# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Hongjie Zhang' _publ_contact_author_email HONGJIE@CIAC.JL.CN _publ_section_title ; Three-dimensional metal-organic framework with two kinds of channels and high carbon dioxide uptake ; loop_ _publ_author_name 'Hongjie Zhang' 'Huadong Guo' 'Zhiyong Guo' 'Guanghua Li' 'Zhenjun Si' ; Jiangbo Yu ; # Attachment 'CIF1.cif' data_sad _database_code_depnum_ccdc_archive 'CCDC 721250' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C61 H59 Cu3 N7 O19 S3' _chemical_formula_sum 'C61 H59 Cu3 N7 O19 S3' _chemical_formula_weight 1480.95 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a _symmetry_space_group_name_Hall -I4ad loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 29.3618(6) _cell_length_b 29.3618(6) _cell_length_c 37.1534(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 32030.5(15) _cell_formula_units_Z 16 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 15733 _cell_measurement_theta_min 1.39 _cell_measurement_theta_max 26.05 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12176 _exptl_absorpt_coefficient_mu 0.931 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7384 _exptl_absorpt_correction_T_max 0.7957 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 89662 _diffrn_reflns_av_R_equivalents 0.0757 _diffrn_reflns_av_sigmaI/netI 0.0646 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 26.05 _reflns_number_total 15773 _reflns_number_gt 8900 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _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. To keep anisotropic thermal parameters of some atoms within reasonable limits the displacement components were restrained using ISOR shelxl instruction. To keep anisotropic thermal parameters of some coplanar or conjoint atoms within the same level were restrained using EADP shelxl instruction. ; _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^)+(0.1672P)^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 15773 _refine_ls_number_parameters 577 _refine_ls_number_restraints 96 _refine_ls_R_factor_all 0.1313 _refine_ls_R_factor_gt 0.0938 _refine_ls_wR_factor_ref 0.2743 _refine_ls_wR_factor_gt 0.2542 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.027 _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 0.719616(19) 0.50611(2) 0.103152(16) 0.0415(2) Uani 1 1 d . . . Cu2 Cu 0.78884(2) 0.50160(2) 0.149316(18) 0.0475(2) Uani 1 1 d . . . Cu3 Cu 0.53707(2) 0.72299(3) 0.372156(19) 0.0618(3) Uani 1 1 d . . . O1 O 0.68342(11) 0.51394(13) 0.14740(9) 0.0518(9) Uani 1 1 d . . . O2 O 0.74162(12) 0.51413(13) 0.18608(10) 0.0551(9) Uani 1 1 d . . . O3 O 0.50005(15) 0.68972(16) 0.33642(13) 0.0800(13) Uani 1 1 d . . . O4 O 0.44171(15) 0.73834(17) 0.33317(14) 0.0875(15) Uani 1 1 d . . . O5 O 0.32105(12) 0.51492(14) 0.14488(11) 0.0624(11) Uani 1 1 d . . . O6 O 0.31738(14) 0.45511(14) 0.10742(11) 0.0642(11) Uani 1 1 d . . . O7 O 0.82450(12) 0.49163(15) 0.10495(11) 0.0624(11) Uani 1 1 d . . . O8 O 0.76575(13) 0.49757(15) 0.06623(11) 0.0690(11) Uani 1 1 d . . . O9 O 0.99483(19) 0.30979(18) -0.08954(14) 