# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_globa _journal_name_full CrystEngComm _journal_coden_cambridge 1350 #TrackingRef '- p.cif' #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Li, Bao Department of Chemistry and Chemical Engineering Huazhong University of Science and Technology Wuhan, 430074 P. R. China ; _publ_contact_author_phone 86-592-2185191 _publ_contact_author_fax 86-592-2183047 _publ_contact_author_email libao@mail.hust.edu.cn _publ_requested_coeditor_name ? _publ_contact_letter ; ; #================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Structure and Magnetism of Heptanuclear Complexes Self-assembled by the Encapsulation of Hexacyanoferrate with Copper(II) Cations of Tridentate Ligands ; loop_ _publ_author_name _publ_author_address 'Fan Yu' ; School of chemistry and environmental engineering, Jianghan University, Wuhan, Hubei 430056, P.R. China ; 'Bao Li' ; Department of Chemistry and Chemical Engineering Huazhong University of Science and Technology Wuhan, 430074 P. R. China ; _publ_section_exptl_refinement ; All H atoms were placed geometrically with C---H = 0.93 (aromatic) or 0.96 \%A (CH~3~), N---H distances of 0.86\%A and refined using a riding atom model with their isotropic displacement factors, U~iso~ fixed at 1.2 time the U~eq~ of the parent C and N atom. ; _publ_contact_author_name 'Li, Bao' #==================================================================== #==================================================================== data_compound1 _database_code_depnum_ccdc_archive 'CCDC 822455' #TrackingRef '- p.cif' _symmetry_space_group_name_hall 'P 2 2ab' _audit_update_record ; 2011-03-14 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H32 Cu N4 O8' _chemical_formula_weight 688.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 22.708(5) _cell_length_b 10.553(2) _cell_length_c 19.758(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4734.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.965 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1428 _exptl_absorpt_coefficient_mu 0.501 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8643 _exptl_absorpt_correction_T_max 0.9065 _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID imaging plate' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7921 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0695 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7921 _reflns_number_gt 3849 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PROCESS-AUTO (Rigaku Corporation,1998)' _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan (Molecular Structure Corporation & Rigaku Corporation, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1839P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.59(3) _refine_ls_number_reflns 7921 _refine_ls_number_parameters 413 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1426 _refine_ls_R_factor_gt 0.0962 _refine_ls_wR_factor_ref 0.2804 _refine_ls_wR_factor_gt 0.2501 _refine_ls_goodness_of_fit_ref 0.919 _refine_ls_restrained_S_all 0.919 _refine_ls_shift/su_max 0.016 _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 0.22300(4) 0.65734(11) 0.28153(5) 0.0936(4) Uani 1 1 d . . . N1 N 0.1627(3) 0.7179(8) 0.3498(4) 0.102(2) Uani 1 1 d . . . N2 N -0.0055(7) 1.3645(8) 0.8241(5) 0.151(4) Uani 1 1 d . . . N3 N 0.1752(3) 0.7606(6) 0.2013(3) 0.0860(18) Uani 1 1 d . . . N4 N 0.2173(4) 1.0992(8) -0.2157(5) 0.1275(19) Uani 1 1 d . . . O5 O 0.1746(3) 0.5017(7) 0.2632(4) 0.122(2) Uani 1 1 d . . . O6 O 0.2125(4) 0.3578(9) 0.3321(4) 0.150(3) Uani 1 1 d . . . O1 O 0.0365(2) 0.8647(6) 0.4784(3) 0.0995(16) Uani 1 1 d . . . O2 O -0.0275(3) 1.1508(10) 0.6475(4) 0.138(3) Uani 1 1 d . . . O3 O 0.0698(2) 0.9646(5) 0.0736(4) 0.117(2) Uani 1 1 d . . . O4 O 0.0774(3) 0.9831(6) -0.0971(3) 0.1069(18) Uani 1 1 d . . . C1 C 0.1769(4) 0.7919(17) 0.3962(6) 0.161(6) Uani 1 1 d . . . H1A H 0.2165 0.8141 0.3987 0.194 Uiso 1 1 calc R . . C2 C 0.1384(5) 0.8473(19) 0.4468(6) 0.175(7) Uani 1 1 d . . . H2A H 0.1525 0.8966 0.4822 0.210 Uiso 1 1 calc R . . C3 C 0.0814(3) 0.8227(10) 0.4389(4) 0.093(2) Uani 1 1 d . . . C4 C 0.0654(4) 0.7375(11) 0.3844(6) 0.112(3) Uani 1 1 d . . . H4A H 0.0263 0.7135 0.3786 0.135 Uiso 1 1 calc R . . C5 C 0.1064(3) 0.6938(9) 0.3429(5) 0.094(2) Uani 1 1 d . . . H5A H 0.0946 0.6432 0.3068 0.113 Uiso 1 1 calc R . . C6 C 0.0541(4) 0.9622(11) 0.5227(5) 0.112(3) Uani 1 1 d . . . H6A H 0.0664 1.0357 0.4968 0.135 Uiso 1 1 calc R . . H6B H 0.0874 0.9340 0.5496 0.135 Uiso 1 1 calc R . . C26 C 0.0000 1.0000 -0.0129(5) 0.094(3) Uani 1 2 d S . . C19 C 0.0312(4) 0.8948(9) 0.0276(4) 0.093(2) Uani 1 1 d . . . H19A H 0.0029 0.8440 0.0525 0.112 Uiso 1 1 calc R . . H19B H 0.0537 0.8400 -0.0021 0.112 Uiso 1 1 calc R . . C15 C 0.1386(4) 0.9549(10) 0.1637(5) 0.104(3) Uani 1 1 d . . . H15A H 0.1368 1.0427 0.1668 0.125 Uiso 1 1 calc R . . C13 C 0.0000 1.0000 0.5718(5) 0.090(3) Uani 1 2 d S . . C22 C 0.1238(3) 1.0260(9) -0.1308(4) 0.089(2) Uani 1 1 d . . . C25 C 0.0452(4) 1.0750(9) -0.0568(4) 0.093(2) Uani 1 1 d . . . H25A H 0.0249 1.1345 -0.0860 0.111 Uiso 1 1 calc R . . H25B H 0.0721 1.1219 -0.0280 0.111 Uiso 1 1 calc R . . C16 C 0.1046(3) 0.8949(8) 0.1158(4) 0.0796(19) Uani 1 1 d . . . C17 C 0.1099(4) 0.7633(8) 0.1105(4) 0.088(2) Uani 1 1 d . . . H17A H 0.0902 0.7175 0.0773 0.105 Uiso 1 1 calc R . . C9 C -0.0172(5) 1.2245(11) 0.7040(6) 0.127(4) Uani 1 1 d . . . C28 C 0.1225(4) 0.3124(10) 0.2780(6) 0.117(3) Uani 1 1 d . . . C29 C 0.0801(4) 0.3521(12) 0.2340(5) 0.112(3) Uani 1 1 d . . . H29A H 0.0822 0.4322 0.2145 0.134 Uiso 1 1 calc R . . C18 C 0.1448(3) 0.7069(8) 0.1558(4) 0.087(2) Uani 1 1 d . . . H18A H 0.1471 0.6190 0.1537 0.104 Uiso 1 1 calc R . . C23 C 0.1518(5) 0.9408(12) -0.1694(6) 0.1275(19) Uani 1 1 d . . . H23A H 0.1423 0.8552 -0.1680 0.153 Uiso 1 1 calc R . . O7 O 0.2870(3) 0.7179(10) 0.3405(4) 0.142(3) Uani 1 1 d . . . C24 C 0.1979(5) 0.9888(10) -0.2137(6) 0.1275(19) Uani 1 1 d . . . H24A H 0.2147 0.9310 -0.2435 0.153 Uiso 1 1 calc R . . C10 C 0.0392(5) 1.2573(11) 0.7293(6) 0.124(3) Uani 1 1 d . . . H10A H 0.0734 1.2347 0.7064 0.149 Uiso 1 1 calc R . . C31 C 0.0239(5) 0.162(2) 0.2460(8) 0.153(5) Uani 1 1 d . . . H31A H -0.0083 0.1130 0.2332 0.184 Uiso 1 1 calc R . . C12 C 0.0206(3) 1.1082(8) 0.6085(4) 0.089(2) Uani 1 1 d . . . H12A H 0.0533 1.0852 0.6376 0.106 Uiso 1 1 calc R . . H12B H 0.0335 1.1740 0.5776 0.106 Uiso 1 1 calc R . . C14 C 0.1735(4) 0.8935(8) 0.2052(4) 0.086(2) Uani 1 1 d . . . H14A H 0.1966 0.9368 0.2364 0.104 Uiso 1 1 calc R . . C20 C 0.1879(4) 1.1758(11) -0.1748(5) 0.111(3) Uani 1 1 d . . . H20A H 0.1997 1.2602 -0.1742 0.133 Uiso 1 1 calc R . . C32 C 0.0650(7) 0.1245(10) 0.2953(8) 0.158(5) Uani 1 1 d . . . H32A H 0.0587 0.0493 0.3187 0.189 Uiso 1 1 calc R . . C35 C 0.3604(8) 0.901(2) 0.3940(7) 0.253(13) Uani 1 1 d . . . H35A H 0.3718 0.9826 0.3767 0.380 Uiso 1 1 calc R . . H35B H 0.3947 0.8494 0.3998 0.380 Uiso 1 1 calc R . . H35C H 0.3410 0.9120 0.4368 0.380 Uiso 1 1 calc R . . C33 C 0.1137(6) 0.1948(9) 0.3100(5) 0.121(3) Uani 1 1 d . . . H33A H 0.1412 0.1650 0.3411 0.145 Uiso 1 1 calc R . . C27 C 0.1758(4) 0.3950(9) 0.2974(6) 0.104(3) Uani 1 1 d . . . O8 O 0.3002(4) 0.8924(10) 0.2872(6) 0.164(4) Uani 1 1 d . . . C11 C 0.0411(8) 1.3241(10) 0.7890(7) 0.148(5) Uani 1 1 d . . . H11A H 0.0781 1.3427 0.8065 0.178 Uiso 1 1 calc R . . C30 C 0.0361(7) 0.2757(15) 0.2194(7) 0.153(5) Uani 1 1 d . . . H30A H 0.0102 0.3043 0.1864 0.184 Uiso 1 1 calc R . . C7 C -0.0548(8) 1.3165(13) 0.8019(5) 0.171(7) Uani 1 1 d . . . H7A H -0.0859 1.3205 0.8323 0.205 Uiso 1 1 calc R . . C34 C 0.3102(4) 0.8252(15) 0.3347(7) 0.115(3) Uani 1 1 d . . . C8 C -0.0677(7) 1.2627(13) 0.7428(7) 0.152(5) Uani 1 1 d . . . H8A H -0.1062 1.2508 0.7279 0.182 Uiso 1 1 calc R . . C21 C 0.1429(4) 1.1442(8) -0.1340(5) 0.099(2) Uani 1 1 d . . . H21A H 0.1250 1.2062 -0.1076 0.118 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 0.0820(5) 0.1071(7) 0.0919(6) -0.0068(6) 0.0032(5) 0.0036(5) N1 0.076(4) 0.112(5) 0.118(6) -0.024(4) -0.001(4) 0.018(4) N2 0.275(14) 0.056(5) 0.123(7) -0.016(4) 0.002(9) 0.028(7) N3 0.088(4) 0.084(5) 0.086(4) 0.009(3) 0.019(3) 0.002(3) N4 0.122(4) 0.118(4) 0.143(4) -0.022(4) 0.045(4) -0.032(3) O5 0.108(4) 0.107(5) 0.153(6) -0.012(4) 0.019(4) -0.009(4) O6 0.135(5) 0.160(7) 0.153(6) 0.040(6) -0.052(5) -0.013(5) O1 0.083(3) 0.119(5) 0.096(3) -0.007(3) 0.000(3) 0.001(3) O2 0.099(4) 0.207(8) 0.108(4) -0.036(5) 0.001(3) -0.025(5) O3 0.083(3) 0.077(3) 0.192(6) 0.038(4) -0.057(4) -0.008(3) O4 0.121(4) 0.105(4) 0.095(3) -0.011(3) 0.035(3) -0.028(4) C1 0.083(6) 0.259(17) 0.142(9) -0.100(11) -0.002(6) 0.040(8) C2 0.108(7) 0.31(2) 0.108(7) -0.126(11) -0.030(5) 0.045(10) C3 0.053(4) 0.121(7) 0.106(5) -0.037(5) 0.008(3) 0.013(4) C4 0.068(5) 0.129(8) 0.140(8) 0.030(7) -0.005(5) -0.012(5) C5 0.069(5) 0.114(7) 0.099(5) -0.008(5) 0.000(4) 0.000(4) C6 0.073(5) 0.144(8) 0.120(6) 0.007(7) -0.030(5) 0.044(5) C26 0.108(8) 0.127(10) 0.046(5) 0.000 0.000 0.019(7) C19 0.105(5) 0.103(6) 0.072(4) -0.006(4) -0.015(4) -0.003(5) C15 0.105(6) 0.086(6) 0.122(7) -0.007(5) 0.013(6) 0.012(5) C13 0.086(7) 0.129(10) 0.054(5) 0.000 0.000 -0.002(7) C22 0.075(4) 