# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_j11001_H2LNMe(H2O) _database_code_depnum_ccdc_archive 'CCDC 895814' #TrackingRef 'combined_CIF.cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H37 N5 O3' _chemical_formula_sum 'C40 H37 N5 O3' _chemical_formula_weight 635.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.1353(7) _cell_length_b 14.7940(10) _cell_length_c 18.6824(13) _cell_angle_alpha 68.452(6) _cell_angle_beta 80.755(5) _cell_angle_gamma 82.839(5) _cell_volume 3324.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8036 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.90166 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1042 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 57357 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.48 _reflns_number_total 14984 _reflns_number_gt 10735 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen et al., 2004)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One water molecule is bound to each macrocycle. Protons of the water could not be located and are thus not present in the structure. However they are included in the UNIT instruction. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+1.4687P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14984 _refine_ls_number_parameters 867 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0821 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1322 _refine_ls_wR_factor_gt 0.1171 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C101 C 0.91809(14) 0.02116(13) 0.88190(10) 0.0286(4) Uani 1 1 d . . . H101 H 0.8656 -0.0184 0.9154 0.034 Uiso 1 1 calc R . . C102 C 0.88959(13) 0.11976(13) 0.83540(10) 0.0259(4) Uani 1 1 d . . . C103 C 0.79457(14) 0.17185(13) 0.83525(11) 0.0297(4) Uani 1 1 d . . . H103 H 0.7320 0.1477 0.8659 0.036 Uiso 1 1 calc R . . C104 C 0.80715(13) 0.26697(13) 0.78160(10) 0.0270(4) Uani 1 1 d . . . H104 H 0.7549 0.3189 0.7698 0.032 Uiso 1 1 calc R . . C105 C 0.90939(13) 0.27081(12) 0.74928(10) 0.0231(4) Uani 1 1 d . . . C106 C 0.96274(13) 0.35033(12) 0.68137(10) 0.0239(4) Uani 1 1 d . . . C107 C 0.95775(13) 0.33373(14) 0.60554(10) 0.0278(4) Uani 1 1 d . . . C108 C 0.99853(14) 0.25482(15) 0.58408(11) 0.0342(4) Uani 1 1 d . . . H108 H 1.0335 0.2001 0.6188 0.041 Uiso 1 1 calc R . . C109 C 0.98683(17) 0.25799(18) 0.51023(13) 0.0466(6) Uani 1 1 d . . . H109 H 1.0150 0.2053 0.4940 0.056 Uiso 1 1 calc R . . C110 C 0.93409(18) 0.3378(2) 0.46021(13) 0.0515(6) Uani 1 1 d . . . H110 H 0.9278 0.3392 0.4099 0.062 Uiso 1 1 calc R . . C111 C 0.89081(17) 0.41489(18) 0.48250(12) 0.0454(6) Uani 1 1 d . . . H111 H 0.8534 0.4681 0.4484 0.054 Uiso 1 1 calc R . . C112 C 0.90278(14) 0.41350(14) 0.55543(11) 0.0326(4) Uani 1 1 d . . . C113 C 0.86714(13) 0.48427(13) 0.59386(11) 0.0309(4) Uani 1 1 d . . . C114 C 0.80786(15) 0.57316(15) 0.56920(13) 0.0427(5) Uani 1 1 d . . . H114 H 0.7835 0.5965 0.5199 0.051 Uiso 1 1 calc R . . C115 C 0.78540(16) 0.62629(15) 0.61771(15) 0.0485(6) Uani 1 1 d . . . H115 H 0.7455 0.6868 0.6013 0.058 Uiso 1 1 calc R . . C116 C 0.81993(16) 0.59312(15) 0.68975(14) 0.0457(6) Uani 1 1 d . . . H116 H 0.8045 0.6313 0.7219 0.055 Uiso 1 1 calc R . . C117 C 0.87755(15) 0.50337(13) 0.71539(12) 0.0354(4) Uani 1 1 d . . . H117 H 0.9003 0.4796 0.7652 0.042 Uiso 1 1 calc R . . C118 C 0.90078(13) 0.44991(13) 0.66681(11) 0.0277(4) Uani 1 1 d . . . C119 C 1.07373(13) 0.35752(12) 0.69152(10) 0.0233(4) Uani 1 1 d . . . C120 C 1.11278(14) 0.39198(15) 0.73996(12) 0.0338(4) Uani 1 1 d . . . H120 H 1.0736 0.4137 0.7787 0.041 Uiso 1 1 calc R . . C121 C 1.22085(14) 0.38935(14) 0.72185(11) 0.0329(4) Uani 1 1 d . . . H121 H 1.2677 0.4091 0.7462 0.039 Uiso 1 1 calc R . . C122 C 1.24693(13) 0.35312(12) 0.66261(11) 0.0262(4) Uani 1 1 d . . . C123 C 1.34435(13) 0.33858(12) 0.61958(10) 0.0262(4) Uani 1 1 d . . . H123 H 1.4049 0.3596 0.6287 0.031 Uiso 1 1 calc R . . C124 C 1.44848(13) 0.29274(13) 0.52464(10) 0.0261(4) Uani 1 1 d . . . C125 C 1.50311(15) 0.37534(14) 0.48414(11) 0.0338(4) Uani 1 1 d . . . H125 H 1.4765 0.4359 0.4889 0.041 Uiso 1 1 calc R . . C126 C 1.59523(16) 0.37130(16) 0.43713(12) 0.0400(5) Uani 1 1 d . . . H126 H 1.6318 0.4282 0.4106 0.048 Uiso 1 1 calc R . . C127 C 1.63347(16) 0.28372(16) 0.42912(12) 0.0414(5) Uani 1 1 d . . . H127 H 1.6963 0.2803 0.3967 0.050 Uiso 1 1 calc R . . C128 C 1.57993(15) 0.20060(15) 0.46855(11) 0.0366(5) Uani 1 1 d . . . H128 H 1.6065 0.1406 0.4627 0.044 Uiso 1 1 calc R . . C129 C 1.48836(14) 0.20436(13) 0.51619(10) 0.0291(4) Uani 1 1 d . . . C130 C 1.42443(16) 0.08434(14) 0.63670(11) 0.0366(5) Uani 1 1 d . . . H13A H 1.3747 0.1292 0.6555 0.044 Uiso 1 1 calc R . . H13B H 1.4913 0.0814 0.6558 0.044 Uiso 1 1 calc R . . C131 C 1.38449(15) -0.01571(14) 0.66696(12) 0.0340(4) Uani 1 1 d . . . H13C H 1.4199 -0.0523 0.6339 0.041 Uiso 1 1 calc R . . H13D H 1.4033 -0.0505 0.7200 0.041 Uiso 1 1 calc R . . C132 C 1.23718(17) 0.03312(17) 0.59275(13) 0.0456(5) Uani 1 1 d . . . H13E H 1.2529 0.1017 0.5734 0.068 Uiso 1 1 calc R . . H13F H 1.1624 0.0291 0.5970 0.068 Uiso 1 1 calc R . . H13G H 1.2729 0.0019 0.5567 0.068 Uiso 1 1 calc R . . C133 C 1.24253(16) -0.11856(14) 0.70110(12) 0.0366(5) Uani 1 1 d . . . H13H H 1.2935 -0.1576 0.6771 0.044 Uiso 1 1 calc R . . H13I H 1.1745 -0.1196 0.6851 0.044 Uiso 1 1 calc R . . C134 C 1.23557(15) -0.16748(13) 0.78819(12) 0.0331(4) Uani 1 1 d . . . H13J H 1.2316 -0.2386 0.8032 0.040 Uiso 1 1 calc R . . H13K H 1.2973 -0.1563 0.8071 0.040 Uiso 1 1 calc R . . C135 C 1.10910(13) -0.16972(12) 0.89817(10) 0.0265(4) Uani 1 1 d . . . C136 C 1.13883(14) -0.26395(13) 0.94437(12) 0.0319(4) Uani 1 1 d . . . H136 H 1.1865 -0.3038 0.9229 0.038 Uiso 1 1 calc R . . C137 C 1.09859(16) -0.29961(14) 1.02205(12) 0.0375(5) Uani 1 1 d . . . H137 H 1.1195 -0.3638 1.0537 0.045 Uiso 1 1 calc R . . C138 C 1.02875(17) -0.24309(15) 1.05384(12) 0.0389(5) Uani 1 1 d . . . H138 H 1.0021 -0.2679 1.1072 0.047 Uiso 1 1 calc R . . C139 C 0.99719(16) -0.14914(14) 1.00728(11) 0.0337(4) Uani 1 1 d . . . H139 H 0.9488 -0.1102 1.0292 0.040 Uiso 1 1 calc R . . C140 C 1.03580(14) -0.11193(12) 0.92924(10) 0.0270(4) Uani 1 1 d . . . C201 C 0.41771(14) 0.10926(13) 0.82684(10) 0.0288(4) Uani 1 1 d . . . H201 H 0.3650 0.1609 0.8197 0.035 Uiso 1 1 calc R . . C202 C 0.39211(14) 0.01183(13) 0.87491(11) 0.0276(4) Uani 1 1 d . . . C203 C 0.30145(14) -0.02284(13) 0.92062(11) 0.0312(4) Uani 1 1 d . . . H203 H 0.2389 0.0151 0.9264 0.037 Uiso 1 1 calc R . . C204 C 0.31845(14) -0.12454(13) 0.95712(11) 0.0281(4) Uani 1 1 d . . . H204 H 0.2700 -0.1675 0.9925 0.034 Uiso 1 1 calc R . . C205 C 0.41851(13) -0.14986(12) 0.93189(10) 0.0246(4) Uani 1 1 d . . . C206 C 0.47815(13) -0.24793(12) 0.94336(10) 0.0249(4) Uani 1 1 d . . . C207 C 0.48599(13) -0.27436(12) 0.87014(11) 0.0261(4) Uani 1 1 d . . . C208 C 0.53398(14) -0.22645(13) 0.79600(11) 0.0306(4) Uani 1 1 d . . . H208 H 0.5687 -0.1693 0.7849 0.037 Uiso 1 1 calc R . . C209 C 0.53009(16) -0.26431(14) 0.73811(12) 0.0372(5) Uani 1 1 d . . . H209 H 0.5626 -0.2325 0.6871 0.045 Uiso 1 1 calc R . . C210 C 0.47937(17) -0.34770(15) 0.75420(12) 0.0407(5) Uani 1 1 d . . . H210 H 0.4771 -0.3721 0.7140 0.049 Uiso 1 1 calc R . . C211 C 0.43180(16) -0.39596(14) 0.82852(12) 0.0366(5) Uani 1 1 d . . . H211 H 0.3973 -0.4532 0.8394 0.044 Uiso 1 1 calc R . . C212 C 0.43553(13) -0.35922(12) 0.88665(11) 0.0275(4) Uani 1 1 d . . . C213 C 0.39426(13) -0.39514(12) 0.96897(11) 0.0268(4) Uani 1 1 d . . . C214 C 0.33910(14) -0.47646(13) 1.01298(12) 0.0332(4) Uani 1 1 d . . . H214 H 0.3215 -0.5187 0.9896 0.040 Uiso 1 1 calc R . . C215 C 0.31049(14) -0.49448(13) 1.09123(12) 0.0349(5) Uani 1 1 d . . . H215 H 0.2726 -0.5494 1.1218 0.042 Uiso 1 1 calc R . . C216 C 0.33650(14) -0.43305(13) 1.12568(12) 0.0334(4) Uani 1 1 d . . . H216 H 0.3175 -0.4472 1.1797 0.040 Uiso 1 1 calc R . . C217 C 0.39025(14) -0.35082(13) 1.08172(11) 0.0292(4) Uani 1 1 d . . . H217 H 0.4071 -0.3084 1.1052 0.035 Uiso 1 1 calc R . . C218 C 0.41848(13) -0.33225(12) 1.00344(11) 0.0255(4) Uani 1 1 d . . . C219 C 0.58375(13) -0.24611(12) 0.96566(10) 0.0259(4) Uani 1 1 d . . . C220 C 0.61231(15) -0.21656(16) 1.02089(12) 0.0371(5) Uani 1 1 d . . . H220 H 0.5672 -0.1887 1.0537 0.045 Uiso 1 1 calc R . . C221 C 0.71990(15) -0.23483(17) 1.02021(12) 0.0405(5) Uani 1 1 d . . . H221 H 0.7605 -0.2230 1.0532 0.049 Uiso 1 1 calc R . . C222 C 0.75589(14) -0.27306(14) 0.96296(11) 0.0314(4) Uani 1 1 d . . . C223 C 0.85742(14) -0.29708(14) 0.93028(11) 0.0320(4) Uani 1 1 d . . . H223 H 0.9159 -0.2999 0.9553 0.038 Uiso 1 1 calc R . . C224 C 0.96950(14) -0.33872(15) 0.83539(12) 0.0340(4) Uani 1 1 d . . . C225 C 1.02903(16) -0.42081(16) 0.87585(13) 0.0409(5) Uani 1 1 d . . . H225 H 1.0038 -0.4594 0.9273 0.049 Uiso 1 1 calc R . . C226 C 1.12496(17) -0.44753(16) 0.84229(14) 0.0452(5) Uani 1 1 d . . . H226 H 1.1651 -0.5034 0.8708 0.054 Uiso 1 1 calc R . . C227 C 1.16112(16) -0.39210(16) 0.76730(14) 0.0428(5) Uani 1 1 d . . . H227 H 1.2262 -0.4099 0.7437 0.051 Uiso 1 1 calc R . . C228 C 1.10256(15) -0.31059(15) 0.72654(13) 0.0378(5) Uani 1 1 d . . . H228 H 1.1281 -0.2729 0.6749 0.045 Uiso 1 1 calc R . . C229 C 1.00758(15) -0.28257(14) 0.75920(12) 0.0331(4) Uani 1 1 d . . . C230 C 0.92203(18) -0.12263(16) 0.74332(13) 0.0443(5) Uani 1 1 d . . . H23A H 0.9791 -0.1125 0.7677 0.053 Uiso 1 1 calc R . . H23B H 0.8613 -0.1400 0.7834 0.053 Uiso 1 1 calc R . . C231 C 0.89511(16) -0.02979(16) 0.67786(13) 0.0423(5) Uani 1 1 d . . . H23C H 0.9069 0.0265 0.6913 0.051 Uiso 1 1 calc R . . H23D H 0.9426 -0.0275 0.6305 0.051 Uiso 1 1 calc R . . C232 C 0.76727(19) -0.09973(17) 0.63724(16) 0.0537(6) Uani 1 1 d . . . H23E H 0.8134 -0.0986 0.5902 0.081 Uiso 1 1 calc R . . H23F H 0.6952 -0.0915 0.6269 0.081 Uiso 1 1 calc R . . H23G H 0.7790 -0.1622 0.6790 0.081 Uiso 1 1 calc R . . C233 C 0.76686(17) 0.07451(15) 0.59924(12) 0.0422(5) Uani 1 1 d . . . H23H H 0.7049 0.0695 0.5773 0.051 Uiso 1 1 calc R . . H23I H 0.8256 0.0851 0.5573 0.051 Uiso 1 1 calc R . . C234 C 0.74885(16) 0.16352(15) 0.62222(13) 0.0409(5) Uani 1 1 d . . . H23J H 0.8047 0.1651 0.6515 0.049 Uiso 1 1 calc R . . H23K H 0.7490 0.2233 0.5753 0.049 Uiso 1 1 calc R . . C235 C 0.61133(14) 0.24115(13) 0.68608(11) 0.0280(4) Uani 1 1 d . . . C236 C 0.64181(15) 0.33491(14) 0.64361(12) 0.0339(4) Uani 1 1 d . . . H236 H 0.6931 0.3457 0.5998 0.041 Uiso 1 1 calc R . . C237 C 0.59695(15) 0.41292(13) 0.66550(12) 0.0372(5) Uani 1 1 d . . . H237 H 0.6182 0.4767 0.6367 0.045 Uiso 1 1 calc R . . C238 C 0.52243(16) 0.39815(14) 0.72829(12) 0.0366(5) Uani 1 1 d . . . H238 H 0.4926 0.4515 0.7432 0.044 Uiso 1 1 calc R . . C239 C 0.49052(15) 0.30512(13) 0.77014(11) 0.0317(4) Uani 1 1 d . . . H239 H 0.4386 0.2954 0.8134 0.038 Uiso 1 1 calc R . . C240 C 0.53365(14) 0.22586(12) 0.74948(10) 0.0273(4) Uani 1 1 d . . . N101 N 1.01182(12) -0.01535(10) 0.87979(9) 0.0281(3) Uani 1 1 d . . . N102 N 0.95889(11) 0.18168(10) 0.78215(8) 0.0244(3) Uani 1 1 d . . . H102 H 1.0249 0.1660 0.7711 0.029 Uiso 1 1 calc R . . N103 N 1.15609(11) 0.33397(10) 0.64548(8) 0.0244(3) Uani 1 1 d . . . H10A H 1.1516 0.3098 0.6096 0.029 Uiso 1 1 calc R . . N104 N 1.35124(11) 0.29774(11) 0.56904(9) 0.0284(3) Uani 1 1 d . . . N105 N 1.27228(12) -0.01679(11) 0.66948(9) 0.0321(4) Uani 1 1 d . . . N201 N 0.50992(12) 0.12829(11) 0.79333(9) 0.0298(3) Uani 1 1 d . . . N202 N 0.46279(11) -0.06706(10) 0.88284(9) 0.0274(3) Uani 1 1 d . . . H202 H 0.5268 -0.0645 0.8598 0.033 Uiso 1 1 calc R . . N203 N 0.67129(11) -0.27890(10) 0.93063(9) 0.0271(3) Uani 1 1 d . . . H20A H 0.6736 -0.3008 0.8925 0.033 Uiso 1 1 calc R . . N204 N 0.86873(12) -0.31477(12) 0.86698(10) 0.0356(4) Uani 1 1 d . . . N205 N 0.78867(13) -0.01967(12) 0.66072(10) 0.0363(4) Uani 1 1 d . . . O101 O 1.43792(11) 0.11986(10) 0.55261(8) 0.0372(3) Uani 1 1 d . . . O102 O 1.14406(9) -0.12589(9) 0.82087(7) 0.0315(3) Uani 1 1 d . . . O201 O 0.95312(11) -0.20144(10) 0.71369(8) 0.0422(4) Uani 1 1 d . . . O202 O 0.65131(10) 0.15943(9) 0.66928(8) 0.0340(3) Uani 1 1 d . . . O301 O 1.16094(11) 0.09670(10) 0.75772(9) 0.0476(4) Uani 1 1 d . . . O302 O 0.66698(11) -0.03241(10) 0.80524(9) 0.0477(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C101 0.0314(10) 0.0248(9) 0.0270(10) -0.0071(7) 0.0016(8) -0.0054(8) C102 0.0254(9) 0.0244(9) 0.0254(9) -0.0073(7) 0.0005(7) -0.0017(7) C103 0.0251(9) 0.0304(10) 0.0294(10) -0.0072(8) 0.0025(8) -0.0041(8) C104 0.0226(9) 0.0265(9) 0.0283(10) -0.0077(7) -0.0011(7) 0.0023(7) C105 0.0236(9) 0.0216(8) 0.0221(9) -0.0060(7) -0.0027(7) 0.0003(7) C106 0.0215(9) 0.0229(8) 0.0240(9) -0.0054(7) -0.0014(7) -0.0008(7) C107 0.0219(9) 0.0352(10) 0.0246(9) -0.0085(8) 0.0027(7) -0.0101(8) C108 0.0291(10) 0.0432(11) 0.0331(11) -0.0169(9) 0.0046(8) -0.0133(9) C109 0.0447(13) 0.0629(15) 0.0433(13) -0.0311(12) 0.0107(10) -0.0265(11) C110 0.0538(14) 0.0777(18) 0.0283(11) -0.0164(12) -0.0018(10) -0.0354(13) C111 0.0437(13) 0.0585(14) 0.0290(11) -0.0022(10) -0.0076(9) -0.0235(11) C112 0.0225(9) 0.0416(11) 0.0259(10) 0.0003(8) -0.0003(7) -0.0157(8) C113 0.0205(9) 0.0311(10) 0.0304(10) 0.0023(8) -0.0006(7) -0.0079(8) C114 0.0264(10) 0.0376(11) 0.0430(12) 0.0117(10) -0.0057(9) -0.0051(9) C115 0.0314(11) 0.0278(11) 0.0629(16) 0.0045(10) 0.0050(10) 0.0050(9) C116 0.0399(12) 0.0277(10) 0.0554(15) -0.0058(10) 0.0089(10) 0.0015(9) C117 0.0324(11) 0.0263(10) 0.0393(11) -0.0065(8) 0.0030(9) 0.0021(8) C118 0.0202(9) 0.0228(9) 0.0311(10) -0.0007(7) 0.0011(7) -0.0020(7) C119 0.0242(9) 0.0186(8) 0.0234(9) -0.0048(7) -0.0003(7) -0.0003(7) C120 0.0293(10) 0.0418(11) 0.0356(11) -0.0225(9) 0.0015(8) -0.0019(8) C121 0.0273(10) 0.0391(11) 0.0389(11) -0.0207(9) -0.0051(8) -0.0039(8) C122 0.0237(9) 0.0222(8) 0.0318(10) -0.0088(7) -0.0047(7) 0.0009(7) C123 0.0221(9) 0.0244(9) 0.0305(10) -0.0080(8) -0.0055(7) 0.0013(7) C124 0.0216(9) 0.0320(10) 0.0253(9) -0.0104(8) -0.0058(7) 0.0008(7) C125 0.0363(11) 0.0306(10) 0.0338(11) -0.0102(8) -0.0062(9) -0.0018(8) C126 0.0379(11) 0.0430(12) 0.0333(11) -0.0061(9) 0.0005(9) -0.0116(9) C127 0.0319(11) 0.0546(13) 0.0309(11) -0.0117(10) 0.0069(9) -0.0032(10) C128 0.0379(11) 0.0385(11) 0.0306(11) -0.0141(9) 0.0018(9) 0.0052(9) C129 0.0305(10) 0.0304(10) 0.0265(10) -0.0102(8) -0.0031(8) -0.0021(8) C130 0.0414(12) 0.0345(11) 0.0328(11) -0.0100(9) -0.0024(9) -0.0078(9) C131 0.0319(10) 0.0288(10) 0.0397(11) -0.0108(9) -0.0040(8) -0.0002(8) C132 0.0396(12) 0.0486(13) 0.0427(13) -0.0077(10) -0.0102(10) -0.0011(10) C133 0.0394(11) 0.0326(10) 0.0408(12) -0.0175(9) 0.0006(9) -0.0069(9) C134 0.0310(10) 0.0246(9) 0.0427(12) -0.0131(8) -0.0017(8) 0.0010(8) C135 0.0242(9) 0.0236(9) 0.0306(10) -0.0054(7) -0.0078(7) -0.0051(7) C136 0.0268(10) 0.0225(9) 0.0436(12) -0.0053(8) -0.0107(8) -0.0028(7) C137 0.0385(11) 0.0254(10) 0.0427(12) 0.0008(9) -0.0185(9) -0.0040(8) C138 0.0508(13) 0.0347(11) 0.0281(10) -0.0025(8) -0.0125(9) -0.0091(10) C139 0.0404(11) 0.0294(10) 0.0308(10) -0.0085(8) -0.0065(9) -0.0044(8) C140 0.0287(9) 0.0223(9) 0.0290(10) -0.0054(7) -0.0070(8) -0.0059(7) C201 0.0330(10) 0.0245(9) 0.0292(10) -0.0107(8) -0.0031(8) 0.0001(8) C202 0.0297(10) 0.0225(9) 0.0296(10) -0.0092(7) -0.0009(8) -0.0022(7) C203 0.0271(10) 0.0279(9) 0.0381(11) -0.0131(8) 0.0001(8) -0.0017(8) C204 0.0256(9) 0.0277(9) 0.0306(10) -0.0096(8) 0.0004(8) -0.0083(7) C205 0.0265(9) 0.0217(8) 0.0256(9) -0.0074(7) -0.0018(7) -0.0063(7) C206 0.0241(9) 0.0230(8) 0.0275(9) -0.0086(7) -0.0011(7) -0.0050(7) C207 0.0242(9) 0.0231(9) 0.0319(10) -0.0110(7) -0.0066(7) 0.0029(7) C208 0.0346(10) 0.0248(9) 0.0310(10) -0.0082(8) -0.0055(8) -0.0006(8) C209 0.0486(12) 0.0332(10) 0.0283(10) -0.0103(8) -0.0056(9) 0.0018(9) C210 0.0556(13) 0.0347(11) 0.0378(12) -0.0187(9) -0.0150(10) 0.0051(10) C211 0.0412(12) 0.0287(10) 0.0455(12) -0.0175(9) -0.0127(9) 0.0001(9) C212 0.0244(9) 0.0226(9) 0.0370(11) -0.0109(8) -0.0103(8) 0.0026(7) C213 0.0210(9) 0.0210(8) 0.0370(10) -0.0087(8) -0.0058(7) 0.0017(7) C214 0.0300(10) 0.0222(9) 0.0480(12) -0.0120(8) -0.0075(9) -0.0025(8) C215 0.0277(10) 0.0220(9) 0.0475(12) -0.0053(8) 0.0027(9) -0.0060(8) C216 0.0313(10) 0.0273(9) 0.0341(11) -0.0056(8) 0.0028(8) -0.0007(8) C217 0.0269(9) 0.0255(9) 0.0334(10) -0.0092(8) -0.0009(8) -0.0031(7) C218 0.0194(8) 0.0205(8) 0.0339(10) -0.0065(7) -0.0043(7) -0.0008(7) C219 0.0255(9) 0.0229(9) 0.0266(9) -0.0055(7) -0.0004(7) -0.0053(7) C220 0.0314(11) 0.0511(13) 0.0354(11) -0.0233(10) 0.0009(8) -0.0085(9) C221 0.0320(11) 0.0611(14) 0.0359(11) -0.0237(10) -0.0032(9) -0.0120(10) C222 0.0270(10) 0.0332(10) 0.0335(10) -0.0093(8) -0.0045(8) -0.0079(8) C223 0.0265(10) 0.0347(10) 0.0348(11) -0.0103(8) -0.0054(8) -0.0064(8) C224 0.0260(10) 0.0407(11) 0.0423(12) -0.0219(9) -0.0064(8) -0.0031(8) C225 0.0420(12) 0.0403(12) 0.0436(12) -0.0179(10) -0.0079(10) -0.0019(10) C226 0.0412(12) 0.0388(12) 0.0630(16) -0.0271(11) -0.0119(11) 0.0059(10) C227 0.0327(11) 0.0419(12) 0.0627(15) -0.0328(11) 0.0023(10) -0.0014(9) C228 0.0357(11) 0.0395(11) 0.0459(12) -0.0254(10) 0.0022(9) -0.0079(9) C229 0.0304(10) 0.0356(10) 0.0391(11) -0.0189(9) -0.0070(8) -0.0028(8) C230 0.0429(12) 0.0449(12) 0.0520(14) -0.0244(11) -0.0139(10) 0.0047(10) C231 0.0359(11) 0.0420(12) 0.0494(13) -0.0160(10) -0.0021(10) -0.0081(9) C232 0.0548(15) 0.0467(13) 0.0680(17) -0.0252(12) -0.0212(13) -0.0018(11) C233 0.0462(13) 0.0408(12) 0.0320(11) -0.0078(9) 0.0000(9) 0.0024(10) C234 0.0348(11) 0.0333(11) 0.0434(12) -0.0049(9) 0.0075(9) -0.0049(9) C235 0.0256(9) 0.0247(9) 0.0335(10) -0.0073(8) -0.0104(8) -0.0017(7) C236 0.0290(10) 0.0320(10) 0.0354(11) -0.0015(8) -0.0093(8) -0.0084(8) C237 0.0379(11) 0.0207(9) 0.0484(13) 0.0008(8) -0.0181(10) -0.0090(8) C238 0.0427(12) 0.0229(9) 0.0472(12) -0.0122(9) -0.0157(10) -0.0016(8) C239 0.0366(11) 0.0279(9) 0.0307(10) -0.0089(8) -0.0072(8) -0.0028(8) C240 0.0295(10) 0.0219(9) 0.0283(10) -0.0030(7) -0.0099(8) -0.0037(7) N101 0.0316(9) 0.0210(7) 0.0280(8) -0.0054(6) -0.0022(6) -0.0009(6) N102 0.0204(7) 0.0222(7) 0.0253(8) -0.0046(6) 0.0003(6) 0.0019(6) N103 0.0230(7) 0.0236(7) 0.0266(8) -0.0100(6) -0.0022(6) 0.0004(6) N104 0.0217(8) 0.0296(8) 0.0343(9) -0.0130(7) -0.0039(6) 0.0016(6) N105 0.0308(9) 0.0287(8) 0.0352(9) -0.0101(7) -0.0027(7) -0.0015(7) N201 0.0348(9) 0.0222(7) 0.0293(8) -0.0062(6) -0.0005(7) -0.0046(6) N202 0.0258(8) 0.0227(7) 0.0306(8) -0.0075(6) 0.0024(6) -0.0042(6) N203 0.0258(8) 0.0269(8) 0.0304(8) -0.0121(7) -0.0024(6) -0.0037(6) N204 0.0265(8) 0.0429(10) 0.0396(10) -0.0172(8) -0.0024(7) -0.0050(7) N205 0.0353(9) 0.0332(9) 0.0371(10) -0.0091(7) -0.0037(7) -0.0020(7) O101 0.0471(8) 0.0334(7) 0.0331(8) -0.0155(6) 0.0038(6) -0.0100(6) O102 0.0284(7) 0.0264(7) 0.0324(7) -0.0046(5) -0.0013(5) 0.0034(5) O201 0.0457(9) 0.0431(8) 0.0419(9) -0.0210(7) -0.0101(7) 0.0063(7) O202 0.0289(7) 0.0284(7) 0.0417(8) -0.0103(6) 0.0026(6) -0.0067(5) O301 0.0383(8) 0.0286(7) 0.0599(10) -0.0051(7) 0.0079(7) 0.0051(6) O302 0.0399(8) 0.0325(8) 0.0550(10) -0.0030(7) 0.0099(7) -0.0042(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C101 N101 1.282(2) . ? C101 C102 1.435(2) . ? C101 H101 0.9500 . ? C102 N102 1.380(2) . ? C102 C103 1.383(2) . ? C103 C104 1.407(2) . ? C103 H103 0.9500 . ? C104 C105 1.380(2) . ? C104 H104 0.9500 . ? C105 N102 1.363(2) . ? C105 C106 1.519(2) . ? C106 C119 1.521(2) . ? C106 C107 1.537(2) . ? C106 C118 1.544(2) . ? C107 C108 1.389(3) . ? C107 C112 1.408(3) . ? C108 C109 1.396(3) . ? C108 H108 0.9500 . ? C109 C110 1.393(3) . ? C109 H109 0.9500 . ? C110 C111 1.381(3) . ? C110 H110 0.9500 . ? C111 C112 1.389(3) . ? C111 H111 0.9500 . ? C112 C113 1.467(3) . ? C113 C118 1.393(3) . ? C113 C114 1.401(3) . ? C114 C115 1.381(3) . ? C114 H114 0.9500 . ? C115 C116 1.383(3) . ? C115 H115 0.9500 . ? C116 C117 1.401(3) . ? C116 H116 0.9500 . ? C117 C118 1.386(3) . ? C117 H117 0.9500 . ? C119 N103 1.363(2) . ? C119 C120 1.377(2) . ? C120 C121 1.405(3) . ? C120 H120 0.9500 . ? C121 C122 1.378(3) . ? C121 H121 0.9500 . ? C122 N103 1.371(2) . ? C122 C123 1.435(2) . ? C123 N104 1.282(2) . ? C123 H123 0.9500 . ? C124 C125 1.395(3) . ? C124 C129 1.401(2) . ? C124 N104 1.416(2) . ? C125 C126 1.385(3) . ? C125 H125 0.9500 . ? C126 C127 1.382(3) . ? C126 H126 0.9500 . ? C127 C128 1.390(3) . ? C127 H127 0.9500 . ? C128 C129 1.385(3) . ? C128 H128 0.9500 . ? C129 O101 1.379(2) . ? C130 O101 1.450(2) . ? C130 C131 1.506(3) . ? C130 H13A 0.9900 . ? C130 H13B 0.9900 . ? C131 N105 1.469(2) . ? C131 H13C 0.9900 . ? C131 H13D 0.9900 . ? C132 N105 1.470(3) . ? C132 H13E 0.9800 . ? C132 H13F 0.9800 . ? C132 H13G 0.9800 . ? C133 N105 1.479(2) . ? C133 C134 1.511(3) . ? C133 H13H 0.9900 . ? C133 H13I 0.9900 . ? C134 O102 1.433(2) . ? C134 H13J 0.9900 . ? C134 H13K 0.9900 . ? C135 O102 1.375(2) . ? C135 C136 1.389(2) . ? C135 C140 1.405(3) . ? C136 C137 1.387(3) . ? C136 H136 0.9500 . ? C137 C138 1.375(3) . ? C137 H137 0.9500 . ? C138 C139 1.394(3) . ? C138 H138 0.9500 . ? C139 C140 1.389(3) . ? C139 H139 0.9500 . ? C140 N101 1.416(2) . ? C201 N201 1.284(2) . ? C201 C202 1.439(2) . ? C201 H201 0.9500 . ? C202 N202 1.376(2) . ? C202 C203 1.384(3) . ? C203 C204 1.411(3) . ? C203 H203 0.9500 . ? C204 C205 1.378(2) . ? C204 H204 0.9500 . ? C205 N202 1.364(2) . ? C205 C206 1.519(2) . ? C206 C219 1.517(2) . ? C206 C218 1.537(2) . ? C206 C207 1.540(2) . ? C207 C208 1.389(3) . ? C207 C212 1.403(2) . ? C208 C209 1.399(3) . ? C208 H208 0.9500 . ? C209 C210 1.387(3) . ? C209 H209 0.9500 . ? C210 C211 1.390(3) . ? C210 H210 0.9500 . ? C211 C212 1.391(3) . ? C211 H211 0.9500 . ? C212 C213 1.465(3) . ? C213 C214 1.396(3) . ? C213 C218 1.401(2) . ? C214 C215 1.383(3) . ? C214 H214 0.9500 . ? C215 C216 1.391(3) . ? C215 H215 0.9500 . ? C216 C217 1.395(3) . ? C216 H216 0.9500 . ? C217 C218 1.381(3) . ? C217 H217 0.9500 . ? C219 N203 1.356(2) . ? C219 C220 1.376(3) . ? C220 C221 1.404(3) . ? C220 H220 0.9500 . ? C221 C222 1.379(3) . ? C221 H221 0.9500 . ? C222 N203 1.373(2) . ? C222 C223 1.434(3) . ? C223 N204 1.285(2) . ? C223 H223 0.9500 . ? C224 C225 1.392(3) . ? C224 C229 1.404(3) . ? C224 N204 1.418(2) . ? C225 C226 1.393(3) . ? C225 H225 0.9500 . ? C226 C227 1.378(3) . ? C226 H226 0.9500 . ? C227 C228 1.381(3) . ? C227 H227 0.9500 . ? C228 C229 1.383(3) . ? C228 H228 0.9500 . ? C229 O201 1.381(2) . ? C230 O201 1.454(2) . ? C230 C231 1.514(3) . ? C230 H23A 0.9900 . ? C230 H23B 0.9900 . ? C231 N205 1.461(3) . ? C231 H23C 0.9900 . ? C231 H23D 0.9900 . ? C232 N205 1.476(3) . ? C232 H23E 0.9800 . ? C232 H23F 0.9800 . ? C232 H23G 0.9800 . ? C233 N205 1.474(3) . ? C233 C234 1.510(3) . ? C233 H23H 0.9900 . ? C233 H23I 0.9900 . ? C234 O202 1.427(2) . ? C234 H23J 0.9900 . ? C234 H23K 0.9900 . ? C235 O202 1.380(2) . ? C235 C236 1.393(3) . ? C235 C240 1.403(3) . ? C236 C237 1.395(3) . ? C236 H236 0.9500 . ? C237 C238 1.370(3) . ? C237 H237 0.9500 . ? C238 C239 1.389(3) . ? C238 H238 0.9500 . ? C239 C240 1.393(3) . ? C239 H239 0.9500 . ? C240 N201 1.419(2) . ? N102 H102 0.8800 . ? N103 H10A 0.8800 . ? N202 H202 0.8800 . ? N203 H20A 0.8800 . ? 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 N101 C101 C102 122.31(17) . . ? N101 C101 H101 118.8 . . ? C102 C101 H101 118.8 . . ? N102 C102 C103 107.25(15) . . ? N102 C102 C101 123.39(16) . . ? C103 C102 C101 129.34(17) . . ? C102 C103 C104 107.77(16) . . ? C102 C103 H103 126.1 . . ? C104 C103 H103 126.1 . . ? C105 C104 C103 107.33(15) . . ? C105 C104 H104 126.3 . . ? C103 C104 H104 126.3 . . ? N102 C105 C104 108.15(15) . . ? N102 C105 C106 121.37(14) . . ? C104 C105 C106 129.97(15) . . ? C105 C106 C119 112.53(14) . . ? C105 C106 C107 109.72(14) . . ? C119 C106 C107 111.11(14) . . ? C105 C106 C118 111.21(14) . . ? C119 C106 C118 110.46(14) . . ? C107 C106 C118 101.27(14) . . ? C108 C107 C112 121.14(18) . . ? C108 C107 C106 128.84(17) . . ? C112 C107 C106 110.02(16) . . ? C107 C108 C109 118.2(2) . . ? C107 C108 H108 120.9 . . ? C109 C108 H108 120.9 . . ? C110 C109 C108 120.5(2) . . ? C110 C109 H109 119.8 . . ? C108 C109 H109 119.8 . . ? C111 C110 C109 121.2(2) . . ? C111 C110 H110 119.4 . . ? C109 C110 H110 119.4 . . ? C110 C111 C112 119.1(2) . . ? C110 C111 H111 120.5 . . ? C112 C111 H111 120.5 . . ? C111 C112 C107 119.8(2) . . ? C111 C112 C113 131.07(19) . . ? C107 C112 C113 109.11(16) . . ? C118 C113 C114 120.06(19) . . ? C118 C113 C112 109.00(16) . . ? C114 C113 C112 130.94(19) . . ? C115 C114 C113 118.9(2) . . ? C115 C114 H114 120.6 . . ? C113 C114 H114 120.6 . . ? C114 C115 C116 121.23(19) . . ? C114 C115 H115 119.4 . . ? C116 C115 H115 119.4 . . ? C115 C116 C117 120.2(2) . . ? C115 C116 H116 119.9 . . ? C117 C116 H116 119.9 . . ? C118 C117 C116 118.9(2) . . ? C118 C117 H117 120.6 . . ? C116 C117 H117 120.6 . . ? C117 C118 C113 120.76(17) . . ? C117 C118 C106 128.66(17) . . ? C113 C118 C106 110.58(16) . . ? N103 C119 C120 106.88(15) . . ? N103 C119 C106 122.08(15) . . ? C120 C119 C106 130.90(16) . . ? C119 C120 C121 107.84(16) . . ? C119 C120 H120 126.1 . . ? C121 C120 H120 126.1 . . ? C122 C121 C120 107.94(16) . . ? C122 C121 H121 126.0 . . ? C120 C121 H121 126.0 . . ? N103 C122 C121 106.54(15) . . ? N103 C122 C123 121.40(16) . . ? C121 C122 C123 132.00(17) . . ? N104 C123 C122 121.23(16) . . ? N104 C123 H123 119.4 . . ? C122 C123 H123 119.4 . . ? C125 C124 C129 118.38(17) . . ? C125 C124 N104 121.73(16) . . ? C129 C124 N104 119.74(16) . . ? C126 C125 C124 121.62(18) . . ? C126 C125 H125 119.2 . . ? C124 C125 H125 119.2 . . ? C127 C126 C125 119.38(19) . . ? C127 C126 H126 120.3 . . ? C125 C126 H126 120.3 . . ? C126 C127 C128 119.97(19) . . ? C126 C127 H127 120.0 . . ? C128 C127 H127 120.0 . . ? C129 C128 C127 120.69(19) . . ? C129 C128 H128 119.7 . . ? C127 C128 H128 119.7 . . ? O101 C129 C128 117.95(17) . . ? O101 C129 C124 122.08(16) . . ? C128 C129 C124 119.96(17) . . ? O101 C130 C131 109.09(16) . . ? O101 C130 H13A 109.9 . . ? C131 C130 H13A 109.9 . . ? O101 C130 H13B 109.9 . . ? C131 C130 H13B 109.9 . . ? H13A C130 H13B 108.3 . . ? N105 C131 C130 114.84(16) . . ? N105 C131 H13C 108.6 . . ? C130 C131 H13C 108.6 . . ? N105 C131 H13D 108.6 . . ? C130 C131 H13D 108.6 . . ? H13C C131 H13D 107.5 . . ? N105 C132 H13E 109.5 . . ? N105 C132 H13F 109.5 . . ? H13E C132 H13F 109.5 . . ? N105 C132 H13G 109.5 . . ? H13E C132 H13G 109.5 . . ? H13F C132 H13G 109.5 . . ? N105 C133 C134 115.77(16) . . ? N105 C133 H13H 108.3 . . ? C134 C133 H13H 108.3 . . ? N105 C133 H13I 108.3 . . ? C134 C133 H13I 108.3 . . ? H13H C133 H13I 107.4 . . ? O102 C134 C133 107.25(15) . . ? O102 C134 H13J 110.3 . . ? C133 C134 H13J 110.3 . . ? O102 C134 H13K 110.3 . . ? C133 C134 H13K 110.3 . . ? H13J C134 H13K 108.5 . . ? O102 C135 C136 125.23(17) . . ? O102 C135 C140 114.59(15) . . ? C136 C135 C140 120.17(17) . . ? C137 C136 C135 119.72(19) . . ? C137 C136 H136 120.1 . . ? C135 C136 H136 120.1 . . ? C138 C137 C136 120.80(18) . . ? C138 C137 H137 119.6 . . ? C136 C137 H137 119.6 . . ? C137 C138 C139 119.64(19) . . ? C137 C138 H138 120.2 . . ? C139 C138 H138 120.2 . . ? C140 C139 C138 120.70(19) . . ? C140 C139 H139 119.6 . . ? C138 C139 H139 119.6 . . ? C139 C140 C135 118.92(16) . . ? C139 C140 N101 123.63(17) . . ? C135 C140 N101 117.25(16) . . ? N201 C201 C202 121.73(17) . . ? N201 C201 H201 119.1 . . ? C202 C201 H201 119.1 . . ? N202 C202 C203 107.15(15) . . ? N202 C202 C201 121.96(16) . . ? C203 C202 C201 130.88(17) . . ? C202 C203 C204 107.81(16) . . ? C202 C203 H203 126.1 . . ? C204 C203 H203 126.1 . . ? C205 C204 C203 107.13(16) . . ? C205 C204 H204 126.4 . . ? C203 C204 H204 126.4 . . ? N202 C205 C204 108.22(15) . . ? N202 C205 C206 119.31(15) . . ? C204 C205 C206 132.20(15) . . ? C219 C206 C205 109.49(14) . . ? C219 C206 C218 111.48(14) . . ? C205 C206 C218 111.99(14) . . ? C219 C206 C207 112.02(14) . . ? C205 C206 C207 110.72(14) . . ? C218 C206 C207 100.96(13) . . ? C208 C207 C212 120.69(17) . . ? C208 C207 C206 128.88(16) . . ? C212 C207 C206 110.43(15) . . ? C207 C208 C209 118.46(17) . . ? C207 C208 H208 120.8 . . ? C209 C208 H208 120.8 . . ? C210 C209 C208 120.89(19) . . ? C210 C209 H209 119.6 . . ? C208 C209 H209 119.6 . . ? C209 C210 C211 120.65(18) . . ? C209 C210 H210 119.7 . . ? C211 C210 H210 119.7 . . ? C210 C211 C212 118.98(18) . . ? C210 C211 H211 120.5 . . ? C212 C211 H211 120.5 . . ? C211 C212 C207 120.32(18) . . ? C211 C212 C213 130.67(17) . . ? C207 C212 C213 109.01(15) . . ? C214 C213 C218 120.38(18) . . ? C214 C213 C212 130.79(17) . . ? C218 C213 C212 108.83(15) . . ? C215 C214 C213 118.79(18) . . ? C215 C214 H214 120.6 . . ? C213 C214 H214 120.6 . . ? C214 C215 C216 120.73(17) . . ? C214 C215 H215 119.6 . . ? C216 C215 H215 119.6 . . ? C215 C216 C217 120.72(19) . . ? C215 C216 H216 119.6 . . ? C217 C216 H216 119.6 . . ? C218 C217 C216 118.74(17) . . ? C218 C217 H217 120.6 . . ? C216 C217 H217 120.6 . . ? C217 C218 C213 120.63(16) . . ? C217 C218 C206 128.62(16) . . ? C213 C218 C206 110.75(16) . . ? N203 C219 C220 107.27(16) . . ? N203 C219 C206 121.66(15) . . ? C220 C219 C206 131.06(17) . . ? C219 C220 C221 107.85(17) . . ? C219 C220 H220 126.1 . . ? C221 C220 H220 126.1 . . ? C222 C221 C220 107.55(17) . . ? C222 C221 H221 126.2 . . ? C220 C221 H221 126.2 . . ? N203 C222 C221 106.80(16) . . ? N203 C222 C223 119.51(17) . . ? C221 C222 C223 133.44(18) . . ? N204 C223 C222 119.53(17) . . ? N204 C223 H223 120.2 . . ? C222 C223 H223 120.2 . . ? C225 C224 C229 118.78(18) . . ? C225 C224 N204 121.66(19) . . ? C229 C224 N204 119.39(18) . . ? C224 C225 C226 121.3(2) . . ? C224 C225 H225 119.4 . . ? C226 C225 H225 119.4 . . ? C227 C226 C225 119.3(2) . . ? C227 C226 H226 120.3 . . ? C225 C226 H226 120.3 . . ? C226 C227 C228 119.87(19) . . ? C226 C227 H227 120.1 . . ? C228 C227 H227 120.1 . . ? C227 C228 C229 121.5(2) . . ? C227 C228 H228 119.2 . . ? C229 C228 H228 119.2 . . ? O201 C229 C228 117.68(18) . . ? O201 C229 C224 123.08(17) . . ? C228 C229 C224 119.20(19) . . ? O201 C230 C231 109.97(18) . . ? O201 C230 H23A 109.7 . . ? C231 C230 H23A 109.7 . . ? O201 C230 H23B 109.7 . . ? C231 C230 H23B 109.7 . . ? H23A C230 H23B 108.2 . . ? N205 C231 C230 114.29(17) . . ? N205 C231 H23C 108.7 . . ? C230 C231 H23C 108.7 . . ? N205 C231 H23D 108.7 . . ? C230 C231 H23D 108.7 . . ? H23C C231 H23D 107.6 . . ? N205 C232 H23E 109.5 . . ? N205 C232 H23F 109.5 . . ? H23E C232 H23F 109.5 . . ? N205 C232 H23G 109.5 . . ? H23E C232 H23G 109.5 . . ? H23F C232 H23G 109.5 . . ? N205 C233 C234 116.97(18) . . ? N205 C233 H23H 108.1 . . ? C234 C233 H23H 108.1 . . ? N205 C233 H23I 108.1 . . ? C234 C233 H23I 108.1 . . ? H23H C233 H23I 107.3 . . ? O202 C234 C233 108.57(16) . . ? O202 C234 H23J 110.0 . . ? C233 C234 H23J 110.0 . . ? O202 C234 H23K 110.0 . . ? C233 C234 H23K 110.0 . . ? H23J C234 H23K 108.4 . . ? O202 C235 C236 124.25(17) . . ? O202 C235 C240 115.85(15) . . ? C236 C235 C240 119.89(17) . . ? C235 C236 C237 119.92(19) . . ? C235 C236 H236 120.0 . . ? C237 C236 H236 120.0 . . ? C238 C237 C236 120.44(17) . . ? C238 C237 H237 119.8 . . ? C236 C237 H237 119.8 . . ? C237 C238 C239 119.93(19) . . ? C237 C238 H238 120.0 . . ? C239 C238 H238 120.0 . . ? C238 C239 C240 120.91(19) . . ? C238 C239 H239 119.5 . . ? C240 C239 H239 119.5 . . ? C239 C240 C235 118.87(16) . . ? C239 C240 N201 123.43(17) . . ? C235 C240 N201 117.46(16) . . ? C101 N101 C140 119.74(15) . . ? C105 N102 C102 109.50(14) . . ? C105 N102 H102 125.2 . . ? C102 N102 H102 125.2 . . ? C119 N103 C122 110.79(15) . . ? C119 N103 H10A 124.6 . . ? C122 N103 H10A 124.6 . . ? C123 N104 C124 117.94(15) . . ? C131 N105 C132 112.39(16) . . ? C131 N105 C133 109.71(15) . . ? C132 N105 C133 109.58(16) . . ? C201 N201 C240 120.25(16) . . ? C205 N202 C202 109.67(14) . . ? C205 N202 H202 125.2 . . ? C202 N202 H202 125.2 . . ? C219 N203 C222 110.50(15) . . ? C219 N203 H20A 124.7 . . ? C222 N203 H20A 124.7 . . ? C223 N204 C224 118.97(16) . . ? C231 N205 C233 111.07(16) . . ? C231 N205 C232 111.35(17) . . ? C233 N205 C232 109.46(17) . . ? C129 O101 C130 115.96(14) . . ? C135 O102 C134 118.96(14) . . ? C229 O201 C230 117.52(15) . . ? C235 O202 C234 118.23(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N101 C101 C102 N102 3.3(3) . . . . ? N101 C101 C102 C103 -174.51(19) . . . . ? N102 C102 C103 C104 -0.6(2) . . . . ? C101 C102 C103 C104 177.49(18) . . . . ? C102 C103 C104 C105 0.7(2) . . . . ? C103 C104 C105 N102 -0.6(2) . . . . ? C103 C104 C105 C106 171.12(17) . . . . ? N102 C105 C106 C119 -42.7(2) . . . . ? C104 C105 C106 C119 146.58(18) . . . . ? N102 C105 C106 C107 81.58(19) . . . . ? C104 C105 C106 C107 -89.2(2) . . . . ? N102 C105 C106 C118 -167.20(15) . . . . ? C104 C105 C106 C118 22.1(3) . . . . ? C105 C106 C107 C108 -61.3(2) . . . . ? C119 C106 C107 C108 63.8(2) . . . . ? C118 C106 C107 C108 -178.90(17) . . . . ? C105 C106 C107 C112 118.65(15) . . . . ? C119 C106 C107 C112 -116.27(16) . . . . ? C118 C106 C107 C112 1.05(17) . . . . ? C112 C107 C108 C109 2.2(3) . . . . ? C106 C107 C108 C109 -177.83(17) . . . . ? C107 C108 C109 C110 -1.0(3) . . . . ? C108 C109 C110 C111 -1.0(3) . . . . ? C109 C110 C111 C112 1.7(3) . . . . ? C110 C111 C112 C107 -0.5(3) . . . . ? C110 C111 C112 C113 179.22(19) . . . . ? C108 C107 C112 C111 -1.5(3) . . . . ? C106 C107 C112 C111 178.55(16) . . . . ? C108 C107 C112 C113 178.72(16) . . . . ? C106 C107 C112 C113 -1.24(19) . . . . ? C111 C112 C113 C118 -178.85(18) . . . . ? C107 C112 C113 C118 0.9(2) . . . . ? C111 C112 C113 C114 2.0(3) . . . . ? C107 C112 C113 C114 -178.20(18) . . . . ? C118 C113 C114 C115 1.2(3) . . . . ? C112 C113 C114 C115 -179.80(18) . . . . ? C113 C114 C115 C116 -0.3(3) . . . . ? C114 C115 C116 C117 -1.0(3) . . . . ? C115 C116 C117 C118 1.3(3) . . . . ? C116 C117 C118 C113 -0.3(3) . . . . ? C116 C117 C118 C106 179.77(17) . . . . ? C114 C113 C118 C117 -0.9(3) . . . . ? C112 C113 C118 C117 179.89(16) . . . . ? C114 C113 C118 C106 179.02(15) . . . . ? C112 C113 C118 C106 -0.20(19) . . . . ? C105 C106 C118 C117 62.9(2) . . . . ? C119 C106 C118 C117 -62.8(2) . . . . ? C107 C106 C118 C117 179.41(18) . . . . ? C105 C106 C118 C113 -117.02(16) . . . . ? C119 C106 C118 C113 117.29(16) . . . . ? C107 C106 C118 C113 -0.50(18) . . . . ? C105 C106 C119 N103 112.47(17) . . . . ? C107 C106 C119 N103 -11.0(2) . . . . ? C118 C106 C119 N103 -122.59(17) . . . . ? C105 C106 C119 C120 -72.3(2) . . . . ? C107 C106 C119 C120 164.18(19) . . . . ? C118 C106 C119 C120 52.6(2) . . . . ? N103 C119 C120 C121 0.4(2) . . . . ? C106 C119 C120 C121 -175.38(17) . . . . ? C119 C120 C121 C122 -0.1(2) . . . . ? C120 C121 C122 N103 -0.2(2) . . . . ? C120 C121 C122 C123 177.03(19) . . . . ? N103 C122 C123 N104 -7.3(3) . . . . ? C121 C122 C123 N104 175.8(2) . . . . ? C129 C124 C125 C126 -0.7(3) . . . . ? N104 C124 C125 C126 -176.15(18) . . . . ? C124 C125 C126 C127 0.9(3) . . . . ? C125 C126 C127 C128 -0.5(3) . . . . ? C126 C127 C128 C129 -0.2(3) . . . . ? C127 C128 C129 O101 178.85(18) . . . . ? C127 C128 C129 C124 0.4(3) . . . . ? C125 C124 C129 O101 -178.36(16) . . . . ? N104 C124 C129 O101 -2.8(3) . . . . ? C125 C124 C129 C128 0.0(3) . . . . ? N104 C124 C129 C128 175.58(17) . . . . ? O101 C130 C131 N105 -82.3(2) . . . . ? N105 C133 C134 O102 73.1(2) . . . . ? O102 C135 C136 C137 179.39(16) . . . . ? C140 C135 C136 C137 -2.3(3) . . . . ? C135 C136 C137 C138 0.6(3) . . . . ? C136 C137 C138 C139 0.6(3) . . . . ? C137 C138 C139 C140 -0.2(3) . . . . ? C138 C139 C140 C135 -1.4(3) . . . . ? C138 C139 C140 N101 -176.14(17) . . . . ? O102 C135 C140 C139 -178.85(15) . . . . ? C136 C135 C140 C139 2.6(3) . . . . ? O102 C135 C140 N101 -3.8(2) . . . . ? C136 C135 C140 N101 177.71(16) . . . . ? N201 C201 C202 N202 -5.0(3) . . . . ? N201 C201 C202 C203 174.03(19) . . . . ? N202 C202 C203 C204 0.4(2) . . . . ? C201 C202 C203 C204 -178.75(19) . . . . ? C202 C203 C204 C205 -1.0(2) . . . . ? C203 C204 C205 N202 1.1(2) . . . . ? C203 C204 C205 C206 -172.66(18) . . . . ? N202 C205 C206 C219 53.0(2) . . . . ? C204 C205 C206 C219 -133.7(2) . . . . ? N202 C205 C206 C218 177.22(15) . . . . ? C204 C205 C206 C218 -9.6(3) . . . . ? N202 C205 C206 C207 -71.0(2) . . . . ? C204 C205 C206 C207 102.3(2) . . . . ? C219 C206 C207 C208 -59.8(2) . . . . ? C205 C206 C207 C208 62.8(2) . . . . ? C218 C206 C207 C208 -178.50(17) . . . . ? C219 C206 C207 C212 120.21(16) . . . . ? C205 C206 C207 C212 -117.26(16) . . . . ? C218 C206 C207 C212 1.49(18) . . . . ? C212 C207 C208 C209 0.5(3) . . . . ? C206 C207 C208 C209 -179.50(17) . . . . ? C207 C208 C209 C210 0.1(3) . . . . ? C208 C209 C210 C211 -0.4(3) . . . . ? C209 C210 C211 C212 0.2(3) . . . . ? C210 C211 C212 C207 0.4(3) . . . . ? C210 C211 C212 C213 -179.00(18) . . . . ? C208 C207 C212 C211 -0.8(3) . . . . ? C206 C207 C212 C211 179.22(16) . . . . ? C208 C207 C212 C213 178.76(16) . . . . ? C206 C207 C212 C213 -1.23(19) . . . . ? C211 C212 C213 C214 -0.1(3) . . . . ? C207 C212 C213 C214 -179.61(18) . . . . ? C211 C212 C213 C218 179.88(18) . . . . ? C207 C212 C213 C218 0.4(2) . . . . ? C218 C213 C214 C215 -1.1(3) . . . . ? C212 C213 C214 C215 178.94(18) . . . . ? C213 C214 C215 C216 -0.3(3) . . . . ? C214 C215 C216 C217 1.3(3) . . . . ? C215 C216 C217 C218 -0.9(3) . . . . ? C216 C217 C218 C213 -0.5(3) . . . . ? C216 C217 C218 C206 -179.46(17) . . . . ? C214 C213 C218 C217 1.4(3) . . . . ? C212 C213 C218 C217 -178.56(16) . . . . ? C214 C213 C218 C206 -179.39(16) . . . . ? C212 C213 C218 C206 0.61(19) . . . . ? C219 C206 C218 C217 58.7(2) . . . . ? C205 C206 C218 C217 -64.3(2) . . . . ? C207 C206 C218 C217 177.83(17) . . . . ? C219 C206 C218 C213 -120.36(16) . . . . ? C205 C206 C218 C213 116.57(16) . . . . ? C207 C206 C218 C213 -1.25(18) . . . . ? C205 C206 C219 N203 -132.49(16) . . . . ? C218 C206 C219 N203 103.03(19) . . . . ? C207 C206 C219 N203 -9.3(2) . . . . ? C205 C206 C219 C220 49.0(3) . . . . ? C218 C206 C219 C220 -75.5(2) . . . . ? C207 C206 C219 C220 172.20(19) . . . . ? N203 C219 C220 C221 -1.7(2) . . . . ? C206 C219 C220 C221 177.03(18) . . . . ? C219 C220 C221 C222 1.5(2) . . . . ? C220 C221 C222 N203 -0.8(2) . . . . ? C220 C221 C222 C223 173.1(2) . . . . ? N203 C222 C223 N204 6.6(3) . . . . ? C221 C222 C223 N204 -166.8(2) . . . . ? C229 C224 C225 C226 0.3(3) . . . . ? N204 C224 C225 C226 175.50(18) . . . . ? C224 C225 C226 C227 -0.6(3) . . . . ? C225 C226 C227 C228 0.5(3) . . . . ? C226 C227 C228 C229 0.1(3) . . . . ? C227 C228 C229 O201 -178.51(17) . . . . ? C227 C228 C229 C224 -0.4(3) . . . . ? C225 C224 C229 O201 178.24(17) . . . . ? N204 C224 C229 O201 2.9(3) . . . . ? C225 C224 C229 C228 0.3(3) . . . . ? N204 C224 C229 C228 -175.07(17) . . . . ? O201 C230 C231 N205 85.2(2) . . . . ? N205 C233 C234 O202 -71.0(2) . . . . ? O202 C235 C236 C237 -179.73(17) . . . . ? C240 C235 C236 C237 1.7(3) . . . . ? C235 C236 C237 C238 -0.5(3) . . . . ? C236 C237 C238 C239 -0.6(3) . . . . ? C237 C238 C239 C240 0.3(3) . . . . ? C238 C239 C240 C235 0.9(3) . . . . ? C238 C239 C240 N201 175.08(17) . . . . ? O202 C235 C240 C239 179.40(15) . . . . ? C236 C235 C240 C239 -1.9(3) . . . . ? O202 C235 C240 N201 4.9(2) . . . . ? C236 C235 C240 N201 -176.44(16) . . . . ? C102 C101 N101 C140 177.56(16) . . . . ? C139 C140 N101 C101 -44.8(3) . . . . ? C135 C140 N101 C101 140.41(17) . . . . ? C104 C105 N102 C102 0.2(2) . . . . ? C106 C105 N102 C102 -172.34(15) . . . . ? C103 C102 N102 C105 0.2(2) . . . . ? C101 C102 N102 C105 -177.98(16) . . . . ? C120 C119 N103 C122 -0.5(2) . . . . ? C106 C119 N103 C122 175.72(15) . . . . ? C121 C122 N103 C119 0.4(2) . . . . ? C123 C122 N103 C119 -177.15(15) . . . . ? C122 C123 N104 C124 175.19(16) . . . . ? C125 C124 N104 C123 -52.6(2) . . . . ? C129 C124 N104 C123 131.99(18) . . . . ? C130 C131 N105 C132 58.6(2) . . . . ? C130 C131 N105 C133 -179.19(16) . . . . ? C134 C133 N105 C131 78.4(2) . . . . ? C134 C133 N105 C132 -157.73(17) . . . . ? C202 C201 N201 C240 -176.84(16) . . . . ? C239 C240 N201 C201 36.7(3) . . . . ? C235 C240 N201 C201 -149.07(17) . . . . ? C204 C205 N202 C202 -0.9(2) . . . . ? C206 C205 N202 C202 173.83(15) . . . . ? C203 C202 N202 C205 0.3(2) . . . . ? C201 C202 N202 C205 179.55(16) . . . . ? C220 C219 N203 C222 1.2(2) . . . . ? C206 C219 N203 C222 -177.66(15) . . . . ? C221 C222 N203 C219 -0.2(2) . . . . ? C223 C222 N203 C219 -175.17(16) . . . . ? C222 C223 N204 C224 -179.81(17) . . . . ? C225 C224 N204 C223 61.4(3) . . . . ? C229 C224 N204 C223 -123.4(2) . . . . ? C230 C231 N205 C233 177.10(18) . . . . ? C230 C231 N205 C232 -60.6(2) . . . . ? C234 C233 N205 C231 -76.8(2) . . . . ? C234 C233 N205 C232 159.82(19) . . . . ? C128 C129 O101 C130 119.24(19) . . . . ? C124 C129 O101 C130 -62.3(2) . . . . ? C131 C130 O101 C129 -170.78(15) . . . . ? C136 C135 O102 C134 -16.6(2) . . . . ? C140 C135 O102 C134 164.96(15) . . . . ? C133 C134 O102 C135 168.16(15) . . . . ? C228 C229 O201 C230 -124.3(2) . . . . ? C224 C229 O201 C230 57.7(2) . . . . ? C231 C230 O201 C229 161.99(17) . . . . ? C236 C235 O202 C234 19.8(3) . . . . ? C240 C235 O202 C234 -161.60(17) . . . . ? C233 C234 O202 C235 -169.35(16) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.545 _refine_diff_density_min -0.248 _refine_diff_density_rms 0.044 data_jl9017_K2(LP) _database_code_depnum_ccdc_archive 'CCDC 895815' #TrackingRef 'combined_CIF.cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H40 K2 N4 O5 C6H6 C6H6' _chemical_formula_sum 'C47 H52 K2 N4 O5' _chemical_formula_weight 831.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.9201(7) _cell_length_b 20.8977(11) _cell_length_c 15.4577(8) _cell_angle_alpha 90.00 _cell_angle_beta 117.565(2) _cell_angle_gamma 90.00 _cell_volume 4272.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8764 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 26.4 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 0.273 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6430 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 42106 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 26.42 _reflns_number_total 8764 _reflns_number_gt 7237 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Siemans, 1993)' _computing_cell_refinement 'SAINT (Siemans, 1995)' _computing_data_reduction 'SAINT (Siemans, 1995)' _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Farrugia, 2008)' _computing_publication_material 'enCIFer (Allen et al., 2004)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0805P)^2^+4.8986P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8764 _refine_ls_number_parameters 519 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0866 _refine_ls_R_factor_gt 0.0718 _refine_ls_wR_factor_ref 0.1845 _refine_ls_wR_factor_gt 0.1750 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C01 C 0.7365(2) 0.17875(16) 0.7433(2) 0.0318(6) Uani 1 1 d . . . H023 H 0.6710 0.1601 0.7152 0.038 Uiso 1 1 calc R . . C02 C 0.8210(2) 0.13717(14) 0.7898(2) 0.0283(6) Uani 1 1 d . . . C03 C 0.8187(2) 0.07057(15) 0.8003(2) 0.0336(7) Uani 1 1 d . . . H032 H 0.7605 0.0440 0.7761 0.040 Uiso 1 1 calc R . . C04 C 0.9182(2) 0.05148(14) 0.8530(2) 0.0310(6) Uani 1 1 d . . . H026 H 0.9422 0.0092 0.8727 0.037 Uiso 1 1 calc R . . C05 C 0.9770(2) 0.10748(13) 0.87146(18) 0.0230(5) Uani 1 1 d . . . C06 C 1.0914(2) 0.11447(13) 0.92419(19) 0.0241(6) Uani 1 1 d . . . C07 C 1.1228(2) 0.15618(13) 1.01634(19) 0.0273(6) Uani 1 1 d . . . H02C H 1.1965 0.1641 1.0461 0.033 Uiso 1 1 calc R . . H02D H 1.0883 0.1981 0.9965 0.033 Uiso 1 1 calc R . . C08 C 1.0982(2) 0.12657(15) 1.0932(2) 0.0344(7) Uani 1 1 d . . . H03E H 1.0274 0.1127 1.0623 0.052 Uiso 1 1 calc R . . H03F H 1.1091 0.1584 1.1437 0.052 Uiso 1 1 calc R . . H03G H 1.1423 0.0896 1.1230 0.052 Uiso 1 1 calc R . . C09 C 1.1401(2) 0.04704(13) 0.9506(2) 0.0287(6) Uani 1 1 d . . . H02A H 1.1121 0.0242 0.9889 0.034 Uiso 1 1 calc R . . H02B H 1.1204 0.0227 0.8895 0.034 Uiso 1 1 calc R . . C10 C 1.2542(2) 0.04694(16) 1.0083(2) 0.0389(7) Uani 1 1 d . . . H04A H 1.2830 0.0701 0.9718 0.058 Uiso 1 1 calc R . . H04B H 1.2789 0.0027 1.0190 0.058 Uiso 1 1 calc R . . H04C H 1.2747 0.0679 1.0713 0.058 Uiso 1 1 calc R . . C11 C 1.12283(19) 0.14780(13) 0.85490(19) 0.0231(5) Uani 1 1 d . . . C12 C 1.1765(2) 0.20592(13) 0.8677(2) 0.0276(6) Uani 1 1 d . . . H018 H 1.2050 0.2318 0.9246 0.033 Uiso 1 1 calc R . . C13 C 1.1792(2) 0.21740(14) 0.7809(2) 0.0294(6) Uani 1 1 d . . . H016 H 1.2096 0.2528 0.7660 0.035 Uiso 1 1 calc R . . C14 C 1.1276(2) 0.16595(13) 0.71923(19) 0.0250(6) Uani 1 1 d . . . C15 C 1.1094(2) 0.15744(14) 0.6209(2) 0.0266(6) Uani 1 1 d . . . H013 H 1.1382 0.1873 0.5946 0.032 Uiso 1 1 calc R . . C16 C 1.0457(2) 0.10554(13) 0.4708(2) 0.0283(6) Uani 1 1 d . . . C17 C 1.1179(2) 0.12615(15) 0.4433(2) 0.0340(7) Uani 1 1 d . . . H22 H 1.1763 0.1482 0.4894 0.041 Uiso 1 1 calc R . . C18 C 1.1061(3) 0.11504(16) 0.3493(2) 0.0400(8) Uani 1 1 d . . . H23 H 1.1563 0.1291 0.3320 0.048 Uiso 1 1 calc R . . C19 C 1.0214(3) 0.08371(16) 0.2822(2) 0.0429(8) Uani 1 1 d . . . H24 H 1.0131 0.0761 0.2183 0.052 Uiso 1 1 calc R . . C20 C 0.9477(3) 0.06302(15) 0.3069(2) 0.0401(8) Uani 1 1 d . . . H25 H 0.8889 0.0420 0.2597 0.048 Uiso 1 1 calc R . . C21 C 0.9601(2) 0.07317(13) 0.4008(2) 0.0305(6) Uani 1 1 d . . . C22 C 0.7983(2) 0.02771(16) 0.3588(2) 0.0381(7) Uani 1 1 d . . . H03C H 0.8110 -0.0091 0.3255 0.046 Uiso 1 1 calc R . . H03D H 0.7606 0.0607 0.3093 0.046 Uiso 1 1 calc R . . C23 C 0.7384(3) 0.00656(16) 0.4099(2) 0.0405(8) Uani 1 1 d . . . H03H H 0.6693 -0.0051 0.3601 0.049 Uiso 1 1 calc R . . H03I H 0.7703 -0.0323 0.4485 0.049 Uiso 1 1 calc R . . C24 C 0.6636(3) 0.10433(19) 0.4246(3) 0.0476(9) Uani 1 1 d . . . H04D H 0.5928 0.0899 0.4004 0.057 Uiso 1 1 calc R . . H04E H 0.6726 0.1192 0.3683 0.057 Uiso 1 1 calc R . . C25 C 0.6872(3) 0.15739(19) 0.4975(3) 0.0500(9) Uani 1 1 d . . . H02E H 0.6391 0.1930 0.4663 0.060 Uiso 1 1 calc R . . H02F H 0.6770 0.1416 0.5526 0.060 Uiso 1 1 calc R . . C26 C 0.8037(3) 0.21308(17) 0.4614(3) 0.0468(9) Uani 1 1 d . . . H04J H 0.7429 0.2381 0.4184 0.056 Uiso 1 1 calc R . . H04K H 0.8163 0.1812 0.4209 0.056 Uiso 1 1 calc R . . C27 C 0.8908(3) 0.25584(19) 0.5082(3) 0.0497(9) Uani 1 1 d . . . C28 C 0.8191(3) 0.35674(18) 0.5269(3) 0.0519(9) Uani 1 1 d . . . H04F H 0.8137 0.3633 0.4612 0.062 Uiso 1 1 calc R . . H04G H 0.8512 0.3954 0.5662 0.062 Uiso 1 1 calc R . . C29 C 0.7165(3) 0.34996(19) 0.5175(3) 0.0552(10) Uani 1 1 d . . . H04H H 0.6794 0.3910 0.4962 0.066 Uiso 1 1 calc R . . H04I H 0.6784 0.3168 0.4684 0.066 Uiso 1 1 calc R . . C30 C 0.6397(3) 0.31829(18) 0.6168(3) 0.0501(9) Uani 1 1 d . . . C31 C 0.5471(3) 0.3456(2) 0.5572(4) 0.0730(13) Uani 1 1 d . . . H052 H 0.5402 0.3744 0.5069 0.088 Uiso 1 1 calc R . . C32 C 0.4643(4) 0.3308(2) 0.5711(4) 0.0813(15) Uani 1 1 d . . . H049 H 0.4003 0.3489 0.5292 0.098 Uiso 1 1 calc R . . C33 C 0.4733(3) 0.2907(2) 0.6438(4) 0.0738(13) Uani 1 1 d . . . H054 H 0.4169 0.2825 0.6550 0.089 Uiso 1 1 calc R . . C34 C 0.5662(3) 0.2619(2) 0.7019(3) 0.0529(9) Uani 1 1 d . . . H040 H 0.5724 0.2339 0.7528 0.063 Uiso 1 1 calc R . . C35 C 0.6499(3) 0.27287(17) 0.6873(2) 0.0414(8) Uani 1 1 d . . . C36 C 0.5740(3) 0.8531(2) 0.5079(3) 0.111(2) Uani 1 1 d GD . . H201 H 0.5515 0.8301 0.4485 0.134 Uiso 1 1 calc R . . C37 C 0.5942(3) 0.82097(15) 0.5937(4) 0.106(2) Uani 1 1 d GD . . H206 H 0.5856 0.7759 0.5930 0.127 Uiso 1 1 calc R . . C38 C 0.6271(3) 0.8547(2) 0.6806(3) 0.0907(17) Uani 1 1 d GD . . H205 H 0.6410 0.8328 0.7392 0.109 Uiso 1 1 calc R . . C39 C 0.6398(3) 0.92069(19) 0.6816(2) 0.0876(16) Uani 1 1 d GD . . H204 H 0.6622 0.9438 0.7410 0.105 Uiso 1 1 calc R . . C40 C 0.6195(3) 0.95286(15) 0.5958(3) 0.0927(17) Uani 1 1 d GD . . H203 H 0.6282 0.9979 0.5965 0.111 Uiso 1 1 calc R . . C41 C 0.5866(3) 0.9191(2) 0.5089(2) 0.1005(19) Uani 1 1 d GD . . H202 H 0.5728 0.9411 0.4503 0.121 Uiso 1 1 calc R . . C42 C 0.5216(3) 0.8966(2) 0.2389(3) 0.0642(11) Uani 1 1 d . . . H050 H 0.4970 0.8710 0.2742 0.077 Uiso 1 1 calc R . . C43 C 0.4758(3) 0.9538(2) 0.1985(3) 0.0608(11) Uani 1 1 d . . . H048 H 0.4176 0.9669 0.2039 0.073 Uiso 1 1 calc R . . C44 C 0.5131(3) 0.9920(2) 0.1507(3) 0.0582(10) Uani 1 1 d . . . H051 H 0.4822 1.0320 0.1246 0.070 Uiso 1 1 calc R . . C45 C 0.5954(3) 0.9720(2) 0.1406(3) 0.0526(9) Uani 1 1 d . . . H039 H 0.6216 0.9984 0.1075 0.063 Uiso 1 1 calc R . . C46 C 0.6404(3) 0.9138(2) 0.1783(3) 0.0513(9) Uani 1 1 d . . . H033 H 0.6965 0.8997 0.1701 0.062 Uiso 1 1 calc R . . C47 C 0.6039(3) 0.8768(2) 0.2274(3) 0.0583(10) Uani 1 1 d . . . H038 H 0.6352 0.8370 0.2540 0.070 Uiso 1 1 calc R . . N1 N 0.74225(18) 0.23998(13) 0.73658(17) 0.0327(6) Uani 1 1 d . . . N2 N 0.91927(17) 0.15897(11) 0.83369(16) 0.0247(5) Uani 1 1 d . . . N3 N 1.09387(17) 0.12356(11) 0.76579(15) 0.0241(5) Uani 1 1 d . . . N4 N 1.05566(17) 0.11110(11) 0.56550(16) 0.0271(5) Uani 1 1 d . . . O1 O 0.89202(16) 0.05329(10) 0.43150(14) 0.0343(5) Uani 1 1 d . . . O2 O 0.73121(16) 0.05368(10) 0.47300(15) 0.0366(5) Uani 1 1 d . . . O3 O 0.78734(19) 0.18115(11) 0.53444(16) 0.0434(6) Uani 1 1 d . . . O4 O 0.88154(18) 0.30373(11) 0.57061(16) 0.0442(6) Uani 1 1 d . . . O5 O 0.7265(2) 0.33199(14) 0.61078(19) 0.0575(7) Uani 1 1 d . . . K1 