Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 186 _publ_contact_author_name 'Prof Andrew Borovik' _publ_contact_author_address ; Department of Chemistry University of Kansas 2010 Millott Hall Lawrence Kansas 66045 USA ; _publ_contact_author_email aborovik@ku.edu _publ_contact_author_fax 1(785)8645396 _publ_contact_author_phone 1(785)8644067 _publ_requested_journal 'Dalton Trans.' loop_ _publ_author_name _publ_author_address 'Zart, Matthew K.' ; Department of Chemistry University of Kansas Rm 2010 Malott Hall 1251 Wescoe Hall Dr. Lawrence, KS 66045-7582 USA ; 'Sorrell, Thomas N.' ; Department of Chemistry University of North Carolina - Chapel Hill CB# 3290 Venable Hall Chapel Hill, North Carolina 27599-3290 USA ; 'Powell, Douglas R.' ; Department of Chemistry University of Kansas Rm 2010 Malott Hall 1251 Wescoe Hall Dr. Lawrence, KS 66045-7582 USA ; 'Borovik, Andrew S.' ; Department of Chemistry University of Kansas Rm 2010 Malott Hall 1251 Wescoe Hall Dr. Lawrence, KS 66045-7582 USA ; _publ_section_title ; Development of bio-inspired chelates with hydrogen bond donors: synthesis and structure of monomeric metal acetate complexes with intramolecular hydrogen bonds ; _publ_section_references ; Bruker (1998) SMART and SAINT, Bruker AXS, Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (2000) SADABS, University of Gottingen, Germany Sheldrick, G. M. (1997) SHELXTL, Bruker AXS, Inc., Madison, Wisconsin, USA. ; _publ_section_acknowledgements ; The authors wish to thank the National Science Foundation (CHE-0079282) and the University of Kansas for funds to acquire the diffractometer and computers used in this work. ; #============================================================ data_02100 _database_code_CSD 196774 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; (K1) 1+, (C22 H37 Co1 N6 O4) 1-, x(C4 H9 N1 O1), 1-x(H2 O1), x=0.93 ; _chemical_formula_sum 'C25.72 H45.51 Co K N6.93 O5' _chemical_formula_weight 629.89 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2758(14) _cell_length_b 11.0982(15) _cell_length_c 14.4052(19) _cell_angle_alpha 78.561(3) _cell_angle_beta 82.114(3) _cell_angle_gamma 85.728(3) _cell_volume 1593.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6542 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 30.00 _exptl_crystal_description plate _exptl_crystal_colour magenta _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 669 _exptl_absorpt_coefficient_mu 0.713 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7733 _exptl_absorpt_correction_T_max 0.9321 _exptl_absorpt_process_details 'SADABS, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_device 'Bruker APEX' _diffrn_measurement_method '\w scan frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 190 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.24 _diffrn_reflns_number 13274 _diffrn_reflns_av_R_equivalents 0.0163 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 30.06 _reflns_number_total 8448 _reflns_number_gt 7586 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0620P)^2^+0.8100P] 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 8448 _refine_ls_number_parameters 391 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1091 _refine_ls_wR_factor_gt 0.1057 _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 K1 K 0.50180(3) 0.45090(3) 0.14564(2) 0.02235(8) Uani 1 1 d D . . Co1 Co 0.093752(19) 0.456578(18) 0.233591(14) 0.01552(7) Uani 1 1 d . . . N1 N 0.05438(13) 0.65475(12) 0.18282(10) 0.0197(3) Uani 1 1 d . . . C2 C 0.08916(17) 0.67649(15) 0.07832(12) 0.0229(3) Uani 1 1 d . . . H2A H 0.1027 0.7651 0.0537 0.027 Uiso 1 1 calc R . . H2B H 0.0165 0.6526 0.0482 0.027 Uiso 1 1 calc R . . C3 C 0.21443(17) 0.60118(15) 0.05298(12) 0.0222(3) Uani 1 1 d . . . H3A H 0.2298 0.6036 -0.0167 0.027 Uiso 1 1 calc R . . H3B H 0.2909 0.6352 0.0720 0.027 Uiso 1 1 calc R . . N4 N 0.19778(13) 0.47431(12) 0.10424(9) 0.0186(2) Uani 1 1 d . B . C5 C 0.26897(15) 0.38894(14) 0.06118(11) 0.0181(3) Uani 1 1 d . . . O6 O 0.36225(12) 0.41279(11) -0.00452(9) 0.0243(2) Uani 1 1 d . . . N7 N 0.23268(14) 0.26962(13) 0.09327(10) 0.0211(3) Uani 1 1 d . A . H7 H 0.1572 0.2574 0.1300 0.025 Uiso 1 1 calc R . . C8 C 0.31180(18) 0.16088(15) 0.07018(12) 0.0244(3) Uani 1 1 d . . . C9 C 0.2414(2) 0.04934(16) 0.13010(14) 0.0301(4) Uani 1 1 d . A . H9A H 0.2424 0.0493 0.1980 0.045 Uiso 1 1 d R . . H9B H 0.2866 -0.0262 0.1142 0.045 Uiso 1 1 d R . . H9C H 0.1502 0.0534 0.1164 0.045 Uiso 1 1 d R . . C10 C 0.45174(19) 0.15808(18) 0.09548(17) 0.0357(4) Uani 1 1 d . A . H10A H 0.4485 0.1665 0.1622 0.053 Uiso 1 1 d R . . H10B H 0.4990 0.2261 0.0539 0.053 Uiso 1 1 d R . . H10C H 0.4974 0.0797 0.0866 0.053 Uiso 1 1 d R . . C11 C 0.3129(3) 0.15611(19) -0.03519(15) 0.0427(5) Uani 1 1 d . A 1 H11A H 0.2224 0.1538 -0.0490 0.064 Uiso 1 1 d R A 1 H11B H 0.3634 0.0821 -0.0494 0.064 Uiso 1 1 d R A 1 H11C H 0.3536 0.2292 -0.0748 0.064 Uiso 1 1 d R A 1 C12 C -0.08697(16) 0.67514(15) 0.21360(13) 0.0236(3) Uani 1 1 d . . . H12A H -0.1194 0.7541 0.1769 0.028 Uiso 1 1 calc R . . H12B H -0.1004 0.6804 0.2821 0.028 Uiso 1 1 calc R . . C13 C -0.16475(16) 0.57087(15) 0.19810(14) 0.0253(3) Uani 1 1 d . . . H13A H -0.2567 0.5784 0.2284 0.030 Uiso 1 1 calc R . . H13B H -0.1658 0.5748 0.1289 0.030 Uiso 1 1 calc R . . N14 N -0.10228(13) 0.45346(12) 0.24055(10) 0.0198(3) Uani 1 1 d . . . C15 C -0.17931(15) 0.35746(15) 0.24847(12) 0.0203(3) Uani 1 1 d . . . O16 O -0.29173(12) 0.36593(12) 0.22358(10) 0.0293(3) Uani 1 1 d . . . N17 N -0.12752(13) 0.24433(12) 0.29101(10) 0.0209(3) Uani 1 1 d . . . H17 H -0.0567 0.2433 0.3193 0.025 Uiso 1 1 calc R . . C18 C -0.18329(16) 0.12643(15) 0.29181(12) 0.0219(3) Uani 1 1 d . . . C19 C -0.08775(18) 0.02697(16) 0.33723(14) 0.0285(4) Uani 1 1 d . . . H19A H -0.0800 0.0381 0.4020 0.043 Uiso 1 1 d R . . H19B H -0.0012 0.0334 0.2988 0.043 Uiso 1 1 d R . . H19C H -0.1208 -0.0544 0.3399 0.043 Uiso 1 1 d R . . C20 C -0.1948(2) 0.10904(19) 0.19038(14) 0.0322(4) Uani 1 1 d . . . H20A H -0.2589 0.1704 0.1622 0.048 Uiso 1 1 d R . . H20B H -0.2239 0.0263 0.1927 0.048 Uiso 1 1 d R . . H20C H -0.1089 0.1193 0.1514 0.048 Uiso 1 1 d R . . C21 C -0.31802(18) 0.11679(17) 0.35300(14) 0.0288(4) Uani 1 1 d . . . H21A H -0.3799 0.1798 0.3238 0.043 Uiso 1 1 d R . . H21B H -0.3092 0.1294 0.4172 0.043 Uiso 1 1 d R . . H21C H -0.3510 0.0350 0.3571 0.043 Uiso 1 1 d R . . C22 C 0.13414(17) 0.72432(15) 0.22859(12) 0.0239(3) Uani 1 1 d . . . H22A H 0.0938 0.8083 0.2278 0.029 Uiso 1 1 calc R . . H22B H 0.2234 0.7317 0.1926 0.029 Uiso 1 1 calc R . . C23 C 0.14363(16) 0.66046(16) 0.33013(12) 0.0232(3) Uani 1 1 d . . . N24 N 0.14134(13) 0.53698(13) 0.34711(10) 0.0205(3) Uani 1 1 d . . . C25 C 0.15317(16) 0.47533(17) 0.43602(12) 0.0237(3) Uani 1 1 d . . . H25 H 0.1520 0.3881 0.4482 0.028 Uiso 1 1 calc R . . C26 C 0.16697(17) 0.53323(19) 0.51064(13) 0.0295(4) Uani 1 1 d . . . H26 H 0.1752 0.4866 0.5726 0.035 Uiso 1 1 calc R . . C27 C 0.16858(19) 0.6601(2) 0.49330(14) 0.0342(4) Uani 1 1 d . . . H27 H 0.1776 0.7023 0.5432 0.041 Uiso 1 1 calc R . . C28 C 0.15676(19) 0.72460(19) 0.40185(14) 0.0312(4) Uani 1 1 d . . . H28 H 0.1576 0.8119 0.3882 0.037 Uiso 1 1 calc R . . O29 O 0.14182(11) 0.27878(10) 0.30309(8) 0.0200(2) Uani 1 1 d . B . C30 C 0.25760(16) 0.24790(15) 0.32513(11) 0.0198(3) Uani 1 1 d . . . O31 O 0.35516(12) 0.30845(12) 0.29527(9) 0.0280(3) Uani 1 1 d . B . C32 C 0.26999(19) 0.12720(17) 0.39537(13) 0.0290(4) Uani 1 1 d . B . H32D H 0.2338 0.0616 0.3715 0.044 Uiso 1 1 d R . . H32E H 0.2212 0.1355 0.4574 0.044 Uiso 1 1 d R . . H32F H 0.3629 0.1066 0.4026 0.044 Uiso 1 1 d R . . O1S O 0.4433(4) 0.6512(2) 0.2255(2) 0.0267(8) Uani 0.846(3) 1 d PD B 1 N1S N 0.51304(19) 0.74662(17) 0.33103(12) 0.0284(4) Uani 0.846(3) 1 d PD B 1 C1S C 0.48312(18) 0.6444(2) 0.30255(14) 0.0233(4) Uani 0.846(3) 1 d PD B 1 C2S C 0.4968(3) 0.5238(2) 0.37056(16) 0.0288(5) Uani 0.846(3) 1 d PD B 1 H2SA H 0.4492 0.5301 0.4334 0.043 Uiso 0.846(3) 1 d PR B 1 H2SB H 0.5903 0.5042 0.3764 0.043 Uiso 0.846(3) 1 d PR B 1 H2SC H 0.4608 0.4587 0.3461 0.043 Uiso 0.846(3) 1 d PR B 1 C3S C 0.4984(5) 0.8655(3) 0.2691(2) 0.0357(9) Uani 0.846(3) 1 d PD B 1 H3SA H 0.4551 0.8556 0.2147 0.054 Uiso 0.846(3) 1 d PR B 1 H3SB H 0.5850 0.8992 0.2458 0.054 Uiso 0.846(3) 1 d PR B 1 H3SC H 0.4445 0.9220 0.3047 0.054 Uiso 0.846(3) 1 d PR B 1 C4S C 0.5620(4) 0.7476(3) 0.42107(19) 0.0423(7) Uani 0.846(3) 1 d PD B 1 H4SA H 0.5920 0.6637 0.4481 0.063 Uiso 0.846(3) 1 d PR B 1 H4SB H 0.4918 0.7767 0.4659 0.063 Uiso 0.846(3) 1 d PR B 1 H4SC H 0.6357 0.8020 0.4098 0.063 Uiso 0.846(3) 1 d PR B 1 O1S' O 0.463(4) 0.6533(16) 0.2252(17) 0.019(8) Uiso 0.083(3) 1 d PD B 2 N1S' N 0.5340(14) 0.6512(12) 0.3663(9) 0.016(3) Uiso 0.083(3) 1 d PD B 2 C1S' C 0.4842(17) 0.7094(12) 0.2865(9) 0.015(4) Uiso 0.083(3) 1 d PD B 2 C2S' C 0.479(5) 0.8477(13) 0.269(3) 0.039(14) Uiso 0.083(3) 1 d PD B 2 H2S1 H 0.4849 0.8763 0.1998 0.059 Uiso 0.083(3) 1 d PR B 2 H2S2 H 0.5539 0.8768 0.2928 0.059 Uiso 0.083(3) 1 d PR B 2 H2S3 H 0.3969 0.8802 0.3000 0.059 Uiso 0.083(3) 1 d PR B 2 C3S' C 0.549(3) 0.5175(12) 0.3834(15) 0.029(6) Uiso 0.083(3) 1 d PD B 2 H3S1 H 0.6103 0.4904 0.3324 0.043 Uiso 0.083(3) 1 d PR B 2 H3S2 H 0.4642 0.4802 0.3877 0.043 Uiso 0.083(3) 1 d PR B 2 H3S3 H 0.5848 0.4922 0.4443 0.043 Uiso 0.083(3) 1 d PR B 2 C4S' C 0.598(4) 0.710(2) 0.429(2) 0.050(10) Uiso 0.083(3) 1 d PD B 2 H4S1 H 0.6838 0.6882 0.4515 0.074 Uiso 0.083(3) 1 d PR B 2 H4S2 H 0.5281 0.6833 0.4812 0.074 Uiso 0.083(3) 1 d PR B 2 H4S3 H 0.5883 0.7989 0.4071 0.074 Uiso 0.083(3) 1 d PR B 2 O1W O 0.5138(19) 0.4014(18) 0.4022(14) 0.030 Uiso 0.070(2) 1 d P C 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.01709(16) 0.02503(18) 0.02214(16) 0.00317(13) -0.00193(12) -0.00467(12) Co1 0.01418(10) 0.01371(11) 0.01750(11) -0.00013(7) -0.00109(7) -0.00238(7) N1 0.0188(6) 0.0161(6) 0.0234(6) -0.0020(5) -0.0015(5) -0.0019(5) C2 0.0268(8) 0.0155(7) 0.0239(7) 0.0019(6) -0.0032(6) -0.0005(6) C3 0.0265(8) 0.0153(7) 0.0213(7) 0.0018(6) 0.0018(6) -0.0014(6) N4 0.0207(6) 0.0136(6) 0.0190(6) 0.0013(5) -0.0003(5) -0.0021(5) C5 0.0176(7) 0.0173(7) 0.0185(7) 0.0002(5) -0.0037(5) -0.0024(5) O6 0.0242(6) 0.0210(6) 0.0235(6) 0.0007(4) 0.0055(4) -0.0025(4) N7 0.0211(6) 0.0157(6) 0.0245(6) -0.0019(5) 0.0021(5) -0.0021(5) C8 0.0297(8) 0.0163(8) 0.0248(8) -0.0025(6) 0.0015(6) 0.0008(6) C9 0.0355(10) 0.0160(8) 0.0370(10) -0.0017(7) -0.0027(8) -0.0026(7) C10 0.0246(9) 0.0232(9) 0.0537(12) -0.0005(8) 0.0019(8) 0.0037(7) C11 0.0756(16) 0.0239(10) 0.0272(9) -0.0075(8) -0.0025(10) 0.0069(10) C12 0.0196(7) 0.0165(8) 0.0330(9) -0.0025(6) -0.0017(6) 0.0016(6) C13 0.0182(7) 0.0179(8) 0.0381(9) 0.0003(7) -0.0067(6) -0.0001(6) N14 0.0172(6) 0.0153(6) 0.0260(7) -0.0006(5) -0.0038(5) -0.0015(5) C15 0.0174(7) 0.0192(8) 0.0237(7) -0.0024(6) -0.0020(6) -0.0022(5) O16 0.0188(6) 0.0255(7) 0.0434(7) -0.0006(5) -0.0106(5) -0.0039(5) N17 0.0178(6) 0.0160(6) 0.0290(7) -0.0010(5) -0.0058(5) -0.0045(5) C18 0.0209(7) 0.0184(8) 0.0260(8) -0.0037(6) 0.0002(6) -0.0063(6) C19 0.0277(9) 0.0176(8) 0.0375(10) 0.0002(7) -0.0011(7) -0.0043(6) C20 0.0359(10) 0.0333(10) 0.0302(9) -0.0112(8) -0.0034(7) -0.0067(8) C21 0.0228(8) 0.0266(9) 0.0353(9) -0.0046(7) 0.0040(7) -0.0089(6) C22 0.0246(8) 0.0171(8) 0.0299(8) -0.0041(6) -0.0019(6) -0.0051(6) C23 0.0187(7) 0.0245(8) 0.0269(8) -0.0071(6) -0.0002(6) -0.0045(6) N24 0.0163(6) 0.0228(7) 0.0221(6) -0.0039(5) 0.0002(5) -0.0036(5) C25 0.0176(7) 0.0315(9) 0.0218(7) -0.0044(6) -0.0017(6) -0.0027(6) C26 0.0215(8) 0.0447(11) 0.0240(8) -0.0093(7) -0.0029(6) -0.0040(7) C27 0.0271(9) 0.0493(12) 0.0316(9) -0.0207(9) -0.0011(7) -0.0069(8) C28 0.0286(9) 0.0314(10) 0.0375(10) -0.0159(8) -0.0018(7) -0.0066(7) O29 0.0188(5) 0.0163(5) 0.0231(5) 0.0014(4) -0.0016(4) -0.0041(4) C30 0.0210(7) 0.0192(7) 0.0181(7) -0.0011(6) -0.0010(5) -0.0029(5) O31 0.0186(6) 0.0322(7) 0.0299(6) 0.0034(5) -0.0017(5) -0.0076(5) C32 0.0298(9) 0.0227(9) 0.0319(9) 0.0047(7) -0.0090(7) -0.0012(7) O1S 0.0207(15) 0.0308(12) 0.0298(12) -0.0065(6) -0.0051(7) -0.0044(7) N1S 0.0299(9) 0.0306(10) 0.0259(9) -0.0046(7) -0.0064(7) -0.0062(7) C1S 0.0152(8) 0.0258(11) 0.0250(9) 0.0001(8) 0.0047(7) -0.0022(7) C2S 0.0364(13) 0.0270(11) 0.0226(10) 0.0004(8) -0.0054(9) -0.0102(9) C3S 0.050(2) 0.0220(12) 0.0388(17) -0.0083(10) -0.0157(13) 0.0000(14) C4S 0.064(2) 0.0359(15) 0.0331(13) -0.0086(11) -0.0201(13) -0.0103(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 