# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1612 ############################################################################## # IUMSC CIF Archive file # ############################################################################## data_MSC96136 _audit_creation_method 'minor manual editing of SDT2CIF v. 1.2 BETA output' _chemical_formula_sum 'C50 H60 Cl4 N8 O7 V2' _chemical_formula_moiety 'C44 H36 Cl2 N16 O V2 2+, 2(Cl 1-), 6(C H4 O)' _chemical_formula_weight 1128.77 _cell_length_a 13.2692(17) _cell_length_b 29.629(3) _cell_length_c 14.3184(19) _cell_angle_alpha 90 _cell_angle_beta 114.928(6) _cell_angle_gamma 90 _cell_volume 5104.8(11) _cell_formula_units_Z 4 _cell_measurement_reflns_used 160 _cell_measurement_theta_min 10.16 _cell_measurement_theta_max 17.36 _cell_measurement_temperature 101 _exptl_crystal_colour 'dark purple/black' _exptl_crystal_description prismatic _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 0.635 _exptl_absorpt_correction_type none _exptl_absorpt_process_details none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z 1/2+x,1/2-y,1/2+z -x,-y,-z _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature 101 _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 13338 _diffrn_reflns_av_R_equivalents 0.057 _diffrn_reflns_theta_min 3.0 _diffrn_reflns_theta_max 22.5 _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_standards_number 4 _diffrn_standards_decay_% -2.6 _diffrn_standards_interval_count 200 _reflns_number_total 6684 _reflns_number_gt 4874 _reflns_threshold_expression F>3.0\s(F) 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 6684 _refine_ls_number_parameters 224 _refine_ls_hydrogen_treatment noref _refine_ls_extinction_coef 0.000000054(18) _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 0.0603 _refine_ls_wR_factor_ref 0.0616 _refine_ls_goodness_of_fit_ref 1.3855 _refine_ls_shift/su_max 0.004 _refine_diff_density_max 0.94 _refine_diff_density_min -0.57 _refine_special_details ; The asymmetric unit contains the desired cation, two Cl anions and a total of six molecules of methanol solvent. Two of the solvent molecules are disordered. O(68)-C(69)-O(68)' has a common carbon atom and two positions for the oxygen of 65 and 35% occupancy, respectively for O(68) and O(68)'. O(70)-C(71) and O(72)-C(73) are two positions for the sixth solvent molecule, with occupancies of 68 and 32% respectively. The methanol molecules are involved in hydrogen bonding to the Cl-anions. Many hydrogen atoms were located on the main cation, hydrogen atoms were introduced in fixed calculated positions for the final cycles of least-squares refinement. Atoms 1 through 67 were refined using anisotropic thermal parameters and the disordered solvent atoms were refined with isotropic thermal parameters. The largest delta/sigma was 0.04 for thermal parameters and 0.002 for positional parameters. Hydrogen atoms were not introduced on all solvent molecules ; _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 0.55737(8) 0.37894(3) 0.14307(7) 0.0152 Uani 1 0 . O2 O 0.5967(3) 0.37751(13) 0.2789(3) 0.0161 Uani 1 0 . V3 V 0.63645(8) 0.37418(3) 0.41499(7) 0.0156 Uani 1 0 . Cl4 Cl 0.51161(13) 0.37762(5) -0.03805(11) 0.0234 Uani 1 0 . Cl5 Cl 0.68796(13) 0.36895(6) 0.59798(11) 0.0243 Uani 1 0 . N6 N 0.4270(4) 0.42896(16) 0.0958(3) 0.0161 Uani 1 0 . C7 C 0.3174(5) 0.4202(2) 0.0445(5) 0.0234 Uani 1 0 . C8 C 0.2367(5) 0.4529(2) 0.0138(5) 0.0254 Uani 1 0 . C9 C 0.2683(5) 0.4974(2) 0.0306(5) 0.0254 Uani 1 0 . C10 C 0.3811(5) 0.5075(2) 0.0773(5) 0.0215 Uani 1 0 . C11 C 0.4589(5) 0.4726(2) 0.1102(4) 0.0174 Uani 1 0 . C12 C 0.5799(5) 0.4813(2) 0.1574(4) 0.0172 Uani 1 0 . C13 C 0.6243(5) 0.5238(2) 0.1850(5) 0.0228 Uani 1 0 . C14 C 0.7380(5) 0.5293(2) 0.2269(5) 0.0252 Uani 1 0 . C15 C 0.8044(5) 0.4918(2) 0.2420(5) 0.023 Uani 1 0 . C16 C 0.7558(5) 0.4496(2) 0.2152(4) 0.0183 Uani 1 0 . N17 N 0.6445(4) 0.44413(17) 0.1707(4) 0.0186 Uani 1 0 . C18 C 0.8245(5) 0.4078(2) 0.2329(5) 0.0243 Uani 1 0 . C19 C 0.8043(5) 0.3815(2) 0.1335(5) 0.0258 Uani 1 0 . N20 N 0.6731(4) 0.32686(17) 0.1431(4) 0.0198 Uani 1 0 . C21 C 0.7696(5) 0.3342(2) 0.1344(4) 0.0202 Uani 1 0 . C22 C 0.8324(5) 0.2984(2) 0.1256(5) 0.0273 Uani 1 0 . C23 C 0.7971(6) 0.2548(2) 0.1248(5) 0.0315 Uani 1 0 . C24 C 0.6963(6) 0.2473(2) 0.1286(5) 0.0295 Uani 1 0 . C25 C 0.6361(5) 0.2839(2) 0.1393(4) 0.0203 Uani 1 0 . C26 C 0.5281(5) 0.2784(2) 0.1445(4) 0.0158 Uani 1 0 . C27 C 0.4895(5) 0.2361(2) 0.1575(4) 0.0208 Uani 1 0 . C28 C 0.3864(5) 0.2331(2) 0.1611(5) 0.027 Uani 1 0 . C29 C 0.3264(5) 0.2721(2) 0.1517(5) 0.0249 Uani 1 0 . C30 C 0.3693(5) 0.3127(2) 0.1391(4) 0.022 Uani 1 0 . N31 N 0.4684(4) 0.31663(17) 0.1351(3) 0.0178 Uani 1 0 . N32 N 0.7498(4) 0.43036(17) 0.4648(4) 0.018 Uani 1 0 . C33 C 0.8593(5) 0.4263(2) 0.5157(4) 0.0231 Uani 1 0 . C34 C 0.9297(5) 0.4628(2) 0.5562(5) 0.0262 Uani 1 0 . C35 C 0.8842(5) 0.5055(2) 0.5435(5) 0.0275 Uani 1 0 . C36 C 0.7701(5) 0.5103(2) 0.4947(5) 0.0253 Uani 1 0 . C37 C 0.7046(5) 0.4722(2) 0.4558(4) 0.0203 Uani 1 0 . C38 C 0.5808(5) 0.4745(2) 0.4085(4) 0.0173 Uani 1 0 . C39 C 0.5250(5) 0.5151(2) 0.3858(5) 0.0228 Uani 1 0 . C40 C 0.4099(5) 0.5146(2) 0.3455(5) 0.024 Uani 1 0 . C41 C 0.3562(5) 0.4733(2) 0.3276(5) 0.0241 Uani 1 0 . C42 C 0.4172(5) 0.4338(2) 0.3503(5) 0.0228 Uani 1 0 . N43 N 0.5301(4) 0.43403(17) 0.3921(3) 0.0145 Uani 1 0 . C44 C 0.3635(5) 0.3884(2) 0.3295(5) 0.0252 Uani 1 0 . C45 C 0.3954(5) 0.3607(2) 0.4287(5) 0.0297 Uani 1 0 . N46 N 0.5380(4) 0.31494(17) 0.4127(3) 0.0203 Uani 1 0 . C47 C 0.4422(5) 0.3154(2) 0.4236(4) 0.0224 Uani 1 0 . C48 C 0.3917(5) 0.2758(2) 0.4331(5) 0.0272 Uani 1 0 . C49 C 0.4423(6) 0.2350(2) 0.4364(5) 0.0306 Uani 1 0 . C50 C 0.5423(5) 0.2341(2) 0.4286(5) 0.0248 Uani 1 0 . C51 C 0.5877(5) 0.2745(2) 0.4151(4) 0.0189 Uani 1 0 . C52 C 0.6961(5) 0.2760(2) 0.4079(4) 0.017 Uani 1 0 . C53 C 0.7462(5) 0.2371(2) 0.3942(4) 0.0213 Uani 1 0 . C54 C 0.8483(5) 0.2396(2) 0.3911(5) 0.025 Uani 1 0 . C55 C 0.8986(5) 0.2815(2) 0.4022(5) 0.026 Uani 1 0 . C56 C 0.8441(5) 0.3193(2) 0.4155(4) 0.0191 Uani 1 0 . N57 N 0.7423(4) 0.31704(17) 0.4177(3) 0.017 Uani 1 0 . Cl58 Cl 1.10812(14) 0.37003(6) 0.59676(14) 0.0351 Uani 1 0 . Cl59 Cl 0.58752(13) 0.13577(6) 0.59174(12) 0.0308 Uani 1 0 . O60 O 0.3859(4) 0.07655(18) 0.4477(4) 0.0421 Uani 1 0 . C61 C 0.3009(7) 0.1055(3) 0.3797(6) 0.0552 Uani 1 0 . O62 O 1.1343(4) 0.36198(18) 0.8228(4) 0.0441 Uani 1 0 . C63 C 1.0330(7) 0.3817(3) 0.8059(6) 0.0461 Uani 1 0 . O64 O 1.3398(4) 0.39672(17) 0.6187(4) 0.0398 Uani 1 0 . C65 C 1.4212(6) 0.3671(3) 0.6847(5) 0.0403 Uani 1 0 . O66 O 0.5712(4) 0.05230(16) 0.7253(4) 0.0367 Uani 1 0 . C67 C 0.5548(6) 0.0128(3) 0.6648(6) 0.041 Uani 1 0 . O68 O 0.6404(6) 0.1829(3) 0.7911(6) 0.0463 Uiso 0.65 0 . C69 C 0.6060(7) 0.1537(3) 0.8478(7) 0.0561 Uiso 1 0 . O68' O 0.6519(12) 0.1812(5) 0.9333(11) 0.0443 Uiso 0.35 0 . O70 O 0.5501(8) 0.2656(4) 0.7876(7) 0.0748 Uiso 0.68 0 . C71 C 0.6347(11) 0.2978(5) 0.8251(10) 0.0541 Uiso 0.68 0 . O72 O 0.5859(16) 0.2792(7) 0.6740(15) 0.0694 Uiso 0.32 0 . C73 C 0.627(2) 0.2808(11) 0.774(2) 0.0606 Uiso 0.32 0 . H1 H 0.2968 0.3889 0.0298 0.033 Uiso 1 0 . H2 H 0.1585 0.4443 -0.0184 0.0356 Uiso 1 0 . H3 H 0.2139 0.5216 0.0103 0.0345 Uiso 1 0 . H4 H 0.4056 0.5385 0.0862 0.0328 Uiso 1 0 . H5 H 0.5754 0.549 0.176 0.0346 Uiso 1 0 . H6 H 0.7718 0.5587 0.2456 0.0385 Uiso 1 0 . H7 H 0.8838 0.4945 0.2708 0.0331 Uiso 1 0 . H8 H 0.9027 0.4163 0.2668 0.0365 Uiso 1 0 . H9 H 0.8101 0.3885 0.2795 0.0365 Uiso 1 0 . H10 H 0.748 0.3969 0.0768 0.039 Uiso 1 0 . H11 H 0.871 0.3813 0.1231 0.039 Uiso 1 0 . H12 H 0.9018 0.304 0.1219 0.0362 Uiso 1 0 . H13 H 0.8428 0.2301 0.1221 0.044 Uiso 1 0 . H14 H 0.6672 0.217 0.1241 0.0426 Uiso 1 0 . H15 H 0.5338 0.2099 0.1613 0.0353 Uiso 1 0 . H16 H 0.3584 0.2041 0.1697 0.0405 Uiso 1 0 . H17 H 0.2548 0.2711 0.1556 0.0381 Uiso 1 0 . H18 H 0.3253 0.3397 0.1304 0.0347 Uiso 1 0 . H19 H 0.8915 0.3968 0.5272 0.0335 Uiso 1 0 . H20 H 1.0094 0.4586 0.5877 0.0392 Uiso 1 0 . H21 H 0.931 0.5311 0.5723 0.0393 Uiso 1 0 . H22 H 0.7363 0.5398 0.4856 0.0354 Uiso 1 0 . H23 H 0.5654 0.5432 0.4005 0.0344 Uiso 1 0 . H24 H 0.367 0.5422 0.3286 0.0375 Uiso 1 0 . H25 H 0.2761 0.472 0.2994 0.0324 Uiso 1 0 . H26 H 0.2846 0.3921 0.2968 0.0368 Uiso 1 0 . H27 H 0.3861 0.3723 0.2836 0.0368 Uiso 1 0 . H28 H 0.4508 0.3772 0.4853 0.0402 Uiso 1 0 . H29 H 0.3318 0.3571 0.4433 0.0402 Uiso 1 0 . H30 H 0.3212 0.2772 0.4385 0.0391 Uiso 1 0 . H31 H 0.408 0.2072 0.4454 0.0444 Uiso 1 0 . H32 H 0.5789 0.206 0.4302 0.0387 Uiso 1 0 . H33 H 0.7078 0.2081 0.3879 0.0318 Uiso 1 0 . H34 H 0.886 0.2134 0.3824 0.0389 Uiso 1 0 . H35 H 0.9697 0.2844 0.4002 0.0367 Uiso 1 0 . H36 H 0.879 0.3486 0.4235 0.0334 Uiso 1 0 . H37 H 0.461 0.0895 0.4983 0.038 Uiso 1 0 . H38 H 0.281 0.1272 0.4187 0.0634 Uiso 1 0 . H39 H 0.3249 0.1208 0.3348 0.0634 Uiso 1 0 . H40 H 0.2363 0.088 0.34 0.0634 Uiso 1 0 . H41 H 1.1422 0.366 0.7583 0.038 Uiso 1 0 . H42 H 1.0229 0.3814 0.8687 0.0577 Uiso 1 0 . H43 H 0.9729 0.3657 0.7548 0.0577 Uiso 1 0 . H44 H 1.0309 0.4124 0.7847 0.0577 Uiso 1 0 . H45 H 1.2667 0.3861 0.6227 0.038 Uiso 1 0 . H46 H 1.4933 0.3808 0.7083 0.0502 Uiso 1 0 . H47 H 1.4221 0.3398 0.649 0.0502 Uiso 1 0 . H48 H 1.4077 0.3596 