K 0.93396(6) 0.26858(4) 0.75073(5) 0.0443(2) Uani 1 1 d . . . K2 K 0.91508(5) 0.07242(3) 0.63424(5) 0.03534(18) Uani 1 1 d . . . H03A H 0.954(3) 0.2279(17) 0.551(3) 0.042 Uiso 1 1 d . . . H03B H 0.898(3) 0.2778(17) 0.458(3) 0.042 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C01 0.0255(14) 0.0445(18) 0.0235(13) -0.0068(13) 0.0097(12) -0.0025(13) C02 0.0281(14) 0.0324(15) 0.0237(13) -0.0025(12) 0.0114(12) -0.0030(12) C03 0.0321(15) 0.0344(16) 0.0360(16) -0.0053(13) 0.0172(13) -0.0098(13) C04 0.0381(16) 0.0234(14) 0.0342(15) -0.0014(12) 0.0190(13) -0.0042(12) C05 0.0293(14) 0.0229(13) 0.0173(12) -0.0006(10) 0.0113(11) -0.0010(11) C06 0.0277(14) 0.0209(13) 0.0199(12) 0.0007(10) 0.0079(11) -0.0003(11) C07 0.0317(15) 0.0245(14) 0.0217(13) -0.0017(11) 0.0088(12) -0.0008(12) C08 0.0457(18) 0.0349(16) 0.0204(13) -0.0030(12) 0.0133(13) -0.0016(14) C09 0.0344(15) 0.0244(14) 0.0244(13) 0.0030(11) 0.0112(12) 0.0034(12) C10 0.0360(17) 0.0358(17) 0.0378(17) 0.0040(14) 0.0110(14) 0.0087(14) C11 0.0205(12) 0.0249(13) 0.0203(12) 0.0023(10) 0.0065(10) 0.0022(11) C12 0.0280(14) 0.0247(14) 0.0248(13) -0.0025(11) 0.0077(11) -0.0035(11) C13 0.0292(15) 0.0260(14) 0.0312(14) 0.0037(12) 0.0124(12) -0.0024(12) C14 0.0218(13) 0.0265(14) 0.0241(13) 0.0024(11) 0.0084(11) -0.0001(11) C15 0.0228(13) 0.0299(15) 0.0277(14) 0.0082(12) 0.0122(12) 0.0029(11) C16 0.0379(16) 0.0238(14) 0.0256(14) 0.0048(11) 0.0168(12) 0.0050(12) C17 0.0424(17) 0.0315(16) 0.0329(15) 0.0035(13) 0.0214(14) -0.0013(13) C18 0.059(2) 0.0364(17) 0.0389(17) 0.0081(14) 0.0347(17) 0.0060(15) C19 0.071(2) 0.0368(18) 0.0318(16) -0.0023(14) 0.0329(17) 0.0022(17) C20 0.057(2) 0.0326(16) 0.0314(16) -0.0072(13) 0.0207(15) -0.0034(15) C21 0.0433(17) 0.0235(14) 0.0271(14) 0.0009(12) 0.0183(13) 0.0010(13) C22 0.0396(17) 0.0353(17) 0.0307(15) -0.0093(13) 0.0087(14) -0.0098(14) C23 0.0392(18) 0.0354(17) 0.0365(17) -0.0045(14) 0.0087(14) -0.0093(14) C24 0.0376(18) 0.056(2) 0.0389(18) 0.0015(16) 0.0092(15) 0.0056(16) C25 0.053(2) 0.052(2) 0.053(2) 0.0015(18) 0.0314(19) 0.0044(18) C26 0.070(2) 0.0400(19) 0.0420(19) 0.0074(15) 0.0359(19) 0.0071(18) C27 0.056(2) 0.051(2) 0.050(2) 0.0155(18) 0.0312(19) 0.0134(19) C28 0.067(3) 0.046(2) 0.0370(18) 0.0123(16) 0.0194(18) 0.0000(18) C29 0.065(3) 0.043(2) 0.043(2) 0.0119(16) 0.0130(18) 0.0030(19) C30 0.045(2) 0.044(2) 0.056(2) 0.0032(17) 0.0195(18) 0.0092(17) C31 0.051(3) 0.054(3) 0.094(4) 0.017(2) 0.017(2) 0.014(2) C32 0.052(3) 0.061(3) 0.118(4) 0.013(3) 0.028(3) 0.024(2) C33 0.050(2) 0.075(3) 0.103(4) 0.000(3) 0.041(3) 0.016(2) C34 0.0407(19) 0.061(2) 0.058(2) -0.0057(19) 0.0231(18) 0.0103(18) C35 0.0410(18) 0.0452(19) 0.0331(16) -0.0030(14) 0.0128(14) 0.0099(15) C36 0.097(5) 0.129(6) 0.081(4) -0.032(4) 0.018(4) 0.013(4) C37 0.057(3) 0.080(4) 0.137(6) -0.011(4) 0.008(3) 0.012(3) C38 0.081(4) 0.113(5) 0.079(4) 0.021(3) 0.038(3) 0.011(3) C39 0.093(4) 0.093(4) 0.066(3) -0.014(3) 0.029(3) 0.002(3) C40 0.089(4) 0.083(4) 0.082(4) 0.000(3) 0.019(3) -0.010(3) C41 0.108(5) 0.127(6) 0.070(4) -0.002(4) 0.044(3) -0.010(4) C42 0.059(3) 0.066(3) 0.072(3) -0.003(2) 0.034(2) -0.013(2) C43 0.039(2) 0.086(3) 0.056(2) -0.006(2) 0.0209(19) 0.002(2) C44 0.045(2) 0.067(3) 0.050(2) 0.002(2) 0.0114(18) 0.0122(19) C45 0.045(2) 0.067(3) 0.0398(19) 0.0042(18) 0.0148(17) 0.0049(19) C46 0.045(2) 0.065(3) 0.0376(18) -0.0051(18) 0.0146(16) 0.0090(18) C47 0.059(2) 0.046(2) 0.062(2) -0.0065(19) 0.021(2) 0.0021(19) N1 0.0296(13) 0.0401(15) 0.0238(12) 0.0013(11) 0.0084(10) 0.0071(11) N2 0.0270(12) 0.0247(12) 0.0201(11) 0.0012(9) 0.0091(9) -0.0010(9) N3 0.0243(11) 0.0262(12) 0.0186(10) 0.0007(9) 0.0072(9) -0.0014(9) N4 0.0279(12) 0.0307(13) 0.0231(11) 0.0004(10) 0.0122(10) -0.0016(10) O1 0.0371(11) 0.0382(12) 0.0263(10) -0.0070(9) 0.0135(9) -0.0098(9) O2 0.0355(12) 0.0403(12) 0.0270(10) 0.0026(9) 0.0084(9) -0.0022(10) O3 0.0628(16) 0.0395(13) 0.0370(12) 0.0041(10) 0.0308(12) -0.0019(11) O4 0.0529(14) 0.0412(13) 0.0377(12) 0.0069(10) 0.0203(11) -0.0017(11) O5 0.0470(15) 0.0643(17) 0.0525(15) 0.0264(13) 0.0157(13) 0.0085(13) K1 0.0458(4) 0.0418(4) 0.0439(4) 0.0219(3) 0.0196(3) 0.0029(3) K2 0.0298(3) 0.0461(4) 0.0246(3) 0.0022(3) 0.0080(3) -0.0099(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C01 N1 1.290(4) . ? C01 C02 1.422(4) . ? C01 K1 3.451(3) . ? C01 H023 0.9500 . ? C02 N2 1.378(4) . ? C02 C03 1.403(4) . ? C02 K1 3.419(3) . ? C03 C04 1.381(4) . ? C03 K2 3.475(3) . ? C03 H032 0.9500 . ? C04 C05 1.411(4) . ? C04 K2 3.388(3) . ? C04 H026 0.9500 . ? C05 N2 1.333(3) . ? C05 C06 1.520(4) . ? C05 K2 3.420(3) . ? C06 C11 1.522(4) . ? C06 C07 1.546(4) . ? C06 C09 1.551(4) . ? C07 C08 1.528(4) . ? C07 H02C 0.9900 . ? C07 H02D 0.9900 . ? C08 H03E 0.9800 . ? C08 H03F 0.9800 . ? C08 H03G 0.9800 . ? C09 C10 1.512(4) . ? C09 H02A 0.9900 . ? C09 H02B 0.9900 . ? C10 H04A 0.9800 . ? C10 H04B 0.9800 . ? C10 H04C 0.9800 . ? C11 N3 1.338(3) . ? C11 C12 1.418(4) . ? C12 C13 1.381(4) . ? C12 K1 3.468(3) . ? C12 H018 0.9500 . ? C13 C14 1.407(4) . ? C13 H016 0.9500 . ? C14 N3 1.375(3) . ? C14 C15 1.426(4) . ? C14 K2 3.427(3) . ? C15 N4 1.296(4) . ? C15 K2 3.487(3) . ? C15 H013 0.9500 . ? C16 C17 1.398(4) . ? C16 N4 1.405(3) . ? C16 C21 1.407(4) . ? C17 C18 1.401(4) . ? C17 H22 0.9500 . ? C18 C19 1.375(5) . ? C18 K1 3.348(3) 4_565 ? C18 H23 0.9500 . ? C19 C20 1.389(5) . ? C19 K1 3.298(3) 4_565 ? C19 K2 3.476(3) 3_756 ? C19 H24 0.9500 . ? C20 C21 1.393(4) . ? C20 K2 3.362(3) 3_756 ? C20 H25 0.9500 . ? C21 O1 1.369(4) . ? C22 O1 1.431(4) . ? C22 C23 1.508(5) . ? C22 H03C 0.9900 . ? C22 H03D 0.9900 . ? C23 O2 1.425(4) . ? C23 K2 3.523(3) . ? C23 H03H 0.9900 . ? C23 H03I 0.9900 . ? C24 O2 1.414(4) . ? C24 C25 1.502(5) . ? C24 H04D 0.9900 . ? C24 H04E 0.9900 . ? C25 O3 1.419(4) . ? C25 K2 3.539(4) . ? C25 H02E 0.9900 . ? C25 H02F 0.9900 . ? C26 O3 1.427(4) . ? C26 C27 1.463(6) . ? C26 H04J 0.9900 . ? C26 H04K 0.9900 . ? C27 O4 1.441(5) . ? C27 K1 3.509(4) . ? C27 H03A 1.04(4) . ? C27 H03B 0.95(4) . ? C28 O4 1.403(4) . ? C28 C29 1.476(6) . ? C28 H04F 0.9900 . ? C28 H04G 0.9900 . ? C29 O5 1.429(4) . ? C29 H04H 0.9900 . ? C29 H04I 0.9900 . ? C30 O5 1.371(5) . ? C30 C31 1.380(5) . ? C30 C35 1.400(5) . ? C31 C32 1.383(7) . ? C31 H052 0.9500 . ? C32 C33 1.357(7) . ? C32 H049 0.9500 . ? C33 C34 1.392(6) . ? C33 H054 0.9500 . ? C34 C35 1.387(5) . ? C34 H040 0.9500 . ? C35 N1 1.407(4) . ? C36 C37 1.3900 . ? C36 C41 1.3900 . ? C36 H201 0.9500 . ? C37 C38 1.3900 . ? C37 H206 0.9500 . ? C38 C39 1.3900 . ? C38 H205 0.9500 . ? C39 C40 1.3900 . ? C39 H204 0.9500 . ? C40 C41 1.3900 . ? C40 H203 0.9500 . ? C41 H202 0.9500 . ? C42 C43 1.375(6) . ? C42 C47 1.382(6) . ? C42 H050 0.9500 . ? C43 C44 1.370(6) . ? C43 H048 0.9500 . ? C44 C45 1.372(5) . ? C44 H051 0.9500 . ? C45 C46 1.381(6) . ? C45 H039 0.9500 . ? C46 C47 1.361(6) . ? C46 H033 0.9500 . ? C47 H038 0.9500 . ? N1 K1 2.830(3) . ? N2 K1 2.683(2) . ? N3 K2 2.715(2) . ? N4 K2 2.871(2) . ? O1 K2 3.017(2) . ? O2 K2 2.750(2) . ? O3 K2 2.908(2) . ? O4 K1 2.625(2) . ? O5 K1 3.134(3) . ? K1 C19 3.298(3) 4_566 ? K1 C18 3.348(3) 4_566 ? K2 C20 3.362(3) 3_756 ? K2 C19 3.476(3) 3_756 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C01 C02 124.8(3) . . ? N1 C01 K1 51.32(15) . . ? C02 C01 K1 76.82(17) . . ? N1 C01 H023 117.6 . . ? C02 C01 H023 117.6 . . ? K1 C01 H023 156.9 . . ? N2 C02 C03 110.4(3) . . ? N2 C02 C01 122.7(3) . . ? C03 C02 C01 127.0(3) . . ? N2 C02 K1 47.29(13) . . ? C03 C02 K1 149.0(2) . . ? C01 C02 K1 79.29(17) . . ? C04 C03 C02 106.1(3) . . ? C04 C03 K2 74.89(17) . . ? C02 C03 K2 82.16(17) . . ? C04 C03 H032 126.9 . . ? C02 C03 H032 126.9 . . ? K2 C03 H032 109.3 . . ? C03 C04 C05 106.2(3) . . ? C03 C04 K2 81.94(17) . . ? C05 C04 K2 79.34(15) . . ? C03 C04 H026 126.9 . . ? C05 C04 H026 126.9 . . ? K2 C04 H026 105.7 . . ? N2 C05 C04 111.4(2) . . ? N2 C05 C06 119.7(2) . . ? C04 C05 C06 128.9(2) . . ? N2 C05 K2 84.50(14) . . ? C04 C05 K2 76.75(15) . . ? C06 C05 K2 105.96(15) . . ? C05 C06 C11 107.5(2) . . ? C05 C06 C07 109.6(2) . . ? C11 C06 C07 109.2(2) . . ? C05 C06 C09 109.1(2) . . ? C11 C06 C09 110.0(2) . . ? C07 C06 C09 111.4(2) . . ? C08 C07 C06 114.1(2) . . ? C08 C07 H02C 108.7 . . ? C06 C07 H02C 108.7 . . ? C08 C07 H02D 108.7 . . ? C06 C07 H02D 108.7 . . ? H02C C07 H02D 107.6 . . ? C07 C08 H03E 109.5 . . ? C07 C08 H03F 109.5 . . ? H03E C08 H03F 109.5 . . ? C07 C08 H03G 109.5 . . ? H03E C08 H03G 109.5 . . ? H03F C08 H03G 109.5 . . ? C10 C09 C06 114.8(2) . . ? C10 C09 H02A 108.6 . . ? C06 C09 H02A 108.6 . . ? C10 C09 H02B 108.6 . . ? C06 C09 H02B 108.6 . . ? H02A C09 H02B 107.5 . . ? C09 C10 H04A 109.5 . . ? C09 C10 H04B 109.5 . . ? H04A C10 H04B 109.5 . . ? C09 C10 H04C 109.5 . . ? H04A C10 H04C 109.5 . . ? H04B C10 H04C 109.5 . . ? N3 C11 C12 111.1(2) . . ? N3 C11 C06 119.6(2) . . ? C12 C11 C06 129.2(2) . . ? C13 C12 C11 106.4(2) . . ? C13 C12 K1 85.42(17) . . ? C11 C12 K1 82.22(16) . . ? C13 C12 H018 126.8 . . ? C11 C12 H018 126.8 . . ? K1 C12 H018 100.3 . . ? C12 C13 C14 105.8(2) . . ? C12 C13 H016 127.1 . . ? C14 C13 H016 127.1 . . ? N3 C14 C13 110.8(2) . . ? N3 C14 C15 122.8(2) . . ? C13 C14 C15 126.3(3) . . ? N3 C14 K2 48.36(13) . . ? C13 C14 K2 144.57(19) . . ? C15 C14 K2 80.46(16) . . ? N4 C15 C14 123.5(2) . . ? N4 C15 K2 51.76(14) . . ? C14 C15 K2 75.75(15) . . ? N4 C15 H013 118.2 . . ? C14 C15 H013 118.2 . . ? K2 C15 H013 156.1 . . ? C17 C16 N4 124.5(3) . . ? C17 C16 C21 117.9(3) . . ? N4 C16 C21 117.5(2) . . ? C16 C17 C18 121.4(3) . . ? C16 C17 H22 119.3 . . ? C18 C17 H22 119.3 . . ? C19 C18 C17 119.5(3) . . ? C19 C18 K1 76.0(2) . 4_565 ? C17 C18 K1 93.05(19) . 4_565 ? C19 C18 H23 120.3 . . ? C17 C18 H23 120.3 . . ? K1 C18 H23 100.8 4_565 . ? C18 C19 C20 120.6(3) . . ? C18 C19 K1 80.11(19) . 4_565 ? C20 C19 K1 91.3(2) . 4_565 ? C18 C19 K2 99.7(2) . 3_756 ? C20 C19 K2 73.74(19) . 3_756 ? K1 C19 K2 162.65(11) 4_565 3_756 ? C18 C19 H24 119.7 . . ? C20 C19 H24 119.7 . . ? K1 C19 H24 98.7 4_565 . ? K2 C19 H24 96.4 3_756 . ? C19 C20 C21 120.0(3) . . ? C19 C20 K2 82.9(2) . 3_756 ? C21 C20 K2 94.3(2) . 3_756 ? C19 C20 H25 120.0 . . ? C21 C20 H25 120.0 . . ? K2 C20 H25 92.8 3_756 . ? O1 C21 C20 123.6(3) . . ? O1 C21 C16 115.7(2) . . ? C20 C21 C16 120.7(3) . . ? O1 C22 C23 107.3(2) . . ? O1 C22 H03C 110.2 . . ? C23 C22 H03C 110.2 . . ? O1 C22 H03D 110.2 . . ? C23 C22 H03D 110.2 . . ? H03C C22 H03D 108.5 . . ? O2 C23 C22 114.0(3) . . ? O2 C23 K2 46.76(13) . . ? C22 C23 K2 92.66(18) . . ? O2 C23 H03H 108.7 . . ? C22 C23 H03H 108.7 . . ? K2 C23 H03H 153.8 . . ? O2 C23 H03I 108.7 . . ? C22 C23 H03I 108.7 . . ? K2 C23 H03I 78.2 . . ? H03H C23 H03I 107.6 . . ? O2 C24 C25 107.1(3) . . ? O2 C24 H04D 110.3 . . ? C25 C24 H04D 110.3 . . ? O2 C24 H04E 110.3 . . ? C25 C24 H04E 110.3 . . ? H04D C24 H04E 108.6 . . ? O3 C25 C24 113.5(3) . . ? O3 C25 K2 52.70(16) . . ? C24 C25 K2 84.5(2) . . ? O3 C25 H02E 108.9 . . ? C24 C25 H02E 108.9 . . ? K2 C25 H02E 161.3 . . ? O3 C25 H02F 108.9 . . ? C24 C25 H02F 108.9 . . ? K2 C25 H02F 78.9 . . ? H02E C25 H02F 107.7 . . ? O3 C26 C27 109.4(3) . . ? O3 C26 H04J 109.8 . . ? C27 C26 H04J 109.8 . . ? O3 C26 H04K 109.8 . . ? C27 C26 H04K 109.8 . . ? H04J C26 H04K 108.2 . . ? O4 C27 C26 114.6(3) . . ? O4 C27 K1 42.14(15) . . ? C26 C27 K1 104.9(2) . . ? O4 C27 H03A 107.9(19) . . ? C26 C27 H03A 107.9(19) . . ? K1 C27 H03A 72.9(19) . . ? O4 C27 H03B 107(2) . . ? C26 C27 H03B 108(2) . . ? K1 C27 H03B 143(2) . . ? H03A C27 H03B 112(3) . . ? O4 C28 C29 113.5(3) . . ? O4 C28 H04F 108.9 . . ? C29 C28 H04F 108.9 . . ? O4 C28 H04G 108.9 . . ? C29 C28 H04G 108.9 . . ? H04F C28 H04G 107.7 . . ? O5 C29 C28 107.9(3) . . ? O5 C29 H04H 110.1 . . ? C28 C29 H04H 110.1 . . ? O5 C29 H04I 110.1 . . ? C28 C29 H04I 110.1 . . ? H04H C29 H04I 108.4 . . ? O5 C30 C31 123.6(4) . . ? O5 C30 C35 115.3(3) . . ? C31 C30 C35 121.0(4) . . ? C30 C31 C32 119.5(5) . . ? C30 C31 H052 120.2 . . ? C32 C31 H052 120.2 . . ? C33 C32 C31 121.0(4) . . ? C33 C32 H049 119.5 . . ? C31 C32 H049 119.5 . . ? C32 C33 C34 119.2(4) . . ? C32 C33 H054 120.4 . . ? C34 C33 H054 120.4 . . ? C35 C34 C33 121.8(4) . . ? C35 C34 H040 119.1 . . ? C33 C34 H040 119.1 . . ? C34 C35 C30 117.2(3) . . ? C34 C35 N1 124.1(3) . . ? C30 C35 N1 118.7(3) . . ? C37 C36 C41 120.0 . . ? C37 C36 H201 120.0 . . ? C41 C36 H201 120.0 . . ? C38 C37 C36 120.0 . . ? C38 C37 H206 120.0 . . ? C36 C37 H206 120.0 . . ? C37 C38 C39 120.0 . . ? C37 C38 H205 120.0 . . ? C39 C38 H205 120.0 . . ? C38 C39 C40 120.0 . . ? C38 C39 H204 120.0 . . ? C40 C39 H204 120.0 . . ? C39 C40 C41 120.0 . . ? C39 C40 H203 120.0 . . ? C41 C40 H203 120.0 . . ? C40 C41 C36 120.0 . . ? C40 C41 H202 120.0 . . ? C36 C41 H202 120.0 . . ? C43 C42 C47 119.1(4) . . ? C43 C42 H050 120.5 . . ? C47 C42 H050 120.5 . . ? C44 C43 C42 120.7(4) . . ? C44 C43 H048 119.6 . . ? C42 C43 H048 119.6 . . ? C43 C44 C45 119.5(4) . . ? C43 C44 H051 120.2 . . ? C45 C44 H051 120.2 . . ? C44 C45 C46 120.4(4) . . ? C44 C45 H039 119.8 . . ? C46 C45 H039 119.8 . . ? C47 C46 C45 119.6(4) . . ? C47 C46 H033 120.2 . . ? C45 C46 H033 120.2 . . ? C46 C47 C42 120.7(4) . . ? C46 C47 H038 119.7 . . ? C42 C47 H038 119.7 . . ? C01 N1 C35 116.3(3) . . ? C01 N1 K1 107.83(18) . . ? C35 N1 K1 129.8(2) . . ? C05 N2 C02 105.9(2) . . ? C05 N2 K1 136.00(18) . . ? C02 N2 K1 110.54(17) . . ? C11 N3 C14 105.8(2) . . ? C11 N3 K2 131.10(17) . . ? C14 N3 K2 109.40(16) . . ? C15 N4 C16 119.0(2) . . ? C15 N4 K2 107.48(17) . . ? C16 N4 K2 128.20(18) . . ? C21 O1 C22 116.9(2) . . ? C21 O1 K2 124.98(16) . . ? C22 O1 K2 117.78(17) . . ? C24 O2 C23 114.6(2) . . ? C24 O2 K2 122.77(19) . . ? C23 O2 K2 111.05(18) . . ? C25 O3 C26 112.3(3) . . ? C25 O3 K2 104.45(19) . . ? C26 O3 K2 118.4(2) . . ? C28 O4 C27 118.3(3) . . ? C28 O4 K1 122.5(2) . . ? C27 O4 K1 116.2(2) . . ? C30 O5 C29 117.5(3) . . ? C30 O5 K1 121.8(2) . . ? C29 O5 K1 114.6(2) . . ? O4 K1 N2 134.09(8) . . ? O4 K1 N1 100.53(8) . . ? N2 K1 N1 63.48(7) . . ? O4 K1 O5 55.60(7) . . ? N2 K1 O5 114.70(7) . . ? N1 K1 O5 52.82(7) . . ? O4 K1 C19 78.33(8) . 4_566 ? N2 K1 C19 147.43(8) . 4_566 ? N1 K1 C19 121.72(9) . 4_566 ? O5 K1 C19 84.43(9) . 4_566 ? O4 K1 C18 93.93(8) . 4_566 ? N2 K1 C18 128.15(8) . 4_566 ? N1 K1 C18 136.37(8) . 4_566 ? O5 K1 C18 108.16(9) . 4_566 ? C19 K1 C18 23.86(9) 4_566 4_566 ? O4 K1 C02 118.88(7) . . ? N2 K1 C02 22.17(7) . . ? N1 K1 C02 44.00(7) . . ? O5 K1 C02 92.94(7) . . ? C19 K1 C02 156.82(8) 4_566 . ? C18 K1 C02 147.16(8) 4_566 . ? O4 K1 C01 106.64(7) . . ? N2 K1 C01 45.10(7) . . ? N1 K1 C01 20.84(7) . . ? O5 K1 C01 69.61(7) . . ? C19 K1 C01 141.94(8) 4_566 . ? C18 K1 C01 150.90(7) 4_566 . ? C02 K1 C01 23.89(7) . . ? O4 K1 C12 112.67(8) . . ? N2 K1 C12 74.03(7) . . ? N1 K1 C12 137.25(7) . . ? O5 K1 C12 168.17(7) . . ? C19 K1 C12 91.74(8) 4_566 . ? C18 K1 C12 68.97(8) 4_566 . ? C02 K1 C12 94.92(7) . . ? C01 K1 C12 118.76(7) . . ? O4 K1 C27 21.61(8) . . ? N2 K1 C27 115.52(9) . . ? N1 K1 C27 102.85(9) . . ? O5 K1 C27 70.14(8) . . ? C19 K1 C27 95.33(9) 4_566 . ? C18 K1 C27 105.30(9) 4_566 . ? C02 K1 C27 105.45(8) . . ? C01 K1 C27 101.06(8) . . ? C12 K1 C27 99.17(8) . . ? N3 K2 O2 163.14(7) . . ? N3 K2 N4 62.20(7) . . ? O2 K2 N4 107.33(7) . . ? N3 K2 O3 105.39(7) . . ? O2 K2 O3 59.76(7) . . ? N4 K2 O3 89.73(7) . . ? N3 K2 O1 115.49(6) . . ? O2 K2 O1 56.86(6) . . ? N4 K2 O1 53.45(6) . . ? O3 K2 O1 79.67(6) . . ? N3 K2 C20 82.21(8) . 3_756 ? O2 K2 C20 110.64(8) . 3_756 ? N4 K2 C20 83.09(8) . 3_756 ? O3 K2 C20 165.69(7) . 3_756 ? O1 K2 C20 86.11(7) . 3_756 ? N3 K2 C04 75.43(7) . . ? O2 K2 C04 115.68(7) . . ? N4 K2 C04 136.94(7) . . ? O3 K2 C04 109.47(7) . . ? O1 K2 C04 164.11(7) . . ? C20 K2 C04 84.01(7) 3_756 . ? N3 K2 C05 55.13(6) . . ? O2 K2 C05 131.57(7) . . ? N4 K2 C05 117.07(7) . . ? O3 K2 C05 100.78(7) . . ? O1 K2 C05 170.50(6) . . ? C20 K2 C05 93.52(7) 3_756 . ? C04 K2 C05 23.91(7) . . ? N3 K2 C14 22.24(6) . . ? O2 K2 C14 141.86(7) . . ? N4 K2 C14 43.66(6) . . ? O3 K2 C14 91.18(7) . . ? O1 K2 C14 96.56(6) . . ? C20 K2 C14 92.12(8) 3_756 . ? C04 K2 C14 96.21(7) . . ? C05 K2 C14 73.96(6) . . ? N3 K2 C03 92.87(7) . . ? O2 K2 C03 95.03(7) . . ? N4 K2 C03 154.08(7) . . ? O3 K2 C03 90.40(7) . . ? O1 K2 C03 151.48(7) . . ? C20 K2 C03 101.47(8) 3_756 . ? C04 K2 C03 23.17(7) . . ? C05 K2 C03 37.76(7) . . ? C14 K2 C03 110.42(7) . . ? N3 K2 C19 94.97(8) . 3_756 ? O2 K2 C19 100.92(8) . 3_756 ? N4 K2 C19 106.35(8) . 3_756 ? O3 K2 C19 158.42(8) . 3_756 ? O1 K2 C19 98.18(7) . 3_756 ? C20 K2 C19 23.36(8) 3_756 3_756 ? C04 K2 C19 68.43(7) . 3_756 ? C05 K2 C19 84.87(7) . 3_756 ? C14 K2 C19 110.37(8) . 3_756 ? C03 K2 C19 81.36(7) . 3_756 ? N3 K2 C15 44.62(6) . . ? O2 K2 C15 121.80(7) . . ? N4 K2 C15 20.75(7) . . ? O3 K2 C15 85.94(7) . . ? O1 K2 C15 72.80(6) . . ? C20 K2 C15 91.50(8) 3_756 . ? C04 K2 C15 119.80(7) . . ? C05 K2 C15 97.74(7) . . ? C14 K2 C15 23.79(6) . . ? C03 K2 C15 133.55(7) . . ? C19 K2 C15 114.15(8) 3_756 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C01 C02 N2 0.5(4) . . . . ? K1 C01 C02 N2 19.8(2) . . . . ? N1 C01 C02 C03 179.0(3) . . . . ? K1 C01 C02 C03 -161.7(3) . . . . ? N1 C01 C02 K1 -19.3(3) . . . . ? N2 C02 C03 C04 0.7(3) . . . . ? C01 C02 C03 C04 -178.0(3) . . . . ? K1 C02 C03 C04 38.9(5) . . . . ? N2 C02 C03 K2 -70.97(19) . . . . ? C01 C02 C03 K2 110.3(3) . . . . ? K1 C02 C03 K2 -32.8(4) . . . . ? C02 C03 C04 C05 -0.6(3) . . . . ? K2 C03 C04 C05 76.37(19) . . . . ? C02 C03 C04 K2 -77.0(2) . . . . ? C03 C04 C05 N2 0.3(3) . . . . ? K2 C04 C05 N2 78.57(19) . . . . ? C03 C04 C05 C06 -178.3(3) . . . . ? K2 C04 C05 C06 -100.0(3) . . . . ? C03 C04 C05 K2 -78.3(2) . . . . ? N2 C05 C06 C11 -54.6(3) . . . . ? C04 C05 C06 C11 123.8(3) . . . . ? K2 C05 C06 C11 38.2(2) . . . . ? N2 C05 C06 C07 64.0(3) . . . . ? C04 C05 C06 C07 -117.5(3) . . . . ? K2 C05 C06 C07 156.79(16) . . . . ? N2 C05 C06 C09 -173.8(2) . . . . ? C04 C05 C06 C09 4.6(4) . . . . ? K2 C05 C06 C09 -81.1(2) . . . . ? C05 C06 C07 C08 64.3(3) . . . . ? C11 C06 C07 C08 -178.1(2) . . . . ? C09 C06 C07 C08 -56.5(3) . . . . ? C05 C06 C09 C10 -177.0(2) . . . . ? C11 C06 C09 C10 65.3(3) . . . . ? C07 C06 C09 C10 -56.0(3) . . . . ? C05 C06 C11 N3 -54.2(3) . . . . ? C07 C06 C11 N3 -173.1(2) . . . . ? C09 C06 C11 N3 64.5(3) . . . . ? C05 C06 C11 C12 121.7(3) . . . . ? C07 C06 C11 C12 2.9(4) . . . . ? C09 C06 C11 C12 -119.6(3) . . . . ? N3 C11 C12 C13 0.5(3) . . . . ? C06 C11 C12 C13 -175.7(3) . . . . ? N3 C11 C12 K1 83.4(2) . . . . ? C06 C11 C12 K1 -92.8(3) . . . . ? C11 C12 C13 C14 -0.2(3) . . . . ? K1 C12 C13 C14 -80.7(2) . . . . ? C12 C13 C14 N3 -0.1(3) . . . . ? C12 C13 C14 C15 178.9(3) . . . . ? C12 C13 C14 K2 46.1(4) . . . . ? N3 C14 C15 N4 3.5(4) . . . . ? C13 C14 C15 N4 -175.4(3) . . . . ? K2 C14 C15 N4 -20.9(3) . . . . ? N3 C14 C15 K2 24.5(2) . . . . ? C13 C14 C15 K2 -154.4(3) . . . . ? N4 C16 C17 C18 175.5(3) . . . . ? C21 C16 C17 C18 -0.1(4) . . . . ? C16 C17 C18 C19 0.6(5) . . . . ? C16 C17 C18 K1 76.2(3) . . . 4_565 ? C17 C18 C19 C20 -0.1(5) . . . . ? K1 C18 C19 C20 -85.6(3) 4_565 . . . ? C17 C18 C19 K1 85.5(3) . . . 4_565 ? C17 C18 C19 K2 -76.8(3) . . . 3_756 ? K1 C18 C19 K2 -162.39(11) 4_565 . . 3_756 ? C18 C19 C20 C21 -0.9(5) . . . . ? K1 C19 C20 C21 -80.2(3) 4_565 . . . ? K2 C19 C20 C21 90.9(3) 3_756 . . . ? C18 C19 C20 K2 -91.8(3) . . . 3_756 ? K1 C19 C20 K2 -171.11(9) 4_565 . . 3_756 ? C19 C20 C21 O1 -178.8(3) . . . . ? K2 C20 C21 O1 -94.5(3) 3_756 . . . ? C19 C20 C21 C16 1.4(5) . . . . ? K2 C20 C21 C16 85.7(3) 3_756 . . . ? C17 C16 C21 O1 179.3(3) . . . . ? N4 C16 C21 O1 3.4(4) . . . . ? C17 C16 C21 C20 -0.9(4) . . . . ? N4 C16 C21 C20 -176.8(3) . . . . ? O1 C22 C23 O2 49.9(4) . . . . ? O1 C22 C23 K2 6.8(2) . . . . ? O2 C24 C25 O3 60.8(4) . . . . ? O2 C24 C25 K2 15.6(2) . . . . ? O3 C26 C27 O4 -58.4(4) . . . . ? O3 C26 C27 K1 -14.7(3) . . . . ? O4 C28 C29 O5 50.8(4) . . . . ? O5 C30 C31 C32 -177.4(4) . . . . ? C35 C30 C31 C32 3.9(7) . . . . ? C30 C31 C32 C33 1.3(8) . . . . ? C31 C32 C33 C34 -3.2(8) . . . . ? C32 C33 C34 C35 -0.1(7) . . . . ? C33 C34 C35 C30 5.0(6) . . . . ? C33 C34 C35 N1 -172.9(4) . . . . ? O5 C30 C35 C34 174.3(3) . . . . ? C31 C30 C35 C34 -6.9(6) . . . . ? O5 C30 C35 N1 -7.6(5) . . . . ? C31 C30 C35 N1 171.1(4) . . . . ? C41 C36 C37 C38 0.0 . . . . ? C36 C37 C38 C39 0.0 . . . . ? C37 C38 C39 C40 0.0 . . . . ? C38 C39 C40 C41 0.0 . . . . ? C39 C40 C41 C36 0.0 . . . . ? C37 C36 C41 C40 0.0 . . . . ? C47 C42 C43 C44 -2.4(7) . . . . ? C42 C43 C44 C45 1.9(6) . . . . ? C43 C44 C45 C46 0.0(6) . . . . ? C44 C45 C46 C47 -1.3(6) . . . . ? C45 C46 C47 C42 0.7(6) . . . . ? C43 C42 C47 C46 1.1(6) . . . . ? C02 C01 N1 C35 179.7(3) . . . . ? K1 C01 N1 C35 155.4(3) . . . . ? C02 C01 N1 K1 24.3(3) . . . . ? C34 C35 N1 C01 44.9(4) . . . . ? C30 C35 N1 C01 -132.9(3) . . . . ? C34 C35 N1 K1 -166.1(3) . . . . ? C30 C35 N1 K1 16.0(4) . . . . ? C04 C05 N2 C02 0.2(3) . . . . ? C06 C05 N2 C02 178.9(2) . . . . ? K2 C05 N2 C02 73.60(17) . . . . ? C04 C05 N2 K1 -145.0(2) . . . . ? C06 C05 N2 K1 33.7(4) . . . . ? K2 C05 N2 K1 -71.5(2) . . . . ? C03 C02 N2 C05 -0.6(3) . . . . ? C01 C02 N2 C05 178.2(2) . . . . ? K1 C02 N2 C05 -154.9(2) . . . . ? C03 C02 N2 K1 154.34(19) . . . . ? C01 C02 N2 K1 -26.9(3) . . . . ? C12 C11 N3 C14 -0.5(3) . . . . ? C06 C11 N3 C14 176.1(2) . . . . ? C12 C11 N3 K2 -135.4(2) . . . . ? C06 C11 N3 K2 41.2(3) . . . . ? C13 C14 N3 C11 0.4(3) . . . . ? C15 C14 N3 C11 -178.6(2) . . . . ? K2 C14 N3 C11 -145.5(2) . . . . ? C13 C14 N3 K2 145.93(19) . . . . ? C15 C14 N3 K2 -33.1(3) . . . . ? C14 C15 N4 C16 -177.5(3) . . . . ? K2 C15 N4 C16 156.4(3) . . . . ? C14 C15 N4 K2 26.2(3) . . . . ? C17 C16 N4 C15 28.6(4) . . . . ? C21 C16 N4 C15 -155.8(3) . . . . ? C17 C16 N4 K2 179.5(2) . . . . ? C21 C16 N4 K2 -4.9(4) . . . . ? C20 C21 O1 C22 -7.7(4) . . . . ? C16 C21 O1 C22 172.2(3) . . . . ? C20 C21 O1 K2 179.3(2) . . . . ? C16 C21 O1 K2 -0.9(3) . . . . ? C23 C22 O1 C21 177.5(3) . . . . ? C23 C22 O1 K2 -8.9(3) . . . . ? C25 C24 O2 C23 -164.1(3) . . . . ? C25 C24 O2 K2 -24.2(4) . . . . ? C22 C23 O2 C24 75.0(4) . . . . ? K2 C23 O2 C24 144.5(3) . . . . ? C22 C23 O2 K2 -69.5(3) . . . . ? C24 C25 O3 C26 66.9(4) . . . . ? K2 C25 O3 C26 129.5(3) . . . . ? C24 C25 O3 K2 -62.6(3) . . . . ? C27 C26 O3 C25 159.1(3) . . . . ? C27 C26 O3 K2 -79.1(3) . . . . ? C29 C28 O4 C27 96.8(4) . . . . ? C29 C28 O4 K1 -63.1(4) . . . . ? C26 C27 O4 C28 -76.0(4) . . . . ? K1 C27 O4 C28 -161.1(4) . . . . ? C26 C27 O4 K1 85.1(3) . . . . ? C31 C30 O5 C29 -29.5(6) . . . . ? C35 C30 O5 C29 149.3(3) . . . . ? C31 C30 O5 K1 179.4(3) . . . . ? C35 C30 O5 K1 -1.9(4) . . . . ? C28 C29 O5 C30 -175.1(3) . . . . ? C28 C29 O5 K1 -21.9(4) . . . . ? C28 O4 K1 N2 125.0(2) . . . . ? C27 O4 K1 N2 -35.2(3) . . . . ? C28 O4 K1 N1 61.9(3) . . . . ? C27 O4 K1 N1 -98.3(2) . . . . ? C28 O4 K1 O5 32.6(2) . . . . ? C27 O4 K1 O5 -127.6(3) . . . . ? C28 O4 K1 C19 -58.6(3) . . . 4_566 ? C27 O4 K1 C19 141.2(2) . . . 4_566 ? C28 O4 K1 C18 -76.8(3) . . . 4_566 ? C27 O4 K1 C18 123.0(2) . . . 4_566 ? C28 O4 K1 C02 104.7(2) . . . . ? C27 O4 K1 C02 -55.5(2) . . . . ? C28 O4 K1 C01 82.4(3) . . . . ? C27 O4 K1 C01 -77.8(2) . . . . ? C28 O4 K1 C12 -145.6(2) . . . . ? C27 O4 K1 C12 54.2(2) . . . . ? C28 O4 K1 C27 160.2(4) . . . . ? C05 N2 K1 O4 90.6(3) . . . . ? C02 N2 K1 O4 -53.5(2) . . . . ? C05 N2 K1 N1 169.1(3) . . . . ? C02 N2 K1 N1 25.06(17) . . . . ? C05 N2 K1 O5 155.7(2) . . . . ? C02 N2 K1 O5 11.7(2) . . . . ? C05 N2 K1 C19 -82.8(3) . . . 4_566 ? C02 N2 K1 C19 133.12(19) . . . 4_566 ? C05 N2 K1 C18 -61.4(3) . . . 4_566 ? C02 N2 K1 C18 154.59(16) . . . 4_566 ? C05 N2 K1 C02 144.0(3) . . . . ? C05 N2 K1 C01 156.8(3) . . . . ? C02 N2 K1 C01 12.80(16) . . . . ? C05 N2 K1 C12 -15.7(2) . . . . ? C02 N2 K1 C12 -159.78(18) . . . . ? C05 N2 K1 C27 77.0(3) . . . . ? C02 N2 K1 C27 -67.07(19) . . . . ? C01 N1 K1 O4 109.29(19) . . . . ? C35 N1 K1 O4 -41.7(3) . . . . ? C01 N1 K1 N2 -24.99(17) . . . . ? C35 N1 K1 N2 -175.9(3) . . . . ? C01 N1 K1 O5 139.7(2) . . . . ? C35 N1 K1 O5 -11.2(2) . . . . ? C01 N1 K1 C19 -168.01(17) . . . 4_566 ? C35 N1 K1 C19 41.0(3) . . . 4_566 ? C01 N1 K1 C18 -143.49(18) . . . 4_566 ? C35 N1 K1 C18 65.6(3) . . . 4_566 ? C01 N1 K1 C02 -11.69(16) . . . . ? C35 N1 K1 C02 -162.6(3) . . . . ? C35 N1 K1 C01 -150.9(4) . . . . ? C01 N1 K1 C12 -31.9(2) . . . . ? C35 N1 K1 C12 177.2(2) . . . . ? C01 N1 K1 C27 87.34(19) . . . . ? C35 N1 K1 C27 -63.6(3) . . . . ? C30 O5 K1 O4 149.0(3) . . . . ? C29 O5 K1 O4 -2.9(2) . . . . ? C30 O5 K1 N2 21.2(3) . . . . ? C29 O5 K1 N2 -130.7(2) . . . . ? C30 O5 K1 N1 6.2(2) . . . . ? C29 O5 K1 N1 -145.8(3) . . . . ? C30 O5 K1 C19 -131.3(3) . . . 4_566 ? C29 O5 K1 C19 76.7(2) . . . 4_566 ? C30 O5 K1 C18 -128.9(3) . . . 4_566 ? C29 O5 K1 C18 79.2(3) . . . 4_566 ? C30 O5 K1 C02 25.6(3) . . . . ? C29 O5 K1 C02 -126.3(2) . . . . ? C30 O5 K1 C01 20.4(3) . . . . ? C29 O5 K1 C01 -131.6(3) . . . . ? C30 O5 K1 C12 157.2(3) . . . . ? C29 O5 K1 C12 5.2(5) . . . . ? C30 O5 K1 C27 131.0(3) . . . . ? C29 O5 K1 C27 -21.0(2) . . . . ? N2 C02 K1 O4 138.78(17) . . . . ? C03 C02 K1 O4 86.8(4) . . . . ? C01 C02 K1 O4 -64.03(17) . . . . ? C03 C02 K1 N2 -52.0(4) . . . . ? C01 C02 K1 N2 157.2(3) . . . . ? N2 C02 K1 N1 -146.9(2) . . . . ? C03 C02 K1 N1 161.1(4) . . . . ? C01 C02 K1 N1 10.26(14) . . . . ? N2 C02 K1 O5 -169.37(18) . . . . ? C03 C02 K1 O5 138.7(4) . . . . ? C01 C02 K1 O5 -12.18(16) . . . . ? N2 C02 K1 C19 -86.7(3) . . . 4_566 ? C03 C02 K1 C19 -138.7(4) . . . 4_566 ? C01 C02 K1 C19 70.5(3) . . . 4_566 ? N2 C02 K1 C18 -38.5(2) . . . 4_566 ? C03 C02 K1 C18 -90.4(4) . . . 4_566 ? C01 C02 K1 C18 118.73(19) . . . 4_566 ? N2 C02 K1 C01 -157.2(3) . . . . ? C03 C02 K1 C01 150.8(5) . . . . ? N2 C02 K1 C12 19.48(18) . . . . ? C03 C02 K1 C12 -32.5(4) . . . . ? C01 C02 K1 C12 176.68(16) . . . . ? N2 C02 K1 C27 120.42(18) . . . . ? C03 C02 K1 C27 68.5(4) . . . . ? C01 C02 K1 C27 -82.38(17) . . . . ? N1 C01 K1 O4 -75.59(19) . . . . ? C02 C01 K1 O4 124.76(16) . . . . ? N1 C01 K1 N2 147.7(2) . . . . ? C02 C01 K1 N2 -11.92(14) . . . . ? C02 C01 K1 N1 -159.7(3) . . . . ? N1 C01 K1 O5 -33.33(18) . . . . ? C02 C01 K1 O5 167.01(17) . . . . ? N1 C01 K1 C19 16.7(2) . . . 4_566 ? C02 C01 K1 C19 -143.00(17) . . . 4_566 ? N1 C01 K1 C18 57.6(3) . . . 4_566 ? C02 C01 K1 C18 -102.1(2) . . . 4_566 ? N1 C01 K1 C02 159.7(3) . . . . ? N1 C01 K1 C12 155.88(18) . . . . ? C02 C01 K1 C12 -3.78(18) . . . . ? N1 C01 K1 C27 -97.11(19) . . . . ? C02 C01 K1 C27 103.23(16) . . . . ? C13 C12 K1 O4 -0.10(19) . . . . ? C11 C12 K1 O4 -107.34(16) . . . . ? C13 C12 K1 N2 131.57(18) . . . . ? C11 C12 K1 N2 24.33(15) . . . . ? C13 C12 K1 N1 137.95(17) . . . . ? C11 C12 K1 N1 30.7(2) . . . . ? C13 C12 K1 O5 -7.4(5) . . . . ? C11 C12 K1 O5 -114.6(4) . . . . ? C13 C12 K1 C19 -78.17(17) . . . 4_566 ? C11 C12 K1 C19 174.59(16) . . . 4_566 ? C13 C12 K1 C18 -85.45(17) . . . 4_566 ? C11 C12 K1 C18 167.31(17) . . . 4_566 ? C13 C12 K1 C02 124.05(17) . . . . ? C11 C12 K1 C02 16.81(16) . . . . ? C13 C12 K1 C01 125.58(17) . . . . ? C11 C12 K1 C01 18.34(18) . . . . ? C13 C12 K1 C27 17.51(18) . . . . ? C11 C12 K1 C27 -89.73(17) . . . . ? C26 C27 K1 O4 -110.4(3) . . . . ? O4 C27 K1 N2 152.7(2) . . . . ? C26 C27 K1 N2 42.2(3) . . . . ? O4 C27 K1 N1 86.2(2) . . . . ? C26 C27 K1 N1 -24.3(2) . . . . ? O4 C27 K1 O5 44.0(2) . . . . ? C26 C27 K1 O5 -66.4(2) . . . . ? O4 C27 K1 C19 -38.1(2) . . . 4_566 ? C26 C27 K1 C19 -148.5(2) . . . 4_566 ? O4 C27 K1 C18 -60.1(2) . . . 4_566 ? C26 C27 K1 C18 -170.6(2) . . . 4_566 ? O4 C27 K1 C02 131.5(2) . . . . ? C26 C27 K1 C02 21.1(2) . . . . ? O4 C27 K1 C01 107.4(2) . . . . ? C26 C27 K1 C01 -3.0(2) . . . . ? O4 C27 K1 C12 -130.7(2) . . . . ? C26 C27 K1 C12 118.8(2) . . . . ? C11 N3 K2 O2 108.5(3) . . . . ? C14 N3 K2 O2 -25.2(3) . . . . ? C11 N3 K2 N4 163.1(3) . . . . ? C14 N3 K2 N4 29.39(16) . . . . ? C11 N3 K2 O3 81.8(2) . . . . ? C14 N3 K2 O3 -51.95(18) . . . . ? C11 N3 K2 O1 167.5(2) . . . . ? C14 N3 K2 O1 33.76(19) . . . . ? C11 N3 K2 C20 -110.6(2) . . . 3_756 ? C14 N3 K2 C20 115.65(18) . . . 3_756 ? C11 N3 K2 C04 -24.8(2) . . . . ? C14 N3 K2 C04 -158.55(19) . . . . ? C11 N3 K2 C05 -10.8(2) . . . . ? C14 N3 K2 C05 -144.5(2) . . . . ? C11 N3 K2 C14 133.7(3) . . . . ? C11 N3 K2 C03 -9.4(2) . . . . ? C14 N3 K2 C03 -143.16(18) . . . . ? C11 N3 K2 C19 -91.0(2) . . . 3_756 ? C14 N3 K2 C19 135.27(17) . . . 3_756 ? C11 N3 K2 C15 149.2(3) . . . . ? C14 N3 K2 C15 15.50(16) . . . . ? C24 O2 K2 N3 -33.5(4) . . . . ? C23 O2 K2 N3 107.6(3) . . . . ? C24 O2 K2 N4 -82.6(2) . . . . ? C23 O2 K2 N4 58.50(19) . . . . ? C24 O2 K2 O3 -3.4(2) . . . . ? C23 O2 K2 O3 137.7(2) . . . . ? C24 O2 K2 O1 -101.0(2) . . . . ? C23 O2 K2 O1 40.06(18) . . . . ? C24 O2 K2 C20 -171.6(2) . . . 3_756 ? C23 O2 K2 C20 -30.5(2) . . . 3_756 ? C24 O2 K2 C04 95.1(2) . . . . ? C23 O2 K2 C04 -123.80(18) . . . . ? C24 O2 K2 C05 73.4(2) . . . . ? C23 O2 K2 C05 -145.46(18) . . . . ? C24 O2 K2 C14 -48.7(3) . . . . ? C23 O2 K2 C14 92.4(2) . . . . ? C24 O2 K2 C03 84.1(2) . . . . ? C23 O2 K2 C03 -134.78(19) . . . . ? C24 O2 K2 C19 166.3(2) . . . 3_756 ? C23 O2 K2 C19 -52.64(19) . . . 3_756 ? C24 O2 K2 C15 -66.2(2) . . . . ? C23 O2 K2 C15 74.9(2) . . . . ? C15 N4 K2 N3 -28.41(17) . . . . ? C16 N4 K2 N3 178.1(2) . . . . ? C15 N4 K2 O2 137.26(17) . . . . ? C16 N4 K2 O2 -16.2(2) . . . . ? C15 N4 K2 O3 79.19(18) . . . . ? C16 N4 K2 O3 -74.3(2) . . . . ? C15 N4 K2 O1 156.5(2) . . . . ? C16 N4 K2 O1 3.0(2) . . . . ? C15 N4 K2 C20 -113.22(18) . . . 3_756 ? C16 N4 K2 C20 93.3(2) . . . 3_756 ? C15 N4 K2 C04 -39.7(2) . . . . ? C16 N4 K2 C04 166.8(2) . . . . ? C15 N4 K2 C05 -22.8(2) . . . . ? C16 N4 K2 C05 -176.3(2) . . . . ? C15 N4 K2 C14 -12.80(16) . . . . ? C16 N4 K2 C14 -166.3(3) . . . . ? C15 N4 K2 C03 -11.2(3) . . . . ? C16 N4 K2 C03 -164.7(2) . . . . ? C15 N4 K2 C19 -115.39(18) . . . 3_756 ? C16 N4 K2 C19 91.1(2) . . . 3_756 ? C16 N4 K2 C15 -153.5(3) . . . . ? C25 O3 K2 N3 -156.95(18) . . . . ? C26 O3 K2 N3 77.3(2) . . . . ? C25 O3 K2 O2 31.73(18) . . . . ? C26 O3 K2 O2 -94.0(2) . . . . ? C25 O3 K2 N4 142.06(19) . . . . ? C26 O3 K2 N4 16.3(2) . . . . ? C25 O3 K2 O1 89.25(19) . . . . ? C26 O3 K2 O1 -36.5(2) . . . . ? C25 O3 K2 C20 82.4(4) . . . 3_756 ? C26 O3 K2 C20 -43.3(4) . . . 3_756 ? C25 O3 K2 C04 -77.29(19) . . . . ? C26 O3 K2 C04 157.0(2) . . . . ? C25 O3 K2 C05 -100.40(19) . . . . ? C26 O3 K2 C05 133.9(2) . . . . ? C25 O3 K2 C14 -174.30(19) . . . . ? C26 O3 K2 C14 60.0(2) . . . . ? C25 O3 K2 C03 -63.86(19) . . . . ? C26 O3 K2 C03 170.4(2) . . . . ? C25 O3 K2 C19 3.1(3) . . . 3_756 ? C26 O3 K2 C19 -122.6(3) . . . 3_756 ? C25 O3 K2 C15 162.49(19) . . . . ? C26 O3 K2 C15 36.8(2) . . . . ? C21 O1 K2 N3 -5.8(2) . . . . ? C22 O1 K2 N3 -178.73(19) . . . . ? C21 O1 K2 O2 157.0(2) . . . . ? C22 O1 K2 O2 -15.99(19) . . . . ? C21 O1 K2 N4 -0.94(19) . . . . ? C22 O1 K2 N4 -173.9(2) . . . . ? C21 O1 K2 O3 96.5(2) . . . . ? C22 O1 K2 O3 -76.5(2) . . . . ? C21 O1 K2 C20 -85.2(2) . . . 3_756 ? C22 O1 K2 C20 101.8(2) . . . 3_756 ? C21 O1 K2 C04 -136.8(3) . . . . ? C22 O1 K2 C04 50.2(4) . . . . ? C21 O1 K2 C05 2.9(5) . . . . ? C22 O1 K2 C05 -170.1(4) . . . . ? C21 O1 K2 C14 6.5(2) . . . . ? C22 O1 K2 C14 -166.5(2) . . . . ? C21 O1 K2 C03 167.8(2) . . . . ? C22 O1 K2 C03 -5.2(3) . . . . ? C21 O1 K2 C19 -105.3(2) . . . 3_756 ? C22 O1 K2 C19 81.8(2) . . . 3_756 ? C21 O1 K2 C15 7.6(2) . . . . ? C22 O1 K2 C15 -165.4(2) . . . . ? C03 C04 K2 N3 137.64(18) . . . . ? C05 C04 K2 N3 29.41(16) . . . . ? C03 C04 K2 O2 -28.83(19) . . . . ? C05 C04 K2 O2 -137.05(16) . . . . ? C03 C04 K2 N4 147.95(17) . . . . ? C05 C04 K2 N4 39.7(2) . . . . ? C03 C04 K2 O3 36.16(19) . . . . ? C05 C04 K2 O3 -72.06(18) . . . . ? C03 C04 K2 O1 -87.0(3) . . . . ? C05 C04 K2 O1 164.7(2) . . . . ? C03 C04 K2 C20 -138.88(18) . . . 3_756 ? C05 C04 K2 C20 112.90(18) . . . 3_756 ? C03 C04 K2 C05 108.2(3) . . . . ? C03 C04 K2 C14 129.63(17) . . . . ? C05 C04 K2 C14 21.41(17) . . . . ? C05 C04 K2 C03 -108.2(3) . . . . ? C03 C04 K2 C19 -120.89(19) . . . 3_756 ? C05 C04 K2 C19 130.89(19) . . . 3_756 ? C03 C04 K2 C15 132.82(17) . . . . ? C05 C04 K2 C15 24.60(19) . . . . ? N2 C05 K2 N3 101.85(17) . . . . ? C04 C05 K2 N3 -144.60(19) . . . . ? C06 C05 K2 N3 -17.51(15) . . . . ? N2 C05 K2 O2 -58.40(18) . . . . ? C04 C05 K2 O2 55.16(19) . . . . ? C06 C05 K2 O2 -177.75(14) . . . . ? N2 C05 K2 N4 95.79(16) . . . . ? C04 C05 K2 N4 -150.66(16) . . . . ? C06 C05 K2 N4 -23.57(18) . . . . ? N2 C05 K2 O3 0.51(16) . . . . ? C04 C05 K2 O3 114.07(17) . . . . ? C06 C05 K2 O3 -118.84(16) . . . . ? N2 C05 K2 O1 92.3(4) . . . . ? C04 C05 K2 O1 -154.1(4) . . . . ? C06 C05 K2 O1 -27.0(5) . . . . ? N2 C05 K2 C20 179.82(16) . . . 3_756 ? C04 C05 K2 C20 -66.62(18) . . . 3_756 ? C06 C05 K2 C20 60.47(17) . . . 3_756 ? N2 C05 K2 C04 -113.6(2) . . . . ? C06 C05 K2 C04 127.1(3) . . . . ? N2 C05 K2 C14 88.63(15) . . . . ? C04 C05 K2 C14 -157.81(18) . . . . ? C06 C05 K2 C14 -30.72(15) . . . . ? N2 C05 K2 C03 -75.94(17) . . . . ? C04 C05 K2 C03 37.61(17) . . . . ? C06 C05 K2 C03 164.7(2) . . . . ? N2 C05 K2 C19 -158.45(16) . . . 3_756 ? C04 C05 K2 C19 -44.90(17) . . . 3_756 ? C06 C05 K2 C19 82.19(17) . . . 3_756 ? N2 C05 K2 C15 87.82(15) . . . . ? C04 C05 K2 C15 -158.62(17) . . . . ? C06 C05 K2 C15 -31.53(17) . . . . ? C13 C14 K2 N3 -64.6(3) . . . . ? C15 C14 K2 N3 152.3(3) . . . . ? N3 C14 K2 O2 168.46(16) . . . . ? C13 C14 K2 O2 103.9(3) . . . . ? C15 C14 K2 O2 -39.3(2) . . . . ? N3 C14 K2 N4 -141.0(2) . . . . ? C13 C14 K2 N4 154.4(4) . . . . ? C15 C14 K2 N4 11.22(14) . . . . ? N3 C14 K2 O3 130.59(18) . . . . ? C13 C14 K2 O3 66.0(3) . . . . ? C15 C14 K2 O3 -77.15(16) . . . . ? N3 C14 K2 O1 -149.67(17) . . . . ? C13 C14 K2 O1 145.7(3) . . . . ? C15 C14 K2 O1 2.59(16) . . . . ? N3 C14 K2 C20 -63.34(18) . . . 3_756 ? C13 C14 K2 C20 -127.9(3) . . . 3_756 ? C15 C14 K2 C20 88.92(16) . . . 3_756 ? N3 C14 K2 C04 20.86(18) . . . . ? C13 C14 K2 C04 -43.7(3) . . . . ? C15 C14 K2 C04 173.12(16) . . . . ? N3 C14 K2 C05 29.71(17) . . . . ? C13 C14 K2 C05 -34.9(3) . . . . ? C15 C14 K2 C05 -178.02(17) . . . . ? N3 C14 K2 C03 39.72(19) . . . . ? C13 C14 K2 C03 -24.9(3) . . . . ? C15 C14 K2 C03 -168.01(15) . . . . ? N3 C14 K2 C19 -48.40(19) . . . 3_756 ? C13 C14 K2 C19 -113.0(3) . . . 3_756 ? C15 C14 K2 C19 103.86(16) . . . 3_756 ? N3 C14 K2 C15 -152.3(3) . . . . ? C13 C14 K2 C15 143.1(4) . . . . ? C04 C03 K2 N3 -40.77(18) . . . . ? C02 C03 K2 N3 68.37(18) . . . . ? C04 C03 K2 O2 154.13(17) . . . . ? C02 C03 K2 O2 -96.73(17) . . . . ? C04 C03 K2 N4 -56.0(3) . . . . ? C02 C03 K2 N4 53.2(3) . . . . ? C04 C03 K2 O3 -146.20(18) . . . . ? C02 C03 K2 O3 -37.06(18) . . . . ? C04 C03 K2 O1 145.07(17) . . . . ? C02 C03 K2 O1 -105.8(2) . . . . ? C04 C03 K2 C20 41.86(19) . . . 3_756 ? C02 C03 K2 C20 151.00(17) . . . 3_756 ? C02 C03 K2 C04 109.1(3) . . . . ? C04 C03 K2 C05 -38.95(16) . . . . ? C02 C03 K2 C05 70.18(18) . . . . ? C04 C03 K2 C14 -54.78(18) . . . . ? C02 C03 K2 C14 54.35(18) . . . . ? C04 C03 K2 C19 53.83(18) . . . 3_756 ? C02 C03 K2 C19 162.96(18) . . . 3_756 ? C04 C03 K2 C15 -61.4(2) . . . . ? C02 C03 K2 C15 47.7(2) . . . . ? N4 C15 K2 N3 143.2(2) . . . . ? C14 C15 K2 N3 -14.53(14) . . . . ? N4 C15 K2 O2 -49.7(2) . . . . ? C14 C15 K2 O2 152.61(15) . . . . ? C14 C15 K2 N4 -157.7(3) . . . . ? N4 C15 K2 O3 -100.03(18) . . . . ? C14 C15 K2 O3 102.26(16) . . . . ? N4 C15 K2 O1 -19.59(17) . . . . ? C14 C15 K2 O1 -177.31(17) . . . . ? N4 C15 K2 C20 65.87(18) . . . 3_756 ? C14 C15 K2 C20 -91.84(16) . . . 3_756 ? N4 C15 K2 C04 149.82(18) . . . . ? C14 C15 K2 C04 -7.89(18) . . . . ? N4 C15 K2 C05 159.63(18) . . . . ? C14 C15 K2 C05 1.92(16) . . . . ? N4 C15 K2 C14 157.7(3) . . . . ? N4 C15 K2 C03 173.29(17) . . . . ? C14 C15 K2 C03 15.6(2) . . . . ? N4 C15 K2 C19 71.80(19) . . . 3_756 ? C14 C15 K2 C19 -85.91(17) . . . 3_756 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.880 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.070 data_lppd_pdlnme _database_code_depnum_ccdc_archive 'CCDC 895816' #TrackingRef 'combined_CIF.cif.cif' _audit_creation_method SHELXL-2012 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H35 N5 O2 Pd' _chemical_formula_weight 628.05 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.7164(9) _cell_length_b 23.209(2) _cell_length_c 25.187(3) _cell_angle_alpha 90 _cell_angle_beta 91.0660(10) _cell_angle_gamma 90 _cell_volume 5678.9(10) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 16369 _cell_measurement_theta_min 1.9323 _cell_measurement_theta_max 30.471 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.469 _exptl_crystal_F_000 2592 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_absorpt_coefficient_mu 0.692 _shelx_estimated_absorpt_T_min 0.874 _shelx_estimated_absorpt_T_max 0.874 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8052 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_special_details ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.873 RESPONSE: The data set is 100% complete to 0.8 A. Some higher angle data were included in the refinement. See the table in _refine_special_details. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury diffractometer' _diffrn_measurement_method 'phi or omega oscillation scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 43926 _diffrn_reflns_sigmaI/netI 0.0410 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.840 _diffrn_reflns_theta_max 30.508 _diffrn_reflns_theta_full 26.000 _diffrn_measured_fraction_theta_max 0.873 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.873 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.873 _diffrn_reflns_point_group_measured_fraction_full 0.996 _reflns_number_total 15119 _reflns_number_gt 12143 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; The reflections were merged according to the crystal class for structure refinement and the calculation of statistics. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007), SORTAV (Blessing, 1995)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-2012 (Sheldrick, 2012)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; INTENSITY STATISTICS FOR DATASET # 1 lppd.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s Rmerge Rsigma Inf - 3.00 232 246 94.3 5.17 106.6 118.14 0.0191 0.0061 3.00 - 2.00 544 551 98.7 5.31 59.1 87.17 0.0227 0.0079 2.00 - 1.58 785 795 98.7 4.19 41.8 60.25 0.0277 0.0131 1.58 - 1.38 766 772 99.2 3.89 26.1 44.71 0.0247 0.0183 1.38 - 1.25 812 817 99.4 3.71 23.4 38.37 0.0252 0.0200 1.25 - 1.16 779 785 99.2 3.36 17.7 31.59 0.0256 0.0247 1.16 - 1.09 783 786 99.6 3.28 16.2 26.92 0.0276 0.0278 1.09 - 1.04 728 734 99.2 3.04 12.8 20.32 0.0334 0.0374 1.04 - 0.99 856 856 100.0 3.00 12.0 19.12 0.0354 0.0424 0.99 - 0.95 812 816 99.5 2.83 10.4 15.90 0.0396 0.0476 0.95 - 0.92 728 730 99.7 2.70 10.9 14.47 0.0384 0.0527 0.92 - 0.89 790 792 99.7 2.66 8.6 11.71 0.0456 0.0654 0.89 - 0.86 956 958 99.8 2.50 7.4 9.54 0.0505 0.0761 0.86 - 0.84 672 674 99.7 2.45 6.6 8.33 0.0591 0.0862 0.84 - 0.82 778 779 99.9 2.39 6.0 7.69 0.0633 0.0985 0.82 - 0.80 831 839 99.0 2.24 5.5 6.73 0.0668 0.1132 0.80 - 0.78 918 933 98.4 2.18 5.1 5.84 0.0756 0.1306 0.78 - 0.77 511 519 98.5 2.14 4.2 5.11 0.0960 0.1483 0.77 - 0.75 948 1062 89.3 1.78 3.5 4.15 0.0963 0.1797 0.75 - 0.73 727 1224 59.4 0.86 2.9 3.11 0.1000 0.2393 0.73 - 0.70 497 2058 24.1 0.27 2.3 2.16 0.1010 0.3099 #----------------------------------------------------------------------------- 0.80 - 0.70 3601 5796 62.1 1.14 3.7 4.23 0.0877 0.1778 Inf - 0.70 15453 17726 87.2 2.50 15.0 21.91 0.0297 0.0371 Merged [A], lowest resolution = 11.07 Angstroms ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0735P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 15119 _refine_ls_number_parameters 727 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0622 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1298 _refine_ls_wR_factor_gt 0.1184 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C101 C 0.5285(3) 0.33767(10) 0.15066(10) 0.0219(5) Uani 1 1 d D . . H101 H 0.6182 0.3217 0.1543 0.026 Uiso 1 1 calc RD . . C102 C 0.5047(3) 0.38777(10) 0.11953(10) 0.0214(5) Uani 1 1 d D . . C103 C 0.5821(3) 0.42580(10) 0.08826(10) 0.0244(5) Uani 1 1 d D . . H103 H 0.6777 0.4236 0.0813 0.029 Uiso 1 1 calc RD . . C104 C 0.4892(3) 0.46734(10) 0.06971(11) 0.0252(5) Uani 1 1 d D . . H104 H 0.5107 0.4991 0.0475 0.030 Uiso 1 1 calc RD . . C105 C 0.3579(3) 0.45427(10) 0.08953(10) 0.0218(5) Uani 1 1 d D . . C106 C 0.2230(3) 0.48440(10) 0.07707(11) 0.0235(5) Uani 1 1 d D . . C107 C 0.1809(3) 0.46977(11) 0.01858(11) 0.0286(6) Uani 1 1 d D . . H10F H 0.1097 0.4975 0.0064 0.034 Uiso 1 1 calc RD . . H10G H 0.2621 0.4749 -0.0041 0.034 Uiso 1 1 calc RD . . C108 C 0.1256(3) 0.40867(11) 0.01104(12) 0.0328(6) Uani 1 1 d D . . H10A H 0.1851 0.3814 0.0304 0.049 Uiso 1 1 calc RD . . H10B H 0.1240 0.3990 -0.0268 0.049 Uiso 1 1 calc RD . . H10C H 0.0320 0.4064 0.0247 0.049 Uiso 1 1 calc RD . . C109 C 0.2431(3) 0.55074(10) 0.08037(11) 0.0279(6) Uani 1 1 d D . . H10D H 0.3175 0.5620 0.0561 0.033 Uiso 1 1 calc RD . . H10E H 0.1574 0.5698 0.0677 0.033 Uiso 1 1 calc RD . . C110 C 0.2787(4) 0.57287(11) 0.13576(12) 0.0374(7) Uani 1 1 d D . . H11A H 0.2059 0.5619 0.1602 0.056 Uiso 1 1 calc RD . . H11B H 0.2869 0.6149 0.1349 0.056 Uiso 1 1 calc RD . . H11C H 0.3663 0.5560 0.1479 0.056 Uiso 1 1 calc RD . . C111 C 0.1052(3) 0.46719(10) 0.11223(11) 0.0231(5) Uani 1 1 d D . . C112 C -0.0253(3) 0.49266(11) 0.11630(11) 0.0277(6) Uani 1 1 d D . . H112 H -0.0543 0.5273 0.0994 0.033 Uiso 1 1 calc RD . . C113 C -0.1054(3) 0.45857(11) 0.14936(11) 0.0279(6) Uani 1 1 d D . . H113 H -0.1981 0.4652 0.1590 0.033 Uiso 1 1 calc RD . . C114 C -0.0210(3) 0.41250(10) 0.16551(11) 0.0240(5) Uani 1 1 d D . . C115 C -0.0304(3) 0.36404(10) 0.19890(11) 0.0247(5) Uani 1 1 d D . . H115 H -0.1139 0.3553 0.2162 0.030 Uiso 1 1 calc RD . . C116 C 0.0708(3) 0.28232(10) 0.23961(11) 0.0247(5) Uani 1 1 d D . . C117 C 0.1753(3) 0.27321(11) 0.27672(11) 0.0274(6) Uani 1 1 d D . . H117 H 0.2482 0.3003 0.2796 0.033 Uiso 1 1 calc RD . . C118 C 0.1761(3) 0.22555(12) 0.30972(12) 0.0337(6) Uani 1 1 d D . . H118 H 0.2486 0.2201 0.3350 0.040 Uiso 1 1 calc RD . . C119 C 0.0696(4) 0.18575(12) 0.30537(13) 0.0384(7) Uani 1 1 d D . . H119 H 0.0707 0.1523 0.3271 0.046 Uiso 1 1 calc RD . . C120 C -0.0382(3) 0.19467(12) 0.26947(12) 0.0346(7) Uani 1 1 d D . . H120 H -0.1119 0.1678 0.2675 0.042 Uiso 1 1 calc RD . . C121 C -0.0393(3) 0.24276(11) 0.23619(11) 0.0280(6) Uani 1 1 d D . . C122 C -0.2059(3) 0.20819(11) 0.17201(12) 0.0319(6) Uani 1 1 d D . . H12E H -0.2779 0.2234 0.1475 0.038 Uiso 1 1 calc RD . . H12F H -0.2506 0.1813 0.1968 0.038 Uiso 1 1 calc RD . . C123 C -0.1002(3) 0.17560(11) 0.14030(12) 0.0304(6) Uani 1 1 d D . . H12J H -0.0498 0.1488 0.1642 0.036 Uiso 1 1 calc RD . . H12K H -0.1484 0.1523 0.1128 0.036 Uiso 1 1 calc RD . . C124 C -0.0681(3) 0.25146(14) 0.07581(14) 0.0430(8) Uani 1 1 d D . . H12G H -0.1158 0.2283 0.0487 0.065 Uiso 1 1 calc RD . . H12H H 0.0020 0.2753 0.0590 0.065 Uiso 1 1 calc RD . . H12I H -0.1346 0.2763 0.0936 0.065 Uiso 1 1 calc RD . . C125 C 0.1115(3) 0.18086(12) 0.09309(11) 0.0295(6) Uani 1 1 d D . . H12C H 0.1559 0.2042 0.0653 0.035 Uiso 1 1 calc RD . . H12D H 0.0752 0.1453 0.0761 0.035 Uiso 1 1 calc RD . . C126 C 0.2171(3) 0.16483(11) 0.13478(11) 0.0270(6) Uani 1 1 d D . . H12A H 0.1713 0.1496 0.1666 0.032 Uiso 1 1 calc RD . . H12B H 0.2791 0.1347 0.1211 0.032 Uiso 1 1 calc RD . . C127 C 0.3829(3) 0.21209(10) 0.19054(10) 0.0227(5) Uani 1 1 d D . . C128 C 0.4110(3) 0.16190(10) 0.21925(11) 0.0253(6) Uani 1 1 d D . . H128 H 0.3688 0.1266 0.2090 0.030 Uiso 1 1 calc RD . . C129 C 0.5006(3) 0.16351(11) 0.26279(11) 0.0270(6) Uani 1 1 d D . . H129 H 0.5187 0.1292 0.2823 0.032 Uiso 1 1 calc RD . . C130 C 0.5639(3) 0.21437(11) 0.27824(11) 0.0277(6) Uani 1 1 d D . . H130 H 0.6235 0.2154 0.3086 0.033 Uiso 1 1 calc RD . . C131 C 0.5386(3) 0.26394(10) 0.24853(11) 0.0259(5) Uani 1 1 d D . . H131 H 0.5832 0.2989 0.2584 0.031 Uiso 1 1 calc RD . . C132 C 0.4500(3) 0.26327(10) 0.20506(11) 0.0229(5) Uani 1 1 d D . . N101 N 0.4241(2) 0.31408(8) 0.17422(9) 0.0214(4) Uani 1 1 d D . . N102 N 0.3707(2) 0.40598(8) 0.11860(9) 0.0216(4) Uani 1 1 d D . . N103 N 0.1048(2) 0.41902(8) 0.14225(9) 0.0220(4) Uani 1 1 d D . . N104 N 0.0778(2) 0.33135(9) 0.20552(9) 0.0229(4) Uani 1 1 d D . . N105 N -0.0022(3) 0.21332(9) 0.11490(10) 0.0290(5) Uani 1 1 d D . . O101 O -0.1464(2) 0.25505(7) 0.20162(8) 0.0303(4) Uani 1 1 d D . . O102 O 0.29443(19) 0.21561(7) 0.14822(7) 0.0252(4) Uani 1 1 d D . . Pd1 Pd 0.24392(2) 0.362274(7) 0.161936(8) 0.01986(7) Uani 1 1 d D . . C201 C 0.7433(3) 0.34386(11) 0.34556(11) 0.0252(6) Uani 1 1 d D . . H201 H 0.8269 0.3513 0.3279 0.030 Uiso 1 1 calc RD . . C202 C 0.7311(3) 0.29635(11) 0.38036(11) 0.0258(6) Uani 1 1 d D . . C203 C 0.8116(3) 0.24951(11) 0.39720(12) 0.0314(6) Uani 1 1 d D . . H203 H 0.9030 0.2411 0.3870 0.038 Uiso 1 1 calc RD . . C204 C 0.7318(3) 0.21802(11) 0.43153(12) 0.0308(6) Uani 1 1 d D . . H204 H 0.7592 0.1839 0.4497 0.037 Uiso 1 1 calc RD . . C205 C 0.6026(3) 0.24520(11) 0.43485(11) 0.0276(6) Uani 1 1 d D . . C206 C 0.4817(3) 0.22896(10) 0.46935(11) 0.0269(6) Uani 1 1 d D . . C207 C 0.5169(3) 0.24594(12) 0.52823(12) 0.0359(7) Uani 1 1 d D . . H20A H 0.4416 0.2325 0.5511 0.043 Uiso 1 1 calc RD . . H20B H 0.6020 0.2256 0.5396 0.043 Uiso 1 1 calc RD . . C208 C 0.5374(4) 0.31039(13) 0.53699(13) 0.0430(8) Uani 1 1 d D . . H20E H 0.6177 0.3234 0.5173 0.065 Uiso 1 1 calc RD . . H20F H 0.5523 0.3180 0.5749 0.065 Uiso 1 1 calc RD . . H20G H 0.4554 0.3312 0.5243 0.065 Uiso 1 1 calc RD . . C209 C 0.4619(3) 0.16223(11) 0.46785(12) 0.0335(7) Uani 1 1 d D . . H20C H 0.5510 0.1436 0.4767 0.040 Uiso 1 1 calc RD . . H20D H 0.3960 0.1512 0.4956 0.040 Uiso 1 1 calc RD . . C210 C 0.4098(4) 0.13930(11) 0.41477(13) 0.0378(7) Uani 1 1 d D . . H21A H 0.3164 0.1537 0.4077 0.057 Uiso 1 1 calc RD . . H21B H 0.4085 0.0971 0.4157 0.057 Uiso 1 1 calc RD . . H21C H 0.4707 0.1523 0.3866 0.057 Uiso 1 1 calc RD . . C211 C 0.3473(3) 0.25782(10) 0.45381(10) 0.0241(5) Uani 1 1 d D . . C212 C 0.2144(3) 0.24550(11) 0.47255(11) 0.0293(6) Uani 1 1 d D . . H212 H 0.1915 0.2153 0.4962 0.035 Uiso 1 1 calc RD . . C213 C 0.1231(3) 0.28507(11) 0.45049(11) 0.0274(6) Uani 1 1 d D . . H213 H 0.0268 0.2872 0.4561 0.033 Uiso 1 1 calc RD . . C214 C 0.2010(3) 0.32127(10) 0.41833(11) 0.0227(5) Uani 1 1 d D . . C215 C 0.1800(3) 0.37040(10) 0.38650(10) 0.0225(5) Uani 1 1 d D . . H215 H 0.0905 0.3861 0.3812 0.027 Uiso 1 1 calc RD . . C216 C 0.2689(3) 0.44589(10) 0.33469(10) 0.0231(5) Uani 1 1 d D . . C217 C 0.1795(3) 0.44967(10) 0.29166(11) 0.0255(5) Uani 1 1 d D . . H217 H 0.1268 0.4170 0.2812 0.031 Uiso 1 1 calc RD . . C218 C 0.1658(3) 0.50085(11) 0.26347(11) 0.0289(6) Uani 1 1 d D . . H218 H 0.1044 0.5033 0.2338 0.035 Uiso 1 1 calc RD . . C219 C 0.2431(3) 0.54823(11) 0.27935(11) 0.0300(6) Uani 1 1 d D . . H219 H 0.2339 0.5833 0.2602 0.036 Uiso 1 1 calc RD . . C220 C 0.3337(3) 0.54550(10) 0.32264(11) 0.0267(6) Uani 1 1 d D . . H220 H 0.3854 0.5785 0.3331 0.032 Uiso 1 1 calc RD . . C221 C 0.3478(3) 0.49387(10) 0.35047(10) 0.0232(5) Uani 1 1 d D . . C222 C 0.5409(3) 0.52599(11) 0.40296(11) 0.0274(6) Uani 1 1 d D . . H22F H 0.5050 0.5605 0.4212 0.033 Uiso 1 1 calc RD . . H22G H 0.5829 0.5382 0.3693 0.033 Uiso 1 1 calc RD . . C223 C 0.6468(3) 0.49490(12) 0.43835(12) 0.0314(6) Uani 1 1 d D . . H22J H 0.6048 0.4843 0.4725 0.038 Uiso 1 1 calc RD . . H22K H 0.6775 0.4591 0.4207 0.038 Uiso 1 1 calc RD . . C224 C 0.7688(4) 0.55345(15) 0.50297(13) 0.0432(8) Uani 1 1 d D . . H22A H 0.7874 0.5210 0.5269 0.065 Uiso 1 1 calc RD . . H22B H 0.6802 0.5709 0.5116 0.065 Uiso 1 1 calc RD . . H22C H 0.8420 0.5822 0.5071 0.065 Uiso 1 1 calc RD . . C225 C 0.8948(3) 0.50867(12) 0.43229(12) 0.0319(6) Uani 1 1 d D . . H22D H 0.9022 0.4689 0.4463 0.038 Uiso 1 1 calc RD . . H22E H 0.9702 0.5316 0.4487 0.038 Uiso 1 1 calc RD . . C226 C 0.9136(3) 0.50732(12) 0.37326(12) 0.0325(6) Uani 1 1 d D . . H22H H 0.8756 0.5431 0.3574 0.039 Uiso 1 1 calc RD . . H22I H 1.0131 0.5059 0.3656 0.039 Uiso 1 1 calc RD . . C227 C 0.7536(3) 0.46626(10) 0.30840(11) 0.0259(5) Uani 1 1 d D . . C228 C 0.7593(3) 0.51200(11) 0.27246(12) 0.0312(6) Uani 1 1 d D . . H228 H 0.8322 0.5392 0.2751 0.037 Uiso 1 1 calc RD . . C229 C 0.6591(3) 0.51794(11) 0.23298(12) 0.0342(7) Uani 1 1 d D . . H229 H 0.6635 0.5494 0.2089 0.041 Uiso 1 1 calc RD . . C230 C 0.5530(3) 0.47868(12) 0.22817(12) 0.0324(6) Uani 1 1 d D . . H230 H 0.4843 0.4831 0.2011 0.039 Uiso 1 1 calc RD . . C231 C 0.5475(3) 0.43235(11) 0.26346(11) 0.0283(6) Uani 1 1 d D . . H231 H 0.4747 0.4052 0.2602 0.034 Uiso 1 1 calc RD . . C232 C 0.6465(3) 0.42541(10) 0.30306(11) 0.0256(5) Uani 1 1 d D . . N201 N 0.6356(2) 0.37750(8) 0.33838(9) 0.0229(4) Uani 1 1 d D . . N202 N 0.6055(2) 0.29193(8) 0.40359(9) 0.0245(5) Uani 1 1 d D . . N203 N 0.3359(2) 0.30390(8) 0.42195(9) 0.0230(4) Uani 1 1 d D . . N204 N 0.2873(2) 0.39399(8) 0.36429(9) 0.0227(4) Uani 1 1 d D . . N205 N 0.7642(3) 0.53286(10) 0.44794(10) 0.0303(5) Uani 1 1 