K1 O16 2.5665(13) 1_655 ? K1 O6 2.5862(12) 2_665 ? K1 O1S 2.6927(16) . ? K1 O1S' 2.699(6) . ? K1 O31 2.7437(13) . ? K1 O6 2.8668(14) . ? K1 H10B 3.0497 . ? K1 H2SC 2.8782 . ? Co1 N4 1.9982(13) . ? Co1 N14 2.0056(14) . ? Co1 O29 2.0849(12) . ? Co1 N24 2.1383(14) . ? Co1 N1 2.2014(14) . ? N1 C22 1.465(2) . ? N1 C12 1.474(2) . ? N1 C2 1.474(2) . ? C2 C3 1.523(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N4 1.465(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N4 C5 1.350(2) . ? C5 O6 1.2546(19) . ? C5 N7 1.375(2) . ? O6 K1 2.5862(12) 2_665 ? N7 C8 1.472(2) . ? N7 H7 0.8800 . ? C8 C11 1.528(3) . ? C8 C10 1.528(3) . ? C8 C9 1.529(3) . ? C9 H9A 0.9800 . ? C9 H9B 0.9799 . ? C9 H9C 0.9801 . ? C10 H10A 0.9800 . ? C10 H10B 0.9801 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9801 . ? C11 H11C 0.9800 . ? C12 C13 1.522(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N14 1.467(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? N14 C15 1.352(2) . ? C15 O16 1.2473(19) . ? C15 N17 1.386(2) . ? O16 K1 2.5665(13) 1_455 ? N17 C18 1.465(2) . ? N17 H17 0.8800 . ? C18 C19 1.529(2) . ? C18 C20 1.533(2) . ? C18 C21 1.535(2) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9801 . ? C22 C23 1.506(2) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 N24 1.345(2) . ? C23 C28 1.392(2) . ? N24 C25 1.344(2) . ? C25 C26 1.385(2) . ? C25 H25 0.9500 . ? C26 C27 1.381(3) . ? C26 H26 0.9500 . ? C27 C28 1.386(3) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? O29 C30 1.2780(19) . ? C30 O31 1.228(2) . ? C30 C32 1.519(2) . ? C32 H32D 0.9799 . ? C32 H32E 0.9800 . ? C32 H32F 0.9800 . ? O1S C1S 1.222(3) . ? N1S C1S 1.350(3) . ? N1S C3S 1.449(3) . ? N1S C4S 1.456(2) . ? N1S H2S2 1.5088 . ? C1S C2S 1.503(3) . ? C2S H2SA 0.9799 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? C2S H3S1 1.2807 . ? C2S H3S2 0.6015 . ? C2S H3S3 1.4616 . ? C3S H3SA 0.9800 . ? C3S H3SB 0.9800 . ? C3S H3SC 0.9801 . ? C3S H2S1 1.0081 . ? C3S H2S2 0.7340 . ? C3S H2S3 1.0903 . ? C4S H4SA 0.9800 . ? C4S H4SB 0.9799 . ? C4S H4SC 0.9800 . ? C4S H4S1 1.4513 . ? C4S H4S2 1.0437 . ? C4S H4S3 0.6325 . ? O1S' C1S' 1.225(5) . ? N1S' C1S' 1.349(5) . ? N1S' C3S' 1.455(4) . ? N1S' C4S' 1.455(4) . ? N1S' H4SA 1.4245 . ? C1S' C2S' 1.504(5) . ? C2S' H3SA 0.8404 . ? C2S' H3SB 1.2383 . ? C2S' H3SC 1.0696 . ? C2S' H2S1 0.9800 . ? C2S' H2S2 0.9800 . ? C2S' H2S3 0.9800 . ? C3S' H2SA 1.1839 . ? C3S' H2SB 0.4449 . ? C3S' H2SC 1.3760 . ? C3S' H3S1 0.9800 . ? C3S' H3S2 0.9800 . ? C3S' H3S3 0.9800 . ? C4S' H4SA 0.5324 . ? C4S' H4SB 1.3783 . ? C4S' H4SC 1.0945 . ? C4S' H4S1 0.9800 . ? C4S' H4S2 0.9800 . ? C4S' H4S3 0.9800 . ? O1W H2SB 1.3934 . ? O1W H2SC 1.1043 . ? O1W H3S2 0.9788 . ? 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 O16 K1 O6 92.27(4) 1_655 2_665 ? O16 K1 O1S 99.70(8) 1_655 . ? O6 K1 O1S 88.47(9) 2_665 . ? O16 K1 O1S' 96.0(6) 1_655 . ? O6 K1 O1S' 86.1(8) 2_665 . ? O1S K1 O1S' 4.4(9) . . ? O16 K1 O31 88.29(4) 1_655 . ? O6 K1 O31 179.31(4) 2_665 . ? O1S K1 O31 91.05(9) . . ? O1S' K1 O31 93.4(8) . . ? O16 K1 O6 139.30(4) 1_655 . ? O6 K1 O6 81.82(4) 2_665 . ? O1S K1 O6 120.20(7) . . ? O1S' K1 O6 123.4(5) . . ? O31 K1 O6 98.01(4) . . ? O16 K1 H10B 92.1 1_655 . ? O6 K1 H10B 97.5 2_665 . ? O1S K1 H10B 166.6 . . ? O1S' K1 H10B 171.0 . . ? O31 K1 H10B 82.9 . . ? O6 K1 H10B 49.6 . . ? O16 K1 H2SC 69.7 1_655 . ? O6 K1 H2SC 130.8 2_665 . ? O1S K1 H2SC 52.8 . . ? O1S' K1 H2SC 52.9 . . ? O31 K1 H2SC 49.1 . . ? O6 K1 H2SC 140.8 . . ? H10B K1 H2SC 127.4 . . ? N4 Co1 N14 117.22(6) . . ? N4 Co1 O29 105.12(5) . . ? N14 Co1 O29 101.69(5) . . ? N4 Co1 N24 124.52(6) . . ? N14 Co1 N24 109.42(5) . . ? O29 Co1 N24 92.65(5) . . ? N4 Co1 N1 81.01(5) . . ? N14 Co1 N1 82.43(5) . . ? O29 Co1 N1 169.56(5) . . ? N24 Co1 N1 76.91(5) . . ? C22 N1 C12 111.09(13) . . ? C22 N1 C2 112.14(13) . . ? C12 N1 C2 113.81(13) . . ? C22 N1 Co1 109.03(10) . . ? C12 N1 Co1 104.24(10) . . ? C2 N1 Co1 106.00(9) . . ? N1 C2 C3 109.70(13) . . ? N1 C2 H2A 109.7 . . ? C3 C2 H2A 109.7 . . ? N1 C2 H2B 109.7 . . ? C3 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? N4 C3 C2 107.77(13) . . ? N4 C3 H3A 110.2 . . ? C2 C3 H3A 110.2 . . ? N4 C3 H3B 110.2 . . ? C2 C3 H3B 110.2 . . ? H3A C3 H3B 108.5 . . ? C5 N4 C3 114.16(13) . . ? C5 N4 Co1 130.01(11) . . ? C3 N4 Co1 115.26(10) . . ? O6 C5 N4 124.23(15) . . ? O6 C5 N7 120.11(14) . . ? N4 C5 N7 115.65(14) . . ? C5 O6 K1 155.80(11) . 2_665 ? C5 O6 K1 84.10(9) . . ? K1 O6 K1 98.18(4) 2_665 . ? C5 N7 C8 124.28(14) . . ? C5 N7 H7 117.9 . . ? C8 N7 H7 117.9 . . ? N7 C8 C11 110.05(15) . . ? N7 C8 C10 112.04(15) . . ? C11 C8 C10 110.94(17) . . ? N7 C8 C9 105.81(14) . . ? C11 C8 C9 108.36(16) . . ? C10 C8 C9 109.46(15) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.4 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.4 . . ? C8 C10 H10B 109.6 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.4 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.4 . . ? C8 C11 H11B 109.4 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 C13 110.78(13) . . ? N1 C12 H12A 109.5 . . ? C13 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? N14 C13 C12 108.58(13) . . ? N14 C13 H13A 110.0 . . ? C12 C13 H13A 110.0 . . ? N14 C13 H13B 110.0 . . ? C12 C13 H13B 110.0 . . ? H13A C13 H13B 108.4 . . ? C15 N14 C13 112.56(13) . . ? C15 N14 Co1 129.93(11) . . ? C13 N14 Co1 113.71(10) . . ? O16 C15 N14 124.63(15) . . ? O16 C15 N17 119.98(15) . . ? N14 C15 N17 115.34(14) . . ? C15 O16 K1 161.76(12) . 1_455 ? C15 N17 C18 124.09(13) . . ? C15 N17 H17 118.0 . . ? C18 N17 H17 118.0 . . ? N17 C18 C19 106.03(14) . . ? N17 C18 C20 111.33(14) . . ? C19 C18 C20 109.33(15) . . ? N17 C18 C21 110.38(14) . . ? C19 C18 C21 109.18(14) . . ? C20 C18 C21 110.46(15) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.4 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 C22 C23 110.25(14) . . ? N1 C22 H22A 109.6 . . ? C23 C22 H22A 109.6 . . ? N1 C22 H22B 109.6 . . ? C23 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? N24 C23 C28 121.80(17) . . ? N24 C23 C22 115.89(14) . . ? C28 C23 C22 122.30(16) . . ? C25 N24 C23 118.25(15) . . ? C25 N24 Co1 124.91(12) . . ? C23 N24 Co1 116.34(11) . . ? N24 C25 C26 122.98(17) . . ? N24 C25 H25 118.5 . . ? C26 C25 H25 118.5 . . ? C27 C26 C25 118.75(18) . . ? C27 C26 H26 120.6 . . ? C25 C26 H26 120.6 . . ? C26 C27 C28 118.77(17) . . ? C26 C27 H27 120.6 . . ? C28 C27 H27 120.6 . . ? C27 C28 C23 119.45(18) . . ? C27 C28 H28 120.3 . . ? C23 C28 H28 120.3 . . ? C30 O29 Co1 121.37(10) . . ? O31 C30 O29 125.19(15) . . ? O31 C30 C32 119.57(15) . . ? O29 C30 C32 115.24(14) . . ? C30 O31 K1 148.91(11) . . ? C30 C32 H32D 109.5 . . ? C30 C32 H32E 109.4 . . ? H32D C32 H32E 109.5 . . ? C30 C32 H32F 109.5 . . ? H32D C32 H32F 109.5 . . ? H32E C32 H32F 109.5 . . ? C1S O1S K1 114.79(16) . . ? C1S N1S C3S 119.5(2) . . ? C1S N1S C4S 124.7(2) . . ? C3S N1S C4S 115.8(2) . . ? C1S N1S H2S2 142.0 . . ? C3S N1S H2S2 28.6 . . ? C4S N1S H2S2 90.7 . . ? O1S C1S N1S 120.7(2) . . ? O1S C1S C2S 122.0(2) . . ? N1S C1S C2S 117.30(18) . . ? C1S C2S H2SA 109.8 . . ? C1S C2S H2SB 108.9 . . ? H2SA C2S H2SB 109.5 . . ? C1S C2S H2SC 109.7 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? C1S C2S H3S1 96.6 . . ? H2SA C2S H3S1 140.3 . . ? H2SB C2S H3S1 31.7 . . ? H2SC C2S H3S1 87.5 . . ? C1S C2S H3S2 138.0 . . ? H2SA C2S H3S2 67.3 . . ? H2SB C2S H3S2 111.3 . . ? H2SC C2S H3S2 44.5 . . ? H3S1 C2S H3S2 111.3 . . ? C1S C2S H3S3 127.4 . . ? H2SA C2S H3S3 69.4 . . ? H2SB C2S H3S3 40.3 . . ? H2SC C2S H3S3 120.1 . . ? H3S1 C2S H3S3 71.1 . . ? H3S2 C2S H3S3 92.1 . . ? N1S C3S H3SA 109.0 . . ? N1S C3S H3SB 110.0 . . ? H3SA C3S H3SB 109.5 . . ? N1S C3S H3SC 109.4 . . ? H3SA C3S H3SC 109.5 . . ? H3SB C3S H3SC 109.5 . . ? N1S C3S H2S1 123.6 . . ? H3SA C3S H2S1 23.5 . . ? H3SB C3S H2S1 86.4 . . ? H3SC C3S H2S1 114.9 . . ? N1S C3S H2S2 80.2 . . ? H3SA C3S H2S2 155.3 . . ? H3SB C3S H2S2 46.5 . . ? H3SC C3S H2S2 87.7 . . ? H2S1 C3S H2S2 132.8 . . ? N1S C3S H2S3 92.8 . . ? H3SA C3S H2S3 81.9 . . ? H3SB C3S H2S3 148.3 . . ? H3SC C3S H2S3 40.1 . . ? H2S1 C3S H2S3 99.3 . . ? H2S2 C3S H2S3 121.4 . . ? N1S C4S H4SA 108.7 . . ? N1S C4S H4SB 110.1 . . ? H4SA C4S H4SB 109.5 . . ? N1S C4S H4SC 109.6 . . ? H4SA C4S H4SC 109.5 . . ? H4SB C4S H4SC 109.5 . . ? N1S C4S H4S1 126.3 . . ? H4SA C4S H4S1 44.0 . . ? H4SB C4S H4S1 122.1 . . ? H4SC C4S H4S1 65.5 . . ? N1S C4S H4S2 118.6 . . ? H4SA C4S H4S2 46.5 . . ? H4SB C4S H4S2 63.5 . . ? H4SC C4S H4S2 130.7 . . ? H4S1 C4S H4S2 77.9 . . ? N1S C4S H4S3 95.2 . . ? H4SA C4S H4S3 135.7 . . ? H4SB C4S H4S3 95.7 . . ? H4SC C4S H4S3 26.2 . . ? H4S1 C4S H4S3 91.7 . . ? H4S2 C4S H4S3 144.3 . . ? C1S' O1S' K1 150.0(15) . . ? C1S' N1S' C3S' 118.1(14) . . ? C1S' N1S' C4S' 125.7(15) . . ? C3S' N1S' C4S' 115.1(6) . . ? C1S' N1S' H4SA 146.6 . . ? C3S' N1S' H4SA 95.1 . . ? C4S' N1S' H4SA 21.3 . . ? O1S' C1S' N1S' 121.4(16) . . ? O1S' C1S' C2S' 121.8(7) . . ? N1S' C1S' C2S' 115.9(15) . . ? C1S' C2S' H3SA 93.9 . . ? C1S' C2S' H3SB 117.6 . . ? H3SA C2S' H3SB 98.9 . . ? C1S' C2S' H3SC 140.1 . . ? H3SA C2S' H3SC 113.3 . . ? H3SB C2S' H3SC 87.5 . . ? C1S' C2S' H2S1 106.8 . . ? H3SA C2S' H2S1 24.3 . . ? H3SB C2S' H2S1 74.7 . . ? H3SC C2S' H2S1 109.7 . . ? C1S' C2S' H2S2 110.5 . . ? H3SA C2S' H2S2 133.7 . . ? H3SB C2S' H2S2 35.1 . . ? H3SC C2S' H2S2 71.6 . . ? H2S1 C2S' H2S2 109.5 . . ? C1S' C2S' H2S3 111.1 . . ? H3SA C2S' H2S3 96.3 . . ? H3SB C2S' H2S3 127.4 . . ? H3SC C2S' H2S3 40.6 . . ? H2S1 C2S' H2S3 109.5 . . ? H2S2 C2S' H2S3 109.5 . . ? N1S' C3S' H2SA 80.1 . . ? N1S' C3S' H2SB 112.3 . . ? H2SA C3S' H2SB 155.9 . . ? N1S' C3S' H2SC 116.0 . . ? H2SA C3S' H2SC 77.0 . . ? H2SB C3S' H2SC 112.6 . . ? N1S' C3S' H3S1 110.4 . . ? H2SA C3S' H3S1 159.2 . . ? H2SB C3S' H3S1 37.3 . . ? H2SC C3S' H3S1 82.3 . . ? N1S' C3S' H3S2 111.5 . . ? H2SA C3S' H3S2 49.9 . . ? H2SB C3S' H3S2 132.8 . . ? H2SC C3S' H3S2 28.4 . . ? H3S1 C3S' H3S2 109.5 . . ? N1S' C3S' H3S3 106.4 . . ? H2SA C3S' H3S3 83.2 . . ? H2SB C3S' H3S3 73.5 . . ? H2SC C3S' H3S3 128.5 . . ? H3S1 C3S' H3S3 109.5 . . ? H3S2 C3S' H3S3 109.5 . . ? N1S' C4S' H4SA 76.1 . . ? N1S' C4S' H4SB 100.0 . . ? H4SA C4S' H4SB 104.9 . . ? N1S' C4S' H4SC 124.9 . . ? H4SA C4S' H4SC 157.9 . . ? H4SB C4S' H4SC 79.8 . . ? N1S' C4S' H4S1 128.5 . . ? H4SA C4S' H4S1 77.7 . . ? H4SB C4S' H4S1 129.5 . . ? H4SC C4S' H4S1 82.8 . . ? N1S' C4S' H4S2 89.8 . . ? H4SA C4S' H4S2 54.7 . . ? H4SB C4S' H4S2 50.3 . . ? H4SC C4S' H4S2 124.8 . . ? H4S1 C4S' H4S2 109.5 . . ? N1S' C4S' H4S3 107.8 . . ? H4SA C4S' H4S3 164.1 . . ? H4SB C4S' H4S3 59.4 . . ? H4SC C4S' H4S3 27.1 . . ? H4S1 C4S' H4S3 109.5 . . ? H4S2 C4S' H4S3 109.5 . . ? H2SB O1W H2SC 78.8 . . ? H2SB O1W H3S2 65.1 . . ? H2SC O1W H3S2 38.3 . . ? 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 Co1 N1 C22 -103.73(11) . . . . ? N14 Co1 N1 C22 137.06(11) . . . . ? O29 Co1 N1 C22 23.1(3) . . . . ? N24 Co1 N1 C22 25.02(10) . . . . ? N4 Co1 N1 C12 137.57(11) . . . . ? N14 Co1 N1 C12 18.35(10) . . . . ? O29 Co1 N1 C12 -95.6(3) . . . . ? N24 Co1 N1 C12 -93.69(10) . . . . ? N4 Co1 N1 C2 17.18(10) . . . . ? N14 Co1 N1 C2 -102.04(10) . . . . ? O29 Co1 N1 C2 144.0(2) . . . . ? N24 Co1 N1 C2 145.92(11) . . . . ? C22 N1 C2 C3 78.57(16) . . . . ? C12 N1 C2 C3 -154.27(14) . . . . ? Co1 N1 C2 C3 -40.31(15) . . . . ? N1 C2 C3 N4 49.86(17) . . . . ? C2 C3 N4 C5 152.97(14) . . . . ? C2 C3 N4 Co1 -34.80(16) . . . . ? N14 Co1 N4 C5 -102.51(14) . . . . ? O29 Co1 N4 C5 9.52(15) . . . . ? N24 Co1 N4 C5 113.64(14) . . . . ? N1 Co1 N4 C5 -179.13(15) . . . . ? N14 Co1 N4 C3 86.75(12) . . . . ? O29 Co1 N4 C3 -161.22(11) . . . . ? N24 Co1 N4 C3 -57.10(13) . . . . ? N1 Co1 N4 C3 10.13(11) . . . . ? C3 N4 C5 O6 14.8(2) . . . . ? Co1 N4 C5 O6 -155.98(12) . . . . ? C3 N4 C5 N7 -164.66(14) . . . . ? Co1 N4 C5 N7 24.5(2) . . . . ? N4 C5 O6 K1 -23.5(4) . . . 2_665 ? N7 C5 O6 K1 156.0(2) . . . 2_665 ? N4 C5 O6 K1 73.37(15) . . . . ? N7 C5 O6 K1 -107.16(14) . . . . ? O16 K1 O6 C5 120.35(10) 1_655 . . . ? O6 K1 O6 C5 -155.72(11) 2_665 . . . ? O1S K1 O6 C5 -72.32(14) . . . . ? O1S' K1 O6 C5 -75.9(11) . . . . ? O31 K1 O6 C5 23.60(10) . . . . ? O16 K1 O6 K1 -83.93(7) 1_655 . . 2_665 ? O6 K1 O6 K1 0.0 2_665 . . 2_665 ? O1S K1 O6 K1 83.40(11) . . . 2_665 ? O1S' K1 O6 K1 79.8(11) . . . 2_665 ? O31 K1 O6 K1 179.32(4) . . . 