0.0985(16) Uani 1 1 d U . . O10 O 1.05966(18) 0.27128(19) -0.09495(14) 0.0972(16) Uani 1 1 d U . . O11 O 1.18675(12) 0.47823(13) 0.10104(10) 0.0578(10) Uani 1 1 d . . . O12 O 1.18972(12) 0.53463(14) 0.14146(10) 0.0584(10) Uani 1 1 d . . . O13 O 0.66414(17) 0.51096(18) 0.06605(14) 0.0937(10) Uani 1 1 d . . . O14 O 0.84427(18) 0.49409(17) 0.18601(14) 0.0937(10) Uani 1 1 d U . . N1 N 0.52536(16) 0.52056(19) 0.19571(13) 0.0689(14) Uani 1 1 d . . . N2 N 0.51896(17) 0.5781(2) 0.23966(14) 0.0777(16) Uani 1 1 d . . . N3 N 0.45583(17) 0.5584(2) 0.20513(17) 0.0825(17) Uani 1 1 d . . . N4 N 0.97986(15) 0.4778(2) 0.05286(14) 0.0715(15) Uani 1 1 d . . . N5 N 0.98388(17) 0.4289(2) 0.00178(16) 0.092(2) Uani 1 1 d . . . N6 N 1.0513(2) 0.4490(2) 0.03413(17) 0.0861(17) Uani 1 1 d U . . N7 N 0.59901(18) 0.68365(18) 0.37348(14) 0.0657(14) Uani 1 1 d . . . C1 C 0.54349(19) 0.5472(2) 0.22131(18) 0.0684(17) Uani 1 1 d . . . C2 C 0.4768(2) 0.5833(3) 0.2298(2) 0.079(2) Uani 1 1 d . . . C3 C 0.4815(2) 0.5272(2) 0.18948(17) 0.0699(17) Uani 1 1 d . . . C4 C 0.5926(2) 0.5443(2) 0.22908(19) 0.0786(7) Uani 1 1 d . . . C5 C 0.6224(2) 0.5312(2) 0.20163(19) 0.0786(7) Uani 1 1 d . . . H5 H 0.6110 0.5232 0.1791 0.110 Uiso 1 1 calc . . . C6 C 0.6688(2) 0.5300(2) 0.20784(19) 0.0786(7) Uani 1 1 d . . . C7 C 0.6849(2) 0.5415(2) 0.24243(19) 0.0786(7) Uani 1 1 d . . . H7 H 0.7159 0.5397 0.2474 0.110 Uiso 1 1 calc . . . C8 C 0.6554(2) 0.5554(2) 0.26879(19) 0.0786(7) Uani 1 1 d . . . H8 H 0.6663 0.5636 0.2914 0.110 Uiso 1 1 calc . . . C9 C 0.6100(2) 0.5571(2) 0.26162(18) 0.0786(7) Uani 1 1 d . . . H9 H 0.5902 0.5674 0.2794 0.110 Uiso 1 1 calc . . . C10 C 0.70107(17) 0.51792(15) 0.17821(14) 0.0418(11) Uani 1 1 d . . . C11 C 0.4499(3) 0.6201(3) 0.2479(2) 0.093(2) Uani 1 1 d U . . C12 C 0.4674(2) 0.6427(2) 0.2768(2) 0.080(2) Uani 1 1 d . . . H12 H 0.4957 0.6345 0.2859 0.110 Uiso 1 1 calc . . . C13 C 0.4434(3) 0.6772(3) 0.2924(2) 0.084(2) Uani 1 1 d U . . C14 C 0.4014(2) 0.6915(2) 0.27743(18) 0.0786(7) Uani 1 1 d . . . H14 H 0.3859 0.7161 0.2873 0.110 Uiso 1 1 calc . . . C15 C 0.3843(2) 0.6697(2) 0.24936(19) 0.0786(7) Uani 1 1 d . . . H15 H 0.3556 0.6774 0.2408 0.110 Uiso 1 1 calc . . . C16 C 0.4089(2) 0.6355(2) 0.23268(19) 0.0786(7) Uani 1 1 d . . . H16 H 0.3983 0.6228 0.2113 0.110 Uiso 1 1 calc . . . C17 C 0.4632(2) 0.7035(2) 0.32366(18) 0.0708(18) Uani 1 1 d . . . C18 C 0.4586(2) 0.4973(2) 0.16237(17) 0.0699(17) Uani 1 1 d . . . C19 C 0.4128(2) 0.5024(2) 0.15690(16) 0.0622(16) Uani 1 1 d . . . H19 H 0.3973 0.5249 0.1696 0.110 Uiso 1 1 calc . . . C20 C 0.3886(2) 0.4748(2) 0.13273(18) 0.0668(17) Uani 1 1 d . . . C21 C 0.4121(3) 0.4422(3) 0.1139(2) 0.084(2) Uani 1 1 d U . . H21 H 0.3967 0.4235 0.0978 0.110 Uiso 1 1 calc . . . C22 C 0.4596(4) 0.4367(3) 0.1189(2) 0.111(3) Uani 1 1 d U . . H22 H 0.4755 0.4152 0.1054 0.110 Uiso 1 1 calc . . . C23 C 0.4819(2) 0.4633(3) 0.1437(2) 0.104(3) Uani 1 1 d . . . H23 H 0.5127 0.4586 0.1480 0.110 Uiso 1 1 calc . . . C24 C 0.3386(2) 0.4821(2) 0.12760(17) 0.0593(15) Uani 1 1 d . . . C25 C 0.96130(19) 0.4551(2) 0.02631(17) 