# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Plieger, Paul' 'Wenzel, Marco' 'Knapp, Quintin' _publ_contact_author_name 'Plieger, Paul' _publ_contact_author_email p.g.plieger@massey.ac.nz _publ_section_title ; A bis-salicylaldoximato-copper(II) receptor for selective sulfate uptake ; # Attachment 'NO3.cif' data_mw72c _database_code_depnum_ccdc_archive 'CCDC 783210' #TrackingRef 'NO3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H100 Cu2 N9 O11, 3(N O3)' _chemical_formula_sum 'C64 H100 Cu2 N12 O20' _chemical_formula_weight 1484.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 '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 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 11.847(2) _cell_length_b 19.317(4) _cell_length_c 37.831(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.95(3) _cell_angle_gamma 90.00 _cell_volume 8637(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 11394 _cell_measurement_theta_min 6.6 _cell_measurement_theta_max 66.5 _exptl_crystal_description chip _exptl_crystal_colour green _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.142 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3144 _exptl_absorpt_coefficient_mu 1.154 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8079 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details Empirical _exptl_special_details ; Absorption correction in FSP: Higashi, T. (1995). ABSCOR: Empirical Absorption Correction based on Fourier Series Approximation. Rigaku Corporation, 3-9-12 Matsubara, Akishima, Tokyo 196-8666, JAPAN. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'confocal optics' _diffrn_measurement_device_type 'Rigaku Spider' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 84887 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 6.56 _diffrn_reflns_theta_max 61.16 _reflns_number_total 13237 _reflns_number_gt 9141 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crystal Clear (Rigaku, 2005)' _computing_cell_refinement 'FS Process (Rigaku, 1998)' _computing_data_reduction 'FS Process (Rigaku, 1998)' _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. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.065 0.435 0.000 969 125 ' ' 2 -0.226 0.226 0.500 969 125 ' ' _platon_squeeze_details ; 250 e- per cell, approximating to 2(CH3CH2OH) and 0.75(H2O) (= 61.5 e-) per formula unit ; _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^)+(0.1613P)^2^+5.7876P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13237 _refine_ls_number_parameters 974 _refine_ls_number_restraints 81 _refine_ls_R_factor_all 0.1092 _refine_ls_R_factor_gt 0.0860 _refine_ls_wR_factor_ref 0.2767 _refine_ls_wR_factor_gt 0.2575 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _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 0.66667(5) 0.96344(4) 0.274701(18) 0.0555(2) Uani 1 1 d . . . Cu2 Cu 0.84221(6) 0.63936(4) 0.28891(2) 0.0659(3) Uani 1 1 d . . . O11 O 0.5915(3) 0.95248(17) 0.22901(9) 0.0627(9) Uani 1 1 d . . . C11 C 0.6342(4) 0.9569(2) 0.19754(13) 0.0565(12) Uani 1 1 d . . . C21 C 0.7394(4) 0.9890(3) 0.19217(14) 0.0603(12) Uani 1 1 d . . . C211 C 0.8096(4) 1.0187(3) 0.22090(14) 0.0584(12) Uani 1 1 d . . . H21A H 0.8735 1.0431 0.2152 0.070 Uiso 1 1 calc R . . N212 N 0.7907(3) 1.0139(2) 0.25389(12) 0.0605(10) Uani 1 1 d . . . O213 O 0.8727(3) 1.0480(2) 0.27593(10) 0.0754(10) Uani 1 1 d . . . H213 H 0.8700 1.0338 0.2963 0.113 Uiso 1 1 calc R . . C31 C 0.7747(5) 0.9930(3) 0.15786(14) 0.0667(14) Uani 1 1 d . . . H31A H 0.8432 1.0146 0.1543 0.080 Uiso 1 1 calc R . . C41 C 0.7121(5) 0.9661(3) 0.12888(15) 0.0727(15) Uani 1 1 d . . . C411 C 0.7527(7) 0.9696(4) 0.09054(18) 0.100(2) Uani 1 1 d . . . C412 C 0.8538(9) 1.0161(7) 0.0886(2) 0.174(5) Uani 1 1 d . . . H41A H 0.8780 1.0158 0.0649 0.260 Uiso 1 1 calc R . . H41B H 0.9142 0.9998 0.1047 0.260 Uiso 1 1 calc R . . H41C H 0.8339 1.0624 0.0949 0.260 Uiso 1 1 calc R . . C413 C 0.6567(8) 0.9970(5) 0.06485(19) 0.125(3) Uani 1 1 d . . . H41D H 0.6818 0.9985 0.0413 0.187 Uiso 1 1 calc R . . H41E H 0.6358 1.0427 0.0719 0.187 Uiso 1 1 calc R . . H41F H 0.5924 0.9668 0.0653 0.187 Uiso 1 1 calc R . . C414 C 0.7826(9) 0.8938(5) 0.0793(2) 0.145(4) Uani 1 1 d . . . H41G H 0.8095 0.8945 0.0559 0.218 Uiso 1 1 calc R . . H41H H 0.7162 0.8653 0.0793 0.218 Uiso 1 1 calc R . . H41I H 0.8403 0.8754 0.0957 0.218 Uiso 1 1 calc R . . C51 C 0.6136(5) 0.9327(3) 0.13532(14) 0.0697(14) Uani 1 1 d . . . H51A H 0.5716 0.9132 0.1162 0.084 Uiso 1 1 calc R . . C61 C 0.5731(4) 0.9262(3) 0.16841(13) 0.0583(12) Uani 1 1 d . . . C611 C 0.4718(4) 0.8856(3) 0.17488(14) 0.0633(13) Uani 1 1 d . . . H61A H 0.4321 0.8736 0.1524 0.076 Uiso 1 1 calc R . . H61B H 0.4214 0.9132 0.1883 0.076 Uiso 1 1 calc R . . N612 N 0.5033(3) 0.8208(2) 0.19500(11) 0.0618(10) Uani 1 1 d . . . H612 H 0.5538 0.8332 0.2131 0.074 Uiso 1 1 calc R . . C613 C 0.5626(5) 0.7707(3) 0.17246(18) 0.0859(18) Uani 1 1 d . . . H61C H 0.6268 0.7929 0.1632 0.129 Uiso 1 1 calc R . . H61D H 0.5115 0.7555 0.1532 0.129 Uiso 1 1 calc R . . H61E H 0.5876 0.7315 0.1865 0.129 Uiso 1 1 calc R . . C614 C 0.4037(4) 0.7888(3) 0.21145(14) 0.0659(13) Uani 1 1 d . . . H61F H 0.3623 0.8246 0.2231 0.079 Uiso 1 1 calc R . . H61G H 0.3532 0.7685 0.1930 0.079 Uiso 1 1 calc R . . C615 C 0.4401(5) 0.7342(3) 0.23785(16) 0.0742(15) Uani 1 1 d . . . H61H H 0.5002 0.7523 0.2540 0.089 Uiso 1 1 calc R . . H61I H 0.4697 0.6947 0.2256 0.089 Uiso 1 1 calc R . . C616 C 0.3408(6) 0.7109(3) 0.25903(17) 0.0877(18) Uani 1 1 d . . . H61J H 0.3076 0.7514 0.2693 0.105 Uiso 1 1 calc R . . H61K H 0.2836 0.6901 0.2428 0.105 Uiso 1 1 calc R . . O12 O 0.7777(3) 0.6458(2) 0.33367(10) 0.0797(11) Uani 1 1 d . . . C12 C 0.8297(5) 0.6521(3) 0.36525(18) 0.0834(17) Uani 1 1 d . . . C22 C 0.9468(5) 0.6673(3) 0.37166(17) 0.0793(16) Uani 1 1 d . . . C221 C 1.0219(5) 0.6756(3) 0.34286(19) 0.0778(16) Uani 1 1 d . . . H22A H 1.0973 0.6866 0.3487 0.093 Uiso 1 1 calc R . . N222 N 0.9895(4) 0.6685(2) 0.31035(14) 0.0698(12) Uani 1 1 d . . . O223 O 1.0765(3) 0.6803(2) 0.28768(11) 0.0801(11) Uani 1 1 d . . . H223 H 1.0520 0.6748 0.2671 0.120 Uiso 1 1 calc R . . C32 C 0.9911(5) 0.6748(4) 0.40725(18) 0.0879(18) Uani 1 1 d . . . H32A H 1.0676 0.6851 0.4112 0.105 Uiso 1 1 calc R . . C42 C 0.9277(5) 0.6677(4) 0.43634(19) 0.0915(19) Uani 1 1 d . . . C421 C 0.9765(6) 0.6712(5) 0.4755(2) 0.106(2) Uani 1 1 d . . . C422 C 1.1035(6) 0.6852(4) 0.4769(2) 0.111(2) Uani 1 1 d . . . H42A H 1.1331 0.6867 0.5012 0.167 Uiso 1 1 calc R . . H42B H 1.1170 0.7287 0.4657 0.167 Uiso 1 1 calc R . . H42C H 1.1404 0.6489 0.4647 0.167 Uiso 1 1 calc R . . C423 C 0.9170(8) 0.7245(6) 0.4947(2) 0.145(4) Uani 1 1 d . . . H42D H 0.9476 0.7263 0.5189 0.218 Uiso 1 1 calc R . . H42E H 0.8379 0.7134 0.4942 0.218 Uiso 1 1 calc R . . H42F H 0.9266 0.7687 0.4837 0.218 Uiso 1 1 calc R . . C424 C 0.9588(7) 0.5996(5) 0.4940(2) 0.119(3) Uani 1 1 d . . . H42G H 0.9898 0.6017 0.5181 0.179 Uiso 1 1 calc R . . H42H H 0.9965 0.5639 0.4816 0.179 Uiso 1 1 calc R . . H42I H 0.8794 0.5894 0.4936 0.179 Uiso 1 1 calc R . . C52 C 0.8122(6) 0.6523(4) 0.42944(19) 0.102(2) Uani 1 1 d . . . H52A H 0.7662 0.6493 0.4483 0.122 Uiso 1 1 calc R . . C62 C 0.7654(6) 0.6414(4) 0.39559(19) 0.095(2) Uani 1 1 d . . . C621 C 0.6396(6) 0.6199(4) 0.3893(2) 0.102(2) Uani 1 1 d . . . H62A H 0.6343 0.5723 0.3813 0.122 Uiso 1 1 calc R . . H62B H 0.6018 0.6238 0.4112 0.122 Uiso 1 1 calc R . . N622 N 0.5875(5) 0.6650(4) 0.36294(15) 0.1034(19) Uani 1 1 d . . . H622 H 0.6346 0.6651 0.3449 0.124 Uiso 1 1 calc R . . C623 C 0.5853(7) 0.7430(4) 0.3765(2) 0.112(2) Uani 1 1 d . . . H62C H 0.6594 0.7559 0.3861 0.168 Uiso 1 1 calc R . . H62D H 0.5325 0.7471 0.3946 0.168 Uiso 1 1 calc R . . H62E H 0.5626 0.7730 0.3571 0.168 Uiso 1 1 calc R . . C624 C 0.4750(5) 0.6408(4) 0.34663(17) 0.091(2) Uani 1 1 d . . . H62F H 0.4159 0.6466 0.3629 0.109 Uiso 1 1 calc R . . H62G H 0.4781 0.5925 0.3397 0.109 Uiso 1 1 calc R . . C625 C 0.4547(6) 0.6892(4) 0.3134(2) 0.106(2) Uani 1 1 d . . . H62H H 0.4299 0.7343 0.3210 0.127 Uiso 1 1 calc R . . H62I H 0.5255 0.6953 0.3023 0.127 Uiso 1 1 calc R . . C626 C 0.3708(6) 0.6608(4) 0.28777(17) 0.0897(18) Uani 1 1 d . . . H62J H 0.3033 0.6488 0.2996 0.108 Uiso 1 1 calc R . . H62K H 0.4000 0.6188 0.2777 0.108 Uiso 1 1 calc R . . O13 O 0.8991(3) 0.6547(2) 0.24376(11) 0.0751(10) Uani 1 1 d . . . C13 C 0.8494(5) 0.6458(3) 0.21157(17) 0.0724(15) Uani 1 1 d . . . C23 C 0.7420(5) 0.6117(3) 0.20547(16) 0.0686(14) Uani 1 1 d . . . C231 C 0.6814(5) 0.5841(3) 0.23403(16) 0.0667(14) Uani 1 1 d . . . H23A H 0.6143 0.5607 0.2280 0.080 Uiso 1 1 calc R . . N232 N 0.7120(3) 0.5892(2) 0.26712(12) 0.0628(11) Uani 1 1 d . . . O233 O 0.6377(3) 0.55493(19) 0.28881(10) 0.0751(10) Uani 1 1 d . . . H233 H 0.6497 0.5679 0.3094 0.113 Uiso 1 1 calc R . . C33 C 0.6989(5) 0.6020(3) 0.17036(17) 0.0777(16) Uani 1 1 d . . . H33A H 0.6307 0.5785 0.1664 0.093 Uiso 1 1 calc R . . C43 C 0.7521(6) 0.6254(3) 0.14150(17) 0.0860(18) Uani 1 1 d . . . C431 C 0.7030(7) 0.6151(4) 0.10349(18) 0.101(2) Uani 1 1 d . . . C432 C 0.6068(10) 0.5666(6) 0.1003(2) 0.172(5) Uani 1 1 d . . . H43A H 0.5798 0.5627 0.0759 0.258 Uiso 1 1 calc R . . H43B H 0.5471 0.5836 0.1139 0.258 Uiso 1 1 calc R . . H43C H 0.6308 0.5220 0.1091 0.258 Uiso 1 1 calc R . . C433 C 0.7952(10) 0.5901(7) 0.0788(3) 0.174(5) Uani 1 1 d . . . H43D H 0.7619 0.5842 0.0552 0.262 Uiso 1 1 calc R . . H43E H 0.8259 0.5467 0.0874 0.262 Uiso 1 1 calc R . . H43F H 0.8546 0.6239 0.0788 0.262 Uiso 1 1 calc R . . C434 C 0.6643(13) 0.6839(6) 0.0892(2) 0.191(6) Uani 1 1 d . . . H43G H 0.6329 0.6785 0.0653 0.286 Uiso 1 1 calc R . . H43H H 0.7274 0.7151 0.0896 0.286 Uiso 1 1 calc R . . H43I H 0.6076 0.7023 0.1036 0.286 Uiso 1 1 calc R . . C53 C 0.8539(6) 0.6611(3) 0.14850(18) 0.0854(18) Uani 1 1 d . . . H53A H 0.8915 0.6783 0.1296 0.102 Uiso 1 1 calc R . . C63 C 0.9002(5) 0.6716(3) 0.18238(17) 0.0754(15) Uani 1 1 d . . . C631 C 1.0037(5) 0.7161(3) 0.18963(18) 0.0886(18) Uani 1 1 d . B . H63A H 1.0558 0.6934 0.2069 0.106 Uiso 1 1 calc R . . H63B H 1.0418 0.7223 0.1680 0.106 Uiso 1 1 calc R . . N632 N 0.9702(4) 0.7852(3) 0.20355(14) 0.0843(14) Uani 1 1 d D . . H632 H 0.9230 0.7776 0.2211 0.101 Uiso 1 1 calc R A 1 C633 C 0.9074(6) 0.8281(4) 0.1755(2) 0.114(3) Uani 1 1 d . B . H63C H 0.8420 0.8031 0.1661 0.171 Uiso 1 1 calc R . . H63D H 0.9561 0.8377 0.1569 0.171 Uiso 1 1 calc R . . H63E H 0.8840 0.8708 0.1858 0.171 Uiso 1 1 calc R . . C634 C 1.0814(15) 0.8190(17) 0.2207(14) 0.092(7) Uani 0.60 1 d PD B 1 H63F H 1.1213 0.7855 0.2360 0.138 Uiso 0.60 1 calc PR B 1 H63G H 1.1303 0.8314 0.2021 0.138 Uiso 0.60 1 calc PR B 1 C635 C 1.058(2) 0.8789(14) 0.2405(8) 0.194(19) Uani 0.60 1 d PD B 1 H63H H 1.0143 0.8631 0.2597 0.291 Uiso 0.60 1 calc PR B 1 H63I H 1.0072 0.9068 0.2252 0.291 Uiso 0.60 1 calc PR B 1 C636 C 1.1396(12) 0.9256(12) 0.2562(3) 0.182(14) Uani 0.60 1 d PD B 1 H63J H 1.1999 0.9327 0.2405 0.273 Uiso 0.60 1 calc PR B 1 H63K H 1.1047 0.9699 0.2605 0.273 Uiso 0.60 1 calc PR B 1 C63A C 1.0666(17) 0.833(2) 0.2202(18) 0.088(14) Uani 0.40 1 d PD B 2 H63L H 1.1075 0.8078 0.2391 0.131 Uiso 0.40 1 calc PR B 2 H63M H 1.1192 0.8422 0.2022 0.131 Uiso 0.40 1 calc PR B 2 C63B C 1.0342(16) 0.8978(10) 0.2342(7) 0.057(4) Uani 0.40 1 d PD B 2 H63N H 1.0022 0.9259 0.2147 0.085 Uiso 0.40 1 calc PR B 2 H63O H 0.9745 0.8895 0.2500 0.085 Uiso 0.40 1 calc PR B 2 C63C C 1.120(2) 0.9366(10) 0.2527(6) 0.23(3) Uani 0.40 1 d PD B 2 H63P H 1.1901 0.9164 0.2457 0.342 Uiso 0.40 1 calc PR B 2 H63Q H 1.1156 0.9820 0.2418 0.342 Uiso 0.40 1 calc PR B 2 O14 O 0.7484(3) 0.9485(2) 0.31905(9) 0.0685(9) Uani 1 1 d . . . C14 C 0.7062(4) 0.9380(3) 0.34967(14) 0.0684(14) Uani 1 1 d . . . C24 C 0.5922(4) 0.9229(3) 0.35487(13) 0.0616(13) Uani 1 1 d . . . C241 C 0.5077(4) 0.9185(2) 0.32607(14) 0.0580(12) Uani 1 1 d . . . H24A H 0.4350 0.9053 0.3310 0.070 Uiso 1 1 calc R . . N242 N 0.5265(3) 0.9316(2) 0.29419(11) 0.0549(9) Uani 1 1 d . . . O243 O 0.4314(3) 0.92361(19) 0.27025(9) 0.0683(9) Uani 1 1 d . . . H243 H 0.4488 0.9325 0.2501 0.102 Uiso 1 1 calc R . . C34 C 0.5583(5) 0.9114(3) 0.38976(13) 0.0641(13) Uani 1 1 d . . . H34A H 0.4824 0.9026 0.3929 0.077 Uiso 1 1 calc R . . C44 C 0.6345(5) 0.9127(3) 0.41928(14) 0.0731(15) Uani 1 1 d . . . C441 C 0.5976(6) 0.8997(3) 0.45720(16) 0.0836(17) Uani 1 1 d . . . C442 C 0.6590(8) 0.8362(4) 0.47213(18) 0.119(3) Uani 1 1 d . . . H44A H 0.6376 0.8278 0.4958 0.178 Uiso 1 1 calc R . . H44B H 0.7392 0.8437 0.4726 0.178 Uiso 1 1 calc R . . H44C H 0.6390 0.7969 0.4575 0.178 Uiso 1 1 calc R . . C443 C 0.6301(6) 0.9655(4) 0.47914(17) 0.096(2) Uani 1 1 d . . . H44D H 0.6107 0.9591 0.5031 0.145 Uiso 1 1 calc R . . H44E H 0.5898 1.0047 0.4690 0.145 Uiso 1 1 calc R . . H44F H 0.7100 0.9735 0.4788 0.145 Uiso 1 1 calc R . . C444 C 0.4730(6) 0.8895(4) 0.45875(16) 0.0917(19) Uani 1 1 d . . . H44G H 0.4560 0.8809 0.4828 0.137 Uiso 1 1 calc R . . H44H H 0.4491 0.8507 0.4442 0.137 Uiso 1 1 calc R . . H44I H 0.4340 0.9304 0.4502 0.137 Uiso 1 1 calc R . . C54 C 0.7450(6) 0.9282(4) 0.41337(16) 0.097(2) Uani 1 1 d . . . H54A H 0.7975 0.9292 0.4328 0.116 Uiso 1 1 calc R . . C64 C 0.7836(5) 0.9427(4) 0.38005(17) 0.094(2) Uani 1 1 d . . . C641 C 0.9114(6) 0.9652(4) 0.3710(2) 0.114(3) Uani 1 1 d . . . H64A H 0.9105 1.0081 0.3576 0.137 Uiso 1 1 calc R . . H64B H 0.9602 0.9707 0.3925 0.137 Uiso 1 1 calc R . . N642 N 0.9467(5) 0.9096(4) 0.35059(18) 0.119(2) Uani 1 1 d D . . H642 H 0.8920 0.9069 0.3325 0.143 Uiso 1 1 calc R C 1 C643 C 0.9509(8) 0.8382(5) 0.3653(3) 0.140(3) Uani 1 1 d . . . H64C H 0.8805 0.8278 0.3754 0.210 Uiso 1 1 calc R . . H64D H 1.0116 0.8348 0.3834 0.210 Uiso 1 1 calc R . . H64E H 0.9632 0.8057 0.3468 0.210 Uiso 1 1 calc R . . C644 C 1.0565(10) 0.9279(7) 0.3313(4) 0.081(4) Uani 0.60 1 d PD B 1 H64F H 1.0388 0.9655 0.3149 0.122 Uiso 0.60 1 calc PR B 1 H64G H 1.1134 0.9446 0.3490 0.122 Uiso 0.60 1 calc PR B 1 C645 C 1.1038(10) 0.8729(6) 0.3125(4) 0.094(4) Uani 0.60 1 d PD B 1 H64H H 1.0433 0.8478 0.2995 0.141 Uiso 0.60 1 calc PR B 1 H64I H 1.1417 0.8411 0.3292 0.141 Uiso 0.60 1 calc PR B 1 C646 C 1.1828(8) 0.8965(6) 0.2881(3) 0.093(4) Uani 0.60 1 d PD B 1 H64J H 1.2316 0.9305 0.3002 0.140 Uiso 0.60 1 calc PR B 1 H64K H 1.2301 0.8575 0.2826 0.140 Uiso 0.60 1 calc PR B 1 C64A C 1.053(2) 0.9563(15) 0.3435(6) 0.149(15) Uani 0.40 1 d PD B 2 H64L H 1.0345 1.0046 0.3392 0.224 Uiso 0.40 1 calc PR B 2 H64M H 1.1151 0.9516 0.3614 0.224 Uiso 0.40 1 calc PR B 2 C64B C 1.067(3) 0.9180(19) 0.3124(6) 0.30(4) Uani 0.40 1 d PD B 2 H64N H 0.9941 0.9111 0.2999 0.451 Uiso 0.40 1 calc PR B 2 H64O H 1.0977 0.8728 0.3190 0.451 Uiso 0.40 1 calc PR B 2 C64C C 1.1404(17) 0.9500(14) 0.2892(6) 0.129(10) Uani 0.40 1 d PD B 2 H64P H 1.1363 0.9997 0.2927 0.193 Uiso 0.40 1 calc PR B 2 H64Q H 1.2173 0.9358 0.2962 0.193 Uiso 0.40 1 calc PR B 2 N1 N 0.7537(4) 0.8001(3) 0.2641(2) 0.0895(17) Uani 1 1 d . . . O1 O 0.8527(4) 0.7979(3) 0.27680(17) 0.1292(19) Uani 1 1 d . . . O2 O 0.7293(8) 0.8156(4) 0.2353(3) 0.212(5) Uani 1 1 d . . . O3 O 0.6789(6) 0.7961(6) 0.2810(3) 0.252(7) Uani 1 1 d . . . N2 N 0.3347(5) 0.6100(2) 0.17350(14) 0.0777(13) Uani 1 1 d . . . O4 O 0.3868(5) 0.6412(3) 0.15091(14) 0.1162(17) Uani 1 1 d . . . O5 O 0.3874(3) 0.5793(2) 0.19853(12) 0.0820(11) Uani 1 1 d . . . O6 O 0.2278(4) 0.6101(2) 0.17109(11) 0.0834(11) Uani 1 1 d . . . N3 N 0.8629(5) 0.4833(3) 0.3374(2) 0.1021(18) Uani 1 1 d . . . O7 O 0.7560(4) 0.4853(2) 0.33873(14) 0.0978(14) Uani 1 1 d . . . O8 O 0.9121(4) 0.5189(3) 0.31688(18) 0.1183(19) Uani 1 1 d . . . O9 O 0.9177(5) 0.4418(4) 0.3577(2) 0.159(3) Uani 1 1 d . . . N4 N 1.2719(15) 0.8039(7) 0.3872(4) 0.113(6) Uani 0.60 1 d PD D 1 O21 O 1.2665(15) 0.8648(8) 0.3856(4) 0.175(7) Uani 0.60 1 d PD D 1 O22 O 1.275(2) 0.7722(12) 0.3605(6) 0.294(14) Uani 0.60 1 d PD D 1 O23 O 1.2433(12) 0.7752(9) 0.4125(4) 0.138(4) Uani 0.60 1 d PD D 1 N5 N 1.266(3) 0.7850(12) 0.3882(7) 0.56(10) Uani 0.40 