# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email jc671@cam.ac.uk _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_name 'Jack Clegg' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; ENTER SECTION TITLE ; loop_ _publ_author_name P.D.Bonnitcha B.J.Kim R.Hocking J.Clegg P.Turner S.Neville ; T.Hambley ; data_1 _database_code_depnum_ccdc_archive 'CCDC 866265' #TrackingRef '- combined revised cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C80 H121 Cl8 Co4 N16 O42.50' _chemical_formula_sum 'C80 H121 Cl8 Co4 N16 O42.50' _chemical_formula_weight 2506.25 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Intl_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.3978(8) _cell_length_b 28.7543(18) _cell_length_c 26.4339(17) _cell_angle_alpha 90.00 _cell_angle_beta 93.677(4) _cell_angle_gamma 90.00 _cell_volume 10162.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8292 _cell_measurement_theta_min 2.532 _cell_measurement_theta_max 31.915 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.280 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5188 _exptl_absorpt_coefficient_mu 0.951 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.766 _exptl_absorpt_correction_T_max 0.827 _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 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type APEXII-FR591 _diffrn_measurement_method \w+\f _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 218559 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 31.80 _reflns_number_total 34567 _reflns_number_gt 23279 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX (Bruker-Nonius, 2003)' _computing_cell_refinement 'SAINT (Bruker-Nonius, 2003)' _computing_data_reduction 'SAINT (Bruker-Nonius, 2003), XPREP (Bruker-Nonius, 2003)' _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 1.1 (CCDC, 2005)' _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^)+(0.0534P)^2^+1.8638P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 34567 _refine_ls_number_parameters 1507 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.0613 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.1054 _refine_ls_wR_factor_gt 0.0931 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.13415(11) 0.25853(5) 0.56266(5) 0.0210(3) Uani 1 1 d . . . H1A H 0.0632 0.2622 0.5503 0.025 Uiso 1 1 calc R . . H1B H 0.1707 0.2438 0.5355 0.025 Uiso 1 1 calc R . . C2 C 0.17939(12) 0.30561(5) 0.57621(5) 0.0247(3) Uani 1 1 d . . . H2A H 0.1945 0.3225 0.5449 0.030 Uiso 1 1 calc R . . H2B H 0.1313 0.3244 0.5944 0.030 Uiso 1 1 calc R . . C3 C 0.06689(10) 0.24389(5) 0.64671(5) 0.0201(3) Uani 1 1 d . . . H3A H 0.0380 0.2161 0.6623 0.024 Uiso 1 1 calc R . . H3B H 0.0117 0.2615 0.6288 0.024 Uiso 1 1 calc R . . C4 C 0.11777(11) 0.27422(5) 0.68779(5) 0.0217(3) Uani 1 1 d . . . H4A H 0.1213 0.3068 0.6758 0.026 Uiso 1 1 calc R . . H4B H 0.0792 0.2737 0.7185 0.026 Uiso 1 1 calc R . . C5 C 0.12941(10) 0.17825(5) 0.59773(5) 0.0205(3) Uani 1 1 d . . . H5A H 0.1651 0.1700 0.5673 0.025 Uiso 1 1 calc R . . H5B H 0.0577 0.1706 0.5911 0.025 Uiso 1 1 calc R . . C6 C 0.17295(11) 0.15142(5) 0.64357(5) 0.0228(3) Uani 1 1 d . . . H6A H 0.1293 0.1549 0.6722 0.027 Uiso 1 1 calc R . . H6B H 0.1777 0.1180 0.6353 0.027 Uiso 1 1 calc R . . C7 C 0.58099(11) 0.23805(6) 0.68730(5) 0.0254(3) Uani 1 1 d . . . H7A H 0.5787 0.2686 0.7037 0.038 Uiso 1 1 calc R . . H7B H 0.6403 0.2362 0.6675 0.038 Uiso 1 1 calc R . . H7C H 0.5842 0.2136 0.7132 0.038 Uiso 1 1 calc R . . C8 C 0.48857(10) 0.23152(5) 0.65269(5) 0.0183(3) Uani 1 1 d . . . C9 C 0.49793(10) 0.21358(5) 0.60383(5) 0.0184(3) Uani 1 1 d . . . H9 H 0.5626 0.2046 0.5948 0.022 Uiso 1 1 calc R . . C10 C 0.41830(10) 0.20816(4) 0.56782(5) 0.0156(2) Uani 1 1 d . . . C11 C 0.43504(10) 0.19303(4) 0.51523(5) 0.0157(2) Uani 1 1 d . . . C12 C 0.51414(10) 0.16489(5) 0.50458(5) 0.0173(3) Uani 1 1 d . . . H12 H 0.5610 0.1558 0.5312 0.021 Uiso 1 1 calc R . . C13 C 0.52685(10) 0.14924(5) 0.45441(5) 0.0174(3) Uani 1 1 d . . . C14 C 0.60479(11) 0.11829(5) 0.44307(5) 0.0227(3) Uani 1 1 d . . . H14 H 0.6510 0.1080 0.4694 0.027 Uiso 1 1 calc R . . C15 C 0.61413(12) 0.10301(5) 0.39418(5) 0.0264(3) Uani 1 1 d . . . H15 H 0.6656 0.0817 0.3872 0.032 Uiso 1 1 calc R . . C16 C 0.54714(11) 0.11908(5) 0.35448(5) 0.0244(3) Uani 1 1 d . . . H16 H 0.5544 0.1088 0.3208 0.029 Uiso 1 1 calc R . . C17 C 0.47183(11) 0.14938(5) 0.36431(5) 0.0220(3) Uani 1 1 d . . . H17 H 0.4280 0.1603 0.3372 0.026 Uiso 1 1 calc R . . C18 C 0.45871(10) 0.16455(5) 0.41449(5) 0.0173(3) Uani 1 1 d . . . C19 C 0.37877(10) 0.19437(5) 0.42617(5) 0.0203(3) Uani 1 1 d . . . H19 H 0.3336 0.2053 0.3996 0.024 Uiso 1 1 calc R . . C20 C 0.36583(10) 0.20765(5) 0.47501(5) 0.0190(3) Uani 1 1 d . . . H20 H 0.3105 0.2267 0.4822 0.023 Uiso 1 1 calc R . . C21 C 0.62062(10) 0.06963(5) 0.58267(5) 0.0190(3) Uani 1 1 d . . . H21A H 0.5491 0.0750 0.5725 0.023 Uiso 1 1 calc R . . H21B H 0.6598 0.0736 0.5524 0.023 Uiso 1 1 calc R . . C22 C 0.65566(10) 0.10390(5) 0.62340(5) 0.0219(3) Uani 1 1 d . . . H22A H 0.6624 0.1352 0.6085 0.026 Uiso 1 1 calc R . . H22B H 0.6063 0.1057 0.6496 0.026 Uiso 1 1 calc R . . C23 C 0.63431(11) -0.01411(5) 0.56268(5) 0.0219(3) Uani 1 1 d . . . H23A H 0.6708 -0.0023 0.5339 0.026 Uiso 1 1 calc R . . H23B H 0.5646 -0.0209 0.5502 0.026 Uiso 1 1 calc R . . C24 C 0.68410(12) -0.05809(5) 0.58371(5) 0.0257(3) Uani 1 1 d . . . H24A H 0.6369 -0.0757 0.6037 0.031 Uiso 1 1 calc R . . H24B H 0.7038 -0.0781 0.5556 0.031 Uiso 1 1 calc R . . C25 C 0.55882(10) 0.01099(5) 0.64171(5) 0.0188(3) Uani 1 1 d . . . H25A H 0.5039 -0.0078 0.6254 0.023 Uiso 1 1 calc R . . H25B H 0.5300 0.0404 0.6537 0.023 Uiso 1 1 calc R . . C26 C 0.60744(10) -0.01546(5) 0.68637(5) 0.0203(3) Uani 1 1 d . . . H26A H 0.5650 -0.0139 0.7156 0.024 Uiso 1 1 calc R . . H26B H 0.6164 -0.0485 0.6773 0.024 Uiso 1 1 calc R . . C27 C 1.06851(11) 0.01906(5) 0.69071(5) 0.0241(3) Uani 1 1 d . . . H27A H 1.0770 0.0465 0.7126 0.036 Uiso 1 1 calc R . . H27B H 1.1280 0.0151 0.6714 0.036 Uiso 1 1 calc R . . H27C H 1.0594 -0.0086 0.7116 0.036 Uiso 1 1 calc R . . C28 C 0.97823(10) 0.02552(5) 0.65467(5) 0.0171(2) Uani 1 1 d . . . C29 C 0.99130(10) 0.03943(5) 0.60457(5) 0.0180(3) Uani 1 1 d . . . H29 H 1.0572 0.0465 0.5956 0.022 Uiso 1 1 calc R . . C30 C 0.91360(10) 0.04354(4) 0.56734(4) 0.0148(2) Uani 1 1 d . . . C31 C 0.93325(10) 0.05788(4) 0.51477(4) 0.0154(2) Uani 1 1 d . . . C32 C 1.01110(10) 0.08706(5) 0.50530(5) 0.0178(3) Uani 1 1 d . . . H32 H 1.0559 0.0968 0.5325 0.021 Uiso 1 1 calc R . . C33 C 1.02556(10) 0.10285(5) 0.45521(5) 0.0176(3) Uani 1 1 d . . . C34 C 1.10166(11) 0.13520(5) 0.44479(5) 0.0242(3) Uani 1 1 d . . . H34 H 1.1454 0.1466 0.4717 0.029 Uiso 1 1 calc R . . C35 C 1.11258(12) 0.15018(5) 0.39618(6) 0.0275(3) Uani 1 1 d . . . H35 H 1.1629 0.1723 0.3898 0.033 Uiso 1 1 calc R . . C36 C 1.04969(11) 0.13298(5) 0.35568(5) 0.0253(3) Uani 1 1 d . . . H36 H 1.0586 0.1432 0.3221 0.030 Uiso 1 1 calc R . . C37 C 0.97565(11) 0.10162(5) 0.36454(5) 0.0220(3) Uani 1 1 d . . . H37 H 0.9341 0.0900 0.3369 0.026 Uiso 1 1 calc R . . C38 C 0.96043(10) 0.08644(5) 0.41455(5) 0.0174(3) Uani 1 1 d . . . C39 C 0.88120(10) 0.05579(5) 0.42534(5) 0.0199(3) Uani 1 1 d . . . H39 H 0.8376 0.0444 0.3984 0.024 Uiso 1 1 calc R . . C40 C 0.86701(10) 0.04248(5) 0.47401(5) 0.0184(3) Uani 1 1 d . . . H40 H 0.8124 0.0228 0.4806 0.022 Uiso 1 1 calc R . . C41 C 0.94278(10) 0.26259(5) 0.35315(5) 0.0193(3) Uani 1 1 d . . . H41A H 0.9981 0.2441 0.3696 0.023 Uiso 1 1 calc R . . H41B H 0.9710 0.2920 0.3409 0.023 Uiso 1 1 calc R . . C42 C 0.89445(10) 0.23569(5) 0.30873(5) 0.0208(3) Uani 1 1 d . . . H42A H 0.9366 0.2374 0.2793 0.025 Uiso 1 1 calc R . . H42B H 0.8865 0.2026 0.3180 0.025 Uiso 1 1 calc R . . C43 C 0.88000(10) 0.32137(5) 0.41179(5) 0.0191(3) Uani 1 1 d . . . H43A H 0.9514 0.3270 0.4220 0.023 Uiso 1 1 calc R . . H43B H 0.8407 0.3254 0.4420 0.023 Uiso 1 1 calc R . . C44 C 0.84450(10) 0.35528(5) 0.37068(5) 0.0216(3) Uani 1 1 d . . . H44A H 0.8373 0.3867 0.3853 0.026 Uiso 1 1 calc R . . H44B H 0.8938 0.3570 0.3444 0.026 Uiso 1 1 calc R . . C45 C 0.86804(11) 0.23759(5) 0.43254(5) 0.0226(3) Uani 1 1 d . . . H45A H 0.8312 0.2493 0.4612 0.027 Uiso 1 1 calc R . . H45B H 0.9379 0.2312 0.4451 0.027 Uiso 1 1 calc R . . C46 C 0.81943(12) 0.19350(5) 0.41163(6) 0.0266(3) Uani 1 1 d . . . H46A H 0.8666 0.1764 0.3911 0.032 Uiso 1 1 calc R . . H46B H 0.8013 0.1731 0.4398 0.032 Uiso 1 1 calc R . . C47 C 0.43240(11) 0.26734(6) 0.30483(5) 0.0247(3) Uani 1 1 d . . . H47A H 0.4234 0.2944 0.2824 0.037 Uiso 1 1 calc R . . H47B H 0.3730 0.2635 0.3242 0.037 Uiso 1 1 calc R . . H47C H 0.4420 0.2394 0.2845 0.037 Uiso 1 1 calc R . . C48 C 0.52271(10) 0.27470(5) 0.34076(5) 0.0178(3) Uani 1 1 d . . . C49 C 0.50951(10) 0.28865(5) 0.39071(5) 0.0184(3) Uani 1 1 d . . . H49 H 0.4433 0.2947 0.3999 0.022 Uiso 1 1 calc R . . C50 C 0.58720(10) 0.29416(4) 0.42766(5) 0.0154(2) Uani 1 1 d . . . C51 C 0.56766(10) 0.30888(4) 0.47987(5) 0.0156(2) Uani 1 1 d . . . C52 C 0.48957(10) 0.33812(5) 0.48884(5) 0.0181(3) Uani 1 1 d . . . H52 H 0.4446 0.3474 0.4614 0.022 Uiso 1 1 calc R . . C53 C 0.47499(10) 0.35468(5) 0.53844(5) 0.0182(3) Uani 1 1 d . . . C54 C 0.39884(11) 0.38729(5) 0.54785(5) 0.0253(3) Uani 1 1 d . . . H54 H 0.3549 0.3979 0.5206 0.030 Uiso 1 1 calc R . . C55 C 0.38825(12) 0.40366(5) 0.59615(6) 0.0285(3) Uani 1 1 d . . . H55 H 0.3388 0.4264 0.6019 0.034 Uiso 1 1 calc R . . C56 C 0.45087(12) 0.38675(5) 0.63712(5) 0.0267(3) Uani 1 1 d . . . H56 H 0.4419 0.3975 0.6705 0.032 Uiso 1 1 calc R . . C57 C 0.52429(11) 0.35501(5) 0.62906(5) 0.0236(3) Uani 1 1 d . . . H57 H 0.5653 0.3436 0.6570 0.028 Uiso 1 1 calc R . . C58 C 0.53994(10) 0.33893(5) 0.57955(5) 0.0185(3) Uani 1 1 d . . . C59 C 0.61897(11) 0.30822(5) 0.56933(5) 0.0214(3) Uani 1 1 d . . . H59 H 0.6622 0.2972 0.5966 0.026 Uiso 1 1 calc R . . C60 C 0.63422(10) 0.29412(5) 0.52093(5) 0.0203(3) Uani 1 1 d . . . H60 H 0.6892 0.2745 0.5147 0.024 Uiso 1 1 calc R . . C61 C 0.37089(10) 0.42523(5) 0.39672(5) 0.0210(3) Uani 1 1 d . . . H61A H 0.3350 0.4171 0.4271 0.025 Uiso 1 1 calc R . . H61B H 0.4424 0.4171 0.4033 0.025 Uiso 1 1 calc R . . C62 C 0.32674(11) 0.39893(5) 0.35085(5) 0.0227(3) Uani 1 1 d . . . H62A H 0.3705 0.4023 0.3223 0.027 Uiso 1 1 calc R . . H62B H 0.3212 0.3654 0.3590 0.027 Uiso 1 1 calc R . . C63 C 0.36842(11) 0.50542(5) 0.43227(5) 0.0216(3) Uani 1 1 d . . . H63A H 0.4394 0.5085 0.4447 0.026 Uiso 1 1 calc R . . H63B H 0.3312 0.4909 0.4593 0.026 Uiso 1 1 calc R . . C64 C 0.32472(12) 0.55284(5) 0.41868(5) 0.0253(3) Uani 1 1 d . . . H64A H 0.3108 0.5700 0.4499 0.030 Uiso 1 1 calc R . . H64B H 0.3731 0.5711 0.4001 0.030 Uiso 1 1 calc R . . C65 C 0.43492(10) 0.49056(5) 0.34820(5) 0.0214(3) Uani 1 1 d . . . H65A H 0.4630 0.4626 0.3325 0.026 Uiso 1 1 calc R . . H65B H 0.4906 0.5077 0.3663 0.026 Uiso 1 1 calc R . . C66 C 0.38531(11) 0.52141(5) 0.30723(5) 0.0220(3) Uani 1 1 d . . . H66A H 0.3827 0.5539 0.3194 0.026 Uiso 1 1 calc R . . H66B H 0.4240 0.5207 0.2766 0.026 Uiso 1 1 calc R . . C67 C -0.07921(11) 0.48928(6) 0.30813(5) 0.0265(3) Uani 1 1 d . . . H67A H -0.0736 0.5188 0.2901 0.040 Uiso 1 1 calc R . . H67B H -0.1380 0.4901 0.3283 0.040 Uiso 1 1 calc R . . H67C H -0.0862 0.4638 0.2836 0.040 Uiso 1 1 calc R . . C68 C 0.01321(10) 0.48176(5) 0.34251(5) 0.0188(3) Uani 1 1 d . . . C69 C 0.00311(10) 0.46423(5) 0.39143(5) 0.0190(3) Uani 1 1 d . . . H69 H -0.0621 0.4565 0.4009 0.023 Uiso 1 1 calc R . . C70 C 0.08328(10) 0.45742(4) 0.42708(5) 0.0158(2) Uani 1 1 d . . . C71 C 0.06594(10) 0.44218(5) 0.47954(5) 0.0161(2) Uani 1 1 d . . . C72 C -0.01387(10) 0.41434(5) 0.48973(5) 0.0180(3) Uani 1 1 d . . . H72 H -0.0611 0.4059 0.4630 0.022 Uiso 1 1 calc R . . C73 C -0.02678(10) 0.39804(5) 0.53966(5) 0.0179(3) Uani 1 1 d . . . C74 C -0.10485(11) 0.36681(5) 0.55033(5) 0.0241(3) Uani 1 1 d . . . H74 H -0.1513 0.3570 0.5238 0.029 Uiso 1 1 calc R . . C75 C -0.11354(12) 0.35082(5) 0.59874(6) 0.0274(3) Uani 1 1 d . . . H75 H -0.1646 0.3292 0.6054 0.033 Uiso 1 1 calc R . . C76 C -0.04694(12) 0.36636(5) 0.63885(5) 0.0260(3) Uani 1 1 d . . . H76 H -0.0544 0.3556 0.6724 0.031 Uiso 1 1 calc R . . C77 C 0.02828(11) 0.39689(5) 0.62964(5) 0.0238(3) Uani 1 1 d . . . H77 H 0.0720 0.4075 0.6570 0.029 Uiso 1 1 calc R . . C78 C 0.04170(10) 0.41290(5) 0.57973(5) 0.0188(3) Uani 1 1 d . . . C79 C 0.12190(11) 0.44257(5) 0.56850(5) 0.0224(3) Uani 1 1 d . . . H79 H 0.1672 0.4531 0.5952 0.027 Uiso 1 1 calc R . . C80 C 0.13499(10) 0.45615(5) 0.51986(5) 0.0210(3) Uani 1 1 d . . . H80 H 0.1906 0.4751 0.5129 0.025 Uiso 1 1 calc R . . N1 N 0.14159(8) 0.22892(4) 0.60914(4) 0.0164(2) Uani 1 1 d . . . N2 N 0.27403(10) 0.29866(4) 0.60929(4) 0.0209(2) Uani 1 1 d D . . N3 N 0.22019(9) 0.25582(4) 0.69982(4) 0.0190(2) Uani 1 1 d D . . N4 N 0.27434(9) 0.17046(4) 0.65786(4) 0.0185(2) Uani 1 1 d D . . N5 N 0.63503(8) 0.02159(4) 0.60373(4) 0.0157(2) Uani 1 1 d . . . N6 N 0.75457(9) 0.08802(4) 0.64670(4) 0.0180(2) Uani 1 1 d D . . N7 N 0.77514(9) -0.04472(4) 0.61686(4) 0.0208(2) Uani 1 1 d D . . N8 N 0.70598(9) 0.00661(4) 0.69933(4) 0.0189(2) Uani 1 1 d D . . N9 N 0.86637(8) 0.27311(4) 0.39122(4) 0.0157(2) Uani 1 1 d . . . N10 N 0.79516(9) 0.25704(4) 0.29578(4) 0.0192(2) Uani 1 1 d D . . N11 N 0.74581(9) 0.33887(4) 0.34762(4) 0.0180(2) Uani 1 1 d D . . N12 N 0.72723(9) 0.20640(4) 0.37929(4) 0.0210(2) Uani 1 1 d D . . N13 N 0.36005(8) 0.47597(4) 0.38545(4) 0.0169(2) Uani 1 1 d . . . N14 N 0.22575(9) 0.41853(4) 0.33662(4) 0.0189(2) Uani 1 1 d D . . N15 N 0.22915(10) 0.54640(4) 0.38605(4) 0.0214(2) Uani 1 1 d D . . N16 N 0.28251(9) 0.50366(4) 0.29510(4) 0.0193(2) Uani 1 1 d D . . O1 O 0.40662(7) 0.24390(3) 0.67105(3) 0.02001(19) Uani 1 1 d . . . O2 O 0.32562(7) 0.21641(3) 0.57565(3) 0.01762(19) Uani 1 1 d . . . O3 O 0.89446(7) 0.01720(3) 0.67322(3) 0.01855(19) Uani 1 1 d . . . O4 O 0.82072(7) 0.03503(3) 0.57375(3) 0.01700(18) Uani 1 1 d . . . O5 O 0.60693(7) 0.26729(3) 0.32195(3) 0.01923(19) Uani 1 1 d . . . O6 O 0.68063(7) 0.28652(3) 0.42105(3) 0.01708(18) Uani 1 1 d . . . O7 O 0.09553(7) 0.49300(3) 0.32380(3) 0.0202(2) Uani 1 1 d . . . O8 O 0.17587(7) 0.46423(3) 0.41897(3) 0.01756(19) Uani 1 1 d . . . O9 O 0.24678(10) 0.08031(6) 0.54382(5) 0.0545(4) Uani 1 1 d . . . O10 O 0.38186(9) 0.02866(4) 0.55289(4) 0.0355(3) Uani 1 1 d . . . O11 O 0.38178(8) 0.09624(4) 0.60283(4) 0.0321(3) Uani 1 1 d . . . O12 O 0.27033(11) 0.03593(5) 0.61736(5) 0.0459(3) Uani 1 1 d . . . O13 O 0.96428(8) 0.12421(4) 0.68726(4) 0.0338(3) Uani 1 1 d . H . O14 O 0.9669(5) 0.1890(2) 0.7464(6) 0.077(3) Uani 0.50 1 d PD H . O15 O 1.02075(10) 0.11675(5) 0.77274(5) 0.0479(3) Uani 1 1 d D H . O16 O 0.85218(9) 0.12999(8) 0.75045(5) 0.0809(7) Uani 1 1 d D H . O17 O 0.89186(10) 0.22705(5) 0.55152(5) 0.0464(3) Uani 1 1 d . . . O18 O 0.87407(10) 0.15199(5) 0.58267(6) 0.0477(3) Uani 1 1 d . . . O19 O 0.77562(13) 0.21116(6) 0.61207(6) 0.0619(4) Uani 1 1 d . . . O20 O 0.74584(10) 0.18464(5) 0.52996(5) 0.0536(4) Uani 1 1 d . . . O21 O 0.72258(13) 0.46607(6) 0.38625(6) 0.0673(5) Uani 1 1 d . . . O22 O 0.62518(10) 0.40410(5) 0.41010(6) 0.0486(4) Uani 1 1 d . . . O23 O 0.61072(10) 0.47535(5) 0.45035(5) 0.0507(4) Uani 1 1 d . . . O24 O 0.75719(11) 0.43172(6) 0.46433(5) 0.0594(4) Uani 1 1 d . . . O25 O 0.73951(10) 0.12045(5) 0.19703(4) 0.0299(3) Uani 0.875 1 d P A 1 O26 O 0.71012(10) 0.16322(4) 0.27063(5) 0.0328(3) Uani 0.875 1 d P A 1 O27 O 0.87297(10) 0.13826(5) 0.25587(5) 0.0328(3) Uani 0.875 1 d P A 1 O28 O 0.75138(12) 0.08398(5) 0.27704(5) 0.0398(3) Uani 0.875 1 d P A 1 O29 O 0.47893(10) 0.36589(5) 0.22126(5) 0.0484(3) Uani 1 1 d . B . O30 O 0.53674(8) 0.37411(4) 0.30659(4) 0.0340(3) Uani 1 1 d . B . O31 O 0.64875(9) 0.37870(8) 0.24349(5) 0.0774(6) Uani 1 1 d . B . O32 O 0.5544(3) 0.43715(16) 0.25167(18) 0.0415(9) Uani 0.50 1 d P B 1 O33 O 0.25846(10) 0.32828(5) 0.45013(5) 0.0503(4) Uani 1 1 d . . . O34 O 0.22428(11) 0.28204(5) 0.37831(5) 0.0448(3) Uani 1 1 d . . . O35 O 0.11907(9) 0.27886(4) 0.44604(4) 0.0337(3) Uani 1 1 d . . . O36 O 0.11974(8) 0.34486(4) 0.39373(4) 0.0310(2) Uani 1 1 d . . . O37 O 0.25381(12) 0.16614(5) 0.27486(5) 0.0394(3) Uani 0.875 1 d P C 1 O38 O 0.21150(10) 0.08685(5) 0.27162(5) 0.0345(3) Uani 0.875 1 d P C 1 O39 O 0.24160(10) 0.12746(5) 0.19635(4) 0.0305(3) Uani 0.875 1 d P C 1 O40 O 0.37484(10) 0.11055(5) 0.25569(5) 0.0343(3) Uani 0.875 1 d P C 1 O1W O 0.29789(8) 0.07081(4) 0.72070(4) 0.0312(2) Uani 1 1 d D . . O2W O 0.20093(9) 0.31757(4) 0.27483(4) 0.0319(2) Uani 1 1 d D . . O3W O 0.3381(6) 0.0182(3) 0.1941(3) 0.0908(18) Uiso 0.25 1 d P D 2 O4W O 0.8392(6) 0.2307(3) 0.1911(3) 0.0908(18) Uiso 0.25 1 d P E 3 Cl1 Cl 0.32020(3) 0.060250(13) 0.578770(12) 0.02289(7) Uani 1 1 d . . . Cl2 Cl 0.95135(3) 0.139187(13) 0.737866(12) 0.02441(7) Uani 1 1 d . . . Cl3 Cl 0.82241(3) 0.193871(12) 0.569142(13) 0.02374(7) Uani 1 1 d . . . Cl4 Cl 0.67848(3) 0.444373(13) 0.427767(13) 0.02468(7) Uani 1 1 d . . . Cl5 Cl 0.76892(8) 0.12631(5) 0.25015(5) 0.02256(18) Uani 0.875 1 d P A 1 Cl6 Cl 0.54917(3) 0.388554(13) 0.255907(12) 0.02465(7) Uani 1 1 d . . . Cl7 Cl 0.18040(2) 0.308492(12) 0.417569(12) 0.02215(7) Uani 1 1 d . . . Cl8 Cl 0.27071(5) 0.12274(3) 0.24964(3) 0.02206(13) Uani 0.875 1 d P C 1 Cl5A Cl 0.7415(6) 0.1318(4) 0.2478(4) 0.0310(17) Uani 0.125 1 d P F 2 O25A O 0.6363(9) 0.1201(4) 0.2408(4) 0.0534(11) Uiso 0.125 1 d P F 2 O26A O 0.7920(9) 0.0969(4) 0.2220(5) 0.0534(11) Uiso 0.125 1 d P F 2 O27A O 0.7646(9) 0.1350(4) 0.3020(4) 0.0534(11) Uiso 0.125 1 d P F 2 O28A O 0.7592(9) 0.1760(4) 0.2230(4) 0.0534(11) Uiso 0.125 1 d P F 2 O37A O 0.2607(9) 0.1155(4) 0.3036(4) 0.0534(11) Uiso 0.125 1 d P G 2 Cl8A Cl 0.2363(4) 0.1192(3) 0.2501(3) 0.0371(14) Uani 0.125 1 d P G 2 O38A O 0.1359(9) 0.1304(4) 0.2416(4) 0.0534(11) Uiso 0.125 1 d P G 2 O39A O 0.2549(9) 0.0724(4) 0.2260(4) 0.0534(11) Uiso 0.125 1 d P G 2 O40A O 0.2948(9) 0.1521(4) 0.2259(5) 0.0534(11) Uiso 0.125 1 d P G 2 O14A O 0.9723(6) 0.1865(2) 0.7375(6) 0.076(3) Uani 0.50 1 d PD H 2 O32A O 0.5096(2) 0.43669(16) 0.25121(16) 0.0371(9) Uani 0.50 1 d P B 2 Co1 Co 0.278310(13) 0.235794(6) 0.638181(6) 0.01412(4) Uani 1 1 d . . . Co2 Co 0.768997(13) 0.021002(6) 0.636867(6) 0.01342(4) Uani 1 1 d . . . Co3 Co 0.732267(13) 0.271890(6) 0.358205(6) 0.01362(4) Uani 1 1 d . . . Co4 Co 0.223552(13) 0.483823(6) 0.356655(6) 0.01438(4) Uani 1 1 d . . . H1N H 0.2796(12) 0.3216(4) 0.6325(4) 0.022 Uiso 1 1 d D . . H2N H 0.3285(7) 0.3010(6) 0.5912(5) 0.022 Uiso 1 1 d D . . H3N H 0.2567(10) 0.2776(4) 0.7171(5) 0.022 Uiso 1 1 d D . . H4N H 0.2119(12) 0.2323(4) 0.7216(5) 0.022 Uiso 1 1 d D . . H5N H 0.2885(11) 0.1647(5) 0.69100(15) 0.022 Uiso 1 1 d D . . H6N H 0.3193(9) 0.1539(5) 0.6415(5) 0.022 Uiso 1 1 d D . . H7N H 0.7607(12) 0.0967(5) 0.67947(17) 0.022 Uiso 1 1 d D . . H8N H 0.8033(8) 0.1020(5) 0.6304(5) 0.022 Uiso 1 1 d D . . H9N H 0.8299(7) -0.0485(6) 0.5993(5) 0.022 Uiso 1 1 d D . . H10N H 0.7820(12) -0.0648(4) 0.6429(4) 0.022 Uiso 1 1 d D . . H11N H 0.7434(10) -0.0130(4) 0.7191(5) 0.022 Uiso 1 1 d D . . H12N H 0.6961(12) 0.0326(3) 0.7174(5) 0.022 Uiso 1 1 d D . . H13N H 0.8056(12) 0.2825(3) 0.2771(5) 0.022 Uiso 1 1 d D . . H14N H 0.7566(10) 0.2369(4) 0.2772(5) 0.022 Uiso 1 1 d D . . H15N H 0.6965(8) 0.3531(5) 0.3633(5) 0.022 Uiso 1 1 d D . . H16N H 0.7392(12) 0.3481(5) 0.31505(18) 0.022 Uiso 1 1 d D . . H17N H 0.7181(12) 0.1865(4) 0.3531(4) 0.022 Uiso 1 1 d D . . H18N H 0.6733(7) 0.2028(6) 0.3975(5) 0.022 Uiso 1 1 d D . . H19N H 0.1814(9) 0.4026(5) 0.3541(5) 0.022 Uiso 1 1 d D . . H20N H 0.2123(11) 0.4138(5) 0.30322(13) 0.022 Uiso 1 1 d D . . H21N H 0.1768(7) 0.5492(6) 0.4056(5) 0.022 Uiso 1 1 d D . . H22N H 0.2234(12) 0.5696(4) 0.3632(4) 0.022 Uiso 1 1 d D . . H23N H 0.2878(12) 0.4796(4) 0.2737(5) 0.022 Uiso 1 1 d D . . H24N H 0.2441(10) 0.5250(4) 0.2783(5) 0.022 Uiso 1 1 d D . . H1W H 0.2918(12) 0.0581(5) 0.6896(2) 0.022 Uiso 1 1 d D . . H2W H 0.3592(5) 0.0836(5) 0.7210(6) 0.022 Uiso 1 1 d D . . H3W H 0.2096(12) 0.3070(5) 0.3068(2) 0.022 Uiso 1 1 d D . . H4W H 0.1386(5) 0.3294(5) 0.2718(6) 0.022 Uiso 1 1 d 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 0.0193(7) 0.0265(7) 0.0170(6) 0.0010(5) -0.0005(5) 0.0037(6) C2 0.0294(8) 0.0232(7) 0.0216(6) 0.0058(5) 0.0020(5) 0.0045(6) C3 0.0168(6) 0.0240(7) 0.0200(6) -0.0036(5) 0.0042(5) 0.0012(6) C4 0.0221(7) 0.0222(7) 0.0211(6) -0.0048(5) 0.0046(5) 0.0014(6) C5 0.0175(7) 0.0190(6) 0.0250(6) -0.0067(5) 0.0012(5) -0.0019(5) C6 0.0197(7) 0.0190(7) 0.0302(7) -0.0007(5) 0.0050(5) -0.0032(6) C7 0.0187(7) 0.0371(8) 0.0200(6) -0.0003(6) -0.0031(5) -0.0043(6) C8 0.0175(6) 0.0198(6) 0.0174(6) 0.0027(5) 0.0000(5) -0.0040(5) C9 0.0145(6) 0.0230(7) 0.0177(6) 0.0005(5) 0.0013(5) -0.0007(5) C10 0.0166(6) 0.0149(6) 0.0155(5) 0.0011(4) 0.0023(4) -0.0005(5) C11 0.0149(6) 0.0166(6) 0.0158(5) 0.0021(4) 0.0017(4) -0.0013(5) C12 0.0171(6) 0.0197(6) 0.0152(5) 0.0013(5) 0.0005(4) 0.0025(5) C13 0.0178(7) 0.0166(6) 0.0180(6) 0.0011(5) 0.0023(5) -0.0015(5) C14 0.0224(7) 0.0235(7) 0.0225(6) 0.0008(5) 0.0042(5) 0.0034(6) C15 0.0271(8) 0.0241(7) 0.0286(7) -0.0037(6) 0.0076(6) 0.0015(6) C16 0.0284(8) 0.0256(7) 0.0201(6) -0.0061(5) 0.0075(5) -0.0067(6) C17 0.0244(7) 0.0246(7) 0.0172(6) -0.0012(5) 0.0018(5) -0.0061(6) C18 0.0182(7) 0.0182(6) 0.0158(5) 0.0007(5) 0.0021(5) -0.0040(5) C19 0.0186(7) 0.0250(7) 0.0171(6) 0.0027(5) -0.0003(5) 0.0007(6) C20 0.0173(7) 0.0216(7) 0.0183(6) 0.0025(5) 0.0015(5) 0.0032(5) C21 0.0156(6) 0.0214(6) 0.0200(6) 0.0079(5) 0.0008(5) 0.0010(5) C22 0.0188(7) 0.0177(6) 0.0291(7) 0.0028(5) 0.0013(5) 0.0029(5) C23 0.0197(7) 0.0281(7) 0.0179(6) -0.0053(5) 0.0002(5) -0.0060(6) C24 0.0263(8) 0.0227(7) 0.0283(7) -0.0085(6) 0.0048(6) -0.0052(6) C25 0.0146(6) 0.0235(7) 0.0188(6) 0.0037(5) 0.0047(5) -0.0006(5) C26 0.0178(7) 0.0231(7) 0.0202(6) 0.0051(5) 0.0046(5) 0.0011(5) C27 0.0160(7) 0.0371(8) 0.0188(6) -0.0002(5) -0.0025(5) 0.0040(6) C28 0.0148(6) 0.0190(6) 0.0174(6) -0.0024(5) -0.0002(4) 0.0033(5) C29 0.0138(6) 0.0234(7) 0.0169(6) -0.0015(5) 0.0017(4) 0.0011(5) C30 0.0149(6) 0.0143(6) 0.0153(5) -0.0013(4) 0.0027(4) 0.0006(5) C31 0.0146(6) 0.0167(6) 0.0151(5) -0.0016(4) 0.0019(4) 0.0007(5) C32 0.0168(6) 0.0205(6) 0.0162(6) -0.0014(5) 0.0020(5) -0.0016(5) C33 0.0161(6) 0.0179(6) 0.0191(6) -0.0004(5) 0.0042(5) 0.0007(5) C34 0.0237(7) 0.0236(7) 0.0257(7) 0.0010(5) 0.0049(5) -0.0054(6) C35 0.0251(8) 0.0266(8) 0.0317(7) 0.0078(6) 0.0100(6) 0.0000(6) C36 0.0267(8) 0.0274(7) 0.0228(6) 0.0088(6) 0.0093(5) 0.0079(6) C37 0.0241(7) 0.0239(7) 0.0184(6) 0.0019(5) 0.0032(5) 0.0062(6) C38 0.0185(7) 0.0171(6) 0.0170(6) 0.0001(5) 0.0033(5) 0.0040(5) C39 0.0196(7) 0.0232(7) 0.0168(6) -0.0029(5) 0.0002(5) -0.0002(6) C40 0.0169(7) 0.0213(7) 0.0173(6) -0.0025(5) 0.0021(5) -0.0024(5) C41 0.0135(6) 0.0231(7) 0.0217(6) -0.0041(5) 0.0044(5) 0.0001(5) C42 0.0189(7) 0.0220(7) 0.0222(6) -0.0069(5) 0.0059(5) -0.0009(5) C43 0.0153(6) 0.0219(7) 0.0200(6) -0.0072(5) 0.0010(5) -0.0015(5) C44 0.0198(7) 0.0167(6) 0.0284(7) -0.0030(5) 0.0022(5) -0.0031(5) C45 0.0206(7) 0.0274(7) 0.0199(6) 0.0059(5) 0.0017(5) 0.0047(6) C46 0.0271(8) 0.0219(7) 0.0313(7) 0.0082(6) 0.0057(6) 0.0060(6) C47 0.0160(7) 0.0374(8) 0.0202(6) 0.0004(6) -0.0019(5) -0.0052(6) C48 0.0151(6) 0.0193(6) 0.0188(6) 0.0027(5) 0.0005(5) -0.0032(5) C49 0.0139(6) 0.0235(7) 0.0180(6) 0.0008(5) 0.0023(5) -0.0025(5) C50 0.0147(6) 0.0145(6) 0.0173(6) 0.0019(4) 0.0034(4) -0.0002(5) C51 0.0141(6) 0.0174(6) 0.0155(5) 0.0011(4) 0.0025(4) -0.0007(5) C52 0.0181(7) 0.0204(6) 0.0158(6) 0.0017(5) 0.0020(5) 0.0028(5) C53 0.0189(7) 0.0172(6) 0.0189(6) 0.0013(5) 0.0042(5) -0.0014(5) C54 0.0249(8) 0.0268(7) 0.0247(7) 0.0006(6) 0.0059(5) 0.0057(6) C55 0.0305(8) 0.0260(7) 0.0302(7) -0.0062(6) 0.0107(6) 0.0021(7) C56 0.0293(8) 0.0294(8) 0.0224(7) -0.0082(6) 0.0092(6) -0.0110(7) C57 0.0258(8) 0.0270(7) 0.0182(6) -0.0022(5) 0.0040(5) -0.0079(6) C58 0.0184(7) 0.0195(6) 0.0177(6) 0.0009(5) 0.0022(5) -0.0050(5) C59 0.0200(7) 0.0278(7) 0.0164(6) 0.0027(5) 0.0008(5) -0.0001(6) C60 0.0171(7) 0.0247(7) 0.0193(6) 0.0036(5) 0.0023(5) 0.0035(6) C61 0.0187(7) 0.0187(6) 0.0259(7) 0.0064(5) 0.0029(5) 0.0018(5) C62 0.0213(7) 0.0173(6) 0.0300(7) 0.0008(5) 0.0056(5) 0.0035(5) C63 0.0197(7) 0.0271(7) 0.0180(6) -0.0024(5) -0.0001(5) -0.0038(6) C64 0.0301(8) 0.0218(7) 0.0244(7) -0.0048(5) 0.0036(6) -0.0055(6) C65 0.0169(7) 0.0243(7) 0.0236(6) 0.0049(5) 0.0051(5) -0.0002(6) C66 0.0210(7) 0.0226(7) 0.0231(6) 0.0047(5) 0.0065(5) -0.0018(6) C67 0.0187(7) 0.0388(9) 0.0216(7) 0.0006(6) -0.0023(5) 0.0045(6) C68 0.0164(6) 0.0214(6) 0.0183(6) -0.0018(5) -0.0008(5) 0.0036(5) C69 0.0150(6) 0.0229(7) 0.0191(6) -0.0006(5) 0.0024(5) -0.0002(5) C70 0.0162(6) 0.0144(6) 0.0169(5) -0.0016(4) 0.0024(4) -0.0001(5) C71 0.0160(6) 0.0171(6) 0.0155(5) -0.0022(4) 0.0032(4) 0.0007(5) C72 0.0182(7) 0.0193(6) 0.0163(6) -0.0010(5) 0.0007(5) -0.0014(5) C73 0.0187(7) 0.0178(6) 0.0176(6) -0.0010(5) 0.0040(5) 0.0010(5) C74 0.0255(8) 0.0246(7) 0.0228(6) -0.0014(5) 0.0059(5) -0.0054(6) C75 0.0313(9) 0.0244(7) 0.0276(7) 0.0045(6) 0.0111(6) 0.0001(7) C76 0.0286(8) 0.0284(8) 0.0218(6) 0.0065(6) 0.0087(5) 0.0097(7) C77 0.0246(8) 0.0296(8) 0.0173(6) 0.0006(5) 0.0026(5) 0.0085(6) C78 0.0196(7) 0.0197(6) 0.0172(6) -0.0015(5) 0.0020(5) 0.0043(5) C79 0.0195(7) 0.0297(7) 0.0179(6) -0.0038(5) -0.0001(5) 0.0001(6) C80 0.0168(7) 0.0272(7) 0.0189(6) -0.0049(5) 0.0017(5) -0.0038(6) N1 0.0150(5) 0.0186(5) 0.0156(5) -0.0023(4) 0.0014(4) 0.0001(4) N2 0.0248(6) 0.0168(5) 0.0214(5) 0.0008(4) 0.0037(5) -0.0017(5) N3 0.0213(6) 0.0202(6) 0.0157(5) -0.0028(4) 0.0017(4) -0.0015(5) N4 0.0190(6) 0.0179(5) 0.0187(5) 0.0016(4) 0.0026(4) 0.0009(5) N5 0.0143(5) 0.0190(5) 0.0137(5) 0.0013(4) 0.0013(4) -0.0012(4) N6 0.0174(6) 0.0172(5) 0.0195(5) -0.0009(4) 0.0015(4) -0.0002(4) N7 0.0214(6) 0.0183(6) 0.0232(6) -0.0001(4) 0.0052(5) 0.0021(5) N8 0.0186(6) 0.0233(6) 0.0149(5) 0.0035(4) 0.0024(4) 0.0025(5) N9 0.0133(5) 0.0181(5) 0.0157(5) -0.0017(4) 0.0017(4) 0.0011(4) N10 0.0179(6) 0.0231(6) 0.0169(5) -0.0035(4) 0.0027(4) -0.0030(5) N11 0.0175(6) 0.0172(5) 0.0194(5) 0.0016(4) 0.0017(4) 0.0000(4) N12 0.0230(6) 0.0160(5) 0.0247(6) -0.0002(4) 0.0062(5) -0.0019(5) N13 0.0150(5) 0.0188(5) 0.0171(5) 0.0029(4) 0.0018(4) -0.0006(4) N14 0.0209(6) 0.0172(5) 0.0189(5) -0.0005(4) 0.0028(4) -0.0009(5) N15 0.0260(7) 0.0174(6) 0.0213(6) -0.0004(4) 0.0054(5) 0.0013(5) N16 0.0217(6) 0.0191(6) 0.0175(5) 0.0030(4) 0.0031(4) 0.0018(5) O1 0.0174(5) 0.0267(5) 0.0159(4) -0.0024(4) 0.0003(3) -0.0031(4) O2 0.0142(5) 0.0234(5) 0.0154(4) -0.0016(3) 0.0018(3) 0.0004(4) O3 0.0137(4) 0.0261(5) 0.0157(4) 0.0022(4) 0.0002(3) 0.0023(4) O4 0.0126(4) 0.0240(5) 0.0145(4) 0.0011(3) 0.0020(3) -0.0016(4) O5 0.0146(5) 0.0268(5) 0.0162(4) -0.0022(4) 0.0009(3) -0.0022(4) O6 0.0141(5) 0.0222(5) 0.0151(4) -0.0012(3) 0.0025(3) 0.0020(4) O7 0.0170(5) 0.0258(5) 0.0178(4) 0.0034(4) 0.0009(3) 0.0028(4) O8 0.0138(5) 0.0221(5) 0.0170(4) 0.0016(3) 0.0030(3) -0.0004(4) O9 0.0355(7) 0.0785(11) 0.0472(8) 0.0016(7) -0.0145(6) 0.0220(7) O10 0.0294(6) 0.0469(7) 0.0299(6) -0.0201(5) -0.0010(5) 0.0085(5) O11 0.0233(6) 0.0291(6) 0.0443(6) -0.0124(5) 0.0061(5) -0.0034(5) O12 0.0548(9) 0.0493(8) 0.0355(7) -0.0098(6) 0.0183(6) -0.0264(7) O13 0.0285(6) 0.0457(7) 0.0279(5) -0.0168(5) 0.0084(4) -0.0074(5) O14 0.166(6) 0.031(3) 0.032(5) -0.0209(19) -0.007(4) 0.014(3) O15 0.0417(7) 0.0574(9) 0.0426(7) -0.0001(6) -0.0133(6) 0.0083(7) O16 0.0176(6) 0.194(2) 0.0316(7) -0.0110(10) 0.0094(5) -0.0150(9) O17 0.0402(7) 0.0545(8) 0.0431(7) 0.0219(6) -0.0081(6) -0.0255(6) O18 0.0333(7) 0.0373(7) 0.0734(9) 0.0202(6) 0.0113(6) 0.0131(6) O19 0.0646(11) 0.0646(10) 0.0600(9) -0.0163(8) 0.0304(8) 0.0080(8) O20 0.0349(7) 0.0725(10) 0.0510(8) 0.0121(7) -0.0164(6) -0.0207(7) O21 0.0702(11) 0.0701(11) 0.0644(10) 0.0152(8) 0.0264(8) -0.0226(9) O22 0.0318(7) 0.0374(7) 0.0777(10) -0.0236(7) 0.0117(6) -0.0110(6) O23 0.0425(8) 0.0599(9) 0.0485(8) -0.0279(7) -0.0072(6) 0.0258(7) O24 0.0362(8) 0.0921(12) 0.0479(8) -0.0100(8) -0.0129(6) 0.0270(8) O25 0.0326(7) 0.0374(7) 0.0190(5) -0.0083(5) -0.0036(5) -0.0025(6) O26 0.0357(7) 0.0259(6) 0.0381(7) -0.0143(5) 0.0129(6) -0.0025(6) O27 0.0258(7) 0.0458(8) 0.0266(6) -0.0113(6) -0.0009(5) -0.0032(6) O28 0.0650(10) 0.0244(7) 0.0302(7) -0.0010(5) 0.0054(6) -0.0076(7) O29 0.0400(7) 0.0575(9) 0.0455(7) -0.0053(6) -0.0152(6) -0.0047(7) O30 0.0280(6) 0.0460(7) 0.0291(5) 0.0171(5) 0.0096(4) 0.0082(5) O31 0.0176(6) 0.186(2) 0.0297(7) 0.0095(9) 0.0091(5) 0.0150(9) O32 0.040(2) 0.0336(16) 0.0504(17) 0.0187(12) 0.0013(19) -0.007(2) O33 0.0328(7) 0.0733(10) 0.0432(7) 0.0047(7) -0.0114(6) -0.0240(7) O34 0.0550(9) 0.0469(8) 0.0342(6) 0.0060(6) 0.0158(6) 0.0240(7) O35 0.0295(6) 0.0430(7) 0.0284(5) 0.0159(5) -0.0001(4) -0.0091(5) O36 0.0231(6) 0.0277(6) 0.0427(6) 0.0112(5) 0.0052(5) 0.0043(5) O37 0.0634(10) 0.0243(6) 0.0303(7) 0.0008(5) 0.0021(6) 0.0047(7) O38 0.0353(7) 0.0274(7) 0.0421(7) 0.0150(6) 0.0141(6) 0.0015(6) O39 0.0310(7) 0.0383(7) 0.0214(6) 0.0070(5) -0.0041(5) 0.0033(6) O40 0.0250(7) 0.0501(8) 0.0274(6) 0.0116(6) -0.0024(5) 0.0030(6) O1W 0.0307(6) 0.0394(6) 0.0230(5) 0.0050(5) -0.0026(4) -0.0102(5) O2W 0.0321(6) 0.0395(6) 0.0234(5) -0.0046(5) -0.0035(4) 0.0100(5) Cl1 0.01634(16) 0.03116(18) 0.02109(15) -0.00515(13) 0.00057(11) 0.00116(14) Cl2 0.02092(16) 0.03144(18) 0.02145(15) -0.00395(13) 0.00593(12) -0.00100(14) Cl3 0.01965(17) 0.02579(17) 0.02576(16) 0.00623(13) 0.00121(12) -0.00086(14) Cl4 0.02042(17) 0.02759(17) 0.02592(16) -0.00673(13) 0.00067(12) 0.00151(14) Cl5 0.0294(5) 0.0212(4) 0.0173(3) -0.0073(2) 0.0026(3) -0.0021(3) Cl6 0.02112(16) 0.03158(18) 0.02187(15) 0.00338(13) 0.00615(12) 0.00111(14) Cl7 0.01671(16) 0.02891(17) 0.02070(14) 0.00462(12) 0.00033(11) -0.00113(13) Cl8 0.0270(3) 0.0217(3) 0.0174(2) 0.00713(16) 0.0011(3) 0.0025(3) Cl5A 0.041(5) 0.024(3) 0.028(2) 0.0013(17) 0.003(3) -0.002(3) Cl8A 0.036(3) 0.044(3) 0.030(2) 0.0013(16) 0.000(3) -0.003(3) O14A 0.174(7) 0.027(2) 0.030(4) -0.016(2) 0.022(3) -0.019(4) O32A 0.039(2) 0.0267(16) 0.0456(17) 0.0110(11) 0.004(2) 0.0108(18) Co1 0.01397(9) 0.01513(8) 0.01333(8) -0.00072(6) 0.00148(6) -0.00126(7) Co2 0.01236(9) 0.01569(8) 0.01228(8) 0.00076(6) 0.00140(6) 0.00060(7) Co3 0.01209(8) 0.01512(8) 0.01379(8) -0.00105(6) 0.00188(6) -0.00085(7) Co4 0.01451(9) 0.01477(8) 0.01400(8) 0.00125(6) 0.00202(6) 0.00103(7) _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 N1 1.4929(17) . ? C1 C2 1.517(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N2 1.5067(19) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N1 1.5166(17) . ? C3 C4 1.5197(19) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N3 1.4859(18) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 N1 1.4947(17) . ? C5 C6 1.5209(19) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N4 1.4905(18) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.5034(18) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 O1 1.2792(16) . ? C8 C9 1.4037(18) . ? C9 C10 1.3921(17) . ? C9 H9 0.9500 . ? C10 O2 1.2938(16) . ? C10 C11 1.4875(17) . ? C11 C12 1.3766(18) . ? C11 C20 1.4284(17) . ? C12 C13 1.4210(17) . ? C12 H12 0.9500 . ? C13 C14 1.4185(19) . ? C13 C18 1.4203(18) . ? C14 C15 1.3782(19) . ? C14 H14 0.9500 . ? C15 C16 1.414(2) . ? C15 H15 0.9500 . ? C16 C17 1.370(2) . ? C16 H16 0.9500 . ? C17 C18 1.4180(17) . ? C17 H17 0.9500 . ? C18 C19 1.4212(19) . ? C19 C20 1.3681(18) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 N5 1.4972(16) . ? C21 C22 1.5120(19) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 N6 1.4964(17) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 N5 1.4936(17) . ? C23 C24 1.518(2) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 N7 1.5054(19) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 N5 1.5082(16) . ? C25 C26 1.5158(18) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 N8 1.4850(18) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.5024(18) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 O3 1.2759(16) . ? C28 C29 1.4053(18) . ? C29 C30 1.3908(17) . ? C29 H29 0.9500 . ? C30 O4 1.2899(15) . ? C30 C31 1.4892(17) . ? C31 C32 1.3741(18) . ? C31 C40 1.4220(17) . ? C32 C33 1.4245(17) . ? C32 H32 0.9500 . ? C33 C34 1.4202(19) . ? C33 C38 1.4208(18) . ? C34 C35 1.3719(19) . ? C34 H34 0.9500 . ? C35 C36 1.409(2) . ? C35 H35 0.9500 . ? C36 C37 1.372(2) . ? C36 H36 0.9500 . ? C37 C38 1.4193(18) . ? C37 H37 0.9500 . ? C38 C39 1.4225(19) . ? C39 C40 1.3672(18) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 N9 1.5113(17) . ? C41 C42 1.5162(18) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 N10 1.4849(18) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 N9 1.4973(16) . ? C43 C44 1.5137(19) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 N11 1.4964(17) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 N9 1.4946(17) . ? C45 C46 1.514(2) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 N12 1.5030(19) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.5045(18) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 O5 1.2797(16) . ? C48 C49 1.4019(18) . ? C49 C50 1.3900(18) . ? C49 H49 0.9500 . ? C50 O6 1.2937(15) . ? C50 C51 1.4830(17) . ? C51 C52 1.3745(18) . ? C51 C60 1.4244(18) . ? C52 C53 1.4199(17) . ? C52 H52 0.9500 . ? C53 C54 1.419(2) . ? C53 C58 1.4222(18) . ? C54 C55 1.377(2) . ? C54 H54 0.9500 . ? C55 C56 1.413(2) . ? C55 H55 0.9500 . ? C56 C57 1.368(2) . ? C56 H56 0.9500 . ? C57 C58 1.4162(18) . ? C57 H57 0.9500 . ? C58 C59 1.418(2) . ? C59 C60 1.3700(18) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 N13 1.4944(17) . ? C61 C62 1.5167(19) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 N14 1.4916(18) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 N13 1.4977(17) . ? C63 C64 1.518(2) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 N15 1.5086(19) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 N13 1.5096(17) . ? C65 C66 1.5196(19) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 N16 1.4845(18) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.5038(19) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 O7 1.2789(17) . ? C68 C69 1.4027(18) . ? C69 C70 1.3964(18) . ? C69 H69 0.9500 . ? C70 O8 1.2873(16) . ? C70 C71 1.4868(17) . ? C71 C72 1.3761(18) . ? C71 C80 1.4237(18) . ? C72 C73 1.4217(17) . ? C72 H72 0.9500 . ? C73 C74 1.4204(19) . ? C73 C78 1.4218(18) . ? C74 C75 1.3718(19) . ? C74 H74 0.9500 . ? C75 C76 1.414(2) . ? C75 H75 0.9500 . ? C76 C77 1.370(2) . ? C76 H76 0.9500 . ? C77 C78 1.4195(18) . ? C77 H77 0.9500 . ? C78 C79 1.418(2) . ? C79 C80 1.3656(19) . ? C79 H79 0.9500 . ? C80 H80 0.9500 . ? N1 Co1 1.9501(11) . ? N2 Co1 1.9618(12) . ? N2 H1N 0.9000(10) . ? N2 H2N 0.8999(10) . ? N3 Co1 1.9379(11) . ? N3 H3N 0.8998(10) . ? N3 H4N 0.8999(10) . ? N4 Co1 1.9509(12) . ? N4 H5N 0.9000(10) . ? N4 H6N 0.8999(10) . ? N5 Co2 1.9461(11) . ? N6 Co2 1.9557(12) . ? N6 H7N 0.8999(10) . ? N6 H8N 0.8998(10) . ? N7 Co2 1.9655(12) . ? N7 H9N 0.9000(10) . ? N7 H10N 0.8999(10) . ? N8 Co2 1.9467(11) . ? N8 H11N 0.9001(10) . ? N8 H12N 0.8998(10) . ? N9 Co3 1.9467(11) . ? N10 Co3 1.9478(11) . ? N10 H13N 0.8997(10) . ? N10 H14N 0.9000(10) . ? N11 Co3 1.9562(12) . ? N11 H15N 0.8999(10) . ? N11 H16N 0.9000(10) . ? N12 Co3 1.9662(12) . ? N12 H17N 0.9000(10) . ? N12 H18N 0.9000(10) . ? N13 Co4 1.9484(11) . ? N14 Co4 1.9516(11) . ? N14 H19N 0.9000(10) . ? N14 H20N 0.8998(10) . ? N15 Co4 1.9595(12) . ? N15 H21N 0.8999(10) . ? N15 H22N 0.8998(10) . ? N16 Co4 1.9395(11) . ? N16 H23N 0.8999(10) . ? N16 H24N 0.8998(10) . ? O1 Co1 1.8902(10) . ? O2 Co1 1.8918(9) . ? O3 Co2 1.8851(9) . ? O4 Co2 1.8909(9) . ? O5 Co3 1.8841(9) . ? O6 Co3 1.8876(9) . ? O7 Co4 1.8907(10) . ? O8 Co4 1.8904(9) . ? O9 Cl1 1.4274(12) . ? O10 Cl1 1.4310(11) . ? O11 Cl1 1.4453(11) . ? O12 Cl1 1.4363(12) . ? O13 Cl2 1.4265(10) . ? O14 Cl2 1.462(8) . ? O15 Cl2 1.4215(13) . ? O16 Cl2 1.4152(13) . ? O17 Cl3 1.4313(12) . ? O18 Cl3 1.4231(12) . ? O19 Cl3 1.4209(14) . ? O20 Cl3 1.4351(12) . ? O21 Cl4 1.4233(15) . ? O22 Cl4 1.4236(12) . ? O23 Cl4 1.4295(13) . ? O24 Cl4 1.4310(13) . ? O25 Cl5 1.4440(17) . ? O26 Cl5 1.4473(16) . ? O27 Cl5 1.4343(18) . ? O28 Cl5 1.436(2) . ? O29 Cl6 1.4278(13) . ? O30 Cl6 1.4227(10) . ? O31 Cl6 1.4227(13) . ? O32 Cl6 1.404(5) . ? O33 Cl7 1.4293(12) . ? O34 Cl7 1.4420(12) . ? O35 Cl7 1.4307(11) . ? O36 Cl7 1.4442(11) . ? O37 Cl8 1.4395(16) . ? O38 Cl8 1.4462(14) . ? O39 Cl8 1.4436(14) . ? O40 Cl8 1.4374(14) . ? O1W H1W 0.8997(10) . ? O1W H2W 0.8996(10) . ? O2W H3W 0.8998(10) . ? O2W H4W 0.8997(10) . ? Cl2 O14A 1.388(6) . ? Cl6 O32A 1.485(4) . ? Cl5A O26A 1.410(15) . ? Cl5A O25A 1.449(15) . ? Cl5A O27A 1.450(16) . ? Cl5A O28A 1.455(17) . ? O37A Cl8A 1.433(14) . ? Cl8A O38A 1.388(13) . ? Cl8A O40A 1.407(13) . ? Cl8A O39A 1.516(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 108.07(10) . . ? N1 C1 H1A 110.1 . . ? C2 C1 H1A 110.1 . . ? N1 C1 H1B 110.1 . . ? C2 C1 H1B 110.1 . . ? H1A C1 H1B 108.4 . . ? N2 C2 C1 109.11(11) . . ? N2 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? N2 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? N1 C3 C4 110.25(11) . . ? N1 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 . . ? N1 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? N3 C4 C3 108.32(11) . . ? N3 C4 H4A 110.0 . . ? C3 C4 H4A 110.0 . . ? N3 C4 H4B 110.0 . . ? C3 C4 H4B 110.0 . . ? H4A C4 H4B 108.4 . . ? N1 C5 C6 107.60(10) . . ? N1 C5 H5A 110.2 . . ? C6 C5 H5A 110.2 . . ? N1 C5 H5B 110.2 . . ? C6 C5 H5B 110.2 . . ? H5A C5 H5B 108.5 . . ? N4 C6 C5 108.19(11) . . ? N4 C6 H6A 110.1 . . ? C5 C6 H6A 110.1 . . ? N4 C6 H6B 110.1 . . ? C5 C6 H6B 110.1 . . ? H6A C6 H6B 108.4 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O1 C8 C9 125.52(12) . . ? O1 C8 C7 115.32(12) . . ? C9 C8 C7 119.15(13) . . ? C10 C9 C8 124.08(13) . . ? C10 C9 H9 118.0 . . ? C8 C9 H9 118.0 . . ? O2 C10 C9 124.85(12) . . ? O2 C10 C11 114.01(11) . . ? C9 C10 C11 121.12(12) . . ? C12 C11 C20 119.49(12) . . ? C12 C11 C10 121.82(11) . . ? C20 C11 C10 118.68(12) . . ? C11 C12 C13 121.13(12) . