# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_wy475 _database_code_depnum_ccdc_archive 'CCDC 874284' #TrackingRef 'MMCF-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H40 Cd2 N4 O9' _chemical_formula_weight 945.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0007 0.0007 '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 0.0018 0.0015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0039 0.0027 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -2.2124 0.6286 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.8372(19) _cell_length_b 21.164(2) _cell_length_c 21.721(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.300(2) _cell_angle_gamma 90.00 _cell_volume 8199.7(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.766 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 0.181 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9910 _exptl_absorpt_correction_T_max 0.9982 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.49594 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'BRUKER SMART APEXII CCD' _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 91148 _diffrn_reflns_av_R_equivalents 0.0648 _diffrn_reflns_av_sigmaI/netI 0.0744 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 0.80 _diffrn_reflns_theta_max 18.13 _reflns_number_total 16212 _reflns_number_gt 9873 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2010)' _computing_cell_refinement 'APEX2 (Bruker, 2010); SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009);XPREP(Sheldrick,2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material 'APEX2 (Bruker, 2010)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1200P)^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 16212 _refine_ls_number_parameters 497 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1012 _refine_ls_R_factor_gt 0.0725 _refine_ls_wR_factor_ref 0.2019 _refine_ls_wR_factor_gt 0.1930 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.032 _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 Cd1 Cd 0.39801(2) -0.340682(18) 0.485519(17) 0.04448(15) Uani 1 1 d . . . Cd2 Cd 0.79964(2) 0.084147(17) 0.517109(16) 0.03930(14) Uani 1 1 d . . . C1 C 0.6331(3) 0.0633(3) 0.4759(2) 0.0430(11) Uani 1 1 d U . . H1A H 0.6185 0.1055 0.4914 0.052 Uiso 1 1 calc R . . H1B H 0.5870 0.0379 0.4707 0.052 Uiso 1 1 calc R . . C2 C 0.6717(3) 0.0705(3) 0.4134(3) 0.0710(18) Uani 1 1 d . . . H2A H 0.6816 0.0279 0.3964 0.085 Uiso 1 1 calc R . . H2B H 0.6371 0.0925 0.3848 0.085 Uiso 1 1 calc R . . C3 C 0.7322(3) 0.1727(3) 0.4182(2) 0.0582(13) Uani 