# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Wu, Biao' _publ_contact_author_name 'Wu, Biao' _publ_contact_author_email wubiao@lzb.ac.cn _publ_section_title ; Anion binding in metal complexes of 5,5'-dicarbamate-2,2'-bipyridine ligands: coordination-driven pre-organization of metallo-ligand anion receptors ; # Attachment '- bipy.cif' data_L1FeSO4 _database_code_depnum_ccdc_archive 'CCDC 800531' #TrackingRef '- bipy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H166 Fe2 N24 O49 S2' _chemical_formula_weight 2760.47 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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 13.853(18) _cell_length_b 16.35(2) _cell_length_c 17.75(2) _cell_angle_alpha 109.45(2) _cell_angle_beta 95.93(2) _cell_angle_gamma 106.38(2) _cell_volume 3549(8) _cell_formula_units_Z 1 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1458 _exptl_absorpt_coefficient_mu 0.323 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9237 _exptl_absorpt_correction_T_max 0.9872 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 233(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 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17218 _diffrn_reflns_av_R_equivalents 0.1146 _diffrn_reflns_av_sigmaI/netI 0.2825 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11832 _reflns_number_gt 3921 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 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^)+(0.1665P)^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 11832 _refine_ls_number_parameters 838 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.2526 _refine_ls_R_factor_gt 0.1182 _refine_ls_wR_factor_ref 0.3450 _refine_ls_wR_factor_gt 0.2773 _refine_ls_goodness_of_fit_ref 0.881 _refine_ls_restrained_S_all 0.883 _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 Fe Fe 0.85124(10) 0.72338(9) 0.56966(9) 0.0389(4) Uani 1 1 d . . . N1 N 0.7021(6) 0.6679(5) 0.5235(5) 0.0393(19) Uani 1 1 d . . . N2 N 0.5083(6) 0.5582(6) 0.3325(6) 0.061(2) Uani 1 1 d . . . H2A H 0.5490 0.5410 0.3011 0.073 Uiso 1 1 calc R . . N3 N 0.8031(6) 0.7303(5) 0.6716(5) 0.045(2) Uani 1 1 d . . . N4 N 0.9004(8) 0.8057(6) 0.8934(6) 0.065(3) Uani 1 1 d . . . H4A H 0.9650 0.8166 0.8911 0.078 Uiso 1 1 calc R . . N5 N 0.8690(5) 0.6062(5) 0.5605(5) 0.0358(18) Uani 1 1 d . . . N6 N 0.7359(6) 0.3579(5) 0.4781(5) 0.053(2) Uani 1 1 d . . . H6A H 0.6962 0.3558 0.4358 0.064 Uiso 1 1 calc R . . N7 N 0.9990(5) 0.7724(5) 0.6236(4) 0.0359(19) Uani 1 1 d . . . N8 N 1.2291(6) 0.9797(6) 0.7373(6) 0.061(3) Uani 1 1 d . . . H8A H 1.2850 0.9901 0.7714 0.073 Uiso 1 1 calc R . . N9 N 0.8850(5) 0.7191(5) 0.4639(5) 0.0345(18) Uani 1 1 d . . . N10 N 0.9163(6) 0.5692(6) 0.2734(5) 0.047(2) Uani 1 1 d . . . H10A H 0.8802 0.5187 0.2778 0.056 Uiso 1 1 calc R . . N11 N 0.8443(5) 0.8457(5) 0.5767(5) 0.0366(19) Uani 1 1 d . . . N12 N 0.7682(6) 1.0404(5) 0.6889(5) 0.045(2) Uani 1 1 d . . . H12A H 0.7811 1.0963 0.6903 0.054 Uiso 1 1 calc R . . O1 O 0.3420(8) 0.5599(8) 0.3286(7) 0.129(4) Uani 1 1 d . . . O2 O 0.4040(6) 0.5161(6) 0.2155(6) 0.085(3) Uani 1 1 d . . . O3 O 0.7922(9) 0.8184(8) 0.9810(6) 0.125(4) Uani 1 1 d . . . O4 O 0.9617(8) 0.8557(7) 1.0241(5) 0.092(3) Uani 1 1 d . . . O5 O 0.7704(7) 0.2699(5) 0.5478(6) 0.088(3) Uani 1 1 d . . . O6 O 0.6288(6) 0.2189(6) 0.4451(6) 0.086(3) Uani 1 1 d . . . O7 O 1.1406(6) 1.0543(5) 0.6857(5) 0.073(2) Uani 1 1 d . . . O8 O 1.2904(6) 1.1296(5) 0.7810(5) 0.081(3) Uani 1 1 d . . . O9 O 1.0239(6) 0.6223(5) 0.1975(5) 0.078(3) Uani 1 1 d . . . O10 O 0.9351(6) 0.4714(5) 0.1629(5) 0.070(2) Uani 1 1 d . . . O11 O 0.6859(6) 0.9429(5) 0.7477(5) 0.076(2) Uani 1 1 d . . . O12 O 0.6968(6) 1.0936(5) 0.7904(5) 0.070(2) Uani 1 1 d . . . C1 C 0.6544(7) 0.6322(6) 0.4445(7) 0.042(3) Uani 1 1 d . . . H1A H 0.6945 0.6309 0.4048 0.050 Uiso 1 1 calc R . . C2 C 0.5467(8) 0.5966(7) 0.4187(8) 0.056(3) Uani 1 1 d . . . C3 C 0.4868(9) 0.5981(8) 0.4760(8) 0.066(3) Uani 1 1 d . . . H3A H 0.4145 0.5757 0.4599 0.079 Uiso 1 1 calc R . . C4 C 0.5357(9) 0.6335(8) 0.5583(8) 0.063(3) Uani 1 1 d . . . H4B H 0.4961 0.6340 0.5983 0.076 Uiso 1 1 calc R . . C5 C 0.6434(8) 0.6683(6) 0.5818(7) 0.047(3) Uani 1 1 d . . . C6 C 0.7016(8) 0.7012(7) 0.6643(6) 0.047(3) Uani 1 1 d . . . C7 C 0.6563(9) 0.7024(8) 0.7316(8) 0.064(3) Uani 1 1 d . . . H7A H 0.5843 0.6798 0.7245 0.077 Uiso 1 1 calc R . . C8 C 0.7214(11) 0.7384(9) 0.8108(8) 0.074(4) Uani 1 1 d . . . H8B H 0.6929 0.7423 0.8572 0.089 Uiso 1 1 calc R . . C9 C 0.8265(9) 0.7674(7) 0.8186(7) 0.054(3) Uani 1 1 d . . . C10 C 0.8666(8) 0.7640(6) 0.7488(6) 0.047(3) Uani 1 1 d . . . H10B H 0.9385 0.7851 0.7543 0.057 Uiso 1 1 calc R . . C11 C 0.4110(10) 0.5468(9) 0.2965(10) 0.075(4) Uani 1 1 d . . . C12 C 0.3068(12) 0.5074(12) 0.1642(13) 0.129(7) Uani 1 1 d . . . H12B H 0.2467 0.4784 0.1835 0.155 Uiso 1 1 calc R . . C13 C 0.3089(16) 0.5989(15) 0.1694(13) 0.197(11) Uani 1 1 d . . . H13A H 0.3096 0.6359 0.2251 0.295 Uiso 1 1 calc R . . H13B H 0.2482 0.5934 0.1329 0.295 Uiso 1 1 calc R . . H13C H 0.3703 0.6283 0.1536 0.295 Uiso 1 1 calc R . . C14 C 0.3039(14) 0.4463(13) 0.0780(11) 0.145(7) Uani 1 1 d . . . H14A H 0.2420 0.4385 0.0416 0.218 Uiso 1 1 calc R . . H14B H 0.3039 0.3865 0.0770 0.218 Uiso 1 1 calc R . . H14C H 0.3641 0.4745 0.0602 0.218 Uiso 1 1 calc R . . C15 C 0.8778(12) 0.8257(9) 0.9662(9) 0.073(4) Uani 1 1 d . . . C16 C 0.9537(13) 0.8856(10) 1.1106(8) 0.092(5) Uani 1 1 d . . . H16A H 0.8810 0.8760 1.1150 0.111 Uiso 1 1 calc R . . C17 C 1.0168(14) 0.9842(12) 1.1511(10) 0.128(6) Uani 1 1 d . . . H17A H 0.9871 1.0199 1.1277 0.192 Uiso 1 1 calc R . . H17B H 1.0865 0.9928 1.1429 0.192 Uiso 1 1 calc R . . H17C H 1.0180 1.0047 1.2092 0.192 Uiso 1 1 calc R . . C18 C 0.9958(15) 0.8264(12) 1.1442(9) 0.135(7) Uani 1 1 d . . . H18A H 0.9507 0.7627 1.1178 0.203 Uiso 1 1 calc R . . H18B H 0.9996 0.8470 1.2027 0.203 Uiso 1 1 calc R . . H18C H 1.0642 0.8313 1.1338 0.203 Uiso 1 1 calc R . . C19 C 0.7984(7) 0.5222(6) 0.5233(6) 0.038(2) Uani 1 1 d . . . H19A H 0.7339 0.5166 0.4954 0.046 Uiso 1 1 calc R . . C20 C 0.8165(7) 0.4415(6) 0.5238(6) 0.044(2) Uani 1 1 d . . . C21 C 0.9092(8) 0.4494(7) 0.5672(6) 0.053(3) Uani 1 1 d . . . H21A H 0.9219 0.3972 0.5711 0.063 Uiso 1 1 calc R . . C22 C 0.9833(8) 0.5363(7) 0.6051(7) 0.056(3) Uani 1 1 d . . . H22A H 1.0473 0.5435 0.6350 0.067 Uiso 1 1 calc R . . C23 C 0.9632(7) 0.6131(6) 0.5989(6) 0.039(2) Uani 1 1 d . . . C24 C 1.0385(7) 0.7075(6) 0.6344(6) 0.042(2) Uani 1 1 d . . . C25 C 1.1398(7) 0.7303(7) 0.6710(6) 0.047(3) Uani 1 1 d . . . H25A H 1.1656 0.6836 0.6731 0.056 Uiso 1 1 calc R . . C26 C 1.2034(9) 0.8197(7) 0.7043(7) 0.062(3) Uani 1 1 d . . . H26A H 1.2717 0.8354 0.7318 0.075 Uiso 1 1 calc R . . C27 C 1.1652(8) 0.8873(7) 0.6970(6) 0.048(3) Uani 1 1 d . . . C28 C 1.0627(7) 0.8617(6) 0.6562(6) 0.043(2) Uani 1 1 d . . . H28A H 1.0372 0.9077 0.6512 0.052 Uiso 1 1 calc R . . C29 C 0.7150(11) 0.2789(8) 0.4952(9) 0.069(3) Uani 1 1 d . . . C30 C 0.5848(13) 0.1357(10) 0.4641(14) 0.136(6) Uani 1 1 d U . . H30A H 0.6316 0.1308 0.5071 0.163 Uiso 1 1 calc R . . C31 C 0.5595(17) 0.0612(12) 0.3874(15) 0.199(9) Uani 1 1 d U . . H31A H 0.5324 0.0034 0.3947 0.298 Uiso 1 1 calc R . . H31B H 0.6208 0.0626 0.3653 0.298 Uiso 1 1 calc R . . H31C H 0.5079 0.0665 0.3498 0.298 Uiso 1 1 calc R . . C32 C 0.4838(16) 0.1352(12) 0.4832(15) 0.182(8) Uani 1 1 d U . . H32A H 0.4936 0.1832 0.5361 0.273 Uiso 1 1 calc R . . H32B H 0.4470 0.0757 0.4844 0.273 Uiso 1 1 calc R . . H32C H 0.4441 0.1461 0.4415 0.273 Uiso 1 1 calc R . . C33 C 1.2130(9) 1.0543(7) 0.7288(8) 0.061(3) Uani 1 1 d . . . C34 C 1.2937(12) 1.2224(9) 0.7834(10) 0.097(5) Uani 1 1 d . . . H34A H 1.2224 1.2233 0.7730 0.117 Uiso 1 1 calc R . . C35 C 1.3481(14) 1.2866(10) 0.8702(12) 0.145(7) Uani 1 1 d . . . H35A H 1.3081 1.2699 0.9078 0.217 Uiso 1 1 calc R . . H35B H 1.3554 1.3495 0.8765 0.217 Uiso 1 1 calc R . . H35C H 1.4157 1.2818 0.8820 0.217 Uiso 1 1 calc R . . C36 C 1.3444(12) 1.2399(11) 0.7193(10) 0.129(6) Uani 1 1 d . . . H36A H 1.3041 1.1947 0.6662 0.194 Uiso 1 1 calc R . . H36B H 1.4127 1.2353 0.7276 0.194 Uiso 1 1 calc R . . H36C H 1.3501 1.3012 0.7215 0.194 Uiso 1 1 calc R . . C37 C 0.8958(6) 0.6495(7) 0.4065(6) 0.036(2) Uani 1 1 d . . . H37A H 0.8883 0.5954 0.4165 0.044 Uiso 1 1 calc R . . C38 C 0.9179(7) 0.6494(7) 0.3307(6) 0.039(2) Uani 1 1 d . . . C39 C 0.9407(8) 0.7356(7) 0.3225(6) 0.049(3) Uani 1 1 d . . . H39A H 0.9635 0.7424 0.2761 0.058 Uiso 1 1 calc R . . C40 C 0.9299(7) 0.8062(7) 0.3795(6) 0.048(3) Uani 1 1 d . . . H40A H 0.9431 0.8623 0.3720 0.057 Uiso 1 1 calc R . . C41 C 0.8989(7) 0.8005(6) 0.4520(6) 0.040(2) Uani 1 1 d . . . C42 C 0.8718(7) 0.8682(6) 0.5137(6) 0.039(2) Uani 1 1 d . . . C43 C 0.8697(8) 0.9550(6) 0.5114(7) 0.048(3) Uani 1 1 d . . . H43A H 0.8933 0.9740 0.4702 0.058 Uiso 1 1 calc R . . C44 C 0.8336(8) 1.0087(6) 0.5686(6) 0.045(3) Uani 1 1 d . . . H44A H 0.8287 1.0636 0.5653 0.054 Uiso 1 1 calc R . . C45 C 0.8039(7) 0.9840(6) 0.6319(6) 0.038(2) Uani 1 1 d . . . C46 C 0.8095(7) 0.9001(6) 0.6333(6) 0.037(2) Uani 1 1 d . . . H46A H 0.7880 0.8816 0.6754 0.044 Uiso 1 1 calc R . . C47 C 0.9649(8) 0.5593(7) 0.2100(6) 0.049(3) Uani 1 1 d . . . C48 C 0.9754(13) 0.4426(9) 0.0927(11) 0.109(6) Uani 1 1 d . . . H48A H 1.0322 0.4939 0.0906 0.131 Uiso 1 1 calc R . . C49 C 0.879(2) 0.4058(17) 0.0164(12) 0.205(11) Uani 1 1 d . . . H49A H 0.8564 0.4566 0.0156 0.307 Uiso 1 1 calc R . . H49B H 0.8227 0.3586 0.0221 0.307 Uiso 1 1 calc R . . H49C H 0.8998 0.3800 -0.0343 0.307 Uiso 1 1 calc R . . C50 C 1.0062(17) 0.3665(13) 0.0869(15) 0.198(13) Uani 1 1 d . . . H50A H 1.0617 0.3837 0.1332 0.298 Uiso 1 1 calc R . . H50B H 1.0301 0.3467 0.0365 0.298 Uiso 1 1 calc R . . H50C H 0.9483 0.3165 0.0868 0.298 Uiso 1 1 calc R . . C51 C 0.7145(9) 1.0191(8) 0.7439(7) 0.055(3) Uani 1 1 d . . . C52 C 0.6344(12) 1.0837(10) 0.8524(9) 0.095(5) Uani 1 1 d . . . H52A H 0.5775 1.0238 0.8297 0.114 Uiso 1 1 calc R . . C53 C 0.5917(17) 1.1627(12) 0.8696(13) 0.181(10) Uani 1 1 d . . . H53A H 0.5487 1.1604 0.9091 0.271 Uiso 1 1 calc R . . H53B H 0.5509 1.1572 0.8192 0.271 Uiso 1 1 calc R . . H53C H 0.6483 1.2209 0.8914 0.271 Uiso 1 1 calc R . . C54 C 0.7043(17) 1.0914(15) 0.9292(10) 0.168(9) Uani 1 1 d . . . H54A H 0.7332 1.0421 0.9151 0.252 Uiso 1 1 calc R . . H54B H 0.6641 1.0865 0.9701 0.252 Uiso 1 1 calc R . . H54C H 0.7596 1.1504 0.9509 0.252 Uiso 1 1 calc R . . S S 0.6696(2) 0.41164(19) 0.28101(18) 0.0532(8) Uani 1 1 d . . . O13 O 0.6593(5) 0.4940(5) 0.2660(5) 0.067(2) Uani 1 1 d . . . O15 O 0.7734(6) 0.4142(5) 0.2801(5) 0.076(3) Uani 1 1 d . . . O14 O 0.6445(6) 0.4133(6) 0.3586(5) 0.087(3) Uani 1 1 d . . . O16 O 0.5957(8) 0.3304(6) 0.2157(6) 0.126(4) Uani 1 1 d . . . O17 O 0.1908(6) 0.7806(5) 0.3186(5) 0.079(2) Uani 1 1 d . . . O18 O 0.8909(7) 0.1514(7) 0.1265(6) 0.101(3) Uani 1 1 d . . . O19 O 0.7625(8) 0.2565(7) 0.1297(6) 0.113(3) Uani 1 1 d . . . O20 O 0.4063(12) 0.1412(12) 1.0091(8) 0.210(7) Uani 1 1 d . . . O21 O 0.3627(13) 0.9860(9) 0.8718(10) 0.234(9) Uani 1 1 d . . . O22 O 0.5121(13) 0.1579(11) 0.2150(17) 0.280(13) Uani 1 1 d . . . O23 O 0.5198(16) 0.3175(13) 0.0684(9) 0.273(10) Uani 1 1 d . . . O24 O 0.5495(16) 0.1193(14) 0.0997(19) 0.307(12) Uani 1 1 d . . . O25 O 0.304(3) 0.504(2) 0.8877(15) 0.184(12) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0382(9) 0.0469(9) 0.0391(9) 0.0248(8) 0.0069(7) 0.0157(6) N1 0.029(4) 0.048(5) 0.048(6) 0.025(5) 0.003(4) 0.018(4) N2 0.034(5) 0.072(6) 0.076(8) 0.035(6) 0.003(5) 0.014(4) N3 0.041(5) 0.045(5) 0.055(6) 0.019(5) 0.012(5) 0.021(4) N4 0.086(8) 0.083(7) 0.037(6) 0.021(6) 0.027(6) 0.044(6) N5 0.033(5) 0.043(5) 0.038(5) 0.019(4) 0.010(4) 0.019(4) N6 0.045(5) 0.053(5) 0.069(7) 0.036(5) 0.005(5) 0.013(4) N7 0.042(5) 0.049(5) 0.026(5) 0.018(4) 0.011(4) 0.024(4) N8 0.042(5) 0.054(6) 0.071(7) 0.022(5) -0.025(5) 0.008(4) N9 0.028(4) 0.042(4) 0.044(5) 0.026(4) 0.012(4) 0.015(3) N10 0.066(6) 0.055(5) 0.034(5) 0.022(5) 0.023(5) 0.032(4) N11 0.032(5) 0.042(5) 0.035(5) 0.018(4) 0.001(4) 0.009(4) N12 0.056(6) 0.040(5) 0.046(6) 0.018(5) 0.014(5) 0.022(4) O1 0.053(6) 0.212(12) 0.108(9) 0.030(8) -0.002(6) 0.066(7) O2 0.055(6) 0.101(7) 0.092(7) 0.043(6) -0.016(5) 0.022(5) O3 0.093(8) 0.202(12) 0.072(7) 0.041(8) 0.033(7) 0.048(8) O4 0.101(8) 0.136(8) 0.050(6) 0.043(6) 0.021(6) 0.044(6) O5 0.085(6) 0.075(5) 0.116(8) 0.069(6) -0.003(6) 0.014(4) O6 0.068(6) 0.071(5) 0.115(8) 0.059(6) -0.015(6) -0.001(5) O7 0.062(5) 0.056(5) 0.087(6) 0.039(5) -0.027(5) 0.003(4) O8 0.077(6) 0.067(5) 0.082(7) 0.030(5) -0.014(5) 0.006(5) O9 0.093(6) 0.060(5) 0.081(6) 0.031(5) 0.041(5) 0.015(4) O10 0.106(7) 0.043(5) 0.050(5) 0.002(4) 0.045(5) 0.016(4) O11 0.096(6) 0.060(5) 0.089(7) 0.039(5) 0.044(5) 0.030(4) O12 0.096(6) 0.065(5) 0.055(5) 0.017(5) 0.035(5) 0.035(4) C1 0.030(6) 0.042(5) 0.066(8) 0.036(6) 0.010(6) 0.013(4) C2 0.035(6) 0.065(7) 0.069(9) 0.027(7) 0.001(6) 0.024(5) C3 0.036(7) 0.074(8) 0.090(11) 0.029(8) 0.030(8) 0.020(6) C4 0.048(8) 0.091(9) 0.061(9) 0.035(8) 0.020(7) 0.029(6) C5 0.039(6) 0.046(6) 0.056(8) 0.014(6) 0.016(6) 0.017(5) C6 0.056(7) 0.062(7) 0.043(7) 0.029(6) 0.021(6) 0.032(6) C7 0.058(8) 0.078(8) 0.081(10) 0.047(8) 0.034(8) 0.029(6) C8 0.104(11) 0.092(9) 0.060(9) 0.043(8) 0.044(9) 0.058(8) C9 0.067(8) 0.071(7) 0.043(8) 0.032(7) 0.027(7) 0.035(6) C10 0.054(7) 0.049(6) 0.047(7) 0.023(6) 0.007(6) 0.025(5) C11 0.038(8) 0.077(9) 0.087(12) 0.022(9) -0.020(8) 0.007(7) C12 0.063(10) 0.117(13) 0.17(2) 0.043(14) -0.055(12) 0.020(9) C13 0.19(2) 0.20(2) 0.18(2) 0.042(18) -0.083(18) 0.112(18) C14 0.127(16) 0.156(18) 0.109(16) 0.033(15) -0.037(13) 0.026(13) C15 0.078(11) 0.085(9) 0.062(10) 0.027(8) 0.019(9) 0.034(8) C16 0.142(14) 0.088(10) 0.045(9) 0.024(9) 0.037(9) 0.031(9) C17 0.161(17) 0.138(16) 0.087(13) 0.040(12) 0.036(13) 0.056(13) C18 0.21(2) 0.152(16) 0.079(12) 0.082(12) 0.037(13) 0.065(14) C19 0.041(6) 0.040(6) 0.037(6) 0.019(5) 0.007(5) 0.015(5) C20 0.044(6) 0.033(5) 0.054(7) 0.017(5) 0.009(6) 0.012(5) C21 0.041(6) 0.062(7) 0.060(8) 0.035(7) -0.002(6) 0.018(6) C22 0.047(7) 0.066(7) 0.059(8) 0.036(7) -0.007(6) 0.018(6) C23 0.028(5) 0.039(5) 0.048(7) 0.023(5) -0.001(5) 0.006(4) C24 0.044(6) 0.043(6) 0.043(7) 0.022(5) 0.002(5) 0.015(5) C25 0.042(6) 0.049(6) 0.056(7) 0.024(6) 0.002(6) 0.022(5) C26 0.050(7) 0.065(8) 0.073(9) 0.025(7) -0.008(6) 0.029(6) C27 0.052(7) 0.054(7) 0.033(6) 0.016(6) -0.003(5) 0.017(5) C28 0.052(7) 0.038(6) 0.043(7) 0.021(5) 0.002(5) 0.014(5) C29 0.079(10) 0.066(8) 0.076(10) 0.043(8) 0.019(8) 0.023(7) C30 0.120(12) 0.069(8) 0.235(19) 0.099(10) 0.032(13) 0.009(9) C31 0.224(17) 0.089(11) 0.28(2) 0.106(13) 0.058(17) -0.003(12) C32 0.160(16) 0.137(12) 0.27(2) 0.123(13) 0.073(16) 0.016(12) C33 0.058(8) 0.049(7) 0.064(9) 0.023(7) 0.002(7) 0.003(6) C34 0.095(11) 0.062(8) 0.109(13) 0.032(9) -0.033(10) 0.009(7) C35 0.151(17) 0.081(11) 0.136(17) -0.003(12) -0.037(14) 0.017(10) C36 0.103(12) 0.135(14) 0.128(15) 0.084(13) -0.015(11) -0.022(10) C37 0.029(5) 0.049(6) 0.039(6) 0.025(6) 0.004(5) 0.017(4) C38 0.037(6) 0.053(6) 0.033(6) 0.020(6) 0.009(5) 0.020(5) C39 0.074(8) 0.061(7) 0.039(7) 0.031(6) 0.035(6) 0.040(6) C40 0.056(7) 0.052(6) 0.055(7) 0.038(6) 0.022(6) 0.022(5) C41 0.036(6) 0.047(6) 0.052(7) 0.032(6) 0.013(5) 0.018(5) C42 0.033(6) 0.045(6) 0.043(6) 0.019(5) 0.010(5) 0.019(4) C43 0.061(7) 0.036(6) 0.049(7) 0.021(6) 0.007(6) 0.014(5) C44 0.066(7) 0.026(5) 0.043(7) 0.011(5) 0.011(6) 0.019(5) C45 0.036(6) 0.032(5) 0.042(6) 0.015(5) -0.003(5) 0.007(4) C46 0.031(5) 0.043(6) 0.030(6) 0.006(5) -0.002(5) 0.014(4) C47 0.069(8) 0.043(7) 0.039(7) 0.009(6) 0.023(6) 0.031(6) C48 0.146(15) 0.052(9) 0.126(15) 0.022(9) 0.086(14) 0.023(9) C49 0.27(3) 0.25(3) 0.100(16) 0.099(18) 0.011(19) 0.08(2) C50 0.22(2) 0.126(15) 0.30(3) 0.076(19) 0.20(3) 0.092(16) C51 0.064(8) 0.064(8) 0.037(7) 0.015(7) 0.008(6) 0.028(6) C52 0.110(12) 0.095(10) 0.093(12) 0.021(9) 0.066(11) 0.056(9) C53 0.27(3) 0.149(16) 0.24(2) 0.112(17) 0.19(2) 0.145(18) C54 0.22(2) 0.22(2) 0.054(11) 0.051(14) 0.041(14) 0.056(18) S 0.0379(16) 0.0683(19) 0.055(2) 0.0342(17) 0.0016(15) 0.0094(14) O13 0.068(5) 0.079(5) 0.079(6) 0.053(5) 0.020(4) 0.034(4) O15 0.066(5) 0.085(5) 0.140(8) 0.087(6) 0.063(5) 0.052(4) O14 0.074(6) 0.145(8) 0.091(7) 0.086(6) 0.043(5) 0.051(5) O16 0.127(9) 0.092(7) 0.093(8) 0.033(6) -0.047(7) -0.033(6) O17 0.096(6) 0.067(5) 0.083(6) 0.046(5) 0.008(5) 0.023(4) O18 0.097(7) 0.137(8) 0.093(7) 0.067(7) 0.022(6) 0.046(6) O19 0.122(8) 0.137(8) 0.091(7) 0.038(7) 0.020(7) 0.065(7) O20 0.187(15) 0.264(18) 0.114(11) 0.052(12) 0.033(11) 0.004(12) O21 0.263(17) 0.116(9) 0.211(15) 0.057(10) -0.174(14) -0.014(10) O22 0.210(16) 0.181(13) 0.61(4) 0.26(2) 0.25(2) 0.119(12) O23 0.29(2) 0.29(2) 0.119(12) 0.079(13) -0.097(13) -0.033(16) O24 0.189(18) 0.27(2) 0.46(4) 0.21(2) 0.02(2) 0.012(15) O25 0.28(3) 0.27(3) 0.119(19) 0.16(2) 0.09(2) 0.15(3) _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 Fe N5 1.955(7) . ? Fe N1 1.965(8) . ? Fe N9 1.965(8) . ? Fe N3 1.972(8) . ? Fe N7 1.976(8) . ? Fe N11 1.991(7) . ? N1 C1 1.339(12) . ? N1 C5 1.381(12) . ? N2 C11 1.364(14) . ? N2 C2 1.422(14) . ? N3 C6 1.328(12) . ? N3 C10 1.388(12) . ? N4 C15 1.316(14) . ? N4 C9 1.417(14) . ? N5 C19 1.335(11) . ? N5 C23 1.365(11) . ? N6 C29 1.381(13) . ? N6 C20 1.409(12) . ? N7 C28 1.360(11) . ? N7 C24 1.380(10) . ? N8 C33 1.350(13) . ? N8 C27 1.405(12) . ? N9 C37 1.308(10) . ? N9 C41 1.380(10) . ? N10 C47 1.358(11) . ? N10 C38 1.359(11) . ? N11 C46 1.334(10) . ? N11 C42 1.348(11) . ? N12 C51 1.363(12) . ? N12 C45 1.363(11) . ? O1 C11 1.196(15) . ? O2 C11 1.338(16) . ? O2 C12 1.488(15) . ? O3 C15 1.222(14) . ? O4 C15 1.321(15) . ? O4 C16 1.475(14) . ? O5 C29 1.221(14) . ? O6 C29 1.311(15) . ? O6 C30 1.487(14) . ? O7 C33 1.198(13) . ? O8 C33 1.346(13) . ? O8 C34 1.492(14) . ? O9 C47 1.222(11) . ? O10 C47 1.314(11) . ? O10 C48 1.410(14) . ? O11 C51 1.222(12) . ? O12 C51 1.329(12) . ? O12 C52 1.490(14) . ? C1 C2 1.401(13) . ? C2 C3 1.376(14) . ? C3 C4 1.393(16) . ? C4 C5 1.399(14) . ? C5 C6 1.440(14) . ? C6 C7 1.402(14) . ? C7 C8 1.423(16) . ? C8 C9 1.374(16) . ? C9 C10 1.401(13) . ? C12 C13 1.46(2) . ? C12 C14 1.51(2) . ? C16 C17 1.478(19) . ? C16 C18 1.504(19) . ? C19 C20 1.414(11) . ? C20 C21 1.377(13) . ? C21 C22 1.387(14) . ? C22 C23 1.396(12) . ? C23 C24 1.475(12) . ? C24 C25 1.374(13) . ? C25 C26 1.360(13) . ? C26 C27 1.389(13) . ? C27 C28 1.403(13) . ? C30 C31 1.42(3) . ? C30 C32 1.47(2) . ? C34 C36 1.46(2) . ? C34 C35 1.51(2) . ? C37 C38 1.410(12) . ? C38 C39 1.415(12) . ? C39 C40 1.316(12) . ? C40 C41 1.421(13) . ? C41 C42 1.441(12) . ? C42 C43 1.442(12) . ? C43 C44 1.344(12) . ? C44 C45 1.379(12) . ? C45 C46 1.404(11) . ? C48 C50 1.40(2) . ? C48 C49 1.62(2) . ? C52 C53 1.522(18) . ? C52 C54 1.53(2) . ? S O15 1.429(7) . ? S O14 1.448(8) . ? S O16 1.455(9) . ? S O13 1.497(7) . ? 