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? C14 C13 C18 118.97(12) . . ? C14 C13 C12 122.00(12) . . ? C18 C13 C12 119.03(12) . . ? C15 C14 C13 120.70(13) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 120.01(14) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C17 C16 C15 120.46(13) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 120.66(13) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C17 C18 C13 119.16(13) . . ? C17 C18 C19 121.94(12) . . ? C13 C18 C19 118.90(11) . . ? C20 C19 C18 121.07(12) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C19 C20 C11 120.32(13) . . ? C19 C20 H20 119.8 . . ? C11 C20 H20 119.8 . . ? N5 C21 C22 108.04(10) . . ? N5 C21 H21A 110.1 . . ? C22 C21 H21A 110.1 . . ? N5 C21 H21B 110.1 . . ? C22 C21 H21B 110.1 . . ? H21A C21 H21B 108.4 . . ? N6 C22 C21 108.69(11) . . ? N6 C22 H22A 110.0 . . ? C21 C22 H22A 110.0 . . ? N6 C22 H22B 110.0 . . ? C21 C22 H22B 110.0 . . ? H22A C22 H22B 108.3 . . ? N5 C23 C24 108.92(11) . . ? N5 C23 H23A 109.9 . . ? C24 C23 H23A 109.9 . . ? N5 C23 H23B 109.9 . . ? C24 C23 H23B 109.9 . . ? H23A C23 H23B 108.3 . . ? N7 C24 C23 108.72(11) . . ? N7 C24 H24A 109.9 . . ? C23 C24 H24A 109.9 . . ? N7 C24 H24B 109.9 . . ? C23 C24 H24B 109.9 . . ? H24A C24 H24B 108.3 . . ? N5 C25 C26 110.14(11) . . ? N5 C25 H25A 109.6 . . ? C26 C25 H25A 109.6 . . ? N5 C25 H25B 109.6 . . ? C26 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? N8 C26 C25 107.25(11) . . ? N8 C26 H26A 110.3 . . ? C25 C26 H26A 110.3 . . ? N8 C26 H26B 110.3 . . ? C25 C26 H26B 110.3 . . ? H26A C26 H26B 108.5 . . ? C28 C27 H27A 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C28 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O3 C28 C29 125.55(12) . . ? O3 C28 C27 115.18(11) . . ? C29 C28 C27 119.27(12) . . ? C30 C29 C28 123.92(12) . . ? C30 C29 H29 118.0 . . ? C28 C29 H29 118.0 . . ? O4 C30 C29 125.15(11) . . ? O4 C30 C31 113.87(11) . . ? C29 C30 C31 120.97(12) . . ? C32 C31 C40 119.74(12) . . ? C32 C31 C30 121.39(11) . . ? C40 C31 C30 118.81(11) . . ? C31 C32 C33 120.93(12) . . ? C31 C32 H32 119.5 . . ? C33 C32 H32 119.5 . . ? C34 C33 C38 118.98(12) . . ? C34 C33 C32 122.08(12) . . ? C38 C33 C32 118.93(12) . . ? C35 C34 C33 120.56(14) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C34 C35 C36 120.46(14) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C37 C36 C35 120.31(13) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C36 C37 C38 120.66(13) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? C37 C38 C33 118.98(13) . . ? C37 C38 C39 122.06(12) . . ? C33 C38 C39 118.95(11) . . ? C40 C39 C38 120.84(12) . . ? C40 C39 H39 119.6 . . ? C38 C39 H39 119.6 . . ? C39 C40 C31 120.54(13) . . ? C39 C40 H40 119.7 . . ? C31 C40 H40 119.7 . . ? N9 C41 C42 110.11(11) . . ? N9 C41 H41A 109.6 . . ? C42 C41 H41A 109.6 . . ? N9 C41 H41B 109.6 . . ? C42 C41 H41B 109.6 . . ? H41A C41 H41B 108.2 . . ? N10 C42 C41 107.43(11) . . ? N10 C42 H42A 110.2 . . ? C41 C42 H42A 110.2 . . ? N10 C42 H42B 110.2 . . ? C41 C42 H42B 110.2 . . ? H42A C42 H42B 108.5 . . ? N9 C43 C44 108.10(10) . . ? N9 C43 H43A 110.1 . . ? C44 C43 H43A 110.1 . . ? N9 C43 H43B 110.1 . . ? C44 C43 H43B 110.1 . . ? H43A C43 H43B 108.4 . . ? N11 C44 C43 108.55(11) . . ? N11 C44 H44A 110.0 . . ? C43 C44 H44A 110.0 . . ? N11 C44 H44B 110.0 . . ? C43 C44 H44B 110.0 . . ? H44A C44 H44B 108.4 . . ? N9 C45 C46 108.64(11) . . ? N9 C45 H45A 110.0 . . ? C46 C45 H45A 110.0 . . ? N9 C45 H45B 110.0 . . ? C46 C45 H45B 110.0 . . ? H45A C45 H45B 108.3 . . ? N12 C46 C45 108.64(11) . . ? N12 C46 H46A 110.0 . . ? C45 C46 H46A 110.0 . . ? N12 C46 H46B 110.0 . . ? C45 C46 H46B 110.0 . . ? H46A C46 H46B 108.3 . . ? C48 C47 H47A 109.5 . . ? C48 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C48 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? O5 C48 C49 125.54(12) . . ? O5 C48 C47 115.13(12) . . ? C49 C48 C47 119.32(12) . . ? C50 C49 C48 124.08(13) . . ? C50 C49 H49 118.0 . . ? C48 C49 H49 118.0 . . ? O6 C50 C49 124.97(12) . . ? O6 C50 C51 113.84(11) . . ? C49 C50 C51 121.17(12) . . ? C52 C51 C60 119.81(12) . . ? C52 C51 C50 121.12(11) . . ? C60 C51 C50 119.00(12) . . ? C51 C52 C53 121.04(12) . . ? C51 C52 H52 119.5 . . ? C53 C52 H52 119.5 . . ? C54 C53 C52 121.76(12) . . ? C54 C53 C58 119.21(12) . . ? C52 C53 C58 119.02(12) . . ? C55 C54 C53 120.42(14) . . ? C55 C54 H54 119.8 . . ? C53 C54 H54 119.8 . . ? C54 C55 C56 120.13(14) . . ? C54 C55 H55 119.9 . . ? C56 C55 H55 119.9 . . ? C57 C56 C55 120.49(13) . . ? C57 C56 H56 119.8 . . ? C55 C56 H56 119.8 . . ? C56 C57 C58 120.82(13) . . ? C56 C57 H57 119.6 . . ? C58 C57 H57 119.6 . . ? C57 C58 C59 122.42(12) . . ? C57 C58 C53 118.85(13) . . ? C59 C58 C53 118.72(12) . . ? C60 C59 C58 121.34(12) . . ? C60 C59 H59 119.3 . . ? C58 C59 H59 119.3 . . ? C59 C60 C51 119.99(13) . . ? C59 C60 H60 120.0 . . ? C51 C60 H60 120.0 . . ? N13 C61 C62 107.43(10) . . ? N13 C61 H61A 110.2 . . ? C62 C61 H61A 110.2 . . ? N13 C61 H61B 110.2 . . ? C62 C61 H61B 110.2 . . ? H61A C61 H61B 108.5 . . ? N14 C62 C61 108.31(11) . . ? N14 C62 H62A 110.0 . . ? C61 C62 H62A 110.0 . . ? N14 C62 H62B 110.0 . . ? C61 C62 H62B 110.0 . . ? H62A C62 H62B 108.4 . . ? N13 C63 C64 107.75(11) . . ? N13 C63 H63A 110.2 . . ? C64 C63 H63A 110.2 . . ? N13 C63 H63B 110.2 . . ? C64 C63 H63B 110.2 . . ? H63A C63 H63B 108.5 . . ? N15 C64 C63 108.99(11) . . ? N15 C64 H64A 109.9 . . ? C63 C64 H64A 109.9 . . ? N15 C64 H64B 109.9 . . ? C63 C64 H64B 109.9 . . ? H64A C64 H64B 108.3 . . ? N13 C65 C66 110.40(11) . . ? N13 C65 H65A 109.6 . . ? C66 C65 H65A 109.6 . . ? N13 C65 H65B 109.6 . . ? C66 C65 H65B 109.6 . . ? H65A C65 H65B 108.1 . . ? N16 C66 C65 108.09(11) . . ? N16 C66 H66A 110.1 . . ? C65 C66 H66A 110.1 . . ? N16 C66 H66B 110.1 . . ? C65 C66 H66B 110.1 . . ? H66A C66 H66B 108.4 . . ? C68 C67 H67A 109.5 . . ? C68 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C68 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? O7 C68 C69 125.73(12) . . ? O7 C68 C67 115.28(12) . . ? C69 C68 C67 118.99(13) . . ? C70 C69 C68 123.84(13) . . ? C70 C69 H69 118.1 . . ? C68 C69 H69 118.1 . . ? O8 C70 C69 125.04(12) . . ? O8 C70 C71 114.21(11) . . ? C69 C70 C71 120.74(12) . . ? C72 C71 C80 119.57(12) . . ? C72 C71 C70 121.59(11) . . ? C80 C71 C70 118.83(12) . . ? C71 C72 C73 121.05(12) . . ? C71 C72 H72 119.5 . . ? C73 C72 H72 119.5 . . ? C74 C73 C72 121.85(12) . . ? C74 C73 C78 119.36(12) . . ? C72 C73 C78 118.78(12) . . ? C75 C74 C73 120.31(14) . . ? C75 C74 H74 119.8 . . ? C73 C74 H74 119.8 . . ? C74 C75 C76 120.43(14) . . ? C74 C75 H75 119.8 . . ? C76 C75 H75 119.8 . . ? C77 C76 C75 120.35(13) . . ? C77 C76 H76 119.8 . . ? C75 C76 H76 119.8 . . ? C76 C77 C78 120.76(13) . . ? C76 C77 H77 119.6 . . ? C78 C77 H77 119.6 . . ? C79 C78 C77 122.17(12) . . ? C79 C78 C73 119.08(12) . . ? C77 C78 C73 118.73(13) . . ? C80 C79 C78 120.93(12) . . ? C80 C79 H79 119.5 . . ? C78 C79 H79 119.5 . . ? C79 C80 C71 120.50(13) . . ? C79 C80 H80 119.8 . . ? C71 C80 H80 119.8 . . ? C1 N1 C5 112.90(10) . . ? C1 N1 C3 111.40(10) . . ? C5 N1 C3 109.91(11) . . ? C1 N1 Co1 106.12(8) . . ? C5 N1 Co1 105.42(8) . . ? C3 N1 Co1 110.86(8) . . ? C2 N2 Co1 110.53(9) . . ? C2 N2 H1N 109.2(10) . . ? Co1 N2 H1N 114.2(10) . . ? C2 N2 H2N 111.2(10) . . ? Co1 N2 H2N 105.8(10) . . ? H1N N2 H2N 105.8(15) . . ? C4 N3 Co1 109.95(8) . . ? C4 N3 H3N 109.0(10) . . ? Co1 N3 H3N 113.5(10) . . ? C4 N3 H4N 104.7(11) . . ? Co1 N3 H4N 112.8(10) . . ? H3N N3 H4N 106.4(14) . . ? C6 N4 Co1 109.04(8) . . ? C6 N4 H5N 108.1(10) . . ? Co1 N4 H5N 115.5(10) . . ? C6 N4 H6N 108.2(10) . . ? Co1 N4 H6N 110.4(10) . . ? H5N N4 H6N 105.4(14) . . ? C23 N5 C21 111.67(10) . . ? C23 N5 C25 111.82(10) . . ? C21 N5 C25 110.94(10) . . ? C23 N5 Co2 106.49(8) . . ? C21 N5 Co2 105.58(8) . . ? C25 N5 Co2 110.05(8) . . ? C22 N6 Co2 109.79(8) . . ? C22 N6 H7N 109.6(10) . . ? Co2 N6 H7N 113.4(10) . . ? C22 N6 H8N 108.5(10) . . ? Co2 N6 H8N 107.1(10) . . ? H7N N6 H8N 108.3(14) . . ? C24 N7 Co2 110.85(9) . . ? C24 N7 H9N 109.0(10) . . ? Co2 N7 H9N 107.7(11) . . ? C24 N7 H10N 108.7(10) . . ? Co2 N7 H10N 114.6(10) . . ? H9N N7 H10N 105.8(15) . . ? C26 N8 Co2 108.82(8) . . ? C26 N8 H11N 108.6(10) . . ? Co2 N8 H11N 111.8(11) . . ? C26 N8 H12N 108.6(11) . . ? Co2 N8 H12N 111.1(10) . . ? H11N N8 H12N 107.9(14) . . ? C45 N9 C43 111.84(10) . . ? C45 N9 C41 111.76(10) . . ? C43 N9 C41 110.81(10) . . ? C45 N9 Co3 106.58(8) . . ? C43 N9 Co3 105.50(8) . . ? C41 N9 Co3 110.06(8) . . ? C42 N10 Co3 108.97(8) . . ? C42 N10 H13N 107.1(10) . . ? Co3 N10 H13N 112.1(10) . . ? C42 N10 H14N 109.5(10) . . ? Co3 N10 H14N 109.8(11) . . ? H13N N10 H14N 109.3(14) . . ? C44 N11 Co3 109.87(8) . . ? C44 N11 H15N 108.9(10) . . ? Co3 N11 H15N 107.7(10) . . ? C44 N11 H16N 109.0(10) . . ? Co3 N11 H16N 115.1(10) . . ? H15N N11 H16N 106.0(14) . . ? C46 N12 Co3 110.84(9) . . ? C46 N12 H17N 110.3(10) . . ? Co3 N12 H17N 113.4(10) . . ? C46 N12 H18N 109.1(10) . . ? Co3 N12 H18N 107.7(11) . . ? H17N N12 H18N 105.3(14) . . ? C61 N13 C63 112.71(10) . . ? C61 N13 C65 109.95(11) . . ? C63 N13 C65 111.36(11) . . ? C61 N13 Co4 105.53(8) . . ? C63 N13 Co4 106.02(8) . . ? C65 N13 Co4 111.05(8) . . ? C62 N14 Co4 108.92(8) . . ? C62 N14 H19N 107.2(10) . . ? Co4 N14 H19N 109.2(10) . . ? C62 N14 H20N 108.1(10) . . ? Co4 N14 H20N 113.9(10) . . ? H19N N14 H20N 109.2(14) . . ? C64 N15 Co4 110.42(9) . . ? C64 N15 H21N 109.0(10) . . ? Co4 N15 H21N 107.3(11) . . ? C64 N15 H22N 109.1(10) . . ? Co4 N15 H22N 114.5(10) . . ? H21N N15 H22N 106.4(15) . . ? C66 N16 Co4 110.01(8) . . ? C66 N16 H23N 106.9(11) . . ? Co4 N16 H23N 110.7(10) . . ? C66 N16 H24N 111.4(10) . . ? Co4 N16 H24N 111.4(10) . . ? H23N N16 H24N 106.2(14) . . ? C8 O1 Co1 124.66(8) . . ? C10 O2 Co1 124.92(8) . . ? C28 O3 Co2 124.81(8) . . ? C30 O4 Co2 124.57(8) . . ? C48 O5 Co3 124.74(8) . . ? C50 O6 Co3 124.69(8) . . ? C68 O7 Co4 124.51(8) . . ? C70 O8 Co4 125.00(8) . . ? H1W O1W H2W 101.8(14) . . ? H3W O2W H4W 105.9(14) . . ? O9 Cl1 O10 110.00(8) . . ? O9 Cl1 O12 108.89(9) . . ? O10 Cl1 O12 109.85(8) . . ? O9 Cl1 O11 110.23(9) . . ? O10 Cl1 O11 109.52(7) . . ? O12 Cl1 O11 108.33(7) . . ? O14A Cl2 O16 112.2(4) . . ? O14A Cl2 O15 109.0(4) . . ? O16 Cl2 O15 110.35(10) . . ? O14A Cl2 O13 104.6(6) . . ? O16 Cl2 O13 109.65(8) . . ? O15 Cl2 O13 110.94(8) . . ? O14A Cl2 O14 10.1(12) . . ? O16 Cl2 O14 105.8(4) . . ? O15 Cl2 O14 105.3(4) . . ? O13 Cl2 O14 114.6(6) . . ? O19 Cl3 O18 109.14(9) . . ? O19 Cl3 O17 110.85(10) . . ? O18 Cl3 O17 109.26(8) . . ? O19 Cl3 O20 108.03(10) . . ? O18 Cl3 O20 109.79(9) . . ? O17 Cl3 O20 109.75(8) . . ? O21 Cl4 O22 109.15(10) . . ? O21 Cl4 O23 110.79(10) . . ? O22 Cl4 O23 108.98(8) . . ? O21 Cl4 O24 107.93(11) . . ? O22 Cl4 O24 110.31(10) . . ? O23 Cl4 O24 109.67(8) . . ? O27 Cl5 O28 109.86(11) . . ? O27 Cl5 O25 109.46(12) . . ? O28 Cl5 O25 109.83(12) . . ? O27 Cl5 O26 109.48(12) . . ? O28 Cl5 O26 109.04(12) . . ? O25 Cl5 O26 109.15(10) . . ? O32 Cl6 O31 97.31(17) . . ? O32 Cl6 O30 112.0(2) . . ? O31 Cl6 O30 109.10(8) . . ? O32 Cl6 O29 115.95(18) . . ? O31 Cl6 O29 110.51(9) . . ? O30 Cl6 O29 111.02(8) . . ? O32 Cl6 O32A 23.78(15) . . ? O31 Cl6 O32A 120.11(16) . . ? O30 Cl6 O32A 106.75(17) . . ? O29 Cl6 O32A 98.89(17) . . ? O33 Cl7 O35 110.06(7) . . ? O33 Cl7 O34 109.09(9) . . ? O35 Cl7 O34 109.80(8) . . ? O33 Cl7 O36 110.13(8) . . ? O35 Cl7 O36 109.56(7) . . ? O34 Cl7 O36 108.18(7) . . ? O40 Cl8 O37 109.89(10) . . ? O40 Cl8 O39 109.33(9) . . ? O37 Cl8 O39 109.25(9) . . ? O40 Cl8 O38 109.56(9) . . ? O37 Cl8 O38 109.03(10) . . ? O39 Cl8 O38 109.77(9) . . ? O26A Cl5A O25A 105.5(10) . . ? O26A Cl5A O27A 116.4(9) . . ? O25A Cl5A O27A 106.5(10) . . ? O26A Cl5A O28A 107.9(10) . . ? O25A Cl5A O28A 109.3(8) . . ? O27A Cl5A O28A 110.9(10) . . ? O38A Cl8A O40A 109.4(9) . . ? O38A Cl8A O37A 109.5(8) . . ? O40A Cl8A O37A 113.6(9) . . ? O38A Cl8A O39A 108.8(8) . . ? O40A Cl8A O39A 107.1(8) . . ? O37A Cl8A O39A 108.4(8) . . ? O1 Co1 O2 95.29(4) . . ? O1 Co1 N3 88.83(5) . . ? O2 Co1 N3 175.84(5) . . ? O1 Co1 N1 175.56(4) . . ? O2 Co1 N1 89.14(4) . . ? N3 Co1 N1 86.74(5) . . ? O1 Co1 N4 92.05(5) . . ? O2 Co1 N4 88.03(4) . . ? N3 Co1 N4 92.44(5) . . ? N1 Co1 N4 88.07(5) . . ? O1 Co1 N2 93.92(5) . . ? O2 Co1 N2 86.24(5) . . ? N3 Co1 N2 92.88(5) . . ? N1 Co1 N2 86.38(5) . . ? N4 Co1 N2 172.08(5) . . ? O3 Co2 O4 95.56(4) . . ? O3 Co2 N5 175.15(4) . . ? O4 Co2 N5 88.89(4) . . ? O3 Co2 N8 88.65(4) . . ? O4 Co2 N8 175.79(4) . . ? N5 Co2 N8 86.90(5) . . ? O3 Co2 N6 94.70(4) . . ? O4 Co2 N6 87.25(4) . . ? N5 Co2 N6 87.42(5) . . ? N8 Co2 N6 92.56(5) . . ? O3 Co2 N7 91.72(5) . . ? O4 Co2 N7 86.77(5) . . ? N5 Co2 N7 86.59(5) . . ? N8 Co2 N7 92.97(5) . . ? N6 Co2 N7 171.62(5) . . ? O5 Co3 O6 95.64(4) . . ? O5 Co3 N9 175.00(4) . . ? O6 Co3 N9 88.93(4) . . ? O5 Co3 N10 88.48(4) . . ? O6 Co3 N10 175.87(5) . . ? N9 Co3 N10 86.95(5) . . ? O5 Co3 N11 94.83(5) . . ? O6 Co3 N11 87.08(4) . . ? N9 Co3 N11 87.41(5) . . ? N10 Co3 N11 92.61(5) . . ? O5 Co3 N12 91.79(5) . . ? O6 Co3 N12 86.73(5) . . ? N9 Co3 N12 86.43(5) . . ? N10 Co3 N12 93.13(5) . . ? N11 Co3 N12 171.34(5) . . ? O8 Co4 O7 95.43(4) . . ? O8 Co4 N16 175.72(5) . . ? O7 Co4 N16 88.84(5) . . ? O8 Co4 N13 89.21(4) . . ? O7 Co4 N13 175.36(4) . . ? N16 Co4 N13 86.52(5) . . ? O8 Co4 N14 87.80(4) . . ? O7 Co4 N14 92.21(5) . . ? N16 Co4 N14 92.36(5) . . ? N13 Co4 N14 87.97(5) . . ? O8 Co4 N15 86.25(5) . . ? O7 Co4 N15 93.70(5) . . ? N16 Co4 N15 93.17(5) . . ? N13 Co4 N15 86.58(5) . . ? N14 Co4 N15 171.98(5) . . ? 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 N1 C1 C2 N2 42.32(15) . . . . ? N1 C3 C4 N3 -37.27(15) . . . . ? N1 C5 C6 N4 -49.38(14) . . . . ? O1 C8 C9 C10 2.1(2) . . . . ? C7 C8 C9 C10 -176.80(13) . . . . ? C8 C9 C10 O2 -4.1(2) . . . . ? C8 C9 C10 C11 174.28(12) . . . . ? O2 C10 C11 C12 -151.99(13) . . . . ? C9 C10 C11 C12 29.49(19) . . . . ? O2 C10 C11 C20 26.98(17) . . . . ? C9 C10 C11 C20 -151.54(13) . . . . ? C20 C11 C12 C13 -1.5(2) . . . . ? C10 C11 C12 C13 177.48(12) . . . . ? C11 C12 C13 C14 -176.65(13) . . . . ? C11 C12 C13 C18 2.5(2) . . . . ? C18 C13 C14 C15 -0.4(2) . . . . ? C12 C13 C14 C15 178.77(13) . . . . ? C13 C14 C15 C16 1.6(2) . . . . ? C14 C15 C16 C17 -0.9(2) . . . . ? C15 C16 C17 C18 -1.0(2) . . . . ? C16 C17 C18 C13 2.2(2) . . . . ? C16 C17 C18 C19 -177.27(13) . . . . ? C14 C13 C18 C17 -1.46(19) . . . . ? C12 C13 C18 C17 179.34(12) . . . . ? C14 C13 C18 C19 178.02(13) . . . . ? C12 C13 C18 C19 -1.19(19) . . . . ? C17 C18 C19 C20 178.26(13) . . . . ? C13 C18 C19 C20 -1.2(2) . . . . ? C18 C19 C20 C11 2.3(2) . . . . ? C12 C11 C20 C19 -0.9(2) . . . . ? C10 C11 C20 C19 -179.94(12) . . . . ? N5 C21 C22 N6 46.19(14) . . . . ? N5 C23 C24 N7 -41.62(15) . . . . ? N5 C25 C26 N8 42.16(14) . . . . ? O3 C28 C29 C30 -3.7(2) . . . . ? C27 C28 C29 C30 175.73(13) . . . . ? C28 C29 C30 O4 -0.3(2) . . . . ? C28 C29 C30 C31 -179.16(12) . . . . ? O4 C30 C31 C32 150.41(13) . . . . ? C29 C30 C31 C32 -30.64(19) . . . . ? O4 C30 C31 C40 -26.83(17) . . . . ? C29 C30 C31 C40 152.12(13) . . . . ? C40 C31 C32 C33 1.1(2) . . . . ? C30 C31 C32 C33 -176.10(12) . . . . ? C31 C32 C33 C34 176.11(13) . . . . ? C31 C32 C33 C38 -2.5(2) . . . . ? C38 C33 C34 C35 -0.4(2) . . . . ? C32 C33 C34 C35 -179.06(14) . . . . ? C33 C34 C35 C36 -1.3(2) . . . . ? C34 C35 C36 C37 1.1(2) . . . . ? C35 C36 C37 C38 0.7(2) . . . . ? C36 C37 C38 C33 -2.4(2) . . . . ? C36 C37 C38 C39 176.76(13) . . . . ? C34 C33 C38 C37 2.20(19) . . . . ? C32 C33 C38 C37 -179.10(12) . . . . ? C34 C33 C38 C39 -176.98(13) . . . . ? C32 C33 C38 C39 1.72(19) . . . . ? C37 C38 C39 C40 -178.64(13) . . . . ? C33 C38 C39 C40 0.5(2) . . . . ? C38 C39 C40 C31 -2.0(2) . . . . ? C32 C31 C40 C39 1.2(2) . . . . ? C30 C31 C40 C39 178.47(12) . . . . ? N9 C41 C42 N10 41.86(15) . . . . ? N9 C43 C44 N11 46.25(14) . . . . ? N9 C45 C46 N12 -42.70(15) . . . . ? O5 C48 C49 C50 -3.3(2) . . . . ? C47 C48 C49 C50 176.61(13) . . . . ? C48 C49 C50 O6 -1.1(2) . . . . ? C48 C49 C50 C51 -179.78(12) . . . . ? O6 C50 C51 C52 149.10(13) . . . . ? C49 C50 C51 C52 -32.07(19) . . . . ? O6 C50 C51 C60 -27.82(17) . . . . ? C49 C50 C51 C60 151.00(13) . . . . ? C60 C51 C52 C53 1.2(2) . . . . ? C50 C51 C52 C53 -175.72(12) . . . . ? C51 C52 C53 C54 175.74(13) . . . . ? C51 C52 C53 C58 -2.8(2) . . . . ? C52 C53 C54 C55 -178.24(14) . . . . ? C58 C53 C54 C55 0.3(2) . . . . ? C53 C54 C55 C56 -2.4(2) . . . . ? C54 C55 C56 C57 1.8(2) . . . . ? C55 C56 C57 C58 0.8(2) . . . . ? C56 C57 C58 C59 176.15(14) . . . . ? C56 C57 C58 C53 -2.9(2) . . . . ? C54 C53 C58 C57 2.3(2) . . . . ? C52 C53 C58 C57 -179.12(12) . . . . ? C54 C53 C58 C59 -176.77(13) . . . . ? C52 C53 C58 C59 1.83(19) . . . . ? C57 C58 C59 C60 -178.22(13) . . . . ? C53 C58 C59 C60 0.8(2) . . . . ? C58 C59 C60 C51 -2.5(2) . . . . ? C52 C51 C60 C59 1.5(2) . . . . ? C50 C51 C60 C59 178.45(13) . . . . ? N13 C61 C62 N14 -49.50(14) . . . . ? N13 C63 C64 N15 43.17(15) . . . . ? N13 C65 C66 N16 -37.26(15) . . . . ? O7 C68 C69 C70 1.2(2) . . . . ? C67 C68 C69 C70 -177.69(13) . . . . ? C68 C69 C70 O8 -3.4(2) . . . . ? C68 C69 C70 C71 175.18(12) . . . . ? O8 C70 C71 C72 -150.38(13) . . . . ? C69 C70 C71 C72 30.94(19) . . . . ? O8 C70 C71 C80 28.40(17) . . . . ? C69 C70 C71 C80 -150.28(13) . . . . ? C80 C71 C72 C73 -2.0(2) . . . . ? C70 C71 C72 C73 176.74(12) . . . . ? C71 C72 C73 C74 -175.76(13) . . . . ? C71 C72 C73 C78 3.1(2) . . . . ? C72 C73 C74 C75 178.27(14) . . . . ? C78 C73 C74 C75 -0.6(2) . . . . ? C73 C74 C75 C76 2.0(2) . . . . ? C74 C75 C76 C77 -1.3(2) . . . . ? C75 C76 C77 C78 -1.0(2) . . . . ? C76 C77 C78 C79 -176.64(14) . . . . ? C76 C77 C78 C73 2.4(2) . . . . ? C74 C73 C78 C79 177.44(13) . . . . ? C72 C73 C78 C79 -1.4(2) . . . . ? C74 C73 C78 C77 -1.6(2) . . . . ? C72 C73 C78 C77 179.52(12) . . . . ? C77 C78 C79 C80 177.73(14) . . . . ? C73 C78 C79 C80 -1.3(2) . . . . ? C78 C79 C80 C71 2.4(2) . . . . ? C72 C71 C80 C79 -0.7(2) . . . . ? C70 C71 C80 C79 -179.54(13) . . . . ? C2 C1 N1 C5 -162.19(11) . . . . ? C2 C1 N1 C3 73.56(14) . . . . ? C2 C1 N1 Co1 -47.20(12) . . . . ? C6 C5 N1 C1 160.82(11) . . . . ? C6 C5 N1 C3 -74.12(13) . . . . ? C6 C5 N1 Co1 45.41(12) . . . . ? C4 C3 N1 C1 -99.07(13) . . . . ? C4 C3 N1 C5 135.01(12) . . . . ? C4 C3 N1 Co1 18.87(13) . . . . ? C1 C2 N2 Co1 -17.47(13) . . . . ? C3 C4 N3 Co1 39.10(13) . . . . ? C5 C6 N4 Co1 28.78(12) . . . . ? C24 C23 N5 C21 160.35(11) . . . . ? C24 C23 N5 C25 -74.66(14) . . . . ? C24 C23 N5 Co2 45.58(12) . . . . ? C22 C21 N5 C23 -161.59(11) . . . . ? C22 C21 N5 C25 72.94(13) . . . . ? C22 C21 N5 Co2 -46.25(11) . . . . ? C26 C25 N5 C23 94.96(13) . . . . ? C26 C25 N5 C21 -139.65(11) . . . . ? C26 C25 N5 Co2 -23.18(13) . . . . ? C21 C22 N6 Co2 -23.65(13) . . . . ? C23 C24 N7 Co2 18.09(13) . . . . ? C25 C26 N8 Co2 -41.71(12) . . . . ? C46 C45 N9 C43 160.61(11) . . . . ? C46 C45 N9 C41 -74.49(14) . . . . ? C46 C45 N9 Co3 45.79(12) . . . . ? C44 C43 N9 C45 -161.88(11) . . . . ? C44 C43 N9 C41 72.69(13) . . . . ? C44 C43 N9 Co3 -46.40(12) . . . . ? C42 C41 N9 C45 94.97(13) . . . . ? C42 C41 N9 C43 -139.55(11) . . . . ? C42 C41 N9 Co3 -23.25(13) . . . . ? C41 C42 N10 Co3 -41.20(12) . . . . ? C43 C44 N11 Co3 -23.59(13) . . . . ? C45 C46 N12 Co3 19.60(14) . . . . ? C62 C61 N13 C63 160.89(11) . . . . ? C62 C61 N13 C65 -74.22(13) . . . . ? C62 C61 N13 Co4 45.62(12) . . . . ? C64 C63 N13 C61 -162.44(11) . . . . ? C64 C63 N13 C65 73.44(14) . . . . ? C64 C63 N13 Co4 -47.47(12) . . . . ? C66 C65 N13 C61 135.23(12) . . . . ? C66 C65 N13 C63 -99.10(13) . . . . ? C66 C65 N13 Co4 18.81(14) . . . . ? C61 C62 N14 Co4 28.83(12) . . . . ? C63 C64 N15 Co4 -18.54(13) . . . . ? C65 C66 N16 Co4 39.14(13) . . . . ? C9 C8 O1 Co1 5.63(19) . . . . ? C7 C8 O1 Co1 -175.45(9) . . . . ? C9 C10 O2 Co1 -1.98(19) . . . . ? C11 C10 O2 Co1 179.56(8) . . . . ? C29 C28 O3 Co2 0.88(19) . . . . ? C27 C28 O3 Co2 -178.59(9) . . . . ? C29 C30 O4 Co2 6.46(18) . . . . ? C31 C30 O4 Co2 -174.64(8) . . . . ? C49 C48 O5 Co3 1.89(19) . . . . ? C47 C48 O5 Co3 -178.06(9) . . . . ? C49 C50 O6 Co3 6.19(18) . . . . ? C51 C50 O6 Co3 -175.05(8) . . . . ? C69 C68 O7 Co4 5.11(19) . . . . ? C67 C68 O7 Co4 -175.94(9) . . . . ? C69 C70 O8 Co4 -1.23(19) . . . . ? C71 C70 O8 Co4 -179.84(8) . . . . ? C8 O1 Co1 O2 -8.62(11) . . . . ? C8 O1 Co1 N3 172.00(11) . . . . ? C8 O1 Co1 N1 171.1(6) . . . . ? C8 O1 Co1 N4 79.59(11) . . . . ? C8 O1 Co1 N2 -95.20(11) . . . . ? C10 O2 Co1 O1 6.88(11) . . . . ? C10 O2 Co1 N3 178(78) . . . . ? C10 O2 Co1 N1 -173.10(11) . . . . ? C10 O2 Co1 N4 -84.99(11) . . . . ? C10 O2 Co1 N2 100.47(11) . . . . ? C4 N3 Co1 O1 156.46(9) . . . . ? C4 N3 Co1 O2 -15.1(7) . . . . ? C4 N3 Co1 N1 -23.61(9) . . . . ? C4 N3 Co1 N4 -111.54(9) . . . . ? C4 N3 Co1 N2 62.60(9) . . . . ? C1 N1 Co1 O1 124.4(6) . . . . ? C5 N1 Co1 O1 -115.6(6) . . . . ? C3 N1 Co1 O1 3.3(6) . . . . ? C1 N1 Co1 O2 -55.90(8) . . . . ? C5 N1 Co1 O2 64.09(8) . . . . ? C3 N1 Co1 O2 -177.01(9) . . . . ? C1 N1 Co1 N3 123.48(9) . . . . ? C5 N1 Co1 N3 -116.53(8) . . . . ? C3 N1 Co1 N3 2.37(9) . . . . ? C1 N1 Co1 N4 -143.96(8) . . . . ? C5 N1 Co1 N4 -23.97(8) . . . . ? C3 N1 Co1 N4 94.93(9) . . . . ? C1 N1 Co1 N2 30.38(8) . . . . ? C5 N1 Co1 N2 150.38(8) . . . . ? C3 N1 Co1 N2 -90.73(9) . . . . ? C6 N4 Co1 O1 172.80(9) . . . . ? C6 N4 Co1 O2 -91.98(9) . . . . ? C6 N4 Co1 N3 83.89(9) . . . . ? C6 N4 Co1 N1 -2.77(9) . . . . ? C6 N4 Co1 N2 -48.3(4) . . . . ? C2 N2 Co1 O1 177.15(9) . . . . ? C2 N2 Co1 O2 82.10(9) . . . . ? C2 N2 Co1 N3 -93.83(9) . . . . ? C2 N2 Co1 N1 -7.28(9) . . . . ? C2 N2 Co1 N4 38.4(4) . . . . ? C28 O3 Co2 O4 3.55(11) . . . . ? C28 O3 Co2 N5 160.0(5) . . . . ? C28 O3 Co2 N8 -176.59(11) . . . . ? C28 O3 Co2 N6 -84.13(11) . . . . ? C28 O3 Co2 N7 90.47(11) . . . . ? C30 O4 Co2 O3 -7.09(11) . . . . ? C30 O4 Co2 N5 174.85(11) . . . . ? C30 O4 Co2 N8 175(9) . . . . ? C30 O4 Co2 N6 87.37(11) . . . . ? C30 O4 Co2 N7 -98.50(11) . . . . ? C23 N5 Co2 O3 -98.3(5) . . . . ? C21 N5 Co2 O3 142.9(5) . . . . ? C25 N5 Co2 O3 23.1(6) . . . . ? C23 N5 Co2 O4 58.33(8) . . . . ? C21 N5 Co2 O4 -60.51(8) . . . . ? C25 N5 Co2 O4 179.71(9) . . . . ? C23 N5 Co2 N8 -121.67(9) . . . . ? C21 N5 Co2 N8 119.49(8) . . . . ? C25 N5 Co2 N8 -0.29(9) . . . . ? C23 N5 Co2 N6 145.62(9) . . . . ? C21 N5 Co2 N6 26.78(8) . . . . ? C25 N5 Co2 N6 -93.00(9) . . . . ? C23 N5 Co2 N7 -28.50(8) . . . . ? C21 N5 Co2 N7 -147.34(8) . . . . ? C25 N5 Co2 N7 92.88(9) . . . . ? C26 N8 Co2 O3 -154.06(9) . . . . ? C26 N8 Co2 O4 24.0(7) . . . . ? C26 N8 Co2 N5 24.01(9) . . . . ? C26 N8 Co2 N6 111.29(9) . . . . ? C26 N8 Co2 N7 -62.41(9) . . . . ? C22 N6 Co2 O3 -177.51(8) . . . . ? C22 N6 Co2 O4 87.13(9) . . . . ? C22 N6 Co2 N5 -1.88(9) . . . . ? C22 N6 Co2 N8 -88.66(9) . . . . ? C22 N6 Co2 N7 42.6(4) . . . . ? C24 N7 Co2 O3 -178.71(9) . . . . ? C24 N7 Co2 O4 -83.23(9) . . . . ? C24 N7 Co2 N5 5.85(9) . . . . ? C24 N7 Co2 N8 92.56(9) . . . . ? C24 N7 Co2 N6 -38.7(4) . . . . ? C48 O5 Co3 O6 2.03(11) . . . . ? C48 O5 Co3 N9 158.0(5) . . . . ? C48 O5 Co3 N10 -178.00(11) . . . . ? C48 O5 Co3 N11 -85.50(11) . . . . ? C48 O5 Co3 N12 88.91(11) . . . . ? C50 O6 Co3 O5 -5.92(11) . . . . ? C50 O6 Co3 N9 176.12(11) . . . . ? C50 O6 Co3 N10 174.4(6) . . . . ? C50 O6 Co3 N11 88.66(11) . . . . ? C50 O6 Co3 N12 -97.39(11) . . . . ? C45 N9 Co3 O5 -97.2(5) . . . . ? C43 N9 Co3 O5 143.7(5) . . . . ? C41 N9 Co3 O5 24.1(6) . . . . ? C45 N9 Co3 O6 58.80(8) . . . . ? C43 N9 Co3 O6 -60.24(8) . . . . ? C41 N9 Co3 O6 -179.83(9) . . . . ? C45 N9 Co3 N10 -121.32(9) . . . . ? C43 N9 Co3 N10 119.64(8) . . . . ? C41 N9 Co3 N10 0.05(9) . . . . ? C45 N9 Co3 N11 145.92(9) . . . . ? C43 N9 Co3 N11 26.88(8) . . . . ? C41 N9 Co3 N11 -92.71(9) . . . . ? C45 N9 Co3 N12 -27.99(9) . . . . ? C43 N9 Co3 N12 -147.03(8) . . . . ? C41 N9 Co3 N12 93.38(9) . . . . ? C42 N10 Co3 O5 -154.45(9) . . . . ? C42 N10 Co3 O6 25.2(7) . . . . ? C42 N10 Co3 N9 23.51(9) . . . . ? C42 N10 Co3 N11 110.78(9) . . . . ? C42 N10 Co3 N12 -62.75(9) . . . . ? C44 N11 Co3 O5 -177.47(8) . . . . ? C44 N11 Co3 O6 87.11(9) . . . . ? C44 N11 Co3 N9 -1.95(9) . . . . ? C44 N11 Co3 N10 -88.78(9) . . . . ? C44 N11 Co3 N12 42.8(4) . . . . ? C46 N12 Co3 O5 -179.95(9) . . . . ? C46 N12 Co3 O6 -84.40(9) . . . . ? C46 N12 Co3 N9 4.73(9) . . . . ? C46 N12 Co3 N10 91.47(9) . . . . ? C46 N12 Co3 N11 -40.0(4) . . . . ? C70 O8 Co4 O7 5.35(11) . . . . ? C70 O8 Co4 N16 -179(79) . . . . ? C70 O8 Co4 N13 -174.66(11) . . . . ? C70 O8 Co4 N14 -86.67(11) . . . . ? C70 O8 Co4 N15 98.72(11) . . . . ? C68 O7 Co4 O8 -7.19(11) . . . . ? C68 O7 Co4 N16 173.12(11) . . . . ? C68 O7 Co4 N13 172.9(5) . . . . ? C68 O7 Co4 N14 80.80(11) . . . . ? C68 O7 Co4 N15 -93.77(11) . . . . ? C66 N16 Co4 O8 -19.5(7) . . . . ? C66 N16 Co4 O7 156.25(9) . . . . ? C66 N16 Co4 N13 -23.77(9) . . . . ? C66 N16 Co4 N14 -111.58(9) . . . . ? C66 N16 Co4 N15 62.61(9) . . . . ? C61 N13 Co4 O8 63.69(8) . . . . ? C63 N13 Co4 O8 -56.09(8) . . . . ? C65 N13 Co4 O8 -177.20(9) . . . . ? C61 N13 Co4 O7 -116.4(6) . . . . ? C63 N13 Co4 O7 123.8(6) . . . . ? C65 N13 Co4 O7 2.7(6) . . . . ? C61 N13 Co4 N16 -116.63(8) . . . . ? C63 N13 Co4 N16 123.59(9) . . . . ? C65 N13 Co4 N16 2.48(9) . . . . ? C61 N13 Co4 N14 -24.14(8) . . . . ? C63 N13 Co4 N14 -143.92(9) . . . . ? C65 N13 Co4 N14 94.97(9) . . . . ? C61 N13 Co4 N15 149.98(8) . . . . ? C63 N13 Co4 N15 30.20(8) . . . . ? C65 N13 Co4 N15 -90.91(9) . . . . ? C62 N14 Co4 O8 -91.94(9) . . . . ? C62 N14 Co4 O7 172.72(9) . . . . ? C62 N14 Co4 N16 83.78(9) . . . . ? C62 N14 Co4 N13 -2.65(9) . . . . ? C62 N14 Co4 N15 -49.8(4) . . . . ? C64 N15 Co4 O8 82.82(9) . . . . ? C64 N15 Co4 O7 178.03(9) . . . . ? C64 N15 Co4 N16 -92.93(9) . . . . ? C64 N15 Co4 N13 -6.61(9) . . . . ? C64 N15 Co4 N14 40.6(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H1N O39 0.9000(10) 2.317(6) 3.1822(17) 161.3(14) 4_566 N2 H1N O40A 0.9000(10) 2.578(14) 3.388(12) 150.1(13) 4_566 N3 H3N O40A 0.8998(10) 2.097(15) 2.899(12) 148.0(14) 4_566 N3 H3N O37 0.8998(10) 2.227(9) 3.0098(17) 145.1(14) 4_566 N3 H3N Cl8 0.8998(10) 2.995(9) 3.7778(15) 146.4(13) 4_566 N3 H4N O2W 0.8999(10) 2.021(2) 2.9184(16) 175.1(15) 4_566 N4 H5N O2W 0.9000(10) 2.624(11) 3.3221(16) 135.1(13) 4_566 N4 H6N O11 0.8999(10) 2.146(6) 3.0019(16) 158.5(14) . N6 H7N O16 0.8999(10) 2.376(8) 3.1981(18) 152.0(14) . N6 H7N O31 0.8999(10) 2.438(11) 3.1523(17) 136.5(13) 4_566 N6 H8N O18 0.8998(10) 2.171(6) 3.0265(17) 158.6(14) . N6 H8N O13 0.8998(10) 2.628(14) 3.1209(16) 115.3(11) . N7 H10N O37A 0.8999(10) 2.134(14) 2.988(12) 158.1(15) 3_656 N7 H10N O38 0.8999(10) 2.342(7) 3.1815(17) 155.2(14) 3_656 N8 H11N O38 0.9001(10) 2.216(10) 2.9875(17) 143.4(13) 3_656 N8 H11N O39A 0.9001(10) 2.239(15) 3.033(12) 146.9(14) 3_656 N8 H12N O32 0.8998(10) 2.325(13) 3.002(4) 131.9(13) 4_566 N10 H13N O14 0.8997(10) 2.494(17) 3.129(12) 128.0(13) 4_565 N10 H14N O26 0.9000(10) 2.212(9) 2.9865(17) 143.9(13) . N10 H14N O28A 0.9000(10) 2.264(15) 3.040(12) 144.2(14) . N11 H15N O22 0.8999(10) 2.179(6) 3.0333(17) 158.3(14) . N11 H15N O30 0.8999(10) 2.604(14) 3.1080(16) 116.2(11) . N11 H16N O31 0.9000(10) 2.351(7) 3.1813(18) 153.4(14) . N11 H16N O16 0.9000(10) 2.436(11) 3.1464(18) 136.0(13) 4_565 N12 H17N O27A 0.9000(10) 2.124(14) 2.961(12) 154.3(15) . N12 H17N O26 0.9000(10) 2.277(6) 3.1240(17) 156.7(14) . N14 H19N O36 0.9000(10) 2.156(6) 3.0095(16) 157.9(14) . N14 H20N O1W 0.8998(10) 2.567(11) 3.2859(16) 137.4(13) 4_565 N15 H22N O25 0.8998(10) 2.241(6) 3.1067(17) 161.3(14) 2_655 N15 H22N O26A 0.8998(10) 2.380(14) 3.199(12) 151.4(14) 2_655 N16 H23N O1W 0.8999(10) 2.026(2) 2.9236(16) 175.2(15) 4_565 N16 H24N O26A 0.8998(10) 2.124(16) 2.886(12) 142.0(14) 2_655 N16 H24N O28 0.8998(10) 2.242(10) 3.0109(17) 143.1(14) 2_655 O1W H1W O12 0.8997(10) 2.015(3) 2.9113(16) 173.8(15) . O1W H1W Cl1 0.8997(10) 2.978(8) 3.7949(11) 151.9(13) . O1W H2W O29 0.8996(10) 2.163(5) 3.0318(18) 162.0(14) 4_566 O1W H2W O32A 0.8996(10) 2.198(12) 2.906(4) 135.2(13) 4_566 O1W H2W Cl6 0.8996(10) 2.769(5) 3.6282(12) 160.2(13) 4_566 O2W H3W O34 0.8998(10) 2.019(2) 2.9181(16) 177.9(16) . O2W H3W Cl7 0.8998(10) 2.978(7) 3.8097(11) 154.5(13) . O2W H4W O14A 0.8997(10) 2.395(12) 3.160(8) 142.9(13) 4_465 O2W H4W O15 0.8997(10) 2.214(7) 3.0626(18) 157.1(14) 4_465 O2W H4W Cl2 0.8997(10) 2.762(4) 3.6417(12) 166.0(13) 4_465 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 31.80 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.628 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.068 data_2 _database_code_depnum_ccdc_archive 'CCDC 866266' #TrackingRef '- combined revised cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H24 Co N5 O2, 2(Cl O4)' _chemical_formula_sum 'C13 H24 Cl2 Co N5 O10' _chemical_formula_weight 540.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.1320(6) _cell_length_b 13.5840(9) _cell_length_c 16.711(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2073.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.731 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 1.149 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8046 _exptl_absorpt_correction_T_max 0.9015 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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_reflns_number 4887 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 28.01 _reflns_number_total 4887 _reflns_number_gt 4569 _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 'teXsan (MSC, 1992-1997)' _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_molecular_graphics 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' _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^)+(0.0887P)^2^+0.5342P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.021(17) _refine_ls_number_reflns 4887 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1264 _refine_ls_wR_factor_gt 0.1219 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 0.5376(4) 0.3982(3) 0.3041(2) 0.0511(8) Uani 1 1 d . . . H1A H 0.5803 0.3875 0.2517 0.061 Uiso 1 1 calc R . . H1B H 0.4319 0.3978 0.2983 0.061 Uiso 1 1 calc R . . C2 C 0.5829(4) 0.3161(3) 0.3594(2) 0.0532(8) Uani 1 1 d . . . H2A H 0.5119 0.3090 0.4022 0.064 Uiso 1 1 calc R . . H2B H 0.5875 0.2545 0.3302 0.064 Uiso 1 1 calc R . . C3 C 0.4652(4) 0.5491(3) 0.3781(2) 0.0559(9) Uani 1 1 d . . . H3A H 0.4909 0.6177 0.3855 0.067 Uiso 1 1 calc R . . H3B H 0.3763 0.5461 0.3464 0.067 Uiso 1 1 calc R . . C4 C 0.4404(4) 0.5019(3) 0.4570(3) 0.0628(10) Uani 1 1 d . . . H4A H 0.3872 0.4406 0.4501 0.075 Uiso 1 1 calc R . . H4B H 0.3829 0.5449 0.4910 0.075 Uiso 1 1 calc R . . C5 C 0.6503(4) 0.5592(3) 0.2701(2) 0.0528(8) Uani 1 1 d . . . H5A H 0.5875 0.5576 0.2233 0.063 Uiso 1 1 calc R . . H5B H 0.6589 0.6269 0.2879 0.063 Uiso 1 1 calc R . . C6 C 0.7988(5) 0.5187(3) 0.2498(2) 0.0602(9) Uani 1 1 d . . . H6A H 0.7884 0.4586 0.2190 0.072 Uiso 1 1 calc R . . H6B H 0.8527 0.5660 0.2179 0.072 Uiso 1 1 calc R . . C7 C 0.9389(3) 0.5475(2) 0.51232(19) 0.0406(6) Uani 1 1 d . . . C8 C 1.0636(3) 0.5528(2) 0.56769(17) 0.0404(6) Uani 1 1 d . . . C9 C 1.1288(4) 0.6416(3) 0.5912(2) 0.0495(7) Uani 1 1 d . . . H9 H 1.0921 0.7009 0.5720 0.059 Uiso 1 1 calc R . . C10 C 1.2465(4) 0.6415(3) 0.6424(2) 0.0563(8) Uani 1 1 d . . . H10 H 1.2897 0.7006 0.6574 0.068 Uiso 1 1 calc R . . C11 C 1.3004(4) 0.5539(4) 0.6716(2) 0.0607(10) Uani 1 1 d . . . H11 H 1.3787 0.5542 0.7071 0.073 Uiso 1 1 calc R . . C12 C 1.2392(5) 0.4659(3) 0.6484(3) 0.0625(9) Uani 1 1 d . . . H12 H 1.2782 0.4071 0.6672 0.075 Uiso 1 1 calc R . . C13 C 1.1195(4) 0.4641(3) 0.5970(2) 0.0497(7) Uani 1 1 d . . . H13 H 1.0771 0.4045 0.5823 0.060 Uiso 1 1 calc R . . N1 N 0.5858(3) 0.4969(2) 0.33561(15) 0.0427(7) Uani 1 1 d . . . N2 N 0.7274(3) 0.33964(19) 0.39294(18) 0.0462(6) Uani 1 1 d . . . H2C H 0.7980 0.3213 0.3584 0.055 Uiso 1 1 calc R . . H2D H 0.7408 0.3064 0.4390 0.055 Uiso 1 1 calc R . . N3 N 0.5866(3) 0.4821(3) 0.49489(17) 0.0515(7) Uani 1 1 d . . . H3C H 0.5843 0.4238 0.5204 0.062 Uiso 1 1 calc R . . H3D H 0.6065 0.5292 0.5311 0.062 Uiso 1 1 calc R . . N4 N 0.8797(3) 0.4980(2) 0.32576(18) 0.0458(7) Uani 1 1 d . . . H4C H 0.9401 0.5484 0.3371 0.055 Uiso 1 1 calc R . . H4D H 0.9342 0.4432 0.3200 0.055 Uiso 1 1 calc R . . N5 N 0.8751(3) 0.6267(2) 0.48448(18) 0.0478(6) Uani 1 1 d . . . H5 H 0.9051 0.6841 0.4988 0.057 Uiso 1 1 calc R . . O1 O 0.8916(3) 0.46342(17) 0.48914(15) 0.0473(6) Uani 1 1 d . . . O2 O 0.7599(3) 0.61755(16) 0.43221(13) 0.0463(5) Uani 1 1 d . . . O3 O 1.0821(4) 0.8015(4) 0.4070(3) 0.1018(13) Uani 1 1 d . . . O4 O 1.1099(6) 0.7819(5) 0.2724(3) 0.1309(19) Uani 1 1 d . . . O5 O 1.1209(5) 0.6456(3) 0.3512(3) 0.1112(15) Uani 1 1 d . . . O6 O 1.3100(4) 0.7611(4) 0.3538(4) 0.1183(17) Uani 1 1 d . . . O7 O 1.1237(6) 0.3633(3) 0.3627(3) 0.1108(16) Uani 1 1 d . . . O8 O 1.2543(5) 0.2241(4) 0.3380(3) 0.1175(17) Uani 1 1 d . . . O9 O 1.2393(6) 0.2862(3) 0.4653(2) 0.1020(14) Uani 1 1 d . . . O10 O 1.0359(4) 0.2097(4) 0.4078(3) 0.1115(15) Uani 1 1 d . . . Cl1 Cl 1.15886(10) 0.74629(7) 0.34926(6) 0.0560(2) Uani 1 1 d . . . Cl2 Cl 1.15846(10) 0.26903(7) 0.39114(5) 0.0519(2) Uani 1 1 d . . . Co1 Co 0.74025(4) 0.48010(3) 0.41285(2) 0.03467(12) 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 0.0477(18) 0.0470(17) 0.0587(19) -0.0057(15) -0.0154(15) -0.0049(14) C2 0.0532(19) 0.0378(16) 0.069(2) -0.0003(15) -0.0118(17) -0.0082(14) C3 0.0380(16) 0.056(2) 0.074(2) -0.0050(17) -0.0039(16) 0.0110(15) C4 0.0413(17) 0.071(3) 0.076(3) -0.013(2) 0.0109(16) 0.0004(17) C5 0.060(2) 0.0462(17) 0.0526(18) 0.0118(14) -0.0103(16) -0.0002(16) C6 0.069(2) 0.067(2) 0.0440(17) 0.0104(16) 0.0047(15) 0.001(2) C7 0.0384(14) 0.0389(15) 0.0446(15) -0.0008(12) 0.0010(12) -0.0040(12) C8 0.0365(14) 0.0457(16) 0.0389(14) -0.0025(12) 0.0004(11) -0.0039(12) C9 0.0446(16) 0.0476(17) 0.0562(17) -0.0102(15) -0.0013(15) -0.0038(13) C10 0.0451(18) 0.060(2) 0.0642(19) -0.0156(16) -0.0057(17) -0.0105(18) C11 0.0424(18) 0.086(3) 0.0542(19) -0.0093(19) -0.0118(14) -0.0015(17) C12 0.052(2) 0.070(2) 0.065(2) 0.0064(18) -0.0148(18) 0.006(2) C13 0.0470(17) 0.0498(18) 0.0524(17) 0.0001(14) -0.0054(14) -0.0005(14) N1 0.0343(12) 0.048(2) 0.0464(14) 0.0016(12) -0.0084(10) 0.0010(11) N2 0.0491(15) 0.0341(12) 0.0554(14) 0.0031(11) -0.0097(12) -0.0026(11) N3 0.0521(16) 0.0551(17) 0.0472(14) 0.0003(14) 0.0072(12) -0.0026(15) N4 0.0422(13) 0.0389(18) 0.0562(15) 0.0024(11) 0.0094(11) 0.0009(11) N5 0.0471(15) 0.0358(13) 0.0606(16) -0.0090(11) -0.0139(13) -0.0010(11) O1 0.0498(13) 0.0352(12) 0.0567(13) 0.0055(9) -0.0184(11) -0.0017(9) O2 0.0451(12) 0.0373(10) 0.0566(11) -0.0009(9) -0.0146(10) 0.0019(9) O3 0.081(2) 0.111(3) 0.114(3) -0.038(3) -0.008(2) 0.025(2) O4 0.150(4) 0.159(5) 0.083(3) 0.029(3) -0.010(3) 0.009(4) O5 0.091(3) 0.069(2) 0.173(4) -0.010(3) 0.040(3) -0.031(2) O6 0.059(2) 0.098(3) 0.198(5) -0.022(3) 0.006(3) -0.013(2) O7 0.128(4) 0.083(3) 0.122(3) 0.046(2) 0.012(3) 0.039(3) O8 0.086(3) 0.118(3) 0.149(4) -0.075(3) 0.033(3) 0.000(3) O9 0.129(4) 0.101(3) 0.075(2) 0.0212(19) -0.025(2) -0.028(3) O10 0.070(2) 0.128(4) 0.137(3) 0.052(3) -0.002(3) -0.033(2) Cl1 0.0464(4) 0.0503(5) 0.0714(5) 0.0014(4) 0.0025(4) -0.0055(4) Cl2 0.0519(4) 0.0467(4) 0.0573(4) 0.0052(3) 0.0062(3) 0.0037(4) Co1 0.03320(19) 0.0317(2) 0.0391(2) 0.00193(13) -0.00294(15) -0.00131(15) _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 N1 1.506(4) . ? C1 C2 1.507(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.469(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.484(6) . ? C3 N1 1.490(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N3 1.502(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.502(6) . ? C5 N1 1.503(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N4 1.495(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 O1 1.281(4) . ? C7 N5 1.309(4) . ? C7 C8 1.469(4) . ? C8 C13 1.397(5) . ? C8 C9 1.401(5) . ? C9 C10 1.374(5) . ? C9 H9 0.9300 . ? C10 C11 1.377(6) . ? C10 H10 0.9300 . ? C11 C12 1.375(6) . ? C11 H11 0.9300 . ? C12 C13 1.390(5) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? N1 Co1 1.925(3) . ? N2 Co1 1.940(3) . ? N2 H2C 0.9000 . ? N2 H2D 0.9000 . ? N3 Co1 1.962(3) . ? N3 H3C 0.9000 . ? N3 H3D 0.9000 . ? N4 Co1 1.949(3) . ? N4 H4C 0.9000 . ? N4 H4D 0.9000 . ? N5 O2 1.373(3) . ? N5 H5 0.8600 . ? O1 Co1 1.894(2) . ? O2 Co1 1.903(2) . ? O3 Cl1 1.409(4) . ? O4 Cl1 1.444(5) . ? O5 Cl1 1.411(4) . ? O6 Cl1 1.396(4) . ? O7 Cl2 1.402(4) . ? O8 Cl2 1.388(4) . ? O9 Cl2 1.461(4) . ? O10 Cl2 1.407(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 111.4(3) . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? N2 C2 C1 108.6(3) . . ? N2 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? N2 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? H2A C2 H2B 108.3 . . ? C4 C3 N1 109.3(3) . . ? C4 C3 H3A 109.8 . . ? N1 C3 H3A 109.8 . . ? C4 C3 H3B 109.8 . . ? N1 C3 H3B 109.8 . . ? H3A C3 H3B 108.3 . . ? C3 C4 N3 108.4(3) . . ? C3 C4 H4A 110.0 . . ? N3 C4 H4A 110.0 . . ? C3 C4 H4B 110.0 . . ? N3 C4 H4B 110.0 . . ? H4A C4 H4B 108.4 . . ? C6 C5 N1 108.2(3) . . ? C6 C5 H5A 110.1 . . ? N1 C5 H5A 110.1 . . ? C6 C5 H5B 110.1 . . ? N1 C5 H5B 110.1 . . ? H5A C5 H5B 108.4 . . ? N4 C6 C5 108.9(3) . . ? N4 C6 H6A 109.9 . . ? C5 C6 H6A 109.9 . . ? N4 C6 H6B 109.9 . . ? C5 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? O1 C7 N5 118.4(3) . . ? O1 C7 C8 119.7(3) . . ? N5 C7 C8 121.9(3) . . ? C13 C8 C9 119.3(3) . . ? C13 C8 C7 117.5(3) . . ? C9 C8 C7 123.2(3) . . ? C10 C9 C8 120.4(3) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 120.1(3) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C12 C11 C10 120.4(3) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 120.6(4) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C12 C13 C8 119.2(3) . . ? C12 C13 H13 120.4 . . ? C8 C13 H13 120.4 . . ? C3 N1 C5 111.6(3) . . ? C3 N1 C1 111.9(3) . . ? C5 N1 C1 111.2(3) . . ? C3 N1 Co1 106.2(2) . . ? C5 N1 Co1 105.5(2) . . ? C1 N1 Co1 110.1(2) . . ? C2 N2 Co1 109.5(2) . . ? C2 N2 H2C 109.8 . . ? Co1 N2 H2C 109.8 . . ? C2 N2 H2D 109.8 . . ? Co1 N2 H2D 109.8 . . ? H2C N2 H2D 108.2 . . ? C4 N3 Co1 110.1(2) . . ? C4 N3 H3C 109.6 . . ? Co1 N3 H3C 109.6 . . ? C4 N3 H3D 109.6 . . ? Co1 N3 H3D 109.6 . . ? H3C N3 H3D 108.2 . . ? C6 N4 Co1 109.5(2) . . ? C6 N4 H4C 109.8 . . ? Co1 N4 H4C 109.8 . . ? C6 N4 H4D 109.8 . . ? Co1 N4 H4D 109.8 . . ? H4C N4 H4D 108.2 . . ? C7 N5 O2 119.5(3) . . ? C7 N5 H5 120.2 . . ? O2 N5 H5 120.2 . . ? C7 O1 Co1 110.1(2) . . ? N5 O2 Co1 105.63(17) . . ? O6 Cl1 O3 112.2(3) . . ? O6 Cl1 O5 112.4(3) . . ? O3 Cl1 O5 112.2(3) . . ? O6 Cl1 O4 107.8(4) . . ? O3 Cl1 O4 106.0(3) . . ? O5 Cl1 O4 105.7(4) . . ? O8 Cl2 O7 109.1(3) . . ? O8 Cl2 O10 112.1(3) . . ? O7 Cl2 O10 114.2(3) . . ? O8 Cl2 O9 107.1(3) . . ? O7 Cl2 O9 104.9(3) . . ? O10 Cl2 O9 109.0(3) . . ? O1 Co1 O2 86.22(10) . . ? O1 Co1 N1 179.78(12) . . ? O2 Co1 N1 93.84(11) . . ? O1 Co1 N2 92.40(11) . . ? O2 Co1 N2 178.03(12) . . ? N1 Co1 N2 87.55(12) . . ? O1 Co1 N4 92.33(12) . . ? O2 Co1 N4 86.73(12) . . ? N1 Co1 N4 87.88(12) . . ? N2 Co1 N4 91.93(12) . . ? O1 Co1 N3 93.05(12) . . ? O2 Co1 N3 86.28(14) . . ? N1 Co1 N3 86.74(12) . . ? N2 Co1 N3 95.19(15) . . ? N4 Co1 N3 170.88(14) . . ? 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 N1 C1 C2 N2 -36.8(4) . . . . ? N1 C3 C4 N3 43.8(4) . . . . ? N1 C5 C6 N4 -45.4(4) . . . . ? O1 C7 C8 C13 -4.2(5) . . . . ? N5 C7 C8 C13 177.0(3) . . . . ? O1 C7 C8 C9 175.1(3) . . . . ? N5 C7 C8 C9 -3.8(5) . . . . ? C13 C8 C9 C10 0.1(5) . . . . ? C7 C8 C9 C10 -179.2(3) . . . . ? C8 C9 C10 C11 -0.6(5) . . . . ? C9 C10 C11 C12 1.4(6) . . . . ? C10 C11 C12 C13 -1.8(6) . . . . ? C11 C12 C13 C8 1.3(6) . . . . ? C9 C8 C13 C12 -0.5(5) . . . . ? C7 C8 C13 C12 178.8(3) . . . . ? C4 C3 N1 C5 -160.7(3) . . . . ? C4 C3 N1 C1 73.9(4) . . . . ? C4 C3 N1 Co1 -46.2(3) . . . . ? C6 C5 N1 C3 160.9(3) . . . . ? C6 C5 N1 C1 -73.4(4) . . . . ? C6 C5 N1 Co1 45.9(3) . . . . ? C2 C1 N1 C3 -98.5(4) . . . . ? C2 C1 N1 C5 135.9(3) . . . . ? C2 C1 N1 Co1 19.3(4) . . . . ? C1 C2 N2 Co1 37.0(4) . . . . ? C3 C4 N3 Co1 -20.8(4) . . . . ? C5 C6 N4 Co1 23.0(4) . . . . ? O1 C7 N5 O2 0.4(5) . . . . ? C8 C7 N5 O2 179.3(3) . . . . ? N5 C7 O1 Co1 3.0(4) . . . . ? C8 C7 O1 Co1 -175.9(2) . . . . ? C7 N5 O2 Co1 -3.5(4) . . . . ? C7 O1 Co1 O2 -3.9(2) . . . . ? C7 O1 Co1 N2 174.7(2) . . . . ? C7 O1 Co1 N4 82.7(2) . . . . ? C7 O1 Co1 N3 -89.9(2) . . . . ? N5 O2 Co1 O1 3.8(2) . . . . ? N5 O2 Co1 N1 -176.4(2) . . . . ? N5 O2 Co1 N4 -88.7(2) . . . . ? N5 O2 Co1 N3 97.1(2) . . . . ? C3 N1 Co1 O2 -58.8(2) . . . . ? C5 N1 Co1 O2 59.8(2) . . . . ? C1 N1 Co1 O2 179.9(2) . . . . ? C3 N1 Co1 N2 122.6(2) . . . . ? C5 N1 Co1 N2 -118.8(2) . . . . ? C1 N1 Co1 N2 1.3(2) . . . . ? C3 N1 Co1 N4 -145.4(2) . . . . ? C5 N1 Co1 N4 -26.8(2) . . . . ? C1 N1 Co1 N4 93.3(2) . . . . ? C3 N1 Co1 N3 27.3(2) . . . . ? C5 N1 Co1 N3 145.9(2) . . . . ? C1 N1 Co1 N3 -94.1(2) . . . . ? C2 N2 Co1 O1 157.9(2) . . . . ? C2 N2 Co1 N1 -21.9(3) . . . . ? C2 N2 Co1 N4 -109.7(3) . . . . ? C2 N2 Co1 N3 64.6(3) . . . . ? C6 N4 Co1 O1 -177.6(3) . . . . ? C6 N4 Co1 O2 -91.5(3) . . . . ? C6 N4 Co1 N1 2.4(3) . . . . ? C6 N4 Co1 N2 89.9(3) . . . . ? C4 N3 Co1 O1 176.2(3) . . . . ? C4 N3 Co1 O2 90.2(3) . . . . ? C4 N3 Co1 N1 -3.9(3) . . . . ? C4 N3 Co1 N2 -91.1(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2C O4 0.90 2.40 3.234(6) 153.6 4_745 N2 H2D O9 0.90 2.04 2.923(4) 168.7 3_456 N3 H3C O10 0.90 2.22 3.106(6) 168.7 3_456 N3 H3D O3 0.90 2.53 3.366(6) 154.6 3_466 N4 H4C O5 0.90 2.13 3.009(5) 166.4 . N4 H4D O7 0.90 2.16 2.948(5) 145.2 . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.082 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.079 data_3 _database_code_depnum_ccdc_archive 'CCDC 866267' #TrackingRef '- combined revised cif.cif' #------------------------------------------------------------------------------ _audit_creation_date 1999-11-09 _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Sheldrick, G.M. (1985). In: "Crystallographic Computing 3" (Eds G.M. Sheldrick, C. Kruger and R. Goddard) Oxford University Press, pp. 175-189. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #------------------------------------------------------------------------------ _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'teXsan (MSC, 1992-1997)' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SHELXS86 (Sheldrick, 1985) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 8.455(3) _cell_length_b 9.447(3) _cell_length_c 12.232(4) _cell_angle_alpha 98.584(6) _cell_angle_beta 101.007(6) _cell_angle_gamma 112.488(6) _cell_volume 859.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 273.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-p 1' loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.848 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 478.13 _chemical_formula_analytical ? _chemical_formula_sum 'C8 H22 Cl2 Co N5 O10 ' _chemical_formula_moiety 'C8 H22 Co N5 O2, 2(Cl O4)' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 492.00 _exptl_absorpt_coefficient_mu 1.372 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.283766 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 273.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\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 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 3992 _reflns_number_total 3992 _reflns_number_gt 2975 _reflns_threshold_expression I>2.50\s(I) _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI 0.100 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.94 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 16 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 44 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 20 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 4 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 10 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Co 0 2 0.299 0.973 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Co(1) 0.04859(9) 0.53004(8) 0.27673(6) 0.0300(2) 1.000 . Uani d ? Cl(1) 0.2762(2) 0.2421(2) 0.4814(1) 0.0419(4) 1.000 . Uani d ? Cl(2) 0.3740(2) 0.1921(2) 0.0908(1) 0.0453(4) 1.000 . Uani d ? O(1) -0.0707(5) 0.3492(4) 0.3303(3) 0.035(1) 1.000 . Uani d ? O(2) -0.0607(5) 0.3946(4) 0.1267(3) 0.039(1) 1.000 . Uani d ? O(3) 0.2943(7) 0.4017(5) 0.5133(4) 0.076(2) 1.000 . Uani d ? O(4) 0.1964(8) 0.1590(6) 0.5580(4) 0.085(2) 1.000 . Uani d ? O(5) 0.1722(7) 0.1659(6) 0.3668(4) 0.075(2) 1.000 . Uani d ? O(6) 0.4456(6) 0.2397(6) 0.4919(4) 0.076(2) 1.000 . Uani d ? O(7) 0.2081(6) 0.2010(6) 0.0788(4) 0.077(2) 1.000 . Uani d ? O(8) 0.4813(6) 0.2704(6) 0.2042(4) 0.072(2) 1.000 . Uani d ? O(9) 0.4645(8) 0.2688(8) 0.0152(5) 0.107(3) 1.000 . Uani d ? O(10) 0.3488(7) 0.0302(5) 0.0677(4) 0.083(2) 1.000 . Uani d ? N(1) 0.1635(6) 0.7129(5) 0.2197(3) 0.032(1) 1.000 . Uani d ? N(3) 0.2559(6) 0.4855(5) 0.2708(4) 0.036(1) 1.000 . Uani d ? N(2) 0.1608(6) 0.6655(5) 0.4315(4) 0.036(1) 1.000 . Uani d ? N(4) -0.1586(6) 0.5790(5) 0.2567(4) 0.038(1) 1.000 . Uani d ? N(5) -0.1499(6) 0.2449(5) 0.1410(4) 0.041(1) 1.000 . Uani d ? C(1) 0.2733(7) 0.6726(6) 0.1499(4) 0.037(2) 1.000 . Uani d ? C(2) 0.3745(8) 0.5950(7) 0.2151(5) 0.040(2) 1.000 . Uani d ? C(3) 0.2801(7) 0.8531(6) 0.3194(4) 0.038(2) 1.000 . Uani d ? C(4) 0.2160(8) 0.8330(6) 0.4264(4) 0.041(2) 1.000 . Uani d ? C(5) 0.0177(8) 0.7389(7) 0.1466(5) 0.045(2) 1.000 . Uani d ? C(6) -0.1262(8) 0.7176(8) 0.2036(5) 0.051(2) 1.000 . Uani d ? C(7) -0.1555(7) 0.2259(7) 0.2450(5) 0.039(2) 1.000 . Uani d ? C(8) -0.2626(9) 0.0697(7) 0.2611(5) 0.056(2) 1.000 . Uani d ? H(1) 0.3207 0.4979 0.3468 0.043 1.000 . Uiso c ? H(2) 0.2161 0.3798 0.2281 0.043 1.000 . Uiso c ? H(3) 0.0788 0.6397 0.4766 0.044 1.000 . Uiso c ? H(4) 0.2623 0.6503 0.4650 0.044 1.000 . Uiso c ? H(5) -0.2600 0.4899 0.2079 0.045 1.000 . Uiso c ? H(6) -0.1789 0.6040 0.3294 0.045 1.000 . Uiso c ? H(7) -0.2067 0.1565 0.0765 0.049 1.000 . Uiso c ? H(8) 0.1984 0.6018 0.0785 0.044 1.000 . Uiso c ? H(9) 0.3549 0.7661 0.1366 0.044 1.000 . Uiso c ? H(10) 0.4756 0.6738 0.2722 0.047 1.000 . Uiso c ? H(11) 0.4119 0.5374 0.1634 0.047 1.000 . Uiso c ? H(12) 0.3987 0.8629 0.3343 0.046 1.000 . Uiso c ? H(13) 0.2768 0.9460 0.3002 0.046 1.000 . Uiso c ? H(14) 0.1178 0.8595 0.4228 0.049 1.000 . Uiso c ? H(15) 0.3095 0.8997 0.4927 0.049 1.000 . Uiso c ? H(16) 0.0642 0.8432 0.1360 0.054 1.000 . Uiso c ? H(17) -0.0284 0.6649 0.0741 0.054 1.000 . Uiso c ? H(18) -0.2321 0.6993 0.1485 0.061 1.000 . Uiso c ? H(19) -0.0929 0.8103 0.2618 0.061 1.000 . Uiso c ? H(20) -0.3830 0.0345 0.2190 0.067 1.000 . Uiso c ? H(21) -0.2183 -0.0035 0.2343 0.067 1.000 . Uiso c ? H(22) -0.2555 0.0772 0.3403 0.067 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co(1) 0.0309(4) 0.0226(4) 0.0361(4) 0.0096(3) 0.0099(3) 0.0085(3) Cl(1) 0.0442(9) 0.0321(8) 0.0463(8) 0.0149(7) 0.0069(7) 0.0107(6) Cl(2) 0.0454(9) 0.0383(9) 0.0550(9) 0.0199(7) 0.0147(7) 0.0113(7) O(1) 0.042(2) 0.028(2) 0.034(2) 0.012(2) 0.012(2) 0.011(2) O(2) 0.043(2) 0.029(2) 0.037(2) 0.008(2) 0.008(2) 0.006(2) O(3) 0.117(4) 0.033(3) 0.072(3) 0.035(3) 0.008(3) 0.009(2) O(4) 0.123(5) 0.054(3) 0.089(4) 0.026(3) 0.065(3) 0.031(3) O(5) 0.082(4) 0.072(4) 0.056(3) 0.044(3) -0.019(2) -0.010(3) O(6) 0.043(3) 0.088(4) 0.086(3) 0.023(3) 0.008(3) 0.010(3) O(7) 0.052(3) 0.081(4) 0.095(4) 0.035(3) 0.010(3) 0.002(3) O(8) 0.068(3) 0.075(4) 0.064(3) 0.034(3) 0.004(3) 0.000(3) O(9) 0.124(5) 0.124(6) 0.122(5) 0.064(4) 0.077(4) 0.085(4) O(10) 0.094(4) 0.036(3) 0.105(4) 0.029(3) 0.000(3) 0.002(3) N(1) 0.034(3) 0.029(2) 0.032(2) 0.012(2) 0.007(2) 0.010(2) N(3) 0.034(3) 0.031(3) 0.046(3) 0.014(2) 0.016(2) 0.012(2) N(2) 0.037(3) 0.030(3) 0.041(2) 0.010(2) 0.014(2) 0.012(2) N(4) 0.031(3) 0.034(3) 0.050(3) 0.014(2) 0.015(2) 0.010(2) N(5) 0.049(3) 0.025(3) 0.043(3) 0.011(2) 0.012(2) 0.009(2) C(1) 0.039(3) 0.034(3) 0.034(3) 0.009(3) 0.013(2) 0.007(2) C(2) 0.037(3) 0.037(3) 0.048(3) 0.016(3) 0.019(3) 0.009(3) C(3) 0.043(3) 0.022(3) 0.041(3) 0.007(3) 0.010(3) 0.005(2) C(4) 0.050(4) 0.026(3) 0.041(3) 0.013(3) 0.011(3) 0.004(3) C(5) 0.047(4) 0.043(4) 0.050(3) 0.022(3) 0.009(3) 0.025(3) C(6) 0.048(4) 0.056(4) 0.068(4) 0.033(3) 0.019(3) 0.029(4) C(7) 0.037(3) 0.030(3) 0.051(3) 0.015(3) 0.010(3) 0.012(3) C(8) 0.068(5) 0.033(4) 0.060(4) 0.015(3) 0.008(3) 0.019(3) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2975 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0944 _refine_ls_R_factor_gt 0.0720 _refine_ls_wR_factor_all 0.0826 _refine_ls_wR_factor_ref 0.0787 _refine_ls_goodness_of_fit_all 2.256 _refine_ls_goodness_of_fit_ref 2.510 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0020 _refine_diff_density_min -1.26 _refine_diff_density_max 1.48 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co(1) O(1) 1.906(4) . . yes Co(1) O(2) 1.899(3) . . yes Co(1) N(1) 1.936(4) . . yes Co(1) N(3) 1.964(4) . . yes Co(1) N(2) 1.945(4) . . yes Co(1) N(4) 1.958(4) . . yes Cl(1) O(3) 1.440(4) . . yes Cl(1) O(4) 1.416(5) . . yes Cl(1) O(5) 1.414(4) . . yes Cl(1) O(6) 1.423(5) . . yes Cl(2) O(7) 1.418(4) . . yes Cl(2) O(8) 1.412(4) . . yes Cl(2) O(9) 1.419(5) . . yes Cl(2) O(10) 1.437(4) . . yes O(1) C(7) 1.293(6) . . yes O(2) N(5) 1.381(5) . . yes N(1) C(1) 1.487(6) . . yes N(1) C(3) 1.507(6) . . yes N(1) C(5) 1.502(6) . . yes N(3) C(2) 1.489(7) . . yes N(3) H(1) 0.95 . . no N(3) H(2) 0.95 . . no N(2) C(4) 1.483(7) . . yes N(2) H(3) 0.95 . . no N(2) H(4) 0.95 . . no N(4) C(6) 1.502(7) . . yes N(4) H(5) 0.95 . . no N(4) H(6) 0.95 . . no N(5) C(7) 1.318(6) . . yes N(5) H(7) 0.95 . . no C(1) C(2) 1.516(7) . . yes C(1) H(8) 0.95 . . no C(1) H(9) 0.95 . . no C(2) H(10) 0.95 . . no C(2) H(11) 0.95 . . no C(3) C(4) 1.519(7) . . yes C(3) H(12) 0.95 . . no C(3) H(13) 0.95 . . no C(4) H(14) 0.95 . . no C(4) H(15) 0.95 . . no C(5) C(6) 1.479(8) . . yes C(5) H(16) 0.95 . . no C(5) H(17) 0.95 . . no C(6) H(18) 0.95 . . no C(6) H(19) 0.95 . . no C(7) C(8) 1.473(8) . . yes C(8) H(20) 0.95 . . no C(8) H(21) 0.95 . . no C(8) H(22) 0.95 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Co(1) O(2) 86.2(1) . . . yes O(1) Co(1) N(1) 178.4(2) . . . yes O(1) Co(1) N(3) 94.9(2) . . . yes O(1) Co(1) N(2) 92.9(2) . . . yes O(1) Co(1) N(4) 91.3(2) . . . yes O(2) Co(1) N(1) 92.9(2) . . . yes O(2) Co(1) N(3) 86.4(2) . . . yes O(2) Co(1) N(2) 178.9(2) . . . yes O(2) Co(1) N(4) 86.8(2) . . . yes N(1) Co(1) N(3) 86.3(2) . . . yes N(1) Co(1) N(2) 88.0(2) . . . yes N(1) Co(1) N(4) 87.3(2) . . . yes N(3) Co(1) N(2) 93.1(2) . . . yes N(3) Co(1) N(4) 170.4(2) . . . yes N(2) Co(1) N(4) 93.8(2) . . . yes O(3) Cl(1) O(4) 108.0(3) . . . yes O(3) Cl(1) O(5) 111.7(3) . . . yes O(3) Cl(1) O(6) 110.8(3) . . . yes O(4) Cl(1) O(5) 110.2(3) . . . yes O(4) Cl(1) O(6) 108.0(3) . . . yes O(5) Cl(1) O(6) 108.1(3) . . . yes O(7) Cl(2) O(8) 109.0(3) . . . yes O(7) Cl(2) O(9) 110.7(3) . . . yes O(7) Cl(2) O(10) 110.5(3) . . . yes O(8) Cl(2) O(9) 107.7(4) . . . yes O(8) Cl(2) O(10) 109.4(3) . . . yes O(9) Cl(2) O(10) 109.5(4) . . . yes Co(1) O(1) C(7) 110.1(3) . . . yes Co(1) O(2) N(5) 106.1(3) . . . yes Co(1) N(1) C(1) 106.7(3) . . . yes Co(1) N(1) C(3) 109.6(3) . . . yes Co(1) N(1) C(5) 106.6(3) . . . yes C(1) N(1) C(3) 110.2(4) . . . yes C(1) N(1) C(5) 111.1(4) . . . yes C(3) N(1) C(5) 112.3(4) . . . yes Co(1) N(3) C(2) 111.0(3) . . . yes Co(1) N(3) H(1) 109.1 . . . no Co(1) N(3) H(2) 109.1 . . . no C(2) N(3) H(1) 109.1 . . . no C(2) N(3) H(2) 109.1 . . . no H(1) N(3) H(2) 109.5 . . . no Co(1) N(2) C(4) 109.3(3) . . . yes Co(1) N(2) H(3) 109.5 . . . no Co(1) N(2) H(4) 109.5 . . . no C(4) N(2) H(3) 109.5 . . . no C(4) N(2) H(4) 109.5 . . . no H(3) N(2) H(4) 109.5 . . . no Co(1) N(4) C(6) 109.9(3) . . . yes Co(1) N(4) H(5) 109.4 . . . no Co(1) N(4) H(6) 109.4 . . . no C(6) N(4) H(5) 109.4 . . . no C(6) N(4) H(6) 109.4 . . . no H(5) N(4) H(6) 109.5 . . . no O(2) N(5) C(7) 119.4(4) . . . yes O(2) N(5) H(7) 120.3 . . . no C(7) N(5) H(7) 120.3 . . . no N(1) C(1) C(2) 108.8(4) . . . yes N(1) C(1) H(8) 109.6 . . . no N(1) C(1) H(9) 109.6 . . . no C(2) C(1) H(8) 109.6 . . . no C(2) C(1) H(9) 109.6 . . . no H(8) C(1) H(9) 109.5 . . . no N(3) C(2) C(1) 109.1(5) . . . yes N(3) C(2) H(10) 109.5 . . . no N(3) C(2) H(11) 109.5 . . . no C(1) C(2) H(10) 109.6 . . . no C(1) C(2) H(11) 109.6 . . . no H(10) C(2) H(11) 109.5 . . . no N(1) C(3) C(4) 110.7(4) . . . yes N(1) C(3) H(12) 109.2 . . . no N(1) C(3) H(13) 109.2 . . . no C(4) C(3) H(12) 109.2 . . . no C(4) C(3) H(13) 109.2 . . . no H(12) C(3) H(13) 109.5 . . . no N(2) C(4) C(3) 108.3(4) . . . yes N(2) C(4) H(14) 109.7 . . . no N(2) C(4) H(15) 109.8 . . . no C(3) C(4) H(14) 109.8 . . . no C(3) C(4) H(15) 109.8 . . . no H(14) C(4) H(15) 109.5 . . . no N(1) C(5) C(6) 109.8(4) . . . yes N(1) C(5) H(16) 109.4 . . . no N(1) C(5) H(17) 109.4 . . . no C(6) C(5) H(16) 109.4 . . . no C(6) C(5) H(17) 109.4 . . . no H(16) C(5) H(17) 109.5 . . . no N(4) C(6) C(5) 110.1(5) . . . yes N(4) C(6) H(18) 109.3 . . . no N(4) C(6) H(19) 109.3 . . . no C(5) C(6) H(18) 109.3 . . . no C(5) C(6) H(19) 109.3 . . . no H(18) C(6) H(19) 109.5 . . . no O(1) C(7) N(5) 117.8(5) . . . yes O(1) C(7) C(8) 121.9(5) . . . yes N(5) C(7) C(8) 120.2(5) . . . yes C(7) C(8) H(20) 109.5 . . . no C(7) C(8) H(21) 109.5 . . . no C(7) C(8) H(22) 109.5 . . . no H(20) C(8) H(21) 109.5 . . . no H(20) C(8) H(22) 109.5 . . . no H(21) C(8) H(22) 109.5 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) N(2) 3.160(5) . 2_566 no O(1) O(5) 3.164(6) . . no O(1) O(3) 3.261(6) . . no O(1) O(8) 3.543(6) . 1_455 no O(2) C(1) 3.353(6) . 2_565 no O(2) O(7) 3.496(6) . . no O(2) C(5) 3.529(7) . 2_565 no O(3) N(3) 3.171(6) . . no O(3) N(4) 3.241(7) . 2_566 no O(3) O(6) 3.276(7) . 2_666 no O(3) N(2) 3.309(6) . . no O(3) O(3) 3.37(1) . 2_666 no O(4) C(6) 3.224(8) . 2_566 no O(4) N(4) 3.253(7) . 2_566 no O(4) C(4) 3.334(7) . 1_545 no O(4) O(4) 3.37(1) . 2_556 no O(4) C(8) 3.429(8) . 2_556 no O(4) C(4) 3.558(8) . 2_566 no O(5) C(7) 3.177(7) . . no O(5) N(3) 3.277(7) . . no O(5) C(8) 3.360(8) . . no O(5) C(3) 3.414(7) . 1_545 no O(5) C(4) 3.469(7) . 1_545 no O(5) O(8) 3.516(7) . . no O(6) N(2) 3.005(6) . 2_666 no O(6) C(4) 3.205(7) . 2_666 no O(6) N(3) 3.387(6) . 2_666 no O(6) C(3) 3.405(7) . 2_666 no O(6) C(4) 3.458(8) . 1_545 no O(6) C(2) 3.467(7) . 2_666 no O(6) C(3) 3.523(7) . 1_545 no O(7) N(3) 3.135(7) . . no O(7) C(5) 3.295(7) . 2_565 no O(7) N(5) 3.415(7) . . no O(7) C(2) 3.444(8) . . no O(8) N(4) 3.176(7) . 1_655 no O(8) C(7) 3.212(7) . 1_655 no O(8) N(3) 3.390(6) . . no O(8) C(8) 3.425(8) . 1_655 no O(8) N(5) 3.438(7) . 1_655 no O(8) C(2) 3.505(7) . . no O(9) C(1) 3.226(7) . 2_665 no O(9) N(5) 3.436(8) . 1_655 no O(9) C(2) 3.557(7) . 2_665 no O(9) C(6) 3.581(8) . 2_565 no O(10) N(5) 3.023(6) . 2 no O(10) O(10) 3.47(1) . 2_655 no O(10) C(5) 3.504(8) . 1_545 no O(10) C(8) 3.516(8) . 1_655 no O(10) C(1) 3.528(7) . 1_545 no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Co(1) O(1) C(7) N(5) . . . . -1.6(6) no Co(1) O(1) C(7) C(8) . . . . -178.8(4) no Co(1) O(2) N(5) C(7) . . . . 5.1(5) no Co(1) N(1) C(1) C(2) . . . . -45.3(5) no Co(1) N(1) C(3) C(4) . . . . -24.3(5) no Co(1) N(1) C(5) C(6) . . . . 42.4(5) no Co(1) N(3) C(2) C(1) . . . . -16.6(5) no Co(1) N(2) C(4) C(3) . . . . -36.7(5) no Co(1) N(4) C(6) C(5) . . . . 19.7(6) no O(1) Co(1) O(2) N(5) . . . . -4.5(3) no O(1) Co(1) N(1) C(1) . . . . -113(6) no O(1) Co(1) N(1) C(3) . . . . 128(6) no O(1) Co(1) N(1) C(5) . . . . 6(6) no O(1) Co(1) N(3) C(2) . . . . 172.0(3) no O(1) Co(1) N(2) C(4) . . . . -159.3(3) no O(1) Co(1) N(4) C(6) . . . . -175.7(4) no O(1) C(7) N(5) O(2) . . . . -2.5(7) no O(2) Co(1) O(1) C(7) . . . . 3.6(3) no O(2) Co(1) N(1) C(1) . . . . -57.2(3) no O(2) Co(1) N(1) C(3) . . . . -176.5(3) no O(2) Co(1) N(1) C(5) . . . . 61.6(4) no O(2) Co(1) N(3) C(2) . . . . 86.1(3) no O(2) Co(1) N(2) C(4) . . . . 167(9) no O(2) Co(1) N(4) C(6) . . . . -89.5(4) no O(2) N(5) C(7) C(8) . . . . 174.8(5) no N(1) Co(1) O(1) C(7) . . . . 59(6) no N(1) Co(1) O(2) N(5) . . . . 176.8(3) no N(1) Co(1) N(3) C(2) . . . . -7.0(3) no N(1) Co(1) N(2) C(4) . . . . 19.4(4) no N(1) Co(1) N(4) C(6) . . . . 3.5(4) no N(1) C(1) C(2) N(3) . . . . 40.4(6) no N(1) C(3) C(4) N(2) . . . . 39.9(6) no N(1) C(5) C(6) N(4) . . . . -40.8(7) no N(3) Co(1) O(1) C(7) . . . . -82.5(4) no N(3) Co(1) O(2) N(5) . . . . 90.7(3) no N(3) Co(1) N(1) C(1) . . . . 29.0(3) no N(3) Co(1) N(1) C(3) . . . . -90.3(3) no N(3) Co(1) N(1) C(5) . . . . 147.8(4) no N(3) Co(1) N(2) C(4) . . . . 105.6(4) no N(3) Co(1) N(4) C(6) . . . . -45(1) no N(2) Co(1) O(1) C(7) . . . . -175.9(3) no N(2) Co(1) O(2) N(5) . . . . 30(9) no N(2) Co(1) N(1) C(1) . . . . 122.3(3) no N(2) Co(1) N(1) C(3) . . . . 2.9(3) no N(2) Co(1) N(1) C(5) . . . . -118.9(4) no N(2) Co(1) N(3) C(2) . . . . -94.8(3) no N(2) Co(1) N(4) C(6) . . . . 91.3(4) no N(4) Co(1) O(1) C(7) . . . . 90.3(4) no N(4) Co(1) O(2) N(5) . . . . -96.0(3) no N(4) Co(1) N(1) C(1) . . . . -143.9(3) no N(4) Co(1) N(1) C(3) . . . . 96.8(3) no N(4) Co(1) N(1) C(5) . . . . -25.1(4) no N(4) Co(1) N(3) C(2) . . . . 41(1) no N(4) Co(1) N(2) C(4) . . . . -67.8(4) no C(1) N(1) C(3) C(4) . . . . -141.5(4) no C(1) N(1) C(5) C(6) . . . . 158.3(5) no C(2) C(1) N(1) C(3) . . . . 73.7(5) no C(2) C(1) N(1) C(5) . . . . -161.1(4) no C(3) N(1) C(5) C(6) . . . . -77.7(6) no C(4) C(3) N(1) C(5) . . . . 94.0(5) no #------------------------------------------------------------------------------ data_4 _database_code_depnum_ccdc_archive 'CCDC 866268' #TrackingRef '- combined revised cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H27 Co N4 O2, 2(Cl0.70 I0.30 O2.80)' _chemical_formula_sum 'C16 H27 Cl1.40 Co I0.60 N4 O7.60' _chemical_formula_weight 581.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.139(2) _cell_length_b 14.370(3) _cell_length_c 15.118(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2202.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9934 _cell_measurement_theta_min 2.4185 _cell_measurement_theta_max 27.836 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1178 _exptl_absorpt_coefficient_mu 1.838 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.649 _exptl_absorpt_correction_T_max 0.759 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; ? ; _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 219 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.07 _diffrn_reflns_number 22247 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 28.37 _reflns_number_total 5347 _reflns_number_gt 4869 _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., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997), WINGX-32 (Farrugia, 1999)' _computing_publication_material 'enCIFer (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^)+(0.0421P)^2^+0.4812P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(5) _refine_ls_number_reflns 5347 _refine_ls_number_parameters 308 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0777 _refine_ls_wR_factor_gt 0.0756 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 3.474 _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 1.6111(11) 1.0685(8) 0.8569(7) 0.036(2) Uani 1 1 d . . . H1A H 1.5803 1.1188 0.8173 0.043 Uiso 1 1 calc R . . H1B H 1.5458 1.0173 0.8544 0.043 Uiso 1 1 calc R . . C2 C 1.6196(12) 1.1045(9) 0.9493(8) 0.046(3) Uani 1 1 d . . . H2A H 1.5310 1.1047 0.9769 0.055 Uiso 1 1 calc R . . H2B H 1.6538 1.1690 0.9492 0.055 Uiso 1 1 calc R . . C3 C 1.8178(11) 1.1047(7) 0.7739(7) 0.035(2) Uani 1 1 d . . . H3A H 1.7580 1.1360 0.7315 0.043 Uiso 1 1 calc R . . H3B H 1.8895 1.0745 0.7400 0.043 Uiso 1 1 calc R . . C4 C 1.8744(12) 1.1746(7) 0.8366(8) 0.043(3) Uani 1 1 d . . . H4A H 1.9463 1.2094 0.8072 0.052 Uiso 1 1 calc R . . H4B H 1.8053 1.2195 0.8543 0.052 Uiso 1 1 calc R . . C5 C 1.7247(11) 0.9451(7) 0.7737(6) 0.031(2) Uani 1 1 d . . . H5A H 1.8060 0.9305 0.7402 0.037 Uiso 1 1 calc R . . H5B H 1.6515 0.9527 0.7310 0.037 Uiso 1 1 calc R . . C6 C 1.6937(11) 0.8669(7) 0.8371(7) 0.034(2) Uani 1 1 d . . . H6A H 1.6014 0.8721 0.8581 0.040 Uiso 1 1 calc R . . H6B H 1.7045 0.8061 0.8072 0.040 Uiso 1 1 calc R . . C7 C 2.0948(10) 0.8899(7) 1.1199(6) 0.032(2) Uani 1 1 d . . . H7A H 2.0700 0.9351 1.1655 0.048 Uiso 1 1 calc R . . H7B H 2.1905 0.8802 1.1213 0.048 Uiso 1 1 calc R . . H7C H 2.0499 0.8307 1.1312 0.048 Uiso 1 1 calc R . . C8 C 2.0553(9) 0.9260(6) 1.0309(6) 0.0241(18) Uani 1 1 d . . . C9 C 2.1346(10) 0.9086(6) 0.9573(6) 0.0269(19) Uani 1 1 d . . . H9 H 2.2185 0.8812 0.9677 0.032 Uiso 1 1 calc R . . C10 C 2.1009(9) 0.9279(6) 0.8704(6) 0.0230(18) Uani 1 1 d . . . C11 C 2.1895(9) 0.9050(6) 0.7955(6) 0.0242(18) Uani 1 1 d . . . C12 C 2.1564(10) 0.9361(7) 0.7109(6) 0.031(2) Uani 1 1 d . . . H12 H 2.0784 0.9716 0.7025 0.037 Uiso 1 1 calc R . . C13 C 2.2365(11) 0.9155(7) 0.6387(7) 0.034(2) Uani 1 1 d . . . H13 H 2.2129 0.9367 0.5813 0.040 Uiso 1 1 calc R . . C14 C 2.3504(11) 0.8643(7) 0.6509(7) 0.033(2) Uani 1 1 d . . . H14 H 2.4056 0.8505 0.6019 0.039 Uiso 1 1 calc R . . C15 C 2.3842(9) 0.8330(7) 0.7345(7) 0.031(2) Uani 1 1 d . . . H15 H 2.4626 0.7977 0.7426 0.038 Uiso 1 1 calc R . . C16 C 2.3043(10) 0.8530(7) 0.8065(7) 0.030(2) Uani 1 1 d . . . H16 H 2.3280 0.8310 0.8636 0.036 Uiso 1 1 calc R . . N1 N 1.7433(7) 1.0333(6) 0.8252(5) 0.0266(17) Uani 1 1 d . . . N2 N 1.7105(8) 1.0424(5) 1.0004(5) 0.0264(16) Uani 1 1 d . . . H2C H 1.6646 0.9917 1.0212 0.032 Uiso 1 1 calc R . . H2D H 1.7439 1.0742 1.0482 0.032 Uiso 1 1 calc R . . N3 N 1.9269(8) 1.1266(6) 0.9164(6) 0.0336(19) Uani 1 1 d . . . H3C H 1.9049 1.1600 0.9662 0.040 Uiso 1 1 calc R . . H3D H 2.0174 1.1235 0.9132 0.040 Uiso 1 1 calc R . . N4 N 1.7867(8) 0.8743(5) 0.9134(5) 0.0268(16) Uani 1 1 d . . . H4C H 1.8560 0.8339 0.9051 0.032 Uiso 1 1 calc R . . H4D H 1.7439 0.8574 0.9646 0.032 Uiso 1 1 calc R . . O1 O 1.9440(7) 0.9691(5) 1.0297(4) 0.0273(14) Uani 1 1 d . . . O2 O 1.9903(7) 0.9648(5) 0.8478(4) 0.0270(13) Uani 1 1 d . . . O3 O 1.9540(10) 0.7168(7) 1.0065(6) 0.035(2) Uani 0.70 1 d PD A 1 O4 O 2.1440(9) 0.6732(7) 0.9279(6) 0.035(2) Uani 0.70 1 d PD A 1 O5 O 1.9461(12) 0.7019(11) 0.8541(7) 0.057(4) Uani 0.70 1 d PD A 1 O6 O 1.9700(13) 0.5691(8) 0.9463(12) 0.065(4) Uani 0.70 1 d PD A 1 Cl1 Cl 2.005(3) 0.6644(19) 0.9325(18) 0.0312(12) Uani 0.70 1 d PD A 1 O7 O 2.2165(14) 1.1426(10) 0.9271(10) 0.079(5) Uani 0.70 1 d PD B 1 O8 O 2.3377(13) 1.1852(9) 0.8044(7) 0.053(3) Uani 0.70 1 d PD B 1 O9 O 2.1743(13) 1.2837(9) 0.8610(9) 0.065(4) Uani 0.70 1 d PD B 1 O10 O 2.3716(15) 1.2593(15) 0.9354(12) 0.116(8) Uani 0.70 1 d PD B 1 Cl2 Cl 2.273(3) 1.2187(17) 0.8832(17) 0.0329(15) Uani 0.70 1 d PD B 1 Co1 Co 1.85423(11) 1.00085(8) 0.92531(7) 0.0213(3) Uani 1 1 d . . . I1 I 1.9950(16) 0.6584(12) 0.9386(11) 0.0312(12) Uani 0.30 1 d P C 2 I2 I 2.2793(16) 1.2281(10) 0.8936(10) 0.0329(15) Uani 0.30 1 d P D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.029(5) 0.047(6) 0.032(5) -0.003(5) -0.002(4) 0.016(5) C2 0.040(6) 0.053(7) 0.044(6) -0.005(6) 0.002(5) 0.021(5) C3 0.039(6) 0.033(5) 0.034(5) 0.013(4) 0.004(4) 0.011(4) C4 0.044(6) 0.028(5) 0.058(7) 0.011(5) 0.003(6) -0.001(5) C5 0.032(5) 0.038(5) 0.022(4) -0.008(4) -0.003(4) 0.001(4) C6 0.040(6) 0.034(5) 0.027(5) -0.008(4) -0.004(4) -0.007(4) C7 0.036(5) 0.033(5) 0.027(5) 0.004(4) -0.003(4) 0.001(4) C8 0.026(4) 0.018(4) 0.028(5) 0.000(3) -0.004(4) -0.006(4) C9 0.026(4) 0.028(5) 0.027(4) 0.001(4) -0.004(4) 0.005(4) C10 0.022(4) 0.019(4) 0.028(4) 0.000(3) 0.001(3) -0.002(3) C11 0.023(4) 0.020(4) 0.030(5) -0.002(3) 0.003(4) -0.003(3) C12 0.034(5) 0.027(5) 0.033(5) 0.005(4) 0.006(4) 0.007(4) C13 0.040(6) 0.029(5) 0.031(5) 0.003(4) 0.010(4) 0.003(4) C14 0.031(5) 0.030(5) 0.038(5) -0.005(4) 0.010(4) -0.005(4) C15 0.019(4) 0.032(5) 0.043(6) -0.008(4) 0.001(4) -0.001(4) C16 0.026(5) 0.031(5) 0.033(5) -0.005(4) -0.004(4) 0.000(4) N1 0.026(4) 0.030(4) 0.024(4) 0.001(3) 0.000(3) 0.006(3) N2 0.030(4) 0.024(4) 0.025(4) -0.004(3) 0.001(3) 0.001(3) N3 0.030(4) 0.025(4) 0.046(5) -0.001(4) 0.004(4) -0.002(3) N4 0.032(4) 0.023(4) 0.026(4) -0.002(3) 0.002(3) 0.002(3) O1 0.028(3) 0.030(3) 0.024(3) -0.003(3) -0.003(3) 0.004(3) O2 0.022(3) 0.033(3) 0.026(3) 0.002(3) -0.001(3) 0.005(3) O3 0.042(6) 0.035(6) 0.029(5) -0.001(4) 0.008(4) -0.003(5) O4 0.028(5) 0.052(6) 0.027(5) 0.002(4) -0.001(4) -0.001(5) O5 0.054(7) 0.090(10) 0.027(5) -0.014(6) -0.014(5) 0.041(7) O6 0.050(8) 0.025(6) 0.121(13) -0.016(7) -0.006(8) -0.002(5) Cl1 0.028(2) 0.032(2) 0.033(2) -0.0048(15) -0.0039(16) 0.0041(16) O7 0.050(7) 0.087(10) 0.099(11) 0.064(9) 0.015(8) -0.001(8) O8 0.060(8) 0.061(8) 0.038(6) -0.007(5) 0.009(6) 0.015(6) O9 0.070(9) 0.052(8) 0.073(9) 0.020(7) 0.023(7) 0.023(7) O10 0.058(9) 0.17(2) 0.122(15) -0.107(15) 0.008(10) -0.039(11) Cl2 0.0304(15) 0.034(3) 0.035(3) 0.003(2) 0.0008(19) -0.0045(17) Co1 0.0213(5) 0.0209(5) 0.0218(5) -0.0005(5) -0.0001(4) 0.0023(5) I1 0.028(2) 0.032(2) 0.033(2) -0.0048(15) -0.0039(16) 0.0041(16) I2 0.0304(15) 0.034(3) 0.035(3) 0.003(2) 0.0008(19) -0.0045(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.492(15) . ? C1 N1 1.511(12) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N2 1.498(14) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N1 1.492(13) . ? C3 C4 1.496(17) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N3 1.488(14) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 N1 1.499(12) . ? C5 C6 1.510(14) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N4 1.494(12) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.497(13) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 O1 1.287(12) . ? C8 C9 1.395(13) . ? C9 C10 1.386(13) . ? C9 H9 0.9500 . ? C10 O2 1.287(11) . ? C10 C11 1.483(12) . ? C11 C16 1.393(13) . ? C11 C12 1.395(14) . ? C12 C13 1.392(13) . ? C12 H12 0.9500 . ? C13 C14 1.383(15) . ? C13 H13 0.9500 . ? C14 C15 1.384(15) . ? C14 H14 0.9500 . ? C15 C16 1.387(14) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? N1 Co1 1.942(8) . ? N2 Co1 1.941(8) . ? N2 H2C 0.9200 . ? N2 H2D 0.9200 . ? N3 Co1 1.956(8) . ? N3 H3C 0.9200 . ? N3 H3D 0.9200 . ? N4 Co1 1.952(8) . ? N4 H4C 0.9200 . ? N4 H4D 0.9200 . ? O1 Co1 1.878(7) . ? O2 Co1 1.883(6) . ? O3 Cl1 1.45(3) . ? O4 Cl1 1.41(3) . ? O5 Cl1 1.43(3) . ? O6 Cl1 1.43(3) . ? O7 Cl2 1.40(3) . ? O8 Cl2 1.44(2) . ? O9 Cl2 1.41(3) . ? O10 Cl2 1.40(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 N1 111.2(9) . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1B 109.4 . . ? N1 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? C1 C2 N2 108.2(9) . . ? C1 C2 H2A 110.1 . . ? N2 C2 H2A 110.1 . . ? C1 C2 H2B 110.1 . . ? N2 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? N1 C3 C4 109.0(8) . . ? N1 C3 H3A 109.9 . . ? C4 C3 H3A 109.9 . . ? N1 C3 H3B 109.9 . . ? C4 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? N3 C4 C3 109.9(8) . . ? N3 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? N3 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? N1 C5 C6 109.0(7) . . ? N1 C5 H5A 109.9 . . ? C6 C5 H5A 109.9 . . ? N1 C5 H5B 109.9 . . ? C6 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? N4 C6 C5 107.8(8) . . ? N4 C6 H6A 110.1 . . ? C5 C6 H6A 110.1 . . ? N4 C6 H6B 110.1 . . ? C5 C6 H6B 110.1 . . ? H6A C6 H6B 108.5 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O1 C8 C9 125.5(9) . . ? O1 C8 C7 114.5(8) . . ? C9 C8 C7 120.0(9) . . ? C10 C9 C8 125.3(9) . . ? C10 C9 H9 117.4 . . ? C8 C9 H9 117.4 . . ? O2 C10 C9 123.3(9) . . ? O2 C10 C11 114.6(8) . . ? C9 C10 C11 122.0(8) . . ? C16 C11 C12 118.8(9) . . ? C16 C11 C10 122.3(8) . . ? C12 C11 C10 118.9(8) . . ? C13 C12 C11 120.7(9) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C14 C13 C12 119.7(10) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C15 120.1(9) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C16 120.3(9) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C11 120.4(9) . . ? C15 C16 H16 119.8 . . ? C11 C16 H16 119.8 . . ? C3 N1 C5 112.0(8) . . ? C3 N1 C1 112.6(8) . . ? C5 N1 C1 109.6(8) . . ? C3 N1 Co1 106.1(6) . . ? C5 N1 Co1 105.9(6) . . ? C1 N1 Co1 110.3(6) . . ? C2 N2 Co1 110.1(6) . . ? C2 N2 H2C 109.6 . . ? Co1 N2 H2C 109.6 . . ? C2 N2 H2D 109.6 . . ? Co1 N2 H2D 109.6 . . ? H2C N2 H2D 108.2 . . ? C4 N3 Co1 110.4(7) . . ? C4 N3 H3C 109.6 . . ? Co1 N3 H3C 109.6 . . ? C4 N3 H3D 109.6 . . ? Co1 N3 H3D 109.6 . . ? H3C N3 H3D 108.1 . . ? C6 N4 Co1 111.0(6) . . ? C6 N4 H4C 109.4 . . ? Co1 N4 H4C 109.4 . . ? C6 N4 H4D 109.4 . . ? Co1 N4 H4D 109.4 . . ? H4C N4 H4D 108.0 . . ? C8 O1 Co1 123.6(6) . . ? C10 O2 Co1 125.9(6) . . ? O4 Cl1 O6 109.9(19) . . ? O4 Cl1 O5 110.0(19) . . ? O6 Cl1 O5 112(2) . . ? O4 Cl1 O3 110.4(19) . . ? O6 Cl1 O3 107.2(19) . . ? O5 Cl1 O3 107.1(18) . . ? O10 Cl2 O7 110(2) . . ? O10 Cl2 O9 111(2) . . ? O7 Cl2 O9 109.8(19) . . ? O10 Cl2 O8 106.3(19) . . ? O7 Cl2 O8 108.5(18) . . ? O9 Cl2 O8 110.4(18) . . ? O1 Co1 O2 95.8(3) . . ? O1 Co1 N2 87.0(3) . . ? O2 Co1 N2 177.0(3) . . ? O1 Co1 N1 173.6(3) . . ? O2 Co1 N1 90.3(3) . . ? N2 Co1 N1 87.0(3) . . ? O1 Co1 N4 91.2(3) . . ? O2 Co1 N4 86.7(3) . . ? N2 Co1 N4 94.5(3) . . ? N1 Co1 N4 87.1(3) . . ? O1 Co1 N3 95.7(4) . . ? O2 Co1 N3 86.3(3) . . ? N2 Co1 N3 92.2(4) . . ? N1 Co1 N3 86.7(4) . . ? N4 Co1 N3 170.6(4) . . ? 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 N1 C1 C2 N2 -38.3(13) . . . . ? N1 C3 C4 N3 41.0(12) . . . . ? N1 C5 C6 N4 -44.7(11) . . . . ? O1 C8 C9 C10 -5.8(15) . . . . ? C7 C8 C9 C10 171.4(9) . . . . ? C8 C9 C10 O2 -0.1(15) . . . . ? C8 C9 C10 C11 -178.4(9) . . . . ? O2 C10 C11 C16 -170.7(8) . . . . ? C9 C10 C11 C16 7.8(14) . . . . ? O2 C10 C11 C12 8.9(12) . . . . ? C9 C10 C11 C12 -172.6(9) . . . . ? C16 C11 C12 C13 0.0(15) . . . . ? C10 C11 C12 C13 -179.6(9) . . . . ? C11 C12 C13 C14 -0.4(15) . . . . ? C12 C13 C14 C15 0.4(15) . . . . ? C13 C14 C15 C16 -0.1(15) . . . . ? C14 C15 C16 C11 -0.3(15) . . . . ? C12 C11 C16 C15 0.3(15) . . . . ? C10 C11 C16 C15 179.9(9) . . . . ? C4 C3 N1 C5 -159.8(8) . . . . ? C4 C3 N1 C1 76.1(10) . . . . ? C4 C3 N1 Co1 -44.7(9) . . . . ? C6 C5 N1 C3 160.3(8) . . . . ? C6 C5 N1 C1 -73.9(10) . . . . ? C6 C5 N1 Co1 45.1(9) . . . . ? C2 C1 N1 C3 -95.4(11) . . . . ? C2 C1 N1 C5 139.2(10) . . . . ? C2 C1 N1 Co1 22.9(11) . . . . ? C1 C2 N2 Co1 36.4(12) . . . . ? C3 C4 N3 Co1 -17.5(11) . . . . ? C5 C6 N4 Co1 23.1(9) . . . . ? C9 C8 O1 Co1 9.8(13) . . . . ? C7 C8 O1 Co1 -167.5(6) . . . . ? C9 C10 O2 Co1 0.6(13) . . . . ? C11 C10 O2 Co1 179.1(6) . . . . ? C8 O1 Co1 O2 -7.3(7) . . . . ? C8 O1 Co1 N2 173.9(7) . . . . ? C8 O1 Co1 N1 154(3) . . . . ? C8 O1 Co1 N4 79.5(7) . . . . ? C8 O1 Co1 N3 -94.2(7) . . . . ? C10 O2 Co1 O1 2.4(7) . . . . ? C10 O2 Co1 N2 158(6) . . . . ? C10 O2 Co1 N1 -175.6(7) . . . . ? C10 O2 Co1 N4 -88.5(7) . . . . ? C10 O2 Co1 N3 97.7(7) . . . . ? C2 N2 Co1 O1 162.6(8) . . . . ? C2 N2 Co1 O2 6(7) . . . . ? C2 N2 Co1 N1 -19.6(8) . . . . ? C2 N2 Co1 N4 -106.4(8) . . . . ? C2 N2 Co1 N3 67.0(8) . . . . ? C3 N1 Co1 O1 141(3) . . . . ? C5 N1 Co1 O1 -100(3) . . . . ? C1 N1 Co1 O1 18(3) . . . . ? C3 N1 Co1 O2 -58.1(6) . . . . ? C5 N1 Co1 O2 61.1(6) . . . . ? C1 N1 Co1 O2 179.6(7) . . . . ? C3 N1 Co1 N2 120.5(6) . . . . ? C5 N1 Co1 N2 -120.2(6) . . . . ? C1 N1 Co1 N2 -1.7(7) . . . . ? C3 N1 Co1 N4 -144.8(6) . . . . ? C5 N1 Co1 N4 -25.6(6) . . . . ? C1 N1 Co1 N4 92.9(7) . . . . ? C3 N1 Co1 N3 28.1(6) . . . . ? C5 N1 Co1 N3 147.4(6) . . . . ? C1 N1 Co1 N3 -94.1(7) . . . . ? C6 N4 Co1 O1 175.3(6) . . . . ? C6 N4 Co1 O2 -89.0(6) . . . . ? C6 N4 Co1 N2 88.2(7) . . . . ? C6 N4 Co1 N1 1.5(6) . . . . ? C6 N4 Co1 N3 -47(2) . . . . ? C4 N3 Co1 O1 179.7(7) . . . . ? C4 N3 Co1 O2 84.3(7) . . . . ? C4 N3 Co1 N2 -93.1(7) . . . . ? C4 N3 Co1 N1 -6.2(7) . . . . ? C4 N3 Co1 N4 42(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2C O6 0.92 2.21 3.027(16) 147.1 3_467 N2 H2C O4 0.92 2.50 3.350(13) 153.9 3_467 N2 H2C I1 0.92 2.83 3.736(19) 170.5 3_467 N3 H3D I2 0.92 3.07 3.875(18) 147.7 . N3 H3D O7 0.92 2.05 2.950(17) 166.2 . N3 H3D I2 0.92 3.07 3.875(18) 147.7 . N4 H4C O5 0.92 2.24 3.090(14) 153.1 . N4 H4C O3 0.92 2.48 3.159(13) 130.4 . N4 H4C I1 0.92 2.93 3.771(19) 152.3 . N4 H4D O4 0.92 1.97 2.884(12) 176.5 3_467 N4 H4D Cl1 0.92 2.89 3.73(3) 151.1 3_467 N4 H4D I1 0.92 2.93 3.738(19) 148.0 3_467 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.609 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.074 data_5 _database_code_depnum_ccdc_archive 'CCDC 866269' #TrackingRef '- combined revised cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' C11 H25 Co N4 O2, 2(Cl), 2(H2 O)' _chemical_formula_sum 'C11 H29 Cl2 Co N4 O4' _chemical_formula_weight 411.21 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1 ' _symmetry_space_group_name_Hall 'P 1' _symmetry_Int_Tables_number 1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 7.779(3) _cell_length_b 7.864(3) _cell_length_c 8.045(3) _cell_angle_alpha 100.627(6) _cell_angle_beta 106.855(6) _cell_angle_gamma 102.071(6) _cell_volume 444.5(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3380 _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 27.99 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.339 _exptl_crystal_size_mid 0.255 _exptl_crystal_size_min 0.129 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 212 _exptl_absorpt_coefficient_mu 1.286 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _diffrn_crystal_treatment ; attached with Exxon Paratone N, to a short length of fibre supported on a thin piece of copper wire inserted in a copper mounting pin. The crystal was quenched in a cold nitrogen gas stream from an Oxford Cryosystems Cryostream. ; _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 88 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.04 _diffrn_reflns_number 4102 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0155 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 27.95 _reflns_number_total 3778 _reflns_number_gt 3772 _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 ; xtal 3.6 (Hall,du Boulay, D.J. & Olthof-Hazekamp, R. 1999) ORTEPII (Johnson,C.K., 1976). WinGX (Farrugia, 1999) ; _computing_publication_material ? _refine_special_details ; Twinned by 2 fold rotation about 0 0 1 Nine batch scale factors refined for overlapping reflections. 