0.113(7) 0.080(4) -0.016(4) 0.016(4) -0.006(4) C25 0.083(4) 0.102(6) 0.094(5) 0.007(4) 0.019(4) 0.010(4) C16 0.085(5) 0.079(5) 0.075(4) -0.006(4) -0.005(4) -0.014(4) C17 0.085(5) 0.085(6) 0.093(5) 0.004(4) 0.007(4) 0.003(4) C9 0.132(8) 0.103(7) 0.145(9) 0.009(7) 0.040(7) -0.027(6) C28 0.106(6) 0.114(8) 0.130(7) -0.012(7) 0.030(6) 0.005(5) C29 0.104(6) 0.115(7) 0.116(7) 0.011(6) -0.011(5) -0.005(6) C18 0.090(5) 0.084(5) 0.086(5) 0.008(4) -0.010(4) 0.003(4) C23 0.122(4) 0.118(4) 0.143(4) -0.022(4) 0.045(4) -0.032(3) O7 0.104(5) 0.172(8) 0.149(6) -0.033(5) 0.018(4) -0.009(5) C24 0.122(4) 0.118(4) 0.143(4) -0.022(4) 0.045(4) -0.032(3) C10 0.108(7) 0.146(9) 0.118(7) -0.018(7) -0.001(6) -0.015(6) C31 0.109(7) 0.212(16) 0.138(9) -0.036(11) -0.022(7) -0.016(10) C12 0.084(5) 0.105(6) 0.077(4) -0.010(4) 0.008(4) -0.013(4) C14 0.105(5) 0.089(6) 0.065(4) 0.001(4) -0.011(4) 0.023(4) C20 0.103(6) 0.112(7) 0.117(6) 0.000(6) 0.015(5) -0.003(6) C32 0.211(14) 0.085(7) 0.177(12) 0.011(7) 0.033(11) -0.067(8) C35 0.261(19) 0.39(3) 0.111(8) -0.056(12) -0.052(10) 0.24(2) C33 0.180(10) 0.071(6) 0.110(6) -0.011(5) 0.031(7) 0.002(6) C27 0.092(6) 0.072(5) 0.148(9) 0.011(6) 0.031(6) -0.016(4) O8 0.185(8) 0.153(7) 0.155(7) -0.036(6) -0.072(7) 0.018(6) C11 0.219(14) 0.070(6) 0.155(10) -0.018(7) -0.081(10) -0.004(7) C30 0.204(14) 0.138(10) 0.117(8) -0.007(8) 0.020(9) -0.040(10) C7 0.278(17) 0.142(11) 0.094(7) -0.044(7) 0.048(8) -0.121(13) C34 0.067(5) 0.141(10) 0.135(8) -0.019(8) -0.001(5) -0.016(6) C8 0.184(11) 0.140(10) 0.132(9) -0.019(7) 0.076(9) -0.010(9) C21 0.104(5) 0.063(5) 0.128(7) -0.011(5) 0.016(5) -0.008(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O7 1.970(9) . ? Cu1 N4 1.977(8) 3_545 ? Cu1 O5 2.009(7) . ? Cu1 N1 2.025(7) . ? Cu1 N3 2.209(7) . ? N1 C1 1.247(13) . ? N1 C5 1.312(10) . ? N2 C7 1.303(18) . ? N2 C11 1.336(19) . ? N3 C18 1.267(10) . ? N3 C14 1.405(10) . ? N4 C24 1.246(13) . ? N4 C20 1.323(12) . ? N4 Cu1 1.977(8) 3 ? O5 C27 1.313(12) . ? O6 C27 1.149(12) . ? O1 C3 1.360(9) . ? O1 C6 1.409(12) . ? O2 C9 1.381(14) . ? O2 C12 1.409(10) . ? O3 C16 1.363(10) . ? O3 C19 1.462(10) . ? O4 C22 1.328(9) . ? O4 C25 1.452(10) . ? C1 C2 1.451(14) . ? C1 H1A 0.9300 . ? C2 C3 1.328(13) . ? C2 H2A 0.9300 . ? C3 C4 1.449(14) . ? C4 C5 1.323(13) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 C13 1.616(11) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C26 C19 1.540(10) . ? C26 C19 1.540(10) 2_575 ? C26 C25 1.560(9) 2_575 ? C26 C25 1.560(9) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C15 C14 1.311(12) . ? C15 C16 1.376(12) . ? C15 H15A 0.9300 . ? C13 C12 1.432(9) . ? C13 C12 1.432(9) 2_575 ? C13 C6 1.616(11) 2_575 ? C22 C21 1.322(12) . ? C22 C23 1.339(13) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C16 C17 1.398(11) . ? C17 C18 1.335(11) . ? C17 H17A 0.9300 . ? C9 C10 1.417(15) . ? C9 C8 1.437(16) . ? C28 C29 1.363(14) . ? C28 C33 1.407(15) . ? C28 C27 1.542(15) . ? C29 C30 1.315(16) . ? C29 H29A 0.9300 . ? C18 H18A 0.9300 . ? C23 C24 1.454(14) . ? C23 H23A 0.9300 . ? O7 C34 1.255(14) . ? C24 H24A 0.9300 . ? C10 C11 1.375(17) . ? C10 H10A 0.9300 . ? C31 C30 1.34(2) . ? C31 C32 1.406(19) . ? C31 H31A 0.9300 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C14 H14A 0.9300 . ? C20 C21 1.344(13) . ? C20 H20A 0.9300 . ? C32 C33 1.364(17) . ? C32 H32A 0.9300 . ? C35 C34 1.82(2) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C33 H33A 0.9300 . ? O8 C34 1.198(15) . ? C11 H11A 0.9300 . ? C30 H30A 0.9300 . ? C7 C8 1.331(17) . ? C7 H7A 0.9300 . ? C8 H8A 0.9300 . ? C21 H21A 0.9300 . ? 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 O7 Cu1 N4 89.1(4) . 3_545 ? O7 Cu1 O5 140.8(4) . . ? N4 Cu1 O5 90.2(4) 3_545 . ? O7 Cu1 N1 90.1(3) . . ? N4 Cu1 N1 179.2(4) 3_545 . ? O5 Cu1 N1 90.5(3) . . ? O7 Cu1 N3 128.9(4) . . ? N4 Cu1 N3 91.0(3) 3_545 . ? O5 Cu1 N3 90.3(3) . . ? N1 Cu1 N3 89.5(3) . . ? C1 N1 C5 116.8(8) . . ? C1 N1 Cu1 120.9(7) . . ? C5 N1 Cu1 121.9(6) . . ? C7 N2 C11 112.4(10) . . ? C18 N3 C14 118.1(8) . . ? C18 N3 Cu1 123.8(6) . . ? C14 N3 Cu1 117.8(6) . . ? C24 N4 C20 112.0(9) . . ? C24 N4 Cu1 123.6(8) . 3 ? C20 N4 Cu1 123.9(7) . 3 ? C27 O5 Cu1 126.6(7) . . ? C3 O1 C6 112.4(6) . . ? C9 O2 C12 119.4(7) . . ? C16 O3 C19 117.2(6) . . ? C22 O4 C25 116.5(7) . . ? N1 C1 C2 127.0(11) . . ? N1 C1 H1A 116.5 . . ? C2 C1 H1A 116.5 . . ? C3 C2 C1 115.4(9) . . ? C3 C2 H2A 122.3 . . ? C1 C2 H2A 122.3 . . ? C2 C3 O1 126.9(8) . . ? C2 C3 C4 116.9(7) . . ? O1 C3 C4 116.1(7) . . ? C5 C4 C3 120.0(7) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? N1 C5 C4 123.6(9) . . ? N1 C5 H5A 118.2 . . ? C4 C5 H5A 118.2 . . ? O1 C6 C13 109.7(7) . . ? O1 C6 H6A 109.7 . . ? C13 C6 H6A 109.7 . . ? O1 C6 H6B 109.7 . . ? C13 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? C19 C26 C19 117.4(9) . 