0.743 0.0502 Uiso 1 0 . H49 H 0.4823 0.012 0.6111 0.0505 Uiso 1 0 . H50 H 0.6081 0.0112 0.6365 0.0505 Uiso 1 0 . H51 H 0.5646 -0.0134 0.708 0.0505 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 0.0169 0.0133 0.0111 -0.0002 0.0019 0.001 O2 0.0149 0.0147 0.0149 0.0014 0.0026 0.001 V3 0.0162 0.0147 0.0117 -0.0002 0.0019 0.0004 Cl4 0.0301 0.0218 0.0149 0.0005 0.006 0.0019 Cl5 0.0288 0.0262 0.0129 0.002 0.004 0.0004 N6 0.0171 0.0138 0.0117 -0.0023 0.0006 0.0025 C7 0.0203 0.0142 0.0294 0.0013 0.0044 0.0033 C8 0.0151 0.0329 0.0218 -0.0004 0.0015 0.0057 C9 0.0224 0.028 0.0243 0.0061 0.0084 0.0023 C10 0.0281 0.0147 0.0202 0.0013 0.0087 -0.0008 C11 0.0181 0.0191 0.0098 -0.0016 0.0008 0.001 C12 0.0178 0.0173 0.0162 0.0043 0.0069 0.0018 C13 0.0277 0.0191 0.0183 0.0014 0.0064 0.0002 C14 0.0344 0.0165 0.0225 -0.0105 0.0098 -0.0045 C15 0.0186 0.0249 0.0192 -0.0022 0.0019 0 C16 0.0183 0.0169 0.0151 -0.0033 0.0025 0.001 N17 0.0178 0.0209 0.0129 -0.0042 0.0025 0.0027 C18 0.0205 0.0254 0.0221 -0.0007 0.0044 -0.0006 C19 0.0191 0.0307 0.0289 0.002 0.0113 0.0016 N20 0.0224 0.0205 0.0112 0.0038 0.0019 0.0019 C21 0.0203 0.0222 0.0163 0.0047 0.006 0.0043 C22 0.0277 0.0316 0.0206 0.0027 0.0082 0.0019 C23 0.0378 0.0325 0.0237 0.0141 0.0124 0.0066 C24 0.0388 0.0191 0.0278 -0.0016 0.0112 -0.0021 C25 0.0248 0.0169 0.0149 -0.0009 0.0043 0.0027 C26 0.0184 0.0187 0.0048 0.0002 -0.0005 0.0002 C27 0.0262 0.0165 0.0121 -0.0004 0.0006 0.0016 C28 0.032 0.0196 0.0168 -0.0125 -0.0021 -0.0008 C29 0.0247 0.0276 0.0181 -0.0063 0.0047 0.0004 C30 0.0198 0.0294 0.0131 -0.0061 0.0032 -0.0018 N31 0.0291 0.0147 0.005 -0.0007 0.0027 0.0021 N32 0.0158 0.0205 0.0149 0.0005 0.0036 0.0025 C33 0.0278 0.0218 0.0148 0.0065 0.0041 -0.0002 C34 0.0243 0.028 0.0208 -0.0033 0.0041 -0.0055 C35 0.026 0.0227 0.0272 -0.0081 0.0047 -0.0027 C36 0.024 0.024 0.0265 0.0049 0.0093 0.0012 C37 0.0247 0.0236 0.0114 0.0011 0.0066 0.0039 C38 0.0189 0.0213 0.0127 0.0002 0.0078 -0.0006 C39 0.0266 0.0218 0.0179 0.0052 0.0074 0.0008 C40 0.0249 0.0271 0.0198 0.0058 0.0093 0.0062 C41 0.0153 0.0342 0.0215 0.0047 0.0066 -0.0016 C42 0.0246 0.0289 0.017 0.0004 0.0108 -0.0066 N43 0.0112 0.02 0.0081 0.0016 0 -0.0021 C44 0.0189 0.0249 0.029 -0.0061 0.0074 -0.0057 C45 0.0318 0.0382 0.0246 -0.0063 0.0173 -0.0037 N46 0.0283 0.0213 0.0073 0.0014 0.0038 0.0004 C47 0.024 0.0338 0.0112 -0.0016 0.009 -0.0019 C48 0.0274 0.0382 0.0204 -0.0134 0.0145 -0.0029 C49 0.0401 0.0276 0.0268 -0.0117 0.0167 -0.0014 C50 0.0263 0.0294 0.0163 -0.0056 0.0067 -0.0021 C51 0.0244 0.0196 0.0094 -0.0056 0.0039 -0.0027 C52 0.0187 0.0156 0.0099 -0.0027 -0.0006 0.0025 C53 0.0286 0.0182 0.0092 -0.0011 0.0003 0 C54 0.0328 0.0196 0.0166 0.0047 0.0044 -0.0041 C55 0.0202 0.0325 0.0193 0.0034 0.0023 0.0035 C56 0.0186 0.0218 0.0121 0.0018 0.0018 0.0019 N57 0.0209 0.0165 0.0093 0.0002 0.0022 0.0008 Cl58 0.0285 0.0262 0.0481 0.002 0.0138 -0.0031 Cl59 0.0213 0.0369 0.0272 -0.0027 0.0034 0.0115 O60 0.0425 0.0458 0.0313 -0.0108 0.009 -0.0041 C61 0.0523 0.0743 0.0255 -0.0168 0.0032 0.0088 O62 0.0406 0.04 0.049 0.0092 0.0164 0.0072 C63 0.0498 0.0427 0.0463 0.0089 0.0208 -0.0096 O64 0.0436 0.0334 0.0519 -0.0004 0.0295 0.0096 C65 0.048 0.0387 0.0256 -0.0002 0.0073 0.0025 O66 0.035 0.0342 0.0375 -0.0005 0.0119 -0.0037 C67 0.029 0.0418 0.0499 -0.0042 0.0143 -0.0037 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 Cl4 2.4018(11) . . no V1 O2 1.789(2) . . no V1 N6 2.158(3) . . no V1 N17 2.200(2) . . no V1 N20 2.177(4) . . no V1 N31 2.168(3) . . no V3 Cl5 2.4180(10) . . no V3 O2 1.794(2) . . no V3 N32 2.153(3) . . no V3 N43 2.203(3) . . no V3 N46 2.180(3) . . no V3 N57 2.190(3) . . no O60 C61 1.425(5) . . no O62 C63 1.390(9) . . no O64 C65 1.403(5) . . no O66 C67 1.418(3) . . no O68 C69 1.388(9) . . no O68' C69 1.381(6) . . no O70 C71 1.397(11) . . no O70 C73 1.21(3) . . no O72 C73 1.303(17) . . no N6 C7 1.350(7) . . no N6 C11 1.348(2) . . no N17 C12 1.358(5) . . no N17 C16 1.349(7) . . no N20 C21 1.355(8) . . no N20 C25 1.358(3) . . no N31 C26 1.356(5) . . no N31 C30 1.346(9) . . no N32 C33 1.329(7) . . no N32 C37 1.359(3) . . no N43 C38 1.346(3) . . no N43 C42 1.359(8) . . no N46 C47 1.344(9) . . no N46 C51 1.359(4) . . no N57 C52 1.344(3) . . no N57 C56 1.365(8) . . no C7 C8 1.372(6) . . no C8 C9 1.374(2) . . no C9 C10 1.391(8) . . no C10 C11 1.397(5) . . no C11 C12 1.479(8) . . no C12 C13 1.377(3) . . no C13 C14 1.378(9) . . no C14 C15 1.377(6) . . no C15 C16 1.384(3) . . no C16 C18 1.494(5) . . no C18 C19 1.544(5) . . no C19 C21 1.479(3) . . no C21 C22 1.385(6) . . no C22 C23 1.374(4) . . no C23 C24 1.379(11) . . no C24 C25 1.392(6) . . no C25 C26 1.474(9) . . no C26 C27 1.395(4) . . no C27 C28 1.393(10) . . no C28 C29 1.377(5) . . no C29 C30 1.377(5) . . no C33 C34 1.389(5) . . no C34 C35 1.378(4) . . no C35 C36 1.383(9) . . no C36 C37 1.392(4) . . no C37 C38 1.491(8) . . no C38 C39 1.376(4) . . no C39 C40 1.387(9) . . no C40 C41 1.386(4) . . no C41 C42 1.381(5) . . no C42 C44 1.491(4) . . no C44 C45 1.537(4) . . no C45 C47 1.495(4) . . no C47 C48 1.387(5) . . no C48 C49 1.372(5) . . no C49 C50 1.379(11) . . no C50 C51 1.389(5) . . no C51 C52 1.486(9) . . no C52 C53 1.383(5) . . no C53 C54 1.375(10) . . no C54 C55 1.384(4) . . no C55 C56 1.390(6) . . no C71 C73 0.857(17) . . no O60 H37 1.027(4) . . no O62 H41 0.980(4) . . no O64 H45 1.043(5) . . no C7 H1 0.9644(13) . . no C8 H2 0.974(6) . . no C9 H3 0.972(4) . . no C10 H4 0.9640(19) . . no C13 H5 0.963(4) . . no C14 H6 0.966(2) . . no C15 H7 0.959(6) . . no C18 H8 0.975(6) . . no C18 H9 0.956(4) . . no C19 H10 0.955(3) . . no C19 H11 0.958(7) . . no C22 H12 0.958(7) . . no C23 H13 0.960(5) . . no C24 H14 0.968(3) . . no C27 H15 0.962(4) . . no C28 H16 0.964(3) . . no C29 H17 0.976(7) . . no C30 H18 0.965(4) . . no C33 H19 0.954(2) . . no C34 H20 0.968(6) . . no C35 H21 0.957(3) . . no C36 H22 0.965(3) . . no C39 H23 0.965(3) . . no C40 H24 0.966(3) . . no C41 H25 0.966(6) . . no C44 H26 0.956(6) . . no C44 H27 0.957(5) . . no C45 H28 0.965(3) . . no C45 H29 0.957(7) . . no C48 H30 0.971(7) . . no C49 H31 0.975(4) . . no C50 H32 0.961(4) . . no C53 H33 0.985(3) . . no C54 H34 0.962(4) . . no C55 H35 0.961(7) . . no C56 H36 0.968(3) . . no C61 H38 0.958(6) . . no C61 H39 0.944(7) . . no C61 H40 0.958(6) . . no C63 H42 0.965(6) . . no C63 H43 0.950(5) . . no C63 H44 0.9544(16) . . no C65 H46 0.960(7) . . no C65 H47 0.958(3) . . no C65 H48 0.952(6) . . no C67 H49 0.945(5) . . no C67 H50 0.952(8) . . no C67 H51 0.966(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 Cl4 V1 O2 176.90(10) . . . no Cl4 V1 N6 82.42(8) . . . no Cl4 V1 N17 94.78(8) . . . no Cl4 V1 N20 81.14(7) . . . no Cl4 V1 N31 92.58(7) . . . no O2 V1 N6 100.67(12) . . . no O2 V1 N17 86.25(9) . . . no O2 V1 N20 95.77(11) . . . no O2 V1 N31 86.55(9) . . . no N6 V1 N17 75.21(14) . . . no N6 V1 N20 163.48(9) . . . no N6 V1 N31 102.80(16) . . . no N17 V1 N20 107.77(16) . . . no N17 V1 N31 172.03(14) . . . no N20 V1 N31 76.40(16) . . . no Cl5 V3 O2 179.20(11) . . . no Cl5 V3 N32 81.48(8) . . . no Cl5 V3 N43 94.80(8) . . . no Cl5 V3 N46 81.86(7) . . . no Cl5 V3 N57 92.57(7) . . . no O2 V3 N32 99.30(11) . . . no O2 V3 N43 85.27(10) . . . no O2 V3 N46 97.36(10) . . . no O2 V3 N57 87.40(11) . . . no N32 V3 N43 75.00(14) . . . no N32 V3 N46 163.29(9) . . . no N32 V3 N57 103.80(15) . . . no N43 V3 N46 107.68(16) . . . no N43 V3 N57 172.26(12) . . . no N46 V3 N57 75.73(16) . . . no V1 O2 V3 178.20(2) . . . no C71 O70 C73 37.5(8) . . . no V1 N6 C7 125.13(7) . . . no V1 N6 C11 116.9(4) . . . no C7 N6 C11 117.7(3) . . . no V1 N17 C12 115.7(4) . . . no V1 N17 C16 125.30(13) . . . no C12 N17 C16 118.1(2) . . . no V1 N20 C21 125.49(8) . . . no V1 N20 C25 115.0(4) . . . no C21 N20 C25 119.1(4) . . . no V1 N31 C26 115.1(4) . . . no V1 N31 C30 126.24(15) . . . no C26 N31 C30 117.7(3) . . . no V3 N32 C33 124.09(8) . . . no V3 N32 C37 117.0(4) . . . no C33 N32 C37 118.2(3) . . . no V3 N43 C38 116.7(4) . . . no V3 N43 C42 125.41(9) . . . no C38 N43 C42 117.3(3) . . . no V3 N46 C47 125.49(12) . . . no V3 N46 C51 115.3(4) . . . no C47 N46 C51 118.5(3) . . . no V3 N57 C52 115.9(4) . . . no V3 N57 C56 126.50(10) . . . no C52 N57 C56 117.0(3) . . . no N6 C7 C8 123.7(2) . . . no C7 C8 C9 118.8(5) . . . no C8 C9 C10 118.7(4) . . . no C9 C10 C11 119.6(2) . . . no N6 C11 C10 121.3(5) . . . no N6 C11 C12 116.6(3) . . . no C10 C11 C12 122.0(2) . . . no N17 C12 C11 115.0(2) . . . no N17 C12 C13 122.2(5) . . . no C11 C12 C13 122.8(4) . . . no C12 C13 C14 119.3(4) . . . no C13 C14 C15 119.0(3) . . . no C14 C15 C16 119.5(5) . . . no N17 C16 C15 121.9(3) . . . no N17 C16 C18 116.7(2) . . . no C15 C16 C18 121.5(5) . . . no C16 C18 C19 113.9(3) . . . no C18 C19 C21 113.8(3) . . . no N20 C21 C19 117.5(4) . . . no N20 C21 C22 120.9(3) . . . no C19 C21 C22 121.6(6) . . . no C21 C22 C23 120.3(6) . . . no C22 C23 C24 118.9(5) . . . no C23 C24 C25 119.4(3) . . . no N20 C25 C24 121.3(6) . . . no N20 C25 C26 116.3(4) . . . no C24 C25 C26 122.3(3) . . . no N31 C26 C25 116.3(3) . . . no N31 C26 C27 122.0(6) . . . no C25 C26 C27 121.7(4) . . . no C26 C27 C28 119.0(4) . . . no C27 C28 C29 118.6(3) . . . no C28 C29 C30 119.6(6) . . . no N31 C30 C29 