Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Paul Plieger' 'Andrew Parkin' 'Simon Parsons' 'Peter A. Tasker' _publ_contact_author_name 'Dr Paul Plieger' _publ_contact_author_address ; Department of Chemistry University of Edinburgh West Mains Road Edinburgh EH9 3JJ UNITED KINGDOM ; _publ_contact_author_email 'PAT04@HOLYROOD.ED.AC.UK' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Transport of metal salts; encapsulation of anions in dinuclear Cu(II) complexes [Cu2L2SO4]SO4 and [Cu2L2BF4](BF4)3, where L = Bis-(4-tert-butyl-2-[{6-(methyl-amino)-hexyl}-methyl-amino)-methyl]-6-phenyl iminomethyl-phenol) ; data_cupp28 _database_code_CSD 191879 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Cu2(C44H60N4O2)2(SO4)](SO4)' _chemical_formula_sum 'C88 H116 Cu2 N8 O12 S2' _chemical_formula_weight 1669.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.980(3) _cell_length_b 25.614(5) _cell_length_c 48.948(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 21289(7) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8105 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 26 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 1.05 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.41 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.042 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7088 _exptl_absorpt_coefficient_mu 0.491 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_correction_T_min 0.426 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details Sadabs _exptl_special_details ; Data completeness statistics (XPREP before Squeeze): INTENSITY STATISTICS FOR DATASET # 1 cupp28.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.25 1072 1186 90.4 5.20 106.8 58.16 0.0392 0.0087 2.25 - 1.80 1042 1042 100.0 6.64 35.0 35.92 0.0530 0.0183 1.80 - 1.55 1190 1191 99.9 6.04 18.8 22.18 0.0695 0.0333 1.55 - 1.40 1156 1158 99.8 5.44 13.9 16.03 0.0862 0.0486 1.40 - 1.30 1098 1098 100.0 5.09 9.2 10.95 0.1103 0.0758 1.30 - 1.20 1478 1478 100.0 4.75 6.7 7.72 0.1320 0.1122 1.20 - 1.10 2064 2064 100.0 4.41 4.6 5.19 0.1713 0.1716 1.10 - 1.05 1346 1346 100.0 4.10 3.1 3.44 0.2341 0.2655 1.05 - 1.00 1589 1591 99.9 3.92 2.5 2.70 0.2991 0.3404 1.00 - 0.95 1948 1959 99.4 3.73 1.7 1.97 0.3878 0.4839 0.95 - 0.90 2391 2418 98.9 3.50 1.2 1.31 0.5779 0.7313 0.90 - 0.85 2849 3000 95.0 2.92 0.8 0.86 0.9107 1.1634 0.85 - 0.82 874 2045 42.7 0.62 1.0 0.96 0.7879 1.1525 #----------------------------------------------------------------------------- 0.95 - 0.82 6114 7463 81.9 2.48 1.0 1.05 0.7156 0.9553 Inf - 0.82 20097 21576 93.1 3.98 11.8 9.85 0.0783 0.0692 Merged [A], lowest resolution = 5.53 Angstroms, 3604 outliers downweighted #------------------------------------------------------------------------------ Acta Checks: 063_ALERT A Crystal Probably too Large for Beam Size ..... 1.05 mm Cutting the crystals led to shattering. 223_ALERT A Large Solvent/Anion H Ueq(max)/Ueq(min) . 5.52 Ratio 241_ALERT A Check High U(eq) as Compared to Neighbors .... C65B 242_ALERT A Check Low U(eq) as Compared to Neighbors .... C41A 242_ALERT A Check Low U(eq) as Compared to Neighbors .... C41C 242_ALERT A Check Low U(eq) as Compared to Neighbors .... 2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1932P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18770 _refine_ls_number_parameters 1008 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.1590 _refine_ls_R_factor_gt 0.1024 _refine_ls_wR_factor_ref 0.3198 _refine_ls_wR_factor_gt 0.2916 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.037 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.43894(5) 0.18424(3) 0.187943(17) 0.0624(3) Uani 1 1 d . . . O1A O 0.3313(2) 0.20265(16) 0.18334(9) 0.0660(11) Uani 1 1 d . . . C1A C 0.2978(3) 0.2478(2) 0.18571(11) 0.0540(14) Uani 1 1 d . . . C2A C 0.3343(3) 0.2923(2) 0.19675(11) 0.0532(14) Uani 1 1 d . . . C21A C 0.4119(3) 0.2921(2) 0.20746(11) 0.0539(14) Uani 1 1 d . . . H21D H 0.4295 0.3235 0.2158 0.065 Uiso 1 1 calc R . . N2A N 0.4621(3) 0.25273(18) 0.20703(9) 0.0487(11) Uani 1 1 d . . . C22A C 0.5350(4) 0.2614(3) 0.22025(11) 0.0556(15) Uani 1 1 d . . . C23A C 0.5808(5) 0.3028(3) 0.21435(18) 0.088(2) Uani 1 1 d . . . H23D H 0.5651 0.3273 0.2008 0.106 Uiso 1 1 calc R . . C24A C 0.6525(6) 0.3092(5) 0.2286(3) 0.127(4) Uani 1 1 d . . . H24D H 0.6867 0.3375 0.2246 0.153 Uiso 1 1 calc R . . C25A C 0.6715(6) 0.2731(6) 0.2485(2) 0.124(4) Uani 1 1 d . . . H25D H 0.7193 0.2777 0.2583 0.148 Uiso 1 1 calc R . . C26A C 0.6258(6) 0.2317(5) 0.2548(2) 0.111(3) Uani 1 1 d . . . H26D H 0.6402 0.2076 0.2686 0.134 Uiso 1 1 calc R . . C27A C 0.5586(5) 0.2263(4) 0.24039(15) 0.090(2) Uani 1 1 d . . . H27E H 0.5257 0.1971 0.2442 0.108 Uiso 1 1 calc R . . C3A C 0.2911(4) 0.3394(3) 0.19808(14) 0.0719(18) Uani 1 1 d . . . H3AA H 0.3164 0.3691 0.2057 0.086 Uiso 1 1 calc R . . C4A C 0.2162(4) 0.3449(3) 0.18928(15) 0.0737(19) Uani 1 1 d . . . C41A C 0.1701(6) 0.3956(4) 0.1923(2) 0.114(3) Uani 1 1 d . . . C42A C 0.1993(9) 0.4298(4) 0.2141(2) 0.165(6) Uani 1 1 d . . . H42A H 0.1624 0.4588 0.2167 0.199 Uiso 1 1 calc R . . H42B H 0.2511 0.4437 0.2089 0.199 Uiso 1 1 calc R . . H42C H 0.2040 0.4099 0.2311 0.199 Uiso 1 1 calc R . . C43A C 0.0868(7) 0.3815(5) 0.2039(4) 0.229(9) Uani 1 1 d . . . H43A H 0.0488 0.4083 0.1984 0.275 Uiso 1 1 calc R . . H43B H 0.0893 0.3798 0.2239 0.275 Uiso 1 1 calc R . . H43C H 0.0703 0.3475 0.1967 0.275 Uiso 1 1 calc R . . C44A C 0.1649(11) 0.4202(7) 0.1654(4) 0.224(7) Uiso 1 1 d . . . H44J H 0.2180 0.4282 0.1588 0.336 Uiso 1 1 calc R . . H44K H 0.1343 0.4525 0.1668 0.336 Uiso 1 1 calc R . . H44L H 0.1390 0.3963 0.1526 0.336 Uiso 1 1 calc R . . C5A C 0.1796(4) 0.3004(3) 0.17776(14) 0.0721(18) Uani 1 1 d . . . H5AA H 0.1273 0.3030 0.1710 0.087 Uiso 1 1 calc R . . C6A C 0.2191(3) 0.2526(3) 0.17618(12) 0.0594(16) Uani 1 1 d . . . C61A C 0.1807(4) 0.2062(3) 0.16463(14) 0.0694(17) Uani 1 1 d . . . H61G H 0.1252 0.2147 0.1602 0.083 Uiso 1 1 calc R . . H61H H 0.1807 0.1780 0.1784 0.083 Uiso 1 1 calc R . . N6A N 0.2215(3) 0.1875(2) 0.13925(13) 0.0797(17) Uani 1 1 d . A . H6A H 0.2751 0.1853 0.1429 0.096 Uiso 1 1 calc R . . C62A C 0.2099(6) 0.2266(4) 0.11698(18) 0.128(4) Uani 1 1 d . . . H62G H 0.2375 0.2149 0.1005 0.191 Uiso 1 1 calc R . . H62H H 0.2310 0.2604 0.1228 0.191 Uiso 1 1 calc R . . H62I H 0.1536 0.2301 0.1130 0.191 Uiso 1 1 calc R . . C63A C 0.1933(5) 0.1352(4) 0.1319(3) 0.133(4) Uani 1 1 d D . . H63A H 0.1961 0.1332 0.1118 0.160 Uiso 0.517(19) 1 calc PR A 1 H63B H 0.1366 0.1346 0.1367 0.160 Uiso 0.517(19) 1 calc PR A 1 H63C H 0.1401 0.1398 0.1240 0.160 Uiso 0.483(19) 1 calc PR A 2 H63D H 0.1861 0.1160 0.1493 0.160 Uiso 0.483(19) 1 calc PR A 2 C64A C 0.2266(15) 0.0857(5) 0.1423(4) 0.155(11) Uiso 0.517(19) 1 d PD A 1 H64G H 0.1983 0.0749 0.1590 0.186 Uiso 0.517(19) 1 calc PR A 1 H64H H 0.2828 0.0907 0.1470 0.186 Uiso 0.517(19) 1 calc PR A 1 C64X C 0.2368(8) 0.1000(4) 0.1134(3) 0.076(6) Uiso 0.483(19) 1 d PD A 2 H64I H 0.2941 0.1067 0.1150 0.091 Uiso 0.483(19) 1 calc PR A 2 H64J H 0.2209 0.1068 0.0943 0.091 Uiso 0.483(19) 1 calc PR A 2 C65A C 0.2191(6) 0.0437(3) 0.1208(3) 0.133(4) Uani 1 1 d D . . H65A H 0.2204 0.0122 0.1325 0.159 Uiso 0.517(19) 1 calc PR A 1 H65B H 0.1629 0.0477 0.1159 0.159 Uiso 0.517(19) 1 calc PR A 1 H65C H 0.2489 0.0317 0.1370 0.159 Uiso 0.483(19) 1 calc PR A 2 H65D H 0.1622 0.0371 0.1233 0.159 Uiso 0.483(19) 1 calc PR A 2 O1C O 0.5047(3) 0.10548(17) 0.05787(11) 0.0777(13) Uani 1 1 d . C . C1C C 0.5766(4) 0.0871(3) 0.06228(13) 0.0650(17) Uani 1 1 d . . . C2C C 0.6459(4) 0.1153(3) 0.05583(12) 0.0610(16) Uani 1 1 d . . . C21C C 0.6456(4) 0.1676(3) 0.04659(12) 0.0597(16) Uani 1 1 d . . . H21B H 0.6946 0.1814 0.0406 0.072 Uiso 1 1 calc R . . N2C N 0.5850(3) 0.1989(2) 0.04538(9) 0.0558(12) Uani 1 1 d . C . C22C C 0.5997(4) 0.2519(2) 0.03656(12) 0.0593(15) Uani 1 1 d . . . C23C C 0.6670(4) 0.2790(3) 0.04433(14) 0.0720(18) Uani 1 1 d . . . H23A H 0.7048 0.2629 0.0559 0.086 Uiso 1 1 calc R . . C24C C 0.6789(5) 0.3291(3) 0.03530(16) 0.084(2) Uani 1 1 d . . . H24B H 0.7258 0.3473 0.0399 0.101 Uiso 1 1 calc R . . C25C C 0.6227(5) 0.3526(3) 0.01960(17) 0.086(2) Uani 1 1 d . . . H25A H 0.6294 0.3879 0.0141 0.103 Uiso 1 1 calc R . . C26C C 0.5576(5) 0.3260(3) 0.01186(14) 0.079(2) Uani 1 1 d . . . H26B H 0.5197 0.3425 0.0005 0.095 Uiso 1 1 calc R . . C27C C 0.5457(4) 0.2760(3) 0.02003(13) 0.0679(17) Uani 1 1 d . . . H27B H 0.4999 0.2577 0.0143 0.081 Uiso 1 1 calc R . . C3C C 0.7190(4) 0.0915(3) 0.05968(13) 0.0646(17) Uani 1 1 d . . . H3CA H 0.7650 0.1104 0.0547 0.078 Uiso 1 1 calc R . . C4C C 0.7283(4) 0.0421(3) 0.07032(15) 0.0729(18) Uani 1 1 d . . . C41C C 0.8075(4) 0.0169(3) 0.07640(19) 0.090(2) Uani 1 1 d . . . C42C C 0.8744(6) 0.0479(5) 0.0667(4) 0.210(8) Uani 1 1 d . . . H42D H 0.8708 0.0522 