1 1 d U . . H3A H 0.6872 0.1814 0.4433 0.070 Uiso 1 1 calc R . . H3B H 0.7216 0.1875 0.3759 0.070 Uiso 1 1 calc R . . C4 C 0.7969(3) 0.2105(3) 0.4439(2) 0.0559(13) Uani 1 1 d U . . H4A H 0.7844 0.2560 0.4417 0.067 Uiso 1 1 calc R . . H4B H 0.8418 0.2033 0.4182 0.067 Uiso 1 1 calc R . . C5 C 0.7608(3) 0.2199(3) 0.5524(3) 0.0616(15) Uani 1 1 d . . . H5A H 0.7101 0.2155 0.5343 0.074 Uiso 1 1 calc R . . H5B H 0.7711 0.2656 0.5575 0.074 Uiso 1 1 calc R . . C6 C 0.7622(4) 0.1892(3) 0.6136(3) 0.0648(16) Uani 1 1 d . . . H6A H 0.7227 0.2085 0.6395 0.078 Uiso 1 1 calc R . . H6B H 0.8111 0.1981 0.6336 0.078 Uiso 1 1 calc R . . C7 C 0.6706(3) 0.1067(3) 0.6098(2) 0.0589(15) Uani 1 1 d . . . H7A H 0.6461 0.1387 0.5832 0.071 Uiso 1 1 calc R . . H7B H 0.6499 0.1114 0.6517 0.071 Uiso 1 1 calc R . . C8 C 0.6507(4) 0.0420(3) 0.5859(3) 0.0668(17) Uani 1 1 d . . . H8A H 0.5955 0.0374 0.5843 0.080 Uiso 1 1 calc R . . H8B H 0.6709 0.0095 0.6142 0.080 Uiso 1 1 calc R . . C9 C 0.4735(3) -0.2312(3) 0.5037(3) 0.0623(16) Uani 1 1 d . . . C10 C 0.5257(3) -0.1755(2) 0.5079(3) 0.0481(13) Uani 1 1 d . . . C11 C 0.5657(3) -0.1631(3) 0.5612(2) 0.0598(16) Uani 1 1 d . . . H11 H 0.5566 -0.1865 0.5977 0.072 Uiso 1 1 calc R . . C12 C 0.6191(3) -0.1160(3) 0.5602(2) 0.0577(15) Uani 1 1 d . . . H12 H 0.6463 -0.1076 0.5970 0.069 Uiso 1 1 calc R . . C13 C 0.6352(3) -0.0804(2) 0.5088(2) 0.0467(13) Uani 1 1 d . . . C14 C 0.5926(3) -0.0929(3) 0.4567(2) 0.0513(13) Uani 1 1 d . . . H14 H 0.5996 -0.0678 0.4209 0.062 Uiso 1 1 calc R . . C15 C 0.5405(3) -0.1404(3) 0.4555(3) 0.0601(15) Uani 1 1 d . . . H15 H 0.5143 -0.1495 0.4183 0.072 Uiso 1 1 calc R . . C16 C 0.6986(3) -0.0363(2) 0.5095(2) 0.0470(12) Uani 1 1 d . . . H16A H 0.7240 -0.0394 0.4692 0.056 Uiso 1 1 calc R . . H16B H 0.7346 -0.0511 0.5411 0.056 Uiso 1 1 calc R . . C17 C 0.6715(4) 0.1109(5) 0.1201(3) 0.0776(19) Uani 1 1 d U . . C18 C 0.7070(3) 0.1032(3) 0.1840(2) 0.0603(15) Uani 1 1 d . . . C19 C 0.7471(3) 0.1518(3) 0.2122(2) 0.0551(14) Uani 1 1 d . . . H19 H 0.7546 0.1901 0.1904 0.066 Uiso 1 1 calc R . . C20 C 0.7758(3) 0.1459(3) 0.2695(2) 0.0513(13) Uani 1 1 d . . . H20 H 0.8033 0.1800 0.2868 0.062 Uiso 1 1 calc R . . C21 C 0.7660(3) 0.0911(2) 0.3041(2) 0.0481(13) Uani 1 1 d . . . C22 C 0.7289(3) 0.0388(3) 0.2763(2) 0.0637(16) Uani 1 1 d . . . H22 H 0.7222 0.0005 0.2986 0.076 Uiso 1 1 calc R . . C23 C 0.7026(3) 0.0443(3) 0.2166(2) 0.0595(15) Uani 1 1 d . . . H23 H 0.6812 0.0085 0.1968 0.071 Uiso 1 1 calc R . . C24 C 0.7963(3) 0.0850(2) 0.3675(2) 0.0475(12) Uani 1 1 d . . . H24A H 0.8431 0.1101 