2_575 ? C19 C26 C25 103.0(4) . 2_575 ? C19 C26 C25 110.6(5) 2_575 2_575 ? C19 C26 C25 110.6(5) . . ? C19 C26 C25 103.0(4) 2_575 . ? C25 C26 C25 112.4(9) 2_575 . ? O3 C19 C26 103.6(6) . . ? O3 C19 H19A 111.0 . . ? C26 C19 H19A 111.0 . . ? O3 C19 H19B 111.0 . . ? C26 C19 H19B 111.0 . . ? H19A C19 H19B 109.0 . . ? C14 C15 C16 122.8(9) . . ? C14 C15 H15A 118.6 . . ? C16 C15 H15A 118.6 . . ? C12 C13 C12 119.1(9) . 2_575 ? C12 C13 C6 104.6(5) . . ? C12 C13 C6 110.9(5) 2_575 . ? C12 C13 C6 110.9(5) . 2_575 ? C12 C13 C6 104.6(5) 2_575 2_575 ? C6 C13 C6 106.2(8) . 2_575 ? C21 C22 O4 127.3(8) . . ? C21 C22 C23 116.8(8) . . ? O4 C22 C23 115.7(8) . . ? O4 C25 C26 107.3(6) . . ? O4 C25 H25A 110.3 . . ? C26 C25 H25A 110.3 . . ? O4 C25 H25B 110.3 . . ? C26 C25 H25B 110.3 . . ? H25A C25 H25B 108.5 . . ? O3 C16 C15 119.9(7) . . ? O3 C16 C17 122.7(8) . . ? C15 C16 C17 117.3(8) . . ? C18 C17 C16 116.4(9) . . ? C18 C17 H17A 121.8 . . ? C16 C17 H17A 121.8 . . ? O2 C9 C10 125.1(10) . . ? O2 C9 C8 117.0(11) . . ? C10 C9 C8 117.7(12) . . ? C29 C28 C33 117.3(11) . . ? C29 C28 C27 122.7(10) . . ? C33 C28 C27 119.8(11) . . ? C30 C29 C28 119.1(12) . . ? C30 C29 H29A 120.4 . . ? C28 C29 H29A 120.4 . . ? N3 C18 C17 126.8(8) . . ? N3 C18 H18A 116.6 . . ? C17 C18 H18A 116.6 . . ? C22 C23 C24 116.7(10) . . ? C22 C23 H23A 121.6 . . ? C24 C23 H23A 121.6 . . ? C34 O7 Cu1 123.2(9) . . ? N4 C24 C23 126.8(10) . . ? N4 C24 H24A 116.6 . . ? C23 C24 H24A 116.6 . . ? C11 C10 C9 117.1(12) . . ? C11 C10 H10A 121.4 . . ? C9 C10 H10A 121.4 . . ? C30 C31 C32 112.7(13) . . ? C30 C31 H31A 123.7 . . ? C32 C31 H31A 123.7 . . ? O2 C12 C13 106.2(6) . . ? O2 C12 H12A 110.5 . . ? C13 C12 H12A 110.5 . . ? O2 C12 H12B 110.5 . . ? C13 C12 H12B 110.5 . . ? H12A C12 H12B 108.7 . . ? C15 C14 N3 118.4(8) . . ? C15 C14 H14A 120.8 . . ? N3 C14 H14A 120.8 . . ? N4 C20 C21 126.7(10) . . ? N4 C20 H20A 116.6 . . ? C21 C20 H20A 116.6 . . ? C33 C32 C31 122.3(12) . . ? C33 C32 H32A 118.9 . . ? C31 C32 H32A 118.9 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C32 C33 C28 119.9(12) . . ? C32 C33 H33A 120.1 . . ? C28 C33 H33A 120.1 . . ? O6 C27 O5 128.0(9) . . ? O6 C27 C28 121.7(10) . . ? O5 C27 C28 109.9(11) . . ? N2 C11 C10 125.7(13) . . ? N2 C11 H11A 117.1 . . ? C10 C11 H11A 117.1 . . ? C29 C30 C31 128.4(15) . . ? C29 C30 H30A 115.8 . . ? C31 C30 H30A 115.8 . . ? N2 C7 C8 130.6(13) . . ? N2 C7 H7A 114.7 . . ? C8 C7 H7A 114.7 . . ? O8 C34 O7 121.8(11) . . ? O8 C34 C35 111.3(13) . . ? O7 C34 C35 126.9(13) . . ? C7 C8 C9 114.3(15) . . ? C7 C8 H8A 122.9 . . ? C9 C8 H8A 122.9 . . ? C22 C21 C20 120.7(9) . . ? C22 C21 H21A 119.6 . . ? C20 C21 H21A 119.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 Cu1 N1 C1 14.8(11) . . . . ? N4 Cu1 N1 C1 14(26) 3_545 . . . ? O5 Cu1 N1 C1 155.6(11) . . . . ? N3 Cu1 N1 C1 -114.1(11) . . . . ? O7 Cu1 N1 C5 -173.4(8) . . . . ? N4 Cu1 N1 C5 -175(100) 3_545 . . . ? O5 Cu1 N1 C5 -32.6(8) . . . . ? N3 Cu1 N1 C5 57.7(7) . . . . ? O7 Cu1 N3 C18 162.7(6) . . . . ? N4 Cu1 N3 C18 73.1(7) 3_545 . . . ? O5 Cu1 N3 C18 -17.1(7) . . . . ? N1 Cu1 N3 C18 -107.6(7) . . . . ? O7 Cu1 N3 C14 -24.1(7) . . . . ? N4 Cu1 N3 C14 -113.8(6) 3_545 . . . ? O5 Cu1 N3 C14 156.1(6) . . . . ? N1 Cu1 N3 C14 65.6(6) . . . . ? O7 Cu1 O5 C27 5.4(10) . . . . ? N4 Cu1 O5 C27 94.1(7) 3_545 . . . ? N1 Cu1 O5 C27 -85.4(7) . . . . ? N3 Cu1 O5 C27 -174.9(7) . . . . ? C5 N1 C1 C2 5(2) . . . . ? Cu1 N1 C1 C2 177.2(14) . . . . ? N1 C1 C2 C3 -5(3) . . . . ? C1 C2 C3 O1 -178.8(12) . . . . ? C1 C2 C3 C4 4(2) . . . . ? C6 O1 C3 C2 12.7(17) . . . . ? C6 O1 C3 C4 -170.3(8) . . . . ? C2 C3 C4 C5 -3.8(17) . . . . ? O1 C3 C4 C5 178.9(8) . . . . ? C1 N1 C5 C4 -4.1(16) . . . . ? Cu1 N1 C5 C4 -176.2(8) . . . . ? C3 C4 C5 N1 3.6(15) . . . . ? C3 O1 C6 C13 -175.7(7) . . . . ? C16 O3 C19 C26 -178.8(7) . . . . ? C19 C26 C19 O3 -53.0(5) 2_575 . . . ? C25 C26 C19 O3 -174.9(6) 2_575 . . . ? C25 C26 C19 O3 64.8(8) . . . . ? O1 C6 C13 C12 -173.5(7) . . . . ? O1 C6 C13 C12 56.9(8) . . . 2_575 ? O1 C6 C13 C6 -56.2(5) . . . 