9) . . . no C68 C72 H66 109.0(10) . . . no H64 C72 H65 110.0(10) . . . no H64 C72 H66 109.2(9) . . . no H65 C72 H66 109.5(10) . . . no H84 C72 H85 109.4(9) . . . no H84 C72 H86 108.9(10) . . . no H85 C72 H86 109.5(10) . . . no C69 C73 H67 109.9(11) . . . no C69 C73 H68 109.3(16) . . . no C69 C73 H69 110.1(10) . . . no H67 C73 H68 108.6(10) . . . no H67 C73 H69 110.1(19) . . . no H68 C73 H69 108.9(12) . . . no H87 C73 H88 108.9(18) . . . no H87 C73 H89 108.6(11) . . . no H88 C73 H89 108.8(12) . . . no C70 C74 H70 109.5(9) . . . no C70 C74 H71 109.9(12) . . . no C70 C74 H72 109.8(10) . . . no H70 C74 H71 108.7(11) . . . no H70 C74 H72 109.6(13) . . . no H71 C74 H72 109.3(9) . . . no H90 C74 H91 109.3(13) . . . no H90 C74 H92 108.7(11) . . . no H91 C74 H92 109.3(10) . . . no C71 C75 H73 110.5(10) . . . no C71 C75 H74 109.1(9) . . . no C71 C75 H75 109.8(10) . . . no H73 C75 H74 109.5(9) . . . no H73 C75 H75 109.8(9) . . . no H74 C75 H75 108.0(9) . . . no H93 C75 H94 109.9(9) . . . no H93 C75 H95 109.3(9) . . . no H94 C75 H95 108.0(9) . . . no C77 C78 H96 109.9(9) . . . no C77 C78 H97 109.7(9) . . . no C77 C78 H98 109.1(8) . . . no H96 C78 H97 109.9(9) . . . no H96 C78 H98 109.3(9) . . . no H97 C78 H98 108.9(9) . . . no C80 C81 H99 108.8(10) . . . no C80 C81 H100 108.9(9) . . . no C80 C81 H101 110.0(11) . . . no H99 C81 H100 109.1(12) . . . no H99 C81 H101 110.1(10) . . . no H100 C81 H101 110.0(11) . . . no # The following lines may be used to test the character set of files sent by # network email or other means. They are not part of the CIF data archive. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ #===END ############################################################################## # IUMSC CIF Archive file # ############################################################################## data_MSC96004 _audit_creation_method 'minor manual editing of SDT2CIF v. 1.1 BETA output' _chemical_formula_sum 'C44 H106 N7 O36 V15' _chemical_formula_moiety ? _chemical_formula_weight 2073.47 _cell_length_a 22.105(3) _cell_length_b 13.7840(19) _cell_length_c 26.604(4) _cell_angle_alpha 90 _cell_angle_beta 107.560(7) _cell_angle_gamma 90 _cell_volume 7728.4(18) _cell_formula_units_Z 4 _cell_measurement_reflns_used 132 _cell_measurement_theta_min 10.8 _cell_measurement_theta_max 15.77 _cell_measurement_temperature ? _exptl_crystal_colour ? _exptl_crystal_description ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_diffrn 1.782 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4208 _exptl_absorpt_coefficient_mu 1.8045 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details Tompa _exptl_absorpt_correction_T_min 0.714 _exptl_absorpt_correction_T_max 0.815 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2+x,1/2+y,z -x,y,1/2-z 1/2-x,1/2+y,1/2-z x,-y,1/2+z 1/2+x,1/2-y,1/2+z -x,-y,-z 1/2-x,1/2-y,-z _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature ? _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 13681 _diffrn_reflns_av_R_equivalents 0.064 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max ? _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min ? _diffrn_reflns_limit_h_max ? _diffrn_reflns_limit_k_min ? _diffrn_reflns_limit_k_max ? _diffrn_reflns_limit_l_min ? _diffrn_reflns_limit_l_max ? _diffrn_standards_number 4 _diffrn_standards_decay_% 0.9 _diffrn_standards_interval_count 300 _reflns_number_total 6847 _reflns_number_gt 4190 _reflns_threshold_expression F^2^>2.33\s(F^2^) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source V V 0.267 0.53 'International Tables Vol. IV (1974) Table 2.2B' O O 0.008 0.006 'International Tables Vol. IV (1974) Table 2.2B' N N 0.004 0.003 'International Tables Vol. IV (1974) Table 2.2B' C C 0.002 0.002 'International Tables Vol. IV (1974) Table 2.2B' H H 0 0 'International Tables Vol. IV (1974) Table 2.2B' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_number_reflns ? _refine_ls_number_parameters ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_coef 0.3841E-7 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_expression ; Larson, A. C. (1967). Acta Cryst. 23, p. 664. Eq. (3) ; _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack ? _refine_ls_weighting_scheme calc _refine_ls_weighting_details w^-1^=\s^2^(F)+(.05F)^2^ _refine_ls_R_factor_gt 0.1111 _refine_ls_wR_factor_ref 0.1125 _refine_ls_goodness_of_fit_ref 2.5203 _refine_ls_shift/su_max 0.7513 _refine_diff_density_max ? _refine_diff_density_min ? _computing_data_collection 'NPS, local program' _computing_cell_refinement 'XTEL, local package' _computing_data_reduction 'XTEL, local package' _computing_structure_solution MULTAN78 _computing_structure_refinement 'XTEL, local package' _computing_molecular_graphics 'XTEL, local package' _computing_publication_material 'XTEL, local package' 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_disorder_group _atom_site_disorder_assembly V1 V 1 0.5392(3) 0.25 0.0275(15) Uani 1 0 . V2 V 0.99886(10) 0.4455(2) 0.14682(10) 0.0271(11) Uani 1 0 . V3 V 0.87024(10) 0.4098(2) 0.15476(10) 0.0320(11) Uani 1 0 . V4 V 1.12870(10) 0.4108(3) 0.21998(10) 0.0354(11) Uani 1 0 . V5 V 0.91450(10) 0.2205(2) 0.12556(10) 0.0281(13) Uani 1 0 . V6 V 1.08240(10) 0.2219(2) 0.16745(10) 0.0295(13) Uani 1 0 . V7 V 0.9991(2) 0.0698(3) 0.1869(2) 0.0621(15) Uani 1 0 . V8 V 0.86236(10) 0.1747(2) 0.21602(10) 0.0312(13) Uani 1 0 . O9 O 0.9420(5) 0.4912(9) 0.1840(4) 0.030(4) Uani 1 0 . O10 O 1.0567(5) 0.4934(8) 0.2116(5) 0.031(4) Uani 1 0 . O11 O 0.9372(5) 0.3524(8) 0.1208(4) 0.026(4) Uani 1 0 . O12 O 1.0625(5) 0.3549(8) 0.1529(4) 0.024(4) Uani 1 0 . O13 O 0.8594(5) 0.2745(8) 0.1629(4) 0.025(4) Uani 1 0 . O14 O 0.8420(5) 0.4370(9) 0.2102(4) 0.032(4) Uani 1 0 . O15 O 1.1384(5) 0.2753(9) 0.2314(4) 0.031(4) Uani 1 0 . O16 O 0.9994(5) 0.1855(8) 0.1354(4) 0.029(4) Uani 1 0 . O17 O 0.9174(5) 0.1215(9) 0.1761(4) 0.031(4) Uani 1 0 . O18 O 1.0808(5) 0.1219(9) 0.2170(4) 0.032(4) Uani 1 0 . O19 O 1 0.0126(15) 0.25 0.061(9) Uani 1 0 . O20 O 1 0.6561(12) 0.25 0.035(7) Uani 1 0 . O21 O 0.9965(5) 0.5182(9) 0.1001(4) 0.031(4) Uani 1 0 . O22 O 0.8174(5) 0.4532(9) 0.1048(5) 0.040(5) Uani 1 0 . O23 O 1.1816(6) 0.4543(11) 0.1950(5) 0.055(6) Uani 1 0 . O24 O 0.8743(5) 0.1855(10) 0.0690(4) 0.036(5) Uani 1 0 . O25 