Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Leonard Lindoy' _publ_contact_author_address ; School of Chemistry F11 University of Sydney Sydney NSW 2006. AUSTRALIA ; _publ_contact_author_email LINDOY@CHEM.USYD.EDU.AU _publ_section_title ; Neutral (bis-beta-diketonato) iron(III), cobalt(II), nickel(II), copper(II) and zinc(II) metallocycles: structural, electrochemical and solvent extraction studies ; loop_ _publ_author_name 'Leonard Lindoy' 'David J. Bray' 'Jack K. Clegg' 'Kerstin Gloe' 'Karsten Gloe' 'Michael J. Hayter' ; K.A.Jolliffe ; 'G. A. Lawrance' 'John C. McMurtrie' 'George V. Meehan' 'Marco Wenzel' data_lj28sad _database_code_depnum_ccdc_archive 'CCDC 635435' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H60 Co2 N4 O8, 2.25(C H Cl3), 0.5(H2 O)' _chemical_formula_sum 'C58.25 H63.25 Cl6.75 Co2 N4 O8.5' _chemical_formula_weight 1312.53 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 39.887(3) _cell_length_b 14.9550(12) _cell_length_c 22.3180(18) _cell_angle_alpha 90.00 _cell_angle_beta 113.9660(10) _cell_angle_gamma 90.00 _cell_volume 12165.2(17) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14862 _cell_measurement_theta_min 2.160 _cell_measurement_theta_max 28.197 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5420 _exptl_absorpt_coefficient_mu 0.898 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.743 _exptl_absorpt_correction_T_max 0.922 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; The crystal was coated in Exxon Paratone N hydrocarbon oil and mounted on a thin mohair fibre attached to a copper pin. Upon mounting on the diffractometer, the crystal was quenched to 150(K) under a cold nitrogen gas stream supplied by an Oxford Cryosystems Cryostream and data were collected at this temperature. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 149 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.19 _diffrn_reflns_number 58133 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -52 _diffrn_reflns_limit_h_max 53 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 28.40 _reflns_number_total 14591 _reflns_number_gt 9578 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker,1995)' _computing_cell_refinement 'SAINT (Bruker,1995)' _computing_data_reduction 'SAINT and XPREP (Bruker, 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEPIII (Farrugia, 1997) WINGX-32 (Farrugia, 1999) ; _computing_publication_material 'enCIFer 1.0 (CCDC, 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+100.0000P] 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 14591 _refine_ls_number_parameters 727 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.1084 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.1506 _refine_ls_wR_factor_gt 0.1330 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.063 _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 C1A C 0.66651(15) 0.3980(4) -0.1399(2) 0.0570(14) Uani 0.50 1 d P A 1 H1A1 H 0.6400 0.3923 -0.1659 0.085 Uiso 0.50 1 calc PR A 1 H1A2 H 0.6792 0.3466 -0.1485 0.085 Uiso 0.50 1 calc PR A 1 H1A3 H 0.6754 0.4532 -0.1521 0.085 Uiso 0.50 1 calc PR A 1 C2A C 0.6742(3) 0.4008(7) -0.0665(4) 0.043(2) Uiso 0.50 1 d P A 1 H2A1 H 0.6617 0.4536 -0.0582 0.051 Uiso 0.50 1 calc PR A 1 H2A2 H 0.6635 0.3468 -0.0554 0.051 Uiso 0.50 1 calc PR A 1 C3A C 0.71190(15) 0.4051(5) -0.0247(2) 0.0738(19) Uani 0.50 1 d PU A 1 H3A1 H 0.7208 0.4646 -0.0312 0.089 Uiso 0.50 1 calc PR A 1 H3A2 H 0.7246 0.3603 -0.0408 0.089 Uiso 0.50 1 calc PR A 1 C1B C 0.66651(15) 0.3980(4) -0.1399(2) 0.0570(14) Uani 0.50 1 d P A 2 H1B1 H 0.6469 0.3584 -0.1685 0.085 Uiso 0.50 1 calc PR A 2 H1B2 H 0.6855 0.4035 -0.1571 0.085 Uiso 0.50 1 calc PR A 2 H1B3 H 0.6563 0.4571 -0.1385 0.085 Uiso 0.50 1 calc PR A 2 C2B C 0.6838(2) 0.3577(6) -0.0690(4) 0.0340(18) Uiso 0.50 1 d P A 2 H2B1 H 0.6643 0.3521 -0.0526 0.041 Uiso 0.50 1 calc PR A 2 H2B2 H 0.6928 0.2966 -0.0716 0.041 Uiso 0.50 1 calc PR A 2 C3B C 0.71190(15) 0.4051(5) -0.0247(2) 0.0738(19) Uani 0.50 1 d P A 2 H3B1 H 0.7052 0.4690 -0.0332 0.089 Uiso 0.50 1 calc PR A 2 H3B2 H 0.7334 0.3955 -0.0355 0.089 Uiso 0.50 1 calc PR A 2 C4 C 0.72501(11) 0.3911(3) 0.04848(18) 0.0333(9) Uani 1 1 d . . . C5 C 0.76266(10) 0.3840(3) 0.08584(18) 0.0305(8) Uani 1 1 d . A . H5 H 0.7782 0.3879 0.0630 0.037 Uiso 1 1 calc R . . C6 C 0.77983(10) 0.3718(2) 0.15409(17) 0.0242(7) Uani 1 1 d . . . C7 C 0.82062(10) 0.3613(2) 0.18774(18) 0.0263(8) Uani 1 1 d . A . C8 C 0.84313(11) 0.3483(3) 0.1540(2) 0.0357(9) Uani 1 1 d . . . H8 H 0.8327 0.3484 0.1074 0.043 Uiso 1 1 calc R A . C9 C 0.88019(12) 0.3352(3) 0.1878(2) 0.0452(11) Uani 1 1 d . A . H9 H 0.8951 0.3258 0.1642 0.054 Uiso 1 1 calc R . . C10 C 0.89616(12) 0.3356(3) 0.2553(2) 0.0417(10) Uani 1 1 d . . . H10 H 0.9219 0.3270 0.2779 0.050 Uiso 1 1 calc R A . C11 C 0.87461(11) 0.3487(3) 0.29076(19) 0.0319(8) Uani 1 1 d . A . C12 C 0.83731(10) 0.3616(2) 0.25599(18) 0.0272(8) Uani 1 1 d . . . H12 H 0.8225 0.3710 0.2796 0.033 Uiso 1 1 calc R A . C13 C 0.89020(11) 0.3499(3) 0.3646(2) 0.0363(9) Uani 1 1 d . . . C14 C 0.92668(11) 0.3258(3) 0.4013(2) 0.0433(11) Uani 1 1 d . A . H14 H 0.9401 0.3028 0.3779 0.052 Uiso 1 1 calc R . . C15 C 0.94534(11) 0.3326(4) 0.4699(2) 0.0455(11) Uani 1 1 d . . . C16 C 0.98475(12) 0.3016(4) 0.5028(2) 0.0526(13) Uani 1 1 d . A . H16A H 1.0002 0.3517 0.5285 0.063 Uiso 1 1 calc R . . H16B H 0.9935 0.2847 0.4688 0.063 Uiso 1 1 calc R . . C17 C 0.98932(14) 0.2218(4) 0.5484(3) 0.0633(15) Uani 1 1 d . . . H17A H 1.0158 0.2090 0.5725 0.076 Uiso 1 1 calc R A . H17B H 0.9794 0.2378 0.5810 0.076 Uiso 1 1 calc R . . C18 C 0.97025(17) 0.1382(4) 0.5125(3) 0.0772(18) Uani 1 1 d . A . H18A H 0.9744 0.0894 0.5440 0.116 Uiso 1 1 calc R . . H18B H 0.9801 0.1215 0.4804 0.116 Uiso 1 1 calc R . . H18C H 0.9439 0.1496 0.4898 0.116 Uiso 1 1 calc R . . C19 C 0.59133(15) 0.5584(4) 0.1712(3) 0.0696(17) Uani 1 1 d . . . H19A H 0.5813 0.6137 0.1471 0.104 Uiso 1 1 calc R . . H19B H 0.6181 0.5629 0.1931 0.104 Uiso 1 1 calc R . . H19C H 0.5812 0.5490 0.2041 0.104 Uiso 1 1 calc R . . C20 C 0.58100(13) 0.4803(4) 0.1239(2) 0.0496(12) Uani 1 1 d . . . H20A H 0.5908 0.4911 0.0903 0.060 Uiso 1 1 calc R . . H20B H 0.5539 0.4772 0.1013 0.060 Uiso 1 1 calc R . . C21 C 0.59539(11) 0.3905(3) 0.1569(2) 0.0390(10) Uani 1 1 d . . . H21A H 0.5864 0.3806 0.1917 0.047 Uiso 1 1 calc R . . H21B H 0.5854 0.3422 0.1240 0.047 Uiso 1 1 calc R . . C22 C 0.63690(10) 0.3846(3) 0.18688(19) 0.0294(8) Uani 1 1 d . . . C23 C 0.65528(10) 0.3761(3) 0.25532(18) 0.0282(8) Uani 1 1 d . . . H23 H 0.6407 0.3756 0.2801 0.034 Uiso 1 1 calc R . . C24 C 0.69341(10) 0.3682(2) 0.29001(17) 0.0233(7) Uani 1 1 d . . . C25 C 0.70992(10) 0.3630(2) 0.36397(17) 0.0242(7) Uani 1 1 d . . . C26 C 0.68931(11) 0.3440(3) 0.39997(19) 0.0329(9) Uani 1 1 d . . . H26 H 0.6637 0.3329 0.3780 0.040 Uiso 1 1 calc R . . C27 C 0.70613(12) 0.3414(3) 0.4677(2) 0.0438(11) Uani 1 1 d . . . H27 H 0.6920 0.3281 0.4921 0.053 Uiso 1 1 calc R . . C28 C 0.74323(12) 0.3577(3) 0.5003(2) 0.0412(10) Uani 1 1 d . . . H28 H 0.7543 0.3569 0.5469 0.049 Uiso 1 1 calc R . . C29 C 0.76483(10) 0.3755(3) 0.46544(18) 0.0281(8) Uani 1 1 d . . . C30 C 0.74754(10) 0.3772(2) 0.39729(17) 0.0242(7) Uani 1 1 d . . . H30 H 0.7618 0.3883 0.3728 0.029 Uiso 1 1 calc R . . C31 C 0.80550(11) 0.3886(3) 0.49819(18) 0.0314(8) Uani 1 1 d . . . C32 C 0.82264(12) 0.4009(3) 0.56631(19) 0.0379(10) Uani 1 1 d . . . H32 H 0.8070 0.4072 0.5889 0.045 Uiso 1 1 calc R . . C33 C 0.86029(12) 0.4049(3) 0.6041(2) 0.0405(10) Uani 1 1 d . . . C34 C 0.87358(13) 0.4161(4) 0.6779(2) 0.0518(13) Uani 1 1 d . . . H34A H 0.8850 0.4759 0.6903 0.062 Uiso 1 1 calc R . . H34B H 0.8521 0.4141 0.6895 0.062 Uiso 1 1 calc R . . C35 C 0.90047(16) 0.3473(4) 0.7168(2) 0.0614(15) Uani 1 1 d . . . H35A H 0.9224 0.3507 0.7066 0.074 Uiso 1 1 calc R . . H35B H 0.8894 0.2873 0.7036 0.074 Uiso 1 1 calc R . . C36 C 0.91233(15) 0.3583(4) 0.7902(2) 0.0605(15) Uani 1 1 d . . . H36A H 0.9299 0.3112 0.8134 0.091 Uiso 1 1 calc R . . H36B H 0.8908 0.3540 0.8008 0.091 Uiso 1 1 calc R . . H36C H 0.9239 0.4169 0.8039 0.091 Uiso 1 1 calc R . . C37 C 0.68277(11) 0.1858(3) 0.18359(19) 0.0302(8) Uani 1 1 d . . . H37 H 0.6692 0.2180 0.2030 0.036 Uiso 1 1 calc R . . C38 C 0.68091(11) 0.0938(3) 0.1830(2) 0.0338(9) Uani 1 1 d . . . H38 H 0.6665 0.0638 0.2018 0.041 Uiso 1 1 calc R . . C39 C 0.70020(12) 0.0464(3) 0.1548(2) 0.0408(10) Uani 1 1 d . . . H39 H 0.6994 -0.0171 0.1536 0.049 Uiso 1 1 calc R . . C40 C 0.72090(13) 0.0930(3) 0.1282(2) 0.0459(12) Uani 1 1 d . . . H40 H 0.7346 0.0620 0.1084 0.055 Uiso 1 1 calc R . . C41 C 0.72136(12) 0.1850(3) 0.1308(2) 0.0375(10) Uani 1 1 d . . . H41 H 0.7356 0.2164 0.1124 0.045 Uiso 1 1 calc R . . C42 C 0.73474(11) 0.5694(3) 0.15721(19) 0.0322(9) Uani 1 1 d . . . H42 H 0.7463 0.5391 0.1332 0.039 Uiso 1 1 calc R . . C43 C 0.73997(12) 0.6603(3) 0.1665(2) 0.0354(9) Uani 1 1 d . . . H43 H 0.7548 0.6915 0.1493 0.042 Uiso 1 1 calc R . . C44 C 0.72349(12) 0.7054(3) 0.20091(19) 0.0349(9) Uani 1 1 d . . . H44 H 0.7267 0.7680 0.2081 0.042 Uiso 1 1 calc R . . C45 C 0.70204(12) 0.6571(3) 0.2248(2) 0.0361(9) Uani 1 1 d . . . H45 H 0.6900 0.6862 0.2485 0.043 Uiso 1 1 calc R . . C46 C 0.69828(12) 0.5663(3) 0.21389(19) 0.0328(9) Uani 1 1 d . . . H46 H 0.6837 0.5338 0.2310 0.039 Uiso 1 1 calc R . . C47 C 0.86105(12) 0.1795(4) 0.4504(2) 0.0522(13) Uani 1 1 d . . . H47 H 0.8485 0.2033 0.4075 0.063 Uiso 1 1 calc R . . C48 C 0.86200(14) 0.0878(4) 0.4583(3) 0.0618(15) Uani 1 1 d . . . H48 H 0.8503 0.0498 0.4216 0.074 Uiso 1 1 calc R . . C49 C 0.87983(15) 0.0526(4) 0.5194(3) 0.0657(15) Uani 1 1 d . . . H49 H 0.8808 -0.0103 0.5259 0.079 Uiso 1 1 calc R . . C50 C 0.89656(15) 0.1097(4) 0.5719(3) 0.0636(15) Uani 1 1 d . . . H50 H 0.9091 0.0868 0.6150 0.076 Uiso 1 1 calc R . . C51 C 0.89464(13) 0.1998(4) 0.5605(2) 0.0537(13) Uani 1 1 d . . . H51 H 0.9063 0.2388 0.5966 0.064 Uiso 1 1 calc R . . C52 C 0.90668(13) 0.5645(4) 0.4577(2) 0.0584(15) Uani 1 1 d . . . H52 H 0.9213 0.5270 0.4437 0.070 Uiso 1 1 calc R . . C53 C 0.90916(15) 0.6566(4) 0.4529(3) 0.0640(16) Uani 1 1 d . . . H53 H 0.9264 0.6811 0.4380 0.077 Uiso 1 1 calc R . . C54 C 0.88689(18) 0.7133(4) 0.4695(3) 0.0677(16) Uani 1 1 d . . . H54 H 0.8872 0.7761 0.4635 0.081 Uiso 1 1 calc R . . C55 C 0.86452(18) 0.6751(4) 0.4947(3) 0.0661(16) Uani 1 1 d . . . H55 H 0.8494 0.7116 0.5083 0.079 Uiso 1 1 calc R . . C56 C 0.86382(16) 0.5829(4) 0.5006(2) 0.0574(14) Uani 1 1 d . . . H56 H 0.8482 0.5583 0.5190 0.069 Uiso 1 1 calc R . . N1 N 0.70267(9) 0.2324(2) 0.15814(15) 0.0280(7) Uani 1 1 d . A . N2 N 0.71413(9) 0.5215(2) 0.18033(15) 0.0271(7) Uani 1 1 d . A . N3 N 0.87680(10) 0.2362(3) 0.49984(18) 0.0456(10) Uani 1 1 d . A . N4 N 0.88378(10) 0.5263(3) 0.48204(18) 0.0495(10) Uani 1 1 d . A . O1 O 0.70033(7) 0.38686(18) 0.07057(12) 0.0292(6) Uani 1 1 d . A . O2 O 0.76263(7) 0.36707(17) 0.19116(11) 0.0250(5) Uani 1 1 d . A . O3 O 0.86792(7) 0.3734(2) 0.38928(13) 0.0425(7) Uani 1 1 d . A . O4 O 0.93180(8) 0.3645(3) 0.50828(15) 0.0534(9) Uani 1 1 d . A . O5 O 0.65226(7) 0.38821(17) 0.14674(12) 0.0283(6) Uani 1 1 d . A . O6 O 0.71626(6) 0.36738(16) 0.26394(12) 0.0244(5) Uani 1 1 d . A . O7 O 0.82221(7) 0.3878(2) 0.46040(12) 0.0364(7) Uani 1 1 d . A . O8 O 0.88512(8) 0.3993(2) 0.58256(14) 0.0466(8) Uani 1 1 d . A . Co1 Co 0.707443(13) 0.37731(3) 0.16707(2) 0.02272(11) Uani 1 1 d . . . Co2 Co 0.877355(15) 0.38134(5) 0.48650(3) 0.04213(16) Uani 1 1 d . . . C57A C 0.96113(19) 0.8097(6) 0.6116(4) 0.064(2) Uani 0.75 1 d PD B 1 H57A H 0.9538 0.7485 0.5927 0.077 Uiso 0.75 1 calc PR B 1 Cl1A Cl 1.00660(6) 0.80529(18) 0.66880(11) 0.0830(7) Uani 0.75 1 d PD B 1 Cl2A Cl 0.93182(6) 0.84143(19) 0.64970(13) 0.0856(7) Uani 0.75 1 d PD B 1 Cl3A Cl 0.95557(6) 0.88299(15) 0.54778(11) 0.0736(6) Uani 0.75 1 d PD B 1 C57B C 0.9490(7) 0.8630(12) 0.6189(14) 0.1188(18) Uiso 0.25 1 d PD C 2 H57B H 0.9297 0.8573 0.5733 0.143 Uiso 0.25 1 calc PR C 2 Cl1B Cl 0.9275(3) 0.8967(7) 0.6681(5) 0.1188(18) Uiso 0.25 1 d PD C 2 Cl2B Cl 0.9690(3) 0.7589(6) 0.6421(5) 0.1188(18) Uiso 0.25 1 d PD C 2 Cl3B Cl 0.9804(3) 0.9410(6) 0.6171(5) 0.1188(18) Uiso 0.25 1 d PD C 2 C58 C 0.96856(15) 0.4886(4) 0.6248(3) 0.0659(16) Uani 1 1 d . . . H58 H 0.9464 0.4703 0.5853 0.079 Uiso 1 1 calc R . . Cl4 Cl 0.98906(5) 0.39237(15) 0.66963(8) 0.0886(6) Uani 1 1 d . . . Cl5 Cl 0.95535(6) 0.56279(19) 0.66984(13) 0.1235(9) Uani 1 1 d . . . Cl6 Cl 1.00010(6) 0.53955(15) 0.59832(10) 0.1023(6) Uani 1 1 d . . . Cl7 Cl 1.00125(17) 1.0416(4) 0.6902(3) 0.0690(7) Uiso 0.25 1 d PD D 3 C59 C 1.0000 1.1149(10) 0.7500 0.0690(7) Uiso 0.50 2 d SPD . 3 Cl8 Cl 0.96386(9) 1.1879(2) 0.74299(16) 0.0690(7) Uiso 0.50 1 d PD E 3 O1W O 0.96829(19) 1.1331(5) 0.7615(3) 0.0520(16) Uiso 0.50 1 d P F 4 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 C1A 0.066(3) 0.069(4) 0.029(2) 0.004(2) 0.013(2) -0.017(3) C3A 0.052(3) 0.142(5) 0.031(2) 0.015(3) 0.020(2) -0.019(3) C1B 0.066(3) 0.069(4) 0.029(2) 0.004(2) 0.013(2) -0.017(3) C3B 0.052(3) 0.142(5) 0.031(2) 0.015(3) 0.020(2) -0.019(3) C4 0.037(2) 0.043(2) 0.0226(18) 0.0006(16) 0.0152(16) -0.0058(18) C5 0.034(2) 0.039(2) 0.0250(18) -0.0034(16) 0.0181(16) -0.0066(17) C6 0.0318(19) 0.0199(17) 0.0254(17) -0.0004(14) 0.0163(15) -0.0035(14) C7 0.0318(19) 0.0230(18) 0.0307(19) 0.0014(14) 0.0194(16) -0.0023(15) C8 0.039(2) 0.043(2) 0.032(2) 0.0010(18) 0.0214(18) 0.0022(19) C9 0.040(2) 0.066(3) 0.043(3) 0.000(2) 0.030(2) 0.007(2) C10 0.030(2) 0.059(3) 0.044(2) 0.005(2) 0.0228(19) 0.008(2) C11 0.030(2) 0.037(2) 0.033(2) 0.0035(17) 0.0184(17) 0.0013(17) C12 0.0301(19) 0.0286(19) 0.0294(18) 0.0029(15) 0.0186(16) 0.0007(15) C13 0.027(2) 0.050(3) 0.035(2) 0.0044(19) 0.0168(17) 0.0000(18) C14 0.030(2) 0.065(3) 0.040(2) 0.007(2) 0.0198(19) 0.004(2) C15 0.025(2) 0.066(3) 0.045(3) 0.007(2) 0.0149(19) 0.000(2) C16 0.029(2) 0.079(4) 0.048(3) 0.009(3) 0.014(2) 0.003(2) C17 0.039(3) 0.087(4) 0.057(3) 0.015(3) 0.013(2) 0.009(3) C18 0.057(4) 0.080(5) 0.094(5) 0.006(4) 0.030(3) 0.004(3) C19 0.053(3) 0.064(4) 0.083(4) -0.006(3) 0.019(3) 0.019(3) C20 0.035(2) 0.067(3) 0.047(3) 0.009(2) 0.016(2) 0.011(2) C21 0.028(2) 0.054(3) 0.037(2) 0.001(2) 0.0150(18) -0.0037(19) C22 0.0291(19) 0.0262(19) 0.036(2) -0.0007(16) 0.0164(16) -0.0027(15) C23 0.0289(19) 0.0300(19) 0.0321(19) -0.0004(16) 0.0190(16) -0.0015(16) C24 0.0291(18) 0.0195(17) 0.0279(18) -0.0012(14) 0.0185(15) -0.0023(14) C25 0.0316(19) 0.0204(17) 0.0263(18) 0.0013(14) 0.0176(15) 0.0024(14) C26 0.030(2) 0.043(2) 0.032(2) 0.0040(17) 0.0190(17) 0.0000(17) C27 0.039(2) 0.071(3) 0.033(2) 0.005(2) 0.026(2) 0.002(2) C28 0.039(2) 0.065(3) 0.026(2) 0.004(2) 0.0198(18) 0.005(2) C29 0.0320(19) 0.0310(19) 0.0269(18) 0.0015(15) 0.0177(16) 0.0035(16) C30 0.0300(18) 0.0210(17) 0.0286(18) 0.0019(14) 0.0193(15) 0.0021(15) C31 0.035(2) 0.037(2) 0.0274(19) 0.0030(16) 0.0177(17) 0.0052(17) C32 0.038(2) 0.053(3) 0.026(2) -0.0018(18) 0.0164(18) 0.002(2) C33 0.041(2) 0.053(3) 0.029(2) 0.0004(19) 0.0151(19) 0.002(2) C34 0.043(3) 0.082(4) 0.028(2) -0.007(2) 0.012(2) 0.006(3) C35 0.072(4) 0.078(4) 0.036(3) 0.008(3) 0.024(3) -0.001(3) C36 0.056(3) 0.091(4) 0.034(2) 0.010(3) 0.018(2) 0.002(3) C37 0.033(2) 0.030(2) 0.034(2) -0.0021(16) 0.0195(17) -0.0016(16) C38 0.041(2) 0.029(2) 0.039(2) -0.0013(17) 0.0237(19) -0.0055(17) C39 0.053(3) 0.023(2) 0.055(3) -0.0069(18) 0.030(2) -0.0034(18) C40 0.060(3) 0.030(2) 0.068(3) -0.011(2) 0.047(3) -0.004(2) C41 0.048(2) 0.031(2) 0.049(3) -0.0070(18) 0.035(2) -0.0059(18) C42 0.039(2) 0.031(2) 0.032(2) -0.0014(16) 0.0209(18) -0.0020(17) C43 0.045(2) 0.028(2) 0.040(2) -0.0017(17) 0.024(2) -0.0075(18) C44 0.047(2) 0.026(2) 0.031(2) -0.0027(16) 0.0145(19) -0.0040(18) C45 0.053(3) 0.029(2) 0.036(2) -0.0021(17) 0.028(2) 0.0009(18) C46 0.044(2) 0.028(2) 0.036(2) 0.0007(16) 0.0263(19) -0.0010(17) C47 0.030(2) 0.088(4) 0.038(3) -0.005(3) 0.013(2) -0.001(2) C48 0.038(3) 0.084(4) 0.062(3) -0.015(3) 0.019(3) -0.007(3) C49 0.051(3) 0.074(4) 0.074(4) 0.002(3) 0.027(3) -0.001(3) C50 0.055(3) 0.081(4) 0.055(3) 0.012(3) 0.022(3) 0.009(3) C51 0.038(3) 0.083(4) 0.038(3) -0.002(3) 0.014(2) 0.005(3) C52 0.037(3) 0.099(5) 0.034(2) 0.012(3) 0.008(2) -0.004(3) C53 0.048(3) 0.083(4) 0.048(3) 0.023(3) 0.006(2) -0.022(3) C54 0.084(4) 0.070(4) 0.040(3) -0.003(3) 0.015(3) -0.016(3) C55 0.090(4) 0.066(4) 0.048(3) -0.010(3) 0.034(3) -0.019(3) C56 0.070(4) 0.069(4) 0.042(3) -0.010(2) 0.032(3) -0.016(3) N1 0.0313(17) 0.0260(16) 0.0305(17) -0.0022(13) 0.0164(14) -0.0036(13) N2 0.0363(18) 0.0221(15) 0.0270(16) 0.0002(12) 0.0171(14) -0.0015(13) N3 0.0254(18) 0.078(3) 0.034(2) -0.0020(19) 0.0132(16) 0.0026(18) N4 0.037(2) 0.079(3) 0.0288(19) 0.0058(19) 0.0091(16) -0.010(2) O1 0.0306(14) 0.0352(15) 0.0247(13) -0.0001(11) 0.0142(11) -0.0027(11) O2 0.0272(13) 0.0284(13) 0.0240(12) 0.0012(10) 0.0152(10) -0.0008(11) O3 0.0246(14) 0.077(2) 0.0284(14) 0.0027(15) 0.0136(12) 0.0053(15) O4 0.0291(16) 0.096(3) 0.0357(16) 0.0029(18) 0.0138(13) 0.0042(17) O5 0.0275(13) 0.0323(14) 0.0279(13) 0.0016(11) 0.0143(11) -0.0010(11) O6 0.0260(13) 0.0271(13) 0.0260(12) 0.0010(10) 0.0168(10) 0.0001(10) O7 0.0283(14) 0.0599(19) 0.0244(13) 0.0033(13) 0.0143(11) 0.0019(13) O8 0.0336(16) 0.077(2) 0.0280(15) 0.0007(15) 0.0116(13) 0.0011(16) Co1 0.0258(2) 0.0237(2) 0.0226(2) -0.00036(19) 0.01393(19) -0.0015(2) Co2 0.0262(3) 0.0747(5) 0.0269(3) 0.0010(3) 0.0123(2) 0.0014(3) C57A 0.054(4) 0.066(5) 0.069(5) 0.012(4) 0.021(4) 0.005(4) Cl1A 0.0549(11) 0.1102(19) 0.0756(14) -0.0100(13) 0.0178(10) 0.0114(12) Cl2A 0.0686(13) 0.1063(19) 0.1020(18) 0.0129(15) 0.0553(13) -0.0021(13) Cl3A 0.0721(13) 0.0764(14) 0.0814(14) 0.0137(11) 0.0406(11) 0.0004(11) C58 0.046(3) 0.095(5) 0.047(3) 0.004(3) 0.009(2) -0.007(3) Cl4 0.0730(10) 0.1322(16) 0.0514(8) 0.0251(9) 0.0157(8) 0.0006(10) Cl5 0.0861(14) 0.158(2) 0.1368(19) -0.0477(17) 0.0555(14) -0.0065(14) Cl6 0.1111(15) 0.1134(16) 0.1020(14) 0.0084(12) 0.0634(12) -0.0282(12) _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 C1A C2A 1.541(10) . ? C1A H1A1 0.9800 . ? C1A H1A2 0.9800 . ? C1A H1A3 0.9800 . ? C2A C3A 1.412(10) . ? C2A H2A1 0.9900 . ? C2A H2A2 0.9900 . ? C3A C4 1.514(6) . ? C3A H3A1 0.9900 . ? C3A H3A2 0.9900 . ? C2B H2B1 0.9900 . ? C2B H2B2 0.9900 . ? C4 O1 1.269(4) . ? C4 C5 1.394(5) . ? C5 C6 1.406(5) . ? C5 H5 0.9500 . ? C6 O2 1.273(4) . ? C6 C7 1.498(5) . ? C7 C8 1.400(5) . ? C7 C12 1.393(5) . ? C8 C9 1.373(6) . ? C8 H8 0.9500 . ? C9 C10 1.378(6) . ? C9 H9 0.9500 . ? C10 C11 1.398(5) . ? C10 H10 0.9500 . ? C11 C12 1.384(5) . ? C11 C13 1.507(5) . ? C12 H12 0.9500 . ? C13 O3 1.270(5) . ? C13 C14 1.396(6) . ? C14 C15 1.409(6) . ? C14 H14 0.9500 . ? C15 O4 1.276(5) . ? C15 C16 1.513(6) . ? C16 C17 1.530(7) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.512(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.515(7) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.526(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.516(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 O5 1.275(4) . ? C22 C23 1.406(5) . ? C23 C24 1.404(5) . ? C23 H23 0.9500 . ? C24 O6 1.265(4) . ? C24 C25 1.510(5) . ? C25 C30 1.394(5) . ? C25 C26 1.392(5) . ? C26 C27 1.384(6) . ? C26 H26 0.9500 . ? C27 C28 1.380(6) . ? C27 H27 0.9500 . ? C28 C29 1.400(5) . ? C28 H28 0.9500 . ? C29 C30 1.392(5) . ? C29 C31 1.497(5) . ? C30 H30 0.9500 . ? C31 O7 1.270(4) . ? C31 C32 1.403(5) . ? C32 C33 1.394(6) . ? C32 H32 0.9500 . ? C33 O8 1.268(5) . ? C33 C34 1.519(6) . ? C34 C35 1.486(7) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.518(6) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 N1 1.343(5) . ? C37 C38 1.377(5) . ? C37 H37 0.9500 . ? C38 C39 1.373(6) . ? C38 H38 0.9500 . ? C39 C40 1.386(6) . ? C39 H39 0.9500 . ? C40 C41 1.376(6) . ? C40 H40 0.9500 . ? C41 N1 1.342(5) . ? C41 H41 0.9500 . ? C42 N2 1.341(5) . ? C42 C43 1.379(5) . ? C42 H42 0.9500 . ? C43 C44 1.373(6) . ? C43 H43 0.9500 . ? C44 C45 1.381(6) . ? C44 H44 0.9500 . ? C45 C46 1.377(5) . ? C45 H45 0.9500 . ? C46 N2 1.340(5) . ? C46 H46 0.9500 . ? C47 N3 1.329(6) . ? C47 C48 1.381(8) . ? C47 H47 0.9500 . ? C48 C49 1.362(8) . ? C48 H48 0.9500 . ? C49 C50 1.382(8) . ? C49 H49 0.9500 . ? C50 C51 1.368(8) . ? C50 H50 0.9500 . ? C51 N3 1.362(6) . ? C51 H51 0.9500 . ? C52 N4 1.363(6) . ? C52 C53 1.390(8) . ? C52 H52 0.9500 . ? C53 C54 1.382(9) . ? C53 H53 0.9500 . ? C54 C55 1.360(8) . ? C54 H54 0.9500 . ? C55 C56 1.386(8) . ? C55 H55 0.9500 . ? C56 N4 1.338(7) . ? C56 H56 0.9500 . ? N1 Co1 2.178(3) . ? N2 Co1 2.178(3) . ? N3 Co2 2.192(5) . ? N4 Co2 2.191(5) . ? O1 Co1 2.060(2) . ? O2 Co1 2.049(2) . ? O3 Co2 2.049(3) . ? O4 Co2 2.039(3) . ? O5 Co1 2.065(3) . ? O6 Co1 2.050(2) . ? O7 Co2 2.036(3) . ? O8 Co2 2.055(3) . ? C57A Cl3A 1.740(8) . ? C57A Cl1A 1.744(7) . ? C57A Cl2A 1.766(8) . ? C57A H57A 1.0000 . ? C57B Cl3B 1.725(18) . ? C57B Cl1B 1.719(18) . ? C57B Cl2B 1.731(18) . ? C57B H57B 1.0000 . ? C58 Cl5 1.718(7) . ? C58 Cl4 1.754(6) . ? C58 Cl6 1.765(6) . ? C58 H58 1.0000 . ? Cl7 C59 1.744(10) . ? C59 Cl7 1.744(10) 2_756 ? C59 Cl8 1.764(9) . ? C59 Cl8 1.764(9) 2_756 ? 