# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _publ_contact_author_email powell@chemie.uni-karlsruhe.de _publ_contact_author_name 'Annie K. Powell' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author ; Annie K. Powell ; _publ_contact_author_address ; Institute for Inorganic Chemistry University of Karlsruhe Engesserstrasse Geb. 30.45 Karlsruhe D 76128 GERMANY ; _publ_contact_author_phone '+44 721 608 2135' _publ_section_title ; A Novel Nonanuclear Carboxylate-Bridged CuII Aggregate with a S = 7/2 Ground Spin State. ; loop_ _publ_author_name _publ_author_address 'Muralee Murugesu' ; Institut fur Anorganische Chemie Universitat Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; 'Philippa J. King' ; Institut fur Anorganische Chemie Universitat Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; 'Rodolphe Clerac' ; Centre de Recherche Paul Pascal CNRS UPR 8641 Avenur Dr. A. Schweitzer 33600 Pessac France ; 'Christopher E. Anson' ; Institut fur Anorganische Chemie Universitat Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; 'Annie K. Powell' ; Institut fur Anorganische Chemie Universitat Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; data_cu9 _database_code_depnum_ccdc_archive 'CCDC 226039' _chemical_name_common ; (hexakis-(N-(carboxymethyl)-N-(2’-carboxyphenyl)glycinato)- tris(methanol)-nonacopper(ii)) hexamehanol solvate ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; [hexakis-{N-(carboxymethyl)-N- (2’-carboxyphenyl)glycinato}-tris(methanol)-nonacopper(II)] hexamehanol solvate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H96 Cu9 N6 O48' _chemical_formula_weight 2457.47 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.6762(9) _cell_length_b 17.3686(11) _cell_length_c 21.3680(18) _cell_angle_alpha 90.00 _cell_angle_beta 95.453(9) _cell_angle_gamma 90.00 _cell_volume 4683.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 7123 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 24.17 _exptl_crystal_description chunk _exptl_crystal_colour green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.743 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2502 _exptl_absorpt_coefficient_mu 2.103 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29723 _diffrn_reflns_av_R_equivalents 0.0667 _diffrn_reflns_av_sigmaI/netI 0.0760 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 25.97 _reflns_number_total 8575 _reflns_number_gt 5481 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS 2.92 (Stoe & Cie GmbH, 1999)' _computing_cell_refinement 'IPDS 2.92 (Stoe & Cie GmbH, 1999)' _computing_data_reduction 'IPDS 2.92 (Stoe & Cie GmbH, 1999)' _computing_structure_solution 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_structure_refinement 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_molecular_graphics 