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^)+(0.08P)^2^+0.5P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.40(5) _refine_ls_number_reflns 3778 _refine_ls_number_parameters 212 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1505 _refine_ls_wR_factor_gt 0.1505 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.78996(8) 0.66743(9) 0.32979(9) 0.0117(2) Uani 1 1 d . . . O1 O 0.8058(8) 0.4879(12) 0.1458(13) 0.0170(13) Uani 1 1 d . . . O2 O 0.5240(7) 0.5987(9) 0.2518(10) 0.0156(12) Uani 1 1 d . . . N1 N 0.7998(10) 0.8553(14) 0.5266(13) 0.0161(15) Uani 1 1 d . . . N2 N 1.0608(9) 0.7441(12) 0.4142(13) 0.0148(14) Uani 1 1 d . . . H2A H 1.1064 0.6693 0.4757 0.018 Uiso 1 1 calc R . . H2B H 1.1010 0.7405 0.3198 0.018 Uiso 1 1 calc R . . N3 N 0.7800(18) 0.5094(16) 0.4909(16) 0.014(2) Uani 1 1 d . . . H3A H 0.6767 0.4154 0.4384 0.016 Uiso 1 1 calc R . . H3B H 0.8802 0.4658 0.5095 0.016 Uiso 1 1 calc R . . N4 N 0.7706(17) 0.8402(16) 0.1803(17) 0.018(3) Uani 1 1 d . . . H4A H 0.8694 0.8591 0.1425 0.021 Uiso 1 1 calc R . . H4B H 0.6658 0.7950 0.0829 0.021 Uiso 1 1 calc R . . C1 C 0.7127(11) 0.2290(17) -0.0956(17) 0.028(2) Uani 1 1 d . . . H1A H 0.8188 0.2902 -0.1210 0.042 Uiso 1 1 calc R . . H1B H 0.6076 0.1791 -0.2053 0.042 Uiso 1 1 calc R . . H1C H 0.7417 0.1340 -0.0429 0.042 Uiso 1 1 calc R . . C2 C 0.6649(11) 0.3626(13) 0.0356(13) 0.0176(17) Uani 1 1 d . . . C3 C 0.4826(12) 0.3415(14) 0.0244(14) 0.021(2) Uani 1 1 d . . . H3 H 0.3933 0.2400 -0.0581 0.026 Uiso 1 1 calc R . . C4 C 0.4206(11) 0.4626(12) 0.1288(12) 0.0182(19) Uani 1 1 d . . . C5 C 0.2150(10) 0.4256(15) 0.0961(16) 0.026(2) Uani 1 1 d . . . H5A H 0.1802 0.5360 0.0982 0.039 Uiso 1 1 calc R . . H5B H 0.1862 0.3757 0.1883 0.039 Uiso 1 1 calc R . . H5C H 0.1467 0.3414 -0.0193 0.039 Uiso 1 1 calc R . . C6 C 0.9991(11) 0.9578(16) 0.6404(16) 0.0187(17) Uani 1 1 d . . . H6A H 1.0363 0.9147 0.7471 0.022 Uiso 1 1 calc R . . H6B H 1.0082 1.0848 0.6786 0.022 Uiso 1 1 calc R . . C7 C 1.1298(12) 0.9337(12) 0.5346(12) 0.0182(19) Uani 1 1 d . . . H7A H 1.1321 1.0198 0.4624 0.022 Uiso 1 1 calc R . . H7B H 1.2558 0.9548 0.6166 0.022 Uiso 1 1 calc R . . C8 C 0.705(2) 0.7652(18) 0.6388(17) 0.018(3) Uani 1 1 d . . . H8A H 0.7328 0.8487 0.7544 0.022 Uiso 1 1 calc R . . H8B H 0.5706 0.7263 0.5783 0.022 Uiso 1 1 calc R . . C9 C 0.778(2) 0.606(2) 0.665(2) 0.026(3) Uani 1 1 d . . . H9A H 0.9028 0.6456 0.7531 0.031 Uiso 1 1 calc R . . H9B H 0.6975 0.5263 0.7080 0.031 Uiso 1 1 calc R . . C10 C 0.695(2) 0.975(2) 0.4417(19) 0.021(3) Uani 1 1 d . . . H10A H 0.7189 1.0876 0.5297 0.026 Uiso 1 1 calc R . . H10B H 0.5617 0.9168 0.3951 0.026 Uiso 1 1 calc R . . C11 C 0.766(2) 1.012(2) 0.2871(19) 0.018(3) Uani 1 1 d . . . H11A H 0.6828 1.0646 0.2111 0.022 Uiso 1 1 calc R . . H11B H 0.8898 1.0955 0.3362 0.022 Uiso 1 1 calc R . . Cl1 Cl 1.1651(5) 0.9144(4) 0.0996(4) 0.0232(8) Uani 1 1 d . . . Cl2 Cl 1.1799(4) 0.4241(4) 0.5944(4) 0.0225(7) Uani 1 1 d . . . O3 O 0.4389(15) 0.2407(14) 0.4288(16) 0.026(2) Uani 1 1 d . . . O4 O 0.4281(14) 0.7876(14) -0.1074(14) 0.024(2) 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 Co1 0.0090(4) 0.0108(10) 0.0126(11) 0.0003(3) 0.0021(7) 0.0018(6) O1 0.011(3) 0.013(5) 0.021(5) -0.003(2) 0.003(3) 0.002(3) O2 0.009(3) 0.016(4) 0.020(4) 0.002(2) 0.005(3) 0.004(3) N1 0.021(4) 0.013(5) 0.013(6) 0.001(3) 0.008(4) 0.003(4) N2 0.012(3) 0.011(5) 0.016(5) -0.001(3) 0.003(3) -0.003(3) N3 0.017(5) 0.014(5) 0.012(5) 0.000(4) 0.006(4) 0.009(4) N4 0.012(6) 0.021(6) 0.017(6) 0.007(5) 0.002(4) 0.001(4) C1 0.024(4) 0.028(7) 0.023(7) -0.006(3) 0.006(5) 0.003(5) C2 0.018(4) 0.016(5) 0.016(5) 0.002(3) 0.001(4) 0.005(4) C3 0.013(4) 0.022(6) 0.017(6) -0.009(4) 0.002(4) -0.003(4) C4 0.016(4) 0.016(5) 0.020(5) 0.005(3) 0.005(4) 0.003(3) C5 0.009(4) 0.024(6) 0.035(7) -0.003(4) 0.004(4) 0.000(4) C6 0.019(4) 0.015(6) 0.015(6) -0.001(3) 0.004(5) -0.004(5) C7 0.014(4) 0.013(4) 0.015(4) -0.002(3) -0.003(3) -0.007(3) C8 0.025(7) 0.017(6) 0.011(5) -0.001(5) 0.009(5) 0.004(5) C9 0.033(8) 0.022(6) 0.019(7) 0.009(5) 0.006(6) 0.002(5) C10 0.029(7) 0.025(7) 0.017(6) 0.010(6) 0.008(5) 0.017(6) C11 0.018(6) 0.018(6) 0.015(6) 0.004(5) 0.000(5) 0.005(5) Cl1 0.0216(19) 0.0266(17) 0.0196(17) 0.0042(15) 0.0094(15) 0.0013(14) Cl2 0.0197(18) 0.0207(17) 0.0243(18) 0.0021(14) 0.0044(14) 0.0075(14) O3 0.021(5) 0.024(5) 0.037(6) 0.008(4) 0.011(4) 0.009(4) O4 0.013(5) 0.030(5) 0.022(5) 0.003(4) 0.002(4) 0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 1.899(6) . ? Co1 O2 1.902(5) . ? Co1 N1 1.927(6) . ? Co1 N2 1.937(6) . ? Co1 N3 1.961(10) . ? Co1 N4 1.974(10) . ? O1 C2 1.273(9) . ? O2 C4 1.249(9) . ? N1 C10 1.502(17) . ? N1 C8 1.504(17) . ? N1 C6 1.508(10) . ? N2 C7 1.510(10) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 C9 1.47(2) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N4 C11 1.47(2) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? C1 C2 1.529(10) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.367(11) . ? C3 C4 1.406(10) . ? C3 H3 0.9300 . ? C4 C5 1.499(11) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.522(13) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.50(2) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.545(18) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O2 95.3(2) . . ? O1 Co1 N1 174.5(3) . . ? O2 Co1 N1 90.2(3) . . ? O1 Co1 N2 86.4(2) . . ? O2 Co1 N2 178.2(3) . . ? N1 Co1 N2 88.1(3) . . ? O1 Co1 N3 93.8(6) . . ? O2 Co1 N3 86.6(5) . . ? N1 Co1 N3 85.9(6) . . ? N2 Co1 N3 93.6(5) . . ? O1 Co1 N4 93.1(6) . . ? O2 Co1 N4 87.1(5) . . ? N1 Co1 N4 87.8(6) . . ? N2 Co1 N4 92.5(5) . . ? N3 Co1 N4 171.1(3) . . ? C2 O1 Co1 123.4(5) . . ? C4 O2 Co1 124.5(5) . . ? C10 N1 C8 111.8(7) . . ? C10 N1 C6 111.5(12) . . ? C8 N1 C6 109.5(11) . . ? C10 N1 Co1 105.8(8) . . ? C8 N1 Co1 106.9(8) . . ? C6 N1 Co1 111.2(5) . . ? C7 N2 Co1 109.4(5) . . ? C7 N2 H2A 109.8 . . ? Co1 N2 H2A 109.8 . . ? C7 N2 H2B 109.8 . . ? Co1 N2 H2B 109.8 . . ? H2A N2 H2B 108.2 . . ? C9 N3 Co1 111.6(9) . . ? C9 N3 H3A 109.3 . . ? Co1 N3 H3A 109.3 . . ? C9 N3 H3B 109.3 . . ? Co1 N3 H3B 109.3 . . ? H3A N3 H3B 108.0 . . ? C11 N4 Co1 109.4(9) . . ? C11 N4 H4A 109.8 . . ? Co1 N4 H4A 109.8 . . ? C11 N4 H4B 109.8 . . ? Co1 N4 H4B 109.8 . . ? H4A N4 H4B 108.2 . . ? 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 126.3(7) . . ? O1 C2 C1 114.1(7) . . ? C3 C2 C1 119.5(7) . . ? C2 C3 C4 124.5(7) . . ? C2 C3 H3 117.7 . . ? C4 C3 H3 117.7 . . ? O2 C4 C3 125.2(8) . . ? O2 C4 C5 116.2(7) . . ? C3 C4 C5 118.5(7) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C7 110.5(7) . . ? N1 C6 H6A 109.5 . . ? C7 C6 H6A 109.5 . . ? N1 C6 H6B 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? N2 C7 C6 108.8(7) . . ? N2 C7 H7A 109.9 . . ? C6 C7 H7A 109.9 . . ? N2 C7 H7B 109.9 . . ? C6 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? C9 C8 N1 107.6(11) . . ? C9 C8 H8A 110.2 . . ? N1 C8 H8A 110.2 . . ? C9 C8 H8B 110.2 . . ? N1 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? N3 C9 C8 108.3(11) . . ? N3 C9 H9A 110.0 . . ? C8 C9 H9A 110.0 . . ? N3 C9 H9B 110.0 . . ? C8 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? N1 C10 C11 107.1(11) . . ? N1 C10 H10A 110.3 . . ? C11 C10 H10A 110.3 . . ? N1 C10 H10B 110.3 . . ? C11 C10 H10B 110.3 . . ? H10A C10 H10B 108.6 . . ? N4 C11 C10 109.1(11) . . ? N4 C11 H11A 109.9 . . ? C10 C11 H11A 109.9 . . ? N4 C11 H11B 109.9 . . ? C10 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A Cl2 0.90 2.40 3.292(13) 168.8 . N2 H2B Cl1 0.90 2.53 3.294(12) 143.6 . N3 H3A O3 0.90 2.03 2.873(17) 154.8 . N3 H3B Cl2 0.90 2.34 3.224(12) 166.3 . N4 H4B O4 0.90 2.01 2.870(16) 158.9 . _diffrn_measured_fraction_theta_max 0.879 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.769 _refine_diff_density_min -0.940 _refine_diff_density_rms 0.133 data_6 _database_code_depnum_ccdc_archive 'CCDC 866270' #TrackingRef '- combined revised cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H28 Co N5 O2, 2(Cl O4)' _chemical_formula_sum 'C18 H28 Cl2 Co N5 O10' _chemical_formula_weight 604.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' _Int_tables_symmetry_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.2091(3) _cell_length_b 16.7587(7) _cell_length_c 17.1486(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.560(2) _cell_angle_gamma 90.00 _cell_volume 2354.65(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9999 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 30.01 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 1.022 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6688 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2007)' _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 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type APEXII-FR591 _diffrn_measurement_method \w+\f _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 38930 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 30.00 _reflns_number_total 6851 _reflns_number_gt 5628 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX (Bruker-Nonius, 2003)' _computing_cell_refinement 'SAINT (Bruker-Nonius, 2003)' _computing_data_reduction 'SAINT (Bruker-Nonius, 2003), XPREP (Bruker-Nonius, 2003)' _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) POV-Ray 3.5 (Cason, 2002) WebLab ViewerPro 3.7 (Molecular Simulations, 2000) ; _computing_publication_material 'enCIFer 1.1 (CCDC, 2005)' _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^)+(0.0704P)^2^+0.3289P] 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 6851 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.1215 _refine_ls_wR_factor_gt 0.0988 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.132 _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 0.6474(2) 0.47913(11) 0.38070(11) 0.0143(3) Uani 1 1 d . . . H1A H 0.6318 0.4964 0.4349 0.017 Uiso 1 1 calc R . . H1B H 0.6886 0.5251 0.3515 0.017 Uiso 1 1 calc R . . C2 C 0.7692(2) 0.41056(12) 0.38081(12) 0.0171(4) Uani 1 1 d . . . H2A H 0.8093 0.4037 0.3280 0.021 Uiso 1 1 calc R . . H2B H 0.8638 0.4222 0.4177 0.021 Uiso 1 1 calc R . . C3 C 0.3490(2) 0.50301(12) 0.36308(11) 0.0158(4) Uani 1 1 d . . . H3A H 0.3474 0.5521 0.3309 0.019 Uiso 1 1 calc R . . H3B H 0.3627 0.5187 0.4187 0.019 Uiso 1 1 calc R . . C4 C 0.1895(2) 0.45764(12) 0.34821(12) 0.0173(4) Uani 1 1 d . . . H4A H 0.1011 0.4844 0.3750 0.021 Uiso 1 1 calc R . . H4B H 0.1585 0.4561 0.2915 0.021 Uiso 1 1 calc R . . C5 C 0.5002(2) 0.44279(12) 0.25519(10) 0.0170(4) Uani 1 1 d . . . H5A H 0.6165 0.4387 0.2433 0.020 Uiso 1 1 calc R . . H5B H 0.4542 0.4911 0.2290 0.020 Uiso 1 1 calc R . . C6 C 0.4082(3) 0.36917(12) 0.22352(11) 0.0182(4) Uani 1 1 d . . . H6A H 0.2896 0.3801 0.2177 0.022 Uiso 1 1 calc R . . H6B H 0.4460 0.3542 0.1718 0.022 Uiso 1 1 calc R . . C7 C 0.4055(2) 0.24809(12) 0.50328(11) 0.0145(3) Uani 1 1 d . . . C8 C 0.3810(2) 0.17441(12) 0.55115(12) 0.0183(4) Uani 1 1 d . . . H8A H 0.2842 0.1453 0.5286 0.022 Uiso 1 1 calc R . . H8B H 0.3580 0.1906 0.6049 0.022 Uiso 1 1 calc R . . C9 C 0.5267(2) 0.11808(12) 0.55526(11) 0.0164(4) Uani 1 1 d . . . C10 C 0.5203(2) 0.04808(12) 0.60333(11) 0.0162(4) Uani 1 1 d . . . C11 C 0.3822(3) 0.02887(12) 0.64601(12) 0.0208(4) Uani 1 1 d . . . H11 H 0.2889 0.0625 0.6420 0.025 Uiso 1 1 calc R . . C12 C 0.3821(3) -0.03770(13) 0.69300(13) 0.0261(5) Uani 1 1 d . . . H12 H 0.2887 -0.0498 0.7208 0.031 Uiso 1 1 calc R . . C13 C 0.5199(3) -0.08812(13) 0.70013(13) 0.0292(5) Uani 1 1 d . . . H13 H 0.5202 -0.1329 0.7341 0.035 Uiso 1 1 calc R . . C14 C 0.6523(3) -0.07277(13) 0.65859(13) 0.0264(5) Uani 1 1 d . . . H14 H 0.7431 -0.1080 0.6628 0.032 Uiso 1 1 calc R . . C15 C 0.6572(3) -0.00500(12) 0.60892(11) 0.0199(4) Uani 1 1 d . . . C16 C 0.7958(3) 0.01236(14) 0.56597(13) 0.0244(4) Uani 1 1 d . . . H16 H 0.8869 -0.0227 0.5691 0.029 Uiso 1 1 calc R . . C17 C 0.7988(3) 0.07886(15) 0.52040(13) 0.0263(5) Uani 1 1 d . . . H17 H 0.8918 0.0897 0.4918 0.032 Uiso 1 1 calc R . . C18 C 0.6641(3) 0.13210(14) 0.51525(12) 0.0220(4) Uani 1 1 d . . . H18 H 0.6688 0.1784 0.4835 0.026 Uiso 1 1 calc R . . N1 N 0.48820(18) 0.45055(9) 0.34255(9) 0.0123(3) Uani 1 1 d . . . N4 N 0.68563(19) 0.33576(10) 0.40511(10) 0.0144(3) Uani 1 1 d . . . H4C H 0.7112 0.3261 0.4573 0.017 Uiso 1 1 calc R . . H4D H 0.7216 0.2932 0.3770 0.017 Uiso 1 1 calc R . . N3 N 0.21455(19) 0.37435(10) 0.37925(9) 0.0152(3) Uani 1 1 d . . . H3C H 0.1586 0.3388 0.3466 0.018 Uiso 1 1 calc R . . H3D H 0.1735 0.3707 0.4278 0.018 Uiso 1 1 calc R . . N2 N 0.4425(2) 0.30358(10) 0.28087(9) 0.0149(3) Uani 1 1 d . . . H2C H 0.5413 0.2803 0.2722 0.018 Uiso 1 1 calc R . . H2D H 0.3628 0.2651 0.2748 0.018 Uiso 1 1 calc R . . N5 N 0.4275(2) 0.31741(10) 0.53716(9) 0.0150(3) Uani 1 1 d . . . H5 H 0.4280 0.3216 0.5883 0.018 Uiso 1 1 calc R . . O2 O 0.45017(16) 0.38460(8) 0.49142(7) 0.0144(3) Uani 1 1 d . . . O1 O 0.40648(16) 0.24377(8) 0.42823(8) 0.0154(3) Uani 1 1 d . . . O3 O 1.0126(2) 0.27662(11) 0.49968(10) 0.0333(4) Uani 1 1 d . . . O4 O 0.81888(19) 0.34081(11) 0.57426(10) 0.0318(4) Uani 1 1 d . . . O5 O 1.0704(2) 0.40260(11) 0.55295(12) 0.0407(5) Uani 1 1 d . . . O6 O 1.0633(2) 0.29094(13) 0.63594(10) 0.0421(5) Uani 1 1 d . . . O7 O 0.4278(2) 0.34789(9) 0.70769(9) 0.0246(3) Uani 1 1 d . . . O8 O 0.4377(4) 0.32093(17) 0.84203(12) 0.0754(9) Uani 1 1 d . . . O9 O 0.5925(2) 0.24546(14) 0.76038(15) 0.0547(6) Uani 1 1 d . . . O10 O 0.3111(2) 0.23040(14) 0.75392(14) 0.0533(6) Uani 1 1 d . . . Cl1 Cl 0.99110(6) 0.32729(3) 0.56642(3) 0.01823(11) Uani 1 1 d . . . Cl2 Cl 0.44165(6) 0.28650(3) 0.76648(3) 0.02102(12) Uani 1 1 d . . . Co1 Co 0.44773(3) 0.346495(14) 0.386825(14) 0.01070(8) 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 0.0127(8) 0.0137(9) 0.0165(8) -0.0011(7) 0.0003(6) -0.0031(7) C2 0.0133(8) 0.0176(9) 0.0207(9) 0.0012(7) 0.0022(7) -0.0022(7) C3 0.0142(8) 0.0127(9) 0.0208(9) 0.0007(7) 0.0032(7) 0.0011(7) C4 0.0124(8) 0.0136(9) 0.0258(9) 0.0036(7) 0.0009(7) 0.0024(7) C5 0.0212(9) 0.0181(10) 0.0117(8) 0.0008(7) 0.0022(7) -0.0041(7) C6 0.0238(10) 0.0167(9) 0.0138(8) 0.0002(7) -0.0014(7) -0.0024(8) C7 0.0132(8) 0.0144(9) 0.0163(8) 0.0020(7) 0.0035(6) 0.0012(7) C8 0.0183(9) 0.0166(9) 0.0206(9) 0.0064(7) 0.0060(7) 0.0035(7) C9 0.0185(9) 0.0140(9) 0.0169(8) 0.0002(7) 0.0014(7) 0.0026(7) C10 0.0218(9) 0.0134(9) 0.0133(8) -0.0008(7) 0.0005(7) 0.0016(7) C11 0.0285(11) 0.0152(9) 0.0192(9) 0.0017(7) 0.0052(8) 0.0019(8) C12 0.0395(13) 0.0155(10) 0.0241(10) 0.0010(8) 0.0084(9) -0.0025(9) C13 0.0507(15) 0.0126(10) 0.0241(11) 0.0020(8) 0.0003(10) 0.0023(10) C14 0.0391(13) 0.0148(10) 0.0244(10) -0.0019(8) -0.0053(9) 0.0086(9) C15 0.0261(10) 0.0164(9) 0.0169(9) -0.0046(7) -0.0023(7) 0.0063(8) C16 0.0236(10) 0.0246(11) 0.0248(10) -0.0056(8) -0.0014(8) 0.0114(9) C17 0.0197(10) 0.0336(13) 0.0263(11) -0.0022(9) 0.0071(8) 0.0056(9) C18 0.0212(10) 0.0234(11) 0.0220(10) 0.0044(8) 0.0052(8) 0.0025(8) N1 0.0117(7) 0.0131(7) 0.0122(7) -0.0004(6) 0.0010(5) -0.0009(6) N4 0.0123(7) 0.0151(8) 0.0160(7) -0.0008(6) 0.0014(6) 0.0009(6) N3 0.0136(7) 0.0140(8) 0.0181(7) 0.0017(6) 0.0021(6) -0.0010(6) N2 0.0176(8) 0.0134(8) 0.0135(7) -0.0019(6) 0.0005(6) -0.0014(6) N5 0.0191(8) 0.0136(8) 0.0124(7) 0.0030(6) 0.0038(6) 0.0007(6) O2 0.0201(7) 0.0112(6) 0.0122(6) 0.0007(5) 0.0028(5) -0.0006(5) O1 0.0188(7) 0.0129(6) 0.0147(6) 0.0008(5) 0.0027(5) -0.0012(5) O3 0.0290(9) 0.0429(11) 0.0286(8) -0.0133(7) 0.0057(7) 0.0042(8) O4 0.0144(7) 0.0487(12) 0.0325(9) -0.0087(8) 0.0041(6) 0.0037(7) O5 0.0347(10) 0.0276(10) 0.0604(13) 0.0000(9) 0.0062(9) -0.0104(8) O6 0.0396(11) 0.0625(14) 0.0233(9) 0.0136(9) -0.0040(7) 0.0112(9) O7 0.0335(9) 0.0194(8) 0.0209(7) 0.0079(6) 0.0014(6) 0.0002(6) O8 0.129(3) 0.0794(18) 0.0182(10) -0.0011(11) 0.0069(12) 0.0206(18) O9 0.0276(10) 0.0581(14) 0.0789(16) 0.0309(12) 0.0083(10) 0.0214(10) O10 0.0326(10) 0.0586(14) 0.0676(14) 0.0393(12) -0.0062(9) -0.0196(9) Cl1 0.0141(2) 0.0240(3) 0.0166(2) -0.00056(17) 0.00045(16) 0.00032(17) Cl2 0.0175(2) 0.0277(3) 0.0180(2) 0.00992(18) 0.00169(17) 0.00421(19) Co1 0.01088(13) 0.00997(14) 0.01130(13) 0.00003(8) 0.00106(9) -0.00033(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 N1 1.503(2) . ? C1 C2 1.523(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N4 1.500(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N1 1.501(2) . ? C3 C4 1.522(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N3 1.503(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 N1 1.513(2) . ? C5 C6 1.529(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N2 1.490(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O1 1.290(2) . ? C7 N5 1.306(3) . ? C7 C8 1.503(3) . ? C8 C9 1.522(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C18 1.376(3) . ? C9 C10 1.437(3) . ? C10 C11 1.424(3) . ? C10 C15 1.432(3) . ? C11 C12 1.376(3) . ? C11 H11 0.9500 . ? C12 C13 1.411(3) . ? C12 H12 0.9500 . ? C13 C14 1.360(4) . ? C13 H13 0.9500 . ? C14 C15 1.422(3) . ? C14 H14 0.9500 . ? C15 C16 1.423(3) . ? C16 C17 1.362(3) . ? C16 H16 0.9500 . ? C17 C18 1.420(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? N1 Co1 1.9389(16) . ? N4 Co1 1.9669(16) . ? N4 H4C 0.9200 . ? N4 H4D 0.9200 . ? N3 Co1 1.9668(16) . ? N3 H3C 0.9200 . ? N3 H3D 0.9200 . ? N2 Co1 1.9521(16) . ? N2 H2C 0.9200 . ? N2 H2D 0.9200 . ? N5 O2 1.391(2) . ? N5 H5 0.8800 . ? O2 Co1 1.9029(13) . ? O1 Co1 1.9006(14) . ? O3 Cl1 1.4448(17) . ? O4 Cl1 1.4463(16) . ? O5 Cl1 1.4451(18) . ? O6 Cl1 1.4336(17) . ? O7 Cl2 1.4398(15) . ? O8 Cl2 1.420(2) . ? O9 Cl2 1.4258(19) . ? O10 Cl2 1.432(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 108.25(15) . . ? N1 C1 H1A 110.0 . . ? C2 C1 H1A 110.0 . . ? N1 C1 H1B 110.0 . . ? C2 C1 H1B 110.0 . . ? H1A C1 H1B 108.4 . . ? N4 C2 C1 108.63(15) . . ? N4 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? N4 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? H2A C2 H2B 108.3 . . ? N1 C3 C4 109.13(15) . . ? N1 C3 H3A 109.9 . . ? C4 C3 H3A 109.9 . . ? N1 C3 H3B 109.9 . . ? C4 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? N3 C4 C3 107.90(15) . . ? N3 C4 H4A 110.1 . . ? C3 C4 H4A 110.1 . . ? N3 C4 H4B 110.1 . . ? C3 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? N1 C5 C6 111.10(15) . . ? N1 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? N1 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? N2 C6 C5 106.96(15) . . ? N2 C6 H6A 110.3 . . ? C5 C6 H6A 110.3 . . ? N2 C6 H6B 110.3 . . ? C5 C6 H6B 110.3 . . ? H6A C6 H6B 108.6 . . ? O1 C7 N5 118.98(17) . . ? O1 C7 C8 120.55(17) . . ? N5 C7 C8 120.47(17) . . ? C7 C8 C9 113.78(17) . . ? C7 C8 H8A 108.8 . . ? C9 C8 H8A 108.8 . . ? C7 C8 H8B 108.8 . . ? C9 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C18 C9 C10 119.06(18) . . ? C18 C9 C8 122.48(18) . . ? C10 C9 C8 118.46(17) . . ? C11 C10 C15 118.15(18) . . ? C11 C10 C9 122.57(18) . . ? C15 C10 C9 119.28(18) . . ? C12 C11 C10 120.9(2) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C11 C12 C13 120.4(2) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C14 C13 C12 120.2(2) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 121.2(2) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C14 C15 C16 121.81(19) . . ? C14 C15 C10 119.0(2) . . ? C16 C15 C10 119.20(19) . . ? C17 C16 C15 120.51(19) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 120.5(2) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C9 C18 C17 121.4(2) . . ? C9 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C3 N1 C1 111.43(14) . . ? C3 N1 C5 112.35(14) . . ? C1 N1 C5 110.48(14) . . ? C3 N1 Co1 106.47(11) . . ? C1 N1 Co1 106.36(11) . . ? C5 N1 Co1 109.49(11) . . ? C2 N4 Co1 110.23(12) . . ? C2 N4 H4C 109.6 . . ? Co1 N4 H4C 109.6 . . ? C2 N4 H4D 109.6 . . ? Co1 N4 H4D 109.6 . . ? H4C N4 H4D 108.1 . . ? C4 N3 Co1 110.78(12) . . ? C4 N3 H3C 109.5 . . ? Co1 N3 H3C 109.5 . . ? C4 N3 H3D 109.5 . . ? Co1 N3 H3D 109.5 . . ? H3C N3 H3D 108.1 . . ? C6 N2 Co1 109.56(12) . . ? C6 N2 H2C 109.8 . . ? Co1 N2 H2C 109.8 . . ? C6 N2 H2D 109.8 . . ? Co1 N2 H2D 109.8 . . ? H2C N2 H2D 108.2 . . ? C7 N5 O2 119.25(15) . . ? C7 N5 H5 120.4 . . ? O2 N5 H5 120.4 . . ? N5 O2 Co1 105.41(10) . . ? C7 O1 Co1 109.53(12) . . ? O6 Cl1 O3 110.15(12) . . ? O6 Cl1 O5 109.70(12) . . ? O3 Cl1 O5 107.96(12) . . ? O6 Cl1 O4 110.19(11) . . ? O3 Cl1 O4 109.50(10) . . ? O5 Cl1 O4 109.30(11) . . ? O8 Cl2 O9 109.40(17) . . ? O8 Cl2 O10 110.14(17) . . ? O9 Cl2 O10 108.52(15) . . ? O8 Cl2 O7 110.07(14) . . ? O9 Cl2 O7 108.92(12) . . ? O10 Cl2 O7 109.76(11) . . ? O1 Co1 O2 86.76(6) . . ? O1 Co1 N1 178.86(6) . . ? O2 Co1 N1 94.31(6) . . ? O1 Co1 N2 91.14(6) . . ? O2 Co1 N2 177.89(6) . . ? N1 Co1 N2 87.78(7) . . ? O1 Co1 N3 92.55(6) . . ? O2 Co1 N3 86.32(6) . . ? N1 Co1 N3 87.15(6) . . ? N2 Co1 N3 93.50(7) . . ? O1 Co1 N4 93.19(6) . . ? O2 Co1 N4 85.88(6) . . ? N1 Co1 N4 87.26(6) . . ? N2 Co1 N4 94.52(7) . . ? N3 Co1 N4 170.04(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 N1 C1 C2 N4 -44.18(19) . . . . ? N1 C3 C4 N3 43.6(2) . . . . ? N1 C5 C6 N2 -41.0(2) . . . . ? O1 C7 C8 C9 71.7(2) . . . . ? N5 C7 C8 C9 -107.7(2) . . . . ? C7 C8 C9 C18 -3.1(3) . . . . ? C7 C8 C9 C10 176.32(17) . . . . ? C18 C9 C10 C11 -179.42(19) . . . . ? C8 C9 C10 C11 1.1(3) . . . . ? C18 C9 C10 C15 0.5(3) . . . . ? C8 C9 C10 C15 -179.02(17) . . . . ? C15 C10 C11 C12 1.7(3) . . . . ? C9 C10 C11 C12 -178.38(19) . . . . ? C10 C11 C12 C13 0.4(3) . . . . ? C11 C12 C13 C14 -2.1(3) . . . . ? C12 C13 C14 C15 1.7(3) . . . . ? C13 C14 C15 C16 179.1(2) . . . . ? C13 C14 C15 C10 0.5(3) . . . . ? C11 C10 C15 C14 -2.1(3) . . . . ? C9 C10 C15 C14 177.97(18) . . . . ? C11 C10 C15 C16 179.16(18) . . . . ? C9 C10 C15 C16 -0.7(3) . . . . ? C14 C15 C16 C17 -178.3(2) . . . . ? C10 C15 C16 C17 0.4(3) . . . . ? C15 C16 C17 C18 0.2(3) . . . . ? C10 C9 C18 C17 0.2(3) . . . . ? C8 C9 C18 C17 179.6(2) . . . . ? C16 C17 C18 C9 -0.5(3) . . . . ? C4 C3 N1 C1 -160.33(15) . . . . ? C4 C3 N1 C5 75.08(19) . . . . ? C4 C3 N1 Co1 -44.77(16) . . . . ? C2 C1 N1 C3 161.12(15) . . . . ? C2 C1 N1 C5 -73.25(18) . . . . ? C2 C1 N1 Co1 45.49(16) . . . . ? C6 C5 N1 C3 -93.49(19) . . . . ? C6 C5 N1 C1 141.40(16) . . . . ? C6 C5 N1 Co1 24.59(18) . . . . ? C1 C2 N4 Co1 21.93(18) . . . . ? C3 C4 N3 Co1 -21.95(18) . . . . ? C5 C6 N2 Co1 38.28(18) . . . . ? O1 C7 N5 O2 0.4(3) . . . . ? C8 C7 N5 O2 179.91(15) . . . . ? C7 N5 O2 Co1 -2.07(19) . . . . ? N5 C7 O1 Co1 1.5(2) . . . . ? C8 C7 O1 Co1 -177.98(14) . . . . ? C7 O1 Co1 O2 -2.10(12) . . . . ? C7 O1 Co1 N1 -163(3) . . . . ? C7 O1 Co1 N2 178.18(13) . . . . ? C7 O1 Co1 N3 -88.27(13) . . . . ? C7 O1 Co1 N4 83.58(13) . . . . ? N5 O2 Co1 O1 2.17(10) . . . . ? N5 O2 Co1 N1 -178.20(10) . . . . ? N5 O2 Co1 N2 9.8(18) . . . . ? N5 O2 Co1 N3 94.94(11) . . . . ? N5 O2 Co1 N4 -91.27(11) . . . . ? C3 N1 Co1 O1 101(3) . . . . ? C1 N1 Co1 O1 -140(3) . . . . ? C5 N1 Co1 O1 -21(3) . . . . ? C3 N1 Co1 O2 -60.19(11) . . . . ? C1 N1 Co1 O2 58.75(12) . . . . ? C5 N1 Co1 O2 178.13(12) . . . . ? C3 N1 Co1 N2 119.52(12) . . . . ? C1 N1 Co1 N2 -121.54(12) . . . . ? C5 N1 Co1 N2 -2.16(12) . . . . ? C3 N1 Co1 N3 25.91(11) . . . . ? C1 N1 Co1 N3 144.84(12) . . . . ? C5 N1 Co1 N3 -95.78(12) . . . . ? C3 N1 Co1 N4 -145.84(12) . . . . ? C1 N1 Co1 N4 -26.91(12) . . . . ? C5 N1 Co1 N4 92.47(12) . . . . ? C6 N2 Co1 O1 158.62(13) . . . . ? C6 N2 Co1 O2 151.0(17) . . . . ? C6 N2 Co1 N1 -21.01(13) . . . . ? C6 N2 Co1 N3 66.00(13) . . . . ? C6 N2 Co1 N4 -108.08(13) . . . . ? C4 N3 Co1 O1 178.93(12) . . . . ? C4 N3 Co1 O2 92.34(13) . . . . ? C4 N3 Co1 N1 -2.17(12) . . . . ? C4 N3 Co1 N2 -89.77(13) . . . . ? C4 N3 Co1 N4 53.8(4) . . . . ? C2 N4 Co1 O1 -178.23(12) . . . . ? C2 N4 Co1 O2 -91.71(12) . . . . ? C2 N4 Co1 N1 2.81(12) . . . . ? C2 N4 Co1 N2 90.37(13) . . . . ? C2 N4 Co1 N3 -53.1(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4C O4 0.92 2.16 3.037(2) 160.1 . N4 H4C Cl1 0.92 2.87 3.6193(16) 139.2 . N4 H4D O10 0.92 2.31 3.057(3) 137.8 4_665 N3 H3C O9 0.92 2.09 2.990(3) 164.7 4_565 N3 H3D O5 0.92 2.42 3.307(3) 163.3 1_455 N3 H3D O3 0.92 2.44 3.181(3) 137.8 1_455 N3 H3D Cl1 0.92 2.98 3.8757(17) 166.0 1_455 N2 H2C O10 0.92 2.26 3.141(3) 159.4 4_665 N2 H2C O6 0.92 2.64 3.158(2) 116.4 4_565 N2 H2D O9 0.92 2.22 2.989(2) 140.0 4_565 N5 H5 O7 0.88 2.09 2.969(2) 172.4 . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.648 _refine_diff_density_min -0.619 _refine_diff_density_rms 0.172 data_7 _database_code_depnum_ccdc_archive 'CCDC 866271' #TrackingRef '- combined revised cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C23 H24 Cl Co N4 O2), 4(Cl O4), (H2 O) ' _chemical_formula_sum 'C46 H50 Cl6 Co2 N8 O21' _chemical_formula_weight 1381.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M CC _symmetry_space_group_name_Hall 'C -2yc' _symmetry_Intl_tables_number 9 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 17.281(6) _cell_length_b 17.298(6) _cell_length_c 18.867(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.172(7) _cell_angle_gamma 90.00 _cell_volume 5640(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15269 _cell_measurement_theta_min 2.357 _cell_measurement_theta_max 27.820 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.460 _exptl_crystal_size_mid 0.310 _exptl_crystal_size_min 0.250 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.627 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2824 _exptl_absorpt_coefficient_mu 0.957 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.670 _exptl_absorpt_correction_T_max 0.787 _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 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 331 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0.01 _diffrn_reflns_number 27035 _diffrn_reflns_av_R_equivalents 0.0736 _diffrn_reflns_av_sigmaI/netI 0.0632 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 28.35 _reflns_number_total 13195 _reflns_number_gt 12072 _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 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 (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^)+(0.1428P)^2^+28.7493P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(1) _refine_ls_number_reflns 13195 _refine_ls_number_parameters 835 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.0887 _refine_ls_R_factor_gt 0.0836 _refine_ls_wR_factor_ref 0.2292 _refine_ls_wR_factor_gt 0.2239 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 0.0277(7) 0.7124(8) 0.1679(11) 0.057(4) Uani 0.75 1 d P A 3 H1A H -0.0288 0.7084 0.1672 0.086 Uiso 0.75 1 calc PR A 3 H1B H 0.0433 0.7631 0.1498 0.086 Uiso 0.75 1 calc PR A 3 H1C H 0.0465 0.7064 0.2167 0.086 Uiso 0.75 1 calc PR A 3 C2 C 0.0629(7) 0.6480(7) 0.1208(7) 0.031(3) Uani 0.75 1 d P A 3 C3 C 0.0661(7) 0.6564(7) 0.0482(7) 0.035(2) Uani 0.75 1 d P A 3 C4 C 0.0922(7) 0.6035(8) 0.0013(7) 0.028(3) Uani 0.75 1 d P A 3 C5 C 0.0901(9) 0.6153(9) -0.0788(7) 0.049(3) Uani 0.75 1 d P A 3 H5A H 0.0405 0.5971 -0.0976 0.074 Uiso 0.75 1 calc PR A 3 H5B H 0.1323 0.5859 -0.1007 0.074 Uiso 0.75 1 calc PR A 3 H5C H 0.0964 0.6703 -0.0896 0.074 Uiso 0.75 1 calc PR A 3 C7 C 0.2083(7) 0.3158(7) -0.0122(7) 0.040(3) Uani 0.75 1 d P B 1 H7 H 0.2152 0.3033 -0.0608 0.048 Uiso 0.75 1 calc PR B 1 C8 C 0.2273(9) 0.2615(8) 0.0399(11) 0.045(3) Uani 0.75 1 d P B 1 H8 H 0.2460 0.2120 0.0265 0.054 Uiso 0.75 1 calc PR B 1 C9 C 0.2187(7) 0.2803(6) 0.1129(7) 0.034(2) Uani 0.75 1 d P B 1 H9 H 0.2299 0.2445 0.1496 0.041 Uiso 0.75 1 calc PR B 1 C10 C 0.1931(7) 0.3536(8) 0.1262(8) 0.033(3) Uani 0.75 1 d P B 1 C6 C 0.1789(9) 0.3896(10) 0.0069(7) 0.027(3) Uani 0.75 1 d P B 1 H6 H 0.1640 0.4263 -0.0281 0.032 Uiso 0.75 1 calc PR B 1 N2 N 0.1728(5) 0.4055(5) 0.0769(5) 0.0294(18) Uani 0.75 1 d P B 1 C11 C 0.1833(10) 0.3805(8) 0.2024(8) 0.049(3) Uani 0.75 1 d P B 1 H11A H 0.1535 0.3412 0.2291 0.059 Uiso 0.75 1 calc PR B 1 H11B H 0.2348 0.3854 0.2250 0.059 Uiso 0.75 1 calc PR B 1 N1 N 0.1416(7) 0.4575(6) 0.2065(5) 0.039(2) Uani 0.75 1 d P B 1 C17 C 0.1920(8) 0.5192(7) 0.2453(6) 0.052(3) Uani 0.75 1 d P B 1 H17A H 0.1594 0.5631 0.2605 0.063 Uiso 0.75 1 calc PR B 1 H17B H 0.2166 0.4962 0.2878 0.063 Uiso 0.75 1 calc PR B 1 C23 C 0.0678(7) 0.4550(9) 0.2389(5) 0.057(3) Uani 0.75 1 d P B 1 H23A H 0.0542 0.5064 0.2582 0.068 Uiso 0.75 1 calc PR B 1 H23B H 0.0679 0.4172 0.2784 0.068 Uiso 0.75 1 calc PR B 1 C12 C 0.2804(5) 0.5641(5) 0.0743(6) 0.042(2) Uani 1 1 d . . . H12 H 0.2647 0.5584 0.0263 0.050 Uiso 1 1 calc R . . C13 C 0.3540(6) 0.5972(6) 0.0911(9) 0.063(4) Uani 1 1 d . . . H13 H 0.3887 0.6123 0.0547 0.076 Uiso 1 1 calc R . . C14 C 0.3745(8) 0.6071(8) 0.1653(10) 0.075(5) Uani 1 1 d . . . H14 H 0.4213 0.6316 0.1791 0.090 Uiso 1 1 calc R . . C15 C 0.3235(9) 0.5799(9) 0.2139(8) 0.069(4) Uani 1 1 d . B . H15 H 0.3360 0.5835 0.2629 0.083 Uiso 1 1 calc R . . C16 C 0.2538(6) 0.5470(6) 0.1939(6) 0.046(2) Uani 1 1 d . . . C18 C -0.0148(5) 0.4306(6) 0.0605(5) 0.039(2) Uani 1 1 d . . . H18 H 0.0018 0.4414 0.0136 0.047 Uiso 1 1 calc R . . C19 C -0.0878(6) 0.3952(7) 0.0706(8) 0.055(3) Uani 1 1 d . . . H19 H -0.1204 0.3834 0.0315 0.066 Uiso 1 1 calc R . . C20 C -0.1096(7) 0.3788(8) 0.1377(10) 0.071(4) Uani 1 1 d . . . H20 H -0.1580 0.3547 0.1464 0.085 Uiso 1 1 calc R . . C21 C -0.0608(7) 0.3974(9) 0.1936(9) 0.074(5) Uani 1 1 d . B . H21 H -0.0764 0.3866 0.2408 0.089 Uiso 1 1 calc R . . C22 C 0.0086(7) 0.4306(7) 0.1818(6) 0.052(3) Uani 1 1 d . . . C24 C 0.4142(6) 0.3933(7) -0.0437(6) 0.051(3) Uani 1 1 d . . . H24A H 0.3704 0.4293 -0.0431 0.076 Uiso 1 1 calc R . . H24B H 0.3974 0.3429 -0.0258 0.076 Uiso 1 1 calc R . . H24C H 0.4332 0.3877 -0.0923 0.076 Uiso 1 1 calc R . . C25 C 0.4783(5) 0.4244(5) 0.0030(5) 0.0316(16) Uani 1 1 d . . . C26 C 0.4691(5) 0.4238(5) 0.0772(5) 0.0353(18) Uani 1 1 d . . . C27 C 0.5251(5) 0.4521(5) 0.1232(4) 0.0309(16) Uani 1 1 d . . . C28 C 0.5137(7) 0.4476(8) 0.2017(6) 0.056(3) Uani 1 1 d . . . H28A H 0.5565 0.4740 0.2258 0.084 Uiso 1 1 calc R . . H28B H 0.5124 0.3933 0.2164 0.084 Uiso 1 1 calc R . . H28C H 0.4647 0.4726 0.2143 0.084 Uiso 1 1 calc R . . C29 C 0.5601(5) 0.6415(5) 0.0489(5) 0.0381(19) Uani 1 1 d . . . H29 H 0.5655 0.6276 0.0974 0.046 Uiso 1 1 calc R . . C30 C 0.5269(6) 0.7141(7) 0.0289(7) 0.050(3) Uani 1 1 d . . . H30 H 0.5084 0.7484 0.0643 0.060 Uiso 1 1 calc R . . C31 C 0.5221(6) 0.7333(6) -0.0373(8) 0.058(3) Uani 1 1 d . . . H31 H 0.4986 0.7810 -0.0498 0.070 Uiso 1 1 calc R . . C32 C 0.5509(7) 0.6851(6) -0.0907(6) 0.053(3) Uani 1 1 d . . . H32 H 0.5499 0.7006 -0.1390 0.063 Uiso 1 1 calc R . . C33 C 0.5804(6) 0.6149(6) -0.0710(5) 0.045(2) Uani 1 1 d . . . C34 C 0.6107(7) 0.5539(6) -0.1223(5) 0.045(2) Uani 1 1 d . . . H34A H 0.5672 0.5227 -0.1412 0.054 Uiso 1 1 calc R . . H34B H 0.6371 0.5792 -0.1627 0.054 Uiso 1 1 calc R . . C35 C 0.7395(6) 0.5466(6) 0.1159(6) 0.045(2) Uani 1 1 d . . . H35 H 0.7044 0.5334 0.1527 0.054 Uiso 1 1 calc R . . C36 C 0.8121(7) 0.5789(8) 0.1299(7) 0.062(3) Uani 1 1 d . . . H36 H 0.8226 0.5897 0.1784 0.075 Uiso 1 1 calc R . . C37 C 0.8663(8) 0.5960(8) 0.0867(13) 0.089(6) Uani 1 1 d . . . H37 H 0.9159 0.6139 0.1011 0.107 Uiso 1 1 calc R . . C38 C 0.8432(7) 0.5847(6) 0.0107(10) 0.068(4) Uani 1 1 d . . . H38 H 0.8776 0.5986 -0.0264 0.081 Uiso 1 1 calc R . . C39 C 0.7720(5) 0.5541(5) -0.0046(5) 0.0362(19) Uani 1 1 d . . . C40 C 0.7455(7) 0.5404(7) -0.0788(6) 0.050(2) Uani 1 1 d . . . H40A H 0.7835 0.5067 -0.1029 0.060 Uiso 1 1 calc R . . H40B H 0.7444 0.5904 -0.1043 0.060 Uiso 1 1 calc R . . C41 C 0.6935(5) 0.3453(5) 0.0623(6) 0.038(2) Uani 1 1 d . . . H41 H 0.6812 0.3623 0.1088 0.045 Uiso 1 1 calc R . . C42 C 0.7299(6) 0.2751(6) 0.0562(7) 0.048(2) Uani 1 1 d . . . H42 H 0.7413 0.2436 0.0961 0.058 Uiso 1 1 calc R . . C43 C 0.7491(7) 0.2529(6) -0.0133(8) 0.056(3) Uani 1 1 d . . . H43 H 0.7748 0.2052 -0.0214 0.068 Uiso 1 1 calc R . . C44 C 0.7314(6) 0.2986(6) -0.0673(7) 0.052(3) Uani 1 1 d . . . H44 H 0.7453 0.2835 -0.1139 0.062 Uiso 1 1 calc R . . C45 C 0.6923(6) 0.3692(6) -0.0566(5) 0.042(2) Uani 1 1 d . . . C46 C 0.6662(7) 0.4242(6) -0.1133(5) 0.042(2) Uani 1 1 d . . . H46A H 0.7017 0.4215 -0.1544 0.050 Uiso 1 1 calc R . . H46B H 0.6135 0.4102 -0.1298 0.050 Uiso 1 1 calc R . . Cl1A Cl 0.2424(7) 0.2463(6) 0.0074(7) 0.043(2) Uani 0.25 1 d P B 4 O1A O 0.1479(19) 0.4545(19) 0.0190(17) 0.0488(17) Uiso 0.25 1 d P B 4 O2A O 0.1841(19) 0.397(2) 0.1510(18) 0.0488(17) Uiso 0.25 1 d P B 4 C3A C 0.209(3) 0.328(3) 0.048(2) 0.0488(17) Uiso 0.25 1 d PD B 4 C1A C 0.184(3) 0.379(3) -0.078(2) 0.0488(17) Uiso 0.25 1 d PD B 4 H1A1 H 0.1702 0.4303 -0.0965 0.073 Uiso 0.25 1 calc PR B 4 H1A2 H 0.1432 0.3420 -0.0912 0.073 Uiso 0.25 1 calc PR B 4 H1A3 H 0.2332 0.3625 -0.0979 0.073 Uiso 0.25 1 calc PR B 4 C5A C 0.236(3) 0.264(3) 0.164(2) 0.0488(17) Uiso 0.25 1 d P B 4 H5A1 H 0.2299 0.2774 0.2146 0.073 Uiso 0.25 1 calc PR B 4 H5A2 H 0.2905 0.2544 0.1541 0.073 Uiso 0.25 1 calc PR B 4 H5A3 H 0.2054 0.2179 0.1536 0.073 Uiso 0.25 1 calc PR B 4 C2A C 0.190(6) 0.383(5) 0.004(2) 0.0488(17) Uiso 0.25 1 d PD B 4 C4A C 0.206(4) 0.334(5) 0.118(3) 0.0488(17) Uiso 0.25 1 d PD B 4 N1A N 0.131(2) 0.528(2) 0.206(2) 0.0488(17) Uiso 0.25 1 d P B 2 C17A C 0.1920(8) 0.5192(7) 0.2453(6) 0.052(3) Uani 0.25 1 d P B 2 H17C H 0.2001 0.4645 0.2590 0.063 Uiso 0.25 1 calc PR B 2 H17D H 0.1899 0.5518 0.2884 0.063 Uiso 0.25 1 calc PR B 2 C23A C 0.0678(7) 0.4550(9) 0.2389(5) 0.057(3) Uani 0.25 1 d P B 2 H23C H 0.0984 0.4094 0.2538 0.068 Uiso 0.25 1 calc PR B 2 H23D H 0.0400 0.4748 0.2810 0.068 Uiso 0.25 1 calc PR B 2 C11A C 0.093(3) 0.605(3) 0.207(2) 0.0488(17) Uiso 0.25 1 d P B 2 H11C H 0.0442 0.6029 0.2339 0.059 Uiso 0.25 1 calc PR B 2 H11D H 0.1275 0.6435 0.2294 0.059 Uiso 0.25 1 calc PR B 2 N2A N 0.094(2) 0.582(2) 0.0780(17) 0.0488(17) Uiso 0.25 1 d PD B 2 C6A C 0.077(2) 0.628(3) 0.134(2) 0.0488(17) Uiso 0.25 1 d PD B 2 C10A C 0.080(3) 0.602(3) 0.010(2) 0.0488(17) Uiso 0.25 1 d PD B 2 H4A H 0.0944 0.5670 -0.0265 0.059 Uiso 0.25 1 calc PR B 2 C7A C 0.045(2) 0.672(2) -0.008(2) 0.0488(17) Uiso 0.25 1 d PD B 2 H7A H 0.0354 0.6856 -0.0564 0.059 Uiso 0.25 1 calc PR B 2 C9A C 0.042(2) 0.699(3) 0.118(2) 0.0488(17) Uiso 0.25 1 d PD B 2 H9A H 0.0300 0.7337 0.1554 0.059 Uiso 0.25 1 calc PR B 2 C8A C 0.025(2) 0.721(3) 0.0479(17) 0.0488(17) Uiso 0.25 1 d PD B 2 H8A H 0.0002 0.7686 0.0387 0.059 Uiso 0.25 1 calc PR B 2 N4 N 0.2346(5) 0.5415(4) 0.1263(4) 0.0355(16) Uani 1 1 d . B . N3 N 0.0323(5) 0.4498(5) 0.1154(4) 0.0367(16) Uani 1 1 d . B . N8 N 0.5833(4) 0.5939(4) -0.0026(4) 0.0297(14) Uani 1 1 d . . . N6 N 0.7220(5) 0.5350(4) 0.0447(5) 0.0407(18) Uani 1 1 d . . . N7 N 0.6737(4) 0.3920(4) 0.0084(4) 0.0310(14) Uani 1 1 d . . . N5 N 0.6660(6) 0.5033(5) -0.0837(5) 0.044(2) Uani 1 1 d . . . O2 O 0.0867(5) 0.5875(5) 0.1537(4) 0.0331(16) Uani 0.75 1 d P A 3 O1 O 0.1198(5) 0.5372(4) 0.0190(4) 0.0281(15) Uani 0.75 1 d P A 3 O4 O 0.5356(4) 0.4481(4) -0.0298(4) 0.0415(15) Uani 1 1 d . . . O3 O 0.5908(4) 0.4789(4) 0.1040(3) 0.0371(13) Uani 1 1 d . . . O5 O 0.6838(15) 0.3432(11) 0.2415(7) 0.187(12) Uani 1 1 d D . . O6 O 0.7845(11) 0.2606(9) 0.2284(10) 0.159(10) Uani 1 1 d D . . O7 O 0.6836(11) 0.2067(8) 0.2774(16) 0.211(14) Uani 1 1 d D . . O8 O 0.7377(10) 0.2943(7) 0.3420(5) 0.101(5) Uani 1 1 d D . . O9 O 0.5177(8) 0.9124(11) 0.8701(10) 0.082(5) Uani 0.65 1 d P C 1 O10 O 0.4272(13) 1.0088(10) 0.8692(15) 0.118(10) Uani 0.65 1 d P C 1 O11 O 0.4251(8) 0.9157(14) 0.7804(7) 0.093(6) Uani 0.65 1 d P C 1 O12 O 0.3833(11) 0.8809(15) 0.8898(10) 0.105(8) Uani 0.65 1 d P C 1 O9A O 0.4009(13) 0.9785(14) 0.8186(12) 0.0488(17) Uiso 0.35 1 d P C 2 O10A O 0.4783(13) 0.8709(13) 0.8378(12) 0.0488(17) Uiso 0.35 1 d P C 2 O11A O 0.4991(10) 0.9630(13) 0.8980(10) 0.0488(17) Uiso 0.35 1 d PD C 2 O12A O 0.3941(15) 0.9041(14) 0.9202(14) 0.0488(17) Uiso 0.35 1 d P C 2 O13 O 0.3814(11) 0.4042(18) 0.4387(7) 0.126(9) Uani 0.70 1 d PD D 1 O14 O 0.4105(11) 0.4612(10) 0.3424(11) 0.168(15) Uani 0.70 1 d PD D 1 O15 O 0.3124(13) 0.3535(10) 0.3304(15) 0.133(9) Uani 0.70 1 d PD D 1 O16 O 0.2888(8) 0.4756(9) 0.3916(9) 0.105(8) Uani 0.70 1 d PD D 1 O13A O 0.3400(14) 0.3924(18) 0.2950(7) 0.063(4) Uiso 