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 C2A C1A H1A1 109.5 . . ? C2A C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? C2A C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? C3A C2A C1A 113.6(7) . . ? C3A C2A H2A1 108.8 . . ? C1A C2A H2A1 108.8 . . ? C3A C2A H2A2 108.8 . . ? C1A C2A H2A2 108.8 . . ? H2A1 C2A H2A2 107.7 . . ? C2A C3A C4 120.9(5) . . ? C2A C3A H3A1 107.1 . . ? C4 C3A H3A1 107.1 . . ? C2A C3A H3A2 107.1 . . ? C4 C3A H3A2 107.1 . . ? H3A1 C3A H3A2 106.8 . . ? H2B1 C2B H2B2 107.5 . . ? O1 C4 C5 125.5(3) . . ? O1 C4 C3A 116.3(4) . . ? C5 C4 C3A 118.2(4) . . ? C4 C5 C6 126.2(3) . . ? C4 C5 H5 116.9 . . ? C6 C5 H5 116.9 . . ? O2 C6 C5 123.9(3) . . ? O2 C6 C7 115.5(3) . . ? C5 C6 C7 120.6(3) . . ? C8 C7 C12 117.5(4) . . ? C8 C7 C6 123.3(3) . . ? C12 C7 C6 119.2(3) . . ? C9 C8 C7 120.5(4) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C10 C9 C8 121.0(4) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C9 C10 C11 120.2(4) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C12 C11 C10 118.1(4) . . ? C12 C11 C13 118.9(3) . . ? C10 C11 C13 123.0(4) . . ? C11 C12 C7 122.7(3) . . ? C11 C12 H12 118.7 . . ? C7 C12 H12 118.7 . . ? O3 C13 C14 124.3(4) . . ? O3 C13 C11 115.3(3) . . ? C14 C13 C11 120.5(4) . . ? C13 C14 C15 125.7(4) . . ? C13 C14 H14 117.2 . . ? C15 C14 H14 117.2 . . ? O4 C15 C14 125.2(4) . . ? O4 C15 C16 115.4(4) . . ? C14 C15 C16 119.5(4) . . ? C15 C16 C17 112.4(4) . . ? C15 C16 H16A 109.1 . . ? C17 C16 H16A 109.1 . . ? C15 C16 H16B 109.1 . . ? C17 C16 H16B 109.1 . . ? H16A C16 H16B 107.9 . . ? C18 C17 C16 113.2(5) . . ? C18 C17 H17A 108.9 . . ? C16 C17 H17A 108.9 . . ? C18 C17 H17B 108.9 . . ? C16 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C19 C20 C21 113.6(4) . . ? C19 C20 H20A 108.9 . . ? C21 C20 H20A 108.9 . . ? C19 C20 H20B 108.9 . . ? C21 C20 H20B 108.9 . . ? H20A C20 H20B 107.7 . . ? C22 C21 C20 113.1(4) . . ? C22 C21 H21A 108.9 . . ? C20 C21 H21A 108.9 . . ? C22 C21 H21B 108.9 . . ? C20 C21 H21B 108.9 . . ? H21A C21 H21B 107.8 . . ? O5 C22 C23 125.4(3) . . ? O5 C22 C21 116.0(3) . . ? C23 C22 C21 118.6(3) . . ? C22 C23 C24 125.2(3) . . ? C22 C23 H23 117.4 . . ? C24 C23 H23 117.4 . . ? O6 C24 C23 124.7(3) . . ? O6 C24 C25 115.2(3) . . ? C23 C24 C25 120.1(3) . . ? C30 C25 C26 118.9(3) . . ? C30 C25 C24 118.2(3) . . ? C26 C25 C24 122.9(3) . . ? C27 C26 C25 119.9(4) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C28 120.7(4) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C27 C28 C29 120.7(4) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C30 C29 C28 117.8(4) . . ? C30 C29 C31 119.3(3) . . ? C28 C29 C31 122.9(3) . . ? C29 C30 C25 121.9(3) . . ? C29 C30 H30 119.0 . . ? C25 C30 H30 119.0 . . ? O7 C31 C32 124.4(4) . . ? O7 C31 C29 115.6(3) . . ? C32 C31 C29 120.0(3) . . ? C33 C32 C31 126.4(4) . . ? C33 C32 H32 116.8 . . ? C31 C32 H32 116.8 . . ? O8 C33 C32 125.7(4) . . ? O8 C33 C34 115.8(4) . . ? C32 C33 C34 118.5(4) . . ? C35 C34 C33 114.1(4) . . ? C35 C34 H34A 108.7 . . ? C33 C34 H34A 108.7 . . ? C35 C34 H34B 108.7 . . ? C33 C34 H34B 108.7 . . ? H34A C34 H34B 107.6 . . ? C34 C35 C36 113.0(5) . . ? C34 C35 H35A 109.0 . . ? C36 C35 H35A 109.0 . . ? C34 C35 H35B 109.0 . . ? C36 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N1 C37 C38 123.6(4) . . ? N1 C37 H37 118.2 . . ? C38 C37 H37 118.2 . . ? C39 C38 C37 118.9(4) . . ? C39 C38 H38 120.6 . . ? C37 C38 H38 120.6 . . ? C38 C39 C40 118.6(4) . . ? C38 C39 H39 120.7 . . ? C40 C39 H39 120.7 . . ? C41 C40 C39 119.0(4) . . ? C41 C40 H40 120.5 . . ? C39 C40 H40 120.5 . . ? N1 C41 C40 123.2(4) . . ? N1 C41 H41 118.4 . . ? C40 C41 H41 118.4 . . ? N2 C42 C43 123.2(4) . . ? N2 C42 H42 118.4 . . ? C43 C42 H42 118.4 . . ? C44 C43 C42 119.4(4) . . ? C44 C43 H43 120.3 . . ? C42 C43 H43 120.3 . . ? C43 C44 C45 118.1(4) . . ? C43 C44 H44 121.0 . . ? C45 C44 H44 121.0 . . ? C46 C45 C44 119.2(4) . . ? C46 C45 H45 120.4 . . ? C44 C45 H45 120.4 . . ? N2 C46 C45 123.4(4) . . ? N2 C46 H46 118.3 . . ? C45 C46 H46 118.3 . . ? N3 C47 C48 123.2(5) . . ? N3 C47 H47 118.4 . . ? C48 C47 H47 118.4 . . ? C49 C48 C47 119.2(6) . . ? C49 C48 H48 120.4 . . ? C47 C48 H48 120.4 . . ? C50 C49 C48 119.0(6) . . ? C50 C49 H49 120.5 . . ? C48 C49 H49 120.5 . . ? C51 C50 C49 118.7(6) . . ? C51 C50 H50 120.7 . . ? C49 C50 H50 120.7 . . ? N3 C51 C50 123.1(5) . . ? N3 C51 H51 118.4 . . ? C50 C51 H51 118.4 . . ? N4 C52 C53 121.7(6) . . ? N4 C52 H52 119.1 . . ? C53 C52 H52 119.1 . . ? C54 C53 C52 120.9(5) . . ? C54 C53 H53 119.5 . . ? C52 C53 H53 119.5 . . ? C55 C54 C53 117.1(6) . . ? C55 C54 H54 121.5 . . ? C53 C54 H54 121.5 . . ? C54 C55 C56 119.9(6) . . ? C54 C55 H55 120.0 . . ? C56 C55 H55 120.0 . . ? N4 C56 C55 124.2(5) . . ? N4 C56 H56 117.9 . . ? C55 C56 H56 117.9 . . ? C37 N1 C41 116.8(3) . . ? C37 N1 Co1 121.5(2) . . ? C41 N1 Co1 121.6(3) . . ? C42 N2 C46 116.7(3) . . ? C42 N2 Co1 122.5(3) . . ? C46 N2 Co1 120.8(2) . . ? C47 N3 C51 116.7(5) . . ? C47 N3 Co2 123.1(4) . . ? C51 N3 Co2 120.1(4) . . ? C56 N4 C52 116.0(5) . . ? C56 N4 Co2 121.1(3) . . ? C52 N4 Co2 122.8(4) . . ? C4 O1 Co1 127.6(2) . . ? C6 O2 Co1 129.1(2) . . ? C13 O3 Co2 128.0(3) . . ? C15 O4 Co2 125.9(3) . . ? C22 O5 Co1 128.0(2) . . ? C24 O6 Co1 129.6(2) . . ? C31 O7 Co2 127.4(3) . . ? C33 O8 Co2 126.5(3) . . ? O6 Co1 O2 90.69(9) . . ? O6 Co1 O1 178.20(10) . . ? O2 Co1 O1 87.51(10) . . ? O6 Co1 O5 87.04(10) . . ? O2 Co1 O5 177.70(10) . . ? O1 Co1 O5 94.76(10) . . ? O6 Co1 N2 88.24(11) . . ? O2 Co1 N2 88.80(11) . . ? O1 Co1 N2 91.76(11) . . ? O5 Co1 N2 90.72(11) . . ? O6 Co1 N1 89.74(11) . . ? O2 Co1 N1 89.68(11) . . ? O1 Co1 N1 90.20(11) . . ? O5 Co1 N1 90.72(11) . . ? N2 Co1 N1 177.46(13) . . ? O7 Co2 O4 174.96(14) . . ? O7 Co2 O3 89.28(10) . . ? O4 Co2 O3 88.00(11) . . ? O7 Co2 O8 88.84(11) . . ? O4 Co2 O8 94.17(12) . . ? O3 Co2 O8 175.49(14) . . ? O7 Co2 N3 90.94(13) . . ? O4 Co2 N3 85.06(15) . . ? O3 Co2 N3 94.52(14) . . ? O8 Co2 N3 89.61(14) . . ? O7 Co2 N4 94.18(14) . . ? O4 Co2 N4 90.01(15) . . ? O3 Co2 N4 89.08(14) . . ? O8 Co2 N4 86.97(14) . . ? N3 Co2 N4 173.78(14) . . ? Cl3A C57A Cl1A 111.8(4) . . ? Cl3A C57A Cl2A 109.6(4) . . ? Cl1A C57A Cl2A 110.7(4) . . ? Cl3A C57A H57A 108.2 . . ? Cl1A C57A H57A 108.2 . . ? Cl2A C57A H57A 108.2 . . ? Cl3B C57B Cl1B 111.9(13) . . ? Cl3B C57B Cl2B 111.3(13) . . ? Cl1B C57B Cl2B 111.3(13) . . ? Cl3B C57B H57B 107.4 . . ? Cl1B C57B H57B 107.4 . . ? Cl2B C57B H57B 107.4 . . ? Cl5 C58 Cl4 112.2(3) . . ? Cl5 C58 Cl6 110.3(4) . . ? Cl4 C58 Cl6 108.4(3) . . ? Cl5 C58 H58 108.6 . . ? Cl4 C58 H58 108.6 . . ? Cl6 C58 H58 108.6 . . ? Cl7 C59 Cl7 102.0(9) 2_756 . ? Cl7 C59 Cl8 100.4(2) 2_756 . ? Cl7 C59 Cl8 126.7(2) . . ? Cl7 C59 Cl8 126.7(2) 2_756 2_756 ? Cl7 C59 Cl8 100.4(2) . 2_756 ? Cl8 C59 Cl8 103.5(8) . 2_756 ? 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 C1A C2A C3A C4 -168.5(6) . . . . ? C2A C3A C4 O1 -8.7(10) . . . . ? C2A C3A C4 C5 171.5(7) . . . . ? O1 C4 C5 C6 -0.4(7) . . . . ? C3A C4 C5 C6 179.4(5) . . . . ? C4 C5 C6 O2 -1.4(6) . . . . ? C4 C5 C6 C7 177.3(4) . . . . ? O2 C6 C7 C8 167.9(3) . . . . ? C5 C6 C7 C8 -10.9(6) . . . . ? O2 C6 C7 C12 -9.9(5) . . . . ? C5 C6 C7 C12 171.3(4) . . . . ? C12 C7 C8 C9 0.7(6) . . . . ? C6 C7 C8 C9 -177.1(4) . . . . ? C7 C8 C9 C10 -0.7(7) . . . . ? C8 C9 C10 C11 0.5(8) . . . . ? C9 C10 C11 C12 -0.4(7) . . . . ? C9 C10 C11 C13 -180.0(4) . . . . ? C10 C11 C12 C7 0.5(6) . . . . ? C13 C11 C12 C7 -179.9(4) . . . . ? C8 C7 C12 C11 -0.7(6) . . . . ? C6 C7 C12 C11 177.3(3) . . . . ? C12 C11 C13 O3 -7.8(6) . . . . ? C10 C11 C13 O3 171.7(4) . . . . ? C12 C11 C13 C14 171.7(4) . . . . ? C10 C11 C13 C14 -8.8(7) . . . . ? O3 C13 C14 C15 -7.1(8) . . . . ? C11 C13 C14 C15 173.5(5) . . . . ? C13 C14 C15 O4 -2.3(9) . . . . ? C13 C14 C15 C16 178.6(5) . . . . ? O4 C15 C16 C17 65.3(6) . . . . ? C14 C15 C16 C17 -115.5(5) . . . . ? C15 C16 C17 C18 65.3(6) . . . . ? C19 C20 C21 C22 -64.8(5) . . . . ? C20 C21 C22 O5 -64.7(5) . . . . ? C20 C21 C22 C23 115.2(4) . . . . ? O5 C22 C23 C24 -1.5(6) . . . . ? C21 C22 C23 C24 178.7(4) . . . . ? C22 C23 C24 O6 -0.3(6) . . . . ? C22 C23 C24 C25 177.6(3) . . . . ? O6 C24 C25 C30 13.5(5) . . . . ? C23 C24 C25 C30 -164.6(3) . . . . ? O6 C24 C25 C26 -165.9(3) . . . . ? C23 C24 C25 C26 16.0(5) . . . . ? C30 C25 C26 C27 1.3(6) . . . . ? C24 C25 C26 C27 -179.2(4) . . . . ? C25 C26 C27 C28 0.3(7) . . . . ? C26 C27 C28 C29 -1.4(7) . . . . ? C27 C28 C29 C30 0.8(7) . . . . ? C27 C28 C29 C31 -176.5(4) . . . . ? C28 C29 C30 C25 0.9(6) . . . . ? C31 C29 C30 C25 178.2(3) . . . . ? C26 C25 C30 C29 -1.9(5) . . . . ? C24 C25 C30 C29 178.6(3) . . . . ? C30 C29 C31 O7 -9.7(6) . . . . ? C28 C29 C31 O7 167.5(4) . . . . ? C30 C29 C31 C32 170.2(4) . . . . ? C28 C29 C31 C32 -12.6(6) . . . . ? O7 C31 C32 C33 -7.0(8) . . . . ? C29 C31 C32 C33 173.1(4) . . . . ? C31 C32 C33 O8 1.1(8) . . . . ? C31 C32 C33 C34 -178.3(5) . . . . ? O8 C33 C34 C35 -53.3(6) . . . . ? C32 C33 C34 C35 126.2(5) . . . . ? C33 C34 C35 C36 -178.1(5) . . . . ? N1 C37 C38 C39 -0.3(7) . . . . ? C37 C38 C39 C40 0.2(7) . . . . ? C38 C39 C40 C41 -0.1(7) . . . . ? C39 C40 C41 N1 0.1(8) . . . . ? N2 C42 C43 C44 -0.1(7) . . . . ? C42 C43 C44 C45 -0.2(6) . . . . ? C43 C44 C45 C46 0.6(6) . . . . ? C44 C45 C46 N2 -0.7(7) . . . . ? N3 C47 C48 C49 0.0(8) . . . . ? C47 C48 C49 C50 -0.1(8) . . . . ? C48 C49 C50 C51 -0.1(8) . . . . ? C49 C50 C51 N3 0.4(8) . . . . ? N4 C52 C53 C54 -3.5(8) . . . . ? C52 C53 C54 C55 4.4(8) . . . . ? C53 C54 C55 C56 -2.3(8) . . . . ? C54 C55 C56 N4 -0.9(9) . . . . ? C38 C37 N1 C41 0.2(6) . . . . ? C38 C37 N1 Co1 -175.5(3) . . . . ? C40 C41 N1 C37 -0.2(7) . . . . ? C40 C41 N1 Co1 175.6(4) . . . . ? C43 C42 N2 C46 0.0(6) . . . . ? C43 C42 N2 Co1 -178.4(3) . . . . ? C45 C46 N2 C42 0.4(6) . . . . ? C45 C46 N2 Co1 178.9(3) . . . . ? C48 C47 N3 C51 0.3(7) . . . . ? C48 C47 N3 Co2 177.2(4) . . . . ? C50 C51 N3 C47 -0.5(7) . . . . ? C50 C51 N3 Co2 -177.5(4) . . . . ? C55 C56 N4 C52 1.9(8) . . . . ? C55 C56 N4 Co2 -175.2(4) . . . . ? C53 C52 N4 C56 0.3(7) . . . . ? C53 C52 N4 Co2 177.3(4) . . . . ? C5 C4 O1 Co1 4.5(6) . . . . ? C3A C4 O1 Co1 -175.3(4) . . . . ? C5 C6 O2 Co1 -1.2(5) . . . . ? C7 C6 O2 Co1 -180.0(2) . . . . ? C14 C13 O3 Co2 -1.0(7) . . . . ? C11 C13 O3 Co2 178.5(3) . . . . ? C14 C15 O4 Co2 18.2(7) . . . . ? C16 C15 O4 Co2 -162.6(3) . . . . ? C23 C22 O5 Co1 2.9(6) . . . . ? C21 C22 O5 Co1 -177.2(3) . . . . ? C23 C24 O6 Co1 0.3(5) . . . . ? C25 C24 O6 Co1 -177.7(2) . . . . ? C32 C31 O7 Co2 11.8(6) . . . . ? C29 C31 O7 Co2 -168.4(3) . . . . ? C32 C33 O8 Co2 -0.8(7) . . . . ? C34 C33 O8 Co2 178.7(3) . . . . ? C24 O6 Co1 O2 -179.8(3) . . . . ? C24 O6 Co1 O5 0.6(3) . . . . ? C24 O6 Co1 N2 91.4(3) . . . . ? C24 O6 Co1 N1 -90.1(3) . . . . ? C6 O2 Co1 O6 -176.6(3) . . . . ? C6 O2 Co1 O1 3.4(3) . . . . ? C6 O2 Co1 N2 -88.4(3) . . . . ? C6 O2 Co1 N1 93.6(3) . . . . ? C4 O1 Co1 O2 -5.0(3) . . . . ? C4 O1 Co1 O5 174.6(3) . . . . ? C4 O1 Co1 N2 83.7(3) . . . . ? C4 O1 Co1 N1 -94.7(3) . . . . ? C22 O5 Co1 O6 -2.2(3) . . . . ? C22 O5 Co1 O1 177.8(3) . . . . ? C22 O5 Co1 N2 -90.4(3) . . . . ? C22 O5 Co1 N1 87.5(3) . . . . ? C42 N2 Co1 O6 134.5(3) . . . . ? C46 N2 Co1 O6 -43.8(3) . . . . ? C42 N2 Co1 O2 43.8(3) . . . . ? C46 N2 Co1 O2 -134.5(3) . . . . ? C42 N2 Co1 O1 -43.7(3) . . . . ? C46 N2 Co1 O1 138.0(3) . . . . ? C42 N2 Co1 O5 -138.4(3) . . . . ? C46 N2 Co1 O5 43.2(3) . . . . ? C37 N1 Co1 O6 45.0(3) . . . . ? C41 N1 Co1 O6 -130.6(3) . . . . ? C37 N1 Co1 O2 135.6(3) . . . . ? C41 N1 Co1 O2 -39.9(3) . . . . ? C37 N1 Co1 O1 -136.8(3) . . . . ? C41 N1 Co1 O1 47.6(3) . . . . ? C37 N1 Co1 O5 -42.1(3) . . . . ? C41 N1 Co1 O5 142.3(3) . . . . ? C31 O7 Co2 O3 175.3(4) . . . . ? C31 O7 Co2 O8 -8.8(4) . . . . ? C31 O7 Co2 N3 80.7(4) . . . . ? C31 O7 Co2 N4 -95.7(4) . . . . ? C15 O4 Co2 O3 -18.9(4) . . . . ? C15 O4 Co2 O8 165.0(4) . . . . ? C15 O4 Co2 N3 75.8(4) . . . . ? C15 O4 Co2 N4 -108.0(4) . . . . ? C13 O3 Co2 O7 -165.0(4) . . . . ? C13 O3 Co2 O4 10.8(4) . . . . ? C13 O3 Co2 N3 -74.1(4) . . . . ? C13 O3 Co2 N4 100.8(4) . . . . ? C33 O8 Co2 O7 3.4(4) . . . . ? C33 O8 Co2 O4 -172.5(4) . . . . ? C33 O8 Co2 N3 -87.5(4) . . . . ? C33 O8 Co2 N4 97.7(4) . . . . ? C47 N3 Co2 O7 68.5(3) . . . . ? C51 N3 Co2 O7 -114.8(3) . . . . ? C47 N3 Co2 O4 -108.5(3) . . . . ? C51 N3 Co2 O4 68.3(3) . . . . ? C47 N3 Co2 O3 -20.9(3) . . . . ? C51 N3 Co2 O3 155.9(3) . . . . ? C47 N3 Co2 O8 157.3(3) . . . . ? C51 N3 Co2 O8 -25.9(3) . . . . ? C56 N4 Co2 O7 36.3(4) . . . . ? C52 N4 Co2 O7 -140.6(3) . . . . ? C56 N4 Co2 O4 -146.5(4) . . . . ? C52 N4 Co2 O4 36.6(4) . . . . ? C56 N4 Co2 O3 125.5(4) . . . . ? C52 N4 Co2 O3 -51.4(3) . . . . ? C56 N4 Co2 O8 -52.4(4) . . . . ? C52 N4 Co2 O8 130.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.597 _refine_diff_density_min -0.865 _refine_diff_density_rms 0.094 data_lj75sad _database_code_depnum_ccdc_archive 'CCDC 635436' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H84 N4 O8 Zn2' _chemical_formula_sum 'C68 H84 N4 O8 Zn2' _chemical_formula_weight 1216.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.434(7) _cell_length_b 17.760(10) _cell_length_c 18.194(10) _cell_angle_alpha 111.153(10) _cell_angle_beta 107.481(9) _cell_angle_gamma 102.511(10) _cell_volume 3327(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7077 _cell_measurement_theta_min 2.163 _cell_measurement_theta_max 23.3695 _exptl_crystal_description Prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.416 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 0.775 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.713 _exptl_absorpt_correction_T_max 0.897 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; The crystal was coated in Exxon Paratone N hydrocarbon oil and mounted on a thin mohair fibre attached to a copper pin. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 58 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.24 _diffrn_reflns_number 31706 _diffrn_reflns_av_R_equivalents 0.0589 _diffrn_reflns_av_sigmaI/netI 0.0888 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 28.03 _reflns_number_total 14944 _reflns_number_gt 8056 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT and XPREP (Siemens, 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 (Farrugia, 2005) WINGX-32 (Farrugia, 2005) ; _computing_publication_material 'enCIFer 1.0 (CCDC, 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0927P)^2^+0.7548P] 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 14944 _refine_ls_number_parameters 754 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1247 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.2032 _refine_ls_wR_factor_gt 0.1659 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.2851(8) 0.5020(6) 0.0618(6) 0.0816(12) Uiso 0.60 1 d P A 1 H1A H -0.2033 0.5094 0.0686 0.122 Uiso 0.60 1 calc PR A 1 H1B H -0.2853 0.5512 0.1069 0.122 Uiso 0.60 1 calc PR A 1 H1C H -0.3317 0.4970 0.0064 0.122 Uiso 0.60 1 calc PR A 1 C2 C -0.3411(8) 0.3438(6) -0.0033(6) 0.0816(12) Uiso 0.60 1 d P A 1 H2A H -0.3946 0.3367 -0.0579 0.122 Uiso 0.60 1 calc PR A 1 H2B H -0.3673 0.2915 0.0017 0.122 Uiso 0.60 1 calc PR A 1 H2C H -0.2603 0.3556 0.0000 0.122 Uiso 0.60 1 calc PR A 1 C3 C -0.4765(8) 0.3985(6) 0.0501(6) 0.0816(12) Uiso 0.60 1 d P A 1 H3A H -0.4836 0.4466 0.0920 0.122 Uiso 0.60 1 calc PR A 1 H3B H -0.5093 0.3468 0.0543 0.122 Uiso 0.60 1 calc PR A 1 H3C H -0.5205 0.3907 -0.0071 0.122 Uiso 0.60 1 calc PR A 1 C1A C -0.4578(12) 0.4375(9) 0.0643(9) 0.0816(12) Uiso 0.40 1 d P A 2 H1A1 H -0.4362 0.4925 0.1125 0.122 Uiso 0.40 1 calc PR A 2 H1A2 H -0.5137 0.3932 0.0673 0.122 Uiso 0.40 1 calc PR A 2 H1A3 H -0.4950 0.4400 0.0112 0.122 Uiso 0.40 1 calc PR A 2 C2A C -0.2762(12) 0.4651(9) 0.0399(9) 0.0816(12) Uiso 0.40 1 d P A 2 H2A1 H -0.2161 0.4423 0.0294 0.122 Uiso 0.40 1 calc PR A 2 H2A2 H -0.2372 0.5244 0.0838 0.122 Uiso 0.40 1 calc PR A 2 H2A3 H -0.3294 0.4621 -0.0126 0.122 Uiso 0.40 1 calc PR A 2 C3A C -0.3743(13) 0.3129(8) 0.0026(9) 0.0816(12) Uiso 0.40 1 d P A 2 H3A1 H -0.4320 0.2968 -0.0543 0.122 Uiso 0.40 1 calc PR A 2 H3A2 H -0.4074 0.2769 0.0252 0.122 Uiso 0.40 1 calc PR A 2 H3A3 H -0.3013 0.3053 -0.0003 0.122 Uiso 0.40 1 calc PR A 2 C4 C -0.3431(4) 0.4164(3) 0.0676(3) 0.0697(12) Uani 1 1 d . . . C5 C -0.2624(3) 0.4255(3) 0.1551(2) 0.0576(9) Uani 1 1 d . A . C6 C -0.3079(4) 0.4261(3) 0.2160(2) 0.0653(11) Uani 1 1 d . . . H6 H -0.3864 0.4255 0.2027 0.078 Uiso 1 1 calc R A . C7 C -0.2483(3) 0.4274(2) 0.2953(2) 0.0518(9) Uani 1 1 d . A . C8 C -0.3158(3) 0.4247(2) 0.3502(2) 0.0514(9) Uani 1 1 d . . . C9 C -0.4417(3) 0.4010(3) 0.3196(3) 0.0656(11) Uani 1 1 d . A . H9 H -0.4879 0.3835 0.2615 0.079 Uiso 1 1 calc R . . C10 C -0.4969(4) 0.4032(3) 0.3739(3) 0.0732(12) Uani 1 1 d . . . H10 H -0.5806 0.3876 0.3525 0.088 Uiso 1 1 calc R A . C11 C -0.4317(3) 0.4280(3) 0.4596(2) 0.0627(10) Uani 1 1 d . A . H11 H -0.4714 0.4294 0.4958 0.075 Uiso 1 1 calc R . . C12 C -0.3061(3) 0.4512(2) 0.4932(2) 0.0496(8) Uani 1 1 d . . . C13 C -0.2509(3) 0.4495(2) 0.4375(2) 0.0500(8) Uani 1 1 d . A . H13 H -0.1671 0.4655 0.4591 0.060 Uiso 1 1 calc R . . C14 C -0.2293(3) 0.4806(2) 0.5868(2) 0.0519(9) Uani 1 1 d . A . C15 C -0.2821(4) 0.4605(3) 0.6371(2) 0.0597(10) Uani 1 1 d . . . H15 H -0.3650 0.4288 0.6100 0.072 Uiso 1 1 calc R A . C16 C -0.2243(4) 0.4827(2) 0.7244(2) 0.0571(9) Uani 1 1 d . A . C17 C -0.2967(4) 0.4565(3) 0.7722(3) 0.0751(13) Uani 1 1 d D . . C18 C -0.4427(8) 0.4166(6) 0.7146(6) 0.0839(13) Uiso 0.60 1 d P A 1 H18A H -0.4836 0.4002 0.7466 0.126 Uiso 0.60 1 calc PR A 1 H18B H -0.4629 0.3666 0.6615 0.126 Uiso 0.60 1 calc PR A 1 H18C H -0.4674 0.4596 0.7016 0.126 Uiso 0.60 1 calc PR A 1 C19 C -0.2566(8) 0.3985(6) 0.8007(6) 0.0839(13) Uiso 0.60 1 d P A 1 H19A H -0.3019 0.3827 0.8307 0.126 Uiso 0.60 1 calc PR A 1 H19B H -0.1720 0.4263 0.8390 0.126 Uiso 0.60 1 calc PR A 1 H19C H -0.2688 0.3473 0.7515 0.126 Uiso 0.60 1 calc PR A 1 C20 C -0.2769(8) 0.5428(6) 0.8477(6) 0.0839(13) Uiso 0.60 1 d P A 1 H20A H -0.3018 0.5802 0.8248 0.126 Uiso 0.60 1 calc PR A 1 H20B H -0.1927 0.5707 0.8868 0.126 Uiso 0.60 1 calc PR A 1 H20C H -0.3240 0.5309 0.8781 0.126 Uiso 0.60 1 calc PR A 1 C18A C -0.313(2) 0.3564(12) 0.7402(17) 0.0839(13) Uiso 0.20 1 d PD A 2 H18D H -0.3578 0.3322 0.7663 0.126 Uiso 0.20 1 calc PR A 2 H18E H -0.2349 0.3515 0.7568 0.126 Uiso 0.20 1 calc PR A 2 H18F H -0.3564 0.3253 0.6783 0.126 Uiso 0.20 1 calc PR A 2 C19A C -0.219(2) 0.5055(17) 0.8706(15) 0.0839(13) Uiso 0.20 1 d P A 2 H19D H -0.1381 0.5072 0.8824 0.126 Uiso 0.10 1 calc PR A 2 H19E H -0.2532 0.4763 0.8984 0.126 Uiso 0.10 1 calc PR A 2 H19F H -0.2188 0.5636 0.8925 0.126 Uiso 0.10 1 calc PR A 2 H19G H -0.2686 0.5242 0.8998 0.126 Uiso 0.10 1 calc PR A 2 H19H H -0.1535 0.5552 0.8839 0.126 Uiso 0.10 1 calc PR A 2 H19I H -0.1879 0.4678 0.8897 0.126 Uiso 0.10 1 calc PR A 2 C20A C -0.414(3) 0.4529(18) 0.7501(18) 0.0839(13) Uiso 0.20 1 d P A 2 H20D H -0.4459 0.4359 0.7862 0.126 Uiso 0.10 1 calc PR A 2 H20E H -0.4628 0.4113 0.6905 0.126 Uiso 0.10 1 calc PR A 2 H20F H -0.4165 0.5090 0.7583 0.126 Uiso 0.10 1 calc PR A 2 H20G H -0.4376 0.4682 0.7038 0.126 Uiso 0.10 1 calc PR A 2 H20H H -0.4207 0.4928 0.7995 0.126 Uiso 0.10 1 calc PR A 2 H20I H -0.4670 0.3951 0.7317 0.126 Uiso 0.10 1 calc PR A 2 C18B C -0.2027(19) 0.4414(16) 0.8436(14) 0.0839(13) Uiso 0.20 1 d PD A 3 H18G H -0.2370 0.4335 0.8822 0.126 Uiso 0.20 1 calc PR A 3 H18H H -0.1285 0.4910 0.8759 0.126 Uiso 0.20 1 calc PR A 3 H18I H -0.1866 0.3908 0.8150 0.126 Uiso 0.20 1 calc PR A 3 C19B C -0.404(2) 0.3776(13) 0.7162(13) 0.0839(13) Uiso 0.20 1 d PD A 3 H19J H -0.4480 0.3672 0.7490 0.126 Uiso 0.20 1 calc PR A 3 H19K H -0.3802 0.3294 0.6933 0.126 Uiso 0.20 1 calc PR A 3 H19L H -0.4549 0.3843 0.6693 0.126 Uiso 0.20 1 calc PR A 3 C20B C -0.323(2) 0.5356(12) 0.8214(15) 0.0839(13) Uiso 0.20 1 d PD A 3 H20J H -0.3981 0.5341 0.7850 0.126 Uiso 0.20 1 calc PR A 3 H20K H -0.2587 0.5876 0.8374 0.126 Uiso 0.20 1 calc PR A 3 H20L H -0.3279 0.5346 0.8727 0.126 Uiso 0.20 1 calc PR A 3 C21 C -0.6284(6) 0.1846(4) -0.3305(5) 0.122(2) Uani 1 1 d . . . H21A H -0.6379 0.1264 -0.3664 0.183 Uiso 1 1 calc R . . H21B H -0.5450 0.2167 -0.2902 0.183 Uiso 1 1 calc R . . H21C H -0.6523 0.2120 -0.3661 0.183 Uiso 1 1 calc R . . C22 C -0.6890(8) 0.2740(4) -0.2237(4) 0.139(3) Uani 1 1 d . . . H22A H -0.6091 0.3021 -0.1776 0.208 Uiso 1 1 calc R . . H22B H -0.7480 0.2729 -0.1997 0.208 Uiso 1 1 calc R . . H22C H -0.6990 0.3054 -0.2570 0.208 Uiso 1 1 calc R . . C23 C -0.8375(6) 0.1344(5) -0.3464(5) 0.144(3) Uani 1 1 d . . . H23A H -0.8579 0.1628 -0.3816 0.216 Uiso 1 1 calc R . . H23B H -0.8887 0.1342 -0.3160 0.216 Uiso 1 1 calc R . . H23C H -0.8490 0.0758 -0.3825 0.216 Uiso 1 1 calc R . . C24 C -0.7063(4) 0.1825(3) -0.2815(3) 0.0732(12) Uani 1 1 d . . . C25 C -0.6773(3) 0.1283(3) -0.2329(3) 0.0599(10) Uani 1 1 d . . . C26 C -0.6691(4) 0.1545(3) -0.1499(3) 0.0660(11) Uani 1 1 d . . . H26 H -0.6750 0.2081 -0.1234 0.079 Uiso 1 1 calc R . . C27 C -0.6529(3) 0.1094(3) -0.1009(3) 0.0571(9) Uani 1 1 d . . . C28 C -0.6563(3) 0.1458(2) -0.0142(3) 0.0575(9) Uani 1 1 d . . . C29 C -0.7244(4) 0.1977(3) 0.0042(3) 0.0690(11) Uani 1 1 d . . . H29 H -0.7652 0.2127 -0.0370 0.083 Uiso 1 1 calc R . . C30 C -0.7307(4) 0.2263(3) 0.0830(3) 0.0767(13) Uani 1 1 d . . . H30 H -0.7767 0.2602 0.0947 0.092 Uiso 1 1 calc R . . C31 C -0.6705(4) 0.2057(3) 0.1443(3) 0.0674(11) Uani 1 1 d . . . H31 H -0.6751 0.2266 0.1977 0.081 Uiso 1 1 calc R . . C32 C -0.6018(3) 0.1537(2) 0.1291(2) 0.0558(9) Uani 1 1 d . . . C33 C -0.5965(3) 0.1247(2) 0.0491(2) 0.0559(9) Uani 1 1 d . . . H33 H -0.5515 0.0899 0.0373 0.067 Uiso 1 1 calc R . . C34 C -0.5373(3) 0.1273(2) 0.1937(2) 0.0571(9) Uani 1 1 d . . . C35 C -0.5676(4) 0.1349(3) 0.2624(3) 0.0685(11) Uani 1 1 d . . . H35 H -0.6292 0.1561 0.2649 0.082 Uiso 1 1 calc R . . C36 C -0.5163(4) 0.1141(3) 0.3287(3) 0.0628(10) Uani 1 1 d . B . C37 C -0.5593(5) 0.1308(3) 0.4025(3) 0.0817(13) Uani 1 1 d D . . C38 C -0.7018(11) 0.0956(9) 0.3643(9) 0.0924(16) Uiso 0.45 1 d P B 1 H38A H -0.7273 0.0963 0.4094 0.139 Uiso 0.45 1 calc PR B 1 H38B H -0.7337 0.0373 0.3188 0.139 Uiso 0.45 1 calc PR B 1 H38C H -0.7314 0.1318 0.3416 0.139 Uiso 0.45 1 calc PR B 1 C39 C -0.5158(14) 0.2237(8) 0.4584(9) 0.0924(16) Uiso 0.45 1 d P B 1 H39A H -0.4296 0.2481 0.4777 0.139 Uiso 0.45 1 calc PR B 1 H39B H -0.5348 0.2336 0.5076 0.139 Uiso 0.45 1 calc PR B 1 H39C H -0.5542 0.2506 0.4267 0.139 Uiso 0.45 1 calc PR B 1 C40 C -0.5184(13) 0.0773(9) 0.4516(9) 0.0924(16) Uiso 0.45 1 d P B 1 H40A H -0.4316 0.0980 0.4786 0.139 Uiso 0.45 1 calc PR B 1 H40B H -0.5495 0.0170 0.4109 0.139 Uiso 0.45 1 calc PR B 1 H40C H -0.5494 0.0846 0.4951 0.139 Uiso 0.45 1 calc PR B 1 C38A C -0.4456(15) 0.2091(10) 0.4838(10) 0.0924(16) Uiso 0.35 1 d P B 2 H38D H -0.4205 0.2549 0.4693 0.139 Uiso 0.35 1 calc PR B 2 H38E H -0.3803 0.1894 0.4997 0.139 Uiso 0.35 1 