# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Krista Walton' _publ_contact_author_email KRISTA.WALTON@CHBE.GATECH.EDU _publ_section_title ; A Metal-Organic Framework with Coordinatively Unsaturated Metal Centers and Nanoporous Structure ; loop_ _publ_author_name 'Krista Walton' 'Yougui Huang.' 'Bin Mu.' # Attachment 'a08p2m.cif' data_c:\cdbtb\a08p2m _database_code_depnum_ccdc_archive 'CCDC 763063' #TrackingRef 'a08p2m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C74 H74 Cd3 N4 O16' _chemical_formula_sum 'C74 H74 Cd3 N4 O16' _chemical_formula_weight 1612.57 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4595(9) _cell_length_b 14.3920(13) _cell_length_c 14.7634(13) _cell_angle_alpha 69.6080(10) _cell_angle_beta 82.4760(10) _cell_angle_gamma 88.0430(10) _cell_volume 2065.0(3) _cell_formula_units_Z 1 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 16890 _cell_measurement_theta_min 2.0236 _cell_measurement_theta_max 27.3565 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 818 _exptl_absorpt_coefficient_mu 0.825 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9003 _exptl_absorpt_correction_T_max 0.9638 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 Mercury CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22830 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.06 _diffrn_reflns_theta_max 30.06 _reflns_number_total 11602 _reflns_number_gt 9303 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku, 2000)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _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. All non-hydrogen atoms were refined with anisotropic temperature parameters. The hydrogen atoms were positioned geometrically and refined using a riding model. The routine SQUEEZE is applied to remove the very diffuse electron density associated with the disordered uncoordinated solvent molecules. For one of the coordinated DEF molecule, the following distance restraints are imposed: C36-C37A C37A-C37B and C37B-C36 1.46(2). The C36 C37A and C37B atoms are also restrained to vibrate in a nearly isotropically within a standard uncertainty of 0.1. C37A and C37B are refined as disordered model with partial occupancies of 0.4 and 0.6, respectively. ; _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^)+(0.0719P)^2^+2.2591P] 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 11602 _refine_ls_number_parameters 497 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0698 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1471 _refine_ls_wR_factor_gt 0.1389 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.052 _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 Cd1 Cd 0.0000 0.0000 0.0000 0.02802(9) Uani 1 2 d S . . Cd2 Cd -0.08541(3) -0.112327(18) -0.188480(18) 0.03565(9) Uani 1 1 d . . . O1 O -0.2426(3) -0.1862(2) -0.0577(2) 0.0479(11) Uani 1.000(12) 1 d . . . O2 O -0.0601(2) -0.14260(18) -0.02315(18) 0.0356(8) Uani 1.000(10) 1 d . . . O3 O -0.1180(3) -0.9073(2) 0.8843(2) 0.0449(10) Uani 1.000(11) 1 d . . . O4 O -0.1099(3) -0.9527(2) 0.7530(2) 0.0563(13) Uani 1.000(12) 1 