O 1.1246(6) 0.1851(11) 0.1311(5) 0.046(5) Uani 1 0 . O26 O 0.0004(7) 0.9786(11) 0.1507(7) 0.072(7) Uani 1 0 . O27 O 0.7962(5) 0.1178(10) 0.2001(4) 0.040(5) Uani 1 0 . N28 N 1.1743(6) 0.5647(13) 0.0466(5) 0.040(6) Uani 1 0 . C29 C 1.1472(10) 0.491(2) 0.0764(11) 0.074(11) Uani 1 0 . C30 C 1.1274(14) 0.394(2) 0.0472(12) 0.093(15) Uani 1 0 . C31 C 1.1933(11) 0.649(2) 0.0824(10) 0.086(13) Uani 1 0 . C32 C 1.2167(12) 0.737(2) 0.0634(13) 0.097(14) Uani 1 0 . C33 C 0.1237(9) 0.5958(17) 0.9985(8) 0.050(8) Uani 1 0 . C34 C 1.0631(9) 0.6334(18) 0.0059(7) 0.056(9) Uani 1 0 . C35 C 1.2297(8) 0.5303(14) 0.0316(7) 0.034(7) Uani 1 0 . C36 C 1.2831(9) 0.4937(17) 0.0746(8) 0.050(8) Uani 1 0 . N37 N 1.1498(7) -0.2055(13) 0.2394(6) 0.043(7) Uani 1 0 . C38 C 1.1661(16) -0.312(3) 0.2599(14) 0.060(9) Uiso 0.67351 0 . C39 C 1.2228(11) -0.3260(18) 0.3016(10) 0.054(6) Uiso 0.924709 0 . C40 C 1.1959(12) -0.169(2) 0.2143(11) 0.043(6) Uiso 0.75171 0 . C41 C 1.1840(15) -0.063(3) 0.1864(13) 0.055(9) Uiso 0.705677 0 . C42 C 1.0815(10) -0.1949(17) 0.2024(9) 0.030(5) Uiso 0.743763 0 . C43 C 0.0657(10) 0.7474(15) 0.1528(9) 0.050(5) Uiso 0.998564 0 . C44 C 1.1563(15) -0.128(2) 0.2863(13) 0.065(9) Uiso 0.735977 0 . C45 C 1.1161(15) -0.159(2) 0.3223(13) 0.070(9) Uiso 0.780323 0 . C46 C 1.218(5) -0.232(9) 0.268(5) 0.11(3) Uiso 0.278307 0 . C47 C 1.166(3) -0.105(5) 0.210(3) 0.047(16) Uiso 0.308673 0 . C48 C 0.199(3) 0.879(5) 0.172(3) 0.085(19) Uiso 0.429366 0 . C49 C 1.124(3) -0.284(6) 0.208(3) 0.044(18) Uiso 0.274947 0 . C50 C 0.104(2) 0.817(4) 0.271(2) 0.052(14) Uiso 0.394475 0 . N51 N 0.9724(15) -0.020(3) 0.0018(14) 0.053(9) Uiso 0.5 0 . C52 C 0.0204(15) 0.937(2) 0.9738(12) 0.069(9) Uiso 0.813825 0 . C53 C 0.001(4) 0.866(7) 0.991(4) 0.14(3) Uiso 0.443147 0 . C54 C 0.9519(19) 0.908(3) 0.0367(17) 0.062(11) Uiso 0.549332 0 . C55 C 0.942(3) -0.184(4) 0.013(2) 0.095(18) Uiso 0.527122 0 . C56 C 0.908(2) 0.062(4) 0.965(2) 0.080(14) Uiso 0.540589 0 . C57 C 0.850(3) 0.013(4) 0.961(2) 0.084(16) Uiso 0.4875 0 . C58 C 0.913(2) -0.010(4) -0.0508(19) 0.089(14) Uiso 0.638486 0 . C59 C 0.868(2) 0.674(4) 0.092(2) 0.032(13) Uiso 0.317341 0 . C60 C 0.882(4) 0.741(7) 0.072(3) 0.08(2) Uiso 0.317341 0 . N61 N 0.897(3) -0.190(5) 0.057(2) 0.061(16) Uiso 0.317341 0 . C62 C 0.719(2) 0.634(4) 0.060(2) 0.033(13) Uiso 0.3273 0 . C63 C 0.759(3) 0.702(5) 0.044(2) 0.044(15) Uiso 0.3273 0 . N64 N 0.770(3) 0.761(5) 0.018(2) 0.063(16) Uiso 0.3273 0 . H1 H 1.1784 0.478 0.1088 0.0867 Uiso 1 0 . H2 H 1.1109 0.5192 0.0823 0.0867 Uiso 1 0 . H3 H 1.1117 0.3527 0.0691 0.1063 Uiso 1 0 . H4 H 1.095 0.4059 0.0152 0.1063 Uiso 1 0 . H5 H 1.1629 0.3656 0.0406 0.1063 Uiso 1 0 . H6 H 1.157 0.6678 0.0922 0.0976 Uiso 1 0 . H7 H 1.2258 0.6281 0.1127 0.0976 Uiso 1 0 . H8 H 1.254 0.7219 0.0543 0.1074 Uiso 1 0 . H9 H 1.1852 0.7612 0.0334 0.1074 Uiso 1 0 . H10 H 1.2264 0.7846 0.0905 0.1074 Uiso 1 0 . H11 H 0.141 0.6457 0.9823 0.06 Uiso 1 0 . H12 H 0.1134 0.5414 0.9753 0.06 Uiso 1 0 . H13 H 1.0715 0.6899 0.0273 0.0677 Uiso 1 0 . H14 H 1.0337 0.649 -0.0275 0.0677 Uiso 1 0 . H15 H 1.0448 0.585 0.0225 0.0677 Uiso 1 0 . H16 H 1.2159 0.48 0.0065 0.0429 Uiso 1 0 . H17 H 1.2446 0.5835 0.0158 0.0429 Uiso 1 0 . H18 H 1.269 0.4417 0.0917 0.0625 Uiso 1 0 . H19 H 1.3154 0.4714 0.0608 0.0625 Uiso 1 0 . H20 H 1.2993 0.5443 0.0993 0.0625 Uiso 1 0 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 V1 0.032(2) 0.028(3) 0.022(2) 0 0.008(2) 0 V2 0.027(2) 0.039(2) 0.0150(10) -0.0013(10) 0.0065(10) 0.0011(10) V3 0.0223(10) 0.040(2) 0.028(2) 0.0041(10) -0.0008(10) -0.002(2) V4 0.0187(10) 0.057(2) 0.033(2) -0.0029(10) 0.0100(10) 0.009(2) V5 0.027(2) 0.042(2) 0.016(2) -0.0079(10) 0.0070(10) -0.0009(10) V6 0.027(2) 0.046(2) 0.016(2) 0.0074(10) 0.0081(10) -0.0064(10) V7 0.046(2) 0.039(2) 0.077(3) 0.011(2) -0.018(2) -0.025(2) V8 0.024(2) 0.048(2) 0.021(2) -0.0153(10) 0.0043(10) 0.003(2) O9 0.027(6) 0.045(8) 0.022(6) 0.004(6) 0.012(5) 0.000(6) O10 0.028(6) 0.028(7) 0.034(7) -0.010(5) 0.006(5) 0.004(6) O11 0.023(6) 0.039(8) 0.012(6) -0.004(5) -0.001(5) 0.003(5) O12 0.020(5) 0.045(8) 0.009(6) -0.000(5) 0.011(4) -0.004(5) O13 0.017(5) 0.039(7) 0.022(6) -0.004(5) 0.013(5) 0.000(6) O14 0.036(7) 0.045(8) 0.013(6) 0.009(6) 0.006(5) 0.006(6) O15 0.029(6) 0.038(7) 0.020(6) 0.013(6) -0.002(5) -0.005(6) O16 0.039(7) 0.022(7) 0.022(7) 0.002(5) 0.005(5) -0.003(5) O17 0.031(6) 0.045(8) 0.022(7) 0.010(6) 0.015(5) 0.004(6) O18 0.027(6) 0.039(8) 0.025(7) 0.001(6) 0.003(5) -0.002(6) O19 0.055(13) 0.042(13) 0.062(15) 0 -0.022(11) 0 O20 0.039(10) 0.025(10) 0.047(12) 0 0.021(9) 0 O21 0.026(6) 0.039(8) 0.029(7) -0.001(6) 0.008(5) 0.005(6) O22 0.019(6) 0.049(9) 0.049(8) 0.009(6) 0.005(6) -0.009(7) O23 0.033(7) 0.083(12) 0.049(9) -0.013(8) 0.009(6) 0.019(8) O24 0.032(6) 0.057(9) 0.021(7) 0.001(6) 0.008(5) -0.004(6) O25 0.036(7) 0.081(11) 0.026(7) 0.021(7) 0.015(6) -0.004(7) O26 0.060(10) 0.044(10) 0.090(13) 0.014(8) -0.012(9) -0.004(9) O27 0.032(7) 0.075(10) 0.013(6) -0.011(7) 0.007(5) 0.009(6) N28 0.024(8) 0.071(12) 0.021(8) 0.011(8) 0.002(6) -0.011(8) C29 0.043(13) 0.10(2) 0.077(18) -0.016(14) 0.015(12) 0.038(17) C30 0.10(2) 0.10(2) 0.09(2) -0.01(2) 0.039(18) 0.030(19) C31 0.049(15) 0.12(3) 0.063(18) 0.037(17) -0.027(13) -0.004(18) C32 0.059(17) 0.09(2) 0.11(3) 0.013(16) -0.033(16) -0.05(2) C33 0.046(12) 0.070(16) 0.038(12) 0.014(11) 0.019(10) 0.030(12) C34 0.048(12) 0.098(19) 0.020(10) 0.032(12) 0.005(9) -0.018(11) C35 0.035(10) 0.053(12) 0.028(10) 0.011(9) 0.031(8) 0.008(9) C36 0.036(11) 0.070(16) 0.038(12) 0.005(11) 0.004(9) 0.005(11) N37 0.027(8) 0.068(13) 0.041(10) -0.001(8) 0.021(7) 0.013(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O9 1.951(11) . . no V1 O9 1.951(11) . 3_755 no N51 N51 1.37(6) . 7_755 no V1 O10 1.947(11) . . no V1 O10 1.947(11) . 3_755 no N51 C52 1.31(4) . 7_666 no V1 O20 1.611(17) . . no V1 O20 1.611(17) . 3_755 no N51 C52 1.58(5) . 1_644 no V2 O9 1.925(11) . . no N51 C53 1.74(10) . 1_644 no V2 O10 1.926(12) . . no N51 C54 1.52(5) . 1_545 no V2 O11 1.849(11) . . no N51 C56 1.85(6) . 1_554 no V2 O12 1.852(11) . . no N51 C58 1.61(6) . . no V2 O21 1.584(11) . . no N61 C55 1.75(8) . . no V3 O9 1.906(12) . . no N61 C60 1.11(9) . 1_545 no V3 O11 2.107(11) . . no N64 N64 1.14(10) . 8_665 no V3 O13 1.901(12) . . no N64 C63 1.12(8) . . no V3 O14 1.805(11) . . no N64 C63 1.66(9) . 