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_publication_material 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _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^)+(0.0721P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8575 _refine_ls_number_parameters 718 _refine_ls_number_restraints 78 _refine_ls_R_factor_all 0.0862 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1293 _refine_ls_wR_factor_gt 0.1189 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.935 _refine_ls_shift/su_max 0.001 _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 0.5000 0.5000 0.5000 0.0294(2) Uani 1 2 d S . . Cu2 Cu 0.30720(6) 0.39135(4) 0.56680(3) 0.03351(17) Uani 1 1 d . . . Cu3 Cu 0.56795(6) 0.60450(4) 0.65904(3) 0.03600(18) Uani 1 1 d . A . Cu4 Cu 0.31598(6) 0.66167(4) 0.45146(3) 0.03491(17) Uani 1 1 d . . . Cu5 Cu 0.19682(6) 0.64776(4) 0.66314(3) 0.04102(19) Uani 1 1 d . B . N1 N 0.1725(4) 0.3885(3) 0.5069(2) 0.0355(10) Uani 1 1 d . . . C1 C 0.0917(5) 0.3764(3) 0.5504(2) 0.0339(12) Uani 1 1 d . . . C2 C 0.0816(5) 0.4316(3) 0.5980(3) 0.0375(13) Uani 1 1 d . . . C3 C 0.0063(5) 0.4221(4) 0.6394(3) 0.0430(14) Uani 1 1 d . . . H3 H -0.0021 0.4600 0.6693 0.052 Uiso 1 1 calc R . . C4 C -0.0572(5) 0.3573(4) 0.6375(3) 0.0468(15) Uani 1 1 d . . . H4 H -0.1074 0.3511 0.6662 0.056 Uiso 1 1 calc R . . C5 C -0.0452(5) 0.3019(4) 0.5924(3) 0.0460(15) Uani 1 1 d . . . H5 H -0.0871 0.2579 0.5913 0.055 Uiso 1 1 calc R . . C6 C 0.0287(5) 0.3105(3) 0.5483(3) 0.0414(14) Uani 1 1 d . . . H6 H 0.0356 0.2729 0.5180 0.050 Uiso 1 1 calc R . . C7 C 0.1583(5) 0.4972(3) 0.6100(2) 0.0364(13) Uani 1 1 d . . . O1 O 0.2554(3) 0.4861(2) 0.60540(17) 0.0393(9) Uani 1 1 d . . . O2 O 0.1195(3) 0.5600(2) 0.62556(19) 0.0468(10) Uani 1 1 d . . . C8 C 0.1608(5) 0.4616(3) 0.4699(2) 0.0345(12) Uani 1 1 d . . . H8A H 0.1157 0.4966 0.4906 0.041 Uiso 1 1 calc R . . H8B H 0.1261 0.4504 0.4285 0.041 Uiso 1 1 calc R . . C9 C 0.2660(5) 0.5009(3) 0.4628(2) 0.0318(12) Uani 1 1 d . . . O3 O 0.3480(3) 0.4717(2) 0.49136(16) 0.0329(8) Uani 1 1 d . . . O4 O 0.2602(3) 0.5607(2) 0.42985(16) 0.0360(9) Uani 1 1 d . . . C10 C 0.1890(5) 0.3232(3) 0.4645(2) 0.0392(14) Uani 1 1 d . . . H10A H 0.2241 0.3413 0.4289 0.047 Uiso 1 1 calc R . . H10B H 0.1210 0.3018 0.4487 0.047 Uiso 1 1 calc R . . C11 C 0.2556(5) 0.2613(3) 0.4988(3) 0.0445(15) Uani 1 1 d . . . O5 O 0.3185(3) 0.2838(2) 0.54579(19) 0.0438(10) Uani 1 1 d . . . O6 O 0.2501(4) 0.1933(3) 0.4801(2) 0.0649(14) Uani 1 1 d . . . N2 N 0.5717(4) 0.5205(3) 0.7264(2) 0.0448(13) Uani 1 1 d . . . C12 C 0.6582(7) 0.5243(4) 0.7738(4) 0.064(2) Uani 1 1 d . . . C13 C 0.7537(7) 0.5410(5) 0.7585(3) 0.068(2) Uani 1 1 d . . . C14 C 0.8429(9) 0.5332(6) 0.8053(4) 0.096(3) Uani 1 1 d . . . H14 H 0.9115 0.5391 0.7940 0.115 Uiso 1 1 calc R . . C15 C 0.8253(9) 0.5162(8) 0.8702(5) 0.131(5) Uani 1 1 d . . . H15 H 0.8797 0.5199 