# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_email M.J.Hardie@leeds.ac.uk _publ_contact_author_name 'Michaele Hardie' loop_ _publ_author_name 'Michaele Hardie' 'Marc Little' 'Tanya Ronson' data_3ph4py_new _database_code_depnum_ccdc_archive 'CCDC 822478' #TrackingRef '- 3ph4py_new.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(+-)-2,7,12-trimethoxy-3,8,13-tris[3- (4-pyridyl)benzoyl]-10,15-dihydro-5H- tribenzo[a,d,g]cyclononane] chloroform clathrate ; _chemical_name_common ; ((+-)-2,7,12-trimethoxy-3,8,13-tris(3-(4-pyridyl)benzoyl)- 10,15-dihydro-5H-tribenzo(a,d,g)cyclononane) chloroform clathrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C61.50 H46.50 Cl4.50 N3 O9' _chemical_formula_weight 1131.04 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' _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 12.4628(11) _cell_length_b 14.9274(14) _cell_length_c 15.6631(16) _cell_angle_alpha 88.510(6) _cell_angle_beta 73.191(6) _cell_angle_gamma 84.999(6) _cell_volume 2778.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1170 _exptl_absorpt_coefficient_mu 0.298 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9428 _exptl_absorpt_correction_T_max 0.9823 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 X8 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32601 _diffrn_reflns_av_R_equivalents 0.0872 _diffrn_reflns_av_sigmaI/netI 0.2208 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 23.00 _reflns_number_total 7699 _reflns_number_gt 2992 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour)' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Two methyl CH3 and one pyridyl C5H4N groups were each disordered across two positions. SIMU or SADI restraints were applied to displacement parameters for these atoms and the disordered pyridyl rings were restrained to be FLAT. The following restraints were used: SADI c55 c59 c55' c59' SADI c58 c59 c58' c59' SADI c58 n3 c58' n3' SADI n3 c57 n3' c57' SADI c56 c57 c56' c57' SADI c55 c56 c55' c56' SIMU c34 c34' SIMU c47 c47' SADI o6 c47 o6 c47' SADI c54 c55 c54 c55' SIMU n3 n3' SIMU c58 c58' c59 c59' c55 c55' c56 c56' c57 c57' FLAT c55 c56 c57 c58 c59 n3 FLAT c55' c56' c57' c58' c59' n3' ; _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^)+(0.1885P)^2^+15.1391P] 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 7699 _refine_ls_number_parameters 695 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.2739 _refine_ls_R_factor_gt 0.1252 _refine_ls_wR_factor_ref 0.4363 _refine_ls_wR_factor_gt 0.3095 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.008 _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 O1 O 1.1675(6) -1.5688(5) -0.0474(6) 0.067(3) Uani 1 1 d . A . O2 O 1.2929(6) -1.6895(5) -0.0933(6) 0.071(3) Uani 1 1 d . A . O3 O 1.2723(8) -1.4912(6) -0.2051(7) 0.086(3) Uani 1 1 d . . . O4 O 1.0697(6) -1.1539(5) 0.3373(6) 0.057(2) Uani 1 1 d . B . O5 O 1.1028(8) -1.2157(7) 0.4629(6) 0.080(3) Uani 1 1 d . B . O6 O 1.0121(7) -1.3218(6) 0.3289(7) 0.098(4) Uani 1 1 d D . . O7 O 1.3885(6) -1.0382(5) -0.1966(5) 0.054(2) Uani 1 1 d . A . O8 O 1.5599(7) -0.9838(5) -0.2243(5) 0.061(2) Uani 1 1 d . A . O9 O 1.3483(6) -0.9496(5) -0.0458(5) 0.051(2) Uani 1 1 d . . . N1 N 1.0514(9) -2.1246(7) -0.1639(7) 0.063(3) Uani 1 1 d . A . N2 N 0.5987(11) -0.8124(10) 0.3560(10) 0.099(4) Uani 1 1 d . B . C1 C 1.5020(8) -1.3239(7) -0.0624(7) 0.047(3) Uani 1 1 d . A . H1A H 1.5575 -1.3311 -0.1220 0.057 Uiso 1 1 calc R . . H1B H 1.5425 -1.3386 -0.0173 0.057 Uiso 1 1 calc R . . C2 C 1.4129(8) -1.3917(7) -0.0535(10) 0.053(3) Uani 1 1 d . A . C3 C 1.3843(9) -1.4085(8) -0.1311(9) 0.055(3) Uani 1 1 d . . . H3 H 1.4187 -1.3781 -0.1848 0.066 Uiso 1 1 calc R A . C4 C 1.3044(10) -1.4707(9) -0.1304(11) 0.066(4) Uani 1 1 d . A . C5 C 1.2555(9) -1.5123(7) -0.0510(11) 0.055(4) Uani 1 1 d . . . C6 C 1.2836(9) -1.4969(8) 0.0244(10) 0.056(3) Uani 1 1 d . A . H6 H 1.2497 -1.5287 0.0773 0.068 Uiso 1 1 calc R . . C7 C 1.3624(8) -1.4346(7) 0.0259(9) 0.050(3) Uani 1 1 d . . . C8 C 1.3861(9) -1.4185(7) 0.1143(9) 0.054(3) Uani 1 1 d . A . H8A H 1.4638 -1.4008 0.1019 0.065 Uiso 1 1 calc R . . H8B H 1.3814 -1.4756 0.1483 0.065 Uiso 1 1 calc R . . C9 C 1.3041(8) -1.3452(8) 0.1724(8) 0.052(3) Uani 1 1 d . . . C10 C 1.1976(9) -1.3669(8) 0.2241(8) 0.066(4) Uani 1 1 d . A . H10 H 1.1782 -1.4267 0.2212 0.079 Uiso 1 1 calc R . . C11 C 1.1191(10) -1.3067(9) 0.2787(9) 0.074(4) Uani 1 1 d . A . C12 C 1.1512(9) -1.2191(8) 0.2845(8) 0.056(3) Uani 1 1 d . . . C13 C 1.2528(8) -1.1930(8) 0.2332(7) 0.052(3) Uani 1 1 d . A . H13 H 1.2705 -1.1327 0.2358 0.062 Uiso 1 1 calc R . . C14 C 1.3314(8) -1.2555(7) 0.1763(7) 0.046(3) Uani 1 1 d . A . C15 C 1.4411(7) -1.2212(7) 0.1168(8) 0.047(3) Uani 1 1 d . . . H15A H 1.4668 -1.1763 0.1503 0.056 Uiso 1 1 calc R A . H15B H 1.4998 -1.2720 0.1018 0.056 Uiso 1 1 calc R . . C16 C 1.4273(8) -1.1788(8) 0.0314(8) 0.046(3) Uani 1 1 d . A . C17 C 1.3886(7) -1.0859(8) 0.0335(8) 0.044(3) Uani 1 1 d . . . H17 H 1.3681 -1.0546 0.0886 0.053 Uiso 1 1 calc R A . C18 C 1.3800(8) -1.0403(8) -0.0423(9) 0.041(3) Uani 1 1 d . A . C19 C 1.4060(8) -1.0863(9) -0.1223(9) 0.045(3) Uani 1 1 d . . . C20 C 1.4434(8) -1.1775(8) -0.1269(8) 0.049(3) Uani 1 1 d . A . H20 H 1.4618 -1.2082 -0.1823 0.058 Uiso 1 1 calc R . . C21 C 1.4540(8) -1.2240(8) -0.0506(9) 0.049(3) Uani 1 1 d . . . C22 C 1.1972(10) -1.6562(8) -0.0734(8) 0.055(3) Uani 1 1 d . . . C23 C 1.0956(8) -1.7043(7) -0.0711(8) 0.048(3) Uani 1 1 d . A . C24 C 0.9853(9) -1.6604(8) -0.0427(8) 0.057(3) Uani 1 1 d . . . H24 H 0.9745 -1.5991 -0.0249 0.069 Uiso 1 1 calc R A . C25 C 0.8939(9) -1.7076(8) -0.0410(8) 0.056(3) Uani 1 1 d . A . H25 H 0.8201 -1.6784 -0.0216 0.068 Uiso 1 1 calc R . . C26 C 0.9085(9) -1.7968(8) -0.0674(8) 0.057(3) Uani 1 1 d . . . H26 H 0.8449 -1.8277 -0.0671 0.069 Uiso 1 1 calc R A . C27 C 1.0172(9) -1.8421(8) -0.0948(7) 0.050(3) Uani 1 1 d . A . C28 C 1.1100(8) -1.7950(7) -0.0960(7) 0.047(3) Uani 1 1 d . . . H28 H 1.1835 -1.8249 -0.1140 0.056 Uiso 1 1 calc R A . C29 C 1.0305(8) -1.9386(8) -0.1206(8) 0.049(3) Uani 1 1 d . . . C30 C 1.1138(9) -1.9982(8) -0.1029(8) 0.051(3) Uani 1 1 d . A . H30 H 1.1667 -1.9772 -0.0765 0.061 Uiso 1 1 calc R . . C31 C 1.1189(9) -2.0880(9) -0.1240(8) 0.061(4) Uani 1 1 d . . . H31 H 1.1751 -2.1272 -0.1091 0.073 Uiso 1 1 calc R A . C32 C 0.9733(10) -2.0673(9) -0.1834(8) 0.061(4) Uani 1 1 d . . . H32 H 0.9247 -2.0898 -0.2130 0.074 Uiso 1 1 calc R A . C33 C 0.9596(9) -1.9758(8) -0.1624(8) 0.058(3) Uani 1 1 d . A . H33 H 0.9014 -1.9385 -0.1766 0.069 Uiso 1 1 calc R . . C34 C 1.333(3) -1.457(3) -0.292(3) 0.116(13) Uiso 0.50 1 d PU A 1 H34A H 1.3009 -1.4761 -0.3372 0.174 Uiso 0.50 1 calc PR A 1 H34B H 1.4126 -1.4798 -0.3060 0.174 Uiso 0.50 1 calc PR A 1 H34C H 1.3279 -1.3908 -0.2896 0.174 Uiso 0.50 1 calc PR A 1 C34' C 1.283(3) -1.422(2) -0.275(2) 0.088(10) Uiso 0.50 1 d PU A 2 H34D H 1.2588 -1.4440 -0.3244 0.132 Uiso 0.50 1 calc PR A 2 H34E H 1.3621 -1.4080 -0.2978 0.132 Uiso 0.50 1 calc PR A 2 H34F H 1.2364 -1.3671 -0.2505 0.132 Uiso 0.50 1 calc PR A 2 C35 C 1.0491(11) -1.1639(9) 0.4279(11) 0.062(4) Uani 1 1 d . . . C36 C 0.9465(10) -1.1033(9) 0.4791(9) 0.063(4) Uani 1 1 d . B . C37 C 0.9101(12) -1.1133(10) 0.5722(10) 0.080(4) Uani 1 1 d . . . H37 H 0.9509 -1.1540 0.6013 0.096 Uiso 1 1 calc R B . C38 C 0.8145(13) -1.0635(11) 0.6210(11) 0.088(5) Uani 1 1 d . B . H38 H 0.7904 -1.0686 0.6841 0.106 Uiso 1 1 calc R . . C39 C 0.7538(12) -1.0059(10) 0.5775(11) 0.079(4) Uani 1 1 d . . . H39 H 0.6856 -0.9746 0.6110 0.095 Uiso 1 1 calc R B . C40 C 0.7910(10) -0.9935(9) 0.4863(10) 0.064(4) Uani 1 1 d . B . C41 C 0.8879(10) -1.0441(9) 0.4356(9) 0.063(4) Uani 1 1 d . . . H41 H 0.9129 -1.0378 0.3726 0.075 Uiso 1 1 calc R B . C42 C 0.7270(11) -0.9302(10) 0.4410(10) 0.072(4) Uani 1 1 d . . . C43 C 0.7775(12) -0.8777(9) 0.3708(11) 0.078(4) Uani 1 1 d . B . H43 H 0.8573 -0.8803 0.3495 0.094 Uiso 1 1 calc R . . C44 C 0.7131(13) -0.8206(12) 0.3304(10) 0.093(5) Uani 1 1 d . . . H44 H 0.7512 -0.7850 0.2817 0.112 Uiso 1 1 calc R B . C45 C 0.5493(14) -0.8614(14) 0.4248(13) 0.099(6) Uani 1 1 d . . . H45 H 0.4694 -0.8550 0.4455 0.119 Uiso 1 1 calc R B . C46 C 0.6052(11) -0.9215(11) 0.4691(11) 0.085(5) Uani 1 1 d . B . H46 H 0.5645 -0.9564 0.5172 0.102 Uiso 1 1 calc R . . C47 C 0.984(3) -1.4161(15) 0.333(2) 0.091(11) Uiso 0.50 1 d PDU B 1 H47A H 0.9064 -1.4200 0.3706 0.137 Uiso 0.50 1 calc PR B 1 H47B H 1.0355 -1.4536 0.3584 0.137 Uiso 0.50 1 calc PR B 1 H47C H 0.9907 -1.4371 0.2728 0.137 Uiso 0.50 1 calc PR B 1 C47' C 0.9595(19) -1.3929(15) 0.2961(17) 0.052(7) Uiso 0.50 1 d PDU B 2 H47D H 0.8842 -1.3990 0.3367 0.078 Uiso 0.50 1 calc PR B 2 H47E H 1.0056 -1.4500 0.2933 0.078 Uiso 0.50 1 calc PR B 2 H47F H 0.9536 -1.3770 0.2364 0.078 Uiso 0.50 1 calc PR B 2 C48 C 1.4663(11) -0.9783(8) -0.2352(8) 0.054(3) Uani 1 1 d . . . C49 C 1.4207(10) -0.9064(8) -0.2845(8) 0.052(3) Uani 1 1 d . A . C50 C 1.3116(11) -0.9018(10) -0.2938(8) 0.067(4) Uani 1 1 d . . . H50 H 1.2652 -0.9496 -0.2727 0.081 Uiso 1 1 calc R A . C51 C 1.2719(12) -0.8276(12) -0.3338(10) 0.084(4) Uani 1 1 d . A . H51 H 1.1971 -0.8237 -0.3380 0.100 Uiso 1 1 calc R . . C52 C 1.3398(14) -0.7593(11) -0.3676(11) 0.099(5) Uani 1 1 d . . . H52 H 1.3114 -0.7100 -0.3967 0.119 Uiso 1 1 calc R A . C53 C 1.4499(12) -0.7602(10) -0.3604(10) 0.081(4) Uani 1 1 d . A . C54 C 1.4889(10) -0.8361(9) -0.3186(8) 0.067(4) Uani 1 1 d D . . H54 H 1.5632 -0.8397 -0.3134 0.080 Uiso 1 1 calc R A . C55 C 1.5177(18) -0.6948(13) -0.4097(14) 0.049(6) Uiso 0.50 1 d PDU A 1 C56 C 1.631(2) -0.700(3) -0.4301(18) 0.084(12) Uiso 0.50 1 d PDU A 1 H56 H 1.6684 -0.7532 -0.4131 0.101 Uiso 0.50 1 calc PR A 1 C57 C 1.698(3) -0.6333(18) -0.4743(19) 0.079(10) Uiso 0.50 1 d PDU A 1 H57 H 1.7769 -0.6451 -0.4889 0.094 Uiso 0.50 1 calc PR A 1 N3 N 1.6590(17) -0.5573(15) -0.4965(14) 0.071(6) Uiso 0.50 1 d PDU A 1 C58 C 1.548(2) -0.550(2) -0.482(2) 0.096(9) Uiso 0.50 1 d PDU . 1 H58 H 1.5142 -0.4961 -0.4992 0.116 Uiso 0.50 1 calc PR . 1 C59 C 1.478(2) -0.6185(17) -0.4422(17) 0.083(8) Uiso 0.50 1 d PDU A 1 H59 H 1.4007 -0.6103 -0.4382 0.099 Uiso 0.50 1 calc PR A 1 C55' C 1.532(2) -0.6794(14) -0.3673(18) 0.075(8) Uiso 0.50 1 d PDU A 2 C56' C 1.637(2) -0.690(3) -0.424(2) 0.088(12) Uiso 0.50 1 d PDU A 2 H56' H 1.6640 -0.7475 -0.4506 0.106 Uiso 0.50 1 calc PR A 2 C57' C 1.708(3) -0.6207(19) -0.443(2) 0.083(10) Uiso 0.50 1 d PDU A 2 H57' H 1.7822 -0.6316 -0.4812 0.100 Uiso 0.50 1 calc PR A 2 N3' N 1.673(2) -0.542(2) -0.4107(18) 0.107(8) Uiso 0.50 1 d PDU A 2 C58' C 1.573(3) -0.534(3) -0.351(2) 0.133(13) Uiso 0.50 1 d PDU A 2 H58' H 1.5509 -0.4779 -0.3200 0.160 Uiso 0.50 1 calc PR A 2 C59' C 1.496(3) -0.5993(19) -0.329(2) 0.101(10) Uiso 0.50 1 d PDU A 2 H59' H 1.4222 -0.5878 -0.2888 0.121 Uiso 0.50 1 calc PR A 2 C60 C 1.3136(9) -0.8984(8) 0.0367(8) 0.056(3) Uani 1 1 d . . . H60A H 1.3744 -0.9036 0.0651 0.084 Uiso 1 1 calc R . . H60B H 1.2462 -0.9219 0.0770 0.084 Uiso 1 1 calc R . . H60C H 1.2969 -0.8350 0.0236 0.084 Uiso 1 1 calc R . . C61 C 1.9776(13) -0.3147(9) -0.2061(10) 0.105(6) Uani 1 1 d D . . H61 H 2.0128 -0.2687 -0.1802 0.126 Uiso 1 1 calc R . . Cl1 Cl 2.0324(4) -0.3124(4) -0.3244(3) 0.1314(19) Uani 1 1 d D . . Cl2 Cl 1.8291(4) -0.2868(4) -0.1766(5) 0.184(3) Uani 1 1 d D . . Cl3 Cl 2.0066(5) -0.4180(4) -0.1647(3) 0.1366(19) Uani 1 1 d D . . C62 C 1.7323(16) -0.3830(14) -0.4185(15) 0.082(8) Uiso 0.50 1 d PD . . H62 H 1.7173 -0.4248 -0.4619 0.098 Uiso 0.50 1 calc PR . . Cl4 Cl 1.7465(13) -0.4437(10) -0.3239(10) 0.200(6) Uiso 0.50 1 d PD . . Cl5 Cl 1.6076(7) -0.3080(6) -0.3714(6) 0.114(3) Uiso 0.50 1 d PD . . Cl6 Cl 1.8422(6) -0.3251(5) -0.4701(5) 0.086(2) Uiso 0.50 1 d PD . . 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 O1 0.043(4) 0.037(5) 0.114(7) -0.029(5) -0.006(4) -0.005(4) O2 0.039(5) 0.045(5) 0.121(8) -0.031(5) -0.006(4) -0.003(4) O3 0.092(7) 0.079(7) 0.096(8) -0.006(6) -0.038(6) -0.029(5) O4 0.045(4) 0.053(5) 0.060(6) -0.014(5) 0.008(4) -0.005(4) O5 0.083(7) 0.073(7) 0.067(7) -0.001(6) 0.006(5) -0.007(5) O6 0.061(5) 0.067(6) 0.128(8) -0.038(6) 0.043(5) -0.027(5) O7 0.053(5) 0.050(5) 0.059(6) -0.009(5) -0.012(4) -0.014(4) O8 0.043(5) 0.070(6) 0.061(6) -0.006(4) 0.000(4) -0.011(4) O9 0.047(4) 0.043(5) 0.060(6) -0.004(4) -0.011(4) -0.004(4) N1 0.046(6) 0.044(7) 0.088(8) -0.011(6) 0.000(6) -0.005(5) N2 0.075(10) 0.124(12) 0.085(11) -0.038(9) -0.008(8) 0.012(8) C1 0.040(6) 0.047(8) 0.048(7) -0.015(6) -0.001(5) -0.003(5) C2 0.038(6) 0.027(7) 0.079(10) -0.014(7) 0.010(7) -0.004(5) C3 0.051(7) 0.056(8) 0.056(9) -0.014(7) -0.009(6) -0.015(6) C4 0.056(8) 0.055(9) 0.081(11) -0.016(8) -0.010(8) -0.002(7) C5 0.033(6) 0.032(8) 0.088(11) -0.016(8) 0.004(7) -0.003(5) C6 0.039(7) 0.041(8) 0.076(10) -0.002(7) -0.001(7) 0.013(6) C7 0.031(6) 0.026(7) 0.083(11) -0.016(7) -0.002(6) 0.005(5) C8 0.046(6) 0.020(7) 0.083(10) -0.007(6) 0.002(6) 0.007(5) C9 0.041(6) 0.050(8) 0.057(8) -0.005(6) -0.001(6) -0.004(5) C10 0.054(7) 0.050(8) 0.080(10) -0.012(7) 0.005(7) -0.011(6) C11 0.053(8) 0.067(10) 0.082(10) -0.015(8) 0.015(7) -0.020(7) C12 0.045(7) 0.056(9) 0.057(9) -0.017(7) -0.001(6) -0.002(6) C13 0.044(7) 0.043(8) 0.060(8) 0.000(6) -0.001(6) -0.005(5) C14 0.044(6) 0.040(8) 0.051(8) -0.007(6) -0.007(5) -0.007(5) C15 0.025(5) 0.047(7) 0.061(9) -0.017(6) 0.001(5) -0.005(5) C16 0.035(6) 0.041(8) 0.056(9) -0.008(7) 0.000(6) -0.009(5) C17 0.025(5) 0.050(9) 0.048(8) -0.020(7) 0.007(5) -0.008(5) C18 0.035(6) 0.031(8) 0.052(9) -0.004(7) -0.003(5) -0.013(5) C19 0.039(6) 0.052(9) 0.046(9) -0.002(7) -0.011(6) -0.016(6) C20 0.042(6) 0.047(9) 0.046(9) -0.018(7) 0.009(5) -0.016(6) C21 0.027(6) 0.044(8) 0.061(9) -0.004(7) 0.013(5) -0.013(5) C22 0.052(8) 0.032(8) 0.074(9) -0.022(6) -0.006(6) -0.008(6) C23 0.042(6) 0.035(7) 0.063(8) -0.001(6) -0.008(5) -0.002(5) C24 0.041(7) 0.037(7) 0.089(10) -0.015(7) -0.012(6) 0.001(5) C25 0.034(6) 0.046(8) 0.081(10) -0.016(7) -0.004(6) 0.003(5) C26 0.035(6) 0.044(8) 0.088(10) -0.008(7) -0.010(6) -0.003(5) C27 0.043(7) 0.050(8) 0.055(8) -0.010(6) -0.011(6) -0.002(6) C28 0.038(6) 0.034(7) 0.066(8) -0.012(6) -0.008(5) -0.006(5) C29 0.034(6) 0.046(8) 0.062(8) -0.017(6) -0.001(5) -0.007(6) C30 0.038(6) 0.045(8) 0.065(9) -0.013(6) -0.004(5) -0.006(6) C31 0.040(7) 0.059(10) 0.076(10) -0.002(7) -0.003(6) -0.013(6) C32 0.047(7) 0.057(10) 0.075(10) -0.022(8) -0.003(6) -0.021(7) C33 0.048(7) 0.049(9) 0.075(9) -0.008(7) -0.012(6) -0.012(6) C35 0.065(9) 0.040(9) 0.068(12) -0.003(8) 0.003(8) -0.014(7) C36 0.055(8) 0.059(9) 0.063(10) -0.012(8) 0.006(7) -0.021(7) C37 0.081(10) 0.081(11) 0.063(11) -0.006(8) 0.010(8) -0.025(8) C38 0.073(10) 0.102(13) 0.069(11) -0.031(10) 0.017(9) -0.007(9) C39 0.057(9) 0.079(11) 0.079(12) -0.020(9) 0.018(8) -0.009(8) C40 0.045(7) 0.065(10) 0.067(10) -0.015(8) 0.012(7) -0.016(7) C41 0.052(8) 0.064(9) 0.063(9) -0.023(8) 0.003(7) -0.017(7) C42 0.067(9) 0.073(10) 0.061(10) -0.024(8) 0.014(8) -0.020(8) C43 0.065(9) 0.050(9) 0.108(13) -0.011(9) -0.009(9) 0.004(7) C44 0.074(11) 0.104(14) 0.083(12) -0.025(10) 0.007(9) -0.001(9) C45 0.067(10) 0.130(17) 0.079(13) -0.063(12) 0.015(10) 0.000(11) C46 0.051(9) 0.099(13) 0.091(12) -0.036(10) 0.005(8) 0.000(8) C48 0.056(8) 0.046(8) 0.050(8) -0.012(7) 0.007(6) -0.015(7) C49 0.058(8) 0.045(8) 0.046(8) -0.007(6) -0.002(6) -0.014(6) C50 0.066(9) 0.075(11) 0.055(9) -0.007(8) -0.006(7) -0.015(7) C51 0.066(9) 0.097(13) 0.084(11) 0.008(10) -0.019(8) 0.001(9) C52 0.081(12) 0.096(14) 0.104(13) 0.030(10) -0.009(9) 0.012(10) C53 0.070(10) 0.071(11) 0.078(11) 0.001(9) 0.013(8) -0.002(8) C54 0.056(8) 0.067(10) 0.069(10) -0.009(8) -0.002(7) -0.011(7) C60 0.045(6) 0.043(8) 0.068(9) -0.012(7) 0.004(6) -0.010(5) C61 0.123(13) 0.061(11) 0.102(13) -0.016(9) 0.015(10) -0.017(9) Cl1 0.118(4) 0.134(4) 0.123(4) 0.013(3) -0.002(3) -0.020(3) Cl2 0.107(4) 0.124(5) 0.266(8) -0.031(5) 0.041(4) -0.020(3) Cl3 0.163(5) 0.117(4) 0.125(4) 0.007(3) -0.026(3) -0.043(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 O1 C22 1.364(12) . ? O1 C5 1.428(13) . ? O2 C22 1.206(12) . ? O3 C4 1.391(15) . ? O3 C34 1.45(4) . ? O3 C34' 1.48(3) . ? O4 C35 1.374(16) . ? O4 C12 1.431(12) . ? O5 C35 1.202(15) . ? O6 C11 1.373(13) . ? O6 C47' 1.471(18) . ? O6 C47 1.48(2) . ? O7 C48 1.375(13) . ? O7 C19 1.412(13) . ? O8 C48 1.221(14) . ? O9 C18 1.380(12) . ? O9 C60 1.454(12) . ? N1 C32 1.336(15) . ? N1 C31 1.342(15) . ? N2 C45 1.31(2) . ? N2 C44 1.360(18) . ? C1 C2 1.542(15) . ? C1 C21 1.552(15) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C7 1.389(16) . ? C2 C3 1.397(16) . ? C3 C4 1.416(17) . ? C3 H3 0.9500 . ? C4 C5 1.376(17) . ? C5 C6 1.356(16) . ? C6 C7 1.417(16) . ? C6 H6 0.9500 . ? C7 C8 1.525(16) . ? C8 C9 1.546(14) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.400(15) . ? C9 C14 1.416(15) . ? C10 C11 1.378(16) . ? C10 H10 0.9500 . ? C11 C12 1.412(16) . ? C12 C13 1.373(14) . ? C13 C14 1.415(14) . ? C13 H13 0.9500 . ? C14 C15 1.536(14) . ? C15 C16 1.513(15) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C21 1.405(15) . ? C16 C17 1.426(15) . ? C17 C18 1.380(15) . ? C17 H17 0.9500 . ? C18 C19 1.385(15) . ? C19 C20 1.396(15) . ? C20 C21 1.400(15) . ? C20 H20 0.9500 . ? C22 C23 1.501(15) . ? C23 C28 1.400(14) . ? C23 C24 1.422(14) . ? C24 C25 1.386(15) . ? C24 H24 0.9500 . ? C25 C26 1.385(14) . ? C25 H25 0.9500 . ? C26 C27 1.413(14) . ? C26 H26 0.9500 . ? C27 C28 1.400(14) . ? C27 C29 1.489(15) . ? C28 H28 0.9500 . ? C29 C30 1.392(15) . ? C29 C33 1.399(15) . ? C30 C31 1.382(15) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.397(15) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C34' H34D 0.9800 . ? C34' H34E 0.9800 . ? C34' H34F 0.9800 . ? C35 C36 1.529(18) . ? C36 C41 1.387(17) . ? C36 C37 1.403(17) . ? C37 C38 1.380(18) . ? C37 H37 0.9500 . ? C38 C39 1.39(2) . ? C38 H38 0.9500 . ? C39 C40 1.381(18) . ? C39 H39 0.9500 . ? C40 C41 1.406(16) . ? C40 C42 1.482(19) . ? C41 H41 0.9500 . ? C42 C43 1.364(18) . ? C42 C46 1.448(18) . ? C43 C44 1.38(2) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.38(2) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C47' H47D 0.9800 . ? C47' H47E 0.9800 . ? C47' H47F 0.9800 . ? C48 C49 1.475(17) . ? C49 C54 1.403(16) . ? C49 C50 1.405(17) . ? C50 C51 1.383(18) . ? C50 H50 0.9500 . ? C51 C52 1.38(2) . ? C51 H51 0.9500 . ? C52 C53 1.41(2) . ? C52 H52 0.9500 . ? C53 C55 1.41(2) . ? C53 C54 1.414(18) . ? C53 C55' 1.63(3) . ? C54 H54 0.9500 . ? C55 C59 1.35(3) . ? C55 C56 1.36(2) . ? C56 C57 1.39(2) . ? C56 H56 0.9500 . ? C57 N3 1.27(2) . ? C57 H57 0.9500 . ? N3 C58 1.33(3) . ? C58 C59 1.41(3) . ? C58 C58 2.01(6) 2_844 ? C58 H58 0.9500 . ? C59 H59 0.9500 . ? C55' C59' 1.34(3) . ? C55' C56' 1.35(2) . ? C56' C57' 1.39(2) . ? C56' H56' 0.9500 . ? C57' N3' 1.28(2) . ? C57' H57' 0.9500 . ? N3' C58' 1.33(3) . ? C58' C59' 1.40(3) . ? C58' H58' 0.9500 . ? C59' H59' 0.9500 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 Cl3 1.708(15) . ? C61 Cl1 1.780(15) . ? C61 Cl2 1.788(16) . ? C61 H61 1.0000 . ? C62 Cl6 1.675(19) . ? C62 Cl4 1.76(2) . ? C62 Cl5 1.81(2) . ? C62 H62 1.0000 . ? 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 C22 O1 C5 117.9(8) . . ? C4 O3 C34 118.9(18) . . ? C4 O3 C34' 117.0(15) . . ? C34 O3 C34' 30.2(18) . . ? C35 O4 C12 115.1(10) . . ? C11 O6 C47' 115.8(12) . . ? C11 O6 C47 115.6(15) . . ? C47' O6 C47 31.0(14) . . ? C48 O7 C19 116.0(9) . . ? C18 O9 C60 118.6(9) . . ? C32 N1 C31 115.3(10) . . ? C45 N2 C44 116.0(15) . . ? C2 C1 C21 114.5(8) . . ? C2 C1 H1A 108.6 . . ? C21 C1 H1A 108.6 . . ? C2 C1 H1B 108.6 . . ? C21 C1 H1B 108.6 . . ? H1A C1 H1B 107.6 . . ? C7 C2 C3 120.6(11) . . ? C7 C2 C1 123.4(12) . . ? C3 C2 C1 116.0(11) . . ? C2 C3 C4 120.5(12) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 O3 118.4(12) . . ? C5 C4 C3 117.9(13) . . ? O3 C4 C3 123.7(13) . . ? C6 C5 C4 121.9(12) . . ? C6 C5 O1 119.5(12) . . ? C4 C5 O1 118.4(14) . . ? C5 C6 C7 121.4(12) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C2 C7 C6 117.6(12) . . ? C2 C7 C8 124.3(11) . . ? C6 C7 C8 118.2(12) . . ? C7 C8 C9 113.6(9) . . ? C7 C8 H8A 108.9 . . ? C9 C8 H8A 108.9 . . ? C7 C8 H8B 108.9 . . ? C9 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C10 C9 C14 117.5(10) . . ? C10 C9 C8 119.5(10) . . ? C14 C9 C8 122.9(9) . . ? C11 C10 C9 123.9(11) . . ? C11 C10 H10 118.0 . . ? C9 C10 H10 118.0 . . ? O6 C11 C10 127.4(12) . . ? O6 C11 C12 115.5(10) . . ? C10 C11 C12 117.1(10) . . ? C13 C12 C11 121.5(10) . . ? C13 C12 O4 119.7(11) . . ? C11 C12 O4 118.4(9) . . ? C12 C13 C14 120.3(10) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C13 C14 C9 119.4(9) . . ? C13 C14 C15 117.9(9) . . ? C9 C14 C15 122.5(9) . . ? C16 C15 C14 112.5(8) . . ? C16 C15 H15A 109.1 . . ? C14 C15 H15A 109.1 . . ? C16 C15 H15B 109.1 . . ? C14 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? C21 C16 C17 117.8(11) . . ? C21 C16 C15 124.4(11) . . ? C17 C16 C15 117.8(10) . . ? C18 C17 C16 121.9(11) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C17 C18 O9 124.8(11) . . ? C17 C18 C19 119.3(11) . . ? O9 C18 C19 115.9(11) . . ? C18 C19 C20 120.5(12) . . ? C18 C19 O7 117.2(11) . . ? C20 C19 O7 122.3(11) . . ? C19 C20 C21 120.5(11) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C20 C21 C16 120.0(11) . . ? C20 C21 C1 117.3(11) . . ? C16 C21 C1 122.7(12) . . ? O2 C22 O1 123.5(10) . . ? O2 C22 C23 125.5(10) . . ? O1 C22 C23 111.0(9) . . ? C28 C23 C24 119.5(9) . . ? C28 C23 C22 119.0(9) . . ? C24 C23 C22 121.4(10) . . ? C25 C24 C23 119.5(10) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C26 C25 C24 120.9(10) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C25 C26 C27 120.5(10) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C28 C27 C26 118.9(10) . . ? C28 C27 C29 121.6(9) . . ? C26 C27 C29 119.5(9) . . ? C27 C28 C23 120.6(9) . . ? C27 C28 H28 119.7 . . ? C23 C28 H28 119.7 . . ? C30 C29 C33 115.6(11) . . ? C30 C29 C27 121.7(10) . . ? C33 C29 C27 122.7(11) . . ? C31 C30 C29 119.4(11) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? N1 C31 C30 125.5(12) . . ? N1 C31 H31 117.2 . . ? C30 C31 H31 117.2 . . ? N1 C32 C33 123.3(11) . . ? N1 C32 H32 118.3 . . ? C33 C32 H32 118.3 . . ? C32 C33 C29 120.8(11) . . ? C32 C33 H33 119.6 . . ? C29 C33 H33 119.6 . . ? O3 C34 H34A 109.5 . . ? O3 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O3 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O3 C34' H34D 109.5 . . ? O3 C34' H34E 109.5 . . ? H34D C34' H34E 109.5 . . ? O3 C34' H34F 109.5 . . ? H34D C34' H34F 109.5 . . ? H34E C34' H34F 109.5 . . ? O5 C35 O4 124.4(12) . . ? O5 C35 C36 124.0(15) . . ? O4 C35 C36 111.6(14) . . ? C41 C36 C37 121.0(12) . . ? C41 C36 C35 121.7(13) . . ? C37 C36 C35 117.2(14) . . ? C38 C37 C36 119.5(15) . . ? C38 C37 H37 120.2 . . ? C36 C37 H37 120.2 . . ? C37 C38 C39 119.8(15) . . ? C37 C38 H38 120.1 . . ? C39 C38 H38 120.1 . . ? C40 C39 C38 121.0(13) . . ? C40 C39 H39 119.5 . . ? C38 C39 H39 119.5 . . ? C39 C40 C41 119.7(14) . . ? C39 C40 C42 120.6(12) . . ? C41 C40 C42 119.7(13) . . ? C36 C41 C40 118.9(13) . . ? C36 C41 H41 120.6 . . ? C40 C41 H41 120.6 . . ? C43 C42 C46 116.0(16) . . ? C43 C42 C40 123.0(13) . . ? C46 C42 C40 121.0(14) . . ? C42 C43 C44 120.3(15) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? N2 C44 C43 124.1(16) . . ? N2 C44 H44 118.0 . . ? C43 C44 H44 118.0 . . ? N2 C45 C46 124.6(16) . . ? N2 C45 H45 117.7 . . ? C46 C45 H45 117.7 . . ? C45 C46 C42 118.9(16) . . ? C45 C46 H46 120.6 . . ? C42 C46 H46 120.6 . . ? O6 C47 H47A 109.5 . . ? O6 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? O6 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? O6 C47' H47D 109.5 . . ? O6 C47' H47E 109.5 . . ? H47D C47' H47E 109.5 . . ? O6 C47' H47F 109.5 . . ? H47D C47' H47F 109.5 . . ? H47E C47' H47F 109.5 . . ? O8 C48 O7 121.9(12) . . ? O8 C48 C49 125.7(11) . . ? O7 C48 C49 112.3(11) . . ? C54 C49 C50 119.0(13) . . ? C54 C49 C48 117.2(12) . . ? C50 C49 C48 123.7(12) . . ? C51 C50 C49 119.9(13) . . ? C51 C50 H50 120.1 . . ? C49 C50 H50 120.1 . . ? C52 C51 C50 120.6(15) . . ? C52 C51 H51 119.7 . . ? C50 C51 H51 119.7 . . ? C51 C52 C53 122.0(15) . . ? C51 C52 H52 119.0 . . ? C53 C52 H52 119.0 . . ? C52 C53 C55 116.9(17) . . ? C52 C53 C54 116.6(13) . . ? C55 C53 C54 125.3(16) . . ? C52 C53 C55' 131.3(16) . . ? C55 C53 C55' 28.6(12) . . ? C54 C53 C55' 110.0(15) . . ? C49 C54 C53 121.8(13) . . ? C49 C54 H54 119.1 . . ? C53 C54 H54 119.1 . . ? C59 C55 C56 111(3) . . ? C59 C55 C53 125(2) . . ? C56 C55 C53 124(2) . . ? C55 C56 C57 124(3) . . ? C55 C56 H56 118.0 . . ? C57 C56 H56 118.0 . . ? N3 C57 C56 125(3) . . ? N3 C57 H57 117.7 . . ? C56 C57 H57 117.7 . . ? C57 N3 C58 114(3) . . ? N3 C58 C59 124(3) . . ? N3 C58 C58 128(3) . 2_844 ? C59 C58 C58 108(2) . 2_844 ? N3 C58 H58 118.1 . . ? C59 C58 H58 118.1 . . ? C58 C58 H58 10.9 2_844 . ? C55 C59 C58 122(3) . . ? C55 C59 H59 118.8 . . ? C58 C59 H59 118.8 . . ? C59' C55' C56' 119(3) . . ? C59' C55' C53 123(2) . . ? C56' C55' C53 118(2) . . ? C55' C56' C57' 122(4) . . ? C55' C56' H56' 119.0 . . ? C57' C56' H56' 119.0 . . ? N3' C57' C56' 121(4) . . ? N3' C57' H57' 119.5 . . ? C56' C57' H57' 119.5 . . ? C57' N3' C58' 116(3) . . ? N3' C58' C59' 126(4) . . ? N3' C58' H58' 116.9 . . ? C59' C58' H58' 116.9 . . ? C55' C59' C58' 115(3) . . ? C55' C59' H59' 122.3 . . ? C58' C59' H59' 122.3 . . ? O9 C60 H60A 109.5 . . ? O9 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? O9 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? Cl3 C61 Cl1 111.0(8) . . ? Cl3 C61 Cl2 110.3(8) . . ? Cl1 C61 Cl2 108.8(9) . . ? Cl3 C61 H61 108.9 . . ? Cl1 C61 H61 108.9 . . ? Cl2 C61 H61 108.9 . . ? Cl6 C62 Cl4 114.7(13) . . ? Cl6 C62 Cl5 111.1(12) . . ? Cl4 C62 Cl5 101.9(12) . . ? Cl6 C62 H62 109.6 . . ? Cl4 C62 H62 109.6 . . ? Cl5 C62 H62 109.6 . . ? 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 C21 C1 C2 C7 -93.8(13) . . . . ? C21 C1 C2 C3 86.2(12) . . . . ? C7 C2 C3 C4 -0.9(17) . . . . ? C1 C2 C3 C4 179.1(10) . . . . ? C34 O3 C4 C5 -172(2) . . . . ? C34' O3 C4 C5 153.5(18) . . . . ? C34 O3 C4 C3 8(3) . . . . ? C34' O3 C4 C3 -26(2) . . . . ? C2 C3 C4 C5 0.9(17) . . . . ? C2 C3 C4 O3 -179.6(10) . . . . ? O3 C4 C5 C6 178.9(10) . . . . ? C3 C4 C5 C6 -1.5(17) . . . . ? O3 C4 C5 O1 -5.1(16) . . . . ? C3 C4 C5 O1 174.4(9) . . . . ? C22 O1 C5 C6 -98.7(12) . . . . ? C22 O1 C5 C4 85.3(14) . . . . ? C4 C5 C6 C7 2.2(17) . . . . ? O1 C5 C6 C7 -173.7(9) . . . . ? C3 C2 C7 C6 1.4(15) . . . . ? C1 C2 C7 C6 -178.6(9) . . . . ? C3 C2 C7 C8 -178.3(10) . . . . ? C1 C2 C7 C8 1.7(16) . . . . ? C5 C6 C7 C2 -2.1(15) . . . . ? C5 C6 C7 C8 177.7(9) . . . . ? C2 C7 C8 C9 92.7(12) . . . . ? C6 C7 C8 C9 -87.1(12) . . . . ? C7 C8 C9 C10 80.7(14) . . . . ? C7 C8 C9 C14 -99.3(13) . . . . ? C14 C9 C10 C11 -1(2) . . . . ? C8 C9 C10 C11 179.2(13) . . . . ? C47' O6 C11 C10 -26(2) . . . . ? C47 O6 C11 C10 8(3) . . . . ? C47' O6 C11 C12 153.8(16) . . . . ? C47 O6 C11 C12 -171.8(19) . . . . ? C9 C10 C11 O6 177.6(13) . . . . ? C9 C10 C11 C12 -2(2) . . . . ? O6 C11 C12 C13 -175.4(12) . . . . ? C10 C11 C12 C13 5(2) . . . . ? O6 C11 C12 O4 -3.0(18) . . . . ? C10 C11 C12 O4 177.0(12) . . . . ? C35 O4 C12 C13 -112.1(12) . . . . ? C35 O4 C12 C11 75.4(14) . . . . ? C11 C12 C13 C14 -3.7(19) . . . . ? O4 C12 C13 C14 -176.0(10) . . . . ? C12 C13 C14 C9 0.4(17) . . . . ? C12 C13 C14 C15 176.8(11) . . . . ? C10 C9 C14 C13 1.8(17) . . . . ? C8 C9 C14 C13 -178.2(11) . . . . ? C10 C9 C14 C15 -174.5(11) . . . . ? C8 C9 C14 C15 5.5(18) . . . . ? C13 C14 C15 C16 -83.4(12) . . . . ? C9 C14 C15 C16 92.9(13) . . . . ? C14 C15 C16 C21 -96.2(11) . . . . ? C14 C15 C16 C17 86.2(11) . . . . ? C21 C16 C17 C18 -1.7(14) . . . . ? C15 C16 C17 C18 176.0(8) . . . . ? C16 C17 C18 O9 -176.8(9) . . . . ? C16 C17 C18 C19 2.2(14) . . . . ? C60 O9 C18 C17 -4.5(13) . . . . ? C60 O9 C18 C19 176.5(8) . . . . ? C17 C18 C19 C20 -1.7(14) . . . . ? O9 C18 C19 C20 177.4(9) . . . . ? C17 C18 C19 O7 175.7(8) . . . . ? O9 C18 C19 O7 -5.2(12) . . . . ? C48 O7 C19 C18 75.4(11) . . . . ? C48 O7 C19 C20 -107.3(11) . . . . ? C18 C19 C20 C21 0.7(14) . . . . ? O7 C19 C20 C21 -176.6(8) . . . . ? C19 C20 C21 C16 -0.2(14) . . . . ? C19 C20 C21 C1 -176.9(9) . . . . ? C17 C16 C21 C20 0.7(13) . . . . ? C15 C16 C21 C20 -176.9(9) . . . . ? C17 C16 C21 C1 177.2(9) . . . . ? C15 C16 C21 C1 -0.4(14) . . . . ? C2 C1 C21 C20 -88.5(12) . . . . ? C2 C1 C21 C16 94.9(12) . . . . ? C5 O1 C22 O2 5.2(19) . . . . ? C5 O1 C22 C23 -176.4(11) . . . . ? O2 C22 C23 C28 -1.8(19) . . . . ? O1 C22 C23 C28 179.8(10) . . . . ? O2 C22 C23 C24 177.0(12) . . . . ? O1 C22 C23 C24 -1.4(16) . . . . ? C28 C23 C24 C25 -0.7(18) . . . . ? C22 C23 C24 C25 -179.6(11) . . . . ? C23 C24 C25 C26 -0.5(19) . . . . ? C24 C25 C26 C27 1.4(19) . . . . ? C25 C26 C27 C28 -0.9(18) . . . . ? C25 C26 C27 C29 178.4(11) . . . . ? C26 C27 C28 C23 -0.4(17) . . . . ? C29 C27 C28 C23 -179.7(11) . . . . ? C24 C23 C28 C27 1.2(17) . . . . ? C22 C23 C28 C27 -180.0(11) . . . . ? C28 C27 C29 C30 33.9(17) . . . . ? C26 C27 C29 C30 -145.4(11) . . . . ? C28 C27 C29 C33 -147.3(11) . . . . ? C26 C27 C29 C33 33.4(17) . . . . ? C33 C29 C30 C31 -2.2(15) . . . . ? C27 C29 C30 C31 176.7(10) . . . . ? C32 N1 C31 C30 -0.4(17) . . . . ? C29 C30 C31 N1 2.3(17) . . . . ? C31 N1 C32 C33 -1.5(17) . . . . ? N1 C32 C33 C29 1.5(18) . . . . ? C30 C29 C33 C32 0.5(16) . . . . ? C27 C29 C33 C32 -178.3(10) . . . . ? C12 O4 C35 O5 8.6(17) . . . . ? C12 O4 C35 C36 -169.3(9) . . . . ? O5 C35 C36 C41 179.5(12) . . . . ? O4 C35 C36 C41 -2.6(16) . . . . ? O5 C35 C36 C37 -3.8(19) . . . . ? O4 C35 C36 C37 174.1(10) . . . . ? C41 C36 C37 C38 0.0(19) . . . . ? C35 C36 C37 C38 -176.7(12) . . . . ? C36 C37 C38 C39 2(2) . . . . ? C37 C38 C39 C40 -4(2) . . . . ? C38 C39 C40 C41 4(2) . . . . ? C38 C39 C40 C42 -178.4(13) . . . . ? C37 C36 C41 C40 0.3(18) . . . . ? C35 C36 C41 C40 176.8(10) . . . . ? C39 C40 C41 C36 -2.3(17) . . . . ? C42 C40 C41 C36 -179.8(11) . . . . ? C39 C40 C42 C43 142.9(13) . . . . ? C41 C40 C42 C43 -39.6(19) . . . . ? C39 C40 C42 C46 -37.6(19) . . . . ? C41 C40 C42 C46 139.8(12) . . . . ? C46 C42 C43 C44 0(2) . . . . ? C40 C42 C43 C44 179.1(12) . . . . ? C45 N2 C44 C43 1(2) . . . . ? C42 C43 C44 N2 0(2) . . . . ? C44 N2 C45 C46 -3(2) . . . . ? N2 C45 C46 C42 2(2) . . . . ? C43 C42 C46 C45 -1(2) . . . . ? C40 C42 C46 C45 179.9(13) . . . . ? C19 O7 C48 O8 20.3(15) . . . . ? C19 O7 C48 C49 -156.2(9) . . . . ? O8 C48 C49 C54 -3.0(17) . . . . ? O7 C48 C49 C54 173.4(10) . . . . ? O8 C48 C49 C50 -178.7(11) . . . . ? O7 C48 C49 C50 -2.3(15) . . . . ? C54 C49 C50 C51 -1.8(18) . . . . ? C48 C49 C50 C51 173.8(12) . . . . ? C49 C50 C51 C52 2(2) . . . . ? C50 C51 C52 C53 -2(2) . . . . ? C51 C52 C53 C55 170.0(16) . . . . ? C51 C52 C53 C54 2(2) . . . . ? C51 C52 C53 C55' -159.9(18) . . . . ? C50 C49 C54 C53 1.2(18) . . . . ? C48 C49 C54 C53 -174.7(11) . . . . ? C52 C53 C54 C49 -1.1(19) . . . . ? C55 C53 C54 C49 -168.5(16) . . . . ? C55' C53 C54 C49 164.2(14) . . . . ? C52 C53 C55 C59 19(3) . . . . ? C54 C53 C55 C59 -174(2) . . . . ? C55' C53 C55 C59 -109(4) . . . . ? C52 C53 C55 C56 -161.3(18) . . . . ? C54 C53 C55 C56 6(3) . . . . ? C55' C53 C55 C56 71(3) . . . . ? C59 C55 C56 C57 3(2) . . . . ? C53 C55 C56 C57 -176(2) . . . . ? C55 C56 C57 N3 4(2) . . . . ? C56 C57 N3 C58 -7(3) . . . . ? C57 N3 C58 C59 3(4) . . . . ? C57 N3 C58 C58 -173(3) . . . 2_844 ? C56 C55 C59 C58 -7(3) . . . . ? C53 C55 C59 C58 172(2) . . . . ? N3 C58 C59 C55 5(4) . . . . ? C58 C58 C59 C55 -179(2) 2_844 . . . ? C52 C53 C55' C59' 43(3) . . . . ? C55 C53 C55' C59' 112(4) . . . . ? C54 C53 C55' C59' -119(2) . . . . ? C52 C53 C55' C56' -128.4(19) . . . . ? C55 C53 C55' C56' -59(3) . . . . ? C54 C53 C55' C56' 69(2) . . . . ? C59' C55' C56' C57' -1(2) . . . . ? C53 C55' C56' C57' 171(2) . . . . ? C55' C56' C57' N3' -3(2) . . . . ? C56' C57' N3' C58' 7(4) . . . . ? C57' N3' C58' C59' -9(5) . . . . ? C56' C55' C59' C58' 0(4) . . . . ? C53 C55' C59' C58' -172(2) . . . . ? N3' C58' C59' C55' 5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.167 _refine_diff_density_min -0.767 _refine_diff_density_rms 0.094 # Attachment '- 4ph3py_new.CIF' data_4ph3py_new _database_code_depnum_ccdc_archive 'CCDC 822479' #TrackingRef '- 4ph3py_new.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(+-)-2,7,12-trimethoxy-3,8,13-tris[4- (3-pyridyl)benzoyl]-10,15-dihydro-5H- tribenzo[a,d,g]cyclononane] diethylether N-methylpyrrolidone clathrate ; _chemical_name_common ; ((+-)-2,7,12-trimethoxy-3,8,13-tris(4-(3-pyridyl)benzoyl)- 10,15-dihydro-5H-tribenzo(a,d,g)cyclononane) diethylether N- methylpyrrolidone clathrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C148 H146 N10 O24' _chemical_formula_weight 2448.75 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc 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' _cell_length_a 29.169(3) _cell_length_b 16.8460(16) _cell_length_c 32.562(4) _cell_angle_alpha 90.00 _cell_angle_beta 114.432(4) _cell_angle_gamma 90.00 _cell_volume 14568(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.117 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5184 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9565 _exptl_absorpt_correction_T_max 0.9902 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 X8 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 89435 _diffrn_reflns_av_R_equivalents 0.0736 _diffrn_reflns_av_sigmaI/netI 0.0732 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.96 _reflns_number_total 27444 _reflns_number_gt 20664 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour)' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. C-C and C-O bond lengths of solvent di-ethyl ether molecules were restrained using the following DFIX commands: DFIX 1.54 0.02 C147 C148 DFIX 1.54 0.02 C145 C146 DFIX 1.45 0.02 C146 O24 DFIX 1.45 0.02 C147 O24 DFIX 1.54 0.02 C141 C142 DFIX 1.54 0.02 C143 C144 DFIX 1.45 0.02 C143 O23 DFIX 1.45 0.02 C142 O23 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type bloc _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1948P)^2^+23.2480P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 1.3(11) _refine_ls_number_reflns 27444 _refine_ls_number_parameters 1649 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1266 _refine_ls_R_factor_gt 0.1017 _refine_ls_wR_factor_ref 0.2950 _refine_ls_wR_factor_gt 0.2729 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.042 _refine_ls_shift/su_mean 0.009 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 O1 O 0.40095(14) 0.1226(2) 0.48618(13) 0.0359(8) Uani 1 1 d . . . O2 O 0.43250(13) -0.0272(2) 0.48482(12) 0.0321(8) Uani 1 1 d . . . O3 O 0.36013(13) -0.0437(2) 0.42052(12) 0.0337(8) Uani 1 1 d . . . O4 O 0.68076(13) -0.0936(2) 0.48091(12) 0.0339(8) Uani 1 1 d . . . O5 O 0.73676(13) 0.0332(2) 0.47763(12) 0.0310(8) Uani 1 1 d . . . O6 O 0.73967(13) -0.0275(2) 0.41561(11) 0.0308(8) Uani 1 1 d . . . O7 O 0.64970(13) 0.4321(2) 0.48063(13) 0.0346(8) Uani 1 1 d . . . O8 O 0.55909(14) 0.4571(2) 0.48301(12) 0.0324(8) Uani 1 1 d . . . O9 O 0.53898(15) 0.5327(2) 0.41902(12) 0.0349(8) Uani 1 1 d . . . O10 O 0.69453(14) 0.6526(2) 0.83112(12) 0.0309(8) Uani 1 1 d . . . O11 O 0.70705(13) 0.7297(2) 0.89253(11) 0.0309(8) Uani 1 1 d . . . O12 O 0.60016(14) 0.6279(2) 0.82644(13) 0.0377(9) Uani 1 1 d . . . O13 O 0.50747(12) 0.2195(2) 0.82600(11) 0.0307(7) Uani 1 1 d . . . O14 O 0.50773(13) 0.1651(2) 0.89078(12) 0.0337(8) Uani 1 1 d . . . O15 O 0.56611(14) 0.0962(2) 0.82478(13) 0.0359(8) Uani 1 1 d . . . O16 O 0.81448(12) 0.1680(2) 0.82945(12) 0.0303(8) Uani 1 1 d . . . O17 O 0.88664(13) 0.1460(2) 0.89267(12) 0.0309(7) Uani 1 1 d . . . O18 O 0.84874(13) 0.3191(2) 0.83124(12) 0.0340(8) Uani 1 1 d . . . O19 O 0.8059(3) 0.7099(4) 0.64302(17) 0.088(2) Uani 1 1 d . . . O20 O 0.9782(2) 0.3402(4) 0.78272(16) 0.0814(18) Uani 1 1 d . . . C135 C 1.0133(4) 0.1570(6) 0.6882(4) 0.097(3) Uani 1 1 d . . . H13A H 0.9766 0.1540 0.6718 0.145 Uiso 1 1 calc R . . H13B H 1.0245 0.1194 0.7135 0.145 Uiso 1 1 calc R . . H13C H 1.0292 0.1435 0.6678 0.145 Uiso 1 1 calc R . . O22 O 0.7555(2) 0.6578(4) 0.52758(16) 0.0737(16) Uani 1 1 d . . . O23 O 0.6361(3) 0.1668(8) 0.5662(3) 0.210(8) Uani 1 1 d D . . O24 O 0.6504(4) 0.3683(8) 0.7446(4) 0.234(9) Uani 1 1 d D . . N1 N 0.3408(2) -0.3687(3) 0.62854(16) 0.0524(14) Uani 1 1 d . . . N2 N 0.6179(3) 0.8753(4) 0.6446(2) 0.083(2) Uani 1 1 d . . . N3 N 1.05252(18) 0.0059(4) 0.62936(17) 0.0509(13) Uani 1 1 d . . . N4 N 0.7337(2) 1.0360(3) 0.67938(17) 0.0551(15) Uani 1 1 d . . . N5 N 0.9406(3) -0.0622(6) 0.6665(2) 0.088(2) Uani 1 1 d . . . N6 N 0.1912(2) 0.1534(4) 0.68184(17) 0.0520(14) Uani 1 1 d . . . N7 N 0.7830(3) 0.8294(4) 0.6039(2) 0.0757(19) Uani 1 1 d . . . N8 N 0.8973(3) 0.3760(4) 0.7322(3) 0.079(2) Uani 1 1 d . . . C131 C 0.9969(3) 0.2994(5) 0.6922(2) 0.064(2) Uani 1 1 d . . . N10 N 0.7707(3) 0.5503(5) 0.5775(2) 0.079(2) Uani 1 1 d . . . C1 C 0.48213(16) 0.2202(3) 0.38685(15) 0.0226(9) Uani 1 1 d . . . H1A H 0.4520 0.2548 0.3756 0.027 Uiso 1 1 calc R . . H1B H 0.4853 0.1967 0.3603 0.027 Uiso 1 1 calc R . . C2 C 0.47389(16) 0.1530(3) 0.41499(15) 0.0228(9) Uani 1 1 d . . . C3 C 0.44506(17) 0.1712(3) 0.44025(16) 0.0263(10) Uani 1 1 d . . . H3 H 0.4349 0.2244 0.4414 0.032 Uiso 1 1 calc R . . C4 C 0.43153(18) 0.1119(3) 0.46330(16) 0.0286(10) Uani 1 1 d . . . C5 C 0.44752(17) 0.0341(3) 0.46207(17) 0.0277(10) Uani 1 1 d . . . C6 C 0.47672(17) 0.0150(3) 0.43895(17) 0.0284(11) Uani 1 1 d . . . H6 H 0.4880 -0.0381 0.4396 0.034 Uiso 1 1 calc R . . C7 C 0.49008(16) 0.0736(3) 0.41426(15) 0.0230(9) Uani 1 1 d . . . C8 C 0.51921(16) 0.0474(3) 0.38647(16) 0.0250(10) Uani 1 1 d . . . H8A H 0.5094 0.0826 0.3598 0.030 Uiso 1 1 calc R . . H8B H 0.5084 -0.0071 0.3752 0.030 Uiso 1 1 calc R . . C9 C 0.57754(16) 0.0482(3) 0.41175(15) 0.0226(9) Uani 1 1 d . . . C10 C 0.60116(18) -0.0209(3) 0.43597(16) 0.0267(10) Uani 1 1 d . . . H10 H 0.5809 -0.0640 0.4376 0.032 Uiso 1 1 calc R . . C11 C 0.65412(18) -0.0273(3) 0.45780(16) 0.0276(10) Uani 1 1 d . . . C12 C 0.68323(17) 0.0382(3) 0.45483(16) 0.0269(10) Uani 1 1 d . . . C13 C 0.66073(17) 0.1071(3) 0.43185(16) 0.0243(10) Uani 1 1 d . . . H13 H 0.6811 0.1504 0.4308 0.029 Uiso 1 1 calc R . . C14 C 0.60682(16) 0.1131(3) 0.40966(15) 0.0219(9) Uani 1 1 d . . . C15 C 0.58499(18) 0.1906(3) 0.38287(17) 0.0255(10) Uani 1 1 d . . . H15A H 0.6084 0.2099 0.3701 0.031 Uiso 1 1 calc R . . H15B H 0.5526 0.1781 0.3573 0.031 Uiso 1 1 calc R . . C16 C 0.57627(17) 0.2577(3) 0.41086(16) 0.0230(9) Uani 1 1 d . . . C17 C 0.61795(18) 0.3089(3) 0.43424(16) 0.0244(9) Uani 1 1 d . . . H17 H 0.6497 0.2982 0.4337 0.029 Uiso 1 1 calc R . . C18 C 0.61229(19) 0.3765(3) 0.45857(16) 0.0279(10) Uani 1 1 d . . . C19 C 0.56498(19) 0.3906(3) 0.45877(16) 0.0266(10) Uani 1 1 d . . . C20 C 0.52462(18) 0.3389(3) 0.43716(17) 0.0260(10) Uani 1 1 d . . . H20 H 0.4934 0.3488 0.4389 0.031 Uiso 1 1 calc R . . C21 C 0.52915(17) 0.2722(3) 0.41275(15) 0.0227(9) Uani 1 1 d . . . C22 C 0.3840(2) 0.2041(4) 0.4883(2) 0.0403(13) Uani 1 1 d . . . H22A H 0.3692 0.2268 0.4578 0.060 Uiso 1 1 calc R . . H22B H 0.4128 0.2364 0.5076 0.060 Uiso 1 1 calc R . . H22C H 0.3587 0.2035 0.5008 0.060 Uiso 1 1 calc R . . C23 C 0.38538(18) -0.0589(3) 0.46051(16) 0.0275(10) Uani 1 1 d . . . C24 C 0.36848(19) -0.1130(3) 0.48890(17) 0.0323(11) Uani 1 1 d . . . C25 C 0.32472(19) -0.1586(3) 0.46634(18) 0.0315(11) Uani 1 1 d . . . H25 H 0.3063 -0.1537 0.4346 0.038 Uiso 1 1 calc R . . C26 C 0.3083(2) -0.2115(3) 0.49112(19) 0.0354(12) Uani 1 1 d . . . H26 H 0.2791 -0.2429 0.4759 0.043 Uiso 1 1 calc R . . C27 C 0.3348(2) -0.2182(3) 0.53793(17) 0.0308(11) Uani 1 1 d . . . C28 C 0.3776(2) -0.1694(4) 0.56067(18) 0.0428(14) Uani 1 1 d . . . H28 H 0.3946 -0.1719 0.5926 0.051 Uiso 1 1 calc R . . C29 C 0.3951(2) -0.1170(3) 0.53642(19) 0.0383(13) Uani 1 1 d . . . H29 H 0.4241 -0.0851 0.5516 0.046 Uiso 1 1 calc R . . C30 C 0.3189(2) -0.2777(3) 0.56420(18) 0.0373(12) Uani 1 1 d . . . C31 C 0.2670(2) -0.3013(4) 0.5493(2) 0.0455(14) Uani 1 1 d . . . H31 H 0.2419 -0.2785 0.5229 0.055 Uiso 1 1 calc R . . C32 C 0.2537(3) -0.3581(4) 0.5740(2) 0.0519(16) Uani 1 1 d . . . H32 H 0.2199 -0.3752 0.5644 0.062 Uiso 1 1 calc R . . C33 C 0.2923(3) -0.3891(4) 0.6135(2) 0.0503(16) Uani 1 1 d . . . H33 H 0.2831 -0.4267 0.6306 0.060 Uiso 1 1 calc R . . C34 C 0.3530(2) -0.3120(4) 0.60381(18) 0.0447(14) Uani 1 1 d . . . H34 H 0.3872 -0.2955 0.6147 0.054 Uiso 1 1 calc R . . C35 C 0.6521(3) -0.1587(3) 0.4869(2) 0.0426(14) Uani 1 1 d . . . H35A H 0.6255 -0.1735 0.4577 0.064 Uiso 1 1 calc R . . H35B H 0.6369 -0.1426 0.5074 0.064 Uiso 1 1 calc R . . H35C H 0.6743 -0.2042 0.4997 0.064 Uiso 1 1 calc R . . C36 C 0.76096(18) -0.0044(3) 0.45436(16) 0.0270(10) Uani 