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 N5 Fe N1 94.2(3) . . ? N5 Fe N9 95.0(3) . . ? N1 Fe N9 93.4(3) . . ? N5 Fe N3 89.1(3) . . ? N1 Fe N3 81.2(4) . . ? N9 Fe N3 173.5(3) . . ? N5 Fe N7 82.2(3) . . ? N1 Fe N7 174.2(3) . . ? N9 Fe N7 91.3(3) . . ? N3 Fe N7 94.3(3) . . ? N5 Fe N11 175.3(3) . . ? N1 Fe N11 89.6(3) . . ? N9 Fe N11 82.0(3) . . ? N3 Fe N11 94.2(3) . . ? N7 Fe N11 94.3(3) . . ? C1 N1 C5 118.9(8) . . ? C1 N1 Fe 127.4(6) . . ? C5 N1 Fe 113.7(7) . . ? C11 N2 C2 123.4(11) . . ? C6 N3 C10 118.8(9) . . ? C6 N3 Fe 116.1(7) . . ? C10 N3 Fe 125.2(7) . . ? C15 N4 C9 124.4(11) . . ? C19 N5 C23 117.8(7) . . ? C19 N5 Fe 126.9(6) . . ? C23 N5 Fe 115.3(6) . . ? C29 N6 C20 125.2(10) . . ? C28 N7 C24 117.1(8) . . ? C28 N7 Fe 128.1(6) . . ? C24 N7 Fe 114.6(6) . . ? C33 N8 C27 127.0(9) . . ? C37 N9 C41 118.7(8) . . ? C37 N9 Fe 127.4(6) . . ? C41 N9 Fe 113.9(6) . . ? C47 N10 C38 127.1(8) . . ? C46 N11 C42 120.6(7) . . ? C46 N11 Fe 125.9(6) . . ? C42 N11 Fe 113.4(6) . . ? C51 N12 C45 127.2(8) . . ? C11 O2 C12 116.5(13) . . ? C15 O4 C16 119.3(11) . . ? C29 O6 C30 115.2(11) . . ? C33 O8 C34 119.5(9) . . ? C47 O10 C48 120.1(8) . . ? C51 O12 C52 117.3(9) . . ? N1 C1 C2 122.4(10) . . ? C3 C2 C1 119.5(11) . . ? C3 C2 N2 125.0(10) . . ? C1 C2 N2 115.4(10) . . ? C2 C3 C4 118.5(10) . . ? C3 C4 C5 120.4(10) . . ? N1 C5 C4 120.2(10) . . ? N1 C5 C6 114.8(9) . . ? C4 C5 C6 124.9(10) . . ? N3 C6 C7 122.4(10) . . ? N3 C6 C5 114.1(9) . . ? C7 C6 C5 123.6(10) . . ? C6 C7 C8 118.8(11) . . ? C9 C8 C7 119.0(10) . . ? C8 C9 C10 119.1(11) . . ? C8 C9 N4 125.2(10) . . ? C10 C9 N4 115.6(10) . . ? N3 C10 C9 121.8(10) . . ? O1 C11 O2 124.3(12) . . ? O1 C11 N2 128.4(15) . . ? O2 C11 N2 107.4(13) . . ? C13 C12 O2 109.1(13) . . ? C13 C12 C14 111.7(19) . . ? O2 C12 C14 105.9(15) . . ? O3 C15 N4 126.6(14) . . ? O3 C15 O4 122.6(13) . . ? N4 C15 O4 110.8(12) . . ? O4 C16 C17 107.4(12) . . ? O4 C16 C18 105.2(11) . . ? C17 C16 C18 112.1(15) . . ? N5 C19 C20 122.9(9) . . ? C21 C20 N6 125.2(8) . . ? C21 C20 C19 119.0(9) . . ? N6 C20 C19 115.8(9) . . ? C20 C21 C22 118.3(9) . . ? C21 C22 C23 120.2(9) . . ? N5 C23 C22 121.6(8) . . ? N5 C23 C24 114.3(7) . . ? C22 C23 C24 124.1(9) . . ? C25 C24 N7 121.9(8) . . ? C25 C24 C23 124.7(8) . . ? N7 C24 C23 113.3(8) . . ? C26 C25 C24 120.9(8) . . ? C25 C26 C27 118.6(10) . . ? C26 C27 C28 119.3(9) . . ? C26 C27 N8 117.8(9) . . ? C28 C27 N8 122.6(8) . . ? N7 C28 C27 122.0(8) . . ? O5 C29 O6 128.3(11) . . ? O5 C29 N6 123.8(13) . . ? O6 C29 N6 107.9(11) . . ? C31 C30 C32 103.6(18) . . ? C31 C30 O6 104.1(16) . . ? C32 C30 O6 107.7(12) . . ? O7 C33 O8 125.7(10) . . ? O7 C33 N8 126.4(10) . . ? O8 C33 N8 107.8(11) . . ? C36 C34 O8 108.3(13) . . ? C36 C34 C35 115.9(13) . . ? O8 C34 C35 104.2(12) . . ? N9 C37 C38 125.1(8) . . ? N10 C38 C37 118.7(8) . . ? N10 C38 C39 126.2(8) . . ? C37 C38 C39 115.2(9) . . ? C40 C39 C38 120.1(9) . . ? C39 C40 C41 122.2(8) . . ? N9 C41 C40 118.1(8) . . ? N9 C41 C42 114.0(8) . . ? C40 C41 C42 127.6(8) . . ? N11 C42 C41 116.0(7) . . ? N11 C42 C43 118.9(8) . . ? C41 C42 C43 125.1(9) . . ? C44 C43 C42 119.7(9) . . ? C43 C44 C45 120.7(8) . . ? N12 C45 C44 119.0(8) . . ? N12 C45 C46 123.0(9) . . ? C44 C45 C46 118.0(9) . . ? N11 C46 C45 122.0(9) . . ? O9 C47 O10 125.7(9) . . ? O9 C47 N10 125.4(10) . . ? O10 C47 N10 108.9(9) . . ? C50 C48 O10 111.9(15) . . ? C50 C48 C49 105.8(16) . . ? O10 C48 C49 104.9(14) . . ? O11 C51 O12 126.4(10) . . ? O11 C51 N12 124.8(10) . . ? O12 C51 N12 108.8(10) . . ? O12 C52 C53 104.4(12) . . ? O12 C52 C54 109.4(12) . . ? C53 C52 C54 111.9(15) . . ? O15 S O14 111.3(5) . . ? O15 S O16 111.9(6) . . ? O14 S O16 108.7(6) . . ? O15 S O13 107.3(4) . . ? O14 S O13 110.3(5) . . ? O16 S O13 107.1(6) . . ? 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 N5 Fe N1 C1 -87.8(7) . . . . ? N9 Fe N1 C1 7.5(7) . . . . ? N3 Fe N1 C1 -176.2(7) . . . . ? N7 Fe N1 C1 -138(3) . . . . ? N11 Fe N1 C1 89.5(7) . . . . ? N5 Fe N1 C5 92.8(6) . . . . ? N9 Fe N1 C5 -171.9(6) . . . . ? N3 Fe N1 C5 4.4(6) . . . . ? N7 Fe N1 C5 43(3) . . . . ? N11 Fe N1 C5 -89.9(6) . . . . ? N5 Fe N3 C6 -97.1(7) . . . . ? N1 Fe N3 C6 -2.8(6) . . . . ? N9 Fe N3 C6 32(3) . . . . ? N7 Fe N3 C6 -179.2(6) . . . . ? N11 Fe N3 C6 86.2(7) . . . . ? N5 Fe N3 C10 83.9(7) . . . . ? N1 Fe N3 C10 178.3(7) . . . . ? N9 Fe N3 C10 -147(3) . . . . ? N7 Fe N3 C10 1.9(7) . . . . ? N11 Fe N3 C10 -92.7(7) . . . . ? N1 Fe N5 C19 7.9(8) . . . . ? N9 Fe N5 C19 -86.0(7) . . . . ? N3 Fe N5 C19 89.0(8) . . . . ? N7 Fe N5 C19 -176.6(8) . . . . ? N11 Fe N5 C19 -136(4) . . . . ? N1 Fe N5 C23 -169.9(6) . . . . ? N9 Fe N5 C23 96.3(6) . . . . ? N3 Fe N5 C23 -88.8(7) . . . . ? N7 Fe N5 C23 5.6(6) . . . . ? N11 Fe N5 C23 46(4) . . . . ? N5 Fe N7 C28 -179.4(8) . . . . ? N1 Fe N7 C28 -129(3) . . . . ? N9 Fe N7 C28 85.8(8) . . . . ? N3 Fe N7 C28 -90.9(8) . . . . ? N11 Fe N7 C28 3.6(8) . . . . ? N5 Fe N7 C24 -4.9(6) . . . . ? N1 Fe N7 C24 46(3) . . . . ? N9 Fe N7 C24 -99.7(6) . . . . ? N3 Fe N7 C24 83.6(7) . . . . ? N11 Fe N7 C24 178.2(6) . . . . ? N5 Fe N9 C37 10.2(8) . . . . ? N1 Fe N9 C37 -84.3(7) . . . . ? N3 Fe N9 C37 -118(3) . . . . ? N7 Fe N9 C37 92.4(7) . . . . ? N11 Fe N9 C37 -173.4(7) . . . . ? N5 Fe N9 C41 -169.2(6) . . . . ? N1 Fe N9 C41 96.3(6) . . . . ? N3 Fe N9 C41 62(3) . . . . ? N7 Fe N9 C41 -87.0(6) . . . . ? N11 Fe N9 C41 7.1(6) . . . . ? N5 Fe N11 C46 -139(4) . . . . ? N1 Fe N11 C46 77.2(7) . . . . ? N9 Fe N11 C46 170.7(7) . . . . ? N3 Fe N11 C46 -4.0(7) . . . . ? N7 Fe N11 C46 -98.6(7) . . . . ? N5 Fe N11 C42 46(4) . . . . ? N1 Fe N11 C42 -98.1(6) . . . . ? N9 Fe N11 C42 -4.6(6) . . . . ? N3 Fe N11 C42 -179.2(6) . . . . ? N7 Fe N11 C42 86.1(6) . . . . ? C5 N1 C1 C2 1.2(12) . . . . ? Fe N1 C1 C2 -178.2(6) . . . . ? N1 C1 C2 C3 0.1(14) . . . . ? N1 C1 C2 N2 -177.8(8) . . . . ? C11 N2 C2 C3 23.2(16) . . . . ? C11 N2 C2 C1 -158.9(9) . . . . ? C1 C2 C3 C4 -1.3(15) . . . . ? N2 C2 C3 C4 176.4(10) . . . . ? C2 C3 C4 C5 1.2(16) . . . . ? C1 N1 C5 C4 -1.3(13) . . . . ? Fe N1 C5 C4 178.1(7) . . . . ? C1 N1 C5 C6 175.2(7) . . . . ? Fe N1 C5 C6 -5.3(10) . . . . ? C3 C4 C5 N1 0.1(15) . . . . ? C3 C4 C5 C6 -176.1(10) . . . . ? C10 N3 C6 C7 -0.8(13) . . . . ? Fe N3 C6 C7 -179.8(8) . . . . ? C10 N3 C6 C5 179.7(8) . . . . ? Fe N3 C6 C5 0.7(10) . . . . ? N1 C5 C6 N3 3.1(12) . . . . ? C4 C5 C6 N3 179.4(9) . . . . ? N1 C5 C6 C7 -176.5(9) . . . . ? C4 C5 C6 C7 -0.1(16) . . . . ? N3 C6 C7 C8 1.9(15) . . . . ? C5 C6 C7 C8 -178.7(9) . . . . ? C6 C7 C8 C9 -2.7(16) . . . . ? C7 C8 C9 C10 2.4(16) . . . . ? C7 C8 C9 N4 179.1(10) . . . . ? C15 N4 C9 C8 -6.1(17) . . . . ? C15 N4 C9 C10 170.7(10) . . . . ? C6 N3 C10 C9 0.6(13) . . . . ? Fe N3 C10 C9 179.4(7) . . . . ? C8 C9 C10 N3 -1.4(15) . . . . ? N4 C9 C10 N3 -178.4(8) . . . . ? C12 O2 C11 O1 6(2) . . . . ? C12 O2 C11 N2 -174.2(10) . . . . ? C2 N2 C11 O1 -6(2) . . . . ? C2 N2 C11 O2 175.2(9) . . . . ? C11 O2 C12 C13 76(2) . . . . ? C11 O2 C12 C14 -163.3(14) . . . . ? C9 N4 C15 O3 -3(2) . . . . ? C9 N4 C15 O4 176.6(9) . . . . ? C16 O4 C15 O3 -2.8(19) . . . . ? C16 O4 C15 N4 177.6(10) . . . . ? C15 O4 C16 C17 -117.9(14) . . . . ? C15 O4 C16 C18 122.6(14) . . . . ? C23 N5 C19 C20 1.6(13) . . . . ? Fe N5 C19 C20 -176.2(7) . . . . ? C29 N6 C20 C21 29.5(16) . . . . ? C29 N6 C20 C19 -151.0(10) . . . . ? N5 C19 C20 C21 2.6(15) . . . . ? N5 C19 C20 N6 -176.9(8) . . . . ? N6 C20 C21 C22 176.1(9) . . . . ? C19 C20 C21 C22 -3.4(15) . . . . ? C20 C21 C22 C23 0.1(16) . . . . ? C19 N5 C23 C22 -5.0(14) . . . . ? Fe N5 C23 C22 173.0(8) . . . . ? C19 N5 C23 C24 176.7(8) . . . . ? Fe N5 C23 C24 -5.3(10) . . . . ? C21 C22 C23 N5 4.2(16) . . . . ? C21 C22 C23 C24 -177.6(9) . . . . ? C28 N7 C24 C25 -4.7(14) . . . . ? Fe N7 C24 C25 -179.9(7) . . . . ? C28 N7 C24 C23 178.5(8) . . . . ? Fe N7 C24 C23 3.3(10) . . . . ? N5 C23 C24 C25 -175.4(9) . . . . ? C22 C23 C24 C25 6.2(16) . . . . ? N5 C23 C24 N7 1.3(12) . . . . ? C22 C23 C24 N7 -177.1(9) . . . . ? N7 C24 C25 C26 5.5(16) . . . . ? C23 C24 C25 C26 -178.1(10) . . . . ? C24 C25 C26 C27 -3.2(17) . . . . ? C25 C26 C27 C28 0.4(16) . . . . ? C25 C26 C27 N8 175.0(10) . . . . ? C33 N8 C27 C26 169.9(11) . . . . ? C33 N8 C27 C28 -15.7(17) . . . . ? C24 N7 C28 C27 1.9(13) . . . . ? Fe N7 C28 C27 176.3(7) . . . . ? C26 C27 C28 N7 0.2(15) . . . . ? N8 C27 C28 N7 -174.1(9) . . . . ? C30 O6 C29 O5 11(2) . . . . ? C30 O6 C29 N6 -169.9(11) . . . . ? C20 N6 C29 O5 -7.2(18) . . . . ? C20 N6 C29 O6 173.4(9) . . . . ? C29 O6 C30 C31 -133.1(16) . . . . ? C29 O6 C30 C32 117.2(17) . . . . ? C34 O8 C33 O7 -4.6(19) . . . . ? C34 O8 C33 N8 178.7(11) . . . . ? C27 N8 C33 O7 1(2) . . . . ? C27 N8 C33 O8 177.4(9) . . . . ? C33 O8 C34 C36 -84.8(14) . . . . ? C33 O8 C34 C35 151.3(12) . . . . ? C41 N9 C37 C38 -2.1(13) . . . . ? Fe N9 C37 C38 178.5(7) . . . . ? C47 N10 C38 C37 -157.5(9) . . . . ? C47 N10 C38 C39 22.1(15) . . . . ? N9 C37 C38 N10 -173.2(8) . . . . ? N9 C37 C38 C39 7.2(13) . . . . ? N10 C38 C39 C40 173.4(9) . . . . ? C37 C38 C39 C40 -7.0(14) . . . . ? C38 C39 C40 C41 2.2(15) . . . . ? C37 N9 C41 C40 -3.3(12) . . . . ? Fe N9 C41 C40 176.1(7) . . . . ? C37 N9 C41 C42 172.2(8) . . . . ? Fe N9 C41 C42 -8.4(9) . . . . ? C39 C40 C41 N9 3.3(14) . . . . ? C39 C40 C41 C42 -171.5(10) . . . . ? C46 N11 C42 C41 -174.2(8) . . . . ? Fe N11 C42 C41 1.3(10) . . . . ? C46 N11 C42 C43 4.2(12) . . . . ? Fe N11 C42 C43 179.7(7) . . . . ? N9 C41 C42 N11 4.6(12) . . . . ? C40 C41 C42 N11 179.6(9) . . . . ? N9 C41 C42 C43 -173.7(8) . . . . ? C40 C41 C42 C43 1.3(16) . . . . ? N11 C42 C43 C44 -4.7(14) . . . . ? C41 C42 C43 C44 173.6(9) . . . . ? C42 C43 C44 C45 3.5(15) . . . . ? C51 N12 C45 C44 164.0(10) . . . . ? C51 N12 C45 C46 -14.3(15) . . . . ? C43 C44 C45 N12 179.7(9) . . . . ? C43 C44 C45 C46 -1.9(14) . . . . ? C42 N11 C46 C45 -2.7(13) . . . . ? Fe N11 C46 C45 -177.7(6) . . . . ? N12 C45 C46 N11 179.7(8) . . . . ? C44 C45 C46 N11 1.4(13) . . . . ? C48 O10 C47 O9 3.1(19) . . . . ? C48 O10 C47 N10 -179.4(12) . . . . ? C38 N10 C47 O9 5.0(17) . . . . ? C38 N10 C47 O10 -172.6(9) . . . . ? C47 O10 C48 C50 133.4(15) . . . . ? C47 O10 C48 C49 -112.4(13) . . . . ? C52 O12 C51 O11 -1.2(17) . . . . ? C52 O12 C51 N12 177.2(10) . . . . ? C45 N12 C51 O11 -3.5(17) . . . . ? C45 N12 C51 O12 178.0(9) . . . . ? C51 O12 C52 C53 -157.8(13) . . . . ? C51 O12 C52 C54 82.3(15) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N10 H10A O15 0.87 1.93 2.788(11) 166.8 . N6 H6A O14 0.87 2.08 2.881(11) 153.7 . N2 H2A O13 0.87 1.96 2.792(11) 158.6 . _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 1.308 _refine_diff_density_min -0.810 _refine_diff_density_rms 0.140 ########## data_L1FeBF4 _database_code_depnum_ccdc_archive 'CCDC 800532' #TrackingRef '- bipy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H62 B2 F8 Fe N12 O14' _chemical_formula_weight 1284.59 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.774(17) _cell_length_b 25.57(2) _cell_length_c 15.47(2) _cell_angle_alpha 90.00 _cell_angle_beta 117.83(3) _cell_angle_gamma 90.00 _cell_volume 6567(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2664 _exptl_absorpt_coefficient_mu 0.318 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9539 _exptl_absorpt_correction_T_max 0.9689 _exptl_absorpt_process_details SADABS _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 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 13912 _diffrn_reflns_av_R_equivalents 0.0903 _diffrn_reflns_av_sigmaI/netI 0.1051 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 23.30 _reflns_number_total 4686 _reflns_number_gt 2435 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 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^)+(0.1360P)^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 4686 _refine_ls_number_parameters 398 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.1416 _refine_ls_R_factor_gt 0.0771 _refine_ls_wR_factor_ref 0.2478 _refine_ls_wR_factor_gt 0.2107 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.012 _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 Fe1 Fe 0.5000 0.15340(4) 0.2500 0.0514(4) Uani 1 2 d S . . O1 O 0.5030(5) 0.3673(3) 0.5465(5) 0.165(3) Uani 1 1 d . . . O2 O 0.6093(4) 0.3329(2) 0.6801(4) 0.135(2) Uani 1 1 d . . . O3 O 0.1107(4) 0.1521(2) -0.1710(4) 0.117(2) Uani 1 1 d . . . O4 O 0.1344(3) 0.07321(19) -0.2172(3) 0.0928(16) Uani 1 1 d . . . O5 O 0.3270(3) -0.0119(2) 0.4762(4) 0.0914(16) Uani 1 1 d . . . O6 O 0.3238(3) 0.05727(19) 0.5664(4) 0.0956(17) Uani 1 1 d . . . N1 N 0.4707(3) 0.20866(17) 0.3189(4) 0.0537(12) Uani 1 1 d . . . N2 N 0.3833(3) 0.15837(17) 0.1557(3) 0.0521(12) Uani 1 1 d . . . N3 N 0.5460(4) 0.2833(2) 0.5486(4) 0.0790(17) Uani 1 1 d . . . H3A H 0.5808 0.2607 0.5856 0.095 Uiso 1 1 d R . . N4 N 0.2218(3) 0.1033(2) -0.0715(4) 0.0801(17) Uani 1 1 d . . . H4A H 0.2451 0.0738 -0.0679 0.096 Uiso 1 1 d R . . N9 N 0.4756(3) 0.09436(16) 0.3158(3) 0.0498(12) Uani 1 1 d . . . N11 N 0.3879(3) 0.06605(19) 0.4786(4) 0.0700(15) Uani 1 1 d . . . H11 H 0.3980 0.0965 0.5053 0.084 Uiso 1 1 calc R . . C1 C 0.3926(4) 0.2260(2) 0.2682(4) 0.0593(16) Uani 1 1 d . . . C2 C 0.3633(5) 0.2654(2) 0.3063(5) 0.077(2) Uani 1 1 d . . . H2 H 0.3110 0.2776 0.2695 0.093 Uiso 1 1 calc R . . C3 C 0.4118(5) 0.2863(3) 0.3985(5) 0.086(2) Uani 1 1 d . . . H3 H 0.3923 0.3120 0.4244 0.103 Uiso 1 1 calc R . . C4 C 0.4909(5) 0.2676(2) 0.4513(5) 0.0648(18) Uani 1 1 d . . . C5 C 0.5181(4) 0.2295(2) 0.4078(4) 0.0580(16) Uani 1 1 d . . . H5 H 0.5712 0.2181 0.4419 0.070 Uiso 1 1 calc R . . C6 C 0.3433(4) 0.1986(2) 0.1755(4) 0.0566(16) Uani 1 1 d . . . C7 C 0.2626(4) 0.2093(3) 0.1113(5) 0.078(2) Uani 1 1 d . . . H7 H 0.2369 0.2367 0.1253 0.094 Uiso 1 1 calc R . . C8 C 0.2199(4) 0.1800(3) 0.0270(5) 0.082(2) Uani 1 1 d . . . H8 H 0.1667 0.1879 -0.0164 0.098 Uiso 1 1 calc R . . C9 C 0.2599(4) 0.1375(2) 0.0091(4) 0.0625(16) Uani 1 1 d . . . C10 C 0.3414(4) 0.1293(2) 0.0760(4) 0.0578(16) Uani 1 1 d . . . H10 H 0.3679 0.1018 0.0639 0.069 Uiso 1 1 calc R . . C11 C 0.5472(6) 0.3319(4) 0.5874(7) 0.109(3) Uani 1 1 d . . . C12 C 0.6238(10) 0.3826(5) 0.7366(9) 0.217(7) Uani 1 1 d . . . H12A H 0.6316 0.3756 0.8021 0.260 Uiso 1 1 calc R . . H12B H 0.5786 0.4063 0.7043 0.260 Uiso 1 1 calc R . . C13 C 0.7005(13) 0.4061(7) 0.7401(15) 0.289(10) Uani 1 1 d U . . H13A H 0.7060 0.4418 0.7614 0.433 Uiso 1 1 calc R . . H13B H 0.6968 0.4047 0.6761 0.433 Uiso 1 1 calc R . . H13C H 0.7466 0.3865 0.7850 0.433 Uiso 1 1 calc R . . C14 C 0.1517(4) 0.1132(3) -0.1547(5) 0.076(2) Uani 1 1 d . . . C15 C 0.0692(6) 0.0823(4) -0.3171(6) 0.126(3) Uani 1 1 d . . . H15A H 0.0276 0.1039 -0.3147 0.151 Uiso 1 1 calc R . . H15B H 0.0902 0.1005 -0.3553 0.151 Uiso 1 1 calc R . . C16 C 0.0349(6) 0.0317(4) -0.3629(7) 0.155(4) Uani 1 1 d . . . H16A H 0.0777 0.0074 -0.3503 0.232 Uiso 1 1 calc R . . H16B H 0.0029 0.0363 -0.4321 0.232 Uiso 1 1 calc R . . H16C H 0.0017 0.0182 -0.3360 0.232 Uiso 1 1 calc R . . C17 C 0.4833(3) 0.0458(2) 0.2842(4) 0.0531(15) Uani 1 1 d . . . C18 C 0.4581(4) 0.0006(2) 0.3155(4) 0.0622(17) Uani 1 1 d . . . H18 H 0.4631 -0.0322 0.2931 0.075 Uiso 1 1 calc R . . C19 C 0.4255(4) 0.0055(2) 0.3805(4) 0.0651(17) Uani 1 1 d . . . H19 H 0.4087 -0.0239 0.4015 0.078 Uiso 1 1 calc R . . C20 C 0.4189(4) 0.0550(2) 0.4126(4) 0.0576(16) Uani 1 1 d . . . C21 C 0.4451(4) 0.0984(2) 0.3795(4) 0.0562(16) Uani 1 1 d . . . H21 H 0.4413 0.1314 0.4023 0.067 Uiso 1 1 calc R . . C22 C 0.3439(4) 0.0332(3) 0.5036(5) 0.0713(19) Uani 1 1 d . . . C23 C 0.2671(6) 0.0297(3) 0.5930(7) 0.107(3) Uani 1 1 d . . . H23A H 0.2790 -0.0074 0.6002 0.129 Uiso 1 1 calc R . . H23B H 0.2731 0.0429 0.6548 0.129 Uiso 1 1 calc R . . C24 C 0.1839(7) 0.0382(5) 0.5157(9) 0.170(5) Uani 1 1 d . . . H24A H 0.1772 0.0742 0.4955 0.255 Uiso 1 1 calc R . . H24B H 0.1469 0.0299 0.5405 0.255 Uiso 1 1 calc R . . H24C H 0.1733 0.0162 0.4609 0.255 Uiso 1 1 calc R . . F1 F 0.1058(5) 0.3794(3) 0.0945(7) 0.220(4) Uani 1 1 d . . . F2 F 0.1563(4) 0.3039(2) 0.1487(5) 0.183(3) Uani 1 1 d . . . F3 F 0.2101(6) 0.3680(4) 0.2456(7) 0.256(5) Uani 1 1 d . . . F4 F 0.0849(5) 0.3461(4) 0.2057(6) 0.260(5) Uani 1 1 d . . . B1 B 0.1418(9) 0.3489(6) 0.1777(10) 0.114(4) Uani 1 1 d . . . O7 O 0.4195(5) 0.1704(3) 0.5524(6) 0.165(3) Uani 1 1 d D . . H7A H 0.4578 0.1621 0.6046 0.248 Uiso 1 1 calc R . . C25 C 0.3607(14) 0.2022(10) 0.5715(17) 0.390(14) Uani 1 1 d DU . . H25A H 0.3687 0.1953 0.6364 0.585 Uiso 1 1 calc R . . H25B H 0.3067 0.1930 0.5249 0.585 Uiso 1 1 calc R . . H25C H 0.3693 0.2388 0.5653 0.585 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 Fe1 0.0509(8) 0.0458(7) 0.0559(8) 0.000 0.0237(6) 0.000 O1 0.215(8) 0.088(5) 0.113(5) -0.030(4) 0.011(5) 0.046(5) O2 0.156(6) 0.115(5) 0.090(4) -0.046(4) 0.019(4) 0.006(4) O3 0.106(5) 0.108(4) 0.087(4) -0.012(3) 0.001(3) 0.035(4) O4 0.079(4) 0.097(4) 0.073(3) -0.022(3) 0.011(3) 0.005(3) O5 0.110(4) 0.069(3) 0.116(4) -0.010(3) 0.071(4) -0.026(3) O6 0.117(5) 0.091(4) 0.110(4) -0.012(3) 0.080(4) -0.023(3) N1 0.058(3) 0.043(3) 0.060(3) -0.001(2) 0.027(3) -0.003(3) N2 0.056(3) 0.045(3) 0.056(3) -0.002(2) 0.027(3) 0.002(3) N3 0.093(5) 0.061(4) 0.076(4) -0.018(3) 0.034(4) 0.002(3) N4 0.060(4) 0.073(4) 0.086(4) -0.018(3) 0.016(3) 0.013(3) N9 0.047(3) 0.042(3) 0.054(3) -0.004(2) 0.018(3) -0.004(2) N11 0.089(4) 0.057(3) 0.081(4) -0.005(3) 0.054(4) -0.012(3) C1 0.061(4) 0.050(4) 0.062(4) -0.004(3) 0.026(4) 0.004(3) C2 0.084(5) 0.068(4) 0.079(5) -0.011(4) 0.037(4) 0.015(4) C3 0.091(6) 0.081(5) 0.084(5) -0.022(4) 