0.0469 0.315 Uiso 1 1 calc R . . H42E H 0.9236 0.0299 0.0713 0.315 Uiso 1 1 calc R . . H42F H 0.8736 0.0822 0.0755 0.315 Uiso 1 1 calc R . . C43C C 0.8239(9) 0.0157(8) 0.1071(3) 0.240(10) Uani 1 1 d . . . H43D H 0.8753 -0.0005 0.1104 0.359 Uiso 1 1 calc R . . H43E H 0.7828 -0.0046 0.1163 0.359 Uiso 1 1 calc R . . H43F H 0.8241 0.0514 0.1143 0.359 Uiso 1 1 calc R . . C44C C 0.8086(6) -0.0386(4) 0.0669(3) 0.138(4) Uani 1 1 d . . . H44A H 0.8600 -0.0542 0.0710 0.207 Uiso 1 1 calc R . . H44B H 0.7994 -0.0397 0.0471 0.207 Uiso 1 1 calc R . . H44C H 0.7672 -0.0583 0.0762 0.207 Uiso 1 1 calc R . . C5C C 0.6585(4) 0.0157(3) 0.07748(14) 0.0720(18) Uani 1 1 d . . . H5CA H 0.6624 -0.0180 0.0855 0.086 Uiso 1 1 calc R . . C6C C 0.5845(4) 0.0369(2) 0.07319(13) 0.0603(15) Uani 1 1 d . . . C61C C 0.5112(4) 0.0092(3) 0.08155(14) 0.0703(18) Uani 1 1 d . . . H61C H 0.5243 -0.0268 0.0874 0.084 Uiso 1 1 calc R . . H61D H 0.4747 0.0070 0.0658 0.084 Uiso 1 1 calc R . . N6C N 0.4717(3) 0.0380(2) 0.10480(11) 0.0659(14) Uani 1 1 d . . . H6C H 0.4678 0.0730 0.0998 0.079 Uiso 1 1 calc R . . C62C C 0.5166(5) 0.0357(4) 0.13005(15) 0.092(2) Uani 1 1 d . . . H62D H 0.5699 0.0490 0.1268 0.139 Uiso 1 1 calc R . . H62E H 0.5196 -0.0006 0.1363 0.139 Uiso 1 1 calc R . . H62F H 0.4906 0.0570 0.1440 0.139 Uiso 1 1 calc R . . C63C C 0.3905(4) 0.0184(3) 0.10962(17) 0.087(2) Uani 1 1 d . A . H63E H 0.3918 -0.0201 0.1111 0.104 Uiso 1 1 calc R . . H63F H 0.3708 0.0325 0.1272 0.104 Uiso 1 1 calc R . . C64C C 0.3390(5) 0.0327(6) 0.0887(2) 0.150(5) Uani 1 1 d . . . H64C H 0.3544 0.0140 0.0718 0.180 Uiso 1 1 calc R A . H64D H 0.3451 0.0706 0.0852 0.180 Uiso 1 1 calc R . . C65C C 0.2502(6) 0.0212(5) 0.0946(3) 0.147(4) Uani 1 1 d . A . H65C' H 0.2184 0.0350 0.0793 0.176 Uiso 1 1 calc R . . H65D' H 0.2427 -0.0172 0.0951 0.176 Uiso 1 1 calc R . . Cu2 Cu 0.47414(5) 0.17602(3) 0.057962(19) 0.0698(3) Uani 1 1 d . . . O1B O 0.5472(2) 0.16568(17) 0.18802(8) 0.0612(11) Uani 1 1 d . . . C1B C 0.5768(4) 0.1187(3) 0.18909(12) 0.0592(15) Uani 1 1 d . . . C2B C 0.5352(4) 0.0736(2) 0.19870(13) 0.0574(15) Uani 1 1 d . . . C21B C 0.4565(4) 0.0751(2) 0.20822(12) 0.0576(15) Uani 1 1 d . . . H21C H 0.4359 0.0435 0.2155 0.069 Uiso 1 1 calc R . . N2B N 0.4092(3) 0.11538(19) 0.20810(9) 0.0555(12) Uani 1 1 d . . . C22B C 0.3323(4) 0.1073(3) 0.21896(13) 0.0660(18) Uani 1 1 d . . . C23B C 0.2835(5) 0.0704(3) 0.2089(2) 0.098(3) Uani 1 1 d . . . H23C H 0.2991 0.0486 0.1941 0.118 Uiso 1 1 calc R . . C24B C 0.2085(6) 0.0653(4) 0.2211(3) 0.133(4) Uani 1 1 d . . . H24C H 0.1719 0.0411 0.2137 0.160 Uiso 1 1 calc R . . C25B C 0.1880(8) 0.0939(5) 0.2429(3) 0.143(5) Uani 1 1 d . . . H25C H 0.1394 0.0873 0.2519 0.171 Uiso 1 1 calc R . . C26B C 0.2374(8) 0.1333(6) 0.2524(2) 0.137(4) Uani 1 1 d . . . H26C H 0.2202 0.1559 0.2666 0.164 Uiso 1 1 calc R . . C27B C 0.3108(5) 0.1394(4) 0.24128(16) 0.099(3) Uani 1 1 d . . . H27C H 0.3464 0.1646 0.2484 0.118 Uiso 1 1 calc R . . C3B C 0.5730(4) 0.0250(3) 0.19933(15) 0.0736(19) Uani 1 1 d . . . H3BA H 0.5442 -0.0046 0.2055 0.088 Uiso 1 1 calc R . . C4B C 0.6508(4) 0.0184(3) 0.19135(17) 0.083(2) Uani 1 1 d . B . C41B C 0.6890(5) -0.0374(3) 0.19392(19) 0.106(3) Uani 1 1 d D . . C42B C 0.7769(7) -0.0350(7) 0.1923(4) 0.116(6) Uiso 0.558(14) 1 d PD B 1 H42G H 0.7982 -0.0705 0.1909 0.139 Uiso 0.558(14) 1 calc PR B 1 H42H H 0.7977 -0.0181 0.2087 0.139 Uiso 0.558(14) 1 calc PR B 1 H42I H 0.7924 -0.0149 0.1761 0.139 Uiso 0.558(14) 1 calc PR B 1 C43B C 0.6530(10) -0.0744(7) 0.1729(3) 0.119(7) Uiso 0.558(14) 1 d PD B 1 H43G H 0.6802 -0.1081 0.1737 0.143 Uiso 0.558(14) 1 calc PR B 1 H43H H 0.6589 -0.0594 0.1546 0.143 Uiso 0.558(14) 1 calc PR B 1 H43I H 0.5970 -0.0794 0.1769 0.143 Uiso 0.558(14) 1 calc PR B 1 C44B C 0.6619(9) -0.0642(6) 0.2214(3) 0.097(5) Uiso 0.558(14) 1 d PD B 1 H44D H 0.6045 -0.0686 0.2212 0.117 Uiso 0.558(14) 1 calc PR B 1 H44E H 0.6770 -0.0422 0.2369 0.117 Uiso 0.558(14) 1 calc PR B 1 H44F H 0.6872 -0.0984 0.2231 0.117 Uiso 0.558(14) 1 calc PR B 1 C42' C 0.6304(14) -0.0786(10) 0.2010(6) 0.164(12) Uiso 0.442(14) 1 d PD B 2 H42J H 0.6533 -0.1131 0.1975 0.197 Uiso 0.442(14) 1 calc PR B 2 H42K H 0.5831 -0.0742 0.1898 0.197 Uiso 0.442(14) 1 calc PR B 2 H42L H 0.6163 -0.0757 0.2204 0.197 Uiso 0.442(14) 1 calc PR B 2 C43' C 0.7574(11) -0.0276(9) 0.2135(4) 0.120(8) Uiso 0.442(14) 1 d PD B 2 H43J H 0.7368 -0.0212 0.2319 0.144 Uiso 0.442(14) 1 calc PR B 2 H43K H 0.7874 0.0029 0.2074 0.144 Uiso 0.442(14) 1 calc PR B 2 H43L H 0.7919 -0.0583 0.2138 0.144 Uiso 0.442(14) 1 calc PR B 2 C44' C 0.7229(17) -0.0454(12) 0.1650(4) 0.172(13) Uiso 0.442(14) 1 d PD B 2 H44G H 0.7463 -0.0802 0.1636 0.207 Uiso 0.442(14) 1 calc PR B 2 H44H H 0.7633 -0.0189 0.1614 0.207 Uiso 0.442(14) 1 calc PR B 2 H44I H 0.6805 -0.0420 0.1515 0.207 Uiso 0.442(14) 1 calc PR B 2 C5B C 0.6913(4) 0.0617(3) 0.18262(15) 0.076(2) Uani 1 1 d . . . H5BA H 0.7448 0.0582 0.1772 0.092 Uiso 1 1 calc R B . C6B C 0.6562(4) 0.1104(3) 0.18154(13) 0.0643(17) Uani 1 1 d . B . C61B C 0.7025(4) 0.1587(3) 0.17349(16) 0.077(2) Uani 1 1 d . . . H61E H 0.6942 0.1863 0.1873 0.092 Uiso 1 1 calc R B . H61F H 0.7593 0.1502 0.1731 0.092 Uiso 1 1 calc R . . N6B N 0.6776(3) 0.1787(2) 0.14603(12) 0.0738(15) Uani 1 1 d . B . H6B H 0.6230 0.1813 0.1462 0.089 Uiso 1 1 calc R . . C62B C 0.6991(6) 0.1439(4) 0.12321(19) 0.124(4) Uani 1 1 d . . . H62J H 0.6777 0.1090 0.1265 0.185 Uiso 1 1 calc R B . H62K H 0.7566 0.1419 0.1218 0.185 Uiso 1 1 calc R . . H62L H 0.6774 0.1578 0.1061 0.185 Uiso 1 1 calc R . . C63B C 0.7095(5) 0.2320(4) 0.1414(2) 0.104(3) Uani 1 1 d D . . H63H H 0.7654 0.2329 0.1471 0.125 Uiso 1 1 calc R B . H63I H 0.7072 0.2401 0.1216 0.125 Uiso 1 1 calc R . . C64B C 0.6665(8) 0.2714(4) 0.1563(2) 0.161(5) Uani 1 1 d D B . H64E H 0.6763 0.2664 0.1760 0.193 Uiso 1 1 calc R . . H64F H 0.6095 0.2659 0.1531 0.193 Uiso 1 1 calc R . . C65B C 0.6862(11) 0.3263(5) 0.1490(2) 0.221(9) Uani 1 1 d D . . H65E H 0.6496 0.3500 0.1587 0.265 Uiso 1 1 calc R B . H65F H 0.7402 0.3341 0.1555 0.265 Uiso 1 1 calc R . . O1D O 0.4423(3) 0.24478(17) 0.06456(8) 0.0650(11) Uani 1 1 d . C . C1D C 0.3737(4) 0.2666(2) 0.06042(11) 0.0571(15) Uani 1 1 d . . . C2D C 0.3097(4) 0.2424(2) 0.04718(12) 0.0598(15) Uani 1 1 d . C . C21D C 0.3148(4) 0.1918(2) 0.03440(11) 0.0564(15) Uani 1 1 d . . . H21A H 0.2703 0.1807 0.0241 0.068 Uiso 1 1 calc R C . N2D N 0.3743(3) 0.1597(2) 0.03551(9) 0.0570(12) Uani 1 1 d . C . C22D C 0.3662(4) 0.1116(2) 0.02112(12) 0.0548(14) Uani 1 1 d . . . C23D C 0.3006(4) 0.0810(3) 0.02398(14) 0.0711(18) Uani 1 1 d . C . H23B H 0.2583 0.0920 0.0353 0.085 Uiso 1 1 calc R . . C24D C 0.2964(5) 0.0334(3) 0.00999(17) 0.087(2) Uani 1 1 d . . . H24A H 0.2512 0.0120 0.0122 0.105 Uiso 1 1 calc R C . C25D C 0.3548(6) 0.0174(3) -0.00642(16) 0.094(3) Uani 1 1 d . C . H25B H 0.3506 -0.0145 -0.0162 0.113 Uiso 1 1 calc R . . C26D C 0.4221(6) 0.0486(3) -0.00878(16) 0.089(2) Uani 1 1 d . . . H26A H 0.4647 0.0376 -0.0200 0.107 Uiso 1 1 calc R C . C27D C 0.4263(4) 0.0943(3) 0.00489(14) 0.076(2) Uani 1 1 d . C . H27A H 0.4724 0.1150 0.0032 0.091 Uiso 1 1 calc R . . C3D C 0.2388(4) 0.2698(3) 0.04362(13) 0.0662(17) Uani 1 1 d . . . H3DA H 0.1973 0.2532 0.0340 0.079 Uiso 1 1 calc R C . C4D C 0.2264(4) 0.3194(3) 0.05330(13) 0.0673(17) Uani 1 1 d . C . C41D C 0.1466(5) 0.3494(3) 0.05032(15) 0.081(2) Uani 1 1 d . . . C42D C 0.0819(5) 0.3144(3) 0.03966(19) 0.100(3) Uani 1 1 d . C . H42M H 0.0964 0.3013 0.0215 0.150 Uiso 1 1 calc R . . H42N H 0.0327 0.3342 0.0384 0.150 Uiso 1 1 calc R . . H42O H 0.0746 0.2849 0.0522 0.150 Uiso 1 1 calc R . . C43D C 0.1598(6) 0.3963(4) 0.0321(2) 0.126(4) Uani 1 1 d . C . H43M H 0.1761 0.3846 0.0139 0.189 Uiso 1 1 calc R . . H43N H 0.2010 0.4185 0.0400 0.189 Uiso 1 1 calc R . . H43O H 0.1108 0.4163 0.0306 0.189 Uiso 1 1 calc R . . C44D C 0.1209(5) 0.3678(4) 0.0787(2) 0.117(3) Uani 1 1 d . C . H44M H 0.1138 0.3375 0.0906 0.176 Uiso 1 1 calc R . . H44N H 0.0711 0.3869 0.0772 0.176 Uiso 1 1 calc R . . H44O H 0.1614 0.3908 0.0863 0.176 Uiso 1 1 calc R . . C5D C 0.2902(4) 0.3434(3) 0.06606(13) 0.0695(18) Uani 1 1 d . . . H5DA H 0.2845 0.3782 0.0725 0.083 Uiso 1 1 calc R C . C6D C 0.3612(4) 0.3183(2) 0.06961(13) 0.0640(17) Uani 1 1 d . C . C61D C 0.4312(4) 0.3456(3) 0.08212(14) 0.077(2) Uani 1 1 d . . . H61A H 0.4778 0.3402 0.0703 0.092 Uiso 1 1 calc R C . H61B H 0.4206 0.3835 0.0830 0.092 Uiso 1 1 calc R . . N6D N 0.4489(4) 0.3261(2) 0.11008(12) 0.0768(16) Uani 1 1 d . C . H6D H 0.4518 0.2899 0.1094 0.092 Uiso 1 1 calc R . . C62D C 0.3829(6) 0.3412(5) 0.12944(16) 0.132(4) Uani 1 1 d . . . H62A H 0.3327 0.3281 0.1223 0.198 Uiso 1 1 calc R C . H62B H 0.3804 0.3794 0.1310 0.198 Uiso 1 1 calc R . . H62C H 0.3928 0.3261 0.1475 0.198 Uiso 1 1 calc R . . C63D C 0.5265(5) 0.3467(4) 0.1205(2) 0.115(3) Uani 1 1 d . . . H63J