1 1 d . . . C37 C 0.81666(19) -0.0119(3) 0.48369(17) 0.0320(11) Uani 1 1 d . . . C38 C 0.8470(2) -0.0565(4) 0.46679(19) 0.0390(13) Uani 1 1 d . . . H38 H 0.8325 -0.0793 0.4375 0.047 Uiso 1 1 calc R . . C39 C 0.8985(2) -0.0659(4) 0.49411(19) 0.0411(14) Uani 1 1 d . . . H39 H 0.9185 -0.0957 0.4830 0.049 Uiso 1 1 calc R . . C40 C 0.92164(19) -0.0321(4) 0.53810(18) 0.0363(12) Uani 1 1 d . . . C41 C 0.8905(2) 0.0139(4) 0.55305(18) 0.0385(13) Uani 1 1 d . . . H41 H 0.9051 0.0389 0.5817 0.046 Uiso 1 1 calc R . . C42 C 0.8396(2) 0.0231(4) 0.52685(18) 0.0371(12) Uani 1 1 d . . . H42 H 0.8197 0.0534 0.5380 0.045 Uiso 1 1 calc R . . C43 C 0.9763(2) -0.0439(4) 0.56857(19) 0.0376(12) Uani 1 1 d . . . C44 C 1.0021(2) -0.1136(5) 0.5680(3) 0.069(2) Uani 1 1 d . . . H44 H 0.9854 -0.1539 0.5466 0.083 Uiso 1 1 calc R . . C45 C 1.0527(3) -0.1247(5) 0.5989(4) 0.088(3) Uani 1 1 d . . . H45 H 1.0706 -0.1716 0.5984 0.105 Uiso 1 1 calc R . . C46 C 1.0754(2) -0.0654(5) 0.6299(2) 0.0567(17) Uani 1 1 d . . . H46 H 1.1083 -0.0743 0.6525 0.068 Uiso 1 1 calc R . . C47 C 1.0042(2) 0.0131(4) 0.5998(2) 0.0476(15) Uani 1 1 d . . . H47 H 0.9876 0.0614 0.6003 0.057 Uiso 1 1 calc R . . C48 C 0.69954(19) 0.4132(3) 0.48466(19) 0.0336(11) Uani 1 1 d . . . H48A H 0.6987 0.4049 0.4546 0.050 Uiso 1 1 calc R . . H48B H 0.7115 0.3648 0.5026 0.050 Uiso 1 1 calc R . . H48C H 0.7224 0.4572 0.4995 0.050 Uiso 1 1 calc R . . C49 C 0.54956(18) 0.5282(3) 0.45910(16) 0.0262(10) Uani 1 1 d . . . C50 C 0.55325(18) 0.5986(3) 0.48945(17) 0.0279(10) Uani 1 1 d . . . C51 C 0.5666(2) 0.5904(3) 0.53610(18) 0.0334(11) Uani 1 1 d . . . H51 H 0.5720 0.5389 0.5492 0.040 Uiso 1 1 calc R . . C52 C 0.5718(2) 0.6572(3) 0.56330(17) 0.0335(11) Uani 1 1 d . . . H52 H 0.5814 0.6509 0.5948 0.040 Uiso 1 1 calc R . . C53 C 0.5629(2) 0.7346(3) 0.54399(18) 0.0337(11) Uani 1 1 d . . . C54 C 0.5476(2) 0.7434(3) 0.49731(19) 0.0357(12) Uani 1 1 d . . . H54 H 0.5403 0.7947 0.4840 0.043 Uiso 1 1 calc R . . C55 C 0.5432(2) 0.6751(3) 0.46967(18) 0.0338(11) Uani 1 1 d . . . H55 H 0.5335 0.6811 0.4382 0.041 Uiso 1 1 calc R . . C56 C 0.5687(2) 0.8065(3) 0.5735(2) 0.0437(14) Uani 1 1 d . . . C57 C 0.6092(3) 0.8115(4) 0.6177(2) 0.0503(15) Uani 1 1 d . . . H57 H 0.6310 0.7671 0.6285 0.060 Uiso 1 1 calc R . . C58 C 0.5844(5) 0.9371(5) 0.6300(3) 0.103(4) Uani 1 1 d . . . H58 H 0.5894 0.9812 0.6495 0.123 Uiso 1 1 calc R . . C59 C 0.5413(4) 0.9385(5) 0.5859(3) 0.099(4) Uani 1 1 d . . . H59 H 0.5192 0.9828 0.5760 0.118 Uiso 1 1 calc R . . C60 C 0.5347(3) 0.8704(4) 0.5593(2) 0.066(2) Uani 1 1 d . . . H60 H 0.5065 0.8673 0.5309 0.079 Uiso 1 1 calc R . . C61 C 0.76227(19) 0.4127(3) 0.92714(17) 0.0279(10) Uani 1 1 d . . . H61A H 0.7564 0.3881 0.9521 0.034 Uiso 1 1 calc R . . H61B H 0.7926 0.4466 0.9407 0.034 Uiso 1 1 calc R . . C62 C 0.71708(18) 0.4656(3) 0.89992(16) 0.0243(10) Uani 1 1 d . . . C63 C 0.72455(18) 0.5327(3) 0.87703(17) 0.0255(10) Uani 1 1 d . . . H63 H 0.7570 0.5422 0.8778 0.031 Uiso 1 1 calc R . . C64 C 0.68573(18) 0.5844(3) 0.85374(16) 0.0250(10) Uani 1 1 d . . . C65 C 0.63613(19) 0.5717(3) 0.85039(18) 0.0298(11) Uani 1 1 d . . . C66 C 0.62763(17) 0.5047(3) 0.87197(16) 0.0248(10) Uani 1 1 d . . . H66 H 0.5947 0.4944 0.8697 0.030 Uiso 1 1 calc R . . C67 C 0.66763(16) 0.4520(2) 0.89715(16) 0.0224(9) Uani 1 1 d . . . C68 C 0.65520(17) 0.3829(3) 0.92287(16) 0.0239(9) Uani 1 1 d . . . H68A H 0.6862 0.3695 0.9498 0.029 Uiso 1 1 calc R . . H68B H 0.6301 0.4022 0.9337 0.029 Uiso 1 1 calc R . . C69 C 0.63488(18) 0.3069(3) 0.89560(16) 0.0263(10) Uani 1 1 d . . . C70 C 0.58230(18) 0.2980(3) 0.87143(16) 0.0272(10) Uani 1 1 d . . . H70 H 0.5610 0.3411 0.8708 0.033 Uiso 1 1 calc R . . C71 C 0.56032(17) 0.2284(3) 0.84843(16) 0.0277(10) Uani 1 1 d . . . C72 C 0.59129(19) 0.1635(3) 0.84764(18) 0.0307(11) Uani 1 1 d . . . C73 C 0.64406(18) 0.1714(3) 0.87094(17) 0.0270(10) Uani 1 1 d . . . H73 H 0.6653 0.1292 0.8701 0.032 Uiso 1 1 calc R . . C74 C 0.66611(17) 0.2419(3) 0.89582(16) 0.0253(10) Uani 1 1 d . . . C75 C 0.72336(16) 0.2406(3) 0.92407(17) 0.0253(10) Uani 1 1 d . . . H75A H 0.7313 0.2757 0.9505 0.030 Uiso 1 1 calc R . . H75B H 0.7334 0.1860 0.9355 0.030 Uiso 1 1 calc R . . C76 C 0.75494(17) 0.2665(3) 0.89911(16) 0.0251(10) Uani 1 1 d . . . C77 C 0.76934(17) 0.2087(3) 0.87496(16) 0.0262(10) Uani 1 1 d . . . H77 H 0.7572 0.1559 0.8733 0.031 Uiso 1 1 calc R . . C78 C 0.80060(18) 0.2272(3) 0.85374(16) 0.0272(10) Uani 1 1 d . . . C79 C 0.81766(17) 0.3069(3) 0.85394(17) 0.0269(10) Uani 1 1 d . . . C80 C 0.80350(17) 0.3651(3) 0.87717(16) 0.0257(10) Uani 1 1 d . . . H80 H 0.8147 0.4182 0.8776 0.031 Uiso 1 1 calc R . . C81 C 0.77307(16) 0.3465(3) 0.89986(16) 0.0239(9) Uani 1 1 d . . . C82 C 0.70325(18) 0.7236(3) 0.85414(16) 0.0255(10) Uani 1 1 d . . . C83 C 0.7083(2) 0.7898(3) 0.82533(17) 0.0307(11) Uani 1 1 d . . . C84 C 0.7127(2) 0.8684(3) 0.84166(18) 0.0353(12) Uani 1 1 d . . . H84 H 0.7140 0.8778 0.8709 0.042 Uiso 1 1 calc R . . C85 C 0.7151(2) 0.9333(3) 0.81502(18) 0.0370(12) Uani 1 1 d . . . H85 H 0.7191 0.9855 0.8270 0.044 Uiso 1 1 calc R . . C86 C 0.7118(2) 0.9215(3) 0.77107(18) 0.0363(12) Uani 1 1 d . . . C87 C 0.7090(2) 0.8403(3) 0.75576(19) 0.0415(13) Uani 1 1 d . . . H87 H 0.7085 0.8304 0.7269 0.050 Uiso 1 1 calc R . . C88 C 0.7070(2) 0.7766(3) 0.78177(18) 0.0361(12) Uani 1 1 d . . . H88 H 0.7047 0.7241 0.7705 0.043 Uiso 1 1 calc R . . C89 C 0.7123(2) 0.9877(3) 0.74092(19) 0.0421(13) Uani 1 1 d . . . C90 C 0.6887(4) 1.0605(4) 0.7402(3) 0.067(2) Uani 1 1 d . . . H90 H 0.6735 1.0700 0.7605 0.081 Uiso 1 1 calc R . . C91 C 0.6876(3) 1.1196(5) 0.7091(3) 0.074(2) Uani 1 1 d . . . H91 H 0.6723 1.1695 0.7086 0.089 Uiso 1 1 calc R . . C92 C 0.7095(3) 1.1034(4) 0.6789(2) 0.0542(16) Uani 1 1 d . . . H92 H 0.7070 1.1424 0.6570 0.065 Uiso 1 1 calc R . . C93 C 0.7340(2) 0.9780(4) 0.70987(19) 0.0441(14) Uani 1 1 d . . . H93 H 0.7499 0.9288 0.7098 0.053 Uiso 1 1 calc R . . C94 C 0.5487(2) 0.6144(3) 0.8205(2) 0.0404(13) Uani 1 1 d . . . H94A H 0.5369 0.5633 0.8054 0.061 Uiso 1 1 calc R . . H94B H 0.5271 0.6571 0.8020 0.061 Uiso 1 1 calc R . . H94C H 0.5472 0.6137 0.8500 0.061 Uiso 1 1 calc R . . C95 C 0.48502(17) 0.1807(3) 0.85074(17) 0.0256(10) Uani 1 1 d . . . C96 C 0.43059(18) 0.1632(3) 0.82224(17) 0.0271(10) Uani 1 1 d . . . C97 C 0.4005(2) 0.1352(4) 0.84439(19) 0.0391(13) Uani 1 1 d . . . H97 H 0.4154 0.1277 0.8762 0.047 Uiso 1 1 calc R . . C98 C 0.3491(2) 0.1186(4) 0.81970(19) 0.0416(13) Uani 1 1 d . . . H98 H 0.3294 0.1004 0.8348 0.050 Uiso 1 1 calc R . . C99 C 0.32680(18) 0.1288(3) 0.77244(18) 0.0317(11) Uani 1 1 d . . . C100 C 0.35660(19) 0.1570(3) 0.75042(18) 0.0356(12) Uani 1 1 d . . . H100 H 0.3418 0.1650 0.7187 0.043 Uiso 1 1 calc R . . C101 C 0.40780(19) 0.1732(3) 0.77525(18) 0.0329(11) Uani 1 1 d . . . H101 H 0.4275 0.1914 0.7600 0.039 Uiso 1 1 calc R . . C102 C 0.27071(19) 0.1154(3) 0.74665(19) 0.0356(12) Uani 1 1 d . . . C103 C 0.2424(2) 0.0629(4) 0.7616(2) 0.0474(14) Uani 1 1 d . . . H103 H 0.2586 0.0336 0.7887 0.057 Uiso 1 1 calc R . . C104 C 0.1907(2) 0.0552(4) 0.7358(3) 0.0530(16) Uani 1 1 d . . . H104 H 0.1715 0.0194 0.7450 0.064 Uiso 1 1 calc R . . C105 C 0.1676(2) 0.0994(4) 0.6973(2) 0.0512(16) Uani 1 1 d . . . H105 H 0.1325 0.0916 0.6802 0.061 Uiso 1 1 calc R . . C106 C 0.2421(2) 0.1593(4) 0.70649(19) 0.0448(14) Uani 1 1 d . . . H106 H 0.2599 0.1955 0.6961 0.054 Uiso 1 1 calc R . . C107 C 0.5966(2) 0.0294(3) 0.8219(2) 0.0429(13) Uani 1 1 d . . . H10A H 0.6174 0.0463 0.8064 0.064 Uiso 1 1 calc R . . H10B H 0.5745 -0.0140 0.8050 0.064 Uiso 1 1 calc R . . H10C H 0.6183 0.0111 0.8524 0.064 Uiso 1 1 calc R . . C108 C 0.86234(18) 0.1352(3) 0.85274(16) 0.0243(9) Uani 1 1 d . . . C109 C 0.87687(18) 0.0844(3) 0.82197(16) 0.0268(10) Uani 1 1 d . . . C110 C 0.8478(2) 0.0773(4) 0.77541(19) 0.0390(12) Uani 1 1 d . . . H110 H 0.8159 0.1026 0.7624 0.047 Uiso 1 1 calc R . . C111 C 0.8644(2) 0.0347(4) 0.74816(19) 0.0429(13) Uani 1 1 d . . . H111 H 0.8439 0.0313 0.7167 0.051 Uiso 1 1 calc R . . C112 C 0.9118(2) -0.0041(3) 0.76651(18) 0.0375(12) Uani 1 1 d . . . C113 C 0.94147(19) 0.0008(3) 0.81417(17) 0.0338(11) Uani 1 1 d . . . H113 H 0.9727 -0.0266 0.8274 0.041 Uiso 1 1 calc R . . C114 C 0.92449(19) 0.0457(3) 0.84109(18) 0.0309(11) Uani 1 1 d . . . H114 H 0.9449 0.0506 0.8725 0.037 Uiso 1 1 calc R . . C115 C 0.9303(2) -0.0518(4) 0.73745(19) 0.0418(13) Uani 1 1 d . . . C116 C 0.9551(3) -0.1247(5) 0.7519(3) 0.068(2) Uani 1 1 d . . . H116 H 0.9606 -0.1454 0.7806 0.081 Uiso 1 1 calc R . . C117 C 0.9719(4) -0.1668(7) 0.7232(3) 0.096(4) Uani 1 1 d . . . H117 H 0.9887 -0.2163 0.7322 0.115 Uiso 1 1 calc R . . C118 C 0.9634(5) -0.1345(8) 0.6824(3) 0.113(5) Uani 1 1 d . . . H118 H 0.9740 -0.1643 0.6632 0.136 Uiso 1 1 calc R . . C119 C 0.9228(3) -0.0244(4) 0.6939(2) 0.0543(17) Uani 1 1 d . . . H119 H 0.9043 0.0232 0.6833 0.065 Uiso 1 1 calc R . . C120 C 0.8628(2) 0.4007(3) 0.8280(2) 0.0347(11) Uani 1 1 d . . . H12A H 0.8324 0.4332 0.8143 0.052 Uiso 1 1 calc R . . H12B H 0.8818 0.4030 0.8092 0.052 Uiso 1 1 calc R . . H12C H 0.8838 0.4209 0.8582 0.052 Uiso 1 1 calc R . . C121 C 0.8105(4) 0.7617(6) 0.6203(3) 0.076(2) Uani 1 1 d . . . C122 C 0.8486(4) 0.7583(7) 0.5974(3) 0.088(3) Uani 1 1 d . . . H12Q H 0.8833 0.7690 0.6198 0.105 Uiso 1 1 calc R . . H12R H 0.8477 0.7055 0.5837 0.105 Uiso 1 1 calc R . . C123 C 0.8311(4) 0.8221(6) 0.5616(4) 0.083(3) Uani 1 1 d . . . H12L H 0.8101 0.7992 0.5317 0.100 Uiso 1 1 calc R . . H12M H 0.8602 0.8497 0.5598 0.100 Uiso 1 1 calc R . . C124 C 0.7999(3) 0.8801(5) 0.5771(3) 0.074(2) Uani 1 1 d . . . H12J H 0.8210 0.9242 0.5953 0.089 Uiso 1 1 calc R . . H12K H 0.7710 0.9023 0.5509 0.089 Uiso 1 1 calc R . . C125 C 0.7457(5) 0.8527(7) 0.6200(4) 0.105(4) Uani 1 1 d . . . H12D H 0.7295 0.9021 0.6051 0.158 Uiso 1 1 calc R . . H12E H 0.7620 0.8611 0.6527 0.158 Uiso 1 1 calc R . . H12F H 0.7203 0.8108 0.6131 0.158 Uiso 1 1 calc R . . C126 C 0.9340(3) 0.3219(5) 0.7574(2) 0.0601(18) Uani 1 1 d . . . C127 C 0.9093(3) 0.2392(5) 0.7468(3) 0.0665(19) Uani 1 1 d . . . H5 H 0.9216 0.2086 0.7274 0.080 Uiso 1 1 calc R . . H7 H 0.9168 0.2089 0.7749 0.080 Uiso 1 1 calc R . . C128 C 0.8527(3) 0.2554(5) 0.7222(3) 0.071(2) Uani 1 1 d . . . H8 H 0.8358 0.2145 0.6990 0.085 Uiso 1 1 calc R . . H12G H 0.8365 0.2573 0.7436 0.085 Uiso 1 1 calc R . . C129 C 0.8514(4) 0.3345(8) 0.7013(4) 0.102(3) Uani 1 1 d . . . H12H H 0.8514 0.3285 0.6710 0.122 Uiso 1 1 calc R . . H12I H 0.8209 0.3644 0.6982 0.122 Uiso 1 1 calc R . . C130 C 0.9097(7) 0.4609(7) 0.7279(6) 0.144(6) Uani 1 1 d . . . H13D H 0.8789 0.4893 0.7088 0.217 Uiso 1 1 calc R . . H13E H 0.9340 0.4635 0.7142 0.217 Uiso 1 1 calc R . . H13F H 0.9244 0.4854 0.7579 0.217 Uiso 1 1 calc R . . N9 N 1.0279(2) 0.2377(4) 0.7056(2) 0.0678(17) Uani 1 1 d . . . C132 C 1.0807(3) 0.2553(5) 0.7315(3) 0.0653(19) Uani 1 1 d . . . H1 H 1.0997 0.2540 0.7124 0.078 Uiso 1 1 calc R . . H2 H 1.0962 0.2180 0.7570 0.078 Uiso 1 1 calc R . . C133 C 1.0776(3) 0.3422(5) 0.7484(3) 0.073(2) Uani 1 1 d . . . H9 H 1.0766 0.3411 0.7784 0.087 Uiso 1 1 calc R . . H11 H 1.1068 0.3743 0.7503 0.087 Uiso 1 1 calc R . . C134 C 1.0300(4) 0.3750(5) 0.7138(3) 0.078(2) Uani 1 1 d . . . H4 H 1.0365 0.4056 0.6908 0.093 Uiso 1 1 calc R . . H12 H 1.0132 0.4099 0.7278 0.093 Uiso 1 1 calc R . . O21 O 0.9520(2) 0.3021(5) 0.66843(18) 0.0887(19) Uani 1 1 d . . . C136 C 0.7441(3) 0.6134(5) 0.5533(2) 0.0578(17) Uani 1 1 d . . . C137 C 0.6985(3) 0.6227(5) 0.5642(2) 0.0587(17) Uani 1 1 d . . . H13M H 0.7027 0.6694 0.5838 0.070 Uiso 1 1 calc R . . H13N H 0.6676 0.6299 0.5362 0.070 Uiso 1 1 calc R . . C138 C 0.6950(3) 0.5480(5) 0.5880(3) 0.069(2) Uani 1 1 d . . . H13Q H 0.6718 0.5091 0.5667 0.083 Uiso 1 1 calc R . . H13R H 0.6835 0.5594 0.6121 0.083 Uiso 1 1 calc R . . C139 C 0.7511(4) 0.5166(6) 0.6085(3) 0.089(3) Uani 1 1 d . . . H13O H 0.7701 0.5362 0.6396 0.107 Uiso 1 1 calc R . . H13P H 0.7523 0.4579 0.6084 0.107 Uiso 1 1 calc R . . C140 C 0.8201(4) 0.5279(7) 0.5791(5) 0.119(4) Uani 1 1 d . . . H14A H 0.8328 0.4810 0.5984 0.178 Uiso 1 1 calc R . . H14B H 0.8438 0.5720 0.5915 0.178 Uiso 1 1 calc R . . H14C H 0.8168 0.5157 0.5486 0.178 Uiso 1 1 calc R . . C141 C 0.6616(6) 0.2997(8) 0.5768(5) 0.142(6) Uani 1 1 d D . . H14N H 0.6951 0.2811 0.5810 0.212 Uiso 1 1 calc R . . H14O H 0.6598 0.3026 0.6062 0.212 Uiso 1 1 calc R . . H14P H 0.6554 0.3524 0.5628 0.212 Uiso 1 1 calc R . . C142 C 0.6207(9) 0.2401(9) 0.5455(5) 0.190(10) Uani 1 1 d D . . H14T H 0.5869 0.2542 0.5437 0.228 Uiso 1 1 calc R . . H14U H 0.6196 0.2400 0.5147 0.228 Uiso 1 1 calc R . . C143 C 0.6064(4) 0.0986(6) 0.5362(4) 0.097(3) Uani 1 1 d D . . H14D H 0.6071 0.1027 0.5061 0.117 Uiso 1 1 calc R . . H14E H 0.5708 0.1009 0.5321 0.117 Uiso 1 1 calc R . . C144 C 0.6305(7) 0.0203(8) 0.5589(6) 0.160(7) Uani 1 1 d D . . H14H H 0.6539 0.0307 0.5902 0.240 Uiso 1 1 calc R . . H14I H 0.6488 -0.0034 0.5426 0.240 Uiso 1 1 calc R . . H14J H 0.6042 -0.0163 0.5584 0.240 Uiso 1 1 calc R . . C145 C 0.7235(6) 0.3366(10) 0.7302(7) 0.174(10) Uani 1 1 d D . . H14Q H 0.7405 0.3881 0.7346 0.261 Uiso 1 1 calc R . . H14R H 0.6989 0.3318 0.6988 0.261 Uiso 1 1 calc R . . H14S H 0.7485 0.2939 0.7371 0.261 Uiso 1 1 calc R . . C146 C 0.6966(7) 0.3302(11) 0.7616(6) 0.29(2) Uani 1 1 d D . . H14V H 0.6915 0.2734 0.7665 0.345 Uiso 1 1 calc R . . H14W H 0.7182 0.3536 0.7912 0.345 Uiso 1 1 calc R . . C147 C 0.6228(6) 0.3715(10) 0.7752(4) 0.120(5) Uani 1 1 d D . . H14F H 0.6068 0.3197 0.7754 0.144 Uiso 1 1 calc R . . H14G H 0.6464 0.3847 0.8064 0.144 Uiso 1 1 calc R . . C148 C 0.5836(7) 0.4349(13) 0.7562(6) 0.215(12) Uani 1 1 d D . . H14K H 0.5594 0.4309 0.7698 0.322 Uiso 1 1 calc R . . H14L H 0.5660 0.4281 0.7235 0.322 Uiso 1 1 calc R . . H14M H 0.5998 0.4871 0.7629 0.322 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 O1 0.037(2) 0.031(2) 0.054(2) 0.0035(17) 0.0334(18) 0.0017(16) O2 0.0259(18) 0.0296(19) 0.0434(19) 0.0122(15) 0.0168(15) -0.0018(14) O3 0.0283(19) 0.032(2) 0.042(2) 0.0070(16) 0.0153(16) 0.0038(15) O4 0.0279(18) 0.0224(17) 0.052(2) 0.0078(15) 0.0175(16) 0.0043(14) O5 0.0239(18) 0.0294(19) 0.0398(18) -0.0081(15) 0.0133(15) 0.0014(14) O6 0.0225(17) 0.0314(19) 0.0393(19) -0.0025(15) 0.0136(15) 0.0000(14) O7 0.0318(19) 0.0249(18) 0.054(2) -0.0065(16) 0.0243(17) -0.0063(14) O8 0.042(2) 0.0227(18) 0.0407(19) -0.0010(14) 0.0248(17) -0.0036(15) O9 0.045(2) 0.0236(18) 0.039(2) -0.0024(15) 0.0201(17) 0.0048(15) O10 0.042(2) 0.0212(17) 0.0389(18) -0.0004(14) 0.0262(16) -0.0064(14) O11 0.037(2) 0.0229(18) 0.0357(19) 0.0031(14) 0.0182(16) -0.0035(14) O12 0.035(2) 0.0234(18) 0.054(2) 0.0083(16) 0.0184(17) 0.0068(15) O13 0.0240(17) 0.0275(18) 0.0400(19) 0.0048(15) 0.0127(15) -0.0007(14) O14 0.0215(18) 0.035(2) 0.041(2) 0.0078(16) 0.0091(15) -0.0062(14) O15 0.034(2) 0.0250(19) 0.050(2) -0.0071(16) 0.0184(17) -0.0085(15) O16 0.0202(17) 0.0249(18) 0.045(2) -0.0089(15) 0.0122(15) 0.0015(13) O17 0.0297(18) 0.0249(18) 0.0391(19) -0.0008(15) 0.0151(15) 0.0013(14) O18 0.032(2) 0.035(2) 0.045(2) -0.0034(16) 0.0251(16) 0.0000(15) O19 0.144(6) 0.064(4) 0.048(3) 0.012(2) 0.031(3) -0.017(4) O20 0.089(4) 0.108(5) 0.040(2) -0.005(3) 0.019(3) -0.038(3) C135 0.099(8) 0.067(6) 0.114(8) -0.027(5) 0.034(6) -0.018(5) O22 0.061(3) 0.109(5) 0.046(3) -0.002(3) 0.017(2) -0.010(3) O23 0.059(5) 0.38(2) 0.171(9) 0.180(11) 0.029(5) 0.024(7) O24 0.146(9) 0.220(13) 0.212(11) 0.147(11) -0.049(8) -0.083(9) N1 0.072(4) 0.045(3) 0.038(3) 0.010(2) 0.020(3) -0.015(3) N2 0.122(6) 0.045(4) 0.053(3) -0.007(3) 0.007(4) -0.014(4) N3 0.030(3) 0.075(4) 0.043(3) -0.003(3) 0.010(2) -0.008(3) N4 0.073(4) 0.051(3) 0.047(3) 0.005(2) 0.030(3) -0.026(3) N5 0.085(5) 0.131(7) 0.059(4) 0.007(4) 0.041(4) 0.035(5) N6 0.039(3) 0.073(4) 0.038(3) -0.003(3) 0.010(2) 0.004(3) N7 0.105(6) 0.053(4) 0.070(4) 0.006(3) 0.037(4) 0.005(4) N8 0.114(6) 0.046(4) 0.092(5) 0.001(3) 0.058(5) 0.012(4) C131 0.039(4) 0.098(6) 0.051(4) 0.003(4) 0.016(3) 0.002(4) N10 0.068(4) 0.074(5) 0.083(5) -0.018(4) 0.017(4) 0.013(4) C1 0.016(2) 0.018(2) 0.035(2) 0.0033(18) 0.0112(18) -0.0003(16) C2 0.012(2) 0.022(2) 0.033(2) -0.0003(18) 0.0080(18) -0.0021(17) C3 0.020(2) 0.021(2) 0.042(3) -0.004(2) 0.017(2) -0.0032(18) C4 0.023(2) 0.029(3) 0.034(3) -0.003(2) 0.012(2) -0.0029(19) C5 0.013(2) 0.028(2) 0.042(3) 0.009(2) 0.0108(19) 0.0004(18) C6 0.020(2) 0.017(2) 0.047(3) 0.001(2) 0.012(2) -0.0044(17) C7 0.012(2) 0.020(2) 0.035(2) 0.0007(19) 0.0082(18) -0.0010(16) C8 0.011(2) 0.026(2) 0.037(3) -0.001(2) 0.0085(18) 0.0015(17) C9 0.018(2) 0.019(2) 0.034(2) -0.0016(18) 0.0139(18) 0.0037(17) C10 0.031(3) 0.012(2) 0.043(3) 0.0011(19) 0.022(2) -0.0005(18) C11 0.029(3) 0.017(2) 0.038(3) 0.0016(19) 0.015(2) 0.0065(18) C12 0.020(2) 0.026(2) 0.035(2) -0.009(2) 0.0117(19) 0.0059(18) C13 0.025(2) 0.015(2) 0.039(3) -0.0034(18) 0.019(2) -0.0023(17) C14 0.020(2) 0.017(2) 0.033(2) -0.0020(18) 0.0145(19) 0.0044(17) C15 0.029(2) 0.013(2) 0.041(3) -0.0006(19) 0.021(2) 0.0005(18) C16 0.021(2) 0.015(2) 0.036(2) 0.0052(18) 0.0150(19) -0.0010(17) C17 0.023(2) 0.016(2) 0.041(3) -0.0009(19) 0.020(2) -0.0024(17) C18 0.033(3) 0.018(2) 0.037(3) 0.0005(19) 0.019(2) -0.0039(19) C19 0.034(3) 0.017(2) 0.034(2) 0.0006(19) 0.019(2) -0.0014(18) C20 0.030(3) 0.014(2) 0.043(3) 0.0051(19) 0.024(2) 0.0032(18) C21 0.025(2) 0.016(2) 0.032(2) 0.0033(18) 0.0159(19) 0.0027(17) C22 0.044(3) 0.039(3) 0.050(3) -0.006(2) 0.031(3) 0.001(2) C23 0.024(2) 0.023(2) 0.040(3) 0.001(2) 0.018(2) 0.0013(18) C24 0.029(3) 0.029(3) 0.039(3) 0.008(2) 0.014(2) -0.004(2) C25 0.024(2) 0.029(3) 0.040(3) 0.005(2) 0.011(2) -0.0013(19) C26 0.032(3) 0.026(3) 0.048(3) 0.005(2) 0.017(2) -0.010(2) C27 0.035(3) 0.021(2) 0.041(3) 0.003(2) 0.020(2) -0.003(2) C28 0.053(4) 0.046(3) 0.029(3) 0.006(2) 0.016(2) -0.017(3) C29 0.039(3) 0.029(3) 0.048(3) 0.004(2) 0.019(2) -0.015(2) C30 0.056(4) 0.025(3) 0.040(3) 0.000(2) 0.030(3) -0.012(2) C31 0.039(3) 0.038(3) 0.068(4) 0.015(3) 0.031(3) 0.005(2) C32 0.054(4) 0.041(3) 0.077(4) 0.008(3) 0.042(3) -0.005(3) C33 0.073(5) 0.042(3) 0.055(4) 0.005(3) 0.045(3) -0.007(3) C34 0.044(3) 0.050(4) 0.036(3) 0.001(3) 0.012(2) -0.012(3) C35 0.059(4) 0.023(3) 0.058(3) 0.011(2) 0.035(3) 0.006(2) C36 0.027(2) 0.018(2) 0.039(3) -0.0015(19) 0.017(2) 0.0024(18) C37 0.024(2) 0.033(3) 0.040(3) -0.008(2) 0.015(2) 0.001(2) C38 0.027(3) 0.049(3) 0.042(3) -0.013(3) 0.015(2) 0.006(2) C39 0.027(3) 0.052(4) 0.049(3) -0.019(3) 0.020(2) 0.006(2) C40 0.022(3) 0.049(3) 0.038(3) -0.007(2) 0.013(2) -0.005(2) C41 0.031(3) 0.052(4) 0.030(3) -0.010(2) 0.011(2) -0.003(2) C42 0.027(3) 0.047(3) 0.041(3) -0.012(2) 0.018(2) 0.000(2) C43 0.026(3) 0.048(3) 0.044(3) -0.001(2) 0.019(2) 0.002(2) C44 0.018(3) 0.069(5) 0.099(6) -0.030(4) 0.003(3) 0.009(3) C45 0.032(4) 0.065(5) 0.132(8) -0.028(5) 0.000(4) 0.015(3) C46 0.022(3) 0.070(5) 0.068(4) 0.002(4) 0.009(3) 0.002(3) C47 0.032(3) 0.060(4) 0.050(3) 0.000(3) 0.017(3) 0.003(3) C48 0.027(3) 0.027(3) 0.046(3) -0.002(2) 0.014(2) -0.006(2) C49 0.028(2) 0.017(2) 0.038(3) 0.0039(19) 0.018(2) 0.0030(18) C50 0.025(2) 0.018(2) 0.046(3) -0.004(2) 0.020(2) -0.0001(17) C51 0.035(3) 0.023(2) 0.048(3) 0.006(2) 0.023(2) 0.006(2) C52 0.041(3) 0.030(3) 0.032(3) 0.000(2) 0.017(2) 0.005(2) C53 0.039(3) 0.020(2) 0.045(3) -0.007(2) 0.020(2) -0.002(2) C54 0.048(3) 0.017(2) 0.047(3) 0.000(2) 0.024(3) -0.003(2) C55 0.046(3) 0.022(3) 0.036(3) 0.000(2) 0.020(2) 0.001(2) C56 0.055(4) 0.023(3) 0.053(3) -0.012(2) 0.023(3) 0.001(2) C57 0.058(4) 0.042(3) 0.043(3) 0.000(3) 0.013(3) 0.003(3) C58 0.181(12) 0.050(5) 0.060(5) -0.017(4) 0.032(6) -0.016(6) C59 0.128(8) 0.043(4) 0.088(6) -0.031(4) 0.007(6) 0.034(5) C60 0.080(5) 0.044(4) 0.049(4) -0.012(3) 0.001(3) 0.025(4) C61 0.029(3) 0.018(2) 0.038(3) -0.009(2) 0.016(2) -0.0013(19) C62 0.026(2) 0.018(2) 0.034(2) -0.0046(18) 0.017(2) 0.0039(17) C63 0.022(2) 0.019(2) 0.041(3) -0.0046(19) 0.019(2) -0.0039(17) C64 0.032(3) 0.012(2) 0.040(3) -0.0003(18) 0.025(2) -0.0038(18) C65 0.029(3) 0.017(2) 0.046(3) -0.004(2) 0.018(2) -0.0010(19) C66 0.021(2) 0.021(2) 0.039(3) -0.0005(19) 0.019(2) -0.0003(17) C67 0.019(2) 0.012(2) 0.041(3) -0.0054(18) 0.0176(19) -0.0057(16) C68 0.020(2) 0.017(2) 0.036(2) 0.0035(19) 0.0134(19) -0.0006(17) C69 0.025(2) 0.018(2) 0.040(3) 0.0093(19) 0.018(2) 0.0021(18) C70 0.027(2) 0.020(2) 0.039(3) 0.0089(19) 0.018(2) 0.0012(18) C71 0.021(2) 0.027(3) 0.037(3) 0.005(2) 0.015(2) 0.0022(19) C72 0.032(3) 0.018(2) 0.044(3) 0.003(2) 0.018(2) -0.0042(19) C73 0.021(2) 0.022(2) 0.040(3) 0.000(2) 0.014(2) 0.0024(18) C74 0.018(2) 0.023(2) 0.038(3) 0.0022(19) 0.015(2) 0.0004(18) C75 0.016(2) 0.019(2) 0.042(3) -0.0005(19) 0.0119(19) -0.0015(17) C76 0.017(2) 0.019(2) 0.040(3) 0.0032(19) 0.0123(19) 0.0031(17) C77 0.017(2) 0.019(2) 0.038(3) -0.0019(19) 0.0073(19) -0.0014(17) C78 0.024(2) 0.023(2) 0.035(2) -0.0018(19) 0.012(2) 0.0030(18) C79 0.019(2) 0.022(2) 0.043(3) -0.004(2) 0.016(2) -0.0033(18) C80 0.024(2) 0.016(2) 0.035(2) -0.0003(18) 0.010(2) -0.0056(17) C81 0.016(2) 0.021(2) 0.037(2) -0.0054(19) 0.0133(19) -0.0001(17) C82 0.026(2) 0.017(2) 0.038(3) 0.0004(19) 0.017(2) -0.0017(17) C83 0.033(3) 0.023(2) 0.039(3) 0.000(2) 0.019(2) -0.009(2) C84 0.052(3) 0.021(2) 0.041(3) -0.005(2) 0.028(3) -0.008(2) C85 0.057(4) 0.019(2) 0.040(3) -0.002(2) 0.025(3) -0.006(2) C86 0.051(3) 0.022(3) 0.039(3) -0.001(2) 0.021(2) -0.015(2) C87 0.063(4) 0.030(3) 0.039(3) -0.008(2) 0.029(3) -0.012(3) C88 0.046(3) 0.023(3) 0.043(3) -0.004(2) 0.023(2) -0.008(2) C89 0.047(3) 0.036(3) 0.045(3) 0.008(2) 0.021(3) -0.012(3) C90 0.102(6) 0.038(4) 0.082(5) 0.024(3) 0.058(5) 0.016(4) C91 0.088(6) 0.046(4) 0.114(7) 0.039(4) 0.069(5) 0.022(4) C92 0.066(4) 0.051(4) 0.049(3) 0.016(3) 0.027(3) 0.000(3) C93 0.057(4) 0.037(3) 0.043(3) 0.002(2) 0.026(3) -0.013(3) C94 0.034(3) 0.019(3) 0.061(4) 0.000(2) 0.013(3) 0.005(2) C95 0.022(2) 0.010(2) 0.044(3) -0.0001(18) 0.013(2) -0.0003(17) C96 0.021(2) 0.021(2) 0.042(3) 0.0053(19) 0.015(2) 0.0010(17) C97 0.022(2) 0.053(3) 0.041(3) 0.014(2) 0.012(2) -0.004(2) C98 0.029(3) 0.051(3) 0.046(3) 0.014(3) 0.017(2) -0.005(2) C99 0.020(2) 0.025(2) 0.045(3) 0.007(2) 0.009(2) -0.0027(18) C100 0.027(3) 0.036(3) 0.037(3) 0.000(2) 0.007(2) -0.004(2) C101 0.027(3) 0.033(3) 0.044(3) 0.000(2) 0.020(2) -0.002(2) C102 0.025(3) 0.030(3) 0.049(3) 0.001(2) 0.011(2) -0.002(2) C103 0.038(3) 0.037(3) 0.064(4) 0.004(3) 0.018(3) -0.007(2) C104 0.036(3) 0.038(3) 0.082(5) -0.006(3) 0.020(3) -0.004(3) C105 0.031(3) 0.066(4) 0.049(3) -0.016(3) 0.009(3) -0.011(3) C106 0.033(3) 0.060(4) 0.039(3) -0.001(3) 0.012(2) -0.008(3) C107 0.043(3) 0.028(3) 0.067(4) -0.011(3) 0.032(3) 0.002(2) C108 0.024(2) 0.013(2) 0.036(2) -0.0008(18) 0.0136(19) -0.0023(17) C109 0.022(2) 0.021(2) 0.038(3) -0.0015(19) 0.0133(19) 0.0015(17) C110 0.031(3) 0.040(3) 0.043(3) 0.001(2) 0.012(2) 0.003(2) C111 0.041(3) 0.052(4) 0.034(3) 0.001(2) 0.013(2) 0.006(3) C112 0.044(3) 0.032(3) 0.039(3) -0.001(2) 0.019(2) 0.003(2) C113 0.028(3) 0.032(3) 0.039(3) 0.002(2) 0.011(2) 0.012(2) C114 0.031(3) 0.019(2) 0.040(3) -0.002(2) 0.012(2) 0.0038(19) C115 0.036(3) 0.045(3) 0.044(3) 0.005(2) 0.017(2) 0.012(2) C116 0.089(6) 0.068(5) 0.056(4) 0.006(3) 0.040(4) 0.040(4) C117 0.116(8) 0.106(7) 0.066(5) -0.012(5) 0.039(5) 0.064(6) C118 0.122(9) 0.147(10) 0.068(5) -0.011(6) 0.036(5) 0.088(8) C119 0.063(4) 0.059(4) 0.047(3) 0.006(3) 0.029(3) 0.026(3) C120 0.034(3) 0.024(2) 0.056(3) -0.003(2) 0.029(2) -0.003(2) C121 0.082(6) 0.079(6) 0.060(4) 0.010(4) 0.023(4) -0.010(4) C122 0.076(6) 0.088(7) 0.100(6) 0.021(5) 0.037(5) -0.018(5) C123 0.091(7) 0.073(6) 0.112(7) 0.004(5) 0.069(6) 0.005(5) C124 0.066(5) 0.071(5) 0.085(5) 0.000(4) 0.032(4) 0.001(4) C125 0.150(10) 0.106(8) 0.107(7) -0.018(6) 0.101(8) 0.004(7) C126 0.088(5) 0.059(4) 0.039(3) 0.002(3) 0.032(3) 0.005(4) C127 0.078(5) 0.056(4) 0.070(4) 0.003(4) 0.034(4) 0.008(4) C128 0.072(5) 0.072(5) 0.066(4) -0.006(4) 0.026(4) 0.006(4) C129 0.077(7) 0.124(9) 0.090(6) 0.030(6) 0.021(5) 0.008(6) C130 0.211(17) 0.051(6) 0.202(15) -0.007(7) 0.117(13) 0.015(8) N9 0.060(4) 0.072(4) 0.061(3) -0.007(3) 0.015(3) 0.000(3) C132 0.051(4) 0.072(5) 0.074(5) 0.005(4) 0.026(4) 0.011(4) C133 0.052(4) 0.068(5) 0.095(6) -0.023(4) 0.028(4) -0.021(4) C134 0.080(6) 0.055(5) 0.084(5) 0.007(4) 0.020(5) -0.005(4) O21 0.066(4) 0.139(6) 0.051(3) -0.005(3) 0.014(3) 0.007(4) C136 0.055(4) 0.064(4) 0.048(3) -0.011(3) 0.015(3) -0.004(3) C137 0.054(4) 0.068(5) 0.050(4) 0.000(3) 0.017(3) 0.011(3) C138 0.075(5) 0.070(5) 0.063(4) -0.005(4) 0.029(4) 0.007(4) C139 0.109(8) 0.070(6) 0.075(5) 0.025(4) 0.025(5) 0.019(5) C140 0.060(6) 0.097(8) 0.193(12) -0.039(8) 0.046(7) 0.013(5) C141 0.214(17) 0.110(10) 0.172(13) 0.049(9) 0.150(13) 0.070(11) C142 0.33(3) 0.145(14) 0.109(10) 0.047(10) 0.104(15) 0.070(17) C143 0.071(6) 0.099(8) 0.113(7) -0.043(6) 0.029(5) -0.029(5) C144 0.223(19) 0.112(11) 0.174(13) -0.038(10) 0.112(14) -0.082(12) C145 0.092(9) 0.112(11) 0.27(2) -0.066(13) 0.029(12) 0.014(8) C146 0.25(3) 0.118(13) 0.24(2) -0.022(14) -0.15(2) 0.070(15) C147 0.146(12) 0.165(13) 0.082(7) 0.014(7) 0.079(8) 0.020(9) C148 0.18(2) 0.32(3) 0.163(15) -0.105(19) 0.097(15) -0.14(2) _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 O1 C4 1.390(6) . ? O1 C22 1.471(7) . ? O2 C23 1.378(6) . ? O2 C5 1.442(6) . ? O3 C23 1.229(6) . ? O4 C11 1.390(6) . ? O4 C35 1.441(7) . ? O5 C36 1.384(6) . ? O5 C12 1.427(6) . ? O6 C36 1.217(6) . ? O7 C18 1.391(6) . ? O7 C48 1.440(6) . ? O8 C49 1.392(6) . ? O8 C19 1.422(6) . ? O9 C49 1.213(6) . ? O10 C82 1.378(6) . ? O10 C64 1.443(5) . ? O11 C82 1.213(6) . ? O12 C65 1.389(6) . ? O12 C94 1.451(7) . ? O13 C95 1.393(6) . ? O13 C71 1.414(6) . ? O14 C95 1.222(6) . ? O15 C72 1.388(6) . ? O15 C107 1.460(7) . ? O16 C108 1.398(6) . ? O16 C78 1.431(6) . ? O17 C108 1.210(6) . ? O18 C79 1.402(6) . ? O18 C120 1.450(6) . ? O19 C121 1.189(10) . ? O20 C126 1.247(10) . ? C135 N9 1.467(12) . ? O22 C136 1.266(9) . ? O23 C142 1.389(14) . ? O23 C143 1.524(14) . ? O24 C146 1.385(15) . ? O24 C147 1.518(14) . ? N1 C33 1.339(9) . ? N1 C34 1.386(8) . ? N2 C57 1.341(9) . ? N2 C58 1.371(14) . ? N3 C47 1.344(8) . ? N3 C46 1.370(9) . ? N4 C92 1.332(10) . ? N4 C93 1.390(7) . ? N5 C119 1.363(9) . ? N5 C118 1.382(13) . ? N6 C105 1.358(9) . ? N6 C106 1.369(8) . ? N7 C121 1.370(12) . ? N7 C125 1.443(13) . ? N7 C124 1.445(12) . ? N8 C126 1.387(11) . ? N8 C129 1.477(14) . ? N8 C130 1.496(14) . ? C131 O21 1.215(9) . ? C131 N9 1.326(11) . ? C131 C134 1.578(12) . ? N10 C136 1.360(10) . ? N10 C139 1.462(13) . ? N10 C140 1.471(13) . ? C1 C2 1.537(6) . ? C1 C21 1.549(6) . ? C2 C7 1.423(6) . ? C2 C3 1.432(7) . ? C3 C4 1.400(7) . ? C4 C5 1.397(7) . ? C5 C6 1.388(7) . ? C6 C7 1.425(7) . ? C7 C8 1.540(7) . ? C8 C9 1.554(6) . ? C9 C14 1.406(6) . ? C9 C10 1.415(6) . ? C10 C11 1.412(7) . ? C11 C12 1.420(7) . ? C12 C13 1.389(7) . ? C13 C14 1.437(6) . ? C14 C15 1.553(6) . ? C15 C16 1.538(6) . ? C16 C21 1.422(6) . ? C16 C17 1.427(6) . ? C17 C18 1.435(7) . ? C18 C19 1.403(7) . ? C19 C20 1.398(7) . ? C20 C21 1.414(6) . ? C23 C24 1.519(7) . ? C24 C25 1.408(7) . ? C24 C29 1.417(8) . ? C25 C26 1.412(7) . ? C26 C27 1.399(8) . ? C27 C28 1.420(8) . ? C27 C30 1.511(7) . ? C28 C29 1.414(7) . ? C30 C34 1.389(8) . ? C30 C31 1.439(8) . ? C31 C32 1.403(8) . ? C32 C33 1.413(10) . ? C36 C37 1.512(7) . ? C37 C42 1.412(7) . ? C37 C38 1.433(7) . ? C38 C39 1.402(8) . ? C39 C40 1.426(8) . ? C40 C41 1.424(8) . ? C40 C43 1.504(7) . ? C41 C42 1.382(8) . ? C43 C47 1.391(9) . ? C43 C44 1.397(9) . ? C44 C45 1.415(10) . ? C45 C46 1.378(11) . ? C49 C50 1.519(7) . ? C50 C51 1.411(7) . ? C50 C55 1.416(7) . ? C51 C52 1.401(7) . ? C52 C53 1.424(7) . ? C53 C54 1.404(8) . ? C53 C56 1.513(7) . ? C54 C55 1.433(7) . ? C56 C60 1.406(9) . ? C56 C57 1.438(9) . ? C58 C59 1.467(14) . ? C59 C60 1.403(10) . ? C61 C62 1.533(7) . ? C61 C81 1.538(6) . ? C62 C63 1.419(7) . ? C62 C67 1.426(6) . ? C63 C64 1.381(7) . ? C64 C65 1.422(7) . ? C65 C66 1.404(7) . ? C66 C67 1.425(7) . ? C67 C68 1.562(6) . ? C68 C69 1.531(7) . ? C69 C70 1.413(7) . ? C69 C74 1.422(7) . ? C70 C71 1.396(7) . ? C71 C72 1.426(7) . ? C72 C73 1.413(7) . ? C73 C74 1.433(7) . ? C74 C75 1.538(6) . ? C75 C76 1.523(7) . ? C76 C77 1.420(7) . ? C76 C81 1.443(6) . ? C77 C78 1.388(7) . ? C78 C79 1.431(7) . ? C79 C80 1.401(7) . ? C80 C81 1.405(7) . ? C82 C83 1.503(7) . ? C83 C84 1.412(7) . ? C83 C88 1.420(8) . ? C84 C85 1.415(7) . ? C85 C86 1.407(8) . ? C86 C87 1.447(7) . ? C86 C89 1.489(7) . ? C87 C88 1.383(8) . ? C89 C90 1.402(10) . ? C89 C93 1.409(9) . ? C90 C91 1.409(10) . ? C91 C92 1.406(11) . ? C95 C96 1.500(7) . ? C96 C101 1.404(7) . ? C96 C97 1.426(7) . ? C97 C98 1.406(8) . ? C98 C99 1.411(8) . ? C99 C100 1.419(8) . ? C99 C102 1.515(7) . ? C100 C101 1.400(7) . ? C102 C103 1.425(8) . ? C102 C106 1.432(8) . ? C103 C104 1.398(9) . ? C104 C105 1.372(10) . ? C108 C109 1.506(7) . ? C109 C110 1.403(8) . ? C109 C114 1.424(7) . ? C110 C111 1.374(8) . ? C111 C112 1.420(8) . ? C112 C113 1.433(7) . ? C112 C115 1.501(8) . ? C113 C114 1.395(7) . ? C115 C116 1.404(9) . ? C115 C119 1.419(9) . ? C116 C117 1.411(10) . ? C117 C118 1.359(15) . ? C121 C122 1.572(14) . ? C122 C123 1.511(14) . ? C123 C124 1.556(13) . ? C126 C127 1.541(12) . ? C127 C128 1.534(12) . ? C128 C129 1.490(14) . ? N9 C132 1.449(10) . ? C132 C133 1.580(12) . ? C133 C134 1.485(13) . ? C136 C137 1.520(11) . ? C137 C138 1.504(12) . ? C138 C139 1.581(14) . ? C141 C142 1.569(16) . ? C143 C144 1.534(15) . ? C145 C146 1.530(18) . ? C147 C148 1.498(17) . ? 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 C4 O1 C22 116.5(4) . . ? C23 O2 C5 115.1(4) . . ? C11 O4 C35 117.3(4) . . ? C36 O5 C12 116.0(4) . . ? C18 O7 C48 116.4(4) . . ? C49 O8 C19 114.2(4) . . ? C82 O10 C64 116.4(3) . . ? C65 O12 C94 117.9(4) . . ? C95 O13 C71 115.1(4) . . ? C72 O15 C107 117.5(4) . . ? C108 O16 C78 115.0(3) . . ? C79 O18 C120 116.2(4) . . ? C142 O23 C143 112.1(11) . . ? C146 O24 C147 116.5(13) . . ? C33 N1 C34 116.9(5) . . ? C57 N2 C58 117.8(7) . . ? C47 N3 C46 116.7(6) . . ? C92 N4 C93 117.1(6) . . ? C119 N5 C118 114.7(7) . . ? C105 N6 C106 115.1(5) . . ? C121 N7 C125 119.6(8) . . ? C121 N7 C124 115.8(8) . . ? C125 N7 C124 123.7(8) . . ? C126 N8 C129 110.8(7) . . ? C126 N8 C130 121.7(11) . . ? C129 N8 C130 125.1(10) . . ? O21 C131 N9 130.3(9) . . ? O21 C131 C134 123.6(8) . . ? N9 C131 C134 106.1(6) . . ? C136 N10 C139 114.3(7) . . ? C136 N10 C140 122.5(10) . . ? C139 N10 C140 122.2(9) . . ? C2 C1 C21 114.4(4) . . ? C7 C2 C3 119.2(4) . . ? C7 C2 C1 123.3(4) . . ? C3 C2 C1 117.3(4) . . ? C4 C3 C2 121.3(4) . . ? O1 C4 C5 115.6(4) . . ? O1 C4 C3 125.5(4) . . ? C5 C4 C3 118.8(4) . . ? C6 C5 C4 121.4(4) . . ? C6 C5 O2 119.8(4) . . ? C4 C5 O2 118.8(4) . . ? C5 C6 C7 121.2(4) . . ? C2 C7 C6 118.2(4) . . ? C2 C7 C8 123.1(4) . . ? C6 C7 C8 118.7(4) . . ? C7 C8 C9 115.8(4) . . ? C14 C9 C10 120.1(4) . . ? C14 C9 C8 122.3(4) . . ? C10 C9 C8 117.6(4) . . ? C11 C10 C9 121.5(4) . . ? O4 C11 C10 125.7(4) . . ? O4 C11 C12 116.4(4) . . ? C10 C11 C12 117.8(4) . . ? C13 C12 C11 121.5(4) . . ? C13 C12 O5 120.0(4) . . ? C11 C12 O5 118.4(4) . . ? C12 C13 C14 120.3(4) . . ? C9 C14 C13 118.8(4) . . ? C9 C14 C15 124.4(4) . . ? C13 C14 C15 116.8(4) . . ? C16 C15 C14 114.5(4) . . ? C21 C16 C17 119.9(4) . . ? C21 C16 C15 123.4(4) . . ? C17 C16 C15 116.6(4) . . ? C16 C17 C18 120.5(4) . . ? O7 C18 C19 116.6(4) . . ? O7 C18 C17 125.1(4) . . ? C19 C18 C17 118.3(4) . . ? C20 C19 C18 121.2(4) . . ? C20 C19 O8 120.0(4) . . ? C18 C19 O8 118.7(4) . . ? C19 C20 C21 121.5(4) . . ? C20 C21 C16 118.5(4) . . ? C20 C21 C1 119.1(4) . . ? C16 C21 C1 122.3(4) . . ? O3 C23 O2 123.1(4) . . ? O3 C23 C24 124.5(4) . . ? O2 C23 C24 112.3(4) . . ? C25 C24 C29 120.9(5) . . ? C25 C24 C23 117.5(4) . . ? C29 C24 C23 121.6(4) . . ? C24 C25 C26 119.6(5) . . ? C27 C26 C25 120.6(5) . . ? C26 C27 C28 119.4(4) . . ? C26 C27 C30 120.6(5) . . ? C28 C27 C30 119.9(5) . . ? C29 C28 C27 120.9(5) . . ? C28 C29 C24 118.5(5) . . ? C34 C30 C31 116.7(5) . . ? C34 C30 C27 122.1(5) . . ? C31 C30 C27 121.2(5) . . ? C32 C31 C30 119.7(6) . . ? C31 C32 C33 118.1(6) . . ? N1 C33 C32 124.0(5) . . ? N1 C34 C30 124.6(6) . . ? O6 C36 O5 123.8(4) . . ? O6 C36 C37 125.6(4) . . ? O5 C36 C37 110.5(4) . . ? C42 C37 C38 119.2(5) . . ? C42 C37 C36 122.4(4) . . ? C38 C37 C36 118.3(4) . . ? C39 C38 C37 119.0(5) . . ? C38 C39 C40 122.0(5) . . ? C41 C40 C39 117.2(5) . . ? C41 C40 C43 120.0(5) . . ? C39 C40 C43 122.8(5) . . ? C42 C41 C40 121.6(5) . . ? C41 C42 C37 120.9(5) . . ? C47 C43 C44 115.8(5) . . ? C47 C43 C40 122.0(5) . . ? C44 C43 C40 122.2(5) . . ? C43 C44 C45 120.7(7) . . ? C46 C45 C44 117.9(7) . . ? N3 C46 C45 122.9(6) . . ? N3 C47 C43 125.7(6) . . ? O9 C49 O8 124.0(4) . . ? O9 C49 C50 124.7(4) . . ? O8 C49 C50 111.3(4) . . ? C51 C50 C55 119.5(4) . . ? C51 C50 C49 122.6(4) . . ? C55 C50 C49 118.0(4) . . ? C52 C51 C50 120.8(4) . . ? C51 C52 C53 120.3(5) . . ? C54 C53 C52 119.5(4) . . ? C54 C53 C56 120.4(5) . . ? C52 C53 C56 120.1(5) . . ? C53 C54 C55 120.1(5) . . ? C50 C55 C54 119.8(5) . . ? C60 C56 C57 117.5(5) . . ? C60 C56 C53 121.6(5) . . ? C57 C56 C53 120.9(5) . . ? N2 C57 C56 123.7(6) . . ? N2 C58 C59 123.5(7) . . ? C60 C59 C58 115.7(7) . . ? C59 C60 C56 121.6(7) . . ? C62 C61 C81 114.9(4) . . ? C63 C62 C67 117.7(4) . . ? C63 C62 C61 119.0(4) . . ? C67 C62 C61 123.3(4) . . ? C64 C63 C62 121.5(4) . . ? C63 C64 C65 121.6(4) . . ? C63 C64 O10 120.3(4) . . ? C65 C64 O10 118.1(4) . . ? O12 C65 C66 125.5(4) . . ? O12 C65 C64 116.6(4) . . ? C66 C65 C64 117.9(4) . . ? C65 C66 C67 121.1(4) . . ? C66 C67 C62 120.2(4) . . ? C66 C67 C68 117.2(4) . . ? C62 C67 C68 122.6(4) . . ? C69 C68 C67 115.6(4) . . ? C70 C69 C74 117.8(4) . . ? C70 C69 C68 118.8(4) . . ? C74 C69 C68 123.2(4) . . ? C71 C70 C69 122.7(4) . . ? C70 C71 O13 121.8(4) . . ? C70 C71 C72 120.0(4) . . ? O13 C71 C72 118.2(4) . . ? O15 C72 C73 125.6(5) . . ? O15 C72 C71 115.9(4) . . ? C73 C72 C71 118.4(4) . . ? C72 C73 C74 121.1(4) . . ? C69 C74 C73 119.9(4) . . ? C69 C74 C75 123.3(4) . . ? C73 C74 C75 116.6(4) . . ? C76 C75 C74 115.1(4) . . ? C77 C76 C81 117.3(4) . . ? C77 C76 C75 118.8(4) . . ? C81 C76 C75 123.8(4) . . ? C78 C77 C76 121.8(4) . . ? C77 C78 C79 120.5(4) . . ? C77 C78 O16 120.9(4) . . ? C79 C78 O16 118.6(4) . . ? C80 C79 O18 125.6(4) . . ? C80 C79 C78 118.6(4) . . ? O18 C79 C78 115.8(4) . . ? C79 C80 C81 121.3(4) . . ? C80 C81 C76 120.4(4) . . ? C80 C81 C61 117.8(4) . . ? C76 C81 C61 121.7(4) . . ? O11 C82 O10 123.5(4) . . ? O11 C82 C83 126.1(4) . . ? O10 C82 C83 110.4(4) . . ? C84 C83 C88 118.9(4) . . ? C84 C83 C82 118.5(4) . . ? C88 C83 C82 122.6(4) . . ? C83 C84 C85 120.8(5) . . ? C86 C85 C84 121.0(5) . . ? C85 C86 C87 116.9(5) . . ? C85 C86 C89 123.4(5) . . ? C87 C86 C89 119.7(5) . . ? C88 C87 C86 122.2(5) . . ? C87 C88 C83 120.0(5) . . ? C90 C89 C93 116.9(5) . . ? C90 C89 C86 121.9(6) . . ? C93 C89 C86 121.1(6) . . ? C89 C90 C91 119.7(7) . . ? C92 C91 C90 119.0(7) . . ? N4 C92 C91 123.2(6) . . ? N4 C93 C89 124.0(6) . . ? O14 C95 O13 122.7(4) . . ? O14 C95 C96 125.9(4) . . ? O13 C95 C96 111.4(4) . . ? C101 C96 C97 118.6(4) . . ? C101 C96 C95 123.6(4) . . ? C97 C96 C95 117.8(4) . . ? C98 C97 C96 120.7(5) . . ? C97 C98 C99 120.1(5) . . ? C98 C99 C100 119.3(4) . . ? C98 C99 C102 119.5(5) . . ? C100 C99 C102 121.1(5) . . ? C101 C100 C99 120.3(5) . . ? C100 C101 C96 121.2(5) . . ? C103 C102 C106 115.5(5) . . ? C103 C102 C99 123.2(5) . . ? C106 C102 C99 121.2(5) . . ? C104 C103 C102 119.2(6) . . ? C105 C104 C103 119.8(6) . . ? N6 C105 C104 124.8(6) . . ? N6 C106 C102 125.4(6) . . ? O17 C108 O16 122.2(4) . . ? O17 C108 C109 126.8(4) . . ? O16 C108 C109 110.9(4) . . ? C110 C109 C114 118.5(5) . . ? C110 C109 C108 123.9(4) . . ? C114 C109 C108 117.5(4) . . ? C111 C110 C109 121.8(5) . . ? C110 C111 C112 120.7(5) . . ? C111 C112 C113 118.4(5) . . ? C111 C112 C115 121.5(5) . . ? C113 C112 C115 120.0(5) . . ? C114 C113 C112 120.0(5) . . ? C113 C114 C109 120.6(5) . . ? C116 C115 C119 117.5(6) . . ? C116 C115 C112 121.8(5) . . ? C119 C115 C112 120.6(5) . . ? C115 C116 C117 119.4(7) . . ? C118 C117 C116 118.2(8) . . ? C117 C118 N5 125.8(7) . . ? N5 C119 C115 124.2(6) . . ? O19 C121 N7 130.9(10) . . ? O19 C121 C122 123.6(9) . . ? N7 C121 C122 105.1(7) . . ? C123 C122 C121 105.2(8) . . ? C122 C123 C124 104.6(8) . . ? N7 C124 C123 102.5(7) . . ? O20 C126 N8 124.2(8) . . ? O20 C126 C127 129.2(7) . . ? N8 C126 C127 106.6(7) . . ? C128 C127 C126 105.0(7) . . ? C129 C128 C127 102.5(8) . . ? N8 C129 C128 105.5(7) . . ? C131 N9 C132 116.6(7) . . ? C131 N9 C135 123.4(7) . . ? C132 N9 C135 118.8(7) . . ? N9 C132 C133 101.1(6) . . ? C134 C133 C132 104.5(7) . . ? C133 C134 C131 104.2(7) . . ? O22 C136 N10 127.1(8) . . ? O22 C136 C137 126.1(7) . . ? N10 C136 C137 106.8(7) . . ? C138 C137 C136 106.7(6) . . ? C137 C138 C139 102.6(7) . . ? N10 C139 C138 102.2(6) . . ? O23 C142 C141 104.3(13) . . ? O23 C143 C144 108.2(9) . . ? O24 C146 C145 112.6(14) . . ? C148 C147 O24 106.0(11) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.96 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.432 _refine_diff_density_min -0.732 _refine_diff_density_rms 0.127 # Attachment '- complex1_new.CIF' data_complex1_new _database_code_depnum_ccdc_archive 'CCDC 822480' #TrackingRef '- complex1_new.