0.0664(17) Uani 1 1 d . . . C26 C 1.0295(3) 0.4291(3) 0.0070(2) 0.088(2) Uani 1 1 d U . . C27 C 1.0246(2) 0.4733(2) 0.05620(18) 0.0737(19) Uani 1 1 d . . . C28 C 0.9114(3) 0.4578(3) 0.0205(2) 0.0902(6) Uani 1 1 d . . . C29 C 0.8848(3) 0.4733(3) 0.0488(2) 0.0902(6) Uani 1 1 d . . . H29 H 0.8978 0.4797 0.0711 0.110 Uiso 1 1 calc . . . C30 C 0.8369(3) 0.4795(3) 0.0431(2) 0.0902(6) Uani 1 1 d . . . C31 C 0.8191(3) 0.4710(3) 0.0091(2) 0.0902(6) Uani 1 1 d . . . H31 H 0.7881 0.4750 0.0052 0.110 Uiso 1 1 calc . . . C32 C 0.8464(3) 0.4567(3) -0.0191(2) 0.0902(6) Uani 1 1 d . . . H32 H 0.8339 0.4520 -0.0418 0.110 Uiso 1 1 calc . . . C33 C 0.8940(3) 0.4492(3) -0.0130(2) 0.0902(6) Uani 1 1 d . . . H33 H 0.9127 0.4388 -0.0314 0.110 Uiso 1 1 calc . . . C34 C 0.80719(18) 0.48976(19) 0.07350(17) 0.0562(14) Uani 1 1 d . . . C35 C 1.0559(3) 0.4013(3) -0.0173(2) 0.0902(6) Uani 1 1 d . . . C36 C 1.0354(3) 0.3675(3) -0.0391(2) 0.0902(6) Uani 1 1 d . . . H36 H 1.0040 0.3639 -0.0377 0.110 Uiso 1 1 calc . . . C37 C 1.0589(3) 0.3401(3) -0.0620(2) 0.0902(6) Uani 1 1 d . . . C38 C 1.1089(3) 0.3468(3) -0.0638(2) 0.0902(6) Uani 1 1 d . . . H38 H 1.1265 0.3269 -0.0774 0.110 Uiso 1 1 calc . . . C39 C 1.1300(3) 0.3827(3) -0.0452(2) 0.0902(6) Uani 1 1 d . . . H39 H 1.1607 0.3890 -0.0489 0.110 Uiso 1 1 calc . . . C40 C 1.1045(3) 0.4090(3) -0.0209(2) 0.0902(6) Uani 1 1 d . . . H40 H 1.1187 0.4313 -0.0072 0.110 Uiso 1 1 calc . . . C41 C 1.0372(3) 0.3042(3) -0.0835(2) 0.0902(6) Uani 1 1 d U . . C42 C 1.0485(2) 0.5004(3) 0.08413(18) 0.0766(19) Uani 1 1 d . . . C43 C 1.09483(19) 0.4920(2) 0.09027(17) 0.0664(16) Uani 1 1 d . . . H43 H 1.1093 0.4682 0.0783 0.110 Uiso 1 1 calc . . . C44 C 1.11913(19) 0.5189(2) 0.11414(17) 0.0647(16) Uani 1 1 d . . . C45 C 1.0968(2) 0.5552(3) 0.13244(18) 0.0734(19) Uani 1 1 d . . . H45 H 1.1133 0.5734 0.1483 0.110 Uiso 1 1 calc . . . C46 C 1.0514(3) 0.5639(3) 0.1269(2) 0.095(2) Uani 1 1 d U . . H46 H 1.0372 0.5875 0.1392 0.110 Uiso 1 1 calc . . . C47 C 1.0258(2) 0.5364(3) 0.1021(2) 0.097(3) Uani 1 1 d . . . H47 H 0.9951 0.5421 0.0979 0.110 Uiso 1 1 calc . . . C48 C 1.1684(2) 0.5102(2) 0.11991(15) 0.0571(15) Uani 1 1 d . . . C49 C 0.6236(3) 0.6800(3) 0.3447(2) 0.098(2) Uani 1 1 d U . . H49 H 0.6117 0.6919 0.3235 0.110 Uiso 1 1 calc . . . C50 C 0.6674(3) 0.6591(3) 0.3428(3) 0.110(3) Uani 1 1 d U . . H50 H 0.6844 0.6568 0.3217 0.110 Uiso 1 1 calc . . . C51 C 0.6821(3) 0.6425(3) 0.3760(2) 0.110(3) Uani 1 1 d U . . H51 H 0.7100 0.6275 0.3766 0.110 Uiso 1 1 calc . . . C52 C 0.6600(3) 0.6462(3) 0.4058(2) 0.100(2) Uani 1 1 d U . . H52 H 0.6716 0.6353 0.4275 0.110 Uiso 1 1 calc . . . C53 C 0.6161(3) 0.6682(3) 0.4036(3) 0.108(3) Uani 1 1 d U . . H53 H 0.5993 0.6717 0.4246 0.110 Uiso 1 1 calc . . . C54 C 0.6533(3) 0.5478(3) 0.0413(2) 0.0937(10) Uani 1 1 d . . . H54A H 0.6261 0.5404 0.0282 0.110 Uiso 1 1 calc . . . H54B H 0.6780 0.5520 0.0248 0.110 Uiso 1 1 calc . . . H54C H 0.6485 0.5754 0.0547 0.110 Uiso 1 1 calc . . . C55 C 0.8871(5) 0.5274(5) 0.1755(4) 0.0937(10) Uani 0.50 1 d P . . H55A H 0.8859 0.5343 0.1502 0.110 Uiso 0.50 1 calc P . . H55B H 0.9152 0.5122 0.1809 0.110 Uiso 0.50 1 calc P . . H55C H 0.8852 0.5551 0.1891 0.110 Uiso 0.50 1 calc P . . C55' C 0.8389(5) 0.4801(5) 0.2223(4) 0.0937(10) Uani 0.50 1 d P . . H55D H 0.8127 0.4607 0.2242 0.110 Uiso 0.50 1 calc P . . H55E H 0.8347 0.5064 0.2373 0.110 Uiso 0.50 1 calc P . . H55F H 0.8655 0.4638 0.2299 0.110 Uiso 0.50 1 calc P . . 