2_575 ? C25 O4 C22 C21 -2.7(13) . . . . ? C25 O4 C22 C23 -177.9(9) . . . . ? C22 O4 C25 C26 -170.6(7) . . . . ? C19 C26 C25 O4 53.4(8) . . . . ? C19 C26 C25 O4 179.7(6) 2_575 . . . ? C25 C26 C25 O4 -61.2(5) 2_575 . . . ? C19 O3 C16 C15 -175.2(8) . . . . ? C19 O3 C16 C17 8.4(12) . . . . ? C14 C15 C16 O3 -179.1(8) . . . . ? C14 C15 C16 C17 -2.4(13) . . . . ? O3 C16 C17 C18 -179.1(7) . . . . ? C15 C16 C17 C18 4.3(12) . . . . ? C12 O2 C9 C10 -3.4(16) . . . . ? C12 O2 C9 C8 -178.5(10) . . . . ? C33 C28 C29 C30 -5.4(15) . . . . ? C27 C28 C29 C30 179.4(10) . . . . ? C14 N3 C18 C17 -0.9(13) . . . . ? Cu1 N3 C18 C17 172.2(6) . . . . ? C16 C17 C18 N3 -2.8(13) . . . . ? C21 C22 C23 C24 -3.5(15) . . . . ? O4 C22 C23 C24 172.2(10) . . . . ? N4 Cu1 O7 C34 85.9(8) 3_545 . . . ? O5 Cu1 O7 C34 175.0(7) . . . . ? N1 Cu1 O7 C34 -94.1(8) . . . . ? N3 Cu1 O7 C34 -4.7(9) . . . . ? C20 N4 C24 C23 -4.3(19) . . . . ? Cu1 N4 C24 C23 -176.3(10) 3 . . . ? C22 C23 C24 N4 6(2) . . . . ? O2 C9 C10 C11 -175.5(10) . . . . ? C8 C9 C10 C11 -0.4(16) . . . . ? C9 O2 C12 C13 158.4(9) . . . . ? C12 C13 C12 O2 -60.7(5) 2_575 . . . ? C6 C13 C12 O2 174.8(7) . . . . ? C6 C13 C12 O2 60.8(9) 2_575 . . . ? C16 C15 C14 N3 -1.3(14) . . . . ? C18 N3 C14 C15 3.0(12) . . . . ? Cu1 N3 C14 C15 -170.5(6) . . . . ? C24 N4 C20 C21 0.9(17) . . . . ? Cu1 N4 C20 C21 172.9(8) 3 . . . ? C30 C31 C32 C33 -4(2) . . . . ? C31 C32 C33 C28 3.5(18) . . . . ? C29 C28 C33 C32 1.4(15) . . . . ? C27 C28 C33 C32 176.7(10) . . . . ? Cu1 O5 C27 O6 -20.7(16) . . . . ? Cu1 O5 C27 C28 166.6(6) . . . . ? C29 C28 C27 O6 -176.3(11) . . . . ? C33 C28 C27 O6 8.7(15) . . . . ? C29 C28 C27 O5 -3.1(13) . . . . ? C33 C28 C27 O5 -178.1(8) . . . . ? C7 N2 C11 C10 10.6(17) . . . . ? C9 C10 C11 N2 -2.5(18) . . . . ? C28 C29 C30 C31 5(2) . . . . ? C32 C31 C30 C29 0(2) . . . . ? C11 N2 C7 C8 -19(2) . . . . ? Cu1 O7 C34 O8 -9.7(15) . . . . ? Cu1 O7 C34 C35 169.0(7) . . . . ? N2 C7 C8 C9 17(2) . . . . ? O2 C9 C8 C7 170.2(11) . . . . ? C10 C9 C8 C7 -5.3(17) . . . . ? O4 C22 C21 C20 -174.5(9) . . . . ? C23 C22 C21 C20 0.6(14) . . . . ? N4 C20 C21 C22 1.0(16) . . . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 1.542 _refine_diff_density_min -0.277 _refine_diff_density_rms 0.069 # SQUEEZE RESULTS (APPEND TO CIF) 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 1 0.209 -0.050 0.009 2025.4 1.8 _platon_squeeze_details ; ; #================================================================= data_compound2 _database_code_depnum_ccdc_archive 'CCDC 822456' #TrackingRef '- p.cif' _symmetry_space_group_name_hall '-P 2yc' #Added by publCIF _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H60 Cu4 N4 O24' _chemical_formula_weight 1307.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 10.0124(6) _cell_length_b 14.1908(9) _cell_length_c 21.6482(16) _cell_angle_alpha 90.00 _cell_angle_beta 102.265(2) _cell_angle_gamma 90.00 _cell_volume 3005.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 1.474 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7570 _exptl_absorpt_correction_T_max 0.8666 _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID imaging plate' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27113 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5861 _reflns_number_gt 4465 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PROCESS-AUTO (Rigaku Corporation,1998)' _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan (Molecular Structure Corporation & Rigaku Corporation, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0687P)^2^+1.3363P] 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 5861 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0660 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1346 _refine_ls_wR_factor_gt 0.1254 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _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 -0.06252(5) 0.33362(3) 0.05985(2) 0.04342(16) Uani 1 1 d . . . Cu2 Cu 0.12532(4) 0.50551(3) 0.05193(2) 0.03929(15) Uani 1 1 d . . . O3 O 0.0123(2) 0.41120(16) 0.00035(11) 0.0357(5) Uani 1 1 d . . . H3A H 0.0634 0.3740 -0.0250 0.043 Uiso 1 1 calc R . . O2 O 0.6416(2) 1.09781(17) 0.22533(11) 0.0414(6) Uani 1 1 d . . . O1 O 0.4213(3) 0.85206(18) 0.17632(13) 0.0483(7) Uani 1 1 d . . . O7 O 0.2650(3) 0.42033(19) 0.09353(13) 0.0503(7) Uani 1 1 d . . . C1 C 0.1714(4) 0.6632(3) 0.1429(2) 0.0512(10) Uani 1 1 d . . . H1A H 0.0916 0.6426 0.1542 0.061 Uiso 1 1 calc R . . O4 O -0.0796(3) 0.22412(18) 0.00352(14) 0.0532(7) Uani 1 1 d . . . C9 C 0.6973(4) 1.1510(2) 0.18527(17) 0.0374(8) Uani 1 1 d . . . N1 N 0.2204(3) 0.6128(2) 0.10113(15) 0.0446(7) Uani 1 1 d . . . O8 O -0.0731(3) 0.4528(2) 0.11050(15) 0.0633(8) Uani 1 1 d . . . N2 N 0.8312(3) 1.2618(2) 0.11207(15) 0.0450(7) Uani 1 1 d . . . C12 C 0.5352(3) 1.0335(2) 0.19729(16) 0.0337(7) Uani 1 1 d . . . H12A H 0.5660 0.9937 0.1667 0.040 Uiso 1 1 calc R . . H12B H 0.4552 1.0681 0.1758 0.040 Uiso 1 1 calc R . . C13 C 0.5000 0.9735(3) 0.2500 0.0287(9) Uani 