0.30 1 d PD D 2 O14A O 0.4206(8) 0.4503(17) 0.3908(14) 0.063(4) Uiso 0.30 1 d PD D 2 O15A O 0.2760(10) 0.4546(15) 0.3991(14) 0.063(4) Uiso 0.30 1 d PD D 2 O16A O 0.3660(17) 0.3408(9) 0.3967(16) 0.063(4) Uiso 0.30 1 d PD D 2 O17 O 0.6142(12) 0.2638(9) 0.8025(8) 0.128(6) Uani 1 1 d . . . O18 O 0.6068(15) 0.3678(8) 0.7288(7) 0.145(8) Uani 1 1 d . . . O19 O 0.5380(7) 0.2587(6) 0.6992(5) 0.076(3) Uani 1 1 d . . . O20 O 0.5112(14) 0.3442(16) 0.7947(10) 0.178(11) Uani 1 1 d . . . O1W O 0.9160(10) 0.3023(9) 0.3623(9) 0.054(4) Uiso 0.50 1 d P . . O2W O 0.3378(11) 0.2298(10) 0.2488(9) 0.058(4) Uiso 0.50 1 d P . . Cl1 Cl 0.0279(3) 0.7427(2) 0.0111(3) 0.0597(10) Uani 0.75 1 d P A 3 Cl2 Cl 0.38479(17) 0.38481(19) 0.11277(19) 0.0589(7) Uani 1 1 d . . . Cl3 Cl 0.7204(2) 0.2788(2) 0.27029(19) 0.0729(10) Uani 1 1 d D . . Cl4 Cl 0.43682(17) 0.92902(19) 0.85547(16) 0.0559(6) Uani 1 1 d D . . Cl5 Cl 0.3453(2) 0.4176(2) 0.36999(18) 0.0727(10) Uani 1 1 d D . . Cl6 Cl 0.56647(19) 0.30637(17) 0.75621(15) 0.0558(7) Uani 1 1 d . . . Co1 Co 0.13219(7) 0.49663(6) 0.11163(6) 0.0290(3) Uani 1 1 d . . . Co2 Co 0.62698(6) 0.49164(6) 0.01197(5) 0.0260(2) 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 0.023(6) 0.041(7) 0.107(13) -0.036(8) -0.018(7) 0.002(5) C2 0.020(5) 0.029(6) 0.043(6) -0.004(4) 0.001(4) -0.004(4) C3 0.031(6) 0.035(6) 0.039(6) -0.002(5) 0.002(5) -0.003(4) C4 0.019(5) 0.020(4) 0.045(7) 0.002(4) -0.005(4) -0.003(4) C5 0.055(8) 0.060(8) 0.032(6) -0.001(6) -0.020(6) 0.001(6) C7 0.031(6) 0.041(6) 0.048(7) -0.013(5) 0.009(5) 0.005(5) C8 0.044(8) 0.022(6) 0.069(11) 0.002(7) 0.000(7) 0.008(5) C9 0.030(5) 0.012(4) 0.060(7) -0.006(4) 0.002(5) 0.002(4) C10 0.017(6) 0.038(9) 0.044(7) 0.014(6) -0.004(5) -0.005(5) C6 0.018(6) 0.019(5) 0.043(6) -0.002(4) 0.002(4) 0.010(4) N2 0.018(4) 0.030(4) 0.040(5) -0.004(4) -0.006(3) -0.001(3) C11 0.060(9) 0.034(6) 0.053(8) 0.007(5) -0.012(6) -0.007(6) N1 0.054(6) 0.040(5) 0.023(4) 0.007(4) -0.014(4) 0.009(5) C17 0.064(7) 0.058(6) 0.034(5) -0.020(5) -0.018(5) 0.016(5) C23 0.052(6) 0.092(9) 0.027(4) 0.019(5) 0.011(4) 0.020(6) C12 0.026(4) 0.033(4) 0.066(6) 0.005(4) -0.011(4) -0.008(3) C13 0.023(4) 0.029(4) 0.137(12) 0.000(6) -0.029(6) -0.009(3) C14 0.036(6) 0.055(7) 0.133(14) -0.024(8) -0.031(8) 0.007(5) C15 0.057(8) 0.075(8) 0.075(8) -0.027(7) -0.032(7) 0.020(7) C16 0.046(5) 0.039(5) 0.052(5) -0.018(4) -0.033(5) 0.015(4) C18 0.028(4) 0.046(5) 0.044(5) -0.008(4) 0.004(4) -0.011(4) C19 0.022(4) 0.061(6) 0.082(8) 0.007(6) -0.004(5) -0.009(4) C20 0.034(6) 0.054(7) 0.124(13) 0.007(7) 0.008(7) -0.014(5) C21 0.037(6) 0.091(10) 0.093(10) 0.035(8) 0.032(7) 0.017(6) C22 0.045(6) 0.054(6) 0.056(6) 0.019(5) 0.015(5) 0.013(5) C24 0.039(5) 0.058(6) 0.056(6) 0.010(5) -0.028(5) -0.015(4) C25 0.027(4) 0.031(4) 0.037(4) 0.000(3) 0.001(3) 0.007(3) C26 0.016(3) 0.038(4) 0.051(5) 0.005(4) 0.007(3) 0.001(3) C27 0.029(4) 0.033(4) 0.031(4) 0.005(3) 0.012(3) 0.011(3) C28 0.054(6) 0.067(7) 0.048(6) 0.012(5) 0.027(5) 0.017(5) C29 0.031(4) 0.038(4) 0.045(5) 0.004(4) -0.005(4) 0.004(3) C30 0.030(5) 0.051(6) 0.069(7) -0.002(5) 0.010(5) -0.003(4) C31 0.033(5) 0.038(5) 0.105(10) 0.026(6) -0.031(6) 0.004(4) C32 0.061(7) 0.040(5) 0.058(6) 0.006(4) -0.042(5) 0.001(4) C33 0.045(5) 0.055(6) 0.035(5) 0.012(4) -0.012(4) -0.014(4) C34 0.059(6) 0.045(5) 0.031(4) 0.017(4) -0.015(4) -0.005(4) C35 0.043(5) 0.044(5) 0.048(5) -0.013(4) -0.023(4) 0.002(4) C36 0.049(7) 0.074(8) 0.064(7) -0.022(6) -0.019(6) 0.009(6) C37 0.038(7) 0.049(7) 0.18(2) -0.022(9) 0.032(9) -0.003(5) C38 0.034(5) 0.037(5) 0.131(13) -0.028(7) 0.009(6) -0.005(4) C39 0.028(4) 0.031(4) 0.049(5) 0.002(4) 0.005(4) 0.010(3) C40 0.048(6) 0.051(6) 0.050(6) 0.008(4) 0.012(5) -0.010(5) C41 0.024(4) 0.030(4) 0.060(6) 0.013(4) -0.011(4) -0.002(3) C42 0.031(4) 0.040(5) 0.073(7) 0.003(5) -0.023(5) -0.007(4) C43 0.047(6) 0.029(5) 0.093(9) -0.016(5) 0.008(6) 0.001(4) C44 0.037(5) 0.045(6) 0.073(7) -0.019(5) 0.000(5) 0.002(4) C45 0.033(4) 0.043(5) 0.049(5) -0.014(4) 0.007(4) -0.003(4) C46 0.055(6) 0.044(5) 0.026(4) 0.000(4) 0.004(4) -0.005(4) Cl1A 0.047(5) 0.028(4) 0.054(6) -0.020(4) 0.010(5) -0.001(4) C17A 0.064(7) 0.058(6) 0.034(5) -0.020(5) -0.018(5) 0.016(5) C23A 0.052(6) 0.092(9) 0.027(4) 0.019(5) 0.011(4) 0.020(6) N4 0.037(4) 0.027(3) 0.043(4) -0.005(3) -0.013(3) 0.001(3) N3 0.034(4) 0.040(4) 0.036(4) 0.001(3) 0.000(3) 0.001(3) N8 0.025(3) 0.028(3) 0.036(4) 0.007(3) -0.003(3) -0.004(2) N6 0.047(5) 0.029(3) 0.046(4) -0.005(3) -0.012(4) 0.001(3) N7 0.022(3) 0.036(4) 0.035(3) 0.000(3) -0.006(3) -0.007(3) N5 0.052(5) 0.050(5) 0.030(4) 0.011(3) -0.002(3) -0.016(4) O2 0.035(4) 0.034(4) 0.030(4) -0.005(3) -0.004(3) 0.006(3) O1 0.036(4) 0.024(3) 0.025(3) 0.006(3) -0.004(3) 0.002(3) O4 0.046(4) 0.039(3) 0.039(3) -0.002(3) -0.006(3) -0.006(3) O3 0.030(3) 0.046(3) 0.035(3) -0.003(3) -0.004(2) -0.005(3) O5 0.30(3) 0.189(19) 0.068(8) -0.002(10) 0.048(13) 0.14(2) O6 0.24(2) 0.098(10) 0.136(13) 0.043(9) 0.123(16) 0.066(12) O7 0.130(15) 0.093(11) 0.41(4) -0.016(16) -0.15(2) -0.020(10) O8 0.181(15) 0.062(6) 0.060(6) -0.010(5) 0.019(7) 0.024(7) O9 0.037(7) 0.095(12) 0.114(13) 0.031(10) -0.016(8) 0.014(7) O10 0.106(15) 0.070(11) 0.18(2) -0.065(13) 0.075(16) -0.030(10) O11 0.040(7) 0.19(2) 0.046(7) -0.021(10) -0.019(6) -0.027(10) O12 0.076(11) 0.18(2) 0.060(9) 0.036(11) -0.028(8) -0.071(13) O13 0.057(9) 0.23(3) 0.091(12) 0.029(15) -0.018(9) 0.037(13) O14 0.32(4) 0.061(9) 0.125(16) -0.009(10) 0.17(2) -0.033(15) O15 0.100(14) 0.089(12) 0.21(2) -0.031(15) -0.092(16) -0.015(11) O16 0.108(15) 0.098(12) 0.109(14) 0.030(11) -0.077(13) -0.028(11) O17 0.188(17) 0.104(10) 0.092(9) 0.001(7) -0.084(10) 0.049(10) O18 0.28(2) 0.066(7) 0.083(9) 0.003(6) -0.037(12) -0.065(11) O19 0.106(8) 0.062(5) 0.061(5) -0.018(4) -0.028(5) -0.010(5) O20 0.162(19) 0.25(3) 0.120(13) -0.082(16) -0.009(13) 0.079(18) Cl1 0.058(2) 0.0357(17) 0.085(3) 0.0102(17) -0.0147(19) 0.0107(15) Cl2 0.0362(13) 0.0654(17) 0.0754(19) 0.0065(14) 0.0157(12) -0.0025(12) Cl3 0.0603(18) 0.095(2) 0.0637(18) -0.0344(17) 0.0139(14) -0.0262(17) Cl4 0.0452(14) 0.0688(17) 0.0537(14) 0.0049(12) 0.0052(11) 0.0010(12) Cl5 0.077(2) 0.073(2) 0.0676(19) 0.0190(16) -0.0243(17) -0.0288(18) Cl6 0.0660(17) 0.0549(14) 0.0466(13) -0.0099(11) -0.0199(12) 0.0149(12) Co1 0.0334(6) 0.0318(6) 0.0217(5) -0.0013(4) -0.0035(4) -0.0061(5) Co2 0.0300(6) 0.0246(5) 0.0234(5) 0.0007(4) -0.0050(4) 0.0011(5) _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 1.551(18) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 O2 1.284(15) . ? C2 C3 1.378(18) . ? C3 C4 1.351(19) . ? C3 Cl1 1.775(13) . ? C4 O1 1.287(14) . ? C4 C5 1.526(18) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C7 C8 1.40(2) . ? C7 C6 1.421(17) . ? C7 H7 0.9500 . ? C8 C9 1.42(2) . ? C8 H8 0.9500 . ? C9 C10 1.367(17) . ? C9 H9 0.9500 . ? C10 N2 1.339(16) . ? C10 C11 1.52(2) . ? C6 N2 1.354(17) . ? C6 H6 0.9500 . ? N2 Co1 1.845(9) . ? C11 N1 1.516(17) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? N1 C23 1.417(16) . ? N1 C17 1.559(16) . ? N1 Co1 1.920(9) . ? C17 C16 1.522(19) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C23 C22 1.542(18) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C12 N4 1.322(14) . ? C12 C13 1.429(12) . ? C12 H12 0.9500 . ? C13 C14 1.45(2) . ? C13 H13 0.9500 . ? C14 C15 1.36(2) . ? C14 H14 0.9500 . ? C15 C16 1.384(17) . ? C15 H15 0.9500 . ? C16 N4 1.321(12) . ? C18 N3 1.356(12) . ? C18 C19 1.415(13) . ? C18 H18 0.9500 . ? C19 C20 1.35(2) . ? C19 H19 0.9500 . ? C20 C21 1.39(2) . ? C20 H20 0.9500 . ? C21 C22 1.350(18) . ? C21 H21 0.9500 . ? C22 N3 1.359(13) . ? C24 C25 1.511(12) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 O4 1.239(11) . ? C25 C26 1.410(13) . ? C26 C27 1.387(13) . ? C26 Cl2 1.741(9) . ? C27 O3 1.279(11) . ? C27 C28 1.497(14) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 N8 1.336(13) . ? C29 C30 1.431(15) . ? C29 H29 0.9500 . ? C30 C31 1.293(19) . ? C30 H30 0.9500 . ? C31 C32 1.40(2) . ? C31 H31 0.9500 . ? C32 C33 1.369(15) . ? C32 H32 0.9500 . ? C33 N8 1.341(12) . ? C33 C34 1.527(17) . ? C34 N5 1.485(13) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 N6 1.390(13) . ? C35 C36 1.397(16) . ? C35 H35 0.9500 . ? C36 C37 1.28(2) . ? C36 H36 0.9500 . ? C37 C38 1.50(3) . ? C37 H37 0.9500 . ? C38 C39 1.371(15) . ? C38 H38 0.9500 . ? C39 N6 1.314(13) . ? C39 C40 1.490(15) . ? C40 N5 1.520(14) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 N7 1.343(12) . ? C41 C42 1.372(14) . ? C41 H41 0.9500 . ? C42 C43 1.406(19) . ? C42 H42 0.9500 . ? C43 C44 1.324(19) . ? C43 H43 0.9500 . ? C44 C45 1.411(14) . ? C44 H44 0.9500 . ? C45 N7 1.330(12) . ? C45 C46 1.501(15) . ? C46 N5 1.477(13) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? Cl1A C3A 1.72(5) . ? O1A C2A 1.47(9) . ? O1A Co1 1.91(3) . ? O2A C4A 1.32(7) . ? O2A Co1 2.08(4) . ? C3A C2A 1.31(6) . ? C3A C4A 1.31(6) . ? C1A C2A 1.542(10) . ? C1A H1A1 0.9800 . ? C1A H1A2 0.9800 . ? C1A H1A3 0.9800 . ? C5A C4A 1.57(8) . ? C5A H5A1 0.9800 . ? C5A H5A2 0.9800 . ? C5A H5A3 0.9800 . ? N1A C11A 1.49(6) . ? N1A Co1 1.86(4) . ? C11A C6A 1.46(7) . ? C11A H11C 0.9900 . ? C11A H11D 0.9900 . ? N2A C10A 1.349(10) . ? N2A C6A 1.354(10) . ? N2A Co1 1.73(4) . ? C6A C9A 1.40(3) . ? C6A Co1 2.50(5) . ? C10A C7A 1.40(3) . ? C10A H4A 0.9500 . ? C7A C8A 1.40(3) . ? C7A H7A 0.9500 . ? C9A C8A 1.40(3) . ? C9A H9A 0.9500 . ? C8A H8A 0.9500 . ? N4 Co1 1.951(8) . ? N3 Co1 1.909(8) . ? N8 Co2 1.942(7) . ? N6 Co2 1.907(8) . ? N7 Co2 1.904(8) . ? N5 Co2 1.939(9) . ? O2 Co1 1.930(8) . ? O1 Co1 1.895(7) . ? O4 Co2 1.917(7) . ? O3 Co2 1.861(7) . ? O5 Cl3 1.390(10) . ? O6 Cl3 1.398(10) . ? O7 Cl3 1.406(10) . ? O8 Cl3 1.411(9) . ? O9 Cl4 1.452(13) . ? O10 Cl4 1.414(16) . ? O11 Cl4 1.449(13) . ? O12 Cl4 1.405(16) . ? O9A Cl4 1.26(2) . ? O10A Cl4 1.28(2) . ? O11A Cl4 1.463(9) . ? O12A Cl4 1.49(2) . ? O13 Cl5 1.455(8) . ? O14 Cl5 1.453(8) . ? O15 Cl5 1.453(8) . ? O16 Cl5 1.460(8) . ? O13A Cl5 1.484(7) . ? O14A Cl5 1.470(7) . ? O15A Cl5 1.466(7) . ? O16A Cl5 1.465(8) . ? O17 Cl6 1.408(11) . ? O18 Cl6 1.373(15) . ? O19 Cl6 1.440(9) . ? O20 Cl6 1.368(18) . ? 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 O2 C2 C3 123.6(11) . . ? O2 C2 C1 115.7(12) . . ? C3 C2 C1 120.8(13) . . ? C4 C3 C2 126.4(12) . . ? C4 C3 Cl1 115.8(10) . . ? C2 C3 Cl1 117.7(10) . . ? O1 C4 C3 124.0(12) . . ? O1 C4 C5 112.4(12) . . ? C3 C4 C5 123.5(12) . . ? C8 C7 C6 120.5(14) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C9 120.1(13) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C10 C9 C8 115.2(12) . . ? C10 C9 H9 122.4 . . ? C8 C9 H9 122.4 . . ? N2 C10 C9 125.3(14) . . ? N2 C10 C11 115.0(12) . . ? C9 C10 C11 119.7(12) . . ? N2 C6 C7 117.4(12) . . ? N2 C6 H6 121.3 . . ? C7 C6 H6 121.3 . . ? C10 N2 C6 121.3(12) . . ? C10 N2 Co1 115.2(9) . . ? C6 N2 Co1 123.4(8) . . ? N1 C11 C10 111.7(11) . . ? N1 C11 H11A 109.3 . . ? C10 C11 H11A 109.3 . . ? N1 C11 H11B 109.3 . . ? C10 C11 H11B 109.3 . . ? H11A C11 H11B 107.9 . . ? C23 N1 C11 115.1(11) . . ? C23 N1 C17 108.7(10) . . ? C11 N1 C17 111.1(10) . . ? C23 N1 Co1 109.9(7) . . ? C11 N1 Co1 107.6(8) . . ? C17 N1 Co1 104.0(7) . . ? C16 C17 N1 108.1(8) . . ? C16 C17 H17A 110.1 . . ? N1 C17 H17A 110.1 . . ? C16 C17 H17B 110.1 . . ? N1 C17 H17B 110.1 . . ? H17A C17 H17B 108.4 . . ? N1 C23 C22 107.6(9) . . ? N1 C23 H23A 110.2 . . ? C22 C23 H23A 110.2 . . ? N1 C23 H23B 110.2 . . ? C22 C23 H23B 110.2 . . ? H23A C23 H23B 108.5 . . ? N4 C12 C13 119.2(11) . . ? N4 C12 H12 120.4 . . ? C13 C12 H12 120.4 . . ? C12 C13 C14 118.4(14) . . ? C12 C13 H13 120.8 . . ? C14 C13 H13 120.8 . . ? C15 C14 C13 117.0(11) . . ? C15 C14 H14 121.5 . . ? C13 C14 H14 121.5 . . ? C14 C15 C16 121.5(13) . . ? C14 C15 H15 119.2 . . ? C16 C15 H15 119.2 . . ? N4 C16 C15 120.7(13) . . ? N4 C16 C17 114.7(9) . . ? C15 C16 C17 124.6(11) . . ? N3 C18 C19 122.4(10) . . ? N3 C18 H18 118.8 . . ? C19 C18 H18 118.8 . . ? C20 C19 C18 117.9(12) . . ? C20 C19 H19 121.0 . . ? C18 C19 H19 121.0 . . ? C19 C20 C21 119.5(11) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C22 C21 C20 120.8(13) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 N3 121.8(13) . . ? C21 C22 C23 126.0(12) . . ? N3 C22 C23 112.1(10) . . ? C25 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C25 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O4 C25 C26 126.2(8) . . ? O4 C25 C24 114.3(8) . . ? C26 C25 C24 119.5(8) . . ? C27 C26 C25 122.6(8) . . ? C27 C26 Cl2 118.6(7) . . ? C25 C26 Cl2 118.8(7) . . ? O3 C27 C26 124.7(8) . . ? O3 C27 C28 114.7(9) . . ? C26 C27 C28 120.4(9) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N8 C29 C30 118.1(9) . . ? N8 C29 H29 121.0 . . ? C30 C29 H29 121.0 . . ? C31 C30 C29 120.3(11) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C31 C32 121.4(9) . . ? C30 C31 H31 119.3 . . ? C32 C31 H31 119.3 . . ? C33 C32 C31 117.7(10) . . ? C33 C32 H32 121.2 . . ? C31 C32 H32 121.2 . . ? N8 C33 C32 121.0(11) . . ? N8 C33 C34 114.3(9) . . ? C32 C33 C34 124.7(9) . . ? N5 C34 C33 108.5(8) . . ? N5 C34 H34A 110.0 . . ? C33 C34 H34A 110.0 . . ? N5 C34 H34B 110.0 . . ? C33 C34 H34B 110.0 . . ? H34A C34 H34B 108.4 . . ? N6 C35 C36 115.7(11) . . ? N6 C35 H35 122.2 . . ? C36 C35 H35 122.2 . . ? C37 C36 C35 129.1(15) . . ? C37 C36 H36 115.4 . . ? C35 C36 H36 115.4 . . ? C36 C37 C38 112.7(14) . . ? C36 C37 H37 123.6 . . ? C38 C37 H37 123.6 . . ? C39 C38 C37 119.2(13) . . ? C39 C38 H38 120.4 . . ? C37 C38 H38 120.4 . . ? N6 C39 C38 122.7(11) . . ? N6 C39 C40 115.2(9) . . ? C38 C39 C40 122.2(11) . . ? C39 C40 N5 113.5(8) . . ? C39 C40 H40A 108.9 . . ? N5 C40 H40A 108.9 . . ? C39 C40 H40B 108.9 . . ? N5 C40 H40B 108.9 . . ? H40A C40 H40B 107.7 . . ? N7 C41 C42 125.8(11) . . ? N7 C41 H41 117.1 . . ? C42 C41 H41 117.1 . . ? C41 C42 C43 115.5(11) . . ? C41 C42 H42 122.3 . . ? C43 C42 H42 122.3 . . ? C44 C43 C42 120.0(10) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 121.1(11) . . ? C43 C44 H44 119.4 . . ? C45 C44 H44 119.4 . . ? N7 C45 C44 120.4(11) . . ? N7 C45 C46 113.4(8) . . ? C44 C45 C46 126.2(10) . . ? N5 C46 C45 108.6(7) . . ? N5 C46 H46A 110.0 . . ? C45 C46 H46A 110.0 . . ? N5 C46 H46B 110.0 . . ? C45 C46 H46B 110.0 . . ? H46A C46 H46B 108.4 . . ? C2A O1A Co1 125(3) . . ? C4A O2A Co1 130(4) . . ? C2A C3A C4A 126(6) . . ? C2A C3A Cl1A 113(4) . . ? C4A C3A Cl1A 121(4) . . ? 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 . . ? C4A C5A H5A1 109.5 . . ? C4A C5A H5A2 109.5 . . ? H5A1 C5A H5A2 109.5 . . ? C4A C5A H5A3 109.5 . . ? H5A1 C5A H5A3 109.5 . . ? H5A2 C5A H5A3 109.5 . . ? C3A C2A O1A 127(4) . . ? C3A C2A C1A 129(6) . . ? O1A C2A C1A 102(4) . . ? C3A C4A O2A 123(6) . . ? C3A C4A C5A 120(6) . . ? O2A C4A C5A 117(5) . . ? C11A N1A Co1 106(3) . . ? C6A C11A N1A 109(4) . . ? C6A C11A H11C 110.0 . . ? N1A C11A H11C 110.0 . . ? C6A C11A H11D 110.0 . . ? N1A C11A H11D 110.0 . . ? H11C C11A H11D 108.3 . . ? C10A N2A C6A 123(5) . . ? C10A N2A Co1 129(3) . . ? C6A N2A Co1 108(3) . . ? N2A C6A C9A 117(5) . . ? N2A C6A C11A 122(5) . . ? C9A C6A C11A 121(3) . . ? N2A C6A Co1 41(2) . . ? C9A C6A Co1 158(3) . . ? C11A C6A Co1 81(3) . . ? N2A C10A C7A 123(5) . . ? N2A C10A H4A 118.7 . . ? C7A C10A H4A 118.7 . . ? C10A C7A C8A 116(4) . . ? C10A C7A H7A 122.0 . . ? C8A C7A H7A 122.0 . . ? C8A C9A C6A 121(5) . . ? C8A C9A H9A 119.3 . . ? C6A C9A H9A 119.3 . . ? C9A C8A C7A 120(4) . . ? C9A C8A H8A 119.9 . . ? C7A C8A H8A 119.9 . . ? C16 N4 C12 123.1(9) . . ? C16 N4 Co1 113.0(8) . . ? C12 N4 Co1 123.9(6) . . ? C18 N3 C22 117.6(9) . . ? C18 N3 Co1 128.0(7) . . ? C22 N3 Co1 114.4(8) . . ? C29 N8 C33 121.4(8) . . ? C29 N8 Co2 125.2(6) . . ? C33 N8 Co2 113.4(7) . . ? C39 N6 C35 120.4(9) . . ? C39 N6 Co2 115.9(7) . . ? C35 N6 Co2 123.7(8) . . ? C45 N7 C41 117.3(9) . . ? C45 N7 Co2 113.9(7) . . ? C41 N7 Co2 128.7(7) . . ? C46 N5 C34 111.2(8) . . ? C46 N5 C40 114.3(9) . . ? C34 N5 C40 111.1(8) . . ? C46 N5 Co2 104.9(5) . . ? C34 N5 Co2 107.1(7) . . ? C40 N5 Co2 107.7(6) . . ? C2 O2 Co1 126.5(8) . . ? C4 O1 Co1 127.5(8) . . ? C25 O4 Co2 125.7(6) . . ? C27 O3 Co2 127.5(6) . . ? O5 Cl3 O6 108.7(11) . . ? O5 Cl3 O7 122.8(15) . . ? O6 Cl3 O7 102.3(14) . . ? O5 Cl3 O8 108.6(9) . . ? O6 Cl3 O8 114.7(12) . . ? O7 Cl3 O8 99.9(13) . . ? O9A Cl4 O10A 131.5(14) . . ? O9A Cl4 O12 109.4(14) . . ? O10A Cl4 O12 91.5(16) . . ? O9A Cl4 O10 51.9(16) . . ? O10A Cl4 O10 151.7(13) . . ? O12 Cl4 O10 114.5(15) . . ? O9A Cl4 O11 60.1(14) . . ? O10A Cl4 O11 72.4(13) . . ? O12 Cl4 O11 105.5(11) . . ? O10 Cl4 O11 108.6(16) . . ? O9A Cl4 O9 135.2(13) . . ? O10A Cl4 O9 49.8(12) . . ? O12 Cl4 O9 115.5(12) . . ? O10 Cl4 O9 105.8(13) . . ? O11 Cl4 O9 106.6(11) . . ? O9A Cl4 O11A 112.9(14) . . ? O10A Cl4 O11A 92.7(14) . . ? O12 Cl4 O11A 118.0(11) . . ? O10 Cl4 O11A 66.0(15) . . ? O11 Cl4 O11A 134.5(11) . . ? O9 Cl4 O11A 43.1(11) . . ? O9A Cl4 O12A 113.8(14) . . ? O10A Cl4 O12A 105.4(14) . . ? O12 Cl4 O12A 28.7(10) . . ? O10 Cl4 O12A 94.2(13) . . ? O11 Cl4 O12A 133.3(13) . . ? O9 Cl4 O12A 105.4(13) . . ? O11A Cl4 O12A 91.9(14) . . ? O14 Cl5 O15 121.0(15) . . ? O14 Cl5 O13 94.1(14) . . ? O15 Cl5 O13 120.1(16) . . ? O14 Cl5 O16 105.3(11) . . ? O15 Cl5 O16 114.0(12) . . ? O13 Cl5 O16 98.4(12) . . ? O14 Cl5 O16A 113.9(15) . . ? O15 Cl5 O16A 65.1(16) . . ? O13 Cl5 O16A 56.3(16) . . ? O16 Cl5 O16A 133.7(14) . . ? O14 Cl5 O15A 122.9(14) . . ? O15 Cl5 O15A 101.9(15) . . ? O13 Cl5 O15A 94.9(14) . . ? O16 Cl5 O15A 17.6(13) . . ? O16A Cl5 O15A 117.8(9) . . ? O14 Cl5 O14A 37.8(13) . . ? O15 Cl5 O14A 140.9(14) . . ? O13 Cl5 O14A 56.4(15) . . ? O16 Cl5 O14A 104.7(13) . . ? O16A Cl5 O14A 92.4(18) . . ? O15A Cl5 O14A 117.1(8) . . ? O14 Cl5 O13A 81.8(12) . . ? O15 Cl5 O13A 42.4(15) . . ? O13 Cl5 O13A 145.9(16) . . ? O16 Cl5 O13A 115.4(14) . . ? O16A Cl5 O13A 94.3(17) . . ? O15A Cl5 O13A 115.9(8) . . ? O14A Cl5 O13A 114.9(8) . . ? O20 Cl6 O18 100.7(16) . . ? O20 Cl6 O17 109.2(12) . . ? O18 Cl6 O17 110.0(13) . . ? O20 Cl6 O19 115.7(11) . . ? O18 Cl6 O19 109.6(7) . . ? O17 Cl6 O19 111.2(8) . . ? N2A Co1 N2 137.8(11) . . ? N2A Co1 N1A 95.7(16) . . ? N2 Co1 N1A 126.2(12) . . ? N2A Co1 O1 46.1(11) . . ? N2 Co1 O1 91.8(4) . . ? N1A Co1 O1 140.8(12) . . ? N2A Co1 N3 91.9(12) . . ? N2 Co1 N3 89.8(4) . . ? N1A Co1 N3 94.1(13) . . ? O1 Co1 N3 95.3(4) . . ? N2A Co1 O1A 92.5(15) . . ? N2 Co1 O1A 45.3(10) . . ? N1A Co1 O1A 170.5(16) . . ? O1 Co1 O1A 46.7(10) . . ? N3 Co1 O1A 90.2(10) . . ? N2A Co1 N1 132.2(11) . . ? N2 Co1 N1 89.9(4) . . ? N1A Co1 N1 37.8(13) . . ? O1 Co1 N1 178.0(4) . . ? N3 Co1 N1 83.6(4) . . ? O1A Co1 N1 134.9(10) . . ? N2A Co1 O2 45.8(11) . . ? N2 Co1 O2 175.7(4) . . ? N1A Co1 O2 50.6(12) . . ? O1 Co1 O2 91.9(3) . . ? N3 Co1 O2 87.7(4) . . ? O1A Co1 O2 138.1(10) . . ? N1 Co1 O2 86.4(4) . . ? N2A Co1 N4 93.2(12) . . ? N2 Co1 N4 92.5(4) . . ? N1A Co1 N4 76.4(13) . . ? O1 Co1 N4 94.7(3) . . ? N3 Co1 N4 169.6(4) . . ? O1A Co1 N4 98.6(10) . . ? N1 Co1 N4 86.2(4) . . ? O2 Co1 N4 89.3(3) . . ? N2A Co1 O2A 176.7(15) . . ? N2 Co1 O2A 41.8(10) . . ? N1A Co1 O2A 84.5(16) . . ? O1 Co1 O2A 133.1(10) . . ? N3 Co1 O2A 91.3(9) . . ? O1A Co1 O2A 87.0(14) . . ? N1 Co1 O2A 48.7(10) . . ? O2 Co1 O2A 134.8(10) . . ? N4 Co1 O2A 83.7(9) . . ? N2A Co1 C6A 31.0(12) . . ? N2 Co1 C6A 168.7(12) . . ? N1A Co1 C6A 64.8(17) . . ? O1 Co1 C6A 77.0(12) . . ? N3 Co1 C6A 91.9(9) . . ? O1A Co1 C6A 123.6(15) . . ? N1 Co1 C6A 101.4(12) . . ? O2 Co1 C6A 15.2(11) . . ? N4 Co1 C6A 87.8(9) . . ? O2A Co1 C6A 149.2(16) . . ? O3 Co2 N7 94.0(3) . . ? O3 Co2 N6 92.0(3) . . ? N7 Co2 N6 90.1(3) . . ? O3 Co2 O4 93.3(3) . . ? N7 Co2 O4 88.8(3) . . ? N6 Co2 O4 174.6(4) . . ? O3 Co2 N5 178.9(4) . . ? N7 Co2 N5 85.0(4) . . ? N6 Co2 N5 87.7(4) . . ? O4 Co2 N5 86.9(3) . . ? O3 Co2 N8 96.2(3) . . ? N7 Co2 N8 169.6(3) . . ? N6 Co2 N8 91.2(3) . . ? O4 Co2 N8 88.9(3) . . ? N5 Co2 N8 84.8(4) . . ? 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 O2 C2 C3 C4 2(2) . . . . ? C1 C2 C3 C4 -177.0(11) . . . . ? O2 C2 C3 Cl1 178.1(9) . . . . ? C1 C2 C3 Cl1 -0.7(15) . . . . ? C2 C3 C4 O1 -2(2) . . . . ? Cl1 C3 C4 O1 -178.2(9) . . . . ? C2 C3 C4 C5 176.7(12) . . . . ? Cl1 C3 C4 C5 0.3(16) . . . . ? C6 C7 C8 C9 -1(2) . . . . ? C7 C8 C9 C10 -1.5(19) . . . . ? C8 C9 C10 N2 3.4(19) . . . . ? C8 C9 C10 C11 -178.8(12) . . . . ? C8 C7 C6 N2 2(2) . . . . ? C9 C10 N2 C6 -2(2) . . . . ? C11 C10 N2 C6 179.7(13) . . . . ? C9 C10 N2 Co1 174.7(10) . . . . ? C11 C10 N2 Co1 -3.2(14) . . . . ? C7 C6 N2 C10 -1(2) . . . . ? C7 C6 N2 Co1 -177.4(10) . . . . ? N2 C10 C11 N1 7.9(17) . . . . ? C9 C10 C11 N1 -170.1(11) . . . . ? C10 C11 N1 C23 114.3(12) . . . . ? C10 C11 N1 C17 -121.7(12) . . . . ? C10 C11 N1 Co1 -8.5(14) . . . . ? C23 N1 C17 C16 -155.4(9) . . . . ? C11 N1 C17 C16 77.0(12) . . . . ? Co1 N1 C17 C16 -38.4(10) . . . . ? C11 N1 C23 C22 -84.1(12) . . . . ? C17 N1 C23 C22 150.6(9) . . . . ? Co1 N1 C23 C22 37.4(12) . . . . ? N4 C12 C13 C14 -2.1(14) . . . . ? C12 C13 C14 C15 3.7(16) . . . . ? C13 C14 C15 C16 -2.6(19) . . . . ? C14 C15 C16 N4 -0.3(18) . . . . ? C14 C15 C16 C17 -176.6(11) . . . . ? N1 C17 C16 N4 26.8(12) . . . . ? N1 C17 C16 C15 -156.6(10) . . . . ? N3 C18 C19 C20 -1.5(17) . . . . ? C18 C19 C20 C21 0(2) . . . . ? C19 C20 C21 C22 -1(2) . . . . ? C20 C21 C22 N3 2(2) . . . . ? C20 C21 C22 C23 179.3(13) . . . . ? N1 C23 C22 C21 156.8(12) . . . . ? N1 C23 C22 N3 -26.1(14) . . . . ? O4 C25 C26 C27 1.2(14) . . . . ? C24 C25 C26 C27 -179.2(9) . . . . ? O4 C25 C26 Cl2 -177.9(7) . . . . ? C24 C25 C26 Cl2 1.6(12) . . . . ? C25 C26 C27 O3 -2.4(14) . . . . ? Cl2 C26 C27 O3 176.7(7) . . . . ? C25 C26 C27 C28 -177.8(9) . . . . ? Cl2 C26 C27 C28 1.3(12) . . . . ? N8 C29 C30 C31 -2.1(15) . . . . ? C29 C30 C31 C32 -1.8(16) . . . . ? C30 C31 C32 C33 3.6(16) . . . . ? C31 C32 C33 N8 -1.6(16) . . . . ? C31 C32 C33 C34 177.2(10) . . . . ? N8 C33 C34 N5 -24.7(12) . . . . ? C32 C33 C34 N5 156.4(10) . . . . ? N6 C35 C36 C37 -4(2) . . . . ? C35 C36 C37 C38 6(2) . . . . ? C36 C37 C38 C39 -4.0(18) . . . . ? C37 C38 C39 N6 1.0(16) . . . . ? C37 C38 C39 C40 -179.3(11) . . . . ? N6 C39 C40 N5 -2.5(13) . . . . ? C38 C39 C40 N5 177.8(9) . . . . ? N7 C41 C42 C43 1.8(14) . . . . ? C41 C42 C43 C44 -0.5(15) . . . . ? C42 C43 C44 C45 -0.9(17) . . . . ? C43 C44 C45 N7 1.4(16) . . . . ? C43 C44 C45 C46 -177.3(10) . . . . ? N7 C45 C46 N5 30.2(11) . . . . ? C44 C45 C46 N5 -151.0(10) . . . . ? C4A C3A C2A O1A -14(14) . . . . ? Cl1A C3A C2A O1A 169(7) . . . . ? C4A C3A C2A C1A -173(7) . . . . ? Cl1A C3A C2A C1A 10(12) . . . . ? Co1 O1A C2A C3A 16(13) . . . . ? Co1 O1A C2A C1A -180(3) . . . . ? C2A C3A C4A O2A 0(12) . . . . ? Cl1A C3A C4A O2A 177(5) . . . . ? C2A C3A C4A C5A -176(7) . . . . ? Cl1A C3A C4A C5A 1(9) . . . . ? Co1 O2A C4A C3A 10(10) . . . . ? Co1 O2A C4A C5A -174(3) . . . . ? Co1 N1A C11A C6A -4(4) . . . . ? C10A N2A C6A C9A 0(2) . . . . ? Co1 N2A C6A C9A -178(3) . . . . ? C10A N2A C6A C11A -180(4) . . . . ? Co1 N2A C6A C11A 2(4) . . . . ? C10A N2A C6A Co1 178(3) . . . . ? N1A C11A C6A N2A 1(5) . . . . ? N1A C11A C6A C9A -179(3) . . . . ? N1A C11A C6A Co1 3(3) . . . . ? C6A N2A C10A C7A -1(3) . . . . ? Co1 N2A C10A C7A 177(3) . . . . ? N2A C10A C7A C8A 0(3) . . . . ? N2A C6A C9A C8A 1(3) . . . . ? C11A C6A C9A C8A -179(4) . . . . ? Co1 C6A C9A C8A -3(7) . . . . ? C6A C9A C8A C7A -2(4) . . . . ? C10A C7A C8A C9A 2(3) . . . . ? C15 C16 N4 C12 2.2(15) . . . . ? C17 C16 N4 C12 178.9(9) . . . . ? C15 C16 N4 Co1 -177.9(8) . . . . ? C17 C16 N4 Co1 -1.2(10) . . . . ? C13 C12 N4 C16 -0.9(14) . . . . ? C13 C12 N4 Co1 179.2(7) . . . . ? C19 C18 N3 C22 2.9(15) . . . . ? C19 C18 N3 Co1 179.4(8) . . . . ? C21 C22 N3 C18 -3.4(16) . . . . ? C23 C22 N3 C18 179.4(9) . . . . ? C21 C22 N3 Co1 179.7(10) . . . . ? C23 C22 N3 Co1 2.5(11) . . . . ? C30 C29 N8 C33 4.1(13) . . . . ? C30 C29 N8 Co2 -178.1(6) . . . . ? C32 C33 N8 C29 -2.3(15) . . . . ? C34 C33 N8 C29 178.8(9) . . . . ? C32 C33 N8 Co2 179.7(8) . . . . ? C34 C33 N8 Co2 0.8(10) . . . . ? C38 C39 N6 C35 1.1(14) . . . . ? C40 C39 N6 C35 -178.6(9) . . . . ? C38 C39 N6 Co2 -179.0(8) . . . . ? C40 C39 N6 Co2 1.3(10) . . . . ? C36 C35 N6 C39 -0.1(14) . . . . ? C36 C35 N6 Co2 179.9(8) . . . . ? C44 C45 N7 C41 -0.2(13) . . . . ? C46 C45 N7 C41 178.6(8) . . . . ? C44 C45 N7 Co2 176.3(7) . . . . ? C46 C45 N7 Co2 -4.8(10) . . . . ? C42 C41 N7 C45 -1.4(13) . . . . ? C42 C41 N7 Co2 -177.4(7) . . . . ? C45 C46 N5 C34 -154.9(9) . . . . ? C45 C46 N5 C40 78.2(10) . . . . ? C45 C46 N5 Co2 -39.5(9) . . . . ? C33 C34 N5 C46 150.1(8) . . . . ? C33 C34 N5 C40 -81.3(11) . . . . ? C33 C34 N5 Co2 36.0(9) . . . . ? C39 C40 N5 C46 -113.8(10) . . . . ? C39 C40 N5 C34 119.3(10) . . . . ? C39 C40 N5 Co2 2.4(11) . . . . ? C3 C2 O2 Co1 0.5(16) . . . . ? C1 C2 O2 Co1 179.3(7) . . . . ? C3 C4 O1 Co1 -0.5(16) . . . . ? C5 C4 O1 Co1 -179.1(8) . . . . ? C26 C25 O4 Co2 -0.8(13) . . . . ? C24 C25 O4 Co2 179.6(7) . . . . ? C26 C27 O3 Co2 3.2(13) . . . . ? C28 C27 O3 Co2 178.9(7) . . . . ? C10A N2A Co1 N2 5(4) . . . . ? C6A N2A Co1 N2 -177.8(15) . . . . ? C10A N2A Co1 N1A 178(3) . . . . ? C6A N2A Co1 N1A -4(2) . . . . ? C10A N2A Co1 O1 8(2) . . . . ? C6A N2A Co1 O1 -174(3) . . . . ? C10A N2A Co1 N3 -87(3) . . . . ? C6A N2A Co1 N3 90.5(17) . . . . ? C10A N2A Co1 O1A 3(3) . . . . ? C6A N2A Co1 O1A -179.2(19) . . . . ? C10A N2A Co1 N1 -170(2) . . . . ? C6A N2A Co1 N1 7(2) . . . . ? C10A N2A Co1 O2 -172(3) . . . . ? C6A N2A Co1 O2 5.5(15) . . . . ? C10A N2A Co1 N4 102(3) . . . . ? C6A N2A Co1 N4 -80.5(17) . . . . ? C10A N2A Co1 O2A 85(26) . . . . ? C6A N2A Co1 O2A -97(26) . . . . ? C10A N2A Co1 C6A -178(3) . . . . ? C10 N2 Co1 N2A -177.9(18) . . . . ? C6 N2 Co1 N2A -1(2) . . . . ? C10 N2 Co1 N1A 9.6(18) . . . . ? C6 N2 Co1 N1A -173.3(19) . . . . ? C10 N2 Co1 O1 179.3(8) . . . . ? C6 N2 Co1 O1 -3.6(12) . . . . ? C10 N2 Co1 N3 -85.4(8) . . . . ? C6 N2 Co1 N3 91.7(12) . . . . ? C10 N2 Co1 O1A -175.9(18) . . . . ? C6 N2 Co1 O1A 1.2(18) . . . . ? C10 N2 Co1 N1 -1.7(9) . . . . ? C6 N2 Co1 N1 175.4(12) . . . . ? C10 N2 Co1 O2 -31(6) . . . . ? C6 N2 Co1 O2 146(5) . . . . ? C10 N2 Co1 N4 84.5(8) . . . . ? C6 N2 Co1 N4 -98.4(12) . . . . ? C10 N2 Co1 O2A 6.9(15) . . . . ? C6 N2 Co1 O2A -176.0(19) . . . . ? C10 N2 Co1 C6A 176(5) . . . . ? C6 N2 Co1 C6A -7(5) . . . . ? C11A N1A Co1 N2A 4(3) . . . . ? C11A N1A Co1 N2 179(2) . . . . ? C11A N1A Co1 O1 16(4) . . . . ? C11A N1A Co1 N3 -88(3) . . . . ? C11A N1A Co1 O1A 155(9) . . . . ? C11A N1A Co1 N1 -162(4) . . . . ? C11A N1A Co1 O2 -4(2) . . . . ? C11A N1A Co1 N4 96(3) . . . . ? C11A N1A Co1 O2A -179(3) . . . . ? C11A N1A Co1 C6A 2(2) . . . . ? C4 O1 Co1 N2A 2.2(19) . . . . ? C4 O1 Co1 N2 179.6(9) . . . . ? C4 O1 Co1 N1A -13(2) . . . . ? C4 O1 Co1 N3 89.7(9) . . . . ? C4 O1 Co1 O1A 175.0(18) . . . . ? C4 O1 Co1 N1 32(13) . . . . ? C4 O1 Co1 O2 1.8(9) . . . . ? C4 O1 Co1 N4 -87.7(9) . . . . ? C4 O1 Co1 O2A -173.4(14) . . . . ? C4 O1 Co1 C6A -1.0(12) . . . . ? C18 N3 Co1 N2A 66.2(14) . . . . ? C22 N3 Co1 N2A -117.2(13) . . . . ? C18 N3 Co1 N2 -71.5(9) . . . . ? C22 N3 Co1 N2 105.0(8) . . . . ? C18 N3 Co1 N1A 162.1(15) . . . . ? C22 N3 Co1 N1A -21.3(14) . . . . ? C18 N3 Co1 O1 20.2(9) . . . . ? C22 N3 Co1 O1 -163.3(7) . . . . ? C18 N3 Co1 O1A -26.3(13) . . . . ? C22 N3 Co1 O1A 150.3(12) . . . . ? C18 N3 Co1 N1 -161.5(9) . . . . ? C22 N3 Co1 N1 15.1(8) . . . . ? C18 N3 Co1 O2 111.9(9) . . . . ? C22 N3 Co1 O2 -71.6(7) . . . . ? C18 N3 Co1 N4 -174.5(15) . . . . ? C22 N3 Co1 N4 2(2) . . . . ? C18 N3 Co1 O2A -113.3(13) . . . . ? C22 N3 Co1 O2A 63.2(12) . . . . ? C18 N3 Co1 C6A 97.3(14) . . . . ? C22 N3 Co1 C6A -86.2(14) . . . . ? C2A O1A Co1 N2A 171(6) . . . . ? C2A O1A Co1 N2 -7(5) . . . . ? C2A O1A Co1 N1A 20(12) . . . . ? C2A O1A Co1 O1 166(6) . . . . ? C2A O1A Co1 N3 -97(6) . . . . ? C2A O1A Co1 N1 -16(6) . . . . ? C2A O1A Co1 O2 176(5) . . . . ? C2A O1A Co1 N4 78(6) . . . . ? C2A O1A Co1 O2A -6(6) . . . . ? C2A O1A Co1 C6A 171(6) . . . . ? C23 N1 Co1 N2A 56.5(19) . . . . ? C11 N1 Co1 N2A -177.6(17) . . . . ? C17 N1 Co1 N2A -59.7(18) . . . . ? C23 N1 Co1 N2 -120.1(9) . . . . ? C11 N1 Co1 N2 5.8(9) . . . . ? C17 N1 Co1 N2 123.7(7) . . . . ? C23 N1 Co1 N1A 75(2) . . . . ? C11 N1 Co1 N1A -159(2) . . . . ? C17 N1 Co1 N1A -41(2) . . . . ? C23 N1 Co1 O1 27(14) . . . . ? C11 N1 Co1 O1 153(13) . . . . ? C17 N1 Co1 O1 -89(13) . . . . ? C23 N1 Co1 N3 -30.3(9) . . . . ? C11 N1 Co1 N3 95.6(9) . . . . ? C17 N1 Co1 N3 -146.5(8) . . . . ? C23 N1 Co1 O1A -114.2(17) . . . . ? C11 N1 Co1 O1A 11.7(18) . . . . ? C17 N1 Co1 O1A 129.6(15) . . . . ? C23 N1 Co1 O2 57.8(9) . . . . ? C11 N1 Co1 O2 -176.3(9) . . . . ? C17 N1 Co1 O2 -58.4(7) . . . . ? C23 N1 Co1 N4 147.4(9) . . . . ? C11 N1 Co1 N4 -86.7(9) . . . . ? C17 N1 Co1 N4 31.2(7) . . . . ? C23 N1 Co1 O2A -127.7(16) . . . . ? C11 N1 Co1 O2A -1.8(14) . . . . ? C17 N1 Co1 O2A 116.1(15) . . . . ? C23 N1 Co1 C6A 60.3(13) . . . . ? C11 N1 Co1 C6A -173.7(12) . . . . ? C17 N1 Co1 C6A -55.9(12) . . . . ? C2 O2 Co1 N2A -2.2(18) . . . . ? C2 O2 Co1 N2 -151(5) . . . . ? C2 O2 Co1 N1A 165.7(19) . . . . ? C2 O2 Co1 O1 -1.8(9) . . . . ? C2 O2 Co1 N3 -97.1(9) . . . . ? C2 O2 Co1 O1A -9.3(19) . . . . ? C2 O2 Co1 N1 179.2(10) . . . . ? C2 O2 Co1 N4 92.9(9) . . . . ? C2 O2 Co1 O2A 173.3(15) . . . . ? C2 O2 Co1 C6A 9(4) . . . . ? C16 N4 Co1 N2A 113.3(12) . . . . ? C12 N4 Co1 N2A -66.8(13) . . . . ? C16 N4 Co1 N2 -108.5(7) . . . . ? C12 N4 Co1 N2 71.4(8) . . . . ? C16 N4 Co1 N1A 18.2(14) . . . . ? C12 N4 Co1 N1A -161.9(15) . . . . ? C16 N4 Co1 O1 159.5(6) . . . . ? C12 N4 Co1 O1 -20.6(8) . . . . ? C16 N4 Co1 N3 -6(2) . . . . ? C12 N4 Co1 N3 174.0(16) . . . . ? C16 N4 Co1 O1A -153.6(12) . . . . ? C12 N4 Co1 O1A 26.3(12) . . . . ? C16 N4 Co1 N1 -18.8(7) . . . . ? C12 N4 Co1 N1 161.1(8) . . . . ? C16 N4 Co1 O2 67.6(7) . . . . ? C12 N4 Co1 O2 -112.5(8) . . . . ? C16 N4 Co1 O2A -67.6(12) . . . . ? C12 N4 Co1 O2A 112.3(12) . . . . ? C16 N4 Co1 C6A 82.7(13) . . . . ? C12 N4 Co1 C6A -97.4(14) . . . . ? C4A O2A Co1 N2A -89(26) . . . . ? C4A O2A Co1 N2 -4(5) . . . . ? C4A O2A Co1 N1A 178(5) . . . . ? C4A O2A Co1 O1 -15(6) . . . . ? C4A O2A Co1 N3 84(5) . . . . ? C4A O2A Co1 O1A -6(5) . . . . ? C4A O2A Co1 N1 164(6) . . . . ? C4A O2A Co1 O2 172(5) . . . . ? C4A O2A Co1 N4 -105(5) . . . . ? C4A O2A Co1 C6A 180(5) . . . . ? C9A C6A Co1 N2A 6(6) . . . . ? C11A C6A Co1 N2A -178(3) . . . . ? N2A C6A Co1 N2 8(5) . . . . ? C9A C6A Co1 N2 13(9) . . . . ? C11A C6A Co1 N2 -170(4) . . . . ? N2A C6A Co1 N1A 176(2) . . . . ? C9A C6A Co1 N1A -178(6) . . . . ? C11A C6A Co1 N1A -2(2) . . . . ? N2A C6A Co1 O1 4.5(19) . . . . ? C9A C6A Co1 O1 10(5) . . . . ? C11A C6A Co1 O1 -174(2) . . . . ? N2A C6A Co1 N3 -90.6(19) . . . . ? C9A C6A Co1 N3 -85(6) . . . . ? C11A C6A Co1 N3 91(2) . . . . ? N2A C6A Co1 O1A 1(2) . . . . ? C9A C6A Co1 O1A 7(6) . . . . ? C11A C6A Co1 O1A -177(2) . . . . ? N2A C6A Co1 N1 -174.4(19) . . . . ? C9A C6A Co1 N1 -169(5) . . . . ? C11A C6A Co1 N1 8(2) . . . . ? N2A C6A Co1 O2 -165(4) . . . . ? C9A C6A Co1 O2 -159(8) . . . . ? C11A C6A Co1 O2 17(3) . . . . ? N2A C6A Co1 N4 99.8(19) . . . . ? C9A C6A Co1 N4 106(6) . . . . ? C11A C6A Co1 N4 -78(2) . . . . ? N2A C6A Co1 O2A 174(3) . . . . ? C9A C6A Co1 O2A 179(5) . . . . ? C11A C6A Co1 O2A -4(4) . . . . ? C27 O3 Co2 N7 -91.3(8) . . . . ? C27 O3 Co2 N6 178.5(8) . . . . ? C27 O3 Co2 O4 -2.2(8) . . . . ? C27 O3 Co2 N5 -105(19) . . . . ? C27 O3 Co2 N8 87.0(8) . . . . ? C45 N7 Co2 O3 164.9(6) . . . . ? C41 N7 Co2 O3 -19.0(7) . . . . ? C45 N7 Co2 N6 -103.0(7) . . . . ? C41 N7 Co2 N6 73.1(8) . . . . ? C45 N7 Co2 O4 71.7(6) . . . . ? C41 N7 Co2 O4 -112.2(7) . . . . ? C45 N7 Co2 N5 -15.3(7) . . . . ? C41 N7 Co2 N5 160.8(8) . . . . ? C45 N7 Co2 N8 -6(2) . . . . ? C41 N7 Co2 N8 170.6(14) . . . . ? C39 N6 Co2 O3 179.0(7) . . . . ? C35 N6 Co2 O3 -1.0(8) . . . . ? C39 N6 Co2 N7 85.0(7) . . . . ? C35 N6 Co2 N7 -95.0(8) . . . . ? C39 N6 Co2 O4 7(4) . . . . ? C35 N6 Co2 O4 -173(3) . . . . ? C39 N6 Co2 N5 0.1(7) . . . . ? C35 N6 Co2 N5 -180.0(8) . . . . ? C39 N6 Co2 N8 -84.7(7) . . . . ? C35 N6 Co2 N8 95.3(8) . . . . ? C25 O4 Co2 O3 1.0(8) . . . . ? C25 O4 Co2 N7 94.9(7) . . . . ? C25 O4 Co2 N6 173(3) . . . . ? C25 O4 Co2 N5 180.0(8) . . . . ? C25 O4 Co2 N8 -95.2(7) . . . . ? C46 N5 Co2 O3 45(20) . . . . ? C34 N5 Co2 O3 163(19) . . . . ? C40 N5 Co2 O3 -78(19) . . . . ? C46 N5 Co2 N7 30.5(7) . . . . ? C34 N5 Co2 N7 148.8(7) . . . . ? C40 N5 Co2 N7 -91.7(7) . . . . ? C46 N5 Co2 N6 120.8(7) . . . . ? C34 N5 Co2 N6 -120.9(7) . . . . ? C40 N5 Co2 N6 -1.4(7) . . . . ? C46 N5 Co2 O4 -58.6(7) . . . . ? C34 N5 Co2 O4 59.7(6) . . . . ? C40 N5 Co2 O4 179.3(7) . . . . ? C46 N5 Co2 N8 -147.8(7) . . . . ? C34 N5 Co2 N8 -29.5(6) . . . . ? C40 N5 Co2 N8 90.1(7) . . . . ? C29 N8 Co2 O3 18.6(8) . . . . ? C33 N8 Co2 O3 -163.5(6) . . . . ? C29 N8 Co2 N7 -171.0(14) . . . . ? C33 N8 Co2 N7 7(2) . . . . ? C29 N8 Co2 N6 -73.6(8) . . . . ? C33 N8 Co2 N6 104.3(7) . . . . ? C29 N8 Co2 O4 111.8(7) . . . . ? C33 N8 Co2 O4 -70.2(7) . . . . ? C29 N8 Co2 N5 -161.2(8) . . . . ? C33 N8 Co2 N5 16.8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.756 _refine_diff_density_min -0.589 _refine_diff_density_rms 0.120 data_8 _database_code_depnum_ccdc_archive 'CCDC 866272' #TrackingRef '- combined revised cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H27 Co N5 O2, (C2 H6 O1), Cl O4, 2(H2 O)' _chemical_formula_sum 'C31 H30 Cl Co N5 O9' _chemical_formula_weight 710.