# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_contact_author_name 'Jian-Fang Ma' _publ_contact_author_address ; Department of Chemistry Northeast Normal University Changchun 130024 P.R.China ; _publ_contact_author_email jianfangma@yahoo.com.cn _publ_contact_author_fax +86-431-85098620 _publ_contact_author_phone +86-431-85098620 _publ_author_name 'Jian-Fang Ma' #============================================================================= data_Compound-1 _database_code_depnum_ccdc_archive 'CCDC 857025' #TrackingRef 'CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H42 Co2 N8 O12, 4.25(H2O)' _chemical_formula_sum 'C50 H52.5 Co2 N8 O16.25' _chemical_formula_weight 1143.28 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'p 21/c' _symmetry_space_group_name_hall '-p 2ybc' 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 9.7419(6) _cell_length_b 18.7520(8) _cell_length_c 32.0657(15) _cell_angle_alpha 90.00 _cell_angle_beta 96.542(5) _cell_angle_gamma 90.00 _cell_volume 5819.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3886 _cell_measurement_theta_min 2.9 _cell_measurement_theta_max 25.0 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.293 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2328.0 _exptl_absorpt_coefficient_mu 0.640 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.890 _exptl_absorpt_correction_T_max 0.921 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36706 _diffrn_reflns_av_R_equivalents 0.1034 _diffrn_reflns_av_sigmaI/netI 0.1192 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 25.03 _reflns_number_total 10204 _reflns_number_gt 5168 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^)+(0.0579P)^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 10204 _refine_ls_number_parameters 757 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.1606 _refine_ls_R_factor_gt 0.0810 _refine_ls_wR_factor_ref 0.1965 _refine_ls_wR_factor_gt 0.1685 _refine_ls_goodness_of_fit_ref 1.185 _refine_ls_restrained_S_all 1.183 _refine_ls_shift/su_max 0.004 _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 C1 C 1.1229(7) 0.0625(3) 0.58543(18) 0.0576(17) Uani 1 1 d . . . H1 H 1.1188 0.0145 0.5782 0.069 Uiso 1 1 calc R . . C2 C 1.0702(7) 0.1711(3) 0.59159(18) 0.0597(17) Uani 1 1 d . . . H2 H 1.0209 0.2137 0.5900 0.072 Uiso 1 1 calc R . . C3 C 1.2021(8) 0.1637(3) 0.60853(18) 0.0620(18) Uani 1 1 d . . . H3 H 1.2600 0.1997 0.6202 0.074 Uiso 1 1 calc R . . C4 C 1.3602(7) 0.0571(3) 0.62096(17) 0.0557(16) Uani 1 1 d . . . H4A H 1.4378 0.0866 0.6154 0.067 Uiso 1 1 calc R . . H4B H 1.3656 0.0131 0.6054 0.067 Uiso 1 1 calc R . . C5 C 1.3756(7) 0.0389(3) 0.66903(16) 0.0503(15) Uani 1 1 d . . . C6 C 1.2524(7) -0.0047(3) 0.68169(18) 0.0603(17) Uani 1 1 d . . . H6A H 1.2564 -0.0034 0.7120 0.072 Uiso 1 1 calc R . . H6B H 1.1681 0.0195 0.6705 0.072 Uiso 1 1 calc R . . C7 C 1.235(3) -0.1110(10) 0.6299(6) 0.059(5) Uani 0.40 1 d PU . . C7' C 1.148(2) -0.1025(11) 0.6311(6) 0.101(6) Uani 0.60 1 d PU . . C8 C 1.239(3) -0.1856(18) 0.6367(12) 0.062(9) Uani 0.30 1 d PU . . C8' C 1.1619(17) -0.1767(8) 0.6348(5) 0.075(4) Uani 0.70 1 d PU . . C9 C 1.2606(8) -0.1348(3) 0.69343(19) 0.0655(19) Uani 1 1 d . . . H9 H 1.2961 -0.1316 0.7215 0.079 Uiso 1 1 calc R . . C10 C 1.3711(7) 0.1119(3) 0.69186(17) 0.0574(17) Uani 1 1 d . . . H10A H 1.4053 0.1481 0.6740 0.069 Uiso 1 1 calc R . . H10B H 1.2751 0.1231 0.6943 0.069 Uiso 1 1 calc R . . C11 C 1.4284(9) 0.0878(4) 0.7710(2) 0.091(3) Uani 1 1 d . . . H11 H 1.3582 0.0565 0.7762 0.109 Uiso 1 1 calc R . . C12 C 1.5314(10) 0.1122(4) 0.7993(2) 0.098(3) Uani 1 1 d . . . H12 H 1.5457 0.0984 0.8273 0.118 Uiso 1 1 calc R . . C13 C 1.5543(7) 0.1618(3) 0.74161(19) 0.0596(17) Uani 1 1 d . . . H13 H 1.5858 0.1913 0.7214 0.071 Uiso 1 1 calc R . . C14 C 1.5078(7) -0.0046(3) 0.68014(19) 0.0607(17) Uani 1 1 d . . . H14A H 1.5258 -0.0076 0.7105 0.073 Uiso 1 1 calc R . . H14B H 1.4916 -0.0527 0.6696 0.073 Uiso 1 1 calc R . . C15 C 1.7340(8) 0.0642(4) 0.6836(2) 0.0660(18) Uani 1 1 d . . . H15 H 1.7434 0.0793 0.7114 0.079 Uiso 1 1 calc R . . C16 C 1.8194(7) 0.0788(3) 0.6549(2) 0.0635(18) Uani 1 1 d . . . H16 H 1.8993 0.1061 0.6597 0.076 Uiso 1 1 calc R . . C17 C 1.6600(7) 0.0133(3) 0.6245(2) 0.0585(17) Uani 1 1 d . . . H17 H 1.6072 -0.0145 0.6047 0.070 Uiso 1 1 calc R . . C18 C 0.7548(7) 0.1872(4) 0.5279(2) 0.0636(18) Uani 1 1 d . . . C19 C 0.7458(7) 0.2565(3) 0.50584(19) 0.0553(16) Uani 1 1 d . . . C20 C 0.7337(8) 0.2590(3) 0.4626(2) 0.077(2) Uani 1 1 d . . . H20 H 0.7298 0.2168 0.4473 0.093 Uiso 1 1 calc R . . C21 C 0.7274(9) 0.3241(3) 0.44177(19) 0.081(2) Uani 1 1 d . . . H21 H 0.7214 0.3252 0.4126 0.098 Uiso 1 1 calc R . . C22 C 0.7301(7) 0.3859(3) 0.46380(18) 0.0583(17) Uani 1 1 d . . . C23 C 0.7444(7) 0.3843(3) 0.50703(19) 0.0639(18) Uani 1 1 d . . . H23 H 0.7505 0.4264 0.5224 0.077 Uiso 1 1 calc R . . C24 C 0.7498(7) 0.3190(3) 0.52725(19) 0.0622(18) Uani 1 1 d . . . H24 H 0.7563 0.3179 0.5564 0.075 Uiso 1 1 calc R . . C25 C 0.6939(7) 0.5120(3) 0.46108(17) 0.0607(18) Uani 1 1 d . . . H25A H 0.7765 0.5267 0.4787 0.073 Uiso 1 1 calc R . . H25B H 0.6201 0.5059 0.4787 0.073 Uiso 1 1 calc R . . C26 C 0.6547(7) 0.5671(3) 0.42850(17) 0.0531(16) Uani 1 1 d . . . C27 C 0.5321(8) 0.5434(3) 0.39787(18) 0.0653(19) Uani 1 1 d . . . H27A H 0.4937 0.5839 0.3817 0.078 Uiso 1 1 calc R . . H27B H 0.5616 0.5083 0.3786 0.078 Uiso 1 1 calc R . . C28 C 0.3113(8) 0.4871(3) 0.39926(19) 0.0643(19) Uani 1 1 d . . . C29 C 0.2659(8) 0.5066(4) 0.3597(2) 0.074(2) Uani 1 1 d . . . H29 H 0.3159 0.5390 0.3454 0.089 Uiso 1 1 calc R . . C30 C 0.1460(9) 0.4784(4) 0.3409(2) 0.081(2) Uani 1 1 d . . . H30 H 0.1150 0.4929 0.3137 0.097 Uiso 1 1 calc R . . C31 C 0.0678(8) 0.4294(3) 0.3600(2) 0.0660(19) Uani 1 1 d . . . C32 