8_665 no V3 O22 1.597(12) . . no C29 C30 1.55(4) . . no V4 O10 1.914(12) . . no C31 C32 1.47(4) . . no V4 O12 2.083(11) . . no C33 C34 1.50(3) . 1_456 no V4 O14 1.810(11) . 3_755 no C35 C36 1.46(3) . . no V4 O15 1.894(12) . . no C38 C39 1.41(4) . . no V4 O23 1.623(12) . . no C38 C46 1.55(12) . . no V5 O11 1.900(12) . . no C38 C49 1.47(8) . . no V5 O13 1.939(10) . . no C39 C46 1.55(12) . . no V5 O16 1.877(11) . . no C40 C41 1.63(4) . . no V5 O17 1.903(12) . . no C40 C46 1.63(12) . . no V5 O24 1.576(12) . . no C40 C47 1.10(7) . . no V6 O12 1.897(12) . . no C40 C48 1.33(7) . 1_645 no V6 O15 1.922(11) . . no C41 C47 1.03(7) . . no V6 O16 1.845(11) . . no C41 C48 0.98(7) . 1_645 no V6 O18 1.915(12) . . no C42 C43 1.49(3) . 1_645 no V6 O25 1.614(11) . . no C42 C49 1.53(8) . . no V7 O16 2.103(12) . . no C42 C50 1.76(6) . 1_645 no V7 O17 1.882(11) . . no C43 C49 1.69(7) . 1_465 no V7 O18 1.884(11) . . no C44 C45 1.55(4) . . no V7 O19 1.850(10) . . no V7 O19 1.850(10) . 3_755 no C44 C50 1.33(6) . 1_645 no V7 O26 1.589(16) . 1_645 no C45 C50 1.34(6) . 1_645 no V8 O13 1.959(11) . . no C47 C48 1.45(9) . 1_645 no V8 O15 1.973(12) . 3_755 no C52 C53 1.21(9) . . no V8 O17 1.981(11) . . no C52 C56 1.90(6) . 7_667 no V8 O18 1.982(11) . 3_755 no C53 C54 1.94(10) . 1_456 no V8 O27 1.599(12) . . no C53 C55 1.73(10) . 1_466 no N28 C29 1.51(3) . . no C54 C55 1.39(7) . 1_565 no N28 C31 1.48(3) . . no C56 C57 1.43(7) . . no N28 C33 1.49(2) . 1_654 no C56 C58 1.08(6) . 1_556 no N28 C35 1.474(19) . . no C57 C58 1.56(7) . 1_556 no N37 C38 1.58(4) . . no C59 C60 1.16(10) . . no N37 C40 1.46(3) . . no C62 C63 1.45(8) . . no N37 C42 1.54(3) . . no N37 C44 1.61(4) . . no N37 C46 1.51(12) . . no N37 C47 1.68(7) . . no N37 C49 1.38(7) . . no N37 C50 1.53(5) . 1_645 no C29 H1 0.94(2) . . no C29 H2 0.94(3) . . no C30 H3 0.95(3) . . no C30 H4 0.95(3) . . no C30 H5 0.94(3) . . no C31 H6 0.95(3) . . no C31 H7 0.95(2) . . no C32 H8 0.95(3) . . no C32 H9 0.95(3) . . no C32 H10 0.95(3) . . no C33 H11 0.951(19) . . no C33 H12 0.95(2) . . no C34 H13 0.95(2) . . no C34 H14 0.954(19) . . no C34 H15 0.95(3) . . no C35 H16 0.947(19) . . no C35 H17 0.953(17) . . no C36 H18 0.95(2) . . no C36 H19 0.95(2) . . no C36 H20 0.95(2) . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 V1 O9 140.3(8) . . 3_755 no O9 V1 O9 140.3(8) 3_755 . . no O9 V1 O10 90.6(5) . . 3_755 no O9 V1 O10 90.6(5) 3_755 . . no O9 V1 O10 76.7(4) . . . no O9 V1 O10 76.7(4) 3_755 . 3_755 no O9 V1 O10 90.6(5) . . 3_755 no O9 V1 O10 90.6(5) 3_755 . . no O9 V1 O20 109.8(4) . . . no O9 V1 O20 109.8(4) . . 3_755 no O9 V1 O20 109.8(4) 3_755 . . no O9 V1 O20 109.8(4) 3_755 . 3_755 no O10 V1 O10 142.1(7) . . 3_755 no O10 V1 O10 142.1(7) 3_755 . . no O10 V1 O20 108.9(4) . . . no O10 V1 O20 108.9(4) . . 3_755 no O10 V1 O20 108.9(4) 3_755 . . no O10 V1 O20 108.9(4) 3_755 . 