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 0.0354(3) 0.0376(3) 0.0514(4) 0.0005(3) -0.0067(3) 0.0024(2) Cu2 0.0388(4) 0.0479(4) 0.0557(4) -0.0002(3) -0.0077(3) 0.0063(3) Cu3 0.0486(4) 0.0738(5) 0.0631(5) 0.0068(4) 0.0000(3) 0.0154(4) O1 0.0378(19) 0.065(2) 0.052(2) -0.0160(18) -0.0026(17) -0.0002(16) O2 0.040(2) 0.065(2) 0.060(2) -0.0027(19) -0.0059(18) 0.0060(17) O3 0.068(3) 0.083(3) 0.088(3) -0.014(3) -0.010(3) 0.023(2) O4 0.064(3) 0.098(4) 0.100(3) -0.033(3) -0.021(3) 0.026(3) O5 0.038(2) 0.060(2) 0.089(3) -0.014(2) -0.009(2) 0.0071(18) O6 0.053(2) 0.067(3) 0.072(3) -0.017(2) -0.009(2) 0.005(2) O7 0.038(2) 0.089(3) 0.060(2) -0.010(2) -0.0013(19) 0.0006(19) O8 0.046(2) 0.099(3) 0.062(2) -0.004(2) 0.0020(19) 0.004(2) O9 0.0971(18) 0.0999(18) 0.0985(18) -0.0037(10) -0.0007(10) 0.0017(10) O10 0.0960(18) 0.0977(18) 0.0978(18) -0.0036(10) -0.0006(10) 0.0023(10) O11 0.046(2) 0.063(2) 0.064(2) -0.012(2) -0.0054(18) -0.0129(18) O12 0.036(2) 0.085(3) 0.054(2) -0.011(2) 0.0010(17) -0.0085(19) O13 0.0934(12) 0.0947(12) 0.0931(12) 0.0009(9) -0.0086(9) 0.0022(9) O14 0.0934(12) 0.0947(12) 0.0931(12) 0.0009(9) -0.0086(9) 0.0022(9) N1 0.047(3) 0.104(4) 0.056(3) -0.018(3) -0.006(2) 0.016(3) N2 0.055(3) 0.108(4) 0.070(3) -0.042(3) -0.007(3) 0.016(3) N3 0.045(3) 0.100(4) 0.103(4) -0.032(4) -0.008(3) 0.008(3) N4 0.040(3) 0.103(4) 0.071(3) -0.023(3) -0.001(2) -0.013(3) N5 0.037(3) 0.145(6) 0.093(4) -0.050(4) -0.009(3) 0.002(3) N6 0.0843(19) 0.0875(19) 0.0866(19) -0.0026(10) -0.0003(10) -0.0002(10) N7 0.056(3) 0.070(3) 0.071(3) 0.007(3) -0.006(3) 0.005(2) C1 0.042(3) 0.089(5) 0.074(4) -0.009(4) 0.001(3) 0.014(3) C2 0.040(3) 0.105(5) 0.091(5) -0.036(4) -0.005(3) 0.025(3) C3 0.041(3) 0.093(5) 0.075(4) -0.021(4) 0.005(3) 0.010(3) C4 0.0600(13) 0.0945(17) 0.0811(16) -0.0272(13) -0.0182(11) 0.0222(12) C5 0.0600(13) 0.0945(17) 0.0811(16) -0.0272(13) -0.0182(11) 0.0222(12) C6 0.0600(13) 0.0945(17) 0.0811(16) -0.0272(13) -0.0182(11) 0.0222(12) C7 0.0600(13) 0.0945(17) 0.0811(16) -0.0272(13) -0.0182(11) 0.0222(12) C8 0.0600(13) 0.0945(17) 0.0811(16) -0.0272(13) -0.0182(11) 0.0222(12) C9 0.0600(13) 0.0945(17) 0.0811(16) -0.0272(13) -0.0182(11) 0.0222(12) C10 0.045(3) 0.032(2) 0.049(3) -0.007(2) -0.004(2) -0.001(2) C11 0.092(2) 0.094(2) 0.094(2) -0.0017(10) -0.0004(10) 0.0005(10) C12 0.049(4) 0.095(5) 0.095(5) -0.035(4) -0.007(3) 0.012(3) C13 0.083(2) 0.084(2) 0.084(2) -0.0011(10) -0.0005(10) 0.0013(10) C14 0.0600(13) 0.0945(17) 0.0811(16) -0.0272(13) -0.0182(11) 0.0222(12) C15 0.0600(13) 0.0945(17) 0.0811(16) -0.0272(13) -0.0182(11) 0.0222(12) C16 0.0600(13) 0.0945(17) 0.0811(16) -0.0272(13) -0.0182(11) 0.0222(12) C17 0.052(4) 0.085(5) 0.075(4) -0.023(4) 0.008(3) 0.013(3) C18 