0.3707 0.057 Uiso 1 1 calc R . . H24B H 0.8095 0.0402 0.3750 0.057 Uiso 1 1 calc R . . C25 C 1.1071(3) 0.0179(2) 0.4811(2) 0.0431(12) Uani 1 1 d . . . C26 C 1.0549(3) 0.0713(2) 0.4913(2) 0.0375(11) Uani 1 1 d . . . C27 C 1.0262(3) 0.0818(2) 0.5483(2) 0.0481(13) Uani 1 1 d . . . H27 H 1.0421 0.0559 0.5816 0.058 Uiso 1 1 calc R . . C28 C 0.9745(3) 0.1292(2) 0.5592(2) 0.0471(12) Uani 1 1 d . . . H28 H 0.9542 0.1346 0.5992 0.056 Uiso 1 1 calc R . . C29 C 0.9524(3) 0.1688(2) 0.5116(2) 0.0451(12) Uani 1 1 d . . . C30 C 0.9839(3) 0.1598(3) 0.4523(2) 0.0541(14) Uani 1 1 d . . . H30 H 0.9697 0.1865 0.4190 0.065 Uiso 1 1 calc R . . C31 C 1.0356(3) 0.1114(3) 0.4434(2) 0.0507(13) Uani 1 1 d . . . H31 H 1.0579 0.1059 0.4041 0.061 Uiso 1 1 calc R . . C32 C 0.8938(3) 0.2184(2) 0.5218(3) 0.0515(13) Uani 1 1 d . . . H32A H 0.9031 0.2545 0.4938 0.062 Uiso 1 1 calc R . . H32B H 0.8976 0.2341 0.5646 0.062 Uiso 1 1 calc R . . C33 C 0.6679(3) 0.1279(3) 0.9083(2) 0.0503(13) Uani 1 1 d . . . C34 C 0.7011(3) 0.1151(2) 0.8459(2) 0.0470(12) Uani 1 1 d . . . C35 C 0.7510(3) 0.1578(3) 0.8199(2) 0.0531(14) Uani 1 1 d . . . H35 H 0.7658 0.1942 0.8426 0.064 Uiso 1 1 calc R . . C36 C 0.7796(3) 0.1484(3) 0.7614(2) 0.0555(14) Uani 1 1 d . . . H36 H 0.8142 0.1779 0.7448 0.067 Uiso 1 1 calc R . . C37 C 0.7580(3) 0.0958(2) 0.7266(2) 0.0494(13) Uani 1 1 d . . . C38 C 0.7106(3) 0.0532(3) 0.7531(2) 0.0553(14) Uani 1 1 d . . . H38 H 0.6984 0.0157 0.7313 0.066 Uiso 1 1 calc R . . C39 C 0.6795(3) 0.0631(3) 0.8113(2) 0.0599(16) Uani 1 1 d . . . H39 H 0.6436 0.0342 0.8271 0.072 Uiso 1 1 calc R . . C40 C 0.7893(3) 0.0845(2) 0.6641(2) 0.0431(12) Uani 1 1 d . . . H40A H 0.7867 0.0387 0.6553 0.052 Uiso 1 1 calc R . . H40B H 0.8429 0.0967 0.6645 0.052 Uiso 1 1 calc R . . N1 N 0.7439(2) 0.1063(2) 0.41663(19) 0.0528(11) Uani 1 1 d . . . N2 N 0.6831(2) 0.0322(2) 0.52158(18) 0.0459(10) Uani 1 1 d U . . N3 N 0.8153(2) 0.19319(19) 0.5104(2) 0.0508(11) Uani 1 1 d . . . N4 N 0.7505(2) 0.1196(2) 0.61209(17) 0.0496(11) Uani 1 1 d . . . O1 O 0.4821(3) -0.2769(2) 0.5416(2) 0.0799(13) Uani 1 1 d . . . O2 O 0.4264(2) -0.2331(2) 0.4664(2) 0.0780(13) Uani 1 1 d . . . O3 O 0.6498(3) 0.0617(4) 0.0939(2) 0.119(2) Uani 1 1 d . . . O4 O 0.6716(3) 0.1637(3) 0.09938(19) 0.0828(14) Uani 1 1 d U . . O5 O 1.1356(2) 0.00673(17) 0.42998(15) 0.0532(9) Uani 1 1 d . . . O6 O 1.1247(2) -0.01488(17) 0.52874(15) 0.0526(9) Uani 1 1 d . . . O7 O 0.6899(2) 0.1748(2) 0.93700(18) 0.0688(12) Uani 1 1 d . . . O8 O 0.6192(2) 0.09224(18) 0.92877(17) 0.0652(11) Uani 1 1 d . . . O9 O 0.5106(6) -0.3830(5) 0.4465(4) 0.193(4) Uani 1 1 d . . . 