Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'J.Chem.Soc.,Dalton Trans.' _journal_coden_Cambridge 0186 loop_ _publ_author_name 'Karl Wieghardt' 'Kil Sik Min' 'Thomas Weyhermuller' _publ_contact_author_name 'Prof Karl Wieghardt' _publ_contact_author_address ; Max-Planck-Institut fur Strahlenchemie Stiftstrasse 34-36 Mulheim an der Ruhr D-45470 GERMANY ; _publ_contact_author_email WIEGHARDT@MPI-MUELHEIM.MPG.DE _publ_section_title ; O,N-Coordinated o-Iminobenzoquinone, LIBQ, and o-Iminobenzosemiquinonato(1-),(LISQ)1-, Ligands in [NiII(tren)(LIBQ)](PF6)2, [NiII(tren)(LISQ)](CIO4), [CoIII-(tren)(LISQ)](CIO4)2, and [FeIII(tren)(LISQ)](CIO4)2 Complexes ; data_1 _database_code_CSD 197833 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[C26 H43 N5 Ni O]2+, 2 (P F6)-' _chemical_formula_sum 'C26 H43 F12 N5 Ni O P2' _chemical_formula_weight 790.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.9270(6) _cell_length_b 17.4997(9) _cell_length_c 15.2769(9) _cell_angle_alpha 90.00 _cell_angle_beta 92.95(1) _cell_angle_gamma 90.00 _cell_volume 3451.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent parallelepiped' _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 0.749 _exptl_absorpt_correction_type 'Gaussian, face indexed' _exptl_absorpt_correction_T_min 0.8769 _exptl_absorpt_correction_T_max 0.8959 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Monius Kappa-CCD' _diffrn_measurement_method '1072 images at 1.0 deg. in \w and 20 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 72291 _diffrn_reflns_av_R_equivalents 0.1144 _diffrn_reflns_av_sigmaI/netI 0.0487 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 26.36 _reflns_number_total 7025 _reflns_number_gt 5377 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO, Nonius Collect Software' _computing_cell_refinement 'DENZO, Nonius Collect Software' _computing_data_reduction 'DENZO, Nonius Collect Software' _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 w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+7.0719P] 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 7025 _refine_ls_number_parameters 482 _refine_ls_number_restraints 186 _refine_ls_R_factor_all 0.0774 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1201 _refine_ls_wR_factor_gt 0.1095 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.061 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.78472(3) 0.83770(2) 0.85805(3) 0.01598(11) Uani 1 d . . . O1 O 0.62383(16) 0.86167(12) 0.84924(14) 0.0199(5) Uani 1 d . . . C1 C 0.5664(2) 0.80555(19) 0.8527(2) 0.0188(7) Uani 1 d . . . C2 C 0.4532(2) 0.81003(19) 0.8508(2) 0.0203(7) Uani 1 d . . . C3 C 0.4026(2) 0.74322(19) 0.8592(2) 0.0229(7) Uani 1 d . . . H3 H 0.3292 0.7455 0.8596 0.027 Uiso 1 calc R . . C4 C 0.4503(2) 0.66732(18) 0.8679(2) 0.0197(7) Uani 1 d . . . C5 C 0.5545(2) 0.66055(18) 0.8689(2) 0.0188(6) Uani 1 d . . . H5 H 0.5859 0.6116 0.8738 0.023 Uiso 1 calc R . . C6 C 0.6172(2) 0.72756(18) 0.8623(2) 0.0181(7) Uani 1 d . . . N7 N 0.7177(2) 0.73138(15) 0.86209(17) 0.0186(6) Uani 1 d . . . C8 C 0.7824(2) 0.66541(17) 0.8757(2) 0.0154(6) Uani 1 d . . . C9 C 0.7807(3) 0.62654(19) 0.9586(2) 0.0247(7) Uani 1 d . . . H9 H 0.7330 0.6407 1.0010 0.030 Uiso 1 calc R . . C10 C 0.8511(3) 0.5675(2) 0.9744(2) 0.0306(8) Uani 1 d . . . H10 H 0.8525 0.5411 1.0288 0.037 Uiso 1 calc R . . C11 C 0.9196(3) 0.5467(2) 0.9109(3) 0.0346(9) Uani 1 d . . . H11 H 0.9664 0.5055 0.9219 0.042 Uiso 1 calc R . . C12 C 0.9196(3) 0.5854(2) 0.8326(3) 0.0315(8) Uani 1 d . . . H12 H 0.9669 0.5711 0.7898 0.038 Uiso 1 calc R . . C13 C 0.8512(2) 0.64519(19) 0.8157(2) 0.0240(7) Uani 1 d . . . H13 H 0.8524 0.6722 0.7618 0.029 Uiso 1 calc R . . C14 C 0.3997(3) 0.88759(19) 0.8392(3) 0.0278(8) Uani 1 d . . . C15 C 0.4363(3) 0.9415(2) 0.9145(3) 0.0425(11) Uani 1 d . . . H15A H 0.4058 0.9922 0.9046 0.064 Uiso 1 calc R . . H15B H 0.5120 0.9454 0.9166 0.064 Uiso 1 calc R . . H15C H 0.4142 0.9210 0.9703 0.064 Uiso 1 calc R . . C16 C 0.4263(3) 0.9213(2) 0.7501(3) 0.0410(10) Uani 1 d . . . H16A H 0.3923 0.9710 0.7419 0.061 Uiso 1 calc R . . H16B H 0.4021 0.8865 0.7031 0.061 Uiso 1 calc R . . H16C H 0.5015 0.9278 0.7485 0.061 Uiso 1 calc R . . C17 C 0.2818(3) 0.8795(2) 0.8402(3) 0.0371(10) Uani 1 d . . . H17A H 0.2492 0.9291 0.8275 0.056 Uiso 1 calc R . . H17B H 0.2628 0.8618 0.8981 0.056 Uiso 1 calc R . . H17C H 0.2578 0.8423 0.7956 0.056 Uiso 1 calc R . . C18 C 0.3778(3) 0.5994(2) 0.8773(2) 0.0261(8) Uani 1 d . . . C19 C 0.3272(3) 0.6085(2) 0.9666(3) 0.0446(11) Uani 1 d . . . H19A H 0.2890 0.6568 0.9674 0.067 Uiso 1 calc R . . H19B H 0.3812 0.6083 1.0141 0.067 Uiso 1 calc R . . H19C H 0.2794 0.5659 0.9749 0.067 Uiso 1 calc R . . C20 C 0.4344(3) 0.5234(2) 0.8761(3) 0.0327(9) Uani 1 d . . . H20A H 0.3843 0.4816 0.8789 0.049 Uiso 1 calc R . . H20B H 0.4840 0.5204 0.9267 0.049 Uiso 1 calc R . . H20C H 0.4715 0.5191 0.8220 0.049 Uiso 1 calc R . . C21 C 0.2936(3) 0.5996(2) 0.8022(3) 0.0440(11) Uani 1 d . . . H21A H 0.2631 0.6508 0.7965 0.066 Uiso 1 calc R . . H21B H 0.2396 0.5626 0.8150 0.066 Uiso 1 calc R . . H21C H 0.3246 0.5856 0.7472 0.066 Uiso 1 calc R . . N30 N 0.8278(2) 0.95175(15) 0.86194(17) 0.0196(6) Uani 1 d . . . C31 C 0.7795(3) 0.98604(19) 0.7802(2) 0.0250(7) Uani 1 d . . . H31A H 0.8082 1.0378 0.7716 0.030 Uiso 1 calc R . . H31B H 0.7038 0.9909 0.7858 0.030 Uiso 1 calc R . . C32 C 0.8004(3) 0.9363(2) 0.7012(2) 0.0271(8) Uani 1 d . . . H32A H 0.7562 0.9534 0.6501 0.033 Uiso 1 calc R . . H32B H 0.8737 0.9420 0.6865 0.033 Uiso 1 calc R . . N33 N 0.7785(2) 0.85457(16) 0.71991(18) 0.0232(6) Uani 1 d . . . H33A H 0.8266 0.8239 0.6948 0.028 Uiso 1 calc R . . H33B H 0.7139 0.8416 0.6964 0.028 Uiso 1 calc R . . C34 C 0.9427(2) 0.9577(2) 0.8666(2) 0.0238(7) Uani 1 d . . . H34A H 0.9673 0.9661 0.9283 0.029 Uiso 1 calc R . . H34B H 0.9634 1.0026 0.8322 0.029 Uiso 1 calc R . . C35 C 0.9946(3) 0.8866(2) 0.8319(2) 0.0254(8) Uani 1 d . . . H35A H 0.9904 0.8872 0.7670 0.031 Uiso 1 calc R . . H35B H 1.0687 0.8861 0.8520 0.031 Uiso 1 calc R . . N36 N 0.9430(2) 0.81716(15) 0.86383(17) 0.0206(6) Uani 1 d . . . H36A H 0.9659 0.8066 0.9206 0.025 Uiso 1 calc R . . H36B H 0.9577 0.7759 0.8293 0.025 Uiso 1 calc R . . C37 C 0.7829(3) 0.98371(19) 0.9420(2) 0.0237(7) Uani 1 d . . . H37A H 0.7069 0.9892 0.9322 0.028 Uiso 1 calc R . . H37B H 0.8125 1.0349 0.9548 0.028 Uiso 1 calc R . . C38 C 0.8070(3) 0.93056(19) 1.0193(2) 0.0238(7) Uani 1 d . . . H38A H 0.8821 0.9322 1.0357 0.029 Uiso 1 calc R . . H38B H 0.7688 0.9474 1.0704 0.029 Uiso 1 calc R . . N39 N 0.7763(2) 0.85166(15) 0.99475(17) 0.0206(6) Uani 1 d . . . H39A H 0.7098 0.8424 1.0107 0.025 Uiso 1 calc R . . H39B H 0.8198 0.8173 1.0237 0.025 Uiso 1 calc R . . P1 P 0.5790(2) 0.7594(2) 1.14251(17) 0.0290(6) Uani 0.698(8) d PD A 1 F11 F 0.5891(7) 0.7549(4) 1.2477(3) 0.0467(15) Uani 0.698(8) d PD A 1 F12 F 0.5695(6) 0.7673(6) 1.0384(3) 0.050(3) Uani 0.698(8) d PD A 1 F13 F 0.5870(5) 0.8498(2) 1.1487(5) 0.0575(17) Uani 0.698(8) d PD A 1 F14 F 0.7018(3) 0.7547(3) 1.1400(4) 0.0629(18) Uani 0.698(8) d PD A 1 F15 F 0.5730(6) 0.6696(2) 1.1369(3) 0.085(2) Uani 0.698(8) d PD A 1 F16 F 0.4573(3) 0.7636(4) 1.1471(3) 0.066(2) Uani 0.698(8) d PD A 1 P1X P 0.5589(5) 0.7808(4) 1.1393(4) 0.0290(6) Uani 0.302(8) d PD A 2 F11X F 0.5619(12) 0.7800(11) 1.2435(5) 0.048(4) Uani 0.302(8) d PD A 2 F12X F 0.5591(17) 0.7816(12) 1.0351(5) 0.046(5) Uani 0.302(8) d PD A 2 F13X F 0.4575(6) 0.8321(9) 1.1372(6) 0.081(5) Uani 0.302(8) d PD A 2 F14X F 0.4892(10) 0.7058(7) 1.1356(6) 0.079(6) Uani 0.302(8) d PD A 2 F15X F 0.6605(8) 0.7293(6) 1.1406(9) 0.063(4) Uani 0.302(8) d PD A 2 F16X F 0.6285(9) 0.8553(5) 1.1437(10) 0.056(4) Uani 0.302(8) d PD A 2 P2 P 1.07129(7) 0.78925(5) 1.10160(6) 0.0275(2) Uani 1 d . . . F21 F 1.1470(3) 0.74170(19) 1.0484(2) 0.0822(10) Uani 1 d . . . F22 F 1.1630(3) 0.82833(19) 1.1559(2) 0.0911(12) Uani 1 d . . . F23 F 0.9918(3) 0.83787(18) 1.15490(19) 0.0863(11) Uani 1 d . . . F24 F 0.9740(2) 0.75208(15) 1.04945(17) 0.0570(8) Uani 1 d . . . F25 F 1.07194(19) 0.85646(13) 1.02933(14) 0.0453(6) Uani 1 d . . . F26 F 1.06832(17) 0.72311(13) 1.17392(14) 0.0404(6) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01294(19) 0.0186(2) 0.0164(2) 0.00002(17) 0.00134(14) -0.00078(17) O1 0.0171(11) 0.0199(12) 0.0227(12) 0.0011(9) 0.0010(9) -0.0017(9) C1 0.0195(16) 0.0241(17) 0.0128(15) -0.0007(13) 0.0009(12) -0.0027(14) C2 0.0153(15) 0.0240(17) 0.0217(17) -0.0021(13) 0.0012(13) 0.0013(13) C3 0.0133(15) 0.0268(18) 0.0285(19) 0.0003(14) 0.0013(13) -0.0001(13) C4 0.0222(16) 0.0194(16) 0.0177(16) -0.0032(13) 0.0021(12) -0.0019(13) C5 0.0212(16) 0.0179(15) 0.0171(16) 0.0005(13) 0.0005(12) -0.0001(13) C6 0.0148(15) 0.0245(17) 0.0150(16) 0.0005(13) 0.0010(12) 0.0006(13) N7 0.0180(14) 0.0222(14) 0.0154(13) -0.0019(11) 0.0006(10) 0.0004(11) C8 0.0071(13) 0.0115(14) 0.0266(17) -0.0057(13) -0.0071(12) 0.0021(12) C9 0.0197(17) 0.0260(18) 0.0281(19) 0.0037(15) -0.0017(14) -0.0023(14) C10 0.030(2) 0.0256(19) 0.034(2) 0.0066(16) -0.0136(16) -0.0002(15) C11 0.028(2) 0.027(2) 0.048(2) -0.0033(17) -0.0116(17) 0.0074(16) C12 0.0223(18) 0.031(2) 0.042(2) -0.0114(17) 0.0018(16) 0.0060(15) C13 0.0207(17) 0.0220(18) 0.0289(19) -0.0025(14) -0.0021(14) 0.0001(13) C14 0.0149(17) 0.0216(18) 0.047(2) -0.0013(16) 0.0016(15) 0.0006(14) C15 0.0210(19) 0.029(2) 0.077(3) -0.023(2) 0.0045(19) 0.0032(16) C16 0.023(2) 0.033(2) 0.066(3) 0.022(2) -0.0010(19) 0.0024(16) C17 0.0204(19) 0.0226(19) 0.068(3) -0.0022(18) 0.0023(18) 0.0036(15) C18 0.0230(18) 0.0234(18) 0.032(2) 0.0004(15) 0.0045(15) -0.0039(14) C19 0.047(3) 0.037(2) 0.052(3) -0.003(2) 0.028(2) -0.0115(19) C20 0.028(2) 0.0259(19) 0.045(2) 0.0021(16) 0.0057(17) -0.0068(15) C21 0.032(2) 0.034(2) 0.064(3) -0.001(2) -0.015(2) -0.0117(18) N30 0.0168(13) 0.0245(15) 0.0174(14) 0.0011(11) 0.0008(10) -0.0023(11) C31 0.0245(18) 0.0229(18) 0.0274(19) 0.0059(14) 0.0002(14) -0.0005(14) C32 0.0254(18) 0.033(2) 0.0225(18) 0.0088(15) 0.0000(14) -0.0014(15) N33 0.0183(14) 0.0300(16) 0.0211(15) -0.0040(12) -0.0008(11) -0.0009(12) C34 0.0182(17) 0.0285(19) 0.0246(18) -0.0015(14) -0.0003(13) -0.0091(14) C35 0.0155(16) 0.033(2) 0.0279(19) -0.0016(15) 0.0015(14) -0.0033(14) N36 0.0181(14) 0.0255(15) 0.0180(14) -0.0025(11) -0.0001(11) 0.0007(11) C37 0.0227(17) 0.0195(17) 0.0293(19) -0.0053(14) 0.0042(14) -0.0003(14) C38 0.0196(17) 0.0317(19) 0.0204(17) -0.0074(14) 0.0050(13) -0.0017(14) N39 0.0178(14) 0.0250(15) 0.0192(14) 0.0007(11) 0.0039(11) 0.0003(11) P1 0.0322(13) 0.0316(15) 0.0245(6) -0.0003(9) 0.0138(7) -0.0051(11) F11 0.056(4) 0.059(4) 0.026(2) 0.0063(19) 0.0142(19) -0.016(3) F12 0.056(5) 0.072(4) 0.023(4) -0.007(3) 0.012(3) -0.020(4) F13 0.082(4) 0.032(3) 0.058(3) -0.002(2) -0.008(3) -0.001(2) F14 0.035(3) 0.106(4) 0.049(3) 0.030(3) 0.018(2) 0.011(3) F15 0.157(6) 0.035(2) 0.067(3) -0.008(2) 0.046(4) -0.019(3) F16 0.030(2) 0.124(6) 0.047(3) -0.015(3) 0.0162(18) -0.017(3) P1X 0.0322(13) 0.0316(15) 0.0245(6) -0.0003(9) 0.0138(7) -0.0051(11) F11X 0.052(10) 0.069(11) 0.023(5) -0.006(5) 0.010(4) -0.021(7) F12X 0.041(8) 0.071(11) 0.028(9) 0.014(6) 0.009(6) -0.014(7) F13X 0.061(7) 0.139(14) 0.044(6) 0.027(7) 0.022(5) 0.041(8) F14X 0.110(13) 0.102(11) 0.027(5) 0.002(7) 0.005(6) -0.084(10) F15X 0.051(9) 0.074(9) 0.064(7) 0.010(6) 0.015(7) 0.036(7) F16X 0.076(10) 0.065(8) 0.028(5) -0.008(5) 0.009(6) -0.038(6) P2 0.0295(5) 0.0289(5) 0.0234(5) 0.0034(4) -0.0063(4) -0.0012(4) F21 0.088(2) 0.093(2) 0.070(2) 0.0131(17) 0.0421(18) 0.0438(19) F22 0.111(3) 0.085(2) 0.070(2) 0.0375(17) -0.0615(19) -0.060(2) F23 0.129(3) 0.077(2) 0.0556(18) 0.0125(16) 0.0307(18) 0.055(2) F24 0.0539(16) 0.0628(17) 0.0510(16) 0.0297(13) -0.0301(13) -0.0282(13) F25 0.0591(16) 0.0400(13) 0.0349(13) 0.0124(10) -0.0160(11) -0.0191(11) F26 0.0427(13) 0.0429(13) 0.0343(13) 0.0158(10) -0.0099(10) -0.0021(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N7 2.054(3) . ? Ni1 N30 2.072(3) . ? Ni1 N36 2.074(3) . ? Ni1 N39 2.111(3) . ? Ni1 O1 2.119(2) . ? Ni1 N33 2.128(3) . ? O1 C1 1.234(4) . ? C1 C2 1.463(4) . ? C1 C6 1.519(4) . ? C2 C3 1.349(5) . ? C2 C14 1.529(5) . ? C3 C4 1.467(4) . ? C4 C5 1.352(4) . ? C4 C18 1.524(4) . ? C5 C6 1.432(4) . ? C6 N7 1.301(4) . ? N7 C8 1.435(4) . ? C8 C13 1.355(4) . ? C8 C9 1.439(4) . ? C9 C10 1.390(5) . ? C10 C11 1.395(5) . ? C11 C12 1.376(5) . ? C12 C13 1.386(5) . ? C14 C17 1.533(5) . ? C14 C16 1.538(5) . ? C14 C15 1.543(5) . ? C18 C20 1.519(5) . ? C18 C21 1.541(5) . ? C18 C19 1.552(5) . ? N30 C34 1.486(4) . ? N30 C37 