d D . . O201 O 0.8457(2) 0.45804(8) 0.34920(8) 0.0307(4) Uani 1 1 d D . . O202 O 0.4333(2) 0.48553(7) 0.39304(8) 0.0278(4) Uani 1 1 d D . . Pd2 Pd 0.46659(2) 0.347058(7) 0.380395(8) 0.02124(7) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C101 0.0171(13) 0.0227(11) 0.0256(13) -0.0020(9) -0.0041(10) 0.0025(9) C102 0.0186(13) 0.0197(11) 0.0258(13) 0.0007(9) 0.0009(10) -0.0005(9) C103 0.0184(13) 0.0306(12) 0.0242(13) -0.0002(10) 0.0010(10) -0.0032(10) C104 0.0266(15) 0.0231(11) 0.0260(14) 0.0041(10) 0.0007(11) -0.0038(10) C105 0.0227(13) 0.0206(11) 0.0219(13) 0.0017(9) -0.0025(10) -0.0012(9) C106 0.0263(14) 0.0198(11) 0.0244(13) 0.0022(9) -0.0018(11) 0.0004(9) C107 0.0295(16) 0.0310(13) 0.0252(14) 0.0004(10) -0.0038(11) 0.0047(11) C108 0.0367(17) 0.0293(13) 0.0321(16) -0.0071(11) -0.0080(13) 0.0067(12) C109 0.0313(16) 0.0182(11) 0.0341(15) 0.0040(10) -0.0029(12) -0.0001(10) C110 0.050(2) 0.0234(13) 0.0381(17) -0.0012(11) -0.0064(15) -0.0027(12) C111 0.0211(13) 0.0219(11) 0.0261(13) -0.0023(9) -0.0031(10) 0.0026(9) C112 0.0293(15) 0.0246(12) 0.0290(15) -0.0016(10) -0.0066(12) 0.0079(10) C113 0.0198(14) 0.0334(13) 0.0304(15) -0.0071(11) -0.0037(11) 0.0057(10) C114 0.0180(13) 0.0261(12) 0.0280(14) -0.0058(10) 0.0018(10) 0.0016(9) C115 0.0200(14) 0.0283(12) 0.0258(14) -0.0048(10) 0.0013(11) -0.0035(10) C116 0.0265(14) 0.0225(11) 0.0252(14) -0.0027(9) 0.0046(11) -0.0019(10) C117 0.0289(15) 0.0251(12) 0.0283(14) -0.0034(10) 0.0027(11) -0.0012(10) C118 0.0395(18) 0.0342(14) 0.0274(15) -0.0002(11) 0.0027(13) 0.0009(12) C119 0.052(2) 0.0270(13) 0.0362(17) 0.0043(12) 0.0072(15) -0.0029(13) C120 0.0419(19) 0.0287(13) 0.0336(16) -0.0002(11) 0.0074(14) -0.0110(12) C121 0.0294(15) 0.0267(12) 0.0280(15) -0.0026(10) 0.0048(12) -0.0045(11) C122 0.0277(16) 0.0306(13) 0.0373(17) -0.0042(11) 0.0011(12) -0.0074(11) C123 0.0284(15) 0.0265(13) 0.0363(16) -0.0029(11) 0.0017(12) -0.0034(11) C124 0.0361(19) 0.0467(17) 0.046(2) 0.0157(15) 0.0042(15) 0.0121(14) C125 0.0257(15) 0.0338(13) 0.0289(15) -0.0028(11) -0.0026(12) 0.0004(11) C126 0.0275(15) 0.0221(11) 0.0312(15) -0.0030(10) -0.0016(12) -0.0027(10) C127 0.0219(13) 0.0216(11) 0.0244(13) -0.0009(9) -0.0018(10) 0.0029(9) C128 0.0271(15) 0.0189(11) 0.0300(15) 0.0008(10) 0.0024(11) 0.0006(10) C129 0.0290(15) 0.0220(11) 0.0299(15) 0.0039(10) -0.0012(12) 0.0049(10) C130 0.0281(15) 0.0280(12) 0.0267(14) 0.0021(10) -0.0046(11) 0.0028(11) C131 0.0238(14) 0.0218(11) 0.0320(15) -0.0005(10) -0.0020(11) 0.0015(10) C132 0.0226(13) 0.0199(11) 0.0262(13) 0.0015(9) 0.0028(10) 0.0025(9) N101 0.0170(11) 0.0189(9) 0.0283(12) 0.0009(8) -0.0034(9) 0.0027(7) N102 0.0185(11) 0.0189(9) 0.0272(12) 0.0032(8) -0.0001(9) -0.0005(8) N103 0.0189(11) 0.0193(9) 0.0278(12) 0.0004(8) 0.0002(9) 0.0030(8) N104 0.0200(12) 0.0226(9) 0.0261(12) -0.0020(8) 0.0045(9) -0.0047(8) N105 0.0278(13) 0.0291(11) 0.0299(13) 0.0017(9) 0.0009(10) 0.0017(9) O101 0.0258(11) 0.0261(9) 0.0388(12) -0.0041(8) -0.0015(9) -0.0061(7) O102 0.0272(10) 0.0206(8) 0.0274(10) 0.0020(7) -0.0060(8) -0.0021(7) Pd1 0.01744(11) 0.01672(10) 0.02541(12) 0.00116(6) 0.00011(8) -0.00025(6) C201 0.0218(14) 0.0257(12) 0.0281(14) -0.0076(10) 0.0021(11) -0.0033(9) C202 0.0201(13) 0.0246(12) 0.0325(15) -0.0063(10) -0.0031(11) 0.0029(10) C203 0.0234(15) 0.0300(13) 0.0404(17) -0.0077(12) -0.0085(12) 0.0055(11) C204 0.0301(16) 0.0230(12) 0.0387(17) -0.0024(11) -0.0102(13) 0.0061(11) C205 0.0288(15) 0.0238(12) 0.0299(15) -0.0039(10) -0.0053(12) 0.0033(10) C206 0.0311(16) 0.0221(11) 0.0274(14) 0.0019(10) -0.0028(11) 0.0029(10) C207 0.0377(18) 0.0399(15) 0.0298(16) 0.0048(12) -0.0049(13) 0.0079(13) C208 0.052(2) 0.0412(16) 0.0357(18) -0.0082(13) -0.0106(15) 0.0045(15) C209 0.0387(18) 0.0223(12) 0.0397(17) 0.0079(11) 0.0027(14) 0.0042(11) C210 0.046(2) 0.0236(13) 0.0437(19) -0.0003(12) 0.0024(15) 0.0010(12) C211 0.0273(15) 0.0213(11) 0.0237(13) -0.0008(9) -0.0003(11) 0.0008(10) C212 0.0330(16) 0.0244(12) 0.0308(15) 0.0038(10) 0.0038(12) -0.0031(11) C213 0.0269(15) 0.0274(12) 0.0279(14) -0.0014(10) 0.0020(11) -0.0033(10) C214 0.0190(13) 0.0238(11) 0.0253(13) -0.0028(9) -0.0007(10) 0.0002(9) C215 0.0197(13) 0.0237(11) 0.0240(13) -0.0031(9) -0.0008(10) 0.0021(9) C216 0.0228(14) 0.0203(11) 0.0263(14) -0.0002(9) 0.0042(11) 0.0047(9) C217 0.0254(14) 0.0213(11) 0.0300(14) -0.0004(10) 0.0016(11) 0.0019(10) C218 0.0317(16) 0.0293(13) 0.0256(14) 0.0004(10) -0.0041(12) 0.0057(11) C219 0.0364(17) 0.0216(12) 0.0320(15) 0.0066(10) 0.0007(12) 0.0062(11) C220 0.0305(15) 0.0182(11) 0.0314(15) -0.0012(10) 0.0005(12) 0.0008(10) C221 0.0224(14) 0.0231(11) 0.0242(13) -0.0002(9) 0.0015(10) 0.0017(9) C222 0.0272(15) 0.0282(12) 0.0266(14) -0.0025(10) -0.0007(11) -0.0023(10) C223 0.0269(16) 0.0350(14) 0.0321(16) -0.0004(11) -0.0008(12) -0.0040(11) C224 0.039(2) 0.0528(18) 0.0379(19) -0.0153(14) 0.0036(15) -0.0060(15) C225 0.0240(15) 0.0344(14) 0.0371(17) -0.0043(12) -0.0022(12) 0.0009(11) C226 0.0315(17) 0.0322(14) 0.0339(16) -0.0077(11) 0.0048(13) -0.0055(12) C227 0.0282(15) 0.0239(11) 0.0258(14) -0.0032(10) 0.0051(11) 0.0006(10) C228 0.0392(18) 0.0243(12) 0.0306(15) -0.0019(10) 0.0098(13) -0.0009(11) C229 0.048(2) 0.0253(12) 0.0296(16) 0.0017(11) 0.0124(14) 0.0073(12) C230 0.0355(17) 0.0327(14) 0.0291(15) -0.0031(11) 0.0007(12) 0.0107(12) C231 0.0271(15) 0.0265(12) 0.0313(15) -0.0039(10) 0.0030(12) 0.0046(10) C232 0.0276(15) 0.0224(11) 0.0270(14) -0.0037(10) 0.0089(11) 0.0024(10) N201 0.0201(11) 0.0210(9) 0.0277(12) -0.0009(8) 0.0028(9) 0.0000(8) N202 0.0219(12) 0.0223(10) 0.0292(12) -0.0020(8) -0.0013(9) 0.0036(8) N203 0.0198(11) 0.0202(9) 0.0288(12) 0.0009(8) -0.0016(9) 0.0003(8) N204 0.0206(11) 0.0208(9) 0.0267(12) 0.0007(8) -0.0007(9) 0.0036(8) N205 0.0253(13) 0.0321(11) 0.0334(14) -0.0049(10) 0.0015(10) -0.0021(9) O201 0.0358(12) 0.0258(9) 0.0305(11) -0.0010(8) -0.0015(9) -0.0057(8) O202 0.0268(11) 0.0267(9) 0.0298(10) 0.0022(7) -0.0056(8) -0.0028(7) Pd2 0.01962(12) 0.01839(10) 0.02572(12) 0.00078(7) 0.00042(8) 0.00125(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 C101 N101 1.304(3) . ? C101 C102 1.419(3) . ? C101 H101 0.9500 . ? C102 N102 1.369(3) . ? C102 C103 1.410(3) . ? C103 C104 1.395(4) . ? C103 H103 0.9500 . ? C104 C105 1.412(4) . ? C104 H104 0.9500 . ? C105 N102 1.343(3) . ? C105 C106 1.513(4) . ? C106 C111 1.514(4) . ? C106 C109 1.554(3) . ? C106 C107 1.559(4) . ? C107 C108 1.527(4) . ? C107 H10F 0.9900 . ? C107 H10G 0.9900 . ? C108 H10A 0.9800 . ? C108 H10B 0.9800 . ? C108 H10C 0.9800 . ? C109 C110 1.520(4) . ? C109 H10D 0.9900 . ? C109 H10E 0.9900 . ? C110 H11A 0.9800 . ? C110 H11B 0.9800 . ? C110 H11C 0.9800 . ? C111 N103 1.350(3) . ? C111 C112 1.405(4) . ? C112 C113 1.396(4) . ? C112 H112 0.9500 . ? C113 C114 1.403(4) . ? C113 H113 0.9500 . ? C114 N103 1.373(3) . ? C114 C115 1.408(4) . ? C115 N104 1.305(3) . ? C115 H115 0.9500 . ? C116 C117 1.383(4) . ? C116 C121 1.411(4) . ? C116 N104 1.428(3) . ? C117 C118 1.384(4) . ? C117 H117 0.9500 . ? C118 C119 1.390(4) . ? C118 H118 0.9500 . ? C119 C120 1.386(5) . ? C119 H119 0.9500 . ? C120 C121 1.396(4) . ? C120 H120 0.9500 . ? C121 O101 1.374(3) . ? C122 O101 1.434(3) . ? C122 C123 1.515(4) . ? C122 H12E 0.9900 . ? C122 H12F 0.9900 . ? C123 N105 1.451(3) . ? C123 H12J 0.9900 . ? C123 H12K 0.9900 . ? C124 N105 1.463(4) . ? C124 H12G 0.9800 . ? C124 H12H 0.9800 . ? C124 H12I 0.9800 . ? C125 N105 1.453(3) . ? C125 C126 1.501(4) . ? C125 H12C 0.9900 . ? C125 H12D 0.9900 . ? C126 O102 1.435(3) . ? C126 H12A 0.9900 . ? C126 H12B 0.9900 . ? C127 O102 1.359(3) . ? C127 C128 1.395(3) . ? C127 C132 1.401(3) . ? C128 C129 1.388(4) . ? C128 H128 0.9500 . ? C129 C130 1.384(4) . ? C129 H129 0.9500 . ? C130 C131 1.392(3) . ? C130 H130 0.9500 . ? C131 C132 1.380(4) . ? C131 H131 0.9500 . ? C132 N101 1.432(3) . ? N101 Pd1 2.096(2) . ? N102 Pd1 1.946(2) . ? N103 Pd1 1.945(2) . ? N104 Pd1 2.096(2) . ? C201 N201 1.315(3) . ? C201 C202 1.415(4) . ? C201 H201 0.9500 . ? C202 N202 1.368(3) . ? C202 C203 1.400(4) . ? C203 C204 1.381(4) . ? C203 H203 0.9500 . ? C204 C205 1.409(4) . ? C204 H204 0.9500 . ? C205 N202 1.341(3) . ? C205 C206 1.521(4) . ? C206 C211 1.513(4) . ? C206 C209 1.561(3) . ? C206 C207 1.566(4) . ? C207 C208 1.524(4) . ? C207 H20A 0.9900 . ? C207 H20B 0.9900 . ? C208 H20E 0.9800 . ? C208 H20F 0.9800 . ? C208 H20G 0.9800 . ? C209 C210 1.517(4) . ? C209 H20C 0.9900 . ? C209 H20D 0.9900 . ? C210 H21A 0.9800 . ? C210 H21B 0.9800 . ? C210 H21C 0.9800 . ? C211 N203 1.340(3) . ? C211 C212 1.412(4) . ? C212 C213 1.386(4) . ? C212 H212 0.9500 . ? C213 C214 1.399(4) . ? C213 H213 0.9500 . ? C214 N203 1.373(3) . ? C214 C215 1.406(3) . ? C215 N204 1.312(3) . ? C215 H215 0.9500 . ? C216 C217 1.379(4) . ? C216 C221 1.405(4) . ? C216 N204 1.426(3) . ? C217 C218 1.389(3) . ? C217 H217 0.9500 . ? C218 C219 1.386(4) . ? C218 H218 0.9500 . ? C219 C220 1.390(4) . ? C219 H219 0.9500 . ? C220 C221 1.394(3) . ? C220 H220 0.9500 . ? C221 O202 1.358(3) . ? C222 O202 1.424(3) . ? C222 C223 1.530(4) . ? C222 H22F 0.9900 . ? C222 H22G 0.9900 . ? C223 N205 1.458(3) . ? C223 H22J 0.9900 . ? C223 H22K 0.9900 . ? C224 N205 1.466(4) . ? C224 H22A 0.9800 . ? C224 H22B 0.9800 . ? C224 H22C 0.9800 . ? C225 N205 1.449(4) . ? C225 C226 1.502(4) . ? C225 H22D 0.9900 . ? C225 H22E 0.9900 . ? C226 O201 1.447(3) . ? C226 H22H 0.9900 . ? C226 H22I 0.9900 . ? C227 O201 1.364(3) . ? C227 C228 1.397(4) . ? C227 C232 1.412(4) . ? C228 C229 1.386(5) . ? C228 H228 0.9500 . ? C229 C230 1.380(4) . ? C229 H229 0.9500 . ? C230 C231 1.397(4) . ? C230 H230 0.9500 . ? C231 C232 1.381(4) . ? C231 H231 0.9500 . ? C232 N201 1.429(3) . ? N201 Pd2 2.093(2) . ? N202 Pd2 1.942(2) . ? N203 Pd2 1.939(2) . ? N204 Pd2 2.088(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 N101 C101 C102 118.4(2) . . ? N101 C101 H101 120.8 . . ? C102 C101 H101 120.8 . . ? N102 C102 C103 108.3(2) . . ? N102 C102 C101 114.0(2) . . ? C103 C102 C101 137.6(2) . . ? C104 C103 C102 105.7(2) . . ? C104 C103 H103 127.1 . . ? C102 C103 H103 127.1 . . ? C103 C104 C105 108.5(2) . . ? C103 C104 H104 125.8 . . ? C105 C104 H104 125.8 . . ? N102 C105 C104 107.3(2) . . ? N102 C105 C106 124.7(2) . . ? C104 C105 C106 127.8(2) . . ? C105 C106 C111 114.7(2) . . ? C105 C106 C109 109.8(2) . . ? C111 C106 C109 109.0(2) . . ? C105 C106 C107 107.8(2) . . ? C111 C106 C107 107.9(2) . . ? C109 C106 C107 107.3(2) . . ? C108 C107 C106 113.9(2) . . ? C108 C107 H10F 108.8 . . ? C106 C107 H10F 108.8 . . ? C108 C107 H10G 108.8 . . ? C106 C107 H10G 108.8 . . ? H10F C107 H10G 107.7 . . ? C107 C108 H10A 109.5 . . ? C107 C108 H10B 109.5 . . ? H10A C108 H10B 109.5 . . ? C107 C108 H10C 109.5 . . ? H10A C108 H10C 109.5 . . ? H10B C108 H10C 109.5 . . ? C110 C109 C106 114.2(2) . . ? C110 C109 H10D 108.7 . . ? C106 C109 H10D 108.7 . . ? C110 C109 H10E 108.7 . . ? C106 C109 H10E 108.7 . . ? H10D C109 H10E 107.6 . . ? C109 C110 H11A 109.5 . . ? C109 C110 H11B 109.5 . . ? H11A C110 H11B 109.5 . . ? C109 C110 H11C 109.5 . . ? H11A C110 H11C 109.5 . . ? H11B C110 H11C 109.5 . . ? N103 C111 C112 107.2(2) . . ? N103 C111 C106 123.8(2) . . ? C112 C111 C106 128.7(2) . . ? C113 C112 C111 108.6(2) . . ? C113 C112 H112 125.7 . . ? C111 C112 H112 125.7 . . ? C112 C113 C114 106.0(2) . . ? C112 C113 H113 127.0 . . ? C114 C113 H113 127.0 . . ? N103 C114 C113 108.2(2) . . ? N103 C114 C115 114.3(2) . . ? C113 C114 C115 137.5(3) . . ? N104 C115 C114 118.7(2) . . ? N104 C115 H115 120.7 . . ? C114 C115 H115 120.7 . . ? C117 C116 C121 119.2(2) . . ? C117 C116 N104 119.1(2) . . ? C121 C116 N104 121.7(2) . . ? C116 C117 C118 121.6(3) . . ? C116 C117 H117 119.2 . . ? C118 C117 H117 119.2 . . ? C117 C118 C119 119.2(3) . . ? C117 C118 H118 120.4 . . ? C119 C118 H118 120.4 . . ? C120 C119 C118 120.3(3) . . ? C120 C119 H119 119.9 . . ? C118 C119 H119 119.9 . . ? C119 C120 C121 120.6(3) . . ? C119 C120 H120 119.7 . . ? C121 C120 H120 119.7 . . ? O101 C121 C120 123.0(3) . . ? O101 C121 C116 117.9(2) . . ? C120 C121 C116 119.1(3) . . ? O101 C122 C123 112.5(2) . . ? O101 C122 H12E 109.1 . . ? C123 C122 H12E 109.1 . . ? O101 C122 H12F 109.1 . . ? C123 C122 H12F 109.1 . . ? H12E C122 H12F 107.8 . . ? N105 C123 C122 112.8(2) . . ? N105 C123 H12J 109.0 . . ? C122 C123 H12J 109.0 . . ? N105 C123 H12K 109.0 . . ? C122 C123 H12K 109.0 . . ? H12J C123 H12K 107.8 . . ? N105 C124 H12G 109.5 . . ? N105 C124 H12H 109.5 . . ? H12G C124 H12H 109.5 . . ? N105 C124 H12I 109.5 . . ? H12G C124 H12I 109.5 . . ? H12H C124 H12I 109.5 . . ? N105 C125 C126 112.2(2) . . ? N105 C125 H12C 109.2 . . ? C126 C125 H12C 109.2 . . ? N105 C125 H12D 109.2 . . ? C126 C125 H12D 109.2 . . ? H12C C125 H12D 107.9 . . ? O102 C126 C125 108.0(2) . . ? O102 C126 H12A 110.1 . . ? C125 C126 H12A 110.1 . . ? O102 C126 H12B 110.1 . . ? C125 C126 H12B 110.1 . . ? H12A C126 H12B 108.4 . . ? O102 C127 C128 124.9(2) . . ? O102 C127 C132 116.0(2) . . ? C128 C127 C132 119.1(2) . . ? C129 C128 C127 120.1(2) . . ? C129 C128 H128 120.0 . . ? C127 C128 H128 120.0 . . ? C130 C129 C128 121.0(2) . . ? C130 C129 H129 119.5 . . ? C128 C129 H129 119.5 . . ? C129 C130 C131 118.7(3) . . ? C129 C130 H130 120.6 . . ? C131 C130 H130 120.6 . . ? C132 C131 C130 121.2(2) . . ? C132 C131 H131 119.4 . . ? C130 C131 H131 119.4 . . ? C131 C132 C127 119.8(2) . . ? C131 C132 N101 121.5(2) . . ? C127 C132 N101 118.7(2) . . ? C101 N101 C132 117.5(2) . . ? C101 N101 Pd1 111.29(16) . . ? C132 N101 Pd1 131.11(17) . . ? C105 N102 C102 110.2(2) . . ? C105 N102 Pd1 133.43(18) . . ? C102 N102 Pd1 116.19(16) . . ? C111 N103 C114 110.0(2) . . ? C111 N103 Pd1 133.97(18) . . ? C114 N103 Pd1 115.87(17) . . ? C115 N104 C116 119.5(2) . . ? C115 N104 Pd1 111.14(17) . . ? C116 N104 Pd1 129.32(17) . . ? C123 N105 C125 111.3(2) . . ? C123 N105 C124 112.3(2) . . ? C125 N105 C124 112.7(2) . . ? C121 O101 C122 117.7(2) . . ? C127 O102 C126 117.15(19) . . ? N103 Pd1 N102 87.03(9) . . ? N103 Pd1 N104 80.03(9) . . ? N102 Pd1 N104 166.91(8) . . ? N103 Pd1 N101 166.86(9) . . ? N102 Pd1 N101 79.93(8) . . ? N104 Pd1 N101 112.92(8) . . ? N201 C201 C202 118.2(3) . . ? N201 C201 H201 120.9 . . ? C202 C201 H201 120.9 . . ? N202 C202 C203 108.0(2) . . ? N202 C202 C201 114.1(2) . . ? C203 C202 C201 137.8(3) . . ? C204 C203 C202 106.5(3) . . ? C204 C203 H203 126.8 . . ? C202 C203 H203 126.8 . . ? C203 C204 C205 108.1(2) . . ? C203 C204 H204 125.9 . . ? C205 C204 H204 125.9 . . ? N202 C205 C204 107.4(3) . . ? N202 C205 C206 124.1(2) . . ? C204 C205 C206 128.4(2) . . ? C211 C206 C205 114.5(2) . . ? C211 C206 C209 109.1(2) . . ? C205 C206 C209 109.2(2) . . ? C211 C206 C207 107.8(2) . . ? C205 C206 C207 108.7(2) . . ? C209 C206 C207 107.3(2) . . ? C208 C207 C206 114.2(2) . . ? C208 C207 H20A 108.7 . . ? C206 C207 H20A 108.7 . . ? C208 C207 H20B 108.7 . . ? C206 C207 H20B 108.7 . . ? H20A C207 H20B 107.6 . . ? C207 C208 H20E 109.5 . . ? C207 C208 H20F 109.5 . . ? H20E C208 H20F 109.5 . . ? C207 C208 H20G 109.5 . . ? H20E C208 H20G 109.5 . . ? H20F C208 H20G 109.5 . . ? C210 C209 C206 114.1(2) . . ? C210 C209 H20C 108.7 . . ? C206 C209 H20C 108.7 . . ? C210 C209 H20D 108.7 . . ? C206 C209 H20D 108.7 . . ? H20C C209 H20D 107.6 . . ? C209 C210 H21A 109.5 . . ? C209 C210 H21B 109.5 . . ? H21A C210 H21B 109.5 . . ? C209 C210 H21C 109.5 . . ? H21A C210 H21C 109.5 . . ? H21B C210 H21C 109.5 . . ? N203 C211 C212 107.2(2) . . ? N203 C211 C206 124.7(2) . . ? C212 C211 C206 127.9(2) . . ? C213 C212 C211 108.3(2) . . ? C213 C212 H212 125.8 . . ? C211 C212 H212 125.8 . . ? C212 C213 C214 106.3(3) . . ? C212 C213 H213 126.8 . . ? C214 C213 H213 126.8 . . ? N203 C214 C213 108.1(2) . . ? N203 C214 C215 113.8(2) . . ? C213 C214 C215 137.9(3) . . ? N204 C215 C214 118.2(2) . . ? N204 C215 H215 120.9 . . ? C214 C215 H215 120.9 . . ? C217 C216 C221 120.3(2) . . ? C217 C216 N204 122.4(2) . . ? C221 C216 N204 117.3(2) . . ? C216 C217 C218 120.6(2) . . ? C216 C217 H217 119.7 . . ? C218 C217 H217 119.7 . . ? C219 C218 C217 119.0(3) . . ? C219 C218 H218 120.5 . . ? C217 C218 H218 120.5 . . ? C218 C219 C220 121.5(2) . . ? C218 C219 H219 119.3 . . ? C220 C219 H219 119.3 . . ? C219 C220 C221 119.3(2) . . ? C219 C220 H220 120.4 . . ? C221 C220 H220 120.4 . . ? O202 C221 C220 125.0(2) . . ? O202 C221 C216 115.6(2) . . ? C220 C221 C216 119.4(2) . . ? O202 C222 C223 105.9(2) . . ? O202 C222 H22F 110.5 . . ? C223 C222 H22F 110.5 . . ? O202 C222 H22G 110.5 . . ? C223 C222 H22G 110.5 . . ? H22F C222 H22G 108.7 . . ? N205 C223 C222 109.1(2) . . ? N205 C223 H22J 109.9 . . ? C222 C223 H22J 109.9 . . ? N205 C223 H22K 109.9 . . ? C222 C223 H22K 109.9 . . ? H22J C223 H22K 108.3 . . ? N205 C224 H22A 109.5 . . ? N205 C224 H22B 109.5 . . ? H22A C224 H22B 109.5 . . ? N205 C224 H22C 109.5 . . ? H22A C224 H22C 109.5 . . ? H22B C224 H22C 109.5 . . ? N205 C225 C226 113.6(3) . . ? N205 C225 H22D 108.8 . . ? C226 C225 H22D 108.8 . . ? N205 C225 H22E 108.8 . . ? C226 C225 H22E 108.8 . . ? H22D C225 H22E 107.7 . . ? O201 C226 C225 111.6(2) . . ? O201 C226 H22H 109.3 . . ? C225 C226 H22H 109.3 . . ? O201 C226 H22I 109.3 . . ? C225 C226 H22I 109.3 . . ? H22H C226 H22I 108.0 . . ? O201 C227 C228 124.1(3) . . ? O201 C227 C232 116.8(2) . . ? C228 C227 C232 119.1(3) . . ? C229 C228 C227 120.3(3) . . ? C229 C228 H228 119.8 . . ? C227 C228 H228 119.8 . . ? C230 C229 C228 120.8(3) . . ? C230 C229 H229 119.6 . . ? C228 C229 H229 119.6 . . ? C229 C230 C231 119.3(3) . . ? C229 C230 H230 120.3 . . ? C231 C230 H230 120.3 . . ? C232 C231 C230 121.0(3) . . ? C232 C231 H231 119.5 . . ? C230 C231 H231 119.5 . . ? C231 C232 C227 119.5(2) . . ? C231 C232 N201 118.8(2) . . ? C227 C232 N201 121.7(3) . . ? C201 N201 C232 118.7(2) . . ? C201 N201 Pd2 111.08(18) . . ? C232 N201 Pd2 130.18(17) . . ? C205 N202 C202 109.9(2) . . ? C205 N202 Pd2 133.5(2) . . ? C202 N202 Pd2 116.28(18) . . ? C211 N203 C214 110.0(2) . . ? C211 N203 Pd2 133.47(19) . . ? C214 N203 Pd2 116.50(17) . . ? C215 N204 C216 118.8(2) . . ? C215 N204 Pd2 111.48(16) . . ? C216 N204 Pd2 129.66(17) . . ? C225 N205 C223 114.0(2) . . ? C225 N205 C224 111.8(2) . . ? C223 N205 C224 111.4(2) . . ? C227 O201 C226 119.5(2) . . ? C221 O202 C222 118.7(2) . . ? N203 Pd2 N202 87.45(9) . . ? N203 Pd2 N204 79.76(9) . . ? N202 Pd2 N204 167.14(9) . . ? N203 Pd2 N201 167.17(8) . . ? N202 Pd2 N201 80.05(9) . . ? N204 Pd2 N201 112.65(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N101 C101 C102 N102 0.7(3) . . . . ? N101 C101 C102 C103 -179.6(3) . . . . ? N102 C102 C103 C104 0.9(3) . . . . ? C101 C102 C103 C104 -178.8(3) . . . . ? C102 C103 C104 C105 -0.1(3) . . . . ? C103 C104 C105 N102 -0.7(3) . . . . ? C103 C104 C105 C106 -175.2(2) . . . . ? N102 C105 C106 C111 17.0(4) . . . . ? C104 C105 C106 C111 -169.3(2) . . . . ? N102 C105 C106 C109 140.2(3) . . . . ? C104 C105 C106 C109 -46.1(4) . . . . ? N102 C105 C106 C107 -103.2(3) . . . . ? C104 C105 C106 C107 70.4(3) . . . . ? C105 C106 C107 C108 75.0(3) . . . . ? C111 C106 C107 C108 -49.5(3) . . . . ? C109 C106 C107 C108 -166.8(2) . . . . ? C105 C106 C109 C110 -65.6(3) . . . . ? C111 C106 C109 C110 60.9(3) . . . . ? C107 C106 C109 C110 177.5(2) . . . . ? C105 C106 C111 N103 -17.5(4) . . . . ? C109 C106 C111 N103 -141.1(2) . . . . ? C107 C106 C111 N103 102.7(3) . . . . ? C105 C106 C111 C112 169.7(2) . . . . ? C109 C106 C111 C112 46.1(4) . . . . ? C107 C106 C111 C112 -70.1(3) . . . . ? N103 C111 C112 C113 -0.3(3) . . . . ? C106 C111 C112 C113 173.5(3) . . . . ? C111 C112 C113 C114 0.5(3) . . . . ? C112 C113 C114 N103 -0.5(3) . . . . ? C112 C113 C114 C115 177.8(3) . . . . ? N103 C114 C115 N104 1.3(4) . . . . ? C113 C114 C115 N104 -176.9(3) . . . . ? C121 C116 C117 C118 1.6(4) . . . . ? N104 C116 C117 C118 -178.0(2) . . . . ? C116 C117 C118 C119 0.2(4) . . . . ? C117 C118 C119 C120 -1.9(5) . . . . ? C118 C119 C120 C121 1.8(5) . . . . ? C119 C120 C121 O101 -177.0(3) . . . . ? C119 C120 C121 C116 -0.1(4) . . . . ? C117 C116 C121 O101 175.5(2) . . . . ? N104 C116 C121 O101 -5.0(4) . . . . ? C117 C116 C121 C120 -1.6(4) . . . . ? N104 C116 C121 C120 178.0(2) . . . . ? O101 C122 C123 N105 -41.5(3) . . . . ? N105 C125 C126 O102 -74.6(3) . . . . ? O102 C127 C128 C129 -178.3(3) . . . . ? C132 C127 C128 C129 2.4(4) . . . . ? C127 C128 C129 C130 -0.4(4) . . . . ? C128 C129 C130 C131 -1.4(4) . . . . ? C129 C130 C131 C132 1.4(4) . . . . ? C130 C131 C132 C127 0.6(4) . . . . ? C130 C131 C132 N101 -179.7(2) . . . . ? O102 C127 C132 C131 178.1(2) . . . . ? C128 C127 C132 C131 -2.5(4) . . . . ? O102 C127 C132 N101 -1.6(4) . . . . ? C128 C127 C132 N101 177.8(2) . . . . ? C102 C101 N101 C132 179.5(2) . . . . ? C102 C101 N101 Pd1 -3.3(3) . . . . ? C131 C132 N101 C101 61.3(3) . . . . ? C127 C132 N101 C101 -119.0(3) . . . . ? C131 C132 N101 Pd1 -115.3(3) . . . . ? C127 C132 N101 Pd1 64.4(3) . . . . ? C104 C105 N102 C102 1.3(3) . . . . ? C106 C105 N102 C102 176.0(2) . . . . ? C104 C105 N102 Pd1 176.06(19) . . . . ? C106 C105 N102 Pd1 -9.2(4) . . . . ? C103 C102 N102 C105 -1.4(3) . . . . ? C101 C102 N102 C105 178.4(2) . . . . ? C103 C102 N102 Pd1 -177.17(17) . . . . ? C101 C102 N102 Pd1 2.6(3) . . . . ? C112 C111 N103 C114 0.0(3) . . . . ? C106 C111 N103 C114 -174.2(2) . . . . ? C112 C111 N103 Pd1 -175.45(19) . . . . ? C106 C111 N103 Pd1 10.4(4) . . . . ? C113 C114 N103 C111 0.4(3) . . . . ? C115 C114 N103 C111 -178.4(2) . . . . ? C113 C114 N103 Pd1 176.68(17) . . . . ? C115 C114 N103 Pd1 -2.1(3) . . . . ? C114 C115 N104 C116 179.4(2) . . . . ? C114 C115 N104 Pd1 0.0(3) . . . . ? C117 C116 N104 C115 -132.6(3) . . . . ? C121 C116 N104 C115 47.8(4) . . . . ? C117 C116 N104 Pd1 46.7(3) . . . . ? C121 C116 N104 Pd1 -132.9(2) . . . . ? C122 C123 N105 C125 169.6(2) . . . . ? C122 C123 N105 C124 -63.0(3) . . . . ? C126 C125 N105 C123 -80.0(3) . . . . ? C126 C125 N105 C124 152.8(2) . . . . ? C120 C121 O101 C122 -42.4(4) . . . . ? C116 C121 O101 C122 140.7(2) . . . . ? C123 C122 O101 C121 -55.8(3) . . . . ? C128 C127 O102 C126 4.8(4) . . . . ? C132 C127 O102 C126 -175.8(2) . . . . ? C125 C126 O102 C127 171.2(2) . . . . ? N201 C201 C202 N202 -1.1(4) . . . . ? N201 C201 C202 C203 175.8(3) . . . . ? N202 C202 C203 C204 -1.1(3) . . . . ? C201 C202 C203 C204 -178.1(3) . . . . ? C202 C203 C204 C205 0.9(3) . . . . ? C203 C204 C205 N202 -0.4(3) . . . . ? C203 C204 C205 C206 -176.7(3) . . . . ? N202 C205 C206 C211 18.4(4) . . . . ? C204 C205 C206 C211 -165.8(3) . . . . ? N202 C205 C206 C209 141.0(3) . . . . ? C204 C205 C206 C209 -43.2(4) . . . . ? N202 C205 C206 C207 -102.2(3) . . . . ? C204 C205 C206 C207 73.6(3) . . . . ? C211 C206 C207 C208 -61.6(3) . . . . ? C205 C206 C207 C208 63.0(3) . . . . ? C209 C206 C207 C208 -179.0(3) . . . . ? C211 C206 C209 C210 56.3(3) . . . . ? C205 C206 C209 C210 -69.5(3) . . . . ? C207 C206 C209 C210 172.8(3) . . . . ? C205 C206 C211 N203 -15.9(4) . . . . ? C209 C206 C211 N203 -138.5(3) . . . . ? C207 C206 C211 N203 105.3(3) . . . . ? C205 C206 C211 C212 169.8(2) . . . . ? C209 C206 C211 C212 47.2(4) . . . . ? C207 C206 C211 C212 -69.0(3) . . . . ? N203 C211 C212 C213 0.7(3) . . . . ? C206 C211 C212 C213 175.8(3) . . . . ? C211 C212 C213 C214 0.1(3) . . . . ? C212 C213 C214 N203 -0.8(3) . . . . ? C212 C213 C214 C215 -177.1(3) . . . . ? N203 C214 C215 N204 -0.1(3) . . . . ? C213 C214 C215 N204 176.1(3) . . . . ? C221 C216 C217 C218 -0.2(4) . . . . ? N204 C216 C217 C218 -179.2(2) . . . . ? C216 C217 C218 C219 -0.2(4) . . . . ? C217 C218 C219 C220 0.1(4) . . . . ? C218 C219 C220 C221 0.4(4) . . . . ? C219 C220 C221 O202 179.5(3) . . . . ? C219 C220 C221 C216 -0.9(4) . . . . ? C217 C216 C221 O202 -179.6(2) . . . . ? N204 C216 C221 O202 -0.5(3) . . . . ? C217 C216 C221 C220 0.8(4) . . . . ? N204 C216 C221 C220 179.8(2) . . . . ? O202 C222 C223 N205 177.0(2) . . . . ? N205 C225 C226 O201 -81.8(3) . . . . ? O201 C227 C228 C229 -178.2(3) . . . . ? C232 C227 C228 C229 1.6(4) . . . . ? C227 C228 C229 C230 -0.6(4) . . . . ? C228 C229 C230 C231 -0.3(4) . . . . ? C229 C230 C231 C232 0.2(4) . . . . ? C230 C231 C232 C227 0.9(4) . . . . ? C230 C231 C232 N201 179.5(2) . . . . ? O201 C227 C232 C231 178.1(2) . . . . ? C228 C227 C232 C231 -1.8(4) . . . . ? O201 C227 C232 N201 -0.5(4) . . . . ? C228 C227 C232 N201 179.6(2) . . . . ? C202 C201 N201 C232 -179.6(2) . . . . ? C202 C201 N201 Pd2 -2.5(3) . . . . ? C231 C232 N201 C201 128.5(3) . . . . ? C227 C232 N201 C201 -52.9(3) . . . . ? C231 C232 N201 Pd2 -48.0(3) . . . . ? C227 C232 N201 Pd2 130.6(2) . . . . ? C204 C205 N202 C202 -0.3(3) . . . . ? C206 C205 N202 C202 176.3(2) . . . . ? C204 C205 N202 Pd2 172.37(19) . . . . ? C206 C205 N202 Pd2 -11.1(4) . . . . ? C203 C202 N202 C205 0.9(3) . . . . ? C201 C202 N202 C205 178.7(2) . . . . ? C203 C202 N202 Pd2 -173.22(17) . . . . ? C201 C202 N202 Pd2 4.6(3) . . . . ? C212 C211 N203 C214 -1.3(3) . . . . ? C206 C211 N203 C214 -176.6(2) . . . . ? C212 C211 N203 Pd2 -179.13(19) . . . . ? C206 C211 N203 Pd2 5.6(4) . . . . ? C213 C214 N203 C211 1.3(3) . . . . ? C215 C214 N203 C211 178.6(2) . . . . ? C213 C214 N203 Pd2 179.60(17) . . . . ? C215 C214 N203 Pd2 -3.1(3) . . . . ? C214 C215 N204 C216 -176.1(2) . . . . ? C214 C215 N204 Pd2 2.9(3) . . . . ? C217 C216 N204 C215 -58.1(3) . . . . ? C221 C216 N204 C215 122.9(3) . . . . ? C217 C216 N204 Pd2 123.1(2) . . . . ? C221 C216 N204 Pd2 -55.9(3) . . . . ? C226 C225 N205 C223 74.0(3) . . . . ? C226 C225 N205 C224 -158.6(2) . . . . ? C222 C223 N205 C225 -123.3(3) . . . . ? C222 C223 N205 C224 109.0(3) . . . . ? C228 C227 O201 C226 29.2(4) . . . . ? C232 C227 O201 C226 -150.7(2) . . . . ? C225 C226 O201 C227 125.6(3) . . . . ? C220 C221 O202 C222 -16.5(4) . . . . ? C216 C221 O202 C222 163.8(2) . . . . ? C223 C222 O202 C221 -159.6(2) . . . . ? _refine_diff_density_max 2.523 _refine_diff_density_min -0.645 _refine_diff_density_rms 0.164 _shelxl_version_number 2012-4 _shelx_res_file ; TITL lppd_PdLNMe in P 21/c CELL 0.71073 9.7164 23.2090 25.1870 90.000 91.066 90.000 ZERR 8.00 0.0009 0.0020 0.0030 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O PD UNIT 256 280 40 16 8 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! MERG 2 OMIT -4.00 180.00 OMIT 0 2 1 OMIT -1 2 16 FMAP 2 PLAN 20 size 0.2 0.2 0.2 rem yellow block ACTA 52 BOND $H CONF L.S. 16 TEMP -150.00 WGHT 0.073500 FVAR 2.24103 MOLE 1 C101 1 0.528454 0.337672 0.150661 11.00000 0.01712 0.02266 = 0.02563 -0.00200 -0.00409 0.00250 AFIX 43 H101 2 0.618159 0.321693 0.154260 11.00000 -1.20000 AFIX 0 C102 1 0.504722 0.387773 0.119531 11.00000 0.01862 0.01967 = 0.02578 0.00075 0.00087 -0.00052 C103 1 0.582136 0.425796 0.088255 11.00000 0.01844 0.03060 = 0.02424 -0.00024 0.00101 -0.00318 AFIX 43 H103 2 0.677728 0.423591 0.081254 11.00000 -1.20000 AFIX 0 C104 1 0.489239 0.467342 0.069715 11.00000 0.02660 0.02308 = 0.02596 0.00410 0.00072 -0.00380 AFIX 43 H104 2 0.510729 0.499060 0.047515 11.00000 -1.20000 AFIX 0 C105 1 0.357881 0.454267 0.089532 11.00000 0.02268 0.02063 = 0.02194 0.00166 -0.00247 -0.00120 C106 1 0.222986 0.484398 0.077072 11.00000 0.02626 0.01976 = 0.02443 0.00220 -0.00182 0.00044 C107 1 0.180927 0.469766 0.018582 11.00000 0.02948 0.03100 = 0.02519 0.00037 -0.00375 0.00468 AFIX 23 H10F 2 0.109655 0.497480 0.006363 11.00000 -1.20000 H10G 2 0.262139 0.474862 -0.004110 11.00000 -1.20000 AFIX 0 C108 1 0.125557 0.408669 0.011037 11.00000 0.03671 0.02930 = 0.03211 -0.00705 -0.00795 0.00670 AFIX 137 H10A 2 0.185117 0.381449 0.030360 11.00000 -1.50000 H10B 2 0.124042 0.398966 -0.026837 11.00000 -1.50000 H10C 2 0.031981 0.406386 0.024747 11.00000 -1.50000 AFIX 0 C109 1 0.243114 0.550742 0.080374 11.00000 0.03127 0.01816 = 0.03412 0.00397 -0.00292 -0.00014 AFIX 23 H10D 2 0.317515 0.561984 0.056126 11.00000 -1.20000 H10E 2 0.157444 0.569779 0.067702 11.00000 -1.20000 AFIX 0 C110 1 0.278723 0.572868 0.135760 11.00000 0.05047 0.02339 = 0.03805 -0.00120 -0.00637 -0.00274 AFIX 137 H11A 2 0.205883 0.561884 0.160180 11.00000 -1.50000 H11B 2 0.286948 0.614940 0.134892 11.00000 -1.50000 H11C 2 0.366292 0.556042 0.147909 11.00000 -1.50000 AFIX 0 C111 1 0.105205 0.467189 0.112232 11.00000 0.02110 0.02187 = 0.02613 -0.00225 -0.00306 0.00264 C112 1 -0.025318 0.492655 0.116295 11.00000 0.02930 0.02462 = 0.02904 -0.00164 -0.00661 0.00789 AFIX 43 H112 2 -0.054265 0.527289 0.099370 11.00000 -1.20000 AFIX 0 C113 1 -0.105398 0.458570 0.149360 11.00000 0.01975 0.03337 = 0.03037 -0.00709 -0.00375 0.00567 AFIX 43 H113 2 -0.198145 0.465207 0.158968 11.00000 -1.20000 AFIX 0 C114 1 -0.020959 0.412503 0.165513 11.00000 0.01797 0.02607 = 0.02796 -0.00578 0.00184 0.00163 C115 1 -0.030398 0.364039 0.198896 11.00000 0.01998 0.02825 = 0.02577 -0.00483 0.00131 -0.00348 AFIX 43 H115 2 -0.113856 0.355328 0.216242 11.00000 -1.20000 AFIX 0 C116 1 0.070802 0.282320 0.239611 11.00000 0.02653 0.02247 = 0.02519 -0.00267 0.00458 -0.00189 C117 1 0.175258 0.273209 0.276723 11.00000 0.02891 0.02513 = 0.02827 -0.00341 0.00273 -0.00123 AFIX 43 H117 2 0.248205 0.300347 0.279625 11.00000 -1.20000 AFIX 0 C118 1 0.176126 0.225545 0.309724 11.00000 0.03953 0.03423 = 0.02736 -0.00021 0.00273 0.00092 AFIX 43 H118 2 0.248636 0.220087 0.335047 11.00000 -1.20000 AFIX 0 C119 1 0.069611 0.185747 0.305374 11.00000 0.05208 0.02703 = 0.03619 0.00431 0.00724 -0.00290 AFIX 43 H119 2 0.070663 0.152284 0.327101 11.00000 -1.20000 AFIX 0 C120 1 -0.038156 0.194672 0.269466 11.00000 0.04187 0.02870 = 0.03362 -0.00023 0.00737 -0.01096 AFIX 43 H120 2 -0.111862 0.167817 0.267494 11.00000 -1.20000 AFIX 0 C121 1 -0.039323 0.242763 0.236187 11.00000 0.02942 0.02669 = 0.02800 -0.00260 0.00483 -0.00455 C122 1 -0.205920 0.208195 0.172011 11.00000 0.02774 0.03057 = 0.03734 -0.00422 0.00109 -0.00743 AFIX 23 H12E 2 -0.277938 0.223418 0.147482 11.00000 -1.20000 H12F 2 -0.250585 0.181271 0.196843 11.00000 -1.20000 AFIX 0 C123 1 -0.100239 0.175600 0.140297 11.00000 0.02842 0.02654 = 0.03626 -0.00293 0.00166 -0.00336 AFIX 23 H12J 2 -0.049788 0.148774 0.164223 11.00000 -1.20000 H12K 2 -0.148395 0.152323 0.112750 11.00000 -1.20000 AFIX 0 C124 1 -0.068075 0.251459 0.075810 11.00000 0.03611 0.04671 = 0.04644 0.01565 0.00417 0.01214 AFIX 137 H12G 2 -0.115834 0.228291 0.048656 11.00000 -1.50000 H12H 2 0.002029 0.275340 0.059035 11.00000 -1.50000 H12I 2 -0.134580 0.276301 0.093551 11.00000 -1.50000 AFIX 0 C125 1 0.111466 0.180856 0.093086 11.00000 0.02572 0.03380 = 0.02886 -0.00279 -0.00257 0.00044 AFIX 23 H12C 2 0.155906 0.204180 0.065312 11.00000 -1.20000 H12D 2 0.075235 0.145336 0.076140 11.00000 -1.20000 AFIX 0 C126 1 0.217099 0.164829 0.134776 11.00000 0.02747 0.02213 = 0.03120 -0.00304 -0.00157 -0.00268 AFIX 23 H12A 2 0.171303 0.149588 0.166630 11.00000 -1.20000 H12B 2 0.279118 0.134676 0.121052 11.00000 -1.20000 AFIX 0 C127 1 0.382892 0.212088 0.190541 11.00000 0.02188 0.02162 = 0.02444 -0.00094 -0.00175 0.00294 C128 1 0.411022 0.161895 0.219250 11.00000 0.02713 0.01893 = 0.02998 0.00079 0.00239 0.00065 AFIX 43 H128 2 0.368809 0.126592 0.208984 11.00000 -1.20000 AFIX 0 C129 1 0.500615 0.163505 0.262787 11.00000 0.02899 0.02204 = 0.02989 0.00385 -0.00118 0.00493 AFIX 43 H129 2 0.518726 0.129193 0.282260 11.00000 -1.20000 AFIX 0 C130 1 0.563940 0.214365 0.278240 11.00000 0.02811 0.02801 = 0.02669 0.00206 -0.00462 0.00277 AFIX 43 H130 2 0.623549 0.215428 0.308552 11.00000 -1.20000 AFIX 0 C131 1 0.538650 0.263944 0.248530 11.00000 0.02380 0.02178 = 0.03197 -0.00049 -0.00205 0.00146 AFIX 43 H131 2 0.583196 0.298893 0.258355 11.00000 -1.20000 AFIX 0 C132 1 0.450049 0.263270 0.205059 11.00000 0.02262 0.01994 = 0.02623 0.00150 0.00285 0.00248 N101 3 0.424146 0.314082 0.174215 11.00000 0.01696 0.01891 = 0.02830 0.00086 -0.00344 0.00274 N102 3 0.370692 0.405982 0.118602 11.00000 0.01854 0.01895 = 0.02717 0.00323 -0.00008 -0.00047 N103 3 0.104774 0.419018 0.142247 11.00000 0.01886 0.01934 = 0.02775 0.00041 0.00024 0.00295 N104 3 0.077796 0.331350 0.205517 11.00000 0.02003 0.02264 = 0.02610 -0.00197 0.00450 -0.00467 N105 3 -0.002161 0.213315 0.114898 11.00000 0.02783 0.02915 = 0.02994 0.00175 0.00086 0.00172 O101 4 -0.146414 0.255050 0.201619 11.00000 0.02578 0.02614 = 0.03883 -0.00411 -0.00148 -0.00608 O102 4 0.294425 0.215612 0.148216 11.00000 0.02722 0.02060 = 0.02744 0.00197 -0.00599 -0.00206 PD1 5 0.243919 0.362274 0.161936 11.00000 0.01744 0.01672 = 0.02541 0.00116 0.00011 -0.00025 MOLE 2 C201 1 0.743265 0.343862 0.345558 11.00000 0.02184 0.02565 = 0.02814 -0.00760 0.00209 -0.00329 AFIX 43 H201 2 0.826920 0.351264 0.327856 11.00000 -1.20000 AFIX 0 C202 1 0.731139 0.296352 0.380364 11.00000 0.02015 0.02459 = 0.03253 -0.00631 -0.00311 0.00292 C203 1 0.811564 0.249511 0.397205 11.00000 0.02336 0.02996 = 0.04043 -0.00775 -0.00854 0.00550 AFIX 43 H203 2 0.903028 0.241054 0.387028 11.00000 -1.20000 AFIX 0 C204 1 0.731768 0.218018 0.431525 11.00000 0.03014 0.02303 = 0.03868 -0.00239 -0.01022 0.00611 AFIX 43 H204 2 0.759227 0.183937 0.449729 11.00000 -1.20000 AFIX 0 C205 1 0.602608 0.245205 0.434850 11.00000 0.02885 0.02378 = 0.02995 -0.00388 -0.00535 0.00327 C206 1 0.481722 0.228960 0.469350 11.00000 0.03114 0.02213 = 0.02743 0.00191 -0.00277 0.00290 C207 1 0.516943 0.245937 0.528233 11.00000 0.03772 0.03990 = 0.02983 0.00480 -0.00488 0.00787 AFIX 23 H20A 2 0.441637 0.232499 0.551102 11.00000 -1.20000 H20B 2 0.601992 0.225560 0.539628 11.00000 -1.20000 AFIX 0 C208 1 0.537416 0.310387 0.536987 11.00000 0.05185 0.04116 = 0.03569 -0.00819 -0.01064 0.00453 AFIX 137 H20E 2 0.617710 0.323448 0.517316 11.00000 -1.50000 H20F 2 0.552298 0.317951 0.574941 11.00000 -1.50000 H20G 2 0.455400 0.331195 0.524332 11.00000 -1.50000 AFIX 0 C209 1 0.461874 0.162230 0.467846 11.00000 0.03866 0.02231 = 0.03967 0.00788 0.00265 0.00416 AFIX 23 H20C 2 0.551031 0.143582 0.476681 11.00000 -1.20000 H20D 2 0.395974 0.151182 0.495573 11.00000 -1.20000 AFIX 0 C210 1 0.409760 0.139302 0.414775 11.00000 0.04619 0.02360 = 0.04372 -0.00033 0.00238 0.00098 AFIX 137 H21A 2 0.316404 0.153710 0.407694 11.00000 -1.50000 H21B 2 0.408474 0.097094 0.415725 11.00000 -1.50000 H21C 2 0.470735 0.152292 0.386620 11.00000 -1.50000 AFIX 0 C211 1 0.347255 0.257818 0.453807 11.00000 0.02733 0.02129 = 0.02372 -0.00084 -0.00026 0.00077 C212 1 0.214424 0.245498 0.472551 11.00000 0.03296 0.02437 = 0.03078 0.00381 0.00378 -0.00315 AFIX 43 H212 2 0.191549 0.215263 0.496232 11.00000 -1.20000 AFIX 0 C213 1 0.123081 0.285074 0.450487 11.00000 0.02685 0.02740 = 0.02788 -0.00135 0.00196 -0.00328 AFIX 43 H213 2 0.026794 0.287194 0.456087 11.00000 -1.20000 AFIX 0 C214 1 0.200988 0.321273 0.418325 11.00000 0.01902 0.02383 = 0.02529 -0.00280 -0.00074 0.00025 C215 1 0.180002 0.370400 0.386498 11.00000 0.01971 0.02367 = 0.02405 -0.00310 -0.00080 0.00207 AFIX 43 H215 2 0.090486 0.386091 0.381219 11.00000 -1.20000 AFIX 0 C216 1 0.268947 0.445888 0.334687 11.00000 0.02283 0.02030 = 0.02627 -0.00019 0.00418 0.00467 C217 1 0.179517 0.449674 0.291657 11.00000 0.02538 0.02130 = 0.02997 -0.00036 0.00164 0.00190 AFIX 43 H217 2 0.126808 0.416977 0.281203 11.00000 -1.20000 AFIX 0 C218 1 0.165815 0.500848 0.263471 11.00000 0.03173 0.02926 = 0.02559 0.00042 -0.00414 0.00574 AFIX 43 H218 2 0.104425 0.503343 0.233762 11.00000 -1.20000 AFIX 0 C219 1 0.243073 0.548226 0.279347 11.00000 0.03636 0.02159 = 0.03199 0.00664 0.00071 0.00625 AFIX 43 H219 2 0.233897 0.583336 0.260218 11.00000 -1.20000 AFIX 0 C220 1 0.333690 0.545500 0.322643 11.00000 0.03047 0.01825 = 0.03144 -0.00120 0.00054 0.00077 AFIX 43 H220 2 0.385384 0.578461 0.333144 11.00000 -1.20000 AFIX 0 C221 1 0.347846 0.493875 0.350467 11.00000 0.02237 0.02309 = 0.02417 -0.00015 0.00152 0.00171 C222 1 0.540930 0.525995 0.402962 11.00000 0.02724 0.02823 = 0.02659 -0.00253 -0.00073 -0.00226 AFIX 23 H22F 2 0.505002 0.560512 0.421178 11.00000 -1.20000 H22G 2 0.582929 0.538184 0.369258 11.00000 -1.20000 AFIX 0 C223 1 0.646817 0.494898 0.438348 11.00000 0.02690 0.03498 = 0.03214 -0.00041 -0.00082 -0.00400 AFIX 23 H22J 2 0.604816 0.484310 0.472505 11.00000 -1.20000 H22K 2 0.677535 0.459124 0.420738 11.00000 -1.20000 AFIX 0 C224 1 0.768830 0.553450 0.502966 11.00000 0.03909 0.05275 = 0.03788 -0.01527 0.00365 -0.00603 AFIX 137 H22A 2 0.787386 0.520977 0.526917 11.00000 -1.50000 H22B 2 0.680194 0.570906 0.511624 11.00000 -1.50000 H22C 2 0.842028 0.582234 0.507142 11.00000 -1.50000 AFIX 0 C225 1 0.894762 0.508673 0.432286 11.00000 0.02402 0.03441 = 0.03708 -0.00427 -0.00218 0.00095 AFIX 23 H22D 2 0.902178 0.468899 0.446253 11.00000 -1.20000 H22E 2 0.970156 0.531595 0.448738 11.00000 -1.20000 AFIX 0 C226 1 0.913593 0.507315 0.373262 11.00000 0.03149 0.03225 = 0.03394 -0.00770 0.00484 -0.00548 AFIX 23 H22H 2 0.875634 0.543105 0.357402 11.00000 -1.20000 H22I 2 1.013112 0.505851 0.365625 11.00000 -1.20000 AFIX 0 C227 1 0.753576 0.466255 0.308404 11.00000 0.02822 0.02385 = 0.02582 -0.00319 0.00510 0.00063 C228 1 0.759297 0.512000 0.272464 11.00000 0.03916 0.02427 = 0.03058 -0.00193 0.00982 -0.00085 AFIX 43 H228 2 0.832244 0.539164 0.275103 11.00000 -1.20000 AFIX 0 C229 1 0.659071 0.517943 0.232980 11.00000 0.04803 0.02532 = 0.02960 0.00175 0.01238 0.00733 AFIX 43 H229 2 0.663481 0.549410 0.208949 11.00000 -1.20000 AFIX 0 C230 1 0.552961 0.478683 0.228171 11.00000 0.03554 0.03269 = 0.02906 -0.00313 0.00067 0.01070 AFIX 43 H230 2 0.484287 0.483115 0.201138 11.00000 -1.20000 AFIX 0 C231 1 0.547548 0.432348 0.263463 11.00000 0.02707 0.02647 = 0.03134 -0.00387 0.00301 0.00462 AFIX 43 H231 2 0.474734 0.405189 0.260185 11.00000 -1.20000 AFIX 0 C232 1 0.646451 0.425408 0.303059 11.00000 0.02761 0.02239 = 0.02703 -0.00369 0.00886 0.00243 N201 3 0.635576 0.377498 0.338378 11.00000 0.02012 0.02096 = 0.02766 -0.00091 0.00276 0.00002 N202 3 0.605478 0.291926 0.403595 11.00000 0.02192 0.02232 = 0.02916 -0.00204 -0.00135 0.00355 N203 3 0.335917 0.303897 0.421954 11.00000 0.01982 0.02018 = 0.02882 0.00086 -0.00158 0.00026 N204 3 0.287333 0.393992 0.364287 11.00000 0.02055 0.02078 = 0.02667 0.00069 -0.00066 0.00358 N205 3 0.764167 0.532859 0.447944 11.00000 0.02531 0.03207 = 0.03343 -0.00487 0.00147 -0.00211 O201 4 0.845725 0.458043 0.349202 11.00000 0.03578 0.02579 = 0.03051 -0.00104 -0.00152 -0.00568 O202 4 0.433315 0.485526 0.393037 11.00000 0.02679 0.02668 = 0.02983 0.00222 -0.00557 -0.00275 PD2 5 0.466586 0.347058 0.380395 11.00000 0.01962 0.01839 = 0.02572 0.00078 0.00042 0.00125 HKLF 4 REM lppd_PdLNMe in P 21/c REM R1 = 0.0494 for 12143 Fo > 4sig(Fo) and 0.0622 for all 15119 data REM 727 parameters refined using 0 restraints END WGHT 0.0731 0.0000 REM Highest difference peak 2.523, deepest hole -0.645, 1-sigma level 0.164 Q1 1 0.8248 0.3610 0.0783 11.00000 0.05 2.04 Q2 1 0.0484 0.3474 0.2968 11.00000 0.05 1.99 Q3 1 0.7541 0.4430 0.3377 11.00000 0.05 1.73 Q4 1 0.4683 0.3771 0.3805 11.00000 0.05 1.66 Q5 1 0.5360 0.4275 0.1189 11.00000 0.05 1.63 Q6 1 0.0239 0.3481 -0.0562 11.00000 0.05 1.32 Q7 1 0.5715 0.3215 0.3828 11.00000 0.05 1.30 Q8 1 -0.3115 0.1381 0.0993 11.00000 0.05 1.28 Q9 1 -0.0500 0.4294 0.2032 11.00000 0.05 1.01 Q10 1 0.8225 0.5546 0.5764 11.00000 0.05 0.98 Q11 1 -0.1761 0.3343 0.0769 11.00000 0.05 0.94 Q12 1 0.1531 0.3986 0.1510 11.00000 0.05 0.92 Q13 1 0.3315 0.3898 0.1347 11.00000 0.05 0.87 Q14 1 0.3727 0.3706 0.3551 11.00000 0.05 0.86 Q15 1 0.2289 0.3394 0.1220 11.00000 0.05 0.86 Q16 1 0.4042 0.3688 0.3459 11.00000 0.05 0.85 Q17 1 0.0455 0.3753 0.2970 11.00000 0.05 0.84 Q18 1 0.1505 0.3310 0.1514 11.00000 0.05 0.81 Q19 1 0.3397 0.3302 0.1759 11.00000 0.05 0.81 Q20 1 0.3991 0.6530 0.1418 11.00000 0.05 0.79 ; data_Pd(LNMes) _database_code_depnum_ccdc_archive 'CCDC 895817' #TrackingRef 'combined_CIF.cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H50 N5 O2 Pd' _chemical_formula_sum 'C43 H50 N5 O2 Pd' _chemical_formula_weight 775.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' 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 16.211(6) _cell_length_b 12.099(4) _cell_length_c 20.592(7) _cell_angle_alpha 90.00 _cell_angle_beta 111.477(5) _cell_angle_gamma 90.00 _cell_volume 3758(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10245 _cell_measurement_theta_min 28 _cell_measurement_theta_max 2.2 _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1620 _exptl_absorpt_coefficient_mu 0.537 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.873 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_specimen_support Loop _diffrn_detector CCD _diffrn_measurement_device ; AFC8: Eulerian 3 circle ; _diffrn_measurement_device_type ; Rigaku Saturn70 (2x2 bin mode) ; _diffrn_detector_area_resol_mean 28.5714 _diffrn_measurement_method 'profile data from \w-scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 36963 _diffrn_reflns_av_R_equivalents 0.0964 _diffrn_reflns_av_sigmaI/netI 0.0766 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 25.37 _reflns_number_total 6873 _reflns_number_gt 6133 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009) ; _computing_cell_refinement ; CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009) ; _computing_data_reduction ; CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009) ; _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen et al., 2004)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0701P)^2^+6.2634P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0028(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6873 _refine_ls_number_parameters 468 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0622 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1481 _refine_ls_wR_factor_gt 0.1439 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0995(2) 0.2067(3) 0.4115(2) 0.0308(8) Uani 1 1 d . . . H1 H 0.1229 0.2685 0.4410 0.037 Uiso 1 1 calc R . . C2 C 0.0097(3) 0.2036(3) 0.3657(2) 0.0316(8) Uani 1 1 d . . . C3 C -0.0668(3) 0.2675(4) 0.3506(2) 0.0367(9) Uani 1 1 d . . . H3 H -0.0716 0.3362 0.3713 0.044 Uiso 1 1 calc R . . C4 C -0.1350(3) 0.2113(3) 0.2992(2) 0.0369(9) Uani 1 1 d . . . H4 H -0.1947 0.2354 0.2780 0.044 Uiso 1 1 calc R . . C5 C -0.0996(2) 0.1123(3) 0.2843(2) 0.0305(8) Uani 1 1 d . . . C6 C -0.1458(3) 0.0243(4) 0.2301(2) 0.0317(8) Uani 1 1 d . . . C7 C -0.1589(3) 0.0713(4) 0.1566(2) 0.0386(10) Uani 1 1 d . . . H7A H -0.1965 0.0196 0.1206 0.046 Uiso 1 1 calc R . . H7B H -0.1907 0.1427 0.1503 0.046 Uiso 1 1 calc R . . C8 C -0.0725(3) 0.0889(4) 0.1450(2) 0.0460(11) Uani 1 1 d . . . H8A H -0.0349 0.1406 0.1801 0.069 Uiso 1 1 calc R . . H8B H -0.0851 0.1195 0.0983 0.069 Uiso 1 1 calc R . . H8C H -0.0416 0.0181 0.1492 0.069 Uiso 1 1 calc R . . C9 C -0.2400(3) 0.0033(4) 0.2322(2) 0.0392(11) Uani 1 1 d . . . H9A H -0.2742 0.0731 0.2207 0.047 Uiso 1 1 calc R . . H9B H -0.2713 -0.0516 0.1959 0.047 Uiso 1 1 calc R . . C10 C -0.2384(3) -0.0380(5) 0.3019(3) 0.0537(12) Uani 1 1 d . . . H10A H -0.2014 -0.1045 0.3153 0.081 Uiso 1 1 calc R . . H10B H -0.2989 -0.0558 0.2984 0.081 Uiso 1 1 calc R . . H10C H -0.2139 0.0194 0.3374 0.081 Uiso 1 1 calc R . . C11 C -0.0972(2) -0.0845(3) 0.2388(2) 0.0306(8) Uani 1 1 d . . . C12 C -0.1266(3) -0.1838(4) 0.2026(2) 0.0387(10) Uani 1 1 d . . . H12 H -0.1841 -0.1969 0.1688 0.046 Uiso 1 1 calc R . . C13 C -0.0577(3) -0.2602(3) 0.2244(2) 0.0389(10) Uani 1 1 d . . . H13 H -0.0592 -0.3345 0.2090 0.047 Uiso 1 1 calc R . . C14 C 0.0145(2) -0.2056(3) 0.2735(2) 0.0304(8) Uani 1 1 d . . . C15 C 0.1014(2) -0.2311(3) 0.3202(2) 0.0312(8) Uani 1 1 d . . . H15 H 0.1256 -0.3028 0.3210 0.037 Uiso 1 1 calc R . . C16 C 0.2315(2) -0.1806(3) 0.4151(2) 0.0296(8) Uani 1 1 d . . . C17 C 0.2477(3) -0.1499(3) 0.4832(2) 0.0368(9) Uani 1 1 d . . . H17 H 0.2035 -0.1106 0.4938 0.044 Uiso 1 1 calc R . . C18 C 0.3280(3) -0.1755(4) 0.5371(2) 0.0442(11) Uani 1 1 d . . . H18 H 0.3382 -0.1542 0.5838 0.053 Uiso 1 1 calc R . . C19 C 0.3919(3) -0.2321(4) 0.5212(2) 0.0479(12) Uani 1 1 d . . . H19 H 0.4462 -0.2508 0.5574 0.057 Uiso 1 1 calc R . . C20 C 0.3781(3) -0.2621(4) 0.4534(2) 0.0405(10) Uani 1 1 d . . . H20 H 0.4230 -0.3008 0.4434 0.049 Uiso 1 1 calc R . . C21 C 0.2979(2) -0.2357(3) 0.3991(2) 0.0327(9) Uani 1 1 d . . . C22 C 0.3525(3) -0.2680(3) 0.3062(2) 0.0355(9) Uani 1 1 d . . . H22A H 0.3701 -0.3464 0.3065 0.043 Uiso 1 1 calc R . . H22B H 0.4043 -0.2258 0.3373 0.043 Uiso 1 1 calc R . . C23 C 0.3224(3) -0.2223(3) 0.2333(2) 0.0368(9) Uani 1 1 d . . . H23A H 0.3597 -0.2542 0.2092 0.044 Uiso 1 1 calc R . . H23B H 0.2605 -0.2462 0.2076 0.044 Uiso 1 1 calc R . . C24 C 0.3360(3) -0.0582(3) 0.1685(2) 0.0338(9) Uani 1 1 d . . . C25 C 0.4219(3) -0.0324(4) 0.1735(2) 0.0366(9) Uani 1 1 d . . . C26 C 0.4995(3) -0.0518(4) 0.2400(2) 0.0409(10) Uani 1 1 d . . . H26A H 0.4901 -0.0126 0.2783 0.061 Uiso 1 1 calc R . . H26B H 0.5537 -0.0244 0.2348 0.061 Uiso 1 1 calc R . . H26C H 0.5054 -0.1312 0.2502 0.061 Uiso 1 1 calc R . . C27 C 0.4333(4) 0.0111(3) 0.1138(3) 0.0411(11) Uani 1 1 d . . . H27 H 0.4915 0.0283 0.1161 0.049 Uiso 1 1 calc R . . C28 C 0.3623(4) 0.0296(4) 0.0519(3) 0.0476(11) Uani 1 1 d . . . C29 C 0.3766(4) 0.0783(5) -0.0109(3) 0.0686(16) Uani 1 1 d . . . H29A H 0.4349 0.1138 0.0040 0.103 Uiso 1 1 calc R . . H29B H 0.3304 0.1332 -0.0332 0.103 Uiso 1 1 calc R . . H29C H 0.3737 0.0193 -0.0443 0.103 Uiso 1 1 calc R . . C30 C 0.2771(4) 0.0018(4) 0.0483(3) 0.0499(13) Uani 1 1 d . . . H30 H 0.2279 0.0140 0.0062 0.060 Uiso 1 1 calc R . . C31 C 0.2633(3) -0.0431(4) 0.1051(2) 0.0420(10) Uani 1 1 d . . . C32 C 0.1699(3) -0.0762(5) 0.0966(3) 0.0554(13) Uani 1 1 d . . . H32A H 0.1359 -0.0102 0.0985 0.083 Uiso 1 1 calc R . . H32B H 0.1719 -0.1268 0.1343 0.083 Uiso 1 1 calc R . . H32C H 0.1415 -0.1132 0.0515 0.083 Uiso 1 1 calc R . . C33 C 0.2709(3) -0.0365(4) 0.2586(2) 0.0344(9) Uani 1 1 d . . . H33A H 0.2231 -0.0837 0.2627 0.041 Uiso 1 1 calc R . . H33B H 0.2431 0.0256 0.2269 0.041 Uiso 1 1 calc R . . C34 C 0.3280(3) 0.0078(3) 0.3301(2) 0.0308(9) Uani 1 1 d . . . H34A H 0.3607 -0.0533 0.3608 0.037 Uiso 1 1 calc R . . H34B H 0.3716 0.0619 0.3258 0.037 Uiso 1 1 calc R . . C35 C 0.3031(3) 0.0869(3) 0.4279(2) 0.0305(8) Uani 1 1 d . . . C36 C 0.3924(2) 0.0849(3) 0.4700(2) 0.0337(9) Uani 1 1 d . . . H36 H 0.4354 0.0646 0.4508 0.040 Uiso 1 1 calc R . . C37 C 0.4188(3) 0.1126(4) 0.5404(2) 0.0403(10) Uani 1 1 d . . . H37 H 0.4799 0.1099 0.5691 0.048 Uiso 1 1 calc R . . C38 C 0.3581(3) 0.1437(4) 0.5687(2) 0.0381(10) Uani 1 1 d . . . H38 H 0.3767 0.1618 0.6169 0.046 Uiso 1 1 calc R . . C39 C 0.2684(3) 0.1486(3) 0.5261(2) 0.0346(9) Uani 1 1 d . . . H39 H 0.2261 0.1714 0.5454 0.042 Uiso 1 1 calc R . . C40 C 0.2404(2) 0.1208(3) 0.4564(2) 0.0279(8) Uani 1 1 d . . . N1 N 0.1494(2) 0.1202(3) 0.41187(16) 0.0289(7) Uani 1 1 d . . . N2 N -0.0125(2) 0.1099(3) 0.32434(16) 0.0293(7) Uani 1 1 d . . . N3 N -0.0118(2) -0.0994(3) 0.28100(17) 0.0294(7) Uani 1 1 d . . . N4 N 0.14790(19) -0.1532(3) 0.36245(16) 0.0284(7) Uani 1 1 d . . . N5 N 0.3264(2) -0.1013(3) 0.23010(17) 0.0331(7) Uani 1 1 d . . . O1 O 0.27968(17) -0.2584(2) 0.33007(15) 0.0351(6) Uani 1 1 d . . . O2 O 0.26976(17) 0.0597(2) 0.35865(13) 0.0307(6) Uani 1 1 d . . . Pd1 Pd 0.076339(17) -0.00533(2) 0.347032(15) 0.02556(15) Uani 1 1 d . . . C1S C 0.0615(6) 0.2279(9) 0.5795(5) 0.132(3) Uani 1 1 d DU . . H1S1 H 0.1113 0.1961 0.6180 0.198 Uiso 1 1 calc R . . H1S2 H 0.0245 0.2715 0.5984 0.198 Uiso 1 1 calc R . . H1S3 H 0.0841 0.2757 0.5514 0.198 Uiso 1 1 calc R . . C2S C 0.0136(5) 0.1474(6) 0.5400(4) 0.082(2) Uani 1 1 d DU . . H2S1 H -0.0113 0.1788 0.4923 0.098 Uiso 1 1 calc R . . H2S2 H -0.0373 0.1378 0.5552 0.098 Uiso 1 1 calc R . . C3S C 0.0433(3) 0.0273(5) 0.5303(2) 0.0516(12) Uani 1 1 d DU . . H3S1 H 0.0596 -0.0152 0.5743 0.062 Uiso 1 1 calc R . . H3S2 H 0.0947 0.0289 0.5153 0.062 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.036(2) 0.029(2) 0.0254(19) 0.0000(16) 0.0084(16) 0.0014(16) C2 0.034(2) 0.032(2) 0.027(2) -0.0045(17) 0.0089(16) 0.0003(16) C3 0.037(2) 0.035(2) 0.037(2) -0.0036(18) 0.0120(18) 0.0070(17) C4 0.030(2) 0.040(2) 0.039(2) 0.0003(19) 0.0102(17) 0.0091(17) C5 0.0281(18) 0.034(2) 0.027(2) 0.0010(17) 0.0079(16) 0.0000(15) C6 0.0238(19) 0.038(2) 0.029(2) 0.0009(18) 0.0042(16) -0.0002(16) C7 0.039(2) 0.045(3) 0.026(2) 0.0024(18) 0.0041(17) 0.0025(18) C8 0.048(3) 0.049(3) 0.042(3) 0.007(2) 0.017(2) 0.002(2) C9 0.022(2) 0.054(3) 0.036(3) -0.0034(18) 0.0045(18) 0.0007(16) C10 0.036(2) 0.083(4) 0.044(3) -0.006(3) 0.016(2) -0.015(2) C11 0.0237(18) 0.036(2) 0.028(2) 0.0027(17) 0.0049(15) -0.0021(15) C12 0.027(2) 0.041(2) 0.039(2) -0.0040(19) 0.0004(17) -0.0063(17) C13 0.036(2) 0.031(2) 0.043(2) -0.0081(19) 0.0065(18) -0.0077(17) C14 0.0295(19) 0.029(2) 0.029(2) -0.0002(16) 0.0069(16) -0.0022(15) C15 0.0307(19) 0.026(2) 0.037(2) -0.0016(17) 0.0120(17) -0.0021(15) C16 0.0269(18) 0.0217(18) 0.035(2) 0.0050(16) 0.0047(16) -0.0020(14) C17 0.036(2) 0.033(2) 0.037(2) 0.0026(18) 0.0085(18) -0.0040(17) C18 0.039(2) 0.050(3) 0.035(2) 0.009(2) 0.0033(19) -0.003(2) C19 0.035(2) 0.054(3) 0.042(3) 0.018(2) -0.0026(19) -0.001(2) C20 0.033(2) 0.037(2) 0.048(3) 0.011(2) 0.0104(19) 0.0027(17) C21 0.0283(19) 0.026(2) 0.039(2) 0.0039(17) 0.0076(16) -0.0025(15) C22 0.033(2) 0.029(2) 0.047(2) 0.0031(19) 0.0174(18) 0.0039(16) C23 0.040(2) 