0.038(5) 0.017(5) C4 0.083(5) 0.048(4) 0.062(4) -0.005(3) 0.033(4) -0.008(4) C5 0.061(4) 0.047(3) 0.063(4) -0.007(3) 0.027(4) -0.007(3) C6 0.056(4) 0.046(3) 0.066(4) 0.004(3) 0.026(3) 0.007(3) C7 0.069(5) 0.072(5) 0.078(5) -0.012(4) 0.022(4) 0.023(4) C8 0.059(5) 0.082(5) 0.082(5) -0.011(4) 0.015(4) 0.020(4) C9 0.062(4) 0.057(4) 0.062(4) -0.010(3) 0.023(4) 0.004(3) C10 0.052(4) 0.051(4) 0.061(4) -0.005(3) 0.019(3) 0.009(3) C11 0.129(8) 0.095(7) 0.084(6) -0.025(5) 0.034(6) 0.004(6) C12 0.261(18) 0.167(11) 0.158(11) -0.102(10) 0.044(12) 0.021(12) C13 0.277(13) 0.253(13) 0.305(13) -0.047(9) 0.110(9) 0.002(9) C14 0.064(5) 0.080(5) 0.066(5) -0.009(4) 0.014(4) 0.000(4) C15 0.127(8) 0.119(7) 0.079(6) -0.019(5) 0.003(6) 0.007(6) C16 0.153(10) 0.170(10) 0.120(8) -0.064(8) 0.046(7) -0.031(8) C17 0.054(4) 0.046(3) 0.056(4) 0.000(3) 0.023(3) 0.000(3) C18 0.072(5) 0.047(4) 0.067(4) 0.000(3) 0.032(4) 0.000(3) C19 0.084(5) 0.047(4) 0.070(4) 0.006(3) 0.040(4) -0.008(3) C20 0.057(4) 0.057(4) 0.058(4) 0.001(3) 0.026(3) -0.006(3) C21 0.059(4) 0.051(4) 0.057(4) 0.000(3) 0.026(3) -0.004(3) C22 0.076(5) 0.073(5) 0.072(5) -0.005(4) 0.041(4) -0.017(4) C23 0.116(8) 0.122(7) 0.121(7) -0.004(6) 0.087(7) -0.026(6) C24 0.102(9) 0.240(14) 0.190(12) 0.010(10) 0.086(9) -0.009(9) F1 0.276(10) 0.167(6) 0.254(9) 0.065(7) 0.153(9) 0.069(7) F2 0.144(5) 0.106(4) 0.224(7) -0.057(5) 0.023(5) 0.029(4) F3 0.198(8) 0.274(10) 0.275(10) -0.184(9) 0.094(8) -0.068(7) F4 0.186(8) 0.425(15) 0.205(8) 0.023(8) 0.122(7) 0.041(8) B1 0.120(11) 0.119(10) 0.110(9) -0.003(8) 0.059(9) -0.007(9) O7 0.179(8) 0.108(5) 0.220(8) -0.044(6) 0.101(7) -0.020(5) C25 0.400(17) 0.422(17) 0.379(17) 0.032(10) 0.207(11) -0.008(10) _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 Fe1 N9 1.990(4) . ? Fe1 N9 1.990(4) 2_655 ? Fe1 N2 1.991(5) . ? Fe1 N2 1.991(5) 2_655 ? Fe1 N1 1.996(5) . ? Fe1 N1 1.996(5) 2_655 ? O1 C11 1.192(10) . ? O2 C11 1.362(10) . ? O2 C12 1.491(10) . ? O3 C14 1.212(8) . ? O4 C14 1.338(8) . ? O4 C15 1.475(9) . ? O5 C22 1.219(7) . ? O6 C22 1.344(8) . ? O6 C23 1.486(8) . ? N1 C5 1.350(7) . ? N1 C1 1.374(8) . ? N2 C10 1.336(7) . ? N2 C6 1.390(7) . ? N3 C11 1.375(9) . ? N3 C4 1.429(8) . ? N3 H3A 0.8599 . ? N4 C14 1.368(8) . ? N4 C9 1.415(8) . ? N4 H4A 0.8600 . ? N9 C21 1.356(7) . ? N9 C17 1.367(6) . ? N11 C22 1.355(8) . ? N11 C20 1.422(7) . ? N11 H11 0.8600 . ? C1 C2 1.402(8) . ? C1 C6 1.470(8) . ? C2 C3 1.392(9) . ? C2 H2 0.9300 . ? C3 C4 1.405(9) . ? C3 H3 0.9300 . ? C4 C5 1.408(8) . ? C5 H5 0.9300 . ? C6 C7 1.396(9) . ? C7 C8 1.390(9) . ? C7 H7 0.9300 . ? C8 C9 1.418(8) . ? C8 H8 0.9300 . ? C9 C10 1.407(8) . ? C10 H10 0.9300 . ? C12 C13 1.54(2) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C15 C16 1.472(11) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.417(7) . ? C17 C17 1.458(11) 2_655 ? C18 C19 1.405(8) . ? C18 H18 0.9300 . ? C19 C20 1.385(8) . ? C19 H19 0.9300 . ? C20 C21 1.403(7) . ? C21 H21 0.9300 . ? C23 C24 1.474(13) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? F1 B1 1.382(13) . ? F2 B1 1.310(13) . ? F3 B1 1.315(14) . ? F4 B1 1.327(13) . ? O7 C25 1.506(17) . ? O7 H7A 0.8200 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N9 Fe1 N9 81.3(3) . 2_655 ? N9 Fe1 N2 89.17(19) . . ? N9 Fe1 N2 96.38(19) 2_655 . ? N9 Fe1 N2 96.38(19) . 2_655 ? N9 Fe1 N2 89.17(19) 2_655 2_655 ? N2 Fe1 N2 172.7(3) . 2_655 ? N9 Fe1 N1 94.43(19) . . ? N9 Fe1 N1 175.50(18) 2_655 . ? N2 Fe1 N1 82.1(2) . . ? N2 Fe1 N1 92.7(2) 2_655 . ? N9 Fe1 N1 175.51(18) . 2_655 ? N9 Fe1 N1 94.43(19) 2_655 2_655 ? N2 Fe1 N1 92.7(2) . 2_655 ? N2 Fe1 N1 82.1(2) 2_655 2_655 ? N1 Fe1 N1 89.9(3) . 2_655 ? C11 O2 C12 117.8(8) . . ? C14 O4 C15 116.0(6) . . ? C22 O6 C23 117.5(6) . . ? C5 N1 C1 118.4(5) . . ? C5 N1 Fe1 127.4(4) . . ? C1 N1 Fe1 114.2(4) . . ? C10 N2 C6 118.0(5) . . ? C10 N2 Fe1 127.8(4) . . ? C6 N2 Fe1 114.1(4) . . ? C11 N3 C4 124.8(7) . . ? C11 N3 H3A 117.6 . . ? C4 N3 H3A 117.6 . . ? C14 N4 C9 125.7(6) . . ? C14 N4 H4A 117.4 . . ? C9 N4 H4A 117.0 . . ? C21 N9 C17 118.7(5) . . ? C21 N9 Fe1 126.2(4) . . ? C17 N9 Fe1 114.7(4) . . ? C22 N11 C20 126.2(5) . . ? C22 N11 H11 116.9 . . ? C20 N11 H11 116.9 . . ? N1 C1 C2 121.0(6) . . ? N1 C1 C6 115.0(5) . . ? C2 C1 C6 124.0(6) . . ? C3 C2 C1 120.7(7) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 118.2(6) . . ? C2 C3 H3 120.9 . . ? C4 C3 H3 120.9 . . ? C3 C4 C5 118.6(6) . . ? C3 C4 N3 124.4(6) . . ? C5 C4 N3 116.9(6) . . ? N1 C5 C4 123.0(6) . . ? N1 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? N2 C6 C7 120.4(6) . . ? N2 C6 C1 114.1(5) . . ? C7 C6 C1 125.5(6) . . ? C8 C7 C6 121.3(6) . . ? C8 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C7 C8 C9 118.1(6) . . ? C7 C8 H8 120.9 . . ? C9 C8 H8 120.9 . . ? C10 C9 N4 119.0(5) . . ? C10 C9 C8 117.6(6) . . ? N4 C9 C8 123.4(6) . . ? N2 C10 C9 124.4(5) . . ? N2 C10 H10 117.8 . . ? C9 C10 H10 117.8 . . ? O1 C11 O2 125.9(8) . . ? O1 C11 N3 126.0(9) . . ? O2 C11 N3 108.1(8) . . ? O2 C12 C13 105.4(13) . . ? O2 C12 H12A 110.7 . . ? C13 C12 H12A 110.7 . . ? O2 C12 H12B 110.7 . . ? C13 C12 H12B 110.7 . . ? H12A C12 H12B 108.8 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O3 C14 O4 124.2(7) . . ? O3 C14 N4 125.9(7) . . ? O4 C14 N4 109.9(7) . . ? C16 C15 O4 109.2(8) . . ? C16 C15 H15A 109.8 . . ? O4 C15 H15A 109.8 . . ? C16 C15 H15B 109.8 . . ? O4 C15 H15B 109.8 . . ? H15A C15 H15B 108.3 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N9 C17 C18 120.6(5) . . ? N9 C17 C17 114.3(3) . 2_655 ? C18 C17 C17 125.0(3) . 2_655 ? C19 C18 C17 120.0(5) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C20 C19 C18 118.6(5) . . ? C20 C19 H19 120.7 . . ? C18 C19 H19 120.7 . . ? C19 C20 C21 119.1(5) . . ? C19 C20 N11 125.1(5) . . ? C21 C20 N11 115.8(5) . . ? N9 C21 C20 122.9(5) . . ? N9 C21 H21 118.5 . . ? C20 C21 H21 118.5 . . ? O5 C22 O6 124.8(6) . . ? O5 C22 N11 125.6(6) . . ? O6 C22 N11 109.6(6) . . ? C24 C23 O6 109.3(7) . . ? C24 C23 H23A 109.8 . . ? O6 C23 H23A 109.8 . . ? C24 C23 H23B 109.8 . . ? O6 C23 H23B 109.8 . . ? H23A C23 H23B 108.3 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? F2 B1 F3 108.6(12) . . ? F2 B1 F4 113.1(12) . . ? F3 B1 F4 113.2(11) . . ? F2 B1 F1 105.4(10) . . ? F3 B1 F1 113.9(12) . . ? F4 B1 F1 102.5(12) . . ? C25 O7 H7A 109.5 . . ? O7 C25 H25A 109.5 . . ? O7 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O7 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3A F2 0.86 2.10 2.943(9) 167.9 8_556 O7 H7A F4 0.82 2.17 2.928(13) 154.2 8_556 N4 H4A O5 0.86 2.09 2.922(8) 163.9 6 N11 H11 O7 0.86 2.00 2.854(9) 173.5 . _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 23.30 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.763 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.073 ############### data_L2Fe(Et2O)BF4 _database_code_depnum_ccdc_archive 'CCDC 800533' #TrackingRef '- bipy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H94 B2 F8 Fe N12 O16' _chemical_formula_weight 1516.98 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 18.4694(16) _cell_length_b 19.7057(17) _cell_length_c 23.748(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.2390(10) _cell_angle_gamma 90.00 _cell_volume 8209.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.227 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3192 _exptl_absorpt_coefficient_mu 0.266 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9487 _exptl_absorpt_correction_T_max 0.9611 _exptl_absorpt_process_details SADABS _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 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 37981 _diffrn_reflns_av_R_equivalents 0.0496 _diffrn_reflns_av_sigmaI/netI 0.0428 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 21.08 _reflns_number_total 8777 _reflns_number_gt 5911 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 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^)+(0.1351P)^2^+12.1585P] 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 8777 _refine_ls_number_parameters 948 _refine_ls_number_restraints 148 _refine_ls_R_factor_all 0.1114 _refine_ls_R_factor_gt 0.0740 _refine_ls_wR_factor_ref 0.2390 _refine_ls_wR_factor_gt 0.2047 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.079 _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 Fe1 Fe 0.24700(5) 0.49285(4) -0.00138(3) 0.0412(3) Uani 1 1 d . . . B1 B 0.6282(8) 0.3114(7) 0.1422(7) 0.187(8) Uani 1 1 d DU . . F1 F 0.6132(5) 0.3636(5) 0.1061(5) 0.267(6) Uani 1 1 d D . . F2 F 0.5636(5) 0.2817(7) 0.1400(6) 0.339(8) Uani 1 1 d D . . F3 F 0.6637(7) 0.3302(7) 0.1985(5) 0.291(6) Uani 1 1 d D . . F4 F 0.6761(6) 0.2705(6) 0.1276(5) 0.274(6) Uani 1 1 d D . . B2 B 0.0127(8) 0.3712(8) 0.2011(6) 0.176(7) Uani 1 1 d DU . . F5 F -0.0058(5) 0.4025(5) 0.1509(3) 0.227(5) Uani 1 1 d D . . F6 F 0.0846(5) 0.3801(6) 0.2311(4) 0.251(5) Uani 1 1 d D . . F7 F -0.0295(7) 0.3884(9) 0.2326(5) 0.325(9) Uani 1 1 d D . . F8 F -0.0020(8) 0.3054(6) 0.1947(6) 0.336(8) Uani 1 1 d D . . N1 N 0.3555(3) 0.5173(2) 0.0246(2) 0.0448(12) Uani 1 1 d . . . N2 N 0.2908(3) 0.4006(2) 0.01193(19) 0.0445(12) Uani 1 1 d . . . N3 N 0.4825(3) 0.6629(3) 0.0524(3) 0.0741(17) Uani 1 1 d . . . H3A H 0.4478 0.6906 0.0327 0.089 Uiso 1 1 calc R . . N4 N 0.2397(3) 0.2221(3) -0.0070(2) 0.0715(17) Uani 1 1 d . . . H4A H 0.1949 0.2301 -0.0310 0.086 Uiso 1 1 calc R . . N5 N 0.2420(3) 0.4909(2) 0.0808(2) 0.0428(12) Uani 1 1 d . . . N6 N 0.1411(3) 0.4611(2) -0.01875(19) 0.0414(12) Uani 1 1 d . . . N7 N 0.3523(4) 0.5236(3) 0.2343(2) 0.0803(19) Uani 1 1 d . . . H7A H 0.3871 0.5455 0.2248 0.096 Uiso 1 1 calc R . . N8 N -0.0272(3) 0.4145(3) -0.1396(2) 0.0598(15) Uani 1 1 d . . . H8A H -0.0104 0.4312 -0.1666 0.072 Uiso 1 1 calc R . . N9 N 0.2107(3) 0.5870(2) -0.0188(2) 0.0429(12) Uani 1 1 d . . . N10 N 0.2424(3) 0.4962(2) -0.0852(2) 0.0425(12) Uani 1 1 d . . . N11 N 0.1631(3) 0.7387(3) 0.0490(2) 0.0670(16) Uani 1 1 d . . . H11A H 0.1565 0.7187 0.0792 0.080 Uiso 1 1 calc R . . N12 N 0.2708(3) 0.3931(3) -0.2031(2) 0.0663(16) Uani 1 1 d . . . H12A H 0.3006 0.3643 -0.1798 0.080 Uiso 1 1 calc R . . O1 O 0.6086(3) 0.6587(2) 0.1060(2) 0.0844(16) Uani 1 1 d . . . O2 O 0.5466(3) 0.7568(3) 0.0757(3) 0.120(2) Uani 1 1 d . . . O3 O 0.3119(4) 0.1370(3) 0.0460(4) 0.142(3) Uani 1 1 d . . . O4 O 0.1984(4) 0.1182(3) -0.0218(3) 0.120(2) Uani 1 1 d . . . O5 O 0.3211(4) 0.4882(4) 0.3138(2) 0.115(2) Uani 1 1 d . . . O6 O 0.4287(4) 0.5430(4) 0.3228(2) 0.119(2) Uani 1 1 d . . . O7 O -0.1310(3) 0.3605(2) -0.1280(2) 0.0669(13) Uani 1 1 d . . . O8 O -0.1151(3) 0.3766(3) -0.21807(19) 0.0780(15) Uani 1 1 d . . . O9 O 0.1659(6) 0.8426(3) 0.0102(3) 0.151(3) Uani 1 1 d . . . O10 O 0.1574(5) 0.8283(3) 0.1008(3) 0.123(2) Uani 1 1 d . . . O11 O 0.2146(5) 0.4154(3) -0.3007(3) 0.130(3) Uani 1 1 d . . . O12 O 0.2721(4) 0.3162(3) -0.2684(2) 0.104(2) Uani 1 1 d . . . O13 O 0.4614(8) 0.6133(7) 0.2039(5) 0.230(4) Uani 1 1 d DU . . O14 O 0.0918(4) 0.2457(3) 0.4134(3) 0.112(2) Uani 1 1 d . . . O15 O 0.3558(5) 0.7459(4) -0.0062(4) 0.157(3) Uani 1 1 d . . . H15 H 0.3698 0.7488 -0.0357 0.235 Uiso 1 1 calc R . . O16 O 0.0413(5) 0.0414(7) 0.2764(4) 0.185(4) Uani 1 1 d D . . H16A H 0.0867 0.0324 0.2844 0.278 Uiso 1 1 calc R . . C1 C 0.3846(4) 0.5798(3) 0.0276(3) 0.0515(16) Uani 1 1 d . . . H1 H 0.3513 0.6156 0.0128 0.062 Uiso 1 1 calc R . . C2 C 0.4615(4) 0.5941(3) 0.0514(3) 0.0566(17) Uani 1 1 d . . . C3 C 0.5111(4) 0.5405(4) 0.0725(3) 0.0648(19) Uani 1 1 d . . . H3 H 0.5632 0.5479 0.0891 0.078 Uiso 1 1 calc R . . C4 C 0.4815(4) 0.4760(3) 0.0682(3) 0.0608(18) Uani 1 1 d . . . H4 H 0.5142 0.4395 0.0817 0.073 Uiso 1 1 calc R . . C5 C 0.4047(4) 0.4646(3) 0.0445(3) 0.0476(15) Uani 1 1 d . . . C6 C 0.3674(4) 0.3986(3) 0.0370(2) 0.0499(16) Uani 1 1 d . . . C7 C 0.4043(4) 0.3373(3) 0.0511(3) 0.0649(19) Uani 1 1 d . . . H7 H 0.4568 0.3363 0.0690 0.078 Uiso 1 1 calc R . . C8 C 0.3640(4) 0.2770(3) 0.0388(3) 0.072(2) Uani 1 1 d . . . H8 H 0.3888 0.2356 0.0492 0.086 Uiso 1 1 calc R . . C9 C 0.2867(4) 0.2791(3) 0.0110(3) 0.0557(17) Uani 1 1 d . . . C10 C 0.2520(4) 0.3419(3) -0.0005(2) 0.0488(16) Uani 1 1 d . . . H10 H 0.1993 0.3436 -0.0176 0.059 Uiso 1 1 calc R . . C11 C 0.5513(5) 0.6898(4) 0.0810(4) 0.080(2) Uani 1 1 d . . . C12 C 0.6166(6) 0.7976(5) 0.1035(5) 0.120(3) Uani 1 1 d . . . H12 H 0.6626 0.7736 0.1025 0.144 Uiso 1 1 calc R . . C13 C 0.6062(8) 0.8621(6) 0.0694(6) 0.165(5) Uani 1 1 d . . . H13A H 0.5589 0.8829 0.0689 0.248 Uiso 1 1 calc R . . H13B H 0.6053 0.8528 0.0296 0.248 Uiso 1 1 calc R . . H13C H 0.6476 0.8923 0.0879 0.248 Uiso 1 1 calc R . . C14 C 0.6142(9) 0.8047(7) 0.1622(5) 0.179(6) Uani 1 1 d . . . H14A H 0.5735 0.8348 0.1625 0.268 Uiso 1 1 calc R . . H14B H 0.6618 0.8229 0.1869 0.268 Uiso 1 1 calc R . . H14C H 0.6058 0.7611 0.1771 0.268 Uiso 1 1 calc R . . C15 C 0.2550(6) 0.1570(4) 0.0082(4) 0.100(3) Uani 1 1 d . . . C16 C 0.1987(8) 0.0448(5) -0.0071(8) 0.171(6) Uani 1 1 d U . . H16 H 0.2232 0.0369 0.0354 0.206 Uiso 1 1 calc R . . C17 C 0.2407(11) 0.0131(8) -0.0419(9) 0.231(8) Uani 1 1 d U . . H17A H 0.2416 -0.0351 -0.0360 0.346 Uiso 1 1 calc R . . H17B H 0.2919 0.0302 -0.0299 0.346 Uiso 1 1 calc R . . H17C H 0.2165 0.0231 -0.0831 0.346 Uiso 1 1 calc R . . C18 C 0.1192(9) 0.0219(7) -0.0262(9) 0.238(10) Uani 1 1 d . . . H18A H 0.0938 0.0386 -0.0654 0.357 Uiso 1 1 calc R . . H18B H 0.0941 0.0389 0.0007 0.357 Uiso 1 1 calc R . . H18C H 0.1178 -0.0268 -0.0264 0.357 Uiso 1 1 calc R . . C19 C 0.2969(4) 0.5089(3) 0.1307(3) 0.0521(17) Uani 1 1 d . . . H19 H 0.3415 0.5277 0.1272 0.062 Uiso 1 1 calc R . . C20 C 0.2909(4) 0.5009(3) 0.1874(3) 0.0547(17) Uani 1 1 d . . . C21 C 0.2245(4) 0.4727(3) 0.1923(3) 0.0642(19) Uani 1 1 d . . . H21 H 0.2186 0.4661 0.2294 0.077 Uiso 1 1 calc R . . C22 C 0.1675(4) 0.4544(3) 0.1418(3) 0.0567(17) Uani 1 1 d . . . H22 H 0.1224 0.4358 0.1444 0.068 Uiso 1 1 calc R . . C23 C 0.1774(4) 0.4639(3) 0.0863(2) 0.0451(15) Uani 1 1 d . . . C24 C 0.1188(3) 0.4475(3) 0.0296(2) 0.0436(15) Uani 1 1 d . . . C25 C 0.0482(4) 0.4216(3) 0.0237(3) 0.0547(17) Uani 1 1 d . . . H25 H 0.0347 0.4122 0.0574 0.066 Uiso 1 1 calc R . . C26 C -0.0036(4) 0.4090(3) -0.0315(3) 0.0548(17) Uani 1 1 d . . . H26 H -0.0515 0.3910 -0.0353 0.066 Uiso 1 1 calc R . . C27 C 0.0182(4) 0.4240(3) -0.0809(3) 0.0497(16) Uani 1 1 d . . . C28 C 0.0903(4) 0.4498(3) -0.0722(3) 0.0470(15) Uani 1 1 d . . . H28 H 0.1045 0.4600 -0.1055 0.056 Uiso 1 1 calc R . . C29 C 0.3637(5) 0.5156(4) 0.2922(3) 0.075(2) Uani 1 1 d . . . C30 C 0.4508(8) 0.5410(8) 0.3878(4) 0.156(5) Uani 1 1 d U . . H30 H 0.4169 0.5124 0.4021 0.187 Uiso 1 1 calc R . . C31 C 0.5300(9) 0.5187(8) 0.4097(6) 0.207(7) Uani 1 1 d U . . H31A H 0.5366 0.4794 0.3879 0.311 Uiso 1 1 calc R . . H31B H 0.5428 0.5074 0.4510 0.311 Uiso 1 1 calc R . . H31C H 0.5627 0.5545 0.4047 0.311 Uiso 1 1 calc R . . C32 C 0.4479(12) 0.6124(10) 0.4041(6) 0.260(8) Uani 1 1 d U . . H32A H 0.4979 0.6319 0.4132 0.389 Uiso 1 1 calc R . . H32B H 0.4306 0.6155 0.4381 0.389 Uiso 1 1 calc R . . H32C H 0.4134 0.6365 0.3715 0.389 Uiso 1 1 calc R . . C33 C -0.0951(4) 0.3815(3) -0.1585(3) 0.0619(19) Uani 1 1 d . . . C34 C -0.1835(5) 0.3361(4) -0.2484(3) 0.086(2) Uani 1 1 d . . . H34 H -0.2241 0.3465 -0.2313 0.103 Uiso 1 1 calc R . . C35 C -0.2066(7) 0.3604(6) -0.3118(4) 0.142(4) Uani 1 1 d . . . H35A H -0.2127 0.4088 -0.3127 0.213 Uiso 1 1 calc R . . H35B H -0.2539 0.3395 -0.3339 0.213 Uiso 1 1 calc R . . H35C H -0.1678 0.3484 -0.3291 0.213 Uiso 1 1 calc R . . C36 C -0.1648(6) 0.2626(5) -0.2407(4) 0.115(3) Uani 1 1 d . . . H36A H -0.1254 0.2522 -0.2578 0.173 Uiso 1 1 calc R . . H36B H -0.2095 0.2364 -0.2601 0.173 Uiso 1 1 calc R . . H36C H -0.1474 0.2517 -0.1992 0.173 Uiso 1 1 calc R . . C37 C 0.1982(3) 0.6316(3) 0.0203(3) 0.0458(15) Uani 1 1 d . . . H37 H 0.2069 0.6178 0.0593 0.055 Uiso 1 1 calc R . . C38 C 0.1731(4) 0.6967(3) 0.0045(3) 0.0536(16) Uani 1 1 d . . . C39 C 0.1584(5) 0.7164(4) -0.0541(3) 0.078(2) Uani 1 1 d . . . H39 H 0.1397 0.7596 -0.0664 0.093 Uiso 1 1 calc R . . C40 C 0.1720(5) 0.6714(3) -0.0931(3) 0.078(2) Uani 1 1 d . . . H40 H 0.1627 0.6842 -0.1325 0.094 Uiso 1 1 calc R . . C41 C 0.1990(4) 0.6074(3) -0.0754(3) 0.0539(17) Uani 1 1 d . . . C42 C 0.2165(4) 0.5550(3) -0.1131(3) 0.0552(17) Uani 1 1 d . . . C43 C 0.2084(5) 0.5625(4) -0.1729(3) 0.082(2) Uani 1 1 d . . . H43 H 0.1907 0.6033 -0.1920 0.098 Uiso 1 1 calc R . . C44 C 0.2264(5) 0.5105(4) -0.2037(3) 0.079(2) Uani 1 1 d . . . H44 H 0.2214 0.5159 -0.2436 0.095 Uiso 1 1 calc R . . C45 C 0.2515(4) 0.4507(3) -0.1760(3) 0.0537(17) Uani 1 1 d . . . C46 C 0.2598(3) 0.4458(3) -0.1163(3) 0.0479(16) Uani 1 1 d . . . H46 H 0.2784 0.4055 -0.0969 0.058 Uiso 1 1 calc R . . C47 C 0.1627(6) 0.8059(4) 0.0497(4) 0.095(3) Uani 1 1 d . . . C48 C 0.1661(11) 0.9021(5) 0.1131(5) 0.152(6) Uani 1 1 d . . . H48 H 0.1525 0.9277 0.0759 0.183 Uiso 1 1 calc R . . C49 C 0.1157(9) 0.9191(7) 0.1458(7) 0.208(8) Uani 1 1 d . . . H49A H 0.0657 0.9019 0.1256 0.311 Uiso 1 1 calc R . . H49B H 0.1134 0.9675 0.1493 0.311 Uiso 1 1 calc R . . H49C H 0.1341 0.8993 0.1847 0.311 Uiso 1 1 calc R . . C50 C 0.2506(10) 0.9150(7) 0.1494(8) 0.209(8) Uani 1 1 d . . . H50A H 0.2595 0.9630 0.1542 0.313 Uiso 1 1 calc R . . H50B H 0.2830 0.8960 0.1288 0.313 Uiso 1 1 calc R . . H50C H 0.2616 0.8941 0.1877 0.313 Uiso 1 1 calc R . . C51 C 0.2485(6) 0.3776(4) -0.2610(4) 0.085(2) Uani 1 1 d . . . C52 C 0.2559(11) 0.2892(7) -0.3290(5) 0.172(5) Uani 1 1 d U . . H52 H 0.2589 0.3229 -0.3586 0.206 Uiso 1 1 calc R . . C53 C 0.1803(13) 0.2560(9) -0.3416(7) 0.255(9) Uani 1 1 d U . . H53A H 0.1566 0.2706 -0.3131 0.382 Uiso 1 1 calc R . . H53B H 0.1868 0.2076 -0.3393 0.382 Uiso 1 1 calc R . . H53C H 0.1487 0.2683 -0.3807 0.382 Uiso 1 1 calc R . . C54 C 0.3034(11) 0.2283(8) -0.3264(6) 0.211(6) Uani 1 1 d U . . H54A H 0.2955 0.1970 -0.2979 0.317 Uiso 1 1 calc R . . H54B H 0.3562 0.2412 -0.3147 0.317 Uiso 1 1 calc R . . H54C H 0.2895 0.2072 -0.3647 0.317 Uiso 1 1 calc R . . C55 C 0.3542(12) 0.7002(10) 0.1672(9) 0.269(8) Uani 1 1 d DU . . H55A H 0.3398 0.6702 0.1337 0.404 Uiso 1 1 calc R . . H55B H 0.3517 0.7463 0.1537 0.404 Uiso 1 1 calc R . . H55C H 0.3201 0.6943 0.1901 0.404 Uiso 1 1 calc R . . C56 C 0.4365(12) 0.6839(11) 