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; diaquo(dimethylacetamide)trisnitroso [(+-)-2,7,12-trimethoxy-3,8,13-tris[4- (4-pyridyl)benzoyl]-10,15-dihydro-5H- tribenzo[a,d,g]cyclononane]cadmium(II) nitrate dimethylacetamide clathrate ; _chemical_name_common ; diaquo(dimethylacetamide)trisnitroso ((+-)-2,7,12-trimethoxy- 3,8,13-tris(4-(4-pyridyl)benzoyl)-10,15-dihydro-5H- tribenzo(a,d,g)cyclononane)cadmium(ii) nitrate dimethylacetamide clathrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H103 Cd2 N13 O29' _chemical_formula_weight 1983.59 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.8154(17) _cell_length_b 17.6539(19) _cell_length_c 23.970(3) _cell_angle_alpha 71.274(4) _cell_angle_beta 85.877(4) _cell_angle_gamma 66.204(4) _cell_volume 5786.7(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.138 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2052 _exptl_absorpt_coefficient_mu 0.435 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8769 _exptl_absorpt_correction_T_max 0.9416 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 X8 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 75397 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0626 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 26.34 _reflns_number_total 22616 _reflns_number_gt 13425 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour)' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One nitrate anion (N6, O16-O18) showed signs of disorder but a disorder model could not be satisfactorily refined. This anion was therefore refined with restrained bond lengths and a group Uiso. Some disordered groups (aquo ligands, pyridyl, solvent) were also refined isotropically. Large residual e-density peak is 1.1 A from Cd. ; _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^)+(0.1962P)^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 22616 _refine_ls_number_parameters 916 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1339 _refine_ls_R_factor_gt 0.0986 _refine_ls_wR_factor_ref 0.3126 _refine_ls_wR_factor_gt 0.2868 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.56441(5) -1.63905(4) 0.75358(4) 0.1080(3) Uani 1 1 d . . . O1 O 0.8808(3) -1.1302(3) 0.61786(18) 0.0547(10) Uani 1 1 d . . . N1 N 0.5897(3) -0.0682(3) 0.33120(18) 0.0452(10) Uani 1 1 d . . . C1 C 1.1433(4) -1.1204(4) 0.7084(2) 0.0493(13) Uani 1 1 d . . . H1A H 1.1970 -1.1052 0.6953 0.059 Uiso 1 1 calc R . . H1B H 1.1654 -1.1848 0.7217 0.059 Uiso 1 1 calc R . . Cd2 Cd 0.50759(3) 0.08173(3) 0.288936(17) 0.04862(17) Uani 1 1 d . . . O2 O 0.8486(3) -0.9765(3) 0.52873(17) 0.0544(10) Uani 1 1 d . . . N2 N 0.5785(4) -0.9155(4) 1.2010(2) 0.0664(15) Uani 1 1 d . . . C2 C 1.0700(4) -1.0799(4) 0.6569(2) 0.0473(13) Uani 1 1 d . . . O3 O 0.9565(3) -0.6375(2) 0.55009(17) 0.0530(10) Uani 1 1 d . . . N3 N 0.6290(4) -1.5395(3) 0.7085(2) 0.0661(14) Uani 1 1 d . A . C3 C 1.0106(4) -1.1220(4) 0.6571(3) 0.0512(14) Uani 1 1 d . . . H3 H 1.0194 -1.1754 0.6872 0.061 Uiso 1 1 calc R . . O4 O 0.9827(3) -0.6389(3) 0.65942(19) 0.0588(11) Uani 1 1 d . . . N4 N 0.3344(4) 0.1212(5) 0.2365(3) 0.0731(16) Uani 1 1 d . . . C4 C 0.9396(4) -1.0856(3) 0.6136(2) 0.0442(12) Uani 1 1 d . . . O5 O 0.9623(3) -0.9968(4) 0.89740(17) 0.0733(13) Uani 1 1 d . . . N5 N 0.5949(4) 0.1789(4) 0.3174(3) 0.0680(15) Uani 1 1 d . . . C5 C 0.9227(4) -1.0060(4) 0.5685(2) 0.0453(13) Uani 1 1 d . . . O6 O 0.9562(4) -1.1395(4) 0.8828(2) 0.0858(15) Uani 1 1 d . . . O20B O 0.6437(11) -1.6623(10) 0.8459(7) 0.131(5) Uiso 0.50 1 d P A 2 C6 C 0.9828(4) -0.9664(3) 0.5673(2) 0.0451(13) Uani 1 1 d . . . H6 H 0.9742 -0.9135 0.5366 0.054 Uiso 1 1 calc R . . O7 O 0.9699(3) -1.2014(3) 0.55744(17) 0.0606(11) Uani 1 1 d . . . C7 C 1.0567(4) -1.0025(3) 0.6106(2) 0.0405(11) Uani 1 1 d . . . O8 O 0.8186(3) -0.6426(3) 0.5808(2) 0.0663(12) Uani 1 1 d . . . N8 N 0.3824(4) 0.0742(4) 0.4637(2) 0.0618(14) Uani 1 1 d . . . C8 C 1.1231(4) -0.9573(3) 0.6030(2) 0.0410(12) Uani 1 1 d . . . H8A H 1.1821 -0.9995 0.6260 0.049 Uiso 1 1 calc R . . H8B H 1.1365 -0.9405 0.5608 0.049 Uiso 1 1 calc R . . O9 O 0.8303(4) -0.9289(5) 0.8405(2) 0.125(3) Uani 1 1 d . . . N9 N 0.7834(4) -1.8655(3) 0.7124(2) 0.0573(12) Uani 1 1 d . A . C9 C 1.0868(4) -0.8764(3) 0.6223(2) 0.0393(11) Uani 1 1 d . . . O10 O 0.3934(3) 0.0419(3) 0.2511(2) 0.0709(12) Uani 1 1 d . . . C10 C 1.0346(4) -0.7953(3) 0.5803(2) 0.0429(12) Uani 1 1 d . . . H10 H 1.0215 -0.7930 0.5416 0.051 Uiso 1 1 calc R . . O11 O 0.3562(4) 0.1792(3) 0.2398(3) 0.0825(15) Uani 1 1 d . . . C11 C 1.0022(4) -0.7189(4) 0.5945(3) 0.0483(13) Uani 1 1 d . . . O12 O 0.2548(5) 0.1372(4) 0.2181(3) 0.122(2) Uani 1 1 d . . . C12 C 1.0188(4) -0.7202(4) 0.6517(2) 0.0478(13) Uani 1 1 d . . . O13 O 0.5184(4) 0.2131(3) 0.2854(2) 0.0741(13) Uani 1 1 d . . . C13 C 1.0682(4) -0.7994(4) 0.6929(2) 0.0467(13) Uani 1 1 d . . . H13 H 1.0795 -0.8008 0.7317 0.056 Uiso 1 1 calc R . . O14 O 0.6371(3) 0.0958(3) 0.3318(2) 0.0627(11) Uani 1 1 d . . . C14 C 1.1026(4) -0.8778(3) 0.6802(2) 0.0414(12) Uani 1 1 d . . . O15 O 0.6269(4) 0.2214(4) 0.3325(3) 0.110(2) Uani 1 1 d . . . C15 C 1.1591(4) -0.9627(4) 0.7295(2) 0.0477(13) Uani 1 1 d . . . H15A H 1.2072 -1.0022 0.7112 0.057 Uiso 1 1 calc R . . H15B H 1.1913 -0.9482 0.7559 0.057 Uiso 1 1 calc R . . O16 O 0.4944(10) -1.6515(9) 0.6737(6) 0.228(3) Uiso 1 1 d D A . C16 C 1.1039(4) -1.0125(4) 0.7675(2) 0.0433(12) Uani 1 1 d . . . O17 O 0.4105(10) -1.5190(9) 0.6909(6) 0.228(3) Uiso 1 1 d D A . C17 C 1.0562(4) -0.9824(4) 0.8131(2) 0.0518(14) Uani 1 1 d . . . H17 H 1.0570 -0.9317 0.8185 0.062 Uiso 1 1 calc R . . C18 C 1.0086(5) -1.0264(5) 0.8497(2) 0.0595(16) Uani 1 1 d . . . O19 O 0.6890(4) -1.7458(3) 0.7321(2) 0.0795(14) Uani 1 1 d . A . C19 C 1.0054(5) -1.1006(5) 0.8437(2) 0.0680(19) Uani 1 1 d . . . O20A O 0.5191(12) -1.5689(11) 0.8247(7) 0.141(5) Uiso 0.50 1 d P A 1 C20 C 1.0523(5) -1.1304(4) 0.7986(2) 0.0609(16) Uani 1 1 d . . . H20 H 1.0517 -1.1815 0.7938 0.073 Uiso 1 1 calc R . . C21 C 1.1011(4) -1.0856(4) 0.7598(2) 0.0499(13) Uani 1 1 d . . . O25 O 0.4475(3) 0.0885(3) 0.37693(17) 0.0595(11) Uani 1 1 d . . . C22 C 0.9069(4) -1.1917(4) 0.5894(2) 0.0488(13) Uani 1 1 d . . . O23 O 0.4517(8) -0.2132(7) 0.4790(5) 0.072(3) Uiso 0.50 1 d P B 1 C23 C 0.8236(4) -0.8902(4) 0.4869(3) 0.0588(15) Uani 1 1 d . . . H23A H 0.8091 -0.8478 0.5081 0.088 Uiso 1 1 calc R . . H23B H 0.7693 -0.8755 0.4619 0.088 Uiso 1 1 calc R . . H23C H 0.8755 -0.8887 0.4623 0.088 Uiso 1 1 calc R . . O24A O 0.5159(10) -1.7185(9) 0.8372(6) 0.114(4) Uiso 0.50 1 d P A 1 O24B O 0.4720(12) -1.7135(10) 0.7960(7) 0.140(5) Uiso 0.50 1 d P A 2 C24 C 0.8614(4) -0.6039(4) 0.5499(3) 0.0510(14) Uani 1 1 d . . . C25 C 1.0067(7) -0.6331(5) 0.7127(3) 0.094(3) Uani 1 1 d . . . H25A H 0.9775 -0.6621 0.7450 0.141 Uiso 1 1 calc R . . H25B H 0.9852 -0.5715 0.7098 0.141 Uiso 1 1 calc R . . H25C H 1.0742 -0.6616 0.7204 0.141 Uiso 1 1 calc R . . C26 C 0.8688(6) -0.9512(6) 0.8873(3) 0.079(2) Uani 1 1 d . . . C27 C 0.9462(7) -1.2124(7) 0.8752(4) 0.108(3) Uani 1 1 d . . . H27A H 0.9128 -1.1943 0.8371 0.163 Uiso 1 1 calc R . . H27B H 0.9113 -1.2344 0.9071 0.163 Uiso 1 1 calc R . . H27C H 1.0076 -1.2587 0.8763 0.163 Uiso 1 1 calc R . . C28 C 0.8508(4) -1.2445(3) 0.6061(2) 0.0467(13) Uani 1 1 d . . . C29 C 0.7911(4) -1.2388(4) 0.6516(3) 0.0537(14) Uani 1 1 d . . . H29 H 0.7817 -1.1968 0.6708 0.064 Uiso 1 1 calc R . . C30 C 0.7445(4) -1.2955(4) 0.6693(3) 0.0555(15) Uani 1 1 d . . . H30 H 0.7029 -1.2909 0.6999 0.067 Uiso 1 1 calc R . . C31 C 0.7594(4) -1.3584(3) 0.6418(2) 0.0479(13) Uani 1 1 d . . . C32 C 0.8189(5) -1.3633(4) 0.5963(3) 0.0562(15) Uani 1 1 d . . . H32 H 0.8279 -1.4049 0.5769 0.067 Uiso 1 1 calc R . . C33 C 0.8662(5) -1.3075(4) 0.5786(3) 0.0580(16) Uani 1 1 d . . . H33 H 0.9081 -1.3126 0.5482 0.070 Uiso 1 1 calc R . . C34 C 0.7126(4) -1.4199(4) 0.6644(3) 0.0519(14) Uani 1 1 d . . . C35 C 0.6251(5) -1.3962(4) 0.6868(3) 0.0677(18) Uani 1 1 d . A . H35 H 0.5924 -1.3382 0.6878 0.081 Uiso 1 1 calc R . . C36 C 0.5857(5) -1.4560(5) 0.7075(3) 0.074(2) Uani 1 1 d . . . H36 H 0.5255 -1.4374 0.7216 0.089 Uiso 1 1 calc R A . C37 C 0.7144(5) -1.5646(4) 0.6878(3) 0.0672(18) Uani 1 1 d . . . H37 H 0.7474 -1.6239 0.6898 0.081 Uiso 1 1 calc R A . C38 C 0.7544(5) -1.5068(4) 0.6641(3) 0.0621(17) Uani 1 1 d . A . H38 H 0.8121 -1.5258 0.6469 0.075 Uiso 1 1 calc R . . C39 C 0.8193(4) -0.5131(3) 0.5088(2) 0.0486(13) Uani 1 1 d . . . C40 C 0.7244(4) -0.4678(4) 0.5092(3) 0.0535(14) Uani 1 1 d . . . H40 H 0.6894 -0.4955 0.5350 0.064 Uiso 1 1 calc R . . C41 C 0.6800(4) -0.3820(4) 0.4722(3) 0.0584(15) Uani 1 1 d . . . H41 H 0.6149 -0.3518 0.4724 0.070 Uiso 1 1 calc R . . C42 C 0.7318(4) -0.3399(4) 0.4342(3) 0.0505(13) Uani 1 1 d . . . C43 C 0.8285(4) -0.3857(4) 0.4355(3) 0.0537(14) Uani 1 1 d . . . H43 H 0.8648 -0.3578 0.4116 0.064 Uiso 1 1 calc R . . C44 C 0.8706(4) -0.4718(4) 0.4719(3) 0.0503(13) Uani 1 1 d . . . H44 H 0.9355 -0.5029 0.4716 0.060 Uiso 1 1 calc R . . C45 C 0.6840(4) -0.2470(3) 0.3976(2) 0.0463(13) Uani 1 1 d . . . C46 C 0.5966(5) -0.2158(4) 0.3675(3) 0.0670(18) Uani 1 1 d . . . H46 H 0.5686 -0.2546 0.3683 0.080 Uiso 1 1 calc R . . C47 C 0.5530(4) -0.1276(4) 0.3371(3) 0.0578(15) Uani 1 1 d . . . H47 H 0.4930 -0.1071 0.3189 0.069 Uiso 1 1 calc R . . C48 C 0.6741(4) -0.1001(4) 0.3591(3) 0.0532(14) Uani 1 1 d . . . H48 H 0.7015 -0.0603 0.3567 0.064 Uiso 1 1 calc R . . C49 C 0.7232(4) -0.1872(3) 0.3909(2) 0.0480(13) Uani 1 1 d . . . H49 H 0.7835 -0.2060 0.4080 0.058 Uiso 1 1 calc R . . C50 C 0.8232(6) -0.9393(5) 0.9423(3) 0.076(2) Uani 1 1 d . . . C51 C 0.7287(7) -0.8828(7) 0.9373(3) 0.132(4) Uani 1 1 d . . . H51 H 0.6969 -0.8534 0.8993 0.158 Uiso 1 1 calc R . . C52 C 0.6813(8) -0.8693(8) 0.9861(4) 0.136(5) Uani 1 1 d . . . H52 H 0.6201 -0.8257 0.9819 0.164 Uiso 1 1 calc R . . C53 C 0.7259(6) -0.9219(6) 1.0426(3) 0.083(2) Uani 1 1 d . C . C54 C 0.8181(6) -0.9729(8) 1.0466(3) 0.114(4) Uani 1 1 d . . . H54 H 0.8497 -1.0034 1.0846 0.137 Uiso 1 1 calc R . . C55 C 0.8671(6) -0.9817(7) 0.9978(3) 0.098(3) Uani 1 1 d . . . H55 H 0.9316 -1.0174 1.0024 0.118 Uiso 1 1 calc R . . C56 C 0.6742(5) -0.9163(6) 1.0973(3) 0.077(2) Uani 1 1 d . . . C57A C 0.6179(15) -0.8464(14) 1.1065(9) 0.106(6) Uiso 0.50 1 d P C 2 H57A H 0.6094 -0.7916 1.0780 0.127 Uiso 0.50 1 calc PR C 2 C57B C 0.6955(10) -0.8835(8) 1.1357(5) 0.060(3) Uiso 0.50 1 d P C 1 H57B H 0.7428 -0.8620 1.1275 0.072 Uiso 0.50 1 calc PR C 1 C58A C 0.5669(16) -0.8478(15) 1.1588(9) 0.113(6) Uiso 0.50 1 d P C 2 H58A H 0.5215 -0.7940 1.1614 0.136 Uiso 0.50 1 calc PR C 2 C58B C 0.6474(10) -0.8810(8) 1.1884(6) 0.063(3) Uiso 0.50 1 d P C 1 H58B H 0.6613 -0.8566 1.2147 0.075 Uiso 0.50 1 calc PR C 1 C59A C 0.6345(8) -0.9935(7) 1.1912(5) 0.046(2) Uiso 0.50 1 d P C 2 H59A H 0.6392 -1.0462 1.2209 0.055 Uiso 0.50 1 calc PR C 2 C59B C 0.5464(14) -0.9183(11) 1.1581(8) 0.096(5) Uiso 0.50 1 d P C 1 H59B H 0.4874 -0.9209 1.1601 0.115 Uiso 0.50 1 calc PR C 1 C60A C 0.6833(8) -1.0008(7) 1.1423(5) 0.047(2) Uiso 0.50 1 d P C 2 H60A H 0.7204 -1.0557 1.1374 0.056 Uiso 0.50 1 calc PR C 2 C60B C 0.5926(17) -0.9179(14) 1.1028(10) 0.122(7) Uiso 0.50 1 d P C 1 H60B H 0.5622 -0.9188 1.0703 0.146 Uiso 0.50 1 calc PR C 1 C65 C 0.7078(5) -1.8210(5) 0.7323(3) 0.0628(16) Uani 1 1 d . . . C66 C 0.6388(6) -1.8615(5) 0.7566(4) 0.094(3) Uani 1 1 d . A . H66A H 0.6718 -1.9210 0.7833 0.141 Uiso 1 1 calc R . . H66B H 0.6066 -1.8633 0.7239 0.141 Uiso 1 1 calc R . . H66C H 0.5936 -1.8263 0.7782 0.141 Uiso 1 1 calc R . . C67 C 0.8549(5) -1.8316(5) 0.6949(4) 0.085(2) Uani 1 1 d . . . H67A H 0.8411 -1.7930 0.6539 0.127 Uiso 1 1 calc R A . H67B H 0.9152 -1.8804 0.6985 0.127 Uiso 1 1 calc R . . H67C H 0.8564 -1.7987 0.7206 0.127 Uiso 1 1 calc R . . C68 C 0.8119(6) -1.9590(5) 0.7165(4) 0.087(2) Uani 1 1 d . . . H68A H 0.7721 -1.9830 0.7427 0.130 Uiso 1 1 calc R A . H68B H 0.8765 -1.9926 0.7323 0.130 Uiso 1 1 calc R . . H68C H 0.8059 -1.9626 0.6771 0.130 Uiso 1 1 calc R . . C69 C 0.3988(4) 0.0577(4) 0.4134(3) 0.0580(16) Uani 1 1 d . . . C70 C 0.3589(5) 0.0022(5) 0.4000(3) 0.0622(16) Uani 1 1 d . . . H70A H 0.3634 0.0075 0.3580 0.093 Uiso 1 1 calc R . . H70B H 0.2937 0.0212 0.4092 0.093 Uiso 1 1 calc R . . H70C H 0.3932 -0.0588 0.4239 0.093 Uiso 1 1 calc R . . C71 C 0.4165(5) 0.1357(5) 0.4752(3) 0.0692(18) Uani 1 1 d . . . H71A H 0.4582 0.1484 0.4448 0.104 Uiso 1 1 calc R . . H71B H 0.4499 0.1090 0.5141 0.104 Uiso 1 1 calc R . . H71C H 0.3637 0.1901 0.4741 0.104 Uiso 1 1 calc R . . C72 C 0.3263(6) 0.0424(6) 0.5085(3) 0.087(2) Uani 1 1 d . . . H72A H 0.2670 0.0907 0.5083 0.130 Uiso 1 1 calc R . . H72B H 0.3593 0.0185 0.5474 0.130 Uiso 1 1 calc R . . H72C H 0.3151 -0.0035 0.4998 0.130 Uiso 1 1 calc R . . C73 C 0.4609(15) -0.3609(14) 0.5687(9) 0.095(6) Uiso 0.50 1 d P B 1 H73A H 0.5065 -0.3361 0.5681 0.143 Uiso 0.50 1 calc PR B 1 H73B H 0.4925 -0.4246 0.5796 0.143 Uiso 0.50 1 calc PR B 1 H73C H 0.4158 -0.3455 0.5978 0.143 Uiso 0.50 1 calc PR B 1 C74 C 0.3366(19) -0.3639(16) 0.5171(11) 0.134(8) Uiso 0.50 1 d P B 1 H74A H 0.3608 -0.4252 0.5423 0.201 Uiso 0.50 1 calc PR B 1 H74B H 0.3186 -0.3598 0.4776 0.201 Uiso 0.50 1 calc PR B 1 H74C H 0.2825 -0.3295 0.5342 0.201 Uiso 0.50 1 calc PR B 1 C75 C 0.3517(8) -0.2295(7) 0.4142(5) 0.122(3) Uiso 0.50 1 d P B 1 H75A H 0.3505 -0.1754 0.3849 0.183 Uiso 0.50 1 calc PR B 1 H75B H 0.2881 -0.2230 0.4231 0.183 Uiso 0.50 1 calc PR B 1 H75C H 0.3814 -0.2781 0.3983 0.183 Uiso 0.50 1 calc PR B 1 C76 C 0.4057(13) -0.2478(12) 0.4702(8) 0.081(5) Uiso 0.50 1 d P B 1 N10 N 0.4148(12) -0.3270(11) 0.5124(8) 0.101(5) Uiso 0.50 1 d P B 1 C76B C 0.4309(13) -0.2669(12) 0.5049(8) 0.082(4) Uiso 0.50 1 d P D 2 C73B C 0.4721(17) -0.3301(15) 0.5715(10) 0.112(7) Uiso 0.50 1 d P D 2 H73D H 0.4236 -0.3455 0.5936 0.168 Uiso 0.50 1 calc PR D 2 H73E H 0.4932 -0.2995 0.5912 0.168 Uiso 0.50 1 calc PR D 2 H73F H 0.5243 -0.3833 0.5698 0.168 Uiso 0.50 1 calc PR D 2 C74B C 0.4069(17) -0.3988(13) 0.4979(9) 0.114(6) Uiso 0.50 1 d P D 2 H74D H 0.4680 -0.4343 0.4879 0.171 Uiso 0.50 1 calc PR D 2 H74E H 0.3588 -0.4020 0.4763 0.171 Uiso 0.50 1 calc PR D 2 H74F H 0.4010 -0.4209 0.5404 0.171 Uiso 0.50 1 calc PR D 2 N10B N 0.3943(16) -0.2931(17) 0.4789(11) 0.129(7) Uiso 0.50 1 d P D 2 O23B O 0.4181(11) -0.1930(10) 0.4911(7) 0.108(5) Uiso 0.50 1 d P D 2 C75B C 0.3517(8) -0.2295(7) 0.4142(5) 0.122(3) Uiso 0.50 1 d P D 2 H75D H 0.2949 -0.1805 0.4170 0.183 Uiso 0.50 1 calc PR D 2 H75E H 0.3373 -0.2617 0.3924 0.183 Uiso 0.50 1 calc PR D 2 H75F H 0.3967 -0.2071 0.3934 0.183 Uiso 0.50 1 calc PR D 2 N6 N 0.4413(12) -1.5747(11) 0.6597(8) 0.228(3) Uiso 1 1 d D . . O18 O 0.3697(10) -1.5540(9) 0.6253(6) 0.228(3) Uiso 1 1 d D A . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0876(5) 0.0815(4) 0.1661(7) -0.0459(4) 0.0591(5) -0.0484(4) O1 0.053(2) 0.069(2) 0.067(2) -0.041(2) 0.023(2) -0.037(2) N1 0.046(3) 0.053(2) 0.043(2) -0.0202(19) 0.010(2) -0.025(2) C1 0.053(4) 0.050(3) 0.050(3) -0.019(2) 0.010(3) -0.025(3) Cd2 0.0471(3) 0.0540(3) 0.0469(3) -0.02100(18) 0.01854(19) -0.0213(2) O2 0.046(2) 0.067(2) 0.059(2) -0.0227(19) 0.004(2) -0.029(2) N2 0.065(4) 0.082(4) 0.048(3) -0.022(3) 0.012(3) -0.025(3) C2 0.042(3) 0.059(3) 0.049(3) -0.028(3) 0.016(3) -0.022(3) O3 0.043(2) 0.052(2) 0.060(2) -0.0120(18) 0.0076(19) -0.0204(19) N3 0.067(4) 0.058(3) 0.074(3) -0.022(3) 0.020(3) -0.028(3) C3 0.060(4) 0.050(3) 0.057(3) -0.029(3) 0.027(3) -0.031(3) O4 0.055(3) 0.058(2) 0.075(3) -0.035(2) 0.013(2) -0.025(2) N4 0.052(4) 0.085(4) 0.074(4) -0.030(3) 0.001(3) -0.015(4) C4 0.046(3) 0.054(3) 0.053(3) -0.031(3) 0.016(3) -0.032(3) O5 0.059(3) 0.129(4) 0.038(2) -0.034(2) 0.019(2) -0.041(3) N5 0.063(4) 0.060(3) 0.099(4) -0.043(3) 0.036(3) -0.033(3) C5 0.040(3) 0.056(3) 0.051(3) -0.031(3) 0.013(3) -0.021(3) O6 0.095(4) 0.117(4) 0.061(3) -0.021(3) 0.033(3) -0.067(4) C6 0.046(3) 0.051(3) 0.044(3) -0.023(2) 0.016(3) -0.022(3) O7 0.079(3) 0.075(3) 0.055(2) -0.037(2) 0.029(2) -0.050(3) C7 0.040(3) 0.049(3) 0.036(3) -0.015(2) 0.012(2) -0.022(2) O8 0.049(3) 0.067(3) 0.076(3) -0.007(2) 0.010(2) -0.031(2) N8 0.055(3) 0.080(3) 0.050(3) -0.017(2) 0.018(2) -0.031(3) C8 0.040(3) 0.054(3) 0.034(2) -0.018(2) 0.010(2) -0.021(3) O9 0.083(4) 0.193(7) 0.039(3) -0.029(3) 0.002(3) -0.003(4) N9 0.049(3) 0.070(3) 0.060(3) -0.026(2) 0.011(2) -0.030(3) C9 0.036(3) 0.055(3) 0.039(3) -0.023(2) 0.014(2) -0.026(3) O10 0.065(3) 0.076(3) 0.067(3) -0.016(2) -0.004(2) -0.028(3) C10 0.044(3) 0.057(3) 0.038(3) -0.018(2) 0.012(2) -0.029(3) O11 0.064(3) 0.074(3) 0.115(4) -0.049(3) -0.002(3) -0.018(3) C11 0.037(3) 0.049(3) 0.061(3) -0.018(3) 0.007(3) -0.019(3) O12 0.078(4) 0.110(5) 0.169(7) -0.028(4) -0.031(4) -0.035(4) C12 0.044(3) 0.055(3) 0.053(3) -0.024(3) 0.009(3) -0.025(3) O13 0.056(3) 0.063(3) 0.100(4) -0.030(3) 0.025(3) -0.020(2) C13 0.043(3) 0.065(3) 0.048(3) -0.028(3) 0.011(3) -0.031(3) O14 0.050(3) 0.062(3) 0.079(3) -0.030(2) 0.019(2) -0.021(2) C14 0.033(3) 0.060(3) 0.041(3) -0.019(2) 0.009(2) -0.028(3) O15 0.086(4) 0.100(4) 0.195(7) -0.098(4) 0.043(4) -0.053(4) C15 0.040(3) 0.065(3) 0.046(3) -0.024(3) 0.009(2) -0.025(3) C16 0.039(3) 0.061(3) 0.028(2) -0.013(2) 0.007(2) -0.020(3) C17 0.044(3) 0.074(4) 0.037(3) -0.022(3) 0.007(3) -0.022(3) C18 0.059(4) 0.090(4) 0.031(3) -0.022(3) 0.011(3) -0.030(4) O19 0.077(3) 0.070(3) 0.101(4) -0.028(3) 0.028(3) -0.042(3) C19 0.069(5) 0.104(5) 0.036(3) -0.013(3) 0.015(3) -0.049(4) C20 0.067(4) 0.079(4) 0.040(3) -0.010(3) 0.004(3) -0.041(4) C21 0.045(3) 0.060(3) 0.048(3) -0.015(3) 0.010(3) -0.028(3) O25 0.059(3) 0.081(3) 0.057(2) -0.036(2) 0.030(2) -0.040(2) C22 0.056(4) 0.049(3) 0.044(3) -0.015(2) 0.002(3) -0.023(3) C23 0.052(4) 0.062(4) 0.064(4) -0.022(3) -0.004(3) -0.023(3) C24 0.054(4) 0.047(3) 0.057(3) -0.017(3) 0.010(3) -0.026(3) C25 0.148(9) 0.075(5) 0.078(5) -0.046(4) 0.013(5) -0.048(5) C26 0.074(5) 0.112(6) 0.051(4) -0.033(4) 0.014(4) -0.033(5) C27 0.114(8) 0.125(7) 0.093(6) -0.013(5) 0.047(6) -0.077(7) C28 0.047(3) 0.051(3) 0.047(3) -0.021(2) 0.009(3) -0.021(3) C29 0.061(4) 0.051(3) 0.058(3) -0.026(3) 0.016(3) -0.027(3) C30 0.052(4) 0.052(3) 0.065(4) -0.022(3) 0.022(3) -0.023(3) C31 0.049(3) 0.048(3) 0.053(3) -0.019(2) 0.012(3) -0.026(3) C32 0.070(4) 0.060(3) 0.055(3) -0.028(3) 0.017(3) -0.037(3) C33 0.071(4) 0.077(4) 0.051(3) -0.035(3) 0.025(3) -0.046(4) C34 0.047(3) 0.053(3) 0.061(3) -0.024(3) 0.011(3) -0.023(3) C35 0.056(4) 0.055(3) 0.090(5) -0.022(3) 0.013(4) -0.022(3) C36 0.045(4) 0.072(4) 0.102(5) -0.027(4) 0.027(4) -0.024(3) C37 0.064(4) 0.062(4) 0.091(5) -0.036(3) 0.023(4) -0.036(4) C38 0.070(4) 0.056(3) 0.075(4) -0.032(3) 0.032(3) -0.036(3) C39 0.047(3) 0.047(3) 0.055(3) -0.019(2) 0.007(3) -0.022(3) C40 0.045(3) 0.049(3) 0.066(4) -0.013(3) 0.006(3) -0.024(3) C41 0.036(3) 0.064(4) 0.077(4) -0.017(3) 0.007(3) -0.028(3) C42 0.048(3) 0.049(3) 0.060(3) -0.014(3) 0.008(3) -0.028(3) C43 0.047(4) 0.060(3) 0.059(3) -0.023(3) 0.012(3) -0.025(3) C44 0.037(3) 0.056(3) 0.065(4) -0.026(3) 0.011(3) -0.022(3) C45 0.036(3) 0.048(3) 0.052(3) -0.019(2) 0.007(2) -0.013(3) C46 0.062(4) 0.064(4) 0.086(5) -0.018(3) 0.002(4) -0.040(4) C47 0.043(3) 0.059(4) 0.067(4) -0.016(3) -0.006(3) -0.019(3) C48 0.046(4) 0.067(4) 0.061(3) -0.029(3) 0.021(3) -0.032(3) C49 0.040(3) 0.047(3) 0.056(3) -0.011(2) 0.007(3) -0.021(3) C50 0.073(5) 0.101(5) 0.053(4) -0.026(4) 0.024(4) -0.035(4) C51 0.108(8) 0.160(9) 0.041(4) -0.002(5) 0.017(5) 0.004(7) C52 0.117(9) 0.146(9) 0.071(5) -0.014(5) 0.037(6) 0.000(7) C53 0.085(6) 0.132(7) 0.050(4) -0.040(4) 0.023(4) -0.055(5) C54 0.061(5) 0.217(11) 0.042(4) -0.049(5) 0.019(4) -0.030(6) C55 0.058(5) 0.192(9) 0.040(3) -0.041(5) 0.012(3) -0.043(6) C56 0.064(5) 0.114(6) 0.063(4) -0.042(4) 0.029(4) -0.041(5) C65 0.052(4) 0.069(4) 0.076(4) -0.024(3) 0.009(3) -0.033(3) C66 0.082(6) 0.090(5) 0.137(7) -0.039(5) 0.020(5) -0.061(5) C67 0.065(5) 0.084(5) 0.092(5) -0.005(4) 0.016(4) -0.037(4) C68 0.093(6) 0.077(5) 0.086(5) -0.037(4) 0.013(5) -0.023(5) C69 0.042(3) 0.062(4) 0.053(3) -0.009(3) 0.012(3) -0.012(3) C70 0.051(4) 0.082(4) 0.064(4) -0.032(3) 0.012(3) -0.031(3) C71 0.067(5) 0.090(5) 0.066(4) -0.039(4) 0.011(4) -0.037(4) C72 0.097(6) 0.131(7) 0.057(4) -0.034(4) 0.031(4) -0.070(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O19 2.275(5) . ? Cd1 N3 2.317(5) . ? Cd1 O24B 2.320(17) . ? Cd1 O24A 2.327(14) . ? Cd1 O20A 2.328(16) . ? Cd1 O16 2.390(13) . ? Cd1 O20B 2.458(15) . ? Cd1 O17 2.645(14) . ? O1 C22 1.375(6) . ? O1 C4 1.422(6) . ? N1 C48 1.352(7) . ? N1 C47 1.356(7) . ? N1 Cd2 2.327(4) . ? C1 C2 1.534(8) . ? C1 C21 1.541(8) . ? Cd2 O25 2.269(4) . ? Cd2 N2 2.311(5) 1_564 ? Cd2 O13 2.368(5) . ? Cd2 O11 2.421(5) . ? Cd2 O14 2.488(5) . ? Cd2 O10 2.500(5) . ? O2 C5 1.380(7) . ? O2 C23 1.440(7) . ? N2 C59B 1.203(19) . ? N2 C58A 1.25(2) . ? N2 C59A 1.389(12) . ? N2 C58B 1.420(15) . ? N2 Cd2 2.311(5) 1_546 ? C2 C7 1.403(7) . ? C2 C3 1.412(8) . ? O3 C24 1.375(7) . ? O3 C11 1.418(7) . ? N3 C36 1.345(8) . ? N3 C37 1.352(8) . ? C3 C4 1.385(8) . ? O4 C12 1.385(6) . ? O4 C25 1.403(8) . ? N4 O11 1.232(8) . ? N4 O12 1.253(8) . ? N4 O10 1.277(7) . ? C4 C5 1.406(8) . ? O5 C26 1.364(9) . ? O5 C18 1.439(7) . ? N5 O15 1.207(7) . ? N5 O14 1.279(7) . ? N5 O13 1.290(8) . ? C5 C6 1.382(8) . ? O6 C19 1.367(8) . ? O6 C27 1.425(11) . ? C6 C7 1.414(8) . ? O7 C22 1.202(7) . ? C7 C8 1.524(7) . ? O8 C24 1.203(7) . ? N8 C69 1.314(8) . ? N8 C72 1.460(8) . ? N8 C71 1.494(9) . ? C8 C9 1.520(7) . ? O9 C26 1.185(8) . ? N9 C65 1.296(8) . ? N9 C67 1.458(8) . ? N9 C68 1.496(9) . ? C9 C10 1.410(7) . ? C9 C14 1.420(7) . ? C10 C11 1.382(7) . ? C11 C12 1.405(8) . ? C12 C13 1.373(8) . ? C13 C14 1.392(7) . ? C14 C15 1.541(7) . ? C15 C16 1.534(7) . ? O16 N6 1.219(13) . ? C16 C21 1.380(8) . ? C16 C17 1.406(7) . ? O17 N6 1.340(14) . ? C17 C18 1.371(9) . ? C18 C19 1.384(10) . ? O19 C65 1.236(8) . ? C19 C20 1.390(9) . ? C20 C21 1.415(8) . ? O25 C69 1.260(7) . ? C22 C28 1.481(8) . ? O23 C76 1.19(2) . ? C24 C39 1.484(8) . ? C26 C50 1.490(9) . ? C28 C29 1.392(8) . ? C28 C33 1.401(8) . ? C29 C30 1.416(8) . ? C30 C31 1.400(8) . ? C31 C32 1.388(8) . ? C31 C34 1.495(8) . ? C32 C33 1.411(8) . ? C34 C35 1.395(9) . ? C34 C38 1.406(8) . ? C35 C36 1.378(9) . ? C37 C38 1.364(9) . ? C39 C40 1.388(8) . ? C39 C44 1.389(8) . ? C40 C41 1.393(8) . ? C41 C42 1.415(8) . ? C42 C43 1.410(8) . ? C42 C45 1.483(8) . ? C43 C44 1.389(8) . ? C45 C49 1.389(8) . ? C45 C46 1.417(9) . ? C46 C47 1.381(9) . ? C48 C49 1.384(8) . ? C50 C55 1.374(10) . ? C50 C51 1.410(12) . ? C51 C52 1.378(11) . ? C52 C53 1.411(12) . ? C53 C54 1.361(11) . ? C53 C56 1.504(9) . ? C54 C55 1.372(9) . ? C56 C57A 1.28(2) . ? C56 C60B 1.30(2) . ? C56 C57B 1.357(15) . ? C56 C60A 1.491(13) . ? C57A C58A 1.44(3) . ? C57B C58B 1.431(18) . ? C59A C60A 1.370(15) . ? C59B C60B 1.47(3) . ? C65 C66 1.520(9) . ? C69 C70 1.479(9) . ? C73 N10 1.41(2) . ? C74 N10 1.60(3) . ? C75 C76 1.52(2) . ? C76 N10 1.40(3) . ? C76B O23B 1.17(2) . ? C76B N10B 1.18(3) . ? C76B C73B 1.62(3) . ? C74B N10B 1.70(3) . ? N6 O18 1.303(14) . ? 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 O19 Cd1 N3 89.45(18) . . ? O19 Cd1 O24B 101.6(4) . . ? N3 Cd1 O24B 168.3(4) . . ? O19 Cd1 O24A 102.0(4) . . ? N3 Cd1 O24A 150.9(4) . . ? O24B Cd1 O24A 30.1(4) . . ? O19 Cd1 O20A 140.0(4) . . ? N3 Cd1 O20A 86.6(4) . . ? O24B Cd1 O20A 87.3(6) . . ? O24A Cd1 O20A 67.4(5) . . ? O19 Cd1 O16 81.0(4) . . ? N3 Cd1 O16 104.4(4) . . ? O24B Cd1 O16 74.0(6) . . ? O24A Cd1 O16 103.7(5) . . ? O20A Cd1 O16 138.3(6) . . ? O19 Cd1 O20B 91.8(4) . . ? N3 Cd1 O20B 86.5(4) . . ? O24B Cd1 O20B 96.8(6) . . ? O24A Cd1 O20B 66.7(5) . . ? O20A Cd1 O20B 48.3(6) . . ? O16 Cd1 O20B 166.7(5) . . ? O19 Cd1 O17 132.2(3) . . ? N3 Cd1 O17 85.3(4) . . ? O24B Cd1 O17 84.5(5) . . ? O24A Cd1 O17 105.3(5) . . ? O20A Cd1 O17 87.0(5) . . ? O16 Cd1 O17 54.9(4) . . ? O20B Cd1 O17 135.0(5) . . ? C22 O1 C4 116.2(4) . . ? C48 N1 C47 115.4(5) . . ? C48 N1 Cd2 120.3(4) . . ? C47 N1 Cd2 123.6(4) . . ? C2 C1 C21 109.5(5) . . ? O25 Cd2 N2 172.93(18) . 1_564 ? O25 Cd2 N1 89.59(15) . . ? N2 Cd2 N1 93.07(17) 1_564 . ? O25 Cd2 O13 83.00(16) . . ? N2 Cd2 O13 90.70(19) 1_564 . ? N1 Cd2 O13 138.73(18) . . ? O25 Cd2 O11 89.39(18) . . ? N2 Cd2 O11 93.11(19) 1_564 . ? N1 Cd2 O11 137.03(18) . . ? O13 Cd2 O11 83.63(19) . . ? O25 Cd2 O14 82.83(15) . . ? N2 Cd2 O14 90.84(18) 1_564 . ? N1 Cd2 O14 85.67(15) . . ? O13 Cd2 O14 53.17(16) . . ? O11 Cd2 O14 136.67(16) . . ? O25 Cd2 O10 98.31(16) . . ? N2 Cd2 O10 88.44(19) 1_564 . ? N1 Cd2 O10 85.21(16) . . ? O13 Cd2 O10 136.00(18) . . ? O11 Cd2 O10 52.53(17) . . ? O14 Cd2 O10 170.80(15) . . ? C5 O2 C23 116.5(4) . . ? C59B N2 C58A 70.3(13) . . ? C59B N2 C59A 71.6(10) . . ? C58A N2 C59A 115.5(12) . . ? C59B N2 C58B 113.6(12) . . ? C58A N2 C58B 58.6(11) . . ? C59A N2 C58B 94.1(8) . . ? C59B N2 Cd2 124.5(11) . 1_546 ? C58A N2 Cd2 124.7(11) . 1_546 ? C59A N2 Cd2 119.7(6) . 1_546 ? C58B N2 Cd2 118.8(6) . 1_546 ? C7 C2 C3 118.2(5) . . ? C7 C2 C1 124.0(5) . . ? C3 C2 C1 117.7(5) . . ? C24 O3 C11 114.6(4) . . ? C36 N3 C37 117.8(6) . . ? C36 N3 Cd1 120.2(4) . . ? C37 N3 Cd1 121.7(4) . . ? C4 C3 C2 120.2(5) . . ? C12 O4 C25 118.0(5) . . ? O11 N4 O12 121.9(7) . . ? O11 N4 O10 120.6(6) . . ? O12 N4 O10 117.5(7) . . ? C3 C4 C5 122.2(5) . . ? C3 C4 O1 117.0(5) . . ? C5 C4 O1 120.8(5) . . ? C26 O5 C18 114.8(5) . . ? O15 N5 O14 120.9(7) . . ? O15 N5 O13 123.3(6) . . ? O14 N5 O13 115.8(6) . . ? O2 C5 C6 126.5(5) . . ? O2 C5 C4 116.1(5) . . ? C6 C5 C4 117.4(5) . . ? C19 O6 C27 118.8(6) . . ? C5 C6 C7 121.7(5) . . ? C2 C7 C6 120.1(5) . . ? C2 C7 C8 122.2(5) . . ? C6 C7 C8 117.7(4) . . ? C69 N8 C72 125.0(6) . . ? C69 N8 C71 118.8(5) . . ? C72 N8 C71 116.0(5) . . ? C9 C8 C7 114.2(4) . . ? C65 N9 C67 120.2(6) . . ? C65 N9 C68 123.5(6) . . ? C67 N9 C68 115.2(6) . . ? C10 C9 C14 118.1(5) . . ? C10 C9 C8 118.1(4) . . ? C14 C9 C8 123.8(5) . . ? N4 O10 Cd2 90.7(4) . . ? C11 C10 C9 121.0(5) . . ? N4 O11 Cd2 95.6(4) . . ? C10 C11 C12 120.9(5) . . ? C10 C11 O3 119.7(5) . . ? C12 C11 O3 119.3(5) . . ? C13 C12 O4 127.3(5) . . ? C13 C12 C11 118.2(5) . . ? O4 C12 C11 114.5(5) . . ? N5 O13 Cd2 97.9(3) . . ? C12 C13 C14 122.8(5) . . ? N5 O14 Cd2 92.6(4) . . ? C13 C14 C9 119.1(5) . . ? C13 C14 C15 118.4(5) . . ? C9 C14 C15 122.4(5) . . ? C16 C15 C14 116.1(4) . . ? N6 O16 Cd1 91.5(12) . . ? C21 C16 C17 119.3(5) . . ? C21 C16 C15 123.3(5) . . ? C17 C16 C15 117.4(5) . . ? N6 O17 Cd1 78.3(10) . . ? C18 C17 C16 119.9(6) . . ? C17 C18 C19 122.4(5) . . ? C17 C18 O5 119.6(6) . . ? C19 C18 O5 118.0(6) . . ? C65 O19 Cd1 135.6(5) . . ? O6 C19 C18 117.5(6) . . ? O6 C19 C20 124.6(7) . . ? C18 C19 C20 117.9(6) . . ? C19 C20 C21 120.9(6) . . ? C16 C21 C20 119.7(5) . . ? C16 C21 C1 124.2(5) . . ? C20 C21 C1 116.1(5) . . ? C69 O25 Cd2 139.3(4) . . ? O7 C22 O1 122.5(5) . . ? O7 C22 C28 126.6(5) . . ? O1 C22 C28 110.8(5) . . ? O8 C24 O3 123.9(5) . . ? O8 C24 C39 124.7(6) . . ? O3 C24 C39 111.3(5) . . ? O9 C26 O5 122.3(7) . . ? O9 C26 C50 125.7(8) . . ? O5 C26 C50 111.8(6) . . ? C29 C28 C33 120.0(5) . . ? C29 C28 C22 122.0(5) . . ? C33 C28 C22 117.7(5) . . ? C28 C29 C30 120.0(5) . . ? C31 C30 C29 120.2(5) . . ? C32 C31 C30 119.3(5) . . ? C32 C31 C34 122.7(5) . . ? C30 C31 C34 118.0(5) . . ? C31 C32 C33 121.0(5) . . ? C28 C33 C32 119.5(5) . . ? C35 C34 C38 115.1(6) . . ? C35 C34 C31 123.3(5) . . ? C38 C34 C31 121.6(5) . . ? C36 C35 C34 120.7(6) . . ? N3 C36 C35 122.8(6) . . ? N3 C37 C38 121.7(6) . . ? C37 C38 C34 121.8(6) . . ? C40 C39 C44 119.5(5) . . ? C40 C39 C24 117.3(5) . . ? C44 C39 C24 123.2(5) . . ? C39 C40 C41 120.7(5) . . ? C40 C41 C42 120.0(6) . . ? C43 C42 C41 118.7(5) . . ? C43 C42 C45 121.9(5) . . ? C41 C42 C45 119.2(5) . . ? C44 C43 C42 119.9(6) . . ? C43 C44 C39 121.1(5) . . ? C49 C45 C46 117.2(5) . . ? C49 C45 C42 121.6(5) . . ? C46 C45 C42 121.2(5) . . ? C47 C46 C45 118.5(6) . . ? N1 C47 C46 124.8(6) . . ? N1 C48 C49 124.1(6) . . ? C48 C49 C45 119.8(5) . . ? C55 C50 C51 117.9(7) . . ? C55 C50 C26 123.9(7) . . ? C51 C50 C26 118.1(7) . . ? C52 C51 C50 121.6(8) . . ? C51 C52 C53 118.4(9) . . ? C54 C53 C52 118.7(7) . . ? C54 C53 C56 120.6(7) . . ? C52 C53 C56 120.6(8) . . ? C53 C54 C55 122.3(7) . . ? C54 C55 C50 120.3(8) . . ? C57A C56 C60B 71.3(14) . . ? C57A C56 C57B 57.5(10) . . ? C60B C56 C57B 113.5(13) . . ? C57A C56 C60A 117.2(12) . . ? C60B C56 C60A 72.0(11) . . ? C57B C56 C60A 95.5(8) . . ? C57A C56 C53 125.9(12) . . ? C60B C56 C53 122.3(12) . . ? C57B C56 C53 121.4(8) . . ? C60A C56 C53 116.6(8) . . ? C56 C57A C58A 122.0(18) . . ? C56 C57B C58B 120.6(12) . . ? N2 C58A C57A 124(2) . . ? N2 C58B C57B 119.3(11) . . ? C60A C59A N2 125.4(9) . . ? N2 C59B C60B 124.1(19) . . ? C59A C60A C56 115.2(9) . . ? C56 C60B C59B 121(2) . . ? O19 C65 N9 122.3(6) . . ? O19 C65 C66 118.2(7) . . ? N9 C65 C66 119.5(6) . . ? O25 C69 N8 120.8(6) . . ? O25 C69 C70 120.3(6) . . ? N8 C69 C70 118.8(6) . . ? O23 C76 N10 117.0(18) . . ? O23 C76 C75 129.5(17) . . ? N10 C76 C75 112.2(18) . . ? C76 N10 C73 125.0(19) . . ? C76 N10 C74 121.2(19) . . ? C73 N10 C74 107.4(17) . . ? O23B C76B N10B 122(2) . . ? O23B C76B C73B 119.5(18) . . ? N10B C76B C73B 116(2) . . ? C76B N10B C74B 125(2) . . ? O16 N6 O18 114.5(17) . . ? O16 N6 O17 131.2(18) . . ? O18 N6 O17 104.2(15) . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 26.34 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 5.476 _refine_diff_density_min -2.808 _refine_diff_density_rms 0.121 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.003 0.418 1.000 2294 406 ' ' _platon_squeeze_details ; TGA indicates ~4 molecules of solvate dimethylacetamide is present per formula unit however only one was found crystallographically. An additional 3 DMA (= 6 per unit cell) were removed by the squeeze routine and is consistent with the calculated void electron count. These have been included in the formula ; # Attachment '- complex2_new.CIF' data_complex2_new _database_code_depnum_ccdc_archive 'CCDC 822481' #TrackingRef '- complex2_new.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; aquotriflouroaceto[(+-)-2,7,12-trimethoxy-3,8,13-tris[4- (4-pyridyl)benzoyl]-10,15-dihydro-5H-tribenzo[a,d,g] cyclononane]zinc(II) trifluoroacetate N-methylpyrrolidone clathrate ; _chemical_name_common ; aquotriflouroaceto((+-)-2,7,12-trimethoxy-3,8,13-tris(4-(4- pyridyl)benzoyl)-10,15-dihydro-5H-tribenzo(a,d,g) cyclononane)zinc(ii) trifluoroacetate N-methylpyrrolidone clathrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C318 H310 F12 N26 O60 Zn2' _chemical_formula_weight 5814.85 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' F F 0.0171 0.0103 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 24.869(3) _cell_length_b 25.357(3) _cell_length_c 31.526(4) _cell_angle_alpha 80.258(6) _cell_angle_beta 80.218(6) _cell_angle_gamma 67.429(6) _cell_volume 17972(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.075 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6096 _exptl_absorpt_coefficient_mu 0.21 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9297 _exptl_absorpt_correction_T_max 0.9751 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 X8 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 188848 _diffrn_reflns_av_R_equivalents 0.0699 _diffrn_reflns_av_sigmaI/netI 0.1488 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.00 _reflns_number_total 63125 _reflns_number_gt 21712 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour)' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Three aromatic ring were refined as AFIX 66 (rigid body refinement) and some bond lengths of disordered groups restrained. There was considerable disorder and two counter-anions could not be located in the difference map but are included in formula etc. Solvent and disordered groups refined isotropically. Bond length restraints used: DFIX 1.2 0.05 O28 C156 DFIX 1.3 0.05 O27 C156 DFIX 1.4 0.05 C157 C156 DFIX 1.54 0.02 N301 C305 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type bloc _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1825P)^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 63125 _refine_ls_number_parameters 2818 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.2050 _refine_ls_R_factor_gt 0.1102 _refine_ls_wR_factor_ref 0.3330 _refine_ls_wR_factor_gt 0.2958 _refine_ls_goodness_of_fit_ref 0.918 _refine_ls_restrained_S_all 0.918 _refine_ls_shift/su_max 0.008 _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 0.83861(3) 0.39363(2) 0.35163(2) 0.0607(2) Uani 1 1 d . . . Zn2 Zn 0.20644(3) 1.03555(2) 0.14690(2) 0.0576(2) Uani 1 1 d . . . F4 F 0.8513(3) 0.3554(3) 0.1975(2) 0.179(2) Uiso 1 1 d . . . F5 F 0.9396(4) 0.3246(3) 0.1917(3) 0.227(3) Uiso 1 1 d . . . F6 F 0.8874(3) 0.2855(3) 0.2422(2) 0.188(2) Uiso 1 1 d . . . F1A F 0.1027(3) 1.1481(3) 0.2611(3) 0.087(2) Uiso 0.50 1 d P A 2 F3A F 0.1921(4) 1.0957(3) 0.2868(3) 0.099(2) Uiso 0.50 1 d P A 2 F2A F 0.1094(4) 1.0812(4) 0.3131(3) 0.108(2) Uiso 0.50 1 d P A 2 O1 O 0.5496(2) 1.31521(17) 0.04483(17) 0.1019(16) Uani 1 1 d . . . O2 O 0.43782(19) 1.36017(18) 0.08143(13) 0.0856(13) Uani 1 1 d . . . O3 O 0.4203(2) 1.36832(18) 0.01185(15) 0.0961(15) Uani 1 1 d . . . O4 O 0.3603(2) 1.5362(3) 0.22703(18) 0.144(2) Uani 1 1 d . . . O5 O 0.4455(2) 1.5556(3) 0.25559(17) 0.1192(19) Uani 1 1 d . . . O6 O 0.3694(2) 1.6421(3) 0.2584(2) 0.135(2) Uani 1 1 d . . . O7 O 0.73415(15) 1.44350(15) 0.16312(13) 0.0647(10) Uani 1 1 d . . . O8 O 0.76302(14) 1.38550(13) 0.09453(13) 0.0626(10) Uani 1 1 d . . . O9 O 0.80992(14) 1.44840(14) 0.06890(12) 0.0587(10) Uani 1 1 d . . . O10 O 0.65391(14) 0.68108(13) 0.17566(13) 0.0631(10) Uani 1 1 d . . . O11 O 0.60443(14) 0.62084(13) 0.19732(12) 0.0584(10) Uani 1 1 d . . . O12 O 0.67660(15) 0.62372(14) 0.10564(12) 0.0619(10) Uani 1 1 d . . . O13 O 0.93872(14) 0.56434(15) -0.00477(12) 0.0644(10) Uani 1 1 d . . . O14 O 0.8488(2) 0.6255(2) 0.01075(16) 0.1264(19) Uani 1 1 d . . . O15 O 1.02815(17) 0.57913(18) 0.02173(13) 0.0784(12) Uani 1 1 d . . . O16 O 0.98179(15) 0.70807(14) 0.19397(12) 0.0602(10) Uani 1 1 d . . . O17 O 0.9936(5) 0.7163(4) 0.1223(2) 0.271(6) Uani 1 1 d . . . O18 O 0.86823(17) 0.74875(15) 0.22764(15) 0.0836(13) Uani 1 1 d . . . O19 O 0.81756(19) 0.40899(15) 0.41961(15) 0.0925(14) Uani 1 1 d . . . O21 O 0.85327(15) 0.37599(15) 0.28654(13) 0.0640(10) Uani 1 1 d . . . O22 O 0.9220(2) 0.4037(2) 0.24283(16) 0.1101(15) Uiso 1 1 d . . . O23 O 0.36395(16) 0.80981(16) 0.39555(14) 0.0743(11) Uani 1 1 d . . . O24 O 0.38819(14) 0.74634(15) 0.32868(14) 0.0733(12) Uani 1 1 d . . . O25 O 0.43578(15) 0.80688(15) 0.29658(14) 0.0723(11) Uani 1 1 d . . . O26 O 0.17168(18) 0.67964(16) 0.27267(18) 0.1052(17) Uani 1 1 d . . . O27 O 0.05816(16) 0.72538(15) 0.30608(13) 0.0678(11) Uani 1 1 d D . . O28 O 0.1150(3) 0.6668(3) 0.3598(2) 0.068(2) Uiso 0.50 1 d PD B 1 O29 O 0.00643(17) 0.87683(18) 0.47445(13) 0.0808(12) Uani 1 1 d . . . O30 O 0.09217(18) 0.9044(2) 0.49742(14) 0.0817(12) Uani 1 1 d . . . O31 O 0.1399(4) 0.8191(4) 0.5090(3) 0.105(3) Uiso 0.50 1 d P C 2 O31A O 0.0202(4) 0.9801(4) 0.5114(3) 0.091(3) Uiso 0.50 1 d P . 1 O32 O 1.28155(14) 0.04250(15) 0.39979(13) 0.0657(10) Uani 1 1 d . . . O33 O 1.23582(16) -0.01895(17) 0.43286(15) 0.0822(13) Uani 1 1 d . . . O34 O 1.30461(16) -0.01047(17) 0.32883(13) 0.0745(11) Uani 1 1 d . . . O35 O 1.5861(2) -0.0948(2) 0.22297(19) 0.1103(16) Uani 1 1 d . . . O36 O 1.6656(2) -0.1749(2) 0.21065(18) 0.1142(17) Uani 1 1 d . . . O37 O 1.6754(2) -0.0782(2) 0.25197(19) 0.1257(19) Uani 1 1 d . . . O38 O 1.60383(18) 0.07090(16) 0.40872(14) 0.0840(13) Uani 1 1 d . . . O39 O 1.64676(19) 0.03916(19) 0.47023(15) 0.0926(14) Uani 1 1 d . . . O40 O 1.49366(19) 0.11061(16) 0.44769(16) 0.0919(14) Uani 1 1 d . . . O41 O 0.18875(16) 1.05427(15) 0.21222(13) 0.0688(11) Uani 1 1 d . . . O42 O 0.1170(4) 1.0324(3) 0.2555(3) 0.193(3) Uiso 1 1 d . . . O43 O 0.22988(18) 1.02259(16) 0.07837(16) 0.0934(14) Uani 1 1 d . . . O45 O 0.2972(3) 0.5134(3) 0.1069(2) 0.0590(18) Uiso 0.50 1 d P D 1 O46 O 0.1209(7) 0.5061(6) 0.2294(5) 0.181(5) Uiso 0.50 1 d P E 1 C272 C -0.3236(4) 0.7494(4) 0.3014(3) 0.041(2) Uiso 0.50 1 d P F 1 H27A H -0.2932 0.7334 0.2779 0.049 Uiso 0.50 1 calc PR F 1 H27B H -0.3206 0.7846 0.3079 0.049 Uiso 0.50 1 calc PR F 1 H27C H -0.3623 0.7585 0.2925 0.049 Uiso 0.50 1 calc PR F 1 C282 C 0.1127(6) 0.7546(5) 0.5210(4) 0.082(4) Uiso 0.50 1 d P G 1 H28A H 0.1330 0.7659 0.5398 0.098 Uiso 0.50 1 calc PR G 1 H28B H 0.1084 0.7182 0.5337 0.098 Uiso 0.50 1 calc PR G 1 H28C H 0.0739 0.7845 0.5180 0.098 Uiso 0.50 1 calc PR G 1 O49 O 1.5504(3) -0.2338(3) 0.4673(2) 0.0461(16) Uiso 0.50 1 d P H 1 C257 C 0.8669(5) 0.7718(4) -0.0034(3) 0.167(4) Uiso 1 1 d . I 1 H25A H 0.8347 0.7976 -0.0198 0.200 Uiso 1 1 calc R I 1 H25B H 0.8922 0.7403 -0.0203 0.200 Uiso 1 1 calc R I 1 H25C H 0.8899 0.7934 0.0022 0.200 Uiso 1 1 calc R I 1 N1 N 0.24879(17) 1.09967(16) 0.13138(15) 0.0559(12) Uani 1 1 d . . . N3 N 1.12538(18) 1.10749(17) 0.13333(16) 0.0648(13) Uani 1 1 d . . . N4 N 0.28966(17) 0.96861(16) 0.16225(14) 0.0516(11) Uani 1 1 d . . . N6 N 1.16584(19) 0.97130(18) 0.15456(16) 0.0678(13) Uani 1 1 d . . . N7 N 0.75702(18) 0.46432(18) 0.33883(15) 0.0599(12) Uani 1 1 d . . . N10 N 0.91588(18) 0.3179(2) 0.36692(15) 0.0618(12) Uani 1 1 d . . . N12 N 1.78548(18) 0.33656(17) 0.36657(15) 0.0591(12) Uani 1 1 d . . . N13 N 1.4788(4) -0.2652(4) 0.5013(3) 0.065(2) Uiso 0.50 1 d P H 1 C268 C -0.2709(4) 0.6550(4) 0.3407(3) 0.037(2) Uiso 0.50 1 d P F 1 C281 C 0.1998(7) 0.7587(6) 0.4617(5) 0.098(4) Uiso 0.50 1 d P G 1 N16 N 0.2548(7) 0.4664(7) 0.0725(5) 0.144(5) Uiso 0.50 1 d P D 1 N17 N 0.1299(5) 0.5555(6) 0.1545(4) 0.110(4) Uiso 0.50 1 d P E 1 C253 C 0.7929(5) 0.7480(4) 0.0421(3) 0.137(3) Uiso 1 1 d . I 1 C1 C 0.5767(2) 1.5018(2) 0.03426(18) 0.0578(15) Uani 1 1 d . . . H1A H 0.5523 1.5432 0.0301 0.069 Uiso 1 1 calc R . . H1B H 0.6011 1.4912 0.0065 0.069 Uiso 1 1 calc R . . C2 C 0.5367(2) 1.4669(2) 0.04625(18) 0.0572(15) Uani 1 1 d . . . C3 C 0.5606(3) 1.4088(2) 0.03942(18) 0.0652(16) Uani 1 1 d . . . H3 H 0.6001 1.3934 0.0267 0.078 Uiso 1 1 calc R . . C4 C 0.5289(3) 1.3724(2) 0.0506(2) 0.0703(17) Uani 1 1 d . . . C5 C 0.4721(3) 1.3962(3) 0.0677(2) 0.079(2) Uani 1 1 d . . . C6 C 0.4467(3) 1.4539(2) 0.07558(18) 0.0666(16) Uani 1 1 d . . . H6 H 0.4072 1.4688 0.0884 0.080 Uiso 1 1 calc R . . C7 C 0.4792(2) 1.4896(2) 0.06461(18) 0.0572(15) Uani 1 1 d . . . C8 C 0.4490(2) 1.5515(2) 0.0762(2) 0.0766(19) Uani 1 1 d . . . H8A H 0.4693 1.5756 0.0580 0.092 Uiso 1 1 calc R . . H8B H 0.4081 1.5666 0.0691 0.092 Uiso 1 1 calc R . . C9 C 0.4483(2) 1.5571(3) 0.1228(2) 0.0774(19) Uani 1 1 d . . . C10 C 0.4032(3) 1.5469(3) 0.1519(2) 0.094(2) Uani 1 1 d . . . H10 H 0.3736 1.5395 0.1412 0.112 Uiso 1 1 calc R . . C11 C 0.4008(3) 1.5474(4) 0.1952(3) 0.115(3) Uani 1 1 d . . . C12 C 0.4454(3) 1.5593(3) 0.2114(2) 0.101(2) Uani 1 1 d . . . C13 C 0.4903(2) 1.5680(3) 0.1815(2) 0.083(2) Uani 1 1 d . . . H13 H 0.5200 1.5757 0.1918 0.099 Uiso 1 1 calc R . . C14 C 0.4934(2) 1.5659(2) 0.1384(2) 0.0677(17) Uani 1 1 d . . . C15 C 0.5447(2) 1.5774(2) 0.1083(2) 0.0734(18) Uani 1 1 d . . . H15A H 0.5322 1.5934 0.0792 0.088 Uiso 1 1 calc R . . H15B H 0.5537 1.6069 0.1197 0.088 Uiso 1 1 calc R . . C16 C 0.6010(2) 1.5235(2) 0.10405(18) 0.0540(14) Uani 1 1 d . . . C17 C 0.6389(2) 1.5083(2) 0.13648(18) 0.0542(14) Uani 1 1 d . . . H17 H 0.6276 1.5298 0.1606 0.065 Uiso 1 1 calc R . . C18 C 0.6928(2) 1.4623(2) 0.13386(19) 0.0590(15) Uani 1 1 d . . . C19 C 0.7092(2) 1.4316(2) 0.09824(19) 0.0574(15) Uani 1 1 d . . . C20 C 0.6704(2) 1.4468(2) 0.06599(17) 0.0543(14) Uani 1 1 d . . . H20 H 0.6817 1.4258 0.0416 0.065 Uiso 1 1 calc R . . C21 C 0.6170(2) 1.49118(19) 0.06943(17) 0.0461(13) Uani 1 1 d . . . C22 C 0.6086(4) 1.2911(3) 0.0277(3) 0.128(3) Uani 1 1 d . . . H22A H 0.6185 1.2504 0.0250 0.154 Uiso 1 1 calc R . . H22B H 0.6337 1.2945 0.0471 0.154 Uiso 1 1 calc R . . H22C H 0.6149 1.3115 -0.0009 0.154 Uiso 1 1 calc R . . C23 C 0.4150(3) 1.3482(3) 0.0498(2) 0.0780(19) Uani 1 1 d . . . C24 C 0.3837(3) 1.3088(2) 0.06663(19) 0.0657(17) Uani 1 1 d . . . C25 C 0.3579(3) 1.2922(3) 0.0380(2) 0.084(2) Uani 1 1 d . . . H25 H 0.3599 1.3079 0.0085 0.100 Uiso 1 1 calc R . . C26 C 0.3294(3) 1.2537(2) 0.0509(2) 0.0732(18) Uani 1 1 d . . . H26 H 0.3114 1.2442 0.0306 0.088 Uiso 1 1 calc R . . C27 C 0.3274(2) 1.2291(2) 0.09396(19) 0.0577(15) Uani 1 1 d . . . C28 C 0.3517(3) 1.2457(3) 0.1235(2) 0.090(2) Uani 1 1 d . . . H28 H 0.3491 1.2314 0.1533 0.108 Uiso 1 1 calc R . . C29 C 0.3807(3) 1.2853(3) 0.1073(2) 0.090(2) Uani 1 1 d . . . H29 H 0.3991 1.2953 0.1270 0.108 Uiso 1 1 calc R . . C30 C 0.2984(2) 1.1857(2) 0.10780(17) 0.0528(14) Uani 1 1 d . . . C31 C 0.2704(2) 1.1724(2) 0.0787(2) 0.0606(15) Uani 1 1 d . . . H31 H 0.2673 1.1919 0.0502 0.073 Uiso 1 1 calc R . . C32 C 0.2471(2) 1.1297(2) 0.0927(2) 0.0659(16) Uani 1 1 d . . . H32 H 0.2282 1.1212 0.0724 0.079 Uiso 1 1 calc R . . C33 C 0.2750(2) 1.1131(2) 0.1601(2) 0.0632(16) Uani 1 1 d . . . H33 H 0.2760 1.0934 0.1886 0.076 Uiso 1 1 calc R . . C34 C 0.3006(2) 1.1548(2) 0.14981(19) 0.0567(15) Uani 1 1 d . . . H34 H 0.3193 1.1623 0.1708 0.068 Uiso 1 1 calc R . . C35 C 0.3210(3) 1.5141(4) 0.2139(3) 0.139(3) Uani 1 1 d . . . H35A H 0.2938 1.5083 0.2389 0.167 Uiso 1 1 calc R . . H35B H 0.3437 1.4774 0.2023 0.167 Uiso 1 1 calc R . . H35C H 0.2988 1.5416 0.1914 0.167 Uiso 1 1 calc R . . C36 C 0.4009(4) 1.5968(4) 0.2779(2) 0.106(3) Uani 1 1 d . . . C37 C 0.4008(3) 1.5835(4) 0.3230(3) 0.105(3) Uani 1 1 d . . . C38 C 0.3609(3) 1.6186(3) 0.3550(3) 0.111(3) Uani 1 1 d . . . H38 H 0.3317 1.6534 0.3447 0.133 Uiso 1 1 calc R . . C39 C 0.3616(4) 1.6057(4) 0.3998(3) 0.126(3) Uani 1 1 d . . . H39 H 0.3332 1.6310 0.4187 0.152 Uiso 1 1 calc R . . C40 C 0.4044(4) 1.5553(4) 0.4167(3) 0.122(3) Uani 1 1 d . . . C41 C 0.4450(4) 1.5196(4) 0.3856(3) 0.129(3) Uani 1 1 d . . . H41 H 0.4746 1.4851 0.3958 0.155 Uiso 1 1 calc R . . C42 C 0.4428(4) 1.5331(4) 0.3419(3) 0.122(3) Uani 1 1 d . . . H42 H 0.4709 1.5074 0.3232 0.146 Uiso 1 1 calc R . . C43 C 0.4078(3) 1.5448(3) 0.46503(14) 0.124(3) Uani 1 1 d G . . C44 C 0.4357(4) 1.4887(2) 0.4831(2) 0.275(9) Uani 1 1 d G . . H44 H 0.4519 1.4584 0.4653 0.330 Uiso 1 1 calc R . . C45 C 0.4397(4) 1.4769(2) 0.5274(2) 0.278(10) Uani 1 1 d G . . H45 H 0.4588 1.4386 0.5398 0.334 Uiso 1 1 calc R . . N2 N 0.4159(3) 1.5213(3) 0.55360(15) 0.192(4) Uani 1 1 d G . . C46 C 0.3880(3) 1.5773(3) 0.53549(18) 0.147(4) Uani 1 1 d G . . H46 H 0.3718 1.6076 0.5534 0.176 Uiso 1 1 calc R . . C47 C 0.3840(2) 1.5891(2) 0.4912(2) 0.128(3) Uani 1 1 d G . . H47 H 0.3649 1.6274 0.4788 0.154 Uiso 1 1 calc R . . C48 C 0.7165(3) 1.4688(3) 0.20279(19) 0.0750(18) Uani 1 1 d . . . H48A H 0.7487 1.4523 0.2210 0.090 Uiso 1 1 calc R . . H48B H 0.6821 1.4610 0.2181 0.090 Uiso 1 1 calc R . . H48C H 0.7067 1.5104 0.1966 0.090 Uiso 1 1 calc R . . C49 C 0.8122(2) 1.3996(2) 0.08213(17) 0.0530(14) Uani 1 1 d . . . C50 C 0.8664(2) 1.3475(2) 0.08835(18) 0.0548(14) Uani 1 1 d . . . C51 C 0.9205(2) 1.3557(2) 0.08193(18) 0.0596(15) Uani 1 1 d . . . H51 H 0.9218 1.3929 0.0729 0.072 Uiso 1 1 calc R . . C52 C 0.9725(2) 1.3083(2) 0.08903(17) 0.0537(14) Uani 1 1 d . . . H52 H 1.0090 1.3136 0.0847 0.064 Uiso 1 1 calc R . . C53 C 0.9707(2) 1.2534(2) 0.10253(18) 0.0584(15) Uani 1 1 d . . . C54 C 0.9173(2) 1.2454(2) 0.1072(2) 0.0762(19) Uani 1 1 d . . . H54 H 0.9164 1.2078 0.1144 0.091 Uiso 1 1 calc R . . C55 C 0.8651(2) 1.2924(2) 0.1015(2) 0.0754(19) Uani 1 1 d . . . H55 H 0.8288 1.2869 0.1065 0.091 Uiso 1 1 calc R . . C56 C 1.0247(2) 1.2031(2) 0.1125(2) 0.0630(16) Uani 1 1 d . . . C57 C 1.0630(2) 1.2054(2) 0.13952(18) 0.0554(14) Uani 1 1 d . . . H57 H 1.0556 1.2399 0.1513 0.066 Uiso 1 1 calc R . . C58 C 1.1111(2) 1.1576(2) 0.14872(19) 0.0623(16) Uani 1 1 d . . . H58 H 1.1361 1.1603 0.1673 0.075 Uiso 1 1 calc R . . C59 C 1.0890(3) 1.1041(2) 0.1072(2) 0.0757(19) Uani 1 1 d . . . H59 H 1.0982 1.0688 0.0960 0.091 Uiso 1 1 calc R . . C60 C 1.0393(3) 1.1501(2) 0.0960(2) 0.0734(18) Uani 1 1 d . . . H60 H 1.0151 1.1461 0.0774 0.088 Uiso 1 1 calc R . . C61 C 0.8481(2) 0.5615(2) 0.22495(17) 0.0504(13) Uani 1 1 d . . . H61A H 0.8269 0.5664 0.2544 0.060 Uiso 1 1 calc R . . H61B H 0.8745 0.5207 0.2247 0.060 Uiso 1 1 calc R . . C62 C 0.80344(19) 0.5755(2) 0.19266(17) 0.0471(13) Uani 1 1 d . . . C63 