C 0.1165(9) 0.4095(4) 0.4004(2) 0.092(3) Uani 1 1 d . . . H32 H 0.0679 0.3762 0.4145 0.110 Uiso 1 1 calc R . . C33 C 0.2361(9) 0.4384(4) 0.41993(19) 0.091(3) Uani 1 1 d . . . H33 H 0.2671 0.4252 0.4473 0.109 Uiso 1 1 calc R . . C34 C -0.0539(9) 0.3956(4) 0.3373(2) 0.075(2) Uani 1 1 d . . . C35 C 0.6147(7) 0.6368(3) 0.44960(18) 0.0566(16) Uani 1 1 d . . . H35A H 0.5887 0.6730 0.4286 0.068 Uiso 1 1 calc R . . H35B H 0.5373 0.6286 0.4656 0.068 Uiso 1 1 calc R . . C36 C 0.7352(8) 0.7301(3) 0.48894(18) 0.0598(17) Uani 1 1 d . . . C37 C 0.6251(7) 0.7745(3) 0.48320(19) 0.0649(18) Uani 1 1 d . . . H37 H 0.5405 0.7580 0.4704 0.078 Uiso 1 1 calc R . . C38 C 0.6393(7) 0.8436(3) 0.49630(19) 0.0635(18) Uani 1 1 d . . . H38 H 0.5631 0.8738 0.4925 0.076 Uiso 1 1 calc R . . C39 C 0.7628(7) 0.8698(3) 0.51491(17) 0.0528(16) Uani 1 1 d . . . C40 C 0.8750(7) 0.8242(3) 0.51994(18) 0.0598(17) Uani 1 1 d . . . H40 H 0.9606 0.8409 0.5318 0.072 Uiso 1 1 calc R . . C41 C 0.8600(8) 0.7539(3) 0.50744(18) 0.0613(17) Uani 1 1 d . . . H41 H 0.9348 0.7229 0.5116 0.074 Uiso 1 1 calc R . . C42 C 0.7780(8) 0.9450(3) 0.52979(18) 0.0562(17) Uani 1 1 d . . . C43 C 0.7786(7) 0.5803(3) 0.40374(19) 0.0638(18) Uani 1 1 d . . . H43A H 0.8573 0.5971 0.4224 0.077 Uiso 1 1 calc R . . H43B H 0.8045 0.5364 0.3907 0.077 Uiso 1 1 calc R . . C44 C 0.8392(10) 0.6566(3) 0.3500(2) 0.068(2) Uani 1 1 d . . . C45 C 0.7919(9) 0.7022(4) 0.3163(2) 0.082(2) Uani 1 1 d . . . H45 H 0.6986 0.7135 0.3109 0.099 Uiso 1 1 calc R . . C46 C 0.8863(13) 0.7297(4) 0.2915(2) 0.098(3) Uani 1 1 d . . . H46 H 0.8558 0.7595 0.2692 0.118 Uiso 1 1 calc R . . C47 C 1.0260(12) 0.7134(4) 0.2993(3) 0.091(3) Uani 1 1 d . . . C48 C 1.0668(9) 0.6703(4) 0.3322(2) 0.087(2) Uani 1 1 d . . . H48 H 1.1602 0.6592 0.3376 0.105 Uiso 1 1 calc R . . C49 C 0.9763(10) 0.6416(4) 0.3581(2) 0.082(2) Uani 1 1 d . . . H49 H 1.0088 0.6127 0.3807 0.098 Uiso 1 1 calc R . . N1 N 1.0191(5) 0.1066(2) 0.57696(13) 0.0519(12) Uani 1 1 d . . . N2 N 1.2347(6) 0.0933(3) 0.60537(14) 0.0530(13) Uani 1 1 d . . . N3 N 1.2407(6) -0.0788(2) 0.66868(15) 0.0620(15) Uani 1 1 d . . . N4 N 1.2257(6) -0.1957(2) 0.67481(15) 0.0598(14) Uani 1 1 d . . . N5 N 1.4480(6) 0.1182(3) 0.73345(15) 0.0581(14) Uani 1 1 d . . . N6 N 1.6116(6) 0.1601(3) 0.78079(15) 0.0597(14) Uani 1 1 d . . . N7 N 1.6299(6) 0.0227(3) 0.66418(16) 0.0561(13) Uani 1 1 d . . . N8 N 1.7712(6) 0.0473(3) 0.61699(15) 0.0566(13) Uani 1 1 d . . . O1 O 0.7484(5) 0.1845(2) 0.56630(15) 0.0755(13) Uani 1 1 d U . . O2 O 0.7748(5) 0.1309(2) 0.50755(13) 0.0728(13) Uani 1 1 d . . . O1W O 0.5878(6) 0.0668(3) 0.44495(14) 0.0939(16) Uani 1 1 d . . . O3 O 0.7186(5) 0.4463(2) 0.44025(12) 0.0767(15) Uani 1 1 d . . . O2W O 1.5646(7) 0.2237(3) 0.62887(18) 0.126(2) Uani 1 1 d . . . O4 O 0.4294(5) 0.5131(2) 0.42141(12) 0.0708(13) Uani 1 1 d . . . O3W O 1.0722(8) 0.0922(5) 0.7363(2) 0.101(3) Uani 0.70 1 d P . . O5 O -0.1074(6) 0.4220(3) 0.30315(18) 0.1034(18) Uani 1 1 d . . . O4W O 1.421(2) -0.1558(13) 0.8160(7) 0.139(9) Uani 0.30 1 d P . . O6 O -0.1026(5) 0.3389(2) 0.35081(12) 0.0784(15) Uani 1 1 d . . . O5W O 1.7090(15) -0.0370(6) 0.7751(3) 0.119(4) Uani 0.50 1 d P . . O7 O 0.7333(5) 0.6588(2) 0.47671(13) 0.0663(12) Uani 1 1 d . . . O6W O 1.720(3) -0.1982(13) 0.6562(7) 0.122(8) Uani 0.25 1 d PU . . O8 O 0.6711(5) 0.9831(2) 0.53111(12) 0.0613(11) Uani 1 1 d . . . O7W O 1.4400(13) 0.5906(5) 0.2835(3) 0.101(4) Uani 0.50 1 d P . . O9 O 0.8956(5) 0.9689(2) 0.54265(13) 0.0657(12) Uani 1 1 d . . . O10 O 0.7387(5) 0.6327(2) 0.37237(13) 0.0722(13) Uani 1 1 d . . . Co1 Co 0.82793(9) 0.06744(4) 0.55849(2) 0.0522(3) Uani 1 1 d . . . Co2 Co 1.20731(10) 0.79417(4) 0.19961(2) 0.0571(3) Uani 1 1 d . . . C50 C 1.098(3) 0.7431(17) 0.2645(9) 0.056(7) Uani 0.50 1 d PU . . O11 O 1.111(2) 0.7778(14) 0.2449(8) 0.092(7) Uani 0.50 1 d PU . . O12' O 1.225(3) 0.7263(13) 0.2687(6) 0.082(6) Uani 0.50 1 d PU . . O12 O 1.272(2) 0.7215(11) 0.2875(5) 0.092(6) Uani 0.50 1 d PU . . C50' C 1.153(3) 0.7406(18) 0.2756(9) 0.062(9) Uani 0.50 1 d PU . . O11' O 1.0456(18) 0.7835(12) 0.2356(6) 0.076(5) Uani 0.50 1 d PU . . 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 C1 0.056(5) 0.034(4) 0.081(4) -0.010(3) -0.001(4) -0.005(4) C2 0.059(5) 0.032(4) 0.084(4) -0.003(3) -0.012(4) -0.007(3) C3 0.059(5) 0.032(4) 0.089(4) -0.003(3) -0.017(4) -0.010(3) C4 0.049(5) 0.048(4) 0.070(4) -0.002(3) 0.003(3) 0.000(3) C5 0.053(5) 0.042(3) 0.057(3) 0.004(3) 0.009(3) -0.006(3) C6 0.062(5) 0.045(4) 0.076(4) -0.002(3) 0.015(3) -0.004(3) C7 0.098(15) 0.039(9) 0.041(9) 0.012(6) 0.015(10) 0.009(11) C7' 0.101(13) 0.086(11) 0.112(11) 0.025(8) -0.002(11) -0.022(11) C8 0.080(18) 0.037(13) 0.070(15) 0.013(10) 0.018(15) -0.005(14) C8' 0.107(12) 0.045(7) 0.067(7) 0.011(5) -0.012(9) -0.022(9) C9 0.076(6) 0.049(4) 0.067(4) 0.005(3) -0.013(4) -0.005(4) C10 0.061(5) 0.042(4) 0.069(4) 0.006(3) 0.005(3) -0.006(3) C11 0.111(8) 0.082(5) 0.080(5) 0.012(4) 0.022(5) -0.048(5) C12 0.134(9) 0.093(6) 0.062(4) 0.009(4) -0.012(5) -0.043(6) C13 0.069(5) 0.046(4) 0.062(4) 0.007(3) 0.000(4) -0.007(4) C14 0.059(5) 0.048(4) 0.076(4) 0.010(3) 0.011(3) 0.000(4) C15 0.062(5) 0.069(4) 0.065(4) -0.009(3) -0.004(4) -0.003(4) C16 0.051(5) 0.067(4) 0.072(4) -0.012(3) 0.001(4) -0.012(4) C17 0.047(5) 0.051(4) 0.075(5) -0.006(3) -0.002(3) -0.004(3) C18 0.047(5) 0.062(5) 0.079(5) 0.005(4) -0.004(4) 0.000(4) C19 0.054(5) 0.042(4) 0.070(4) 0.003(3) 0.007(3) -0.001(3) C20 0.108(7) 0.044(4) 0.080(5) -0.006(3) 0.010(4) 0.006(4) C21 0.141(8) 0.041(4) 0.066(4) -0.003(3) 0.023(4) 0.012(4) C22 0.081(6) 0.036(4) 0.061(4) 0.001(3) 0.022(3) -0.001(3) C23 0.078(6) 0.043(4) 0.072(4) -0.005(3) 0.012(4) -0.002(3) C24 0.075(5) 0.051(4) 0.063(4) 0.000(3) 0.016(3) -0.005(4) C25 0.082(6) 0.030(3) 0.072(4) -0.004(3) 