1 d PD E 2 O31 O 1.250(5) 0.809(2) 0.4163(11) 0.38(4) Uani 0.40 1 d PD E 2 O32 O 1.325(2) 0.8164(17) 0.3698(10) 0.243(17) Uani 0.40 1 d PD E 2 O33 O 1.269(2) 0.7237(12) 0.3865(8) 0.25(2) Uani 0.40 1 d PD E 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 0.0442(4) 0.0619(5) 0.0610(5) 0.0006(3) 0.0072(3) 0.0015(3) Cu2 0.0504(4) 0.0656(5) 0.0818(6) -0.0021(4) 0.0066(4) 0.0008(3) O11 0.0508(19) 0.071(2) 0.068(2) 0.0009(17) 0.0130(16) -0.0012(15) C11 0.055(3) 0.054(3) 0.061(3) 0.006(2) 0.013(2) 0.004(2) C21 0.056(3) 0.056(3) 0.071(3) 0.005(2) 0.013(2) 0.000(2) C211 0.049(3) 0.057(3) 0.070(3) 0.002(2) 0.011(2) -0.004(2) N212 0.048(2) 0.064(3) 0.069(3) -0.006(2) 0.004(2) -0.0043(19) O213 0.060(2) 0.091(3) 0.075(2) -0.006(2) 0.0020(18) -0.0211(19) C31 0.069(3) 0.066(3) 0.068(3) 0.007(3) 0.022(3) -0.004(3) C41 0.083(4) 0.074(4) 0.062(3) 0.007(3) 0.015(3) -0.013(3) C411 0.111(5) 0.123(6) 0.069(4) -0.002(4) 0.029(4) -0.035(4) C412 0.166(9) 0.278(13) 0.081(5) 0.001(6) 0.037(5) -0.132(9) C413 0.154(8) 0.153(7) 0.068(4) 0.029(5) 0.013(5) -0.019(6) C414 0.213(11) 0.135(7) 0.096(6) -0.008(5) 0.073(6) 0.022(7) C51 0.072(4) 0.080(4) 0.057(3) -0.003(3) 0.005(3) -0.003(3) C61 0.051(3) 0.062(3) 0.061(3) 0.004(2) 0.001(2) 0.002(2) C611 0.060(3) 0.070(3) 0.059(3) 0.003(2) 0.002(2) 0.004(3) N612 0.052(2) 0.064(3) 0.069(3) -0.009(2) 0.008(2) -0.0079(19) C613 0.087(4) 0.073(4) 0.102(5) -0.014(3) 0.039(4) -0.011(3) C614 0.063(3) 0.067(3) 0.068(3) -0.005(3) 0.014(3) -0.012(3) C615 0.069(3) 0.073(4) 0.081(4) -0.003(3) 0.006(3) -0.013(3) C616 0.092(4) 0.080(4) 0.094(4) 0.014(3) 0.024(4) -0.004(3) O12 0.056(2) 0.108(3) 0.075(3) -0.013(2) 0.0011(19) 0.001(2) C12 0.059(3) 0.103(5) 0.088(4) -0.017(4) 0.003(3) 0.006(3) C22 0.050(3) 0.097(4) 0.090(4) -0.012(3) -0.002(3) 0.005(3) C221 0.053(3) 0.068(4) 0.112(5) 0.004(3) 0.003(3) 0.000(3) N222 0.053(3) 0.066(3) 0.090(3) 0.007(2) 0.006(2) 0.001(2) O223 0.052(2) 0.086(3) 0.103(3) 0.019(2) 0.010(2) -0.0082(18) C32 0.059(3) 0.111(5) 0.092(5) -0.016(4) -0.004(3) 0.000(3) C42 0.058(4) 0.115(5) 0.099(5) -0.019(4) -0.007(3) 0.004(3) C421 0.070(4) 0.154(7) 0.091(5) -0.022(5) -0.006(4) 0.015(4) C422 0.075(4) 0.141(7) 0.113(6) -0.004(5) -0.023(4) 0.002(4) C423 0.109(6) 0.193(9) 0.128(7) -0.059(7) -0.037(5) 0.053(6) C424 0.098(6) 0.150(7) 0.109(6) 0.017(5) 0.002(4) -0.002(5) C52 0.069(4) 0.154(7) 0.082(4) -0.010(4) -0.001(3) 0.008(4) C62 0.069(4) 0.129(6) 0.089(5) -0.010(4) 0.008(4) 0.001(4) C621 0.080(4) 0.120(6) 0.107(5) 0.010(4) 0.011(4) 0.021(4) N622 0.081(4) 0.153(6) 0.079(4) 0.010(4) 0.024(3) 0.024(4) C623 0.132(7) 0.103(6) 0.102(5) -0.002(4) 0.016(5) 0.014(5) C624 0.059(4) 0.123(5) 0.088(4) -0.020(4) -0.016(3) 0.021(3) C625 0.073(4) 0.123(6) 0.121(6) 0.027(5) 0.009(4) -0.007(4) C626 0.097(5) 0.092(4) 0.080(4) 0.007(3) 0.006(4) -0.011(4) O13 0.059(2) 0.086(3) 0.080(3) 0.005(2) 0.0012(19) -0.0045(18) C13 0.070(4) 0.056(3) 0.094(4) -0.009(3) 0.018(3) -0.001(3) C23 0.072(3) 0.055(3) 0.080(4) -0.010(3) 0.014(3) 0.000(3) C231 0.059(3) 0.057(3) 0.086(4) -0.009(3) 0.016(3) -0.007(2) N232 0.055(2) 0.060(2) 0.075(3) 0.000(2) 0.016(2) -0.0012(19) O233 0.057(2) 0.082(2) 0.088(3) -0.005(2) 0.0159(19) -0.0129(18) C33 0.084(4) 0.063(3) 0.088(4) -0.017(3) 0.017(3) -0.011(3) C43 0.105(5) 0.078(4) 0.077(4) -0.021(3) 0.024(4) -0.012(4) C431 0.124(6) 0.107(5) 0.075(4) -0.028(4) 0.021(4) -0.022(5) C432 0.215(12) 0.212(11) 0.089(6) -0.024(6) 0.002(6) -0.112(10) C433 0.185(11) 0.225(12) 0.116(7) -0.072(8) 0.034(7) -0.023(9) C434 0.319(18) 0.152(9) 0.090(6) -0.029(6) -0.067(8) 0.025(10) C53 0.099(5) 0.081(4) 0.080(4) -0.008(3) 0.030(4) -0.007(4) C63 0.072(4) 0.070(4) 0.086(4) -0.003(3) 0.023(3) -0.005(3) C631 0.073(4) 0.098(5) 0.096(5) 0.014(4) 0.024(3) -0.004(3) N632 0.068(3) 0.086(3) 0.099(4) 0.003(3) 0.010(3) -0.014(3) C633 0.082(5) 0.094(5) 0.160(7) 0.030(5) -0.030(5) -0.011(4) C634 0.073(11) 0.098(10) 0.105(18) 0.006(11) 0.010(15) -0.021(10) C635 0.16(3) 0.31(4) 0.12(2) -0.05(2) 0.071(19) -0.08(3) C636 0.099(11) 0.39(4) 0.057(7) -0.020(12) -0.003(7) -0.167(17) C63A 0.037(10) 0.15(4) 0.07(2) 0.01(2) -0.004(11) 0.006(13) C63B 0.032(7) 0.073(9) 0.066(11) -0.020(8) 0.000(7) -0.029(7) C63C 0.19(4) 0.061(15) 0.45(8) 0.07(3) 0.15(5) 0.07(2) O14 0.0505(19) 0.088(3) 0.067(2) 0.0033(18) 0.0066(17) 0.0074(17) C14 0.056(3) 0.091(4) 0.058(3) 0.006(3) 0.006(3) 0.007(3) C24 0.058(3) 0.065(3) 0.062(3) -0.001(2) 0.006(2) 0.002(2) C241 0.050(3) 0.057(3) 0.067(3) 0.003(2) 0.004(2) -0.002(2) N242 0.046(2) 0.060(2) 0.059(2) 0.0013(19) 0.0027(19) 0.0019(18) O243 0.0504(19) 0.089(3) 0.066(2) 0.0020(18) 0.0026(16) -0.0090(17) C34 0.062(3) 0.069(3) 0.062(3) -0.001(2) 0.010(3) 0.004(2) C44 0.071(4) 0.092(4) 0.057(3) -0.001(3) 0.010(3) 0.014(3) C441 0.088(4) 0.098(4) 0.065(4) 0.002(3) 0.001(3) 0.017(3) C442 0.160(8) 0.122(6) 0.076(4) 0.029(4) 0.023(5) 0.047(6) C443 0.092(5) 0.129(6) 0.070(4) -0.013(4) 0.020(3) 0.005(4) C444 0.097(5) 0.112(5) 0.068(4) 0.003(3) 0.029(3) -0.010(4) C54 0.077(4) 0.152(6) 0.060(4) -0.007(4) -0.004(3) 0.028(4) C64 0.058(3) 0.153(6) 0.072(4) 0.000(4) 0.007(3) 0.005(4) C641 0.092(5) 0.125(6) 0.117(6) -0.044(5) -0.044(4) 0.039(4) N642 0.074(4) 0.158(7) 0.121(5) -0.001(5) -0.023(4) 0.028(4) C643 0.117(7) 0.154(8) 0.147(8) 0.010(7) 0.003(6) 0.037(6) C644 0.061(7) 0.142(11) 0.045(12) 0.000(7) 0.027(7) 0.013(7) C645 0.063(9) 0.092(8) 0.124(12) -0.022(7) -0.012(7) -0.001(6) C646 0.053(6) 0.083(8) 0.149(12) -0.020(8) 0.036(7) -0.007(5) C64A 0.072(13) 0.34(5) 0.035(13) 0.016(18) 0.034(10) 0.05(2) C64B 0.076(18) 0.78(12) 0.049(16) -0.06(3) 0.040(15) -0.10(4) C64C 0.052(10) 0.15(2) 0.19(3) -0.075(19) 0.024(13) -0.030(12) N1 0.043(3) 0.069(3) 0.157(6) 0.002(3) 0.017(3) -0.003(2) O1 0.062(3) 0.144(5) 0.180(5) 0.041(4) 0.005(3) 0.020(3) O2 0.187(8) 0.200(8) 0.234(9) 0.137(7) -0.093(7) -0.079(6) O3 0.101(5) 0.346(14) 0.317(12) -0.195(11) 0.066(7) -0.085(7) N2 0.089(4) 0.062(3) 0.082(3) -0.003(3) 0.010(3) -0.019(3) O4 0.116(4) 0.127(4) 0.106(4) 0.022(3) 0.014(3) -0.043(3) O5 0.078(3) 0.065(2) 0.101(3) 0.010(2) -0.004(2) -0.0091(19) O6 0.077(3) 0.077(3) 0.096(3) 0.015(2) 0.006(2) 0.000(2) N3 0.077(4) 0.074(4) 0.155(6) 0.006(4) 0.013(4) 0.019(3) O7 0.070(3) 0.085(3) 0.139(4) 0.019(3) 0.014(3) 0.005(2) O8 0.074(3) 0.084(3) 0.201(6) 0.027(3) 0.041(3) 0.007(2) O9 0.099(4) 0.167(6) 0.212(7) 0.063(5) 0.024(4) 0.048(4) N4 0.079(11) 0.120(12) 0.138(17) 0.049(12) -0.003(10) -0.010(9) O21 0.141(12) 0.219(17) 0.154(12) 0.052(12) -0.079(10) -0.066(11) O22 0.24(3) 0.31(3) 0.35(3) -0.08(3) 0.14(2) -0.01(2) O23 0.134(10) 0.146(12) 0.135(11) 0.035(9) 0.007(9) -0.029(8) N5 0.054(19) 1.4(3) 0.25(5) -0.49(11) 0.06(2) -0.08(5) O31 0.50(9) 0.22(5) 0.44(8) -0.11(5) 0.11(6) -0.04(4) O32 0.17(2) 0.23(3) 0.34(4) -0.04(2) 0.13(2) -0.14(2) O33 0.058(11) 0.55(6) 0.13(2) 0.06(3) 0.003(12) -0.03(2) _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 O14 1.900(4) . ? Cu1 O11 1.901(4) . ? Cu1 N242 1.961(4) . ? Cu1 N212 1.973(4) . ? Cu2 O13 1.902(4) . ? Cu2 O12 1.909(4) . ? Cu2 N232 1.954(4) . ? Cu2 N222 1.956(5) . ? O11 C11 1.328(6) . ? C11 C61 1.406(7) . ? C11 C21 1.419(7) . ? C21 C31 1.393(7) . ? C21 C211 1.442(7) . ? C211 N212 1.286(6) . ? N212 O213 1.400(5) . ? C31 C41 1.382(8) . ? C41 C51 1.369(8) . ? C41 C411 1.561(8) . ? C411 C412 1.503(10) . ? C411 C413 1.538(11) . ? C411 C414 1.572(11) . ? C51 C61 1.377(7) . ? C61 C611 1.469(7) . ? C611 N612 1.498(6) . ? N612 C613 1.497(7) . ? N612 C614 1.505(6) . ? C614 C615 1.495(8) . ? C615 C616 1.536(8) . ? C616 C626 1.480(9) . ? O12 C12 1.312(7) . ? C12 C22 1.422(8) . ? C12 C62 1.435(9) . ? C22 C32 1.418(8) . ? C22 C221 1.462(9) . ? C221 N222 1.270(7) . ? N222 O223 1.404(6) . ? C32 C42 1.381(9) . ? C42 C52 1.408(9) . ? C42 C421 1.553(9) . ? C421 C423 1.470(11) . ? C421 C422 1.526(10) . ? C421 C424 1.571(11) . ? C52 C62 1.376(9) . ? C62 C621 1.550(10) . ? C621 N622 1.431(9) . ? N622 C624 1.505(8) . ? N622 C623 1.593(10) . ? C624 C625 1.573(9) . ? C625 C626 1.448(9) . ? O13 C13 1.327(7) . ? C13 C63 1.386(8) . ? C13 C23 1.437(8) . ? C23 C33 1.402(8) . ? C23 C231 1.440(8) . ? C231 N232 1.283(7) . ? N232 O233 1.410(5) . ? C33 C43 1.375(8) . ? C43 C53 1.398(9) . ? C43 C431 1.527(9) . ? C431 C432 1.473(11) . ? C431 C434 1.494(12) . ? C431 C433 1.561(11) . ? C53 C63 1.374(9) . ? C63 C631 1.507(9) . ? C631 N632 1.498(8) . ? N632 C633 1.501(8) . ? N632 C634 1.570(9) . ? N632 C63A 1.571(10) . ? C634 C635 1.418(10) . ? C635 C636 1.419(9) . ? C636 C646 1.399(9) . ? C63A C63B 1.417(10) . ? C63B C63C 1.412(10) . ? C63C C64C 1.408(10) . ? O14 C14 1.309(6) . ? C14 C24 1.408(7) . ? C14 C64 1.423(8) . ? C24 C34 1.424(7) . ? C24 C241 1.430(7) . ? C241 N242 1.267(6) . ? N242 O243 1.405(5) . ? C34 C44 1.387(7) . ? C44 C54 1.377(9) . ? C44 C441 1.548(8) . ? C441 C444 1.494(9) . ? C441 C442 1.515(9) . ? C441 C443 1.552(9) . ? C54 C64 1.398(9) . ? C64 C641 1.634(10) . ? C641 N642 1.403(9) . ? N642 C643 1.488(11) . ? N642 C644 1.574(9) . ? N642 C64A 1.586(11) . ? C644 C645 1.417(9) . ? C645 C646 1.432(9) . ? C64A C64B 1.410(10) . ? C64B C64C 1.417(10) . ? N1 O3 1.131(9) . ? N1 O2 1.149(9) . ? N1 O1 1.237(7) . ? N2 O4 1.245(6) . ? N2 O5 1.247(6) . ? N2 O6 1.264(6) . ? N3 O8 1.216(7) . ? N3 O9 1.258(8) . ? N3 O7 1.271(7) . ? N4 O23 1.178(10) . ? N4 O21 1.180(10) . ? N4 O22 1.182(11) . ? N5 O31 1.187(11) . ? N5 O33 1.188(12) . ? N5 O32 1.189(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 O14 Cu1 O11 164.63(16) . . ? O14 Cu1 N242 90.77(16) . . ? O11 Cu1 N242 87.21(15) . . ? O14 Cu1 N212 94.55(17) . . ? O11 Cu1 N212 90.42(16) . . ? N242 Cu1 N212 168.05(17) . . ? O13 Cu2 O12 167.02(18) . . ? O13 Cu2 N232 90.95(18) . . ? O12 Cu2 N232 93.07(18) . . ? O13 Cu2 N222 88.07(19) . . ? O12 Cu2 N222 90.80(19) . . ? N232 Cu2 N222 166.66(18) . . ? C11 O11 Cu1 128.7(3) . . ? O11 C11 C61 118.0(4) . . ? O11 C11 C21 123.3(5) . . ? C61 C11 C21 118.7(5) . . ? C31 C21 C11 118.7(5) . . ? C31 C21 C211 119.0(5) . . ? C11 C21 C211 122.2(5) . . ? N212 C211 C21 124.9(4) . . ? C211 N212 O213 112.6(4) . . ? C211 N212 Cu1 127.4(3) . . ? O213 N212 Cu1 120.0(3) . . ? C41 C31 C21 122.6(5) . . ? C51 C41 C31 116.9(5) . . ? C51 C41 C411 120.5(5) . . ? C31 C41 C411 122.5(5) . . ? C412 C411 C413 108.7(7) . . ? C412 C411 C41 111.8(6) . . ? C413 C411 C41 109.9(6) . . ? C412 C411 C414 110.3(8) . . ? C413 C411 C414 108.6(7) . . ? C41 C411 C414 107.5(6) . . ? C41 C51 C61 124.0(5) . . ? C51 C61 C11 118.8(5) . . ? C51 C61 C611 122.7(5) . . ? C11 C61 C611 118.4(5) . . ? C61 C611 N612 110.7(4) . . ? C613 N612 C611 111.2(4) . . ? C613 N612 C614 112.5(4) . . ? C611 N612 C614 112.2(4) . . ? C615 C614 N612 111.6(4) . . ? C614 C615 C616 111.1(5) . . ? C626 C616 C615 115.0(6) . . ? C12 O12 Cu2 128.5(4) . . ? O12 C12 C22 124.5(6) . . ? O12 C12 C62 118.2(5) . . ? C22 C12 C62 117.3(6) . . ? C32 C22 C12 118.4(6) . . ? C32 C22 C221 119.5(5) . . ? C12 C22 C221 122.1(6) . . ? N222 C221 C22 123.5(5) . . ? C221 N222 O223 112.9(5) . . ? C221 N222 Cu2 129.3(4) . . ? O223 N222 Cu2 117.7(4) . . ? C42 C32 C22 124.1(6) . . ? C32 C42 C52 116.6(6) . . ? C32 C42 C421 124.7(6) . . ? C52 C42 C421 118.6(6) . . ? C423 C421 C422 111.3(7) . . ? C423 C421 C42 110.1(6) . . ? C422 C421 C42 110.0(6) . . ? C423 C421 C424 108.2(8) . . ? C422 C421 C424 107.5(6) . . ? C42 C421 C424 109.6(7) . . ? C62 C52 C42 121.9(7) . . ? C52 C62 C12 121.4(6) . . ? C52 C62 C621 120.3(6) . . ? C12 C62 C621 118.2(6) . . ? N622 C621 C62 108.0(6) . . ? C621 N622 C624 115.1(6) . . ? C621 N622 C623 111.5(6) . . ? C624 N622 C623 113.1(5) . . ? N622 C624 C625 103.0(6) . . ? C626 C625 C624 111.7(6) . . ? C625 C626 C616 111.2(6) . . ? C13 O13 Cu2 129.9(4) . . ? O13 C13 C63 119.7(5) . . ? O13 C13 C23 122.6(5) . . ? C63 C13 C23 117.7(6) . . ? C33 C23 C13 118.3(5) . . ? C33 C23 C231 119.6(5) . . ? C13 C23 C231 122.0(5) . . ? N232 C231 C23 125.6(5) . . ? C231 N232 O233 112.7(4) . . ? C231 N232 Cu2 127.7(4) . . ? O233 N232 Cu2 119.6(3) . . ? C43 C33 C23 123.5(6) . . ? C33 C43 C53 116.6(6) . . ? C33 C43 C431 122.6(6) . . ? C53 C43 C431 120.7(6) . . ? C432 C431 C434 108.6(10) . . ? C432 C431 C43 113.7(6) . . ? C434 C431 C43 108.2(6) . . ? C432 C431 C433 108.9(7) . . ? C434 C431 C433 105.6(8) . . ? C43 C431 C433 111.4(7) . . ? C63 C53 C43 122.3(6) . . ? C53 C63 C13 121.5(6) . . ? C53 C63 C631 121.5(6) . . ? C13 C63 C631 116.9(6) . . ? N632 C631 C63 109.8(5) . . ? C631 N632 C633 112.0(6) . . ? C631 N632 C634 106.3(11) . . ? C633 N632 C634 115(2) . . ? C631 N632 C63A 117.7(10) . . ? C633 N632 C63A 106(2) . . ? C634 N632 C63A 12(2) . . ? C635 C634 N632 111.7(13) . . ? C634 C635 C636 126(2) . . ? C646 C636 C635 107.6(19) . . ? C63B C63A N632 117.5(13) . . ? C63C C63B C63A 116.5(16) . . ? C64C C63C C63B 131(2) . . ? C14 O14 Cu1 127.1(3) . . ? O14 C14 C24 125.7(5) . . ? O14 C14 C64 116.1(5) . . ? C24 C14 C64 118.1(5) . . ? C14 C24 C34 119.8(5) . . ? C14 C24 C241 122.2(5) . . ? C34 C24 C241 118.0(5) . . ? N242 C241 C24 123.6(5) . . ? C241 N242 O243 113.9(4) . . ? C241 N242 Cu1 129.0(3) . . ? O243 N242 Cu1 117.0(3) . . ? C44 C34 C24 122.3(5) . . ? C54 C44 C34 116.5(5) . . ? C54 C44 C441 121.2(5) . . ? C34 C44 C441 122.2(5) . . ? C444 C441 C442 109.2(6) . . ? C444 C441 C44 113.6(5) . . ? C442 C441 C44 108.5(5) . . ? C444 C441 C443 107.2(5) . . ? C442 C441 C443 111.6(6) . . ? C44 C441 C443 106.7(5) . . ? C44 C54 C64 124.3(6) . . ? C54 C64 C14 118.9(6) . . ? C54 C64 C641 127.4(6) . . ? C14 C64 C641 113.7(5) . . ? N642 C641 C64 103.1(6) . . ? C641 N642 C643 120.5(7) . . ? C641 N642 C644 111.7(8) . . ? C643 N642 C644 112.0(8) . . ? C641 N642 C64A 85.9(11) . . ? C643 N642 C64A 125.7(15) . . ? C644 N642 C64A 26.3(8) . . ? C645 C644 N642 115.7(10) . . ? C644 C645 C646 112.7(10) . . ? C636 C646 C645 117.8(11) . . ? C64B C64A N642 89.2(11) . . ? C64A C64B C64C 114(2) . . ? C63C C64C C64B 117(2) . . ? O3 N1 O2 113.6(9) . . ? O3 N1 O1 122.4(10) . . ? O2 N1 O1 123.2(8) . . ? O4 N2 O5 120.4(6) . . ? O4 N2 O6 119.4(6) . . ? O5 N2 O6 120.2(5) . . ? O8 N3 O9 120.0(6) . . ? O8 N3 O7 122.0(6) . . ? O9 N3 O7 118.0(7) . . ? O23 N4 O21 119.5(8) . . ? O23 N4 O22 118.7(8) . . ? O21 N4 O22 118.6(8) . . ? O31 N5 O33 117.0(13) . . ? O31 N5 O32 117.1(13) . . ? O33 N5 O32 116.9(13) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 61.16 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.786 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.077 # Attachment 'SO4-Cl.cif' data_rf19 _database_code_depnum_ccdc_archive 'CCDC 783211' #TrackingRef 'SO4-Cl.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H100 Cu2 N8 O12 S, 2(C H4 O), 2(Cl)' _chemical_formula_sum 'C66 H108 Cl2 Cu2 N8 O14 S' _chemical_formula_weight 1467.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 '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 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 19.805(4) _cell_length_b 20.320(4) _cell_length_c 21.840(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.52(3) _cell_angle_gamma 90.00 _cell_volume 8283(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 22177 _cell_measurement_theta_min 6.8 _cell_measurement_theta_max 72.05 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3120 _exptl_absorpt_coefficient_mu 1.933 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5947 _exptl_absorpt_correction_T_max 0.9095 _exptl_absorpt_process_details Empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'ratating anode' _diffrn_radiation_monochromator 'confocal optics' _diffrn_measurement_device_type 'Rigaku Spider' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_detector_area_resol_mean 10.0000 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 72361 _diffrn_reflns_av_R_equivalents 0.0772 _diffrn_reflns_av_sigmaI/netI 0.0755 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 6.81 _diffrn_reflns_theta_max 65.08 _reflns_number_total 14014 _reflns_number_gt 9908 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crystal Clear (Rigaku, 2005)' _computing_cell_refinement 'FS Process (Rigaku, 1998)' _computing_data_reduction 'FS Process (Rigaku, 1998)' _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. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 126 22 ' ' 2 0.000 0.016 0.462 1315 181 ' ' 3 0.000 0.500 0.500 126 22 ' ' 4 0.375 0.551 0.443 11 2 ' ' 5 0.375 0.949 0.943 11 2 ' ' 6 0.625 0.051 0.056 11 2 ' ' 7 0.625 0.449 0.556 11 2 ' ' _platon_squeeze_details ; 234 electrons per cell were squeezed out corresponding to 13 MeOH per cell ; _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^)+(0.1188P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14014 _refine_ls_number_parameters 852 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0821 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.1946 _refine_ls_wR_factor_gt 0.1820 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.003 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 0.42838(2) 0.29266(2) 0.24846(2) 0.03088(16) Uani 1 1 d . . . O1 O 0.39526(13) 0.07677(12) 0.19862(12) 0.0443(6) Uani 1 1 d . . . Cl1 Cl 0.67116(6) 0.20036(7) 0.03814(5) 0.0725(4) Uani 1 1 d . . . Cl2 Cl 0.17973(7) 0.16847(8) 0.45863(6) 0.0736(4) Uani 0.90 1 d P A 1 Cl3 Cl 0.1998(10) 0.0957(10) 0.4783(9) 0.130(6) Uani 0.10 1 d P B 2 Cu2 Cu 0.41764(2) -0.03136(3) 0.22576(2) 0.03520(17) Uani 1 1 d . . . O2 O 0.41782(14) 0.19246(12) 0.19769(12) 0.0483(7) Uani 1 1 d . . . S3 S 0.43077(4) 0.13313(4) 0.23915(4) 0.0322(2) Uani 1 1 d . . . O3 O 0.50902(13) 0.12232(12) 0.26427(12) 0.0475(7) Uani 1 1 d . . . O4 O 0.40358(14) 0.14259(13) 0.29259(12) 0.0513(7) Uani 1 1 d . . . O11 O 0.34576(12) 0.28819(11) 0.27378(11) 0.0354(6) Uani 1 1 d . . . C11 C 0.27826(18) 0.28390(17) 0.23442(18) 0.0369(8) Uani 1 1 d . . . O12 O 0.51465(11) -0.02819(11) 0.28285(12) 0.0368(6) Uani 1 1 d . . . C12 C 0.57341(18) -0.02514(18) 0.26729(19) 0.0386(9) Uani 1 1 d . . . O13 O 0.32022(12) -0.04024(11) 0.17021(11) 0.0366(6) Uani 1 1 d . . . C13 C 0.26477(18) -0.03203(16) 0.19029(17) 0.0339(8) Uani 1 1 d . . . O14 O 0.51210(12) 0.30299(11) 0.22547(11) 0.0358(6) Uani 1 1 d . . . C14 C 0.57992(17) 0.29325(17) 0.26404(16) 0.0314(8) Uani 1 1 d . . . C21 C 0.25494(18) 0.30409(17) 0.16880(17) 0.0362(8) Uani 1 1 d . . . C22 C 0.57491(19) -0.03655(17) 0.2036(2) 0.0405(9) Uani 1 1 d . . . C23 C 0.26443(18) -0.04884(16) 0.25316(17) 0.0343(8) Uani 1 1 d . . . C24 C 0.60241(17) 0.29823(15) 0.33214(17) 0.0316(8) Uani 1 1 d . . . C31 C 0.18126(18) 0.29967(17) 0.13150(18) 0.0394(9) Uani 1 1 d . . . H31A H 0.1664 0.3129 0.0882 0.047 Uiso 1 1 calc R . . C32 C 0.6419(2) -0.03503(18) 0.1931(2) 0.0456(10) Uani 1 1 d . . . H32A H 0.6429 -0.0443 0.1517 0.055 Uiso 1 1 calc R . . C33 C 0.19995(18) -0.04351(17) 0.26699(18) 0.0380(9) Uani 1 1 d . . . H33A H 0.1996 -0.0571 0.3076 0.046 Uiso 1 1 calc R . . C34 C 0.67647(17) 0.29224(16) 0.36757(18) 0.0337(8) Uani 1 1 d . . . H34A H 0.6920 0.2982 0.4124 0.040 Uiso 1 1 calc R . . C41 C 0.13074(18) 0.27649(19) 0.15709(19) 0.0419(9) Uani 1 1 d . . . C42 C 0.7060(2) -0.02039(18) 0.2419(2) 0.0480(11) Uani 1 1 d . . . C43 C 0.13747(18) -0.01917(18) 0.22329(18) 0.0391(9) Uani 1 1 d . . . C44 C 0.72657(18) 0.27781(17) 0.33784(18) 0.0365(8) Uani 1 1 d . . . C51 C 0.15490(17) 0.25510(18) 0.22227(18) 0.0402(9) Uani 1 1 d . . . H51A H 0.1220 0.2383 0.2403 0.048 Uiso 1 1 calc R . . C52 C 0.7021(2) -0.00745(19) 0.3035(2) 0.0484(10) Uani 1 1 d . . . H52A H 0.7442 0.0025 0.3372 0.058 Uiso 1 1 calc R . . C53 C 0.14095(19) 0.00288(18) 0.16321(18) 0.0395(9) Uani 1 1 d . . . H53A H 0.1005 0.0220 0.1335 0.047 Uiso 1 1 calc R . . C54 C 0.70216(18) 0.26836(17) 0.27111(17) 0.0364(8) Uani 1 1 d . . . H54A H 0.7349 0.2574 0.2506 0.044 Uiso 1 1 calc R . . C61 C 0.22666(18) 0.25860(18) 0.26008(17) 0.0364(8) Uani 1 1 d . . . C62 C 0.63758(19) -0.00884(17) 0.31650(19) 0.0400(9) Uani 1 1 d . . . C63 C 0.20216(18) -0.00297(17) 0.14696(17) 0.0365(8) Uani 1 1 d . . . C64 C 0.62948(17) 0.27480(17) 0.23362(17) 0.0335(8) Uani 1 1 d . . . O100 O 0.2521(2) -0.0724(2) -0.01831(18) 0.0940(11) Uani 1 1 d . . . H100 H 0.2780 -0.0996 -0.0271 0.141 Uiso 1 1 calc R . . C100 C 0.1789(3) -0.0800(3) -0.0628(2) 0.0858(16) Uani 1 1 d . . . H10A H 0.1535 -0.1103 -0.0447 0.129 Uiso 1 1 calc R . . H10B H 0.1799 -0.0967 -0.1037 0.129 Uiso 1 1 calc R . . H10C H 0.1552 -0.0381 -0.0695 0.129 Uiso 1 1 calc R . . O200 O 0.1140(3) 0.3109(2) 0.4473(2) 0.1160(15) Uani 1 1 d D . . H200 H 0.1350 0.2758 0.4584 0.174 Uiso 1 1 calc R . . C200 C 0.1274(3) 0.3345(3) 0.3944(3) 0.0940(18) Uani 1 1 d D . . H20A H 0.1178 0.3809 0.3905 0.141 Uiso 1 1 calc R . . H20B H 0.0972 0.3124 0.3562 0.141 Uiso 1 1 calc R . . H20C H 0.1767 0.3268 0.3991 0.141 Uiso 1 1 calc R . . C211 C 0.30321(18) 0.32586(16) 0.13531(17) 0.0359(8) Uani 1 1 d . . . H21A H 0.2837 0.3419 0.0932 0.043 Uiso 1 1 calc R . . N212 N 0.37104(14) 0.32384(13) 0.16123(13) 0.0335(7) Uani 1 1 d . . . O213 O 0.40878(12) 0.34388(12) 0.12018(11) 0.0407(6) Uani 1 1 d . . . H213 H 0.4520 0.3418 0.1399 0.061 Uiso 1 1 calc R . . C221 C 0.5124(2) -0.04700(17) 0.1478(2) 0.0424(9) Uani 1 1 d . . . H22A H 0.5187 -0.0559 0.1083 0.051 Uiso 1 1 calc R . . N222 N 0.44793(16) -0.04471(14) 0.14921(15) 0.0387(7) Uani 1 1 d . . . O223 O 0.39568(13) -0.05424(12) 0.08892(12) 0.0462(6) Uani 1 1 d . . . H223 H 0.3559 -0.0524 0.0928 0.069 Uiso 1 1 calc R . . C231 C 0.32891(18) -0.06512(17) 0.30658(17) 0.0368(8) Uani 1 1 d . . . H23A H 0.3247 -0.0825 0.3446 0.044 Uiso 1 1 calc R . . N232 N 0.39152(15) -0.05616(14) 0.30277(14) 0.0352(7) Uani 1 1 d . . . O233 O 0.44782(12) -0.07111(12) 0.35938(11) 0.0402(6) Uani 1 1 d . . . H233 H 0.4861 -0.0646 0.3535 0.060 Uiso 1 1 calc R . . C241 C 0.55406(17) 0.30291(16) 0.36859(17) 0.0317(8) Uani 1 1 d . . . H24A H 0.5726 0.3099 0.4132 0.038 Uiso 1 1 calc R . . N242 N 0.48624(14) 0.29769(13) 0.34131(13) 0.0320(7) Uani 1 1 d . . . O243 O 0.44802(12) 0.30190(12) 0.38526(11) 0.0387(6) Uani 1 1 d . . . H243 H 0.4050 0.2983 0.3654 0.058 Uiso 1 1 calc R . . C411 C 0.05006(19) 0.2740(2) 0.1170(2) 0.0532(11) Uani 1 1 d . . . C412 C 0.0354(2) 0.2886(3) 0.0476(2) 0.095(2) Uani 1 1 d . . . H41A H 0.0585 0.2564 0.0293 0.142 Uiso 1 1 calc R . . H41B H 0.0534 0.3316 0.0433 0.142 Uiso 1 1 calc R . . H41C H -0.0154 0.2874 0.0252 0.142 Uiso 1 1 calc R . . C413 C 0.0117(2) 0.3256(3) 0.1471(3) 0.105(2) Uani 1 1 d . . . H41D H 0.0211 0.3156 0.1921 0.157 Uiso 1 1 calc R . . H41E H -0.0390 0.3240 0.1244 0.157 Uiso 1 1 calc R . . H41F H 0.0293 0.3688 0.1431 0.157 Uiso 1 1 calc R . . C414 C 0.0194(3) 0.2070(3) 0.1261(3) 0.099(2) Uani 1 1 d . . . H41G H 0.0410 0.1732 0.1080 0.149 Uiso 1 1 calc R . . H41H H -0.0315 0.2070 0.1044 0.149 Uiso 1 1 calc R . . H41I H 0.0296 0.1989 0.1716 0.149 Uiso 1 1 calc R . . C421 C 0.7774(2) -0.0147(2) 0.2292(2) 0.0524(11) Uani 1 1 d . . . C422 C 0.8345(2) -0.0538(3) 0.2798(3) 0.105(2) Uani 1 1 d . . . H42A H 0.8394 -0.0374 0.3223 0.158 Uiso 1 1 calc R . . H42B H 0.8793 -0.0494 0.2722 0.158 Uiso 1 1 calc R . . H42C H 0.8209 -0.0993 0.2770 0.158 Uiso 1 1 calc R . . C423 C 0.7723(3) -0.0438(3) 0.1625(3) 0.0886(18) Uani 1 1 d . . . H42D H 0.7369 -0.0201 0.1287 0.133 Uiso 1 1 calc R . . H42E H 0.7590 -0.0894 0.1609 0.133 Uiso 1 1 calc R . . H42F H 0.8180 -0.0400 0.1564 0.133 Uiso 1 1 calc R . . C424 C 0.7978(2) 0.05661(19) 0.2296(2) 0.0577(12) Uani 1 1 d . . . H42G H 0.8017 0.0757 0.2709 0.086 Uiso 1 1 calc R . . H42H H 0.7618 0.0795 0.1957 0.086 Uiso 1 1 calc R . . H42I H 0.8430 0.0601 0.2226 0.086 Uiso 1 1 calc R . . C431 C 0.06597(19) -0.0183(2) 0.2376(2) 0.0466(10) Uani 1 1 d . . . C432 C 0.0792(2) -0.0118(3) 0.3102(2) 0.099(2) Uani 1 1 d . . . H43A H 0.0342 -0.0113 0.3178 0.148 Uiso 1 1 calc R . . H43B H 0.1046 0.0284 0.3260 0.148 Uiso 1 1 calc R . . H43C H 0.1072 -0.0485 0.3327 0.148 Uiso 1 1 calc R . . C433 C 0.0294(3) -0.0832(3) 0.2180(3) 0.115(2) Uani 1 1 d . . . H43D H -0.0152 -0.0833 0.2263 0.172 Uiso 1 1 calc R . . H43E H 0.0596 -0.1178 0.2425 0.172 Uiso 1 1 calc R . . H43F H 0.0205 -0.0904 0.1725 0.172 Uiso 1 1 calc R . . C434 C 0.0185(3) 0.0363(4) 0.2020(4) 0.179(5) Uani 1 1 d . . . H43G H -0.0256 0.0353 0.2113 0.269 Uiso 1 1 calc R . . H43H H 0.0085 0.0309 0.1562 0.269 Uiso 1 1 calc R . . H43I H 0.0420 0.0777 0.2156 0.269 Uiso 1 1 calc R . . C441 C 0.80663(18) 0.26889(19) 0.37714(18) 0.0400(9) Uani 1 1 d . . . C442 C 0.8276(2) 0.1966(2) 0.3727(2) 0.0646(13) Uani 1 1 d . . . H44A H 0.8007 0.1689 0.3917 0.097 Uiso 1 1 calc R . . H44B H 0.8779 0.1911 0.3957 0.097 Uiso 1 1 calc R . . H44C H 0.8174 0.1848 0.3280 0.097 Uiso 1 1 calc R . . C443 C 0.8241(2) 0.2887(3) 0.4465(2) 0.0759(16) Uani 1 1 d . . . H44D H 0.7968 0.2623 0.4663 0.114 Uiso 1 1 calc R . . H44E H 0.8123 0.3342 0.4487 0.114 Uiso 1 1 calc R . . H44F H 0.8743 0.2822 0.4691 0.114 Uiso 1 1 calc R . . C444 C 0.8518(2) 0.3120(2) 0.3463(2) 0.0607(12) Uani 1 1 d . . . H44G H 0.8392 0.3574 0.3477 0.091 Uiso 1 1 calc R . . H44H H 0.8424 0.2989 0.3020 0.091 Uiso 1 1 calc R . . H44I H 0.9018 0.3062 0.3702 0.091 Uiso 1 1 calc R . . C611 C 0.25218(17) 0.23551(17) 0.32870(17) 0.0371(8) Uani 1 1 d . . . H61A H 0.2113 0.2290 0.3431 0.045 Uiso 1 1 calc R . . H61B H 0.2824 0.2691 0.3560 0.045 Uiso 1 1 calc R . . N612 N 0.29425(15) 0.17135(14) 0.33675(14) 0.0378(7) Uani 1 1 d . . . H612 H 0.3241 0.1746 0.3130 0.045 Uiso 1 1 calc R . . C613 C 0.2447(2) 0.11509(19) 0.31048(19) 0.0487(10) Uani 1 1 d . . . H61C H 0.2719 0.0752 0.3151 0.073 Uiso 1 1 calc R . . H61D H 0.2186 0.1226 0.2653 0.073 Uiso 1 1 calc R . . H61E H 0.2118 0.1113 0.3340 0.073 Uiso 1 1 calc R . . C614 C 0.33940(18) 0.16130(17) 0.40615(16) 0.0370(8) Uani 1 1 d . . . H61F H 0.3091 0.1637 0.4329 0.044 Uiso 1 1 calc R . . H61G H 0.3741 0.1967 0.4193 0.044 Uiso 1 1 calc R . . C615 C 0.3793(2) 0.09543(18) 0.41867(18) 0.0433(9) Uani 1 1 d . . . H61H H 0.3999 0.0875 0.3848 0.052 Uiso 1 1 calc R . . H61I H 0.3457 0.0602 0.4171 0.052 Uiso 1 1 calc R . . C616 C 0.4388(2) 0.0952(2) 0.48495(18) 0.0521(11) Uani 1 1 d . . . H61J H 0.4597 0.0515 0.4928 0.063 Uiso 1 1 calc R . . H61K H 0.4176 0.1040 0.5182 0.063 Uiso 1 1 calc R . . C621 C 0.63389(19) 0.00753(17) 0.38223(18) 0.0417(9) Uani 1 1 d . . . H62A H 0.6819 0.0089 0.4137 0.050 Uiso 1 1 calc R . . H62B H 0.6073 -0.0265 0.3955 0.050 Uiso 1 1 calc R . . N622 N 0.59798(15) 0.07300(13) 0.38101(15) 0.0381(7) Uani 1 1 d . . . H622 H 0.5606 0.0758 0.3430 0.046 Uiso 1 1 calc R . . C623 C 0.6495(2) 0.12762(18) 0.3820(2) 0.0502(10) Uani 1 1 d . . . H62C H 0.6666 0.1227 0.3460 0.075 Uiso 1 1 calc R . . H62D H 0.6893 0.1259 0.4219 0.075 Uiso 1 1 calc R . . H62E H 0.6257 0.1692 0.3789 0.075 Uiso 1 1 calc R . . C624 C 0.5683(2) 0.07808(17) 0.43605(18) 0.0420(9) Uani 1 1 d . . . H62F H 0.6067 0.0701 0.4767 0.050 Uiso 1 1 calc R . . H62G H 0.5326 0.0439 0.4310 0.050 Uiso 1 1 calc R . . C625 C 0.5345(2) 0.14427(18) 0.43988(18) 0.0425(9) Uani 1 1 d . . . H62H H 0.4986 0.1540 0.3982 0.051 Uiso 1 1 calc R . . H62I H 0.5710 0.1782 0.4488 0.051 Uiso 1 1 calc R . . C626 C 0.4998(2) 0.1459(2) 0.49209(18) 0.0516(10) Uani 1 1 d . . . H62J H 0.4806 0.1896 0.4929 0.062 Uiso 1 1 calc R . . H62K H 0.5368 0.1387 0.5338 0.062 Uiso 1 1 calc R . . C631 C 0.20741(19) 0.02236(18) 0.08473(17) 0.0386(9) Uani 1 1 d . . . H63A H 0.1602 0.0353 0.0563 0.046 Uiso 1 1 calc R . . H63B H 0.2247 -0.0124 0.0633 0.046 Uiso 1 1 calc R . . N632 N 0.25750(15) 0.08061(14) 0.09619(14) 0.0372(7) Uani 1 1 d . . . H632 H 0.2981 0.0701 0.1294 0.045 Uiso 1 1 calc R . . C633 C 0.2258(2) 0.13997(18) 0.11623(19) 0.0479(10) Uani 1 1 d . . . H63C H 0.2591 0.1759 0.1239 0.072 Uiso 1 1 calc R . . H63D H 0.2155 0.1305 0.1553 0.072 Uiso 1 1 calc R . . H63E H 0.1822 0.1517 0.0823 0.072 Uiso 1 1 calc R . . C634 C 0.2780(2) 0.09323(18) 0.03704(17) 0.0419(9) Uani 1 1 d . . . H63F H 0.2348 0.0944 -0.0007 0.050 Uiso 1 1 calc R . . H63G H 0.3071 0.0568 0.0314 0.050 Uiso 1 1 calc R . . C635 C 0.3194(2) 0.15734(18) 0.03969(18) 0.0452(9) Uani 1 1 d . . . H63H H 0.2862 0.1940 0.0301 0.054 Uiso 1 1 calc R . . H63I H 0.3531 0.1634 0.0833 0.054 Uiso 1 1 calc R . . C636 C 0.3602(2) 0.1572(2) -0.00860(18) 0.0490(10) Uani 1 1 d . . . H63J H 0.3268 0.1469 -0.0514 0.059 Uiso 1 1 calc R . . H63K H 0.3783 0.2012 -0.0105 0.059 Uiso 1 1 calc R . . C641 C 0.60020(17) 0.25597(17) 0.16380(16) 0.0345(8) Uani 1 1 d . . . H64A H 0.6391 0.2515 0.1464 0.041 Uiso 1 1 calc R . . H64B H 0.5682 0.2901 0.1395 0.041 Uiso 1 1 calc R . . N642 N 0.56006(14) 0.19172(13) 0.15643(13) 0.0342(7) Uani 1 1 d . . . H642 H 0.5321 0.1937 0.1820 0.041 Uiso 1 1 calc R . . C643 C 0.6123(2) 0.13621(18) 0.18092(18) 0.0456(10) Uani 1 1 d . . . H64C H 0.6410 0.1445 0.2253 0.068 Uiso 1 1 calc R . . H64D H 0.6426 0.1330 0.1548 0.068 Uiso 1 1 calc R . . H64E H 0.5865 0.0957 0.1784 0.068 Uiso 1 1 calc R . . C644 C 0.51133(18) 0.18274(18) 0.08736(16) 0.0380(8) Uani 1 1 d . . . H64F H 0.5387 0.1896 0.0584 0.046 Uiso 1 1 calc R . . H64G H 0.4740 0.2160 0.0775 0.046 Uiso 1 1 calc R . . C645 C 0.4763(2) 0.11444(19) 0.07419(18) 0.0440(9) Uani 1 1 d . . . H64H H 0.5131 0.0814 0.0797 0.053 Uiso 1 1 calc R . . H64I H 0.4526 0.1057 0.1057 0.053 Uiso 1 1 calc R . . C646 C 0.4226(2) 0.1090(2) 0.00703(18) 0.0519(11) Uani 1 1 d . . . H64J H 0.4034 0.0647 0.0011 0.062 Uiso 1 1 calc R . . H64K H 0.4473 0.1156 -0.0241 0.062 Uiso 1 1 calc R . . 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 0.0338(3) 0.0279(3) 0.0358(3) 0.0002(2) 0.0181(2) 0.00077(19) O1 0.0576(15) 0.0287(16) 0.0497(16) -0.0018(12) 0.0221(13) -0.0012(12) Cl1 0.0602(7) 0.1092(11) 0.0533(7) -0.0153(6) 0.0258(5) 0.0147(6) Cl2 0.0624(8) 0.1054(13) 0.0638(8) 0.0048(8) 0.0357(6) 0.0085(7) Cl3 0.129(14) 0.113(16) 0.133(15) -0.009(12) 0.024(12) -0.035(12) Cu2 0.0397(3) 0.0294(3) 0.0440(3) 0.0019(2) 0.0240(2) 0.0020(2) O2 0.0795(19) 0.0267(15) 0.0426(16) 0.0004(11) 0.0257(14) 0.0007(13) S3 0.0429(5) 0.0238(5) 0.0360(5) -0.0004(3) 0.0213(4) 0.0017(3) O3 0.0478(15) 0.0386(17) 0.0607(17) -0.0065(13) 0.0243(13) -0.0015(12) O4 0.0563(16) 0.064(2) 0.0459(16) -0.0029(13) 0.0333(13) 0.0008(13) O11 0.0368(13) 0.0323(15) 0.0403(14) -0.0037(10) 0.0171(11) -0.0011(10) C11 0.0349(19) 0.033(2) 0.045(2) -0.0082(16) 0.0162(16) 0.0002(15) O12 0.0348(13) 0.0320(15) 0.0521(16) 0.0048(11) 0.0258(12) 0.0051(10) C12 0.042(2) 0.023(2) 0.058(2) 0.0071(17) 0.0277(19) 0.0034(15) O13 0.0428(13) 0.0310(15) 0.0435(15) -0.0023(11) 0.0245(12) 0.0010(10) C13 0.043(2) 0.022(2) 0.040(2) -0.0055(15) 0.0182(16) -0.0033(15) O14 0.0353(13) 0.0392(15) 0.0380(14) 0.0015(11) 0.0192(11) 0.0009(10) C14 0.0330(18) 0.025(2) 0.038(2) 0.0043(14) 0.0150(15) -0.0013(13) C21 0.043(2) 0.027(2) 0.043(2) -0.0019(16) 0.0202(17) 0.0040(15) C22 0.048(2) 0.018(2) 0.068(3) 0.0067(17) 0.037(2) 0.0044(15) C23 0.043(2) 0.025(2) 0.042(2) -0.0019(15) 0.0236(16) -0.0055(15) C24 0.0398(19) 0.0156(19) 0.043(2) 0.0005(14) 0.0190(16) 0.0001(13) C31 0.0370(19) 0.038(2) 0.044(2) -0.0031(17) 0.0154(16) 0.0043(16) C32 0.052(2) 0.034(2) 0.062(3) 0.0033(19) 0.033(2) 0.0021(17) C33 0.044(2) 0.031(2) 0.044(2) -0.0053(16) 0.0230(17) -0.0077(16) C34 0.0363(19) 0.024(2) 0.042(2) -0.0023(15) 0.0156(16) -0.0035(14) C41 0.0345(19) 0.038(2) 0.055(2) -0.0136(18) 0.0173(17) -0.0041(16) C42 0.052(2) 0.021(2) 0.087(3) 0.012(2) 0.045(2) 0.0083(17) C43 0.041(2) 0.033(2) 0.048(2) -0.0070(17) 0.0213(17) -0.0044(16) C44 0.0353(19) 0.026(2) 0.052(2) 0.0020(16) 0.0186(17) -0.0021(14) C51 0.0349(19) 0.039(2) 0.052(2) -0.0113(18) 0.0211(17) -0.0077(16) C52 0.041(2) 0.036(3) 0.071(3) 0.009(2) 0.023(2) 0.0010(17) C53 0.041(2) 0.035(2) 0.044(2) -0.0030(17) 0.0169(17) 0.0009(16) C54 0.0404(19) 0.031(2) 0.043(2) 0.0009(16) 0.0214(16) 0.0070(15) C61 0.0416(19) 0.035(2) 0.039(2) -0.0077(16) 0.0211(16) -0.0009(16) C62 0.047(2) 0.023(2) 0.060(3) 0.0102(17) 0.0307(19) 0.0041(16) C63 0.0397(19) 0.029(2) 0.042(2) -0.0047(16) 0.0150(16) -0.0014(15) C64 0.0353(18) 0.032(2) 0.039(2) 0.0033(15) 0.0202(15) 0.0018(15) O100 0.092(3) 0.100(3) 