123.1(4) . . . no N32 C33 C34 123.1(3) . . . no C33 C34 C35 118.7(5) . . . no C34 C35 C36 119.2(3) . . . no C35 C36 C37 118.9(3) . . . no N32 C37 C36 121.8(5) . . . no N32 C37 C38 116.3(3) . . . no C36 C37 C38 121.8(3) . . . no N43 C38 C37 114.3(3) . . . no N43 C38 C39 123.9(5) . . . no C37 C38 C39 121.8(3) . . . no C38 C39 C40 118.6(3) . . . no C39 C40 C41 118.3(3) . . . no C40 C41 C42 120.1(5) . . . no N43 C42 C41 121.8(3) . . . no N43 C42 C44 116.0(3) . . . no C41 C42 C44 122.3(5) . . . no C42 C44 C45 111.9(2) . . . no C44 C45 C47 113.1(4) . . . no N46 C47 C45 116.5(4) . . . no N46 C47 C48 121.6(4) . . . no C45 C47 C48 121.9(6) . . . no C47 C48 C49 119.9(6) . . . no C48 C49 C50 119.2(4) . . . no C49 C50 C51 118.9(3) . . . no N46 C51 C50 121.9(6) . . . no N46 C51 C52 116.5(3) . . . no C50 C51 C52 121.5(4) . . . no N57 C52 C51 115.5(3) . . . no N57 C52 C53 122.9(6) . . . no C51 C52 C53 121.6(3) . . . no C52 C53 C54 119.9(3) . . . no C53 C54 C55 118.5(4) . . . no C54 C55 C56 119.0(6) . . . no N57 C56 C55 122.7(3) . . . no O70 C71 C73 59(2) . . . no O70 C73 O72 99.7(18) . . . no O70 C73 C71 83(3) . . . no O72 C73 C71 143.3(13) . . . no C61 O60 H37 120.64(18) . . . no C63 O62 H41 105.4(3) . . . no C65 O64 H45 104.1(3) . . . no N6 C7 H1 116.4(4) . . . no C8 C7 H1 119.9(5) . . . no C7 C8 H2 120.01(19) . . . no C9 C8 H2 121.2(4) . . . no C8 C9 H3 121.5(6) . . . no C10 C9 H3 119.8(2) . . . no C9 C10 H4 120.3(4) . . . no C11 C10 H4 120.1(6) . . . no C12 C13 H5 119.3(6) . . . no C14 C13 H5 121.3(2) . . . no C13 C14 H6 121.5(4) . . . no C15 C14 H6 119.6(6) . . . no C14 C15 H7 120.9(3) . . . no C16 C15 H7 119.6(4) . . . no C16 C18 H8 108.45(19) . . . no C16 C18 H9 109.0(5) . . . no C19 C18 H8 108.8(5) . . . no C19 C18 H9 109.51(16) . . . no H8 C18 H9 106.9(3) . . . no C18 C19 H10 108.2(3) . . . no C18 C19 H11 109.5(4) . . . no C21 C19 H10 109.0(4) . . . no C21 C19 H11 107.8(3) . . . no H10 C19 H11 108.4(4) . . . no C21 C22 H12 120.1(3) . . . no C23 C22 H12 119.6(5) . . . no C22 C23 H13 119.8(7) . . . no C24 C23 H13 121.3(3) . . . no C23 C24 H14 120.8(5) . . . no C25 C24 H14 119.8(7) . . . no C26 C27 H15 118.8(6) . . . no C28 C27 H15 122.1(3) . . . no C27 C28 H16 120.1(4) . . . no C29 C28 H16 121.3(7) . . . no C28 C29 H17 120.4(4) . . . no C30 C29 H17 120.0(4) . . . no N31 C30 H18 118.2(3) . . . no C29 C30 H18 118.7(6) . . . no N32 C33 H19 119.0(3) . . . no C34 C33 H19 117.9(5) . . . no C33 C34 H20 120.3(3) . . . no C35 C34 H20 120.9(4) . . . no C34 C35 H21 120.1(6) . . . no C36 C35 H21 120.5(3) . . . no C35 C36 H22 120.6(3) . . . no C37 C36 H22 120.4(6) . . . no C38 C39 H23 120.6(6) . . . no C40 C39 H23 120.8(3) . . . no C39 C40 H24 121.7(3) . . . no C41 C40 H24 119.9(6) . . . no C40 C41 H25 120.0(3) . . . no C42 C41 H25 119.9(3) . . . no C42 C44 H26 109.1(3) . . . no C42 C44 H27 109.1(5) . . . no C45 C44 H26 109.4(5) . . . no C45 C44 H27 108.8(3) . . . no H26 C44 H27 108.4(3) . . . no C44 C45 H28 108.8(3) . . . no C44 C45 H29 109.7(5) . . . no C47 C45 H28 108.0(4) . . . no C47 C45 H29 109.4(3) . . . no H28 C45 H29 107.6(5) . . . no C47 C48 H30 119.6(3) . . . no C49 C48 H30 120.6(4) . . . no C48 C49 H31 119.9(7) . . . no C50 C49 H31 120.9(4) . . . no C49 C50 H32 120.6(4) . . . no C51 C50 H32 120.5(7) . . . no C52 C53 H33 118.6(6) . . . no C54 C53 H33 121.5(4) . . . no C53 C54 H34 122.3(3) . . . no C55 C54 H34 119.2(7) . . . no C54 C55 H35 120.7(4) . . . no C56 C55 H35 120.3(3) . . . no N57 C56 H36 118.0(4) . . . no C55 C56 H36 119.3(6) . . . no O60 C61 H38 109.8(4) . . . no O60 C61 H39 111.0(8) . . . no O60 C61 H40 109.41(13) . . . no H38 C61 H39 109.23(9) . . . no H38 C61 H40 108.1(9) . . . no H39 C61 H40 109.3(4) . . . no O62 C63 H42 109.8(4) . . . no O62 C63 H43 111.1(4) . . . no O62 C63 H44 110.7(7) . . . no H42 C63 H43 108.3(8) . . . no H42 C63 H44 107.9(4) . . . no H43 C63 H44 109.1(4) . . . no O64 C65 H46 110.1(3) . . . no O64 C65 H47 110.4(3) . . . no O64 C65 H48 111.2(7) . . . no H46 C65 H47 108.0(8) . . . no H46 C65 H48 108.5(3) . . . no H47 C65 H48 108.6(3) . . . no O66 C67 H49 111.0(5) . . . no O66 C67 H50 110.6(5) . . . no O66 C67 H51 109.1(3) . . . no H49 C67 H50 109.7(4) . . . no H49 C67 H51 108.5(5) . . . no H50 C67 H51 107.9(5) . . . 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_MSC98004 _audit_creation_method 'minor manual editing of SDT2CIF v. 1.0 BETA output' _chemical_formula_sum 'C24 H26 Cl3 Cr1 N4 O2' _chemical_formula_moiety ? _chemical_formula_weight 560.85 _cell_length_a 23.106(3) _cell_length_b 8.3376(9) _cell_length_c 25.770(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4964.6(10) _cell_formula_units_Z 8 _cell_measurement_reflns_used 118 _cell_measurement_theta_min 9.75 _cell_measurement_theta_max 12.26 _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 1.501 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2312 _exptl_absorpt_coefficient_mu 0.8136 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details Tompa _exptl_absorpt_correction_T_min 0.793 _exptl_absorpt_correction_T_max 0.874 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,z x,1/2-y,1/2+z 1/2-x,-y,1/2+z 1/2+x,y,1/2-z -x,1/2+y,1/2-z 1/2+x,1/2-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 5151 _diffrn_reflns_av_R_equivalents 0.057 _diffrn_reflns_theta_min 3.01279 _diffrn_reflns_theta_max 25.0006 _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 0 _diffrn_standards_number 4 _diffrn_standards_decay_% 1.3 _diffrn_standards_interval_count 300 _reflns_number_total 4358 _reflns_number_gt 2484 _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 CR Cr 0.284 0.624 '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 2858 _refine_ls_number_parameters 412 _refine_ls_hydrogen_treatment ? _refine_ls_extinction_coef 0.000000091(13) _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)+(.03F)^2^ _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.0427 _refine_ls_goodness_of_fit_ref 1.2179 _refine_ls_shift/su_max 0.0947 _refine_diff_density_max 0.49 _refine_diff_density_min -0.5 _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 CR1 CR 0.36542(3) 0.26239(10) 0.29392(3) 0.0107(2) Uani 1 0 . CL2 CL 0.36445(6) 0.53732(15) 0.30019(5) 0.0152(4) Uani 1 0 . CL3 CL 0.36710(7) 0.98836(15) 0.28784(5) 0.0161(4) Uani 1 0 . N4 N 0.30714(18) 0.2564(6) 0.35496(16) 0.0138(14) Uani 1 0 . C5 C 0.2511(3) 0.2979(7) 0.3543(2) 0.0151(17) Uani 1 0 . C6 C 0.2131(2) 0.2673(7) 0.3943(2) 0.0182(18) Uani 1 0 . C7 C 0.2339(3) 0.1891(7) 0.4377(2) 0.0198(18) Uani 1 0 . C8 C 0.2929(3) 0.1532(7) 0.4408(2) 0.0171(17) Uani 1 0 . C9 C 0.3285(3) 0.1915(7) 0.3995(2) 0.0174(17) Uani 1 0 . N10 N 0.42001(18) 0.2431(5) 0.35939(15) 0.0127(13) Uani 1 0 . C11 C 0.3926(2) 0.1902(6) 0.4023(2) 0.0152(16) Uani 1 0 . C12 C 0.4217(3) 0.1540(7) 0.4480(2) 0.0177(18) Uani 1 0 . C13 C 0.4806(2) 0.1792(7) 0.4502(2) 0.0208(18) Uani 1 0 . C14 C 0.5078(3) 0.2412(8) 0.4081(2) 0.0202(18) Uani 1 0 . C15 C 0.4777(2) 0.2712(6) 0.3623(2) 0.0157(16) Uani 1 0 . C16 C 0.5069(3) 0.3320(7) 0.3146(2) 0.0190(18) Uani 1 0 . C17 C 0.5073(2) 0.2045(7) 0.2708(2) 0.0161(17) Uani 1 0 . C18 C 0.4765(2) 0.2601(7) 0.2236(2) 0.0148(16) Uani 1 0 . C19 C 0.5053(2) 0.2887(7) 0.1771(2) 0.0167(17) Uani 1 0 . C20 C 0.4764(3) 0.3520(7) 0.1354(2) 0.0192(18) Uani 1 0 . C21 C 0.4172(2) 0.3788(7) 0.1394(2) 0.0171(17) Uani 1 0 . C22 C 0.3893(2) 0.3402(6) 0.1852(2) 0.0147(16) Uani 1 0 . N23 N 0.41848(19) 0.2860(5) 0.22762(16) 0.0113(13) Uani 1 0 . N24 N 0.30586(18) 0.2664(6) 0.23382(16) 0.0127(14) Uani 1 0 . C25 C 0.3256(2) 0.3350(6) 0.1894(2) 0.0124(16) Uani 1 0 . C26 C 0.2883(3) 0.3793(7) 0.1499(2) 0.0188(18) Uani 1 0 . C27 C 0.2307(3) 0.3448(7) 0.1544(2) 0.0209(19) Uani 1 0 . C28 C 0.2111(2) 0.2600(7) 0.1971(2) 0.0192(17) Uani 1 0 . C29 C 0.2498(2) 0.2247(7) 0.2360(2) 0.0153(17) Uani 1 0 . CL30 CL 0.65281(6) 0.12724(17) 0.45874(6) 0.0208(4) Uani 1 0 . O31 O 0.57526(17) 0.2768(5) 0.05323(15) 0.0233(14) Uani 1 0 . C32 C 0.5656(3) 0.1077(9) 0.0536(3) 0.033(2) Uani 1 0 . O33 O 0.8712(2) 0.9862(6) 0.42820(16) 0.0333(15) Uani 1 0 . C34 C 0.8346(3) 0.0938(9) 0.4555(3) 0.036(2) Uani 1 0 . H1 H 0.243(2) 0.340(6) 0.3273(18) 0.006(11) Uiso 1 0 . H2 H 0.178(2) 0.301(6) 0.3916(18) 0.013(11) Uiso 1 0 . H3 H 0.211(2) 0.169(7) 0.465(2) 0.033(11) Uiso 1 0 . H4 H 0.307(2) 0.098(7) 0.472(2) 0.024(11) Uiso 1 0 . H5 H 0.401(2) 0.111(7) 0.476(2) 0.025(11) Uiso 1 0 . H6 H 0.501(3) 0.157(7) 0.482(2) 0.039(11) Uiso 1 0 . H7 H 0.544(2) 0.253(6) 0.4073(16) -0.005(10) Uiso 1 0 . H8 H 0.486(2) 0.421(6) 0.3017(17) -0.000(10) Uiso 1 0 . H9 H 0.547(3) 0.369(8) 0.323(2) 0.040(11) Uiso 1 0 . H10 H 0.547(2) 0.189(5) 0.2657(17) 0.001(10) Uiso 1 0 . H11 H 0.487(2) 0.105(6) 0.2831(18) 0.006(10) Uiso 1 0 . H12 H 0.549(3) 0.272(8) 0.175(2) 0.053(10) Uiso 1 0 . H13 H 0.492(2) 0.376(6) 0.104(2) 0.013(11) Uiso 1 0 . H14 H 0.400(2) 0.424(7) 0.114(2) 0.026(11) Uiso 1 0 . H15 H 0.299(2) 0.432(7) 0.122(2) 0.028(11) Uiso 1 0 . H16 H 0.206(2) 0.374(7) 0.128(2) 0.031(11) Uiso 1 0 . H17 H 0.171(2) 0.220(6) 0.2001(19) 0.016(11) Uiso 1 0 . H18 H 0.240(2) 0.167(6) 0.2633(16) -0.004(10) Uiso 1 0 . H19 H 0.538(3) 0.087(8) 0.073(2) 0.041(10) Uiso 1 0 . H20 H 0.564(3) 0.075(9) 0.019(3) 0.055(10) Uiso 1 0 . H21 