calc PR B 2 H38F H -0.4674 0.2305 0.5317 0.139 Uiso 0.35 1 calc PR B 2 C39A C -0.6597(16) 0.1668(13) 0.3934(11) 0.0924(16) Uiso 0.35 1 d P B 2 H39D H -0.6835 0.1731 0.4401 0.139 Uiso 0.35 1 calc PR B 2 H39E H -0.7280 0.1278 0.3392 0.139 Uiso 0.35 1 calc PR B 2 H39F H -0.6314 0.2224 0.3950 0.139 Uiso 0.35 1 calc PR B 2 C40A C -0.5816(16) 0.0536(11) 0.4170(11) 0.0924(16) Uiso 0.35 1 d P B 2 H40D H -0.5150 0.0340 0.4191 0.139 Uiso 0.35 1 calc PR B 2 H40E H -0.6550 0.0084 0.3705 0.139 Uiso 0.35 1 calc PR B 2 H40F H -0.5893 0.0680 0.4709 0.139 Uiso 0.35 1 calc PR B 2 C38B C -0.6888(19) 0.0557(16) 0.3573(18) 0.0924(16) Uiso 0.20 1 d PD B 3 H38G H -0.7182 0.0553 0.4004 0.139 Uiso 0.20 1 calc PR B 3 H38H H -0.6822 0.0008 0.3289 0.139 Uiso 0.20 1 calc PR B 3 H38I H -0.7442 0.0657 0.3155 0.139 Uiso 0.20 1 calc PR B 3 C39B C -0.592(3) 0.218(2) 0.429(2) 0.0924(16) Uiso 0.20 1 d P B 3 H39G H -0.6403 0.2193 0.3780 0.139 Uiso 0.10 1 calc PR B 3 H39H H -0.5184 0.2682 0.4616 0.139 Uiso 0.10 1 calc PR B 3 H39I H -0.6361 0.2179 0.4645 0.139 Uiso 0.10 1 calc PR B 3 H39J H -0.5562 0.2509 0.4914 0.139 Uiso 0.10 1 calc PR B 3 H39K H -0.6782 0.2021 0.4078 0.139 Uiso 0.10 1 calc PR B 3 H39L H -0.5604 0.2524 0.4050 0.139 Uiso 0.10 1 calc PR B 3 C40B C -0.486(3) 0.123(2) 0.4756(19) 0.0924(16) Uiso 0.20 1 d P B 3 H40G H -0.5194 0.1345 0.5179 0.139 Uiso 0.10 1 calc PR B 3 H40H H -0.4049 0.1639 0.5009 0.139 Uiso 0.10 1 calc PR B 3 H40I H -0.4853 0.0652 0.4567 0.139 Uiso 0.10 1 calc PR B 3 H40J H -0.4203 0.1079 0.4657 0.139 Uiso 0.10 1 calc PR B 3 H40K H -0.5349 0.0786 0.4828 0.139 Uiso 0.10 1 calc PR B 3 H40L H -0.4544 0.1772 0.5270 0.139 Uiso 0.10 1 calc PR B 3 C41 C 0.0785(5) 0.6525(4) 0.4084(3) 0.0914(15) Uani 1 1 d . . . H41 H 0.0904 0.6317 0.4492 0.110 Uiso 1 1 calc R . . C42 C 0.1244(6) 0.7420(4) 0.4379(4) 0.1011(17) Uani 1 1 d . C . H42 H 0.1648 0.7794 0.4970 0.121 Uiso 1 1 calc R . . C43 C 0.1094(5) 0.7740(4) 0.3792(4) 0.0919(15) Uani 1 1 d D . . C44 C 0.0469(5) 0.7153(4) 0.2950(4) 0.1011(17) Uani 1 1 d . C . H44 H 0.0326 0.7340 0.2525 0.121 Uiso 1 1 calc R . . C45 C 0.0051(5) 0.6299(4) 0.2718(3) 0.0904(15) Uani 1 1 d . . . H45 H -0.0372 0.5917 0.2130 0.108 Uiso 1 1 calc R C . C46 C 0.1667(16) 0.8765(8) 0.3973(12) 0.113(3) Uiso 0.60 1 d P C 1 H46A H 0.2408 0.8877 0.3889 0.136 Uiso 0.60 1 calc PR C 1 H46B H 0.1089 0.8905 0.3603 0.136 Uiso 0.60 1 calc PR C 1 C47 C 0.1889(11) 0.9225(8) 0.4847(8) 0.113(3) Uiso 0.60 1 d P C 1 H47A H 0.2277 0.9834 0.5043 0.170 Uiso 0.60 1 calc PR C 1 H47B H 0.2406 0.9035 0.5189 0.170 Uiso 0.60 1 calc PR C 1 H47C H 0.1136 0.9121 0.4905 0.170 Uiso 0.60 1 calc PR C 1 C47A C 0.135(5) 0.929(3) 0.494(3) 0.113(3) Uiso 0.15 1 d PD C 2 H47D H 0.1882 0.9843 0.5068 0.170 Uiso 0.15 1 calc PR C 2 H47E H 0.1607 0.9181 0.5431 0.170 Uiso 0.15 1 calc PR C 2 H47F H 0.0539 0.9275 0.4791 0.170 Uiso 0.15 1 calc PR C 2 C46A C 0.140(5) 0.861(3) 0.420(3) 0.113(3) Uiso 0.15 1 d PD C 2 H46C H 0.0995 0.8719 0.3723 0.136 Uiso 0.15 1 calc PR C 2 H46D H 0.2248 0.8816 0.4314 0.136 Uiso 0.15 1 calc PR C 2 C46B C 0.179(4) 0.8659(12) 0.403(3) 0.113(3) Uiso 0.25 1 d PD C 3 H46E H 0.2632 0.8758 0.4330 0.136 Uiso 0.25 1 calc PR C 3 H46F H 0.1692 0.8678 0.3494 0.136 Uiso 0.25 1 calc PR C 3 C47B C 0.159(3) 0.9428(16) 0.4561(17) 0.113(3) Uiso 0.25 1 d PD C 3 H47G H 0.1898 0.9901 0.4452 0.170 Uiso 0.25 1 calc PR C 3 H47H H 0.1996 0.9588 0.5164 0.170 Uiso 0.25 1 calc PR C 3 H47I H 0.0734 0.9293 0.4407 0.170 Uiso 0.25 1 calc PR C 3 C48 C 0.0542(4) 0.2894(3) 0.2234(3) 0.0800(13) Uani 1 1 d . . . H48 H 0.1304 0.3328 0.2500 0.096 Uiso 1 1 calc R . . C49 C 0.0474(5) 0.2055(3) 0.1926(4) 0.0971(17) Uani 1 1 d D D . H49 H 0.1174 0.1932 0.1974 0.116 Uiso 1 1 calc R . . C50 C -0.0632(5) 0.1389(3) 0.1544(3) 0.0847(14) Uani 1 1 d D . . C51 C -0.1610(4) 0.1627(3) 0.1494(3) 0.0775(13) Uani 1 1 d D D . H51 H -0.2376 0.1205 0.1250 0.093 Uiso 1 1 calc R . . C52 C -0.1476(4) 0.2484(3) 0.1801(3) 0.0686(11) Uani 1 1 d . . . H52 H -0.2168 0.2621 0.1744 0.082 Uiso 1 1 calc R D . C53 C -0.0801(18) 0.0448(6) 0.1095(12) 0.137(3) Uiso 0.60 1 d PD D 1 H53A H -0.1211 0.0150 0.1344 0.165 Uiso 0.60 1 calc PR D 1 H53B H -0.1350 0.0219 0.0493 0.165 Uiso 0.60 1 calc PR D 1 C54 C 0.0220(11) 0.0206(8) 0.1105(9) 0.137(3) Uiso 0.60 1 d P D 1 H54A H -0.0018 -0.0317 0.0586 0.206 Uiso 0.60 1 calc PR D 1 H54B H 0.0529 0.0109 0.1600 0.206 Uiso 0.60 1 calc PR D 1 H54C H 0.0839 0.0661 0.1136 0.206 Uiso 0.60 1 calc PR D 1 C53B C -0.070(3) 0.0464(9) 0.1302(18) 0.137(3) Uiso 0.40 1 d PD D 3 H53E H -0.1412 0.0181 0.1360 0.165 Uiso 0.40 1 calc PR D 3 H53F H -0.0889 0.0196 0.0688 0.165 Uiso 0.40 1 calc PR D 3 C54B C 0.0137(18) 0.0242(13) 0.1660(13) 0.137(3) Uiso 0.40 1 d P D 3 H54G H 0.0091 -0.0299 0.1246 0.206 Uiso 0.40 1 calc PR D 3 H54H H 0.0043 0.0178 0.2142 0.206 Uiso 0.40 1 calc PR D 3 H54I H 0.0910 0.0680 0.1861 0.206 Uiso 0.40 1 calc PR D 3 C55 C -0.8873(4) -0.1008(3) -0.3312(3) 0.0780(13) Uani 1 1 d . . . H55 H -0.8758 -0.0426 -0.3143 0.094 Uiso 1 1 calc R . . C56 C -1.0031(5) -0.1608(3) -0.3791(4) 0.0960(17) Uani 1 1 d . E . H56 H -1.0677 -0.1428 -0.3945 0.115 Uiso 1 1 calc R . . C57 C -1.0241(4) -0.2479(3) -0.4046(3) 0.0841(14) Uani 1 1 d . . . C58 C -0.9245(5) -0.2694(3) -0.3806(3) 0.0756(13) Uani 1 1 d . E . H58 H -0.9337 -0.3272 -0.3966 0.091 Uiso 1 1 calc R . . C59 C -0.8113(4) -0.2061(3) -0.3330(3) 0.0686(11) Uani 1 1 d . . . H59 H -0.7451 -0.2224 -0.3174 0.082 Uiso 1 1 calc R E . C60 C -1.1579(15) -0.3094(11) -0.4406(9) 0.0859(18) Uiso 0.45 1 d P E 1 H60A H -1.1609 -0.3646 -0.4411 0.103 Uiso 0.45 1 calc PR E 1 H60B H -1.1972 -0.2836 -0.4051 0.103 Uiso 0.45 1 calc PR E 1 C61 C -1.2208(12) -0.3220(9) -0.5335(9) 0.0859(18) Uiso 0.45 1 d P E 1 H61A H -1.3047 -0.3579 -0.5580 0.129 Uiso 0.45 1 calc PR E 1 H61B H -1.1825 -0.3492 -0.5683 0.129 Uiso 0.45 1 calc PR E 1 H61C H -1.2143 -0.2665 -0.5321 0.129 Uiso 0.45 1 calc PR E 1 C61A C -1.1950(14) -0.3382(10) -0.5553(9) 0.0859(18) Uiso 0.40 1 d P E 2 H61D H -1.2745 -0.3823 -0.5851 0.129 Uiso 0.40 1 calc PR E 2 H61E H -1.1424 -0.3591 -0.5797 0.129 Uiso 0.40 1 calc PR E 2 H61F H -1.1992 -0.2873 -0.5616 0.129 Uiso 0.40 1 calc PR E 2 C60A C -1.1483(19) -0.3169(13) -0.4651(12) 0.0859(18) Uiso 0.40 1 d P E 2 H60C H -1.1477 -0.3698 -0.4610 0.103 Uiso 0.40 1 calc PR E 2 H60D H -1.2055 -0.2992 -0.4432 0.103 Uiso 0.40 1 calc PR E 2 C60B C -1.127(4) -0.338(3) -0.481(3) 0.0859(18) Uiso 0.15 1 d P E 3 H60E H -1.1196 -0.3536 -0.5355 0.103 Uiso 0.15 1 calc PR E 3 H60F H -1.1308 -0.3855 -0.4659 0.103 Uiso 0.15 1 calc PR E 3 C61B C -1.232(3) -0.309(2) -0.481(3) 0.0859(18) Uiso 0.15 1 d P E 3 H61G H -1.3061 -0.3583 -0.5189 0.129 Uiso 0.15 1 calc PR E 3 H61H H -1.2284 -0.2664 -0.5015 0.129 Uiso 0.15 1 calc PR E 3 H61I H -1.2273 -0.2852 -0.4235 0.129 Uiso 0.15 1 calc PR E 3 C62 C -0.3831(4) 0.1162(3) -0.2122(3) 0.0803(13) Uani 1 1 d . . . H62 H -0.4386 0.1034 -0.2665 0.096 Uiso 1 1 calc R . . C63 C -0.2696(5) 0.1736(4) -0.1811(4) 0.0993(17) Uani 1 1 d . F . H63 H -0.2496 0.1999 -0.2136 0.119 Uiso 1 1 calc R . . C64 C -0.1843(5) 0.1933(5) -0.1023(4) 0.125(2) Uani 1 1 d D . . C65 C -0.2205(5) 0.1532(5) -0.0584(4) 0.118(2) Uani 1 1 d . F . H65 H -0.1657 0.1642 -0.0045 0.142 Uiso 1 1 calc R . . C66 C -0.3379(5) 0.0961(4) -0.0928(3) 0.0885(15) Uani 1 1 d . . . H66 H -0.3605 0.0699 -0.0610 0.106 Uiso 1 1 calc R F . C67 C -0.0461(17) 0.2434(15) -0.066(3) 0.162(5) Uiso 0.40 1 d PD F 1 H67A H -0.0022 0.2367 -0.0161 0.194 Uiso 0.40 1 calc PR F 1 H67B H -0.0159 0.2225 -0.1096 0.194 Uiso 0.40 1 calc PR F 1 C68 C -0.033(2) 0.3379(14) -0.0398(16) 0.162(5) Uiso 0.40 1 d PD F 1 H68A H 0.0506 0.3723 -0.0210 0.243 Uiso 0.40 1 calc PR F 1 H68B H -0.0572 0.3585 0.0066 0.243 Uiso 0.40 1 calc PR F 1 H68C H -0.0824 0.3423 -0.0886 0.243 Uiso 0.40 1 calc PR F 1 C67A C -0.062(3) 0.286(2) -0.059(2) 0.162(5) Uiso 0.40 1 d P F 2 H67C H -0.0715 0.3213 -0.0888 0.194 Uiso 0.40 1 calc PR F 2 H67D H -0.0322 0.3204 0.0032 0.194 Uiso 0.40 1 calc PR F 2 C68A C -0.005(3) 0.2374(19) -0.0810(19) 0.162(5) Uiso 0.40 1 d P F 2 H68D H 0.0784 0.2722 -0.0607 0.243 Uiso 0.40 1 calc PR F 2 H68E H -0.0400 0.2050 -0.1431 0.243 Uiso 0.40 1 calc PR F 2 H68F H -0.0104 0.1981 -0.0562 0.243 Uiso 0.40 1 calc PR F 2 C67B C -0.063(4) 0.269(4) -0.040(3) 0.162(5) Uiso 0.20 1 d PD F 3 H67E H -0.0795 0.3198 -0.0116 0.194 Uiso 0.20 1 calc PR F 3 H67F H -0.0200 0.2545 0.0036 0.194 Uiso 0.20 1 calc PR F 3 C68B C 0.009(5) 0.288(4) -0.080(3) 0.162(5) Uiso 0.20 1 d P F 3 H68G H 0.0913 0.3205 -0.0375 0.243 Uiso 0.20 1 calc PR F 3 H68H H -0.0184 0.3207 -0.1079 0.243 Uiso 0.20 1 calc PR F 3 H68I H 0.0059 0.2346 -0.1226 0.243 Uiso 0.20 1 calc PR F 3 N1 N 0.0197(3) 0.5964(2) 0.3264(2) 0.0692(9) Uani 1 1 d . A . N2 N -0.0409(3) 0.3133(2) 0.2178(2) 0.0621(8) Uani 1 1 d . A . N3 N -0.7915(3) -0.1215(2) -0.3078(2) 0.0644(9) Uani 1 1 d . E . N4 N -0.4195(3) 0.0772(2) -0.1693(2) 0.0721(9) Uani 1 1 d . E . O1 O -0.1556(2) 0.43005(19) 0.16522(16) 0.0651(7) Uani 1 1 d . . . O2 O -0.1410(2) 0.43134(18) 0.32554(15) 0.0598(7) Uani 1 1 d . . . O3 O -0.1179(2) 0.52301(17) 0.61275(15) 0.0576(6) Uani 1 1 d . . . O4 O -0.1118(2) 0.52507(19) 0.77085(16) 0.0639(7) Uani 1 1 d . . . O5 O -0.6679(2) 0.05826(19) -0.27746(18) 0.0663(7) Uani 1 1 d . E . O6 O -0.6353(2) 0.03825(18) -0.12354(17) 0.0626(7) Uani 1 1 d . E . O7 O -0.4565(3) 0.09795(18) 0.18011(17) 0.0640(7) Uani 1 1 d . . . O8 O -0.4339(3) 0.0828(2) 0.33466(18) 0.0696(7) Uani 1 1 d . . . Zn1 Zn -0.01850(4) 0.45089(3) 0.27437(3) 0.05825(16) Uani 1 1 d . . . Zn2 Zn -0.60918(4) -0.02384(3) -0.23264(3) 0.06166(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C4 0.062(2) 0.103(3) 0.050(2) 0.039(2) 0.0244(19) 0.033(2) C5 0.053(2) 0.070(3) 0.048(2) 0.0279(19) 0.0175(17) 0.0212(19) C6 0.053(2) 0.095(3) 0.050(2) 0.035(2) 0.0217(17) 0.026(2) C7 0.051(2) 0.061(2) 0.0436(19) 0.0245(17) 0.0199(16) 0.0182(17) C8 0.0486(19) 0.059(2) 0.0440(19) 0.0194(17) 0.0199(16) 0.0204(17) C9 0.050(2) 0.087(3) 0.049(2) 0.029(2) 0.0167(17) 0.016(2) C10 0.045(2) 0.107(4) 0.060(2) 0.035(2) 0.0202(19) 0.021(2) C11 0.051(2) 0.085(3) 0.058(2) 0.033(2) 0.0314(18) 0.024(2) C12 0.0478(19) 0.055(2) 0.0499(19) 0.0243(17) 0.0239(16) 0.0205(16) C13 0.0427(18) 0.056(2) 0.053(2) 0.0248(17) 0.0237(16) 0.0167(16) C14 0.049(2) 0.058(2) 0.051(2) 0.0253(17) 0.0248(16) 0.0185(17) C15 0.055(2) 0.069(3) 0.053(2) 0.0242(19) 0.0303(18) 0.0142(19) C16 0.067(2) 0.056(2) 0.057(2) 0.0263(19) 0.038(2) 0.019(2) C17 0.081(3) 0.082(3) 0.061(3) 0.034(2) 0.039(2) 0.011(2) C21 0.144(6) 0.138(5) 0.149(6) 0.112(5) 0.075(5) 0.067(5) C22 0.242(9) 0.086(4) 0.105(4) 0.061(4) 0.058(5) 0.079(5) C23 0.103(4) 0.153(6) 0.158(6) 0.114(5) -0.005(4) 0.022(4) C24 0.079(3) 0.075(3) 0.071(3) 0.047(2) 0.021(2) 0.028(2) C25 0.052(2) 0.060(3) 0.061(2) 0.029(2) 0.0156(18) 0.0154(19) C26 0.072(3) 0.064(3) 0.068(3) 0.035(2) 0.025(2) 0.032(2) C27 0.051(2) 0.058(2) 0.063(2) 0.0286(19) 0.0208(18) 0.0228(18) C28 0.059(2) 0.053(2) 0.064(2) 0.0280(19) 0.0253(19) 0.0242(18) C29 0.069(3) 0.075(3) 0.075(3) 0.038(2) 0.030(2) 0.040(2) C30 0.083(3) 0.080(3) 0.079(3) 0.034(2) 0.036(2) 0.053(3) C31 0.071(3) 0.073(3) 0.060(2) 0.026(2) 0.028(2) 0.036(2) C32 0.052(2) 0.055(2) 0.057(2) 0.0222(18) 0.0219(17) 0.0198(18) C33 0.057(2) 0.054(2) 0.063(2) 0.0269(19) 0.0273(18) 0.0261(18) C34 0.057(2) 0.057(2) 0.054(2) 0.0224(18) 0.0236(18) 0.0205(19) C35 0.070(3) 0.082(3) 0.070(3) 0.035(2) 0.039(2) 0.041(2) C36 0.061(2) 0.071(3) 0.058(2) 0.028(2) 0.0279(19) 0.026(2) C37 0.089(3) 0.098(4) 0.077(3) 0.043(3) 0.047(3) 0.043(3) C41 0.122(4) 0.095(4) 0.071(3) 0.039(3) 0.049(3) 0.049(3) C42 0.129(5) 0.087(4) 0.075(3) 0.023(3) 0.042(3) 0.041(4) C43 0.085(3) 0.077(4) 0.110(4) 0.043(3) 0.036(3) 0.031(3) C44 0.109(4) 0.091(4) 0.093(4) 0.055(3) 0.024(3) 0.022(3) C45 0.096(4) 0.095(4) 0.073(3) 0.049(3) 0.020(3) 0.028(3) C48 0.064(3) 0.078(3) 0.101(4) 0.042(3) 0.042(3) 0.018(2) C49 0.078(3) 0.077(4) 0.148(5) 0.045(3) 0.067(3) 0.030(3) C50 0.092(4) 0.064(3) 0.100(4) 0.030(3) 0.057(3) 0.021(3) C51 0.070(3) 0.075(3) 0.067(3) 0.021(2) 0.032(2) 0.005(2) C52 0.058(2) 0.082(3) 0.055(2) 0.028(2) 0.0231(19) 0.015(2) C55 0.070(3) 0.065(3) 0.110(4) 0.047(3) 0.041(3) 0.028(2) C56 0.068(3) 0.086(4) 0.140(5) 0.067(3) 0.033(3) 0.027(3) C57 0.073(3) 0.074(3) 0.091(3) 0.043(3) 0.019(3) 0.012(2) C58 0.097(4) 0.062(3) 0.060(3) 0.028(2) 0.026(2) 0.027(3) C59 0.082(3) 0.067(3) 0.057(2) 0.027(2) 0.027(2) 0.032(2) C62 0.075(3) 0.098(4) 0.076(3) 0.051(3) 0.032(2) 0.028(3) C63 0.082(4) 0.115(4) 0.098(4) 0.059(3) 0.037(3) 0.015(3) C64 0.075(4) 0.155(6) 0.101(4) 0.053(4) 0.024(3) -0.009(4) C65 0.084(4) 0.156(6) 0.080(4) 0.057(4) 0.013(3) 0.006(4) C66 0.094(4) 0.104(4) 0.066(3) 0.042(3) 0.035(3) 0.028(3) N1 0.071(2) 0.080(2) 0.063(2) 0.034(2) 0.0330(18) 0.0298(19) N2 0.0546(19) 0.071(2) 0.0591(19) 0.0297(17) 0.0275(16) 0.0155(17) N3 0.070(2) 0.063(2) 0.063(2) 0.0273(17) 0.0311(17) 0.0279(18) N4 0.070(2) 0.077(2) 0.068(2) 0.034(2) 0.0284(19) 0.0259(19) O1 0.0568(16) 0.095(2) 0.0505(15) 0.0415(15) 0.0229(12) 0.0239(14) O2 0.0491(14) 0.093(2) 0.0489(14) 0.0406(14) 0.0238(11) 0.0288(13) O3 0.0474(14) 0.0795(18) 0.0515(14) 0.0369(13) 0.0231(11) 0.0176(13) O4 0.0629(17) 0.0822(19) 0.0516(15) 0.0344(14) 0.0307(13) 0.0190(15) O5 0.0692(18) 0.0735(19) 0.0642(17) 0.0382(15) 0.0278(14) 0.0285(15) O6 0.0751(18) 0.0673(18) 0.0637(16) 0.0363(14) 0.0354(14) 0.0381(15) O7 0.0706(17) 0.0766(19) 0.0650(17) 0.0380(14) 0.0372(14) 0.0405(15) O8 0.0750(18) 0.084(2) 0.0656(18) 0.0386(15) 0.0371(15) 0.0393(16) Zn1 0.0516(3) 0.0802(3) 0.0478(3) 0.0333(2) 0.0232(2) 0.0221(2) Zn2 0.0658(3) 0.0700(3) 0.0614(3) 0.0346(2) 0.0311(2) 0.0321(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 C1 C4 1.589(10) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C4 1.470(10) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.529(10) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C1A C4 1.542(14) . ? C1A H1A1 0.9600 . ? C1A H1A2 0.9600 . ? C1A H1A3 0.9600 . ? C2A C4 1.396(13) . ? C2A H2A1 0.9600 . ? C2A H2A2 0.9600 . ? C2A H2A3 0.9600 . ? C3A C4 1.666(14) . ? C3A H3A1 0.9600 . ? C3A H3A2 0.9600 . ? C3A H3A3 0.9600 . ? C4 C5 1.533(5) . ? C5 O1 1.265(4) . ? C5 C6 1.385(5) . ? C6 C7 1.400(5) . ? C6 H6 0.9300 . ? C7 O2 1.257(4) . ? C7 C8 1.491(5) . ? C8 C13 1.392(5) . ? C8 C9 1.400(5) . ? C9 C10 1.356(6) . ? C9 H9 0.9300 . ? C10 C11 1.369(5) . ? C10 H10 0.9300 . ? C11 C12 1.397(5) . ? C11 H11 0.9300 . ? C12 C13 1.379(5) . ? C12 C14 1.501(5) . ? C13 H13 0.9300 . ? C14 O3 1.267(4) . ? C14 C15 1.376(5) . ? C15 C16 1.390(5) . ? C15 H15 0.9300 . ? C16 O4 1.269(5) . ? C16 C17 1.538(5) . ? C17 C20A 1.38(3) . ? C17 C19 1.425(10) . ? C17 C19B 1.459(19) . ? C17 C20B 1.531(15) . ? C17 C19A 1.54(2) . ? C17 C20 1.552(10) . ? C17 C18A 1.602(16) . ? C17 C18B 1.611(14) . ? C17 C18 1.631(10) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C18A H18D 0.9600 . ? C18A H18E 0.9600 . ? C18A H18F 0.9600 . ? C19A H19D 0.9600 . ? C19A H19E 0.9600 . ? C19A H19F 0.9600 . ? C19A H19G 0.9600 . ? C19A H19H 0.9600 . ? C19A H19I 0.9600 . ? C20A H20D 0.9600 . ? C20A H20E 0.9600 . ? C20A H20F 0.9600 . ? C20A H20G 0.9600 . ? C20A H20H 0.9600 . ? C20A H20I 0.9600 . ? C18B H18G 0.9600 . ? C18B H18H 0.9600 . ? C18B H18I 0.9600 . ? C19B H19J 0.9600 . ? C19B H19K 0.9600 . ? C19B H19L 0.9600 . ? C20B H20J 0.9600 . ? C20B H20K 0.9600 . ? C20B H20L 0.9600 . ? C21 C24 1.503(7) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C24 1.509(8) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.515(7) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.553(6) . ? C25 O5 1.269(5) . ? C25 C26 1.373(6) . ? C26 C27 1.398(5) . ? C26 H26 0.9300 . ? C27 O6 1.270(5) . ? C27 C28 1.492(6) . ? C28 C33 1.392(5) . ? C28 C29 1.400(5) . ? C29 C30 1.370(6) . ? C29 H29 0.9300 . ? C30 C31 1.362(6) . ? C30 H30 0.9300 . ? C31 C32 1.398(5) . ? C31 H31 0.9300 . ? C32 C33 1.387(5) . ? C32 C34 1.496(5) . ? C33 H33 0.9300 . ? C34 O7 1.275(4) . ? C34 C35 1.382(5) . ? C35 C36 1.399(6) . ? C35 H35 0.9300 . ? C36 O8 1.263(5) . ? C36 C37 1.546(6) . ? C37 C40B 1.44(3) . ? C37 C39 1.455(13) . ? C37 C40A 1.473(17) . ? C37 C39A 1.515(16) . ? C37 C38 1.576(13) . ? C37 C40 1.584(15) . ? C37 C38A 1.590(16) . ? C37 C38B 1.591(17) . ? C37 C39B 1.63(3) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C38A H38D 0.9600 . ? C38A H38E 0.9600 . ? C38A H38F 0.9600 . ? C39A H39D 0.9600 . ? C39A H39E 0.9600 . ? C39A H39F 0.9600 . ? C40A H40D 0.9600 . ? C40A H40E 0.9600 . ? C40A H40F 0.9600 . ? C38B H38G 0.9600 . ? C38B H38H 0.9600 . ? C38B H38I 0.9600 . ? C39B H39G 0.9600 . ? C39B H39H 0.9600 . ? C39B H39I 0.9600 . ? C39B H39J 0.9600 . ? C39B H39K 0.9600 . ? C39B H39L 0.9600 . ? C40B H40G 0.9600 . ? C40B H40H 0.9600 . ? C40B H40I 0.9600 . ? C40B H40J 0.9600 . ? C40B H40K 0.9600 . ? C40B H40L 0.9600 . ? C41 N1 1.308(6) . ? C41 C42 1.394(8) . ? C41 H41 0.9300 . ? C42 C43 1.366(8) . ? C42 H42 0.9300 . ? C43 C46A 1.35(4) . ? C43 C44 1.349(7) . ? C43 C46B 1.496(19) . ? C43 C46 1.670(14) . ? C44 C45 1.348(7) . ? C44 H44 0.9300 . ? C45 N1 1.318(6) . ? C45 H45 0.9300 . ? C46 C47 1.404(19) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C47A C46A 1.47(2) . ? C47A H47D 0.9600 . ? C47A H47E 0.9600 . ? C47A H47F 0.9600 . ? C46A H46C 0.9700 . ? C46A H46D 0.9700 . ? C46B C47B 1.480(19) . ? C46B H46E 0.9700 . ? C46B H46F 0.9700 . ? C47B H47G 0.9600 . ? C47B H47H 0.9600 . ? C47B H47I 0.9600 . ? C48 N2 1.329(5) . ? C48 C49 1.362(7) . ? C48 H48 0.9300 . ? C49 C50 1.379(7) . ? C49 H49 0.9300 . ? C50 C51 1.360(7) . ? C50 C53 1.506(8) . ? C50 C53B 1.514(9) . ? C51 C52 1.369(6) . ? C51 H51 0.9300 . ? C52 N2 1.334(5) . ? C52 H52 0.9300 . ? C53 C54 1.42(2) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C53B C54B 1.28(3) . ? C53B H53E 0.9700 . ? C53B H53F 0.9700 . ? C54B H54G 0.9600 . ? C54B H54H 0.9600 . ? C54B H54I 0.9600 . ? C55 N3 1.317(5) . ? C55 C56 1.371(7) . ? C55 H55 0.9300 . ? C56 C57 1.383(7) . ? C56 H56 0.9300 . ? C57 C58 1.368(7) . ? C57 C60A 1.51(2) . ? C57 C60 1.559(17) . ? C57 C60B 1.61(4) . ? C58 C59 1.369(6) . ? C58 H58 0.9300 . ? C59 N3 1.342(5) . ? C59 H59 0.9300 . ? C60 C61 1.54(2) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C61A C60A 1.43(2) . ? C61A H61D 0.9600 . ? C61A H61E 0.9600 . ? C61A H61F 0.9600 . ? C60A H60C 0.9700 . ? C60A H60D 0.9700 . ? C60B C61B 1.49(5) . ? C60B H60E 0.9700 . ? C60B H60F 0.9700 . ? C61B H61G 0.9600 . ? C61B H61H 0.9600 . ? C61B H61I 0.9600 . ? C62 N4 1.326(6) . ? C62 C63 1.354(7) . ? C62 H62 0.9300 . ? C63 C64 1.366(8) . ? C63 H63 0.9300 . ? C64 C65 1.356(8) . ? C64 C67B 1.53(2) . ? C64 C67 1.553(17) . ? C64 C67A 1.70(3) . ? C65 C66 1.379(7) . ? C65 H65 0.9300 . ? C66 N4 1.321(6) . ? C66 H66 0.9300 . ? C67 C68 1.525(19) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C67A C68A 1.26(5) . ? C67A H67C 0.9700 . ? C67A H67D 0.9700 . ? C68A H68D 0.9600 . ? C68A H68E 0.9600 . ? C68A H68F 0.9600 . ? C67B C68B 1.37(8) . ? C67B H67E 0.9700 . ? C67B H67F 0.9700 . ? C68B H68G 0.9600 . ? C68B H68H 0.9600 . ? C68B H68I 0.9600 . ? N1 Zn1 2.288(4) . ? N2 Zn1 2.197(4) . ? N3 Zn2 2.177(4) . ? N4 Zn2 2.270(4) . ? O1 Zn1 2.037(3) . ? O2 Zn1 2.040(3) . ? O3 Zn1 2.047(3) 2_566 ? O4 Zn1 2.059(3) 2_566 ? O5 Zn2 2.070(3) . ? O6 Zn2 2.055(3) . ? O7 Zn2 2.053(3) 2_455 ? O8 Zn2 2.065(3) 2_455 ? Zn1 O3 2.047(3) 2_566 ? Zn1 O4 2.059(3) 2_566 ? Zn2 O7 2.053(3) 2_455 ? Zn2 O8 2.065(3) 2_455 ? 