0.051(4) 0.088(5) 0.070(4) -0.016(4) -0.002(3) 0.004(3) C19 0.049(3) 0.075(4) 0.063(4) -0.015(3) -0.001(3) 0.016(3) C20 0.042(3) 0.070(4) 0.088(4) -0.019(3) -0.007(3) 0.011(3) C21 0.083(2) 0.084(2) 0.085(2) -0.0019(10) -0.0010(10) 0.0008(10) C22 0.110(3) 0.111(3) 0.111(3) -0.0017(10) -0.0002(10) 0.0012(10) C23 0.058(4) 0.127(7) 0.128(7) -0.065(6) -0.020(4) 0.033(4) C24 0.044(3) 0.056(4) 0.078(4) 0.005(3) -0.001(3) 0.004(3) C25 0.041(3) 0.084(4) 0.074(4) -0.020(4) 0.013(3) 0.000(3) C26 0.087(2) 0.088(2) 0.088(2) -0.0019(10) 0.0002(10) 0.0004(10) C27 0.043(3) 0.103(5) 0.076(4) -0.032(4) 0.007(3) -0.014(3) C28 0.0822(9) 0.0969(10) 0.0915(10) -0.0107(8) 0.0012(8) 0.0005(8) C29 0.0822(9) 0.0969(10) 0.0915(10) -0.0107(8) 0.0012(8) 0.0005(8) C30 0.0822(9) 0.0969(10) 0.0915(10) -0.0107(8) 0.0012(8) 0.0005(8) C31 0.0822(9) 0.0969(10) 0.0915(10) -0.0107(8) 0.0012(8) 0.0005(8) C32 0.0822(9) 0.0969(10) 0.0915(10) -0.0107(8) 0.0012(8) 0.0005(8) C33 0.0822(9) 0.0969(10) 0.0915(10) -0.0107(8) 0.0012(8) 0.0005(8) C34 0.037(3) 0.059(4) 0.072(4) -0.016(3) 0.000(3) 0.003(2) C35 0.0822(9) 0.0969(10) 0.0915(10) -0.0107(8) 0.0012(8) 0.0005(8) C36 0.0822(9) 0.0969(10) 0.0915(10) -0.0107(8) 0.0012(8) 0.0005(8) C37 0.0822(9) 0.0969(10) 0.0915(10) -0.0107(8) 0.0012(8) 0.0005(8) C38 0.0822(9) 0.0969(10) 0.0915(10) -0.0107(8) 0.0012(8) 0.0005(8) C39 0.0822(9) 0.0969(10) 0.0915(10) -0.0107(8) 0.0012(8) 0.0005(8) C40 0.0822(9) 0.0969(10) 0.0915(10) -0.0107(8) 0.0012(8) 0.0005(8) C41 0.0822(9) 0.0969(10) 0.0915(10) -0.0107(8) 0.0012(8) 0.0005(8) C42 0.047(4) 0.114(6) 0.069(4) -0.014(4) 0.007(3) -0.003(3) C43 0.042(3) 0.089(5) 0.068(4) -0.013(3) -0.002(3) -0.011(3) C44 0.041(3) 0.083(4) 0.070(4) -0.012(3) -0.002(3) -0.010(3) C45 0.052(4) 0.083(5) 0.086(5) -0.027(4) -0.004(3) 0.003(3) C46 0.095(3) 0.095(3) 0.096(3) -0.0012(10) -0.0002(10) 0.0003(10) C47 0.049(4) 0.127(7) 0.115(6) -0.043(5) -0.014(4) 0.014(4) C48 0.051(3) 0.067(4) 0.054(3) -0.001(3) 0.008(3) -0.014(3) C49 0.098(3) 0.098(3) 0.099(3) -0.0002(10) -0.0002(10) 0.0011(10) C50 0.110(3) 0.110(3) 0.111(3) -0.0004(10) 0.0004(10) 0.0003(10) C51 0.110(3) 0.110(3) 0.111(3) -0.0003(10) -0.0008(10) 0.0005(10) C52 0.100(3) 0.100(3) 0.100(3) 0.0011(10) -0.0013(10) 0.0004(10) C53 0.107(3) 0.108(3) 0.108(3) 0.0002(10) -0.0006(10) 0.0008(10) C54 0.0934(12) 0.0947(12) 0.0931(12) 0.0009(9) -0.0086(9) 0.0022(9) C55 0.0934(12) 0.0947(12) 0.0931(12) 0.0009(9) -0.0086(9) 0.0022(9) C55' 0.0934(12) 0.0947(12) 0.0931(12) 0.0009(9) -0.0086(9) 0.0022(9) _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 O8 1.944(4) . ? Cu1 O5 1.961(4) 12_766 ? Cu1 O12 1.963(4) 12_756 ? Cu1 O1 1.971(3) . ? Cu1 O13 2.139(5) . ? Cu1 Cu2 2.6627(9) . ? Cu2 O6 1.956(4) 12_766 ? Cu2 O11 1.969(4) 12_756 ? Cu2 O7 1.975(4) . ? Cu2 O2 1.981(4) . ? Cu2 O14 2.135(5) . ? Cu3 O4 1.943(5) 6_564 ? Cu3 O9 1.957(5) 2_665 ? Cu3 O3 1.975(5) . ? Cu3 O10 1.986(6) 5_455 ? Cu3 N7 2.155(5) . ? Cu3 Cu3 2.6931(14) 6_564 ? O1 C10 1.262(6) . ? O2 C10 1.231(6) . ? O3 C17 1.248(7) . ? O4 C17 1.253(7) . ? O4 Cu3 1.943(5) 6_564 ? O5 C24 1.268(7) . ? O5 Cu1 1.961(4) 