2_665 ? O6 C5 N7 C8 13.0(2) . . . . ? N4 C5 N7 C8 -167.47(14) . . . . ? C5 N7 C8 C11 -69.6(2) . . . . ? C5 N7 C8 C10 54.3(2) . . . . ? C5 N7 C8 C9 173.57(15) . . . . ? C22 N1 C12 C13 -158.52(14) . . . . ? C2 N1 C12 C13 73.78(17) . . . . ? Co1 N1 C12 C13 -41.23(15) . . . . ? N1 C12 C13 N14 50.50(19) . . . . ? C12 C13 N14 C15 166.72(14) . . . . ? C12 C13 N14 Co1 -32.94(17) . . . . ? N4 Co1 N14 C15 88.58(15) . . . . ? O29 Co1 N14 C15 -25.37(15) . . . . ? N24 Co1 N14 C15 -122.44(14) . . . . ? N1 Co1 N14 C15 164.36(15) . . . . ? N4 Co1 N14 C13 -67.52(13) . . . . ? O29 Co1 N14 C13 178.52(11) . . . . ? N24 Co1 N14 C13 81.46(12) . . . . ? N1 Co1 N14 C13 8.26(11) . . . . ? C13 N14 C15 O16 -0.5(2) . . . . ? Co1 N14 C15 O16 -156.87(13) . . . . ? C13 N14 C15 N17 -177.96(14) . . . . ? Co1 N14 C15 N17 25.7(2) . . . . ? N14 C15 O16 K1 14.4(5) . . . 1_455 ? N17 C15 O16 K1 -168.3(3) . . . 1_455 ? O16 C15 N17 C18 13.5(2) . . . . ? N14 C15 N17 C18 -169.00(15) . . . . ? C15 N17 C18 C19 174.56(15) . . . . ? C15 N17 C18 C20 55.7(2) . . . . ? C15 N17 C18 C21 -67.3(2) . . . . ? C12 N1 C22 C23 77.54(17) . . . . ? C2 N1 C22 C23 -153.86(13) . . . . ? Co1 N1 C22 C23 -36.79(15) . . . . ? N1 C22 C23 N24 31.7(2) . . . . ? N1 C22 C23 C28 -149.62(16) . . . . ? C28 C23 N24 C25 -0.5(2) . . . . ? C22 C23 N24 C25 178.20(14) . . . . ? C28 C23 N24 Co1 171.74(13) . . . . ? C22 C23 N24 Co1 -9.55(18) . . . . ? N4 Co1 N24 C25 -127.86(13) . . . . ? N14 Co1 N24 C25 85.94(13) . . . . ? O29 Co1 N24 C25 -17.44(13) . . . . ? N1 Co1 N24 C25 162.91(14) . . . . ? N4 Co1 N24 C23 60.47(13) . . . . ? N14 Co1 N24 C23 -85.73(12) . . . . ? O29 Co1 N24 C23 170.89(12) . . . . ? N1 Co1 N24 C23 -8.76(11) . . . . ? C23 N24 C25 C26 0.3(2) . . . . ? Co1 N24 C25 C26 -171.23(12) . . . . ? N24 C25 C26 C27 0.1(3) . . . . ? C25 C26 C27 C28 -0.2(3) . . . . ? C26 C27 C28 C23 0.0(3) . . . . ? N24 C23 C28 C27 0.4(3) . . . . ? C22 C23 C28 C27 -178.25(17) . . . . ? N4 Co1 O29 C30 66.75(12) . . . . ? N14 Co1 O29 C30 -170.58(12) . . . . ? N24 Co1 O29 C30 -60.13(12) . . . . ? N1 Co1 O29 C30 -58.2(3) . . . . ? Co1 O29 C30 O31 -12.9(2) . . . . ? Co1 O29 C30 C32 165.95(11) . . . . ? O29 C30 O31 K1 -41.8(3) . . . . ? C32 C30 O31 K1 139.34(18) . . . . ? O16 K1 O31 C30 -148.4(2) 1_655 . . . ? O6 K1 O31 C30 67(4) 2_665 . . . ? O1S K1 O31 C30 111.9(2) . . . . ? O1S' K1 O31 C30 115.7(6) . . . . ? O6 K1 O31 C30 -8.8(2) . . . . ? O16 K1 O1S C1S -25.7(3) 1_655 . . . ? O6 K1 O1S C1S -117.7(3) 2_665 . . . ? O1S' K1 O1S C1S -60(8) . . . . ? O31 K1 O1S C1S 62.7(3) . . . . ? O6 K1 O1S C1S 162.6(3) . . . . ? K1 O1S C1S N1S 151.20(17) . . . . ? K1 O1S C1S C2S -30.8(4) . . . . ? C3S N1S C1S O1S -0.4(4) . . . . ? C4S N1S C1S O1S -179.5(3) . . . . ? C3S N1S C1S C2S -178.5(3) . . . . ? C4S N1S C1S C2S 2.4(3) . . . . ? O16 K1 O1S' C1S' -18(6) 1_655 . . . ? O6 K1 O1S' C1S' -110(6) 2_665 . . . ? O1S K1 O1S' C1S' 128(13) . . . . ? O31 K1 O1S' C1S' 71(6) . . . . ? O6 K1 O1S' C1S' 173(5) . . . . ? K1 O1S' C1S' N1S' -17(7) . . . . ? K1 O1S' C1S' C2S' 152(5) . . . . ? C3S' N1S' C1S' O1S' -7(4) . . . . ? C4S' N1S' C1S' O1S' 161(3) . . . . ? C3S' N1S' C1S' C2S' -176(3) . . . . ? C4S' N1S' C1S' C2S' -8(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 N7 H7 O29 0.88 2.53 3.0578(18) 119.0 . N17 H17 O29 0.88 2.08 2.8553(18) 146.6 . _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.988 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.079 #===END data_02078m _database_code_CSD 196775 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(K1) 1+, (C17 H34 Fe1 N5 O4) 1-' _chemical_formula_sum 'C17 H34 Fe K N5 O4' _chemical_formula_weight 467.44 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4396(6) _cell_length_b 15.1673(9) _cell_length_c 17.0455(10) _cell_angle_alpha 70.427(2) _cell_angle_beta 74.547(2) _cell_angle_gamma 70.066(2) _cell_volume 2355.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8136 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 30.00 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 0.847 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8036 _exptl_absorpt_correction_T_max 0.8979 _exptl_absorpt_process_details 'SADABS, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method '\w scan frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 237 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.17 _diffrn_reflns_number 19279 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 30.01 _reflns_number_total 12406 _reflns_number_gt 10250 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0540P)^2^+3.6000P] 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 12406 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1381 _refine_ls_wR_factor_gt 0.1325 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _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 K1 K -0.33722(7) 1.03872(4) -0.03278(4) 0.02774(14) Uani 1 1 d . . . K2 K 0.17150(6) 0.49248(4) 0.51355(3) 0.02155(12) Uani 1 1 d . . . Fe1A Fe 0.13701(4) 0.76047(3) 0.16104(2) 0.01777(9) Uani 1 1 d . . . N1A N 0.0467(2) 0.87388(15) 0.22962(13) 0.0195(4) Uani 1 1 d . . . C2A C -0.0282(3) 0.95964(19) 0.16918(16) 0.0228(5) Uani 1 1 d . . . H2AA H 0.0367 0.9977 0.1327 0.027 Uiso 1 1 calc R . . H2AB H -0.1026 1.0019 0.2012 0.027 Uiso 1 1 calc R . . C3A C -0.0915(3) 0.93107(19) 0.11358(17) 0.0233(5) Uani 1 1 d . . . H3AA H -0.1736 0.9090 0.1472 0.028 Uiso 1 1 calc R . . H3AB H -0.1218 0.9883 0.0664 0.028 Uiso 1 1 calc R . . N4A N 0.0105(2) 0.85255(16) 0.07964(14) 0.0219(4) Uani 1 1 d . . . C5A C -0.0207(3) 0.83899(19) 0.01358(16) 0.0222(5) Uani 1 1 d . . . O6A O -0.1282(2) 0.88702(14) -0.01791(12) 0.0252(4) Uani 1 1 d . . . N7A N 0.0796(3) 0.76955(19) -0.02271(16) 0.0308(5) Uani 1 1 d . . . H7AA H 0.1646 0.7544 -0.0136 0.037 Uiso 1 1 calc R . . C8A C 0.0543(3) 0.7194(2) -0.07525(18) 0.0299(6) Uani 1 1 d . . . C9A C 0.1889(4) 0.6398(3) -0.0895(2) 0.0481(9) Uani 1 1 d . . . H9AA H 0.2097 0.5947 -0.0350 0.072 Uiso 1 1 d R . . H9AB H 0.2648 0.6697 -0.1180 0.072 Uiso 1 1 d R . . H9AC H 0.1783 0.6041 -0.1248 0.072 Uiso 1 1 d R . . C10A C 0.0257(4) 0.7896(3) -0.1609(2) 0.0427(8) Uani 1 1 d . . . H10A H -0.0574 0.8429 -0.1526 0.064 Uiso 1 1 d R . . H10B H 0.0113 0.7548 -0.1956 0.064 Uiso 1 1 d R . . H10C H 0.1048 0.8160 -0.1895 0.064 Uiso 1 1 d R . . C11A C -0.0626(5) 0.6733(3) -0.0299(3) 0.0572(12) Uani 1 1 d . . . H11A H -0.1489 0.7244 -0.0217 0.086 Uiso 1 1 d R . . H11B H -0.0419 0.6297 0.0252 0.086 Uiso 1 1 d R . . H11C H -0.0728 0.6359 -0.0639 0.086 Uiso 1 1 d R . . C12A C -0.0496(3) 0.83011(19) 0.30096(16) 0.0231(5) Uani 1 1 d . . . H12A H -0.1304 0.8317 0.2800 0.028 Uiso 1 1 calc R . . H12B H -0.0834 0.8684 0.3430 0.028 Uiso 1 1 calc R . . C13A C 0.0235(3) 0.72481(19) 0.34284(16) 0.0229(5) Uani 1 1 d . . . H13A H 0.0976 0.7231 0.3699 0.027 Uiso 1 1 calc R . . H13B H -0.0432 0.6936 0.3868 0.027 Uiso 1 1 calc R . . N14A N 0.0827(2) 0.67298(15) 0.27703(13) 0.0193(4) Uani 1 1 d . . . C15A C 0.0919(3) 0.57777(18) 0.30332(16) 0.0191(5) Uani 1 1 d . . . O16A O 0.0640(2) 0.53050(13) 0.37970(11) 0.0217(4) Uani 1 1 d . . . N17A N 0.1271(3) 0.53234(16) 0.23958(14) 0.0271(5) Uani 1 1 d . . . H17A H 0.1024 0.5671 0.1904 0.033 Uiso 1 1 calc R . . C18A C 0.2042(3) 0.4283(2) 0.24945(18) 0.0281(6) Uani 1 1 d . . . C19A C 0.2440(5) 0.4161(3) 0.1599(2) 0.0572(12) Uani 1 1 d . . . H19A H 0.3043 0.4572 0.1249 0.086 Uiso 1 1 d R . . H19B H 0.1603 0.4354 0.1355 0.086 Uiso 1 1 d R . . H19C H 0.2929 0.3478 0.1618 0.086 Uiso 1 1 d R . . C20A C 0.3335(3) 0.4044(2) 0.2857(3) 0.0432(9) Uani 1 1 d . . . H20A H 0.3075 0.4126 0.3430 0.065 Uiso 1 1 d R . . H20B H 0.3897 0.4481 0.2499 0.065 Uiso 1 1 d R . . H20C H 0.3871 0.3368 0.2876 0.065 Uiso 1 1 d R . . C21A C 0.1123(3) 0.3632(2) 0.3037(2) 0.0303(6) Uani 1 1 d . . . H21A H 0.0820 0.3738 0.3602 0.045 Uiso 1 1 d R . . H21B H 0.1644 0.2949 0.3082 0.045 Uiso 1 1 d R . . H21C H 0.0313 0.3790 0.2777 0.045 Uiso 1 1 d R . . C22A C 0.1422(3) 0.9013(2) 0.26124(18) 0.0275(6) Uani 1 1 d . . . H22A H 0.0894 0.9517 0.2906 0.041 Uiso 1 1 d R . . H22B H 0.2087 0.9264 0.2136 0.041 Uiso 1 1 d R . . H22C H 0.1918 0.8439 0.3005 0.041 Uiso 1 1 d R . . O23A O 0.3428(2) 0.77015(14) 0.09848(12) 0.0249(4) Uani 1 1 d . . . C24A C 0.3727(3) 0.6924(2) 0.07692(16) 0.0243(5) Uani 1 1 d . . . O25A O 0.2838(2) 0.64683(15) 0.09385(12) 0.0273(4) Uani 1 1 d . . . C26A C 0.5148(3) 0.6524(3) 0.0310(2) 0.0351(7) Uani 1 1 d . . . H26A H 0.5065 0.6352 -0.0176 0.053 Uiso 1 1 d R . . H26B H 0.5648 0.5942 0.0694 0.053 Uiso 1 1 d R . . H26C H 0.5655 0.7017 0.0113 0.053 Uiso 1 1 d R . . Fe1B Fe 0.57998(4) 0.74216(2) 0.33249(2) 0.01663(9) Uani 1 1 d . . . N1B N 0.6530(2) 0.62467(15) 0.26871(13) 0.0189(4) Uani 1 1 d . . . C2B C 0.5205(3) 0.60854(19) 0.26969(16) 0.0216(5) Uani 1 1 d . . . H2BA H 0.5392 0.5483 0.2528 0.026 Uiso 1 1 calc R . . H2BB H 0.4696 0.6637 0.2283 0.026 Uiso 1 1 calc R . . C3B C 0.4318(3) 0.59952(19) 0.35771(16) 0.0225(5) Uani 1 1 d . . . H3BA H 0.3393 0.5963 0.3562 0.027 Uiso 1 1 calc R . . H3BB H 0.4760 0.5394 0.3981 0.027 Uiso 1 1 calc R . . N4B N 0.4184(2) 0.68471(16) 0.38412(13) 0.0203(4) Uani 1 1 d . . . C5B C 0.3207(3) 0.69835(19) 0.45246(16) 0.0215(5) Uani 1 1 d . . . O6B O 0.2533(2) 0.63902(15) 0.49739(12) 0.0265(4) Uani 1 1 d . . . N7B N 0.2964(2) 0.78625(17) 0.46876(15) 0.0260(5) Uani 1 1 d . . . H7BA H 0.3275 0.8316 0.4279 0.031 Uiso 1 1 calc R . . C8B C 0.2229(3) 0.8107(2) 0.54856(19) 0.0301(6) Uani 1 1 d . . . C9B C 0.2348(4) 0.9120(2) 0.5391(2) 0.0393(8) Uani 1 1 d . . . H9BA H 0.1948 0.9586 0.4901 0.059 Uiso 1 1 d R . . H9BB H 0.3325 0.9093 0.5310 0.059 Uiso 1 1 d R . . H9BC H 0.1848 0.9328 0.5902 0.059 Uiso 1 1 d R . . C10B C 0.2913(5) 0.7380(3) 0.6222(2) 0.0537(11) Uani 1 1 d . . . H10D H 0.2855 0.6729 0.6279 0.081 Uiso 1 1 d R . . H10E H 0.2438 0.7571 0.6744 0.081 Uiso 1 1 d R . . H10F H 0.3886 0.7372 0.6117 0.081 Uiso 1 1 d R . . C11B C 0.0713(4) 0.8155(3) 0.5619(3) 0.0578(12) Uani 1 1 d . . . H11D H 0.0629 0.7512 0.5674 0.087 Uiso 1 1 d R . . H11E H 0.0306 0.8629 0.5135 0.087 Uiso 1 1 d R . . H11F H 0.0225 0.8355 0.6136 0.087 Uiso 1 1 d R . . C12B C 0.7189(3) 0.67016(18) 0.18293(16) 0.0208(5) Uani 1 1 d . . . H12C H 0.7262 0.6319 0.1441 0.025 Uiso 1 1 calc R . . H12D H 0.8137 0.6684 0.1848 0.025 Uiso 1 1 calc R . . C13B C 0.6380(3) 0.77488(18) 0.14872(15) 0.0201(5) Uani 1 1 d . . . H13C H 0.6936 0.8065 0.0969 0.024 Uiso 1 1 calc R . . H13D H 0.5517 0.7764 0.1339 0.024 Uiso 1 1 calc R . . N14B N 0.6046(2) 0.82785(15) 0.21274(13) 0.0198(4) Uani 1 1 d . . . C15B C 0.5531(3) 0.92464(19) 0.18409(16) 0.0234(5) Uani 1 1 d . . . O16B O 0.5199(2) 0.96795(14) 0.11184(12) 0.0262(4) Uani 1 1 d . . . N17B N 0.5432(4) 0.97661(19) 0.23831(17) 0.0518(10) Uani 1 1 d . . . H17B H 0.5824 0.9442 0.2833 0.062 Uiso 1 1 calc R . . C18B C 0.4746(4) 1.0803(2) 0.22951(19) 0.0370(8) Uani 1 1 d . . . C19B C 0.4891(9) 1.0999(3) 0.3080(3) 0.113(3) Uani 1 1 d . . . H19D H 0.4414 1.0613 0.3583 0.170 Uiso 1 1 d R . . H19E H 0.4479 1.1693 0.3048 0.170 Uiso 1 1 d R . . H19F H 0.5873 1.0818 0.3116 0.170 Uiso 1 1 d R . . C20B C 0.5513(4) 1.1412(3) 0.1545(3) 0.0481(9) Uani 1 1 d . . . H20D H 0.5333 1.1381 0.1020 0.072 Uiso 1 1 d R . . H20E H 0.6508 1.1158 0.1556 0.072 Uiso 1 1 d R . . H20F H 0.5195 1.2089 0.1573 0.072 Uiso 1 1 d R . . C21B C 0.3266(5) 1.1061(4) 0.2214(5) 0.104(3) Uani 1 1 d . . . H21D H 0.3209 1.0920 0.1706 0.156 Uiso 1 1 d R . . H21E H 0.2839 1.1757 0.2170 0.156 Uiso 1 1 d R . . H21F H 0.2778 1.0678 0.2713 0.156 Uiso 1 1 d R . . C22B C 0.7502(3) 0.53172(19) 0.30446(17) 0.0245(5) Uani 1 1 d . . . H22D H 0.7735 0.4884 0.2680 0.037 Uiso 1 1 d R . . H22E H 0.7072 0.5010 0.3611 0.037 Uiso 1 1 d R . . H22F H 0.8346 0.5438 0.3081 0.037 Uiso 1 1 d R . . O23B O 0.7035(2) 0.69772(14) 0.42946(12) 0.0255(4) Uani 1 1 d . . . C24B C 0.6575(3) 0.78070(19) 0.44419(16) 0.0215(5) Uani 1 1 d . . . O25B O 0.5667(2) 0.84644(14) 0.40578(11) 0.0234(4) Uani 1 1 d . . . C26B C 0.7118(3) 0.7999(2) 0.50829(19) 0.0321(6) Uani 1 1 d . . . H26D H 0.7010 0.8698 0.4950 0.048 Uiso 1 1 d R . . H26E H 0.8100 0.7643 0.5069 0.048 Uiso 1 1 d R . . H26F H 0.6600 0.7780 0.5648 0.048 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0309(3) 0.0222(3) 0.0212(3) 0.0013(2) -0.0038(2) -0.0040(2) K2 0.0259(3) 0.0201(3) 0.0192(2) -0.00271(19) -0.0048(2) -0.0089(2) Fe1A 0.02068(17) 0.01564(17) 0.01496(16) -0.00312(12) -0.00110(13) -0.00502(13) N1A 0.0256(11) 0.0160(10) 0.0167(9) -0.0023(8) -0.0023(8) -0.0086(8) C2A 0.0298(13) 0.0167(12) 0.0201(11) -0.0045(9) -0.0009(10) -0.0071(10) C3A 0.0270(13) 0.0168(12) 0.0241(12) -0.0055(9) -0.0045(10) -0.0034(9) N4A 