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 0.0539(3) 0.0476(3) 0.0320(2) -0.00320(16) 0.00123(17) 0.00375(18) Cd2 0.0449(2) 0.0431(2) 0.0300(2) 0.00282(15) 0.00373(15) 0.01060(17) C1 0.033(2) 0.062(3) 0.034(2) 0.009(2) -0.0081(19) 0.012(2) C2 0.060(4) 0.111(5) 0.041(3) 0.005(3) -0.019(3) 0.022(4) C3 0.071(3) 0.061(3) 0.042(3) 0.018(2) 0.006(2) 0.024(3) C4 0.061(3) 0.060(3) 0.047(3) 0.017(2) 0.003(2) 0.007(2) C5 0.058(4) 0.060(4) 0.066(4) -0.001(3) 0.017(3) 0.001(3) C6 0.079(4) 0.066(4) 0.049(3) -0.003(3) 0.009(3) 0.020(3) C7 0.069(4) 0.068(4) 0.041(3) 0.001(3) 0.014(3) 0.017(3) C8 0.068(4) 0.057(4) 0.075(4) 0.014(3) 0.028(3) 0.017(3) C9 0.050(4) 0.047(4) 0.090(5) -0.005(3) -0.012(3) 0.006(3) C10 0.027(3) 0.050(3) 0.067(4) 0.009(3) 0.001(2) -0.001(2) C11 0.065(4) 0.077(4) 0.038(3) 0.022(3) -0.005(3) -0.007(3) C12 0.082(4) 0.057(3) 0.034(3) -0.003(3) -0.011(3) -0.007(3) C13 0.054(3) 0.033(3) 0.054(3) 0.006(2) 0.008(3) 0.016(2) C14 0.056(3) 0.053(3) 0.045(3) 0.016(2) 0.012(3) -0.013(3) C15 0.068(4) 0.060(4) 0.052(3) -0.006(3) -0.025(3) 0.006(3) C16 0.052(3) 0.045(3) 0.044(3) 0.011(2) -0.009(2) 0.001(2) C17 0.060(4) 0.133(6) 0.040(3) -0.006(4) 0.007(3) -0.006(4) C18 0.064(4) 0.086(4) 0.031(3) 0.010(3) 0.010(3) 0.007(3) C19 0.062(4) 0.069(4) 0.034(3) 0.007(3) 0.010(3) -0.005(3) C20 0.057(3) 0.062(4) 0.035(3) 0.007(2) 0.003(2) -0.010(3) C21 0.047(3) 0.055(3) 0.043(3) -0.006(2) 0.004(2) 0.012(3) C22 0.083(4) 0.071(4) 0.038(3) 0.012(3) 0.006(3) -0.007(3) C23 0.061(4) 0.084(4) 0.034(3) -0.013(3) 0.011(2) -0.015(3) C24 0.055(3) 0.053(3) 0.035(3) 0.003(2) 0.006(2) 0.009(2) C25 0.029(2) 0.049(3) 0.051(3) -0.003(2) 0.005(2) -0.008(2) C26 0.034(2) 0.033(3) 0.046(3) -0.003(2) 0.009(2) -0.001(2) C27 0.069(4) 0.040(3) 0.036(3) 0.008(2) 0.008(2) 0.004(3) C28 0.052(3) 0.055(3) 0.034(3) -0.005(2) 0.007(2) 0.002(3) C29 0.058(3) 0.040(3) 0.037(3) 0.000(2) 0.012(2) -0.002(2) C30 0.061(4) 0.059(3) 0.043(3) 0.010(2) 0.009(3) 0.017(3) C31 0.053(3) 0.054(3) 0.046(3) 0.010(3) 0.014(2) 0.004(3) C32 0.046(3) 0.040(3) 0.069(4) -0.007(3) 0.001(3) 0.012(2) C33 0.051(3) 0.064(4) 0.036(3) -0.008(3) -0.007(2) -0.012(3) C34 0.050(3) 0.052(3) 0.040(3) 0.003(2) -0.001(2) 0.002(3) C35 0.053(3) 0.064(4) 0.042(3) -0.010(3) 0.008(2) 0.000(3) C36 0.060(4) 0.064(4) 0.042(3) 0.002(3) 0.006(3) -0.016(3) C37 0.062(3) 0.050(3) 0.036(3) -0.003(2) 0.004(2) 0.008(3) C38 0.063(4) 0.050(3) 0.053(3) -0.012(3) 0.013(3) -0.017(3) C39 0.080(4) 0.064(4) 0.035(3) -0.015(3) 0.015(3) -0.026(3) C40 0.049(3) 0.056(3) 