H 0.5271 0.3852 0.1186 0.138 Uiso 1 1 calc R C . H63K H 0.5313 0.3383 0.1402 0.138 Uiso 1 1 calc R . . C64D C 0.5940(8) 0.3252(5) 0.1061(3) 0.155(5) Uani 1 1 d . B . H64A H 0.5943 0.3394 0.0873 0.186 Uiso 1 1 calc R . . H64B H 0.5869 0.2869 0.1046 0.186 Uiso 1 1 calc R . . C65D C 0.6817(7) 0.3368(5) 0.1202(2) 0.147(5) Uani 1 1 d D B . H65J H 0.7216 0.3151 0.1107 0.177 Uiso 1 1 calc R . . H65K H 0.6955 0.3738 0.1170 0.177 Uiso 1 1 calc R . . S1 S 0.44893(9) 0.18002(6) 0.12423(3) 0.0563(4) Uani 1 1 d . . . O1S O 0.4291(3) 0.14839(18) 0.14803(9) 0.0765(13) Uani 1 1 d . C . O2S O 0.4661(7) 0.1474(4) 0.09998(19) 0.073(3) Uiso 0.488(10) 1 d P C 1 O3S O 0.3681(7) 0.2041(5) 0.1175(2) 0.095(4) Uiso 0.488(10) 1 d P C 1 O4S O 0.5086(6) 0.2176(4) 0.1288(2) 0.080(3) Uiso 0.488(10) 1 d P C 1 O2S' O 0.4178(5) 0.1584(3) 0.09980(16) 0.058(3) Uiso 0.512(10) 1 d P C 2 O3S' O 0.4194(6) 0.2338(4) 0.1274(2) 0.091(4) Uiso 0.512(10) 1 d P C 2 O4S' O 0.5360(7) 0.1819(5) 0.1236(2) 0.102(4) Uiso 0.512(10) 1 d P C 2 S2 S -0.04509(18) 0.1680(3) 0.12354(6) 0.1630(18) Uani 1 1 d . . . O5S O -0.1044(6) 0.1633(7) 0.1431(2) 0.283(7) Uani 1 1 d . . . O6S O 0.0100(5) 0.2071(5) 0.1301(2) 0.213(5) Uani 1 1 d . . . O7S O -0.0744(7) 0.1798(5) 0.0978(2) 0.239(6) Uani 1 1 d . . . O8S O -0.0065(6) 0.1166(5) 0.12346(17) 0.170(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0598(5) 0.0462(5) 0.0813(6) -0.0068(4) -0.0098(4) 0.0010(3) O1A 0.057(2) 0.048(3) 0.094(3) -0.008(2) -0.014(2) 0.001(2) C1A 0.062(4) 0.050(4) 0.050(3) -0.002(3) 0.005(3) -0.004(3) C2A 0.062(4) 0.051(4) 0.046(3) 0.003(3) 0.007(3) 0.010(3) C21A 0.061(4) 0.050(4) 0.050(3) -0.008(3) -0.002(3) -0.002(3) N2A 0.053(3) 0.049(3) 0.043(3) -0.003(2) -0.003(2) -0.001(2) C22A 0.063(4) 0.060(4) 0.044(3) -0.014(3) -0.004(3) 0.012(3) C23A 0.086(5) 0.076(5) 0.103(6) -0.018(4) -0.012(5) -0.005(4) C24A 0.092(7) 0.132(9) 0.157(10) -0.041(8) -0.017(7) -0.040(6) C25A 0.089(7) 0.174(12) 0.108(8) -0.046(8) -0.047(6) 0.032(7) C26A 0.105(7) 0.128(9) 0.101(7) -0.030(6) -0.036(6) 0.010(6) C27A 0.086(5) 0.120(7) 0.064(5) -0.005(4) -0.013(4) 0.013(5) C3A 0.082(5) 0.060(4) 0.073(4) -0.010(3) -0.003(4) 0.000(4) C4A 0.073(5) 0.062(5) 0.086(5) 0.002(4) -0.006(4) 0.021(4) C41A 0.120(8) 0.086(6) 0.136(8) -0.010(6) -0.030(6) 0.049(6) C42A 0.269(16) 0.090(7) 0.137(9) -0.036(7) -0.028(10) 0.089(9) C43A 0.122(10) 0.140(12) 0.43(3) -0.095(14) 0.047(13) 0.043(9) C5A 0.070(4) 0.082(5) 0.064(4) -0.004(4) -0.005(3) 0.014(4) C6A 0.055(3) 0.076(5) 0.047(3) 0.011(3) 0.006(3) 0.001(3) C61A 0.061(4) 0.077(5) 0.070(4) -0.001(4) 0.000(3) -0.003(3) N6A 0.059(3) 0.088(4) 0.092(4) -0.024(4) 0.002(3) -0.012(3) C62A 0.165(10) 0.138(9) 0.080(6) -0.011(6) 0.017(6) -0.064(7) C63A 0.083(6) 0.107(8) 0.210(11) -0.069(8) -0.018(7) -0.024(5) C65A 0.092(6) 0.070(6) 0.236(14) -0.032(7) -0.026(8) -0.021(5) O1C 0.059(3) 0.055(3) 0.119(4) 0.009(3) 0.007(3) -0.003(2) C1C 0.066(4) 0.063(4) 0.066(4) -0.006(3) 0.009(3) -0.006(3) C2C 0.071(4) 0.057(4) 0.055(4) -0.006(3) 0.007(3) -0.005(3) C21C 0.060(4) 0.068(4) 0.051(4) -0.006(3) 0.009(3) -0.012(3) N2C 0.061(3) 0.057(3) 0.049(3) -0.006(2) 0.003(2) -0.005(3) C22C 0.069(4) 0.061(4) 0.048(3) -0.006(3) 0.004(3) -0.007(3) C23C 0.077(4) 0.076(5) 0.062(4) -0.007(3) -0.001(3) -0.014(4) C24C 0.110(6) 0.062(5) 0.081(5) -0.001(4) -0.006(5) -0.024(4) C25C 0.114(6) 0.057(5) 0.087(5) 0.014(4) 0.004(5) -0.008(4) C26C 0.102(6) 0.075(5) 0.061(4) 0.007(4) 0.001(4) 0.001(4) C27C 0.081(4) 0.068(5) 0.055(4) 0.002(3) -0.004(3) -0.002(4) C3C 0.059(4) 0.061(4) 0.074(4) -0.009(3) 0.013(3) -0.004(3) C4C 0.063(4) 0.079(5) 0.077(5) -0.015(4) 0.005(3) 0.002(4) C41C 0.078(5) 0.073(5) 0.118(7) -0.012(5) -0.002(5) 0.017(4) C42C 0.080(7) 0.127(10) 0.42(3) 0.086(13) -0.011(11) -0.002(7) C43C 0.189(14) 0.36(2) 0.168(13) -0.108(15) -0.092(11) 0.144(15) C44C 0.102(7) 0.096(7) 0.217(12) -0.033(7) -0.028(7) 0.029(6) C5C 0.075(5) 0.059(4) 0.082(5) -0.010(3) 0.002(4) 0.006(4) C6C 0.065(4) 0.045(4) 0.071(4) -0.006(3) 0.006(3) 0.001(3) C61C 0.081(4) 0.053(4) 0.076(4) -0.014(3) 0.008(4) -0.010(3) N6C 0.069(3) 0.058(3) 0.071(4) -0.004(3) 0.014(3) -0.012(3) C62C 0.091(5) 0.118(7) 0.068(5) 0.006(4) 0.002(4) -0.013(5) C63C 0.072(5) 0.090(6) 0.098(6) 0.010(4) 0.006(4) -0.010(4) C64C 0.085(6) 0.245(14) 0.119(8) 0.039(9) -0.011(6) -0.047(8) C65C 0.105(8) 0.156(11) 0.180(12) 0.021(9) -0.039(8) -0.035(7) Cu2 0.0608(5) 0.0594(5) 0.0892(6) 0.0038(4) 0.0051(4) -0.0032(4) O1B 0.060(2) 0.056(3) 0.068(3) -0.009(2) -0.009(2) -0.003(2) C1B 0.062(4) 0.054(4) 0.061(4) -0.010(3) -0.009(3) 0.005(3) C2B 0.057(4) 0.051(4) 0.064(4) -0.005(3) -0.004(3) 0.005(3) C21B 0.076(4) 0.039(3) 0.057(4) 0.004(3) -0.002(3) 0.000(3) N2B 0.062(3) 0.055(3) 0.049(3) -0.002(2) 0.005(2) 0.002(2) C22B 0.074(4) 0.068(5) 0.056(4) 0.022(3) 0.016(3) 0.015(4) C23B 0.072(5) 0.086(6) 0.136(8) 0.010(5) 0.031(5) -0.003(4) C24B 0.079(6) 0.113(8) 0.208(12) 0.022(8) 0.037(7) -0.010(5) C25B 0.137(10) 0.123(10) 0.168(11) 0.071(9) 0.096(9) 0.056(8) C26B 0.154(11) 0.159(12) 0.097(7) 0.026(8) 0.069(7) 0.033(9) C27B 0.104(6) 0.122(7) 0.070(5) 0.005(5) 0.021(5) 0.026(5) C3B 0.072(4) 0.050(4) 0.099(5) 0.002(3) -0.009(4) 0.006(3) C4B 0.066(4) 0.070(5) 0.112(6) -0.021(4) -0.016(4) 0.012(4) C41B 0.079(5) 0.094(6) 0.145(8) -0.020(6) -0.011(5) 0.035(5) C5B 0.062(4) 0.072(5) 0.096(5) -0.020(4) -0.008(4) 0.002(4) C6B 0.058(4) 0.065(4) 0.070(4) -0.004(3) -0.011(3) 0.000(3) C61B 0.054(4) 0.089(5) 0.088(5) -0.007(4) -0.012(4) -0.012(4) N6B 0.062(3) 0.079(4) 0.080(4) -0.013(3) 0.011(3) -0.006(3) C62B 0.150(9) 0.116(8) 0.105(7) -0.053(6) 0.027(6) -0.013(7) C63B 0.075(5) 0.112(7) 0.126(8) -0.020(6) 0.016(5) -0.026(5) C64B 0.207(13) 0.158(11) 0.118(9) -0.021(8) 0.012(9) -0.078(11) C65B 0.35(2) 0.173(13) 0.141(11) -0.028(10) 0.062(13) -0.171(14) O1D 0.063(3) 0.071(3) 0.061(3) -0.003(2) 0.003(2) -0.006(2) C1D 0.072(4) 0.054(4) 0.045(3) 0.002(3) 0.009(3) -0.010(3) C2D 0.070(4) 0.057(4) 0.052(4) -0.001(3) 0.009(3) 0.002(3) C21D 0.068(4) 0.058(4) 0.043(3) 0.002(3) -0.002(3) -0.001(3) N2D 0.063(3) 0.057(3) 0.051(3) 0.000(2) 0.002(2) 0.004(3) C22D 0.067(4) 0.048(4) 0.050(3) 0.002(3) 0.001(3) 0.004(3) C23D 0.067(4) 0.066(5) 0.080(5) 0.002(4) -0.003(4) 0.005(3) C24D 0.101(6) 0.056(5) 0.105(6) -0.002(4) -0.015(5) -0.008(4) C25D 0.150(8) 0.059(5) 0.073(5) -0.012(4) -0.013(5) 0.031(5) C26D 0.120(7) 0.065(5) 0.084(5) -0.012(4) 0.030(5) 0.005(5) C27D 0.087(5) 0.067(5) 0.074(5) -0.008(4) 0.025(4) -0.003(4) C3D 0.080(4) 0.062(4) 0.056(4) -0.006(3) -0.002(3) 0.004(3) C4D 0.085(5) 0.059(4) 0.058(4) -0.002(3) -0.003(3) 0.007(4) C41D 0.104(6) 0.065(5) 0.075(5) -0.011(4) -0.008(4) 0.029(4) C42D 0.087(5) 0.096(6) 0.116(7) -0.014(5) -0.030(5) 0.019(5) C43D 0.149(9) 0.094(7) 0.135(8) 0.041(6) -0.010(7) 0.040(6) C44D 0.097(6) 0.128(8) 0.127(8) -0.047(6) -0.007(6) 0.036(6) C5D 0.099(5) 0.054(4) 0.056(4) -0.003(3) 0.007(4) 0.003(4) C6D 0.088(5) 0.052(4) 0.051(4) -0.007(3) 0.008(3) -0.013(4) C61D 0.095(5) 0.070(5) 0.065(4) -0.003(4) 0.014(4) -0.011(4) N6D 0.098(4) 0.063(4) 0.069(4) -0.009(3) 0.001(3) -0.021(3) C62D 0.117(7) 0.221(12) 0.059(5) -0.027(6) 0.025(5) -0.061(8) C63D 0.097(6) 0.089(7) 0.160(9) -0.044(6) 0.025(6) -0.043(5) C64D 0.181(12) 0.150(11) 0.135(10) -0.015(8) 0.005(9) -0.041(9) C65D 0.165(10) 0.139(9) 0.139(10) 0.017(7) -0.015(8) -0.102(8) S1 0.0636(9) 0.0549(9) 0.0506(9) -0.0064(7) 0.0050(7) -0.0117(7) O1S 0.094(3) 0.076(3) 0.060(3) -0.002(2) -0.007(2) -0.021(3) S2 0.0828(18) 0.317(6) 0.089(2) -0.002(3) -0.0155(15) -0.023(3) O5S 0.121(7) 0.52(2) 0.205(10) 0.014(13) 0.065(7) -0.012(10) O6S 0.101(6) 0.258(12) 0.280(12) -0.091(10) -0.058(7) 0.033(7) O7S 0.238(11) 0.346(16) 0.132(7) -0.046(8) -0.081(7) 0.093(10) O8S 0.148(7) 0.236(11) 0.126(6) 0.041(7) -0.043(5) -0.032(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1B 1.899(4) . ? Cu1 O1A 1.901(4) . ? Cu1 N2A 2.026(5) . ? Cu1 N2B 2.083(5) . ? Cu1 O1S 2.165(4) . ? O1A C1A 1.293(7) . ? C1A C2A 1.406(8) . ? C1A C6A 1.421(8) . ? C2A C3A 1.413(8) . ? C2A C21A 1.418(8) . ? C21A N2A 1.321(7) . ? N2A C22A 1.414(7) . ? C22A C23A 1.346(10) . ? C22A C27A 1.393(9) . ? C23A C24A 1.413(12) . ? C24A C25A 1.380(15) . ? C25A C26A 1.350(15) . ? C26A C27A 1.348(11) . ? C3A C4A 1.350(9) . ? C4A C5A 1.416(10) . ? C4A C41A 1.523(10) . ? C41A C44A 1.464(18) . ? C41A C42A 1.466(13) . ? C41A C43A 1.567(16) . ? C5A C6A 1.398(9) . ? C6A C61A 1.468(9) . ? C61A N6A 1.502(8) . ? N6A C63A 1.466(10) . ? N6A C62A 1.493(11) . ? C63A C64X 1.478(10) . ? C63A C64A 1.478(11) . ? C64A C65A 1.510(11) . ? C64X C65A 1.518(10) . ? C65A C65C 1.499(15) . ? O1C C1C 1.327(8) . ? O1C Cu2 1.880(5) . ? C1C C6C 1.399(9) . ? C1C C2C 1.416(9) . ? C2C C3C 1.396(9) . ? C2C C21C 1.415(9) . ? C21C N2C 1.305(8) . ? N2C C22C 1.445(8) . ? N2C Cu2 2.066(5) . ? C22C C27C 1.371(9) . ? C22C C23C 1.390(9) . ? C23C C24C 