0.0256(11) 0.0188(10) 0.0202(10) -0.0066(8) -0.0037(8) -0.0035(8) C5A 0.0266(12) 0.0192(12) 0.0193(11) -0.0032(9) -0.0017(10) -0.0080(10) O6A 0.0292(10) 0.0232(9) 0.0215(9) -0.0023(7) -0.0068(8) -0.0071(8) N7A 0.0312(13) 0.0357(14) 0.0285(12) -0.0173(11) -0.0100(10) -0.0008(10) C8A 0.0402(16) 0.0285(15) 0.0231(13) -0.0113(11) -0.0053(12) -0.0080(12) C9A 0.057(2) 0.045(2) 0.0430(19) -0.0287(17) -0.0127(17) 0.0058(17) C10A 0.067(2) 0.0388(18) 0.0234(14) -0.0122(13) -0.0098(15) -0.0103(16) C11A 0.073(3) 0.050(2) 0.060(2) -0.031(2) 0.019(2) -0.038(2) C12A 0.0269(13) 0.0181(12) 0.0211(11) -0.0058(9) 0.0025(10) -0.0069(10) C13A 0.0314(13) 0.0170(12) 0.0182(11) -0.0048(9) -0.0008(10) -0.0066(10) N14A 0.0250(10) 0.0145(9) 0.0166(9) -0.0042(7) -0.0012(8) -0.0051(8) C15A 0.0208(11) 0.0179(11) 0.0181(11) -0.0047(9) -0.0031(9) -0.0050(9) O16A 0.0299(9) 0.0156(8) 0.0169(8) -0.0017(6) -0.0024(7) -0.0068(7) N17A 0.0459(14) 0.0153(10) 0.0169(10) -0.0037(8) -0.0044(10) -0.0058(9) C18A 0.0383(15) 0.0164(12) 0.0268(13) -0.0081(10) -0.0007(11) -0.0058(11) C19A 0.105(4) 0.0249(16) 0.0314(17) -0.0154(14) 0.0111(19) -0.0149(19) C20A 0.0283(15) 0.0252(15) 0.073(3) -0.0180(16) 0.0006(15) -0.0059(12) C21A 0.0346(15) 0.0178(13) 0.0386(16) -0.0073(11) -0.0081(12) -0.0063(11) C22A 0.0338(15) 0.0281(14) 0.0239(12) -0.0046(11) -0.0039(11) -0.0157(11) O23A 0.0233(9) 0.0264(10) 0.0228(9) -0.0059(7) -0.0027(7) -0.0058(7) C24A 0.0239(12) 0.0295(14) 0.0150(11) -0.0038(10) -0.0032(9) -0.0041(10) O25A 0.0285(10) 0.0253(10) 0.0251(9) -0.0079(8) 0.0009(8) -0.0067(8) C26A 0.0251(14) 0.0449(18) 0.0298(14) -0.0156(13) 0.0009(12) -0.0020(12) Fe1B 0.02096(17) 0.01370(16) 0.01429(16) -0.00178(12) -0.00237(13) -0.00611(13) N1B 0.0239(10) 0.0150(10) 0.0155(9) -0.0023(7) -0.0025(8) -0.0052(8) C2B 0.0276(13) 0.0210(12) 0.0179(11) -0.0055(9) -0.0038(10) -0.0087(10) C3B 0.0280(13) 0.0213(12) 0.0201(11) -0.0046(9) -0.0014(10) -0.0123(10) N4B 0.0246(10) 0.0175(10) 0.0194(10) -0.0037(8) -0.0022(8) -0.0092(8) C5B 0.0248(12) 0.0204(12) 0.0190(11) -0.0023(9) -0.0043(10) -0.0085(10) O6B 0.0313(10) 0.0282(10) 0.0223(9) -0.0059(8) 0.0027(8) -0.0174(8) N7B 0.0301(12) 0.0220(11) 0.0249(11) -0.0081(9) 0.0058(9) -0.0123(9) C8B 0.0342(15) 0.0279(14) 0.0287(14) -0.0132(11) 0.0066(12) -0.0131(12) C9B 0.0448(18) 0.0308(16) 0.0422(18) -0.0194(14) 0.0074(15) -0.0123(14) C10B 0.096(3) 0.039(2) 0.0294(16) -0.0116(15) -0.0105(19) -0.021(2) C11B 0.0345(18) 0.065(3) 0.080(3) -0.043(2) 0.0231(19) -0.0227(18) C12B 0.0266(12) 0.0149(11) 0.0186(11) -0.0047(9) -0.0001(9) -0.0055(9) C13B 0.0270(12) 0.0171(11) 0.0153(10) -0.0037(9) -0.0008(9) -0.0079(9) N14B 0.0273(11) 0.0151(10) 0.0144(9) -0.0027(7) -0.0019(8) -0.0054(8) C15B 0.0294(13) 0.0183(12) 0.0175(11) -0.0041(9) -0.0013(10) -0.0033(10) O16B 0.0346(11) 0.0188(9) 0.0182(8) 0.0000(7) -0.0061(8) -0.0024(8) N17B 0.110(3) 0.0131(12) 0.0212(12) -0.0032(9) -0.0207(15) 0.0024(14) C18B 0.063(2) 0.0126(12) 0.0272(14) -0.0074(10) 0.0008(14) -0.0054(13) C19B 0.271(9) 0.0231(19) 0.034(2) -0.0122(16) -0.033(4) -0.017(3) C20B 0.062(2) 0.0305(17) 0.051(2) -0.0146(16) 0.0042(18) -0.0192(16) C21B 0.040(2) 0.065(3) 0.223(8) -0.097(5) 0.025(3) -0.014(2) C22B 0.0292(13) 0.0167(12) 0.0249(12) -0.0034(10) -0.0089(10) -0.0021(10) O23B 0.0300(10) 0.0217(9) 0.0247(9) -0.0067(7) -0.0069(8) -0.0050(8) C24B 0.0254(12) 0.0231(12) 0.0160(10) -0.0035(9) -0.0003(9) -0.0110(10) O25B 0.0302(10) 0.0198(9) 0.0190(8) -0.0036(7) -0.0037(7) -0.0076(7) C26B 0.0410(17) 0.0347(16) 0.0259(13) -0.0130(12) -0.0082(12) -0.0102(13) _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 K1 O6A 2.569(2) . ? K1 O16B 2.610(2) 1_455 ? K1 O16B 2.656(2) 2_575 ? K1 O23A 2.721(2) 2_575 ? K2 O6B 2.550(2) . ? K2 O16A 2.615(2) . ? K2 O23B 2.683(2) 2_666 ? K2 O16A 2.6927(19) 2_566 ? Fe1A N4A 2.010(2) . ? Fe1A N14A 2.037(2) . ? Fe1A O23A 2.1600(19) . ? Fe1A N1A 2.207(2) . ? Fe1A O25A 2.284(2) . ? N1A C22A 1.475(4) . ? N1A C12A 1.481(3) . ? N1A C2A 1.484(3) . ? C2A C3A 1.525(4) . ? C2A H2AA 0.9900 . ? C2A H2AB 0.9900 . ? C3A N4A 1.468(3) . ? C3A H3AA 0.9900 . ? C3A H3AB 0.9900 . ? N4A C5A 1.346(4) . ? C5A O6A 1.257(3) . ? C5A N7A 1.388(4) . ? N7A C8A 1.472(4) . ? N7A H7AA 0.8800 . ? C8A C11A 1.515(5) . ? C8A C10A 1.525(4) . ? C8A C9A 1.533(5) . ? C9A H9AA 0.9800 . ? C9A H9AB 0.9800 . ? C9A H9AC 0.9800 . ? C10A H10A 0.9800 . ? C10A H10B 0.9800 . ? C10A H10C 0.9800 . ? C11A H11A 0.9800 . ? C11A H11B 0.9800 . ? C11A H11C 0.9800 . ? C12A C13A 1.529(4) . ? C12A H12A 0.9900 . ? C12A H12B 0.9900 . ? C13A N14A 1.466(3) . ? C13A H13A 0.9900 . ? C13A H13B 0.9900 . ? N14A C15A 1.338(3) . ? C15A O16A 1.268(3) . ? C15A N17A 1.381(3) . ? O16A K2 2.6927(19) 2_566 ? N17A C18A 1.481(3) . ? N17A H17A 0.8800 . ? C18A C20A 1.515(5) . ? C18A C21A 1.520(4) . ? C18A C19A 1.529(4) . ? C19A H19A 0.9800 . ? C19A H19B 0.9800 . ? C19A H19C 0.9800 . ? C20A H20A 0.9800 . ? C20A H20B 0.9800 . ? C20A H20C 0.9800 . ? C21A H21A 0.9800 . ? C21A H21B 0.9800 . ? C21A H21C 0.9800 . ? C22A H22A 0.9800 . ? C22A H22B 0.9800 . ? C22A H22C 0.9800 . ? O23A C24A 1.265(4) . ? O23A K1 2.721(2) 2_575 ? C24A O25A 1.259(4) . ? C24A C26A 1.506(4) . ? C26A H26A 0.9800 . ? C26A H26B 0.9800 . ? C26A H26C 0.9800 . ? Fe1B N4B 2.019(2) . ? Fe1B N14B 2.023(2) . ? Fe1B O23B 2.155(2) . ? Fe1B N1B 2.206(2) . ? Fe1B O25B 2.272(2) . ? N1B C22B 1.472(3) . ? N1B C2B 1.480(3) . ? N1B C12B 1.483(3) . ? C2B C3B 1.529(3) . ? C2B H2BA 0.9900 . ? C2B H2BB 0.9900 . ? C3B N4B 1.458(3) . ? C3B H3BA 0.9900 . ? C3B H3BB 0.9900 . ? N4B C5B 1.351(3) . ? C5B O6B 1.254(3) . ? C5B N7B 1.378(4) . ? N7B C8B 1.471(4) . ? N7B H7BA 0.8800 . ? C8B C11B 1.517(5) . ? C8B C10B 1.521(5) . ? C8B C9B 1.536(4) . ? C9B H9BA 0.9800 . ? C9B H9BB 0.9800 . ? C9B H9BC 0.9800 . ? C10B H10D 0.9800 . ? C10B H10E 0.9800 . ? C10B H10F 0.9800 . ? C11B H11D 0.9800 . ? C11B H11E 0.9800 . ? C11B H11F 0.9800 . ? C12B C13B 1.517(3) . ? C12B H12C 0.9900 . ? C12B H12D 0.9900 . ? C13B N14B 1.467(3) . ? C13B H13C 0.9900 . ? C13B H13D 0.9900 . ? N14B C15B 1.343(3) . ? C15B O16B 1.264(3) . ? C15B N17B 1.367(4) . ? O16B K1 2.610(2) 1_655 ? O16B K1 2.656(2) 2_575 ? N17B C18B 1.462(4) . ? N17B H17B 0.8800 . ? C18B C21B 1.491(6) . ? C18B C20B 1.516(5) . ? C18B C19B 1.520(6) . ? C19B H19D 0.9800 . ? C19B H19E 0.9800 . ? C19B H19F 0.9800 . ? C20B H20D 0.9800 . ? C20B H20E 0.9800 . ? C20B H20F 0.9800 . ? C21B H21D 0.9800 . ? C21B H21E 0.9800 . ? C21B H21F 0.9800 . ? C22B H22D 0.9800 . ? C22B H22E 0.9800 . ? C22B H22F 0.9800 . ? O23B C24B 1.270(3) . ? O23B K2 2.683(2) 2_666 ? C24B O25B 1.253(3) . ? C24B C26B 1.502(4) . ? C26B H26D 0.9800 . ? C26B H26E 0.9800 . ? C26B H26F 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 O6A K1 O16B 93.83(6) . 1_455 ? O6A K1 O16B 113.59(7) . 2_575 ? O16B K1 O16B 89.46(6) 1_455 2_575 ? O6A K1 O23A 129.28(7) . 2_575 ? O16B K1 O23A 124.60(6) 1_455 2_575 ? O16B K1 O23A 99.84(6) 2_575 2_575 ? O6B K2 O16A 106.73(6) . . ? O6B K2 O23B 128.93(7) . 2_666 ? O16A K2 O23B 112.41(6) . 2_666 ? O6B K2 O16A 119.28(6) . 2_566 ? O16A K2 O16A 93.05(6) . 2_566 ? O23B K2 O16A 90.39(6) 2_666 2_566 ? N4A Fe1A N14A 127.00(9) . . ? N4A Fe1A O23A 105.81(8) . . ? N14A Fe1A O23A 127.17(8) . . ? N4A Fe1A N1A 83.70(9) . . ? N14A Fe1A N1A 82.28(8) . . ? O23A Fe1A N1A 107.41(8) . . ? N4A Fe1A O25A 105.59(8) . . ? N14A Fe1A O25A 100.64(8) . . ? O23A Fe1A O25A 58.97(8) . . ? N1A Fe1A O25A 164.90(8) . . ? C22A N1A C12A 110.4(2) . . ? C22A N1A C2A 110.3(2) . . ? C12A N1A C2A 111.8(2) . . ? C22A N1A Fe1A 117.55(17) . . ? C12A N1A Fe1A 101.89(15) . . ? C2A N1A Fe1A 104.58(15) . . ? N1A C2A C3A 112.5(2) . . ? N1A C2A H2AA 109.1 . . ? C3A C2A H2AA 109.1 . . ? N1A C2A H2AB 109.1 . . ? C3A C2A H2AB 109.1 . . ? H2AA C2A H2AB 107.8 . . ? N4A C3A C2A 110.0(2) . . ? N4A C3A H3AA 109.7 . . ? C2A C3A H3AA 109.7 . . ? N4A C3A H3AB 109.7 . . ? C2A C3A H3AB 109.7 . . ? H3AA C3A H3AB 108.2 . . ? C5A N4A C3A 114.7(2) . . ? C5A N4A Fe1A 129.69(18) . . ? C3A N4A Fe1A 112.54(17) . . ? O6A C5A N4A 124.7(2) . . ? O6A C5A N7A 120.0(2) . . ? N4A C5A N7A 115.2(2) . . ? C5A O6A K1 148.42(18) . . ? C5A N7A C8A 124.9(3) . . ? C5A N7A H7AA 117.6 . . ? C8A N7A H7AA 117.6 . . ? N7A C8A C11A 110.8(3) . . ? N7A C8A C10A 110.5(3) . . ? C11A C8A C10A 111.5(3) . . ? N7A C8A C9A 105.8(3) . . ? C11A C8A C9A 109.6(3) . . ? C10A C8A C9A 108.4(3) . . ? C8A C9A H9AA 109.5 . . ? C8A C9A H9AB 109.5 . . ? H9AA C9A H9AB 109.5 . . ? C8A C9A H9AC 109.5 . . ? H9AA C9A H9AC 109.5 . . ? H9AB C9A H9AC 109.5 . . ? C8A C10A H10A 109.5 . . ? C8A C10A H10B 109.5 . . ? H10A C10A H10B 109.5 . . ? C8A C10A H10C 109.5 . . ? H10A C10A H10C 109.5 . . ? H10B C10A H10C 109.5 . . ? C8A C11A H11A 109.5 . . ? C8A C11A H11B 109.5 . . ? H11A C11A H11B 109.5 . . ? C8A C11A H11C 109.5 . . ? H11A C11A H11C 109.5 . . ? H11B C11A H11C 109.5 . . ? N1A C12A C13A 110.2(2) . . ? N1A C12A H12A 109.6 . . ? C13A C12A H12A 109.6 . . ? N1A C12A H12B 109.6 . . ? C13A C12A H12B 109.6 . . ? H12A C12A H12B 108.1 . . ? N14A C13A C12A 107.8(2) . . ? N14A C13A H13A 110.1 . . ? C12A C13A H13A 110.1 . . ? N14A C13A H13B 110.1 . . ? C12A C13A H13B 110.1 . . ? H13A C13A H13B 108.5 . . ? C15A N14A C13A 115.1(2) . . ? C15A N14A Fe1A 131.63(17) . . ? C13A N14A Fe1A 113.27(16) . . ? O16A C15A N14A 124.9(2) . . ? O16A C15A N17A 120.0(2) . . ? N14A C15A N17A 114.9(2) . . ? C15A O16A K2 132.76(17) . . ? C15A O16A K2 134.36(16) . 2_566 ? K2 O16A K2 86.95(6) . 2_566 ? C15A N17A C18A 123.6(2) . . ? C15A N17A H17A 118.2 . . ? C18A N17A H17A 118.2 . . ? N17A C18A C20A 110.4(3) . . ? N17A C18A C21A 110.8(2) . . ? C20A C18A C21A 111.5(3) . . ? N17A C18A C19A 104.9(2) . . ? C20A C18A C19A 109.8(3) . . ? C21A C18A C19A 109.3(3) . . ? C18A C19A H19A 109.5 . . ? C18A C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C18A C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? C18A C20A H20A 109.5 . . ? C18A C20A H20B 109.5 . . ? H20A C20A H20B 109.5 . . ? C18A C20A H20C 109.5 . . ? H20A C20A H20C 109.5 . . ? H20B C20A H20C 109.5 . . ? C18A C21A H21A 109.5 . . ? C18A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C18A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? N1A C22A H22A 109.5 . . ? N1A C22A H22B 109.5 . . ? H22A C22A H22B 109.5 . . ? N1A C22A H22C 109.5 . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? C24A O23A Fe1A 93.02(17) . . ? C24A O23A K1 141.51(17) . 2_575 ? Fe1A O23A K1 108.85(8) . 2_575 ? O25A C24A O23A 120.4(2) . . ? O25A C24A C26A 118.7(3) . . ? O23A C24A C26A 120.9(3) . . ? C24A O25A Fe1A 87.54(16) . . ? C24A C26A H26A 109.5 . . ? C24A C26A H26B 109.5 . . ? H26A C26A H26B 109.5 . . ? C24A C26A H26C 109.5 . . ? H26A C26A H26C 109.5 . . ? H26B C26A H26C 109.5 . . ? N4B Fe1B N14B 123.08(9) . . ? N4B Fe1B O23B 106.69(8) . . ? N14B Fe1B O23B 130.20(9) . . ? N4B Fe1B N1B 82.69(8) . . ? N14B Fe1B N1B 83.09(8) . . ? O23B Fe1B N1B 106.49(8) . . ? N4B Fe1B O25B 107.83(8) . . ? N14B Fe1B O25B 100.40(8) . . ? O23B Fe1B O25B 59.19(7) . . ? N1B Fe1B O25B 163.80(8) . . ? C22B N1B C2B 110.0(2) . . ? C22B N1B C12B 109.0(2) . . ? C2B N1B C12B 113.1(2) . . ? C22B N1B Fe1B 119.93(17) . . ? C2B N1B Fe1B 101.00(15) . . ? C12B N1B Fe1B 103.63(15) . . ? N1B C2B C3B 110.8(2) . . ? N1B C2B H2BA 109.5 . . ? C3B C2B H2BA 109.5 . . ? N1B C2B H2BB 109.5 . . ? C3B C2B H2BB 109.5 . . ? H2BA C2B H2BB 108.1 . . ? N4B C3B C2B 108.0(2) . . ? N4B C3B H3BA 110.1 . . ? C2B C3B H3BA 110.1 . . ? N4B C3B H3BB 110.1 . . ? C2B C3B H3BB 110.1 . . ? H3BA C3B H3BB 108.4 . . ? C5B N4B C3B 115.4(2) . . ? C5B N4B Fe1B 128.78(19) . . ? C3B N4B Fe1B 113.66(16) . . ? O6B C5B N4B 124.6(3) . . ? O6B C5B N7B 121.2(2) . . ? N4B C5B N7B 114.2(2) . . ? C5B O6B K2 148.49(18) . . ? C5B N7B C8B 125.6(2) . . ? C5B N7B H7BA 117.2 . . ? C8B N7B H7BA 117.2 . . ? N7B C8B C11B 110.3(3) . . ? N7B C8B C10B 110.5(3) . . ? C11B C8B C10B 111.6(3) . . ? N7B C8B C9B 106.1(2) . . ? C11B C8B C9B 109.0(3) . . ? C10B C8B C9B 109.1(3) . . ? C8B C9B H9BA 109.5 . . ? C8B C9B H9BB 109.5 . . ? H9BA C9B H9BB 109.5 . . ? C8B C9B H9BC 109.5 . . ? H9BA C9B H9BC 109.5 . . ? H9BB C9B H9BC 109.5 . . ? C8B C10B H10D 109.5 . . ? C8B C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? C8B C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? C8B C11B H11D 109.5 . . ? C8B C11B H11E 109.5 . . ? H11D C11B H11E 109.5 . . ? C8B C11B H11F 109.5 . . ? H11D C11B H11F 109.5 . . ? H11E C11B H11F 109.5 . . ? N1B C12B C13B 112.2(2) . . ? N1B C12B H12C 109.2 . . ? C13B C12B H12C 109.2 . . ? N1B C12B H12D 109.2 . . ? C13B C12B H12D 109.2 . . ? H12C C12B H12D 107.9 . . ? N14B C13B C12B 109.6(2) . . ? N14B C13B H13C 109.8 . . ? C12B C13B H13C 109.8 . . ? N14B C13B H13D 109.8 . . ? C12B C13B H13D 109.8 . . ? H13C C13B H13D 108.2 . . ? C15B N14B C13B 114.2(2) . . ? C15B N14B Fe1B 128.71(17) . . ? C13B N14B Fe1B 113.16(15) . . ? O16B C15B N14B 124.7(3) . . ? O16B C15B N17B 120.4(2) . . ? N14B C15B N17B 114.9(2) . . ? C15B O16B K1 131.44(19) . 