1.490(4) . ? N30 C31 1.493(4) . ? C31 C32 1.523(5) . ? C32 N33 1.489(4) . ? C34 C35 1.523(5) . ? C35 N36 1.481(4) . ? C37 C38 1.523(5) . ? C38 N39 1.479(4) . ? P1 F15 1.575(4) . ? P1 F16 1.580(4) . ? P1 F13 1.589(4) . ? P1 F14 1.593(4) . ? P1 F12 1.594(4) . ? P1 F11 1.608(4) . ? P1X F16X 1.584(6) . ? P1X F13X 1.587(6) . ? P1X F14X 1.590(6) . ? P1X F11X 1.590(6) . ? P1X F15X 1.593(6) . ? P1X F12X 1.593(6) . ? P2 F21 1.547(3) . ? P2 F22 1.569(3) . ? P2 F23 1.590(3) . ? P2 F24 1.593(2) . ? P2 F26 1.602(2) . ? P2 F25 1.613(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Ni1 N30 169.91(10) . . ? N7 Ni1 N36 104.96(10) . . ? N30 Ni1 N36 84.40(11) . . ? N7 Ni1 N39 91.83(10) . . ? N30 Ni1 N39 83.55(10) . . ? N36 Ni1 N39 94.51(10) . . ? N7 Ni1 O1 76.54(9) . . ? N30 Ni1 O1 94.18(9) . . ? N36 Ni1 O1 178.12(10) . . ? N39 Ni1 O1 86.54(9) . . ? N7 Ni1 N33 99.25(10) . . ? N30 Ni1 N33 83.76(10) . . ? N36 Ni1 N33 93.06(11) . . ? N39 Ni1 N33 164.50(10) . . ? O1 Ni1 N33 85.55(10) . . ? C1 O1 Ni1 115.5(2) . . ? O1 C1 C2 124.0(3) . . ? O1 C1 C6 117.4(3) . . ? C2 C1 C6 118.5(3) . . ? C3 C2 C1 116.2(3) . . ? C3 C2 C14 124.2(3) . . ? C1 C2 C14 119.7(3) . . ? C2 C3 C4 126.1(3) . . ? C5 C4 C3 119.6(3) . . ? C5 C4 C18 123.2(3) . . ? C3 C4 C18 117.2(3) . . ? C4 C5 C6 119.7(3) . . ? N7 C6 C5 127.7(3) . . ? N7 C6 C1 112.4(3) . . ? C5 C6 C1 119.9(3) . . ? C6 N7 C8 122.2(3) . . ? C6 N7 Ni1 118.0(2) . . ? C8 N7 Ni1 119.30(19) . . ? C13 C8 N7 120.7(3) . . ? C13 C8 C9 120.8(3) . . ? N7 C8 C9 118.2(3) . . ? C10 C9 C8 117.7(3) . . ? C9 C10 C11 120.5(3) . . ? C12 C11 C10 120.3(3) . . ? C11 C12 C13 120.3(3) . . ? C8 C13 C12 120.4(3) . . ? C2 C14 C17 111.2(3) . . ? C2 C14 C16 108.8(3) . . ? C17 C14 C16 108.2(3) . . ? C2 C14 C15 109.7(3) . . ? C17 C14 C15 108.4(3) . . ? C16 C14 C15 110.6(3) . . ? C20 C18 C4 112.5(3) . . ? C20 C18 C21 108.4(3) . . ? C4 C18 C21 110.0(3) . . ? C20 C18 C19 108.9(3) . . ? C4 C18 C19 107.0(3) . . ? C21 C18 C19 109.9(3) . . ? C34 N30 C37 111.4(2) . . ? C34 N30 C31 112.7(3) . . ? C37 N30 C31 111.8(3) . . ? C34 N30 Ni1 109.6(2) . . ? C37 N30 Ni1 105.62(19) . . ? C31 N30 Ni1 105.23(19) . . ? N30 C31 C32 110.4(3) . . ? N33 C32 C31 110.7(3) . . ? C32 N33 Ni1 109.0(2) . . ? N30 C34 C35 112.5(3) . . ? N36 C35 C34 110.0(3) . . ? C35 N36 Ni1 107.7(2) . . ? N30 C37 C38 109.5(3) . . ? N39 C38 C37 109.4(3) . . ? C38 N39 Ni1 109.37(19) . . ? F15 P1 F16 90.2(3) . . ? F15 P1 F13 179.0(3) . . ? F16 P1 F13 90.7(3) . . ? F15 P1 F14 89.7(3) . . ? F16 P1 F14 178.8(3) . . ? F13 P1 F14 89.4(3) . . ? F15 P1 F12 91.8(4) . . ? F16 P1 F12 90.8(3) . . ? F13 P1 F12 88.5(4) . . ? F14 P1 F12 90.3(3) . . ? F15 P1 F11 90.4(3) . . ? F16 P1 F11 89.3(4) . . ? F13 P1 F11 89.3(3) . . ? F14 P1 F11 89.6(4) . . ? F12 P1 F11 177.8(4) . . ? F16X P1X F13X 90.1(4) . . ? F16X P1X F14X 179.6(6) . . ? F13X P1X F14X 90.0(4) . . ? F16X P1X F11X 88.9(9) . . ? F13X P1X F11X 90.2(4) . . ? F14X P1X F11X 90.8(9) . . ? F16X P1X F15X 89.9(4) . . ? F13X P1X F15X 179.5(6) . . ? F14X P1X F15X 90.0(4) . . ? F11X P1X F15X 90.3(4) . . ? F16X P1X F12X 90.3(4) . . ? F13X P1X F12X 91.0(10) . . ? F14X P1X F12X 90.1(4) . . ? F11X P1X F12X 178.5(10) . . ? F15X P1X F12X 88.5(10) . . ? F21 P2 F22 91.7(2) . . ? F21 P2 F23 178.9(2) . . ? F22 P2 F23 89.3(2) . . ? F21 P2 F24 91.28(19) . . ? F22 P2 F24 177.0(2) . . ? F23 P2 F24 87.73(19) . . ? F21 P2 F26 90.67(15) . . ? F22 P2 F26 89.70(13) . . ? F23 P2 F26 89.69(15) . . ? F24 P2 F26 90.21(12) . . ? F21 P2 F25 90.40(16) . . ? F22 P2 F25 90.78(13) . . ? F23 P2 F25 89.23(15) . . ? F24 P2 F25 89.27(12) . . ? F26 P2 F25 178.81(14) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.696 _refine_diff_density_min -0.447 _refine_diff_density_rms 0.078 #===END data_2 _database_code_CSD 197834 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[C26 H43 N5 Ni O]+, (B F4)-' _chemical_formula_sum 'C26 H43 B F4 N5 Ni O' _chemical_formula_weight 587.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 36.162(2) _cell_length_b 20.3647(8) _cell_length_c 11.9060(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8767.9(7) _cell_formula_units_Z 12 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent parallelepiped' _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3732 _exptl_absorpt_coefficient_mu 0.717 _exptl_absorpt_correction_type 'Gaussian, face-indexed' _exptl_absorpt_correction_T_min 0.8081 _exptl_absorpt_correction_T_max 0.9553 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '661 images at 0.5 deg. in \w and 90 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55386 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.0702 _diffrn_reflns_limit_h_min -50 _diffrn_reflns_limit_h_max 50 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 30.00 _reflns_number_total 21156 _reflns_number_gt 17088 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO, Nonius Collect Software' _computing_cell_refinement 'DENZO, Nonius Collect Software' _computing_data_reduction 'DENZO, Nonius Collect Software' _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 w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+3.2999P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.000(6) _refine_ls_number_reflns 21156 _refine_ls_number_parameters 1045 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.0839 _refine_ls_wR_factor_gt 0.0768 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.685083(8) 0.170588(13) 0.09756(3) 0.01246(6) Uani 1 d . . . Ni2 Ni 0.475848(8) 0.173201(14) 0.58641(3) 0.01666(7) Uani 1 d . . . Ni3 Ni 0.342380(8) 0.189723(13) 0.08935(3) 0.01511(6) Uani 1 d . . . O1 O 0.64293(5) 0.22012(8) 0.17610(14) 0.0157(4) Uani 1 d . . . C1 C 0.64259(7) 0.28228(11) 0.15357(19) 0.0125(5) Uani 1 d . . . C2 C 0.61442(7) 0.32628(12) 0.1929(2) 0.0149(5) Uani 1 d . . . C3 C 0.61661(7) 0.39104(12) 0.1611(2) 0.0158(5) Uani 1 d . . . H3 H 0.5972 0.4195 0.1840 0.019 Uiso 1 calc R . . C4 C 0.64595(6) 0.41855(10) 0.0962(2) 0.0153(4) Uani 1 d . . . C5 C 0.67389(7) 0.37778(11) 0.06189(18) 0.0127(5) Uani 1 d . . . H5 H 0.6942 0.3955 0.0214 0.015 Uiso 1 calc R . . C6 C 0.67292(6) 0.30899(10) 0.0860(2) 0.0123(4) Uani 1 d . . . N7 N 0.69869(6) 0.26440(10) 0.05640(16) 0.0132(4) Uani 1 d . . . C8 C 0.72970(7) 0.28253(11) -0.0101(2) 0.0127(5) Uani 1 d . . . C9 C 0.72614(8) 0.31264(12) -0.1159(2) 0.0171(5) Uani 1 d . . . H9 H 0.7023 0.3226 -0.1450 0.021 Uiso 1 calc R . . C10 C 0.75759(8) 0.32781(12) -0.1778(2) 0.0198(6) Uani 1 d . . . H10 H 0.7551 0.3484 -0.2490 0.024 Uiso 1 calc R . . C11 C 0.79268(8) 0.31318(13) -0.1365(2) 0.0200(6) Uani 1 d . . . H11 H 0.8141 0.3250 -0.1781 0.024 Uiso 1 calc R . . C12 C 0.79618(7) 0.28105(12) -0.0337(2) 0.0174(5) Uani 1 d . . . H12 H 0.8200 0.2696 -0.0062 0.021 Uiso 1 calc R . . C13 C 0.76472(7) 0.26576(11) 0.0286(2) 0.0148(5) Uani 1 d . . . H13 H 0.7672 0.2436 0.0983 0.018 Uiso 1 calc R . . C14 C 0.58339(7) 0.30030(13) 0.2695(2) 0.0170(5) Uani 1 d . . . C15 C 0.56039(8) 0.24896(15) 0.2066(2) 0.0264(6) Uani 1 d . . . H15A H 0.5506 0.2683 0.1374 0.040 Uiso 1 calc R . . H15B H 0.5399 0.2345 0.2543 0.040 Uiso 1 calc R . . H15C H 0.5760 0.2112 0.1879 0.040 Uiso 1 calc R . . C16 C 0.55727(8) 0.35565(15) 0.3071(3) 0.0305(7) Uani 1 d . . . H16A H 0.5714 0.3892 0.3475 0.046 Uiso 1 calc R . . H16B H 0.5382 0.3376 0.3568 0.046 Uiso 1 calc R . . H16C H 0.5455 0.3754 0.2411 0.046 Uiso 1 calc R . . C17 C 0.60066(8) 0.27033(14) 0.3768(2) 0.0216(6) Uani 1 d . . . H17A H 0.6168 0.2337 0.3560 0.032 Uiso 1 calc R . . H17B H 0.5809 0.2544 0.4262 0.032 Uiso 1 calc R . . H17C H 0.6151 0.3039 0.4160 0.032 Uiso 1 calc R . . C18 C 0.64380(7) 0.49130(12) 0.0623(2) 0.0168(5) Uani 1 d . . . C19 C 0.68047(8) 0.51751(13) 0.0160(2) 0.0234(6) Uani 1 d . . . H19A H 0.6874 0.4924 -0.0509 0.035 Uiso 1 calc R . . H19B H 0.6998 0.5130 0.0733 0.035 Uiso 1 calc R . . H19C H 0.6776 0.5639 -0.0040 0.035 Uiso 1 calc R . . C20 C 0.63273(9) 0.53479(13) 0.1629(2) 0.0279(6) Uani 1 d . . . H20A H 0.6335 0.5811 0.1404 0.042 Uiso 1 calc R . . H20B H 0.6501 0.5276 0.2250 0.042 Uiso 1 calc R . . H20C H 0.6077 0.5234 0.1872 0.042 Uiso 1 calc R . . C21 C 0.61414(7) 0.49837(13) -0.0303(2) 0.0243(6) Uani 1 d . . . H21A H 0.6223 0.4751 -0.0979 0.036 Uiso 1 calc R . . H21B H 0.6106 0.5450 -0.0478 0.036 Uiso 1 calc R . . H21C H 0.5908 0.4796 -0.0039 0.036 Uiso 1 calc R . . N30 N 0.66448(6) 0.07654(10) 0.13620(17) 0.0149(4) Uani 1 d . . . C31 C 0.68835(7) 0.02594(11) 0.0819(2) 0.0188(5) Uani 1 d . . . H31A H 0.6727 -0.0110 0.0564 0.023 Uiso 1 calc R . . H31B H 0.7060 0.0086 0.1381 0.023 Uiso 1 calc R . . C32 C 0.71002(7) 0.05306(12) -0.0188(2) 0.0189(5) Uani 1 d . . . H32A H 0.7302 0.0224 -0.0386 0.023 Uiso 1 calc R . . H32B H 0.6934 0.0571 -0.0845 0.023 Uiso 1 calc R . . N33 N 0.72569(6) 0.11832(10) 0.00927(17) 0.0161(4) Uani 1 d . . . H33A H 0.7320 0.1404 -0.0553 0.019 Uiso 1 calc R . . H33B H 0.7465 0.1136 0.0528 0.019 Uiso 1 calc R . . C34 C 0.62583(6) 0.07592(11) 0.0953(3) 0.0197(5) Uani 1 d . . . H34A H 0.6105 0.1047 0.1433 0.024 Uiso 1 calc R . . H34B H 0.6158 0.0308 0.1001 0.024 Uiso 1 calc R . . C35 C 0.62399(7) 0.09983(13) -0.0264(2) 0.0214(6) Uani 1 d . . . H35A H 0.6334 0.0652 -0.0773 0.026 Uiso 1 calc R . . H35B H 0.5980 0.1093 -0.0470 0.026 Uiso 1 calc R . . N36 N 0.64665(6) 0.16005(10) -0.03899(17) 0.0171(4) Uani 1 d . . . H36A H 0.6314 0.1961 -0.0413 0.021 Uiso 1 calc R . . H36B H 0.6595 0.1582 -0.1057 0.021 Uiso 1 calc R . . C37 C 0.66588(7) 0.07170(13) 0.2610(2) 0.0197(5) Uani 1 d . . . H37A H 0.6620 0.0255 0.2840 0.024 Uiso 1 calc R . . H37B H 0.6458 0.0985 0.2940 0.024 Uiso 1 calc R . . C38 C 0.70276(8) 0.09543(13) 0.3050(2) 0.0200(6) Uani 1 d . . . H38A H 0.7019 0.0985 0.3879 0.024 Uiso 1 calc R . . H38B H 0.7224 0.0637 0.2843 0.024 Uiso 1 calc R . . N39 N 0.71147(6) 0.16071(10) 0.25686(17) 0.0167(4) Uani 1 d . . . H39A H 0.7366 0.1651 0.2486 0.020 Uiso 1 calc R . . H39B H 0.7033 0.1932 0.3046 0.020 Uiso 1 calc R . . O41 O 0.51936(5) 0.21542(8) 0.66629(15) 0.0198(4) Uani 1 d . . . C41 C 0.52055(7) 0.27845(12) 0.6555(2) 0.0155(5) Uani 1 d . . . C42 C 0.54854(7) 0.31801(12) 0.70706(19) 0.0158(5) Uani 1 d . . . C43 C 0.54686(7) 0.38488(12) 0.6915(2) 0.0166(5) Uani 1 d . . . H43 H 0.5658 0.4110 0.7239 0.020 Uiso 1 calc R . . C44 C 0.51844(7) 0.41775(12) 0.6297(2) 0.0150(5) Uani 1 d . . . C45 C 0.49125(6) 0.38044(11) 0.5811(2) 0.0155(5) Uani 1 d . . . H45 H 0.4720 0.4015 0.5404 0.019 Uiso 1 calc R . . C46 C 0.49128(6) 0.31091(11) 0.5906(3) 0.0149(4) Uani 1 d . . . N47 N 0.46545(6) 0.26912(10) 0.55095(17) 0.0162(4) Uani 1 d . . . C48 C 0.43493(7) 0.29257(11) 0.4871(2) 0.0154(5) Uani 1 d . . . C49 C 0.43940(8) 0.32311(12) 0.3822(2) 0.0173(5) Uani 1 d . . . H49 H 0.4635 0.3304 0.3530 0.021 Uiso 1 calc R . . C50 C 0.40864(8) 0.34262(13) 0.3213(2) 0.0188(6) Uani 1 d . . . H50 H 0.4117 0.3634 0.2505 0.023 Uiso 1 calc R . . C51 C 0.37343(8) 0.33208(12) 0.3630(2) 0.0195(5) Uani 1 d . . . H51 H 0.3525 0.3464 0.3217 0.023 Uiso 1 calc R . . C52 C 0.36884(7) 0.30048(12) 0.4654(2) 0.0193(5) Uani 1 d . . . H52 H 0.3446 0.2925 0.4932 0.023 Uiso 1 calc R . . C53 C 0.39930(7) 0.28057(13) 0.5272(2) 0.0191(5) Uani 1 d . . . H53 H 0.3959 0.2587 0.5970 0.023 Uiso 1 calc R . . C54 C 0.57822(7) 0.28434(13) 0.7803(2) 0.0170(5) Uani 1 d . . . C55 C 0.60161(8) 0.23877(15) 0.7062(2) 0.0275(6) Uani 1 d . . . H55A H 0.5857 0.2051 0.6726 0.041 Uiso 1 calc R . . H55B H 0.6207 0.2176 0.7521 0.041 Uiso 1 calc R . . H55C H 0.6134 0.2645 0.6465 0.041 Uiso 1 calc R . . C56 C 0.55908(8) 0.24598(14) 0.8750(2) 0.0229(6) Uani 1 d . . . H56A H 0.5429 0.2756 0.9173 0.034 Uiso 1 calc R . . H56B H 0.5778 0.2276 0.9255 0.034 Uiso 1 calc R . . H56C H 0.5443 0.2103 0.8426 0.034 Uiso 1 calc R . . C57 C 0.60381(8) 0.33453(15) 0.8362(3) 0.0287(7) Uani 1 d . . . H57A H 0.6160 0.3610 0.7783 0.043 Uiso 1 calc R . . H57B H 0.6225 0.3115 0.8808 0.043 Uiso 1 calc R . . H57C H 0.5893 0.3632 0.8853 0.043 Uiso 1 calc R . . C58 C 0.52020(7) 0.49274(12) 0.6209(2) 0.0173(5) Uani 1 d . . . C59 C 0.52153(8) 0.52274(14) 0.7398(2) 0.0277(6) Uani 1 d . . . H59A H 0.5210 0.5708 0.7344 0.042 Uiso 1 calc R . . H59B H 0.5443 0.5090 0.7775 0.042 Uiso 1 calc R . . H59C H 0.5001 0.5076 0.7831 0.042 Uiso 1 calc R . . C60 C 0.48624(8) 0.52138(13) 0.5620(2) 0.0242(6) Uani 1 d . . . H60A H 0.4885 0.5693 0.5584 0.036 Uiso 1 calc R . . H60B H 0.4639 0.5096 0.6041 0.036 Uiso 1 calc R . . H60C H 0.4846 0.5036 0.4857 0.036 Uiso 1 calc R . . C61 C 0.55503(8) 0.51305(14) 0.5559(3) 0.0310(7) Uani 1 d . . . H61A H 0.5539 0.4951 