1 2 d S . . C8 C 0.6607(4) 1.1477(3) 0.12044(17) 0.0432(9) Uani 1 1 d . . . H8A H 0.5898 1.1089 0.1003 0.052 Uiso 1 1 calc R . . C6 C 0.3775(3) 0.9109(2) 0.22170(17) 0.0369(8) Uani 1 1 d . . . H6A H 0.3508 0.8731 0.2544 0.044 Uiso 1 1 calc R . . H6B H 0.3001 0.9492 0.2016 0.044 Uiso 1 1 calc R . . O6 O 0.1383(3) 0.3071(2) 0.12414(15) 0.0601(8) Uani 1 1 d . . . C2 C 0.2316(4) 0.7439(3) 0.17052(19) 0.0468(9) Uani 1 1 d . . . H2A H 0.1931 0.7774 0.1993 0.056 Uiso 1 1 calc R . . C23 C 0.2489(4) 0.3440(3) 0.12265(19) 0.0475(9) Uani 1 1 d . . . O5 O 0.0927(3) 0.2519(2) -0.04410(17) 0.0662(9) Uani 1 1 d . . . C14 C -0.0040(4) 0.2010(3) -0.0334(2) 0.0493(9) Uani 1 1 d . . . C11 C 0.8630(4) 1.2666(3) 0.17508(18) 0.0482(9) Uani 1 1 d . . . H11A H 0.9311 1.3083 0.1940 0.058 Uiso 1 1 calc R . . C10 C 0.7999(4) 1.2129(3) 0.21329(18) 0.0436(9) Uani 1 1 d . . . H10A H 0.8253 1.2179 0.2571 0.052 Uiso 1 1 calc R . . C3 C 0.3501(4) 0.7743(2) 0.15463(18) 0.0408(8) Uani 1 1 d . . . O9 O -0.2575(4) 0.4742(3) 0.03829(18) 0.0807(10) Uani 1 1 d . . . C7 C 0.7304(4) 1.2025(3) 0.08609(18) 0.0503(10) Uani 1 1 d . . . H7A H 0.7067 1.1985 0.0422 0.060 Uiso 1 1 calc R . . C4 C 0.4056(4) 0.7207(3) 0.1124(2) 0.0594(12) Uani 1 1 d . . . H4A H 0.4867 0.7386 0.1012 0.071 Uiso 1 1 calc R . . C17 C -0.1616(7) -0.0367(4) -0.0809(3) 0.093(2) Uani 1 1 d . . . H17A H -0.2295 -0.0749 -0.0710 0.112 Uiso 1 1 calc R . . C15 C -0.0347(5) 0.1076(3) -0.0662(2) 0.0597(11) Uani 1 1 d . . . C5 C 0.3382(4) 0.6411(3) 0.0877(2) 0.0614(12) Uani 1 1 d . . . H5A H 0.3763 0.6048 0.0602 0.074 Uiso 1 1 calc R . . C21 C -0.1860(5) 0.4911(3) 0.0913(2) 0.0570(11) Uani 1 1 d . . . C16 C -0.1338(5) 0.0494(3) -0.0525(2) 0.0738(15) Uani 1 1 d . . . H16A H -0.1836 0.0689 -0.0230 0.089 Uiso 1 1 calc R . . C20 C 0.0384(6) 0.0805(4) -0.1104(3) 0.0858(17) Uani 1 1 d . . . H20A H 0.1052 0.1195 -0.1206 0.103 Uiso 1 1 calc R . . C24 C 0.3779(5) 0.2976(4) 0.1572(3) 0.0841(17) Uani 1 1 d . . . H24A H 0.3557 0.2411 0.1771 0.126 Uiso 1 1 calc R . . H24B H 0.4266 0.3399 0.1887 0.126 Uiso 1 1 calc R . . H24C H 0.4341 0.2823 0.1278 0.126 Uiso 1 1 calc R . . C18 C -0.0904(8) -0.0649(4) -0.1228(4) 0.102(2) Uani 1 1 d . . . H18A H -0.1077 -0.1241 -0.1410 0.123 Uiso 1 1 calc R . . C19 C 0.0092(8) -0.0087(5) -0.1402(4) 0.112(3) Uani 1 1 d . . . H19A H 0.0557 -0.0289 -0.1707 0.134 Uiso 1 1 calc R . . C22 C -0.2419(8) 0.5649(7) 0.1293(4) 0.148(4) Uani 1 1 d . . . H22A H -0.1796 0.5735 0.1692 0.222 Uiso 1 1 calc R . . H22B H -0.3290 0.5448 0.1363 0.222 Uiso 1 1 calc R . . H22C H -0.2526 0.6234 0.1065 0.222 Uiso 1 1 calc R . . O1W O 0.5128(4) 0.6218(4) -0.0263(3) 0.1183(16) Uani 1 1 d . . . H1WC H 0.6069 0.6216 -0.0030 0.142 Uiso 1 1 calc R . . H1WD H 0.4643 0.6774 -0.0170 0.142 Uiso 1 1 calc R . . O2W O 0.6262(5) 0.7949(5) 0.0116(3) 0.163(2) Uani 1 1 d . . . H2WC H 0.7203 0.7952 0.0349 0.195 Uiso 1 1 calc R . . H2WD H 0.5753 0.8495 0.0206 0.195 Uiso 1 1 calc R . . O3W O 0.4973(12) 0.9482(8) 0.0429(5) 0.273(5) Uani 1 1 d . . . H3WA H 0.5902 0.9573 0.0665 0.327 Uiso 1 1 calc R . . H3WB H 0.4344 0.9962 0.0511 0.327 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 0.0562(3) 0.0328(3) 0.0411(3) 0.00425(19) 0.0099(2) -0.01436(19) Cu2 0.0429(3) 0.0282(2) 0.0422(3) -0.00265(18) -0.00111(19) -0.01036(17) O3 0.0421(12) 0.0289(12) 0.0354(13) -0.0039(10) 0.0070(10) -0.0107(9) O2 0.0541(14) 0.0358(13) 0.0336(13) 0.0003(10) 0.0073(11) -0.0180(11) O1 0.0520(14) 0.0396(14) 0.0586(17) -0.0220(13) 0.0236(13) -0.0186(11) O7 0.0480(14) 0.0404(15) 0.0578(17) 0.0075(13) 0.0010(13) -0.0092(11) C1 0.048(2) 0.050(2) 0.057(3) -0.012(2) 0.0138(19) -0.0152(17) O4 0.0685(18) 0.0355(14) 0.0564(18) -0.0026(13) 0.0150(15) -0.0164(12) C9 0.0441(18) 0.0294(17) 0.039(2) 0.0036(15) 0.0099(16) -0.0038(14) N1 0.0435(16) 0.0361(17) 0.0514(19) -0.0075(14) 0.0034(15) -0.0102(13) O8 0.069(2) 0.065(2) 0.0543(19) 0.0103(15) 0.0110(16) -0.0065(16) N2 0.0468(17) 0.0455(18) 0.0403(18) 0.0039(14) 0.0041(14) -0.0147(14) C12 0.0404(17) 0.0244(16) 0.0352(19) -0.0006(14) 0.0059(15) -0.0043(13) C13 0.031(2) 0.023(2) 0.032(2) 0.000 0.0057(19) 0.000 C8 0.0455(19) 0.041(2) 0.040(2) 0.0044(16) 0.0008(16) -0.0165(15) C6 0.0398(17) 0.0280(17) 0.044(2) -0.0039(15) 0.0111(16) -0.0043(13) O6 0.0588(17) 0.0526(17) 0.065(2) 0.0195(15) 0.0049(15) -0.0116(14) C2 0.047(2) 0.042(2) 0.053(2) -0.0136(18) 0.0140(18) -0.0096(16) C23 0.055(2) 0.040(2) 0.047(2) 0.0013(17) 0.0085(18) -0.0009(17) O5 0.0653(18) 0.0480(17) 0.092(2) -0.0132(16) 0.0315(18) -0.0090(14) C14 0.058(2) 0.0296(19) 0.056(3) 0.0037(18) 0.002(2) -0.0006(17) C11 0.058(2) 