1.373(9) . ? C24C C25C 1.365(10) . ? C25C C26C 1.354(10) . ? C26C C27C 1.357(9) . ? C3C C4C 1.376(9) . ? C4C C5C 1.409(9) . ? C4C C41C 1.521(10) . ? C41C C42C 1.464(13) . ? C41C C44C 1.498(12) . ? C41C C43C 1.527(15) . ? C5C C6C 1.386(9) . ? C6C C61C 1.490(8) . ? C61C N6C 1.514(8) . ? N6C C62C 1.453(9) . ? N6C C63C 1.486(8) . ? C63C C64C 1.396(11) . ? C64C C65C 1.564(13) . ? Cu2 O1D 1.870(5) . ? Cu2 N2D 2.063(5) . ? Cu2 O2S 2.188(10) . ? Cu2 O2S' 2.305(8) . ? O1B C1B 1.305(7) . ? C1B C6B 1.414(9) . ? C1B C2B 1.433(9) . ? C2B C3B 1.401(8) . ? C2B C21B 1.416(8) . ? C21B N2B 1.308(7) . ? N2B C22B 1.425(8) . ? C22B C23B 1.350(10) . ? C22B C27B 1.416(10) . ? C23B C24B 1.412(12) . ? C24B C25B 1.340(15) . ? C25B C26B 1.392(17) . ? C26B C27B 1.368(13) . ? C3B C4B 1.388(9) . ? C4B C5B 1.374(10) . ? C4B C41B 1.575(11) . ? C41B C42' 1.492(14) . ? C41B C42B 1.497(12) . ? C41B C43B 1.527(12) . ? C41B C43' 1.528(13) . ? C41B C44' 1.542(14) . ? C41B C44B 1.579(12) . ? C5B C6B 1.382(9) . ? C6B C61B 1.519(9) . ? C61B N6B 1.499(9) . ? N6B C62B 1.474(9) . ? N6B C63B 1.487(10) . ? C63B C64B 1.443(9) . ? C64B C65B 1.489(9) . ? C65B C65D 1.439(9) . ? O1D C1D 1.308(7) . ? C1D C2D 1.408(9) . ? C1D C6D 1.416(8) . ? C2D C3D 1.405(9) . ? C2D C21D 1.442(8) . ? C21D N2D 1.304(7) . ? N2D C22D 1.425(7) . ? C22D C27D 1.367(8) . ? C22D C23D 1.369(9) . ? C23D C24D 1.401(10) . ? C24D C25D 1.341(11) . ? C25D C26D 1.399(11) . ? C26D C27D 1.350(10) . ? C3D C4D 1.371(9) . ? C4D C5D 1.394(9) . ? C4D C41D 1.565(10) . ? C41D C42D 1.511(11) . ? C41D C43D 1.514(11) . ? C41D C44D 1.529(11) . ? C5D C6D 1.378(9) . ? C6D C61D 1.508(9) . ? C61D N6D 1.487(9) . ? N6D C63D 1.508(10) . ? N6D C62D 1.519(10) . ? C63D C64D 1.454(15) . ? C64D C65D 1.668(16) . ? S1 O4S 1.416(10) . ? S1 O2S' 1.420(8) . ? S1 O1S 1.458(5) . ? S1 O3S' 1.475(11) . ? S1 O4S' 1.480(12) . ? S1 O2S 1.481(10) . ? S1 O3S 1.540(11) . ? S2 O7S 1.387(9) . ? S2 O5S 1.396(10) . ? S2 O6S 1.408(11) . ? S2 O8S 1.471(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1B Cu1 O1A 173.30(19) . . ? O1B Cu1 N2A 91.59(18) . . ? O1A Cu1 N2A 91.54(18) . . ? O1B Cu1 N2B 91.25(19) . . ? O1A Cu1 N2B 91.89(19) . . ? N2A Cu1 N2B 124.19(18) . . ? O1B Cu1 O1S 88.31(18) . . ? O1A Cu1 O1S 85.63(19) . . ? N2A Cu1 O1S 142.97(18) . . ? N2B Cu1 O1S 92.83(18) . . ? C1A O1A Cu1 129.3(4) . . ? O1A C1A C2A 124.5(5) . . ? O1A C1A C6A 117.5(5) . . ? C2A C1A C6A 118.0(6) . . ? C1A C2A C3A 118.8(6) . . ? C1A C2A C21A 123.2(5) . . ? C3A C2A C21A 118.0(6) . . ? N2A C21A C2A 126.7(5) . . ? C21A N2A C22A 116.0(5) . . ? C21A N2A Cu1 122.9(4) . . ? C22A N2A Cu1 121.1(4) . . ? C23A C22A C27A 119.7(7) . . ? C23A C22A N2A 122.0(6) . . ? C27A C22A N2A 118.3(6) . . ? C22A C23A C24A 118.9(9) . . ? C25A C24A C23A 118.2(10) . . ? C26A C25A C24A 123.4(9) . . ? C27A C26A C25A 116.8(10) . . ? C26A C27A C22A 123.0(9) . . ? C4A C3A C2A 124.3(7) . . ? C3A C4A C5A 117.2(6) . . ? C3A C4A C41A 122.8(7) . . ? C5A C4A C41A 120.0(7) . . ? C44A C41A C42A 114.7(11) . . ? C44A C41A C4A 108.0(11) . . ? C42A C41A C4A 114.0(8) . . ? C44A C41A C43A 111.8(12) . . ? C42A C41A C43A 100.4(11) . . ? C4A C41A C43A 107.6(9) . . ? C6A C5A C4A 121.1(6) . . ? C5A C6A C1A 120.7(6) . . ? C5A C6A C61A 121.1(6) . . ? C1A C6A C61A 118.3(6) . . ? C6A C61A N6A 111.8(5) . . ? C63A N6A C62A 113.0(8) . . ? C63A N6A C61A 110.0(6) . . ? C62A N6A C61A 109.2(6) . . ? N6A C63A C64X 122.9(9) . . ? N6A C63A C64A 125.1(11) . . ? C64X C63A C64A 59.7(10) . . ? C63A C64A C65A 110.0(11) . . ? C63A C64X C65A 109.6(10) . . ? C65C C65A C64A 147.0(13) . . ? C65C C65A C64X 95.3(11) . . ? C64A C65A C64X 58.1(10) . . ? C1C O1C Cu2 126.5(4) . . ? O1C C1C C6C 118.4(6) . . ? O1C C1C C2C 123.2(6) . . ? C6C C1C C2C 118.3(6) . . ? C3C C2C C21C 117.4(6) . . ? C3C C2C C1C 119.1(6) . . ? C21C C2C C1C 123.5(6) . . ? N2C C21C C2C 126.8(6) . . ? C21C N2C C22C 117.0(5) . . ? C21C N2C Cu2 122.0(4) . . ? C22C N2C Cu2 120.9(4) . . ? C27C C22C C23C 119.1(6) . . ? C27C C22C N2C 118.9(6) . . ? C23C C22C N2C 122.0(6) . . ? C24C C23C C22C 120.0(7) . . ? C25C C24C C23C 119.4(7) . . ? C26C C25C C24C 120.4(7) . . ? C25C C26C C27C 121.1(7) . . ? C26C C27C C22C 119.9(7) . . ? C4C C3C C2C 123.6(6) . . ? C3C C4C C5C 116.1(6) . . ? C3C C4C C41C 124.4(7) . . ? C5C C4C C41C 119.3(7) . . ? C42C C41C C44C 113.8(9) . . ? C42C C41C C4C 113.2(8) . . ? C44C C41C C4C 110.7(7) . . ? C42C C41C C43C 100.8(11) . . ? C44C C41C C43C 106.5(10) . . ? C4C C41C C43C 111.3(7) . . ? C6C C5C C4C 122.4(7) . . ? C5C C6C C1C 120.4(6) . . ? C5C C6C C61C 121.9(6) . . ? C1C C6C C61C 117.6(6) . . ? C6C C61C N6C 110.1(5) . . ? C62C N6C C63C 109.7(6) . . ? C62C N6C C61C 112.8(6) . . ? C63C N6C C61C 111.4(5) . . ? C64C C63C N6C 112.1(7) . . ? C63C C64C C65C 114.7(9) . . ? C65A C65C C64C 115.2(10) . . ? O1D Cu2 O1C 170.1(2) . . ? O1D Cu2 N2D 92.64(19) . . ? O1C Cu2 N2D 91.7(2) . . ? O1D Cu2 N2C 92.71(19) . . ? O1C Cu2 N2C 91.2(2) . . ? N2D Cu2 N2C 130.36(19) . . ? O1D Cu2 O2S 97.8(3) . . ? O1C Cu2 O2S 72.4(3) . . ? N2D Cu2 O2S 112.4(3) . . ? N2C Cu2 O2S 115.6(3) . . ? O1D Cu2 O2S' 84.9(2) . . ? O1C Cu2 O2S' 85.9(3) . . ? N2D Cu2 O2S' 95.3(3) . . ? N2C Cu2 O2S' 134.3(3) . . ? O2S Cu2 O2S' 22.1(3) . . ? C1B O1B Cu1 127.1(4) . . ? O1B C1B C6B 119.7(6) . . ? O1B C1B C2B 124.5(6) . . ? C6B C1B C2B 115.7(6) . . ? C3B C2B C21B 116.6(6) . . ? C3B C2B C1B 119.9(6) . . ? C21B C2B C1B 123.5(5) . . ? N2B C21B C2B 126.8(6) . . ? C21B N2B C22B 116.5(5) . . ? C21B N2B Cu1 121.4(4) . . ? C22B N2B Cu1 121.5(4) . . ? C23B C22B C27B 122.0(7) . . ? C23B C22B N2B 121.8(6) . . ? C27B C22B N2B 116.1(7) . . ? C22B C23B C24B 117.6(9) . . ? C25B C24B C23B 121.3(11) . . ? C24B C25B C26B 120.4(10) . . ? C27B C26B C25B 119.9(11) . . ? C26B C27B C22B 118.3(10) . . ? C4B C3B C2B 122.5(7) . . ? C5B C4B C3B 117.8(7) . . ? C5B C4B C41B 123.5(7) . . ? C3B C4B C41B 118.7(7) . . ? C42' C41B C42B 135.0(15) . . ? C42' C41B C43B 56.7(12) . . ? C42B C41B C43B 112.8(10) . . ? C42' C41B C43' 118.5(14) . . ? C42B C41B C43' 43.0(9) . . ? C43B C41B C43' 146.0(13) . . ? C42' C41B C44' 111.6(14) . . ? C42B C41B C44' 65.4(11) . . ? C43B C41B C44' 56.4(11) . . ? C43' C41B C44' 108.4(12) . . ? C42' C41B C4B 112.8(13) . . ? C42B C41B C4B 111.7(10) . . ? C43B C41B C4B 110.2(9) . . ? C43' C41B C4B 102.4(11) . . ? C44' C41B C4B 101.6(14) . . ? C42' C41B C44B 45.5(11) . . ? C42B C41B C44B 110.8(10) . . ? C43B C41B C44B 100.8(9) . . ? C43' C41B C44B 76.0(10) . . ? C44' C41B C44B 146.4(14) . . ? C4B C41B C44B 110.1(8) . . ? C4B C5B C6B 121.5(7) . . ? C5B C6B C1B 122.5(6) . . ? C5B C6B C61B 121.4(6) . . ? C1B C6B C61B 116.0(6) . . ? N6B C61B C6B 111.4(5) . . ? C62B N6B C63B 110.4(7) . . ? C62B N6B C61B 113.8(7) . . ? C63B N6B C61B 110.3(6) . . ? C64B C63B N6B 112.4(7) . . ? C63B C64B C65B 115.2(11) . . ? C65D C65B C64B 113.4(10) . . ? C1D O1D Cu2 129.2(4) . . ? O1D C1D C2D 124.8(6) . . ? O1D C1D C6D 118.9(6) . . ? C2D C1D C6D 116.3(6) . . ? C3D C2D C1D 119.8(6) . . ? C3D C2D C21D 116.6(6) . . ? C1D C2D C21D 123.3(6) . . ? N2D C21D C2D 126.5(6) . . ? C21D N2D C22D 116.7(5) . . ? C21D N2D Cu2 122.0(4) . . ? C22D N2D Cu2 121.2(4) . . ? C27D C22D C23D 118.8(6) . . ? C27D C22D N2D 119.7(6) . . ? C23D C22D N2D 121.4(6) . . ? C22D C23D C24D 119.3(7) . . ? C25D C24D C23D 121.4(8) . . ? C24D C25D C26D 118.7(7) . . ? C27D C26D C25D 119.8(7) . . ? C26D C27D C22D 122.0(7) . . ? C4D C3D C2D 123.5(6) . . ? C3D C4D C5D 116.4(6) . . ? C3D C4D C41D 123.8(6) . . ? C5D C4D C41D 119.8(6) . . ? C42D C41D C43D 112.1(7) . . ? C42D C41D C44D 106.9(7) . . ? C43D C41D C44D 109.3(7) . . ? C42D C41D C4D 111.7(6) . . ? C43D C41D C4D 108.5(7) . . ? C44D C41D C4D 108.3(6) . . ? C6D C5D C4D 122.1(6) . . ? C5D C6D C1D 121.8(6) . . ? C5D C6D C61D 121.7(6) . . ? C1D C6D C61D 116.4(6) . . ? N6D C61D C6D 112.2(5) . . ? C61D N6D C63D 111.8(6) . . ? C61D N6D C62D 109.8(6) . . ? C63D N6D C62D 110.2(6) . . ? C64D C63D N6D 113.1(8) . . ? C63D C64D C65D 115.8(10) . . ? C65B C65D C64D 114.9(11) . . ? O4S S1 O2S' 131.6(5) . . ? O4S S1 O1S 114.7(4) . . ? O2S' S1 O1S 111.7(4) . . ? O4S S1 O3S' 65.9(6) . . ? O2S' S1 O3S' 109.1(6) . . ? O1S S1 O3S' 110.9(4) . . ? O4S S1 O4S' 42.8(5) . . ? O2S' S1 O4S' 111.5(6) . . ? O1S S1 O4S' 105.4(5) . . ? O3S' S1 O4S' 108.1(6) . . ? O4S S1 O2S 111.6(6) . . ? O2S' S1 O2S 34.7(4) . . ? O1S S1 O2S 111.9(4) . . ? O3S' S1 O2S 132.8(6) . . ? O4S' S1 O2S 78.7(6) . . ? O4S S1 O3S 113.5(6) . . ? O2S' S1 O3S 69.1(6) . . ? O1S S1 O3S 100.9(5) . . ? O3S' S1 O3S 49.1(5) . . ? O4S' S1 O3S 150.7(7) . . ? O2S S1 O3S 103.2(6) . . ? S1 O1S Cu1 117.9(3) . . ? S1 O2S Cu2 125.2(6) . . ? S1 O2S' Cu2 121.2(5) . . ? O7S S2 O5S 112.6(8) . . ? O7S S2 O6S 106.9(9) . . ? O5S S2 O6S 112.5(9) . . ? O7S S2 O8S 110.7(7) . . ? O5S S2 O8S 104.2(9) . . ? O6S S2 O8S 110.0(5) . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 25.62 _diffrn_measured_fraction_theta_full 0.935 _refine_diff_density_max 0.997 _refine_diff_density_min -0.606 _refine_diff_density_rms 0.092 #===END data_pgp532 _database_code_CSD 191880 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Cu2(C44H56O2N4)2(BF4)][BF4]3.1.5MeOH.1.5(Et2O).625H2O ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Cu2(C44H60N4O2)2(BF4)](BF4)3(CH3OH)1.5(CH3CH2OCH2CH3)1.5(H2O)0.625' _chemical_formula_sum 'C95.50 H134 B4 Cu2 F16 N8 O7.63' _chemical_formula_weight 1990.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.636(3) _cell_length_b 18.598(4) _cell_length_c 22.746(5) _cell_angle_alpha 90.040(3) _cell_angle_beta 106.749(3) _cell_angle_gamma 101.869(3) _cell_volume 5394(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6796 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26.5 _exptl_crystal_description block _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.225 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2092 _exptl_absorpt_coefficient_mu 0.474 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_correction_T_min 0.684 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details SADabs _exptl_special_details ; Acta Checks: 063_ALERT A Crystal Probably too Large for Beam Size ..... 1.05 mm Cutting the crystals led to shattering. 223_ALERT A Large Solvent/Anion H Ueq(max)/Ueq(min) . 5.50 Ratio This structure exhibits high thermal motion owing to the flexible nature of the ligand and symmetrical anion. 430_ALERT A Short Inter D...A Contact:2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1559P)^2^+26.3841P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21671 _refine_ls_number_parameters 1216 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1437 _refine_ls_R_factor_gt 0.1059 _refine_ls_wR_factor_ref 0.3280 _refine_ls_wR_factor_gt 0.3075 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.41176(7) 0.07598(5) 0.13945(4) 0.0316(2) Uani 1 1 d . . . C1A C 0.2803(6) 0.1683(4) 0.0674(3) 0.0326(15) Uani 1 1 d . . . O1A O 0.2983(4) 0.1238(3) 0.1131(2) 0.0350(11) Uani 1 1 d . . . C2A C 0.3465(6) 0.1874(4) 0.0291(3) 0.0348(16) Uani 1 1 d . . . C21A C 0.4357(6) 0.1563(4) 0.0321(3) 0.0325(15) Uani 1 1 d . . . H21A H 0.4725 0.1714 0.0029 0.039 Uiso 1 1 calc R . . N2A N 0.4715(5) 0.1090(3) 0.0713(2) 0.0331(13) Uani 1 1 d . . . C22A C 0.5637(6) 0.0859(4) 0.0651(3) 0.0322(15) Uani 1 1 d . . . C23A C 0.5702(7) 0.0126(4) 0.0759(3) 0.0429(18) Uani 1 1 d . . . H23A H 0.5151 -0.0200 0.0864 0.051 Uiso 1 1 calc R . . C24A C 0.6566(8) -0.0124(5) 0.0715(4) 0.055(2) Uani 1 1 d . . . H24A H 0.6604 -0.0622 0.0788 0.065 Uiso 1 1 calc R . . C25A C 0.7375(9) 0.0340(6) 0.0565(4) 0.063(3) Uani 1 1 d . . . H25A H 0.7972 0.0167 0.0542 0.076 Uiso 1 1 calc R . . C26A C 0.7306(7) 0.1071(6) 0.0447(4) 0.054(2) Uani 1 1 d . . . H26A H 0.7847 0.1390 0.0330 0.065 Uiso 1 1 calc R . . C27A C 0.6455(7) 0.1327(5) 0.0502(3) 0.0454(19) Uani 1 1 d . . . H27A H 0.6427 0.1828 0.0438 0.055 Uiso 1 1 calc R . . C3A C 0.3200(6) 0.2368(4) -0.0180(3) 0.0334(15) Uani 1 1 d . . . H3A H 0.3638 0.2486 -0.0439 0.040 Uiso 1 1 calc R . . C4A C 0.2329(6) 0.2686(4) -0.0278(3) 0.0395(17) Uani 1 1 d . . . C41A C 0.2056(7) 0.3230(5) -0.0776(3) 0.0441(19) Uani 1 1 d . . . C42A C 0.1004(7) 0.2878(5) -0.1247(4) 0.050(2) Uani 1 1 d . . . H42A H 0.0811 0.3225 -0.1562 0.075 Uiso 1 1 calc R . . H42B H 0.0460 0.2757 -0.1039 0.075 Uiso 1 1 calc R . . H42C H 0.1071 0.2427 -0.1442 0.075 Uiso 1 1 calc R . . C43A C 0.2897(7) 0.3447(5) -0.1102(4) 0.052(2) Uani 1 1 d . . . H43A H 0.3567 0.3671 -0.0800 0.077 Uiso 1 1 calc R . . H43B H 0.2692 0.3803 -0.1407 0.077 Uiso 1 1 calc R . . H43C H 0.2973 0.3009 -0.1310 0.077 Uiso 1 1 calc R . . C44A C 0.1920(8) 0.3950(5) -0.0480(4) 0.056(2) Uani 1 1 d . . . H44A H 0.2570 0.4171 -0.0160 0.083 Uiso 1 1 calc R . . H44B H 0.1343 0.3830 -0.0296 0.083 Uiso 1 1 calc R . . H44C H 0.1762 0.4300 -0.0798 0.083 Uiso 1 1 calc R . . C5A C 0.1673(6) 0.2468(4) 0.0096(3) 0.0392(17) Uani 1 1 d . . . H5A H 0.1057 0.2657 0.0030 0.047 Uiso 1 1 calc R . . C6A C 0.1896(6) 0.1982(4) 0.0560(3) 0.0353(16) Uani 1 1 d . . . C61A C 0.1214(6) 0.1785(4) 0.0981(3) 0.0367(16) Uani 1 1 d . . . H61A H 0.1036 0.1243 0.1001 0.044 Uiso 1 1 calc R . . H61B H 0.0554 0.1958 0.0819 0.044 Uiso 1 1 calc R . . N6A N 0.1806(5) 0.2146(3) 0.1623(3) 0.0341(13) Uani 1 1 d . . . H6A H 0.2494 0.2088 0.1710 0.041 Uiso 1 1 calc R . . C62A C 0.1838(8) 0.2956(5) 0.1634(4) 0.050(2) Uani 1 1 d . . . H62A H 0.1145 0.3038 0.1622 0.075 Uiso 1 1 calc R . . H62B H 0.2031 0.3161 0.1277 0.075 Uiso 1 1 calc R . . H62C H 0.2357 0.3197 0.2012 0.075 Uiso 1 1 calc R . . C63A C 0.1363(6) 0.1780(4) 0.2111(3) 0.0391(17) Uani 1 1 d . . . H63A H 0.0658 0.1880 0.2056 0.047 Uiso 1 1 calc R . . H63B H 0.1284 0.1240 0.2059 0.047 Uiso 1 1 calc R . . C64A C 0.2053(6) 0.2048(4) 0.2753(3) 0.0369(16) Uani 1 1 d . . . H64A H 0.2000 0.2558 0.2841 0.044 Uiso 1 1 calc R . . H64B H 0.2792 0.2053 0.2780 0.044 Uiso 1 1 calc R . . C65A C 0.1724(6) 0.1549(4) 0.3232(3) 0.0389(17) Uani 1 1 d . . . H65A H 0.1892 0.1063 0.3185 0.047 Uiso 1 1 calc R . . H65B H 0.0955 0.1471 0.3151 0.047 Uiso 1 1 calc R . . C1B C 0.5609(5) 0.0180(3) 0.2367(3) 0.0271(13) Uani 1 1 d . . . O1B O 0.5429(4) 0.0615(3) 0.1906(2) 0.0339(11) Uani 1 1 d . . . C2B C 0.4809(5) -0.0292(4) 0.2565(3) 0.0265(13) Uani 1 1 d . . . C21B C 0.3705(5) -0.0357(4) 0.2257(3) 0.0309(14) Uani 1 1 d . . . H21B H 0.3227 -0.0687 0.2416 0.037 Uiso 1 1 calc R . . N2B N 0.3303(4) -0.0009(3) 0.1783(2) 0.0302(12) Uani 1 1 d . . . C22B C 0.2166(6) -0.0183(4) 0.1547(3) 0.0386(17) Uani 1 1 d . . . C23B C 0.1708(7) -0.0370(5) 0.0915(4) 0.048(2) Uani 1 1 d . . . H23B H 0.2140 -0.0363 0.0652 0.057 Uiso 1 1 calc R . . C24B C 0.0622(8) -0.0564(5) 0.0671(5) 0.066(3) Uani 1 1 d . . . H24B H 0.0315 -0.0701 0.0245 0.079 Uiso 1 1 calc R . . C25B C -0.0015(7) -0.0557(6) 0.1052(6) 0.069(3) Uani 1 1 d . . . H25B H -0.0757 -0.0693 0.0890 0.083 Uiso 1 1 calc R . . C26B C 0.0458(7) -0.0346(6) 0.1682(5) 0.062(3) Uani 1 1 d . . . H26B H 0.0029 -0.0318 0.1941 0.075 Uiso 1 1 calc R . . C27B C 0.1526(6) -0.0182(5) 0.1927(4) 0.048(2) Uani 1 1 d . . . H27B H 0.1832 -0.0068 0.2356 0.058 Uiso 1 1 calc R . . C3B C 0.5104(5) -0.0733(4) 0.3074(3) 0.0276(13) Uani 1 1 d . . . H3B H 0.4571 -0.1049 0.3200 0.033 Uiso 1 1 calc R . . C4B C 0.6140(6) -0.0714(4) 0.3387(3) 0.0315(15) Uani 1 1 d . . . C41B C 0.6487(6) -0.1178(4) 0.3944(3) 0.0399(17) Uani 1 1 d . . . C42B C 0.7128(9) -0.1702(6) 0.3775(5) 0.064(3) Uani 1 1 d . . . H42D H 0.7753 -0.1411 0.3691 0.096 Uiso 1 1 calc R . . H42E H 0.6694 -0.2017 0.3408 0.096 Uiso 1 1 calc R . . H42F H 0.7340 -0.2010 0.4118 0.096 Uiso 1 1 calc R . . C43B C 0.5535(7) -0.1633(5) 0.4110(4) 0.052(2) Uani 1 1 d . . . H43D H 0.5779 -0.1906 0.4472 0.078 Uiso 1 1 calc R . . H43E H 0.5105 -0.1980 0.3762 0.078 Uiso 1 1 calc R . . H43F H 0.5115 -0.1302 0.4199 0.078 Uiso 1 1 calc R . . C44B C 0.7182(8) -0.0680(6) 0.4503(4) 0.062(3) Uani 1 1 d . . . H44D H 0.6790 -0.0340 0.4610 0.094 Uiso 1 1 calc R . . H44E H 0.7803 -0.0398 0.4407 0.094 Uiso 1 1 calc R . . H44F H 0.7402 -0.0980 0.4850 0.094 Uiso 1 1 calc R . . C5B C 0.6912(5) -0.0253(4) 0.3186(3) 0.0333(15) Uani 1 1 d . . . H5B H 0.7628 -0.0235 0.3398 0.040 Uiso 1 1 calc R . . C6B C 0.6674(5) 0.0177(4) 0.2691(3) 0.0295(14) Uani 1 1 d . . . C61B C 0.7510(6) 0.0664(4) 0.2463(3) 0.0372(16) Uani 1 1 d . . . H61C H 0.8213 0.0627 0.2728 0.045 Uiso 1 1 calc R . . H61D H 0.7443 0.0490 0.2038 0.045 Uiso 1 1 calc R . . N6B N 0.7407(5) 0.1449(3) 0.2470(3) 0.0336(13) Uani 1 1 d . . . H6B H 0.6709 0.1450 0.2270 0.040 Uiso 1 1 calc R . . C62B C 0.7639(7) 0.1781(5) 0.3100(4) 0.047(2) Uani 1 1 d . . . H62D H 0.7268 0.1444 0.3335 0.071 Uiso 1 1 calc R . . H62E H 0.7407 0.2248 0.3078 0.071 Uiso 1 1 calc R . . H62F H 0.8396 0.1871 0.3304 0.071 Uiso 1 1 calc R . . C63B C 0.8056(6) 0.1912(4) 0.2109(3) 0.0388(17) Uani 1 1 d . . . H63C H 0.7927 0.1657 0.1702 0.047 Uiso 1 1 calc R . . H63D H 0.8811 0.1979 0.2333 0.047 Uiso 1 1 calc R . . C64B C 0.7759(6) 0.2657(4) 0.2022(4) 0.0430(18) Uani 1 1 d . . . H64C H 0.8077 0.2960 0.2415 0.052 Uiso 1 1 calc R . . H64D H 0.6988 0.2583 0.1926 0.052 Uiso 1 1 calc R . . C65B C 0.8103(6) 0.3086(4) 0.1512(4) 0.0422(18) Uani 1 1 d . . . H65C H 0.7753 0.2803 0.1111 0.051 Uiso 1 1 calc R . . H65D H 0.8870 0.3148 0.1594 0.051 Uiso 1 1 calc R . . Cu2 Cu 0.56946(6) 0.40519(4) 0.34794(3) 0.0252(2) Uani 1 1 d . . . C1C C 0.6844(5) 0.3043(4) 0.4203(3) 0.0239(13) Uani 1 1 d . . . O1C O 0.5932(3) 0.3228(2) 0.39583(19) 0.0261(9) Uani 1 1 d . . . C2C C 0.7802(5) 0.3403(4) 0.4113(3) 0.0311(15) Uani 1 1 d . . . C21C C 0.7928(5) 0.4068(4) 0.3798(3) 0.0293(14) Uani 1 1 d . . . H21C H 0.8617 0.4271 0.3779 0.035 Uiso 1 1 calc R . . N2C N 0.7207(4) 0.4425(3) 0.3535(2) 0.0277(12) Uani 1 1 d . . . C22C C 0.7552(5) 0.5104(4) 0.3281(3) 0.0293(14) Uani 1 1 d . . . C23C C 0.8299(5) 0.5185(4) 0.2962(3) 0.0351(15) Uani 1 1 d . . . H23C H 0.8589 0.4779 0.2897 0.042 Uiso 1 1 calc R . . C24C C 0.8619(6) 0.5866(4) 0.2738(4) 0.0423(18) Uani 1 1 d . . . H24C H 0.9140 0.5925 0.2530 0.051 Uiso 1 1 calc R . . C25C C 0.8183(7) 0.6459(5) 0.2817(4) 0.050(2) Uani 1 1 d . . . H25C H 0.8399 0.6919 0.2662 0.060 Uiso 1 1 calc R . . C26C C 0.7433(7) 0.6370(4) 0.3123(4) 0.049(2) Uani 1 1 d . . . H26C H 0.7132 0.6774 0.3177 0.059 Uiso 1 1 calc R . . C27C C 0.7108(6) 0.5697(4) 0.3355(3) 0.0369(16) Uani 1 1 d . . . H27C H 0.6587 0.5644 0.3563 0.044 Uiso 1 1 calc R . . C3C C 0.8734(6) 0.3136(4) 0.4394(3) 0.0395(17) Uani 1 1 d . . . H3C H 0.9373 0.3378 0.4326 0.047 Uiso 1 1 calc R . . C4C C 0.8743(5) 0.2548(4) 0.4755(3) 0.0386(17) Uani 1 1 d . . . C41C C 0.9752(6) 0.2278(6) 0.5080(4) 0.056(2) Uani 1 1 d . . . C42C C 1.0716(7) 0.2744(8) 0.4937(6) 0.101(5) Uani 1 1 d . . . H42G H 1.0637 0.2681 0.4497 0.152 Uiso 1 1 calc R . . H42H H 1.1348 0.2584 0.5175 0.152 Uiso 1 1 calc R . . H42I H 1.0778 0.3264 0.5049 0.152 Uiso 1 1 calc R . . C43C C 0.9932(8) 0.2363(7) 0.5793(5) 0.074(3) Uani 1 1 d . . . H43G H 1.0100 0.2887 0.5926 0.110 Uiso 1 1 calc R . . H43H H 1.0515 0.2137 0.6009 0.110 Uiso 1 1 calc R . . H43I H 0.9294 0.2118 0.5890 0.110 Uiso 1 1 calc R . . C44C C 0.9611(9) 0.1483(7) 0.4888(6) 0.086(4) Uani 1 1 d . . . H44G H 0.9033 0.1188 0.5016 0.128 Uiso 1 1 calc R . . H44H H 1.0258 0.1315 0.5083 0.128 Uiso 1 1 calc R . . H44I H 0.9450 0.1426 0.4440 0.128 Uiso 1 1 calc R . . C5C C 0.7778(6) 0.2198(4) 0.4846(3) 0.0380(17) Uani 1 1 d . . . H5C H 0.7764 0.1795 0.5102 0.046 Uiso 1 1 calc R . . C6C C 0.6842(5) 0.2426(4) 0.4571(3) 0.0306(14) Uani 1 1 d . . . C61C C 0.5822(5) 0.2045(4) 0.4670(3) 0.0302(14) Uani 1 1 d . . . H61E H 0.5483 0.2413 0.4802 0.036 Uiso 1 1 calc R . . H61F H 0.5956 0.1698 0.4999 0.036 Uiso 1 1 calc R . . N6C N 0.5099(4) 0.1629(3) 0.4077(2) 0.0306(12) Uani 1 1 d . . . H6C H 0.5137 0.1935 0.3758 0.037 Uiso 1 1 calc R . . C62C C 0.5473(7) 0.0951(4) 0.3953(4) 0.048(2) Uani 1 1 d . . . H62G H 0.6222 0.1086 0.3988 0.071 Uiso 1 1 calc R . . H62H H 0.5080 0.0737 0.3537 0.071 Uiso 1 1 calc R . . H62I H 0.5360 0.0590 0.4254 0.071 Uiso 1 1 calc R . . C63C C 0.3966(5) 0.1411(4) 0.4062(3) 0.0335(15) Uani 1 1 d . . . H63E H 0.3912 0.1122 0.4422 0.040 Uiso 1 1 calc R . . H63F H 0.3566 0.1092 0.3686 0.040 Uiso 1 1 calc R . . C64C C 0.3476(6) 0.2079(4) 0.4073(3) 0.0345(15) Uani 1 1 d . . . H64E H 0.3685 0.2430 0.3782 0.041 Uiso 1 1 calc R . . H64F H 0.3756 0.2330 0.4490 0.041 Uiso 1 1 calc R . . C65C C 0.2276(6) 0.1874(5) 0.3902(3) 0.0401(17) Uani 1 1 d . . . H65E H 0.2018 0.2320 0.3963 0.048 Uiso 1 1 calc R . . H65F H 0.2072 0.1511 0.4186 0.048 Uiso 1 1 calc R . . C1D C 0.4290(5) 0.4666(4) 0.2495(3) 0.0259(13) Uani 1 1 d . . . O1D O 0.5217(3) 0.4499(3) 0.2731(2) 0.0291(10) Uani 1 1 d . . . C2D C 0.3508(5) 0.4611(3) 0.2806(3) 0.0263(13) Uani 1 1 d . . . C21D C 0.3682(5) 0.4409(3) 0.3436(3) 0.0254(13) Uani 1 1 d . . . H21D H 0.3143 0.4435 0.3617 0.030 Uiso 1 1 calc R . . N2D N 0.4503(4) 0.4195(3) 0.3781(2) 0.0230(10) Uani 1 1 d . . . C22D C 0.4533(5) 0.4064(3) 0.4414(3) 0.0259(13) Uani 1 1 d . . . C23D C 0.3633(5) 0.3810(4) 0.4595(3) 0.0330(15) Uani 1 1 d . . . H23D H 0.2963 0.3712 0.4296 0.040 Uiso 1 1 calc R . . C24D C 0.3717(6) 0.3700(4) 0.5214(3) 0.0382(16) Uani 1 1 d . . . H24D H 0.3102 0.3531 0.5335 0.046 Uiso 1 1 calc R . . C25D C 0.4708(6) 0.3838(4) 0.5658(3) 0.0410(17) Uani 1 1 d . . . H25D H 0.4765 0.3764 0.6079 0.049 Uiso 1 1 calc R . . C26D C 0.5593(6) 0.4083(4) 0.5475(3) 0.0391(17) Uani 1 1 d . . . H26D H 0.6264 0.4167 0.5772 0.047 Uiso 1 1 calc R . . C27D C 0.5518(5) 0.4207(4) 0.4864(3) 0.0311(14) Uani 1 1 d . . . H27D H 0.6135 0.4391 0.4749 0.037 Uiso 1 1 calc R . . C3D C 0.2514(5) 0.4775(4) 0.2496(3) 0.0291(14) Uani 1 1 d . . . H3D H 0.1994 0.4724 0.2704 0.035 Uiso 1 1 calc R . . C4D C 0.2287(5) 0.5004(4) 0.1905(3) 0.0333(15) Uani 1 1 d . . . C41D C 0.1217(6) 0.5185(4) 0.1560(3) 0.0388(17) Uani 1 1 d . . . C42D C 0.0491(6) 0.5146(6) 0.1976(4) 0.055(2) Uani 1 1 d . . . H42J H 0.0790 0.5541 0.2303 0.083 Uiso 1 1 calc R . . H42K H 0.0428 0.4668 0.2160 0.083 Uiso 1 1 calc R . . H42L H -0.0204 0.5204 0.1730 0.083 Uiso 1 1 calc R . . C43D C 0.1390(7) 0.5969(5) 0.1338(5) 0.062(3) Uani 1 1 d . . . H43J H 0.0712 0.6079 0.1117 0.093 Uiso 1 1 calc R . . H43K H 0.1832 0.6005 0.1063 0.093 Uiso 1 1 calc R . . H43L H 0.1737 0.6322 0.1694 0.093 Uiso 1 1 calc R . . C44D C 0.0675(8) 0.4637(7) 0.0997(5) 0.081(4) Uani 1 1 d . . . H44J H 0.0605 0.4133 0.1131 0.121 Uiso 1 1 calc R . . H44K H 0.1095 0.4700 0.0709 0.121 Uiso 1 1 calc R . . H44L H -0.0023 0.4728 0.0793 0.121 Uiso 1 1 calc R . . C5D C 0.3076(6) 0.5087(4) 0.1617(3) 0.0360(16) Uani 1 1 d . . . H5D H 0.2933 0.5250 0.1212 0.043 Uiso 1 1 calc R . . C6D C 0.4062(5) 0.4942(4) 0.1893(3) 0.0325(15) Uani 1 1 d . . . C61D C 0.4924(6) 0.5063(4) 0.1594(3) 0.0384(17) Uani 1 1 d . . . H61G H 0.5544 0.5413 0.1857 0.046 Uiso 1 1 calc R . . H61H H 0.4689 0.5280 0.1193 0.046 Uiso 1 1 calc R . . N6D N 0.5216(5) 0.4346(3) 0.1495(3) 0.0362(14) Uani 1 1 d . . . H6D H 0.5275 0.4111 0.1860 0.043 Uiso 1 1 calc R . . C62D C 0.4380(7) 0.3847(5) 0.1007(4) 0.055(2) Uani 1 1 d . . . H62J H 0.3702 0.3813 0.1086 0.082 Uiso 1 1 calc R . . H62K H 0.4540 0.3357 0.1012 0.082 Uiso 1 1 calc R . . H62L H 0.4349 0.4045 0.0605 0.082 Uiso 1 1 calc R . . C63D C 0.6283(6) 0.4466(5) 0.1386(3) 0.0418(18) Uani 1 1 d . . . H63G H 0.6236 0.4654 0.0974 0.050 Uiso 1 1 calc R . . H63H H 0.6792 0.4839 0.1697 0.050 Uiso 1 1 calc R . . C64D C 0.6650(6) 0.3765(5) 0.1428(4) 0.0457(19) Uani 1 1 d . . . H64G H 0.6229 0.3439 0.1059 0.055 Uiso 1 1 calc R . . H64H H 0.6516 0.3519 0.1791 0.055 Uiso 1 1 calc R . . C65D C 0.7818(6) 0.3850(5) 0.1479(4) 0.0429(18) Uani 1 1 d . . . H65G H 0.8252 0.4163 0.1853 0.051 Uiso 1 1 calc R . . H65H H 0.7966 0.4093 0.1117 0.051 Uiso 1 1 calc R . . B1 B 0.4910(7) 0.2437(5) 0.2365(4) 0.0382(18) Uani 1 1 d . . . F1 F 0.5169(4) 0.2103(3) 0.1891(2) 0.0560(13) Uani 1 1 d . . . F2 F 0.5779(4) 0.3043(3) 0.2634(2) 0.0613(14) Uani 1 1 d . . . F3 F 0.4772(6) 0.1950(3) 0.2797(3) 0.0802(18) Uani 1 1 d . . . F4 F 0.4039(5) 0.2718(3) 0.2114(3) 0.0748(16) Uani 1 1 d . . . B2 B 0.0393(7) 0.3341(6) 0.3110(4) 0.043(2) Uani 1 1 d . . . F5 F 0.0434(4) 0.3255(4) 0.2513(3) 0.0696(16) Uani 1 1 d . . . F6 F 0.1393(4) 0.3634(3) 0.3491(3) 0.0742(17) Uani 1 1 d . . . F7 F 0.0039(4) 0.2658(3) 0.3306(3) 0.0711(16) Uani 1 1 d . . . F8 F -0.0278(4) 0.3801(3) 0.3131(3) 0.0706(16) Uani 1 1 d . . . B3 B 0.6993(8) 0.0662(5) 0.5995(5) 0.047(2) Uani 1 1 d . . . F9 F 0.7077(5) 0.0263(3) 0.6518(2) 0.0679(15) Uani 1 1 d . . . F10 F 0.6037(5) 0.0388(3) 0.5548(3) 0.0720(16) Uani 1 1 d . . . F11 F 0.7021(7) 0.1381(3) 0.6125(4) 0.110(3) Uani 1 1 d . . . F12 F 0.7783(5) 0.0645(5) 0.5749(3) 0.107(3) Uani 1 1 d . . . B4 B 0.3910(11) 0.6349(7) 0.0320(5) 0.063(3) Uani 1 1 d . . . F13 F 0.4041(6) 0.6987(3) 0.0006(3) 0.086(2) Uani 1 1 d . . . F14 F 0.4440(6) 0.5865(4) 0.0151(3) 0.090(2) Uani 1 1 d . . . F15 F 0.4305(7) 0.6526(4) 0.0945(3) 0.099(2) Uani 1 1 d . . . F16 F 0.2869(7) 0.6021(6) 0.0177(4) 0.126(3) Uani 1 1 d . . . C1H C 0.7744(11) -0.1271(9) 0.2021(7) 0.110(5) Uani 1 1 d . . . H1HA H 0.7512 -0.1748 0.1786 0.165 Uiso 1 1 calc R . . H1HB H 0.7904 -0.0881 0.1751 0.165 Uiso 1 1 calc R . . H1HC H 0.7185 -0.1178 0.2183 0.165 Uiso 1 1 calc R . . C2H C 0.8739(11) -0.1277(7) 0.2561(6) 0.087(4) Uani 1 1 d . . . H2HA H 0.8588 -0.1680 0.2828 0.104 Uiso 1 1 calc R . . H2HB H 0.9309 -0.1362 0.2400 0.104 Uiso 1 1 calc R . . O3H O 0.9052(5) -0.0598(4) 0.2905(3) 0.0679(18) Uani 1 1 d . . . C4H C 1.0012(9) -0.0519(7) 0.3381(6) 0.076(3) Uani 1 1 d . . . H4HA H 1.0603 -0.0395 0.3203 0.092 Uiso 1 1 calc R . . H4HB H 1.0044 -0.0992 0.3577 0.092 Uiso 1 1 calc R . . C5H C 1.0122(8) 0.0066(6) 0.3855(6) 0.073(3) Uani 1 1 d . . . H5HA H 1.0792 0.0107 0.4176 0.109 Uiso 1 1 calc R . . H5HB H 0.9545 -0.0061 0.4038 0.109 Uiso 1 1 calc R . . H5HC H 1.0101 0.0537 0.3664 0.109 Uiso 1 1 calc R . . C1J C 0.8694(15) 0.2133(11) 0.7396(9) 0.060(5) Uiso 0.50 1 d P . . H1JA H 0.9271 0.2163 0.7215 0.090 Uiso 0.50 1 calc PR . . H1JB H 0.8252 0.1636 0.7313 0.090 Uiso 0.50 1 calc PR . . H1JC H 0.8980 0.2245 0.7841 0.090 Uiso 0.50 1 calc PR . . C2J C 0.8045(16) 0.2684(11) 0.7116(10) 0.063(5) Uiso 0.50 1 d P . . H2JA H 0.8485 0.3189 0.7196 0.076 Uiso 0.50 1 calc PR . . H2JB H 0.7757 0.2579 0.6665 0.076 Uiso 0.50 1 calc PR . . O3J O 0.7220(9) 0.2626(7) 0.7385(5) 0.052(3) Uiso 0.50 1 d P . . C4J C 0.6546(14) 0.3114(10) 0.7149(9) 0.055(4) Uiso 0.50 1 d P . . H4JA H 0.6219 0.2996 0.6702 0.066 Uiso 0.50 1 calc PR . . H4JB H 0.6966 0.3625 0.7208 0.066 Uiso 0.50 1 calc PR . . C5J C 0.5714(15) 0.3069(10) 0.7451(9) 0.056(4) Uiso 0.50 1 d P . . H5JA H 0.5276 0.3418 0.7278 0.084 Uiso 0.50 1 calc PR . . H5JB H 0.6034 0.3190 0.7894 0.084 Uiso 0.50 1 calc PR . . H5JC H 0.5281 0.2568 0.7383 0.084 Uiso 0.50 1 calc PR . . O1M O 0.9046(7) 0.2240(5) -0.0207(4) 0.093(3) Uani 1 1 d . . . C1M C 0.8897(9) 0.2860(6) 0.0037(5) 0.072(3) Uiso 1 1 d . . . H1M1 H 0.9057 0.2838 0.0484 0.108 Uiso 1 1 calc R . . H1M2 H 0.8166 0.2900 -0.0138 0.108 Uiso 1 1 calc R . . H1M3 H 0.9361 0.3290 -0.0059 0.108 Uiso 1 1 calc R . . O2M O 0.7516(10) 0.2000(6) -0.1396(5) 0.050(3) Uani 0.50 1 d PD . . C2M C 0.6530(16) 0.1856(14) -0.1237(12) 0.085(7) Uiso 0.50 1 d PD . . O1W O 0.874(2) 0.4420(16) 0.5771(13) 0.069(7) Uiso 0.25 1 d P A 1 O2W O 0.879(3) 0.494(2) 0.5472(16) 0.088(9) Uiso 0.25 1 d P B 2 O3W O 1.0000 0.5000 0.5000 0.059(9) Uiso 0.25 2 d SP . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0388(5) 0.0337(5) 0.0235(4) 0.0106(3) 0.0083(3) 0.0115(4) C1A 0.042(4) 0.029(4) 0.027(3) 0.008(3) 0.009(3) 0.010(3) O1A 0.048(3) 0.036(3) 0.026(2) 0.017(2) 0.013(2) 0.016(2) C2A 0.048(4) 0.030(4) 0.028(3) 0.005(3) 0.010(3) 0.013(3) C21A 0.046(4) 0.037(4) 0.017(3) 0.002(3) 0.010(3) 0.012(3) N2A 0.048(4) 0.031(3) 0.022(3) 0.006(2) 0.010(2) 0.013(3) C22A 0.045(4) 0.037(4) 0.019(3) 0.007(3) 0.011(3) 0.015(3) C23A 0.063(5) 0.043(4) 0.023(3) 0.003(3) 0.006(3) 0.021(4) C24A 0.085(7) 0.053(5) 0.028(4) 0.001(4) 0.004(4) 0.038(5) C25A 0.072(7) 0.077(7) 0.056(6) 0.007(5) 0.021(5) 0.045(6) C26A 0.059(5) 0.073(6) 0.044(5) 0.014(4) 0.027(4) 0.028(5) C27A 0.056(5) 0.051(5) 0.029(4) 0.008(3) 0.010(3) 0.015(4) C3A 0.045(4) 0.034(4) 0.024(3) 0.008(3) 0.013(3) 0.011(3) C4A 0.056(5) 0.038(4) 0.029(4) 0.009(3) 0.011(3) 0.021(4) C41A 0.061(5) 0.049(5) 0.028(4) 0.019(3) 0.013(3) 0.027(4) C42A 0.062(5) 0.056(5) 0.030(4) 0.017(4) 0.004(4) 0.020(4) C43A 0.055(5) 0.046(5) 0.054(5) 0.029(4) 0.016(4) 0.014(4) C44A 0.088(7) 0.042(5) 0.039(4) 0.012(4) 0.010(4) 0.032(5) C5A 0.044(4) 0.037(4) 0.039(4) 0.009(3) 0.010(3) 0.018(3) C6A 0.046(4) 0.042(4) 0.019(3) 0.007(3) 0.009(3) 0.013(3) C61A 0.034(4) 0.042(4) 0.033(4) 0.007(3) 0.006(3) 0.013(3) N6A 0.032(3) 0.042(3) 0.033(3) 0.009(3) 0.014(2) 0.012(3) C62A 0.070(6) 0.045(5) 0.045(5) 0.009(4) 0.027(4) 0.020(4) C63A 0.039(4) 0.040(4) 0.043(4) 0.019(3) 0.015(3) 0.013(3) C64A 0.038(4) 0.045(4) 0.030(4) 0.008(3) 0.013(3) 0.010(3) C65A 0.031(4) 0.048(4) 0.038(4) 0.015(3) 0.012(3) 0.006(3) C1B 0.039(4) 0.023(3) 0.022(3) 0.007(2) 0.013(3) 0.008(3) O1B 0.034(3) 0.038(3) 0.030(2) 0.014(2) 0.009(2) 0.008(2) C2B 0.029(3) 0.031(3) 0.015(3) 0.001(2) 0.000(2) 0.006(3) C21B 0.035(4) 0.031(4) 0.029(3) 0.009(3) 0.011(3) 0.011(3) N2B 0.031(3) 0.031(3) 0.027(3) 0.005(2) 0.004(2) 0.010(2) C22B 0.041(4) 0.036(4) 0.041(4) 0.014(3) 0.008(3) 0.017(3) C23B 0.045(5) 0.056(5) 0.043(4) 0.003(4) 0.006(4) 0.022(4) C24B 0.060(6) 0.055(6) 0.064(6) 0.005(5) -0.017(5) 0.021(5) C25B 0.035(5) 0.070(7) 0.101(8) 0.034(6) 0.010(5) 0.021(4) C26B 0.044(5) 0.082(7) 0.069(6) 0.035(5) 0.020(5) 0.026(5) C27B 0.044(5) 0.057(5) 0.052(5) 0.028(4) 0.019(4) 0.021(4) C3B 0.035(4) 0.025(3) 0.023(3) 0.006(3) 0.010(3) 0.006(3) C4B 0.040(4) 0.031(4) 0.032(3) 0.010(3) 0.017(3) 0.017(3) C41B 0.037(4) 0.051(5) 0.037(4) 0.018(3) 0.012(3) 0.019(3) C42B 0.085(7) 0.067(6) 0.063(6) 0.035(5) 0.033(5) 0.052(6) C43B 0.054(5) 0.057(5) 0.053(5) 0.041(4) 0.023(4) 0.021(4) C44B 0.074(7) 0.071(6) 0.034(4) 0.021(4) 0.007(4) 0.010(5) C5B 0.025(3) 0.046(4) 0.028(3) 0.004(3) 0.005(3) 0.010(3) C6B 0.028(3) 0.037(4) 0.026(3) 0.008(3) 0.011(3) 0.009(3) C61B 0.040(4) 0.042(4) 0.033(4) 0.012(3) 0.015(3) 0.011(3) N6B 0.030(3) 0.040(3) 0.030(3) 0.008(3) 0.010(2) 0.004(3) C62B 0.058(5) 0.049(5) 0.036(4) 0.004(3) 0.025(4) -0.001(4) C63B 0.037(4) 0.047(4) 0.035(4) 0.010(3) 0.017(3) 0.003(3) C64B 0.038(4) 0.049(5) 0.049(5) 0.016(4) 0.021(4) 0.010(3) C65B 0.044(4) 0.046(5) 0.041(4) 0.015(3) 0.020(3) 0.009(4) Cu2 0.0194(4) 0.0336(4) 0.0250(4) 0.0086(3) 0.0075(3) 0.0097(3) C1C 0.018(3) 0.034(3) 0.022(3) 0.005(3) 0.008(2) 0.010(3) O1C 0.025(2) 0.032(2) 0.023(2) 0.0086(18) 0.0073(18) 0.0081(18) C2C 0.018(3) 0.047(4) 0.031(3) 0.013(3) 0.005(3) 0.016(3) C21C 0.018(3) 0.042(4) 0.029(3) 0.008(3) 0.010(3) 0.004(3) N2C 0.020(3) 0.035(3) 0.030(3) 0.010(2) 0.008(2) 0.010(2) C22C 0.022(3) 0.036(4) 0.025(3) 0.002(3) 0.001(3) 0.004(3) C23C 0.031(4) 0.038(4) 0.041(4) 0.013(3) 0.015(3) 0.013(3) C24C 0.046(4) 0.043(4) 0.043(4) 0.014(3) 0.021(4) 0.010(4) C25C 0.058(5) 0.039(4) 0.049(5) 0.014(4) 0.015(4) 0.002(4) C26C 0.055(5) 0.033(4) 0.061(5) 0.002(4) 0.015(4) 0.015(4) C27C 0.043(4) 0.034(4) 0.038(4) 0.005(3) 0.016(3) 0.013(3) C3C 0.027(4) 0.055(5) 0.040(4) 0.021(4) 0.013(3) 0.012(3) C4C 0.026(3) 0.055(5) 0.041(4) 0.022(3) 0.011(3) 0.021(3) C41C 0.036(4) 0.082(7) 0.062(5) 0.048(5) 0.020(4) 0.032(4) C42C 0.030(5) 0.168(13) 0.129(10) 0.104(10) 0.034(6) 0.056(7) C43C 0.047(5) 0.097(8) 0.062(6) 0.034(6) -0.007(5) 0.018(5) C44C 0.062(7) 0.107(10) 0.103(9) 0.022(7) 0.016(6) 0.063(7) C5C 0.046(4) 0.042(4) 0.032(4) 0.018(3) 0.014(3) 0.018(3) C6C 0.028(3) 0.038(4) 0.029(3) 0.009(3) 0.011(3) 0.008(3) C61C 0.029(3) 0.039(4) 0.023(3) 0.007(3) 0.009(3) 0.007(3) N6C 0.034(3) 0.035(3) 0.027(3) 0.006(2) 0.015(2) 0.009(2) C62C 0.049(5) 0.035(4) 0.068(6) -0.004(4) 0.030(4) 0.011(4) C63C 0.028(3) 0.037(4) 0.037(4) 0.007(3) 0.013(3) 0.006(3) C64C 0.037(4) 0.033(4) 0.036(4) 0.005(3) 0.012(3) 0.011(3) C65C 0.038(4) 0.054(5) 0.036(4) 0.016(3) 0.016(3) 0.018(4) C1D 0.025(3) 0.028(3) 0.027(3) 0.008(3) 0.008(3) 0.009(3) O1D 0.023(2) 0.038(3) 0.028(2) 0.010(2) 0.0087(18) 0.0109(19) C2D 0.026(3) 0.027(3) 0.024(3) 0.003(2) 0.003(3) 0.008(3) C21D 0.020(3) 0.028(3) 0.028(3) 0.001(3) 0.008(2) 0.003(2) N2D 0.018(2) 0.025(3) 0.027(3) 0.003(2) 0.007(2) 0.004(2) C22D 0.030(3) 0.020(3) 0.028(3) 0.001(2) 0.007(3) 0.011(3) C23D 0.029(3) 0.036(4) 0.036(4) 0.003(3) 0.011(3) 0.008(3) C24D 0.040(4) 0.039(4) 0.041(4) 0.010(3) 0.020(3) 0.010(3) C25D 0.052(5) 0.046(4) 0.029(4) 0.007(3) 0.014(3) 0.018(4) C26D 0.043(4) 0.044(4) 0.027(3) -0.002(3) 0.003(3) 0.014(3) C27D 0.031(4) 0.031(4) 0.031(3) 0.000(3) 0.010(3) 0.007(3) C3D 0.023(3) 0.033(4) 0.036(4) 0.005(3) 0.011(3) 0.010(3) C4D 0.031(4) 0.036(4) 0.034(4) 0.008(3) 0.008(3) 0.014(3) C41D 0.035(4) 0.045(4) 0.039(4) 0.015(3) 0.010(3) 0.017(3) C42D 0.035(4) 0.075(6) 0.067(6) 0.028(5) 0.020(4) 0.029(4) C43D 0.039(5) 0.072(6) 0.090(7) 0.046(5) 0.028(5) 0.033(4) C44D 0.062(6) 0.100(9) 0.064(6) -0.023(6) -0.023(5) 0.041(6) C5D 0.036(4) 0.044(4) 0.029(3) 0.012(3) 0.008(3) 0.012(3) C6D 0.033(4) 0.038(4) 0.029(3) 0.009(3) 0.009(3) 0.012(3) C61D 0.036(4) 0.048(4) 0.035(4) 0.015(3) 0.012(3) 0.014(3) N6D 0.037(3) 0.048(4) 0.028(3) 0.012(3) 0.011(3) 0.017(3) C62D 0.048(5) 0.071(6) 0.052(5) 0.001(4) 0.024(4) 0.014(4) C63D 0.045(4) 0.056(5) 0.032(4) 0.015(3) 0.018(3) 0.017(4) C64D 0.039(4) 0.049(5) 0.057(5) 0.016(4) 0.024(4) 0.013(4) C65D 0.036(4) 0.054(5) 0.046(4) 0.021(4) 0.023(3) 0.012(4) B1 0.040(5) 0.042(5) 0.035(4) 0.003(4) 0.014(4) 0.009(4) F1 0.058(3) 0.060(3) 0.051(3) -0.012(2) 0.027(2) -0.002(2) F2 0.066(3) 0.059(3) 0.058(3) -0.010(3) 0.027(3) -0.002(3) F3 0.118(5) 0.068(4) 0.064(4) 0.028(3) 0.044(4) 0.017(4) F4 0.060(3) 0.079(4) 0.093(4) 0.010(3) 0.023(3) 0.030(3) B2 0.025(4) 0.056(6) 0.050(5) 0.012(4) 0.010(4) 0.012(4) F5 0.065(4) 0.098(4) 0.061(3) 0.015(3) 0.030(3) 0.037(3) F6 0.043(3) 0.080(4) 0.078(4) 0.024(3) -0.005(3) -0.003(3) F7 0.049(3) 0.071(4) 0.086(4) 0.031(3) 0.016(3) 0.000(3) F8 0.063(3) 0.088(4) 0.073(4) 0.004(3) 0.022(3) 0.041(3) B3 0.051(6) 0.040(5) 0.053(6) 0.010(4) 0.022(5) 0.006(4) F9 0.085(4) 0.061(3) 0.044(3) 0.012(2) 0.009(3) -0.002(3) F10 0.064(4) 0.073(4) 0.068(4) 0.025(3) 0.005(3) 0.009(3) F11 0.141(7) 0.048(4) 0.122(6) 0.001(4) 0.017(5) 0.014(4) F12 0.068(4) 0.187(8) 0.088(5) 0.035(5) 0.039(4) 0.057(5) B4 0.083(8) 0.061(7) 0.056(6) 0.021(5) 0.034(6) 0.024(6) F13 0.125(6) 0.059(4) 0.075(4) 0.035(3) 0.032(4) 0.018(4) F14 0.139(6) 0.086(4) 0.059(4) 0.007(3) 0.032(4) 0.057(4) F15 0.184(8) 0.084(4) 0.044(3) 0.012(3) 0.036(4) 0.062(5) F16 0.101(6) 0.150(8) 0.127(7) 0.022(6) 0.052(5) 0.000(6) C1H 0.095(10) 0.112(11) 0.113(11) -0.033(9) 0.002(9) 0.040(9) C2H 0.109(10) 0.069(8) 0.102(9) 0.010(7) 0.054(8) 0.031(7) O3H 0.065(4) 0.058(4) 0.079(5) 0.006(4) 0.014(4) 0.021(3) C4H 0.059(6) 0.074(7) 0.089(8) 0.018(6) 0.009(6) 0.016(5) C5H 0.055(6) 0.068(7) 0.094(8) 0.021(6) 0.015(6) 0.018(5) O1M 0.077(5) 0.101(6) 0.105(7) 0.010(5) 0.035(5) 0.017(5) O2M 0.075(8) 0.028(5) 0.035(6) -0.001(4) -0.009(5) 0.017(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1A 1.891(5) . ? Cu1 O1B 1.903(5) . ? Cu1 N2B 1.993(6) . ? Cu1 N2A 1.993(6) . ? C1A O1A 1.328(8) . ? C1A C6A 1.416(10) . ? C1A C2A 1.424(10) . ? C2A C3A 1.426(9) . ? C2A C21A 1.434(10) . ? C21A N2A 1.318(8) . ? N2A C22A 1.452(9) . ? C22A