0.018(4) -0.005(3) C26 0.063(5) 0.031(3) 0.067(4) -0.010(3) 0.015(3) -0.009(3) C27 0.088(6) 0.044(4) 0.067(4) -0.006(3) 0.023(4) -0.015(4) C28 0.076(6) 0.061(4) 0.058(4) -0.018(3) 0.015(4) -0.015(4) C29 0.070(6) 0.078(5) 0.073(5) 0.010(4) 0.003(4) -0.023(4) C30 0.090(7) 0.077(5) 0.074(4) 0.019(4) 0.010(4) -0.015(5) C31 0.072(5) 0.061(4) 0.066(4) -0.012(3) 0.011(4) -0.017(4) C32 0.115(8) 0.096(6) 0.063(5) -0.001(4) 0.009(4) -0.062(5) C33 0.120(8) 0.102(6) 0.049(4) 0.012(4) 0.003(4) -0.061(6) C34 0.090(7) 0.074(5) 0.062(4) -0.008(4) 0.011(4) -0.013(5) C35 0.052(5) 0.043(4) 0.074(4) -0.006(3) 0.002(3) -0.007(3) C36 0.061(5) 0.043(4) 0.076(4) -0.011(3) 0.011(4) -0.009(4) C37 0.046(5) 0.051(4) 0.095(5) -0.017(3) 0.000(4) -0.001(4) C38 0.048(5) 0.042(4) 0.099(5) -0.016(3) -0.001(4) -0.001(3) C39 0.054(5) 0.042(4) 0.063(4) -0.007(3) 0.011(3) -0.008(3) C40 0.044(5) 0.048(4) 0.085(4) -0.013(3) -0.001(3) -0.010(3) C41 0.058(5) 0.043(4) 0.080(4) -0.009(3) -0.003(4) 0.001(4) C42 0.064(6) 0.040(4) 0.064(4) -0.001(3) 0.003(4) 0.000(4) C43 0.078(6) 0.041(4) 0.076(4) 0.005(3) 0.023(4) -0.001(3) C44 0.086(7) 0.047(4) 0.073(5) -0.001(3) 0.018(4) -0.012(4) C45 0.103(7) 0.059(5) 0.087(5) 0.003(4) 0.021(5) -0.011(4) C46 0.166(11) 0.060(5) 0.076(5) 0.003(4) 0.047(6) -0.024(6) C47 0.134(9) 0.054(5) 0.098(6) -0.013(4) 0.065(6) -0.020(5) C48 0.092(7) 0.070(5) 0.106(6) 0.003(4) 0.037(5) -0.011(5) C49 0.097(8) 0.069(5) 0.084(5) 0.007(4) 0.030(5) -0.015(5) N1 0.047(4) 0.033(3) 0.073(3) -0.004(2) -0.002(3) -0.004(3) N2 0.044(4) 0.046(3) 0.067(3) -0.003(2) -0.004(3) -0.001(3) N3 0.083(5) 0.038(3) 0.066(3) -0.005(2) 0.014(3) -0.022(3) N4 0.075(4) 0.038(3) 0.067(3) -0.003(2) 0.010(3) -0.010(3) N5 0.061(4) 0.048(3) 0.063(3) 0.002(2) -0.005(3) -0.014(3) N6 0.065(4) 0.049(3) 0.063(3) 0.002(2) -0.002(3) -0.013(3) N7 0.047(4) 0.052(3) 0.068(3) 0.005(2) 0.000(3) 0.003(3) N8 0.047(4) 0.051(3) 0.071(3) -0.002(2) 0.003(3) -0.006(3) O1 0.071(4) 0.070(3) 0.085(3) 0.020(2) 0.008(3) 0.012(3) O2 0.076(4) 0.044(3) 0.092(3) 0.002(2) -0.015(3) -0.003(2) O1W 0.098(4) 0.098(4) 0.085(3) -0.029(3) 0.012(3) -0.017(3) O3 0.131(5) 0.034(3) 0.072(3) -0.0004(19) 0.041(3) 0.006(3) O2W 0.109(5) 0.130(5) 0.144(5) 0.033(4) 0.034(4) 0.018(4) O4 0.081(4) 0.071(3) 0.063(3) -0.012(2) 0.023(3) -0.036(3) O3W 0.081(6) 0.147(7) 0.078(4) -0.008(4) 0.017(4) 0.020(5) O5 0.087(5) 0.117(5) 0.104(4) 0.012(3) -0.001(3) -0.033(4) O4W 0.070(15) 0.17(2) 0.171(19) -0.117(17) -0.009(13) 0.024(14) O6 0.103(4) 0.062(3) 0.069(3) -0.006(2) 0.004(3) -0.031(3) O5W 0.173(13) 0.094(8) 0.086(7) 0.005(5) 0.000(7) 0.030(8) O7 0.063(3) 0.042(3) 0.091(3) -0.009(2) -0.004(2) -0.004(2) O6W 0.122(8) 0.122(8) 0.122(8) 0.0005(10) 0.0140(13) 0.0004(10) O8 0.057(3) 0.041(2) 0.083(3) -0.0079(19) -0.004(2) 0.000(2) O7W 0.155(12) 0.070(7) 0.066(6) 0.005(5) -0.036(6) 0.008(7) O9 0.052(3) 0.043(2) 0.100(3) -0.019(2) 0.003(3) -0.014(2) O10 0.073(4) 0.059(3) 0.086(3) 0.019(2) 0.017(3) -0.007(3) Co1 0.0478(6) 0.0354(5) 0.0714(5) -0.0015(3) -0.0022(4) -0.0032(4) Co2 0.0685(7) 0.0426(5) 0.0590(5) 0.0002(3) 0.0024(4) 0.0029(4) C50 0.059(14) 0.048(10) 0.064(13) -0.011(9) 0.013(11) -0.005(11) O11 0.109(16) 0.070(10) 0.096(11) 0.008(8) 0.010(11) 0.001(12) O12' 0.082(14) 0.086(10) 0.080(11) 0.002(9) 0.022(10) -0.020(9) O12 0.099(14) 0.075(8) 0.106(12) -0.008(9) 0.033(9) -0.022(9) C50' 0.066(18) 0.051(11) 0.070(15) -0.022(10) 0.009(14) -0.011(13) O11' 0.095(12) 0.069(8) 0.071(9) 0.019(7) 0.042(9) 0.016(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N1 1.311(7) . ? C1 N2 1.330(7) . ? C2 C3 1.344(8) . ? C2 N1 1.370(7) . ? C3 N2 1.365(7) . ? C4 N2 1.437(7) . ? C4 C5 1.569(7) . ? C5 C14 1.532(8) . ? C5 C6 1.545(8) . ? C5 C10 1.556(8) . ? C6 N3 1.452(7) . ? C7 C7' 0.87(2) . ? C7 N3 1.378(19) . ? C7 C8 1.41(4) . ? C7 C8' 1.44(3) . ? C7' C8' 1.40(2) . ? C7' N3 1.488(19) . ? C7' C8 1.79(4) . ? C8 C8' 0.77(3) . ? C8 N4 1.26(4) . ? C8 C9 2.04(4) . ? C8' N4 1.408(15) . ? C9 N4 1.314(7) . ? C9 N3 1.317(7) . ? C10 N5 1.458(7) . ? C11 C12 1.353(10) . ? C11 N5 1.367(7) . ? C12 N6 1.369(9) . ? C13 N6 1.316(7) . ? C13 N5 1.322(8) . ? C14 N7 1.441(8) . ? C15 C16 1.337(8) . ? C15 N7 1.369(8) . ? C16 N8 1.385(7) . ? C17 N8 1.303(7) . ? C17 N7 1.349(7) . ? C18 O1 1.240(7) . ? C18 O2 1.267(7) . ? C18 C19 1.478(8) . ? C18 Co1 2.519(7) . ? C19 C24 1.357(8) . ? C19 C20 1.378(8) . ? C20 C21 1.390(8) . ? C21 C22 1.356(8) . ? C22 O3 1.358(6) . ? C22 C23 1.378(7) . ? C23 C24 1.383(8) . ? C25 O3 1.436(6) . ? C25 C26 1.488(8) . ? C26 C27 1.524(9) . ? C26 C43 1.539(8) . ? C26 C35 1.541(7) . ? C27 O4 1.437(7) . ? C28 C29 1.346(8) . ? C28 O4 1.371(8) . ? C28 C33 1.386(8) . ? C29 C30 1.360(9) . ? C30 C31 1.382(9) . ? C31 C32 1.380(9) . ? C31 C34 1.462(10) . ? C32 C33 1.370(10) . ? C34 O5 1.260(8) . ? C34 O6 1.262(8) . ? C35 O7 1.426(7) . ? C36 C37 1.354(8) . ? C36 C41 1.366(9) . ? C36 O7 1.392(7) . ? C37 C38 1.365(8) . ? C38 C39 1.372(8) . ? C39 C40 1.383(8) . ? C39 C42 1.489(8) . ? C40 C41 1.380(8) . ? C42 O9 1.256(7) . ? C42 O8 1.268(7) . ? C42 Co1 2.501(6) 1_565 ? C43 O10 1.428(7) . ? C44 O10 1.354(8) . ? C44 C49 1.362(10) . ? C44 C45 1.412(10) . ? C45 C46 1.382(11) . ? C46 C47 1.389(12) . ? C47 C48 1.351(11) . ? C47 C50 1.49(3) . ? C47 C50' 1.61(4) . ? C48 C49 1.388(9) . ? N1 Co1 2.026(5) . ? N4 Co2 2.027(5) 4_566 ? N6 Co2 1.997(5) 3_866 ? N8 Co1 2.050(5) 1_655 ? O1 Co1 2.351(4) . ? O2 Co1 2.040(4) . ? O4W O7W 1.63(3) 4_566 ? O6 Co2 1.995(4) 2_645 ? O8 Co1 2.302(4) 1_565 ? O7W O4W 1.63(3) 4_565 ? O9 Co1 2.046(4) 1_565 ? Co1 O9 2.046(4) 1_545 ? Co1 N8 2.050(5) 1_455 ? Co1 O8 2.302(4) 1_545 ? Co1 C42 2.501(6) 1_545 ? Co2 O11 1.84(3) . ? Co2 O6 1.995(4) 2_655 ? Co2 N6 1.997(5) 3_866 ? Co2 N4 2.027(5) 4_565 ? Co2 O11' 2.066(17) . ? C50 C50' 0.61(4) . ? C50 O11 0.92(3) . ? C50 O11' 1.26(4) . ? C50 O12' 1.27(4) . ? C50 O12 1.81(3) . ? O11 O11' 0.68(3) . ? O11 C50' 1.24(4) . ? O11 O12' 1.60(3) . ? O12' O12 0.72(2) . ? O12' C50' 0.80(3) . ? O12 C50' 1.22(4) . ? C50' O11' 1.76(4) . ? 