0.087(3) -0.028(2) 0.026(2) 0.008(2) C100 0.089(4) 0.107(5) 0.065(3) 0.002(3) 0.030(3) -0.013(3) O200 0.187(5) 0.078(3) 0.118(4) -0.012(3) 0.099(4) -0.006(3) C200 0.107(4) 0.074(4) 0.096(4) -0.008(3) 0.028(4) -0.004(3) C211 0.041(2) 0.024(2) 0.044(2) 0.0022(16) 0.0155(16) 0.0022(15) N212 0.0360(16) 0.0282(18) 0.0416(17) 0.0005(13) 0.0200(13) 0.0009(12) O213 0.0382(13) 0.0459(16) 0.0443(15) 0.0119(12) 0.0224(11) 0.0054(11) C221 0.057(2) 0.027(2) 0.056(2) 0.0028(17) 0.036(2) 0.0054(17) N222 0.0507(18) 0.0236(18) 0.049(2) 0.0009(13) 0.0263(16) 0.0031(13) O223 0.0551(16) 0.0459(17) 0.0425(15) -0.0015(12) 0.0228(13) 0.0034(12) C231 0.044(2) 0.033(2) 0.040(2) 0.0020(16) 0.0223(17) 0.0005(16) N232 0.0396(16) 0.0286(18) 0.0415(18) 0.0027(13) 0.0192(14) 0.0014(13) O233 0.0350(13) 0.0462(17) 0.0409(15) 0.0082(12) 0.0145(11) 0.0023(11) C241 0.0388(19) 0.022(2) 0.037(2) -0.0062(14) 0.0162(15) -0.0040(14) N242 0.0395(16) 0.0245(17) 0.0393(17) -0.0038(12) 0.0230(13) -0.0036(12) O243 0.0370(13) 0.0481(17) 0.0394(14) -0.0063(11) 0.0238(11) -0.0044(11) C411 0.036(2) 0.059(3) 0.061(3) -0.010(2) 0.0112(19) -0.0044(19) C412 0.042(3) 0.160(6) 0.073(4) 0.024(3) 0.006(2) -0.011(3) C413 0.043(3) 0.120(5) 0.141(5) -0.056(4) 0.017(3) 0.008(3) C414 0.072(3) 0.117(5) 0.090(4) 0.008(3) 0.001(3) -0.051(3) C421 0.049(2) 0.042(3) 0.080(3) 0.011(2) 0.041(2) 0.0054(19) C422 0.057(3) 0.130(5) 0.153(6) 0.084(4) 0.068(4) 0.037(3) C423 0.072(3) 0.091(4) 0.134(5) -0.036(3) 0.074(3) -0.016(3) C424 0.057(2) 0.040(3) 0.093(3) 0.003(2) 0.048(2) -0.0044(19) C431 0.040(2) 0.051(3) 0.056(3) -0.006(2) 0.0256(19) -0.0003(18) C432 0.054(3) 0.181(7) 0.075(4) -0.034(4) 0.039(3) -0.017(3) C433 0.077(4) 0.125(6) 0.178(6) -0.080(5) 0.089(4) -0.054(3) C434 0.134(6) 0.213(8) 0.263(10) 0.178(7) 0.161(7) 0.130(6) C441 0.0358(19) 0.036(2) 0.050(2) 0.0007(17) 0.0177(17) 0.0007(16) C442 0.047(2) 0.039(3) 0.102(4) 0.009(2) 0.018(2) 0.0076(19) C443 0.046(3) 0.121(5) 0.057(3) -0.017(3) 0.013(2) 0.008(3) C444 0.037(2) 0.060(3) 0.083(3) 0.011(2) 0.018(2) -0.005(2) C611 0.0387(19) 0.027(2) 0.053(2) -0.0077(17) 0.0261(17) -0.0038(15) N612 0.0456(17) 0.0323(19) 0.0451(18) -0.0087(14) 0.0278(14) -0.0058(13) C613 0.056(2) 0.034(2) 0.060(3) -0.0157(19) 0.025(2) -0.0134(18) C614 0.048(2) 0.032(2) 0.038(2) -0.0060(16) 0.0239(17) 0.0002(16) C615 0.061(2) 0.032(2) 0.049(2) 0.0009(17) 0.0335(19) -0.0025(18) C616 0.078(3) 0.046(3) 0.045(2) 0.0069(19) 0.038(2) 0.015(2) C621 0.039(2) 0.023(2) 0.064(3) 0.0067(18) 0.0185(18) 0.0006(15) N622 0.0389(16) 0.0237(18) 0.0527(19) 0.0038(13) 0.0169(14) -0.0033(12) C623 0.055(2) 0.028(2) 0.069(3) 0.0048(19) 0.022(2) -0.0114(17) C624 0.050(2) 0.030(2) 0.048(2) 0.0005(17) 0.0183(18) -0.0033(16) C625 0.051(2) 0.027(2) 0.048(2) -0.0035(17) 0.0143(18) -0.0046(17) C626 0.065(3) 0.046(3) 0.035(2) -0.0013(18) 0.0054(19) 0.010(2) C631 0.046(2) 0.035(2) 0.038(2) -0.0057(16) 0.0196(17) -0.0029(16) N632 0.0431(16) 0.0309(19) 0.0395(17) 0.0014(13) 0.0163(13) 0.0050(13) C633 0.064(3) 0.030(2) 0.053(2) -0.0039(18) 0.025(2) 0.0076(18) C634 0.058(2) 0.032(2) 0.039(2) 0.0023(16) 0.0201(18) 0.0004(17) C635 0.057(2) 0.032(2) 0.046(2) 0.0050(17) 0.0159(19) 0.0024(18) C636 0.065(3) 0.045(3) 0.033(2) 0.0065(18) 0.0117(18) -0.013(2) C641 0.0392(18) 0.029(2) 0.043(2) 0.0044(16) 0.0237(16) 0.0020(15) N642 0.0450(16) 0.0284(18) 0.0355(17) 0.0038(13) 0.0219(13) 0.0028(13) C643 0.057(2) 0.034(2) 0.047(2) 0.0050(18) 0.0192(19) 0.0096(18) C644 0.046(2) 0.040(2) 0.033(2) 0.0024(16) 0.0198(16) 0.0016(17) C645 0.055(2) 0.039(2) 0.044(2) 0.0002(18) 0.0262(19) -0.0020(18) C646 0.074(3) 0.052(3) 0.039(2) -0.0053(19) 0.032(2) -0.012(2) _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 O11 1.896(2) . ? Cu1 O14 1.898(2) . ? Cu1 N242 1.970(3) . ? Cu1 N212 1.968(3) . ? Cu1 O2 2.294(2) . ? O1 S3 1.474(3) . ? O1 Cu2 2.280(2) . ? Cu2 O12 1.910(2) . ? Cu2 O13 1.914(2) . ? Cu2 N222 1.975(3) . ? Cu2 N232 1.983(3) . ? O2 S3 1.478(3) . ? S3 O4 1.452(2) . ? S3 O3 1.477(3) . ? O11 C11 1.329(4) . ? C11 C21 1.412(5) . ? C11 C61 1.416(4) . ? O12 C12 1.318(4) . ? C12 C62 1.403(5) . ? C12 C22 1.421(5) . ? O13 C13 1.322(4) . ? C13 C63 1.413(5) . ? C13 C23 1.417(5) . ? O14 C14 1.340(4) . ? C14 C24 1.407(5) . ? C14 C64 1.407(4) . ? C21 C31 1.417(5) . ? C21 C211 1.453(4) . ? C22 C32 1.419(5) . ? C22 C221 1.433(5) . ? C23 C33 1.411(4) . ? C23 C231 1.451(5) . ? C24 C34 1.416(5) . ? C24 C241 1.438(4) . ? C31 C41 1.382(5) . ? C31 H31A 0.9300 . ? C32 C42 1.391(6) . ? C32 H32A 0.9300 . ? C33 C43 1.377(5) . ? C33 H33A 0.9300 . ? C34 C44 1.387(4) . ? C34 H34A 0.9300 . ? C41 C51 1.410(5) . ? C41 C411 1.545(5) . ? C42 C52 1.397(5) . ? C42 C421 1.533(5) . ? C43 C53 1.410(5) . ? C43 C431 1.549(4) . ? C44 C54 1.387(5) . ? C44 C441 1.541(5) . ? C51 C61 1.387(5) . ? C51 H51A 0.9300 . ? C52 C62 1.400(5) . ? C52 H52A 0.9300 . ? C53 C63 1.377(4) . ? C53 H53A 0.9300 . ? C54 C64 1.404(5) . ? C54 H54A 0.9300 . ? C61 C611 1.488(5) . ? C62 C621 1.499(5) . ? C63 C631 1.489(5) . ? C64 C641 1.489(5) . ? O100 C100 1.459(6) . ? O100 H100 0.8200 . ? C100 H10A 0.9600 . ? C100 H10B 0.9600 . ? C100 H10C 0.9600 . ? O200 C200 1.357(6) . ? O200 H200 0.8200 . ? C200 H20A 0.9600 . ? C200 H20B 0.9600 . ? C200 H20C 0.9600 . ? C211 N212 1.272(4) . ? C211 H21A 0.9300 . ? N212 O213 1.406(3) . ? O213 H213 0.8200 . ? C221 N222 1.287(4) . ? C221 H22A 0.9300 . ? N222 O223 1.390(4) . ? O223 H223 0.8200 . ? C231 N232 1.283(4) . ? C231 H23A 0.9300 . ? N232 O233 1.394(3) . ? O233 H233 0.8200 . ? C241 N242 1.279(4) . ? C241 H24A 0.9300 . ? N242 O243 1.409(3) . ? O243 H243 0.8200 . ? C411 C412 1.474(6) . ? C411 C414 1.529(6) . ? C411 C413 1.564(6) . ? C412 H41A 0.9600 . ? C412 H41B 0.9600 . ? C412 H41C 0.9600 . ? C413 H41D 0.9600 . ? C413 H41E 0.9600 . ? C413 H41F 0.9600 . ? C414 H41G 0.9600 . ? C414 H41H 0.9600 . ? C414 H41I 0.9600 . ? C421 C424 1.504(5) . ? C421 C422 1.515(6) . ? C421 C423 1.544(6) . ? C422 H42A 0.9600 . ? C422 H42B 0.9600 . ? C422 H42C 0.9600 . ? C423 H42D 0.9600 . ? C423 H42E 0.9600 . ? C423 H42F 0.9600 . ? C424 H42G 0.9600 . ? C424 H42H 0.9600 . ? C424 H42I 0.9600 . ? C431 C434 1.493(6) . ? C431 C433 1.498(6) . ? C431 C432 1.524(6) . ? C432 H43A 0.9600 . ? C432 H43B 0.9600 . ? C432 H43C 0.9600 . ? C433 H43D 0.9600 . ? C433 H43E 0.9600 . ? C433 H43F 0.9600 . ? C434 H43G 0.9600 . ? C434 H43H 0.9600 . ? C434 H43I 0.9600 . ? C441 C443 1.491(5) . ? C441 C442 1.538(5) . ? C441 C444 1.557(5) . ? C442 H44A 0.9600 . ? C442 H44B 0.9600 . ? C442 H44C 0.9600 . ? C443 H44D 0.9600 . ? C443 H44E 0.9600 . ? C443 H44F 0.9600 . ? C444 H44G 0.9600 . ? C444 H44H 0.9600 . ? C444 H44I 0.9600 . ? C611 N612 1.525(4) . ? C611 H61A 0.9700 . ? C611 H61B 0.9700 . ? N612 C613 1.491(4) . ? N612 C614 1.494(4) . ? N612 H612 0.9100 . ? C613 H61C 0.9600 . ? C613 H61D 0.9600 . ? C613 H61E 0.9600 . ? C614 C615 1.532(5) . ? C614 H61F 0.9700 . ? C614 H61G 0.9700 . ? C615 C616 1.531(5) . ? C615 H61H 0.9700 . ? C615 H61I 0.9700 . ? C616 C626 1.555(6) . ? C616 H61J 0.9700 . ? C616 H61K 0.9700 . ? C621 N622 1.505(4) . ? C621 H62A 0.9700 . ? C621 H62B 0.9700 . ? N622 C623 1.503(4) . ? N622 C624 1.507(4) . ? N622 H622 0.9100 . ? C623 H62C 0.9600 . ? C623 H62D 0.9600 . ? C623 H62E 0.9600 . ? C624 C625 1.517(5) . ? C624 H62F 0.9700 . ? C624 H62G 0.9700 . ? C625 C626 1.515(5) . ? C625 H62H 0.9700 . ? C625 H62I 0.9700 . ? C626 H62J 0.9700 . ? C626 H62K 0.9700 . ? C631 N632 1.510(4) . ? C631 H63A 0.9700 . ? C631 H63B 0.9700 . ? N632 C633 1.492(4) . ? N632 C634 1.500(4) . ? N632 H632 0.9100 . ? C633 H63C 0.9600 . ? C633 H63D 0.9600 . ? C633 H63E 0.9600 . ? C634 C635 1.530(5) . ? C634 H63F 0.9700 . ? C634 H63G 0.9700 . ? C635 C636 1.527(5) . ? C635 H63H 0.9700 . ? C635 H63I 0.9700 . ? C636 C646 1.523(5) . ? C636 H63J 0.9700 . ? C636 H63K 0.9700 . ? C641 N642 1.509(4) . ? C641 H64A 0.9700 . ? C641 H64B 0.9700 . ? N642 C643 1.502(4) . ? N642 C644 1.506(4) . ? N642 H642 0.9100 . ? C643 H64C 0.9600 . ? C643 H64D 0.9600 . ? C643 H64E 0.9600 . ? C644 C645 1.536(5) . ? C644 H64F 0.9700 . ? C644 H64G 0.9700 . ? C645 C646 1.501(5) . ? C645 H64H 0.9700 . ? C645 H64I 0.9700 . ? C646 H64J 0.9700 . ? C646 H64K 0.9700 . ? 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 O11 Cu1 O14 176.12(10) . . ? O11 Cu1 N242 87.94(11) . . ? O14 Cu1 N242 90.43(10) . . ? O11 Cu1 N212 91.30(10) . . ? O14 Cu1 N212 88.90(11) . . ? N242 Cu1 N212 158.18(11) . . ? O11 Cu1 O2 98.64(10) . . ? O14 Cu1 O2 85.24(10) . . ? N242 Cu1 O2 118.11(10) . . ? N212 Cu1 O2 83.57(10) . . ? S3 O1 Cu2 125.46(15) . . ? O12 Cu2 O13 176.35(10) . . ? O12 Cu2 N222 91.91(11) . . ? O13 Cu2 N222 88.71(11) . . ? O12 Cu2 N232 86.88(11) . . ? O13 Cu2 N232 91.16(11) . . ? N222 Cu2 N232 157.28(12) . . ? O12 Cu2 O1 101.70(10) . . ? O13 Cu2 O1 81.89(9) . . ? N222 Cu2 O1 90.00(10) . . ? N232 Cu2 O1 112.48(10) . . ? S3 O2 Cu1 117.30(14) . . ? O4 S3 O1 110.78(15) . . ? O4 S3 O3 110.23(16) . . ? O1 S3 O3 109.76(14) . . ? O4 S3 O2 110.45(15) . . ? O1 S3 O2 108.39(15) . . ? O3 S3 O2 107.13(15) . . ? C11 O11 Cu1 126.4(2) . . ? O11 C11 C21 123.7(3) . . ? O11 C11 C61 118.1(3) . . ? C21 C11 C61 118.2(3) . . ? C12 O12 Cu2 128.0(2) . . ? O12 C12 C62 117.7(3) . . ? O12 C12 C22 123.6(3) . . ? C62 C12 C22 118.6(3) . . ? C13 O13 Cu2 123.4(2) . . ? O13 C13 C63 118.1(3) . . ? O13 C13 C23 124.4(3) . . ? C63 C13 C23 117.5(3) . . ? C14 O14 Cu1 126.7(2) . . ? O14 C14 C24 123.4(3) . . ? O14 C14 C64 117.0(3) . . ? C24 C14 C64 119.6(3) . . ? C11 C21 C31 119.3(3) . . ? C11 C21 C211 123.5(3) . . ? C31 C21 C211 117.0(3) . . ? C12 C22 C32 118.7(4) . . ? C12 C22 C221 124.1(3) . . ? C32 C22 C221 117.1(4) . . ? C33 C23 C13 119.1(3) . . ? C33 C23 C231 117.5(3) . . ? C13 C23 C231 123.1(3) . . ? C14 C24 C34 118.4(3) . . ? C14 C24 C241 123.8(3) . . ? C34 C24 C241 117.6(3) . . ? C41 C31 C21 122.3(3) . . ? C41 C31 H31A 118.8 . . ? C21 C31 H31A 118.8 . . ? C42 C32 C22 123.0(4) . . ? C42 C32 H32A 118.5 . . ? C22 C32 H32A 118.5 . . ? C43 C33 C23 123.2(3) . . ? C43 C33 H33A 118.4 . . ? C23 C33 H33A 118.4 . . ? C44 C34 C24 122.3(3) . . ? C44 C34 H34A 118.8 . . ? C24 C34 H34A 118.8 . . ? C31 C41 C51 117.8(3) . . ? C31 C41 C411 122.2(4) . . ? C51 C41 C411 120.0(3) . . ? C32 C42 C52 116.6(3) . . ? C32 C42 C421 122.6(4) . . ? C52 C42 C421 120.7(4) . . ? C33 C43 C53 116.5(3) . . ? C33 C43 C431 122.3(3) . . ? C53 C43 C431 121.1(3) . . ? C54 C44 C34 117.9(3) . . ? C54 C44 C441 120.1(3) . . ? C34 C44 C441 121.9(3) . . ? C61 C51 C41 121.3(3) . . ? C61 C51 H51A 119.3 . . ? C41 C51 H51A 119.3 . . ? C62 C52 C42 122.7(4) . . ? C62 C52 H52A 118.7 . . ? C42 C52 H52A 118.7 . . ? C63 C53 C43 122.2(3) . . ? C63 C53 H53A 118.9 . . ? C43 C53 H53A 118.9 . . ? C44 C54 C64 122.0(3) . . ? C44 C54 H54A 119.0 . . ? C64 C54 H54A 119.0 . . ? C51 C61 C11 121.0(3) . . ? C51 C61 C611 121.3(3) . . ? C11 C61 C611 117.8(3) . . ? C52 C62 C12 120.3(4) . . ? C52 C62 C621 122.0(4) . . ? C12 C62 C621 117.7(3) . . ? C53 C63 C13 120.9(3) . . ? C53 C63 C631 122.8(3) . . ? C13 C63 C631 116.2(3) . . ? C54 C64 C14 119.4(3) . . ? C54 C64 C641 123.1(3) . . ? C14 C64 C641 117.2(3) . . ? C100 O100 H100 109.5 . . ? O100 C100 H10A 109.5 . . ? O100 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? O100 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? C200 O200 H200 109.5 . . ? O200 C200 H20A 109.5 . . ? O200 C200 H20B 109.5 . . ? H20A C200 H20B 109.5 . . ? O200 C200 H20C 109.5 . . ? H20A C200 H20C 109.5 . . ? H20B C200 H20C 109.5 . . ? N212 C211 C21 122.7(3) . . ? N212 C211 H21A 118.6 . . ? C21 C211 H21A 118.6 . . ? C211 N212 O213 114.5(3) . . ? C211 N212 Cu1 128.5(2) . . ? O213 N212 Cu1 116.92(18) . . ? N212 O213 H213 109.5 . . ? N222 C221 C22 123.9(4) . . ? N222 C221 H22A 118.1 . . ? C22 C221 H22A 118.1 . . ? C221 N222 O223 113.8(3) . . ? C221 N222 Cu2 127.5(3) . . ? O223 N222 Cu2 118.7(2) . . ? N222 O223 H223 109.5 . . ? N232 C231 C23 121.7(3) . . ? N232 C231 H23A 119.1 . . ? C23 C231 H23A 119.2 . . ? C231 N232 O233 114.6(3) . . ? C231 N232 Cu2 128.5(3) . . ? O233 N232 Cu2 116.72(18) . . ? N232 O233 H233 109.5 . . ? N242 C241 C24 121.8(3) . . ? N242 C241 H24A 119.1 . . ? C24 C241 H24A 119.1 . . ? C241 N242 O243 113.4(3) . . ? C241 N242 Cu1 130.0(2) . . ? O243 N242 Cu1 116.36(19) . . ? N242 O243 H243 109.5 . . ? C412 C411 C414 111.3(4) . . ? C412 C411 C41 112.8(3) . . ? C414 C411 C41 109.6(4) . . ? C412 C411 C413 109.8(4) . . ? C414 C411 C413 105.8(4) . . ? C41 C411 C413 107.2(3) . . ? C411 C412 H41A 109.5 . . ? C411 C412 H41B 109.5 . . ? H41A C412 H41B 109.5 . . ? C411 C412 H41C 109.5 . . ? H41A C412 H41C 109.5 . . ? H41B C412 H41C 109.5 . . ? C411 C413 H41D 109.5 . . ? C411 C413 H41E 109.5 . . ? H41D C413 H41E 109.5 . . ? C411 C413 H41F 109.5 . . ? H41D C413 H41F 109.5 . . ? H41E C413 H41F 109.5 . . ? C411 C414 H41G 109.5 . . ? C411 C414 H41H 109.5 . . ? H41G C414 H41H 109.5 . . ? C411 C414 H41I 109.5 . . ? H41G C414 H41I 109.5 . . ? H41H C414 H41I 109.5 . . ? C424 C421 C422 111.5(4) . . ? C424 C421 C42 109.5(3) . . ? C422 C421 C42 109.7(3) . . ? C424 C421 C423 107.9(4) . . ? C422 C421 C423 106.6(4) . . ? C42 C421 C423 111.7(4) . . ? C421 C422 H42A 109.5 . . ? C421 C422 H42B 109.5 . . ? H42A C422 H42B 109.5 . . ? C421 C422 H42C 109.5 . . ? H42A C422 H42C 109.5 . . ? H42B C422 H42C 109.5 . . ? C421 C423 H42D 109.5 . . ? C421 C423 H42E 109.5 . . ? H42D C423 H42E 109.5 . . ? C421 C423 H42F 109.5 . . ? H42D C423 H42F 109.5 . . ? H42E C423 H42F 109.5 . . ? C421 C424 H42G 109.5 . . ? C421 C424 H42H 109.5 . . ? H42G C424 H42H 109.5 . . ? C421 C424 H42I 109.5 . . ? H42G C424 H42I 109.5 . . ? H42H C424 H42I 109.5 . . ? C434 C431 C433 110.2(5) . . ? C434 C431 C432 109.7(5) . . ? C433 C431 C432 105.8(4) . . ? C434 C431 C43 111.3(3) . . ? C433 C431 C43 108.5(3) . . ? C432 C431 C43 111.1(3) . . ? C431 C432 H43A 109.5 . . ? C431 C432 H43B 109.5 . . ? H43A C432 H43B 109.5 . . ? C431 C432 H43C 109.5 . . ? H43A C432 H43C 109.5 . . ? H43B C432 H43C 109.5 . . ? C431 C433 H43D 109.5 . . ? C431 C433 H43E 109.5 . . ? H43D C433 H43E 109.5 . . ? C431 C433 H43F 109.5 . . ? H43D C433 H43F 109.5 . . ? H43E C433 H43F 109.5 . . ? C431 C434 H43G 109.5 . . ? C431 C434 H43H 109.5 . . ? H43G C434 H43H 109.5 . . ? C431 C434 H43I 109.5 . . ? H43G C434 H43I 109.5 . . ? H43H C434 H43I 109.5 . . ? C443 C441 C44 112.3(3) . . ? C443 C441 C442 110.2(4) . . ? C44 C441 C442 109.1(3) . . ? C443 C441 C444 108.4(3) . . ? C44 C441 C444 109.0(3) . . ? C442 C441 C444 107.7(3) . . ? C441 C442 H44A 109.5 . . ? C441 C442 H44B 109.5 . . ? H44A C442 H44B 109.5 . . ? C441 C442 H44C 109.5 . . ? H44A C442 H44C 109.5 . . ? H44B C442 H44C 109.5 . . ? C441 C443 H44D 109.5 . . ? C441 C443 H44E 109.5 . . ? H44D C443 H44E 109.5 . . ? C441 C443 H44F 109.5 . . ? H44D C443 H44F 109.5 . . ? H44E C443 H44F 109.5 . . ? C441 C444 H44G 109.5 . . ? C441 C444 H44H 109.5 . . ? H44G C444 H44H 109.5 . . ? C441 C444 H44I 109.5 . . ? H44G C444 H44I 109.5 . . ? H44H C444 H44I 109.5 . . ? C61 C611 N612 112.0(3) . . ? C61 C611 H61A 109.2 . . ? N612 C611 H61A 109.2 . . ? C61 C611 H61B 109.2 . . ? N612 C611 H61B 109.2 . . ? H61A C611 H61B 107.9 . . ? C613 N612 C614 112.3(3) . . ? C613 N612 C611 110.3(3) . . ? C614 N612 C611 110.6(2) . . ? C613 N612 H612 107.8 . . ? C614 N612 H612 107.8 . . ? C611 N612 H612 107.8 . . ? N612 C613 H61C 109.5 . . ? N612 C613 H61D 109.5 . . ? H61C C613 H61D 109.5 . . ? N612 C613 H61E 109.5 . . ? H61C C613 H61E 109.5 . . ? H61D C613 H61E 109.5 . . ? N612 C614 C615 113.5(3) . . ? N612 C614 H61F 108.9 . . ? C615 C614 H61F 108.9 . . ? N612 C614 H61G 108.9 . . ? C615 C614 H61G 108.9 . . ? H61F C614 H61G 107.7 . . ? C614 C615 C616 111.1(3) . . ? C614 C615 H61H 109.4 . . ? C616 C615 H61H 109.4 . . ? C614 C615 H61I 109.4 . . ? C616 C615 H61I 109.4 . . ? H61H C615 H61I 108.0 . . ? C615 C616 C626 114.8(3) . . ? C615 C616 H61J 108.6 . . ? C626 C616 H61J 108.6 . . ? C615 C616 H61K 108.6 . . ? C626 C616 H61K 108.6 . . ? H61J C616 H61K 107.5 . . ? C62 C621 N622 110.7(3) . . ? C62 C621 H62A 109.5 . . ? N622 C621 H62A 109.5 . . ? C62 C621 H62B 109.5 . . ? N622 C621 H62B 109.5 . . ? H62A C621 H62B 108.1 . . ? C623 N622 C621 109.7(3) . . ? C623 N622 C624 112.4(3) . . ? C621 N622 C624 110.8(3) . . ? C623 N622 H622 107.9 . . ? C621 N622 H622 107.9 . . ? C624 N622 H622 107.9 . . ? N622 C623 H62C 109.5 . . ? N622 C623 H62D 109.5 . . ? H62C C623 H62D 109.5 . . ? N622 C623 H62E 109.5 . . ? H62C C623 H62E 109.5 . . ? H62D C623 H62E 109.5 . . ? N622 C624 C625 113.7(3) . . ? N622 C624 H62F 108.8 . . ? C625 C624 H62F 108.8 . . ? N622 C624 H62G 108.8 . . ? C625 C624 H62G 108.8 . . ? H62F C624 H62G 107.7 . . ? C624 C625 C626 112.3(3) . . ? C624 C625 H62H 109.1 . . ? C626 C625 H62H 109.1 . . ? C624 C625 H62I 109.1 . . ? C626 C625 H62I 109.1 . . ? H62H C625 H62I 107.9 . . ? C625 C626 C616 116.3(3) . . ? C625 C626 H62J 108.2 . . ? C616 C626 H62J 108.2 . . ? C625 C626 H62K 108.2 . . ? C616 C626 H62K 108.2 . . ? H62J C626 H62K 107.4 . . ? C63 C631 N632 111.2(3) . . ? C63 C631 H63A 109.4 . . ? N632 C631 H63A 109.4 . . ? C63 C631 H63B 109.4 . . ? N632 C631 H63B 109.4 . . ? H63A C631 H63B 108.0 . . ? C633 N632 C634 112.1(3) . . ? C633 N632 C631 111.4(3) . . ? C634 N632 C631 110.1(3) . . ? C633 N632 H632 107.7 . . ? C634 N632 H632 107.7 . . ? C631 N632 H632 107.7 . . ? N632 C633 H63C 109.5 . . ? N632 C633 H63D 109.5 . . ? H63C C633 H63D 109.5 . . ? N632 C633 H63E 109.5 . . ? H63C C633 H63E 109.5 . . ? H63D C633 H63E 109.5 . . ? N632 C634 C635 114.1(3) . . ? N632 C634 H63F 108.7 . . ? C635 C634 H63F 108.7 . . ? N632 C634 H63G 108.7 . . ? C635 C634 H63G 108.7 . . ? H63F C634 H63G 107.6 . . ? C636 C635 C634 111.9(3) . . ? C636 C635 H63H 109.2 . . ? C634 C635 H63H 109.2 . . ? C636 C635 H63I 109.2 . . ? C634 C635 H63I 109.2 . . ? H63H C635 H63I 107.9 . . ? C646 C636 C635 115.0(3) . . ? C646 C636 H63J 108.5 . . ? C635 C636 H63J 108.5 . . ? C646 C636 H63K 108.5 . . ? C635 C636 H63K 108.5 . . ? H63J C636 H63K 107.5 . . ? C64 C641 N642 110.0(3) . . ? C64 C641 H64A 109.7 . . ? N642 C641 H64A 109.7 . . ? C64 C641 H64B 109.7 . . ? N642 C641 H64B 109.7 . . ? H64A C641 H64B 108.2 . . ? C643 N642 C644 113.6(3) . . ? C643 N642 C641 109.6(3) . . ? C644 N642 C641 110.5(2) . . ? C643 N642 H642 107.6 . . ? C644 N642 H642 107.6 . . ? C641 N642 H642 107.6 . . ? N642 C643 H64C 109.5 . . ? N642 C643 H64D 109.5 . . ? H64C C643 H64D 109.5 . . ? N642 C643 H64E 109.5 . . ? H64C C643 H64E 109.5 . . ? H64D C643 H64E 109.5 . . ? N642 C644 C645 113.3(3) . . ? N642 C644 H64F 108.9 . . ? C645 C644 H64F 108.9 . . ? N642 C644 H64G 108.9 . . ? C645 C644 H64G 108.9 . . ? H64F C644 H64G 107.7 . . ? C646 C645 C644 112.2(3) . . ? C646 C645 H64H 109.2 . . ? C644 C645 H64H 109.2 . . ? C646 C645 H64I 109.2 . . ? C644 C645 H64I 109.2 . . ? H64H C645 H64I 107.9 . . ? C645 C646 C636 115.4(3) . . ? C645 C646 H64J 108.4 . . ? C636 C646 H64J 108.4 . . ? C645 C646 H64K 108.4 . . ? C636 C646 H64K 108.4 . . ? H64J C646 H64K 107.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 65.08 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.925 _refine_diff_density_min -0.446 _refine_diff_density_rms 0.082 # Attachment 'SO4-HPO4.cif' data_mw110sq _database_code_depnum_ccdc_archive 'CCDC 783212' #TrackingRef 'SO4-HPO4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H100 Cu2 N8 O8 (O4 S), 2(O4 P)' _chemical_formula_sum 'C64 H100 Cu2 N8 O20 P2 S' _chemical_formula_weight 1522.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' 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 20.2187(4) _cell_length_b 21.9011(4) _cell_length_c 38.781(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17172.6(13) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 35768 _cell_measurement_theta_min 6.5 _cell_measurement_theta_max 72.2 _exptl_crystal_description chip _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.178 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6432 _exptl_absorpt_coefficient_mu 1.721 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.596 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details Empirical _exptl_special_details ; Absorption correction in FSP: Higashi, T. (1995). ABSCOR: Empirical Absorption Correction based on Fourier Series Approximation. Rigaku Corporation, 3-9-12 Matsubara, Akishima, Tokyo 196-8666, JAPAN. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'confocal optics' _diffrn_measurement_device_type 'Rigaku Spider' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_detector_area_resol_mean 10.0000 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 126497 _diffrn_reflns_av_R_equivalents 0.1134 _diffrn_reflns_av_sigmaI/netI 0.0908 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 6.55 _diffrn_reflns_theta_max 61.16 _reflns_number_total 13160 _reflns_number_gt 7141 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crystal Clear (Rigaku, 2009)' _computing_cell_refinement 'FS Process (Rigaku, 1998)' _computing_data_reduction 'FS Process (Rigaku, 1998)' _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. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.010 0.023 0.250 951 147 ' ' 2 0.012 0.523 0.250 948 146 ' ' 3 -0.010 0.477 0.750 950 149 ' ' 4 0.006 0.977 0.750 949 148 ' ' _platon_squeeze_details ; in total 590 e- per unit cell 1(CH3CH2OH), 2(CH3OH) and 1(H2O) (= 72 e-) per formula unit ; _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^)+(0.1298P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00005(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 13160 _refine_ls_number_parameters 930 _refine_ls_number_restraints 246 _refine_ls_R_factor_all 0.1223 _refine_ls_R_factor_gt 0.0758 _refine_ls_wR_factor_ref 0.2330 _refine_ls_wR_factor_gt 0.1998 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 1.130 _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 0.70422(4) 0.27008(4) 0.02889(2) 0.0443(3) Uani 1 1 d . . . Cu2 Cu 1.02567(4) 0.23500(4) 0.04043(2) 0.0511(3) Uani 1 1 d . . . S1 S 0.86295(8) 0.25041(7) 0.03001(4) 0.0455(4) Uani 1 1 d . . . O1 O 0.8000(2) 0.2203(2) 0.03966(12) 0.0703(14) Uani 1 1 d . . . O2 O 0.91635(19) 0.21828(18) 0.04862(10) 0.0518(11) Uani 1 1 d . . . O3 O 0.8701(2) 0.2432(2) -0.00739(10) 0.0656(13) Uani 1 1 d . . . O4 O 0.8603(3) 0.3151(2) 0.03963(11) 0.0796(15) Uani 1 1 d . . . O11 O 0.70717(19) 0.31938(18) 0.06917(9) 0.0478(11) Uani 1 1 d . . . C11 C 0.7123(3) 0.2994(3) 0.10167(14) 0.0452(16) Uani 1 1 d . . . O12 O 1.02497(19) 0.26539(18) -0.00612(10) 0.0494(11) Uani 1 1 d . . . C12 C 1.0218(3) 0.2324(3) -0.03480(16) 0.0462(16) Uani 1 1 d . . . O13 O 1.03214(19) 0.2050(2) 0.08638(10) 0.0539(11) Uani 1 1 d . . . C13 C 1.0214(3) 0.2402(3) 0.11423(16) 0.0537(18) Uani 1 1 d . . . O14 O 0.69687(18) 0.22381(18) -0.01244(10) 0.0474(11) Uani 1 1 d . . . C14 C 0.7029(3) 0.2430(3) -0.04451(15) 0.0414(15) Uani 1 1 d . . . C21 C 0.6920(3) 0.2399(3) 0.11198(15) 0.0482(16) Uani 1 1 d . . . C22 C 1.0320(3) 0.1696(3) -0.03658(14) 0.0468(16) Uani 1 1 d . . . C23 C 1.0385(3) 0.3017(3) 0.11705(15) 0.0493(16) Uani 1 1 d . . . C24 C 0.6997(3) 0.3048(3) -0.05464(15) 0.0460(16) Uani 1 1 d . . . C31 C 0.6959(3) 0.2245(3) 0.14713(14) 0.0503(17) Uani 1 1 d . . . H31A H 0.6800 0.1867 0.1541 0.060 Uiso 1 1 calc R . . C33 C 1.0314(3) 0.3312(3) 0.14918(16) 0.0561(18) Uani 1 1 d . . . H33A H 1.0450 0.3716 0.1509 0.067 Uiso 1 1 calc R . . C34 C 0.7063(3) 0.3203(3) -0.09004(14) 0.0493(16) Uani 1 1 d . . . H34A H 0.7030 0.3611 -0.0965 0.059 Uiso 1 1 calc R . . C41 C 0.7220(3) 0.2629(3) 0.17162(15) 0.0497(17) Uani 1 1 d . . . C42 C 1.0173(3) 0.1683(3) -0.09944(15) 0.0488(16) Uani 1 1 d . . . C43 C 1.0058(3) 0.3038(3) 0.17792(16) 0.0574(18) Uani 1 1 d . . . C44 C 0.7174(3) 0.2774(3) -0.11499(14) 0.0466(16) Uani 1 1 d . . . C51 C 0.7450(3) 0.3177(3) 0.16070(14) 0.0515(17) Uani 1 1 d . . . H51A H 0.7640 0.3438 0.1768 0.062 Uiso 1 1 calc R . . C52 C 1.0054(3) 0.2327(3) -0.09704(15) 0.0517(17) Uani 1 1 d . . . H52A H 0.9969 0.2545 -0.1171 0.062 Uiso 1 1 calc R . . C53 C 0.9828(3) 0.2436(3) 0.17419(16) 0.0588(19) Uani 1 1 d . . . H53A H 0.9619 0.2244 0.1926 0.071 Uiso 1 1 calc R . . C54 C 0.7232(3) 0.2167(3) -0.10463(15) 0.0521(17) Uani 1 1 d . . . H54A H 0.7307 0.1868 -0.1212 0.063 Uiso 1 1 calc R . . C61 C 0.7415(3) 0.3372(3) 0.12632(14) 0.0441(15) Uani 1 1 d . . . C62 C 1.0061(3) 0.2635(3) -0.06604(15) 0.0482(16) Uani 1 1 d . . . C63 C 0.9910(3) 0.2120(3) 0.14286(17) 0.0538(17) Uani 1 1 d . . . C64 C 0.7180(3) 0.1994(3) -0.06995(14) 0.0424(15) Uani 1 1 d . . . C211 C 0.6678(3) 0.1935(3) 0.08797(14) 0.0460(15) Uani 1 1 d . . . H21A H 0.6505 0.1574 0.0968 0.055 Uiso 1 1 calc R . . N212 N 0.6697(2) 0.2008(2) 0.05537(11) 0.0444(12) Uani 1 1 d . . . O213 O 0.6489(2) 0.14862(19) 0.03667(9) 0.0548(11) Uani 1 1 d . . . H213 H 0.6513 0.1556 0.0159 0.066 Uiso 1 1 calc R . . C221 C 1.0424(3) 0.1312(3) -0.00646(16) 0.0514(17) Uani 1 1 d . . . H22A H 1.0512 0.0899 -0.0098 0.062 Uiso 1 1 calc R . . N222 N 1.0400(2) 0.1518(2) 0.02471(14) 0.0538(14) Uani 1 1 d . . . O223 O 1.0504(2) 0.1049(2) 0.04921(11) 0.0628(13) Uani 1 1 d . . . H223 H 1.0491 0.1194 0.0687 0.075 Uiso 1 1 calc R . . C231 C 1.0566(3) 0.3382(3) 0.08745(15) 0.0554(18) Uani 1 1 d . . . H23A H 1.0743 0.3770 0.0908 0.066 Uiso 1 1 calc R . . N232 N 1.0487(2) 0.3181(2) 0.05620(13) 0.0524(14) Uani 1 1 d . . . O233 O 1.0652(2) 0.3608(2) 0.03072(10) 0.0592(12) Uani 1 1 d . . . H233 H 1.0594 0.3456 0.0116 0.071 Uiso 1 1 calc R . . C241 C 0.6968(3) 0.3539(3) -0.03013(14) 0.0445(15) Uani 1 1 d . . . H24A H 0.6909 0.3934 -0.0383 0.053 Uiso 1 1 calc R . . N242 N 0.7020(2) 0.3459(2) 0.00242(12) 0.0426(12) Uani 1 1 d . . . O243 O 0.70036(19) 0.40035(18) 0.02138(9) 0.0526(11) Uani 1 1 d . . . H243 H 0.7037 0.3926 0.0420 0.063 Uiso 1 1 calc R . . C411 C 0.7230(4) 0.2436(3) 0.20980(15) 0.061(2) Uani 1 1 d . . . C412 C 0.7680(6) 0.1897(5) 0.21418(19) 0.151(5) Uani 1 1 d . . . H41A H 0.8123 0.2012 0.2082 0.226 Uiso 1 1 calc R . . H41B H 0.7535 0.1571 0.1994 0.226 Uiso 1 1 calc R . . H41C H 0.7668 0.1763 0.2377 0.226 Uiso 1 1 calc R . . C413 C 0.6520(4) 0.2252(4) 0.22048(19) 0.111(3) Uani 1 1 d . . . H41D H 0.6376 0.1913 0.2067 0.167 Uiso 1 1 calc R . . H41E H 0.6227 0.2592 0.2170 0.167 Uiso 1 1 calc R . . H41F H 0.6516 0.2138 0.2444 0.167 Uiso 1 1 calc R . . C414 C 0.7430(5) 0.2964(4) 0.23324(17) 0.113(3) Uani 1 1 d . . . H41G H 0.7869 0.3096 0.2275 0.169 Uiso 1 1 calc R . . H41H H 0.7419 0.2832 0.2568 0.169 Uiso 1 1 calc R . . H41I H 0.7127 0.3297 0.2302 0.169 Uiso 1 1 calc R . . C421 C 1.0138(3) 0.1354(3) -0.13440(16) 0.0597(18) Uani 1 1 d . . . C422 C 1.0349(4) 0.0698(3) -0.13194(17) 0.089(3) Uani 1 1 d . . . H42A H 1.0056 0.0483 -0.1167 0.133 Uiso 1 1 calc R . . H42B H 1.0792 0.0678 -0.1231 0.133 Uiso 1 1 calc R . . H42C H 1.0333 0.0515 -0.1544 0.133 Uiso 1 1 calc R . . C423 C 0.9436(3) 0.1388(4) -0.14922(18) 0.084(3) Uani 1 1 d . . . H42D H 0.9136 0.1179 -0.1341 0.126 Uiso 1 1 calc R . . H42E H 0.9427 0.1199 -0.1715 0.126 Uiso 1 1 calc R . . H42F H 0.9304 0.1807 -0.1513 0.126 Uiso 1 1 calc R . . C424 C 1.0611(3) 0.1692(4) -0.16017(16) 0.074(2) Uani 1 1 d . . . H42G H 1.0594 0.1495 -0.1822 0.111 Uiso 1 1 calc R . . H42H H 1.1056 0.1679 -0.1515 0.111 Uiso 1 1 calc R . . H42I H 1.0474 0.2110 -0.1625 0.111 Uiso 1 1 calc R . . C431 C 0.9985(4) 0.3380(3) 0.21255(17) 0.068(2) Uani 1 1 d . . . C432 C 0.9797(4) 0.2951(4) 0.24180(17) 0.093(3) Uani 1 1 d . . . H43A H 0.9382 0.2759 0.2366 0.140 Uiso 1 1 calc R . . H43B H 0.9758 0.3179 0.2628 0.140 Uiso 1 1 calc R . . H43C H 1.0132 0.2645 0.2444 0.140 Uiso 1 1 calc R . . C433 C 1.0635(4) 0.3684(3) 0.22144(18) 0.080(2) Uani 1 1 d . . . H43D H 1.0590 0.3905 0.2427 0.120 Uiso 1 1 calc R . . H43E H 1.0756 0.3963 0.2034 0.120 Uiso 1 1 calc R . . H43F H 1.0973 0.3379 0.2239 0.120 Uiso 1 1 calc R . . C434 C 0.9423(4) 0.3830(4) 0.2092(2) 0.115(3) Uani 1 1 d . . . H43G H 0.9023 0.3615 0.2038 0.172 Uiso 1 1 calc R . . H43H H 0.9522 0.4116 0.1912 0.172 Uiso 1 1 calc R . . H43I H 0.9369 0.4044 0.2306 0.172 Uiso 1 1 calc R . . C441 C 0.7263(3) 0.2936(3) -0.15349(15) 0.0540(17) Uani 1 1 d . . . C442 C 0.6722(3) 0.2615(4) -0.17395(16) 0.079(2) Uani 1 1 d . . . H44A H 0.6768 0.2713 -0.1980 0.118 Uiso 1 1 calc R . . H44B H 0.6297 0.2748 -0.1659 0.118 Uiso 1 1 calc R . . H44C H 0.6761 0.2181 -0.1709 0.118 Uiso 1 1 calc R . . C443 C 0.7949(3) 0.2724(4) -0.16564(17) 0.073(2) Uani 1 1 d . . . H44D H 0.8285 0.2937 -0.1529 0.110 Uiso 1 1 calc R . . H44E H 0.7999 0.2809 -0.1898 0.110 Uiso 1 1 calc R . . H44F H 0.7993 0.2293 -0.1618 0.110 Uiso 1 1 calc R . . C444 C 0.7223(4) 0.3600(4) -0.15997(17) 0.083(2) Uani 1 1 d . . . H44G H 0.7564 0.3805 -0.1473 0.125 Uiso 1 1 calc R . . H44H H 0.6798 0.3749 -0.1527 0.125 Uiso 1 1 calc R . . H44I H 0.7279 0.3678 -0.1842 0.125 Uiso 1 1 calc R . . C611 C 0.7672(3) 0.3980(3) 0.11469(14) 0.0459(15) Uani 1 1 d . . . H61A H 0.7771 0.4229 0.1347 0.055 Uiso 1 1 calc R . . H61B H 0.7334 0.4187 0.1014 0.055 Uiso 1 1 calc R . . N612 N 0.8293(2) 0.3911(2) 0.09280(11) 0.0479(13) Uani 1 1 d . . . H612 H 0.8214 0.3610 0.0772 0.057 Uiso 1 1 calc R . . C613 C 0.8872(3) 0.3717(3) 0.11397(17) 0.064(2) Uani 1 1 d . . . H61C H 0.9249 0.3661 0.0993 0.096 Uiso 1 1 calc R . . H61D H 0.8771 0.3339 0.1254 0.096 Uiso 1 1 calc R . . H61E H 0.8968 0.4025 0.1309 0.096 Uiso 1 1 calc R . . C614 C 0.8426(3) 0.4488(3) 0.07270(15) 0.0523(17) Uani 1 1 d . . . H61F H 0.8424 0.4831 0.0886 0.063 Uiso 1 1 calc R . . H61G H 0.8067 0.4549 0.0564 0.063 Uiso 1 1 calc R . . C615 C 0.9071(3) 0.4491(3) 0.05315(16) 0.0534(17) Uani 1 1 d . . . H61H H 0.9432 0.4551 0.0693 0.064 Uiso 1 1 calc R . . H61I H 0.9132 0.4097 0.0422 0.064 Uiso 1 1 calc R . . C616 C 0.9096(3) 0.4975(3) 0.02651(18) 0.063(2) Uani 1 1 d . . . H61J H 0.9542 0.4993 0.0174 0.076 Uiso 1 1 calc R . . H61K H 0.9006 0.5363 0.0376 0.076 Uiso 1 1 calc R . . C621 C 0.9926(3) 0.3305(3) -0.06417(15) 0.0479(16) Uani 1 1 d . . . H62A H 0.9923 0.3475 -0.0873 0.057 Uiso 1 1 calc R . . H62B H 1.0276 0.3504 -0.0513 0.057 Uiso 1 1 calc R . . N622 N 0.9264(2) 0.3432(2) -0.04687(12) 0.0470(13) Uani 1 1 d . . . H622 H 0.9231 0.3183 -0.0282 0.056 Uiso 1 1 calc R . . C623 C 0.8711(3) 0.3273(3) -0.07124(16) 0.0598(19) Uani 1 1 d . . . H62C H 0.8294 0.3342 -0.0601 0.090 Uiso 1 1 calc R . . H62D H 0.8745 0.2851 -0.0777 0.090 Uiso 1 1 calc R . . H62E H 0.8742 0.3523 -0.0915 0.090 Uiso 1 1 calc R . . C624 C 0.9244(3) 0.4075(3) -0.03438(15) 0.0497(16) Uani 1 1 d . . . H62F H 0.9349 0.4346 -0.0534 0.060 Uiso 1 1 calc R . . H62G H 0.9581 0.4129 -0.0168 0.060 Uiso 1 1 calc R . . C625 C 0.8585(3) 0.4256(3) -0.01960(16) 0.0561(17) Uani 1 1 d . . . H62H H 0.8454 0.3963 -0.0021 0.067 Uiso 1 1 calc R . . H62I H 0.8253 0.4252 -0.0377 0.067 Uiso 1 1 calc R . . C626 C 0.8624(4) 0.4902(3) -0.00343(19) 0.069(2) Uani 1 1 d . . . H62J H 0.8753 0.5188 -0.0213 0.083 Uiso 1 1 calc R . . H62K H 0.8185 0.5017 0.0043 0.083 Uiso 1 1 calc R . . C631 C 0.9635(3) 0.1490(3) 0.13787(16) 0.0585(18) Uani 1 1 d . . . H63A H 0.9477 0.1334 0.1598 0.070 Uiso 1 1 calc R . . H63B H 0.9981 0.1221 0.1296 0.070 Uiso 1 1 calc R . . N632 N 0.9073(2) 0.1500(2) 0.11222(12) 0.0477(13) Uani 1 1 d . . . H632 H 0.9207 0.1727 0.0938 0.057 Uiso 1 1 calc R . . C633 C 0.8474(3) 0.1795(3) 0.12648(16) 0.0576(18) Uani 1 1 d . . . H63C H 0.8136 0.1808 0.1091 0.086 Uiso 1 1 calc R . . H63D H 0.8579 0.2202 0.1337 0.086 Uiso 1 1 calc R . . H63E H 0.8318 0.1564 0.1459 0.086 Uiso 1 1 calc R . . C634 C 0.8921(3) 0.0868(3) 0.09922(17) 0.0609(18) Uani 1 1 d . . . H63F H 0.9301 0.0717 0.0866 0.073 Uiso 1 1 calc R . . H63G H 0.8855 0.0601 0.1189 0.073 Uiso 1 1 calc R . . C635 C 0.8330(3) 0.0829(3) 0.07657(15) 0.0528(17) Uani 1 1 d . . . H63H H 0.8314 0.1186 0.0618 0.063 Uiso 1 1 calc R . . H63I H 0.7934 0.0828 0.0907 0.063 Uiso 1 1 calc R . . C636 C 0.8342(4) 0.0261(3) 0.05455(18) 0.0643(19) Uani 1 1 d . . . H63J H 0.7902 0.0198 0.0453 0.077 Uiso 1 1 calc R . . H63K H 0.8442 -0.0084 0.0693 