C 0.7488(2) 0.61967(19) 0.19824(17) 0.0481(13) Uani 1 1 d . . . H63 H 0.7394 0.6403 0.2226 0.058 Uiso 1 1 calc R . . C64 C 0.7082(2) 0.63420(19) 0.16932(19) 0.0541(14) Uani 1 1 d . . . C65 C 0.7202(2) 0.6057(2) 0.13286(18) 0.0530(14) Uani 1 1 d . . . C66 C 0.7739(2) 0.5601(2) 0.12698(17) 0.0475(13) Uani 1 1 d . . . H66 H 0.7820 0.5391 0.1029 0.057 Uiso 1 1 calc R . . C67 C 0.8153(2) 0.54496(19) 0.15542(17) 0.0471(13) Uani 1 1 d . . . C68 C 0.8737(2) 0.49454(19) 0.14643(17) 0.0475(13) Uani 1 1 d . . . H68A H 0.8908 0.4768 0.1739 0.057 Uiso 1 1 calc R . . H68B H 0.8665 0.4649 0.1339 0.057 Uiso 1 1 calc R . . C69 C 0.91700(19) 0.51616(19) 0.11478(18) 0.0497(14) Uani 1 1 d . . . C69A C 0.0602(5) 0.9346(5) 0.5250(4) 0.061(3) Uiso 0.50 1 d P J 1 C70A C 0.0652(9) 0.9214(9) 0.5697(5) 0.076(4) Uiso 0.50 1 d P J 1 C71A C 0.1145(4) 0.8729(4) 0.5861(4) 0.044(2) Uiso 0.50 1 d P J 1 H71A H 0.1439 0.8497 0.5664 0.053 Uiso 0.50 1 calc PR J 1 C72A C 0.1187(5) 0.8605(5) 0.6303(4) 0.064(3) Uiso 0.50 1 d P J 1 H72A H 0.1523 0.8294 0.6393 0.077 Uiso 0.50 1 calc PR J 1 C73A C 0.0776(5) 0.8899(6) 0.6629(5) 0.051(3) Uiso 0.50 1 d P J 1 C74A C 0.0309(5) 0.9360(5) 0.6461(4) 0.050(3) Uiso 0.50 1 d P J 1 H74A H 0.0015 0.9584 0.6661 0.059 Uiso 0.50 1 calc PR J 1 C75A C 0.0241(6) 0.9513(6) 0.6028(4) 0.066(3) Uiso 0.50 1 d P J 1 H75A H -0.0094 0.9833 0.5946 0.079 Uiso 0.50 1 calc PR J 1 C70 C 0.9105(2) 0.5275(2) 0.07016(17) 0.0513(13) Uani 1 1 d . . . H70 H 0.8808 0.5196 0.0600 0.062 Uiso 1 1 calc R . . C71 C 0.9468(2) 0.5502(2) 0.04079(17) 0.0521(13) Uani 1 1 d . . . C72 C 0.9936(2) 0.5586(2) 0.05407(19) 0.0569(14) Uani 1 1 d . . . C73 C 1.0025(2) 0.54608(19) 0.09728(17) 0.0488(13) Uani 1 1 d . . . H73 H 1.0353 0.5502 0.1060 0.059 Uiso 1 1 calc R . . C74 C 0.9637(2) 0.52712(19) 0.12927(17) 0.0482(13) Uani 1 1 d . . . C75 C 0.9722(2) 0.5213(2) 0.17562(16) 0.0493(13) Uani 1 1 d . . . H75B H 1.0147 0.5057 0.1785 0.059 Uiso 1 1 calc R . . H75C H 0.9551 0.4937 0.1925 0.059 Uiso 1 1 calc R . . C76 C 0.9432(2) 0.57961(19) 0.19416(16) 0.0453(13) Uani 1 1 d . . . C77 C 0.9743(2) 0.6165(2) 0.18622(17) 0.0535(14) Uani 1 1 d . . . H77 H 1.0134 0.6039 0.1723 0.064 Uiso 1 1 calc R . . C78 C 0.9481(2) 0.6720(2) 0.19882(18) 0.0538(14) Uani 1 1 d . . . C79 C 0.8901(2) 0.6928(2) 0.21760(18) 0.0533(14) Uani 1 1 d . . . C80 C 0.8600(2) 0.6552(2) 0.22636(17) 0.0526(14) Uani 1 1 d . . . H80 H 0.8211 0.6680 0.2406 0.063 Uiso 1 1 calc R . . C76A C 0.0482(7) 0.8974(6) 0.7031(5) 0.082(4) Uiso 0.50 1 d P C 2 C77A C 0.0399(8) 0.8507(8) 0.7344(6) 0.120(5) Uiso 0.50 1 d P C 2 H77A H 0.0441 0.8147 0.7265 0.144 Uiso 0.50 1 calc PR C 2 C78A C 0.0253(7) 0.8643(8) 0.7766(7) 0.107(5) Uiso 0.50 1 d P C 2 H78A H 0.0155 0.8362 0.7969 0.128 Uiso 0.50 1 calc PR C 2 N9A N 0.0227(7) 0.9089(7) 0.7934(5) 0.131(5) Uiso 0.50 1 d P C 2 C79A C 0.0346(7) 0.9502(8) 0.7666(6) 0.126(6) Uiso 0.50 1 d P C 2 H79A H 0.0374 0.9812 0.7781 0.151 Uiso 0.50 1 calc PR C 2 C80A C 0.0439(6) 0.9490(6) 0.7184(5) 0.091(4) Uiso 0.50 1 d P C 2 H80A H 0.0467 0.9811 0.6990 0.109 Uiso 0.50 1 calc PR C 2 C81 C 0.8849(2) 0.5991(2) 0.21495(16) 0.0480(13) Uani 1 1 d . . . C82 C 0.6043(2) 0.6698(2) 0.18688(18) 0.0542(14) Uani 1 1 d . . . C83 C 0.5511(2) 0.7223(2) 0.1851(2) 0.0627(16) Uani 1 1 d . . . C84 C 0.5542(3) 0.7771(2) 0.1721(3) 0.095(2) Uani 1 1 d . . . H84 H 0.5914 0.7805 0.1650 0.114 Uiso 1 1 calc R . . C85 C 0.5033(2) 0.8266(2) 0.1694(3) 0.105(3) Uani 1 1 d . . . H85 H 0.5062 0.8631 0.1598 0.126 Uiso 1 1 calc R . . C86 C 0.4488(2) 0.8220(2) 0.18074(19) 0.0629(16) Uani 1 1 d . . . C87 C 0.4460(2) 0.7678(2) 0.19603(18) 0.0610(15) Uani 1 1 d . . . H87 H 0.4087 0.7651 0.2057 0.073 Uiso 1 1 calc R . . C88 C 0.4955(2) 0.7184(2) 0.19756(18) 0.0577(14) Uani 1 1 d . . . H88 H 0.4922 0.6820 0.2069 0.069 Uiso 1 1 calc R . . C89 C 0.3940(2) 0.8742(2) 0.17598(19) 0.0606(15) Uani 1 1 d . . . C90 C 0.3428(2) 0.8825(2) 0.2046(2) 0.0659(16) Uani 1 1 d . . . H90 H 0.3423 0.8557 0.2295 0.079 Uiso 1 1 calc R . . C91 C 0.2927(2) 0.9298(2) 0.19654(17) 0.0534(14) Uani 1 1 d . . . H91 H 0.2586 0.9347 0.2167 0.064 Uiso 1 1 calc R . . C92 C 0.3385(3) 0.9636(2) 0.1359(2) 0.0802(19) Uani 1 1 d . . . H92 H 0.3377 0.9926 0.1123 0.096 Uiso 1 1 calc R . . C93 C 0.3914(3) 0.9169(3) 0.1416(2) 0.095(2) Uani 1 1 d . . . H93 H 0.4255 0.9146 0.1218 0.114 Uiso 1 1 calc R . . C94 C 0.6921(2) 0.6005(2) 0.06563(18) 0.0673(16) Uani 1 1 d . . . H94A H 0.6582 0.6159 0.0492 0.081 Uiso 1 1 calc R . . H94B H 0.7046 0.5585 0.0710 0.081 Uiso 1 1 calc R . . H94C H 0.7244 0.6109 0.0490 0.081 Uiso 1 1 calc R . . C95 C 0.8911(2) 0.6074(3) -0.0166(2) 0.0755(18) Uani 1 1 d . . . C96 C 0.8916(2) 0.6267(2) -0.06303(18) 0.0587(15) Uani 1 1 d . . . C97 C 0.8438(3) 0.6694(3) -0.0778(2) 0.095(2) Uani 1 1 d . . . H97 H 0.8112 0.6866 -0.0576 0.114 Uiso 1 1 calc R . . C98 C 0.8411(3) 0.6890(3) -0.1221(2) 0.093(2) Uani 1 1 d . . . H98 H 0.8069 0.7189 -0.1316 0.112 Uiso 1 1 calc R . . C99 C 0.8887(2) 0.6642(2) -0.1520(2) 0.0629(16) Uani 1 1 d . . . C100 C 0.9375(2) 0.6206(2) -0.13710(19) 0.0647(16) Uani 1 1 d . . . H100 H 0.9705 0.6032 -0.1570 0.078 Uiso 1 1 calc R . . C101 C 0.9387(2) 0.6016(2) -0.09227(19) 0.0618(15) Uani 1 1 d . . . H101 H 0.9724 0.5713 -0.0823 0.074 Uiso 1 1 calc R . . C102 C 0.8853(2) 0.6829(2) -0.20053(12) 0.0725(18) Uani 1 1 d G . . C103 C 0.8333(2) 0.7230(3) -0.21432(17) 0.264(8) Uani 1 1 d G . . H103 H 0.8005 0.7386 -0.1937 0.317 Uiso 1 1 calc R . . C104 C 0.8291(2) 0.7404(3) -0.25828(19) 0.352(13) Uani 1 1 d G . . H104 H 0.7935 0.7679 -0.2677 0.423 Uiso 1 1 calc R . . N5 N 0.8771(3) 0.7176(3) -0.28845(13) 0.129(2) Uani 1 1 d G . . C105 C 0.9292(2) 0.6775(3) -0.27466(15) 0.190(5) Uani 1 1 d G . . H105 H 0.9619 0.6619 -0.2953 0.228 Uiso 1 1 calc R . . C106 C 0.93327(19) 0.6601(3) -0.23070(17) 0.220(7) Uani 1 1 d G . . H106 H 0.9689 0.6326 -0.2213 0.264 Uiso 1 1 calc R . . C107 C 1.0786(4) 0.5832(5) 0.0353(3) 0.178(5) Uani 1 1 d . . . H10A H 1.1002 0.5982 0.0104 0.214 Uiso 1 1 calc R . . H10B H 1.1041 0.5450 0.0468 0.214 Uiso 1 1 calc R . . H10C H 1.0659 0.6092 0.0578 0.214 Uiso 1 1 calc R . . C108 C 0.9946(5) 0.7345(4) 0.1567(2) 0.140(4) Uani 1 1 d . . . C109 C 1.0322(3) 0.7684(2) 0.15622(15) 0.106(3) Uani 1 1 d G . . C110 C 1.0555(3) 0.7907(3) 0.11738(12) 0.226(7) Uani 1 1 d G . . H110 H 1.0521 0.7802 0.0907 0.271 Uiso 1 1 calc R . . C111 C 1.0837(3) 0.8285(3) 0.11754(12) 0.223(7) Uani 1 1 d G . . H111 H 1.0997 0.8438 0.0910 0.267 Uiso 1 1 calc R . . C112 C 1.0887(2) 0.8440(2) 0.15654(14) 0.089(2) Uani 1 1 d G . . C113 C 1.06537(19) 0.82168(18) 0.19538(12) 0.0790(19) Uani 1 1 d G . . H113 H 1.0687 0.8323 0.2220 0.095 Uiso 1 1 calc R . . C114 C 1.03713(19) 0.78388(18) 0.19522(12) 0.0789(19) Uani 1 1 d G . . H114 H 1.0212 0.7686 0.2218 0.095 Uiso 1 1 calc R . . C115 C 1.1159(3) 0.8879(3) 0.1574(2) 0.083(2) Uani 1 1 d . . . C116 C 1.1727(3) 0.8798(3) 0.1370(3) 0.107(3) Uani 1 1 d . . . H116 H 1.1956 0.8458 0.1239 0.129 Uiso 1 1 calc R . . C117 C 1.1949(3) 0.9224(3) 0.1362(3) 0.102(2) Uani 1 1 d . . . H117 H 1.2331 0.9167 0.1217 0.123 Uiso 1 1 calc R . . C118 C 1.1162(3) 0.9755(3) 0.1767(2) 0.087(2) Uani 1 1 d . . . H118 H 1.0958 1.0079 0.1923 0.104 Uiso 1 1 calc R . . C119 C 1.0915(3) 0.9348(3) 0.1787(2) 0.100(2) Uani 1 1 d . . . H119 H 1.0550 0.9401 0.1961 0.120 Uiso 1 1 calc R . . C120 C 0.8064(3) 0.7724(3) 0.2402(3) 0.132(4) Uani 1 1 d . . . H12A H 0.7954 0.8120 0.2467 0.158 Uiso 1 1 calc R . . H12B H 0.7960 0.7492 0.2660 0.158 Uiso 1 1 calc R . . H12C H 0.7855 0.7724 0.2165 0.158 Uiso 1 1 calc R . . C121 C 0.1709(2) 0.9399(2) 0.34574(18) 0.0560(14) Uani 1 1 d . . . H12D H 0.1797 0.9699 0.3564 0.067 Uiso 1 1 calc R . . H12E H 0.1550 0.9560 0.3177 0.067 Uiso 1 1 calc R . . C122 C 0.2286(2) 0.8868(2) 0.33879(19) 0.0581(15) Uani 1 1 d . . . C123 C 0.2690(2) 0.8738(2) 0.3694(2) 0.0631(16) Uani 1 1 d . . . H123 H 0.2598 0.8971 0.3922 0.076 Uiso 1 1 calc R . . C124 C 0.3223(2) 0.8270(2) 0.36642(18) 0.0624(15) Uiso 1 1 d . . . C125 C 0.3348(2) 0.7951(2) 0.3309(2) 0.0698(17) Uani 1 1 d . . . C126 C 0.2955(2) 0.8061(2) 0.3024(2) 0.0696(17) Uani 1 1 d . . . H126 H 0.3043 0.7820 0.2802 0.084 Uiso 1 1 calc R . . C127 C 0.2417(2) 0.8531(2) 0.30550(19) 0.0581(15) Uani 1 1 d . . . C128 C 0.1999(2) 0.8636(2) 0.27147(19) 0.0650(16) Uani 1 1 d . . . H12F H 0.2234 0.8530 0.2434 0.078 Uiso 1 1 calc R . . H12G H 0.1756 0.9051 0.2675 0.078 Uiso 1 1 calc R . . C129 C 0.1590(2) 0.8291(2) 0.28403(18) 0.0560(15) Uani 1 1 d . . . C130 C 0.1832(2) 0.7714(2) 0.2730(2) 0.078(2) Uani 1 1 d . . . H130 H 0.2221 0.7569 0.2590 0.093 Uiso 1 1 calc R . . C131 C 0.1503(3) 0.7365(2) 0.2826(2) 0.0745(18) Uani 1 1 d . . . C132 C 0.0925(2) 0.7591(2) 0.30162(19) 0.0580(15) Uani 1 1 d . . . C133 C 0.0693(2) 0.8142(2) 0.31126(18) 0.0571(14) Uani 1 1 d . . . H133 H 0.0296 0.8288 0.3236 0.069 Uiso 1 1 calc R B . C134 C 0.1020(2) 0.8510(2) 0.30367(17) 0.0498(13) Uani 1 1 d . . . C135 C 0.0735(2) 0.9109(2) 0.31816(17) 0.0525(14) Uani 1 1 d . . . H13A H 0.0312 0.9261 0.3145 0.063 Uiso 1 1 calc R B . H13B H 0.0914 0.9367 0.2994 0.063 Uiso 1 1 calc R . . C136 C 0.0804(2) 0.91107(19) 0.36592(18) 0.0520(14) Uani 1 1 d . J . C137 C 0.0398(2) 0.8967(2) 0.39716(17) 0.0527(14) Uani 1 1 d . . . H137 H 0.0088 0.8896 0.3883 0.063 Uiso 1 1 calc R B . C138 C 0.0441(2) 0.8925(2) 0.44132(19) 0.0602(15) Uani 1 1 d . J . C139 C 0.0884(2) 0.9055(2) 0.45343(18) 0.0553(14) Uani 1 1 d . J . C140 C 0.1276(2) 0.9206(2) 0.42299(19) 0.0604(15) Uani 1 1 d . . . H140 H 0.1575 0.9291 0.4322 0.073 Uiso 1 1 calc R J . C141 C 0.1249(2) 0.9239(2) 0.37825(17) 0.0499(13) Uani 1 1 d . J . C142 C 0.3475(3) 0.8380(3) 0.4334(2) 0.0829(19) Uani 1 1 d . . . H14A H 0.3800 0.8229 0.4512 0.099 Uiso 1 1 calc R . . H14B H 0.3131 0.8313 0.4499 0.099 Uiso 1 1 calc R . . H14C H 0.3379 0.8794 0.4253 0.099 Uiso 1 1 calc R . . C143 C 0.4372(2) 0.7597(2) 0.3114(2) 0.0702(17) Uani 1 1 d . . . C144 C 0.4925(2) 0.7062(2) 0.3156(2) 0.0651(17) Uani 1 1 d . . . C145 C 0.4914(2) 0.6546(2) 0.3393(2) 0.083(2) Uani 1 1 d . . . H145 H 0.4554 0.6521 0.3536 0.099 Uiso 1 1 calc R . . C146 C 0.5433(3) 0.6071(3) 0.3420(2) 0.085(2) Uani 1 1 d . . . H146 H 0.5424 0.5721 0.3580 0.102 Uiso 1 1 calc R . . C147 C 0.5967(2) 0.6100(2) 0.3215(2) 0.0653(16) Uani 1 1 d . . . C148 C 0.5973(2) 0.6621(2) 0.29841(19) 0.0665(16) Uani 1 1 d . . . H148 H 0.6334 0.6651 0.2847 0.080 Uiso 1 1 calc R . . C149 C 0.5452(2) 0.7099(2) 0.2954(2) 0.0648(16) Uani 1 1 d . . . H149 H 0.5459 0.7450 0.2795 0.078 Uiso 1 1 calc R . . C150 C 0.6516(2) 0.5597(2) 0.3260(2) 0.0627(16) Uani 1 1 d . . . C151 C 0.6596(3) 0.5243(3) 0.3651(2) 0.093(2) Uani 1 1 d . . . H151 H 0.6292 0.5318 0.3886 0.112 Uiso 1 1 calc R . . C152 C 0.7118(3) 0.4783(3) 0.3698(2) 0.095(2) Uani 1 1 d . . . H152 H 0.7157 0.4550 0.3969 0.114 Uiso 1 1 calc R . . C153 C 0.7479(2) 0.4977(2) 0.29999(18) 0.0563(14) Uani 1 1 d . . . H153 H 0.7781 0.4880 0.2766 0.068 Uiso 1 1 calc R . . C154 C 0.6978(2) 0.5441(2) 0.29269(19) 0.0591(15) Uani 1 1 d . . . H154 H 0.6944 0.5658 0.2649 0.071 Uiso 1 1 calc R . . C155 C 0.2335(4) 0.6515(4) 0.2642(5) 0.244(8) Uani 1 1 d . . . H15C H 0.2425 0.6123 0.2577 0.293 Uiso 1 1 calc R B . H15D H 0.2520 0.6498 0.2897 0.293 Uiso 1 1 calc R . . H15E H 0.2486 0.6728 0.2394 0.293 Uiso 1 1 calc R . . C157 C 0.0479(4) 0.6362(4) 0.3332(3) 0.046(2) Uiso 0.50 1 d PD B 1 C158 C 0.0031(2) 0.6495(2) 0.30582(17) 0.0565(14) Uiso 1 1 d . . . H158 H -0.0085 0.6850 0.2877 0.068 Uiso 1 1 calc R B 1 C159 C -0.0238(2) 0.6104(2) 0.30572(19) 0.0650(15) Uiso 1 1 d . B . H159 H -0.0513 0.6181 0.2858 0.078 Uiso 1 1 calc R K 1 C160 C -0.0112(5) 0.5604(4) 0.3342(3) 0.048(2) Uiso 0.50 1 d P B 1 C161 C 0.0339(5) 0.5458(5) 0.3630(4) 0.073(3) Uiso 0.50 1 d P B 1 H161 H 0.0456 0.5098 0.3804 0.087 Uiso 0.50 1 calc PR B 1 C162 C 0.0596(6) 0.5852(5) 0.3644(4) 0.085(4) Uiso 0.50 1 d P B 1 H162 H 0.0847 0.5788 0.3858 0.102 Uiso 0.50 1 calc PR B 1 C163 C -0.0445(4) 0.5216(4) 0.3368(3) 0.040(2) Uiso 0.50 1 d P B 1 N8 N -0.1149(3) 0.4536(2) 0.34189(18) 0.0873(16) Uiso 1 1 d . . . C168 C -0.0403(3) 0.8648(4) 0.4610(3) 0.135(3) Uani 1 1 d . . . H16A H -0.0644 0.8548 0.4866 0.162 Uiso 1 1 calc R . . H16B H -0.0233 0.8327 0.4434 0.162 Uiso 1 1 calc R . . H16C H -0.0648 0.8990 0.4438 0.162 Uiso 1 1 calc R . . C169 C 0.1099(6) 0.8706(6) 0.5214(5) 0.082(4) Uiso 0.50 1 d P C 2 C170 C 0.0951(6) 0.8772(5) 0.5674(4) 0.061(3) Uiso 0.50 1 d P C 2 C171 C 0.1176(6) 0.8345(6) 0.5990(4) 0.075(3) Uiso 0.50 1 d P C 2 H171 H 0.1447 0.7985 0.5908 0.090 Uiso 0.50 1 calc PR C 2 C172 C 0.1025(6) 0.8413(6) 0.6437(4) 0.078(4) Uiso 0.50 1 d P C 2 H172 H 0.1195 0.8103 0.6647 0.093 Uiso 0.50 1 calc PR C 2 C173 C 0.0630(6) 0.8928(7) 0.6564(5) 0.054(3) Uiso 0.50 1 d P C 2 C174 C 0.0384(7) 0.9374(7) 0.6228(5) 0.085(4) Uiso 0.50 1 d P C 2 H174 H 0.0099 0.9736 0.6294 0.102 Uiso 0.50 1 calc PR C 2 C175 C 0.0580(6) 0.9255(6) 0.5804(4) 0.043(3) Uiso 0.50 1 d P C 2 H175 H 0.0427 0.9558 0.5583 0.051 Uiso 0.50 1 calc PR C 2 C176 C 0.0860(6) 0.8745(5) 0.7101(4) 0.065(3) Uiso 0.50 1 d P J 1 C177 C 0.1379(6) 0.8534(5) 0.7241(4) 0.079(4) Uiso 0.50 1 d P J 1 H177 H 0.1709 0.8460 0.7027 0.095 Uiso 0.50 1 calc PR J 1 C178 C 0.1493(8) 0.8404(7) 0.7685(6) 0.119(5) Uiso 0.50 1 d P J 1 H178 H 0.1876 0.8262 0.7772 0.143 Uiso 0.50 1 calc PR J 1 N9 N 0.0992(6) 0.8508(5) 0.7969(4) 0.111(4) Uiso 0.50 1 d P J 1 C179 C 0.0479(9) 0.8671(8) 0.7855(6) 0.109(5) Uiso 0.50 1 d P J 1 H179 H 0.0164 0.8692 0.8077 0.131 Uiso 0.50 1 calc PR J 1 C180 C 0.0342(6) 0.8830(6) 0.7404(5) 0.075(3) Uiso 0.50 1 d P J 1 H180 H -0.0044 0.8972 0.7323 0.090 Uiso 0.50 1 calc PR J 1 C181 C 1.4741(2) -0.0792(2) 0.4491(2) 0.0677(17) Uani 1 1 d . . . H18A H 1.5007 -0.1199 0.4486 0.081 Uiso 1 1 calc R . . H18B H 1.4525 -0.0747 0.4785 0.081 Uiso 1 1 calc R . . C182 C 1.4314(2) -0.0647(2) 0.4168(2) 0.0638(16) Uani 1 1 d . . . C183 C 1.3756(2) -0.0206(2) 0.4240(2) 0.0635(16) Uani 1 1 d . . . H183 H 1.3655 -0.0018 0.4494 0.076 Uiso 1 1 calc R . . C184 C 1.3354(2) -0.0045(2) 0.3935(2) 0.0609(16) Uani 1 1 d . . . C185 C 1.3476(2) -0.0300(2) 0.3565(2) 0.0644(16) Uani 1 1 d . . . C186 C 1.4031(2) -0.0745(2) 0.3486(2) 0.0720(17) Uani 1 1 d . . . H186 H 1.4129 -0.0927 0.3228 0.086 Uiso 1 1 calc R . . C187 C 1.4438(2) -0.0916(2) 0.3796(2) 0.0686(17) Uani 1 1 d . . . C188 C 1.5019(2) -0.1432(2) 0.3705(2) 0.0715(18) Uani 1 1 d . . . H18C H 1.5168 -0.1628 0.3984 0.086 Uiso 1 1 calc R . . H18D H 1.4936 -0.1711 0.3566 0.086 Uiso 1 1 calc R . . C189 C 1.5499(2) -0.1254(2) 0.3410(2) 0.0738(19) Uani 1 1 d . . . C190 C 1.5491(3) -0.1197(3) 0.2980(3) 0.088(2) Uani 1 1 d . . . H190 H 1.5195 -0.1265 0.2868 0.106 Uiso 1 1 calc R . . C191 C 1.5920(3) -0.1037(3) 0.2690(3) 0.099(2) Uani 1 1 d . . . C192 C 1.6353(3) -0.0935(3) 0.2837(3) 0.098(2) Uani 1 1 d . . . C193 C 1.6386(3) -0.1010(3) 0.3274(3) 0.091(2) Uani 1 1 d . . . H193 H 1.6694 -0.0957 0.3381 0.109 Uiso 1 1 calc R . . C194 C 1.5950(2) -0.1168(2) 0.3567(2) 0.0765(19) Uani 1 1 d . . . C195 C 1.6009(2) -0.1213(3) 0.4043(2) 0.086(2) Uani 1 1 d . . . H19A H 1.6428 -0.1361 0.4088 0.103 Uiso 1 1 calc R . . H19B H 1.5828 -0.1481 0.4213 0.103 Uiso 1 1 calc R . . C196 C 1.5692(2) -0.0601(2) 0.4195(2) 0.0738(18) Uani 1 1 d . . . C197 C 1.6001(3) -0.0223(3) 0.4108(2) 0.0814(19) Uani 1 1 d . . . H197 H 1.6397 -0.0353 0.3981 0.098 Uiso 1 1 calc R . . C198 C 1.5732(3) 0.0332(2) 0.4208(2) 0.0736(18) Uani 1 1 d . . . C199 C 1.5147(3) 0.0537(2) 0.4399(2) 0.0725(17) Uani 1 1 d . . . C200 C 1.4853(2) 0.0160(2) 0.4486(2) 0.0681(17) Uani 1 1 d . . . H200 H 1.4458 0.0293 0.4616 0.082 Uiso 1 1 calc R . . C201 C 1.5107(2) -0.0403(2) 0.4393(2) 0.0746(18) Uani 1 1 d . . . C202 C 1.2318(2) 0.0292(3) 0.41708(19) 0.0669(17) Uani 1 1 d . . . C203 C 1.1770(2) 0.0801(3) 0.41136(18) 0.0620(16) Uani 1 1 d . . . C204 C 1.1776(3) 0.1326(3) 0.3910(2) 0.092(2) Uani 1 1 d . . . H204 H 1.2142 0.1372 0.3822 0.111 Uiso 1 1 calc R . . C205 C 1.1259(3) 0.1791(3) 0.3828(2) 0.111(3) Uani 1 1 d . . . H205 H 1.1276 0.2142 0.3675 0.133 Uiso 1 1 calc R . . C206 C 1.0731(2) 0.1739(3) 0.39688(19) 0.0686(17) Uani 1 1 d . L . C207 C 1.0715(2) 0.1211(3) 0.4186(2) 0.094(2) Uani 1 1 d . . . H207 H 1.0350 0.1167 0.4286 0.112 Uiso 1 1 calc R . . C208 C 1.1235(2) 0.0756(3) 0.4253(2) 0.081(2) Uani 1 1 d . . . H208 H 1.1220 0.0401 0.4400 0.097 Uiso 1 1 calc R . . C209 C 1.0173(2) 0.2223(3) 0.38623(19) 0.0691(17) Uani 1 1 d . . . C210 C 1.0054(4) 0.2861(4) 0.3977(3) 0.042(2) Uiso 0.50 1 d P L 1 H210 H 1.0332 0.2933 0.4109 0.051 Uiso 0.50 1 calc PR L 1 C211 C 0.9549(4) 0.3287(4) 0.3879(3) 0.039(2) Uiso 0.50 1 d P L 1 H211 H 0.9459 0.3662 0.3953 0.046 Uiso 0.50 1 calc PR L 1 C212 C 0.9269(4) 0.2697(4) 0.3537(3) 0.046(2) Uiso 0.50 1 d P L 1 H212 H 0.9006 0.2655 0.3370 0.055 Uiso 0.50 1 calc PR L 1 C213 C 0.9769(4) 0.2234(4) 0.3635(3) 0.046(2) Uiso 0.50 1 d P L 1 H213 H 0.9828 0.1886 0.3527 0.055 Uiso 0.50 1 calc PR L 1 C214 C 0.9711(5) 0.2321(5) 0.4195(4) 0.071(3) Uiso 0.50 1 d P L 2 H214 H 0.9727 0.2080 0.4462 0.085 Uiso 0.50 1 calc PR L 2 C215 C 0.9198(5) 0.2833(5) 0.4090(4) 0.064(3) Uiso 0.50 1 d P L 2 H215 H 0.8875 0.2945 0.4308 0.077 Uiso 0.50 1 calc PR L 2 C216 C 0.9620(5) 0.2874(5) 0.3360(4) 0.075(3) Uiso 0.50 1 d P L 2 H216 H 0.9586 0.3006 0.3062 0.090 Uiso 0.50 1 calc PR L 2 C217 C 1.0102(6) 0.2408(5) 0.3464(4) 0.075(3) Uiso 0.50 1 d P L 2 H217 H 1.0385 0.2220 0.3241 0.090 Uiso 0.50 1 calc PR L 2 C218 C 1.3167(3) -0.0334(3) 0.2897(2) 0.0854(19) Uani 1 1 d . . . H21A H 1.2825 -0.0155 0.2736 0.102 Uiso 1 1 calc R . . H21B H 1.3258 -0.0750 0.2953 0.102 Uiso 1 1 calc R . . H21C H 1.3504 -0.0260 0.2725 0.102 Uiso 1 1 calc R . . C219 C 1.6266(3) -0.1298(3) 0.1955(3) 0.087(2) Uani 1 1 d . . . C220 C 1.6194(3) -0.1115(3) 0.1518(2) 0.0800(19) Uani 1 1 d . . . C221 C 1.5789(4) -0.0593(3) 0.1400(3) 0.114(3) Uani 1 1 d . . . H221 H 1.5565 -0.0345 0.1613 0.137 Uiso 1 1 calc R . . C222 C 1.5706(4) -0.0422(4) 0.0964(3) 0.135(3) Uani 1 1 d . . . H222 H 1.5416 -0.0057 0.0889 0.163 Uiso 1 1 calc R . . C223 C 1.6033(4) -0.0767(4) 0.0620(3) 0.112(3) Uani 1 1 d . . . C224 C 1.6461(3) -0.1311(4) 0.0772(3) 0.116(3) Uani 1 1 d . . . H224 H 1.6700 -0.1559 0.0563 0.139 Uiso 1 1 calc R . . C225 C 1.6546(3) -0.1494(4) 0.1200(2) 0.105(2) Uani 1 1 d . . . H225 H 1.6828 -0.1859 0.1284 0.125 Uiso 1 1 calc R . . C226 C 1.5924(4) -0.0570(5) 0.0155(3) 0.129(3) Uani 1 1 d . . . C227 C 1.5722(5) 0.0012(5) -0.0006(4) 0.190(5) Uani 1 1 d . . . H227 H 1.5652 0.0291 0.0183 0.228 Uiso 1 1 calc R . . C228 C 1.5627(6) 0.0181(7) -0.0412(5) 0.260(9) Uani 1 1 d . . . H228 H 1.5524 0.0576 -0.0520 0.312 Uiso 1 1 calc R . . N11 N 1.5676(5) -0.0225(6) -0.0695(3) 0.239(7) Uani 1 1 d . . . C229 C 1.5850(5) -0.0780(6) -0.0561(4) 0.195(6) Uani 1 1 d . . . H229 H 1.5902 -0.1057 -0.0748 0.234 Uiso 1 1 calc R . . C230 C 1.5956(4) -0.0940(4) -0.0121(3) 0.148(4) Uani 1 1 d . . . H230 H 1.6057 -0.1335 -0.0012 0.178 Uiso 1 1 calc R . . C231 C 1.7149(4) -0.0592(4) 0.2668(3) 0.160(4) Uani 1 1 d . . . H23A H 1.7402 -0.0493 0.2420 0.192 Uiso 1 1 calc R . . H23B H 1.7390 -0.0900 0.2865 0.192 Uiso 1 1 calc R . . H23C H 1.6927 -0.0253 0.2820 0.192 Uiso 1 1 calc R . . C232 C 1.6393(2) 0.0716(3) 0.4369(2) 0.0776(19) Uani 1 1 d . . . C233 C 1.6613(2) 0.1196(2) 0.4233(2) 0.0656(16) Uani 1 1 d . . . C234 C 1.6932(2) 0.1290(2) 0.4522(2) 0.0697(17) Uani 1 1 d . . . H234 H 1.7001 0.1052 0.4790 0.084 Uiso 1 1 calc R . . C235 C 1.7149(3) 0.1737(2) 0.4413(2) 0.0699(17) Uani 1 1 d . . . H235 H 1.7353 0.1810 0.4611 0.084 Uiso 1 1 calc R . . C236 C 1.7064(2) 0.2084(2) 0.4002(2) 0.0632(16) Uani 1 1 d . . . C237 C 1.6771(3) 0.1962(2) 0.3718(2) 0.0709(17) Uani 1 1 d . . . H237 H 1.6727 0.2174 0.3439 0.085 Uiso 1 1 calc R . . C238 C 1.6538(3) 0.1526(3) 0.3840(2) 0.0757(18) Uani 1 1 d . . . H238 H 1.6325 0.1458 0.3646 0.091 Uiso 1 1 calc R . . C239 C 1.7310(2) 0.2543(2) 0.3887(2) 0.0600(15) Uani 1 1 d . . . C240 C 1.7476(2) 0.2730(2) 0.3456(2) 0.0690(17) Uani 1 1 d . . . H240 H 1.7403 0.2578 0.3226 0.083 Uiso 1 1 calc R . . C241 C 1.7740(2) 0.3128(2) 0.33615(19) 0.0595(15) Uani 1 1 d . . . H241 H 1.7847 0.3239 0.3066 0.071 Uiso 1 1 calc R . . C242 C 1.7678(2) 0.3223(2) 0.4071(2) 0.0722(17) Uani 1 1 d . . . H242 H 1.7731 0.3409 0.4289 0.087 Uiso 1 1 calc R . . C243 C 1.7414(3) 0.2808(3) 0.4201(2) 0.0754(18) Uani 1 1 d . . . H243 H 1.7308 0.2711 0.4500 0.090 Uiso 1 1 calc R . . C244 C 1.4310(3) 0.1335(3) 0.4637(3) 0.114(3) Uani 1 1 d . . . H24A H 1.4194 0.1738 0.4685 0.136 Uiso 1 1 calc R . . H24B H 1.4237 0.1111 0.4911 0.136 Uiso 1 1 calc R . . H24C H 1.4080 0.1309 0.4423 0.136 Uiso 1 1 calc R . . C245 C 0.8889(3) 0.3752(2) 0.25433(19) 0.0643(15) Uiso 1 1 d . . . C246 C 0.9004(5) 0.3247(5) 0.2235(4) 0.147(3) Uiso 1 1 d . . . C251 C 0.1549(3) 1.0578(3) 0.2424(2) 0.0791(18) Uiso 1 1 d . A . C252 C 0.1440(4) 1.0995(4) 0.2764(3) 0.106(2) Uiso 1 1 d . . . N18 N 0.8432(4) 0.7485(4) 0.0375(3) 0.148(3) Uiso 1 1 d . . . C254 C 0.8885(5) 0.7087(4) 0.0642(3) 0.155(4) Uiso 1 1 d . I . H25D H 0.9114 0.7277 0.0741 0.185 Uiso 1 1 calc R . . H25E H 0.9151 0.6748 0.0496 0.185 Uiso 1 1 calc R . . C255 C 0.8438(5) 0.6937(5) 0.1017(4) 0.186(4) Uiso 1 1 d . . . H25F H 0.8601 0.6521 0.1118 0.223 Uiso 1 1 calc R I . H25G H 0.8395 0.7150 0.1264 0.223 Uiso 1 1 calc R . . C256 C 0.7865(4) 0.7075(4) 0.0885(3) 0.120(3) Uiso 1 1 d . I . H25H H 0.7546 0.7293 0.1095 0.144 Uiso 1 1 calc R M 1 H25I H 0.7801 0.6728 0.0840 0.144 Uiso 1 1 calc R M 1 O50 O 0.7538(2) 0.7701(2) 0.01860(17) 0.1094(15) Uiso 1 1 d . . . C258 C 0.1327(5) 0.5462(5) 0.1984(4) 0.075(3) Uiso 0.50 1 d P E 1 C259 C 0.1388(6) 0.5979(5) 0.2174(4) 0.081(4) Uiso 0.50 1 d P E 1 H25J H 0.1008 0.6243 0.2302 0.097 Uiso 0.50 1 calc PR E 1 H25K H 0.1679 0.5845 0.2385 0.097 Uiso 0.50 1 calc PR E 1 C260 C 0.1582(7) 0.6205(7) 0.1789(5) 0.110(5) Uiso 0.50 1 d P E 1 H26A H 0.2012 0.6091 0.1775 0.132 Uiso 0.50 1 calc PR E 1 H26B H 0.1408 0.6629 0.1778 0.132 Uiso 0.50 1 calc PR E 1 C261 C 0.1453(5) 0.6041(5) 0.1403(4) 0.074(3) Uiso 0.50 1 d P E 1 H26C H 0.1126 0.6359 0.1273 0.089 Uiso 0.50 1 calc PR E 1 H26D H 0.1802 0.5947 0.1184 0.089 Uiso 0.50 1 calc PR E 1 C262 C 0.1259(5) 0.5192(4) 0.1388(3) 0.056(3) Uiso 0.50 1 d P E 1 H26E H 0.1240 0.5307 0.1077 0.067 Uiso 0.50 1 calc PR E 1 H26F H 0.0902 0.5123 0.1521 0.067 Uiso 0.50 1 calc PR E 1 H26G H 0.1602 0.4839 0.1435 0.067 Uiso 0.50 1 calc PR E 1 C263 C 0.2737(5) 0.4798(5) 0.1009(4) 0.065(3) Uiso 0.50 1 d P D 1 C264 C 0.2657(7) 0.4320(6) 0.1479(5) 0.110(5) Uiso 0.50 1 d P D 1 H26H H 0.3036 0.4011 0.1538 0.131 Uiso 0.50 1 calc PR D 1 H26I H 0.2478 0.4526 0.1738 0.131 Uiso 0.50 1 calc PR D 1 C265 C 0.2254(11) 0.4095(11) 0.1336(8) 0.206(10) Uiso 0.50 1 d P D 1 H26J H 0.1852 0.4266 0.1483 0.247 Uiso 0.50 1 calc PR D 1 H26K H 0.2389 0.3672 0.1405 0.247 Uiso 0.50 1 calc PR D 1 C266 C 0.2265(5) 0.4274(4) 0.0810(3) 0.052(3) Uiso 0.50 1 d P D 1 H26L H 0.2483 0.3934 0.0652 0.062 Uiso 0.50 1 calc PR D 1 H26M H 0.1862 0.4454 0.0726 0.062 Uiso 0.50 1 calc PR D 1 C267 C 0.2558(6) 0.4923(5) 0.0322(4) 0.085(4) Uiso 0.50 1 d P D 1 H26N H 0.2398 0.4751 0.0142 0.102 Uiso 0.50 1 calc PR D 1 H26O H 0.2963 0.4875 0.0205 0.102 Uiso 0.50 1 calc PR D 1 H26P H 0.2320 0.5333 0.0321 0.102 Uiso 0.50 1 calc PR D 1 N14 N -0.3156(3) 0.7075(3) 0.3400(2) 0.0437(19) Uiso 0.50 1 d P F 1 C269 C -0.3516(6) 0.7185(5) 0.3792(4) 0.076(3) Uiso 0.50 1 d P F 1 H26Q H -0.3934 0.7330 0.3744 0.091 Uiso 0.50 1 calc PR F 1 H26R H -0.3447 0.7477 0.3925 0.091 Uiso 0.50 1 calc PR F 1 C270 C -0.3364(6) 0.6630(5) 0.4081(4) 0.090(4) Uiso 0.50 1 d P F 1 H27D H -0.3637 0.6433 0.4074 0.108 Uiso 0.50 1 calc PR F 1 H27E H -0.3361 0.6686 0.4383 0.108 Uiso 0.50 1 calc PR F 1 C271 C -0.2728(5) 0.6292(5) 0.3863(4) 0.068(3) Uiso 0.50 1 d P F 1 H27F H -0.2427 0.6336 0.4009 0.082 Uiso 0.50 1 calc PR F 1 H27G H -0.2657 0.5877 0.3881 0.082 Uiso 0.50 1 calc PR F 1 O273 O -0.2394(3) 0.6379(2) 0.3095(2) 0.0444(16) Uiso 0.50 1 d P F 1 C273 C 1.5156(5) -0.2593(4) 0.4721(4) 0.056(3) Uiso 0.50 1 d P H 1 C274 C 1.5069(6) -0.2930(6) 0.4361(4) 0.090(4) Uiso 0.50 1 d P H 1 H27H H 1.4977 -0.2672 0.4088 0.108 Uiso 0.50 1 calc PR H 1 H27I H 1.5430 -0.3265 0.4297 0.108 Uiso 0.50 1 calc PR H 1 C275 C 1.4582(6) -0.3120(6) 0.4541(5) 0.099(4) Uiso 0.50 1 d P H 1 H27J H 1.4697 -0.3536 0.4525 0.118 Uiso 0.50 1 calc PR H 1 H27K H 1.4238 -0.2906 0.4381 0.118 Uiso 0.50 1 calc PR H 1 C276 C 1.4444(5) -0.2994(5) 0.5008(4) 0.069(3) Uiso 0.50 1 d P H 1 H27L H 1.4021 -0.2776 0.5081 0.083 Uiso 0.50 1 calc PR H 1 H27M H 1.4568 -0.3351 0.5210 0.083 Uiso 0.50 1 calc PR H 1 C277 C 1.4751(5) -0.2413(5) 0.5432(4) 0.076(3) Uiso 0.50 1 d P H 1 H27N H 1.4441 -0.2487 0.5641 0.091 Uiso 0.50 1 calc PR H 1 H27O H 1.4661 -0.1997 0.5373 0.091 Uiso 0.50 1 calc PR H 1 H27P H 1.5127 -0.2599 0.5552 0.091 Uiso 0.50 1 calc PR H 1 C278 C 0.2151(6) 0.7560(6) 0.4153(4) 0.082(4) Uiso 0.50 1 d P G 1 H27Q H 0.2557 0.7293 0.4080 0.098 Uiso 0.50 1 calc PR G 1 H27R H 0.2092 0.7943 0.3989 0.098 Uiso 0.50 1 calc PR G 1 C279 C 0.1699(5) 0.7327(5) 0.4092(4) 0.066(3) Uiso 0.50 1 d P G 1 H27S H 0.1499 0.7559 0.3839 0.080 Uiso 0.50 1 calc PR G 1 H27T H 0.1910 0.6930 0.4015 0.080 Uiso 0.50 1 calc PR G 1 C280 C 0.1290(6) 0.7312(5) 0.4418(4) 0.077(3) Uiso 0.50 1 d P G 1 H28D H 0.1275 0.6921 0.4487 0.092 Uiso 0.50 1 calc PR G 1 H28E H 0.0899 0.7587 0.4348 0.092 Uiso 0.50 1 calc PR G 1 N15 N 0.1470(4) 0.7474(4) 0.4781(3) 0.072(3) Uiso 0.50 1 d P G 1 O48 O 0.2172(4) 0.7796(3) 0.4892(3) 0.080(2) Uiso 0.50 1 d P G 1 C156 C 0.0795(5) 0.6747(5) 0.3338(4) 0.062(3) Uiso 0.50 1 d PD B 1 O28B O 0.0376(6) 0.7224(6) 0.3772(5) 0.172(5) Uiso 0.50 1 d P B 2 C60B C -0.0532(7) 0.5909(6) 0.3417(5) 0.090(4) Uiso 0.50 1 d P B 2 C57B C 0.0043(6) 0.6681(6) 0.3429(4) 0.080(4) Uiso 0.50 1 d P B 2 C56B C 0.0393(7) 0.7044(7) 0.3439(6) 0.100(4) Uiso 0.50 1 d P B 2 C59B C -0.0493(9) 0.6068(9) 0.3818(7) 0.160(7) Uiso 0.50 1 d P B 2 H59B H -0.0642 0.5906 0.4083 0.192 Uiso 0.50 1 calc PR B 2 C58B C -0.0214(8) 0.6487(8) 0.3811(6) 0.132(6) Uiso 0.50 1 d P B 2 H58B H -0.0213 0.6625 0.4073 0.159 Uiso 0.50 1 calc PR B 2 C67B C -0.0528(5) 0.5033(5) 0.3154(4) 0.066(3) Uiso 0.50 1 d P B 2 H67B H -0.0193 0.5023 0.2954 0.079 Uiso 0.50 1 calc PR B 2 C66B C -0.0771(5) 0.4592(5) 0.3171(4) 0.057(3) Uiso 0.50 1 d P B 2 H66B H -0.0606 0.4328 0.2961 0.069 Uiso 0.50 1 calc PR B 2 C63B C -0.0772(7) 0.5472(6) 0.3425(4) 0.076(4) Uiso 0.50 1 d P B 2 C64B C -0.1278(7) 0.5487(6) 0.3652(5) 0.095(4) Uiso 0.50 1 d P B 2 H64B H -0.1474 0.5781 0.3837 0.114 Uiso 0.50 1 calc PR B 2 C65B C -0.1536(6) 0.5086(5) 0.3633(5) 0.087(4) Uiso 0.50 1 d P B 2 H65B H -0.1933 0.5151 0.3746 0.104 Uiso 0.50 1 calc PR B 2 C64C C -0.1002(6) 0.5423(5) 0.3283(4) 0.067(3) Uiso 0.50 1 d P B 1 H64C H -0.1194 0.5824 0.3206 0.080 Uiso 0.50 1 calc PR B 1 C67C C -0.0155(8) 0.4635(7) 0.3464(5) 0.115(5) Uiso 0.50 1 d P B 1 H67C H 0.0244 0.4476 0.3518 0.137 Uiso 0.50 1 calc PR B 1 C65C C -0.1308(5) 0.5044(5) 0.3307(4) 0.064(3) Uiso 0.50 1 d P B 1 H65C H -0.1692 0.5217 0.3222 0.077 Uiso 0.50 1 calc PR B 1 C66C C -0.0501(7) 0.4274(7) 0.3477(5) 0.109(5) Uiso 0.50 1 d P B 1 H66C H -0.0316 0.3868 0.3522 0.131 Uiso 0.50 1 calc PR B 1 C304 C 0.6076(6) 1.4131(5) 0.3493(4) 0.083(4) Uiso 0.50 1 d P . . H30A H 0.5845 1.4467 0.3653 0.100 Uiso 0.50 1 calc PR . . H30B H 0.6446 1.3919 0.3624 0.100 Uiso 0.50 1 calc PR . . C303 C 0.6185(6) 1.4295(6) 0.3099(4) 0.091(4) Uiso 0.50 1 d P . . H30C H 0.6600 1.4259 0.3025 0.109 Uiso 0.50 1 calc PR . . H30D H 0.5927 1.4697 0.3018 0.109 Uiso 0.50 1 calc PR . . C300 C 0.5751(7) 1.3765(7) 0.3521(6) 0.105(5) Uiso 0.50 1 d P . . N301 N 0.5678(8) 1.3702(8) 0.3200(7) 0.166(6) Uiso 0.50 1 d PD . . C302 C 0.6044(10) 1.3850(9) 0.2878(7) 0.158(7) Uiso 0.50 1 d P . . H30E H 0.5848 1.4035 0.2613 0.189 Uiso 0.50 1 calc PR . . H30F H 0.6401 1.3516 0.2806 0.189 Uiso 0.50 1 calc PR . . O306 O 0.5482(6) 1.3656(5) 0.3899(4) 0.143(4) Uiso 0.50 1 d P . . C305 C 0.5460(10) 1.3226(9) 0.3169(8) 0.198(9) Uiso 0.50 1 d PD . . H30G H 0.5453 1.3199 0.2863 0.238 Uiso 0.50 1 calc PR . . H30H H 0.5065 1.3313 0.3322 0.238 Uiso 0.50 1 calc PR . . H30I H 0.5724 1.2859 0.3300 0.238 Uiso 0.50 1 calc PR . . F1 F 0.1590(5) 1.1495(4) 0.2516(3) 0.148(3) Uiso 0.50 1 d P A 1 F2 F 0.0936(6) 1.1311(6) 0.2967(4) 0.169(4) Uiso 0.50 1 d P A 1 F3 F 0.1789(4) 1.0802(4) 0.3063(3) 0.111(3) Uiso 0.50 1 d P A 1 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 0.0492(4) 0.0458(4) 0.0929(5) -0.0156(3) -0.0060(4) -0.0216(3) Zn2 0.0391(4) 0.0385(3) 0.0979(5) -0.0064(3) -0.0063(3) -0.0185(3) O1 0.118(4) 0.064(3) 0.149(5) -0.007(3) -0.029(3) -0.057(3) O2 0.111(3) 0.104(3) 0.083(3) 0.015(2) -0.027(3) -0.088(3) O3 0.144(4) 0.099(3) 0.086(3) 0.019(3) -0.034(3) -0.093(3) O4 0.113(4) 0.257(7) 0.131(5) -0.095(5) 0.034(3) -0.132(5) O5 0.076(3) 0.204(6) 0.112(4) -0.077(4) 0.015(3) -0.075(4) O6 0.095(4) 0.185(6) 0.134(5) -0.057(4) -0.019(4) -0.045(4) O7 0.047(2) 0.063(2) 0.087(3) -0.004(2) -0.027(2) -0.0169(19) O8 0.039(2) 0.041(2) 0.109(3) -0.006(2) -0.017(2) -0.0134(18) O9 0.045(2) 0.049(2) 0.086(3) -0.0026(19) -0.0140(19) -0.0201(18) O10 0.044(2) 0.0337(19) 0.108(3) -0.0109(19) -0.002(2) -0.0118(17) O11 0.038(2) 0.0416(19) 0.090(3) -0.0079(18) -0.0035(19) -0.0102(17) O12 0.047(2) 0.052(2) 0.089(3) -0.0029(19) -0.017(2) -0.0185(18) O13 0.038(2) 0.069(2) 0.083(3) -0.020(2) 0.0080(19) -0.0170(19) O14 0.078(3) 0.142(4) 0.096(4) -0.011(3) -0.015(3) 0.031(3) O15 0.060(3) 0.104(3) 0.080(3) -0.006(2) -0.002(2) -0.044(2) O16 0.054(2) 0.063(2) 0.083(3) -0.0091(19) -0.0144(19) -0.0393(19) O17 0.577(16) 0.333(10) 0.111(5) 0.074(6) -0.130(7) -0.397(12) O18 0.071(3) 0.058(2) 0.138(4) -0.041(2) -0.003(3) -0.034(2) O19 0.084(3) 0.040(2) 0.125(4) 0.003(2) 0.008(3) -0.005(2) O21 0.052(2) 0.060(2) 0.079(3) -0.019(2) 0.008(2) -0.0213(19) O23 0.048(2) 0.070(2) 0.106(3) -0.024(2) -0.013(2) -0.017(2) O24 0.035(2) 0.056(2) 0.132(4) -0.035(2) 0.009(2) -0.0166(18) O25 0.050(2) 0.049(2) 0.119(3) -0.024(2) 0.000(2) -0.0174(19) O26 0.064(3) 0.060(3) 0.207(5) -0.045(3) -0.041(3) -0.016(2) O27 0.071(3) 0.062(2) 0.089(3) 0.004(2) -0.026(2) -0.043(2) O29 0.068(3) 0.095(3) 0.081(3) 0.001(2) -0.004(2) -0.038(2) O30 0.066(3) 0.108(3) 0.064(3) -0.030(2) 0.001(2) -0.018(2) O32 0.035(2) 0.071(2) 0.095(3) -0.018(2) -0.0085(19) -0.0195(19) O33 0.049(2) 0.066(2) 0.135(4) -0.032(2) -0.004(2) -0.019(2) O34 0.052(2) 0.090(3) 0.083(3) -0.023(2) -0.010(2) -0.021(2) O35 0.073(3) 0.102(3) 0.145(5) -0.028(3) 0.017(3) -0.027(3) O36 0.086(4) 0.113(4) 0.149(5) -0.039(3) 0.005(3) -0.040(3) O37 0.108(4) 0.128(4) 0.159(5) -0.055(4) 0.044(3) -0.073(4) O38 0.092(3) 0.073(3) 0.113(4) 0.001(2) -0.032(3) -0.054(2) O39 0.086(3) 0.104(3) 0.112(4) 0.026(3) -0.031(3) -0.068(3) O40 0.085(3) 0.055(2) 0.140(4) -0.020(3) -0.027(3) -0.021(2) O41 0.052(2) 0.070(2) 0.089(3) -0.031(2) 0.009(2) -0.026(2) O43 0.077(3) 0.064(3) 0.150(4) 0.010(3) -0.020(3) -0.044(2) N1 0.045(3) 0.044(2) 0.088(4) 0.001(2) -0.017(2) -0.026(2) N3 0.048(3) 0.043(3) 0.113(4) -0.018(3) -0.012(3) -0.022(2) N4 0.037(2) 0.045(2) 0.069(3) -0.002(2) 0.008(2) -0.019(2) N6 0.054(3) 0.048(3) 0.110(4) -0.022(3) 0.005(3) -0.029(2) N7 0.051(3) 0.058(3) 0.069(3) -0.007(2) 0.009(2) -0.025(2) N10 0.039(3) 0.080(3) 0.074(3) -0.025(3) 0.001(2) -0.026(2) N12 0.049(3) 0.046(2) 0.075(3) 0.002(2) -0.010(2) -0.011(2) C1 0.048(3) 0.049(3) 0.090(4) -0.002(3) -0.015(3) -0.033(3) C2 0.057(4) 0.051(3) 0.074(4) 0.009(3) -0.021(3) -0.033(3) C3 0.069(4) 0.065(4) 0.077(4) -0.001(3) -0.016(3) -0.041(3) C4 0.072(4) 0.060(4) 0.099(5) -0.003(3) -0.021(4) -0.044(4) C5 0.099(5) 0.095(5) 0.081(5) 0.015(4) -0.028(4) -0.081(5) C6 0.064(4) 0.085(4) 0.069(4) -0.009(3) -0.014(3) -0.045(4) C7 0.051(3) 0.061(3) 0.073(4) 0.000(3) -0.020(3) -0.033(3) C8 0.032(3) 0.068(4) 0.136(6) -0.018(4) -0.022(3) -0.018(3) C9 0.042(4) 0.095(5) 0.109(5) -0.045(4) -0.008(4) -0.028(3) C10 0.051(4) 0.139(6) 0.116(6) -0.064(5) 0.009(4) -0.049(4) C11 0.074(5) 0.190(8) 0.126(7) -0.083(6) 0.023(5) -0.085(6) C12 0.072(5) 0.141(6) 0.111(6) -0.064(5) 0.004(4) -0.048(5) C13 0.045(4) 0.099(5) 0.118(6) -0.040(4) -0.010(4) -0.031(4) C14 0.043(3) 0.073(4) 0.096(5) -0.029(4) -0.011(3) -0.022(3) C15 0.057(4) 0.070(4) 0.107(5) -0.020(4) -0.021(4) -0.030(3) C16 0.039(3) 0.040(3) 0.086(4) 0.001(3) -0.015(3) -0.018(3) C17 0.047(3) 0.047(3) 0.075(4) -0.010(3) 0.001(3) -0.026(3) C18 0.050(4) 0.054(3) 0.083(4) 0.006(3) -0.016(3) -0.032(3) C19 0.043(3) 0.047(3) 0.085(4) 0.002(3) -0.009(3) -0.023(3) C20 0.056(4) 0.053(3) 0.063(4) 0.001(3) -0.013(3) -0.031(3) C21 0.037(3) 0.036(3) 0.071(4) 0.006(3) -0.017(3) -0.020(2) C22 0.147(8) 0.062(5) 0.185(9) -0.031(5) -0.025(7) -0.039(5) C23 0.100(5) 0.084(4) 0.076(5) 0.003(4) -0.028(4) -0.060(4) C24 0.085(4) 0.075(4) 0.062(4) 0.016(3) -0.026(3) -0.058(4) C25 0.115(5) 0.091(4) 0.078(5) 0.020(4) -0.031(4) -0.077(4) C26 0.080(4) 0.083(4) 0.081(5) 0.016(4) -0.027(4) -0.060(4) C27 0.049(3) 0.049(3) 0.084(4) 0.000(3) -0.013(3) -0.029(3) C28 0.115(6) 0.088(5) 0.098(5) 0.019(4) -0.029(4) -0.077(5) C29 0.096(5) 0.097(5) 0.111(6) 0.005(4) -0.031(4) -0.071(4) C30 0.054(3) 0.039(3) 0.067(4) -0.001(3) -0.006(3) -0.022(3) C31 0.053(3) 0.047(3) 0.089(4) 0.000(3) -0.022(3) -0.024(3) C32 0.062(4) 0.059(4) 0.085(5) 0.005(3) -0.028(3) -0.028(3) C33 0.051(3) 0.046(3) 0.092(5) 0.017(3) -0.019(3) -0.023(3) C34 0.046(3) 0.050(3) 0.085(4) 0.000(3) -0.013(3) -0.030(3) C35 0.101(6) 0.210(9) 0.147(8) -0.090(7) 0.029(5) -0.091(7) C36 0.110(7) 0.180(9) 0.070(5) -0.056(6) 0.007(5) -0.091(7) C37 0.058(5) 0.125(7) 0.154(8) -0.051(6) 0.006(5) -0.051(5) C38 0.078(5) 0.120(6) 0.151(8) -0.047(6) 0.012(5) -0.053(5) C39 0.121(8) 0.172(9) 0.118(7) -0.050(7) 0.028(6) -0.092(7) C40 0.119(8) 0.150(8) 0.129(8) -0.035(7) 0.029(6) -0.094(7) C41 0.112(7) 0.126(7) 0.167(9) -0.049(7) 0.022(7) -0.066(6) C42 0.138(8) 0.177(9) 0.093(6) -0.069(6) 0.045(6) -0.106(7) C43 0.149(8) 0.118(7) 0.109(7) -0.015(6) 0.030(6) -0.071(6) C44 0.55(3) 0.200(13) 0.136(11) 0.009(9) 0.014(14) -0.241(18) C45 0.52(3) 0.180(12) 0.102(9) -0.013(8) -0.035(13) -0.096(16) N2 0.257(12) 0.204(10) 0.129(8) -0.014(7) 0.058(7) -0.136(10) C46 0.135(8) 0.162(9) 0.139(9) -0.026(8) 0.025(7) -0.063(8) C47 0.105(7) 0.184(9) 0.102(7) -0.053(7) 0.018(5) -0.058(7) C48 0.070(4) 0.086(4) 0.082(5) 0.003(4) -0.026(4) -0.042(4) C49 0.040(3) 0.054(3) 0.068(4) -0.008(3) -0.011(3) -0.019(3) C50 0.041(3) 0.046(3) 0.082(4) -0.003(3) -0.015(3) -0.019(3) C51 0.047(3) 0.040(3) 0.087(4) -0.007(3) -0.012(3) -0.010(3) C52 0.038(3) 0.049(3) 0.080(4) -0.018(3) 0.003(3) -0.021(3) C53 0.043(3) 0.059(3) 0.074(4) -0.011(3) -0.010(3) -0.017(3) C54 0.050(4) 0.039(3) 0.143(6) 0.003(3) -0.030(4) -0.018(3) C55 0.040(3) 0.052(3) 0.133(6) 0.009(4) -0.028(4) -0.017(3) C56 0.050(3) 0.052(3) 0.094(5) -0.010(3) -0.012(3) -0.023(3) C57 0.047(3) 0.044(3) 0.080(4) -0.014(3) -0.014(3) -0.018(3) C58 0.047(3) 0.056(4) 0.091(5) -0.009(3) -0.017(3) -0.023(3) C59 0.064(4) 0.057(4) 0.119(6) -0.023(4) -0.031(4) -0.023(3) C60 0.068(4) 0.070(4) 0.098(5) -0.018(4) -0.026(4) -0.033(4) C61 0.034(3) 0.048(3) 0.074(4) -0.020(3) 0.011(3) -0.022(2) C62 0.030(3) 0.048(3) 0.073(4) -0.011(3) 0.003(3) -0.027(2) C63 0.037(3) 0.043(3) 0.072(4) -0.019(3) 0.012(3) -0.025(3) C64 0.037(3) 0.033(3) 0.096(5) -0.008(3) -0.006(3) -0.017(3) C65 0.045(3) 0.049(3) 0.075(4) -0.005(3) -0.001(3) -0.030(3) C66 0.035(3) 0.052(3) 0.062(4) -0.011(3) 0.000(3) -0.022(3) C67 0.036(3) 0.040(3) 0.073(4) -0.010(3) 0.003(3) -0.024(2) C68 0.037(3) 0.042(3) 0.063(4) -0.017(3) 0.002(3) -0.013(2) C69 0.026(3) 0.038(3) 0.085(4) -0.027(3) 0.013(3) -0.010(2) C70 0.031(3) 0.056(3) 0.068(4) -0.020(3) -0.001(3) -0.014(3) C71 0.045(3) 0.048(3) 0.058(4) -0.011(3) -0.002(3) -0.010(3) C72 0.038(3) 0.066(4) 0.075(4) -0.019(3) 0.011(3) -0.030(3) C73 0.029(3) 0.047(3) 0.068(4) -0.015(3) 0.009(3) -0.013(2) C74 0.041(3) 0.037(3) 0.065(4) -0.017(3) -0.005(3) -0.007(2) C75 0.027(3) 0.053(3) 0.073(4) -0.019(3) 0.002(3) -0.019(2) C76 0.032(3) 0.043(3) 0.063(4) -0.003(3) -0.012(3) -0.015(2) C77 0.032(3) 0.055(3) 0.077(4) -0.016(3) -0.008(3) -0.016(3) C78 0.050(3) 0.052(3) 0.071(4) -0.001(3) -0.014(3) -0.030(3) C79 0.034(3) 0.046(3) 0.085(4) -0.019(3) -0.003(3) -0.018(3) C80 0.034(3) 0.052(3) 0.080(4) -0.027(3) 0.007(3) -0.022(3) C81 0.039(3) 0.057(3) 0.058(4) -0.014(3) -0.007(3) -0.024(3) C82 0.038(3) 0.035(3) 0.092(4) -0.013(3) 0.001(3) -0.017(2) C83 0.041(3) 0.038(3) 0.105(5) -0.003(3) -0.007(3) -0.013(3) C84 0.039(4) 0.055(4) 0.183(8) 0.004(4) -0.003(4) -0.021(3) C85 0.037(4) 0.045(4) 0.222(9) 0.002(4) -0.018(4) -0.009(3) C86 0.044(3) 0.044(3) 0.093(5) -0.006(3) -0.009(3) -0.008(3) C87 0.047(3) 0.062(4) 0.079(4) -0.006(3) -0.007(3) -0.027(3) C88 0.043(3) 0.048(3) 0.081(4) -0.003(3) -0.007(3) -0.017(3) C89 0.048(3) 0.048(3) 0.085(5) -0.002(3) -0.005(3) -0.020(3) C90 0.060(4) 0.043(3) 0.083(5) -0.005(3) 0.007(3) -0.013(3) C91 0.043(3) 0.047(3) 0.067(4) -0.013(3) 0.005(3) -0.015(3) C92 0.053(4) 0.055(4) 0.107(5) 0.017(3) 0.004(4) -0.009(3) C93 0.050(4) 0.082(5) 0.134(6) 0.024(4) 0.011(4) -0.028(4) C94 0.060(4) 0.079(4) 0.074(4) 0.007(3) -0.024(3) -0.038(3) C95 0.022(3) 0.086(4) 0.091(5) -0.038(4) 0.014(3) 0.013(3) C96 0.034(3) 0.067(4) 0.069(4) -0.021(3) 0.002(3) -0.009(3) C97 0.054(4) 0.128(6) 0.075(5) -0.016(4) -0.018(4) 0.004(4) C98 0.043(4) 0.107(5) 0.112(6) -0.020(5) -0.017(4) -0.001(4) C99 0.045(3) 0.054(3) 0.095(5) -0.011(3) 0.002(3) -0.026(3) C100 0.054(4) 0.061(4) 0.068(4) -0.005(3) 0.009(3) -0.016(3) C101 0.051(4) 0.051(3) 0.090(5) -0.023(3) -0.002(3) -0.022(3) C102 0.058(4) 0.057(4) 0.103(5) 0.003(4) -0.026(4) -0.020(3) C103 0.245(15) 0.231(13) 0.121(9) 0.084(9) -0.014(9) 0.081(11) C104 0.31(2) 0.311(19) 0.153(12) 0.103(12) -0.018(12) 0.141(16) N5 0.144(7) 0.130(6) 0.104(6) 0.041(4) -0.023(5) -0.060(5) C105 0.127(9) 0.251(13) 0.100(8) 0.000(8) 0.003(7) 0.017(9) C106 0.102(7) 0.367(17) 0.060(6) -0.023(8) -0.016(5) 0.058(9) C107 0.135(8) 0.359(15) 0.106(7) 0.076(8) -0.048(6) -0.190(10) C108 0.276(11) 0.178(8) 0.068(5) 0.022(5) -0.057(6) -0.195(8) C109 0.180(8) 0.111(5) 0.088(5) 0.009(4) -0.039(5) -0.118(6) C110 0.46(2) 0.274(13) 0.105(8) 0.020(8) -0.051(10) -0.321(15) C111 0.44(2) 0.283(13) 0.102(7) -0.031(8) 0.012(9) -0.314(15) C112 0.122(6) 0.088(5) 0.092(5) -0.014(4) -0.006(4) -0.077(5) C113 0.097(5) 0.080(4) 0.087(5) 0.013(4) -0.025(4) -0.066(4) C114 0.080(4) 0.075(4) 0.102(5) 0.018(4) -0.026(4) -0.056(4) C115 0.119(6) 0.082(4) 0.076(5) -0.028(4) 0.018(4) -0.072(5) C116 0.082(5) 0.073(4) 0.184(8) -0.033(5) -0.012(5) -0.041(4) C117 0.061(4) 0.067(4) 0.180(8) -0.033(5) 0.006(5) -0.025(4) C118 0.076(4) 0.079(4) 0.126(6) -0.047(4) 0.028(4) -0.053(4) C119 0.110(6) 0.124(6) 0.101(6) -0.043(5) 0.037(4) -0.089(5) C120 0.050(4) 0.077(5) 0.278(11) -0.093(6) 0.021(5) -0.020(4) C121 0.043(3) 0.050(3) 0.085(4) -0.013(3) -0.010(3) -0.025(3) C122 0.032(3) 0.061(3) 0.091(4) -0.030(3) 0.005(3) -0.024(3) C123 0.042(3) 0.049(3) 0.102(5) -0.030(3) -0.002(3) -0.015(3) C125 0.032(3) 0.061(4) 0.120(5) -0.026(4) 0.004(3) -0.020(3) C126 0.048(4) 0.076(4) 0.106(5) -0.036(4) 0.000(3) -0.039(3) C127 0.029(3) 0.062(3) 0.094(5) -0.028(3) 0.001(3) -0.024(3) C128 0.042(3) 0.067(4) 0.094(5) -0.028(3) -0.001(3) -0.024(3) C129 0.037(3) 0.056(3) 0.084(4) -0.022(3) -0.011(3) -0.020(3) C130 0.044(3) 0.060(4) 0.144(6) -0.038(4) -0.015(4) -0.022(3) C131 0.063(4) 0.057(4) 0.118(5) -0.028(4) -0.029(4) -0.021(3) C132 0.053(4) 0.043(3) 0.089(4) -0.011(3) -0.014(3) -0.024(3) C133 0.039(3) 0.062(3) 0.073(4) 0.001(3) -0.011(3) -0.024(3) C134 0.033(3) 0.052(3) 0.070(4) -0.005(3) -0.013(3) -0.020(3) C135 0.030(3) 0.045(3) 0.080(4) -0.013(3) 0.001(3) -0.010(2) C136 0.032(3) 0.034(3) 0.081(4) -0.014(3) -0.009(3) 0.002(2) C137 0.038(3) 0.049(3) 0.069(4) -0.008(3) -0.003(3) -0.014(3) C138 0.045(3) 0.056(3) 0.068(4) -0.006(3) 0.004(3) -0.010(3) C139 0.029(3) 0.056(3) 0.074(4) -0.008(3) -0.010(3) -0.006(3) C140 0.040(3) 0.050(3) 0.087(5) -0.025(3) -0.017(3) -0.001(3) C141 0.029(3) 0.043(3) 0.070(4) -0.010(3) -0.003(3) -0.005(2) C142 0.054(4) 0.089(4) 0.112(6) -0.018(4) -0.023(4) -0.025(4) C143 0.040(3) 0.064(4) 0.109(5) -0.030(3) -0.006(3) -0.015(3) C144 0.034(3) 0.059(4) 0.111(5) -0.039(3) 0.000(3) -0.017(3) C145 0.045(4) 0.063(4) 0.141(6) -0.022(4) 0.017(4) -0.028(3) C146 0.065(4) 0.057(4) 0.126(6) -0.022(4) 0.022(4) -0.024(3) C147 0.044(3) 0.050(3) 0.102(5) -0.026(3) 0.018(3) -0.020(3) C148 0.052(4) 0.067(4) 0.090(5) -0.018(3) 0.000(3) -0.032(3) C149 0.042(3) 0.045(3) 0.106(5) -0.020(3) -0.006(3) -0.010(3) C150 0.057(4) 0.045(3) 0.086(5) -0.012(3) -0.001(3) -0.020(3) C151 0.072(5) 0.080(5) 0.096(6) -0.019(4) 0.031(4) -0.006(4) C152 0.100(6) 0.070(4) 0.080(5) 0.007(4) 0.016(4) -0.011(4) C153 0.044(3) 