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 N1 C1 N2 113.3(5) . . ? C3 C2 N1 109.9(6) . . ? C2 C3 N2 106.9(5) . . ? N2 C4 C5 115.3(5) . . ? C14 C5 C6 108.4(5) . . ? C14 C5 C10 115.3(5) . . ? C6 C5 C10 106.1(5) . . ? C14 C5 C4 109.2(4) . . ? C6 C5 C4 112.5(5) . . ? C10 C5 C4 105.4(4) . . ? N3 C6 C5 118.0(5) . . ? C7' C7 N3 79(2) . . ? C7' C7 C8 101(3) . . ? N3 C7 C8 107.3(19) . . ? C7' C7 C8' 70(2) . . ? N3 C7 C8' 104.2(13) . . ? C8 C7 C8' 31.1(13) . . ? C7 C7' C8' 75(2) . . ? C7 C7' N3 66(2) . . ? C8' C7' N3 100.7(13) . . ? C7 C7' C8 51(2) . . ? C8' C7' C8 24.0(13) . . ? N3 C7' C8 86.1(16) . . ? C8' C8 N4 84(4) . . ? C8' C8 C7 76(4) . . ? N4 C8 C7 107(3) . . ? C8' C8 C7' 48(3) . . ? N4 C8 C7' 97(2) . . ? C7 C8 C7' 28.4(12) . . ? C8' C8 C9 88(4) . . ? N4 C8 C9 38.4(11) . . ? C7 C8 C9 71.0(17) . . ? C7' C8 C9 71.5(14) . . ? C8 C8' C7' 108(4) . . ? C8 C8' N4 63(3) . . ? C7' C8' N4 110.8(13) . . ? C8 C8' C7 73(4) . . ? C7' C8' C7 35.5(10) . . ? N4 C8' C7 98.2(13) . . ? N4 C9 N3 113.9(5) . . ? N4 C9 C8 36.5(10) . . ? N3 C9 C8 80.9(10) . . ? N5 C10 C5 117.6(5) . . ? C12 C11 N5 106.3(6) . . ? C11 C12 N6 110.4(6) . . ? N6 C13 N5 114.3(5) . . ? N7 C14 C5 115.7(5) . . ? C16 C15 N7 106.9(6) . . ? C15 C16 N8 109.9(6) . . ? N8 C17 N7 112.6(6) . . ? O1 C18 O2 120.5(6) . . ? O1 C18 C19 120.2(6) . . ? O2 C18 C19 119.2(6) . . ? O1 C18 Co1 67.8(3) . . ? O2 C18 Co1 53.6(3) . . ? C19 C18 Co1 165.6(5) . . ? C24 C19 C20 118.3(5) . . ? C24 C19 C18 121.4(6) . . ? C20 C19 C18 120.4(6) . . ? C19 C20 C21 120.5(6) . . ? C22 C21 C20 120.2(6) . . ? C21 C22 O3 115.3(5) . . ? C21 C22 C23 119.9(5) . . ? O3 C22 C23 124.8(5) . . ? C22 C23 C24 119.0(5) . . ? C19 C24 C23 122.0(6) . . ? O3 C25 C26 108.2(4) . . ? C25 C26 C27 111.7(5) . . ? C25 C26 C43 108.7(6) . . ? C27 C26 C43 108.5(5) . . ? C25 C26 C35 109.7(5) . . ? C27 C26 C35 108.1(5) . . ? C43 C26 C35 110.1(5) . . ? O4 C27 C26 108.5(5) . . ? C29 C28 O4 123.9(6) . . ? C29 C28 C33 119.7(7) . . ? O4 C28 C33 116.4(6) . . ? C28 C29 C30 119.1(6) . . ? C29 C30 C31 123.4(7) . . ? C32 C31 C30 116.7(7) . . ? C32 C31 C34 121.5(6) . . ? C30 C31 C34 121.5(7) . . ? C33 C32 C31 120.3(6) . . ? C32 C33 C28 120.8(6) . . ? O5 C34 O6 119.6(7) . . ? O5 C34 C31 119.7(7) . . ? O6 C34 C31 120.6(7) . . ? O7 C35 C26 106.6(5) . . ? C37 C36 C41 120.7(6) . . ? C37 C36 O7 124.6(6) . . ? C41 C36 O7 114.8(6) . . ? C36 C37 C38 119.4(7) . . ? C37 C38 C39 121.8(7) . . ? C38 C39 C40 118.1(5) . . ? C38 C39 C42 121.9(6) . . ? C40 C39 C42 120.0(6) . . ? C41 C40 C39 120.1(6) . . ? C36 C41 C40 119.9(6) . . ? O9 C42 O8 120.7(6) . . ? O9 C42 C39 119.8(6) . . ? O8 C42 C39 119.5(7) . . ? O9 C42 Co1 54.5(3) . 1_565 ? O8 C42 Co1 66.2(3) . 1_565 ? C39 C42 Co1 174.0(6) . 1_565 ? O10 C43 C26 107.9(5) . . ? O10 C44 C49 125.6(7) . . ? O10 C44 C45 114.4(8) . . ? C49 C44 C45 119.9(7) . . ? C46 C45 C44 119.0(9) . . ? C45 C46 C47 121.1(8) . . ? C48 C47 C46 117.9(8) . . ? C48 C47 C50 133.2(15) . . ? C46 C47 C50 108.4(14) . . ? C48 C47 C50' 112.5(15) . . ? C46 C47 C50' 129.5(14) . . ? C50 C47 C50' 22.4(14) . . ? C47 C48 C49 123.2(9) . . ? C44 C49 C48 118.8(8) . . ? C1 N1 C2 104.1(5) . . ? C1 N1 Co1 119.6(4) . . ? C2 N1 Co1 134.9(5) . . ? C1 N2 C3 105.7(5) . . ? C1 N2 C4 125.4(5) . . ? C3 N2 C4 128.8(6) . . ? C9 N3 C7 100.5(9) . . ? C9 N3 C6 126.1(5) . . ? C7 N3 C6 132.3(9) . . ? C9 N3 C7' 106.5(8) . . ? C7 N3 C7' 34.9(9) . . ? C6 N3 C7' 122.6(9) . . ? C8 N4 C9 105.1(17) . . ? C8 N4 C8' 32.8(14) . . ? C9 N4 C8' 105.0(7) . . ? C8 N4 Co2 122.8(16) . 4_566 ? C9 N4 Co2 130.0(4) . 4_566 ? C8' N4 Co2 122.6(7) . 4_566 ? C13 N5 C11 105.6(5) . . ? C13 N5 C10 122.7(5) . . ? C11 N5 C10 131.6(6) . . ? C13 N6 C12 103.2(6) . . ? C13 N6 Co2 123.6(4) . 3_866 ? C12 N6 Co2 132.3(5) . 3_866 ? C17 N7 C15 105.9(5) . . ? C17 N7 C14 124.4(6) . . ? C15 N7 C14 129.7(6) . . ? C17 N8 C16 104.6(5) . . ? C17 N8 Co1 125.2(4) . 1_655 ? C16 N8 Co1 128.7(5) . 1_655 ? C18 O1 Co1 82.9(4) . . ? C18 O2 Co1 96.5(4) . . ? C22 O3 C25 117.7(4) . . ? C28 O4 C27 117.5(5) . . ? C34 O6 Co2 104.7(4) . 2_645 ? C36 O7 C35 115.7(5) . . ? C42 O8 Co1 83.6(4) . 1_565 ? C42 O9 Co1 95.5(4) . 1_565 ? C44 O10 C43 116.5(6) . . ? N1 Co1 O2 99.41(19) . . ? N1 Co1 O9 95.08(19) . 1_545 ? O2 Co1 O9 112.84(18) . 1_545 ? N1 Co1 N8 97.7(2) . 1_455 ? O2 Co1 N8 140.3(2) . 1_455 ? O9 Co1 N8 100.90(18) 1_545 1_455 ? N1 Co1 O8 155.28(18) . 1_545 ? O2 Co1 O8 89.92(16) . 1_545 ? O9 Co1 O8 60.24(17) 1_545 1_545 ? N8 Co1 O8 89.20(18) 1_455 1_545 ? N1 Co1 O1 86.18(19) . . ? O2 Co1 O1 58.90(16) . . ? O9 Co1 O1 171.72(17) 1_545 . ? N8 Co1 O1 87.01(18) 1_455 . ? O8 Co1 O1 118.00(17) 1_545 . ? N1 Co1 C42 125.0(2) . 1_545 ? O2 Co1 C42 102.73(18) . 1_545 ? O9 Co1 C42 29.98(19) 1_545 1_545 ? N8 Co1 C42 96.10(19) 1_455 1_545 ? O8 Co1 C42 30.26(18) 1_545 1_545 ? O1 Co1 C42 147.6(2) . 1_545 ? N1 Co1 C18 90.0(2) . . ? O2 Co1 C18 29.98(18) . . ? O9 Co1 C18 142.5(2) 1_545 . ? N8 Co1 C18 115.2(2) 1_455 . ? O8 Co1 C18 108.53(19) 1_545 . ? O1 Co1 C18 29.23(16) . . ? C42 Co1 C18 129.8(2) 1_545 . ? O11 Co2 O6 116.7(6) . 2_655 ? O11 Co2 N6 109.5(7) . 3_866 ? O6 Co2 N6 115.2(2) 2_655 3_866 ? O11 Co2 N4 103.5(8) . 