1_655 ? C15B O16B K1 134.04(19) . 2_575 ? K1 O16B K1 90.54(6) 1_655 2_575 ? C15B N17B C18B 126.9(3) . . ? C15B N17B H17B 116.5 . . ? C18B N17B H17B 116.5 . . ? N17B C18B C21B 112.0(3) . . ? N17B C18B C20B 110.2(3) . . ? C21B C18B C20B 110.5(4) . . ? N17B C18B C19B 105.6(3) . . ? C21B C18B C19B 111.5(5) . . ? C20B C18B C19B 106.8(4) . . ? C18B C19B H19D 109.5 . . ? C18B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C18B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C18B C20B H20D 109.5 . . ? C18B C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? C18B C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? C18B C21B H21D 109.5 . . ? C18B C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? C18B C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? N1B C22B H22D 109.5 . . ? N1B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? N1B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? C24B O23B Fe1B 92.64(16) . . ? C24B O23B K2 146.79(17) . 2_666 ? Fe1B O23B K2 118.47(8) . 2_666 ? O25B C24B O23B 120.3(2) . . ? O25B C24B C26B 119.9(3) . . ? O23B C24B C26B 119.8(2) . . ? C24B O25B Fe1B 87.75(16) . . ? C24B C26B H26D 109.5 . . ? C24B C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? C24B C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 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 N4A Fe1A N1A C22A -134.95(18) . . . . ? N14A Fe1A N1A C22A 96.30(18) . . . . ? O23A Fe1A N1A C22A -30.32(19) . . . . ? O25A Fe1A N1A C22A -6.0(4) . . . . ? N4A Fe1A N1A C12A 104.24(17) . . . . ? N14A Fe1A N1A C12A -24.52(16) . . . . ? O23A Fe1A N1A C12A -151.13(15) . . . . ? O25A Fe1A N1A C12A -126.8(3) . . . . ? N4A Fe1A N1A C2A -12.32(16) . . . . ? N14A Fe1A N1A C2A -141.07(17) . . . . ? O23A Fe1A N1A C2A 92.32(16) . . . . ? O25A Fe1A N1A C2A 116.7(3) . . . . ? C22A N1A C2A C3A 161.5(2) . . . . ? C12A N1A C2A C3A -75.2(3) . . . . ? Fe1A N1A C2A C3A 34.2(2) . . . . ? N1A C2A C3A N4A -46.8(3) . . . . ? C2A C3A N4A C5A -163.6(2) . . . . ? C2A C3A N4A Fe1A 34.2(3) . . . . ? N14A Fe1A N4A C5A -95.6(2) . . . . ? O23A Fe1A N4A C5A 82.7(2) . . . . ? N1A Fe1A N4A C5A -171.0(2) . . . . ? O25A Fe1A N4A C5A 21.2(3) . . . . ? N14A Fe1A N4A C3A 63.3(2) . . . . ? O23A Fe1A N4A C3A -118.47(18) . . . . ? N1A Fe1A N4A C3A -12.11(18) . . . . ? O25A Fe1A N4A C3A -179.97(17) . . . . ? C3A N4A C5A O6A -0.9(4) . . . . ? Fe1A N4A C5A O6A 157.6(2) . . . . ? C3A N4A C5A N7A 175.7(2) . . . . ? Fe1A N4A C5A N7A -25.8(4) . . . . ? N4A C5A O6A K1 16.1(5) . . . . ? N7A C5A O6A K1 -160.4(2) . . . . ? O16B K1 O6A C5A -79.7(3) 1_455 . . . ? O16B K1 O6A C5A -170.8(3) 2_575 . . . ? O23A K1 O6A C5A 62.5(3) 2_575 . . . ? O6A C5A N7A C8A -23.9(4) . . . . ? N4A C5A N7A C8A 159.3(3) . . . . ? C5A N7A C8A C11A -53.1(4) . . . . ? C5A N7A C8A C10A 71.0(4) . . . . ? C5A N7A C8A C9A -171.8(3) . . . . ? C22A N1A C12A C13A -77.5(3) . . . . ? C2A N1A C12A C13A 159.3(2) . . . . ? Fe1A N1A C12A C13A 48.2(2) . . . . ? N1A C12A C13A N14A -54.2(3) . . . . ? C12A C13A N14A C15A -150.2(2) . . . . ? C12A C13A N14A Fe1A 30.1(3) . . . . ? N4A Fe1A N14A C15A 101.0(2) . . . . ? O23A Fe1A N14A C15A -76.9(3) . . . . ? N1A Fe1A N14A C15A 177.1(3) . . . . ? O25A Fe1A N14A C15A -17.9(3) . . . . ? N4A Fe1A N14A C13A -79.3(2) . . . . ? O23A Fe1A N14A C13A 102.84(19) . . . . ? N1A Fe1A N14A C13A -3.20(18) . . . . ? O25A Fe1A N14A C13A 161.79(18) . . . . ? C13A N14A C15A O16A -5.7(4) . . . . ? Fe1A N14A C15A O16A 173.97(19) . . . . ? C13A N14A C15A N17A 170.4(2) . . . . ? Fe1A N14A C15A N17A -9.9(4) . . . . ? N14A C15A O16A K2 -62.7(3) . . . . ? N17A C15A O16A K2 121.4(2) . . . . ? N14A C15A O16A K2 80.7(3) . . . 2_566 ? N17A C15A O16A K2 -95.2(3) . . . 2_566 ? O6B K2 O16A C15A 32.9(2) . . . . ? O23B K2 O16A C15A -113.6(2) 2_666 . . . ? O16A K2 O16A C15A 154.7(2) 2_566 . . . ? O6B K2 O16A K2 -121.83(6) . . . 2_566 ? O23B K2 O16A K2 91.68(6) 2_666 . . 2_566 ? O16A K2 O16A K2 0.0 2_566 . . 2_566 ? O16A C15A N17A C18A -33.1(4) . . . . ? N14A C15A N17A C18A 150.6(3) . . . . ? C15A N17A C18A C20A -50.8(4) . . . . ? C15A N17A C18A C21A 73.2(4) . . . . ? C15A N17A C18A C19A -169.1(3) . . . . ? N4A Fe1A O23A C24A -100.43(16) . . . . ? N14A Fe1A O23A C24A 77.83(18) . . . . ? N1A Fe1A O23A C24A 171.33(15) . . . . ? O25A Fe1A O23A C24A -1.47(15) . . . . ? N4A Fe1A O23A K1 47.38(10) . . . 2_575 ? N14A Fe1A O23A K1 -134.36(9) . . . 2_575 ? N1A Fe1A O23A K1 -40.86(10) . . . 2_575 ? O25A Fe1A O23A K1 146.34(11) . . . 2_575 ? Fe1A O23A C24A O25A 2.6(3) . . . . ? K1 O23A C24A O25A -123.2(3) 2_575 . . . ? Fe1A O23A C24A C26A -177.1(2) . . . . ? K1 O23A C24A C26A 57.0(4) 2_575 . . . ? O23A C24A O25A Fe1A -2.5(2) . . . . ? C26A C24A O25A Fe1A 177.3(2) . . . . ? N4A Fe1A O25A C24A 100.80(16) . . . . ? N14A Fe1A O25A C24A -125.71(16) . . . . ? O23A Fe1A O25A C24A 1.47(15) . . . . ? N1A Fe1A O25A C24A -25.9(4) . . . . ? N4B Fe1B N1B C22B -95.74(19) . . . . ? N14B Fe1B N1B C22B 139.5(2) . . . . ? O23B Fe1B N1B C22B 9.6(2) . . . . ? O25B Fe1B N1B C22B 35.9(4) . . . . ? N4B Fe1B N1B C2B 25.22(14) . . . . ? N14B Fe1B N1B C2B -99.52(15) . . . . ? O23B Fe1B N1B C2B 130.52(14) . . . . ? O25B Fe1B N1B C2B 156.9(2) . . . . ? N4B Fe1B N1B C12B 142.52(17) . . . . ? N14B Fe1B N1B C12B 17.77(16) . . . . ? O23B Fe1B N1B C12B -112.18(16) . . . . ? O25B Fe1B N1B C12B -85.8(3) . . . . ? C22B N1B C2B C3B 79.6(3) . . . . ? C12B N1B C2B C3B -158.2(2) . . . . ? Fe1B N1B C2B C3B -48.1(2) . . . . ? N1B C2B C3B N4B 53.3(3) . . . . ? C2B C3B N4B C5B 167.0(2) . . . . ? C2B C3B N4B Fe1B -28.2(3) . . . . ? N14B Fe1B N4B C5B -119.2(2) . . . . ? O23B Fe1B N4B C5B 58.9(2) . . . . ? N1B Fe1B N4B C5B 164.0(2) . . . . ? O25B Fe1B N4B C5B -3.4(2) . . . . ? N14B Fe1B N4B C3B 78.51(19) . . . . ? O23B Fe1B N4B C3B -103.38(17) . . . . ? N1B Fe1B N4B C3B 1.71(17) . . . . ? O25B Fe1B N4B C3B -165.65(16) . . . . ? C3B N4B C5B O6B 7.1(4) . . . . ? Fe1B N4B C5B O6B -154.9(2) . . . . ? C3B N4B C5B N7B -171.1(2) . . . . ? Fe1B N4B C5B N7B 26.8(3) . . . . ? N4B C5B O6B K2 -17.9(5) . . . . ? N7B C5B O6B K2 160.3(2) . . . . ? O16A K2 O6B C5B -50.6(4) . . . . ? O23B K2 O6B C5B 88.4(4) 2_666 . . . ? O16A K2 O6B C5B -154.0(3) 2_566 . . . ? O6B C5B N7B C8B 17.5(4) . . . . ? N4B C5B N7B C8B -164.2(3) . . . . ? C5B N7B C8B C11B -67.6(4) . . . . ? C5B N7B C8B C10B 56.4(4) . . . . ? C5B N7B C8B C9B 174.5(3) . . . . ? C22B N1B C12B C13B -168.5(2) . . . . ? C2B N1B C12B C13B 68.8(3) . . . . ? Fe1B N1B C12B C13B -39.7(2) . . . . ? N1B C12B C13B N14B 48.5(3) . . . . ? C12B C13B N14B C15B 169.7(2) . . . . ? C12B C13B N14B Fe1B -30.7(3) . . . . ? N4B Fe1B N14B C15B 86.5(3) . . . . ? O23B Fe1B N14B C15B -91.1(3) . . . . ? N1B Fe1B N14B C15B 163.1(3) . . . . ? O25B Fe1B N14B C15B -32.9(3) . . . . ? N4B Fe1B N14B C13B -69.5(2) . . . . ? O23B Fe1B N14B C13B 112.89(18) . . . . ? N1B Fe1B N14B C13B 7.10(17) . . . . ? O25B Fe1B N14B C13B 171.10(17) . . . . ? C13B N14B C15B O16B 7.8(4) . . . . ? Fe1B N14B C15B O16B -147.9(2) . . . . ? C13B N14B C15B N17B -169.5(3) . . . . ? Fe1B N14B C15B N17B 34.7(4) . . . . ? N14B C15B O16B K1 -89.4(3) . . . 1_655 ? N17B C15B O16B K1 87.8(3) . . . 1_655 ? N14B C15B O16B K1 61.2(4) . . . 2_575 ? N17B C15B O16B K1 -121.6(3) . . . 2_575 ? O16B C15B N17B C18B 11.5(6) . . . . ? N14B C15B N17B C18B -171.1(3) . . . . ? C15B N17B C18B C21B 56.3(6) . . . . ? C15B N17B C18B C20B -67.2(5) . . . . ? C15B N17B C18B C19B 177.9(5) . . . . ? N4B Fe1B O23B C24B -102.73(16) . . . . ? N14B Fe1B O23B C24B 75.19(18) . . . . ? N1B Fe1B O23B C24B 170.12(15) . . . . ? O25B Fe1B O23B C24B -1.58(14) . . . . ? N4B Fe1B O23B K2 65.19(11) . . . 2_666 ? N14B Fe1B O23B K2 -116.89(11) . . . 2_666 ? N1B Fe1B O23B K2 -21.96(11) . . . 2_666 ? O25B Fe1B O23B K2 166.34(12) . . . 2_666 ? Fe1B O23B C24B O25B 2.9(3) . . . . ? K2 O23B C24B O25B -157.5(2) 2_666 . . . ? Fe1B O23B C24B C26B -177.4(2) . . . . ? K2 O23B C24B C26B 22.2(5) 2_666 . . . ? O23B C24B O25B Fe1B -2.7(2) . . . . ? C26B C24B O25B Fe1B 177.6(2) . . . . ? N4B Fe1B O25B C24B 100.77(16) . . . . ? N14B Fe1B O25B C24B -129.29(15) . . . . ? O23B Fe1B O25B C24B 1.60(14) . . . . ? N1B Fe1B O25B C24B -28.1(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 N7A H7AA O25A 0.88 2.32 3.005(3) 134.4 . N17A H17A O25A 0.88 2.51 2.957(3) 111.9 . N7B H7BA O25B 0.88 2.50 3.071(3) 123.2 . N17B H17B O25B 0.88 2.12 2.894(3) 146.4 . _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 1.319 _refine_diff_density_min -0.530 _refine_diff_density_rms 0.097 #===END data_02090m _database_code_CSD 196776 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(K1) 1+, (C17 H34 Co N5 O4) 1-, (C4 H9 N O)' _chemical_formula_sum 'C21 H43 Co K N6 O5' _chemical_formula_weight 557.64 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' K K 0.2009 0.2494 '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 1 21/n 1' 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 16.3720(9) _cell_length_b 11.1959(6) _cell_length_c 16.8233(9) _cell_angle_alpha 90.00 _cell_angle_beta 113.305(2) _cell_angle_gamma 90.00 _cell_volume 2832.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5349 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 30.0 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1188 _exptl_absorpt_coefficient_mu 0.792 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8087 _exptl_absorpt_correction_T_max 0.8972 _exptl_absorpt_process_details 'SADABS, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method '\w scan frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 286 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.06 _diffrn_reflns_number 23078 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0243 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 30.51 _reflns_number_total 8252 _reflns_number_gt 6987 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0740P)^2^+1.8200P] 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 8252 _refine_ls_number_parameters 362 _refine_ls_number_restraints 194 _refine_ls_R_factor_all 0.0535 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1302 _refine_ls_wR_factor_gt 0.1239 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.064 _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 K1 K 0.48465(4) 0.10263(4) 0.40750(3) 0.03842(13) Uani 1 1 d D . . Co1 Co 0.524241(14) 0.39100(2) 0.698536(14) 0.01618(8) Uani 1 1 d . . . N1 N 0.65240(9) 0.40877(14) 0.69731(10) 0.0193(3) Uani 1 1 d . . . C2 C 0.67996(11) 0.28432(17) 0.69136(12) 0.0236(3) Uani 1 1 d . . . H2A H 0.7016 0.2468 0.7493 0.028 Uiso 1 1 calc R . . H2B H 0.7295 0.2845 0.6716 0.028 Uiso 1 1 calc R . . C3 C 0.60264(11) 0.21160(17) 0.62841(13) 0.0240(3) Uani 1 1 d . . . H3A H 0.5918 0.2340 0.5682 0.029 Uiso 1 1 calc R . . H3B H 0.6174 0.1255 0.6359 0.029 Uiso 1 1 calc R . . N4 N 0.52257(9) 0.23464(14) 0.64496(10) 0.0200(3) Uani 1 1 d . A . C5 C 0.45112(12) 0.17014(17) 0.59629(12) 0.0236(3) Uani 1 1 d . . . O6 O 0.44959(10) 0.10029(15) 0.53696(12) 0.0396(4) Uani 1 1 d . . . N7 N 0.37780(10) 0.17998(15) 0.61662(10) 0.0231(3) Uani 1 1 d . A . H7 H 0.3862 0.1970 0.6704 0.028 Uiso 1 1 calc R . . C8 C 0.28544(11) 0.16334(17) 0.55251(12) 0.0225(3) Uani 1 1 d . . . C9 C 0.22590(13) 0.1948(2) 0.60022(15) 0.0352(5) Uani 1 1 d . A . H9A H 0.1634 0.1903 0.5599 0.053 Uiso 1 1 d R . . H9B H 0.2394 0.2760 0.6234 0.053 Uiso 1 1 d R . . H9C H 0.2366 0.1384 0.6478 0.053 Uiso 1 1 d R . . C10 C 0.26726(14) 0.03317(18) 0.52225(14) 0.0310(4) Uani 1 1 d . A . H10A H 0.2044 0.0242 0.4837 0.047 Uiso 1 1 d R . . H10B H 0.2811 -0.0193 0.5725 0.047 Uiso 1 1 d R . . H10C H 0.3045 0.0115 0.4910 0.047 Uiso 1 1 d R . . C11 C 0.26561(13) 0.24711(19) 0.47548(13) 0.0297(4) Uani 1 1 d . A . H11A H 0.2040 0.2358 0.4343 0.045 Uiso 1 1 d R . . H11B H 0.3060 0.2293 0.4469 0.045 Uiso 1 1 d R . . H11C H 0.2741 0.3301 0.4958 0.045 Uiso 1 1 d R . . C12 C 0.63349(11) 0.47767(17) 0.61644(11) 0.0216(3) Uani 1 1 d . . . H12A H 0.6055 0.4247 0.5658 0.026 Uiso 1 1 calc R . . H12B H 0.6899 0.5083 0.6156 0.026 Uiso 