H 0.599(5) 0.043(12) 0.075(3) 0.118(6) Uiso 1 0 . H22 H 0.839(3) 0.075(8) 0.492(3) 0.051(10) Uiso 1 0 . H23 H 0.846(3) 0.203(8) 0.444(2) 0.040(11) Uiso 1 0 . H24 H 0.794(3) 0.065(7) 0.444(2) 0.040(11) Uiso 1 0 . H25 H 0.634(4) 0.375(10) 0.441(3) 0.088(8) Uiso 1 0 . H26 H 0.595(3) 0.298(7) 0.027(2) 0.028(11) 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 CR1 0.0096(13) 0.0108(4) 0.0117(18) 0.0000(4) 0.0007(4) 0.0012(3) CL2 0.0145(19) 0.0116(6) 0.019(3) 0.0018(6) 0.0006(6) -0.0003(5) CL3 0.016(2) 0.0125(6) 0.020(3) -0.0003(6) -0.0003(6) -0.0003(5) N4 0.014(3) 0.013(2) 0.014(3) -0.000(2) 0.0022(18) 0.001(2) C5 0.014(3) 0.017(3) 0.015(3) 0.005(2) -0.003(2) -0.002(2) C6 0.012(3) 0.015(3) 0.028(5) 0.002(3) 0.003(2) -0.005(3) C7 0.024(5) 0.018(3) 0.018(4) -0.001(3) 0.005(2) -0.001(3) C8 0.022(4) 0.015(3) 0.014(4) -0.003(3) 0.002(2) 0.000(2) C9 0.029(5) 0.010(3) 0.013(3) 0.000(2) 0.002(2) -0.003(2) N10 0.016(3) 0.008(2) 0.014(3) 0.002(2) -0.0022(19) 0.0040(19) C11 0.017(4) 0.011(3) 0.018(4) -0.000(2) -0.002(2) -0.003(2) C12 0.025(5) 0.013(3) 0.015(4) 0.003(2) 0.001(2) -0.001(2) C13 0.021(4) 0.025(3) 0.016(4) 0.002(2) -0.009(3) -0.001(3) C14 0.014(4) 0.019(3) 0.028(5) 0.007(3) -0.002(2) -0.007(3) C15 0.010(3) 0.010(3) 0.027(5) -0.000(2) -0.005(2) -0.008(3) C16 0.014(4) 0.020(3) 0.023(5) 0.002(3) -0.005(2) -0.002(3) C17 0.008(3) 0.019(3) 0.021(4) 0.001(2) 0.002(2) -0.001(2) C18 0.009(3) 0.011(3) 0.025(5) -0.001(2) -0.002(2) -0.004(2) C19 0.012(3) 0.013(3) 0.025(5) -0.000(2) 0.004(2) -0.005(2) C20 0.026(5) 0.012(3) 0.020(4) -0.002(3) 0.006(3) -0.002(3) C21 0.016(4) 0.019(3) 0.016(4) -0.001(3) -0.001(2) 0.003(3) C22 0.017(4) 0.008(3) 0.020(4) -0.002(2) -0.002(2) -0.001(2) N23 0.014(3) 0.006(2) 0.014(3) -0.0001(19) 0.0008(19) -0.0009(18) N24 0.011(3) 0.011(2) 0.017(3) 0.0015(19) 0.0011(18) 0.0049(19) C25 0.009(3) 0.012(3) 0.015(4) 0.003(2) 0.002(2) -0.002(2) C26 0.021(4) 0.019(3) 0.016(4) 0.001(3) 0.000(2) 0.001(3) C27 0.022(4) 0.023(3) 0.018(4) -0.001(3) -0.006(2) -0.001(3) C28 0.012(3) 0.018(3) 0.027(5) 0.000(3) -0.003(2) -0.002(3) C29 0.017(4) 0.014(3) 0.015(3) -0.000(2) 0.003(2) -0.001(2) CL30 0.022(3) 0.0233(8) 0.017(3) 0.0007(6) 0.0000(6) -0.0036(6) O31 0.027(4) 0.019(2) 0.024(4) -0.0018(19) 0.0088(18) -0.0005(19) C32 0.046(7) 0.024(4) 0.029(6) -0.003(3) 0.012(3) -0.001(3) O33 0.030(5) 0.038(3) 0.032(5) 0.001(2) -0.004(2) 0.001(2) C34 0.049(7) 0.029(4) 0.030(6) 0.002(3) -0.007(4) 0.001(3) 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 CR1 CL2 2.2981(17) . . no CR1 CL3 2.2905(17) . 1_545 no CR1 N4 2.071(4) . . no CR1 N10 2.113(4) . . no CR1 N23 2.112(4) . . no CR1 N24 2.072(4) . . no O31 C32 1.428(8) . . no O31 H26 0.84(6) . . no O33 C34 1.418(8) . 1_565 no O33 H25 1.00(8) . 2_655 no N4 C5 1.341(7) . . no N4 C9 1.363(7) . . no N10 C11 1.348(7) . . no N10 C15 1.356(7) . . no N23 C18 1.362(7) . . no N23 C22 1.361(6) . . no N24 C25 1.359(6) . . no N24 C29 1.343(7) . . no C5 C6 1.376(8) . . no C5 H1 0.80(5) . . no C6 C7 1.381(8) . . no C6 H2 0.87(5) . . no C7 C8 1.399(9) . . no C7 H3 0.89(6) . . no C8 C9 1.381(8) . . no C8 H4 0.98(6) . . no C9 C11 1.483(8) . . no C11 C12 1.389(7) . . no C12 C13 1.378(8) . . no C12 H5 0.93(6) . . no C13 C14 1.358(8) . . no C13 H6 0.95(6) . . no C14 C15 1.392(8) . . no C14 H7 0.83(4) . . no C15 C16 1.491(8) . . no C16 C17 1.551(7) . . no C16 H8 0.94(5) . . no C16 H9 1.00(6) . . no C17 C18 1.483(8) . . no C17 H10 0.94(5) . . no C17 H11 1.00(5) . . no C18 C19 1.390(8) . . no C19 C20 1.371(8) . . no C19 H12 1.02(7) . . no C20 C21 1.389(8) . . no C20 H13 0.90(5) . . no C21 C22 1.385(7) . . no C21 H14 0.85(5) . . no C22 C25 1.475(7) . . no C25 C26 1.384(8) . . no C26 C27 1.367(8) . . no C26 H15 0.87(6) . . no C27 C28 1.383(8) . . no C27 H16 0.92(6) . . no C28 C29 1.374(7) . . no C28 H17 1.00(5) . . no C29 H18 0.88(4) . . no C32 H19 0.84(6) . . no C32 H20 0.93(7) . . no C32 H21 1.08(10) . . no C34 H22 0.97(6) . . no C34 H23 0.99(6) . . no C34 H24 1.02(6) . . 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 CL2 CR1 CL3 179.58(7) . . 1_545 no CL2 CR1 N4 87.95(14) . . . no CL2 CR1 N10 91.46(13) . . . no CL2 CR1 N23 88.27(12) . . . no CL2 CR1 N24 91.71(14) . . . no CL3 CR1 N4 92.23(14) 1_545 . . no CL3 CR1 N10 88.21(13) 1_545 . . no CL3 CR1 N23 91.58(13) 1_545 . . no CL3 CR1 N24 88.64(14) 1_545 . . no N4 CR1 N10 77.28(16) . . . no N4 CR1 N23 173.71(18) . . . no N4 CR1 N24 97.83(15) . . . no N10 CR1 N23 107.85(15) . . . no N10 CR1 N24 174.07(17) . . . no N23 CR1 N24 77.26(16) . . . no C32 O31 H26 107(4) . . . no C34 O33 H25 110(5) 1_565 . 2_655 no CR1 N4 C5 127.8(4) . . . no CR1 N4 C9 114.4(4) . . . no C5 N4 C9 117.6(5) . . . no CR1 N10 C11 113.6(3) . . . no CR1 N10 C15 128.2(4) . . . no C11 N10 C15 118.2(5) . . . no CR1 N23 C18 128.2(4) . . . no CR1 N23 C22 113.1(3) . . . no C18 N23 C22 118.6(4) . . . no CR1 N24 C25 114.4(3) . . . no CR1 N24 C29 127.3(4) . . . no C25 N24 C29 117.9(4) . . . no N4 C5 C6 123.9(5) . . . no N4 C5 H1 111(4) . . . no C6 C5 H1 125(4) . . . no C5 C6 C7 118.3(5) . . . no C5 C6 H2 119(3) . . . no C7 C6 H2 123(3) . . . no C6 C7 C8 119.0(5) . . . no C6 C7 H3 121(4) . . . no C8 C7 H3 119(4) . . . no C7 C8 C9 119.2(6) . . . no C7 C8 H4 118(3) . . . no C9 C8 H4 123(3) . . . no N4 C9 C8 121.6(5) . . . no N4 C9 C11 113.9(5) . . . no C8 C9 C11 123.8(5) . . . no N10 C11 C9 115.2(5) . . . no N10 C11 C12 122.7(5) . . . no C9 C11 C12 121.6(5) . . . no C11 C12 C13 118.6(5) . . . no C11 C12 H5 120(3) . . . no C13 C12 H5 122(3) . . . no C12 C13 C14 118.9(5) . . . no C12 C13 H6 119(4) . . . no C14 C13 H6 122(4) . . . no C13 C14 C15 121.0(6) . . . no C13 C14 H7 122(3) . . . no C15 C14 H7 117(3) . . . no N10 C15 C14 120.5(5) . . . no N10 C15 C16 117.2(5) . . . no C14 C15 C16 122.3(5) . . . no C15 C16 C17 111.7(5) . . . no C15 C16 H8 109(3) . . . no C15 C16 H9 111(3) . . . no C17 C16 H8 107(3) . . . no C17 C16 H9 110(4) . . . no H8 C16 H9 107(5) . . . no C16 C17 C18 112.3(5) . . . no C16 C17 H10 102(3) . . . no C16 C17 H11 109(3) . . . no C18 C17 H10 114(3) . . . no C18 C17 H11 107(3) . . . no H10 C17 H11 113(4) . . . no N23 C18 C17 117.4(5) . . . no N23 C18 C19 120.7(5) . . . no C17 C18 C19 122.0(5) . . . no C18 C19 C20 120.5(5) . . . no C18 C19 H12 119(4) . . . no C20 C19 H12 120(4) . . . no C19 C20 C21 119.0(5) . . . no C19 C20 H13 126(3) . . . no C21 C20 H13 115(3) . . . no C20 C21 C22 118.9(5) . . . no C20 C21 H14 118(4) . . . no C22 C21 H14 123(4) . . . no N23 C22 C21 122.1(5) . . . no N23 C22 C25 115.2(5) . . . no C21 C22 C25 122.3(5) . . . no N24 C25 C22 114.2(5) . . . no N24 C25 C26 121.4(5) . . . no C22 C25 C26 124.1(5) . . . no C25 C26 C27 119.3(6) . . . no C25 C26 H15 125(4) . . . no C27 C26 H15 116(4) . . . no C26 C27 C28 119.5(6) . . . no C26 C27 H16 119(4) . . . no C28 C27 H16 122(4) . . . no C27 C28 C29 118.6(5) . . . no C27 C28 H17 123(3) . . . no C29 C28 H17 119(3) . . . no N24 C29 C28 122.7(5) . . . no N24 C29 H18 115(3) . . . no C28 C29 H18 122(3) . . . no O31 C32 H19 109(5) . . . no O31 C32 H20 107(5) . . . no O31 C32 H21 113(5) . . . no H19 C32 H20 119(6) . . . no H19 C32 H21 98(6) . . . no H20 C32 H21 111(7) . . . no O33 C34 H22 109(4) 1_545 . . no O33 C34 H23 106(4) 1_545 . . no O33 C34 H24 105(3) 1_545 . . no H22 C34 H23 114(5) . . . no H22 C34 H24 110(5) . . . no H23 C34 H24 112(5) . . . 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_MSC97130 _audit_creation_method 'minor manual editing of SDT2CIF v. 1.1 BETA output' _chemical_formula_sum 'C28 H28.2 Cl1 Cu2 N4 O9.4' _chemical_formula_moiety 'C28 H28.2 Cu2 N4 O5.4 1+, Cl O4 1-' _chemical_formula_weight 733.70 _cell_length_a 7.7392(18) _cell_length_b 34.342(7) _cell_length_c 11.052(3) _cell_angle_alpha 90 _cell_angle_beta 101.774(12) _cell_angle_gamma 90 _cell_volume 2875.5(11) _cell_formula_units_Z 4 _cell_measurement_reflns_used 60 _cell_measurement_theta_min 10.84 _cell_measurement_theta_max 17.56 _cell_measurement_temperature 105 _exptl_crystal_colour green _exptl_crystal_description prism _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.695 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 1.6361 _exptl_absorpt_correction_type none _exptl_absorpt_process_details none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z x,1/2-y,1/2+z -x,-y,-z _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature 105 _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 8373 _diffrn_reflns_av_R_equivalents 0.059 _diffrn_reflns_theta_min 3.00976 _diffrn_reflns_theta_max 25.035 _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_standards_number 4 _diffrn_standards_decay_% -1.7 _diffrn_standards_interval_count 300 _diffrn_special_details ; 59 reflections suspected of being affected by overlap (due to the 34A axis) were removed from the RAW data file, after an initial data processing run. ; _reflns_number_total 5069 _reflns_number_gt 3236 _reflns_threshold_expression F>3.0\s(F) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source CU Cu 0.263 1.266 '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 5069 _refine_ls_number_parameters 400 _refine_ls_hydrogen_treatment noref _refine_ls_extinction_coef -0.00000007(5) _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 