0.029(2) 0.044(2) -0.0080(18) 0.0186(19) -0.0002(17) C24 0.041(2) 0.031(2) 0.028(2) -0.0020(17) 0.0105(17) 0.0063(17) C25 0.045(2) 0.027(2) 0.035(2) 0.0006(19) 0.0123(19) 0.0036(18) C26 0.036(2) 0.047(3) 0.037(2) -0.004(2) 0.0103(18) -0.0056(19) C27 0.052(3) 0.033(2) 0.043(3) 0.0033(19) 0.023(2) 0.0050(18) C28 0.063(3) 0.042(3) 0.040(3) 0.009(2) 0.022(2) 0.016(2) C29 0.092(4) 0.072(4) 0.051(3) 0.020(3) 0.036(3) 0.020(3) C30 0.070(4) 0.049(3) 0.027(3) -0.0004(19) 0.013(2) 0.018(2) C31 0.044(2) 0.043(3) 0.035(2) -0.007(2) 0.0096(19) 0.007(2) C32 0.045(3) 0.071(4) 0.042(3) -0.007(3) 0.006(2) 0.004(2) C33 0.034(2) 0.035(2) 0.032(2) -0.0033(18) 0.0090(17) 0.0050(18) C34 0.031(2) 0.028(2) 0.035(2) -0.0030(16) 0.0133(18) 0.0016(14) C35 0.036(2) 0.0218(19) 0.031(2) -0.0009(16) 0.0090(16) -0.0028(15) C36 0.0258(19) 0.033(2) 0.036(2) -0.0070(18) 0.0052(16) -0.0047(16) C37 0.029(2) 0.045(3) 0.038(2) -0.006(2) 0.0017(17) -0.0031(17) C38 0.038(2) 0.042(2) 0.027(2) -0.0090(18) 0.0034(17) -0.0066(18) C39 0.032(2) 0.035(2) 0.034(2) -0.0024(18) 0.0081(17) -0.0018(17) C40 0.0280(18) 0.0257(19) 0.0249(19) -0.0028(16) 0.0035(15) -0.0063(15) N1 0.0296(16) 0.0293(17) 0.0248(17) -0.0017(13) 0.0064(13) -0.0014(13) N2 0.0275(16) 0.0332(18) 0.0244(17) -0.0010(14) 0.0061(13) -0.0003(13) N3 0.0278(16) 0.0294(17) 0.0289(17) -0.0011(14) 0.0078(13) -0.0020(13) N4 0.0265(15) 0.0278(17) 0.0278(17) 0.0001(14) 0.0062(13) -0.0009(12) N5 0.0410(18) 0.0268(17) 0.0315(18) -0.0026(14) 0.0133(15) 0.0012(14) O1 0.0298(14) 0.0352(16) 0.0406(17) -0.0013(13) 0.0130(12) 0.0008(11) O2 0.0325(14) 0.0307(15) 0.0270(14) -0.0048(11) 0.0085(11) 0.0021(11) Pd1 0.0225(2) 0.0252(2) 0.0246(2) -0.00196(10) 0.00349(15) -0.00011(10) C1S 0.131(6) 0.156(6) 0.112(6) 0.046(5) 0.048(5) 0.085(5) C2S 0.100(4) 0.108(4) 0.077(4) 0.058(3) 0.079(4) 0.041(3) C3S 0.039(2) 0.095(3) 0.024(2) 0.015(2) 0.0158(19) -0.026(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.322(5) . ? C1 C2 1.415(5) . ? C1 H1 0.9500 . ? C2 N2 1.384(5) . ? C2 C3 1.397(5) . ? C3 C4 1.396(6) . ? C3 H3 0.9500 . ? C4 C5 1.409(5) . ? C4 H4 0.9500 . ? C5 N2 1.350(5) . ? C5 C6 1.526(6) . ? C6 C11 1.510(6) . ? C6 C7 1.558(6) . ? C6 C9 1.564(6) . ? C7 C8 1.519(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.512(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N3 1.351(5) . ? C11 C12 1.402(6) . ? C12 C13 1.392(6) . ? C12 H12 0.9500 . ? C13 C14 1.401(5) . ? C13 H13 0.9500 . ? C14 N3 1.380(5) . ? C14 C15 1.419(5) . ? C15 N4 1.316(5) . ? C15 H15 0.9500 . ? C16 C17 1.380(6) . ? C16 C21 1.403(5) . ? C16 N4 1.430(5) . ? C17 C18 1.401(6) . ? C17 H17 0.9500 . ? C18 C19 1.378(7) . ? C18 H18 0.9500 . ? C19 C20 1.378(7) . ? C19 H19 0.9500 . ? C20 C21 1.407(6) . ? C20 H20 0.9500 . ? C21 O1 1.370(5) . ? C22 O1 1.440(4) . ? C22 C23 1.504(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 N5 1.467(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.394(6) . ? C24 C31 1.415(6) . ? C24 N5 1.432(5) . ? C25 C27 1.409(7) . ? C25 C26 1.501(6) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.388(7) . ? C27 H27 0.9500 . ? C28 C30 1.397(8) . ? C28 C29 1.515(7) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.378(7) . ? C30 H30 0.9500 . ? C31 C32 1.514(6) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 N5 1.469(5) . ? C33 C34 1.521(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 O2 1.427(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 O2 1.368(5) . ? C35 C36 1.389(5) . ? C35 C40 1.407(5) . ? C36 C37 1.394(6) . ? C36 H36 0.9500 . ? C37 C38 1.367(6) . ? C37 H37 0.9500 . ? C38 C39 1.399(6) . ? C38 H38 0.9500 . ? C39 C40 1.379(6) . ? C39 H39 0.9500 . ? C40 N1 1.423(5) . ? N1 Pd1 2.082(3) . ? N2 Pd1 1.934(3) . ? N3 Pd1 1.940(3) . ? N4 Pd1 2.092(3) . ? C1S C2S 1.323(10) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C2S C3S 1.567(8) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C3S C3S 1.637(8) 3_556 ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 117.4(4) . . ? N1 C1 H1 121.3 . . ? C2 C1 H1 121.3 . . ? N2 C2 C3 107.8(3) . . ? N2 C2 C1 113.8(3) . . ? C3 C2 C1 138.3(4) . . ? C4 C3 C2 106.9(4) . . ? C4 C3 H3 126.5 . . ? C2 C3 H3 126.5 . . ? C3 C4 C5 107.9(3) . . ? C3 C4 H4 126.1 . . ? C5 C4 H4 126.1 . . ? N2 C5 C4 107.7(3) . . ? N2 C5 C6 123.7(3) . . ? C4 C5 C6 128.5(3) . . ? C11 C6 C5 115.3(3) . . ? C11 C6 C7 108.2(3) . . ? C5 C6 C7 108.2(3) . . ? C11 C6 C9 109.1(3) . . ? C5 C6 C9 108.4(3) . . ? C7 C6 C9 107.4(3) . . ? C8 C7 C6 113.5(3) . . ? C8 C7 H7A 108.9 . . ? C6 C7 H7A 108.9 . . ? C8 C7 H7B 108.9 . . ? C6 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C6 113.7(4) . . ? C10 C9 H9A 108.8 . . ? C6 C9 H9A 108.8 . . ? C10 C9 H9B 108.8 . . ? C6 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 C12 107.2(3) . . ? N3 C11 C6 124.0(4) . . ? C12 C11 C6 128.6(3) . . ? C13 C12 C11 108.8(3) . . ? C13 C12 H12 125.6 . . ? C11 C12 H12 125.6 . . ? C12 C13 C14 106.2(4) . . ? C12 C13 H13 126.9 . . ? C14 C13 H13 126.9 . . ? N3 C14 C13 108.1(3) . . ? N3 C14 C15 113.4(3) . . ? C13 C14 C15 138.2(4) . . ? N4 C15 C14 118.6(4) . . ? N4 C15 H15 120.7 . . ? C14 C15 H15 120.7 . . ? C17 C16 C21 119.2(4) . . ? C17 C16 N4 118.9(4) . . ? C21 C16 N4 121.9(4) . . ? C16 C17 C18 121.5(4) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C19 C18 C17 118.9(4) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C20 C19 C18 121.0(4) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C19 C20 C21 120.3(4) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? O1 C21 C16 116.5(3) . . ? O1 C21 C20 124.4(4) . . ? C16 C21 C20 119.1(4) . . ? O1 C22 C23 107.6(3) . . ? O1 C22 H22A 110.2 . . ? C23 C22 H22A 110.2 . . ? O1 C22 H22B 110.2 . . ? C23 C22 H22B 110.2 . . ? H22A C22 H22B 108.5 . . ? N5 C23 C22 114.1(3) . . ? N5 C23 H23A 108.7 . . ? C22 C23 H23A 108.7 . . ? N5 C23 H23B 108.7 . . ? C22 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? C25 C24 C31 120.7(4) . . ? C25 C24 N5 116.5(4) . . ? C31 C24 N5 122.7(4) . . ? C24 C25 C27 117.8(4) . . ? C24 C25 C26 120.9(4) . . ? C27 C25 C26 121.4(4) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C25 122.1(5) . . ? C28 C27 H27 118.9 . . ? C25 C27 H27 118.9 . . ? C27 C28 C30 118.8(4) . . ? C27 C28 C29 120.8(5) . . ? C30 C28 C29 120.4(5) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C28 120.9(5) . . ? C31 C30 H30 119.5 . . ? C28 C30 H30 119.5 . . ? C30 C31 C24 119.7(5) . . ? C30 C31 C32 118.2(4) . . ? C24 C31 C32 122.1(4) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N5 C33 C34 109.3(3) . . ? N5 C33 H33A 109.8 . . ? C34 C33 H33A 109.8 . . ? N5 C33 H33B 109.8 . . ? C34 C33 H33B 109.8 . . ? H33A C33 H33B 108.3 . . ? O2 C34 C33 107.0(3) . . ? O2 C34 H34A 110.3 . . ? C33 C34 H34A 110.3 . . ? O2 C34 H34B 110.3 . . ? C33 C34 H34B 110.3 . . ? H34A C34 H34B 108.6 . . ? O2 C35 C36 124.7(4) . . ? O2 C35 C40 115.8(3) . . ? C36 C35 C40 119.5(4) . . ? C35 C36 C37 119.8(4) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? C38 C37 C36 121.0(4) . . ? C38 C37 H37 119.5 . . ? C36 C37 H37 119.5 . . ? C37 C38 C39 119.3(4) . . ? C37 C38 H38 120.3 . . ? C39 C38 H38 120.3 . . ? C40 C39 C38 120.9(4) . . ? C40 C39 H39 119.6 . . ? C38 C39 H39 119.6 . . ? C39 C40 C35 119.5(3) . . ? C39 C40 N1 122.7(3) . . ? C35 C40 N1 117.8(3) . . ? C1 N1 C40 119.2(3) . . ? C1 N1 Pd1 111.7(3) . . ? C40 N1 Pd1 129.0(2) . . ? C5 N2 C2 109.6(3) . . ? C5 N2 Pd1 133.1(3) . . ? C2 N2 Pd1 116.0(2) . . ? C11 N3 C14 109.8(3) . . ? C11 N3 Pd1 133.7(3) . . ? C14 N3 Pd1 116.5(2) . . ? C15 N4 C16 119.3(3) . . ? C15 N4 Pd1 111.1(2) . . ? C16 N4 Pd1 129.2(3) . . ? C24 N5 C23 115.1(3) . . ? C24 N5 C33 116.2(3) . . ? C23 N5 C33 118.0(3) . . ? C21 O1 C22 118.5(3) . . ? C35 O2 C34 117.8(3) . . ? N2 Pd1 N3 87.79(14) . . ? N2 Pd1 N1 80.09(13) . . ? N3 Pd1 N1 167.88(12) . . ? N2 Pd1 N4 167.20(13) . . ? N3 Pd1 N4 80.20(13) . . ? N1 Pd1 N4 111.88(12) . . ? C2S C1S H1S1 109.5 . . ? C2S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? C2S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C1S C2S C3S 128.5(7) . . ? C1S C2S H2S1 105.2 . . ? C3S C2S H2S1 105.2 . . ? C1S C2S H2S2 105.2 . . ? C3S C2S H2S2 105.2 . . ? H2S1 C2S H2S2 105.9 . . ? C2S C3S C3S 104.6(6) . 3_556 ? C2S C3S H3S1 110.8 . . ? C3S C3S H3S1 110.8 3_556 . ? C2S C3S H3S2 110.8 . . ? C3S C3S H3S2 110.8 3_556 . ? H3S1 C3S H3S2 108.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 -2.8(5) . . . . ? N1 C1 C2 C3 174.5(5) . . . . ? N2 C2 C3 C4 -0.5(5) . . . . ? C1 C2 C3 C4 -177.8(5) . . . . ? C2 C3 C4 C5 1.0(5) . . . . ? C3 C4 C5 N2 -1.2(5) . . . . ? C3 C4 C5 C6 -177.3(4) . . . . ? N2 C5 C6 C11 19.0(6) . . . . ? C4 C5 C6 C11 -165.5(4) . . . . ? N2 C5 C6 C7 -102.2(4) . . . . ? C4 C5 C6 C7 73.3(5) . . . . ? N2 C5 C6 C9 141.5(4) . . . . ? C4 C5 C6 C9 -42.9(6) . . . . ? C11 C6 C7 C8 -58.6(5) . . . . ? C5 C6 C7 C8 66.9(5) . . . . ? C9 C6 C7 C8 -176.3(4) . . . . ? C11 C6 C9 C10 65.5(5) . . . . ? C5 C6 C9 C10 -60.8(5) . . . . ? C7 C6 C9 C10 -177.5(4) . . . . ? C5 C6 C11 N3 -13.3(6) . . . . ? C7 C6 C11 N3 107.9(4) . . . . ? C9 C6 C11 N3 -135.5(4) . . . . ? C5 C6 C11 C12 172.3(4) . . . . ? C7 C6 C11 C12 -66.5(5) . . . . ? C9 C6 C11 C12 50.1(6) . . . . ? N3 C11 C12 C13 0.8(5) . . . . ? C6 C11 C12 C13 176.0(4) . . . . ? C11 C12 C13 C14 -0.9(5) . . . . ? C12 C13 C14 N3 0.6(5) . . . . ? C12 C13 C14 C15 173.9(5) . . . . ? N3 C14 C15 N4 -2.5(5) . . . . ? C13 C14 C15 N4 -175.6(5) . . . . ? C21 C16 C17 C18 -2.0(6) . . . . ? N4 C16 C17 C18 179.3(4) . . . . ? C16 C17 C18 C19 0.3(7) . . . . ? C17 C18 C19 C20 0.9(7) . . . . ? C18 C19 C20 C21 -0.3(7) . . . . ? C17 C16 C21 O1 -176.5(3) . . . . ? N4 C16 C21 O1 2.2(5) . . . . ? C17 C16 C21 C20 2.5(6) . . . . ? N4 C16 C21 C20 -178.8(3) . . . . ? C19 C20 C21 O1 177.5(4) . . . . ? C19 C20 C21 C16 -1.4(6) . . . . ? O1 C22 C23 N5 81.2(4) . . . . ? C31 C24 C25 C27 1.3(6) . . . . ? N5 C24 C25 C27 -179.5(4) . . . . ? C31 C24 C25 C26 -177.9(4) . . . . ? N5 C24 C25 C26 1.3(6) . . . . ? C24 C25 C27 C28 0.8(7) . . . . ? C26 C25 C27 C28 -180.0(4) . . . . ? C25 C27 C28 C30 -1.5(7) . . . . ? C25 C27 C28 C29 179.0(5) . . . . ? C27 C28 C30 C31 0.1(7) . . . . ? C29 C28 C30 C31 179.6(5) . . . . ? C28 C30 C31 C24 2.0(7) . . . . ? C28 C30 C31 C32 -177.2(4) . . . . ? C25 C24 C31 C30 -2.7(7) . . . . ? N5 C24 C31 C30 178.1(4) . . . . ? C25 C24 C31 C32 176.5(4) . . . . ? N5 C24 C31 C32 -2.7(7) . . . . ? N5 C33 C34 O2 -173.9(3) . . . . ? O2 C35 C36 C37 -178.9(4) . . . . ? C40 C35 C36 C37 2.2(6) . . . . ? C35 C36 C37 C38 -1.1(7) . . . . ? C36 C37 C38 C39 -0.6(7) . . . . ? C37 C38 C39 C40 1.1(7) . . . . ? C38 C39 C40 C35 0.1(6) . . . . ? C38 C39 C40 N1 177.3(4) . . . . ? O2 C35 C40 C39 179.3(3) . . . . ? C36 C35 C40 C39 -1.7(6) . . . . ? O2 C35 C40 N1 2.0(5) . . . . ? C36 C35 C40 N1 -179.1(3) . . . . ? C2 C1 N1 C40 178.9(3) . . . . ? C2 C1 N1 Pd1 -4.1(4) . . . . ? C39 C40 N1 C1 48.8(5) . . . . ? C35 C40 N1 C1 -133.9(4) . . . . ? C39 C40 N1 Pd1 -127.6(4) . . . . ? C35 C40 N1 Pd1 49.7(5) . . . . ? C4 C5 N2 C2 0.9(4) . . . . ? C6 C5 N2 C2 177.2(4) . . . . ? C4 C5 N2 Pd1 167.2(3) . . . . ? C6 C5 N2 Pd1 -16.5(6) . . . . ? C3 C2 N2 C5 -0.3(5) . . . . ? C1 C2 N2 C5 177.8(3) . . . . ? C3 C2 N2 Pd1 -169.1(3) . . . . ? C1 C2 N2 Pd1 8.9(4) . . . . ? C12 C11 N3 C14 -0.5(4) . . . . ? C6 C11 N3 C14 -175.9(3) . . . . ? C12 C11 N3 Pd1 179.8(3) . . . . ? C6 C11 N3 Pd1 4.4(6) . . . . ? C13 C14 N3 C11 -0.1(5) . . . . ? C15 C14 N3 C11 -175.2(3) . . . . ? C13 C14 N3 Pd1 179.7(3) . . . . ? C15 C14 N3 Pd1 4.5(4) . . . . ? C14 C15 N4 C16 173.1(3) . . . . ? C14 C15 N4 Pd1 -0.5(4) . . . . ? C17 C16 N4 C15 -128.7(4) . . . . ? C21 C16 N4 C15 52.6(5) . . . . ? C17 C16 N4 Pd1 43.5(5) . . . . ? C21 C16 N4 Pd1 -135.2(3) . . . . ? C25 C24 N5 C23 -96.4(4) . . . . ? C31 C24 N5 C23 82.8(5) . . . . ? C25 C24 N5 C33 119.6(4) . . . . ? C31 C24 N5 C33 -61.2(5) . . . . ? C22 C23 N5 C24 154.2(3) . . . . ? C22 C23 N5 C33 -62.5(5) . . . . ? C34 C33 N5 C24 -115.0(4) . . . . ? C34 C33 N5 C23 102.1(4) . . . . ? C16 C21 O1 C22 152.9(3) . . . . ? C20 C21 O1 C22 -26.0(5) . . . . ? C23 C22 O1 C21 -144.9(3) . . . . ? C36 C35 O2 C34 11.2(5) . . . . ? C40 C35 O2 C34 -169.9(3) . . . . ? C33 C34 O2 C35 167.5(3) . . . . ? C5 N2 Pd1 N3 5.7(4) . . . . ? C2 N2 Pd1 N3 171.3(3) . . . . ? C5 N2 Pd1 N1 -174.2(4) . . . . ? C2 N2 Pd1 N1 -8.6(3) . . . . ? C5 N2 Pd1 N4 -14.4(8) . . . . ? C2 N2 Pd1 N4 151.2(5) . . . . ? C11 N3 Pd1 N2 0.4(4) . . . . ? C14 N3 Pd1 N2 -179.3(3) . . . . ? C11 N3 Pd1 N1 0.8(8) . . . . ? C11 N3 Pd1 N4 176.0(4) . . . . ? C14 N3 Pd1 N4 -3.7(3) . . . . ? C1 N1 Pd1 N2 6.9(3) . . . . ? C40 N1 Pd1 N2 -176.6(3) . . . . ? C1 N1 Pd1 N3 6.4(7) . . . . ? C40 N1 Pd1 N3 -177.0(5) . . . . ? C1 N1 Pd1 N4 -168.4(3) . . . . ? C40 N1 Pd1 N4 8.2(4) . . . . ? C15 N4 Pd1 N2 22.8(7) . . . . ? C16 N4 Pd1 N2 -150.0(5) . . . . ? C15 N4 Pd1 N3 2.3(3) . . . . ? C16 N4 Pd1 N3 -170.5(3) . . . . ? C15 N4 Pd1 N1 -178.8(3) . . . . ? C16 N4 Pd1 N1 8.4(3) . . . . ? C1S C2S C3S C3S -174.9(7) . . . 3_556 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.073 _refine_diff_density_min -0.882 _refine_diff_density_rms 0.092 data_j10095_Pd(LfNMe) _database_code_depnum_ccdc_archive 'CCDC 895818' #TrackingRef 'combined_CIF.cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H33 N5 O2 Pd' _chemical_formula_sum 'C40 H33 N5 O2 Pd' _chemical_formula_weight 722.11 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.6736(3) _cell_length_b 14.6814(4) _cell_length_c 25.5451(8) _cell_angle_alpha 90.00 _cell_angle_beta 97.840(3) _cell_angle_gamma 90.00 _cell_volume 3222.52(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11216 _cell_measurement_theta_min 2.8834 _cell_measurement_theta_max 29.1335 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 0.621 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.74721 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1042 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 29081 _diffrn_reflns_av_R_equivalents 0.0567 _diffrn_reflns_av_sigmaI/netI 0.0580 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7284 _reflns_number_gt 6001 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+0.2599P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7284 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1023 _refine_ls_wR_factor_gt 0.0948 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5787(3) 0.22582(18) 0.82447(11) 0.0234(6) Uani 1 1 d . . . H1 H 0.5228 0.2722 0.8041 0.028 Uiso 1 1 calc R . . C2 C 0.6426(3) 0.15152(19) 0.79991(10) 0.0216(6) Uani 1 1 d . . . C3 C 0.6400(3) 0.11472(19) 0.74906(11) 0.0246(6) Uani 1 1 d . . . H3 H 0.5943 0.1416 0.7168 0.030 Uiso 1 1 calc R . . C4 C 0.7170(3) 0.0316(2) 0.75477(11) 0.0262(6) Uani 1 1 d . . . H4 H 0.7330 -0.0089 0.7270 0.031 Uiso 1 1 calc R . . C5 C 0.7667(3) 0.01806(18) 0.80887(10) 0.0216(6) Uani 1 1 d . . . C6 C 0.8701(3) -0.05538(18) 0.83710(10) 0.0218(6) Uani 1 1 d . . . C7 C 1.0412(3) -0.02733(19) 0.83515(10) 0.0226(6) Uani 1 1 d . . . C8 C 1.1191(3) 0.0478(2) 0.85742(11) 0.0309(7) Uani 1 1 d . . . H8 H 1.0686 0.0909 0.8770 0.037 Uiso 1 1 calc R . . C9 C 1.2751(4) 0.0586(2) 0.85021(13) 0.0422(9) Uani 1 1 d . . . H9 H 1.3321 0.1093 0.8658 0.051 Uiso 1 1 calc R . . C10 C 1.3474(4) -0.0028(3) 0.82095(14) 0.0470(10) Uani 1 1 d . . . H10 H 1.4530 0.0067 0.8162 0.056 Uiso 1 1 calc R . . C11 C 1.2695(3) -0.0774(3) 0.79860(13) 0.0414(8) Uani 1 1 d . . . H11 H 1.3199 -0.1192 0.7782 0.050 Uiso 1 1 calc R . . C12 C 1.1143(3) -0.0911(2) 0.80630(11) 0.0288(7) Uani 1 1 d . . . C13 C 1.0061(3) -0.1650(2) 0.78980(11) 0.0292(7) Uani 1 1 d . . . C14 C 1.0263(4) -0.2461(2) 0.76414(13) 0.0435(9) Uani 1 1 d . . . H14 H 1.1233 -0.2598 0.7526 0.052 Uiso 1 1 calc R . . C15 C 0.9046(4) -0.3067(2) 0.75543(13) 0.0454(9) Uani 1 1 d . . . H15 H 0.9188 -0.3632 0.7385 0.054 Uiso 1 1 calc R . . C16 C 0.7633(4) -0.2866(2) 0.77086(13) 0.0417(8) Uani 1 1 d . . . H16 H 0.6801 -0.3289 0.7640 0.050 Uiso 1 1 calc R . . C17 C 0.7398(3) -0.2052(2) 0.79645(11) 0.0309(7) Uani 1 1 d . . . H17 H 0.6413 -0.1912 0.8068 0.037 Uiso 1 1 calc R . . C18 C 0.8630(3) -0.1452(2) 0.80646(11) 0.0246(6) Uani 1 1 d . . . C19 C 0.8460(3) -0.07162(19) 0.89402(11) 0.0236(6) Uani 1 1 d . . . C20 C 0.8793(3) -0.1487(2) 0.92635(11) 0.0281(6) Uani 1 1 d . . . H20 H 0.9114 -0.2066 0.9152 0.034 Uiso 1 1 calc R . . C21 C 0.8572(4) -0.1252(2) 0.97726(12) 0.0323(7) Uani 1 1 d . . . H21 H 0.8705 -0.1637 1.0074 0.039 Uiso 1 1 calc R . . C22 C 0.8114(3) -0.03355(19) 0.97560(11) 0.0269(6) Uani 1 1 d . . . C23 C 0.7748(3) 0.0348(2) 1.01067(11) 0.0291(7) Uani 1 1 d . . . H23 H 0.7809 0.0228 1.0474 0.035 Uiso 1 1 calc R . . C24 C 0.7111(4) 0.1862(2) 1.02831(10) 0.0292(7) Uani 1 1 d . . . C25 C 0.6199(4) 0.1717(2) 1.06810(12) 0.0413(8) Uani 1 1 d . . . H25 H 0.5641 0.1162 1.0695 0.050 Uiso 1 1 calc R . . C26 C 0.6105(5) 0.2390(2) 1.10592(13) 0.0534(10) Uani 1 1 d . . . H26 H 0.5478 0.2296 1.1331 0.064 Uiso 1 1 calc R . . C27 C 0.6917(5) 0.3187(2) 1.10399(13) 0.0494(10) Uani 1 1 d . . . H27 H 0.6876 0.3632 1.1308 0.059 Uiso 1 1 calc R . . C28 C 0.7794(4) 0.3356(2) 1.06377(12) 0.0365(8) Uani 1 1 d . . . H28 H 0.8345 0.3913 1.0627 0.044 Uiso 1 1 calc R . . C29 C 0.7864(3) 0.2702(2) 1.02483(11) 0.0278(7) Uani 1 1 d . . . C30 C 0.9063(4) 0.37304(19) 0.97111(12) 0.0333(7) Uani 1 1 d . . . H30A H 0.9954 0.3948 0.9964 0.040 Uiso 1 1 calc R . . H30B H 0.8164 0.4136 0.9735 0.040 Uiso 1 1 calc R . . C31 C 0.9480(4) 0.3737(2) 0.91534(12) 0.0343(7) Uani 1 1 d . . . H31A H 1.0462 0.3398 0.9145 0.041 Uiso 1 1 calc R . . H31B H 0.8651 0.3426 0.8914 0.041 Uiso 1 1 calc R . . C32 C 1.0417(4) 0.4673(3) 0.84931(13) 0.0519(10) Uani 1 1 d . . . H32A H 0.9774 0.4336 0.8213 0.078 Uiso 1 1 calc R . . H32B H 1.1439 0.4382 0.8569 0.078 Uiso 1 1 calc R . . H32C H 1.0545 0.5302 0.8378 0.078 Uiso 1 1 calc R . . C33 C 0.8237(4) 0.5233(2) 0.89038(13) 0.0409(8) Uani 1 1 d . . . H33A H 0.8551 0.5873 0.8857 0.049 Uiso 1 1 calc R . . H33B H 0.7789 0.5204 0.9240 0.049 Uiso 1 1 calc R . . C34 C 0.6952(4) 0.5009(2) 0.84617(13) 0.0400(8) Uani 1 1 d . . . H34A H 0.6117 0.5469 0.8460 0.048 Uiso 1 1 calc R . . H34B H 0.7370 0.5057 0.8121 0.048 Uiso 1 1 calc R . . C35 C 0.5438(3) 0.39231(19) 0.89021(12) 0.0285(7) Uani 1 1 d . . . C36 C 0.4734(4) 0.4573(2) 0.91875(14) 0.0415(8) Uani 1 1 d . . . H36 H 0.4842 0.5202 0.9111 0.050 Uiso 1 1 calc R . . C37 C 0.3876(4) 0.4312(2) 0.95810(14) 0.0443(9) Uani 1 1 d . . . H37 H 0.3384 0.4763 0.9767 0.053 Uiso 1 1 calc R . . C38 C 0.3726(4) 0.3412(2) 0.97055(13) 0.0396(8) Uani 1 1 d . . . H38 H 0.3143 0.3238 0.9978 0.048 Uiso 1 1 calc R . . C39 C 0.4435(3) 0.2760(2) 0.94294(11) 0.0316(7) Uani 1 1 d . . . H39 H 0.4346 0.2135 0.9518 0.038 Uiso 1 1 calc R . . C40 C 0.5273(3) 0.30024(19) 0.90258(11) 0.0253(6) Uani 1 1 d . . . N1 N 0.5986(3) 0.22915(15) 0.87610(9) 0.0234(5) Uani 1 1 d . . . N2 N 0.7225(3) 0.09082(15) 0.83509(8) 0.0215(5) Uani 1 1 d . . . N3 N 0.8076(3) -0.00327(15) 0.92468(9) 0.0240(5) Uani 1 1 d . . . N4 N 0.7321(3) 0.11536(16) 0.99139(9) 0.0280(6) Uani 1 1 d . . . N5 N 0.9663(3) 0.46725(18) 0.89673(10) 0.0364(6) Uani 1 1 d . . . O1 O 0.8680(2) 0.28130(13) 0.98329(7) 0.0305(5) Uani 1 1 d . . . O2 O 0.6280(2) 0.41104(14) 0.84988(8) 0.0349(5) Uani 1 1 d . . . Pd1 Pd 0.71857(2) 0.116185(14) 0.909466(8) 0.02179(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0200(14) 0.0234(15) 0.0260(15) 0.0047(11) 0.0005(11) -0.0028(11) C2 0.0175(13) 0.0261(14) 0.0218(14) 0.0046(11) 0.0046(11) -0.0033(11) C3 0.0196(14) 0.0336(16) 0.0211(15) 0.0030(12) 0.0045(11) -0.0021(12) C4 0.0212(14) 0.0352(17) 0.0240(15) -0.0084(12) 0.0098(12) -0.0039(12) C5 0.0137(13) 0.0256(15) 0.0272(15) -0.0028(11) 0.0091(11) -0.0051(11) C6 0.0140(13) 0.0250(15) 0.0275(15) -0.0025(11) 0.0069(11) -0.0020(11) C7 0.0161(13) 0.0299(16) 0.0220(14) 0.0061(11) 0.0035(11) -0.0041(11) C8 0.0313(16) 0.0326(17) 0.0281(16) 0.0093(13) 0.0013(13) -0.0082(13) C9 0.0297(17) 0.052(2) 0.0413(19) 0.0219(16) -0.0097(15) -0.0251(16) C10 0.0159(15) 0.071(3) 0.054(2) 0.0267(19) 0.0066(15) -0.0041(16) C11 0.0181(15) 0.059(2) 0.049(2) 0.0151(18) 0.0115(14) 0.0063(16) C12 0.0155(14) 0.0424(18) 0.0289(16) 0.0073(13) 0.0048(12) 0.0039(13) C13 0.0218(15) 0.0383(18) 0.0281(16) -0.0051(13) 0.0055(12) 0.0055(13) C14 0.0340(18) 0.051(2) 0.047(2) -0.0116(16) 0.0083(16) 0.0194(16) C15 0.051(2) 0.039(2) 0.043(2) -0.0171(16) -0.0036(17) 0.0115(17) C16 0.040(2) 0.0351(19) 0.046(2) -0.0070(15) -0.0084(16) -0.0026(15) C17 0.0234(15) 0.0300(17) 0.0387(17) -0.0063(13) 0.0021(13) 0.0002(13) C18 0.0187(14) 0.0275(15) 0.0276(15) -0.0018(12) 0.0037(12) 0.0029(12) C19 0.0186(13) 0.0234(15) 0.0299(15) -0.0024(12) 0.0071(11) -0.0011(11) C20 0.0301(16) 0.0205(14) 0.0350(17) 0.0002(12) 0.0086(13) 0.0043(12) C21 0.0372(18) 0.0267(17) 0.0344(18) 0.0088(13) 0.0100(14) 0.0039(13) C22 0.0307(16) 0.0259(16) 0.0257(15) 0.0035(12) 0.0100(12) 0.0021(12) C23 0.0341(17) 0.0315(17) 0.0233(15) 0.0030(12) 0.0091(12) 0.0027(13) C24 0.0356(17) 0.0327(17) 0.0195(14) 0.0017(12) 0.0048(12) 0.0087(13) C25 0.058(2) 0.0348(19) 0.0352(18) 0.0062(14) 0.0210(16) 0.0092(16) C26 0.086(3) 0.043(2) 0.039(2) 0.0045(16) 0.038(2) 0.013(2) C27 0.084(3) 0.039(2) 0.0289(18) -0.0021(15) 0.0201(18) 0.0198(19) C28 0.050(2) 0.0286(18) 0.0312(17) 0.0001(13) 0.0063(15) 0.0108(15) C29 0.0304(16) 0.0313(17) 0.0218(15) 0.0023(12) 0.0041(12) 0.0114(13) C30 0.0404(19) 0.0280(17) 0.0318(18) 0.0006(13) 0.0064(14) 0.0023(13) C31 0.0316(17) 0.0373(19) 0.0345(18) 0.0025(13) 0.0061(14) 0.0035(14) C32 0.053(2) 0.065(3) 0.040(2) 0.0066(18) 0.0162(17) -0.008(2) C33 0.049(2) 0.0283(18) 0.045(2) 0.0059(15) 0.0065(16) -0.0032(15) C34 0.042(2) 0.0266(17) 0.049(2) 0.0101(14) 0.0010(16) -0.0014(14) C35 0.0257(16) 0.0272(16) 0.0311(17) 0.0000(12) -0.0011(13) 0.0039(12) C36 0.0375(19) 0.0287(18) 0.057(2) -0.0034(16) 0.0004(16) 0.0120(15) C37 0.0370(19) 0.046(2) 0.050(2) -0.0150(17) 0.0067(16) 0.0183(16) C38 0.0306(17) 0.052(2) 0.0381(19) -0.0079(16) 0.0099(14) 0.0075(16) C39 0.0282(16) 0.0356(18) 0.0312(17) -0.0041(13) 0.0055(13) 0.0041(13) C40 0.0221(14) 0.0263(15) 0.0256(15) -0.0026(12) -0.0031(12) 0.0053(12) N1 0.0217(12) 0.0235(13) 0.0251(13) 0.0004(10) 0.0034(10) 0.0016(10) N2 0.0195(11) 0.0245(12) 0.0211(12) -0.0005(9) 0.0053(9) 0.0012(10) N3 0.0272(13) 0.0236(13) 0.0226(12) 0.0033(9) 0.0083(10) 0.0031(10) N4 0.0344(14) 0.0278(14) 0.0230(13) 0.0000(10) 0.0085(11) 0.0060(11) N5 0.0342(15) 0.0393(16) 0.0371(15) 0.0052(12) 0.0104(12) -0.0046(12) O1 0.0366(12) 0.0278(12) 0.0292(11) 0.0018(9) 0.0117(9) 0.0046(9) O2 0.0378(12) 0.0256(11) 0.0408(13) 0.0017(9) 0.0036(10) -0.0004(9) Pd1 0.02459(13) 0.02172(13) 0.01997(13) 0.00074(8) 0.00626(9) 0.00338(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.307(3) . ? C1 C2 1.409(4) . ? C1 H1 0.9500 . ? C2 N2 1.383(3) . ? C2 C3 1.404(4) . ? C3 C4 1.389(4) . ? C3 H3 0.9500 . ? C4 C5 1.405(4) . ? C4 H4 0.9500 . ? C5 N2 1.344(3) . ? C5 C6 1.520(4) . ? C6 C19 1.516(4) . ? C6 C18 1.530(4) . ? C6 C7 1.548(3) . ? C7 C8 1.375(4) . ? C7 C12 1.396(4) . ? C8 C9 1.400(4) . ? C8 H8 0.9500 . ? C9 C10 1.376(5) . ? C9 H9 0.9500 . ? C10 C11 1.371(5) . ? C10 H10 0.9500 . ? C11 C12 1.401(4) . ? C11 H11 0.9500 . ? C12 C13 1.459(4) . ? C13 C14 1.381(4) . ? C13 C18 1.397(4) . ? C14 C15 1.376(5) . ? C14 H14 0.9500 . ? C15 C16 1.370(5) . ? C15 H15 0.9500 . ? C16 C17 1.391(4) . ? C16 H16 0.9500 . ? C17 C18 1.382(4) . ? C17 H17 0.9500 . ? C19 N3 1.342(3) . ? C19 C20 1.408(4) . ? C20 C21 1.384(4) . ? C20 H20 0.9500 . ? C21 C22 1.402(4) . ? C21 H21 0.9500 . ? C22 N3 1.371(3) . ? C22 C23 1.409(4) . ? C23 N4 1.315(4) . ? C23 H23 0.9500 . ? C24 C25 1.387(4) . ? C24 C29 1.404(4) . ? C24 N4 1.432(4) . ? C25 C26 1.392(4) . ? C25 H25 0.9500 . ? C26 C27 1.371(5) . ? C26 H26 0.9500 . ? C27 C28 1.382(5) . ? C27 H27 0.9500 . ? C28 C29 1.390(4) . ? C28 H28 0.9500 . ? C29 O1 1.363(3) . ? C30 O1 1.432(3) . ? C30 C31 1.517(4) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 N5 1.469(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 N5 1.453(4) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 N5 1.476(4) . ? C33 C34 1.511(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 O2 1.451(3) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 O2 1.369(4) . ? C35 C36 1.392(4) . ? C35 C40 1.400(4) . ? C36 C37 1.384(5) . ? C36 H36 0.9500 . ? C37 C38 1.369(5) . ? C37 H37 0.9500 . ? C38 C39 1.382(4) . ? C38 H38 0.9500 . ? C39 C40 1.387(4) . ? C39 H39 0.9500 . ? C40 N1 1.430(3) . ? N1 Pd1 2.078(2) . ? N2 Pd1 1.941(2) . ? N3 Pd1 1.934(2) . ? N4 Pd1 2.080(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 118.2(2) . . ? N1 C1 H1 120.9 . . ? C2 C1 H1 120.9 . . ? N2 C2 C3 107.2(2) . . ? N2 C2 C1 113.7(2) . . ? C3 C2 C1 138.8(3) . . ? C4 C3 C2 107.1(2) . . ? C4 C3 H3 126.4 . . ? C2 C3 H3 126.4 . . ? C3 C4 C5 107.8(2) . . ? C3 C4 H4 126.1 . . ? C5 C4 H4 126.1 . . ? N2 C5 C4 107.9(2) . . ? N2 C5 C6 121.2(2) . . ? C4 C5 C6 130.5(2) . . ? C19 C6 C5 114.6(2) . . ? C19 C6 C18 110.7(2) . . ? C5 C6 C18 112.9(2) . . ? C19 C6 C7 109.3(2) . . ? C5 C6 C7 107.6(2) . . ? C18 C6 C7 100.7(2) . . ? C8 C7 C12 121.6(3) . . ? C8 C7 C6 128.2(3) . . ? C12 C7 C6 110.2(2) . . ? C7 C8 C9 117.7(3) . . ? C7 C8 H8 121.1 . . ? C9 C8 H8 121.1 . . ? C10 C9 C8 121.2(3) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C11 C10 C9 121.0(3) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C12 119.0(3) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? C7 C12 C11 119.5(3) . . ? C7 C12 C13 109.3(2) . . ? C11 C12 C13 131.2(3) . . ? C14 C13 C18 120.0(3) . . ? C14 C13 C12 131.3(3) . . ? C18 C13 C12 108.7(3) . . ? C15 C14 C13 119.4(3) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C16 C15 C14 120.7(3) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 121.0(3) . . ? C15 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? C18 C17 C16 118.4(3) . . ? C18 C17 H17 120.8 . . ? C16 C17 H17 120.8 . . ? C17 C18 C13 120.5(3) . . ? C17 C18 C6 128.4(3) . . ? C13 C18 C6 111.1(2) . . ? N3 C19 C20 107.8(2) . . ? N3 C19 C6 121.3(2) . . ? C20 C19 C6 130.2(2) . . ? C21 C20 C19 107.9(3) . . ? C21 C20 H20 126.1 . . ? C19 C20 H20 126.1 . . ? C20 C21 C22 106.6(3) . . ? C20 C21 H21 126.7 . . ? C22 C21 H21 126.7 . . ? N3 C22 C21 108.0(2) . . ? N3 C22 C23 113.2(3) . . ? C21 C22 C23 138.7(3) . . ? N4 C23 C22 118.6(3) . . ? N4 C23 H23 120.7 . . ? C22 C23 H23 120.7 . . ? C25 C24 C29 119.9(3) . . ? C25 C24 N4 120.5(3) . . ? C29 C24 N4 119.6(3) . . ? C24 C25 C26 119.5(3) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C27 C26 C25 120.2(3) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C28 121.1(3) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? C27 C28 C29 119.4(3) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? O1 C29 C28 123.5(3) . . ? O1 C29 C24 116.8(2) . . ? C28 C29 C24 119.7(3) . . ? O1 C30 C31 107.6(2) . . ? O1 C30 H30A 110.2 . . ? C31 C30 H30A 110.2 . . ? O1 C30 H30B 110.2 . . ? C31 C30 H30B 110.2 . . ? H30A C30 H30B 108.5 . . ? N5 C31 C30 111.1(2) . . ? N5 C31 H31A 109.4 . . ? C30 C31 H31A 109.4 . . ? N5 C31 H31B 109.4 . . ? C30 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? N5 C32 H32A 109.5 . . ? N5 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N5 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N5 C33 C34 118.9(3) . . ? N5 C33 H33A 107.6 . . ? C34 C33 H33A 107.6 . . ? N5 C33 H33B 107.6 . . ? C34 C33 H33B 107.6 . . ? H33A C33 H33B 107.0 . . ? O2 C34 C33 114.3(2) . . ? O2 C34 H34A 108.7 . . ? C33 C34 H34A 108.7 . . ? O2 C34 H34B 108.7 . . ? C33 C34 H34B 108.7 . . ? H34A C34 H34B 107.6 . . ? O2 C35 C36 125.0(3) . . ? O2 C35 C40 116.4(3) . . ? C36 C35 C40 118.6(3) . . ? C37 C36 C35 120.5(3) . . ? C37 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C38 C37 C36 120.9(3) . . ? C38 C37 H37 119.6 . . ? C36 C37 H37 119.6 . . ? C37 C38 C39 119.2(3) . . ? C37 C38 H38 120.4 . . ? C39 C38 H38 120.4 . . ? C38 C39 C40 121.1(3) . . ? C38 C39 H39 119.5 . . ? C40 C39 H39 119.5 . . ? C39 C40 C35 119.7(3) . . ? C39 C40 N1 118.0(3) . . ? C35 C40 N1 122.3(3) . . ? C1 N1 C40 119.9(2) . . ? C1 N1 Pd1 111.95(18) . . ? C40 N1 Pd1 127.83(18) . . ? C5 N2 C2 109.9(2) . . ? C5 N2 Pd1 133.19(19) . . ? C2 N2 Pd1 115.99(18) . . ? C19 N3 C22 109.6(2) . . ? C19 N3 Pd1 133.20(19) . . ? C22 N3 Pd1 116.21(18) . . ? C23 N4 C24 117.5(2) . . ? C23 N4 Pd1 110.86(18) . . ? C24 N4 Pd1 131.57(18) . . ? C32 N5 C31 110.6(3) . . ? C32 N5 C33 111.9(3) . . ? C31 N5 C33 115.5(3) . . ? C29 O1 C30 116.3(2) . . ? C35 O2 C34 119.5(2) . . ? N3 Pd1 N2 87.87(9) . . ? N3 Pd1 N1 165.92(9) . . ? N2 Pd1 N1 79.99(9) . . ? N3 Pd1 N4 80.01(9) . . ? N2 Pd1 N4 167.86(9) . . ? N1 Pd1 N4 111.95(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 -1.0(4) . . . . ? N1 C1 C2 C3 172.3(3) . . . . ? N2 C2 C3 C4 0.8(3) . . . . ? C1 C2 C3 C4 -172.7(3) . . . . ? C2 C3 C4 C5 -0.3(3) . . . . ? C3 C4 C5 N2 -0.4(3) . . . . ? C3 C4 C5 C6 -172.7(3) . . . . ? N2 C5 C6 C19 32.7(3) . . . . ? C4 C5 C6 C19 -155.9(3) . . . . ? N2 C5 C6 C18 160.7(2) . . . . ? C4 C5 C6 C18 -27.9(4) . . . . ? N2 C5 C6 C7 -89.2(3) . . . . ? C4 C5 C6 C7 82.2(3) . . . . ? C19 C6 C7 C8 -61.7(4) . . . . ? C5 C6 C7 C8 63.4(3) . . . . ? C18 C6 C7 C8 -178.3(3) . . . . ? C19 C6 C7 C12 118.2(2) . . . . ? C5 C6 C7 C12 -116.7(2) . . . . ? C18 C6 C7 C12 1.6(3) . . . . ? C12 C7 C8 C9 0.0(4) . . . . ? C6 C7 C8 C9 179.9(3) . . . . ? C7 C8 C9 C10 1.3(4) . . . . ? C8 C9 C10 C11 -1.1(5) . . . . ? C9 C10 C11 C12 -0.6(5) . . . . ? C8 C7 C12 C11 -1.6(4) . . . . ? C6 C7 C12 C11 178.5(3) . . . . ? C8 C7 C12 C13 177.3(3) . . . . ? C6 C7 C12 C13 -2.6(3) . . . . ? C10 C11 C12 C7 1.9(5) . . . . ? C10 C11 C12 C13 -176.8(3) . . . . ? C7 C12 C13 C14 -174.7(3) . . . . ? C11 C12 C13 C14 4.1(6) . . . . ? C7 C12 C13 C18 2.5(3) . . . . ? C11 C12 C13 C18 -178.7(3) . . . . ? C18 C13 C14 C15 -0.2(5) . . . . ? C12 C13 C14 C15 176.8(3) . . . . ? C13 C14 C15 C16 1.5(5) . . . . ? C14 C15 C16 C17 -1.1(5) . . . . ? C15 C16 C17 C18 -0.6(5) . . . . ? C16 C17 C18 C13 1.9(4) . . . . ? C16 C17 C18 C6 -175.3(3) . . . . ? C14 C13 C18 C17 -1.5(4) . . . . ? C12 C13 C18 C17 -179.1(3) . . . . ? C14 C13 C18 C6 176.1(3) . . . . ? C12 C13 C18 C6 -1.5(3) . . . . ? C19 C6 C18 C17 61.8(4) . . . . ? C5 C6 C18 C17 -68.2(4) . . . . ? C7 C6 C18 C17 177.4(3) . . . . ? C19 C6 C18 C13 -115.6(3) . . . . ? C5 C6 C18 C13 114.4(3) . . . . ? C7 C6 C18 C13 0.0(3) . . . . ? C5 C6 C19 N3 -33.6(3) . . . . ? C18 C6 C19 N3 -162.6(2) . . . . ? C7 C6 C19 N3 87.4(3) . . . . ? C5 C6 C19 C20 157.2(3) . . . . ? C18 C6 C19 C20 28.2(4) . . . . ? C7 C6 C19 C20 -81.9(3) . . . . ? N3 C19 C20 C21 1.1(3) . . . . ? C6 C19 C20 C21 171.4(3) . . . . ? C19 C20 C21 C22 -0.4(3) . . . . ? C20 C21 C22 N3 -0.4(3) . . . . ? C20 C21 C22 C23 -177.5(4) . . . . ? N3 C22 C23 N4 4.5(4) . . . . ? C21 C22 C23 N4 -178.5(3) . . . . ? C29 C24 C25 C26 -3.4(5) . . . . ? N4 C24 C25 C26 175.2(3) . . . . ? C24 C25 C26 C27 -0.4(5) . . . . ? C25 C26 C27 C28 2.3(6) . . . . ? C26 C27 C28 C29 -0.5(5) . . . . ? C27 C28 C29 O1 179.0(3) . . . . ? C27 C28 C29 C24 -3.3(4) . . . . ? C25 C24 C29 O1 -176.9(3) . . . . ? N4 C24 C29 O1 4.5(4) . . . . ? C25 C24 C29 C28 5.2(4) . . . . ? N4 C24 C29 C28 -173.3(3) . . . . ? O1 C30 C31 N5 171.6(2) . . . . ? N5 C33 C34 O2 62.0(4) . . . . ? O2 C35 C36 C37 178.5(3) . . . . ? C40 C35 C36 C37 -0.6(5) . . . . ? C35 C36 C37 C38 1.3(5) . . . . ? C36 C37 C38 C39 -0.6(5) . . . . ? C37 C38 C39 C40 -0.8(5) . . . . ? C38 C39 C40 C35 1.5(4) . . . . ? C38 C39 C40 N1 179.4(3) . . . . ? O2 C35 C40 C39 -180.0(2) . . . . ? C36 C35 C40 C39 -0.7(4) . . . . ? O2 C35 C40 N1 2.2(4) . . . . ? C36 C35 C40 N1 -178.6(3) . . . . ? C2 C1 N1 C40 -176.0(2) . . . . ? C2 C1 N1 Pd1 -2.0(3) . . . . ? C39 C40 N1 C1 130.4(3) . . . . ? C35 C40 N1 C1 -51.7(4) . . . . ? C39 C40 N1 Pd1 -42.6(3) . . . . ? C35 C40 N1 Pd1 135.3(2) . . . . ? C4 C5 N2 C2 1.0(3) . . . . ? C6 C5 N2 C2 174.1(2) . . . . ? C4 C5 N2 Pd1 169.20(19) . . . . ? C6 C5 N2 Pd1 -17.7(4) . . . . ? C3 C2 N2 C5 -1.1(3) . . . . ? C1 C2 N2 C5 174.2(2) . . . . ? C3 C2 N2 Pd1 -171.61(17) . . . . ? C1 C2 N2 Pd1 3.7(3) . . . . ? C20 C19 N3 C22 -1.4(3) . . . . ? C6 C19 N3 C22 -172.7(2) . . . . ? C20 C19 N3 Pd1 -169.2(2) . . . . ? C6 C19 N3 Pd1 19.4(4) . . . . ? C21 C22 N3 C19 1.1(3) . . . . ? C23 C22 N3 C19 179.0(2) . . . . ? C21 C22 N3 Pd1 171.3(2) . . . . ? C23 C22 N3 Pd1 -10.8(3) . . . . ? C22 C23 N4 C24 -173.7(3) . . . . ? C22 C23 N4 Pd1 3.3(3) . . . . ? C25 C24 N4 C23 -50.4(4) . . . . ? C29 C24 N4 C23 128.1(3) . . . . ? C25 C24 N4 Pd1 133.3(3) . . . . ? C29 C24 N4 Pd1 -48.2(4) . . . . ? C30 C31 N5 C32 166.3(3) . . . . ? C30 C31 N5 C33 -65.3(3) . . . . ? C34 C33 N5 C32 57.7(4) . . . . ? C34 C33 N5 C31 -70.0(4) . . . . ? C28 C29 O1 C30 -19.5(4) . . . . ? C24 C29 O1 C30 162.7(2) . . . . ? C31 C30 O1 C29 -162.2(2) . . . . ? C36 C35 O2 C34 21.7(4) . . . . ? C40 C35 O2 C34 -159.1(3) . . . . ? C33 C34 O2 C35 67.3(4) . . . . ? C19 N3 Pd1 N2 -2.3(3) . . . . ? C22 N3 Pd1 N2 -169.6(2) . . . . ? C19 N3 Pd1 N1 28.0(5) . . . . ? C22 N3 Pd1 N1 -139.2(3) . . . . ? C19 N3 Pd1 N4 177.0(3) . . . . ? C22 N3 Pd1 N4 9.8(2) . . . . ? C5 N2 Pd1 N3 1.5(2) . . . . ? C2 N2 Pd1 N3 169.16(19) . . . . ? C5 N2 Pd1 N1 -171.4(3) . . . . ? C2 N2 Pd1 N1 -3.68(18) . . . . ? C5 N2 Pd1 N4 -1.6(6) . . . . ? C2 N2 Pd1 N4 166.1(4) . . . . ? C1 N1 Pd1 N3 -27.8(5) . . . . ? C40 N1 Pd1 N3 145.7(3) . . . . ? C1 N1 Pd1 N2 3.05(18) . . . . ? C40 N1 Pd1 N2 176.5(2) . . . . ? C1 N1 Pd1 N4 -174.64(18) . . . . ? C40 N1 Pd1 N4 -1.2(2) . . . . ? C23 N4 Pd1 N3 -7.0(2) . . . . ? C24 N4 Pd1 N3 169.5(3) . . . . ? C23 N4 Pd1 N2 -3.9(6) . . . . ? C24 N4 Pd1 N2 172.6(4) . . . . ? C23 N4 Pd1 N1 165.25(19) . . . . ? C24 N4 Pd1 N1 -18.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.000 _refine_diff_density_min -0.833 _refine_diff_density_rms 0.086 data_j10084cold_TiCl(Lp) _database_code_depnum_ccdc_archive 'CCDC 895819' #TrackingRef 'combined_CIF.cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C0 C39 H48 Cl N4 O6 Ti' _chemical_formula_sum 'C0 C39 H48 Cl N4 O6 Ti' _chemical_formula_weight 752.16 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' C C 0.0033 0.0016 '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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.540(5) _cell_length_b 20.124(5) _cell_length_c 14.798(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 111.333(5) _cell_angle_gamma 90.000(5) _cell_volume 3756(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8341 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1588 _exptl_absorpt_coefficient_mu 0.350 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.98760 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 16.1042 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 24594 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.1154 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8341 _reflns_number_gt 3571 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SIR-92 (Giacovazzo, 1994) ' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1998) ' _computing_molecular_graphics 'ORTEP (Farrugia, 1997) ' _computing_publication_material 'enCIFer (Allen et al., 2004) ' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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. Attempts at splitting atoms in disordered THF and disordered ligand (around C26) led to diverging structures ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0798P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8341 _refine_ls_number_parameters 462 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1173 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1456 _refine_ls_wR_factor_gt 0.1344 _refine_ls_goodness_of_fit_ref 0.817 _refine_ls_restrained_S_all 0.817 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8696(3) 0.30809(16) 0.1645(2) 0.0460(8) Uani 1 1 d . . . H1 H 0.8653 0.3455 0.2021 0.055 Uiso 1 1 calc R . . C2 C 0.7777(3) 0.27300(16) 0.1099(2) 0.0430(8) Uani 1 1 d . . . C3 C 0.6717(3) 0.28089(18) 0.0980(2) 0.0566(9) Uani 1 1 d . . . H3 H 0.6426 0.3153 0.1246 0.068 Uiso 1 1 calc R . . C4 C 0.6171(3) 0.2293(2) 0.0403(3) 0.0615(10) Uani 1 1 d . . . H4 H 0.5429 0.2216 0.0194 0.074 Uiso 1 1 calc R . . C5 C 0.6905(3) 0.19016(17) 0.0179(2) 0.0523(9) Uani 1 1 d . . . C6 C 0.6714(3) 0.1224(2) -0.0303(3) 0.0670(10) Uani 1 1 d . . . C7 C 0.5601(3) 0.1146(3) -0.0999(4) 0.1054(16) Uani 1 1 d . . . H7A H 0.5104 0.1244 -0.0663 0.126 Uiso 1 1 calc R . . H7B H 0.5484 0.0681 -0.1230 0.126 Uiso 1 1 calc R . . C8 C 0.5371(4) 0.1612(3) -0.1867(3) 0.1181(19) Uani 1 1 d . . . H8A H 0.4760 0.1893 -0.1924 0.177 Uiso 1 1 calc R . . H8B H 0.5214 0.1349 -0.2460 0.177 Uiso 1 1 calc R . . H8C H 0.5992 0.1893 -0.1773 0.177 Uiso 1 1 calc R . . C9 C 0.6912(3) 0.06658(18) 0.0576(3) 0.0719(11) Uani 1 1 d . . . H9A H 0.6874 0.0219 0.0287 0.086 Uiso 1 1 calc R . . H9B H 0.7643 0.0724 0.1050 0.086 Uiso 1 1 calc R . . C10 C 0.6199(4) 0.0678(2) 0.1103(3) 0.0963(14) Uani 1 1 d . . . H10A H 0.6231 0.1114 0.1405 0.144 Uiso 1 1 calc R . . H10B H 0.6409 0.0334 0.1607 0.144 Uiso 1 1 calc R . . H10C H 0.5473 0.0592 0.0655 0.144 Uiso 1 1 calc R . . C11 C 0.7520(3) 0.10406(17) -0.0739(2) 0.0508(8) Uani 1 1 d . . . C12 C 0.7413(3) 0.0533(2) -0.1415(3) 0.0698(11) Uani 1 1 d . . . H12 H 0.6779 0.0304 -0.1776 0.084 Uiso 1 1 calc R . . C13 C 0.8402(3) 0.0428(2) -0.1459(3) 0.0789(12) Uani 1 1 d . . . H13 H 0.8579 0.0111 -0.1852 0.095 Uiso 1 1 calc R . . C14 C 0.9089(3) 0.08745(16) -0.0820(2) 0.0500(8) Uani 1 1 d . . . C15 C 1.0170(3) 0.09863(17) -0.0518(2) 0.0535(9) Uani 1 1 d . . . H15 H 1.0610 0.0728 -0.0756 0.064 Uiso 1 1 calc R . . C16 C 1.1641(3) 0.16058(18) 0.0505(2) 0.0471(8) Uani 1 1 d . . . C17 C 1.2475(3) 0.1174(2) 0.0615(2) 0.0665(11) Uani 1 1 d . . . H17 H 1.2341 0.0723 0.0414 0.080 Uiso 1 1 calc R . . C18 C 1.3504(3) 0.1406(3) 0.1021(3) 0.0842(14) Uani 1 1 d . . . H18 H 1.4077 0.1112 0.1094 0.101 Uiso 1 1 calc R . . C19 C 1.3716(3) 0.2056(3) 0.1321(3) 0.0856(14) Uani 1 1 d . . . H19 H 1.4428 0.2207 0.1590 0.103 Uiso 1 1 calc R . . C20 C 1.2889(3) 0.2488(2) 0.1230(2) 0.0685(11) Uani 1 1 d . . . H20 H 1.3022 0.2937 0.1440 0.082 Uiso 1 1 calc R . . C21 C 1.1867(3) 0.22486(18) 0.0825(2) 0.0484(8) Uani 1 1 d . . . C22 C 1.0805(3) 0.3125(2) -0.0052(3) 0.0848(13) Uani 1 1 d . . . H22A H 1.1213 0.3533 0.0226 0.102 Uiso 1 1 calc R . . H22B H 1.1072 0.2947 -0.0543 0.102 Uiso 1 1 calc R . . C23 C 0.9732(3) 0.3290(3) -0.0505(3) 0.1005(16) Uani 1 1 d . . . H23A H 0.9618 0.3485 -0.1149 0.121 Uiso 1 1 calc R . . H23B H 0.9545 0.3631 -0.0112 0.121 Uiso 1 1 calc R . . C24 C 0.8108(3) 0.2742(2) -0.1488(2) 0.0721(11) Uani 1 1 d . . . H24A H 0.7814 0.2287 -0.1619 0.087 Uiso 1 1 calc R . . H24B H 0.8302 0.2880 -0.2044 0.087 Uiso 1 1 calc R . . C25 C 0.7268(3) 0.3205(3) -0.1413(3) 0.0864(13) Uani 1 1 d . . . H25A H 0.6602 0.3141 -0.1978 0.104 Uiso 1 1 calc R . . H25B H 0.7125 0.3105 -0.0817 0.104 Uiso 1 1 calc R . . C26 C 0.7023(4) 0.4316(3) -0.0999(5) 0.122(2) Uani 1 1 d . . . H26A H 0.6273 0.4330 -0.1444 0.147 Uiso 1 1 calc R . . H26B H 0.7047 0.4151 -0.0361 0.147 Uiso 1 1 calc R . . C27 C 0.7474(5) 0.4969(3) -0.0893(4) 0.129(2) Uani 1 1 d . . . H27A H 0.7483 0.5118 -0.1527 0.155 Uiso 1 1 calc R . . H27B H 0.7019 0.5280 -0.0700 0.155 Uiso 1 1 calc R . . C28 C 0.8655(4) 0.5134(2) 0.0789(3) 0.0916(15) Uani 1 1 d . . . H28A H 0.8123 0.4882 0.0965 0.110 Uiso 1 1 calc R . . H28B H 0.8543 0.5614 0.0864 0.110 Uiso 1 1 calc R . . C29 C 0.9729(3) 0.49431(17) 0.1435(3) 0.0720(11) Uani 1 1 d . . . H29A H 1.0260 0.5085 0.1158 0.086 Uiso 1 1 calc R . . H29B H 0.9906 0.5152 0.2080 0.086 Uiso 1 1 calc R . . C30 C 1.0596(3) 0.39356(18) 0.2140(2) 0.0582(9) Uani 1 1 d . . . C31 C 1.1530(4) 0.4265(2) 0.2694(3) 0.0715(11) Uani 1 1 d . . . H31 H 1.1573 0.4735 0.2659 0.086 Uiso 1 1 calc R . . C32 C 1.2392(4) 0.3906(3) 0.3295(3) 0.0801(12) Uani 1 1 d . . . H32 H 1.3029 0.4130 0.3664 0.096 Uiso 1 1 calc R . . C33 C 1.2334(3) 0.3232(2) 0.3360(3) 0.0720(11) Uani 1 1 d . . . H33 H 1.2928 0.2991 0.3778 0.086 Uiso 1 1 calc R . . C34 C 1.1413(3) 0.28985(19) 0.2821(2) 0.0571(9) Uani 1 1 d . . . H34 H 1.1382 0.2429 0.2867 0.069 Uiso 1 1 calc R . . C35 C 1.0534(3) 0.32441(17) 0.2211(2) 0.0477(8) Uani 1 1 d . . . C100 C 0.6727(9) 0.6222(6) 0.1624(5) 0.260(6) Uani 1 1 d . . . H10D H 0.6359 0.6560 0.1873 0.313 Uiso 1 1 calc R . . H10E H 0.7402 0.6105 0.2151 0.313 Uiso 1 1 calc R . . C101 C 0.6927(7) 0.6473(3) 0.0834(7) 0.164(3) Uani 1 1 d . . . H10F H 0.7086 0.6954 0.0908 0.196 Uiso 1 1 calc R . . H10G H 0.7522 0.6236 0.0739 0.196 Uiso 1 1 calc R . . C102 C 0.6034(6) 0.6357(5) 0.0125(6) 0.168(3) Uani 1 1 d . . . H10H H 0.6188 0.6211 -0.0449 0.202 Uiso 1 1 calc R . . H10I H 0.5628 0.6777 -0.0047 0.202 Uiso 1 1 calc R . . C103 C 0.5446(7) 0.5906(7) 0.0325(7) 0.240(6) Uani 1 1 d . . . H10J H 0.5260 0.5554 -0.0176 0.288 Uiso 1 1 calc R . . H10K H 0.4780 0.6111 0.0323 0.288 Uiso 1 1 calc R . . N1 N 0.9606(2) 0.28878(12) 0.16294(16) 0.0416(6) Uani 1 1 d . . . N2 N 0.78993(19) 0.21676(12) 0.06002(17) 0.0434(6) Uani 1 1 d . . . N3 N 0.8533(2) 0.12604(12) -0.03805(17) 0.0443(6) Uani 1 1 d . . . N4 N 1.0555(2) 0.14623(13) 0.01071(17) 0.0443(6) Uani 1 1 d . . . O1 O 1.09773(16) 0.26422(11) 0.07056(14) 0.0487(5) Uani 1 1 d . . . O2 O 0.90459(17) 0.27337(10) -0.06253(14) 0.0489(6) Uani 1 1 d . . . O3 O 0.7620(2) 0.38739(15) -0.13854(19) 0.0832(8) Uani 1 1 d . . . O5 O 0.9720(2) 0.42422(11) 0.15145(17) 0.0663(7) Uani 1 1 d . . . O100 O 0.6040(6) 0.5611(5) 0.1299(10) 0.333(6) Uani 1 1 d . . . O4 O 0.8529(3) 0.49967(16) -0.0188(2) 0.0991(10) Uani 1 1 d . . . Cl1 Cl 1.00848(7) 0.13304(4) 0.20026(6) 0.0589(3) Uani 1 1 d . . . Ti1 Ti 0.94441(4) 0.20166(3) 0.05946(3) 0.03846(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.070(2) 0.031(2) 0.0456(17) 0.0026(14) 0.0316(18) 0.0042(17) C2 0.057(2) 0.036(2) 0.0440(17) 0.0024(15) 0.0289(17) 0.0071(16) C3 0.064(2) 0.046(2) 0.072(2) 0.0055(18) 0.039(2) 0.0153(18) C4 0.045(2) 0.067(3) 0.077(2) 0.007(2) 0.0279(19) 0.0122(19) C5 0.052(2) 0.048(2) 0.062(2) 0.0031(17) 0.0264(18) 0.0047(18) C6 0.050(2) 0.065(3) 0.085(3) -0.026(2) 0.024(2) -0.0133(19) C7 0.075(3) 0.106(4) 0.134(4) -0.034(3) 0.037(3) -0.010(3) C8 0.098(4) 0.151(5) 0.088(3) 0.051(3) 0.013(3) 0.029(3) C9 0.091(3) 0.040(2) 0.094(3) 0.008(2) 0.045(2) -0.001(2) C10 0.103(3) 0.085(4) 0.108(3) 0.006(3) 0.048(3) 0.003(3) C11 0.060(2) 0.042(2) 0.054(2) -0.0029(16) 0.0247(18) -0.0042(17) C12 0.069(3) 0.067(3) 0.074(2) -0.022(2) 0.026(2) -0.021(2) C13 0.089(3) 0.069(3) 0.088(3) -0.041(2) 0.044(2) -0.013(2) C14 0.064(2) 0.036(2) 0.056(2) -0.0103(16) 0.0304(19) -0.0012(17) C15 0.065(2) 0.044(2) 0.064(2) -0.0053(18) 0.038(2) 0.0058(18) C16 0.049(2) 0.057(2) 0.0427(17) 0.0016(16) 0.0248(16) 0.0056(18) C17 0.061(2) 0.078(3) 0.065(2) -0.004(2) 0.028(2) 0.018(2) C18 0.056(3) 0.128(5) 0.073(3) -0.001(3) 0.028(2) 0.027(3) C19 0.052(3) 0.133(5) 0.077(3) -0.015(3) 0.029(2) -0.011(3) C20 0.062(3) 0.082(3) 0.067(2) -0.013(2) 0.031(2) -0.016(2) C21 0.049(2) 0.059(2) 0.0457(18) 0.0012(17) 0.0269(17) 0.0004(18) C22 0.086(3) 0.058(3) 0.111(3) 0.028(2) 0.036(3) -0.003(2) C23 0.079(3) 0.099(4) 0.114(4) 0.055(3) 0.024(3) -0.014(3) C24 0.095(3) 0.064(3) 0.046(2) -0.0010(18) 0.013(2) 0.008(2) C25 0.073(3) 0.106(4) 0.070(3) 0.019(3) 0.013(2) 0.012(3) C26 0.097(4) 0.094(4) 0.203(6) 0.051(4) 0.087(4) 0.039(3) C27 0.148(6) 0.115(5) 0.153(5) 0.044(4) 0.087(5) 0.063(4) C28 0.136(4) 0.043(3) 0.140(4) 0.005(3) 0.102(4) 0.011(3) C29 0.106(3) 0.031(2) 0.097(3) -0.005(2) 0.058(3) 0.002(2) C30 0.086(3) 0.042(2) 0.053(2) -0.0055(18) 0.033(2) -0.011(2) C31 0.107(3) 0.050(3) 0.069(2) -0.017(2) 0.045(3) -0.031(3) C32 0.091(3) 0.085(4) 0.059(2) -0.017(2) 0.022(2) -0.031(3) C33 0.071(3) 0.083(3) 0.056(2) -0.006(2) 0.015(2) -0.008(2) C34 0.071(3) 0.055(2) 0.0459(19) -0.0026(18) 0.0222(19) -0.002(2) C35 0.066(2) 0.042(2) 0.0430(18) -0.0093(16) 0.0293(18) -0.0096(19) C100 0.361(14) 0.370(15) 0.103(5) -0.036(7) 0.147(8) -0.054(12) C101 0.159(7) 0.098(5) 0.220(9) -0.013(5) 0.054(7) -0.016(5) C102 0.091(4) 0.215(9) 0.190(8) 0.094(7) 0.040(5) 0.032(5) C103 0.134(7) 0.323(15) 0.226(9) 0.109(9) 0.022(6) -0.065(8) N1 0.0563(17) 0.0317(16) 0.0436(14) 0.0014(12) 0.0266(13) 0.0013(13) N2 0.0471(16) 0.0391(17) 0.0485(15) 0.0017(12) 0.0229(13) 0.0026(13) N3 0.0503(16) 0.0341(16) 0.0523(15) -0.0035(12) 0.0231(14) 0.0004(13) N4 0.0515(17) 0.0381(17) 0.0494(15) -0.0010(13) 0.0257(14) 0.0042(13) O1 0.0561(14) 0.0433(14) 0.0522(12) 0.0015(11) 0.0263(11) -0.0010(11) O2 0.0654(15) 0.0427(14) 0.0414(12) 0.0054(10) 0.0228(12) 0.0029(11) O3 0.090(2) 0.066(2) 0.0934(19) 0.0172(16) 0.0328(17) 0.0172(17) O5 0.096(2) 0.0293(14) 0.0758(16) -0.0029(12) 0.0341(16) -0.0065(14) O100 0.200(7) 0.263(9) 0.545(17) 0.239(10) 0.145(8) 0.044(6) O4 0.103(2) 0.099(3) 0.103(2) 0.0159(19) 0.047(2) 0.029(2) Cl1 0.0817(6) 0.0442(5) 0.0566(5) 0.0157(4) 0.0318(5) 0.0111(5) Ti1 0.0462(3) 0.0305(3) 0.0443(3) 0.0001(3) 0.0231(3) 0.0029(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.300(4) . ? C1 C2 1.403(4) . ? C1 H1 0.9500 . ? C2 C3 1.390(4) . ? C2 N2 1.393(4) . ? C3 C4 1.377(5) . ? C3 H3 0.9500 . ? C4 C5 1.400(4) . ? C4 H4 0.9500 . ? C5 N2 1.370(4) . ? C5 C6 1.516(5) . ? C6 C7 1.493(5) . ? C6 C11 1.501(4) . ? C6 C9 1.665(5) . ? C7 C8 1.528(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.446(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N3 1.353(4) . ? C11 C12 1.400(5) . ? C12 C13 1.381(5) . ? C12 H12 0.9500 . ? C13 C14 1.388(5) . ? C13 H13 0.9500 . ? C14 C15 1.384(4) . ? C14 N3 1.397(4) . ? C15 N4 1.302(4) . ? C15 H15 0.9500 . ? C16 C21 1.373(4) . ? C16 C17 1.387(4) . ? C16 N4 1.400(4) . ? C17 C18 1.383(5) . ? C17 H17 0.9500 . ? C18 C19 1.376(6) . ? C18 H18 0.9500 . ? C19 C20 1.386(6) . ? C19 H19 0.9500 . ? C20 C21 1.380(5) . ? C20 H20 0.9500 . ? C21 O1 1.398(4) . ? C22 C23 1.400(5) . ? C22 O1 1.438(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 O2 1.423(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O2 1.437(4) . ? C24 C25 1.505(5) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 O3 1.424(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.433(7) . ? C26 O3 1.451(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 O4 1.431(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O4 1.420(5) . ? C28 C29 1.471(5) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O5 1.416(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 O5 1.358(4) . ? C30 C31 1.398(5) . ? C30 C35 1.400(5) . ? C31 C32 1.386(6) . ? C31 H31 0.9500 . ? C32 C33 1.363(6) . ? C32 H32 0.9500 . ? C33 C34 1.385(5) . ? C33 H33 0.9500 . ? C34 C35 1.390(5) . ? C34 H34 0.9500 . ? C35 N1 1.431(4) . ? C100 C101 1.386(9) . ? C100 O100 1.511(12) . ? C100 H10D 0.9900 . ? C100 H10E 0.9900 . ? C101 C102 1.301(8) . ? C101 H10F 0.9900 . ? C101 H10G 0.9900 . ? C102 C103 1.311(9) . ? C102 H10H 0.9900 . ? C102 H10I 0.9900 . ? C103 O100 1.494(10) . ? C103 H10J 0.9900 . ? C103 H10K 0.9900 . ? N1 Ti1 2.285(2) . ? N2 Ti1 2.117(3) . ? N3 Ti1 2.150(3) . ? N4 Ti1 2.195(2) . ? O1 Ti1 2.382(2) . ? O2 Ti1 2.219(2) . ? Cl1 Ti1 2.3843(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 N1 C1 C2 119.1(3) . . ? N1 C1 H1 120.4 . . ? C2 C1 H1 120.4 . . ? C3 C2 N2 110.0(3) . . ? C3 C2 C1 132.3(3) . . ? N2 C2 C1 117.6(3) . . ? C4 C3 C2 106.8(3) . . ? C4 C3 H3 126.6 . . ? C2 C3 H3 126.6 . . ? C3 C4 C5 107.7(3) . . ? C3 C4 H4 126.2 . . ? C5 C4 H4 126.2 . . ? N2 C5 C4 109.7(3) . . ? N2 C5 C6 122.5(3) . . ? C4 C5 C6 127.1(3) . . ? C7 C6 C11 112.7(3) . . ? C7 C6 C5 112.1(3) . . ? C11 C6 C5 113.4(3) . . ? C7 C6 C9 107.6(3) . . ? C11 C6 C9 103.5(3) . . ? C5 C6 C9 106.8(3) . . ? C6 C7 C8 111.2(4) . . ? C6 C7 H7A 109.4 . . ? C8 C7 H7A 109.4 . . ? C6 C7 H7B 109.4 . . ? C8 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C6 117.4(3) . . ? C10 C9 H9A 107.9 . . ? C6 C9 H9A 107.9 . . ? C10 C9 H9B 107.9 . . ? C6 C9 H9B 107.9 . . ? H9A C9 H9B 107.2 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 C12 110.1(3) . . ? N3 C11 C6 122.9(3) . . ? C12 C11 C6 125.8(3) . . ? C13 C12 C11 107.3(3) . . ? C13 C12 H12 126.4 . . ? C11 C12 H12 126.4 . . ? C12 C13 C14 106.8(3) . . ? C12 C13 H13 126.6 . . ? C14 C13 H13 126.6 . . ? C15 C14 C13 133.9(3) . . ? C15 C14 N3 116.4(3) . . ? C13 C14 N3 109.6(3) . . ? N4 C15 C14 116.9(3) . . ? N4 C15 H15 121.5 . . ? C14 C15 H15 121.5 . . ? C21 C16 C17 118.7(3) . . ? C21 C16 N4 114.0(3) . . ? C17 C16 N4 127.3(3) . . ? C18 C17 C16 119.2(4) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C19 C18 C17 121.3(4) . . ? C19 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C18 C19 C20 120.0(4) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C21 C20 C19 118.0(4) . . ? C21 C20 H20 121.0 . . ? C19 C20 H20 121.0 . . ? C16 C21 C20 122.8(3) . . ? C16 C21 O1 114.6(3) . . ? C20 C21 O1 122.6(3) . . ? C23 C22 O1 112.3(3) . . ? C23 C22 H22A 109.2 . . ? O1 C22 H22A 109.2 . . ? C23 C22 H22B 109.2 . . ? O1 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? C22 C23 O2 113.0(4) . . ? C22 C23 H23A 109.0 . . ? O2 C23 H23A 109.0 . . ? C22 C23 H23B 109.0 . . ? O2 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? O2 