0.055(3) 0.074(4) -0.014(3) 0.005(3) -0.024(3) C154 0.039(3) 0.060(3) 0.076(4) -0.015(3) 0.006(3) -0.017(3) C155 0.069(6) 0.125(7) 0.57(2) -0.200(12) -0.052(9) -0.001(5) C168 0.111(6) 0.227(10) 0.112(6) 0.024(6) -0.015(5) -0.130(7) C181 0.041(3) 0.061(4) 0.107(5) -0.010(3) -0.012(3) -0.024(3) C182 0.039(3) 0.063(4) 0.097(5) -0.020(3) -0.004(3) -0.024(3) C183 0.033(3) 0.060(3) 0.101(5) -0.016(3) -0.003(3) -0.021(3) C184 0.028(3) 0.056(3) 0.101(5) -0.034(3) -0.005(3) -0.010(3) C185 0.029(3) 0.059(4) 0.102(5) -0.012(3) -0.007(3) -0.012(3) C186 0.049(4) 0.073(4) 0.104(5) -0.027(4) 0.010(3) -0.035(3) C187 0.028(3) 0.071(4) 0.109(5) -0.013(4) 0.003(3) -0.023(3) C188 0.034(3) 0.049(3) 0.133(6) -0.022(3) -0.002(3) -0.016(3) C189 0.037(3) 0.068(4) 0.117(6) -0.042(4) 0.007(4) -0.013(3) C190 0.052(4) 0.078(4) 0.141(7) -0.040(5) 0.012(4) -0.030(4) C191 0.065(5) 0.104(5) 0.121(6) -0.026(5) 0.001(4) -0.020(4) C192 0.077(5) 0.102(5) 0.128(7) -0.028(5) 0.029(5) -0.056(4) C193 0.066(4) 0.081(5) 0.131(6) -0.036(5) 0.008(5) -0.030(4) C194 0.034(3) 0.055(3) 0.138(6) -0.044(4) 0.026(4) -0.015(3) C195 0.040(4) 0.073(4) 0.143(7) -0.025(4) -0.004(4) -0.015(3) C196 0.045(4) 0.062(4) 0.121(6) -0.024(4) -0.008(3) -0.022(3) C197 0.057(4) 0.081(4) 0.122(6) -0.020(4) -0.006(4) -0.042(4) C198 0.073(4) 0.059(4) 0.106(5) -0.006(3) -0.027(4) -0.037(4) C199 0.062(4) 0.050(3) 0.104(5) -0.007(3) -0.025(4) -0.012(3) C200 0.039(3) 0.047(3) 0.119(5) -0.015(3) -0.019(3) -0.010(3) C201 0.047(4) 0.061(4) 0.126(6) -0.013(4) -0.020(4) -0.025(3) C202 0.050(4) 0.090(4) 0.077(4) -0.046(4) 0.008(3) -0.035(3) C203 0.036(3) 0.083(4) 0.065(4) -0.037(3) 0.001(3) -0.012(3) C204 0.041(4) 0.128(6) 0.091(5) 0.026(4) -0.007(3) -0.029(4) C205 0.037(4) 0.150(7) 0.100(6) 0.047(5) -0.012(4) -0.010(4) C206 0.037(3) 0.097(5) 0.068(4) -0.021(4) -0.007(3) -0.015(3) C207 0.030(3) 0.093(5) 0.166(7) -0.072(5) 0.008(4) -0.016(3) C208 0.033(3) 0.072(4) 0.145(6) -0.038(4) 0.003(4) -0.022(3) C209 0.032(3) 0.105(5) 0.062(4) -0.015(3) 0.004(3) -0.018(3) C218 0.055(4) 0.110(5) 0.090(5) -0.022(4) -0.006(3) -0.025(4) C219 0.060(4) 0.078(4) 0.112(6) -0.019(4) 0.008(4) -0.018(4) C220 0.065(4) 0.082(5) 0.091(5) -0.015(4) 0.016(4) -0.034(4) C221 0.128(7) 0.098(6) 0.115(7) -0.005(5) -0.002(6) -0.047(5) C222 0.119(7) 0.125(7) 0.130(8) -0.018(6) 0.018(6) -0.020(6) C223 0.099(6) 0.107(6) 0.128(7) -0.019(6) 0.011(5) -0.044(5) C224 0.081(6) 0.120(7) 0.134(7) -0.038(6) 0.018(5) -0.026(5) C225 0.082(5) 0.140(7) 0.086(6) -0.018(5) 0.014(4) -0.042(5) C226 0.105(7) 0.190(10) 0.100(7) -0.002(7) 0.008(6) -0.078(7) C227 0.258(14) 0.201(11) 0.132(9) 0.086(8) -0.037(9) -0.143(11) C228 0.239(16) 0.33(2) 0.178(14) 0.131(14) 0.025(12) -0.157(15) N11 0.165(10) 0.314(16) 0.121(8) -0.020(9) 0.031(7) 0.018(10) C229 0.133(10) 0.196(12) 0.159(11) -0.053(9) 0.036(8) 0.037(9) C230 0.173(10) 0.155(9) 0.108(8) -0.037(7) -0.018(7) -0.041(8) C231 0.114(7) 0.188(9) 0.220(11) -0.062(8) 0.050(7) -0.115(7) C232 0.044(3) 0.069(4) 0.125(6) -0.012(4) -0.005(3) -0.028(3) C233 0.051(4) 0.064(4) 0.094(5) -0.010(3) -0.014(3) -0.031(3) C234 0.061(4) 0.067(4) 0.085(5) 0.008(3) -0.018(3) -0.029(3) C235 0.071(4) 0.069(4) 0.088(5) -0.004(3) -0.024(4) -0.041(3) C236 0.048(3) 0.056(3) 0.089(5) -0.002(3) -0.008(3) -0.025(3) C237 0.073(4) 0.075(4) 0.080(5) 0.000(3) -0.018(3) -0.042(4) C238 0.077(4) 0.083(4) 0.086(5) -0.011(4) -0.020(4) -0.044(4) C239 0.043(3) 0.055(3) 0.084(4) -0.010(3) -0.011(3) -0.019(3) C240 0.071(4) 0.046(3) 0.095(5) -0.019(3) -0.013(4) -0.020(3) C241 0.056(4) 0.068(4) 0.066(4) -0.021(3) 0.003(3) -0.035(3) C242 0.064(4) 0.062(4) 0.097(5) -0.013(3) -0.015(3) -0.026(3) C243 0.066(4) 0.088(4) 0.083(5) -0.001(4) -0.011(3) -0.044(4) C244 0.117(6) 0.069(4) 0.149(7) -0.028(5) -0.017(5) -0.019(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 O21 2.115(4) . ? Zn1 N7 2.176(4) . ? Zn1 O19 2.183(5) . ? Zn1 N10 2.186(5) . ? Zn1 N8 2.195(6) 1_655 ? Zn1 N12 2.255(4) 1_455 ? Zn2 O41 2.127(4) . ? Zn2 N4 2.183(4) . ? Zn2 O43 2.187(5) . ? Zn2 N6 2.186(4) 1_455 ? Zn2 N3 2.187(4) 1_455 ? Zn2 N1 2.205(4) . ? F4 C246 1.470(11) . ? F5 C246 1.272(11) . ? F6 C246 1.195(11) . ? F1A C252 1.344(10) . ? F3A C252 1.257(11) . ? F2A C252 1.443(11) . ? O1 C4 1.373(6) . ? O1 C22 1.405(9) . ? O2 C23 1.354(6) . ? O2 C5 1.446(6) . ? O3 C23 1.225(6) . ? O4 C11 1.370(8) . ? O4 C35 1.442(7) . ? O5 C12 1.382(8) . ? O5 C36 1.383(9) . ? O6 C36 1.242(9) . ? O7 C18 1.390(6) . ? O7 C48 1.427(6) . ? O8 C49 1.380(6) . ? O8 C19 1.401(6) . ? O9 C49 1.219(5) . ? O10 C82 1.350(5) . ? O10 C64 1.426(6) . ? O11 C82 1.227(5) . ? O12 C65 1.387(6) . ? O12 C94 1.414(6) . ? O13 C95 1.323(6) . ? O13 C71 1.449(6) . ? O14 C95 1.230(6) . ? O15 C72 1.384(6) . ? O15 C107 1.436(7) . ? O16 C108 1.303(7) . ? O16 C78 1.437(5) . ? O17 C108 1.257(8) . ? O18 C79 1.382(6) . ? O18 C120 1.430(7) . ? O21 C245 1.227(6) . ? O22 C245 1.264(7) . ? O23 C124 1.395(6) . ? O23 C142 1.415(7) . ? O24 C143 1.388(6) . ? O24 C125 1.426(6) . ? O25 C143 1.197(6) . ? O26 C131 1.402(6) . ? O26 C155 1.425(8) . ? O27 C56B 1.309(16) . ? O27 C156 1.396(12) . ? O27 C132 1.400(5) . ? O28 C156 1.243(11) . ? O29 C138 1.392(6) . ? O29 C168 1.452(7) . ? O30 C169 1.051(13) . ? O30 C69A 1.223(11) . ? O30 C139 1.401(6) . ? O31 C169 1.320(14) . ? O31A C69A 1.265(12) . ? O31A O31A 1.330(16) 2_576 ? O32 C202 1.403(6) . ? O32 C184 1.421(6) . ? O33 C202 1.210(7) . ? O34 C185 1.384(6) . ? O34 C218 1.392(6) . ? O35 C219 1.353(7) . ? O35 C191 1.453(8) . ? O36 C219 1.263(7) . ? O37 C192 1.405(8) . ? O37 C231 1.417(8) . ? O38 C232 1.361(7) . ? O38 C198 1.406(6) . ? O39 C232 1.212(7) . ? O40 C199 1.383(6) . ? O40 C244 1.470(8) . ? O41 C251 1.149(7) . ? O42 C251 1.311(9) . ? O45 C263 1.255(12) . ? O46 C258 1.370(17) . ? C272 N14 1.460(11) . ? C282 N15 1.470(14) . ? O49 C273 1.241(11) . ? C257 N18 1.454(11) . ? N1 C32 1.322(6) . ? N1 C33 1.356(6) . ? N3 C58 1.334(6) . ? N3 C59 1.356(6) . ? N3 Zn2 2.187(4) 1_655 ? N4 C91 1.324(6) . ? N4 C92 1.325(6) . ? N6 C118 1.287(7) . ? N6 C117 1.345(7) . ? N6 Zn2 2.186(4) 1_655 ? N7 C152 1.335(7) . ? N7 C153 1.365(6) . ? N10 C212 1.274(10) . ? N10 C211 1.391(9) . ? N10 C216 1.434(13) . ? N10 C215 1.458(11) . ? N12 C242 1.315(7) . ? N12 C241 1.336(6) . ? N12 Zn1 2.255(4) 1_655 ? N13 C273 1.217(12) . ? N13 C276 1.436(13) . ? N13 C277 1.519(14) . ? C268 O273 1.179(12) . ? C268 N14 1.368(12) . ? C268 C271 1.477(15) . ? C281 O48 1.29(2) . ? C281 N15 1.44(2) . ? C281 C278 1.45(2) . ? N16 C263 1.230(16) . ? N16 C267 1.330(17) . ? N16 C266 1.386(17) . ? N17 C262 1.159(13) . ? N17 C258 1.371(16) . ? N17 C261 1.409(15) . ? C253 N18 1.240(13) . ? C253 O50 1.222(13) . ? C253 C256 1.660(14) . ? C1 C2 1.534(6) . ? C1 C21 1.542(7) . ? C2 C7 1.383(7) . ? C2 C3 1.401(7) . ? C3 C4 1.397(7) . ? C4 C5 1.360(8) . ? C5 C6 1.399(8) . ? C6 C7 1.399(7) . ? C7 C8 1.534(7) . ? C8 C9 1.496(8) . ? C9 C10 1.399(8) . ? C9 C14 1.405(7) . ? C10 C11 1.359(9) . ? C11 C12 1.442(8) . ? C12 C13 1.394(9) . ? C13 C14 1.358(8) . ? C14 C15 1.546(8) . ? C15 C16 1.542(7) . ? C16 C21 1.388(7) . ? C16 C17 1.413(7) . ? C17 C18 1.399(7) . ? C18 C19 1.390(7) . ? C19 C20 1.424(7) . ? C20 C21 1.373(7) . ? C23 C24 1.471(7) . ? C24 C29 1.321(8) . ? C24 C25 1.392(7) . ? C25 C26 1.384(7) . ? C26 C27 1.396(7) . ? C27 C28 1.389(7) . ? C27 C30 1.503(6) . ? C28 C29 1.430(7) . ? C30 C31 1.394(7) . ? C30 C34 1.418(7) . ? C31 C32 1.391(7) . ? C33 C34 1.398(6) . ? C36 C37 1.405(10) . ? C37 C42 1.417(11) . ? C37 C38 1.441(10) . ? C38 C39 1.398(10) . ? C39 C40 1.403(12) . ? C40 C41 1.439(11) . ? C40 C43 1.512(10) . ? C41 C42 1.367(11) . ? C43 C44 1.3900 . ? C43 C47 1.3900 . ? C44 C45 1.3900 . ? C45 N2 1.3900 . ? N2 C46 1.3900 . ? C46 C47 1.3900 . ? C49 C50 1.495(7) . ? C50 C55 1.400(7) . ? C50 C51 1.415(7) . ? C51 C52 1.407(7) . ? C52 C53 1.401(7) . ? C53 C54 1.400(7) . ? C53 C56 1.490(7) . ? C54 C55 1.399(7) . ? C56 C57 1.406(7) . ? C56 C60 1.416(7) . ? C57 C58 1.367(7) . ? C59 C60 1.384(7) . ? C61 C81 1.522(6) . ? C61 C62 1.535(7) . ? C62 C63 1.396(6) . ? C62 C67 1.441(7) . ? C63 C64 1.378(7) . ? C64 C65 1.389(7) . ? C65 C66 1.400(7) . ? C66 C67 1.380(6) . ? C67 C68 1.544(6) . ? C68 C69 1.535(6) . ? C69 C70 1.412(7) . ? C69 C74 1.451(6) . ? C69A C70A 1.409(18) . ? C70A C75A 1.42(2) . ? C70A C71A 1.46(2) . ? C71A C72A 1.390(15) . ? C72A C73A 1.404(19) . ? C73A C74A 1.398(18) . ? C73A C176 1.502(18) . ? C74A C75A 1.375(15) . ? C70 C71 1.392(7) . ? C71 C72 1.400(7) . ? C72 C73 1.381(7) . ? C73 C74 1.429(7) . ? C74 C75 1.486(7) . ? C75 C76 1.543(6) . ? C76 C77 1.396(6) . ? C76 C81 1.418(6) . ? C77 C78 1.400(7) . ? C78 C79 1.393(7) . ? C79 C80 1.392(6) . ? C80 C81 1.397(6) . ? C76A C80A 1.430(17) . ? C76A C77A 1.46(2) . ? C76A C173 1.47(2) . ? C77A C78A 1.38(2) . ? C78A N9A 1.30(2) . ? N9A C79A 1.324(19) . ? C79A C80A 1.50(2) . ? C82 C83 1.474(7) . ? C83 C84 1.406(7) . ? C83 C88 1.409(7) . ? C84 C85 1.402(8) . ? C85 C86 1.385(7) . ? C86 C87 1.401(7) . ? C86 C89 1.500(7) . ? C87 C88 1.381(7) . ? C89 C93 1.387(8) . ? C89 C90 1.396(7) . ? C90 C91 1.382(7) . ? C92 C93 1.407(8) . ? C95 C96 1.464(8) . ? C96 C97 1.353(7) . ? C96 C101 1.374(7) . ? C97 C98 1.404(9) . ? C98 C99 1.391(8) . ? C99 C100 1.381(7) . ? C99 C102 1.530(7) . ? C100 C101 1.415(7) . ? C102 C103 1.3900 . ? C102 C106 1.3900 . ? C103 C104 1.3900 . ? C104 N5 1.3900 . ? N5 C105 1.3900 . ? C105 C106 1.3900 . ? C108 C109 1.491(7) . ? C109 C110 1.3900 . ? C109 C114 1.3900 . ? C110 C111 1.3900 . ? C111 C112 1.3900 . ? C112 C113 1.3900 . ? C112 C115 1.514(6) . ? C113 C114 1.3900 . ? C115 C119 1.345(8) . ? C115 C116 1.403(9) . ? C116 C117 1.383(8) . ? C118 C119 1.380(7) . ? C121 C141 1.531(7) . ? C121 C122 1.559(7) . ? C122 C127 1.382(7) . ? C122 C123 1.421(7) . ? C123 C124 1.400(7) . ? C124 C125 1.414(7) . ? C125 C126 1.360(8) . ? C126 C127 1.412(7) . ? C127 C128 1.540(7) . ? C128 C129 1.545(7) . ? C129 C134 1.383(7) . ? C129 C130 1.430(7) . ? C130 C131 1.389(7) . ? C131 C132 1.394(7) . ? C132 C133 1.357(7) . ? C133 C134 1.425(6) . ? C134 C135 1.521(6) . ? C135 C136 1.545(7) . ? C136 C137 1.394(7) . ? C136 C141 1.395(6) . ? C137 C138 1.397(7) . ? C138 C139 1.390(7) . ? C139 C140 1.365(7) . ? C140 C141 1.410(7) . ? C143 C144 1.522(7) . ? C144 C149 1.387(7) . ? C144 C145 1.401(8) . ? C145 C146 1.390(8) . ? C146 C147 1.398(7) . ? C147 C148 1.402(7) . ? C147 C150 1.477(7) . ? C148 C149 1.397(7) . ? C150 C151 1.392(8) . ? C150 C154 1.399(7) . ? C151 C152 1.383(8) . ? C153 C154 1.367(7) . ? C157 C158 1.431(11) . ? C157 C162 1.450(15) . ? C157 C156 1.472(13) . ? C158 C57B 1.342(13) . ? C158 C159 1.393(7) . ? C159 C60B 1.367(15) . ? C159 C160 1.383(11) . ? C160 C161 1.461(14) . ? C160 C163 1.495(13) . ? C161 C162 1.386(15) . ? C163 C64C 1.337(15) . ? C163 C67C 1.376(17) . ? N8 C66B 1.152(11) . ? N8 C65C 1.200(11) . ? N8 C66C 1.518(16) . ? N8 C65B 1.547(15) . ? N8 Zn1 2.195(6) 1_455 ? C169 C170 1.457(17) . ? C170 C175 1.30(2) . ? C170 C171 1.355(17) . ? C171 C172 1.416(17) . ? C172 C173 1.38(2) . ? C173 C174 1.44(2) . ? C174 C175 1.388(18) . ? C176 C177 1.314(16) . ? C176 C180 1.433(18) . ? C177 C178 1.434(19) . ? C178 N9 1.368(19) . ? N9 C179 1.276(18) . ? C179 C180 1.47(2) . ? C181 C182 1.498(7) . ? C181 C201 1.546(7) . ? C182 C187 1.384(8) . ? C182 C183 1.419(7) . ? C183 C184 1.404(7) . ? C184 C185 1.360(7) . ? C185 C186 1.423(7) . ? C186 C187 1.423(8) . ? C187 C188 1.556(7) . ? C188 C189 1.545(8) . ? C189 C190 1.344(9) . ? C189 C194 1.402(8) . ? C190 C191 1.418(9) . ? C191 C192 1.366(9) . ? C192 C193 1.370(9) . ? C193 C194 1.433(8) . ? C194 C195 1.513(9) . ? C195 C196 1.563(8) . ? C196 C197 1.409(7) . ? C196 C201 1.412(8) . ? C197 C198 1.372(8) . ? C198 C199 1.405(8) . ? C199 C200 1.381(7) . ? C200 C201 1.382(7) . ? C202 C203 1.487(8) . ? C203 C208 1.372(7) . ? C203 C204 1.381(8) . ? C204 C205 1.399(8) . ? C205 C206 1.363(8) . ? C206 C207 1.409(8) . ? C206 C209 1.502(8) . ? C207 C208 1.382(8) . ? C209 C217 1.281(13) . ? C209 C213 1.318(10) . ? C209 C214 1.392(12) . ? C209 C210 1.623(10) . ? C210 C211 1.348(12) . ? C212 C213 1.380(13) . ? C214 C215 1.465(15) . ? C216 C217 1.362(16) . ? C219 C220 1.398(9) . ? C220 C221 1.356(9) . ? C220 C225 1.440(9) . ? C221 C222 1.397(10) . ? C222 C223 1.441(11) . ? C223 C224 1.446(10) . ? C223 C226 1.500(11) . ? C224 C225 1.375(10) . ? C226 C230 1.357(11) . ? C226 C227 1.397(12) . ? C227 C228 1.312(15) . ? C228 N11 1.430(19) . ? N11 C229 1.319(15) . ? C229 C230 1.417(13) . ? C232 C233 1.490(7) . ? C233 C238 1.372(8) . ? C233 C234 1.407(7) . ? C234 C235 1.403(7) . ? C235 C236 1.435(8) . ? C236 C237 1.386(7) . ? C236 C239 1.479(7) . ? C237 C238 1.407(7) . ? C239 C243 1.392(7) . ? C239 C240 1.408(8) . ? C240 C241 1.370(7) . ? C242 C243 1.415(7) . ? C245 C246 1.647(11) . ? C251 C252 1.551(10) . ? C252 F3 1.296(11) . ? C252 F2 1.325(13) . ? C252 F1 1.513(12) . ? N18 C254 1.467(11) . ? C254 C255 1.582(13) . ? C255 C256 1.447(12) . ? C258 C259 1.596(16) . ? C259 C260 1.346(17) . ? C260 C261 1.470(17) . ? C263 C264 1.783(18) . ? C264 C265 1.49(2) . ? C265 C266 1.64(2) . ? N14 C269 1.398(13) . ? C269 C270 1.491(16) . ? C270 C271 1.581(16) . ? C273 C274 1.622(16) . ? C274 C275 1.461(17) . ? C275 C276 1.513(16) . ? C278 C279 1.509(15) . ? C279 C280 1.324(15) . ? C280 N15 1.467(14) . ? O28B C56B 1.202(17) . ? C60B C59B 1.42(2) . ? C60B C63B 1.443(17) . ? C57B C58B 1.372(19) . ? C57B C56B 1.497(18) . ? C59B C58B 1.47(2) . ? C67B C63B 1.400(18) . ? C67B C66B 1.452(15) . ? C63B C64B 1.328(19) . ? C64B C65B 1.409(17) . ? C64C C65C 1.424(15) . ? C67C C66C 1.470(19) . ? C304 C303 1.261(16) . ? C304 C300 1.430(18) . ? C303 C302 1.59(2) . ? C300 N301 1.106(19) . ? C300 O306 1.304(17) . ? N301 C302 1.35(2) . ? N301 C305 1.525(16) . ? 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 O21 Zn1 N7 90.30(16) . . ? O21 Zn1 O19 175.17(15) . . ? N7 Zn1 O19 88.15(16) . . ? O21 Zn1 N10 90.48(16) . . ? N7 Zn1 N10 174.88(16) . . ? O19 Zn1 N10 90.66(16) . . ? O21 Zn1 N8 96.70(17) . 1_655 ? N7 Zn1 N8 90.67(18) . 1_655 ? O19 Zn1 N8 87.89(18) . 1_655 ? N10 Zn1 N8 94.26(19) . 1_655 ? O21 Zn1 N12 87.84(15) . 1_455 ? N7 Zn1 N12 86.68(15) . 1_455 ? O19 Zn1 N12 87.51(17) . 1_455 ? N10 Zn1 N12 88.30(15) . 1_455 ? N8 Zn1 N12 174.76(19) 1_655 1_455 ? O41 Zn2 N4 89.02(15) . . ? O41 Zn2 O43 173.79(13) . . ? N4 Zn2 O43 90.49(16) . . ? O41 Zn2 N6 98.16(17) . 1_455 ? N4 Zn2 N6 90.54(16) . 1_455 ? O43 Zn2 N6 88.03(16) . 1_455 ? O41 Zn2 N3 88.47(17) . 1_455 ? N4 Zn2 N3 175.39(14) . 1_455 ? O43 Zn2 N3 91.59(17) . 1_455 ? N6 Zn2 N3 93.63(16) 1_455 1_455 ? O41 Zn2 N1 88.16(16) . . ? N4 Zn2 N1 90.28(14) . . ? O43 Zn2 N1 85.65(15) . . ? N6 Zn2 N1 173.63(18) 1_455 . ? N3 Zn2 N1 85.79(15) 1_455 . ? C4 O1 C22 116.5(5) . . ? C23 O2 C5 116.2(5) . . ? C11 O4 C35 116.4(6) . . ? C12 O5 C36 117.9(6) . . ? C18 O7 C48 116.3(4) . . ? C49 O8 C19 116.3(4) . . ? C82 O10 C64 118.6(3) . . ? C65 O12 C94 116.4(4) . . ? C95 O13 C71 119.0(4) . . ? C72 O15 C107 115.2(5) . . ? C108 O16 C78 122.7(4) . . ? C79 O18 C120 115.7(4) . . ? C245 O21 Zn1 139.5(4) . . ? C124 O23 C142 116.5(4) . . ? C143 O24 C125 113.9(4) . . ? C131 O26 C155 117.8(5) . . ? C56B O27 C156 44.7(7) . . ? C56B O27 C132 122.4(8) . . ? C156 O27 C132 112.3(6) . . ? C138 O29 C168 116.1(5) . . ? C169 O30 C69A 91.1(10) . . ? C169 O30 C139 132.1(9) . . ? C69A O30 C139 132.0(7) . . ? C69A O31A O31A 164.8(13) . 2_576 ? C202 O32 C184 116.9(4) . . ? C185 O34 C218 118.7(5) . . ? C219 O35 C191 120.7(6) . . ? C192 O37 C231 116.6(6) . . ? C232 O38 C198 117.3(5) . . ? C199 O40 C244 114.3(5) . . ? C251 O41 Zn2 142.8(4) . . ? C32 N1 C33 115.9(4) . . ? C32 N1 Zn2 120.0(3) . . ? C33 N1 Zn2 124.0(4) . . ? C58 N3 C59 117.2(5) . . ? C58 N3 Zn2 121.2(3) . 1_655 ? C59 N3 Zn2 121.6(3) . 1_655 ? C91 N4 C92 117.8(5) . . ? C91 N4 Zn2 121.6(3) . . ? C92 N4 Zn2 120.5(4) . . ? C118 N6 C117 116.2(5) . . ? C118 N6 Zn2 125.0(4) . 1_655 ? C117 N6 Zn2 118.8(4) . 1_655 ? C152 N7 C153 115.1(5) . . ? C152 N7 Zn1 120.8(4) . . ? C153 N7 Zn1 124.1(3) . . ? C212 N10 C211 123.0(7) . . ? C212 N10 C216 49.9(6) . . ? C211 N10 C216 92.1(7) . . ? C212 N10 C215 82.2(7) . . ? C211 N10 C215 72.6(6) . . ? C216 N10 C215 109.6(8) . . ? C212 N10 Zn1 122.4(5) . . ? C211 N10 Zn1 114.2(4) . . ? C216 N10 Zn1 125.8(6) . . ? C215 N10 Zn1 122.9(5) . . ? C242 N12 C241 117.1(5) . . ? C242 N12 Zn1 119.7(4) . 1_655 ? C241 N12 Zn1 123.0(4) . 1_655 ? C273 N13 C276 124.4(10) . . ? C273 N13 C277 117.0(9) . . ? C276 N13 C277 118.1(9) . . ? O273 C268 N14 123.1(10) . . ? O273 C268 C271 131.4(11) . . ? N14 C268 C271 105.5(9) . . ? O48 C281 N15 113.3(16) . . ? O48 C281 C278 132.2(17) . . ? N15 C281 C278 113.0(15) . . ? C263 N16 C267 121.4(16) . . ? C263 N16 C266 122.7(16) . . ? C267 N16 C266 115.6(14) . . ? C262 N17 C258 116.7(13) . . ? C262 N17 C261 136.8(14) . . ? C258 N17 C261 104.8(12) . . ? N18 C253 O50 130.7(13) . . ? N18 C253 C256 106.2(11) . . ? O50 C253 C256 123.1(11) . . ? C2 C1 C21 112.0(4) . . ? C7 C2 C3 119.0(5) . . ? C7 C2 C1 123.1(5) . . ? C3 C2 C1 117.8(5) . . ? C4 C3 C2 122.8(6) . . ? C5 C4 O1 117.3(5) . . ? C5 C4 C3 116.9(5) . . ? O1 C4 C3 125.8(6) . . ? C4 C5 C6 122.2(5) . . ? C4 C5 O2 119.3(6) . . ? C6 C5 O2 118.4(6) . . ? C5 C6 C7 120.2(6) . . ? C2 C7 C6 118.8(5) . . ? C2 C7 C8 124.1(4) . . ? C6 C7 C8 116.9(5) . . ? C9 C8 C7 113.9(5) . . ? C10 C9 C14 119.9(6) . . ? C10 C9 C8 117.0(5) . . ? C14 C9 C8 122.8(6) . . ? C11 C10 C9 121.4(6) . . ? C10 C11 O4 127.0(6) . . ? C10 C11 C12 119.1(7) . . ? O4 C11 C12 113.9(7) . . ? O5 C12 C13 122.6(6) . . ? O5 C12 C11 119.2(7) . . ? C13 C12 C11 117.9(7) . . ? C14 C13 C12 122.8(5) . . ? C13 C14 C9 118.7(6) . . ? C13 C14 C15 118.1(5) . . ? C9 C14 C15 123.0(6) . . ? C16 C15 C14 113.7(5) . . ? C21 C16 C17 119.2(5) . . ? C21 C16 C15 123.4(5) . . ? C17 C16 C15 117.4(5) . . ? C18 C17 C16 121.4(5) . . ? C19 C18 O7 114.1(5) . . ? C19 C18 C17 118.8(5) . . ? O7 C18 C17 127.1(5) . . ? C18 C19 O8 120.1(5) . . ? C18 C19 C20 119.4(5) . . ? O8 C19 C20 120.5(5) . . ? C21 C20 C19 121.3(5) . . ? C20 C21 C16 119.9(4) . . ? C20 C21 C1 117.2(5) . . ? C16 C21 C1 122.9(4) . . ? O3 C23 O2 123.2(5) . . ? O3 C23 C24 124.9(5) . . ? O2 C23 C24 112.0(5) . . ? C29 C24 C25 116.6(5) . . ? C29 C24 C23 124.3(5) . . ? C25 C24 C23 118.9(5) . . ? C26 C25 C24 122.6(6) . . ? C25 C26 C27 119.6(5) . . ? C28 C27 C26 119.2(5) . . ? C28 C27 C30 121.0(5) . . ? C26 C27 C30 119.8(5) . . ? C27 C28 C29 117.4(6) . . ? C24 C29 C28 124.5(6) . . ? C31 C30 C34 117.2(4) . . ? C31 C30 C27 120.6(5) . . ? C34 C30 C27 122.1(4) . . ? C32 C31 C30 118.1(5) . . ? N1 C32 C31 126.4(5) . . ? N1 C33 C34 123.1(5) . . ? C33 C34 C30 119.4(5) . . ? O6 C36 O5 120.9(7) . . ? O6 C36 C37 126.4(8) . . ? O5 C36 C37 112.3(8) . . ? C36 C37 C42 121.8(8) . . ? C36 C37 C38 125.6(9) . . ? C42 C37 C38 112.5(8) . . ? C39 C38 C37 125.4(9) . . ? C38 C39 C40 119.7(9) . . ? C39 C40 C41 116.1(9) . . ? C39 C40 C43 118.9(8) . . ? C41 C40 C43 124.9(10) . . ? C42 C41 C40 122.9(10) . . ? C41 C42 C37 123.4(8) . . ? C44 C43 C47 120.0 . . ? C44 C43 C40 118.0(6) . . ? C47 C43 C40 122.0(6) . . ? C45 C44 C43 120.0 . . ? C44 C45 N2 120.0 . . ? C46 N2 C45 120.0 . . ? N2 C46 C47 120.0 . . ? C46 C47 C43 120.0 . . ? O9 C49 O8 123.2(5) . . ? O9 C49 C50 126.6(4) . . ? O8 C49 C50 110.2(4) . . ? C55 C50 C51 119.7(5) . . ? C55 C50 C49 122.7(4) . . ? C51 C50 C49 117.5(4) . . ? C52 C51 C50 119.7(5) . . ? C53 C52 C51 120.2(4) . . ? C54 C53 C52 119.7(5) . . ? C54 C53 C56 119.0(5) . . ? C52 C53 C56 121.3(4) . . ? C53 C54 C55 120.5(5) . . ? C50 C55 C54 120.1(5) . . ? C57 C56 C60 116.6(5) . . ? C57 C56 C53 121.6(4) . . ? C60 C56 C53 121.8(5) . . ? C58 C57 C56 119.6(5) . . ? N3 C58 C57 124.4(5) . . ? N3 C59 C60 122.8(5) . . ? C59 C60 C56 119.5(5) . . ? C81 C61 C62 113.3(4) . . ? C63 C62 C67 116.9(4) . . ? C63 C62 C61 120.3(4) . . ? C67 C62 C61 122.7(4) . . ? C64 C63 C62 121.8(5) . . ? C63 C64 C65 121.3(5) . . ? C63 C64 O10 119.6(5) . . ? C65 C64 O10 119.0(5) . . ? O12 C65 C64 116.9(5) . . ? O12 C65 C66 124.8(5) . . ? C64 C65 C66 118.3(5) . . ? C67 C66 C65 121.4(5) . . ? C66 C67 C62 120.3(4) . . ? C66 C67 C68 118.3(4) . . ? C62 C67 C68 121.5(4) . . ? C69 C68 C67 110.1(4) . . ? C70 C69 C74 118.4(4) . . ? C70 C69 C68 119.4(4) . . ? C74 C69 C68 122.2(5) . . ? O30 C69A O31A 116.2(11) . . ? O30 C69A C70A 124.3(12) . . ? O31A C69A C70A 119.5(13) . . ? C69A C70A C75A 125.3(17) . . ? C69A C70A C71A 121.0(13) . . ? C75A C70A C71A 113.7(14) . . ? C72A C71A C70A 120.1(11) . . ? C71A C72A C73A 125.9(12) . . ? C74A C73A C72A 112.4(12) . . ? C74A C73A C176 125.0(13) . . ? C72A C73A C176 122.6(12) . . ? C75A C74A C73A 125.1(12) . . ? C74A C75A C70A 122.7(14) . . ? C71 C70 C69 121.0(4) . . ? C70 C71 C72 121.0(5) . . ? C70 C71 O13 121.4(4) . . ? C72 C71 O13 117.6(5) . . ? O15 C72 C73 124.7(4) . . ? O15 C72 C71 115.9(5) . . ? C73 C72 C71 119.4(5) . . ? C72 C73 C74 121.7(5) . . ? C73 C74 C69 118.1(5) . . ? C73 C74 C75 118.4(4) . . ? C69 C74 C75 123.5(5) . . ? C74 C75 C76 111.4(4) . . ? C77 C76 C81 119.2(4) . . ? C77 C76 C75 117.5(4) . . ? C81 C76 C75 123.0(4) . . ? C76 C77 C78 120.0(5) . . ? C79 C78 C77 121.6(4) . . ? C79 C78 O16 118.4(4) . . ? C77 C78 O16 119.9(4) . . ? O18 C79 C80 125.6(4) . . ? O18 C79 C78 116.6(4) . . ? C80 C79 C78 117.7(4) . . ? C79 C80 C81 122.3(5) . . ? C80A C76A C77A 119.2(15) . . ? C80A C76A C173 118.1(13) . . ? C77A C76A C173 122.7(14) . . ? C78A C77A C76A 113.3(17) . . ? N9A C78A C77A 131(2) . . ? C78A N9A C79A 117.1(17) . . ? N9A C79A C80A 121.4(16) . . ? C76A C80A C79A 116.9(14) . . ? C80 C81 C76 119.0(4) . . ? C80 C81 C61 118.6(4) . . ? C76 C81 C61 122.5(4) . . ? O11 C82 O10 122.7(4) . . ? O11 C82 C83 124.9(4) . . ? O10 C82 C83 112.4(4) . . ? C84 C83 C88 118.4(5) . . ? C84 C83 C82 121.9(5) . . ? C88 C83 C82 119.7(4) . . ? C85 C84 C83 121.3(5) . . ? C86 C85 C84 119.6(5) . . ? C85 C86 C87 118.9(5) . . ? C85 C86 C89 120.2(5) . . ? C87 C86 C89 120.9(5) . . ? C88 C87 C86 122.2(5) . . ? C87 C88 C83 119.4(5) . . ? C93 C89 C90 116.1(5) . . ? C93 C89 C86 120.8(5) . . ? C90 C89 C86 123.1(5) . . ? C91 C90 C89 119.9(5) . . ? N4 C91 C90 123.6(5) . . ? N4 C92 C93 122.3(6) . . ? C89 C93 C92 120.1(6) . . ? O14 C95 O13 119.5(6) . . ? O14 C95 C96 124.6(5) . . ? O13 C95 C96 115.7(5) . . ? C97 C96 C101 119.0(6) . . ? C97 C96 C95 119.3(5) . . ? C101 C96 C95 121.7(5) . . ? C96 C97 C98 122.0(6) . . ? C99 C98 C97 119.6(6) . . ? C100 C99 C98 118.7(6) . . ? C100 C99 C102 120.9(5) . . ? C98 C99 C102 120.3(5) . . ? C99 C100 C101 120.3(5) . . ? C96 C101 C100 120.5(5) . . ? C103 C102 C106 120.0 . . ? C103 C102 C99 119.0(4) . . ? C106 C102 C99 121.0(4) . . ? C104 C103 C102 120.0 . . ? C103 C104 N5 120.0 . . ? C104 N5 C105 120.0 . . ? C106 C105 N5 120.0 . . ? C105 C106 C102 120.0 . . ? O17 C108 O16 119.7(6) . . ? O17 C108 C109 118.9(7) . . ? O16 C108 C109 116.9(5) . . ? C110 C109 C114 120.0 . . ? C110 C109 C108 121.0(4) . . ? C114 C109 C108 118.4(4) . . ? C111 C110 C109 120.0 . . ? C110 C111 C112 120.0 . . ? C113 C112 C111 120.0 . . ? C113 C112 C115 118.9(4) . . ? C111 C112 C115 121.0(4) . . ? C114 C113 C112 120.0 . . ? C113 C114 C109 120.0 . . ? C119 C115 C116 114.0(5) . . ? C119 C115 C112 125.6(6) . . ? C116 C115 C112 120.3(5) . . ? C117 C116 C115 118.8(6) . . ? N6 C117 C116 124.2(6) . . ? N6 C118 C119 122.3(6) . . ? C115 C119 C118 123.9(6) . . ? C141 C121 C122 111.5(4) . . ? C127 C122 C123 120.0(5) . . ? C127 C122 C121 124.2(5) . . ? C123 C122 C121 115.8(4) . . ? C124 C123 C122 120.8(5) . . ? O23 C124 C123 125.1(5) . . ? O23 C124 C125 117.7(5) . . ? C123 C124 C125 117.2(5) . . ? C126 C125 C124 122.1(5) . . ? C126 C125 O24 120.3(5) . . ? C124 C125 O24 117.2(5) . . ? C125 C126 C127 120.5(5) . . ? C122 C127 C126 119.1(5) . . ? C122 C127 C128 123.3(5) . . ? C126 C127 C128 117.5(5) . . ? C127 C128 C129 113.2(5) . . ? C134 C129 C130 120.2(4) . . ? C134 C129 C128 124.2(4) . . ? C130 C129 C128 115.5(5) . . ? C131 C130 C129 120.5(5) . . ? C130 C131 C132 119.0(5) . . ? C130 C131 O26 123.1(6) . . ? C132 C131 O26 117.8(5) . . ? C133 C132 C131 120.3(5) . . ? C133 C132 O27 121.6(5) . . ? C131 C132 O27 117.8(4) . . ? C132 C133 C134 122.8(5) . . ? C129 C134 C133 117.0(4) . . ? C129 C134 C135 123.9(4) . . ? C133 C134 C135 119.1(4) . . ? C134 C135 C136 112.3(4) . . ? C137 C136 C141 120.4(5) . . ? C137 C136 C135 116.5(4) . . ? C141 C136 C135 123.1(5) . . ? C136 C137 C138 121.0(5) . . ? C139 C138 O29 117.1(5) . . ? C139 C138 C137 118.3(5) . . ? O29 C138 C137 124.6(5) . . ? C140 C139 C138 120.9(5) . . ? C140 C139 O30 119.3(5) . . ? C138 C139 O30 119.7(5) . . ? C139 C140 C141 121.8(5) . . ? C136 C141 C140 117.6(5) . . ? C136 C141 C121 123.2(5) . . ? C140 C141 C121 119.2(4) . . ? O25 C143 O24 124.5(5) . . ? O25 C143 C144 125.5(5) . . ? O24 C143 C144 109.9(5) . . ? C149 C144 C145 119.9(5) . . ? C149 C144 C143 117.9(5) . . ? C145 C144 C143 122.1(5) . . ? C146 C145 C144 119.6(5) . . ? C145 C146 C147 121.1(6) . . ? C146 C147 C148 118.8(5) . . ? C146 C147 C150 120.3(5) . . ? C148 C147 C150 120.9(5) . . ? C149 C148 C147 120.3(5) . . ? C144 C149 C148 120.3(5) . . ? C151 C150 C154 116.1(5) . . ? C151 C150 C147 119.9(5) . . ? C154 C150 C147 124.0(5) . . ? C152 C151 C150 120.0(6) . . ? N7 C152 C151 124.5(6) . . ? N7 C153 C154 124.1(5) . . ? C153 C154 C150 120.2(6) . . ? C158 C157 C162 118.8(9) . . ? C158 C157 C156 122.8(8) . . ? C162 C157 C156 118.2(10) . . ? C57B C158 C159 120.7(8) . . ? C57B C158 C157 46.8(6) . . ? C159 C158 C157 120.0(6) . . ? C60B C159 C160 44.9(6) . . ? C60B C159 C158 123.8(8) . . ? C160 C159 C158 121.2(6) . . ? C159 C160 C161 120.1(9) . . ? C159 C160 C163 120.7(8) . . ? C161 C160 C163 119.2(9) . . ? C162 C161 C160 119.1(11) . . ? C161 C162 C157 120.0(12) . . ? C64C C163 C67C 120.6(12) . . ? C64C C163 C160 121.2(10) . . ? C67C C163 C160 118.1(11) . . ? C66B N8 C65C 75.5(9) . . ? C66B N8 C66C 53.9(8) . . ? C65C N8 C66C 112.3(10) . . ? C66B N8 C65B 113.7(9) . . ? C65C N8 C65B 44.4(7) . . ? C66C N8 C65B 118.7(9) . . ? C66B N8 Zn1 133.5(7) . 1_455 ? C65C N8 Zn1 131.3(7) . 1_455 ? C66C N8 Zn1 116.2(7) . 1_455 ? C65B N8 Zn1 109.6(6) . 1_455 ? O30 C169 O31 117.7(13) . . ? O30 C169 C170 122.0(13) . . ? O31 C169 C170 119.7(13) . . ? C175 C170 C171 116.1(12) . . ? C175 C170 C169 120.6(14) . . ? C171 C170 C169 123.3(13) . . ? C170 C171 C172 122.8(13) . . ? C173 C172 C171 119.9(13) . . ? C172 C173 C174 117.0(14) . . ? C172 C173 C76A 117.8(13) . . ? C174 C173 C76A 125.2(15) . . ? C175 C174 C173 117.1(16) . . ? C170 C175 C174 127.0(16) . . ? C177 C176 C180 120.0(13) . . ? C177 C176 C73A 122.9(12) . . ? C180 C176 C73A 117.0(12) . . ? C176 C177 C178 126.3(14) . . ? N9 C178 C177 112.7(15) . . ? C179 N9 C178 124.2(17) . . ? N9 C179 C180 124.5(18) . . ? C176 C180 C179 112.0(13) . . ? C182 C181 C201 111.7(5) . . ? C187 C182 C183 118.0(5) . . ? C187 C182 C181 123.3(5) . . ? C183 C182 C181 118.7(5) . . ? C184 C183 C182 120.0(5) . . ? C185 C184 C183 122.4(5) . . ? C185 C184 O32 118.4(5) . . ? C183 C184 O32 119.1(5) . . ? C184 C185 O34 117.2(5) . . ? C184 C185 C186 118.8(5) . . ? O34 C185 C186 124.1(5) . . ? C185 C186 C187 119.2(6) . . ? C182 C187 C186 121.6(5) . . ? C182 C187 C188 121.7(5) . . ? C186 C187 C188 116.6(5) . . ? C189 C188 C187 113.2(4) . . ? C190 C189 C194 118.5(6) . . ? C190 C189 C188 117.8(5) . . ? C194 C189 C188 123.7(6) . . ? C189 C190 C191 120.8(6) . . ? C192 C191 C190 121.4(8) . . ? C192 C191 O35 120.8(7) . . ? C190 C191 O35 117.7(6) . . ? C191 C192 C193 119.1(7) . . ? C191 C192 O37 116.4(8) . . ? C193 C192 O37 124.4(7) . . ? C192 C193 C194 119.4(6) . . ? C189 C194 C193 120.6(7) . . ? C189 C194 C195 124.0(6) . . ? C193 C194 C195 115.3(6) . . ? C194 C195 C196 108.4(5) . . ? C197 C196 C201 119.1(5) . . ? C197 C196 C195 117.7(5) . . ? C201 C196 C195 123.2(5) . . ? C198 C197 C196 120.3(6) . . ? C197 C198 C199 121.3(5) . . ? C197 C198 O38 118.7(6) . . ? C199 C198 O38 119.9(5) . . ? C200 C199 O40 127.8(6) . . ? C200 C199 C198 117.7(5) . . ? O40 C199 C198 114.5(5) . . ? C201 C200 C199 123.0(5) . . ? C200 C201 C196 118.7(5) . . ? C200 C201 C181 119.6(5) . . ? C196 C201 C181 121.7(5) . . ? O33 C202 O32 121.7(5) . . ? O33 C202 C203 127.1(5) . . ? O32 C202 C203 111.2(5) . . ? C208 C203 C204 117.6(6) . . ? C208 C203 C202 120.2(6) . . ? C204 C203 C202 122.1(5) . . ? C203 C204 C205 121.9(6) . . ? C206 C205 C204 119.7(7) . . ? C205 C206 C207 119.2(6) . . ? C205 C206 C209 120.3(6) . . ? C207 C206 C209 120.2(5) . . ? C208 C207 C206 119.6(5) . . ? C203 C208 C207 122.0(6) . . ? C217 C209 C213 50.3(6) . . ? C217 C209 C214 123.2(9) . . ? C213 C209 C214 82.6(7) . . ? C217 C209 C206 118.8(8) . . ? C213 C209 C206 129.4(7) . . ? C214 C209 C206 115.3(7) . . ? C217 C209 C210 91.9(8) . . ? C213 C209 C210 110.9(7) . . ? C214 C209 C210 75.7(6) . . ? C206 C209 C210 119.2(5) . . ? C211 C210 C209 117.8(7) . . ? C210 C211 N10 120.2(8) . . ? N10 C212 C213 120.1(9) . . ? C209 C213 C212 127.2(9) . . ? C209 C214 C215 113.1(10) . . ? N10 C215 C214 123.4(10) . . ? C217 C216 N10 124.7(12) . . ? C209 C217 C216 119.8(12) . . ? O36 C219 O35 119.5(7) . . ? O36 C219 C220 126.5(7) . . ? O35 C219 C220 114.0(7) . . ? C221 C220 C219 119.9(7) . . ? C221 C220 C225 121.3(8) . . ? C219 C220 C225 118.7(7) . . ? C220 C221 C222 119.4(8) . . ? C221 C222 C223 123.9(9) . . ? C222 C223 C224 113.1(8) . . ? C222 C223 C226 122.1(9) . . ? C224 C223 C226 124.8(8) . . ? C225 C224 C223 124.2(8) . . ? C224 C225 C220 118.0(8) . . ? C230 C226 C227 115.8(10) . . ? C230 C226 C223 122.0(10) . . ? C227 C226 C223 121.9(10) . . ? C228 C227 C226 121.5(14) . . ? C227 C228 N11 120.5(14) . . ? C229 N11 C228 121.0(12) . . ? N11 C229 C230 116.1(12) . . ? C226 C230 C229 124.7(11) . . ? O39 C232 O38 121.9(5) . . ? O39 C232 C233 126.5(6) . . ? O38 C232 C233 111.3(6) . . ? C238 C233 C234 119.6(5) . . ? C238 C233 C232 123.2(5) . . ? C234 C233 C232 117.1(6) . . ? C235 C234 C233 119.7(5) . . ? C234 C235 C236 120.3(5) . . ? C237 C236 C235 118.5(5) . . ? C237 C236 C239 122.0(5) . . ? C235 C236 C239 119.5(5) . . ? C236 C237 C238 120.3(6) . . ? C233 C238 C237 121.5(5) . . ? C243 C239 C240 115.1(5) . . ? C243 C239 C236 122.1(6) . . ? C240 C239 C236 122.8(5) . . ? C241 C240 C239 121.5(5) . . ? N12 C241 C240 123.0(6) . . ? N12 C242 C243 123.9(6) . . ? C239 C243 C242 119.3(6) . . ? O21 C245 O22 130.4(6) . . ? O21 C245 C246 115.0(6) . . ? O22 C245 C246 114.3(7) . . ? F6 C246 F5 128.9(11) . . ? F6 C246 F4 101.6(9) . . ? F5 C246 F4 94.3(9) . . ? F6 C246 C245 113.2(10) . . ? F5 C246 C245 112.0(9) . . ? F4 C246 C245 98.2(7) . . ? O41 C251 O42 131.4(7) . . ? O41 C251 C252 123.4(6) . . ? O42 C251 C252 105.2(7) . . ? F3A C252 F3 35.0(5) . . ? F3A C252 F2 121.0(9) . . ? F3 C252 F2 103.6(10) . . ? F3A C252 F1A 125.5(8) . . ? F3 C252 F1A 140.6(8) . . ? F2 C252 F1A 51.1(7) . . ? F3A C252 F2A 110.7(8) . . ? F3 C252 F2A 76.3(7) . . ? F2 C252 F2A 52.1(7) . . ? F1A C252 F2A 99.5(7) . . ? F3A C252 F1 72.2(7) . . ? F3 C252 F1 103.9(8) . . ? F2 C252 F1 96.0(9) . . ? F1A C252 F1 58.1(6) . . ? F2A C252 F1 145.6(8) . . ? F3A C252 C251 110.0(8) . . ? F3 C252 C251 115.3(8) . . ? F2 C252 C251 128.7(9) . . ? F1A C252 C251 103.7(7) . . ? F2A C252 C251 105.5(7) . . ? F1 C252 C251 105.3(7) . . ? C253 N18 C257 120.4(10) . . ? C253 N18 C254 122.3(10) . . ? C257 N18 C254 113.5(9) . . ? N18 C254 C255 95.1(8) . . ? C256 C255 C254 113.3(9) . . ? C255 C256 C253 99.3(9) . . ? N17 C258 O46 131.2(13) . . ? N17 C258 C259 113.7(11) . . ? O46 C258 C259 114.0(12) . . ? C260 C259 C258 94.8(11) . . ? C259 C260 C261 116.1(13) . . ? N17 C261 C260 106.2(12) . . ? N16 C263 O45 141.6(14) . . ? N16 C263 C264 104.8(12) . . ? O45 C263 C264 113.5(10) . . ? C265 C264 C263 99.8(13) . . ? C264 C265 C266 106.3(17) . . ? N16 C266 C265 103.9(13) . . ? C268 N14 C269 115.1(8) . . ? C268 N14 C272 122.0(8) . . ? C269 N14 C272 122.9(8) . . ? N14 C269 C270 107.0(10) . . ? C269 C270 C271 100.6(10) . . ? C268 C271 C270 105.4(10) . . ? N13 C273 O49 133.7(10) . . ? N13 C273 C274 100.7(9) . . ? O49 C273 C274 125.6(10) . . ? C275 C274 C273 106.8(11) . . ? C274 C275 C276 105.5(11) . . ? N13 C276 C275 101.3(10) . . ? C281 C278 C279 96.6(12) . . ? C280 C279 C278 118.4(11) . . ? C279 C280 N15 104.3(10) . . ? C281 N15 C282 129.2(11) . . ? C281 N15 C280 106.7(11) . . ? C282 N15 C280 123.9(10) . . ? O28 C156 O27 123.8(9) . . ? O28 C156 C157 124.1(10) . . ? O27 C156 C157 111.4(9) . . ? C159 C60B C59B 116.5(14) . . ? C159 C60B C63B 124.0(12) . . ? C59B C60B C63B 118.3(15) . . ? C158 C57B C58B 119.8(13) . . ? C158 C57B C56B 120.7(13) . . ? C58B C57B C56B 119.1(14) . . ? O28B C56B O27 123.2(15) . . ? O28B C56B C57B 119.2(17) . . ? O27 C56B C57B 115.6(13) . . ? C60B C59B C58B 118.4(19) . . ? C57B C58B C59B 120.3(17) . . ? C63B C67B C66B 121.8(12) . . ? N8 C66B C67B 125.3(11) . . ? C64B C63B C67B 114.1(13) . . ? C64B C63B C60B 122.8(14) . . ? C67B C63B C60B 122.7(14) . . ? C63B C64B C65B 122.9(15) . . ? C64B C65B N8 117.4(12) . . ? C163 C64C C65C 120.1(12) . . ? C163 C67C C66C 115.7(15) . . ? N8 C65C C64C 129.1(12) . . ? C67C C66C N8 121.5(13) . . ? C303 C304 C300 108.3(13) . . ? C304 C303 C302 100.2(13) . . ? N301 C300 O306 128(2) . . ? N301 C300 C304 113(2) . . ? O306 C300 C304 117.5(15) . . ? C300 N301 C302 112(2) . . ? C300 N301 C305 119(2) . . ? C302 N301 C305 121.3(19) . . ? N301 C302 C303 100.1(16) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.367 _refine_diff_density_min -0.619 _refine_diff_density_rms 0.093 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.006 0.000 0.007 6791 1502 ' ' _platon_squeeze_details ; TGA indicates ~14 molecules of solvate N-methylpyrrolidone (NMP) is present per formula unit however only four (disordered across 7 positions were found crystallographically. An additional 10 NMP (= 20 per unit cell) were removed by the squeeze routine and is consistent with the calculated void electron count. These have been included in the formula ; # Attachment '- complex3_new.CIF' data_complex3_new _database_code_depnum_ccdc_archive 'CCDC 822482' #TrackingRef '- complex3_new.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; dinitroso[(+-)-2,7,12-trimethoxy-3,8,13- tris[3-(3-pyridyl)benzoyl]-10,15-dihydro-5H- tribenzo[a,d,g]cyclononane]cobalt(II) N-methylpyrrolidone clathrate ; _chemical_name_common ; dinitroso((+-)-2,7,12-trimethoxy-3,8,13-tris(3-(3- pyridyl)benzoyl)-10,15-dihydro-5H-tribenzo(a,d,g)cyclononane)cobalt(ii) N-methylpyrrolidone clathrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H81 Co N9 O19' _chemical_formula_weight 1531.47 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' Co Co 0.3494 0.9721 '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 11.482(2) _cell_length_b 15.768(3) _cell_length_c 23.647(4) _cell_angle_alpha 78.404(7) _cell_angle_beta 82.580(7) _cell_angle_gamma 76.245(6) _cell_volume 4058.5(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour pink _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1606 _exptl_absorpt_coefficient_mu 0.285 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9453 _exptl_absorpt_correction_T_max 0.9859 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 X8 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37051 _diffrn_reflns_av_R_equivalents 0.1303 _diffrn_reflns_av_sigmaI/netI 0.2210 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 24.00 _reflns_number_total 12699 _reflns_number_gt 4746 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour)' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Solvent groups were refined isotropically H positions on methyl group C75 were initially geometrically calculated then fixed with a torsion angle that ensured no steric clashes with surrounding atoms. ; _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^)+(0.1000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12699 _refine_ls_number_parameters 845 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2794 _refine_ls_R_factor_gt 0.1269 _refine_ls_wR_factor_ref 0.3579 _refine_ls_wR_factor_gt 0.3061 _refine_ls_goodness_of_fit_ref 1.475 _refine_ls_restrained_S_all 1.475 _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 Co1 Co 0.24189(14) 0.17620(11) 0.40061(6) 0.0468(5) Uani 1 1 d . . . O1 O 0.1004(6) 0.3987(5) 0.0671(3) 0.0436(19) Uani 1 1 d . . . N1 N 0.0760(8) 0.1459(6) 0.3918(4) 0.049(3) Uani 1 1 d . . . C1 C 0.0707(9) 0.7194(7) 0.0062(4) 0.036(3) Uani 1 1 d . . . H1A H 0.0660 0.7084 -0.0331 0.043 Uiso 1 1 calc R . . H1B H 0.0117 0.7749 0.0114 0.043 Uiso 1 1 calc R . . O2 O -0.0479(6) 0.4237(5) 0.1642(3) 0.0384(19) Uani 1 1 d . . . N2 N 0.3033(8) 1.0438(7) 0.4456(4) 0.045(3) Uani 1 1 d . . . C2 C 0.0377(9) 0.6426(7) 0.0511(4) 0.034(3) Uani 1 1 d . . . O3 O -0.1910(7) 0.4291(5) 0.1056(3) 0.050(2) Uani 1 1 d . . . N3 N 0.8229(8) 0.6933(6) -0.3540(4) 0.044(2) Uani 1 1 d . . . C3 C 0.0840(9) 0.5599(7) 0.0388(4) 0.034(3) Uani 1 1 d . . . H3 H 0.1341 0.5539 0.0039 0.041 Uiso 1 1 calc R . . O4 O 0.0307(9) 0.7114(6) 0.3192(3) 0.074(3) Uani 1 1 d . . . N4 N 0.2143(13) 0.2498(10) 0.4928(5) 0.081(4) Uani 1 1 d . . . C4 C 0.0603(9) 0.4834(8) 0.0757(5) 0.039(3) Uani 1 1 d . . . O5 O 0.2155(9) 0.7879(6) 0.2813(3) 0.062(2) Uani 1 1 d . . . N5 N 0.4169(13) 0.1315(7) 0.3223(5) 0.066(3) Uani 1 1 d . . . C5 C -0.0158(10) 0.4972(8) 0.1260(5) 0.041(3) Uani 1 1 d . . . O6 O 0.3258(11) 0.6534(9) 0.2762(6) 0.137(5) Uani 1 1 d . . . C6 C -0.0629(10) 0.5814(8) 0.1390(4) 0.040(3) Uani 1 1 d . . . H6 H -0.1145 0.5883 0.1733 0.048 Uiso 1 1 calc R . . O7 O 0.5559(7) 0.7330(5) 0.0218(3) 0.055(2) Uani 1 1 d . . . N7 N 0.9491(16) 0.9727(12) 0.2940(8) 0.145(6) Uiso 1 1 d . . . C7 C -0.0344(10) 0.6559(7) 0.1017(5) 0.040(3) Uani 1 1 d . . . O8 O 0.4994(6) 0.6250(5) -0.0417(3) 0.0404(19) Uani 1 1 d . . . C8 C -0.0831(10) 0.7420(8) 0.1198(5) 0.048(3) Uani 1 1 d . . . H8A H -0.1638 0.7423 0.1406 0.057 Uiso 1 1 calc R . . H8B H -0.0921 0.7894 0.0852 0.057 Uiso 1 1 calc R . . O9 O 0.5220(7) 0.7379(5) -0.1141(3) 0.049(2) Uani 1 1 d . . . C9 C 0.0002(11) 0.7603(7) 0.1596(5) 0.050(3) Uani 1 1 d . . . O10 O 0.1416(10) 0.2172(7) 0.4808(4) 0.087(4) Uani 1 1 d . . . C10 C -0.0248(11) 0.7295(7) 0.2194(5) 0.047(3) Uani 1 1 d . . . H10 H -0.0918 0.7029 0.2321 0.056 Uiso 1 1 calc R . . O11 O 0.3154(11) 0.2445(7) 0.4589(5) 0.099(3) Uani 1 1 d . . . C11 C 0.0478(12) 0.7379(7) 0.2596(5) 0.051(3) Uani 1 1 d . . . O12 O 0.2097(11) 0.2925(11) 0.5332(5) 0.153(6) Uani 1 1 d . . . C12 C 0.1452(12) 0.7778(8) 0.2399(6) 0.053(3) Uani 1 1 d . . . O13 O 0.4400(8) 0.1620(6) 0.3646(4) 0.080(3) Uani 1 1 d . . . C13 C 0.1662(11) 0.8092(7) 0.1823(5) 0.047(3) Uani 1 1 d . . . H13 H 0.2323 0.8371 0.1700 0.057 Uiso 1 1 calc R . . O14 O 0.4989(10) 0.1027(7) 0.2879(5) 0.103(4) Uani 1 1 d . . . C14 C 0.0958(10) 0.8023(7) 0.1415(5) 0.038(3) Uani 1 1 d . . . O15 O 0.3078(8) 0.1324(6) 0.3193(3) 0.059(2) Uani 1 1 d . . . C15 C 0.1262(10) 0.8436(7) 0.0788(4) 0.046(3) Uani 1 1 d . . . H15A H 0.0521 0.8595 0.0581 0.055 Uiso 1 1 calc R . . H15B H 0.1522 0.8992 0.0785 0.055 Uiso 1 1 calc R . . O16 O 1.0862(15) 0.9600(10) 0.3561(6) 0.177(6) Uiso 1 1 d . . . C16 C 0.2227(10) 0.7849(7) 0.0460(4) 0.037(3) Uani 1 1 d . . . C17 C 0.3409(11) 0.7862(7) 0.0493(4) 0.042(3) Uani 1 1 d . . . H17 H 0.3577 0.8237 0.0726 0.050 Uiso 1 1 calc R . . C18 C 0.4368(11) 0.7357(8) 0.0205(5) 0.042(3) Uani 1 1 d . . . O19 O 1.3548(10) 0.9528(8) 0.1120(5) 0.114(4) Uiso 1 1 d . . . C19 C 0.4079(10) 0.6821(7) -0.0129(4) 0.038(3) Uani 1 1 d . . . C20 C 0.2924(10) 0.6793(7) -0.0176(4) 0.035(3) Uani 1 1 d . . . H20 H 0.2766 0.6415 -0.0410 0.043 Uiso 1 1 calc R . . N21 N 0.1967(18) 0.9654(13) -0.0768(8) 0.159(7) Uiso 1 1 d . . . C21 C 0.1964(10) 0.7309(7) 0.0112(4) 0.039(3) Uani 1 1 d . . . C22 C 0.1879(9) 0.3842(7) 0.0183(4) 0.042(3) Uani 1 1 d . . . H22A H 0.1491 0.4089 -0.0178 0.063 Uiso 1 1 calc R . . H22B H 0.2200 0.3204 0.0201 0.063 Uiso 1 1 calc R . . H22C H 0.2537 0.4134 0.0194 0.063 Uiso 1 1 calc R . . C23 C -0.1408(10) 0.3960(8) 0.1487(5) 0.043(3) Uani 1 1 d . . . C24 C -0.1754(10) 0.3209(8) 0.1930(5) 0.043(3) Uani 1 1 d . . . C25 C -0.2731(10) 0.2898(8) 0.1820(5) 0.045(3) Uani 1 1 d . . . H25 H -0.3112 0.3133 0.1471 0.054 Uiso 1 1 calc R . . C26 C -0.3136(10) 0.2247(8) 0.2225(5) 0.049(3) Uani 1 1 d . . . H26 H -0.3820 0.2047 0.2164 0.058 Uiso 1 1 calc R . . C27 C -0.2552(10) 0.1895(7) 0.2708(5) 0.043(3) Uani 1 1 d . . . H27 H -0.2818 0.1427 0.2973 0.052 Uiso 1 1 calc R . . C28 C -0.1582(9) 0.2186(7) 0.2831(4) 0.038(3) Uani 1 1 d . . . C29 C -0.1186(9) 0.2849(7) 0.2425(4) 0.037(3) Uani 1 1 d . . . H29 H -0.0512 0.3056 0.2493 0.045 Uiso 1 1 calc R . . C30 C -0.1011(10) 0.1810(7) 0.3373(5) 0.041(3) Uani 1 1 d . . . C31 C -0.1671(11) 0.1497(8) 0.3889(5) 0.058(4) Uani 1 1 d . . . H31 H -0.2509 0.1533 0.3888 0.070 Uiso 1 1 calc R . . C32 C -0.1122(11) 0.1146(9) 0.4383(5) 0.064(4) Uani 1 1 d . . . H32 