0.0614 _refine_ls_wR_factor_ref 0.0553 _refine_ls_goodness_of_fit_ref 1.1265 _refine_ls_shift/su_max 0.1087 _refine_diff_density_max 0.93 _refine_diff_density_min -0.89 _refine_special_details ; The location of the atoms in the bridging ligand containing O(37) was difficult. A dangling acetate was expected from chemical evidence but the initial difference map in the area seemed to indicate a bridging ethoxy group. Contoured maps were used in the attempts to resolve the disorder, see Fig. 4 in the report. A satisfactory disorder was eventually modelled and refined. For the particular crystal studied the composition of the disorder is 60% ethoxy (O(37) to C(39) and 40% acetate (O(37) and C(40) to C(42)). Many hydrogen atoms on the ordered atoms in the structure were located, all hydrogen atoms (except on the disordered atoms) were then introduced in fixed idealized positions with isotropic thermal parameters equal to 1.0 plus the isotropic equivalent of the parent atom. In addition to the cation of interest the asymmetric unit contained a well ordered perchlorate anion. The final full-matrix least-squares refinement was carried out using anisotropic thermal parameters on atoms Cu(1) through O(37) as well as on the perchlorate anion. The atoms involved in the disorder (C(38) through C(42)) were refined using isotropic thermal parameters. ; _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 CU1 CU 0.51771(13) 0.18550(3) 0.97392(8) 0.0333(3) Uani 1 0 . CU2 CU 0.68410(11) 0.09943(3) 0.99362(7) 0.0216(3) Uani 1 0 . N3 N 0.5145(7) 0.24497(18) 0.9766(5) 0.024(2) Uani 1 0 . C4 C 0.6081(9) 0.2681(3) 1.0654(6) 0.032(3) Uani 1 0 . C5 C 0.6191(10) 0.3078(2) 1.0498(7) 0.031(3) Uani 1 0 . C6 C 0.5343(10) 0.3244(2) 0.9413(7) 0.030(3) Uani 1 0 . C7 C 0.4368(9) 0.3014(2) 0.8490(6) 0.027(3) Uani 1 0 . C8 C 0.4291(9) 0.2617(2) 0.8695(6) 0.024(2) Uani 1 0 . C9 C 0.3304(9) 0.2333(3) 0.7784(6) 0.028(3) Uani 1 0 . C10 C 0.2227(10) 0.2460(3) 0.6696(6) 0.029(3) Uani 1 0 . C11 C 0.1360(10) 0.2176(3) 0.5893(6) 0.038(3) Uani 1 0 . C12 C 0.1625(10) 0.1789(3) 0.6190(7) 0.034(3) Uani 1 0 . C13 C 0.2720(10) 0.1682(3) 0.7289(6) 0.030(3) Uani 1 0 . N14 N 0.3553(8) 0.1953(2) 0.8092(5) 0.028(2) Uani 1 0 . C15 C 0.3054(10) 0.1262(3) 0.7610(6) 0.030(3) Uani 1 0 . C16 C 0.4444(10) 0.1088(2) 0.6970(6) 0.032(3) Uani 1 0 . C17 C 0.4901(9) 0.0677(3) 0.7353(6) 0.028(3) Uani 1 0 . C18 C 0.4284(9) 0.0370(3) 0.6559(6) 0.030(3) Uani 1 0 . C19 C 0.4651(10) -0.0006(3) 0.6917(7) 0.031(3) Uani 1 0 . C20 C 0.5657(9) -0.0078(2) 0.8067(7) 0.027(3) Uani 1 0 . C21 C 0.6306(8) 0.0237(2) 0.8834(6) 0.024(2) Uani 1 0 . N22 N 0.5923(7) 0.0607(2) 0.8500(5) 0.026(2) Uani 1 0 . C23 C 0.7423(8) 0.0172(2) 1.0083(6) 0.023(2) Uani 1 0 . C24 C 0.8041(9) -0.0181(3) 1.0541(7) 0.031(3) Uani 1 0 . C25 C 0.9090(10) -0.0210(3) 1.1726(7) 0.032(3) Uani 1 0 . C26 C 0.9456(9) 0.0127(3) 1.2420(7) 0.032(3) Uani 1 0 . C27 C 0.8780(9) 0.0471(3) 1.1913(6) 0.027(3) Uani 1 0 . N28 N 0.7777(7) 0.05017(19) 1.0765(5) 0.023(2) Uani 1 0 . O29 O 0.3356(7) 0.15921(17) 1.0644(4) 0.033(2) Uani 1 0 . C30 C 0.3495(9) 0.1239(2) 1.0977(6) 0.025(2) Uani 1 0 . O31 O 0.4358(6) 0.09855(17) 1.0555(4) 0.0255(17) Uani 1 0 . C32 C 0.2499(10) 0.1109(3) 1.1936(7) 0.037(3) Uani 1 0 . O33 O 0.6826(7) 0.18706(17) 1.1320(4) 0.038(2) Uani 1 0 . C34 C 0.7919(9) 0.1616(2) 1.1830(6) 0.024(3) Uani 1 0 . O35 O 0.8086(6) 0.12806(17) 1.1433(4) 0.0305(19) Uani 1 0 . C36 C 0.9082(9) 0.1743(3) 1.3031(6) 0.029(3) Uani 1 0 . O37 O 0.6753(6) 0.14847(16) 0.9036(4) 0.0256(17) Uani 1 0 . C38 C 0.8624(19) 0.1564(4) 0.8886(10) 0.021(3) Uiso 0.6 0 . C39 C 0.891(2) 0.1992(5) 0.8797(13) 0.041(4) Uiso 0.6 0 . C40 C 0.800(3) 0.1697(7) 0.8876(16) 0.024(4) Uiso 0.4 0 . O41 O 0.803(2) 0.2055(5) 0.8713(13) 0.038(4) Uiso 0.4 0 . C42 C 0.961(3) 0.1453(6) 0.8860(16) 0.027(4) Uiso 0.4 0 . CL43 CL 0.8536(2) 0.41967(6) 1.01623(16) 0.0299(6) Uani 1 0 . O44 O 0.7084(7) 0.40959(18) 0.9164(5) 0.039(2) Uani 1 0 . O45 O 1.0178(7) 0.41262(19) 0.9782(5) 0.043(2) Uani 1 0 . O46 O 0.8465(8) 0.3962(2) 1.1218(5) 0.064(3) Uani 1 0 . O47 O 0.8395(8) 0.4595(2) 1.0461(6) 0.060(3) Uani 1 0 . H1 H 0.668 0.257 1.1409 0.0445 Uiso 1 0 . H2 H 0.6849 0.3234 1.1143 0.0426 Uiso 1 0 . H3 H 0.5419 0.3515 0.9297 0.0431 Uiso 1 0 . H4 H 0.3769 0.3126 0.7735 0.0397 Uiso 1 0 . H5 H 0.2098 0.2731 0.6499 0.0425 Uiso 1 0 . H6 H 0.058 0.2252 0.5147 0.0508 Uiso 1 0 . H7 H 0.1049 0.1594 0.5644 0.0467 Uiso 1 0 . H8 H 0.3446 0.1237 0.848 0.0428 Uiso 1 0 . H9 H 0.198 0.1121 0.7359 0.0428 Uiso 1 0 . H10 H 0.401 0.1094 0.6101 0.0448 Uiso 1 0 . H11 H 0.5487 0.1242 0.7169 0.0448 Uiso 1 0 . H12 H 0.3599 0.0423 0.5759 0.0428 Uiso 1 0 . H13 H 0.4219 -0.0217 0.6377 0.0439 Uiso 1 0 . H14 H 0.5925 -0.0336 0.8339 0.0398 Uiso 1 0 . H15 H 0.7764 -0.0411 1.005 0.0427 Uiso 1 0 . H16 H 0.9533 -0.0455 1.2045 0.0459 Uiso 1 0 . H17 H 1.0175 0.0118 1.3226 0.0448 Uiso 1 0 . H18 H 0.9033 0.0704 1.2391 0.0396 Uiso 1 0 . H19 H 0.1598 0.1296 1.2012 0.0495 Uiso 1 0 . H20 H 0.1904 0.0865 1.1693 0.0495 Uiso 1 0 . H21 H 0.3254 0.1076 1.2712 0.0495 Uiso 1 0 . H22 H 0.9806 0.1526 1.3396 0.0422 Uiso 1 0 . H23 H 0.9851 0.1946 1.2887 0.0422 Uiso 1 0 . H24 H 0.8399 0.1828 1.3599 0.0422 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 CU1 0.0514(15) 0.020(10) 0.0195(11) -0.0072(5) -0.0134(4) 0.0002(4) CU2 0.0249(8) 0.019(9) 0.0177(10) -0.0030(4) -0.0041(3) -0.0017(4) N3 0.025(3) 0.019(10) 0.024(3) -0.001(3) -0.006(2) -0.002(3) C4 0.030(4) 0.033(17) 0.025(4) -0.002(4) -0.012(3) -0.004(3) C5 0.036(4) 0.023(13) 0.029(4) -0.002(4) -0.001(3) -0.007(3) C6 0.034(4) 0.016(9) 0.040(5) 0.001(3) 0.003(3) -0.002(3) C7 0.032(4) 0.020(11) 0.027(4) -0.002(3) 0.001(3) 0.003(3) C8 0.031(4) 0.022(12) 0.019(4) 0.000(3) -0.000(3) 0.000(3) C9 0.029(4) 0.032(17) 0.021(4) -0.004(4) -0.002(3) -0.003(3) C10 0.037(4) 0.021(12) 0.027(4) 0.001(4) 0.000(3) 0.005(3) C11 0.039(5) 0.05(2) 0.019(4) -0.005(4) -0.014(3) -0.002(4) C12 0.045(5) 0.023(13) 0.027(4) -0.006(4) -0.010(3) -0.002(3) C13 0.034(4) 0.031(17) 0.020(4) -0.006(4) -0.005(3) -0.003(3) N14 0.035(4) 0.024(13) 0.021(3) -0.006(3) -0.007(3) -0.001(3) C15 0.036(4) 0.022(12) 0.026(4) -0.010(4) -0.008(3) -0.001(3) C16 0.042(5) 0.029(16) 0.020(4) -0.011(4) -0.009(3) -0.003(3) C17 0.027(4) 0.031(17) 0.024(4) -0.008(3) -0.003(3) 0.002(3) C18 0.030(4) 0.031(17) 0.021(4) -0.007(4) -0.011(3) -0.005(3) C19 0.035(4) 0.023(13) 0.032(4) -0.011(4) 0.003(3) -0.015(4) C20 0.029(4) 0.017(10) 0.035(4) -0.000(3) 0.004(3) -0.006(3) C21 0.017(3) 0.027(15) 0.026(4) -0.009(3) 0.000(3) 0.001(3) N22 0.023(3) 0.030(16) 0.021(3) -0.008(3) -0.005(2) 0.001(3) C23 0.018(3) 0.022(12) 0.029(4) 0.001(3) 0.004(3) -0.000(3) C24 0.027(4) 0.029(16) 0.037(5) -0.001(4) 0.005(3) -0.001(4) C25 0.034(4) 0.020(11) 0.040(5) -0.001(4) 0.003(3) 0.005(4) C26 0.030(4) 0.031(17) 0.031(4) 0.002(4) 0.000(3) -0.000(4) C27 0.025(4) 0.030(16) 0.022(4) -0.006(3) 0.001(3) -0.001(3) N28 0.024(3) 0.017(10) 0.023(3) -0.003(3) -0.002(2) -0.001(3) O29 0.051(4) 0.016(9) 0.029(3) -0.004(3) 0.001(2) -0.001(2) C30 0.026(4) 0.021(12) 0.021(4) -0.010(3) -0.011(3) -0.004(3) O31 0.025(3) 0.026(14) 0.025(3) 0.000(2) 0.005(2) 0.000(2) C32 0.040(5) 0.026(14) 0.044(5) -0.004(4) 0.010(4) -0.006(4) O33 0.062(4) 0.019(10) 0.024(3) 0.003(3) -0.014(2) -0.007(2) C34 0.024(4) 0.029(15) 0.017(4) -0.003(3) 0.001(3) 0.001(3) O35 0.033(3) 0.028(15) 0.023(3) 0.002(3) -0.010(2) -0.005(2) C36 0.031(4) 0.030(16) 0.022(4) -0.004(3) -0.002(3) -0.005(3) O37 0.032(3) 0.025(13) 0.017(3) -0.010(2) -0.001(2) 0.000(2) CL43 0.0304(13) 0.026(13) 0.0275(17) 0.0007(8) -0.0074(7) 0.0038(8) O44 0.035(3) 0.029(15) 0.044(4) -0.006(3) -0.018(2) -0.002(3) O45 0.033(3) 0.05(3) 0.041(4) 0.002(3) 0.001(2) 0.008(3) O46 0.045(4) 0.09(5) 0.055(5) 0.009(4) 0.010(3) 0.045(4) O47 0.063(4) 0.035(18) 0.066(5) 0.008(3) -0.026(3) -0.022(3) 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 CU1 O29 2.092(5) . . no CU1 O33 1.942(5) . . no CU1 O37 2.024(5) . . no CU1 N3 2.043(6) . . no CU1 N14 2.018(5) . . no CU2 O31 2.168(4) . . no CU2 O35 1.995(5) . . no CU2 O37 1.950(5) . . no CU2 N22 2.082(6) . . no CU2 N28 1.989(6) . . no CL43 O44 1.447(5) . . no CL43 O45 1.438(6) . . no CL43 O46 1.428(6) . . no CL43 O47 1.418(7) . . no O29 C30 1.266(9) . . no O31 C30 1.244(9) . . no O33 C34 1.267(9) . . no O35 C34 1.247(9) . . no O37 C38 1.516(14) . . no O37 C40 1.25(2) . . no O41 C38 1.75(2) . . no O41 C39 0.704(17) . . no O41 C40 1.24(3) . . no N3 C4 1.352(9) . . no N3 C8 1.359(8) . . no N14 C9 1.353(11) . . no N14 C13 1.356(10) . . no N22 C17 1.371(8) . . no N22 C21 1.339(10) . . no N28 C23 1.356(9) . . no N28 C27 1.349(8) . . no C4 C5 1.378(11) . . no C4 H1 0.948(7) . . no C5 C6 1.369(10) . . no C5 H2 0.952(7) . . no C6 C7 1.386(10) . . no C6 H3 0.943(8) . . no C7 C8 1.387(11) . . no C7 H4 0.950(7) . . no C8 C9 1.493(10) . . no C9 C10 1.386(10) . . no C10 C11 1.394(11) . . no C10 H5 0.956(8) . . no C11 C12 1.374(13) . . no C11 H6 0.953(7) . . no C12 C13 1.382(10) . . no C12 H7 0.948(8) . . no C13 C15 1.495(12) . . no C15 C16 1.525(11) . . no C15 H8 0.951(7) . . no C15 H9 0.953(7) . . no C16 C17 1.496(12) . . no C16 H10 0.950(7) . . no C16 H11 0.951(7) . . no C17 C18 1.394(11) . . no C18 C19 1.363(12) . . no C18 H12 0.951(6) . . no C19 C20 1.371(10) . . no C19 H13 0.953(8) . . no C20 C21 1.404(10) . . no C20 H14 0.946(8) . . no C21 C23 1.488(9) . . no C23 C24 1.365(11) . . no C24 C25 1.396(10) . . no C24 H15 0.957(8) . . no C25 C26 1.385(12) . . no C25 H16 0.951(9) . . no C26 C27 1.365(11) . . no C26 H17 0.950(7) . . no C27 H18 0.957(8) . . no C30 C32 1.500(11) . . no C32 H19 0.964(8) . . no C32 H20 0.968(9) . . no C32 H21 0.941(8) . . no C34 C36 1.509(9) . . no C36 H22 0.968(8) . . no C36 H23 0.952(8) . . no C36 H24 0.945(7) . . no C38 C39 1.49(2) . . no C38 C40 0.67(2) . . no C38 C42 0.856(19) . . no C39 C40 1.25(3) . . no C39 C42 1.92(3) . . no C40 C42 1.51(3) . . 