0.4795 0.046 Uiso 1 calc R . . H61B H 0.5770 0.4959 0.5942 0.046 Uiso 1 calc R . . H61C H 0.5564 0.5611 0.5523 0.046 Uiso 1 calc R . . N70 N 0.49278(6) 0.07781(10) 0.62882(18) 0.0197(5) Uani 1 d . . . C71 C 0.49125(8) 0.07505(13) 0.7535(2) 0.0241(6) Uani 1 d . . . H71A H 0.5123 0.1000 0.7852 0.029 Uiso 1 calc R . . H71B H 0.4935 0.0289 0.7785 0.029 Uiso 1 calc R . . C72 C 0.45541(8) 0.10357(14) 0.7967(2) 0.0266(6) Uani 1 d . . . H72A H 0.4347 0.0739 0.7774 0.032 Uiso 1 calc R . . H72B H 0.4565 0.1076 0.8795 0.032 Uiso 1 calc R . . N73 N 0.44889(6) 0.16883(11) 0.74648(18) 0.0225(5) Uani 1 d . . . H73A H 0.4581 0.2010 0.7929 0.027 Uiso 1 calc R . . H73B H 0.4239 0.1757 0.7378 0.027 Uiso 1 calc R . . C74 C 0.53140(7) 0.07191(13) 0.5876(3) 0.0288(6) Uani 1 d . . . H74A H 0.5393 0.0255 0.5923 0.035 Uiso 1 calc R . . H74B H 0.5480 0.0982 0.6362 0.035 Uiso 1 calc R . . C75 C 0.53474(8) 0.09545(15) 0.4675(2) 0.0302(7) Uani 1 d . . . H75A H 0.5612 0.1017 0.4485 0.036 Uiso 1 calc R . . H75B H 0.5245 0.0618 0.4162 0.036 Uiso 1 calc R . . N76 N 0.51469(6) 0.15799(11) 0.45173(19) 0.0227(5) Uani 1 d . . . H76A H 0.5023 0.1572 0.3843 0.027 Uiso 1 calc R . . H76B H 0.5313 0.1922 0.4499 0.027 Uiso 1 calc R . . C77 C 0.46698(8) 0.02931(12) 0.5761(2) 0.0250(6) Uani 1 d . . . H77A H 0.4484 0.0153 0.6323 0.030 Uiso 1 calc R . . H77B H 0.4811 -0.0100 0.5527 0.030 Uiso 1 calc R . . C78 C 0.44706(8) 0.05812(13) 0.4737(2) 0.0232(6) Uani 1 d . . . H78A H 0.4642 0.0596 0.4089 0.028 Uiso 1 calc R . . H78B H 0.4259 0.0297 0.4532 0.028 Uiso 1 calc R . . N79 N 0.43369(6) 0.12501(10) 0.49871(18) 0.0204(5) Uani 1 d . . . H79A H 0.4126 0.1232 0.5417 0.024 Uiso 1 calc R . . H79B H 0.4284 0.1470 0.4332 0.024 Uiso 1 calc R . . O81 O 0.30279(5) 0.24445(8) 0.17062(15) 0.0169(4) Uani 1 d . . . C81 C 0.30504(7) 0.30669(12) 0.1499(2) 0.0137(5) Uani 1 d . . . C82 C 0.28017(7) 0.35432(12) 0.1955(2) 0.0147(5) Uani 1 d . . . C83 C 0.28561(7) 0.41936(12) 0.1673(2) 0.0156(5) Uani 1 d . . . H83 H 0.2688 0.4508 0.1970 0.019 Uiso 1 calc R . . C84 C 0.31472(6) 0.44268(10) 0.0965(2) 0.0137(4) Uani 1 d . . . C85 C 0.33961(7) 0.39804(12) 0.05670(19) 0.0139(5) Uani 1 d . . . H85 H 0.3598 0.4128 0.0124 0.017 Uiso 1 calc R . . C86 C 0.33599(6) 0.32959(10) 0.0801(2) 0.0132(4) Uani 1 d . . . N87 N 0.35930(6) 0.28184(10) 0.04698(17) 0.0154(4) Uani 1 d . . . C88 C 0.39187(7) 0.29762(11) -0.0147(2) 0.0141(5) Uani 1 d . . . C89 C 0.39086(8) 0.32713(12) -0.1210(2) 0.0175(5) Uani 1 d . . . H89 H 0.3678 0.3374 -0.1550 0.021 Uiso 1 calc R . . C90 C 0.42379(8) 0.34131(13) -0.1767(2) 0.0197(6) Uani 1 d . . . H90 H 0.4231 0.3613 -0.2487 0.024 Uiso 1 calc R . . C91 C 0.45763(8) 0.32649(13) -0.1280(2) 0.0202(5) Uani 1 d . . . H91 H 0.4800 0.3376 -0.1653 0.024 Uiso 1 calc R . . C92 C 0.45851(7) 0.29533(13) -0.0245(2) 0.0206(5) Uani 1 d . . . H92 H 0.4816 0.2841 0.0082 0.025 Uiso 1 calc R . . C93 C 0.42591(7) 0.28045(12) 0.0317(2) 0.0180(5) Uani 1 d . . . H93 H 0.4268 0.2585 0.1020 0.022 Uiso 1 calc R . . C94 C 0.24897(7) 0.33330(12) 0.2749(2) 0.0167(5) Uani 1 d . . . C95 C 0.26645(8) 0.30227(14) 0.3814(2) 0.0226(6) Uani 1 d . . . H95A H 0.2472 0.2952 0.4380 0.034 Uiso 1 calc R . . H95B H 0.2853 0.3319 0.4116 0.034 Uiso 1 calc R . . H95C H 0.2778 0.2601 0.3618 0.034 Uiso 1 calc R . . C96 C 0.22293(7) 0.28466(15) 0.2166(2) 0.0236(6) Uani 1 d . . . H96A H 0.2135 0.3042 0.1470 0.035 Uiso 1 calc R . . H96B H 0.2022 0.2744 0.2665 0.035 Uiso 1 calc R . . H96C H 0.2365 0.2442 0.1989 0.035 Uiso 1 calc R . . C97 C 0.22595(8) 0.39198(14) 0.3151(3) 0.0305(7) Uani 1 d . . . H97A H 0.2144 0.4134 0.2503 0.046 Uiso 1 calc R . . H97B H 0.2420 0.4234 0.3539 0.046 Uiso 1 calc R . . H97C H 0.2067 0.3767 0.3667 0.046 Uiso 1 calc R . . C98 C 0.31654(7) 0.51671(11) 0.0710(2) 0.0149(5) Uani 1 d . . . C99 C 0.33123(10) 0.55253(15) 0.1744(3) 0.0383(8) Uani 1 d . . . H99A H 0.3562 0.5367 0.1918 0.058 Uiso 1 calc R . . H99B H 0.3149 0.5440 0.2385 0.058 Uiso 1 calc R . . H99C H 0.3320 0.5998 0.1595 0.058 Uiso 1 calc R . . C100 C 0.27783(8) 0.54312(13) 0.0427(3) 0.0254(6) Uani 1 d . . . H10A H 0.2614 0.5369 0.1073 0.038 Uiso 1 calc R . . H10B H 0.2679 0.5193 -0.0221 0.038 Uiso 1 calc R . . H10C H 0.2795 0.5900 0.0247 0.038 Uiso 1 calc R . . C101 C 0.34154(8) 0.53152(14) -0.0297(3) 0.0302(7) Uani 1 d . . . H10D H 0.3426 0.5791 -0.0419 0.045 Uiso 1 calc R . . H10E H 0.3315 0.5101 -0.0969 0.045 Uiso 1 calc R . . H10F H 0.3665 0.5148 -0.0148 0.045 Uiso 1 calc R . . N110 N 0.32038(6) 0.09720(10) 0.13245(18) 0.0198(5) Uani 1 d . . . C111 C 0.34250(9) 0.04575(13) 0.0772(3) 0.0326(7) Uani 1 d . . . H11A H 0.3256 0.0107 0.0507 0.039 Uiso 1 calc R . . H11B H 0.3594 0.0261 0.1333 0.039 Uiso 1 calc R . . C112 C 0.36506(9) 0.06967(14) -0.0209(3) 0.0335(7) Uani 1 d . . . H11C H 0.3851 0.0378 -0.0362 0.040 Uiso 1 calc R . . H11D H 0.3491 0.0719 -0.0883 0.040 Uiso 1 calc R . . N113 N 0.38134(6) 0.13450(10) -0.00046(18) 0.0204(5) Uani 1 d . . . H11E H 0.3868 0.1548 -0.0675 0.024 Uiso 1 calc R . . H11F H 0.4028 0.1305 0.0404 0.024 Uiso 1 calc R . . C114 C 0.28110(7) 0.09889(12) 0.0973(3) 0.0255(5) Uani 1 d . . . H11G H 0.2671 0.1292 0.1465 0.031 Uiso 1 calc R . . H11H H 0.2702 0.0545 0.1048 0.031 Uiso 1 calc R . . C115 C 0.27817(9) 0.12175(15) -0.0244(3) 0.0341(7) Uani 1 d . . . H11I H 0.2860 0.0859 -0.0753 0.041 Uiso 1 calc R . . H11J H 0.2522 0.1329 -0.0419 0.041 Uiso 1 calc R . . N116 N 0.30191(7) 0.17998(10) -0.04247(18) 0.0220(5) Uani 1 d . . . H11K H 0.2874 0.2171 -0.0447 0.026 Uiso 1 calc R . . H11L H 0.3138 0.1762 -0.1105 0.026 Uiso 1 calc R . . C117 C 0.32280(9) 0.09332(15) 0.2571(2) 0.0315(7) Uani 1 d . . . H11M H 0.3190 0.0472 0.2809 0.038 Uiso 1 calc R . . H11N H 0.3028 0.1201 0.2905 0.038 Uiso 1 calc R . . C118 C 0.35919(10) 0.11696(15) 0.3006(2) 0.0352(8) Uani 1 d . . . H11O H 0.3577 0.1229 0.3830 0.042 Uiso 1 calc R . . H11P H 0.3785 0.0837 0.2849 0.042 Uiso 1 calc R . . N119 N 0.36947(6) 0.17918(10) 0.24784(18) 0.0204(5) Uani 1 d . . . H11Q H 0.3947 0.1805 0.2376 0.025 Uiso 1 calc R . . H11R H 0.3629 0.2134 0.2941 0.025 Uiso 1 calc R . . B1 B 0.34650(10) 0.13417(16) 0.6818(3) 0.0256(7) Uani 1 d . . . F11 F 0.36147(5) 0.18302(8) 0.75116(14) 0.0284(4) Uani 1 d . . . F12 F 0.31537(5) 0.10773(8) 0.73131(14) 0.0328(4) Uani 1 d . . . F13 F 0.33857(6) 0.15893(10) 0.57744(17) 0.0557(5) Uani 1 d . . . F14 F 0.37345(5) 0.08462(9) 0.67010(19) 0.0474(5) Uani 1 d . . . B2 B 0.46752(10) 0.12258(16) 0.1791(3) 0.0274(7) Uani 1 d . . . F21 F 0.45752(5) 0.17470(8) 0.24854(14) 0.0322(4) Uani 1 d . . . F22 F 0.49811(5) 0.09074(8) 0.22286(13) 0.0312(4) Uani 1 d . . . F23 F 0.43814(6) 0.07919(11) 0.1731(2) 0.0684(7) Uani 1 d . . . F24 F 0.47490(7) 0.14497(11) 0.07213(16) 0.0661(7) Uani 1 d . . . B3 B 0.68963(9) 0.11294(15) 0.6863(3) 0.0218(6) Uani 1 d . . . F31 F 0.70237(4) 0.16345(8) 0.75723(13) 0.0265(4) Uani 1 d . . . F32 F 0.65803(4) 0.08560(8) 0.73277(13) 0.0252(3) Uani 1 d . . . F33 F 0.68291(5) 0.13699(8) 0.57998(15) 0.0393(4) Uani 1 d . . . F34 F 0.71756(5) 0.06514(8) 0.68010(16) 0.0344(4) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01315(14) 0.01017(12) 0.01406(15) 0.00088(14) 0.00116(14) -0.00027(11) Ni2 0.01913(16) 0.01312(13) 0.01773(15) 0.00184(16) -0.00573(17) -0.00252(11) Ni3 0.01842(15) 0.01083(12) 0.01607(14) 0.00055(16) 0.00202(17) 0.00040(11) O1 0.0182(9) 0.0130(8) 0.0161(8) 0.0027(7) 0.0044(7) 0.0000(7) C1 0.0119(12) 0.0142(11) 0.0113(11) 0.0021(9) -0.0015(9) -0.0022(9) C2 0.0114(12) 0.0170(12) 0.0164(12) 0.0018(9) -0.0004(9) 0.0002(9) C3 0.0129(13) 0.0171(12) 0.0175(12) 0.0000(9) 0.0022(10) 0.0024(10) C4 0.0169(11) 0.0137(9) 0.0152(11) -0.0002(12) -0.0014(11) -0.0007(8) C5 0.0127(12) 0.0136(11) 0.0118(12) 0.0021(8) 0.0003(8) -0.0022(9) C6 0.0127(11) 0.0125(9) 0.0116(10) 0.0011(11) 0.0009(12) -0.0014(8) N7 0.0111(10) 0.0149(10) 0.0137(10) -0.0004(7) 0.0022(7) 0.0001(8) C8 0.0142(13) 0.0074(10) 0.0165(11) -0.0015(9) 0.0018(10) -0.0019(9) C9 0.0196(14) 0.0142(12) 0.0177(13) -0.0011(9) 0.0017(10) 0.0012(10) C10 0.0292(18) 0.0150(12) 0.0153(13) -0.0013(10) 0.0067(11) -0.0049(11) C11 0.0202(15) 0.0186(13) 0.0213(13) -0.0062(10) 0.0086(11) -0.0061(11) C12 0.0124(13) 0.0157(12) 0.0240(13) -0.0050(10) 0.0042(10) -0.0007(10) C13 0.0142(13) 0.0128(11) 0.0173(12) -0.0022(9) 0.0017(9) 0.0013(9) C14 0.0121(13) 0.0210(13) 0.0178(12) 0.0036(10) 0.0048(10) 0.0009(10) C15 0.0187(15) 0.0417(17) 0.0189(14) 0.0053(12) 0.0012(11) -0.0103(12) C16 0.0226(16) 0.0332(17) 0.0357(17) 0.0086(13) 0.0158(13) 0.0091(13) C17 0.0178(14) 0.0309(15) 0.0160(12) 0.0055(11) 0.0027(10) -0.0017(12) C18 0.0136(12) 0.0151(11) 0.0217(14) 0.0025(9) 0.0023(10) 0.0025(9) C19 0.0219(15) 0.0155(13) 0.0326(15) 0.0049(11) 0.0050(12) -0.0003(11) C20 0.0345(17) 0.0196(14) 0.0296(15) -0.0010(11) 0.0108(13) 0.0033(12) C21 0.0194(14) 0.0215(13) 0.0321(15) 0.0080(12) -0.0034(12) 0.0004(11) N30 0.0151(12) 0.0137(10) 0.0161(10) 0.0004(8) -0.0004(8) -0.0006(8) C31 0.0237(13) 0.0111(10) 0.0215(13) -0.0006(11) -0.0031(13) 0.0003(9) C32 0.0215(14) 0.0154(12) 0.0199(13) -0.0025(10) 0.0011(11) 0.0030(10) N33 0.0178(12) 0.0144(10) 0.0161(10) 0.0004(8) 0.0022(8) 0.0005(8) C34 0.0148(12) 0.0190(11) 0.0254(13) 0.0060(13) -0.0033(13) -0.0048(9) C35 0.0172(14) 0.0220(13) 0.0250(14) -0.0015(11) -0.0074(11) -0.0024(10) N36 0.0175(11) 0.0176(11) 0.0162(10) 0.0023(8) 0.0006(9) 0.0015(9) C37 0.0256(15) 0.0158(12) 0.0176(12) 0.0054(10) 0.0026(11) -0.0021(10) C38 0.0222(15) 0.0230(14) 0.0146(12) 0.0024(10) 0.0013(10) 0.0016(11) N39 0.0161(11) 0.0167(11) 0.0172(10) 0.0003(8) 0.0009(9) 0.0000(8) O41 0.0227(10) 0.0135(9) 0.0233(9) 0.0007(7) -0.0081(8) -0.0001(7) C41 0.0161(13) 0.0162(12) 0.0141(12) 0.0009(9) -0.0008(10) 0.0003(10) C42 0.0141(13) 0.0203(13) 0.0129(11) 0.0024(9) -0.0014(9) 0.0003(10) C43 0.0120(13) 0.0199(13) 0.0177(12) -0.0016(10) -0.0023(10) -0.0025(10) C44 0.0159(13) 0.0142(11) 0.0149(12) 0.0010(9) 0.0016(9) -0.0007(10) C45 0.0139(12) 0.0186(11) 0.0141(12) -0.0002(11) -0.0011(11) 0.0022(8) C46 0.0131(11) 0.0175(10) 0.0139(10) 0.0025(12) -0.0016(12) -0.0026(8) N47 0.0169(11) 0.0125(10) 0.0190(10) 0.0017(8) -0.0067(8) -0.0022(8) C48 0.0163(13) 0.0135(11) 0.0165(12) -0.0016(9) -0.0063(10) -0.0019(9) C49 0.0165(14) 0.0166(13) 0.0188(13) 0.0018(10) -0.0006(10) -0.0013(10) C50 0.0236(15) 0.0146(13) 0.0182(13) 0.0003(10) -0.0052(11) 0.0020(11) C51 0.0202(15) 0.0163(12) 0.0219(13) -0.0033(10) -0.0089(11) 0.0028(10) C52 0.0151(13) 0.0186(13) 0.0243(13) -0.0036(10) -0.0016(11) 0.0009(10) C53 0.0208(15) 0.0187(13) 0.0178(13) 0.0014(10) -0.0014(10) 0.0002(11) C54 0.0142(13) 0.0188(13) 0.0179(12) 0.0033(10) -0.0040(10) -0.0006(10) C55 0.0208(15) 0.0398(17) 0.0217(14) 0.0021(12) -0.0016(11) 0.0117(13) C56 0.0164(15) 0.0311(15) 0.0211(13) 0.0073(11) -0.0026(11) -0.0014(12) C57 0.0202(15) 0.0298(16) 0.0360(16) 0.0077(13) -0.0121(13) -0.0059(13) C58 0.0160(13) 0.0145(12) 0.0215(14) -0.0018(9) -0.0004(10) -0.0010(10) C59 0.0301(17) 0.0256(15) 0.0275(15) -0.0073(12) -0.0116(13) 0.0047(12) C60 0.0291(16) 0.0176(13) 0.0258(15) 0.0000(10) -0.0065(11) 0.0035(11) C61 0.0266(16) 0.0187(13) 0.0476(19) 0.0092(12) 0.0061(13) -0.0032(11) N70 0.0214(13) 0.0159(11) 0.0218(12) 0.0031(8) -0.0034(9) -0.0005(9) C71 0.0362(17) 0.0164(13) 0.0198(13) 0.0045(10) -0.0095(12) -0.0016(11) C72 0.0350(18) 0.0269(15) 0.0178(13) 0.0044(11) -0.0012(12) -0.0029(13) N73 0.0257(13) 0.0201(11) 0.0218(11) -0.0011(9) -0.0062(10) -0.0018(10) C74 0.0290(15) 0.0256(13) 0.0317(15) 0.0018(15) 0.0014(16) 0.0042(11) C75 0.0280(17) 0.0319(17) 0.0307(16) -0.0027(13) 0.0051(13) 0.0001(13) N76 0.0245(14) 0.0234(12) 0.0201(12) 0.0017(9) -0.0027(10) -0.0078(9) C77 0.0359(16) 0.0160(11) 0.0233(15) 0.0024(11) -0.0041(13) -0.0052(10) C78 0.0309(16) 0.0188(13) 0.0199(13) -0.0010(10) -0.0044(12) -0.0083(11) N79 0.0222(13) 0.0191(11) 0.0198(11) 0.0007(9) -0.0032(9) -0.0020(9) O81 0.0185(9) 0.0108(8) 0.0213(9) 0.0001(7) 0.0033(7) -0.0005(7) C81 0.0133(13) 0.0148(11) 0.0128(11) 0.0005(9) -0.0022(9) -0.0003(9) C82 0.0123(12) 0.0181(12) 0.0136(11) 0.0015(9) -0.0002(9) -0.0007(9) C83 0.0141(13) 0.0157(12) 0.0171(12) -0.0009(9) 0.0008(10) 0.0018(9) C84 0.0136(11) 0.0145(10) 0.0131(10) 0.0013(11) -0.0009(11) -0.0023(8) C85 0.0124(12) 0.0147(11) 0.0146(12) 0.0012(8) -0.0007(9) -0.0037(9) C86 0.0134(11) 0.0137(10) 0.0124(11) 0.0014(10) -0.0002(10) -0.0008(8) N87 0.0135(11) 0.0154(10) 0.0173(10) 0.0006(8) 0.0042(8) 0.0003(8) C88 0.0153(13) 0.0104(11) 0.0166(12) -0.0003(9) 0.0033(10) 0.0002(9) C89 0.0170(14) 0.0184(13) 