d . . . O5 O -0.9060(3) -0.1083(2) 0.7003(3) 0.0682(15) Uani 1.000(13) 1 d . . . O6 O -0.9636(3) -0.2519(2) 0.8098(2) 0.0581(13) Uani 1.000(13) 1 d . . . C1 C -0.3343(3) -0.3784(2) 0.4141(2) 0.0288(10) Uani 1.000(15) 1 d . . . C2 C -0.2746(3) -0.4633(2) 0.4706(2) 0.0279(10) Uani 1.000(16) 1 d . . . H2 H -0.2037 -0.4903 0.4412 0.034 Uiso 1.00(8) 1 calc R . . C3 C -0.3175(3) -0.5089(2) 0.5696(2) 0.0298(11) Uani 1.000(16) 1 d . . . C4 C -0.4183(3) -0.4663(2) 0.6125(3) 0.0312(11) Uani 1.000(16) 1 d . . . H4 H -0.4464 -0.4959 0.6802 0.037 Uiso 1.00(8) 1 calc R . . C5 C -0.4785(3) -0.3811(2) 0.5581(3) 0.0305(11) Uani 1.000(15) 1 d . . . C6 C -0.4375(3) -0.3389(2) 0.4586(2) 0.0323(11) Uani 1.000(15) 1 d . . . H6 H -0.4804 -0.2824 0.4204 0.039 Uiso 1 1 calc R . . C7 C -0.2918(3) -0.3306(2) 0.3084(2) 0.0296(10) Uani 1.000(15) 1 d . . . C8 C -0.1619(4) -0.3126(3) 0.2726(3) 0.0389(13) Uani 1.000(16) 1 d . . . H8 H -0.0988 -0.3342 0.3162 0.047 Uiso 1.00(9) 1 calc R . . C9 C -0.1231(4) -0.2638(3) 0.1747(3) 0.0385(12) Uani 1.000(16) 1 d . . . H9 H -0.0342 -0.2497 0.1519 0.046 Uiso 1.00(9) 1 calc R . . C10 C -0.2137(3) -0.2350(3) 0.1091(2) 0.0332(11) Uani 1.000(16) 1 d . . . C11 C -0.3432(4) -0.2556(3) 0.1438(3) 0.0405(13) Uani 1.000(16) 1 d . . . H11 H -0.4055 -0.2382 0.0995 0.049 Uiso 1.00(9) 1 calc R . . C12 C -0.3822(3) -0.3014(3) 0.2426(2) 0.0337(11) Uani 0.997(16) 1 d P . . H12 H -0.4715 -0.3130 0.2656 0.040 Uiso 1 1 calc R . . C13 C -0.2623(3) -0.6046(2) 0.6273(2) 0.0314(11) Uani 1.000(16) 1 d . . . C14 C -0.2267(3) -0.6754(3) 0.5847(2) 0.0332(11) Uani 1.000(16) 1 d . . . H14 H -0.2307 -0.6603 0.5172 0.040 Uiso 1 1 calc R . . C15 C -0.1853(4) -0.7681(3) 0.6400(3) 0.0365(12) Uani 1.000(16) 1 d . . . H15 H -0.1628 -0.8161 0.6101 0.044 Uiso 1.00(9) 1 calc R . . C16 C -0.1764(3) -0.7915(3) 0.7384(3) 0.0354(12) Uani 1.000(16) 1 d . . . C17 C -0.2102(3) -0.7207(3) 0.7810(3) 0.0332(11) Uani 1.000(15) 1 d . . . H17 H -0.2038 -0.7355 0.8482 0.040 Uiso 1.00(8) 1 calc R . . C18 C -0.2535(3) -0.6281(3) 0.7261(3) 0.0342(11) Uani 1.000(16) 1 d . . . H18 H -0.2772 -0.5805 0.7564 0.041 Uiso 1.00(8) 1 calc R . . C19 C -0.5843(3) -0.3352(3) 0.6049(3) 0.0334(11) Uani 1.000(16) 1 d . . . C20 C -0.6706(4) -0.3923(3) 0.6826(3) 0.0383(13) Uani 1.000(17) 1 d . . . H20 H -0.6616 -0.4623 0.7071 0.046 Uiso 1.00(9) 1 calc R . . C21 C -0.7696(4) -0.3485(3) 0.7251(3) 0.0422(13) Uani 1.000(17) 1 d . . . H21 H -0.8270 -0.3888 0.7787 0.051 Uiso 1.00(9) 1 calc R . . C22 C -0.7858(4) -0.2474(3) 0.6907(3) 0.0411(13) Uani 1.000(17) 1 d . . . C23 C -0.7012(4) -0.1895(3) 0.6130(3) 0.0440(14) Uani 1.000(18) 1 d . . . H23 H -0.7118 -0.1196 0.5881 0.053 Uiso 1 1 calc R . . C24 C -0.6005(4) -0.2329(3) 0.5709(3) 0.0424(14) Uani 1.000(17) 1 d . . . H24 H -0.5421 -0.1922 0.5182 0.051 Uiso 1.00(9) 1 calc R . . C25 C -0.1709(3) -0.1846(3) 0.0035(3) 0.0337(11) Uani 1.000(16) 1 d . . . C26 C -0.1298(3) -0.8920(3) 0.7972(3) 0.0357(12) Uani 1.000(16) 1 d . . . C27 C -0.8920(4) -0.1998(3) 0.7372(3) 0.0464(15) Uani 1.000(18) 1 d . . . O7 O -0.2084(4) -0.1402(4) -0.2950(3) 0.0791(18) Uani 