0.024(2) -0.003(2) -0.003(2) 0.003(2) N1 0.041(2) 0.077(3) 0.040(2) 0.007(2) 0.0013(19) 0.019(2) N2 0.049(2) 0.048(2) 0.041(2) 0.0098(18) 0.0052(18) 0.0095(19) N3 0.056(3) 0.035(2) 0.061(3) -0.004(2) -0.005(2) 0.011(2) N4 0.057(3) 0.062(3) 0.030(2) 0.0031(19) 0.0049(19) 0.010(2) O1 0.099(3) 0.067(3) 0.073(3) 0.014(2) -0.019(2) -0.027(2) O2 0.050(2) 0.087(3) 0.097(3) 0.016(3) -0.011(2) -0.018(2) O3 0.112(4) 0.187(6) 0.057(3) -0.042(4) -0.020(3) -0.007(4) O4 0.070(3) 0.133(4) 0.046(2) 0.039(3) -0.010(2) -0.003(3) O5 0.059(2) 0.061(2) 0.0387(19) -0.0113(17) 0.0048(17) 0.0179(18) O6 0.053(2) 0.060(2) 0.045(2) 0.0140(17) 0.0054(16) 0.0187(18) O7 0.086(3) 0.072(3) 0.048(2) -0.022(2) 0.019(2) -0.031(2) O8 0.085(3) 0.067(3) 0.044(2) -0.0011(18) 0.016(2) -0.027(2) O9 0.218(9) 0.221(9) 0.140(7) 0.017(7) 0.078(6) 0.028(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 O4 2.219(4) 2_645 ? Cd1 O7 2.329(4) 2_646 ? Cd1 O1 2.352(4) . ? Cd1 O9 2.360(9) . ? Cd1 O8 2.363(4) 2_646 ? Cd1 O2 2.368(4) . ? Cd1 C33 2.678(5) 2_646 ? Cd1 C9 2.708(6) . ? Cd2 O6 2.231(3) 3_756 ? Cd2 N3 2.329(4) . ? Cd2 N2 2.353(4) . ? Cd2 N4 2.368(4) . ? Cd2 N1 2.439(4) . ? Cd2 O5 2.518(3) 3_756 ? Cd2 C25 2.727(5) 3_756 ? C1 N2 1.484(6) . ? C1 C2 1.531(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N1 1.495(8) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N1 1.420(7) . ? C3 C4 1.510(8) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N3 1.523(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 N3 1.452(7) . ? C5 C6 1.480(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N4 1.489(8) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N4 1.453(7) . ? C7 C8 1.505(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N2 1.529(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O2 1.164(7) . ? C9 O1 1.280(7) . ? C9 C10 1.505(8) . ? C10 C11 1.382(8) . ? C10 C15 1.386(8) . ? C11 C12 1.378(8) . ? C11 H11 0.9500 . ? C12 C13 1.379(7) . ? C12 H12 0.9500 . ? C13 C14 1.385(8) . ? C13 C16 1.466(7) . ? C14 C15 1.370(8) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 N2 1.500(7) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 O4 1.206(9) . ? C17 O3 1.247(9) . ? C17 C18 1.532(9) . ? C18 C19 1.393(8) . ? C18 C23 1.435(8) . ? C19 C20 1.350(7) . ? C19 H19 0.9500 . ? C20 C21 1.393(7) . ? C20 H20 0.9500 . ? C21 C22 1.423(8) . ? C21 C24 1.484(7) . ? C22 C23 1.382(8) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 N1 1.492(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 O5 1.247(6) . ? C25 O6 1.283(6) . ? C25 C26 1.481(7) . ? C25 Cd2 2.727(5) 