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 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? C4 C1A H1A1 109.5 . . ? C4 C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? C4 C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? C4 C2A H2A1 109.5 . . ? C4 C2A H2A2 109.5 . . ? H2A1 C2A H2A2 109.5 . . ? C4 C2A H2A3 109.5 . . ? H2A1 C2A H2A3 109.5 . . ? H2A2 C2A H2A3 109.5 . . ? C4 C3A H3A1 109.5 . . ? C4 C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? C4 C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? C2A C4 C2 82.3(7) . . ? C2A C4 C3 126.1(7) . . ? C2 C4 C3 105.9(6) . . ? C2A C4 C5 110.8(6) . . ? C2 C4 C5 109.8(5) . . ? C3 C4 C5 115.4(5) . . ? C2A C4 C1A 110.3(8) . . ? C2 C4 C1A 123.4(7) . . ? C5 C4 C1A 115.3(6) . . ? C2 C4 C1 106.8(5) . . ? C3 C4 C1 111.0(5) . . ? C5 C4 C1 107.6(4) . . ? C1A C4 C1 90.7(7) . . ? C2A C4 C3A 106.0(8) . . ? C3 C4 C3A 91.2(6) . . ? C5 C4 C3A 101.0(6) . . ? C1A C4 C3A 112.8(7) . . ? C1 C4 C3A 130.3(6) . . ? O1 C5 C6 124.1(3) . . ? O1 C5 C4 115.3(3) . . ? C6 C5 C4 120.6(4) . . ? C5 C6 C7 127.0(4) . . ? C5 C6 H6 116.5 . . ? C7 C6 H6 116.5 . . ? O2 C7 C6 125.6(3) . . ? O2 C7 C8 116.1(3) . . ? C6 C7 C8 118.3(3) . . ? C13 C8 C9 117.4(3) . . ? C13 C8 C7 118.9(3) . . ? C9 C8 C7 123.7(3) . . ? C10 C9 C8 120.7(4) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 121.2(4) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C10 C11 C12 120.4(3) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C13 C12 C11 117.8(3) . . ? C13 C12 C14 119.2(3) . . ? C11 C12 C14 123.0(3) . . ? C12 C13 C8 122.5(3) . . ? C12 C13 H13 118.7 . . ? C8 C13 H13 118.7 . . ? O3 C14 C15 125.3(3) . . ? O3 C14 C12 115.3(3) . . ? C15 C14 C12 119.4(3) . . ? C14 C15 C16 126.6(4) . . ? C14 C15 H15 116.7 . . ? C16 C15 H15 116.7 . . ? O4 C16 C15 124.8(3) . . ? O4 C16 C17 114.7(3) . . ? C15 C16 C17 120.5(4) . . ? C20A C17 C19 122.1(13) . . ? C20A C17 C19B 54.9(14) . . ? C19 C17 C19B 80.4(10) . . ? C20A C17 C20B 60.3(14) . . ? C19 C17 C20B 129.3(11) . . ? C19B C17 C20B 114.0(12) . . ? C20A C17 C19A 112.8(16) . . ? C19 C17 C19A 71.0(11) . . ? C19B C17 C19A 133.6(14) . . ? C20B C17 C19A 64.6(12) . . ? C20A C17 C16 120.2(13) . . ? C19 C17 C16 110.0(5) . . ? C19B C17 C16 113.7(11) . . ? C20B C17 C16 107.2(11) . . ? C19A C17 C16 110.2(10) . . ? C20A C17 C20 80.1(12) . . ? C19 C17 C20 113.4(6) . . ? C19B C17 C20 130.6(11) . . ? C16 C17 C20 105.5(5) . . ? C20A C17 C18A 102.4(16) . . ? C20B C17 C18A 151.1(15) . . ? C19A C17 C18A 108.2(14) . . ? C16 C17 C18A 101.6(10) . . ? C20 C17 C18A 146.9(11) . . ? C20A C17 C18B 135.4(16) . . ? C19B C17 C18B 109.8(11) . . ? C20B C17 C18B 107.1(10) . . ? C16 C17 C18B 104.4(10) . . ? C20 C17 C18B 87.2(10) . . ? C18A C17 C18B 67.7(12) . . ? C19 C17 C18 111.9(6) . . ? C20B C17 C18 83.0(9) . . ? C19A C17 C18 132.1(11) . . ? C16 C17 C18 112.6(5) . . ? C20 C17 C18 103.1(6) . . ? C18A C17 C18 83.3(10) . . ? C18B C17 C18 136.7(10) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? C17 C18A H18D 109.5 . . ? C17 C18A H18E 109.5 . . ? H18D C18A H18E 109.5 . . ? C17 C18A H18F 109.5 . . ? H18D C18A H18F 109.5 . . ? H18E C18A H18F 109.5 . . ? C17 C19A H19D 109.5 . . ? C17 C19A H19E 109.5 . . ? H19D C19A H19E 109.5 . . ? C17 C19A H19F 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? C17 C19A H19G 109.5 . . ? H19D C19A H19G 141.1 . . ? H19E C19A H19G 56.3 . . ? H19F C19A H19G 56.3 . . ? C17 C19A H19H 109.5 . . ? H19D C19A H19H 56.3 . . ? H19E C19A H19H 141.1 . . ? H19F C19A H19H 56.3 . . ? H19G C19A H19H 109.5 . . ? C17 C19A H19I 109.5 . . ? H19D C19A H19I 56.3 . . ? H19E C19A H19I 56.3 . . ? H19F C19A H19I 141.1 . . ? H19G C19A H19I 109.5 . . ? H19H C19A H19I 109.5 . . ? C17 C20A H20D 109.5 . . ? C17 C20A H20E 109.5 . . ? H20D C20A H20E 109.5 . . ? C17 C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? C17 C20A H20G 109.5 . . ? H20D C20A H20G 141.1 . . ? H20E C20A H20G 56.3 . . ? H20F C20A H20G 56.3 . . ? C17 C20A H20H 109.5 . . ? H20D C20A H20H 56.3 . . ? H20E C20A H20H 141.1 . . ? H20F C20A H20H 56.3 . . ? H20G C20A H20H 109.5 . . ? C17 C20A H20I 109.5 . . ? H20D C20A H20I 56.3 . . ? H20E C20A H20I 56.3 . . ? H20F C20A H20I 141.1 . . ? H20G C20A H20I 109.5 . . ? H20H C20A H20I 109.5 . . ? C17 C18B H18G 109.5 . . ? C17 C18B H18H 109.5 . . ? C17 C18B H18I 109.5 . . ? C17 C19B H19J 109.5 . . ? C17 C19B H19K 109.5 . . ? C17 C19B H19L 109.5 . . ? C17 C20B H20J 109.5 . . ? C17 C20B H20K 109.5 . . ? C17 C20B H20L 109.5 . . ? C24 C21 H21A 109.5 . . ? C24 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C24 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C22 H22A 109.5 . . ? C24 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C24 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 C22 109.4(5) . . ? C21 C24 C23 108.5(5) . . ? C22 C24 C23 109.3(5) . . ? C21 C24 C25 109.0(4) . . ? C22 C24 C25 114.3(4) . . ? C23 C24 C25 106.3(4) . . ? O5 C25 C26 124.6(4) . . ? O5 C25 C24 114.4(4) . . ? C26 C25 C24 120.9(4) . . ? C25 C26 C27 127.1(4) . . ? C25 C26 H26 116.4 . . ? C27 C26 H26 116.4 . . ? O6 C27 C26 125.7(4) . . ? O6 C27 C28 115.4(3) . . ? C26 C27 C28 118.9(4) . . ? C33 C28 C29 118.4(4) . . ? C33 C28 C27 120.0(3) . . ? C29 C28 C27 121.5(4) . . ? C30 C29 C28 120.0(4) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C31 C30 C29 120.7(4) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C30 C31 C32 121.6(4) . . ? C30 C31 H31 119.2 . . ? C32 C31 H31 119.2 . . ? C33 C32 C31 117.3(4) . . ? C33 C32 C34 119.4(3) . . ? C31 C32 C34 123.3(4) . . ? C32 C33 C28 122.0(4) . . ? C32 C33 H33 119.0 . . ? C28 C33 H33 119.0 . . ? O7 C34 C35 124.1(4) . . ? O7 C34 C32 116.1(3) . . ? C35 C34 C32 119.8(4) . . ? C34 C35 C36 127.4(4) . . ? C34 C35 H35 116.3 . . ? C36 C35 H35 116.3 . . ? O8 C36 C35 125.0(4) . . ? O8 C36 C37 115.3(4) . . ? C35 C36 C37 119.6(4) . . ? C40B C37 C39 88.1(14) . . ? C40B C37 C40A 53.5(13) . . ? C39 C37 C40A 134.3(9) . . ? C40B C37 C39A 129.2(14) . . ? C39 C37 C39A 67.2(8) . . ? C40A C37 C39A 115.6(10) . . ? C40B C37 C36 115.4(13) . . ? C39 C37 C36 109.7(6) . . ? C40A C37 C36 109.1(8) . . ? C39A C37 C36 114.6(7) . . ? C40B C37 C38 122.4(14) . . ? C39 C37 C38 107.6(8) . . ? C40A C37 C38 80.1(9) . . ? C36 C37 C38 110.5(6) . . ? C39 C37 C40 114.0(8) . . ? C39A C37 C40 132.5(9) . . ? C36 C37 C40 109.2(6) . . ? C38 C37 C40 105.8(8) . . ? C40B C37 C38A 56.5(13) . . ? C40A C37 C38A 109.8(10) . . ? C39A C37 C38A 103.8(10) . . ? C36 C37 C38A 102.9(7) . . ? C38 C37 C38A 139.8(9) . . ? C40 C37 C38A 82.9(8) . . ? C40B C37 C38B 107.5(16) . . ? C39 C37 C38B 132.7(12) . . ? C40A C37 C38B 56.9(12) . . ? C39A C37 C38B 68.6(12) . . ? C36 C37 C38B 103.2(11) . . ? C40 C37 C38B 84.6(12) . . ? C38A C37 C38B 153.5(13) . . ? C40B C37 C39B 113.7(17) . . ? C40A C37 C39B 136.7(13) . . ? C36 C37 C39B 112.9(11) . . ? C38 C37 C39B 75.9(12) . . ? C40 C37 C39B 134.0(12) . . ? C38A C37 C39B 70.8(13) . . ? C38B C37 C39B 102.5(16) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? C37 C38A H38D 109.5 . . ? C37 C38A H38E 109.5 . . ? H38D C38A H38E 109.5 . . ? C37 C38A H38F 109.5 . . ? H38D C38A H38F 109.5 . . ? H38E C38A H38F 109.5 . . ? C37 C39A H39D 109.5 . . ? C37 C39A H39E 109.5 . . ? H39D C39A H39E 109.5 . . ? C37 C39A H39F 109.5 . . ? H39D C39A H39F 109.5 . . ? H39E C39A H39F 109.5 . . ? C37 C40A H40D 109.5 . . ? C37 C40A H40E 109.5 . . ? H40D C40A H40E 109.5 . . ? C37 C40A H40F 109.5 . . ? H40D C40A H40F 109.5 . . ? H40E C40A H40F 109.5 . . ? C37 C38B H38G 109.5 . . ? C37 C38B H38H 109.5 . . ? C37 C38B H38I 109.5 . . ? C37 C39B H39G 109.5 . . ? C37 C39B H39H 109.5 . . ? H39G C39B H39H 109.5 . . ? C37 C39B H39I 109.5 . . ? H39G C39B H39I 109.5 . . ? H39H C39B H39I 109.5 . . ? C37 C39B H39J 109.5 . . ? H39G C39B H39J 141.1 . . ? H39H C39B H39J 56.3 . . ? H39I C39B H39J 56.3 . . ? C37 C39B H39K 109.5 . . ? H39G C39B H39K 56.3 . . ? H39H C39B H39K 141.1 . . ? H39I C39B H39K 56.3 . . ? H39J C39B H39K 109.5 . . ? C37 C39B H39L 109.5 . . ? H39G C39B H39L 56.3 . . ? H39H C39B H39L 56.3 . . ? H39I C39B H39L 141.1 . . ? H39J C39B H39L 109.5 . . ? H39K C39B H39L 109.5 . . ? C37 C40B H40G 109.5 . . ? C37 C40B H40H 109.5 . . ? H40G C40B H40H 109.5 . . ? C37 C40B H40I 109.5 . . ? H40G C40B H40I 109.5 . . ? H40H C40B H40I 109.5 . . ? C37 C40B H40J 109.5 . . ? H40G C40B H40J 141.1 . . ? H40H C40B H40J 56.3 . . ? H40I C40B H40J 56.3 . . ? C37 C40B H40K 109.5 . . ? H40G C40B H40K 56.3 . . ? H40H C40B H40K 141.1 . . ? H40I C40B H40K 56.3 . . ? H40J C40B H40K 109.5 . . ? C37 C40B H40L 109.5 . . ? H40G C40B H40L 56.3 . . ? H40H C40B H40L 56.3 . . ? H40I C40B H40L 141.1 . . ? H40J C40B H40L 109.5 . . ? H40K C40B H40L 109.5 . . ? N1 C41 C42 123.4(5) . . ? N1 C41 H41 118.3 . . ? C42 C41 H41 118.3 . . ? C43 C42 C41 119.3(5) . . ? C43 C42 H42 120.3 . . ? C41 C42 H42 120.3 . . ? C46A C43 C44 132(2) . . ? C46A C43 C42 110(2) . . ? C44 C43 C42 116.4(5) . . ? C44 C43 C46B 120(2) . . ? C42 C43 C46B 122(2) . . ? C44 C43 C46 115.0(8) . . ? C42 C43 C46 128.4(8) . . ? C45 C44 C43 120.5(5) . . ? C45 C44 H44 119.7 . . ? C43 C44 H44 119.7 . . ? N1 C45 C44 124.8(5) . . ? N1 C45 H45 117.6 . . ? C44 C45 H45 117.6 . . ? C47 C46 C43 101.5(11) . . ? C47 C46 H46A 111.5 . . ? C43 C46 H46A 111.5 . . ? C47 C46 H46B 111.5 . . ? C43 C46 H46B 111.5 . . ? H46A C46 H46B 109.3 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46A C47A H47D 109.5 . . ? C46A C47A H47E 109.5 . . ? H47D C47A H47E 109.5 . . ? C46A C47A H47F 109.5 . . ? H47D C47A H47F 109.5 . . ? H47E C47A H47F 109.5 . . ? C43 C46A C47A 141(4) . . ? C43 C46A H46C 101.8 . . ? C47A C46A H46C 101.8 . . ? C43 C46A H46D 101.8 . . ? C47A C46A H46D 101.8 . . ? H46C C46A H46D 104.7 . . ? C47B C46B C43 125(3) . . ? C47B C46B H46E 106.0 . . ? C43 C46B H46E 106.0 . . ? C47B C46B H46F 106.0 . . ? C43 C46B H46F 106.0 . . ? H46E C46B H46F 106.3 . . ? C46B C47B H47G 109.5 . . ? C46B C47B H47H 109.5 . . ? H47G C47B H47H 109.5 . . ? C46B C47B H47I 109.5 . . ? H47G C47B H47I 109.5 . . ? H47H C47B H47I 109.5 . . ? N2 C48 C49 124.2(4) . . ? N2 C48 H48 117.9 . . ? C49 C48 H48 117.9 . . ? C48 C49 C50 120.0(5) . . ? C48 C49 H49 120.0 . . ? C50 C49 H49 120.0 . . ? C51 C50 C49 116.1(4) . . ? C51 C50 C53 120.3(8) . . ? C49 C50 C53 123.1(9) . . ? C51 C50 C53B 122.9(14) . . ? C49 C50 C53B 120.5(14) . . ? C50 C51 C52 120.6(4) . . ? C50 C51 H51 119.7 . . ? C52 C51 H51 119.7 . . ? N2 C52 C51 123.7(4) . . ? N2 C52 H52 118.2 . . ? C51 C52 H52 118.2 . . ? C54 C53 C50 120.1(13) . . ? C54 C53 H53A 107.3 . . ? C50 C53 H53A 107.3 . . ? C54 C53 H53B 107.3 . . ? C50 C53 H53B 107.3 . . ? H53A C53 H53B 106.9 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C54B C53B C50 125(2) . . ? C54B C53B H53E 106.0 . . ? C50 C53B H53E 106.0 . . ? C54B C53B H53F 106.0 . . ? C50 C53B H53F 106.0 . . ? H53E C53B H53F 106.3 . . ? C53B C54B H54G 109.5 . . ? C53B C54B H54H 109.5 . . ? H54G C54B H54H 109.5 . . ? C53B C54B H54I 109.5 . . ? H54G C54B H54I 109.5 . . ? H54H C54B H54I 109.5 . . ? N3 C55 C56 123.3(4) . . ? N3 C55 H55 118.4 . . ? C56 C55 H55 118.4 . . ? C55 C56 C57 120.1(5) . . ? C55 C56 H56 119.9 . . ? C57 C56 H56 119.9 . . ? C58 C57 C56 116.6(4) . . ? C58 C57 C60A 121.2(9) . . ? C56 C57 C60A 121.8(9) . . ? C58 C57 C60 125.2(8) . . ? C56 C57 C60 116.9(7) . . ? C58 C57 C60B 103.6(15) . . ? C56 C57 C60B 136.3(16) . . ? C57 C58 C59 120.2(4) . . ? C57 C58 H58 119.9 . . ? C59 C58 H58 119.9 . . ? N3 C59 C58 123.1(4) . . ? N3 C59 H59 118.5 . . ? C58 C59 H59 118.5 . . ? C61 C60 C57 106.1(10) . . ? C61 C60 H60A 110.5 . . ? C57 C60 H60A 110.5 . . ? C61 C60 H60B 110.5 . . ? C57 C60 H60B 110.5 . . ? H60A C60 H60B 108.7 . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60A C61A H61D 109.5 . . ? C60A C61A H61E 109.5 . . ? H61D C61A H61E 109.5 . . ? C60A C61A H61F 109.5 . . ? H61D C61A H61F 109.5 . . ? H61E C61A H61F 109.5 . . ? C61A C60A C57 119.2(14) . . ? C61A C60A H60C 107.5 . . ? C57 C60A H60C 107.5 . . ? C61A C60A H60D 107.5 . . ? C57 C60A H60D 107.5 . . ? H60C C60A H60D 107.0 . . ? C61B C60B C57 96(3) . . ? C61B C60B H60E 112.5 . . ? C57 C60B H60E 112.5 . . ? C61B C60B H60F 112.5 . . ? C57 C60B H60F 112.5 . . ? H60E C60B H60F 110.0 . . ? C60B C61B H61G 109.5 . . ? C60B C61B H61H 109.5 . . ? H61G C61B H61H 109.5 . . ? C60B C61B H61I 109.5 . . ? H61G C61B H61I 109.5 . . ? H61H C61B H61I 109.5 . . ? N4 C62 C63 123.5(5) . . ? N4 C62 H62 118.3 . . ? C63 C62 H62 118.3 . . ? C62 C63 C64 120.4(5) . . ? C62 C63 H63 119.8 . . ? C64 C63 H63 119.8 . . ? C65 C64 C63 116.4(5) . . ? C65 C64 C67B 109(2) . . ? C63 C64 C67B 133(3) . . ? C65 C64 C67 116.3(17) . . ? C63 C64 C67 126.3(17) . . ? C65 C64 C67A 126.2(14) . . ? C63 C64 C67A 114.6(12) . . ? C64 C65 C66 120.6(5) . . ? C64 C65 H65 119.7 . . ? C66 C65 H65 119.7 . . ? N4 C66 C65 122.5(5) . . ? N4 C66 H66 118.8 . . ? C65 C66 H66 118.8 . . ? C68 C67 C64 104.9(18) . . ? C68 C67 H67A 110.8 . . ? C64 C67 H67A 110.8 . . ? C68 C67 H67B 110.8 . . ? C64 C67 H67B 110.8 . . ? H67A C67 H67B 108.8 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C68A C67A C64 87(2) . . ? C68A C67A H67C 114.2 . . ? C64 C67A H67C 114.2 . . ? C68A C67A H67D 114.2 . . ? C64 C67A H67D 114.2 . . ? H67C C67A H67D 111.4 . . ? C67A C68A H68D 109.5 . . ? C67A C68A H68E 109.5 . . ? H68D C68A H68E 109.5 . . ? C67A C68A H68F 109.5 . . ? H68D C68A H68F 109.5 . . ? H68E C68A H68F 109.5 . . ? C68B C67B C64 114(4) . . ? C68B C67B H67E 108.7 . . ? C64 C67B H67E 108.7 . . ? C68B C67B H67F 108.7 . . ? C64 C67B H67F 108.7 . . ? H67E C67B H67F 107.6 . . ? C67B C68B H68G 109.5 . . ? C67B C68B H68H 109.5 . . ? H68G C68B H68H 109.5 . . ? C67B C68B H68I 109.5 . . ? H68G C68B H68I 109.5 . . ? H68H C68B H68I 109.5 . . ? C41 N1 C45 115.5(5) . . ? C41 N1 Zn1 123.9(3) . . ? C45 N1 Zn1 119.1(3) . . ? C48 N2 C52 115.2(4) . . ? C48 N2 Zn1 121.1(3) . . ? C52 N2 Zn1 123.6(3) . . ? C55 N3 C59 116.8(4) . . ? C55 N3 Zn2 121.8(3) . . ? C59 N3 Zn2 121.4(3) . . ? C66 N4 C62 116.6(4) . . ? C66 N4 Zn2 123.5(3) . . ? C62 N4 Zn2 119.7(3) . . ? C5 O1 Zn1 127.1(2) . . ? C7 O2 Zn1 125.7(2) . . ? C14 O3 Zn1 125.9(2) . 2_566 ? C16 O4 Zn1 125.7(2) . 2_566 ? C25 O5 Zn2 126.4(3) . . ? C27 O6 Zn2 125.8(3) . . ? C34 O7 Zn2 124.5(2) . 2_455 ? C36 O8 Zn2 123.7(3) . 2_455 ? O1 Zn1 O2 89.03(11) . . ? O1 Zn1 O3 177.27(12) . 2_566 ? O2 Zn1 O3 89.80(11) . 2_566 ? O1 Zn1 O4 93.53(11) . 2_566 ? O2 Zn1 O4 177.03(10) . 2_566 ? O3 Zn1 O4 87.57(11) 2_566 2_566 ? O1 Zn1 N2 91.06(12) . . ? O2 Zn1 N2 92.73(12) . . ? O3 Zn1 N2 91.46(12) 2_566 . ? O4 Zn1 N2 88.73(12) 2_566 . ? O1 Zn1 N1 88.85(13) . . ? O2 Zn1 N1 93.71(12) . . ? O3 Zn1 N1 88.76(12) 2_566 . ? O4 Zn1 N1 84.85(12) 2_566 . ? N2 Zn1 N1 173.56(12) . . ? O7 Zn2 O6 89.16(11) 2_455 . ? O7 Zn2 O8 87.84(12) 2_455 2_455 ? O6 Zn2 O8 174.61(11) . 2_455 ? O7 Zn2 O5 176.06(11) 2_455 . ? O6 Zn2 O5 88.13(12) . . ? O8 Zn2 O5 94.64(12) 2_455 . ? O7 Zn2 N3 93.58(13) 2_455 . ? O6 Zn2 N3 96.02(12) . . ? O8 Zn2 N3 88.64(13) 2_455 . ? O5 Zn2 N3 89.55(13) . . ? O7 Zn2 N4 90.13(13) 2_455 . ? O6 Zn2 N4 89.68(13) . . ? O8 Zn2 N4 85.85(13) 2_455 . ? O5 Zn2 N4 87.00(13) . . ? N3 Zn2 N4 173.25(13) . . ? 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 C2A C4 C5 O1 -36.7(8) . . . . ? C2 C4 C5 O1 52.4(6) . . . . ? C3 C4 C5 O1 172.0(5) . . . . ? C1A C4 C5 O1 -162.9(6) . . . . ? C1 C4 C5 O1 -63.5(6) . . . . ? C3A C4 C5 O1 75.3(6) . . . . ? C2A C4 C5 C6 144.9(7) . . . . ? C2 C4 C5 C6 -126.0(5) . . . . ? C3 C4 C5 C6 -6.4(7) . . . . ? C1A C4 C5 C6 18.8(8) . . . . ? C1 C4 C5 C6 118.1(5) . . . . ? C3A C4 C5 C6 -103.1(6) . . . . ? O1 C5 C6 C7 -3.3(7) . . . . ? C4 C5 C6 C7 174.9(4) . . . . ? C5 C6 C7 O2 2.6(7) . . . . ? C5 C6 C7 C8 -177.9(4) . . . . ? O2 C7 C8 C13 17.0(5) . . . . ? C6 C7 C8 C13 -162.6(4) . . . . ? O2 C7 C8 C9 -165.1(4) . . . . ? C6 C7 C8 C9 15.3(6) . . . . ? C13 C8 C9 C10 0.6(6) . . . . ? C7 C8 C9 C10 -177.3(4) . . . . ? C8 C9 C10 C11 -0.4(7) . . . . ? C9 C10 C11 C12 -0.4(7) . . . . ? C10 C11 C12 C13 1.0(6) . . . . ? C10 C11 C12 C14 178.8(4) . . . . ? C11 C12 C13 C8 -0.8(6) . . . . ? C14 C12 C13 C8 -178.7(3) . . . . ? C9 C8 C13 C12 0.0(6) . . . . ? C7 C8 C13 C12 178.1(3) . . . . ? C13 C12 C14 O3 17.9(5) . . . . ? C11 C12 C14 O3 -159.9(4) . . . . ? C13 C12 C14 C15 -162.1(4) . . . . ? C11 C12 C14 C15 20.1(6) . . . . ? O3 C14 C15 C16 0.1(7) . . . . ? C12 C14 C15 C16 -179.9(4) . . . . ? C14 C15 C16 O4 -0.5(7) . . . . ? C14 C15 C16 C17 179.1(4) . . . . ? O4 C16 C17 C20A 146.2(14) . . . . ? C15 C16 C17 C20A -33.5(15) . . . . ? O4 C16 C17 C19 -63.9(6) . . . . ? C15 C16 C17 C19 116.5(6) . . . . ? O4 C16 C17 C19B -152.0(11) . . . . ? C15 C16 C17 C19B 28.4(12) . . . . ? O4 C16 C17 C20B 81.1(10) . . . . ? C15 C16 C17 C20B -98.6(10) . . . . ? O4 C16 C17 C19A 12.5(13) . . . . ? C15 C16 C17 C19A -167.1(12) . . . . ? O4 C16 C17 C20 58.7(6) . . . . ? C15 C16 C17 C20 -120.9(5) . . . . ? O4 C16 C17 C18A -102.0(11) . . . . ? C15 C16 C17 C18A 78.3(11) . . . . ? O4 C16 C17 C18B -32.4(10) . . . . ? C15 C16 C17 C18B 148.0(10) . . . . ? O4 C16 C17 C18 170.5(5) . . . . ? C15 C16 C17 C18 -9.1(7) . . . . ? C21 C24 C25 O5 -43.9(5) . . . . ? C22 C24 C25 O5 -166.5(5) . . . . ? C23 C24 C25 O5 72.9(6) . . . . ? C21 C24 C25 C26 139.0(5) . . . . ? C22 C24 C25 C26 16.4(7) . . . . ? C23 C24 C25 C26 -104.3(5) . . . . ? O5 C25 C26 C27 -2.0(7) . . . . ? C24 C25 C26 C27 174.8(4) . . . . ? C25 C26 C27 O6 4.7(7) . . . . ? C25 C26 C27 C28 -175.1(4) . . . . ? O6 C27 C28 C33 25.2(5) . . . . ? C26 C27 C28 C33 -155.0(4) . . . . ? O6 C27 C28 C29 -151.2(4) . . . . ? C26 C27 C28 C29 28.6(6) . . . . ? C33 C28 C29 C30 0.0(6) . . . . ? C27 C28 C29 C30 176.5(4) . . . . ? C28 C29 C30 C31 0.7(7) . . . . ? C29 C30 C31 C32 -1.0(7) . . . . ? C30 C31 C32 C33 0.6(6) . . . . ? C30 C31 C32 C34 -178.1(4) . . . . ? C31 C32 C33 C28 0.1(6) . . . . ? C34 C32 C33 C28 178.9(3) . . . . ? C29 C28 C33 C32 -0.4(6) . . . . ? C27 C28 C33 C32 -177.0(4) . . . . ? C33 C32 C34 O7 17.2(5) . . . . ? C31 C32 C34 O7 -164.0(4) . . . . ? C33 C32 C34 C35 -162.2(4) . . . . ? C31 C32 C34 C35 16.5(6) . . . . ? O7 C34 C35 C36 1.2(7) . . . . ? C32 C34 C35 C36 -179.4(4) . . . . ? C34 C35 C36 O8 -1.6(7) . . . . ? C34 C35 C36 C37 177.4(4) . . . . ? O8 C36 C37 C40B 10.3(15) . . . . ? C35 C36 C37 C40B -168.8(14) . . . . ? O8 C36 C37 C39 107.8(8) . . . . ? C35 C36 C37 C39 -71.2(8) . . . . ? O8 C36 C37 C40A -47.5(9) . . . . ? C35 C36 C37 C40A 133.4(8) . . . . ? O8 C36 C37 C39A -178.9(9) . . . . ? C35 C36 C37 C39A 2.0(10) . . . . ? O8 C36 C37 C38 -133.7(7) . . . . ? C35 C36 C37 C38 47.2(8) . . . . ? O8 C36 C37 C40 -17.8(8) . . . . ? C35 C36 C37 C40 163.1(7) . . . . ? O8 C36 C37 C38A 69.1(8) . . . . ? C35 C36 C37 C38A -110.0(8) . . . . ? O8 C36 C37 C38B -106.7(12) . . . . ? C35 C36 C37 C38B 74.3(12) . . . . ? O8 C36 C37 C39B 143.4(14) . . . . ? C35 C36 C37 C39B -35.6(15) . . . . ? N1 C41 C42 C43 -0.8(9) . . . . ? C41 C42 C43 C46A 169(2) . . . . ? C41 C42 C43 C44 1.7(9) . . . . ? C41 C42 C43 C46B -165.9(17) . . . . ? C41 C42 C43 C46 -173.6(9) . . . . ? C46A C43 C44 C45 -165(3) . . . . ? C42 C43 C44 C45 -1.5(9) . . . . ? C46B C43 C44 C45 166.5(18) . . . . ? C46 C43 C44 C45 174.4(8) . . . . ? C43 C44 C45 N1 0.3(10) . . . . ? C46A C43 C46 C47 22(6) . . . . ? C44 C43 C46 C47 161.5(9) . . . . ? C42 C43 C46 C47 -23.1(15) . . . . ? C46B C43 C46 C47 -72(13) . . . . ? C44 C43 C46A C47A 130(7) . . . . ? C42 C43 C46A C47A -35(8) . . . . ? C46B C43 C46A C47A -158(15) . . . . ? C46 C43 C46A C47A -179(13) . . . . ? C46A C43 C46B C47B -4(6) . . . . ? C44 C43 C46B C47B 121(4) . . . . ? C42 C43 C46B C47B -72(5) . . . . ? C46 C43 C46B C47B 64(11) . . . . ? N2 C48 C49 C50 -1.5(9) . . . . ? C48 C49 C50 C51 0.5(8) . . . . ? C48 C49 C50 C53 172.4(10) . . . . ? C48 C49 C50 C53B -172.3(14) . . . . ? C49 C50 C51 C52 0.8(7) . . . . ? C53 C50 C51 C52 -171.3(9) . . . . ? C53B C50 C51 C52 173.5(14) . . . . ? C50 C51 C52 N2 -1.4(7) . . . . ? C51 C50 C53 C54 176.2(12) . . . . ? C49 C50 C53 C54 5(2) . . . . ? C53B C50 C53 C54 -78(8) . . . . ? C51 C50 C53B C54B -147(2) . . . . ? C49 C50 C53B C54B 25(4) . . . . ? C53 C50 C53B C54B 130(11) . . . . ? N3 C55 C56 C57 0.8(9) . . . . ? C55 C56 C57 C58 -0.9(8) . . . . ? C55 C56 C57 C60A -173.5(9) . . . . ? C55 C56 C57 C60 166.8(7) . . . . ? C55 C56 C57 C60B -156(2) . . . . ? C56 C57 C58 C59 0.6(7) . . . . ? C60A C57 C58 C59 173.3(9) . . . . ? C60 C57 C58 C59 -166.0(7) . . . . ? C60B C57 C58 C59 163.0(17) . . . . ? C57 C58 C59 N3 -0.1(7) . . . . ? C58 C57 C60 C61 -117.1(10) . . . . ? C56 C57 C60 C61 76.3(11) . . . . ? C60A C57 C60 C61 -34(4) . . . . ? C60B C57 C60 C61 -57(3) . . . . ? C58 C57 C60A C61A -98.7(17) . . . . ? C56 C57 C60A C61A 73.5(16) . . . . ? C60 C57 C60A C61A 153(5) . . . . ? C60B C57 C60A C61A -68(6) . . . . ? C58 C57 C60B C61B 165(2) . . . . ? C56 C57 C60B C61B -38(4) . . . . ? C60A C57 C60B C61B 12(5) . . . . ? C60 C57 C60B C61B 32(2) . . . . ? N4 C62 C63 C64 1.2(9) . . . . ? C62 C63 C64 C65 -0.6(11) . . . . ? C62 C63 C64 C67B -162(5) . . . . ? C62 C63 C64 C67 167.6(13) . . . . ? C62 C63 C64 C67A -162.8(18) . . . . ? C63 C64 C65 C66 -0.3(11) . . . . ? C67B C64 C65 C66 166(4) . . . . ? C67 C64 C65 C66 -169.7(13) . . . . ? C67A C64 C65 C66 159.6(19) . . . . ? C64 C65 C66 N4 0.6(10) . . . . ? C65 C64 C67 C68 -117(2) . . . . ? C63 C64 C67 C68 75(3) . . . . ? C67B C64 C67 C68 -40(7) . . . . ? C67A C64 C67 C68 1(4) . . . . ? C65 C64 C67A C68A 96(3) . . . . ? C63 C64 C67A C68A -104(2) . . . . ? C67B C64 C67A C68A 78(14) . . . . ? C67 C64 C67A C68A 18(5) . . . . ? C65 C64 C67B C68B 151(7) . . . . ? C63 C64 C67B C68B -47(10) . . . . ? C67 C64 C67B C68B 38(5) . . . . ? C67A C64 C67B C68B -45(9) . . . . ? C42 C41 N1 C45 -0.5(8) . . . . ? C42 C41 N1 Zn1 165.5(4) . . . . ? C44 C45 N1 C41 0.8(8) . . . . ? C44 C45 N1 Zn1 -165.9(5) . . . . ? C49 C48 N2 C52 0.9(7) . . . . ? C49 C48 N2 Zn1 177.5(4) . . . . ? C51 C52 N2 C48 0.5(6) . . . . ? C51 C52 N2 Zn1 -176.0(3) . . . . ? C56 C55 N3 C59 -0.2(7) . . . . ? C56 C55 N3 Zn2 179.4(4) . . . . ? C58 C59 N3 C55 -0.1(6) . . . . ? C58 C59 N3 Zn2 -179.8(3) . . . . ? C65 C66 N4 C62 -0.1(8) . . . . ? C65 C66 N4 Zn2 175.2(5) . . . . ? C63 C62 N4 C66 -0.8(8) . . . . ? C63 C62 N4 Zn2 -176.3(4) . . . . ? C6 C5 O1 Zn1 -6.4(6) . . . . ? C4 C5 O1 Zn1 175.3(3) . . . . ? C6 C7 O2 Zn1 7.6(6) . . . . ? C8 C7 O2 Zn1 -172.0(2) . . . . ? C15 C14 O3 Zn1 14.8(6) . . . 2_566 ? C12 C14 O3 Zn1 -165.2(2) . . . 2_566 ? C15 C16 O4 Zn1 -13.8(6) . . . 2_566 ? C17 C16 O4 Zn1 166.5(3) . . . 2_566 ? C26 C25 O5 Zn2 -11.3(6) . . . . ? C24 C25 O5 Zn2 171.7(3) . . . . ? C26 C27 O6 Zn2 6.4(6) . . . . ? C28 C27 O6 Zn2 -173.8(2) . . . . ? C35 C34 O7 Zn2 18.9(5) . . . 2_455 ? C32 C34 O7 Zn2 -160.5(2) . . . 2_455 ? C35 C36 O8 Zn2 -18.0(6) . . . 2_455 ? C37 C36 O8 Zn2 163.0(3) . . . 2_455 ? C5 O1 Zn1 O2 11.3(3) . . . . ? C5 O1 Zn1 O4 -167.2(3) . . . 2_566 ? C5 O1 Zn1 N2 104.0(3) . . . . ? C5 O1 Zn1 N1 -82.4(3) . . . . ? C7 O2 Zn1 O1 -11.8(3) . . . . ? C7 O2 Zn1 O3 165.8(3) . . . 2_566 ? C7 O2 Zn1 N2 -102.8(3) . . . . ? C7 O2 Zn1 N1 77.0(3) . . . . ? C48 N2 Zn1 O1 134.7(3) . . . . ? C52 N2 Zn1 O1 -49.0(3) . . . . ? C48 N2 Zn1 O2 -136.2(3) . . . . ? C52 N2 Zn1 O2 40.1(3) . . . . ? C48 N2 Zn1 O3 -46.3(3) . . . 2_566 ? C52 N2 Zn1 O3 129.9(3) . . . 2_566 ? C48 N2 Zn1 O4 41.2(3) . . . 2_566 ? C52 N2 Zn1 O4 -142.5(3) . . . 2_566 ? C41 N1 Zn1 O1 159.4(4) . . . . ? C45 N1 Zn1 O1 -35.1(4) . . . . ? C41 N1 Zn1 O2 70.4(4) . . . . ? C45 N1 Zn1 O2 -124.1(4) . . . . ? C41 N1 Zn1 O3 -19.3(4) . . . 2_566 ? C45 N1 Zn1 O3 146.2(4) . . . 2_566 ? C41 N1 Zn1 O4 -107.0(4) . . . 2_566 ? C45 N1 Zn1 O4 58.5(4) . . . 2_566 ? C27 O6 Zn2 O7 164.1(3) . . . 2_455 ? C27 O6 Zn2 O5 -13.1(3) . . . . ? C27 O6 Zn2 N3 -102.4(3) . . . . ? C27 O6 Zn2 N4 73.9(3) . . . . ? C25 O5 Zn2 O6 15.7(3) . . . . ? C25 O5 Zn2 O8 -159.7(3) . . . 2_455 ? C25 O5 Zn2 N3 111.7(3) . . . . ? C25 O5 Zn2 N4 -74.1(3) . . . . ? C55 N3 Zn2 O7 154.0(4) . . . 2_455 ? C59 N3 Zn2 O7 -26.3(3) . . . 2_455 ? C55 N3 Zn2 O6 64.5(4) . . . . ? C59 N3 Zn2 O6 -115.8(3) . . . . ? C55 N3 Zn2 O8 -118.2(4) . . . 2_455 ? C59 N3 Zn2 O8 61.4(3) . . . 2_455 ? C55 N3 Zn2 O5 -23.6(4) . . . . ? C59 N3 Zn2 O5 156.1(3) . . . . ? C66 N4 Zn2 O7 -34.6(4) . . . 2_455 ? C62 N4 Zn2 O7 140.6(4) . . . 2_455 ? C66 N4 Zn2 O6 54.6(4) . . . . ? C62 N4 Zn2 O6 -130.3(4) . . . . ? C66 N4 Zn2 O8 -122.4(4) . . . 2_455 ? C62 N4 Zn2 O8 52.7(4) . . . 2_455 ? C66 N4 Zn2 O5 142.7(4) . . . . ? C62 N4 Zn2 O5 -42.