C27A 1.392(11) . ? C22A C23A 1.401(10) . ? C23A C24A 1.381(12) . ? C24A C25A 1.379(14) . ? C25A C26A 1.402(13) . ? C26A C27A 1.379(12) . ? C3A C4A 1.394(10) . ? C4A C5A 1.407(11) . ? C4A C41A 1.535(9) . ? C41A C43A 1.528(12) . ? C41A C42A 1.537(12) . ? C41A C44A 1.567(11) . ? C5A C6A 1.398(10) . ? C6A C61A 1.512(10) . ? C61A N6A 1.526(9) . ? N6A C62A 1.498(10) . ? N6A C63A 1.510(9) . ? C63A C64A 1.510(10) . ? C64A C65A 1.537(10) . ? C65A C65C 1.551(11) . ? C1B O1B 1.323(7) . ? C1B C6B 1.429(9) . ? C1B C2B 1.434(9) . ? C2B C3B 1.428(8) . ? C2B C21B 1.446(9) . ? C21B N2B 1.300(8) . ? N2B C22B 1.452(9) . ? C22B C27B 1.394(11) . ? C22B C23B 1.404(11) . ? C23B C24B 1.391(13) . ? C24B C25B 1.395(15) . ? C25B C26B 1.409(15) . ? C26B C27B 1.369(12) . ? C3B C4B 1.380(10) . ? C4B C5B 1.400(10) . ? C4B C41B 1.549(9) . ? C41B C44B 1.521(12) . ? C41B C43B 1.541(11) . ? C41B C42B 1.551(11) . ? C5B C6B 1.382(9) . ? C6B C61B 1.518(9) . ? C61B N6B 1.496(9) . ? N6B C62B 1.480(9) . ? N6B C63B 1.519(9) . ? C63B C64B 1.520(11) . ? C64B C65B 1.537(10) . ? C65B C65D 1.545(11) . ? Cu2 O1D 1.898(4) . ? Cu2 O1C 1.908(4) . ? Cu2 N2D 2.000(5) . ? Cu2 N2C 2.003(5) . ? C1C O1C 1.323(7) . ? C1C C2C 1.411(9) . ? C1C C6C 1.422(9) . ? C2C C21C 1.434(9) . ? C2C C3C 1.437(9) . ? C21C N2C 1.303(8) . ? N2C C22C 1.435(9) . ? C22C C27C 1.394(10) . ? C22C C23C 1.398(9) . ? C23C C24C 1.398(10) . ? C24C C25C 1.390(12) . ? C25C C26C 1.377(12) . ? C26C C27C 1.396(11) . ? C3C C4C 1.368(10) . ? C4C C5C 1.416(10) . ? C4C C41C 1.546(10) . ? C41C C44C 1.499(16) . ? C41C C42C 1.537(13) . ? C41C C43C 1.572(14) . ? C5C C6C 1.402(10) . ? C6C C61C 1.505(9) . ? C61C N6C 1.520(9) . ? N6C C63C 1.506(8) . ? N6C C62C 1.508(9) . ? C63C C64C 1.530(10) . ? C64C C65C 1.534(10) . ? C1D O1D 1.324(7) . ? C1D C2D 1.426(9) . ? C1D C6D 1.434(9) . ? C2D C3D 1.431(9) . ? C2D C21D 1.446(9) . ? C21D N2D 1.307(8) . ? N2D C22D 1.451(8) . ? C22D C23D 1.397(9) . ? C22D C27D 1.408(9) . ? C23D C24D 1.398(10) . ? C24D C25D 1.409(11) . ? C25D C26D 1.379(11) . ? C26D C27D 1.387(10) . ? C3D C4D 1.377(9) . ? C4D C5D 1.397(10) . ? C4D C41D 1.549(9) . ? C41D C43D 1.537(11) . ? C41D C44D 1.538(13) . ? C41D C42D 1.548(11) . ? C5D C6D 1.392(10) . ? C6D C61D 1.500(10) . ? C61D N6D 1.503(10) . ? N6D C62D 1.491(11) . ? N6D C63D 1.517(9) . ? C63D C64D 1.484(11) . ? C64D C65D 1.538(10) . ? B1 F3 1.364(10) . ? B1 F4 1.368(10) . ? B1 F1 1.408(9) . ? B1 F2 1.442(10) . ? B2 F5 1.384(11) . ? B2 F7 1.385(11) . ? B2 F8 1.385(10) . ? B2 F6 1.386(10) . ? B3 F12 1.356(11) . ? B3 F11 1.361(12) . ? B3 F9 1.391(11) . ? B3 F10 1.397(12) . ? B4 F16 1.367(15) . ? B4 F15 1.380(13) . ? B4 F14 1.381(13) . ? B4 F13 1.393(12) . ? C1H C2H 1.549(18) . ? C2H O3H 1.403(14) . ? O3H C4H 1.419(12) . ? C4H C5H 1.486(16) . ? C1J C2J 1.51(3) . ? C2J O3J 1.41(2) . ? O3J C4J 1.42(2) . ? C4J C5J 1.47(2) . ? O1M C1M 1.356(13) . ? O2M C2M 1.464(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A Cu1 O1B 156.0(2) . . ? O1A Cu1 N2B 92.0(2) . . ? O1B Cu1 N2B 92.9(2) . . ? O1A Cu1 N2A 94.4(2) . . ? O1B Cu1 N2A 92.5(2) . . ? N2B Cu1 N2A 151.2(2) . . ? O1A C1A C6A 118.0(6) . . ? O1A C1A C2A 123.8(6) . . ? C6A C1A C2A 118.1(6) . . ? C1A O1A Cu1 127.9(5) . . ? C1A C2A C3A 118.7(6) . . ? C1A C2A C21A 123.9(6) . . ? C3A C2A C21A 117.2(6) . . ? N2A C21A C2A 126.3(6) . . ? C21A N2A C22A 116.0(6) . . ? C21A N2A Cu1 123.0(5) . . ? C22A N2A Cu1 120.8(4) . . ? C27A C22A C23A 119.0(7) . . ? C27A C22A N2A 123.5(7) . . ? C23A C22A N2A 117.5(7) . . ? C24A C23A C22A 120.1(8) . . ? C25A C24A C23A 120.9(8) . . ? C24A C25A C26A 119.2(8) . . ? C27A C26A C25A 120.2(9) . . ? C26A C27A C22A 120.6(8) . . ? C4A C3A C2A 123.3(7) . . ? C3A C4A C5A 116.4(6) . . ? C3A C4A C41A 123.4(7) . . ? C5A C4A C41A 120.2(7) . . ? C43A C41A C4A 112.8(7) . . ? C43A C41A C42A 109.7(7) . . ? C4A C41A C42A 108.6(7) . . ? C43A C41A C44A 107.8(7) . . ? C4A C41A C44A 109.9(6) . . ? C42A C41A C44A 107.9(7) . . ? C6A C5A C4A 122.4(7) . . ? C5A C6A C1A 120.9(7) . . ? C5A C6A C61A 121.8(7) . . ? C1A C6A C61A 117.3(6) . . ? C6A C61A N6A 109.1(6) . . ? C62A N6A C63A 111.7(6) . . ? C62A N6A C61A 110.6(6) . . ? C63A N6A C61A 112.1(6) . . ? C64A C63A N6A 112.2(6) . . ? C63A C64A C65A 110.8(6) . . ? C64A C65A C65C 112.7(6) . . ? O1B C1B C6B 117.9(6) . . ? O1B C1B C2B 124.7(6) . . ? C6B C1B C2B 117.4(6) . . ? C1B O1B Cu1 128.4(4) . . ? C3B C2B C1B 119.3(6) . . ? C3B C2B C21B 118.4(6) . . ? C1B C2B C21B 122.3(6) . . ? N2B C21B C2B 126.3(6) . . ? C21B N2B C22B 115.8(6) . . ? C21B N2B Cu1 125.1(5) . . ? C22B N2B Cu1 119.0(4) . . ? C27B C22B C23B 119.6(8) . . ? C27B C22B N2B 122.3(7) . . ? C23B C22B N2B 118.1(7) . . ? C24B C23B C22B 120.1(9) . . ? C23B C24B C25B 120.1(9) . . ? C24B C25B C26B 119.0(9) . . ? C27B C26B C25B 121.0(9) . . ? C26B C27B C22B 120.1(9) . . ? C4B C3B C2B 122.1(6) . . ? C3B C4B C5B 117.9(6) . . ? C3B C4B C41B 123.4(6) . . ? C5B C4B C41B 118.7(6) . . ? C44B C41B C43B 108.7(7) . . ? C44B C41B C4B 110.3(7) . . ? C43B C41B C4B 111.3(6) . . ? C44B C41B C42B 108.7(7) . . ? C43B C41B C42B 109.6(7) . . ? C4B C41B C42B 108.2(6) . . ? C6B C5B C4B 122.7(6) . . ? C5B C6B C1B 120.6(6) . . ? C5B C6B C61B 122.7(6) . . ? C1B C6B C61B 116.7(6) . . ? N6B C61B C6B 110.9(6) . . ? C62B N6B C61B 112.9(6) . . ? C62B N6B C63B 111.5(6) . . ? C61B N6B C63B 111.7(5) . . ? N6B C63B C64B 109.6(6) . . ? C63B C64B C65B 114.5(6) . . ? C64B C65B C65D 110.9(6) . . ? O1D Cu2 O1C 153.5(2) . . ? O1D Cu2 N2D 93.7(2) . . ? O1C Cu2 N2D 94.0(2) . . ? O1D Cu2 N2C 93.1(2) . . ? O1C Cu2 N2C 94.7(2) . . ? N2D Cu2 N2C 145.7(2) . . ? O1C C1C C2C 124.8(6) . . ? O1C C1C C6C 116.9(5) . . ? C2C C1C C6C 118.3(5) . . ? C1C O1C Cu2 126.7(4) . . ? C1C C2C C21C 123.7(5) . . ? C1C C2C C3C 119.3(6) . . ? C21C C2C C3C 116.8(6) . . ? N2C C21C C2C 127.4(6) . . ? C21C N2C C22C 116.4(5) . . ? C21C N2C Cu2 122.2(5) . . ? C22C N2C Cu2 121.3(4) . . ? C27C C22C C23C 119.6(7) . . ? C27C C22C N2C 118.0(6) . . ? C23C C22C N2C 122.4(6) . . ? C22C C23C C24C 119.7(7) . . ? C25C C24C C23C 120.7(7) . . ? C26C C25C C24C 119.3(7) . . ? C25C C26C C27C 121.1(7) . . ? C22C C27C C26C 119.7(7) . . ? C4C C3C C2C 122.9(7) . . ? C3C C4C C5C 117.1(6) . . ? C3C C4C C41C 123.2(7) . . ? C5C C4C C41C 119.7(6) . . ? C44C C41C C42C 110.6(9) . . ? C44C C41C C4C 109.3(8) . . ? C42C C41C C4C 111.5(7) . . ? C44C C41C C43C 109.5(8) . . ? C42C C41C C43C 108.0(9) . . ? C4C C41C C43C 107.9(7) . . ? C6C C5C C4C 122.2(6) . . ? C5C C6C C1C 120.2(6) . . ? C5C C6C C61C 121.5(6) . . ? C1C C6C C61C 118.3(6) . . ? C6C C61C N6C 109.7(5) . . ? C63C N6C C62C 109.2(5) . . ? C63C N6C C61C 114.3(5) . . ? C62C N6C C61C 110.4(6) . . ? N6C C63C C64C 112.2(6) . . ? C63C C64C C65C 112.9(6) . . ? C64C C65C C65A 114.6(6) . . ? O1D C1D C2D 124.6(5) . . ? O1D C1D C6D 118.0(6) . . ? C2D C1D C6D 117.4(6) . . ? C1D O1D Cu2 127.5(4) . . ? C1D C2D C3D 119.7(6) . . ? C1D C2D C21D 122.7(6) . . ? C3D C2D C21D 117.6(6) . . ? N2D C21D C2D 126.8(6) . . ? C21D N2D C22D 117.0(5) . . ? C21D N2D Cu2 123.3(4) . . ? C22D N2D Cu2 119.8(4) . . ? C23D C22D C27D 119.0(6) . . ? C23D C22D N2D 123.0(6) . . ? C27D C22D N2D 118.0(6) . . ? C22D C23D C24D 120.1(7) . . ? C23D C24D C25D 120.3(7) . . ? C26D C25D C24D 119.2(7) . . ? C25D C26D C27D 121.0(7) . . ? C26D C27D C22D 120.4(7) . . ? C4D C3D C2D 122.2(6) . . ? C3D C4D C5D 117.4(6) . . ? C3D C4D C41D 123.1(6) . . ? C5D C4D C41D 119.5(6) . . ? C43D C41D C44D 108.9(8) . . ? C43D C41D C42D 107.7(7) . . ? C44D C41D C42D 109.3(8) . . ? C43D C41D C4D 109.8(6) . . ? C44D C41D C4D 109.2(6) . . ? C42D C41D C4D 111.9(6) . . ? C6D C5D C4D 123.4(6) . . ? C5D C6D C1D 119.7(6) . . ? C5D C6D C61D 123.2(6) . . ? C1D C6D C61D 117.1(6) . . ? C6D C61D N6D 110.2(6) . . ? C62D N6D C61D 112.2(6) . . ? C62D N6D C63D 112.8(6) . . ? C61D N6D C63D 111.6(6) . . ? C64D C63D N6D 110.2(6) . . ? C63D C64D C65D 114.7(7) . . ? C64D C65D C65B 109.9(7) . . ? F3 B1 F4 112.3(7) . . ? F3 B1 F1 110.8(7) . . ? F4 B1 F1 109.0(7) . . ? F3 B1 F2 110.2(7) . . ? F4 B1 F2 108.3(7) . . ? F1 B1 F2 106.1(6) . . ? F5 B2 F7 109.2(8) . . ? F5 B2 F8 109.8(7) . . ? F7 B2 F8 109.9(7) . . ? F5 B2 F6 109.1(7) . . ? F7 B2 F6 108.4(7) . . ? F8 B2 F6 110.3(8) . . ? F12 B3 F11 107.3(9) . . ? F12 B3 F9 112.0(8) . . ? F11 B3 F9 111.2(8) . . ? F12 B3 F10 108.8(8) . . ? F11 B3 F10 106.7(8) . . ? F9 B3 F10 110.7(7) . . ? F16 B4 F15 109.6(9) . . ? F16 B4 F14 109.0(10) . . ? F15 B4 F14 109.6(10) . . ? F16 B4 F13 110.0(10) . . ? F15 B4 F13 109.3(10) . . ? F14 B4 F13 109.4(9) . . ? O3H C2H C1H 109.2(10) . . ? C2H O3H C4H 114.0(9) . . ? O3H C4H C5H 111.5(9) . . ? O3J C2J C1J 108.0(16) . . ? C2J O3J C4J 113.0(14) . . ? O3J C4J C5J 112.5(15) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 26.46 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.425 _refine_diff_density_min -0.676 _refine_diff_density_rms 0.133