0.042(2) 0.039(2) 0.0022(17) 0.0007(18) -0.0184(17) C10 0.053(2) 0.043(2) 0.0320(19) -0.0005(16) 0.0043(16) -0.0176(17) C3 0.0398(18) 0.0339(18) 0.047(2) -0.0095(16) 0.0056(16) -0.0090(14) O9 0.066(2) 0.111(3) 0.066(2) -0.024(2) 0.0177(19) -0.0148(19) C7 0.058(2) 0.057(2) 0.034(2) 0.0067(18) 0.0045(18) -0.0143(19) C4 0.050(2) 0.063(3) 0.072(3) -0.032(2) 0.028(2) -0.023(2) C17 0.118(5) 0.041(3) 0.094(5) -0.002(3) -0.038(4) -0.006(3) C15 0.070(3) 0.038(2) 0.060(3) -0.003(2) -0.011(2) 0.0096(19) C5 0.049(2) 0.060(3) 0.078(3) -0.030(2) 0.019(2) -0.0167(19) C21 0.055(2) 0.069(3) 0.052(3) -0.001(2) 0.023(2) -0.011(2) C16 0.097(4) 0.033(2) 0.073(3) 0.005(2) -0.021(3) -0.016(2) C20 0.085(4) 0.068(3) 0.096(4) -0.024(3) 0.000(3) 0.021(3) C24 0.068(3) 0.078(4) 0.101(4) 0.038(3) 0.006(3) 0.014(3) C18 0.113(5) 0.054(3) 0.110(6) -0.018(4) -0.044(4) 0.017(4) C19 0.118(5) 0.096(5) 0.105(5) -0.045(4) -0.010(4) 0.052(4) C22 0.108(5) 0.218(10) 0.123(6) -0.087(7) 0.037(5) 0.009(6) O1W 0.079(3) 0.116(4) 0.171(5) 0.002(3) 0.052(3) 0.002(2) O2W 0.082(3) 0.188(6) 0.221(7) -0.029(5) 0.038(4) -0.012(3) O3W 0.316(12) 0.280(12) 0.242(10) -0.115(9) 0.103(10) -0.072(10) _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 O4 1.960(3) . ? Cu1 O3 1.961(2) . ? Cu1 N2 1.990(3) 1_445 ? Cu1 O8 2.030(3) . ? Cu1 O6 2.221(3) . ? Cu2 O7 1.922(3) . ? Cu2 O3 1.944(2) . ? Cu2 O3 1.979(2) 3_565 ? Cu2 N1 1.982(3) . ? Cu2 Cu2 2.9967(9) 3_565 ? O3 Cu2 1.979(2) 3_565 ? O3 H3A 0.9800 . ? O2 C9 1.356(4) . ? O2 C12 1.435(4) . ? O1 C3 1.343(4) . ? O1 C6 1.428(4) . ? O7 C23 1.280(5) . ? C1 N1 1.327(5) . ? C1 C2 1.371(5) . ? C1 H1A 0.9300 . ? O4 C14 1.256(5) . ? C9 C8 1.374(5) . ? C9 C10 1.389(5) . ? N1 C5 1.335(5) . ? O8 C21 1.244(5) . ? N2 C11 1.335(5) . ? N2 C7 1.342(5) . ? N2 Cu1 1.990(3) 1_665 ? C12 C13 1.524(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C12 1.524(4) 2_655 ? C13 C6 1.533(4) . ? C13 C6 1.533(4) 2_655 ? C8 C7 1.366(5) . ? C8 H8A 0.9300 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? O6 C23 1.232(5) . ? C2 C3 1.373(5) . ? C2 H2A 0.9300 . ? C23 C24 1.500(6) . ? O5 C14 1.267(5) . ? C14 C15 1.505(6) . ? C11 C10 1.373(5) . ? C11 H11A 0.9300 . ? C10 H10A 0.9300 . ? C3 C4 1.393(5) . ? O9 C21 1.240(6) . ? C7 H7A 0.9300 . ? C4 C5 1.364(5) . ? C4 H4A 0.9300 . ? C17 C18 1.329(10) . ? C17 C16 1.369(7) . ? C17 H17A 0.9300 . ? C15 C16 1.372(7) . ? C15 C20 1.378(7) . ? C5 H5A 0.9300 . ? C21 C22 1.511(8) . ? C16 H16A 0.9300 . ? C20 C19 1.421(8) . ? C20 H20A 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C18 C19 1.390(10) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? O1W H1WC 0.9700 . ? O1W H1WD 0.9700 . ? O2W H2WC 0.9700 . ? O2W H2WD 0.9700 . ? O3W H3WA 0.9700 . ? O3W H3WB 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 O4 Cu1 O3 91.81(10) . . ? O4 Cu1 N2 87.75(12) . 1_445 ? O3 Cu1 N2 170.44(12) . 1_445 ? O4 Cu1 O8 171.31(13) . . ? O3 Cu1 O8 87.60(10) . . ? N2 Cu1 O8 91.40(12) 1_445 . ? O4 Cu1 O6 101.73(12) . . ? O3 Cu1 O6 94.90(10) . . ? N2 Cu1 O6 94.54(12) 1_445 . ? O8 Cu1 O6 86.96(13) . . ? O7 Cu2 O3 96.48(11) . . ? O7 Cu2 O3 173.22(11) . 3_565 ? O3 Cu2 O3 80.39(10) . 3_565 ? O7 Cu2 N1 90.72(12) . . ? O3 Cu2 N1 172.65(12) . . ? O3 Cu2 N1 92.60(11) 3_565 . ? O7 Cu2 Cu2 136.79(8) . 3_565 ? O3 Cu2 Cu2 40.62(7) . 3_565 ? O3 Cu2 Cu2 39.77(6) 3_565 3_565 ? N1 Cu2 Cu2 132.34(10) . 3_565 ? Cu2 O3 Cu1 105.43(11) . . ? Cu2 O3 Cu2 99.61(10) . 3_565 ? Cu1 O3 Cu2 113.21(11) . 3_565 ? Cu2 O3 H3A 112.6 . . ? Cu1 O3 H3A 112.6 . . ? Cu2 O3 H3A 112.6 3_565 . ? C9 O2 C12 116.9(3) . . ? C3 O1 C6 120.3(3) . . ? C23 O7 Cu2 127.4(2) . . ? N1 C1 C2 123.7(3) . . ? N1 C1 H1A 118.1 . . ? C2 C1 H1A 118.1 . . ? C14 O4 Cu1 128.2(2) . . ? O2 C9 C8 125.3(3) . . ? O2 C9 C10 116.1(3) . . ? C8 C9 C10 118.7(3) . . ? C1 N1 C5 117.2(3) . . ? C1 N1 Cu2 125.1(2) . . ? C5 N1 Cu2 117.4(3) . . ? C21 O8 Cu1 109.4(3) . . ? C11 N2 C7 117.1(3) . . ? C11 N2 Cu1 120.9(2) . 1_665 ? C7 N2 Cu1 121.9(3) . 1_665 ? O2 C12 C13 107.9(2) . . ? O2 C12 H12A 110.1 . . ? C13 C12 H12A 110.1 . . ? O2 C12 H12B 110.1 . . ? C13 C12 H12B 110.1 . . ? H12A C12 H12B 108.4 . . ? C12 C13 C12 112.1(4) . 2_655 ? C12 C13 C6 108.49(18) . . ? C12 C13 C6 109.29(18) 2_655 . ? C12 C13 C6 109.29(18) . 2_655 ? C12 C13 C6 108.49(18) 2_655 2_655 ? C6 C13 C6 109.2(4) . 