0.9024 0.157 Uiso 1 1 calc R . . C16 C 0.7251(11) 0.4946(7) 0.8815(5) 0.116(4) Uani 1 1 d . . . H16 H 0.7133 0.4771 0.9214 0.139 Uiso 1 1 calc R . . C17 C 0.6397(8) 0.4979(5) 0.8350(4) 0.081(3) Uani 1 1 d . . . H17 H 0.5721 0.4832 0.8438 0.098 Uiso 1 1 calc R . . C18 C 0.7835(6) 0.5699(3) 0.6964(3) 0.0447(15) Uani 1 1 d . . . O7 O 0.7148(3) 0.5915(2) 0.65267(18) 0.0437(10) Uani 1 1 d . . . O8 O 0.8790(4) 0.5733(3) 0.6915(2) 0.0696(15) Uani 1 1 d . . . C19 C 0.5695(6) 0.4447(3) 0.6937(3) 0.0473(16) Uani 1 1 d . . . H19A H 0.5476 0.4055 0.7221 0.057 Uiso 1 1 calc R . . H19B H 0.6407 0.4322 0.6840 0.057 Uiso 1 1 calc R . . C20 C 0.4958(5) 0.4421(3) 0.6331(2) 0.0323(12) Uani 1 1 d . . . O9 O 0.5089(3) 0.4942(2) 0.59409(16) 0.0345(8) Uani 1 1 d . . . O10 O 0.4315(3) 0.3873(2) 0.62743(17) 0.0377(9) Uani 1 1 d . . . C21 C 0.4586(7) 0.5347(4) 0.7565(3) 0.066(2) Uani 1 1 d . . . H21A H 0.4275 0.4854 0.7655 0.079 Uiso 1 1 calc R . . H21B H 0.4716 0.5627 0.7958 0.079 Uiso 1 1 calc R . . C22 C 0.3803(6) 0.5807(4) 0.7110(3) 0.0490(17) Uani 1 1 d . . . O11 O 0.4182(4) 0.6155(3) 0.6674(2) 0.0477(10) Uani 1 1 d . . . O12 O 0.2839(4) 0.5823(2) 0.72190(19) 0.0475(10) Uani 1 1 d . . . N3 N 0.3730(4) 0.7679(3) 0.4719(2) 0.0396(11) Uani 1 1 d . . . C23 C 0.2805(5) 0.8181(3) 0.4745(3) 0.0447(15) Uani 1 1 d . . . C24 C 0.2031(5) 0.7978(3) 0.5135(3) 0.0444(15) Uani 1 1 d . . . C25 C 0.1177(6) 0.8474(4) 0.5186(3) 0.0572(19) Uani 1 1 d . . . H25 H 0.0679 0.8363 0.5465 0.069 Uiso 1 1 calc R . . C26 C 0.1071(8) 0.9136(4) 0.4818(4) 0.072(2) Uani 1 1 d . . . H26 H 0.0498 0.9464 0.4847 0.087 Uiso 1 1 calc R . . C27 C 0.1814(8) 0.9301(4) 0.4412(4) 0.076(3) Uani 1 1 d . . . H27 H 0.1728 0.9730 0.4152 0.091 Uiso 1 1 calc R . . C28 C 0.2682(7) 0.8839(4) 0.4386(3) 0.061(2) Uani 1 1 d . . . H28 H 0.3196 0.8971 0.4122 0.073 Uiso 1 1 calc R . . C29 C 0.2020(5) 0.7220(3) 0.5490(3) 0.0433(15) Uani 1 1 d . . . O13 O 0.2485(3) 0.6641(2) 0.53055(18) 0.0418(10) Uani 1 1 d . . . O14 O 0.1502(4) 0.7217(2) 0.59674(19) 0.0494(11) Uani 1 1 d . . . C30 C 0.4434(5) 0.7633(3) 0.5319(3) 0.0435(15) Uani 1 1 d . . . H30A H 0.4027 0.7762 0.5667 0.052 Uiso 1 1 calc R . . H30B H 0.4998 0.8009 0.5310 0.052 Uiso 1 1 calc R . . C31 C 0.4919(5) 0.6835(3) 0.5430(3) 0.0371(13) Uani 1 1 d . . . O15 O 0.4655(3) 0.6305(2) 0.50602(17) 0.0366(9) Uani 1 1 d . . . O16 O 0.5586(4) 0.6805(2) 0.59077(19) 0.0508(11) Uani 1 1 d . . . C32 C 0.4384(5) 0.7825(3) 0.4188(3) 0.0418(14) Uani 1 1 d . . . H32A H 0.5065 0.7573 0.4270 0.050 Uiso 1 1 calc R . . H32B H 0.4507 0.8374 0.4151 0.050 Uiso 1 1 calc R . . C33 C 0.3827(5) 0.7527(3) 0.3585(3) 0.0448(15) Uani 1 1 d . . . O17 O 0.3219(3) 0.6941(2) 0.36394(17) 0.0398(9) Uani 1 1 d . . . O18 O 0.3993(4) 0.7818(3) 0.3077(2) 0.0591(13) Uani 1 1 d . . . O19 O 0.5945(5) 0.6997(4) 0.7416(3) 0.091(2) Uani 1 1 d . . . C34A C 