0.2061(9) 0.250(6) Uani 1 1 d DU . . H56A H 0.4710 0.7134 0.1941 0.300 Uiso 1 1 calc R . . H56B H 0.4411 0.6948 0.2469 0.300 Uiso 1 1 calc R . . C57 C 0.5410(11) 0.6017(10) 0.2371(8) 0.234(6) Uani 1 1 d DU . . H57A H 0.5527 0.6169 0.2778 0.281 Uiso 1 1 calc R . . H57B H 0.5745 0.6245 0.2188 0.281 Uiso 1 1 calc R . . C58 C 0.5478(11) 0.5235(10) 0.2336(8) 0.239(7) Uani 1 1 d DU . . H58A H 0.4977 0.5037 0.2213 0.359 Uiso 1 1 calc R . . H58B H 0.5761 0.5061 0.2720 0.359 Uiso 1 1 calc R . . H58C H 0.5736 0.5121 0.2056 0.359 Uiso 1 1 calc R . . C59 C 0.1464(10) 0.2246(9) 0.3366(6) 0.205(8) Uani 1 1 d . . . H59A H 0.1881 0.2562 0.3469 0.307 Uiso 1 1 calc R . . H59B H 0.1319 0.2149 0.2950 0.307 Uiso 1 1 calc R . . H59C H 0.1618 0.1834 0.3587 0.307 Uiso 1 1 calc R . . C60 C 0.0839(10) 0.2530(7) 0.3504(5) 0.160(6) Uani 1 1 d . . . H60A H 0.0373 0.2309 0.3269 0.192 Uiso 1 1 calc R . . H60B H 0.0798 0.3008 0.3401 0.192 Uiso 1 1 calc R . . C61 C 0.0296(7) 0.2758(7) 0.4290(7) 0.151(5) Uani 1 1 d . . . H61A H -0.0167 0.2503 0.4106 0.181 Uiso 1 1 calc R . . H61B H 0.0217 0.3219 0.4140 0.181 Uiso 1 1 calc R . . C62 C 0.0454(9) 0.2764(8) 0.4935(7) 0.182(6) Uani 1 1 d . . . H62A H 0.0649 0.2329 0.5095 0.273 Uiso 1 1 calc R . . H62B H -0.0008 0.2858 0.5025 0.273 Uiso 1 1 calc R . . H62C H 0.0825 0.3108 0.5108 0.273 Uiso 1 1 calc R . . C63 C 0.3563(12) 0.8179(9) 0.0216(12) 0.326(15) Uani 1 1 d . . . H63A H 0.3789 0.8152 0.0638 0.489 Uiso 1 1 calc R . . H63B H 0.3050 0.8343 0.0123 0.489 Uiso 1 1 calc R . . H63C H 0.3855 0.8485 0.0057 0.489 Uiso 1 1 calc R . . C64 C 0.0103(15) 0.0701(17) 0.2114(9) 0.46(3) Uani 1 1 d D . . H64A H -0.0435 0.0621 0.1958 0.686 Uiso 1 1 calc R . . H64B H 0.0356 0.0477 0.1869 0.686 Uiso 1 1 calc R . . H64C H 0.0201 0.1180 0.2118 0.686 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 Fe1 0.0370(6) 0.0420(5) 0.0413(5) 0.0011(4) 0.0075(4) 0.0016(4) B1 0.169(11) 0.187(11) 0.190(11) 0.001(9) 0.035(9) 0.012(9) F1 0.188(9) 0.267(11) 0.319(13) 0.140(10) 0.040(8) 0.118(8) F2 0.130(8) 0.385(17) 0.437(19) 0.174(15) -0.005(10) -0.002(9) F3 0.229(13) 0.407(18) 0.209(10) 0.003(10) 0.031(9) 0.047(11) F4 0.183(9) 0.311(13) 0.309(13) 0.075(10) 0.050(8) 0.139(9) B2 0.172(11) 0.183(11) 0.165(10) 0.004(9) 0.040(9) -0.008(9) F5 0.161(7) 0.333(12) 0.170(7) 0.112(7) 0.028(5) -0.079(7) F6 0.149(8) 0.390(14) 0.188(8) 0.094(8) 0.015(6) -0.078(8) F7 0.259(14) 0.52(2) 0.272(12) 0.163(14) 0.187(11) 0.122(14) F8 0.270(15) 0.270(14) 0.378(18) 0.086(13) -0.030(13) -0.023(12) N1 0.038(3) 0.045(3) 0.051(3) 0.004(2) 0.012(2) 0.002(3) N2 0.043(4) 0.047(3) 0.040(3) 0.003(2) 0.008(2) 0.002(3) N3 0.047(4) 0.052(4) 0.111(5) 0.010(3) 0.006(3) -0.003(3) N4 0.063(4) 0.038(3) 0.094(4) 0.005(3) -0.003(3) 0.002(3) N5 0.042(3) 0.039(3) 0.044(3) -0.002(2) 0.008(3) 0.002(2) N6 0.042(3) 0.041(3) 0.038(3) 0.001(2) 0.008(3) 0.003(2) N7 0.072(4) 0.123(5) 0.037(4) -0.005(3) 0.003(3) -0.036(4) N8 0.045(4) 0.081(4) 0.047(3) -0.006(3) 0.004(3) -0.018(3) N9 0.037(3) 0.044(3) 0.046(3) 0.003(2) 0.009(2) 0.001(2) N10 0.038(3) 0.044(3) 0.044(3) 0.001(2) 0.012(2) 0.001(2) N11 0.090(5) 0.040(4) 0.075(4) -0.007(3) 0.031(3) 0.007(3) N12 0.085(5) 0.071(4) 0.042(3) -0.008(3) 0.019(3) 0.014(3) O1 0.054(3) 0.061(3) 0.118(4) -0.005(3) -0.001(3) -0.001(3) O2 0.062(4) 0.059(4) 0.206(7) -0.007(4) -0.007(4) -0.012(3) O3 0.107(6) 0.062(4) 0.209(7) 0.026(4) -0.017(5) 0.004(4) O4 0.103(5) 0.043(3) 0.176(6) 0.009(3) -0.010(4) -0.007(3) O5 0.108(5) 0.163(6) 0.053(3) 0.014(3) -0.004(3) -0.045(4) O6 0.100(5) 0.188(6) 0.050(3) -0.016(3) -0.005(3) -0.062(5) O7 0.053(3) 0.088(3) 0.059(3) -0.011(2) 0.016(3) -0.021(3) O8 0.063(3) 0.106(4) 0.054(3) -0.014(3) 0.003(2) -0.024(3) O9 0.300(11) 0.055(4) 0.103(5) -0.003(3) 0.070(6) -0.007(5) O10 0.211(8) 0.062(4) 0.092(4) -0.022(3) 0.044(4) 0.016(4) O11 0.220(8) 0.096(4) 0.061(4) -0.001(3) 0.024(4) 0.030(5) O12 0.172(6) 0.084(4) 0.062(3) -0.020(3) 0.045(4) 0.004(4) O13 0.216(7) 0.270(7) 0.218(6) 0.009(6) 0.088(6) -0.024(6) O14 0.089(5) 0.102(4) 0.128(6) -0.009(4) 0.008(4) -0.002(4) O15 0.110(6) 0.110(6) 0.227(10) 0.051(5) 0.019(6) 0.023(4) O16 0.131(7) 0.321(12) 0.101(5) -0.035(7) 0.033(5) 0.069(8) C1 0.040(4) 0.051(4) 0.060(4) 0.007(3) 0.012(3) 0.006(3) C2 0.044(5) 0.057(4) 0.065(4) 0.003(3) 0.011(3) 0.003(4) C3 0.035(4) 0.070(5) 0.083(5) -0.003(4) 0.009(3) -0.004(4) C4 0.044(5) 0.052(4) 0.078(5) 0.000(3) 0.008(4) 0.007(3) C5 0.039(4) 0.048(4) 0.053(4) -0.002(3) 0.010(3) 0.005(3) C6 0.044(4) 0.050(4) 0.046(4) 0.001(3) 0.001(3) 0.008(3) C7 0.047(4) 0.063(5) 0.074(5) 0.005(4) 0.003(4) 0.010(4) C8 0.069(6) 0.048(4) 0.084(5) 0.007(4) 0.002(4) 0.014(4) C9 0.052(5) 0.043(4) 0.061(4) 0.004(3) 0.002(3) 0.006(3) C10 0.046(4) 0.048(4) 0.048(4) 0.001(3) 0.008(3) -0.002(3) C11 0.069(6) 0.049(5) 0.111(6) 0.002(4) 0.011(5) -0.010(4) C12 0.119(9) 0.082(7) 0.142(10) 0.010(6) 0.019(7) 0.006(6) C13 0.184(14) 0.096(8) 0.207(13) -0.019(8) 0.049(10) -0.049(8) C14 0.245(18) 0.159(12) 0.107(9) 0.017(8) 0.019(10) -0.055(11) C15 0.083(7) 0.057(6) 0.132(8) 0.009(5) -0.006(6) 0.003(5) C16 0.137(12) 0.065(7) 0.294(17) 0.007(8) 0.042(10) -0.007(7) C17 0.212(16) 0.112(11) 0.36(2) -0.010(11) 0.076(14) -0.015(10) C18 0.165(15) 0.107(10) 0.38(3) 0.054(12) -0.002(15) -0.051(10) C19 0.042(4) 0.055(4) 0.052(4) 0.000(3) 0.004(3) -0.006(3) C20 0.054(5) 0.062(4) 0.041(4) -0.001(3) 0.006(3) -0.008(3) C21 0.069(5) 0.074(5) 0.048(4) -0.002(3) 0.016(4) -0.015(4) C22 0.056(4) 0.064(4) 0.050(4) -0.001(3) 0.015(3) -0.018(3) C23 0.050(4) 0.041(3) 0.042(4) 0.002(3) 0.011(3) -0.001(3) C24 0.041(4) 0.043(3) 0.043(4) 0.001(3) 0.007(3) -0.003(3) C25 0.056(5) 0.058(4) 0.049(4) -0.002(3) 0.014(3) -0.008(3) C26 0.040(4) 0.064(4) 0.057(4) -0.008(3) 0.010(3) -0.010(3) C27 0.044(4) 0.053(4) 0.047(4) -0.002(3) 0.006(3) -0.001(3) C28 0.046(4) 0.049(4) 0.042(4) 0.002(3) 0.007(3) 0.003(3) C29 0.068(6) 0.090(6) 0.056(5) -0.002(4) 0.004(5) -0.021(4) C30 0.152(10) 0.200(11) 0.070(7) -0.020(7) -0.031(6) -0.047(9) C31 0.175(13) 0.254(14) 0.128(10) 0.010(9) -0.045(10) -0.017(11) C32 0.301(17) 0.269(16) 0.136(11) -0.062(11) -0.037(11) 0.071(15) C33 0.060(5) 0.065(5) 0.053(5) -0.011(4) 0.006(4) 0.001(4) C34 0.056(5) 0.111(7) 0.077(5) -0.029(5) 0.000(4) -0.028(5) C35 0.140(10) 0.176(10) 0.066(6) -0.008(6) -0.029(6) -0.042(8) C36 0.112(8) 0.104(8) 0.103(7) -0.032(5) -0.004(6) -0.026(6) C37 0.042(4) 0.045(4) 0.050(4) -0.003(3) 0.013(3) -0.002(3) C38 0.050(4) 0.046(4) 0.064(4) -0.003(3) 0.016(3) 0.001(3) C39 0.106(7) 0.055(4) 0.067(5) 0.009(4) 0.020(4) 0.019(4) C40 0.124(7) 0.052(4) 0.054(4) 0.011(4) 0.022(4) 0.020(4) C41 0.064(5) 0.052(4) 0.044(4) 0.004(3) 0.014(3) 0.005(3) C42 0.064(5) 0.050(4) 0.051(4) 0.002(3) 0.017(3) 0.005(3) C43 0.134(8) 0.059(5) 0.057(5) 0.011(4) 0.037(5) 0.020(4) C44 0.126(8) 0.069(5) 0.049(4) 0.008(4) 0.036(4) 0.015(5) C45 0.058(5) 0.055(4) 0.047(4) -0.001(3) 0.016(3) -0.002(3) C46 0.046(4) 0.047(4) 0.047(4) 0.003(3) 0.009(3) 0.004(3) C47 0.149(9) 0.058(6) 0.077(6) -0.010(5) 0.032(6) 0.004(5) C48 0.294(19) 0.056(6) 0.101(8) -0.016(5) 0.054(10) 0.027(8) C49 0.186(15) 0.151(12) 0.249(16) -0.130(12) 0.015(12) 0.020(10) C50 0.23(2) 0.158(13) 0.258(18) -0.104(12) 0.113(15) -0.072(12) C51 0.121(8) 0.073(6) 0.067(6) -0.001(5) 0.036(5) -0.002(5) C52 0.291(15) 0.139(9) 0.080(7) -0.044(6) 0.051(9) 0.014(10) C53 0.35(2) 0.239(15) 0.135(10) -0.086(10) 0.021(13) -0.046(15) C54 0.262(10) 0.203(9) 0.173(8) -0.055(7) 0.073(8) 0.032(8) C55 0.261(11) 0.271(11) 0.273(11) 0.007(9) 0.081(9) -0.006(9) C56 0.241(9) 0.266(9) 0.243(8) 0.010(7) 0.078(7) -0.018(8) C57 0.212(8) 0.274(9) 0.226(8) 0.010(7) 0.083(7) -0.029(7) C58 0.243(10) 0.280(11) 0.218(10) 0.013(8) 0.106(8) 0.010(9) C59 0.196(18) 0.27(2) 0.156(13) 0.001(12) 0.068(12) 0.080(15) C60 0.213(17) 0.153(11) 0.075(8) 0.017(7) -0.012(8) -0.022(10) C61 0.100(10) 0.158(11) 0.182(13) -0.020(10) 0.024(9) 0.006(8) C62 0.161(14) 0.208(15) 0.189(14) -0.040(12) 0.074(11) -0.043(11) C63 0.22(2) 0.154(16) 0.66(5) 0.12(2) 0.23(3) 0.068(14) C64 0.28(3) 0.77(7) 0.36(4) -0.12(4) 0.15(3) 0.21(4) _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 Fe1 N1 1.964(5) . ? Fe1 N10 1.967(5) . ? Fe1 N6 1.970(5) . ? Fe1 N9 1.971(4) . ? Fe1 N2 1.974(5) . ? Fe1 N5 1.982(5) . ? B1 F1 1.313(13) . ? B1 F2 1.315(13) . ? B1 F4 1.321(13) . ? B1 F3 1.346(13) . ? B2 F7 1.283(13) . ? B2 F5 1.290(12) . ? B2 F6 1.308(12) . ? B2 F8 1.325(13) . ? N1 C1 1.336(7) . ? N1 C5 1.363(7) . ? N2 C10 1.345(7) . ? N2 C6 1.353(7) . ? N3 C11 1.347(9) . ? N3 C2 1.408(8) . ? N4 C15 1.340(9) . ? N4 C9 1.401(8) . ? N5 C19 1.345(7) . ? N5 C23 1.348(7) . ? N6 C28 1.341(7) . ? N6 C24 1.363(7) . ? N7 C29 1.332(9) . ? N7 C20 1.391(8) . ? N8 C33 1.359(9) . ? N8 C27 1.395(7) . ? N9 C37 1.350(7) . ? N9 C41 1.354(7) . ? N10 C46 1.336(7) . ? N10 C42 1.348(7) . ? N11 C47 1.324(9) . ? N11 C38 1.399(8) . ? N12 C51 1.340(9) . ? N12 C45 1.406(8) . ? O1 C11 1.207(9) . ? O2 C11 1.326(9) . ? O2 C12 1.490(11) . ? O3 C15 1.214(9) . ? O4 C15 1.310(10) . ? O4 C16 1.487(12) . ? O5 C29 1.195(9) . ? O6 C29 1.310(9) . ? O6 C30 1.469(11) . ? O7 C33 1.198(8) . ? O8 C33 1.349(8) . ? O8 C34 1.478(8) . ? O9 C47 1.201(9) . ? O10 C47 1.323(9) . ? O10 C48 1.482(10) . ? O11 C51 1.210(9) . ? O12 C51 1.316(9) . ? O12 C52 1.475(11) . ? O13 C57 1.454(15) . ? O13 C56 1.47(2) . ? O14 C61 1.440(13) . ? O14 C60 1.464(12) . ? O15 C63 1.57(2) . ? O16 C64 1.575(18) . ? C1 C2 1.384(9) . ? C2 C3 1.384(9) . ? C3 C4 1.373(9) . ? C4 C5 1.371(9) . ? C5 C6 1.457(8) . ? C6 C7 1.376(8) . ? C7 C8 1.384(9) . ? C8 C9 1.373(9) . ? C9 C10 1.381(8) . ? C12 C14 1.415(14) . ? C12 C13 1.487(14) . ? C16 C17 1.44(2) . ? C16 C18 1.466(18) . ? C19 C20 1.394(9) . ? C20 C21 1.384(9) . ? C21 C22 1.374(8) . ? C22 C23 1.400(8) . ? C23 C24 1.475(8) . ? C24 C25 1.366(8) . ? C25 C26 1.380(8) . ? C26 C27 1.388(8) . ? C27 C28 1.380(8) . ? C30 C31 1.458(19) . ? C30 C32 1.463(19) . ? C34 C36 1.486(11) . ? C34 C35 1.510(11) . ? C37 C38 1.376(8) . ? C38 C39 1.387(9) . ? C39 C40 1.363(9) . ? C40 C41 1.373(9) . ? C41 C42 1.468(8) . ? C42 C43 1.388(9) . ? C43 C44 1.358(9) . ? C44 C45 1.360(9) . ? C45 C46 1.379(8) . ? C48 C49 1.426(19) . ? C48 C50 1.550(19) . ? C52 C54 1.476(18) . ? C52 C53 1.48(2) . ? C55 C56 1.544(16) . ? C57 C58 1.551(16) . ? C59 C60 1.412(18) . ? C61 C62 1.469(15) . ? 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 Fe1 N10 91.52(19) . . ? N1 Fe1 N6 172.95(19) . . ? N10 Fe1 N6 94.20(19) . . ? N1 Fe1 N9 94.66(19) . . ? N10 Fe1 N9 81.49(19) . . ? N6 Fe1 N9 90.27(18) . . ? N1 Fe1 N2 81.3(2) . . ? N10 Fe1 N2 94.50(19) . . ? N6 Fe1 N2 94.11(19) . . ? N9 Fe1 N2 174.3(2) . . ? N1 Fe1 N5 93.0(2) . . ? N10 Fe1 N5 175.0(2) . . ? N6 Fe1 N5 81.4(2) . . ? N9 Fe1 N5 96.16(18) . . ? N2 Fe1 N5 88.14(18) . . ? F1 B1 F2 108.7(11) . . ? F1 B1 F4 109.2(11) . . ? F2 B1 F4 113.1(12) . . ? F1 B1 F3 111.8(12) . . ? F2 B1 F3 108.4(12) . . ? F4 B1 F3 105.7(11) . . ? F7 B2 F5 112.3(12) . . ? F7 B2 F6 110.2(12) . . ? F5 B2 F6 111.7(11) . . ? F7 B2 F8 100.7(11) . . ? F5 B2 F8 112.1(12) . . ? F6 B2 F8 109.2(12) . . ? C1 N1 C5 118.0(5) . . ? C1 N1 Fe1 126.6(4) . . ? C5 N1 Fe1 115.2(4) . . ? C10 N2 C6 118.9(5) . . ? C10 N2 Fe1 126.5(4) . . ? C6 N2 Fe1 114.7(4) . . ? C11 N3 C2 126.7(6) . . ? C15 N4 C9 128.9(6) . . ? C19 N5 C23 117.7(5) . . ? C19 N5 Fe1 127.5(4) . . ? C23 N5 Fe1 114.7(4) . . ? C28 N6 C24 117.3(5) . . ? C28 N6 Fe1 127.3(4) . . ? C24 N6 Fe1 115.4(4) . . ? C29 N7 C20 127.8(7) . . ? C33 N8 C27 126.7(6) . . ? C37 N9 C41 118.7(5) . . ? C37 N9 Fe1 126.1(4) . . ? C41 N9 Fe1 115.3(4) . . ? C46 N10 C42 118.5(5) . . ? C46 N10 Fe1 126.4(4) . . ? C42 N10 Fe1 115.0(4) . . ? C47 N11 C38 127.1(6) . . ? C51 N12 C45 127.8(6) . . ? C11 O2 C12 118.3(7) . . ? C15 O4 C16 119.7(8) . . ? C29 O6 C30 118.5(8) . . ? C33 O8 C34 117.4(6) . . ? C47 O10 C48 118.4(8) . . ? C51 O12 C52 119.2(8) . . ? C57 O13 C56 113.8(15) . . ? C61 O14 C60 112.9(10) . . ? N1 C1 C2 123.6(6) . . ? C1 C2 C3 118.1(6) . . ? C1 C2 N3 116.4(6) . . ? C3 C2 N3 125.5(6) . . ? C4 C3 C2 118.4(6) . . ? C5 C4 C3 121.2(6) . . ? N1 C5 C4 120.6(5) . . ? N1 C5 C6 113.5(5) . . ? C4 C5 C6 125.9(6) . . ? N2 C6 C7 120.2(6) . . ? N2 C6 C5 114.6(5) . . ? C7 C6 C5 125.1(6) . . ? C6 C7 C8 120.6(7) . . ? C9 C8 C7 119.0(6) . . ? C8 C9 C10 118.1(6) . . ? C8 C9 N4 125.0(6) . . ? C10 C9 N4 116.9(6) . . ? N2 C10 C9 123.1(6) . . ? O1 C11 O2 125.0(7) . . ? O1 C11 N3 126.3(7) . . ? O2 C11 N3 108.7(7) . . ? C14 C12 C13 114.5(10) . . ? C14 C12 O2 101.6(10) . . ? C13 C12 O2 105.9(8) . . ? O3 C15 O4 124.9(8) . . ? O3 C15 N4 124.7(8) . . ? O4 C15 N4 110.4(8) . . ? C17 C16 C18 110.8(16) . . ? C17 C16 O4 104.4(14) . . ? C18 C16 O4 107.3(10) . . ? N5 C19 C20 123.8(6) . . ? C21 C20 N7 125.7(6) . . ? C21 C20 C19 117.8(6) . . ? N7 C20 C19 116.5(6) . . ? C22 C21 C20 119.3(6) . . ? C21 C22 C23 119.7(6) . . ? N5 C23 C22 121.6(5) . . ? N5 C23 C24 114.7(5) . . ? C22 C23 C24 123.6(6) . . ? N6 C24 C25 121.1(5) . . ? N6 C24 C23 113.3(5) . . ? C25 C24 C23 125.6(6) . . ? C24 C25 C26 121.4(6) . . ? C25 C26 C27 117.8(6) . . ? C28 C27 C26 118.3(5) . . ? C28 C27 N8 116.7(6) . . ? C26 C27 N8 125.0(6) . . ? N6 C28 C27 124.0(6) . . ? O5 C29 O6 124.1(7) . . ? O5 C29 N7 125.7(7) . . ? O6 C29 N7 110.2(8) . . ? C31 C30 C32 108.1(12) . . ? C31 C30 O6 107.5(12) . . ? C32 C30 O6 103.3(11) . . ? O7 C33 O8 126.0(7) . . ? O7 C33 N8 126.4(6) . . ? O8 C33 N8 107.5(7) . . ? O8 C34 C36 109.7(7) . . ? O8 C34 C35 104.2(7) . . ? C36 C34 C35 114.5(8) . . ? N9 C37 C38 122.4(5) . . ? C37 C38 C39 118.5(6) . . ? C37 C38 N11 117.3(6) . . ? C39 C38 N11 124.2(6) . . ? C40 C39 C38 118.7(6) . . ? C39 C40 C41 121.1(6) . . ? N9 C41 C40 120.5(6) . . ? N9 C41 C42 113.5(5) . . ? C40 C41 C42 125.9(6) . . ? N10 C42 C43 120.2(6) . . ? N10 C42 C41 114.6(5) . . ? C43 C42 C41 125.2(6) . . ? C44 C43 C42 120.3(6) . . ? C43 C44 C45 119.8(6) . . ? C44 C45 C46 118.0(6) . . ? C44 C45 N12 125.1(6) . . ? C46 C45 N12 116.9(5) . . ? N10 C46 C45 123.2(5) . . ? O9 C47 O10 123.4(8) . . ? O9 C47 N11 126.3(8) . . ? O10 C47 N11 110.4(8) . . ? C49 C48 O10 106.9(12) . . ? C49 C48 C50 112.0(11) . . ? O10 C48 C50 107.4(11) . . ? O11 C51 O12 124.9(8) . . ? O11 C51 N12 125.3(8) . . ? O12 C51 N12 109.7(7) . . ? O12 C52 C54 108.4(11) . . ? O12 C52 C53 104.3(13) . . ? C54 C52 C53 99.2(14) . . ? O13 C56 C55 115.8(18) . . ? O13 C57 C58 102.2(15) . . ? C59 C60 O14 111.7(12) . . ? O14 C61 C62 110.9(11) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 21.08 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.659 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.067 ############# data_L1ZnCl _database_code_depnum_ccdc_archive 'CCDC 800534' #TrackingRef '- bipy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H54 Cl4 N8 O11 S3 Zn2' _chemical_formula_weight 1167.61 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.422(4) _cell_length_b 14.320(4) _cell_length_c 14.365(4) _cell_angle_alpha 73.397(4) _cell_angle_beta 77.928(4) _cell_angle_gamma 80.200(4) _cell_volume 2569.4(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1204 _exptl_absorpt_coefficient_mu 1.324 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7776 _exptl_absorpt_correction_T_max 0.8261 _exptl_absorpt_process_details SADABS _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 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17277 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0646 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8854 _reflns_number_gt 5908 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 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^)+(0.0544P)^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 8854 _refine_ls_number_parameters 623 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0776 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1166 _refine_ls_wR_factor_gt 0.1006 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 Zn1 Zn 0.70890(3) 0.32764(3) 0.13369(3) 0.04383(14) Uani 1 1 d . . . Zn2 Zn 0.25280(3) 0.22121(3) 0.36637(3) 0.03864(13) Uani 1 1 d . . . Cl1 Cl 0.75508(10) 0.33129(11) 0.27005(9) 0.0805(4) Uani 1 1 d . . . Cl2 Cl 0.82598(8) 0.37711(9) 0.00165(9) 0.0666(3) Uani 1 1 d . . . Cl3 Cl 0.19569(8) 0.11803(8) 0.51489(8) 0.0565(3) Uani 1 1 d . . . Cl4 Cl 0.23100(8) 0.16439(8) 0.23881(8) 0.0584(3) Uani 1 1 d . . . N1 N 0.5585(2) 0.3854(2) 0.1256(2) 0.0374(7) Uani 1 1 d . . . N2 N 0.6525(2) 0.2046(2) 0.1266(2) 0.0424(8) Uani 1 1 d . . . N3 N 0.3665(2) 0.6014(2) 0.1284(2) 0.0459(8) Uani 1 1 d . . . H3A H 0.3048 0.6159 0.1163 0.055 Uiso 1 1 calc R . . N4 N 0.7230(2) -0.0486(2) 0.1166(2) 0.0468(8) Uani 1 1 d . . . H4A H 0.7781 -0.0584 0.1413 0.056 Uiso 1 1 calc R . . N5 N 0.3199(2) 0.34365(19) 0.3778(2) 0.0339(7) Uani 1 1 d . . . N6 N 0.4147(2) 0.16665(19) 0.3648(2) 0.0335(7) Uani 1 1 d . . . N7 N 0.2600(2) 0.5994(2) 0.3831(2) 0.0420(8) Uani 1 1 d . . . H7A H 0.2072 0.6119 0.3546 0.050 Uiso 1 1 calc R . . N8 N 0.5994(2) -0.0570(2) 0.3775(2) 0.0410(8) Uani 1 1 d . . . H8A H 0.6577 -0.0750 0.3971 0.049 Uiso 1 1 calc R . . O1 O 0.4933(2) 0.6634(2) 0.1660(3) 0.0666(9) Uani 1 1 d . . . O2 O 0.3411(2) 0.75292(18) 0.1432(2) 0.0490(7) Uani 1 1 d . . . O3 O 0.6294(2) -0.1184(2) 0.0440(2) 0.0617(8) Uani 1 1 d . . . O4 O 0.7769(2) -0.19722(18) 0.0930(2) 0.0513(7) Uani 1 1 d . . . O5 O 0.3500(2) 0.66491(19) 0.4623(2) 0.0578(8) Uani 1 1 d . . . O6 O 0.2051(2) 0.74556(17) 0.4091(2) 0.0490(7) Uani 1 1 d . . . O7 O 0.4827(2) -0.11087(19) 0.3167(2) 0.0597(8) Uani 1 1 d . . . O8 O 0.6277(2) -0.20636(17) 0.35685(19) 0.0473(7) Uani 1 1 d . . . C1 C 0.5003(3) 0.3201(3) 0.1189(3) 0.0361(8) Uani 1 1 d . . . C2 C 0.3966(3) 0.3475(3) 0.1157(3) 0.0457(10) Uani 1 1 d . . . H2 H 0.3564 0.3029 0.1106 0.055 Uiso 1 1 calc R . . C3 C 0.3535(3) 0.4402(3) 0.1201(3) 0.0449(10) Uani 1 1 d . . . H3 H 0.2838 0.4582 0.1187 0.054 Uiso 1 1 calc R . . C4 C 0.4132(3) 0.5072(3) 0.1266(3) 0.0384(9) Uani 1 1 d . . . C5 C 0.5164(3) 0.4763(3) 0.1297(3) 0.0391(9) Uani 1 1 d . . . H5 H 0.5577 0.5200 0.1347 0.047 Uiso 1 1 calc R . . C6 C 0.5525(3) 0.2214(3) 0.1169(2) 0.0363(8) Uani 1 1 d . . . C7 C 0.5047(3) 0.1478(3) 0.1055(3) 0.0439(10) Uani 1 1 d . . . H7 H 0.4361 0.1598 0.0981 0.053 Uiso 1 1 calc R . . C8 C 0.5579(3) 