# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Zheng, Qi-Yu' _publ_contact_author_email zhengqy@iccas.ac.cn _publ_section_title ; A novel 1D independent metal-organic nanotube based on cyclotriveratrylene ligand ; loop_ _publ_author_name 'Jin-Tao Yu' 'Junliang Sun' 'Zhi-Tang Huang' 'Qi-Yu Zheng' # Attachment '- Cu-CTV-revised.cif' data_CTV-Cu _database_code_depnum_ccdc_archive 'CCDC 817121' #TrackingRef '- Cu-CTV-revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C102 H86 Cu3 N2 O21' _chemical_formula_sum 'C102 H84 Cu3 N2 O21' _chemical_formula_weight 1864.33 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' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P42/nmc _symmetry_space_group_name_Hall '-P 4ac 2a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x, z+1/2' '-x+1/2, -y+1/2, z' 'y, -x+1/2, z+1/2' 'x+1/2, -y, -z' 'y+1/2, x+1/2, -z+1/2' '-x, y+1/2, -z' '-y, -x, -z+1/2' '-x, -y, -z' 'y-1/2, -x, -z-1/2' 'x-1/2, y-1/2, -z' '-y, x-1/2, -z-1/2' '-x-1/2, y, z' '-y-1/2, -x-1/2, z-1/2' 'x, -y-1/2, z' 'y, x, z-1/2' _cell_length_a 40.284(6) _cell_length_b 40.284(6) _cell_length_c 17.660(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 28659(8) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.864 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7720 _exptl_absorpt_coefficient_mu 0.488 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8512 _exptl_absorpt_correction_T_max 0.9164 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Saturn724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 77142 _diffrn_reflns_av_R_equivalents 0.1047 _diffrn_reflns_av_sigmaI/netI 0.0643 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_k_min -45 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 0.71 _diffrn_reflns_theta_max 24.87 _reflns_number_total 12828 _reflns_number_gt 10377 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELX97 (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. One restrains was added to restraint the occupancy summation of O46a and O46b to be 1. SQUEEZE in Platon was applied in the final refinement due to huge amount of disordered guests. The composition in the void was determined by TG and elemental analysis. ; _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^)+(0.1302P)^2^+35.3436P] 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 12828 _refine_ls_number_parameters 570 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1259 _refine_ls_R_factor_gt 0.1006 _refine_ls_wR_factor_ref 0.2742 _refine_ls_wR_factor_gt 0.2562 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.137 _refine_ls_shift/su_max 0.002 _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 0.2500 1.04436(2) 0.85431(4) 0.0413(3) Uani 1 2 d S . . Cu2 Cu 0.2500 1.10877(2) 0.88896(4) 0.0371(2) Uani 1 2 d S . . Cu3 Cu 0.08097(4) 0.7500 0.49339(8) 0.0874(4) Uani 1 2 d S . . O1 O 0.15161(9) 1.13394(10) 0.4445(2) 0.0591(10) Uani 1 1 d . . . O2 O 0.12074(11) 0.97659(10) 0.1936(2) 0.0682(12) Uani 1 1 d . . . O3 O 0.06544(10) 0.96367(9) 0.64248(18) 0.0561(10) Uani 1 1 d . . . O4 O 0.21667(10) 1.05673(11) 0.7818(2) 0.0650(11) Uani 1 1 d . . . O5 O 0.21602(9) 1.11143(9) 0.80801(18) 0.0492(9) Uani 1 1 d . . . O6 O 0.21601(8) 1.09591(9) -0.03647(17) 0.0452(8) Uani 1 1 d . . . O7 O 0.21566(10) 1.04237(9) -0.0693(2) 0.0595(10) Uani 1 1 d . . . O8 O 0.08203(18) 0.79739(13) 0.4920(4) 0.133(3) Uani 1 1 d . . . O9 O 0.04859(14) 0.79853(12) 0.5937(3) 0.0929(16) Uani 1 1 d . . . O11 O 0.2500 0.99135(13) 0.8409(3) 0.0538(13) Uani 1 2 d S . . H11 H 0.2319 0.9788 0.8423 0.065 Uiso 1 1 d R . . C1 C 0.20708(14) 1.08616(15) 0.7721(3) 0.0515(13) Uani 1 1 d . . . C2 C 0.18163(14) 1.09140(14) 0.7091(2) 0.0499(13) Uani 1 1 d . . . C3 C 0.16609(14) 1.06400(16) 0.6794(3) 0.0598(15) Uani 1 1 d . . . H3A H 0.1698 1.0426 0.7003 0.072 Uiso 1 1 calc R . . C4 C 0.14483(15) 1.06816(15) 0.6181(3) 0.0579(14) Uani 1 1 d . . . H4A H 0.1337 1.0493 0.5980 0.069 Uiso 1 1 calc R . . C5 C 0.13936(13) 1.09894(14) 0.5855(3) 0.0473(12) Uani 1 1 d . . . C6 C 0.15516(16) 1.12626(16) 0.6148(3) 0.0606(15) Uani 1 1 d . . . H6A H 0.1518 1.1474 0.5924 0.073 Uiso 1 1 calc R . . C7 C 0.17652(14) 1.12299(15) 0.6788(3) 0.0537(14) Uani 