C24 C25 112.9(3) . . ? O2 C24 H24A 109.0 . . ? C25 C24 H24A 109.0 . . ? O2 C24 H24B 109.0 . . ? C25 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? O3 C25 C24 109.4(4) . . ? O3 C25 H25A 109.8 . . ? C24 C25 H25A 109.8 . . ? O3 C25 H25B 109.8 . . ? C24 C25 H25B 109.8 . . ? H25A C25 H25B 108.2 . . ? C27 C26 O3 109.3(4) . . ? C27 C26 H26A 109.8 . . ? O3 C26 H26A 109.8 . . ? C27 C26 H26B 109.8 . . ? O3 C26 H26B 109.8 . . ? H26A C26 H26B 108.3 . . ? O4 C27 C26 112.8(5) . . ? O4 C27 H27A 109.0 . . ? C26 C27 H27A 109.0 . . ? O4 C27 H27B 109.0 . . ? C26 C27 H27B 109.0 . . ? H27A C27 H27B 107.8 . . ? O4 C28 C29 109.6(3) . . ? O4 C28 H28A 109.8 . . ? C29 C28 H28A 109.8 . . ? O4 C28 H28B 109.8 . . ? C29 C28 H28B 109.8 . . ? H28A C28 H28B 108.2 . . ? O5 C29 C28 106.1(3) . . ? O5 C29 H29A 110.5 . . ? C28 C29 H29A 110.5 . . ? O5 C29 H29B 110.5 . . ? C28 C29 H29B 110.5 . . ? H29A C29 H29B 108.7 . . ? O5 C30 C31 124.3(4) . . ? O5 C30 C35 116.2(3) . . ? C31 C30 C35 119.5(4) . . ? C32 C31 C30 120.0(4) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C33 C32 C31 120.5(4) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C32 C33 C34 120.3(4) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C33 C34 C35 120.7(4) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? C34 C35 C30 119.0(3) . . ? C34 C35 N1 119.8(3) . . ? C30 C35 N1 121.1(3) . . ? C101 C100 O100 108.3(7) . . ? C101 C100 H10D 110.0 . . ? O100 C100 H10D 110.0 . . ? C101 C100 H10E 110.0 . . ? O100 C100 H10E 110.0 . . ? H10D C100 H10E 108.4 . . ? C102 C101 C100 101.9(8) . . ? C102 C101 H10F 111.4 . . ? C100 C101 H10F 111.4 . . ? C102 C101 H10G 111.4 . . ? C100 C101 H10G 111.4 . . ? H10F C101 H10G 109.3 . . ? C101 C102 C103 113.8(7) . . ? C101 C102 H10H 108.8 . . ? C103 C102 H10H 108.8 . . ? C101 C102 H10I 108.8 . . ? C103 C102 H10I 108.8 . . ? H10H C102 H10I 107.7 . . ? C102 C103 O100 109.5(7) . . ? C102 C103 H10J 109.8 . . ? O100 C103 H10J 109.8 . . ? C102 C103 H10K 109.8 . . ? O100 C103 H10K 109.8 . . ? H10J C103 H10K 108.2 . . ? C1 N1 C35 118.1(3) . . ? C1 N1 Ti1 112.4(2) . . ? C35 N1 Ti1 129.56(19) . . ? C5 N2 C2 105.8(2) . . ? C5 N2 Ti1 138.7(2) . . ? C2 N2 Ti1 115.3(2) . . ? C11 N3 C14 106.1(3) . . ? C11 N3 Ti1 138.3(2) . . ? C14 N3 Ti1 115.5(2) . . ? C15 N4 C16 122.6(3) . . ? C15 N4 Ti1 117.5(2) . . ? C16 N4 Ti1 119.8(2) . . ? C21 O1 C22 111.7(2) . . ? C21 O1 Ti1 113.49(19) . . ? C22 O1 Ti1 114.4(2) . . ? C23 O2 C24 115.3(3) . . ? C23 O2 Ti1 117.1(2) . . ? C24 O2 Ti1 127.3(2) . . ? C25 O3 C26 111.3(4) . . ? C30 O5 C29 118.5(3) . . ? C103 O100 C100 92.1(6) . . ? C28 O4 C27 117.9(4) . . ? N2 Ti1 N3 77.16(9) . . ? N2 Ti1 N4 150.56(10) . . ? N3 Ti1 N4 73.41(10) . . ? N2 Ti1 O2 87.81(9) . . ? N3 Ti1 O2 90.23(9) . . ? N4 Ti1 O2 93.20(8) . . ? N2 Ti1 N1 75.01(9) . . ? N3 Ti1 N1 152.17(9) . . ? N4 Ti1 N1 134.41(10) . . ? O2 Ti1 N1 88.96(8) . . ? N2 Ti1 O1 139.60(9) . . ? N3 Ti1 O1 133.88(8) . . ? N4 Ti1 O1 66.84(9) . . ? O2 Ti1 O1 70.12(8) . . ? N1 Ti1 O1 71.30(8) . . ? N2 Ti1 Cl1 97.22(7) . . ? N3 Ti1 Cl1 96.55(7) . . ? N4 Ti1 Cl1 85.29(7) . . ? O2 Ti1 Cl1 172.30(7) . . ? N1 Ti1 Cl1 86.74(7) . . ? O1 Ti1 Cl1 102.41(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 179.1(3) . . . . ? N1 C1 C2 N2 3.0(4) . . . . ? N2 C2 C3 C4 -0.1(4) . . . . ? C1 C2 C3 C4 -176.3(3) . . . . ? C2 C3 C4 C5 0.3(4) . . . . ? C3 C4 C5 N2 -0.5(4) . . . . ? C3 C4 C5 C6 169.7(3) . . . . ? N2 C5 C6 C7 -159.4(3) . . . . ? C4 C5 C6 C7 31.5(5) . . . . ? N2 C5 C6 C11 -30.3(5) . . . . ? C4 C5 C6 C11 160.6(3) . . . . ? N2 C5 C6 C9 83.0(4) . . . . ? C4 C5 C6 C9 -86.1(4) . . . . ? C11 C6 C7 C8 -62.9(5) . . . . ? C5 C6 C7 C8 66.5(5) . . . . ? C9 C6 C7 C8 -176.4(4) . . . . ? C7 C6 C9 C10 -56.2(5) . . . . ? C11 C6 C9 C10 -175.8(3) . . . . ? C5 C6 C9 C10 64.3(4) . . . . ? C7 C6 C11 N3 158.5(4) . . . . ? C5 C6 C11 N3 29.8(5) . . . . ? C9 C6 C11 N3 -85.5(4) . . . . ? C7 C6 C11 C12 -35.1(5) . . . . ? C5 C6 C11 C12 -163.9(3) . . . . ? C9 C6 C11 C12 80.9(4) . . . . ? N3 C11 C12 C13 1.3(4) . . . . ? C6 C11 C12 C13 -166.6(4) . . . . ? C11 C12 C13 C14 -0.6(5) . . . . ? C12 C13 C14 C15 176.5(4) . . . . ? C12 C13 C14 N3 -0.3(4) . . . . ? C13 C14 C15 N4 179.9(4) . . . . ? N3 C14 C15 N4 -3.5(4) . . . . ? C21 C16 C17 C18 -1.6(5) . . . . ? N4 C16 C17 C18 179.6(3) . . . . ? C16 C17 C18 C19 0.3(6) . . . . ? C17 C18 C19 C20 0.8(6) . . . . ? C18 C19 C20 C21 -0.7(6) . . . . ? C17 C16 C21 C20 1.8(5) . . . . ? N4 C16 C21 C20 -179.3(3) . . . . ? C17 C16 C21 O1 -178.5(3) . . . . ? N4 C16 C21 O1 0.5(4) . . . . ? C19 C20 C21 C16 -0.6(5) . . . . ? C19 C20 C21 O1 179.6(3) . . . . ? O1 C22 C23 O2 -38.4(5) . . . . ? O2 C24 C25 O3 68.3(4) . . . . ? O3 C26 C27 O4 -65.0(6) . . . . ? O4 C28 C29 O5 -77.0(4) . . . . ? O5 C30 C31 C32 -178.4(3) . . . . ? C35 C30 C31 C32 1.2(5) . . . . ? C30 C31 C32 C33 -0.8(5) . . . . ? C31 C32 C33 C34 0.5(6) . . . . ? C32 C33 C34 C35 -0.5(5) . . . . ? C33 C34 C35 C30 0.9(4) . . . . ? C33 C34 C35 N1 177.4(3) . . . . ? O5 C30 C35 C34 178.4(3) . . . . ? C31 C30 C35 C34 -1.2(4) . . . . ? O5 C30 C35 N1 1.9(4) . . . . ? C31 C30 C35 N1 -177.7(3) . . . . ? O100 C100 C101 C102 36.2(11) . . . . ? C100 C101 C102 C103 -19.0(13) . . . . ? C101 C102 C103 O100 -5.2(15) . . . . ? C2 C1 N1 C35 -178.5(3) . . . . ? C2 C1 N1 Ti1 3.3(3) . . . . ? C34 C35 N1 C1 130.5(3) . . . . ? C30 C35 N1 C1 -53.0(4) . . . . ? C34 C35 N1 Ti1 -51.7(3) . . . . ? C30 C35 N1 Ti1 124.8(3) . . . . ? C4 C5 N2 C2 0.4(3) . . . . ? C6 C5 N2 C2 -170.3(3) . . . . ? C4 C5 N2 Ti1 -172.7(2) . . . . ? C6 C5 N2 Ti1 16.6(5) . . . . ? C3 C2 N2 C5 -0.2(3) . . . . ? C1 C2 N2 C5 176.7(3) . . . . ? C3 C2 N2 Ti1 174.74(19) . . . . ? C1 C2 N2 Ti1 -8.4(3) . . . . ? C12 C11 N3 C14 -1.4(4) . . . . ? C6 C11 N3 C14 166.9(3) . . . . ? C12 C11 N3 Ti1 176.5(2) . . . . ? C6 C11 N3 Ti1 -15.2(5) . . . . ? C15 C14 N3 C11 -176.4(3) . . . . ? C13 C14 N3 C11 1.0(4) . . . . ? C15 C14 N3 Ti1 5.2(4) . . . . ? C13 C14 N3 Ti1 -177.4(2) . . . . ? C14 C15 N4 C16 177.0(3) . . . . ? C14 C15 N4 Ti1 0.1(4) . . . . ? C21 C16 N4 C15 155.5(3) . . . . ? C17 C16 N4 C15 -25.6(5) . . . . ? C21 C16 N4 Ti1 -27.7(3) . . . . ? C17 C16 N4 Ti1 151.1(3) . . . . ? C16 C21 O1 C22 -108.0(3) . . . . ? C20 C21 O1 C22 71.8(4) . . . . ? C16 C21 O1 Ti1 23.2(3) . . . . ? C20 C21 O1 Ti1 -157.1(2) . . . . ? C23 C22 O1 C21 150.8(4) . . . . ? C23 C22 O1 Ti1 20.1(5) . . . . ? C22 C23 O2 C24 -145.9(4) . . . . ? C22 C23 O2 Ti1 40.6(5) . . . . ? C25 C24 O2 C23 -77.1(4) . . . . ? C25 C24 O2 Ti1 95.7(4) . . . . ? C24 C25 O3 C26 -161.1(4) . . . . ? C27 C26 O3 C25 174.2(4) . . . . ? C31 C30 O5 C29 -2.2(5) . . . . ? C35 C30 O5 C29 178.2(3) . . . . ? C28 C29 O5 C30 -174.5(3) . . . . ? C102 C103 O100 C100 24.3(12) . . . . ? C101 C100 O100 C103 -36.1(10) . . . . ? C29 C28 O4 C27 162.8(4) . . . . ? C26 C27 O4 C28 -89.8(5) . . . . ? C5 N2 Ti1 N3 -0.3(3) . . . . ? C2 N2 Ti1 N3 -173.0(2) . . . . ? C5 N2 Ti1 N4 -2.2(4) . . . . ? C2 N2 Ti1 N4 -174.88(19) . . . . ? C5 N2 Ti1 O2 90.4(3) . . . . ? C2 N2 Ti1 O2 -82.2(2) . . . . ? C5 N2 Ti1 N1 179.9(3) . . . . ? C2 N2 Ti1 N1 7.26(19) . . . . ? C5 N2 Ti1 O1 145.7(3) . . . . ? C2 N2 Ti1 O1 -27.0(3) . . . . ? C5 N2 Ti1 Cl1 -95.4(3) . . . . ? C2 N2 Ti1 Cl1 91.90(19) . . . . ? C11 N3 Ti1 N2 -0.5(3) . . . . ? C14 N3 Ti1 N2 177.3(2) . . . . ? C11 N3 Ti1 N4 178.5(3) . . . . ? C14 N3 Ti1 N4 -3.7(2) . . . . ? C11 N3 Ti1 O2 -88.2(3) . . . . ? C14 N3 Ti1 O2 89.6(2) . . . . ? C11 N3 Ti1 N1 0.0(4) . . . . ? C14 N3 Ti1 N1 177.78(19) . . . . ? C11 N3 Ti1 O1 -150.3(3) . . . . ? C14 N3 Ti1 O1 27.5(3) . . . . ? C11 N3 Ti1 Cl1 95.4(3) . . . . ? C14 N3 Ti1 Cl1 -86.8(2) . . . . ? C15 N4 Ti1 N2 3.9(3) . . . . ? C16 N4 Ti1 N2 -173.0(2) . . . . ? C15 N4 Ti1 N3 2.0(2) . . . . ? C16 N4 Ti1 N3 -174.9(2) . . . . ? C15 N4 Ti1 O2 -87.3(2) . . . . ? C16 N4 Ti1 O2 95.8(2) . . . . ? C15 N4 Ti1 N1 -179.0(2) . . . . ? C16 N4 Ti1 N1 4.1(3) . . . . ? C15 N4 Ti1 O1 -154.1(2) . . . . ? C16 N4 Ti1 O1 29.0(2) . . . . ? C15 N4 Ti1 Cl1 100.2(2) . . . . ? C16 N4 Ti1 Cl1 -76.7(2) . . . . ? C23 O2 Ti1 N2 124.5(3) . . . . ? C24 O2 Ti1 N2 -48.2(2) . . . . ? C23 O2 Ti1 N3 -158.3(3) . . . . ? C24 O2 Ti1 N3 29.0(2) . . . . ? C23 O2 Ti1 N4 -84.9(3) . . . . ? C24 O2 Ti1 N4 102.4(2) . . . . ? C23 O2 Ti1 N1 49.5(3) . . . . ? C24 O2 Ti1 N1 -123.2(2) . . . . ? C23 O2 Ti1 O1 -21.0(3) . . . . ? C24 O2 Ti1 O1 166.3(2) . . . . ? C23 O2 Ti1 Cl1 -6.5(6) . . . . ? C24 O2 Ti1 Cl1 -179(40) . . . . ? C1 N1 Ti1 N2 -5.75(19) . . . . ? C35 N1 Ti1 N2 176.4(3) . . . . ? C1 N1 Ti1 N3 -6.3(3) . . . . ? C35 N1 Ti1 N3 175.8(2) . . . . ? C1 N1 Ti1 N4 175.72(18) . . . . ? C35 N1 Ti1 N4 -2.2(3) . . . . ? C1 N1 Ti1 O2 82.3(2) . . . . ? C35 N1 Ti1 O2 -95.6(2) . . . . ? C1 N1 Ti1 O1 151.6(2) . . . . ? C35 N1 Ti1 O1 -26.3(2) . . . . ? C1 N1 Ti1 Cl1 -104.12(19) . . . . ? C35 N1 Ti1 Cl1 78.0(2) . . . . ? C21 O1 Ti1 N2 169.56(17) . . . . ? C22 O1 Ti1 N2 -60.6(3) . . . . ? C21 O1 Ti1 N3 -59.6(2) . . . . ? C22 O1 Ti1 N3 70.2(3) . . . . ? C21 O1 Ti1 N4 -26.95(17) . . . . ? C22 O1 Ti1 N4 102.9(3) . . . . ? C21 O1 Ti1 O2 -129.61(18) . . . . ? C22 O1 Ti1 O2 0.2(2) . . . . ? C21 O1 Ti1 N1 134.54(19) . . . . ? C22 O1 Ti1 N1 -95.6(3) . . . . ? C21 O1 Ti1 Cl1 52.35(17) . . . . ? C22 O1 Ti1 Cl1 -177.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.593 _refine_diff_density_min -0.438 _refine_diff_density_rms 0.053 data_jl9054_VClH2OLp _database_code_depnum_ccdc_archive 'CCDC 895820' #TrackingRef 'combined_CIF.cif.cif' _vrf_PLAT026_jl9054_VClH2OLp ; PROBLEM: Ratio Observed / Unique Reflections too Low .... 21 Perc. RESPONSE: Weak data set. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H42 Cl N4 O6 V' _chemical_formula_sum 'C35 H42 Cl N4 O6 V' _chemical_formula_weight 701.12 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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.9312(3) _cell_length_b 16.3385(4) _cell_length_c 21.0755(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.7770(10) _cell_angle_gamma 90.00 _cell_volume 3370.06(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6891 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 26.4 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 0.425 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6623 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_process_details 'SADABS 2007/2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'Phi and Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6891 _diffrn_reflns_av_R_equivalents 0.0570 _diffrn_reflns_av_sigmaI/netI 0.2805 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 26.40 _reflns_number_total 6891 _reflns_number_gt 1414 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Siemans, 1993)' _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen et al., 2004)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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. Hydrogens on O100 were found from the difference map and refined with restraints. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6891 _refine_ls_number_parameters 434 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1356 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1124 _refine_ls_wR_factor_gt 0.0648 _refine_ls_goodness_of_fit_ref 0.782 _refine_ls_restrained_S_all 0.782 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V001 V 0.64440(6) 0.10431(4) 0.80555(3) 0.02142(17) Uani 1 1 d . . . Cl01 Cl 0.48280(10) 0.19945(6) 0.80729(5) 0.0328(2) Uani 1 1 d . . . O4 O 1.0692(2) 0.04327(15) 0.78297(12) 0.0272(6) Uani 1 1 d . . . O2 O 0.8187(3) -0.12414(14) 0.87062(11) 0.0249(6) Uani 1 1 d . . . O1 O 0.7485(2) -0.05716(14) 0.98814(11) 0.0245(6) Uani 1 1 d . . . O3 O 0.9378(2) -0.11135(15) 0.76173(12) 0.0258(6) Uani 1 1 d . . . O5 O 1.0824(3) 0.20631(15) 0.83062(12) 0.0291(6) Uani 1 1 d . . . N1 N 0.7994(3) 0.20049(15) 0.80778(13) 0.0164(6) Uani 1 1 d . . . N4 N 0.6013(3) 0.04882(17) 0.89498(12) 0.0171(6) Uani 1 1 d . . . N3 N 0.5340(3) 0.00596(17) 0.77346(13) 0.0191(6) Uani 1 1 d . . . N2 N 0.6687(3) 0.11105(16) 0.71229(13) 0.0173(6) Uani 1 1 d . . . C6 C 0.4928(4) 0.0186(2) 0.65303(15) 0.0205(7) Uani 1 1 d . . . C35 C 0.8719(3) 0.2438(2) 0.86121(16) 0.0207(7) Uani 1 1 d . . . C34 C 0.8026(4) 0.2832(2) 0.90533(16) 0.0228(8) Uani 1 1 d . . . H34 H 0.7056 0.2818 0.8985 0.027 Uiso 1 1 calc R . . C8 C 0.5887(4) -0.1065(2) 0.59758(19) 0.0308(9) Uani 1 1 d . . . H8A H 0.6782 -0.0803 0.6001 0.046 Uiso 1 1 calc R . . H8B H 0.5700 -0.1403 0.5586 0.046 Uiso 1 1 calc R . . H8C H 0.5887 -0.1411 0.6356 0.046 Uiso 1 1 calc R . . C9 C 0.3695(4) 0.0787(2) 0.64356(17) 0.0241(8) Uani 1 1 d . . . H9A H 0.2846 0.0460 0.6398 0.029 Uiso 1 1 calc R . . H9B H 0.3755 0.1126 0.6829 0.029 Uiso 1 1 calc R . . C7 C 0.4779(4) -0.0406(2) 0.59508(16) 0.0234(8) Uani 1 1 d . . . H7A H 0.3881 -0.0682 0.5913 0.028 Uiso 1 1 calc R . . H7B H 0.4769 -0.0078 0.5555 0.028 Uiso 1 1 calc R . . C5 C 0.6206(3) 0.0694(2) 0.65757(15) 0.0174(7) Uani 1 1 d . . . C4 C 0.6964(4) 0.0929(2) 0.61009(17) 0.0264(8) Uani 1 1 d . . . H4 H 0.6846 0.0728 0.5672 0.032 Uiso 1 1 calc R . . C20 C 0.7859(3) 0.0557(2) 1.06392(17) 0.0240(8) Uani 1 1 d . . . H20 H 0.8447 0.0227 1.0937 0.029 Uiso 1 1 calc R . . C19 C 0.7562(4) 0.1346(2) 1.08075(17) 0.0258(8) Uani 1 1 d . . . H19 H 0.7956 0.1554 1.1218 0.031 Uiso 1 1 calc R . . C21 C 0.7311(3) 0.0243(2) 1.00418(15) 0.0202(7) Uani 1 1 d . . . C2 C 0.7736(4) 0.1621(2) 0.69973(16) 0.0237(8) Uani 1 1 d . . . C32 C 1.0115(4) 0.3249(2) 0.96998(17) 0.0257(8) Uani 1 1 d . . . H32 H 1.0587 0.3531 1.0065 0.031 Uiso 1 1 calc R . . C1 C 0.8379(4) 0.2091(2) 0.75220(16) 0.0222(8) Uani 1 1 d . . . H1 H 0.9085 0.2466 0.7471 0.027 Uiso 1 1 calc R . . C13 C 0.4345(3) -0.1149(2) 0.78977(16) 0.0214(8) Uani 1 1 d . . . H13 H 0.4021 -0.1608 0.8104 0.026 Uiso 1 1 calc R . . C3 C 0.7918(4) 0.1510(2) 0.63691(17) 0.0236(8) Uani 1 1 d . . . H3 H 0.8569 0.1778 0.6160 0.028 Uiso 1 1 calc R . . C25 C 0.8089(3) -0.1478(2) 0.75972(17) 0.0221(8) Uani 1 1 d . . . H25A H 0.7927 -0.1887 0.7246 0.027 Uiso 1 1 calc R . . H25B H 0.7365 -0.1056 0.7512 0.027 Uiso 1 1 calc R . . C12 C 0.4236(4) -0.1035(2) 0.72337(17) 0.0230(8) Uani 1 1 d . . . H12 H 0.3818 -0.1395 0.6904 0.028 Uiso 1 1 calc R . . C23 C 0.8684(4) -0.1522(2) 0.93431(16) 0.0218(8) Uani 1 1 d . . . H23A H 0.9581 -0.1794 0.9360 0.026 Uiso 1 1 calc R . . H23B H 0.8038 -0.1923 0.9477 0.026 Uiso 1 1 calc R . . C15 C 0.5384(3) -0.0225(2) 0.88399(15) 0.0182(7) Uani 1 1 d . . . H15 H 0.5196 -0.0555 0.9185 0.022 Uiso 1 1 calc R . . C14 C 0.5003(4) -0.0480(2) 0.81981(16) 0.0213(8) Uani 1 1 d . . . C33 C 0.8718(4) 0.3239(2) 0.95820(18) 0.0288(9) Uani 1 1 d . . . H33 H 0.8223 0.3513 0.9866 0.035 Uiso 1 1 calc R . . C22 C 0.8824(3) -0.0801(2) 0.97805(17) 0.0218(8) Uani 1 1 d . . . H22A H 0.9403 -0.0942 1.0196 0.026 Uiso 1 1 calc R . . H22B H 0.9258 -0.0342 0.9585 0.026 Uiso 1 1 calc R . . C30 C 1.0150(3) 0.2442(2) 0.87479(16) 0.0221(8) Uani 1 1 d . . . C31 C 1.0845(4) 0.2848(2) 0.92868(17) 0.0264(8) Uani 1 1 d . . . H31 H 1.1815 0.2850 0.9372 0.032 Uiso 1 1 calc R . . C17 C 0.6164(4) 0.1525(2) 0.97784(17) 0.0267(8) Uani 1 1 d . . . H17 H 0.5574 0.1861 0.9485 0.032 Uiso 1 1 calc R . . C26 C 0.9447(4) -0.0551(2) 0.71130(17) 0.0303(9) Uani 1 1 d . . . H26A H 0.8646 -0.0181 0.7060 0.036 Uiso 1 1 calc R . . H26B H 0.9437 -0.0849 0.6704 0.036 Uiso 1 1 calc R . . C11 C 0.4871(3) -0.0277(2) 0.71486(16) 0.0203(7) Uani 1 1 d . . . C24 C 0.8045(4) -0.1882(2) 0.82264(17) 0.0266(8) Uani 1 1 d . . . H24A H 0.7167 -0.2173 0.8214 0.032 Uiso 1 1 calc R . . H24B H 0.8800 -0.2282 0.8327 0.032 Uiso 1 1 calc R . . C16 C 0.6478(3) 0.0737(2) 0.95933(15) 0.0218(8) Uani 1 1 d . . . C18 C 0.6708(4) 0.1828(2) 1.03899(18) 0.0276(8) Uani 1 1 d . . . H18 H 0.6485 0.2364 1.0513 0.033 Uiso 1 1 calc R . . C29 C 1.1831(4) 0.1445(2) 0.85548(18) 0.0299(9) Uani 1 1 d . . . H29A H 1.1535 0.1136 0.8911 0.036 Uiso 1 1 calc R . . H29B H 1.2727 0.1702 0.8716 0.036 Uiso 1 1 calc R . . C27 C 1.0742(4) -0.0059(2) 0.72729(18) 0.0307(9) Uani 1 1 d . . . H27A H 1.1538 -0.0432 0.7356 0.037 Uiso 1 1 calc R . . H27B H 1.0848 0.0296 0.6904 0.037 Uiso 1 1 calc R . . C28 C 1.1927(4) 0.0891(2) 0.79983(18) 0.0287(8) Uani 1 1 d . . . H28A H 1.2090 0.1220 0.7624 0.034 Uiso 1 1 calc R . . H28B H 1.2707 0.0511 0.8115 0.034 Uiso 1 1 calc R . . C10 C 0.3563(4) 0.1352(3) 0.58662(19) 0.0365(10) Uani 1 1 d . . . H10A H 0.4378 0.1699 0.5903 0.055 Uiso 1 1 calc R . . H10B H 0.2752 0.1697 0.5855 0.055 Uiso 1 1 calc R . . H10C H 0.3473 0.1029 0.5470 0.055 Uiso 1 1 calc R . . O100 O 0.8264(3) 0.03724(15) 0.83392(12) 0.0233(5) Uani 1 1 d D . . H101 H 0.831(5) -0.0079(16) 0.852(2) 0.078(18) Uiso 1 1 d D . . H102 H 0.899(3) 0.046(3) 0.821(2) 0.09(2) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V001 0.0238(3) 0.0231(3) 0.0173(3) -0.0001(2) 0.0035(2) -0.0061(3) Cl01 0.0304(5) 0.0325(5) 0.0355(5) -0.0008(4) 0.0051(4) -0.0022(4) O4 0.0167(12) 0.0335(15) 0.0334(15) 0.0021(12) 0.0096(11) -0.0046(11) O2 0.0391(15) 0.0173(13) 0.0186(13) 0.0028(10) 0.0062(11) -0.0012(11) O1 0.0254(13) 0.0220(13) 0.0255(14) -0.0010(10) 0.0027(11) 0.0007(11) O3 0.0241(13) 0.0266(14) 0.0289(15) 0.0020(11) 0.0105(11) 0.0003(11) O5 0.0273(14) 0.0385(16) 0.0214(13) 0.0057(12) 0.0037(11) 0.0061(12) N1 0.0175(14) 0.0085(13) 0.0222(15) 0.0001(11) 0.0008(12) -0.0039(11) N4 0.0195(15) 0.0196(15) 0.0127(13) 0.0020(11) 0.0043(11) 0.0001(12) N3 0.0167(15) 0.0190(15) 0.0221(15) 0.0019(12) 0.0048(12) -0.0015(12) N2 0.0196(15) 0.0160(14) 0.0178(15) 0.0022(11) 0.0074(12) -0.0039(11) C6 0.0260(19) 0.0194(18) 0.0153(17) -0.0054(13) 0.0009(14) -0.0004(15) C35 0.0202(18) 0.0205(18) 0.0199(18) 0.0042(14) -0.0008(14) -0.0019(14) C34 0.0193(18) 0.0231(19) 0.0245(19) 0.0031(14) -0.0005(14) -0.0007(15) C8 0.041(2) 0.025(2) 0.030(2) -0.0030(16) 0.0133(18) -0.0007(18) C9 0.0199(18) 0.030(2) 0.0218(18) 0.0022(15) 0.0013(14) 0.0024(16) C7 0.0236(19) 0.029(2) 0.0178(17) -0.0037(14) 0.0032(14) -0.0125(16) C5 0.0179(17) 0.0229(18) 0.0096(15) -0.0003(13) -0.0032(12) -0.0002(14) C4 0.0218(19) 0.038(2) 0.0204(19) 0.0020(16) 0.0053(15) -0.0017(17) C20 0.0130(17) 0.033(2) 0.0230(18) 0.0031(15) -0.0045(14) -0.0078(15) C19 0.033(2) 0.0232(19) 0.0232(19) -0.0070(15) 0.0089(16) -0.0079(16) C21 0.0246(19) 0.0213(18) 0.0148(17) -0.0020(14) 0.0042(14) -0.0078(15) C2 0.028(2) 0.0236(19) 0.0206(19) 0.0026(14) 0.0068(16) 0.0024(16) C32 0.030(2) 0.0192(19) 0.0234(19) -0.0025(15) -0.0075(15) -0.0066(16) C1 0.0224(19) 0.024(2) 0.0208(18) 0.0065(14) 0.0054(14) -0.0026(15) C13 0.0246(19) 0.0187(17) 0.0230(19) 0.0032(14) 0.0098(15) -0.0010(15) C3 0.032(2) 0.0215(19) 0.0210(19) 0.0099(14) 0.0144(16) 0.0011(16) C25 0.0194(18) 0.0235(19) 0.0237(19) 0.0017(14) 0.0045(14) 0.0054(15) C12 0.0220(18) 0.026(2) 0.0210(19) -0.0098(15) 0.0034(15) -0.0118(15) C23 0.0241(19) 0.0187(18) 0.0203(18) 0.0056(14) -0.0028(15) 0.0041(15) C15 0.0204(17) 0.0194(18) 0.0171(16) -0.0018(14) 0.0098(13) -0.0052(14) C14 0.0202(18) 0.0235(19) 0.0226(18) 0.0013(14) 0.0108(14) -0.0076(15) C33 0.030(2) 0.031(2) 0.0228(19) -0.0058(16) -0.0042(16) 0.0077(17) C22 0.0197(19) 0.0227(19) 0.0228(19) -0.0029(14) 0.0030(14) -0.0012(15) C30 0.0207(19) 0.0220(19) 0.0224(19) 0.0009(14) 0.0002(14) -0.0012(15) C31 0.0151(17) 0.034(2) 0.028(2) 0.0066(16) -0.0008(15) -0.0041(16) C17 0.038(2) 0.0219(19) 0.0207(19) 0.0010(15) 0.0065(16) -0.0032(17) C26 0.045(2) 0.026(2) 0.023(2) 0.0066(16) 0.0154(18) -0.0003(18) C11 0.0201(18) 0.0232(19) 0.0190(17) -0.0023(14) 0.0074(14) -0.0032(15) C24 0.036(2) 0.0180(18) 0.027(2) -0.0089(15) 0.0085(17) -0.0020(16) C16 0.0228(19) 0.030(2) 0.0129(16) -0.0041(14) 0.0039(14) -0.0077(16) C18 0.034(2) 0.0225(19) 0.029(2) -0.0034(16) 0.0116(17) -0.0017(17) C29 0.023(2) 0.040(2) 0.027(2) 0.0126(17) 0.0035(16) 0.0081(17) C27 0.041(2) 0.026(2) 0.029(2) -0.0021(16) 0.0173(18) 0.0068(18) C28 0.0176(19) 0.037(2) 0.033(2) 0.0042(17) 0.0083(16) 0.0026(17) C10 0.028(2) 0.049(3) 0.031(2) 0.0024(19) 0.0017(17) 0.0103(19) O100 0.0276(14) 0.0195(14) 0.0246(14) 0.0070(11) 0.0094(11) 0.0039(11) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 V001 N3 1.998(3) . ? V001 N2 2.023(3) . ? V001 O100 2.111(3) . ? V001 N1 2.195(3) . ? V001 N4 2.198(3) . ? V001 Cl01 2.2390(12) . ? O4 C28 1.429(4) . ? O4 C27 1.430(4) . ? O2 C23 1.425(4) . ? O2 C24 1.445(4) . ? O1 C21 1.391(4) . ? O1 C22 1.432(4) . ? O3 C25 1.405(4) . ? O3 C26 1.416(4) . ? O5 C30 1.382(4) . ? O5 C29 1.455(4) . ? N1 C1 1.300(4) . ? N1 C35 1.419(4) . ? N4 C15 1.323(4) . ? N4 C16 1.416(4) . ? N3 C11 1.360(4) . ? N3 C14 1.398(4) . ? N2 C5 1.354(4) . ? N2 C2 1.394(4) . ? C6 C5 1.506(4) . ? C6 C11 1.516(5) . ? C6 C7 1.545(4) . ? C6 C9 1.556(5) . ? C35 C30 1.401(5) . ? C35 C34 1.403(5) . ? C34 C33 1.377(5) . ? C34 H34 0.9500 . ? C8 C7 1.535(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.502(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C5 C4 1.404(5) . ? C4 C3 1.391(5) . ? C4 H4 0.9500 . ? C20 C19 1.381(5) . ? C20 C21 1.383(4) . ? C20 H20 0.9500 . ? C19 C18 1.364(5) . ? C19 H19 0.9500 . ? C21 C16 1.402(5) . ? C2 C3 1.378(5) . ? C2 C1 1.408(5) . ? C32 C33 1.367(5) . ? C32 C31 1.388(5) . ? C32 H32 0.9500 . ? C1 H1 0.9500 . ? C13 C14 1.372(5) . ? C13 C12 1.398(5) . ? C13 H13 0.9500 . ? C3 H3 0.9500 . ? C25 C24 1.489(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C12 C11 1.415(4) . ? C12 H12 0.9500 . ? C23 C22 1.488(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C15 C14 1.405(4) . ? C15 H15 0.9500 . ? C33 H33 0.9500 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C30 C31 1.393(5) . ? C31 H31 0.9500 . ? C17 C16 1.396(5) . ? C17 C18 1.400(5) . ? C17 H17 0.9500 . ? C26 C27 1.505(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C18 H18 0.9500 . ? C29 C28 1.498(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? O100 H101 0.827(10) . ? O100 H102 0.828(10) . ? 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 N3 V001 N2 82.19(11) . . ? N3 V001 O100 94.17(11) . . ? N2 V001 O100 93.78(10) . . ? N3 V001 N1 157.82(11) . . ? N2 V001 N1 77.47(11) . . ? O100 V001 N1 78.58(10) . . ? N3 V001 N4 77.45(11) . . ? N2 V001 N4 158.13(11) . . ? O100 V001 N4 79.93(10) . . ? N1 V001 N4 121.00(10) . . ? N3 V001 Cl01 102.13(8) . . ? N2 V001 Cl01 100.49(8) . . ? O100 V001 Cl01 159.58(8) . . ? N1 V001 Cl01 90.27(7) . . ? N4 V001 Cl01 91.59(8) . . ? C28 O4 C27 110.5(3) . . ? C23 O2 C24 113.8(3) . . ? C21 O1 C22 116.3(3) . . ? C25 O3 C26 114.4(3) . . ? C30 O5 C29 116.8(3) . . ? C1 N1 C35 118.3(3) . . ? C1 N1 V001 111.8(2) . . ? C35 N1 V001 129.4(2) . . ? C15 N4 C16 119.2(3) . . ? C15 N4 V001 111.6(2) . . ? C16 N4 V001 128.6(2) . . ? C11 N3 C14 107.1(3) . . ? C11 N3 V001 135.7(2) . . ? C14 N3 V001 117.0(2) . . ? C5 N2 C2 107.8(3) . . ? C5 N2 V001 135.8(2) . . ? C2 N2 V001 115.7(2) . . ? C5 C6 C11 112.0(3) . . ? C5 C6 C7 111.2(3) . . ? C11 C6 C7 110.8(3) . . ? C5 C6 C9 107.3(3) . . ? C11 C6 C9 106.4(3) . . ? C7 C6 C9 109.0(3) . . ? C30 C35 C34 117.2(3) . . ? C30 C35 N1 121.6(3) . . ? C34 C35 N1 121.0(3) . . ? C33 C34 C35 121.6(3) . . ? C33 C34 H34 119.2 . . ? C35 C34 H34 119.2 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C6 116.8(3) . . ? C10 C9 H9A 108.1 . . ? C6 C9 H9A 108.1 . . ? C10 C9 H9B 108.1 . . ? C6 C9 H9B 108.1 . . ? H9A C9 H9B 107.3 . . ? C8 C7 C6 116.1(3) . . ? C8 C7 H7A 108.3 . . ? C6 C7 H7A 108.3 . . ? C8 C7 H7B 108.3 . . ? C6 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? N2 C5 C4 108.4(3) . . ? N2 C5 C6 120.2(3) . . ? C4 C5 C6 130.8(3) . . ? C3 C4 C5 107.9(3) . . ? C3 C4 H4 126.0 . . ? C5 C4 H4 126.0 . . ? C19 C20 C21 120.8(3) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C18 C19 C20 120.6(3) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C20 C21 O1 122.1(3) . . ? C20 C21 C16 119.7(3) . . ? O1 C21 C16 118.1(3) . . ? C3 C2 N2 109.1(3) . . ? C3 C2 C1 135.3(3) . . ? N2 C2 C1 115.6(3) . . ? C33 C32 C31 120.1(3) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? N1 C1 C2 119.0(3) . . ? N1 C1 H1 120.5 . . ? C2 C1 H1 120.5 . . ? C14 C13 C12 107.8(3) . . ? C14 C13 H13 126.1 . . ? C12 C13 H13 126.1 . . ? C2 C3 C4 106.8(3) . . ? C2 C3 H3 126.6 . . ? C4 C3 H3 126.6 . . ? O3 C25 C24 109.0(3) . . ? O3 C25 H25A 109.9 . . ? C24 C25 H25A 109.9 . . ? O3 C25 H25B 109.9 . . ? C24 C25 H25B 109.9 . . ? H25A C25 H25B 108.3 . . ? C13 C12 C11 106.5(3) . . ? C13 C12 H12 126.8 . . ? C11 C12 H12 126.8 . . ? O2 C23 C22 108.0(3) . . ? O2 C23 H23A 110.1 . . ? C22 C23 H23A 110.1 . . ? O2 C23 H23B 110.1 . . ? C22 C23 H23B 110.1 . . ? H23A C23 H23B 108.4 . . ? N4 C15 C14 118.1(3) . . ? N4 C15 H15 120.9 . . ? C14 C15 H15 120.9 . . ? C13 C14 N3 109.4(3) . . ? C13 C14 C15 135.2(3) . . ? N3 C14 C15 115.4(3) . . ? C32 C33 C34 120.3(4) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? O1 C22 C23 107.9(3) . . ? O1 C22 H22A 110.1 . . ? C23 C22 H22A 110.1 . . ? O1 C22 H22B 110.1 . . ? C23 C22 H22B 110.1 . . ? H22A C22 H22B 108.4 . . ? O5 C30 C31 122.2(3) . . ? O5 C30 C35 116.8(3) . . ? C31 C30 C35 120.9(3) . . ? C32 C31 C30 119.8(3) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C16 C17 C18 120.9(3) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? O3 C26 C27 109.1(3) . . ? O3 C26 H26A 109.9 . . ? C27 C26 H26A 109.9 . . ? O3 C26 H26B 109.9 . . ? C27 C26 H26B 109.9 . . ? H26A C26 H26B 108.3 . . ? N3 C11 C12 109.3(3) . . ? N3 C11 C6 121.5(3) . . ? C12 C11 C6 128.9(3) . . ? O2 C24 C25 106.8(3) . . ? O2 C24 H24A 110.4 . . ? C25 C24 H24A 110.4 . . ? O2 C24 H24B 110.4 . . ? C25 C24 H24B 110.4 . . ? H24A C24 H24B 108.6 . . ? C17 C16 C21 118.5(3) . . ? C17 C16 N4 118.7(3) . . ? C21 C16 N4 122.7(3) . . ? C19 C18 C17 119.4(3) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? O5 C29 C28 105.6(3) . . ? O5 C29 H29A 110.6 . . ? C28 C29 H29A 110.6 . . ? O5 C29 H29B 110.6 . . ? C28 C29 H29B 110.6 . . ? H29A C29 H29B 108.7 . . ? O4 C27 C26 109.7(3) . . ? O4 C27 H27A 109.7 . . ? C26 C27 H27A 109.7 . . ? O4 C27 H27B 109.7 . . ? C26 C27 H27B 109.7 . . ? H27A C27 H27B 108.2 . . ? O4 C28 C29 110.2(3) . . ? O4 C28 H28A 109.6 . . ? C29 C28 H28A 109.6 . . ? O4 C28 H28B 109.6 . . ? C29 C28 H28B 109.6 . . ? H28A C28 H28B 108.1 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? V001 O100 H101 125(3) . . ? V001 O100 H102 125(3) . . ? H101 O100 H102 108.8(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 V001 N1 C1 18.4(4) . . . . ? N2 V001 N1 C1 -5.5(2) . . . . ? O100 V001 N1 C1 91.0(2) . . . . ? N4 V001 N1 C1 161.8(2) . . . . ? Cl01 V001 N1 C1 -106.2(2) . . . . ? N3 V001 N1 C35 -152.4(3) . . . . ? N2 V001 N1 C35 -176.3(3) . . . . ? O100 V001 N1 C35 -79.8(3) . . . . ? N4 V001 N1 C35 -9.0(3) . . . . ? Cl01 V001 N1 C35 83.0(3) . . . . ? N3 V001 N4 C15 5.8(2) . . . . ? N2 V001 N4 C15 -16.0(4) . . . . ? O100 V001 N4 C15 -90.8(2) . . . . ? N1 V001 N4 C15 -160.8(2) . . . . ? Cl01 V001 N4 C15 107.9(2) . . . . ? N3 V001 N4 C16 176.3(3) . . . . ? N2 V001 N4 C16 154.5(3) . . . . ? O100 V001 N4 C16 79.7(3) . . . . ? N1 V001 N4 C16 9.7(3) . . . . ? Cl01 V001 N4 C16 -81.6(3) . . . . ? N2 V001 N3 C11 -8.3(3) . . . . ? O100 V001 N3 C11 -101.6(3) . . . . ? N1 V001 N3 C11 -31.9(5) . . . . ? N4 V001 N3 C11 179.7(3) . . . . ? Cl01 V001 N3 C11 90.8(3) . . . . ? N2 V001 N3 C14 166.0(3) . . . . ? O100 V001 N3 C14 72.8(2) . . . . ? N1 V001 N3 C14 142.5(3) . . . . ? N4 V001 N3 C14 -5.9(2) . . . . ? Cl01 V001 N3 C14 -94.8(2) . . . . ? N3 V001 N2 C5 4.1(3) . . . . ? O100 V001 N2 C5 97.8(3) . . . . ? N1 V001 N2 C5 175.2(3) . . . . ? N4 V001 N2 C5 25.6(5) . . . . ? Cl01 V001 N2 C5 -96.9(3) . . . . ? N3 V001 N2 C2 -164.5(2) . . . . ? O100 V001 N2 C2 -70.8(2) . . . . ? N1 V001 N2 C2 6.6(2) . . . . ? N4 V001 N2 C2 -143.0(3) . . . . ? Cl01 V001 N2 C2 94.5(2) . . . . ? C1 N1 C35 C30 -47.3(4) . . . . ? V001 N1 C35 C30 122.9(3) . . . . ? C1 N1 C35 C34 137.4(3) . . . . ? V001 N1 C35 C34 -52.3(4) . . . . ? C30 C35 C34 C33 3.0(5) . . . . ? N1 C35 C34 C33 178.5(3) . . . . ? C5 C6 C9 C10 57.1(4) . . . . ? C11 C6 C9 C10 177.1(3) . . . . ? C7 C6 C9 C10 -63.4(4) . . . . ? C5 C6 C7 C8 64.0(4) . . . . ? C11 C6 C7 C8 -61.2(4) . . . . ? C9 C6 C7 C8 -177.9(3) . . . . ? C2 N2 C5 C4 0.9(4) . . . . ? V001 N2 C5 C4 -168.3(3) . . . . ? C2 N2 C5 C6 -170.9(3) . . . . ? V001 N2 C5 C6 19.9(5) . . . . ? C11 C6 C5 N2 -40.5(4) . . . . ? C7 C6 C5 N2 -165.0(3) . . . . ? C9 C6 C5 N2 75.9(4) . . . . ? C11 C6 C5 C4 149.9(4) . . . . ? C7 C6 C5 C4 25.4(5) . . . . ? C9 C6 C5 C4 -93.8(4) . . . . ? N2 C5 C4 C3 -0.6(4) . . . . ? C6 C5 C4 C3 170.0(3) . . . . ? C21 C20 C19 C18 0.7(5) . . . . ? C19 C20 C21 O1 -173.7(3) . . . . ? C19 C20 C21 C16 2.0(5) . . . . ? C22 O1 C21 C20 -72.0(4) . . . . ? C22 O1 C21 C16 112.2(3) . . . . ? C5 N2 C2 C3 -0.9(4) . . . . ? V001 N2 C2 C3 170.8(2) . . . . ? C5 N2 C2 C1 -178.7(3) . . . . ? V001 N2 C2 C1 -7.0(4) . . . . ? C35 N1 C1 C2 175.5(3) . . . . ? V001 N1 C1 C2 3.6(4) . . . . ? C3 C2 C1 N1 -175.2(4) . . . . ? N2 C2 C1 N1 1.9(5) . . . . ? N2 C2 C3 C4 0.5(4) . . . . ? C1 C2 C3 C4 177.7(4) . . . . ? C5 C4 C3 C2 0.1(4) . . . . ? C26 O3 C25 C24 -165.8(3) . . . . ? C14 C13 C12 C11 0.8(4) . . . . ? C24 O2 C23 C22 178.1(3) . . . . ? C16 N4 C15 C14 -176.4(3) . . . . ? V001 N4 C15 C14 -4.9(4) . . . . ? C12 C13 C14 N3 -0.9(4) . . . . ? C12 C13 C14 C15 178.3(4) . . . . ? C11 N3 C14 C13 0.7(4) . . . . ? V001 N3 C14 C13 -175.2(2) . . . . ? C11 N3 C14 C15 -178.7(3) . . . . ? V001 N3 C14 C15 5.4(4) . . . . ? N4 C15 C14 C13 -179.1(4) . . . . ? N4 C15 C14 N3 0.1(5) . . . . ? C31 C32 C33 C34 -0.1(5) . . . . ? C35 C34 C33 C32 -1.8(6) . . . . ? C21 O1 C22 C23 -154.4(3) . . . . ? O2 C23 C22 O1 75.8(3) . . . . ? C29 O5 C30 C31 56.3(4) . . . . ? C29 O5 C30 C35 -127.0(3) . . . . ? C34 C35 C30 O5 -179.1(3) . . . . ? N1 C35 C30 O5 5.5(5) . . . . ? C34 C35 C30 C31 -2.4(5) . . . . ? N1 C35 C30 C31 -177.8(3) . . . . ? C33 C32 C31 C30 0.7(5) . . . . ? O5 C30 C31 C32 177.1(3) . . . . ? C35 C30 C31 C32 0.6(5) . . . . ? C25 O3 C26 C27 166.4(3) . . . . ? C14 N3 C11 C12 -0.2(4) . . . . ? V001 N3 C11 C12 174.5(2) . . . . ? C14 N3 C11 C6 173.5(3) . . . . ? V001 N3 C11 C6 -11.8(5) . . . . ? C13 C12 C11 N3 -0.4(4) . . . . ? C13 C12 C11 C6 -173.4(3) . . . . ? C5 C6 C11 N3 37.1(4) . . . . ? C7 C6 C11 N3 161.9(3) . . . . ? C9 C6 C11 N3 -79.8(4) . . . . ? C5 C6 C11 C12 -150.5(3) . . . . ? C7 C6 C11 C12 -25.8(5) . . . . ? C9 C6 C11 C12 92.6(4) . . . . ? C23 O2 C24 C25 -157.2(3) . . . . ? O3 C25 C24 O2 63.7(4) . . . . ? C18 C17 C16 C21 2.2(5) . . . . ? C18 C17 C16 N4 -173.9(3) . . . . ? C20 C21 C16 C17 -3.4(5) . . . . ? O1 C21 C16 C17 172.5(3) . . . . ? C20 C21 C16 N4 172.5(3) . . . . ? O1 C21 C16 N4 -11.6(5) . . . . ? C15 N4 C16 C17 -131.3(3) . . . . ? V001 N4 C16 C17 58.8(4) . . . . ? C15 N4 C16 C21 52.7(4) . . . . ? V001 N4 C16 C21 -117.2(3) . . . . ? C20 C19 C18 C17 -1.9(5) . . . . ? C16 C17 C18 C19 0.4(5) . . . . ? C30 O5 C29 C28 155.0(3) . . . . ? C28 O4 C27 C26 178.7(3) . . . . ? O3 C26 C27 O4 -65.2(4) . . . . ? C27 O4 C28 C29 176.3(3) . . . . ? O5 C29 C28 O4 -68.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.534 _refine_diff_density_min -2.290 _refine_diff_density_rms 0.130 data_CrClH2OLfNMe _database_code_depnum_ccdc_archive 'CCDC 895821' #TrackingRef 'combined_CIF.cif.cif' _vrf_THETM01_CrClH2OLfNMe ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: The crystals were small and weakly diffracting, and were collected using a Cu source but only out to 1 \%A. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H39 Cl Cr N5 O3' _chemical_formula_weight 797.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.9879(10) _cell_length_b 21.2422(17) _cell_length_c 14.5019(8) _cell_angle_alpha 90.00 _cell_angle_beta 104.939(7) _cell_angle_gamma 90.00 _cell_volume 3865.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 119.98(10) _cell_measurement_reflns_used 5264 _cell_measurement_theta_min 3.1514 _cell_measurement_theta_max 51.7928 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.1180 _exptl_crystal_size_mid 0.0824 _exptl_crystal_size_min 0.0499 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1660 _exptl_absorpt_coefficient_mu 3.464 _exptl_absorpt_correction_T_min 0.784 _exptl_absorpt_correction_T_max 0.882 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details 'CrysAlisPro (Agilent Technologies, 2011)' _exptl_special_details ; Crystal small and weakly diffracting Collected on copper source but could only be collected out to 1A ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3147 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28054 _diffrn_reflns_av_R_equivalents 0.1061 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.78 _diffrn_reflns_theta_max 51.85 _reflns_number_total 4277 _reflns_number_gt 2771 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Farrugia, 1997)' _computing_publication_material mercury _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4277 _refine_ls_number_parameters 506 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1362 _refine_ls_R_factor_gt 0.0940 _refine_ls_wR_factor_ref 0.3010 _refine_ls_wR_factor_gt 0.2542 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O3 O 0.8725(4) 0.2636(3) 0.8336(4) 0.0547(16) Uani 1 1 d . . . Cr1 Cr 0.93196(11) 0.18894(6) 0.77264(9) 0.0472(6) Uani 1 1 d . . . Cl1 Cl 1.02391(19) 0.11141(10) 0.71673(15) 0.0574(7) Uani 1 1 d . . . N3 N 0.8549(6) 0.1264(3) 0.8300(4) 0.0468(18) Uani 1 1 d . . . O1 O 0.9397(5) 0.3826(3) 0.6817(4) 0.0538(16) Uani 1 1 d . . . N2 N 0.8043(5) 0.1868(3) 0.6649(5) 0.0448(18) Uani 1 1 d . . . O2 O 1.0633(5) 0.2963(3) 0.9666(4) 0.0546(16) Uani 1 1 d . . . N1 N 0.9723(5) 0.2554(3) 0.6833(5) 0.0453(18) Uani 1 1 d . . . N4 N 1.0410(6) 0.1761(3) 0.9072(5) 0.0500(19) Uani 1 1 d . . . C5 C 0.7102(7) 0.1561(4) 0.6433(6) 0.049(2) Uani 1 1 d . . . C24 C 1.1461(7) 0.2006(4) 0.9459(6) 0.051(2) Uani 1 1 d . . . N5 N 0.9062(5) 0.3944(3) 0.8721(5) 0.0507(19) Uani 1 1 d . . . C34 C 0.9188(7) 0.4422(4) 0.7193(6) 0.053(2) Uani 1 1 d . . . H34A H 0.8416 0.4511 0.6973 0.063 Uiso 1 1 calc R . . H34B H 0.9569 0.4754 0.6933 0.063 Uiso 1 1 calc R . . C6 C 0.6807(7) 0.1051(4) 0.7060(6) 0.048(2) Uani 1 1 d . . . C22 C 0.9099(8) 0.1015(4) 0.9159(6) 0.054(2) Uani 1 1 d . . . C7 C 0.6621(7) 0.0434(4) 0.6515(6) 0.053(2) Uani 1 1 d . . . C1 C 0.8976(7) 0.2629(4) 0.6026(6) 0.048(2) Uani 1 1 d . . . H1 H 0.9059 0.2921 0.5555 0.057 Uiso 1 1 calc R . . C29 C 1.1560(7) 0.2629(4) 0.9739(6) 0.052(2) Uani 1 1 d . . . C26 C 1.3369(7) 0.1885(5) 0.9900(6) 0.060(3) Uani 1 1 d . . . H26 H 1.3984 0.1630 0.9959 0.072 Uiso 1 1 calc R . . C31 C 0.9626(7) 0.3893(4) 0.9742(6) 0.052(2) Uani 1 1 d . . . H31A H 0.9194 0.3634 1.0070 0.063 Uiso 1 1 calc R . . H31B H 0.9694 0.4319 1.0031 0.063 Uiso 1 1 calc R . . C30 C 1.0711(7) 0.3607(4) 0.9904(6) 0.053(2) Uani 1 1 d . . . H30A H 1.1115 0.3828 0.9509 0.064 Uiso 1 1 calc R . . H30B H 1.1103 0.3658 1.0583 0.064 Uiso 1 1 calc R . . C2 C 0.8057(7) 0.2258(4) 0.5896(6) 0.049(2) Uani 1 1 d . . . C36 C 1.1303(8) 0.4035(5) 0.7128(6) 0.060(3) Uani 1 1 d . . . H36 H 1.1193 0.4477 0.7133 0.072 Uiso 1 1 calc R . . C19 C 0.7631(7) 0.0947(4) 0.8007(6) 0.051(2) Uani 1 1 d . . . C44 C 0.5481(9) 0.4558(5) 0.6159(8) 0.076(3) Uani 1 1 d . . . H44 H 0.5224 0.4978 0.6062 0.091 Uiso 1 1 calc R . . C38 C 1.2504(8) 0.3165(6) 0.7277(7) 0.068(3) Uani 1 1 d . . . H38 H 1.3209 0.3008 0.7378 0.082 Uiso 1 1 calc R . . C35 C 1.0449(7) 0.3629(5) 0.6987(6) 0.051(2) Uani 1 1 d . . . C28 C 1.2581(8) 0.2874(5) 1.0145(6) 0.061(3) Uani 1 1 d . . . H28 H 1.2667 0.3294 1.0377 0.073 Uiso 1 1 calc R . . C27 C 1.3465(7) 0.2490(5) 1.0201(6) 0.061(3) Uani 1 1 d . . . H27 H 1.4157 0.2658 1.0460 0.073 Uiso 1 1 calc R . . C9 C 0.6965(8) -0.0431(5) 0.5600(6) 0.063(3) Uani 1 1 d . . . H9 H 0.7412 -0.0643 0.5276 0.075 Uiso 1 1 calc R . . C8 C 0.7302(7) 0.0122(4) 0.6077(6) 0.053(2) Uani 1 1 d . . . H8 H 0.7990 0.0286 0.6105 0.064 Uiso 1 1 calc R . . C25 C 1.2355(8) 0.1638(5) 0.9502(6) 0.060(3) Uani 1 1 d . . . H25 H 1.2278 0.1220 0.9261 0.072 Uiso 1 1 calc R . . C3 C 0.7101(7) 0.2187(4) 0.5172(6) 0.058(3) Uani 1 1 d . . . H3 H 0.6902 0.2400 0.4577 0.070 Uiso 1 1 calc R . . C41 C 0.6209(8) 0.3326(6) 0.6450(8) 0.075(3) Uani 1 1 d . . . H41 H 0.6475 0.2908 0.6552 0.090 Uiso 1 1 calc R . . C12 C 0.5582(7) 0.0203(4) 0.6459(6) 0.057(2) Uani 1 1 d . . . C18 C 0.5705(7) 0.1172(4) 0.7248(6) 0.049(2) Uani 1 1 d . . . C23 C 1.0118(7) 0.1294(5) 0.9533(6) 0.056(2) Uani 1 1 d . . . H23 H 1.0578 0.1142 1.0109 0.067 Uiso 1 1 calc R . . C20 C 0.7575(8) 0.0480(4) 0.8689(6) 0.059(3) Uani 1 1 d . . . H20 H 0.7007 0.0193 0.8657 0.071 Uiso 1 1 calc R . . C40 C 1.0597(7) 0.2983(5) 0.6975(6) 0.050(2) Uani 1 1 d . . . C46 C 0.6534(8) 0.3740(5) 0.5824(7) 0.071(3) Uani 1 1 d . . . H46 H 0.7014 0.3586 0.5480 0.085 Uiso 1 1 calc R . . C39 C 1.1646(8) 0.2746(5) 0.7143(6) 0.063(3) Uani 1 1 d . . . H39 H 1.1769 0.2305 0.7165 0.075 Uiso 1 1 calc R . . C4 C 0.6511(8) 0.1735(4) 0.5518(6) 0.056(2) Uani 1 1 d . . . H4 H 0.5832 0.1575 0.5191 0.067 Uiso 1 1 calc R . . C17 C 0.5378(8) 0.1668(5) 0.7697(6) 0.063(3) Uani 1 1 d . . . H17 H 0.5849 0.2007 0.7934 0.076 Uiso 1 1 calc R . . C21 C 0.8528(7) 0.0524(4) 0.9427(6) 0.059(3) Uani 1 1 d . . . H21 H 0.8735 0.0272 0.9985 0.070 Uiso 1 1 calc R . . C14 C 0.3981(7) 0.0663(5) 0.7007(6) 0.062(3) Uani 1 1 d . . . H14 H 0.3508 0.0324 0.6774 0.074 Uiso 1 1 calc R . . C43 C 0.5137(8) 0.4171(6) 0.6765(8) 0.077(3) Uani 1 1 d . . . H43 H 0.4647 0.4326 0.7097 0.093 Uiso 1 1 calc R . . C33 C 0.9523(8) 0.4450(4) 0.8262(6) 0.059(2) Uani 1 1 d . . . H33A H 1.0309 0.4424 0.8477 0.070 Uiso 1 1 calc R . . H33B H 0.9305 0.4861 0.8472 0.070 Uiso 1 1 calc R . . C10 C 0.5972(8) -0.0680(4) 0.5589(7) 0.064(3) Uani 1 1 d . . . H10 H 0.5770 -0.1072 0.5282 0.076 Uiso 1 1 calc R . . C45 C 0.6207(9) 0.4338(5) 0.5683(7) 0.075(3) Uani 1 1 d . . . H45 H 0.6467 0.4605 0.5267 0.090 Uiso 1 1 calc R . . C32 C 0.7931(7) 0.4103(4) 0.8664(6) 0.062(3) Uani 1 1 d . . . H32A H 0.7603 0.3759 0.8938 0.094 Uiso 1 1 calc R . . H32B H 0.7543 0.4164 0.7994 0.094 Uiso 1 1 calc R . . H32C H 0.7903 0.4492 0.9021 0.094 Uiso 1 1 calc R . . C11 C 0.5275(7) -0.0377(4) 0.6006(6) 0.058(3) Uani 1 1 d . . . H11 H 0.4600 -0.0556 0.5989 0.069 Uiso 1 1 calc R . . C16 C 0.4335(9) 0.1668(5) 0.7805(7) 0.070(3) Uani 1 1 d . . . H16 H 0.4092 0.2010 0.8115 0.084 Uiso 1 1 calc R . . C42 C 0.5488(8) 0.3557(6) 0.6905(7) 0.076(3) Uani 1 1 d . . . H42 H 0.5227 0.3292 0.7322 0.091 Uiso 1 1 calc R . . C13 C 0.5023(8) 0.0659(4) 0.6901(6) 0.056(2) Uani 1 1 d . . . C37 C 1.2329(8) 0.3795(6) 0.7263(7) 0.069(3) Uani 1 1 d . . . H37 H 1.2915 0.4076 0.7347 0.083 Uiso 1 1 calc R . . C15 C 0.3659(9) 0.1167(5) 0.7456(7) 0.070(3) Uani 1 1 d . . . H15 H 0.2953 0.1173 0.7531 0.084 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O3 0.057(4) 0.063(4) 0.048(4) -0.012(3) 0.020(3) -0.006(3) Cr1 0.0436(10) 0.0594(11) 0.0334(10) -0.0010(6) 0.0005(7) -0.0002(7) Cl1 0.0586(16) 0.0684(16) 0.0400(14) -0.0030(10) 0.0034(11) 0.0063(11) N3 0.053(5) 0.062(5) 0.021(4) -0.003(3) 0.003(4) 0.000(4) O1 0.049(4) 0.065(4) 0.039(4) -0.003(3) -0.004(3) -0.003(3) N2 0.041(5) 0.054(5) 0.033(4) -0.001(3) -0.001(4) -0.002(4) O2 0.046(4) 0.063(4) 0.048(4) -0.005(3) -0.001(3) 0.006(3) N1 0.038(4) 0.066(5) 0.030(4) -0.001(3) 0.004(4) 0.005(4) N4 0.045(5) 0.060(5) 0.039(5) -0.004(4) 0.002(4) 0.000(4) C5 0.045(6) 0.060(6) 0.036(5) 0.000(4) -0.005(5) 0.002(5) C24 0.045(6) 0.072(7) 0.029(5) 0.002(4) -0.002(4) -0.006(5) N5 0.041(5) 0.063(5) 0.044(5) 0.005(4) 0.003(4) 0.004(4) C34 0.057(6) 0.046(6) 0.050(6) -0.003(4) 0.003(5) 0.007(4) C6 0.046(6) 0.055(6) 0.036(5) 0.004(4) 0.000(4) -0.002(4) C22 0.063(7) 0.062(6) 0.032(6) 0.000(4) 0.003(5) 0.001(5) C7 0.056(6) 0.056(6) 0.040(5) 0.004(4) 0.000(5) 0.001(5) C1 0.057(6) 0.053(6) 0.035(6) 0.000(4) 0.015(5) 0.000(5) C29 0.049(6) 0.068(7) 0.030(5) -0.005(4) -0.005(4) -0.006(5) C26 0.033(6) 0.094(8) 0.048(6) -0.004(5) 0.002(5) 0.004(5) C31 0.044(6) 0.073(6) 0.036(5) -0.002(4) 0.003(4) 0.001(5) C30 0.048(6) 0.053(6) 0.050(6) -0.003(4) -0.003(5) -0.001(4) C2 0.055(6) 0.049(6) 0.038(5) 0.008(4) 0.003(5) 0.004(5) C36 0.065(7) 0.077(7) 0.035(5) -0.006(5) 0.008(5) -0.018(6) C19 0.051(6) 0.066(6) 0.036(5) -0.006(5) 0.011(5) 0.001(5) C44 0.077(8) 0.079(8) 0.065(7) -0.006(6) 0.004(6) 0.013(6) C38 0.035(6) 0.098(9) 0.065(7) -0.011(6) 0.001(5) -0.014(6) C35 0.051(7) 0.069(7) 0.029(5) -0.002(4) 0.002(4) -0.012(5) C28 0.052(7) 0.075(7) 0.048(6) 0.005(5) 0.000(5) -0.004(6) C27 0.037(6) 0.081(7) 0.055(6) -0.001(5) -0.003(5) -0.011(5) C9 0.058(7) 0.075(7) 0.048(6) -0.006(5) -0.001(5) 0.014(5) C8 0.043(6) 0.072(7) 0.038(5) 0.000(5) -0.002(4) 0.002(5) C25 0.056(7) 0.081(7) 0.037(6) 0.000(5) 0.000(5) 0.012(6) C3 0.063(7) 0.064(6) 0.041(6) 0.005(5) 0.001(5) -0.001(5) C41 0.055(7) 0.098(8) 0.075(8) -0.007(6) 0.022(6) 0.004(6) C12 0.049(6) 0.060(6) 0.053(6) 0.008(5) -0.001(5) -0.004(5) C18 0.050(6) 0.055(6) 0.041(6) -0.004(4) 0.009(5) 0.001(5) C23 0.048(6) 0.077(7) 0.034(5) 0.001(5) -0.003(5) 0.006(5) C20 0.069(7) 0.072(6) 0.031(5) 0.001(5) 0.003(5) -0.020(5) C40 0.041(6) 0.072(7) 0.034(5) -0.003(4) 0.002(4) -0.008(5) C46 0.052(7) 0.091(9) 0.073(8) -0.011(6) 0.024(6) 0.006(6) C39 0.056(7) 0.076(7) 0.056(6) -0.011(5) 0.013(5) -0.001(6) C4 0.049(6) 0.070(6) 0.043(6) 0.004(5) 0.001(5) 0.000(5) C17 0.063(7) 0.077(7) 0.046(6) 0.003(5) 0.008(5) 0.003(5) C21 0.073(7) 0.065(6) 0.036(6) 0.004(5) 0.011(5) -0.001(5) C14 0.041(6) 0.088(8) 0.052(6) 0.004(5) 0.003(5) -0.004(5) C43 0.053(7) 0.095(9) 0.077(8) -0.023(7) 0.004(6) 0.015(6) C33 0.066(7) 0.058(6) 0.047(6) -0.001(5) 0.004(5) -0.004(5) C10 0.060(7) 0.059(6) 0.063(7) -0.011(5) 0.000(6) 0.000(5) C45 0.075(8) 0.074(8) 0.081(8) 0.002(6) 0.030(7) 0.013(6) C32 0.060(7) 0.078(7) 0.045(6) 0.004(5) 0.005(5) 0.006(5) C11 0.049(6) 0.065(7) 0.051(6) 0.003(5) -0.004(5) -0.002(5) C16 0.075(8) 0.083(8) 0.053(7) 0.002(5) 0.018(6) 0.015(6) C42 0.061(7) 0.104(10) 0.064(7) -0.006(6) 0.017(6) -0.008(7) C13 0.061(7) 0.062(7) 0.042(6) 0.011(5) 0.008(5) 0.007(5) C37 0.052(7) 0.088(8) 0.063(7) -0.007(6) 0.005(5) -0.026(6) C15 0.065(7) 0.085(8) 0.059(7) 0.014(6) 0.014(6) 0.024(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O3 Cr1 2.059(5) . ? Cr1 N2 1.964(7) . ? Cr1 N3 1.972(7) . ? Cr1 N1 2.073(7) . ? Cr1 N4 2.113(7) . ? Cr1 Cl1 2.301(3) . ? N3 C19 1.339(10) . ? N3 C22 1.372(10) . ? O1 C35 1.388(10) . ? O1 C34 1.431(9) . ? N2 C5 1.350(10) . ? N2 C2 1.374(10) . ? O2 C29 1.377(10) . ? O2 C30 1.409(10) . ? N1 C1 1.322(10) . ? N1 C40 1.428(10) . ? N4 C23 1.307(11) . ? N4 C24 1.433(11) . ? C5 C4 1.400(11) . ? C5 C6 1.525(11) . ? C24 C29 1.382(12) . ? C24 C25 1.387(12) . ? N5 C33 1.471(10) . ? N5 C31 1.477(10) . ? N5 C32 1.489(11) . ? C34 C33 1.500(11) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C6 C7 1.518(11) . ? C6 C19 1.524(12) . ? C6 C18 1.546(12) . ? C22 C21 1.392(12) . ? C22 C23 1.423(12) . ? C7 C8 1.383(12) . ? C7 C12 1.418(12) . ? C1 C2 1.402(11) . ? C1 H1 0.9500 . ? C29 C28 1.404(12) . ? C26 C27 1.353(12) . ? C26 C25 1.396(13) . ? C26 H26 0.9500 . ? C31 C30 1.497(11) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C2 C3 1.412(11) . ? C36 C35 1.378(12) . ? C36 C37 1.393(13) . ? C36 H36 0.9500 . ? C19 C20 1.416(11) . ? C44 C43 1.361(14) . ? C44 C45 1.385(13) . ? C44 H44 0.9500 . ? C38 C37 1.355(12) . ? C38 C39 1.400(13) . ? C38 H38 0.9500 . ? C35 C40 1.386(12) . ? C28 C27 1.394(12) . ? C28 H28 0.9500 . ? C27 H27 0.9500 . ? C9 C8 1.375(12) . ? C9 C10 1.390(13) . ? C9 H9 0.9500 . ? C8 H8 0.9500 . ? C25 H25 0.9500 . ? C3 C4 1.400(12) . ? C3 H3 0.9500 . ? C41 C42 1.368(13) . ? C41 C46 1.405(14) . ? C41 H41 0.9500 . ? C12 C11 1.406(12) . ? C12 C13 1.456(12) . ? C18 C17 1.362(12) . ? C18 C13 1.412(12) . ? C23 H23 0.9500 . ? C20 C21 1.415(12) . ? C20 H20 0.9500 . ? C40 C39 1.414(12) . ? C46 C45 1.338(13) . ? C46 H46 0.9500 . ? C39 H39 0.9500 . ? C4 H4 0.9500 . ? C17 C16 1.403(13) . ? C17 H17 0.9500 . ? C21 H21 0.9500 . ? C14 C15 1.373(13) . ? C14 C13 1.401(12) . ? C14 H14 0.9500 . ? C43 C42 1.379(14) . ? C43 H43 0.9500 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C10 C11 1.371(12) . ? C10 H10 0.9500 . ? C45 H45 0.9500 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C11 H11 0.9500 . ? C16 C15 1.391(14) . ? C16 H16 0.9500 . ? C42 H42 0.9500 . ? C37 H37 0.9500 . ? C15 H15 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cr1 N3 84.5(3) . . ? N2 Cr1 O3 91.5(2) . . ? N3 Cr1 O3 92.9(2) . . ? N2 Cr1 N1 79.4(3) . . ? N3 Cr1 N1 163.8(3) . . ? O3 Cr1 N1 85.8(2) . . ? N2 Cr1 N4 163.6(3) . . ? N3 Cr1 N4 79.4(3) . . ? O3 Cr1 N4 86.5(2) . . ? N1 Cr1 N4 116.6(3) . . ? N2 Cr1 Cl1 96.4(2) . . ? N3 Cr1 Cl1 91.9(2) . . ? O3 Cr1 Cl1 171.15(18) . . ? N1 Cr1 Cl1 91.71(19) . . ? N4 Cr1 Cl1 87.0(2) . . ? C19 N3 C22 107.9(7) . . ? C19 N3 Cr1 135.4(6) . . ? C22 N3 Cr1 116.1(6) . . ? C35 O1 C34 118.2(7) . . ? C5 N2 C2 107.7(7) . . ? C5 N2 Cr1 136.4(6) . . ? C2 N2 Cr1 115.9(6) . . ? C29 O2 C30 118.3(7) . . ? C1 N1 C40 115.2(7) . . ? C1 N1 Cr1 112.9(5) . . ? C40 N1 Cr1 131.5(6) . . ? C23 N4 C24 116.7(7) . . ? C23 N4 Cr1 110.9(6) . . ? C24 N4 Cr1 131.2(6) . . ? N2 C5 C4 109.5(8) . . ? N2 C5 C6 123.9(7) . . ? C4 C5 C6 126.3(8) . . ? C29 C24 C25 120.9(9) . . ? C29 C24 N4 118.0(8) . . ? C25 C24 N4 121.1(8) . . ? C33 N5 C31 110.6(6) . . ? C33 N5 C32 108.6(7) . . ? C31 N5 C32 107.4(6) . . ? O1 C34 C33 113.3(7) . . ? O1 C34 H34A 108.9 . . ? C33 C34 H34A 108.9 . . ? O1 C34 H34B 108.9 . . ? C33 C34 H34B 108.9 . . ? H34A C34 H34B 107.7 . . ? C7 C6 C19 108.9(7) . . ? C7 C6 C5 109.5(7) . . ? C19 C6 C5 114.4(7) . . ? C7 C6 C18 101.9(7) . . ? C19 C6 C18 109.4(7) . . ? C5 C6 C18 111.9(7) . . ? N3 C22 C21 110.6(8) . . ? N3 C22 C23 113.6(8) . . ? C21 C22 C23 135.6(9) . . ? C8 C7 C12 121.3(9) . . ? C8 C7 C6 128.2(8) . . ? C12 C7 C6 110.4(8) . . ? N1 C1 C2 117.2(8) . . ? N1 C1 H1 121.4 . . ? C2 C1 H1 121.4 . . ? O2 C29 C24 117.2(8) . . ? O2 C29 C28 123.7(8) . . ? C24 C29 C28 119.0(9) . . ? C27 C26 C25 119.2(9) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? N5 C31 C30 113.0(7) . . ? N5 C31 H31A 109.0 . . ? C30 C31 H31A 109.0 . . ? N5 C31 H31B 109.0 . . ? C30 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? O2 C30 C31 110.5(7) . . ? O2 C30 H30A 109.5 . . ? C31 C30 H30A 109.5 . . ? O2 C30 H30B 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 108.1 . . ? N2 C2 C1 114.6(8) . . ? N2 C2 C3 109.7(8) . . ? C1 C2 C3 135.7(8) . . ? C35 C36 C37 119.7(10) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? N3 C19 C20 109.4(8) . . ? N3 C19 C6 125.1(8) . . ? C20 C19 C6 125.4(8) . . ? C43 C44 C45 119.8(10) . . ? C43 C44 H44 120.1 . . ? C45 C44 H44 120.1 . . ? C37 C38 C39 120.1(10) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C36 C35 C40 120.8(9) . . ? C36 C35 O1 123.8(9) . . ? C40 C35 O1 115.3(8) . . ? C27 C28 C29 118.8(9) . . ? C27 C28 H28 120.6 . . ? C29 C28 H28 120.6 . . ? C26 C27 C28 122.1(9) . . ? C26 C27 H27 118.9 . . ? C28 C27 H27 118.9 . . ? C8 C9 C10 120.3(9) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C9 C8 C7 118.8(9) . . ? C9 C8 H8 120.6 . . ? C7 C8 H8 120.6 . . ? C24 C25 C26 119.8(9) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C4 C3 C2 105.4(8) . . ? C4 C3 H3 127.3 . . ? C2 C3 H3 127.3 . . ? C42 C41 C46 116.4(11) . . ? C42 C41 H41 121.8 . . ? C46 C41 H41 121.8 . . ? C11 C12 C7 118.8(9) . . ? C11 C12 C13 132.5(9) . . ? C7 C12 C13 108.7(8) . . ? C17 C18 C13 121.5(9) . . ? C17 C18 C6 129.0(8) . . ? C13 C18 C6 109.4(7) . . ? N4 C23 C22 119.0(8) . . ? N4 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? C21 C20 C19 106.8(8) . . ? C21 C20 H20 126.6 . . ? C19 C20 H20 126.6 . . ? C35 C40 C39 118.7(8) . . ? C35 C40 N1 121.7(8) . . ? C39 C40 N1 119.5(8) . . ? C45 C46 C41 123.8(10) . . ? C45 C46 H46 118.1 . . ? C41 C46 H46 118.1 . . ? C38 C39 C40 119.6(9) . . ? C38 C39 H39 120.2 . . ? C40 C39 H39 120.2 . . ? C3 C4 C5 107.7(8) . . ? C3 C4 H4 126.2 . . ? C5 C4 H4 126.2 . . ? C18 C17 C16 118.9(10) . . ? C18 C17 H17 120.6 . . ? C16 C17 H17 120.6 . . ? C22 C21 C20 105.2(8) . . ? C22 C21 H21 127.4 . . ? C20 C21 H21 127.4 . . ? C15 C14 C13 118.5(9) . . ? C15 C14 H14 120.8 . . ? C13 C14 H14 120.8 . . ? C44 C43 C42 121.0(10) . . ? C44 C43 H43 119.5 . . ? C42 C43 H43 119.5 . . ? N5 C33 C34 113.3(7) . . ? N5 C33 H33A 108.9 . . ? C34 C33 H33A 108.9 . . ? N5 C33 H33B 108.9 . . ? C34 C33 H33B 108.9 . . ? H33A C33 H33B 107.7 . . ? C11 C10 C9 122.2(9) . . ? C11 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? C46 C45 C44 118.3(10) . . ? C46 C45 H45 120.9 . . ? C44 C45 H45 120.9 . . ? N5 C32 H32A 109.5 . . ? N5 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N5 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C10 C11 C12 118.5(9) . . ? C10 C11 H11 120.8 . . ? C12 C11 H11 120.8 . . ? C15 C16 C17 119.8(10) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C41 C42 C43 120.6(11) . . ? C41 C42 H42 119.7 . . ? C43 C42 H42 119.7 . . ? C14 C13 C18 119.5(9) . . ? C14 C13 C12 131.1(9) . . ? C18 C13 C12 109.4(8) . . ? C38 C37 C36 121.0(9) . . ? C38 C37 H37 119.5 . . ? C36 C37 H37 119.5 . . ? C14 C15 C16 121.9(10) . . ? C14 C15 H15 119.1 . . ? C16 C15 H15 119.