0.0575(3) 0.1052(3) 0.0466(10) Uani 1 1 d . . . H8 H 0.5255 0.0079 0.0984 0.056 Uiso 1 1 calc R . . C9 C 0.6610(3) 0.0404(3) 0.1150(3) 0.0387(9) Uani 1 1 d . . . C10 C 0.7045(3) 0.1171(3) 0.1256(3) 0.0460(10) Uani 1 1 d . . . H10 H 0.7732 0.1068 0.1324 0.055 Uiso 1 1 calc R . . C11 C 0.4081(3) 0.6732(3) 0.1474(3) 0.0420(9) Uani 1 1 d . . . C12 C 0.3746(3) 0.8329(3) 0.1684(3) 0.0563(11) Uani 1 1 d . . . H12A H 0.4358 0.8544 0.1231 0.068 Uiso 1 1 calc R . . H12B H 0.3903 0.8114 0.2348 0.068 Uiso 1 1 calc R . . C13 C 0.2892(3) 0.9148(3) 0.1615(4) 0.0659(13) Uani 1 1 d . . . H13A H 0.2721 0.9332 0.0965 0.099 Uiso 1 1 calc R . . H13B H 0.3102 0.9700 0.1744 0.099 Uiso 1 1 calc R . . H13C H 0.2303 0.8937 0.2092 0.099 Uiso 1 1 calc R . . C14 C 0.7021(3) -0.1213(3) 0.0814(3) 0.0449(10) Uani 1 1 d . . . C15 C 0.7629(4) -0.2774(3) 0.0537(4) 0.0606(12) Uani 1 1 d . . . H15A H 0.7609 -0.2533 -0.0163 0.073 Uiso 1 1 calc R . . H15B H 0.6986 -0.3031 0.0865 0.073 Uiso 1 1 calc R . . C16 C 0.8496(4) -0.3555(3) 0.0708(4) 0.0822(16) Uani 1 1 d . . . H16A H 0.9128 -0.3296 0.0376 0.123 Uiso 1 1 calc R . . H16B H 0.8414 -0.4085 0.0456 0.123 Uiso 1 1 calc R . . H16C H 0.8508 -0.3791 0.1402 0.123 Uiso 1 1 calc R . . C17 C 0.4200(3) 0.3246(2) 0.3885(2) 0.0319(8) Uani 1 1 d . . . C18 C 0.4714(3) 0.3973(2) 0.3972(3) 0.0400(9) Uani 1 1 d . . . H18 H 0.5401 0.3833 0.4040 0.048 Uiso 1 1 calc R . . C19 C 0.4216(3) 0.4897(3) 0.3957(3) 0.0414(9) Uani 1 1 d . . . H19 H 0.4560 0.5386 0.4010 0.050 Uiso 1 1 calc R . . C20 C 0.3189(3) 0.5085(2) 0.3860(3) 0.0351(8) Uani 1 1 d . . . C21 C 0.2715(3) 0.4335(2) 0.3763(3) 0.0359(8) Uani 1 1 d . . . H21 H 0.2030 0.4465 0.3684 0.043 Uiso 1 1 calc R . . C22 C 0.4690(3) 0.2244(2) 0.3886(2) 0.0313(8) Uani 1 1 d . . . C23 C 0.5667(3) 0.1896(3) 0.4116(3) 0.0398(9) Uani 1 1 d . . . H23 H 0.6033 0.2295 0.4295 0.048 Uiso 1 1 calc R . . C24 C 0.6083(3) 0.0967(3) 0.4078(3) 0.0407(9) Uani 1 1 d . . . H24 H 0.6731 0.0730 0.4239 0.049 Uiso 1 1 calc R . . C25 C 0.5541(3) 0.0372(2) 0.3799(2) 0.0328(8) Uani 1 1 d . . . C26 C 0.4546(3) 0.0763(2) 0.3602(3) 0.0361(8) Uani 1 1 d . . . H26 H 0.4156 0.0376 0.3436 0.043 Uiso 1 1 calc R . . C27 C 0.2794(3) 0.6700(3) 0.4217(3) 0.0403(9) Uani 1 1 d . . . C28 C 0.2143(3) 0.8257(3) 0.4508(3) 0.0561(11) Uani 1 1 d . . . H28A H 0.2184 0.8006 0.5203 0.067 Uiso 1 1 calc R . . H28B H 0.2757 0.8564 0.4172 0.067 Uiso 1 1 calc R . . C29 C 0.1225(4) 0.8974(3) 0.4372(4) 0.0755(15) Uani 1 1 d . . . H29A H 0.1193 0.9219 0.3682 0.113 Uiso 1 1 calc R . . H29B H 0.1260 0.9510 0.4638 0.113 Uiso 1 1 calc R . . H29C H 0.0623 0.8663 0.4708 0.113 Uiso 1 1 calc R . . C30 C 0.5618(3) -0.1234(3) 0.3480(3) 0.0398(9) Uani 1 1 d . . . C31 C 0.5970(3) -0.2843(3) 0.3269(3) 0.0521(11) Uani 1 1 d . . . H31A H 0.5865 -0.2616 0.2588 0.063 Uiso 1 1 calc R . . H31B H 0.5334 -0.3051 0.3680 0.063 Uiso 1 1 calc R . . C32 C 0.6811(4) -0.3676(3) 0.3382(4) 0.0662(13) Uani 1 1 d . . . H32A H 0.7427 -0.3471 0.2949 0.099 Uiso 1 1 calc R . . H32B H 0.6618 -0.4218 0.3220 0.099 Uiso 1 1 calc R . . H32C H 0.6928 -0.3875 0.4051 0.099 Uiso 1 1 calc R . . S1 S 0.02203(9) 0.32044(8) 0.32491(10) 0.0593(3) Uani 1 1 d . . . O9 O 0.1210(2) 0.3248(2) 0.3568(3) 0.0777(10) Uani 1 1 d . . . C33 C 0.0296(4) 0.3922(4) 0.2021(4) 0.0908(17) Uani 1 1 d . . . H33A H 0.0560 0.4524 0.1958 0.136 Uiso 1 1 calc R . . H33B H -0.0375 0.4067 0.1844 0.136 Uiso 1 1 calc R . . H33C H 0.0745 0.3567 0.1591 0.136 Uiso 1 1 calc R . . C34 C -0.0656(4) 0.4029(4) 0.3819(4) 0.0796(15) Uani 1 1 d . . . H34A H -0.0769 0.3757 0.4520 0.119 Uiso 1 1 calc R . . H34B H -0.1295 0.4136 0.3582 0.119 Uiso 1 1 calc R . . H34C H -0.0380 0.4642 0.3664 0.119 Uiso 1 1 calc R . . S2A S 0.0027(3) 0.66568(18) 0.2613(3) 0.0760(10) Uani 0.70 1 d P A 1 O10A O 0.0785(9) 0.5976(11) 0.3152(9) 0.107(5) Uani 0.70 1 d P A 1 C35 C 0.0572(5) 0.7667(5) 0.1728(6) 0.124(3) Uani 1 1 d . A 1 H35A H 0.1057 0.7887 0.2000 0.186 Uiso 1 1 calc R A 1 H35B H 0.0039 0.8192 0.1559 0.186 Uiso 1 1 calc R A 1 H35C H 0.0915 0.7466 0.1147 0.186 Uiso 1 1 calc R A 1 C36 C -0.0587(7) 0.7283(6) 0.3495(6) 0.146(3) Uani 1 1 d . A 1 H36A H -0.0767 0.6819 0.4115 0.219 Uiso 1 1 calc R A 1 H36B H -0.1197 0.7673 0.3289 0.219 Uiso 1 1 calc R A 1 H36C H -0.0135 0.7702 0.3564 0.219 Uiso 1 1 calc R A 1 S2B S 0.0132(12) 0.6862(13) 0.2689(15) 0.306(11) Uani 0.30 1 d P B 2 O10B O 0.1154(19) 0.608(2) 0.2714(17) 0.070(6) Uani 0.30 1 d P B 2 S3 S 0.99507(9) 0.01244(9) 0.19728(11) 0.0695(4) Uani 1 1 d . . . O11 O 0.9082(3) -0.0158(2) 0.1653(3) 0.0916(12) Uani 1 1 d . . . C37 C 1.0419(5) 0.1110(5) 0.1010(4) 0.131(3) Uani 1 1 d . . . H37A H 1.0619 0.0909 0.0408 0.196 Uiso 1 1 calc R . . H37B H 1.1002 0.1300 0.1169 0.196 Uiso 1 1 calc R . . H37C H 0.9891 0.1656 0.0929 0.196 Uiso 1 1 calc R . . C38 C 0.9437(4) 0.0798(4) 0.2846(4) 0.0943(18) Uani 1 1 d . . . H38A H 0.9001 0.1365 0.2559 0.141 Uiso 1 1 calc R . . H38B H 0.9985 0.1002 0.3048 0.141 Uiso 1 1 calc R . . H38C H 0.9045 0.0395 0.3408 0.141 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 Zn1 0.0405(3) 0.0409(3) 0.0578(3) -0.0168(2) -0.0190(2) -0.0056(2) Zn2 0.0386(3) 0.0317(2) 0.0514(3) -0.01170(19) -0.0196(2) -0.00348(19) Cl1 0.0714(8) 0.1251(11) 0.0607(8) -0.0220(7) -0.0239(6) -0.0416(8) Cl2 0.0487(6) 0.0825(8) 0.0645(8) -0.0144(6) -0.0076(5) -0.0072(6) Cl3 0.0474(6) 0.0596(6) 0.0593(7) -0.0052(5) -0.0120(5) -0.0120(5) Cl4 0.0549(7) 0.0740(7) 0.0600(7) -0.0280(6) -0.0180(5) -0.0160(6) N1 0.0368(17) 0.0379(17) 0.0429(19) -0.0133(14) -0.0148(14) -0.0045(14) N2 0.0402(19) 0.0394(17) 0.054(2) -0.0144(15) -0.0204(15) -0.0027(15) N3 0.0418(19) 0.0360(17) 0.068(2) -0.0196(16) -0.0230(17) 0.0007(15) N4 0.049(2) 0.0393(18) 0.062(2) -0.0210(16) -0.0249(16) 0.0018(16) N5 0.0353(17) 0.0297(15) 0.0407(18) -0.0101(13) -0.0144(13) -0.0036(13) N6 0.0367(17) 0.0277(15) 0.0405(18) -0.0096(13) -0.0160(13) -0.0032(13) N7 0.0438(19) 0.0314(16) 0.058(2) -0.0174(15) -0.0241(16) 0.0036(14) N8 0.0424(18) 0.0340(16) 0.053(2) -0.0172(15) -0.0206(15) 0.0025(14) O1 0.0526(19) 0.0513(17) 0.116(3) -0.0428(18) -0.0363(18) 0.0033(15) O2 0.0501(16) 0.0363(14) 0.0675(19) -0.0193(13) -0.0223(14) 0.0018(13) O3 0.060(2) 0.0560(18) 0.086(2) -0.0343(17) -0.0310(17) -0.0013(16) O4 0.0604(18) 0.0397(15) 0.0618(19) -0.0215(14) -0.0198(14) -0.0012(14) O5 0.0543(18) 0.0513(17) 0.084(2) -0.0353(16) -0.0348(16) 0.0075(14) O6 0.0530(17) 0.0347(14) 0.0699(19) -0.0258(13) -0.0269(14) 0.0076(13) O7 0.064(2) 0.0439(16) 0.088(2) -0.0307(16) -0.0428(17) 0.0063(15) O8 0.0525(17) 0.0348(14) 0.0621(18) -0.0199(13) -0.0218(14) 0.0020(13) C1 0.039(2) 0.0365(19) 0.035(2) -0.0076(16) -0.0116(16) -0.0079(17) C2 0.041(2) 0.039(2) 0.063(3) -0.0148(19) -0.0157(19) -0.0088(18) C3 0.038(2) 0.042(2) 0.059(3) -0.0139(19) -0.0158(19) -0.0048(18) C4 0.043(2) 0.037(2) 0.036(2) -0.0081(17) -0.0104(17) -0.0047(18) C5 0.042(2) 0.035(2) 0.045(2) -0.0143(17) -0.0114(17) -0.0080(18) C6 0.041(2) 0.037(2) 0.033(2) -0.0074(16) -0.0121(16) -0.0058(17) C7 0.036(2) 0.045(2) 0.059(3) -0.019(2) -0.0152(19) -0.0061(18) C8 0.044(2) 0.037(2) 0.065(3) -0.020(2) -0.008(2) -0.0123(19) C9 0.045(2) 0.036(2) 0.039(2) -0.0110(17) -0.0123(17) -0.0053(18) C10 0.044(2) 0.044(2) 0.059(3) -0.019(2) -0.022(2) 0.0000(19) C11 0.047(2) 0.039(2) 0.043(2) -0.0118(18) -0.0101(19) -0.0060(19) C12 0.058(3) 0.042(2) 0.077(3) -0.027(2) -0.013(2) -0.008(2) C13 0.072(3) 0.044(2) 0.083(4) -0.022(2) -0.013(3) -0.001(2) C14 0.049(3) 0.040(2) 0.049(3) -0.0166(19) -0.007(2) -0.008(2) C15 0.069(3) 0.046(2) 0.077(3) -0.030(2) -0.019(2) -0.003(2) C16 0.109(4) 0.062(3) 0.086(4) -0.039(3) -0.031(3) 0.015(3) C17 0.034(2) 0.0308(18) 0.032(2) -0.0069(15) -0.0088(15) -0.0034(16) C18 0.032(2) 0.036(2) 0.058(3) -0.0160(18) -0.0159(18) -0.0031(17) C19 0.039(2) 0.0327(19) 0.058(3) -0.0174(18) -0.0107(19) -0.0081(17) C20 0.039(2) 0.0315(19) 0.036(2) -0.0082(16) -0.0103(16) -0.0036(17) C21 0.033(2) 0.0340(19) 0.043(2) -0.0111(17) -0.0165(16) 0.0022(16) C22 0.0342(19) 0.0304(18) 0.0294(19) -0.0062(15) -0.0081(15) -0.0031(16) C23 0.034(2) 0.039(2) 0.053(2) -0.0161(18) -0.0139(18) -0.0065(17) C24 0.034(2) 0.038(2) 0.054(2) -0.0159(18) -0.0152(18) 0.0016(17) C25 0.038(2) 0.0288(18) 0.033(2) -0.0075(15) -0.0114(16) -0.0013(16) C26 0.038(2) 0.0330(19) 0.042(2) -0.0114(17) -0.0139(17) -0.0064(17) C27 0.042(2) 0.035(2) 0.045(2) -0.0135(18) -0.0087(19) -0.0008(18) C28 0.062(3) 0.040(2) 0.078(3) -0.031(2) -0.022(2) -0.001(2) C29 0.086(4) 0.057(3) 0.097(4) -0.042(3) -0.033(3) 0.015(3) C30 0.049(2) 0.0312(19) 0.042(2) -0.0125(17) -0.0121(19) -0.0013(18) C31 0.057(3) 0.037(2) 0.071(3) -0.024(2) -0.014(2) -0.007(2) C32 0.078(3) 0.043(2) 0.079(3) -0.028(2) -0.010(3) 0.006(2) S1 0.0507(7) 0.0449(6) 0.0914(9) -0.0137(6) -0.0357(6) -0.0080(5) O9 0.0583(19) 0.0483(17) 0.151(3) -0.0400(19) -0.063(2) 0.0088(15) C33 0.069(4) 0.116(5) 0.080(4) -0.016(3) -0.012(3) -0.006(3) C34 0.057(3) 0.094(4) 0.092(4) -0.031(3) -0.016(3) -0.007(3) S2A 0.0782(18) 0.0451(11) 0.139(3) -0.0472(15) -0.0768(18) 0.0115(12) O10A 0.079(8) 0.060(4) 0.196(14) -0.019(9) -0.082(7) 0.001(5) C35 0.143(7) 0.088(5) 0.139(7) -0.045(5) -0.023(5) 0.020(5) C36 0.184(8) 0.135(7) 0.136(7) -0.068(6) -0.038(6) 0.003(6) S2B 0.174(14) 0.308(19) 0.29(2) 0.075(16) -0.055(13) 0.137(13) O10B 0.082(17) 0.057(11) 0.092(14) -0.032(11) -0.062(11) 0.021(11) S3 0.0533(7) 0.0638(7) 0.1008(10) -0.0269(7) -0.0352(7) 0.0045(6) O11 0.067(2) 0.069(2) 0.163(4) -0.043(2) -0.063(2) 0.0024(18) C37 0.124(6) 0.180(7) 0.088(5) 0.000(5) -0.011(4) -0.085(6) C38 0.104(5) 0.087(4) 0.101(5) -0.038(4) -0.016(4) -0.015(4) _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 Zn1 N1 2.061(3) . ? Zn1 N2 2.068(3) . ? Zn1 Cl1 2.1913(14) . ? Zn1 Cl2 2.2212(13) . ? Zn2 O9 2.108(3) . ? Zn2 N5 2.163(3) . ? Zn2 N6 2.178(3) . ? Zn2 Cl3 2.2853(12) . ? Zn2 Cl4 2.2940(12) . ? N1 C5 1.340(4) . ? N1 C1 1.351(4) . ? N2 C10 1.329(4) . ? N2 C6 1.351(4) . ? N3 C11 1.364(5) . ? N3 C4 1.392(4) . ? N4 C14 1.370(5) . ? N4 C9 1.396(4) . ? N5 C21 1.336(4) . ? N5 C17 1.356(4) . ? N6 C26 1.327(4) . ? N6 C22 1.343(4) . ? N7 C27 1.367(4) . ? N7 C20 1.397(4) . ? N8 C30 1.351(4) . ? N8 C25 1.388(4) . ? O1 C11 1.204(4) . ? O2 C11 1.323(4) . ? O2 C12 1.459(4) . ? O3 C14 1.199(5) . ? O4 C14 1.346(5) . ? O4 C15 1.470(4) . ? O5 C27 1.196(4) . ? O6 C27 1.339(4) . ? O6 C28 1.472(4) . ? O7 C30 1.203(4) . ? O8 C30 1.346(4) . ? O8 C31 1.452(4) . ? C1 C2 1.387(5) . ? C1 C6 1.472(5) . ? C2 C3 1.368(5) . ? C3 C4 1.384(5) . ? C4 C5 1.387(5) . ? C6 C7 1.387(5) . ? C7 C8 1.367(5) . ? C8 C9 1.393(5) . ? C9 C10 1.385(5) . ? C12 C13 1.490(5) . ? C15 C16 1.478(6) . ? C17 C18 1.389(5) . ? C17 C22 1.473(4) . ? C18 C19 1.375(5) . ? C19 C20 1.387(5) . ? C20 C21 1.391(5) . ? C22 C23 1.393(5) . ? C23 C24 1.364(5) . ? C24 C25 1.395(5) . ? C25 C26 1.411(5) . ? C28 C29 1.471(6) . ? C31 C32 1.494(5) . ? S1 O9 1.509(3) . ? S1 C33 1.762(5) . ? S1 C34 1.768(5) . ? S2A O10A 1.465(15) . ? S2A C36 1.746(8) . ? S2A C35 1.779(8) . ? S2B O10B 1.61(3) . ? S3 O11 1.492(3) . ? S3 C38 1.756(5) . ? S3 C37 1.767(6) . ? 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 Zn1 N2 80.85(12) . . ? N1 Zn1 Cl1 112.75(9) . . ? N2 Zn1 Cl1 120.00(9) . . ? N1 Zn1 Cl2 117.29(9) . . ? N2 Zn1 Cl2 110.46(10) . . ? Cl1 Zn1 Cl2 112.33(5) . . ? O9 Zn2 N5 82.47(11) . . ? O9 Zn2 N6 157.78(11) . . ? N5 Zn2 N6 76.06(10) . . ? O9 Zn2 Cl3 98.15(11) . . ? N5 Zn2 Cl3 114.00(8) . . ? N6 Zn2 Cl3 95.75(8) . . ? O9 Zn2 Cl4 93.84(9) . . ? N5 Zn2 Cl4 135.12(8) . . ? N6 Zn2 Cl4 97.32(8) . . ? Cl3 Zn2 Cl4 110.81(5) . . ? C5 N1 C1 120.3(3) . . ? C5 N1 Zn1 126.5(2) . . ? C1 N1 Zn1 113.2(2) . . ? C10 N2 C6 119.7(3) . . ? C10 N2 Zn1 127.3(2) . . ? C6 N2 Zn1 113.0(2) . . ? C11 N3 C4 126.9(3) . . ? C14 N4 C9 124.5(3) . . ? C21 N5 C17 118.8(3) . . ? C21 N5 Zn2 125.9(2) . . ? C17 N5 Zn2 115.3(2) . . ? C26 N6 C22 120.3(3) . . ? C26 N6 Zn2 124.0(2) . . ? C22 N6 Zn2 114.4(2) . . ? C27 N7 C20 125.5(3) . . ? C30 N8 C25 127.1(3) . . ? C11 O2 C12 115.1(3) . . ? C14 O4 C15 113.9(3) . . ? C27 O6 C28 115.1(3) . . ? C30 O8 C31 115.3(3) . . ? N1 C1 C2 119.8(3) . . ? N1 C1 C6 116.6(3) . . ? C2 C1 C6 123.6(3) . . ? C3 C2 C1 119.9(4) . . ? C2 C3 C4 120.3(4) . . ? C3 C4 C5 117.6(3) . . ? C3 C4 N3 118.3(3) . . ? C5 C4 N3 124.2(3) . . ? N1 C5 C4 122.1(3) . . ? N2 C6 C7 120.1(3) . . ? N2 C6 C1 116.4(3) . . ? C7 C6 C1 123.5(3) . . ? C8 C7 C6 120.3(4) . . ? C7 C8 C9 119.5(3) . . ? C10 C9 C8 117.5(3) . . ? C10 C9 N4 117.7(3) . . ? C8 C9 N4 124.8(3) . . ? N2 C10 C9 123.0(4) . . ? O1 C11 O2 126.0(3) . . ? O1 C11 N3 124.0(4) . . ? O2 C11 N3 110.1(3) . . ? O2 C12 C13 107.4(3) . . ? O3 C14 O4 124.0(3) . . ? O3 C14 N4 125.9(4) . . ? O4 C14 N4 110.1(4) . . ? O4 C15 C16 108.5(4) . . ? N5 C17 C18 120.7(3) . . ? N5 C17 C22 116.0(3) . . ? C18 C17 C22 123.3(3) . . ? C19 C18 C17 120.6(3) . . ? C18 C19 C20 118.6(3) . . ? C19 C20 C21 118.5(3) . . ? C19 C20 N7 124.0(3) . . ? C21 C20 N7 117.5(3) . . ? N5 C21 C20 122.9(3) . . ? N6 C22 C23 120.7(3) . . ? N6 C22 C17 116.5(3) . . ? C23 C22 C17 122.8(3) . . ? C24 C23 C22 119.6(3) . . ? C23 C24 C25 120.3(3) . . ? N8 C25 C24 118.3(3) . . ? N8 C25 C26 124.7(3) . . ? C24 C25 C26 116.9(3) . . ? N6 C26 C25 122.1(3) . . ? O5 C27 O6 125.0(3) . . ? O5 C27 N7 125.7(3) . . ? O6 C27 N7 109.3(3) . . ? C29 C28 O6 107.3(3) . . ? O7 C30 O8 124.6(3) . . ? O7 C30 N8 125.9(3) . . ? O8 C30 N8 109.5(3) . . ? O8 C31 C32 107.3(3) . . ? O9 S1 C33 106.4(2) . . ? O9 S1 C34 102.5(2) . . ? C33 S1 C34 98.1(3) . . ? S1 O9 Zn2 129.43(17) . . ? O10A S2A C36 100.3(6) . . ? O10A S2A C35 112.5(5) . . ? C36 S2A C35 97.3(4) . . ? O11 S3 C38 108.2(2) . . ? O11 S3 C37 106.3(3) . . ? C38 S3 C37 97.0(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3A Cl2 0.86 2.66 3.417(3) 148.4 2_665 N8 H8A Cl3 0.86 2.46 3.302(3) 167.9 2_656 N4 H4A O11 0.86 2.07 2.864(5) 153.7 . N7 H7A O10A 0.86 1.99 2.814(14) 161.5 . _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.559 _refine_diff_density_min -0.418 _refine_diff_density_rms 0.063 ############ data_L1ZnNO3 _database_code_depnum_ccdc_archive 'CCDC 800535' #TrackingRef '- bipy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H58 N14 O20 Zn' _chemical_formula_weight 1216.45 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-31c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 13.499(2) _cell_length_b 13.499(2) _cell_length_c 18.540(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2925.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1268 _exptl_absorpt_coefficient_mu 0.504 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8844 _exptl_absorpt_correction_T_max 0.9148 _exptl_absorpt_process_details SADABS _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 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14489 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0210 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.09 _reflns_number_total 1736 _reflns_number_gt 1138 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 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^)+(0.1670P)^2^+1.6282P] 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 1736 _refine_ls_number_parameters 142 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.1098 _refine_ls_R_factor_gt 0.0760 _refine_ls_wR_factor_ref 0.2847 _refine_ls_wR_factor_gt 0.2226 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.118 _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 Zn1 Zn 0.6667 0.3333 0.2500 0.0804(7) Uani 1 6 d S . . N1 N 0.6401(4) 0.1865(4) 0.31387(19) 0.0825(12) Uani 1 1 d . . . N2 N 0.7034(5) 0.1108(5) 0.4882(3) 0.125(2) Uani 1 1 d . . . H2A H 0.7512 0.1804 0.4997 0.150 Uiso 1 1 calc R . . O1 O 0.6220(8) -0.0658(6) 0.5315(3) 0.179(3) Uani 1 1 d . . . O2 O 0.7492(6) 0.0807(5) 0.5949(3) 0.170(3) Uani 1 1 d . B . C1 C 0.5651(5) 0.0849(5) 0.2862(3) 0.0920(15) Uani 1 1 d . . . C2 C 0.5326(7) -0.0138(6) 0.3252(3) 0.130(3) Uani 1 1 d . . . H2 H 0.4802 -0.0844 0.3057 0.156 Uiso 1 1 calc R . . C3 C 0.5768(6) -0.0087(6) 0.3918(4) 0.122(2) Uani 1 1 d . . . H3 H 0.5543 -0.0753 0.4182 0.146 Uiso 1 1 calc R . . C4 C 0.6544(5) 0.0949(5) 0.4197(3) 0.0973(17) Uani 1 1 d . . . C5 C 0.6829(5) 0.1901(5) 0.3787(3) 0.0887(15) Uani 1 1 d . . . H5 H 0.7352 0.2612 0.3975 0.106 Uiso 1 1 calc R . . C6 C 0.6862(8) 0.0344(8) 0.5369(4) 0.123(2) Uani 1 1 d . . . C7 C 0.7351(12) 0.0006(13) 0.6539(6) 0.205(5) Uani 1 1 d DU . . H7A H 0.7500 0.0380 0.7005 0.246 Uiso 1 1 calc R A 1 H7B H 0.6586 -0.0655 0.6538 0.246 Uiso 1 1 calc R A 1 C8 C 0.820(2) -0.031(3) 0.6366(14) 0.220(9) Uani 0.50 1 d PDU B 1 H8A H 0.7985 -0.1043 0.6579 0.330 Uiso 0.50 1 calc PR B 1 H8B H 0.8931 0.0252 0.6553 0.330 Uiso 0.50 1 calc PR B 1 H8C H 0.8253 -0.0362 0.5852 0.330 Uiso 0.50 1 calc PR B 1 C8' C 0.843(2) 0.079(2) 0.6938(16) 0.261(10) Uani 0.50 1 d PDU B 2 H8'1 H 0.9076 0.0959 0.6645 0.392 Uiso 0.50 1 calc PR B 2 H8'2 H 0.8456 0.0434 0.7378 0.392 Uiso 0.50 1 calc PR B 2 H8'3 H 0.8433 0.1492 0.7049 0.392 Uiso 0.50 1 calc PR B 2 N3 N 0.6667 0.3333 0.5758(6) 0.124(3) Uani 1 3 d S . . O3 O 0.5831(12) 0.2946(19) 0.6107(9) 0.286(8) Uani 0.67 1 d P . . O4 O 0.6667 0.3333 0.5182(7) 0.300(12) Uani 1 3 d S . . O5 O 0.538(3) 0.2688(15) 0.7500 0.284(11) Uani 0.67 2 d SP . . 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 Zn1 0.0935(8) 0.0935(8) 0.0541(8) 0.000 0.000 0.0467(4) N1 0.099(3) 0.098(3) 0.056(2) -0.0026(19) -0.0066(19) 0.053(2) N2 0.155(5) 0.113(4) 0.079(3) 0.010(3) -0.035(3) 0.046(3) O1 0.249(7) 0.141(5) 0.117(4) 0.022(4) -0.056(5) 0.075(5) O2 0.205(6) 0.174(5) 0.095(3) 0.024(3) -0.055(4) 0.069(5) C1 0.113(4) 0.097(4) 0.065(3) -0.001(3) -0.012(3) 0.051(3) C2 0.168(6) 0.094(4) 0.090(4) 0.007(3) -0.042(4) 0.037(4) C3 0.155(6) 0.096(4) 0.091(4) 0.012(3) -0.028(4) 0.045(4) C4 0.124(4) 0.107(4) 0.066(3) 0.004(3) -0.013(3) 0.061(4) C5 0.106(4) 0.097(4) 0.064(3) -0.003(2) -0.009(2) 0.051(3) C6 0.147(6) 0.135(6) 0.085(4) 0.012(4) -0.026(4) 0.069(5) C7 0.209(8) 0.236(8) 0.153(7) 0.029(6) -0.056(6) 0.099(6) C8 0.222(11) 0.230(11) 0.206(11) 0.005(9) -0.025(9) 0.112(8) C8' 0.259(12) 0.265(12) 0.244(12) 0.017(9) -0.027(9) 0.119(9) N3 0.147(6) 0.147(6) 0.078(6) 0.000 0.000 0.074(3) O3 0.195(13) 0.299(19) 0.313(17) 0.113(18) 0.086(12) 0.085(17) O4 0.410(19) 0.410(19) 0.080(8) 0.000 0.000 0.205(10) O5 0.46(4) 0.289(14) 0.158(13) -0.032(13) 0.000 0.232(18) _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 Zn1 N1 2.179(4) 4_665 ? Zn1 N1 2.179(4) 5_655 ? Zn1 N1 2.179(4) 2_655 ? Zn1 N1 2.179(4) 3_665 ? Zn1 N1 2.179(4) 6 ? Zn1 N1 2.179(4) . ? N1 C5 1.324(6) . ? N1 C1 1.335(7) . ? N2 C6 1.301(9) . ? N2 C4 1.397(7) . ? O1 C6 1.191(9) . ? O2 C6 1.318(9) . ? O2 C7 1.481(12) . ? C1 C2 1.381(8) . ? C1 C1 1.473(10) 5_655 ? C2 C3 1.359(9) . ? C3 C4 1.363(8) . ? C4 C5 1.373(8) . ? C7 C8 1.451(17) . ? C7 C8' 1.498(18) . ? N3 O4 1.066(15) . ? N3 O3 1.174(14) 2_655 ? N3 O3 1.174(14) 3_665 ? N3 O3 1.174(14) . ? O3 O3 1.69(2) 2_655 ? O3 O3 1.69(2) 3_665 ? 