1 1 d . . . H7A H 0.1870 1.1419 0.7003 0.064 Uiso 1 1 calc R . . C8 C 0.11612(13) 1.10109(13) 0.5195(2) 0.0422(12) Uani 1 1 d . . . C9 C 0.08669(13) 1.08369(13) 0.5260(2) 0.0438(12) Uani 1 1 d . . . H9A H 0.0816 1.0741 0.5738 0.053 Uiso 1 1 calc R . . C10 C 0.06400(12) 1.07916(11) 0.4674(2) 0.0368(10) Uani 1 1 d . . . C11 C 0.07209(11) 1.09288(11) 0.3968(2) 0.0334(10) Uani 1 1 d . . . C12 C 0.10088(12) 1.11187(12) 0.3893(2) 0.0404(11) Uani 1 1 d . . . H12A H 0.1057 1.1221 0.3421 0.049 Uiso 1 1 calc R . . C13 C 0.12259(13) 1.11601(13) 0.4497(3) 0.0460(12) Uani 1 1 d . . . C14 C 0.15823(17) 1.1508(2) 0.3752(4) 0.085(2) Uani 1 1 d . . . H14A H 0.1798 1.1619 0.3784 0.127 Uiso 1 1 calc R . . H14B H 0.1409 1.1673 0.3660 0.127 Uiso 1 1 calc R . . H14C H 0.1585 1.1347 0.3335 0.127 Uiso 1 1 calc R . . C15 C 0.03304(13) 1.06014(12) 0.4858(2) 0.0422(12) Uani 1 1 d . . . H15A H 0.0165 1.0637 0.4452 0.051 Uiso 1 1 calc R . . H15B H 0.0235 1.0686 0.5337 0.051 Uiso 1 1 calc R . . C16 C 0.04014(11) 1.02313(13) 0.4935(2) 0.0406(11) Uani 1 1 d . . . C17 C 0.04922(12) 1.01010(12) 0.5645(2) 0.0391(11) Uani 1 1 d . . . H17A H 0.0505 1.0246 0.6068 0.047 Uiso 1 1 calc R . . C18 C 0.05614(12) 0.97741(13) 0.5743(2) 0.0429(12) Uani 1 1 d . . . C19 C 0.05316(13) 0.95492(13) 0.5139(2) 0.0445(12) Uani 1 1 d . . . C20 C 0.04436(12) 0.96760(13) 0.4439(2) 0.0427(12) Uani 1 1 d . . . H20A H 0.0428 0.9528 0.4022 0.051 Uiso 1 1 calc R . . C21 C 0.03767(12) 1.00103(14) 0.4319(2) 0.0441(12) Uani 1 1 d . . . C22 C 0.07210(18) 0.98644(15) 0.7024(3) 0.0651(17) Uani 1 1 d . . . H22A H 0.0784 0.9741 0.7481 0.098 Uiso 1 1 calc R . . H22B H 0.0522 0.9997 0.7127 0.098 Uiso 1 1 calc R . . H22C H 0.0903 1.0012 0.6876 0.098 Uiso 1 1 calc R . . C23 C 0.05814(14) 0.91830(13) 0.5230(3) 0.0472(12) Uani 1 1 d . . . C24 C 0.07637(16) 0.90045(14) 0.4717(3) 0.0624(16) Uani 1 1 d . . . H24A H 0.0877 0.9115 0.4319 0.075 Uiso 1 1 calc R . . C25 C 0.07825(18) 0.86611(17) 0.4780(4) 0.0761(19) Uani 1 1 d . . . H25A H 0.0907 0.8540 0.4417 0.091 Uiso 1 1 calc R . . C26 C 0.06259(17) 0.84929(15) 0.5356(4) 0.0648(16) Uani 1 1 d . . . C27 C 0.04522(15) 0.86718(15) 0.5887(3) 0.0591(15) Uani 1 1 d . . . H27A H 0.0350 0.8560 0.6299 0.071 Uiso 1 1 calc R . . C28 C 0.04258(14) 0.90115(14) 0.5826(3) 0.0518(13) Uani 1 1 d . . . H28A H 0.0301 0.9131 0.6192 0.062 Uiso 1 1 calc R . . C29 C 0.0636(2) 0.81257(19) 0.5431(5) 0.092(2) Uani 1 1 d . . . C30 C 0.02771(12) 1.01267(13) 0.3526(2) 0.0430(12) Uani 1 1 d . . . H30A H 0.0152 0.9946 0.3274 0.052 Uiso 1 1 calc R . . H30B H 0.0125 1.0319 0.3576 0.052 Uiso 1 1 calc R . . C31 C 0.05636(12) 1.02264(12) 0.3022(2) 0.0385(11) Uani 1 1 d . . . C32 C 0.07476(13) 0.99648(13) 0.2698(2) 0.0468(13) Uani 1 1 d . . . H32A H 0.0687 0.9743 0.2815 0.056 Uiso 1 1 calc R . . C33 C 0.10132(13) 1.00191(13) 0.2216(2) 0.0460(12) Uani 1 1 d . . . C34 C 0.10888(12) 1.03437(12) 0.1997(2) 0.0401(11) Uani 1 1 d . . . C35 C 0.09134(11) 1.05979(13) 0.2333(2) 0.0386(11) Uani 1 1 d . . . H35A H 0.0968 1.0819 0.2195 0.046 Uiso 1 1 calc R . . C36 C 0.06582(11) 1.05508(12) 0.2866(2) 0.0367(11) Uani 1 1 d . . . C37 C 0.11735(18) 0.94458(15) 0.2231(4) 0.0754(19) Uani 1 1 d . . . H37A H 0.1333 0.9297 0.1984 0.113 Uiso 1 1 calc R . . H37B H 0.0947 0.9365 0.2138 0.113 Uiso 1 1 calc R . . H37C H 0.1216 0.9450 0.2777 0.113 Uiso 1 1 calc R . . C38 C 0.13453(12) 1.04206(13) 0.1418(2) 0.0427(12) Uani 1 1 d . . . C39 C 0.15385(13) 1.07064(13) 0.1486(3) 0.0466(12) Uani 1 1 d . . . H39A H 0.1517 1.0843 0.1922 0.056 Uiso 1 1 calc R . . C40 C 0.17643(12) 1.07943(13) 0.0914(3) 0.0452(12) Uani 1 1 d . . . H40A H 0.1889 1.0994 0.0953 0.054 Uiso 1 1 calc R . . C41 C 0.18037(12) 1.05866(13) 0.0288(2) 0.0408(11) Uani 1 1 d . . . C42 C 0.16188(13) 1.03007(13) 0.0229(3) 0.0445(12) Uani 1 1 d . . . H42A H 0.1648 1.0159 -0.0195 0.053 Uiso 1 1 calc R . . C43 C 0.13896(12) 1.02180(13) 0.0787(2) 0.0428(12) Uani 1 1 d . . . H43 H 0.1262 1.0021 0.0738 0.051 Uiso 1 1 calc R . . C44 C 0.20610(13) 1.06666(14) -0.0303(2) 0.0451(12) Uani 1 1 d . . . C45 C 0.05148(12) 1.08554(12) 0.3262(2) 0.0382(11) Uani 1 1 d . . . H45A H 0.0281 1.0813 0.3407 0.046 Uiso 1 1 calc R . . H45B H 0.0520 1.1049 0.2916 0.046 