0.6810(15) 0.7356(10) 0.7813(9) 0.083(6) Uani 0.50 1 d P A 1 H34A H 0.6525 0.7720 0.8091 0.124 Uiso 0.50 1 calc PR A 1 H34B H 0.7275 0.7617 0.7554 0.124 Uiso 0.50 1 calc PR A 1 H34C H 0.7199 0.6967 0.8057 0.124 Uiso 0.50 1 calc PR A 1 C34B C 0.575(3) 0.775(2) 0.7161(18) 0.22(2) Uani 0.50 1 d PU A 2 H34D H 0.5851 0.8122 0.7491 0.337 Uiso 0.50 1 calc PR A 2 H34E H 0.5029 0.7775 0.6973 0.337 Uiso 0.50 1 calc PR A 2 H34F H 0.6224 0.7848 0.6848 0.337 Uiso 0.50 1 calc PR A 2 O20 O 0.0568(4) 0.6601(3) 0.7194(3) 0.0707(15) Uani 1 1 d . . . C35A C 0.049(3) 0.676(2) 0.7768(18) 0.17(2) Uani 0.50 1 d P B 1 H35A H -0.0250 0.6780 0.7840 0.253 Uiso 0.50 1 calc PR B 1 H35B H 0.0810 0.7249 0.7867 0.253 Uiso 0.50 1 calc PR B 1 H35C H 0.0835 0.6369 0.8029 0.253 Uiso 0.50 1 calc PR B 1 C35B C 0.091(2) 0.653(2) 0.7889(8) 0.072(7) Uani 0.50 1 d P B 2 H35D H 0.0305 0.6581 0.8123 0.108 Uiso 0.50 1 calc PR B 2 H35E H 0.1418 0.6920 0.8013 0.108 Uiso 0.50 1 calc PR B 2 H35F H 0.1226 0.6029 0.7971 0.108 Uiso 0.50 1 calc PR B 2 O21 O 0.2635(4) 0.7387(2) 0.7080(2) 0.0575(13) Uani 1 1 d . . . C36A C 0.2226(18) 0.8118(17) 0.7123(11) 0.050(5) Uani 0.50 1 d P B 1 H36A H 0.2728 0.8436 0.7368 0.076 Uiso 0.50 1 calc PR B 1 H36B H 0.1578 0.8095 0.7321 0.076 Uiso 0.50 1 calc PR B 1 H36C H 0.2088 0.8332 0.6709 0.076 Uiso 0.50 1 calc PR B 1 C36B C 0.237(3) 0.8199(18) 0.6952(12) 0.108(15) Uani 0.50 1 d P B 2 H36D H 0.2812 0.8520 0.7233 0.162 Uiso 0.50 1 calc PR B 2 H36E H 0.1641 0.8287 0.7012 0.162 Uiso 0.50 1 calc PR B 2 H36F H 0.2492 0.8319 0.6526 0.162 Uiso 0.50 1 calc PR B 2 O91A O 0.0942(18) 0.1110(9) 0.4075(11) 0.097(6) Uani 0.50 1 d PU C 1 C91A C 0.074(3) 0.141(2) 0.345(3) 0.129(13) Uani 0.50 1 d PU C 1 O91B O 0.125(3) 0.1362(19) 0.3811(15) 0.169(14) Uani 0.50 1 d PU D 2 C91B C 0.101(4) 0.185(2) 0.3343(15) 0.144(14) Uani 0.50 1 d PU D 2 O92A O 0.3878(19) 0.0842(10) 0.5195(13) 0.180(11) Uani 0.50 1 d PU E 1 C92A C 0.495(3) 0.037(2) 0.458(2) 0.22(2) Uani 0.50 1 d PU F 1 O92B O 0.455(5) 0.056(2) 0.389(2) 0.42(3) Uani 0.50 1 d PU G 2 C92B C 0.437(4) 0.043(3) 0.490(3) 0.26(3) Uani 0.50 1 d PU H 2 O93A O 0.582(2) 0.8610(10) 0.6630(8) 0.191(11) Uani 0.50 1 d PU I 1 C93A C 0.6108(19) 0.9476(16) 0.6327(11) 0.102(8) Uani 0.50 1 d PU I 1 O93B O 0.6949(17) 0.7022(10) 0.8426(9) 0.138(6) Uani 0.50 1 d PU J 2 C93B C 0.805(2) 0.728(3) 0.8332(16) 0.208(19) Uani 0.50 1 d PU J 2 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 0.0233(6) 0.0375(5) 0.0277(4) 0.0006(4) 0.0036(3) -0.0010(4) Cu2 0.0273(4) 0.0398(4) 0.0335(3) -0.0009(3) 0.0031(3) -0.0020(3) Cu3 0.0315(4) 0.0437(4) 0.0322(3) 0.0006(3) 0.0003(3) 0.0025(3) Cu4 0.0358(5) 0.0346(3) 0.0341(3) 0.0014(3) 0.0022(3) 0.0024(3) Cu5 0.0333(5) 0.0492(4) 0.0408(4) -0.0113(3) 0.0044(3) 0.0032(3) N1 0.029(3) 0.042(3) 0.037(2) -0.001(2) 0.0079(19) -0.005(2) C1 0.030(4) 0.040(3) 0.032(3) 