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 Zn1 N1 93.28(14) 4_665 5_655 ? N1 Zn1 N1 76.1(2) 4_665 2_655 ? N1 Zn1 N1 163.6(2) 5_655 2_655 ? N1 Zn1 N1 163.6(2) 4_665 3_665 ? N1 Zn1 N1 99.6(2) 5_655 3_665 ? N1 Zn1 N1 93.28(14) 2_655 3_665 ? N1 Zn1 N1 93.28(14) 4_665 6 ? N1 Zn1 N1 93.28(14) 5_655 6 ? N1 Zn1 N1 99.6(2) 2_655 6 ? N1 Zn1 N1 76.1(2) 3_665 6 ? N1 Zn1 N1 99.6(2) 4_665 . ? N1 Zn1 N1 76.1(2) 5_655 . ? N1 Zn1 N1 93.28(14) 2_655 . ? N1 Zn1 N1 93.28(14) 3_665 . ? N1 Zn1 N1 163.6(2) 6 . ? C5 N1 C1 118.7(5) . . ? C5 N1 Zn1 126.1(4) . . ? C1 N1 Zn1 114.9(3) . . ? C6 N2 C4 128.7(6) . . ? C6 O2 C7 116.0(8) . . ? N1 C1 C2 120.1(5) . . ? N1 C1 C1 116.9(3) . 5_655 ? C2 C1 C1 123.0(3) . 5_655 ? C3 C2 C1 120.5(6) . . ? C2 C3 C4 119.4(6) . . ? C3 C4 C5 117.5(5) . . ? C3 C4 N2 124.4(6) . . ? C5 C4 N2 118.1(6) . . ? N1 C5 C4 123.8(5) . . ? O1 C6 N2 125.6(7) . . ? O1 C6 O2 122.5(7) . . ? N2 C6 O2 111.9(8) . . ? C8 C7 O2 102.8(15) . . ? C8 C7 C8' 71.9(15) . . ? O2 C7 C8' 97.0(16) . . ? O4 N3 O3 123.6(10) . 2_655 ? O4 N3 O3 123.6(10) . 3_665 ? O3 N3 O3 92.4(13) 2_655 3_665 ? O4 N3 O3 123.6(10) . . ? O3 N3 O3 92.4(13) 2_655 . ? O3 N3 O3 92.4(13) 3_665 . ? N3 O3 O3 43.8(7) . 2_655 ? N3 O3 O3 43.8(7) . 3_665 ? O3 O3 O3 60.000(6) 2_655 3_665 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.431 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.064 ########## data_L1ZnCl_2 _database_code_depnum_ccdc_archive 'CCDC 800536' #TrackingRef '- bipy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C128 H194 Cl4 N24 O51 Zn2' _chemical_formula_weight 3157.61 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 16.8995(14) _cell_length_b 17.5045(15) _cell_length_c 17.6189(15) _cell_angle_alpha 62.5610(10) _cell_angle_beta 63.3520(10) _cell_angle_gamma 79.811(2) _cell_volume 4131.4(6) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.269 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1666 _exptl_absorpt_coefficient_mu 0.439 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9173 _exptl_absorpt_correction_T_max 0.9492 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 21137 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0701 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14401 _reflns_number_gt 9964 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 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^)+(0.1439P)^2^+0.8113P] 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 14401 _refine_ls_number_parameters 992 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.1024 _refine_ls_R_factor_gt 0.0722 _refine_ls_wR_factor_ref 0.2279 _refine_ls_wR_factor_gt 0.2014 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.065 _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 Zn1 Zn 0.52104(3) 0.71968(3) 0.58178(3) 0.03066(17) Uani 1 1 d . . . N1 N 0.6520(2) 0.6980(2) 0.4865(2) 0.0340(8) Uani 1 1 d . . . N2 N 0.5050(2) 0.5950(2) 0.5934(2) 0.0348(8) Uani 1 1 d . . . N3 N 0.8683(2) 0.8015(3) 0.3115(3) 0.0507(10) Uani 1 1 d . . . H3 H 0.8527 0.8529 0.3096 0.061 Uiso 1 1 calc R . . N4 N 0.3453(3) 0.4162(3) 0.7262(3) 0.0539(11) Uani 1 1 d . . . H4 H 0.3017 0.4431 0.7543 0.065 Uiso 1 1 calc R . . N5 N 0.7261(2) 0.5639(3) 0.7770(3) 0.0492(10) Uani 1 1 d . . . H5 H 0.7686 0.5837 0.7195 0.059 Uiso 1 1 calc R . . N6 N 0.5490(2) 0.6629(2) 0.7040(2) 0.0331(8) Uani 1 1 d . . . N7 N 0.3953(2) 0.7136(2) 0.6928(2) 0.0306(7) Uani 1 1 d . . . N8 N 0.1649(2) 0.7624(3) 0.7364(3) 0.0480(10) Uani 1 1 d . . . H8 H 0.1757 0.7887 0.6763 0.058 Uiso 1 1 calc R . . N9 N 0.6785(2) 0.9708(2) 0.5760(2) 0.0383(8) Uani 1 1 d . . . H9 H 0.6727 0.9302 0.6317 0.046 Uiso 1 1 calc R . . N10 N 0.5625(2) 0.8494(2) 0.5336(2) 0.0310(7) Uani 1 1 d . . . N11 N 0.4805(2) 0.7933(2) 0.4695(2) 0.0311(7) Uani 1 1 d . . . N12 N 0.3856(3) 0.7638(2) 0.3361(2) 0.0422(9) Uani 1 1 d . . . H12 H 0.3412 0.7275 0.3825 0.051 Uiso 1 1 calc R . . O1 O 0.9892(2) 0.7277(3) 0.2571(3) 0.0760(12) Uani 1 1 d . . . O2 O 0.9954(2) 0.8715(2) 0.2074(2) 0.0590(9) Uani 1 1 d . . . O3 O 0.3757(3) 0.2914(2) 0.7080(3) 0.0695(11) Uani 1 1 d . . . O4 O 0.2475(3) 0.3083(2) 0.8185(2) 0.0678(11) Uani 1 1 d . . . O5 O 0.7024(2) 0.4805(2) 0.9306(2) 0.0517(9) Uani 1 1 d . . . O6 O 0.8364(2) 0.4949(2) 0.8097(2) 0.0562(9) Uani 1 1 d . . . O7 O 0.0520(3) 0.7235(4) 0.8811(3) 0.1001(18) Uani 1 1 d . . . O8 O 0.0287(2) 0.7881(3) 0.7504(3) 0.0718(12) Uani 1 1 d . . . O9 O 0.7380(2) 1.1062(2) 0.4692(2) 0.0471(8) Uani 1 1 d . . . O10 O 0.7560(2) 1.0351(2) 0.6047(2) 0.0479(8) Uani 1 1 d . . . O11 O 0.4563(3) 0.8317(3) 0.1755(2) 0.0693(11) Uani 1 1 d . . . O12 O 0.3658(2) 0.7141(2) 0.2517(2) 0.0568(9) Uani 1 1 d . . . C1 C 0.6599(3) 0.6210(3) 0.4855(3) 0.0402(10) Uani 1 1 d . . . C2 C 0.7385(3) 0.5985(3) 0.4287(3) 0.0502(12) Uani 1 1 d . . . H2 H 0.7429 0.5431 0.4299 0.060 Uiso 1 1 calc R . . C3 C 0.8102(3) 0.6553(3) 0.3706(3) 0.0533(13) Uani 1 1 d . . . H3A H 0.8644 0.6399 0.3317 0.064 Uiso 1 1 calc R . . C4 C 0.8016(3) 0.7359(3) 0.3700(3) 0.0439(11) Uani 1 1 d . . . C5 C 0.7216(3) 0.7535(3) 0.4298(3) 0.0401(10) Uani 1 1 d . . . H5A H 0.7158 0.8081 0.4307 0.048 Uiso 1 1 calc R . . C6 C 0.5804(3) 0.5626(3) 0.5471(3) 0.0397(10) Uani 1 1 d . . . C7 C 0.5787(3) 0.4793(3) 0.5584(4) 0.0555(13) Uani 1 1 d . . . H7 H 0.6311 0.4574 0.5246 0.067 Uiso 1 1 calc R . . C8 C 0.5034(3) 0.4275(3) 0.6172(4) 0.0571(14) Uani 1 1 d . . . H8A H 0.5039 0.3697 0.6260 0.069 Uiso 1 1 calc R . . C9 C 0.4258(3) 0.4616(3) 0.6639(3) 0.0480(12) Uani 1 1 d . . . C10 C 0.4323(3) 0.5452(3) 0.6499(3) 0.0426(11) Uani 1 1 d . . . H10 H 0.3809 0.5683 0.6834 0.051 Uiso 1 1 calc R . . C11 C 0.9538(3) 0.7937(4) 0.2581(3) 0.0529(13) Uani 1 1 d . . . C12 C 1.0878(3) 0.8763(4) 0.1426(4) 0.0674(16) Uani 1 1 d . . . H12A H 1.1182 0.8235 0.1705 0.081 Uiso 1 1 calc R . . C13 C 1.0943(4) 0.8861(5) 0.0522(4) 0.084(2) Uani 1 1 d . . . H13A H 1.0637 0.8369 0.0632 0.126 Uiso 1 1 calc R . . H13B H 1.1568 0.8884 0.0091 0.126 Uiso 1 1 calc R . . H13C H 1.0667 0.9394 0.0242 0.126 Uiso 1 1 calc R . . C14 C 1.1253(5) 0.9542(5) 0.1327(5) 0.100(2) Uani 1 1 d . . . H14A H 1.0970 1.0059 0.1026 0.149 Uiso 1 1 calc R . . H14B H 1.1893 0.9598 0.0938 0.149 Uiso 1 1 calc R . . H14C H 1.1138 0.9475 0.1951 0.149 Uiso 1 1 calc R . . C15 C 0.3279(4) 0.3347(4) 0.7475(4) 0.0557(13) Uani 1 1 d . . . C16 C 0.2204(4) 0.2202(4) 0.8538(4) 0.0742(18) Uani 1 1 d . . . H16 H 0.2371 0.2059 0.7998 0.089 Uiso 1 1 calc R . . C17 C 0.2665(6) 0.1607(5) 0.9159(6) 0.119(3) Uani 1 1 d . . . H17A H 0.3308 0.1673 0.8785 0.178 Uiso 1 1 calc R . . H17B H 0.2473 0.1008 0.9412 0.178 Uiso 1 1 calc R . . H17C H 0.2510 0.1756 0.9680 0.178 Uiso 1 1 calc R . . C18 C 0.1221(5) 0.2143(5) 0.9070(5) 0.093(2) Uani 1 1 d . . . H18A H 0.1056 0.2331 0.9564 0.139 Uiso 1 1 calc R . . H18B H 0.1009 0.1545 0.9358 0.139 Uiso 1 1 calc R . . H18C H 0.0950 0.2513 0.8638 0.139 Uiso 1 1 calc R . . C19 C 0.4776(3) 0.6502(3) 0.7865(3) 0.0354(9) Uani 1 1 d . . . C20 C 0.4873(3) 0.6093(3) 0.8700(3) 0.0438(11) Uani 1 1 d . . . H20 H 0.4375 0.6014 0.9276 0.053 Uiso 1 1 calc R . . C21 C 0.5682(3) 0.5797(3) 0.8710(3) 0.0463(12) Uani 1 1 d . . . H21 H 0.5746 0.5515 0.9286 0.056 Uiso 1 1 calc R . . C22 C 0.6401(3) 0.5921(3) 0.7862(3) 0.0404(10) Uani 1 1 d . . . C23 C 0.6269(3) 0.6340(3) 0.7053(3) 0.0373(10) Uani 1 1 d . . . H23 H 0.6761 0.6428 0.6470 0.045 Uiso 1 1 calc R . . C24 C 0.3934(3) 0.6800(3) 0.7792(3) 0.0352(9) Uani 1 1 d . . . C25 C 0.3148(3) 0.6752(3) 0.8566(3) 0.0493(12) Uani 1 1 d . . . H25 H 0.3145 0.6533 0.9171 0.059 Uiso 1 1 calc R . . C26 C 0.2362(3) 0.7026(3) 0.8453(3) 0.0511(13) Uani 1 1 d . . . H26 H 0.1822 0.6994 0.8977 0.061 Uiso 1 1 calc R . . C27 C 0.2386(3) 0.7343(3) 0.7564(3) 0.0375(10) Uani 1 1 d . . . C28 C 0.3200(3) 0.7399(3) 0.6820(3) 0.0341(9) Uani 1 1 d . . . H28 H 0.3223 0.7635 0.6204 0.041 Uiso 1 1 calc R . . C29 C 0.7501(3) 0.5098(3) 0.8473(3) 0.0433(11) Uani 1 1 d . . . C30 C 0.8747(3) 0.4346(4) 0.8738(4) 0.0564(13) Uani 1 1 d . . . H30 H 0.8530 0.4450 0.9311 0.068 Uiso 1 1 calc R . . C31 C 0.8519(4) 0.3442(4) 0.9009(4) 0.0660(16) Uani 1 1 d . . . H31A H 0.7874 0.3358 0.9297 0.099 Uiso 1 1 calc R . . H31B H 0.8756 0.3040 0.9461 0.099 Uiso 1 1 calc R . . H31C H 0.8778 0.3336 0.8446 0.099 Uiso 1 1 calc R . . C32 C 0.9726(4) 0.4529(5) 0.8184(7) 0.111(3) Uani 1 1 d . . . H32A H 0.9929 0.4422 0.7627 0.166 Uiso 1 1 calc R . . H32B H 1.0031 0.4153 0.8578 0.166 Uiso 1 1 calc R . . H32C H 0.9859 0.5132 0.7985 0.166 Uiso 1 1 calc R . . C33 C 0.0788(3) 0.7542(4) 0.7979(4) 0.0569(14) Uani 1 1 d . . . C34 C -0.0692(4) 0.7738(6) 0.8059(7) 0.104(2) Uani 1 1 d U . . H34 H -0.0872 0.7581 0.8739 0.125 Uiso 1 1 calc R . . C35 C -0.0922(7) 0.7043(9) 0.7935(10) 0.175(4) Uani 1 1 d U . . H35A H -0.0716 0.6496 0.8294 0.263 Uiso 1 1 calc R . . H35B H -0.0637 0.7170 0.7266 0.263 Uiso 1 1 calc R . . H35C H -0.1566 0.7002 0.8163 0.263 Uiso 1 1 calc R . . C36 C -0.1051(5) 0.8591(7) 0.7583(9) 0.175(5) Uani 1 1 d U . . H36A H -0.0962 0.8671 0.6961 0.263 Uiso 1 1 calc R . . H36B H -0.0738 0.9059 0.7510 0.263 Uiso 1 1 calc R . . H36C H -0.1685 0.8598 0.7969 0.263 Uiso 1 1 calc R . . C37 C 0.5574(3) 0.9070(3) 0.4534(2) 0.0295(9) Uani 1 1 d . . . C38 C 0.5920(3) 0.9896(3) 0.4086(3) 0.0352(9) Uani 1 1 d . . . H38 H 0.5874 1.0295 0.3518 0.042 Uiso 1 1 calc R . . C39 C 0.6332(3) 1.0147(3) 0.4457(3) 0.0375(10) Uani 1 1 d . . . H39 H 0.6577 1.0716 0.4148 0.045 Uiso 1 1 calc R . . C40 C 0.6385(3) 0.9546(3) 0.5302(3) 0.0358(10) Uani 1 1 d . . . C41 C 0.6017(3) 0.8732(3) 0.5713(3) 0.0329(9) Uani 1 1 d . . . H41 H 0.6041 0.8322 0.6289 0.040 Uiso 1 1 calc R . . C42 C 0.5130(3) 0.8746(3) 0.4158(3) 0.0328(9) Uani 1 1 d . . . C43 C 0.5050(3) 0.9239(3) 0.3323(3) 0.0396(10) Uani 1 1 d . . . H43 H 0.5279 0.9817 0.2952 0.047 Uiso 1 1 calc R . . C44 C 0.4636(3) 0.8892(3) 0.3027(3) 0.0453(11) Uani 1 1 d . . . H44 H 0.4583 0.9224 0.2449 0.054 Uiso 1 1 calc R . . C45 C 0.4299(3) 0.8056(3) 0.3581(3) 0.0359(10) Uani 1 1 d . . . C46 C 0.4402(3) 0.7602(3) 0.4417(3) 0.0343(9) Uani 1 1 d . . . H46 H 0.4171 0.7025 0.4807 0.041 Uiso 1 1 calc R . . C47 C 0.7254(3) 1.0436(3) 0.5423(3) 0.0402(10) Uani 1 1 d . . . C48 C 0.8092(4) 1.1082(3) 0.5778(4) 0.0573(14) Uani 1 1 d . . . H48 H 0.7832 1.1629 0.5461 0.069 Uiso 1 1 calc R . . C49 C 0.9034(4) 1.1052(4) 0.5113(4) 0.0696(16) Uani 1 1 d . . . H49A H 0.9279 1.0500 0.5403 0.104 Uiso 1 1 calc R . . H49B H 0.9388 1.1524 0.4977 0.104 Uiso 1 1 calc R . . H49C H 0.9048 1.1114 0.4525 0.104 Uiso 1 1 calc R . . C50 C 0.7999(5) 1.1021(4) 0.6690(4) 0.0724(17) Uani 1 1 d . . . H50A H 0.8268 1.0495 0.6995 0.109 Uiso 1 1 calc R . . H50B H 0.7369 1.1006 0.7104 0.109 Uiso 1 1 calc R . . H50C H 0.8298 1.1524 0.6568 0.109 Uiso 1 1 calc R . . C51 C 0.4076(3) 0.7763(3) 0.2463(3) 0.0473(12) Uani 1 1 d . . . C52 C 0.3715(4) 0.7230(4) 0.1626(4) 0.0654(16) Uani 1 1 d . . . H52 H 0.4264 0.7566 0.1085 0.078 Uiso 1 1 calc R . . C53 C 0.2892(5) 0.7699(7) 0.1542(5) 0.111(3) Uani 1 1 d . . . H53A H 0.2364 0.7339 0.2055 0.167 Uiso 1 1 calc R . . H53B H 0.2906 0.7820 0.0935 0.167 Uiso 1 1 calc R . . H53C H 0.2873 0.8243 0.1583 0.167 Uiso 1 1 calc R . . C54 C 0.3711(5) 0.6346(5) 0.1720(5) 0.097(2) Uani 1 1 d . . . H54A H 0.4238 0.6056 0.1803 0.146 Uiso 1 1 calc R . . H54B H 0.3715 0.6373 0.1150 0.146 Uiso 1 1 calc R . . H54C H 0.3178 0.6024 0.2268 0.146 Uiso 1 1 calc R . . Cl1 Cl 0.18711(11) 0.63304(9) 0.57836(11) 0.0728(5) Uani 1 1 d D . . O13 O 0.1528(5) 0.5526(3) 0.6335(5) 0.191(4) Uani 1 1 d D . . O14 O 0.2404(5) 0.6428(4) 0.4908(4) 0.166(3) Uani 1 1 d D . . O15' O 0.1488(8) 0.6836(8) 0.6209(9) 0.097(4) Uani 0.450(5) 1 d P . . O15 O 0.1166(7) 0.6821(7) 0.5702(13) 0.260(13) Uani 0.550(5) 1 d PD . . O16 O 0.2420(9) 0.6617(11) 0.5949(8) 0.427(15) Uani 1 1 d D . . Cl2 Cl 0.40459(12) 0.84150(9) 0.87912(10) 0.0717(4) Uani 1 1 d . . . O17 O 0.4410(3) 0.8594(3) 0.7816(3) 0.0899(14) Uani 1 1 d . . . O18 O 0.3133(4) 0.8179(4) 0.9242(4) 0.129(2) Uani 1 1 d . . . O19 O 0.4168(4) 0.9148(3) 0.8873(3) 0.0980(15) Uani 1 1 d . . . O20 O 0.4473(6) 0.7714(4) 0.9228(4) 0.157(3) Uani 1 1 d . . . O21 O 0.8242(3) 0.9731(3) 0.2890(3) 0.0705(11) Uani 1 1 d . . . C55 C 0.7594(5) 0.9714(5) 0.1946(5) 0.0843(19) Uani 1 1 d . . . H55A H 0.8063 0.9410 0.1623 0.126 Uiso 1 1 calc R . . H55B H 0.7289 1.0075 0.1546 0.126 Uiso 1 1 calc R . . H55C H 0.7169 0.9293 0.2543 0.126 Uiso 1 1 calc R . . C56 C 0.7994(5) 1.0272(4) 0.2137(5) 0.083(2) Uani 1 1 d . . . H56A H 0.8520 1.0601 0.1566 0.100 Uiso 1 1 calc R . . H56B H 0.7558 1.0688 0.2312 0.100 Uiso 1 1 calc R . . C57 C 0.8745(5) 1.0195(5) 0.3002(6) 0.092(2) Uani 1 1 d . . . H57A H 0.8397 1.0670 0.3139 0.111 Uiso 1 1 calc R . . H57B H 0.9288 1.0447 0.2414 0.111 Uiso 1 1 calc R . . C58 C 0.8983(6) 0.9615(7) 0.3779(7) 0.122(3) Uani 1 1 d . . . H58A H 0.8447 0.9316 0.4341 0.183 Uiso 1 1 calc R . . H58B H 0.9270 0.9948 0.3912 0.183 Uiso 1 1 calc R . . H58C H 0.9392 0.9191 0.3604 0.183 Uiso 1 1 calc R . . O22 O 0.8519(3) 0.6250(4) 0.5847(3) 0.116(2) Uani 1 1 d . . . C59 C 0.8480(7) 0.4862(8) 0.5948(7) 0.152(4) Uani 1 1 d . . . H59A H 0.8484 0.4462 0.6559 0.228 Uiso 1 1 calc R . . H59B H 0.8726 0.4586 0.5519 0.228 Uiso 1 1 calc R . . H59C H 0.7870 0.5020 0.6033 0.228 Uiso 1 1 calc R . . C60 C 0.9069(7) 0.5713(11) 0.5509(7) 0.194(8) Uani 1 1 d . . . H60A H 0.9563 0.5570 0.5703 0.233 Uiso 1 1 calc R . . H60B H 0.9319 0.5981 0.4812 0.233 Uiso 1 1 calc R . . C61 C 0.9033(6) 0.7057(8) 0.5502(7) 0.141(4) Uani 1 1 d . . . H61A H 0.9322 0.7341 0.4805 0.169 Uiso 1 1 calc R . . H61B H 0.9497 0.6912 0.5739 0.169 Uiso 1 1 calc R . . C62 C 0.8365(8) 0.7660(8) 0.5880(9) 0.165(5) Uani 1 1 d . . . H62A H 0.7861 0.7725 0.5725 0.248 Uiso 1 1 calc R . . H62B H 0.8655 0.8225 0.5590 0.248 Uiso 1 1 calc R . . H62C H 0.8156 0.7412 0.6566 0.248 Uiso 1 1 calc R . . O23 O 0.6418(3) 0.8264(3) 0.7565(3) 0.0976(16) Uani 1 1 d . . . O24 O 0.2217(10) 0.5227(9) 0.8043(9) 0.164(5) Uani 0.550(5) 1 d PD A 1 H24 H 0.1663 0.5168 0.8270 0.246 Uiso 0.550(5) 1 calc PR A 1 C63 C 0.2534(8) 0.4638(11) 0.8762(12) 0.113(5) Uani 0.550(5) 1 d PD A 1 H63A H 0.3169 0.4558 0.8455 0.169 Uiso 0.550(5) 1 calc PR A 1 H63B H 0.2213 0.4080 0.9112 0.169 Uiso 0.550(5) 1 calc PR A 1 H63C H 0.2431 0.4883 0.9197 0.169 Uiso 0.550(5) 1 calc PR A 1 O24' O 0.1743(12) 0.4576(11) 0.9349(12) 0.164(5) Uani 0.450(5) 1 d PD A 2 H24' H 0.1317 0.4282 0.9851 0.246 Uiso 0.450(5) 1 calc PR A 2 C63' C 0.1435(10) 0.5106(15) 0.8689(15) 0.113(5) Uani 0.450(5) 1 d PD A 2 H63D H 0.1937 0.5392 0.8080 0.169 Uiso 0.450(5) 1 calc PR A 2 H63E H 0.1069 0.5541 0.8881 0.169 Uiso 0.450(5) 1 calc PR A 2 H63F H 0.1079 0.4767 0.8632 0.169 Uiso 0.450(5) 1 calc PR A 2 C64 C 0.6708(14) 0.8837(12) 0.8874(12) 0.163(9) Uani 0.550(5) 1 d PD A 1 H64A H 0.6146 0.9083 0.9151 0.244 Uiso 0.550(5) 1 calc PR A 1 H64B H 0.6921 0.9107 0.8187 0.244 Uiso 0.550(5) 1 calc PR A 1 H64C H 0.7147 0.8942 0.9040 0.244 Uiso 0.550(5) 1 calc PR A 1 O25 O 0.6577(9) 0.7926(10) 0.9233(10) 0.137(4) Uani 0.550(5) 1 d PD A 1 H25A H 0.6498 0.7826 0.8849 0.205 Uiso 0.550(5) 1 calc PR A 1 O25' O 0.6441(11) 0.9419(11) 0.8895(15) 0.137(4) Uani 0.450(5) 1 d PD A 2 H25' H 0.6875 0.9429 0.9001 0.205 Uiso 0.450(5) 1 calc PR A 2 C64' C 0.6004(15) 0.8619(14) 0.9485(13) 0.163(9) Uani 0.450(5) 1 d PD A 2 H64D H 0.6197 0.8313 0.9996 0.244 Uiso 0.450(5) 1 calc PR A 2 H64E H 0.6143 0.8285 0.9125 0.244 Uiso 0.450(5) 1 calc PR A 2 H64F H 0.5364 0.8695 0.9752 0.244 Uiso 0.450(5) 1 calc PR A 2 O26 O 0.6371(16) 0.645(3) 0.031(3) 0.42(3) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0325(3) 0.0270(3) 0.0244(3) -0.0102(2) -0.00626(19) 0.00036(19) N1 0.0359(19) 0.0282(19) 0.0270(17) -0.0082(15) -0.0076(15) -0.0007(15) N2 0.040(2) 0.0277(19) 0.0295(17) -0.0113(15) -0.0080(15) -0.0027(15) N3 0.042(2) 0.043(2) 0.050(2) -0.022(2) -0.0030(18) -0.0036(18) N4 0.050(2) 0.041(2) 0.055(2) -0.023(2) 0.000(2) -0.0138(19) N5 0.035(2) 0.060(3) 0.0308(19) -0.0084(19) -0.0073(16) 0.0009(19) N6 0.0320(19) 0.0295(19) 0.0266(17) -0.0081(15) -0.0074(14) 0.0004(15) N7 0.0339(18) 0.0267(18) 0.0256(16) -0.0113(15) -0.0086(14) 0.0027(15) N8 0.038(2) 0.056(3) 0.0320(19) -0.0126(19) -0.0098(17) 0.0089(19) N9 0.054(2) 0.032(2) 0.0337(18) -0.0123(16) -0.0243(17) 0.0025(17) N10 0.0357(18) 0.0279(18) 0.0239(16) -0.0117(15) -0.0083(14) 0.0033(15) N11 0.0336(18) 0.0257(18) 0.0321(17) -0.0134(15) -0.0112(15) 0.0012(15) N12 0.050(2) 0.039(2) 0.0353(19) -0.0139(17) -0.0160(17) -0.0061(18) O1 0.044(2) 0.056(2) 0.080(3) -0.025(2) 0.0052(19) 0.0074(18) O2 0.0439(19) 0.058(2) 0.0499(19) -0.0202(18) 0.0016(16) -0.0116(17) O3 0.078(3) 0.042(2) 0.082(3) -0.023(2) -0.030(2) -0.005(2) O4 0.078(3) 0.058(2) 0.053(2) -0.0216(19) -0.0072(19) -0.031(2) O5 0.0451(18) 0.064(2) 0.0355(17) -0.0184(17) -0.0160(15) 0.0135(17) O6 0.0355(18) 0.060(2) 0.0508(19) -0.0097(18) -0.0171(15) 0.0068(16) O7 0.043(2) 0.162(5) 0.043(2) -0.021(3) -0.0088(18) 0.025(3) O8 0.0372(19) 0.101(3) 0.056(2) -0.029(2) -0.0141(17) 0.019(2) O9 0.064(2) 0.0350(18) 0.0446(18) -0.0097(16) -0.0298(16) -0.0071(16) O10 0.066(2) 0.0412(19) 0.0488(18) -0.0174(16) -0.0356(17) -0.0004(16) O11 0.098(3) 0.067(3) 0.0393(19) -0.0150(19) -0.021(2) -0.033(2) O12 0.071(2) 0.060(2) 0.053(2) -0.0271(18) -0.0293(18) -0.0133(19) C1 0.045(3) 0.032(2) 0.036(2) -0.016(2) -0.011(2) 0.004(2) C2 0.048(3) 0.034(3) 0.051(3) -0.020(2) -0.005(2) 0.002(2) C3 0.047(3) 0.046(3) 0.045(3) -0.023(2) -0.001(2) 