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.526 _refine_diff_density_min -0.630 _refine_diff_density_rms 0.065 data_lj76sad _database_code_depnum_ccdc_archive 'CCDC 635437' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H48 O8 Ni2, 4(N1 C7 H9)' _chemical_formula_sum 'C68 H84 N4 Ni2 O8' _chemical_formula_weight 1202.81 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' Ni Ni 0.3393 1.1124 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2040(16) _cell_length_b 17.332(2) _cell_length_c 18.061(2) _cell_angle_alpha 117.185(2) _cell_angle_beta 99.516(2) _cell_angle_gamma 102.001(2) _cell_volume 3171.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9104 _cell_measurement_theta_min 2.401 _cell_measurement_theta_max 25.5705 _exptl_crystal_description Prism _exptl_crystal_colour green _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.259 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 0.650 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.73745726 _exptl_absorpt_correction_T_max 0.94 _exptl_absorpt_process_details 'SADABS, (Sheldrick, 2003)' _exptl_special_details ; The crystal was coated in Exxon Paratone N hydrocarbon oil and mounted on a thin mohair fibre attached to a copper pin. Upon mounting on the diffractometer, the crystal was quenched to 150(K) under a cold nitrogen gas stream supplied by an Oxford Cryosystems Cryostream and data were collected at this temperature. ; _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 Nonius APEX 2' _diffrn_measurement_method /p _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 48275 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0641 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 28.38 _reflns_number_total 15697 _reflns_number_gt 10707 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX (Bruker Nonius, 2004)' _computing_cell_refinement 'SAINT (Bruker Nonius, 2004)' _computing_data_reduction 'SAINT (ibid), XPREP (Siemens, 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 (Farrugia, 2005) WINGX-32 (Farrugia, 2005) ; _computing_publication_material 'enCIFer 1.0 (CCDC, 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0960P)^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 15697 _refine_ls_number_parameters 741 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0860 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1594 _refine_ls_wR_factor_gt 0.1368 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 C1 C 0.2946(3) -0.0223(2) 0.17020(19) 0.0396(7) Uani 1 1 d . . . H1A H 0.2661 0.0021 0.1341 0.059 Uiso 1 1 calc R . . H1B H 0.2504 -0.0148 0.2123 0.059 Uiso 1 1 calc R . . H1C H 0.2835 -0.0875 0.1329 0.059 Uiso 1 1 calc R . . C2 C 0.4675(3) -0.0054(2) 0.27817(19) 0.0424(7) Uani 1 1 d . . . H2A H 0.4267 0.0081 0.3227 0.064 Uiso 1 1 calc R . . H2B H 0.5523 0.0248 0.3065 0.064 Uiso 1 1 calc R . . H2C H 0.4509 -0.0718 0.2433 0.064 Uiso 1 1 calc R . . C3 C 0.4960(3) 0.0139(2) 0.1539(2) 0.0428(7) Uani 1 1 d . . . H3A H 0.4848 -0.0517 0.1193 0.064 Uiso 1 1 calc R . . H3B H 0.5795 0.0475 0.1857 0.064 Uiso 1 1 calc R . . H3C H 0.4691 0.0357 0.1151 0.064 Uiso 1 1 calc R . . C4 C 0.4251(2) 0.02985(18) 0.21904(16) 0.0288(6) Uani 1 1 d . . . C5 C 0.4424(2) 0.13382(18) 0.26768(16) 0.0254(5) Uani 1 1 d . . . C6 C 0.5211(2) 0.19133(18) 0.35138(16) 0.0279(6) Uani 1 1 d . . . H6 H 0.5574 0.1632 0.3781 0.034 Uiso 1 1 calc R . . C7 C 0.5513(2) 0.28691(18) 0.39936(16) 0.0250(5) Uani 1 1 d . . . C8 C 0.6449(2) 0.33938(17) 0.48597(16) 0.0243(5) Uani 1 1 d . . . C13 C 0.7363(2) 0.30576(18) 0.50132(16) 0.0282(6) Uani 1 1 d . . . H13 H 0.7371 0.2479 0.4583 0.034 Uiso 1 1 calc R . . C12 C 0.8252(2) 0.35780(19) 0.57967(17) 0.0309(6) Uani 1 1 d . . . H12 H 0.8874 0.3355 0.5901 0.037 Uiso 1 1 calc R . . C11 C 0.8248(2) 0.44122(19) 0.64273(16) 0.0287(6) Uani 1 1 d . . . H11 H 0.8861 0.4755 0.6964 0.034 Uiso 1 1 calc R . . C10 C 0.7348(2) 0.47639(17) 0.62873(15) 0.0239(5) Uani 1 1 d . . . C9 C 0.6461(2) 0.42398(17) 0.54950(16) 0.0243(5) Uani 1 1 d . . . H9 H 0.5848 0.4469 0.5387 0.029 Uiso 1 1 calc R . . C14 C 0.7341(2) 0.56908(17) 0.69455(15) 0.0236(5) Uani 1 1 d . . . C15 C 0.8342(2) 0.62987(19) 0.76519(17) 0.0305(6) Uani 1 1 d . . . H15 H 0.9003 0.6094 0.7689 0.037 Uiso 1 1 calc R . . C16 C 0.8463(2) 0.71801(18) 0.83094(16) 0.0272(6) Uani 1 1 d . A . C17 C 0.9597(2) 0.7751(2) 0.90818(17) 0.0347(6) Uani 1 1 d . . . C18 C 0.9218(5) 0.7851(4) 0.9905(3) 0.0579(7) Uiso 0.70 1 d P A 1 H18A H 0.9904 0.8215 1.0425 0.087 Uiso 0.70 1 calc PR A 1 H18B H 0.8893 0.7242 0.9825 0.087 Uiso 0.70 1 calc PR A 1 H18C H 0.8621 0.8158 0.9976 0.087 Uiso 0.70 1 calc PR A 1 C19 C 1.0517(5) 0.7272(4) 0.9054(3) 0.0579(7) Uiso 0.70 1 d P A 1 H19A H 1.0170 0.6684 0.9013 0.087 Uiso 0.70 1 calc PR A 1 H19B H 1.1182 0.7659 0.9587 0.087 Uiso 0.70 1 calc PR A 1 H19C H 1.0790 0.7163 0.8546 0.087 Uiso 0.70 1 calc PR A 1 C20 C 1.0044(5) 0.8662(4) 0.9185(4) 0.0579(7) Uiso 0.70 1 d P A 1 H20A H 1.0690 0.9057 0.9729 0.087 Uiso 0.70 1 calc PR A 1 H20B H 0.9411 0.8932 0.9205 0.087 Uiso 0.70 1 calc PR A 1 H20C H 1.0327 0.8603 0.8691 0.087 Uiso 0.70 1 calc PR A 1 C18A C 1.0678(11) 0.7819(9) 0.8635(8) 0.0579(7) Uiso 0.30 1 d P A 2 H18D H 1.0832 0.7233 0.8384 0.087 Uiso 0.30 1 calc PR A 2 H18E H 1.1389 0.8305 0.9084 0.087 Uiso 0.30 1 calc PR A 2 H18F H 1.0447 0.7958 0.8176 0.087 Uiso 0.30 1 calc PR A 2 C19A C 0.9866(12) 0.7361(9) 0.9597(8) 0.0579(7) Uiso 0.30 1 d P A 2 H19D H 1.0484 0.7825 1.0141 0.087 Uiso 0.30 1 calc PR A 2 H19E H 1.0138 0.6845 0.9276 0.087 Uiso 0.30 1 calc PR A 2 H19F H 0.9162 0.7143 0.9733 0.087 Uiso 0.30 1 calc PR A 2 C20A C 0.9707(12) 0.8777(9) 0.9564(8) 0.0579(7) Uiso 0.30 1 d P A 2 H20D H 1.0515 0.9142 0.9940 0.087 Uiso 0.30 1 calc PR A 2 H20E H 0.9169 0.8877 0.9920 0.087 Uiso 0.30 1 calc PR A 2 H20F H 0.9506 0.8965 0.9137 0.087 Uiso 0.30 1 calc PR A 2 C21 C 0.6521(3) 0.8315(2) 0.50713(17) 0.0382(7) Uani 1 1 d . . . H21A H 0.6013 0.7736 0.4970 0.057 Uiso 1 1 calc R . . H21B H 0.6601 0.8811 0.5653 0.057 Uiso 1 1 calc R . . H21C H 0.7297 0.8265 0.5031 0.057 Uiso 1 1 calc R . . C22 C 0.4797(2) 0.8648(2) 0.44794(17) 0.0351(6) Uani 1 1 d . . . H22A H 0.4419 0.8735 0.4014 0.053 Uiso 1 1 calc R . . H22B H 0.4923 0.9187 0.5047 0.053 Uiso 1 1 calc R . . H22C H 0.4293 0.8103 0.4441 0.053 Uiso 1 1 calc R . . C23 C 0.6795(3) 0.94104(19) 0.45210(19) 0.0385(7) Uani 1 1 d . . . H23A H 0.7562 0.9342 0.4475 0.058 Uiso 1 1 calc R . . H23B H 0.6891 0.9918 0.5101 0.058 Uiso 1 1 calc R . . H23C H 0.6453 0.9539 0.4076 0.058 Uiso 1 1 calc R . . C24 C 0.5978(2) 0.85224(18) 0.43807(15) 0.0267(5) Uani 1 1 d . . . C25 C 0.5900(2) 0.77285(17) 0.34924(14) 0.0221(5) Uani 1 1 d . . . C26 C 0.4804(2) 0.71392(18) 0.28815(16) 0.0275(6) Uani 1 1 d . . . H26 H 0.4131 0.7287 0.3025 0.033 Uiso 1 1 calc R . . C27 C 0.4609(2) 0.63511(16) 0.20782(14) 0.0210(5) Uani 1 1 d . . . C28 C 0.3364(2) 0.57633(17) 0.15301(15) 0.0213(5) Uani 1 1 d . . . C33 C 0.2417(2) 0.58256(18) 0.18716(16) 0.0272(6) Uani 1 1 d . . . H33 H 0.2551 0.6234 0.2475 0.033 Uiso 1 1 calc R . . C32 C 0.1284(2) 0.52930(19) 0.13317(17) 0.0314(6) Uani 1 1 d . . . H32 H 0.0644 0.5345 0.1567 0.038 Uiso 1 1 calc R . . C31 C 0.1072(2) 0.46884(18) 0.04588(16) 0.0267(5) Uani 1 1 d . . . H31 H 0.0289 0.4331 0.0096 0.032 Uiso 1 1 calc R . . C30 C 0.2007(2) 0.45977(16) 0.01027(15) 0.0211(5) Uani 1 1 d . . . C29 C 0.3144(2) 0.51447(16) 0.06551(15) 0.0214(5) Uani 1 1 d . . . H29 H 0.3786 0.5090 0.0422 0.026 Uiso 1 1 calc R . . C34 C 0.1839(2) 0.39522(17) -0.08424(15) 0.0217(5) Uani 1 1 d . . . C35 C 0.0763(2) 0.32514(17) -0.13468(15) 0.0246(5) Uani 1 1 d . . . H35 H 0.0192 0.3205 -0.1057 0.030 Uiso 1 1 calc R . . C36 C 0.0451(2) 0.26139(16) -0.22375(15) 0.0219(5) Uani 1 1 d . . . C37 C -0.0791(2) 0.19241(18) -0.27189(16) 0.0275(6) Uani 1 1 d . . . C38 C -0.1601(2) 0.2016(2) -0.21422(18) 0.0365(7) Uani 1 1 d . . . H38A H -0.1695 0.2623 -0.1907 0.055 Uiso 1 1 calc R . . H38B H -0.1256 0.1939 -0.1660 0.055 Uiso 1 1 calc R . . H38C H -0.2369 0.1543 -0.2490 0.055 Uiso 1 1 calc R . . C39 C -0.0676(3) 0.09677(19) -0.3124(2) 0.0411(7) Uani 1 1 d . . . H39A H -0.0310 0.0871 -0.2662 0.062 Uiso 1 1 calc R . . H39B H -0.0186 0.0909 -0.3514 0.062 Uiso 1 1 calc R . . H39C H -0.1456 0.0508 -0.3458 0.062 Uiso 1 1 calc R . . C40 C -0.1326(2) 0.2085(2) -0.34413(17) 0.0352(6) Uani 1 1 d . . . H40A H -0.0800 0.2059 -0.3802 0.053 Uiso 1 1 calc R . . H40B H -0.1432 0.2689 -0.3181 0.053 Uiso 1 1 calc R . . H40C H -0.2089 0.1611 -0.3805 0.053 Uiso 1 1 calc R . . C41 C 0.2441(2) 0.3129(2) 0.40842(17) 0.0323(6) Uani 1 1 d . . . H41 H 0.3028 0.3715 0.4418 0.039 Uiso 1 1 calc R . . C42 C 0.1551(3) 0.2930(2) 0.44227(18) 0.0374(7) Uani 1 1 d . . . H42 H 0.1525 0.3380 0.4970 0.045 Uiso 1 1 calc R . . C43 C 0.0706(2) 0.2077(2) 0.39640(18) 0.0358(6) Uani 1 1 d . . . C44 C 0.0799(2) 0.1456(2) 0.31711(18) 0.0354(6) Uani 1 1 d . . . H44 H 0.0242 0.0857 0.2835 0.042 Uiso 1 1 calc R . . C45 C 0.1691(2) 0.17022(19) 0.28688(17) 0.0314(6) Uani 1 1 d . . . H45 H 0.1731 0.1264 0.2322 0.038 Uiso 1 1 calc R . . C46 C -0.0254(3) 0.1822(2) 0.4316(2) 0.0528(9) Uani 1 1 d . . . H46A H -0.0291 0.2387 0.4805 0.063 Uiso 1 1 calc R . . H46B H -0.1016 0.1531 0.3853 0.063 Uiso 1 1 calc R . . C47 C -0.0074(4) 0.1181(3) 0.4630(3) 0.0705(12) Uani 1 1 d . . . H47A H -0.0720 0.1037 0.4853 0.106 Uiso 1 1 calc R . . H47B H 0.0671 0.1471 0.5097 0.106 Uiso 1 1 calc R . . H47C H -0.0055 0.0614 0.4145 0.106 Uiso 1 1 calc R . . C48 C 0.5587(2) 0.2687(2) 0.17650(19) 0.0339(6) Uani 1 1 d . . . H48 H 0.5660 0.2265 0.1953 0.041 Uiso 1 1 calc R . . C49 C 0.6301(3) 0.2832(2) 0.1295(2) 0.0389(7) Uani 1 1 d . . . H49 H 0.6842 0.2504 0.1156 0.047 Uiso 1 1 calc R . . C50 C 0.6231(2) 0.34561(19) 0.10243(17) 0.0327(6) Uani 1 1 d . . . C51 C 0.5410(2) 0.38926(18) 0.12304(16) 0.0291(6) Uani 1 1 d . . . H51 H 0.5326 0.4323 0.1055 0.035 Uiso 1 1 calc R . . C52 C 0.4710(2) 0.37036(18) 0.16906(16) 0.0273(5) Uani 1 1 d . . . H52 H 0.4141 0.4005 0.1817 0.033 Uiso 1 1 calc R . . C53 C 0.7025(3) 0.3636(2) 0.0522(2) 0.0447(8) Uani 1 1 d . . . H53A H 0.7023 0.4215 0.0539 0.054 Uiso 1 1 calc R . . H53B H 0.7837 0.3717 0.0811 0.054 Uiso 1 1 calc R . . C54 C 0.6664(4) 0.2880(3) -0.0411(2) 0.0612(10) Uani 1 1 d . . . H54A H 0.7210 0.3031 -0.0703 0.092 Uiso 1 1 calc R . . H54B H 0.5868 0.2808 -0.0707 0.092 Uiso 1 1 calc R . . H54C H 0.6677 0.2306 -0.0434 0.092 Uiso 1 1 calc R . . C55 C 0.8305(2) 0.56247(19) 0.26984(18) 0.0333(6) Uani 1 1 d . . . H55 H 0.8816 0.5790 0.2413 0.040 Uiso 1 1 calc R . . C56 C 0.8531(2) 0.5063(2) 0.3008(2) 0.0414(7) Uani 1 1 d . B . H56 H 0.9187 0.4853 0.2935 0.050 Uiso 1 1 calc R . . C57 C 0.7811(2) 0.4804(2) 0.34212(19) 0.0368(7) Uani 1 1 d . . . C58 C 0.6871(2) 0.51281(19) 0.34981(17) 0.0323(6) Uani 1 1 d . B . H58 H 0.6339 0.4961 0.3770 0.039 Uiso 1 1 calc R . . C59 C 0.6705(2) 0.56919(18) 0.31814(16) 0.0283(6) Uani 1 1 d . . . H59 H 0.6057 0.5913 0.3250 0.034 Uiso 1 1 calc R B . C60 C 0.8007(9) 0.4116(6) 0.3703(6) 0.0504(9) Uiso 0.50 1 d P B 1 H60A H 0.7693 0.4229 0.4201 0.061 Uiso 0.50 1 calc PR B 1 H60B H 0.7532 0.3492 0.3216 0.061 Uiso 0.50 1 calc PR B 1 C61 C 0.9193(6) 0.4123(5) 0.3951(5) 0.0504(9) Uiso 0.50 1 d P B 1 H61A H 0.9218 0.3732 0.4205 0.076 Uiso 0.50 1 calc PR B 1 H61B H 0.9700 0.4751 0.4381 0.076 Uiso 0.50 1 calc PR B 1 H61C H 0.9468 0.3891 0.3434 0.076 Uiso 0.50 1 calc PR B 1 C61A C 0.8860(7) 0.3692(5) 0.3497(5) 0.0504(9) Uiso 0.50 1 d P B 2 H61D H 0.8942 0.3328 0.3775 0.076 Uiso 0.50 1 calc PR B 2 H61E H 0.9637 0.4096 0.3609 0.076 Uiso 0.50 1 calc PR B 2 H61F H 0.8498 0.3281 0.2866 0.076 Uiso 0.50 1 calc PR B 2 C60A C 0.8040(9) 0.4304(6) 0.3892(6) 0.0504(9) Uiso 0.50 1 d P B 2 H60C H 0.7285 0.3901 0.3834 0.061 Uiso 0.50 1 calc PR B 2 H60D H 0.8433 0.4751 0.4521 0.061 Uiso 0.50 1 calc PR B 2 C62 C 0.6604(2) 0.74513(19) 0.09764(17) 0.0343(6) Uani 1 1 d . . . H62 H 0.6201 0.6821 0.0563 0.041 Uiso 1 1 calc R . . C63 C 0.6763(3) 0.8066(2) 0.06777(18) 0.0385(7) Uani 1 1 d . . . H63 H 0.6482 0.7851 0.0072 0.046 Uiso 1 1 calc R . . C64 C 0.7331(2) 0.89871(19) 0.12632(17) 0.0310(6) Uani 1 1 d . . . C65 C 0.7673(2) 0.9244(2) 0.21346(17) 0.0330(6) Uani 1 1 d . . . H65 H 0.8031 0.9874 0.2568 0.040 Uiso 1 1 calc R . . C66 C 0.7497(2) 0.85995(18) 0.23742(16) 0.0298(6) Uani 1 1 d . . . H66 H 0.7753 0.8798 0.2977 0.036 Uiso 1 1 calc R . . C67 C 0.7629(3) 0.9693(2) 0.09921(19) 0.0398(7) Uani 1 1 d . . . H67A H 0.7555 1.0271 0.1434 0.048 Uiso 1 1 calc R . . H67B H 0.8461 0.9816 0.0998 0.048 Uiso 1 1 calc R . . C68 C 0.6894(3) 0.9438(3) 0.0117(2) 0.0518(9) Uani 1 1 d . . . H68A H 0.7153 0.9935 0.0002 0.078 Uiso 1 1 calc R . . H68B H 0.6070 0.9333 0.0106 0.078 Uiso 1 1 calc R . . H68C H 0.6978 0.8877 -0.0331 0.078 Uiso 1 1 calc R . . N1 N 0.25077(19) 0.25345(15) 0.33114(14) 0.0281(5) Uani 1 1 d . . . N2 N 0.47932(18) 0.31147(14) 0.19699(13) 0.0258(5) Uani 1 1 d . . . N3 N 0.74080(17) 0.59484(14) 0.27795(13) 0.0247(4) Uani 1 1 d . B . N4 N 0.69852(18) 0.77030(14) 0.18082(13) 0.0250(4) Uani 1 1 d . B . O1 O 0.38541(15) 0.15960(12) 0.22323(11) 0.0274(4) Uani 1 1 d . . . O2 O 0.50790(15) 0.33567(12) 0.37622(11) 0.0277(4) Uani 1 1 d . . . O3 O 0.63874(15) 0.58542(12) 0.67834(11) 0.0264(4) Uani 1 1 d . . . O4 O 0.76908(15) 0.75741(12) 0.83348(11) 0.0277(4) Uani 1 1 d . . . O5 O 0.68807(15) 0.76548(12) 0.33862(10) 0.0255(4) Uani 1 1 d . B . O6 O 0.53882(14) 0.60826(12) 0.17543(10) 0.0241(4) Uani 1 1 d . B . O7 O 0.27033(14) 0.40982(11) -0.11144(10) 0.0234(4) Uani 1 1 d . . . O8 O 0.11234(14) 0.25564(12) -0.27117(10) 0.0246(4) Uani 1 1 d . . . Ni1 Ni 0.37223(3) 0.28680(2) 0.26924(2) 0.02425(10) Uani 1 1 d . . . Ni2 Ni 0.71195(3) 0.67800(2) 0.226348(18) 0.02129(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0388(17) 0.0298(16) 0.0428(16) 0.0157(14) 0.0087(13) 0.0069(13) C2 0.056(2) 0.0273(16) 0.0408(16) 0.0159(14) 0.0093(14) 0.0151(14) C3 0.0485(19) 0.0374(18) 0.0451(17) 0.0168(15) 0.0266(15) 0.0191(15) C4 0.0291(14) 0.0283(14) 0.0314(13) 0.0149(12) 0.0138(11) 0.0107(12) C5 0.0209(13) 0.0298(14) 0.0307(13) 0.0168(12) 0.0150(10) 0.0090(11) C6 0.0254(14) 0.0303(15) 0.0304(13) 0.0159(12) 0.0098(10) 0.0112(11) C7 0.0184(12) 0.0303(14) 0.0281(12) 0.0144(11) 0.0106(10) 0.0095(11) C8 0.0208(13) 0.0265(14) 0.0280(12) 0.0154(11) 0.0086(10) 0.0075(10) C13 0.0283(14) 0.0287(14) 0.0289(13) 0.0128(12) 0.0108(11) 0.0144(12) C12 0.0268(14) 0.0370(16) 0.0362(14) 0.0202(13) 0.0115(11) 0.0188(12) C11 0.0213(13) 0.0383(16) 0.0277(13) 0.0167(12) 0.0073(10) 0.0120(12) C10 0.0172(12) 0.0285(14) 0.0284(12) 0.0158(11) 0.0089(10) 0.0073(10) C9 0.0188(12) 0.0259(14) 0.0301(13) 0.0146(11) 0.0080(10) 0.0092(10) C14 0.0176(12) 0.0286(14) 0.0278(12) 0.0154(11) 0.0098(10) 0.0086(10) C15 0.0194(13) 0.0342(15) 0.0324(14) 0.0128(12) 0.0040(10) 0.0117(11) C16 0.0186(13) 0.0343(15) 0.0273(13) 0.0151(12) 0.0065(10) 0.0075(11) C17 0.0223(14) 0.0345(16) 0.0329(14) 0.0096(13) 0.0006(11) 0.0061(12) C21 0.0353(16) 0.0516(19) 0.0242(13) 0.0156(13) 0.0090(11) 0.0163(14) C22 0.0246(14) 0.0372(16) 0.0282(13) 0.0041(12) 0.0078(11) 0.0119(12) C23 0.0368(17) 0.0287(16) 0.0371(15) 0.0075(13) 0.0135(13) 0.0066(13) C24 0.0208(13) 0.0288(14) 0.0211(12) 0.0062(11) 0.0049(10) 0.0071(11) C25 0.0197(12) 0.0251(13) 0.0197(11) 0.0096(10) 0.0074(9) 0.0069(10) C26 0.0176(12) 0.0280(14) 0.0255(12) 0.0047(11) 0.0070(10) 0.0070(11) C27 0.0159(12) 0.0230(13) 0.0219(11) 0.0098(10) 0.0066(9) 0.0054(10) C28 0.0144(11) 0.0240(13) 0.0234(11) 0.0110(10) 0.0056(9) 0.0046(10) C33 0.0212(13) 0.0308(15) 0.0215(12) 0.0076(11) 0.0085(10) 0.0049(11) C32 0.0185(13) 0.0394(16) 0.0315(13) 0.0130(13) 0.0127(10) 0.0082(12) C31 0.0113(11) 0.0338(15) 0.0272(12) 0.0114(12) 0.0053(9) 0.0032(10) C30 0.0154(11) 0.0223(13) 0.0238(11) 0.0101(10) 0.0074(9) 0.0055(10) C29 0.0134(11) 0.0246(13) 0.0256(12) 0.0113(11) 0.0080(9) 0.0069(10) C34 0.0159(12) 0.0247(13) 0.0231(11) 0.0113(10) 0.0059(9) 0.0059(10) C35 0.0155(12) 0.0265(14) 0.0244(12) 0.0093(11) 0.0067(9) 0.0008(10) C36 0.0156(12) 0.0219(13) 0.0250(12) 0.0108(10) 0.0059(9) 0.0031(10) C37 0.0159(12) 0.0280(14) 0.0291(13) 0.0106(11) 0.0047(10) 0.0004(10) C38 0.0175(13) 0.0429(18) 0.0362(15) 0.0166(14) 0.0063(11) -0.0046(12) C39 0.0263(15) 0.0240(15) 0.0531(18) 0.0114(14) 0.0004(13) -0.0005(12) C40 0.0201(13) 0.0476(18) 0.0299(14) 0.0157(13) 0.0044(11) 0.0081(12) C41 0.0282(15) 0.0315(15) 0.0296(13) 0.0108(12) 0.0060(11) 0.0087(12) C42 0.0360(17) 0.0382(17) 0.0317(14) 0.0108(13) 0.0140(12) 0.0138(14) C43 0.0273(15) 0.0369(17) 0.0395(15) 0.0149(14) 0.0141(12) 0.0110(13) C44 0.0270(15) 0.0301(15) 0.0379(15) 0.0092(13) 0.0140(12) 0.0046(12) C45 0.0253(14) 0.0304(15) 0.0327(14) 0.0121(12) 0.0090(11) 0.0076(12) C46 0.043(2) 0.047(2) 0.054(2) 0.0116(17) 0.0317(16) 0.0088(16) C47 0.080(3) 0.062(3) 0.083(3) 0.036(2) 0.060(2) 0.022(2) C48 0.0278(15) 0.0342(16) 0.0508(17) 0.0264(14) 0.0183(13) 0.0143(12) C49 0.0326(16) 0.0401(17) 0.0583(19) 0.0295(16) 0.0242(14) 0.0197(14) C50 0.0287(15) 0.0299(15) 0.0354(14) 0.0137(13) 0.0132(12) 0.0061(12) C51 0.0314(15) 0.0222(14) 0.0266(12) 0.0099(11) 0.0044(11) 0.0049(11) C52 0.0223(13) 0.0257(14) 0.0277(12) 0.0095(11) 0.0039(10) 0.0090(11) C53 0.0459(19) 0.0429(19) 0.059(2) 0.0317(17) 0.0309(16) 0.0147(15) C54 0.080(3) 0.052(2) 0.064(2) 0.028(2) 0.049(2) 0.026(2) C55 0.0179(13) 0.0382(16) 0.0479(16) 0.0254(14) 0.0122(12) 0.0065(12) C56 0.0192(14) 0.052(2) 0.064(2) 0.0370(17) 0.0151(13) 0.0133(13) C57 0.0199(14) 0.0432(18) 0.0480(17) 0.0288(15) 0.0034(12) 0.0033(12) C58 0.0230(14) 0.0367(16) 0.0288(13) 0.0153(12) 0.0055(10) -0.0012(12) C59 0.0201(13) 0.0323(15) 0.0268(12) 0.0118(12) 0.0072(10) 0.0054(11) C62 0.0326(15) 0.0270(15) 0.0294(14) 0.0092(12) 0.0006(11) 0.0027(12) C63 0.0410(17) 0.0380(17) 0.0301(14) 0.0153(13) 0.0049(12) 0.0105(14) C64 0.0252(14) 0.0334(15) 0.0354(14) 0.0175(13) 0.0107(11) 0.0101(12) C65 0.0286(15) 0.0282(15) 0.0332(14) 0.0102(12) 0.0101(11) 0.0046(12) C66 0.0272(14) 0.0306(15) 0.0255(12) 0.0103(12) 0.0095(10) 0.0061(12) C67 0.0378(17) 0.0435(18) 0.0448(17) 0.0267(15) 0.0163(13) 0.0131(14) C68 0.052(2) 0.061(2) 0.0529(19) 0.0374(19) 0.0186(16) 0.0179(18) N1 0.0243(12) 0.0293(12) 0.0311(11) 0.0152(10) 0.0079(9) 0.0103(10) N2 0.0201(11) 0.0229(11) 0.0313(11) 0.0125(10) 0.0069(9) 0.0051(9) N3 0.0158(10) 0.0269(12) 0.0235(10) 0.0093(9) 0.0044(8) 0.0018(9) N4 0.0173(10) 0.0270(12) 0.0262(10) 0.0105(9) 0.0061(8) 0.0059(9) O1 0.0246(10) 0.0253(10) 0.0310(9) 0.0135(8) 0.0085(7) 0.0077(8) O2 0.0218(9) 0.0255(10) 0.0328(9) 0.0128(8) 0.0049(7) 0.0095(8) O3 0.0189(9) 0.0250(10) 0.0315(9) 0.0116(8) 0.0050(7) 0.0083(7) O4 0.0208(9) 0.0285(10) 0.0290(9) 0.0114(8) 0.0055(7) 0.0083(8) O5 0.0166(9) 0.0283(10) 0.0232(8) 0.0075(8) 0.0072(7) 0.0036(7) O6 0.0142(8) 0.0263(9) 0.0226(8) 0.0056(7) 0.0066(6) 0.0048(7) O7 0.0138(8) 0.0258(9) 0.0230(8) 0.0083(7) 0.0062(6) 0.0018(7) O8 0.0154(8) 0.0260(9) 0.0236(8) 0.0081(8) 0.0050(7) 0.0021(7) Ni1 0.01804(17) 0.02463(19) 0.02759(17) 0.01170(15) 0.00583(13) 0.00687(14) Ni2 0.01333(16) 0.02310(18) 0.02078(16) 0.00698(14) 0.00561(12) 0.00304(12) _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 C1 C4 1.530(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.526(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.533(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.548(4) . ? C5 O1 1.265(3) . ? C5 C6 1.395(4) . ? C6 C7 1.400(4) . ? C6 H6 0.9500 . ? C7 O2 1.267(3) . ? C7 C8 1.502(3) . ? C8 C9 1.384(4) . ? C8 C13 1.406(3) . ? C13 C12 1.382(4) . ? C13 H13 0.9500 . ? C12 C11 1.374(4) . ? C12 H12 0.9500 . ? C11 C10 1.403(3) . ? C11 H11 0.9500 . ? C10 C9 1.391(3) . ? C10 C14 1.503(4) . ? C9 H9 0.9500 . ? C14 O3 1.273(3) . ? C14 C15 1.397(3) . ? C15 C16 1.399(4) . ? C15 H15 0.9500 . ? C16 O4 1.268(3) . ? C16 C17 1.540(3) . ? C17 C19A 1.413(12) . ? C17 C20 1.471(6) . ? C17 C19 1.524(6) . ? C17 C20A 1.545(13) . ? C17 C18 1.574(6) . ? C17 C18A 1.667(12) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C18A H18D 0.9800 . ? C18A H18E 0.9800 . ? C18A H18F 0.9800 . ? C19A H19D 0.9800 . ? C19A H19E 0.9800 . ? C19A H19F 0.9800 . ? C20A H20D 0.9800 . ? C20A H20E 0.9800 . ? C20A H20F 0.9800 . ? C21 C24 1.536(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.528(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.532(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.534(3) . ? C25 O5 1.266(3) . ? C25 C26 1.402(3) . ? C26 C27 1.403(3) . ? C26 H26 0.9500 . ? C27 O6 1.258(3) . ? C27 C28 1.504(3) . ? C28 C29 1.382(3) . ? C28 C33 1.399(3) . ? C33 C32 1.384(3) . ? C33 H33 0.9500 . ? C32 C31 1.376(3) . ? C32 H32 0.9500 . ? C31 C30 1.401(3) . ? C31 H31 0.9500 . ? C30 C29 1.397(3) . ? C30 C34 1.501(3) . ? C29 H29 0.9500 . ? C34 O7 1.261(3) . ? C34 C35 1.400(3) . ? C35 C36 1.397(3) . ? C35 H35 0.9500 . ? C36 O8 1.267(3) . ? C36 C37 1.531(3) . ? C37 C39 1.525(4) . ? C37 C40 1.528(3) . ? C37 C38 1.530(4) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 N1 1.332(3) . ? C41 C42 1.389(4) . ? C41 H41 0.9500 . ? C42 C43 1.379(4) . ? C42 H42 0.9500 . ? C43 C44 1.385(4) . ? C43 C46 1.503(4) . ? C44 C45 1.372(4) . ? C44 H44 0.9500 . ? C45 N1 1.341(3) . ? C45 H45 0.9500 . ? C46 C47 1.498(5) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 N2 1.338(3) . ? C48 C49 1.375(4) . ? C48 H48 0.9500 . ? C49 C50 1.388(4) . ? C49 H49 0.9500 . ? C50 C51 1.377(4) . ? C50 C53 1.510(4) . ? C51 C52 1.376(4) . ? C51 H51 0.9500 . ? C52 N2 1.343(3) . ? C52 H52 0.9500 . ? C53 C54 1.500(5) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 N3 1.330(3) . ? C55 C56 1.377(4) . ? C55 H55 0.9500 . ? C56 C57 1.374(4) . ? C56 H56 0.9500 . ? C57 C58 1.379(4) . ? C57 C60A 1.501(10) . ? C57 C60 1.540(10) . ? C58 C59 1.370(4) . ? C58 H58 0.9500 . ? C59 N3 1.343(3) . ? C59 H59 0.9500 . ? C60 C61 1.438(12) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C61A C60A 1.620(12) . ? C61A H61D 0.9800 . ? C61A H61E 0.9800 . ? C61A H61F 0.9800 . ? C60A H60C 0.9900 . ? C60A H60D 0.9900 . ? C62 N4 1.323(3) . ? C62 C63 1.391(4) . ? C62 H62 0.9500 . ? C63 C64 1.380(4) . ? C63 H63 0.9500 . ? C64 C65 1.384(4) . ? C64 C67 1.513(4) . ? C65 C66 1.362(4) . ? C65 H65 0.9500 . ? C66 N4 1.335(3) . ? C66 