4_565 ? O6 Co2 N4 97.2(2) 2_655 4_565 ? N6 Co2 N4 113.6(2) 3_866 4_565 ? O11 Co2 O11' 18.9(8) . . ? O6 Co2 O11' 98.1(5) 2_655 . ? N6 Co2 O11' 124.6(6) 3_866 . ? N4 Co2 O11' 103.8(7) 4_565 . ? C50' C50 O11 106(6) . . ? C50' C50 O11' 137(7) . . ? O11 C50 O11' 32(2) . . ? C50' C50 O12' 30(4) . . ? O11 C50 O12' 92(3) . . ? O11' C50 O12' 123(3) . . ? C50' C50 C47 90(6) . . ? O11 C50 C47 152(3) . . ? O11' C50 C47 126(2) . . ? O12' C50 C47 111(2) . . ? C50' C50 O12 14(4) . . ? O11 C50 O12 104(3) . . ? O11' C50 O12 136(2) . . ? O12' C50 O12 17.8(13) . . ? C47 C50 O12 96.1(19) . . ? O11' O11 C50 102(5) . . ? O11' O11 C50' 130(5) . . ? C50 O11 C50' 29(2) . . ? O11' O11 O12' 150(5) . . ? C50 O11 O12' 52(2) . . ? C50' O11 O12' 29.5(16) . . ? O11' O11 Co2 99(4) . . ? C50 O11 Co2 141(3) . . ? C50' O11 Co2 124(2) . . ? O12' O11 Co2 95.0(14) . . ? O12 O12' C50' 107(5) . . ? O12 O12' C50 130(4) . . ? C50' O12' C50 23(3) . . ? O12 O12' O11 145(4) . . ? C50' O12' O11 49(3) . . ? C50 O12' O11 35.1(16) . . ? O12' O12 C50' 39(3) . . ? O12' O12 C50 33(3) . . ? C50' O12 C50 7(2) . . ? C50 C50' O12' 127(7) . . ? C50 C50' O12 159(7) . . ? O12' C50' O12 34(2) . . ? C50 C50' O11 46(5) . . ? O12' C50' O11 101(4) . . ? O12 C50' O11 129(3) . . ? C50 C50' C47 68(5) . . ? O12' C50' C47 140(4) . . ? O12 C50' C47 121(3) . . ? O11 C50' C47 110(3) . . ? C50 C50' O11' 29(5) . . ? O12' C50' O11' 115(4) . . ? O12 C50' O11' 145(3) . . ? O11 C50' O11' 17.1(18) . . ? C47 C50' O11' 93.5(18) . . ? O11 O11' C50 46(4) . . ? O11 O11' C50' 32(4) . . ? C50 O11' C50' 14(2) . . ? O11 O11' Co2 62(3) . . ? C50 O11' Co2 101.4(16) . . ? C50' O11' Co2 91.2(13) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.860 _refine_diff_density_min -0.329 _refine_diff_density_rms 0.081 #=========================END data_Compound-2 _database_code_depnum_ccdc_archive 'CCDC 857026' #TrackingRef 'CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C25 H22 Cd N4 O6), 4(C0.75 H1.5 N0.25 O0.25), 4(H2 O)' _chemical_formula_sum 'C103 H102 Cd4 N17 O29' _chemical_formula_weight 2491.48 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 Monoclinic _symmetry_space_group_name_H-M 'p 2/c' _symmetry_space_group_name_hall '-p 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 9.8633(3) _cell_length_b 16.4409(6) _cell_length_c 18.2187(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.197(3) _cell_angle_gamma 90.00 _cell_volume 2946.45(17) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4329 _cell_measurement_theta_min 2.9 _cell_measurement_theta_max 25.4 _exptl_crystal_description block _exptl_crystal_colour colorness _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1241 _exptl_absorpt_coefficient_mu 0.788 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.833 _exptl_absorpt_correction_T_max 0.855 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11808 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 25.35 _reflns_number_total 5399 _reflns_number_gt 4160 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^)+(0.0903P)^2^+7.1862P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5351 _refine_ls_number_parameters 379 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0774 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1755 _refine_ls_wR_factor_gt 0.1613 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.000 _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 C1 C 0.2127(7) 0.5692(4) 0.4769(4) 0.0490(15) Uani 1 1 d . . . C2 C 0.2577(6) 0.6454(4) 0.4413(4) 0.0514(15) Uani 1 1 d . . . C3 C 0.1910(7) 0.6785(5) 0.3819(5) 0.066(2) Uani 1 1 d . . . H3 H 0.1084 0.6570 0.3630 0.079 Uiso 1 1 calc R . . C4 C 0.2490(10) 0.7480(5) 0.3477(5) 0.089(3) Uani 1 1 d . . . H4 H 0.2051 0.7739 0.3072 0.107 Uiso 1 1 calc R . . C5 C 0.3784(8) 0.7749(5) 0.3796(6) 0.080(3) Uani 1 1 d . . . C6 C 0.4394(12) 0.7431(7) 0.4376(7) 0.119(4) Uani 1 1 d . . . H6 H 0.5230 0.7628 0.4568 0.143 Uiso 1 1 calc R . . C7 C 0.3800(9) 0.6816(6) 0.4691(6) 0.092(3) Uani 1 1 d . . . H7 H 0.4218 0.6609 0.5125 0.110 Uiso 1 1 calc R . . C8 C 0.3886(9) 0.8696(7) 0.2864(4) 0.094(3) Uani 1 1 d . . . H8A H 0.3110 0.9003 0.3011 0.113 Uiso 1 1 calc R . . H8B H 0.3567 0.8283 0.2512 0.113 Uiso 1 1 calc R . . C9 C 0.5000 0.9309(5) 0.2500 0.0425(18) Uani 1 2 d S . . C10 C 0.5756(9) 0.9836(5) 0.3084(5) 0.076(2) Uani 1 1 d . . . H10A H 0.5115 1.0140 0.3356 0.091 Uiso 1 1 calc R . . H10B H 0.6302 0.9498 0.3428 0.091 Uiso 1 1 calc R . . C11 C 0.7252(10) 1.0982(5) 0.3133(5) 0.078(2) Uani 1 1 d . . . C12' C 0.7251(15) 1.1058(8) 0.3860(7) 0.074(3) Uani 0.70 1 d P . . C12 C 0.819(5) 1.0708(19) 0.377(2) 0.101(12) Uani 0.30 1 d P . . C13 C 0.8048(15) 1.1701(9) 0.4233(7) 0.109(5) Uani 0.80 1 d P . . C13' C 0.912(6) 1.1520(15) 0.401(3) 0.112(16) Uani 0.20 1 d PDU . . C14 C 0.8686(8) 1.2245(5) 0.3822(5) 0.071(2) Uani 1 1 d D . . C15 C 0.8419(12) 1.2212(6) 0.3078(6) 0.105(4) Uani 1 1 d . . . H15 H 0.8722 1.2632 0.2790 0.127 Uiso 1 1 calc R . . C16 C 0.7721(13) 1.1579(6) 0.2745(5) 0.110(4) Uani 1 1 d . . . H16 H 0.7574 1.1571 0.2235 0.132 Uiso 1 1 calc R . . C17 C 0.9504(8) 1.2905(6) 0.4201(5) 0.073(2) Uani 1 1 d . . . C18 C 0.3759(6) 0.4186(4) 0.4078(3) 0.0476(15) Uani 1 1 d . . . H18 H 0.3951 0.4690 0.4293 0.057 Uiso 1 1 calc R . . C19 C 0.2864(9) 0.3033(5) 0.3830(5) 0.077(2) Uani 1 1 d . . . H19 H 0.2298 0.2581 0.3834 0.092 Uiso 1 1 calc R . . C20 C 0.3883(8) 0.3137(5) 0.3369(4) 0.070(2) Uani 1 1 d . . . H20 H 0.4151 0.2771 0.3019 0.085 Uiso 1 1 calc R . . C21 C 0.5490(6) 0.4306(4) 0.3176(3) 0.0494(15) Uani 1 1 d . . . H21A H 0.6144 0.3913 0.3023 0.059 Uiso 1 1 calc R . . H21B H 0.5957 0.4656 0.3541 0.059 Uiso 1 1 calc R . . C22 C 0.5000 0.4833(6) 0.2500 0.047(2) Uani 1 2 d S . . C23 C 0.6242(7) 0.5349(5) 0.2307(3) 0.0603(18) Uani 1 1 d . . . H23A H 0.6932 0.4985 0.2143 0.072 Uiso 1 1 calc R . . H23B H 0.5961 0.5704 0.1899 0.072 Uiso 1 1 calc R . . C24 C 0.6457(10) 0.6614(5) 0.3139(5) 0.096(3) Uani 1 1 d . . . H24 H 0.5750 0.6931 0.2928 0.116 Uiso 1 1 calc R . . C25 C 0.7883(6) 0.5635(5) 0.3375(4) 0.0552(16) Uani 1 1 d . . . H25 H 0.8353 0.5147 0.3347 0.066 Uiso 1 1 calc R . . C26 C 0.7279(9) 0.6803(5) 0.3715(5) 0.083(3) Uani 1 1 d . . . H26 H 0.7260 0.7288 0.3975 