0.008(2) C4 0.041(2) 0.040(3) 0.036(2) -0.017(2) -0.001(2) -0.005(2) C5 0.043(3) 0.033(2) 0.037(2) -0.017(2) -0.009(2) 0.001(2) C6 0.042(2) 0.031(2) 0.041(2) -0.016(2) -0.015(2) 0.007(2) C7 0.046(3) 0.044(3) 0.064(3) -0.030(3) -0.008(2) 0.005(2) C8 0.053(3) 0.035(3) 0.071(3) -0.029(3) -0.011(3) 0.003(2) C9 0.057(3) 0.034(3) 0.042(2) -0.016(2) -0.010(2) -0.007(2) C10 0.043(3) 0.037(3) 0.039(2) -0.019(2) -0.006(2) -0.005(2) C11 0.044(3) 0.058(3) 0.038(3) -0.020(3) -0.002(2) -0.005(3) C12 0.037(3) 0.078(4) 0.056(3) -0.016(3) -0.004(2) -0.010(3) C13 0.067(4) 0.092(5) 0.060(4) -0.027(4) -0.005(3) -0.002(4) C14 0.079(5) 0.099(6) 0.091(5) -0.009(4) -0.031(4) -0.036(4) C15 0.066(3) 0.046(3) 0.050(3) -0.020(3) -0.017(3) -0.011(3) C16 0.090(5) 0.057(4) 0.067(4) -0.011(3) -0.030(3) -0.036(3) C17 0.138(7) 0.087(6) 0.101(6) 0.023(5) -0.071(6) -0.058(5) C18 0.089(5) 0.094(5) 0.084(4) -0.036(4) -0.013(4) -0.046(4) C19 0.039(2) 0.031(2) 0.027(2) -0.0121(18) -0.0085(18) 0.0038(18) C20 0.038(2) 0.054(3) 0.030(2) -0.019(2) -0.0082(19) 0.009(2) C21 0.040(3) 0.058(3) 0.031(2) -0.015(2) -0.0125(19) 0.007(2) C22 0.037(2) 0.043(3) 0.033(2) -0.014(2) -0.0131(19) 0.005(2) C23 0.036(2) 0.033(2) 0.029(2) -0.0097(19) -0.0048(18) -0.0027(19) C24 0.033(2) 0.034(2) 0.033(2) -0.0168(19) -0.0098(18) 0.0064(18) C25 0.040(3) 0.065(3) 0.030(2) -0.022(2) -0.008(2) 0.013(2) C26 0.040(3) 0.065(3) 0.032(2) -0.019(2) -0.009(2) 0.015(2) C27 0.035(2) 0.038(2) 0.033(2) -0.016(2) -0.0104(18) 0.0045(19) C28 0.039(2) 0.031(2) 0.030(2) -0.0136(18) -0.0137(18) 0.0055(19) C29 0.040(3) 0.044(3) 0.041(3) -0.016(2) -0.016(2) 0.004(2) C30 0.048(3) 0.064(4) 0.057(3) -0.023(3) -0.029(3) 0.013(3) C31 0.074(4) 0.069(4) 0.053(3) -0.035(3) -0.023(3) 0.021(3) C32 0.059(4) 0.095(6) 0.153(7) -0.026(5) -0.054(5) 0.008(4) C33 0.042(3) 0.070(4) 0.049(3) -0.025(3) -0.017(2) 0.017(3) C34 0.050(3) 0.141(7) 0.143(6) -0.077(5) -0.051(4) 0.032(4) C35 0.102(6) 0.183(9) 0.207(8) -0.082(8) -0.035(6) -0.013(6) C36 0.059(4) 0.151(8) 0.225(9) -0.049(7) -0.032(5) 0.035(5) C37 0.032(2) 0.030(2) 0.0216(18) -0.0114(17) -0.0071(16) 0.0006(17) C38 0.044(2) 0.028(2) 0.027(2) -0.0086(18) -0.0140(18) 0.0019(19) C39 0.047(3) 0.031(2) 0.029(2) -0.0081(19) -0.0144(19) -0.005(2) C40 0.040(2) 0.032(2) 0.034(2) -0.0168(19) -0.0130(18) 0.0022(19) C41 0.038(2) 0.033(2) 0.0244(19) -0.0135(18) -0.0103(17) 0.0031(18) C42 0.035(2) 0.031(2) 0.029(2) -0.0150(19) -0.0087(17) 0.0026(18) C43 0.051(3) 0.031(2) 0.031(2) -0.0090(19) -0.014(2) -0.008(2) C44 0.064(3) 0.039(3) 0.035(2) -0.013(2) -0.024(2) -0.004(2) C45 0.039(2) 0.035(2) 0.035(2) -0.017(2) -0.0134(18) -0.0019(19) C46 0.035(2) 0.030(2) 0.030(2) -0.0140(19) -0.0077(17) 0.0023(18) C47 0.048(3) 0.034(3) 0.039(2) -0.016(2) -0.020(2) 0.006(2) C48 0.081(4) 0.042(3) 0.075(3) -0.025(3) -0.053(3) 0.002(3) C49 0.057(3) 0.080(4) 0.081(4) -0.041(4) -0.028(3) -0.002(3) C50 0.108(5) 0.065(4) 0.080(4) -0.039(3) -0.062(4) 0.008(4) C51 0.059(3) 0.041(3) 0.048(3) -0.019(2) -0.028(2) 0.002(2) C52 0.079(4) 0.083(4) 0.053(3) -0.038(3) -0.033(3) -0.003(3) C53 0.102(6) 0.181(9) 0.101(5) -0.092(6) -0.066(5) 0.047(6) C54 0.129(6) 0.099(6) 0.091(5) -0.060(5) -0.041(5) -0.016(5) Cl1 0.0755(10) 0.0457(8) 0.0704(9) -0.0308(7) 0.0010(8) -0.0094(7) O13 0.163(6) 0.059(3) 0.165(6) -0.036(4) 0.080(5) -0.030(4) O14 0.159(6) 0.132(5) 0.115(5) -0.063(4) 0.051(4) -0.064(5) O15' 0.068(7) 0.129(10) 0.135(9) -0.115(9) -0.024(7) 0.028(7) O15 0.099(9) 0.092(9) 0.54(4) -0.086(16) -0.159(16) 0.051(8) O16 0.292(16) 0.73(4) 0.230(12) -0.144(17) -0.027(11) -0.34(2) Cl2 0.1006(12) 0.0474(8) 0.0551(8) -0.0078(7) -0.0336(8) -0.0094(8) O17 0.130(4) 0.064(3) 0.049(2) -0.006(2) -0.027(2) -0.018(3) O18 0.104(4) 0.152(6) 0.107(4) -0.061(4) 0.000(3) -0.050(4) O19 0.146(5) 0.067(3) 0.091(3) -0.030(3) -0.057(3) -0.011(3) O20 0.285(9) 0.087(4) 0.108(4) -0.040(4) -0.117(5) 0.077(5) O21 0.071(3) 0.058(3) 0.084(3) -0.041(2) -0.024(2) 0.005(2) C55 0.083(5) 0.081(5) 0.081(4) -0.036(4) -0.027(4) 0.005(4) C56 0.087(5) 0.058(4) 0.069(4) -0.022(3) -0.005(4) -0.012(4) C57 0.091(5) 0.089(5) 0.117(6) -0.071(5) -0.031(5) -0.003(4) C58 0.111(7) 0.158(9) 0.158(9) -0.122(8) -0.057(6) 0.022(6) O22 0.055(3) 0.174(6) 0.052(3) -0.020(3) -0.006(2) 0.026(3) C59 0.116(8) 0.195(12) 0.091(6) -0.064(7) -0.001(6) 0.015(8) C60 0.094(7) 0.31(2) 0.082(6) -0.068(9) -0.005(5) 0.077(10) C61 0.082(6) 0.173(11) 0.094(6) -0.005(7) -0.015(5) -0.043(7) C62 0.124(9) 0.133(10) 0.188(12) -0.033(9) -0.053(9) -0.023(8) O23 0.122(4) 0.084(3) 0.052(2) -0.012(2) -0.032(3) 0.016(3) O24 0.171(11) 0.109(8) 0.140(8) -0.083(7) 0.030(8) -0.019(8) C63 0.063(7) 0.122(11) 0.128(11) -0.087(10) 0.028(7) -0.035(7) O24' 0.171(11) 0.109(8) 0.140(8) -0.083(7) 0.030(8) -0.019(8) C63' 0.063(7) 0.122(11) 0.128(11) -0.087(10) 0.028(7) -0.035(7) C64 0.123(13) 0.30(3) 0.105(12) -0.124(16) -0.056(9) 0.053(16) O25 0.125(7) 0.128(9) 0.153(9) -0.025(7) -0.088(7) -0.008(6) O25' 0.125(7) 0.128(9) 0.153(9) -0.025(7) -0.088(7) -0.008(6) C64' 0.123(13) 0.30(3) 0.105(12) -0.124(16) -0.056(9) 0.053(16) O26 0.18(2) 0.64(7) 0.53(5) -0.40(6) -0.03(3) -0.16(3) _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 Zn1 N7 2.124(3) . ? Zn1 N11 2.144(3) . ? Zn1 N10 2.150(3) . ? Zn1 N6 2.150(3) . ? Zn1 N2 2.152(3) . ? Zn1 N1 2.194(3) . ? N1 C5 1.335(5) . ? N1 C1 1.339(5) . ? N2 C10 1.319(5) . ? N2 C6 1.360(5) . ? N3 C11 1.350(6) . ? N3 C4 1.405(6) . ? N3 H3 0.8800 . ? N4 C15 1.348(6) . ? N4 C9 1.388(6) . ? N4 H4 0.8800 . ? N5 C29 1.352(6) . ? N5 C22 1.412(6) . ? N5 H5 0.8800 . ? N6 C23 1.330(5) . ? N6 C19 1.358(5) . ? N7 C28 1.341(5) . ? N7 C24 1.343(5) . ? N8 C33 1.353(6) . ? N8 C27 1.391(6) . ? N8 H8 0.8800 . ? N9 C47 1.357(6) . ? N9 C40 1.398(5) . ? N9 H9 0.8800 . ? N10 C37 1.337(5) . ? N10 C41 1.342(5) . ? N11 C46 1.319(5) . ? N11 C42 1.339(5) . ? N12 C51 1.368(6) . ? N12 C45 1.401(5) . ? N12 H12 0.8800 . ? O1 C11 1.207(6) . ? O2 C11 1.342(6) . ? O2 C12 1.452(6) . ? O3 C15 1.216(6) . ? O4 C15 1.337(6) . ? O4 C16 1.445(7) . ? O5 C29 1.208(5) . ? O6 C29 1.339(5) . ? O6 C30 1.456(6) . ? O7 C33 1.186(6) . ? O8 C33 1.331(6) . ? O8 C34 1.492(8) . ? O9 C47 1.201(5) . ? O10 C47 1.352(5) . ? O10 C48 1.462(6) . ? O11 C51 1.192(6) . ? O12 C51 1.345(6) . ? O12 C52 1.462(5) . ? C1 C2 1.380(6) . ? C1 C6 1.477(6) . ? C2 C3 1.372(7) . ? C2 H2 0.9500 . ? C3 C4 1.388(7) . ? C3 H3A 0.9500 . ? C4 C5 1.381(6) . ? C5 H5A 0.9500 . ? C6 C7 1.381(6) . ? C7 C8 1.369(7) . ? C7 H7 0.9500 . ? C8 C9 1.400(7) . ? C8 H8A 0.9500 . ? C9 C10 1.384(6) . ? C10 H10 0.9500 . ? C12 C13 1.477(8) . ? C12 C14 1.508(9) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C16 C18 1.492(9) . ? C16 C17 1.522(10) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.382(6) . ? C19 C24 1.467(6) . ? C20 C21 1.379(6) . ? C20 H20 0.9500 . ? C21 C22 1.387(6) . ? C21 H21 0.9500 . ? C22 C23 1.372(6) . ? C23 H23 0.9500 . ? C24 C25 1.393(6) . ? C25 C26 1.400(7) . ? C25 H25 0.9500 . ? C26 C27 1.382(6) . ? C26 H26 0.9500 . ? C27 C28 1.390(6) . ? C28 H28 0.9500 . ? C30 C31 1.494(8) . ? C30 C32 1.499(8) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C34 C35 1.471(14) . ? C34 C36 1.511(13) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.375(6) . ? C37 C42 1.504(6) . ? C38 C39 1.372(6) . ? C38 H38 0.9500 . ? C39 C40 1.406(6) . ? C39 H39 0.9500 . ? C40 C41 1.378(6) . ? C41 H41 0.9500 . ? C42 C43 1.376(6) . ? C43 C44 1.379(6) . ? C43 H43 0.9500 . ? C44 C45 1.377(6) . ? C44 H44 0.9500 . ? C45 C46 1.391(6) . ? C46 H46 0.9500 . ? C48 C50 1.497(7) . ? C48 C49 1.505(8) . ? C48 H48 1.0000 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C52 C54 1.480(9) . ? C52 C53 1.517(9) . ? C52 H52 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? Cl1 O15' 1.319(8) . ? Cl1 O16 1.319(8) . ? Cl1 O14 1.336(5) . ? Cl1 O13 1.336(5) . ? Cl1 O15 1.362(9) . ? O15' O15 1.249(18) . ? O15' O16 1.463(16) . ? Cl2 O20 1.391(6) . ? Cl2 O19 1.414(5) . ? Cl2 O18 1.416(6) . ? Cl2 O17 1.433(4) . ? O21 C57 1.400(8) . ? O21 C56 1.426(8) . ? C55 C56 1.507(9) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.461(11) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? O22 C60 1.346(13) . ? O22 C61 1.513(12) . ? C59 C60 1.606(18) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.544(15) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? O24 C63 1.472(10) . ? O24 H24 0.8400 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? O24' C63' 1.364(10) . ? O24' H24' 0.8400 . ? C63' H63D 0.9800 . ? C63' H63E 0.9800 . ? C63' H63F 0.9800 . ? C64 O25 1.435(10) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? O25 H25A 0.8400 . ? O25' C64' 1.385(10) . ? O25' H25' 0.8400 . ? C64' H64D 0.9800 . ? C64' H64E 0.9800 . ? C64' H64F 0.9800 . ? 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 N7 Zn1 N11 96.05(12) . . ? N7 Zn1 N10 99.37(12) . . ? N11 Zn1 N10 76.51(12) . . ? N7 Zn1 N6 76.85(12) . . ? N11 Zn1 N6 169.50(12) . . ? N10 Zn1 N6 96.82(13) . . ? N7 Zn1 N2 94.73(12) . . ? N11 Zn1 N2 96.73(13) . . ? N10 Zn1 N2 164.89(12) . . ? N6 Zn1 N2 91.61(13) . . ? N7 Zn1 N1 168.16(12) . . ? N11 Zn1 N1 92.84(12) . . ? N10 Zn1 N1 90.28(12) . . ? N6 Zn1 N1 95.31(12) . . ? N2 Zn1 N1 76.43(13) . . ? C5 N1 C1 118.3(4) . . ? C5 N1 Zn1 126.9(3) . . ? C1 N1 Zn1 114.7(3) . . ? C10 N2 C6 119.1(4) . . ? C10 N2 Zn1 125.2(3) . . ? C6 N2 Zn1 115.1(3) . . ? C11 N3 C4 126.6(4) . . ? C11 N3 H3 116.7 . . ? C4 N3 H3 116.7 . . ? C15 N4 C9 125.9(4) . . ? C15 N4 H4 117.0 . . ? C9 N4 H4 117.0 . . ? C29 N5 C22 126.9(4) . . ? C29 N5 H5 116.6 . . ? C22 N5 H5 116.6 . . ? C23 N6 C19 119.2(3) . . ? C23 N6 Zn1 125.6(3) . . ? C19 N6 Zn1 114.9(3) . . ? C28 N7 C24 119.4(3) . . ? C28 N7 Zn1 124.7(3) . . ? C24 N7 Zn1 115.9(3) . . ? C33 N8 C27 128.0(4) . . ? C33 N8 H8 116.0 . . ? C27 N8 H8 116.0 . . ? C47 N9 C40 125.9(4) . . ? C47 N9 H9 117.0 . . ? C40 N9 H9 117.0 . . ? C37 N10 C41 119.1(4) . . ? C37 N10 Zn1 115.4(3) . . ? C41 N10 Zn1 125.0(3) . . ? C46 N11 C42 119.3(3) . . ? C46 N11 Zn1 124.3(3) . . ? C42 N11 Zn1 115.3(3) . . ? C51 N12 C45 123.6(4) . . ? C51 N12 H12 118.2 . . ? C45 N12 H12 118.2 . . ? C11 O2 C12 116.9(4) . . ? C15 O4 C16 116.6(5) . . ? C29 O6 C30 117.6(4) . . ? C33 O8 C34 117.3(5) . . ? C47 O10 C48 115.8(4) . . ? C51 O12 C52 116.3(4) . . ? N1 C1 C2 121.2(4) . . ? N1 C1 C6 116.6(4) . . ? C2 C1 C6 122.3(4) . . ? C3 C2 C1 120.6(4) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 118.4(4) . . ? C2 C3 H3A 120.8 . . ? C4 C3 H3A 120.8 . . ? C5 C4 C3 117.8(4) . . ? C5 C4 N3 117.6(4) . . ? C3 C4 N3 124.5(4) . . ? N1 C5 C4 123.7(4) . . ? N1 C5 H5A 118.2 . . ? C4 C5 H5A 118.2 . . ? N2 C6 C7 119.3(4) . . ? N2 C6 C1 116.7(4) . . ? C7 C6 C1 124.0(4) . . ? C8 C7 C6 121.7(4) . . ? C8 C7 H7 119.2 . . ? C6 C7 H7 119.2 . . ? C7 C8 C9 118.6(4) . . ? C7 C8 H8A 120.7 . . ? C9 C8 H8A 120.7 . . ? C10 C9 N4 118.4(4) . . ? C10 C9 C8 116.7(4) . . ? N4 C9 C8 124.8(4) . . ? N2 C10 C9 124.5(4) . . ? N2 C10 H10 117.7 . . ? C9 C10 H10 117.7 . . ? O1 C11 O2 124.5(5) . . ? O1 C11 N3 126.4(5) . . ? O2 C11 N3 109.0(5) . . ? O2 C12 C13 109.8(5) . . ? O2 C12 C14 103.8(5) . . ? C13 C12 C14 112.4(5) . . ? O2 C12 H12A 110.2 . . ? C13 C12 H12A 110.2 . . ? C14 C12 H12A 110.2 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O3 C15 O4 124.1(5) . . ? O3 C15 N4 126.3(5) . . ? O4 C15 N4 109.5(5) . . ? O4 C16 C18 106.5(6) . . ? O4 C16 C17 109.0(5) . . ? C18 C16 C17 112.2(6) . . ? O4 C16 H16 109.7 . . ? C18 C16 H16 109.7 . . ? C17 C16 H16 109.7 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N6 C19 C20 119.6(4) . . ? N6 C19 C24 115.7(3) . . ? C20 C19 C24 124.6(4) . . ? C21 C20 C19 121.0(4) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C20 C21 C22 118.6(4) . . ? C20 C21 H21 120.7 . . ? C22 C21 H21 120.7 . . ? C23 C22 C21 118.0(4) . . ? C23 C22 N5 117.4(4) . . ? C21 C22 N5 124.6(4) . . ? N6 C23 C22 123.6(4) . . ? N6 C23 H23 118.2 . . ? C22 C23 H23 118.2 . . ? N7 C24 C25 120.5(4) . . ? N7 C24 C19 116.5(3) . . ? C25 C24 C19 122.9(4) . . ? C24 C25 C26 120.0(4) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C27 C26 C25 118.7(4) . . ? C27 C26 H26 120.7 . . ? C25 C26 H26 120.7 . . ? C26 C27 C28 118.1(4) . . ? C26 C27 N8 124.1(4) . . ? C28 C27 N8 117.8(4) . . ? N7 C28 C27 123.2(4) . . ? N7 C28 H28 118.4 . . ? C27 C28 H28 118.4 . . ? O5 C29 O6 125.1(4) . . ? O5 C29 N5 126.0(4) . . ? O6 C29 N5 108.9(4) . . ? O6 C30 C31 109.9(4) . . ? O6 C30 C32 104.7(5) . . ? C31 C30 C32 110.7(5) . . ? O6 C30 H30 110.5 . . ? C31 C30 H30 110.5 . . ? C32 C30 H30 110.5 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O7 C33 O8 125.2(5) . . ? O7 C33 N8 125.5(5) . . ? O8 C33 N8 109.3(4) . . ? C35 C34 O8 105.2(7) . . ? C35 C34 C36 112.3(9) . . ? O8 C34 C36 103.4(7) . . ? C35 C34 H34 111.8 . . ? O8 C34 H34 111.8 . . ? C36 C34 H34 111.8 . . ? 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 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N10 C37 C38 121.3(4) . . ? N10 C37 C42 115.6(3) . . ? C38 C37 C42 123.1(3) . . ? C39 C38 C37 120.3(4) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C38 C39 C40 118.7(4) . . ? C38 C39 H39 120.7 . . ? C40 C39 H39 120.7 . . ? C41 C40 N9 117.3(4) . . ? C41 C40 C39 117.6(4) . . ? N9 C40 C39 125.1(4) . . ? N10 C41 C40 122.9(4) . . ? N10 C41 H41 118.5 . . ? C40 C41 H41 118.5 . . ? N11 C42 C43 121.0(4) . . ? N11 C42 C37 115.5(3) . . ? C43 C42 C37 123.5(4) . . ? C42 C43 C44 119.8(4) . . ? C42 C43 H43 120.1 . . ? C44 C43 H43 120.1 . . ? C45 C44 C43 119.2(4) . . ? C45 C44 H44 120.4 . . ? C43 C44 H44 120.4 . . ? C44 C45 C46 117.5(4) . . ? C44 C45 N12 124.4(4) . . ? C46 C45 N12 118.1(4) . . ? N11 C46 C45 123.2(4) . . ? N11 C46 H46 118.4 . . ? C45 C46 H46 118.4 . . ? O9 C47 O10 124.8(4) . . ? O9 C47 N9 126.1(4) . . ? O10 C47 N9 109.1(4) . . ? O10 C48 C50 104.9(4) . . ? O10 C48 C49 110.8(4) . . ? C50 C48 C49 113.8(5) . . ? O10 C48 H48 109.1 . . ? C50 C48 H48 109.1 . . ? C49 C48 H48 109.1 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O11 C51 O12 125.8(4) . . ? O11 C51 N12 126.2(4) . . ? O12 C51 N12 108.1(4) . . ? O12 C52 C54 106.6(5) . . ? O12 C52 C53 104.9(5) . . ? C54 C52 C53 112.0(6) . . ? O12 C52 H52 111.0 . . ? C54 C52 H52 111.0 . . ? C53 C52 H52 111.0 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O15' Cl1 O16 67.4(8) . . ? O15' Cl1 O14 136.9(7) . . ? O16 Cl1 O14 99.1(6) . . ? O15' Cl1 O13 111.3(7) . . ? O16 Cl1 O13 120.0(8) . . ? O14 Cl1 O13 110.7(4) . . ? O15' Cl1 O15 55.5(8) . . ? O16 Cl1 O15 117.0(9) . . ? O14 Cl1 O15 104.6(9) . . ? O13 Cl1 O15 104.4(6) . . ? O15 O15' Cl1 64.0(7) . . ? O15 O15' O16 114.7(10) . . ? Cl1 O15' O16 56.3(6) . . ? O15' O15 Cl1 60.5(6) . . ? Cl1 O16 O15' 56.3(5) . . ? O20 Cl2 O19 111.0(4) . . ? O20 Cl2 O18 107.2(5) . . ? O19 Cl2 O18 109.9(4) . . ? O20 Cl2 O17 108.0(3) . . ? O19 Cl2 O17 109.7(3) . . ? O18 Cl2 O17 110.9(3) . . ? C57 O21 C56 111.1(5) . . ? C56 C55 H55A 109.5 . . ? C56 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C56 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O21 C56 C55 108.5(5) . . ? O21 C56 H56A 110.0 . . ? C55 C56 H56A 110.0 . . ? O21 C56 H56B 110.0 . . ? C55 C56 H56B 110.0 . . ? H56A C56 H56B 108.4 . . ? O21 C57 C58 109.1(7) . . ? O21 C57 H57A 109.9 . . ? C58 C57 H57A 109.9 . . ? O21 C57 H57B 109.9 . . ? C58 C57 H57B 109.9 . . ? H57A C57 H57B 108.3 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C60 O22 C61 109.5(9) . . ? C60 C59 H59A 109.5 . . ? C60 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C60 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? O22 C60 C59 106.0(8) . . ? O22 C60 H60A 110.5 . . ? C59 C60 H60A 110.5 . . ? O22 C60 H60B 110.5 . . ? C59 C60 H60B 110.5 . . ? H60A C60 H60B 108.7 . . ? O22 C61 C62 107.2(7) . . ? O22 C61 H61A 110.3 . . ? C62 C61 H61A 110.3 . . ? O22 C61 H61B 110.3 . . ? C62 C61 H61B 110.3 . . ? H61A C61 H61B 108.5 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C63' O24' H24' 109.5 . . ? O24' C63' H63D 109.5 . . ? O24' C63' H63E 109.5 . . ? H63D C63' H63E 109.5 . . ? O24' C63' H63F 109.5 . . ? H63D C63' H63F 109.5 . . ? H63E C63' H63F 109.5 . . ? C64' O25' H25' 109.5 . . ? O25' C64' H64D 109.5 . . ? O25' C64' H64E 109.5 . . ? H64D C64' H64E 109.5 . . ? O25' C64' H64F 109.5 . . ? H64D C64' H64F 109.5 . . ? H64E C64' H64F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.893 _refine_diff_density_min -0.776 _refine_diff_density_rms 0.086 ########### data_L1CuClO4 _database_code_depnum_ccdc_archive 'CCDC 800537' #TrackingRef '- bipy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H54 Cl2 Cu N8 O19 S3' _chemical_formula_weight 1157.51 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 9.5168(11) _cell_length_b 15.5544(19) _cell_length_c 18.715(2) _cell_angle_alpha 75.716(2) _cell_angle_beta 89.987(2) _cell_angle_gamma 79.958(2) _cell_volume 2641.