3_755 no O9 V2 O10 77.8(5) . . . no O9 V2 O11 84.1(5) . . . no O9 V2 O12 140.5(5) . . . no O9 V2 O21 108.9(5) . . . no O10 V2 O11 142.1(5) . . . no O10 V2 O12 82.6(5) . . . no O10 V2 O21 109.9(5) . . . no O11 V2 O12 91.1(5) . . . no O11 V2 O21 107.4(5) . . . no O12 V2 O21 109.9(5) . . . no O9 V3 O11 77.9(4) . . . no O9 V3 O13 130.4(5) . . . no O9 V3 O14 89.7(5) . . . no O9 V3 O22 115.5(6) . . . no O11 V3 O13 79.0(4) . . . no O11 V3 O14 152.7(5) . . . no O11 V3 O22 102.5(5) . . . no O13 V3 O14 91.3(5) . . . no O13 V3 O22 112.1(6) . . . no O14 V3 O22 104.8(6) . . . no O10 V4 O12 77.0(5) . . . no O10 V4 O14 91.7(5) . . 3_755 no O10 V4 O15 130.9(5) . . . no O10 V4 O23 114.1(6) . . . no O12 V4 O14 153.4(5) . . 3_755 no O12 V4 O15 77.8(5) . . . no O12 V4 O23 101.1(6) . . . no O14 V4 O15 92.5(5) 3_755 . . no O14 V4 O23 105.5(6) 3_755 . . no O15 V4 O23 111.7(7) . . . no O11 V5 O13 83.4(5) . . . no O11 V5 O16 89.0(5) . . . no O11 V5 O17 141.2(5) . . . no O11 V5 O24 108.3(6) . . . no O13 V5 O16 141.6(5) . . . no O13 V5 O17 78.8(5) . . . no O13 V5 O24 110.3(5) . . . no O16 V5 O17 84.1(5) . . . no O16 V5 O24 107.9(5) . . . no O17 V5 O24 110.2(6) . . . no O12 V6 O15 81.8(5) . . . no O12 V6 O16 91.8(5) . . . no O12 V6 O18 141.6(5) . . . no O12 V6 O25 108.8(6) . . . no O15 V6 O16 143.0(5) . . . no O15 V6 O18 78.9(5) . . . no O15 V6 O25 108.4(6) . . . no O16 V6 O18 84.3(5) . . . no O16 V6 O25 108.1(6) . . . no O18 V6 O25 108.6(6) . . . no O16 V7 O17 78.7(5) . . . no O16 V7 O18 78.3(5) . . . no O16 V7 O19 155.9(7) . . . no O16 V7 O19 155.9(7) . . 3_755 no O16 V7 O26 101.6(7) . . 1_645 no O17 V7 O18 132.3(5) . . . no O17 V7 O19 92.6(5) . . . no O17 V7 O19 92.6(5) . . 3_755 no O17 V7 O26 113.6(7) . . 1_645 no O18 V7 O19 91.7(5) . . . no O18 V7 O19 91.7(5) . . 3_755 no O18 V7 O26 111.7(7) . . 1_645 no O19 V7 O26 102.5(9) . . 1_645 no O19 V7 O26 102.5(9) 3_755 . 1_645 no O13 V8 O15 90.7(5) . . 3_755 no O13 V8 O17 76.5(5) . . . no O13 V8 O18 141.3(5) . . 3_755 no O13 V8 O27 108.9(5) . . . no O15 V8 O17 141.1(5) 3_755 . . no O15 V8 O18 76.1(5) 3_755 . 3_755 no O15 V8 O27 109.3(6) 3_755 . . no O17 V8 O18 91.2(5) . . 3_755 no O17 V8 O27 109.7(6) . . . no O18 V8 O27 109.8(6) 3_755 . . no V1 O9 V2 102.7(5) . . . no V1 O9 V2 102.7(5) 3_755 . . no V1 O9 V3 143.8(6) . . . no V1 O9 V3 143.8(6) 3_755 . . no V2 O9 V3 100.9(5) . . . no V1 O10 V2 102.8(5) . . . no V1 O10 V2 102.8(5) 3_755 . . no V1 O10 V4 140.9(6) . . . no V1 O10 V4 140.9(6) 3_755 . . no V2 O10 V4 101.8(6) . . . no V2 O11 V3 96.4(5) . . . no V2 O11 V5 145.0(6) . . . no V3 O11 V5 95.6(5) . . . no V2 O12 V4 98.3(5) . . . no V2 O12 V6 142.5(6) . . . no V4 O12 V6 97.1(5) . . . no V3 O13 V5 101.4(5) . . . no V3 O13 V8 142.5(6) . . . no V5 O13 V8 102.1(5) . . . no V3 O14 V4 133.8(6) . . 3_755 no V4 O15 V6 103.0(5) . . . no V4 O15 V8 141.4(6) . . 3_755 no V6 O15 V8 102.6(6) . . 3_755 no V5 O16 V6 143.9(7) . . . no V5 O16 V7 95.0(5) . . . no V6 O16 V7 95.9(5) . . . no V5 O17 V7 101.8(5) . . . no V5 O17 V8 102.6(5) . . . no V7 O17 V8 140.9(6) . . . no V6 O18 V7 101.3(5) . . . no V6 O18 V8 102.5(6) . . 3_755 no V7 O18 V8 142.1(7) . . 3_755 no V7 O19 V7 129.6(12) . . 3_755 no V7 O19 V7 129.6(12) 3_755 . . no C29 N28 C31 105(2) . . . no C29 N28 C33 109.2(15) . . 1_654 no C29 N28 C35 114.8(17) . . . no C31 N28 C33 108.7(17) . . 