H66 0.9500 . ? C67 C68 1.491(4) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? N1 Ni1 2.136(2) . ? N2 Ni1 2.106(2) . ? N3 Ni2 2.097(2) . ? N4 Ni2 2.128(2) . ? O1 Ni1 2.0234(18) . ? O2 Ni1 2.0139(17) . ? O3 Ni1 2.0170(18) 2_666 ? O4 Ni1 2.0240(17) 2_666 ? O5 Ni2 2.0163(17) . ? O6 Ni2 2.0127(17) . ? O7 Ni2 2.0173(16) 2_665 ? O8 Ni2 2.0313(16) 2_665 ? Ni1 O3 2.0170(18) 2_666 ? Ni1 O4 2.0240(17) 2_666 ? Ni2 O7 2.0173(16) 2_665 ? Ni2 O8 2.0313(16) 2_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 C1 109.2(2) . . ? C2 C4 C3 108.6(2) . . ? C1 C4 C3 110.0(2) . . ? C2 C4 C5 114.2(2) . . ? C1 C4 C5 108.5(2) . . ? C3 C4 C5 106.3(2) . . ? O1 C5 C6 125.4(2) . . ? O1 C5 C4 114.3(2) . . ? C6 C5 C4 120.2(2) . . ? C5 C6 C7 125.7(2) . . ? C5 C6 H6 117.2 . . ? C7 C6 H6 117.2 . . ? O2 C7 C6 126.1(2) . . ? O2 C7 C8 115.0(2) . . ? C6 C7 C8 118.9(2) . . ? C9 C8 C13 119.2(2) . . ? C9 C8 C7 120.3(2) . . ? C13 C8 C7 120.3(2) . . ? C12 C13 C8 119.3(2) . . ? C12 C13 H13 120.4 . . ? C8 C13 H13 120.4 . . ? C11 C12 C13 121.0(2) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C12 C11 C10 120.8(2) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C9 C10 C11 117.9(2) . . ? C9 C10 C14 119.7(2) . . ? C11 C10 C14 122.3(2) . . ? C8 C9 C10 121.8(2) . . ? C8 C9 H9 119.1 . . ? C10 C9 H9 119.1 . . ? O3 C14 C15 125.5(2) . . ? O3 C14 C10 114.6(2) . . ? C15 C14 C10 119.9(2) . . ? C14 C15 C16 126.1(2) . . ? C14 C15 H15 116.9 . . ? C16 C15 H15 116.9 . . ? O4 C16 C15 125.0(2) . . ? O4 C16 C17 114.7(2) . . ? C15 C16 C17 120.3(2) . . ? C19A C17 C20 134.3(6) . . ? C19A C17 C19 54.0(6) . . ? C20 C17 C19 113.9(4) . . ? C19A C17 C16 115.4(6) . . ? C20 C17 C16 109.4(3) . . ? C19 C17 C16 114.6(3) . . ? C19A C17 C20A 117.4(7) . . ? C19 C17 C20A 131.2(6) . . ? C16 C17 C20A 111.3(5) . . ? C19A C17 C18 50.6(5) . . ? C20 C17 C18 109.6(4) . . ? C19 C17 C18 103.7(3) . . ? C16 C17 C18 105.2(3) . . ? C20A C17 C18 79.0(6) . . ? C19A C17 C18A 106.7(7) . . ? C20 C17 C18A 68.2(5) . . ? C19 C17 C18A 54.3(5) . . ? C16 C17 C18A 105.4(5) . . ? C20A C17 C18A 98.3(7) . . ? C18 C17 C18A 148.0(5) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? C17 C18A H18D 109.5 . . ? C17 C18A H18E 109.5 . . ? H18D C18A H18E 109.5 . . ? C17 C18A H18F 109.5 . . ? H18D C18A H18F 109.5 . . ? H18E C18A H18F 109.5 . . ? C17 C19A H19D 109.5 . . ? C17 C19A H19E 109.5 . . ? H19D C19A H19E 109.5 . . ? C17 C19A H19F 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? C17 C20A H20D 109.5 . . ? C17 C20A H20E 109.5 . . ? H20D C20A H20E 109.5 . . ? C17 C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? C24 C21 H21A 109.5 . . ? C24 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C24 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C22 H22A 109.5 . . ? C24 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C24 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 C23 108.9(2) . . ? C22 C24 C25 114.3(2) . . ? C23 C24 C25 108.5(2) . . ? C22 C24 C21 109.0(2) . . ? C23 C24 C21 109.4(2) . . ? C25 C24 C21 106.5(2) . . ? O5 C25 C26 125.0(2) . . ? O5 C25 C24 114.6(2) . . ? C26 C25 C24 120.3(2) . . ? C25 C26 C27 125.9(2) . . ? C25 C26 H26 117.0 . . ? C27 C26 H26 117.0 . . ? O6 C27 C26 126.0(2) . . ? O6 C27 C28 115.4(2) . . ? C26 C27 C28 118.6(2) . . ? C29 C28 C33 118.6(2) . . ? C29 C28 C27 119.0(2) . . ? C33 C28 C27 122.4(2) . . ? C32 C33 C28 120.1(2) . . ? C32 C33 H33 120.0 . . ? C28 C33 H33 120.0 . . ? C31 C32 C33 120.9(2) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C32 C31 C30 120.3(2) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C29 C30 C31 118.1(2) . . ? C29 C30 C34 118.8(2) . . ? C31 C30 C34 123.1(2) . . ? C28 C29 C30 122.0(2) . . ? C28 C29 H29 119.0 . . ? C30 C29 H29 119.0 . . ? O7 C34 C35 125.5(2) . . ? O7 C34 C30 115.8(2) . . ? C35 C34 C30 118.7(2) . . ? C36 C35 C34 126.0(2) . . ? C36 C35 H35 117.0 . . ? C34 C35 H35 117.0 . . ? O8 C36 C35 125.0(2) . . ? O8 C36 C37 114.7(2) . . ? C35 C36 C37 120.3(2) . . ? C39 C37 C40 109.4(2) . . ? C39 C37 C38 110.4(2) . . ? C40 C37 C38 108.2(2) . . ? C39 C37 C36 107.3(2) . . ? C40 C37 C36 107.2(2) . . ? C38 C37 C36 114.1(2) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N1 C41 C42 122.8(3) . . ? N1 C41 H41 118.6 . . ? C42 C41 H41 118.6 . . ? C43 C42 C41 119.9(3) . . ? C43 C42 H42 120.0 . . ? C41 C42 H42 120.0 . . ? C42 C43 C44 116.8(3) . . ? C42 C43 C46 121.7(3) . . ? C44 C43 C46 121.4(3) . . ? C45 C44 C43 120.3(3) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? N1 C45 C44 122.9(3) . . ? N1 C45 H45 118.5 . . ? C44 C45 H45 118.5 . . ? C47 C46 C43 112.6(3) . . ? C47 C46 H46A 109.1 . . ? C43 C46 H46A 109.1 . . ? C47 C46 H46B 109.1 . . ? C43 C46 H46B 109.1 . . ? H46A C46 H46B 107.8 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N2 C48 C49 123.0(3) . . ? N2 C48 H48 118.5 . . ? C49 C48 H48 118.5 . . ? C48 C49 C50 120.0(3) . . ? C48 C49 H49 120.0 . . ? C50 C49 H49 120.0 . . ? C51 C50 C49 117.1(2) . . ? C51 C50 C53 122.2(3) . . ? C49 C50 C53 120.7(3) . . ? C52 C51 C50 119.8(2) . . ? C52 C51 H51 120.1 . . ? C50 C51 H51 120.1 . . ? N2 C52 C51 123.3(2) . . ? N2 C52 H52 118.4 . . ? C51 C52 H52 118.4 . . ? C54 C53 C50 113.1(3) . . ? C54 C53 H53A 109.0 . . ? C50 C53 H53A 109.0 . . ? C54 C53 H53B 109.0 . . ? C50 C53 H53B 109.0 . . ? H53A C53 H53B 107.8 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N3 C55 C56 123.2(3) . . ? N3 C55 H55 118.4 . . ? C56 C55 H55 118.4 . . ? C57 C56 C55 120.3(3) . . ? C57 C56 H56 119.9 . . ? C55 C56 H56 119.9 . . ? C56 C57 C58 116.8(3) . . ? C56 C57 C60A 125.8(5) . . ? C58 C57 C60A 116.9(4) . . ? C56 C57 C60 120.2(4) . . ? C58 C57 C60 122.8(4) . . ? C59 C58 C57 119.8(3) . . ? C59 C58 H58 120.1 . . ? C57 C58 H58 120.1 . . ? N3 C59 C58 123.6(3) . . ? N3 C59 H59 118.2 . . ? C58 C59 H59 118.2 . . ? C61 C60 C57 117.4(7) . . ? C61 C60 H60A 108.0 . . ? C57 C60 H60A 108.0 . . ? C61 C60 H60B 108.0 . . ? C57 C60 H60B 108.0 . . ? H60A C60 H60B 107.2 . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60A C61A H61D 109.5 . . ? C60A C61A H61E 109.5 . . ? H61D C61A H61E 109.5 . . ? C60A C61A H61F 109.5 . . ? H61D C61A H61F 109.5 . . ? H61E C61A H61F 109.5 . . ? C57 C60A C61A 110.6(6) . . ? C57 C60A H60C 109.5 . . ? C61A C60A H60C 109.5 . . ? C57 C60A H60D 109.5 . . ? C61A C60A H60D 109.5 . . ? H60C C60A H60D 108.1 . . ? N4 C62 C63 123.1(3) . . ? N4 C62 H62 118.4 . . ? C63 C62 H62 118.4 . . ? C64 C63 C62 119.8(2) . . ? C64 C63 H63 120.1 . . ? C62 C63 H63 120.1 . . ? C63 C64 C65 116.3(3) . . ? C63 C64 C67 123.4(2) . . ? C65 C64 C67 120.2(3) . . ? C66 C65 C64 120.3(3) . . ? C66 C65 H65 119.8 . . ? C64 C65 H65 119.8 . . ? N4 C66 C65 123.6(2) . . ? N4 C66 H66 118.2 . . ? C65 C66 H66 118.2 . . ? C68 C67 C64 115.6(3) . . ? C68 C67 H67A 108.4 . . ? C64 C67 H67A 108.4 . . ? C68 C67 H67B 108.4 . . ? C64 C67 H67B 108.4 . . ? H67A C67 H67B 107.4 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C41 N1 C45 117.2(2) . . ? C41 N1 Ni1 124.00(18) . . ? C45 N1 Ni1 118.52(17) . . ? C48 N2 C52 116.8(2) . . ? C48 N2 Ni1 121.38(17) . . ? C52 N2 Ni1 121.77(18) . . ? C55 N3 C59 116.3(2) . . ? C55 N3 Ni2 120.34(17) . . ? C59 N3 Ni2 123.33(17) . . ? C62 N4 C66 116.7(2) . . ? C62 N4 Ni2 124.25(18) . . ? C66 N4 Ni2 118.06(16) . . ? C5 O1 Ni1 125.23(16) . . ? C7 O2 Ni1 125.09(17) . . ? C14 O3 Ni1 123.01(16) . 2_666 ? C16 O4 Ni1 123.85(16) . 2_666 ? C25 O5 Ni2 125.32(15) . . ? C27 O6 Ni2 125.02(15) . . ? C34 O7 Ni2 125.08(15) . 2_665 ? C36 O8 Ni2 125.13(15) . 2_665 ? O2 Ni1 O3 87.08(7) . 2_666 ? O2 Ni1 O1 90.46(7) . . ? O3 Ni1 O1 176.90(7) 2_666 . ? O2 Ni1 O4 176.47(7) . 2_666 ? O3 Ni1 O4 90.17(7) 2_666 2_666 ? O1 Ni1 O4 92.22(7) . 2_666 ? O2 Ni1 N2 94.13(8) . . ? O3 Ni1 N2 92.04(8) 2_666 . ? O1 Ni1 N2 90.01(8) . . ? O4 Ni1 N2 88.18(8) 2_666 . ? O2 Ni1 N1 91.05(8) . . ? O3 Ni1 N1 89.75(8) 2_666 . ? O1 Ni1 N1 88.41(8) . . ? O4 Ni1 N1 86.73(8) 2_666 . ? N2 Ni1 N1 174.60(8) . . ? O6 Ni2 O5 90.96(7) . . ? O6 Ni2 O7 87.18(6) . 2_665 ? O5 Ni2 O7 177.74(7) . 2_665 ? O6 Ni2 O8 176.87(7) . 2_665 ? O5 Ni2 O8 92.13(7) . 2_665 ? O7 Ni2 O8 89.72(7) 2_665 2_665 ? O6 Ni2 N3 91.57(7) . . ? O5 Ni2 N3 89.73(8) . . ? O7 Ni2 N3 91.61(7) 2_665 . ? O8 Ni2 N3 88.98(7) 2_665 . ? O6 Ni2 N4 93.53(7) . . ? O5 Ni2 N4 89.23(8) . . ? O7 Ni2 N4 89.60(7) 2_665 . ? O8 Ni2 N4 85.99(7) 2_665 . ? N3 Ni2 N4 174.82(8) . . ? 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 C2 C4 C5 O1 -165.4(2) . . . . ? C1 C4 C5 O1 -43.3(3) . . . . ? C3 C4 C5 O1 74.9(3) . . . . ? C2 C4 C5 C6 18.4(3) . . . . ? C1 C4 C5 C6 140.5(2) . . . . ? C3 C4 C5 C6 -101.3(3) . . . . ? O1 C5 C6 C7 -1.0(4) . . . . ? C4 C5 C6 C7 174.8(2) . . . . ? C5 C6 C7 O2 3.6(4) . . . . ? C5 C6 C7 C8 -175.2(2) . . . . ? O2 C7 C8 C9 26.8(3) . . . . ? C6 C7 C8 C9 -154.2(2) . . . . ? O2 C7 C8 C13 -149.1(2) . . . . ? C6 C7 C8 C13 29.9(3) . . . . ? C9 C8 C13 C12 0.3(4) . . . . ? C7 C8 C13 C12 176.3(2) . . . . ? C8 C13 C12 C11 0.5(4) . . . . ? C13 C12 C11 C10 -0.8(4) . . . . ? C12 C11 C10 C9 0.4(4) . . . . ? C12 C11 C10 C14 -177.3(2) . . . . ? C13 C8 C9 C10 -0.8(4) . . . . ? C7 C8 C9 C10 -176.8(2) . . . . ? C11 C10 C9 C8 0.5(4) . . . . ? C14 C10 C9 C8 178.2(2) . . . . ? C9 C10 C14 O3 12.3(3) . . . . ? C11 C10 C14 O3 -170.0(2) . . . . ? C9 C10 C14 C15 -166.2(2) . . . . ? C11 C10 C14 C15 11.4(4) . . . . ? O3 C14 C15 C16 1.4(4) . . . . ? C10 C14 C15 C16 179.8(2) . . . . ? C14 C15 C16 O4 -3.7(4) . . . . ? C14 C15 C16 C17 176.1(2) . . . . ? O4 C16 C17 C19A 119.3(7) . . . . ? C15 C16 C17 C19A -60.5(7) . . . . ? O4 C16 C17 C20 -51.4(4) . . . . ? C15 C16 C17 C20 128.8(3) . . . . ? O4 C16 C17 C19 179.4(3) . . . . ? C15 C16 C17 C19 -0.4(4) . . . . ? O4 C16 C17 C20A -17.8(6) . . . . ? C15 C16 C17 C20A 162.4(6) . . . . ? O4 C16 C17 C18 66.2(3) . . . . ? C15 C16 C17 C18 -113.6(3) . . . . ? O4 C16 C17 C18A -123.3(5) . . . . ? C15 C16 C17 C18A 56.9(5) . . . . ? C22 C24 C25 O5 175.9(2) . . . . ? C23 C24 C25 O5 54.1(3) . . . . ? C21 C24 C25 O5 -63.6(3) . . . . ? C22 C24 C25 C26 -5.7(3) . . . . ? C23 C24 C25 C26 -127.4(3) . . . . ? C21 C24 C25 C26 114.8(3) . . . . ? O5 C25 C26 C27 3.4(4) . . . . ? C24 C25 C26 C27 -174.8(2) . . . . ? C25 C26 C27 O6 -5.0(4) . . . . ? C25 C26 C27 C28 175.9(2) . . . . ? O6 C27 C28 C29 -16.9(3) . . . . ? C26 C27 C28 C29 162.3(2) . . . . ? O6 C27 C28 C33 163.8(2) . . . . ? C26 C27 C28 C33 -17.0(4) . . . . ? C29 C28 C33 C32 -1.8(4) . . . . ? C27 C28 C33 C32 177.6(2) . . . . ? C28 C33 C32 C31 0.9(4) . . . . ? C33 C32 C31 C30 0.5(4) . . . . ? C32 C31 C30 C29 -0.9(4) . . . . ? C32 C31 C30 C34 180.0(2) . . . . ? C33 C28 C29 C30 1.4(4) . . . . ? C27 C28 C29 C30 -178.0(2) . . . . ? C31 C30 C29 C28 0.0(4) . . . . ? C34 C30 C29 C28 179.1(2) . . . . ? C29 C30 C34 O7 -15.9(3) . . . . ? C31 C30 C34 O7 163.3(2) . . . . ? C29 C30 C34 C35 164.4(2) . . . . ? C31 C30 C34 C35 -16.5(4) . . . . ? O7 C34 C35 C36 -1.9(4) . . . . ? C30 C34 C35 C36 177.8(2) . . . . ? C34 C35 C36 O8 3.1(4) . . . . ? C34 C35 C36 C37 -175.8(2) . . . . ? O8 C36 C37 C39 58.6(3) . . . . ? C35 C36 C37 C39 -122.4(3) . . . . ? O8 C36 C37 C40 -58.9(3) . . . . ? C35 C36 C37 C40 120.1(2) . . . . ? O8 C36 C37 C38 -178.7(2) . . . . ? C35 C36 C37 C38 0.3(3) . . . . ? N1 C41 C42 C43 1.8(4) . . . . ? C41 C42 C43 C44 -0.2(4) . . . . ? C41 C42 C43 C46 178.4(3) . . . . ? C42 C43 C44 C45 -0.8(4) . . . . ? C46 C43 C44 C45 -179.4(3) . . . . ? C43 C44 C45 N1 0.3(4) . . . . ? C42 C43 C46 C47 -106.1(4) . . . . ? C44 C43 C46 C47 72.4(4) . . . . ? N2 C48 C49 C50 1.1(5) . . . . ? C48 C49 C50 C51 -1.4(4) . . . . ? C48 C49 C50 C53 178.9(3) . . . . ? C49 C50 C51 C52 0.4(4) . . . . ? C53 C50 C51 C52 -179.9(3) . . . . ? C50 C51 C52 N2 1.1(4) . . . . ? C51 C50 C53 C54 -104.3(3) . . . . ? C49 C50 C53 C54 75.4(4) . . . . ? N3 C55 C56 C57 0.3(5) . . . . ? C55 C56 C57 C58 0.5(4) . . . . ? C55 C56 C57 C60A -171.3(5) . . . . ? C55 C56 C57 C60 175.2(5) . . . . ? C56 C57 C58 C59 -1.1(4) . . . . ? C60A C57 C58 C59 171.5(5) . . . . ? C60 C57 C58 C59 -175.6(5) . . . . ? C57 C58 C59 N3 0.9(4) . . . . ? C56 C57 C60 C61 31.8(9) . . . . ? C58 C57 C60 C61 -153.8(6) . . . . ? C60A C57 C60 C61 -88(3) . . . . ? C56 C57 C60A C61A -26.9(9) . . . . ? C58 C57 C60A C61A 161.3(5) . . . . ? C60 C57 C60A C61A 41(3) . . . . ? N4 C62 C63 C64 -0.8(5) . . . . ? C62 C63 C64 C65 -2.3(4) . . . . ? C62 C63 C64 C67 175.0(3) . . . . ? C63 C64 C65 C66 3.2(4) . . . . ? C67 C64 C65 C66 -174.2(3) . . . . ? C64 C65 C66 N4 -1.0(4) . . . . ? C63 C64 C67 C68 23.3(4) . . . . ? C65 C64 C67 C68 -159.4(3) . . . . ? C42 C41 N1 C45 -2.2(4) . . . . ? C42 C41 N1 Ni1 171.7(2) . . . . ? C44 C45 N1 C41 1.2(4) . . . . ? C44 C45 N1 Ni1 -173.0(2) . . . . ? C49 C48 N2 C52 0.3(4) . . . . ? C49 C48 N2 Ni1 -180.0(2) . . . . ? C51 C52 N2 C48 -1.4(4) . . . . ? C51 C52 N2 Ni1 178.84(19) . . . . ? C56 C55 N3 C59 -0.5(4) . . . . ? C56 C55 N3 Ni2 -178.8(2) . . . . ? C58 C59 N3 C55 -0.1(4) . . . . ? C58 C59 N3 Ni2 178.12(19) . . . . ? C63 C62 N4 C66 3.1(4) . . . . ? C63 C62 N4 Ni2 -165.2(2) . . . . ? C65 C66 N4 C62 -2.2(4) . . . . ? C65 C66 N4 Ni2 166.8(2) . . . . ? C6 C5 O1 Ni1 -11.2(4) . . . . ? C4 C5 O1 Ni1 172.85(15) . . . . ? C6 C7 O2 Ni1 6.5(4) . . . . ? C8 C7 O2 Ni1 -174.63(15) . . . . ? C15 C14 O3 Ni1 18.1(3) . . . 2_666 ? C10 C14 O3 Ni1 -160.33(15) . . . 2_666 ? C15 C16 O4 Ni1 -14.1(4) . . . 2_666 ? C17 C16 O4 Ni1 166.11(17) . . . 2_666 ? C26 C25 O5 Ni2 8.4(4) . . . . ? C24 C25 O5 Ni2 -173.31(15) . . . . ? C26 C27 O6 Ni2 -5.6(3) . . . . ? C28 C27 O6 Ni2 173.49(14) . . . . ? C35 C34 O7 Ni2 -13.3(3) . . . 2_665 ? C30 C34 O7 Ni2 166.98(15) . . . 2_665 ? C35 C36 O8 Ni2 11.0(3) . . . 2_665 ? C37 C36 O8 Ni2 -169.99(15) . . . 2_665 ? C7 O2 Ni1 O3 165.3(2) . . . 2_666 ? C7 O2 Ni1 O1 -12.8(2) . . . . ? C7 O2 Ni1 N2 -102.8(2) . . . . ? C7 O2 Ni1 N1 75.6(2) . . . . ? C5 O1 Ni1 O2 15.1(2) . . . . ? C5 O1 Ni1 O4 -162.59(19) . . . 2_666 ? C5 O1 Ni1 N2 109.2(2) . . . . ? C5 O1 Ni1 N1 -75.9(2) . . . . ? C48 N2 Ni1 O2 63.2(2) . . . . ? C52 N2 Ni1 O2 -117.08(19) . . . . ? C48 N2 Ni1 O3 150.4(2) . . . 2_666 ? C52 N2 Ni1 O3 -29.86(19) . . . 2_666 ? C48 N2 Ni1 O1 -27.3(2) . . . . ? C52 N2 Ni1 O1 152.46(19) . . . . ? C48 N2 Ni1 O4 -119.5(2) . . . 2_666 ? C52 N2 Ni1 O4 60.24(19) . . . 2_666 ? C41 N1 Ni1 O2 53.7(2) . . . . ? C45 N1 Ni1 O2 -132.45(19) . . . . ? C41 N1 Ni1 O3 -33.4(2) . . . 2_666 ? C45 N1 Ni1 O3 140.47(19) . . . 2_666 ? C41 N1 Ni1 O1 144.1(2) . . . . ? C45 N1 Ni1 O1 -42.03(19) . . . . ? C41 N1 Ni1 O4 -123.5(2) . . . 2_666 ? C45 N1 Ni1 O4 50.29(19) . . . 2_666 ? C27 O6 Ni2 O5 11.96(19) . . . . ? C27 O6 Ni2 O7 -166.75(19) . . . 2_665 ? C27 O6 Ni2 N3 101.72(19) . . . . ? C27 O6 Ni2 N4 -77.33(19) . . . . ? C25 O5 Ni2 O6 -13.3(2) . . . . ? C25 O5 Ni2 O8 166.13(19) . . . 2_665 ? C25 O5 Ni2 N3 -104.9(2) . . . . ? C25 O5 Ni2 N4 80.2(2) . . . . ? C55 N3 Ni2 O6 135.1(2) . . . . ? C59 N3 Ni2 O6 -43.04(19) . . . . ? C55 N3 Ni2 O5 -133.9(2) . . . . ? C59 N3 Ni2 O5 47.91(19) . . . . ? C55 N3 Ni2 O7 47.9(2) . . . 2_665 ? C59 N3 Ni2 O7 -130.27(19) . . . 2_665 ? C55 N3 Ni2 O8 -41.8(2) . . . 2_665 ? C59 N3 Ni2 O8 140.04(19) . . . 2_665 ? C62 N4 Ni2 O6 -60.9(2) . . . . ? C66 N4 Ni2 O6 130.96(19) . . . . ? C62 N4 Ni2 O5 -151.8(2) . . . . ? C66 N4 Ni2 O5 40.04(19) . . . . ? C62 N4 Ni2 O7 26.2(2) . . . 2_665 ? C66 N4 Ni2 O7 -141.89(19) . . . 2_665 ? C62 N4 Ni2 O8 116.0(2) . . . 2_665 ? C66 N4 Ni2 O8 -52.14(19) . . . 2_665 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.060 _refine_diff_density_min -0.943 _refine_diff_density_rms 0.111 data_lj83sad _database_code_depnum_ccdc_archive 'CCDC 635438' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H24 O8 Zn2, 2(N1 C7 H9)' _chemical_formula_sum 'C42 H42 N2 O8 Zn2' _chemical_formula_weight 833.5624 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn _symmetry_space_group_name_Hall '-P 2ab 2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 15.2960(19) _cell_length_b 16.550(2) _cell_length_c 15.0810(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3817.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11759 _cell_measurement_theta_min 2.461 _cell_measurement_theta_max 28.2805 _exptl_crystal_description Prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 1.313 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.717 _exptl_absorpt_correction_T_max 0.90000 _exptl_absorpt_process_details 'SADABS (sheldrick, 2003)' _exptl_special_details ; The crystal was coated in Exxon Paratone N hydrocarbon oil and mounted on a thin mohair fibre attached to a copper pin. Upon mounting on the diffractometer, the crystal was quenched to 150(K) under a cold nitrogen gas stream supplied by an Oxford Cryosystems Cryostream and data were collected at this temperature. ; _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 Nonius APEX 2' _diffrn_measurement_method /p _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 36201 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0173 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 28.34 _reflns_number_total 4715 _reflns_number_gt 3608 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX (Bruker Nonius, 2004)' _computing_cell_refinement 'SAINT (Bruker Nonius, 2004)' _computing_data_reduction 'SAINT (ibid), XPREP (Siemens, 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 (Farrugia, 2005) WINGX-32 (Farrugia, 2005) ; _computing_publication_material 'enCIFer 1.0 (CCDC, 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+2.4240P] 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 4715 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.1065 _refine_ls_wR_factor_gt 0.0955 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 C1 C 0.21725(15) -0.13518(15) 0.19069(18) 0.0490(6) Uani 1 1 d . . . H1A H 0.1780 -0.0884 0.1897 0.073 Uiso 1 1 calc R . . H1B H 0.1896 -0.1793 0.2237 0.073 Uiso 1 1 calc R . . H1C H 0.2290 -0.1528 0.1298 0.073 Uiso 1 1 calc R . . C2 C 0.30201(13) -0.11214(13) 0.23511(14) 0.0343(4) Uani 1 1 d . . . C3 C 0.32582(13) -0.15233(12) 0.31290(14) 0.0351(4) Uani 1 1 d . . . H3 H 0.2860 -0.1914 0.3353 0.042 Uiso 1 1 calc R . . C4 C 0.40296(13) -0.14016(11) 0.36075(13) 0.0296(4) Uani 1 1 d . . . C5 C 0.41749(13) -0.18984(11) 0.44254(13) 0.0299(4) Uani 1 1 d . . . C6 C 0.45890(12) -0.15475(11) 0.51519(12) 0.0275(4) Uani 1 1 d . . . H6 H 0.4780 -0.1002 0.5115 0.033 Uiso 1 1 calc R . . C7 C 0.47288(13) -0.19795(11) 0.59320(13) 0.0280(4) Uani 1 1 d . . . C8 C 0.44576(14) -0.27861(12) 0.59732(14) 0.0342(4) Uani 1 1 d . . . H8 H 0.4554 -0.3092 0.6498 0.041 Uiso 1 1 calc R . . C9 C 0.40495(15) -0.31397(12) 0.52511(15) 0.0398(5) Uani 1 1 d . . . H9 H 0.3865 -0.3687 0.5285 0.048 Uiso 1 1 calc R . . C10 C 0.39076(14) -0.27071(11) 0.44833(14) 0.0357(5) Uani 1 1 d . . . H10 H 0.3628 -0.2957 0.3992 0.043 Uiso 1 1 calc R . . C11 C 0.51236(12) -0.15545(11) 0.67070(12) 0.0281(4) Uani 1 1 d . . . C12 C 0.54618(14) -0.19938(13) 0.74207(13) 0.0346(5) Uani 1 1 d . . . H12 H 0.5454 -0.2566 0.7377 0.042 Uiso 1 1 calc R . . C13 C 0.58125(13) -0.16548(12) 0.81975(13) 0.0331(4) Uani 1 1 d . . . C14 C 0.61917(15) -0.22104(14) 0.88920(15) 0.0439(5) Uani 1 1 d . . . H14A H 0.6829 -0.2151 0.8903 0.066 Uiso 1 1 calc R . . H14B H 0.6040 -0.2771 0.8749 0.066 Uiso 1 1 calc R . . H14C H 0.5952 -0.2070 0.9474 0.066 Uiso 1 1 calc R . . C15 C 0.62909(16) -0.07377(15) 0.21731(16) 0.0468(6) Uani 1 1 d . . . H15 H 0.6229 -0.0890 0.2777 0.056 Uiso 1 1 calc R . . C16 C 0.70533(16) -0.09398(17) 0.17378(17) 0.0536(7) Uani 1 1 d . . . H16 H 0.7507 -0.1214 0.2046 0.064 Uiso 1 1 calc R . . C17 C 0.71564(15) -0.07441(15) 0.08550(16) 0.0429(5) Uani 1 1 d . . . C18 C 0.64770(16) -0.03279(17) 0.04528(15) 0.0480(6) Uani 1 1 d . . . H18 H 0.6517 -0.0177 -0.0153 0.058 Uiso 1 1 calc R . . C19 C 0.57455(16) -0.01362(15) 0.09376(15) 0.0428(5) Uani 1 1 d . . . H19 H 0.5292 0.0157 0.0653 0.051 Uiso 1 1 calc R . . C20 C 0.79789(18) -0.0967(2) 0.0359(2) 0.0673(8) Uani 1 1 d . . . H20A H 0.8463 -0.1005 0.0792 0.081 Uiso 1 1 calc R . . H20B H 0.7896 -0.1512 0.0100 0.081 Uiso 1 1 calc R . . C21 C 0.8245(2) -0.0429(2) -0.0340(3) 0.0880(12) Uani 1 1 d . . . H21A H 0.8780 -0.0634 -0.0617 0.132 Uiso 1 1 calc R . . H21B H 0.8355 0.0109 -0.0094 0.132 Uiso 1 1 calc R . . H21C H 0.7780 -0.0395 -0.0786 0.132 Uiso 1 1 calc R . . N1 N 0.56384(11) -0.03395(10) 0.17849(11) 0.0316(4) Uani 1 1 d . . . O1 O 0.34605(9) -0.05748(8) 0.19693(9) 0.0348(3) Uani 1 1 d . . . O2 O 0.46150(9) -0.08875(9) 0.34189(9) 0.0346(3) Uani 1 1 d . . . O3 O 0.51251(10) -0.07877(8) 0.66469(9) 0.0320(3) Uani 1 1 d . . . O4 O 0.58531(11) -0.09097(9) 0.83689(10) 0.0385(3) Uani 1 1 d . . . Zn1 Zn 0.451544(15) -0.002020(13) 0.245332(14) 0.02839(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0394(12) 0.0478(13) 0.0597(15) 0.0095(12) -0.0175(11) -0.0115(10) C2 0.0315(11) 0.0317(10) 0.0396(11) -0.0044(9) -0.0039(8) -0.0007(8) C3 0.0327(10) 0.0330(10) 0.0396(11) 0.0032(9) -0.0034(9) -0.0090(8) C4 0.0334(10) 0.0249(9) 0.0303(9) -0.0019(7) 0.0003(8) -0.0040(8) C5 0.0312(10) 0.0260(9) 0.0326(10) 0.0014(8) 0.0016(8) -0.0042(7) C6 0.0299(9) 0.0225(8) 0.0301(9) 0.0011(7) 0.0046(7) -0.0020(7) C7 0.0303(9) 0.0244(9) 0.0295(9) 0.0011(7) 0.0052(8) 0.0006(7) C8 0.0428(12) 0.0260(9) 0.0337(10) 0.0057(8) 0.0038(9) -0.0007(8) C9 0.0501(13) 0.0218(9) 0.0475(12) 0.0023(9) 0.0017(10) -0.0075(9) C10 0.0431(11) 0.0271(10) 0.0369(11) -0.0018(8) -0.0023(9) -0.0093(8) C11 0.0278(9) 0.0287(9) 0.0278(9) 0.0030(7) 0.0054(7) 0.0005(7) C12 0.0403(12) 0.0261(10) 0.0375(11) 0.0062(8) -0.0011(8) 0.0034(8) C13 0.0276(10) 0.0367(10) 0.0350(10) 0.0098(8) 0.0020(8) 0.0019(8) C14 0.0426(12) 0.0426(12) 0.0465(13) 0.0138(10) -0.0062(10) 0.0045(10) C15 0.0453(13) 0.0579(15) 0.0373(12) 0.0155(11) -0.0045(10) 0.0065(11) C16 0.0428(14) 0.0671(17) 0.0508(15) 0.0171(13) -0.0081(11) 0.0150(12) C17 0.0350(11) 0.0501(13) 0.0437(12) 0.0028(10) -0.0011(9) 0.0070(10) C18 0.0434(13) 0.0679(16) 0.0326(11) 0.0036(11) 0.0012(10) 0.0164(12) C19 0.0384(12) 0.0586(14) 0.0312(11) 0.0037(10) -0.0038(9) 0.0139(10) C20 0.0455(15) 0.089(2) 0.0677(19) 0.0066(17) 0.0064(13) 0.0267(14) C21 0.064(2) 0.093(3) 0.108(3) 0.028(2) 0.043(2) 0.0263(19) N1 0.0337(9) 0.0307(8) 0.0303(8) -0.0004(7) -0.0035(7) -0.0023(7) O1 0.0361(7) 0.0329(7) 0.0354(8) 0.0020(6) -0.0066(6) -0.0048(6) O2 0.0377(8) 0.0337(7) 0.0326(7) 0.0078(6) -0.0065(6) -0.0113(6) O3 0.0453(8) 0.0243(6) 0.0262(7) 0.0027(5) -0.0022(6) -0.0013(6) O4 0.0478(9) 0.0334(7) 0.0344(8) 0.0068(6) -0.0087(7) -0.0024(7) Zn1 0.03249(15) 0.02710(14) 0.02558(14) 0.00205(8) -0.00194(8) -0.00387(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 C1 C2 1.508(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 O1 1.266(3) . ? C2 C3 1.397(3) . ? C3 C4 1.398(3) . ? C3 H3 0.9500 . ? C4 O2 1.268(2) . ? C4 C5 1.499(3) . ? C5 C6 1.392(3) . ? C5 C10 1.402(3) . ? C6 C7 1.393(3) . ? C6 H6 0.9500 . ? C7 C8 1.399(3) . ? C7 C11 1.492(3) . ? C8 C9 1.385(3) . ? C8 H8 0.9500 . ? C9 C10 1.379(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 O3 1.272(2) . ? C11 C12 1.398(3) . ? C12 C13 1.405(3) . ? C12 H12 0.9500 . ? C13 O4 1.261(2) . ? C13 C14 1.510(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 N1 1.332(3) . ? C15 C16 1.379(4) . ? C15 H15 0.9500 . ? C16 C17 1.379(3) . ? C16 H16 0.9500 . ? C17 C18 1.386(3) . ? C17 C20 1.510(3) . ? C18 C19 1.374(3) . ? C18 H18 0.9500 . ? C19 N1 1.331(3) . ? C19 H19 0.9500 . ? C20 C21 1.439(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? N1 Zn1 2.0605(17) . ? O1 Zn1 1.9947(14) . ? O2 Zn1 2.0503(14) . ? O3 Zn1 1.9828(13) 5_656 ? O4 Zn1 2.0552(14) 5_656 ? Zn1 O3 1.9828(13) 5_656 ? Zn1 O4 2.0552(14) 5_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 125.68(19) . . ? O1 C2 C1 115.85(19) . . ? C3 C2 C1 118.5(2) . . ? C2 C3 C4 125.81(19) . . ? C2 C3 H3 117.1 . . ? C4 C3 H3 117.1 . . ? O2 C4 C3 125.26(18) . . ? O2 C4 C5 116.62(17) . . ? C3 C4 C5 118.10(17) . . ? C6 C5 C10 118.80(18) . . ? C6 C5 C4 119.09(16) . . ? C10 C5 C4 122.11(17) . . ? C5 C6 C7 121.35(17) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C6 C7 C8 118.79(18) . . ? C6 C7 C11 118.80(16) . . ? C8 C7 C11 122.34(17) . . ? C9 C8 C7 120.12(19) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C10 C9 C8 120.79(18) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C9 C10 C5 120.14(19) . . ? C9 C10 H10 119.9 . . ? C5 C10 H10 119.9 . . ? O3 C11 C12 124.95(18) . . ? O3 C11 C7 114.54(16) . . ? C12 C11 C7 120.51(18) . . ? C11 C12 C13 125.1(2) . . ? C11 C12 H12 117.4 . . ? C13 C12 H12 117.4 . . ? O4 C13 C12 125.44(18) . . ? O4 C13 C14 115.75(19) . . ? C12 C13 C14 118.81(19) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 C16 123.0(2) . . ? N1 C15 H15 118.5 . . ? C16 C15 H15 118.5 . . ? C17 C16 C15 119.9(2) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 117.0(2) . . ? C16 C17 C20 121.1(2) . . ? C18 C17 C20 122.0(2) . . ? C19 C18 C17 119.5(2) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? N1 C19 C18 123.6(2) . . ? N1 C19 H19 118.2 . . ? C18 C19 H19 118.2 . . ? C21 C20 C17 116.6(2) . . ? C21 C20 H20A 108.2 . . ? C17 C20 H20A 108.2 . . ? C21 C20 H20B 108.2 . . ? C17 C20 H20B 108.2 . . ? H20A C20 H20B 107.3 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 N1 C15 117.0(2) . . ? C19 N1 Zn1 120.49(15) . . ? C15 N1 Zn1 122.46(15) . . ? C2 O1 Zn1 126.35(13) . . ? C4 O2 Zn1 125.23(13) . . ? C11 O3 Zn1 128.64(12) . 