0.077 Uiso 1 1 calc R . . C641 C 0.7340(3) 0.1367(3) -0.05781(14) 0.0451(15) Uani 1 1 d . . . H64A H 0.7356 0.1088 -0.0773 0.054 Uiso 1 1 calc R . . H64B H 0.7001 0.1225 -0.0420 0.054 Uiso 1 1 calc R . . N642 N 0.8009(2) 0.1381(2) -0.03966(12) 0.0466(13) Uani 1 1 d . . . H642 H 0.8018 0.1718 -0.0260 0.056 Uiso 1 1 calc R . . C643 C 0.8549(3) 0.1446(3) -0.06577(16) 0.0618(19) Uani 1 1 d . . . H64C H 0.8968 0.1469 -0.0542 0.093 Uiso 1 1 calc R . . H64D H 0.8479 0.1812 -0.0789 0.093 Uiso 1 1 calc R . . H64E H 0.8545 0.1099 -0.0809 0.093 Uiso 1 1 calc R . . C644 C 0.8097(3) 0.0830(3) -0.01668(15) 0.0550(17) Uani 1 1 d . . . H64F H 0.8031 0.0462 -0.0302 0.066 Uiso 1 1 calc R . . H64G H 0.7763 0.0838 0.0013 0.066 Uiso 1 1 calc R . . C645 C 0.8774(3) 0.0812(3) -0.00027(17) 0.0565(18) Uani 1 1 d . . . H64H H 0.8850 0.1187 0.0124 0.068 Uiso 1 1 calc R . . H64I H 0.9109 0.0781 -0.0181 0.068 Uiso 1 1 calc R . . C646 C 0.8832(3) 0.0259(3) 0.02459(16) 0.0584(18) Uani 1 1 d . . . H64J H 0.8769 -0.0113 0.0114 0.070 Uiso 1 1 calc R . . H64K H 0.9277 0.0250 0.0339 0.070 Uiso 1 1 calc R . . P2 P 0.89634(16) 0.49146(16) -0.12661(7) 0.1092(10) Uani 1 1 d D . . O21 O 0.9533(3) 0.5086(3) -0.10640(16) 0.122(2) Uani 1 1 d D A . O22 O 0.9089(8) 0.4230(5) -0.1345(3) 0.103(7) Uani 0.414(13) 1 d PDU A 1 O23 O 0.8408(5) 0.4842(7) -0.0989(3) 0.100(6) Uani 0.414(13) 1 d PDU A 1 O24 O 0.8712(6) 0.5190(6) -0.1549(3) 0.093(5) Uani 0.414(13) 1 d PDU A 1 O25 O 0.9270(8) 0.5104(5) -0.1627(2) 0.143(6) Uani 0.586(13) 1 d PDU A 2 O26 O 0.8734(11) 0.4343(7) -0.1288(5) 0.35(2) Uani 0.586(13) 1 d PDU A 2 O27 O 0.8492(6) 0.5436(7) -0.1220(4) 0.201(9) Uani 0.586(13) 1 d PDU A 2 C32 C 1.0296(3) 0.1390(3) -0.06901(15) 0.0496(16) Uani 1 1 d . . . H32A H 1.0367 0.0971 -0.0695 0.059 Uiso 1 1 calc R . . P3 P 1.08603(19) 0.43965(13) -0.15029(7) 0.1103(9) Uani 1 1 d D . . O31 O 1.1570(3) 0.4351(3) -0.14428(18) 0.164(3) Uani 1 1 d D B . O32 O 1.0596(6) 0.4931(5) -0.1673(3) 0.133(5) Uani 0.50 1 d PDU B 1 O33 O 1.0579(5) 0.4441(5) -0.1117(2) 0.096(4) Uani 0.50 1 d PDU B 1 O34 O 1.0597(10) 0.3797(6) -0.1635(4) 0.284(16) Uani 0.50 1 d PDU B 1 O35 O 1.0556(5) 0.4969(4) -0.1369(3) 0.094(4) Uani 0.50 1 d PDU B 2 O36 O 1.0727(7) 0.4466(6) -0.1913(2) 0.149(6) Uani 0.50 1 d PDU B 2 O37 O 1.0422(8) 0.3855(6) -0.1418(4) 0.175(8) Uani 0.50 1 d PDU B 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 0.0413(6) 0.0600(6) 0.0318(5) -0.0013(4) 0.0006(4) 0.0016(4) Cu2 0.0413(6) 0.0707(7) 0.0414(6) -0.0034(5) -0.0010(4) 0.0009(5) S1 0.0370(10) 0.0543(10) 0.0454(9) -0.0023(7) -0.0015(7) 0.0058(8) O1 0.030(3) 0.093(4) 0.089(4) 0.021(3) 0.006(2) -0.002(2) O2 0.044(3) 0.065(3) 0.047(2) 0.012(2) -0.006(2) 0.004(2) O3 0.064(3) 0.090(3) 0.043(3) -0.010(2) -0.006(2) 0.021(3) O4 0.098(4) 0.073(3) 0.068(3) -0.008(3) -0.017(3) 0.012(3) O11 0.048(3) 0.065(3) 0.030(2) -0.0011(19) -0.0038(18) 0.006(2) C11 0.044(4) 0.064(4) 0.027(3) -0.003(3) -0.001(3) 0.004(3) O12 0.041(3) 0.067(3) 0.040(2) -0.004(2) -0.0042(19) -0.004(2) C12 0.030(4) 0.063(5) 0.045(4) -0.002(3) 0.001(3) 0.001(3) O13 0.048(3) 0.075(3) 0.039(2) -0.007(2) -0.005(2) 0.010(2) C13 0.042(4) 0.083(5) 0.036(4) 0.006(4) -0.005(3) 0.011(4) O14 0.037(3) 0.064(3) 0.042(2) -0.005(2) 0.0012(19) -0.005(2) C14 0.018(3) 0.069(4) 0.037(3) 0.004(3) -0.002(3) -0.004(3) C21 0.042(4) 0.067(4) 0.036(3) 0.005(3) 0.006(3) 0.009(3) C22 0.031(4) 0.071(5) 0.037(3) 0.001(3) 0.001(3) 0.005(3) C23 0.037(4) 0.069(5) 0.042(4) 0.004(3) -0.003(3) -0.002(3) C24 0.031(4) 0.068(5) 0.040(3) 0.002(3) -0.001(3) 0.001(3) C31 0.050(4) 0.070(4) 0.031(3) -0.001(3) -0.002(3) 0.011(3) C33 0.040(4) 0.084(5) 0.045(4) -0.005(4) -0.005(3) 0.001(4) C34 0.028(4) 0.080(5) 0.039(3) -0.001(3) -0.004(3) 0.006(3) C41 0.051(4) 0.066(5) 0.032(3) 0.000(3) 0.003(3) 0.008(4) C42 0.048(4) 0.061(4) 0.038(3) -0.005(3) 0.004(3) 0.000(3) C43 0.049(4) 0.077(5) 0.046(4) -0.011(4) -0.003(3) 0.009(4) C44 0.044(4) 0.068(5) 0.028(3) -0.005(3) -0.002(3) 0.005(3) C51 0.045(4) 0.077(5) 0.032(3) -0.006(3) -0.002(3) 0.001(4) C52 0.051(4) 0.072(5) 0.032(3) 0.003(3) 0.004(3) -0.011(4) C53 0.045(4) 0.092(6) 0.040(4) -0.001(4) -0.005(3) 0.009(4) C54 0.050(4) 0.079(5) 0.027(3) -0.009(3) -0.001(3) 0.003(4) C61 0.038(4) 0.061(4) 0.034(3) -0.008(3) 0.001(3) 0.010(3) C62 0.032(4) 0.069(5) 0.044(4) 0.001(3) 0.002(3) -0.001(3) C63 0.037(4) 0.070(5) 0.054(4) -0.003(4) -0.012(3) 0.012(4) C64 0.027(3) 0.064(4) 0.036(3) -0.009(3) 0.002(3) -0.006(3) C211 0.034(4) 0.063(4) 0.041(4) 0.001(3) 0.000(3) 0.002(3) N212 0.044(3) 0.059(3) 0.030(3) -0.013(2) -0.004(2) -0.002(3) O213 0.051(3) 0.076(3) 0.038(2) 0.000(2) 0.001(2) 0.001(2) C221 0.040(4) 0.061(4) 0.053(4) -0.001(3) 0.005(3) 0.006(3) N222 0.043(3) 0.066(4) 0.052(3) 0.003(3) -0.001(3) 0.001(3) O223 0.055(3) 0.079(3) 0.055(3) 0.008(3) 0.000(2) 0.013(2) C231 0.040(4) 0.082(5) 0.045(4) -0.008(4) -0.006(3) -0.004(3) N232 0.042(3) 0.068(4) 0.047(3) 0.004(3) 0.006(3) 0.002(3) O233 0.053(3) 0.080(3) 0.044(2) -0.006(2) 0.004(2) -0.008(2) C241 0.039(4) 0.055(4) 0.040(3) 0.001(3) 0.002(3) 0.006(3) N242 0.043(3) 0.051(3) 0.034(3) -0.003(2) -0.003(2) 0.007(2) O243 0.065(3) 0.058(3) 0.035(2) -0.004(2) -0.004(2) 0.007(2) C411 0.068(5) 0.089(5) 0.025(3) 0.003(3) 0.004(3) 0.006(4) C412 0.210(12) 0.198(11) 0.044(5) 0.029(6) 0.012(6) 0.117(10) C413 0.107(8) 0.180(9) 0.045(5) 0.004(5) 0.008(5) -0.044(7) C414 0.170(10) 0.137(8) 0.031(4) -0.001(5) -0.006(5) -0.056(7) C421 0.061(5) 0.076(5) 0.042(4) -0.005(3) 0.001(3) 0.000(4) C422 0.146(8) 0.071(5) 0.049(4) -0.015(4) 0.002(5) 0.018(5) C423 0.044(5) 0.143(7) 0.065(5) -0.034(5) 0.005(4) -0.023(5) C424 0.059(5) 0.113(6) 0.050(4) -0.016(4) 0.014(4) -0.017(4) C431 0.071(6) 0.087(5) 0.047(4) -0.009(4) -0.006(4) 0.019(5) C432 0.104(7) 0.130(7) 0.045(4) -0.009(5) 0.008(4) -0.024(6) C433 0.083(6) 0.098(6) 0.060(5) -0.021(4) -0.010(4) -0.003(5) C434 0.115(8) 0.155(9) 0.076(6) -0.051(6) -0.026(5) 0.061(7) C441 0.052(4) 0.075(5) 0.036(3) 0.003(3) 0.009(3) -0.003(4) C442 0.057(5) 0.139(7) 0.040(4) -0.006(4) -0.007(4) -0.018(5) C443 0.045(4) 0.124(7) 0.051(4) 0.002(4) 0.015(3) -0.006(4) C444 0.098(6) 0.112(7) 0.040(4) 0.002(4) 0.002(4) -0.006(5) C611 0.039(4) 0.059(4) 0.040(3) -0.005(3) 0.000(3) 0.008(3) N612 0.046(3) 0.059(3) 0.038(3) 0.000(2) -0.003(2) 0.006(3) C613 0.041(4) 0.086(5) 0.065(4) 0.009(4) -0.017(3) 0.006(4) C614 0.045(4) 0.066(4) 0.046(4) -0.005(3) 0.002(3) -0.009(3) C615 0.039(4) 0.057(4) 0.064(4) -0.010(3) 0.004(3) 0.000(3) C616 0.059(5) 0.058(5) 0.072(5) -0.012(4) 0.020(4) -0.006(4) C621 0.043(4) 0.059(4) 0.042(3) -0.002(3) 0.000(3) -0.006(3) N622 0.032(3) 0.062(3) 0.047(3) 0.008(3) 0.003(2) 0.004(3) C623 0.035(4) 0.085(5) 0.060(4) -0.004(4) -0.019(3) -0.010(4) C624 0.045(4) 0.053(4) 0.051(4) -0.001(3) 0.003(3) 0.000(3) C625 0.038(4) 0.076(5) 0.054(4) 0.005(3) -0.004(3) 0.007(4) C626 0.075(5) 0.053(4) 0.079(5) 0.010(4) 0.030(4) 0.018(4) C631 0.057(5) 0.073(5) 0.046(4) 0.007(3) -0.012(3) 0.008(4) N632 0.045(3) 0.056(3) 0.042(3) 0.006(2) 0.004(2) 0.001(3) C633 0.044(4) 0.074(5) 0.054(4) 0.003(3) 0.005(3) 0.012(4) C634 0.056(5) 0.068(5) 0.059(4) 0.004(4) 0.009(4) 0.007(4) C635 0.036(4) 0.068(4) 0.054(4) 0.004(3) 0.001(3) -0.008(3) C636 0.069(5) 0.055(4) 0.069(5) 0.005(4) -0.003(4) -0.005(4) C641 0.032(4) 0.064(4) 0.040(3) -0.006(3) -0.001(3) -0.003(3) N642 0.040(3) 0.052(3) 0.048(3) -0.005(2) 0.008(2) 0.003(3) C643 0.045(4) 0.080(5) 0.060(4) 0.008(4) 0.023(3) -0.002(4) C644 0.052(4) 0.062(4) 0.051(4) 0.002(3) 0.011(3) 0.007(3) C645 0.032(4) 0.072(5) 0.066(4) -0.008(4) 0.001(3) 0.006(3) C646 0.058(5) 0.054(4) 0.063(4) 0.001(3) 0.001(4) -0.001(4) P2 0.113(2) 0.152(3) 0.0629(16) -0.0054(17) -0.0267(16) 0.015(2) O21 0.095(5) 0.149(6) 0.123(5) -0.028(4) -0.026(4) -0.014(4) O22 0.186(17) 0.078(11) 0.044(9) -0.019(8) 0.024(10) -0.038(10) O23 0.078(10) 0.153(15) 0.069(10) 0.024(9) -0.010(8) 0.017(10) O24 0.071(11) 0.141(13) 0.066(10) 0.014(9) 0.026(8) 0.024(9) O25 0.255(19) 0.106(9) 0.067(7) 0.028(6) 0.027(9) 0.033(10) O26 0.43(3) 0.37(3) 0.26(3) 0.18(2) -0.23(2) -0.33(3) O27 0.102(11) 0.30(2) 0.197(18) 0.022(16) -0.007(11) 0.037(12) C32 0.043(4) 0.058(4) 0.048(4) -0.007(3) 0.004(3) 0.008(3) P3 0.157(3) 0.090(2) 0.0834(18) 0.0130(16) 0.0182(18) 0.023(2) O31 0.139(7) 0.189(8) 0.163(7) 0.030(6) 0.059(6) 0.063(6) O32 0.216(15) 0.083(9) 0.100(10) 0.040(8) 0.047(11) 0.064(9) O33 0.114(9) 0.117(9) 0.058(6) -0.002(7) -0.016(6) -0.031(7) O34 0.62(4) 0.113(13) 0.116(14) -0.041(11) -0.21(2) 0.126(19) O35 0.136(10) 0.063(7) 0.082(8) -0.024(6) 0.008(8) -0.004(7) O36 0.271(18) 0.105(10) 0.071(8) 0.012(8) 0.040(10) -0.013(11) O37 0.35(2) 0.076(10) 0.098(12) 0.031(9) -0.060(14) -0.018(12) _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 O11 1.900(4) . ? Cu1 O14 1.902(4) . ? Cu1 N242 1.953(5) . ? Cu1 N212 1.961(5) . ? Cu1 O1 2.261(4) . ? Cu2 O13 1.903(4) . ? Cu2 O12 1.924(4) . ? Cu2 N222 1.943(5) . ? Cu2 N232 1.976(5) . ? Cu2 O2 2.263(4) . ? S1 O3 1.466(4) . ? S1 O4 1.467(5) . ? S1 O2 1.477(4) . ? S1 O1 1.481(4) . ? O11 C11 1.338(6) . ? C11 C61 1.395(7) . ? C11 C21 1.424(8) . ? O12 C12 1.328(7) . ? C12 C22 1.392(8) . ? C12 C62 1.425(8) . ? O13 C13 1.343(7) . ? C13 C23 1.396(9) . ? C13 C63 1.410(8) . ? O14 C14 1.318(6) . ? C14 C64 1.405(8) . ? C14 C24 1.413(8) . ? C21 C31 1.406(8) . ? C21 C211 1.462(8) . ? C22 C32 1.426(8) . ? C22 C221 1.456(8) . ? C23 C33 1.410(8) . ? C23 C231 1.446(8) . ? C24 C34 1.420(8) . ? C24 C241 1.435(8) . ? C31 C41 1.374(8) . ? C33 C43 1.368(8) . ? C34 C44 1.367(8) . ? C41 C51 1.354(8) . ? C41 C411 1.540(8) . ? C42 C32 1.366(8) . ? C42 C52 1.433(8) . ? C42 C421 1.537(8) . ? C43 C53 1.407(9) . ? C43 C431 1.544(8) . ? C44 C54 1.394(8) . ? C44 C441 1.545(8) . ? C51 C61 1.401(7) . ? C52 C62 1.378(8) . ? C53 C63 1.408(8) . ? C54 C64 1.401(7) . ? C61 C611 1.499(8) . ? C62 C621 1.496(8) . ? C63 C631 1.501(8) . ? C64 C641 1.489(8) . ? C211 N212 1.275(6) . ? N212 O213 1.417(5) . ? C221 N222 1.292(7) . ? N222 O223 1.415(6) . ? C231 N232 1.299(7) . ? N232 O233 1.400(6) . ? C241 N242 1.278(6) . ? N242 O243 1.401(5) . ? C411 C412 1.498(10) . ? C411 C414 1.526(9) . ? C411 C413 1.548(10) . ? C421 C422 1.502(9) . ? C421 C423 1.533(8) . ? C421 C424 1.569(8) . ? C431 C434 1.508(9) . ? C431 C433 1.515(9) . ? C431 C432 1.520(9) . ? C441 C444 1.479(9) . ? C441 C442 1.522(8) . ? C441 C443 1.538(8) . ? C611 N612 1.523(7) . ? N612 C613 1.491(7) . ? N612 C614 1.508(7) . ? C614 C615 1.509(8) . ? C615 C616 1.481(8) . ? C616 C626 1.510(9) . ? C621 N622 1.522(7) . ? N622 C624 1.490(7) . ? N622 C623 1.505(7) . ? C624 C625 1.503(8) . ? C625 C626 1.551(8) . ? C631 N632 1.510(7) . ? N632 C633 1.479(7) . ? N632 C634 1.507(7) . ? C634 C635 1.485(8) . ? C635 C636 1.510(8) . ? C636 C646 1.527(9) . ? C641 N642 1.527(7) . ? N642 C643 1.495(7) . ? N642 C644 1.510(7) . ? C644 C645 1.511(8) . ? C645 C646 1.553(8) . ? P2 O26 1.337(10) . ? P2 O24 1.353(9) . ? P2 O21 1.443(5) . ? P2 O27 1.499(11) . ? P2 O22 1.550(10) . ? P2 O23 1.564(9) . ? P2 O25 1.586(9) . ? P3 O32 1.446(8) . ? P3 O31 1.456(6) . ? P3 O35 1.491(8) . ? P3 O34 1.506(11) . ? P3 O37 1.517(10) . ? P3 O33 1.603(8) . ? P3 O36 1.620(9) . ? 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 O11 Cu1 O14 176.44(17) . . ? O11 Cu1 N242 87.12(18) . . ? O14 Cu1 N242 90.48(18) . . ? O11 Cu1 N212 91.18(17) . . ? O14 Cu1 N212 90.06(18) . . ? N242 Cu1 N212 157.7(2) . . ? O11 Cu1 O1 95.46(17) . . ? O14 Cu1 O1 88.04(17) . . ? N242 Cu1 O1 121.74(18) . . ? N212 Cu1 O1 80.51(18) . . ? O13 Cu2 O12 176.47(17) . . ? O13 Cu2 N222 87.7(2) . . ? O12 Cu2 N222 91.8(2) . . ? O13 Cu2 N232 90.7(2) . . ? O12 Cu2 N232 88.48(19) . . ? N222 Cu2 N232 157.7(2) . . ? O13 Cu2 O2 83.11(15) . . ? O12 Cu2 O2 100.40(15) . . ? N222 Cu2 O2 92.19(18) . . ? N232 Cu2 O2 109.65(18) . . ? O3 S1 O4 111.0(3) . . ? O3 S1 O2 111.1(2) . . ? O4 S1 O2 111.3(3) . . ? O3 S1 O1 106.7(3) . . ? O4 S1 O1 109.6(3) . . ? O2 S1 O1 107.0(3) . . ? S1 O1 Cu1 118.4(3) . . ? S1 O2 Cu2 124.6(2) . . ? C11 O11 Cu1 126.2(4) . . ? O11 C11 C61 119.0(6) . . ? O11 C11 C21 122.8(5) . . ? C61 C11 C21 118.2(5) . . ? C12 O12 Cu2 126.7(4) . . ? O12 C12 C22 124.9(6) . . ? O12 C12 C62 117.6(6) . . ? C22 C12 C62 117.5(6) . . ? C13 O13 Cu2 123.0(4) . . ? O13 C13 C23 125.2(6) . . ? O13 C13 C63 116.9(6) . . ? C23 C13 C63 117.9(6) . . ? C14 O14 Cu1 128.2(4) . . ? O14 C14 C64 117.8(6) . . ? O14 C14 C24 124.3(6) . . ? C64 C14 C24 117.7(5) . . ? C31 C21 C11 118.3(6) . . ? C31 C21 C211 118.0(6) . . ? C11 C21 C211 123.6(5) . . ? C12 C22 C32 120.2(6) . . ? C12 C22 C221 123.6(6) . . ? C32 C22 C221 116.1(6) . . ? C13 C23 C33 119.1(6) . . ? C13 C23 C231 122.3(6) . . ? C33 C23 C231 118.3(6) . . ? C14 C24 C34 119.6(6) . . ? C14 C24 C241 122.4(5) . . ? C34 C24 C241 117.8(6) . . ? C41 C31 C21 123.0(6) . . ? C43 C33 C23 123.9(7) . . ? C44 C34 C24 122.4(6) . . ? C51 C41 C31 117.2(6) . . ? C51 C41 C411 122.7(6) . . ? C31 C41 C411 120.1(6) . . ? C32 C42 C52 115.9(6) . . ? C32 C42 C421 123.4(6) . . ? C52 C42 C421 120.7(5) . . ? C33 C43 C53 116.9(6) . . ? C33 C43 C431 122.2(7) . . ? C53 C43 C431 120.8(6) . . ? C34 C44 C54 117.8(6) . . ? C34 C44 C441 123.0(6) . . ? C54 C44 C441 119.2(5) . . ? C41 C51 C61 123.4(6) . . ? C62 C52 C42 122.4(6) . . ? C43 C53 C63 120.6(6) . . ? C44 C54 C64 121.8(6) . . ? C11 C61 C51 119.5(6) . . ? C11 C61 C611 117.8(5) . . ? C51 C61 C611 122.6(5) . . ? C52 C62 C12 120.7(6) . . ? C52 C62 C621 121.4(6) . . ? C12 C62 C621 117.9(5) . . ? C53 C63 C13 121.1(7) . . ? C53 C63 C631 121.2(6) . . ? C13 C63 C631 117.5(6) . . ? C54 C64 C14 120.5(6) . . ? C54 C64 C641 122.4(5) . . ? C14 C64 C641 116.8(5) . . ? N212 C211 C21 122.3(6) . . ? C211 N212 O213 113.4(5) . . ? C211 N212 Cu1 128.8(4) . . ? O213 N212 Cu1 117.5(3) . . ? N222 C221 C22 122.9(6) . . ? C221 N222 O223 111.6(5) . . ? C221 N222 Cu2 128.9(5) . . ? O223 N222 Cu2 119.5(4) . . ? N232 C231 C23 121.5(6) . . ? C231 N232 O233 113.8(5) . . ? C231 N232 Cu2 129.0(5) . . ? O233 N232 Cu2 116.9(4) . . ? N242 C241 C24 123.3(6) . . ? C241 N242 O243 113.6(5) . . ? C241 N242 Cu1 129.5(4) . . ? O243 N242 Cu1 116.6(3) . . ? C412 C411 C414 111.7(7) . . ? C412 C411 C41 109.5(5) . . ? C414 C411 C41 111.6(6) . . ? C412 C411 C413 109.1(8) . . ? C414 C411 C413 106.4(6) . . ? C41 C411 C413 108.4(6) . . ? C422 C421 C423 109.4(6) . . ? C422 C421 C42 112.3(5) . . ? C423 C421 C42 110.6(5) . . ? C422 C421 C424 108.6(6) . . ? C423 C421 C424 107.7(6) . . ? C42 C421 C424 108.2(5) . . ? C434 C431 C433 112.6(7) . . ? C434 C431 C432 106.2(7) . . ? C433 C431 C432 108.6(6) . . ? C434 C431 C43 108.3(6) . . ? C433 C431 C43 109.2(6) . . ? C432 C431 C43 112.0(6) . . ? C444 C441 C442 109.1(6) . . ? C444 C441 C443 107.1(6) . . ? C442 C441 C443 110.4(6) . . ? C444 C441 C44 112.6(5) . . ? C442 C441 C44 108.3(5) . . ? C443 C441 C44 109.4(5) . . ? C61 C611 N612 111.5(5) . . ? C613 N612 C614 112.6(5) . . ? C613 N612 C611 111.6(4) . . ? C614 N612 C611 110.6(4) . . ? N612 C614 C615 114.6(5) . . ? C616 C615 C614 112.5(5) . . ? C615 C616 C626 116.1(5) . . ? C62 C621 N622 111.1(5) . . ? C624 N622 C623 113.8(5) . . ? C624 N622 C621 109.9(4) . . ? C623 N622 C621 109.5(5) . . ? N622 C624 C625 113.4(5) . . ? C624 C625 C626 110.4(5) . . ? C616 C626 C625 116.0(5) . . ? C63 C631 N632 110.5(5) . . ? C633 N632 C634 111.0(5) . . ? C633 N632 C631 112.1(5) . . ? C634 N632 C631 111.1(5) . . ? C635 C634 N632 114.5(5) . . ? C634 C635 C636 111.6(6) . . ? C635 C636 C646 116.3(5) . . ? C64 C641 N642 108.6(5) . . ? C643 N642 C644 113.0(5) . . ? C643 N642 C641 109.7(4) . . ? C644 N642 C641 111.1(5) . . ? N642 C644 C645 112.0(5) . . ? C644 C645 C646 110.5(5) . . ? C636 C646 C645 114.9(5) . . ? O26 P2 O24 103.7(11) . . ? O26 P2 O21 123.6(9) . . ? O24 P2 O21 128.7(7) . . ? O26 P2 O27 120.1(10) . . ? O24 P2 O27 61.1(7) . . ? O21 P2 O27 104.2(6) . . ? O26 P2 O22 30.6(12) . . ? O24 P2 O22 109.5(7) . . ? O21 P2 O22 103.1(7) . . ? O27 P2 O22 149.8(9) . . ? O26 P2 O23 72.6(11) . . ? O24 P2 O23 109.5(7) . . ? O21 P2 O23 103.1(5) . . ? O27 P2 O23 62.5(7) . . ? O22 P2 O23 98.9(7) . . ? O26 P2 O25 108.9(9) . . ? O24 P2 O25 46.6(6) . . ? O21 P2 O25 95.7(6) . . ? O27 P2 O25 98.8(7) . . ? O22 P2 O25 90.9(7) . . ? O23 P2 O25 156.1(7) . . ? C42 C32 C22 123.2(6) . . ? O32 P3 O31 119.5(6) . . ? O32 P3 O35 47.7(5) . . ? O31 P3 O35 114.1(5) . . ? O32 P3 O34 114.9(7) . . ? O31 P3 O34 110.0(7) . . ? O35 P3 O34 134.9(9) . . ? O32 P3 O37 121.1(9) . . ? O31 P3 O37 119.1(7) . . ? O35 P3 O37 109.9(7) . . ? O34 P3 O37 35.5(8) . . ? O32 P3 O33 104.3(6) . . ? O31 P3 O33 101.8(5) . . ? O35 P3 O33 58.4(5) . . ? O34 P3 O33 104.2(7) . . ? O37 P3 O33 68.8(7) . . ? O32 P3 O36 54.1(6) . . ? O31 P3 O36 109.2(6) . . ? O35 P3 O36 101.2(6) . . ? O34 P3 O36 71.9(7) . . ? O37 P3 O36 100.9(6) . . ? O33 P3 O36 148.3(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.669 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.083 # Attachment 'SO4-NO3.cif' data_mw73 _database_code_depnum_ccdc_archive 'CCDC 783213' #TrackingRef 'SO4-NO3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H100 Cu2 N8 O12 S, 3(C2 H6 O), C2 H3 N, 2(N O3), O' _chemical_formula_sum 'C72 H121 Cu2 N11 O22 S' _chemical_formula_weight 1651.