1_654 no C31 N28 C35 109.2(16) . . . no C33 N28 C35 109.3(14) 1_654 . . no C38 N37 C40 110.9(19) . . . no C38 N37 C42 112.8(18) . . . no C38 N37 C44 113(2) . . . no C38 N37 C46 60(5) . . . no C38 N37 C47 151(3) . . . no C38 N37 C49 59(3) . . . no C38 N37 C50 97(3) . . 1_645 no C40 N37 C42 111.1(17) . . . no C40 N37 C44 102.5(19) . . . no C40 N37 C46 66(4) . . . no C40 N37 C47 40(2) . . . no C40 N37 C49 101(3) . . . no C40 N37 C50 148(3) . . 1_645 no C42 N37 C44 105.9(17) . . . no C42 N37 C46 168(5) . . . no C42 N37 C47 86(3) . . . no C42 N37 C49 63(3) . . . no C42 N37 C50 70(2) . . 1_645 no C44 N37 C46 86(5) . . . no C44 N37 C47 80(3) . . . no C44 N37 C49 156(3) . . . no C44 N37 C50 50(2) . . 1_645 no C46 N37 C47 97(5) . . . no C46 N37 C49 106(6) . . . no C46 N37 C50 119(5) . . 1_645 no C47 N37 C49 118(4) . . . no C47 N37 C50 110(3) . . 1_645 no C49 N37 C50 107(4) . . 1_645 no N51 N51 C52 72(3) 7_755 . 7_666 no N51 N51 C52 52(3) 7_755 . 1_644 no N51 N51 C53 89(4) 7_755 . 1_644 no N51 N51 C54 138(4) 7_755 . 1_545 no N51 N51 C56 106(4) 7_755 . 1_554 no N51 N51 C58 114(4) 7_755 . . no C52 N51 C52 124(3) 7_666 . 1_644 no C52 N51 C52 124(3) 1_644 . 7_666 no C52 N51 C53 151(5) 7_666 . 1_644 no C52 N51 C53 42(3) 1_644 . 1_644 no C52 N51 C54 107(3) 7_666 . 1_545 no C52 N51 C54 114(3) 1_644 . 1_545 no C52 N51 C56 72(3) 7_666 . 1_554 no C52 N51 C56 120(3) 1_644 . 1_554 no C52 N51 C58 107(3) 7_666 . . no C52 N51 C58 97(3) 1_644 . . no C53 N51 C54 73(4) 1_644 . 1_545 no C53 N51 C56 136(4) 1_644 . 1_554 no C53 N51 C58 101(4) 1_644 . . no C54 N51 C56 114(3) 1_545 . 1_554 no C54 N51 C58 106(3) 1_545 . . no C56 N51 C58 36(2) 1_554 . . no C55 N61 C60 124(7) . . 1_545 no N64 N64 C63 42(5) 8_665 . 8_665 no N64 N64 C63 95(8) 8_665 . . no C63 N64 C63 137(5) . . 8_665 no C63 N64 C63 137(5) 8_665 . . no N28 C29 C30 114(2) . . . no N28 C31 C32 119(3) . . . no N28 C33 C34 117.1(16) 1_456 . 1_456 no N28 C35 C36 116.0(14) . . . no N37 C38 C39 117(3) . . . no N37 C38 C46 58(5) . . . no N37 C38 C49 54(3) . . . no C39 C38 C46 63(5) . . . no C39 C38 C49 159(4) . . . no C46 C38 C49 100(6) . . . no C38 C39 C46 63(5) . . . no N37 C40 C41 118(2) . . . no N37 C40 C46 58(4) . . . no N37 C40 C47 80(4) . . . no N37 C40 C48 141(4) . . 1_645 no C41 C40 C46 148(5) . . . no C41 C40 C47 39(4) . . . no C41 C40 C48 37(3) . . 1_645 no C46 C40 C47 122(6) . . . no C46 C40 C48 161(5) . . 1_645 no C47 C40 C48 72(5) . . 1_645 no C40 C41 C47 42(4) . . . no C40 C41 C48 55(5) . . 1_645 no C47 C41 C48 93(6) . . 1_645 no N37 C42 C43 116.1(18) . . 1_645 no N37 C42 C49 54(3) . . . no N37 C42 C50 55.0(19) . . 1_645 no C43 C42 C49 68(3) 1_645 . . no C43 C42 C50 153(3) 1_645 . 1_645 no C49 C42 C50 90(3) . . 1_645 no C42 C43 C49 57(3) 1_465 . 1_465 no N37 C44 C45 111(3) . . . no N37 C44 C50 62(3) . . 1_645 no C45 C44 C50 55(3) . . 1_645 no C44 C45 C50 54(3) . . 1_645 no N37 C46 C38 62(5) . . . no N37 C46 C39 113(7) . . . no N37 C46 C40 56(4) . . . no C38 C46 C39 54(4) . . . no C38 C46 C40 104(7) . . . no C39 C46 C40 154(8) . . . no N37 C47 C40 59(4) . . . no N37 C47 C41 157(7) . . . no N37 C47 C48 115(5) . . 1_645 no C40 C47 C41 99(6) . . . no C40 C47 C48 61(4) . . 1_645 no C41 C47 C48 42(4) . . 