5_656 ? C13 O4 Zn1 126.51(13) . 5_656 ? O3 Zn1 O1 141.73(6) 5_656 . ? O3 Zn1 O2 88.02(6) 5_656 . ? O1 Zn1 O2 89.88(6) . . ? O3 Zn1 O4 89.08(6) 5_656 5_656 ? O1 Zn1 O4 84.37(6) . 5_656 ? O2 Zn1 O4 166.68(6) . 5_656 ? O3 Zn1 N1 106.05(6) 5_656 . ? O1 Zn1 N1 112.17(6) . . ? O2 Zn1 N1 96.08(6) . . ? O4 Zn1 N1 97.21(7) 5_656 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C2 C3 C4 -1.3(4) . . . . ? C1 C2 C3 C4 178.0(2) . . . . ? C2 C3 C4 O2 2.4(4) . . . . ? C2 C3 C4 C5 -179.4(2) . . . . ? O2 C4 C5 C6 34.7(3) . . . . ? C3 C4 C5 C6 -143.71(19) . . . . ? O2 C4 C5 C10 -145.3(2) . . . . ? C3 C4 C5 C10 36.3(3) . . . . ? C10 C5 C6 C7 -0.9(3) . . . . ? C4 C5 C6 C7 179.10(17) . . . . ? C5 C6 C7 C8 1.1(3) . . . . ? C5 C6 C7 C11 -176.08(17) . . . . ? C6 C7 C8 C9 -0.7(3) . . . . ? C11 C7 C8 C9 176.32(19) . . . . ? C7 C8 C9 C10 0.3(3) . . . . ? C8 C9 C10 C5 -0.1(3) . . . . ? C6 C5 C10 C9 0.5(3) . . . . ? C4 C5 C10 C9 -179.6(2) . . . . ? C6 C7 C11 O3 14.5(3) . . . . ? C8 C7 C11 O3 -162.53(18) . . . . ? C6 C7 C11 C12 -164.97(18) . . . . ? C8 C7 C11 C12 18.0(3) . . . . ? O3 C11 C12 C13 3.5(3) . . . . ? C7 C11 C12 C13 -177.11(19) . . . . ? C11 C12 C13 O4 1.7(3) . . . . ? C11 C12 C13 C14 -177.2(2) . . . . ? N1 C15 C16 C17 -1.4(4) . . . . ? C15 C16 C17 C18 1.5(4) . . . . ? C15 C16 C17 C20 -179.2(3) . . . . ? C16 C17 C18 C19 -0.3(4) . . . . ? C20 C17 C18 C19 -179.6(3) . . . . ? C17 C18 C19 N1 -1.1(4) . . . . ? C16 C17 C20 C21 -148.6(3) . . . . ? C18 C17 C20 C21 30.6(5) . . . . ? C18 C19 N1 C15 1.2(4) . . . . ? C18 C19 N1 Zn1 179.9(2) . . . . ? C16 C15 N1 C19 0.1(4) . . . . ? C16 C15 N1 Zn1 -178.6(2) . . . . ? C3 C2 O1 Zn1 -9.8(3) . . . . ? C1 C2 O1 Zn1 170.92(15) . . . . ? C3 C4 O2 Zn1 7.4(3) . . . . ? C5 C4 O2 Zn1 -170.84(12) . . . . ? C12 C11 O3 Zn1 -6.2(3) . . . 5_656 ? C7 C11 O3 Zn1 174.34(12) . . . 5_656 ? C12 C13 O4 Zn1 -3.5(3) . . . 5_656 ? C14 C13 O4 Zn1 175.42(14) . . . 5_656 ? C2 O1 Zn1 O3 -72.84(19) . . . 5_656 ? C2 O1 Zn1 O2 13.80(17) . . . . ? C2 O1 Zn1 O4 -154.16(18) . . . 5_656 ? C2 O1 Zn1 N1 110.33(17) . . . . ? C4 O2 Zn1 O3 129.11(16) . . . 5_656 ? C4 O2 Zn1 O1 -12.67(16) . . . . ? C4 O2 Zn1 O4 51.6(3) . . . 5_656 ? C4 O2 Zn1 N1 -124.95(16) . . . . ? C19 N1 Zn1 O3 -112.13(17) . . . 5_656 ? C15 N1 Zn1 O3 66.50(18) . . . 5_656 ? C19 N1 Zn1 O1 65.83(18) . . . . ? C15 N1 Zn1 O1 -115.54(18) . . . . ? C19 N1 Zn1 O2 158.19(17) . . . . ? C15 N1 Zn1 O2 -23.19(18) . . . . ? C19 N1 Zn1 O4 -21.01(18) . . . 5_656 ? C15 N1 Zn1 O4 157.62(18) . . . 5_656 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.581 _refine_diff_density_min -0.446 _refine_diff_density_rms 0.063 data_lj129sad _database_code_depnum_ccdc_archive 'CCDC 635439' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H84 Co2 N4 O8' _chemical_formula_sum 'C68 H84 Co2 N4 O8' _chemical_formula_weight 1203.25 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' _symmetry_space_group_name_Hall '-p 1' _Intl_tables_symmetry_no 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2678(13) _cell_length_b 17.4001(19) _cell_length_c 18.1212(19) _cell_angle_alpha 117.271(2) _cell_angle_beta 100.1050(10) _cell_angle_gamma 101.529(2) _cell_volume 3206.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12454 _cell_measurement_theta_min 2.362 _cell_measurement_theta_max 28.22 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1276 _exptl_absorpt_coefficient_mu 0.573 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.816 _exptl_absorpt_correction_T_max 0.944 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; The crystal was coated in Exxon Paratone N hydrocarbon oil and mounted on a thin mohair fibre attached to a copper pin. Upon mounting on the diffractometer, the crystal was quenched to 150(K) under a cold nitrogen gas stream supplied by an Oxford Cryosystems Cryostream and data were collected at this temperature. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 278 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.02 _diffrn_reflns_number 31964 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 28.39 _reflns_number_total 14965 _reflns_number_gt 11681 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1995)' _computing_cell_refinement 'SAINT (Bruker, 1995)' _computing_data_reduction 'SAINT and XPREP (Bruker, 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997), WINGX-32 (Farrugia, 1999)' _computing_publication_material 'enCIFer 1.0 (Allen et al., 2004)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+1.8685P] 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 14965 _refine_ls_number_parameters 750 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1217 _refine_ls_wR_factor_gt 0.1107 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.027 _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 C1 C 0.5194(2) 0.13479(17) 0.55115(14) 0.0378(5) Uani 1 1 d . . . H1A H 0.5067 0.0815 0.4941 0.057 Uiso 1 1 calc R . . H1B H 0.5570 0.1254 0.5973 0.057 Uiso 1 1 calc R . . H1C H 0.5699 0.1892 0.5558 0.057 Uiso 1 1 calc R . . C2 C 0.3472(2) 0.16814(19) 0.49197(15) 0.0412(6) Uani 1 1 d . . . H2A H 0.2703 0.1737 0.4961 0.062 Uiso 1 1 calc R . . H2B H 0.3385 0.1183 0.4338 0.062 Uiso 1 1 calc R . . H2C H 0.3978 0.2254 0.5019 0.062 Uiso 1 1 calc R . . C3 C 0.3212(2) 0.05966(15) 0.54721(16) 0.0407(6) Uani 1 1 d . . . H3A H 0.2450 0.0668 0.5518 0.061 Uiso 1 1 calc R . . H3B H 0.3560 0.0472 0.5919 0.061 Uiso 1 1 calc R . . H3C H 0.3110 0.0087 0.4893 0.061 Uiso 1 1 calc R . . C4 C 0.40193(18) 0.14778(14) 0.56077(12) 0.0270(4) Uani 1 1 d . L . C5 C 0.41006(17) 0.22703(13) 0.64992(12) 0.0238(4) Uani 1 1 d . . . C6 C 0.52001(18) 0.28659(14) 0.71027(13) 0.0292(4) Uani 1 1 d . L . H6 H 0.5869 0.2727 0.6952 0.035 Uiso 1 1 calc R . . C7 C 0.53944(17) 0.36507(13) 0.79116(12) 0.0228(4) Uani 1 1 d . . . C8 C 0.66384(17) 0.42380(13) 0.84545(12) 0.0226(4) Uani 1 1 d . L . C9 C 0.68641(17) 0.48567(13) 0.93384(12) 0.0220(4) Uani 1 1 d . . . H9 H 0.6231 0.4911 0.9573 0.026 Uiso 1 1 calc R L . C10 C 0.80008(17) 0.53981(13) 0.98854(12) 0.0230(4) Uani 1 1 d . L . C11 C 0.89258(17) 0.53069(14) 0.95319(13) 0.0279(4) Uani 1 1 d . . . H11 H 0.9707 0.5661 0.9897 0.033 Uiso 1 1 calc R L . C12 C 0.87092(19) 0.47035(16) 0.86542(14) 0.0335(5) Uani 1 1 d . L . H12 H 0.9342 0.4651 0.8418 0.040 Uiso 1 1 calc R . . C13 C 0.75751(18) 0.41752(15) 0.81162(13) 0.0293(4) Uani 1 1 d . . . H13 H 0.7435 0.3768 0.7513 0.035 Uiso 1 1 calc R L . C14 C 0.81818(17) 0.60430(13) 1.08348(12) 0.0224(4) Uani 1 1 d . . . C15 C 0.92553(17) 0.67432(14) 1.13350(13) 0.0266(4) Uani 1 1 d . L . H15 H 0.9816 0.6791 1.1044 0.032 Uiso 1 1 calc R . . C16 C 0.95678(17) 0.73785(13) 1.22293(13) 0.0241(4) Uani 1 1 d . . . C17 C 1.08053(18) 0.80810(14) 1.27100(14) 0.0296(4) Uani 1 1 d . L . C18 C 1.0658(2) 0.90271(16) 1.30968(19) 0.0480(7) Uani 1 1 d . . . H18A H 1.0168 0.9084 1.3480 0.072 Uiso 1 1 calc R L . H18B H 1.0285 0.9108 1.2624 0.072 Uiso 1 1 calc R . . H18C H 1.1426 0.9496 1.3434 0.072 Uiso 1 1 calc R . . C19 C 1.1611(2) 0.79856(18) 1.21391(16) 0.0409(6) Uani 1 1 d . . . H19A H 1.2382 0.8445 1.2493 0.061 Uiso 1 1 calc R L . H19B H 1.1277 0.8076 1.1664 0.061 Uiso 1 1 calc R . . H19C H 1.1689 0.7374 1.1895 0.061 Uiso 1 1 calc R . . C20 C 1.1360(2) 0.79407(18) 1.34453(15) 0.0387(5) Uani 1 1 d . . . H20A H 1.1467 0.7339 1.3194 0.058 Uiso 1 1 calc R L . H20B H 1.0847 0.7979 1.3810 0.058 Uiso 1 1 calc R . . H20C H 1.2120 0.8415 1.3802 0.058 Uiso 1 1 calc R . . C21 C 0.4972(2) 0.01310(17) 0.15505(17) 0.0429(6) Uani 1 1 d . . . H21A H 0.4881 -0.0521 0.1219 0.064 Uiso 1 1 calc R . . H21B H 0.5800 0.0481 0.1867 0.064 Uiso 1 1 calc R . . H21C H 0.4680 0.0328 0.1149 0.064 Uiso 1 1 calc R . . C22 C 0.2974(2) -0.02219(15) 0.17130(16) 0.0400(5) Uani 1 1 d . . . H22A H 0.2689 0.0012 0.1344 0.060 Uiso 1 1 calc R . . H22B H 0.2537 -0.0136 0.2133 0.060 Uiso 1 1 calc R . . H22C H 0.2862 -0.0873 0.1348 0.060 Uiso 1 1 calc R . . C23 C 0.4702(3) -0.00569(16) 0.27939(16) 0.0421(6) Uani 1 1 d . . . H23A H 0.4313 0.0094 0.3247 0.063 Uiso 1 1 calc R . . H23B H 0.5549 0.0230 0.3067 0.063 Uiso 1 1 calc R . . H23C H 0.4517 -0.0721 0.2446 0.063 Uiso 1 1 calc R . . C24 C 0.4275(2) 0.02957(14) 0.22037(14) 0.0294(4) Uani 1 1 d . N . C25 C 0.44487(18) 0.13297(14) 0.26898(13) 0.0255(4) Uani 1 1 d . . . C26 C 0.52289(19) 0.19056(14) 0.35313(14) 0.0288(4) Uani 1 1 d . M . H26 H 0.5588 0.1628 0.3805 0.035 Uiso 1 1 calc R . . C27 C 0.55291(18) 0.28654(14) 0.40089(13) 0.0255(4) Uani 1 1 d . . . C28 C 0.64747(18) 0.33861(14) 0.48731(13) 0.0252(4) Uani 1 1 d . M . C29 C 0.64883(18) 0.42436(14) 0.55069(13) 0.0252(4) Uani 1 1 d . . . H29 H 0.5877 0.4473 0.5395 0.030 Uiso 1 1 calc R M . C30 C 0.73818(17) 0.47675(14) 0.62992(13) 0.0248(4) Uani 1 1 d . . . C31 C 0.82802(19) 0.44215(15) 0.64462(14) 0.0294(4) Uani 1 1 d . . . H31 H 0.8896 0.4768 0.6983 0.035 Uiso 1 1 calc R M . C32 C 0.8279(2) 0.35811(16) 0.58183(14) 0.0327(5) Uani 1 1 d . M . H32 H 0.8900 0.3358 0.5924 0.039 Uiso 1 1 calc R . . C33 C 0.73857(19) 0.30629(15) 0.50383(14) 0.0302(4) Uani 1 1 d . . . H33 H 0.7392 0.2484 0.4613 0.036 Uiso 1 1 calc R M . C34 C 0.73716(18) 0.56952(14) 0.69545(13) 0.0249(4) Uani 1 1 d . . . C35 C 0.83823(19) 0.63063(15) 0.76549(14) 0.0315(5) Uani 1 1 d . . . H35 H 0.9047 0.6108 0.7687 0.038 Uiso 1 1 calc R . . C36 C 0.84964(18) 0.71911(15) 0.83162(13) 0.0285(4) Uani 1 1 d . . . C37 C 0.9644(2) 0.77643(16) 0.90794(15) 0.0386(5) Uani 1 1 d . A . C38 C 1.0552(6) 0.7276(4) 0.9086(4) 0.0591(6) Uiso 0.50 1 d P A 1 H38A H 1.1227 0.7680 0.9609 0.089 Uiso 0.50 1 calc PR A 1 H38B H 1.0804 0.7117 0.8565 0.089 Uiso 0.50 1 calc PR A 1 H38C H 1.0205 0.6719 0.9088 0.089 Uiso 0.50 1 calc PR A 1 C39 C 0.9276(6) 0.7889(5) 0.9924(4) 0.0591(6) Uiso 0.50 1 d P A 1 H39A H 0.8897 0.7288 0.9835 0.089 Uiso 0.50 1 calc PR A 1 H39B H 0.8731 0.8242 1.0017 0.089 Uiso 0.50 1 calc PR A 1 H39C H 0.9974 0.8213 1.0436 0.089 Uiso 0.50 1 calc PR A 1 C40 C 1.0095(6) 0.8650(4) 0.9162(4) 0.0591(6) Uiso 0.50 1 d P A 1 H40A H 1.0787 0.9029 0.9677 0.089 Uiso 0.50 1 calc PR A 1 H40B H 0.9494 0.8950 0.9225 0.089 Uiso 0.50 1 calc PR A 1 H40C H 1.0308 0.8565 0.8640 0.089 Uiso 0.50 1 calc PR A 1 C38A C 1.0697(6) 0.7821(5) 0.8648(4) 0.0591(6) Uiso 0.50 1 d P A 2 H38D H 1.1440 0.8213 0.9112 0.089 Uiso 0.50 1 calc PR A 2 H38E H 1.0541 0.8077 0.8274 0.089 Uiso 0.50 1 calc PR A 2 H38F H 1.0743 0.7208 0.8298 0.089 Uiso 0.50 1 calc PR A 2 C39A C 0.9902(6) 0.7378(5) 0.9596(4) 0.0591(6) Uiso 0.50 1 d P A 2 H39D H 1.0626 0.7787 1.0076 0.089 Uiso 0.50 1 calc PR A 2 H39E H 1.0000 0.6787 0.9237 0.089 Uiso 0.50 1 calc PR A 2 H39F H 0.9260 0.7293 0.9834 0.089 Uiso 0.50 1 calc PR A 2 C40A C 0.9750(6) 0.8784(4) 0.9548(4) 0.0591(6) Uiso 0.50 1 d P A 2 H40D H 0.9182 0.8883 0.9872 0.089 Uiso 0.50 1 calc PR A 2 H40E H 0.9594 0.8970 0.9116 0.089 Uiso 0.50 1 calc PR A 2 H40F H 1.0541 0.9145 0.9953 0.089 Uiso 0.50 1 calc PR A 2 C41 C 0.1687(2) 0.44158(17) 0.72984(17) 0.0379(5) Uani 1 1 d . . . H41 H 0.1186 0.4256 0.7585 0.046 Uiso 1 1 calc R B 3 C42 C 0.1474(2) 0.4995(2) 0.7009(2) 0.0504(7) Uani 1 1 d . K . H42 H 0.0836 0.5222 0.7096 0.060 Uiso 1 1 calc R . . C43 C 0.2192(2) 0.52463(18) 0.65900(18) 0.0431(6) Uani 1 1 d . . . C44 C 0.3106(2) 0.48979(16) 0.64928(14) 0.0354(5) Uani 1 1 d . K . H44 H 0.3630 0.5058 0.6219 0.042 Uiso 1 1 calc R . . C45 C 0.32573(19) 0.43172(15) 0.67941(13) 0.0312(5) Uani 1 1 d . . . H45 H 0.3888 0.4080 0.6713 0.037 Uiso 1 1 calc R C 3 C46 C 0.2008(6) 0.5972(5) 0.6365(4) 0.0524(8) Uiso 0.50 1 d PD F . H46A H 0.2627 0.6554 0.6810 0.063 Uiso 0.50 1 calc PR D 1 H46B H 0.2164 0.5800 0.5802 0.063 Uiso 0.50 1 calc PR D 1 C46A C 0.1966(6) 0.5742(5) 0.6106(4) 0.0524(8) Uiso 0.50 1 d P G . H46C H 0.2537 0.6366 0.6456 0.063 Uiso 0.50 1 calc PR E 3 H46D H 0.2148 0.5431 0.5552 0.063 Uiso 0.50 1 calc PR E 3 C47 C 0.0977(6) 0.6159(5) 0.6299(4) 0.0524(8) Uiso 0.50 1 d P F 1 H47A H 0.0334 0.5593 0.5883 0.079 Uiso 0.50 1 calc PR F 1 H47B H 0.1008 0.6594 0.6096 0.079 Uiso 0.50 1 calc PR F 1 H47C H 0.0850 0.6422 0.6871 0.079 Uiso 0.50 1 calc PR F 1 C47B C 0.1370(9) 0.6516(7) 0.6702(7) 0.0524(8) Uiso 0.30 1 d P F 2 H47D H 0.0549 0.6144 0.6501 0.079 Uiso 0.30 1 calc PR F 2 H47E H 0.1436 0.6961 0.6510 0.079 Uiso 0.30 1 calc PR F 2 H47F H 0.1660 0.6838 0.7340 0.079 Uiso 0.30 1 calc PR F 2 C47A C 0.0831(9) 0.5827(7) 0.5898(6) 0.0524(8) Uiso 0.20 1 d PD G 3 H47G H 0.0891 0.6331 0.5784 0.079 Uiso 0.20 1 calc PR G 3 H47H H 0.0521 0.5952 0.6390 0.079 Uiso 0.20 1 calc PR G 3 H47I H 0.0306 0.5258 0.5378 0.079 Uiso 0.20 1 calc PR G 3 C48 C 0.3311(2) 0.25227(16) 0.90454(15) 0.0389(5) Uani 1 1 d . H 3 H48 H 0.3666 0.3154 0.9468 0.047 Uiso 1 1 calc R H 3 C49 C 0.3151(2) 0.19104(17) 0.93356(15) 0.0431(6) Uani 1 1 d . H 3 H49 H 0.3397 0.2124 0.9942 0.052 Uiso 1 1 calc R H 3 C50 C 0.2630(2) 0.09852(15) 0.87383(15) 0.0330(5) Uani 1 1 d . H 3 C51 C 0.2341(2) 0.07333(15) 0.78705(15) 0.0348(5) Uani 1 1 d . H 3 H51 H 0.2009 0.0106 0.7433 0.042 Uiso 1 1 calc R H 3 C52 C 0.2528(2) 0.13814(15) 0.76350(14) 0.0331(5) Uani 1 1 d . H 3 H52 H 0.2314 0.1184 0.7031 0.040 Uiso 1 1 calc R H 3 C53 C 0.2340(2) 0.02792(17) 0.90008(16) 0.0410(6) Uani 1 1 d . H 3 H53A H 0.1514 0.0161 0.8996 0.049 Uiso 1 1 calc R H 3 H53B H 0.2407 -0.0297 0.8554 0.049 Uiso 1 1 calc R H 3 C54 C 0.3085(3) 0.0525(2) 0.98774(19) 0.0533(7) Uani 1 1 d . H 3 H54A H 0.3910 0.0680 0.9906 0.080 Uiso 1 1 calc R H 3 H54B H 0.2877 0.0005 0.9964 0.080 Uiso 1 1 calc R H 3 H54C H 0.2954 0.1051 1.0334 0.080 Uiso 1 1 calc R H 3 C55 C 0.2392(2) 0.31238(16) 0.40806(14) 0.0348(5) Uani 1 1 d . I 3 H55 H 0.2958 0.3715 0.4409 0.042 Uiso 1 1 calc R I 3 C56 C 0.1513(2) 0.29275(16) 0.44133(15) 0.0380(5) Uani 1 1 d . I 3 H56 H 0.1480 0.3382 0.4954 0.046 Uiso 1 1 calc R I 3 C57 C 0.0680(2) 0.20713(17) 0.39625(16) 0.0379(5) Uani 1 1 d . I 3 C58 C 0.0784(2) 0.14436(16) 0.31741(15) 0.0371(5) Uani 1 1 d . I 3 H58 H 0.0239 0.0844 0.2839 0.044 Uiso 1 1 calc R I 3 C59 C 0.1674(2) 0.16923(15) 0.28819(14) 0.0326(5) Uani 1 1 d . I 3 H59 H 0.1721 0.1252 0.2340 0.039 Uiso 1 1 calc R I 3 C60 C -0.0278(3) 0.1816(2) 0.4308(2) 0.0561(8) Uani 1 1 d . I 3 H60A H -0.0317 0.2378 0.4795 0.067 Uiso 1 1 calc R I 3 H60B H -0.1036 0.1524 0.3842 0.067 Uiso 1 1 calc R I 3 C61 C -0.0094(4) 0.1175(2) 0.4625(3) 0.0784(11) Uani 1 1 d . I 3 H61A H 0.0005 0.0637 0.4159 0.118 Uiso 1 1 calc R I 3 H61B H -0.0774 0.0984 0.4789 0.118 Uiso 1 1 calc R I 3 H61C H 0.0607 0.1486 0.5134 0.118 Uiso 1 1 calc R I 3 C62 C 0.47341(19) 0.37065(14) 0.16796(13) 0.0293(4) Uani 1 1 d . J 3 H62 H 0.4185 0.4023 0.1824 0.035 Uiso 1 1 calc R J 3 C63 C 0.5420(2) 0.38927(14) 0.12149(14) 0.0314(5) Uani 1 1 d . J 3 H63 H 0.5348 0.4335 0.1056 0.038 Uiso 1 1 calc R J 3 C64 C 0.6212(2) 0.34302(15) 0.09831(15) 0.0356(5) Uani 1 1 d . J 3 C65 C 0.6267(2) 0.27910(17) 0.12354(18) 0.0433(6) Uani 1 1 d . J 3 H65 H 0.6790 0.2450 0.1083 0.052 Uiso 1 1 calc R J 3 C66 C 0.5565(2) 0.26541(16) 0.17043(16) 0.0360(5) Uani 1 1 d . J 3 H66 H 0.5622 0.2217 0.1873 0.043 Uiso 1 1 calc R J 3 C67 C 0.6989(3) 0.36064(19) 0.04765(19) 0.0498(7) Uani 1 1 d . J 3 H67A H 0.7001 0.4193 0.0512 0.060 Uiso 1 1 calc R J 3 H67B H 0.7796 0.3666 0.0752 0.060 Uiso 1 1 calc R J 3 C68 C 0.6595(4) 0.2865(2) -0.0467(2) 0.0713(10) Uani 1 1 d . J 3 H68A H 0.6545 0.2277 -0.0508 0.107 Uiso 1 1 calc R J 3 H68B H 0.7158 0.2994 -0.0751 0.107 Uiso 1 1 calc R J 3 H68C H 0.5825 0.2841 -0.0758 0.107 Uiso 1 1 calc R J 3 N1 N 0.25631(15) 0.40689(12) 0.71959(11) 0.0271(4) Uani 1 1 d . K 3 N2 N 0.29948(15) 0.22766(12) 0.82089(11) 0.0294(4) Uani 1 1 d . H 3 N3 N 0.24827(16) 0.25228(12) 0.33195(11) 0.0299(4) Uani 1 1 d . I 3 N4 N 0.48028(15) 0.31037(11) 0.19366(11) 0.0275(4) Uani 1 1 d . J 3 O1 O 0.31305(12) 0.23417(9) 0.66139(9) 0.0273(3) Uani 1 1 d . L 3 O2 O 0.46116(12) 0.39112(9) 0.82312(9) 0.0257(3) Uani 1 1 d . L 3 O3 O 0.73301(12) 0.58971(9) 1.11131(8) 0.0244(3) Uani 1 1 d . . 3 O4 O 0.89070(12) 0.74222(9) 1.27000(9) 0.0265(3) Uani 1 1 d . . 3 O7 O 0.64178(12) 0.58609(9) 0.68039(9) 0.0277(3) Uani 1 1 d . . 3 O6 O 0.50916(13) 0.33422(10) 0.37686(9) 0.0286(3) Uani 1 1 d . M 3 O8 O 0.77109(13) 0.75646(10) 0.83464(9) 0.0296(3) Uani 1 1 d . . 3 O5 O 0.38862(13) 0.15949(9) 0.22468(9) 0.0282(3) Uani 1 1 d . N 3 Co1 Co 0.28612(2) 0.321874(18) 0.773014(16) 0.02293(7) Uani 1 1 d . . 3 Co2 Co 0.37187(2) 0.286040(18) 0.268296(17) 0.02518(8) Uani 1 1 d . . 