1 1 calc R . . C13 C 0.57150(11) 0.58197(17) 0.61071(12) 0.0215(3) Uani 1 1 d . . . H13A H 0.6041 0.6447 0.6528 0.026 Uiso 1 1 calc R . . H13B H 0.5492 0.6171 0.5519 0.026 Uiso 1 1 calc R . . N14 N 0.49668(9) 0.53781(13) 0.62979(9) 0.0186(3) Uani 1 1 d . . . C15 C 0.42823(11) 0.61445(16) 0.60978(11) 0.0192(3) Uani 1 1 d . . . O16 O 0.42766(9) 0.71798(12) 0.58106(9) 0.0248(3) Uani 1 1 d . . . N17 N 0.35514(10) 0.57205(15) 0.62185(11) 0.0248(3) Uani 1 1 d . . . H17 H 0.3533 0.4953 0.6324 0.030 Uiso 1 1 calc R . . C18 C 0.27975(11) 0.64658(18) 0.61831(12) 0.0237(3) Uani 1 1 d . . . C19 C 0.21633(13) 0.5634(2) 0.63815(17) 0.0360(5) Uani 1 1 d . . . H19A H 0.1657 0.6094 0.6389 0.054 Uiso 1 1 d R . . H19B H 0.2477 0.5259 0.6948 0.054 Uiso 1 1 d R . . H19C H 0.1948 0.5015 0.5935 0.054 Uiso 1 1 d R . . C20 C 0.23185(13) 0.6992(2) 0.52749(12) 0.0291(4) Uani 1 1 d . . . H20A H 0.1791 0.7432 0.5249 0.044 Uiso 1 1 d R . . H20B H 0.2137 0.6346 0.4848 0.044 Uiso 1 1 d R . . H20C H 0.2720 0.7536 0.5148 0.044 Uiso 1 1 d R . . C21 C 0.30985(13) 0.7465(2) 0.68599(13) 0.0303(4) Uani 1 1 d . . . H21A H 0.2580 0.7929 0.6833 0.045 Uiso 1 1 d R . . H21B H 0.3517 0.7991 0.6743 0.045 Uiso 1 1 d R . . H21C H 0.3391 0.7115 0.7438 0.045 Uiso 1 1 d R . . C22 C 0.71910(12) 0.47025(18) 0.77224(12) 0.0253(4) Uani 1 1 d . . . H22A H 0.7757 0.4738 0.7653 0.038 Uiso 1 1 d R . . H22B H 0.7273 0.4264 0.8253 0.038 Uiso 1 1 d R . . H22C H 0.6987 0.5515 0.7760 0.038 Uiso 1 1 d R . . O23 O 0.54848(9) 0.40053(13) 0.82627(9) 0.0246(3) Uani 1 1 d . . . C24 C 0.46954(12) 0.38608(16) 0.82122(12) 0.0218(3) Uani 1 1 d . . . O25 O 0.40495(9) 0.37111(13) 0.75036(8) 0.0241(3) Uani 1 1 d . . . C26 C 0.45397(16) 0.3864(2) 0.90356(14) 0.0387(5) Uani 1 1 d . . . H26A H 0.4123 0.4505 0.9012 0.058 Uiso 1 1 d R . . H26B H 0.5106 0.3997 0.9529 0.058 Uiso 1 1 d R . . H26C H 0.4290 0.3094 0.9103 0.058 Uiso 1 1 d R . . O1S O 0.4137(2) 0.0819(4) 0.24556(18) 0.0530(10) Uani 0.706(5) 1 d PDU A 1 N1S N 0.46889(15) 0.1604(2) 0.15556(16) 0.0301(6) Uani 0.706(5) 1 d PDU A 1 C1S C 0.44871(16) 0.0691(3) 0.19386(18) 0.0346(7) Uani 0.706(5) 1 d PDU A 1 C2S C 0.4673(6) -0.0541(6) 0.1744(6) 0.0416(19) Uani 0.706(5) 1 d PDU A 1 H2S1 H 0.4416 -0.1149 0.1995 0.062 Uiso 0.706(5) 1 d PR A 1 H2S2 H 0.5320 -0.0642 0.1972 0.062 Uiso 0.706(5) 1 d PR A 1 H2S3 H 0.4425 -0.0629 0.1113 0.062 Uiso 0.706(5) 1 d PR A 1 C3S C 0.4460(6) 0.2846(5) 0.1770(7) 0.0429(19) Uani 0.706(5) 1 d PDU A 1 H3S1 H 0.4258 0.2749 0.2243 0.064 Uiso 0.706(5) 1 d PR A 1 H3S2 H 0.3980 0.3196 0.1267 0.064 Uiso 0.706(5) 1 d PR A 1 H3S3 H 0.4979 0.3374 0.1958 0.064 Uiso 0.706(5) 1 d PR A 1 C4S C 0.5138(4) 0.1346(12) 0.0937(3) 0.043(2) Uani 0.706(5) 1 d PDU A 1 H4S1 H 0.5744 0.1055 0.1265 0.065 Uiso 0.706(5) 1 d PR A 1 H4S2 H 0.5160 0.2066 0.0615 0.065 Uiso 0.706(5) 1 d PR A 1 H4S3 H 0.4793 0.0727 0.0531 0.065 Uiso 0.706(5) 1 d PR A 1 O1S' O 0.4083(5) 0.1246(8) 0.2456(2) 0.0468(18) Uani 0.294(5) 1 d PDU A 2 N1S' N 0.4717(4) 0.0814(6) 0.1535(4) 0.0304(14) Uani 0.294(5) 1 d PDU A 2 C1S' C 0.4407(3) 0.1571(7) 0.1948(3) 0.0361(14) Uani 0.294(5) 1 d PDU A 2 C2S' C 0.4492(13) 0.2827(13) 0.1722(14) 0.039(3) Uani 0.294(5) 1 d PDU A 2 H2S4 H 0.4197 0.2908 0.1092 0.058 Uiso 0.294(5) 1 d PR A 2 H2S5 H 0.5128 0.2996 0.1907 0.058 Uiso 0.294(5) 1 d PR A 2 H2S6 H 0.4231 0.3392 0.2000 0.058 Uiso 0.294(5) 1 d PR A 2 C3S' C 0.4726(13) -0.0541(10) 0.1604(14) 0.037(3) Uani 0.294(5) 1 d PDU A 2 H3S4 H 0.4394 -0.0616 0.1976 0.055 Uiso 0.294(5) 1 d PR A 2 H3S5 H 0.5319 -0.0891 0.1897 0.055 Uiso 0.294(5) 1 d PR A 2 H3S6 H 0.4407 -0.0962 0.1058 0.055 Uiso 0.294(5) 1 d PR A 2 C4S' C 0.5076(8) 0.151(3) 0.0967(7) 0.035(3) Uani 0.294(5) 1 d PDU A 2 H4S4 H 0.4726 0.1344 0.0353 0.053 Uiso 0.294(5) 1 d PR A 2 H4S5 H 0.5695 0.1274 0.1117 0.053 Uiso 0.294(5) 1 d PR A 2 H4S6 H 0.5050 0.2367 0.1077 0.053 Uiso 0.294(5) 1 d PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0545(3) 0.0287(2) 0.0370(2) -0.00088(19) 0.0233(2) -0.0036(2) Co1 0.01553(11) 0.01546(12) 0.01629(11) 0.00092(8) 0.00495(8) -0.00029(8) N1 0.0155(6) 0.0199(7) 0.0200(6) -0.0003(5) 0.0044(5) -0.0003(5) C2 0.0174(7) 0.0218(8) 0.0284(8) 0.0004(7) 0.0055(6) 0.0026(6) C3 0.0191(7) 0.0206(8) 0.0304(9) -0.0023(7) 0.0077(7) 0.0023(6) N4 0.0170(6) 0.0180(7) 0.0231(7) -0.0012(6) 0.0059(5) 0.0007(5) C5 0.0201(7) 0.0179(8) 0.0292(8) -0.0029(7) 0.0057(6) 0.0015(6) O6 0.0251(7) 0.0403(9) 0.0503(10) -0.0272(8) 0.0117(7) -0.0030(6) N7 0.0197(7) 0.0217(7) 0.0250(7) -0.0041(6) 0.0057(6) -0.0031(6) C8 0.0185(7) 0.0195(8) 0.0262(8) -0.0029(7) 0.0053(6) -0.0040(6) C9 0.0238(9) 0.0444(13) 0.0388(11) -0.0112(10) 0.0139(8) -0.0095(9) C10 0.0295(9) 0.0213(9) 0.0349(10) -0.0037(8) 0.0048(8) -0.0076(7) C11 0.0278(9) 0.0266(10) 0.0301(9) 0.0035(8) 0.0066(7) 0.0010(7) C12 0.0202(7) 0.0230(9) 0.0237(8) 0.0026(7) 0.0108(6) 0.0014(6) C13 0.0200(7) 0.0203(8) 0.0248(8) 0.0040(7) 0.0096(6) 0.0005(6) N14 0.0170(6) 0.0188(7) 0.0205(6) 0.0021(6) 0.0078(5) 0.0008(5) C15 0.0196(7) 0.0193(8) 0.0170(7) 0.0006(6) 0.0056(6) 0.0006(6) O16 0.0265(6) 0.0204(6) 0.0281(6) 0.0071(5) 0.0113(5) 0.0044(5) N17 0.0193(7) 0.0212(7) 0.0345(8) 0.0070(7) 0.0114(6) 0.0045(6) C18 0.0171(7) 0.0257(9) 0.0274(8) 0.0026(7) 0.0077(6) 0.0042(7) C19 0.0216(8) 0.0366(12) 0.0529(13) 0.0067(10) 0.0181(9) 0.0035(8) C20 0.0223(8) 0.0324(10) 0.0258(8) -0.0004(8) 0.0023(7) 0.0075(7) C21 0.0262(9) 0.0373(11) 0.0267(9) -0.0032(8) 0.0097(7) 0.0046(8) C22 0.0182(7) 0.0265(9) 0.0258(8) -0.0023(7) 0.0029(6) -0.0025(7) O23 0.0226(6) 0.0299(7) 0.0206(6) 0.0001(5) 0.0077(5) -0.0032(5) C24 0.0256(8) 0.0196(8) 0.0205(7) 0.0005(6) 0.0095(6) -0.0023(6) O25 0.0238(6) 0.0259(7) 0.0204(6) -0.0004(5) 0.0063(5) -0.0020(5) C26 0.0358(11) 0.0601(16) 0.0233(9) -0.0057(9) 0.0150(8) -0.0101(10) O1S 0.0591(17) 0.043(2) 0.082(2) -0.0076(14) 0.0549(15) -0.0049(15) N1S 0.0230(11) 0.0321(14) 0.0311(12) -0.0026(11) 0.0065(9) 0.0000(10) C1S 0.0261(12) 0.0388(16) 0.0414(15) 0.0006(14) 0.0160(12) -0.0016(12) C2S 0.054(3) 0.039(2) 0.039(3) 0.0005(18) 0.026(2) 0.002(2) C3S 0.039(3) 0.036(2) 0.045(4) -0.009(3) 0.006(3) 0.004(3) C4S 0.039(3) 0.060(5) 0.038(3) 0.006(2) 0.023(2) 0.011(2) O1S' 0.046(3) 0.050(4) 0.061(3) -0.027(3) 0.038(2) -0.014(3) N1S' 0.022(2) 0.035(3) 0.034(3) -0.004(2) 0.012(2) 0.003(2) C1S' 0.026(2) 0.042(3) 0.043(3) -0.017(3) 0.017(2) -0.007(2) C2S' 0.032(7) 0.041(5) 0.032(6) -0.012(5) 0.001(5) -0.004(6) C3S' 0.050(5) 0.034(4) 0.036(6) 0.002(4) 0.027(5) 0.003(4) C4S' 0.038(5) 0.037(5) 0.032(5) 0.006(4) 0.015(4) 0.003(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 K1 O16 2.4317(15) 3_666 ? K1 O6 2.4622(19) . ? K1 O1S 2.514(3) . ? K1 O1S' 2.519(4) . ? K1 O6 2.5294(19) 3_656 ? Co1 N14 1.9570(15) . ? Co1 N4 1.9642(15) . ? Co1 O23 2.0278(13) . ? Co1 N1 2.1160(15) . ? Co1 O25 2.4436(14) . ? N1 C22 1.472(2) . ? N1 C2 1.480(2) . ? N1 C12 1.486(2) . ? C2 C3 1.525(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N4 1.467(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N4 C5 1.342(2) . ? C5 O6 1.261(2) . ? C5 N7 1.377(2) . ? O6 K1 2.5294(19) 3_656 ? N7 C8 1.481(2) . ? N7 H7 0.8800 . ? C8 C11 1.527(3) . ? C8 C9 1.529(3) . ? C8 C10 1.534(3) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.525(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N14 1.469(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? N14 C15 1.344(2) . ? C15 O16 1.254(2) . ? C15 N17 1.375(2) . ? O16 K1 2.4317(15) 3_666 ? N17 C18 1.471(2) . ? N17 H17 0.8800 . ? C18 C19 1.527(3) . ? C18 C21 1.532(3) . ? C18 C20 1.533(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? O23 C24 1.272(2) . ? C24 O25 1.253(2) . ? C24 C26 1.504(3) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? O1S C1S 1.225(4) . ? N1S C1S 1.318(4) . ? N1S C4S 1.520(7) . ? N1S C3S 1.520(8) . ? N1S H4S6 1.4509 . ? C1S C2S 1.477(8) . ? C1S H3S4 1.4749 . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? C2S H3S4 0.7133 . ? C2S H3S5 1.0589 . ? C2S H3S6 1.1600 . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9800 . ? C3S H3S3 0.9800 . ? C3S H2S4 1.0502 . ? C3S H2S5 1.0392 . ? C3S H2S6 0.8821 . ? C4S H4S1 0.9800 . ? C4S H4S2 0.9800 . ? C4S H4S3 0.9800 . ? C4S H4S4 0.9462 . ? C4S H4S5 0.8440 . ? C4S H4S6 1.1866 . ? O1S' C1S' 1.225(6) . ? N1S' C1S' 1.318(6) . ? N1S' C3S' 1.521(8) . ? N1S' C4S' 1.521(8) . ? C1S' C2S' 1.477(10) . ? C1S' H3S1 1.4631 . ? C2S' H3S1 1.0896 . ? C2S' H3S2 0.9759 . ? C2S' H3S3 0.9581 . ? C2S' H2S4 0.9800 . ? C2S' H2S5 0.9800 . ? C2S' H2S6 0.9800 . ? C3S' H2S1 1.1905 . ? C3S' H2S2 0.9307 . ? C3S' H2S3 0.7835 . ? C3S' H3S4 0.9800 . ? C3S' H3S5 0.9800 . ? C3S' H3S6 0.9800 . ? C4S' H4S1 1.1282 . ? C4S' H4S2 0.9062 . ? C4S' H4S3 1.1192 . ? C4S' H4S4 0.9800 . ? C4S' H4S5 0.9800 . ? C4S' H4S6 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 O16 K1 O6 106.00(5) 3_666 . ? O16 K1 O1S 99.64(10) 3_666 . ? O6 K1 O1S 142.00(9) . . ? O16 K1 O1S' 91.72(19) 3_666 . ? O6 K1 O1S' 140.15(19) . . ? O1S K1 O1S' 11.1(2) . . ? O16 K1 O6 124.12(5) 3_666 3_656 ? O6 K1 O6 82.98(5) . 3_656 ? O1S K1 O6 105.30(10) . 3_656 ? O1S' K1 O6 116.3(2) . 3_656 ? N14 Co1 N4 121.28(6) . . ? N14 Co1 O23 119.00(6) . . ? N4 Co1 O23 119.64(6) . . ? N14 Co1 N1 85.00(6) . . ? N4 Co1 N1 85.02(6) . . ? O23 Co1 N1 103.08(6) . . ? N14 Co1 O25 104.92(5) . . ? N4 Co1 O25 102.39(6) . . ? O23 Co1 O25 58.38(5) . . ? N1 Co1 O25 161.39(5) . . ? C22 N1 C2 110.83(14) . . ? C22 N1 C12 110.89(15) . . ? C2 N1 C12 112.68(14) . . ? C22 N1 Co1 115.98(11) . . ? C2 N1 Co1 104.01(10) . . ? C12 N1 Co1 102.09(10) . . ? N1 C2 C3 110.98(14) . . ? N1 C2 H2A 109.4 . . ? C3 C2 H2A 109.4 . . ? N1 C2 H2B 109.4 . . ? C3 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? N4 C3 C2 109.45(15) . . ? N4 C3 H3A 109.8 . . ? C2 C3 H3A 109.8 . . ? N4 C3 H3B 109.8 . . ? C2 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? C5 N4 C3 114.72(15) . . ? C5 N4 Co1 127.58(12) . . ? C3 N4 Co1 113.12(11) . . ? O6 C5 N4 123.79(17) . . ? O6 C5 N7 120.02(17) . . ? N4 C5 N7 116.14(16) . . ? C5 O6 K1 139.05(15) . . ? C5 O6 K1 113.11(15) . 3_656 ? K1 O6 K1 97.02(5) . 3_656 ? C5 N7 C8 123.26(15) . . ? C5 N7 H7 118.4 . . ? C8 N7 H7 118.4 . . ? N7 C8 C11 110.72(15) . . ? N7 C8 C9 105.55(15) . . ? C11 C8 C9 109.77(17) . . ? N7 C8 C10 111.67(15) . . ? C11 C8 C10 110.73(16) . . ? C9 C8 C10 108.23(16) . . ? C8 C9 H9A 109.4 . . ? C8 C9 H9B 109.4 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.6 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.4 . . ? C8 C10 H10B 109.6 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.4 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 C13 110.36(14) . . ? N1 C12 H12A 109.6 . . ? C13 C12 H12A 109.6 . . ? N1 C12 H12B 109.6 . . ? C13 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? N14 C13 C12 108.66(14) . . ? N14 C13 H13A 110.0 . . ? C12 C13 H13A 110.0 . . ? N14 C13 H13B 110.0 . . ? C12 C13 H13B 110.0 . . ? H13A C13 H13B 108.3 . . ? C15 N14 C13 114.52(14) . . ? C15 N14 Co1 131.19(12) . . ? C13 N14 Co1 113.23(11) . . ? O16 C15 N14 124.38(16) . . ? O16 C15 N17 120.10(16) . . ? N14 C15 N17 115.51(16) . . ? C15 O16 K1 144.94(12) . 3_666 ? C15 N17 C18 124.29(16) . . ? C15 N17 H17 117.9 . . ? C18 N17 H17 117.9 . . ? N17 C18 C19 106.11(16) . . ? N17 C18 C21 111.48(15) . . ? C19 C18 C21 109.25(17) . . ? N17 C18 C20 110.40(16) . . ? C19 C18 C20 109.18(16) . . ? C21 C18 C20 110.31(17) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.4 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.4 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.4 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 C22 H22A 109.4 . . ? N1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 O23 Co1 98.91(11) . . ? O25 C24 O23 122.24(17) . . ? O25 C24 C26 119.32(18) . . ? O23 C24 C26 118.44(17) . . ? C24 O25 Co1 80.47(11) . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.4 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.6 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C1S O1S K1 129.4(2) . . ? C1S N1S C4S 118.0(5) . . ? C1S N1S C3S 117.4(5) . . ? C4S N1S C3S 124.6(8) . . ? C1S N1S H4S6 164.5 . . ? C4S N1S H4S6 47.0 . . ? C3S N1S H4S6 77.7 . . ? O1S C1S N1S 122.3(4) . . ? O1S C1S C2S 117.5(5) . . ? N1S C1S C2S 120.1(5) . . ? O1S C1S H3S4 90.0 . . ? N1S C1S H3S4 147.1 . . ? C2S C1S H3S4 28.0 . . ? C1S C2S H2S1 113.0 . . ? C1S C2S H2S2 107.8 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 107.