H -0.1552 0.0900 0.4723 0.077 Uiso 1 1 calc R . . C33 C 0.0101(11) 0.1153(8) 0.4382(5) 0.057(4) Uani 1 1 d . . . H33 H 0.0475 0.0927 0.4733 0.068 Uiso 1 1 calc R . . C34 C 0.0190(10) 0.1771(7) 0.3420(5) 0.044(3) Uani 1 1 d . . . H34 H 0.0654 0.1977 0.3080 0.053 Uiso 1 1 calc R . . C35 C -0.0824(14) 0.6789(10) 0.3409(6) 0.094(5) Uani 1 1 d . . . H35A H -0.1521 0.7242 0.3271 0.141 Uiso 1 1 calc R . . H35B H -0.0895 0.6669 0.3834 0.141 Uiso 1 1 calc R . . H35C H -0.0795 0.6242 0.3265 0.141 Uiso 1 1 calc R . . C36 C 0.3071(15) 0.7202(12) 0.2957(6) 0.079(4) Uani 1 1 d . . . C37 C 0.3820(15) 0.7349(10) 0.3368(7) 0.082(5) Uani 1 1 d . . . C38 C 0.4951(16) 0.6748(11) 0.3482(8) 0.109(6) Uani 1 1 d . . . H38 H 0.5199 0.6251 0.3290 0.130 Uiso 1 1 calc R . . C39 C 0.5666(15) 0.6867(13) 0.3851(8) 0.107(6) Uani 1 1 d . . . H39 H 0.6426 0.6471 0.3901 0.129 Uiso 1 1 calc R . . C40 C 0.5326(13) 0.7544(11) 0.4156(6) 0.079(4) Uani 1 1 d . . . H40 H 0.5839 0.7607 0.4423 0.095 Uiso 1 1 calc R . . C41 C 0.4231(12) 0.8147(9) 0.4079(5) 0.060(4) Uani 1 1 d . . . C42 C 0.3468(13) 0.8064(9) 0.3662(5) 0.066(4) Uani 1 1 d . . . H42 H 0.2740 0.8490 0.3590 0.080 Uiso 1 1 calc R . . C43 C 0.3870(11) 0.8888(9) 0.4428(6) 0.054(3) Uani 1 1 d . . . C44 C 0.4165(10) 0.8755(10) 0.4986(6) 0.055(4) Uani 1 1 d . . . H44 H 0.4556 0.8184 0.5170 0.066 Uiso 1 1 calc R . . C45 C 0.3894(11) 0.9441(11) 0.5268(6) 0.060(4) Uani 1 1 d . . . H45 H 0.4087 0.9351 0.5657 0.072 Uiso 1 1 calc R . . C46 C 0.3336(10) 1.0283(10) 0.5003(5) 0.056(4) Uani 1 1 d . . . H46 H 0.3164 1.0758 0.5214 0.067 Uiso 1 1 calc R . . C47 C 0.3271(11) 0.9761(10) 0.4184(5) 0.054(3) Uani 1 1 d . . . H47 H 0.3031 0.9858 0.3803 0.065 Uiso 1 1 calc R . . C48 C 0.5850(12) 0.7853(11) 0.0566(6) 0.088(5) Uani 1 1 d . . . H48A H 0.5507 0.8480 0.0423 0.133 Uiso 1 1 calc R . . H48B H 0.6727 0.7761 0.0554 0.133 Uiso 1 1 calc R . . H48C H 0.5522 0.7688 0.0966 0.133 Uiso 1 1 calc R . . C49 C 0.5445(9) 0.6615(8) -0.0948(4) 0.037(3) Uani 1 1 d . . . C50 C 0.6225(9) 0.5903(7) -0.1257(4) 0.037(3) Uani 1 1 d . . . C51 C 0.6854(10) 0.6159(7) -0.1785(4) 0.037(3) Uani 1 1 d . . . H51 H 0.6798 0.6774 -0.1930 0.045 Uiso 1 1 calc R . . C52 C 0.7541(10) 0.5562(8) -0.2100(4) 0.037(3) Uani 1 1 d . . . C53 C 0.7607(10) 0.4668(8) -0.1876(5) 0.045(3) Uani 1 1 d . . . H53 H 0.8094 0.4239 -0.2087 0.053 Uiso 1 1 calc R . . C54 C 0.7003(10) 0.4386(8) -0.1369(5) 0.048(3) Uani 1 1 d . . . H54 H 0.7062 0.3769 -0.1230 0.058 Uiso 1 1 calc R . . C55 C 0.6311(10) 0.4991(8) -0.1060(5) 0.046(3) Uani 1 1 d . . . H55 H 0.5880 0.4795 -0.0706 0.055 Uiso 1 1 calc R . . C56 C 0.8180(10) 0.5845(8) -0.2658(5) 0.041(3) Uani 1 1 d . . . C57 C 0.9305(10) 0.5381(8) -0.2840(5) 0.043(3) Uani 1 1 d . . . H57 H 0.9691 0.4856 -0.2601 0.052 Uiso 1 1 calc R . . C58 C 0.9859(10) 0.5681(8) -0.3366(5) 0.047(3) Uani 1 1 d . . . H58 H 1.0622 0.5358 -0.3495 0.056 Uiso 1 1 calc R . . C59 C 0.9314(11) 0.6446(9) -0.3705(5) 0.049(3) Uani 1 1 d . . . H59 H 0.9711 0.6643 -0.4069 0.059 Uiso 1 1 calc R . . C60 C 0.7699(10) 0.6600(8) -0.3027(4) 0.039(3) Uani 1 1 d . . . H60 H 0.6922 0.6918 -0.2911 0.047 Uiso 1 1 calc R . . O61 O 0.1436(11) 1.0595(8) -0.0209(5) 0.105(4) Uiso 1 1 d . . . C66 C 0.8425(16) 0.9446(12) 0.2888(7) 0.116(6) Uiso 1 1 d . . . H66A H 0.8603 0.8927 0.2691 0.139 Uiso 1 1 calc R . . H66B H 0.7832 0.9931 0.2678 0.139 Uiso 1 1 calc R . . C67 C 0.8015(16) 0.9220(12) 0.3486(7) 0.117(6) Uiso 1 1 d . . . H67A H 0.7632 0.8705 0.3544 0.141 Uiso 1 1 calc R . . H67B H 0.7416 0.9726 0.3611 0.141 Uiso 1 1 calc R . . C68 C 0.9128(15) 0.8986(11) 0.3845(7) 0.106(5) Uiso 1 1 d . . . H68A H 0.8941 0.9226 0.4210 0.127 Uiso 1 1 calc R . . H68B H 0.9455 0.8339 0.3932 0.127 Uiso 1 1 calc R . . C69 C 0.9932(19) 0.9437(13) 0.3438(9) 0.117(6) Uiso 1 1 d . . . C70 C 1.012(2) 1.0139(16) 0.2415(10) 0.198(10) Uiso 1 1 d . . . H70A H 0.9595 1.0301 0.2097 0.237 Uiso 1 1 calc R . . H70B H 1.0855 0.9719 0.2310 0.237 Uiso 1 1 calc R . . H70C H 1.0328 1.0673 0.2488 0.237 Uiso 1 1 calc R . . C71 C 0.6791(15) 0.4441(11) 0.3268(7) 0.110(6) Uiso 1 1 d . . . H71A H 0.7500 0.3939 0.3312 0.132 Uiso 1 1 calc R . . H71B H 0.6619 0.4699 0.3626 0.132 Uiso 1 1 calc R . . O72 O 0.5954(16) 0.5892(12) 0.1820(8) 0.216(7) Uiso 1 1 d . . . C72 C 0.5723(19) 0.4142(15) 0.3142(9) 0.155(8) Uiso 1 1 d . . . H72A H 0.5943 0.3500 0.3126 0.187 Uiso 1 1 calc R . . H72B H 0.5067 0.4241 0.3453 0.187 Uiso 1 1 calc R . . N73 N 0.7017(16) 0.5162(12) 0.2725(7) 0.151(6) Uiso 1 1 d . . . C73 C 0.5342(19) 0.4618(14) 0.2619(9) 0.149(8) Uiso 1 1 d . . . H73A H 0.4512 0.4970 0.2676 0.179 Uiso 1 1 calc R . . H73B H 0.5341 0.4207 0.2352 0.179 Uiso 1 1 calc R . . C74 C 0.6145(14) 0.5202(10) 0.2371(7) 0.084(5) Uiso 1 1 d . . . C75 C 0.7738(10) 0.5644(8) 0.2672(5) 0.048(3) Uiso 1 1 d . . . H75A H 0.8512 0.5356 0.2499 0.072 Uiso 1 1 d . . . H75B H 0.7834 0.5762 0.3052 0.072 Uiso 1 1 d . . . H75C H 0.7426 0.6209 0.2418 0.072 Uiso 1 1 d . . . N76 N 1.2995(12) 1.0414(10) 0.1793(6) 0.106(4) Uiso 1 1 d . . . C76 C 1.2475(16) 1.1357(12) 0.1873(7) 0.121(6) Uiso 1 1 d . . . H76A H 1.1898 1.1387 0.2222 0.145 Uiso 1 1 calc R . . H76B H 1.3112 1.1672 0.1898 0.145 Uiso 1 1 calc R . . C77 C 1.1858(15) 1.1715(11) 0.1327(7) 0.109(6) Uiso 1 1 d . . . H77A H 1.1903 1.2342 0.1185 0.130 Uiso 1 1 calc R . . H77B H 1.1001 1.1678 0.1394 0.130 Uiso 1 1 calc R . . C78 C 1.2542(14) 1.1122(10) 0.0879(6) 0.089(5) Uiso 1 1 d . . . H78A H 1.1985 1.1041 0.0617 0.107 Uiso 1 1 calc R . . H78B H 1.3190 1.1384 0.0644 0.107 Uiso 1 1 calc R . . C79 C 1.3592(18) 0.9757(13) 0.2269(8) 0.155(8) Uiso 1 1 d . . . H79A H 1.3449 1.0013 0.2623 0.186 Uiso 1 1 calc R . . H79B H 1.4459 0.9601 0.2161 0.186 Uiso 1 1 calc R . . H79C H 1.3261 0.9223 0.2337 0.186 Uiso 1 1 calc R . . C80 C 1.3046(16) 1.0269(13) 0.1251(8) 0.105(5) Uiso 1 1 d . . . C81 C 0.2861(16) 0.9096(12) -0.1145(8) 0.117(6) Uiso 1 1 d . . . H81A H 0.2745 0.9280 -0.1563 0.140 Uiso 1 1 calc R . . H81B H 0.2911 0.8451 -0.1022 0.140 Uiso 1 1 calc R . . C82 C 0.397(3) 0.943(2) -0.0952(14) 0.258(15) Uiso 1 1 d . . . H82A H 0.4578 0.8917 -0.0784 0.309 Uiso 1 1 calc R . . H82B H 0.4361 0.9767 -0.1293 0.309 Uiso 1 1 calc R . . C83 C 0.352(2) 0.9954(17) -0.0559(11) 0.191(10) Uiso 1 1 d . . . H83A H 0.3789 1.0519 -0.0676 0.230 Uiso 1 1 calc R . . H83B H 0.3819 0.9659 -0.0179 0.230 Uiso 1 1 calc R . . C84 C 0.201(2) 1.0164(15) -0.0497(9) 0.126(7) Uiso 1 1 d . . . C85 C 0.0813(18) 0.9512(13) -0.0841(8) 0.145(7) Uiso 1 1 d . . . H85A H 0.0916 0.9058 -0.1083 0.174 Uiso 1 1 calc R . . H85B H 0.0317 1.0068 -0.1029 0.174 Uiso 1 1 calc R . . H85C H 0.0417 0.9314 -0.0461 0.174 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 Co1 0.0398(10) 0.0595(12) 0.0373(10) 0.0072(8) -0.0013(7) -0.0177(9) O1 0.039(5) 0.038(5) 0.052(5) -0.006(4) 0.003(4) -0.012(4) N1 0.043(6) 0.056(7) 0.042(6) 0.008(5) 0.000(5) -0.016(5) C1 0.028(7) 0.039(7) 0.038(6) -0.004(5) 0.002(5) -0.010(6) O2 0.039(5) 0.041(5) 0.038(4) 0.002(4) -0.003(4) -0.020(4) N2 0.041(6) 0.064(8) 0.034(6) 0.002(5) -0.009(5) -0.025(6) C2 0.023(6) 0.036(8) 0.040(7) -0.003(6) 0.003(5) -0.008(6) O3 0.048(5) 0.060(6) 0.044(5) 0.005(4) -0.010(4) -0.025(4) N3 0.034(6) 0.056(7) 0.040(6) -0.001(5) -0.003(5) -0.015(6) C3 0.019(6) 0.041(8) 0.041(7) -0.008(6) 0.009(5) -0.010(6) O4 0.098(8) 0.073(7) 0.049(6) -0.014(5) 0.020(5) -0.028(6) N4 0.060(10) 0.114(12) 0.043(8) 0.016(8) 0.007(7) -0.001(9) C4 0.027(7) 0.040(8) 0.050(8) -0.004(6) -0.001(6) -0.009(6) O5 0.075(7) 0.051(6) 0.055(6) -0.007(5) -0.003(5) -0.010(6) N5 0.086(11) 0.055(8) 0.051(8) 0.005(6) -0.007(8) -0.016(8) C5 0.034(7) 0.050(9) 0.040(7) 0.005(6) 0.002(6) -0.025(7) O6 0.127(11) 0.110(10) 0.184(13) -0.102(10) -0.061(9) 0.046(8) C6 0.040(7) 0.042(8) 0.039(7) -0.009(6) 0.006(5) -0.014(6) O7 0.035(5) 0.078(6) 0.058(5) -0.021(5) 0.005(4) -0.024(5) C7 0.043(8) 0.035(8) 0.045(7) -0.011(6) 0.002(6) -0.015(6) O8 0.041(5) 0.041(5) 0.033(4) 0.001(4) 0.009(4) -0.010(4) C8 0.028(7) 0.061(9) 0.051(8) -0.011(7) 0.013(6) -0.010(7) O9 0.056(6) 0.027(5) 0.052(5) 0.004(4) 0.009(4) -0.002(4) C9 0.045(8) 0.026(7) 0.066(9) -0.009(6) 0.019(7) 0.005(6) O10 0.078(8) 0.125(10) 0.061(7) 0.001(6) -0.021(6) -0.039(7) C10 0.059(9) 0.034(8) 0.047(8) -0.007(6) 0.013(7) -0.018(6) O11 0.099(9) 0.113(9) 0.092(8) -0.004(7) -0.051(7) -0.028(7) C11 0.076(10) 0.032(8) 0.035(8) -0.007(6) 0.016(7) 0.000(7) O12 0.130(11) 0.275(18) 0.090(9) -0.115(11) 0.008(8) -0.053(11) C12 0.056(9) 0.050(9) 0.056(9) -0.018(7) 0.006(7) -0.017(7) O13 0.072(7) 0.087(8) 0.074(7) 0.013(6) -0.011(6) -0.025(6) C13 0.053(8) 0.048(8) 0.039(7) -0.008(6) 0.022(6) -0.023(7) O14 0.072(8) 0.097(9) 0.143(10) -0.042(8) 0.050(7) -0.036(7) C14 0.032(7) 0.031(7) 0.047(7) -0.005(6) 0.007(6) -0.007(6) O15 0.036(5) 0.072(7) 0.062(6) 0.004(4) -0.003(4) -0.014(5) C15 0.055(8) 0.034(7) 0.048(7) -0.006(6) 0.012(6) -0.019(6) C16 0.037(8) 0.032(7) 0.043(7) -0.002(6) 0.009(6) -0.020(6) C17 0.052(9) 0.045(8) 0.031(6) -0.011(6) 0.011(6) -0.022(7) C18 0.040(8) 0.040(8) 0.042(7) 0.000(6) 0.006(6) -0.014(7) C19 0.038(8) 0.035(7) 0.031(7) 0.005(6) 0.017(6) -0.006(6) C20 0.040(8) 0.040(8) 0.026(6) 0.004(5) 0.000(6) -0.018(6) C21 0.040(8) 0.031(7) 0.036(7) 0.012(6) 0.004(6) -0.010(6) C22 0.034(7) 0.044(8) 0.044(7) -0.010(6) 0.013(6) -0.007(6) C23 0.031(7) 0.043(8) 0.049(8) -0.008(7) 0.009(6) -0.007(6) C24 0.041(8) 0.049(8) 0.040(7) 0.000(6) 0.003(6) -0.020(7) C25 0.038(8) 0.058(9) 0.039(7) 0.001(6) -0.006(6) -0.017(7) C26 0.042(8) 0.062(9) 0.050(8) 0.000(7) -0.005(6) -0.033(7) C27 0.048(8) 0.044(8) 0.038(7) 0.003(6) 0.003(6) -0.022(7) C28 0.027(7) 0.050(8) 0.036(7) 0.003(6) 0.003(5) -0.017(6) C29 0.022(6) 0.043(8) 0.043(7) -0.004(6) 0.010(6) -0.010(6) C30 0.036(8) 0.041(8) 0.042(7) 0.003(6) 0.006(6) -0.014(6) C31 0.043(8) 0.067(10) 0.060(9) 0.013(7) -0.002(7) -0.026(7) C32 0.046(9) 0.090(11) 0.044(8) 0.031(7) 0.002(7) -0.031(8) C33 0.055(9) 0.071(10) 0.042(8) 0.018(7) -0.011(7) -0.032(8) C34 0.053(9) 0.047(8) 0.034(7) -0.006(6) 0.006(6) -0.022(7) C35 0.132(15) 0.080(12) 0.067(10) -0.021(8) 0.040(10) -0.034(11) C36 0.089(13) 0.079(13) 0.067(10) -0.029(10) -0.003(9) -0.005(11) C37 0.094(13) 0.065(11) 0.085(11) -0.032(9) -0.010(10) 0.005(10) C38 0.084(14) 0.077(13) 0.153(17) -0.041(12) -0.026(13) 0.033(11) C39 0.061(12) 0.136(18) 0.114(15) -0.035(13) -0.024(11) 0.019(11) C40 0.064(11) 0.080(12) 0.071(10) -0.005(9) -0.013(8) 0.022(9) C41 0.056(10) 0.063(10) 0.052(9) 0.006(7) 0.004(7) -0.013(8) C42 0.073(10) 0.068(11) 0.057(9) 0.001(8) -0.014(8) -0.019(8) C43 0.038(8) 0.063(10) 0.062(9) 0.003(8) -0.007(7) -0.023(7) C44 0.035(8) 0.070(11) 0.060(10) 0.007(8) -0.009(7) -0.024(7) C45 0.044(9) 0.090(12) 0.047(8) 0.022(9) -0.010(7) -0.040(9) C46 0.042(8) 0.081(11) 0.051(9) -0.001(8) 0.000(7) -0.037(8) C47 0.053(9) 0.063(10) 0.043(8) 0.009(8) -0.003(7) -0.024(8) C48 0.055(10) 0.147(16) 0.082(11) -0.052(10) 0.001(8) -0.035(10) C49 0.031(7) 0.041(8) 0.037(7) -0.003(7) 0.007(6) -0.011(6) C50 0.036(7) 0.041(8) 0.035(7) 0.003(6) -0.003(6) -0.017(6) C51 0.045(8) 0.034(7) 0.028(6) 0.012(6) -0.007(6) -0.014(6) C52 0.042(8) 0.037(8) 0.029(6) 0.000(6) 0.002(6) -0.011(6) C53 0.043(8) 0.044(9) 0.046(8) -0.009(6) -0.002(6) -0.009(6) C54 0.052(8) 0.034(8) 0.057(8) -0.014(7) 0.017(7) -0.009(7) C55 0.043(8) 0.049(9) 0.039(7) 0.010(6) 0.001(6) -0.016(7) C56 0.032(8) 0.046(8) 0.048(8) -0.014(7) 0.000(6) -0.012(6) C57 0.041(8) 0.050(8) 0.039(7) -0.006(6) 0.000(6) -0.011(7) C58 0.043(8) 0.052(9) 0.044(8) -0.021(7) 0.004(7) -0.003(7) C59 0.044(8) 0.064(10) 0.034(7) -0.005(7) 0.003(6) -0.009(7) C60 0.031(7) 0.048(8) 0.037(7) -0.005(6) 0.006(6) -0.013(6) _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 Co1 N1 2.115(9) . ? Co1 N3 2.139(9) 2_665 ? Co1 N2 2.141(10) 1_545 ? Co1 O15 2.158(8) . ? Co1 O10 2.217(11) . ? Co1 O11 2.258(9) . ? Co1 O13 2.299(9) . ? O1 C4 1.352(12) . ? O1 C22 1.447(11) . ? N1 C33 1.325(13) . ? N1 C34 1.368(12) . ? C1 C21 1.519(13) . ? C1 C2 1.528(13) . ? O2 C23 1.359(12) . ? O2 C5 1.412(12) . ? N2 C47 1.310(14) . ? N2 C46 1.344(13) . ? N2 Co1 2.141(10) 1_565 ? C2 C3 1.360(14) . ? C2 C7 1.387(14) . ? O3 C23 1.200(12) . ? N3 C60 1.351(12) . ? N3 C59 1.354(13) . ? N3 Co1 2.139(9) 2_665 ? C3 C4 1.401(14) . ? O4 C11 1.388(13) . ? O4 C35 1.500(15) . ? N4 O10 1.169(15) . ? N4 O12 1.263(16) . ? N4 O11 1.319(14) . ? C4 C5 1.404(14) . ? O5 C36 1.332(17) . ? O5 C12 1.401(13) . ? N5 O14 1.225(13) . ? N5 O15 1.259(13) . ? N5 O13 1.275(12) . ? C5 C6 1.388(14) . ? O6 C36 1.195(16) . ? C6 C7 1.399(14) . ? O7 C18 1.362(12) . ? O7 C48 1.395(13) . ? N7 C69 1.30(2) . ? N7 C66 1.42(2) . ? N7 C70 1.47(2) . ? C7 C8 1.466(14) . ? O8 C49 1.364(12) . ? O8 C19 1.410(12) . ? C8 C9 1.535(15) . ? O9 C49 1.178(12) . ? C9 C14 1.391(14) . ? C9 C10 1.417(15) . ? C10 C11 1.387(15) . ? C11 C12 1.395(15) . ? C12 C13 1.363(15) . ? C13 C14 1.372(14) . ? C14 C15 1.528(14) . ? C15 C16 1.505(14) . ? O16 C69 1.24(2) . ? C16 C17 1.375(14) . ? C16 C21 1.400(14) . ? C17 C18 1.384(15) . ? C18 C19 1.386(14) . ? O19 C80 1.254(18) . ? C19 C20 1.356(14) . ? C20 C21 1.395(14) . ? N21 C84 1.14(2) . ? N21 C85 1.43(2) . ? N21 C81 1.51(2) . ? C23 C24 1.509(15) . ? C24 C29 1.368(13) . ? C24 C25 1.398(14) . ? C25 C26 1.379(14) . ? C26 C27 1.352(13) . ? C27 C28 1.385(13) . ? C28 C29 1.390(13) . ? C28 C30 1.466(14) . ? C30 C34 1.383(14) . ? C30 C31 1.415(14) . ? C31 C32 1.355(14) . ? C32 C33 1.407(15) . ? C36 C37 1.463(19) . ? C37 C42 1.394(17) . ? C37 C38 1.435(19) . ? C38 C39 1.341(19) . ? C39 C40 1.359(19) . ? C40 C41 1.393(17) . ? C41 C42 1.443(16) . ? C41 C43 1.512(17) . ? C43 C44 1.368(15) . ? C43 C47 1.426(16) . ? C44 C45 1.337(16) . ? C45 C46 1.389(16) . ? C49 C50 1.509(15) . ? C50 C51 1.396(13) . ? C50 C55 1.403(14) . ? C51 C52 1.356(14) . ? C52 C53 1.391(14) . ? C52 C56 1.466(14) . ? C53 C54 1.354(14) . ? C54 C55 1.359(14) . ? C56 C60 1.370(14) . ? C56 C57 1.386(14) . ? C57 C58 1.369(14) . ? C58 C59 1.369(14) . ? O61 C84 1.10(2) . ? C66 C67 1.433(19) . ? C67 C68 1.56(2) . ? C68 C69 1.45(2) . ? C71 C72 1.50(2) . ? C71 N73 1.57(2) . ? O72 C74 1.52(2) . ? C72 C73 1.38(2) . ? N73 C75 1.230(17) . ? N73 C74 1.368(19) . ? C73 C74 1.45(2) . ? N76 C80 1.338(18) . ? N76 C79 1.48(2) . ? N76 C76 1.504(19) . ? C76 C77 1.497(19) . ? C77 C78 1.564(19) . ? C78 C80 1.48(2) . ? C81 C82 1.64(3) . ? C82 C83 1.34(3) . ? C83 C84 1.67(3) . ? 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 Co1 N3 88.4(3) . 2_665 ? N1 Co1 N2 90.0(3) . 1_545 ? N3 Co1 N2 178.1(4) 2_665 1_545 ? N1 Co1 O15 87.7(4) . . ? N3 Co1 O15 89.3(3) 2_665 . ? N2 Co1 O15 89.7(4) 1_545 . ? N1 Co1 O10 81.6(4) . . ? N3 Co1 O10 89.5(4) 2_665 . ? N2 Co1 O10 91.3(4) 1_545 . ? O15 Co1 O10 169.3(4) . . ? N1 Co1 O11 137.7(4) . . ? N3 Co1 O11 85.6(3) 2_665 . ? N2 Co1 O11 96.3(4) 1_545 . ? O15 Co1 O11 133.9(4) . . ? O10 Co1 O11 56.5(4) . . ? N1 Co1 O13 144.7(4) . . ? N3 Co1 O13 97.1(3) 2_665 . ? N2 Co1 O13 83.7(3) 1_545 . ? O15 Co1 O13 57.6(3) . . ? O10 Co1 O13 133.1(4) . . ? O11 Co1 O13 77.7(4) . . ? C4 O1 C22 116.8(8) . . ? C33 N1 C34 116.3(10) . . ? C33 N1 Co1 120.3(8) . . ? C34 N1 Co1 121.4(7) . . ? C21 C1 C2 112.0(8) . . ? C23 O2 C5 114.6(8) . . ? C47 N2 C46 117.3(11) . . ? C47 N2 Co1 121.0(8) . 1_565 ? C46 N2 Co1 121.2(9) . 1_565 ? C3 C2 C7 121.7(10) . . ? C3 C2 C1 116.0(9) . . ? C7 C2 C1 122.2(10) . . ? C60 N3 C59 115.7(10) . . ? C60 N3 Co1 123.2(8) . 2_665 ? C59 N3 Co1 120.3(8) . 2_665 ? C2 C3 C4 122.3(10) . . ? C11 O4 C35 115.9(10) . . ? O10 N4 O12 129.5(14) . . ? O10 N4 O11 116.6(15) . . ? O12 N4 O11 113.9(15) . . ? O1 C4 C3 126.9(10) . . ? O1 C4 C5 117.1(10) . . ? C3 C4 C5 115.9(11) . . ? C36 O5 C12 116.0(11) . . ? O14 N5 O15 124.0(13) . . ? O14 N5 O13 119.9(14) . . ? O15 N5 O13 116.1(13) . . ? C6 C5 C4 122.1(10) . . ? C6 C5 O2 118.5(10) . . ? C4 C5 O2 119.3(11) . . ? C5 C6 C7 120.2(10) . . ? C18 O7 C48 116.8(9) . . ? C69 N7 C66 114.6(19) . . ? C69 N7 C70 125(2) . . ? C66 N7 C70 118.8(19) . . ? C2 C7 C6 117.7(10) . . ? C2 C7 C8 125.4(10) . . ? C6 C7 C8 116.9(10) . . ? C49 O8 C19 116.1(8) . . ? C7 C8 C9 110.7(9) . . ? C14 C9 C10 119.3(11) . . ? C14 C9 C8 125.8(10) . . ? C10 C9 C8 114.9(10) . . ? N4 O10 Co1 96.5(10) . . ? C11 C10 C9 120.6(11) . . ? N4 O11 Co1 90.3(9) . . ? C10 C11 O4 125.4(12) . . ? C10 C11 C12 118.6(10) . . ? O4 C11 C12 116.0(12) . . ? C13 C12 C11 120.1(11) . . ? C13 C12 O5 122.0(11) . . ? C11 C12 O5 117.8(11) . . ? N5 O13 Co1 89.4(8) . . ? C12 C13 C14 122.6(11) . . ? C13 C14 C9 118.7(10) . . ? C13 C14 C15 117.3(9) . . ? C9 C14 C15 124.0(10) . . ? N5 O15 Co1 96.5(8) . . ? C16 C15 C14 114.6(9) . . ? C17 C16 C21 119.0(10) . . ? C17 C16 C15 118.6(10) . . ? C21 C16 C15 122.4(10) . . ? C16 C17 C18 123.5(10) . . ? O7 C18 C17 126.9(11) . . ? O7 C18 C19 116.9(11) . . ? C17 C18 C19 116.2(11) . . ? C20 C19 C18 122.2(11) . . ? C20 C19 O8 117.3(10) . . ? C18 C19 O8 120.4(10) . . ? C19 C20 C21 121.2(10) . . ? C84 N21 C85 119(2) . . ? C84 N21 C81 135(2) . . ? C85 N21 C81 105.8(18) . . ? C20 C21 C16 118.0(10) . . ? C20 C21 C1 117.4(10) . . ? C16 C21 C1 124.4(10) . . ? O3 C23 O2 123.8(10) . . ? O3 C23 C24 124.1(11) . . ? O2 C23 C24 112.0(10) . . ? C29 C24 C25 120.2(10) . . ? C29 C24 C23 123.5(10) . . ? C25 C24 C23 116.4(10) . . ? C26 C25 C24 119.1(10) . . ? C27 C26 C25 119.6(10) . . ? C26 C27 C28 122.8(10) . . ? C27 C28 C29 117.4(10) . . ? C27 C28 C30 120.8(9) . . ? C29 C28 C30 121.9(9) . . ? C24 C29 C28 120.9(10) . . ? C34 C30 C31 115.7(10) . . ? C34 C30 C28 122.4(9) . . ? C31 C30 C28 121.8(10) . . ? C32 C31 C30 120.8(11) . . ? C31 C32 C33 118.4(10) . . ? N1 C33 C32 123.6(10) . . ? N1 C34 C30 125.0(10) . . ? O6 C36 O5 122.2(15) . . ? O6 C36 C37 123.5(17) . . ? O5 C36 C37 114.4(15) . . ? C42 C37 C38 117.9(15) . . ? C42 C37 C36 121.9(15) . . ? C38 C37 C36 120.2(15) . . ? C39 C38 C37 121.8(16) . . ? C38 C39 C40 121.3(16) . . ? C39 C40 C41 120.4(15) . . ? C40 C41 C42 119.7(14) . . ? C40 C41 C43 119.2(13) . . ? C42 C41 C43 121.0(12) . . ? C37 C42 C41 118.8(14) . . ? C44 C43 C47 117.1(13) . . ? C44 C43 C41 120.8(13) . . ? C47 C43 C41 122.0(12) . . ? C45 C44 C43 118.9(13) . . ? C44 C45 C46 121.5(13) . . ? N2 C46 C45 121.3(13) . . ? N2 C47 C43 123.9(12) . . ? O9 C49 O8 124.0(10) . . ? O9 C49 C50 125.3(10) . . ? O8 C49 C50 110.6(10) . . ? C51 C50 C55 117.4(11) . . ? C51 C50 C49 118.6(10) . . ? C55 C50 C49 123.9(10) . . ? C52 C51 C50 122.3(10) . . ? C51 C52 C53 117.5(10) . . ? C51 C52 C56 121.5(10) . . ? C53 C52 C56 121.0(11) . . ? C54 C53 C52 122.5(11) . . ? C53 C54 C55 119.5(11) . . ? C54 C55 C50 120.8(10) . . ? C60 C56 C57 116.2(10) . . ? C60 C56 C52 121.3(11) . . ? C57 C56 C52 122.5(11) . . ? C58 C57 C56 119.8(11) . . ? C59 C58 C57 120.1(11) . . ? N3 C59 C58 122.2(11) . . ? N3 C60 C56 126.0(11) . . ? N7 C66 C67 100.8(15) . . ? C66 C67 C68 107.8(15) . . ? C69 C68 C67 99.5(15) . . ? O16 C69 N7 124(2) . . ? O16 C69 C68 125(2) . . ? N7 C69 C68 111.0(19) . . ? C72 C71 N73 104.4(15) . . ? C73 C72 C71 108.9(19) . . ? C75 N73 C74 128.5(18) . . ? C75 N73 C71 126.3(16) . . ? C74 N73 C71 104.8(15) . . ? C72 C73 C74 109.0(18) . . ? N73 C74 C73 112.8(16) . . ? N73 C74 O72 122.2(15) . . ? C73 C74 O72 124.4(16) . . ? C80 N76 C79 123.8(16) . . ? C80 N76 C76 115.2(15) . . ? C79 N76 C76 120.1(14) . . ? C77 C76 N76 100.3(13) . . ? C76 C77 C78 105.8(14) . . ? C80 C78 C77 103.2(13) . . ? O19 C80 N76 121.1(17) . . ? O19 C80 C78 130.5(17) . . ? N76 C80 C78 108.1(17) . . ? N21 C81 C82 90.8(17) . . ? C83 C82 C81 108(3) . . ? C82 C83 C84 111(2) . . ? O61 C84 N21 141(3) . . ? O61 C84 C83 124(2) . . ? N21 C84 C83 94(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.564 _refine_diff_density_min -0.562 _refine_diff_density_rms 0.165 # Attachment '- complex4_new.cif' data_complex4_new _database_code_depnum_ccdc_archive 'CCDC 822483' #TrackingRef '- complex4_new.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (N-methylpyrrolidone)tetranitroso bis[(+-)-2,7,12-trimethoxy-3,8,13-tris[4- (4-pyridyl)benzoyl]-10,15-dihydro-5H- tribenzo[a,d,g]cyclononane]dicadmium(II) N-methylpyrrolidone clathrate ; _chemical_name_common ; (N-methylpyrrolidone)tetranitroso bis((+-)-2,7,12-trimethoxy- 3,8,13-tris(4-(4-pyridyl)benzoyl)-10,15-dihydro-5H- tribenzo(a,d,g)cyclononane)dicadmium(ii) N-methylpyrrolidone clathrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C170 H188 Cd2 N20 O44' _chemical_formula_weight 3440.20 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' Cd Cd -0.8075 1.2024 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 20.523(2) _cell_length_b 22.227(2) _cell_length_c 22.922(3) _cell_angle_alpha 79.579(7) _cell_angle_beta 73.913(7) _cell_angle_gamma 72.387(6) _cell_volume 9521.9(18) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.200 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3592 _exptl_absorpt_coefficient_mu 0.299 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9044 _exptl_absorpt_correction_T_max 0.9701 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 X8 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 114080 _diffrn_reflns_av_R_equivalents 0.0727 _diffrn_reflns_av_sigmaI/netI 0.1383 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 25.00 _reflns_number_total 33333 _reflns_number_gt 14780 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Large residual peak is 1.03 A from Cd2. Nitrates refined isotropically. ; _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^)+(0.1802P)^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 33333 _refine_ls_number_parameters 1478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1737 _refine_ls_R_factor_gt 0.1066 _refine_ls_wR_factor_ref 0.3023 _refine_ls_wR_factor_gt 0.2740 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.936 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.30431(4) 0.21717(3) 0.73210(3) 0.0874(3) Uani 1 1 d . . . Cd2 Cd -0.25174(2) 1.24663(2) 1.23252(2) 0.05076(19) Uani 1 1 d . . . O1 O 0.3881(2) 0.6476(2) 0.9857(2) 0.0600(13) Uani 1 1 d . . . O2 O 0.4821(2) 0.60579(19) 0.8828(2) 0.0486(11) Uani 1 1 d . . . O3 O 0.5432(2) 0.52522(18) 0.9397(2) 0.0465(11) Uani 1 1 d . . . O4 O 0.6736(2) 0.8125(2) 0.67663(18) 0.0481(11) Uani 1 1 d . . . O5 O 0.6528(2) 0.93248(19) 0.70317(18) 0.0432(10) Uani 1 1 d . . . O6 O 0.7720(2) 0.9088(2) 0.69061(19) 0.0453(11) Uani 1 1 d . . . O7 O 0.3899(2) 1.03592(19) 0.9674(2) 0.0506(11) Uani 1 1 d . . . O8 O 0.3233(2) 0.9550(2) 1.0460(2) 0.0451(11) Uani 1 1 d . . . O9 O 0.3540(2) 0.97576(19) 1.1272(2) 0.0433(10) Uani 1 1 d . . . O10 O 0.1193(2) -0.1464(2) 0.4979(2) 0.0585(13) Uani 1 1 d . . . O11 O 0.0287(2) -0.1069(2) 0.6024(2) 0.0495(11) Uani 1 1 d . . . O12 O -0.0442(3) -0.0184(2) 0.5624(3) 0.0717(16) Uani 1 1 d . . . O13 O -0.1779(2) -0.2909(2) 0.80666(19) 0.0479(11) Uani 1 1 d . . . O14 O -0.1529(2) -0.41249(19) 0.78458(19) 0.0437(10) Uani 1 1 d . . . O15 O -0.2712(2) -0.39102(19) 0.79378(19) 0.0421(10) Uani 1 1 d . . . O16 O 0.1133(3) -0.5283(2) 0.5301(2) 0.0627(13) Uani 1 1 d . . . O17 O 0.1798(2) -0.4525(2) 0.4456(2) 0.0581(13) Uani 1 1 d . . . O18 O 0.1450(2) -0.4831(2) 0.3718(2) 0.0545(12) Uani 1 1 d . . . O21 O 0.1978(2) 0.2860(2) 0.7707(2) 0.0517(12) Uiso 1 1 d . A 2 O23 O 0.2470(3) 0.1847(3) 0.8378(3) 0.0830(16) Uiso 1 1 d . A . O24 O 0.3380(4) 0.1149(3) 0.7980(3) 0.113(2) Uiso 1 1 d . A . O25 O 0.2652(4) 0.0875(4) 0.8856(4) 0.133(3) Uiso 1 1 d . A . O26 O -0.2177(3) 1.3111(3) 1.2857(3) 0.0726(15) Uiso 1 1 d . . . O27 O -0.2159(9) 1.4093(8) 1.2879(8) 0.281(7) Uiso 1 1 d . . . O28 O -0.1555(7) 1.3604(6) 1.2076(6) 0.211(5) Uiso 1 1 d . . . O29 O -0.2871(3) 1.1739(2) 1.1951(2) 0.0623(13) Uani 1 1 d . . . O30 O -0.1657(7) -0.3605(7) 0.9574(6) 0.242(6) Uiso 1 1 d . . . O31 O 0.4112(8) 0.1466(7) 0.6891(7) 0.235(6) Uiso 1 1 d . A . O32 O 0.4917(7) 0.1507(6) 0.5989(6) 0.211(5) Uiso 1 1 d . A . O33 O 0.4002(7) 0.2259(7) 0.6305(7) 0.226(5) Uiso 1 1 d . A . N1 N 0.3523(4) 0.2802(3) 0.7702(3) 0.077(2) Uani 1 1 d . A . N2 N 0.7353(3) 1.1791(3) 0.3267(3) 0.0522(15) Uani 1 1 d . . . N3 N -0.1312(3) 1.1869(3) 1.2059(3) 0.074(2) Uani 1 1 d . . . N4 N 0.2368(5) 0.1642(3) 0.7017(4) 0.106(3) Uani 1 1 d . A . N5 N -0.2430(3) -0.6862(3) 1.1383(3) 0.0595(16) Uani 1 1 d . . . N6 N 0.6277(3) -0.6979(3) 0.2679(3) 0.0685(18) Uani 1 1 d . . . N8 N 0.2813(5) 0.1296(5) 0.8404(5) 0.115(3) Uiso 1 1 d . . . N9 N -0.2075(8) 1.3539(7) 1.2615(7) 0.177(5) Uiso 1 1 d . . . N10 N -0.2705(4) 1.0926(3) 1.1341(4) 0.091(2) Uani 1 1 d . . . N11 N -0.2217(7) -0.2622(6) 0.9996(6) 0.159(4) Uiso 1 1 d . . . N12 N 0.4304(10) 0.1716(9) 0.6409(9) 0.200(6) Uiso 1 1 d . . . C1 C 0.5275(3) 0.7287(2) 0.9791(3) 0.0307(13) Uani 1 1 d . . . C2 C 0.4634(3) 0.7104(3) 0.9997(3) 0.0376(14) Uani 1 1 d . . . H2 H 0.4305 0.7261 1.0354 0.045 Uiso 1 1 calc R . . C3 C 0.4479(3) 0.6705(3) 0.9690(3) 0.0420(16) Uani 1 1 d . . . C4 C 0.4963(4) 0.6496(3) 0.9136(3) 0.0496(18) Uani 1 1 d . . . C5 C 0.5593(3) 0.6690(3) 0.8916(3) 0.0393(15) Uani 1 1 d . . . H5 H 0.5910 0.6548 0.8548 0.047 Uiso 1 1 calc R . . C6 C 0.5758(3) 0.7090(2) 0.9235(3) 0.0352(14) Uani 1 1 d . . . C7 C 0.6451(3) 0.7279(3) 0.8980(3) 0.0345(14) Uani 1 1 d . . . H7A H 0.6591 0.7380 0.9323 0.041 Uiso 1 1 calc R . . H7B H 0.6819 0.6907 0.8811 0.041 Uiso 1 1 calc R . . C8 C 0.6435(3) 0.7839(3) 0.8490(3) 0.0370(14) Uani 1 1 d . . . C9 C 0.6548(3) 0.7723(3) 0.7869(3) 0.0425(15) Uani 1 1 d . . . H9 H 0.6601 0.7307 0.7781 0.051 Uiso 1 1 calc R . . C10 C 0.6582(3) 0.8213(3) 0.7387(3) 0.0402(15) Uani 1 1 d . . . C11 C 0.6496(3) 0.8827(3) 0.7510(3) 0.0407(15) Uani 1 1 d . . . C12 C 0.6362(3) 0.8965(3) 0.8118(3) 0.0399(15) Uani 1 1 d . . . H12 H 0.6299 0.9387 0.8196 0.048 Uiso 1 1 calc R . . C13 C 0.6320(3) 0.8473(3) 0.8620(3) 0.0379(14) Uani 1 1 d . . . C14 C 0.6193(3) 0.8657(3) 0.9277(3) 0.0399(15) Uani 1 1 d . . . H14A H 0.6435 0.8291 0.9527 0.048 Uiso 1 1 calc R . . H14B H 0.6400 0.9012 0.9253 0.048 Uiso 1 1 calc R . . C15 C 0.5398(3) 0.8856(3) 0.9595(3) 0.0328(13) Uani 1 1 d . . . C16 C 0.5017(3) 0.9507(3) 0.9466(3) 0.0357(14) Uani 1 1 d . . . H16 H 0.5250 0.9788 0.9183 0.043 Uiso 1 1 calc R . . C17 C 0.4297(3) 0.9727(3) 0.9758(3) 0.0395(15) Uani 1 1 d . . . C18 C 0.3970(3) 0.9316(3) 1.0168(3) 0.0403(15) Uani 1 1 d . . . C19 C 0.4324(3) 0.8683(3) 1.0296(3) 0.0388(15) Uani 1 1 d . . . H19 H 0.4079 0.8409 1.0576 0.047 Uiso 1 1 calc R . . C20 C 0.5036(3) 0.8446(3) 1.0018(3) 0.0323(13) Uani 1 1 d . . . C21 C 0.5398(3) 0.7726(3) 1.0185(3) 0.0380(15) Uani 1 1 d . . . H21A H 0.5910 0.7666 1.0121 0.046 Uiso 1 1 calc R . . H21B H 0.5208 0.7603 1.0622 0.046 Uiso 1 1 calc R . . C22 C 0.3405(4) 0.6657(4) 1.0435(4) 0.078(2) Uani 1 1 d . . . H22A H 0.3653 0.6493 1.0764 0.116 Uiso 1 1 calc R . . H22B H 0.3002 0.6480 1.0515 0.116 Uiso 1 1 calc R . . H22C H 0.3239 0.7121 1.0416 0.116 Uiso 1 1 calc R . . C23 C 0.5062(3) 0.5429(3) 0.9037(3) 0.0395(15) Uani 1 1 d . . . C24 C 0.4769(3) 0.5006(3) 0.8782(3) 0.0407(15) Uani 1 1 d . . . C25 C 0.4573(4) 0.5152(3) 0.8244(3) 0.064(2) Uani 1 1 d . . . H25 H 0.4595 0.5550 0.8016 0.077 Uiso 1 1 calc R . . C26 C 0.4334(4) 0.4722(4) 0.8012(4) 0.073(2) Uani 1 1 d . . . H26 H 0.4222 0.4828 0.7624 0.088 Uiso 1 1 calc R . . C27 C 0.4265(4) 0.4149(3) 0.8352(3) 0.060(2) Uani 1 1 d . . . C28 C 0.4470(4) 0.3996(3) 0.8919(3) 0.062(2) Uani 1 1 d . . . H28 H 0.4439 0.3605 0.9158 0.075 Uiso 1 1 calc R . . C29 C 0.4711(4) 0.4415(3) 0.9119(3) 0.0527(19) Uani 1 1 d . . . H29 H 0.4845 0.4306 0.9497 0.063 Uiso 1 1 calc R . . C30 C 0.4005(4) 0.3666(4) 0.8129(4) 0.069(2) Uani 1 1 d . . . C31 C 0.4157(5) 0.3605(4) 0.7495(4) 0.076(2) Uani 1 1 d . A . H31 H 0.4441 0.3840 0.7202 0.092 Uiso 1 1 calc R . . C32 C 0.3873(6) 0.3185(5) 0.7315(5) 0.108(4) Uani 1 1 d . . . H32 H 0.3936 0.3174 0.6890 0.130 Uiso 1 1 calc R A . C33 C 0.3407(4) 0.2858(4) 0.8295(4) 0.067(2) Uani 1 1 d . . . H33 H 0.3145 0.2599 0.8579 0.081 Uiso 1 1 calc R A . C34 C 0.3644(4) 0.3271(3) 0.8522(4) 0.060(2) Uani 1 1 d . A . H34 H 0.3555 0.3278 0.8951 0.072 Uiso 1 1 calc R . . C35 C 0.6781(4) 0.7499(4) 0.6630(3) 0.063(2) Uani 1 1 d . . . H35A H 0.7114 0.7178 0.6836 0.095 Uiso 1 1 calc R . . H35B H 0.6943 0.7478 0.6188 0.095 Uiso 1 1 calc R . . H35C H 0.6316 0.7418 0.6774 0.095 Uiso 1 1 calc R . . C36 C 0.7188(3) 0.9370(3) 0.6717(3) 0.0387(15) Uani 1 1 d . . . C37 C 0.7187(3) 0.9805(3) 0.6134(3) 0.0452(16) Uani 1 1 d . . . C38 C 0.6569(3) 1.0114(3) 0.5931(3) 0.0514(18) Uani 1 1 d . . . H38 H 0.6129 1.0061 0.6176 0.062 Uiso 1 1 calc R . . C39 C 0.6592(4) 1.0498(4) 0.5373(4) 0.065(2) Uani 1 1 d . . . H39 H 0.6170 1.0695 0.5239 0.078 Uiso 1 1 calc R . . C40 C 0.7242(3) 1.0593(3) 0.5007(3) 0.0510(18) Uani 1 1 d . . . C41 C 0.7864(3) 1.0277(3) 0.5214(3) 0.0541(18) Uani 1 1 d . . . H41 H 0.8307 1.0325 0.4972 0.065 Uiso 1 1 calc R . . C42 C 0.7829(3) 0.9893(3) 0.5777(3) 0.0429(16) Uani 1 1 d . . . H42 H 0.8247 0.9692 0.5915 0.052 Uiso 1 1 calc R . . C43 C 0.7273(4) 1.1004(3) 0.4400(3) 0.059(2) Uani 1 1 d . . . C44 C 0.6831(4) 1.1058(4) 0.4003(4) 0.068(2) Uani 1 1 d . . . H44 H 0.6487 1.0826 0.4115 0.082 Uiso 1 1 calc R . . C45 C 0.6896(4) 1.1453(4) 0.3439(3) 0.060(2) Uani 1 1 d . . . H45 H 0.6598 1.1472 0.3180 0.072 Uiso 1 1 calc R . . C46 C 0.7784(4) 1.1739(3) 0.3619(3) 0.058(2) Uani 1 1 d . . . H46 H 0.8123 1.1976 0.3485 0.069 Uiso 1 1 calc R . . C47 C 0.7775(4) 1.1354(4) 0.4182(3) 0.063(2) Uani 1 1 d . . . H47 H 0.8104 1.1332 0.4412 0.076 Uiso 1 1 calc R . . C48 C 0.4195(4) 1.0769(3) 0.9194(3) 0.0585(19) Uani 1 1 d . . . H48A H 0.4620 1.0818 0.9272 0.088 Uiso 1 1 calc R . . H48B H 0.3852 1.1185 0.9170 0.088 Uiso 1 1 calc R . . H48C H 0.4315 1.0587 0.8806 0.088 Uiso 1 1 calc R . . C49 C 0.3087(3) 0.9796(3) 1.1016(3) 0.0367(15) Uani 1 1 d . . . C50 C 0.2317(3) 1.0118(3) 1.1216(3) 0.0396(15) Uani 1 1 d . . . C51 C 0.1827(4) 1.0118(4) 1.0867(3) 0.0592(19) Uani 1 1 d . . . H51 H 0.1986 0.9910 1.0505 0.071 Uiso 1 1 calc R . . C52 C 0.1118(4) 1.0427(4) 1.1069(3) 0.063(2) Uani 1 1 d . . . H52 H 0.0790 1.0406 1.0856 0.075 Uiso 1 1 calc R . . C53 C 0.0875(3) 1.0774(3) 1.1589(3) 0.0474(17) Uani 1 1 d . . . C54 C 0.1345(3) 1.0758(3) 1.1940(3) 0.0478(17) Uani 1 1 d . . . H54 H 0.1185 1.0965 1.2301 0.057 Uiso 1 1 calc R . . C55 C 0.2076(3) 1.0419(3) 1.1741(3) 0.0440(16) Uani 1 1 d . . . H55 H 0.2397 1.0404 1.1976 0.053 Uiso 1 1 calc R . . C56 C 0.0106(3) 1.1135(3) 1.1762(3) 0.0468(17) Uani 1 1 d . . . C57 C -0.0437(4) 1.0941(4) 1.1674(4) 0.065(2) Uani 1 1 d . . . H57 H -0.0330 1.0548 1.1512 0.078 Uiso 1 1 calc R . . C58 C -0.1146(4) 1.1306(3) 1.1818(3) 0.0551(18) Uani 1 1 d . . . H58 H -0.1505 1.1161 1.1747 0.066 Uiso 1 1 calc R . . C59 C -0.0811(3) 1.2062(3) 1.2147(4) 0.067(2) Uani 1 1 d . . . H59 H -0.0932 1.2458 1.2306 0.080 Uiso 1 1 calc R . . C60 C -0.0072(4) 1.1701(3) 1.2015(4) 0.063(2) Uani 1 1 d . . . H60 H 0.0277 1.1850 1.2100 0.076 Uiso 1 1 calc R . . C61 C -0.0721(3) -0.2006(2) 0.5581(3) 0.0321(14) Uani 1 1 d . . . C62 C -0.0557(3) -0.1609(3) 0.5900(3) 0.0414(15) Uani 1 1 d . . . H62 H -0.0882 -0.1444 0.6256 0.050 Uiso 1 1 calc R . . C63 C 0.0096(4) -0.1457(3) 0.5688(3) 0.0460(17) Uani 1 1 d . . . C64 C 0.0586(3) -0.1683(3) 0.5159(3) 0.0424(16) Uani 1 1 d . . . C65 C 0.0415(3) -0.2063(3) 0.4851(3) 0.0396(15) Uani 1 1 d . . . H65 H 0.0741 -0.2223 0.4494 0.048 Uiso 1 1 calc R . . C66 C -0.0236(3) -0.2225(3) 0.5048(3) 0.0357(14) Uani 1 1 d . . . C67 C -0.0346(3) -0.2684(3) 0.4646(3) 0.0409(15) Uani 1 1 d . . . H67A H -0.0856 -0.2622 0.4691 0.049 Uiso 1 1 calc R . . H67B H -0.0132 -0.2580 0.4210 0.049 Uiso 1 1 calc R . . C68 C 0.0000(3) -0.3390(3) 0.4852(3) 0.0375(15) Uani 1 1 d . . . C69 C 0.0708(3) -0.3636(3) 0.4571(3) 0.0447(16) Uani 1 1 d . . . H69 H 0.0952 -0.3378 0.4266 0.054 Uiso 1 1 calc R . . C70 C 0.1058(3) -0.4268(3) 0.4740(3) 0.0499(17) Uani 1 1 d . . . C71 C 0.0720(4) -0.4652(3) 0.5175(3) 0.0462(16) Uani 1 1 d . . . C72 C 0.0004(3) -0.4408(3) 0.5449(3) 0.0422(15) Uani 1 1 d . . . H72 H -0.0234 -0.4676 0.5747 0.051 Uiso 1 1 calc R . . C73 C -0.0373(3) -0.3777(3) 0.5297(3) 0.0346(14) Uani 1 1 d . . . C74 C -0.1159(3) -0.3571(3) 0.5595(3) 0.0482(17) Uani 1 1 d . . . H74A H -0.1364 -0.3931 0.5636 0.058 Uiso 1 1 calc R . . H74B H -0.1394 -0.3220 0.5328 0.058 Uiso 1 1 calc R . . C75 C -0.1308(3) -0.3347(3) 0.6240(3) 0.0396(15) Uani 1 1 d . . . C76 C -0.1339(3) -0.3819(3) 0.6762(3) 0.0408(15) Uani 1 1 d . . . H76 H -0.1254 -0.4251 0.6703 0.049 Uiso 1 1 calc R . . C77 C -0.1490(3) -0.3652(3) 0.7343(3) 0.0442(16) Uani 1 1 d . . . C78 C -0.1607(3) -0.3020(3) 0.7457(3) 0.0411(15) Uani 1 1 d . . . C79 C -0.1576(3) -0.2547(3) 0.6954(3) 0.0402(15) Uani 1 1 d . . . H79 H -0.1651 -0.2119 0.7020 0.048 Uiso 1 1 calc R . . C80 C -0.1431(3) -0.2708(3) 0.6346(3) 0.0362(14) Uani 1 1 d . . . C81 C -0.1450(3) -0.2163(3) 0.5833(3) 0.0402(15) Uani 1 1 d . . . H81A H -0.1810 -0.1780 0.5988 0.048 Uiso 1 1 calc R . . H81B H -0.1589 -0.2277 0.5496 0.048 Uiso 1 1 calc R . . C82 C 0.1643(5) -0.1609(5) 0.4401(4) 0.095(3) Uani 1 1 d . . . H82A H 0.1798 -0.2071 0.4391 0.143 Uiso 1 1 calc R . . H82B H 0.2054 -0.1445 0.4332 0.143 Uiso 1 1 calc R . . H82C H 0.1388 -0.1413 0.4082 0.143 Uiso 1 1 calc R . . C83 C 0.0004(4) -0.0425(3) 0.5917(3) 0.0479(17) Uani 1 1 d . . . C84 C 0.0373(4) -0.0069(3) 0.6172(3) 0.0488(17) Uani 1 1 d . . . C85 C 0.0731(4) -0.0346(3) 0.6635(3) 0.059(2) Uani 1 1 d . . . H85 H 0.0717 -0.0760 0.6825 0.071 Uiso 1 1 calc R . . C86 C 0.1116(5) -0.0006(4) 0.6821(3) 0.074(2) Uani 1 1 d . . . H86 H 0.1368 -0.0198 0.7127 0.088 Uiso 1 1 calc R . . C87 C 0.1119(5) 0.0617(3) 0.6546(4) 0.070(2) Uani 1 1 d . . . C88 C 0.0731(5) 0.0895(4) 0.6102(4) 0.073(2) Uani 1 1 d . . . H88 H 0.0709 0.1321 0.5933 0.088 Uiso 1 1 calc R . . C89 C 0.0380(4) 0.0551(3) 0.5906(4) 0.066(2) Uani 1 1 d . . . H89 H 0.0143 0.0738 0.5589 0.080 Uiso 1 1 calc R . . C90 C 0.1543(5) 0.0969(4) 0.6707(4) 0.076(3) Uani 1 1 d . . . C91 C 0.2237(5) 0.0659(4) 0.6811(5) 0.095(3) Uani 1 1 d . A . H91 H 0.2451 0.0223 0.6760 0.114 Uiso 1 1 calc R . . C92 C 0.2587(7) 0.1032(5) 0.6993(5) 0.125(5) Uani 1 1 d . . . H92 H 0.3017 0.0816 0.7107 0.150 Uiso 1 1 calc R A . C93 C 0.1741(7) 0.1946(4) 0.6871(6) 0.124(5) Uani 1 1 d . . . H93 H 0.1581 0.2395 0.6859 0.148 Uiso 1 1 calc R A . C94 C 0.1320(7) 0.1613(4) 0.6736(7) 0.148(6) Uani 1 1 d . A . H94 H 0.0871 0.1841 0.6664 0.178 Uiso 1 1 calc R . . C95 C 0.0824(5) -0.5650(3) 0.5807(4) 0.069(2) Uani 1 1 d . . . H95A H 0.0641 -0.5407 0.6162 0.104 Uiso 1 1 calc R . . H95B H 0.1179 -0.6040 0.5898 0.104 Uiso 1 1 calc R . . H95C H 0.0438 -0.5759 0.5715 0.104 Uiso 1 1 calc R . . C96 C 0.1924(4) -0.4832(3) 0.3949(3) 0.0460(17) Uani 1 1 d . . . C97 C 0.2685(3) -0.5172(3) 0.3741(3) 0.0416(16) Uani 1 1 d . . . C98 C 0.3218(4) -0.5159(4) 0.4022(4) 0.069(2) Uani 1 1 d . . . H98 H 0.3101 -0.4912 0.4353 0.083 Uiso 1 1 calc R . . C99 C 0.3897(4) -0.5502(4) 0.3816(4) 0.069(2) Uani 1 1 d . . . H99 H 0.4243 -0.5486 0.4011 0.083 Uiso 1 1 calc R . . C100 C 0.4104(3) -0.5869(3) 0.3338(3) 0.0461(16) Uani 1 1 d . . . C101 C 0.3606(4) -0.5877(3) 0.3039(3) 0.061(2) Uani 1 1 d . . . H101 H 0.3738 -0.6118 0.2701 0.073 Uiso 1 1 calc R . . C102 C 0.2886(3) -0.5517(3) 0.3244(3) 0.0557(19) Uani 1 1 d . . . H102 H 0.2545 -0.5517 0.3036 0.067 Uiso 1 1 calc R . . C103 C 0.4862(3) -0.6252(3) 0.3125(3) 0.0497(18) Uani 1 1 d . . . C104 C 0.5430(4) -0.6104(4) 0.3242(3) 0.061(2) Uani 1 1 d . . . H104 H 0.5340 -0.5749 0.3456 0.073 Uiso 1 1 calc R . . C105 C 0.6137(4) -0.6474(4) 0.3047(3) 0.070(2) Uani 1 1 d . . . H105 H 0.6510 -0.6388 0.3159 0.084 Uiso 1 1 calc R . . C106 C 0.5753(4) -0.7104(3) 0.2576(4) 0.063(2) Uani 1 1 d . . . H106 H 0.5845 -0.7447 0.2344 0.076 Uiso 1 1 calc R . . C107 C 0.5054(4) -0.6765(3) 0.2783(4) 0.063(2) Uani 1 1 d . . . H107 H 0.4694 -0.6888 0.2688 0.076 Uiso 1 1 calc R . . C108 C -0.1807(4) -0.2270(3) 0.8166(3) 0.0513(17) Uani 1 1 d . . . H10A H -0.1382 -0.2156 0.7916 0.077 Uiso 1 1 calc R . . H10B H -0.1837 -0.2258 0.8598 0.077 Uiso 1 1 calc R . . H10C H -0.2222 -0.1968 0.8052 0.077 Uiso 1 1 calc R . . C109 C -0.2189(3) -0.4193(3) 0.8140(3) 0.0420(16) Uani 1 1 d . . . C110 C -0.2178(3) -0.4654(3) 0.8692(3) 0.0459(16) Uani 1 1 d . . . C111 C -0.2834(3) -0.4762(3) 0.9064(3) 0.0453(16) Uani 1 1 d . . . H111 H -0.3257 -0.4534 0.8944 0.054 Uiso 1 1 calc R . . C112 C -0.2872(3) -0.5173(3) 0.9575(3) 0.0559(19) Uani 1 1 d . . . H112 H -0.3316 -0.5234 0.9802 0.067 Uiso 1 1 calc R . . C113 C -0.2254(3) -0.5518(3) 0.9776(3) 0.0549(19) Uani 1 1 d . . . C114 C -0.1604(4) -0.5418(4) 0.9424(4) 0.072(3) Uani 1 1 d . . . H114 H -0.1183 -0.5651 0.9544 0.086 Uiso 1 1 calc R . . C115 C -0.1571(3) -0.4982(3) 0.8899(3) 0.0526(18) Uani 1 1 d . . . H115 H -0.1131 -0.4907 0.8680 0.063 Uiso 1 1 calc R . . C116 C -0.2294(3) -0.5986(3) 1.0334(3) 0.059(2) Uani 1 1 d . . . C117 C -0.1780(5) -0.6537(4) 1.0372(5) 0.100(3) Uani 1 1 d . . . H117 H -0.1379 -0.6637 1.0042 0.120 Uiso 1 1 calc R . . C118 C -0.1856(5) -0.6958(4) 1.0912(4) 0.093(3) Uani 1 1 d . . . H118 H -0.1483 -0.7329 1.0946 0.111 Uiso 1 1 calc R . . C119 C -0.2912(4) -0.6361(5) 1.1303(4) 0.089(3) Uani 1 1 d . . . H119 H -0.3333 -0.6293 1.1617 0.107 Uiso 1 1 calc R . . C120 C -0.2888(4) -0.5906(5) 1.0808(4) 0.093(3) Uani 1 1 d . . . H120 H -0.3275 -0.5542 1.0793 0.112 Uiso 1 1 calc R . . C121 C -0.2840(4) 1.1543(4) 1.1441(5) 0.072(2) Uani 1 1 d . . . C122 C -0.2901(7) 1.1922(5) 1.0825(5) 0.118(4) Uani 1 1 d . . . H12A H -0.3302 1.2307 1.0881 0.141 Uiso 1 1 calc R . . H12B H -0.2465 1.2056 1.0627 0.141 Uiso 1 1 calc R . . C123 C -0.3014(10) 1.1500(6) 1.0431(7) 0.190(8) Uani 1 1 d . . . H12C H -0.2741 1.1557 1.0004 0.228 Uiso 1 1 calc R . . H12D H -0.3518 1.1598 1.0432 0.228 Uiso 1 1 calc R . . C124 C -0.2749(8) 1.0807(6) 1.0728(6) 0.157(6) Uani 1 1 d . . . H12E H -0.3087 1.0556 1.0771 0.188 Uiso 1 1 calc R . . H12F H -0.2283 1.0586 1.0488 0.188 Uiso 1 1 calc R . . C125 C -0.2548(7) 1.0402(5) 1.1854(6) 0.141(5) Uani 1 1 d . . . H12G H -0.2040 1.0204 1.1777 0.212 Uiso 1 1 calc R . . H12H H -0.2792 1.0081 1.1869 0.212 Uiso 1 1 calc R . . H12I H -0.2710 1.0584 1.2244 0.212 Uiso 1 1 calc R . . C126 C -0.1673(7) -0.2930(6) 0.9719(5) 0.110(3) Uiso 1 1 d . . . C127 C -0.0976(7) -0.2849(6) 0.9525(6) 0.147(5) Uiso 1 1 d . . . H12J H -0.0773 -0.2871 0.9082 0.177 Uiso 1 1 calc R . . H12K H -0.0649 -0.3143 0.9762 0.177 Uiso 1 1 calc R . . C128 C -0.1214(11) -0.2196(9) 0.9699(9) 0.227(8) Uiso 1 1 d . . . H12L H -0.0915 -0.2160 0.9958 0.273 Uiso 1 1 calc R . . H12M H -0.1132 -0.1902 0.9323 0.273 Uiso 1 1 calc R . . C129 C -0.1903(7) -0.1996(6) 1.0004(6) 0.145(5) Uiso 1 1 d . . . H12N H -0.2153 -0.1604 0.9790 0.174 Uiso 1 1 calc R . . H12O H -0.1944 -0.1920 1.0427 0.174 Uiso 1 1 calc R . . C130 C -0.2819(4) -0.2605(3) 1.0186(3) 0.0492(17) Uiso 1 1 d . . . H13A H -0.2866 -0.3037 1.0325 0.074 Uiso 1 1 calc R . . H13B H -0.3069 -0.2419 0.9861 0.074 Uiso 1 1 calc R . . H13C H -0.3020 -0.2346 1.0529 0.074 Uiso 1 1 calc R . . O22 O 0.1689(7) 0.3890(6) 0.6989(6) 0.205(5) Uiso 1 1 d . A 2 N7 N 0.1962(6) 0.3219(6) 0.7331(6) 0.156(4) Uiso 1 1 d . A 2 O20 O 0.2534(4) 0.3191(4) 0.6719(4) 0.124(2) Uiso 1 1 d . A 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 Cd1 0.1142(6) 0.0756(5) 0.1065(6) -0.0096(4) -0.0566(5) -0.0471(4) Cd2 0.0363(3) 0.0383(3) 0.0642(4) 0.0051(2) -0.0014(2) -0.0062(2) O1 0.055(3) 0.040(3) 0.092(4) -0.012(3) -0.013(3) -0.025(2) O2 0.064(3) 0.043(3) 0.057(3) 0.011(2) -0.038(2) -0.029(2) O3 0.051(3) 0.035(2) 0.071(3) -0.004(2) -0.034(3) -0.019(2) O4 0.052(3) 0.058(3) 0.037(2) -0.011(2) -0.002(2) -0.022(2) O5 0.038(2) 0.050(3) 0.037(2) -0.005(2) 0.000(2) -0.013(2) O6 0.045(3) 0.047(3) 0.045(3) -0.006(2) -0.006(2) -0.017(2) O7 0.053(3) 0.035(2) 0.066(3) -0.015(2) -0.020(2) -0.005(2) O8 0.028(2) 0.054(3) 0.060(3) -0.027(2) -0.007(2) -0.012(2) O9 0.035(2) 0.049(3) 0.054(3) -0.020(2) -0.011(2) -0.013(2) O10 0.050(3) 0.062(3) 0.077(3) -0.014(3) -0.011(3) -0.034(3) O11 0.063(3) 0.043(3) 0.060(3) 0.004(2) -0.034(2) -0.027(2) O12 0.076(4) 0.047(3) 0.118(5) -0.007(3) -0.061(4) -0.021(3) O13 0.045(3) 0.052(3) 0.050(3) -0.018(2) -0.007(2) -0.015(2) O14 0.035(2) 0.044(2) 0.051(3) -0.003(2) -0.005(2) -0.014(2) O15 0.039(2) 0.038(2) 0.050(3) -0.009(2) -0.004(2) -0.014(2) O16 0.067(3) 0.042(3) 0.078(4) -0.026(3) -0.020(3) 0.000(3) O17 0.033(2) 0.070(3) 0.076(3) -0.044(3) -0.009(2) -0.004(2) O18 0.042(3) 0.057(3) 0.066(3) -0.031(3) 0.003(2) -0.016(2) O29 0.065(3) 0.066(3) 0.049(3) -0.015(3) -0.003(3) -0.013(3) N1 0.112(6) 0.081(5) 0.065(5) -0.002(4) -0.032(4) -0.059(5) N2 0.033(3) 0.060(4) 0.063(4) 0.006(3) -0.007(3) -0.023(3) N3 0.034(3) 0.058(4) 0.104(5) 0.027(4) -0.003(3) -0.008(3) N4 0.146(8) 0.058(5) 0.169(8) 0.007(5) -0.108(7) -0.054(5) N5 0.054(4) 0.054(4) 0.054(4) 0.006(3) 0.004(3) -0.012(3) N6 0.060(4) 0.058(4) 0.069(4) -0.007(4) 0.004(4) -0.007(3) N10 