Uiso 1 1 calc R . . O10 O 0.2500 1.16141(19) 0.9133(4) 0.087(2) Uani 1 2 d S . . C46A C 0.2346(7) 1.1705(7) 0.9869(16) 0.107(7) Uiso 0.3101(19) 1 d P . . H46A H 0.2202 1.1513 0.9991 0.129 Uiso 0.3101(19) 1 calc PR . . H46B H 0.2532 1.1694 1.0235 0.129 Uiso 0.3101(19) 1 calc PR . . C47A C 0.2171(16) 1.1966(17) 1.009(4) 0.28(3) Uiso 0.3101(19) 1 d P . . H47A H 0.2161 1.1973 1.0641 0.423 Uiso 0.3101(19) 1 calc PR . . H47B H 0.1946 1.1951 0.9881 0.423 Uiso 0.3101(19) 1 calc PR . . H47C H 0.2278 1.2169 0.9900 0.423 Uiso 0.3101(19) 1 calc PR . . C46B C 0.2500 1.1856(9) 0.860(2) 0.107(7) Uiso 0.380(4) 2 d SP . . C47B C 0.2318(12) 1.2015(14) 0.793(3) 0.131(18) Uiso 0.1899(19) 1 d P . . H47D H 0.2078 1.1992 0.8008 0.197 Uiso 0.1899(19) 1 calc PR . . H47E H 0.2383 1.1904 0.7463 0.197 Uiso 0.1899(19) 1 calc PR . . H47F H 0.2377 1.2251 0.7906 0.197 Uiso 0.1899(19) 1 calc PR . . O12 O 0.1163(3) 0.7500 0.3874(6) 0.166(4) Uiso 1 2 d S . . H12 H 0.1284 0.7670 0.3953 0.249 Uiso 1 1 d R . . N1 N 0.0399(3) 0.7409(3) 0.4280(6) 0.081(4) Uiso 0.50 1 d P . . C48 C 0.0121(3) 0.7575(4) 0.4314(6) 0.075(4) Uiso 0.50 1 d P . . H48 H 0.0101 0.7752 0.4666 0.090 Uiso 0.50 1 calc PR . . C49 C -0.0142(3) 0.7500 0.3855(7) 0.097(3) Uiso 1 2 d S . . H49 H -0.0345 0.7616 0.3929 0.116 Uiso 0.50 1 calc PR . . C50 C -0.0128(4) 0.7273(3) 0.3313(8) 0.076(4) Uiso 0.50 1 d P . . H50 H -0.0307 0.7234 0.2975 0.092 Uiso 0.50 1 calc PR . . C51 C 0.0157(4) 0.7103(5) 0.3276(10) 0.101(5) Uiso 0.50 1 d P . . H51 H 0.0176 0.6937 0.2898 0.122 Uiso 0.50 1 calc PR . . C52 C 0.0416(4) 0.7154(4) 0.3740(9) 0.089(4) Uiso 0.50 1 d P . . H52 H 0.0609 0.7019 0.3703 0.106 Uiso 0.50 1 calc PR . . N2 N 0.1154(3) 0.7421(5) 0.5669(7) 0.135(6) Uiso 0.50 1 d PG . . C53 C 0.1125(3) 0.7507(7) 0.6417(8) 0.144(6) Uiso 1 2 d SG . . H53 H 0.0929 0.7618 0.6579 0.173 Uiso 0.50 1 calc PR . . C54 C 0.1367(5) 0.7438(9) 0.6942(7) 0.248(14) Uiso 0.50 1 d PG . . H54 H 0.1349 0.7518 0.7447 0.297 Uiso 0.50 1 calc PR . . C55 C 0.1639(5) 0.7249(7) 0.6720(14) 0.297 Uiso 0.50 1 d PG . . H55 H 0.1805 0.7191 0.7079 0.297 Uiso 0.50 1 calc PR . . C56 C 0.1668(5) 0.7146(6) 0.5972(18) 0.39(3) Uiso 0.50 1 d PG . . H56 H 0.1854 0.7017 0.5819 0.464 Uiso 0.50 1 calc PR . . C57 C 0.1426(5) 0.7232(5) 0.5446(11) 0.240(16) Uiso 0.50 1 d PG . . H57 H 0.1446 0.7161 0.4935 0.288 Uiso 0.50 1 calc PR . . 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 0.0406(5) 0.0538(6) 0.0295(4) 0.0042(3) 0.000 0.000 Cu2 0.0346(5) 0.0499(5) 0.0268(4) 0.0024(3) 0.000 0.000 Cu3 0.1001(10) 0.0468(7) 0.1153(10) 0.000 0.0224(8) 0.000 O1 0.053(2) 0.072(3) 0.052(2) 0.0102(18) -0.0141(17) -0.016(2) O2 0.099(3) 0.052(2) 0.053(2) 0.0000(18) 0.032(2) 0.000(2) O3 0.087(3) 0.048(2) 0.0333(17) -0.0004(15) -0.0104(17) -0.007(2) O4 0.074(3) 0.067(3) 0.055(2) 0.0014(19) -0.024(2) 0.006(2) O5 0.048(2) 0.061(2) 0.0390(17) -0.0014(16) -0.0077(15) -0.0001(18) O6 0.046(2) 0.051(2) 0.0379(17) 0.0011(15) 0.0121(15) 0.0000(17) O7 0.069(3) 0.049(2) 0.061(2) -0.0064(18) 0.025(2) -0.0023(19) O8 0.170(6) 0.049(3) 0.179(6) -0.002(3) 0.087(5) -0.014(3) O9 0.104(4) 0.055(3) 0.119(4) 0.018(3) 0.008(3) -0.015(3) O11 0.048(3) 0.058(3) 0.055(3) -0.012(2) 0.000 0.000 C1 0.049(3) 0.065(4) 0.040(3) 0.005(3) 0.000(2) 0.000(3) C2 0.060(3) 0.066(4) 0.024(2) -0.006(2) -0.006(2) -0.003(3) C3 0.060(4) 0.066(4) 0.054(3) 0.009(3) -0.019(3) -0.004(3) C4 0.061(4) 0.063(4) 0.050(3) 0.005(3) -0.015(3) -0.009(3) C5 0.044(3) 0.061(3) 0.037(2) 0.002(2) -0.008(2) -0.003(3) C6 0.068(4) 0.061(4) 0.053(3) 0.000(3) -0.013(3) 0.000(3) C7 0.061(4) 0.060(4) 0.040(3) 0.004(2) -0.006(2) -0.001(3) C8 0.047(3) 0.049(3) 0.030(2) 0.005(2) -0.008(2) 0.006(2) C9 0.055(3) 0.051(3) 0.025(2) 0.002(2) -0.003(2) 0.009(3) C10 0.041(3) 0.041(3) 0.029(2) 0.0002(19) 0.0051(19) 0.003(2) C11 0.039(3) 0.034(2) 0.027(2) 0.0016(17) -0.0025(18) 0.001(2) C12 0.044(3) 0.042(3) 0.035(2) 0.010(2) -0.002(2) 0.004(2) C13 0.051(3) 0.051(3) 0.036(2) 0.000(2) -0.010(2) -0.004(3) C14 0.065(4) 0.110(6) 0.079(4) 0.052(4) -0.024(3) -0.039(4) C15 0.052(3) 0.048(3) 0.027(2) 0.0006(19) 0.007(2) -0.001(2) C16 0.036(3) 0.059(3) 0.027(2) 0.006(2) 0.0072(18) -0.008(2) C17 0.049(3) 0.044(3) 0.024(2) -0.0107(19) 0.0004(19) -0.011(2) C18 