15_565 ? O6 C24 1.257(7) . ? O6 Cu2 1.956(4) 15_565 ? O7 C34 1.276(7) . ? O8 C34 1.267(6) . ? O9 C41 1.273(9) . ? O9 Cu3 1.957(5) 2_664 ? O10 C41 1.246(8) . ? O10 Cu3 1.986(5) 5_544 ? O11 C48 1.290(7) . ? O11 Cu2 1.969(4) 15_665 ? O12 C48 1.244(7) . ? O12 Cu1 1.963(4) 15_665 ? O13 C54 1.454(9) . ? O14 C55' 1.418(16) . ? O14 C55 1.640(17) . ? N1 C3 1.324(7) . ? N1 C1 1.341(8) . ? N2 C2 1.299(7) . ? N2 C1 1.345(7) . ? N3 C3 1.319(7) . ? N3 C2 1.324(8) . ? N4 C25 1.309(7) . ? N4 C27 1.325(7) . ? N5 C26 1.354(9) . ? N5 C25 1.365(7) . ? N6 C26 1.329(9) . ? N6 C27 1.340(8) . ? N7 C49 1.295(9) . ? N7 C53 1.306(10) . ? C1 C4 1.472(8) . ? C2 C11 1.500(9) . ? C3 C18 1.496(9) . ? C4 C9 1.366(9) . ? C4 C5 1.398(9) . ? C5 C6 1.383(8) . ? C5 H5 0.9300 . ? C6 C7 1.410(9) . ? C6 C10 1.495(8) . ? C7 C8 1.370(9) . ? C7 H7 0.9300 . ? C8 C9 1.359(8) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C11 C12 1.361(10) . ? C11 C16 1.405(9) . ? C12 C13 1.362(9) . ? C12 H12 0.9300 . ? C13 C14 1.417(9) . ? C13 C17 1.513(9) . ? C14 C15 1.323(8) . ? C14 H14 0.9300 . ? C15 C16 1.382(8) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C18 C19 1.366(8) . ? C18 C23 1.397(9) . ? C19 C20 1.404(8) . ? C19 H19 0.9300 . ? C20 C21 1.372(9) . ? C20 C24 1.496(8) . ? C21 C22 1.415(12) . ? C21 H21 0.9300 . ? C22 C23 1.374(11) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C25 C28 1.483(9) . ? C26 C35 1.443(10) . ? C27 C42 1.484(8) . ? C28 C33 1.367(10) . ? C28 C29 1.389(10) . ? C29 C30 1.434(10) . ? C29 H29 0.9300 . ? C30 C31 1.389(10) . ? C30 C34 1.457(9) . ? C31 C32 1.383(10) . ? C31 H31 0.9300 . ? C32 C33 1.434(10) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C35 C36 1.415(10) . ? C35 C40 1.449(10) . ? C36 C37 1.358(10) . ? C36 H36 0.9300 . ? C37 C41 1.470(10) . ? C37 C38 1.484(10) . ? C38 C39 1.404(10) . ? C38 H38 0.9300 . ? C39 C40 1.404(10) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C42 C43 1.402(8) . ? C42 C47 1.415(10) . ? C43 C44 1.386(8) . ? C43 H43 0.9300 . ? C44 C45 1.425(9) . ? C44 C48 1.484(8) . ? C45 C46 1.374(10) . ? C45 H45 0.9300 . ? C46 C47 1.439(10) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? C49 C50 1.428(11) . ? C49 H49 0.9300 . ? C50 C51 1.393(11) . ? C50 H50 0.9300 . ? C51 C52 1.289(11) . ? C51 H51 0.9300 . ? C52 C53 1.443(12) . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C55' H55D 0.9600 . ? C55' H55E 0.9600 . ? C55' H55F 0.9600 . ? 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 O8 Cu1 O5 89.45(18) . 12_766 ? O8 Cu1 O12 89.32(18) . 12_756 ? O5 Cu1 O12 167.42(17) 12_766 12_756 ? O8 Cu1 O1 168.31(15) . . ? O5 Cu1 O1 88.87(17) 12_766 . ? O12 Cu1 O1 89.81(16) 12_756 . ? O8 Cu1 O13 94.85(18) . . ? O5 Cu1 O13 97.79(18) 12_766 . ? O12 Cu1 O13 94.79(18) 12_756 . ? O1 Cu1 O13 96.85(17) . . ? O8 Cu1 Cu2 85.19(12) . . ? O5 Cu1 Cu2 81.24(12) 12_766 . ? O12 Cu1 Cu2 86.18(12) 12_756 . ? O1 Cu1 Cu2 83.11(10) . . ? O13 Cu1 Cu2 179.03(14) . . ? O6 Cu2 O11 167.78(16) 12_766 12_756 ? O6 Cu2 O7 89.51(18) 12_766 . ? O11 Cu2 O7 89.19(17) 12_756 . ? O6 Cu2 O2 88.19(17) 12_766 . ? O11 Cu2 O2 90.36(16) 