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? C1S C2S H3S4 75.9 . . ? H2S1 C2S H3S4 37.3 . . ? H2S2 C2S H3S4 126.8 . . ? H2S3 C2S H3S4 120.0 . . ? C1S C2S H3S5 124.4 . . ? H2S1 C2S H3S5 101.3 . . ? H2S2 C2S H3S5 16.7 . . ? H2S3 C2S H3S5 99.9 . . ? H3S4 C2S H3S5 128.0 . . ? C1S C2S H3S6 124.8 . . ? H2S1 C2S H3S6 95.2 . . ? H2S2 C2S H3S6 105.4 . . ? H2S3 C2S H3S6 18.2 . . ? H3S4 C2S H3S6 115.3 . . ? H3S5 C2S H3S6 92.2 . . ? N1S C3S H3S1 106.6 . . ? N1S C3S H3S2 110.5 . . ? H3S1 C3S H3S2 109.5 . . ? N1S C3S H3S3 111.3 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? N1S C3S H2S4 80.6 . . ? H3S1 C3S H2S4 139.8 . . ? H3S2 C3S H2S4 36.1 . . ? H3S3 C3S H2S4 103.9 . . ? N1S C3S H2S5 82.2 . . ? H3S1 C3S H2S5 120.1 . . ? H3S2 C3S H2S5 122.7 . . ? H3S3 C3S H2S5 29.2 . . ? H2S4 C3S H2S5 100.0 . . ? N1S C3S H2S6 157.8 . . ? H3S1 C3S H2S6 52.0 . . ? H3S2 C3S H2S6 76.5 . . ? H3S3 C3S H2S6 84.6 . . ? H2S4 C3S H2S6 111.5 . . ? H2S5 C3S H2S6 112.5 . . ? N1S C4S H4S1 109.5 . . ? N1S C4S H4S2 110.9 . . ? H4S1 C4S H4S2 109.5 . . ? N1S C4S H4S3 108.0 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? N1S C4S H4S4 111.8 . . ? H4S1 C4S H4S4 136.9 . . ? H4S2 C4S H4S4 66.1 . . ? H4S3 C4S H4S4 45.4 . . ? N1S C4S H4S5 121.3 . . ? H4S1 C4S H4S5 19.4 . . ? H4S2 C4S H4S5 90.3 . . ? H4S3 C4S H4S5 115.2 . . ? H4S4 C4S H4S5 126.7 . . ? N1S C4S H4S6 63.4 . . ? H4S1 C4S H4S6 112.5 . . ? H4S2 C4S H4S6 49.6 . . ? H4S3 C4S H4S6 137.5 . . ? H4S4 C4S H4S6 96.6 . . ? H4S5 C4S H4S6 102.7 . . ? C1S' O1S' K1 128.0(4) . . ? C1S' N1S' C3S' 126.5(12) . . ? C1S' N1S' C4S' 109.1(13) . . ? C3S' N1S' C4S' 124.4(16) . . ? O1S' C1S' N1S' 122.6(8) . . ? O1S' C1S' C2S' 125.0(14) . . ? N1S' C1S' C2S' 112.4(13) . . ? O1S' C1S' H3S1 81.7 . . ? N1S' C1S' H3S1 155.4 . . ? C2S' C1S' H3S1 43.5 . . ? C1S' C2S' H3S1 67.6 . . ? C1S' C2S' H3S2 117.8 . . ? H3S1 C2S' H3S2 101.4 . . ? C1S' C2S' H3S3 130.5 . . ? H3S1 C2S' H3S3 102.6 . . ? H3S2 C2S' H3S3 111.7 . . ? C1S' C2S' H2S4 108.1 . . ? H3S1 C2S' H2S4 134.2 . . ? H3S2 C2S' H2S4 37.7 . . ? H3S3 C2S' H2S4 111.2 . . ? C1S' C2S' H2S5 107.4 . . ? H3S1 C2S' H2S5 115.3 . . ? H3S2 C2S' H2S5 129.9 . . ? H3S3 C2S' H2S5 30.6 . . ? H2S4 C2S' H2S5 109.5 . . ? C1S' C2S' H2S6 112.9 . . ? H3S1 C2S' H2S6 46.3 . . ? H3S2 C2S' H2S6 72.4 . . ? H3S3 C2S' H2S6 80.7 . . ? H2S4 C2S' H2S6 109.5 . . ? H2S5 C2S' H2S6 109.5 . . ? N1S' C3S' H2S1 128.3 . . ? N1S' C3S' H2S2 98.5 . . ? H2S1 C3S' H2S2 97.2 . . ? N1S' C3S' H2S3 93.6 . . ? H2S1 C3S' H2S3 106.5 . . ? H2S2 C3S' H2S3 137.8 . . ? N1S' C3S' H3S4 98.2 . . ? H2S1 C3S' H3S4 30.0 . . ? H2S2 C3S' H3S4 105.2 . . ? H2S3 C3S' H3S4 112.8 . . ? N1S' C3S' H3S5 114.5 . . ? H2S1 C3S' H3S5 92.7 . . ? H2S2 C3S' H3S5 18.2 . . ? H2S3 C3S' H3S5 124.3 . . ? H3S4 C3S' H3S5 109.5 . . ? N1S' C3S' H3S6 115.0 . . ? H2S1 C3S' H3S6 93.3 . . ? H2S2 C3S' H3S6 126.4 . . ? H2S3 C3S' H3S6 21.6 . . ? H3S4 C3S' H3S6 109.5 . . ? H3S5 C3S' H3S6 109.5 . . ? N1S' C4S' H4S1 92.1 . . ? N1S' C4S' H4S2 163.7 . . ? H4S1 C4S' H4S2 103.2 . . ? N1S' C4S' H4S3 81.2 . . ? H4S1 C4S' H4S3 90.8 . . ? H4S2 C4S' H4S3 103.9 . . ? N1S' C4S' H4S4 110.8 . . ? H4S1 C4S' H4S4 116.2 . . ? H4S2 C4S' H4S4 67.6 . . ? H4S3 C4S' H4S4 40.8 . . ? N1S' C4S' H4S5 108.5 . . ? H4S1 C4S' H4S5 16.4 . . ? H4S2 C4S' H4S5 86.8 . . ? H4S3 C4S' H4S5 94.3 . . ? H4S4 C4S' H4S5 109.5 . . ? N1S' C4S' H4S6 109.1 . . ? H4S1 C4S' H4S6 117.7 . . ? H4S2 C4S' H4S6 58.7 . . ? H4S3 C4S' H4S6 148.5 . . ? H4S4 C4S' H4S6 109.5 . . ? H4S5 C4S' H4S6 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 N14 Co1 N1 C22 94.55(13) . . . . ? N4 Co1 N1 C22 -143.39(13) . . . . ? O23 Co1 N1 C22 -24.09(14) . . . . ? O25 Co1 N1 C22 -28.8(2) . . . . ? N14 Co1 N1 C2 -143.50(11) . . . . ? N4 Co1 N1 C2 -21.44(11) . . . . ? O23 Co1 N1 C2 97.86(11) . . . . ? O25 Co1 N1 C2 93.12(19) . . . . ? N14 Co1 N1 C12 -26.13(11) . . . . ? N4 Co1 N1 C12 95.93(11) . . . . ? O23 Co1 N1 C12 -144.76(11) . . . . ? O25 Co1 N1 C12 -149.50(15) . . . . ? C22 N1 C2 C3 166.29(15) . . . . ? C12 N1 C2 C3 -68.79(19) . . . . ? Co1 N1 C2 C3 40.98(17) . . . . ? N1 C2 C3 N4 -45.5(2) . . . . ? C2 C3 N4 C5 -176.52(16) . . . . ? C2 C3 N4 Co1 25.58(18) . . . . ? N14 Co1 N4 C5 -75.74(17) . . . . ? O23 Co1 N4 C5 100.96(16) . . . . ? N1 Co1 N4 C5 -156.81(17) . . . . ? O25 Co1 N4 C5 40.48(17) . . . . ? N14 Co1 N4 C3 78.71(13) . . . . ? O23 Co1 N4 C3 -104.58(12) . . . . ? N1 Co1 N4 C3 -2.36(12) . . . . ? O25 Co1 N4 C3 -165.07(11) . . . . ? C3 N4 C5 O6 -4.3(3) . . . . ? Co1 N4 C5 O6 149.84(17) . . . . ? C3 N4 C5 N7 173.20(16) . . . . ? Co1 N4 C5 N7 -32.7(2) . . . . ? N4 C5 O6 K1 -51.6(3) . . . . ? N7 C5 O6 K1 131.01(18) . . . . ? N4 C5 O6 K1 82.4(2) . . . 3_656 ? N7 C5 O6 K1 -94.99(18) . . . 3_656 ? O16 K1 O6 C5 14.6(2) 3_666 . . . ? O1S K1 O6 C5 -115.9(2) . . . . ? O1S' K1 O6 C5 -98.5(4) . . . . ? O6 K1 O6 C5 138.2(2) 3_656 . . . ? O16 K1 O6 K1 -123.55(5) 3_666 . . 3_656 ? O1S K1 O6 K1 105.91(16) . . . 3_656 ? O1S' K1 O6 K1 123.4(3) . . . 3_656 ? O6 K1 O6 K1 0.0 3_656 . . 3_656 ? O6 C5 N7 C8 -30.5(3) . . . . ? N4 C5 N7 C8 151.91(17) . . . . ? C5 N7 C8 C11 -55.6(2) . . . . ? C5 N7 C8 C9 -174.30(18) . . . . ? C5 N7 C8 C10 68.3(2) . . . . ? C22 N1 C12 C13 -78.25(18) . . . . ? C2 N1 C12 C13 156.87(14) . . . . ? Co1 N1 C12 C13 45.90(15) . . . . ? N1 C12 C13 N14 -47.85(19) . . . . ? C12 C13 N14 C15 -166.99(15) . . . . ? C12 C13 N14 Co1 23.43(17) . . . . ? N4 Co1 N14 C15 113.18(16) . . . . ? O23 Co1 N14 C15 -63.55(17) . . . . ? N1 Co1 N14 C15 -165.75(16) . . . . ? O25 Co1 N14 C15 -1.76(17) . . . . ? N4 Co1 N14 C13 -79.46(13) . . . . ? O23 Co1 N14 C13 103.82(12) . . . . ? N1 Co1 N14 C13 1.62(12) . . . . ? O25 Co1 N14 C13 165.61(11) . . . . ? C13 N14 C15 O16 -3.4(2) . . . . ? Co1 N14 C15 O16 163.89(14) . . . . ? C13 N14 C15 N17 175.97(15) . . . . ? Co1 N14 C15 N17 -16.8(2) . . . . ? N14 C15 O16 K1 -40.1(3) . . . 3_666 ? N17 C15 O16 K1 140.57(17) . . . 3_666 ? O16 C15 N17 C18 -11.5(3) . . . . ? N14 C15 N17 C18 169.15(16) . . . . ? C15 N17 C18 C19 -178.23(18) . . . . ? C15 N17 C18 C21 -59.4(2) . . . . ? C15 N17 C18 C20 63.6(2) . . . . ? N14 Co1 O23 C24 90.11(12) . . . . ? N4 Co1 O23 C24 -86.67(12) . . . . ? N1 Co1 O23 C24 -178.37(11) . . . . ? O25 Co1 O23 C24 -0.14(10) . . . . ? Co1 O23 C24 O25 0.3(2) . . . . ? Co1 O23 C24 C26 179.91(16) . . . . ? O23 C24 O25 Co1 -0.23(17) . . . . ? C26 C24 O25 Co1 -179.86(19) . . . . ? N14 Co1 O25 C24 -115.02(11) . . . . ? N4 Co1 O25 C24 117.49(11) . . . . ? O23 Co1 O25 C24 0.14(11) . . . . ? N1 Co1 O25 C24 5.6(2) . . . . ? O16 K1 O1S C1S 60.0(4) 3_666 . . . ? O6 K1 O1S C1S -167.9(3) . . . . ? O1S' K1 O1S C1S 104.9(13) . . . . ? O6 K1 O1S C1S -69.6(4) 3_656 . . . ? K1 O1S C1S N1S -91.8(4) . . . . ? K1 O1S C1S C2S 88.9(4) . . . . ? C4S N1S C1S O1S 178.9(2) . . . . ? C3S N1S C1S O1S -0.7(2) . . . . ? C4S N1S C1S C2S -1.8(3) . . . . ? C3S N1S C1S C2S 178.6(3) . . . . ? O16 K1 O1S' C1S' 38.8(9) 3_666 . . . ? O6 K1 O1S' C1S' 156.6(7) . . . . ? O1S K1 O1S' C1S' -97.0(16) . . . . ? O6 K1 O1S' C1S' -91.0(8) 3_656 . . . ? K1 O1S' C1S' N1S' 93.9(8) . . . . ? K1 O1S' C1S' C2S' -86.5(8) . . . . ? C3S' N1S' C1S' O1S' 0.3(3) . . . . ? C4S' N1S' C1S' O1S' -179.5(3) . . . . ? C3S' N1S' C1S' C2S' -179.3(4) . . . . ? C4S' N1S' C1S' C2S' 0.9(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 N7 H7 O25 0.88 2.32 3.008(2) 135.2 . N17 H17 O25 0.88 2.29 3.001(2) 137.4 . _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.914 _refine_diff_density_min -0.931 _refine_diff_density_rms 0.091 #===END data_00381a _database_code_CSD 199772 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 00381a _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H46 Fe K N7 O5' _chemical_formula_weight 631.65 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.339(3) _cell_length_b 11.171(4) _cell_length_c 14.453(5) _cell_angle_alpha 79.414(7) _cell_angle_beta 82.092(7) _cell_angle_gamma 86.388(7) _cell_volume 1624.1(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 0.636 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.805 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9994 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0995 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.07 _reflns_number_total 5634 _reflns_number_gt 3291 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0886P)^2^+6.7579P] 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 5634 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1474 _refine_ls_R_factor_gt 0.0798 _refine_ls_wR_factor_ref 0.2480 _refine_ls_wR_factor_gt 0.1801 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.09633(10) 0.45074(9) 0.23467(7) 0.0361(3) Uani 1 1 d . . . N1 N 0.0557(6) 0.6514(5) 0.1831(4) 0.0389(14) Uani 1 1 d . . . C1 C 0.0924(8) 0.6708(6) 0.0789(5) 0.0462(19) Uani 1 1 d . . . H1A H 0.1079 0.7581 0.0545 0.055 Uiso 1 1 calc R . . H1B H 0.0201 0.6472 0.0485 0.055 Uiso 1 1 calc R . . C2 C 0.2157(7) 0.5948(6) 0.0539(5) 0.0449(18) Uani 1 1 d . . . H2A H 0.2324 0.5979 -0.0156 0.054 Uiso 1 1 calc R . . H2B H 0.2919 0.6275 0.0743 0.054 Uiso 1 1 calc R . . N2 N 0.1965(6) 0.4698(5) 0.1023(4) 0.0403(14) Uani 1 1 d . . . C3 C 0.2692(7) 0.3866(6) 0.0594(5) 0.0352(16) Uani 1 1 d . . . O1 O 0.3648(5) 0.4096(4) -0.0048(4) 0.0458(13) Uani 1 1 d . . . N3 N 0.2354(6) 0.2674(5) 0.0914(4) 0.0447(15) Uani 1 1 d . . . H3A H 0.1618 0.2546 0.1297 0.054 Uiso 1 1 calc R . . C4 C 0.3117(8) 0.1603(6) 0.0668(5) 0.049(2) Uani 1 1 d . . . C5 C 0.3121(11) 0.1563(8) -0.0388(6) 0.076(3) Uani 1 1 d . . . H5A H 0.2220 0.1536 -0.0522 0.114 Uiso 1 1 calc R . . H5B H 0.3619 0.0834 -0.0543 0.114 Uiso 1 1 calc R . . H5C H 0.3525 0.2292 -0.0773 0.114 Uiso 1 1 calc R . . C6 C 0.2411(9) 0.0495(7) 0.1260(7) 0.065(2) Uani 1 1 d . . . H6A H 0.2447 0.0486 0.1935 0.097 Uiso 1 1 calc R . . H6B H 0.2838 -0.0253 0.1082 0.097 Uiso 1 1 calc R . . H6C H 0.1497 0.0544 0.1141 0.097 Uiso 1 1 calc R . . C7 C 0.4488(8) 0.1562(8) 0.0912(7) 0.070(3) Uani 1 1 d . . . H7A H 0.4463 0.1610 0.1585 0.105 Uiso 1 1 calc R . . H7B H 0.4959 0.2251 0.0522 0.105 Uiso 1 1 calc R . . H7C H 0.4937 0.0797 0.0789 0.105 Uiso 1 1 calc R . . C8 C -0.0852(7) 0.6697(7) 0.2133(6) 0.0462(18) Uani 1 1 d . . . H8A H -0.1168 0.7479 0.1777 0.055 Uiso 1 1 calc R . . H8B H -0.0990 0.6749 0.2817 0.055 Uiso 1 1 calc R . . C9 C -0.1639(7) 0.5671(6) 0.1968(6) 0.0465(18) Uani 1 1 d . . . H9A H -0.2552 0.5747 0.2272 0.056 Uiso 1 1 calc R . . H9B H -0.1649 0.5709 0.1280 0.056 Uiso 1 1 calc R . . N4 N -0.1024(6) 0.4503(5) 0.2385(4) 0.0401(14) Uani 1 1 d . . . C10 C -0.1801(7) 0.3548(6) 0.2443(5) 0.0386(16) Uani 1 1 d . . . O2 O -0.2902(5) 0.3626(5) 0.2183(4) 0.0537(14) Uani 1 1 d . . . N5 N -0.1274(6) 0.2435(5) 0.2847(4) 0.0458(16) Uani 1 1 d . . . H5D H -0.0552 0.2434 0.3106 0.055 Uiso 1 1 calc R . . C11 C -0.1844(8) 0.1257(7) 0.2868(6) 0.050(2) Uani 1 1 d . . . C12 C -0.0885(8) 0.0300(7) 0.3323(6) 0.059(2) Uani 1 1 d . . . H12A H -0.0023 0.0378 0.2944 0.089 Uiso 1 1 calc R . . H12B H -0.1199 -0.0516 0.3349 0.089 Uiso 1 1 calc R . . H12C H -0.0820 0.0427 0.3968 0.089 Uiso 1 1 calc R . . C13 C -0.3181(8) 0.1182(8) 0.3480(7) 0.067(3) Uani 1 1 d . . . H13A H -0.3764 0.1847 0.3220 0.101 Uiso 1 1 calc R . . H13B H -0.3076 0.1252 0.4132 0.101 Uiso 1 1 calc R . . H13C H -0.3558 0.0398 0.3481 0.101 Uiso 1 1 calc R . . C14 C -0.1957(10) 0.1068(9) 0.1865(7) 0.073(3) Uani 1 1 d . . . H14A H -0.1104 0.1178 0.1475 0.109 Uiso 1 1 calc R . . H14B H -0.2597 0.1664 0.1588 0.109 Uiso 1 1 calc R . . H14C H -0.2242 0.0243 0.1885 0.109 Uiso 1 1 calc R . . C15 C 0.1349(7) 0.7212(7) 0.2290(6) 0.0472(19) Uani 1 1 d . . . H15A H 0.0965 0.8050 0.2266 0.057 Uiso 1 1 calc R . . H15B H 0.2243 0.7266 0.1941 0.057 Uiso 1 1 calc R . . C16 C 0.1418(7) 0.6626(7) 0.3307(6) 0.0471(19) Uani 1 1 d . . . C17 C 0.1517(9) 0.7309(9) 0.4013(7) 0.067(3) Uani 1 1 d . . . H17A H 0.1497 0.8174 0.3873 0.080 Uiso 1 1 calc R . . C18 C 0.1645(8) 0.6703(10) 0.4906(7) 0.069(3) Uani 1 1 d . . . H18A H 0.1733 0.7145 0.5395 0.083 Uiso 1 1 calc R . . C19 C 0.1646(8) 0.5458(9) 0.5097(6) 0.056(2) Uani 1 1 d . . . H19A H 0.1736 0.5028 0.5718 0.068 Uiso 1 1 calc R . . C20 C 0.1518(7) 0.4843(8) 0.4390(5) 0.051(2) Uani 1 1 d . . . H20A H 0.1508 0.3979 0.4531 0.061 Uiso 1 1 calc R . . N6 N 0.1406(5) 0.5407(5) 0.3498(4) 0.0410(14) Uani 1 1 d . . . O3 O 0.1415(5) 0.2811(4) 0.3112(4) 0.0455(12) Uani 1 1 d . . . O4 O 0.3544(5) 0.3101(5) 0.2957(4) 0.0601(15) Uani 1 1 d . . . C21 C 0.2586(8) 0.2487(7) 0.3277(5) 0.0444(18) Uani 1 1 d . . . C22 C 0.2745(8) 0.1286(7) 0.3940(6) 0.061(2) Uani 1 1 d . . . H22A H 0.3675 