0.104(6) 0.072(5) 0.107(6) -0.009(5) -0.035(5) -0.029(4) C1 0.040(3) 0.020(3) 0.039(3) 0.001(3) -0.017(3) -0.014(3) C2 0.036(3) 0.029(3) 0.043(4) -0.005(3) -0.004(3) -0.007(3) C3 0.043(4) 0.021(3) 0.068(5) 0.006(3) -0.021(4) -0.018(3) C4 0.068(5) 0.021(3) 0.073(5) 0.006(3) -0.037(4) -0.019(3) C5 0.047(4) 0.031(3) 0.035(3) -0.001(3) -0.006(3) -0.008(3) C6 0.043(4) 0.024(3) 0.049(4) 0.001(3) -0.024(3) -0.014(3) C7 0.042(3) 0.031(3) 0.035(3) -0.006(3) -0.010(3) -0.015(3) C8 0.032(3) 0.038(3) 0.047(4) -0.016(3) -0.004(3) -0.016(3) C9 0.040(4) 0.042(4) 0.050(4) -0.013(3) -0.008(3) -0.016(3) C10 0.028(3) 0.056(4) 0.036(4) -0.015(3) 0.000(3) -0.011(3) C11 0.044(4) 0.037(4) 0.037(4) -0.009(3) -0.001(3) -0.012(3) C12 0.039(4) 0.032(3) 0.046(4) -0.005(3) -0.007(3) -0.009(3) C13 0.031(3) 0.037(3) 0.041(4) -0.007(3) 0.000(3) -0.009(3) C14 0.050(4) 0.030(3) 0.040(4) -0.016(3) 0.006(3) -0.019(3) C15 0.036(3) 0.035(3) 0.033(3) -0.013(3) -0.004(3) -0.018(3) C16 0.043(4) 0.040(3) 0.029(3) -0.011(3) -0.008(3) -0.014(3) C17 0.044(4) 0.035(3) 0.047(4) -0.020(3) -0.021(3) -0.002(3) C18 0.031(3) 0.050(4) 0.046(4) -0.024(3) -0.002(3) -0.015(3) C19 0.050(4) 0.038(4) 0.042(4) -0.020(3) -0.007(3) -0.024(3) C20 0.041(4) 0.025(3) 0.034(3) -0.014(3) -0.007(3) -0.009(3) C21 0.035(3) 0.030(3) 0.051(4) -0.002(3) -0.004(3) -0.017(3) C22 0.058(5) 0.083(6) 0.101(7) -0.012(5) -0.003(5) -0.046(5) C23 0.051(4) 0.024(3) 0.047(4) -0.004(3) -0.007(3) -0.020(3) C24 0.048(4) 0.046(4) 0.045(4) -0.001(3) -0.028(3) -0.023(3) C25 0.103(6) 0.058(5) 0.054(5) 0.023(4) -0.037(5) -0.054(5) C26 0.102(7) 0.087(6) 0.060(5) 0.005(5) -0.039(5) -0.057(5) C27 0.103(6) 0.051(4) 0.050(4) 0.009(4) -0.030(4) -0.055(4) C28 0.102(6) 0.052(4) 0.057(5) 0.014(4) -0.040(5) -0.049(4) C29 0.087(5) 0.037(4) 0.053(4) 0.009(3) -0.040(4) -0.032(4) C30 0.084(6) 0.084(6) 0.064(5) 0.012(5) -0.044(5) -0.045(5) C31 0.107(7) 0.067(5) 0.077(6) 0.004(5) -0.037(5) -0.049(5) C32 0.156(10) 0.108(8) 0.109(8) -0.008(7) -0.051(7) -0.088(8) C33 0.086(6) 0.072(5) 0.068(5) -0.004(4) -0.033(5) -0.046(5) C34 0.086(6) 0.047(4) 0.069(5) -0.003(4) -0.042(5) -0.031(4) C35 0.057(5) 0.082(5) 0.059(5) -0.045(4) 0.010(4) -0.031(4) C36 0.047(4) 0.036(3) 0.038(4) -0.012(3) -0.007(3) -0.016(3) C37 0.036(4) 0.045(4) 0.056(4) -0.003(3) -0.008(3) -0.019(3) C38 0.040(4) 0.059(4) 0.047(4) 0.003(4) 0.002(3) -0.016(3) C39 0.035(4) 0.075(5) 0.074(5) 0.016(4) -0.011(4) -0.015(4) C40 0.039(4) 0.060(4) 0.057(4) 0.005(4) -0.008(3) -0.027(3) C41 0.037(4) 0.064(5) 0.064(5) -0.009(4) -0.005(4) -0.023(4) C42 0.034(3) 0.052(4) 0.049(4) 0.008(3) -0.016(3) -0.023(3) C43 0.047(4) 0.060(5) 0.074(5) 0.015(4) -0.020(4) -0.029(4) C44 0.061(5) 0.083(6) 0.072(5) 0.014(5) -0.018(4) -0.046(4) C45 0.065(5) 0.074(5) 0.051(4) 0.002(4) -0.018(4) -0.034(4) C46 0.077(5) 0.074(5) 0.044(4) 0.010(4) -0.021(4) -0.054(4) C47 0.060(5) 0.082(5) 0.056(5) 0.022(4) -0.026(4) -0.035(4) C48 0.066(5) 0.052(4) 0.066(5) -0.004(4) -0.036(4) -0.013(4) C49 0.049(4) 0.022(3) 0.039(4) -0.012(3) -0.002(3) -0.012(3) C50 0.036(4) 0.039(3) 0.043(4) -0.011(3) -0.005(3) -0.009(3) C51 0.039(4) 0.078(5) 0.062(5) -0.028(4) -0.011(4) -0.006(4) C52 0.044(4) 0.088(6) 0.058(5) -0.030(4) -0.008(4) -0.012(4) C53 0.034(4) 0.050(4) 0.052(4) -0.011(4) -0.002(3) -0.006(3) C54 0.033(4) 0.056(4) 0.059(4) -0.022(4) -0.001(3) -0.019(3) C55 0.036(4) 0.042(4) 0.058(4) -0.018(3) -0.010(3) -0.009(3) C56 0.038(4) 0.048(4) 0.044(4) -0.005(3) -0.005(3) 0.001(3) C57 0.048(5) 0.064(5) 0.082(6) -0.024(4) -0.015(4) -0.007(4) C58 0.046(4) 0.048(4) 0.072(5) -0.016(4) -0.021(4) -0.001(3) C59 0.029(4) 0.036(4) 0.129(7) -0.025(4) 0.011(4) -0.014(3) C60 0.043(4) 0.052(4) 0.104(6) -0.025(4) -0.010(4) -0.024(4) C61 0.032(3) 0.025(3) 0.047(4) -0.003(3) -0.019(3) -0.011(3) C62 0.043(4) 0.036(3) 0.049(4) -0.008(3) -0.005(3) -0.019(3) C63 0.056(4) 0.036(4) 0.054(4) 0.003(3) -0.019(4) -0.023(3) C64 0.044(4) 0.041(4) 0.055(4) 0.007(3) -0.019(4) -0.028(3) C65 0.043(4) 0.035(3) 0.044(4) -0.008(3) -0.002(3) -0.019(3) C66 0.046(4) 0.032(3) 0.041(4) -0.006(3) -0.017(3) -0.021(3) C67 0.049(4) 0.037(3) 0.044(4) -0.013(3) -0.008(3) -0.020(3) C68 0.042(4) 0.036(3) 0.041(4) -0.023(3) -0.006(3) -0.012(3) C69 0.039(4) 0.052(4) 0.052(4) -0.025(3) 0.003(3) -0.027(3) C70 0.037(4) 0.051(4) 0.062(5) -0.032(4) -0.001(3) -0.008(3) C71 0.050(4) 0.040(4) 0.053(4) -0.023(3) -0.007(4) -0.012(3) C72 0.057(4) 0.040(4) 0.035(3) -0.016(3) -0.005(3) -0.018(3) C73 0.036(3) 0.031(3) 0.045(4) -0.010(3) -0.013(3) -0.014(3) C74 0.052(4) 0.031(3) 0.054(4) -0.007(3) 0.004(3) -0.014(3) C75 0.030(3) 0.045(4) 0.048(4) -0.023(3) 0.000(3) -0.015(3) C76 0.033(3) 0.032(3) 0.056(4) -0.002(3) -0.005(3) -0.013(3) C77 0.036(4) 0.038(4) 0.055(4) -0.015(3) -0.006(3) -0.005(3) C78 0.035(3) 0.042(4) 0.044(4) -0.001(3) -0.005(3) -0.013(3) C79 0.033(3) 0.036(3) 0.060(4) -0.014(3) -0.007(3) -0.019(3) C80 0.025(3) 0.032(3) 0.054(4) -0.011(3) -0.006(3) -0.011(3) C81 0.041(4) 0.037(3) 0.046(4) -0.012(3) -0.008(3) -0.012(3) C82 0.069(6) 0.130(8) 0.104(7) -0.038(7) 0.013(5) -0.068(6) C83 0.060(5) 0.035(4) 0.058(4) -0.012(3) -0.012(4) -0.025(3) C84 0.059(4) 0.045(4) 0.061(4) 0.000(3) -0.037(4) -0.022(3) C85 0.091(6) 0.054(4) 0.053(4) 0.002(4) -0.022(4) -0.047(4) C86 0.119(7) 0.069(5) 0.064(5) 0.017(4) -0.059(5) -0.052(5) C87 0.107(7) 0.053(5) 0.076(5) 0.010(4) -0.054(5) -0.038(5) C88 0.116(7) 0.054(5) 0.078(6) 0.013(4) -0.057(6) -0.045(5) C89 0.081(6) 0.056(5) 0.090(6) 0.012(4) -0.059(5) -0.036(4) C90 0.125(8) 0.058(5) 0.082(6) 0.013(4) -0.056(6) -0.060(5) C91 0.111(8) 0.066(5) 0.132(9) -0.002(6) -0.066(7) -0.028(5) C92 0.195(12) 0.077(7) 0.174(11) 0.010(7) -0.151(10) -0.054(7) C93 0.170(11) 0.057(6) 0.203(12) -0.008(7) -0.124(11) -0.048(7) C94 0.179(12) 0.061(6) 0.281(17) -0.016(8) -0.188(13) -0.023(7) C95 0.102(6) 0.044(4) 0.074(6) -0.018(4) -0.050(5) -0.003(4) C96 0.043(4) 0.032(3) 0.059(4) -0.016(3) 0.004(4) -0.012(3) C97 0.047(4) 0.036(3) 0.037(4) -0.017(3) 0.008(3) -0.013(3) C98 0.048(5) 0.076(5) 0.087(6) -0.035(5) -0.017(4) -0.005(4) C99 0.057(5) 0.081(5) 0.075(5) -0.045(5) -0.014(4) -0.004(4) C100 0.031(4) 0.047(4) 0.059(4) -0.006(4) -0.009(3) -0.012(3) C101 0.046(4) 0.066(5) 0.069(5) -0.042(4) 0.014(4) -0.016(4) C102 0.037(4) 0.058(4) 0.073(5) -0.017(4) -0.004(4) -0.017(3) C103 0.041(4) 0.039(4) 0.046(4) 0.009(3) 0.006(3) 0.001(3) C104 0.045(4) 0.065(5) 0.067(5) -0.021(4) -0.009(4) -0.001(4) C105 0.050(5) 0.106(7) 0.059(5) -0.022(5) -0.007(4) -0.025(5) C106 0.057(5) 0.040(4) 0.084(6) -0.025(4) 0.019(4) -0.022(4) C107 0.042(4) 0.050(4) 0.090(6) -0.010(4) -0.002(4) -0.011(4) C108 0.051(4) 0.059(4) 0.050(4) -0.019(4) -0.007(3) -0.019(4) C109 0.042(4) 0.040(4) 0.048(4) -0.023(3) 0.000(3) -0.015(3) C110 0.045(4) 0.035(3) 0.059(4) -0.003(3) -0.007(3) -0.017(3) C111 0.034(4) 0.044(4) 0.062(4) -0.002(4) -0.017(3) -0.014(3) C112 0.035(4) 0.053(4) 0.078(5) -0.001(4) -0.005(4) -0.021(3) C113 0.041(4) 0.046(4) 0.074(5) 0.001(4) -0.007(4) -0.016(3) C114 0.034(4) 0.082(6) 0.085(6) 0.037(5) -0.013(4) -0.020(4) C115 0.034(4) 0.054(4) 0.067(5) 0.005(4) -0.008(3) -0.017(3) C116 0.037(4) 0.056(5) 0.073(5) 0.015(4) -0.003(4) -0.019(4) C117 0.074(6) 0.088(7) 0.094(7) 0.024(6) 0.012(5) -0.006(5) C118 0.094(7) 0.076(6) 0.068(6) 0.019(5) 0.001(5) 0.001(5) C119 0.043(5) 0.115(8) 0.083(6) 0.044(6) -0.006(4) -0.025(5) C120 0.047(5) 0.147(9) 0.064(5) 0.037(6) -0.013(4) -0.021(5) C121 0.065(5) 0.054(5) 0.108(8) -0.002(5) -0.032(5) -0.026(4) C122 0.173(11) 0.093(7) 0.105(8) -0.005(7) -0.068(8) -0.033(8) C123 0.36(2) 0.095(9) 0.156(12) -0.031(9) -0.137(15) -0.036(12) C124 0.225(16) 0.142(12) 0.123(10) -0.059(9) -0.079(11) -0.017(11) C125 0.191(13) 0.083(7) 0.184(13) 0.053(8) -0.106(11) -0.069(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O21 2.301(5) . ? Cd1 N1 2.335(6) . ? Cd1 O31 2.350(15) . ? Cd1 N4 2.368(6) . ? Cd1 O23 2.465(6) . ? Cd1 O24 2.513(7) . ? Cd1 O20 2.523(8) . ? Cd1 O33 2.619(14) . ? Cd2 O29 2.330(5) . ? Cd2 N6 2.388(6) 1_476 ? Cd2 N5 2.388(6) 1_575 ? Cd2 N3 2.393(6) . ? Cd2 N2 2.395(5) 1_456 ? Cd2 O26 2.395(6) . ? O1 C3 1.400(7) . ? O1 C22 1.452(9) . ? O2 C23 1.378(7) . ? O2 C4 1.437(7) . ? O3 C23 1.208(7) . ? O4 C10 1.406(7) . ? O4 C35 1.453(8) . ? O5 C36 1.371(7) . ? O5 C11 1.412(7) . ? O6 C36 1.235(7) . ? O7 C17 1.405(7) . ? O7 C48 1.418(8) . ? O8 C49 1.398(7) . ? O8 C18 1.448(7) . ? O9 C49 1.204(7) . ? O10 C64 1.402(7) . ? O10 C82 1.417(10) . ? O11 C83 1.377(8) . ? O11 C63 1.452(7) . ? O12 C83 1.220(8) . ? O13 C78 1.393(8) . ? O13 C108 1.459(7) . ? O14 C109 1.376(7) . ? O14 C77 1.414(7) . ? O15 C109 1.236(7) . ? O16 C95 1.407(9) . ? O16 C71 1.427(8) . ? O17 C96 1.380(8) . ? O17 C70 1.455(7) . ? O18 C96 1.228(8) . ? O21 N7 1.063(12) . ? O23 N8 1.213(10) . ? O24 N8 1.290(10) . ? O25 N8 1.306(10) . ? O26 N9 1.060(14) . ? O27 N9 1.411(18) . ? O28 N9 1.408(16) . ? O29 C121 1.300(10) . ? O30 C126 1.583(16) . ? O31 N12 1.164(18) . ? O32 N12 1.365(18) . ? O33 N12 1.194(18) . ? N1 C32 1.331(11) . ? N1 C33 1.334(10) . ? N2 C45 1.308(8) . ? N2 C46 1.324(8) . ? N2 Cd2 2.394(5) 1_654 ? N3 C59 1.303(9) . ? N3 C58 1.369(9) . ? N4 C92 1.298(11) . ? N4 C93 1.363(12) . ? N5 C119 1.270(10) . ? N5 C118 1.350(10) . ? N5 Cd2 2.388(6) 1_535 ? N6 C106 1.278(9) . ? N6 C105 1.438(10) . ? N6 Cd2 2.388(6) 1_634 ? N10 C121 1.363(10) . ? N10 C124 1.506(13) . ? N10 C125 1.528(12) . ? N11 C130 1.181(13) . ? N11 C126 1.191(14) . ? N11 C129 1.706(16) . ? C1 C2 1.425(8) . ? C1 C6 1.427(8) . ? C1 C21 1.557(8) . ? C2 C3 1.379(8) . ? C2 H2 0.9500 . ? C3 C4 1.433(10) . ? C4 C5 1.417(9) . ? C5 C6 1.414(8) . ? C5 H5 0.9500 . ? C6 C7 1.532(8) . ? C7 C8 1.518(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C13 1.429(8) . ? C8 C9 1.435(8) . ? C9 C10 1.407(8) . ? C9 H9 0.9500 . ? C10 C11 1.392(8) . ? C11 C12 1.417(9) . ? C12 C13 1.440(8) . ? C12 H12 0.9500 . ? C13 C14 1.566(8) . ? C14 C15 1.552(8) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.419(8) . ? C15 C16 1.443(8) . ? C16 C17 1.415(8) . ? C16 H16 0.9500 . ? C17 C18 1.372(8) . ? C18 C19 1.393(9) . ? C19 C20 1.399(8) . ? C19 H19 0.9500 . ? C20 C21 1.575(8) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.525(8) . ? C24 C25 1.354(9) . ? C24 C29 1.419(8) . ? C25 C26 1.432(10) . ? C25 H25 0.9500 . ? C26 C27 1.394(9) . ? C26 H26 0.9500 . ? C27 C28 1.426(9) . ? C27 C30 1.546(10) . ? C28 C29 1.373(9) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C34 1.368(10) . ? C30 C31 1.424(11) . ? C31 C32 1.409(11) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.391(9) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.501(9) . ? C37 C42 1.395(8) . ? C37 C38 1.407(9) . ? C38 C39 1.401(9) . ? C38 H38 0.9500 . ? C39 C40 1.421(9) . ? C39 H39 0.9500 . ? C40 C41 1.422(9) . ? C40 C43 1.516(9) . ? C41 C42 1.409(9) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C47 1.404(9) . ? C43 C44 1.421(10) . ? C44 C45 1.423(10) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.412(9) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.501(9) . ? C50 C55 1.380(9) . ? C50 C51 1.449(9) . ? C51 C52 1.392(9) . ? C51 H51 0.9500 . ? C52 C53 1.429(10) . ? C52 H52 0.9500 . ? C53 C54 1.406(9) . ? C53 C56 1.513(9) . ? C54 C55 1.445(8) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C56 C57 1.385(9) . ? C56 C60 1.387(9) . ? C57 C58 1.414(10) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C59 C60 1.460(9) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C66 1.402(8) . ? C61 C62 1.408(8) . ? C61 C81 1.567(8) . ? C62 C63 1.414(9) . ? C62 H62 0.9500 . ? C63 C64 1.404(9) . ? C64 C65 1.366(8) . ? C65 C66 1.421(8) . ? C65 H65 0.9500 . ? C66 C67 1.594(8) . ? C67 C68 1.559(8) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 C69 1.398(8) . ? C68 C73 1.420(8) . ? C69 C70 1.410(9) . ? C69 H69 0.9500 . ? C70 C71 1.368(9) . ? C71 C72 1.405(9) . ? C72 C73 1.417(8) . ? C72 H72 0.9500 . ? C73 C74 1.527(8) . ? C74 C75 1.564(9) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C80 1.419(8) . ? C75 C76 1.442(8) . ? C76 C77 1.374(9) . ? C76 H76 0.9500 . ? C77 C78 1.412(9) . ? C78 C79 1.415(8) . ? C79 C80 1.432(9) . ? C79 H79 0.9500 . ? C80 C81 1.527(8) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 C84 1.523(9) . ? C84 C85 1.401(9) . ? C84 C89 1.405(9) . ? C85 C86 1.428(9) . ? C85 H85 0.9500 . ? C86 C87 1.415(10) . ? C86 H86 0.9500 . ? C87 C88 1.406(10) . ? C87 C90 1.485(10) . ? C88 C89 1.391(9) . ? C88 H88 0.9500 . ? C89 H89 0.9500 . ? C90 C94 1.372(12) . ? C90 C91 1.447(12) . ? C91 C92 1.424(12) . ? C91 H91 0.9500 . ? C92 H92 0.9500 . ? C93 C94 1.418(12) . ? C93 H93 0.9500 . ? C94 H94 0.9500 . ? C95 H95A 0.9800 . ? C95 H95B 0.9800 . ? C95 H95C 0.9800 . ? C96 C97 1.497(9) . ? C97 C102 1.388(9) . ? C97 C98 1.423(10) . ? C98 C99 1.367(10) . ? C98 H98 0.9500 . ? C99 C100 1.380(10) . ? C99 H99 0.9500 . ? C100 C101 1.384(9) . ? C100 C103 1.522(9) . ? C101 C102 1.443(9) . ? C101 H101 0.9500 . ? C102 H102 0.9500 . ? C103 C107 1.395(10) . ? C103 C104 1.405(10) . ? C104 C105 1.425(10) . ? C104 H104 0.9500 . ? C105 H105 0.9500 . ? C106 C107 1.397(10) . ? C106 H106 0.9500 . ? C107 H107 0.9500 . ? C108 H10A 0.9800 . ? C108 H10B 0.9800 . ? C108 H10C 0.9800 . ? C109 C110 1.477(9) . ? C110 C115 1.401(9) . ? C110 C111 1.443(9) . ? C111 C112 1.348(9) . ? C111 H111 0.9500 . ? C112 C113 1.421(9) . ? C112 H112 0.9500 . ? C113 C114 1.413(9) . ? C113 C116 1.494(9) . ? C114 C115 1.402(9) . ? C114 H114 0.9500 . ? C115 H115 0.9500 . ? C116 C117 1.361(11) . ? C116 C120 1.380(10) . ? C117 C118 1.413(11) . ? C117 H117 0.9500 . ? C118 H118 0.9500 . ? C119 C120 1.378(11) . ? C119 H119 0.9500 . ? C120 H120 0.9500 . ? C121 C122 1.523(12) . ? C122 C123 1.519(14) . ? C122 H12A 0.9900 . ? C122 H12B 0.9900 . ? C123 C124 1.565(16) . ? C123 H12C 0.9900 . ? C123 H12D 0.9900 . ? C124 H12E 0.9900 . ? C124 H12F 0.9900 . ? C125 H12G 0.9800 . ? C125 H12H 0.9800 . ? C125 H12I 0.9800 . ? C126 C127 1.434(15) . ? C127 C128 1.48(2) . ? C127 H12J 0.9900 . ? C127 H12K 0.9900 . ? C128 C129 1.37(2) . ? C128 H12L 0.9900 . ? C128 H12M 0.9900 . ? C129 H12N 0.9900 . ? C129 H12O 0.9900 . ? C130 H13A 0.9800 . ? C130 H13B 0.9800 . ? C130 H13C 0.9800 . ? O22 N7 1.571(15) . ? N7 O20 1.557(13) . ? 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 O21 Cd1 N1 85.0(2) . . ? O21 Cd1 O31 177.5(4) . . ? N1 Cd1 O31 97.0(4) . . ? O21 Cd1 N4 85.3(3) . . ? N1 Cd1 N4 170.2(3) . . ? O31 Cd1 N4 92.7(4) . . ? O21 Cd1 O23 65.65(19) . . ? N1 Cd1 O23 88.9(2) . . ? O31 Cd1 O23 115.8(4) . . ? N4 Cd1 O23 86.2(3) . . ? O21 Cd1 O24 115.9(2) . . ? N1 Cd1 O24 99.4(2) . . ? O31 Cd1 O24 65.3(4) . . ? N4 Cd1 O24 84.0(3) . . ? O23 Cd1 O24 50.7(2) . . ? O21 Cd1 O20 57.6(2) . . ? N1 Cd1 O20 84.6(2) . . ? O31 Cd1 O20 121.0(4) . . ? N4 Cd1 O20 91.0(3) . . ? O23 Cd1 O20 123.2(2) . . ? O24 Cd1 O20 172.2(3) . . ? O21 Cd1 O33 131.6(4) . . ? N1 Cd1 O33 86.7(4) . . ? O31 Cd1 O33 47.3(5) . . ? N4 Cd1 O33 100.5(4) . . ? O23 Cd1 O33 161.6(4) . . ? O24 Cd1 O33 112.5(4) . . ? O20 Cd1 O33 74.1(4) . . ? O29 Cd2 N6 89.5(2) . 1_476 ? O29 Cd2 N5 93.23(19) . 1_575 ? N6 Cd2 N5 91.5(2) 1_476 1_575 ? O29 Cd2 N3 91.3(2) . . ? N6 Cd2 N3 175.1(2) 1_476 . ? N5 Cd2 N3 93.3(2) 1_575 . ? O29 Cd2 N2 85.26(19) . 1_456 ? N6 Cd2 N2 86.9(2) 1_476 1_456 ? N5 Cd2 N2 177.8(2) 1_575 1_456 ? N3 Cd2 N2 88.26(19) . 1_456 ? O29 Cd2 O26 171.12(18) . . ? N6 Cd2 O26 89.8(2) 1_476 . ? N5 Cd2 O26 95.6(2) 1_575 . ? N3 Cd2 O26 88.6(2) . . ? N2 Cd2 O26 85.9(2) 1_456 . ? C3 O1 C22 114.8(5) . . ? C23 O2 C4 114.2(4) . . ? C10 O4 C35 116.6(5) . . ? C36 O5 C11 116.3(5) . . ? C17 O7 C48 118.0(5) . . ? C49 O8 C18 116.0(4) . . ? C64 O10 C82 116.9(5) . . ? C83 O11 C63 115.1(5) . . ? C78 O13 C108 115.1(5) . . ? C109 O14 C77 116.6(5) . . ? C95 O16 C71 116.3(6) . . ? C96 O17 C70 115.0(5) . . ? N7 O21 Cd1 99.2(7) . . ? N8 O23 Cd1 97.5(6) . . ? N8 O24 Cd1 93.1(6) . . ? N9 O26 Cd2 117.1(9) . . ? C121 O29 Cd2 141.1(5) . . ? N12 O31 Cd1 104.8(15) . . ? N12 O33 Cd1 89.9(14) . . ? C32 N1 C33 116.4(7) . . ? C32 N1 Cd1 119.3(6) . . ? C33 N1 Cd1 123.9(5) . . ? C45 N2 C46 118.4(6) . . ? C45 N2 Cd2 123.4(5) . 1_654 ? C46 N2 Cd2 118.1(4) . 1_654 ? C59 N3 C58 119.2(6) . . ? C59 N3 Cd2 121.5(5) . . ? C58 N3 Cd2 119.3(5) . . ? C92 N4 C93 117.0(7) . . ? C92 N4 Cd1 120.0(6) . . ? C93 N4 Cd1 123.0(6) . . ? C119 N5 C118 114.7(7) . . ? C119 N5 Cd2 121.7(5) . 1_535 ? C118 N5 Cd2 123.5(5) . 1_535 ? C106 N6 C105 118.1(6) . . ? C106 N6 Cd2 125.2(5) . 1_634 ? C105 N6 Cd2 116.7(5) . 1_634 ? O23 N8 O24 116.7(10) . . ? O23 N8 O25 122.7(10) . . ? O24 N8 O25 120.5(9) . . ? O26 N9 O28 127.0(16) . . ? O26 N9 O27 125.6(16) . . ? O28 N9 O27 101.2(14) . . ? C121 N10 C124 117.0(8) . . ? C121 N10 C125 119.1(8) . . ? C124 N10 C125 123.9(9) . . ? C130 N11 C126 142.6(14) . . ? C130 N11 C129 122.0(12) . . ? C126 N11 C129 95.0(11) . . ? O31 N12 O33 117(2) . . ? O31 N12 O32 127(2) . . ? O33 N12 O32 114.3(19) . . ? C2 C1 C6 120.3(5) . . ? C2 C1 C21 116.8(5) . . ? C6 C1 C21 122.9(5) . . ? C3 C2 C1 121.6(6) . . ? C3 C2 H2 119.2 . . ? C1 C2 H2 119.2 . . ? C2 C3 O1 126.9(6) . . ? C2 C3 C4 118.8(5) . . ? O1 C3 C4 114.3(5) . . ? C5 C4 C3 120.2(6) . . ? C5 C4 O2 120.6(7) . . ? C3 C4 O2 119.1(6) . . ? C6 C5 C4 121.2(6) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C1 117.9(5) . . ? C5 C6 C7 119.0(6) . . ? C1 C6 C7 123.1(5) . . ? C8 C7 C6 115.7(5) . . ? C8 C7 H7A 108.4 . . ? C6 C7 H7A 108.4 . . ? C8 C7 H7B 108.4 . . ? C6 C7 H7B 108.4 . . ? H7A C7 H7B 107.4 . . ? C13 C8 C9 118.8(5) . . ? C13 C8 C7 122.8(5) . . ? C9 C8 C7 118.4(5) . . ? C10 C9 C8 121.4(5) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C11 C10 O4 115.7(5) . . ? C11 C10 C9 119.9(5) . . ? O4 C10 C9 124.3(5) . . ? C10 C11 O5 120.7(5) . . ? C10 C11 C12 120.5(6) . . ? O5 C11 C12 118.8(5) . . ? C11 C12 C13 120.6(5) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C8 C13 C12 118.7(5) . . ? C8 C13 C14 123.5(5) . . ? C12 C13 C14 117.7(5) . . ? C15 C14 C13 111.9(5) . . ? C15 C14 H14A 109.2 . . ? C13 C14 H14A 109.2 . . ? C15 C14 H14B 109.2 . . ? C13 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C20 C15 C16 118.6(5) . . ? C20 C15 C14 124.1(5) . . ? C16 C15 C14 117.3(5) . . ? C17 C16 C15 120.3(5) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C18 C17 O7 117.3(6) . . ? C18 C17 C16 119.1(5) . . ? O7 C17 C16 123.5(6) . . ? C17 C18 C19 121.8(6) . . ? C17 C18 O8 118.2(5) . . ? C19 C18 O8 120.0(5) . . ? C18 C19 C20 120.9(6) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C19 C20 C15 119.3(5) . . ? C19 C20 C21 117.9(5) . . ? C15 C20 C21 122.8(5) . . ? C1 C21 C20 111.8(5) . . ? C1 C21 H21A 109.3 . . ? C20 C21 H21A 109.3 . . ? C1 C21 H21B 109.3 . . ? C20 C21 H21B 109.3 . . ? H21A C21 H21B 107.9 . . ? O1 C22 H22A 109.5 . . ? O1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O3 C23 O2 123.3(5) . . ? O3 C23 C24 125.7(5) . . ? O2 C23 C24 111.0(5) . . ? C25 C24 C29 117.5(6) . . ? C25 C24 C23 124.2(6) . . ? C29 C24 C23 118.2(5) . . ? C24 C25 C26 121.8(6) . . ? C24 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C27 C26 C25 120.1(6) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C28 118.0(6) . . ? C26 C27 C30 122.7(6) . . ? C28 C27 C30 119.3(6) . . ? C29 C28 C27 120.0(6) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C24 122.5(6) . . ? C28 C29 H29 118.8 . . ? C24 C29 H29 118.8 . . ? C34 C30 C31 117.2(7) . . ? C34 C30 C27 122.6(7) . . ? C31 C30 C27 120.2(7) . . ? C32 C31 C30 117.8(8) . . ? C32 C31 H31 121.1 . . ? C30 C31 H31 121.1 . . ? N1 C32 C31 124.1(9) . . ? N1 C32 H32 117.9 . . ? C31 C32 H32 117.9 . . ? N1 C33 C34 124.2(7) . . ? N1 C33 H33 117.9 . . ? C34 C33 H33 117.9 . . ? C30 C34 C33 120.0(7) . . ? C30 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? O4 C35 H35A 109.5 . . ? O4 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? O4 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O6 C36 O5 122.7(5) . . ? O6 C36 C37 124.3(6) . . ? O5 C36 C37 113.0(5) . . ? C42 C37 C38 119.2(6) . . ? C42 C37 C36 118.2(6) . . ? C38 C37 C36 122.6(6) . . ? C39 C38 C37 121.0(6) . . ? C39 C38 H38 119.5 . . ? C37 C38 H38 119.5 . . ? C38 C39 C40 120.3(6) . . ? C38 C39 H39 119.9 . . ? C40 C39 H39 119.9 . . ? C39 C40 C41 118.3(6) . . ? C39 C40 C43 120.6(6) . . ? C41 C40 C43 121.0(6) . . ? C42 C41 C40 120.5(6) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C37 C42 C41 120.7(6) . . ? C37 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? C47 C43 C44 114.8(6) . . ? C47 C43 C40 120.6(6) . . ? C44 C43 C40 124.6(6) . . ? C43 C44 C45 121.1(6) . . ? C43 C44 H44 119.4 . . ? C45 C44 H44 119.4 . . ? N2 C45 C44 121.9(7) . . ? N2 C45 H45 119.1 . . ? C44 C45 H45 119.1 . . ? N2 C46 C47 124.4(6) . . ? N2 C46 H46 117.8 . . ? C47 C46 H46 117.8 . . ? C43 C47 C46 119.3(6) . . ? C43 C47 H47 120.3 . . ? C46 C47 H47 120.3 . . ? O7 C48 H48A 109.5 . . ? O7 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? O7 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O9 C49 O8 122.4(5) . . ? O9 C49 C50 127.1(5) . . ? O8 C49 C50 110.5(5) . . ? C55 C50 C51 119.7(6) . . ? C55 C50 C49 119.0(6) . . ? C51 C50 C49 121.2(5) . . ? C52 C51 C50 119.0(6) . . ? C52 C51 H51 120.5 . . ? C50 C51 H51 120.5 . . ? C51 C52 C53 121.3(7) . . ? C51 C52 H52 119.3 . . ? C53 C52 H52 119.3 . . ? C54 C53 C52 119.6(6) . . ? C54 C53 C56 121.6(6) . . ? C52 C53 C56 118.8(6) . . ? C53 C54 C55 118.8(6) . . ? C53 C54 H54 120.6 . . ? C55 C54 H54 120.6 . . ? C50 C55 C54 121.3(6) . . ? C50 C55 H55 119.3 . . ? C54 C55 H55 119.3 . . ? C57 C56 C60 117.2(6) . . ? C57 C56 C53 124.1(6) . . ? C60 C56 C53 118.6(6) . . ? C56 C57 C58 122.3(7) . . ? C56 C57 H57 118.8 . . ? C58 C57 H57 118.8 . . ? N3 C58 C57 119.8(7) . . ? N3 C58 H58 120.1 . . ? C57 C58 H58 120.1 . . ? N3 C59 C60 123.4(6) . . ? N3 C59 H59 118.3 . . ? C60 C59 H59 118.3 . . ? C56 C60 C59 118.0(6) . . ? C56 C60 H60 121.0 . . ? C59 C60 H60 121.0 . . ? C66 C61 C62 118.6(5) . . ? C66 C61 C81 123.7(5) . . ? C62 C61 C81 117.7(5) . . ? C61 C62 C63 119.4(6) . . ? C61 C62 H62 120.3 . . ? C63 C62 H62 120.3 . . ? C64 C63 C62 122.1(6) . . ? C64 C63 O11 117.7(5) . . ? C62 C63 O11 120.2(6) . . ? C65 C64 O10 126.1(6) . . ? C65 C64 C63 117.7(6) . . ? O10 C64 C63 116.0(5) . . ? C64 C65 C66 122.0(6) . . ? C64 C65 H65 119.0 . . ? C66 C65 H65 119.0 . . ? C61 C66 C65 120.2(5) . . ? C61 C66 C67 124.1(5) . . ? C65 C66 C67 115.7(5) . . ? C68 C67 C66 110.1(5) . . ? C68 C67 H67A 109.6 . . ? C66 C67 H67A 109.6 . . ? C68 C67 H67B 109.6 . . ? C66 C67 H67B 109.6 . . ? H67A C67 H67B 108.1 . . ? C69 C68 C73 120.4(5) . . ? C69 C68 C67 116.7(5) . . ? C73 C68 C67 123.0(5) . . ? C68 C69 C70 119.8(6) . . ? C68 C69 H69 120.1 . . ? C70 C69 H69 120.1 . . ? C71 C70 C69 121.5(6) . . ? C71 C70 O17 118.4(6) . . ? C69 C70 O17 120.2(6) . . ? C70 C71 C72 118.7(6) . . ? C70 C71 O16 115.9(6) . . ? C72 C71 O16 125.4(6) . . ? C71 C72 C73 122.2(6) . . ? C71 C72 H72 118.9 . . ? C73 C72 H72 118.9 . . ? C72 C73 C68 117.4(5) . . ? C72 C73 C74 118.0(5) . . ? C68 C73 C74 124.6(5) . . ? C73 C74 C75 112.5(5) . . ? C73 C74 H74A 109.1 . . ? C75 C74 H74A 109.1 . . ? C73 C74 H74B 109.1 . . ? C75 C74 H74B 109.1 . . ? H74A C74 H74B 107.8 . . ? C80 C75 C76 117.9(5) . . ? C80 C75 C74 124.3(6) . . ? C76 C75 C74 117.8(5) . . ? C77 C76 C75 120.9(6) . . ? C77 C76 H76 119.5 . . ? C75 C76 H76 119.5 . . ? C76 C77 C78 122.0(6) . . ? C76 C77 O14 119.5(5) . . ? C78 C77 O14 118.5(6) . . ? O13 C78 C77 116.5(5) . . ? O13 C78 C79 124.9(5) . . ? C77 C78 C79 118.5(6) . . ? C78 C79 C80 120.4(5) . . ? C78 C79 H79 119.8 . . ? C80 C79 H79 119.8 . . ? C75 C80 C79 120.3(5) . . ? C75 C80 C81 122.6(5) . . ? C79 C80 C81 117.0(5) . . ? C80 C81 C61 112.3(5) . . ? C80 C81 H81A 109.1 . . ? C61 C81 H81A 109.1 . . ? C80 C81 H81B 109.1 . . ? C61 C81 H81B 109.1 . . ? H81A C81 H81B 107.9 . . ? O10 C82 H82A 109.5 . . ? O10 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? O10 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? O12 C83 O11 124.2(6) . . ? O12 C83 C84 125.9(6) . . ? O11 C83 C84 109.7(6) . . ? C85 C84 C89 119.5(6) . . ? C85 C84 C83 122.7(6) . . ? C89 C84 C83 117.8(6) . . ? C84 C85 C86 120.1(6) . . ? C84 C85 H85 119.9 . . ? C86 C85 H85 119.9 . . ? C87 C86 C85 119.6(6) . . ? C87 C86 H86 120.2 . . ? C85 C86 H86 120.2 . . ? C88 C87 C86 119.2(7) . . ? C88 C87 C90 119.9(6) . . ? C86 C87 C90 120.8(6) . . ? C89 C88 C87 120.7(7) . . ? C89 C88 H88 119.6 . . ? C87 C88 H88 119.6 . . ? C88 C89 C84 120.8(6) . . ? C88 C89 H89 119.6 . . ? C84 C89 H89 119.6 . . ? C94 C90 C91 115.7(7) . . ? C94 C90 C87 122.3(8) . . ? C91 C90 C87 121.9(7) . . ? C92 C91 C90 117.6(8) . . ? C92 C91 H91 121.2 . . ? C90 C91 H91 121.2 . . ? N4 C92 C91 125.6(9) . . ? N4 C92 H92 117.2 . . ? C91 C92 H92 117.2 . . ? N4 C93 C94 122.0(8) . . ? N4 C93 H93 119.0 . . ? C94 C93 H93 119.0 . . ? C90 C94 C93 121.6(9) . . ? C90 C94 H94 119.2 . . ? C93 C94 H94 119.2 . . ? O16 C95 H95A 109.5 . . ? O16 C95 H95B 109.5 . . ? H95A C95 H95B 109.5 . . ? O16 C95 H95C 109.5 . . ? H95A C95 H95C 109.5 . . ? H95B C95 H95C 109.5 . . ? O18 C96 O17 122.2(6) . . ? O18 C96 C97 125.8(6) . . ? O17 C96 C97 111.9(6) . . ? C102 C97 C98 117.9(6) . . ? C102 C97 C96 118.2(6) . . ? C98 C97 C96 123.9(6) . . ? C99 C98 C97 119.9(7) . . ? C99 C98 H98 120.0 . . ? C97 C98 H98 120.0 . . ? C98 C99 C100 123.2(7) . . ? C98 C99 H99 118.4 . . ? C100 C99 H99 118.4 . . ? C99 C100 C101 118.7(6) . . ? C99 C100 C103 121.9(6) . . ? C101 C100 C103 119.4(6) . . ? C100 C101 C102 119.4(6) . . ? C100 C101 H101 120.3 . . ? C102 C101 H101 120.3 . . ? C97 C102 C101 120.8(7) . . ? C97 C102 H102 119.6 . . ? C101 C102 H102 119.6 . . ? C107 C103 C104 114.6(6) . . ? C107 C103 C100 123.0(7) . . ? C104 C103 C100 122.4(6) . . ? C103 C104 C105 121.7(7) . . ? C103 C104 H104 119.1 . . ? C105 C104 H104 119.1 . . ? C104 C105 N6 119.0(7) . . ? C104 C105 H105 120.5 . . ? N6 C105 H105 120.5 . . ? N6 C106 C107 123.8(7) . . ? N6 C106 H106 118.1 . . ? C107 C106 H106 118.1 . . ? C103 C107 C106 122.6(7) . . ? C103 C107 H107 118.7 . . ? C106 C107 H107 118.7 . . ? O13 C108 H10A 109.5 . . ? O13 C108 H10B 109.5 . . ? H10A C108 H10B 109.5 . . ? O13 C108 H10C 109.5 . . ? H10A C108 H10C 109.5 . . ? H10B C108 H10C 109.5 . . ? O15 C109 O14 122.0(6) . . ? O15 C109 C110 125.8(6) . . ? O14 C109 C110 112.2(6) . . ? C115 C110 C111 116.7(6) . . ? C115 C110 C109 124.3(6) . . ? C111 C110 C109 119.0(6) . . ? C112 C111 C110 122.8(6) . . ? C112 C111 H111 118.6 . . ? C110 C111 H111 118.6 . . ? C111 C112 C113 120.5(6) . . ? C111 C112 H112 119.7 . . ? C113 C112 H112 119.7 . . ? C114 C113 C112 118.0(6) . . ? C114 C113 C116 121.5(6) . . ? C112 C113 C116 120.5(6) . . ? C115 C114 C113 121.2(6) . . ? C115 C114 H114 119.4 . . ? C113 C114 H114 119.4 . . ? C110 C115 C114 120.8(6) . . ? C110 C115 H115 119.6 . . ? C114 C115 H115 119.6 . . ? C117 C116 C120 116.9(7) . . ? C117 C116 C113 121.7(7) . . ? C120 C116 C113 121.1(7) . . ? C116 C117 C118 118.5(8) . . ? C116 C117 H117 120.8 . . ? C118 C117 H117 120.8 . . ? N5 C118 C117 123.8(8) . . ? N5 C118 H118 118.1 . . ? C117 C118 H118 118.1 . . ? N5 C119 C120 126.7(8) . . ? N5 C119 H119 116.6 . . ? C120 C119 H119 116.6 . . ? C119 C120 C116 119.1(8) . . ? C119 C120 H120 120.5 . . ? C116 C120 H120 120.5 . . ? O29 C121 N10 125.8(8) . . ? O29 C121 C122 129.4(7) . . ? N10 C121 C122 104.8(8) . . ? C123 C122 C121 108.0(9) . . ? C123 C122 H12A 110.1 . . ? C121 C122 H12A 110.1 . . ? C123 C122 H12B 110.1 . . ? C121 C122 H12B 110.1 . . ? H12A C122 H12B 108.4 . . ? C122 C123 C124 104.9(10) . . ? C122 C123 H12C 110.8 . . ? C124 C123 H12C 110.8 . . ? C122 C123 H12D 110.8 . . ? C124 C123 H12D 110.8 . . ? H12C C123 H12D 108.8 . . ? N10 C124 C123 101.6(9) . . ? N10 C124 H12E 111.5 . . ? C123 C124 H12E 111.5 . . ? N10 C124 H12F 111.5 . . ? C123 C124 H12F 111.5 . . ? H12E C124 H12F 109.3 . . ? N10 C125 H12G 109.5 . . ? N10 C125 H12H 109.5 . . ? H12G C125 H12H 109.5 . . ? N10 C125 H12I 109.5 . . ? H12G C125 H12I 109.5 . . ? H12H C125 H12I 109.5 . . ? N11 C126 C127 133.1(14) . . ? N11 C126 O30 117.4(12) . . ? C127 C126 O30 109.3(12) . . ? C126 C127 C128 92.8(13) . . ? C126 C127 H12J 113.1 . . ? C128 C127 H12J 113.1 . . ? C126 C127 H12K 113.1 . . ? C128 C127 H12K 113.1 . . ? H12J C127 H12K 110.5 . . ? C129 C128 C127 116.2(16) . . ? C129 C128 H12L 108.2 . . ? C127 C128 H12L 108.2 . . ? C129 C128 H12M 108.2 . . ? C127 C128 H12M 108.2 . . ? H12L C128 H12M 107.4 . . ? C128 C129 N11 102.3(13) . . ? C128 C129 H12N 111.3 . . ? N11 C129 H12N 111.3 . . ? C128 C129 H12O 111.3 . . ? N11 C129 H12O 111.3 . . ? H12N C129 H12O 109.2 . . ? N11 C130 H13A 109.5 . . ? N11 C130 H13B 109.5 . . ? H13A C130 H13B 109.5 . . ? N11 C130 H13C 109.5 . . ? H13A C130 H13C 109.5 . . ? H13B C130 H13C 109.5 . . ? O21 N7 O20 124.8(11) . . ? O21 N7 O22 156.2(13) . . ? O20 N7 O22 78.6(8) . . ? N7 O20 Cd1 78.4(6) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 4.800 _refine_diff_density_min -1.024 _refine_diff_density_rms 0.121 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.014 -0.001 -0.007 4361 908 ' ' _platon_squeeze_details ; TGA is consistent with 4 additional water molecules and eight N-methylpyrrolidone molecules than were refined in this crystal strcuture. This is also consistent with void spaces calculated by SQUEEZE. Additional solvent has been included in the formula ; # Attachment '- complex5_new.CIF' data_complex5_new _database_code_depnum_ccdc_archive 'CCDC 822484' #TrackingRef '- complex5_new.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; diaquo[(+-)-2,7,12-trimethoxy-3,8,13- tris[4-(4-pyridyl)benzoyl]-10,15-dihydro-5H- tribenzo[a,d,g]cyclononane]cobalt(II) nitrate ; _chemical_name_common ; diaquo((+-)-2,7,12-trimethoxy-3,8,13-tris(4-(4- pyridyl)benzoyl)-10,15-dihydro-5H-tribenzo(a,d,g)cyclononane)cobalt(ii) nitrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H61 Co N5 O13' _chemical_formula_weight 1191.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.2313(8) _cell_length_b 16.7654(9) _cell_length_c 17.7506(9) _cell_angle_alpha 112.858(2) _cell_angle_beta 94.933(2) _cell_angle_gamma 101.901(2) _cell_volume 4280.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour pink _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.924 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1246 _exptl_absorpt_coefficient_mu 0.250 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9142 _exptl_absorpt_correction_T_max 0.9810 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47497 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 20.81 _reflns_number_total 8817 _reflns_number_gt 5741 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Very disordered Co(H2O)py unit modelled over two sites for py and three for Co with an isotropic refinement. SIMU restraints used for disordered py groups and a FLAT restraint for adjoining phenyl gp. FLAT C24 C25 C26 C27 C28 C29 SIMU C30A C31A C32A N1A C33A C34A SIMU C30B C31B C32B N1B C33B C34B ; _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^)+(0.1000P)^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 8817 _refine_ls_number_parameters 728 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1147 _refine_ls_R_factor_gt 0.0895 _refine_ls_wR_factor_ref 0.2364 _refine_ls_wR_factor_gt 0.2278 _refine_ls_goodness_of_fit_ref 1.503 _refine_ls_restrained_S_all 1.503 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.0000 0.0000 0.5000 0.0734(4) Uani 1 2 d S . . O1 O 1.0230(3) -0.4908(4) 0.4182(3) 0.1163(14) Uani 1 1 d . . . O2 O 0.9920(3) -0.3673(3) 0.4188(3) 0.1150(14) Uani 1 1 d . . . O3 O 0.8427(3) -0.3923(4) 0.4670(3) 0.1482(18) Uani 1 1 d . . . O4 O 0.3844(2) -0.4845(3) 0.1602(3) 0.0917(11) Uani 1 1 d . . . O5 O 0.4962(2) -0.3685(3) 0.2287(2) 0.1011(12) Uani 1 1 d . . . O6 O 0.5167(2) -0.3478(3) 0.0882(3) 0.1049(12) Uani 1 1 d . . . O7 O 0.9194(2) -0.4584(3) -0.1628(2) 0.0792(10) Uani 1 1 d . . . O8 O 0.8928(2) -0.3424(2) -0.0590(2) 0.0873(11) Uani 1 1 d . . . O9 O 1.0324(3) -0.3422(3) 0.0358(2) 0.0972(12) Uani 1 1 d . . . O10 O -0.1032(2) -0.1005(2) 0.4109(2) 0.0970(12) Uani 1 1 d . . . N2 N 0.0863(3) -0.0791(3) 0.4452(3) 0.0779(12) Uani 1 1 d . . . N3 N 0.9795(4) -0.0682(4) -0.4208(4) 0.0841(18) Uani 1 1 d . . . C1 C 0.7681(4) -0.5217(4) 0.2396(4) 0.0846(16) Uani 1 1 d . . . C2 C 0.7670(5) -0.4788(5) 0.3260(4) 0.1006(19) Uani 1 1 d . . . H2 H 0.7136 -0.4846 0.3441 0.121 Uiso 1 1 calc R . . C3 C 0.8393(5) -0.4299(4) 0.3837(4) 0.0988(18) Uani 1 1 d . . . C4 C 0.9160(4) -0.4219(4) 0.3556(5) 0.0938(17) Uani 1 1 d . . . C5 C 0.9199(4) -0.4622(4) 0.2746(4) 0.0871(16) Uani 1 1 d . . . H5 H 0.9743 -0.4555 0.2583 0.105 Uiso 1 1 calc R . . C6 C 0.8478(4) -0.5130(4) 0.2139(4) 0.0772(15) Uani 1 1 d . . . C7 C 0.8576(3) -0.5583(4) 0.1238(3) 0.0784(15) Uani 1 1 d . . . H7A H 0.9096 -0.5806 0.1223 0.094 Uiso 1 1 calc R . . H7B H 0.8078 -0.6109 0.0941 0.094 Uiso 1 1 calc R . . C8 C 0.8641(3) -0.4985(4) 0.0776(3) 0.0726(14) Uani 1 1 d . . . C9 C 0.9441(3) -0.4447(4) 0.0819(3) 0.0777(15) Uani 1 1 d . . . H9 H 0.9926 -0.4434 0.1168 0.093 Uiso 1 1 calc R . . C10 C 0.9543(4) -0.3937(4) 0.0368(4) 0.0797(15) Uani 1 1 d . . . C11 C 0.8844(4) -0.3943(4) -0.0117(4) 0.0840(16) Uani 1 1 d . . . C12 C 0.8025(3) -0.4459(4) -0.0176(3) 0.0761(15) Uani 1 1 d . . . H12 H 0.7545 -0.4448 -0.0516 0.091 Uiso 1 1 calc R . . C13 C 0.7917(3) -0.4996(4) 0.0274(3) 0.0737(14) Uani 1 1 d . . . C14 C 0.7030(3) -0.5545(3) 0.0173(3) 0.0767(15) Uani 1 1 d . . . H14A H 0.7064 -0.6095 0.0245 0.092 Uiso 1 1 calc R . . H14B H 0.6724 -0.5732 -0.0400 0.092 Uiso 1 1 calc R . . C15 C 0.6510(3) -0.5045(4) 0.0792(3) 0.0777(15) Uani 1 1 d . . . C16 C 0.6099(3) -0.4481(4) 0.0573(3) 0.0805(15) Uani 1 1 d . . . H16 H 0.6179 -0.4408 0.0078 0.097 Uiso 1 1 calc R . . C17 C 0.5591(3) -0.4043(4) 0.1056(4) 0.0822(15) Uani 1 1 d . . . C18 C 0.5478(3) -0.4153(4) 0.1769(4) 0.0832(16) Uani 1 1 d . . . C19 C 0.5868(3) -0.4696(4) 0.2000(3) 0.0859(16) Uani 1 1 d . . . H19 H 0.5775 -0.4765 0.2495 0.103 Uiso 1 1 calc R . . C20 C 0.6404(3) -0.5151(4) 0.1514(3) 0.0795(15) Uani 1 1 d . . . C21 C 0.6834(4) -0.5733(4) 0.1809(4) 0.0916(17) Uani 1 1 d . . . H21A H 0.6443 -0.6007 0.2092 0.110 Uiso 1 1 calc R . . H21B H 0.6929 -0.6225 0.1318 0.110 Uiso 1 1 calc R . . C22 C 0.7612(6) -0.3987(7) 0.4947(5) 0.195(4) Uani 1 1 d . . . H22A H 0.7214 -0.3836 0.4609 0.293 Uiso 1 1 calc R . . H22B H 0.7695 -0.3569 0.5532 0.293 Uiso 1 1 calc R . . H22C H 0.7375 -0.4600 0.4887 0.293 Uiso 1 1 calc R . . C23 C 1.0386(5) -0.4094(6) 0.4490(5) 0.112(2) Uani 1 1 d . . . C24 C 1.1080(5) -0.3509(6) 0.5188(5) 0.113(2) Uani 1 1 d D C . C25 C 1.1324(7) -0.2632(8) 0.5447(6) 0.186(4) Uani 1 1 d D . . H25 H 1.1071 -0.2368 0.5132 0.223 Uiso 1 1 calc R . . C26 C 1.1939(8) -0.2069(7) 0.6164(7) 0.221(6) Uani 1 1 d D C . H26 H 1.2094 -0.1438 0.6330 0.265 Uiso 1 1 calc R . . C27 C 1.2313(8) -0.2437(10) 0.6621(6) 0.200(5) Uani 1 1 d D . . C28 C 1.2086(8) -0.3353(10) 0.6348(7) 0.189(4) Uani 1 1 d D C . H28 H 1.2357 -0.3617 0.6651 0.226 Uiso 1 1 calc R . . C29 C 1.1495(6) -0.3883(6) 0.5668(6) 0.145(3) Uani 1 1 d D . . H29 H 1.1347 -0.4514 0.5500 0.174 Uiso 1 1 calc R C . C35 C 0.5338(4) -0.3307(5) 0.0159(5) 0.127(2) Uani 1 1 d . . . H35A H 0.5935 -0.2964 0.0263 0.191 Uiso 1 1 calc R . . H35B H 0.4955 -0.2964 0.0056 0.191 Uiso 1 1 calc R . . H35C H 0.5239 -0.3879 -0.0328 0.191 Uiso 1 1 calc R . . C36 C 0.4138(4) -0.4083(5) 0.2115(4) 0.0795(15) Uani 1 1 d . . . C37 C 0.3599(4) -0.3493(5) 0.2578(4) 0.0812(15) Uani 1 1 d . . . C38 C 0.2713(3) -0.3876(4) 0.2427(4) 0.0958(17) Uani 1 1 d . . . H38 H 0.2469 -0.4488 0.2060 0.115 Uiso 1 1 calc R . . C39 C 0.2205(3) -0.3330(5) 0.2832(4) 0.1005(19) Uani 1 1 d . . . H39 H 0.1605 -0.3581 0.2749 0.121 Uiso 1 1 calc R . . C40 C 0.2539(4) -0.2457(5) 0.3340(4) 0.0868(16) Uani 1 1 d . . . C41 C 0.3415(4) -0.2103(4) 0.3516(4) 0.119(2) Uani 1 1 d . . . H41 H 0.3660 -0.1502 0.3909 0.143 Uiso 1 1 calc R . . C42 C 0.3946(4) -0.2640(5) 0.3107(5) 0.112(2) Uani 1 1 d . . . H42 H 0.4548 -0.2394 0.3210 0.134 Uiso 1 1 calc R . . C43 C 0.1959(4) -0.1866(5) 0.3736(4) 0.0906(18) Uani 1 1 d . . . C44 C 0.1146(5) -0.2089(6) 0.3486(5) 0.168(4) Uani 1 1 d . D . H44 H 0.0890 -0.2645 0.3024 0.202 Uiso 1 1 calc R . . C45 C 0.0630(4) -0.1551(7) 0.3864(5) 0.160(4) Uani 1 1 d . D . H45 H 0.0032 -0.1784 0.3652 0.193 Uiso 1 1 calc R A 2 C48 C 1.1065(3) -0.3311(4) 0.0946(4) 0.1008(18) Uani 1 1 d . . . H48A H 1.0973 -0.3003 0.1514 0.151 Uiso 1 1 calc R . . H48B H 1.1575 -0.2955 0.0857 0.151 Uiso 1 1 calc R . . H48C H 1.1145 -0.3901 0.0863 0.151 Uiso 1 1 calc R . . C49 C 0.9118(3) -0.3832(4) -0.1366(4) 0.0778(15) Uani 1 1 d . . . C50 C 0.9241(3) -0.3236(4) -0.1800(3) 0.0759(14) Uani 1 1 d . . . C51 C 0.9509(4) -0.3537(4) -0.2542(4) 0.108(2) Uani 1 1 d . . . H51 H 0.9612 -0.4114 -0.2763 0.129 Uiso 1 1 calc R . . C52 C 0.9633(4) -0.3004(4) -0.2979(4) 0.109(2) Uani 1 1 d . . . H52 H 0.9843 -0.3218 -0.3485 0.131 Uiso 1 1 calc R . . C53 C 0.9466(4) -0.2192(4) -0.2708(4) 0.0899(17) Uani 1 1 d . E . C54 C 0.9204(5) -0.1877(5) -0.1926(4) 0.141(3) Uani 1 1 d . . . H54 H 0.9106 -0.1297 -0.1699 0.169 Uiso 1 1 calc R . . C55 C 0.9091(5) -0.2402(5) -0.1494(4) 0.140(3) Uani 1 1 d . . . H55 H 0.8907 -0.2186 -0.0975 0.168 Uiso 1 1 calc R . . C56 C 0.9570(4) -0.1646(5) -0.3201(4) 0.0859(17) Uani 1 1 d . . . Co2A Co 1.5000 0.0000 1.0000 0.1995(19) Uiso 0.50 2 d SP . 1 Co2B Co 1.5562(5) 0.0076(5) 0.9736(4) 0.201(3) Uiso 0.25 1 d P . 2 O11A O 1.5260(8) 0.0911(10) 0.9586(9) 0.203(5) Uiso 0.50 1 d P B 1 C30A C 1.2700(16) -0.1862(16) 0.7409(15) 0.172(7) Uiso 0.50 1 d PU C 1 C31A C 1.3169(13) -0.2210(14) 0.7881(12) 0.165(6) Uiso 0.50 1 d PU C 1 H31A H 1.3116 -0.2836 0.7676 0.198 Uiso 0.50 1 calc PR C 1 C32A C 1.3708(14) -0.1616(15) 0.8650(14) 0.181(7) Uiso 0.50 1 d PU C 1 H32A H 1.4060 -0.1855 0.8914 0.217 Uiso 0.50 1 calc PR C 1 N1A N 1.3759(14) -0.0702(14) 0.9048(12) 0.203(7) Uiso 0.50 1 d PU C 1 C33A C 1.315(2) -0.042(2) 0.860(2) 0.238(11) Uiso 0.50 1 d PU C 1 H33A H 1.3099 0.0180 0.8844 0.286 Uiso 0.50 1 calc PR C 1 C34A C 1.270(2) -0.095(2) 0.788(2) 0.242(11) Uiso 0.50 1 d PU C 1 H34A H 1.2330 -0.0716 0.7630 0.291 Uiso 0.50 1 calc PR C 1 C46A C 0.1690(7) -0.0631(8) 0.4885(8) 0.084(3) Uani 0.50 1 d P D 1 H46A H 0.1886 -0.0125 0.5405 0.101 Uiso 0.50 1 calc PR D 1 C47A C 0.2236(8) -0.1175(9) 0.4591(8) 0.082(3) Uani 0.50 1 d P D 1 H47A H 0.2758 -0.1104 0.4926 0.098 Uiso 0.50 1 calc PR D 1 C57A C 1.0292(11) -0.1381(14) -0.3411(13) 0.150(6) Uani 0.50 1 d P E 2 H57A H 1.0798 -0.1502 -0.3222 0.180 Uiso 0.50 1 calc PR E 2 C58A C 1.0313(17) -0.0899(18) -0.3937(15) 0.165(8) Uani 0.50 1 d P E 2 H58A H 1.0857 -0.0740 -0.4076 0.198 Uiso 0.50 1 calc PR E 2 C59A C 0.9067(14) -0.0854(18) -0.3975(18) 0.234(14) Uani 0.50 1 d P E 2 H59A H 0.8660 -0.0542 -0.4043 0.281 Uiso 0.50 1 calc PR E 2 C60A C 0.8852(11) -0.1463(17) -0.3633(14) 0.176(8) Uani 0.50 1 d P E 2 H60A H 0.8272 -0.1754 -0.3673 0.211 Uiso 0.50 1 calc PR E 2 C30B C 1.336(2) -0.172(2) 0.7386(17) 0.221(10) Uiso 0.50 1 d PU C 2 C31B C 1.382(2) -0.209(2) 0.773(2) 0.241(10) Uiso 0.50 1 d PU C 2 H31B H 1.3796 -0.2716 0.7513 0.290 Uiso 0.50 1 calc PR C 2 C32B C 1.4389(18) -0.140(2) 0.8479(18) 0.225(10) Uiso 0.50 1 d PU C 2 H32B H 1.4821 -0.1572 0.8728 0.270 Uiso 0.50 1 calc PR C 2 N1B N 1.4366(15) -0.0622(17) 0.8823(15) 0.224(8) Uiso 0.50 1 d PU . 2 C33B C 1.381(2) -0.032(2) 0.846(2) 0.275(13) Uiso 0.50 1 d PU C 2 H33B H 1.3775 0.0280 0.8746 0.330 Uiso 0.50 1 calc PR C 2 C34B C 1.327(2) -0.087(2) 0.7676(19) 0.220(10) Uiso 0.50 1 d PU C 2 H34B H 1.2898 -0.0666 0.7390 0.264 Uiso 0.50 1 calc PR C 2 C46B C 0.1625(13) -0.0432(13) 0.4321(15) 0.163(8) Uani 0.50 1 d P D 2 H46B H 0.1793 0.0188 0.4439 0.196 Uiso 0.50 1 calc PR D 2 C47B C 0.2179(11) -0.0990(14) 0.4002(17) 0.166(8) Uani 0.50 1 d P D 2 H47B H 0.2743 -0.0710 0.3980 0.199 Uiso 0.50 1 calc PR D 2 C57B C 0.9356(11) -0.2040(7) -0.4000(8) 0.099(5) Uani 0.50 1 d P E 1 H57B H 0.9102 -0.2668 -0.4261 0.119 Uiso 0.50 1 calc PR E 1 C58B C 0.9488(9) -0.1567(7) -0.4482(7) 0.085(3) Uani 0.50 1 d P E 1 H58B H 0.9347 -0.1905 -0.5068 0.102 Uiso 0.50 1 calc PR E 1 C59B C 1.0068(11) -0.0295(8) -0.3363(8) 0.096(4) Uani 0.50 1 d P E 1 H59B H 1.0371 0.0321 -0.3103 0.115 Uiso 0.50 1 calc PR E 1 C60B C 0.9919(11) -0.0774(8) -0.2862(6) 0.100(5) Uani 0.50 1 d P E 1 H60B H 1.0072 -0.0463 -0.2274 0.121 Uiso 0.50 1 calc PR E 1 O11B O 1.4607(4) 0.0404(5) 1.0206(4) 0.0673(18) Uiso 0.50 1 d P . 