12_756 . ? O7 Cu2 O2 167.00(15) . . ? O6 Cu2 O14 96.57(18) 12_766 . ? O11 Cu2 O14 95.65(17) 12_756 . ? O7 Cu2 O14 96.52(18) . . ? O2 Cu2 O14 96.46(18) . . ? O6 Cu2 Cu1 86.43(12) 12_766 . ? O11 Cu2 Cu1 81.35(11) 12_756 . ? O7 Cu2 Cu1 82.79(11) . . ? O2 Cu2 Cu1 84.30(10) . . ? O14 Cu2 Cu1 176.92(14) . . ? O4 Cu3 O9 169.4(2) 6_564 2_665 ? O4 Cu3 O3 88.0(2) 6_564 . ? O9 Cu3 O3 89.0(2) 2_665 . ? O4 Cu3 O10 86.2(2) 6_564 5_455 ? O9 Cu3 O10 93.6(2) 2_665 5_455 ? O3 Cu3 O10 162.0(2) . 5_455 ? O4 Cu3 N7 93.42(19) 6_564 . ? O9 Cu3 N7 97.1(2) 2_665 . ? O3 Cu3 N7 102.40(19) . . ? O10 Cu3 N7 95.0(2) 5_455 . ? O4 Cu3 Cu3 85.13(13) 6_564 6_564 ? O9 Cu3 Cu3 84.42(16) 2_665 6_564 ? O3 Cu3 Cu3 81.17(13) . 6_564 ? O10 Cu3 Cu3 81.35(16) 5_455 6_564 ? N7 Cu3 Cu3 176.12(16) . 6_564 ? C10 O1 Cu1 123.1(3) . . ? C10 O2 Cu2 122.0(3) . . ? C17 O3 Cu3 124.9(4) . . ? C17 O4 Cu3 121.7(4) . 6_564 ? C24 O5 Cu1 126.2(4) . 15_565 ? C24 O6 Cu2 120.6(4) . 15_565 ? C34 O7 Cu2 124.0(3) . . ? C34 O8 Cu1 122.8(4) . . ? C41 O9 Cu3 122.1(5) . 2_664 ? C41 O10 Cu3 125.9(5) . 5_544 ? C48 O11 Cu2 126.4(4) . 15_665 ? C48 O12 Cu1 121.9(4) . 15_665 ? C54 O13 Cu1 128.6(4) . . ? C55' O14 C55 119.0(9) . . ? C55' O14 Cu2 123.5(7) . . ? C55 O14 Cu2 111.7(6) . . ? C3 N1 C1 115.1(5) . . ? C2 N2 C1 116.4(5) . . ? C3 N3 C2 115.0(5) . . ? C25 N4 C27 115.6(5) . . ? C26 N5 C25 112.5(6) . . ? C26 N6 C27 114.7(6) . . ? C49 N7 C53 117.6(7) . . ? C49 N7 Cu3 119.7(5) . . ? C53 N7 Cu3 122.0(5) . . ? N1 C1 N2 122.7(5) . . ? N1 C1 C4 119.6(5) . . ? N2 C1 C4 117.6(6) . . ? N2 C2 N3 125.1(6) . . ? N2 C2 C11 117.4(6) . . ? N3 C2 C11 117.6(6) . . ? N3 C3 N1 125.5(6) . . ? N3 C3 C18 116.6(5) . . ? N1 C3 C18 117.9(5) . . ? C9 C4 C5 119.2(6) . . ? C9 C4 C1 121.6(6) . . ? C5 C4 C1 119.0(6) . . ? C6 C5 C4 120.2(6) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C7 118.4(6) . . ? C5 C6 C10 120.5(6) . . ? C7 C6 C10 121.1(6) . . ? C8 C7 C6 120.8(6) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C9 C8 C7 119.4(6) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C8 C9 C4 122.0(6) . . ? C8 C9 H9 119.0 . . ? C4 C9 H9 119.0 . . ? O2 C10 O1 127.2(5) . . ? O2 C10 C6 117.3(5) . . ? O1 C10 C6 115.5(5) . . ? C12 C11 C16 118.9(7) . . ? C12 C11 C2 120.4(7) . . ? C16 C11 C2 120.2(7) . . ? C11 C12 C13 120.1(7) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C12 C13 C14 120.3(7) . . ? C12 C13 C17 120.6(6) . . ? C14 C13 C17 118.9(6) . . ? C15 C14 C13 119.6(6) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 120.5(6) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C11 120.0(6) . . ? C15 C16 H16 120.0 . . ? C11 C16 H16 120.0 . . ? O3 C17 O4 126.5(6) . . ? O3 C17 C13 117.3(6) . . ? O4 C17 C13 116.1(6) . . ? C19 C18 C23 119.1(6) . . ? C19 C18 C3 118.5(5) . . ? C23 C18 C3 122.3(6) . . ? C18 C19 C20 122.0(5) . . ? C18 C19 H19 119.0 . . ? C20 C19 H19 119.0 . . ? C21 C20 C19 118.4(6) . . ? C21 C20 C24 121.9(6) . . ? C19 C20 C24 119.8(5) . . ? C20 C21 C22 120.5(7) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C23 C22 C21 119.5(8) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C22 C23 