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1202 _exptl_absorpt_coefficient_mu 0.710 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8424 _exptl_absorpt_correction_T_max 0.8710 _exptl_absorpt_process_details SADABS _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 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17772 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9137 _reflns_number_gt 6796 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 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^)+(0.0798P)^2^+2.5263P] 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 9137 _refine_ls_number_parameters 691 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0741 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1562 _refine_ls_wR_factor_gt 0.1396 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.039 _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 Cu1 Cu -0.02095(5) 0.72011(3) 0.51354(2) 0.04097(15) Uani 1 1 d . A 1 C1 C 0.1124(3) 0.8693(2) 0.52278(18) 0.0378(7) Uani 1 1 d . A 1 C2 C 0.1750(4) 0.9446(2) 0.5032(2) 0.0463(9) Uani 1 1 d . A 1 H2 H 0.2139 0.9657 0.5397 0.056 Uiso 1 1 calc R A 1 C3 C 0.1807(4) 0.9891(3) 0.4301(2) 0.0490(9) Uani 1 1 d . A 1 H3 H 0.2235 1.0398 0.4171 0.059 Uiso 1 1 calc R A 1 C4 C 0.1217(4) 0.9572(2) 0.3762(2) 0.0448(8) Uani 1 1 d . A 1 C5 C 0.0575(4) 0.8815(2) 0.39937(19) 0.0432(8) Uani 1 1 d . A 1 H5 H 0.0157 0.8601 0.3639 0.052 Uiso 1 1 calc R A 1 C6 C 0.1050(4) 0.8153(2) 0.59903(19) 0.0388(8) Uani 1 1 d . A 1 C7 C 0.1608(4) 0.8321(3) 0.6618(2) 0.0508(9) Uani 1 1 d . A 1 H7 H 0.2049 0.8819 0.6579 0.061 Uiso 1 1 calc R A 1 C8 C 0.1508(4) 0.7749(3) 0.7299(2) 0.0549(10) Uani 1 1 d . A 1 H8 H 0.1895 0.7854 0.7719 0.066 Uiso 1 1 calc R A 1 C9 C 0.0829(4) 0.7017(3) 0.73585(19) 0.0456(9) Uani 1 1 d . A 1 C10 C 0.0275(4) 0.6887(2) 0.67172(19) 0.0445(8) Uani 1 1 d . A 1 H10 H -0.0194 0.6404 0.6746 0.053 Uiso 1 1 calc R A 1 C11 C 0.1652(5) 1.0735(3) 0.2682(3) 0.0611(11) Uani 1 1 d . A 1 C12 C 0.1975(10) 1.1666(5) 0.1511(4) 0.136(3) Uani 1 1 d DU A 1 H12A H 0.1208 1.1977 0.1149 0.163 Uiso 1 1 calc R A 1 H12B H 0.2085 1.2056 0.1832 0.163 Uiso 1 1 calc R A 1 C13 C 0.3210(13) 1.1515(7) 0.1157(7) 0.238(6) Uani 1 1 d DU A 1 H13A H 0.2995 1.1427 0.0681 0.357 Uiso 1 1 calc R A 1 H13B H 0.3825 1.0986 0.1444 0.357 Uiso 1 1 calc R A 1 H13C H 0.3681 1.2025 0.1096 0.357 Uiso 1 1 calc R A 1 C14 C 0.0232(6) 0.5658(3) 0.8196(2) 0.0696(13) Uani 1 1 d . A 1 C15 C -0.0110(14) 0.4404(7) 0.9177(4) 0.185(5) Uani 1 1 d . A 1 H15A H -0.0932 0.4478 0.9477 0.222 Uiso 1 1 calc R A 1 H15B H -0.0396 0.4200 0.8758 0.222 Uiso 1 1 calc R A 1 C16 C 0.0998(13) 0.3759(6) 0.9595(7) 0.221(7) Uani 1 1 d . A 1 H16A H 0.1765 0.3634 0.9281 0.332 Uiso 1 1 calc R A 1 H16B H 0.0646 0.3214 0.9808 0.332 Uiso 1 1 calc R A 1 H16C H 0.1339 0.3988 0.9981 0.332 Uiso 1 1 calc R A 1 C17 C 0.0035(4) 0.6142(2) 0.40919(18) 0.0389(8) Uani 1 1 d . A 1 C18 C -0.0330(4) 0.5860(3) 0.3484(2) 0.0482(9) Uani 1 1 d . A 1 H18 H 0.0190 0.5335 0.3396 0.058 Uiso 1 1 calc R A 1 C19 C -0.1449(4) 0.6342(3) 0.3009(2) 0.0515(9) Uani 1 1 d . A 1 H19 H -0.1683 0.6147 0.2600 0.062 Uiso 1 1 calc R A 1 C20 C -0.2229(4) 0.7122(3) 0.31452(19) 0.0456(9) Uani 1 1 d . A 1 C21 C -0.1833(4) 0.7365(2) 0.37679(19) 0.0446(8) Uani 1 1 d . A 1 H21 H -0.2353 0.7879 0.3874 0.053 Uiso 1 1 calc R A 1 C22 C 0.1223(4) 0.5678(2) 0.46309(18) 0.0379(7) Uani 1 1 d . A 1 C23 C 0.2178(4) 0.4923(2) 0.4576(2) 0.0468(9) Uani 1 1 d . A 1 H23 H 0.2086 0.4674 0.4179 0.056 Uiso 1 1 calc R A 1 C24 C 0.3264(4) 0.4537(3) 0.5102(2) 0.0497(9) Uani 1 1 d . A 1 H24 H 0.3898 0.4023 0.5066 0.060 Uiso 1 1 calc R A 1 C25 C 0.3400(4) 0.4921(2) 0.5685(2) 0.0437(8) Uani 1 1 d . A 1 C26 C 0.2410(4) 0.5688(2) 0.57055(19) 0.0427(8) Uani 1 1 d . A 1 H26 H 0.2500 0.5961 0.6088 0.051 Uiso 1 1 calc R A 1 C27 C -0.3764(5) 0.7644(3) 0.2016(2) 0.0656(12) Uani 1 1 d . A 1 C28 C -0.5356(10) 0.8365(5) 0.0991(4) 0.146(3) Uani 1 1 d DU A 1 H28A H -0.4561 0.8381 0.0667 0.175 Uiso 1 1 calc R A 1 H28B H -0.5780 0.7845 0.0977 0.175 Uiso 1 1 calc R A 1 C29 C -0.6356(13) 0.9145(7) 0.0765(5) 0.204(4) Uani 1 1 d DU A 1 H29A H -0.5884 0.9657 0.0667 0.306 Uiso 1 1 calc R A 1 H29B H -0.7020 0.9187 0.1146 0.306 Uiso 1 1 calc R A 1 H29C H -0.6860 0.9133 0.0324 0.306 Uiso 1 1 calc R A 1 C30 C 0.5455(4) 0.3829(3) 0.6362(2) 0.0544(10) Uani 1 1 d . A 1 C31 C 0.7347(5) 0.2946(3) 0.7200(3) 0.0747(14) Uani 1 1 d . A 1 H31A H 0.7992 0.2924 0.6801 0.090 Uiso 1 1 calc R A 1 H31B H 0.6957 0.2394 0.7321 0.090 Uiso 1 1 calc R A 1 C32 C 0.8123(6) 0.3052(5) 0.7865(3) 0.106(2) Uani 1 1 d . A 1 H32A H 0.8373 0.3641 0.7760 0.159 Uiso 1 1 calc R A 1 H32B H 0.8976 0.2603 0.7981 0.159 Uiso 1 1 calc R A 1 H32C H 0.7516 0.2981 0.8277 0.159 Uiso 1 1 calc R A 1 C33 C -0.4890(5) 0.7977(4) 0.5210(3) 0.0921(17) Uani 1 1 d . B 1 H33A H -0.4753 0.8104 0.4689 0.138 Uiso 1 1 calc R B 1 H33B H -0.5581 0.8453 0.5316 0.138 Uiso 1 1 calc R B 1 H33C H -0.5225 0.7416 0.5368 0.138 Uiso 1 1 calc R B 1 C34 C -0.37263(16) 0.7443(3) 0.65983(5) 0.0780(14) Uani 1 1 d . B 1 H34A H -0.4142 0.6920 0.6608 0.117 Uiso 1 1 calc R B 1 H34B H -0.4409 0.7885 0.6753 0.117 Uiso 1 1 calc R B 1 H34C H -0.2893 0.7274 0.6926 0.117 Uiso 1 1 calc R B 1 Cl1 Cl 0.58134(9) 0.98842(6) 0.34552(5) 0.0725(3) Uani 1 1 d R B 1 Cl2 Cl 0.26846(10) 0.71765(6) 0.96577(5) 0.1056(5) Uani 1 1 d R B 1 N1 N 0.05360(11) 0.83847(6) 0.47009(5) 0.0385(6) Uani 1 1 d R A 1 N2 N 0.03977(15) 0.74398(6) 0.60564(5) 0.0399(7) Uani 1 1 d R A 1 N3 N 0.12222(12) 0.99411(6) 0.30053(5) 0.0574(9) Uani 1 1 d R A 1 H3A H 0.0932 0.9646 0.2719 0.069 Uiso 1 1 calc R B 1 N4 N 0.0718(4) 0.6448(2) 0.80552(17) 0.0600(9) Uani 1 1 d . A 1 H4A H 0.0984 0.6616 0.8430 0.072 Uiso 1 1 calc R A 1 N5 N -0.0737(3) 0.68926(19) 0.42241(15) 0.0393(6) Uani 1 1 d . A 1 N6 N 0.1342(3) 0.60467(18) 0.52038(15) 0.0387(6) Uani 1 1 d . A 1 N7 N -0.3393(4) 0.7671(2) 0.27099(17) 0.0560(8) Uani 1 1 d . A 1 H7A H -0.3921 0.8059 0.2897 0.067 Uiso 1 1 calc R A 1 N8 N 0.4437(3) 0.4593(2) 0.62633(18) 0.0517(8) Uani 1 1 d . A 1 H8A H 0.4434 0.4900 0.6588 0.062 Uiso 1 1 calc R A 1 O1 O 0.1982(4) 1.1265(2) 0.29875(18) 0.0712(8) Uani 1 1 d . A 1 O2 O 0.1589(5) 1.0841(2) 0.19456(18) 0.0915(12) Uani 1 1 d . A 1 O3 O -0.0249(5) 0.5344(2) 0.77484(16) 0.0919(12) Uani 1 1 d . A 1 O4 O 0.0378(6) 0.5274(3) 0.89143(18) 0.1230(18) Uani 1 1 d . A 1 O5 O -0.3199(5) 0.7118(3) 0.1694(2) 0.1078(15) Uani 1 1 d . A 1 O6 O -0.4857(4) 0.8302(2) 0.17491(17) 0.0825(10) Uani 1 1 d . A 1 O7 O 0.5647(3) 0.3335(2) 0.59576(19) 0.0743(9) Uani 1 1 d . A 1 O8 O 0.6210(3) 0.3723(2) 0.69862(17) 0.0696(8) Uani 1 1 d . A 1 O9 O -0.2249(3) 0.71232(17) 0.54829(15) 0.0511(6) Uani 1 1 d . A 1 O10 O 0.5098(4) 0.9232(3) 0.3292(3) 0.1132(15) Uani 1 1 d . B 1 O11 O 0.7264(4) 0.9534(3) 0.3612(3) 0.1284(19) Uani 1 1 d . B 1 O12 O 0.5189(5) 1.0213(4) 0.4037(3) 0.1282(17) Uani 1 1 d . B 1 O13 O 0.5691(7) 1.0670(4) 0.2848(3) 0.157(2) Uani 1 1 d . B 1 O14 O 0.3793(9) 0.7552(7) 0.9422(6) 0.271(5) Uani 1 1 d . B 1 O15 O 0.1742(9) 0.7237(6) 0.9141(3) 0.205(3) Uani 1 1 d . B 1 O16 O 0.3073(13) 0.6267(7) 0.9946(7) 0.322(7) Uani 1 1 d . B 1 O17 O 0.2105(12) 0.7542(10) 1.0176(5) 0.303(7) Uani 1 1 d . B 1 S2 S 0.8619(4) 0.9162(3) 0.1711(2) 0.0780(10) Uani 0.530(5) 1 d P C 1 C35 C 0.835(3) 1.0326(13) 0.1652(9) 0.143(9) Uani 0.530(5) 1 d P C 1 H35A H 0.8089 1.0429 0.2124 0.215 Uiso 0.530(5) 1 calc PR C 1 H35B H 0.7590 1.0633 0.1292 0.215 Uiso 0.530(5) 1 calc PR C 1 H35C H 0.9207 1.0551 0.1509 0.215 Uiso 0.530(5) 1 calc PR C 1 C36 C 0.956(2) 0.9283(17) 0.0816(8) 0.151(9) Uani 0.530(5) 1 d P C 1 H36A H 0.9537 0.9911 0.0589 0.226 Uiso 0.530(5) 1 calc PR C 1 H36B H 0.9095 0.9021 0.0491 0.226 Uiso 0.530(5) 1 calc PR C 1 H36C H 1.0538 0.8980 0.0913 0.226 Uiso 0.530(5) 1 calc PR C 1 O18 O 0.9885(5) 0.8941(3) 0.2221(2) 0.1122(15) Uani 1 1 d . C 1 S2' S 0.9313(17) 0.9491(8) 0.1426(7) 0.288(8) Uani 0.470(5) 1 d P C 2 C35' C 0.781(3) 1.0192(16) 0.1458(12) 0.170(14) Uani 0.470(5) 1 d P C 2 H35D H 0.7931 1.0798 0.1234 0.255 Uiso 0.470(5) 1 calc PR C 2 H35E H 0.7570 1.0142 0.1963 0.255 Uiso 0.470(5) 1 calc PR C 2 H35F H 0.7058 1.0043 0.1196 0.255 Uiso 0.470(5) 1 calc PR C 2 C36' C 0.8905(13) 0.8877(12) 0.0911(7) 0.144(10) Uani 0.470(5) 1 d P C 2 H36D H 0.8238 0.8516 0.1154 0.215 Uiso 0.470(5) 1 calc PR C 2 H36E H 0.9752 0.8490 0.0821 0.215 Uiso 0.470(5) 1 calc PR C 2 H36F H 0.8480 0.9257 0.0450 0.215 Uiso 0.470(5) 1 calc PR C 2 S1 S -0.32372(11) 0.79028(7) 0.56883(6) 0.0539(3) Uani 1 1 d R . . S3 S 0.4260(4) 0.5734(2) 0.80245(16) 0.0904(13) Uani 0.530(5) 1 d P C 1 C37 C 0.607(3) 0.572(2) 0.8370(15) 0.204(18) Uani 0.530(5) 1 d P C 1 H37A H 0.6739 0.5294 0.8189 0.306 Uiso 0.530(5) 1 calc PR C 1 H37B H 0.6112 0.5547 0.8900 0.306 Uiso 0.530(5) 1 calc PR C 1 H37C H 0.6307 0.6310 0.8203 0.306 Uiso 0.530(5) 1 calc PR C 1 C38 C 0.418(3) 0.4604(17) 0.8644(15) 0.147(8) Uani 0.530(5) 1 d P C 1 H38A H 0.3268 0.4445 0.8568 0.220 Uiso 0.530(5) 1 calc PR C 1 H38B H 0.4293 0.4625 0.9149 0.220 Uiso 0.530(5) 1 calc PR C 1 H38C H 0.4926 0.4162 0.8535 0.220 Uiso 0.530(5) 1 calc PR C 1 O19 O 0.4342(5) 0.5675(3) 0.7276(2) 0.1099(14) Uani 1 1 d . C 1 S3' S 0.5351(5) 0.5168(4) 0.8014(2) 0.123(2) Uani 0.470(5) 1 d P C 2 C37' C 0.544(4) 0.6205(18) 0.8312(12) 0.146(12) Uani 0.470(5) 1 d P C 2 H37D H 0.4868 0.6712 0.7977 0.219 Uiso 0.470(5) 1 calc PR C 2 H37E H 0.6417 0.6294 0.8315 0.219 Uiso 0.470(5) 1 calc PR C 2 H37F H 0.5095 0.6147 0.8800 0.219 Uiso 0.470(5) 1 calc PR C 2 C38' C 0.468(4) 0.475(2) 0.848(2) 0.190(17) Uani 0.470(5) 1 d P C 2 H38D H 0.5041 0.4751 0.8959 0.285 Uiso 0.470(5) 1 calc PR C 2 H38E H 0.4773 0.4146 0.8434 0.285 Uiso 0.470(5) 1 calc PR C 2 H38F H 0.3692 0.5036 0.8416 0.285 Uiso 0.470(5) 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0541(3) 0.0361(2) 0.0353(2) -0.01426(17) -0.00728(18) -0.00754(19) C1 0.0345(17) 0.0366(18) 0.0433(19) -0.0153(15) -0.0035(14) -0.0017(14) C2 0.043(2) 0.044(2) 0.054(2) -0.0174(17) -0.0081(16) -0.0093(16) C3 0.048(2) 0.042(2) 0.060(2) -0.0153(18) -0.0029(17) -0.0147(17) C4 0.045(2) 0.0380(19) 0.049(2) -0.0075(16) 0.0005(16) -0.0067(16) C5 0.052(2) 0.0356(19) 0.045(2) -0.0134(15) -0.0070(16) -0.0094(16) C6 0.0391(18) 0.0353(18) 0.0443(19) -0.0167(15) -0.0042(14) -0.0028(15) C7 0.061(2) 0.052(2) 0.047(2) -0.0205(18) -0.0060(17) -0.0184(19) C8 0.069(3) 0.059(3) 0.043(2) -0.0204(18) -0.0109(18) -0.016(2) C9 0.056(2) 0.044(2) 0.0364(19) -0.0155(15) -0.0053(16) -0.0023(17) C10 0.058(2) 0.0388(19) 0.0404(19) -0.0159(16) -0.0026(16) -0.0114(17) C11 0.068(3) 0.049(3) 0.061(3) -0.002(2) 0.007(2) -0.012(2) C12 0.230(9) 0.085(4) 0.094(5) -0.003(4) 0.062(5) -0.059(5) C13 0.273(12) 0.153(9) 0.272(12) -0.009(8) 0.161(10) -0.061(9) C14 0.110(4) 0.063(3) 0.042(2) -0.015(2) -0.002(2) -0.030(3) C15 0.359(15) 0.155(8) 0.062(4) 0.024(4) -0.042(6) -0.176(10) C16 0.258(13) 0.095(6) 0.274(14) 0.004(8) 0.156(12) -0.002(7) C17 0.049(2) 0.0339(18) 0.0388(18) -0.0135(14) 0.0057(15) -0.0150(15) C18 0.058(2) 0.044(2) 0.048(2) -0.0225(17) 0.0001(17) -0.0092(18) C19 0.070(3) 0.052(2) 0.042(2) -0.0227(17) -0.0010(18) -0.020(2) C20 0.056(2) 0.047(2) 0.0376(19) -0.0115(16) -0.0011(16) -0.0195(17) C21 0.056(2) 0.041(2) 0.0382(18) -0.0150(15) -0.0058(16) -0.0073(17) C22 0.0444(19) 0.0347(18) 0.0395(18) -0.0127(14) 0.0062(14) -0.0153(15) C23 0.056(2) 0.041(2) 0.049(2) -0.0202(16) 0.0034(17) -0.0097(17) C24 0.052(2) 0.038(2) 0.060(2) -0.0181(17) 0.0065(18) -0.0035(17) C25 0.043(2) 0.041(2) 0.047(2) -0.0096(16) 0.0037(16) -0.0090(16) C26 0.048(2) 0.0388(19) 0.0419(19) -0.0130(15) -0.0019(16) -0.0059(16) C27 0.082(3) 0.066(3) 0.050(2) -0.012(2) -0.017(2) -0.020(3) C28 0.206(8) 0.117(5) 0.099(4) -0.028(4) -0.110(5) 0.013(5) C29 0.280(10) 0.158(7) 0.146(6) -0.022(6) -0.123(6) 0.016(7) C30 0.049(2) 0.046(2) 0.061(3) -0.005(2) 0.0046(19) -0.0033(18) C31 0.056(3) 0.064(3) 0.082(3) 0.007(2) 0.002(2) 0.015(2) C32 0.081(4) 0.119(5) 0.085(4) 0.001(3) -0.016(3) 0.030(4) C33 0.059(3) 0.103(4) 0.115(4) -0.044(4) -0.007(3) 0.008(3) C34 0.092(4) 0.076(3) 0.076(3) -0.030(3) 0.028(3) -0.027(3) Cl1 0.0613(7) 0.0641(7) 0.1017(9) -0.0397(7) -0.0064(6) -0.0095(5) Cl2 0.1336(14) 0.1299(14) 0.0646(8) -0.0213(9) -0.0150(8) -0.0584(12) N1 0.0440(16) 0.0343(15) 0.0388(15) -0.0129(12) -0.0066(12) -0.0059(12) N2 0.0481(17) 0.0356(15) 0.0375(15) -0.0137(12) -0.0063(12) -0.0052(13) N3 0.079(2) 0.049(2) 0.0451(18) -0.0069(15) -0.0008(16) -0.0229(17) N4 0.091(3) 0.057(2) 0.0374(17) -0.0169(15) -0.0068(16) -0.0206(19) N5 0.0489(17) 0.0353(15) 0.0360(15) -0.0121(12) -0.0017(12) -0.0094(13) N6 0.0475(17) 0.0330(15) 0.0379(15) -0.0112(12) 0.0005(12) -0.0098(13) N7 0.066(2) 0.060(2) 0.0426(17) -0.0171(15) -0.0142(15) -0.0065(17) N8 0.0511(19) 0.0457(18) 0.0553(19) -0.0150(15) -0.0049(15) 0.0029(15) O1 0.086(2) 0.0512(18) 0.078(2) -0.0090(16) 0.0024(17) -0.0261(16) O2 0.148(3) 0.069(2) 0.057(2) -0.0010(17) 0.018(2) -0.041(2) O3 0.170(4) 0.076(2) 0.0444(17) -0.0148(16) -0.004(2) -0.062(2) O4 0.236(5) 0.105(3) 0.0430(19) -0.0006(19) -0.017(2) -0.099(3) O5 0.147(4) 0.111(3) 0.064(2) -0.047(2) -0.038(2) 0.017(3) O6 0.096(2) 0.084(2) 0.0627(19) -0.0165(17) -0.0393(18) -0.005(2) O7 0.076(2) 0.0581(19) 0.084(2) -0.0248(17) -0.0083(17) 0.0108(16) O8 0.0614(18) 0.0636(19) 0.0688(19) -0.0078(15) -0.0121(15) 0.0159(15) O9 0.0486(15) 0.0485(15) 0.0648(17) -0.0293(13) 0.0024(12) -0.0097(12) O10 0.093(3) 0.117(3) 0.165(4) -0.090(3) -0.004(3) -0.036(2) O11 0.067(2) 0.085(3) 0.248(6) -0.084(3) -0.031(3) 0.007(2) O12 0.114(3) 0.146(4) 0.156(4) -0.106(4) 0.007(3) -0.009(3) O13 0.164(5) 0.113(4) 0.163(5) 0.014(4) -0.006(4) -0.006(4) O14 0.196(8) 0.280(10) 0.397(14) -0.125(10) 0.123(9) -0.149(8) O15 0.265(8) 0.266(9) 0.118(4) -0.094(5) -0.068(5) -0.075(7) O16 0.306(13) 0.212(10) 0.343(14) 0.114(10) -0.076(10) -0.030(9) O17 0.328(12) 0.51(2) 0.197(8) -0.255(11) 0.070(8) -0.183(13) S2 0.0930(19) 0.0765(19) 0.0665(17) -0.0001(13) -0.0026(14) -0.0463(16) C35 0.27(3) 0.111(12) 0.080(10) -0.036(9) 0.009(13) -0.091(15) C36 0.137(15) 0.24(2) 0.062(8) -0.049(12) -0.020(9) 0.031(16) O18 0.166(4) 0.087(3) 0.085(3) -0.031(2) -0.044(3) -0.014(3) S2' 0.402(17) 0.218(10) 0.218(10) -0.136(9) -0.202(11) 0.133(11) C35' 0.19(2) 0.17(2) 0.119(15) -0.075(14) -0.072(14) 0.11(2) C36' 0.141(19) 0.19(2) 0.116(16) -0.060(15) -0.045(13) -0.039(15) S1 0.0577(6) 0.0452(5) 0.0654(6) -0.0258(5) 0.0069(5) -0.0097(5) S3 0.096(2) 0.095(2) 0.0800(19) -0.0302(15) -0.0104(14) -0.0049(17) C37 0.17(2) 0.28(4) 0.145(17) 0.05(2) -0.072(16) -0.14(3) C38 0.16(2) 0.104(14) 0.158(15) 0.048(11) -0.030(13) -0.099(12) O19 0.142(4) 0.108(3) 0.084(3) -0.044(2) -0.020(2) -0.003(3) S3' 0.103(3) 0.170(5) 0.101(3) -0.075(3) -0.021(2) 0.019(3) C37' 0.25(4) 0.15(2) 0.070(11) -0.046(13) -0.015(14) -0.08(2) C38' 0.17(3) 0.101(15) 0.28(4) 0.049(19) -0.06(2) -0.116(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 1.9580(12) . ? Cu1 N5 1.970(3) . ? Cu1 O9 2.061(3) . ? Cu1 N1 2.0665(11) . ? Cu1 N6 2.094(3) . ? C1 N1 1.358(3) . ? C1 C2 1.375(5) . ? C1 C6 1.475(5) . ? C2 C3 1.378(5) . ? C3 C4 1.388(5) . ? C4 N3 1.390(4) . ? C4 C5 1.396(5) . ? C5 N1 1.331(4) . ? C6 N2 1.343(4) . ? C6 C7 1.390(5) . ? C7 C8 1.377(5) . ? C8 C9 1.386(6) . ? C9 C10 1.384(5) . ? C9 N4 1.399(5) . ? C10 N2 1.339(4) . ? C11 O1 1.195(5) . ? C11 O2 1.347(5) . ? C11 N3 1.366(4) . ? C12 C13 1.363(9) . ? C12 O2 1.446(7) . ? C14 O3 1.196(5) . ? C14 O4 1.326(5) . ? C14 N4 1.353(6) . ? C15 C16 1.405(13) . ? C15 O4 1.477(8) . ? C17 N5 1.344(4) . ? C17 C18 1.381(5) . ? C17 C22 1.474(5) . ? C18 C19 1.371(5) . ? C19 C20 1.389(5) . ? C20 C21 1.382(5) . ? C20 N7 1.395(5) . ? C21 N5 1.334(4) . ? C22 N6 1.348(4) . ? C22 C23 1.380(5) . ? C23 C24 1.375(5) . ? C24 C25 1.383(5) . ? C25 C26 1.394(5) . ? C25 N8 1.400(5) . ? C26 N6 1.330(4) . ? C27 O5 1.189(6) . ? C27 O6 1.324(6) . ? C27 N7 1.358(5) . ? C28 C29 1.379(10) . ? C28 O6 1.471(6) . ? C30 O7 1.198(5) . ? C30 O8 1.332(5) . ? C30 N8 1.369(5) . ? C31 O8 1.449(5) . ? C31 C32 1.505(8) . ? C33 S1 1.782(5) . ? C34 S1 1.7729(14) . ? Cl1 O11 1.395(4) . ? Cl1 O12 1.403(4) . ? Cl1 O10 1.407(4) . ? Cl1 O13 1.436(5) . ? Cl2 O15 1.294(5) . ? Cl2 O17 1.316(8) . ? Cl2 O14 1.317(7) . ? Cl2 O16 1.367(10) . ? O9 S1 1.528(3) . ? S2 O18 1.475(6) . ? S2 C35 1.759(19) . ? S2 C36 1.884(17) . ? S2' C36' 1.605(9) . ? S2' C35' 1.65(2) . ? S3 O19 1.428(5) . ? S3 C37 1.83(3) . ? S3 C38 1.866(19) . ? S3' C38' 1.20(3) . ? S3' C37' 1.85(2) . ? 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 N2 Cu1 N5 176.56(9) . . ? N2 Cu1 O9 92.50(8) . . ? N5 Cu1 O9 89.00(11) . . ? N2 Cu1 N1 81.0 . . ? N5 Cu1 N1 100.64(9) . . ? O9 Cu1 N1 125.07(8) . . ? N2 Cu1 N6 96.01(8) . . ? N5 Cu1 N6 80.58(11) . . ? O9 Cu1 N6 121.91(11) . . ? N1 Cu1 N6 113.02(8) . . ? N1 C1 C2 120.2(3) . . ? N1 C1 C6 114.8(3) . . ? C2 C1 C6 124.9(3) . . ? C1 C2 C3 120.8(3) . . ? C2 C3 C4 119.1(3) . . ? C3 C4 N3 125.3(3) . . ? C3 C4 C5 117.6(3) . . ? N3 C4 C5 117.1(3) . . ? N1 C5 C4 122.9(3) . . ? N2 C6 C7 119.5(3) . . ? N2 C6 C1 115.1(3) . . ? C7 C6 C1 125.4(3) . . ? C8 C7 C6 119.9(4) . . ? C7 C8 C9 119.9(3) . . ? C10 C9 C8 117.9(3) . . ? C10 C9 N4 122.8(4) . . ? C8 C9 N4 119.4(3) . . ? N2 C10 C9 121.7(3) . . ? O1 C11 O2 125.2(4) . . ? O1 C11 N3 126.8(4) . . ? O2 C11 N3 108.0(4) . . ? C13 C12 O2 112.5(7) . . ? O3 C14 O4 124.6(4) . . ? O3 C14 N4 126.0(4) . . ? O4 C14 N4 109.4(4) . . ? C16 C15 O4 109.7(9) . . ? N5 C17 C18 119.3(3) . . ? N5 C17 C22 115.5(3) . . ? C18 C17 C22 125.2(3) . . ? C19 C18 C17 121.0(3) . . ? C18 C19 C20 119.3(3) . . ? C21 C20 C19 117.2(3) . . ? C21 C20 N7 117.6(3) . . ? C19 C20 N7 125.1(3) . . ? N5 C21 C20 122.9(3) . . ? N6 C22 C23 120.3(3) . . ? N6 C22 C17 115.3(3) . . ? C23 C22 C17 124.5(3) . . ? C24 C23 C22 120.6(3) . . ? C23 C24 C25 119.2(3) . . ? C24 C25 C26 117.4(3) . . ? C24 C25 N8 125.3(3) . . ? C26 C25 N8 117.2(3) . . ? N6 C26 C25 123.1(3) . . ? O5 C27 O6 124.9(4) . . ? O5 C27 N7 125.7(5) . . ? O6 C27 N7 109.4(4) . . ? C29 C28 O6 107.8(6) . . ? O7 C30 O8 125.2(4) . . ? O7 C30 N8 126.3(4) . . ? O8 C30 N8 108.6(4) . . ? O8 C31 C32 106.5(4) . . ? O11 Cl1 O12 111.3(3) . . ? O11 Cl1 O10 110.5(2) . . ? O12 Cl1 O10 111.2(3) . . ? O11 Cl1 O13 107.8(4) . . ? O12 Cl1 O13 104.2(4) . . ? O10 Cl1 O13 111.6(4) . . ? O15 Cl2 O17 110.6(6) . . ? O15 Cl2 O14 113.8(6) . . ? O17 Cl2 O14 108.5(7) . . ? O15 Cl2 O16 103.4(7) . . ? O17 Cl2 O16 108.6(8) . . ? O14 Cl2 O16 111.7(7) . . ? C5 N1 C1 119.5(2) . . ? C5 N1 Cu1 127.98(16) . . ? C1 N1 Cu1 112.41(16) . . ? C10 N2 C6 121.1(2) . . ? C10 N2 Cu1 122.27(17) . . ? C6 N2 Cu1 116.42(15) . . ? C11 N3 C4 125.1(3) . . ? C14 N4 C9 126.3(3) . . ? C21 N5 C17 120.3(3) . . ? C21 N5 Cu1 123.3(2) . . ? C17 N5 Cu1 116.3(2) . . ? C26 N6 C22 119.3(3) . . ? C26 N6 Cu1 128.4(2) . . ? C22 N6 Cu1 112.2(2) . . ? C27 N7 C20 125.7(4) . . ? C30 N8 C25 126.1(4) . . ? C11 O2 C12 115.5(5) . . ? C14 O4 C15 117.3(4) . . ? C27 O6 C28 115.3(4) . . ? C30 O8 C31 117.7(4) . . ? S1 O9 Cu1 123.12(15) . . ? O18 S2 C35 94.6(7) . . ? O18 S2 C36 98.5(6) . . ? C35 S2 C36 93.2(10) . . ? C36' S2' C35' 104.3(13) . . ? O9 S1 C34 104.64(17) . . ? O9 S1 C33 104.2(2) . . ? C34 S1 C33 98.8(2) . . ? O19 S3 C37 107.9(11) . . ? O19 S3 C38 110.0(10) . . ? C37 S3 C38 92.7(11) . . ? C38' S3' C37' 104(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3A O18 0.86 1.99 2.830(4) 166.3 1_455 N7 H7A O10 0.86 2.19 3.039(5) 167.2 1_455 N4 H4A O15 0.86 2.03 2.871(6) 167.3 . N8 H8A O19 0.86 1.96 2.819(5) 175.8 . _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.670 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.066 #######END