0.1097 0.3986 0.091 Uiso 1 1 calc R . . H22B H 0.2377 0.0638 0.3694 0.091 Uiso 1 1 calc R . . H22C H 0.2284 0.1344 0.4571 0.091 Uiso 1 1 calc R . . K1 K 0.50396(15) 0.44949(15) 0.14487(11) 0.0445(4) Uani 1 1 d . . . O5 O 0.4465(6) 0.6454(5) 0.2276(4) 0.0611(15) Uani 1 1 d . . . C23 C 0.5072(11) 0.5217(8) 0.3721(6) 0.075(3) Uani 1 1 d . . . H23A H 0.4548 0.5239 0.4337 0.112 Uiso 1 1 calc R . . H23B H 0.6000 0.5110 0.3805 0.112 Uiso 1 1 calc R . . H23C H 0.4813 0.4536 0.3455 0.112 Uiso 1 1 calc R . . C24 C 0.4843(9) 0.6446(10) 0.3026(7) 0.068(3) Uani 1 1 d . . . N7 N 0.5074(8) 0.7433(9) 0.3324(6) 0.082(3) Uani 1 1 d . . . C25 C 0.4853(11) 0.8601(8) 0.2716(7) 0.084(3) Uani 1 1 d . . . H25A H 0.4421 0.8472 0.2182 0.126 Uiso 1 1 calc R . . H25B H 0.5692 0.8977 0.2475 0.126 Uiso 1 1 calc R . . H25C H 0.4297 0.9138 0.3082 0.126 Uiso 1 1 calc R . . C26 C 0.5595(14) 0.7443(12) 0.4233(8) 0.118(5) Uani 1 1 d . . . H26A H 0.5820 0.6606 0.4526 0.177 Uiso 1 1 calc R . . H26B H 0.4931 0.7802 0.4665 0.177 Uiso 1 1 calc R . . H26C H 0.6378 0.7928 0.4108 0.177 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0327(6) 0.0350(6) 0.0408(6) -0.0067(4) -0.0049(4) -0.0031(4) N1 0.040(3) 0.031(3) 0.046(4) -0.007(3) -0.004(3) -0.005(3) C1 0.061(5) 0.028(4) 0.048(4) -0.006(3) -0.007(4) 0.004(3) C2 0.055(5) 0.027(4) 0.050(5) -0.004(3) 0.000(4) -0.001(3) N2 0.042(4) 0.030(3) 0.046(4) -0.004(3) 0.000(3) 0.000(3) C3 0.037(4) 0.031(4) 0.042(4) -0.011(3) -0.010(3) 0.001(3) O1 0.043(3) 0.038(3) 0.053(3) -0.009(2) 0.010(3) -0.002(2) N3 0.047(4) 0.024(3) 0.060(4) -0.012(3) 0.010(3) 0.000(3) C4 0.065(5) 0.031(4) 0.051(5) -0.013(3) -0.004(4) 0.007(4) C5 0.126(9) 0.045(5) 0.059(6) -0.021(4) -0.008(6) 0.008(5) C6 0.077(6) 0.031(4) 0.079(6) -0.001(4) 0.003(5) -0.003(4) C7 0.054(6) 0.050(5) 0.104(8) -0.007(5) -0.013(5) 0.008(4) C8 0.038(4) 0.039(4) 0.062(5) -0.013(4) -0.004(4) 0.005(3) C9 0.038(4) 0.041(4) 0.060(5) -0.006(4) -0.012(4) 0.002(3) N4 0.038(3) 0.037(3) 0.047(4) -0.012(3) -0.007(3) -0.001(3) C10 0.035(4) 0.037(4) 0.045(4) -0.011(3) -0.002(3) -0.004(3) O2 0.036(3) 0.045(3) 0.084(4) -0.009(3) -0.023(3) -0.003(2) N5 0.043(4) 0.035(3) 0.062(4) -0.002(3) -0.021(3) -0.007(3) C11 0.048(5) 0.043(4) 0.064(5) -0.017(4) -0.010(4) -0.014(4) C12 0.058(5) 0.040(4) 0.081(6) -0.002(4) -0.020(5) -0.011(4) C13 0.038(5) 0.058(5) 0.103(7) -0.015(5) 0.006(5) -0.019(4) C14 0.082(7) 0.066(6) 0.078(7) -0.033(5) -0.009(5) -0.001(5) C15 0.042(4) 0.036(4) 0.066(5) -0.019(4) -0.003(4) -0.002(3) C16 0.037(4) 0.055(5) 0.054(5) -0.022(4) -0.006(4) -0.003(4) C17 0.068(6) 0.067(6) 0.074(7) -0.036(5) -0.004(5) -0.012(5) C18 0.054(6) 0.105(8) 0.061(6) -0.047(6) 0.002(5) -0.019(5) C19 0.043(5) 0.089(7) 0.040(5) -0.019(4) -0.003(4) -0.012(4) C20 0.040(5) 0.070(5) 0.044(5) -0.012(4) -0.008(4) -0.004(4) N6 0.029(3) 0.048(4) 0.049(4) -0.015(3) -0.005(3) -0.004(3) O3 0.036(3) 0.043(3) 0.055(3) 0.003(2) -0.009(2) -0.006(2) O4 0.041(3) 0.063(4) 0.073(4) -0.001(3) -0.002(3) -0.016(3) C21 0.046(5) 0.049(4) 0.042(4) -0.011(4) -0.014(4) 0.000(4) C22 0.060(6) 0.050(5) 0.069(6) 0.003(4) -0.017(5) 0.002(4) K1 0.0374(9) 0.0484(10) 0.0467(10) -0.0050(8) -0.0054(7) -0.0055(7) O5 0.057(4) 0.065(4) 0.066(4) -0.018(3) -0.015(3) -0.003(3) C23 0.107(8) 0.062(6) 0.056(6) -0.012(5) -0.007(5) -0.014(6) C24 0.043(5) 0.088(7) 0.072(7) -0.019(6) 0.005(5) 0.004(5) N7 0.080(6) 0.093(7) 0.078(6) -0.030(5) -0.002(5) -0.028(5) C25 0.117(9) 0.049(6) 0.089(8) -0.018(5) -0.021(7) -0.001(6) C26 0.169(14) 0.118(11) 0.080(8) -0.029(7) -0.032(8) -0.047(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 Fe1 N2 2.028(6) . ? Fe1 N4 2.048(6) . ? Fe1 O3 2.072(5) . ? Fe1 N6 2.207(6) . ? Fe1 N1 2.260(6) . ? N1 C15 1.462(9) . ? N1 C8 1.474(9) . ? N1 C1 1.481(9) . ? C1 C2 1.525(10) . ? C2 N2 1.455(8) . ? N2 C3 1.345(8) . ? N2 K1 3.306(6) . ? C3 O1 1.263(8) . ? C3 N3 1.378(8) . ? O1 K1 2.599(5) 2_665 ? O1 K1 2.871(6) . ? N3 C4 1.463(8) . ? C4 C7 1.504(11) . ? C4 C6 1.532(11) . ? C4 C5 1.535(11) . ? C8 C9 1.518(10) . ? C9 N4 1.477(9) . ? N4 C10 1.359(9) . ? C10 O2 1.240(8) . ? C10 N5 1.385(9) . ? O2 K1 2.565(5) 1_455 ? N5 C11 1.469(9) . ? C11 C14 1.525(11) . ? C11 C12 1.531(11) . ? C11 C13 1.533(11) . ? C15 C16 1.504(11) . ? C16 N6 1.339(9) . ? C16 C17 1.399(11) . ? C17 C18 1.362(13) . ? C18 C19 1.368(13) . ? C19 C20 1.356(11) . ? C20 N6 1.344(9) . ? O3 C21 1.283(8) . ? O4 C21 1.227(9) . ? O4 K1 2.775(6) . ? C21 C22 1.513(10) . ? K1 O2 2.565(5) 1_655 ? K1 O1 2.599(5) 2_665 ? K1 O5 2.678(6) . ? K1 K1 4.143(3) 2_665 ? O5 C24 1.200(11) . ? C23 C24 1.571(13) . ? C24 N7 1.302(12) . ? N7 C25 1.457(12) . ? N7 C26 1.489(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N4 114.3(2) . . ? N2 Fe1 O3 109.6(2) . . ? N4 Fe1 O3 103.3(2) . . ? N2 Fe1 N6 125.5(2) . . ? N4 Fe1 N6 108.6(2) . . ? O3 Fe1 N6 90.9(2) . . ? N2 Fe1 N1 80.0(2) . . ? N4 Fe1 N1 80.7(2) . . ? O3 Fe1 N1 166.2(2) . . ? N6 Fe1 N1 75.3(2) . . ? C15 N1 C8 111.8(6) . . ? C15 N1 C1 112.1(6) . . ? C8 N1 C1 114.2(6) . . ? C15 N1 Fe1 108.5(4) . . ? C8 N1 Fe1 104.1(4) . . ? C1 N1 Fe1 105.5(4) . . ? N1 C1 C2 110.2(6) . . ? N2 C2 C1 108.2(6) . . ? C3 N2 C2 113.8(6) . . ? C3 N2 Fe1 129.4(5) . . ? C2 N2 Fe1 115.4(4) . . ? C3 N2 K1 67.0(4) . . ? C2 N2 K1 89.3(4) . . ? Fe1 N2 K1 102.5(2) . . ? O1 C3 N2 125.3(6) . . ? O1 C3 N3 119.2(6) . . ? N2 C3 N3 115.4(6) . . ? C3 O1 K1 153.2(4) . 2_665 ? C3 O1 K1 85.5(4) . . ? K1 O1 K1 98.34(17) 2_665 . ? C3 N3 C4 125.3(6) . . ? N3 C4 C7 112.3(6) . . ? N3 C4 C6 105.9(6) . . ? C7 C4 C6 108.8(7) . . ? N3 C4 C5 110.0(6) . . ? C7 C4 C5 110.9(8) . . ? C6 C4 C5 108.8(7) . . ? N1 C8 C9 112.0(6) . . ? N4 C9 C8 108.1(6) . . ? C10 N4 C9 112.2(6) . . ? C10 N4 Fe1 129.2(5) . . ? C9 N4 Fe1 115.0(4) . . ? O2 C10 N4 125.0(6) . . ? O2 C10 N5 120.8(6) . . ? N4 C10 N5 114.2(6) . . ? C10 O2 K1 161.5(5) . 1_455 ? C10 N5 C11 124.1(6) . . ? N5 C11 C14 110.5(7) . . ? N5 C11 C12 105.1(6) . . ? C14 C11 C12 110.0(7) . . ? N5 C11 C13 110.2(6) . . ? C14 C11 C13 110.9(7) . . ? C12 C11 C13 109.9(7) . . ? N1 C15 C16 111.2(6) . . ? N6 C16 C17 121.6(8) . . ? N6 C16 C15 116.2(6) . . ? C17 C16 C15 122.2(8) . . ? C18 C17 C16 118.4(9) . . ? C17 C18 C19 119.8(8) . . ? C20 C19 C18 119.2(8) . . ? N6 C20 C19 122.7(8) . . ? C16 N6 C20 118.2(7) . . ? C16 N6 Fe1 116.2(5) . . ? C20 N6 Fe1 125.2(5) . . ? C21 O3 Fe1 121.8(5) . . ? C21 O4 K1 150.6(5) . . ? O4 C21 O3 124.3(7) . . ? O4 C21 C22 119.8(7) . . ? O3 C21 C22 115.9(7) . . ? O2 K1 O1 93.33(17) 1_655 2_665 ? O2 K1 O5 101.01(18) 1_655 . ? O1 K1 O5 87.81(18) 2_665 . ? O2 K1 O4 88.87(18) 1_655 . ? O1 K1 O4 176.81(17) 2_665 . ? O5 K1 O4 89.50(19) . . ? O2 K1 O1 137.66(17) 1_655 . ? O1 K1 O1 81.66(17) 2_665 . ? O5 K1 O1 120.62(17) . . ? O4 K1 O1 98.26(16) . . ? O2 K1 N2 158.74(16) 1_655 . ? O1 K1 N2 106.90(16) 2_665 . ? O5 K1 N2 86.56(16) . . ? O4 K1 N2 71.21(16) . . ? O1 K1 N2 43.35(14) . . ? O2 K1 K1 123.28(15) 1_655 2_665 ? O1 K1 K1 43.29(12) 2_665 2_665 ? O5 K1 K1 109.20(15) . 2_665 ? O4 K1 K1 136.55(14) . 2_665 ? O1 K1 K1 38.38(10) . 2_665 ? N2 K1 K1 71.25(11) . 2_665 ? C24 O5 K1 118.0(6) . . ? O5 C24 N7 123.2(10) . . ? O5 C24 C23 121.1(9) . . ? N7 C24 C23 115.7(9) . . ? C24 N7 C25 118.0(9) . . ? C24 N7 C26 124.1(10) . . ? C25 N7 C26 117.8(9) . . ? 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 N2 Fe1 N1 C15 -105.2(5) . . . . ? N4 Fe1 N1 C15 137.9(5) . . . . ? O3 Fe1 N1 C15 30.1(11) . . . . ? N6 Fe1 N1 C15 25.7(4) . . . . ? N2 Fe1 N1 C8 135.6(5) . . . . ? N4 Fe1 N1 C8 18.7(4) . . . . ? O3 Fe1 N1 C8 -89.0(9) . . . . ? N6 Fe1 N1 C8 -93.4(4) . . . . ? N2 Fe1 N1 C1 15.1(4) . . . . ? N4 Fe1 N1 C1 -101.8(5) . . . . ? O3 Fe1 N1 C1 150.4(8) . . . . ? N6 Fe1 N1 C1 146.0(5) . . . . ? C15 N1 C1 C2 79.0(7) . . . . ? C8 N1 C1 C2 -152.6(6) . . . . ? Fe1 N1 C1 C2 -38.9(6) . . . . ? N1 C1 C2 N2 51.0(8) . . . . ? C1 C2 N2 C3 154.6(6) . . . . ? C1 C2 N2 Fe1 -37.5(7) . . . . ? C1 C2 N2 K1 -141.0(5) . . . . ? N4 Fe1 N2 C3 -106.8(6) . . . . ? O3 Fe1 N2 C3 8.5(7) . . . . ? N6 Fe1 N2 C3 114.4(6) . . . . ? N1 Fe1 N2 C3 178.3(6) . . . . ? N4 Fe1 N2 C2 87.5(5) . . . . ? O3 Fe1 N2 C2 -157.2(5) . . . . ? N6 Fe1 N2 C2 -51.2(6) . . . . ? N1 Fe1 N2 C2 12.6(5) . . . . ? N4 Fe1 N2 K1 -177.23(19) . . . . ? O3 Fe1 N2 K1 -61.9(2) . . . . ? N6 Fe1 N2 K1 44.0(3) . . . . ? N1 Fe1 N2 K1 107.9(2) . . . . ? C2 N2 C3 O1 13.9(10) . . . . ? Fe1 N2 C3 O1 -151.9(6) . . . . ? K1 N2 C3 O1 -64.5(6) . . . . ? C2 N2 C3 N3 -167.5(6) . . . . ? Fe1 N2 C3 N3 26.7(9) . . . . ? K1 N2 C3 N3 114.1(6) . . . . ? N2 C3 O1 K1 -25.9(15) . . . 2_665 ? N3 C3 O1 K1 155.5(7) . . . 2_665 ? N2 C3 O1 K1 73.7(7) . . . . ? N3 C3 O1 K1 -104.9(6) . . . . ? O1 C3 N3 C4 8.9(10) . . . . ? N2 C3 N3 C4 -169.8(7) . . . . ? C3 N3 C4 C7 56.6(10) . . . . ? C3 N3 C4 C6 175.2(7) . . . . ? C3 N3 C4 C5 -67.4(10) . . . . ? C15 N1 C8 C9 -159.0(6) . . . . ? C1 N1 C8 C9 72.4(8) . . . . ? Fe1 N1 C8 C9 -42.1(7) . . . . ? N1 C8 C9 N4 50.5(8) . . . . ? C8 C9 N4 C10 167.6(6) . . . . ? C8 C9 N4 Fe1 -32.0(7) . . . . ? N2 Fe1 N4 C10 89.5(6) . . . . ? O3 Fe1 N4 C10 -29.5(6) . . . . ? N6 Fe1 N4 C10 -125.1(6) . . . . ? N1 Fe1 N4 C10 164.0(6) . . . . ? N2 Fe1 N4 C9 -67.0(5) . . . . ? O3 Fe1 N4 C9 174.0(5) . . . . ? N6 Fe1 N4 C9 78.5(5) . . . . ? N1 Fe1 N4 C9 7.5(5) . . . . ? C9 N4 C10 O2 -0.2(10) . . . . ? Fe1 N4 C10 O2 -157.2(6) . . . . ? C9 N4 C10 N5 -178.8(6) . . . . ? Fe1 N4 C10 N5 24.2(9) . . . . ? N4 C10 O2 K1 7(2) . . . 1_455 ? N5 C10 O2 K1 -174.3(12) . . . 1_455 ? O2 C10 N5 C11 9.9(11) . . . . ? N4 C10 N5 C11 -171.4(7) . . . . ? C10 N5 C11 C14 57.9(10) . . . . ? C10 N5 C11 C12 176.5(7) . . . . ? C10 N5 C11 C13 -65.1(10) . . . . ? C8 N1 C15 C16 75.7(7) . . . . ? C1 N1 C15 C16 -154.6(6) . . . . ? Fe1 N1 C15 C16 -38.5(7) . . . . ? N1 C15 C16 N6 33.3(9) . . . . ? N1 C15 C16 C17 -148.0(7) . . . . ? N6 C16 C17 C18 2.0(13) . . . . ? C15 C16 C17 C18 -176.6(8) . . . . ? C16 C17 C18 C19 -1.3(13) . . . . ? C17 C18 C19 C20 -0.1(13) . . . . ? C18 C19 C20 N6 0.9(12) . . . . ? C17 C16 N6 C20 -1.3(11) . . . . ? C15 C16 N6 C20 177.4(6) . . . . ? C17 C16 N6 Fe1 171.6(6) . . . . ? C15 C16 N6 Fe1 -9.7(8) . . . . ? C19 C20 N6 C16 -0.2(11) . . . . ? C19 C20 N6 Fe1 -172.4(6) . . . . ? N2 Fe1 N6 C16 56.9(6) . . . . ? N4 Fe1 N6 C16 -83.7(5) . . . . ? O3 Fe1 N6 C16 171.9(5) . . . . ? N1 Fe1 N6 C16 -9.1(5) . . . . ? N2 Fe1 N6 C20 -130.8(6) . . . . ? N4 Fe1 N6 C20 88.6(6) . . . . ? O3 Fe1 N6 C20 -15.7(6) . . . . ? N1 Fe1 N6 C20 163.2(6) . . . . ? N2 Fe1 O3 C21 60.5(6) . . . . ? N4 Fe1 O3 C21 -177.3(5) . . . . ? N6 Fe1 O3 C21 -67.9(5) . . . . ? N1 Fe1 O3 C21 -72.2(11) . . . . ? K1 O4 C21 O3 -47.7(15) . . . . ? K1 O4 C21 C22 134.7(9) . . . . ? Fe1 O3 C21 O4 -4.7(10) . . . . ? Fe1 O3 C21 C22 173.0(5) . . . . ? C21 O4 K1 O2 -144.7(11) . . . 1_655 ? C21 O4 K1 O1 82(3) . . . 2_665 ? C21 O4 K1 O5 114.2(11) . . . . ? C21 O4 K1 O1 -6.7(11) . . . . ? C21 O4 K1 N2 27.7(11) . . . . ? C21 O4 K1 K1 -3.7(12) . . . 2_665 ? C3 O1 K1 O2 120.9(4) . . . 1_655 ? K1 O1 K1 O2 -85.8(3) 2_665 . . 1_655 ? C3 O1 K1 O1 -153.3(4) . . . 2_665 ? K1 O1 K1 O1 0.0 2_665 . . 2_665 ? C3 O1 K1 O5 -70.9(4) . . . . ? K1 O1 K1 O5 82.4(2) 2_665 . . . ? C3 O1 K1 O4 23.5(4) . . . . ? K1 O1 K1 O4 176.77(17) 2_665 . . . ? C3 O1 K1 N2 -27.6(3) . . . . ? K1 O1 K1 N2 125.7(2) 2_665 . . . ? C3 O1 K1 K1 -153.3(4) . . . 2_665 ? C3 N2 K1 O2 -76.1(6) . . . 1_655 ? C2 N2 K1 O2 167.5(5) . . . 1_655 ? Fe1 N2 K1 O2 51.7(5) . . . 1_655 ? C3 N2 K1 O1 85.3(4) . . . 2_665 ? C2 N2 K1 O1 -31.0(4) . . . 2_665 ? Fe1 N2 K1 O1 -146.9(2) . . . 2_665 ? C3 N2 K1 O5 172.0(4) . . . . ? C2 N2 K1 O5 55.6(4) . . . . ? Fe1 N2 K1 O5 -60.2(2) . . . . ? C3 N2 K1 O4 -97.4(4) . . . . ? C2 N2 K1 O4 146.3(4) . . . . ? Fe1 N2 K1 O4 30.4(2) . . . . ? C3 N2 K1 O1 28.2(4) . . . . ? C2 N2 K1 O1 -88.2(4) . . . . ? Fe1 N2 K1 O1 156.0(3) . . . . ? C3 N2 K1 K1 60.3(4) . . . 2_665 ? C2 N2 K1 K1 -56.0(4) . . . 2_665 ? Fe1 N2 K1 K1 -171.9(2) . . . 2_665 ? O2 K1 O5 C24 -24.9(7) 1_655 . . . ? O1 K1 O5 C24 -117.8(7) 2_665 . . . ? O4 K1 O5 C24 63.9(7) . . . . ? O1 K1 O5 C24 163.2(6) . . . . ? N2 K1 O5 C24 135.1(7) . . . . ? K1 K1 O5 C24 -156.1(6) 2_665 . . . ? K1 O5 C24 N7 153.3(7) . . . . ? K1 O5 C24 C23 -27.5(11) . . . . ? O5 C24 N7 C25 0.4(14) . . . . ? C23 C24 N7 C25 -178.8(8) . . . . ? O5 C24 N7 C26 -177.4(10) . . . . ? C23 C24 N7 C26 3.4(14) . . . . ? 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 N5 H5D O3 0.88 2.10 2.924(8) 154.7 . _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.997 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.105