0.004(2) 0.001(2) 0.001(2) C2 0.028(4) 0.048(3) 0.037(3) 0.001(2) 0.003(2) -0.001(2) C3 0.031(4) 0.060(4) 0.039(3) -0.001(3) 0.007(2) 0.006(3) C4 0.033(4) 0.068(4) 0.040(3) 0.009(3) 0.008(3) -0.002(3) C5 0.037(4) 0.057(4) 0.045(3) 0.008(3) 0.005(3) -0.015(3) C6 0.037(4) 0.051(3) 0.035(3) 0.001(2) 0.001(2) -0.007(3) C7 0.029(4) 0.051(3) 0.030(3) -0.008(2) 0.005(2) 0.001(3) O1 0.030(3) 0.050(2) 0.039(2) -0.0098(17) 0.0063(16) -0.0017(17) O2 0.035(3) 0.054(3) 0.053(2) -0.015(2) 0.0096(19) 0.0022(19) C8 0.030(4) 0.037(3) 0.035(3) -0.002(2) 0.002(2) 0.000(2) C9 0.034(4) 0.037(3) 0.025(2) -0.005(2) 0.004(2) -0.002(2) O3 0.030(3) 0.038(2) 0.0318(19) -0.0018(15) 0.0065(16) -0.0017(16) O4 0.035(3) 0.040(2) 0.0331(19) 0.0023(16) 0.0045(16) 0.0013(17) C10 0.037(4) 0.047(3) 0.034(3) -0.008(2) 0.007(2) -0.010(3) C11 0.048(4) 0.039(3) 0.047(3) -0.007(3) 0.011(3) -0.006(3) O5 0.039(3) 0.041(2) 0.051(2) -0.0036(18) -0.0002(19) 0.0000(18) O6 0.076(4) 0.045(3) 0.071(3) -0.015(2) -0.002(3) -0.003(2) N2 0.047(4) 0.054(3) 0.031(2) 0.003(2) -0.007(2) -0.012(2) C12 0.059(6) 0.066(5) 0.063(5) 0.006(3) -0.017(4) 0.000(4) C13 0.071(7) 0.077(5) 0.058(4) 0.012(4) 0.016(4) 0.017(4) C14 0.077(8) 0.131(8) 0.076(6) 0.020(6) -0.014(5) -0.026(6) C15 0.074(9) 0.191(12) 0.118(9) 0.093(9) -0.037(6) -0.045(8) C16 0.122(11) 0.137(9) 0.081(7) 0.033(6) -0.031(6) -0.034(8) C17 0.085(7) 0.106(7) 0.051(4) 0.015(4) 0.001(4) 0.017(5) C18 0.048(5) 0.045(3) 0.040(3) -0.009(3) -0.002(3) 0.001(3) O7 0.031(3) 0.063(3) 0.037(2) 0.0041(18) 0.0025(17) -0.0051(19) O8 0.037(4) 0.096(4) 0.072(3) -0.019(3) -0.012(2) 0.008(3) C19 0.048(5) 0.044(3) 0.047(3) 0.011(3) -0.012(3) -0.005(3) C20 0.027(4) 0.039(3) 0.032(3) -0.001(2) 0.009(2) 0.005(2) O9 0.031(2) 0.040(2) 0.0324(19) -0.0022(16) 0.0015(15) -0.0010(17) O10 0.033(3) 0.041(2) 0.038(2) 0.0047(16) -0.0017(16) -0.0043(17) C21 0.082(6) 0.062(4) 0.051(4) -0.013(3) -0.010(4) 0.018(4) C22 0.051(5) 0.049(4) 0.044(3) -0.020(3) -0.011(3) 0.013(3) O11 0.035(3) 0.062(3) 0.047(2) -0.008(2) 0.0029(19) 0.007(2) O12 0.042(3) 0.057(3) 0.045(2) -0.0086(19) 0.009(2) 0.001(2) N3 0.036(3) 0.039(3) 0.043(3) 0.001(2) -0.004(2) 0.001(2) C23 0.046(5) 0.034(3) 0.051(3) -0.007(2) -0.011(3) 0.004(3) C24 0.041(4) 0.043(3) 0.047(3) -0.011(3) -0.008(3) 0.009(3) C25 0.058(5) 0.056(4) 0.055(4) -0.018(3) -0.007(3) 0.022(3) C26 0.080(7) 0.054(4) 0.078(5) -0.019(4) -0.013(5) 0.038(4) C27 0.100(8) 0.048(4) 0.076(5) -0.002(4) -0.012(5) 0.028(4) C28 0.074(6) 0.043(4) 0.065(4) -0.004(3) -0.002(4) 0.013(3) C29 0.036(4) 0.052(3) 0.040(3) -0.011(3) -0.007(3) 0.012(3) O13 0.042(3) 0.042(2) 0.042(2) -0.0031(17) 0.0071(18) 0.0061(18) O14 0.045(3) 0.061(3) 0.042(2) -0.0135(19) 0.004(2) 0.016(2) C30 0.041(4) 0.045(3) 0.043(3) -0.002(3) -0.007(3) 0.000(3) C31 0.029(4) 0.047(3) 0.035(3) 0.007(3) 0.004(2) 0.000(2) O15 0.032(3) 0.044(2) 