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 Co1 0.0857(7) 0.0895(8) 0.0825(8) 0.0519(6) 0.0442(6) 0.0568(6) O1 0.136(3) 0.123(4) 0.094(3) 0.040(3) 0.005(3) 0.060(3) O2 0.154(4) 0.129(4) 0.097(3) 0.066(3) 0.026(3) 0.070(3) O3 0.175(5) 0.210(5) 0.090(4) 0.065(3) 0.059(3) 0.096(4) O4 0.067(2) 0.120(3) 0.095(3) 0.036(3) 0.035(2) 0.048(2) O5 0.058(2) 0.122(3) 0.105(3) 0.018(2) 0.024(2) 0.041(2) O6 0.077(2) 0.123(3) 0.131(4) 0.049(3) 0.027(2) 0.065(2) O7 0.091(2) 0.093(3) 0.087(3) 0.056(2) 0.042(2) 0.046(2) O8 0.106(3) 0.115(3) 0.094(3) 0.069(2) 0.062(2) 0.071(2) O9 0.090(3) 0.124(3) 0.112(3) 0.067(3) 0.054(3) 0.049(2) O10 0.119(3) 0.111(3) 0.116(3) 0.073(2) 0.058(2) 0.079(2) N2 0.080(3) 0.092(4) 0.085(3) 0.044(3) 0.038(3) 0.047(3) N3 0.101(4) 0.108(5) 0.082(4) 0.053(3) 0.038(3) 0.072(3) C1 0.102(5) 0.113(4) 0.078(4) 0.061(4) 0.035(4) 0.060(4) C2 0.109(5) 0.156(6) 0.081(5) 0.072(5) 0.044(5) 0.074(5) C3 0.130(6) 0.128(5) 0.056(5) 0.039(4) 0.026(5) 0.063(5) C4 0.098(5) 0.127(5) 0.079(5) 0.055(4) 0.020(5) 0.051(4) C5 0.104(5) 0.114(5) 0.086(5) 0.064(4) 0.040(4) 0.063(4) C6 0.082(4) 0.115(4) 0.080(4) 0.065(4) 0.037(4) 0.061(4) C7 0.078(3) 0.105(4) 0.094(4) 0.059(4) 0.050(3) 0.059(3) C8 0.075(4) 0.108(4) 0.070(3) 0.050(3) 0.040(3) 0.059(3) C9 0.067(4) 0.116(4) 0.081(4) 0.054(4) 0.034(3) 0.052(3) C10 0.078(4) 0.107(4) 0.093(4) 0.060(4) 0.047(3) 0.057(3) C11 0.099(5) 0.113(4) 0.090(4) 0.065(4) 0.052(4) 0.072(4) C12 0.071(4) 0.107(4) 0.079(4) 0.047(3) 0.037(3) 0.056(3) C13 0.078(4) 0.107(4) 0.077(4) 0.056(3) 0.045(3) 0.061(3) C14 0.078(4) 0.105(4) 0.085(4) 0.053(3) 0.050(3) 0.060(3) C15 0.066(3) 0.110(4) 0.089(4) 0.059(3) 0.038(3) 0.044(3) C16 0.074(3) 0.110(4) 0.088(4) 0.054(3) 0.035(3) 0.051(3) C17 0.073(3) 0.098(4) 0.091(4) 0.039(4) 0.026(3) 0.050(3) C18 0.063(3) 0.103(4) 0.087(4) 0.027(4) 0.030(3) 0.050(3) C19 0.071(3) 0.113(4) 0.088(4) 0.041(4) 0.042(3) 0.043(3) C20 0.080(3) 0.106(4) 0.077(4) 0.048(3) 0.040(3) 0.047(3) C21 0.102(4) 0.134(5) 0.087(4) 0.070(4) 0.055(4) 0.067(4) C22 0.192(8) 0.298(12) 0.107(6) 0.066(7) 0.093(6) 0.096(8) C23 0.159(7) 0.099(6) 0.110(6) 0.053(6) 0.055(6) 0.067(6) C24 0.165(6) 0.077(5) 0.073(5) 0.013(4) 0.004(5) 0.028(5) C25 0.301(13) 0.142(9) 0.104(7) 0.055(6) -0.027(8) 0.054(8) C26 0.332(15) 0.162(8) 0.111(7) 0.035(7) -0.084(9) 0.038(9) C27 0.258(12) 0.180(10) 0.103(7) 0.057(8) -0.085(8) -0.015(9) C28 0.216(10) 0.186(11) 0.123(8) 0.057(8) -0.059(8) 0.020(9) C29 0.161(7) 0.155(7) 0.136(7) 0.073(7) 0.006(6) 0.060(6) C35 0.117(5) 0.158(6) 0.182(7) 0.118(6) 0.059(5) 0.085(5) C36 0.069(4) 0.096(5) 0.071(4) 0.025(4) 0.018(3) 0.033(4) C37 0.081(4) 0.096(5) 0.075(4) 0.029(4) 0.034(3) 0.048(4) C38 0.063(4) 0.107(4) 0.111(5) 0.029(4) 0.025(3) 0.037(3) C39 0.058(3) 0.117(5) 0.116(5) 0.028(4) 0.033(3) 0.035(4) C40 0.073(4) 0.101(5) 0.094(4) 0.039(4) 0.026(3) 0.037(4) C41 0.091(5) 0.104(5) 0.144(6) 0.024(4) 0.046(4) 0.033(4) C42 0.076(4) 0.114(6) 0.139(6) 0.028(5) 0.052(4) 0.048(4) C43 0.081(4) 0.102(5) 0.112(6) 0.045(4) 0.057(4) 0.056(4) C44 0.100(6) 0.202(8) 0.148(7) -0.016(6) 0.034(5) 0.099(6) C45 0.084(5) 0.163(7) 0.143(7) -0.034(6) -0.017(5) 0.052(5) C48 0.062(3) 0.138(5) 0.111(5) 0.057(4) 0.020(3) 0.033(3) C49 0.076(3) 0.095(4) 0.099(5) 0.059(4) 0.042(3) 0.051(3) C50 0.087(3) 0.091(4) 0.081(4) 0.049(3) 0.043(3) 0.050(3) C51 0.174(6) 0.103(4) 0.097(5) 0.058(4) 0.077(5) 0.087(4) C52 0.189(6) 0.095(4) 0.089(4) 0.055(4) 0.076(4) 0.080(4) C53 0.123(4) 0.090(4) 0.094(4) 0.056(4) 0.057(4) 0.056(4) C54 0.255(9) 0.120(5) 0.127(6) 0.081(5) 0.125(6) 0.120(6) C55 0.258(9) 0.130(6) 0.123(6) 0.090(5) 0.129(6) 0.130(6) C56 0.106(5) 0.097(6) 0.089(5) 0.051(5) 0.060(4) 0.054(4) C46A 0.073(8) 0.070(8) 0.084(9) -0.005(6) 0.014(7) 0.042(6) C47A 0.085(8) 0.083(8) 0.086(10) 0.028(8) 0.022(7) 0.050(7) C57A 0.122(13) 0.185(19) 0.176(18) 0.117(18) -0.007(14) 0.038(13) C58A 0.22(2) 0.19(2) 0.126(17) 0.110(19) 0.098(19) 0.02(2) C59A 0.23(2) 0.34(3) 0.41(4) 0.35(3) 0.24(3) 0.21(2) C60A 0.146(14) 0.29(2) 0.21(2) 0.19(2) 0.085(15) 0.120(17) C46B 0.166(16) 0.190(17) 0.25(2) 0.156(18) 0.124(17) 0.123(14) C47B 0.140(14) 0.134(16) 0.29(3) 0.104(17) 0.153(17) 0.098(12) C57B 0.203(16) 0.050(7) 0.058(9) 0.031(7) 0.051(9) 0.034(8) C58B 0.147(12) 0.031(7) 0.059(7) 0.007(6) 0.001(7) 0.017(7) C59B 0.146(13) 0.065(8) 0.057(8) 0.027(7) -0.006(9) -0.007(8) C60B 0.214(15) 0.048(8) 0.043(6) 0.015(6) 0.047(9) 0.040(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O10 2.111(4) . ? Co1 O10 2.111(4) 2_556 ? Co1 N3 2.137(5) 2_655 ? Co1 N3 2.137(5) 1_456 ? Co1 N2 2.159(4) 2_556 ? Co1 N2 2.159(4) . ? O1 C23 1.216(7) . ? O2 C23 1.341(7) . ? O2 C4 1.455(7) . ? O3 C3 1.354(7) . ? O3 C22 1.449(8) . ? O4 C36 1.207(6) . ? O5 C36 1.315(6) . ? O5 C18 1.418(6) . ? O6 C17 1.387(6) . ? O6 C35 1.455(7) . ? O7 C49 1.198(6) . ? O8 C49 1.373(6) . ? O8 C11 1.420(6) . ? O9 C10 1.385(6) . ? O9 C48 1.452(6) . ? N2 C45 1.248(8) . ? N2 C46B 1.341(18) . ? N2 C46A 1.407(12) . ? N3 C58A 1.12(3) . ? N3 C59A 1.299(17) . ? N3 C58B 1.334(12) . ? N3 C59B 1.371(14) . ? N3 Co1 2.137(5) 1_654 ? C1 C6 1.407(7) . ? C1 C2 1.422(8) . ? C1 C21 1.513(7) . ? C2 C3 1.357(8) . ? C3 C4 1.381(8) . ? C4 C5 1.344(8) . ? C5 C6 1.384(7) . ? C6 C7 1.519(7) . ? C7 C8 1.516(6) . ? C8 C9 1.396(6) . ? C8 C13 1.404(6) . ? C9 C10 1.377(7) . ? C10 C11 1.360(7) . ? C11 C12 1.399(7) . ? C12 C13 1.415(6) . ? C13 C14 1.494(7) . ? C14 C15 1.535(6) . ? C15 C20 1.380(7) . ? C15 C16 1.411(7) . ? C16 C17 1.354(7) . ? C17 C18 1.370(7) . ? C18 C19 1.371(7) . ? C19 C20 1.405(7) . ? C20 C21 1.525(7) . ? C23 C24 1.460(10) . ? C24 C25 1.317(10) . ? C24 C29 1.436(10) . ? C25 C26 1.403(12) . ? C26 C27 1.367(13) . ? C27 C30A 1.35(2) . ? C27 C28 1.374(13) . ? C27 C30B 1.92(3) . ? C28 C29 1.335(11) . ? C36 C37 1.507(8) . ? C37 C42 1.333(7) . ? C37 C38 1.404(7) . ? C38 C39 1.392(7) . ? C39 C40 1.347(7) . ? C40 C41 1.379(7) . ? C40 C43 1.523(8) . ? C41 C42 1.414(8) . ? C43 C44 1.282(8) . ? C43 C47B 1.314(18) . ? C43 C47A 1.466(14) . ? C44 C45 1.380(9) . ? C45 C46B 2.03(2) . ? C49 C50 1.475(7) . ? C50 C51 1.361(7) . ? C50 C55 1.372(7) . ? C51 C52 1.390(7) . ? C52 C53 1.351(7) . ? C53 C54 1.419(8) . ? C53 C56 1.488(7) . ? C54 C55 1.371(8) . ? C56 C57B 1.288(12) . ? C56 C60B 1.317(12) . ? C56 C57A 1.304(19) . ? C56 C60A 1.488(17) . ? Co2A O11A 1.926(14) . ? Co2A O11A 1.926(14) 2_857 ? Co2A N1A 2.28(2) . ? Co2A N1A 2.28(2) 2_857 ? Co2B O11B 0.842(8) 2_857 ? Co2B O11B 1.903(8) . ? Co2B Co2B 2.136(15) 2_857 ? Co2B N1B 2.19(2) . ? Co2B N1B 2.34(3) 2_857 ? C30A C34A 1.42(3) . ? C30A C31A 1.44(3) . ? C31A C32A 1.41(2) . ? C32A N1A 1.40(2) . ? N1A C33A 1.48(3) . ? C33A C34A 1.28(3) . ? C46A C47A 1.390(14) . ? C57A C58A 1.45(2) . ? C59A C60A 1.38(2) . ? C30B C31B 1.32(3) . ? C30B C34B 1.36(3) . ? C31B C32B 1.46(3) . ? C32B N1B 1.22(3) . ? N1B C33B 1.35(4) . ? N1B Co2B 2.34(3) 2_857 ? C33B C34B 1.42(4) . ? C46B C47B 1.42(2) . ? C57B C58B 1.376(14) . ? C59B C60B 1.418(15) . ? O11B Co2B 0.842(8) 2_857 ? 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 O10 Co1 O10 180.0(3) . 2_556 ? O10 Co1 N3 91.60(19) . 2_655 ? O10 Co1 N3 88.40(19) 2_556 2_655 ? O10 Co1 N3 88.40(19) . 1_456 ? O10 Co1 N3 91.60(19) 2_556 1_456 ? N3 Co1 N3 180.000(1) 2_655 1_456 ? O10 Co1 N2 90.68(17) . 2_556 ? O10 Co1 N2 89.32(17) 2_556 2_556 ? N3 Co1 N2 89.78(17) 2_655 2_556 ? N3 Co1 N2 90.22(17) 1_456 2_556 ? O10 Co1 N2 89.32(17) . . ? O10 Co1 N2 90.68(17) 2_556 . ? N3 Co1 N2 90.22(17) 2_655 . ? N3 Co1 N2 89.78(17) 1_456 . ? N2 Co1 N2 180.0(3) 2_556 . ? C23 O2 C4 117.9(6) . . ? C3 O3 C22 116.2(6) . . ? C36 O5 C18 116.5(4) . . ? C17 O6 C35 116.5(4) . . ? C49 O8 C11 115.8(4) . . ? C10 O9 C48 118.0(4) . . ? C45 N2 C46B 103.3(10) . . ? C45 N2 C46A 111.4(6) . . ? C46B N2 C46A 50.6(8) . . ? C45 N2 Co1 124.3(5) . . ? C46B N2 Co1 122.7(8) . . ? C46A N2 Co1 121.5(5) . . ? C58A N3 C59A 114.1(12) . . ? C58A N3 C58B 75.6(13) . . ? C59A N3 C58B 70.6(12) . . ? C58A N3 C59B 61.1(13) . . ? C59A N3 C59B 80.5(13) . . ? C58B N3 C59B 110.5(7) . . ? C58A N3 Co1 123.0(9) . 1_654 ? C59A N3 Co1 122.8(8) . 1_654 ? C58B N3 Co1 124.2(6) . 1_654 ? C59B N3 Co1 124.7(6) . 1_654 ? C6 C1 C2 118.1(6) . . ? C6 C1 C21 123.9(5) . . ? C2 C1 C21 118.0(5) . . ? C3 C2 C1 122.6(6) . . ? O3 C3 C2 125.1(7) . . ? O3 C3 C4 117.3(7) . . ? C2 C3 C4 117.4(6) . . ? C5 C4 C3 121.8(6) . . ? C5 C4 O2 122.2(6) . . ? C3 C4 O2 116.0(6) . . ? C4 C5 C6 122.6(6) . . ? C5 C6 C1 117.5(5) . . ? C5 C6 C7 119.5(5) . . ? C1 C6 C7 123.0(6) . . ? C8 C7 C6 114.6(4) . . ? C9 C8 C13 119.6(4) . . ? C9 C8 C7 119.4(5) . . ? C13 C8 C7 120.9(5) . . ? C10 C9 C8 121.6(5) . . ? C11 C10 C9 119.1(5) . . ? C11 C10 O9 116.7(5) . . ? C9 C10 O9 124.2(5) . . ? C10 C11 C12 121.8(5) . . ? C10 C11 O8 120.5(5) . . ? C12 C11 O8 117.7(5) . . ? C11 C12 C13 119.4(5) . . ? C8 C13 C12 118.4(5) . . ? C8 C13 C14 124.7(5) . . ? C12 C13 C14 116.9(5) . . ? C13 C14 C15 113.3(4) . . ? C20 C15 C16 119.9(4) . . ? C20 C15 C14 123.6(4) . . ? C16 C15 C14 116.5(4) . . ? C17 C16 C15 121.3(5) . . ? C16 C17 C18 119.0(5) . . ? C16 C17 O6 124.6(5) . . ? C18 C17 O6 116.5(5) . . ? C17 C18 C19 121.3(5) . . ? C17 C18 O5 119.6(5) . . ? C19 C18 O5 119.1(5) . . ? C18 C19 C20 120.8(5) . . ? C15 C20 C19 117.8(5) . . ? C15 C20 C21 123.6(4) . . ? C19 C20 C21 118.6(5) . . ? C1 C21 C20 113.2(5) . . ? O1 C23 O2 120.9(8) . . ? O1 C23 C24 123.8(7) . . ? O2 C23 C24 115.3(7) . . ? C25 C24 C29 116.7(8) . . ? C25 C24 C23 123.7(8) . . ? C29 C24 C23 119.5(8) . . ? C24 C25 C26 123.1(8) . . ? C27 C26 C25 119.2(9) . . ? C30A C27 C26 115.4(16) . . ? C30A C27 C28 123.7(14) . . ? C26 C27 C28 118.5(8) . . ? C30A C27 C30B 32.2(12) . . ? C26 C27 C30B 117.5(14) . . ? C28 C27 C30B 121.1(14) . . ? C29 C28 C27 121.8(10) . . ? C28 C29 C24 120.6(9) . . ? O4 C36 O5 122.2(5) . . ? O4 C36 C37 123.5(6) . . ? O5 C36 C37 114.2(6) . . ? C42 C37 C38 121.2(5) . . ? C42 C37 C36 121.6(5) . . ? C38 C37 C36 117.2(6) . . ? C39 C38 C37 117.8(6) . . ? C40 C39 C38 121.8(5) . . ? C39 C40 C41 119.6(5) . . ? C39 C40 C43 120.4(6) . . ? C41 C40 C43 120.0(6) . . ? C40 C41 C42 119.7(6) . . ? C37 C42 C41 119.8(6) . . ? C44 C43 C47B 104.2(10) . . ? C44 C43 C47A 113.2(7) . . ? C47B C43 C47A 50.9(10) . . ? C44 C43 C40 123.4(7) . . ? C47B C43 C40 123.2(8) . . ? C47A C43 C40 120.1(7) . . ? C43 C44 C45 122.5(7) . . ? N2 C45 C44 127.1(7) . . ? N2 C45 C46B 40.0(6) . . ? C44 C45 C46B 92.0(7) . . ? O7 C49 O8 121.8(5) . . ? O7 C49 C50 125.6(5) . . ? O8 C49 C50 112.5(5) . . ? C51 C50 C55 118.9(5) . . ? C51 C50 C49 118.0(5) . . ? C55 C50 C49 123.1(5) . . ? C50 C51 C52 120.5(5) . . ? C53 C52 C51 122.1(5) . . ? C52 C53 C54 117.0(5) . . ? C52 C53 C56 121.4(5) . . ? C54 C53 C56 121.6(5) . . ? C55 C54 C53 120.5(5) . . ? C54 C55 C50 121.0(5) . . ? C57B C56 C60B 117.6(7) . . ? C57B C56 C57A 79.7(11) . . ? C60B C56 C57A 64.2(10) . . ? C57B C56 C53 119.4(7) . . ? C60B C56 C53 122.9(7) . . ? C57A C56 C53 123.4(8) . . ? C57B C56 C60A 59.9(10) . . ? C60B C56 C60A 87.0(11) . . ? C57A C56 C60A 111.0(10) . . ? C53 C56 C60A 124.8(8) . . ? O11A Co2A O11A 180.000(3) . 2_857 ? O11A Co2A N1A 90.9(7) . . ? O11A Co2A N1A 89.1(7) 2_857 . ? O11A Co2A N1A 89.1(7) . 2_857 ? O11A Co2A N1A 90.9(7) 2_857 2_857 ? N1A Co2A N1A 180.0(8) . 2_857 ? O11B Co2B O11B 85.9(8) 2_857 . ? O11B Co2B Co2B 62.8(7) 2_857 2_857 ? O11B Co2B Co2B 23.2(3) . 2_857 ? O11B Co2B N1B 76.3(10) 2_857 . ? O11B Co2B N1B 68.8(8) . . ? Co2B Co2B N1B 65.4(8) 2_857 . ? O11B Co2B N1B 78.7(10) 2_857 2_857 ? O11B Co2B N1B 60.0(7) . 2_857 ? Co2B Co2B N1B 58.5(7) 2_857 2_857 ? N1B Co2B N1B 123.9(7) . 2_857 ? C27 C30A C34A 131(2) . . ? C27 C30A C31A 117(2) . . ? C34A C30A C31A 113(2) . . ? C32A C31A C30A 120(2) . . ? N1A C32A C31A 125(2) . . ? C32A N1A C33A 113(2) . . ? C32A N1A Co2A 109.1(16) . . ? C33A N1A Co2A 135.2(19) . . ? C34A C33A N1A 122(3) . . ? C33A C34A C30A 127(3) . . ? N2 C46A C47A 123.4(10) . . ? C46A C47A C43 116.2(10) . . ? C56 C57A C58A 119.1(15) . . ? N3 C58A C57A 130.9(19) . . ? N3 C59A C60A 123.7(14) . . ? C59A C60A C56 117.0(15) . . ? C31B C30B C34B 131(3) . . ? C31B C30B C27 119(3) . . ? C34B C30B C27 105(3) . . ? C30B C31B C32B 109(3) . . ? N1B C32B C31B 127(3) . . ? C32B N1B C33B 119(3) . . ? C32B N1B Co2B 106(2) . . ? C33B N1B Co2B 132(2) . . ? C32B N1B Co2B 115(2) . 2_857 ? C33B N1B Co2B 112(2) . 2_857 ? Co2B N1B Co2B 56.1(7) . 2_857 ? N1B C33B C34B 122(4) . . ? C30B C34B C33B 111(3) . . ? N2 C46B C47B 119.4(15) . . ? N2 C46B C45 36.7(7) . . ? C47B C46B C45 88.5(13) . . ? C43 C47B C46B 124.1(14) . . ? C56 C57B C58B 121.3(10) . . ? N3 C58B C57B 126.5(10) . . ? N3 C59B C60B 122.8(10) . . ? C56 C60B C59B 120.8(9) . . ? Co2B O11B Co2B 94.1(8) 2_857 . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 20.81 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.722 _refine_diff_density_min -0.799 _refine_diff_density_rms 0.067 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.014 -0.007 -0.008 2073 599 ' ' _platon_squeeze_details ; Four DMF solvent molecules per unit cell that were not found in the crystal structure but were consistent with TGA measurements were included in the formula ; # Attachment '- complex6_new.CIF' data_complex6_new _database_code_depnum_ccdc_archive 'CCDC 822485' #TrackingRef '- complex6_new.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; diaquonitrito[(+-)-2,7,12-trimethoxy-3,8,13- tris[3-(4-pyridyl)benzoyl]-10,15-dihydro-5H- tribenzo[a,d,g]cyclononane]cobalt(II) nitrate ; _chemical_name_common ; diaquonitrito((+-)-2,7,12-trimethoxy-3,8,13-tris(3-(4- pyridyl)benzoyl)-10,15-dihydro-5H-tribenzo(a,d,g)cyclononane)cobalt(ii) nitrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C73.50 H81.50 Co N11.50 O22' _chemical_formula_weight 1536.93 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' Co Co 0.3494 0.9721 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.379(2) _cell_length_b 18.072(4) _cell_length_c 21.416(4) _cell_angle_alpha 105.58(3) _cell_angle_beta 94.60(3) _cell_angle_gamma 94.50(3) _cell_volume 4205.5(14) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description pink _exptl_crystal_colour needle _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1612 _exptl_absorpt_coefficient_mu 0.278 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9622 _exptl_absorpt_correction_T_max 0.9872 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.68890 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Diamond Light Source station I19' _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'Rigaku Saturn CCD' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21516 _diffrn_reflns_av_R_equivalents 0.0853 _diffrn_reflns_av_sigmaI/netI 0.1090 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14861 _reflns_number_gt 7779 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour)' _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. One pyridylphenyl group was refined across two positions with an isotropic refinement. Co1 has a symmetry-imposed disorder. Bond length restraints were applied to a nitrate anion. Not all nitrates were located but are included in the formula. ; _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^)+(0.1000P)^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 14861 _refine_ls_number_parameters 704 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1413 _refine_ls_R_factor_gt 0.1117 _refine_ls_wR_factor_ref 0.2963 _refine_ls_wR_factor_gt 0.2713 _refine_ls_goodness_of_fit_ref 1.359 _refine_ls_restrained_S_all 1.359 _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 Co1 Co 1.54438(16) -0.47499(8) 0.52688(8) 0.0816(5) Uani 0.50 1 d P . . O1 O 0.4759(2) 0.10021(15) 0.47310(12) 0.0513(7) Uani 1 1 d . . . N1 N 0.0931(3) -0.0048(2) 0.09082(17) 0.0603(9) Uani 1 1 d . . . C1 C 0.7608(4) 0.2077(2) 0.54889(18) 0.0510(10) Uani 1 1 d . . . Co2 Co 0.0000 0.0000 0.0000 0.0569(3) Uani 1 2 d S . . O2 O 0.3977(2) 0.22109(19) 0.55609(15) 0.0718(9) Uani 1 1 d . . . N2 N 0.1230(3) 0.0902(2) 0.98981(18) 0.0681(10) Uani 1 1 d . . . C2 C 0.6734(3) 0.1534(2) 0.50909(18) 0.0473(9) Uani 1 1 d . . . H2 H 0.6969 0.1102 0.4782 0.057 Uiso 1 1 calc R . . O3 O 0.6913(3) 0.33441(17) 0.85662(14) 0.0652(8) Uani 1 1 d . . . C3 C 0.5589(4) 0.1597(2) 0.51260(18) 0.0510(9) Uani 1 1 d . . . O4 O 0.8909(3) 0.28083(19) 0.89111(15) 0.0707(8) Uani 1 1 d . . . C4 C 0.5159(4) 0.2206(3) 0.5569(2) 0.0597(11) Uani 1 1 d . . . O5 O 1.0398(2) -0.01345(19) 0.67499(13) 0.0662(8) Uani 1 1 d . . . C5 C 0.6013(4) 0.2749(2) 0.5979(2) 0.0573(10) Uani 1 1 d . . . H5 H 0.5758 0.3173 0.6288 0.069 Uiso 1 1 calc R . . O6 O 0.9117(3) -0.06495(19) 0.56040(15) 0.0695(8) Uani 1 1 d . . . C6 C 0.7207(4) 0.2701(2) 0.59586(19) 0.0526(10) Uani 1 1 d . . . O7 O 0.4525(3) 0.1691(2) 0.40230(16) 0.0853(11) Uani 1 1 d . . . C7 C 0.8065(4) 0.3289(3) 0.6440(2) 0.0577(10) Uani 1 1 d . . . H7A H 0.8817 0.3338 0.6244 0.069 Uiso 1 1 calc R . . H7B H 0.7743 0.3796 0.6527 0.069 Uiso 1 1 calc R . . O8 O 0.6339(3) 0.20969(18) 0.83977(16) 0.0692(8) Uani 1 1 d . . . C8 C 0.8319(3) 0.3103(3) 0.70635(19) 0.0564(10) Uani 1 1 d . . . O9 O 1.1776(3) -0.04120(18) 0.60574(14) 0.0655(8) Uani 1 1 d . . . C9 C 0.7532(4) 0.3271(2) 0.75154(19) 0.0546(10) Uani 1 1 d . . . H9 H 0.6821 0.3474 0.7411 0.066 Uiso 1 1 calc R . . O10 O -0.1012(3) 0.08235(19) 0.05343(13) 0.0680(8) Uani 1 1 d . . . C10 C 0.7745(4) 0.3155(2) 0.8113(2) 0.0576(11) Uani 1 1 d . . . O11 O 1.6862(7) -0.3953(4) 0.5292(4) 0.088(2) Uiso 0.50 1 d P . . C11 C 0.8772(4) 0.2888(3) 0.8296(2) 0.0596(11) Uani 1 1 d . . . O12 O 1.3714(12) -0.5343(7) 0.4806(6) 0.142(4) Uiso 0.50 1 d P . 1 C12 C 0.9573(4) 0.2716(3) 0.7858(2) 0.0608(11) Uani 1 1 d . . . H12 H 1.0294 0.2530 0.7974 0.073 Uiso 1 1 calc R . . O13 O 1.5077(6) -0.5459(3) 0.5733(3) 0.162(2) Uani 1 1 d D . . C13 C 0.9340(4) 0.2812(2) 0.7237(2) 0.0587(11) Uani 1 1 d . . . O14 O 1.6570(6) -0.4861(3) 0.6201(3) 0.0680(16) Uani 0.50 1 d PD . . C14 C 1.0253(4) 0.2523(3) 0.6757(2) 0.0605(11) Uani 1 1 d . . . H14A H 1.0269 0.2828 0.6436 0.073 Uiso 1 1 calc R . . H14B H 1.1052 0.2599 0.6999 0.073 Uiso 1 1 calc R . . O15 O 1.5668(9) -0.5530(4) 0.6796(4) 0.111(3) Uani 0.50 1 d P . . C15 C 0.9954(3) 0.1697(3) 0.6411(2) 0.0575(11) Uani 1 1 d . . . C16 C 1.0315(4) 0.1164(3) 0.6708(2) 0.0674(13) Uani 1 1 d . . . H16 H 1.0771 0.1334 0.7121 0.081 Uiso 1 1 calc R . . C17 C 1.0040(4) 0.0392(3) 0.6428(2) 0.0635(12) Uani 1 1 d . . . C18 C 0.9362(4) 0.0136(3) 0.5837(2) 0.0585(11) Uani 1 1 d . . . C19 C 0.9030(3) 0.0647(3) 0.5527(2) 0.0554(10) Uani 1 1 d . . . H19 H 0.8602 0.0464 0.5107 0.066 Uiso 1 1 calc R . . C20 C 0.9287(3) 0.1430(3) 0.57970(19) 0.0584(11) Uani 1 1 d . . . C21 C 0.8872(3) 0.1975(3) 0.54378(19) 0.0553(10) Uani 1 1 d . . . H21A H 0.9348 0.2483 0.5615 0.066 Uiso 1 1 calc R . . H21B H 0.8999 0.1778 0.4973 0.066 Uiso 1 1 calc R . . C22 C 0.4359(4) 0.1104(3) 0.41543(19) 0.0556(10) Uani 1 1 d . . . C23 C 0.3718(4) 0.0397(2) 0.37219(19) 0.0543(10) Uani 1 1 d . . . C24 C 0.3712(4) -0.0304(2) 0.38555(19) 0.0530(10) Uani 1 1 d . . . H24 H 0.4101 -0.0337 0.4255 0.064 Uiso 1 1 calc R . . C25 C 0.3150(4) -0.0955(2) 0.34178(19) 0.0565(10) Uani 1 1 d . . . H25 H 0.3146 -0.1439 0.3513 0.068 Uiso 1 1 calc R . . C26 C 0.2594(4) -0.0908(3) 0.28440(19) 0.0543(10) Uani 1 1 d . . . H26 H 0.2213 -0.1366 0.2542 0.065 Uiso 1 1 calc R . . C27 C 0.2569(3) -0.0232(3) 0.26919(18) 0.0516(10) Uani 1 1 d . . . C28 C 0.3166(3) 0.0441(3) 0.31407(19) 0.0542(10) Uani 1 1 d . . . H28 H 0.3185 0.0922 0.3040 0.065 Uiso 1 1 calc R . . C29 C 0.2004(4) -0.0161(2) 0.20844(19) 0.0556(10) Uani 1 1 d . . . C30 C 0.1917(4) -0.0764(3) 0.1517(2) 0.0638(12) Uani 1 1 d . . . H30 H 0.2213 -0.1238 0.1525 0.077 Uiso 1 1 calc R . . C31 C 0.1406(5) -0.0674(3) 0.0948(2) 0.0737(13) Uani 1 1 d . . . H31 H 0.1394 -0.1084 0.0561 0.088 Uiso 1 1 calc R . . C32 C 0.1023(4) 0.0521(3) 0.1448(2) 0.0659(12) Uani 1 1 d . . . H32 H 0.0692 0.0982 0.1430 0.079 Uiso 1 1 calc R . . C33 C 0.1559(4) 0.0493(3) 0.2029(2) 0.0672(12) Uani 1 1 d . . . H33 H 0.1622 0.0933 0.2397 0.081 Uiso 1 1 calc R . . C34 C 0.3567(4) 0.2872(3) 0.5983(3) 0.0858(16) Uani 1 1 d . . . H34A H 0.3799 0.2889 0.6438 0.129 Uiso 1 1 calc R . . H34B H 0.2702 0.2841 0.5907 0.129 Uiso 1 1 calc R . . H34C H 0.3919 0.3341 0.5894 0.129 Uiso 1 1 calc R . . C35 C 0.6250(4) 0.2747(3) 0.8663(2) 0.0612(11) Uani 1 1 d . . . C36 C 0.5360(4) 0.3011(3) 0.9125(3) 0.0757(14) Uani 1 1 d . . . C37 C 0.5271(6) 0.3780(3) 0.9421(3) 0.110(2) Uani 1 1 d . . . H37 H 0.5809 0.4174 0.9353 0.132 Uiso 1 1 calc R . . C38 C 0.4405(7) 0.3955(4) 0.9805(4) 0.152(4) Uani 1 1 d . . . H38 H 0.4311 0.4483 0.9997 0.183 Uiso 1 1 calc R . . C39 C 0.3661(8) 0.3408(4) 0.9931(4) 0.164(4) Uani 1 1 d . . . H39 H 0.3111 0.3554 1.0241 0.196 Uiso 1 1 calc R . . C40 C 0.3688(5) 0.2648(3) 0.9617(3) 0.0868(17) Uani 1 1 d . . . C41 C 0.4555(4) 0.2453(3) 0.9221(2) 0.0665(12) Uani 1 1 d . . . H41 H 0.4606 0.1925 0.9007 0.080 Uiso 1 1 calc R . . C42 C 0.2830(5) 0.2060(3) 0.9716(3) 0.0807(15) Uani 1 1 d . . . C43 C 0.2400(6) 0.1419(3) 0.9217(3) 0.0916(17) Uani 1 1 d . . . H43 H 0.2652 0.1354 0.8795 0.110 Uiso 1 1 calc R . . C44 C 0.1612(5) 0.0878(3) 0.9331(3) 0.0782(14) Uani 1 1 d . . . H44 H 0.1314 0.0449 0.8973 0.094 Uiso 1 1 calc R . . C45 C 0.1573(7) 0.1551(4) 1.0332(3) 0.114(2) Uani 1 1 d . . . H45 H 0.1224 0.1644 1.0731 0.137 Uiso 1 1 calc R . . C46 C 0.2399(7) 0.2120(3) 1.0269(3) 0.113(2) Uani 1 1 d . . . H46 H 0.2653 0.2556 1.0629 0.135 Uiso 1 1 calc R . . C47 C 1.0014(5) 0.2602(4) 0.9115(3) 0.0910(16) Uani 1 1 d . . . H47A H 1.0100 0.2070 0.8871 0.136 Uiso 1 1 calc R . . H47B H 1.0059 0.2640 0.9582 0.136 Uiso 1 1 calc R . . H47C H 1.0651 0.2952 0.9036 0.136 Uiso 1 1 calc R . . C48 C 1.1281(4) -0.0545(3) 0.6492(2) 0.0662(12) Uani 1 1 d . . . C49 C 1.1492(5) -0.1162(4) 0.6780(3) 0.0897(18) Uani 1 1 d . . . C50 C 1.1073(6) -0.1204(5) 0.7367(3) 0.138(3) Uani 1 1 d . . . H50 H 1.0425 -0.0927 0.7511 0.165 Uiso 1 1 calc R A 1 C58 C 1.3870(6) -0.3609(4) 0.5409(4) 0.0994(18) Uani 1 1 d . . . H58 H 1.3800 -0.3795 0.4947 0.119 Uiso 1 1 calc R . 1 C59 C 1.3336(6) -0.3022(3) 0.5770(3) 0.0929(18) Uani 1 1 d . . . H59 H 1.2975 -0.2715 0.5528 0.111 Uiso 1 1 calc R B 1 C60 C 0.8313(4) -0.0928(3) 0.5021(2) 0.0660(12) Uani 1 1 d . . . H60A H 0.7544 -0.0732 0.5100 0.099 Uiso 1 1 calc R . . H60B H 0.8213 -0.1494 0.4894 0.099 Uiso 1 1 calc R . . H60C H 0.8633 -0.0749 0.4669 0.099 Uiso 1 1 calc R . . N3A N 1.4520(8) -0.3877(5) 0.5839(4) 0.076(2) Uiso 0.50 1 d P . 1 C51A C 1.1532(11) -0.1605(7) 0.7720(6) 0.086(3) Uiso 0.50 1 d P . 1 H51A H 1.1462 -0.1492 0.8175 0.103 Uiso 0.50 1 calc PR . 1 C52A C 1.2107(12) -0.2185(8) 0.7416(6) 0.092(3) Uiso 0.50 1 d P . 1 H52A H 1.2246 -0.2600 0.7597 0.110 Uiso 0.50 1 calc PR . 1 C53A C 1.2502(9) -0.2161(6) 0.6813(5) 0.069(2) Uiso 0.50 1 d P . 1 C54A C 1.2222(9) -0.1552(6) 0.6565(5) 0.061(2) Uiso 0.50 1 d P . 1 H54A H 1.2624 -0.1451 0.6219 0.073 Uiso 0.50 1 calc PR . 1 C55A C 1.3215(9) -0.2769(6) 0.6494(5) 0.071(2) Uiso 0.50 1 d P . 1 C56A C 1.3982(12) -0.3100(7) 0.6795(7) 0.102(4) Uiso 0.50 1 d P . 1 H56A H 1.4101 -0.2943 0.7258 0.123 Uiso 0.50 1 calc PR . 1 C57A C 1.4628(12) -0.3680(8) 0.6452(7) 0.106(4) Uiso 0.50 1 d P . 1 H57A H 1.5149 -0.3923 0.6683 0.127 Uiso 0.50 1 calc PR . 1 N3B N 1.3674(6) -0.4380(4) 0.5298(3) 0.0611(18) Uiso 0.50 1 d P . 2 C51B C 1.1130(11) -0.2023(7) 0.7514(6) 0.083(3) Uiso 0.50 1 d P . 2 H51B H 1.0799 -0.2111 0.7885 0.100 Uiso 0.50 1 calc PR . 2 C52B C 1.1673(10) -0.2623(7) 0.7095(6) 0.084(3) Uiso 0.50 1 d P . 2 H52B H 1.1748 -0.3090 0.7211 0.101 Uiso 0.50 1 calc PR . 2 C53B C 1.2087(9) -0.2550(6) 0.6535(5) 0.062(2) Uiso 0.50 1 d P . 2 C54B C 1.1943(7) -0.1905(5) 0.6359(4) 0.0434(17) Uiso 0.50 1 d P . 2 H54B H 1.2133 -0.1901 0.5936 0.052 Uiso 0.50 1 calc PR . 2 C55B C 1.2721(9) -0.3159(5) 0.6130(5) 0.061(2) Uiso 0.50 1 d P . 2 C56B C 1.2381(10) -0.3937(6) 0.6110(5) 0.086(3) Uiso 0.50 1 d P . 2 H56B H 1.1788 -0.4072 0.6360 0.103 Uiso 0.50 1 calc PR . 2 C57B C 1.2965(7) -0.4488(5) 0.5705(4) 0.080(3) Uiso 0.50 1 d P . 2 H57B H 1.2821 -0.5003 0.5733 0.096 Uiso 0.50 1 calc PR . 2 N4 N 1.5641(7) -0.5271(5) 0.6298(4) 0.130(4) Uiso 0.50 1 d PRD . . 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 Co1 0.0906(13) 0.0648(9) 0.1066(12) 0.0333(8) 0.0550(9) 0.0315(7) O1 0.0470(16) 0.0600(16) 0.0448(15) 0.0117(13) 0.0038(12) 0.0036(12) N1 0.067(2) 0.067(2) 0.048(2) 0.0135(18) 0.0154(17) 0.0089(18) C1 0.047(2) 0.065(3) 0.042(2) 0.0124(19) 0.0123(17) 0.0116(19) Co2 0.0515(5) 0.0772(6) 0.0432(4) 0.0187(4) 0.0066(3) 0.0045(4) O2 0.0344(16) 0.096(2) 0.0687(19) -0.0071(17) 0.0094(14) 0.0133(15) N2 0.067(3) 0.088(3) 0.048(2) 0.016(2) 0.0149(18) 0.000(2) C2 0.034(2) 0.061(2) 0.044(2) 0.0083(18) 0.0075(16) 0.0047(17) O3 0.0583(19) 0.0655(18) 0.0646(18) -0.0008(15) 0.0285(15) 0.0059(15) C3 0.043(2) 0.065(2) 0.045(2) 0.0136(19) 0.0068(17) 0.0053(18) O4 0.058(2) 0.089(2) 0.0603(19) 0.0138(17) 0.0092(15) 0.0045(16) C4 0.042(2) 0.082(3) 0.050(2) 0.008(2) 0.0051(18) 0.011(2) O5 0.0473(17) 0.103(2) 0.0520(16) 0.0180(17) 0.0160(13) 0.0291(16) C5 0.040(2) 0.062(2) 0.061(2) 0.001(2) 0.0089(19) 0.0074(19) O6 0.0482(18) 0.084(2) 0.074(2) 0.0128(18) 0.0089(15) 0.0186(15) C6 0.045(2) 0.060(2) 0.048(2) 0.0067(19) 0.0084(18) 0.0008(18) O7 0.101(3) 0.081(2) 0.067(2) 0.0270(19) -0.0213(18) -0.018(2) C7 0.044(2) 0.067(3) 0.058(3) 0.010(2) 0.0126(19) 0.0008(19) O8 0.063(2) 0.0574(19) 0.083(2) 0.0061(17) 0.0244(16) 0.0065(15) C8 0.038(2) 0.071(3) 0.050(2) -0.002(2) 0.0079(18) 0.0031(19) O9 0.0566(19) 0.087(2) 0.0571(17) 0.0168(16) 0.0197(15) 0.0271(16) C9 0.038(2) 0.067(3) 0.051(2) 0.001(2) 0.0099(18) 0.0058(18) O10 0.061(2) 0.100(2) 0.0437(15) 0.0224(16) 0.0050(13) 0.0023(16) C10 0.045(2) 0.057(2) 0.063(3) -0.001(2) 0.021(2) 0.0002(19) C11 0.048(3) 0.072(3) 0.051(2) 0.006(2) 0.0069(19) 0.001(2) C12 0.051(3) 0.070(3) 0.052(2) -0.001(2) 0.008(2) 0.009(2) O13 0.220(6) 0.122(4) 0.145(4) 0.025(4) 0.002(4) 0.086(4) C13 0.044(2) 0.063(3) 0.057(3) -0.007(2) 0.0134(19) 0.0024(19) O14 0.078(4) 0.048(3) 0.082(4) 0.019(3) 0.023(3) 0.016(3) C14 0.035(2) 0.086(3) 0.052(2) 0.003(2) 0.0084(18) 0.006(2) O15 0.187(9) 0.074(5) 0.073(5) 0.026(4) 0.003(5) 0.006(5) C15 0.035(2) 0.077(3) 0.053(2) 0.000(2) 0.0107(18) 0.016(2) C16 0.045(3) 0.099(4) 0.052(2) 0.004(3) 0.019(2) 0.013(2) C17 0.054(3) 0.090(3) 0.051(2) 0.017(3) 0.021(2) 0.027(2) C18 0.036(2) 0.075(3) 0.062(3) 0.010(2) 0.0177(19) 0.010(2) C19 0.037(2) 0.076(3) 0.049(2) 0.005(2) 0.0138(17) 0.016(2) C20 0.031(2) 0.090(3) 0.048(2) 0.004(2) 0.0100(17) 0.018(2) C21 0.039(2) 0.076(3) 0.044(2) 0.004(2) 0.0171(17) -0.0045(19) C22 0.055(3) 0.063(3) 0.048(2) 0.016(2) 0.0025(19) 0.006(2) C23 0.051(3) 0.063(3) 0.046(2) 0.010(2) 0.0035(18) 0.0046(19) C24 0.056(3) 0.058(3) 0.047(2) 0.016(2) 0.0129(18) 0.0065(19) C25 0.062(3) 0.057(2) 0.049(2) 0.011(2) 0.007(2) 0.005(2) C26 0.048(2) 0.062(3) 0.051(2) 0.008(2) 0.0144(19) 0.0073(19) C27 0.042(2) 0.075(3) 0.039(2) 0.015(2) 0.0076(17) 0.0114(19) C28 0.046(2) 0.066(3) 0.050(2) 0.015(2) 0.0062(18) 0.0042(19) C29 0.063(3) 0.060(3) 0.043(2) 0.013(2) 0.0115(19) 0.003(2) C30 0.070(3) 0.073(3) 0.046(2) 0.010(2) 0.003(2) 0.016(2) C31 0.087(4) 0.077(3) 0.053(3) 0.012(2) 0.004(2) 0.010(3) C32 0.065(3) 0.079(3) 0.059(3) 0.024(3) 0.007(2) 0.023(2) C33 0.076(3) 0.076(3) 0.046(2) 0.008(2) 0.005(2) 0.018(2) C34 0.046(3) 0.106(4) 0.089(4) -0.008(3) 0.010(2) 0.033(3) C35 0.047(3) 0.074(3) 0.064(3) 0.018(2) 0.020(2) 0.001(2) C36 0.067(3) 0.064(3) 0.084(3) -0.008(3) 0.030(3) 0.010(2) C37 0.126(5) 0.058(3) 0.130(5) -0.014(3) 0.077(4) -0.005(3) C38 0.174(8) 0.080(4) 0.183(8) -0.023(4) 0.136(7) -0.020(4) C39 0.210(9) 0.072(4) 0.195(8) -0.016(5) 0.157(8) -0.024(5) C40 0.087(4) 0.077(3) 0.092(4) 0.009(3) 0.052(3) -0.006(3) C41 0.066(3) 0.072(3) 0.059(3) 0.011(2) 0.018(2) 0.002(2) C42 0.078(4) 0.082(3) 0.074(3) 0.003(3) 0.033(3) -0.004(3) C43 0.105(5) 0.084(4) 0.082(4) 0.016(3) 0.035(3) -0.016(3) C44 0.078(4) 0.088(4) 0.066(3) 0.019(3) 0.011(3) 0.000(3) C45 0.141(6) 0.110(5) 0.071(4) -0.005(4) 0.036(4) -0.040(4) C46 0.154(6) 0.081(4) 0.084(4) -0.008(3) 0.061(4) -0.040(4) C47 0.083(4) 0.110(4) 0.081(4) 0.036(3) 0.001(3) -0.006(3) C48 0.050(3) 0.096(4) 0.054(3) 0.018(3) 0.014(2) 0.020(2) C49 0.072(4) 0.148(5) 0.080(3) 0.065(4) 0.038(3) 0.048(4) C50 0.106(5) 0.236(9) 0.116(5) 0.091(6) 0.066(4) 0.091(6) C58 0.100(5) 0.083(4) 0.127(5) 0.050(4) 0.004(4) 0.012(3) C59 0.121(5) 0.062(3) 0.101(4) 0.035(3) 0.001(4) 0.010(3) C60 0.042(2) 0.072(3) 0.077(3) 0.007(2) 0.011(2) 0.011(2) _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 Co1 O12 0.993(13) 2_846 ? Co1 Co1 1.508(4) 2_846 ? Co1 O13 1.864(6) . ? Co1 O11 2.065(8) . ? Co1 N3B 2.091(7) 2_846 ? Co1 N3A 2.126(8) . ? Co1 N3B 2.171(7) . ? Co1 O12 2.188(14) . ? Co1 O14 2.348(7) . ? Co1 O13 2.315(6) 2_846 ? O1 C22 1.346(5) . ? O1 C3 1.410(5) . ? N1 C31 1.311(6) . ? N1 C32 1.315(6) . ? N1 Co2 2.165(4) . ? C1 C2 1.393(5) . ? C1 C6 1.428(5) . ? C1 C21 1.474(5) . ? Co2 O10 2.101(3) 2 ? Co2 O10 2.101(3) . ? Co2 N2 2.132(4) 2_556 ? Co2 N2 2.132(4) 1_554 ? Co2 N1 2.165(4) 2 ? O2 C4 1.344(5) . ? O2 C34 1.428(5) . ? N2 C45 1.295(7) . ? N2 C44 1.313(6) . ? N2 Co2 2.132(4) 1_556 ? C2 C3 1.323(5) . ? C2 H2 0.9500 . ? O3 C35 1.339(5) . ? O3 C10 1.405(5) . ? C3 C4 1.395(6) . ? O4 C11 1.360(5) . ? O4 C47 1.408(6) . ? C4 C5 1.389(6) . ? O5 C48 1.361(5) . ? O5 C17 1.384(5) . ? C5 C6 1.371(5) . ? C5 H5 0.9500 . ? O6 C18 1.370(5) . ? O6 C60 1.435(5) . ? C6 C7 1.494(6) . ? O7 C22 1.173(5) . ? C7 C8 1.475(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? O8 C35 1.176(5) . ? C8 C9 1.362(5) . ? C8 C13 1.377(6) . ? O9 C48 1.193(5) . ? C9 C10 1.358(6) . ? C9 H9 0.9500 . ? C10 C11 1.367(6) . ? O11 O12 1.340(13) 2_846 ? C11 C12 1.353(6) . ? O12 Co1 0.993(13) 2_846 ? O12 O11 1.340(13) 2_846 ? C12 C13 1.394(6) . ? C12 H12 0.9500 . ? O13 N4 1.271(9) . ? O13 Co1 2.315(6) 2_846 ? C13 C14 1.542(5) . ? O14 N4 1.306(9) . ? C14 C15 1.476(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? O15 N4 1.274(10) . ? C15 C16 1.361(6) . ? C15 C20 1.406(6) . ? C16 C17 1.362(7) . ? C16 H16 0.9500 . ? C17 C18 1.373(6) . ? C18 C19 1.333(6) . ? C19 C20 1.375(6) . ? C19 H19 0.9500 . ? C20 C21 1.486(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.461(6) . ? C23 C24 1.370(6) . ? C23 C28 1.373(6) . ? C24 C25 1.366(6) . ? C24 H24 0.9500 . ? C25 C26 1.363(6) . ? C25 H25 0.9500 . ? C26 C27 1.349(6) . ? C26 H26 0.9500 . ? C27 C28 1.414(6) . ? C27 C29 1.446(5) . ? C28 H28 0.9500 . ? C29 C33 1.352(6) . ? C29 C30 1.387(6) . ? C30 C31 1.364(6) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.357(6) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.488(6) . ? C36 C37 1.380(7) . ? C36 C41 1.376(7) . ? C37 C38 1.337(7) . ? C37 H37 0.9500 . ? C38 C39 1.347(9) . ? C38 H38 0.9500 . ? C39 C40 1.361(8) . ? C39 H39 0.9500 . ? C40 C41 1.359(6) . ? C40 C42 1.455(7) . ? C41 H41 0.9500 . ? C42 C46 1.299(7) . ? C42 C43 1.373(7) . ? C43 C44 1.358(7) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.379(8) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.438(7) . ? C49 C54A 1.173(10) . ? C49 C50 1.399(7) . ? C49 C54B 1.553(10) . ? C50 C51A 1.288(13) . ? C50 C51B 1.599(14) . ? C50 H50 0.9500 . ? C58 N3A 1.347(10) . ? C58 N3B 1.345(9) . ? C58 C59 1.353(8) . ? C58 H58 0.9500 . ? C59 C55B 1.142(10) . ? C59 C55A 1.515(12) . ? C59 H59 0.9500 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? N3A C57A 1.257(14) . ? C51A C52A 1.327(17) . ? C51A H51A 0.9500 . ? C52A C53A 1.412(15) . ? C52A H52A 0.9500 . ? C53A C54A 1.393(13) . ? C53A C55A 1.468(14) . ? C54A H54A 0.9500 . ? C55A C56A 1.317(15) . ? C56A C57A 1.404(17) . ? C56A H56A 0.9500 . ? C57A H57A 0.9500 . ? N3B C57B 1.277(10) . ? N3B Co1 2.091(7) 2_846 ? C51B C52B 1.427(16) . ? C51B H51B 0.9500 . ? C52B C53B 1.358(13) . ? C52B H52B 0.9500 . ? C53B C54B 1.335(11) . ? C53B C55B 1.481(13) . ? C54B H54B 0.9500 . ? C55B C56B 1.417(14) . ? C56B C57B 1.386(13) . ? C56B H56B 0.9500 . ? C57B H57B 0.9500 . ? 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 O12 Co1 Co1 120.7(7) 2_846 2_846 ? O12 Co1 O13 117.5(7) 2_846 . ? Co1 Co1 O13 86.1(2) 2_846 . ? O12 Co1 O11 32.6(7) 2_846 . ? Co1 Co1 O11 133.7(3) 2_846 . ? O13 Co1 O11 135.7(3) . . ? O12 Co1 N3B 58.3(7) 2_846 2_846 ? Co1 Co1 N3B 72.2(2) 2_846 2_846 ? O13 Co1 N3B 85.3(3) . 2_846 ? O11 Co1 N3B 89.7(3) . 2_846 ? O12 Co1 N3A 122.6(8) 2_846 . ? Co1 Co1 N3A 106.9(3) 2_846 . ? O13 Co1 N3A 94.4(3) . . ? O11 Co1 N3A 91.2(3) . . ? N3B Co1 N3A 179.0(3) 2_846 . ? O12 Co1 N3B 149.4(7) 2_846 . ? Co1 Co1 N3B 66.5(2) 2_846 . ? O13 Co1 N3B 91.8(3) . . ? O11 Co1 N3B 119.0(3) . . ? N3B Co1 N3B 138.62(16) 2_846 . ? N3A Co1 N3B 40.5(3) . . ? O12 Co1 O12 143.7(5) 2_846 . ? Co1 Co1 O12 22.9(3) 2_846 . ? O13 Co1 O12 75.1(4) . . ? O11 Co1 O12 149.1(4) . . ? N3B Co1 O12 91.6(4) 2_846 . ? N3A Co1 O12 87.5(4) . . ? N3B Co1 O12 48.3(4) . . ? O12 Co1 O14 74.1(7) 2_846 . ? Co1 Co1 O14 138.06(19) 2_846 . ? O13 Co1 O14 54.6(3) . . ? O11 Co1 O14 81.4(3) . . ? N3B Co1 O14 88.9(2) 2_846 . ? N3A Co1 O14 91.6(3) . . ? N3B Co1 O14 122.3(2) . . ? O12 Co1 O14 129.5(4) . . ? O12 Co1 O13 87.8(7) 2_846 2_846 ? Co1 Co1 O13 53.4(2) 2_846 2_846 ? O13 Co1 O13 139.48(15) . 2_846 ? O11 Co1 O13 82.7(3) . 2_846 ? N3B Co1 O13 82.4(2) 2_846 2_846 ? N3A Co1 O13 97.4(3) . 2_846 ? N3B Co1 O13 73.4(2) . 2_846 ? O12 Co1 O13 66.8(4) . 2_846 ? O14 Co1 O13 161.9(2) . 2_846 ? C22 O1 C3 115.3(3) . . ? C31 N1 C32 116.4(4) . . ? C31 N1 Co2 120.3(3) . . ? C32 N1 Co2 123.2(3) . . ? C2 C1 C6 116.5(4) . . ? C2 C1 C21 120.5(4) . . ? C6 C1 C21 123.0(4) . . ? O10 Co2 O10 180.0(3) 2 . ? O10 Co2 N2 90.18(14) 2 2_556 ? O10 Co2 N2 89.82(14) . 2_556 ? O10 Co2 N2 89.82(14) 2 1_554 ? O10 Co2 N2 90.18(14) . 1_554 ? N2 Co2 N2 180.0(2) 2_556 1_554 ? O10 Co2 N1 90.97(12) 2 . ? O10 Co2 N1 89.03(12) . . ? N2 Co2 N1 86.70(14) 2_556 . ? N2 Co2 N1 93.30(14) 1_554 . ? O10 Co2 N1 89.03(12) 2 2 ? O10 Co2 N1 90.97(12) . 2 ? N2 Co2 N1 93.30(14) 2_556 2 ? N2 Co2 N1 86.70(14) 1_554 2 ? N1 Co2 N1 180.00(9) . 2 ? C4 O2 C34 116.3(4) . . ? C45 N2 C44 112.5(5) . . ? C45 N2 Co2 126.5(3) . 1_556 ? C44 N2 Co2 120.6(4) . 1_556 ? C3 C2 C1 122.5(4) . . ? C3 C2 H2 118.7 . . ? C1 C2 H2 118.7 . . ? C35 O3 C10 116.0(3) . . ? C2 C3 C4 122.8(4) . . ? C2 C3 O1 119.1(4) . . ? C4 C3 O1 117.9(3) . . ? C11 O4 C47 116.5(4) . . ? O2 C4 C5 126.5(4) . . ? O2 C4 C3 117.7(4) . . ? C5 C4 C3 115.8(4) . . ? C48 O5 C17 114.8(3) . . ? C6 C5 C4 123.1(4) . . ? C6 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C18 O6 C60 116.3(4) . . ? C5 C6 C1 119.3(4) . . ? C5 C6 C7 119.6(4) . . ? C1 C6 C7 121.1(4) . . ? C8 C7 C6 113.7(4) . . ? C8 C7 H7A 108.8 . . ? C6 C7 H7A 108.8 . . ? C8 C7 H7B 108.8 . . ? C6 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C9 C8 C13 117.4(4) . . ? C9 C8 C7 118.3(4) . . ? C13 C8 C7 124.2(4) . . ? C10 C9 C8 121.3(4) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C11 121.7(4) . . ? C9 C10 O3 119.3(4) . . ? C11 C10 O3 118.9(4) . . ? O12 O11 Co1 23.5(6) 2_846 . ? C12 C11 O4 124.6(4) . . ? C12 C11 C10 118.4(4) . . ? O4 C11 C10 117.0(4) . . ? Co1 O12 O11 123.9(12) 2_846 2_846 ? Co1 O12 Co1 36.3(5) 2_846 . ? O11 O12 Co1 136.5(8) 2_846 . ? C11 C12 C13 120.0(4) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? N4 O13 Co1 112.1(6) . . ? N4 O13 Co1 152.6(6) . 2_846 ? Co1 O13 Co1 40.52(15) . 2_846 ? C8 C13 C12 121.1(4) . . ? C8 C13 C14 123.1(4) . . ? C12 C13 C14 115.6(4) . . ? N4 O14 Co1 86.7(5) . . ? C15 C14 C13 111.0(3) . . ? C15 C14 H14A 109.4 . . ? C13 C14 H14A 109.4 . . ? C15 C14 H14B 109.4 . . ? C13 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C16 C15 C20 118.1(4) . . ? C16 C15 C14 118.3(4) . . ? C20 C15 C14 123.6(4) . . ? C15 C16 C17 121.7(4) . . ? C15 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C16 C17 C18 119.9(5) . . ? C16 C17 O5 120.2(4) . . ? C18 C17 O5 119.8(5) . . ? C19 C18 O6 125.3(4) . . ? C19 C18 C17 119.4(5) . . ? O6 C18 C17 115.3(4) . . ? C18 C19 C20 122.2(4) . . ? C18 C19 H19 118.9 . . ? C20 C19 H19 118.9 . . ? C19 C20 C15 118.7(4) . . ? C19 C20 C21 120.0(4) . . ? C15 C20 C21 121.3(4) . . ? C1 C21 C20 111.9(3) . . ? C1 C21 H21A 109.2 . . ? C20 C21 H21A 109.2 . . ? C1 C21 H21B 109.2 . . ? C20 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? O7 C22 O1 123.3(4) . . ? O7 C22 C23 125.2(4) . . ? O1 C22 C23 111.5(4) . . ? C24 C23 C28 119.6(4) . . ? C24 C23 C22 122.8(4) . . ? C28 C23 C22 117.4(4) . . ? C25 C24 C23 120.4(4) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C26 C25 C24 119.7(4) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C27 C26 C25 122.0(4) . . ? C27 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? C26 C27 C28 118.2(4) . . ? C26 C27 C29 123.6(4) . . ? C28 C27 C29 118.2(4) . . ? C23 C28 C27 119.9(4) . . ? C23 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C33 C29 C30 116.1(4) . . ? C33 C29 C27 122.6(4) . . ? C30 C29 C27 121.2(4) . . ? C31 C30 C29 119.9(4) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? N1 C31 C30 123.1(5) . . ? N1 C31 H31 118.4 . . ? C30 C31 H31 118.4 . . ? N1 C32 C33 124.3(4) . . ? N1 C32 H32 117.8 . . ? C33 C32 H32 117.8 . . ? C29 C33 C32 119.9(4) . . ? C29 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? O2 C34 H34A 109.5 . . ? O2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O8 C35 O3 123.8(4) . . ? O8 C35 C36 124.5(4) . . ? O3 C35 C36 111.6(4) . . ? C37 C36 C41 119.8(4) . . ? C37 C36 C35 122.9(5) . . ? C41 C36 C35 117.2(4) . . ? C38 C37 C36 117.9(5) . . ? C38 C37 H37 121.0 . . ? C36 C37 H37 121.0 . . ? C37 C38 C39 122.3(6) . . ? C37 C38 H38 118.9 . . ? C39 C38 H38 118.9 . . ? C38 C39 C40 120.7(5) . . ? C38 C39 H39 119.6 . . ? C40 C39 H39 119.6 . . ? C41 C40 C39 118.1(5) . . ? C41 C40 C42 121.0(5) . . ? C39 C40 C42 120.9(5) . . ? C40 C41 C36 120.9(5) . . ? C40 C41 H41 119.6 . . ? C36 C41 H41 119.6 . . ? C46 C42 C43 116.2(5) . . ? C46 C42 C40 122.5(5) . . ? C43 C42 C40 121.3(5) . . ? C44 C43 C42 119.5(5) . . ? C44 C43 H43 120.2 . . ? C42 C43 H43 120.2 . . ? N2 C44 C43 125.1(5) . . ? N2 C44 H44 117.4 . . ? C43 C44 H44 117.4 . . ? N2 C45 C46 125.9(5) . . ? N2 C45 H45 117.0 . . ? C46 C45 H45 117.0 . . ? C42 C46 C45 120.0(6) . . ? C42 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? O4 C47 H47A 109.5 . . ? O4 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? O4 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? O9 C48 O5 122.2(4) . . ? O9 C48 C49 125.3(4) . . ? O5 C48 C49 112.5(4) . . ? C54A C49 C50 119.8(7) . . ? C54A C49 C48 115.7(6) . . ? C50 C49 C48 123.0(5) . . ? C54A C49 C54B 25.5(5) . . ? C50 C49 C54B 116.7(6) . . ? C48 C49 C54B 118.8(5) . . ? C51A C50 C49 122.6(7) . . ? C51A C50 C51B 31.6(6) . . ? C49 C50 C51B 114.7(7) . . ? C51A C50 H50 118.7 . . ? C49 C50 H50 118.7 . . ? C51B C50 H50 116.8 . . ? N3A C58 N3B 67.1(5) . . ? N3A C58 C59 105.8(7) . . ? N3B C58 C59 131.9(6) . . ? N3A C58 H58 127.1 . . ? N3B C58 H58 76.7 . . ? C59 C58 H58 127.1 . . ? C55B C59 C58 117.7(7) . . ? C55B C59 C55A 41.1(6) . . ? C58 C59 C55A 131.2(6) . . ? C55B C59 H59 110.4 . . ? C58 C59 H59 114.4 . . ? C55A C59 H59 114.4 . . ? O6 C60 H60A 109.5 . . ? O6 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? O6 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C57A N3A C58 130.8(10) . . ? C57A N3A Co1 123.5(9) . . ? C58 N3A Co1 105.7(6) . . ? C50 C51A C52A 116.5(12) . . ? C50 C51A H51A 121.8 . . ? C52A C51A H51A 121.8 . . ? C51A C52A C53A 117.4(11) . . ? C51A C52A H52A 121.3 . . ? C53A C52A H52A 121.3 . . ? C54A C53A C52A 118.1(10) . . ? C54A C53A C55A 123.9(9) . . ? C52A C53A C55A 118.0(9) . . ? C49 C54A C53A 120.3(9) . . ? C49 C54A H54A 119.8 . . ? C53A C54A H54A 119.8 . . ? C56A C55A C53A 125.6(10) . . ? C56A C55A C59 108.6(9) . . ? C53A C55A C59 125.2(8) . . ? C55A C56A C57A 121.9(13) . . ? C55A C56A H56A 119.0 . . ? C57A C56A H56A 119.0 . . ? N3A C57A C56A 120.2(13) . . ? N3A C57A H57A 119.9 . . ? C56A C57A H57A 119.9 . . ? C57B N3B C58 105.8(7) . . ? C57B N3B Co1 123.9(6) . 2_846 ? C58 N3B Co1 129.3(5) . 2_846 ? C57B N3B Co1 124.1(6) . . ? C58 N3B Co1 103.4(5) . . ? Co1 N3B Co1 41.38(16) 2_846 . ? C52B C51B C50 120.6(10) . . ? C52B C51B H51B 119.7 . . ? C50 C51B H51B 119.7 . . ? C53B C52B C51B 122.3(11) . . ? C53B C52B H52B 118.9 . . ? C51B C52B H52B 118.9 . . ? C54B C53B C52B 118.8(9) . . ? C54B C53B C55B 119.8(8) . . ? C52B C53B C55B 121.3(9) . . ? C53B C54B C49 126.2(7) . . ? C53B C54B H54B 116.9 . . ? C49 C54B H54B 116.9 . . ? C59 C55B C56B 120.1(9) . . ? C59 C55B C53B 120.9(9) . . ? C56B C55B C53B 118.0(9) . . ? C57B C56B C55B 116.0(10) . . ? C57B C56B H56B 122.0 . . ? C55B C56B H56B 122.0 . . ? N3B C57B C56B 127.0(9) . . ? N3B C57B H57B 116.5 . . ? C56B C57B H57B 116.5 . . ? O13 N4 O15 136.4(9) . . ? O13 N4 O14 100.4(7) . . ? O15 N4 O14 119.8(8) . . ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.915 _refine_diff_density_max 0.924 _refine_diff_density_min -0.742 _refine_diff_density_rms 0.099 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.114 0.348 0.085 1963 656 ' ' _platon_squeeze_details ; TGA analysis indicates that the crystals contain nine additional dimethylformamide molecules per unit cell that were not located crystallographically. These were included in formula, etc. ;