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 O29 CU1 O33 88.0(2) . . . no O29 CU1 O37 115.5(2) . . . no O29 CU1 N3 114.4(2) . . . no O29 CU1 N14 98.4(2) . . . no O33 CU1 O37 91.5(2) . . . no O33 CU1 N3 88.1(2) . . . no O33 CU1 N14 168.6(3) . . . no O37 CU1 N3 130.1(2) . . . no O37 CU1 N14 94.1(2) . . . no N3 CU1 N14 80.7(2) . . . no O31 CU2 O35 93.13(19) . . . no O31 CU2 O37 103.4(2) . . . no O31 CU2 N22 92.6(2) . . . no O31 CU2 N28 96.1(2) . . . no O35 CU2 O37 87.6(2) . . . no O35 CU2 N22 168.2(2) . . . no O35 CU2 N28 88.2(2) . . . no O37 CU2 N22 101.1(2) . . . no O37 CU2 N28 160.2(2) . . . no N22 CU2 N28 81.0(2) . . . no O44 CL43 O45 109.4(3) . . . no O44 CL43 O46 109.5(4) . . . no O44 CL43 O47 108.9(3) . . . no O45 CL43 O46 109.1(4) . . . no O45 CL43 O47 110.2(4) . . . no O46 CL43 O47 109.7(5) . . . no CU1 O29 C30 121.8(5) . . . no CU2 O31 C30 133.4(5) . . . no CU1 O33 C34 129.6(5) . . . no CU2 O35 C34 132.8(5) . . . no CU1 O37 CU2 107.9(2) . . . no CU1 O37 C38 126.3(7) . . . no CU1 O37 C40 103.2(12) . . . no CU2 O37 C38 106.1(6) . . . no CU2 O37 C40 129.0(11) . . . no C38 O37 C40 25.6(10) . . . no C38 O41 C39 57(2) . . . no C38 O41 C40 17.0(10) . . . no C39 O41 C40 74(2) . . . no CU1 N3 C4 126.3(5) . . . no CU1 N3 C8 114.4(5) . . . no C4 N3 C8 118.5(7) . . . no CU1 N14 C9 114.8(5) . . . no CU1 N14 C13 127.0(6) . . . no C9 N14 C13 118.3(6) . . . no CU2 N22 C17 129.4(6) . . . no CU2 N22 C21 111.9(4) . . . no C17 N22 C21 118.4(6) . . . no CU2 N28 C23 116.1(4) . . . no CU2 N28 C27 125.8(6) . . . no C23 N28 C27 118.0(7) . . . no N3 C4 C5 121.8(7) . . . no N3 C4 H1 119.6(9) . . . no C5 C4 H1 118.5(7) . . . no C4 C5 C6 119.5(7) . . . no C4 C5 H2 120.0(7) . . . no C6 C5 H2 120.5(8) . . . no C5 C6 C7 119.9(7) . . . no C5 C6 H3 120.0(7) . . . no C7 C6 H3 120.1(7) . . . no C6 C7 C8 118.4(7) . . . no C6 C7 H4 120.7(8) . . . no C8 C7 H4 120.9(7) . . . no N3 C8 C7 121.8(6) . . . no N3 C8 C9 113.8(7) . . . no C7 C8 C9 124.3(6) . . . no N14 C9 C8 115.6(6) . . . no N14 C9 C10 123.4(7) . . . no C8 C9 C10 121.1(8) . . . no C9 C10 C11 117.4(8) . . . no C9 C10 H5 121.2(8) . . . no C11 C10 H5 121.4(7) . . . no C10 C11 C12 119.7(7) . . . no C10 C11 H6 119.7(9) . . . no C12 C11 H6 120.6(8) . . . no C11 C12 C13 120.1(7) . . . no C11 C12 H7 120.1(7) . . . no C13 C12 H7 119.7(9) . . . no N14 C13 C12 121.2(8) . . . no N14 C13 C15 118.1(6) . . . no C12 C13 C15 120.7(7) . . . no C13 C15 C16 111.8(7) . . . no C13 C15 H8 109.4(7) . . . no C13 C15 H9 108.9(7) . . . no C16 C15 H8 108.9(7) . . . no C16 C15 H9 108.8(7) . . . no H8 C15 H9 109.1(8) . . . no C15 C16 C17 112.7(6) . . . no C15 C16 H10 108.9(7) . . . no C15 C16 H11 108.7(7) . . . no C17 C16 H10 108.7(7) . . . no C17 C16 H11 108.5(7) . . . no H10 C16 H11 109.3(8) . . . no N22 C17 C16 119.1(7) . . . no N22 C17 C18 120.5(8) . . . no C16 C17 C18 120.4(6) . . . no C17 C18 C19 120.7(6) . . . no C17 C18 H12 119.6(9) . . . no C19 C18 H12 119.7(8) . . . no C18 C19 C20 119.0(7) . . . no C18 C19 H13 120.7(8) . . . no C20 C19 H13 120.4(9) . . . no C19 C20 C21 119.2(8) . . . no C19 C20 H14 120.6(7) . . . no C21 C20 H14 120.2(7) . . . no N22 C21 C20 122.2(6) . . . no N22 C21 C23 116.9(7) . . . no C20 C21 C23 120.9(8) . . . no N28 C23 C21 113.8(7) . . . no N28 C23 C24 121.4(6) . . . no C21 C23 C24 124.8(7) . . . no C23 C24 C25 120.2(8) . . . no C23 C24 H15 120.2(7) . . . no C25 C24 H15 119.7(8) . . . no C24 C25 C26 118.3(8) . . . no C24 C25 H16 120.4(8) . . . no C26 C25 H16 121.3(7) . . . no C25 C26 C27 118.6(7) . . . no C25 C26 H17 120.4(8) . . . no C27 C26 H17 121.0(8) . . . no N28 C27 C26 123.5(7) . . . no N28 C27 H18 117.9(8) . . . no C26 C27 H18 118.6(7) . . . no O29 C30 O31 125.6(7) . . . no O29 C30 C32 117.7(7) . . . no O31 C30 C32 116.7(7) . . . no C30 C32 H19 110.4(8) . . . no C30 C32 H20 110.1(7) . . . no C30 C32 H21 111.5(7) . . . no H19 C32 H20 106.8(7) . . . no H19 C32 H21 109.0(8) . . . no H20 C32 H21 108.8(9) . . . no O33 C34 O35 126.1(6) . . . no O33 C34 C36 114.5(7) . . . no O35 C34 C36 119.4(7) . . . no C34 C36 H22 109.5(7) . . . no C34 C36 H23 110.2(6) . . . no C34 C36 H24 111.1(6) . . . no H22 C36 H23 107.8(7) . . . no H22 C36 H24 108.4(7) . . . no H23 C36 H24 109.8(8) . . . no O37 C38 O41 87.2(10) . . . no O37 C38 C39 110.2(13) . . . no O37 C38 C40 54(2) . . . no O37 C38 C42 143(2) . . . no O41 C38 C39 23.5(7) . . . no O41 C38 C40 33(2) . . . no O41 C38 C42 130(2) . . . no C39 C38 C40 56(2) . . . no C39 C38 C42 107(2) . . . no C40 C38 C42 163(3) . . . no O41 C39 C38 99(2) . . . no O41 C39 C40 73(2) . . . no O41 C39 C42 124(2) . . . no C38 C39 C40 26.2(10) . . . no C38 C39 C42 25.2(7) . . . no C40 C39 C42 51.4(13) . . . no O37 C40 O41 130(2) . . . no O37 C40 C38 100(3) . . . no O37 C40 C39 162(2) . . . no O37 C40 C42 109.8(19) . . . no O41 C40 C38 130(3) . . . no O41 C40 C39 32.8(10) . . . no O41 C40 C42 120.4(18) . . . no C38 C40 C39 98(3) . . . no C38 C40 C42 9.6(19) . . . no C39 C40 C42 88.1(16) . . . no C38 C42 C39 47.9(16) . . . no C38 C42 C40 7.5(15) . . . no C39 C42 C40 40.5(10) . . . 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_MSC98029 _audit_creation_method 'minor manual editing of SDT2CIF v. 1.2 BETA output' _chemical_formula_sum 'C26 H24 B1 Cu2 F5 N4 O4' _chemical_formula_moiety ? _chemical_formula_weight 689.396 _cell_length_a 12.613(3) _cell_length_b 13.380(3) _cell_length_c 9.763(2) _cell_angle_alpha 105.410(10) _cell_angle_beta 110.483(10) _cell_angle_gamma 102.894(12) _cell_volume 1393.8(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 103. _exptl_crystal_colour green _exptl_crystal_description multifaceted _exptl_crystal_size_max .30 _exptl_crystal_size_mid .30 _exptl_crystal_size_min .20 _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 1.6 _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 20. _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6407 _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_theta_min 3.00584 _diffrn_reflns_theta_max 25.0328 _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_standards_number 4 _diffrn_standards_decay_% 5.1 _diffrn_standards_interval_count 500 _reflns_number_total 4906 _reflns_number_gt 3183 _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 CU Cu 0.263 1.266 'International Tables Vol. IV (1974) Table 2.2B' F F 0.014 0.01 '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' B B 0 0.001 '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 3542 _refine_ls_number_parameters 503 _refine_ls_hydrogen_treatment ? _refine_ls_extinction_coef -0.00000016(19) _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)+(.03F)^2^ _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.05 _refine_ls_goodness_of_fit_ref 1.9453 _refine_ls_shift/su_max 0.215 _refine_diff_density_max 0.77 _refine_diff_density_min -1.02 _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 CU1 CU 0.77938(7) 0.21619(7) 0.26547(9) 0.0309(4) Uani 1 0 . CU2 CU 0.61092(9) 0.03364(7) -0.09016(10) 0.0524(5) Uani 1 0 . F3 F 0.6196(3) 0.1246(3) 0.1066(4) 0.0310(17) Uani 1 0 . O4 O 0.7538(4) 0.1362(4) -0.1170(5) 0.042(2) Uani 1 0 . C5 C 0.8502(6) 0.2120(5) -0.0146(8) 0.030(3) Uani 1 0 . O6 O 0.8790(3) 0.2489(3) 0.1310(5) 0.031(2) Uani 1 0 . C7 C 0.9321(10) 0.2677(10) -0.0733(14) 0.059(6) Uani 1 0 . O8 O 0.7138(5) -0.0354(4) 0.0231(5) 0.063(3) Uani 1 0 . C9 C 0.7878(6) -0.0061(6) 0.1628(8) 0.037(3) Uani 1 0 . O10 O 0.8152(4) 0.0832(4) 0.2719(5) 0.033(2) Uani 1 0 . C11 C 0.8526(14) -0.0813(9) 0.2067(12) 0.064(6) Uani 1 0 . N12 N 0.9127(4) 0.3003(4) 0.4828(6) 0.028(3) Uani 1 0 . C13 C 0.9988(6) 0.2659(6) 0.5580(8) 0.031(3) Uani 1 0 . C14 C 1.0886(6) 0.3304(6) 0.7080(8) 0.040(4) Uani 1 0 . C15 C 1.0902(7) 0.4344(6) 0.7802(9) 0.045(4) Uani 1 0 . C16 C 1.0024(7) 0.4707(6) 0.7035(8) 0.037(4) Uani 1 0 . C17 C 0.9130(5) 0.4009(5) 0.5526(7) 0.028(3) Uani 1 0 . C18 C 0.8159(5) 0.4333(5) 0.4614(7) 0.027(3) Uani 1 0 . C19 C 0.7988(7) 0.5312(6) 0.5208(9) 0.036(4) Uani 1 0 . C20 C 0.7076(6) 0.5547(6) 0.4264(9) 0.044(4) Uani 1 0 . C21 C 0.6387(7) 0.4845(6) 0.2746(11) 0.068(4) Uani 1 0 . C22 C 0.6582(7) 0.3873(7) 0.2195(10) 0.077(4) Uani 1 0 . N23 N 0.7445(5) 0.3599(5) 0.3119(6) 0.043(3) Uani 1 0 . C24 C 0.5484(13) 0.2954(12) 0.0779(17) 0.027(7) Uani 0.5 0 . C25 C 0.6028(15) 0.2791(13) -0.0438(19) 0.026(8) Uani 0.5 0 . N26 N 0.4861(6) 0.0814(5) -0.2285(6) 0.062(3) Uani 1 0 . C27 C 0.5076(12) 0.1884(10) -0.1991(14) 0.023(6) Uani 0.5 0 . C28 C 0.4164(13) 0.2106(11) -0.3044(16) 0.024(7) Uani 0.5 0 . C29 C 0.3125(7) 