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.464(2) _cell_length_b 18.668(4) _cell_length_c 21.678(4) _cell_angle_alpha 78.77(3) _cell_angle_beta 85.67(3) _cell_angle_gamma 85.96(3) _cell_volume 4135.0(14) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 14691 _cell_measurement_theta_min 6.6 _cell_measurement_theta_max 71.6 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 1.502 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7176 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details Empirical _exptl_special_details ; Higashi, T. (1995). Empirical Absorption Correction based on Fourier Series Approximation. Rigaku Corporation, 3-9-12 Matsubara, Akishima, Tokyo 196-8666, JAPAN.' ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'confocal optics' _diffrn_measurement_device_type 'Rigaku Spider' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 71567 _diffrn_reflns_av_R_equivalents 0.0649 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 6.62 _diffrn_reflns_theta_max 61.16 _reflns_number_total 12207 _reflns_number_gt 8871 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crystal Clear (Rigaku, 2005)' _computing_cell_refinement 'FS Process (Rigaku, 1998)' _computing_data_reduction 'FS Process (Rigaku, 1998)' _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^)+(0.0889P)^2^+6.4773P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12207 _refine_ls_number_parameters 985 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.0921 _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.1944 _refine_ls_wR_factor_gt 0.1689 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.003 _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 0.45513(6) 0.58780(3) 0.25067(3) 0.0274(2) Uani 1 1 d . . . N1 N 0.1717(7) 0.2494(3) 0.4892(3) 0.0617(16) Uani 1 1 d . . . O1W O -0.3594(6) 0.2528(3) 0.5205(2) 0.0998(19) Uani 1 1 d . . . Cu2 Cu 1.07543(6) 0.51387(3) 0.23788(3) 0.0254(2) Uani 1 1 d . . . N2 N 0.3588(5) 0.7171(2) -0.0144(2) 0.0365(11) Uani 1 1 d . . . S1 S 0.76163(11) 0.54545(6) 0.24711(5) 0.0271(3) Uani 1 1 d D . . O1 O 0.8829(3) 0.55751(17) 0.27318(15) 0.0339(8) Uani 1 1 d D A . O2 O 0.7515(4) 0.5853(2) 0.18310(18) 0.0447(12) Uani 0.80 1 d PD A 1 O3 O 0.6540(4) 0.5712(2) 0.2880(2) 0.0394(11) Uani 0.80 1 d PD A 1 O4 O 0.7487(4) 0.4665(2) 0.2500(2) 0.0421(12) Uani 0.80 1 d PD A 1 O2A O 0.8000(14) 0.5357(9) 0.1811(5) 0.0447(12) Uani 0.20 1 d PD A 2 O3A O 0.6686(12) 0.6023(7) 0.2481(7) 0.0394(11) Uani 0.20 1 d PD A 2 O4A O 0.7218(16) 0.4728(7) 0.2792(7) 0.0421(12) Uani 0.20 1 d PD A 2 O11 O 0.4782(3) 0.68243(16) 0.20167(14) 0.0304(8) Uani 1 1 d . A . C11 C 0.5117(4) 0.7394(2) 0.2234(2) 0.0283(11) Uani 1 1 d . . . O12 O 1.0345(3) 0.43102(15) 0.20406(14) 0.0267(7) Uani 1 1 d . . . C12 C 1.0117(4) 0.3644(2) 0.2367(2) 0.0262(11) Uani 1 1 d . . . O13 O 0.4259(3) 0.49284(16) 0.29882(14) 0.0292(8) Uani 1 1 d . A . C13 C 0.4115(4) 0.4323(2) 0.2778(2) 0.0245(11) Uani 1 1 d . . . O14 O 1.1371(3) 0.59349(15) 0.26904(14) 0.0276(8) Uani 1 1 d . . . C14 C 1.1314(4) 0.6627(2) 0.2392(2) 0.0272(11) Uani 1 1 d . . . O20 O 0.0546(6) 0.2722(2) 0.4819(2) 0.0725(14) Uani 1 1 d . . . C21 C 0.4873(4) 0.7494(2) 0.2865(2) 0.0276(11) Uani 1 1 d . A . O21 O 0.1941(6) 0.2064(3) 0.5400(2) 0.0998(19) Uani 1 1 d . . . C22 C 1.0424(4) 0.3384(2) 0.2996(2) 0.0274(11) Uani 1 1 d . . . O22 O 0.2569(6) 0.2683(3) 0.4499(3) 0.109(2) Uani 1 1 d . . . C23 C 0.3830(4) 0.4295(2) 0.2157(2) 0.0267(11) Uani 1 1 d . A . O23 O 0.3715(4) 0.7514(2) 0.02746(18) 0.0515(10) Uani 1 1 d . . . C24 C 1.1465(4) 0.6846(2) 0.1732(2) 0.0250(11) Uani 1 1 d . . . O24 O 0.2474(4) 0.7082(2) -0.0290(2) 0.0563(11) Uani 1 1 d . . . O25 O 0.4538(4) 0.6903(2) -0.04140(18) 0.0619(12) Uani 1 1 d . . . C31 C 0.5233(5) 0.8136(2) 0.3040(2) 0.0330(12) Uani 1 1 d . . . H31A H 0.5042 0.8198 0.3453 0.040 Uiso 1 1 calc R A . C32 C 1.0163(5) 0.2659(2) 0.3290(2) 0.0289(11) Uani 1 1 d . . . H32A H 1.0396 0.2492 0.3701 0.035 Uiso 1 1 calc R . . C33 C 0.3661(5) 0.3615(2) 0.1988(2) 0.0311(12) Uani 1 1 d . . . H33A H 0.3439 0.3611 0.1581 0.037 Uiso 1 1 calc R A . C34 C 1.1556(5) 0.7591(2) 0.1468(2) 0.0317(12) Uani 1 1 d . . . H34A H 1.1713 0.7726 0.1034 0.038 Uiso 1 1 calc R . . C41 C 0.5863(5) 0.8682(2) 0.2622(2) 0.0319(12) Uani 1 1 d . A . C42 C 0.9577(5) 0.2185(2) 0.2995(2) 0.0300(12) Uani 1 1 d . . . C43 C 0.3809(5) 0.2957(2) 0.2401(2) 0.0326(12) Uani 1 1 d . A . C44 C 1.1421(5) 0.8135(2) 0.1827(2) 0.0329(12) Uani 1 1 d . . . C51 C 0.6133(5) 0.8561(2) 0.2008(2) 0.0335(12) Uani 1 1 d . . . H51A H 0.6565 0.8911 0.1718 0.040 Uiso 1 1 calc R A . C52 C 0.9249(5) 0.2464(2) 0.2377(2) 0.0312(12) Uani 1 1 d . . . H52A H 0.8841 0.2167 0.2165 0.037 Uiso 1 1 calc R . . C53 C 0.4140(5) 0.2992(3) 0.3007(2) 0.0333(12) Uani 1 1 d . . . H53A H 0.4255 0.2557 0.3296 0.040 Uiso 1 1 calc R A . C54 C 1.1126(5) 0.7912(2) 0.2469(2) 0.0319(12) Uani 1 1 d . . . H54A H 1.0972 0.8266 0.2719 0.038 Uiso 1 1 calc R . . C61 C 0.5786(5) 0.7943(2) 0.1812(2) 0.0298(12) Uani 1 1 d . A . C62 C 0.9510(4) 0.3164(2) 0.2069(2) 0.0282(11) Uani 1 1 d . . . C63 C 0.4303(4) 0.3643(2) 0.3195(2) 0.0293(11) Uani 1 1 d . A . C64 C 1.1052(5) 0.7180(2) 0.2752(2) 0.0288(11) Uani 1 1 d . . . O100 O -0.1190(6) 0.1909(3) 0.5577(3) 0.0959(17) Uani 1 1 d . . . H10A H -0.0577 0.2093 0.5361 0.144 Uiso 1 1 calc R . . C100 C 1.3956(14) 0.9758(5) -0.0502(4) 0.134(5) Uani 1 1 d . . . N100 N 1.3361(13) 1.0306(5) -0.0468(5) 0.178(5) Uani 1 1 d . . . C101 C 1.4804(14) 0.9086(5) -0.0541(4) 0.171(6) Uani 1 1 d . . . H11B H 1.4745 0.8953 -0.0943 0.256 Uiso 1 1 calc R . . H11C H 1.4536 0.8692 -0.0212 0.256 Uiso 1 1 calc R . . H11D H 1.5677 0.9182 -0.0492 0.256 Uiso 1 1 calc R . . C102 C -0.0851(9) 0.1170(4) 0.5839(4) 0.088(3) Uani 1 1 d . . . H10B H -0.0239 0.1146 0.6158 0.106 Uiso 1 1 calc R . . H10C H -0.0460 0.0920 0.5513 0.106 Uiso 1 1 calc R . . C103 C -0.1987(8) 0.0831(5) 0.6112(5) 0.121(4) Uani 1 1 d . . . H10D H -0.1777 0.0331 0.6301 0.181 Uiso 1 1 calc R . . H10E H -0.2578 0.0845 0.5791 0.181 Uiso 1 1 calc R . . H10F H -0.2374 0.1086 0.6429 0.181 Uiso 1 1 calc R . . C104 C 0.4645(12) 0.1211(9) 0.4675(6) 0.163(6) Uani 1 1 d . . . H10G H 0.5468 0.0937 0.4676 0.195 Uiso 1 1 calc R . . H10H H 0.4631 0.1575 0.4289 0.195 Uiso 1 1 calc R . . C105 C 0.3600(13) 0.0707(7) 0.4692(7) 0.173(6) Uani 1 1 d . . . H10I H 0.3713 0.0478 0.4330 0.259 Uiso 1 1 calc R . . H10J H 0.2786 0.0978 0.4688 0.259 Uiso 1 1 calc R . . H10K H 0.3627 0.0339 0.5069 0.259 Uiso 1 1 calc R . . C106 C -0.0013(9) 0.8405(5) -0.0660(4) 0.095(3) Uani 1 1 d . . . H10L H -0.0667 0.8774 -0.0574 0.114 Uiso 1 1 calc R . . H10M H -0.0351 0.8126 -0.0938 0.114 Uiso 1 1 calc R . . C107 C 0.1188(11) 0.8774(6) -0.0977(5) 0.152(5) Uani 1 1 d . . . H10N H 0.1605 0.8976 -0.0676 0.229 Uiso 1 1 calc R . . H10O H 0.0950 0.9158 -0.1319 0.229 Uiso 1 1 calc R . . H10P H 0.1764 0.8419 -0.1136 0.229 Uiso 1 1 calc R . . O200 O 0.4498(7) 0.1581(4) 0.5223(4) 0.149(3) Uani 1 1 d . . . H20A H 0.5064 0.1870 0.5195 0.224 Uiso 1 1 calc R . . C211 C 0.4302(5) 0.6939(2) 0.3356(2) 0.0311(12) Uani 1 1 d . . . H21A H 0.4059 0.7057 0.3748 0.037 Uiso 1 1 calc R A . N212 N 0.4124(4) 0.63008(19) 0.32709(17) 0.0271(9) Uani 1 1 d . A . O213 O 0.3624(3) 0.58322(17) 0.38071(15) 0.0391(9) Uani 1 1 d . . . H213 H 0.3533 0.5431 0.3721 0.047 Uiso 1 1 calc R A . C221 C 1.0932(4) 0.3830(2) 0.3385(2) 0.0284(11) Uani 1 1 d . . . H22A H 1.1175 0.3607 0.3784 0.034 Uiso 1 1 calc R . . N222 N 1.1064(4) 0.45202(19) 0.32055(18) 0.0271(9) Uani 1 1 d . . . O223 O 1.1487(3) 0.48626(16) 0.36631(14) 0.0319(8) Uani 1 1 d . . . H223 H 1.1552 0.5299 0.3518 0.038 Uiso 1 1 calc R . . C231 C 0.3834(4) 0.4945(2) 0.1661(2) 0.0262(11) Uani 1 1 d . . . H23A H 0.3558 0.4906 0.1272 0.031 Uiso 1 1 calc R A . N232 N 0.4190(4) 0.55627(19) 0.17239(17) 0.0259(9) Uani 1 1 d . A . O233 O 0.4200(3) 0.60775(16) 0.11680(14) 0.0324(8) Uani 1 1 d . . . H233 H 0.4434 0.6465 0.1233 0.039 Uiso 1 1 calc R A . C241 C 1.1430(4) 0.6329(2) 0.1309(2) 0.0254(11) Uani 1 1 d . . . H24A H 1.1667 0.6480 0.0884 0.030 Uiso 1 1 calc R . . N242 N 1.1084(4) 0.5677(2) 0.15038(17) 0.0291(10) Uani 1 1 d . . . O243 O 1.1042(3) 0.52706(16) 0.10221(14) 0.0326(8) Uani 1 1 d . . . H243 H 1.0815 0.4859 0.1176 0.039 Uiso 1 1 calc R . . O300 O 0.0301(5) 0.7931(3) -0.0085(2) 0.0946(17) Uani 1 1 d . . . H30A H 0.0948 0.7675 -0.0148 0.142 Uiso 1 1 calc R . . C411 C 0.6264(6) 0.9364(3) 0.2835(2) 0.0401(14) Uani 1 1 d . . . C412 C 0.7399(7) 0.9157(3) 0.3247(3) 0.070(2) Uani 1 1 d . A . H41A H 0.7162 0.8789 0.3604 0.105 Uiso 1 1 calc R . . H41B H 0.7640 0.9582 0.3389 0.105 Uiso 1 1 calc R . . H41C H 0.8111 0.8970 0.3007 0.105 Uiso 1 1 calc R . . C413 C 0.6727(8) 0.9955(3) 0.2271(3) 0.083(2) Uani 1 1 d . A . H41D H 0.6042 1.0106 0.1995 0.124 Uiso 1 1 calc R . . H41E H 0.7446 0.9756 0.2044 0.124 Uiso 1 1 calc R . . H41F H 0.6980 1.0369 0.2425 0.124 Uiso 1 1 calc R . . C414 C 0.5158(7) 0.9715(4) 0.3186(4) 0.091(3) Uani 1 1 d . A . H41G H 0.4454 0.9844 0.2918 0.136 Uiso 1 1 calc R . . H41H H 0.5432 1.0147 0.3303 0.136 Uiso 1 1 calc R . . H41I H 0.4889 0.9376 0.3557 0.136 Uiso 1 1 calc R . . C421 C 0.9284(5) 0.1405(2) 0.3323(2) 0.0386(13) Uani 1 1 d . . . C422 C 0.7817(6) 0.1356(3) 0.3423(3) 0.0579(18) Uani 1 1 d . . . H42A H 0.7477 0.1689 0.3688 0.087 Uiso 1 1 calc R . . H42B H 0.7620 0.0866 0.3620 0.087 Uiso 1 1 calc R . . H42C H 0.7439 0.1482 0.3023 0.087 Uiso 1 1 calc R . . C423 C 0.9805(6) 0.0861(3) 0.2901(3) 0.0486(15) Uani 1 1 d . . . H42D H 0.9426 0.0988 0.2501 0.073 Uiso 1 1 calc R . . H42E H 0.9594 0.0375 0.3101 0.073 Uiso 1 1 calc R . . H42F H 1.0721 0.0881 0.2836 0.073 Uiso 1 1 calc R . . C424 C 0.9884(7) 0.1183(3) 0.3957(3) 0.0627(19) Uani 1 1 d . . . H42G H 0.9548 0.1508 0.4230 0.094 Uiso 1 1 calc R . . H42H H 1.0799 0.1212 0.3895 0.094 Uiso 1 1 calc R . . H42I H 0.9683 0.0691 0.4143 0.094 Uiso 1 1 calc R . . C431 C 0.3718(5) 0.2218(2) 0.2193(3) 0.0351(13) Uani 1 1 d . . . C432 C 0.3214(7) 0.1643(3) 0.2752(3) 0.069(2) Uani 1 1 d . A . H43A H 0.2359 0.1793 0.2887 0.103 Uiso 1 1 calc R . . H43B H 0.3764 0.1599 0.3095 0.103 Uiso 1 1 calc R . . H43C H 0.3206 0.1179 0.2624 0.103 Uiso 1 1 calc R . . C433 C 0.5065(5) 0.1956(3) 0.1986(3) 0.0504(16) Uani 1 1 d . A . H43D H 0.5402 0.2309 0.1640 0.076 Uiso 1 1 calc R . . H43E H 0.5032 0.1495 0.1856 0.076 Uiso 1 1 calc R . . H43F H 0.5610 0.1899 0.2331 0.076 Uiso 1 1 calc R . . C434 C 0.2856(6) 0.2280(3) 0.1653(3) 0.067(2) Uani 1 1 d . A . H43G H 0.3165 0.2640 0.1304 0.100 Uiso 1 1 calc R . . H43H H 0.1997 0.2424 0.1786 0.100 Uiso 1 1 calc R . . H43I H 0.2861 0.1815 0.1525 0.100 Uiso 1 1 calc R . . C441 C 1.1550(6) 0.8945(3) 0.1512(3) 0.0418(14) Uani 1 1 d . . . C442 C 1.2814(8) 0.9028(3) 0.1134(4) 0.091(3) Uani 1 1 d . . . H44A H 1.2891 0.9532 0.0937 0.136 Uiso 1 1 calc R . . H44B H 1.2855 0.8732 0.0816 0.136 Uiso 1 1 calc R . . H44C H 1.3502 0.8873 0.1407 0.136 Uiso 1 1 calc R . . C443 C 1.1418(10) 0.9453(3) 0.1972(4) 0.112(4) Uani 1 1 d . . . H44D H 1.1503 0.9947 0.1749 0.168 Uiso 1 1 calc R . . H44E H 1.2076 0.9326 0.2266 0.168 Uiso 1 1 calc R . . H44F H 1.0591 0.9414 0.2195 0.168 Uiso 1 1 calc R . . C444 C 1.0481(8) 0.9174(3) 0.1045(4) 0.094(3) Uani 1 1 d . . . H44G H 1.0552 0.9677 0.0845 0.141 Uiso 1 1 calc R . . H44H H 0.9657 0.9114 0.1269 0.141 Uiso 1 1 calc R . . H44I H 1.0572 0.8873 0.0730 0.141 Uiso 1 1 calc R . . C611 C 0.6077(5) 0.7832(2) 0.1149(2) 0.0319(12) Uani 1 1 d . . . H61A H 0.6358 0.8285 0.0889 0.038 Uiso 1 1 calc R A . H61B H 0.5303 0.7709 0.0984 0.038 Uiso 1 1 calc R . . N612 N 0.7115(4) 0.7226(2) 0.11153(18) 0.0316(10) Uani 1 1 d . A . H612 H 0.6899 0.6835 0.1417 0.038 Uiso 1 1 calc R . . C613 C 0.8390(5) 0.7449(3) 0.1258(3) 0.0519(16) Uani 1 1 d . . . H61C H 0.9022 0.7053 0.1241 0.078 Uiso 1 1 calc R A . H61D H 0.8331 0.7566 0.1671 0.078 Uiso 1 1 calc R . . H61E H 0.8635 0.7870 0.0952 0.078 Uiso 1 1 calc R . . C614 C 0.7154(5) 0.6994(3) 0.0494(2) 0.0316(12) Uani 1 1 d . . . H61F H 0.7242 0.7422 0.0162 0.038 Uiso 1 1 calc R A . H61G H 0.6345 0.6790 0.0454 0.038 Uiso 1 1 calc R . . C615 C 0.8244(5) 0.6433(3) 0.0400(2) 0.0375(13) Uani 1 1 d . A . H61H H 0.8352 0.6092 0.0794 0.045 Uiso 1 1 calc R . . H61I H 0.9036 0.6681 0.0285 0.045 Uiso 1 1 calc R . . C616 C 0.8004(5) 0.6004(3) -0.0112(2) 0.0434(15) Uani 1 1 d . . . H61J H 0.7875 0.6350 -0.0501 0.052 Uiso 1 1 calc R A . H61K H 0.8770 0.5698 -0.0181 0.052 Uiso 1 1 calc R . . C621 C 0.9130(5) 0.3456(2) 0.1405(2) 0.0303(12) Uani 1 1 d . . . H62A H 0.8879 0.3056 0.1223 0.036 Uiso 1 1 calc R . . H62B H 0.9861 0.3669 0.1151 0.036 Uiso 1 1 calc R . . N622 N 0.8027(4) 0.4029(2) 0.13928(17) 0.0288(9) Uani 1 1 d . . . H622 H 0.8187 0.4329 0.1660 0.035 Uiso 1 1 calc R . . C623 C 0.6808(5) 0.3675(3) 0.1627(2) 0.0369(13) Uani 1 1 d . . . H62C H 0.6898 0.3394 0.2044 0.055 Uiso 1 1 calc R . . H62D H 0.6615 0.3358 0.1351 0.055 Uiso 1 1 calc R . . H62E H 0.6124 0.4044 0.1637 0.055 Uiso 1 1 calc R . . C624 C 0.7962(5) 0.4484(3) 0.0746(2) 0.0328(12) Uani 1 1 d . A . H62F H 0.7964 0.4161 0.0445 0.039 Uiso 1 1 calc R . . H62G H 0.8728 0.4760 0.0648 0.039 Uiso 1 1 calc R . . C625 C 0.6789(5) 0.5015(3) 0.0663(2) 0.0350(12) Uani 1 1 d . . . H62H H 0.6023 0.4741 0.0705 0.042 Uiso 1 1 calc R A . H62I H 0.6727 0.5303 0.0992 0.042 Uiso 1 1 calc R . . C626 C 0.6858(5) 0.5518(3) 0.0030(2) 0.0396(14) Uani 1 1 d . A . H62J H 0.6077 0.5831 -0.0004 0.048 Uiso 1 1 calc R . . H62K H 0.6874 0.5223 -0.0293 0.048 Uiso 1 1 calc R . . C631 C 0.4773(4) 0.3680(2) 0.3818(2) 0.0298(12) Uani 1 1 d . . . H63A H 0.4727 0.3206 0.4095 0.036 Uiso 1 1 calc R A . H63B H 0.4233 0.4031 0.4010 0.036 Uiso 1 1 calc R . . N632 N 0.6158(4) 0.3908(2) 0.37360(18) 0.0293(10) Uani 1 1 d . A . H632 H 0.6218 0.4284 0.3400 0.035 Uiso 1 1 calc R . . C633 C 0.7045(5) 0.3289(3) 0.3595(3) 0.0442(14) Uani 1 1 d . . . H63C H 0.7911 0.3441 0.3536 0.066 Uiso 1 1 calc R A . H63D H 0.6810 0.3147 0.3218 0.066 Uiso 1 1 calc R . . H63E H 0.6985 0.2881 0.3940 0.066 Uiso 1 1 calc R . . C634 C 0.6498(5) 0.4178(3) 0.4307(2) 0.0329(12) Uani 1 1 d . . . H63F H 0.6287 0.3815 0.4680 0.040 Uiso 1 1 calc R A . H63G H 0.5981 0.4623 0.4339 0.040 Uiso 1 1 calc R . . C635 C 0.7917(5) 0.4333(3) 0.4294(2) 0.0373(13) Uani 1 1 d . A . H63H H 0.8436 0.3878 0.4313 0.045 Uiso 1 1 calc R . . H63I H 0.8157 0.4656 0.3901 0.045 Uiso 1 1 calc R . . C636 C 0.8183(5) 0.4684(3) 0.4843(2) 0.0419(14) Uani 1 1 d . . . H63J H 0.9097 0.4749 0.4829 0.050 Uiso 1 1 calc R A . H63K H 0.7961 0.4349 0.5232 0.050 Uiso 1 1 calc R . . C641 C 1.0586(5) 0.6940(2) 0.3424(2) 0.0306(12) Uani 1 1 d . . . H64A H 1.0531 0.7354 0.3636 0.037 Uiso 1 1 calc R . . H64B H 1.1192 0.6572 0.3634 0.037 Uiso 1 1 calc R . . N642 N 0.9289(4) 0.66283(19) 0.34642(17) 0.0264(9) Uani 1 1 d . . . H642 H 0.9329 0.6313 0.3191 0.032 Uiso 1 1 calc R . . C643 C 0.8275(5) 0.7213(3) 0.3258(2) 0.0378(13) Uani 1 1 d . . . H64C H 0.7461 0.6999 0.3282 0.057 Uiso 1 1 calc R . . H64D H 0.8484 0.7450 0.2831 0.057 Uiso 1 1 calc R . . H64E H 0.8229 0.7567 0.3528 0.057 Uiso 1 1 calc R . . C644 C 0.8988(5) 0.6194(2) 0.4112(2) 0.0290(11) Uani 1 1 d . A . H64F H 0.9198 0.6475 0.4420 0.035 Uiso 1 1 calc R . . H64G H 0.9538 0.5749 0.4169 0.035 Uiso 1 1 calc R . . C645 C 0.7612(5) 0.5989(3) 0.4250(2) 0.0352(12) Uani 1 1 d . . . H64H H 0.7335 0.5792 0.3903 0.042 Uiso 1 1 calc R A . H64I H 0.7067 0.6423 0.4289 0.042 Uiso 1 1 calc R . . C646 C 0.7471(5) 0.5418(3) 0.4863(2) 0.0425(14) Uani 1 1 d . A . H64J H 0.7780 0.5616 0.5202 0.051 Uiso 1 1 calc R . . H64K H 0.6566 0.5339 0.4962 0.051 Uiso 1 1 calc R . . 