0.0171(12) 0.0024(10) 0.0002(10) 0.0041(10) C90 0.0227(16) 0.0197(14) 0.0167(14) 0.0031(10) 0.0027(11) 0.0020(11) C91 0.0178(14) 0.0187(13) 0.0241(13) -0.0026(11) 0.0074(11) -0.0035(11) C92 0.0163(14) 0.0210(13) 0.0246(14) -0.0007(10) 0.0011(11) 0.0012(10) C93 0.0202(14) 0.0163(12) 0.0174(12) 0.0005(9) 0.0032(10) 0.0031(10) C94 0.0147(13) 0.0185(13) 0.0169(12) 0.0033(10) 0.0041(10) 0.0006(10) C95 0.0250(16) 0.0264(14) 0.0164(13) 0.0043(11) 0.0015(11) -0.0070(12) C96 0.0159(14) 0.0359(16) 0.0188(13) 0.0036(11) 0.0008(10) -0.0072(12) C97 0.0258(17) 0.0273(16) 0.0385(17) 0.0049(13) 0.0193(14) 0.0053(13) C98 0.0140(12) 0.0125(11) 0.0183(13) 0.0017(9) -0.0007(10) -0.0002(9) C99 0.058(2) 0.0206(15) 0.0367(18) -0.0002(13) -0.0163(16) -0.0065(15) C100 0.0193(15) 0.0171(13) 0.0400(16) 0.0057(11) 0.0016(12) 0.0036(11) C101 0.0268(16) 0.0222(15) 0.0418(18) 0.0161(13) 0.0102(14) 0.0048(12) N110 0.0210(13) 0.0163(11) 0.0219(11) 0.0022(8) 0.0004(9) -0.0011(9) C111 0.0384(17) 0.0184(12) 0.0410(18) -0.0042(14) 0.0125(16) -0.0010(11) C112 0.051(2) 0.0178(14) 0.0317(17) -0.0050(12) 0.0154(15) -0.0018(13) N113 0.0254(13) 0.0158(11) 0.0199(11) 0.0004(8) 0.0026(9) 0.0011(9) C114 0.0241(14) 0.0224(12) 0.0300(14) 0.0035(14) -0.0005(15) -0.0060(10) C115 0.0305(18) 0.0370(18) 0.0347(17) 0.0081(14) -0.0123(14) -0.0068(14) N116 0.0290(13) 0.0178(11) 0.0190(11) 0.0018(8) 0.0001(10) 0.0032(9) C117 0.0393(19) 0.0311(17) 0.0243(15) 0.0115(12) -0.0017(13) -0.0079(14) C118 0.053(2) 0.0294(17) 0.0227(15) 0.0054(12) -0.0055(14) -0.0105(15) N119 0.0220(12) 0.0180(11) 0.0212(11) -0.0008(9) 0.0009(9) 0.0002(9) B1 0.0303(19) 0.0246(16) 0.0218(16) -0.0061(12) 0.0052(13) -0.0084(14) F11 0.0333(10) 0.0228(9) 0.0292(9) -0.0066(7) 0.0003(7) -0.0068(7) F12 0.0299(10) 0.0333(10) 0.0352(10) -0.0107(7) 0.0077(8) -0.0080(8) F13 0.0902(16) 0.0539(12) 0.0231(10) 0.0022(10) -0.0065(11) -0.0196(11) F14 0.0307(11) 0.0326(10) 0.0789(15) -0.0243(10) 0.0118(10) -0.0036(8) B2 0.0314(19) 0.0223(16) 0.0283(17) -0.0038(13) -0.0076(14) 0.0074(14) F21 0.0400(11) 0.0277(9) 0.0290(9) -0.0075(7) -0.0054(8) 0.0144(8) F22 0.0340(10) 0.0316(9) 0.0280(9) -0.0010(7) -0.0026(8) 0.0131(8) F23 0.0357(12) 0.0390(12) 0.130(2) -0.0235(13) -0.0168(13) 0.0019(10) F24 0.1127(19) 0.0628(14) 0.0228(11) 0.0048(10) 0.0011(12) 0.0448(13) B3 0.0237(18) 0.0193(15) 0.0224(15) -0.0036(12) 0.0035(13) -0.0034(12) F31 0.0280(9) 0.0261(9) 0.0254(8) -0.0073(7) 0.0023(7) -0.0069(7) F32 0.0220(8) 0.0275(9) 0.0259(8) -0.0034(7) 0.0043(7) -0.0051(7) F33 0.0558(11) 0.0415(10) 0.0207(9) 0.0032(8) -0.0006(9) -0.0126(8) F34 0.0250(10) 0.0277(9) 0.0503(11) -0.0101(8) 0.0053(8) 0.0005(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N7 2.033(2) . ? Ni1 O1 2.0531(17) . ? Ni1 N33 2.096(2) . ? Ni1 N30 2.106(2) . ? Ni1 N39 2.133(2) . ? Ni1 N36 2.149(2) . ? Ni2 O41 2.0296(18) . ? Ni2 N47 2.033(2) . ? Ni2 N79 2.092(2) . ? Ni2 N70 2.098(2) . ? Ni2 N73 2.143(2) . ? Ni2 N76 2.154(2) . ? Ni3 N87 2.037(2) . ? Ni3 O81 2.0562(17) . ? Ni3 N113 2.096(2) . ? Ni3 N110 2.109(2) . ? Ni3 N119 2.137(2) . ? Ni3 N116 2.155(2) . ? O1 C1 1.294(3) . ? C1 C2 1.435(3) . ? C1 C6 1.465(3) . ? C2 C3 1.374(3) . ? C2 C14 1.539(3) . ? C3 C4 1.427(3) . ? C4 C5 1.370(3) . ? C4 C18 1.537(3) . ? C5 C6 1.430(3) . ? C6 N7 1.348(3) . ? N7 C8 1.421(3) . ? C8 C13 1.390(3) . ? C8 C9 1.407(3) . ? C9 C10 1.390(4) . ? C10 C11 1.393(4) . ? C11 C12 1.393(4) . ? C12 C13 1.393(3) . ? C14 C15 1.531(4) . ? C14 C16 1.538(4) . ? C14 C17 1.547(3) . ? C18 C19 1.532(3) . ? C18 C20 1.542(4) . ? C18 C21 1.545(4) . ? N30 C34 1.480(3) . ? N30 C37 1.490(3) . ? N30 C31 1.492(3) . ? C31 C32 1.535(4) . ? C32 N33 1.483(3) . ? C34 C35 1.530(4) . ? C35 N36 1.482(3) . ? C37 C38 1.512(4) . ? C38 N39 1.482(3) . ? O41 C41 1.291(3) . ? C41 C42 1.432(3) . ? C41 C46 1.468(3) . ? C42 C43 1.376(3) . ? C42 C54 1.544(3) . ? C43 C44 1.430(3) . ? C44 C45 1.371(3) . ? C44 C58 1.532(3) . ? C45 C46 1.420(3) . ? C46 N47 1.349(3) . ? N47 C48 1.423(3) . ? C48 C53 1.396(4) . ? C48 C49 1.405(3) . ? C49 C50 1.386(4) . ? C50 C51 1.383(4) . ? C51 C52 1.388(4) . ? C52 C53 1.385(3) . ? C54 C57 1.531(4) . ? C54 C55 1.535(4) . ? C54 C56 1.537(3) . ? C58 C60 1.530(4) . ? C58 C61 1.535(4) . ? C58 C59 1.543(4) . ? N70 C74 1.485(3) . ? N70 C71 1.486(3) . ? N70 C77 1.497(3) . ? C71 C72 1.510(4) . ? C72 N73 1.476(3) . ? C74 C75 1.514(4) . ? C75 N76 1.477(4) . ? C77 C78 1.533(4) . ? C78 N79 1.476(3) . ? O81 C81 1.294(3) . ? C81 C82 1.430(3) . ? C81 C86 1.470(3) . ? C82 C83 1.380(3) . ? C82 C94 1.533(3) . ? C83 C84 1.430(3) . ? C84 C85 1.364(3) . ? C84 C98 1.539(3) . ? C85 C86 1.428(3) . ? C86 N87 1.346(3) . ? N87 C88 1.425(3) . ? C88 C93 1.394(3) . ? C88 C89 1.402(3) . ? C89 C90 1.393(4) . ? C90 C91 1.387(4) . ? C91 C92 1.387(4) . ? C92 C93 1.389(4) . ? C94 C97 1.533(4) . ? C94 C96 1.533(4) . ? C94 C95 1.551(3) . ? C98 C99 1.527(4) . ? C98 C101 1.531(4) . ? C98 C100 1.537(3) . ? N110 C111 1.473(3) . ? N110 C114 1.481(3) . ? N110 C117 1.489(3) . ? C111 C112 1.505(4) . ? C112 N113 1.466(3) . ? C114 C115 1.525(4) . ? C115 N116 1.480(4) . ? C117 C118 1.494(4) . ? C118 N119 1.462(3) . ? B1 F13 1.371(4) . ? B1 F12 1.380(4) . ? B1 F11 1.402(3) . ? B1 F14 1.410(4) . ? B2 F24 1.378(4) . ? B2 F23 1.384(4) . ? B2 F22 1.384(4) . ? B2 F21 1.393(4) . ? B3 F33 1.379(4) . ? B3 F32 1.386(3) . ? B3 F34 1.405(4) . ? B3 F31 1.408(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Ni1 O1 80.08(7) . . ? N7 Ni1 N33 100.76(8) . . ? O1 Ni1 N33 176.31(8) . . ? N7 Ni1 N30 173.24(8) . . ? O1 Ni1 N30 94.86(7) . . ? N33 Ni1 N30 84.00(8) . . ? N7 Ni1 N39 101.23(8) . . ? O1 Ni1 N39 88.48(7) . . ? N33 Ni1 N39 94.85(8) . . ? N30 Ni1 N39 83.00(8) . . ? N7 Ni1 N36 93.90(8) . . ? O1 Ni1 N36 85.04(7) . . ? N33 Ni1 N36 91.31(8) . . ? N30 Ni1 N36 81.13(8) . . ? N39 Ni1 N36 162.27(8) . . ? O41 Ni2 N47 80.43(8) . . ? O41 Ni2 N79 175.88(8) . . ? N47 Ni2 N79 102.25(8) . . ? O41 Ni2 N70 93.05(8) . . ? N47 Ni2 N70 173.29(9) . . ? N79 Ni2 N70 84.17(9) . . ? O41 Ni2 N73 87.34(8) . . ? N47 Ni2 N73 98.07(8) . . ? N79 Ni2 N73 95.33(9) . . ? N70 Ni2 N73 83.12(8) . . ? O41 Ni2 N76 84.50(8) . . ? N47 Ni2 N76 95.98(9) . . ? N79 Ni2 N76 92.07(9) . . ? N70 Ni2 N76 81.71(9) . . ? N73 Ni2 N76 162.34(9) . . ? N87 Ni3 O81 80.01(7) . . ? N87 Ni3 N113 99.55(8) . . ? O81 Ni3 N113 177.32(8) . . ? N87 Ni3 N110 175.31(9) . . ? O81 Ni3 N110 96.15(8) . . ? N113 Ni3 N110 84.16(8) . . ? N87 Ni3 N119 99.99(8) . . ? O81 Ni3 N119 87.60(8) . . ? N113 Ni3 N119 95.07(9) . . ? N110 Ni3 N119 82.44(8) . . ? N87 Ni3 N116 96.23(8) . . ? O81 Ni3 N116 85.40(8) . . ? N113 Ni3 N116 92.04(9) . . ? N110 Ni3 N116 80.72(8) . . ? N119 Ni3 N116 160.93(8) . . ? C1 O1 Ni1 113.16(15) . . ? O1 C1 C2 123.4(2) . . ? O1 C1 C6 118.0(2) . . ? C2 C1 C6 118.6(2) . . ? C3 C2 C1 117.9(2) . . ? C3 C2 C14 122.3(2) . . ? C1 C2 C14 119.7(2) . . ? C2 C3 C4 124.7(2) . . ? C5 C4 C3 118.2(2) . . ? C5 C4 C18 122.9(2) . . ? C3 C4 C18 118.9(2) . . ? C4 C5 C6 121.0(2) . . ? N7 C6 C5 126.2(2) . . ? N7 C6 C1 114.3(2) . . ? C5 C6 C1 119.5(2) . . ? C6 N7 C8 121.1(2) . . ? C6 N7 Ni1 113.74(15) . . ? C8 N7 Ni1 124.71(15) . . ? C13 C8 C9 119.1(2) . . ? C13 C8 N7 118.1(2) . . ? C9 C8 N7 122.7(2) . . ? C10 C9 C8 119.8(3) . . ? C9 C10 C11 120.7(2) . . ? C10 C11 C12 119.5(2) . . ? C13 C12 C11 119.9(2) . . ? C8 C13 C12 120.9(2) . . ? C15 C14 C16 108.0(2) . . ? C15 C14 C2 110.0(2) . . ? C16 C14 C2 111.6(2) . . ? C15 C14 C17 110.7(2) . . ? C16 C14 C17 107.2(2) . . ? C2 C14 C17 109.3(2) . . ? C19 C18 C4 112.7(2) . . ? C19 C18 C20 107.7(2) . . ? C4 C18 C20 111.3(2) . . ? C19 C18 C21 108.1(2) . . ? C4 C18 C21 108.2(2) . . ? C20 C18 C21 108.7(2) . . ? C34 N30 C37 111.1(2) . . ? C34 N30 C31 113.4(2) . . ? C37 N30 C31 111.5(2) . . ? C34 N30 Ni1 105.65(14) . . ? C37 N30 Ni1 105.43(15) . . ? C31 N30 Ni1 109.20(15) . . ? N30 C31 C32 112.67(19) . . ? N33 C32 C31 109.99(19) . . ? C32 N33 Ni1 107.48(15) . . ? N30 C34 C35 110.5(2) . . ? N36 C35 C34 109.6(2) . . ? C35 N36 Ni1 111.32(15) . . ? N30 C37 C38 110.7(2) . . ? N39 C38 C37 109.9(2) . . ? C38 N39 Ni1 109.48(15) . . ? C41 O41 Ni2 113.61(16) . . ? O41 C41 C42 122.7(2) . . ? O41 C41 C46 118.4(2) . . ? C42 C41 C46 118.8(2) . . ? C43 C42 C41 117.9(2) . . ? C43 C42 C54 123.1(2) . . ? C41 C42 C54 118.9(2) . . ? C42 C43 C44 124.4(2) . . ? C45 C44 C43 118.2(2) . . ? C45 C44 C58 123.6(2) . . ? C43 C44 C58 118.2(2) . . ? C44 C45 C46 121.2(2) . . ? N47 C46 C45 126.9(2) . . ? N47 C46 C41 113.5(2) . . ? C45 C46 C41 119.4(2) . . ? C46 N47 C48 120.8(2) . . ? C46 N47 Ni2 113.91(16) . . ? C48 N47 Ni2 125.23(15) . . ? C53 C48 C49 119.2(2) . . ? C53 C48 N47 118.3(2) . . ? C49 C48 N47 122.3(2) . . ? C50 C49 C48 120.0(2) . . ? C51 C50 C49 120.4(2) . . ? C50 C51 C52 119.8(2) . . ? C53 C52 C51 120.5(2) . . ? C52 C53 C48 120.1(2) . . ? C57 C54 C55 108.7(2) . . ? C57 C54 C56 107.0(2) . . ? C55 C54 C56 111.3(2) . . ? C57 C54 C42 111.7(2) . . ? C55 C54 C42 109.1(2) . . ? C56 C54 C42 109.1(2) . . ? C60 C58 C44 112.2(2) . . ? C60 C58 C61 108.9(2) . . ? C44 C58 C61 109.7(2) . . ? C60 C58 C59 107.2(2) . . ? C44 C58 C59 109.5(2) . . ? C61 C58 C59 109.3(2) . . ? C74 N70 C71 111.2(2) . . ? C74 N70 C77 113.2(2) . . ? C71 N70 C77 111.8(2) . . ? C74 N70 Ni2 105.66(15) . . ? C71 N70 Ni2 105.33(16) . . ? C77 N70 Ni2 109.15(15) . . ? N70 C71 C72 110.9(2) . . ? N73 C72 C71 110.2(2) . . ? C72 N73 Ni2 108.95(17) . . ? N70 C74 C75 111.2(2) . . ? N76 C75 C74 110.7(2) . . ? C75 N76 Ni2 110.45(17) . . ? N70 C77 C78 112.0(2) . . ? N79 C78 C77 110.3(2) . . ? C78 N79 Ni2 107.17(16) . . ? C81 O81 Ni3 113.43(15) . . ? O81 C81 C82 123.6(2) . . ? O81 C81 C86 117.8(2) . . ? C82 C81 C86 118.6(2) . . ? C83 C82 C81 118.0(2) . . ? C83 C82 C94 121.5(2) . . ? C81 C82 C94 120.5(2) . . ? C82 C83 C84 124.5(2) . . ? C85 C84 C83 118.0(2) . . ? C85 C84 C98 123.8(2) . . ? C83 C84 C98 118.2(2) . . ? C84 C85 C86 121.5(2) . . ? N87 C86 C85 126.2(2) . . ? N87 C86 C81 114.4(2) . . ? C85 C86 C81 119.3(2) . . ? C86 N87 C88 120.4(2) . . ? C86 N87 Ni3 113.86(16) . . ? C88 N87 Ni3 125.72(15) . . ? C93 C88 C89 119.2(2) . . ? C93 C88 N87 118.0(2) . . ? C89 C88 N87 122.7(2) . . ? C90 C89 C88 119.8(2) . . ? C91 C90 C89 120.7(2) . . ? C92 C91 C90 119.4(2) . . ? C91 C92 C93 120.6(2) . . ? C92 C93 C88 120.3(2) . . ? C82 C94 C97 112.0(2) . . ? C82 C94 C96 110.7(2) . . ? C97 C94 C96 108.2(2) . . ? C82 C94 C95 108.5(2) . . ? C97 C94 C95 106.5(2) . . ? C96 C94 C95 110.9(2) . . ? C99 C98 C101 109.4(2) . . ? C99 C98 C100 109.1(2) . . ? C101 C98 C100 107.3(2) . . ? C99 C98 C84 108.9(2) . . ? C101 C98 C84 111.9(2) . . ? C100 C98 C84 110.30(19) . . ? C111 N110 C114 114.3(2) . . ? C111 N110 C117 112.1(2) . . ? C114 N110 C117 109.8(2) . . ? C111 N110 Ni3 108.78(16) . . ? C114 N110 Ni3 105.80(15) . . ? C117 N110 Ni3 105.53(16) . . ? N110 C111 C112 114.2(2) . . ? N113 C112 C111 112.4(2) . . ? C112 N113 Ni3 107.34(17) . . ? N110 C114 C115 110.0(2) . . ? N116 C115 C114 110.0(2) . . ? C115 N116 Ni3 111.20(16) . . ? N110 C117 C118 112.4(2) . . ? N119 C118 C117 110.8(2) . . ? C118 N119 Ni3 110.47(17) . . ? F13 B1 F12 111.1(3) . . ? F13 B1 F11 110.7(2) . . ? F12 B1 F11 109.9(2) . . ? F13 B1 F14 108.6(3) . . ? F12 B1 F14 109.1(2) . . ? F11 B1 F14 107.4(3) . . ? F24 B2 F23 108.2(3) . . ? F24 B2 F22 110.4(3) . . ? F23 B2 F22 109.5(3) . . ? F24 B2 F21 110.3(3) . . ? F23 B2 F21 108.5(3) . . ? F22 B2 F21 109.9(2) . . ? F33 B3 F32 111.3(2) . . ? F33 B3 F34 108.9(2) . . ? F32 B3 F34 109.6(2) . . ? F33 B3 F31 110.4(2) . . ? F32 B3 F31 108.9(2) . . ? F34 B3 F31 107.6(2) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.549 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.064 #===END data_3 _database_code_CSD 197835 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical '[C26 H43 N5 O1 Co]2+, 2 (Cl O4)-, 0.5 CH3OH, 0.5 H2O' _chemical_formula_sum 'C26.50 H46 Cl2 Co N5 O10' _chemical_formula_weight 724.51 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 17.3793(6) _cell_length_b 20.9029(6) _cell_length_c 19.9702(6) _cell_angle_alpha 90.00 _cell_angle_beta 113.35(1) _cell_angle_gamma 90.00 _cell_volume 6660.6(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 220910 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'opaque block' _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_method ? _exptl_crystal_F_000 3048 _exptl_absorpt_coefficient_mu 0.735 _exptl_absorpt_correction_type 'Not corrected' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius Kappa-CCD' _diffrn_measurement_method '588 images at 1 deg. in \w and 20 sec.' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58169 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11691 _reflns_number_observed 10807 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'DENZO, Nonius Collect Software' _computing_cell_refinement 'DENZO, Nonius Collect Software' _computing_data_reduction 'DENZO, Nonius Collect Software' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 16 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+31.8361P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11675 _refine_ls_number_parameters 821 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0741 _refine_ls_R_factor_obs 0.0686 _refine_ls_wR_factor_all 0.1479 _refine_ls_wR_factor_obs 0.1417 _refine_ls_goodness_of_fit_all 1.175 _refine_ls_goodness_of_fit_obs 1.206 _refine_ls_restrained_S_all 1.207 _refine_ls_restrained_S_obs 1.206 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.22704(3) 0.03702(3) 0.95887(3) 0.01842(13) Uani 1 d . . O1 O 0.2331(2) 0.12672(13) 0.96910(15) 0.0216(6) Uani 1 d . . C1 C 0.2846(2) 0.1450(2) 1.0351(2) 0.0208(9) Uani 1 d . . C2 C 0.3069(2) 0.2099(2) 1.0533(2) 0.0208(9) Uani 1 d . . C3 C 0.3626(3) 0.2217(2) 1.1236(2) 0.0245(9) Uani 1 d . . H3 H 0.3796(3) 0.2647(2) 1.1367(2) 0.029 Uiso 1 calc R . C4 C 0.3966(3) 0.1736(2) 1.1783(2) 0.0228(9) Uani 1 d . . C5 C 0.3737(3) 0.1112(2) 1.1609(2) 0.0223(9) Uani 1 d . . H5 H 0.3948(3) 0.0787(2) 1.1968(2) 0.027 Uiso 1 calc R . C6 C 0.3180(2) 0.0954(2) 1.0886(2) 0.0196(8) Uani 1 d . . N7 N 0.2898(2) 0.0366(2) 1.0626(2) 0.0199(7) Uani 1 d . . C8 C 0.3177(3) -0.0202(2) 1.1049(2) 0.0211(9) Uani 1 d . . C9 C 0.4028(3) -0.0374(2) 1.1331(2) 0.0268(9) Uani 1 d . . H9 H 0.4433(3) -0.0097(2) 1.1278(2) 0.032 Uiso 1 calc R . C10 C 0.4270(3) -0.0956(2) 1.1690(2) 0.0330(11) Uani 1 d . . H10 H 0.4843(3) -0.1077(2) 1.1877(2) 0.040 Uiso 1 calc R . C11 C 0.3690(3) -0.1361(2) 1.1779(2) 0.0346(11) Uani 1 d . . H11 H 0.3864(3) -0.1755(2) 1.2031(2) 0.042 Uiso 1 calc R . C12 C 0.2850(3) -0.1188(2) 1.1498(2) 0.0322(11) Uani 1 d . . H12 H 0.2448(3) -0.1467(2) 1.1553(2) 0.039 Uiso 1 calc R . C13 C 0.2596(3) -0.0611(2) 1.1137(2) 0.0254(9) Uani 1 d . . H13 H 0.2021(3) -0.0494(2) 1.0948(2) 0.030 Uiso 1 calc R . C14 C 0.2698(3) 0.2628(2) 0.9965(2) 0.0267(10) Uani 1 d . . C15 C 0.1738(3) 0.2627(2) 0.9704(3) 0.0370(11) Uani 1 d . . H15A H 0.1501(3) 0.2973(11) 0.9351(14) 0.056 Uiso 1 calc R . H15B H 0.1587(3) 0.2691(17) 1.0123(4) 0.056 Uiso 1 calc R . H15C H 0.1516(4) 0.2216(7) 0.9473(17) 0.056 Uiso 1 calc R . C16 C 0.2948(3) 0.2523(2) 0.9316(3) 0.0344(11) Uani 1 d . . H16A H 0.3561(3) 0.2512(16) 0.9491(3) 0.052 Uiso 1 calc R . H16B H 0.2727(18) 0.2873(9) 0.8966(9) 0.052 Uiso 1 calc R . H16C H 0.2716(18) 0.2116(8) 0.9079(11) 0.052 Uiso 1 calc R . C17 C 0.3023(3) 0.3288(2) 1.0279(3) 0.0360(11) Uani 1 d . . H17A H 0.3632(4) 0.3304(6) 1.0429(17) 0.054 Uiso 1 calc R . H17B H 0.2886(19) 0.3369(7) 1.0703(12) 0.054 Uiso 1 calc R . H17C H 0.2758(17) 0.3616(3) 0.9908(7) 0.054 Uiso 1 calc R . C18 C 0.4586(3) 0.1945(2) 1.2547(2) 0.0266(10) Uani 1 d . . C19 C 0.4205(3) 0.2494(3) 1.2834(3) 0.0380(12) Uani 1 d . . H19A H 0.4107(20) 0.2865(6) 1.2511(11) 0.057 Uiso 1 calc R . H19B H 0.4594(10) 0.2611(11) 1.3327(8) 0.057 Uiso 1 calc R . H19C H 0.3673(11) 0.2353(6) 1.2845(18) 0.057 Uiso 1 calc R . C20 C 0.4799(3) 0.1391(2) 1.3091(2) 0.0383(12) Uani 1 d . . H20A H 0.4286(5) 0.1237(11) 1.3129(15) 0.057 Uiso 1 calc R . H20B H 0.5193(18) 0.1539(5) 1.3570(5) 0.057 Uiso 1 calc R . H20C H 0.5055(20) 0.1043(7) 1.2922(10) 0.057 Uiso 1 calc R . C21 C 0.5386(3) 0.2189(2) 1.2487(2) 0.0331(11) Uani 1 d . . H21A H 0.5635(11) 0.1845(5) 1.2305(17) 0.050 Uiso 1 calc R . H21B H 0.5786(9) 0.2326(15) 1.2968(4) 0.050 Uiso 1 calc R . H21C H 0.5251(4) 0.2551(10) 1.2149(14) 0.050 Uiso 1 calc R . N30 N 0.1666(2) 0.0436(2) 0.8526(2) 0.0235(8) Uani 1 d . . C31 C 0.0872(3) 0.0787(2) 0.8410(2) 0.0327(11) Uani 1 d . . H31A H 0.0474(3) 0.0749(2) 0.7894(2) 0.039 Uiso 1 calc R . H31B H 0.0992(3) 0.1247(2) 0.8525(2) 0.039 Uiso 1 calc R . C32 C 0.0494(3) 0.0501(3) 0.8901(2) 0.0366(12) Uani 1 d . . H32A H 0.0040(3) 0.0779(3) 0.8914(2) 0.044 Uiso 1 calc R . H32B H 0.0254(3) 0.0075(3) 0.8716(2) 0.044 Uiso 1 calc R . N33 N 0.1169(2) 0.0438(2) 0.9649(2) 0.0281(8) Uani 1 d . . H33A H 0.1074(2) 0.0080(2) 0.9873(2) 0.034 Uiso 1 calc R . H33B H 0.1162(2) 0.0790(2) 0.9924(2) 0.034 Uiso 1 calc R . C34 C 0.1478(3) -0.0221(2) 0.8191(2) 0.0265(10) Uani 1 d . . H34A H 0.1526(3) -0.0217(2) 0.7714(2) 0.032 Uiso 1 calc R . H34B H 0.0895(3) -0.0340(2) 0.8106(2) 0.032 Uiso 1 calc R . C35 C 0.2073(3) -0.0714(2) 0.8681(2) 0.0338(11) Uani 1 d . . H35A H 0.1829(3) -0.1147(2) 0.8553(2) 0.041 Uiso 1 calc R . H35B H 0.2611(3) -0.0704(2) 0.8620(2) 0.041 Uiso 1 calc R . N36 N 0.2213(2) -0.0557(2) 0.9448(2) 0.0244(8) Uani 1 d . . H36A H 0.2705(2) -0.0741(2) 0.9761(2) 0.029 Uiso 1 calc R . H36B H 0.1781(2) -0.0721(2) 0.9552(2) 0.029 Uiso 1 calc R . C37 C 0.2223(3) 0.0811(2) 0.8263(2) 0.0298(10) Uani 1 d . . H37A H 0.2212(3) 0.1269(2) 0.8386(2) 0.036 Uiso 1 calc R . H37B H 0.2024(3) 0.0772(2) 0.7726(2) 0.036 Uiso 1 calc R . C38 C 0.3107(3) 0.0552(2) 0.8625(2) 0.0312(10) Uani 1 d . . H38A H 0.3158(3) 0.0150(2) 0.8385(2) 0.037 Uiso 1 calc R . H38B H 0.3510(3) 0.0866(2) 0.8580(2) 0.037 Uiso 1 calc R . N39 N 0.3296(2) 0.0430(2) 0.9411(2) 0.0216(7) Uani 1 d . . H39A H 0.3625(2) 0.0757(2) 0.9688(2) 0.026 Uiso 1 calc R . H39B H 0.3594(2) 0.0055(2) 0.9552(2) 0.026 Uiso 1 calc R . Co2 Co 0.16705(4) 0.14084(3) 0.50447(3) 0.02524(15) Uani 1 d . . O41 O 0.1617(2) 0.13741(14) 0.4074(2) 0.0280(7) Uani 1 d . . C41 C 0.2083(3) 0.0915(2) 0.3985(2) 0.0280(10) Uani 1 d . . C42 C 0.2138(3) 0.0779(2) 0.3306(2) 0.0320(11) Uani 1 d . . C43 C 0.2662(3) 0.0287(3) 0.3311(3) 0.0378(12) Uani 1 d . . H43 H 0.2712(3) 0.0192(3) 0.2864(3) 0.045 Uiso 1 calc R . C44 C 0.3138(3) -0.0094(2) 0.3929(3) 0.0362(11) Uani 1 d . . C45 C 0.3069(3) 0.0026(2) 0.4576(3) 0.0340(11) Uani 1 d . . H45 H 0.3371(3) -0.0224(2) 0.4995(3) 0.041 Uiso 1 calc R . C46 C 0.2539(3) 0.0529(2) 0.4611(2) 0.0288(10) Uani 1 d . . N47 N 0.2403(3) 0.0692(2) 0.5207(2) 0.0312(9) Uani 1 d . . C48 C 0.2726(3) 0.0312(2) 0.5853(2) 0.0269(10) Uani 1 d . . C49 C 0.2282(4) -0.0200(3) 0.5933(3) 0.053(2) Uani 1 d . . H49 H 0.1764(4) -0.0309(3) 0.5550(3) 0.063 Uiso 1 calc R . C50 C 0.2579(4) -0.0564(3) 0.6567(3) 0.0484(14) Uani 1 d . . H50 H 0.2264(4) -0.0920(3) 0.6615(3) 0.058 Uiso 1 calc R . C51 C 0.3320(3) -0.0412(3) 0.7118(2) 0.0389(12) Uani 1 d . . H51 H 0.3532(3) -0.0663(3) 0.7550(2) 0.047 Uiso 1 calc R . C52 C 0.3749(4) 0.0104(4) 0.7041(3) 0.077(2) Uani 1 d . . H52 H 0.4262(4) 0.0217(4) 0.7429(3) 0.092 Uiso 1 calc R . C53 C 0.3463(3) 0.0467(3) 0.6417(3) 0.064(2) Uani 1 d . . H53 H 0.3777(3) 0.0827(3) 0.6377(3) 0.076 Uiso 1 calc R . C54 C 0.1628(3) 0.1154(3) 0.2614(2) 0.0374(12) Uani 1 d . . C55 C 0.0691(3) 0.1067(3) 0.2434(3) 0.0400(12) Uani 1 d . . H55A H 0.0552(5) 0.0610(3) 0.2376(19) 0.060 Uiso 1 calc R . H55B H 0.0363(3) 0.1292(15) 0.1979(11) 0.060 Uiso 1 calc R . H55C H 0.0559(5) 0.1242(16) 0.2831(9) 0.060 Uiso 1 calc R . C56 C 0.1854(4) 0.1867(3) 0.2719(3) 0.064(2) Uani 1 d . . H56A H 0.1743(28) 0.2032(6) 0.3131(17) 0.096 Uiso 1 calc R . H56B H 0.1514(22) 0.2102(5) 0.2275(10) 0.096 Uiso 1 calc R . H56C H 0.2449(8) 0.1921(4) 0.2818(26) 0.096 Uiso 1 calc R . C57 C 0.1788(4) 0.0914(4) 0.1953(3) 0.069(2) Uani 1 d . . H57A H 0.2379(8) 0.0977(22) 0.2043(12) 0.103 Uiso 1 calc R . H57B H 0.1436(24) 0.1154(17) 0.1518(6) 0.103 Uiso 1 calc R . H57C H 0.1650(30) 0.0458(7) 0.1878(17) 0.103 Uiso 1 calc R . C58 C 0.3684(4) -0.0635(3) 0.3845(3) 0.050(2) Uani 1 d . . C59 C 0.4282(4) -0.0378(3) 0.3499(3) 0.052(2) Uani 1 d . . H59A H 0.3951(4) -0.0207(18) 0.3012(10) 0.077 Uiso 1 calc R . H59B H 0.4639(18) -0.0727(5) 0.3460(21) 0.077 Uiso 1 calc R . H59C H 0.4634(18) -0.0037(14) 0.3807(12) 0.077 Uiso 1 calc R . C60 C 0.3114(6) -0.1150(3) 0.3340(4) 0.081(3) Uani 1 d . . H60A H 0.2769(27) -0.1343(20) 0.3573(14) 0.121 Uiso 1 calc R . H60B H 0.3460(6) -0.1482(14) 0.3250(25) 0.121 Uiso 1 calc R . H60C H 0.2751(25) -0.0954(6) 0.2876(13) 0.121 Uiso 1 calc R . C61 C 0.4229(5) -0.0942(3) 0.4575(4) 0.069(2) Uani 1 d . . H61A H 0.4611(22) -0.0621(7) 0.4893(11) 0.103 Uiso 1 calc R . H61B H 0.4556(24) -0.1292(16) 0.4491(5) 0.103 Uiso 1 calc R . H61C H 0.3870(5) -0.1111(21) 0.4808(13) 0.103 Uiso 1 calc R . N70 N 0.0896(3) 0.2125(2) 0.4848(3) 0.0457(11) Uani 1 d . . C71 C 0.0580(4) 0.2154(3) 0.5463(3) 0.0482(14) Uani 1 d . . H71A H 0.0364(4) 0.2588(3) 0.5489(3) 0.058 Uiso 1 calc R . H71B H 0.0118(4) 0.1844(3) 0.5368(3) 0.058 Uiso 1 calc R . C72 C 0.1273(3) 0.2001(2) 0.6148(3) 0.0413(12) Uani 1 d . . H72A H 0.1056(3) 0.1901(2) 0.6525(3) 0.050 Uiso 1 calc R . H72B H 0.1653(3) 0.2374(2) 0.6315(3) 0.050 Uiso 1 calc R . N73 N 0.1740(3) 0.1444(2) 0.6043(2) 0.0322(9) Uani 1 d . . H73A H 0.1523(3) 0.1074(2) 0.6147(2) 0.039 Uiso 1 calc R . H73B H 0.2293(3) 0.1473(2) 0.6361(2) 0.039 Uiso 1 calc R . C74 C 0.0190(4) 0.1970(3) 0.4167(3) 0.054(2) Uani 1 d . . H74A H 0.0361(4) 0.2010(3) 0.3752(3) 0.065 Uiso 1 calc R . H74B H -0.0279(4) 0.2270(3) 0.4089(3) 0.065 Uiso 1 calc R . C75 C -0.0087(3) 0.1294(3) 0.4213(3) 0.054(2) Uani 1 d . . H75A H -0.0354(3) 0.1111(3) 0.3717(3) 0.065 Uiso 1 calc R . H75B H -0.0507(3) 0.1295(3) 0.4434(3) 0.065 Uiso 1 calc R . N76 N 0.0656(3) 0.0890(2) 0.4670(2) 0.0312(9) Uani 1 d . . H76A H 0.0723(3) 0.0561(2) 0.4391(2) 0.037 Uiso 1 calc R . H76B H 0.0562(3) 0.0713(2) 0.5053(2) 0.037 Uiso 1 calc R . C77 C 0.1370(7) 0.2721(3) 0.4828(7) 0.131(5) Uani 1 d . . H77A H 0.1057(7) 0.2950(3) 0.4366(7) 0.158 Uiso 1 calc R . H77B H 0.1394(7) 0.3005(3) 0.5233(7) 0.158 Uiso 1 calc R . C78 C 0.2212(5) 0.2609(4) 0.4886(4) 0.079(2) Uani 1 d . . H78A H 0.2211(5) 0.2594(4) 0.4391(4) 0.095 Uiso 1 calc R . H78B H 0.2571(5) 0.2972(4) 0.5149(4) 0.095 Uiso 1 calc R . N79 N 0.2556(3) 0.2038(2) 0.5253(2) 0.0537(13) Uani 1 d . . H79A H 0.2806(3) 0.2112(2) 0.5747(2) 0.064 Uiso 1 calc R . H79B H 0.2958(3) 0.1888(2) 0.5101(2) 0.064 Uiso 1 calc R . Cl1 Cl -0.04405(7) 0.13875(6) 1.00716(7) 0.0367(3) Uani 1 d . . O101 O -0.0909(4) 0.1532(3) 1.0491(3) 0.094(2) Uani 1 d . . O102 O 0.0378(3) 0.1628(2) 1.0349(3) 0.081(2) Uani 1 d . . O103 O -0.0374(3) 0.0702(2) 1.0086(3) 0.079(2) Uani 1 d . . O104 O -0.0876(3) 0.1600(2) 0.9347(2) 0.0634(12) Uani 1 d . . Cl2 Cl 0.35916(11) 0.23904(8) 0.74261(7) 0.0633(5) Uani 1 d . . O201 O 0.3499(3) 0.2930(3) 0.7853(3) 0.102(2) Uani 1 d . . O202 O 0.4470(3) 0.2274(3) 0.7634(3) 0.106(2) Uani 1 d . . O203 O 0.3218(3) 0.2625(2) 0.6699(2) 0.0706(13) Uani 1 d . . O204 O 0.3141(6) 0.1874(4) 0.7472(5) 0.235(7) Uani 1 d . . Cl3 Cl 0.00332(8) -0.05688(5) 0.37114(6) 0.0336(3) Uani 1 d . . O301 O 0.0406(3) -0.0076(2) 0.3442(2) 0.0681(14) Uani 1 d . . O302 O -0.0835(3) -0.0415(2) 0.3522(2) 0.0571(11) Uani 1 d . . O303 O 0.0091(3) -0.1174(2) 0.3401(2) 0.0508(10) Uani 1 d . . O304 O 0.0440(2) -0.0604(2) 0.4492(2) 0.0388(8) Uani 1 d . . Cl4 Cl 0.54789(7) 0.10022(5) 0.05920(6) 0.0260(2) Uani 1 d . . O401 O 0.5277(3) 0.0407(2) 0.0831(3) 0.0629(13) Uani 1 d . . O402 O 0.4726(2) 0.1343(2) 0.0157(2) 0.0432(9) Uani 1 d . . O403 O 0.5960(2) 0.0875(2) 0.0160(2) 0.0325(7) Uani 1 d . . O404 O 0.5975(2) 0.1385(2) 0.1205(2) 0.0392(8) Uani 1 d . . O80 O 0.5060(6) 0.2254(5) 0.6323(5) 0.087(2) Uani 0.598(6) d P 1 C90 C 0.5976(6) -0.1786(5) 0.5473(4) 0.093(3) Uani 0.598(6) d PD 1 O91 O 0.5973(6) -0.1578(5) 0.4807(5) 0.089(2) Uani 0.598(6) d PD 1 O80X O 0.4522(10) 0.1969(7) 0.6299(8) 0.087(2) Uani 0.402(6) d P 2 C90X C 0.5976(6) -0.1786(5) 0.5473(4) 0.093(3) Uani 0.402(6) d P 2 O91X O 0.6646(8) -0.2206(7) 0.5746(7) 0.089(2) Uani 0.402(6) d PD 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0173(3) 0.0213(3) 0.0152(3) -0.0022(2) 0.0049(2) -0.0021(2) O1 0.0222(15) 0.0216(15) 0.0172(14) -0.0033(11) 0.0036(12) -0.0001(12) C1 0.018(2) 0.025(2) 0.020(2) -0.004(2) 0.008(2) 0.001(2) C2 0.019(2) 0.022(2) 0.023(2) -0.005(2) 0.011(2) -0.002(2) C3 0.029(2) 0.023(2) 0.024(2) -0.007(2) 0.013(2) -0.001(2) C4 0.022(2) 0.031(2) 0.018(2) -0.006(2) 0.010(2) -0.005(2) C5 0.025(2) 0.029(2) 0.014(2) -0.001(2) 0.008(2) -0.004(2) C6 0.019(2) 0.022(2) 0.020(2) -0.003(2) 0.009(2) -0.002(2) N7 0.019(2) 0.024(2) 0.016(2) -0.0011(14) 0.0058(14) -0.0024(14) C8 0.028(2) 0.022(2) 0.011(2) -0.005(2) 0.007(2) -0.001(2) C9 0.028(2) 0.030(2) 0.021(2) 0.000(2) 0.009(2) 0.000(2) C10 0.033(3) 0.037(3) 0.024(2) -0.002(2) 0.006(2) 0.007(2) C11 0.049(3) 0.024(2) 0.023(2) 0.002(2) 0.006(2) 0.003(2) C12 