1.000(14) 1 d . . . N1 N -0.1687(5) -0.1595(3) -0.4431(3) 0.0664(11) Uani 1 1 d . . . C28 C -0.1727(5) -0.1088(4) -0.3830(4) 0.0674(14) Uani 1 1 d . . . H28 H -0.1452 -0.0414 -0.4108 0.081 Uiso 1 1 calc R . . C29 C -0.1289(7) -0.1158(5) -0.5460(4) 0.084(3) Uani 1.00(2) 1 d . . . H29A H -0.0601 -0.1571 -0.5648 0.101 Uiso 1 1 calc R . . H29B H -0.0908 -0.0496 -0.5594 0.101 Uiso 1 1 calc R . . C30 C -0.2306(8) -0.1045(5) -0.6081(5) 0.095(2) Uani 1 1 d . . . H30A H -0.2636 -0.1700 -0.6006 0.142 Uiso 1 1 calc R . . H30B H -0.1955 -0.0702 -0.6763 0.142 Uiso 1 1 calc R . . H30C H -0.3009 -0.0656 -0.5890 0.142 Uiso 1 1 calc R . . C31 C -0.2051(6) -0.2646(5) -0.4006(5) 0.0798(17) Uani 1 1 d . . . H31A H -0.2612 -0.2757 -0.3382 0.096 Uiso 1 1 calc R . . H31B H -0.2564 -0.2809 -0.4449 0.096 Uiso 1 1 calc R . . C32 C -0.0968(10) -0.3325(6) -0.3825(7) 0.119(3) Uani 1 1 d . . . H32A H -0.0398 -0.3217 -0.4435 0.179 Uiso 1 1 calc R . . H32B H -0.1293 -0.4010 -0.3567 0.179 Uiso 1 1 calc R . . H32C H -0.0487 -0.3203 -0.3350 0.179 Uiso 1 1 calc R . . O8 O 0.1789(3) -0.0006(2) -0.1049(2) 0.0503(7) Uani 1 1 d . . . N2 N 0.3678(4) -0.0744(4) -0.1274(4) 0.0674(12) Uani 1 1 d . . . C33 C 0.2468(5) -0.0752(4) -0.0897(4) 0.0648(13) Uani 1 1 d . . . H33 H 0.2091 -0.1369 -0.0480 0.078 Uiso 1 1 calc R . . C34 C 0.4417(7) -0.1694(7) -0.1004(7) 0.108(3) Uani 1 1 d . . . H34A H 0.5217 -0.1594 -0.0756 0.130 Uiso 1 1 calc R . . H34B H 0.3892 -0.2212 -0.0474 0.130 Uiso 1 1 calc R . . C35 C 0.4753(10) -0.2035(10) -0.1826(10) 0.166(5) Uani 1 1 d . . . H35A H 0.3967 -0.2228 -0.2013 0.249 Uiso 1 1 calc R . . H35B H 0.5324 -0.2606 -0.1639 0.249 Uiso 1 1 calc R . . H35C H 0.5195 -0.1498 -0.2378 0.249 Uiso 1 1 calc R . . C36 C 0.4305(9) 0.0130(8) -0.1887(8) 0.136(3) Uani 1 1 d DU . . H36 H 0.3661 0.0669 -0.2091 0.163 Uiso 1 1 calc R . . C37B C 0.5223(18) 0.0392(16) -0.1275(15) 0.164(7) Uani 0.60 1 d PDU . . H37A H 0.5066 0.1006 -0.1121 0.197 Uiso 1 1 calc R . . H37B H 0.5625 -0.0155 -0.0786 0.197 Uiso 1 1 calc R . . C37A C 0.5481(17) 0.0476(19) -0.2297(15) 0.136(8) Uani 0.40 1 d PDU . . H37C H 0.5546 0.1154 -0.2788 0.163 Uiso 1 1 calc R . . H37D H 0.6101 0.0004 -0.2457 0.163 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 Cd1 0.02636(16) 0.02579(16) 0.02533(16) -0.00004(12) -0.00609(12) 0.00461(11) Cd2 0.04159(16) 0.02986(14) 0.02691(14) -0.00318(10) 0.00412(10) 0.01189(10) O1 0.0424(17) 0.062(2) 0.0309(15) -0.0052(13) -0.0037(11) -0.0033(13) O2 0.0360(14) 0.0319(14) 0.0312(14) -0.0031(10) 0.0007(10) 0.0006(10) O3 0.0464(17) 0.0415(16) 0.0374(16) 0.0007(12) -0.0165(12) 0.0140(12) O4 0.079(3) 0.0368(17) 0.0417(18) -0.0031(13) -0.0038(15) 0.0238(15) O5 0.064(2) 0.0383(18) 0.089(3) -0.0194(17) 0.0266(19) 0.0115(14) O6 0.068(2) 0.0449(19) 0.047(2) -0.0069(14) 0.0148(15) 0.0205(15) C1 0.0304(18) 0.0256(16) 0.0269(17) -0.0045(12) -0.0047(12) 0.0013(12) C2 0.0277(17) 0.0256(16) 0.0275(17) -0.0058(12) -0.0036(12) 0.0040(11) C3 0.0330(18) 0.0258(17) 0.0271(17) -0.0044(12) -0.0065(12) 0.0036(12) C4 0.0345(19) 0.0280(17) 0.0270(18) -0.0049(13) -0.0032(13) 0.0031(12) C5 0.0322(18) 