0.047(3) 0.057(3) 0.024(2) 0.001(2) -0.0016(19) -0.006(2) C19 0.054(3) 0.047(3) 0.032(2) 0.005(2) 0.008(2) -0.013(2) C20 0.051(3) 0.048(3) 0.030(2) -0.001(2) 0.004(2) -0.013(2) C21 0.043(3) 0.065(4) 0.024(2) 0.000(2) 0.0040(19) -0.014(3) C22 0.109(5) 0.060(4) 0.027(2) 0.002(2) -0.016(3) -0.019(3) C23 0.058(3) 0.048(3) 0.036(2) 0.000(2) -0.003(2) -0.006(3) C24 0.081(4) 0.051(4) 0.056(3) -0.003(3) 0.025(3) -0.007(3) C25 0.087(5) 0.061(4) 0.081(4) -0.015(3) 0.022(4) 0.003(4) C26 0.078(4) 0.051(4) 0.065(4) -0.005(3) 0.009(3) -0.012(3) C27 0.062(4) 0.059(4) 0.056(3) 0.009(3) -0.005(3) -0.003(3) C28 0.064(4) 0.055(3) 0.036(2) 0.001(2) 0.000(2) 0.000(3) C29 0.106(6) 0.060(5) 0.109(6) -0.009(4) 0.025(5) -0.034(4) C30 0.044(3) 0.060(3) 0.025(2) 0.002(2) 0.0017(19) -0.020(2) C31 0.046(3) 0.048(3) 0.0219(19) -0.0039(19) -0.0055(18) -0.012(2) C32 0.065(3) 0.046(3) 0.029(2) 0.004(2) -0.001(2) -0.021(3) C33 0.058(3) 0.052(3) 0.028(2) -0.007(2) 0.008(2) -0.002(3) C34 0.042(3) 0.048(3) 0.030(2) 0.002(2) 0.001(2) -0.007(2) C35 0.041(3) 0.052(3) 0.023(2) -0.0006(19) 0.0024(18) -0.008(2) C36 0.040(3) 0.051(3) 0.0196(18) -0.0004(18) -0.0048(17) -0.010(2) C37 0.091(5) 0.048(4) 0.088(5) 0.004(3) 0.025(4) -0.003(3) C38 0.040(3) 0.053(3) 0.035(2) 0.003(2) -0.001(2) -0.004(2) C39 0.054(3) 0.044(3) 0.042(3) -0.001(2) 0.001(2) 0.001(3) C40 0.042(3) 0.054(3) 0.040(2) 0.004(2) 0.007(2) -0.013(2) C41 0.037(3) 0.057(3) 0.028(2) 0.015(2) 0.0019(19) 0.002(2) C42 0.047(3) 0.055(3) 0.032(2) -0.005(2) 0.005(2) -0.004(3) C43 0.046(3) 0.048(3) 0.035(2) 0.001(2) 0.003(2) -0.003(2) C44 0.049(3) 0.057(3) 0.030(2) 0.002(2) 0.003(2) -0.007(3) C45 0.039(3) 0.052(3) 0.0230(19) 0.0058(19) 0.0029(18) -0.002(2) O10 0.085(5) 0.092(5) 0.085(5) -0.025(4) 0.000 0.000 _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 1.921(4) . ? Cu1 O4 1.921(4) 13_655 ? Cu1 O7 1.934(4) 1_556 ? Cu1 O7 1.934(4) 13_656 ? Cu1 O11 2.149(5) . ? Cu1 Cu2 2.6657(13) . ? Cu2 O6 1.969(3) 1_556 ? Cu2 O6 1.969(3) 13_656 ? Cu2 O5 1.982(3) . ? Cu2 O5 1.982(3) 13_655 ? Cu2 O10 2.164(7) . ? Cu3 O8 1.910(5) . ? Cu3 O8 1.910(5) 15_575 ? Cu3 N2 1.928(12) 15_575 ? Cu3 N2 1.928(12) . ? Cu3 N1 2.051(11) . ? Cu3 N1 2.051(11) 15_575 ? Cu3 O12 2.351(12) . ? O1 C13 1.377(6) . ? O1 C14 1.425(7) . ? O2 C33 1.377(6) . ? O2 C37 1.397(7) . ? O3 C18 1.377(5) . ? O3 C22 1.426(6) . ? O4 C1 1.259(7) . ? O5 C1 1.252(6) . ? O6 C44 1.249(6) . ? O6 Cu2 1.969(3) 1_554 ? O7 C44 1.257(6) . ? O7 Cu1 1.934(4) 1_554 ? O8 C29 1.320(9) . ? O9 C29 1.218(8) . ? O11 H11 0.8892 . ? C1 C2 1.527(7) . ? C2 C3 1.374(8) . ? C2 C7 1.396(8) . ? C3 C4 1.389(7) . ? C3 H3A 0.9500 . ? C4 C5 1.385(8) . ? C4 H4A 0.9500 . ? C5 C6 1.373(8) . ? C5 C8 1.497(6) . ? C6 C7 1.427(7) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C9 1.382(7) . ? C8 C13 1.396(6) . ? C9 C10 1.392(6) . ? C9 H9A 0.9500 . ? C10 C11 1.402(6) . ? C10 C15 1.499(7) . ? C11 C12 1.396(7) . ? C11 C45 1.526(6) . ? C12 C13 1.390(6) . ? C12 H12A 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.524(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C21 1.409(7) . ? C16 C17 1.409(6) . ? C17 C18 1.357(7) . ? C17 H17A 0.9500 . ? C18 C19 1.405(7) . ? C19 C20 1.383(6) . ? C19 C23 1.498(7) . ? C20 C21 1.389(7) . ? C20 H20A 0.9500 . ? C21 C30 1.531(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.370(7) . ? C23 C28 1.406(7) . ? C24 C25 1.390(9) . ? C24 H24A 0.9500 . ? C25 C26 1.375(9) . ? C25 H25A 0.9500 . ? C26 C27 1.373(8) . ? C26 C29 1.485(10) . ? C27 C28 1.377(8) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C30 C31 1.512(6) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C36 1.389(7) . ? C31 C32 1.409(7) . ? C32 C33 1.385(7) . ? C32 H32A 0.9500 . ? C33 C34 1.397(7) . ? C34 C35 1.378(7) . ? C34 C38 1.486(6) . ? C35 C36 1.407(6) . ? C35 H35A 0.9500 . ? C36 C45 1.526(7) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C43 1.392(7) . ? C38 C39 1.395(7) . ? C39 C40 1.404(7) . ? C39 H39A 0.9500 . ? C40 C41 1.396(7) . ? C40 H40A 0.9500 . ? C41 C42 1.375(7) . ? C41 C44 1.506(6) . ? C42 C43 1.391(7) . ? C42 H42A 0.9500 . ? C43 H43 0.9500 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? O10 C46B 1.36(4) . ? O10 C46A 1.49(3) 13_655 ? O10 C46A 