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2 ' _symmetry_space_group_name_Hall 'P 2 2ab' _symmetry_Int_Tables_number 18 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 14.729(5) _cell_length_b 23.560(8) _cell_length_c 9.935(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3447.4(19) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1033 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 26.91 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.501 _exptl_crystal_size_mid 0.255 _exptl_crystal_size_min 0.242 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1468 _exptl_absorpt_coefficient_mu 0.633 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.853 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; SADABS (Sheldrick, 1996) ; _diffrn_crystal_treatment ; attached with Paratone-N oil, to a short length of fibre supported on a thin piece of copper wire inserted in a copper mounting pin. The crystal was quenched in a cold nitrogen gas stream from an Oxford Cryosystems Cryostream. ; _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 SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 212 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.05 _diffrn_reflns_number 34314 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 28.30 _reflns_number_total 8350 _reflns_number_gt 7494 _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 ; xtal 3.6 (Hall,du Boulay, D.J. & Olthof-Hazekamp, R. 1999) ORTEPII (Johnson,C.K., 1976). WinGX (Farrugia, 1999) ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.04P)^2^+4.0P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(2) _refine_ls_number_reflns 8350 _refine_ls_number_parameters 352 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0730 _refine_ls_R_factor_gt 0.0656 _refine_ls_wR_factor_ref 0.1651 _refine_ls_wR_factor_gt 0.1612 _refine_ls_goodness_of_fit_ref 1.393 _refine_ls_restrained_S_all 1.393 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.63384(3) 0.16948(2) 0.55210(5) 0.03198(12) Uani 1 1 d . . . O1 O 0.64393(17) 0.16551(12) 0.7379(2) 0.0344(5) Uani 1 1 d . A . O2 O 0.63923(19) 0.24819(10) 0.5728(3) 0.0369(6) Uani 1 1 d . . . N1 N 0.6259(2) 0.17477(15) 0.3559(3) 0.0391(7) Uani 1 1 d . . . N2 N 0.6271(2) 0.08786(12) 0.5295(3) 0.0342(7) Uani 1 1 d . . . N3 N 0.7625(2) 0.16878(15) 0.5227(3) 0.0372(7) Uani 1 1 d . . . N4 N 0.50367(19) 0.17438(13) 0.5494(3) 0.0344(6) Uani 1 1 d . . . N5 N 0.6566(2) 0.26132(14) 0.7085(4) 0.0390(8) Uani 1 1 d . A . C1 C 0.6230(4) 0.11669(19) 0.2967(4) 0.0530(12) Uani 1 1 d . . . H1A H 0.6771 0.1112 0.2389 0.064 Uiso 1 1 calc R . . H1B H 0.5685 0.1133 0.2389 0.064 Uiso 1 1 calc R . . C2 C 0.6208(3) 0.07044(17) 0.4023(4) 0.0393(9) Uani 1 1 d . . . C3 C 0.6161(3) 0.0132(2) 0.3676(5) 0.0517(11) Uani 1 1 d . . . H3 H 0.6134 0.0016 0.2760 0.062 Uiso 1 1 calc R . . C4 C 0.6154(3) -0.02594(19) 0.4697(5) 0.0541(12) Uani 1 1 d . . . H4 H 0.6113 -0.0652 0.4492 0.065 Uiso 1 1 calc R . . C5 C 0.6207(4) -0.00819(18) 0.6039(5) 0.0500(11) Uani 1 1 d . . . H5 H 0.6204 -0.0351 0.6751 0.060 Uiso 1 1 calc R . . C6 C 0.6266(3) 0.04916(17) 0.6308(4) 0.0406(9) Uani 1 1 d . . . H6 H 0.6303 0.0617 0.7214 0.049 Uiso 1 1 calc R . . C7 C 0.7093(3) 0.2054(2) 0.3146(5) 0.0476(11) Uani 1 1 d . . . H7A H 0.7005 0.2468 0.3260 0.057 Uiso 1 1 calc R . . H7B H 0.7224 0.1978 0.2186 0.057 Uiso 1 1 calc R . . C8 C 0.7868(3) 0.18589(19) 0.3995(5) 0.0431(10) Uani 1 1 d . . . C9 C 0.8760(3) 0.1880(2) 0.3597(5) 0.0540(12) Uani 1 1 d . . . H9 H 0.8913 0.1996 0.2710 0.065 Uiso 1 1 calc R . . C10 C 0.9430(3) 0.1732(2) 0.4497(6) 0.0569(12) Uani 1 1 d . . . H10 H 1.0051 0.1751 0.4243 0.068 Uiso 1 1 calc R . . C11 C 0.9188(3) 0.1553(2) 0.5787(6) 0.0525(12) Uani 1 1 d . . . H11 H 0.9638 0.1451 0.6428 0.063 Uiso 1 1 calc R . . C12 C 0.8269(3) 0.15298(18) 0.6108(5) 0.0419(10) Uani 1 1 d . . . H12 H 0.8092 0.1398 0.6974 0.050 Uiso 1 1 calc R . . C13 C 0.5410(3) 0.2073(2) 0.3278(4) 0.0452(10) Uani 1 1 d . . . H13A H 0.5192 0.1986 0.2358 0.054 Uiso 1 1 calc R . . H13B H 0.5533 0.2485 0.3335 0.054 Uiso 1 1 calc R . . C14 C 0.4701(3) 0.19097(17) 0.4290(5) 0.0405(9) Uani 1 1 d . . . C15 C 0.3779(3) 0.19386(18) 0.4067(5) 0.0471(11) Uani 1 1 d . . . H15 H 0.3548 0.2046 0.3211 0.057 Uiso 1 1 calc R . . C16 C 0.3195(3) 0.18083(18) 0.5115(5) 0.0494(12) Uani 1 1 d . . . H16 H 0.2557 0.1830 0.4984 0.059 Uiso 1 1 calc R . . C17 C 0.3540(3) 0.16469(18) 0.6351(5) 0.0435(9) Uani 1 1 d . . . H17 H 0.3147 0.1559 0.7081 0.052 Uiso 1 1 calc R . . C18 C 0.4477(3) 0.16174(17) 0.6496(4) 0.0387(9) Uani 1 1 d . . . H18 H 0.4725 0.1503 0.7337 0.046 Uiso 1 1 calc R . . C19 C 0.6578(2) 0.21705(17) 0.7852(3) 0.0355(8) Uani 1 1 d D . . C20A C 0.6791(7) 0.2239(4) 0.9322(5) 0.041(3) Uiso 0.75 1 d PD A 1 H20A H 0.6310 0.2059 0.9871 0.050 Uiso 0.75 1 calc PR A 1 H20B H 0.6816 0.2647 0.9556 0.050 Uiso 0.75 1 calc PR A 1 C20B C 0.6830(19) 0.2174(13) 0.9319(9) 0.039(8) Uiso 0.25 1 d PD A 2 H20C H 0.6627 0.2540 0.9701 0.046 Uiso 0.25 1 calc PR A 2 H20D H 0.6472 0.1872 0.9768 0.046 Uiso 0.25 1 calc PR A 2 C21A C 0.77200(19) 0.19560(12) 0.9624(4) 0.0412(13) Uiso 0.75 1 d PG A 1 C22A C 0.8466(2) 0.23040(12) 0.9702(4) 0.0455(13) Uiso 0.75 1 d PG A 1 H22A H 0.8397 0.2698 0.9528 0.055 Uiso 0.75 1 calc PR A 1 C23A C 0.9331(2) 0.20913(15) 1.0035(4) 0.0574(16) Uiso 0.75 1 d PG A 1 H23A H 0.9834 0.2342 1.0089 0.069 Uiso 0.75 1 calc PR A 1 C24A C 0.94467(17) 0.15290(16) 1.0277(4) 0.069(2) Uiso 0.75 1 d PG A 1 H24A H 1.0035 0.1389 1.0486 0.083 Uiso 0.75 1 calc PR A 1 C25A C 0.87048(19) 0.11482(12) 1.0225(3) 0.0590(16) Uiso 0.75 1 d PG A 1 C26A C 0.8804(3) 0.05642(13) 1.0497(5) 0.099(3) Uiso 0.75 1 d PG A 1 H26A H 0.9387 0.0415 1.0706 0.119 Uiso 0.75 1 calc PR A 1 C27A C 0.8071(3) 0.02119(12) 1.0463(5) 0.103(3) Uiso 0.75 1 d PG A 1 H27A H 0.8144 -0.0178 1.0679 0.123 Uiso 0.75 1 calc PR A 1 C28A C 0.7223(3) 0.04154(13) 1.0120(5) 0.070(2) Uiso 0.75 1 d PG A 1 H28A H 0.6725 0.0161 1.0071 0.084 Uiso 0.75 1 calc PR A 1 C29A C 0.7091(2) 0.09764(14) 0.9848(4) 0.0532(15) Uiso 0.75 1 d PG A 1 H29A H 0.6498 0.1111 0.9648 0.064 Uiso 0.75 1 calc PR A 1 C30A C 0.78493(17) 0.13690(11) 0.9864(3) 0.0453(14) Uiso 0.75 1 d PG A 1 C21B C 0.7733(5) 0.2098(3) 0.9680(10) 0.035(3) Uiso 0.25 1 d PG A 2 C22B C 0.8370(6) 0.2522(3) 0.9775(11) 0.039(4) Uiso 0.25 1 d PG A 2 H22B H 0.8177 0.2907 0.9738 0.047 Uiso 0.25 1 calc PR A 2 C23B C 0.9300(6) 0.2402(4) 0.9924(11) 0.036(3) Uiso 0.25 1 d PG A 2 H23B H 0.9726 0.2703 0.9995 0.043 Uiso 0.25 1 calc PR A 2 C24B C 0.9592(5) 0.1855(4) 0.9968(11) 0.053(5) Uiso 0.25 1 d PG A 2 H24B H 1.0222 0.1779 1.0054 0.063 Uiso 0.25 1 calc PR A 2 C25B C 0.8971(5) 0.1398(3) 0.9888(9) 0.063(5) Uiso 0.25 1 d PG A 2 C26B C 0.9254(7) 0.0828(4) 0.9956(13) 0.086(8) Uiso 0.25 1 d PG A 2 H26B H 0.9882 0.0741 1.0040 0.104 Uiso 0.25 1 calc PR A 2 C27B C 0.8635(9) 0.0399(3) 0.9903(14) 0.075(6) Uiso 0.25 1 d PG A 2 H27B H 0.8833 0.0016 0.9980 0.090 Uiso 0.25 1 calc PR A 2 C28B C 0.7723(8) 0.0513(3) 0.9736(13) 0.080(7) Uiso 0.25 1 d PG A 2 H28B H 0.7304 0.0208 0.9670 0.096 Uiso 0.25 1 calc PR A 2 C29B C 0.7413(6) 0.1058(4) 0.9666(12) 0.046(4) Uiso 0.25 1 d PG A 2 H29B H 0.6782 0.1131 0.9585 0.055 Uiso 0.25 1 calc PR A 2 C30B C 0.8051(5) 0.1521(3) 0.9715(8) 0.053(5) Uiso 0.25 1 d PG A 2 Cl1A Cl 0.41407(17) 0.10763(11) 0.0212(2) 0.0357(7) Uiso 0.40 1 d PG B 1 O3A O 0.4711(4) 0.15615(18) 0.0205(6) 0.040(2) Uiso 0.40 1 d PG B 1 O4A O 0.4346(5) 0.0720(2) -0.0902(5) 0.070(3) Uiso 0.40 1 d PG B 1 O5A O 0.3219(2) 0.1260(3) 0.0156(7) 0.071(3) Uiso 0.40 1 d PG B 1 O6A O 0.4279(4) 0.0779(2) 0.1450(4) 0.057(2) Uiso 0.40 1 d PG B 1 Cl1B Cl 0.4281(2) 0.09725(16) 0.0356(4) 0.0222(8) Uiso 0.25 1 d PG C 2 O3B O 0.4835(5) 0.1448(3) 0.0053(9) 0.031(3) Uiso 0.25 1 d PG C 2 O4B O 0.3749(5) 0.0821(4) -0.0783(6) 0.038(2) Uiso 0.25 1 d PG C 2 O5B O 0.3713(5) 0.1113(4) 0.1469(6) 0.045 Uiso 0.25 1 d PG C 2 O6B O 0.4858(5) 0.0512(3) 0.0740(9) 0.046(3) Uiso 0.25 1 d PG C 2 Cl1C Cl 0.4275(5) 0.0897(3) 0.0333(8) 0.144(4) Uiso 0.35 1 d PG D 3 O3C O 0.5033(7) 0.1243(5) 0.0013(15) 0.143(8) Uiso 0.35 1 d PG D 3 O4C O 0.4521(9) 0.0314(4) 0.0276(14) 0.112 Uiso 0.35 1 d PG D 3 O5C O 0.3564(8) 0.1016(6) -0.0599(10) 0.102(5) Uiso 0.35 1 d PG D 3 O6C O 0.3969(8) 0.1043(6) 0.1654(8) 0.093(5) Uiso 0.35 1 d PG D 3 O7A O 0.1327(12) 0.1479(5) 0.7499(15) 0.198(9) Uiso 0.50 1 d P E 1 H7OA H 0.1259 0.1752 0.8034 0.296 Uiso 0.50 1 calc PRD E 1 C31 C 0.1452(11) 0.1074(6) 0.8092(11) 0.092(4) Uiso 0.50 1 d PD E 1 H31A H 0.1906 0.0841 0.7610 0.111 Uiso 0.50 1 calc PR E 1 H31B H 0.0880 0.0854 0.8136 0.111 Uiso 0.50 1 calc PR E 1 C32 C 0.1786(8) 0.1182(5) 0.9505(11) 0.074(3) Uiso 0.50 1 d PD E 1 H32A H 0.1843 0.0820 0.9984 0.110 Uiso 0.50 1 calc PR E 1 H32B H 0.1352 0.1426 0.9979 0.110 Uiso 0.50 1 calc PR E 1 H32C H 0.2379 0.1370 0.9470 0.110 Uiso 0.50 1 calc PR E 1 O7B O 0.1287(5) 0.1531(3) 0.6867(7) 0.0502(15) Uiso 0.50 1 d P F 2 O8A O 0.6912(7) 0.3742(4) 0.7717(11) 0.073(3) Uiso 0.50 1 d P . . O8B O 0.6568(9) 0.3733(6) 0.7791(13) 0.102(4) Uiso 0.50 1 d P . . O9A O 0.1506(5) 0.0825(3) 0.4678(8) 0.069(2) Uiso 0.50 1 d P . . O9B O 0.0892(12) 0.0365(7) 0.4188(18) 0.076(5) Uiso 0.25 1 d P . . O9C O 0.1391(16) -0.0142(9) 0.422(2) 0.098(6) Uiso 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0274(2) 0.0337(2) 0.0348(2) 0.0024(2) -0.0015(2) -0.0024(2) O1 0.0337(13) 0.0372(13) 0.0323(12) -0.0015(11) -0.0017(10) -0.0037(13) O2 0.0345(13) 0.0349(12) 0.0413(15) 0.0046(11) 0.0004(13) -0.0024(11) N1 0.0425(17) 0.0431(17) 0.0317(14) 0.0063(14) -0.0030(14) -0.0047(17) N2 0.0320(14) 0.0346(15) 0.0359(17) -0.0008(12) -0.0012(14) 0.0009(13) N3 0.0292(14) 0.0352(15) 0.0473(19) -0.0033(16) 0.0012(13) -0.0010(14) N4 0.0292(13) 0.0334(15) 0.0408(16) 0.0060(17) -0.0049(13) -0.0008(12) N5 0.0355(18) 0.0373(17) 0.0443(19) -0.0044(14) 0.0013(14) -0.0033(13) C1 0.072(3) 0.049(2) 0.038(2) -0.0002(18) -0.008(2) -0.002(2) C2 0.034(2) 0.042(2) 0.041(2) 0.0007(16) -0.0041(16) -0.0025(17) C3 0.057(3) 0.049(2) 0.049(2) -0.013(2) -0.002(2) -0.004(2) C4 0.064(3) 0.036(2) 0.062(3) -0.004(2) -0.003(2) -0.003(2) C5 0.061(3) 0.036(2) 0.053(2) 0.0053(19) 0.000(2) -0.006(2) C6 0.042(2) 0.0395(19) 0.040(2) 0.0021(16) -0.0075(19) -0.0007(18) C7 0.044(2) 0.056(3) 0.043(2) 0.010(2) 0.0099(19) -0.003(2) C8 0.040(2) 0.043(2) 0.046(2) 0.0027(18) 0.0113(18) -0.0030(17) C9 0.049(3) 0.049(2) 0.064(3) 0.002(2) 0.020(2) 0.000(2) C10 0.0323(19) 0.054(3) 0.085(3) -0.006(3) 0.015(2) -0.0009(19) C11 0.033(2) 0.049(3) 0.075(3) -0.002(2) -0.005(2) -0.0001(18) C12 0.036(2) 0.039(2) 0.051(2) -0.0027(18) -0.0024(18) 0.0000(16) C13 0.045(2) 0.046(2) 0.044(2) 0.0117(19) -0.0134(18) -0.0018(19) C14 0.039(2) 0.0344(18) 0.048(2) 0.0044(18) -0.0088(18) -0.0030(16) C15 0.036(2) 0.039(2) 0.067(3) 0.0101(19) -0.018(2) -0.0024(17) C16 0.0320(19) 0.039(2) 0.077(3) 0.005(2) -0.013(2) -0.0002(16) C17 0.0323(19) 0.0382(19) 0.060(2) 0.004(2) -0.0010(18) 0.0002(17) C18 0.0336(18) 0.034(2) 0.048(2) 0.0053(18) -0.0014(16) -0.0008(15) C19 0.0259(17) 0.039(2) 0.041(2) -0.0055(16) 0.0025(14) -0.0012(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 1.854(2) . ? Co1 O2 1.867(3) . ? Co1 N3 1.918(3) . ? Co1 N4 1.921(3) . ? Co1 N2 1.939(3) . ? Co1 N1 1.956(3) . ? O1 C19 1.318(5) . ? O2 N5 1.407(4) . ? N1 C7 1.483(5) . ? N1 C1 1.490(6) . ? N1 C13 1.492(5) . ? N2 C2 1.332(5) . ? N2 C6 1.358(5) . ? N3 C8 1.337(5) . ? N3 C12 1.343(5) . ? N4 C18 1.326(5) . ? N4 C14 1.352(5) . ? N5 C19 1.292(5) . ? C1 C2 1.513(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.394(6) . ? C3 C4 1.370(7) . ? C3 H3 0.9500 . ? C4 C5 1.400(7) . ? C4 H4 0.9500 . ? C5 C6 1.380(6) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.492(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.373(6) . ? C9 C10 1.377(7) . ? C9 H9 0.9500 . ? C10 C11 1.395(8) . ? C10 H10 0.9500 . ? C11 C12 1.393(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.500(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.377(6) . ? C15 C16 1.385(7) . ? C15 H15 0.9500 . ? C16 C17 1.382(6) . ? C16 H16 0.9500 . ? C17 C18 1.390(5) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20A 1.502(4) . ? C19 C20B 1.504(5) . ? C20A C21A 1.551(9) . ? C20A H20A 0.9900 . ? C20A H20B 0.9900 . ? C20B C21B 1.39(3) . ? C20B H20C 0.9900 . ? C20B H20D 0.9900 . ? C21A C22A 1.3732 . ? C21A C30A 1.4162 . ? C22A C23A 1.4076 . ? C22A H22A 0.9500 . ? C23A C24A 1.3574 . ? C23A H23A 0.9500 . ? C24A C25A 1.4147 . ? C24A H24A 0.9500 . ? C25A C30A 1.4097 . ? C25A C26A 1.4098 . ? C26A C27A 1.3630 . ? C26A H26A 0.9500 . ? C27A C28A 1.3798 . ? C27A H27A 0.9500 . ? C28A C29A 1.3630 . ? C28A H28A 0.9500 . ? C29A C30A 1.4503 . ? C29A H29A 0.9500 . ? C21B C22B 1.3732 . ? C21B C30B 1.4378 . ? C22B C23B 1.4076 . ? C22B H22B 0.9500 . ? C23B C24B 1.3574 . ? C23B H23B 0.9500 . ? C24B C25B 1.4146 . ? C24B H24B 0.9500 . ? C25B C30B 1.3958 . ? C25B C26B 1.4099 . ? C26B C27B 1.3630 . ? C26B H26B 0.9500 . ? C27B C28B 1.3798 . ? C27B H27B 0.9500 . ? C28B C29B 1.3630 . ? C28B H28B 0.9500 . ? C29B C30B 1.4416 . ? C29B H29B 0.9500 . ? Cl1A O3A 1.4189 . ? Cl1A O4A 1.4222 . ? Cl1A O5A 1.4257 . ? Cl1A O6A 1.4293 . ? Cl1B O3B 1.4189 . ? Cl1B O4B 1.4222 . ? Cl1B O5B 1.4257 . ? Cl1B O6B 1.4293 . ? Cl1C O3C 1.4188 . ? Cl1C O4C 1.4223 . ? Cl1C O5C 1.4257 . ? Cl1C O6C 1.4293 . ? O7A C31 1.136(15) . ? O7A H7OA 0.8400 . ? C31 C32 1.508(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O2 86.41(12) . . ? O1 Co1 N3 94.13(13) . . ? O2 Co1 N3 89.04(14) . . ? O1 Co1 N4 95.55(13) . . ? O2 Co1 N4 89.09(13) . . ? N3 Co1 N4 170.00(14) . . ? O1 Co1 N2 93.99(13) . . ? O2 Co1 N2 179.37(14) . . ? N3 Co1 N2 91.42(14) . . ? N4 Co1 N2 90.38(14) . . ? O1 Co1 N1 178.61(14) . . ? O2 Co1 N1 92.79(13) . . ? N3 Co1 N1 84.72(15) . . ? N4 Co1 N1 85.56(15) . . ? N2 Co1 N1 86.83(14) . . ? C19 O1 Co1 108.7(2) . . ? N5 O2 Co1 109.4(2) . . ? C7 N1 C1 111.2(4) . . ? C7 N1 C13 113.1(3) . . ? C1 N1 C13 111.9(4) . . ? C7 N1 Co1 104.9(3) . . ? C1 N1 Co1 109.7(2) . . ? C13 N1 Co1 105.6(3) . . ? C2 N2 C6 119.7(3) . . ? C2 N2 Co1 114.8(3) . . ? C6 N2 Co1 125.5(3) . . ? C8 N3 C12 119.5(4) . . ? C8 N3 Co1 113.6(3) . . ? C12 N3 Co1 126.9(3) . . ? C18 N4 C14 120.1(3) . . ? C18 N4 Co1 126.6(3) . . ? C14 N4 Co1 113.3(3) . . ? C19 N5 O2 113.0(3) . . ? N1 C1 C2 112.8(3) . . ? N1 C1 H1A 109.0 . . ? C2 C1 H1A 109.0 . . ? N1 C1 H1B 109.0 . . ? C2 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? N2 C2 C3 122.4(4) . . ? N2 C2 C1 115.7(4) . . ? C3 C2 C1 121.8(4) . . ? C4 C3 C2 117.9(4) . . ? C4 C3 H3 121.0 . . ? C2 C3 H3 121.0 . . ? C3 C4 C5 120.2(4) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 118.7(4) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? N2 C6 C5 121.0(4) . . ? N2 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? N1 C7 C8 109.1(4) . . ? N1 C7 H7A 109.9 . . ? C8 C7 H7A 109.9 . . ? N1 C7 H7B 109.9 . . ? C8 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? N3 C8 C9 122.0(4) . . ? N3 C8 C7 113.9(4) . . ? C9 C8 C7 124.0(4) . . ? C8 C9 C10 119.4(5) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C9 C10 C11 119.3(4) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C12 C11 C10 118.1(4) . . ? C12 C11 H11 121.0 . . ? C10 C11 H11 121.0 . . ? N3 C12 C11 121.7(4) . . ? N3 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? N1 C13 C14 109.1(3) . . ? N1 C13 H13A 109.9 . . ? C14 C13 H13A 109.9 . . ? N1 C13 H13B 109.9 . . ? C14 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? N4 C14 C15 121.1(4) . . ? N4 C14 C13 114.3(3) . . ? C15 C14 C13 124.5(4) . . ? C14 C15 C16 118.7(4) . . ? C14 C15 H15 120.6 . . ? C16 C15 H15 120.6 . . ? C17 C16 C15 120.0(4) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 118.1(4) . . ? C16 C17 H17 121.0 . . ? C18 C17 H17 121.0 . . ? N4 C18 C17 121.9(4) . . ? N4 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? N5 C19 O1 122.1(3) . . ? N5 C19 C20A 119.3(5) . . ? O1 C19 C20A 118.6(5) . . ? N5 C19 C20B 124.8(13) . . ? O1 C19 C20B 112.9(12) . . ? C19 C20A C21A 109.1(6) . . ? C19 C20A H20A 109.9 . . ? C21A C20A H20A 109.9 . . ? C19 C20A H20B 109.9 . . ? C21A C20A H20B 109.9 . . ? H20A C20A H20B 108.3 . . ? C21B C20B C19 119.0(17) . . ? C21B C20B H20C 107.6 . . ? C19 C20B H20C 107.6 . . ? C21B C20B H20D 107.6 . . ? C19 C20B H20D 107.6 . . ? H20C C20B H20D 107.0 . . ? C22A C21A C30A 117.8 . . ? C22A C21A C20A 117.4(4) . . ? C30A C21A C20A 124.8(4) . . ? C21A C22A C23A 121.6 . . ? C21A C22A H22A 119.2 . . ? C23A C22A H22A 119.2 . . ? C24A C23A C22A 120.2 . . ? C24A C23A H23A 119.9 . . ? C22A C23A H23A 119.9 . . ? C23A C24A C25A 121.0 . . ? C23A C24A H24A 119.5 . . ? C25A C24A H24A 119.5 . . ? C30A C25A C26A 120.1 . . ? C30A C25A C24A 117.8 . . ? C26A C25A C24A 122.1 . . ? C27A C26A C25A 120.5 . . ? C27A C26A H26A 119.8 . . ? C25A C26A H26A 119.8 . . ? C26A C27A C28A 120.8 . . ? C26A C27A H27A 119.6 . . ? C28A C27A H27A 119.6 . . ? C29A C28A C27A 121.0 . . ? C29A C28A H28A 119.5 . . ? C27A C28A H28A 119.5 . . ? C28A C29A C30A 120.4 . . ? C28A C29A H29A 119.8 . . ? C30A C29A H29A 119.8 . . ? C25A C30A C21A 121.5 . . ? C25A C30A C29A 117.1 . . ? C21A C30A C29A 121.2 . . ? C22B C21B C20B 125.3(14) . . ? C22B C21B C30B 117.7 . . ? C20B C21B C30B 116.0(14) . . ? C21B C22B C23B 121.6 . . ? C21B C22B H22B 119.2 . . ? C23B C22B H22B 119.2 . . ? C24B C23B C22B 120.2 . . ? C24B C23B H23B 119.9 . . ? C22B C23B H23B 119.9 . . ? C23B C24B C25B 121.0 . . ? C23B C24B H24B 119.5 . . ? C25B C24B H24B 119.5 . . ? C30B C25B C26B 119.4 . . ? C30B C25B C24B 118.5 . . ? C26B C25B C24B 122.1 . . ? C27B C26B C25B 120.5 . . ? C27B C26B H26B 119.8 . . ? C25B C26B H26B 119.8 . . ? C26B C27B C28B 120.8 . . ? C26B C27B H27B 119.6 . . ? C28B C27B H27B 119.6 . . ? C29B C28B C27B 121.0 . . ? C29B C28B H28B 119.5 . . ? C27B C28B H28B 119.5 . . ? C28B C29B C30B 119.6 . . ? C28B C29B H29B 120.2 . . ? C30B C29B H29B 120.2 . . ? C25B C30B C21B 121.0 . . ? C25B C30B C29B 118.6 . . ? C21B C30B C29B 120.3 . . ? O3A Cl1A O4A 110.3 . . ? O3A Cl1A O5A 108.6 . . ? O4A Cl1A O5A 110.6 . . ? O3A Cl1A O6A 108.3 . . ? O4A Cl1A O6A 110.5 . . ? O5A Cl1A O6A 108.5 . . ? O3B Cl1B O4B 110.3 . . ? O3B Cl1B O5B 108.6 . . ? O4B Cl1B O5B 110.6 . . ? O3B Cl1B O6B 108.3 . . ? O4B Cl1B O6B 110.5 . . ? O5B Cl1B O6B 108.5 . . ? O3C Cl1C O4C 110.3 . . ? O3C Cl1C O5C 108.6 . . ? O4C Cl1C O5C 110.5 . . ? O3C Cl1C O6C 108.3 . . ? O4C Cl1C O6C 110.5 . . ? O5C Cl1C O6C 108.5 . . ? O7A C31 C32 113.3(15) . . ? O7A C31 H31A 108.9 . . ? C32 C31 H31A 108.9 . . ? O7A C31 H31B 108.9 . . ? C32 C31 H31B 108.9 . . ? H31A C31 H31B 107.7 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? 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 O2 Co1 O1 C19 -5.7(2) . . . . ? N3 Co1 O1 C19 83.1(2) . . . . ? N4 Co1 O1 C19 -94.5(2) . . . . ? N2 Co1 O1 C19 174.8(2) . . . . ? O1 Co1 O2 N5 5.8(2) . . . . ? N3 Co1 O2 N5 -88.4(2) . . . . ? N4 Co1 O2 N5 101.4(2) . . . . ? N1 Co1 O2 N5 -173.0(2) . . . . ? O2 Co1 N1 C7 58.7(3) . . . . ? N3 Co1 N1 C7 -30.0(3) . . . . ? N4 Co1 N1 C7 147.6(3) . . . . ? N2 Co1 N1 C7 -121.8(3) . . . . ? O2 Co1 N1 C1 178.2(3) . . . . ? N3 Co1 N1 C1 89.4(3) . . . . ? N4 Co1 N1 C1 -92.9(3) . . . . ? N2 Co1 N1 C1 -2.3(3) . . . . ? O2 Co1 N1 C13 -61.0(3) . . . . ? N3 Co1 N1 C13 -149.8(3) . . . . ? N4 Co1 N1 C13 27.9(3) . . . . ? N2 Co1 N1 C13 118.5(3) . . . . ? O1 Co1 N2 C2 -178.6(3) . . . . ? N3 Co1 N2 C2 -84.4(3) . . . . ? N4 Co1 N2 C2 85.8(3) . . . . ? N1 Co1 N2 C2 0.2(3) . . . . ? O1 Co1 N2 C6 2.7(3) . . . . ? N3 Co1 N2 C6 96.9(3) . . . . ? N4 Co1 N2 C6 -92.9(3) . . . . ? N1 Co1 N2 C6 -178.5(4) . . . . ? O1 Co1 N3 C8 -163.5(3) . . . . ? O2 Co1 N3 C8 -77.2(3) . . . . ? N4 Co1 N3 C8 2.1(10) . . . . ? N2 Co1 N3 C8 102.4(3) . . . . ? N1 Co1 N3 C8 15.7(3) . . . . ? O1 Co1 N3 C12 17.0(4) . . . . ? O2 Co1 N3 C12 103.3(4) . . . . ? N4 Co1 N3 C12 -177.4(7) . . . . ? N2 Co1 N3 C12 -77.1(4) . . . . ? N1 Co1 N3 C12 -163.8(4) . . . . ? O1 Co1 N4 C18 -16.4(3) . . . . ? O2 Co1 N4 C18 -102.7(3) . . . . ? N3 Co1 N4 C18 178.0(7) . . . . ? N2 Co1 N4 C18 77.7(3) . . . . ? N1 Co1 N4 C18 164.4(4) . . . . ? O1 Co1 N4 C14 165.8(3) . . . . ? O2 Co1 N4 C14 79.5(3) . . . . ? N3 Co1 N4 C14 0.2(10) . . . . ? N2 Co1 N4 C14 -100.2(3) . . . . ? N1 Co1 N4 C14 -13.4(3) . . . . ? Co1 O2 N5 C19 -4.8(4) . . . . ? C7 N1 C1 C2 119.3(4) . . . . ? C13 N1 C1 C2 -113.1(4) . . . . ? Co1 N1 C1 C2 3.8(5) . . . . ? C6 N2 C2 C3 -1.8(7) . . . . ? Co1 N2 C2 C3 179.4(3) . . . . ? C6 N2 C2 C1 -179.3(4) . . . . ? Co1 N2 C2 C1 1.9(5) . . . . ? N1 C1 C2 N2 -3.8(6) . . . . ? N1 C1 C2 C3 178.7(4) . . . . ? N2 C2 C3 C4 1.9(7) . . . . ? C1 C2 C3 C4 179.2(5) . . . . ? C2 C3 C4 C5 -1.0(8) . . . . ? C3 C4 C5 C6 0.0(8) . . . . ? C2 N2 C6 C5 0.8(6) . . . . ? Co1 N2 C6 C5 179.4(3) . . . . ? C4 C5 C6 N2 0.1(7) . . . . ? C1 N1 C7 C8 -79.8(4) . . . . ? C13 N1 C7 C8 153.4(4) . . . . ? Co1 N1 C7 C8 38.7(4) . . . . ? C12 N3 C8 C9 -0.2(7) . . . . ? Co1 N3 C8 C9 -179.7(4) . . . . ? C12 N3 C8 C7 -176.6(4) . . . . ? Co1 N3 C8 C7 3.8(5) . . . . ? N1 C7 C8 N3 -29.2(5) . . . . ? N1 C7 C8 C9 154.5(4) . . . . ? N3 C8 C9 C10 -1.3(7) . . . . ? C7 C8 C9 C10 174.8(5) . . . . ? C8 C9 C10 C11 1.1(7) . . . . ? C9 C10 C11 C12 0.4(7) . . . . ? C8 N3 C12 C11 1.8(7) . . . . ? Co1 N3 C12 C11 -178.7(3) . . . . ? C10 C11 C12 N3 -1.9(7) . . . . ? C7 N1 C13 C14 -150.8(4) . . . . ? C1 N1 C13 C14 82.7(4) . . . . ? Co1 N1 C13 C14 -36.6(4) . . . . ? C18 N4 C14 C15 -1.5(6) . . . . ? Co1 N4 C14 C15 176.5(3) . . . . ? C18 N4 C14 C13 176.5(4) . . . . ? Co1 N4 C14 C13 -5.5(4) . . . . ? N1 C13 C14 N4 28.7(5) . . . . ? N1 C13 C14 C15 -153.4(4) . . . . ? N4 C14 C15 C16 1.7(6) . . . . ? C13 C14 C15 C16 -176.1(4) . . . . ? C14 C15 C16 C17 -0.7(7) . . . . ? C15 C16 C17 C18 -0.4(7) . . . . ? C14 N4 C18 C17 0.3(6) . . . . ? Co1 N4 C18 C17 -177.4(3) . . . . ? C16 C17 C18 N4 0.6(6) . . . . ? O2 N5 C19 O1 0.1(5) . . . . ? O2 N5 C19 C20A 177.6(5) . . . . ? O2 N5 C19 C20B 174.2(13) . . . . ? Co1 O1 C19 N5 4.7(4) . . . . ? Co1 O1 C19 C20A -172.9(5) . . . . ? Co1 O1 C19 C20B -170.1(12) . . . . ? N5 C19 C20A C21A -112.3(6) . . . . ? O1 C19 C20A C21A 65.3(8) . . . . ? C20B C19 C20A C21A 40(13) . . . . ? N5 C19 C20B C21B -89(2) . . . . ? O1 C19 C20B C21B 85(2) . . . . ? C20A C19 C20B C21B -118(15) . . . . ? C19 C20A C21A C22A 99.3(6) . . . . ? C19 C20A C21A C30A -82.6(7) . . . . ? C30A C21A C22A C23A -1.3 . . . . ? C20A C21A C22A C23A 177.0(4) . . . . ? C21A C22A C23A C24A 0.5 . . . . ? C22A C23A C24A C25A -1.1 . . . . ? C23A C24A C25A C30A 2.3 . . . . ? C23A C24A C25A C26A -178.8 . . . . ? C30A C25A C26A C27A -2.4 . . . . ? C24A C25A C26A C27A 178.7 . . . . ? C25A C26A C27A C28A 2.1 . . . . ? C26A C27A C28A C29A -2.2 . . . . ? C27A C28A C29A C30A 2.5 . . . . ? C26A C25A C30A C21A 178.0 . . . . ? C24A C25A C30A C21A -3.1 . . . . ? C26A C25A C30A C29A 2.6 . . . . ? C24A C25A C30A C29A -178.4 . . . . ? C22A C21A C30A C25A 2.6 . . . . ? C20A C21A C30A C25A -175.5(4) . . . . ? C22A C21A C30A C29A 177.7 . . . . ? C20A C21A C30A C29A -0.3(4) . . . . ? C28A C29A C30A C25A -2.7 . . . . ? C28A C29A C30A C21A -178.1 . . . . ? C19 C20B C21B C22B 87(2) . . . . ? C19 C20B C21B C30B -82(2) . . . . ? C20B C21B C22B C23B -169.1(11) . . . . ? C30B C21B C22B C23B -1.1 . . . . ? C21B C22B C23B C24B 0.5 . . . . ? C22B C23B C24B C25B -1.1 . . . . ? C23B C24B C25B C30B 2.2 . . . . ? C23B C24B C25B C26B -178.8 . . . . ? C30B C25B C26B C27B -2.3 . . . . ? C24B C25B C26B C27B 178.7 . . . . ? C25B C26B C27B C28B 2.1 . . . . ? C26B C27B C28B C29B -2.2 . . . . ? C27B C28B C29B C30B 2.4 . . . . ? C26B C25B C30B C21B 178.2 . . . . ? C24B C25B C30B C21B -2.8 . . . . ? C26B C25B C30B C29B 2.5 . . . . ? C24B C25B C30B C29B -178.5 . . . . ? C22B C21B C30B C25B 2.3 . . . . ? C20B C21B C30B C25B 171.4(10) . . . . ? C22B C21B C30B C29B 177.9 . . . . ? C20B C21B C30B C29B -12.9(10) . . . . ? C28B C29B C30B C25B -2.5 . . . . ? C28B C29B C30B C21B -178.3 . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.980 _refine_diff_density_min -0.557 _refine_diff_density_rms 0.105 data_9 _database_code_depnum_ccdc_archive 'CCDC 866273' #TrackingRef '- combined revised cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H27 Co N4 O2, 2(Cl O4)' _chemical_formula_sum 'C28 H27 Cl2 Co N4 O10' _chemical_formula_weight 709.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' _Int_tables_symmetry_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.011(2) _cell_length_b 18.474(3) _cell_length_c 13.884(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.166(6) _cell_angle_gamma 90.00 _cell_volume 2958.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 3471 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 23.99 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 0.826 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6793 _exptl_absorpt_correction_T_max 0.7458 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2007)' _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 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type APEXII-FR591 _diffrn_measurement_method \w+\f _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 26163 _diffrn_reflns_av_R_equivalents 0.0711 _diffrn_reflns_av_sigmaI/netI 0.0819 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 28.72 _reflns_number_total 7646 _reflns_number_gt 5192 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX (Bruker-Nonius, 2003)' _computing_cell_refinement 'SAINT (Bruker-Nonius, 2003)' _computing_data_reduction 'SAINT (Bruker-Nonius, 2003), XPREP (Bruker-Nonius, 2003)' _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) POV-Ray 3.5 (Cason, 2002) WebLab ViewerPro 3.7 (Molecular Simulations, 2000) ; _computing_publication_material 'enCIFer 1.1 (CCDC, 2005)' _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^)+(0.0708P)^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 7646 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0887 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1453 _refine_ls_wR_factor_gt 0.1227 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 -0.0008(3) 0.30589(17) 0.4733(2) 0.0290(8) Uani 1 1 d . . . H1A H 0.0510 0.3455 0.4670 0.044 Uiso 1 1 calc R . . H1B H 0.0200 0.2889 0.5429 0.044 Uiso 1 1 calc R . . H1C H -0.0811 0.3232 0.4542 0.044 Uiso 1 1 calc R . . C2 C 0.0109(3) 0.24488(17) 0.4060(2) 0.0199(6) Uani 1 1 d . . . C3 C 0.0594(3) 0.17983(17) 0.4454(2) 0.0218(7) Uani 1 1 d . . . H3 H 0.0854 0.1754 0.5163 0.026 Uiso 1 1 calc R . . C4 C 0.0727(3) 0.12025(16) 0.3880(2) 0.0176(6) Uani 1 1 d . . . C5 C 0.1280(3) 0.05276(17) 0.4378(2) 0.0201(7) Uani 1 1 d . . . C6 C 0.1821(3) 0.00671(16) 0.3861(2) 0.0228(7) Uani 1 1 d . . . H6 H 0.1796 0.0172 0.3186 0.027 Uiso 1 1 calc R . . C7 C 0.2399(3) -0.05461(17) 0.4322(2) 0.0283(8) Uani 1 1 d . . . H7 H 0.2799 -0.0846 0.3973 0.034 Uiso 1 1 calc R . . C8 C 0.2392(3) -0.07215(18) 0.5299(3) 0.0325(8) Uani 1 1 d . . . H8 H 0.2778 -0.1144 0.5613 0.039 Uiso 1 1 calc R . . C9 C 0.1820(3) -0.02750(18) 0.5807(2) 0.0292(8) Uani 1 1 d . . . H9 H 0.1798 -0.0400 0.6465 0.035 Uiso 1 1 calc R . . C10 C 0.1278(3) 0.03537(18) 0.5362(2) 0.0255(7) Uani 1 1 d . . . H10 H 0.0908 0.0665 0.5722 0.031 Uiso 1 1 calc R . . C11 C -0.1932(3) 0.09340(15) 0.1426(2) 0.0181(6) Uani 1 1 d . . . C12 C -0.2950(3) 0.05506(16) 0.1324(2) 0.0226(7) Uani 1 1 d . . . H12 H -0.3086 0.0113 0.0950 0.027 Uiso 1 1 calc R . . C13 C -0.3771(3) 0.08116(17) 0.1772(2) 0.0260(7) Uani 1 1 d . . . H13 H -0.4461 0.0546 0.1726 0.031 Uiso 1 1 calc R . . C14 C -0.3574(3) 0.14608(16) 0.2285(2) 0.0214(7) Uani 1 1 d . . . H14 H -0.4134 0.1654 0.2581 0.026 Uiso 1 1 calc R . . C15 C -0.2547(3) 0.18251(16) 0.2360(2) 0.0193(6) Uani 1 1 d . . . H15 H -0.2408 0.2273 0.2710 0.023 Uiso 1 1 calc R . . C16 C -0.0968(3) 0.06975(15) 0.1014(2) 0.0187(6) Uani 1 1 d . . . H16A H -0.1286 0.0467 0.0350 0.022 Uiso 1 1 calc R . . H16B H -0.0471 0.0341 0.1470 0.022 Uiso 1 1 calc R . . C17 C -0.0832(2) 0.25604(15) 0.0164(2) 0.0163(6) Uani 1 1 d . . . C18 C -0.0883(3) 0.30841(15) -0.0557(2) 0.0198(6) Uani 1 1 d . . . H18 H -0.0902 0.2949 -0.1221 0.024 Uiso 1 1 calc R . . C19 C -0.0905(3) 0.38063(17) -0.0305(2) 0.0237(7) Uani 1 1 d . . . H19 H -0.0932 0.4173 -0.0790 0.028 Uiso 1 1 calc R . . C20 C -0.0888(3) 0.39880(16) 0.0669(2) 0.0233(7) Uani 1 1 d . . . H20 H -0.0930 0.4481 0.0851 0.028 Uiso 1 1 calc R . . C21 C -0.0810(3) 0.34474(15) 0.1370(2) 0.0215(7) Uani 1 1 d . . . H21 H -0.0777 0.3573 0.2041 0.026 Uiso 1 1 calc R . . C22 C -0.0879(3) 0.17600(15) -0.0028(2) 0.0181(6) Uani 1 1 d . . . H22A H -0.0500 0.1648 -0.0559 0.022 Uiso 1 1 calc R . . H22B H -0.1697 0.1601 -0.0264 0.022 Uiso 1 1 calc R . . C23 C 0.1697(3) 0.18216(15) 0.1373(2) 0.0179(6) Uani 1 1 d . . . C24 C 0.2725(3) 0.19820(16) 0.1150(2) 0.0239(7) Uani 1 1 d . . . H24 H 0.2991 0.1687 0.0699 0.029 Uiso 1 1 calc R . . C25 C 0.3357(3) 0.25787(17) 0.1596(2) 0.0245(7) Uani 1 1 d . . . H25 H 0.4068 0.2695 0.1459 0.029 Uiso 1 1 calc R . . C26 C 0.2945(3) 0.30073(16) 0.2247(2) 0.0214(7) Uani 1 1 d . . . H26 H 0.3370 0.3419 0.2558 0.026 Uiso 1 1 calc R . . C27 C 0.1912(3) 0.28266(15) 0.2436(2) 0.0182(6) Uani 1 1 d . . . H27 H 0.1625 0.3120 0.2876 0.022 Uiso 1 1 calc R . . C28 C 0.0949(3) 0.11774(15) 0.0961(2) 0.0171(6) Uani 1 1 d . . . H28A H 0.1008 0.1060 0.0281 0.021 Uiso 1 1 calc R . . H28B H 0.1209 0.0751 0.1398 0.021 Uiso 1 1 calc R . . N4 N -0.1741(2) 0.15631(12) 0.19509(18) 0.0170(5) Uani 1 1 d . . . N2 N -0.0780(2) 0.27419(12) 0.11207(18) 0.0164(5) Uani 1 1 d . . . N3 N 0.1299(2) 0.22388(13) 0.20048(17) 0.0162(5) Uani 1 1 d . . . N1 N -0.0274(2) 0.13578(12) 0.09178(17) 0.0154(5) Uani 1 1 d . . . O1 O -0.02563(18) 0.25989(11) 0.31167(15) 0.0190(5) Uani 1 1 d . . . O2 O 0.04229(18) 0.11847(11) 0.29135(14) 0.0184(5) Uani 1 1 d . . . O3 O 0.3230(2) 0.03030(12) 0.07913(18) 0.0346(6) Uani 1 1 d . . . O4 O 0.4137(3) -0.07174(16) 0.1620(3) 0.0765(12) Uani 1 1 d . . . O5 O 0.3737(3) 0.0265(2) 0.2515(2) 0.0756(12) Uani 1 1 d . . . O6 O 0.2219(2) -0.04558(12) 0.16110(18) 0.0309(6) Uani 1 1 d . . . O7 O 0.1030(3) 0.21336(12) -0.13639(19) 0.0401(7) Uani 1 1 d . . . O8 O 0.0446(2) 0.09342(12) -0.1712(2) 0.0412(7) Uani 1 1 d . . . O9 O 0.2381(3) 0.12653(18) -0.1540(3) 0.0662(10) Uani 1 1 d . . . O10 O 0.0923(2) 0.16471(13) -0.29385(18) 0.0374(6) Uani 1 1 d . . . Cl1 Cl 0.33318(6) -0.01614(4) 0.16418(5) 0.02068(18) Uani 1 1 d . . . Cl2 Cl 0.12077(7) 0.14849(4) -0.18888(6) 0.02157(18) Uani 1 1 d . . . Co1 Co -0.02271(3) 0.19665(2) 0.20708(3) 0.01465(12) 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 0.038(2) 0.0302(18) 0.0198(17) -0.0082(14) 0.0099(15) -0.0011(15) C2 0.0182(15) 0.0293(17) 0.0144(15) -0.0046(13) 0.0079(12) -0.0074(13) C3 0.0266(18) 0.0279(17) 0.0115(14) -0.0018(12) 0.0062(13) -0.0009(14) C4 0.0154(15) 0.0257(16) 0.0120(14) 0.0045(12) 0.0044(11) -0.0014(12) C5 0.0196(16) 0.0264(17) 0.0132(14) 0.0025(12) 0.0027(12) -0.0009(13) C6 0.0329(19) 0.0224(16) 0.0114(15) -0.0011(12) 0.0032(13) -0.0030(14) C7 0.039(2) 0.0229(17) 0.0216(17) -0.0017(14) 0.0071(15) 0.0046(15) C8 0.042(2) 0.0265(18) 0.0254(19) 0.0061(15) 0.0033(16) 0.0058(16) C9 0.035(2) 0.0351(19) 0.0157(16) 0.0120(14) 0.0042(14) -0.0015(16) C10 0.0250(18) 0.0359(19) 0.0168(16) 0.0046(14) 0.0080(13) 0.0034(15) C11 0.0238(16) 0.0163(14) 0.0132(14) 0.0042(11) 0.0035(12) -0.0004(12) C12 0.0283(18) 0.0182(15) 0.0201(16) 0.0034(12) 0.0048(13) -0.0037(13) C13 0.0247(18) 0.0300(18) 0.0219(17) 0.0093(14) 0.0043(14) -0.0043(14) C14 0.0207(16) 0.0237(16) 0.0191(16) 0.0075(13) 0.0045(13) 0.0046(13) C15 0.0184(16) 0.0220(16) 0.0167(15) 0.0011(12) 0.0036(12) 0.0030(12) C16 0.0283(17) 0.0118(14) 0.0164(15) -0.0017(11) 0.0072(13) -0.0029(12) C17 0.0153(15) 0.0163(15) 0.0173(15) 0.0013(11) 0.0046(12) 0.0006(11) C18 0.0199(16) 0.0227(16) 0.0159(15) 0.0013(12) 0.0034(12) -0.0007(13) C19 0.0250(17) 0.0193(16) 0.0258(17) 0.0066(13) 0.0052(14) 0.0033(13) C20 0.0288(18) 0.0133(15) 0.0263(17) -0.0008(13) 0.0053(14) 0.0019(13) C21 0.0267(17) 0.0175(15) 0.0196(16) -0.0031(12) 0.0050(13) 0.0021(13) C22 0.0263(17) 0.0175(15) 0.0095(13) 0.0003(11) 0.0032(12) -0.0004(12) C23 0.0217(16) 0.0174(15) 0.0141(14) 0.0022(11) 0.0041(12) 0.0022(12) C24 0.0270(18) 0.0221(16) 0.0262(17) -0.0034(13) 0.0132(14) 0.0021(14) C25 0.0209(17) 0.0266(17) 0.0280(18) 0.0032(14) 0.0099(14) 0.0000(13) C26 0.0233(17) 0.0196(15) 0.0211(16) 0.0031(13) 0.0059(13) -0.0007(13) C27 0.0231(16) 0.0180(15) 0.0134(14) 0.0013(11) 0.0051(12) 0.0012(12) C28 0.0204(16) 0.0153(14) 0.0170(15) -0.0034(12) 0.0075(12) 0.0018(12) N4 0.0229(14) 0.0151(12) 0.0129(12) 0.0016(10) 0.0050(10) 0.0009(10) N2 0.0187(13) 0.0140(12) 0.0160(13) -0.0006(10) 0.0040(10) 0.0001(10) N3 0.0205(13) 0.0170(12) 0.0105(12) 0.0009(10) 0.0032(10) 0.0004(10) N1 0.0200(13) 0.0153(12) 0.0106(12) 0.0011(9) 0.0039(10) -0.0013(10) O1 0.0214(11) 0.0210(11) 0.0151(11) -0.0036(9) 0.0060(9) -0.0009(9) O2 0.0248(12) 0.0181(11) 0.0121(10) 0.0019(8) 0.0045(9) -0.0003(9) O3 0.0380(15) 0.0333(14) 0.0319(14) 0.0136(11) 0.0089(12) 0.0001(12) O4 0.088(3) 0.0506(19) 0.122(3) 0.048(2) 0.080(2) 0.0482(18) O5 0.062(2) 0.140(3) 0.0336(17) -0.0444(19) 0.0276(16) -0.062(2) O6 0.0292(14) 0.0260(12) 0.0356(14) 0.0011(11) 0.0059(11) -0.0111(10) O7 0.066(2) 0.0272(13) 0.0363(15) -0.0071(11) 0.0301(14) -0.0092(13) O8 0.0581(19) 0.0222(13) 0.0501(17) -0.0003(12) 0.0265(14) -0.0105(12) O9 0.0364(18) 0.071(2) 0.081(2) 0.0081(19) -0.0002(16) 0.0198(16) O10 0.0531(18) 0.0377(14) 0.0217(13) 0.0007(11) 0.0110(12) 0.0003(13) Cl1 0.0211(4) 0.0224(4) 0.0195(4) 0.0013(3) 0.0071(3) 0.0043(3) Cl2 0.0244(4) 0.0203(4) 0.0206(4) 0.0028(3) 0.0072(3) 0.0016(3) Co1 0.0184(2) 0.0145(2) 0.0112(2) -0.00053(15) 0.00430(15) 0.00023(16) _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 1.496(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 O1 1.290(3) . ? C2 C3 1.380(4) . ? C3 C4 1.394(4) . ? C3 H3 0.9500 . ? C4 O2 1.289(3) . ? C4 C5 1.489(4) . ? C5 C6 1.386(4) . ? C5 C10 1.404(4) . ? C6 C7 1.388(4) . ? C6 H6 0.9500 . ? C7 C8 1.397(5) . ? C7 H7 0.9500 . ? C8 C9 1.386(5) . ? C8 H8 0.9500 . ? C9 C10 1.389(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 N4 1.357(4) . ? C11 C12 1.386(4) . ? C11 C16 1.492(4) . ? C12 C13 1.391(4) . ? C12 H12 0.9500 . ? C13 C14 1.381(4) . ? C13 H13 0.9500 . ? C14 C15 1.384(4) . ? C14 H14 0.9500 . ? C15 N4 1.342(4) . ? C15 H15 0.9500 . ? C16 N1 1.505(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 N2 1.354(4) . ? C17 C18 1.382(4) . ? C17 C22 1.501(4) . ? C18 C19 1.382(4) . ? C18 H18 0.9500 . ? C19 C20 1.387(4) . ? C19 H19 0.9500 . ? C20 C21 1.380(4) . ? C20 H20 0.9500 . ? C21 N2 1.352(4) . ? C21 H21 0.9500 . ? C22 N1 1.507(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 N3 1.350(4) . ? C23 C24 1.386(4) . ? C23 C28 1.505(4) . ? C24 C25 1.383(4) . ? C24 H24 0.9500 . ? C25 C26 1.392(4) . ? C25 H25 0.9500 . ? C26 C27 1.378(4) . ? C26 H26 0.9500 . ? C27 N3 1.354(4) . ? C27 H27 0.9500 . ? C28 N1 1.491(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? N4 Co1 1.929(3) . ? N2 Co1 1.935(2) . ? N3 Co1 1.928(3) . ? N1 Co1 1.944(2) . ? O1 Co1 1.872(2) . ? O2 Co1 1.886(2) . ? O3 Cl1 1.437(2) . ? O4 Cl1 1.417(3) . ? O5 Cl1 1.414(3) . ? O6 Cl1 1.433(2) . ? O7 Cl2 1.449(2) . ? O8 Cl2 1.434(2) . ? O9 Cl2 1.415(3) . ? O10 Cl2 1.433(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag 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 125.2(3) . . ? O1 C2 C1 114.1(3) . . ? C3 C2 C1 120.7(3) . . ? C2 C3 C4 124.3(3) . . ? C2 C3 H3 117.9 . . ? C4 C3 H3 117.9 . . ? O2 C4 C3 124.8(3) . . ? O2 C4 C5 115.0(3) . . ? C3 C4 C5 120.2(3) . . ? C6 C5 C10 119.4(3) . . ? C6 C5 C4 119.1(3) . . ? C10 C5 C4 121.5(3) . . ? C5 C6 C7 120.6(3) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C6 C7 C8 120.0(3) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C9 C8 C7 119.6(3) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 120.6(3) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C9 C10 C5 119.8(3) . . ? C9 C10 H10 120.1 . . ? C5 C10 H10 120.1 . . ? N4 C11 C12 120.4(3) . . ? N4 C11 C16 115.1(3) . . ? C12 C11 C16 124.6(3) . . ? C11 C12 C13 119.5(3) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C14 C13 C12 119.4(3) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 118.8(3) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? N4 C15 C14 121.7(3) . . ? N4 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C11 C16 N1 107.8(2) . . ? C11 C16 H16A 110.2 . . ? N1 C16 H16A 110.2 . . ? C11 C16 H16B 110.2 . . ? N1 C16 H16B 110.2 . . ? H16A C16 H16B 108.5 . . ? N2 C17 C18 121.2(3) . . ? N2 C17 C22 114.0(2) . . ? C18 C17 C22 124.7(3) . . ? C19 C18 C17 119.5(3) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 119.0(3) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C21 C20 C19 119.5(3) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? N2 C21 C20 121.2(3) . . ? N2 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C17 C22 N1 110.2(2) . . ? C17 C22 H22A 109.6 . . ? N1 C22 H22A 109.6 . . ? C17 C22 H22B 109.6 . . ? N1 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? N3 C23 C24 121.4(3) . . ? N3 C23 C28 114.6(3) . . ? C24 C23 C28 124.0(3) . . ? C25 C24 C23 118.8(3) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? C24 C25 C26 119.6(3) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C27 C26 C25 119.2(3) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? N3 C27 C26 121.1(3) . . ? N3 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? N1 C28 C23 108.4(2) . . ? N1 C28 H28A 110.0 . . ? C23 C28 H28A 110.0 . . ? N1 C28 H28B 110.0 . . ? C23 C28 H28B 110.0 . . ? H28A C28 H28B 108.4 . . ? C15 N4 C11 120.1(3) . . ? C15 N4 Co1 126.7(2) . . ? C11 N4 Co1 113.1(2) . . ? C21 N2 C17 119.5(3) . . ? C21 N2 Co1 124.6(2) . . ? C17 N2 Co1 113.50(19) . . ? C23 N3 C27 119.9(3) . . ? C23 N3 Co1 113.2(2) . . ? C27 N3 Co1 126.5(2) . . ? C28 N1 C16 112.3(2) . . ? C28 N1 C22 112.1(2) . . ? C16 N1 C22 109.4(2) . . ? C28 N1 Co1 107.09(17) . . ? C16 N1 Co1 106.58(17) . . ? C22 N1 Co1 109.17(17) . . ? C2 O1 Co1 125.36(19) . . ? C4 O2 Co1 125.1(2) . . ? O5 Cl1 O4 110.4(2) . . ? O5 Cl1 O6 109.43(16) . . ? O4 Cl1 O6 111.17(18) . . ? O5 Cl1 O3 107.57(19) . . ? O4 Cl1 O3 108.49(17) . . ? O6 Cl1 O3 109.70(14) . . ? O9 Cl2 O10 109.92(18) . . ? O9 Cl2 O8 111.08(19) . . ? O10 Cl2 O8 109.86(16) . . ? O9 Cl2 O7 109.68(19) . . ? O10 Cl2 O7 108.17(15) . . ? O8 Cl2 O7 108.08(15) . . ? O1 Co1 O2 95.21(9) . . ? O1 Co1 N3 95.60(10) . . ? O2 Co1 N3 89.68(10) . . ? O1 Co1 N4 95.01(10) . . ? O2 Co1 N4 88.57(9) . . ? N3 Co1 N4 169.36(10) . . ? O1 Co1 N2 89.42(10) . . ? O2 Co1 N2 173.75(10) . . ? N3 Co1 N2 85.67(10) . . ? N4 Co1 N2 95.23(10) . . ? O1 Co1 N1 175.80(9) . . ? O2 Co1 N1 88.85(9) . . ? N3 Co1 N1 85.51(10) . . ? N4 Co1 N1 83.97(10) . . ? N2 Co1 N1 86.62(10) . . ? 