0.0265(17) 0.0324(19) -0.0092(13) -0.0059(13) 0.0037(12) C6 0.037(2) 0.0257(17) 0.0315(19) -0.0057(13) -0.0083(13) 0.0056(12) C7 0.0310(18) 0.0245(16) 0.0288(18) -0.0037(12) -0.0046(12) 0.0040(12) C8 0.033(2) 0.042(2) 0.034(2) -0.0016(15) -0.0075(14) 0.0021(14) C9 0.0301(19) 0.041(2) 0.035(2) -0.0011(15) -0.0030(14) 0.0017(14) C10 0.0338(19) 0.0321(18) 0.0280(18) -0.0035(13) -0.0041(13) 0.0009(13) C11 0.035(2) 0.046(2) 0.032(2) -0.0018(16) -0.0080(14) 0.0004(15) C12 0.0243(17) 0.039(2) 0.0284(18) 0.0009(14) -0.0039(12) -0.0012(13) C13 0.0295(18) 0.0292(18) 0.0298(18) -0.0028(13) -0.0057(12) 0.0043(12) C14 0.040(2) 0.0318(18) 0.0253(17) -0.0063(13) -0.0089(13) 0.0118(13) C15 0.043(2) 0.0296(19) 0.033(2) -0.0067(14) -0.0075(14) 0.0127(14) C16 0.0325(19) 0.0312(19) 0.034(2) -0.0004(14) -0.0070(13) 0.0064(13) C17 0.0328(19) 0.0344(19) 0.0258(18) -0.0019(13) -0.0052(12) 0.0048(13) C18 0.038(2) 0.0307(18) 0.0314(19) -0.0076(14) -0.0054(14) 0.0069(13) C19 0.037(2) 0.0299(18) 0.0302(19) -0.0072(14) -0.0044(13) 0.0067(13) C20 0.046(2) 0.0280(19) 0.036(2) -0.0079(15) -0.0011(15) 0.0077(14) C21 0.045(2) 0.038(2) 0.039(2) -0.0110(17) 0.0029(16) 0.0062(16) C22 0.041(2) 0.038(2) 0.045(2) -0.0172(17) -0.0037(16) 0.0106(15) C23 0.050(2) 0.0276(19) 0.050(3) -0.0109(16) 0.0029(18) 0.0091(15) C24 0.045(2) 0.030(2) 0.045(2) -0.0076(16) 0.0054(17) 0.0037(15) C25 0.0332(19) 0.0304(18) 0.0320(19) -0.0047(14) -0.0021(13) 0.0031(13) C26 0.0309(19) 0.0303(19) 0.035(2) 0.0010(14) -0.0025(13) 0.0088(13) C27 0.049(3) 0.043(2) 0.048(3) -0.0193(19) -0.0032(18) 0.0113(17) O7 0.075(3) 0.111(4) 0.051(2) -0.026(2) -0.0107(19) -0.003(2) N1 0.078(3) 0.062(3) 0.058(3) -0.017(2) -0.009(2) -0.011(2) C28 0.067(3) 0.067(3) 0.064(3) -0.016(3) -0.014(3) -0.004(3) C29 0.097(5) 0.085(5) 0.057(4) -0.012(3) 0.005(3) -0.016(4) C30 0.137(6) 0.080(4) 0.066(4) -0.022(3) -0.008(4) -0.048(4) C31 0.075(4) 0.078(4) 0.066(4) -0.001(3) -0.005(3) -0.007(3) C32 0.152(8) 0.071(5) 0.146(8) -0.039(5) -0.052(6) -0.010(5) O8 0.0432(15) 0.0467(16) 0.0439(16) -0.0002(13) 0.0083(12) 0.0095(12) N2 0.038(2) 0.090(3) 0.080(3) -0.041(3) 0.000(2) 0.010(2) C33 0.051(3) 0.063(3) 0.067(3) -0.011(3) 0.006(2) 0.010(2) C34 0.072(4) 0.120(6) 0.134(7) -0.049(5) -0.016(4) 0.048(4) C35 0.124(8) 0.202(12) 0.245(14) -0.168(12) -0.039(8) 0.048(8) C36 0.097(5) 0.114(6) 0.166(7) -0.025(5) 0.022(5) 0.006(5) C37B 0.147(10) 0.148(10) 0.199(11) -0.060(8) -0.039(9) 0.024(8) C37A 0.112(11) 0.124(11) 0.148(12) -0.024(8) 0.004(8) 0.013(8) _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 Cd1 O3 2.252(2) 1_564 ? Cd1 O3 2.252(2) 2_546 ? Cd1 O8 2.269(3) . ? Cd1 O8 2.269(3) 2 ? Cd1 O2 2.315(3) . ? Cd1 O2 2.315(3) 2 ? Cd2 O4 2.173(3) 1_564 ? Cd2 O7 2.301(4) . ? Cd2 O5 2.314(3) 1_654 ? Cd2 O1 2.328(3) . ? Cd2 O6 2.348(3) 1_654 ? Cd2 O2 2.374(3) . ? Cd2 C27 2.663(4) 1_654 ? Cd2 C25 2.695(4) . ? O1 C25 1.255(4) . ? O2 C25 1.275(4) . ? O3 C26 1.249(5) . ? O3 Cd1 2.252(2) 1_546 ? O4 C26 1.258(5) . ? O4 Cd2 2.173(3) 1_546 ? O5 C27 1.250(5) . ? O5 Cd2 2.314(3) 1_456 ? O6 C27 1.240(5) . ? O6 Cd2 2.348(3) 1_456 ? C1 C2 1.397(4) . ? C1 