1.49(3) . ? C46A C47A 1.33(6) . ? C46A H46A 0.9900 . ? C46A H46B 0.9900 . ? C47A H47A 0.9800 . ? C47A H47B 0.9800 . ? C47A H47C 0.9800 . ? C46B C47B 1.52(5) . ? C46B C47B 1.52(5) 13_655 ? C47B H47D 0.9800 . ? C47B H47E 0.9800 . ? C47B H47F 0.9800 . ? O12 H12 0.8524 . ? N1 N1 0.74(2) 15_575 ? N1 C48 1.123(13) 15_575 ? N1 C48 1.305(14) . ? N1 C52 1.403(18) . ? C48 C49 1.367(15) . ? C48 H48 0.9500 . ? C49 C50 1.324(15) . ? C49 H49 0.9500 . ? C50 C51 1.34(2) . ? C50 H50 0.9500 . ? C51 C52 1.34(2) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? N2 C53 1.36(2) . ? N2 C57 1.3900 . ? C53 C54 1.3751 . ? C53 H53 0.9500 . ? C54 C55 1.3900 . ? C54 H54 0.9500 . ? C55 C56 1.3900 . ? C55 H55 0.9500 . ? C56 C57 1.3900 . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? 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 O4 88.7(3) . 13_655 ? O4 Cu1 O7 88.60(18) . 1_556 ? O4 Cu1 O7 167.33(18) 13_655 1_556 ? O4 Cu1 O7 167.33(18) . 13_656 ? O4 Cu1 O7 88.60(18) 13_655 13_656 ? O7 Cu1 O7 91.4(3) 1_556 13_656 ? O4 Cu1 O11 100.64(16) . . ? O4 Cu1 O11 100.64(16) 13_655 . ? O7 Cu1 O11 92.03(15) 1_556 . ? O7 Cu1 O11 92.03(15) 13_656 . ? O4 Cu1 Cu2 84.29(13) . . ? O4 Cu1 Cu2 84.29(13) 13_655 . ? O7 Cu1 Cu2 83.12(11) 1_556 . ? O7 Cu1 Cu2 83.12(11) 13_656 . ? O11 Cu1 Cu2 173.03(14) . . ? O6 Cu2 O6 88.1(2) 1_556 13_656 ? O6 Cu2 O5 90.94(14) 1_556 . ? O6 Cu2 O5 167.62(16) 13_656 . ? O6 Cu2 O5 167.62(16) 1_556 13_655 ? O6 Cu2 O5 90.94(14) 13_656 13_655 ? O5 Cu2 O5 87.3(2) . 13_655 ? O6 Cu2 O10 97.18(18) 1_556 . ? O6 Cu2 O10 97.18(18) 13_656 . ? O5 Cu2 O10 95.18(18) . . ? O5 Cu2 O10 95.18(19) 13_655 . ? O6 Cu2 Cu1 84.12(11) 1_556 . ? O6 Cu2 Cu1 84.12(11) 13_656 . ? O5 Cu2 Cu1 83.51(11) . . ? O5 Cu2 Cu1 83.51(11) 13_655 . ? O10 Cu2 Cu1 178.2(2) . . ? O8 Cu3 O8 177.1(4) . 15_575 ? O8 Cu3 N2 80.0(6) . 15_575 ? O8 Cu3 N2 99.1(6) 15_575 15_575 ? O8 Cu3 N2 99.1(6) . . ? O8 Cu3 N2 80.0(6) 15_575 . ? N2 Cu3 N2 19.1(11) 15_575 . ? O8 Cu3 N1 100.9(4) . . ? O8 Cu3 N1 80.3(4) 15_575 . ? N2 Cu3 N1 171.9(5) 15_575 . ? N2 Cu3 N1 158.5(6) . . ? O8 Cu3 N1 80.3(4) . 15_575 ? O8 Cu3 N1 100.9(4) 15_575 15_575 ? N2 Cu3 N1 158.5(6) 15_575 15_575 ? N2 Cu3 N1 171.9(5) . 15_575 ? N1 Cu3 N1 20.6(6) . 15_575 ? O8 Cu3 O12 88.64(19) . . ? O8 Cu3 O12 88.64(19) 15_575 . ? N2 Cu3 O12 95.8(5) 15_575 . ? N2 Cu3 O12 95.8(5) . . ? N1 Cu3 O12 92.3(4) . . ? N1 Cu3 O12 92.3(4) 15_575 . ? C13 O1 C14 117.7(4) . . ? C33 O2 C37 119.6(4) . . ? C18 O3 C22 116.2(4) . . ? C1 O4 Cu1 123.4(4) . . ? C1 O5 Cu2 121.3(4) . . ? C44 O6 Cu2 121.9(3) . 1_554 ? C44 O7 Cu1 124.7(3) . 1_554 ? C29 O8 Cu3 116.2(5) . . ? Cu1 O11 H11 124.3 . . ? O5 C1 O4 127.5(5) . . ? O5 C1 C2 116.7(5) . . ? O4 C1 C2 115.8(5) . . ? C3 C2 C7 121.2(5) . . ? C3 C2 C1 118.3(5) . . ? C7 C2 C1 120.3(5) . . ? C2 C3 C4 118.8(6) . . ? C2 C3 H3A 120.6 . . ? C4 C3 H3A 120.6 . . ? C5 C4 C3 122.0(5) . . ? C5 C4 H4A 119.0 . . ? C3 C4 H4A 119.0 . . ? C6 C5 C4 119.1(5) . . ? C6 C5 C8 122.5(5) . . ? C4 C5 C8 118.4(5) . . ? C5 C6 C7 120.3(5) . . ? C5 C6 H6A 119.9 . . ? C7 C6 H6A 119.9 . . ? C2 C7 C6 118.5(5) . . ? C2 C7 H7A 120.8 . . ? C6 C7 H7A 120.8 . . ? C9 C8 C13 116.8(4) . . ? C9 C8 C5 116.3(4) . . ? C13 C8 C5 126.5(5) . . ? C8 C9 C10 124.6(4) . . ? C8 C9 H9A 117.7 . . ? C10 C9 H9A 117.7 . . ? C9 C10 C11 117.2(4) . . ? C9 C10 C15 116.9(4) . . ? C11 C10 C15 125.9(4) . . ? C12 C11 C10 119.6(4) . . ? C12 C11 C45 118.7(4) . . ? C10 C11 C45 121.6(4) . . ? C13 C12 C11 121.0(4) . . ? C13 C12 H12A 119.5 . . ? C11 C12 H12A 119.5 . . ? O1 C13 C12 123.1(4) . . ? O1 C13 C8 116.3(4) . . ? C12 C13 C8 120.6(5) . . ? O1 C14 H14A 109.5 . . ? O1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C15 C16 111.3(4) . . ? C10 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? C10 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C21 C16 C17 118.1(5) . . ? C21 C16 C15 122.4(4) . . ? C17 C16 C15 119.5(4) . . ? C18 C17 C16 121.9(4) . . ? C18 C17 H17A 119.1 . . ? C16 C17 H17A 119.1 . . ? C17 C18 O3 123.9(4) . . ? C17 C18 C19 120.7(4) . . ? O3 C18 C19 115.4(5) . . ? C20 C19 C18 117.5(5) . . ? C20 C19 C23 119.6(4) . . ? C18 C19 C23 122.8(4) . . ? C19 C20 C21 123.0(4) . . ? C19 C20 H20A 118.5 . . ? C21 C20 H20A 118.5 . . ? C20 C21 C16 118.7(4) . . ? C20 