0.099 Uiso 1 1 calc R . . C27 C -0.067(3) 0.8710(14) 0.3936(15) 0.069(9) Uani 0.25 1 d PD . . C28 C 0.088(5) 1.009(3) 0.381(3) 0.120(15) Uiso 0.25 1 d P . . C29 C 0.020(4) 0.936(2) 0.2768(18) 0.078(9) Uiso 0.25 1 d P . . N1 N 0.2800(5) 0.3685(4) 0.4280(3) 0.0525(13) Uani 1 1 d . . . N2 N 0.4417(5) 0.3872(4) 0.3523(3) 0.0501(13) Uani 1 1 d . . . N3 N 0.6852(6) 0.5847(4) 0.2908(3) 0.0560(14) Uani 1 1 d . . . N4 N 0.8164(5) 0.6180(3) 0.3874(3) 0.0506(13) Uani 1 1 d . . . N5 N 0.010(3) 0.9319(16) 0.3445(14) 0.071(7) Uiso 0.25 1 d PD . . O1 O 0.2894(5) 0.5349(3) 0.5245(3) 0.0679(13) Uani 1 1 d . . . O2 O 0.0978(4) 0.5395(3) 0.4538(2) 0.0497(10) Uani 1 1 d . . . O1W O 1.0000 0.437(2) 0.2500 0.153(10) Uiso 0.50 2 d SP . . O1W' O 0.900(3) 0.4199(16) 0.2447(15) 0.090(7) Uiso 0.25 1 d P . . O3 O 0.4545(6) 0.8358(4) 0.3443(4) 0.103(2) Uani 1 1 d . . . O2W O 0.412(2) 1.0087(16) 0.4809(14) 0.190(9) Uiso 0.50 1 d P . . O4 O 0.6582(7) 1.0363(4) 0.2721(3) 0.0876(18) Uani 1 1 d . . . O5 O 0.9562(6) 1.3586(4) 0.3884(4) 0.0861(17) Uani 1 1 d . . . O6 O 1.0081(7) 1.2781(4) 0.4806(3) 0.093(2) Uani 1 1 d . . . O7 O -0.028(3) 0.8851(18) 0.2333(17) 0.104(9) Uiso 0.25 1 d P . . Cd1 Cd 0.10043(4) 0.40827(3) 0.49601(2) 0.04074(19) 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 C1 0.055(4) 0.042(3) 0.052(4) 0.001(3) 0.015(3) -0.004(3) C2 0.046(3) 0.046(4) 0.063(4) 0.007(3) 0.010(3) -0.003(3) C3 0.048(4) 0.060(4) 0.092(6) 0.024(4) 0.018(4) 0.003(3) C4 0.111(7) 0.062(5) 0.097(6) 0.036(5) 0.028(5) 0.041(5) C5 0.060(4) 0.042(4) 0.141(8) 0.001(5) 0.028(5) -0.026(4) C6 0.108(8) 0.127(9) 0.117(8) 0.058(8) -0.024(6) -0.053(7) C7 0.083(6) 0.097(7) 0.096(6) 0.014(5) 0.005(5) -0.048(5) C8 0.092(6) 0.123(8) 0.063(5) -0.016(5) -0.021(4) 0.068(6) C9 0.042(4) 0.031(4) 0.054(5) 0.000 0.005(4) 0.000 C10 0.101(6) 0.051(4) 0.074(5) 0.017(4) -0.003(4) -0.011(4) C11 0.106(7) 0.056(5) 0.069(5) -0.013(4) -0.009(5) -0.025(4) C12' 0.090(9) 0.056(7) 0.078(8) -0.010(6) 0.017(7) -0.037(7) C12 0.15(3) 0.054(18) 0.09(2) -0.021(17) -0.04(2) -0.01(2) C13 0.124(10) 0.120(11) 0.083(8) -0.014(7) 0.020(7) -0.085(9) C13' 0.10(2) 0.13(2) 0.10(2) -0.024(18) -0.013(17) -0.011(18) C14 0.079(5) 0.055(4) 0.079(5) -0.019(4) 0.007(4) -0.024(4) C15 0.153(10) 0.070(6) 0.088(7) 0.008(5) -0.025(6) -0.048(6) C16 0.180(11) 0.069(6) 0.075(6) 0.000(5) -0.023(6) -0.053(7) C17 0.066(5) 0.080(6) 0.077(6) -0.037(5) 0.027(4) -0.034(4) C18 0.045(3) 0.064(4) 0.034(3) -0.001(3) 0.001(2) -0.005(3) C19 0.087(5) 0.057(5) 0.089(6) -0.010(4) 0.032(5) -0.013(4) C20 0.081(5) 0.058(5) 0.077(5) -0.008(4) 0.034(4) -0.002(4) C21 0.045(3) 0.069(4) 0.034(3) 0.004(3) 0.003(2) -0.002(3) C22 0.046(4) 0.067(6) 0.028(4) 0.000 -0.005(3) 0.000 C23 0.069(4) 0.082(5) 0.029(3) 0.004(3) 0.000(3) -0.015(4) C24 0.126(8) 0.050(5) 0.104(7) 0.002(5) -0.063(6) 0.009(5) C25 0.050(3) 0.066(4) 0.049(4) -0.010(3) 0.000(3) 0.003(3) C26 0.110(6) 0.041(4) 0.090(6) -0.004(4) -0.041(5) 0.006(4) C27 0.074(18) 0.025(12) 0.10(2) -0.005(14) -0.037(16) 0.027(13) N1 0.054(3) 0.059(3) 0.045(3) 0.004(3) 0.007(2) -0.005(3) N2 0.046(3) 0.067(4) 0.037(3) 0.006(2) 0.002(2) -0.002(3) N3 0.063(3) 0.069(4) 0.035(3) 0.003(2) -0.003(2) -0.013(3) N4 0.053(3) 0.052(3) 0.046(3) 0.006(3) -0.003(2) -0.006(3) O1 0.077(3) 0.073(3) 0.053(3) 0.017(3) -0.003(2) 0.004(3) O2 0.046(2) 0.039(2) 0.065(3) 0.004(2) 0.0086(19) -0.0126(18) O3 0.077(4) 0.101(5) 0.127(5) 0.033(4) -0.027(4) -0.017(3) O4 0.124(5) 0.074(4) 0.065(3) -0.010(3) 0.008(3) -0.040(4) O5 0.079(4) 0.065(4) 0.114(5) -0.027(3) 0.008(3) -0.025(3) O6 0.111(5) 0.107(5) 0.064(4) -0.031(3) 0.020(3) -0.065(4) Cd1 0.0421(3) 0.0392(3) 0.0405(3) 0.00268(17) 0.00025(17) -0.00954(18) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 O1 1.243(8) . ? C1 O2 1.277(7) . ? C1 C2 1.493(9) . ? C2 C3 1.341(10) . ? C2 C7 1.406(10) . ? C3 C4 1.440(11) . ? C3 H3 0.9300 . ? C4 C5 1.433(13) . ? C4 H4 0.9300 . ? C5 C6 1.289(13) . ? C5 O3 1.433(10) . ? C6 C7 1.319(12) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O3 1.320(9) . ? C8 C9 1.665(12) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.523(9) 2_655 ? C9 C10 1.523(9) . ? C9 C8 1.665(12) 2_655 ? C10 O4 1.390(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C16 1.313(12) . ? C11 C12' 1.331(15) . ? C11 O4 1.401(9) . ? C11 C12 1.50(4) . ? C12' C12 1.11(4) . ? C12' C13 1.456(15) . ? C12' C13' 2.00(6) . ? C12 C13' 1.66(6) . ? C12 C13 1.85(4) . ? C13 C13' 1.20(6) . ? C13 C14 1.353(14) . ? C13' C14 1.304(10) . ? C14 C15 1.362(12) . ? C14 C17 1.492(10) . ? C15 C16 1.365(12) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 O6 1.220(11) . ? C17 O5 1.263(11) . ? C17 Cd1 2.748(7) 1_665 ? C18 N1 1.326(8) . ? C18 N2 1.345(8) . ? C18 H18 0.9300 . ? C19 N1 1.354(9) . ? C19 C20 1.367(10) . ? C19 H19 0.9300 . ? C20 N2 1.340(9) . ? C20 H20 0.9300 . ? C21 N2 1.457(8) . ? C21 C22 1.554(8) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.551(9) . ? C22 C23 1.551(9) 2_655 ? C22 C21 1.554(8) 2_655 ? C23 N3 1.461(8) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C26 1.315(11) . ? C24 N3 1.395(10) . ? C24 H24 0.9300 . ? C25 N4 1.292(9) . ? C25 N3 1.323(8) . ? C25 H25 0.9300 . ? C26 N4 1.362(9) . ? C26 H26 0.9300 . ? C27 N5 1.575(10) . ? C28 N5 1.61(6) . ? C29 O7 0.87(4) 2 ? C29 C29 1.03(6) 2 ? C29 N5 1.25(4) . ? C29 O7 1.23(4) . ? N1 Cd1 2.328(5) . ? N4 Cd1 2.262(5) 3_666 ? N5 O7 1.63(4) 2 ? O2 Cd1 2.289(4) . ? O2 Cd1 2.379(4) 3_566 ? O1W O1W' 1.02(3) . ? O1W O1W' 1.02(3) 2_755 ? O5 Cd1 2.474(6) 1_665 ? O6 Cd1 2.335(6) 1_665 ? O7 O7 0.79(5) 2 ? O7 C29 0.87(4) 2 ? O7 N5 1.63(4) 2 ? Cd1 N4 2.262(5) 3_666 ? Cd1 O6 2.335(6) 1_445 ? Cd1 O2 2.379(4) 3_566 ? Cd1 O5 2.474(6) 1_445 ? Cd1 C17 2.748(7) 1_445 ? 