C6 1.397(5) . ? C1 C7 1.482(4) . ? C2 C3 1.396(4) . ? C2 H2 0.9500 . ? C3 C4 1.393(5) . ? C3 C13 1.487(4) . ? C4 C5 1.392(5) . ? C4 H4 0.9500 . ? C5 C6 1.393(5) . ? C5 C19 1.486(5) . ? C6 H6 0.9500 . ? C7 C8 1.391(5) . ? C7 C12 1.395(4) . ? C8 C9 1.381(5) . ? C8 H8 0.9500 . ? C9 C10 1.393(5) . ? C9 H9 0.9500 . ? C10 C11 1.387(5) . ? C10 C25 1.486(5) . ? C11 C12 1.385(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.390(5) . ? C13 C18 1.393(5) . ? C14 C15 1.388(5) . ? C14 H14 0.9500 . ? C15 C16 1.387(5) . ? C15 H15 0.9500 . ? C16 C17 1.387(5) . ? C16 C26 1.507(5) . ? C17 C18 1.392(5) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.389(5) . ? C19 C24 1.393(5) . ? C20 C21 1.388(5) . ? C20 H20 0.9500 . ? C21 C22 1.377(5) . ? C21 H21 0.9500 . ? C22 C23 1.382(6) . ? C22 C27 1.500(5) . ? C23 C24 1.393(5) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C27 Cd2 2.663(4) 1_456 ? O7 C28 1.227(7) . ? N1 C28 1.328(7) . ? N1 C29 1.437(7) . ? N1 C31 1.463(8) . ? C28 H28 0.9500 . ? C29 C30 1.462(9) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.459(11) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? O8 C33 1.237(6) . ? N2 C33 1.313(6) . ? N2 C36 1.393(10) . ? N2 C34 1.501(8) . ? C33 H33 0.9500 . ? C34 C35 1.458(12) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37A 1.328(15) . ? C36 C37B 1.539(15) . ? C36 H36 1.0000 . ? C37B C37A 1.460(16) . ? C37B H37A 0.9900 . ? C37B H37B 0.9900 . ? C37A H37C 0.9900 . ? C37A H37D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Cd1 O3 180.0(2) 1_564 2_546 ? O3 Cd1 O8 95.30(11) 1_564 . ? O3 Cd1 O8 84.70(11) 2_546 . ? O3 Cd1 O8 84.70(11) 1_564 2 ? O3 Cd1 O8 95.30(11) 2_546 2 ? O8 Cd1 O8 180.0(2) . 2 ? O3 Cd1 O2 90.67(10) 1_564 . ? O3 Cd1 O2 89.33(10) 2_546 . ? O8 Cd1 O2 85.72(10) . . ? O8 Cd1 O2 94.28(10) 2 . ? O3 Cd1 O2 89.33(10) 1_564 2 ? O3 Cd1 O2 90.67(10) 2_546 2 ? O8 Cd1 O2 94.28(10) . 2 ? O8 Cd1 O2 85.72(10) 2 2 ? O2 Cd1 O2 180.00(11) . 2 ? O4 Cd2 O7 93.10(15) 1_564 . ? O4 Cd2 O5 93.08(12) 1_564 1_654 ? O7 Cd2 O5 87.82(15) . 1_654 ? O4 Cd2 O1 111.11(12) 1_564 . ? O7 Cd2 O1 91.06(12) . . ? O5 Cd2 O1 155.80(12) 1_654 . ? O4 Cd2 O6 148.71(12) 1_564 1_654 ? O7 Cd2 O6 88.70(15) . 1_654 ? O5 Cd2 O6 55.74(11) 1_654 1_654 ? O1 Cd2 O6 100.08(11) . 1_654 ? O4 Cd2 O2 103.20(11) 1_564 . ? O7 Cd2 O2 146.52(12) . . ? O5 Cd2 O2 119.70(13) 1_654 . ? O1 Cd2 O2 55.88(9) . . ? O6 Cd2 O2 91.91(10) 1_654 . ? O4 Cd2 C27 121.06(13) 1_564 1_654 ? O7 Cd2 C27 87.52(15) . 1_654 ? O5 Cd2 C27 27.99(12) 1_654 1_654 ? O1 Cd2 C27 127.82(13) . 1_654 ? O6 Cd2 C27 27.76(12) 1_654 1_654 ? O2 Cd2 C27 107.79(12) . 1_654 ? O4 Cd2 C25 110.80(11) 1_564 . ? O7 Cd2 C25 118.44(13) . . ? O5 Cd2 C25 142.10(13) 1_654 . ? O1 Cd2 C25 27.71(10) . . ? O6 Cd2 C25 95.51(11) 1_654 . ? O2 Cd2 C25 28.23(9) . . ? C27 Cd2 C25 120.20(12) 1_654 . ? C25 O1 Cd2 92.6(2) . . ? C25 O2 Cd1 126.1(2) . . ? C25 O2 Cd2 90.0(2) . . ? Cd1 O2 Cd2 111.58(9) . . ? C26 O3 Cd1 139.4(2) . 1_546 ? C26 O4 Cd2 129.4(2) . 1_546 ? C27 O5 Cd2 91.7(3) . 1_456 ? C27 O6 Cd2 90.4(2) . 