0.0341(19) 0.0034(17) 0.0016(16) 0.0040(17) O16 0.052(3) 0.051(2) 0.046(2) 0.0129(19) -0.014(2) -0.007(2) C32 0.042(4) 0.035(3) 0.048(3) 0.010(2) 0.002(3) -0.001(3) C33 0.043(4) 0.044(3) 0.046(3) 0.013(3) -0.001(3) 0.005(3) O17 0.039(3) 0.040(2) 0.039(2) 0.0044(16) -0.0020(17) -0.0015(18) O18 0.064(4) 0.061(3) 0.050(3) 0.026(2) -0.010(2) -0.017(2) O19 0.062(5) 0.076(4) 0.132(6) -0.037(4) -0.010(4) 0.002(3) C34A 0.080(14) 0.076(11) 0.091(13) -0.050(10) 0.000(10) 0.004(9) C34B 0.13(3) 0.29(4) 0.27(4) -0.24(4) 0.12(3) -0.10(3) O20 0.058(4) 0.088(4) 0.072(3) -0.027(3) 0.033(3) -0.006(3) C35A 0.09(3) 0.22(4) 0.20(4) -0.14(3) 0.07(3) -0.12(3) C35B 0.049(15) 0.149(18) 0.021(6) -0.024(8) 0.019(7) -0.029(12) O21 0.055(3) 0.047(3) 0.067(3) -0.020(2) -0.013(2) 0.006(2) C36A 0.048(12) 0.067(12) 0.033(12) 0.006(9) -0.012(7) -0.003(7) C36B 0.23(4) 0.054(15) 0.031(13) -0.023(11) -0.005(14) 0.023(16) O91A 0.093(14) 0.055(8) 0.135(18) 0.006(8) -0.024(10) 0.001(7) C91A 0.08(2) 0.14(3) 0.16(4) 0.04(3) 0.001(19) 0.00(2) O91B 0.18(3) 0.16(3) 0.15(3) 0.011(19) -0.05(2) -0.02(2) C91B 0.17(4) 0.18(4) 0.076(17) -0.01(2) -0.023(19) 0.01(3) O92A 0.17(2) 0.079(11) 0.27(3) -0.003(13) -0.107(19) 0.027(11) C92A 0.20(4) 0.19(3) 0.29(4) 0.14(3) 0.18(4) 0.11(3) O92B 0.63(7) 0.20(3) 0.38(5) -0.02(3) -0.30(5) -0.12(4) C92B 0.26(5) 0.19(4) 0.38(6) -0.09(4) 0.22(5) -0.12(4) O93A 0.35(3) 0.083(11) 0.120(13) -0.046(10) -0.072(16) 0.069(15) C93A 0.078(16) 0.14(2) 0.094(14) -0.049(14) 0.032(12) -0.053(14) O93B 0.154(19) 0.130(13) 0.128(14) -0.054(11) 0.005(12) -0.005(12) C93B 0.09(2) 0.35(5) 0.18(3) -0.18(3) 0.012(19) -0.05(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O3 1.980(4) 3_666 yes Cu1 O3 1.980(4) . yes Cu1 O9 2.005(3) 3_666 yes Cu1 O9 2.005(3) . yes Cu1 O15 2.315(4) . yes Cu1 O15 2.315(4) 3_666 yes Cu2 O5 1.929(4) . yes Cu2 O10 1.943(4) . yes Cu2 O1 1.980(4) . yes Cu2 N1 2.035(5) . yes Cu2 O3 2.230(4) . yes Cu3 O7 1.893(4) . yes Cu3 O11 1.933(5) . yes Cu3 O16 1.963(4) . yes Cu3 N2 2.046(5) . yes Cu3 O19 2.419(6) . yes Cu3 O9 2.441(4) . yes Cu4 O4 1.931(4) . yes Cu4 O17 1.961(4) . yes Cu4 O13 1.966(4) . yes Cu4 N3 2.014(5) . yes Cu4 O15 2.196(4) . yes Cu5 O2 1.945(4) . yes Cu5 O12 1.955(5) . yes Cu5 O14 1.963(4) . yes Cu5 O21 1.993(4) . yes Cu5 O20 2.247(5) . yes N1 C1 1.463(7) . ? N1 C10 1.478(7) . ? N1 C8 1.495(7) . ? C1 C6 1.394(8) . ? C1 C2 1.412(8) . ? C2 C3 1.372(8) . ? C2 C7 1.503(8) . ? C3 C4 1.382(9) . ? C4 C5 1.382(9) . ? C5 C6 1.398(8) . ? C7 O2 1.253(7) . ? C7 O1 1.260(7) . ? C8 C9 1.519(8) . ? C9 O4 1.252(6) . ? C9 O3 1.260(6) . ? C10 C11 1.512(9) . ? C11 O6 1.247(7) . ? C11 O5 1.283(7) . ? N2 C12 1.422(9) . ? N2 C19 1.489(8) . ? N2 C21 1.645(10) . ? C12 C13 1.317(11) . ? C12 C17 1.425(11) . ? C13 C14 1.443(12) . ? C13 C18 1.500(10) . ? C14 C15 1.456(14) . ? C15 C16 1.368(16) . ? C16 C17 1.400(13) . ? C18 