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 O1 C1 O2 122.5(6) . . ? O1 C1 C2 119.9(6) . . ? O2 C1 C2 117.6(6) . . ? C3 C2 C7 118.4(7) . . ? C3 C2 C1 123.2(6) . . ? C7 C2 C1 118.3(7) . . ? C2 C3 C4 119.0(7) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 116.1(8) . . ? C5 C4 H4 122.0 . . ? C3 C4 H4 122.0 . . ? C6 C5 C4 123.8(8) . . ? C6 C5 O3 115.0(8) . . ? C4 C5 O3 120.9(9) . . ? C5 C6 C7 118.1(10) . . ? C5 C6 H6 120.9 . . ? C7 C6 H6 120.9 . . ? C6 C7 C2 124.4(10) . . ? C6 C7 H7 117.8 . . ? C2 C7 H7 117.8 . . ? O3 C8 C9 105.8(7) . . ? O3 C8 H8A 110.6 . . ? C9 C8 H8A 110.6 . . ? O3 C8 H8B 110.6 . . ? C9 C8 H8B 110.6 . . ? H8A C8 H8B 108.7 . . ? C10 C9 C10 110.8(8) 2_655 . ? C10 C9 C8 111.6(4) 2_655 2_655 ? C10 C9 C8 108.6(4) . 2_655 ? C10 C9 C8 108.6(4) 2_655 . ? C10 C9 C8 111.6(4) . . ? C8 C9 C8 105.4(7) 2_655 . ? O4 C10 C9 107.2(6) . . ? O4 C10 H10A 110.3 . . ? C9 C10 H10A 110.3 . . ? O4 C10 H10B 110.3 . . ? C9 C10 H10B 110.3 . . ? H10A C10 H10B 108.5 . . ? C16 C11 C12' 119.4(8) . . ? C16 C11 O4 115.2(8) . . ? C12' C11 O4 124.5(8) . . ? C16 C11 C12 114.9(18) . . ? C12' C11 C12 45.8(17) . . ? O4 C11 C12 115.8(13) . . ? C12 C12' C11 75(2) . . ? C12 C12' C13 91(2) . . ? C11 C12' C13 119.6(10) . . ? C12 C12' C13' 56(2) . . ? C11 C12' C13' 96(2) . . ? C13 C12' C13' 36.8(15) . . ? C12' C12 C11 59.3(19) . . ? C12' C12 C13' 90(3) . . ? C11 C12 C13' 105(2) . . ? C12' C12 C13 51.9(16) . . ? C11 C12 C13 92(2) . . ? C13' C12 C13 40(2) . . ? C13' C13 C14 61.0(14) . . ? C13' C13 C12' 97(3) . . ? C14 C13 C12' 118.6(10) . . ? C13' C13 C12 62(3) . . ? C14 C13 C12 106.1(17) . . ? C12' C13 C12 36.9(14) . . ? C13 C13' C14 65.1(18) . . ? C13 C13' C12 79(4) . . ? C14 C13' C12 120(4) . . ? C13 C13' C12' 46(2) . . ? C14 C13' C12' 92(3) . . ? C12 C13' C12' 33.8(19) . . ? C13' C14 C13 54(3) . . ? C13' C14 C15 105(3) . . ? C13 C14 C15 117.5(8) . . ? C13' C14 C17 113(2) . . ? C13 C14 C17 118.8(8) . . ? C15 C14 C17 123.3(8) . . ? C14 C15 C16 121.8(9) . . ? C14 C15 H15 119.1 . . ? C16 C15 H15 119.1 . . ? C11 C16 C15 121.1(9) . . ? C11 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? O6 C17 O5 121.8(7) . . ? O6 C17 C14 119.9(9) . . ? O5 C17 C14 118.3(9) . . ? O6 C17 Cd1 57.7(4) . 1_665 ? O5 C17 Cd1 64.2(4) . 1_665 ? C14 C17 Cd1 177.4(7) . 1_665 ? N1 C18 N2 111.4(6) . . ? N1 C18 H18 124.3 . . ? N2 C18 H18 124.3 . . ? N1 C19 C20 110.0(7) . . ? N1 C19 H19 125.0 . . ? C20 C19 H19 125.0 . . ? N2 C20 C19 106.3(6) . . ? N2 C20 H20 126.8 . . ? C19 C20 H20 126.8 . . ? N2 C21 C22 115.0(4) . . ? N2 C21 H21A 108.5 . . ? C22 C21 H21A 108.5 . . ? N2 C21 H21B 108.5 . . ? C22 C21 H21B 108.5 . . ? H21A C21 H21B 107.5 . . ? C23 C22 C23 113.7(9) . 2_655 ? C23 C22 C21 109.3(3) . 2_655 ? C23 C22 C21 106.2(3) 2_655 2_655 ? C23 C22 C21 106.2(3) . . ? C23 C22 C21 109.3(3) 2_655 . ? C21 C22 C21 112.3(8) 2_655 . ? N3 C23 C22 115.2(5) . . ? N3 C23 H23A 108.5 . . ? C22 C23 H23A 108.5 . . ? N3 C23 H23B 108.5 . . ? C22 C23 H23B 108.5 . . ? H23A C23 H23B 107.5 . . ? C26 C24 N3 106.5(7) . . ? C26 C24 H24 126.8 . . ? N3 C24 H24 126.8 . . ? N4 C25 N3 112.7(7) . . ? N4 C25 H25 123.7 . . ? N3 C25 H25 123.7 . . ? C24 C26 N4 109.9(7) . . ? C24 C26 H26 125.0 . . ? N4 C26 H26 125.0 . . ? O7 C29 C29 80(3) 2 2 ? O7 C29 N5 100(4) 2 . ? C29 C29 N5 153(6) 2 . ? O7 C29 O7 40(3) 2 . ? C29 C29 O7 44.1(19) 2 . ? N5 C29 O7 123(3) . . ? C18 N1 C19 105.0(6) . . ? C18 N1 Cd1 124.0(5) . . ? C19 N1 Cd1 128.0(5) . . ? C20 N2 C18 107.4(5) . . ? C20 N2 C21 129.7(6) . . ? C18 N2 C21 122.9(6) . . ? C25 N3 C24 105.2(6) . . ? C25 N3 C23 126.1(6) . . ? C24 N3 C23 128.6(6) . . ? C25 N4 C26 105.7(6) . . ? C25 N4 Cd1 125.0(5) . 3_666 ? C26 N4 Cd1 121.7(5) . 3_666 ? C29 N5 C28 107(3) . . ? C29 N5 O7 31(2) . 2 ? C28 N5 O7 131(3) . 2 ? C29 N5 C27 132(3) . . ? C28 N5 C27 120(3) . . ? O7 N5 C27 106(2) 2 . ? C1 O2 Cd1 105.2(4) . . ? C1 O2 Cd1 118.1(4) . 3_566 ? Cd1 O2 Cd1 101.58(15) . 3_566 ? O1W' O1W O1W' 149(5) . 2_755 ? C8 O3 C5 114.1(8) . . ? C10 O4 C11 118.0(7) . . ? C17 O5 Cd1 88.5(5) . 1_665 ? C17 O6 Cd1 96.2(5) . 1_665 ? O7 O7 C29 96(3) 2 2 ? O7 O7 C29 45(2) 2 . ? C29 O7 C29 56(4) 2 . ? O7 O7 N5 124(5) 2 2 ? C29 O7 N5 49(3) 2 2 ? C29 O7 N5 100(3) . 2 ? N4 Cd1 O2 119.32(18) 3_666 . ? N4 Cd1 N1 102.03(19) 3_666 . ? O2 Cd1 N1 94.37(17) . . ? N4 Cd1 O6 92.8(2) 3_666 1_445 ? O2 Cd1 O6 146.0(2) . 1_445 ? N1 Cd1 O6 89.1(2) . 1_445 ? N4 Cd1 O2 87.70(18) 3_666 3_566 ? O2 Cd1 O2 78.42(15) . 3_566 ? N1 Cd1 O2 169.93(17) . 3_566 ? O6 Cd1 O2 93.03(19) 1_445 3_566 ? N4 Cd1 O5 146.0(2) 3_666 1_445 ? O2 Cd1 O5 93.06(19) . 1_445 ? N1 Cd1 O5 84.35(19) . 1_445 ? O6 Cd1 O5 53.5(2) 1_445 1_445 ? O2 Cd1 O5 89.00(17) 3_566 1_445 ? N4 Cd1 C17 118.9(3) 3_666 1_445 ? O2 Cd1 C17 120.2(3) . 1_445 ? N1 Cd1 C17 86.4(2) . 1_445 ? O6 Cd1 C17 26.2(3) 1_445 1_445 ? O2 Cd1 C17 91.17(19) 3_566 1_445 ? O5 Cd1 C17 27.3(2) 1_445 1_445 ? 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 O1 C1 C2 C3 169.1(7) . . . . ? O2 C1 C2 C3 -7.4(10) . . . . ? O1 C1 C2 C7 -7.4(10) . . . . ? O2 C1 C2 C7 176.1(7) . . . . ? C7 C2 C3 C4 1.9(11) . . . . ? C1 C2 C3 C4 -174.5(7) . . . . ? C2 C3 C4 C5 1.8(12) . . . . ? C3 C4 C5 C6 -3.4(15) . . . . ? C3 C4 C5 O3 171.1(8) . . . . ? C4 C5 C6 C7 0.7(19) . . . . ? O3 C5 C6 C7 -174.2(11) . . . . ? C5 C6 C7 C2 4(2) . . . . ? C3 C2 C7 C6 -5.1(15) . . . . ? C1 C2 C7 C6 171.6(11) . . . . ? O3 C8 C9 C10 -169.7(6) . . . 2_655 ? O3 C8 C9 C10 -47.3(9) . . . . ? O3 C8 C9 C8 70.5(6) . . . 