C21 C30 119.2(4) . . ? C16 C21 C30 122.1(5) . . ? O3 C22 H22A 109.5 . . ? O3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C28 118.4(5) . . ? C24 C23 C19 121.1(5) . . ? C28 C23 C19 120.3(5) . . ? C23 C24 C25 119.9(5) . . ? C23 C24 H24A 120.1 . . ? C25 C24 H24A 120.1 . . ? C26 C25 C24 121.6(6) . . ? C26 C25 H25A 119.2 . . ? C24 C25 H25A 119.2 . . ? C27 C26 C25 118.6(6) . . ? C27 C26 C29 118.4(6) . . ? C25 C26 C29 122.9(6) . . ? C26 C27 C28 120.6(6) . . ? C26 C27 H27A 119.7 . . ? C28 C27 H27A 119.7 . . ? C27 C28 C23 120.8(5) . . ? C27 C28 H28A 119.6 . . ? C23 C28 H28A 119.6 . . ? O9 C29 O8 124.5(7) . . ? O9 C29 C26 121.0(7) . . ? O8 C29 C26 114.6(7) . . ? C31 C30 C21 114.8(4) . . ? C31 C30 H30A 108.6 . . ? C21 C30 H30A 108.6 . . ? C31 C30 H30B 108.6 . . ? C21 C30 H30B 108.6 . . ? H30A C30 H30B 107.5 . . ? C36 C31 C32 118.6(4) . . ? C36 C31 C30 125.2(4) . . ? C32 C31 C30 116.2(4) . . ? C33 C32 C31 122.5(5) . . ? C33 C32 H32A 118.8 . . ? C31 C32 H32A 118.8 . . ? O2 C33 C32 122.8(5) . . ? O2 C33 C34 118.0(4) . . ? C32 C33 C34 119.1(5) . . ? C35 C34 C33 117.7(4) . . ? C35 C34 C38 119.8(4) . . ? C33 C34 C38 122.5(4) . . ? C34 C35 C36 124.2(5) . . ? C34 C35 H35A 117.9 . . ? C36 C35 H35A 117.9 . . ? C31 C36 C35 117.4(4) . . ? C31 C36 C45 124.2(4) . . ? C35 C36 C45 118.4(4) . . ? O2 C37 H37A 109.5 . . ? O2 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O2 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C43 C38 C39 118.8(4) . . ? C43 C38 C34 121.1(4) . . ? C39 C38 C34 120.1(4) . . ? C38 C39 C40 120.5(5) . . ? C38 C39 H39A 119.7 . . ? C40 C39 H39A 119.7 . . ? C41 C40 C39 119.5(5) . . ? C41 C40 H40A 120.3 . . ? C39 C40 H40A 120.3 . . ? C42 C41 C40 120.0(4) . . ? C42 C41 C44 120.0(4) . . ? C40 C41 C44 119.9(5) . . ? C41 C42 C43 120.4(4) . . ? C41 C42 H42A 119.8 . . ? C43 C42 H42A 119.8 . . ? C42 C43 C38 120.8(5) . . ? C42 C43 H43 119.6 . . ? C38 C43 H43 119.6 . . ? O6 C44 O7 126.1(4) . . ? O6 C44 C41 118.8(5) . . ? O7 C44 C41 115.1(5) . . ? C36 C45 C11 108.9(4) . . ? C36 C45 H45A 109.9 . . ? C11 C45 H45A 109.9 . . ? C36 C45 H45B 109.9 . . ? C11 C45 H45B 109.9 . . ? H45A C45 H45B 108.3 . . ? C46B O10 Cu2 124.4(16) . . ? C46A O10 Cu2 114.5(12) 13_655 . ? C46A O10 Cu2 114.5(12) . . ? C47A C46A O10 132(4) . . ? C47A C46A H46A 104.2 . . ? O10 C46A H46A 104.2 . . ? C47A C46A H46B 104.2 . . ? O10 C46A H46B 104.2 . . ? H46A C46A H46B 105.5 . . ? C46A C47A H47A 109.5 . . ? C46A C47A H47B 109.5 . . ? H47A C47A H47B 109.5 . . ? C46A C47A H47C 109.5 . . ? H47A C47A H47C 109.5 . . ? H47B C47A H47C 109.5 . . ? O10 C46B C47B 147(3) . . ? O10 C46B C47B 147(3) . 13_655 ? C47B C46B C47B 57(4) . 13_655 ? C46B C47B H47D 109.5 . . ? C46B C47B H47E 109.5 . . ? H47D C47B H47E 109.5 . . ? C46B C47B H47F 109.5 . . ? H47D C47B H47F 109.5 . . ? H47E C47B H47F 109.5 . . ? Cu3 O12 H12 102.5 . . ? C48 N1 C52 97.4(12) 15_575 . ? C48 N1 C52 116.6(12) . . ? N1 N1 Cu3 79.7(3) 15_575 . ? C48 N1 Cu3 139.8(10) 15_575 . ? C48 N1 Cu3 125.1(9) . . ? C52 N1 Cu3 118.3(10) . . ? N1 C48 C49 121.7(12) . . ? N1 C48 H48 119.2 . . ? C49 C48 H48 119.2 . . ? C50 C49 C48 123.1(13) . . ? C50 C49 H49 118.4 . . ? C48 C49 H49 118.4 . . ? C49 C50 C51 115.2(15) . . ? C49 C50 H50 122.4 . . ? C51 C50 H50 122.4 . . ? C50 C51 C52 124.0(17) . . ? C50 C51 H51 118.0 . . ? C52 C51 H51 118.0 . . ? C51 C52 N1 119.2(15) . . ? C51 C52 C48 85.8(12) . 15_575 ? C51 C52 H52 120.4 . . ? N1 C52 H52 120.4 . . ? C48 C52 H52 151.0 15_575 . ? N2 N2 C57 123.2(10) 15_575 . ? C53 N2 C57 117.5(12) 15_575 . ? C53 N2 C57 118.7 . . ? C53 N2 C57 95.6(19) 15_575 15_575 ? C53 N2 C57 93.8(4) . 15_575 ? C53 N2 Cu3 123.8(13) 15_575 . ? C53 N2 Cu3 123.0(11) . . ? C57 N2 Cu3 117.9(11) . . ? C57 N2 Cu3 99.2(12) 15_575 . ? C54 C53 N2 123.6(16) . . ? C54 C53 H53 118.8 . . ? N2 C53 H53 118.8 . . ? C53 C54 C55 118.6 . . ? C53 C54 H54 120.7 . . ? C55 C54 H54 120.7 . . ? C56 C55 C54 120.0 . . ? C56 C55 C54 119.50(18) . 15_575 ? C56 C55 H55 120.0 . . ? C54 C55 H55 120.0 . . ? C54 C55 H55 118.5 15_575 . ? C55 C55 H55 104.4 15_575 . ? C55 C56 C57 120.0 . . ? C55 C56 H56 120.0 . . ? C57 C56 H56 120.0 . . ? C56 C57 N2 120.0 . . ? C56 C57 N2 118.0(4) . 15_575 ? C56 C57 H57 120.0 . . ? N2 C57 H57 120.0 . . ? N2 C57 H57 119.1 15_575 . ? 