2_655 ? C7 C8 C9 118.7(3) . . ? C7 C8 H8A 120.7 . . ? C9 C8 H8A 120.7 . . ? O1 C6 C13 106.1(2) . . ? O1 C6 H6A 110.5 . . ? C13 C6 H6A 110.5 . . ? O1 C6 H6B 110.5 . . ? C13 C6 H6B 110.5 . . ? H6A C6 H6B 108.7 . . ? C23 O6 Cu1 127.6(3) . . ? C1 C2 C3 118.5(3) . . ? C1 C2 H2A 120.8 . . ? C3 C2 H2A 120.8 . . ? O6 C23 O7 125.5(4) . . ? O6 C23 C24 119.0(4) . . ? O7 C23 C24 115.6(4) . . ? O4 C14 O5 123.7(4) . . ? O4 C14 C15 116.1(4) . . ? O5 C14 C15 120.2(4) . . ? N2 C11 C10 123.2(3) . . ? N2 C11 H11A 118.4 . . ? C10 C11 H11A 118.4 . . ? C11 C10 C9 118.7(3) . . ? C11 C10 H10A 120.7 . . ? C9 C10 H10A 120.7 . . ? O1 C3 C2 126.3(3) . . ? O1 C3 C4 115.0(3) . . ? C2 C3 C4 118.7(3) . . ? N2 C7 C8 123.7(4) . . ? N2 C7 H7A 118.2 . . ? C8 C7 H7A 118.2 . . ? C5 C4 C3 118.4(3) . . ? C5 C4 H4A 120.8 . . ? C3 C4 H4A 120.8 . . ? C18 C17 C16 119.2(7) . . ? C18 C17 H17A 120.4 . . ? C16 C17 H17A 120.4 . . ? C16 C15 C20 119.9(5) . . ? C16 C15 C14 120.9(4) . . ? C20 C15 C14 119.3(4) . . ? N1 C5 C4 123.5(4) . . ? N1 C5 H5A 118.3 . . ? C4 C5 H5A 118.3 . . ? O9 C21 O8 122.0(4) . . ? O9 C21 C22 115.5(5) . . ? O8 C21 C22 122.5(5) . . ? C17 C16 C15 121.8(6) . . ? C17 C16 H16A 119.1 . . ? C15 C16 H16A 119.1 . . ? C15 C20 C19 118.4(6) . . ? C15 C20 H20A 120.8 . . ? C19 C20 H20A 120.8 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C17 C18 C19 122.2(6) . . ? C17 C18 H18A 118.9 . . ? C19 C18 H18A 118.9 . . ? C18 C19 C20 118.5(7) . . ? C18 C19 H19A 120.7 . . ? C20 C19 H19A 120.7 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? H1WC O1W H1WD 111.6 . . ? H2WC O2W H2WD 112.7 . . ? H3WA O3W H3WB 113.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 Cu2 O3 Cu1 68.60(12) . . . . ? O3 Cu2 O3 Cu1 -117.48(14) 3_565 . . . ? N1 Cu2 O3 Cu1 -99.9(9) . . . . ? Cu2 Cu2 O3 Cu1 -117.48(14) 3_565 . . . ? O7 Cu2 O3 Cu2 -173.92(11) . . . 3_565 ? O3 Cu2 O3 Cu2 0.0 3_565 . . 3_565 ? N1 Cu2 O3 Cu2 17.5(9) . . . 3_565 ? O4 Cu1 O3 Cu2 -152.92(13) . . . . ? N2 Cu1 O3 Cu2 119.9(7) 1_445 . . . ? O8 Cu1 O3 Cu2 35.76(13) . . . . ? O6 Cu1 O3 Cu2 -50.99(13) . . . . ? O4 Cu1 O3 Cu2 99.21(13) . . . 3_565 ? N2 Cu1 O3 Cu2 12.1(8) 1_445 . . 3_565 ? O8 Cu1 O3 Cu2 -72.11(13) . . . 3_565 ? O6 Cu1 O3 Cu2 -158.86(13) . . . 3_565 ? O3 Cu2 O7 C23 -51.9(3) . . . . ? O3 Cu2 O7 C23 -114.0(8) 3_565 . . . ? N1 Cu2 O7 C23 126.6(3) . . . . ? Cu2 Cu2 O7 C23 -57.7(4) 3_565 . . . ? O3 Cu1 O4 C14 33.2(3) . . . . ? N2 Cu1 O4 C14 -156.4(3) 1_445 . . . ? O8 Cu1 O4 C14 119.1(8) . . . . ? O6 Cu1 O4 C14 -62.2(3) . . . . ? C12 O2 C9 C8 -0.4(5) . . . . ? C12 O2 C9 C10 179.9(3) . . . . ? C2 C1 N1 C5 2.9(7) . . . . ? C2 C1 N1 Cu2 -171.7(3) . . . . ? O7 Cu2 N1 C1 -115.4(3) . . . . ? O3 Cu2 N1 C1 53.3(11) . . . . ? O3 Cu2 N1 C1 70.5(3) 3_565 . . . ? Cu2 Cu2 N1 C1 68.6(4) 3_565 . . . ? O7 Cu2 N1 C5 70.1(3) . . . . ? O3 Cu2 N1 C5 -121.3(9) . . . . ? O3 Cu2 N1 C5 -104.0(3) 3_565 . . . ? Cu2 Cu2 N1 C5 -105.9(3) 3_565 . . . ? O4 Cu1 O8 C21 3.5(9) . . . . ? O3 Cu1 O8 C21 89.8(3) . . . . ? N2 Cu1 O8 C21 -80.7(3) 1_445 . . . ? O6 Cu1 O8 C21 -175.2(3) . . . . ? C9 O2 C12 C13 173.3(3) . . . . ? O2 C12 C13 C12 54.00(18) . . . 2_655 ? O2 C12 C13 C6 174.8(2) . . . . ? O2 C12 C13 C6 -66.3(3) . . . 2_655 ? O2 C9 C8 C7 -177.0(4) . . . . ? C10 C9 C8 C7 2.7(6) . . . . ? C3 O1 C6 C13 163.6(3) . . . . ? C12 C13 C6 O1 61.8(3) . . . . ? C12 C13 C6 O1 -175.7(3) 2_655 . . . ? C6 C13 C6 O1 -57.2(2) 2_655 . . . ? O4 Cu1 O6 C23 101.7(4) . . . . ? O3 Cu1 O6 C23 8.8(4) . . . . ? N2 Cu1 O6 C23 -169.7(4) 1_445 . . . ? O8 Cu1 O6 C23 -78.5(4) . . . . ? N1 C1 C2 C3 -0.6(7) . . . . ? Cu1 O6 C23 O7 17.5(6) . . . . ? Cu1 O6 C23 C24 -162.3(4) . . . . ? Cu2 O7 C23 O6 7.1(6) . . . . ? Cu2 O7 C23 C24 -173.1(3) . . . . ? Cu1 O4 C14 O5 -6.5(6) . . . . ? Cu1 O4 C14 C15 174.2(3) . . . . ? C7 N2 C11 C10 1.5(6) . . . . ? Cu1 N2 C11 C10 -174.8(3) 1_665 . . . ? N2 C11 C10 C9 -0.5(6) . . . . ? O2 C9 C10 C11 178.1(3) . . . . ? C8 C9 C10 C11 -1.6(6) . . . . ? C6 O1 C3 C2 1.9(6) . . . . ? C6 O1 C3 C4 -177.7(4) . . . . ? C1 C2 C3 O1 179.0(4) . . . . ? C1 C2 C3 C4 -1.5(6) . . . . ? C11 N2 C7 C8 -0.3(6) . . . . ? Cu1 N2 C7 C8 175.9(3) 1_665 . . . ? C9 C8 C7 N2 -1.8(6) . . . . ? O1 C3 C4 C5 -179.3(4) . . . . ? C2 C3 C4 C5 1.2(7) . . . . ? O4 C14 C15 C16 -4.3(6) . . . . ? O5 C14 C15 C16 176.3(4) . . . . ? O4 C14 C15 C20 175.8(4) . . . . ? O5 C14 C15 C20 -3.5(6) . . . . ? C1 N1 C5 C4 -3.2(7) . . . . ? Cu2 N1 C5 C4 171.8(4) . . . . ? C3 C4 C5 N1 1.2(8) . . . . ? Cu1 O8 C21 O9 -20.3(5) . . . . ? Cu1 O8 C21 C22 163.0(5) . . . . ? C18 C17 C16 C15 0.2(8) . . . . ? C20 C15 C16 C17 1.1(7) . . . . ? C14 C15 C16 C17 -178.8(4) . . . . ? C16 C15 C20 C19 -0.7(8) . . . . ? C14 C15 C20 C19 179.1(5) . . . . ? C16 C17 C18 C19 -1.9(9) . . . . ? C17 C18 C19 C20 2.2(10) . . . . ? C15 C20 C19 C18 -0.8(9) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.932 _refine_diff_density_min -0.613 _refine_diff_density_rms 0.073 #_eof #End of Crystallographic Information File