3_756 ? C26 C27 1.361(7) . ? C26 C31 1.385(7) . ? C27 C28 1.383(7) . ? C27 H27 0.9500 . ? C28 C29 1.386(7) . ? C28 H28 0.9500 . ? C29 C30 1.420(7) . ? C29 C32 1.500(7) . ? C30 C31 1.393(7) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 N3 1.517(7) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 O7 1.234(6) . ? C33 O8 1.235(6) . ? C33 C34 1.507(7) . ? C33 Cd1 2.678(5) 2_656 ? C34 C39 1.387(7) . ? C34 C35 1.391(7) . ? C35 C36 1.387(7) . ? C35 H35 0.9500 . ? C36 C37 1.398(7) . ? C36 H36 0.9500 . ? C37 C38 1.364(7) . ? C37 C40 1.490(7) . ? C38 C39 1.399(7) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 N4 1.515(6) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? O4 Cd1 2.219(4) 2_655 ? O5 Cd2 2.518(3) 3_756 ? O6 Cd2 2.231(3) 3_756 ? O7 Cd1 2.329(4) 2_656 ? O8 Cd1 2.363(4) 2_656 ? 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 Cd1 O7 102.64(16) 2_645 2_646 ? O4 Cd1 O1 139.31(18) 2_645 . ? O7 Cd1 O1 88.56(17) 2_646 . ? O4 Cd1 O9 101.0(3) 2_645 . ? O7 Cd1 O9 152.8(2) 2_646 . ? O1 Cd1 O9 82.1(3) . . ? O4 Cd1 O8 127.26(18) 2_645 2_646 ? O7 Cd1 O8 54.83(13) 2_646 2_646 ? O1 Cd1 O8 91.26(15) . 2_646 ? O9 Cd1 O8 99.7(2) . 2_646 ? O4 Cd1 O2 86.16(19) 2_645 . ? O7 Cd1 O2 97.86(16) 2_646 . ? O1 Cd1 O2 53.36(15) . . ? O9 Cd1 O2 96.8(3) . . ? O8 Cd1 O2 138.08(16) 2_646 . ? O4 Cd1 C33 118.67(17) 2_645 2_646 ? O7 Cd1 C33 27.42(14) 2_646 2_646 ? O1 Cd1 C33 88.75(16) . 2_646 ? O9 Cd1 C33 126.4(2) . 2_646 ? O8 Cd1 C33 27.46(14) 2_646 2_646 ? O2 Cd1 C33 118.97(17) . 2_646 ? O4 Cd1 C9 111.1(2) 2_645 . ? O7 Cd1 C9 96.35(18) 2_646 . ? O1 Cd1 C9 28.19(17) . . ? O9 Cd1 C9 87.4(3) . . ? O8 Cd1 C9 117.78(18) 2_646 . ? O2 Cd1 C9 25.41(16) . . ? C33 Cd1 C9 107.89(19) 2_646 . ? O6 Cd2 N3 123.35(15) 3_756 . ? O6 Cd2 N2 104.37(14) 3_756 . ? N3 Cd2 N2 124.86(15) . . ? O6 Cd2 N4 145.56(13) 3_756 . ? N3 Cd2 N4 77.63(16) . . ? N2 Cd2 N4 77.37(15) . . ? O6 Cd2 N1 88.38(13) 3_756 . ? N3 Cd2 N1 78.58(16) . . ? N2 Cd2 N1 76.73(15) . . ? N4 Cd2 N1 124.59(14) . . ? O6 Cd2 O5 54.87(11) 3_756 3_756 ? N3 Cd2 O5 136.91(14) . 3_756 ? N2 Cd2 O5 91.59(13) . 3_756 ? N4 Cd2 O5 90.88(13) . 3_756 ? N1 Cd2 O5 137.66(13) . 3_756 ? O6 Cd2 C25 27.77(13) 3_756 3_756 ? N3 Cd2 C25 135.42(14) . 3_756 ? N2 Cd2 C25 99.69(13) . 3_756 ? N4 Cd2 C25 117.86(15) . 3_756 ? N1 Cd2 C25 114.26(15) . 