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 O4 Cu1 Cu2 O6 91.03(17) . . . 1_556 ? O4 Cu1 Cu2 O6 -179.73(16) 13_655 . . 1_556 ? O7 Cu1 Cu2 O6 1.76(16) 1_556 . . 1_556 ? O7 Cu1 Cu2 O6 -90.46(16) 13_656 . . 1_556 ? O4 Cu1 Cu2 O6 179.73(16) . . . 13_656 ? O4 Cu1 Cu2 O6 -91.03(17) 13_655 . . 13_656 ? O7 Cu1 Cu2 O6 90.46(16) 1_556 . . 13_656 ? O7 Cu1 Cu2 O6 -1.76(16) 13_656 . . 13_656 ? O4 Cu1 Cu2 O5 -0.60(16) . . . . ? O4 Cu1 Cu2 O5 88.65(17) 13_655 . . . ? O7 Cu1 Cu2 O5 -89.87(17) 1_556 . . . ? O7 Cu1 Cu2 O5 177.92(16) 13_656 . . . ? O4 Cu1 Cu2 O5 -88.65(17) . . . 13_655 ? O4 Cu1 Cu2 O5 0.60(16) 13_655 . . 13_655 ? O7 Cu1 Cu2 O5 -177.92(16) 1_556 . . 13_655 ? O7 Cu1 Cu2 O5 89.87(17) 13_656 . . 13_655 ? O4 Cu1 O4 C1 -82.6(5) 13_655 . . . ? O7 Cu1 O4 C1 85.0(5) 1_556 . . . ? O7 Cu1 O4 C1 -4.9(11) 13_656 . . . ? O11 Cu1 O4 C1 176.8(4) . . . . ? Cu2 Cu1 O4 C1 1.8(4) . . . . ? O6 Cu2 O5 C1 -84.4(4) 1_556 . . . ? O6 Cu2 O5 C1 1.1(9) 13_656 . . . ? O5 Cu2 O5 C1 83.4(4) 13_655 . . . ? O10 Cu2 O5 C1 178.3(4) . . . . ? Cu1 Cu2 O5 C1 -0.4(4) . . . . ? N2 Cu3 O8 C29 -86.4(8) 15_575 . . . ? N2 Cu3 O8 C29 -86.8(8) . . . . ? N1 Cu3 O8 C29 85.4(8) . . . . ? N1 Cu3 O8 C29 84.9(8) 15_575 . . . ? O12 Cu3 O8 C29 177.5(8) . . . . ? Cu2 O5 C1 O4 2.0(8) . . . . ? Cu2 O5 C1 C2 -177.9(3) . . . . ? Cu1 O4 C1 O5 -2.9(8) . . . . ? Cu1 O4 C1 C2 177.0(3) . . . . ? O5 C1 C2 C3 -166.6(5) . . . . ? O4 C1 C2 C3 13.4(7) . . . . ? O5 C1 C2 C7 18.6(7) . . . . ? O4 C1 C2 C7 -161.4(5) . . . . ? C7 C2 C3 C4 -0.3(9) . . . . ? C1 C2 C3 C4 -175.0(5) . . . . ? C2 C3 C4 C5 1.2(9) . . . . ? C3 C4 C5 C6 -0.6(9) . . . . ? C3 C4 C5 C8 179.8(5) . . . . ? C4 C5 C6 C7 -1.0(9) . . . . ? C8 C5 C6 C7 178.6(5) . . . . ? C3 C2 C7 C6 -1.2(8) . . . . ? C1 C2 C7 C6 173.5(5) . . . . ? C5 C6 C7 C2 1.8(9) . . . . ? C6 C5 C8 C9 -135.1(6) . . . . ? C4 C5 C8 C9 44.5(7) . . . . ? C6 C5 C8 C13 51.9(8) . . . . ? C4 C5 C8 C13 -128.5(6) . . . . ? C13 C8 C9 C10 2.4(8) . . . . ? C5 C8 C9 C10 -171.4(5) . . . . ? C8 C9 C10 C11 1.1(7) . . . . ? C8 C9 C10 C15 -178.7(5) . . . . ? C9 C10 C11 C12 -3.9(7) . . . . ? C15 C10 C11 C12 175.8(4) . . . . ? C9 C10 C11 C45 171.6(4) . . . . ? C15 C10 C11 C45 -8.6(7) . . . . ? C10 C11 C12 C13 3.4(7) . . . . ? C45 C11 C12 C13 -172.3(4) . . . . ? C14 O1 C13 C12 4.4(8) . . . . ? C14 O1 C13 C8 -177.1(6) . . . . ? C11 C12 C13 O1 178.6(5) . . . . ? C11 C12 C13 C8 0.3(8) . . . . ? C9 C8 C13 O1 178.5(5) . . . . ? C5 C8 C13 O1 -8.5(8) . . . . ? C9 C8 C13 C12 -3.0(8) . . . . ? C5 C8 C13 C12 170.0(5) . . . . ? C9 C10 C15 C16 -74.2(5) . . . . ? C11 C10 C15 C16 106.0(5) . . . . ? C10 C15 C16 C21 -91.5(5) . . . . ? C10 C15 C16 C17 89.1(5) . . . . ? C21 C16 C17 C18 1.3(7) . . . . ? C15 C16 C17 C18 -179.3(4) . . . . ? C16 C17 C18 O3 179.3(5) . . . . ? C16 C17 C18 C19 -2.6(8) . . . . ? C22 O3 C18 C17 -8.4(8) . . . . ? C22 O3 C18 C19 173.4(5) . . . . ? C17 C18 C19 C20 2.7(7) . . . . ? O3 C18 C19 C20 -179.0(4) . . . . ? C17 C18 C19 C23 -175.5(5) . . . . ? O3 C18 C19 C23 2.8(7) . . . . ? C18 C19 C20 C21 -1.6(8) . . . . ? C23 C19 C20 C21 176.7(5) . . . . ? C19 C20 C21 C16 0.4(7) . . . . ? C19 C20 C21 C30 -179.3(5) . . . . ? C17 C16 C21 C20 -0.2(7) . . . . ? C15 C16 C21 C20 -179.6(4) . . . . ? C17 C16 C21 C30 179.5(4) . . . . ? C15 C16 C21 C30 0.1(7) . . . . ? C20 C19 C23 C24 46.1(8) . . . . ? C18 C19 C23 C24 -135.7(6) . . . . ? C20 C19 C23 C28 -130.4(5) . . . . ? C18 C19 C23 C28 47.8(7) . . . . ? C28 C23 C24 C25 2.0(9) . . . . ? C19 C23 C24 C25 -174.6(6) . . . . ? C23 C24 C25 C26 -1.0(11) . . . . ? C24 C25 C26 C27 -1.2(11) . . . . ? C24 C25 C26 C29 178.8(7) . . . . ? C25 C26 C27 C28 2.3(10) . . . . ? C29 C26 C27 C28 -177.7(6) . . . . ? C26 C27 C28 C23 -1.3(9) . . . . ? C24 C23 C28 C27 -0.9(8) . . . . ? C19 C23 C28 C27 175.7(5) . . . . ? Cu3 O8 C29 O9 6.3(13) . . . . ? Cu3 O8 C29 C26 -174.5(5) . . . . ? C27 C26 C29 O9 2.1(12) . . . . ? C25 C26 C29 O9 -177.9(8) . . . . ? C27 C26 C29 O8 -177.0(7) . . . . ? C25 C26 C29 O8 3.0(12) . . . . ? C20 C21 C30 C31 -89.6(6) . . . . ? C16 C21 C30 C31 90.7(6) . . . . ? C21 C30 C31 C36 -102.1(6) . . . . ? C21 C30 C31 C32 77.1(5) . . . . ? C36 C31 C32 C33 -1.7(7) . . . . ? C30 C31 C32 C33 