1_456 ? C2 C1 C6 118.9(3) . . ? C2 C1 C7 121.5(3) . . ? C6 C1 C7 119.6(3) . . ? C3 C2 C1 120.9(3) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C4 C3 C2 118.9(3) . . ? C4 C3 C13 120.2(3) . . ? C2 C3 C13 120.8(3) . . ? C5 C4 C3 121.3(3) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C4 C5 C6 118.9(3) . . ? C4 C5 C19 120.9(3) . . ? C6 C5 C19 120.2(3) . . ? C5 C6 C1 121.0(3) . . ? C5 C6 H6 119.5 . . ? C1 C6 H6 119.5 . . ? C8 C7 C12 118.5(3) . . ? C8 C7 C1 121.2(3) . . ? C12 C7 C1 120.4(3) . . ? C9 C8 C7 121.0(3) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C8 C9 C10 120.3(3) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C11 C10 C9 119.0(3) . . ? C11 C10 C25 121.0(3) . . ? C9 C10 C25 120.0(3) . . ? C12 C11 C10 120.5(3) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C7 120.6(3) . . ? C11 C12 H12 119.7 . . ? C7 C12 H12 119.7 . . ? C14 C13 C18 118.5(3) . . ? C14 C13 C3 120.1(3) . . ? C18 C13 C3 121.2(3) . . ? C15 C14 C13 120.6(3) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C16 C15 C14 120.9(3) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C17 118.8(3) . . ? C15 C16 C26 120.3(3) . . ? C17 C16 C26 120.9(3) . . ? C16 C17 C18 120.5(3) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C13 120.7(3) . . ? C17 C18 H18 119.6 . . ? C13 C18 H18 119.7 . . ? C20 C19 C24 118.0(3) . . ? C20 C19 C5 121.5(3) . . ? C24 C19 C5 120.5(3) . . ? C21 C20 C19 120.9(3) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C22 C21 C20 120.9(4) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C23 119.0(4) . . ? C21 C22 C27 120.9(4) . . ? C23 C22 C27 120.1(4) . . ? C22 C23 C24 120.4(3) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C19 C24 C23 120.9(4) . . ? C19 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? O1 C25 O2 121.3(3) . . ? O1 C25 C10 119.6(3) . . ? O2 C25 C10 119.1(3) . . ? O1 C25 Cd2 59.67(19) . . ? O2 C25 Cd2 61.77(18) . . ? C10 C25 Cd2 173.9(3) . . ? O3 C26 O4 126.8(3) . . ? O3 C26 C16 117.5(3) . . ? O4 C26 C16 115.7(3) . . ? O6 C27 O5 122.1(4) . . ? O6 C27 C22 119.6(4) . . ? O5 C27 C22 118.3(4) . . ? O6 C27 Cd2 61.9(2) . 1_456 ? O5 C27 Cd2 60.3(2) . 1_456 ? C22 C27 Cd2 177.2(3) . 1_456 ? C28 O7 Cd2 120.5(4) . . ? C28 N1 C29 122.8(5) . . ? C28 N1 C31 117.4(5) . . ? C29 N1 C31 119.8(5) . . ? O7 C28 N1 126.6(6) . . ? O7 C28 H28 116.7 . . ? N1 C28 H28 116.7 . . ? N1 C29 C30 115.5(6) . . ? N1 C29 H29A 108.4 . . ? C30 C29 H29A 108.4 . . ? N1 C29 H29B 108.4 . . ? C30 C29 H29B 108.4 . . ? H29A C29 H29B 107.5 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 N1 114.8(6) . . ? C32 C31 H31A 108.6 . . ? N1 C31 H31A 108.6 . . ? C32 C31 H31B 108.6 . . ? N1 C31 H31B 108.6 . . ? H31A C31 H31B 107.6 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C33 O8 Cd1 120.2(3) . . ? C33 N2 C36 121.5(6) . . ? C33 N2 C34 119.1(6) . . ? C36 N2 C34 119.3(6) . . ? O8 C33 N2 124.1(5) . . ? O8 C33 H33 117.9 . . ? N2 C33 H33 117.9 . . ? C35 C34 N2 112.4(8) . . ? C35 C34 H34A 109.1 . . ? N2 C34 H34A 109.1 . . ? C35 C34 H34B 109.1 . . ? N2 C34 H34B 109.1 . . ? H34A C34 H34B 107.9 . . ? 