0.1229(6) -0.4564(8) 0.043(4) Uani 1 0 . C30 C 0.3314(6) 0.0245(5) -0.4883(8) 0.029(3) Uani 1 0 . C31 C 0.4163(5) 0.0046(5) -0.3762(7) 0.024(3) Uani 1 0 . C32 C 0.4399(5) -0.1003(5) -0.4027(7) 0.024(3) Uani 1 0 . C33 C 0.3731(7) -0.1920(6) -0.5413(8) 0.047(4) Uani 1 0 . C34 C 0.3983(8) -0.2871(8) -0.5557(9) 0.067(5) Uani 1 0 . C35 C 0.4927(7) -0.2889(7) -0.4341(8) 0.047(4) Uani 1 0 . C36 C 0.5580(6) -0.1959(6) -0.2987(8) 0.031(3) Uani 1 0 . N37 N 0.5324(4) -0.1027(4) -0.2847(5) 0.024(2) Uani 1 0 . B38 B 0.3054(7) 0.4305(6) 0.1530(8) 0.028(3) Uani 1 0 . F39 F 0.2170(3) 0.4753(3) 0.1479(4) 0.047(2) Uani 1 0 . F40 F 0.2604(5) 0.3212(4) 0.1044(9) 0.134(4) Uani 1 0 . F41 F 0.3949(5) 0.4674(5) 0.2969(5) 0.109(3) Uani 1 0 . F42 F 0.3491(4) 0.4508(5) 0.0515(6) 0.102(4) Uani 1 0 . O43 N 0.0796(7) 0.1735(6) 0.2838(10) 0.065(4) Uiso 0.90(2) 0 . O44 N 0.0994(9) 0.1281(9) 0.1673(13) 0.123(6) Uiso 0.99(3) 0 . C45 C 0.1344(15) 0.0521(16) 0.208(2) 0.060(8) Uiso 0.48(3) 0 . C24A C 0.6130(15) 0.3227(12) 0.0273(18) 0.023(8) Uani 0.5 0 . C25A C 0.4852(13) 0.2501(11) -0.0227(16) 0.028(7) Uani 0.5 0 . C27A C 0.4321(12) 0.1698(10) -0.1908(13) 0.020(6) Uani 0.5 0 . C28A C 0.3478(13) 0.1889(12) -0.3083(17) 0.027(7) Uani 0.5 0 . H1 H 0.999(5) 0.286(5) -0.014(7) 0.02(2) Uiso 1 0 . H2 H 0.941(7) 0.207(7) -0.161(9) 0.09(3) Uiso 1 0 . H3 H 0.904(6) 0.329(6) -0.102(8) 0.07(3) Uiso 1 0 . H4 H 0.869(8) -0.079(7) 0.318(10) 0.10(3) Uiso 1 0 . H5 H 0.817(7) -0.148(7) 0.150(9) 0.06(3) Uiso 1 0 . H6 H 0.910(8) -0.060(9) 0.220(13) 0.10(5) Uiso 1 0 . H7 H 0.996(5) 0.193(5) 0.502(6) 0.027(17) Uiso 1 0 . H8 H 1.150(5) 0.300(5) 0.747(6) 0.026(16) Uiso 1 0 . H9 H 1.151(6) 0.485(6) 0.883(8) 0.06(2) Uiso 1 0 . H10 H 0.994(5) 0.533(5) 0.742(7) 0.03(2) Uiso 1 0 . H11 H 0.848(5) 0.574(5) 0.616(7) 0.024(17) Uiso 1 0 . H12 H 0.687(5) 0.616(5) 0.468(7) 0.034(18) Uiso 1 0 . H13 H 0.575(6) 0.498(5) 0.215(7) 0.05(2) Uiso 1 0 . H14 H 0.5253 0.229 0.0939 0.0377 Uiso 0.5 0 . H15 H 0.4816 0.3174 0.0393 0.0377 Uiso 0.5 0 . H16 H 0.6316 0.3441 -0.0637 0.0411 Uiso 0.5 0 . H17 H 0.6728 0.2538 -0.0118 0.0411 Uiso 0.5 0 . H18 H 0.4259 0.2894 -0.2807 0.0431 Uiso 0.5 0 . H19 H 0.242 0.134 -0.5214 0.0632 Uiso 0.5 0 . H20 H 0.299(4) -0.025(4) -0.579(6) 0.005(14) Uiso 1 0 . H21 H 0.314(6) -0.184(5) -0.613(7) 0.05(2) Uiso 1 0 . H22 H 0.361(7) -0.348(7) -0.649(9) 0.08(3) Uiso 1 0 . H23 H 0.518(5) -0.346(5) -0.429(7) 0.037(19) Uiso 1 0 . H24 H 0.629(5) -0.196(5) -0.218(7) 0.037(18) Uiso 1 0 . H14A H 0.6146 0.3743 -0.0322 0.0328 Uiso 0.5 0 . H15A H 0.6601 0.28 -0.003 0.0328 Uiso 0.5 0 . H16A H 0.4866 0.2131 0.0491 0.0359 Uiso 0.5 0 . H17A H 0.4372 0.2979 -0.0088 0.0359 Uiso 0.5 0 . H18A H 0.3224 0.2522 -0.281 0.0388 Uiso 0.5 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 CU1 0.0313(19) 0.034(2) 0.0198(8) 0.0159(4) 0.0068(4) 0.0027(4) CU2 0.071(4) 0.0197(15) 0.0257(10) 0.0022(5) -0.0126(5) 0.0054(4) F3 0.021(2) 0.046(4) 0.027(2) 0.0064(17) 0.0108(16) 0.0193(18) O4 0.062(5) 0.027(3) 0.028(3) 0.004(3) 0.018(2) 0.007(2) C5 0.034(5) 0.031(4) 0.043(5) 0.017(3) 0.027(4) 0.020(4) O6 0.026(3) 0.031(3) 0.029(3) -0.002(2) 0.015(2) 0.006(2) C7 0.051(7) 0.084(10) 0.078(8) 0.024(6) 0.049(6) 0.052(6) O8 0.082(6) 0.021(3) 0.036(3) 0.009(3) -0.019(3) 0.003(2) C9 0.035(5) 0.026(4) 0.031(4) -0.004(3) 0.001(3) 0.013(3) O10 0.028(3) 0.037(4) 0.027(3) 0.008(2) 0.007(2) 0.010(2) C11 0.082(11) 0.027(6) 0.041(6) 0.008(6) -0.011(6) 0.010(4) N12 0.030(4) 0.036(4) 0.020(3) 0.011(3) 0.015(3) 0.010(3) C13 0.027(4) 0.042(5) 0.030(4) 0.012(3) 0.016(3) 0.017(4) C14 0.032(5) 0.049(6) 0.038(5) 0.005(4) 0.007(3) 0.030(4) C15 0.044(6) 0.039(6) 0.032(5) -0.008(4) 0.001(4) 0.019(4) C16 0.048(6) 0.032(5) 0.024(4) 0.005(4) 0.010(3) 0.015(4) C17 0.031(4) 0.035(5) 0.018(3) 0.006(3) 0.016(3) 0.009(3) C18 0.026(4) 0.030(4) 0.024(4) 0.006(3) 0.016(3) 0.005(3) C19 0.037(5) 0.028(5) 0.033(4) 0.003(4) 0.016(4) 0.003(4) C20 0.033(5) 0.026(4) 0.066(6) 0.012(4) 0.025(4) 0.004(4) C21 0.029(5) 0.031(5) 0.084(7) 0.011(4) -0.014(4) -0.012(4) C22 0.062(7) 0.042(6) 0.060(6) 0.035(5) -0.027(4) -0.015(4) N23 0.037(4) 0.038(5) 0.029(3) 0.021(3) -0.000(3) -0.005(3) C24 0.017(8) 0.031(9) 0.043(9) 0.017(7) 0.018(8) 0.014(8) C25 0.034(9) 0.022(10) 0.039(11) 0.015(8) 0.026(9) 0.015(8) N26 0.109(9) 0.021(4) 0.023(3) 0.015(4) -0.002(3) 0.007(3) C27 0.025(8) 0.019(7) 0.029(7) 0.005(6) 0.017(7) 0.010(6) C28 0.033(9) 0.022(8) 0.042(9) 0.019(7) 0.032(8) 0.021(6) C29 0.072(7) 0.043(5) 0.031(4) 0.027(4) 0.032(4) 0.019(4) C30 0.032(4) 0.028(4) 0.021(4) 0.003(3) 0.013(3) 0.004(3) C31 0.031(4) 0.023(4) 0.018(3) 0.002(3) 0.014(3) 0.009(3) C32 0.019(3) 0.032(4) 0.019(3) 0.006(3) 0.011(3) 0.007(3) C33 0.048(6) 0.045(6) 0.033(4) 0.029(4) 0.003(4) 0.005(4) C34 0.090(9) 0.062(7) 0.024(4) 0.049(5) 0.002(4) -0.005(4) C35 0.071(7) 0.050(6) 0.029(4) 0.042(5) 0.023(4) 0.010(4) C36 0.029(4) 0.043(5) 0.025(4) 0.016(3) 0.014(3) 0.012(3) N37 0.025(3) 0.031(4) 0.019(3) 0.004(2) 0.015(2) 0.010(2) B38 0.039(5) 0.028(5) 0.015(4) 0.013(4) 0.009(3) 0.006(3) F39 0.047(4) 0.069(6) 0.026(2) 0.040(2) 0.0132(18) 0.010(2) F40 0.072(6) 0.036(4) 0.243(12) 0.018(3) 0.022(4) 0.037(4) F41 0.109(8) 0.154(12) 0.030(3) 0.109(4) -0.006(3) -0.009(3) F42 0.080(6) 0.212(16) 0.129(7) 0.104(4) 0.077(4) 0.141(5) C24A 0.037(9) 0.021(9) 0.024(9) 0.018(8) 0.024(8) 0.007(7) C25A 0.029(8) 0.030(8) 0.024(8) 0.006(7) 0.010(7) 0.012(7) C27A 0.018(7) 0.021(7) 0.015(6) -0.001(6) 0.004(6) 0.007(5) C28A 0.026(9) 0.040(9) 0.036(9) 0.017(8) 0.027(8) 0.025(7) 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 CU1 F3 1.916(3) . . no CU1 O6 2.171(4) . . no CU1 O10 1.943(4) . . no CU1 N12 1.996(5) . . no CU1 N23 2.038(5) . . no CU2 F3 1.933(3) . . no CU2 O4 2.149(5) . . no CU2 O8 1.959(5) . . no CU2 N26 2.032(6) . . no CU2 N37 1.988(5) . . no F39 B38 1.372(8) . . no F40 B38 1.326(8) . . no F41 B38 1.328(8) . . no F42 B38 1.348(8) . . no O4 C5 1.251(7) . . no O6 C5 1.257(7) . . no O8 C9 1.244(7) . . no O10 C9 1.250(7) . . no N12 C13 1.333(8) . . no N12 C17 1.335(7) . . no N23 C18 1.352(7) . . no N23 C22 1.342(8) . . no N26 C27 1.326(13) . . no N26 C31 1.353(7) . . no N26 C27A 1.517(14) . . no N37 C32 1.337(7) . . no N37 C36 1.340(8) . . no O43 O44 1.275(11) . . no O43 C45 1.97(2) . . no O44 C45 1.297(18) . . no C5 C7 1.500(10) . . no C7 H1 0.77(6) . . no C7 H2 1.06(8) . . no C7 H3 1.03(7) . . no C9 C11 1.488(12) . . no C11 H4 1.02(8) . . no C11 H5 0.83(8) . . no C11 H6 0.66(10) . . no C13 C14 1.380(9) . . no C13 H7 0.97(5) . . no C14 C15 1.375(10) . . no C14 H8 0.96(5) . . no C15 C16 1.369(10) . . no C15 H9 0.96(7) . . no C16 C17 1.397(9) . . no C16 H10 0.87(6) . . no C17 C18 1.470(8) . . no C18 C19 1.381(9) . . no C19 C20 1.359(10) . . no C19 H11 0.86(5) . . no C20 C21 1.352(10) . . no C20 H12 0.94(6) . . no C21 C22 1.379(10) . . no C21 H13 0.89(6) . . no C22 C24 1.529(16) . . no C22 C24A 1.662(16) . . no C24 C25 1.559(19) . . no C24 C24A 1.134(19) . . no C24 C25A 0.943(15) . . no C24 H14 0.942(14) . . no C24 H15 0.942(12) . . no C24 H16A 1.094(15) . . no C24 H17A 1.375(13) . . no C25 C27 1.521(19) . . no C25 C24A 0.726(14) . . no C25 C25A 1.55(2) . . no C25 H16 0.962(15) . . no C25 H17 0.993(16) . . no C25 H14A 1.219(15) . . no C25 H15A 0.688(16) . . no C27 C28 1.398(18) . . no C27 C25A 1.848(18) . . no C27 C27A 0.966(14) . . no C27 C28A 1.925(18) . . no C28 C29 1.525(16) . . no C28 C27A 1.335(17) . . no C28 C28A 0.833(14) . . no C28 H18 0.988(13) . . no C28 H18A 1.478(13) . . no C29 C30 1.366(9) . . no C29 C28A 1.328(15) . . no C29 H19 0.963(7) . . no C30 C31 1.370(8) . . no C30 H20 0.84(5) . . no C31 C32 1.473(8) . . no C32 C33 1.380(9) . . no C33 C34 1.362(10) . . no C33 H21 0.87(6) . . no C34 C35 1.367(10) . . no C34 H22 0.92(8) . . no C35 C36 1.371(9) . . no C35 H23 0.90(6) . . no C36 H24 0.96(6) . . no C24A C25A 1.51(2) . . no C24A H16 1.085(16) . . no C24A H17 1.374(15) . . no C24A H14A 1.016(16) . . no C24A H15A 0.976(15) . . no C25A C27A 1.506(17) . . no C25A H14 1.209(13) . . no C25A H15 0.963(14) . . no C25A H16A 0.957(13) . . no C25A H17A 0.989(13) . . no C27A C28A 1.392(18) . . no C28A H18 1.372(15) . . no C28A H18A 0.976(14) . . no H14 H16A 0.47879(12) . . no H15 H17A 0.53643(13) . . no H16 H14A 0.56765(9) . . no H17 H15A 0.41655(7) . . 