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Cr1 N3 C19 5.9(8) . . . . ? O3 Cr1 N3 C19 97.1(8) . . . . ? N1 Cr1 N3 C19 12.3(15) . . . . ? N4 Cr1 N3 C19 -177.0(8) . . . . ? Cl1 Cr1 N3 C19 -90.4(8) . . . . ? N2 Cr1 N3 C22 175.5(6) . . . . ? O3 Cr1 N3 C22 -93.3(6) . . . . ? N1 Cr1 N3 C22 -178.1(8) . . . . ? N4 Cr1 N3 C22 -7.4(6) . . . . ? Cl1 Cr1 N3 C22 79.3(6) . . . . ? N3 Cr1 N2 C5 -0.2(8) . . . . ? O3 Cr1 N2 C5 -93.0(8) . . . . ? N1 Cr1 N2 C5 -178.4(8) . . . . ? N4 Cr1 N2 C5 -10.3(15) . . . . ? Cl1 Cr1 N2 C5 91.1(8) . . . . ? N3 Cr1 N2 C2 179.5(6) . . . . ? O3 Cr1 N2 C2 86.8(6) . . . . ? N1 Cr1 N2 C2 1.3(6) . . . . ? N4 Cr1 N2 C2 169.4(8) . . . . ? Cl1 Cr1 N2 C2 -89.2(5) . . . . ? N2 Cr1 N1 C1 -0.5(5) . . . . ? N3 Cr1 N1 C1 -7.0(12) . . . . ? O3 Cr1 N1 C1 -92.8(5) . . . . ? N4 Cr1 N1 C1 -176.8(5) . . . . ? Cl1 Cr1 N1 C1 95.7(5) . . . . ? N2 Cr1 N1 C40 172.1(7) . . . . ? N3 Cr1 N1 C40 165.6(9) . . . . ? O3 Cr1 N1 C40 79.8(7) . . . . ? N4 Cr1 N1 C40 -4.2(8) . . . . ? Cl1 Cr1 N1 C40 -91.7(7) . . . . ? N2 Cr1 N4 C23 18.8(13) . . . . ? N3 Cr1 N4 C23 8.6(6) . . . . ? O3 Cr1 N4 C23 102.2(6) . . . . ? N1 Cr1 N4 C23 -174.3(6) . . . . ? Cl1 Cr1 N4 C23 -83.9(6) . . . . ? N2 Cr1 N4 C24 -174.8(8) . . . . ? N3 Cr1 N4 C24 175.0(8) . . . . ? O3 Cr1 N4 C24 -91.4(7) . . . . ? N1 Cr1 N4 C24 -7.9(8) . . . . ? Cl1 Cr1 N4 C24 82.5(7) . . . . ? C2 N2 C5 C4 2.1(10) . . . . ? Cr1 N2 C5 C4 -178.2(6) . . . . ? C2 N2 C5 C6 175.8(7) . . . . ? Cr1 N2 C5 C6 -4.5(13) . . . . ? C23 N4 C24 C29 -119.2(9) . . . . ? Cr1 N4 C24 C29 75.0(10) . . . . ? C23 N4 C24 C25 64.3(11) . . . . ? Cr1 N4 C24 C25 -101.5(9) . . . . ? C35 O1 C34 C33 -63.0(10) . . . . ? N2 C5 C6 C7 -117.8(9) . . . . ? C4 C5 C6 C7 54.8(11) . . . . ? N2 C5 C6 C19 4.8(12) . . . . ? C4 C5 C6 C19 177.4(8) . . . . ? N2 C5 C6 C18 130.0(8) . . . . ? C4 C5 C6 C18 -57.4(11) . . . . ? C19 N3 C22 C21 0.2(10) . . . . ? Cr1 N3 C22 C21 -172.1(6) . . . . ? C19 N3 C22 C23 177.5(7) . . . . ? Cr1 N3 C22 C23 5.1(9) . . . . ? C19 C6 C7 C8 -71.1(11) . . . . ? C5 C6 C7 C8 54.7(11) . . . . ? C18 C6 C7 C8 173.3(8) . . . . ? C19 C6 C7 C12 111.6(8) . . . . ? C5 C6 C7 C12 -122.6(8) . . . . ? C18 C6 C7 C12 -4.0(9) . . . . ? C40 N1 C1 C2 -174.2(7) . . . . ? Cr1 N1 C1 C2 -0.3(9) . . . . ? C30 O2 C29 C24 -177.0(7) . . . . ? C30 O2 C29 C28 8.0(12) . . . . ? C25 C24 C29 O2 179.5(7) . . . . ? N4 C24 C29 O2 3.0(11) . . . . ? C25 C24 C29 C28 -5.3(13) . . . . ? N4 C24 C29 C28 178.2(7) . . . . ? C33 N5 C31 C30 -73.4(9) . . . . ? C32 N5 C31 C30 168.2(7) . . . . ? C29 O2 C30 C31 177.6(7) . . . . ? N5 C31 C30 O2 -69.8(9) . . . . ? C5 N2 C2 C1 177.9(7) . . . . ? Cr1 N2 C2 C1 -1.9(9) . . . . ? C5 N2 C2 C3 -1.1(10) . . . . ? Cr1 N2 C2 C3 179.1(5) . . . . ? N1 C1 C2 N2 1.4(11) . . . . ? N1 C1 C2 C3 -179.9(9) . . . . ? C22 N3 C19 C20 0.2(9) . . . . ? Cr1 N3 C19 C20 170.4(6) . . . . ? C22 N3 C19 C6 -176.7(7) . . . . ? Cr1 N3 C19 C6 -6.5(13) . . . . ? C7 C6 C19 N3 123.1(9) . . . . ? C5 C6 C19 N3 0.1(12) . . . . ? C18 C6 C19 N3 -126.3(8) . . . . ? C7 C6 C19 C20 -53.4(11) . . . . ? C5 C6 C19 C20 -176.3(8) . . . . ? C18 C6 C19 C20 57.2(11) . . . . ? C37 C36 C35 C40 -0.2(13) . . . . ? C37 C36 C35 O1 -177.9(8) . . . . ? C34 O1 C35 C36 -27.7(11) . . . . ? C34 O1 C35 C40 154.4(7) . . . . ? O2 C29 C28 C27 178.5(8) . . . . ? C24 C29 C28 C27 3.7(13) . . . . ? C25 C26 C27 C28 1.3(14) . . . . ? C29 C28 C27 C26 -1.7(14) . . . . ? C10 C9 C8 C7 -2.2(13) . . . . ? C12 C7 C8 C9 -1.6(12) . . . . ? C6 C7 C8 C9 -178.6(8) . . . . ? C29 C24 C25 C26 4.9(13) . . . . ? N4 C24 C25 C26 -178.7(8) . . . . ? C27 C26 C25 C24 -2.9(14) . . . . ? N2 C2 C3 C4 -0.3(10) . . . . ? C1 C2 C3 C4 -179.0(9) . . . . ? C8 C7 C12 C11 4.6(13) . . . . ? C6 C7 C12 C11 -177.9(7) . . . . ? C8 C7 C12 C13 -174.4(7) . . . . ? C6 C7 C12 C13 3.1(10) . . . . ? C7 C6 C18 C17 -178.6(8) . . . . ? C19 C6 C18 C17 66.2(11) . . . . ? C5 C6 C18 C17 -61.7(11) . . . . ? C7 C6 C18 C13 3.5(9) . . . . ? C19 C6 C18 C13 -111.7(8) . . . . ? C5 C6 C18 C13 120.4(8) . . . . ? C24 N4 C23 C22 -177.3(8) . . . . ? Cr1 N4 C23 C22 -8.7(10) . . . . ? N3 C22 C23 N4 3.0(12) . . . . ? C21 C22 C23 N4 179.3(9) . . . . ? N3 C19 C20 C21 -0.5(10) . . . . ? C6 C19 C20 C21 176.4(7) . . . . ? C36 C35 C40 C39 2.1(12) . . . . ? O1 C35 C40 C39 -179.9(7) . . . . ? C36 C35 C40 N1 179.9(8) . . . . ? O1 C35 C40 N1 -2.2(11) . . . . ? C1 N1 C40 C35 58.4(10) . . . . ? Cr1 N1 C40 C35 -114.1(8) . . . . ? C1 N1 C40 C39 -123.9(8) . . . . ? Cr1 N1 C40 C39 63.6(10) . . . . ? C42 C41 C46 C45 2.3(16) . . . . ? C37 C38 C39 C40 1.2(14) . . . . ? C35 C40 C39 C38 -2.6(13) . . . . ? N1 C40 C39 C38 179.6(8) . . . . ? C2 C3 C4 C5 1.5(10) . . . . ? N2 C5 C4 C3 -2.3(10) . . . . ? C6 C5 C4 C3 -175.8(8) . . . . ? C13 C18 C17 C16 -0.8(13) . . . . ? C6 C18 C17 C16 -178.5(8) . . . . ? N3 C22 C21 C20 -0.6(10) . . . . ? C23 C22 C21 C20 -176.9(10) . . . . ? C19 C20 C21 C22 0.7(10) . . . . ? C45 C44 C43 C42 -1.0(16) . . . . ? C31 N5 C33 C34 165.2(7) . . . . ? C32 N5 C33 C34 -77.2(9) . . . . ? O1 C34 C33 N5 -54.3(10) . . . . ? C8 C9 C10 C11 3.1(14) . . . . ? C41 C46 C45 C44 -2.1(16) . . . . ? C43 C44 C45 C46 1.3(16) . . . . ? C9 C10 C11 C12 -0.1(14) . . . . ? C7 C12 C11 C10 -3.6(13) . . . . ? C13 C12 C11 C10 175.0(9) . . . . ? C18 C17 C16 C15 0.2(14) . . . . ? C46 C41 C42 C43 -1.8(15) . . . . ? C44 C43 C42 C41 1.3(16) . . . . ? C15 C14 C13 C18 -0.6(13) . . . . ? C15 C14 C13 C12 -179.4(9) . . . . ? C17 C18 C13 C14 1.0(13) . . . . ? C6 C18 C13 C14 179.1(7) . . . . ? C17 C18 C13 C12 -179.9(8) . . . . ? C6 C18 C13 C12 -1.8(9) . . . . ? C11 C12 C13 C14 -0.6(16) . . . . ? C7 C12 C13 C14 178.1(9) . . . . ? C11 C12 C13 C18 -179.5(9) . . . . ? C7 C12 C13 C18 -0.8(10) . . . . ? C39 C38 C37 C36 0.8(15) . . . . ? C35 C36 C37 C38 -1.3(14) . . . . ? C13 C14 C15 C16 0.0(14) . . . . ? C17 C16 C15 C14 0.2(15) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 51.85 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.179 _refine_diff_density_min -0.677 _refine_diff_density_rms 0.113 data_j10088a_CoH2OOHLfP _database_code_depnum_ccdc_archive 'CCDC 895822' #TrackingRef 'combined_CIF.cif.cif' _vrf_PLAT029_j10088a_CoH2OOHLfP ; PROBLEM: diffrn_measured_fraction_theta_full Low ....... 0.872 RESPONSE: Crystals poorly diffracting. We were unable to model disordered solvent satisfactorily, so the SQUEEZE routine of PLATON was used and accounted for 11 electrons in 1608 \%A3. We have not attempted to over-analyse this structure. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H38 Co N4 O8' _chemical_formula_sum 'C43 H38 Co N4 O8' _chemical_formula_weight 797.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.8243(9) _cell_length_b 24.612(3) _cell_length_c 15.1874(10) _cell_angle_alpha 90.00 _cell_angle_beta 100.065(6) _cell_angle_gamma 90.00 _cell_volume 5087.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9245 _cell_measurement_theta_min 2.9809 _cell_measurement_theta_max 29.2064 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.029 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.041 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1660 _exptl_absorpt_coefficient_mu 0.383 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.70945 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1042 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 43497 _diffrn_reflns_av_R_equivalents 0.0939 _diffrn_reflns_av_sigmaI/netI 0.1349 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 29.27 _reflns_number_total 12094 _reflns_number_gt 5264 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SUPERFLIP (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen et al., 2004)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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. Disordered solvent unable to model satisfactorily. PLATON used to SQUEEZE giving 11 electrons ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12094 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1944 _refine_ls_R_factor_gt 0.1286 _refine_ls_wR_factor_ref 0.3930 _refine_ls_wR_factor_gt 0.3741 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.131 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3516(5) 0.1834(3) 0.1974(5) 0.0569(18) Uani 1 1 d . . . H1 H 0.3445 0.1540 0.2364 0.068 Uiso 1 1 calc R . . C2 C 0.2702(5) 0.2132(3) 0.1572(5) 0.0549(18) Uani 1 1 d . . . C3 C 0.1681(5) 0.2164(3) 0.1595(5) 0.065(2) Uani 1 1 d . . . H3 H 0.1316 0.1925 0.1905 0.078 Uiso 1 1 calc R . . C4 C 0.1331(4) 0.2592(3) 0.1101(5) 0.0532(18) Uani 1 1 d . . . H4 H 0.0667 0.2712 0.0996 0.064 Uiso 1 1 calc R . . C5 C 0.2114(4) 0.2836(3) 0.0762(4) 0.0461(16) Uani 1 1 d . . . C6 C 0.2111(4) 0.3354(3) 0.0223(4) 0.0436(15) Uani 1 1 d . . . C7 C 0.1963(4) 0.3837(3) 0.0794(4) 0.0488(16) Uani 1 1 d . . . C8 C 0.2559(5) 0.4029(3) 0.1547(5) 0.0586(18) Uani 1 1 d . . . H8 H 0.3171 0.3859 0.1766 0.070 Uiso 1 1 calc R . . C9 C 0.2250(6) 0.4478(3) 0.1987(6) 0.075(2) Uani 1 1 d . . . H9 H 0.2663 0.4611 0.2509 0.090 Uiso 1 1 calc R . . C10 C 0.1384(7) 0.4731(3) 0.1698(6) 0.070(2) Uani 1 1 d . . . H10 H 0.1190 0.5033 0.2016 0.084 Uiso 1 1 calc R . . C11 C 0.0791(6) 0.4546(3) 0.0941(6) 0.065(2) Uani 1 1 d . . . H11 H 0.0187 0.4725 0.0727 0.078 Uiso 1 1 calc R . . C12 C 0.1065(4) 0.4100(3) 0.0486(5) 0.0485(16) Uani 1 1 d . . . C13 C 0.0588(4) 0.3819(3) -0.0333(5) 0.0519(17) Uani 1 1 d . . . C14 C -0.0296(5) 0.3921(3) -0.0908(5) 0.063(2) Uani 1 1 d . . . H14 H -0.0712 0.4212 -0.0801 0.076 Uiso 1 1 calc R . . C15 C -0.0543(5) 0.3586(4) -0.1632(5) 0.069(2) Uani 1 1 d . . . H15 H -0.1149 0.3646 -0.2023 0.083 Uiso 1 1 calc R . . C16 C 0.0048(5) 0.3167(4) -0.1819(5) 0.073(2) Uani 1 1 d . . . H16 H -0.0147 0.2951 -0.2338 0.087 Uiso 1 1 calc R . . C17 C 0.0928(5) 0.3060(3) -0.1252(5) 0.0555(18) Uani 1 1 d . . . H17 H 0.1336 0.2768 -0.1370 0.067 Uiso 1 1 calc R . . C18 C 0.1198(4) 0.3391(3) -0.0503(4) 0.0490(16) Uani 1 1 d . . . C19 C 0.3048(4) 0.3436(3) -0.0168(4) 0.0467(16) Uani 1 1 d . . . C20 C 0.3255(5) 0.3841(3) -0.0744(4) 0.0518(17) Uani 1 1 d . . . H20 H 0.2807 0.4108 -0.1021 0.062 Uiso 1 1 calc R . . C21 C 0.4233(5) 0.3787(3) -0.0845(5) 0.0528(17) Uani 1 1 d . . . H21 H 0.4578 0.4007 -0.1201 0.063 Uiso 1 1 calc R . . C22 C 0.4600(4) 0.3345(3) -0.0317(4) 0.0406(14) Uani 1 1 d . . . C23 C 0.5495(4) 0.3060(3) -0.0086(4) 0.0481(16) Uani 1 1 d . . . H23 H 0.6053 0.3157 -0.0338 0.058 Uiso 1 1 calc R . . C24 C 0.6394(4) 0.2321(3) 0.0622(4) 0.0468(17) Uani 1 1 d . . . C25 C 0.6249(5) 0.1770(3) 0.0579(4) 0.0577(19) Uani 1 1 d . . . H25 H 0.5599 0.1630 0.0462 0.069 Uiso 1 1 calc R . . C26 C 0.7045(6) 0.1413(4) 0.0705(5) 0.075(2) Uani 1 1 d . . . H26 H 0.6939 0.1031 0.0678 0.090 Uiso 1 1 calc R . . C27 C 0.7987(6) 0.1619(4) 0.0869(5) 0.081(3) Uani 1 1 d . . . H27 H 0.8535 0.1380 0.0957 0.097 Uiso 1 1 calc R . . C28 C 0.8125(5) 0.2171(4) 0.0905(5) 0.073(2) Uani 1 1 d . . . H28 H 0.8776 0.2312 0.1011 0.088 Uiso 1 1 calc R . . C29 C 0.7333(4) 0.2531(3) 0.0789(4) 0.0480(17) Uani 1 1 d . . . C30 C 0.8382(5) 0.3335(4) 0.0961(6) 0.080(3) Uani 1 1 d . . . H30A H 0.8808 0.3186 0.1500 0.096 Uiso 1 1 calc R . . H30B H 0.8697 0.3258 0.0437 0.096 Uiso 1 1 calc R . . C31 C 0.8275(6) 0.3906(4) 0.1057(6) 0.082(3) Uani 1 1 d . . . H31A H 0.7875 0.3980 0.1524 0.098 Uiso 1 1 calc R . . H31B H 0.8929 0.4074 0.1245 0.098 Uiso 1 1 calc R . . C32 C 0.7424(7) 0.4653(4) 0.0301(7) 0.095(3) Uani 1 1 d . . . H32A H 0.7380 0.4840 -0.0281 0.114 Uiso 1 1 calc R . . H32B H 0.7873 0.4865 0.0753 0.114 Uiso 1 1 calc R . . C33 C 0.6407(6) 0.4638(4) 0.0561(8) 0.092(3) Uani 1 1 d . . . H33A H 0.6082 0.4995 0.0442 0.110 Uiso 1 1 calc R . . H33B H 0.5995 0.4360 0.0203 0.110 Uiso 1 1 calc R . . C34 C 0.5618(7) 0.4356(5) 0.1729(8) 0.101(3) Uani 1 1 d . . . H34A H 0.5257 0.4100 0.1288 0.121 Uiso 1 1 calc R . . H34B H 0.5198 0.4679 0.1763 0.121 Uiso 1 1 calc R . . C35 C 0.5854(8) 0.4098(6) 0.2603(8) 0.122(5) Uani 1 1 d . . . H35A H 0.5250 0.4063 0.2866 0.147 Uiso 1 1 calc R . . H35B H 0.6327 0.4326 0.3006 0.147 Uiso 1 1 calc R . . C36 C 0.6589(7) 0.3283(6) 0.3332(6) 0.115(4) Uani 1 1 d . . . H36A H 0.6053 0.3286 0.3687 0.138 Uiso 1 1 calc R . . H36B H 0.7160 0.3474 0.3680 0.138 Uiso 1 1 calc R . . C37 C 0.6866(6) 0.2711(5) 0.3181(6) 0.095(3) Uani 1 1 d . . . H37A H 0.7385 0.2701 0.2806 0.114 Uiso 1 1 calc R . . H37B H 0.7122 0.2533 0.3759 0.114 Uiso 1 1 calc R . . C38 C 0.6035(5) 0.1886(5) 0.2670(5) 0.075(3) Uani 1 1 d . . . C39 C 0.6811(6) 0.1560(5) 0.3067(6) 0.087(3) Uani 1 1 d . . . H39 H 0.7385 0.1726 0.3392 0.104 Uiso 1 1 calc R . . C40 C 0.6772(7) 0.1035(6) 0.3003(7) 0.106(4) Uani 1 1 d . . . H40 H 0.7316 0.0824 0.3283 0.127 Uiso 1 1 calc R . . C41 C 0.5970(8) 0.0781(5) 0.2543(8) 0.113(4) Uani 1 1 d . . . H41 H 0.5950 0.0396 0.2515 0.136 Uiso 1 1 calc R . . C42 C 0.5158(6) 0.1088(4) 0.2102(6) 0.072(2) Uani 1 1 d . . . H42 H 0.4602 0.0913 0.1764 0.086 Uiso 1 1 calc R . . C43 C 0.5194(5) 0.1630(4) 0.2176(4) 0.059(2) Uani 1 1 d . . . O1 O 0.7425(3) 0.3078(2) 0.0844(4) 0.0710(15) Uani 1 1 d . . . O2 O 0.7814(4) 0.4135(3) 0.0237(4) 0.0845(17) Uani 1 1 d . . . O3 O 0.6510(4) 0.4513(3) 0.1467(5) 0.102(2) Uani 1 1 d . . . O4 O 0.6279(4) 0.3558(3) 0.2524(4) 0.092(2) Uani 1 1 d . . . O5 O 0.6013(4) 0.2439(3) 0.2743(4) 0.0833(19) Uani 1 1 d . . . O6 O 0.4511(3) 0.31001(18) 0.1821(3) 0.0495(11) Uani 1 1 d . . . O7 O 0.3923(3) 0.20210(18) -0.0043(3) 0.0524(11) Uani 1 1 d . . . O100 O 0.3805(7) 0.2108(5) -0.1682(5) 0.178(4) Uani 1 1 d . . . Co1 Co 0.42183(6) 0.25590(4) 0.08649(6) 0.0434(3) Uani 1 1 d . . . N1 N 0.4378(3) 0.1966(2) 0.1803(3) 0.0420(12) Uani 1 1 d . . . N2 N 0.2924(3) 0.2553(2) 0.1073(3) 0.0396(12) Uani 1 1 d . . . N3 N 0.3859(3) 0.31288(19) 0.0074(3) 0.0349(11) Uani 1 1 d . . . N4 N 0.5535(4) 0.2658(2) 0.0485(4) 0.0491(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.047(4) 0.072(5) 0.052(4) 0.024(4) 0.009(3) 0.010(3) C2 0.047(4) 0.059(5) 0.059(5) 0.015(4) 0.013(3) 0.003(3) C3 0.036(3) 0.079(5) 0.090(6) 0.026(5) 0.035(4) 0.005(3) C4 0.026(3) 0.064(5) 0.074(5) 0.016(4) 0.024(3) 0.003(3) C5 0.023(3) 0.060(4) 0.056(4) -0.002(3) 0.009(3) 0.000(3) C6 0.027(3) 0.062(4) 0.042(4) 0.007(3) 0.009(2) 0.007(3) C7 0.044(3) 0.055(4) 0.050(4) 0.006(3) 0.014(3) 0.000(3) C8 0.052(4) 0.075(5) 0.048(4) -0.005(4) 0.006(3) -0.002(3) C9 0.082(6) 0.071(6) 0.074(6) 0.000(5) 0.017(5) -0.019(5) C10 0.097(6) 0.048(5) 0.070(6) 0.001(4) 0.030(5) 0.007(4) C11 0.065(5) 0.055(5) 0.084(6) 0.021(4) 0.039(4) 0.011(4) C12 0.042(3) 0.052(4) 0.055(4) 0.010(3) 0.019(3) 0.002(3) C13 0.036(3) 0.062(4) 0.060(4) 0.016(4) 0.016(3) 0.006(3) C14 0.035(3) 0.081(5) 0.075(5) 0.021(5) 0.014(3) 0.015(3) C15 0.032(3) 0.134(8) 0.042(4) 0.012(5) 0.009(3) 0.008(4) C16 0.040(4) 0.112(7) 0.066(5) -0.011(5) 0.009(4) -0.004(4) C17 0.038(3) 0.075(5) 0.054(4) 0.002(4) 0.007(3) 0.003(3) C18 0.026(3) 0.067(4) 0.052(4) 0.012(3) 0.003(3) 0.002(3) C19 0.038(3) 0.054(4) 0.049(4) -0.004(3) 0.008(3) -0.002(3) C20 0.044(4) 0.059(4) 0.052(4) 0.008(3) 0.005(3) -0.002(3) C21 0.048(4) 0.063(4) 0.048(4) -0.002(3) 0.009(3) -0.002(3) C22 0.032(3) 0.062(4) 0.032(3) 0.002(3) 0.017(2) 0.000(3) C23 0.031(3) 0.066(5) 0.050(4) -0.006(4) 0.015(3) -0.006(3) C24 0.036(3) 0.079(5) 0.029(3) 0.006(3) 0.015(3) 0.009(3) C25 0.045(4) 0.086(6) 0.043(4) 0.006(4) 0.010(3) 0.012(4) C26 0.063(5) 0.093(6) 0.074(6) 0.012(5) 0.025(4) 0.026(4) C27 0.058(5) 0.120(8) 0.064(5) 0.021(5) 0.012(4) 0.037(5) C28 0.032(4) 0.121(8) 0.069(6) 0.018(5) 0.012(3) 0.017(4) C29 0.036(3) 0.081(5) 0.026(3) 0.006(3) 0.002(2) 0.006(3) C30 0.031(4) 0.131(8) 0.074(6) 0.028(6) -0.004(3) -0.007(4) C31 0.052(5) 0.100(7) 0.089(7) 0.002(6) -0.003(4) -0.021(4) C32 0.089(7) 0.086(7) 0.116(8) -0.003(6) 0.035(6) -0.022(5) C33 0.069(6) 0.083(7) 0.122(9) -0.026(6) 0.011(6) -0.010(5) C34 0.082(7) 0.125(9) 0.106(9) -0.032(7) 0.042(6) -0.012(6) C35 0.105(8) 0.161(12) 0.111(10) -0.078(9) 0.046(7) -0.047(8) C36 0.066(6) 0.230(15) 0.041(5) -0.039(7) -0.012(4) -0.037(8) C37 0.054(5) 0.174(11) 0.053(6) 0.005(6) -0.004(4) -0.017(6) C38 0.042(4) 0.144(9) 0.041(4) 0.015(5) 0.011(3) 0.015(5) C39 0.047(5) 0.157(10) 0.056(5) 0.019(6) 0.010(4) 0.036(6) C40 0.060(6) 0.175(12) 0.085(7) 0.068(8) 0.024(5) 0.058(7) C41 0.091(7) 0.119(9) 0.147(10) 0.069(8) 0.067(7) 0.059(7) C42 0.062(5) 0.084(6) 0.072(5) 0.032(5) 0.020(4) 0.026(4) C43 0.042(4) 0.094(6) 0.040(4) 0.025(4) 0.009(3) 0.012(4) O1 0.029(2) 0.096(4) 0.085(4) 0.007(3) 0.002(2) -0.003(2) O2 0.084(4) 0.106(5) 0.067(4) 0.012(4) 0.024(3) 0.011(3) O3 0.069(4) 0.138(6) 0.104(5) -0.034(5) 0.026(4) -0.034(4) O4 0.062(4) 0.150(6) 0.066(4) -0.035(4) 0.017(3) -0.025(4) O5 0.037(3) 0.143(6) 0.067(4) -0.008(4) 0.003(3) -0.001(3) O6 0.048(2) 0.069(3) 0.031(2) 0.003(2) 0.0050(19) 0.001(2) O7 0.049(3) 0.051(3) 0.057(3) -0.002(2) 0.007(2) 0.000(2) O100 0.154(8) 0.328(13) 0.072(5) 0.025(7) 0.073(5) 0.044(8) Co1 0.0269(4) 0.0686(7) 0.0350(5) 0.0055(4) 0.0061(3) 0.0035(4) N1 0.031(3) 0.063(3) 0.032(3) 0.011(2) 0.006(2) 0.009(2) N2 0.020(2) 0.062(3) 0.038(3) 0.006(2) 0.0079(19) 0.001(2) N3 0.023(2) 0.054(3) 0.026(2) 0.006(2) 0.0004(18) 0.0000(19) N4 0.038(3) 0.069(4) 0.040(3) 0.002(3) 0.005(2) 0.001(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.304(8) . ? C1 C2 1.393(9) . ? C1 H1 0.9500 . ? C2 N2 1.349(8) . ? C2 C3 1.421(9) . ? C3 C4 1.334(9) . ? C3 H3 0.9500 . ? C4 C5 1.413(8) . ? C4 H4 0.9500 . ? C5 N2 1.334(7) . ? C5 C6 1.514(9) . ? C6 C7 1.506(9) . ? C6 C18 1.526(8) . ? C6 C19 1.529(8) . ? C7 C8 1.371(9) . ? C7 C12 1.406(8) . ? C8 C9 1.396(10) . ? C8 H8 0.9500 . ? C9 C10 1.353(11) . ? C9 H9 0.9500 . ? C10 C11 1.367(11) . ? C10 H10 0.9500 . ? C11 C12 1.386(10) . ? C11 H11 0.9500 . ? C12 C13 1.474(10) . ? C13 C14 1.395(9) . ? C13 C18 1.401(9) . ? C14 C15 1.369(11) . ? C14 H14 0.9500 . ? C15 C16 1.376(11) . ? C15 H15 0.9500 . ? C16 C17 1.387(9) . ? C16 H16 0.9500 . ? C17 C18 1.397(9) . ? C17 H17 0.9500 . ? C19 N3 1.349(7) . ? C19 C20 1.389(9) . ? C20 C21 1.393(9) . ? C20 H20 0.9500 . ? C21 C22 1.395(9) . ? C21 H21 0.9500 . ? C22 N3 1.377(7) . ? C22 C23 1.411(8) . ? C23 N4 1.311(8) . ? C23 H23 0.9500 . ? C24 C25 1.371(10) . ? C24 C29 1.379(9) . ? C24 N4 1.434(8) . ? C25 C26 1.395(10) . ? C25 H25 0.9500 . ? C26 C27 1.378(11) . ? C26 H26 0.9500 . ? C27 C28 1.373(12) . ? C27 H27 0.9500 . ? C28 C29 1.396(10) . ? C28 H28 0.9500 . ? C29 O1 1.353(8) . ? C30 C31 1.423(12) . ? C30 O1 1.450(8) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 O2 1.413(10) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 O2 1.393(10) . ? C32 C33 1.526(11) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 O3 1.392(11) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 O3 1.415(10) . ? C34 C35 1.456(15) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 O4 1.465(14) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 O4 1.402(12) . ? C36 C37 1.486(14) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 O5 1.417(10) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 O5 1.367(11) . ? C38 C39 1.390(12) . ? C38 C43 1.417(11) . ? C39 C40 1.297(14) . ? C39 H39 0.9500 . ? C40 C41 1.355(15) . ? C40 H40 0.9500 . ? C41 C42 1.420(11) . ? C41 H41 0.9500 . ? C42 C43 1.339(11) . ? C42 H42 0.9500 . ? C43 N1 1.432(8) . ? O6 Co1 1.959(4) . ? O7 Co1 1.904(4) . ? Co1 N3 1.856(5) . ? Co1 N2 1.870(4) . ? Co1 N4 2.018(5) . ? Co1 N1 2.025(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 118.5(6) . . ? N1 C1 H1 120.8 . . ? C2 C1 H1 120.8 . . ? N2 C2 C1 113.9(6) . . ? N2 C2 C3 107.3(6) . . ? C1 C2 C3 138.4(7) . . ? C4 C3 C2 107.0(6) . . ? C4 C3 H3 126.5 . . ? C2 C3 H3 126.5 . . ? C3 C4 C5 108.4(5) . . ? C3 C4 H4 125.8 . . ? C5 C4 H4 125.8 . . ? N2 C5 C4 107.3(6) . . ? N2 C5 C6 123.7(5) . . ? C4 C5 C6 128.7(5) . . ? C7 C6 C5 110.0(5) . . ? C7 C6 C18 101.0(5) . . ? C5 C6 C18 111.4(5) . . ? C7 C6 C19 109.2(5) . . ? C5 C6 C19 113.4(5) . . ? C18 C6 C19 111.2(5) . . ? C8 C7 C12 119.1(7) . . ? C8 C7 C6 129.0(6) . . ? C12 C7 C6 111.8(6) . . ? C7 C8 C9 118.8(7) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? C10 C9 C8 122.4(8) . . ? C10 C9 H9 118.8 . . ? C8 C9 H9 118.8 . . ? C9 C10 C11 119.1(8) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C10 C11 C12 120.5(7) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C11 C12 C7 120.0(7) . . ? C11 C12 C13 132.2(7) . . ? C7 C12 C13 107.7(6) . . ? C14 C13 C18 120.7(7) . . ? C14 C13 C12 131.1(7) . . ? C18 C13 C12 108.2(5) . . ? C15 C14 C13 117.5(7) . . ? C15 C14 H14 121.2 . . ? C13 C14 H14 121.2 . . ? C14 C15 C16 122.9(7) . . ? C14 C15 H15 118.5 . . ? C16 C15 H15 118.5 . . ? C15 C16 C17 120.2(8) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C16 C17 C18 118.3(7) . . ? C16 C17 H17 120.8 . . ? C18 C17 H17 120.8 . . ? C17 C18 C13 120.3(6) . . ? C17 C18 C6 128.5(6) . . ? C13 C18 C6 111.1(6) . . ? N3 C19 C20 108.7(5) . . ? N3 C19 C6 122.7(6) . . ? C20 C19 C6 128.4(6) . . ? C19 C20 C21 108.2(6) . . ? C19 C20 H20 125.9 . . ? C21 C20 H20 125.9 . . ? C20 C21 C22 105.8(6) . . ? C20 C21 H21 127.1 . . ? C22 C21 H21 127.1 . . ? N3 C22 C21 109.0(5) . . ? N3 C22 C23 112.8(5) . . ? C21 C22 C23 138.2(6) . . ? N4 C23 C22 118.2(5) . . ? N4 C23 H23 120.9 . . ? C22 C23 H23 120.9 . . ? C25 C24 C29 120.4(6) . . ? C25 C24 N4 117.0(6) . . ? C29 C24 N4 122.7(7) . . ? C24 C25 C26 120.7(7) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C27 C26 C25 119.4(9) . . ? C27 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? C28 C27 C26 119.5(7) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C27 C28 C29 121.5(7) . . ? C27 C28 H28 119.3 . . ? C29 C28 H28 119.3 . . ? O1 C29 C24 117.4(6) . . ? O1 C29 C28 124.1(7) . . ? C24 C29 C28 118.5(8) . . ? C31 C30 O1 109.5(7) . . ? C31 C30 H30A 109.8 . . ? O1 C30 H30A 109.8 . . ? C31 C30 H30B 109.8 . . ? O1 C30 H30B 109.8 . . ? H30A C30 H30B 108.2 . . ? O2 C31 C30 110.1(8) . . ? O2 C31 H31A 109.6 . . ? C30 C31 H31A 109.6 . . ? O2 C31 H31B 109.6 . . ? C30 C31 H31B 109.6 . . ? H31A C31 H31B 108.2 . . ? O2 C32 C33 112.5(7) . . ? O2 C32 H32A 109.1 . . ? C33 C32 H32A 109.1 . . ? O2 C32 H32B 109.1 . . ? C33 C32 H32B 109.1 . . ? H32A C32 H32B 107.8 . . ? O3 C33 C32 108.7(8) . . ? O3 C33 H33A 109.9 . . ? C32 C33 H33A 109.9 . . ? O3 C33 H33B 109.9 . . ? C32 C33 H33B 109.9 . . ? H33A C33 H33B 108.3 . . ? O3 C34 C35 108.0(9) . . ? O3 C34 H34A 110.1 . . ? C35 C34 H34A 110.1 . . ? O3 C34 H34B 110.1 . . ? C35 C34 H34B 110.1 . . ? H34A C34 H34B 108.4 . . ? C34 C35 O4 110.6(9) . . ? C34 C35 H35A 109.5 . . ? O4 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? O4 C35 H35B 109.5 . . ? H35A C35 H35B 108.1 . . ? O4 C36 C37 111.8(8) . . ? O4 C36 H36A 109.3 . . ? C37 C36 H36A 109.3 . . ? O4 C36 H36B 109.3 . . ? C37 C36 H36B 109.3 . . ? H36A C36 H36B 107.9 . . ? O5 C37 C36 107.7(8) . . ? O5 C37 H37A 110.2 . . ? C36 C37 H37A 110.2 . . ? O5 C37 H37B 110.2 . . ? C36 C37 H37B 110.2 . . ? H37A C37 H37B 108.5 . . ? O5 C38 C39 124.5(9) . . ? O5 C38 C43 117.2(7) . . ? C39 C38 C43 118.3(11) . . ? C40 C39 C38 121.6(10) . . ? C40 C39 H39 119.2 . . ? C38 C39 H39 119.2 . . ? C39 C40 C41 121.1(9) . . ? C39 C40 H40 119.4 . . ? C41 C40 H40 119.4 . . ? C40 C41 C42 120.4(10) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C43 C42 C41 118.4(9) . . ? C43 C42 H42 120.8 . . ? C41 C42 H42 120.8 . . ? C42 C43 C38 120.1(7) . . ? C42 C43 N1 121.8(7) . . ? C38 C43 N1 118.0(8) . . ? C29 O1 C30 121.0(6) . . ? C32 O2 C31 115.1(8) . . ? C33 O3 C34 113.3(8) . . ? C36 O4 C35 115.7(9) . . ? C38 O5 C37 118.7(8) . . ? N3 Co1 N2 87.7(2) . . ? N3 Co1 O7 93.3(2) . . ? N2 Co1 O7 91.5(2) . . ? N3 Co1 O6 87.87(19) . . ? N2 Co1 O6 87.7(2) . . ? O7 Co1 O6 178.55(19) . . ? N3 Co1 N4 82.9(2) . . ? N2 Co1 N4 170.6(2) . . ? O7 Co1 N4 88.1(2) . . ? O6 Co1 N4 92.9(2) . . ? N3 Co1 N1 169.62(19) . . ? N2 Co1 N1 82.3(2) . . ? O7 Co1 N1 89.5(2) . . ? O6 Co1 N1 89.2(2) . . ? N4 Co1 N1 107.2(2) . . ? C1 N1 C43 117.4(5) . . ? C1 N1 Co1 109.2(4) . . ? C43 N1 Co1 132.5(4) . . ? C5 N2 C2 109.9(5) . . ? C5 N2 Co1 134.8(4) . . ? C2 N2 Co1 114.8(4) . . ? C19 N3 C22 108.2(5) . . ? C19 N3 Co1 135.7(4) . . ? C22 N3 Co1 115.8(4) . . ? C23 N4 C24 118.1(5) . . ? C23 N4 Co1 110.2(4) . . ? C24 N4 Co1 130.9(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 -3.2(10) . . . . ? N1 C1 C2 C3 -174.9(9) . . . . ? N2 C2 C3 C4 1.1(9) . . . . ? C1 C2 C3 C4 173.2(9) . . . . ? C2 C3 C4 C5 -0.1(9) . . . . ? C3 C4 C5 N2 -1.0(9) . . . . ? C3 C4 C5 C6 -175.1(7) . . . . ? N2 C5 C6 C7 -105.5(7) . . . . ? C4 C5 C6 C7 67.8(9) . . . . ? N2 C5 C6 C18 143.4(6) . . . . ? C4 C5 C6 C18 -43.4(9) . . . . ? N2 C5 C6 C19 17.1(9) . . . . ? C4 C5 C6 C19 -169.6(7) . . . . ? C5 C6 C7 C8 63.9(8) . . . . ? C18 C6 C7 C8 -178.3(7) . . . . ? C19 C6 C7 C8 -61.1(9) . . . . ? C5 C6 C7 C12 -114.3(6) . . . . ? C18 C6 C7 C12 3.4(7) . . . . ? C19 C6 C7 C12 120.6(6) . . . . ? C12 C7 C8 C9 0.4(10) . . . . ? C6 C7 C8 C9 -177.8(6) . . . . ? C7 C8 C9 C10 0.0(11) . . . . ? C8 C9 C10 C11 -0.8(12) . . . . ? C9 C10 C11 C12 1.1(11) . . . . ? C10 C11 C12 C7 -0.7(10) . . . . ? C10 C11 C12 C13 -179.6(7) . . . . ? C8 C7 C12 C11 -0.1(9) . . . . ? C6 C7 C12 C11 178.4(6) . . . . ? C8 C7 C12 C13 179.0(6) . . . . ? C6 C7 C12 C13 -2.5(7) . . . . ? C11 C12 C13 C14 0.4(12) . . . . ? C7 C12 C13 C14 -178.5(7) . . . . ? C11 C12 C13 C18 179.3(7) . . . . ? C7 C12 C13 C18 0.3(7) . . . . ? C18 C13 C14 C15 0.6(10) . . . . ? C12 C13 C14 C15 179.3(7) . . . . ? C13 C14 C15 C16 -1.3(11) . . . . ? C14 C15 C16 C17 1.5(12) . . . . ? C15 C16 C17 C18 -1.0(11) . . . . ? C16 C17 C18 C13 0.3(10) . . . . ? C16 C17 C18 C6 179.1(7) . . . . ? C14 C13 C18 C17 -0.1(10) . . . . ? C12 C13 C18 C17 -179.1(6) . . . . ? C14 C13 C18 C6 -179.1(6) . . . . ? C12 C13 C18 C6 1.9(7) . . . . ? C7 C6 C18 C17 177.9(6) . . . . ? C5 C6 C18 C17 -65.3(8) . . . . ? C19 C6 C18 C17 62.2(9) . . . . ? C7 C6 C18 C13 -3.2(7) . . . . ? C5 C6 C18 C13 113.6(6) . . . . ? C19 C6 C18 C13 -118.9(6) . . . . ? C7 C6 C19 N3 112.0(6) . . . . ? C5 C6 C19 N3 -11.1(9) . . . . ? C18 C6 C19 N3 -137.5(6) . . . . ? C7 C6 C19 C20 -62.3(8) . . . . ? C5 C6 C19 C20 174.7(6) . . . . ? C18 C6 C19 C20 48.3(9) . . . . ? N3 C19 C20 C21 -1.2(8) . . . . ? C6 C19 C20 C21 173.7(6) . . . . ? C19 C20 C21 C22 -0.2(8) . . . . ? C20 C21 C22 N3 1.5(7) . . . . ? C20 C21 C22 C23 -179.5(7) . . . . ? N3 C22 C23 N4 -3.3(8) . . . . ? C21 C22 C23 N4 177.7(7) . . . . ? C29 C24 C25 C26 0.2(10) . . . . ? N4 C24 C25 C26 -180.0(6) . . . . ? C24 C25 C26 C27 -0.4(11) . . . . ? C25 C26 C27 C28 -0.1(12) . . . . ? C26 C27 C28 C29 0.8(13) . . . . ? C25 C24 C29 O1 -178.5(6) . . . . ? N4 C24 C29 O1 1.6(9) . . . . ? C25 C24 C29 C28 0.5(10) . . . . ? N4 C24 C29 C28 -179.3(6) . . . . ? C27 C28 C29 O1 178.0(7) . . . . ? C27 C28 C29 C24 -1.0(11) . . . . ? O1 C30 C31 O2 -69.5(9) . . . . ? O2 C32 C33 O3 74.8(10) . . . . ? O3 C34 C35 O4 -72.6(10) . . . . ? O4 C36 C37 O5 -63.4(10) . . . . ? O5 C38 C39 C40 177.3(9) . . . . ? C43 C38 C39 C40 -1.0(13) . . . . ? C38 C39 C40 C41 0.1(16) . . . . ? C39 C40 C41 C42 1.4(16) . . . . ? C40 C41 C42 C43 -2.0(14) . . . . ? C41 C42 C43 C38 1.1(12) . . . . ? C41 C42 C43 N1 -175.6(7) . . . . ? O5 C38 C43 C42 -178.0(7) . . . . ? C39 C38 C43 C42 0.4(11) . . . . ? O5 C38 C43 N1 -1.2(10) . . . . ? C39 C38 C43 N1 177.2(6) . . . . ? C24 C29 O1 C30 -176.1(6) . . . . ? C28 C29 O1 C30 4.9(10) . . . . ? C31 C30 O1 C29 -176.2(7) . . . . ? C33 C32 O2 C31 -82.7(10) . . . . ? C30 C31 O2 C32 162.8(7) . . . . ? C32 C33 O3 C34 -165.1(8) . . . . ? C35 C34 O3 C33 164.6(9) . . . . ? C37 C36 O4 C35 171.3(8) . . . . ? C34 C35 O4 C36 176.5(8) . . . . ? C39 C38 O5 C37 5.9(12) . . . . ? C43 C38 O5 C37 -175.8(7) . . . . ? C36 C37 O5 C38 -168.6(8) . . . . ? C2 C1 N1 C43 -175.8(7) . . . . ? C2 C1 N1 Co1 -5.2(8) . . . . ? C42 C43 N1 C1 48.8(10) . . . . ? C38 C43 N1 C1 -128.0(7) . . . . ? C42 C43 N1 Co1 -119.2(7) . . . . ? C38 C43 N1 Co1 64.0(8) . . . . ? N3 Co1 N1 C1 23.0(14) . . . . ? N2 Co1 N1 C1 8.5(5) . . . . ? O7 Co1 N1 C1 -83.0(5) . . . . ? O6 Co1 N1 C1 96.4(5) . . . . ? N4 Co1 N1 C1 -170.9(5) . . . . ? N3 Co1 N1 C43 -168.3(10) . . . . ? N2 Co1 N1 C43 177.2(7) . . . . ? O7 Co1 N1 C43 85.7(6) . . . . ? O6 Co1 N1 C43 -94.9(6) . . . . ? N4 Co1 N1 C43 -2.2(7) . . . . ? C4 C5 N2 C2 1.7(8) . . . . ? C6 C5 N2 C2 176.2(6) . . . . ? C4 C5 N2 Co1 172.9(5) . . . . ? C6 C5 N2 Co1 -12.6(10) . . . . ? C1 C2 N2 C5 -176.0(6) . . . . ? C3 C2 N2 C5 -1.7(8) . . . . ? C1 C2 N2 Co1 10.8(8) . . . . ? C3 C2 N2 Co1 -174.9(5) . . . . ? N3 Co1 N2 C5 1.0(6) . . . . ? O7 Co1 N2 C5 -92.3(6) . . . . ? O6 Co1 N2 C5 88.9(6) . . . . ? N4 Co1 N2 C5 -5.0(18) . . . . ? N1 Co1 N2 C5 178.4(6) . . . . ? N3 Co1 N2 C2 171.9(5) . . . . ? O7 Co1 N2 C2 78.7(5) . . . . ? O6 Co1 N2 C2 -100.1(5) . . . . ? N4 Co1 N2 C2 165.9(12) . . . . ? N1 Co1 N2 C2 -10.6(5) . . . . ? C20 C19 N3 C22 2.1(7) . . . . ? C6 C19 N3 C22 -173.1(6) . . . . ? C20 C19 N3 Co1 174.5(4) . . . . ? C6 C19 N3 Co1 -0.7(9) . . . . ? C21 C22 N3 C19 -2.2(7) . . . . ? C23 C22 N3 C19 178.5(5) . . . . ? C21 C22 N3 Co1 -176.4(4) . . . . ? C23 C22 N3 Co1 4.4(7) . . . . ? N2 Co1 N3 C19 5.9(6) . . . . ? O7 Co1 N3 C19 97.2(6) . . . . ? O6 Co1 N3 C19 -81.9(6) . . . . ? N4 Co1 N3 C19 -175.1(6) . . . . ? N1 Co1 N3 C19 -8.5(15) . . . . ? N2 Co1 N3 C22 177.9(4) . . . . ? O7 Co1 N3 C22 -90.8(4) . . . . ? O6 Co1 N3 C22 90.1(4) . . . . ? N4 Co1 N3 C22 -3.1(4) . . . . ? N1 Co1 N3 C22 163.5(10) . . . . ? C22 C23 N4 C24 171.3(6) . . . . ? C22 C23 N4 Co1 0.8(7) . . . . ? C25 C24 N4 C23 -130.8(7) . . . . ? C29 C24 N4 C23 49.1(9) . . . . ? C25 C24 N4 Co1 37.4(8) . . . . ? C29 C24 N4 Co1 -142.7(5) . . . . ? N3 Co1 N4 C23 1.2(4) . . . . ? N2 Co1 N4 C23 7.3(17) . . . . ? O7 Co1 N4 C23 94.8(5) . . . . ? O6 Co1 N4 C23 -86.2(5) . . . . ? N1 Co1 N4 C23 -176.3(4) . . . . ? N3 Co1 N4 C24 -167.7(6) . . . . ? N2 Co1 N4 C24 -161.6(12) . . . . ? O7 Co1 N4 C24 -74.1(6) . . . . ? O6 Co1 N4 C24 104.8(6) . . . . ? N1 Co1 N4 C24 14.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.872 _diffrn_reflns_theta_full 29.27 _diffrn_measured_fraction_theta_full 0.872 _refine_diff_density_max 1.335 _refine_diff_density_min -1.401 _refine_diff_density_rms 0.119 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.007 0.000 0.000 804.4 5.3 2 0.020 0.500 0.500 804.3 5.5 _platon_squeeze_details ; 'Disordered solvent unable to model satisfactorily.' 'PLATON used to SQUEEZE giving 11 electrons per asymmetric unit' ; data_j12003_Co(H2O)(LfNMe) _database_code_depnum_ccdc_archive 'CCDC 895823' #TrackingRef 'combined_CIF.cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H35 Co N5 O3, C6 H6' _chemical_formula_sum 'C46 H41 Co N5 O3' _chemical_formula_weight 770.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.0941(2) _cell_length_b 17.0962(2) _cell_length_c 14.9472(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.537(2) _cell_angle_gamma 90.00 _cell_volume 3733.67(8) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 16725 _cell_measurement_theta_min 2.9298 _cell_measurement_theta_max 26.6724 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.6016 _exptl_crystal_size_mid 0.4388 _exptl_crystal_size_min 0.2147 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.371 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1612 _exptl_absorpt_coefficient_mu 0.510 _exptl_absorpt_correction_T_min 0.88671 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1042 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41617 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0186 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 26.73 _reflns_number_total 7918 _reflns_number_gt 6915 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+2.8056P] 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 7918 _refine_ls_number_parameters 503 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0420 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0941 _refine_ls_wR_factor_gt 0.0896 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.37061(11) 0.22368(9) 0.11415(11) 0.0197(3) Uani 1 1 d . . . C2 C 0.34386(12) 0.24883(10) 0.19284(12) 0.0245(4) Uani 1 1 d . . . H2 H 0.2892 0.2349 0.2094 0.029 Uiso 1 1 calc R . . C3 C 0.41275(12) 0.29821(11) 0.24230(12) 0.0258(4) Uani 1 1 d . . . H3 H 0.4141 0.3244 0.2987 0.031 Uiso 1 1 calc R . . C4 C 0.47922(12) 0.30134(10) 0.19205(11) 0.0215(3) Uani 1 1 d . . . C5 C 0.56675(12) 0.33541(10) 0.20024(12) 0.0236(3) Uani 1 1 d . . . H5 H 0.5924 0.3707 0.2489 0.028 Uiso 1 1 calc R . . C6 C 0.69654(12) 0.35450(10) 0.14312(12) 0.0254(4) Uani 1 1 d . . . C7 C 0.77759(14) 0.32221(12) 0.19433(15) 0.0358(4) Uani 1 1 d . . . H7 H 0.7760 0.2747 0.2269 0.043 Uiso 1 1 calc R . . C8 C 0.86137(14) 0.35810(13) 0.19897(15) 0.0396(5) Uani 1 1 d . . . H8 H 0.9164 0.3355 0.2347 0.048 Uiso 1 1 calc R . . C9 C 0.86377(13) 0.42636(13) 0.15157(14) 0.0365(5) Uani 1 1 d . . . H9 H 0.9209 0.4508 0.1541 0.044 Uiso 1 1 calc R . . C10 C 0.78362(13) 0.46008(12) 0.09996(13) 0.0312(4) Uani 1 1 d . . . H10 H 0.7861 0.5077 0.0679 0.037 Uiso 1 1 calc R . . C11 C 0.69956(12) 0.42456(10) 0.09495(12) 0.0248(4) Uani 1 1 d . . . C12 C 0.61436(14) 0.52133(11) -0.01096(14) 0.0320(4) Uani 1 1 d . . . H12A H 0.6562 0.5619 0.0233 0.038 Uiso 1 1 calc R . . H12B H 0.5517 0.5433 -0.0272 0.038 Uiso 1 1 calc R . . C13 C 0.64200(13) 0.50158(11) -0.09903(14) 0.0308(4) Uani 1 1 d . . . H13A H 0.6290 0.5470 -0.1414 0.037 Uiso 1 1 calc R . . H13B H 0.7087 0.4916 -0.0841 0.037 Uiso 1 1 calc R . . C14 C 0.50096(14) 0.45326(13) -0.19909(14) 0.0369(5) Uani 1 1 d . . . H14A H 0.4649 0.4717 -0.1571 0.055 Uiso 1 1 calc R . . H14B H 0.4716 0.4070 -0.2325 0.055 Uiso 1 1 calc R . . H14C H 0.5045 0.4947 -0.2434 0.055 Uiso 1 1 calc R . . C15 C 0.64560(15) 0.39386(12) -0.20365(13) 0.0339(4) Uani 1 1 d . . . H15A H 0.6649 0.4332 -0.2435 0.041 Uiso 1 1 calc R . . H15B H 0.6057 0.3554 -0.2443 0.041 Uiso 1 1 calc R . . C16 C 0.72922(14) 0.35238(11) -0.14640(14) 0.0323(4) Uani 1 1 d . . . H16A H 0.7669 0.3322 -0.1868 0.039 Uiso 1 1 calc R . . H16B H 0.7669 0.3891 -0.1013 0.039 Uiso 1 1 calc R . . C17 C 0.76423(13) 0.25039(11) -0.03461(14) 0.0286(4) Uani 1 1 d . . . C18 C 0.85765(13) 0.26436(12) -0.01664(16) 0.0362(5) Uani 1 1 d . . . H18 H 0.8800 0.3041 -0.0496 0.043 Uiso 1 1 calc R . . C19 C 0.91846(14) 0.22024(13) 0.04942(17) 0.0424(5) Uani 1 1 d . . . H19 H 0.9822 0.2308 0.0622 0.051 Uiso 1 1 calc R . . C20 C 0.88725(14) 0.16140(14) 0.09648(17) 0.0439(5) Uani 1 1 d . . . H20 H 0.9292 0.1306 0.1405 0.053 Uiso 1 1 calc R . . C21 C 0.79344(14) 0.14737(12) 0.07898(15) 0.0361(5) Uani 1 1 d . . . H21 H 0.7717 0.1069 0.1114 0.043 Uiso 1 1 calc R . . C22 C 0.73170(12) 0.19188(11) 0.01480(13) 0.0266(4) Uani 1 1 d . . . C23 C 0.60127(12) 0.11624(10) -0.04608(12) 0.0232(3) Uani 1 1 d . . . H23 H 0.6379 0.0825 -0.0724 0.028 Uiso 1 1 calc R . . C24 C 0.50749(12) 0.10036(10) -0.05468(11) 0.0215(3) Uani 1 1 d . . . C25 C 0.44431(12) 0.04152(10) -0.09105(12) 0.0251(4) Uani 1 1 d . . . H25 H 0.4539 -0.0024 -0.1264 0.030 Uiso 1 1 calc R . . C26 C 0.36442(12) 0.06032(10) -0.06507(12) 0.0242(4) Uani 1 1 d . . . H26 H 0.3087 0.0317 -0.0802 0.029 Uiso 1 1 calc R . . C27 C 0.38149(11) 0.12918(9) -0.01257(11) 0.0196(3) Uani 1 1 d . . . C28 C 0.31827(11) 0.17301(10) 0.03467(11) 0.0196(3) Uani 1 1 d . . . C29 C 0.25398(11) 0.11642(10) 0.06666(12) 0.0223(3) Uani 1 1 d . . . C30 C 0.27699(13) 0.05670(11) 0.13065(13) 0.0274(4) Uani 1 1 d . . . H30 H 0.3393 0.0470 0.1609 0.033 Uiso 1 1 calc R . . C31 C 0.20772(14) 0.01091(12) 0.15024(14) 0.0354(4) Uani 1 1 d . . . H31 H 0.2227 -0.0301 0.1944 0.043 Uiso 1 1 calc R . . C32 C 0.11684(15) 0.02522(13) 0.10520(16) 0.0415(5) Uani 1 1 d . . . H32 H 0.0701 -0.0063 0.1189 0.050 Uiso 1 1 calc R . . C33 C 0.09352(13) 0.08456(13) 0.04084(15) 0.0377(5) Uani 1 1 d . . . H33 H 0.0313 0.0937 0.0100 0.045 Uiso 1 1 calc R . . C34 C 0.16266(12) 0.13099(11) 0.02174(13) 0.0267(4) Uani 1 1 d . . . C35 C 0.15936(12) 0.19760(11) -0.04152(12) 0.0277(4) Uani 1 1 d . . . C36 C 0.08535(14) 0.23462(14) -0.10139(15) 0.0389(5) Uani 1 1 d . . . H36 H 0.0244 0.2181 -0.1054 0.047 Uiso 1 1 calc R . . C37 C 0.10308(16) 0.29614(14) -0.15497(15) 0.0438(5) Uani 1 1 d . . . H37 H 0.0535 0.3220 -0.1961 0.053 Uiso 1 1 calc R . . C38 C 0.19204(16) 0.32057(12) -0.14960(14) 0.0384(5) Uani 1 1 d . . . H38 H 0.2025 0.3627 -0.1871 0.046 Uiso 1 1 calc R . . C39 C 0.26612(14) 0.28390(11) -0.08978(13) 0.0295(4) Uani 1 1 d . . . H39 H 0.3270 0.3004 -0.0861 0.035 Uiso 1 1 calc R . . C40 C 0.24872(12) 0.22264(10) -0.03579(11) 0.0225(3) Uani 1 1 d . . . N1 N 0.45176(10) 0.25580(8) 0.11414(10) 0.0208(3) Uani 1 1 d . . . N2 N 0.61076(10) 0.31646(8) 0.13849(10) 0.0238(3) Uani 1 1 d . . . N3 N 0.63549(10) 0.17917(8) -0.00051(10) 0.0235(3) Uani 1 1 d . . . N4 N 0.46725(9) 0.15343(8) -0.00782(9) 0.0196(3) Uani 1 1 d . . . N5 N 0.59341(10) 0.43290(9) -0.14569(11) 0.0277(3) Uani 1 1 d . . . O1 O 0.61665(8) 0.45423(8) 0.04815(9) 0.0289(3) Uani 1 1 d . . . O2 O 0.69861(9) 0.28917(8) -0.09918(10) 0.0328(3) Uani 1 1 d . . . O3 O 0.50444(9) 0.31385(7) -0.06547(9) 0.0271(3) Uani 1 1 d D . . Co1 Co 0.542648(15) 0.235686(13) 0.051033(16) 0.02039(7) Uani 1 1 d . . . H47 H 0.4964(14) 0.2849(10) -0.1112(10) 0.024 Uiso 1 1 d D . . H48 H 0.5460(10) 0.3431(10) -0.0700(14) 0.024 Uiso 1 1 d D . . C41 C 0.14379(18) 0.12702(17) 0.6348(2) 0.0577(7) Uani 1 1 d . . . H41 H 0.1585 0.1772 0.6153 0.069 Uiso 1 1 calc R . . C42 C 0.11180(16) 0.07020(17) 0.57108(17) 0.0513(6) Uani 1 1 d . . . H42 H 0.1038 0.0810 0.5072 0.062 Uiso 1 1 calc R . . C43 C 0.09125(16) -0.00205(16) 0.59863(18) 0.0520(6) Uani 1 1 d . . . H43 H 0.0699 -0.0417 0.5539 0.062 Uiso 1 1 calc R . . C44 C 0.10133(16) -0.01782(15) 0.6911(2) 0.0529(6) Uani 1 1 d . . . H44 H 0.0869 -0.0682 0.7102 0.063 Uiso 1 1 calc R . . C45 C 0.13256(17) 0.04020(17) 0.75593(17) 0.0531(6) Uani 1 1 d . . . H45 H 0.1384 0.0303 0.8197 0.064 Uiso 1 1 calc R . . C46 C 0.1549(2) 0.11203(17) 0.72747(19) 0.0585(7) Uani 1 1 d . . . H46 H 0.1782 0.1516 0.7718 0.070 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0187(8) 0.0193(8) 0.0203(8) 0.0005(6) 0.0036(6) 0.0004(6) C2 0.0217(8) 0.0305(9) 0.0223(8) -0.0018(7) 0.0072(7) -0.0009(7) C3 0.0293(9) 0.0272(9) 0.0213(8) -0.0041(7) 0.0072(7) -0.0014(7) C4 0.0243(8) 0.0194(8) 0.0197(8) -0.0025(6) 0.0035(6) -0.0012(6) C5 0.0260(9) 0.0212(8) 0.0215(8) -0.0030(6) 0.0023(7) -0.0030(7) C6 0.0216(8) 0.0274(9) 0.0265(9) -0.0047(7) 0.0046(7) -0.0052(7) C7 0.0304(10) 0.0341(10) 0.0382(11) 0.0043(9) 0.0000(8) -0.0029(8) C8 0.0228(9) 0.0494(13) 0.0415(12) 0.0004(10) -0.0015(8) 0.0000(9) C9 0.0227(9) 0.0497(12) 0.0370(11) -0.0071(9) 0.0073(8) -0.0109(8) C10 0.0292(10) 0.0332(10) 0.0329(10) -0.0030(8) 0.0105(8) -0.0094(8) C11 0.0222(8) 0.0280(9) 0.0252(9) -0.0054(7) 0.0080(7) -0.0028(7) C12 0.0323(10) 0.0241(9) 0.0405(11) 0.0024(8) 0.0109(8) 0.0016(7) C13 0.0306(10) 0.0254(9) 0.0372(10) 0.0062(8) 0.0099(8) -0.0002(7) C14 0.0316(10) 0.0452(12) 0.0321(10) 0.0116(9) 0.0046(8) 0.0065(9) C15 0.0412(11) 0.0349(10) 0.0278(10) 0.0061(8) 0.0126(8) 0.0029(8) C16 0.0342(10) 0.0291(10) 0.0391(11) 0.0053(8) 0.0192(9) 0.0019(8) C17 0.0253(9) 0.0263(9) 0.0366(10) 0.0012(7) 0.0123(8) 0.0031(7) C18 0.0265(10) 0.0340(10) 0.0514(13) 0.0052(9) 0.0162(9) 0.0001(8) C19 0.0193(9) 0.0477(13) 0.0597(14) 0.0036(11) 0.0091(9) 0.0023(8) C20 0.0257(10) 0.0505(13) 0.0534(14) 0.0128(11) 0.0060(9) 0.0098(9) C21 0.0287(10) 0.0365(11) 0.0441(12) 0.0098(9) 0.0113(9) 0.0047(8) C22 0.0210(8) 0.0273(9) 0.0334(10) -0.0004(7) 0.0103(7) 0.0024(7) C23 0.0274(9) 0.0225(8) 0.0219(8) 0.0023(7) 0.0101(7) 0.0055(7) C24 0.0261(9) 0.0195(8) 0.0194(8) 0.0009(6) 0.0067(7) 0.0030(6) C25 0.0325(9) 0.0214(8) 0.0205(8) -0.0034(7) 0.0051(7) 0.0006(7) C26 0.0255(9) 0.0217(8) 0.0234(8) -0.0023(7) 0.0020(7) -0.0034(7) C27 0.0198(8) 0.0200(8) 0.0178(8) 0.0013(6) 0.0025(6) 0.0004(6) C28 0.0174(8) 0.0212(8) 0.0196(8) -0.0011(6) 0.0036(6) -0.0012(6) C29 0.0204(8) 0.0243(8) 0.0227(8) -0.0050(7) 0.0065(7) -0.0038(6) C30 0.0255(9) 0.0283(9) 0.0277(9) -0.0004(7) 0.0056(7) -0.0031(7) C31 0.0410(11) 0.0317(10) 0.0358(11) 0.0024(8) 0.0137(9) -0.0074(8) C32 0.0359(11) 0.0426(12) 0.0507(13) -0.0028(10) 0.0196(10) -0.0162(9) C33 0.0199(9) 0.0465(12) 0.0463(12) -0.0063(10) 0.0078(8) -0.0075(8) C34 0.0204(8) 0.0315(9) 0.0276(9) -0.0056(7) 0.0049(7) -0.0012(7) C35 0.0237(9) 0.0331(10) 0.0245(9) -0.0056(7) 0.0026(7) 0.0034(7) C36 0.0243(10) 0.0526(13) 0.0351(11) -0.0018(9) -0.0013(8) 0.0097(9) C37 0.0427(12) 0.0486(13) 0.0334(11) 0.0018(10) -0.0029(9) 0.0218(10) C38 0.0544(13) 0.0292(10) 0.0301(10) 0.0034(8) 0.0080(9) 0.0124(9) C39 0.0370(10) 0.0250(9) 0.0262(9) -0.0013(7) 0.0073(8) 0.0028(8) C40 0.0243(8) 0.0229(8) 0.0194(8) -0.0050(6) 0.0035(7) 0.0023(7) N1 0.0206(7) 0.0211(7) 0.0211(7) -0.0037(5) 0.0059(6) -0.0029(5) N2 0.0226(7) 0.0242(7) 0.0235(7) -0.0007(6) 0.0035(6) -0.0050(6) N3 0.0205(7) 0.0230(7) 0.0283(8) 0.0025(6) 0.0087(6) 0.0014(6) N4 0.0207(7) 0.0191(7) 0.0192(7) -0.0012(5) 0.0055(5) 0.0002(5) N5 0.0254(8) 0.0292(8) 0.0278(8) 0.0037(6) 0.0054(6) 0.0016(6) O1 0.0237(6) 0.0308(7) 0.0327(7) 0.0041(5) 0.0079(5) -0.0009(5) O2 0.0251(7) 0.0318(7) 0.0426(8) 0.0117(6) 0.0106(6) 0.0007(5) O3 0.0345(7) 0.0230(6) 0.0250(6) 0.0007(5) 0.0095(6) -0.0044(5) Co1 0.01875(12) 0.02052(12) 0.02231(12) -0.00229(9) 0.00589(9) -0.00236(8) C41 0.0504(15) 0.0562(16) 0.0641(17) 0.0041(13) 0.0095(13) -0.0077(12) C42 0.0375(12) 0.0754(18) 0.0405(12) -0.0020(12) 0.0088(10) 0.0117(12) C43 0.0374(12) 0.0564(15) 0.0539(15) -0.0201(12) -0.0042(10) 0.0139(11) C44 0.0346(12) 0.0431(13) 0.0766(18) 0.0100(12) 0.0058(12) 0.0066(10) C45 0.0459(14) 0.0718(18) 0.0392(13) 0.0031(12) 0.0061(11) 0.0115(12) C46 0.0620(17) 0.0570(16) 0.0501(15) -0.0172(12) 0.0022(12) -0.0044(13) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.342(2) . ? C1 C2 1.403(2) . ? C1 C28 1.521(2) . ? C2 C3 1.398(2) . ? C2 H2 0.9500 . ? C3 C4 1.397(2) . ? C3 H3 0.9500 . ? C4 N1 1.375(2) . ? C4 C5 1.421(2) . ? C5 N2 1.306(2) . ? C5 H5 0.9500 . ? C6 C7 1.385(3) . ? C6 C11 1.404(3) . ? C6 N2 1.435(2) . ? C7 C8 1.392(3) . ? C7 H7 0.9500 . ? C8 C9 1.370(3) . ? C8 H8 0.9500 . ? C9 C10 1.387(3) . ? C9 H9 0.9500 . ? C10 C11 1.391(2) . ? C10 H10 0.9500 . ? C11 O1 1.369(2) . ? C12 O1 1.443(2) . ? C12 C13 1.515(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N5 1.465(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N5 1.465(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 N5 1.469(2) . ? C15 C16 1.512(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O2 1.429(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 O2 1.368(2) . ? C17 C18 1.388(3) . ? C17 C22 1.403(3) . ? C18 C19 1.390(3) . ? C18 H18 0.9500 . ? C19 C20 1.377(3) . ? C19 H19 0.9500 . ? C20 C21 1.395(3) . ? C20 H20 0.9500 . ? C21 C22 1.385(3) . ? C21 H21 0.9500 . ? C22 N3 1.429(2) . ? C23 N3 1.308(2) . ? C23 C24 1.415(2) . ? C23 H23 0.9500 . ? C24 N4 1.377(2) . ? C24 C25 1.399(2) . ? C25 C26 1.394(3) . ? C25 H25 0.9500 . ? C26 C27 1.402(2) . ? C26 H26 0.9500 . ? C27 N4 1.344(2) . ? C27 C28 1.520(2) . ? C28 C29 1.529(2) . ? C28 C40 1.541(2) . ? C29 C30 1.383(3) . ? C29 C34 1.396(2) . ? C30 C31 1.395(3) . ? C30 H30 0.9500 . ? C31 C32 1.390(3) . ? C31 H31 0.9500 . ? C32 C33 1.382(3) . ? C32 H32 0.9500 . ? C33 C34 1.397(3) . ? C33 H33 0.9500 . ? C34 C35 1.473(3) . ? C35 C36 1.395(3) . ? C35 C40 1.397(3) . ? C36 C37 1.388(3) . ? C36 H36 0.9500 . ? C37 C38 1.389(3) . ? C37 H37 0.9500 . ? C38 C39 1.393(3) . ? C38 H38 0.9500 . ? C39 C40 1.387(3) . ? C39 H39 0.9500 . ? N1 Co1 1.8814(14) . ? N2 Co1 1.9995(14) . ? N3 Co1 2.0082(14) . ? N4 Co1 1.8826(14) . ? O3 Co1 2.1556(13) . ? O3 H47 0.829(9) . ? O3 H48 0.818(9) . ? C41 C42 1.361(4) . ? C41 C46 1.377(4) . ? C41 H41 0.9500 . ? C42 C43 1.362(4) . ? C42 H42 0.9500 . ? C43 C44 1.379(4) . ? C43 H43 0.9500 . ? C44 C45 1.384(4) . ? C44 H44 0.9500 . ? C45 C46 1.369(4) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 109.22(15) . . ? N1 C1 C28 121.86(14) . . ? C2 C1 C28 128.80(15) . . ? C3 C2 C1 107.22(15) . . ? C3 C2 H2 126.4 . . ? C1 C2 H2 126.4 . . ? C4 C3 C2 106.14(15) . . ? C4 C3 H3 126.9 . . ? C2 C3 H3 126.9 . . ? N1 C4 C3 109.21(15) . . ? N1 C4 C5 112.41(15) . . ? C3 C4 C5 138.34(16) . . ? N2 C5 C4 117.66(15) . . ? N2 C5 H5 121.2 . . ? C4 C5 H5 121.2 . . ? C7 C6 C11 119.06(17) . . ? C7 C6 N2 120.48(17) . . ? C11 C6 N2 120.46(16) . . ? C6 C7 C8 121.16(19) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C9 C8 C7 119.44(19) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C8 C9 C10 120.60(18) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C9 C10 C11 120.33(18) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? O1 C11 C10 124.76(17) . . ? O1 C11 C6 115.78(15) . . ? C10 C11 C6 119.42(17) . . ? O1 C12 C13 112.66(15) . . ? O1 C12 H12A 109.1 . . ? C13 C12 H12A 109.1 . . ? O1 C12 H12B 109.1 . . ? C13 C12 H12B 109.1 . . ? H12A C12 H12B 107.8 . . ? N5 C13 C12 112.21(15) . . ? N5 C13 H13A 109.2 . . ? C12 C13 H13A 109.2 . . ? N5 C13 H13B 109.2 . . ? C12 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? N5 C14 H14A 109.5 . . ? N5 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N5 C15 C16 111.98(16) . . ? N5 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? N5 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? O2 C16 C15 107.86(16) . . ? O2 C16 H16A 110.1 . . ? C15 C16 H16A 110.1 . . ? O2 C16 H16B 110.1 . . ? C15 C16 H16B 110.1 . . ? H16A C16 H16B 108.4 . . ? O2 C17 C18 124.99(17) . . ? O2 C17 C22 115.45(16) . . ? C18 C17 C22 119.56(18) . . ? C17 C18 C19 120.12(19) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C20 C19 C18 120.65(19) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 119.4(2) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? C22 C21 C20 120.68(19) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C17 119.51(17) . . ? C21 C22 N3 120.49(17) . . ? C17 C22 N3 120.00(16) . . ? N3 C23 C24 117.40(15) . . ? N3 C23 H23 121.3 . . ? C24 C23 H23 121.3 . . ? N4 C24 C25 109.07(15) . . ? N4 C24 C23 112.72(15) . . ? C25 C24 C23 137.91(16) . . ? C26 C25 C24 106.20(15) . . ? C26 C25 H25 126.9 . . ? C24 C25 H25 126.9 . . ? C25 C26 C27 107.41(15) . . ? C25 C26 H26 126.3 . . ? C27 C26 H26 126.3 . . ? N4 C27 C26 109.13(15) . . ? N4 C27 C28 122.15(14) . . ? C26 C27 C28 128.71(15) . . ? C27 C28 C1 112.33(13) . . ? C27 C28 C29 110.79(13) . . ? C1 C28 C29 111.22(13) . . ? C27 C28 C40 110.69(13) . . ? C1 C28 C40 110.56(13) . . ? C29 C28 C40 100.67(13) . . ? C30 C29 C34 120.72(16) . . ? C30 C29 C28 127.92(15) . . ? C34 C29 C28 111.36(15) . . ? C29 C30 C31 119.24(17) . . ? C29 C30 H30 120.4 . . ? C31 C30 H30 120.4 . . ? C32 C31 C30 120.02(19) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C33 C32 C31 120.98(18) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C32 C33 C34 119.13(18) . . ? C32 C33 H33 120.4 . . ? C34 C33 H33 120.4 . . ? C29 C34 C33 119.91(18) . . ? C29 C34 C35 108.48(15) . . ? C33 C34 C35 131.61(17) . . ? C36 C35 C40 120.37(19) . . ? C36 C35 C34 130.91(18) . . ? C40 C35 C34 108.72(15) . . ? C37 C36 C35 118.3(2) . . ? C37 C36 H36 120.8 . . ? C35 C36 H36 120.8 . . ? C36 C37 C38 121.20(19) . . ? C36 C37 H37 119.4 . . ? C38 C37 H37 119.4 . . ? C37 C38 C39 120.7(2) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C40 C39 C38 118.33(19) . . ? C40 C39 H39 120.8 . . ? C38 C39 H39 120.8 . . ? C39 C40 C35 121.10(17) . . ? C39 C40 C28 128.12(16) . . ? C35 C40 C28 110.78(15) . . ? C1 N1 C4 108.21(14) . . ? C1 N1 Co1 134.87(12) . . ? C4 N1 Co1 115.16(11) . . ? C5 N2 C6 117.79(15) . . ? C5 N2 Co1 111.35(11) . . ? C6 N2 Co1 130.85(12) . . ? C23 N3 C22 117.45(15) . . ? C23 N3 Co1 111.90(11) . . ? C22 N3 Co1 130.12(12) . . ? C27 N4 C24 108.17(14) . . ? C27 N4 Co1 135.76(12) . . ? C24 N4 Co1 115.96(11) . . ? C13 N5 C14 111.31(15) . . ? C13 N5 C15 111.49(15) . . ? C14 N5 C15 111.41(15) . . ? C11 O1 C12 119.07(14) . . ? C17 O2 C16 116.63(15) . . ? Co1 O3 H47 104.5(14) . . ? Co1 O3 H48 113.0(14) . . ? H47 O3 H48 105(2) . . ? N1 Co1 N4 86.53(6) . . ? N1 Co1 N2 82.30(6) . . ? N4 Co1 N2 166.58(6) . . ? N1 Co1 N3 161.29(6) . . ? N4 Co1 N3 81.93(6) . . ? N2 Co1 N3 106.82(6) . . ? N1 Co1 O3 102.17(6) . . ? N4 Co1 O3 94.46(5) . . ? N2 Co1 O3 95.13(5) . . ? N3 Co1 O3 93.40(5) . . ? C42 C41 C46 120.2(3) . . ? C42 C41 H41 119.9 . . ? C46 C41 H41 119.9 . . ? C41 C42 C43 120.2(2) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C42 C43 C44 120.3(2) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C43 C44 C45 119.6(2) . . ? C43 C44 H44 120.2 . . ? C45 C44 H44 120.2 . . ? C46 C45 C44 119.5(2) . . ? C46 C45 H45 120.3 . . ? C44 C45 H45 120.3 . . ? C45 C46 C41 120.1(2) . . ? C45 C46 H46 119.9 . . ? C41 C46 H46 119.