0.043(3) 0.029(2) 0.023(2) -0.001(2) 0.012(2) -0.009(2) C13 0.029(2) 0.029(2) 0.016(2) -0.003(2) 0.006(2) -0.001(2) C14 0.032(2) 0.020(2) 0.026(2) -0.001(2) 0.010(2) 0.004(2) C15 0.032(3) 0.033(3) 0.040(3) -0.002(2) 0.008(2) 0.010(2) C16 0.049(3) 0.028(2) 0.028(2) 0.004(2) 0.018(2) 0.002(2) C17 0.046(3) 0.023(2) 0.037(3) 0.000(2) 0.014(2) 0.002(2) C18 0.029(2) 0.030(2) 0.021(2) -0.005(2) 0.011(2) -0.008(2) C19 0.045(3) 0.046(3) 0.029(3) -0.016(2) 0.021(2) -0.012(2) C20 0.045(3) 0.041(3) 0.019(2) -0.002(2) 0.002(2) -0.017(2) C21 0.032(3) 0.046(3) 0.023(2) -0.007(2) 0.012(2) -0.011(2) N30 0.025(2) 0.025(2) 0.017(2) -0.0014(14) 0.0055(15) -0.0007(15) C31 0.029(2) 0.038(3) 0.021(2) -0.002(2) -0.001(2) 0.007(2) C32 0.021(2) 0.057(3) 0.025(2) -0.006(2) 0.002(2) 0.007(2) N33 0.021(2) 0.039(2) 0.023(2) -0.003(2) 0.007(2) -0.003(2) C34 0.027(2) 0.029(2) 0.019(2) -0.006(2) 0.004(2) -0.007(2) C35 0.041(3) 0.032(3) 0.026(2) -0.008(2) 0.010(2) -0.004(2) N36 0.027(2) 0.024(2) 0.020(2) -0.0038(14) 0.006(2) -0.007(2) C37 0.040(3) 0.032(2) 0.017(2) -0.001(2) 0.011(2) -0.009(2) C38 0.033(3) 0.039(3) 0.026(2) -0.006(2) 0.017(2) -0.013(2) N39 0.019(2) 0.023(2) 0.021(2) -0.0061(14) 0.0066(14) -0.0034(14) Co2 0.0342(3) 0.0204(3) 0.0177(3) -0.0044(2) 0.0068(2) -0.0021(3) O41 0.035(2) 0.028(2) 0.0176(15) -0.0017(12) 0.0066(13) -0.0054(14) C41 0.028(2) 0.035(3) 0.020(2) -0.005(2) 0.008(2) -0.014(2) C42 0.033(3) 0.046(3) 0.020(2) -0.008(2) 0.013(2) -0.017(2) C43 0.046(3) 0.052(3) 0.024(2) -0.010(2) 0.023(2) -0.019(3) C44 0.047(3) 0.038(3) 0.035(3) -0.010(2) 0.029(2) -0.012(2) C45 0.044(3) 0.038(3) 0.026(2) -0.004(2) 0.021(2) -0.004(2) C46 0.034(2) 0.034(3) 0.021(2) -0.007(2) 0.013(2) -0.006(2) N47 0.043(2) 0.036(2) 0.015(2) -0.002(2) 0.012(2) 0.009(2) C48 0.030(2) 0.038(3) 0.014(2) -0.002(2) 0.011(2) 0.012(2) C49 0.051(3) 0.032(3) 0.042(3) 0.005(2) -0.017(3) -0.008(2) C50 0.047(3) 0.031(3) 0.057(4) 0.015(3) 0.010(3) 0.007(2) C51 0.051(3) 0.044(3) 0.018(2) 0.001(2) 0.010(2) 0.018(3) C52 0.048(4) 0.092(5) 0.046(4) 0.028(4) -0.028(3) -0.022(4) C53 0.030(3) 0.084(5) 0.058(4) 0.031(4) -0.003(3) -0.016(3) C54 0.033(3) 0.062(3) 0.020(2) 0.001(2) 0.013(2) -0.015(2) C55 0.035(3) 0.061(3) 0.022(2) 0.002(2) 0.009(2) -0.016(2) C56 0.056(4) 0.073(4) 0.046(3) 0.025(3) 0.001(3) -0.037(3) C57 0.046(3) 0.144(7) 0.022(3) 0.010(3) 0.020(3) 0.006(4) C58 0.087(5) 0.036(3) 0.052(3) -0.002(3) 0.054(3) -0.003(3) C59 0.076(4) 0.041(3) 0.061(4) 0.000(3) 0.051(3) 0.004(3) C60 0.148(7) 0.052(4) 0.091(5) -0.032(4) 0.099(6) -0.038(4) C61 0.121(6) 0.047(4) 0.073(4) 0.009(3) 0.076(5) 0.027(4) N70 0.060(3) 0.025(2) 0.055(3) 0.013(2) 0.027(2) 0.011(2) C71 0.059(4) 0.037(3) 0.059(4) -0.009(3) 0.035(3) 0.001(3) C72 0.045(3) 0.037(3) 0.054(3) -0.010(2) 0.033(3) -0.004(2) N73 0.035(2) 0.036(2) 0.023(2) -0.012(2) 0.010(2) 0.002(2) C74 0.064(4) 0.071(4) 0.037(3) 0.032(3) 0.030(3) 0.040(3) C75 0.031(3) 0.091(5) 0.036(3) -0.003(3) 0.009(2) 0.004(3) N76 0.046(2) 0.030(2) 0.020(2) -0.003(2) 0.016(2) -0.010(2) C77 0.187(11) 0.023(3) 0.267(14) 0.052(6) 0.177(11) 0.039(5) C78 0.101(6) 0.067(5) 0.057(4) 0.020(4) 0.018(4) -0.029(4) N79 0.066(3) 0.057(3) 0.035(3) -0.020(2) 0.017(2) -0.033(3) Cl1 0.0266(6) 0.0475(7) 0.0381(6) 0.0127(5) 0.0149(5) 0.0041(5) O101 0.095(4) 0.137(5) 0.075(3) 0.003(3) 0.061(3) 0.027(4) O102 0.044(3) 0.086(4) 0.085(3) 0.034(3) -0.004(2) -0.029(2) O103 0.074(3) 0.042(3) 0.123(4) 0.025(3) 0.042(3) -0.005(2) O104 0.057(3) 0.082(3) 0.043(2) 0.028(2) 0.011(2) -0.006(2) Cl2 0.0717(11) 0.0621(10) 0.0267(7) 0.0014(6) -0.0116(7) -0.0183(8) O201 0.069(3) 0.160(6) 0.067(3) -0.041(4) 0.018(3) -0.006(4) O202 0.083(4) 0.101(4) 0.068(3) -0.045(3) -0.041(3) 0.052(3) O203 0.072(3) 0.084(3) 0.036(2) 0.002(2) 0.001(2) 0.009(3) O204 0.218(9) 0.140(7) 0.179(8) 0.118(6) -0.099(7) -0.115(7) Cl3 0.0515(7) 0.0295(6) 0.0164(5) -0.0022(4) 0.0100(5) -0.0167(5) O301 0.126(4) 0.053(3) 0.046(2) -0.013(2) 0.055(3) -0.049(3) O302 0.059(3) 0.039(2) 0.055(3) 0.016(2) 0.003(2) 0.001(2) O303 0.080(3) 0.038(2) 0.029(2) -0.011(2) 0.016(2) -0.011(2) O304 0.049(2) 0.045(2) 0.017(2) -0.0035(14) 0.0066(15) -0.007(2) Cl4 0.0272(5) 0.0200(5) 0.0361(6) -0.0016(4) 0.0182(5) -0.0014(4) O401 0.075(3) 0.024(2) 0.121(4) 0.013(2) 0.073(3) 0.000(2) O402 0.020(2) 0.031(2) 0.067(3) -0.010(2) 0.005(2) 0.0007(14) O403 0.035(2) 0.038(2) 0.030(2) -0.0007(14) 0.0191(15) 0.0062(15) O404 0.049(2) 0.042(2) 0.024(2) -0.0053(15) 0.010(2) 0.007(2) O80 0.087(7) 0.073(6) 0.095(5) -0.008(5) 0.029(5) 0.002(4) C90 0.091(6) 0.121(8) 0.067(5) 0.023(5) 0.031(5) -0.016(6) O91 0.080(5) 0.123(7) 0.072(5) 0.000(5) 0.040(4) 0.001(5) O80X 0.087(7) 0.073(6) 0.095(5) -0.008(5) 0.029(5) 0.002(4) C90X 0.091(6) 0.121(8) 0.067(5) 0.023(5) 0.031(5) -0.016(6) O91X 0.080(5) 0.123(7) 0.072(5) 0.000(5) 0.040(4) 0.001(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 Co1 O1 1.885(3) . ? Co1 N7 1.921(3) . ? Co1 N36 1.956(3) . ? Co1 N39 1.955(3) . ? Co1 N30 1.964(3) . ? Co1 N33 1.971(4) . ? O1 C1 1.323(5) . ? C1 C2 1.418(6) . ? C1 C6 1.436(6) . ? C2 C3 1.376(6) . ? C2 C14 1.531(6) . ? C3 C4 1.430(6) . ? C4 C5 1.367(6) . ? C4 C18 1.541(6) . ? C5 C6 1.421(6) . ? C6 N7 1.349(5) . ? N7 C8 1.425(5) . ? C8 C13 1.385(6) . ? C8 C9 1.405(6) . ? C9 C10 1.389(6) . ? C10 C11 1.380(7) . ? C11 C12 1.387(7) . ? C12 C13 1.385(6) . ? C14 C17 1.530(6) . ? C14 C16 1.536(6) . ? C14 C15 1.538(6) . ? C18 C20 1.530(6) . ? C18 C21 1.530(6) . ? C18 C19 1.544(6) . ? N30 C37 1.494(6) . ? N30 C31 1.499(6) . ? N30 C34 1.506(5) . ? C31 C32 1.503(7) . ? C32 N33 1.495(5) . ? C34 C35 1.511(6) . ? C35 N36 1.489(6) . ? C37 C38 1.515(7) . ? C38 N39 1.491(5) . ? Co2 O41 1.906(3) . ? Co2 N47 1.908(4) . ? Co2 N79 1.941(4) . ? Co2 N70 1.948(4) . ? Co2 N76 1.949(4) . ? Co2 N73 1.951(4) . ? O41 C41 1.312(6) . ? C41 C42 1.424(6) . ? C41 C46 1.436(6) . ? C42 C43 1.371(7) . ? C42 C54 1.530(7) . ? C43 C44 1.426(7) . ? C44 C45 1.368(6) . ? C44 C58 1.527(7) . ? C45 C46 1.416(7) . ? C46 N47 1.346(5) . ? N47 C48 1.427(6) . ? C48 C49 1.365(7) . ? C48 C53 1.368(7) . ? C49 C50 1.389(7) . ? C50 C51 1.360(7) . ? C51 C52 1.355(8) . ? C52 C53 1.374(8) . ? C54 C56 1.533(8) . ? C54 C55 1.533(7) . ? C54 C57 1.537(7) . ? C58 C61 1.530(9) . ? C58 C60 1.538(9) . ? C58 C59 1.554(7) . ? N70 C74 1.462(8) . ? N70 C77 1.503(9) . ? N70 C71 1.531(7) . ? C71 C72 1.456(8) . ? C72 N73 1.480(6) . ? C74 C75 1.506(9) . ? C75 N76 1.511(7) . ? C77 C78 1.440(11) . ? C78 N79 1.404(9) . ? Cl1 O102 1.399(4) . ? Cl1 O101 1.413(5) . ? Cl1 O104 1.413(4) . ? Cl1 O103 1.437(5) . ? Cl2 O204 1.358(7) . ? Cl2 O203 1.422(4) . ? Cl2 O202 1.435(6) . ? Cl2 O201 1.460(6) . ? Cl3 O303 1.430(4) . ? Cl3 O301 1.430(4) . ? Cl3 O304 1.435(3) . ? Cl3 O302 1.438(4) . ? Cl4 O401 1.426(4) . ? Cl4 O404 1.430(3) . ? Cl4 O402 1.440(3) . ? Cl4 O403 1.445(3) . ? C90 O91 1.398(9) . ? C90X O91X 1.386(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 N7 84.52(13) . . ? O1 Co1 N36 177.84(14) . . ? N7 Co1 N36 97.19(15) . . ? O1 Co1 N39 86.56(14) . . ? N7 Co1 N39 91.56(14) . . ? N36 Co1 N39 92.07(15) . . ? O1 Co1 N30 91.75(13) . . ? N7 Co1 N30 175.79(15) . . ? N36 Co1 N30 86.49(15) . . ? N39 Co1 N30 86.27(15) . . ? O1 Co1 N33 86.30(15) . . ? N7 Co1 N33 94.85(14) . . ? N36 Co1 N33 94.9(2) . . ? N39 Co1 N33 169.9(2) . . ? N30 Co1 N33 86.83(15) . . ? C1 O1 Co1 112.5(2) . . ? O1 C1 C2 122.6(4) . . ? O1 C1 C6 116.6(4) . . ? C2 C1 C6 120.8(4) . . ? C3 C2 C1 116.3(4) . . ? C3 C2 C14 123.1(4) . . ? C1 C2 C14 120.6(4) . . ? C2 C3 C4 124.3(4) . . ? C5 C4 C3 119.1(4) . . ? C5 C4 C18 122.8(4) . . ? C3 C4 C18 118.1(4) . . ? C4 C5 C6 119.5(4) . . ? N7 C6 C5 126.9(4) . . ? N7 C6 C1 113.2(3) . . ? C5 C6 C1 119.9(4) . . ? C6 N7 C8 123.0(3) . . ? C6 N7 Co1 112.0(3) . . ? C8 N7 Co1 123.9(3) . . ? C13 C8 C9 119.7(4) . . ? C13 C8 N7 119.7(4) . . ? C9 C8 N7 120.5(4) . . ? C10 C9 C8 119.1(4) . . ? C11 C10 C9 121.0(4) . . ? C10 C11 C12 119.5(4) . . ? C13 C12 C11 120.3(4) . . ? C12 C13 C8 120.3(4) . . ? C17 C14 C2 111.6(4) . . ? C17 C14 C16 107.1(4) . . ? C2 C14 C16 110.2(4) . . ? C17 C14 C15 108.3(4) . . ? C2 C14 C15 109.3(4) . . ? C16 C14 C15 110.2(4) . . ? C20 C18 C21 109.6(4) . . ? C20 C18 C4 111.4(4) . . ? C21 C18 C4 108.5(3) . . ? C20 C18 C19 108.5(4) . . ? C21 C18 C19 108.6(4) . . ? C4 C18 C19 110.1(4) . . ? C37 N30 C31 112.0(4) . . ? C37 N30 C34 112.3(3) . . ? C31 N30 C34 110.7(3) . . ? C37 N30 Co1 105.9(3) . . ? C31 N30 Co1 105.5(3) . . ? C34 N30 Co1 110.2(3) . . ? N30 C31 C32 108.5(4) . . ? N33 C32 C31 108.3(4) . . ? C32 N33 Co1 109.9(3) . . ? N30 C34 C35 111.2(3) . . ? N36 C35 C34 107.9(4) . . ? C35 N36 Co1 110.1(3) . . ? N30 C37 C38 108.7(4) . . ? N39 C38 C37 108.9(3) . . ? C38 N39 Co1 111.4(3) . . ? O41 Co2 N47 84.48(14) . . ? O41 Co2 N79 87.6(2) . . ? N47 Co2 N79 94.4(2) . . ? O41 Co2 N70 94.2(2) . . ? N47 Co2 N70 178.0(2) . . ? N79 Co2 N70 87.0(2) . . ? O41 Co2 N76 85.22(14) . . ? N47 Co2 N76 94.0(2) . . ? N79 Co2 N76 168.4(2) . . ? N70 Co2 N76 84.4(2) . . ? O41 Co2 N73 179.3(2) . . ? N47 Co2 N73 95.1(2) . . ? N79 Co2 N73 91.8(2) . . ? N70 Co2 N73 86.2(2) . . ? N76 Co2 N73 95.4(2) . . ? C41 O41 Co2 112.4(3) . . ? O41 C41 C42 123.6(4) . . ? O41 C41 C46 116.8(4) . . ? C42 C41 C46 119.6(4) . . ? C43 C42 C41 116.0(4) . . ? C43 C42 C54 122.4(4) . . ? C41 C42 C54 121.6(5) . . ? C42 C43 C44 125.5(4) . . ? C45 C44 C43 118.4(5) . . ? C45 C44 C58 122.1(5) . . ? C43 C44 C58 119.5(4) . . ? C44 C45 C46 119.1(5) . . ? N47 C46 C45 125.3(4) . . ? N47 C46 C41 113.4(4) . . ? C45 C46 C41 121.3(4) . . ? C46 N47 C48 120.9(4) . . ? C46 N47 Co2 112.8(3) . . ? C48 N47 Co2 126.0(3) . . ? C49 C48 C53 118.6(5) . . ? C49 C48 N47 120.3(4) . . ? C53 C48 N47 121.1(5) . . ? C48 C49 C50 120.9(5) . . ? C51 C50 C49 120.0(5) . . ? C52 C51 C50 118.9(5) . . ? C51 C52 C53 121.7(5) . . ? C48 C53 C52 120.0(6) . . ? C42 C54 C56 110.5(4) . . ? C42 C54 C55 109.4(4) . . ? C56 C54 C55 109.8(5) . . ? C42 C54 C57 111.8(5) . . ? C56 C54 C57 108.1(5) . . ? C55 C54 C57 107.2(4) . . ? C44 C58 C61 112.6(4) . . ? C44 C58 C60 108.8(6) . . ? C61 C58 C60 109.0(5) . . ? C44 C58 C59 110.3(4) . . ? C61 C58 C59 107.4(5) . . ? C60 C58 C59 108.7(4) . . ? C74 N70 C77 115.3(6) . . ? C74 N70 C71 108.6(4) . . ? C77 N70 C71 111.3(5) . . ? C74 N70 Co2 105.9(3) . . ? C77 N70 Co2 107.5(4) . . ? C71 N70 Co2 107.9(3) . . ? C72 C71 N70 108.5(5) . . ? C71 C72 N73 109.7(4) . . ? C72 N73 Co2 111.0(3) . . ? N70 C74 C75 108.8(4) . . ? C74 C75 N76 110.1(4) . . ? C75 N76 Co2 110.3(3) . . ? C78 C77 N70 114.5(5) . . ? N79 C78 C77 112.9(6) . . ? C78 N79 Co2 109.1(4) . . ? O102 Cl1 O101 115.0(4) . . ? O102 Cl1 O104 110.0(3) . . ? O101 Cl1 O104 109.9(3) . . ? O102 Cl1 O103 106.8(3) . . ? O101 Cl1 O103 105.1(4) . . ? O104 Cl1 O103 109.9(3) . . ? O204 Cl2 O203 107.6(4) . . ? O204 Cl2 O202 114.9(6) . . ? O203 Cl2 O202 110.9(4) . . ? O204 Cl2 O201 112.0(7) . . ? O203 Cl2 O201 102.6(3) . . ? O202 Cl2 O201 108.2(3) . . ? O303 Cl3 O301 110.7(2) . . ? O303 Cl3 O304 109.7(2) . . ? O301 Cl3 O304 110.1(2) . . ? O303 Cl3 O302 109.3(3) . . ? O301 Cl3 O302 108.9(3) . . ? O304 Cl3 O302 108.1(2) . . ? O401 Cl4 O404 110.3(3) . . ? O401 Cl4 O402 110.3(2) . . ? O404 Cl4 O402 109.6(2) . . ? O401 Cl4 O403 108.5(2) . . ? O404 Cl4 O403 108.6(2) . . ? O402 Cl4 O403 109.5(2) . . ? _refine_diff_density_max 1.113 _refine_diff_density_min -0.892 _refine_diff_density_rms 0.084 #===END data_4 _database_code_CSD 197836 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical '[C26 H40 N5 O1 Fe]2+, 2 (CLO4)-, 0.5 CH3OH, 0.5 H2O' _chemical_formula_sum 'C26.50 H46 Cl2 Fe N5 O10' _chemical_formula_weight 721.43 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 16.8198(3) _cell_length_b 21.0452(6) _cell_length_c 20.6800(6) _cell_angle_alpha 90.00 _cell_angle_beta 113.60(1) _cell_angle_gamma 90.00 _cell_volume 6708.0(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 142490 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'opaque block' _exptl_crystal_colour 'deep blue' _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method ? _exptl_crystal_F_000 3040 _exptl_absorpt_coefficient_mu 0.668 _exptl_absorpt_correction_type 'not corrected' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Nonius Kappa-CCD' _diffrn_measurement_method '554 images at 1 deg. in \w and 30 sec.' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 82667 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 31.00 _reflns_number_total 21218 _reflns_number_observed 17467 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'DENZO, Nonius Collect Software' _computing_cell_refinement 'DENZO, Nonius Collect Software' _computing_data_reduction 'DENZO, Nonius Collect Software' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 79 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+10.4200P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21139 _refine_ls_number_parameters 810 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0756 _refine_ls_R_factor_obs 0.0603 _refine_ls_wR_factor_all 0.1595 _refine_ls_wR_factor_obs 0.1465 _refine_ls_goodness_of_fit_all 1.052 _refine_ls_goodness_of_fit_obs 1.097 _refine_ls_restrained_S_all 1.081 _refine_ls_restrained_S_obs 1.097 _refine_ls_shift/esd_max -0.383 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.78038(2) 0.036664(13) 0.552814(15) 0.01792(7) Uani 1 d . . Fe2 Fe 0.82962(2) 0.14522(2) 0.98512(2) 0.02378(8) Uani 1 d . . N2 N 0.72647(11) 0.04030(8) 0.45494(9) 0.0184(3) Uani 1 d . . O1 O 0.78425(10) 0.12688(7) 0.54450(8) 0.0196(3) Uani 1 d . . C1 C 0.73506(13) 0.14716(9) 0.48201(10) 0.0176(3) Uani 1 d . . C2 C 0.70091(13) 0.09880(9) 0.42858(10) 0.0173(3) Uani 1 d . . C3 C 0.64769(13) 0.11493(10) 0.35737(10) 0.0194(4) Uani 1 d . . H3 H 0.62724(13) 0.08300(10) 0.32204(10) 0.023 Uiso 1 calc R . C4 C 0.62661(13) 0.17752(10) 0.34090(11) 0.0196(4) Uani 1 d . . C5 C 0.66083(14) 0.22484(10) 0.39564(11) 0.0199(4) Uani 1 d . . H5 H 0.64467(14) 0.26780(10) 0.38302(11) 0.024 Uiso 1 calc R . C6 C 0.71491(13) 0.21265(9) 0.46452(11) 0.0181(3) Uani 1 d . . C7 C 0.70921(15) -0.01418(10) 0.40951(11) 0.0220(4) Uani 1 d . . C8 C 0.7756(2) -0.0373(2) 0.39196(14) 0.0412(7) Uani 1 d . . H8 H 0.8290(2) -0.0151(2) 0.40648(14) 0.049 Uiso 1 calc R . C9 C 0.7635(2) -0.0928(2) 0.3534(2) 0.0561(10) Uani 1 d . . H9 H 0.8088(2) -0.1086(2) 0.3416(2) 0.067 Uiso 1 calc R . C10 C 0.6874(3) -0.12447(14) 0.3323(2) 0.0503(9) Uani 1 d . . H10 H 0.6797(3) -0.16232(14) 0.3054(2) 0.060 Uiso 1 calc R . C11 C 0.6206(2) -0.10267(14) 0.34927(15) 0.0452(7) Uani 1 d . . H11 H 0.5674(2) -0.12546(14) 0.33437(15) 0.054 Uiso 1 calc R . C12 C 0.6319(2) -0.04651(13) 0.38875(14) 0.0353(5) Uani 1 d . . H12 H 0.5866(2) -0.03105(13) 0.40095(14) 0.042 Uiso 1 calc R . N13 N 0.90425(13) 0.03131(10) 0.56286(11) 0.0281(4) Uani 1 d . . H13A H 0.91327(13) -0.00725(10) 0.54593(11) 0.034 Uiso 1 calc R . H13B H 0.91450(13) 0.06279(10) 0.53629(11) 0.034 Uiso 1 calc R . C13 C 0.9663(2) 0.0384(2) 0.63829(14) 0.0382(6) Uani 1 d . . H13A' H 1.0165(2) 0.0646(2) 0.64132(14) 0.046 Uiso 1 calc R . H13B' H 0.9880(2) -0.0039(2) 0.65887(14) 0.046 Uiso 1 calc R . C14 C 0.9191(2) 0.06983(13) 0.67839(13) 0.0335(5) Uani 1 d . . H14A H 0.9535(2) 0.06550(13) 0.72978(13) 0.040 Uiso 1 calc R . H14B H 0.9115(2) 0.11567(13) 0.66678(13) 0.040 Uiso 1 calc R . N15 N 0.77582(14) -0.05790(9) 0.56339(10) 0.0253(4) Uani 1 d . . H15A H 0.72064(14) -0.06995(9) 0.55714(10) 0.030 Uiso 1 calc R . H15B H 0.78956(14) -0.07788(9) 0.52964(10) 0.030 Uiso 1 calc R . C15 C 0.8385(2) -0.07693(12) 0.63494(13) 0.0344(6) Uani 1 d . . H15C H 0.8973(2) -0.08091(12) 0.63534(13) 0.041 Uiso 1 calc R . H15D H 0.8217(2) -0.11868(12) 0.64762(13) 0.041 Uiso 1 calc R . C16 C 0.8388(2) -0.02716(11) 0.68820(13) 0.0307(5) Uani 1 d . . H16A H 0.7892(2) -0.03473(11) 0.70148(13) 0.037 Uiso 1 calc R . H16B H 0.8929(2) -0.03112(11) 0.73134(13) 0.037 Uiso 1 calc R . N17 N 0.66803(12) 0.04983(9) 0.56359(10) 0.0226(3) Uani 1 d . . H17A H 0.64042(12) 0.08500(9) 0.53803(10) 0.027 Uiso 1 calc R . H17B H 0.63268(12) 0.01523(9) 0.54539(10) 0.027 Uiso 1 calc R . C17 C 0.6813(2) 0.05876(13) 0.63892(13) 0.0320(5) Uani 1 d . . H17C H 0.6688(2) 0.01859(13) 0.65798(13) 0.038 Uiso 1 calc R . H17D H 0.6413(2) 0.09187(13) 0.64234(13) 0.038 Uiso 1 calc R . C18 C 0.7745(2) 0.07855(11) 0.68110(12) 0.0288(5) Uani 1 d . . H18A H 0.7820(2) 0.12406(11) 0.67280(12) 0.035 Uiso 1 calc R . H18B H 0.7894(2) 0.07248(11) 0.73211(12) 0.035 Uiso 1 calc R . N19 N 0.83267(13) 0.03909(9) 0.65879(10) 0.0244(4) Uani 1 d . . C20 C 0.56613(15) 0.19949(11) 0.26687(11) 0.0239(4) Uani 1 d . . C21 C 0.6072(2) 0.25525(13) 0.24294(14) 0.0358(6) Uani 1 d . . H21A H 0.5679(2) 0.26882(13) 0.19556(14) 0.054 Uiso 1 calc R . H21B H 0.6625(2) 0.24163(13) 0.24212(14) 0.054 Uiso 1 calc R . H21C H 0.6173(2) 0.29079(13) 0.27592(14) 0.054 Uiso 1 calc R . C22 C 0.4810(2) 0.22290(14) 0.26998(13) 0.0352(6) Uani 1 d . . H22A H 0.4413(2) 0.23721(14) 0.22303(13) 0.053 Uiso 1 calc R . H22B H 0.4934(2) 0.25830(14) 0.30339(13) 0.053 Uiso 1 calc R . H22C H 0.4541(2) 0.18809(14) 0.28550(13) 0.053 Uiso 1 calc R . C23 C 0.5460(2) 0.14557(12) 0.21286(12) 0.0318(5) Uani 1 d . . H23A H 0.5073(2) 0.16127(12) 0.16624(12) 0.048 Uiso 1 calc R . H23B H 0.5177(2) 0.11060(12) 0.22682(12) 0.048 Uiso 1 calc R . H23C H 0.6001(2) 0.13034(12) 0.21098(12) 0.048 Uiso 1 calc R . C24 C 0.75283(14) 0.26400(10) 0.52056(12) 0.0222(4) Uani 1 d . . C25 C 0.7282(2) 0.25190(13) 0.58359(14) 0.0347(5) Uani 1 d . . H25A H 0.7531(2) 0.28535(13) 0.61895(14) 0.052 Uiso 1 calc R . H25B H 0.7509(2) 0.21052(13) 0.60460(14) 0.052 Uiso 1 calc R . H25C H 0.6649(2) 0.25214(13) 0.56737(14) 0.052 Uiso 1 calc R . C26 C 0.7184(2) 0.32996(11) 0.49123(14) 0.0313(5) Uani 1 d . . H26A H 0.7438(2) 0.36188(11) 0.52835(14) 0.047 Uiso 1 calc R . H26B H 0.6551(2) 0.33053(11) 0.47503(14) 0.047 Uiso 1 calc R . H26C H 0.7342(2) 0.33965(11) 0.45156(14) 0.047 Uiso 1 calc R . C27 C 0.8523(2) 0.26396(12) 0.54551(15) 0.0323(5) Uani 1 d . . H27A H 0.8773(2) 0.29682(12) 0.58157(15) 0.048 Uiso 1 calc R . H27B H 0.8675(2) 0.27273(12) 0.50533(15) 0.048 Uiso 1 calc R . H27C H 0.8752(2) 0.22231(12) 0.56549(15) 0.048 Uiso 1 calc R . O31 O 0.83641(11) 0.14505(8) 1.08036(9) 0.0269(3) Uani 1 d . . C31 C 0.79206(14) 0.10005(10) 1.09230(12) 0.0232(4) Uani 1 d . . N32 N 0.75504(14) 0.07772(10) 0.97457(10) 0.0285(4) Uani 1 d . . C32 C 0.74382(15) 0.06011(11) 1.03277(12) 0.0242(4) Uani 1 d . . C33 C 0.6915(2) 0.00952(11) 1.03899(13) 0.0274(4) Uani 1 d . . H33 H 0.6589(2) -0.01600(11) 0.99929(13) 0.033 Uiso 1 calc R . C34 C 0.6890(2) -0.00173(11) 1.10312(14) 0.0290(5) Uani 1 d . . C35 C 0.7387(2) 0.03797(12) 1.16188(13) 0.0284(5) Uani 1 d . . H35 H 0.7362(2) 0.02860(12) 1.20597(13) 0.034 Uiso 1 calc R . C36 C 0.78930(15) 0.08821(11) 1.15977(12) 0.0252(4) Uani 1 d . . C37 C 0.7159(2) 0.04095(13) 0.91085(12) 0.0343(6) Uani 1 d . . C38 C 0.6408(2) 0.0641(2) 0.8569(2) 0.0587(10) Uani 1 d . . H38 H 0.6140(2) 0.1022(2) 0.8626(2) 0.070 Uiso 1 calc R . C39 C 0.6065(2) 0.0293(3) 0.7941(2) 0.0723(14) Uani 1 d . . H39 H 0.5555(2) 0.0440(3) 0.7565(2) 0.087 Uiso 1 calc R . C40 C 0.6453(2) -0.0262(2) 0.7858(2) 0.0550(10) Uani 1 d . . H40 H 0.6198(2) -0.0502(2) 0.7435(2) 0.066 Uiso 1 calc R . C41 C 0.7208(3) -0.0466(2) 0.8387(2) 0.0616(11) Uani 1 d . . H41 H 0.7494(3) -0.0835(2) 0.8323(2) 0.074 Uiso 1 calc R . C42 C 0.7556(3) -0.01288(14) 0.9020(2) 0.0576(11) Uani 1 d . . H42 H 0.8071(3) -0.02749(14) 0.9392(2) 0.069 Uiso 1 calc R . N43 N 0.93843(15) 0.09372(10) 1.02344(11) 0.0307(4) Uani 1 d . . H43A H 0.93071(15) 0.05957(10) 1.04809(11) 0.037 Uiso 1 calc R . H43B H 0.95054(15) 0.07837(10) 0.98672(11) 0.037 Uiso 1 calc R . C43 C 1.0132(2) 0.13304(14) 1.0712(2) 0.0388(6) Uani 1 d . . H43A' H 1.0618(2) 0.12972(14) 1.0560(2) 0.047 Uiso 1 calc R . H43B' H 1.0333(2) 0.11661(14) 1.1200(2) 0.047 Uiso 1 calc R . C44 C 0.9867(2) 0.20235(14) 1.0697(2) 0.0407(6) Uani 1 d . . H44A H 0.9671(2) 0.21059(14) 1.1081(2) 0.049 Uiso 1 calc R . H44B H 1.0369(2) 0.23025(14) 1.0769(2) 0.049 Uiso 1 calc R . N45 N 0.7450(2) 0.21605(12) 0.96467(13) 0.0384(5) Uani 1 d . . H45A H 0.7252(2) 0.22757(12) 0.91793(13) 0.046 Uiso 1 calc R . H45B H 0.6982(2) 0.20392(12) 0.97419(13) 0.046 Uiso 1 calc R . C45 C 0.7908(2) 0.26964(15) 1.0104(2) 0.0485(8) Uani 1 d . . H45C H 0.8025(2) 0.26009(15) 1.0602(2) 0.058 Uiso 1 calc R . H45D H 0.7551(2) 0.30868(15) 0.9963(2) 0.058 Uiso 1 calc R . C46 C 0.8735(2) 0.27864(14) 1.0018(2) 0.0507(8) Uani 1 d . . H46A H 0.9136(2) 0.30459(14) 1.0413(2) 0.061 Uiso 1 calc R . H46B H 0.8622(2) 0.30187(14) 0.9573(2) 0.061 Uiso 1 calc R . N47 N 0.82184(14) 0.14443(10) 0.88593(11) 0.0290(4) Uani 1 d . . H47A H 0.84521(14) 0.10728(10) 0.87785(11) 0.035 Uiso 1 calc R . H47B H 0.76457(14) 0.14619(10) 0.85487(11) 0.035 Uiso 1 calc R . C47 C 0.8696(2) 0.19970(12) 0.87396(14) 0.0321(5) Uani 1 d . . H47C H 0.8309(2) 0.23722(12) 0.85911(14) 0.039 Uiso 1 calc R . H47D H 0.8900(2) 0.18972(12) 0.83636(14) 0.039 Uiso 1 calc R . C48 C 0.9460(2) 0.21346(12) 0.9424(2) 0.0331(5) Uani 1 d . . H48A H 0.9902(2) 0.17965(12) 0.9522(2) 0.040 Uiso 1 calc R . H48B H 0.9728(2) 0.25448(12) 0.9389(2) 0.040 Uiso 1 calc R . N49 N 0.91516(14) 0.21624(9) 1.00027(12) 0.0293(4) Uani 1 d . . C50 C 0.6383(2) -0.05680(13) 1.1166(2) 0.0431(7) Uani 1 d . . C51 C 0.5799(3) -0.0893(2) 1.0476(2) 0.0601(11) Uani 1 d . . H51A H 0.5484(3) -0.1243(2) 1.0580(2) 0.090 Uiso 1 calc R . H51B H 0.6156(3) -0.1060(2) 1.0239(2) 0.090 Uiso 1 calc R . H51C H 0.5384(3) -0.0584(2) 1.0168(2) 0.090 Uiso 1 calc R . C52 C 0.7051(3) -0.1054(2) 1.1645(2) 0.0640(12) Uani 1 d . . H52A H 0.6744(3) -0.1414(2) 1.1740(2) 0.096 Uiso 1 calc R . H52B H 0.7417(3) -0.0850(2) 1.2091(2) 0.096 Uiso 1 calc R . H52C H 0.7414(3) -0.1207(2) 1.1407(2) 0.096 Uiso 1 calc R . C53 C 0.5813(3) -0.0329(2) 1.1542(2) 0.0556(10) Uani 1 d . . H53A H 0.5493(3) -0.0686(2) 1.1625(2) 0.083 Uiso 1 calc R . H53B H 0.5402(3) -0.0011(2) 1.1246(2) 0.083 Uiso 1 calc R . H53C H 0.6182(3) -0.0136(2) 1.1995(2) 0.083 Uiso 1 calc R . C54 C 0.8416(2) 0.12882(13) 1.22415(12) 0.0291(5) Uani 1 d . . C55 C 0.8258(2) 0.1080(2) 1.28914(15) 0.0465(7) Uani 1 d . . H55A H 0.8600(2) 0.1347(2) 1.32952(15) 0.070 Uiso 1 calc R . H55B H 0.8432(2) 0.0635(2) 1.30002(15) 0.070 Uiso 1 calc R . H55C H 0.7640(2) 0.1124(2) 1.27937(15) 0.070 Uiso 1 calc R . C56 C 0.8167(2) 0.19941(15) 1.2097(2) 0.0433(7) Uani 1 d . . H56A H 0.8508(2) 0.22461(15) 1.2515(2) 0.065 Uiso 1 calc R . H56B H 0.7548(2) 0.20457(15) 1.1991(2) 0.065 Uiso 1 calc R . H56C H 0.8285(2) 0.21396(15) 1.1695(2) 0.065 Uiso 1 calc R . C57 C 0.9393(2) 0.12200(13) 1.24165(14) 0.0329(5) Uani 1 d . . H57A H 0.9724(2) 0.14813(13) 1.28292(14) 0.049 Uiso 1 calc R . H57B H 0.9512(2) 0.13614(13) 1.20124(14) 0.049 Uiso 1 calc R . H57C H 0.9564(2) 0.07739(13) 1.25193(14) 0.049 Uiso 1 calc R . Cl1 Cl 0.45545(4) 0.09593(2) 0.42744(3) 0.02659(11) Uani 1 d . . O10 O 0.4849(2) 0.04238(11) 0.4005(2) 0.0575(7) Uani 1 d . . O11 O 0.3871(2) 0.12762(12) 0.37082(12) 0.0524(6) Uani 1 d . . O12 O 0.4207(2) 0.07500(11) 0.47693(12) 0.0490(6) Uani 1 d . . O13 O 0.52570(12) 0.13918(9) 0.46249(13) 0.0398(5) Uani 1 d . . Cl2 Cl 0.52166(4) 0.44570(3) 0.37928(3) 0.03124(13) Uani 1 d . . O20 O 0.4301(2) 0.45544(12) 0.35655(13) 0.0525(6) Uani 1 d . . O21 O 0.5365(2) 0.38643(10) 0.35217(11) 0.0495(6) Uani 1 d . . O22 O 0.5560(2) 0.49774(11) 0.35482(12) 0.0522(6) Uani 1 d . . O23 O 0.5600(2) 0.44362(10) 0.45553(10) 0.0445(5) Uani 1 d . . Cl4 Cl 0.47761(4) -0.36211(3) 1.01704(3) 0.03243(13) Uani 1 d . . O40 O 0.4735(2) -0.35585(11) 0.94709(12) 0.0480(5) Uani 1 d . . O41 O 0.5308(2) -0.31269(10) 1.06048(13) 0.0537(6) Uani 1 d . . O42 O 0.5129(2) -0.42317(11) 1.04508(14) 0.0596(7) Uani 1 d . . O43 O 0.3927(2) -0.3573(2) 1.0169(2) 0.0659(8) Uani 1 d . . Cl5 Cl 0.62700(5) 0.23661(4) 0.74736(4) 0.0427(2) Uani 1 d . . O50 O 0.6362(2) 0.2947(2) 0.7132(2) 0.0749(9) Uani 1 d . . O51 O 0.5376(2) 0.2201(2) 0.7214(2) 0.0933(13) Uani 1 d . . O52 O 0.6565(2) 0.2550(2) 0.8193(2) 0.0872(11) Uani 1 d . . O53 O 0.6847(2) 0.1897(2) 0.7418(2) 0.0927(12) Uani 1 d . . O70 O 0.5046(3) -0.2135(2) 1.1393(2) 0.1151(15) Uani 1 d . . C80X C 0.4093(2) -0.1910(2) 0.9482(2) 0.0544(9) Uani 0.503(5) d P 2 H80A H 0.3782(32) -0.1641(17) 0.9070(8) 0.082 Uiso 0.503(5) calc PR 2 H80B H 0.3880(35) -0.2347(10) 0.9380(20) 0.082 Uiso 0.503(5) calc PR 2 H80C H 0.4715(4) -0.1900(27) 0.9588(12) 0.082 Uiso 0.503(5) calc PR 2 O80X O 0.3946(3) -0.1673(3) 1.0086(3) 0.0471(8) Uani 0.503(5) d PD 2 H80X H 0.3673(54) -0.1947(19) 1.0212(31) 0.071 Uiso 0.503(5) calc PR 2 C80 C 0.4093(2) -0.1910(2) 0.9482(2) 0.0544(9) Uani 0.497(5) d PD 1 H80D H 0.3695(17) -0.2227(10) 0.9172(4) 0.082 Uiso 0.497(5) calc PR 1 H80E H 0.4668(30) -0.1962(16) 0.9474(4) 0.082 Uiso 0.497(5) calc PR 1 H80F H 0.3874(54) -0.1482(6) 0.9316(7) 0.082 Uiso 0.497(5) calc PR 1 O80 O 0.4153(3) -0.1993(3) 1.0183(3) 0.0471(8) Uani 0.497(5) d PD 1 H80 H 0.4412(53) -0.2335(22) 1.0347(18) 0.071 Uiso 0.497(5) calc PR 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02088(14) 0.01626(13) 