3_756 ? O5 Cd2 C25 27.13(12) 3_756 3_756 ? N2 C1 C2 111.5(4) . . ? N2 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? N2 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 108.0 . . ? N1 C2 C1 113.5(5) . . ? N1 C2 H2A 108.9 . . ? C1 C2 H2A 108.9 . . ? N1 C2 H2B 108.9 . . ? C1 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? N1 C3 C4 115.0(5) . . ? N1 C3 H3A 108.5 . . ? C4 C3 H3A 108.5 . . ? N1 C3 H3B 108.5 . . ? C4 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? C3 C4 N3 112.5(4) . . ? C3 C4 H4A 109.1 . . ? N3 C4 H4A 109.1 . . ? C3 C4 H4B 109.1 . . ? N3 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? N3 C5 C6 112.7(5) . . ? N3 C5 H5A 109.1 . . ? C6 C5 H5A 109.1 . . ? N3 C5 H5B 109.1 . . ? C6 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? C5 C6 N4 114.3(5) . . ? C5 C6 H6A 108.7 . . ? N4 C6 H6A 108.7 . . ? C5 C6 H6B 108.7 . . ? N4 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? N4 C7 C8 114.3(5) . . ? N4 C7 H7A 108.7 . . ? C8 C7 H7A 108.7 . . ? N4 C7 H7B 108.7 . . ? C8 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C7 C8 N2 110.4(4) . . ? C7 C8 H8A 109.6 . . ? N2 C8 H8A 109.6 . . ? C7 C8 H8B 109.6 . . ? N2 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? O2 C9 O1 120.2(6) . . ? O2 C9 C10 121.0(6) . . ? O1 C9 C10 118.8(5) . . ? O2 C9 Cd1 60.8(3) . . ? O1 C9 Cd1 60.3(3) . . ? C10 C9 Cd1 170.5(4) . . ? C11 C10 C15 119.1(5) . . ? C11 C10 C9 121.1(5) . . ? C15 C10 C9 119.3(5) . . ? C12 C11 C10 118.5(5) . . ? C12 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? C11 C12 C13 123.7(5) . . ? C11 C12 H12 118.2 . . ? C13 C12 H12 118.2 . . ? C12 C13 C14 116.3(5) . . ? C12 C13 C16 120.2(5) . . ? C14 C13 C16 123.3(5) . . ? C15 C14 C13 121.6(5) . . ? C15 C14 H14 119.2 . . ? C13 C14 H14 119.2 . . ? C14 C15 C10 120.7(5) . . ? C14 C15 H15 119.7 . . ? C10 C15 H15 119.7 . . ? C13 C16 N2 118.4(4) . . ? C13 C16 H16A 107.7 . . ? N2 C16 H16A 107.7 . . ? C13 C16 H16B 107.7 . . ? N2 C16 H16B 107.7 . . ? H16A C16 H16B 107.1 . . ? O4 C17 O3 127.3(7) . . ? O4 C17 C18 115.8(7) . . ? O3 C17 C18 116.7(8) . . ? C19 C18 C23 117.0(5) . . ? C19 C18 C17 121.9(6) . . ? C23 C18 C17 121.1(6) . . ? C20 C19 C18 121.9(5) . . ? C20 C19 H19 119.0 . . ? C18 C19 H19 119.0 . . ? C19 C20 C21 121.7(5) . . ? C19 C20 H20 119.1 . . ? C21 C20 H20 119.1 . . ? C20 C21 C22 118.6(5) . . ? C20 C21 C24 121.8(5) . . ? C22 C21 C24 119.5(5) . . ? C23 C22 C21 119.1(5) . . ? C23 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? C22 C23 C18 121.2(6) . . ? C22 C23 H23 119.4 . . ? C18 C23 H23 119.4 . . ? C21 C24 N1 114.3(4) . . ? C21 C24 H24A 108.7 . . ? N1 C24 H24A 108.7 . . ? C21 C24 H24B 108.7 . . ? N1 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? O5 C25 O6 121.1(5) . . ? O5 C25 C26 122.5(5) . . ? O6 C25 C26 116.4(4) . . ? O5 C25 Cd2 67.1(3) . 