C18 120.4(7) . . ? C22 C23 H23 119.8 . . ? C18 C23 H23 119.8 . . ? O6 C24 O5 125.4(5) . . ? O6 C24 C20 118.3(5) . . ? O5 C24 C20 116.3(5) . . ? N4 C25 N5 126.0(5) . . ? N4 C25 C28 119.6(5) . . ? N5 C25 C28 114.3(6) . . ? N6 C26 N5 125.9(7) . . ? N6 C26 C35 117.7(7) . . ? N5 C26 C35 116.1(7) . . ? N4 C27 N6 125.1(6) . . ? N4 C27 C42 118.7(6) . . ? N6 C27 C42 115.9(5) . . ? C33 C28 C29 122.6(7) . . ? C33 C28 C25 119.5(7) . . ? C29 C28 C25 117.6(7) . . ? C28 C29 C30 118.9(7) . . ? C28 C29 H29 120.6 . . ? C30 C29 H29 120.6 . . ? C31 C30 C29 118.6(7) . . ? C31 C30 C34 121.2(7) . . ? C29 C30 C34 119.9(7) . . ? C32 C31 C30 121.8(7) . . ? C32 C31 H31 119.1 . . ? C30 C31 H31 119.1 . . ? C31 C32 C33 119.4(7) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? C28 C33 C32 118.6(7) . . ? C28 C33 H33 120.7 . . ? C32 C33 H33 120.7 . . ? O8 C34 O7 124.7(5) . . ? O8 C34 C30 116.5(6) . . ? O7 C34 C30 118.7(5) . . ? C36 C35 C26 121.6(7) . . ? C36 C35 C40 118.4(7) . . ? C26 C35 C40 119.9(7) . . ? C37 C36 C35 123.8(7) . . ? C37 C36 H36 118.1 . . ? C35 C36 H36 118.1 . . ? C36 C37 C41 123.0(7) . . ? C36 C37 C38 117.0(7) . . ? C41 C37 C38 119.9(7) . . ? C39 C38 C37 120.8(7) . . ? C39 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C38 C39 C40 119.5(7) . . ? C38 C39 H39 120.2 . . ? C40 C39 H39 120.2 . . ? C39 C40 C35 120.0(7) . . ? C39 C40 H40 120.0 . . ? C35 C40 H40 120.0 . . ? O10 C41 O9 123.8(8) . . ? O10 C41 C37 120.8(7) . . ? O9 C41 C37 115.3(7) . . ? C43 C42 C47 120.8(6) . . ? C43 C42 C27 118.5(6) . . ? C47 C42 C27 120.5(6) . . ? C44 C43 C42 120.2(6) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C43 C44 C45 119.8(6) . . ? C43 C44 C48 119.7(6) . . ? C45 C44 C48 120.5(5) . . ? C46 C45 C44 120.9(6) . . ? C46 C45 H45 119.5 . . ? C44 C45 H45 119.5 . . ? C45 C46 C47 119.9(7) . . ? C45 C46 H46 120.1 . . ? C47 C46 H46 120.1 . . ? C42 C47 C46 118.4(6) . . ? C42 C47 H47 120.8 . . ? C46 C47 H47 120.8 . . ? O12 C48 O11 124.0(6) . . ? O12 C48 C44 119.0(6) . . ? O11 C48 C44 117.0(5) . . ? N7 C49 C50 125.3(8) . . ? N7 C49 H49 117.3 . . ? C50 C49 H49 117.3 . . ? C51 C50 C49 112.7(9) . . ? C51 C50 H50 123.7 . . ? C49 C50 H50 123.7 . . ? C52 C51 C50 125.1(10) . . ? C52 C51 H51 117.4 . . ? C50 C51 H51 117.4 . . ? C51 C52 C53 115.9(9) . . ? C51 C52 H52 122.0 . . ? C53 C52 H52 122.0 . . ? N7 C53 C52 123.2(8) . . ? N7 C53 H53 118.4 . . ? C52 C53 H53 118.4 . . ? O13 C54 H54A 109.5 . . ? O13 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? O13 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O14 C55 H55A 109.5 . . ? O14 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? O14 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O14 C55' H55D 109.5 . . ? O14 C55' H55E 109.5 . . ? H55D C55' H55E 109.5 . . ? O14 C55' H55F 109.5 . . ? H55D C55' H55F 109.5 . . ? H55E C55' H55F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.399 _refine_diff_density_min -0.950 _refine_diff_density_rms 0.128 # 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 _platon_squeeze_void_content 1 0.451 0.001 -0.001 6208 2287 ' ' _platon_squeeze_details ; ;