179.0(4) . . . . ? C37 O2 C33 C32 -10.3(8) . . . . ? C37 O2 C33 C34 170.1(5) . . . . ? C31 C32 C33 O2 175.7(5) . . . . ? C31 C32 C33 C34 -4.6(7) . . . . ? O2 C33 C34 C35 -174.2(4) . . . . ? C32 C33 C34 C35 6.2(7) . . . . ? O2 C33 C34 C38 6.5(7) . . . . ? C32 C33 C34 C38 -173.2(4) . . . . ? C33 C34 C35 C36 -1.7(7) . . . . ? C38 C34 C35 C36 177.7(4) . . . . ? C32 C31 C36 C35 6.1(6) . . . . ? C30 C31 C36 C35 -174.7(4) . . . . ? C32 C31 C36 C45 -170.9(4) . . . . ? C30 C31 C36 C45 8.3(7) . . . . ? C34 C35 C36 C31 -4.6(6) . . . . ? C34 C35 C36 C45 172.6(4) . . . . ? C35 C34 C38 C43 -142.4(5) . . . . ? C33 C34 C38 C43 37.0(7) . . . . ? C35 C34 C38 C39 35.2(7) . . . . ? C33 C34 C38 C39 -145.4(5) . . . . ? C43 C38 C39 C40 2.4(7) . . . . ? C34 C38 C39 C40 -175.3(5) . . . . ? C38 C39 C40 C41 -2.4(8) . . . . ? C39 C40 C41 C42 0.9(7) . . . . ? C39 C40 C41 C44 -176.0(5) . . . . ? C40 C41 C42 C43 0.6(7) . . . . ? C44 C41 C42 C43 177.5(5) . . . . ? C41 C42 C43 C38 -0.7(8) . . . . ? C39 C38 C43 C42 -0.9(7) . . . . ? C34 C38 C43 C42 176.8(5) . . . . ? Cu2 O6 C44 O7 -0.7(7) 1_554 . . . ? Cu2 O6 C44 C41 179.2(3) 1_554 . . . ? Cu1 O7 C44 O6 3.2(8) 1_554 . . . ? Cu1 O7 C44 C41 -176.6(3) 1_554 . . . ? C42 C41 C44 O6 160.6(5) . . . . ? C40 C41 C44 O6 -22.6(7) . . . . ? C42 C41 C44 O7 -19.6(7) . . . . ? C40 C41 C44 O7 157.3(5) . . . . ? C31 C36 C45 C11 89.1(5) . . . . ? C35 C36 C45 C11 -87.9(5) . . . . ? C12 C11 C45 C36 84.9(5) . . . . ? C10 C11 C45 C36 -90.7(5) . . . . ? O6 Cu2 O10 C46B -135.51(11) 1_556 . . . ? O6 Cu2 O10 C46B 135.50(10) 13_656 . . . ? O5 Cu2 O10 C46B -43.90(11) . . . . ? O5 Cu2 O10 C46B 43.90(11) 13_655 . . . ? O6 Cu2 O10 C46A 71.8(12) 1_556 . . 13_655 ? O6 Cu2 O10 C46A -17.2(12) 13_656 . . 13_655 ? O5 Cu2 O10 C46A 163.4(12) . . . 13_655 ? O5 Cu2 O10 C46A -108.8(12) 13_655 . . 13_655 ? O6 Cu2 O10 C46A 17.2(12) 1_556 . . . ? O6 Cu2 O10 C46A -71.8(12) 13_656 . . . ? O5 Cu2 O10 C46A 108.8(12) . . . . ? O5 Cu2 O10 C46A -163.4(12) 13_655 . . . ? C46B O10 C46A C47A 9(6) . . . . ? C46A O10 C46A C47A 112(5) 13_655 . . . ? Cu2 O10 C46A C47A -146(5) . . . . ? C46A O10 C46B C47B -146(5) 13_655 . . . ? C46A O10 C46B C47B -91(6) . . . . ? Cu2 O10 C46B C47B 62(6) . . . . ? C46A O10 C46B C47B 91(6) 13_655 . . 13_655 ? C46A O10 C46B C47B 146(5) . . . 13_655 ? Cu2 O10 C46B C47B -62(6) . . . 13_655 ? O8 Cu3 N1 C48 -73.3(18) . . . 15_575 ? O8 Cu3 N1 C48 109.4(18) 15_575 . . 15_575 ? N2 Cu3 N1 C48 85(2) . . . 15_575 ? O12 Cu3 N1 C48 -162.3(18) . . . 15_575 ? O8 Cu3 N1 C48 -41.5(11) . . . . ? O8 Cu3 N1 C48 141.2(11) 15_575 . . . ? N2 Cu3 N1 C48 117.2(17) . . . . ? O12 Cu3 N1 C48 -130.6(10) . . . . ? O8 Cu3 N1 C52 136.9(10) . . . . ? O8 Cu3 N1 C52 -40.4(10) 15_575 . . . ? N2 Cu3 N1 C52 -64.4(19) . . . . ? O12 Cu3 N1 C52 47.8(10) . . . . ? Cu3 N1 C52 C48 160.9(15) . . . 15_575 ? O8 Cu3 N2 C53 69(2) . . . 15_575 ? O8 Cu3 N2 C53 -113(2) 15_575 . . 15_575 ? N2 Cu3 N2 C53 68(2) 15_575 . . 15_575 ? N1 Cu3 N2 C53 -89(3) . . . 15_575 ? O12 Cu3 N2 C53 159(2) . . . 15_575 ? O8 Cu3 N2 C53 66.9(12) . . . . ? O8 Cu3 N2 C53 -116.0(12) 15_575 . . . ? N1 Cu3 N2 C53 -92.0(19) . . . . ? O12 Cu3 N2 C53 156.4(11) . . . . ? O8 Cu3 N2 C57 -121.2(12) . . . . ? O8 Cu3 N2 C57 56.0(12) 15_575 . . . ? N1 Cu3 N2 C57 80.0(18) . . . . ? O12 Cu3 N2 C57 -31.6(13) . . . . ? O8 Cu3 N2 C57 -33.8(9) . . . 15_575 ? O8 Cu3 N2 C57 143.4(9) 15_575 . . 15_575 ? O12 Cu3 N2 C57 55.8(9) . . . 15_575 ? C57 N2 C53 C54 -78.9(7) 15_575 . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.87 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.637 _refine_diff_density_min -0.608 _refine_diff_density_rms 0.107 # 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 -0.017 0.195 0.920 12265 1288 ' ' 2 0.028 0.158 0.341 10 0 ' ' 3 0.028 0.342 0.341 10 1 ' ' 4 0.158 0.029 0.841 10 0 ' ' 5 0.158 0.471 0.841 10 -1 ' ' 6 0.341 0.028 0.841 10 1 ' ' 7 0.342 0.471 0.841 10 0 ' ' 8 0.471 0.158 0.341 10 0 ' ' 9 0.471 0.342 0.341 10 0 ' ' 10 0.528 0.658 0.659 10 0 ' ' 11 0.528 0.842 0.659 10 1 ' ' 12 0.658 0.529 0.159 10 0 ' ' 13 0.658 0.971 0.159 10 0 ' ' 14 0.842 0.529 0.159 10 1 ' ' 15 0.842 0.971 0.159 10 0 ' ' 16 0.971 0.658 0.659 10 0 ' ' 17 0.971 0.842 0.659 10 0 ' ' _platon_squeeze_details ; ;