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -0.2(2) . . . . ? C28 C1 C2 C3 -176.22(16) . . . . ? C1 C2 C3 C4 -0.1(2) . . . . ? C2 C3 C4 N1 0.3(2) . . . . ? C2 C3 C4 C5 -176.9(2) . . . . ? N1 C4 C5 N2 -3.8(2) . . . . ? C3 C4 C5 N2 173.4(2) . . . . ? C11 C6 C7 C8 0.2(3) . . . . ? N2 C6 C7 C8 179.54(19) . . . . ? C6 C7 C8 C9 -0.4(3) . . . . ? C7 C8 C9 C10 0.6(3) . . . . ? C8 C9 C10 C11 -0.6(3) . . . . ? C9 C10 C11 O1 178.08(17) . . . . ? C9 C10 C11 C6 0.4(3) . . . . ? C7 C6 C11 O1 -178.10(17) . . . . ? N2 C6 C11 O1 2.6(2) . . . . ? C7 C6 C11 C10 -0.2(3) . . . . ? N2 C6 C11 C10 -179.54(16) . . . . ? O1 C12 C13 N5 49.1(2) . . . . ? N5 C15 C16 O2 66.6(2) . . . . ? O2 C17 C18 C19 -178.7(2) . . . . ? C22 C17 C18 C19 0.4(3) . . . . ? C17 C18 C19 C20 1.2(4) . . . . ? C18 C19 C20 C21 -1.5(4) . . . . ? C19 C20 C21 C22 0.1(4) . . . . ? C20 C21 C22 C17 1.5(3) . . . . ? C20 C21 C22 N3 -177.74(19) . . . . ? O2 C17 C22 C21 177.39(17) . . . . ? C18 C17 C22 C21 -1.8(3) . . . . ? O2 C17 C22 N3 -3.3(3) . . . . ? C18 C17 C22 N3 177.48(18) . . . . ? N3 C23 C24 N4 -3.3(2) . . . . ? N3 C23 C24 C25 -176.15(19) . . . . ? N4 C24 C25 C26 0.05(19) . . . . ? C23 C24 C25 C26 173.0(2) . . . . ? C24 C25 C26 C27 -0.90(19) . . . . ? C25 C26 C27 N4 1.45(19) . . . . ? C25 C26 C27 C28 -177.96(16) . . . . ? N4 C27 C28 C1 -22.5(2) . . . . ? C26 C27 C28 C1 156.87(16) . . . . ? N4 C27 C28 C29 -147.55(15) . . . . ? C26 C27 C28 C29 31.8(2) . . . . ? N4 C27 C28 C40 101.65(17) . . . . ? C26 C27 C28 C40 -79.0(2) . . . . ? N1 C1 C28 C27 30.3(2) . . . . ? C2 C1 C28 C27 -154.14(17) . . . . ? N1 C1 C28 C29 155.13(15) . . . . ? C2 C1 C28 C29 -29.3(2) . . . . ? N1 C1 C28 C40 -93.91(18) . . . . ? C2 C1 C28 C40 81.7(2) . . . . ? C27 C28 C29 C30 62.6(2) . . . . ? C1 C28 C29 C30 -63.1(2) . . . . ? C40 C28 C29 C30 179.79(17) . . . . ? C27 C28 C29 C34 -116.96(16) . . . . ? C1 C28 C29 C34 117.34(16) . . . . ? C40 C28 C29 C34 0.18(18) . . . . ? C34 C29 C30 C31 -0.1(3) . . . . ? C28 C29 C30 C31 -179.70(17) . . . . ? C29 C30 C31 C32 0.4(3) . . . . ? C30 C31 C32 C33 -0.1(3) . . . . ? C31 C32 C33 C34 -0.5(3) . . . . ? C30 C29 C34 C33 -0.5(3) . . . . ? C28 C29 C34 C33 179.15(16) . . . . ? C30 C29 C34 C35 179.78(16) . . . . ? C28 C29 C34 C35 -0.6(2) . . . . ? C32 C33 C34 C29 0.8(3) . . . . ? C32 C33 C34 C35 -179.5(2) . . . . ? C29 C34 C35 C36 -180.0(2) . . . . ? C33 C34 C35 C36 0.3(4) . . . . ? C29 C34 C35 C40 0.8(2) . . . . ? C33 C34 C35 C40 -178.9(2) . . . . ? C40 C35 C36 C37 0.4(3) . . . . ? C34 C35 C36 C37 -178.78(19) . . . . ? C35 C36 C37 C38 0.1(3) . . . . ? C36 C37 C38 C39 -0.2(3) . . . . ? C37 C38 C39 C40 -0.1(3) . . . . ? C38 C39 C40 C35 0.6(3) . . . . ? C38 C39 C40 C28 179.73(17) . . . . ? C36 C35 C40 C39 -0.7(3) . . . . ? C34 C35 C40 C39 178.62(16) . . . . ? C36 C35 C40 C28 179.98(16) . . . . ? C34 C35 C40 C28 -0.7(2) . . . . ? C27 C28 C40 C39 -61.7(2) . . . . ? C1 C28 C40 C39 63.4(2) . . . . ? C29 C28 C40 C39 -178.92(17) . . . . ? C27 C28 C40 C35 117.53(16) . . . . ? C1 C28 C40 C35 -117.33(16) . . . . ? C29 C28 C40 C35 0.32(17) . . . . ? C2 C1 N1 C4 0.42(19) . . . . ? C28 C1 N1 C4 176.77(14) . . . . ? C2 C1 N1 Co1 163.99(13) . . . . ? C28 C1 N1 Co1 -19.7(3) . . . . ? C3 C4 N1 C1 -0.48(19) . . . . ? C5 C4 N1 C1 177.52(14) . . . . ? C3 C4 N1 Co1 -167.68(12) . . . . ? C5 C4 N1 Co1 10.32(18) . . . . ? C4 C5 N2 C6 176.15(15) . . . . ? C4 C5 N2 Co1 -4.0(2) . . . . ? C7 C6 N2 C5 90.5(2) . . . . ? C11 C6 N2 C5 -90.2(2) . . . . ? C7 C6 N2 Co1 -89.3(2) . . . . ? C11 C6 N2 Co1 90.0(2) . . . . ? C24 C23 N3 C22 174.97(15) . . . . ? C24 C23 N3 Co1 2.40(19) . . . . ? C21 C22 N3 C23 -73.6(2) . . . . ? C17 C22 N3 C23 107.1(2) . . . . ? C21 C22 N3 Co1 97.4(2) . . . . ? C17 C22 N3 Co1 -81.9(2) . . . . ? C26 C27 N4 C24 -1.42(18) . . . . ? C28 C27 N4 C24 178.05(14) . . . . ? C26 C27 N4 Co1 -177.18(13) . . . . ? C28 C27 N4 Co1 2.3(3) . . . . ? C25 C24 N4 C27 0.85(18) . . . . ? C23 C24 N4 C27 -174.06(14) . . . . ? C25 C24 N4 Co1 177.56(11) . . . . ? C23 C24 N4 Co1 2.65(18) . . . . ? C12 C13 N5 C14 80.03(19) . . . . ? C12 C13 N5 C15 -154.90(16) . . . . ? C16 C15 N5 C13 71.2(2) . . . . ? C16 C15 N5 C14 -163.75(16) . . . . ? C10 C11 O1 C12 8.8(3) . . . . ? C6 C11 O1 C12 -173.42(15) . . . . ? C13 C12 O1 C11 72.6(2) . . . . ? C18 C17 O2 C16 -4.7(3) . . . . ? C22 C17 O2 C16 176.15(16) . . . . ? C15 C16 O2 C17 -172.04(16) . . . . ? C1 N1 Co1 N4 -0.02(17) . . . . ? C4 N1 Co1 N4 162.70(12) . . . . ? C1 N1 Co1 N2 -172.58(17) . . . . ? C4 N1 Co1 N2 -9.86(12) . . . . ? C1 N1 Co1 N3 -51.9(3) . . . . ? C4 N1 Co1 N3 110.9(2) . . . . ? C1 N1 Co1 O3 93.80(17) . . . . ? C4 N1 Co1 O3 -103.48(12) . . . . ? C27 N4 Co1 N1 9.15(16) . . . . ? C24 N4 Co1 N1 -166.37(12) . . . . ? C27 N4 Co1 N2 42.7(4) . . . . ? C24 N4 Co1 N2 -132.8(2) . . . . ? C27 N4 Co1 N3 174.39(17) . . . . ? C24 N4 Co1 N3 -1.13(12) . . . . ? C27 N4 Co1 O3 -92.80(16) . . . . ? C24 N4 Co1 O3 91.68(12) . . . . ? C5 N2 Co1 N1 7.52(12) . . . . ? C6 N2 Co1 N1 -172.62(16) . . . . ? C5 N2 Co1 N4 -26.3(3) . . . . ? C6 N2 Co1 N4 153.5(2) . . . . ? C5 N2 Co1 N3 -155.73(12) . . . . ? C6 N2 Co1 N3 24.13(17) . . . . ? C5 N2 Co1 O3 109.14(12) . . . . ? C6 N2 Co1 O3 -71.00(16) . . . . ? C23 N3 Co1 N1 51.7(2) . . . . ? C22 N3 Co1 N1 -119.6(2) . . . . ? C23 N3 Co1 N4 -0.70(12) . . . . ? C22 N3 Co1 N4 -172.07(16) . . . . ? C23 N3 Co1 N2 168.86(11) . . . . ? C22 N3 Co1 N2 -2.51(16) . . . . ? C23 N3 Co1 O3 -94.73(12) . . . . ? C22 N3 Co1 O3 93.90(15) . . . . ? C46 C41 C42 C43 -0.5(4) . . . . ? C41 C42 C43 C44 1.0(4) . . . . ? C42 C43 C44 C45 -0.1(4) . . . . ? C43 C44 C45 C46 -1.4(4) . . . . ? C44 C45 C46 C41 2.0(4) . . . . ? C42 C41 C46 C45 -1.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.354 _refine_diff_density_min -0.500 _refine_diff_density_rms 0.050 data_jl0042_Co(LMes) _database_code_depnum_ccdc_archive 'CCDC 895824' #TrackingRef 'combined_CIF.cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H50 Co N5 O2' _chemical_formula_weight 727.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.3981(6) _cell_length_b 11.9955(3) _cell_length_c 20.8155(8) _cell_angle_alpha 90.00 _cell_angle_beta 113.323(5) _cell_angle_gamma 90.00 _cell_volume 3759.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16436 _cell_measurement_theta_min 2.3095 _cell_measurement_theta_max 73.1614 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.509 _exptl_crystal_size_mid 0.152 _exptl_crystal_size_min 0.100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 3.912 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.40871 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 34244 _diffrn_reflns_av_R_equivalents 0.0707 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 73.32 _reflns_number_total 7461 _reflns_number_gt 6142 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Siemans, 1993)' _computing_cell_refinement 'SAINT (Siemans, 1995)' _computing_data_reduction 'SAINT (Siemans, 1995)' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP(Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen et al.,2004)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0740P)^2^+2.0603P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7461 _refine_ls_number_parameters 466 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0646 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1417 _refine_ls_wR_factor_gt 0.1341 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C100 C 0.4925(2) 0.5370(4) 0.52667(17) 0.0512(9) Uani 1 1 d . . . H80A H 0.5156 0.4997 0.5717 0.061 Uiso 1 1 calc R . . H80B H 0.4292 0.5471 0.5130 0.061 Uiso 1 1 calc R . . C101 C 0.5171(2) 0.7294(4) 0.58419(19) 0.0569(10) Uani 1 1 d . . . H80C H 0.4543 0.7419 0.5676 0.085 Uiso 1 1 calc R . . H10D H 0.5468 0.7991 0.5863 0.085 Uiso 1 1 calc R . . H10E H 0.5382 0.6968 0.6300 0.085 Uiso 1 1 calc R . . C102 C 0.5362(2) 0.6509(4) 0.53455(17) 0.0571(11) Uani 1 1 d . . . H10F H 0.6000 0.6407 0.5511 0.068 Uiso 1 1 calc R . . H10G H 0.5162 0.6858 0.4888 0.068 Uiso 1 1 calc R . . Co1 Co 0.72783(2) 0.49664(3) 0.651028(18) 0.02035(12) Uani 1 1 d . . . 01 O 0.94456(12) 0.73930(15) 0.66771(9) 0.0279(4) Uani 1 1 d . . . N1 N 0.73882(13) 0.38151(17) 0.58698(10) 0.0224(4) Uani 1 1 d . . . 02 O 0.91011(11) 0.43618(15) 0.64310(9) 0.0252(4) Uani 1 1 d . . . N4 N 0.78001(13) 0.63765(18) 0.63272(10) 0.0230(4) Uani 1 1 d . . . N2 N 0.66416(13) 0.38462(18) 0.67253(10) 0.0234(4) Uani 1 1 d . . . N3 N 0.70523(14) 0.58578(18) 0.71550(10) 0.0241(4) Uani 1 1 d . . . C14 C 0.73602(16) 0.6935(2) 0.72127(12) 0.0254(5) Uani 1 1 d . . . C40 C 0.78663(16) 0.3831(2) 0.54322(12) 0.0232(5) Uani 1 1 d . . . C2 C 0.64706(16) 0.2908(2) 0.63114(12) 0.0231(5) Uani 1 1 d . . . N5 N 1.09122(15) 0.59501(19) 0.77225(11) 0.0278(5) Uani 1 1 d . . . C21 C 0.89489(17) 0.7211(2) 0.59776(13) 0.0264(5) Uani 1 1 d . . . C1 C 0.69190(16) 0.2915(2) 0.58562(12) 0.0232(5) Uani 1 1 d . . . H1 H 0.6886 0.2317 0.5562 0.028 Uiso 1 1 calc R . . C5 C 0.61841(16) 0.3765(2) 0.71410(12) 0.0248(5) Uani 1 1 d . . . C15 C 0.77608(16) 0.7178(2) 0.67432(12) 0.0246(5) Uani 1 1 d . . . H15 H 0.7990 0.7882 0.6728 0.029 Uiso 1 1 calc R . . C17 C 0.76159(17) 0.6431(2) 0.51118(13) 0.0282(5) Uani 1 1 d . . . H17 H 0.7079 0.6058 0.4995 0.034 Uiso 1 1 calc R . . C35 C 0.87707(16) 0.4125(2) 0.57305(12) 0.0235(5) Uani 1 1 d . . . C37 C 0.8839(2) 0.3919(3) 0.46037(15) 0.0347(6) Uani 1 1 d . . . H37 H 0.9163 0.3949 0.4325 0.042 Uiso 1 1 calc R . . C16 C 0.81299(17) 0.6673(2) 0.58071(12) 0.0242(5) Uani 1 1 d . . . C24 C 1.16147(17) 0.5557(2) 0.83521(13) 0.0274(5) Uani 1 1 d . . . C38 C 0.7951(2) 0.3645(2) 0.43062(14) 0.0336(6) Uani 1 1 d . . . H38 H 0.7677 0.3492 0.3830 0.040 Uiso 1 1 calc R . . C12 C 0.66627(19) 0.6736(2) 0.79361(13) 0.0314(6) Uani 1 1 d . . . H12 H 0.6420 0.6872 0.8264 0.038 Uiso 1 1 calc R . . C6 C 0.62540(17) 0.4619(2) 0.76954(13) 0.0272(5) Uani 1 1 d . . . C36 C 0.92595(17) 0.4151(2) 0.53182(14) 0.0289(5) Uani 1 1 d . . . H36 H 0.9862 0.4322 0.5516 0.035 Uiso 1 1 calc R . . C11 C 0.66259(16) 0.5719(2) 0.75858(12) 0.0256(5) Uani 1 1 d . . . C39 C 0.74677(18) 0.3598(2) 0.47240(13) 0.0293(5) Uani 1 1 d . . . H39 H 0.6869 0.3408 0.4525 0.035 Uiso 1 1 calc R . . C3 C 0.58818(17) 0.2218(2) 0.64650(13) 0.0272(5) Uani 1 1 d . . . H3 H 0.5655 0.1535 0.6260 0.033 Uiso 1 1 calc R . . C34 C 0.99703(17) 0.4829(2) 0.67311(13) 0.0262(5) Uani 1 1 d . . . H34A H 1.0028 0.5429 0.6439 0.031 Uiso 1 1 calc R . . H34B H 1.0412 0.4265 0.6771 0.031 Uiso 1 1 calc R . . C4 C 0.57046(17) 0.2762(2) 0.69879(13) 0.0295(5) Uani 1 1 d . . . H4 H 0.5334 0.2505 0.7198 0.035 Uiso 1 1 calc R . . C22 C 1.03869(17) 0.7553(2) 0.69087(14) 0.0291(5) Uani 1 1 d . . . H22A H 1.0519 0.8335 0.6879 0.035 Uiso 1 1 calc R . . H22B H 1.0612 0.7129 0.6617 0.035 Uiso 1 1 calc R . . C13 C 0.71265(19) 0.7501(2) 0.77049(14) 0.0307(6) Uani 1 1 d . . . H13 H 0.7255 0.8238 0.7848 0.037 Uiso 1 1 calc R . . C25 C 1.24195(18) 0.5289(2) 0.83083(13) 0.0273(5) Uani 1 1 d . . . C18 C 0.7896(2) 0.6741(3) 0.45851(14) 0.0346(6) Uani 1 1 d . . . H18 H 0.7547 0.6576 0.4120 0.042 Uiso 1 1 calc R . . C33 C 1.01069(18) 0.5273(2) 0.74531(13) 0.0294(5) Uani 1 1 d . . . H33A H 0.9600 0.5720 0.7422 0.035 Uiso 1 1 calc R . . H33B H 1.0160 0.4656 0.7768 0.035 Uiso 1 1 calc R . . C26 C 1.25355(19) 0.5457(3) 0.76319(14) 0.0330(6) Uani 1 1 d . . . H26A H 1.3092 0.5143 0.7672 0.050 Uiso 1 1 calc R . . H26B H 1.2529 0.6240 0.7534 0.050 Uiso 1 1 calc R . . H26C H 1.2060 0.5095 0.7258 0.050 Uiso 1 1 calc R . . C7 C 0.53288(19) 0.4783(2) 0.77225(14) 0.0317(6) Uani 1 1 d . . . H7A H 0.5147 0.4084 0.7860 0.038 Uiso 1 1 calc R . . H7B H 0.5384 0.5328 0.8082 0.038 Uiso 1 1 calc R . . C9 C 0.68931(19) 0.4152(3) 0.84196(13) 0.0331(6) Uani 1 1 d . . . H9A H 0.6880 0.4648 0.8783 0.040 Uiso 1 1 calc R . . H9B H 0.6673 0.3432 0.8491 0.040 Uiso 1 1 calc R . . C20 C 0.92235(19) 0.7530(2) 0.54514(15) 0.0319(6) Uani 1 1 d . . . H20 H 0.9761 0.7900 0.5564 0.038 Uiso 1 1 calc R . . C31 C 1.15149(19) 0.5431(3) 0.89880(14) 0.0340(6) Uani 1 1 d . . . C28 C 1.3024(2) 0.4713(2) 0.95296(14) 0.0345(6) Uani 1 1 d . . . C19 C 0.8690(2) 0.7291(3) 0.47566(14) 0.0365(6) Uani 1 1 d . . . H19 H 0.8872 0.7506 0.4405 0.044 Uiso 1 1 calc R . . C23 C 1.08183(17) 0.7157(2) 0.76595(14) 0.0293(5) Uani 1 1 d . . . H23A H 1.1401 0.7495 0.7879 0.035 Uiso 1 1 calc R . . H23B H 1.0464 0.7407 0.7911 0.035 Uiso 1 1 calc R . . C32 C 1.0670(2) 0.5773(3) 0.90695(16) 0.0436(7) Uani 1 1 d . . . H32A H 1.0302 0.5130 0.9020 0.065 Uiso 1 1 calc R . . H32B H 1.0355 0.6311 0.8717 0.065 Uiso 1 1 calc R . . H32C H 1.0818 0.6096 0.9524 0.065 Uiso 1 1 calc R . . C10 C 0.7852(2) 0.4017(3) 0.85012(15) 0.0388(7) Uani 1 1 d . . . H10A H 0.8083 0.4728 0.8444 0.058 Uiso 1 1 calc R . . H10B H 0.7876 0.3509 0.8153 0.058 Uiso 1 1 calc R . . H10C H 0.8201 0.3729 0.8958 0.058 Uiso 1 1 calc R . . C8 C 0.46029(19) 0.5165(3) 0.70362(15) 0.0369(6) Uani 1 1 d . . . H8A H 0.4504 0.4601 0.6686 0.055 Uiso 1 1 calc R . . H8B H 0.4783 0.5845 0.6886 0.055 Uiso 1 1 calc R . . H8C H 0.4064 0.5292 0.7103 0.055 Uiso 1 1 calc R . . C27 C 1.31118(19) 0.4873(2) 0.88968(14) 0.0308(6) Uani 1 1 d . . . H27 H 1.3648 0.4697 0.8867 0.037 Uiso 1 1 calc R . . C29 C 1.3781(2) 0.4247(3) 1.01572(15) 0.0451(7) Uani 1 1 d . . . H29A H 1.3561 0.3676 1.0370 0.068 Uiso 1 1 calc R . . H29B H 1.4044 0.4833 1.0489 0.068 Uiso 1 1 calc R . . H29C H 1.4219 0.3935 1.0012 0.068 Uiso 1 1 calc R . . C30 C 1.2217(2) 0.5001(3) 0.95598(15) 0.0374(7) Uani 1 1 d . . . H30 H 1.2147 0.4902 0.9978 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C100 0.0256(13) 0.083(3) 0.0435(17) 0.0355(18) 0.0123(13) 0.0095(15) C101 0.0342(16) 0.079(3) 0.0497(19) 0.0229(18) 0.0079(14) -0.0136(17) C102 0.0280(14) 0.097(3) 0.0383(17) 0.0303(18) 0.0048(13) -0.0073(17) Co1 0.02318(19) 0.0226(2) 0.01804(19) -0.00046(15) 0.01117(15) -0.00009(15) 01 0.0263(9) 0.0309(10) 0.0287(9) -0.0019(7) 0.0134(7) -0.0019(7) N1 0.0216(9) 0.0262(11) 0.0197(9) 0.0003(8) 0.0085(8) 0.0013(8) 02 0.0254(8) 0.0276(9) 0.0223(8) -0.0011(7) 0.0091(7) -0.0025(7) N4 0.0241(9) 0.0250(10) 0.0217(9) 0.0017(8) 0.0108(8) 0.0012(8) N2 0.0245(10) 0.0278(11) 0.0198(9) -0.0003(8) 0.0107(8) 0.0003(8) N3 0.0263(10) 0.0262(11) 0.0216(9) 0.0006(8) 0.0116(8) 0.0021(8) C14 0.0263(11) 0.0282(13) 0.0235(11) -0.0017(10) 0.0117(10) -0.0006(10) C40 0.0272(12) 0.0233(12) 0.0224(11) -0.0024(9) 0.0134(10) 0.0010(9) C2 0.0233(11) 0.0238(12) 0.0215(11) 0.0018(9) 0.0081(9) 0.0013(9) N5 0.0295(11) 0.0251(11) 0.0260(10) -0.0029(8) 0.0079(9) -0.0051(9) C21 0.0297(12) 0.0262(13) 0.0266(12) 0.0029(10) 0.0147(10) 0.0053(10) C1 0.0247(11) 0.0255(12) 0.0176(10) -0.0014(9) 0.0066(9) -0.0002(9) C5 0.0254(11) 0.0294(13) 0.0228(11) 0.0031(10) 0.0127(10) 0.0003(10) C15 0.0237(11) 0.0258(13) 0.0239(11) 0.0014(9) 0.0090(10) 0.0011(9) C17 0.0303(12) 0.0300(13) 0.0272(12) 0.0019(10) 0.0145(10) 0.0024(10) C35 0.0282(12) 0.0210(12) 0.0219(11) -0.0014(9) 0.0107(10) 0.0011(9) C37 0.0421(15) 0.0388(16) 0.0355(14) -0.0094(12) 0.0283(13) -0.0054(12) C16 0.0296(12) 0.0221(12) 0.0245(11) 0.0029(9) 0.0144(10) 0.0047(9) C24 0.0310(12) 0.0241(13) 0.0262(12) -0.0025(10) 0.0103(10) -0.0061(10) C38 0.0432(15) 0.0365(15) 0.0274(12) -0.0091(11) 0.0208(12) -0.0046(12) C12 0.0401(14) 0.0334(14) 0.0273(12) -0.0029(11) 0.0203(11) 0.0008(11) C6 0.0312(12) 0.0317(13) 0.0229(11) 0.0003(10) 0.0150(10) 0.0015(10) C36 0.0284(12) 0.0299(13) 0.0335(13) -0.0060(11) 0.0177(11) -0.0036(10) C11 0.0275(12) 0.0294(13) 0.0220(11) 0.0002(10) 0.0122(10) 0.0021(10) C39 0.0316(13) 0.0336(14) 0.0250(12) -0.0042(10) 0.0135(11) -0.0019(11) C3 0.0275(12) 0.0267(13) 0.0276(12) 0.0004(10) 0.0112(10) -0.0030(10) C34 0.0243(12) 0.0260(13) 0.0289(12) -0.0027(10) 0.0110(10) -0.0017(9) C4 0.0301(12) 0.0325(14) 0.0307(12) 0.0039(11) 0.0173(11) -0.0008(10) C22 0.0274(12) 0.0251(13) 0.0366(14) -0.0014(10) 0.0146(11) -0.0012(10) C13 0.0396(14) 0.0276(13) 0.0293(13) -0.0075(10) 0.0183(11) -0.0020(11) C25 0.0317(13) 0.0239(12) 0.0266(12) -0.0029(10) 0.0119(10) -0.0039(10) C18 0.0413(15) 0.0407(16) 0.0239(12) 0.0052(11) 0.0152(11) 0.0063(12) C33 0.0303(13) 0.0310(13) 0.0270(12) -0.0014(10) 0.0115(10) -0.0032(11) C26 0.0338(13) 0.0400(16) 0.0278(13) -0.0020(11) 0.0148(11) -0.0008(12) C7 0.0362(14) 0.0356(14) 0.0318(13) 0.0004(11) 0.0225(12) -0.0005(11) C9 0.0420(15) 0.0362(15) 0.0242(12) 0.0053(11) 0.0164(11) 0.0023(12) C20 0.0343(14) 0.0295(14) 0.0374(14) 0.0066(11) 0.0200(12) 0.0016(11) C31 0.0373(14) 0.0385(16) 0.0297(13) -0.0063(11) 0.0170(12) -0.0089(12) C28 0.0425(15) 0.0289(14) 0.0270(13) -0.0023(11) 0.0084(12) -0.0031(12) C19 0.0464(16) 0.0406(16) 0.0312(13) 0.0116(12) 0.0247(13) 0.0081(13) C23 0.0294(12) 0.0256(13) 0.0317(13) -0.0056(10) 0.0108(11) -0.0035(10) C32 0.0390(16) 0.064(2) 0.0343(14) -0.0021(14) 0.0210(13) -0.0041(15) C10 0.0373(15) 0.0456(18) 0.0313(14) 0.0085(12) 0.0113(12) 0.0050(13) C8 0.0311(14) 0.0480(18) 0.0370(14) 0.0022(13) 0.0193(12) 0.0053(12) C27 0.0348(14) 0.0248(13) 0.0317(13) -0.0024(10) 0.0121(11) -0.0012(10) C29 0.0545(19) 0.0457(18) 0.0298(14) 0.0039(13) 0.0109(14) 0.0088(15) C30 0.0498(17) 0.0388(17) 0.0243(13) -0.0020(11) 0.0155(12) -0.0089(13) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C100 C100 1.515(8) 3_666 ? C100 C102 1.522(6) . ? C100 H80A 0.9700 . ? C100 H80B 0.9700 . ? C101 C102 1.519(6) . ? C101 H80C 0.9600 . ? C101 H10D 0.9600 . ? C101 H10E 0.9600 . ? C102 H10F 0.9700 . ? C102 H10G 0.9700 . ? Co1 N2 1.862(2) . ? Co1 N3 1.864(2) . ? Co1 N1 1.977(2) . ? Co1 N4 1.999(2) . ? 01 C21 1.375(3) . ? 01 C22 1.436(3) . ? N1 C1 1.320(3) . ? N1 C40 1.418(3) . ? 02 C35 1.369(3) . ? 02 C34 1.425(3) . ? N4 C15 1.312(3) . ? N4 C16 1.433(3) . ? N2 C5 1.355(3) . ? N2 C2 1.377(3) . ? N3 C11 1.348(3) . ? N3 C14 1.375(3) . ? C14 C13 1.403(3) . ? C14 C15 1.407(3) . ? C40 C39 1.384(3) . ? C40 C35 1.407(3) . ? C2 C3 1.402(3) . ? C2 C1 1.411(3) . ? N5 C24 1.439(3) . ? N5 C23 1.456(4) . ? N5 C33 1.460(3) . ? C21 C20 1.393(3) . ? C21 C16 1.403(4) . ? C1 H1 0.9300 . ? C5 C4 1.403(4) . ? C5 C6 1.513(4) . ? C15 H15 0.9300 . ? C17 C16 1.387(4) . ? C17 C18 1.396(3) . ? C17 H17 0.9300 . ? C35 C36 1.387(3) . ? C37 C38 1.378(4) . ? C37 C36 1.398(4) . ? C37 H37 0.9300 . ? C24 C25 1.396(4) . ? C24 C31 1.405(4) . ? C38 C39 1.390(3) . ? C38 H38 0.9300 . ? C12 C13 1.393(4) . ? C12 C11 1.410(4) . ? C12 H12 0.9300 . ? C6 C11 1.509(4) . ? C6 C7 1.553(4) . ? C6 C9 1.560(4) . ? C36 H36 0.9300 . ? C39 H39 0.9300 . ? C3 C4 1.395(4) . ? C3 H3 0.9300 . ? C34 C33 1.525(3) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C4 H4 0.9300 . ? C22 C23 1.514(4) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C13 H13 0.9300 . ? C25 C27 1.392(4) . ? C25 C26 1.507(3) . ? C18 C19 1.375(4) . ? C18 H18 0.9300 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C7 C8 1.524(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C9 C10 1.522(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C20 C19 1.392(4) . ? C20 H20 0.9300 . ? C31 C30 1.387(4) . ? C31 C32 1.518(4) . ? C28 C30 1.393(5) . ? C28 C27 1.394(4) . ? C28 C29 1.508(4) . ? C19 H19 0.9300 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C27 H27 0.9300 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30 0.9300 . ? 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 C100 C100 C102 113.6(3) 3_666 . ? C100 C100 H80A 108.9 3_666 . ? C102 C100 H80A 108.9 . . ? C100 C100 H80B 108.9 3_666 . ? C102 C100 H80B 108.9 . . ? H80A C100 H80B 107.7 . . ? C102 C101 H80C 109.5 . . ? C102 C101 H10D 109.5 . . ? H80C C101 H10D 109.5 . . ? C102 C101 H10E 109.5 . . ? H80C C101 H10E 109.5 . . ? H10D C101 H10E 109.5 . . ? C101 C102 C100 114.5(3) . . ? C101 C102 H10F 108.6 . . ? C100 C102 H10F 108.6 . . ? C101 C102 H10G 108.6 . . ? C100 C102 H10G 108.6 . . ? H10F C102 H10G 107.6 . . ? N2 Co1 N3 87.17(9) . . ? N2 Co1 N1 82.38(9) . . ? N3 Co1 N1 169.55(9) . . ? N2 Co1 N4 168.40(9) . . ? N3 Co1 N4 82.76(9) . . ? N1 Co1 N4 107.60(8) . . ? C21 01 C22 118.94(19) . . ? C1 N1 C40 117.6(2) . . ? C1 N1 Co1 112.21(15) . . ? C40 N1 Co1 130.18(17) . . ? C35 02 C34 116.99(18) . . ? C15 N4 C16 116.6(2) . . ? C15 N4 Co1 110.96(16) . . ? C16 N4 Co1 132.19(17) . . ? C5 N2 C2 108.3(2) . . ? C5 N2 Co1 135.30(18) . . ? C2 N2 Co1 115.73(15) . . ? C11 N3 C14 109.1(2) . . ? C11 N3 Co1 135.35(19) . . ? C14 N3 Co1 115.53(16) . . ? N3 C14 C13 108.7(2) . . ? N3 C14 C15 113.0(2) . . ? C13 C14 C15 138.1(3) . . ? C39 C40 C35 119.4(2) . . ? C39 C40 N1 122.2(2) . . ? C35 C40 N1 118.3(2) . . ? N2 C2 C3 109.2(2) . . ? N2 C2 C1 112.6(2) . . ? C3 C2 C1 138.2(2) . . ? C24 N5 C23 115.2(2) . . ? C24 N5 C33 116.3(2) . . ? C23 N5 C33 118.1(2) . . ? 01 C21 C20 123.3(2) . . ? 01 C21 C16 116.6(2) . . ? C20 C21 C16 120.2(2) . . ? N1 C1 C2 116.4(2) . . ? N1 C1 H1 121.8 . . ? C2 C1 H1 121.8 . . ? N2 C5 C4 108.6(2) . . ? N2 C5 C6 123.0(2) . . ? C4 C5 C6 128.3(2) . . ? N4 C15 C14 117.7(2) . . ? N4 C15 H15 121.2 . . ? C14 C15 H15 121.2 . . ? C16 C17 C18 120.7(3) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? 02 C35 C36 124.9(2) . . ? 02 C35 C40 115.2(2) . . ? C36 C35 C40 119.9(2) . . ? C38 C37 C36 120.9(2) . . ? C38 C37 H37 119.5 . . ? C36 C37 H37 119.5 . . ? C17 C16 C21 119.0(2) . . ? C17 C16 N4 118.8(2) . . ? C21 C16 N4 122.2(2) . . ? C25 C24 C31 120.2(3) . . ? C25 C24 N5 116.9(2) . . ? C31 C24 N5 122.9(2) . . ? C37 C38 C39 119.4(2) . . ? C37 C38 H38 120.3 . . ? C39 C38 H38 120.3 . . ? C13 C12 C11 108.0(2) . . ? C13 C12 H12 126.0 . . ? C11 C12 H12 126.0 . . ? C11 C6 C5 113.0(2) . . ? C11 C6 C7 110.7(2) . . ? C5 C6 C7 109.5(2) . . ? C11 C6 C9 107.6(2) . . ? C5 C6 C9 108.2(2) . . ? C7 C6 C9 107.6(2) . . ? C35 C36 C37 119.4(2) . . ? C35 C36 H36 120.3 . . ? C37 C36 H36 120.3 . . ? N3 C11 C12 108.1(2) . . ? N3 C11 C6 123.8(2) . . ? C12 C11 C6 128.0(2) . . ? C40 C39 C38 120.8(2) . . ? C40 C39 H39 119.6 . . ? C38 C39 H39 119.6 . . ? C4 C3 C2 106.1(2) . . ? C4 C3 H3 127.0 . . ? C2 C3 H3 127.0 . . ? 02 C34 C33 107.5(2) . . ? 02 C34 H34A 110.2 . . ? C33 C34 H34A 110.2 . . ? 02 C34 H34B 110.2 . . ? C33 C34 H34B 110.2 . . ? H34A C34 H34B 108.5 . . ? C3 C4 C5 107.9(2) . . ? C3 C4 H4 126.1 . . ? C5 C4 H4 126.1 . . ? 01 C22 C23 107.8(2) . . ? 01 C22 H22A 110.1 . . ? C23 C22 H22A 110.1 . . ? 01 C22 H22B 110.1 . . ? C23 C22 H22B 110.1 . . ? H22A C22 H22B 108.5 . . ? C12 C13 C14 106.1(2) . . ? C12 C13 H13 126.9 . . ? C14 C13 H13 126.9 . . ? C27 C25 C24 119.2(2) . . ? C27 C25 C26 120.6(2) . . ? C24 C25 C26 120.2(2) . . ? C19 C18 C17 119.7(3) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? N5 C33 C34 109.3(2) . . ? N5 C33 H33A 109.8 . . ? C34 C33 H33A 109.8 . . ? N5 C33 H33B 109.8 . . ? C34 C33 H33B 109.8 . . ? H33A C33 H33B 108.3 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C8 C7 C6 114.6(2) . . ? C8 C7 H7A 108.6 . . ? C6 C7 H7A 108.6 . . ? C8 C7 H7B 108.6 . . ? C6 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? C10 C9 C6 114.5(2) . . ? C10 C9 H9A 108.6 . . ? C6 C9 H9A 108.6 . . ? C10 C9 H9B 108.6 . . ? C6 C9 H9B 108.6 . . ? H9A C9 H9B 107.6 . . ? C19 C20 C21 119.7(3) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C30 C31 C24 118.8(3) . . ? C30 C31 C32 119.3(3) . . ? C24 C31 C32 121.9(3) . . ? C30 C28 C27 117.6(3) . . ? C30 C28 C29 121.6(3) . . ? C27 C28 C29 120.8(3) . . ? C18 C19 C20 120.6(2) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? N5 C23 C22 113.2(2) . . ? N5 C23 H23A 108.9 . . ? C22 C23 H23A 108.9 . . ? N5 C23 H23B 108.9 . . ? C22 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C25 C27 C28 121.8(3) . . ? C25 C27 H27 119.1 . . ? C28 C27 H27 119.1 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C28 122.3(3) . . ? C31 C30 H30 118.8 . . ? C28 C30 H30 118.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C100 C100 C102 C101 176.1(3) 3_666 . . . ? N2 Co1 N1 C1 5.74(17) . . . . ? N3 Co1 N1 C1 4.3(6) . . . . ? N4 Co1 N1 C1 -168.20(16) . . . . ? N2 Co1 N1 C40 -175.6(2) . . . . ? N3 Co1 N1 C40 -177.1(4) . . . . ? N4 Co1 N1 C40 10.5(2) . . . . ? N2 Co1 N4 C15 32.2(5) . . . . ? N3 Co1 N4 C15 2.25(17) . . . . ? N1 Co1 N4 C15 -179.12(16) . . . . ? N2 Co1 N4 C16 -142.3(4) . . . . ? N3 Co1 N4 C16 -172.2(2) . . . . ? N1 Co1 N4 C16 6.4(2) . . . . ? N3 Co1 N2 C5 3.1(2) . . . . ? N1 Co1 N2 C5 -176.6(3) . . . . ? N4 Co1 N2 C5 -26.7(6) . . . . ? N3 Co1 N2 C2 172.15(18) . . . . ? N1 Co1 N2 C2 -7.58(17) . . . . ? N4 Co1 N2 C2 142.4(4) . . . . ? N2 Co1 N3 C11 0.9(2) . . . . ? N1 Co1 N3 C11 2.4(6) . . . . ? N4 Co1 N3 C11 175.1(3) . . . . ? N2 Co1 N3 C14 -176.94(18) . . . . ? N1 Co1 N3 C14 -175.5(4) . . . . ? N4 Co1 N3 C14 -2.71(18) . . . . ? C11 N3 C14 C13 0.5(3) . . . . ? Co1 N3 C14 C13 178.94(17) . . . . ? C11 N3 C14 C15 -175.7(2) . . . . ? Co1 N3 C14 C15 2.7(3) . . . . ? C1 N1 C40 C39 52.1(3) . . . . ? Co1 N1 C40 C39 -126.5(2) . . . . ? C1 N1 C40 C35 -129.7(2) . . . . ? Co1 N1 C40 C35 51.7(3) . . . . ? C5 N2 C2 C3 0.6(3) . . . . ? Co1 N2 C2 C3 -171.36(16) . . . . ? C5 N2 C2 C1 179.9(2) . . . . ? Co1 N2 C2 C1 8.0(3) . . . . ? C22 01 C21 C20 -22.2(4) . . . . ? C22 01 C21 C16 157.6(2) . . . . ? C40 N1 C1 C2 178.2(2) . . . . ? Co1 N1 C1 C2 -2.9(3) . . . . ? N2 C2 C1 N1 -3.0(3) . . . . ? C3 C2 C1 N1 176.1(3) . . . . ? C2 N2 C5 C4 -0.5(3) . . . . ? Co1 N2 C5 C4 169.10(19) . . . . ? C2 N2 C5 C6 176.4(2) . . . . ? Co1 N2 C5 C6 -14.0(4) . . . . ? C16 N4 C15 C14 174.0(2) . . . . ? Co1 N4 C15 C14 -1.4(3) . . . . ? N3 C14 C15 N4 -0.7(3) . . . . ? C13 C14 C15 N4 -175.4(3) . . . . ? C34 02 C35 C36 9.9(4) . . . . ? C34 02 C35 C40 -170.5(2) . . . . ? C39 C40 C35 02 178.7(2) . . . . ? N1 C40 C35 02 0.5(3) . . . . ? C39 C40 C35 C36 -1.6(4) . . . . ? N1 C40 C35 C36 -179.9(2) . . . . ? C18 C17 C16 C21 -1.6(4) . . . . ? C18 C17 C16 N4 177.6(2) . . . . ? 01 C21 C16 C17 -177.7(2) . . . . ? C20 C21 C16 C17 2.2(4) . . . . ? 01 C21 C16 N4 3.2(4) . . . . ? C20 C21 C16 N4 -177.0(2) . . . . ? C15 N4 C16 C17 -125.7(3) . . . . ? Co1 N4 C16 C17 48.5(3) . . . . ? C15 N4 C16 C21 53.4(3) . . . . ? Co1 N4 C16 C21 -132.4(2) . . . . ? C23 N5 C24 C25 -97.1(3) . . . . ? C33 N5 C24 C25 118.4(3) . . . . ? C23 N5 C24 C31 83.4(3) . . . . ? C33 N5 C24 C31 -61.1(3) . . . . ? C36 C37 C38 C39 -0.1(5) . . . . ? N2 C5 C6 C11 18.8(3) . . . . ? C4 C5 C6 C11 -164.9(3) . . . . ? N2 C5 C6 C7 142.6(2) . . . . ? C4 C5 C6 C7 -41.1(4) . . . . ? N2 C5 C6 C9 -100.3(3) . . . . ? C4 C5 C6 C9 76.0(3) . . . . ? 02 C35 C36 C37 -178.4(3) . . . . ? C40 C35 C36 C37 2.0(4) . . . . ? C38 C37 C36 C35 -1.2(4) . . . . ? C14 N3 C11 C12 -0.3(3) . . . . ? Co1 N3 C11 C12 -178.27(19) . . . . ? C14 N3 C11 C6 -175.8(2) . . . . ? Co1 N3 C11 C6 6.3(4) . . . . ? C13 C12 C11 N3 0.0(3) . . . . ? C13 C12 C11 C6 175.2(3) . . . . ? C5 C6 C11 N3 -15.4(3) . . . . ? C7 C6 C11 N3 -138.6(2) . . . . ? C9 C6 C11 N3 104.0(3) . . . . ? C5 C6 C11 C12 170.1(3) . . . . ? C7 C6 C11 C12 46.9(4) . . . . ? C9 C6 C11 C12 -70.5(3) . . . . ? C35 C40 C39 C38 0.4(4) . . . . ? N1 C40 C39 C38 178.6(3) . . . . ? C37 C38 C39 C40 0.4(4) . . . . ? N2 C2 C3 C4 -0.4(3) . . . . ? C1 C2 C3 C4 -179.5(3) . . . . ? C35 02 C34 C33 166.8(2) . . . . ? C2 C3 C4 C5 0.0(3) . . . . ? N2 C5 C4 C3 0.3(3) . . . . ? C6 C5 C4 C3 -176.4(2) . . . . ? C21 01 C22 C23 -151.7(2) . . . . ? C11 C12 C13 C14 0.3(3) . . . . ? N3 C14 C13 C12 -0.5(3) . . . . ? C15 C14 C13 C12 174.3(3) . . . . ? C31 C24 C25 C27 1.4(4) . . . . ? N5 C24 C25 C27 -178.1(2) . . . . ? C31 C24 C25 C26 -178.1(3) . . . . ? N5 C24 C25 C26 2.4(4) . . . . ? C16 C17 C18 C19 0.1(4) . . . . ? C24 N5 C33 C34 -117.4(2) . . . . ? C23 N5 C33 C34 99.2(3) . . . . ? 02 C34 C33 N5 -168.9(2) . . . . ? C11 C6 C7 C8 66.4(3) . . . . ? C5 C6 C7 C8 -58.7(3) . . . . ? C9 C6 C7 C8 -176.2(2) . . . . ? C11 C6 C9 C10 -56.6(3) . . . . ? C5 C6 C9 C10 65.8(3) . . . . ? C7 C6 C9 C10 -176.0(3) . . . . ? 01 C21 C20 C19 178.5(2) . . . . ? C16 C21 C20 C19 -1.3(4) . . . . ? C25 C24 C31 C30 -2.2(4) . . . . ? N5 C24 C31 C30 177.2(3) . . . . ? C25 C24 C31 C32 176.5(3) . . . . ? N5 C24 C31 C32 -4.0(4) . . . . ? C17 C18 C19 C20 0.8(4) . . . . ? C21 C20 C19 C18 -0.2(4) . . . . ? C24 N5 C23 C22 154.9(2) . . . . ? C33 N5 C23 C22 -61.3(3) . . . . ? 01 C22 C23 N5 79.4(3) . . . . ? C24 C25 C27 C28 0.2(4) . . . . ? C26 C25 C27 C28 179.8(3) . . . . ? C30 C28 C27 C25 -1.0(4) . . . . ? C29 C28 C27 C25 179.2(3) . . . . ? C24 C31 C30 C28 1.5(4) . . . . ? C32 C31 C30 C28 -177.4(3) . . . . ? C27 C28 C30 C31 0.1(4) . . . . ? C29 C28 C30 C31 179.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 73.32 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.599 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.065 data_Fe2(2+2LP) _database_code_depnum_ccdc_archive 'CCDC 895825' #TrackingRef 'combined_CIF.cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C73 H83 Fe2 N8 O10' _chemical_formula_sum 'C73 H83 Fe2 N8 O10' _chemical_formula_weight 1344.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.120(3) _cell_length_b 13.077(3) _cell_length_c 20.726(5) _cell_angle_alpha 95.077(8) _cell_angle_beta 90.782(6) _cell_angle_gamma 95.088(11) _cell_volume 3258.4(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10937 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 29.0 _exptl_crystal_description Plate _exptl_crystal_colour Red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1418 _exptl_absorpt_coefficient_mu 0.513 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.368 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type ; Rigaku Mercury (2x2 bin mode) ; _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 14.7059 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 20681 _diffrn_reflns_av_R_equivalents 0.0704 _diffrn_reflns_av_sigmaI/netI 0.0956 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 25.35 _reflns_number_total 11277 _reflns_number_gt 8773 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009) ; _computing_cell_refinement ; CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009) ; _computing_data_reduction ; CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009) ; _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen et al., 2004)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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. Disordered Benzene solvent on plane of symmetry. Attempted to model splitting results in diverging Max shift. Benzene molecule restrained using ISOR 0.02 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1333P)^2^+4.6907P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11277 _refine_ls_number_parameters 842 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1010 _refine_ls_R_factor_gt 0.0825 _refine_ls_wR_factor_ref 0.2489 _refine_ls_wR_factor_gt 0.2247 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3244(4) 0.1526(3) 0.9375(2) 0.0279(9) Uani 1 1 d . . . H1 H 0.3457 0.1136 0.9714 0.033 Uiso 1 1 calc R . . C2 C 0.3839(4) 0.2491(3) 0.9283(2) 0.0264(9) Uani 1 1 d . . . C3 C 0.4705(4) 0.3071(4) 0.9633(2) 0.0321(10) Uani 1 1 d . . . H3 H 0.5071 0.2892 1.0009 0.039 Uiso 1 1 calc R . . C4 C 0.4931(4) 0.3970(4) 0.9319(2) 0.0329(10) Uani 1 1 d . . . H4 H 0.5481 0.4519 0.9441 0.039 Uiso 1 1 calc R . . C5 C 0.4188(4) 0.3899(3) 0.8790(2) 0.0277(9) Uani 1 1 d . . . C6 C 0.4048(4) 0.4646(3) 0.8276(2) 0.0287(10) Uani 1 1 d . . . C7 C 0.4668(4) 0.5706(4) 0.8506(2) 0.0343(11) Uani 1 1 d . . . H7A H 0.4341 0.5968 0.8916 0.041 Uiso 1 1 calc R . . H7B H 0.5451 0.5602 0.8601 0.041 Uiso 1 1 calc R . . C8 C 0.4644(5) 0.6529(4) 0.8028(3) 0.0464(13) Uani 1 1 d . . . H8A H 0.4957 0.6277 0.7617 0.070 Uiso 1 1 calc R . . H8B H 0.5082 0.7158 0.8207 0.070 Uiso 1 1 calc R . . H8C H 0.3877 0.6679 0.7954 0.070 Uiso 1 1 calc R . . C9 C 0.4507(4) 0.4209(4) 0.7624(2) 0.0302(10) Uani 1 1 d . . . H9A H 0.4126 0.3515 0.7505 0.036 Uiso 1 1 calc R . . H9B H 0.4319 0.4655 0.7284 0.036 Uiso 1 1 calc R . . C10 C 0.5763(4) 0.4125(5) 0.7623(3) 0.0420(12) Uani 1 1 d . . . H10A H 0.6153 0.4817 0.7689 0.063 Uiso 1 1 calc R . . H10B H 0.5969 0.3788 0.7207 0.063 Uiso 1 1 calc R . . H10C H 0.5968 0.3718 0.7974 0.063 Uiso 1 1 calc R . . C11 C 0.2816(4) 0.4747(3) 0.8203(2) 0.0260(9) Uani 1 1 d . . . C12 C 0.2214(4) 0.5487(3) 0.8534(2) 0.0279(9) Uani 1 1 d . . . H12 H 0.2509 0.6042 0.8831 0.033 Uiso 1 1 calc R . . C13 C 0.1092(4) 0.5262(3) 0.8346(2) 0.0298(10) Uani 1 1 d . . . H13 H 0.0485 0.5624 0.8494 0.036 Uiso 1 1 calc R . . C14 C 0.1056(4) 0.4400(3) 0.7899(2) 0.0287(10) Uani 1 1 d . . . C15 C 0.0182(4) 0.3970(3) 0.7476(2) 0.0295(10) Uani 1 1 d . . . H15 H -0.0543 0.4179 0.7537 0.035 Uiso 1 1 calc R . . C16 C -0.0501(4) 0.2797(4) 0.6590(2) 0.0301(10) Uani 1 1 d . . . C17 C -0.1623(4) 0.2863(4) 0.6695(2) 0.0329(10) Uani 1 1 d . . . H17 H -0.1846 0.3260 0.7069 0.039 Uiso 1 1 calc R . . C18 C -0.2429(4) 0.2359(4) 0.6265(3) 0.0404(12) Uani 1 1 d . . . H18 H -0.3193 0.2417 0.6342 0.048 Uiso 1 1 calc R . . C19 C -0.2105(5) 0.1776(4) 0.5727(3) 0.0443(13) Uani 1 1 d . . . H19 H -0.2650 0.1442 0.5427 0.053 Uiso 1 1 calc R . . C20 C -0.0977(4) 0.1669(4) 0.5613(3) 0.0382(11) Uani 1 1 d . . . H20 H -0.0763 0.1252 0.5245 0.046 Uiso 1 1 calc R . . C21 C -0.0185(4) 0.2174(4) 0.6041(2) 0.0319(10) Uani 1 1 d . . . C22 C 0.1351(4) 0.1434(4) 0.5474(2) 0.0343(11) Uani 1 1 d . . . H22A H 0.0827 0.0808 0.5401 0.041 Uiso 1 1 calc R . . H22B H 0.2077 0.1220 0.5609 0.041 Uiso 1 1 calc R . . C23 C 0.1476(4) 0.1954(4) 0.4847(2) 0.0380(11) Uani 1 1 d . . . H23A H 0.0747 0.2149 0.4704 0.046 Uiso 1 1 calc R . . H23B H 0.1986 0.2589 0.4921 0.046 Uiso 1 1 calc R . . C24 C 0.3086(5) 0.1208(5) 0.4433(3) 0.0514(14) Uani 1 1 d . . . H24A H 0.3260 0.0493 0.4308 0.062 Uiso 1 1 calc R . . H24B H 0.3297 0.1375 0.4896 0.062 Uiso 1 1 calc R . . C25 C 0.3763(5) 0.1925(4) 0.4038(3) 0.0497(14) Uani 1 1 d . . . H25A H 0.4561 0.1867 0.4119 0.060 Uiso 1 1 calc R . . H25B H 0.3600 0.1731 0.3571 0.060 Uiso 1 1 calc R . . C26 C 0.4168(5) 0.3675(5) 0.3844(3) 0.0590(16) Uani 1 1 d . . . H26A H 0.4149 0.3438 0.3377 0.071 Uiso 1 1 calc R . . H26B H 0.4949 0.3748 0.4001 0.071 Uiso 1 1 calc R . . C27 C 0.3673(5) 0.4699(5) 0.3951(3) 0.0527(15) Uani 1 1 d . . . H27A H 0.3521 0.4834 0.4418 0.063 Uiso 1 1 calc R . . H27B H 0.4223 0.5252 0.3833 0.063 Uiso 1 1 calc R . . C28 C 0.1697(5) 0.4441(5) 0.3914(3) 0.0487(14) Uani 1 1 d . . . H28A H 0.1777 0.3768 0.4086 0.058 Uiso 1 1 calc R . . H28B H 0.1070 0.4343 0.3597 0.058 Uiso 1 1 calc R . . C29 C 0.1419(5) 0.5197(4) 0.4463(2) 0.0439(13) Uani 1 1 d . . . H29A H 0.1757 0.5894 0.4393 0.053 Uiso 1 1 calc R . . H29B H 0.0606 0.5220 0.4483 0.053 Uiso 1 1 calc R . . C30 C 0.1717(4) 0.5545(4) 0.5609(2) 0.0353(11) Uani 1 1 d . . . C31 C 0.1199(5) 0.6459(4) 0.5603(3) 0.0432(13) Uani 1 1 d . . . H31 H 0.0917 0.6655 0.5206 0.052 Uiso 1 1 calc R . . C32 C 0.1097(5) 0.7077(4) 0.6169(3) 0.0461(13) Uani 1 1 d . . . H32 H 0.0762 0.7705 0.6159 0.055 Uiso 1 1 calc R . . C33 C 0.1476(5) 0.6792(4) 0.6749(3) 0.0439(13) Uani 1 1 d . . . H33 H 0.1406 0.7220 0.7139 0.053 Uiso 1 1 calc R . . C34 C 0.1963(4) 0.5870(4) 0.6760(2) 0.0364(11) Uani 1 1 d . . . H34 H 0.2216 0.5671 0.7162 0.044 Uiso 1 1 calc R . . C35 C 0.2090(4) 0.5232(4) 0.6198(2) 0.0306(10) Uani 1 1 d . . . C36 C 0.3359(4) 0.3988(4) 0.5899(2) 0.0310(10) Uani 1 1 d . . . H36 H 0.3633 0.4407 0.5574 0.037 Uiso 1 1 calc R . . C37 C 0.3825(4) 0.3048(4) 0.5990(2) 0.0314(10) Uani 1 1 d . . . C38 C 0.4678(4) 0.2565(4) 0.5689(2) 0.0347(11) Uani 1 1 d . . . H38 H 0.5119 0.2807 0.5348 0.042 Uiso 1 1 calc R . . C39 C 0.4767(4) 0.1644(4) 0.5986(2) 0.0372(11) Uani 1 1 d . . . H39 H 0.5280 0.1148 0.5884 0.045 Uiso 1 1 calc R . . C40 C 0.3958(4) 0.1601(4) 0.6459(2) 0.0294(10) Uani 1 1 d . . . C41 C 0.3696(4) 0.0805(4) 0.6947(2) 0.0323(10) Uani 1 1 d . . . C42 C 0.4106(4) -0.0232(4) 0.6675(3) 0.0369(11) Uani 1 1 d . . . H42A H 0.3690 -0.0472 0.6267 0.044 Uiso 1 1 calc R . . H42B H 0.4898 -0.0112 0.6567 0.044 Uiso 1 1 calc R . . C43 C 0.3981(5) -0.1087(4) 0.7133(3) 0.0464(13) Uani 1 1 d . . . H43A H 0.4516 -0.0928 0.7495 0.070 Uiso 1 1 calc R . . H43B H 0.4119 -0.1745 0.6898 0.070 Uiso 1 1 calc R . . H43C H 0.3228 -0.1134 0.7301 0.070 Uiso 1 1 calc R . . C44 C 0.4264(4) 0.1168(4) 0.7612(2) 0.0343(11) Uani 1 1 d . . . H44A H 0.4017 0.1850 0.7760 0.041 Uiso 1 1 calc R . . H44B H 0.3998 0.0682 0.7927 0.041 Uiso 1 1 calc R . . C45 C 0.5534(4) 0.1259(4) 0.7630(3) 0.0424(12) Uani 1 1 d . . . H45A H 0.5794 0.0578 0.7522 0.064 Uiso 1 1 calc R . . H45B H 0.5805 0.1528 0.8065 0.064 Uiso 1 1 calc R . . H45C H 0.5813 0.1729 0.7314 0.064 Uiso 1 1 calc R . . C46 C 0.2441(4) 0.0689(3) 0.7016(2) 0.0274(9) Uani 1 1 d . . . C47 C 0.1693(4) -0.0075(3) 0.6704(2) 0.0313(10) Uani 1 1 d . . . H47 H 0.1872 -0.0619 0.6400 0.038 Uiso 1 1 calc R . . C48 C 0.0637(4) 0.0106(3) 0.6917(2) 0.0322(10) Uani 1 1 d . . . H48 H -0.0038 -0.0291 0.6790 0.039 Uiso 1 1 calc R . . C49 C 0.0765(4) 0.0983(3) 0.7355(2) 0.0275(9) Uani 1 1 d . . . C50 C -0.0020(4) 0.1377(3) 0.7787(2) 0.0278(9) Uani 1 1 d . . . H50 H -0.0781 0.1132 0.7741 0.033 Uiso 1 1 calc R . . C51 C -0.0429(4) 0.2529(3) 0.8686(2) 0.0257(9) Uani 1 1 d . . . C52 C -0.1584(4) 0.2451(4) 0.8595(2) 0.0306(10) Uani 1 1 d . . . H52 H -0.1911 0.2091 0.8211 0.037 Uiso 1 1 calc R . . C53 C -0.2252(4) 0.2896(4) 0.9058(2) 0.0312(10) Uani 1 1 d . . . H53 H -0.3034 0.2824 0.8999 0.037 Uiso 1 1 calc R . . C54 C -0.1771(4) 0.3446(4) 0.9612(2) 0.0320(10) Uani 1 1 d . . . H54 H -0.2230 0.3739 0.9933 0.038 Uiso 1 1 calc R . . C55 C -0.0624(4) 0.3574(3) 0.9701(2) 0.0287(10) Uani 1 1 d . . . H55 H -0.0302 0.3965 1.0076 0.034 Uiso 1 1 calc R . . C56 C 0.0050(4) 0.3124(3) 0.9235(2) 0.0266(9) Uani 1 1 d . . . C57 C 0.1761(4) 0.3834(4) 0.9802(2) 0.0309(10) Uani 1 1 d . . . H57A H 0.1373 0.4462 0.9903 0.037 Uiso 1 1 calc R . . H57B H 0.2524 0.4052 0.9674 0.037 Uiso 1 1 calc R . . C58 C 0.1811(5) 0.3245(4) 1.0409(2) 0.0398(12) Uani 1 1 d . . . H58A H 0.1503 0.2522 1.0300 0.048 Uiso 1 1 calc R . . H58B H 0.2594 0.3235 1.0547 0.048 Uiso 1 1 calc R . . C59 C 0.1839(4) 0.4326(4) 1.1431(2) 0.0372(11) Uani 1 1 d . . . H59A H 0.1601 0.5033 1.1457 0.045 Uiso 1 1 calc R . . H59B H 0.2634 0.4365 1.1324 0.045 Uiso 1 1 calc R . . C60 C 0.1673(4) 0.3882(4) 1.2077(2) 0.0373(11) Uani 1 1 d . . . H60A H 0.1970 0.4391 1.2433 0.045 Uiso 1 1 calc R . . H60B H 0.0873 0.3715 1.2147 0.045 Uiso 1 1 calc R . . C61 C 0.1851(5) 0.2318(4) 1.2556(3) 0.0428(12) Uani 1 1 d . . . H61A H 0.1032 0.2202 1.2531 0.051 Uiso 1 1 calc R . . H61B H 0.2071 0.2646 1.2993 0.051 Uiso 1 1 calc R . . C62 C 0.2356(5) 0.1294(4) 1.2438(3) 0.0460(13) Uani 1 1 d . . . H62A H 0.3150 0.1436 1.2344 0.055 Uiso 1 1 calc R . . H62B H 0.2309 0.0942 1.2842 0.055 Uiso 1 1 calc R . . C63 C 0.1977(5) 0.0996(4) 1.1306(2) 0.0384(11) Uani 1 1 d . . . H63A H 0.2767 0.1200 1.1228 0.046 Uiso 1 1 calc R . . H63B H 0.1554 0.1604 1.1275 0.046 Uiso 1 1 calc R . . C64 C 0.1542(4) 0.0136(4) 1.0819(2) 0.0341(11) Uani 1 1 d . . . H64A H 0.1936 -0.0486 1.0863 0.041 Uiso 1 1 calc R . . H64B H 0.0740 -0.0040 1.0876 0.041 Uiso 1 1 calc R . . C65 C 0.1516(4) -0.0158(4) 0.9662(2) 0.0313(10) Uani 1 1 d . . . C66 C 0.1006(4) -0.1145(4) 0.9674(2) 0.0381(11) Uani 1 1 d . . . H66 H 0.0795 -0.1386 1.0078 0.046 Uiso 1 1 calc R . . C67 C 0.0797(4) -0.1791(4) 0.9112(3) 0.0394(12) Uani 1 1 d . . . H67 H 0.0457 -0.2470 0.9134 0.047 Uiso 1 1 calc R . . C68 C 0.1082(4) -0.1446(4) 0.8520(2) 0.0369(11) Uani 1 1 d . . . H68 H 0.0921 -0.1882 0.8133 0.044 Uiso 1 1 calc R . . C69 C 0.1606(4) -0.0459(4) 0.8494(2) 0.0350(11) Uani 1 1 d . . . H69 H 0.1798 -0.0227 0.8085 0.042 Uiso 1 1 calc R . . C70 C 0.1855(4) 0.0196(3) 0.9054(2) 0.0288(10) Uani 1 1 d . . . N1 N 0.2408(3) 0.1183(3) 0.89928(18) 0.0279(8) Uani 1 1 d . . . N2 N 0.3523(3) 0.3008(3) 0.87636(18) 0.0278(8) Uani 1 1 d . . . N3 N 0.2116(3) 0.4055(3) 0.78150(18) 0.0270(8) Uani 1 1 d . . . N4 N 0.0367(3) 0.3284(3) 0.70007(18) 0.0277(8) Uani 1 1 d . . . N5 N 0.2556(3) 0.4272(3) 0.62652(18) 0.0286(8) Uani 1 1 d . . . N6 N 0.3390(3) 0.2452(3) 0.64674(18) 0.0284(8) Uani 1 1 d . . . N7 N 0.1885(3) 0.1361(3) 0.74176(17) 0.0253(8) Uani 1 1 d . . . N8 N 0.0317(3) 0.2085(3) 0.82496(18) 0.0263(8) Uani 1 1 d . . . O1 O 0.0948(3) 0.2127(3) 0.59858(16) 0.0344(8) Uani 1 1 d . . . O2 O 0.1905(3) 0.1267(3) 0.43532(19) 0.0498(10) Uani 1 1 d . . . O3 O 0.3523(3) 0.2945(3) 0.41971(19) 0.0503(10) Uani 1 1 d . . . O4 O 0.2678(4) 0.4741(3) 0.35888(19) 0.0532(10) Uani 1 1 d . . . O5 O 0.1837(3) 0.4884(3) 0.50610(16) 0.0433(9) Uani 1 1 d . . . O6 O 0.1192(2) 0.3212(2) 0.92657(15) 0.0277(7) Uani 1 1 d . . . O7 O 0.1209(3) 0.3692(3) 1.09345(16) 0.0398(8) Uani 1 1 d . . . O8 O 0.2236(3) 0.2977(3) 1.20736(17) 0.0397(8) Uani 1 1 d . . . O9 O 0.1854(3) 0.0621(3) 1.19287(17) 0.0441(9) Uani 1 1 d . . . O10 O 0.1741(3) 0.0518(2) 1.01983(16) 0.0357(8) Uani 1 1 d . . . Fe01 Fe 0.20710(5) 0.30624(5) 0.69174(3) 0.0277(2) Uani 1 1 d . . . Fe02 Fe 0.20755(5) 0.23370(5) 0.83271(3) 0.0263(2) Uani 1 1 d . . . C101 C 0.4667(8) 1.0003(9) 0.0648(7) 0.143(5) Uani 1 1 d DU . . H101 H 0.4409 0.9969 0.1077 0.172 Uiso 1 1 calc R . . C102 C 0.4193(8) 0.9311(8) 0.0145(6) 0.115(4) Uani 1 1 d DU . . H102 H 0.3617 0.8825 0.0262 0.139 Uiso 1 1 calc R . . C103 C 0.4473(8) 0.9250(7) -0.0519(6) 0.155(5) Uani 1 1 d DU . . H103 H 0.4120 0.8762 -0.0841 0.186 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.021(2) 0.030(2) 0.033(2) 0.0070(18) 0.0007(18) 0.0050(18) C2 0.022(2) 0.028(2) 0.030(2) 0.0046(17) 0.0031(17) 0.0055(18) C3 0.026(2) 0.037(3) 0.034(3) 0.005(2) -0.0044(19) 0.0018(19) C4 0.024(2) 0.035(3) 0.039(3) 0.006(2) -0.0001(19) 0.0009(19) C5 0.020(2) 0.031(2) 0.031(2) 0.0039(18) 0.0036(17) -0.0036(18) C6 0.027(2) 0.031(2) 0.029(2) 0.0047(18) 0.0028(18) 0.0012(18) C7 0.027(2) 0.030(2) 0.044(3) 0.005(2) 0.000(2) -0.0033(19) C8 0.049(3) 0.034(3) 0.055(3) 0.015(2) 0.001(3) -0.010(2) C9 0.025(2) 0.035(3) 0.031(2) 0.0081(19) 0.0030(18) 0.0005(19) C10 0.027(3) 0.058(3) 0.041(3) 0.009(2) 0.005(2) 0.000(2) C11 0.026(2) 0.024(2) 0.029(2) 0.0132(17) -0.0004(17) -0.0012(17) C12 0.031(2) 0.025(2) 0.028(2) 0.0035(17) 0.0004(18) -0.0009(18) C13 0.030(3) 0.030(2) 0.031(2) 0.0061(18) 0.0028(19) 0.0063(19) C14 0.024(2) 0.031(2) 0.032(2) 0.0100(18) -0.0005(18) 0.0017(18) C15 0.024(2) 0.032(2) 0.035(2) 0.0115(19) 0.0028(18) 0.0060(19) C16 0.026(2) 0.033(2) 0.033(2) 0.0127(19) -0.0033(18) -0.0003(19) C17 0.023(2) 0.038(3) 0.038(3) 0.009(2) 0.0013(19) -0.0018(19) C18 0.027(3) 0.051(3) 0.044(3) 0.013(2) 0.001(2) -0.005(2) C19 0.036(3) 0.043(3) 0.053(3) 0.007(2) -0.010(2) -0.007(2) C20 0.037(3) 0.034(3) 0.042(3) 0.003(2) -0.002(2) -0.006(2) C21 0.029(3) 0.028(2) 0.039(3) 0.0061(19) -0.003(2) -0.0002(19) C22 0.034(3) 0.030(2) 0.038(3) -0.0017(19) -0.001(2) 0.002(2) C23 0.033(3) 0.044(3) 0.037(3) 0.003(2) -0.001(2) 0.007(2) C24 0.046(3) 0.049(3) 0.058(4) -0.001(3) 0.002(3) 0.007(3) C25 0.046(3) 0.052(3) 0.050(3) -0.004(3) 0.007(3) 0.009(3) C26 0.042(3) 0.080(5) 0.053(4) 0.010(3) 0.011(3) -0.011(3) C27 0.056(4) 0.048(3) 0.053(4) 0.013(3) -0.005(3) -0.005(3) C28 0.053(4) 0.050(3) 0.043(3) 0.009(2) -0.001(3) -0.003(3) C29 0.056(4) 0.041(3) 0.035(3) 0.008(2) -0.007(2) 0.003(3) C30 0.036(3) 0.034(3) 0.035(3) 0.003(2) -0.001(2) -0.003(2) C31 0.049(3) 0.039(3) 0.045(3) 0.015(2) -0.006(2) 0.013(2) C32 0.053(4) 0.034(3) 0.052(3) 0.001(2) -0.001(3) 0.010(2) C33 0.050(3) 0.036(3) 0.046(3) 0.001(2) 0.001(2) 0.006(2) C34 0.043(3) 0.036(3) 0.031(3) 0.010(2) 0.000(2) 0.005(2) C35 0.030(3) 0.030(2) 0.032(2) 0.0061(19) 0.0001(19) -0.0006(19) C36 0.031(3) 0.032(2) 0.029(2) 0.0063(18) -0.0032(19) -0.0057(19) C37 0.026(2) 0.034(3) 0.034(2) 0.0068(19) 0.0018(19) -0.0003(19) C38 0.029(3) 0.035(3) 0.040(3) 0.008(2) 0.005(2) -0.003(2) C39 0.022(2) 0.049(3) 0.042(3) 0.003(2) 0.003(2) 0.008(2) C40 0.017(2) 0.035(3) 0.036(2) 0.0056(19) 0.0008(18) 0.0004(18) C41 0.028(3) 0.033(3) 0.037(3) 0.0043(19) 0.0073(19) 0.0050(19) C42 0.030(3) 0.036(3) 0.045(3) 0.003(2) 0.009(2) 0.006(2) C43 0.042(3) 0.040(3) 0.060(4) 0.009(3) 0.010(3) 0.014(2) C44 0.028(3) 0.039(3) 0.038(3) 0.008(2) 0.002(2) 0.007(2) C45 0.028(3) 0.054(3) 0.045(3) 0.008(2) -0.001(2) 0.004(2) C46 0.022(2) 0.028(2) 0.034(2) 0.0069(18) 0.0039(18) 0.0049(18) C47 0.031(3) 0.027(2) 0.035(3) -0.0007(18) 0.0024(19) 0.0005(19) C48 0.027(2) 0.027(2) 0.041(3) 0.0036(19) 0.000(2) -0.0047(19) C49 0.022(2) 0.028(2) 0.033(2) 0.0098(18) -0.0006(18) -0.0014(18) C50 0.025(2) 0.029(2) 0.030(2) 0.0074(18) -0.0007(18) 0.0006(18) C51 0.024(2) 0.027(2) 0.028(2) 0.0099(17) 0.0043(17) 0.0043(18) C52 0.029(2) 0.030(2) 0.034(2) 0.0084(19) 0.0025(19) 0.0040(19) C53 0.021(2) 0.033(2) 0.042(3) 0.010(2) 0.0074(19) 0.0049(18) C54 0.026(2) 0.032(2) 0.038(3) 0.0072(19) 0.0106(19) 0.0039(19) C55 0.027(2) 0.029(2) 0.031(2) 0.0072(18) 0.0027(18) 0.0056(19) C56 0.025(2) 0.027(2) 0.030(2) 0.0121(18) 0.0023(18) 0.0040(18) C57 0.025(2) 0.032(2) 0.035(3) 0.0028(19) -0.0022(19) 0.0002(19) C58 0.039(3) 0.049(3) 0.033(3) 0.003(2) 0.002(2) 0.013(2) C59 0.029(3) 0.038(3) 0.043(3) 0.006(2) 0.001(2) -0.006(2) C60 0.040(3) 0.036(3) 0.035(3) 0.001(2) -0.001(2) 0.004(2) C61 0.044(3) 0.051(3) 0.035(3) 0.010(2) -0.002(2) 0.008(2) C62 0.050(3) 0.045(3) 0.043(3) 0.006(2) -0.007(2) 0.007(3) C63 0.046(3) 0.036(3) 0.035(3) 0.010(2) 0.000(2) 0.003(2) C64 0.036(3) 0.033(3) 0.035(3) 0.010(2) 0.006(2) 0.000(2) C65 0.029(2) 0.030(2) 0.037(3) 0.0091(19) 0.0020(19) 0.0034(19) C66 0.039(3) 0.039(3) 0.038(3) 0.014(2) 0.005(2) -0.002(2) C67 0.041(3) 0.032(3) 0.045(3) 0.008(2) 0.000(2) -0.003(2) C68 0.042(3) 0.031(3) 0.036(3) 0.006(2) -0.002(2) -0.004(2) C69 0.032(3) 0.037(3) 0.038(3) 0.013(2) 0.002(2) 0.004(2) C70 0.028(2) 0.025(2) 0.033(2) 0.0067(18) 0.0002(18) 0.0022(18) N1 0.0225(19) 0.031(2) 0.031(2) 0.0072(15) 0.0013(15) -0.0001(15) N2 0.0199(19) 0.030(2) 0.035(2) 0.0060(15) 0.0038(15) 0.0028(15) N3 0.024(2) 0.028(2) 0.031(2) 0.0053(15) 0.0019(15) 0.0039(15) N4 0.026(2) 0.0263(19) 0.032(2) 0.0067(15) 0.0003(15) 0.0018(15) N5 0.026(2) 0.028(2) 0.032(2) 0.0049(15) 0.0018(16) 0.0002(15) N6 0.023(2) 0.030(2) 0.032(2) 0.0055(16) 0.0040(15) -0.0007(15) N7 0.0195(18) 0.029(2) 0.0273(19) 0.0034(15) 0.0003(14) 0.0013(15) N8 0.0220(19) 0.029(2) 0.0288(19) 0.0112(15) 0.0009(15) 0.0002(15) O1 0.0258(17) 0.0364(18) 0.0401(19) 0.0021(14) -0.0007(14) -0.0001(14) O2 0.048(2) 0.055(2) 0.043(2) -0.0033(17) 0.0014(17) -0.0035(18) O3 0.051(2) 0.057(2) 0.045(2) 0.0127(18) 0.0085(18) 0.0044(19) O4 0.051(2) 0.064(3) 0.045(2) 0.0094(18) 0.0002(18) -0.003(2) O5 0.057(2) 0.045(2) 0.0296(18) 0.0079(15) -0.0042(16) 0.0114(18) O6 0.0173(15) 0.0328(17) 0.0330(17) 0.0037(13) -0.0019(12) 0.0006(12) O7 0.0271(18) 0.055(2) 0.0347(19) -0.0021(15) 0.0007(14) -0.0034(16) O8 0.039(2) 0.041(2) 0.0402(19) 0.0043(15) -0.0008(15) 0.0063(16) O9 0.055(2) 0.041(2) 0.0353(19) 0.0072(15) -0.0054(17) -0.0015(17) O10 0.044(2) 0.0322(18) 0.0305(17) 0.0074(14) 0.0057(15) -0.0020(15) Fe01 0.0231(4) 0.0299(4) 0.0310(4) 0.0058(3) 0.0034(3) 0.0035(3) Fe02 0.0211(4) 0.0280(4) 0.0299(4) 0.0069(3) -0.0005(3) -0.0006(3) C101 0.101(8) 0.146(10) 0.216(12) 0.113(9) 0.072(8) 0.091(8) C102 0.063(5) 0.104(7) 0.206(11) 0.116(8) 0.065(7) 0.042(5) C103 0.082(6) 0.143(8) 0.279(13) 0.152(9) 0.059(7) 0.085(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.300(6) . ? C1 C2 1.425(6) . ? C1 H1 0.9500 . ? C2 N2 1.388(6) . ? C2 C3 1.394(6) . ? C3 C4 1.400(7) . ? C3 H3 0.9500 . ? C4 C5 1.401(6) . ? C4 H4 0.9500 . ? C5 N2 1.353(6) . ? C5 C6 1.526(6) . ? C6 C11 1.517(6) . ? C6 C7 1.549(6) . ? C6 C9 1.551(6) . ? C7 C8 1.528(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.536(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N3 1.379(6) . ? C11 C12 1.401(6) . ? C12 C13 1.407(7) . ? C12 H12 0.9500 . ? C13 C14 1.392(7) . ? C13 H13 0.9500 . ? C14 N3 1.408(6) . ? C14 C15 1.410(6) . ? C15 N4 1.308(6) . ? C15 H15 0.9500 . ? C16 C17 1.390(7) . ? C16 N4 1.413(6) . ? C16 C21 1.417(7) . ? C17 C18 1.394(7) . ? C17 H17 0.9500 . ? C18 C19 1.376(8) . ? C18 H18 0.9500 . ? C19 C20 1.407(8) . ? C19 H19 0.9500 . ? C20 C21 1.381(7) . ? C20 H20 0.9500 . ? C21 O1 1.386(6) . ? C22 O1 1.452(6) . ? C22 C23 1.523(7) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 O2 1.435(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O2 1.449(7) . ? C24 C25 1.498(9) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 O3 1.403(7) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O3 1.437(7) . ? C26 C27 1.515(9) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 O4 1.420(7) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O4 1.418(7) . ? C28 C29 1.501(8) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O5 1.439(6) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 O5 1.382(6) . ? C30 C31 1.400(7) . ? C30 C35 1.403(7) . ? C31 C32 1.379(8) . ? C31 H31 0.9500 . ? C32 C33 1.374(8) . ? C32 H32 0.9500 . ? C33 C34 1.390(7) . ? C33 H33 0.9500 . ? C34 C35 1.391(7) . ? C34 H34 0.9500 . ? C35 N5 1.439(6) . ? C36 N5 1.301(6) . ? C36 C37 1.423(7) . ? C36 H36 0.9500 . ? C37 C38 1.386(7) . ? C37 N6 1.394(6) . ? C38 C39 1.412(7) . ? C38 H38 0.9500 . ? C39 C40 1.398(7) . ? C39 H39 0.9500 . ? C40 N6 1.359(6) . ? C40 C41 1.531(7) . ? C41 C46 1.525(6) . ? C41 C42 1.548(6) . ? C41 C44 1.548(7) . ? C42 C43 1.528(7) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.532(7) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 N7 1.383(5) . ? C46 C47 1.396(6) . ? C47 C48 1.393(7) . ? C47 H47 0.9500 . ? C48 C49 1.394(7) . ? C48 H48 0.9500 . ? C49 N7 1.403(6) . ? C49 C50 1.414(6) . ? C50 N8 1.307(6) . ? C50 H50 0.9500 . ? C51 C52 1.404(6) . ? C51 C56 1.408(6) . ? C51 N8 1.412(6) . ? C52 C53 1.387(6) . ? C52 H52 0.9500 . ? C53 C54 1.391(7) . ? C53 H53 0.9500 . ? C54 C55 1.393(7) . ? C54 H54 0.9500 . ? C55 C56 1.396(6) . ? C55 H55 0.9500 . ? C56 O6 1.379(5) . ? C57 O6 1.446(5) . ? C57 C58 1.536(7) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 O7 1.430(6) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 O7 1.430(6) . ? C59 C60 1.516(7) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 O8 1.418(6) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 O8 1.433(6) . ? C61 C62 1.522(8) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 O9 1.408(6) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 O9 1.426(6) . ? C63 C64 1.497(7) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 O10 1.436(5) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 O10 1.366(6) . ? C65 C66 1.384(7) . ? C65 C70 1.434(6) . ? C66 C67 1.382(7) . ? C66 H66 0.9500 . ? C67 C68 1.382(7) . ? C67 H67 0.9500 . ? C68 C69 1.394(7) . ? C68 H68 0.9500 . ? C69 C70 1.393(7) . ? C69 H69 0.9500 . ? C70 N1 1.418(6) . ? N1 Fe02 2.192(4) . ? N2 Fe02 2.052(4) . ? N3 Fe01 2.169(4) . ? N4 Fe01 2.118(4) . ? N5 Fe01 2.216(4) . ? N6 Fe01 2.049(4) . ? N7 Fe02 2.178(4) . ? N8 Fe02 2.130(4) . ? C101 C102 1.402(7) . ? C101 C103 1.408(7) 2_675 ? C101 H101 0.9500 . ? C102 C103 1.419(7) . ? C102 H102 0.9500 . ? C103 C101 1.408(7) 2_675 ? C103 H103 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 119.7(4) . . ? N1 C1 H1 120.2 . . ? C2 C1 H1 120.2 . . ? N2 C2 C3 109.9(4) . . ? N2 C2 C1 117.8(4) . . ? C3 C2 C1 132.3(4) . . ? C2 C3 C4 106.5(4) . . ? C2 C3 H3 126.7 . . ? C4 C3 H3 126.7 . . ? C3 C4 C5 106.5(4) . . ? C3 C4 H4 126.8 . . ? C5 C4 H4 126.8 . . ? N2 C5 C4 110.6(4) . . ? N2 C5 C6 119.2(4) . . ? C4 C5 C6 130.1(4) . . ? C11 C6 C5 107.0(4) . . ? C11 C6 C7 110.3(4) . . ? C5 C6 C7 109.2(4) . . ? C11 C6 C9 109.9(4) . . ? C5 C6 C9 109.7(4) . . ? C7 C6 C9 110.7(4) . . ? C8 C7 C6 115.4(4) . . ? C8 C7 H7A 108.4 . . ? C6 C7 H7A 108.4 . . ? C8 C7 H7B 108.4 . . ? C6 C7 H7B 108.4 . . ? H7A C7 H7B 107.