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0309(12) 0.0377(12) 0.0268(11) 0.0015(9) 0.0091(9) 0.0131(10) C2 0.0436(14) 0.0539(15) 0.0250(11) 0.0167(11) 0.0123(10) 0.0207(12) C3 0.0421(14) 0.0259(11) 0.0352(12) 0.0040(10) 0.0105(10) 0.0040(10) C4 0.0259(10) 0.0248(10) 0.0194(9) 0.0037(8) 0.0050(8) 0.0074(8) C5 0.0256(10) 0.0222(9) 0.0205(9) 0.0082(8) 0.0082(8) 0.0075(8) C6 0.0233(10) 0.0271(10) 0.0236(10) 0.0034(8) 0.0066(8) 0.0063(8) C7 0.0216(9) 0.0222(9) 0.0206(9) 0.0086(8) 0.0068(7) 0.0046(8) C8 0.0213(9) 0.0209(9) 0.0213(9) 0.0081(8) 0.0061(7) 0.0049(7) C9 0.0201(9) 0.0209(9) 0.0222(9) 0.0086(8) 0.0077(7) 0.0057(7) C10 0.0226(9) 0.0213(9) 0.0225(9) 0.0093(8) 0.0077(8) 0.0061(8) C11 0.0174(9) 0.0313(11) 0.0263(10) 0.0101(9) 0.0057(8) 0.0036(8) C12 0.0231(10) 0.0398(12) 0.0289(11) 0.0099(9) 0.0135(9) 0.0077(9) C13 0.0272(11) 0.0299(11) 0.0220(10) 0.0067(8) 0.0099(8) 0.0064(9) C14 0.0207(9) 0.0223(9) 0.0196(9) 0.0083(8) 0.0051(7) 0.0054(7) C15 0.0206(10) 0.0279(10) 0.0235(10) 0.0096(8) 0.0068(8) 0.0010(8) C16 0.0196(9) 0.0218(9) 0.0249(9) 0.0102(8) 0.0039(8) 0.0019(7) C17 0.0219(10) 0.0263(10) 0.0280(10) 0.0089(9) 0.0031(8) -0.0004(8) C18 0.0349(13) 0.0246(12) 0.0626(17) 0.0134(12) 0.0015(12) 0.0006(10) C19 0.0252(11) 0.0447(14) 0.0396(13) 0.0188(11) 0.0075(10) -0.0056(10) C20 0.0268(11) 0.0465(14) 0.0328(12) 0.0156(11) 0.0040(9) 0.0083(10) C21 0.0551(16) 0.0344(13) 0.0444(14) 0.0172(11) 0.0282(12) 0.0211(12) C22 0.0430(14) 0.0246(11) 0.0426(13) 0.0130(10) 0.0100(11) 0.0049(10) C23 0.0599(16) 0.0272(11) 0.0379(13) 0.0158(10) 0.0110(12) 0.0167(11) C24 0.0370(12) 0.0236(10) 0.0288(10) 0.0124(9) 0.0135(9) 0.0112(9) C25 0.0265(10) 0.0244(10) 0.0289(10) 0.0138(8) 0.0144(8) 0.0086(8) C26 0.0323(11) 0.0260(10) 0.0297(10) 0.0142(9) 0.0102(9) 0.0120(9) C27 0.0252(10) 0.0263(10) 0.0258(10) 0.0125(8) 0.0115(8) 0.0087(8) C28 0.0249(10) 0.0254(10) 0.0251(10) 0.0127(8) 0.0083(8) 0.0080(8) C29 0.0240(10) 0.0247(10) 0.0281(10) 0.0135(8) 0.0083(8) 0.0096(8) C30 0.0240(10) 0.0245(10) 0.0257(10) 0.0120(8) 0.0096(8) 0.0078(8) C31 0.0270(11) 0.0323(11) 0.0271(10) 0.0139(9) 0.0064(8) 0.0111(9) C32 0.0308(11) 0.0361(12) 0.0346(11) 0.0179(10) 0.0099(9) 0.0178(10) C33 0.0334(11) 0.0273(10) 0.0301(11) 0.0120(9) 0.0121(9) 0.0149(9) C34 0.0244(10) 0.0245(10) 0.0251(10) 0.0120(8) 0.0085(8) 0.0073(8) C35 0.0245(10) 0.0318(11) 0.0304(11) 0.0102(9) 0.0042(9) 0.0115(9) C36 0.0238(10) 0.0305(11) 0.0269(10) 0.0130(9) 0.0054(8) 0.0062(9) C37 0.0292(12) 0.0326(12) 0.0343(12) 0.0074(10) -0.0025(9) 0.0066(10) C41 0.0249(11) 0.0437(13) 0.0541(15) 0.0311(12) 0.0161(10) 0.0096(10) C42 0.0277(12) 0.0620(17) 0.084(2) 0.0526(17) 0.0207(13) 0.0173(12) C43 0.0280(12) 0.0489(15) 0.0535(15) 0.0344(13) 0.0038(11) 0.0011(11) C44 0.0298(11) 0.0390(12) 0.0288(11) 0.0168(10) 0.0053(9) -0.0016(10) C45 0.0270(11) 0.0319(11) 0.0257(10) 0.0101(9) 0.0076(8) 0.0037(9) C48 0.0447(14) 0.0266(11) 0.0299(11) 0.0085(9) -0.0010(10) 0.0072(10) C49 0.0576(16) 0.0360(13) 0.0262(11) 0.0130(10) 0.0022(11) 0.0130(12) C50 0.0303(11) 0.0334(12) 0.0364(12) 0.0181(10) 0.0114(9) 0.0107(9) C51 0.0369(12) 0.0259(11) 0.0320(11) 0.0091(9) 0.0115(10) 0.0053(9) C52 0.0366(12) 0.0285(11) 0.0270(10) 0.0093(9) 0.0105(9) 0.0078(9) C53 0.0471(14) 0.0391(13) 0.0414(13) 0.0228(11) 0.0172(11) 0.0138(11) C54 0.0592(18) 0.0583(18) 0.0498(16) 0.0349(14) 0.0164(14) 0.0151(14) C55 0.0361(12) 0.0287(11) 0.0296(11) 0.0102(9) 0.0057(9) 0.0063(9) C56 0.0420(13) 0.0326(12) 0.0305(11) 0.0079(10) 0.0134(10) 0.0134(10) C57 0.0327(12) 0.0376(12) 0.0387(12) 0.0136(10) 0.0151(10) 0.0135(10) C58 0.0322(12) 0.0311(12) 0.0367(12) 0.0098(10) 0.0115(10) 0.0062(10) C59 0.0353(12) 0.0271(11) 0.0283(11) 0.0086(9) 0.0108(9) 0.0092(9) C60 0.0477(16) 0.0458(16) 0.0565(17) 0.0090(13) 0.0315(14) 0.0090(13) C61 0.101(3) 0.062(2) 0.089(3) 0.037(2) 0.071(2) 0.026(2) C62 0.0302(11) 0.0239(10) 0.0268(10) 0.0087(8) 0.0054(8) 0.0092(8) C63 0.0382(12) 0.0218(10) 0.0277(10) 0.0103(8) 0.0060(9) 0.0063(9) C64 0.0370(12) 0.0287(11) 0.0390(12) 0.0160(10) 0.0150(10) 0.0069(10) C65 0.0417(14) 0.0395(13) 0.0649(17) 0.0319(13) 0.0295(13) 0.0205(11) C66 0.0343(12) 0.0321(12) 0.0524(14) 0.0269(11) 0.0187(11) 0.0139(10) C67 0.0564(17) 0.0466(15) 0.0657(18) 0.0359(14) 0.0372(15) 0.0200(13) C68 0.109(3) 0.0531(18) 0.073(2) 0.0339(17) 0.063(2) 0.0318(19) N1 0.0224(8) 0.0257(9) 0.0248(8) 0.0095(7) 0.0050(7) 0.0016(7) N2 0.0251(9) 0.0265(9) 0.0282(9) 0.0093(7) 0.0063(7) 0.0056(7) N3 0.0311(10) 0.0281(9) 0.0279(9) 0.0131(8) 0.0072(7) 0.0091(8) N4 0.0254(9) 0.0225(8) 0.0287(9) 0.0105(7) 0.0059(7) 0.0047(7) O1 0.0227(7) 0.0251(7) 0.0225(7) 0.0047(6) 0.0073(6) 0.0035(6) O2 0.0203(7) 0.0236(7) 0.0225(7) 0.0044(6) 0.0070(5) 0.0038(6) O3 0.0194(7) 0.0225(7) 0.0216(7) 0.0055(6) 0.0071(5) 0.0016(5) O4 0.0219(7) 0.0252(7) 0.0222(7) 0.0071(6) 0.0054(6) 0.0014(6) O7 0.0241(7) 0.0238(7) 0.0305(7) 0.0107(6) 0.0055(6) 0.0087(6) O6 0.0284(8) 0.0237(7) 0.0295(7) 0.0111(6) 0.0052(6) 0.0093(6) O8 0.0264(7) 0.0268(7) 0.0281(7) 0.0098(6) 0.0052(6) 0.0074(6) O5 0.0302(8) 0.0235(7) 0.0273(7) 0.0109(6) 0.0075(6) 0.0079(6) Co1 0.01890(13) 0.02092(14) 0.02021(13) 0.00514(11) 0.00623(10) 0.00254(10) Co2 0.02452(15) 0.02120(14) 0.02548(14) 0.00940(11) 0.00534(11) 0.00720(11) _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 C1 C4 1.530(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.528(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.535(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.539(3) . ? C5 O1 1.264(2) . ? C5 C6 1.405(3) . ? C6 C7 1.408(3) . ? C6 H6 0.9500 . ? C7 O2 1.262(2) . ? C7 C8 1.507(3) . ? C8 C13 1.394(3) . ? C8 C9 1.395(3) . ? C9 C10 1.396(3) . ? C9 H9 0.9500 . ? C10 C11 1.399(3) . ? C10 C14 1.505(3) . ? C11 C12 1.383(3) . ? C11 H11 0.9500 . ? C12 C13 1.387(3) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 O3 1.268(2) . ? C14 C15 1.403(3) . ? C15 C16 1.402(3) . ? C15 H15 0.9500 . ? C16 O4 1.264(2) . ? C16 C17 1.541(3) . ? C17 C18 1.530(3) . ? C17 C19 1.530(3) . ? C17 C20 1.531(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C24 1.535(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.531(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.526(3) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.545(3) . ? C25 O5 1.267(2) . ? C25 C26 1.396(3) . ? C26 C27 1.411(3) . ? C26 H26 0.9500 . ? C27 O6 1.262(2) . ? C27 C28 1.504(3) . ? C28 C33 1.394(3) . ? C28 C29 1.399(3) . ? C29 C30 1.394(3) . ? C29 H29 0.9500 . ? C30 C31 1.399(3) . ? C30 C34 1.507(3) . ? C31 C32 1.381(3) . ? C31 H31 0.9500 . ? C32 C33 1.381(3) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 O7 1.273(2) . ? C34 C35 1.401(3) . ? C35 C36 1.411(3) . ? C35 H35 0.9500 . ? C36 O8 1.261(3) . ? C36 C37 1.543(3) . ? C37 C39A 1.409(7) . ? C37 C40 1.456(7) . ? C37 C38 1.532(7) . ? C37 C40A 1.540(7) . ? C37 C39 1.603(7) . ? C37 C38A 1.633(7) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C38A H38D 0.9800 . ? C38A H38E 0.9800 . ? C38A H38F 0.9800 . ? C39A H39D 0.9800 . ? C39A H39E 0.9800 . ? C39A H39F 0.9800 . ? C40A H40D 0.9800 . ? C40A H40E 0.9800 . ? C40A H40F 0.9800 . ? C41 N1 1.334(3) . ? C41 C42 1.379(3) . ? C41 H41 0.9500 . ? C42 C43 1.388(4) . ? C42 H42 0.9500 . ? C43 C44 1.379(4) . ? C43 C46A 1.514(7) . ? C43 C46 1.538(7) . ? C44 C45 1.378(3) . ? C44 H44 0.9500 . ? C45 N1 1.342(3) . ? C45 H45 0.9500 . ? C46 C47B 1.347(12) . ? C46 C47 1.365(10) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C46A C47A 1.433(14) . ? C46A H46C 0.9900 . ? C46A H46D 0.9900 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C47B H47D 0.9800 . ? C47B H47E 0.9800 . ? C47B H47F 0.9800 . ? C47A H47G 0.9800 . ? C47A H47H 0.9800 . ? C47A H47I 0.9800 . ? C48 N2 1.328(3) . ? C48 C49 1.384(3) . ? C48 H48 0.9500 . ? C49 C50 1.386(3) . ? C49 H49 0.9500 . ? C50 C51 1.379(3) . ? C50 C53 1.511(3) . ? C51 C52 1.371(3) . ? C51 H51 0.9500 . ? C52 N2 1.336(3) . ? C52 H52 0.9500 . ? C53 C54 1.501(4) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 N3 1.337(3) . ? C55 C56 1.383(3) . ? C55 H55 0.9500 . ? C56 C57 1.383(3) . ? C56 H56 0.9500 . ? C57 C58 1.393(3) . ? C57 C60 1.509(4) . ? C58 C59 1.373(3) . ? C58 H58 0.9500 . ? C59 N3 1.342(3) . ? C59 H59 0.9500 . ? C60 C61 1.505(5) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 N4 1.339(3) . ? C62 C63 1.383(3) . ? C62 H62 0.9500 . ? C63 C64 1.384(3) . ? C63 H63 0.9500 . ? C64 C65 1.391(3) . ? C64 C67 1.514(3) . ? C65 C66 1.372(3) . ? C65 H65 0.9500 . ? C66 N4 1.339(3) . ? C66 H66 0.9500 . ? C67 C68 1.504(4) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? N1 Co1 2.1596(18) . ? N2 Co1 2.1974(19) . ? N3 Co2 2.2030(19) . ? N4 Co2 2.1699(18) . ? O1 Co1 2.0340(14) . ? O2 Co1 2.0412(14) . ? O3 Co1 2.0439(13) 2_667 ? O4 Co1 2.0493(14) 2_667 ? O7 Co2 2.0374(14) 2_666 ? O6 Co2 2.0424(14) . ? O8 Co2 2.0424(15) 2_666 ? O5 Co2 2.0394(14) . ? Co1 O3 2.0439(13) 2_667 ? Co1 O4 2.0493(14) 2_667 ? Co2 O7 2.0374(14) 2_666 ? Co2 O8 2.0424(15) 2_666 ? 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 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 C1 109.18(19) . . ? C2 C4 C3 109.66(19) . . ? C1 C4 C3 108.83(19) . . ? C2 C4 C5 106.73(17) . . ? C1 C4 C5 114.34(17) . . ? C3 C4 C5 108.04(17) . . ? O1 C5 C6 124.98(18) . . ? O1 C5 C4 115.08(17) . . ? C6 C5 C4 119.91(17) . . ? C5 C6 C7 125.50(19) . . ? C5 C6 H6 117.2 . . ? C7 C6 H6 117.2 . . ? O2 C7 C6 125.65(18) . . ? O2 C7 C8 116.21(16) . . ? C6 C7 C8 118.14(17) . . ? C13 C8 C9 118.66(18) . . ? C13 C8 C7 122.86(17) . . ? C9 C8 C7 118.46(17) . . ? C8 C9 C10 121.43(18) . . ? C8 C9 H9 119.3 . . ? C10 C9 H9 119.3 . . ? C9 C10 C11 118.66(18) . . ? C9 C10 C14 118.60(17) . . ? C11 C10 C14 122.73(18) . . ? C12 C11 C10 120.31(19) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 120.46(19) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C8 120.46(18) . . ? C12 C13 H13 119.8 . . ? C8 C13 H13 119.8 . . ? O3 C14 C15 125.53(17) . . ? O3 C14 C10 115.88(17) . . ? C15 C14 C10 118.59(17) . . ? C16 C15 C14 125.31(18) . . ? C16 C15 H15 117.3 . . ? C14 C15 H15 117.3 . . ? O4 C16 C15 124.87(18) . . ? O4 C16 C17 115.24(17) . . ? C15 C16 C17 119.88(18) . . ? C18 C17 C19 110.7(2) . . ? C18 C17 C20 109.8(2) . . ? C19 C17 C20 107.81(19) . . ? C18 C17 C16 106.87(18) . . ? C19 C17 C16 114.43(17) . . ? C20 C17 C16 107.13(18) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C24 C21 H21A 109.5 . . ? C24 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C24 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C22 H22A 109.5 . . ? C24 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C24 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C23 C24 C22 109.1(2) . . ? C23 C24 C21 108.7(2) . . ? C22 C24 C21 109.78(19) . . ? C23 C24 C25 114.23(18) . . ? C22 C24 C25 108.63(18) . . ? C21 C24 C25 106.34(17) . . ? O5 C25 C26 124.67(19) . . ? O5 C25 C24 114.65(18) . . ? C26 C25 C24 120.56(18) . . ? C25 C26 C27 125.5(2) . . ? C25 C26 H26 117.2 . . ? C27 C26 H26 117.2 . . ? O6 C27 C26 125.85(19) . . ? O6 C27 C28 115.82(18) . . ? C26 C27 C28 118.32(18) . . ? C33 C28 C29 118.90(19) . . ? C33 C28 C27 121.50(18) . . ? C29 C28 C27 119.46(18) . . ? C30 C29 C28 121.22(19) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C29 C30 C31 118.44(18) . . ? C29 C30 C34 119.29(18) . . ? C31 C30 C34 122.24(18) . . ? C32 C31 C30 120.6(2) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C33 C32 C31 120.6(2) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 C28 120.24(19) . . ? C32 C33 H33 119.9 . . ? C28 C33 H33 119.9 . . ? O7 C34 C35 125.19(19) . . ? O7 C34 C30 115.37(17) . . ? C35 C34 C30 119.43(18) . . ? C34 C35 C36 125.6(2) . . ? C34 C35 H35 117.2 . . ? C36 C35 H35 117.2 . . ? O8 C36 C35 124.81(19) . . ? O8 C36 C37 115.56(19) . . ? C35 C36 C37 119.63(19) . . ? C39A C37 C40 135.2(4) . . ? C39A C37 C38 52.2(4) . . ? C40 C37 C38 114.3(4) . . ? C39A C37 C40A 118.0(4) . . ? C38 C37 C40A 131.7(4) . . ? C39A C37 C36 114.1(3) . . ? C40 C37 C36 109.9(3) . . ? C38 C37 C36 115.4(3) . . ? C40A C37 C36 110.9(3) . . ? C39A C37 C39 50.5(3) . . ? C40 C37 C39 110.1(4) . . ? C38 C37 C39 101.7(4) . . ? C40A C37 C39 78.7(4) . . ? C36 C37 C39 104.6(3) . . ? C39A C37 C38A 107.0(4) . . ? C40 C37 C38A 67.0(4) . . ? C38 C37 C38A 56.3(3) . . ? C40A C37 C38A 98.2(4) . . ? C36 C37 C38A 106.7(3) . . ? C39 C37 C38A 147.4(4) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? C37 C38A H38D 109.5 . . ? C37 C38A H38E 109.5 . . ? H38D C38A H38E 109.5 . . ? C37 C38A H38F 109.5 . . ? H38D C38A H38F 109.5 . . ? H38E C38A H38F 109.5 . . ? C37 C39A H39D 109.5 . . ? C37 C39A H39E 109.5 . . ? H39D C39A H39E 109.5 . . ? C37 C39A H39F 109.5 . . ? H39D C39A H39F 109.5 . . ? H39E C39A H39F 109.5 . . ? C37 C40A H40D 109.5 . . ? C37 C40A H40E 109.5 . . ? H40D C40A H40E 109.5 . . ? C37 C40A H40F 109.5 . . ? H40D C40A H40F 109.5 . . ? H40E C40A H40F 109.5 . . ? N1 C41 C42 123.3(2) . . ? N1 C41 H41 118.4 . . ? C42 C41 H41 118.4 . . ? C41 C42 C43 119.9(2) . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C44 C43 C42 116.9(2) . . ? C44 C43 C46A 116.0(3) . . ? C42 C43 C46A 126.4(3) . . ? C44 C43 C46 124.3(3) . . ? C42 C43 C46 118.4(3) . . ? C45 C44 C43 119.7(2) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? N1 C45 C44 123.6(2) . . ? N1 C45 H45 118.2 . . ? C44 C45 H45 118.2 . . ? C47B C46 C43 123.9(7) . . ? C47 C46 C43 122.0(6) . . ? C47B C46 H46A 78.5 . . ? C47 C46 H46A 106.8 . . ? C43 C46 H46A 106.8 . . ? C47B C46 H46B 125.5 . . ? C47 C46 H46B 106.8 . . ? C43 C46 H46B 106.8 . . ? H46A C46 H46B 106.7 . . ? C47A C46A C43 119.5(8) . . ? C47A C46A H46C 107.4 . . ? C43 C46A H46C 107.4 . . ? C47A C46A H46D 107.4 . . ? C43 C46A H46D 107.4 . . ? H46C C46A H46D 107.0 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? C46 C47B H47D 109.5 . . ? C46 C47B H47E 109.5 . . ? H47D C47B H47E 109.5 . . ? C46 C47B H47F 109.5 . . ? H47D C47B H47F 109.5 . . ? H47E C47B H47F 109.5 . . ? C46A C47A H47G 109.5 . . ? C46A C47A H47H 109.5 . . ? C46A C47A H47I 109.5 . . ? N2 C48 C49 123.6(2) . . ? N2 C48 H48 118.2 . . ? C49 C48 H48 118.2 . . ? C48 C49 C50 119.8(2) . . ? C48 C49 H49 120.1 . . ? C50 C49 H49 120.1 . . ? C51 C50 C49 116.2(2) . . ? C51 C50 C53 120.6(2) . . ? C49 C50 C53 123.2(2) . . ? C52 C51 C50 120.5(2) . . ? C52 C51 H51 119.8 . . ? C50 C51 H51 119.8 . . ? N2 C52 C51 123.5(2) . . ? N2 C52 H52 118.2 . . ? C51 C52 H52 118.2 . . ? C54 C53 C50 115.7(2) . . ? C54 C53 H53A 108.4 . . ? C50 C53 H53A 108.4 . . ? C54 C53 H53B 108.4 . . ? C50 C53 H53B 108.4 . . ? H53A C53 H53B 107.4 . . ? N3 C55 C56 123.2(2) . . ? N3 C55 H55 118.4 . . ? C56 C55 H55 118.4 . . ? C55 C56 C57 120.3(2) . . ? C55 C56 H56 119.9 . . ? C57 C56 H56 119.9 . . ? C56 C57 C58 116.4(2) . . ? C56 C57 C60 122.3(2) . . ? C58 C57 C60 121.3(2) . . ? C59 C58 C57 119.9(2) . . ? C59 C58 H58 120.0 . . ? C57 C58 H58 120.0 . . ? N3 C59 C58 123.6(2) . . ? N3 C59 H59 118.2 . . ? C58 C59 H59 118.2 . . ? C61 C60 C57 112.8(2) . . ? C61 C60 H60A 109.0 . . ? C57 C60 H60A 109.0 . . ? C61 C60 H60B 109.0 . . ? C57 C60 H60B 109.0 . . ? H60A C60 H60B 107.8 . . ? N4 C62 C63 123.4(2) . . ? N4 C62 H62 118.3 . . ? C63 C62 H62 118.3 . . ? C62 C63 C64 119.4(2) . . ? C62 C63 H63 120.3 . . ? C64 C63 H63 120.3 . . ? C63 C64 C65 117.1(2) . . ? C63 C64 C67 121.8(2) . . ? C65 C64 C67 121.1(2) . . ? C66 C65 C64 119.8(2) . . ? C66 C65 H65 120.1 . . ? C64 C65 H65 120.1 . . ? N4 C66 C65 123.4(2) . . ? N4 C66 H66 118.3 . . ? C65 C66 H66 118.3 . . ? C68 C67 C64 113.1(2) . . ? C68 C67 H67A 108.9 . . ? C64 C67 H67A 108.9 . . ? C68 C67 H67B 108.9 . . ? C64 C67 H67B 108.9 . . ? H67A C67 H67B 107.8 . . ? C41 N1 C45 116.5(2) . . ? C41 N1 Co1 119.97(15) . . ? C45 N1 Co1 123.40(15) . . ? C48 N2 C52 116.3(2) . . ? C48 N2 Co1 124.56(15) . . ? C52 N2 Co1 117.94(15) . . ? C55 N3 C59 116.53(19) . . ? C55 N3 Co2 124.26(15) . . ? C59 N3 Co2 118.77(14) . . ? C66 N4 C62 116.76(19) . . ? C66 N4 Co2 121.72(15) . . ? C62 N4 Co2 121.52(14) . . ? C5 O1 Co1 127.04(13) . . ? C7 O2 Co1 126.37(12) . . ? C14 O3 Co1 125.77(12) . 2_667 ? C16 O4 Co1 126.41(12) . 2_667 ? C34 O7 Co2 124.03(13) . 2_666 ? C27 O6 Co2 126.16(13) . . ? C36 O8 Co2 124.75(13) . 2_666 ? C25 O5 Co2 127.02(13) . . ? O1 Co1 O2 89.03(5) . . ? O1 Co1 O3 177.07(6) . 2_667 ? O2 Co1 O3 88.63(5) . 2_667 ? O1 Co1 O4 94.53(6) . 2_667 ? O2 Co1 O4 176.44(5) . 2_667 ? O3 Co1 O4 87.81(5) 2_667 2_667 ? O1 Co1 N1 90.11(6) . . ? O2 Co1 N1 91.13(6) . . ? O3 Co1 N1 91.69(6) 2_667 . ? O4 Co1 N1 89.05(6) 2_667 . ? O1 Co1 N2 89.31(6) . . ? O2 Co1 N2 94.11(6) . . ? O3 Co1 N2 89.11(6) 2_667 . ? O4 Co1 N2 85.76(6) 2_667 . ? N1 Co1 N2 174.72(7) . . ? O7 Co2 O5 176.41(6) 2_666 . ? O7 Co2 O8 88.39(6) 2_666 2_666 ? O5 Co2 O8 94.48(6) . 2_666 ? O7 Co2 O6 88.46(6) 2_666 . ? O5 Co2 O6 88.58(6) . . ? O8 Co2 O6 175.94(6) 2_666 . ? O7 Co2 N4 92.25(6) 2_666 . ? O5 Co2 N4 90.00(6) . . ? O8 Co2 N4 88.13(6) 2_666 . ? O6 Co2 N4 94.56(6) . . ? O7 Co2 N3 89.62(6) 2_666 . ? O5 Co2 N3 88.39(6) . . ? O8 Co2 N3 86.69(6) 2_666 . ? O6 Co2 N3 90.72(6) . . ? N4 Co2 N3 174.44(7) . . ? 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 C2 C4 C5 O1 64.5(2) . . . . ? C1 C4 C5 O1 -174.68(19) . . . . ? C3 C4 C5 O1 -53.4(2) . . . . ? C2 C4 C5 C6 -113.5(2) . . . . ? C1 C4 C5 C6 7.3(3) . . . . ? C3 C4 C5 C6 128.6(2) . . . . ? O1 C5 C6 C7 -2.5(4) . . . . ? C4 C5 C6 C7 175.3(2) . . . . ? C5 C6 C7 O2 3.5(4) . . . . ? C5 C6 C7 C8 -176.8(2) . . . . ? O2 C7 C8 C13 -164.15(19) . . . . ? C6 C7 C8 C13 16.1(3) . . . . ? O2 C7 C8 C9 17.3(3) . . . . ? C6 C7 C8 C9 -162.45(19) . . . . ? C13 C8 C9 C10 -0.9(3) . . . . ? C7 C8 C9 C10 177.68(18) . . . . ? C8 C9 C10 C11 -0.4(3) . . . . ? C8 C9 C10 C14 -179.27(18) . . . . ? C9 C10 C11 C12 1.2(3) . . . . ? C14 C10 C11 C12 -180.0(2) . . . . ? C10 C11 C12 C13 -0.7(4) . . . . ? C11 C12 C13 C8 -0.7(4) . . . . ? C9 C8 C13 C12 1.5(3) . . . . ? C7 C8 C13 C12 -177.1(2) . . . . ? C9 C10 C14 O3 16.1(3) . . . . ? C11 C10 C14 O3 -162.67(19) . . . . ? C9 C10 C14 C15 -163.99(19) . . . . ? C11 C10 C14 C15 17.2(3) . . . . ? O3 C14 C15 C16 1.8(3) . . . . ? C10 C14 C15 C16 -178.04(19) . . . . ? C14 C15 C16 O4 -2.3(4) . . . . ? C14 C15 C16 C17 176.6(2) . . . . ? O4 C16 C17 C18 -60.0(2) . . . . ? C15 C16 C17 C18 121.0(2) . . . . ? O4 C16 C17 C19 177.05(19) . . . . ? C15 C16 C17 C19 -2.0(3) . . . . ? O4 C16 C17 C20 57.6(2) . . . . ? C15 C16 C17 C20 -121.4(2) . . . . ? C23 C24 C25 O5 -165.8(2) . . . . ? C22 C24 C25 O5 -43.8(2) . . . . ? C21 C24 C25 O5 74.3(2) . . . . ? C23 C24 C25 C26 17.8(3) . . . . ? C22 C24 C25 C26 139.9(2) . . . . ? C21 C24 C25 C26 -102.0(2) . . . . ? O5 C25 C26 C27 -1.4(3) . . . . ? C24 C25 C26 C27 174.6(2) . . . . ? C25 C26 C27 O6 4.2(4) . . . . ? C25 C26 C27 C28 -174.07(19) . . . . ? O6 C27 C28 C33 -148.8(2) . . . . ? C26 C27 C28 C33 29.7(3) . . . . ? O6 C27 C28 C29 26.9(3) . . . . ? C26 C27 C28 C29 -154.7(2) . . . . ? C33 C28 C29 C30 -1.0(3) . . . . ? C27 C28 C29 C30 -176.79(18) . . . . ? C28 C29 C30 C31 0.8(3) . . . . ? C28 C29 C30 C34 178.79(18) . . . . ? C29 C30 C31 C32 0.1(3) . . . . ? C34 C30 C31 C32 -177.8(2) . . . . ? C30 C31 C32 C33 -0.7(3) . . . . ? C31 C32 C33 C28 0.4(3) . . . . ? C29 C28 C33 C32 0.5(3) . . . . ? C27 C28 C33 C32 176.1(2) . . . . ? C29 C30 C34 O7 13.2(3) . . . . ? C31 C30 C34 O7 -168.87(19) . . . . ? C29 C30 C34 C35 -165.5(2) . . . . ? C31 C30 C34 C35 12.4(3) . . . . ? O7 C34 C35 C36 1.8(4) . . . . ? C30 C34 C35 C36 -179.7(2) . . . . ? C34 C35 C36 O8 -2.8(4) . . . . ? C34 C35 C36 C37 176.2(2) . . . . ? O8 C36 C37 C39A 116.6(4) . . . . ? C35 C36 C37 C39A -62.5(4) . . . . ? O8 C36 C37 C40 -54.4(4) . . . . ? C35 C36 C37 C40 126.5(4) . . . . ? O8 C36 C37 C38 174.5(3) . . . . ? C35 C36 C37 C38 -4.6(4) . . . . ? O8 C36 C37 C40A -19.6(4) . . . . ? C35 C36 C37 C40A 161.4(3) . . . . ? O8 C36 C37 C39 63.7(3) . . . . ? C35 C36 C37 C39 -115.4(3) . . . . ? O8 C36 C37 C38A -125.4(3) . . . . ? C35 C36 C37 C38A 55.5(4) . . . . ? N1 C41 C42 C43 -0.2(4) . . . . ? C41 C42 C43 C44 -0.6(4) . . . . ? C41 C42 C43 C46A 169.2(4) . . . . ? C41 C42 C43 C46 -173.5(4) . . . . ? C42 C43 C44 C45 1.0(4) . . . . ? C46A C43 C44 C45 -169.8(3) . . . . ? C46 C43 C44 C45 173.5(4) . . . . ? C43 C44 C45 N1 -0.8(3) . . . . ? C44 C43 C46 C47B -158.1(7) . . . . ? C42 C43 C46 C47B 14.3(9) . . . . ? C46A C43 C46 C47B 138(2) . . . . ? C44 C43 C46 C47 166.1(5) . . . . ? C42 C43 C46 C47 -21.5(8) . . . . ? C46A C43 C46 C47 101.7(18) . . . . ? C44 C43 C46A C47A 157.1(5) . . . . ? C42 C43 C46A C47A -12.8(8) . . . . ? C46 C43 C46A C47A -78.9(17) . . . . ? N2 C48 C49 C50 -0.3(4) . . . . ? C48 C49 C50 C51 2.4(4) . . . . ? C48 C49 C50 C53 -175.2(2) . . . . ? C49 C50 C51 C52 -2.4(4) . . . . ? C53 C50 C51 C52 175.3(2) . . . . ? C50 C51 C52 N2 0.3(4) . . . . ? C51 C50 C53 C54 155.8(2) . . . . ? C49 C50 C53 C54 -26.7(4) . . . . ? N3 C55 C56 C57 1.0(4) . . . . ? C55 C56 C57 C58 -0.3(4) . . . . ? C55 C56 C57 C60 178.4(3) . . . . ? C56 C57 C58 C59 -0.4(4) . . . . ? C60 C57 C58 C59 -179.1(3) . . . . ? C57 C58 C59 N3 0.4(4) . . . . ? C56 C57 C60 C61 -107.2(3) . . . . ? C58 C57 C60 C61 71.4(4) . . . . ? N4 C62 C63 C64 1.1(3) . . . . ? C62 C63 C64 C65 0.2(3) . . . . ? C62 C63 C64 C67 -179.9(2) . . . . ? C63 C64 C65 C66 -0.9(4) . . . . ? C67 C64 C65 C66 179.1(3) . . . . ? C64 C65 C66 N4 0.5(4) . . . . ? C63 C64 C67 C68 -104.5(3) . . . . ? C65 C64 C67 C68 75.5(4) . . . . ? C42 C41 N1 C45 0.5(4) . . . . ? C42 C41 N1 Co1 177.1(2) . . . . ? C44 C45 N1 C41 0.0(3) . . . . ? C44 C45 N1 Co1 -176.48(16) . . . . ? C49 C48 N2 C52 -1.8(4) . . . . ? C49 C48 N2 Co1 165.5(2) . . . . ? C51 C52 N2 C48 1.8(3) . . . . ? C51 C52 N2 Co1 -166.35(19) . . . . ? C56 C55 N3 C59 -0.9(3) . . . . ? C56 C55 N3 Co2 171.39(18) . . . . ? C58 C59 N3 C55 0.2(3) . . . . ? C58 C59 N3 Co2 -172.55(19) . . . . ? C65 C66 N4 C62 0.8(3) . . . . ? C65 C66 N4 Co2 -179.8(2) . . . . ? C63 C62 N4 C66 -1.6(3) . . . . ? C63 C62 N4 Co2 178.99(16) . . . . ? C6 C5 O1 Co1 -7.9(3) . . . . ? C4 C5 O1 Co1 174.16(13) . . . . ? C6 C7 O2 Co1 6.0(3) . . . . ? C8 C7 O2 Co1 -173.71(12) . . . . ? C15 C14 O3 Co1 14.2(3) . . . 2_667 ? C10 C14 O3 Co1 -165.95(13) . . . 2_667 ? C15 C16 O4 Co1 -13.4(3) . . . 2_667 ? C17 C16 O4 Co1 167.68(13) . . . 2_667 ? C35 C34 O7 Co2 18.7(3) . . . 2_666 ? C30 C34 O7 Co2 -159.88(13) . . . 2_666 ? C26 C27 O6 Co2 6.5(3) . . . . ? C28 C27 O6 Co2 -175.21(12) . . . . ? C35 C36 O8 Co2 -16.9(3) . . . 2_666 ? C37 C36 O8 Co2 164.06(15) . . . 2_666 ? C26 C25 O5 Co2 -11.7(3) . . . . ? C24 C25 O5 Co2 172.13(13) . . . . ? C5 O1 Co1 O2 12.17(17) . . . . ? C5 O1 Co1 O4 -167.64(17) . . . 2_667 ? C5 O1 Co1 N1 103.30(17) . . . . ? C5 O1 Co1 N2 -81.95(17) . . . . ? C7 O2 Co1 O1 -11.18(17) . . . . ? C7 O2 Co1 O3 167.07(16) . . . 2_667 ? C7 O2 Co1 N1 -101.27(17) . . . . ? C7 O2 Co1 N2 78.06(17) . . . . ? C41 N1 Co1 O1 137.01(17) . . . . ? C45 N1 Co1 O1 -46.63(16) . . . . ? C41 N1 Co1 O2 -133.96(17) . . . . ? C45 N1 Co1 O2 42.40(16) . . . . ? C41 N1 Co1 O3 -45.30(17) . . . 2_667 ? C45 N1 Co1 O3 131.06(16) . . . 2_667 ? C41 N1 Co1 O4 42.48(17) . . . 2_667 ? C45 N1 Co1 O4 -141.16(16) . . . 2_667 ? C48 N2 Co1 O1 154.86(19) . . . . ? C52 N2 Co1 O1 -38.06(16) . . . . ? C48 N2 Co1 O2 65.89(19) . . . . ? C52 N2 Co1 O2 -127.03(16) . . . . ? C48 N2 Co1 O3 -22.67(19) . . . 2_667 ? C52 N2 Co1 O3 144.41(16) . . . 2_667 ? C48 N2 Co1 O4 -110.54(19) . . . 2_667 ? C52 N2 Co1 O4 56.54(16) . . . 2_667 ? C25 O5 Co2 O8 -161.51(16) . . . 2_666 ? C25 O5 Co2 O6 15.80(16) . . . . ? C25 O5 Co2 N4 110.37(17) . . . . ? C25 O5 Co2 N3 -74.95(17) . . . . ? C27 O6 Co2 O7 164.87(16) . . . 2_666 ? C27 O6 Co2 O5 -13.10(16) . . . . ? C27 O6 Co2 N4 -102.99(16) . . . . ? C27 O6 Co2 N3 75.27(17) . . . . ? C66 N4 Co2 O7 153.62(17) . . . 2_666 ? C62 N4 Co2 O7 -26.96(16) . . . 2_666 ? C66 N4 Co2 O5 -23.59(17) . . . . ? C62 N4 Co2 O5 155.83(16) . . . . ? C66 N4 Co2 O8 -118.07(17) . . . 2_666 ? C62 N4 Co2 O8 61.35(16) . . . 2_666 ? C66 N4 Co2 O6 64.98(18) . . . . ? C62 N4 Co2 O6 -115.60(16) . . . . ? C55 N3 Co2 O7 -31.98(18) . . . 2_666 ? C59 N3 Co2 O7 140.16(17) . . . 2_666 ? C55 N3 Co2 O5 145.03(18) . . . . ? C59 N3 Co2 O5 -42.83(16) . . . . ? C55 N3 Co2 O8 -120.39(18) . . . 2_666 ? C59 N3 Co2 O8 51.75(16) . . . 2_666 ? C55 N3 Co2 O6 56.47(18) . . . . ? C59 N3 Co2 O6 -131.39(16) . . . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.972 _refine_diff_density_min -0.742 _refine_diff_density_rms 0.063