2_655 ? C10 C9 C10 O4 -54.6(5) 2_655 . . . ? C8 C9 C10 O4 68.4(8) 2_655 . . . ? C8 C9 C10 O4 -175.8(6) . . . . ? C16 C11 C12' C12 -97(2) . . . . ? O4 C11 C12' C12 94(2) . . . . ? C16 C11 C12' C13 -15(2) . . . . ? O4 C11 C12' C13 176.6(13) . . . . ? C12 C11 C12' C13 83(2) . . . . ? C16 C11 C12' C13' -44.3(15) . . . . ? O4 C11 C12' C13' 146.9(10) . . . . ? C12 C11 C12' C13' 53(2) . . . . ? C13 C12' C12 C11 -120.4(10) . . . . ? C13' C12' C12 C11 -108(2) . . . . ? C11 C12' C12 C13' 108(2) . . . . ? C13 C12' C12 C13' -13(2) . . . . ? C11 C12' C12 C13 120.4(10) . . . . ? C13' C12' C12 C13 13(2) . . . . ? C16 C11 C12 C12' 108(2) . . . . ? O4 C11 C12 C12' -114.0(15) . . . . ? C16 C11 C12 C13' 27(4) . . . . ? C12' C11 C12 C13' -81(3) . . . . ? O4 C11 C12 C13' 165(3) . . . . ? C16 C11 C12 C13 65(2) . . . . ? C12' C11 C12 C13 -42.8(12) . . . . ? O4 C11 C12 C13 -156.8(10) . . . . ? C12 C12' C13 C13' 18(3) . . . . ? C11 C12' C13 C13' -55(3) . . . . ? C12 C12' C13 C14 78(3) . . . . ? C11 C12' C13 C14 5(2) . . . . ? C13' C12' C13 C14 60.6(19) . . . . ? C11 C12' C13 C12 -73(2) . . . . ? C13' C12' C13 C12 -18(3) . . . . ? C12' C12 C13 C13' -160(4) . . . . ? C11 C12 C13 C13' -112(3) . . . . ? C12' C12 C13 C14 -116(2) . . . . ? C11 C12 C13 C14 -69(2) . . . . ? C13' C12 C13 C14 43(2) . . . . ? C11 C12 C13 C12' 47.9(16) . . . . ? C13' C12 C13 C12' 160(4) . . . . ? C12' C13 C13' C14 119.0(16) . . . . ? C12 C13 C13' C14 131(3) . . . . ? C14 C13 C13' C12 -131(3) . . . . ? C12' C13 C13' C12 -12(2) . . . . ? C14 C13 C13' C12' -119.0(16) . . . . ? C12 C13 C13' C12' 12(2) . . . . ? C12' C12 C13' C13 16(3) . . . . ? C11 C12 C13' C13 74(4) . . . . ? C12' C12 C13' C14 -36(6) . . . . ? C11 C12 C13' C14 22(6) . . . . ? C13 C12 C13' C14 -52(3) . . . . ? C11 C12 C13' C12' 58(2) . . . . ? C13 C12 C13' C12' -16(3) . . . . ? C12 C12' C13' C13 -158(4) . . . . ? C11 C12' C13' C13 134(2) . . . . ? C12 C12' C13' C14 149(5) . . . . ? C11 C12' C13' C14 81(3) . . . . ? C13 C12' C13' C14 -52.5(17) . . . . ? C11 C12' C13' C12 -68(3) . . . . ? C13 C12' C13' C12 158(4) . . . . ? C12 C13' C14 C13 59(4) . . . . ? C12' C13' C14 C13 39.3(15) . . . . ? C13 C13' C14 C15 -113(2) . . . . ? C12 C13' C14 C15 -55(5) . . . . ? C12' C13' C14 C15 -74(2) . . . . ? C13 C13' C14 C17 110(2) . . . . ? C12 C13' C14 C17 169(4) . . . . ? C12' C13' C14 C17 149.2(11) . . . . ? C12' C13 C14 C13' -82(3) . . . . ? C12 C13 C14 C13' -44(3) . . . . ? C13' C13 C14 C15 89(3) . . . . ? C12' C13 C14 C15 7(2) . . . . ? C12 C13 C14 C15 44.9(19) . . . . ? C13' C13 C14 C17 -98(3) . . . . ? C12' C13 C14 C17 -180.0(12) . . . . ? C12 C13 C14 C17 -142.2(15) . . . . ? C13' C14 C15 C16 46(3) . . . . ? C13 C14 C15 C16 -10.6(19) . . . . ? C17 C14 C15 C16 176.8(11) . . . . ? C12' C11 C16 C15 12(2) . . . . ? O4 C11 C16 C15 -178.6(11) . . . . ? C12 C11 C16 C15 -40(2) . . . . ? C14 C15 C16 C11 1(2) . . . . ? C13' C14 C17 O6 -29(3) . . . . ? C13 C14 C17 O6 31.6(15) . . . . ? C15 C14 C17 O6 -155.9(10) . . . . ? C13' C14 C17 O5 152(3) . . . . ? C13 C14 C17 O5 -147.5(12) . . . . ? C15 C14 C17 O5 25.0(13) . . . . ? C13' C14 C17 Cd1 -48(14) . . . 1_665 ? C13 C14 C17 Cd1 12(14) . . . 1_665 ? C15 C14 C17 Cd1 -175(13) . . . 1_665 ? N1 C19 C20 N2 -2.0(10) . . . . ? N2 C21 C22 C23 170.4(6) . . . . ? N2 C21 C22 C23 47.3(8) . . . 2_655 ? N2 C21 C22 C21 -70.3(5) . . . 2_655 ? C23 C22 C23 N3 64.4(5) 2_655 . . . ? C21 C22 C23 N3 -177.1(6) 2_655 . . . ? C21 C22 C23 N3 -55.8(8) . . . . ? N3 C24 C26 N4 -1.5(12) . . . . ? N2 C18 N1 C19 -0.1(8) . . . . ? N2 C18 N1 Cd1 -161.6(4) . . . . ? C20 C19 N1 C18 1.3(9) . . . . ? C20 C19 N1 Cd1 161.8(5) . . . . ? C19 C20 N2 C18 1.9(9) . . . . ? C19 C20 N2 C21 -177.0(7) . . . . ? N1 C18 N2 C20 -1.1(8) . . . . ? N1 C18 N2 C21 177.8(5) . . . . ? C22 C21 N2 C20 87.7(9) . . . . ? C22 C21 N2 C18 -91.0(7) . . . . ? N4 C25 N3 C24 0.6(9) . . . . ? N4 C25 N3 C23 -176.6(6) . . . . ? C26 C24 N3 C25 0.5(10) . . . . ? C26 C24 N3 C23 177.7(7) . . . . ? C22 C23 N3 C25 93.3(8) . . . . ? C22 C23 N3 C24 -83.3(10) . . . . ? N3 C25 N4 C26 -1.5(9) . . . . ? N3 C25 N4 Cd1 148.0(5) . . . 3_666 ? C24 C26 N4 C25 1.8(10) . . . . ? C24 C26 N4 Cd1 -148.9(7) . . . 3_666 ? O7 C29 N5 C28 144(4) 2 . . . ? C29 C29 N5 C28 -128(4) 2 . . . ? O7 C29 N5 C28 179(3) . . . . ? C29 C29 N5 O7 88(5) 2 . . 2 ? O7 C29 N5 O7 35(4) . . . 2 ? O7 C29 N5 C27 -40(6) 2 . . . ? C29 C29 N5 C27 48(7) 2 . . . ? O7 C29 N5 C27 -5(6) . . . . ? O1 C1 O2 Cd1 -13.2(7) . . . . ? C2 C1 O2 Cd1 163.1(5) . . . . ? O1 C1 O2 Cd1 99.2(6) . . . 3_566 ? C2 C1 O2 Cd1 -84.5(6) . . . 3_566 ? C9 C8 O3 C5 -174.7(7) . . . . ? C6 C5 O3 C8 -177.9(10) . . . . ? C4 C5 O3 C8 7.1(12) . . . . ? C9 C10 O4 C11 172.0(7) . . . . ? C16 C11 O4 C10 -163.0(10) . . . . ? C12' C11 O4 C10 6.2(16) . . . . ? C12 C11 O4 C10 59(2) . . . . ? O6 C17 O5 Cd1 0.0(8) . . . 1_665 ? C14 C17 O5 Cd1 179.0(6) . . . 1_665 ? O5 C17 O6 Cd1 0.0(8) . . . 1_665 ? C14 C17 O6 Cd1 -179.0(6) . . . 1_665 ? C29 C29 O7 O7 149(10) 2 . . 2 ? N5 C29 O7 O7 -62(7) . . . 2 ? O7 C29 O7 C29 -149(10) 2 . . 2 ? N5 C29 O7 C29 149(7) . . . 2 ? O7 C29 O7 N5 -129(7) 2 . . 2 ? C29 C29 O7 N5 21(5) 2 . . 2 ? N5 C29 O7 N5 169(3) . . . 2 ? C1 O2 Cd1 N4 42.9(4) . . . 3_666 ? Cd1 O2 Cd1 N4 -80.7(2) 3_566 . . 3_666 ? C1 O2 Cd1 N1 -63.5(4) . . . . ? Cd1 O2 Cd1 N1 172.90(17) 3_566 . . . ? C1 O2 Cd1 O6 -158.4(4) . . . 1_445 ? Cd1 O2 Cd1 O6 78.0(3) 3_566 . . 1_445 ? C1 O2 Cd1 O2 123.6(4) . . . 3_566 ? Cd1 O2 Cd1 O2 0.0 3_566 . . 3_566 ? C1 O2 Cd1 O5 -148.1(4) . . . 1_445 ? Cd1 O2 Cd1 O5 88.35(19) 3_566 . . 1_445 ? C1 O2 Cd1 C17 -151.9(4) . . . 1_445 ? Cd1 O2 Cd1 C17 84.5(2) 3_566 . . 1_445 ? C18 N1 Cd1 N4 -93.2(5) . . . 3_666 ? C19 N1 Cd1 N4 109.7(6) . . . 3_666 ? C18 N1 Cd1 O2 28.0(5) . . . . ? C19 N1 Cd1 O2 -129.1(6) . . . . ? C18 N1 Cd1 O6 174.1(5) . . . 1_445 ? C19 N1 Cd1 O6 17.0(6) . . . 1_445 ? C18 N1 Cd1 O2 71.8(11) . . . 3_566 ? C19 N1 Cd1 O2 -85.3(12) . . . 3_566 ? C18 N1 Cd1 O5 120.6(5) . . . 1_445 ? C19 N1 Cd1 O5 -36.5(6) . . . 1_445 ? C18 N1 Cd1 C17 148.0(5) . . . 1_445 ? C19 N1 Cd1 C17 -9.1(7) . . . 1_445 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.988 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.119 #=========================END