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 -1.8(5) . . . . ? C1 C2 C3 C4 179.5(3) . . . . ? C2 C3 C4 O2 0.4(5) . . . . ? C2 C3 C4 C5 179.0(3) . . . . ? O2 C4 C5 C6 24.2(4) . . . . ? C3 C4 C5 C6 -154.4(3) . . . . ? O2 C4 C5 C10 -156.6(3) . . . . ? C3 C4 C5 C10 24.7(4) . . . . ? C10 C5 C6 C7 -2.7(5) . . . . ? C4 C5 C6 C7 176.5(3) . . . . ? C5 C6 C7 C8 3.0(5) . . . . ? C6 C7 C8 C9 -0.9(5) . . . . ? C7 C8 C9 C10 -1.6(5) . . . . ? C8 C9 C10 C5 1.9(5) . . . . ? C6 C5 C10 C9 0.2(5) . . . . ? C4 C5 C10 C9 -178.9(3) . . . . ? N4 C11 C12 C13 -0.7(4) . . . . ? C16 C11 C12 C13 177.7(3) . . . . ? C11 C12 C13 C14 2.1(5) . . . . ? C12 C13 C14 C15 -1.6(4) . . . . ? C13 C14 C15 N4 -0.2(4) . . . . ? N4 C11 C16 N1 -23.5(3) . . . . ? C12 C11 C16 N1 158.1(3) . . . . ? N2 C17 C18 C19 -1.4(5) . . . . ? C22 C17 C18 C19 175.9(3) . . . . ? C17 C18 C19 C20 -0.6(5) . . . . ? C18 C19 C20 C21 2.2(5) . . . . ? C19 C20 C21 N2 -1.7(5) . . . . ? N2 C17 C22 N1 -28.6(4) . . . . ? C18 C17 C22 N1 153.9(3) . . . . ? N3 C23 C24 C25 0.7(5) . . . . ? C28 C23 C24 C25 -178.2(3) . . . . ? C23 C24 C25 C26 -0.6(5) . . . . ? C24 C25 C26 C27 0.1(5) . . . . ? C25 C26 C27 N3 0.4(4) . . . . ? N3 C23 C28 N1 28.9(3) . . . . ? C24 C23 C28 N1 -152.2(3) . . . . ? C14 C15 N4 C11 1.6(4) . . . . ? C14 C15 N4 Co1 -175.2(2) . . . . ? C12 C11 N4 C15 -1.2(4) . . . . ? C16 C11 N4 C15 -179.7(3) . . . . ? C12 C11 N4 Co1 176.0(2) . . . . ? C16 C11 N4 Co1 -2.5(3) . . . . ? C20 C21 N2 C17 -0.3(4) . . . . ? C20 C21 N2 Co1 161.0(2) . . . . ? C18 C17 N2 C21 1.9(4) . . . . ? C22 C17 N2 C21 -175.7(3) . . . . ? C18 C17 N2 Co1 -161.4(2) . . . . ? C22 C17 N2 Co1 21.0(3) . . . . ? C24 C23 N3 C27 -0.1(4) . . . . ? C28 C23 N3 C27 178.8(2) . . . . ? C24 C23 N3 Co1 173.3(2) . . . . ? C28 C23 N3 Co1 -7.7(3) . . . . ? C26 C27 N3 C23 -0.4(4) . . . . ? C26 C27 N3 Co1 -172.9(2) . . . . ? C23 C28 N1 C16 -151.9(2) . . . . ? C23 C28 N1 C22 84.4(3) . . . . ? C23 C28 N1 Co1 -35.3(3) . . . . ? C11 C16 N1 C28 154.4(2) . . . . ? C11 C16 N1 C22 -80.5(3) . . . . ? C11 C16 N1 Co1 37.5(3) . . . . ? C17 C22 N1 C28 -96.3(3) . . . . ? C17 C22 N1 C16 138.4(2) . . . . ? C17 C22 N1 Co1 22.2(3) . . . . ? C3 C2 O1 Co1 0.7(4) . . . . ? C1 C2 O1 Co1 179.5(2) . . . . ? C3 C4 O2 Co1 1.8(4) . . . . ? C5 C4 O2 Co1 -176.78(19) . . . . ? C2 O1 Co1 O2 1.0(2) . . . . ? C2 O1 Co1 N3 -89.2(2) . . . . ? C2 O1 Co1 N4 90.0(2) . . . . ? C2 O1 Co1 N2 -174.8(2) . . . . ? C4 O2 Co1 O1 -2.2(2) . . . . ? C4 O2 Co1 N3 93.4(2) . . . . ? C4 O2 Co1 N4 -97.1(2) . . . . ? C4 O2 Co1 N1 178.9(2) . . . . ? C23 N3 Co1 O1 173.1(2) . . . . ? C27 N3 Co1 O1 -13.9(2) . . . . ? C23 N3 Co1 O2 77.9(2) . . . . ? C27 N3 Co1 O2 -109.1(2) . . . . ? C23 N3 Co1 N4 -2.6(7) . . . . ? C27 N3 Co1 N4 170.4(5) . . . . ? C23 N3 Co1 N2 -97.9(2) . . . . ? C27 N3 Co1 N2 75.1(2) . . . . ? C23 N3 Co1 N1 -10.9(2) . . . . ? C27 N3 Co1 N1 162.0(2) . . . . ? C15 N4 Co1 O1 13.2(2) . . . . ? C11 N4 Co1 O1 -163.78(19) . . . . ? C15 N4 Co1 O2 108.3(2) . . . . ? C11 N4 Co1 O2 -68.68(19) . . . . ? C15 N4 Co1 N3 -171.1(5) . . . . ? C11 N4 Co1 N3 12.0(6) . . . . ? C15 N4 Co1 N2 -76.7(2) . . . . ? C11 N4 Co1 N2 106.3(2) . . . . ? C15 N4 Co1 N1 -162.7(2) . . . . ? C11 N4 Co1 N1 20.31(19) . . . . ? C21 N2 Co1 O1 12.8(3) . . . . ? C17 N2 Co1 O1 175.2(2) . . . . ? C21 N2 Co1 N3 -82.8(3) . . . . ? C17 N2 Co1 N3 79.5(2) . . . . ? C21 N2 Co1 N4 107.8(3) . . . . ? C17 N2 Co1 N4 -89.9(2) . . . . ? C21 N2 Co1 N1 -168.6(3) . . . . ? C17 N2 Co1 N1 -6.2(2) . . . . ? C28 N1 Co1 O2 -63.71(17) . . . . ? C16 N1 Co1 O2 56.68(18) . . . . ? C22 N1 Co1 O2 174.75(19) . . . . ? C28 N1 Co1 N3 26.06(17) . . . . ? C16 N1 Co1 N3 146.45(19) . . . . ? C22 N1 Co1 N3 -95.48(19) . . . . ? C28 N1 Co1 N4 -152.40(18) . . . . ? C16 N1 Co1 N4 -32.01(18) . . . . ? C22 N1 Co1 N4 86.07(19) . . . . ? C28 N1 Co1 N2 111.98(18) . . . . ? C16 N1 Co1 N2 -127.63(19) . . . . ? C22 N1 Co1 N2 -9.56(19) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.72 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.905 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.100 data_10 _database_code_depnum_ccdc_archive 'CCDC 866274' #TrackingRef '- combined revised cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H48 Co2 N8 O4, 2(Cl O4)' _chemical_formula_sum 'C56 H48 Cl2 Co2 N8 O12' _chemical_formula_weight 1213.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' _Int_tables_symmetry_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.553(3) _cell_length_b 10.8220(14) _cell_length_c 22.239(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.066(9) _cell_angle_gamma 90.00 _cell_volume 5179.7(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2139 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 21.06 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2496 _exptl_absorpt_coefficient_mu 0.818 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6688 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2007)' _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 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type APEXII-FR591 _diffrn_measurement_method \w+\f _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 52547 _diffrn_reflns_av_R_equivalents 0.1921 _diffrn_reflns_av_sigmaI/netI 0.1731 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 0.95 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9100 _reflns_number_gt 4288 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX (Bruker-Nonius, 2003)' _computing_cell_refinement 'SAINT (Bruker-Nonius, 2003)' _computing_data_reduction 'SAINT (Bruker-Nonius, 2003), XPREP (Bruker-Nonius, 2003)' _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) POV-Ray 3.5 (Cason, 2002) WebLab ViewerPro 3.7 (Molecular Simulations, 2000) ; _computing_publication_material 'enCIFer 1.1 (CCDC, 2005)' _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^)+(0.0429P)^2^+3.2810P] 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 9100 _refine_ls_number_parameters 721 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.1819 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.1313 _refine_ls_wR_factor_gt 0.1058 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.940 _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 0.3497(3) 0.0056(5) 0.6369(3) 0.0199(14) Uani 1 1 d . . . C2 C 0.3487(3) -0.1722(5) 0.6978(3) 0.0213(15) Uani 1 1 d . . . H2 H 0.3390 -0.2102 0.7346 0.026 Uiso 1 1 calc R . . C3 C 0.3777(3) -0.2398(5) 0.6550(3) 0.0244(15) Uani 1 1 d . . . H3 H 0.3873 -0.3245 0.6617 0.029 Uiso 1 1 calc R . . C4 C 0.3927(3) -0.1822(6) 0.6019(3) 0.0291(16) Uani 1 1 d . . . H4 H 0.4115 -0.2282 0.5714 0.035 Uiso 1 1 calc R . . C5 C 0.3803(2) -0.0585(5) 0.5934(3) 0.0244(15) Uani 1 1 d . . . H5 H 0.3925 -0.0175 0.5581 0.029 Uiso 1 1 calc R . . C6 C 0.3290(3) 0.1383(5) 0.6323(3) 0.0212(15) Uani 1 1 d . . . H6A H 0.3572 0.1864 0.6075 0.025 Uiso 1 1 calc R . . H6B H 0.2863 0.1437 0.6136 0.025 Uiso 1 1 calc R . . C7 C 0.4081(3) 0.1509(5) 0.7794(3) 0.0218(15) Uani 1 1 d . . . C8 C 0.3727(3) 0.0065(5) 0.8479(3) 0.0218(15) Uani 1 1 d . . . H8 H 0.3425 -0.0527 0.8583 0.026 Uiso 1 1 calc R . . C9 C 0.4231(3) 0.0282(5) 0.8870(3) 0.0252(15) Uani 1 1 d . . . H9 H 0.4277 -0.0152 0.9241 0.030 Uiso 1 1 calc R . . C11 C 0.4669(3) 0.1132(5) 0.8718(3) 0.0289(16) Uani 1 1 d . . . H11 H 0.5020 0.1288 0.8983 0.035 Uiso 1 1 calc R . . C12 C 0.4598(3) 0.1761(5) 0.8176(3) 0.0273(16) Uani 1 1 d . . . H12 H 0.4897 0.2354 0.8067 0.033 Uiso 1 1 calc R . . C13 C 0.3979(3) 0.2055(5) 0.7184(3) 0.0236(15) Uani 1 1 d . . . H13A H 0.4261 0.1660 0.6904 0.028 Uiso 1 1 calc R . . H13B H 0.4075 0.2950 0.7200 0.028 Uiso 1 1 calc R . . C14 C 0.2630(3) 0.3013(5) 0.7610(3) 0.0203(14) Uani 1 1 d . . . C15 C 0.2242(3) 0.1759(6) 0.8355(3) 0.0244(15) Uani 1 1 d . . . H15 H 0.2198 0.0962 0.8528 0.029 Uiso 1 1 calc R . . C16 C 0.1983(3) 0.2774(6) 0.8627(3) 0.0295(16) Uani 1 1 d . . . H16 H 0.1750 0.2675 0.8974 0.035 Uiso 1 1 calc R . . C17 C 0.2069(3) 0.3939(6) 0.8385(3) 0.0330(17) Uani 1 1 d . . . H17 H 0.1899 0.4646 0.8568 0.040 Uiso 1 1 calc R . . C18 C 0.2401(3) 0.4063(5) 0.7880(3) 0.0287(16) Uani 1 1 d . . . H18 H 0.2474 0.4858 0.7717 0.034 Uiso 1 1 calc R . . C19 C 0.2924(3) 0.3022(5) 0.7016(3) 0.0235(15) Uani 1 1 d . . . H19A H 0.3191 0.3761 0.6987 0.028 Uiso 1 1 calc R . . H19B H 0.2597 0.3058 0.6686 0.028 Uiso 1 1 calc R . . C20 C 0.1792(2) -0.0264(5) 0.7100(2) 0.0145(13) Uani 1 1 d . . . C21 C 0.1996(3) -0.0957(5) 0.7633(3) 0.0193(14) Uani 1 1 d . . . C22 C 0.1608(3) -0.1822(5) 0.7860(3) 0.0190(14) Uani 1 1 d U . . H22 H 0.1743 -0.2288 0.8204 0.023 Uiso 1 1 calc R . . C23 C 0.1005(3) -0.2033(5) 0.7589(3) 0.0205(15) Uani 1 1 d . . . C24 C 0.0603(3) -0.2958(5) 0.7815(3) 0.0288(16) Uani 1 1 d . . . H24 H 0.0732 -0.3414 0.8164 0.035 Uiso 1 1 calc R . . C25 C 0.0034(3) -0.3193(5) 0.7532(3) 0.0306(16) Uani 1 1 d . . . H25 H -0.0223 -0.3828 0.7676 0.037 Uiso 1 1 calc R . . C26 C -0.0167(3) -0.2485(5) 0.7024(3) 0.0297(17) Uani 1 1 d . . . H26 H -0.0565 -0.2639 0.6834 0.036 Uiso 1 1 calc R . . C27 C 0.0202(3) -0.1584(5) 0.6803(3) 0.0243(16) Uani 1 1 d . . . H27 H 0.0058 -0.1116 0.6461 0.029 Uiso 1 1 calc R . . C28 C 0.0799(2) -0.1341(5) 0.7080(3) 0.0164(14) Uani 1 1 d . . . C29 C 0.1205(2) -0.0457(5) 0.6840(2) 0.0169(13) Uani 1 1 d . . . H29 H 0.1071 0.0008 0.6495 0.020 Uiso 1 1 calc R . . C30 C 0.1613(3) -0.0298(5) 1.1355(3) 0.0223(15) Uani 1 1 d . . . C32 C 0.1621(3) 0.1481(5) 1.0765(3) 0.0262(16) Uani 1 1 d . . . H32 H 0.1709 0.1874 1.0397 0.031 Uiso 1 1 calc R . . C33 C 0.1371(3) 0.2158(6) 1.1221(3) 0.0311(17) Uani 1 1 d . . . H33 H 0.1296 0.3018 1.1171 0.037 Uiso 1 1 calc R . . C35 C 0.1230(3) 0.1580(6) 1.1750(3) 0.0336(18) Uani 1 1 d . . . H35 H 0.1060 0.2038 1.2066 0.040 Uiso 1 1 calc R . . C36 C 0.1339(3) 0.0321(6) 1.1815(3) 0.0294(16) Uani 1 1 d . . . H36 H 0.1228 -0.0104 1.2167 0.035 Uiso 1 1 calc R . . C37 C 0.1828(3) -0.1630(5) 1.1389(3) 0.0250(15) Uani 1 1 d . . . H37A H 0.2259 -0.1674 1.1565 0.030 Uiso 1 1 calc R . . H37B H 0.1557 -0.2115 1.1647 0.030 Uiso 1 1 calc R . . C38 C 0.2465(3) -0.3205(5) 1.0078(3) 0.0193(14) Uani 1 1 d . . . C39 C 0.2651(3) -0.1993(5) 0.9241(3) 0.0230(15) Uani 1 1 d . . . H39 H 0.2614 -0.1219 0.9041 0.028 Uiso 1 1 calc R . . C40 C 0.2933(3) -0.2965(6) 0.8958(3) 0.0299(16) Uani 1 1 d . . . H40 H 0.3089 -0.2863 0.8570 0.036 Uiso 1 1 calc R . . C41 C 0.2984(3) -0.4094(5) 0.9255(3) 0.0287(16) Uani 1 1 d . . . H41 H 0.3187 -0.4772 0.9078 0.034 Uiso 1 1 calc R . . C42 C 0.2732(2) -0.4213(5) 0.9812(3) 0.0232(14) Uani 1 1 d . . . H42 H 0.2744 -0.4989 1.0012 0.028 Uiso 1 1 calc R . . C43 C 0.2236(3) -0.3200(5) 1.0699(3) 0.0228(15) Uani 1 1 d . . . H43A H 0.2591 -0.3120 1.0998 0.027 Uiso 1 1 calc R . . H43B H 0.2020 -0.3988 1.0776 0.027 Uiso 1 1 calc R . . C44 C 0.0920(3) -0.1805(5) 1.0004(3) 0.0286(16) Uani 1 1 d . . . C45 C 0.0363(3) -0.2065(7) 0.9706(4) 0.057(2) Uani 1 1 d . . . H45 H 0.0102 -0.2705 0.9839 0.068 Uiso 1 1 calc R . . C46 C 0.0193(4) -0.1365(8) 0.9203(4) 0.071(3) Uani 1 1 d U . . H46 H -0.0192 -0.1519 0.8988 0.085 Uiso 1 1 calc R . . C47 C 0.0581(3) -0.0441(7) 0.9012(3) 0.061(2) Uani 1 1 d . . . H47 H 0.0466 0.0033 0.8664 0.073 Uiso 1 1 calc R . . C48 C 0.1128(3) -0.0218(6) 0.9329(3) 0.0336(17) Uani 1 1 d . . . H48 H 0.1387 0.0439 0.9210 0.040 Uiso 1 1 calc R . . C49 C 0.1142(3) -0.2489(5) 1.0559(3) 0.0229(15) Uani 1 1 d . . . H49A H 0.1125 -0.3388 1.0478 0.028 Uiso 1 1 calc R . . H49B H 0.0861 -0.2311 1.0886 0.028 Uiso 1 1 calc R . . C50 C 0.3197(3) 0.0216(5) 1.0495(3) 0.0185(14) Uani 1 1 d . . . C51 C 0.2927(3) 0.0864(5) 0.9979(2) 0.0172(13) Uani 1 1 d . . . C52 C 0.3243(3) 0.1811(5) 0.9725(3) 0.0193(14) Uani 1 1 d . . . H52 H 0.3061 0.2231 0.9385 0.023 Uiso 1 1 calc R . . C53 C 0.3838(3) 0.2176(5) 0.9964(3) 0.0178(14) Uani 1 1 d . . . C54 C 0.4184(3) 0.3118(5) 0.9691(3) 0.0291(17) Uani 1 1 d . . . H54 H 0.4020 0.3511 0.9335 0.035 Uiso 1 1 calc R . . C55 C 0.4759(3) 0.3465(5) 0.9938(3) 0.0354(18) Uani 1 1 d . . . H55 H 0.4988 0.4089 0.9748 0.043 Uiso 1 1 calc R . . C56 C 0.5007(3) 0.2909(6) 1.0466(3) 0.0346(18) Uani 1 1 d . . . H56 H 0.5397 0.3173 1.0640 0.041 Uiso 1 1 calc R . . C57 C 0.4685(3) 0.1980(5) 1.0732(3) 0.0307(17) Uani 1 1 d . . . H57 H 0.4857 0.1613 1.1092 0.037 Uiso 1 1 calc R . . C58 C 0.4105(3) 0.1554(5) 1.0487(3) 0.0211(15) Uani 1 1 d . . . C59 C 0.3770(2) 0.0580(5) 1.0744(3) 0.0205(14) Uani 1 1 d . . . H59 H 0.3942 0.0169 1.1092 0.025 Uiso 1 1 calc R . . N4 N 0.3340(2) -0.0519(4) 0.6879(2) 0.0190(11) Uani 1 1 d . . . N2 N 0.3651(2) 0.0678(4) 0.7951(2) 0.0203(11) Uani 1 1 d . . . N3 N 0.2554(2) 0.1885(4) 0.7848(2) 0.0205(12) Uani 1 1 d . . . N1 N 0.3309(2) 0.1868(4) 0.6953(2) 0.0200(12) Uani 1 1 d . . . N8 N 0.1741(2) 0.0269(4) 1.0841(2) 0.0213(12) Uani 1 1 d . . . N7 N 0.2428(2) -0.2113(4) 0.9790(2) 0.0194(12) Uani 1 1 d . . . N6 N 0.1309(2) -0.0919(4) 0.9810(2) 0.0204(12) Uani 1 1 d . . . N5 N 0.1797(2) -0.2140(4) 1.0765(2) 0.0201(12) Uani 1 1 d . . . O2 O 0.22083(16) 0.0529(3) 0.68874(16) 0.0198(9) Uani 1 1 d . . . O1 O 0.25731(16) -0.0713(3) 0.78596(16) 0.0188(9) Uani 1 1 d . . . O3 O 0.4274(3) -0.3342(4) 0.8032(3) 0.084(2) Uani 1 1 d D A . O4A O 0.3788(7) -0.4606(11) 0.7389(8) 0.0621(15) Uani 0.25 1 d PD A 2 O4 O 0.4199(3) -0.4935(6) 0.7306(3) 0.0621(15) Uani 0.75 1 d P A 1 O5 O 0.3913(3) -0.5343(6) 0.8299(3) 0.101(2) Uani 1 1 d D A . O6 O 0.4929(3) -0.5044(6) 0.8090(3) 0.0621(15) Uani 0.75 1 d P A 1 O6A O 0.4728(7) -0.5061(10) 0.7752(8) 0.0621(15) Uani 0.25 1 d PD A 2 O9 O 0.28564(16) -0.0702(3) 1.07175(17) 0.0201(9) Uani 1 1 d . . . O8 O 0.23667(16) 0.0465(3) 0.97688(17) 0.0208(10) Uani 1 1 d . . . O10 O 0.0803(2) 0.3216(4) 0.9513(2) 0.0625(17) Uani 1 1 d . . . O11 O 0.1102(2) 0.5311(4) 0.9420(2) 0.0606(15) Uani 1 1 d . . . O12 O 0.1688(2) 0.3961(4) 1.0045(2) 0.0549(15) Uani 1 1 d . . . O13 O 0.0704(2) 0.4582(4) 1.0322(2) 0.0453(13) Uani 1 1 d . . . Cl2 Cl 0.42757(8) -0.46289(14) 0.79275(8) 0.0355(4) Uani 1 1 d . . . Cl3 Cl 0.10686(7) 0.42728(14) 0.98222(8) 0.0331(4) Uani 1 1 d . . . Co1 Co 0.29282(3) 0.05745(7) 0.74147(3) 0.0176(2) Uani 1 1 d . . . Co2 Co 0.20935(3) -0.08090(7) 1.02586(4) 0.0177(2) 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 0.014(3) 0.033(4) 0.012(4) 0.004(3) -0.004(3) -0.003(3) C2 0.025(4) 0.013(3) 0.025(4) 0.012(3) -0.003(3) -0.002(3) C3 0.023(4) 0.025(3) 0.026(4) 0.000(3) 0.000(3) 0.004(3) C4 0.025(4) 0.035(4) 0.028(4) -0.007(3) 0.007(3) 0.008(3) C5 0.021(3) 0.034(4) 0.019(4) 0.004(3) 0.007(3) -0.007(3) C6 0.030(4) 0.024(3) 0.010(4) 0.003(3) 0.005(3) -0.005(3) C7 0.017(4) 0.020(3) 0.029(4) -0.009(3) -0.001(3) -0.004(3) C8 0.021(4) 0.024(3) 0.020(4) -0.006(3) -0.002(3) 0.001(3) C9 0.026(4) 0.027(3) 0.022(4) -0.001(3) 0.003(3) 0.006(3) C11 0.020(4) 0.033(4) 0.033(5) -0.008(3) -0.002(3) 0.002(3) C12 0.020(4) 0.025(4) 0.037(5) -0.004(3) 0.001(3) -0.004(3) C13 0.027(4) 0.019(3) 0.025(4) -0.004(3) 0.003(3) -0.005(3) C14 0.015(3) 0.032(4) 0.014(4) 0.000(3) 0.000(3) -0.001(3) C15 0.019(4) 0.034(4) 0.021(4) 0.000(3) 0.002(3) 0.000(3) C16 0.031(4) 0.039(4) 0.018(4) -0.003(3) 0.003(3) 0.001(3) C17 0.033(4) 0.042(4) 0.023(4) -0.014(3) 0.002(3) 0.007(3) C18 0.030(4) 0.024(4) 0.031(4) 0.001(3) -0.007(3) 0.006(3) C19 0.021(4) 0.012(3) 0.037(5) 0.001(3) 0.000(3) -0.001(3) C20 0.019(3) 0.016(3) 0.009(3) -0.002(2) 0.005(3) -0.002(3) C21 0.020(4) 0.023(3) 0.015(4) -0.005(3) 0.001(3) 0.002(3) C22 0.026(3) 0.023(3) 0.008(3) 0.010(3) 0.003(3) -0.005(3) C23 0.012(3) 0.024(3) 0.026(4) -0.004(3) 0.004(3) 0.000(3) C24 0.034(4) 0.030(3) 0.024(4) 0.000(3) 0.010(3) -0.003(3) C25 0.017(4) 0.029(4) 0.046(5) -0.009(3) 0.007(3) -0.010(3) C26 0.016(4) 0.033(4) 0.042(5) -0.011(3) 0.010(3) -0.003(3) C27 0.016(4) 0.026(3) 0.030(4) -0.011(3) 0.000(3) 0.003(3) C28 0.007(3) 0.021(3) 0.021(4) -0.003(3) 0.004(3) 0.003(2) C29 0.017(3) 0.019(3) 0.014(3) -0.002(3) -0.001(3) 0.004(3) C30 0.022(4) 0.022(3) 0.022(4) -0.001(3) -0.008(3) -0.009(3) C32 0.019(4) 0.024(4) 0.033(5) 0.000(3) -0.015(3) -0.001(3) C33 0.033(4) 0.024(4) 0.035(5) -0.011(3) -0.003(3) 0.002(3) C35 0.035(4) 0.035(4) 0.030(5) -0.020(3) 0.000(4) 0.007(3) C36 0.025(4) 0.035(4) 0.027(4) -0.006(3) 0.000(3) -0.003(3) C37 0.032(4) 0.022(3) 0.021(4) 0.005(3) 0.006(3) -0.003(3) C38 0.015(3) 0.021(3) 0.022(4) 0.003(3) -0.002(3) -0.005(3) C39 0.024(4) 0.026(3) 0.020(4) 0.003(3) 0.010(3) -0.004(3) C40 0.031(4) 0.040(4) 0.019(4) -0.001(3) 0.012(3) -0.007(3) C41 0.027(4) 0.026(4) 0.033(4) -0.009(3) 0.002(3) 0.002(3) C42 0.023(4) 0.024(3) 0.022(4) -0.002(3) 0.000(3) -0.002(3) C43 0.028(4) 0.024(3) 0.016(4) 0.008(3) 0.002(3) 0.000(3) C44 0.027(4) 0.035(4) 0.024(4) 0.000(3) 0.002(3) -0.004(3) C45 0.035(5) 0.080(6) 0.054(6) 0.033(5) -0.016(4) -0.029(4) C46 0.035(4) 0.101(6) 0.073(6) 0.032(5) -0.023(4) -0.029(4) C47 0.042(5) 0.090(6) 0.048(5) 0.041(5) -0.027(4) -0.016(5) C48 0.031(4) 0.040(4) 0.029(4) 0.020(3) -0.005(3) -0.004(3) C49 0.021(4) 0.027(3) 0.021(4) -0.003(3) 0.006(3) -0.009(3) C50 0.018(3) 0.021(3) 0.017(4) -0.001(3) 0.006(3) 0.007(3) C51 0.022(3) 0.017(3) 0.014(3) 0.003(3) 0.002(3) -0.002(3) C52 0.023(4) 0.019(3) 0.015(4) -0.001(3) -0.002(3) 0.002(3) C53 0.020(4) 0.015(3) 0.020(4) 0.000(3) 0.011(3) -0.007(3) C54 0.038(4) 0.019(3) 0.032(5) -0.001(3) 0.015(3) -0.003(3) C55 0.042(5) 0.023(4) 0.043(5) -0.013(3) 0.020(4) -0.012(3) C56 0.018(4) 0.032(4) 0.055(6) -0.019(4) 0.008(4) -0.001(3) C57 0.019(4) 0.024(4) 0.049(5) -0.008(3) 0.009(3) 0.000(3) C58 0.013(3) 0.020(3) 0.031(4) -0.011(3) 0.001(3) 0.003(3) C59 0.014(3) 0.020(3) 0.027(4) -0.003(3) -0.002(3) 0.003(3) N4 0.020(3) 0.020(3) 0.017(3) 0.002(2) -0.002(2) -0.005(2) N2 0.023(3) 0.025(3) 0.013(3) -0.001(2) 0.000(2) -0.001(2) N3 0.017(3) 0.021(3) 0.023(3) -0.002(2) -0.001(3) -0.001(2) N1 0.017(3) 0.024(3) 0.019(3) -0.002(2) 0.002(2) -0.001(2) N8 0.024(3) 0.018(3) 0.022(3) -0.004(2) 0.000(2) 0.003(2) N7 0.017(3) 0.026(3) 0.014(3) 0.005(2) -0.004(2) -0.006(2) N6 0.013(3) 0.025(3) 0.023(3) -0.003(2) 0.002(2) -0.002(2) N5 0.022(3) 0.016(3) 0.022(3) -0.001(2) 0.003(2) -0.009(2) O2 0.019(2) 0.024(2) 0.016(2) 0.0023(18) -0.0019(18) -0.0049(19) O1 0.018(2) 0.026(2) 0.012(2) -0.0005(19) -0.0023(18) -0.0057(18) O3 0.156(6) 0.028(3) 0.064(4) -0.015(3) -0.030(4) 0.020(3) O4A 0.063(4) 0.048(3) 0.071(4) 0.011(3) -0.036(3) -0.013(3) O4 0.063(4) 0.048(3) 0.071(4) 0.011(3) -0.036(3) -0.013(3) O5 0.107(5) 0.095(5) 0.109(6) 0.052(4) 0.079(4) 0.015(4) O6 0.063(4) 0.048(3) 0.071(4) 0.011(3) -0.036(3) -0.013(3) O6A 0.063(4) 0.048(3) 0.071(4) 0.011(3) -0.036(3) -0.013(3) O9 0.018(2) 0.022(2) 0.020(2) 0.0053(19) 0.0026(18) -0.0055(18) O8 0.019(2) 0.018(2) 0.025(3) 0.0093(18) -0.0001(19) -0.0016(18) O10 0.053(4) 0.072(4) 0.065(4) -0.046(3) 0.023(3) -0.030(3) O11 0.078(4) 0.056(3) 0.050(4) 0.033(3) 0.021(3) 0.015(3) O12 0.033(3) 0.050(3) 0.081(4) 0.017(3) -0.003(3) -0.009(2) O13 0.060(3) 0.038(3) 0.040(3) -0.010(2) 0.027(3) -0.002(2) Cl2 0.0424(11) 0.0343(10) 0.0299(11) 0.0014(8) 0.0015(9) -0.0026(8) Cl3 0.0344(10) 0.0304(9) 0.0352(11) -0.0045(8) 0.0085(8) -0.0026(8) Co1 0.0187(5) 0.0199(4) 0.0144(5) 0.0016(4) 0.0006(4) -0.0017(4) Co2 0.0189(5) 0.0185(4) 0.0156(5) 0.0012(4) 0.0008(4) -0.0031(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N4 1.353(7) . ? C1 C5 1.386(8) . ? C1 C6 1.505(7) . ? C2 N4 1.355(6) . ? C2 C3 1.377(8) . ? C2 H2 0.9500 . ? C3 C4 1.389(8) . ? C3 H3 0.9500 . ? C4 C5 1.376(8) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 N1 1.495(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N2 1.351(7) . ? C7 C12 1.392(7) . ? C7 C13 1.486(8) . ? C8 N2 1.351(7) . ? C8 C9 1.376(7) . ? C8 H8 0.9500 . ? C9 C11 1.373(8) . ? C9 H9 0.9500 . ? C11 C12 1.385(8) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 N1 1.519(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N3 1.344(7) . ? C14 C18 1.389(8) . ? C14 C19 1.495(8) . ? C15 N3 1.351(7) . ? C15 C16 1.385(8) . ? C15 H15 0.9500 . ? C16 C17 1.387(8) . ? C16 H16 0.9500 . ? C17 C18 1.369(8) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 N1 1.511(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 O2 1.345(6) . ? C20 C29 1.379(7) . ? C20 C21 1.450(7) . ? C21 O1 1.343(6) . ? C21 C22 1.370(7) . ? C22 C23 1.421(7) . ? C22 H22 0.9500 . ? C23 C28 1.408(8) . ? C23 C24 1.433(8) . ? C24 C25 1.371(8) . ? C24 H24 0.9500 . ? C25 C26 1.413(9) . ? C25 H25 0.9500 . ? C26 C27 1.367(8) . ? C26 H26 0.9500 . ? C27 C28 1.422(7) . ? C27 H27 0.9500 . ? C28 C29 1.421(7) . ? C29 H29 0.9500 . ? C30 N8 1.340(7) . ? C30 C36 1.382(8) . ? C30 C37 1.515(8) . ? C32 N8 1.345(7) . ? C32 C33 1.384(8) . ? C32 H32 0.9500 . ? C33 C35 1.381(9) . ? C33 H33 0.9500 . ? C35 C36 1.388(8) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 N5 1.491(7) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 N7 1.344(7) . ? C38 C42 1.382(7) . ? C38 C43 1.492(8) . ? C39 N7 1.341(7) . ? C39 C40 1.383(8) . ? C39 H39 0.9500 . ? C40 C41 1.390(8) . ? C40 H40 0.9500 . ? C41 C42 1.385(8) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 N5 1.499(7) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 N6 1.360(7) . ? C44 C45 1.369(8) . ? C44 C49 1.496(8) . ? C45 C46 1.384(10) . ? C45 H45 0.9500 . ? C46 C47 1.384(9) . ? C46 H46 0.9500 . ? C47 C48 1.364(8) . ? C47 H47 0.9500 . ? C48 N6 1.353(7) . ? C48 H48 0.9500 . ? C49 N5 1.507(6) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 O9 1.345(6) . ? C50 C59 1.384(7) . ? C50 C51 1.441(7) . ? C51 O8 1.343(6) . ? C51 C52 1.369(7) . ? C52 C53 1.418(7) . ? C52 H52 0.9500 . ? C53 C54 1.418(7) . ? C53 C58 1.437(8) . ? C54 C55 1.379(8) . ? C54 H54 0.9500 . ? C55 C56 1.400(9) . ? C55 H55 0.9500 . ? C56 C57 1.373(8) . ? C56 H56 0.9500 . ? C57 C58 1.415(7) . ? C57 H57 0.9500 . ? C58 C59 1.415(8) . ? C59 H59 0.9500 . ? N4 Co1 1.929(5) . ? N2 Co1 1.914(4) . ? N3 Co1 1.917(5) . ? N1 Co1 1.943(5) . ? N8 Co2 1.929(5) . ? N7 Co2 1.918(5) . ? N6 Co2 1.920(4) . ? N5 Co2 1.958(5) . ? O2 Co1 1.895(3) . ? O1 Co1 1.894(4) . ? O3 Cl2 1.412(4) . ? O4A Cl2 1.551(15) . ? O4 Cl2 1.422(7) . ? O5 Cl2 1.400(5) . ? O6 Cl2 1.504(7) . ? O6A Cl2 1.168(17) . ? O9 Co2 1.892(3) . ? O8 Co2 1.871(4) . ? O10 Cl3 1.437(4) . ? O11 Cl3 1.440(5) . ? O12 Cl3 1.439(4) . ? O13 Cl3 1.434(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 C1 C5 120.3(5) . . ? N4 C1 C6 114.2(5) . . ? C5 C1 C6 125.5(6) . . ? N4 C2 C3 120.6(6) . . ? N4 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C2 C3 C4 118.9(5) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 120.1(6) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C1 119.2(6) . . ? C4 C5 H5 120.4 . . ? C1 C5 H5 120.4 . . ? N1 C6 C1 106.1(5) . . ? N1 C6 H6A 110.5 . . ? C1 C6 H6A 110.5 . . ? N1 C6 H6B 110.5 . . ? C1 C6 H6B 110.5 . . ? H6A C6 H6B 108.7 . . ? N2 C7 C12 120.7(6) . . ? N2 C7 C13 115.5(5) . . ? C12 C7 C13 123.7(5) . . ? N2 C8 C9 121.3(5) . . ? N2 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C11 C9 C8 119.3(6) . . ? C11 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C9 C11 C12 119.9(6) . . ? C9 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C7 118.9(6) . . ? C11 C12 H12 120.6 . . ? C7 C12 H12 120.6 . . ? C7 C13 N1 110.3(5) . . ? C7 C13 H13A 109.6 . . ? N1 C13 H13A 109.6 . . ? C7 C13 H13B 109.6 . . ? N1 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? N3 C14 C18 121.2(6) . . ? N3 C14 C19 114.9(5) . . ? C18 C14 C19 123.7(5) . . ? N3 C15 C16 120.9(6) . . ? N3 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C15 C16 C17 119.1(6) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C18 C17 C16 119.6(6) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C14 119.2(6) . . ? C17 C18 H18 120.4 . . ? C14 C18 H18 120.4 . . ? C14 C19 N1 109.7(5) . . ? C14 C19 H19A 109.7 . . ? N1 C19 H19A 109.7 . . ? C14 C19 H19B 109.7 . . ? N1 C19 H19B 109.7 . . ? H19A C19 H19B 108.2 . . ? O2 C20 C29 124.2(5) . . ? O2 C20 C21 116.0(5) . . ? C29 C20 C21 119.7(5) . . ? O1 C21 C22 124.6(5) . . ? O1 C21 C20 116.0(5) . . ? C22 C21 C20 119.3(5) . . ? C21 C22 C23 121.1(5) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C28 C23 C22 119.8(5) . . ? C28 C23 C24 118.8(5) . . ? C22 C23 C24 121.3(5) . . ? C25 C24 C23 120.8(6) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C26 119.7(6) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C27 C26 C25 121.0(6) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 C28 120.4(6) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C23 C28 C29 119.1(5) . . ? C23 C28 C27 119.3(5) . . ? C29 C28 C27 121.5(5) . . ? C20 C29 C28 120.9(5) . . ? C20 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? N8 C30 C36 121.7(5) . . ? N8 C30 C37 113.7(5) . . ? C36 C30 C37 124.5(6) . . ? N8 C32 C33 120.3(6) . . ? N8 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C32 C33 C35 119.8(6) . . ? C32 C33 H33 120.1 . . ? C35 C33 H33 120.1 . . ? C33 C35 C36 119.3(6) . . ? C33 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? C30 C36 C35 118.4(6) . . ? C30 C36 H36 120.8 . . ? C35 C36 H36 120.8 . . ? N5 C37 C30 107.9(5) . . ? N5 C37 H37A 110.1 . . ? C30 C37 H37A 110.1 . . ? N5 C37 H37B 110.1 . . ? C30 C37 H37B 110.1 . . ? H37A C37 H37B 108.4 . . ? N7 C38 C42 120.3(6) . . ? N7 C38 C43 115.2(5) . . ? C42 C38 C43 124.4(5) . . ? N7 C39 C40 121.8(6) . . ? N7 C39 H39 119.1 . . ? C40 C39 H39 119.1 . . ? C39 C40 C41 118.6(6) . . ? C39 C40 H40 120.7 . . ? C41 C40 H40 120.7 . . ? C42 C41 C40 118.8(6) . . ? C42 C41 H41 120.6 . . ? C40 C41 H41 120.6 . . ? C38 C42 C41 120.1(6) . . ? C38 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C38 C43 N5 109.5(4) . . ? C38 C43 H43A 109.8 . . ? N5 C43 H43A 109.8 . . ? C38 C43 H43B 109.8 . . ? N5 C43 H43B 109.8 . . ? H43A C43 H43B 108.2 . . ? N6 C44 C45 122.0(6) . . ? N6 C44 C49 115.8(5) . . ? C45 C44 C49 122.2(6) . . ? C44 C45 C46 117.9(7) . . ? C44 C45 H45 121.1 . . ? C46 C45 H45 121.1 . . ? C47 C46 C45 120.4(7) . . ? C47 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? C48 C47 C46 119.3(6) . . ? C48 C47 H47 120.4 . . ? C46 C47 H47 120.4 . . ? N6 C48 C47 121.0(6) . . ? N6 C48 H48 119.5 . . ? C47 C48 H48 119.5 . . ? C44 C49 N5 112.3(5) . . ? C44 C49 H49A 109.1 . . ? N5 C49 H49A 109.1 . . ? C44 C49 H49B 109.1 . . ? N5 C49 H49B 109.1 . . ? H49A C49 H49B 107.9 . . ? O9 C50 C59 123.8(5) . . ? O9 C50 C51 116.6(5) . . ? C59 C50 C51 119.6(5) . . ? O8 C51 C52 123.8(5) . . ? O8 C51 C50 115.9(5) . . ? C52 C51 C50 120.3(5) . . ? C51 C52 C53 121.0(5) . . ? C51 C52 H52 119.5 . . ? C53 C52 H52 119.5 . . ? C52 C53 C54 121.7(6) . . ? C52 C53 C58 119.1(5) . . ? C54 C53 C58 119.1(5) . . ? C55 C54 C53 120.4(6) . . ? C55 C54 H54 119.8 . . ? C53 C54 H54 119.8 . . ? C54 C55 C56 120.8(6) . . ? C54 C55 H55 119.6 . . ? C56 C55 H55 119.6 . . ? C57 C56 C55 119.8(6) . . ? C57 C56 H56 120.1 . . ? C55 C56 H56 120.1 . . ? C56 C57 C58 121.9(6) . . ? C56 C57 H57 119.0 . . ? C58 C57 H57 119.0 . . ? C59 C58 C57 123.1(6) . . ? C59 C58 C53 119.0(5) . . ? C57 C58 C53 117.8(5) . . ? C50 C59 C58 120.9(5) . . ? C50 C59 H59 119.5 . . ? C58 C59 H59 119.5 . . ? C1 N4 C2 120.8(5) . . ? C1 N4 Co1 112.3(4) . . ? C2 N4 Co1 126.9(4) . . ? C8 N2 C7 119.9(5) . . ? C8 N2 Co1 124.7(4) . . ? C7 N2 Co1 115.1(4) . . ? C14 N3 C15 119.9(5) . . ? C14 N3 Co1 114.2(4) . . ? C15 N3 Co1 125.9(4) . . ? C6 N1 C19 112.9(4) . . ? C6 N1 C13 110.0(4) . . ? C19 N1 C13 112.1(4) . . ? C6 N1 Co1 104.5(3) . . ? C19 N1 Co1 107.2(3) . . ? C13 N1 Co1 109.8(3) . . ? C30 N8 C32 120.4(5) . . ? C30 N8 Co2 113.7(4) . . ? C32 N8 Co2 125.9(5) . . ? C39 N7 C38 120.3(5) . . ? C39 N7 Co2 125.9(4) . . ? C38 N7 Co2 113.7(4) . . ? C48 N6 C44 119.3(5) . . ? C48 N6 Co2 125.8(4) . . ? C44 N6 Co2 114.8(4) . . ? C37 N5 C43 112.1(4) . . ? C37 N5 C49 111.7(4) . . ? C43 N5 C49 111.3(4) . . ? C37 N5 Co2 105.3(3) . . ? C43 N5 Co2 106.2(3) . . ? C49 N5 Co2 109.8(3) . . ? C20 O2 Co1 109.7(3) . . ? C21 O1 Co1 109.9(3) . . ? C50 O9 Co2 108.8(3) . . ? C51 O8 Co2 109.9(3) . . ? O6A Cl2 O5 118.6(6) . . ? O6A Cl2 O3 117.3(6) . . ? O5 Cl2 O3 116.2(4) . . ? O6A Cl2 O4 68.8(8) . . ? O5 Cl2 O4 113.9(4) . . ? O3 Cl2 O4 112.8(4) . . ? O6A Cl2 O4A 107.0(8) . . ? O5 Cl2 O4A 95.1(5) . . ? O3 Cl2 O4A 96.0(5) . . ? O4 Cl2 O4A 38.2(7) . . ? O6A Cl2 O6 34.1(9) . . ? O5 Cl2 O6 103.8(4) . . ? O3 Cl2 O6 105.4(4) . . ? O4 Cl2 O6 102.9(4) . . ? O4A Cl2 O6 141.1(7) . . ? O13 Cl3 O10 109.6(3) . . ? O13 Cl3 O12 109.0(3) . . ? O10 Cl3 O12 108.4(3) . . ? O13 Cl3 O11 110.3(3) . . ? O10 Cl3 O11 110.9(3) . . ? O12 Cl3 O11 108.6(3) . . ? O1 Co1 O2 87.92(15) . . ? O1 Co1 N2 93.19(18) . . ? O2 Co1 N2 178.10(18) . . ? O1 Co1 N3 95.12(18) . . ? O2 Co1 N3 88.74(17) . . ? N2 Co1 N3 89.62(19) . . ? O1 Co1 N4 94.78(18) . . ? O2 Co1 N4 89.47(17) . . ? N2 Co1 N4 91.97(19) . . ? N3 Co1 N4 169.9(2) . . ? O1 Co1 N1 178.55(18) . . ? O2 Co1 N1 92.70(18) . . ? N2 Co1 N1 86.2(2) . . ? N3 Co1 N1 86.2(2) . . ? N4 Co1 N1 83.92(19) . . ? O8 Co2 O9 88.70(16) . . ? O8 Co2 N7 94.96(18) . . ? O9 Co2 N7 89.82(17) . . ? O8 Co2 N6 92.25(18) . . ? O9 Co2 N6 178.65(19) . . ? N7 Co2 N6 91.06(19) . . ? O8 Co2 N8 95.29(19) . . ? O9 Co2 N8 87.88(18) . . ? N7 Co2 N8 169.4(2) . . ? N6 Co2 N8 91.08(19) . . ? O8 Co2 N5 179.22(18) . . ? O9 Co2 N5 92.07(18) . . ? N7 Co2 N5 85.2(2) . . ? N6 Co2 N5 87.0(2) . . ? N8 Co2 N5 84.6(2) . . ? 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 N4 C2 C3 C4 1.1(8) . . . . ? C2 C3 C4 C5 2.0(9) . . . . ? C3 C4 C5 C1 -3.6(8) . . . . ? N4 C1 C5 C4 2.1(8) . . . . ? C6 C1 C5 C4 -175.6(5) . . . . ? N4 C1 C6 N1 32.1(6) . . . . ? C5 C1 C6 N1 -150.2(5) . . . . ? N2 C8 C9 C11 -0.5(9) . . . . ? C8 C9 C11 C12 0.1(9) . . . . ? C9 C11 C12 C7 -0.3(9) . . . . ? N2 C7 C12 C11 0.8(9) . . . . ? C13 C7 C12 C11 -175.3(6) . . . . ? N2 C7 C13 N1 18.3(7) . . . . ? C12 C7 C13 N1 -165.4(5) . . . . ? N3 C15 C16 C17 -2.5(9) . . . . ? C15 C16 C17 C18 0.7(9) . . . . ? C16 C17 C18 C14 1.9(9) . . . . ? N3 C14 C18 C17 -2.8(9) . . . . ? C19 C14 C18 C17 171.6(5) . . . . ? N3 C14 C19 N1 -24.6(6) . . . . ? C18 C14 C19 N1 160.7(5) . . . . ? O2 C20 C21 O1 1.1(7) . . . . ? C29 C20 C21 O1 -179.9(4) . . . . ? O2 C20 C21 C22 -177.1(5) . . . . ? C29 C20 C21 C22 1.9(8) . . . . ? O1 C21 C22 C23 -179.3(5) . . . . ? C20 C21 C22 C23 -1.2(8) . . . . ? C21 C22 C23 C28 -0.3(9) . . . . ? C21 C22 C23 C24 178.3(5) . . . . ? C28 C23 C24 C25 1.8(9) . . . . ? C22 C23 C24 C25 -176.9(6) . . . . ? C23 C24 C25 C26 -2.2(9) . . . . ? C24 C25 C26 C27 1.2(9) . . . . ? C25 C26 C27 C28 0.1(9) . . . . ? C22 C23 C28 C29 1.2(8) . . . . ? C24 C23 C28 C29 -177.5(5) . . . . ? C22 C23 C28 C27 178.3(5) . . . . ? C24 C23 C28 C27 -0.4(8) . . . . ? C26 C27 C28 C23 -0.5(8) . . . . ? C26 C27 C28 C29 176.5(5) . . . . ? O2 C20 C29 C28 177.9(5) . . . . ? C21 C20 C29 C28 -1.0(8) . . . . ? C23 C28 C29 C20 -0.5(8) . . . . ? C27 C28 C29 C20 -177.6(5) . . . . ? N8 C32 C33 C35 -1.6(9) . . . . ? C32 C33 C35 C36 -0.3(9) . . . . ? N8 C30 C36 C35 -3.8(8) . . . . ? C37 C30 C36 C35 172.6(5) . . . . ? C33 C35 C36 C30 2.9(9) . . . . ? N8 C30 C37 N5 -31.0(6) . . . . ? C36 C30 C37 N5 152.3(5) . . . . ? N7 C39 C40 C41 0.2(9) . . . . ? C39 C40 C41 C42 2.0(9) . . . . ? N7 C38 C42 C41 2.1(8) . . . . ? C43 C38 C42 C41 -173.9(5) . . . . ? C40 C41 C42 C38 -3.1(8) . . . . ? N7 C38 C43 N5 22.4(6) . . . . ? C42 C38 C43 N5 -161.4(5) . . . . ? N6 C44 C45 C46 -2.1(12) . . . . ? C49 C44 C45 C46 178.8(7) . . . . ? C44 C45 C46 C47 0.5(14) . . . . ? C45 C46 C47 C48 -0.8(14) . . . . ? C46 C47 C48 N6 2.8(12) . . . . ? N6 C44 C49 N5 -5.7(8) . . . . ? C45 C44 C49 N5 173.5(6) . . . . ? O9 C50 C51 O8 -1.0(7) . . . . ? C59 C50 C51 O8 -179.2(5) . . . . ? O9 C50 C51 C52 179.9(5) . . . . ? C59 C50 C51 C52 1.7(8) . . . . ? O8 C51 C52 C53 -179.1(5) . . . . ? C50 C51 C52 C53 0.0(8) . . . . ? C51 C52 C53 C54 177.0(5) . . . . ? C51 C52 C53 C58 -1.3(8) . . . . ? C52 C53 C54 C55 179.1(5) . . . . ? C58 C53 C54 C55 -2.6(8) . . . . ? C53 C54 C55 C56 -0.8(9) . . . . ? C54 C55 C56 C57 2.0(10) . . . . ? C55 C56 C57 C58 0.4(9) . . . . ? C56 C57 C58 C59 178.5(6) . . . . ? C56 C57 C58 C53 -3.8(8) . . . . ? C52 C53 C58 C59 0.9(8) . . . . ? C54 C53 C58 C59 -177.4(5) . . . . ? C52 C53 C58 C57 -176.8(5) . . . . ? C54 C53 C58 C57 4.8(8) . . . . ? O9 C50 C59 C58 180.0(5) . . . . ? C51 C50 C59 C58 -2.0(8) . . . . ? C57 C58 C59 C50 178.4(5) . . . . ? C53 C58 C59 C50 0.7(8) . . . . ? C5 C1 N4 C2 1.0(8) . . . . ? C6 C1 N4 C2 178.9(5) . . . . ? C5 C1 N4 Co1 179.4(4) . . . . ? C6 C1 N4 Co1 -2.7(6) . . . . ? C3 C2 N4 C1 -2.7(8) . . . . ? C3 C2 N4 Co1 179.3(4) . . . . ? C9 C8 N2 C7 1.0(8) . . . . ? C9 C8 N2 Co1 -173.3(4) . . . . ? C12 C7 N2 C8 -1.2(8) . . . . ? C13 C7 N2 C8 175.3(5) . . . . ? C12 C7 N2 Co1 173.6(4) . . . . ? C13 C7 N2 Co1 -9.9(6) . . . . ? C18 C14 N3 C15 1.0(8) . . . . ? C19 C14 N3 C15 -173.8(5) . . . . ? C18 C14 N3 Co1 -178.2(4) . . . . ? C19 C14 N3 Co1 6.9(6) . . . . ? C16 C15 N3 C14 1.6(8) . . . . ? C16 C15 N3 Co1 -179.2(4) . . . . ? C1 C6 N1 C19 -161.0(4) . . . . ? C1 C6 N1 C13 73.1(5) . . . . ? C1 C6 N1 Co1 -44.8(5) . . . . ? C14 C19 N1 C6 144.2(5) . . . . ? C14 C19 N1 C13 -91.0(5) . . . . ? C14 C19 N1 Co1 29.6(5) . . . . ? C7 C13 N1 C6 -132.3(5) . . . . ? C7 C13 N1 C19 101.2(5) . . . . ? C7 C13 N1 Co1 -17.8(5) . . . . ? C36 C30 N8 C32 1.9(8) . . . . ? C37 C30 N8 C32 -174.8(5) . . . . ? C36 C30 N8 Co2 -177.8(4) . . . . ? C37 C30 N8 Co2 5.5(6) . . . . ? C33 C32 N8 C30 0.8(8) . . . . ? C33 C32 N8 Co2 -179.5(4) . . . . ? C40 C39 N7 C38 -1.2(8) . . . . ? C40 C39 N7 Co2 174.3(4) . . . . ? C42 C38 N7 C39 0.1(8) . . . . ? C43 C38 N7 C39 176.5(5) . . . . ? C42 C38 N7 Co2 -175.9(4) . . . . ? C43 C38 N7 Co2 0.4(6) . . . . ? C47 C48 N6 C44 -4.4(10) . . . . ? C47 C48 N6 Co2 174.5(5) . . . . ? C45 C44 N6 C48 4.1(9) . . . . ? C49 C44 N6 C48 -176.7(6) . . . . ? C45 C44 N6 Co2 -175.0(6) . . . . ? C49 C44 N6 Co2 4.2(7) . . . . ? C30 C37 N5 C43 155.3(4) . . . . ? C30 C37 N5 C49 -78.9(5) . . . . ? C30 C37 N5 Co2 40.2(5) . . . . ? C38 C43 N5 C37 -147.5(5) . . . . ? C38 C43 N5 C49 86.5(5) . . . . ? C38 C43 N5 Co2 -33.0(5) . . . . ? C44 C49 N5 C37 120.8(5) . . . . ? C44 C49 N5 C43 -112.9(5) . . . . ? C44 C49 N5 Co2 4.4(6) . . . . ? C29 C20 O2 Co1 176.2(4) . . . . ? C21 C20 O2 Co1 -4.9(6) . . . . ? C22 C21 O1 Co1 -178.6(5) . . . . ? C20 C21 O1 Co1 3.3(5) . . . . ? C59 C50 O9 Co2 177.0(4) . . . . ? C51 C50 O9 Co2 -1.1(6) . . . . ? C52 C51 O8 Co2 -178.3(5) . . . . ? C50 C51 O8 Co2 2.6(6) . . . . ? C21 O1 Co1 O2 -4.8(3) . . . . ? C21 O1 Co1 N2 173.6(3) . . . . ? C21 O1 Co1 N3 83.7(3) . . . . ? C21 O1 Co1 N4 -94.1(3) . . . . ? C21 O1 Co1 N1 -120(7) . . . . ? C20 O2 Co1 O1 5.4(3) . . . . ? C20 O2 Co1 N2 -120(6) . . . . ? C20 O2 Co1 N3 -89.8(3) . . . . ? C20 O2 Co1 N4 100.2(3) . . . . ? C20 O2 Co1 N1 -175.9(3) . . . . ? C8 N2 Co1 O1 -7.6(5) . . . . ? C7 N2 Co1 O1 177.9(4) . . . . ? C8 N2 Co1 O2 118(6) . . . . ? C7 N2 Co1 O2 -56(6) . . . . ? C8 N2 Co1 N3 87.5(5) . . . . ? C7 N2 Co1 N3 -87.0(4) . . . . ? C8 N2 Co1 N4 -102.5(5) . . . . ? C7 N2 Co1 N4 83.0(4) . . . . ? C8 N2 Co1 N1 173.7(5) . . . . ? C7 N2 Co1 N1 -0.8(4) . . . . ? C14 N3 Co1 O1 -171.6(4) . . . . ? C15 N3 Co1 O1 9.2(5) . . . . ? C14 N3 Co1 O2 -83.8(4) . . . . ? C15 N3 Co1 O2 97.0(5) . . . . ? C14 N3 Co1 N2 95.2(4) . . . . ? C15 N3 Co1 N2 -84.0(5) . . . . ? C14 N3 Co1 N4 -3.9(13) . . . . ? C15 N3 Co1 N4 176.9(9) . . . . ? C14 N3 Co1 N1 9.0(4) . . . . ? C15 N3 Co1 N1 -170.2(5) . . . . ? C1 N4 Co1 O1 160.9(3) . . . . ? C2 N4 Co1 O1 -20.9(4) . . . . ? C1 N4 Co1 O2 73.0(4) . . . . ? C2 N4 Co1 O2 -108.8(4) . . . . ? C1 N4 Co1 N2 -105.8(4) . . . . ? C2 N4 Co1 N2 72.4(4) . . . . ? C1 N4 Co1 N3 -6.9(13) . . . . ? C2 N4 Co1 N3 171.4(9) . . . . ? C1 N4 Co1 N1 -19.8(4) . . . . ? C2 N4 Co1 N1 158.4(5) . . . . ? C6 N1 Co1 O1 62(8) . . . . ? C19 N1 Co1 O1 -178(100) . . . . ? C13 N1 Co1 O1 -56(8) . . . . ? C6 N1 Co1 O2 -53.0(3) . . . . ? C19 N1 Co1 O2 67.1(4) . . . . ? C13 N1 Co1 O2 -170.9(3) . . . . ? C6 N1 Co1 N2 128.6(3) . . . . ? C19 N1 Co1 N2 -111.4(4) . . . . ? C13 N1 Co1 N2 10.6(4) . . . . ? C6 N1 Co1 N3 -141.5(3) . . . . ? C19 N1 Co1 N3 -21.5(4) . . . . ? C13 N1 Co1 N3 100.5(4) . . . . ? C6 N1 Co1 N4 36.2(3) . . . . ? C19 N1 Co1 N4 156.3(4) . . . . ? C13 N1 Co1 N4 -81.8(4) . . . . ? C51 O8 Co2 O9 -2.6(3) . . . . ? C51 O8 Co2 N7 -92.3(3) . . . . ? C51 O8 Co2 N6 176.4(3) . . . . ? C51 O8 Co2 N8 85.1(4) . . . . ? C51 O8 Co2 N5 169(71) . . . . ? C50 O9 Co2 O8 2.1(3) . . . . ? C50 O9 Co2 N7 97.0(3) . . . . ? C50 O9 Co2 N6 -133(7) . . . . ? C50 O9 Co2 N8 -93.3(4) . . . . ? C50 O9 Co2 N5 -177.8(3) . . . . ? C39 N7 Co2 O8 -11.5(5) . . . . ? C38 N7 Co2 O8 164.2(4) . . . . ? C39 N7 Co2 O9 -100.2(4) . . . . ? C38 N7 Co2 O9 75.6(4) . . . . ? C39 N7 Co2 N6 80.8(5) . . . . ? C38 N7 Co2 N6 -103.4(4) . . . . ? C39 N7 Co2 N8 -177.6(9) . . . . ? C38 N7 Co2 N8 -1.8(13) . . . . ? C39 N7 Co2 N5 167.7(5) . . . . ? C38 N7 Co2 N5 -16.5(4) . . . . ? C48 N6 Co2 O8 -0.1(5) . . . . ? C44 N6 Co2 O8 178.8(4) . . . . ? C48 N6 Co2 O9 135(7) . . . . ? C44 N6 Co2 O9 -46(8) . . . . ? C48 N6 Co2 N7 -95.1(5) . . . . ? C44 N6 Co2 N7 83.8(4) . . . . ? C48 N6 Co2 N8 95.2(5) . . . . ? C44 N6 Co2 N8 -85.8(4) . . . . ? C48 N6 Co2 N5 179.8(5) . . . . ? C44 N6 Co2 N5 -1.3(4) . . . . ? C30 N8 Co2 O8 -165.6(4) . . . . ? C32 N8 Co2 O8 14.7(5) . . . . ? C30 N8 Co2 O9 -77.1(4) . . . . ? C32 N8 Co2 O9 103.2(5) . . . . ? C30 N8 Co2 N7 0.4(13) . . . . ? C30 N8 Co2 N6 102.0(4) . . . . ? C32 N8 Co2 N6 -77.7(5) . . . . ? C30 N8 Co2 N5 15.2(4) . . . . ? C32 N8 Co2 N5 -164.5(5) . . . . ? C37 N5 Co2 O8 -115(15) . . . . ? C43 N5 Co2 O8 126(15) . . . . ? C49 N5 Co2 O8 5(15) . . . . ? C37 N5 Co2 O9 56.7(3) . . . . ? C43 N5 Co2 O9 -62.3(3) . . . . ? C49 N5 Co2 O9 177.2(4) . . . . ? C37 N5 Co2 N7 146.4(4) . . . . ? C43 N5 Co2 N7 27.3(3) . . . . ? C49 N5 Co2 N7 -93.2(4) . . . . ? C37 N5 Co2 N6 -122.3(4) . . . . ? C43 N5 Co2 N6 118.6(3) . . . . ? C49 N5 Co2 N6 -1.9(4) . . . . ? C37 N5 Co2 N8 -30.9(3) . . . . ? C43 N5 Co2 N8 -150.0(4) . . . . ? C49 N5 Co2 N8 89.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.744 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.107 data_11 _database_code_depnum_ccdc_archive 'CCDC 866275' #TrackingRef '- combined revised cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H29 Co N4 O2, 2(Cl O4)' _chemical_formula_sum 'C32 H29 Cl2 Co N4 O10' _chemical_formula_weight 759.