3_756 ? O6 C25 Cd2 54.1(2) . 3_756 ? C26 C25 Cd2 170.4(4) . 3_756 ? C27 C26 C31 119.3(4) . . ? C27 C26 C25 120.0(5) . . ? C31 C26 C25 120.6(4) . . ? C26 C27 C28 121.9(5) . . ? C26 C27 H27 119.0 . . ? C28 C27 H27 119.0 . . ? C27 C28 C29 119.9(4) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C28 C29 C30 118.9(5) . . ? C28 C29 C32 120.6(4) . . ? C30 C29 C32 120.4(5) . . ? C31 C30 C29 119.3(5) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C26 C31 C30 120.6(5) . . ? C26 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C29 C32 N3 111.9(4) . . ? C29 C32 H32A 109.2 . . ? N3 C32 H32A 109.2 . . ? C29 C32 H32B 109.2 . . ? N3 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? O7 C33 O8 122.1(5) . . ? O7 C33 C34 118.3(5) . . ? O8 C33 C34 119.6(5) . . ? O7 C33 Cd1 60.4(3) . 2_656 ? O8 C33 Cd1 61.9(3) . 2_656 ? C34 C33 Cd1 174.8(4) . 2_656 ? C39 C34 C35 118.2(5) . . ? C39 C34 C33 121.4(5) . . ? C35 C34 C33 120.2(5) . . ? C36 C35 C34 121.2(5) . . ? C36 C35 H35 119.4 . . ? C34 C35 H35 119.4 . . ? C35 C36 C37 120.6(5) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C38 C37 C36 117.8(5) . . ? C38 C37 C40 121.0(5) . . ? C36 C37 C40 121.1(5) . . ? C37 C38 C39 122.2(5) . . ? C37 C38 H38 118.9 . . ? C39 C38 H38 118.9 . . ? C34 C39 C38 119.8(5) . . ? C34 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C37 C40 N4 115.4(4) . . ? C37 C40 H40A 108.4 . . ? N4 C40 H40A 108.4 . . ? C37 C40 H40B 108.4 . . ? N4 C40 H40B 108.4 . . ? H40A C40 H40B 107.5 . . ? C3 N1 C24 114.1(4) . . ? C3 N1 C2 112.1(4) . . ? C24 N1 C2 110.9(4) . . ? C3 N1 Cd2 103.1(3) . . ? C24 N1 Cd2 109.1(3) . . ? C2 N1 Cd2 106.9(3) . . ? C1 N2 C16 114.9(4) . . ? C1 N2 C8 108.8(4) . . ? C16 N2 C8 111.2(4) . . ? C1 N2 Cd2 107.0(3) . . ? C16 N2 Cd2 106.3(3) . . ? C8 N2 Cd2 108.2(3) . . ? C5 N3 C32 112.3(4) . . ? C5 N3 C4 111.1(4) . . ? C32 N3 C4 105.3(4) . . ? C5 N3 Cd2 105.4(3) . . ? C32 N3 Cd2 116.7(3) . . ? C4 N3 Cd2 105.8(3) . . ? C7 N4 C6 108.9(4) . . ? C7 N4 C40 112.2(4) . . ? C6 N4 C40 113.9(4) . . ? C7 N4 Cd2 106.1(3) . . ? C6 N4 Cd2 106.3(3) . . ? C40 N4 Cd2 109.0(3) . . ? C9 O1 Cd1 91.6(4) . . ? C9 O2 Cd1 93.8(4) . . ? C17 O4 Cd1 105.6(5) . 2_655 ? C25 O5 Cd2 85.8(3) . 3_756 ? C25 O6 Cd2 98.1(3) . 3_756 ? C33 O7 Cd1 92.2(3) . 2_656 ? C33 O8 Cd1 90.6(3) . 2_656 ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 18.13 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 1.397 _refine_diff_density_min -1.569 _refine_diff_density_rms 0.120 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 -0.006 -0.006 -0.002 5124 3222 ' ' _platon_squeeze_details ; ;