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 0.0288(4) 0.0278(4) 0.0268(4) -0.0098(3) 0.0000(3) 0.0010(3) N1 0.095(5) 0.048(3) 0.047(3) -0.017(3) -0.023(4) 0.008(3) O1W 0.164(6) 0.058(3) 0.073(3) -0.006(2) -0.001(4) 0.005(3) Cu2 0.0255(4) 0.0246(3) 0.0268(4) -0.0080(3) 0.0006(3) -0.0009(3) N2 0.044(3) 0.033(2) 0.033(2) -0.0058(19) -0.006(2) -0.002(2) S1 0.0246(7) 0.0346(6) 0.0236(6) -0.0092(5) -0.0022(5) -0.0007(5) O1 0.028(2) 0.0411(19) 0.0376(19) -0.0207(15) -0.0022(16) -0.0017(15) O2 0.053(3) 0.051(3) 0.028(2) 0.001(2) -0.007(2) -0.006(2) O3 0.027(2) 0.059(3) 0.034(3) -0.018(2) 0.004(2) 0.003(2) O4 0.044(3) 0.028(2) 0.059(4) -0.018(2) -0.003(3) -0.0014(19) O2A 0.053(3) 0.051(3) 0.028(2) 0.001(2) -0.007(2) -0.006(2) O3A 0.027(2) 0.059(3) 0.034(3) -0.018(2) 0.004(2) 0.003(2) O4A 0.044(3) 0.028(2) 0.059(4) -0.018(2) -0.003(3) -0.0014(19) O11 0.035(2) 0.0290(17) 0.0289(18) -0.0071(14) -0.0036(15) -0.0046(14) C11 0.023(3) 0.027(2) 0.037(3) -0.013(2) -0.008(2) 0.004(2) O12 0.0273(19) 0.0218(15) 0.0320(18) -0.0068(13) -0.0015(15) -0.0042(13) C12 0.022(3) 0.027(2) 0.029(3) -0.007(2) 0.001(2) 0.004(2) O13 0.031(2) 0.0274(16) 0.0297(18) -0.0076(13) 0.0007(15) -0.0015(14) C13 0.016(3) 0.027(2) 0.032(3) -0.012(2) 0.000(2) 0.0034(19) O14 0.030(2) 0.0226(15) 0.0322(18) -0.0080(13) -0.0040(15) -0.0035(13) C14 0.019(3) 0.029(2) 0.033(3) -0.005(2) 0.000(2) -0.002(2) O20 0.111(4) 0.063(3) 0.048(3) -0.018(2) -0.004(3) -0.009(3) C21 0.026(3) 0.024(2) 0.034(3) -0.009(2) -0.001(2) 0.001(2) O21 0.155(6) 0.085(4) 0.052(3) -0.001(3) -0.027(3) 0.030(4) C22 0.021(3) 0.032(2) 0.030(3) -0.012(2) -0.003(2) 0.006(2) O22 0.094(5) 0.116(5) 0.094(4) 0.031(4) 0.003(4) -0.002(4) C23 0.019(3) 0.031(2) 0.030(3) -0.009(2) 0.001(2) 0.000(2) O23 0.056(3) 0.058(2) 0.049(2) -0.026(2) -0.011(2) -0.004(2) C24 0.017(3) 0.026(2) 0.032(3) -0.0071(19) 0.002(2) -0.0013(19) O24 0.044(3) 0.064(3) 0.069(3) -0.026(2) -0.019(2) -0.005(2) O25 0.053(3) 0.089(3) 0.047(2) -0.028(2) -0.005(2) 0.019(2) C31 0.032(3) 0.032(2) 0.037(3) -0.011(2) -0.005(2) 0.010(2) C32 0.027(3) 0.024(2) 0.036(3) -0.008(2) 0.000(2) -0.002(2) C33 0.026(3) 0.037(3) 0.033(3) -0.014(2) -0.003(2) 0.001(2) C34 0.029(3) 0.031(2) 0.033(3) -0.004(2) 0.001(2) 0.000(2) C41 0.039(3) 0.021(2) 0.036(3) -0.007(2) -0.006(2) 0.005(2) C42 0.027(3) 0.025(2) 0.038(3) -0.008(2) 0.001(2) -0.004(2) C43 0.021(3) 0.034(3) 0.044(3) -0.010(2) 0.002(2) -0.001(2) C44 0.025(3) 0.031(2) 0.042(3) -0.008(2) 0.000(2) -0.003(2) C51 0.035(3) 0.026(2) 0.038(3) -0.002(2) -0.007(2) 0.000(2) C52 0.026(3) 0.027(2) 0.043(3) -0.016(2) 0.001(2) -0.003(2) C53 0.030(3) 0.030(2) 0.039(3) -0.005(2) -0.002(2) 0.003(2) C54 0.030(3) 0.028(2) 0.040(3) -0.011(2) -0.002(2) -0.002(2) C61 0.032(3) 0.026(2) 0.031(3) -0.005(2) -0.007(2) 0.005(2) C62 0.024(3) 0.030(2) 0.034(3) -0.014(2) -0.001(2) 0.004(2) C63 0.022(3) 0.032(2) 0.034(3) -0.009(2) 0.000(2) 0.000(2) C64 0.025(3) 0.029(2) 0.034(3) -0.010(2) -0.001(2) -0.003(2) O100 0.129(5) 0.062(3) 0.094(4) -0.012(3) 0.005(3) -0.009(3) C100 0.283(16) 0.066(6) 0.051(5) 0.005(4) 0.004(7) -0.054(8) N100 0.303(15) 0.084(6) 0.131(8) 0.023(6) 0.007(8) -0.047(8) C101 0.37(2) 0.063(6) 0.080(7) -0.011(5) -0.005(9) -0.029(9) C102 0.116(7) 0.068(5) 0.078(5) -0.008(4) 0.003(5) -0.010(5) C103 0.077(7) 0.110(7) 0.155(9) 0.022(7) -0.007(6) -0.008(6) C104 0.109(10) 0.261(17) 0.141(11) -0.107(12) -0.020(8) 0.030(10) C105 0.151(12) 0.178(12) 0.217(15) -0.108(11) -0.090(11) 0.077(10) C106 0.122(8) 0.086(6) 0.070(5) -0.003(4) -0.017(5) 0.026(5) C107 0.181(12) 0.134(9) 0.118(8) 0.062(7) -0.024(8) -0.065(8) O200 0.133(6) 0.167(7) 0.154(7) -0.041(6) -0.004(5) -0.019(5) C211 0.030(3) 0.035(3) 0.029(3) -0.011(2) 0.002(2) 0.002(2) N212 0.025(2) 0.031(2) 0.026(2) -0.0059(16) -0.0011(17) 0.0007(17) O213 0.051(2) 0.0336(18) 0.0327(19) -0.0087(15) 0.0104(17) -0.0109(16) C221 0.024(3) 0.031(2) 0.032(3) -0.010(2) -0.003(2) 0.001(2) N222 0.023(2) 0.030(2) 0.032(2) -0.0147(17) -0.0009(18) 0.0005(17) O223 0.043(2) 0.0264(16) 0.0282(18) -0.0073(14) -0.0048(16) -0.0083(15) C231 0.021(3) 0.028(2) 0.031(3) -0.010(2) -0.001(2) 0.003(2) N232 0.024(2) 0.028(2) 0.026(2) -0.0055(16) 0.0007(17) 0.0034(17) O233 0.040(2) 0.0291(16) 0.0284(18) -0.0054(14) -0.0017(16) -0.0020(15) C241 0.019(3) 0.030(2) 0.026(2) -0.0051(19) -0.001(2) 0.004(2) N242 0.032(3) 0.031(2) 0.027(2) -0.0129(17) -0.0003(18) 0.0007(18) O243 0.041(2) 0.0287(16) 0.0309(18) -0.0126(14) 0.0010(16) -0.0036(15) O300 0.094(4) 0.085(4) 0.092(4) 0.000(3) 0.025(3) 0.007(3) C411 0.058(4) 0.026(2) 0.039(3) -0.007(2) -0.015(3) -0.004(2) C412 0.089(6) 0.042(3) 0.088(5) -0.021(3) -0.028(4) -0.007(3) C413 0.152(8) 0.033(3) 0.064(4) -0.005(3) -0.009(5) -0.025(4) C414 0.083(6) 0.058(4) 0.148(8) -0.070(5) 0.026(5) -0.014(4) C421 0.049(4) 0.023(2) 0.046(3) -0.010(2) -0.004(3) -0.007(2) C422 0.059(4) 0.030(3) 0.082(5) -0.010(3) 0.024(4) -0.013(3) C423 0.053(4) 0.026(3) 0.069(4) -0.014(3) 0.000(3) -0.004(2) C424 0.103(6) 0.036(3) 0.047(4) 0.006(3) -0.017(4) -0.014(3) C431 0.026(3) 0.026(2) 0.055(3) -0.014(2) -0.001(3) 0.000(2) C432 0.088(5) 0.038(3) 0.084(5) -0.026(3) 0.030(4) -0.026(3) C433 0.038(4) 0.048(3) 0.071(4) -0.030(3) 0.000(3) 0.002(3) C434 0.060(5) 0.045(3) 0.110(6) -0.040(4) -0.050(4) 0.008(3) C441 0.050(4) 0.027(3) 0.047(3) -0.006(2) 0.001(3) -0.003(2) C442 0.105(6) 0.042(4) 0.109(6) 0.004(4) 0.048(5) -0.011(4) C443 0.227(11) 0.033(3) 0.073(5) -0.012(3) 0.032(6) -0.025(5) C444 0.109(7) 0.040(4) 0.129(7) 0.006(4) -0.046(6) 0.003(4) C611 0.036(3) 0.026(2) 0.032(3) -0.003(2) -0.004(2) 0.001(2) N612 0.029(3) 0.036(2) 0.030(2) -0.0070(18) -0.0039(19) -0.0013(18) C613 0.033(4) 0.074(4) 0.056(4) -0.028(3) -0.008(3) -0.004(3) C614 0.033(3) 0.035(3) 0.028(3) -0.008(2) -0.006(2) 0.001(2) C615 0.034(3) 0.042(3) 0.033(3) -0.003(2) 0.003(2) 0.002(2) C616 0.054(4) 0.049(3) 0.023(3) -0.003(2) -0.001(3) 0.021(3) C621 0.028(3) 0.030(2) 0.037(3) -0.016(2) -0.001(2) 0.002(2) N622 0.023(2) 0.036(2) 0.031(2) -0.0136(17) -0.0034(18) 0.0000(17) C623 0.024(3) 0.055(3) 0.032(3) -0.011(2) 0.004(2) -0.005(2) C624 0.028(3) 0.036(3) 0.038(3) -0.015(2) -0.004(2) -0.001(2) C625 0.022(3) 0.043(3) 0.044(3) -0.018(2) -0.009(2) 0.009(2) C626 0.044(4) 0.046(3) 0.033(3) -0.018(2) -0.012(3) 0.014(3) C631 0.026(3) 0.033(2) 0.029(3) -0.004(2) 0.004(2) -0.004(2) N632 0.027(2) 0.032(2) 0.029(2) -0.0059(17) -0.0005(18) -0.0015(18) C633 0.033(3) 0.057(3) 0.047(3) -0.023(3) -0.004(3) 0.014(3) C634 0.035(3) 0.031(2) 0.033(3) -0.007(2) 0.001(2) -0.002(2) C635 0.032(3) 0.038(3) 0.039(3) -0.002(2) 0.000(2) -0.005(2) C636 0.042(4) 0.055(3) 0.028(3) -0.001(2) -0.008(3) -0.014(3) C641 0.033(3) 0.032(2) 0.030(3) -0.012(2) -0.006(2) -0.001(2) N642 0.027(2) 0.0295(19) 0.024(2) -0.0105(16) -0.0015(17) 0.0007(17) C643 0.041(3) 0.036(3) 0.033(3) -0.005(2) 0.000(2) 0.007(2) C644 0.031(3) 0.034(2) 0.023(2) -0.010(2) -0.002(2) -0.002(2) C645 0.033(3) 0.047(3) 0.028(3) -0.015(2) -0.003(2) 0.002(2) C646 0.047(4) 0.061(3) 0.023(3) -0.015(2) 0.002(3) -0.016(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 O11 1.897(3) . ? Cu1 O13 1.906(3) . ? Cu1 N232 1.971(4) . ? Cu1 N212 1.979(4) . ? Cu1 O3A 2.264(14) . ? Cu1 O3 2.269(4) . ? N1 O22 1.208(7) . ? N1 O21 1.257(6) . ? N1 O20 1.280(7) . ? Cu2 O14 1.917(3) . ? Cu2 O12 1.922(3) . ? Cu2 N222 1.969(4) . ? Cu2 N242 1.983(4) . ? Cu2 O1 2.256(3) . ? N2 O23 1.228(5) . ? N2 O25 1.240(5) . ? N2 O24 1.260(5) . ? S1 O3A 1.391(10) . ? S1 O2 1.448(4) . ? S1 O4A 1.471(11) . ? S1 O1 1.476(3) . ? S1 O4 1.478(4) . ? S1 O3 1.491(4) . ? S1 O2A 1.498(10) . ? O11 C11 1.322(5) . ? C11 C21 1.418(6) . ? C11 C61 1.419(6) . ? O12 C12 1.333(5) . ? C12 C62 1.410(7) . ? C12 C22 1.410(6) . ? O13 C13 1.321(5) . ? C13 C23 1.412(7) . ? C13 C63 1.419(6) . ? O14 C14 1.327(5) . ? C14 C24 1.409(6) . ? C14 C64 1.410(6) . ? C21 C31 1.409(6) . ? C21 C211 1.459(6) . ? C22 C32 1.414(6) . ? C22 C221 1.446(7) . ? C23 C33 1.415(6) . ? C23 C231 1.455(6) . ? C24 C34 1.403(6) . ? C24 C241 1.459(6) . ? C31 C41 1.393(7) . ? C32 C42 1.386(7) . ? C33 C43 1.378(7) . ? C34 C44 1.390(6) . ? C41 C51 1.398(7) . ? C41 C411 1.530(7) . ? C42 C52 1.400(7) . ? C42 C421 1.533(6) . ? C43 C53 1.399(7) . ? C43 C431 1.543(6) . ? C44 C54 1.391(7) . ? C44 C441 1.543(6) . ? C51 C61 1.384(6) . ? C52 C62 1.382(6) . ? C53 C63 1.380(6) . ? C54 C64 1.390(6) . ? C61 C611 1.496(6) . ? C62 C621 1.510(7) . ? C63 C631 1.487(7) . ? C64 C641 1.494(6) . ? O100 C102 1.418(8) . ? C100 N100 1.172(14) . ? C100 C101 1.496(16) . ? C102 C103 1.421(10) . ? C104 O200 1.478(12) . ? C104 C105 1.486(16) . ? C106 O300 1.426(8) . ? C106 C107 1.527(12) . ? C211 N212 1.269(6) . ? N212 O213 1.402(5) . ? C221 N222 1.285(6) . ? N222 O223 1.394(5) . ? C231 N232 1.271(6) . ? N232 O233 1.387(4) . ? C241 N242 1.277(5) . ? N242 O243 1.410(5) . ? C411 C414 1.517(8) . ? C411 C412 1.523(8) . ? C411 C413 1.552(8) . ? C421 C424 1.525(8) . ? C421 C423 1.541(7) . ? C421 C422 1.541(8) . ? C431 C434 1.514(8) . ? C431 C433 1.524(7) . ? C431 C432 1.540(7) . ? C441 C443 1.498(8) . ? C441 C442 1.504(8) . ? C441 C444 1.548(9) . ? C611 N612 1.521(6) . ? N612 C614 1.490(6) . ? N612 C613 1.495(7) . ? C614 C615 1.524(6) . ? C615 C616 1.533(7) . ? C616 C626 1.531(8) . ? C621 N622 1.515(5) . ? N622 C623 1.488(6) . ? N622 C624 1.495(6) . ? C624 C625 1.521(6) . ? C625 C626 1.503(7) . ? C631 N632 1.527(6) . ? N632 C633 1.496(6) . ? N632 C634 1.500(6) . ? C634 C635 1.530(7) . ? C635 C636 1.519(7) . ? C636 C646 1.519(7) . ? C641 N642 1.504(6) . ? N642 C643 1.496(6) . ? N642 C644 1.502(5) . ? C644 C645 1.508(7) . ? C645 C646 1.539(7) . ? 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 O11 Cu1 O13 177.92(15) . . ? O11 Cu1 N232 87.67(14) . . ? O13 Cu1 N232 91.17(14) . . ? O11 Cu1 N212 90.66(14) . . ? O13 Cu1 N212 89.68(14) . . ? N232 Cu1 N212 155.51(16) . . ? O11 Cu1 O3A 75.1(4) . . ? O13 Cu1 O3A 106.9(4) . . ? N232 Cu1 O3A 108.0(4) . . ? N212 Cu1 O3A 95.2(4) . . ? O11 Cu1 O3 96.14(16) . . ? O13 Cu1 O3 85.94(16) . . ? N232 Cu1 O3 121.47(14) . . ? N212 Cu1 O3 83.01(15) . . ? O3A Cu1 O3 24.2(4) . . ? O22 N1 O21 121.3(7) . . ? O22 N1 O20 122.2(6) . . ? O21 N1 O20 116.5(7) . . ? O14 Cu2 O12 173.20(13) . . ? O14 Cu2 N222 87.63(14) . . ? O12 Cu2 N222 91.79(14) . . ? O14 Cu2 N242 89.64(14) . . ? O12 Cu2 N242 88.62(14) . . ? N222 Cu2 N242 160.18(16) . . ? O14 Cu2 O1 83.15(12) . . ? O12 Cu2 O1 103.65(12) . . ? N222 Cu2 O1 92.34(14) . . ? N242 Cu2 O1 106.82(14) . . ? O23 N2 O25 120.7(5) . . ? O23 N2 O24 119.1(4) . . ? O25 N2 O24 120.1(5) . . ? O3A S1 O2 72.0(6) . . ? O3A S1 O4A 115.2(8) . . ? O2 S1 O4A 132.4(7) . . ? O3A S1 O1 113.7(6) . . ? O2 S1 O1 112.1(2) . . ? O4A S1 O1 107.1(7) . . ? O3A S1 O4 130.6(7) . . ? O2 S1 O4 110.3(3) . . ? O4A S1 O4 27.5(6) . . ? O1 S1 O4 110.4(2) . . ? O3A S1 O3 38.3(6) . . ? O2 S1 O3 109.1(3) . . ? O4A S1 O3 82.9(7) . . ? O1 S1 O3 107.6(2) . . ? O4 S1 O3 107.2(3) . . ? O3A S1 O2A 111.5(7) . . ? O2 S1 O2A 40.9(6) . . ? O4A S1 O2A 103.9(7) . . ? O1 S1 O2A 104.5(6) . . ? O4 S1 O2A 76.7(6) . . ? O3 S1 O2A 143.5(6) . . ? S1 O1 Cu2 122.51(17) . . ? S1 O3 Cu1 118.0(2) . . ? S1 O3A Cu1 123.6(9) . . ? C11 O11 Cu1 125.3(3) . . ? O11 C11 C21 124.6(4) . . ? O11 C11 C61 118.2(4) . . ? C21 C11 C61 117.2(4) . . ? C12 O12 Cu2 126.5(3) . . ? O12 C12 C62 118.3(4) . . ? O12 C12 C22 124.6(4) . . ? C62 C12 C22 117.1(4) . . ? C13 O13 Cu1 127.8(3) . . ? O13 C13 C23 124.9(4) . . ? O13 C13 C63 118.3(4) . . ? C23 C13 C63 116.8(4) . . ? C14 O14 Cu2 124.6(3) . . ? O14 C14 C24 124.0(4) . . ? O14 C14 C64 118.5(4) . . ? C24 C14 C64 117.5(4) . . ? C31 C21 C11 119.9(4) . . ? C31 C21 C211 117.7(4) . . ? C11 C21 C211 122.4(4) . . ? C12 C22 C32 119.6(4) . . ? C12 C22 C221 123.7(4) . . ? C32 C22 C221 116.5(4) . . ? C13 C23 C33 120.0(4) . . ? C13 C23 C231 121.5(4) . . ? C33 C23 C231 118.2(4) . . ? C34 C24 C14 119.4(4) . . ? C34 C24 C241 118.5(4) . . ? C14 C24 C241 121.9(4) . . ? C41 C31 C21 122.9(4) . . ? C42 C32 C22 123.2(5) . . ? C43 C33 C23 122.9(5) . . ? C44 C34 C24 122.8(4) . . ? C31 C41 C51 116.3(4) . . ? C31 C41 C411 121.2(4) . . ? C51 C41 C411 122.5(4) . . ? C32 C42 C52 116.0(4) . . ? C32 C42 C421 122.7(4) . . ? C52 C42 C421 121.3(4) . . ? C33 C43 C53 116.3(4) . . ? C33 C43 C431 122.0(5) . . ? C53 C43 C431 121.5(4) . . ? C34 C44 C54 116.6(4) . . ? C34 C44 C441 120.5(4) . . ? C54 C44 C441 122.9(4) . . ? C61 C51 C41 122.9(4) . . ? C62 C52 C42 122.5(5) . . ? C63 C53 C43 122.9(4) . . ? C64 C54 C44 122.4(4) . . ? C51 C61 C11 120.8(4) . . ? C51 C61 C611 121.6(4) . . ? C11 C61 C611 117.5(4) . . ? C52 C62 C12 121.6(5) . . ? C52 C62 C621 121.5(4) . . ? C12 C62 C621 116.9(4) . . ? C53 C63 C13 121.0(5) . . ? C53 C63 C631 123.1(4) . . ? C13 C63 C631 115.8(4) . . ? C54 C64 C14 120.5(4) . . ? C54 C64 C641 122.6(4) . . ? C14 C64 C641 116.7(4) . . ? N100 C100 C101 175.8(15) . . ? O100 C102 C103 108.1(7) . . ? O200 C104 C105 111.2(11) . . ? O300 C106 C107 109.6(7) . . ? N212 C211 C21 122.5(4) . . ? C211 N212 O213 114.3(4) . . ? C211 N212 Cu1 128.6(3) . . ? O213 N212 Cu1 117.0(3) . . ? N222 C221 C22 123.2(5) . . ? C221 N222 O223 114.5(4) . . ? C221 N222 Cu2 128.5(3) . . ? O223 N222 Cu2 117.0(2) . . ? N232 C231 C23 124.5(5) . . ? C231 N232 O233 113.2(4) . . ? C231 N232 Cu1 128.0(3) . . ? O233 N232 Cu1 118.5(3) . . ? N242 C241 C24 122.2(4) . . ? C241 N242 O243 114.1(4) . . ? C241 N242 Cu2 129.4(3) . . ? O243 N242 Cu2 116.3(3) . . ? C414 C411 C412 110.6(6) . . ? C414 C411 C41 111.4(5) . . ? C412 C411 C41 109.3(4) . . ? C414 C411 C413 107.1(5) . . ? C412 C411 C413 106.1(5) . . ? C41 C411 C413 112.2(4) . . ? C424 C421 C42 112.2(4) . . ? C424 C421 C423 108.4(5) . . ? C42 C421 C423 109.8(4) . . ? C424 C421 C422 109.3(5) . . ? C42 C421 C422 108.7(4) . . ? C423 C421 C422 108.4(4) . . ? C434 C431 C433 109.0(5) . . ? C434 C431 C432 109.3(5) . . ? C433 C431 C432 108.0(4) . . ? C434 C431 C43 112.2(4) . . ? C433 C431 C43 108.0(4) . . ? C432 C431 C43 110.2(4) . . ? C443 C441 C442 110.2(6) . . ? C443 C441 C44 113.3(5) . . ? C442 C441 C44 109.6(4) . . ? C443 C441 C444 107.7(6) . . ? C442 C441 C444 107.1(6) . . ? C44 C441 C444 108.7(5) . . ? C61 C611 N612 111.4(4) . . ? C614 N612 C613 112.4(4) . . ? C614 N612 C611 110.4(4) . . ? C613 N612 C611 111.3(4) . . ? N612 C614 C615 113.7(4) . . ? C614 C615 C616 112.7(4) . . ? C626 C616 C615 115.5(4) . . ? C62 C621 N622 111.3(3) . . ? C623 N622 C624 112.8(4) . . ? C623 N622 C621 110.1(4) . . ? C624 N622 C621 110.0(3) . . ? N622 C624 C625 114.1(4) . . ? C626 C625 C624 111.6(4) . . ? C625 C626 C616 116.3(4) . . ? C63 C631 N632 110.0(4) . . ? C633 N632 C634 112.5(4) . . ? C633 N632 C631 110.1(4) . . ? C634 N632 C631 110.1(3) . . ? N632 C634 C635 113.2(4) . . ? C636 C635 C634 111.1(4) . . ? C635 C636 C646 115.5(4) . . ? C64 C641 N642 110.5(4) . . ? C643 N642 C644 112.9(3) . . ? C643 N642 C641 111.2(4) . . ? C644 N642 C641 110.6(4) . . ? N642 C644 C645 115.1(4) . . ? C644 C645 C646 110.7(4) . . ? C636 C646 C645 114.8(4) . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 61.16 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.968 _refine_diff_density_min -0.659 _refine_diff_density_rms 0.086