O8 1.227(8) . ? C18 O7 1.271(7) . ? C19 C20 1.523(8) . ? C20 O10 1.251(7) . ? C20 O9 1.253(6) . ? C21 C22 1.545(9) . ? C22 O11 1.244(8) . ? C22 O12 1.267(8) . ? N3 C23 1.466(8) . ? N3 C32 1.489(8) . ? N3 C30 1.493(7) . ? C23 C28 1.378(9) . ? C23 C24 1.392(9) . ? C24 C25 1.396(9) . ? C24 C29 1.520(9) . ? C25 C26 1.391(11) . ? C26 C27 1.371(13) . ? C27 C28 1.367(11) . ? C29 O13 1.248(7) . ? C29 O14 1.264(7) . ? C30 C31 1.525(8) . ? C31 O15 1.238(7) . ? C31 O16 1.263(7) . ? C32 C33 1.502(9) . ? C33 O18 1.234(7) . ? C33 O17 1.289(7) . ? O19 C34B 1.42(5) . ? O19 C34A 1.461(18) . ? O20 C35A 1.27(3) . ? O20 C35B 1.512(19) . ? O21 C36A 1.38(3) . ? O21 C36B 1.47(3) . ? O91A C91A 1.44(6) . ? O91B C91B 1.32(5) . ? O93A C93A 1.69(3) . ? O93B C93B 1.50(3) . ? 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 O3 Cu1 O3 180.00(19) 3_666 . yes O3 Cu1 O9 92.44(15) 3_666 3_666 yes O3 Cu1 O9 87.56(15) . 3_666 yes O3 Cu1 O9 87.56(15) 3_666 . yes O3 Cu1 O9 92.44(15) . . yes O9 Cu1 O9 180.000(1) 3_666 . yes O3 Cu1 O15 86.51(14) 3_666 . yes O3 Cu1 O15 93.49(14) . . yes O9 Cu1 O15 90.76(14) 3_666 . yes O9 Cu1 O15 89.24(14) . . yes O3 Cu1 O15 93.49(14) 3_666 3_666 yes O3 Cu1 O15 86.51(14) . 3_666 yes O9 Cu1 O15 89.24(14) 3_666 3_666 yes O9 Cu1 O15 90.76(14) . 3_666 yes O15 Cu1 O15 180.000(1) . 3_666 yes O5 Cu2 O10 92.66(17) . . yes O5 Cu2 O1 159.41(18) . . yes O10 Cu2 O1 91.86(16) . . yes O5 Cu2 N1 84.62(18) . . yes O10 Cu2 N1 175.52(17) . . yes O1 Cu2 N1 89.49(18) . . yes O5 Cu2 O3 114.22(15) . . yes O10 Cu2 O3 106.01(15) . . yes O1 Cu2 O3 83.67(14) . . yes N1 Cu2 O3 78.38(16) . . yes O7 Cu3 O11 178.34(19) . . yes O7 Cu3 O16 90.99(19) . . yes O11 Cu3 O16 90.7(2) . . yes O7 Cu3 N2 90.5(2) . . yes O11 Cu3 N2 87.9(2) . . yes O16 Cu3 N2 176.25(18) . . yes O7 Cu3 O19 93.7(2) . . yes O11 Cu3 O19 86.3(2) . . yes O16 Cu3 O19 94.4(2) . . yes N2 Cu3 O19 89.0(2) . . yes O7 Cu3 O9 96.64(15) . . yes O11 Cu3 O9 83.08(15) . . yes O16 Cu3 O9 96.43(15) . . yes N2 Cu3 O9 79.97(16) . . yes O19 Cu3 O9 164.9(2) . . yes O4 Cu4 O17 94.55(15) . . yes O4 Cu4 O13 92.62(16) . . yes O17 Cu4 O13 150.78(17) . . yes O4 Cu4 N3 178.64(17) . . yes O17 Cu4 N3 84.16(18) . . yes O13 Cu4 N3 88.31(19) . . yes O4 Cu4 O15 100.45(15) . . yes O17 Cu4 O15 117.87(16) . . yes O13 Cu4 O15 88.45(16) . . yes N3 Cu4 O15 80.57(17) . . yes O2 Cu5 O12 92.34(18) . . yes O2 Cu5 O14 96.28(19) . . yes O12 Cu5 O14 163.2(2) . . yes O2 Cu5 O21 173.7(2) . . yes O12 Cu5 O21 87.95(19) . . yes O14 Cu5 O21 85.05(19) . . yes O2 Cu5 O20 84.41(19) . . yes O12 Cu5 O20 97.9(2) . . yes O14 Cu5 O20 97.2(2) . . yes O21 Cu5 O20 89.3(2) . . yes C1 N1 C10 115.4(4) . . ? C1 N1 C8 114.6(4) . . ? C10 N1 C8 109.9(4) . . ? C1 N1 Cu2 101.5(3) . . ? C10 N1 Cu2 104.2(4) . . ? C8 N1 Cu2 110.3(3) . . ? C6 C1 C2 119.4(5) . . ? C6 C1 N1 122.0(5) . . ? C2 C1 N1 118.5(5) . . ? C3 C2 