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 . . ? C37A C36 N2 140.4(14) . . ? C37A C36 C37B 60.7(8) . . ? N2 C36 C37B 105.6(11) . . ? C37A C36 H36 109.8 . . ? N2 C36 H36 109.8 . . ? C37B C36 H36 109.8 . . ? C37A C37B C36 52.5(8) . . ? C37A C37B H37A 118.5 . . ? C36 C37B H37A 118.5 . . ? C37A C37B H37B 118.5 . . ? C36 C37B H37B 118.5 . . ? H37A C37B H37B 115.8 . . ? C36 C37A C37B 66.8(9) . . ? C36 C37A H37C 117.0 . . ? C37B C37A H37C 117.0 . . ? C36 C37A H37D 117.0 . . ? C37B C37A H37D 117.0 . . ? H37C C37A H37D 114.0 . . ? 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 Cd2 O1 C25 -94.8(2) 1_564 . . . ? O7 Cd2 O1 C25 171.5(2) . . . . ? O5 Cd2 O1 C25 84.4(4) 1_654 . . . ? O6 Cd2 O1 C25 82.6(2) 1_654 . . . ? O2 Cd2 O1 C25 -2.8(2) . . . . ? C27 Cd2 O1 C25 83.8(3) 1_654 . . . ? O3 Cd1 O2 C25 -72.9(3) 1_564 . . . ? O3 Cd1 O2 C25 107.1(3) 2_546 . . . ? O8 Cd1 O2 C25 -168.2(3) . . . . ? O8 Cd1 O2 C25 11.8(3) 2 . . . ? O2 Cd1 O2 C25 -4(100) 2 . . . ? O3 Cd1 O2 Cd2 33.84(12) 1_564 . . . ? O3 Cd1 O2 Cd2 -146.16(12) 2_546 . . . ? O8 Cd1 O2 Cd2 -61.42(12) . . . . ? O8 Cd1 O2 Cd2 118.58(12) 2 . . . ? O2 Cd1 O2 Cd2 102(100) 2 . . . ? O4 Cd2 O2 C25 109.5(2) 1_564 . . . ? O7 Cd2 O2 C25 -7.6(3) . . . . ? O5 Cd2 O2 C25 -149.1(2) 1_654 . . . ? O1 Cd2 O2 C25 2.8(2) . . . . ? O6 Cd2 O2 C25 -98.1(2) 1_654 . . . ? C27 Cd2 O2 C25 -121.3(2) 1_654 . . . ? O4 Cd2 O2 Cd1 -19.76(14) 1_564 . . . ? O7 Cd2 O2 Cd1 -136.8(2) . . . . ? O5 Cd2 O2 Cd1 81.62(14) 1_654 . . . ? O1 Cd2 O2 Cd1 -126.50(15) . . . . ? O6 Cd2 O2 Cd1 132.62(13) 1_654 . . . ? C27 Cd2 O2 Cd1 109.41(13) 1_654 . . . ? C25 Cd2 O2 Cd1 -129.3(2) . . . . ? C6 C1 C2 C3 0.6(5) . . . . ? C7 C1 C2 C3 -178.5(3) . . . . ? C1 C2 C3 C4 -2.4(5) . . . . ? C1 C2 C3 C13 174.0(3) . . . . ? C2 C3 C4 C5 1.7(5) . . . . ? C13 C3 C4 C5 -174.7(3) . . . . ? C3 C4 C5 C6 0.8(5) . . . . ? C3 C4 C5 C19 -178.9(3) . . . . ? C4 C5 C6 C1 -2.6(5) . . . . ? C19 C5 C6 C1 177.1(3) . . . . ? C2 C1 C6 C5 1.9(5) . . . . ? C7 C1 C6 C5 -178.9(3) . . . . ? C2 C1 C7 C8 -46.7(5) . . . . ? C6 C1 C7 C8 134.2(4) . . . . ? C2 C1 C7 C12 134.2(3) . . . . ? C6 C1 C7 C12 -45.0(5) . . . . ? C12 C7 C8 C9 2.3(6) . . . . ? C1 C7 C8 C9 -176.9(3) . . . . ? C7 C8 C9 C10 -2.5(6) . . . . ? C8 C9 C10 C11 0.3(6) . . . . ? C8 C9 C10 C25 -178.6(4) . . . . ? C9 C10 C11 C12 2.0(6) . . . . ? C25 C10 C11 C12 -179.1(4) . . . . ? C10 C11 C12 C7 -2.2(6) . . . . ? C8 C7 C12 C11 0.1(5) . . . . ? C1 C7 C12 C11 179.2(3) . . . . ? C4 C3 C13 C14 141.0(3) . . . . ? C2 C3 C13 C14 -35.4(5) . . . . ? C4 C3 C13 C18 -34.5(5) . . . . ? C2 C3 C13 C18 149.1(3) . . . . ? C18 C13 C14 C15 1.0(5) . . . . ? C3 C13 C14 C15 -174.5(3) . . . . ? C13 C14 C15 C16 -1.1(6) . . . . ? C14 C15 C16 C17 0.3(6) . . . . ? C14 C15 C16 C26 -179.3(3) . . . . ? C15 C16 C17 C18 0.6(5) . . . . ? C26 C16 C17 C18 -179.8(3) . . . . ? C16 C17 C18 C13 -0.7(5) . . . . ? C14 C13 C18 C17 -0.1(5) . . . . ? C3 C13 C18 C17 175.4(3) . . . . ? C4 C5 C19 C20 -33.6(5) . . . . ? C6 C5 C19 C20 146.8(4) . . . . ? C4 C5 C19 C24 147.1(4) . . . . ? C6 C5 C19 C24 -32.6(5) . . . . ? C24 C19 C20 C21 -0.1(6) . . . . ? C5 C19 C20 C21 -179.5(4) . . . . ? C19 C20 C21 C22 0.7(6) . . . . ? C20 C21 C22 C23 -0.3(6) . . . . ? C20 C21 C22 C27 -179.4(4) . . . . ? C21 C22 C23 C24 -0.6(7) . . . . ? C27 C22 C23 C24 178.5(4) . . . . ? C20 C19 C24 C23 -0.8(6) . . . . ? C5 C19 C24 C23 178.6(4) . . . . ? C22 C23 C24 C19 1.1(7) . . . . ? Cd2 O1 C25 O2 5.1(4) . . . . ? Cd2 O1 C25 C10 -173.0(3) . . . . ? Cd1 O2 C25 O1 112.1(4) . . . . ? Cd2 O2 C25 O1 -5.0(4) . . . . ? Cd1 O2 C25 C10 -69.8(4) . . . . ? Cd2 O2 C25 C10 173.1(3) . . . . ? Cd1 O2 C25 Cd2 117.1(2) . . . . ? C11 C10 C25 O1 -21.0(5) . . . . ? C9 C10 C25 O1 157.9(4) . . . . ? C11 C10 C25 O2 160.8(4) . . . . ? C9 C10 C25 O2 -20.3(5) . . . . ? C11 C10 C25 Cd2 -103(2) . . . . ? C9 C10 C25 Cd2 76(2) . . . . ? O4 Cd2 C25 O1 96.0(2) 1_564 . . . ? O7 Cd2 C25 O1 -9.7(3) . . . . ? O5 Cd2 C25 O1 -138.4(3) 1_654 . . . ? O6 Cd2 C25 O1 -101.2(2) 1_654 . . . ? O2 Cd2 C25 O1 175.0(4) . . . . ? C27 Cd2 C25 O1 -114.7(2) 1_654 . . . ? O4 Cd2 C25 O2 -79.0(2) 1_564 . . . ? O7 Cd2 C25 O2 175.3(2) . . . . ? O5 Cd2 C25 O2 46.6(3) 1_654 . . . ? O1 Cd2 C25 O2 -175.0(4) . . . . ? O6 Cd2 C25 O2 83.8(2) 1_654 . . . ? C27 Cd2 C25 O2 70.3(2) 1_654 . . . ? O4 Cd2 C25 C10 -179(100) 1_564 . . . ? O7 Cd2 C25 C10 75(2) . . . . ? O5 Cd2 C25 C10 -53(2) 1_654 . . . ? O1 Cd2 C25 C10 85(2) . . . . ? O6 Cd2 C25 C10 -16(2) 1_654 . . . ? O2 Cd2 C25 C10 -100(2) . . . . ? C27 Cd2 C25 C10 -30(2) 1_654 . . . ? Cd1 O3 C26 O4 30.0(7) 1_546 . . . ? Cd1 O3 C26 C16 -151.8(3) 1_546 . . . ? Cd2 O4 C26 O3 13.5(6) 1_546 . . . ? Cd2 O4 C26 C16 -164.7(3) 1_546 . . . ? C15 C16 C26 O3 176.7(3) . . . . ? C17 C16 C26 O3 -2.9(5) . . . . ? C15 C16 C26 O4 -4.9(5) . . . . ? C17 C16 C26 O4 175.5(4) . . . . ? Cd2 O6 C27 O5 2.0(5) 1_456 . . . ? Cd2 O6 C27 C22 -177.2(4) 1_456 . . . ? Cd2 O5 C27 O6 -2.0(5) 1_456 . . . ? Cd2 O5 C27 C22 177.2(3) 1_456 . . . ? C21 C22 C27 O6 2.5(7) . . . . ? C23 C22 C27 O6 -176.6(4) . . . . ? C21 C22 C27 O5 -176.8(4) . . . . ? C23 C22 C27 O5 4.2(7) . . . . ? C21 C22 C27 Cd2 -118(6) . . . 1_456 ? C23 C22 C27 Cd2 63(6) . . . 1_456 ? O4 Cd2 O7 C28 64.5(5) 1_564 . . . ? O5 Cd2 O7 C28 -28.4(5) 1_654 . . . ? O1 Cd2 O7 C28 175.7(5) . . . . ? O6 Cd2 O7 C28 -84.2(5) 1_654 . . . ? O2 Cd2 O7 C28 -175.7(4) . . . . ? C27 Cd2 O7 C28 -56.4(5) 1_654 . . . ? C25 Cd2 O7 C28 -179.8(4) . . . . ? Cd2 O7 C28 N1 131.7(5) . . . . ? C29 N1 C28 O7 178.1(6) . . . . ? C31 N1 C28 O7 -2.8(9) . . . . ? C28 N1 C29 C30 -110.9(7) . . . . ? C31 N1 C29 C30 70.1(8) . . . . ? C28 N1 C31 C32 -98.2(8) . . . . ? C29 N1 C31 C32 80.9(8) . . . . ? O3 Cd1 O8 C33 -144.0(4) 1_564 . . . ? O3 Cd1 O8 C33 36.0(4) 2_546 . . . ? O8 Cd1 O8 C33 108(100) 2 . . . ? O2 Cd1 O8 C33 -53.7(4) . . . . ? O2 Cd1 O8 C33 126.3(4) 2 . . . ? Cd1 O8 C33 N2 -159.2(4) . . . . ? C36 N2 C33 O8 0.3(11) . . . . ? C34 N2 C33 O8 177.8(6) . . . . ? C33 N2 C34 C35 113.0(8) . . . . ? C36 N2 C34 C35 -69.6(11) . . . . ? C33 N2 C36 C37A 168.6(19) . . . . ? C34 N2 C36 C37A -9(2) . . . . ? C33 N2 C36 C37B 106.0(11) . . . . ? C34 N2 C36 C37B -71.4(11) . . . . ? N2 C36 C37B C37A 139.5(16) . . . . ? N2 C36 C37A C37B -79(2) . . . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 1.528 _refine_diff_density_min -0.546 _refine_diff_density_rms 0.123