1_645 no C40 C48 C41 88(6) 1_465 . 1_465 no C40 C48 C47 46(4) 1_465 . 1_465 no C41 C48 C47 45(4) 1_465 . 1_465 no N37 C49 C38 67(4) . . . no N37 C49 C42 63(3) . . . no N37 C49 C43 113(5) . . 1_645 no C38 C49 C42 119(5) . . . no C38 C49 C43 169(5) . . 1_645 no C42 C49 C43 55(3) . . 1_645 no N37 C50 C42 55(2) 1_465 . 1_465 no N37 C50 C44 68(3) 1_465 . 1_465 no N37 C50 C45 130(4) 1_465 . 1_465 no C42 C50 C44 108(4) 1_465 . 1_465 no C42 C50 C45 170(5) 1_465 . 1_465 no C44 C50 C45 71(3) 1_465 . 1_465 no N51 C52 N51 56(3) 7_666 . 1_466 no N51 C52 N51 56(3) 1_466 . 7_666 no N51 C52 C53 76(5) 1_466 . . no N51 C52 C53 122(6) 7_666 . . no N51 C52 C56 95(3) 1_466 . 7_667 no N51 C52 C56 68(3) 7_666 . 7_667 no C53 C52 C56 89(5) . . 7_667 no N51 C53 C52 62(5) 1_466 . . no N51 C53 C54 48(3) 1_466 . 1_456 no N51 C53 C55 87(5) 1_466 . 1_466 no C52 C53 C54 109(7) . . 1_456 no C52 C53 C55 147(8) . . 1_466 no C54 C53 C55 44(3) 1_456 . 1_466 no N51 C54 C53 59(4) 1_565 . 1_654 no N51 C54 C55 111(4) 1_565 . 1_565 no C53 C54 C55 60(4) 1_654 . 1_565 no N61 C55 C53 153(5) . . 1_644 no N61 C55 C54 78(4) . . 1_545 no C53 C55 C54 76(5) 1_644 . 1_545 no N51 C56 C52 40.9(17) 1_556 . 7_667 no N51 C56 C57 106(4) 1_556 . . no N51 C56 C58 60(4) 1_556 . 1_556 no C52 C56 C57 124(4) 7_667 . . no C52 C56 C58 101(5) 7_667 . 1_556 no C57 C56 C58 75(5) . . 1_556 no C56 C57 C58 42(3) . . 1_556 no N51 C58 C56 84(5) . . 1_554 no N51 C58 C57 113(4) . . 1_554 no C56 C58 C57 63(4) 1_554 . 1_554 no N61 C60 C59 173(10) 1_565 . . no N64 C63 N64 43(5) . . 8_665 no N64 C63 N64 43(5) 8_665 . . no N64 C63 C62 114(5) 8_665 . . no N64 C63 C62 155(7) . . . no N28 C29 H1 108.2(19) . . . no N28 C29 H2 108(2) . . . no C30 C29 H1 108(3) . . . no C30 C29 H2 108(2) . . . no H1 C29 H2 110(3) . . . no C29 C30 H3 108(3) . . . no C29 C30 H4 109(3) . . . no C29 C30 H5 109(3) . . . no H3 C30 H4 110(3) . . . no H3 C30 H5 110(3) . . . no H4 C30 H5 111(3) . . . no N28 C31 H6 107(3) . . . no N28 C31 H7 108(3) . . . no C32 C31 H6 106(3) . . . no C32 C31 H7 107(3) . . . no H6 C31 H7 110(3) . . . no C31 C32 H8 109(3) . . . no C31 C32 H9 109(3) . . . no C31 C32 H10 109(4) . . . no H8 C32 H9 110(4) . . . no H8 C32 H10 110(3) . . . no H9 C32 H10 110(3) . . . no N28 C33 H11 107.3(18) 1_456 . . no N28 C33 H12 107.4(18) 1_456 . . no C34 C33 H11 108(2) 1_456 . . no C34 C33 H12 107.9(18) 1_456 . . no H11 C33 H12 109.0(19) . . . no C33 C34 H13 110(2) 1_654 . . no C33 C34 H14 109.7(16) 1_654 . . no C33 C34 H15 110(2) 1_654 . . no H13 C34 H14 109(2) . . . no H13 C34 H15 109.3(18) . . . no H14 C34 H15 109(2) . . . no N28 C35 H16 108.0(15) . . . no N28 C35 H17 107.3(16) . . . no C36 C35 H16 108.2(17) . . . no C36 C35 H17 107.8(17) . . . no H16 C35 H17 109.5(15) . . . no C35 C36 H18 109.3(17) . . . no C35 C36 H19 109.3(18) . . . no C35 C36 H20 110(2) . . . no H18 C36 H19 110(2) . . . no H18 C36 H20 110(2) . . . no H19 C36 H20 109.6(19) . . . no # The following lines may be used to test the character set of files sent by # network email or other means. They are not part of the CIF data archive. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ #===END