C1 119.9(5) . . ? C3 C2 C7 117.3(5) . . ? C1 C2 C7 122.4(5) . . ? C2 C3 C4 121.2(6) . . ? C5 C4 C3 119.0(6) . . ? C4 C5 C6 121.4(6) . . ? C1 C6 C5 118.9(6) . . ? O2 C7 O1 124.4(5) . . ? O2 C7 C2 116.2(5) . . ? O1 C7 C2 119.4(5) . . ? C7 O1 Cu2 121.7(4) . . yes C7 O2 Cu5 126.6(4) . . yes N1 C8 C9 113.0(4) . . ? O4 C9 O3 127.4(5) . . ? O4 C9 C8 115.1(5) . . ? O3 C9 C8 117.5(5) . . ? C9 O3 Cu1 134.1(3) . . yes C9 O3 Cu2 111.4(3) . . yes Cu1 O3 Cu2 112.23(17) . . yes C9 O4 Cu4 128.2(3) . . yes N1 C10 C11 110.7(4) . . ? O6 C11 O5 123.4(6) . . ? O6 C11 C10 120.4(6) . . ? O5 C11 C10 116.1(5) . . ? C11 O5 Cu2 115.0(4) . . ? C12 N2 C19 110.7(5) . . ? C12 N2 C21 110.8(5) . . ? C19 N2 C21 109.7(5) . . ? C12 N2 Cu3 115.7(4) . . ? C19 N2 Cu3 107.6(3) . . ? C21 N2 Cu3 101.9(4) . . ? C13 C12 N2 119.8(7) . . ? C13 C12 C17 122.3(7) . . ? N2 C12 C17 117.1(8) . . ? C12 C13 C14 119.1(7) . . ? C12 C13 C18 127.5(8) . . ? C14 C13 C18 113.4(8) . . ? C13 C14 C15 119.9(9) . . ? C16 C15 C14 117.0(9) . . ? C15 C16 C17 122.1(10) . . ? C16 C17 C12 118.8(10) . . ? O8 C18 O7 122.4(6) . . ? O8 C18 C13 115.1(6) . . ? O7 C18 C13 122.4(7) . . ? C18 O7 Cu3 126.3(4) . . ? N2 C19 C20 114.1(5) . . ? O10 C20 O9 127.7(5) . . ? O10 C20 C19 116.6(5) . . ? O9 C20 C19 115.7(5) . . ? C20 O9 Cu1 134.9(3) . . yes C20 O9 Cu3 104.0(3) . . yes Cu1 O9 Cu3 121.02(16) . . yes C20 O10 Cu2 121.1(3) . . yes C22 C21 N2 111.3(6) . . ? O11 C22 O12 125.1(6) . . ? O11 C22 C21 116.9(7) . . ? O12 C22 C21 118.0(7) . . ? C22 O11 Cu3 118.3(4) . . yes C22 O12 Cu5 113.0(4) . . yes C23 N3 C32 115.6(5) . . ? C23 N3 C30 114.4(5) . . ? C32 N3 C30 109.5(5) . . ? C23 N3 Cu4 106.3(4) . . ? C32 N3 Cu4 101.9(3) . . ? C30 N3 Cu4 108.1(3) . . ? C28 C23 C24 119.7(6) . . ? C28 C23 N3 121.4(6) . . ? C24 C23 N3 118.9(5) . . ? C23 C24 C25 119.0(6) . . ? C23 C24 C29 124.0(5) . . ? C25 C24 C29 116.9(6) . . ? C26 C25 C24 120.1(8) . . ? C27 C26 C25 119.7(7) . . ? C28 C27 C26 120.5(7) . . ? C27 C28 C23 120.9(8) . . ? O13 C29 O14 123.3(6) . . ? O13 C29 C24 120.9(6) . . ? O14 C29 C24 115.8(5) . . ? C29 O13 Cu4 123.1(4) . . yes C29 O14 Cu5 116.2(4) . . yes N3 C30 C31 112.4(5) . . ? O15 C31 O16 127.2(5) . . ? O15 C31 C30 119.7(5) . . ? O16 C31 C30 113.1(5) . . ? C31 O15 Cu4 108.8(4) . . yes C31 O15 Cu1 136.3(3) . . yes Cu4 O15 Cu1 111.69(16) . . yes C31 O16 Cu3 128.1(4) . . yes N3 C32 C33 110.2(5) . . ? O18 C33 O17 123.8(6) . . ? O18 C33 C32 120.6(6) . . ? O17 C33 C32 115.5(5) . . ? C33 O17 Cu4 113.0(4) . . ? C34B O19 C34A 85.9(15) . . ? C34B O19 Cu3 109.8(12) . . ? C34A O19 Cu3 139.5(8) . . ? C35A O20 C35B 28(3) . . ? C35A O20 Cu5 132.7(16) . . ? C35B O20 Cu5 110.4(10) . . ? C36A O21 C36B 17.7(19) . . ? C36A O21 Cu5 128.1(10) . . ? C36B O21 Cu5 126.3(14) . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 1.437 _refine_diff_density_min -0.355 _refine_diff_density_rms 0.109