0.01464(13) 0.00357(9) 0.00503(10) 0.00246(10) Fe2 0.0254(2) 0.02270(15) 0.02149(15) 0.00453(11) 0.00748(12) -0.00810(11) N2 0.0212(8) 0.0163(7) 0.0168(7) 0.0022(6) 0.0068(6) 0.0026(6) O1 0.0213(7) 0.0177(6) 0.0170(6) 0.0031(5) 0.0046(5) -0.0004(5) C1 0.0166(8) 0.0188(8) 0.0172(8) 0.0032(7) 0.0064(7) 0.0007(6) C2 0.0173(8) 0.0181(8) 0.0166(8) 0.0032(6) 0.0069(7) 0.0024(6) C3 0.0202(9) 0.0217(9) 0.0157(8) 0.0030(7) 0.0067(7) 0.0032(7) C4 0.0203(9) 0.0230(9) 0.0165(8) 0.0045(7) 0.0083(7) 0.0052(7) C5 0.0222(9) 0.0183(8) 0.0197(9) 0.0044(7) 0.0091(8) 0.0032(7) C6 0.0176(8) 0.0179(8) 0.0198(9) 0.0029(7) 0.0086(7) 0.0006(7) C7 0.0305(11) 0.0179(8) 0.0158(8) 0.0032(7) 0.0073(8) 0.0044(7) C8 0.0367(14) 0.058(2) 0.0260(12) -0.0113(11) 0.0096(11) 0.0128(12) C9 0.059(2) 0.068(2) 0.0309(14) -0.0176(14) 0.0073(14) 0.030(2) C10 0.095(3) 0.0269(12) 0.0259(12) 0.0014(10) 0.021(2) 0.0187(15) C11 0.073(2) 0.0344(13) 0.0298(13) -0.0048(10) 0.0225(14) -0.0203(14) C12 0.0425(14) 0.0364(13) 0.0314(12) -0.0089(10) 0.0195(11) -0.0106(11) N13 0.0247(9) 0.0338(10) 0.0247(9) 0.0070(8) 0.0089(8) 0.0066(8) C13 0.0247(11) 0.052(2) 0.0295(12) 0.0121(11) 0.0018(10) 0.0016(11) C14 0.0305(12) 0.0409(13) 0.0200(10) 0.0029(9) 0.0004(9) -0.0060(10) N15 0.0349(10) 0.0175(8) 0.0217(9) 0.0040(6) 0.0096(8) 0.0046(7) C15 0.050(2) 0.0234(10) 0.0229(11) 0.0074(8) 0.0077(10) 0.0098(10) C16 0.0439(14) 0.0248(10) 0.0207(10) 0.0075(8) 0.0101(10) 0.0045(9) N17 0.0245(9) 0.0203(8) 0.0236(9) 0.0004(6) 0.0103(7) -0.0023(6) C17 0.0370(13) 0.0368(12) 0.0270(11) -0.0010(9) 0.0178(10) 0.0003(10) C18 0.0407(13) 0.0254(10) 0.0194(10) -0.0011(8) 0.0111(9) 0.0015(9) N19 0.0313(10) 0.0229(8) 0.0169(8) 0.0031(6) 0.0072(7) 0.0006(7) C20 0.0275(10) 0.0274(10) 0.0166(9) 0.0059(7) 0.0086(8) 0.0102(8) C21 0.050(2) 0.0349(13) 0.0255(11) 0.0125(10) 0.0181(11) 0.0067(11) C22 0.0300(12) 0.0489(15) 0.0246(11) 0.0053(10) 0.0088(10) 0.0180(11) C23 0.0361(13) 0.0349(12) 0.0180(10) 0.0023(8) 0.0041(9) 0.0115(10) C24 0.0258(10) 0.0169(8) 0.0234(10) 0.0000(7) 0.0094(8) 0.0000(7) C25 0.052(2) 0.0294(12) 0.0288(12) -0.0021(9) 0.0224(12) 0.0036(11) C26 0.0387(13) 0.0172(9) 0.0332(12) 0.0003(8) 0.0093(10) 0.0023(9) C27 0.0247(11) 0.0268(11) 0.0376(13) -0.0028(9) 0.0043(10) -0.0048(9) O31 0.0288(8) 0.0273(8) 0.0221(7) 0.0023(6) 0.0076(6) -0.0070(6) C31 0.0238(10) 0.0232(9) 0.0218(9) 0.0049(7) 0.0083(8) 0.0004(8) N32 0.0319(10) 0.0323(10) 0.0189(8) 0.0023(7) 0.0077(8) -0.0153(8) C32 0.0271(10) 0.0248(10) 0.0205(9) 0.0044(8) 0.0093(8) -0.0043(8) C33 0.0325(12) 0.0231(10) 0.0311(11) 0.0028(8) 0.0177(10) -0.0053(8) C34 0.0374(13) 0.0217(10) 0.0377(13) 0.0059(9) 0.0255(11) 0.0015(9) C35 0.0338(12) 0.0304(11) 0.0274(11) 0.0091(9) 0.0191(10) 0.0076(9) C36 0.0257(10) 0.0286(10) 0.0212(10) 0.0047(8) 0.0094(8) 0.0075(8) C37 0.0394(13) 0.0451(14) 0.0189(10) -0.0005(9) 0.0122(10) -0.0259(11) C38 0.0266(14) 0.109(3) 0.034(2) -0.020(2) 0.0063(12) -0.004(2) C39 0.037(2) 0.135(4) 0.034(2) -0.028(2) 0.0038(14) -0.015(2) C40 0.065(2) 0.078(2) 0.0249(13) -0.0142(14) 0.0211(14) -0.046(2) C41 0.104(3) 0.0299(14) 0.036(2) -0.0057(12) 0.013(2) -0.024(2) C42 0.093(3) 0.0240(12) 0.0296(14) 0.0018(10) -0.004(2) -0.0113(14) N43 0.0368(11) 0.0229(9) 0.0271(10) 0.0018(7) 0.0072(8) -0.0001(8) C43 0.0313(13) 0.0437(15) 0.0320(13) -0.0025(11) 0.0027(10) -0.0022(11) C44 0.0359(14) 0.0433(15) 0.0426(15) -0.0159(12) 0.0155(12) -0.0179(12) N45 0.0309(11) 0.0484(13) 0.0396(12) 0.0191(10) 0.0182(10) 0.0075(10) C45 0.055(2) 0.0353(14) 0.066(2) 0.0073(14) 0.036(2) 0.0113(13) C46 0.059(2) 0.0251(12) 0.086(3) -0.0065(14) 0.048(2) -0.0022(12) N47 0.0292(10) 0.0333(10) 0.0231(9) 0.0075(8) 0.0091(8) -0.0089(8) C47 0.0322(12) 0.0305(11) 0.0379(13) 0.0146(10) 0.0184(10) -0.0019(9) C48 0.0337(12) 0.0239(10) 0.0489(15) 0.0029(10) 0.0241(12) -0.0051(9) N49 0.0314(10) 0.0191(8) 0.0433(12) -0.0047(8) 0.0210(9) -0.0076(7) C50 0.073(2) 0.0248(11) 0.058(2) -0.0008(11) 0.054(2) -0.0083(12) C51 0.095(3) 0.040(2) 0.075(2) -0.020(2) 0.066(2) -0.039(2) C52 0.127(4) 0.0304(14) 0.064(2) 0.0164(14) 0.069(3) 0.013(2) C53 0.075(2) 0.045(2) 0.078(2) -0.011(2) 0.064(2) -0.018(2) C54 0.0260(11) 0.0377(12) 0.0208(10) 0.0018(9) 0.0066(8) 0.0070(9) C55 0.040(2) 0.076(2) 0.0241(12) -0.0029(13) 0.0137(11) -0.0005(15) C56 0.043(2) 0.0420(15) 0.0334(13) -0.0080(11) 0.0036(12) 0.0172(12) C57 0.0270(11) 0.0395(13) 0.0271(11) 0.0005(10) 0.0054(9) 0.0082(10) Cl1 0.0255(2) 0.0204(2) 0.0356(3) -0.0012(2) 0.0140(2) 0.0001(2) O10 0.062(2) 0.0319(11) 0.088(2) -0.0172(11) 0.0401(15) 0.0020(10) O11 0.0496(13) 0.0587(14) 0.0358(11) 0.0006(10) 0.0035(10) 0.0116(11) O12 0.068(2) 0.0424(11) 0.0484(12) -0.0077(9) 0.0358(12) -0.0254(11) O13 0.0245(8) 0.0249(8) 0.0686(14) -0.0043(8) 0.0170(9) -0.0027(7) Cl2 0.0478(3) 0.0200(2) 0.0196(2) 0.0011(2) 0.0067(2) -0.0036(2) O20 0.0542(14) 0.0485(13) 0.0505(14) 0.0147(10) 0.0166(11) 0.0078(10) O21 0.080(2) 0.0276(9) 0.0317(10) -0.0050(8) 0.0132(11) 0.0084(10) O22 0.078(2) 0.0359(11) 0.0444(12) 0.0062(9) 0.0259(12) -0.0168(11) O23 0.0669(14) 0.0365(10) 0.0207(8) -0.0007(7) 0.0077(9) 0.0040(10) Cl4 0.0370(3) 0.0314(3) 0.0306(3) -0.0059(2) 0.0154(2) -0.0072(2) O40 0.0587(14) 0.0556(13) 0.0385(11) -0.0048(10) 0.0288(11) -0.0070(11) O41 0.068(2) 0.0333(11) 0.0463(13) -0.0097(9) 0.0090(11) -0.0159(10) O42 0.087(2) 0.0283(10) 0.059(2) -0.0040(10) 0.0242(14) -0.0008(11) O43 0.0496(14) 0.100(2) 0.063(2) -0.0019(15) 0.0384(13) -0.0101(14) Cl5 0.0408(4) 0.0533(4) 0.0275(3) 0.0063(3) 0.0069(3) 0.0133(3) O50 0.059(2) 0.075(2) 0.074(2) 0.032(2) 0.0102(14) -0.0063(14) O51 0.053(2) 0.081(2) 0.107(3) 0.041(2) -0.009(2) -0.020(2) O52 0.098(2) 0.112(3) 0.0400(14) -0.003(2) 0.015(2) 0.042(2) O53 0.096(3) 0.079(2) 0.080(2) -0.029(2) 0.011(2) 0.036(2) O70 0.154(4) 0.097(3) 0.106(3) 0.005(2) 0.065(3) -0.021(3) C80X 0.039(2) 0.080(3) 0.040(2) 0.010(2) 0.0122(13) 0.013(2) O80X 0.040(2) 0.052(2) 0.060(2) 0.018(2) 0.030(2) 0.009(2) C80 0.039(2) 0.080(3) 0.040(2) 0.010(2) 0.0122(13) 0.013(2) O80 0.040(2) 0.052(2) 0.060(2) 0.018(2) 0.030(2) 0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 1.859(2) . ? Fe1 O1 1.9100(15) . ? Fe1 N15 2.007(2) . ? Fe1 N17 2.009(2) . ? Fe1 N19 2.009(2) . ? Fe1 N13 2.012(2) . ? Fe2 N32 1.849(2) . ? Fe2 O31 1.927(2) . ? Fe2 N45 1.987(2) . ? Fe2 N43 1.998(2) . ? Fe2 N47 2.002(2) . ? Fe2 N49 2.010(2) . ? N2 C2 1.345(2) . ? N2 C7 1.436(3) . ? O1 C1 1.296(2) . ? C1 C6 1.431(3) . ? C1 C2 1.442(3) . ? C2 C3 1.425(3) . ? C3 C4 1.371(3) . ? C4 C5 1.443(3) . ? C4 C20 1.531(3) . ? C5 C6 1.373(3) . ? C6 C24 1.525(3) . ? C7 C12 1.375(4) . ? C7 C8 1.392(4) . ? C8 C9 1.382(4) . ? C9 C10 1.352(6) . ? C10 C11 1.383(5) . ? C11 C12 1.405(4) . ? N13 C13 1.497(3) . ? C13 C14 1.510(4) . ? C14 N19 1.492(3) . ? N15 C15 1.487(3) . ? C15 C16 1.518(4) . ? C16 N19 1.508(3) . ? N17 C17 1.494(3) . ? C17 C18 1.516(4) . ? C18 N19 1.490(3) . ? C20 C23 1.532(3) . ? C20 C22 1.540(3) . ? C20 C21 1.540(4) . ? C24 C26 1.533(3) . ? C24 C25 1.539(3) . ? C24 C27 1.540(3) . ? O31 C31 1.289(3) . ? C31 C36 1.436(3) . ? C31 C32 1.442(3) . ? N32 C32 1.343(3) . ? N32 C37 1.440(3) . ? C32 C33 1.419(3) . ? C33 C34 1.364(3) . ? C34 C35 1.435(4) . ? C34 C50 1.529(3) . ? C35 C36 1.369(3) . ? C36 C54 1.529(3) . ? C37 C42 1.364(5) . ? C37 C38 1.396(5) . ? C38 C39 1.398(5) . ? C39 C40 1.382(7) . ? C40 C41 1.372(6) . ? C41 C42 1.395(4) . ? N43 C43 1.499(3) . ? C43 C44 1.522(4) . ? C44 N49 1.486(4) . ? N45 C45 1.475(5) . ? C45 C46 1.483(4) . ? C46 N49 1.494(3) . ? N47 C47 1.489(3) . ? C47 C48 1.511(4) . ? C48 N49 1.483(3) . ? C50 C51 1.531(5) . ? C50 C53 1.542(4) . ? C50 C52 1.549(5) . ? C54 C55 1.535(4) . ? C54 C56 1.540(4) . ? C54 C57 1.541(3) . ? Cl1 O10 1.431(2) . ? Cl1 O11 1.435(2) . ? Cl1 O12 1.437(2) . ? Cl1 O13 1.437(2) . ? Cl2 O22 1.423(2) . ? Cl2 O21 1.430(2) . ? Cl2 O20 1.434(3) . ? Cl2 O23 1.446(2) . ? Cl4 O40 1.426(2) . ? Cl4 O41 1.430(2) . ? Cl4 O43 1.431(3) . ? Cl4 O42 1.437(2) . ? Cl5 O52 1.420(3) . ? Cl5 O53 1.421(3) . ? Cl5 O51 1.423(3) . ? Cl5 O50 1.452(3) . ? C80X O80X 1.455(6) . ? C80 O80 1.422(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 O1 83.13(7) . . ? N2 Fe1 N15 97.83(8) . . ? O1 Fe1 N15 178.80(7) . . ? N2 Fe1 N17 92.56(8) . . ? O1 Fe1 N17 86.58(7) . . ? N15 Fe1 N17 92.64(8) . . ? N2 Fe1 N19 175.20(8) . . ? O1 Fe1 N19 93.28(7) . . ? N15 Fe1 N19 85.73(8) . . ? N17 Fe1 N19 84.03(8) . . ? N2 Fe1 N13 98.52(8) . . ? O1 Fe1 N13 89.64(8) . . ? N15 Fe1 N13 90.93(9) . . ? N17 Fe1 N13 167.78(8) . . ? N19 Fe1 N13 84.59(8) . . ? N32 Fe2 O31 83.05(8) . . ? N32 Fe2 N45 99.01(11) . . ? O31 Fe2 N45 87.89(9) . . ? N32 Fe2 N43 95.77(10) . . ? O31 Fe2 N43 85.62(9) . . ? N45 Fe2 N43 163.00(10) . . ? N32 Fe2 N47 96.30(8) . . ? O31 Fe2 N47 179.34(7) . . ? N45 Fe2 N47 92.34(10) . . ? N43 Fe2 N47 94.33(9) . . ? N32 Fe2 N49 177.25(10) . . ? O31 Fe2 N49 95.53(8) . . ? N45 Fe2 N49 83.25(10) . . ? N43 Fe2 N49 81.76(9) . . ? N47 Fe2 N49 85.12(9) . . ? C2 N2 C7 121.2(2) . . ? C2 N2 Fe1 114.59(14) . . ? C7 N2 Fe1 124.21(13) . . ? C1 O1 Fe1 112.70(13) . . ? O1 C1 C6 124.1(2) . . ? O1 C1 C2 115.5(2) . . ? C6 C1 C2 120.3(2) . . ? N2 C2 C3 127.1(2) . . ? N2 C2 C1 111.8(2) . . ? C3 C2 C1 121.1(2) . . ? C4 C3 C2 118.6(2) . . ? C3 C4 C5 119.1(2) . . ? C3 C4 C20 122.7(2) . . ? C5 C4 C20 118.2(2) . . ? C6 C5 C4 125.1(2) . . ? C5 C6 C1 115.7(2) . . ? C5 C6 C24 123.9(2) . . ? C1 C6 C24 120.4(2) . . ? C12 C7 C8 120.1(2) . . ? C12 C7 N2 121.2(2) . . ? C8 C7 N2 118.5(2) . . ? C9 C8 C7 119.8(3) . . ? C10 C9 C8 120.3(3) . . ? C9 C10 C11 121.0(3) . . ? C10 C11 C12 119.4(3) . . ? C7 C12 C11 119.3(3) . . ? C13 N13 Fe1 111.3(2) . . ? N13 C13 C14 108.4(2) . . ? N19 C14 C13 109.2(2) . . ? C15 N15 Fe1 109.43(15) . . ? N15 C15 C16 109.4(2) . . ? N19 C16 C15 111.4(2) . . ? C17 N17 Fe1 112.26(15) . . ? N17 C17 C18 108.8(2) . . ? N19 C18 C17 109.0(2) . . ? C18 N19 C14 111.3(2) . . ? C18 N19 C16 109.7(2) . . ? C14 N19 C16 112.9(2) . . ? C18 N19 Fe1 107.28(14) . . ? C14 N19 Fe1 105.13(14) . . ? C16 N19 Fe1 110.24(14) . . ? C4 C20 C23 111.7(2) . . ? C4 C20 C22 108.2(2) . . ? C23 C20 C22 109.2(2) . . ? C4 C20 C21 110.3(2) . . ? C23 C20 C21 109.1(2) . . ? C22 C20 C21 108.3(2) . . ? C6 C24 C26 111.4(2) . . ? C6 C24 C25 110.7(2) . . ? C26 C24 C25 107.3(2) . . ? C6 C24 C27 108.8(2) . . ? C26 C24 C27 108.7(2) . . ? C25 C24 C27 109.9(2) . . ? C31 O31 Fe2 113.28(14) . . ? O31 C31 C36 124.0(2) . . ? O31 C31 C32 115.8(2) . . ? C36 C31 C32 120.1(2) . . ? C32 N32 C37 119.7(2) . . ? C32 N32 Fe2 116.0(2) . . ? C37 N32 Fe2 124.12(15) . . ? N32 C32 C33 127.1(2) . . ? N32 C32 C31 111.8(2) . . ? C33 C32 C31 121.1(2) . . ? C34 C33 C32 118.7(2) . . ? C33 C34 C35 119.2(2) . . ? C33 C34 C50 123.0(2) . . ? C35 C34 C50 117.7(2) . . ? C36 C35 C34 125.5(2) . . ? C35 C36 C31 115.3(2) . . ? C35 C36 C54 123.5(2) . . ? C31 C36 C54 121.2(2) . . ? C42 C37 C38 121.2(3) . . ? C42 C37 N32 119.9(3) . . ? C38 C37 N32 118.7(3) . . ? C37 C38 C39 117.7(4) . . ? C40 C39 C38 121.2(4) . . ? C41 C40 C39 119.8(3) . . ? C40 C41 C42 119.8(4) . . ? C37 C42 C41 120.2(3) . . ? C43 N43 Fe2 110.8(2) . . ? N43 C43 C44 110.7(2) . . ? N49 C44 C43 109.0(2) . . ? C45 N45 Fe2 106.9(2) . . ? N45 C45 C46 107.2(3) . . ? C45 C46 N49 111.1(2) . . ? C47 N47 Fe2 110.2(2) . . ? N47 C47 C48 107.9(2) . . ? N49 C48 C47 108.8(2) . . ? C48 N49 C44 111.2(2) . . ? C48 N49 C46 111.7(2) . . ? C44 N49 C46 110.9(2) . . ? C48 N49 Fe2 107.72(15) . . ? C44 N49 Fe2 104.8(2) . . ? C46 N49 Fe2 110.2(2) . . ? C34 C50 C51 111.5(2) . . ? C34 C50 C53 110.4(2) . . ? C51 C50 C53 108.6(3) . . ? C34 C50 C52 107.6(3) . . ? C51 C50 C52 109.3(3) . . ? C53 C50 C52 109.3(3) . . ? C36 C54 C55 111.2(2) . . ? C36 C54 C56 110.7(2) . . ? C55 C54 C56 108.4(2) . . ? C36 C54 C57 109.9(2) . . ? C55 C54 C57 108.1(2) . . ? C56 C54 C57 108.5(2) . . ? O10 Cl1 O11 109.7(2) . . ? O10 Cl1 O12 109.8(2) . . ? O11 Cl1 O12 107.6(2) . . ? O10 Cl1 O13 110.63(14) . . ? O11 Cl1 O13 110.20(14) . . ? O12 Cl1 O13 108.79(14) . . ? O22 Cl2 O21 111.9(2) . . ? O22 Cl2 O20 108.0(2) . . ? O21 Cl2 O20 109.3(2) . . ? O22 Cl2 O23 110.11(14) . . ? O21 Cl2 O23 109.25(13) . . ? O20 Cl2 O23 108.3(2) . . ? O40 Cl4 O41 109.51(15) . . ? O40 Cl4 O43 110.3(2) . . ? O41 Cl4 O43 108.9(2) . . ? O40 Cl4 O42 109.7(2) . . ? O41 Cl4 O42 110.1(2) . . ? O43 Cl4 O42 108.4(2) . . ? O52 Cl5 O53 108.1(2) . . ? O52 Cl5 O51 109.5(3) . . ? O53 Cl5 O51 117.0(2) . . ? O52 Cl5 O50 102.7(2) . . ? O53 Cl5 O50 109.6(2) . . ? O51 Cl5 O50 109.0(2) . . ? _refine_diff_density_max 1.341 _refine_diff_density_min -0.891 _refine_diff_density_rms 0.089 #===END