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.836(5) _cell_length_b 17.758(7) _cell_length_c 14.707(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.636(7) _cell_angle_gamma 90.00 _cell_volume 3244(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 975 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 26.89 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.345 _exptl_crystal_size_mid 0.267 _exptl_crystal_size_min 0.198 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 0.759 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.737 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ; SADABS (Sheldrick, 1996) ; _diffrn_crystal_treatment ; attached with perfluoropolyether oil, to a short length of fibre supported on a thin piece of copper wire inserted in a copper mounting pin. The crystal was quenched in a cold nitrogen gas stream from an Oxford Cryosystems Cryostream. ; _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 SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 207 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.06 _diffrn_reflns_number 31644 _diffrn_reflns_av_R_equivalents 0.0813 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 28.08 _reflns_number_total 7718 _reflns_number_gt 5676 _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 ; xtal 3.6 (Hall,du Boulay, D.J. & Olthof-Hazekamp, R. 1999) ORTEPII (Johnson,C.K., 1976). WinGX (Farrugia, 1999) ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.03P)^2^+0.5P] 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 7718 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.0995 _refine_ls_wR_factor_gt 0.0944 _refine_ls_goodness_of_fit_ref 1.205 _refine_ls_restrained_S_all 1.205 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.44477(2) 0.223171(15) 0.692691(19) 0.02124(8) Uani 1 1 d . . . O1 O 0.42688(12) 0.29854(8) 0.77663(10) 0.0262(3) Uani 1 1 d . . . O2 O 0.48998(12) 0.14825(8) 0.78512(9) 0.0245(3) Uani 1 1 d . . . N1 N 0.45029(15) 0.15013(9) 0.59573(12) 0.0239(4) Uani 1 1 d . . . N2 N 0.41340(14) 0.29733(9) 0.59361(12) 0.0236(4) Uani 1 1 d . . . N3 N 0.59448(14) 0.24071(9) 0.70060(12) 0.0231(4) Uani 1 1 d . . . N4 N 0.29850(14) 0.18760(10) 0.67255(12) 0.0247(4) Uani 1 1 d . . . C1 C 0.4247(2) 0.36021(13) 0.91655(16) 0.0373(6) Uani 1 1 d . . . H1A H 0.4671 0.4032 0.9042 0.056 Uiso 1 1 calc R . . H1B H 0.4422 0.3503 0.9843 0.056 Uiso 1 1 calc R . . H1C H 0.3478 0.3717 0.8940 0.056 Uiso 1 1 calc R . . C2 C 0.45087(18) 0.29194(12) 0.86622(15) 0.0276(5) Uani 1 1 d . . . C3 C 0.4983(2) 0.22916(13) 0.91525(16) 0.0325(5) Uani 1 1 d . . . H3 H 0.5202 0.2326 0.9818 0.039 Uiso 1 1 calc R . . C4 C 0.51627(17) 0.16126(12) 0.87416(15) 0.0263(5) Uani 1 1 d . . . C5 C 0.57123(18) 0.09852(12) 0.93418(15) 0.0273(5) Uani 1 1 d . . . C6 C 0.57032(19) 0.09352(13) 1.03022(15) 0.0328(5) Uani 1 1 d . . . H6 H 0.5319 0.1299 1.0563 0.039 Uiso 1 1 calc R . . C7 C 0.6241(2) 0.03693(14) 1.08558(16) 0.0350(5) Uani 1 1 d . . . H7 H 0.6213 0.0337 1.1494 0.042 Uiso 1 1 calc R . . C8 C 0.68347(19) -0.01679(13) 1.04914(15) 0.0313(5) Uani 1 1 d . . . C9 C 0.7421(2) -0.07546(14) 1.10524(17) 0.0386(6) Uani 1 1 d . . . H9 H 0.7397 -0.0802 1.1690 0.046 Uiso 1 1 calc R . . C10 C 0.8016(2) -0.12479(14) 1.06875(17) 0.0400(6) Uani 1 1 d . . . H10 H 0.8408 -0.1635 1.1073 0.048 Uiso 1 1 calc R . . C11 C 0.8053(2) -0.11894(14) 0.97434(16) 0.0374(6) Uani 1 1 d . . . H11 H 0.8478 -0.1533 0.9497 0.045 Uiso 1 1 calc R . . C12 C 0.7483(2) -0.06424(13) 0.91775(16) 0.0327(5) Uani 1 1 d . . . H12 H 0.7508 -0.0613 0.8538 0.039 Uiso 1 1 calc R . . C13 C 0.68571(18) -0.01206(12) 0.95334(15) 0.0275(5) Uani 1 1 d . . . C14 C 0.62741(18) 0.04609(12) 0.89700(15) 0.0273(5) Uani 1 1 d . . . H14 H 0.6271 0.0489 0.8324 0.033 Uiso 1 1 calc R . . C15 C 0.40211(19) 0.18575(12) 0.50106(14) 0.0270(5) Uani 1 1 d . . . H15A H 0.4412 0.1679 0.4551 0.032 Uiso 1 1 calc R . . H15B H 0.3258 0.1703 0.4784 0.032 Uiso 1 1 calc R . . C16 C 0.40891(17) 0.26964(11) 0.50785(15) 0.0249(4) Uani 1 1 d . . . C17 C 0.4061(2) 0.31643(13) 0.43210(16) 0.0333(5) Uani 1 1 d . . . H17 H 0.4047 0.2960 0.3721 0.040 Uiso 1 1 calc R . . C18 C 0.4054(2) 0.39357(13) 0.44533(17) 0.0379(6) Uani 1 1 d . . . H18 H 0.4020 0.4268 0.3940 0.045 Uiso 1 1 calc R . . C19 C 0.40981(19) 0.42172(13) 0.53319(16) 0.0339(5) Uani 1 1 d . . . H19 H 0.4096 0.4746 0.5433 0.041 Uiso 1 1 calc R . . C20 C 0.41453(18) 0.37266(12) 0.60638(16) 0.0285(5) Uani 1 1 d . . . H20 H 0.4187 0.3922 0.6673 0.034 Uiso 1 1 calc R . . C21 C 0.56434(18) 0.12729(12) 0.60711(16) 0.0287(5) Uani 1 1 d . . . H21A H 0.5763 0.1141 0.5451 0.034 Uiso 1 1 calc R . . H21B H 0.5806 0.0824 0.6481 0.034 Uiso 1 1 calc R . . C22 C 0.63732(18) 0.19083(12) 0.64988(15) 0.0267(5) Uani 1 1 d . . . C23 C 0.74153(19) 0.19858(13) 0.64301(17) 0.0326(5) Uani 1 1 d . . . H23 H 0.7702 0.1648 0.6055 0.039 Uiso 1 1 calc R . . C24 C 0.80400(19) 0.25617(14) 0.69134(17) 0.0355(5) Uani 1 1 d . . . H24 H 0.8764 0.2620 0.6877 0.043 Uiso 1 1 calc R . . C25 C 0.76120(19) 0.30521(13) 0.74489(15) 0.0311(5) Uani 1 1 d . . . H25 H 0.8040 0.3443 0.7796 0.037 Uiso 1 1 calc R . . C26 C 0.65533(18) 0.29651(12) 0.74705(15) 0.0261(5) Uani 1 1 d . . . H26 H 0.6247 0.3310 0.7824 0.031 Uiso 1 1 calc R . . C27 C 0.38025(19) 0.08558(11) 0.60904(15) 0.0274(5) Uani 1 1 d . . . H27A H 0.3585 0.0555 0.5506 0.033 Uiso 1 1 calc R . . H27B H 0.4197 0.0524 0.6603 0.033 Uiso 1 1 calc R . . C28 C 0.28337(18) 0.11816(12) 0.63314(14) 0.0269(5) Uani 1 1 d . . . C29 C 0.18568(19) 0.08122(14) 0.61964(15) 0.0343(5) Uani 1 1 d . . . H29 H 0.1755 0.0329 0.5910 0.041 Uiso 1 1 calc R . . C30 C 0.1036(2) 0.11573(15) 0.64848(16) 0.0386(6) Uani 1 1 d . . . H30 H 0.0367 0.0906 0.6419 0.046 Uiso 1 1 calc R . . C31 C 0.1188(2) 0.18694(14) 0.68698(17) 0.0367(6) Uani 1 1 d . . . H31 H 0.0621 0.2116 0.7061 0.044 Uiso 1 1 calc R . . C32 C 0.21662(18) 0.22208(13) 0.69757(15) 0.0298(5) Uani 1 1 d . . . H32 H 0.2265 0.2715 0.7230 0.036 Uiso 1 1 calc R . . Cl1 Cl 0.57333(5) 0.12296(3) 0.32557(4) 0.03460(14) Uani 1 1 d . . . O3 O 0.6000(2) 0.18690(12) 0.38488(18) 0.0859(9) Uani 1 1 d . . . O4 O 0.5263(2) 0.14730(13) 0.23249(15) 0.0734(7) Uani 1 1 d . . . O5 O 0.49791(17) 0.07735(10) 0.35802(15) 0.0554(5) Uani 1 1 d . . . O6 O 0.66680(15) 0.07923(11) 0.32478(14) 0.0517(5) Uani 1 1 d . . . Cl2 Cl 0.66480(5) 0.49217(3) 0.84932(4) 0.03280(14) Uani 1 1 d . . . O7 O 0.56667(17) 0.47721(12) 0.78258(14) 0.0636(6) Uani 1 1 d . . . O8 O 0.7037(2) 0.42399(12) 0.89543(14) 0.0876(9) Uani 1 1 d . . . O9 O 0.7373(2) 0.52192(15) 0.80015(19) 0.0950(10) Uani 1 1 d . . . O10 O 0.64872(16) 0.54531(9) 0.91799(12) 0.0439(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.02242(15) 0.01539(14) 0.02478(15) -0.00262(11) 0.00388(11) 0.00071(11) O1 0.0287(8) 0.0195(7) 0.0295(8) -0.0051(6) 0.0058(6) 0.0027(6) O2 0.0289(8) 0.0188(7) 0.0245(7) -0.0013(6) 0.0044(6) 0.0020(6) N1 0.0292(10) 0.0162(8) 0.0257(9) -0.0013(7) 0.0057(7) -0.0004(7) N2 0.0233(9) 0.0186(9) 0.0266(9) -0.0018(7) 0.0022(7) 0.0006(7) N3 0.0230(9) 0.0186(9) 0.0258(9) 0.0006(7) 0.0028(7) 0.0021(7) N4 0.0259(10) 0.0220(9) 0.0250(9) 0.0006(7) 0.0041(7) -0.0017(8) C1 0.0417(14) 0.0327(13) 0.0353(13) -0.0113(10) 0.0057(11) 0.0112(11) C2 0.0242(11) 0.0285(12) 0.0299(12) -0.0089(9) 0.0062(9) 0.0000(9) C3 0.0384(13) 0.0313(13) 0.0261(11) -0.0038(9) 0.0051(10) 0.0080(11) C4 0.0237(11) 0.0267(12) 0.0285(11) -0.0008(9) 0.0068(9) -0.0014(9) C5 0.0271(12) 0.0248(11) 0.0289(11) 0.0004(9) 0.0047(9) 0.0001(9) C6 0.0364(13) 0.0329(13) 0.0302(12) -0.0009(10) 0.0106(10) 0.0050(10) C7 0.0397(14) 0.0409(14) 0.0250(11) 0.0038(10) 0.0091(10) 0.0048(11) C8 0.0314(12) 0.0309(12) 0.0306(12) 0.0020(9) 0.0060(10) -0.0001(10) C9 0.0431(15) 0.0399(14) 0.0304(12) 0.0086(10) 0.0049(11) 0.0030(12) C10 0.0452(15) 0.0325(13) 0.0375(13) 0.0090(11) 0.0016(11) 0.0093(12) C11 0.0412(14) 0.0308(13) 0.0360(13) -0.0028(10) 0.0018(11) 0.0073(11) C12 0.0401(14) 0.0283(12) 0.0268(11) -0.0011(9) 0.0031(10) 0.0045(10) C13 0.0281(12) 0.0255(11) 0.0269(11) -0.0007(9) 0.0033(9) -0.0013(9) C14 0.0323(12) 0.0259(11) 0.0230(10) -0.0003(8) 0.0055(9) -0.0023(9) C15 0.0328(12) 0.0227(11) 0.0242(11) -0.0023(8) 0.0048(9) -0.0014(9) C16 0.0223(11) 0.0217(11) 0.0287(11) -0.0001(8) 0.0029(9) -0.0014(9) C17 0.0401(14) 0.0287(12) 0.0284(12) 0.0005(9) 0.0039(10) -0.0033(10) C18 0.0449(15) 0.0271(13) 0.0388(13) 0.0077(10) 0.0054(11) -0.0019(11) C19 0.0333(13) 0.0204(11) 0.0438(14) 0.0028(10) 0.0022(11) 0.0028(10) C20 0.0270(12) 0.0221(11) 0.0339(12) -0.0021(9) 0.0029(9) 0.0033(9) C21 0.0303(12) 0.0211(11) 0.0350(12) -0.0041(9) 0.0091(10) 0.0053(9) C22 0.0287(12) 0.0211(11) 0.0298(11) 0.0019(9) 0.0067(9) 0.0047(9) C23 0.0299(13) 0.0284(12) 0.0409(13) 0.0012(10) 0.0117(10) 0.0081(10) C24 0.0230(12) 0.0347(13) 0.0473(14) 0.0077(11) 0.0062(11) 0.0011(10) C25 0.0307(13) 0.0253(12) 0.0328(12) 0.0034(9) -0.0004(10) -0.0037(10) C26 0.0281(12) 0.0194(11) 0.0279(11) -0.0003(8) 0.0020(9) -0.0008(9) C27 0.0365(13) 0.0160(10) 0.0283(11) -0.0028(8) 0.0054(9) -0.0061(9) C28 0.0315(12) 0.0224(11) 0.0245(11) 0.0012(8) 0.0028(9) -0.0036(9) C29 0.0357(14) 0.0303(13) 0.0321(12) 0.0023(10) -0.0006(10) -0.0114(11) C30 0.0283(13) 0.0467(15) 0.0367(13) 0.0082(11) 0.0009(10) -0.0102(11) C31 0.0274(13) 0.0420(15) 0.0393(13) 0.0067(11) 0.0062(10) 0.0025(11) C32 0.0276(12) 0.0289(12) 0.0320(12) 0.0021(9) 0.0061(9) 0.0038(10) Cl1 0.0419(3) 0.0243(3) 0.0421(3) 0.0007(2) 0.0189(3) 0.0021(2) O3 0.135(2) 0.0466(13) 0.0999(18) -0.0371(13) 0.0728(18) -0.0438(15) O4 0.0850(17) 0.0797(17) 0.0571(13) 0.0204(12) 0.0208(12) 0.0388(14) O5 0.0623(13) 0.0319(10) 0.0869(15) -0.0070(10) 0.0464(12) -0.0074(9) O6 0.0324(10) 0.0545(12) 0.0675(13) 0.0008(10) 0.0117(9) 0.0064(9) Cl2 0.0290(3) 0.0251(3) 0.0429(3) -0.0092(2) 0.0065(2) 0.0006(2) O7 0.0477(12) 0.0574(13) 0.0696(13) -0.0130(11) -0.0150(10) 0.0031(10) O8 0.135(2) 0.0467(13) 0.0529(12) -0.0147(10) -0.0291(13) 0.0530(14) O9 0.100(2) 0.100(2) 0.112(2) -0.0592(17) 0.0777(18) -0.0537(17) O10 0.0581(12) 0.0293(9) 0.0500(10) -0.0098(8) 0.0240(9) 0.0036(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 Co1 O1 1.8739(15) . ? Co1 O2 1.8857(15) . ? Co1 N3 1.9211(19) . ? Co1 N2 1.9296(18) . ? Co1 N4 1.9316(19) . ? Co1 N1 1.9421(17) . ? O1 C2 1.280(3) . ? O2 C4 1.288(2) . ? N1 C21 1.487(3) . ? N1 C27 1.500(3) . ? N1 C15 1.512(3) . ? N2 C16 1.341(3) . ? N2 C20 1.350(3) . ? N3 C26 1.338(3) . ? N3 C22 1.360(3) . ? N4 C32 1.346(3) . ? N4 C28 1.355(3) . ? C1 C2 1.502(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.382(3) . ? C3 C4 1.394(3) . ? C3 H3 0.9500 . ? C4 C5 1.484(3) . ? C5 C14 1.373(3) . ? C5 C6 1.418(3) . ? C6 C7 1.365(3) . ? C6 H6 0.9500 . ? C7 C8 1.409(3) . ? C7 H7 0.9500 . ? C8 C13 1.419(3) . ? C8 C9 1.421(3) . ? C9 C10 1.358(3) . ? C9 H9 0.9500 . ? C10 C11 1.405(3) . ? C10 H10 0.9500 . ? C11 C12 1.365(3) . ? C11 H11 0.9500 . ? C12 C13 1.411(3) . ? C12 H12 0.9500 . ? C13 C14 1.414(3) . ? C14 H14 0.9500 . ? C15 C16 1.494(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.383(3) . ? C17 C18 1.384(3) . ? C17 H17 0.9500 . ? C18 C19 1.373(3) . ? C18 H18 0.9500 . ? C19 C20 1.374(3) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.500(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.374(3) . ? C23 C24 1.381(3) . ? C23 H23 0.9500 . ? C24 C25 1.378(3) . ? C24 H24 0.9500 . ? C25 C26 1.376(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.493(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.384(3) . ? C29 C30 1.376(3) . ? C29 H29 0.9500 . ? C30 C31 1.379(4) . ? C30 H30 0.9500 . ? C31 C32 1.375(3) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? Cl1 O4 1.417(2) . ? Cl1 O3 1.420(2) . ? Cl1 O6 1.4316(19) . ? Cl1 O5 1.4333(18) . ? Cl2 O7 1.413(2) . ? Cl2 O8 1.416(2) . ? Cl2 O9 1.417(2) . ? Cl2 O10 1.4348(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O2 95.49(7) . . ? O1 Co1 N3 97.56(7) . . ? O2 Co1 N3 87.12(7) . . ? O1 Co1 N2 88.46(7) . . ? O2 Co1 N2 173.41(7) . . ? N3 Co1 N2 87.12(7) . . ? O1 Co1 N4 93.35(7) . . ? O2 Co1 N4 89.42(7) . . ? N3 Co1 N4 168.82(7) . . ? N2 Co1 N4 95.63(7) . . ? O1 Co1 N1 173.73(7) . . ? O2 Co1 N1 89.79(7) . . ? N3 Co1 N1 86.06(7) . . ? N2 Co1 N1 86.60(8) . . ? N4 Co1 N1 83.30(8) . . ? C2 O1 Co1 125.09(14) . . ? C4 O2 Co1 124.07(14) . . ? C21 N1 C27 112.48(17) . . ? C21 N1 C15 112.31(16) . . ? C27 N1 C15 108.70(16) . . ? C21 N1 Co1 108.49(13) . . ? C27 N1 Co1 106.28(12) . . ? C15 N1 Co1 108.32(12) . . ? C16 N2 C20 119.36(18) . . ? C16 N2 Co1 114.27(14) . . ? C20 N2 Co1 125.33(15) . . ? C26 N3 C22 119.85(19) . . ? C26 N3 Co1 126.66(15) . . ? C22 N3 Co1 113.45(14) . . ? C32 N4 C28 119.58(19) . . ? C32 N4 Co1 127.26(15) . . ? C28 N4 Co1 113.06(15) . . ? 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 124.78(19) . . ? O1 C2 C1 114.1(2) . . ? C3 C2 C1 121.2(2) . . ? C2 C3 C4 124.8(2) . . ? C2 C3 H3 117.6 . . ? C4 C3 H3 117.6 . . ? O2 C4 C3 124.5(2) . . ? O2 C4 C5 115.65(18) . . ? C3 C4 C5 119.83(19) . . ? C14 C5 C6 119.4(2) . . ? C14 C5 C4 119.39(19) . . ? C6 C5 C4 121.1(2) . . ? C7 C6 C5 120.7(2) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C6 C7 C8 120.8(2) . . ? C6 C7 H7 119.6 . . ? C8 C7 H7 119.6 . . ? C7 C8 C13 119.1(2) . . ? C7 C8 C9 122.3(2) . . ? C13 C8 C9 118.6(2) . . ? C10 C9 C8 120.8(2) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C9 C10 C11 120.4(2) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C12 C11 C10 120.6(2) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C13 120.6(2) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C12 C13 C14 121.9(2) . . ? C12 C13 C8 119.1(2) . . ? C14 C13 C8 119.0(2) . . ? C5 C14 C13 121.02(19) . . ? C5 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C16 C15 N1 110.62(16) . . ? C16 C15 H15A 109.5 . . ? N1 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? N1 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? N2 C16 C17 121.57(19) . . ? N2 C16 C15 114.60(18) . . ? C17 C16 C15 123.77(19) . . ? C16 C17 C18 118.8(2) . . ? C16 C17 H17 120.6 . . ? C18 C17 H17 120.6 . . ? C19 C18 C17 119.5(2) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 119.3(2) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? N2 C20 C19 121.5(2) . . ? N2 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? N1 C21 C22 109.56(17) . . ? N1 C21 H21A 109.8 . . ? C22 C21 H21A 109.8 . . ? N1 C21 H21B 109.8 . . ? C22 C21 H21B 109.8 . . ? H21A C21 H21B 108.2 . . ? N3 C22 C23 120.7(2) . . ? N3 C22 C21 115.07(19) . . ? C23 C22 C21 124.15(19) . . ? C22 C23 C24 119.1(2) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C25 C24 C23 119.9(2) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C26 C25 C24 118.7(2) . . ? C26 C25 H25 120.6 . . ? C24 C25 H25 120.6 . . ? N3 C26 C25 121.6(2) . . ? N3 C26 H26 119.2 . . ? C25 C26 H26 119.2 . . ? C28 C27 N1 107.30(17) . . ? C28 C27 H27A 110.3 . . ? N1 C27 H27A 110.3 . . ? C28 C27 H27B 110.3 . . ? N1 C27 H27B 110.3 . . ? H27A C27 H27B 108.5 . . ? N4 C28 C29 121.3(2) . . ? N4 C28 C27 114.59(19) . . ? C29 C28 C27 124.1(2) . . ? C30 C29 C28 118.8(2) . . ? C30 C29 H29 120.6 . . ? C28 C29 H29 120.6 . . ? C29 C30 C31 119.6(2) . . ? C29 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? C32 C31 C30 119.6(2) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? N4 C32 C31 121.1(2) . . ? N4 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? O4 Cl1 O3 109.10(16) . . ? O4 Cl1 O6 108.12(12) . . ? O3 Cl1 O6 111.49(16) . . ? O4 Cl1 O5 109.59(15) . . ? O3 Cl1 O5 108.99(12) . . ? O6 Cl1 O5 109.52(12) . . ? O7 Cl2 O8 108.45(15) . . ? O7 Cl2 O9 107.51(16) . . ? O8 Cl2 O9 111.45(19) . . ? O7 Cl2 O10 110.56(13) . . ? O8 Cl2 O10 108.74(12) . . ? O9 Cl2 O10 110.11(12) . . ? 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 O2 Co1 O1 C2 4.90(17) . . . . ? N3 Co1 O1 C2 -82.92(17) . . . . ? N2 Co1 O1 C2 -169.81(17) . . . . ? N4 Co1 O1 C2 94.64(17) . . . . ? O1 Co1 O2 C4 -11.74(17) . . . . ? N3 Co1 O2 C4 85.59(16) . . . . ? N4 Co1 O2 C4 -105.05(16) . . . . ? N1 Co1 O2 C4 171.65(16) . . . . ? O2 Co1 N1 C21 -65.90(14) . . . . ? N3 Co1 N1 C21 21.23(14) . . . . ? N2 Co1 N1 C21 108.57(14) . . . . ? N4 Co1 N1 C21 -155.35(14) . . . . ? O2 Co1 N1 C27 55.27(14) . . . . ? N3 Co1 N1 C27 142.40(14) . . . . ? N2 Co1 N1 C27 -130.25(14) . . . . ? N4 Co1 N1 C27 -34.17(13) . . . . ? O2 Co1 N1 C15 171.93(13) . . . . ? N3 Co1 N1 C15 -100.94(14) . . . . ? N2 Co1 N1 C15 -13.60(14) . . . . ? N4 Co1 N1 C15 82.48(14) . . . . ? O1 Co1 N2 C16 -176.02(15) . . . . ? N3 Co1 N2 C16 86.33(15) . . . . ? N4 Co1 N2 C16 -82.81(15) . . . . ? N1 Co1 N2 C16 0.11(15) . . . . ? O1 Co1 N2 C20 15.80(18) . . . . ? N3 Co1 N2 C20 -81.85(18) . . . . ? N4 Co1 N2 C20 109.01(18) . . . . ? N1 Co1 N2 C20 -168.07(19) . . . . ? O1 Co1 N3 C26 -5.69(18) . . . . ? O2 Co1 N3 C26 -100.85(17) . . . . ? N2 Co1 N3 C26 82.37(18) . . . . ? N4 Co1 N3 C26 -173.0(3) . . . . ? N1 Co1 N3 C26 169.16(18) . . . . ? O1 Co1 N3 C22 176.52(14) . . . . ? O2 Co1 N3 C22 81.36(15) . . . . ? N2 Co1 N3 C22 -95.42(15) . . . . ? N4 Co1 N3 C22 9.2(4) . . . . ? N1 Co1 N3 C22 -8.63(14) . . . . ? O1 Co1 N4 C32 12.80(18) . . . . ? O2 Co1 N4 C32 108.26(18) . . . . ? N3 Co1 N4 C32 -179.8(3) . . . . ? N2 Co1 N4 C32 -75.98(18) . . . . ? N1 Co1 N4 C32 -161.88(18) . . . . ? O1 Co1 N4 C28 -163.45(14) . . . . ? O2 Co1 N4 C28 -67.99(15) . . . . ? N3 Co1 N4 C28 4.0(4) . . . . ? N2 Co1 N4 C28 107.77(15) . . . . ? N1 Co1 N4 C28 21.87(14) . . . . ? Co1 O1 C2 C3 3.0(3) . . . . ? Co1 O1 C2 C1 -177.99(15) . . . . ? O1 C2 C3 C4 -7.2(4) . . . . ? C1 C2 C3 C4 173.9(2) . . . . ? Co1 O2 C4 C3 11.2(3) . . . . ? Co1 O2 C4 C5 -167.54(14) . . . . ? C2 C3 C4 O2 -0.7(4) . . . . ? C2 C3 C4 C5 178.0(2) . . . . ? O2 C4 C5 C14 25.3(3) . . . . ? C3 C4 C5 C14 -153.5(2) . . . . ? O2 C4 C5 C6 -157.2(2) . . . . ? C3 C4 C5 C6 23.9(3) . . . . ? C14 C5 C6 C7 -0.4(3) . . . . ? C4 C5 C6 C7 -177.9(2) . . . . ? C5 C6 C7 C8 1.4(4) . . . . ? C6 C7 C8 C13 -0.9(4) . . . . ? C6 C7 C8 C9 178.7(2) . . . . ? C7 C8 C9 C10 -177.7(2) . . . . ? C13 C8 C9 C10 1.8(4) . . . . ? C8 C9 C10 C11 -0.5(4) . . . . ? C9 C10 C11 C12 -0.8(4) . . . . ? C10 C11 C12 C13 0.8(4) . . . . ? C11 C12 C13 C14 178.8(2) . . . . ? C11 C12 C13 C8 0.5(4) . . . . ? C7 C8 C13 C12 177.8(2) . . . . ? C9 C8 C13 C12 -1.8(3) . . . . ? C7 C8 C13 C14 -0.5(3) . . . . ? C9 C8 C13 C14 179.9(2) . . . . ? C6 C5 C14 C13 -1.0(3) . . . . ? C4 C5 C14 C13 176.5(2) . . . . ? C12 C13 C14 C5 -176.8(2) . . . . ? C8 C13 C14 C5 1.5(3) . . . . ? C21 N1 C15 C16 -96.1(2) . . . . ? C27 N1 C15 C16 138.82(18) . . . . ? Co1 N1 C15 C16 23.7(2) . . . . ? C20 N2 C16 C17 0.4(3) . . . . ? Co1 N2 C16 C17 -168.50(18) . . . . ? C20 N2 C16 C15 -176.9(2) . . . . ? Co1 N2 C16 C15 14.2(2) . . . . ? N1 C15 C16 N2 -25.3(3) . . . . ? N1 C15 C16 C17 157.5(2) . . . . ? N2 C16 C17 C18 -1.5(4) . . . . ? C15 C16 C17 C18 175.5(2) . . . . ? C16 C17 C18 C19 1.4(4) . . . . ? C17 C18 C19 C20 -0.1(4) . . . . ? C16 N2 C20 C19 0.8(3) . . . . ? Co1 N2 C20 C19 168.47(17) . . . . ? C18 C19 C20 N2 -1.0(4) . . . . ? C27 N1 C21 C22 -146.24(17) . . . . ? C15 N1 C21 C22 90.7(2) . . . . ? Co1 N1 C21 C22 -29.0(2) . . . . ? C26 N3 C22 C23 -2.3(3) . . . . ? Co1 N3 C22 C23 175.64(17) . . . . ? C26 N3 C22 C21 175.40(18) . . . . ? Co1 N3 C22 C21 -6.6(2) . . . . ? N1 C21 C22 N3 23.9(3) . . . . ? N1 C21 C22 C23 -158.5(2) . . . . ? N3 C22 C23 C24 2.5(3) . . . . ? C21 C22 C23 C24 -175.0(2) . . . . ? C22 C23 C24 C25 -0.5(3) . . . . ? C23 C24 C25 C26 -1.5(3) . . . . ? C22 N3 C26 C25 0.2(3) . . . . ? Co1 N3 C26 C25 -177.49(15) . . . . ? C24 C25 C26 N3 1.8(3) . . . . ? C21 N1 C27 C28 158.43(17) . . . . ? C15 N1 C27 C28 -76.55(19) . . . . ? Co1 N1 C27 C28 39.85(18) . . . . ? C32 N4 C28 C29 -1.2(3) . . . . ? Co1 N4 C28 C29 175.33(16) . . . . ? C32 N4 C28 C27 -179.61(18) . . . . ? Co1 N4 C28 C27 -3.0(2) . . . . ? N1 C27 C28 N4 -24.6(2) . . . . ? N1 C27 C28 C29 157.0(2) . . . . ? N4 C28 C29 C30 -1.1(3) . . . . ? C27 C28 C29 C30 177.2(2) . . . . ? C28 C29 C30 C31 2.2(3) . . . . ? C29 C30 C31 C32 -1.1(4) . . . . ? C28 N4 C32 C31 2.4(3) . . . . ? Co1 N4 C32 C31 -173.65(16) . . . . ? C30 C31 C32 N4 -1.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.663 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.076 data_12 _database_code_depnum_ccdc_archive 'CCDC 866276' #TrackingRef '- combined revised cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H25 Co N4 O2, 2(Cl O4), H2 O' _chemical_formula_sum 'C23 H27 Cl2 Co N4 O11' _chemical_formula_weight 665.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' _Int_tables_symmetry_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.9070(8) _cell_length_b 8.9780(4) _cell_length_c 19.1400(9) _cell_angle_alpha 90.00 _cell_angle_beta 97.115(3) _cell_angle_gamma 90.00 _cell_volume 2712.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 8039 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 29.50 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 0.897 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6640 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2007)' _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 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type APEXII-FR591 _diffrn_measurement_method \w+\f _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 30220 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0510 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 30.05 _reflns_number_total 7922 _reflns_number_gt 6203 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX (Bruker-Nonius, 2003)' _computing_cell_refinement 'SAINT (Bruker-Nonius, 2003)' _computing_data_reduction 'SAINT (Bruker-Nonius, 2003), XPREP (Bruker-Nonius, 2003)' _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) POV-Ray 3.5 (Cason, 2002) WebLab ViewerPro 3.7 (Molecular Simulations, 2000) ; _computing_publication_material 'enCIFer 1.1 (CCDC, 2005)' _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^)+(0.0541P)^2^+2.6309P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7922 _refine_ls_number_parameters 378 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0593 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1189 _refine_ls_wR_factor_gt 0.1074 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 0.56445(14) 0.3327(2) 1.02729(11) 0.0180(4) Uani 1 1 d . . . H1A H 0.5649 0.4143 1.0613 0.027 Uiso 1 1 calc R . . H1B H 0.5602 0.2374 1.0515 0.027 Uiso 1 1 calc R . . H1C H 0.5158 0.3442 0.9910 0.027 Uiso 1 1 calc R . . C2 C 0.64495(13) 0.3362(2) 0.99358(10) 0.0131(4) Uani 1 1 d . . . C3 C 0.69669(14) 0.2114(2) 0.99603(11) 0.0159(4) Uani 1 1 d . . . H3 H 0.6806 0.1264 1.0208 0.019 Uiso 1 1 calc R . . C4 C 0.77127(13) 0.2033(2) 0.96424(10) 0.0146(4) Uani 1 1 d . . . C5 C 0.82793(15) 0.0690(2) 0.97811(12) 0.0214(4) Uani 1 1 d . . . H5A H 0.8505 0.0404 0.9346 0.032 Uiso 1 1 calc R . . H5B H 0.7952 -0.0139 0.9942 0.032 Uiso 1 1 calc R . . H5C H 0.8749 0.0933 1.0144 0.032 Uiso 1 1 calc R . . C6 C 0.71373(14) 0.3546(2) 0.77074(11) 0.0175(4) Uani 1 1 d . . . C7 C 0.67319(17) 0.2817(3) 0.71172(12) 0.0261(5) Uani 1 1 d . . . H7 H 0.7039 0.2502 0.6748 0.031 Uiso 1 1 calc R . . C8 C 0.58644(19) 0.2560(3) 0.70816(12) 0.0328(6) Uani 1 1 d . . . H8 H 0.5578 0.2036 0.6692 0.039 Uiso 1 1 calc R . . C9 C 0.54158(16) 0.3066(3) 0.76118(12) 0.0258(5) Uani 1 1 d . . . H9 H 0.4820 0.2931 0.7580 0.031 Uiso 1 1 calc R . . C10 C 0.58558(14) 0.3772(2) 0.81893(11) 0.0185(4) Uani 1 1 d . . . H10 H 0.5556 0.4117 0.8557 0.022 Uiso 1 1 calc R . . C11 C 0.80679(14) 0.3910(2) 0.78199(11) 0.0189(4) Uani 1 1 d . . . H11A H 0.8395 0.3043 0.8025 0.023 Uiso 1 1 calc R . . H11B H 0.8270 0.4165 0.7366 0.023 Uiso 1 1 calc R . . C12 C 0.73326(13) 0.7537(2) 0.82766(10) 0.0153(4) Uani 1 1 d . . . C13 C 0.71229(16) 0.9000(2) 0.80875(12) 0.0217(5) Uani 1 1 d . . . H13 H 0.7383 0.9486 0.7729 0.026 Uiso 1 1 calc R . . C14 C 0.65281(17) 0.9737(2) 0.84323(13) 0.0238(5) Uani 1 1 d . . . H14 H 0.6374 1.0734 0.8310 0.029 Uiso 1 1 calc R . . C15 C 0.61560(15) 0.9007(2) 0.89607(12) 0.0198(4) Uani 1 1 d . . . H15 H 0.5745 0.9496 0.9199 0.024 Uiso 1 1 calc R . . C16 C 0.63967(13) 0.7561(2) 0.91298(11) 0.0159(4) Uani 1 1 d . . . H16 H 0.6157 0.7063 0.9496 0.019 Uiso 1 1 calc R . . C17 C 0.79429(14) 0.6634(2) 0.79154(11) 0.0170(4) Uani 1 1 d . . . H17A H 0.8459 0.7229 0.7878 0.020 Uiso 1 1 calc R . . H17B H 0.7682 0.6386 0.7433 0.020 Uiso 1 1 calc R . . C18 C 0.90031(13) 0.6018(2) 0.94146(11) 0.0160(4) Uani 1 1 d . . . C19 C 0.96644(14) 0.6796(3) 0.97937(12) 0.0209(4) Uani 1 1 d . . . H19 H 1.0185 0.6932 0.9607 0.025 Uiso 1 1 calc R . . C20 C 0.95524(15) 0.7371(3) 1.04504(12) 0.0216(4) Uani 1 1 d . . . H20 H 0.9994 0.7917 1.0715 0.026 Uiso 1 1 calc R . . C21 C 0.87882(15) 0.7140(2) 1.07169(11) 0.0198(4) Uani 1 1 d . . . H21 H 0.8707 0.7511 1.1169 0.024 Uiso 1 1 calc R . . C22 C 0.81446(14) 0.6361(2) 1.03156(11) 0.0164(4) Uani 1 1 d . . . H22 H 0.7619 0.6211 1.0493 0.020 Uiso 1 1 calc R . . C23 C 0.90556(14) 0.5292(3) 0.87100(11) 0.0185(4) Uani 1 1 d . . . H23A H 0.9430 0.5881 0.8439 0.022 Uiso 1 1 calc R . . H23B H 0.9295 0.4277 0.8779 0.022 Uiso 1 1 calc R . . N4 N 0.67009(11) 0.39793(19) 0.82400(9) 0.0146(3) Uani 1 1 d . . . N2 N 0.69687(11) 0.68382(19) 0.87832(9) 0.0131(3) Uani 1 1 d . . . N3 N 0.82576(11) 0.58149(19) 0.96774(9) 0.0139(3) Uani 1 1 d . . . N1 N 0.81817(11) 0.52153(19) 0.83153(9) 0.0137(3) Uani 1 1 d . . . O1 O 0.65895(9) 0.46101(16) 0.96357(8) 0.0146(3) Uani 1 1 d . . . O2 O 0.79676(9) 0.30254(16) 0.92341(8) 0.0153(3) Uani 1 1 d . . . O3 O 0.61211(12) 0.6291(2) 0.69139(9) 0.0310(4) Uani 1 1 d . . . O4 O 0.71238(11) 0.6167(2) 0.61135(10) 0.0317(4) Uani 1 1 d . . . O5 O 0.56821(12) 0.5736(2) 0.57200(10) 0.0352(4) Uani 1 1 d . . . O6 O 0.61414(14) 0.8163(2) 0.60481(11) 0.0375(5) Uani 1 1 d . . . O7 O 0.97985(19) 0.8653(3) 0.84220(13) 0.0601(7) Uani 1 1 d . . . O8 O 1.04687(14) 1.0601(3) 0.78899(11) 0.0495(6) Uani 1 1 d . . . O9 O 0.91236(15) 1.0930(3) 0.82404(12) 0.0551(7) Uani 1 1 d . . . O10 O 0.92740(16) 0.9411(2) 0.72754(10) 0.0453(6) Uani 1 1 d . . . O1W O 0.86182(16) 1.1913(3) 0.63183(12) 0.0469(6) Uani 1 1 d D . . H1O H 0.874(3) 1.120(3) 0.6622(17) 0.070 Uiso 1 1 d D . . H2O H 0.898(2) 1.263(3) 0.641(2) 0.070 Uiso 1 1 d D . . Cl1 Cl 0.62638(3) 0.65904(6) 0.61970(3) 0.01768(11) Uani 1 1 d . . . Cl2 Cl 0.96626(4) 0.99074(6) 0.79497(3) 0.01947(12) Uani 1 1 d . . . Co1 Co 0.741132(17) 0.48743(3) 0.901687(13) 0.01085(8) 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 0.0195(10) 0.0182(10) 0.0177(9) 0.0021(8) 0.0079(8) -0.0007(8) C2 0.0148(9) 0.0139(9) 0.0101(8) -0.0011(7) 0.0001(7) -0.0033(7) C3 0.0195(10) 0.0114(9) 0.0169(9) 0.0034(7) 0.0023(7) -0.0010(7) C4 0.0168(10) 0.0115(9) 0.0149(9) 0.0006(7) -0.0008(7) 0.0015(7) C5 0.0215(11) 0.0152(10) 0.0276(11) 0.0052(8) 0.0034(9) 0.0055(8) C6 0.0231(11) 0.0151(10) 0.0149(9) 0.0026(7) 0.0043(8) -0.0021(8) C7 0.0388(14) 0.0261(12) 0.0135(10) -0.0001(9) 0.0034(9) -0.0096(10) C8 0.0423(15) 0.0396(15) 0.0148(10) 0.0034(10) -0.0031(10) -0.0210(12) C9 0.0230(12) 0.0313(13) 0.0213(11) 0.0102(9) -0.0046(9) -0.0115(10) C10 0.0174(10) 0.0177(10) 0.0197(10) 0.0074(8) -0.0001(8) -0.0031(8) C11 0.0215(11) 0.0198(10) 0.0166(9) -0.0030(8) 0.0074(8) 0.0005(8) C12 0.0146(9) 0.0156(10) 0.0152(9) 0.0015(7) -0.0003(7) -0.0031(7) C13 0.0295(12) 0.0153(10) 0.0202(10) 0.0038(8) 0.0024(9) -0.0035(9) C14 0.0345(13) 0.0112(10) 0.0248(11) 0.0028(8) -0.0007(9) 0.0030(9) C15 0.0207(11) 0.0128(10) 0.0253(11) -0.0029(8) 0.0003(8) 0.0032(8) C16 0.0149(10) 0.0124(9) 0.0203(10) -0.0002(7) 0.0023(7) 0.0004(7) C17 0.0160(10) 0.0199(10) 0.0153(9) 0.0051(8) 0.0029(7) -0.0012(8) C18 0.0128(9) 0.0186(10) 0.0162(9) 0.0040(7) 0.0000(7) 0.0012(8) C19 0.0142(10) 0.0248(11) 0.0225(10) 0.0048(9) -0.0020(8) -0.0016(8) C20 0.0206(11) 0.0192(11) 0.0226(10) 0.0021(8) -0.0074(8) -0.0006(9) C21 0.0248(11) 0.0157(10) 0.0175(10) 0.0004(8) -0.0025(8) 0.0029(8) C22 0.0186(10) 0.0139(9) 0.0165(9) 0.0010(7) 0.0021(7) 0.0021(8) C23 0.0117(9) 0.0283(11) 0.0156(9) 0.0012(8) 0.0026(7) 0.0023(8) N4 0.0170(8) 0.0116(8) 0.0149(8) 0.0028(6) 0.0012(6) 0.0001(6) N2 0.0121(8) 0.0110(8) 0.0157(8) 0.0015(6) -0.0004(6) 0.0009(6) N3 0.0145(8) 0.0137(8) 0.0134(7) 0.0026(6) 0.0011(6) 0.0026(6) N1 0.0125(8) 0.0154(8) 0.0134(7) 0.0002(6) 0.0030(6) 0.0002(6) O1 0.0154(7) 0.0121(7) 0.0173(7) 0.0012(5) 0.0061(5) 0.0005(5) O2 0.0157(7) 0.0134(7) 0.0173(7) 0.0017(5) 0.0039(5) 0.0031(6) O3 0.0338(10) 0.0397(11) 0.0215(8) 0.0080(7) 0.0107(7) 0.0142(8) O4 0.0202(9) 0.0382(11) 0.0388(10) -0.0006(8) 0.0118(7) -0.0015(8) O5 0.0305(10) 0.0357(11) 0.0370(10) -0.0081(8) -0.0052(8) -0.0107(8) O6 0.0450(12) 0.0174(9) 0.0468(12) 0.0104(8) -0.0074(9) -0.0001(8) O7 0.090(2) 0.0405(13) 0.0458(13) 0.0221(11) -0.0095(13) -0.0153(13) O8 0.0387(13) 0.0731(16) 0.0395(12) -0.0098(11) 0.0166(10) -0.0233(12) O9 0.0460(14) 0.0738(18) 0.0454(13) -0.0166(12) 0.0058(10) 0.0311(13) O10 0.0707(16) 0.0364(11) 0.0270(10) -0.0064(9) -0.0017(10) -0.0177(11) O1W 0.0478(14) 0.0490(14) 0.0411(12) -0.0006(10) -0.0056(10) 0.0071(11) Cl1 0.0181(2) 0.0166(2) 0.0184(2) 0.00182(18) 0.00257(18) -0.00128(18) Cl2 0.0232(3) 0.0166(2) 0.0201(2) -0.00080(18) 0.00830(19) -0.00128(19) Co1 0.01041(13) 0.01042(13) 0.01199(13) 0.00136(9) 0.00245(9) 0.00095(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.504(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 O1 1.291(2) . ? C2 C3 1.387(3) . ? C3 C4 1.401(3) . ? C3 H3 0.9500 . ? C4 O2 1.284(2) . ? C4 C5 1.509(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 N4 1.359(3) . ? C6 C7 1.393(3) . ? C6 C11 1.505(3) . ? C7 C8 1.392(4) . ? C7 H7 0.9500 . ? C8 C9 1.387(4) . ? C8 H8 0.9500 . ? C9 C10 1.386(3) . ? C9 H9 0.9500 . ? C10 N4 1.349(3) . ? C10 H10 0.9500 . ? C11 N1 1.504(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N2 1.345(3) . ? C12 C13 1.392(3) . ? C12 C17 1.498(3) . ? C13 C14 1.387(3) . ? C13 H13 0.9500 . ? C14 C15 1.397(3) . ? C14 H14 0.9500 . ? C15 C16 1.380(3) . ? C15 H15 0.9500 . ? C16 N2 1.356(3) . ? C16 H16 0.9500 . ? C17 N1 1.510(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 N3 1.356(3) . ? C18 C19 1.390(3) . ? C18 C23 1.509(3) . ? C19 C20 1.391(3) . ? C19 H19 0.9500 . ? C20 C21 1.391(3) . ? C20 H20 0.9500 . ? C21 C22 1.390(3) . ? C21 H21 0.9500 . ? C22 N3 1.349(3) . ? C22 H22 0.9500 . ? C23 N1 1.499(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? N4 Co1 1.9281(18) . ? N2 Co1 1.9304(17) . ? N3 Co1 1.9240(18) . ? N1 Co1 1.9510(17) . ? O1 Co1 1.8847(14) . ? O2 Co1 1.9027(14) . ? O3 Cl1 1.4434(17) . ? O4 Cl1 1.4476(18) . ? O5 Cl1 1.4386(18) . ? O6 Cl1 1.4488(18) . ? O7 Cl2 1.444(2) . ? O8 Cl2 1.442(2) . ? O9 Cl2 1.416(2) . ? O10 Cl2 1.431(2) . ? O1W H1O 0.87(3) . ? O1W H2O 0.87(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag 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 125.56(19) . . ? O1 C2 C1 114.30(18) . . ? C3 C2 C1 120.14(18) . . ? C2 C3 C4 123.94(19) . . ? C2 C3 H3 118.0 . . ? C4 C3 H3 118.0 . . ? O2 C4 C3 125.23(19) . . ? O2 C4 C5 115.77(19) . . ? C3 C4 C5 119.00(19) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N4 C6 C7 121.0(2) . . ? N4 C6 C11 114.52(18) . . ? C7 C6 C11 124.5(2) . . ? C6 C7 C8 118.3(2) . . ? C6 C7 H7 120.9 . . ? C8 C7 H7 120.9 . . ? C9 C8 C7 120.4(2) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C10 C9 C8 118.6(2) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? N4 C10 C9 121.4(2) . . ? N4 C10 H10 119.3 . . ? C9 C10 H10 119.3 . . ? N1 C11 C6 107.39(17) . . ? N1 C11 H11A 110.2 . . ? C6 C11 H11A 110.2 . . ? N1 C11 H11B 110.2 . . ? C6 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? N2 C12 C13 121.1(2) . . ? N2 C12 C17 116.21(18) . . ? C13 C12 C17 122.61(19) . . ? C14 C13 C12 118.8(2) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C13 C14 C15 119.7(2) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 118.7(2) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? N2 C16 C15 121.3(2) . . ? N2 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C12 C17 N1 111.07(16) . . ? C12 C17 H17A 109.4 . . ? N1 C17 H17A 109.4 . . ? C12 C17 H17B 109.4 . . ? N1 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? N3 C18 C19 120.9(2) . . ? N3 C18 C23 114.90(18) . . ? C19 C18 C23 124.1(2) . . ? C18 C19 C20 119.0(2) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C21 C20 C19 119.5(2) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C22 C21 C20 119.3(2) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? N3 C22 C21 120.8(2) . . ? N3 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? N1 C23 C18 108.64(17) . . ? N1 C23 H23A 110.0 . . ? C18 C23 H23A 110.0 . . ? N1 C23 H23B 110.0 . . ? C18 C23 H23B 110.0 . . ? H23A C23 H23B 108.3 . . ? C10 N4 C6 120.24(19) . . ? C10 N4 Co1 126.64(15) . . ? C6 N4 Co1 113.12(14) . . ? C12 N2 C16 120.27(18) . . ? C12 N2 Co1 114.59(14) . . ? C16 N2 Co1 124.86(14) . . ? C22 N3 C18 120.51(19) . . ? C22 N3 Co1 126.42(15) . . ? C18 N3 Co1 112.83(14) . . ? C23 N1 C11 112.66(17) . . ? C23 N1 C17 112.07(17) . . ? C11 N1 C17 109.55(16) . . ? C23 N1 Co1 106.42(12) . . ? C11 N1 Co1 105.95(13) . . ? C17 N1 Co1 109.94(12) . . ? C2 O1 Co1 124.06(13) . . ? C4 O2 Co1 124.41(13) . . ? H1O O1W H2O 109(4) . . ? O5 Cl1 O3 109.84(12) . . ? O5 Cl1 O4 109.40(12) . . ? O3 Cl1 O4 108.55(11) . . ? O5 Cl1 O6 109.56(12) . . ? O3 Cl1 O6 109.60(12) . . ? O4 Cl1 O6 109.88(12) . . ? O9 Cl2 O10 109.95(15) . . ? O9 Cl2 O8 109.81(16) . . ? O10 Cl2 O8 110.59(13) . . ? O9 Cl2 O7 108.10(17) . . ? O10 Cl2 O7 109.64(14) . . ? O8 Cl2 O7 108.70(16) . . ? O1 Co1 O2 95.33(6) . . ? O1 Co1 N3 97.22(7) . . ? O2 Co1 N3 88.32(7) . . ? O1 Co1 N4 92.65(7) . . ? O2 Co1 N4 90.99(7) . . ? N3 Co1 N4 170.13(7) . . ? O1 Co1 N2 89.95(7) . . ? O2 Co1 N2 173.66(7) . . ? N3 Co1 N2 87.52(7) . . ? N4 Co1 N2 92.28(7) . . ? O1 Co1 N1 174.92(7) . . ? O2 Co1 N1 88.42(7) . . ? N3 Co1 N1 86.29(7) . . ? N4 Co1 N1 83.84(7) . . ? N2 Co1 N1 86.53(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 O1 C2 C3 C4 -1.6(3) . . . . ? C1 C2 C3 C4 177.94(19) . . . . ? C2 C3 C4 O2 -7.3(3) . . . . ? C2 C3 C4 C5 172.4(2) . . . . ? N4 C6 C7 C8 0.9(3) . . . . ? C11 C6 C7 C8 -179.6(2) . . . . ? C6 C7 C8 C9 2.1(4) . . . . ? C7 C8 C9 C10 -2.7(4) . . . . ? C8 C9 C10 N4 0.4(3) . . . . ? N4 C6 C11 N1 -25.0(2) . . . . ? C7 C6 C11 N1 155.5(2) . . . . ? N2 C12 C13 C14 0.1(3) . . . . ? C17 C12 C13 C14 177.6(2) . . . . ? C12 C13 C14 C15 0.3(4) . . . . ? C13 C14 C15 C16 0.4(3) . . . . ? C14 C15 C16 N2 -1.4(3) . . . . ? N2 C12 C17 N1 -13.5(3) . . . . ? C13 C12 C17 N1 168.81(19) . . . . ? N3 C18 C19 C20 -0.1(3) . . . . ? C23 C18 C19 C20 -177.7(2) . . . . ? C18 C19 C20 C21 0.8(3) . . . . ? C19 C20 C21 C22 -1.2(3) . . . . ? C20 C21 C22 N3 0.8(3) . . . . ? N3 C18 C23 N1 28.9(3) . . . . ? C19 C18 C23 N1 -153.4(2) . . . . ? C9 C10 N4 C6 2.5(3) . . . . ? C9 C10 N4 Co1 -177.78(16) . . . . ? C7 C6 N4 C10 -3.2(3) . . . . ? C11 C6 N4 C10 177.27(18) . . . . ? C7 C6 N4 Co1 177.08(17) . . . . ? C11 C6 N4 Co1 -2.5(2) . . . . ? C13 C12 N2 C16 -1.1(3) . . . . ? C17 C12 N2 C16 -178.83(18) . . . . ? C13 C12 N2 Co1 -175.33(16) . . . . ? C17 C12 N2 Co1 7.0(2) . . . . ? C15 C16 N2 C12 1.8(3) . . . . ? C15 C16 N2 Co1 175.41(16) . . . . ? C21 C22 N3 C18 -0.1(3) . . . . ? C21 C22 N3 Co1 -173.97(15) . . . . ? C19 C18 N3 C22 -0.3(3) . . . . ? C23 C18 N3 C22 177.47(18) . . . . ? C19 C18 N3 Co1 174.41(16) . . . . ? C23 C18 N3 Co1 -7.8(2) . . . . ? C18 C23 N1 C11 -150.45(18) . . . . ? C18 C23 N1 C17 85.5(2) . . . . ? C18 C23 N1 Co1 -34.8(2) . . . . ? C6 C11 N1 C23 155.45(17) . . . . ? C6 C11 N1 C17 -79.1(2) . . . . ? C6 C11 N1 Co1 39.48(18) . . . . ? C12 C17 N1 C23 -104.80(19) . . . . ? C12 C17 N1 C11 129.39(18) . . . . ? C12 C17 N1 Co1 13.3(2) . . . . ? C3 C2 O1 Co1 12.6(3) . . . . ? C1 C2 O1 Co1 -166.94(13) . . . . ? C3 C4 O2 Co1 3.6(3) . . . . ? C5 C4 O2 Co1 -176.13(14) . . . . ? C2 O1 Co1 O2 -12.49(16) . . . . ? C2 O1 Co1 N3 -101.47(16) . . . . ? C2 O1 Co1 N4 78.75(16) . . . . ? C2 O1 Co1 N2 171.03(16) . . . . ? C2 O1 Co1 N1 125.0(7) . . . . ? C4 O2 Co1 O1 4.74(17) . . . . ? C4 O2 Co1 N3 101.84(16) . . . . ? C4 O2 Co1 N4 -88.01(16) . . . . ? C4 O2 Co1 N2 150.9(6) . . . . ? C4 O2 Co1 N1 -171.82(16) . . . . ? C22 N3 Co1 O1 -12.73(18) . . . . ? C18 N3 Co1 O1 172.96(14) . . . . ? C22 N3 Co1 O2 -107.89(17) . . . . ? C18 N3 Co1 O2 77.80(14) . . . . ? C22 N3 Co1 N4 166.0(4) . . . . ? C18 N3 Co1 N4 -8.3(5) . . . . ? C22 N3 Co1 N2 76.91(17) . . . . ? C18 N3 Co1 N2 -97.40(15) . . . . ? C22 N3 Co1 N1 163.59(18) . . . . ? C18 N3 Co1 N1 -10.72(14) . . . . ? C10 N4 Co1 O1 17.92(18) . . . . ? C6 N4 Co1 O1 -162.36(14) . . . . ? C10 N4 Co1 O2 113.30(17) . . . . ? C6 N4 Co1 O2 -66.98(15) . . . . ? C10 N4 Co1 N3 -160.8(4) . . . . ? C6 N4 Co1 N3 18.9(5) . . . . ? C10 N4 Co1 N2 -72.13(18) . . . . ? C6 N4 Co1 N2 107.59(15) . . . . ? C10 N4 Co1 N1 -158.39(18) . . . . ? C6 N4 Co1 N1 21.33(14) . . . . ? C12 N2 Co1 O1 -175.40(15) . . . . ? C16 N2 Co1 O1 10.69(17) . . . . ? C12 N2 Co1 O2 38.2(7) . . . . ? C16 N2 Co1 O2 -135.7(6) . . . . ? C12 N2 Co1 N3 87.37(15) . . . . ? C16 N2 Co1 N3 -86.54(17) . . . . ? C12 N2 Co1 N4 -82.75(15) . . . . ? C16 N2 Co1 N4 103.34(17) . . . . ? C12 N2 Co1 N1 0.94(15) . . . . ? C16 N2 Co1 N1 -172.97(17) . . . . ? C23 N1 Co1 O1 159.6(7) . . . . ? C11 N1 Co1 O1 -80.3(8) . . . . ? C17 N1 Co1 O1 38.0(8) . . . . ? C23 N1 Co1 O2 -62.75(14) . . . . ? C11 N1 Co1 O2 57.39(13) . . . . ? C17 N1 Co1 O2 175.68(13) . . . . ? C23 N1 Co1 N3 25.68(14) . . . . ? C11 N1 Co1 N3 145.81(14) . . . . ? C17 N1 Co1 N3 -95.90(14) . . . . ? C23 N1 Co1 N4 -153.91(14) . . . . ? C11 N1 Co1 N4 -33.77(13) . . . . ? C17 N1 Co1 N4 84.51(14) . . . . ? C23 N1 Co1 N2 113.41(14) . . . . ? C11 N1 Co1 N2 -126.45(14) . . . . ? C17 N1 Co1 N2 -8.16(13) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1O O10 0.87(3) 2.15(3) 3.003(3) 168(4) . O1W H1O Cl2 0.87(3) 3.01(2) 3.804(2) 153(4) . O1W H2O O7 0.87(3) 2.13(2) 2.953(4) 157(4) 2_756 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.113 _refine_diff_density_min -0.727 _refine_diff_density_rms 0.093