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 F3 CU1 O6 103.69(14) . . . no F3 CU1 O10 88.91(16) . . . no F3 CU1 N12 157.34(16) . . . no F3 CU1 N23 95.98(18) . . . no O6 CU1 O10 93.88(17) . . . no O6 CU1 N12 98.97(17) . . . no O6 CU1 N23 97.6(2) . . . no O10 CU1 N12 89.19(19) . . . no O10 CU1 N23 166.1(2) . . . no N12 CU1 N23 81.3(2) . . . no F3 CU2 O4 103.59(15) . . . no F3 CU2 O8 89.86(18) . . . no F3 CU2 N26 95.2(2) . . . no F3 CU2 N37 151.63(17) . . . no O4 CU2 O8 94.0(2) . . . no O4 CU2 N26 91.8(2) . . . no O4 CU2 N37 104.65(17) . . . no O8 CU2 N26 171.3(2) . . . no O8 CU2 N37 90.9(2) . . . no N26 CU2 N37 81.3(2) . . . no CU1 F3 CU2 115.12(16) . . . no CU2 O4 C5 130.0(4) . . . no CU1 O6 C5 131.8(4) . . . no CU2 O8 C9 133.4(5) . . . no CU1 O10 C9 130.6(4) . . . no CU1 N12 C13 126.0(5) . . . no CU1 N12 C17 114.3(4) . . . no C13 N12 C17 119.7(6) . . . no CU1 N23 C18 113.1(4) . . . no CU1 N23 C22 129.2(5) . . . no C18 N23 C22 117.5(6) . . . no CU2 N26 C27 119.2(7) . . . no CU2 N26 C31 113.7(4) . . . no CU2 N26 C27A 132.6(5) . . . no C27 N26 C31 121.2(7) . . . no C27 N26 C27A 39.0(6) . . . no C31 N26 C27A 111.4(7) . . . no CU2 N37 C32 114.4(4) . . . no CU2 N37 C36 125.4(4) . . . no C32 N37 C36 119.9(5) . . . no O44 O43 C45 40.4(7) . . . no O43 O44 C45 100.0(12) . . . no O4 C5 O6 125.0(6) . . . no O4 C5 C7 116.6(7) . . . no O6 C5 C7 118.2(7) . . . no C5 C7 H1 111(5) . . . no C5 C7 H2 110(5) . . . no C5 C7 H3 109(4) . . . no H1 C7 H2 93(6) . . . no H1 C7 H3 115(7) . . . no H2 C7 H3 118(6) . . . no O8 C9 O10 125.7(7) . . . no O8 C9 C11 118.4(7) . . . no O10 C9 C11 115.9(6) . . . no C9 C11 H4 113(5) . . . no C9 C11 H5 115(5) . . . no C9 C11 H6 109(10) . . . no H4 C11 H5 105(7) . . . no H4 C11 H6 97(10) . . . no H5 C11 H6 117(11) . . . no N12 C13 C14 122.1(7) . . . no N12 C13 H7 117(3) . . . no C14 C13 H7 121(3) . . . no C13 C14 C15 118.6(7) . . . no C13 C14 H8 115(3) . . . no C15 C14 H8 126(3) . . . no C14 C15 C16 119.7(7) . . . no C14 C15 H9 124(4) . . . no C16 C15 H9 117(4) . . . no C15 C16 C17 119.0(7) . . . no C15 C16 H10 126(4) . . . no C17 C16 H10 115(4) . . . no N12 C17 C16 120.9(6) . . . no N12 C17 C18 116.4(5) . . . no C16 C17 C18 122.7(6) . . . no N23 C18 C17 114.5(5) . . . no N23 C18 C19 122.0(6) . . . no C17 C18 C19 123.4(6) . . . no C18 C19 C20 119.1(7) . . . no C18 C19 H11 117(4) . . . no C20 C19 H11 124(4) . . . no C19 C20 C21 119.6(7) . . . no C19 C20 H12 121(4) . . . no C21 C20 H12 120(4) . . . no C20 C21 C22 119.6(8) . . . no C20 C21 H13 119(4) . . . no C22 C21 H13 121(4) . . . no N23 C22 C21 122.0(7) . . . no N23 C22 C24 119.0(8) . . . no N23 C22 C24A 114.2(8) . . . no C21 C22 C24 114.5(7) . . . no C21 C22 C24A 120.3(9) . . . no C24 C22 C24A 41.4(8) . . . no C22 C24 C25 98.9(11) . . . no C22 C24 C24A 75.6(12) . . . no C22 C24 C25A 165.7(18) . . . no C22 C24 H14 114.0(12) . . . no C22 C24 H15 113.7(12) . . . no C22 C24 H16A 138.8(13) . . . no C22 C24 H17A 129.7(9) . . . no C25 C24 C24A 25.6(9) . . . no C25 C24 C25A 71.7(14) . . . no C25 C24 H14 109.9(11) . . . no C25 C24 H15 108.6(13) . . . no C25 C24 H16A 105.3(11) . . . no C25 C24 H17A 102.3(11) . . . no C24A C24 C25A 92.8(17) . . . no C24A C24 H14 129.5(14) . . . no C24A C24 H15 108.6(15) . . . no C24A C24 H16A 130.5(14) . . . no C24A C24 H17A 109.4(14) . . . no C25A C24 H14 79.8(15) . . . no C25A C24 H15 61.5(12) . . . no C25A C24 H16A 55.5(12) . . . no C25A C24 H17A 46.0(10) . . . no H14 C24 H15 110.9(15) . . . no H14 C24 H16A 25.8(4) . . . no H14 C24 H17A 100.7(12) . . . no H15 C24 H16A 89.5(12) . . . no H15 C24 H17A 16.0(4) . . . no H16A C24 H17A 76.9(9) . . . no C24 C25 C27 108.8(12) . . . no C24 C25 C24A 42(2) . . . no C24 C25 C25A 35.3(6) . . . no C24 C25 H16 115.1(14) . . . no C24 C25 H17 113.0(14) . . . no C24 C25 H14A 88.4(11) . . . no C24 C25 H15A 105.4(17) . . . no C27 C25 C24A 145(3) . . . no C27 C25 C25A 74.1(10) . . . no C27 C25 H16 108.6(14) . . . no C27 C25 H17 105.8(13) . . . no C27 C25 H14A 116.9(13) . . . no C27 C25 H15A 125.2(17) . . . no C24A C25 C25A 73(2) . . . no C24A C25 H16 79(2) . . . no C24A C25 H17 105(3) . . . no C24A C25 H14A 56.3(19) . . . no C24A C25 H15A 87(3) . . . no C25A C25 H16 122.2(14) . . . no C25A C25 H17 130.6(14) . . . no C25A C25 H14A 98.2(11) . . . no C25A C25 H15A 133.5(19) . . . no H16 C25 H17 105.0(15) . . . no H16 C25 H14A 27.0(4) . . . no H16 C25 H15A 93.4(17) . . . no H17 C25 H14A 122.5(15) . . . no H17 C25 H15A 19.8(5) . . . no H14A C25 H15A 105.5(17) . . . no N26 C27 C25 123.3(11) . . . no N26 C27 C28 113.8(11) . . . no N26 C27 C25A 108.7(9) . . . no N26 C27 C27A 81.2(12) . . . no N26 C27 C28A 101.5(9) . . . no C25 C27 C28 121.0(12) . . . no C25 C27 C25A 53.6(8) . . . no C25 C27 C27A 107.9(14) . . . no C25 C27 C28A 123.8(10) . . . no C28 C27 C25A 96.4(10) . . . no C28 C27 C27A 65.9(12) . . . no C28 C27 C28A 22.7(7) . . . no C25A C27 C27A 54.3(10) . . . no C25A C27 C28A 82.7(8) . . . no C27A C27 C28A 43.4(10) . . . no C27 C28 C29 124.2(11) . . . no C27 C28 C27A 41.3(7) . . . no C27 C28 C28A 117.0(19) . . . no C27 C28 H18 116.1(14) . . . no C27 C28 H18A 129.5(11) . . . no C29 C28 C27A 108.1(11) . . . no C29 C28 C28A 60.4(15) . . . no C29 C28 H18 119.5(12) . . . no C29 C28 H18A 85.0(8) . . . no C27A C28 C28A 76.0(16) . . . no C27A C28 H18 120.4(13) . . . no C27A C28 H18A 94.1(10) . . . no C28A C28 H18 97.4(17) . . . no C28A C28 H18A 38.5(12) . . . no H18 C28 H18A 59.0(6) . . . no C28 C29 C30 110.7(7) . . . no C28 C29 C28A 33.0(6) . . . no C28 C29 H19 125.4(8) . . . no C30 C29 C28A 120.3(8) . . . no C30 C29 H19 123.9(7) . . . no C28A C29 H19 107.3(8) . . . no C29 C30 C31 121.7(6) . . . no C29 C30 H20 123(3) . . . no C31 C30 H20 115(3) . . . no N26 C31 C30 121.9(6) . . . no N26 C31 C32 113.9(5) . . . no C30 C31 C32 124.2(6) . . . no N37 C32 C31 116.4(5) . . . no N37 C32 C33 120.4(6) . . . no C31 C32 C33 123.2(6) . . . no C32 C33 C34 119.9(7) . . . no C32 C33 H21 115(5) . . . no C34 C33 H21 125(5) . . . no C33 C34 C35 119.2(8) . . . no C33 C34 H22 123(5) . . . no C35 C34 H22 117(5) . . . no C34 C35 C36 119.3(7) . . . no C34 C35 H23 128(4) . . . no C36 C35 H23 113(4) . . . no N37 C36 C35 121.2(6) . . . no N37 C36 H24 120(4) . . . no C35 C36 H24 119(4) . . . no O43 C45 O44 39.6(8) . . . no C22 C24A C24 63.0(11) . . . no C22 C24A C25 157(3) . . . no C22 C24A C25A 101.2(11) . . . no C22 C24A H16 135.3(13) . . . no C22 C24A H17 115.5(11) . . . no C22 C24A H14A 113.8(12) . . . no C22 C24A H15A 116.8(13) . . . no C24 C24A C25 112(3) . . . no C24 C24A C25A 38.6(9) . . . no C24 C24A H16 151.5(18) . . . no C24 C24A H17 117.8(14) . . . no C24 C24A H14A 130.3(16) . . . no C24 C24A H15A 123.9(16) . . . no C25 C24A C25A 79(2) . . . no C25 C24A H16 60.3(19) . . . no C25 C24A H17 44.3(18) . . . no C25 C24A H14A 87(2) . . . no C25 C24A H15A 44.8(17) . . . no C25A C24A H16 116.2(13) . . . no C25A C24A H17 107.0(11) . . . no C25A C24A H14A 111.1(14) . . . no C25A C24A H15A 112.0(13) . . . no H16 C24A H17 77.3(9) . . . no H16 C24A H14A 31.1(5) . . . no H16 C24A H15A 72.1(10) . . . no H17 C24A H14A 107.9(12) . . . no H17 C24A H15A 6.1(3) . . . no H14A C24A H15A 102.3(14) . . . no C24 C25A C25 73.0(13) . . . no C24 C25A C27 124.3(15) . . . no C24 C25A C24A 48.6(12) . . . no C24 C25A C27A 154.6(17) . . . no C24 C25A H14 50.1(12) . . . no C24 C25A H15 59.2(12) . . . no C24 C25A H16A 70.3(14) . . . no C24 C25A H17A 90.7(15) . . . no C25 C25A C27 52.3(8) . . . no C25 C25A C24A 27.4(6) . . . no C25 C25A C27A 83.7(10) . . . no C25 C25A H14 97.0(11) . . . no C25 C25A H15 108.2(13) . . . no C25 C25A H16A 114.3(13) . . . no C25 C25A H17A 127.4(13) . . . no C27 C25A C24A 79.2(9) . . . no C27 C25A C27A 31.4(6) . . . no C27 C25A H14 121.3(10) . . . no C27 C25A H15 142.2(12) . . . no C27 C25A H16A 120.2(11) . . . no C27 C25A H17A 128.6(11) . . . no C24A C25A C27A 110.3(11) . . . no C24A C25A H14 86.7(11) . . . no C24A C25A H15 83.0(11) . . . no C24A C25A H16A 108.1(13) . . . no C24A C25A H17A 108.6(13) . . . no C27A C25A H14 125.8(11) . . . no C27A C25A H15 140.9(13) . . . no C27A C25A H16A 112.1(12) . . . no C27A C25A H17A 111.8(12) . . . no H14 C25A H15 90.4(10) . . . no H14 C25A H16A 21.8(3) . . . no H14 C25A H17A 110.0(11) . . . no H15 C25A H16A 96.9(12) . . . no H15 C25A H17A 31.9(4) . . . no H16A C25A H17A 105.7(12) . . . no N26 C27A C27 59.8(10) . . . no N26 C27A C28 106.1(10) . . . no N26 C27A C25A 118.5(9) . . . no N26 C27A C28A 122.1(10) . . . no C27 C27A C28 72.8(13) . . . no C27 C27A C25A 94.2(13) . . . no C27 C27A C28A 108.1(14) . . . no C28 C27A C25A 118.1(11) . . . no C28 C27A C28A 35.5(7) . . . no C25A C27A C28A 118.7(12) . . . no C27 C28A C28 40.3(14) . . . no C27 C28A C29 103.6(9) . . . no C27 C28A C27A 28.5(6) . . . no C27 C28A H18 74.1(7) . . . no C27 C28A H18A 124.2(12) . . . no C28 C28A C29 86.5(16) . . . no C28 C28A C27A 68.5(15) . . . no C28 C28A H18 45.6(13) . . . no C28 C28A H18A 109.4(19) . . . no C29 C28A C27A 116.8(12) . . . no C29 C28A H18 108.2(10) . . . no C29 C28A H18A 122.8(13) . . . no C27A C28A H18 94.1(10) . . . no C27A C28A H18A 120.1(13) . . . no H18 C28A H18A 63.9(8) . . . no F39 B38 F40 110.8(6) . . . no F39 B38 F41 112.9(5) . . . no F39 B38 F42 109.7(6) . . . no F40 B38 F41 107.4(6) . . . no F40 B38 F42 105.7(7) . . . no F41 B38 F42 110.1(7) . . . no C24 H14 C25A 50.1(9) . . . no C24 H14 H16A 95.2(9) . . . no C25A H14 H16A 48.0(7) . . . no C24 H15 C25A 59.3(9) . . . no C24 H15 H17A 135.1(9) . . . no C25A H15 H17A 76.7(8) . . . no C25 H16 C24A 41.0(9) . . . no C25 H16 H14A 102.6(9) . . . no C24A H16 H14A 67.7(8) . . . no C25 H17 C24A 30.7(10) . . . no C25 H17 H15A 34.0(9) . . . no C24A H17 H15A 14.4(7) . . . no C28 H18 C28A 37.0(8) . . . no C25 H14A C24A 36.5(8) . . . no C25 H14A H16 50.3(7) . . . no C24A H14A H16 81.2(8) . . . no C25 H15A C24A 48.0(13) . . . no C25 H15A H17 126.3(13) . . . no C24A H15A H17 159.5(10) . . . no C24 H16A C25A 54.2(9) . . . no C24 H16A H14 59.0(7) . . . no C25A H16A H14 110.2(9) . . . no C24 H17A C25A 43.3(8) . . . no C24 H17A H15 28.9(6) . . . no C25A H17A H15 71.4(8) . . . no C28 H18A C28A 32.1(9) . . . 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