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C6 115.1(4) . . ? C10 C9 H9A 108.5 . . ? C6 C9 H9A 108.5 . . ? C10 C9 H9B 108.5 . . ? C6 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 C12 110.3(4) . . ? N3 C11 C6 123.0(4) . . ? C12 C11 C6 126.6(4) . . ? C11 C12 C13 107.7(4) . . ? C11 C12 H12 126.2 . . ? C13 C12 H12 126.2 . . ? C14 C13 C12 105.8(4) . . ? C14 C13 H13 127.1 . . ? C12 C13 H13 127.1 . . ? C13 C14 N3 111.0(4) . . ? C13 C14 C15 129.1(4) . . ? N3 C14 C15 119.0(4) . . ? N4 C15 C14 120.3(4) . . ? N4 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C17 C16 N4 125.1(4) . . ? C17 C16 C21 118.5(4) . . ? N4 C16 C21 116.5(4) . . ? C16 C17 C18 121.5(5) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C19 C18 C17 119.2(5) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C18 C19 C20 121.0(5) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C21 C20 C19 119.4(5) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C20 C21 O1 125.0(4) . . ? C20 C21 C16 120.5(5) . . ? O1 C21 C16 114.6(4) . . ? O1 C22 C23 110.9(4) . . ? O1 C22 H22A 109.5 . . ? C23 C22 H22A 109.5 . . ? O1 C22 H22B 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 108.0 . . ? O2 C23 C22 110.0(4) . . ? O2 C23 H23A 109.7 . . ? C22 C23 H23A 109.7 . . ? O2 C23 H23B 109.7 . . ? C22 C23 H23B 109.7 . . ? H23A C23 H23B 108.2 . . ? O2 C24 C25 113.0(5) . . ? O2 C24 H24A 109.0 . . ? C25 C24 H24A 109.0 . . ? O2 C24 H24B 109.0 . . ? C25 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? O3 C25 C24 110.3(5) . . ? O3 C25 H25A 109.6 . . ? C24 C25 H25A 109.6 . . ? O3 C25 H25B 109.6 . . ? C24 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? O3 C26 C27 107.7(5) . . ? O3 C26 H26A 110.2 . . ? C27 C26 H26A 110.2 . . ? O3 C26 H26B 110.2 . . ? C27 C26 H26B 110.2 . . ? H26A C26 H26B 108.5 . . ? O4 C27 C26 113.7(5) . . ? O4 C27 H27A 108.8 . . ? C26 C27 H27A 108.8 . . ? O4 C27 H27B 108.8 . . ? C26 C27 H27B 108.8 . . ? H27A C27 H27B 107.7 . . ? O4 C28 C29 114.2(5) . . ? O4 C28 H28A 108.7 . . ? C29 C28 H28A 108.7 . . ? O4 C28 H28B 108.7 . . ? C29 C28 H28B 108.7 . . ? H28A C28 H28B 107.6 . . ? O5 C29 C28 109.1(4) . . ? O5 C29 H29A 109.9 . . ? C28 C29 H29A 109.9 . . ? O5 C29 H29B 109.9 . . ? C28 C29 H29B 109.9 . . ? H29A C29 H29B 108.3 . . ? O5 C30 C31 123.4(5) . . ? O5 C30 C35 116.6(4) . . ? C31 C30 C35 119.9(5) . . ? C32 C31 C30 120.3(5) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C33 C32 C31 120.6(5) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 C34 119.3(5) . . ? C32 C33 H33 120.4 . . ? C34 C33 H33 120.4 . . ? C33 C34 C35 121.8(5) . . ? C33 C34 H34 119.1 . . ? C35 C34 H34 119.1 . . ? C34 C35 C30 118.1(4) . . ? C34 C35 N5 117.4(4) . . ? C30 C35 N5 124.4(4) . . ? N5 C36 C37 119.6(4) . . ? N5 C36 H36 120.2 . . ? C37 C36 H36 120.2 . . ? C38 C37 N6 109.2(4) . . ? C38 C37 C36 132.5(5) . . ? N6 C37 C36 118.3(4) . . ? C37 C38 C39 106.7(4) . . ? C37 C38 H38 126.6 . . ? C39 C38 H38 126.6 . . ? C40 C39 C38 107.0(4) . . ? C40 C39 H39 126.5 . . ? C38 C39 H39 126.5 . . ? N6 C40 C39 109.5(4) . . ? N6 C40 C41 120.1(4) . . ? C39 C40 C41 130.3(4) . . ? C46 C41 C40 107.2(4) . . ? C46 C41 C42 110.1(4) . . ? C40 C41 C42 108.5(4) . . ? C46 C41 C44 110.1(4) . . ? C40 C41 C44 110.7(4) . . ? C42 C41 C44 110.3(4) . . ? C43 C42 C41 114.6(4) . . ? C43 C42 H42A 108.6 . . ? C41 C42 H42A 108.6 . . ? C43 C42 H42B 108.6 . . ? C41 C42 H42B 108.6 . . ? H42A C42 H42B 107.6 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 C41 116.3(4) . . ? C45 C44 H44A 108.2 . . ? C41 C44 H44A 108.2 . . ? C45 C44 H44B 108.2 . . ? C41 C44 H44B 108.2 . . ? H44A C44 H44B 107.4 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N7 C46 C47 110.2(4) . . ? N7 C46 C41 122.7(4) . . ? C47 C46 C41 127.1(4) . . ? C48 C47 C46 107.7(4) . . ? C48 C47 H47 126.2 . . ? C46 C47 H47 126.2 . . ? C47 C48 C49 106.5(4) . . ? C47 C48 H48 126.8 . . ? C49 C48 H48 126.8 . . ? C48 C49 N7 110.4(4) . . ? C48 C49 C50 128.3(4) . . ? N7 C49 C50 120.3(4) . . ? N8 C50 C49 119.0(4) . . ? N8 C50 H50 120.5 . . ? C49 C50 H50 120.5 . . ? C52 C51 C56 119.0(4) . . ? C52 C51 N8 124.8(4) . . ? C56 C51 N8 116.2(4) . . ? C53 C52 C51 120.6(4) . . ? C53 C52 H52 119.7 . . ? C51 C52 H52 119.7 . . ? C52 C53 C54 119.7(4) . . ? C52 C53 H53 120.2 . . ? C54 C53 H53 120.2 . . ? C55 C54 C53 120.8(4) . . ? C55 C54 H54 119.6 . . ? C53 C54 H54 119.6 . . ? C54 C55 C56 119.5(4) . . ? C54 C55 H55 120.2 . . ? C56 C55 H55 120.2 . . ? O6 C56 C55 124.7(4) . . ? O6 C56 C51 115.1(4) . . ? C55 C56 C51 120.2(4) . . ? O6 C57 C58 111.9(4) . . ? O6 C57 H57A 109.2 . . ? C58 C57 H57A 109.2 . . ? O6 C57 H57B 109.2 . . ? C58 C57 H57B 109.2 . . ? H57A C57 H57B 107.9 . . ? O7 C58 C57 112.6(4) . . ? O7 C58 H58A 109.1 . . ? C57 C58 H58A 109.1 . . ? O7 C58 H58B 109.1 . . ? C57 C58 H58B 109.1 . . ? H58A C58 H58B 107.8 . . ? O7 C59 C60 110.0(4) . . ? O7 C59 H59A 109.7 . . ? C60 C59 H59A 109.7 . . ? O7 C59 H59B 109.7 . . ? C60 C59 H59B 109.7 . . ? H59A C59 H59B 108.2 . . ? O8 C60 C59 108.5(4) . . ? O8 C60 H60A 110.0 . . ? C59 C60 H60A 110.0 . . ? O8 C60 H60B 110.0 . . ? C59 C60 H60B 110.0 . . ? H60A C60 H60B 108.4 . . ? O8 C61 C62 108.8(4) . . ? O8 C61 H61A 109.9 . . ? C62 C61 H61A 109.9 . . ? O8 C61 H61B 109.9 . . ? C62 C61 H61B 109.9 . . ? H61A C61 H61B 108.3 . . ? O9 C62 C61 114.9(4) . . ? O9 C62 H62A 108.5 . . ? C61 C62 H62A 108.5 . . ? O9 C62 H62B 108.5 . . ? C61 C62 H62B 108.5 . . ? H62A C62 H62B 107.5 . . ? O9 C63 C64 106.8(4) . . ? O9 C63 H63A 110.4 . . ? C64 C63 H63A 110.4 . . ? O9 C63 H63B 110.4 . . ? C64 C63 H63B 110.4 . . ? H63A C63 H63B 108.6 . . ? O10 C64 C63 105.3(4) . . ? O10 C64 H64A 110.7 . . ? C63 C64 H64A 110.7 . . ? O10 C64 H64B 110.7 . . ? C63 C64 H64B 110.7 . . ? H64A C64 H64B 108.8 . . ? O10 C65 C66 124.4(4) . . ? O10 C65 C70 116.4(4) . . ? C66 C65 C70 119.2(4) . . ? C67 C66 C65 121.6(5) . . ? C67 C66 H66 119.2 . . ? C65 C66 H66 119.2 . . ? C66 C67 C68 119.9(5) . . ? C66 C67 H67 120.0 . . ? C68 C67 H67 120.0 . . ? C67 C68 C69 119.8(5) . . ? C67 C68 H68 120.1 . . ? C69 C68 H68 120.1 . . ? C68 C69 C70 121.4(4) . . ? C68 C69 H69 119.3 . . ? C70 C69 H69 119.3 . . ? C69 C70 N1 118.5(4) . . ? C69 C70 C65 118.0(4) . . ? N1 C70 C65 123.4(4) . . ? C1 N1 C70 120.1(4) . . ? C1 N1 Fe02 109.9(3) . . ? C70 N1 Fe02 129.9(3) . . ? C5 N2 C2 106.4(4) . . ? C5 N2 Fe02 140.2(3) . . ? C2 N2 Fe02 112.0(3) . . ? C11 N3 C14 105.1(4) . . ? C11 N3 Fe01 141.8(3) . . ? C14 N3 Fe01 107.6(3) . . ? C15 N4 C16 121.6(4) . . ? C15 N4 Fe01 112.3(3) . . ? C16 N4 Fe01 126.0(3) . . ? C36 N5 C35 120.9(4) . . ? C36 N5 Fe01 109.9(3) . . ? C35 N5 Fe01 129.2(3) . . ? C40 N6 C37 107.5(4) . . ? C40 N6 Fe01 139.8(3) . . ? C37 N6 Fe01 112.5(3) . . ? C46 N7 C49 105.2(4) . . ? C46 N7 Fe02 141.8(3) . . ? C49 N7 Fe02 107.0(3) . . ? C50 N8 C51 121.8(4) . . ? C50 N8 Fe02 112.6(3) . . ? C51 N8 Fe02 125.2(3) . . ? C21 O1 C22 118.8(4) . . ? C23 O2 C24 112.2(4) . . ? C25 O3 C26 113.0(5) . . ? C28 O4 C27 114.6(4) . . ? C30 O5 C29 116.1(4) . . ? C56 O6 C57 119.2(3) . . ? C59 O7 C58 117.0(4) . . ? C60 O8 C61 112.9(4) . . ? C62 O9 C63 114.0(4) . . ? C65 O10 C64 117.3(4) . . ? N6 Fe01 N4 153.25(15) . . ? N6 Fe01 N3 126.83(15) . . ? N4 Fe01 N3 79.92(14) . . ? N6 Fe01 N5 79.48(14) . . ? N4 Fe01 N5 99.14(14) . . ? N3 Fe01 N5 97.47(14) . . ? N2 Fe02 N8 152.87(15) . . ? N2 Fe02 N7 127.44(14) . . ? N8 Fe02 N7 79.57(14) . . ? N2 Fe02 N1 79.60(14) . . ? N8 Fe02 N1 99.84(14) . . ? N7 Fe02 N1 100.09(14) . . ? C102 C101 C103 120.1(12) . 2_675 ? C102 C101 H101 119.9 . . ? C103 C101 H101 120.0 2_675 . ? C101 C102 C103 127.6(9) . . ? C101 C102 H102 116.2 . . ? C103 C102 H102 116.2 . . ? C102 C103 C101 112.3(10) . 2_675 ? C102 C103 H103 123.8 . . ? C101 C103 H103 123.8 2_675 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 -2.7(6) . . . . ? N1 C1 C2 C3 175.5(5) . . . . ? N2 C2 C3 C4 -0.1(5) . . . . ? C1 C2 C3 C4 -178.4(5) . . . . ? C2 C3 C4 C5 0.1(5) . . . . ? C3 C4 C5 N2 -0.1(5) . . . . ? C3 C4 C5 C6 -179.8(4) . . . . ? N2 C5 C6 C11 46.0(5) . . . . ? C4 C5 C6 C11 -134.2(5) . . . . ? N2 C5 C6 C7 165.4(4) . . . . ? C4 C5 C6 C7 -14.9(7) . . . . ? N2 C5 C6 C9 -73.2(5) . . . . ? C4 C5 C6 C9 106.6(5) . . . . ? C11 C6 C7 C8 -65.1(5) . . . . ? C5 C6 C7 C8 177.6(4) . . . . ? C9 C6 C7 C8 56.8(5) . . . . ? C11 C6 C9 C10 176.8(4) . . . . ? C5 C6 C9 C10 -65.8(5) . . . . ? C7 C6 C9 C10 54.8(5) . . . . ? C5 C6 C11 N3 -83.5(5) . . . . ? C7 C6 C11 N3 157.8(4) . . . . ? C9 C6 C11 N3 35.6(6) . . . . ? C5 C6 C11 C12 92.4(5) . . . . ? C7 C6 C11 C12 -26.3(6) . . . . ? C9 C6 C11 C12 -148.5(4) . . . . ? N3 C11 C12 C13 -0.4(5) . . . . ? C6 C11 C12 C13 -176.7(4) . . . . ? C11 C12 C13 C14 -0.9(5) . . . . ? C12 C13 C14 N3 1.9(5) . . . . ? C12 C13 C14 C15 -167.2(5) . . . . ? C13 C14 C15 N4 166.2(5) . . . . ? N3 C14 C15 N4 -2.1(6) . . . . ? N4 C16 C17 C18 179.9(4) . . . . ? C21 C16 C17 C18 -2.0(7) . . . . ? C16 C17 C18 C19 0.6(8) . . . . ? C17 C18 C19 C20 1.2(8) . . . . ? C18 C19 C20 C21 -1.4(8) . . . . ? C19 C20 C21 O1 179.7(4) . . . . ? C19 C20 C21 C16 -0.1(7) . . . . ? C17 C16 C21 C20 1.8(7) . . . . ? N4 C16 C21 C20 180.0(4) . . . . ? C17 C16 C21 O1 -178.0(4) . . . . ? N4 C16 C21 O1 0.2(6) . . . . ? O1 C22 C23 O2 178.4(4) . . . . ? O2 C24 C25 O3 57.8(7) . . . . ? O3 C26 C27 O4 -76.1(6) . . . . ? O4 C28 C29 O5 -95.8(6) . . . . ? O5 C30 C31 C32 179.2(5) . . . . ? C35 C30 C31 C32 2.9(8) . . . . ? C30 C31 C32 C33 -1.7(9) . . . . ? C31 C32 C33 C34 -0.2(9) . . . . ? C32 C33 C34 C35 0.8(9) . . . . ? C33 C34 C35 C30 0.4(8) . . . . ? C33 C34 C35 N5 -177.1(5) . . . . ? O5 C30 C35 C34 -178.8(5) . . . . ? C31 C30 C35 C34 -2.2(8) . . . . ? O5 C30 C35 N5 -1.5(7) . . . . ? C31 C30 C35 N5 175.1(5) . . . . ? N5 C36 C37 C38 -178.8(5) . . . . ? N5 C36 C37 N6 0.7(7) . . . . ? N6 C37 C38 C39 0.4(6) . . . . ? C36 C37 C38 C39 179.9(5) . . . . ? C37 C38 C39 C40 0.1(6) . . . . ? C38 C39 C40 N6 -0.5(6) . . . . ? C38 C39 C40 C41 -177.4(5) . . . . ? N6 C40 C41 C46 39.8(6) . . . . ? C39 C40 C41 C46 -143.6(5) . . . . ? N6 C40 C41 C42 158.6(4) . . . . ? C39 C40 C41 C42 -24.8(7) . . . . ? N6 C40 C41 C44 -80.2(5) . . . . ? C39 C40 C41 C44 96.4(6) . . . . ? C46 C41 C42 C43 -67.5(6) . . . . ? C40 C41 C42 C43 175.6(4) . . . . ? C44 C41 C42 C43 54.2(6) . . . . ? C46 C41 C44 C45 176.5(4) . . . . ? C40 C41 C44 C45 -65.3(5) . . . . ? C42 C41 C44 C45 54.8(6) . . . . ? C40 C41 C46 N7 -82.5(5) . . . . ? C42 C41 C46 N7 159.8(4) . . . . ? C44 C41 C46 N7 38.0(6) . . . . ? C40 C41 C46 C47 97.7(5) . . . . ? C42 C41 C46 C47 -20.0(7) . . . . ? C44 C41 C46 C47 -141.8(5) . . . . ? N7 C46 C47 C48 -0.9(5) . . . . ? C41 C46 C47 C48 179.0(4) . . . . ? C46 C47 C48 C49 0.3(5) . . . . ? C47 C48 C49 N7 0.4(5) . . . . ? C47 C48 C49 C50 -168.0(4) . . . . ? C48 C49 C50 N8 166.3(4) . . . . ? N7 C49 C50 N8 -1.2(6) . . . . ? C56 C51 C52 C53 -4.3(6) . . . . ? N8 C51 C52 C53 178.6(4) . . . . ? C51 C52 C53 C54 1.7(7) . . . . ? C52 C53 C54 C55 1.2(7) . . . . ? C53 C54 C55 C56 -1.5(7) . . . . ? C54 C55 C56 O6 178.9(4) . . . . ? C54 C55 C56 C51 -1.2(6) . . . . ? C52 C51 C56 O6 -176.1(4) . . . . ? N8 C51 C56 O6 1.3(5) . . . . ? C52 C51 C56 C55 4.0(6) . . . . ? N8 C51 C56 C55 -178.6(4) . . . . ? O6 C57 C58 O7 -115.7(4) . . . . ? O7 C59 C60 O8 72.0(5) . . . . ? O8 C61 C62 O9 -77.6(6) . . . . ? O9 C63 C64 O10 -176.6(4) . . . . ? O10 C65 C66 C67 179.7(5) . . . . ? C70 C65 C66 C67 -1.3(8) . . . . ? C65 C66 C67 C68 -1.1(8) . . . . ? C66 C67 C68 C69 1.7(8) . . . . ? C67 C68 C69 C70 0.1(8) . . . . ? C68 C69 C70 N1 178.8(4) . . . . ? C68 C69 C70 C65 -2.5(7) . . . . ? O10 C65 C70 C69 -177.9(4) . . . . ? C66 C65 C70 C69 3.0(7) . . . . ? O10 C65 C70 N1 0.8(7) . . . . ? C66 C65 C70 N1 -178.3(4) . . . . ? C2 C1 N1 C70 176.0(4) . . . . ? C2 C1 N1 Fe02 -4.7(5) . . . . ? C69 C70 N1 C1 -134.3(5) . . . . ? C65 C70 N1 C1 47.1(6) . . . . ? C69 C70 N1 Fe02 46.5(6) . . . . ? C65 C70 N1 Fe02 -132.1(4) . . . . ? C4 C5 N2 C2 0.0(5) . . . . ? C6 C5 N2 C2 179.8(4) . . . . ? C4 C5 N2 Fe02 164.7(4) . . . . ? C6 C5 N2 Fe02 -15.5(7) . . . . ? C3 C2 N2 C5 0.1(5) . . . . ? C1 C2 N2 C5 178.6(4) . . . . ? C3 C2 N2 Fe02 -169.4(3) . . . . ? C1 C2 N2 Fe02 9.2(5) . . . . ? C12 C11 N3 C14 1.5(5) . . . . ? C6 C11 N3 C14 178.0(4) . . . . ? C12 C11 N3 Fe01 149.8(4) . . . . ? C6 C11 N3 Fe01 -33.7(7) . . . . ? C13 C14 N3 C11 -2.1(5) . . . . ? C15 C14 N3 C11 168.2(4) . . . . ? C13 C14 N3 Fe01 -162.2(3) . . . . ? C15 C14 N3 Fe01 8.2(5) . . . . ? C14 C15 N4 C16 176.5(4) . . . . ? C14 C15 N4 Fe01 -5.6(5) . . . . ? C17 C16 N4 C15 -10.1(7) . . . . ? C21 C16 N4 C15 171.8(4) . . . . ? C17 C16 N4 Fe01 172.3(3) . . . . ? C21 C16 N4 Fe01 -5.8(6) . . . . ? C37 C36 N5 C35 178.2(4) . . . . ? C37 C36 N5 Fe01 -3.7(5) . . . . ? C34 C35 N5 C36 -131.6(5) . . . . ? C30 C35 N5 C36 51.1(7) . . . . ? C34 C35 N5 Fe01 50.8(6) . . . . ? C30 C35 N5 Fe01 -126.6(4) . . . . ? C39 C40 N6 C37 0.8(5) . . . . ? C41 C40 N6 C37 178.0(4) . . . . ? C39 C40 N6 Fe01 176.0(4) . . . . ? C41 C40 N6 Fe01 -6.7(7) . . . . ? C38 C37 N6 C40 -0.7(5) . . . . ? C36 C37 N6 C40 179.7(4) . . . . ? C38 C37 N6 Fe01 -177.4(3) . . . . ? C36 C37 N6 Fe01 3.0(5) . . . . ? C47 C46 N7 C49 1.1(5) . . . . ? C41 C46 N7 C49 -178.8(4) . . . . ? C47 C46 N7 Fe02 147.7(4) . . . . ? C41 C46 N7 Fe02 -32.1(7) . . . . ? C48 C49 N7 C46 -0.9(5) . . . . ? C50 C49 N7 C46 168.6(4) . . . . ? C48 C49 N7 Fe02 -160.1(3) . . . . ? C50 C49 N7 Fe02 9.4(5) . . . . ? C49 C50 N8 C51 178.4(4) . . . . ? C49 C50 N8 Fe02 -8.3(5) . . . . ? C52 C51 N8 C50 -15.0(6) . . . . ? C56 C51 N8 C50 167.8(4) . . . . ? C52 C51 N8 Fe02 172.6(3) . . . . ? C56 C51 N8 Fe02 -4.6(5) . . . . ? C20 C21 O1 C22 -5.4(7) . . . . ? C16 C21 O1 C22 174.3(4) . . . . ? C23 C22 O1 C21 86.6(5) . . . . ? C22 C23 O2 C24 -77.5(5) . . . . ? C25 C24 O2 C23 -95.2(6) . . . . ? C24 C25 O3 C26 178.6(5) . . . . ? C27 C26 O3 C25 168.4(5) . . . . ? C29 C28 O4 C27 71.0(6) . . . . ? C26 C27 O4 C28 91.2(6) . . . . ? C31 C30 O5 C29 1.5(7) . . . . ? C35 C30 O5 C29 178.0(4) . . . . ? C28 C29 O5 C30 175.5(5) . . . . ? C55 C56 O6 C57 -2.0(6) . . . . ? C51 C56 O6 C57 178.1(4) . . . . ? C58 C57 O6 C56 81.6(5) . . . . ? C60 C59 O7 C58 -119.9(5) . . . . ? C57 C58 O7 C59 -100.6(5) . . . . ? C59 C60 O8 C61 -160.7(4) . . . . ? C62 C61 O8 C60 170.2(4) . . . . ? C61 C62 O9 C63 65.0(6) . . . . ? C64 C63 O9 C62 172.3(4) . . . . ? C66 C65 O10 C64 7.0(7) . . . . ? C70 C65 O10 C64 -172.0(4) . . . . ? C63 C64 O10 C65 173.8(4) . . . . ? C40 N6 Fe01 N4 -89.2(6) . . . . ? C37 N6 Fe01 N4 85.8(4) . . . . ? C40 N6 Fe01 N3 89.8(5) . . . . ? C37 N6 Fe01 N3 -95.1(3) . . . . ? C40 N6 Fe01 N5 -178.7(5) . . . . ? C37 N6 Fe01 N5 -3.6(3) . . . . ? C15 N4 Fe01 N6 -173.2(3) . . . . ? C16 N4 Fe01 N6 4.6(6) . . . . ? C15 N4 Fe01 N3 7.6(3) . . . . ? C16 N4 Fe01 N3 -174.7(4) . . . . ? C15 N4 Fe01 N5 -88.5(3) . . . . ? C16 N4 Fe01 N5 89.3(4) . . . . ? C11 N3 Fe01 N6 24.5(5) . . . . ? C14 N3 Fe01 N6 172.3(3) . . . . ? C11 N3 Fe01 N4 -155.9(5) . . . . ? C14 N3 Fe01 N4 -8.1(3) . . . . ? C11 N3 Fe01 N5 -57.9(5) . . . . ? C14 N3 Fe01 N5 89.9(3) . . . . ? C36 N5 Fe01 N6 4.0(3) . . . . ? C35 N5 Fe01 N6 -178.1(4) . . . . ? C36 N5 Fe01 N4 -148.9(3) . . . . ? C35 N5 Fe01 N4 29.0(4) . . . . ? C36 N5 Fe01 N3 130.2(3) . . . . ? C35 N5 Fe01 N3 -51.9(4) . . . . ? C5 N2 Fe02 N8 -81.4(6) . . . . ? C2 N2 Fe02 N8 82.7(4) . . . . ? C5 N2 Fe02 N7 92.5(5) . . . . ? C2 N2 Fe02 N7 -103.4(3) . . . . ? C5 N2 Fe02 N1 -172.7(5) . . . . ? C2 N2 Fe02 N1 -8.6(3) . . . . ? C50 N8 Fe02 N2 -174.8(3) . . . . ? C51 N8 Fe02 N2 -1.8(5) . . . . ? C50 N8 Fe02 N7 10.2(3) . . . . ? C51 N8 Fe02 N7 -176.8(3) . . . . ? C50 N8 Fe02 N1 -88.4(3) . . . . ? C51 N8 Fe02 N1 84.6(3) . . . . ? C46 N7 Fe02 N2 26.5(5) . . . . ? C49 N7 Fe02 N2 172.9(2) . . . . ? C46 N7 Fe02 N8 -156.3(5) . . . . ? C49 N7 Fe02 N8 -9.9(3) . . . . ? C46 N7 Fe02 N1 -58.0(5) . . . . ? C49 N7 Fe02 N1 88.3(3) . . . . ? C1 N1 Fe02 N2 7.3(3) . . . . ? C70 N1 Fe02 N2 -173.5(4) . . . . ? C1 N1 Fe02 N8 -145.1(3) . . . . ? C70 N1 Fe02 N8 34.1(4) . . . . ? C1 N1 Fe02 N7 133.8(3) . . . . ? C70 N1 Fe02 N7 -47.0(4) . . . . ? C103 C101 C102 C103 0.0(16) 2_675 . . . ? C101 C102 C103 C101 0.0(15) . . . 2_675 ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 1.132 _refine_diff_density_min -1.065 _refine_diff_density_rms 0.110 data_jl0024_Mn2(2+2LP) _database_code_depnum_ccdc_archive 'CCDC 895826' #TrackingRef 'combined_CIF.cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C70 H79 Mn2 N8 O10' _chemical_formula_sum 'C70 H79 Mn2 N8 O10' _chemical_formula_weight 1302.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 25.365(5) _cell_length_b 12.448(5) _cell_length_c 20.697(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 105.979(5) _cell_angle_gamma 90.000(5) _cell_volume 6282(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 23636 _cell_measurement_theta_min 1.8101 _cell_measurement_theta_max 73.2589 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.2156 _exptl_crystal_size_mid 0.1466 _exptl_crystal_size_min 0.0666 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2740 _exptl_absorpt_coefficient_mu 3.818 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.88379 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 5.1574 _diffrn_standards_number 62546 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 60916 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 73.41 _reflns_number_total 12465 _reflns_number_gt 9643 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen et al., 2004)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0628P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12465 _refine_ls_number_parameters 811 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0447 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0861 _refine_ls_wR_factor_gt 0.0829 _refine_ls_goodness_of_fit_ref 0.851 _refine_ls_restrained_S_all 0.851 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C01 C 0.09010(7) -0.05575(14) 0.78802(9) 0.0270(3) Uani 1 1 d . . . H01 H 0.0547 -0.0850 0.7687 0.032 Uiso 1 1 calc R . . C02 C 0.09571(7) 0.05023(14) 0.81240(9) 0.0262(3) Uani 1 1 d . . . C03 C 0.05643(7) 0.13071(15) 0.80864(9) 0.0293(4) Uani 1 1 d . . . H03 H 0.0178 0.1238 0.7910 0.035 Uiso 1 1 calc R . . C04 C 0.08512(7) 0.22304(15) 0.83583(9) 0.0293(4) Uani 1 1 d . . . H04 H 0.0699 0.2916 0.8400 0.035 Uiso 1 1 calc R . . C05 C 0.14093(7) 0.19476(14) 0.85596(8) 0.0238(3) Uani 1 1 d . . . C06 C 0.18975(7) 0.26147(13) 0.89423(8) 0.0241(3) Uani 1 1 d . . . C07 C 0.17481(7) 0.38136(14) 0.88442(9) 0.0284(4) Uani 1 1 d . . . H07A H 0.1654 0.3979 0.8358 0.034 Uiso 1 1 calc R . . H07B H 0.1416 0.3944 0.8996 0.034 Uiso 1 1 calc R . . C08 C 0.21958(8) 0.45901(15) 0.92145(11) 0.0359(4) Uani 1 1 d . . . H08A H 0.2065 0.5331 0.9123 0.054 Uiso 1 1 calc R . . H08B H 0.2524 0.4486 0.9060 0.054 Uiso 1 1 calc R . . H08C H 0.2285 0.4453 0.9699 0.054 Uiso 1 1 calc R . . C09 C 0.20370(7) 0.23079(14) 0.96952(9) 0.0262(3) Uani 1 1 d . . . H09A H 0.2115 0.1528 0.9738 0.031 Uiso 1 1 calc R . . H09B H 0.2377 0.2689 0.9937 0.031 Uiso 1 1 calc R . . C10 C 0.15925(8) 0.25617(17) 1.00398(10) 0.0348(4) Uani 1 1 d . . . H10A H 0.1716 0.2341 1.0512 0.052 Uiso 1 1 calc R . . H10B H 0.1256 0.2172 0.9815 0.052 Uiso 1 1 calc R . . H10C H 0.1519 0.3336 1.0014 0.052 Uiso 1 1 calc R . . C11 C 0.23762(6) 0.23475(13) 0.86620(8) 0.0233(3) Uani 1 1 d . . . C12 C 0.24935(7) 0.28341(15) 0.81102(9) 0.0287(4) Uani 1 1 d . . . H12 H 0.2295 0.3405 0.7848 0.034 Uiso 1 1 calc R . . C13 C 0.29557(7) 0.23297(14) 0.80141(9) 0.0274(3) Uani 1 1 d . . . H13 H 0.3131 0.2484 0.7674 0.033 Uiso 1 1 calc R . . C14 C 0.31106(6) 0.15583(13) 0.85124(8) 0.0237(3) Uani 1 1 d . . . C15 C 0.35866(7) 0.09154(14) 0.86865(9) 0.0251(3) Uani 1 1 d . . . H15 H 0.3827 0.0906 0.8407 0.030 Uiso 1 1 calc R . . C16 C 0.41439(7) -0.03744(14) 0.94097(9) 0.0270(4) Uani 1 1 d . . . C17 C 0.44581(8) -0.07031(16) 0.89939(10) 0.0338(4) Uani 1 1 d . . . H17 H 0.4380 -0.0430 0.8549 0.041 Uiso 1 1 calc R . . C18 C 0.48867(8) -0.14275(18) 0.92199(11) 0.0391(5) Uani 1 1 d . . . H18 H 0.5105 -0.1634 0.8934 0.047 Uiso 1 1 calc R . . C19 C 0.49942(8) -0.18462(17) 0.98607(11) 0.0382(4) Uani 1 1 d . . . H19 H 0.5281 -0.2356 1.0010 0.046 Uiso 1 1 calc R . . C20 C 0.46891(8) -0.15298(17) 1.02843(10) 0.0367(4) Uani 1 1 d . . . H20 H 0.4767 -0.1814 1.0726 0.044 Uiso 1 1 calc R . . C21 C 0.42685(7) -0.07938(15) 1.00616(10) 0.0309(4) Uani 1 1 d . . . C22 C 0.41088(8) -0.05613(17) 1.11593(10) 0.0355(4) Uani 1 1 d . . . H22A H 0.3989 0.0060 1.1382 0.043 Uiso 1 1 calc R . . H22B H 0.4514 -0.0604 1.1318 0.043 Uiso 1 1 calc R . . C23 C 0.38622(8) -0.15793(17) 1.13461(10) 0.0379(4) Uani 1 1 d . . . H23A H 0.3459 -0.1567 1.1156 0.045 Uiso 1 1 calc R . . H23B H 0.4008 -0.2210 1.1161 0.045 Uiso 1 1 calc R . . C24 C 0.35745(8) -0.12444(16) 1.23249(10) 0.0345(4) Uani 1 1 d . . . H24A H 0.3267 -0.1763 1.2242 0.041 Uiso 1 1 calc R . . H24B H 0.3433 -0.0560 1.2099 0.041 Uiso 1 1 calc R . . C25 C 0.38059(8) -0.10618(16) 1.30711(11) 0.0361(4) Uani 1 1 d . . . H25A H 0.3499 -0.0904 1.3267 0.043 Uiso 1 1 calc R . . H25B H 0.3983 -0.1733 1.3279 0.043 Uiso 1 1 calc R . . C26 C 0.39579(9) 0.08063(18) 1.30648(12) 0.0446(5) Uani 1 1 d . . . H26A H 0.3601 0.0848 1.3172 0.054 Uiso 1 1 calc R . . H26B H 0.3892 0.0927 1.2576 0.054 Uiso 1 1 calc R . . C27 C 0.43469(9) 0.16652(18) 1.34576(11) 0.0419(5) Uani 1 1 d . . . H27A H 0.4193 0.1966 1.3809 0.050 Uiso 1 1 calc R . . H27B H 0.4704 0.1329 1.3684 0.050 Uiso 1 1 calc R . . C28 C 0.48097(8) 0.2214(2) 1.26812(11) 0.0443(5) Uani 1 1 d . . . H28A H 0.4725 0.1486 1.2488 0.053 Uiso 1 1 calc R . . H28B H 0.5187 0.2209 1.2986 0.053 Uiso 1 1 calc R . . C29 C 0.47683(8) 0.3013(2) 1.21330(10) 0.0458(5) Uani 1 1 d . . . H29A H 0.4735 0.3749 1.2299 0.055 Uiso 1 1 calc R . . H29B H 0.5099 0.2981 1.1967 0.055 Uiso 1 1 calc R . . C30 C 0.41886(7) 0.33202(16) 1.10229(9) 0.0303(4) Uani 1 1 d . . . C31 C 0.44872(8) 0.42211(17) 1.09376(11) 0.0372(4) Uani 1 1 d . . . H30 H 0.4780 0.4469 1.1299 0.045 Uiso 1 1 calc R . . C32 C 0.43594(8) 0.47574(17) 1.03290(11) 0.0388(4) Uani 1 1 d . . . H31 H 0.4561 0.5379 1.0277 0.047 Uiso 1 1 calc R . . C33 C 0.39399(8) 0.43913(16) 0.97968(10) 0.0347(4) Uani 1 1 d . . . H32 H 0.3851 0.4763 0.9380 0.042 Uiso 1 1 calc R . . C34 C 0.36483(7) 0.34733(14) 0.98741(9) 0.0288(4) Uani 1 1 d . . . H33 H 0.3368 0.3213 0.9502 0.035 Uiso 1 1 calc R . . C35 C 0.37580(7) 0.29322(14) 1.04817(9) 0.0264(3) Uani 1 1 d . . . C36 C 0.32453(6) 0.19155(14) 1.10515(9) 0.0255(3) Uani 1 1 d . . . C37 C 0.28961(7) 0.10464(14) 1.10904(9) 0.0252(3) Uani 1 1 d . . . C38 C 0.26141(7) 0.08320(15) 1.15672(9) 0.0290(4) Uani 1 1 d . . . H37 H 0.2632 0.1231 1.1964 0.035 Uiso 1 1 calc R . . C39 C 0.23007(7) -0.00817(16) 1.13462(9) 0.0302(4) Uani 1 1 d . . . H38 H 0.2067 -0.0433 1.1568 0.036 Uiso 1 1 calc R . . C40 C 0.23946(7) -0.03861(14) 1.07340(9) 0.0251(3) Uani 1 1 d . . . C41 C 0.21071(7) -0.12687(14) 1.02572(8) 0.0248(3) Uani 1 1 d . . . C42 C 0.19579(7) -0.21875(15) 1.06820(9) 0.0295(4) Uani 1 1 d . . . H41A H 0.2302 -0.2495 1.0973 0.035 Uiso 1 1 calc R . . H41B H 0.1751 -0.1877 1.0979 0.035 Uiso 1 1 calc R . . C43 C 0.16187(8) -0.30959(16) 1.02760(11) 0.0360(4) Uani 1 1 d . . . H42A H 0.1544 -0.3638 1.0583 0.054 Uiso 1 1 calc R . . H42B H 0.1822 -0.3425 0.9988 0.054 Uiso 1 1 calc R . . H42C H 0.1271 -0.2808 0.9996 0.054 Uiso 1 1 calc R . . C44 C 0.15818(7) -0.07867(14) 0.97613(9) 0.0265(3) Uani 1 1 d . . . H43A H 0.1694 -0.0176 0.9522 0.032 Uiso 1 1 calc R . . H43B H 0.1419 -0.1340 0.9421 0.032 Uiso 1 1 calc R . . C45 C 0.11374(7) -0.03940(16) 1.00739(10) 0.0336(4) Uani 1 1 d . . . H44A H 0.0828 -0.0107 0.9721 0.050 Uiso 1 1 calc R . . H44B H 0.1287 0.0172 1.0402 0.050 Uiso 1 1 calc R . . H44C H 0.1011 -0.0994 1.0299 0.050 Uiso 1 1 calc R . . C46 C 0.24824(7) -0.16862(13) 0.98528(8) 0.0247(3) Uani 1 1 d . . . C47 C 0.28260(7) -0.25881(14) 1.00092(9) 0.0294(4) Uani 1 1 d . . . H46 H 0.2861 -0.3058 1.0380 0.035 Uiso 1 1 calc R . . C48 C 0.31045(7) -0.26654(15) 0.95212(10) 0.0308(4) Uani 1 1 d . . . H47 H 0.3369 -0.3191 0.9495 0.037 Uiso 1 1 calc R . . C49 C 0.29189(7) -0.18176(14) 0.90761(9) 0.0263(3) Uani 1 1 d . . . C50 C 0.30316(7) -0.16045(14) 0.84616(9) 0.0269(3) Uani 1 1 d . . . H49 H 0.3310 -0.1999 0.8339 0.032 Uiso 1 1 calc R . . C51 C 0.28825(7) -0.05957(14) 0.74536(9) 0.0267(3) Uani 1 1 d . . . C52 C 0.33596(8) -0.08770(15) 0.72853(10) 0.0324(4) Uani 1 1 d . . . H51 H 0.3629 -0.1303 0.7586 0.039 Uiso 1 1 calc R . . C53 C 0.34449(8) -0.05414(16) 0.66823(11) 0.0377(4) Uani 1 1 d . . . H52 H 0.3769 -0.0747 0.6569 0.045 Uiso 1 1 calc R . . C54 C 0.30598(9) 0.00899(16) 0.62475(10) 0.0356(4) Uani 1 1 d . . . H53 H 0.3120 0.0318 0.5835 0.043 Uiso 1 1 calc R . . C55 C 0.25858(8) 0.03945(16) 0.64069(10) 0.0337(4) Uani 1 1 d . . . H54 H 0.2324 0.0839 0.6109 0.040 Uiso 1 1 calc R . . C56 C 0.24947(7) 0.00472(15) 0.70047(9) 0.0294(4) Uani 1 1 d . . . C57 C 0.15392(8) 0.05681(17) 0.67155(10) 0.0371(4) Uani 1 1 d . . . H56A H 0.1231 0.0164 0.6805 0.044 Uiso 1 1 calc R . . H56B H 0.1568 0.0359 0.6265 0.044 Uiso 1 1 calc R . . C58 C 0.14285(8) 0.17494(16) 0.67266(10) 0.0353(4) Uani 1 1 d . . . H57A H 0.1375 0.1968 0.7164 0.042 Uiso 1 1 calc R . . H57B H 0.1735 0.2170 0.6643 0.042 Uiso 1 1 calc R . . C59 C 0.06651(8) 0.28618(17) 0.62700(11) 0.0392(4) Uani 1 1 d . . . H58A H 0.0893 0.3490 0.6227 0.047 Uiso 1 1 calc R . . H58B H 0.0595 0.2887 0.6717 0.047 Uiso 1 1 calc R . . C60 C 0.01301(8) 0.28819(17) 0.57230(12) 0.0423(5) Uani 1 1 d . . . H59A H -0.0094 0.3489 0.5808 0.051 Uiso 1 1 calc R . . H59B H 0.0209 0.3017 0.5287 0.051 Uiso 1 1 calc R . . C61 C -0.03594(9) 0.16863(19) 0.62474(11) 0.0443(5) Uani 1 1 d . . . H60A H -0.0606 0.2263 0.6320 0.053 Uiso 1 1 calc R . . H60B H -0.0039 0.1650 0.6648 0.053 Uiso 1 1 calc R . . C62 C -0.06576(8) 0.06298(18) 0.61515(13) 0.0446(5) Uani 1 1 d . . . H61A H -0.0914 0.0624 0.6436 0.053 Uiso 1 1 calc R . . H61B H -0.0880 0.0579 0.5678 0.053 Uiso 1 1 calc R . . C63 C -0.00229(8) -0.05430(18) 0.58303(10) 0.0386(4) Uani 1 1 d . . . H62A H 0.0256 0.0017 0.5841 0.046 Uiso 1 1 calc R . . H62B H -0.0277 -0.0568 0.5372 0.046 Uiso 1 1 calc R . . C64 C 0.02494(8) -0.16159(17) 0.60111(10) 0.0360(4) Uani 1 1 d . . . H63A H -0.0027 -0.2175 0.6016 0.043 Uiso 1 1 calc R . . H63B H 0.0448 -0.1825 0.5681 0.043 Uiso 1 1 calc R . . C65 C 0.09127(7) -0.23647(15) 0.69768(10) 0.0315(4) Uani 1 1 d . . . C66 C 0.08743(8) -0.33911(16) 0.67057(11) 0.0375(4) Uani 1 1 d . . . H65 H 0.0617 -0.3537 0.6286 0.045 Uiso 1 1 calc R . . C67 C 0.12116(9) -0.42008(16) 0.70472(12) 0.0428(5) Uani 1 1 d . . . H66 H 0.1174 -0.4909 0.6869 0.051 Uiso 1 1 calc R . . C68 C 0.16051(9) -0.39903(16) 0.76478(12) 0.0416(5) Uani 1 1 d . . . H67 H 0.1851 -0.4539 0.7865 0.050 Uiso 1 1 calc R . . C69 C 0.16367(8) -0.29759(15) 0.79279(10) 0.0343(4) Uani 1 1 d . . . H68 H 0.1903 -0.2834 0.8341 0.041 Uiso 1 1 calc R . . C70 C 0.12850(7) -0.21627(14) 0.76146(9) 0.0282(4) Uani 1 1 d . . . N1 N 0.13379(6) -0.11411(12) 0.79201(7) 0.0262(3) Uani 1 1 d . . . N2 N 0.14766(5) 0.09109(11) 0.84133(7) 0.0231(3) Uani 1 1 d . . . N3 N 0.27447(5) 0.15500(11) 0.89077(7) 0.0225(3) Uani 1 1 d . . . N4 N 0.36964(5) 0.03341(11) 0.92309(7) 0.0246(3) Uani 1 1 d . . . N5 N 0.34424(5) 0.20106(12) 1.05333(7) 0.0248(3) Uani 1 1 d . . . N6 N 0.27603(5) 0.02886(11) 1.05826(7) 0.0228(3) Uani 1 1 d . . . N7 N 0.25378(6) -0.11976(11) 0.92862(7) 0.0251(3) Uani 1 1 d . . . N8 N 0.27573(6) -0.08688(12) 0.80564(7) 0.0255(3) Uani 1 1 d . . . O1 O 0.39402(6) -0.04078(12) 1.04415(7) 0.0368(3) Uani 1 1 d . . . O2 O 0.39984(5) -0.16538(12) 1.20618(7) 0.0359(3) Uani 1 1 d . . . O3 O 0.41940(5) -0.02115(11) 1.32399(7) 0.0367(3) Uani 1 1 d . . . O4 O 0.44322(6) 0.25027(12) 1.30411(7) 0.0398(3) Uani 1 1 d . . . O5 O 0.42906(5) 0.27409(12) 1.16076(7) 0.0351(3) Uani 1 1 d . . . O6 O 0.20414(5) 0.02986(12) 0.72150(7) 0.0354(3) Uani 1 1 d . . . O7 O 0.09378(5) 0.19001(11) 0.61972(7) 0.0369(3) Uani 1 1 d . . . O8 O -0.01824(6) 0.19210(12) 0.56703(7) 0.0397(3) Uani 1 1 d . . . O9 O -0.03177(6) -0.02985(12) 0.63062(8) 0.0412(3) Uani 1 1 d . . . O10 O 0.06225(6) -0.15015(11) 0.66636(7) 0.0374(3) Uani 1 1 d . . . Mn01 Mn 0.209548(10) -0.02151(2) 0.840652(13) 0.02324(7) Uani 1 1 d . . . Mn02 Mn 0.313367(10) 0.06382(2) 0.982192(13) 0.02257(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C01 0.0255(8) 0.0319(9) 0.0229(8) -0.0016(7) 0.0058(6) -0.0031(7) C02 0.0237(8) 0.0322(9) 0.0221(8) -0.0028(7) 0.0050(6) -0.0012(6) C03 0.0228(7) 0.0351(9) 0.0288(9) -0.0030(7) 0.0051(7) 0.0024(7) C04 0.0266(8) 0.0308(9) 0.0298(9) -0.0027(7) 0.0067(7) 0.0054(7) C05 0.0238(7) 0.0279(8) 0.0193(8) -0.0002(6) 0.0055(6) 0.0026(6) C06 0.0243(7) 0.0245(8) 0.0221(8) -0.0022(6) 0.0042(6) 0.0020(6) C07 0.0288(8) 0.0268(8) 0.0281(9) -0.0015(7) 0.0051(7) 0.0035(7) C08 0.0395(10) 0.0258(9) 0.0381(11) -0.0056(8) 0.0036(8) 0.0016(7) C09 0.0255(8) 0.0301(8) 0.0224(8) -0.0015(7) 0.0054(6) 0.0023(6) C10 0.0328(9) 0.0467(11) 0.0253(9) -0.0034(8) 0.0086(7) 0.0047(8) C11 0.0230(7) 0.0221(7) 0.0226(8) -0.0027(6) 0.0028(6) -0.0014(6) C12 0.0287(8) 0.0313(9) 0.0249(9) 0.0038(7) 0.0056(7) 0.0035(7) C13 0.0284(8) 0.0326(9) 0.0215(8) 0.0014(7) 0.0075(6) -0.0004(7) C14 0.0238(7) 0.0250(8) 0.0222(8) -0.0030(6) 0.0063(6) -0.0020(6) C15 0.0237(7) 0.0271(8) 0.0251(8) -0.0033(7) 0.0076(6) -0.0013(6) C16 0.0226(7) 0.0267(8) 0.0307(9) -0.0003(7) 0.0057(6) 0.0017(6) C17 0.0326(9) 0.0378(10) 0.0316(10) 0.0014(8) 0.0100(7) 0.0066(8) C18 0.0331(9) 0.0465(11) 0.0399(11) 0.0009(9) 0.0137(8) 0.0119(8) C19 0.0302(9) 0.0407(11) 0.0424(11) 0.0018(9) 0.0080(8) 0.0120(8) C20 0.0329(9) 0.0417(10) 0.0342(10) 0.0055(8) 0.0070(8) 0.0117(8) C21 0.0259(8) 0.0355(9) 0.0309(9) 0.0000(8) 0.0072(7) 0.0048(7) C22 0.0343(9) 0.0428(10) 0.0293(10) 0.0036(8) 0.0087(7) 0.0067(8) C23 0.0351(9) 0.0443(11) 0.0311(10) 0.0013(8) 0.0040(8) 0.0035(8) C24 0.0309(9) 0.0347(9) 0.0367(10) 0.0029(8) 0.0073(8) 0.0017(7) C25 0.0361(9) 0.0359(10) 0.0380(11) 0.0030(8) 0.0131(8) 0.0001(8) C26 0.0376(10) 0.0427(11) 0.0464(12) 0.0068(10) -0.0005(9) -0.0011(9) C27 0.0418(11) 0.0419(11) 0.0381(11) 0.0051(9) 0.0044(9) -0.0037(9) C28 0.0289(9) 0.0659(14) 0.0339(11) -0.0036(10) 0.0017(8) -0.0039(9) C29 0.0319(9) 0.0729(15) 0.0286(10) -0.0022(10) 0.0015(8) -0.0197(10) C30 0.0244(8) 0.0398(10) 0.0272(9) -0.0052(8) 0.0081(7) -0.0034(7) C31 0.0294(9) 0.0439(11) 0.0385(11) -0.0112(9) 0.0095(8) -0.0103(8) C32 0.0396(10) 0.0348(10) 0.0461(12) -0.0060(9) 0.0186(9) -0.0100(8) C33 0.0390(10) 0.0311(9) 0.0362(10) 0.0002(8) 0.0142(8) -0.0006(8) C34 0.0281(8) 0.0292(8) 0.0287(9) -0.0039(7) 0.0072(7) 0.0016(7) C35 0.0214(7) 0.0286(8) 0.0301(9) -0.0056(7) 0.0084(7) -0.0010(6) C36 0.0212(7) 0.0303(8) 0.0231(8) -0.0022(7) 0.0026(6) 0.0022(6) C37 0.0231(7) 0.0298(8) 0.0212(8) -0.0024(7) 0.0037(6) 0.0005(6) C38 0.0282(8) 0.0375(10) 0.0212(8) -0.0062(7) 0.0066(7) -0.0026(7) C39 0.0291(8) 0.0389(10) 0.0241(9) -0.0023(7) 0.0095(7) -0.0061(7) C40 0.0218(7) 0.0301(9) 0.0226(8) -0.0002(7) 0.0048(6) -0.0004(6) C41 0.0250(7) 0.0271(8) 0.0217(8) -0.0001(7) 0.0056(6) -0.0030(6) C42 0.0305(8) 0.0313(9) 0.0269(9) 0.0033(7) 0.0083(7) -0.0030(7) C43 0.0367(9) 0.0310(9) 0.0409(11) 0.0012(8) 0.0116(8) -0.0069(7) C44 0.0255(8) 0.0296(8) 0.0232(8) -0.0004(7) 0.0048(6) -0.0020(6) C45 0.0276(8) 0.0429(11) 0.0299(10) -0.0005(8) 0.0072(7) 0.0019(7) C46 0.0263(8) 0.0243(8) 0.0218(8) -0.0012(6) 0.0038(6) -0.0045(6) C47 0.0348(9) 0.0272(8) 0.0249(9) 0.0020(7) 0.0062(7) 0.0029(7) C48 0.0323(9) 0.0287(8) 0.0301(9) 0.0001(7) 0.0064(7) 0.0053(7) C49 0.0255(8) 0.0251(8) 0.0278(9) -0.0021(7) 0.0065(7) 0.0014(6) C50 0.0278(8) 0.0251(8) 0.0277(9) -0.0041(7) 0.0075(7) 0.0017(6) C51 0.0322(8) 0.0252(8) 0.0237(8) -0.0036(7) 0.0093(7) -0.0030(7) C52 0.0342(9) 0.0322(9) 0.0329(10) -0.0015(8) 0.0125(7) -0.0005(7) C53 0.0398(10) 0.0389(10) 0.0409(11) -0.0048(9) 0.0222(9) -0.0041(8) C54 0.0465(11) 0.0365(10) 0.0283(10) -0.0021(8) 0.0177(8) -0.0081(8) C55 0.0397(10) 0.0352(10) 0.0266(9) 0.0016(8) 0.0099(8) -0.0019(8) C56 0.0323(9) 0.0316(9) 0.0261(9) -0.0034(7) 0.0110(7) -0.0020(7) C57 0.0346(9) 0.0418(11) 0.0341(10) 0.0037(9) 0.0084(8) -0.0017(8) C58 0.0331(9) 0.0414(10) 0.0297(10) 0.0000(8) 0.0054(7) -0.0026(8) C59 0.0345(9) 0.0390(10) 0.0412(11) -0.0005(9) 0.0057(8) -0.0020(8) C60 0.0355(10) 0.0393(11) 0.0470(12) 0.0054(9) 0.0030(9) -0.0017(8) C61 0.0434(11) 0.0474(12) 0.0410(12) 0.0041(10) 0.0098(9) 0.0015(9) C62 0.0331(10) 0.0490(12) 0.0528(13) 0.0090(10) 0.0139(9) 0.0021(9) C63 0.0355(9) 0.0511(12) 0.0277(10) 0.0053(9) 0.0062(8) -0.0050(8) C64 0.0333(9) 0.0491(11) 0.0252(9) -0.0069(8) 0.0073(7) -0.0086(8) C65 0.0313(9) 0.0323(9) 0.0331(10) -0.0058(8) 0.0124(7) -0.0048(7) C66 0.0399(10) 0.0369(10) 0.0395(11) -0.0124(9) 0.0173(8) -0.0096(8) C67 0.0514(12) 0.0296(10) 0.0553(14) -0.0123(9) 0.0279(10) -0.0086(9) C68 0.0516(12) 0.0292(9) 0.0491(13) 0.0018(9) 0.0226(10) 0.0030(8) C69 0.0384(9) 0.0312(9) 0.0348(10) 0.0027(8) 0.0126(8) -0.0006(7) C70 0.0301(8) 0.0282(9) 0.0288(9) -0.0038(7) 0.0121(7) -0.0038(7) N1 0.0281(7) 0.0271(7) 0.0230(7) -0.0027(6) 0.0062(6) -0.0017(6) N2 0.0219(6) 0.0258(7) 0.0200(7) -0.0006(5) 0.0031(5) 0.0011(5) N3 0.0231(6) 0.0240(7) 0.0199(7) -0.0009(5) 0.0049(5) 0.0008(5) N4 0.0215(6) 0.0267(7) 0.0252(7) -0.0014(6) 0.0058(5) 0.0008(5) N5 0.0218(6) 0.0280(7) 0.0228(7) -0.0027(6) 0.0032(5) 0.0002(5) N6 0.0215(6) 0.0253(7) 0.0208(7) -0.0007(6) 0.0047(5) 0.0001(5) N7 0.0256(6) 0.0263(7) 0.0229(7) -0.0001(6) 0.0059(5) 0.0014(5) N8 0.0270(7) 0.0263(7) 0.0238(7) -0.0022(6) 0.0081(6) -0.0012(5) O1 0.0364(7) 0.0486(8) 0.0273(7) 0.0094(6) 0.0122(5) 0.0185(6) O2 0.0333(6) 0.0439(7) 0.0292(7) 0.0069(6) 0.0066(5) 0.0071(6) O3 0.0314(6) 0.0374(7) 0.0392(8) 0.0008(6) 0.0059(5) 0.0018(5) O4 0.0444(7) 0.0403(8) 0.0347(7) 0.0016(6) 0.0110(6) -0.0020(6) O5 0.0248(6) 0.0500(8) 0.0278(7) -0.0038(6) 0.0026(5) -0.0089(5) O6 0.0343(7) 0.0467(8) 0.0265(7) 0.0064(6) 0.0107(5) 0.0108(6) O7 0.0302(6) 0.0408(7) 0.0358(7) 0.0018(6) 0.0025(5) 0.0007(5) O8 0.0345(7) 0.0442(8) 0.0369(8) 0.0047(6) 0.0037(6) -0.0052(6) O9 0.0394(7) 0.0448(8) 0.0426(8) 0.0081(7) 0.0167(6) 0.0022(6) O10 0.0399(7) 0.0369(7) 0.0293(7) -0.0062(6) -0.0007(6) -0.0003(6) Mn01 0.02279(12) 0.02601(13) 0.02023(13) -0.00001(11) 0.00477(9) 0.00385(10) Mn02 0.02142(12) 0.02756(13) 0.01880(13) 0.00062(10) 0.00566(9) 0.00198(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C01 N1 1.308(2) . ? C01 C02 1.406(3) . ? C01 H01 0.9500 . ? C02 N2 1.386(2) . ? C02 C03 1.400(2) . ? C03 C04 1.393(3) . ? C03 H03 0.9500 . ? C04 C05 1.406(2) . ? C04 H04 0.9500 . ? C05 N2 1.347(2) . ? C05 C06 1.520(2) . ? C06 C11 1.520(2) . ? C06 C07 1.539(2) . ? C06 C09 1.548(2) . ? C07 C08 1.527(3) . ? C07 H07A 0.9900 . ? C07 H07B 0.9900 . ? C08 H08A 0.9800 . ? C08 H08B 0.9800 . ? C08 H08C 0.9800 . ? C09 C10 1.524(3) . ? C09 H09A 0.9900 . ? C09 H09B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N3 1.362(2) . ? C11 C12 1.395(3) . ? C12 C13 1.391(3) . ? C12 H12 0.9500 . ? C13 C14 1.385(3) . ? C13 H13 0.9500 . ? C14 N3 1.396(2) . ? C14 C15 1.410(2) . ? C15 N4 1.303(2) . ? C15 H15 0.9500 . ? C16 C17 1.386(3) . ? C16 C21 1.399(3) . ? C16 N4 1.404(2) . ? C17 C18 1.391(3) . ? C17 H17 0.9500 . ? C18 C19 1.381(3) . ? C18 H18 0.9500 . ? C19 C20 1.377(3) . ? C19 H19 0.9500 . ? C20 C21 1.385(3) . ? C20 H20 0.9500 . ? C21 O1 1.380(2) . ? C22 O1 1.441(2) . ? C22 C23 1.510(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 O2 1.428(2) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O2 1.426(2) . ? C24 C25 1.511(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 O3 1.422(2) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O3 1.406(3) . ? C26 C27 1.528(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 O4 1.407(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O4 1.412(3) . ? C28 C29 1.491(3) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O5 1.428(2) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 O5 1.371(2) . ? C30 C31 1.391(3) . ? C30 C35 1.417(2) . ? C31 C32 1.383(3) . ? C31 H30 0.9500 . ? C32 C33 1.381(3) . ? C32 H31 0.9500 . ? C33 C34 1.394(3) . ? C33 H32 0.9500 . ? C34 C35 1.386(3) . ? C34 H33 0.9500 . ? C35 N5 1.420(2) . ? C36 N5 1.307(2) . ? C36 C37 1.414(3) . ? C37 N6 1.383(2) . ? C37 C38 1.395(3) . ? C38 C39 1.391(3) . ? C38 H37 0.9500 . ? C39 C40 1.404(3) . ? C39 H38 0.9500 . ? C40 N6 1.351(2) . ? C40 C41 1.522(2) . ? C41 C46 1.522(3) . ? C41 C42 1.552(2) . ? C41 C44 1.561(2) . ? C42 C43 1.525(3) . ? C42 H41A 0.9900 . ? C42 H41B 0.9900 . ? C43 H42A 0.9800 . ? C43 H42B 0.9800 . ? C43 H42C 0.9800 . ? C44 C45 1.526(3) . ? C44 H43A 0.9900 . ? C44 H43B 0.9900 . ? C45 H44A 0.9800 . ? C45 H44B 0.9800 . ? C45 H44C 0.9800 . ? C46 N7 1.362(2) . ? C46 C47 1.404(2) . ? C47 C48 1.386(3) . ? C47 H46 0.9500 . ? C48 C49 1.395(3) . ? C48 H47 0.9500 . ? C49 N7 1.397(2) . ? C49 C50 1.403(3) . ? C50 N8 1.306(2) . ? C50 H49 0.9500 . ? C51 C52 1.393(3) . ? C51 C56 1.403(3) . ? C51 N8 1.411(2) . ? C52 C53 1.388(3) . ? C52 H51 0.9500 . ? C53 C54 1.378(3) . ? C53 H52 0.9500 . ? C54 C55 1.384(3) . ? C54 H53 0.9500 . ? C55 C56 1.389(3) . ? C55 H54 0.9500 . ? C56 O6 1.373(2) . ? C57 O6 1.442(2) . ? C57 C58 1.498(3) . ? C57 H56A 0.9900 . ? C57 H56B 0.9900 . ? C58 O7 1.426(2) . ? C58 H57A 0.9900 . ? C58 H57B 0.9900 . ? C59 O7 1.411(3) . ? C59 C60 1.509(3) . ? C59 H58A 0.9900 . ? C59 H58B 0.9900 . ? C60 O8 1.422(3) . ? C60 H59A 0.9900 . ? C60 H59B 0.9900 . ? C61 O8 1.417(3) . ? C61 C62 1.503(3) . ? C61 H60A 0.9900 . ? C61 H60B 0.9900 . ? C62 O9 1.424(3) . ? C62 H61A 0.9900 . ? C62 H61B 0.9900 . ? C63 O9 1.424(3) . ? C63 C64 1.503(3) . ? C63 H62A 0.9900 . ? C63 H62B 0.9900 . ? C64 O10 1.427(2) . ? C64 H63A 0.9900 . ? C64 H63B 0.9900 . ? C65 O10 1.362(2) . ? C65 C66 1.388(3) . ? C65 C70 1.418(3) . ? C66 C67 1.384(3) . ? C66 H65 0.9500 . ? C67 C68 1.388(3) . ? C67 H66 0.9500 . ? C68 C69 1.383(3) . ? C68 H67 0.9500 . ? C69 C70 1.387(3) . ? C69 H68 0.9500 . ? C70 N1 1.410(2) . ? N1 Mn01 2.2293(15) . ? N2 Mn01 2.1074(14) . ? N3 Mn02 2.1940(14) . ? N4 Mn02 2.1536(15) . ? N5 Mn02 2.2505(15) . ? N6 Mn02 2.0943(15) . ? N7 Mn01 2.2235(15) . ? N8 Mn01 2.1622(15) . ? O1 Mn02 2.4658(13) . ? O6 Mn01 2.5145(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C01 C02 119.88(15) . . ? N1 C01 H01 120.1 . . ? C02 C01 H01 120.1 . . ? N2 C02 C03 109.82(15) . . ? N2 C02 C01 119.33(15) . . ? C03 C02 C01 130.67(16) . . ? C04 C03 C02 106.46(15) . . ? C04 C03 H03 126.8 . . ? C02 C03 H03 126.8 . . ? C03 C04 C05 106.53(16) . . ? C03 C04 H04 126.7 . . ? C05 C04 H04 126.7 . . ? N2 C05 C04 110.66(15) . . ? N2 C05 C06 120.33(14) . . ? C04 C05 C06 128.83(16) . . ? C11 C06 C05 107.66(13) . . ? C11 C06 C07 110.81(14) . . ? C05 C06 C07 108.99(13) . . ? C11 C06 C09 110.18(13) . . ? C05 C06 C09 108.52(14) . . ? C07 C06 C09 110.59(14) . . ? C08 C07 C06 115.18(14) . . ? C08 C07 H07A 108.5 . . ? C06 C07 H07A 108.5 . . ? C08 C07 H07B 108.5 . . ? C06 C07 H07B 108.5 . . ? H07A C07 H07B 107.5 . . ? C07 C08 H08A 109.5 . . ? C07 C08 H08B 109.5 . . ? H08A C08 H08B 109.5 . . ? C07 C08 H08C 109.5 . . ? H08A C08 H08C 109.5 . . ? H08B C08 H08C 109.5 . . ? C10 C09 C06 115.24(14) . . ? C10 C09 H09A 108.5 . . ? C06 C09 H09A 108.5 . . ? C10 C09 H09B 108.5 . . ? C06 C09 H09B 108.5 . . ? H09A C09 H09B 107.5 . . ? C09 C10 H10A 109.5 . . ? C09 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C09 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 C12 110.06(15) . . ? N3 C11 C06 123.71(15) . . ? C12 C11 C06 126.18(15) . . ? C13 C12 C11 107.40(15) . . ? C13 C12 H12 126.3 . . ? C11 C12 H12 126.3 . . ? C14 C13 C12 106.50(16) . . ? C14 C13 H13 126.7 . . ? C12 C13 H13 126.7 . . ? C13 C14 N3 110.09(15) . . ? C13 C14 C15 129.16(16) . . ? N3 C14 C15 120.43(15) . . ? N4 C15 C14 120.03(16) . . ? N4 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 C16 C21 118.20(16) . . ? C17 C16 N4 125.67(17) . . ? C21 C16 N4 116.11(16) . . ? C16 C17 C18 120.83(19) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C19 C18 C17 119.82(19) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C20 C19 C18 120.45(18) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 119.58(19) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? O1 C21 C20 124.83(18) . . ? O1 C21 C16 114.08(15) . . ? C20 C21 C16 121.10(18) . . ? O1 C22 C23 110.43(17) . . ? O1 C22 H22A 109.6 . . ? C23 C22 H22A 109.6 . . ? O1 C22 H22B 109.6 . . ? C23 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? O2 C23 C22 108.73(16) . . ? O2 C23 H23A 109.9 . . ? C22 C23 H23A 109.9 . . ? O2 C23 H23B 109.9 . . ? C22 C23 H23B 109.9 . . ? H23A C23 H23B 108.3 . . ? O2 C24 C25 108.82(15) . . ? O2 C24 H24A 109.9 . . ? C25 C24 H24A 109.9 . . ? O2 C24 H24B 109.9 . . ? C25 C24 H24B 109.9 . . ? H24A C24 H24B 108.3 . . ? O3 C25 C24 114.27(17) . . ? O3 C25 H25A 108.7 . . ? C24 C25 H25A 108.7 . . ? O3 C25 H25B 108.7 . . ? C24 C25 H25B 108.7 . . ? H25A C25 H25B 107.6 . . ? O3 C26 C27 109.06(17) . . ? O3 C26 H26A 109.9 . . ? C27 C26 H26A 109.9 . . ? O3 C26 H26B 109.9 . . ? C27 C26 H26B 109.9 . . ? H26A C26 H26B 108.3 . . ? O4 C27 C26 112.22(18) . . ? O4 C27 H27A 109.2 . . ? C26 C27 H27A 109.2 . . ? O4 C27 H27B 109.2 . . ? C26 C27 H27B 109.2 . . ? H27A C27 H27B 107.9 . . ? O4 C28 C29 108.40(19) . . ? O4 C28 H28A 110.0 . . ? C29 C28 H28A 110.0 . . ? O4 C28 H28B 110.0 . . ? C29 C28 H28B 110.0 . . ? H28A C28 H28B 108.4 . . ? O5 C29 C28 106.76(17) . . ? O5 C29 H29A 110.4 . . ? C28 C29 H29A 110.4 . . ? O5 C29 H29B 110.4 . . ? C28 C29 H29B 110.4 . . ? H29A C29 H29B 108.6 . . ? O5 C30 C31 123.99(16) . . ? O5 C30 C35 115.82(16) . . ? C31 C30 C35 120.17(18) . . ? C32 C31 C30 120.36(18) . . ? C32 C31 H30 119.8 . . ? C30 C31 H30 119.8 . . ? C33 C32 C31 120.20(19) . . ? C33 C32 H31 119.9 . . ? C31 C32 H31 119.9 . . ? C32 C33 C34 119.69(19) . . ? C32 C33 H32 120.2 . . ? C34 C33 H32 120.2 . . ? C35 C34 C33 121.49(17) . . ? C35 C34 H33 119.3 . . ? C33 C34 H33 119.3 . . ? C34 C35 C30 118.05(17) . . ? C34 C35 N5 118.99(15) . . ? C30 C35 N5 122.96(17) . . ? N5 C36 C37 120.18(16) . . ? N6 C37 C38 109.76(15) . . ? N6 C37 C36 120.48(16) . . ? C38 C37 C36 129.63(17) . . ? C39 C38 C37 106.36(16) . . ? C39 C38 H37 126.8 . . ? C37 C38 H37 126.8 . . ? C38 C39 C40 107.10(16) . . ? C38 C39 H38 126.5 . . ? C40 C39 H38 126.5 . . ? N6 C40 C39 109.83(15) . . ? N6 C40 C41 122.39(15) . . ? C39 C40 C41 127.58(16) . . ? C46 C41 C40 110.03(13) . . ? C46 C41 C42 110.30(14) . . ? C40 C41 C42 108.23(14) . . ? C46 C41 C44 108.64(14) . . ? C40 C41 C44 108.59(14) . . ? C42 C41 C44 111.03(14) . . ? C43 C42 C41 115.02(15) . . ? C43 C42 H41A 108.5 . . ? C41 C42 H41A 108.5 . . ? C43 C42 H41B 108.5 . . ? C41 C42 H41B 108.5 . . ? H41A C42 H41B 107.5 . . ? C42 C43 H42A 109.5 . . ? C42 C43 H42B 109.5 . . ? H42A C43 H42B 109.5 . . ? C42 C43 H42C 109.5 . . ? H42A C43 H42C 109.5 . . ? H42B C43 H42C 109.5 . . ? C45 C44 C41 116.15(15) . . ? C45 C44 H43A 108.2 . . ? C41 C44 H43A 108.2 . . ? C45 C44 H43B 108.2 . . ? C41 C44 H43B 108.2 . . ? H43A C44 H43B 107.4 . . ? C44 C45 H44A 109.5 . . ? C44 C45 H44B 109.5 . . ? H44A C45 H44B 109.5 . . ? C44 C45 H44C 109.5 . . ? H44A C45 H44C 109.5 . . ? H44B C45 H44C 109.5 . . ? N7 C46 C47 110.55(16) . . ? N7 C46 C41 123.33(15) . . ? C47 C46 C41 126.11(16) . . ? C48 C47 C46 107.23(16) . . ? C48 C47 H46 126.4 . . ? C46 C47 H46 126.4 . . ? C47 C48 C49 106.36(16) . . ? C47 C48 H47 126.8 . . ? C49 C48 H47 126.8 . . ? C48 C49 N7 110.44(16) . . ? C48 C49 C50 128.73(16) . . ? N7 C49 C50 120.57(15) . . ? N8 C50 C49 120.61(16) . . ? N8 C50 H49 119.7 . . ? C49 C50 H49 119.7 . . ? C52 C51 C56 118.47(17) . . ? C52 C51 N8 125.67(17) . . ? C56 C51 N8 115.82(16) . . ? C53 C52 C51 120.68(18) . . ? C53 C52 H51 119.7 . . ? C51 C52 H51 119.7 . . ? C54 C53 C52 120.06(19) . . ? C54 C53 H52 120.0 . . ? C52 C53 H52 120.0 . . ? C53 C54 C55 120.45(19) . . ? C53 C54 H53 119.8 . . ? C55 C54 H53 119.8 . . ? C54 C55 C56 119.71(18) . . ? C54 C55 H54 120.1 . . ? C56 C55 H54 120.1 . . ? O6 C56 C55 124.81(17) . . ? O6 C56 C51 114.56(16) . . ? C55 C56 C51 120.62(17) . . ? O6 C57 C58 110.47(16) . . ? O6 C57 H56A 109.6 . . ? C58 C57 H56A 109.6 . . ? O6 C57 H56B 109.6 . . ? C58 C57 H56B 109.6 . . ? H56A C57 H56B 108.1 . . ? O7 C58 C57 104.18(15) . . ? O7 C58 H57A 110.9 . . ? C57 C58 H57A 110.9 . . ? O7 C58 H57B 110.9 . . ? C57 C58 H57B 110.9 . . ? H57A C58 H57B 108.9 . . ? O7 C59 C60 107.45(17) . . ? O7 C59 H58A 110.2 . . ? C60 C59 H58A 110.2 . . ? O7 C59 H58B 110.2 . . ? C60 C59 H58B 110.2 . . ? H58A C59 H58B 108.5 . . ? O8 C60 C59 114.23(17) . . ? O8 C60 H59A 108.7 . . ? C59 C60 H59A 108.7 . . ? O8 C60 H59B 108.7 . . ? C59 C60 H59B 108.7 . . ? H59A C60 H59B 107.6 . . ? O8 C61 C62 109.50(19) . . ? O8 C61 H60A 109.8 . . ? C62 C61 H60A 109.8 . . ? O8 C61 H60B 109.8 . . ? C62 C61 H60B 109.8 . . ? H60A C61 H60B 108.2 . . ? O9 C62 C61 115.39(18) . . ? O9 C62 H61A 108.4 . . ? C61 C62 H61A 108.4 . . ? O9 C62 H61B 108.4 . . ? C61 C62 H61B 108.4 . . ? H61A C62 H61B 107.5 . . ? O9 C63 C64 108.09(16) . . ? O9 C63 H62A 110.1 . . ? C64 C63 H62A 110.1 . . ? O9 C63 H62B 110.1 . . ? C64 C63 H62B 110.1 . . ? H62A C63 H62B 108.4 . . ? O10 C64 C63 106.65(16) . . ? O10 C64 H63A 110.4 . . ? C63 C64 H63A 110.4 . . ? O10 C64 H63B 110.4 . . ? C63 C64 H63B 110.4 . . ? H63A C64 H63B 108.6 . . ? O10 C65 C66 124.43(18) . . ? O10 C65 C70 115.94(16) . . ? C66 C65 C70 119.62(19) . . ? C67 C66 C65 120.0(2) . . ? C67 C66 H65 120.0 . . ? C65 C66 H65 120.0 . . ? C66 C67 C68 120.73(19) . . ? C66 C67 H66 119.6 . . ? C68 C67 H66 119.6 . . ? C69 C68 C67 119.5(2) . . ? C69 C68 H67 120.3 . . ? C67 C68 H67 120.3 . . ? C68 C69 C70 121.0(2) . . ? C68 C69 H68 119.5 . . ? C70 C69 H68 119.5 . . ? C69 C70 N1 118.63(17) . . ? C69 C70 C65 118.93(17) . . ? N1 C70 C65 122.28(16) . . ? C01 N1 C70 119.87(15) . . ? C01 N1 Mn01 110.56(12) . . ? C70 N1 Mn01 129.24(11) . . ? C05 N2 C02 106.53(14) . . ? C05 N2 Mn01 141.21(11) . . ? C02 N2 Mn01 112.00(11) . . ? C11 N3 C14 105.91(14) . . ? C11 N3 Mn02 142.98(12) . . ? C14 N3 Mn02 107.19(10) . . ? C15 N4 C16 122.78(15) . . ? C15 N4 Mn02 112.10(11) . . ? C16 N4 Mn02 125.09(12) . . ? C36 N5 C35 119.06(15) . . ? C36 N5 Mn02 108.98(11) . . ? C35 N5 Mn02 131.76(12) . . ? C40 N6 C37 106.93(14) . . ? C40 N6 Mn02 141.74(12) . . ? C37 N6 Mn02 111.09(11) . . ? C46 N7 C49 105.40(14) . . ? C46 N7 Mn01 143.33(12) . . ? C49 N7 Mn01 106.59(11) . . ? C50 N8 C51 121.81(15) . . ? C50 N8 Mn01 111.98(12) . . ? C51 N8 Mn01 126.17(11) . . ? C21 O1 C22 119.14(14) . . ? C21 O1 Mn02 115.60(11) . . ? C22 O1 Mn02 125.06(11) . . ? C24 O2 C23 112.35(14) . . ? C26 O3 C25 112.99(15) . . ? C27 O4 C28 112.06(18) . . ? C30 O5 C29 117.49(15) . . ? C56 O6 C57 118.50(15) . . ? C56 O6 Mn01 115.38(11) . . ? C57 O6 Mn01 124.15(12) . . ? C59 O7 C58 112.29(15) . . ? C61 O8 C60 114.07(17) . . ? C63 O9 C62 114.74(17) . . ? C65 O10 C64 120.17(15) . . ? N2 Mn01 N8 154.29(6) . . ? N2 Mn01 N7 124.69(6) . . ? N8 Mn01 N7 78.71(6) . . ? N2 Mn01 N1 78.22(6) . . ? N8 Mn01 N1 107.84(6) . . ? N7 Mn01 N1 105.26(6) . . ? N2 Mn01 O6 89.87(5) . . ? N8 Mn01 O6 66.72(5) . . ? N7 Mn01 O6 145.27(5) . . ? N1 Mn01 O6 83.17(5) . . ? N6 Mn02 N4 153.90(6) . . ? N6 Mn02 N3 124.52(5) . . ? N4 Mn02 N3 79.17(6) . . ? N6 Mn02 N5 79.27(6) . . ? N4 Mn02 N5 109.84(5) . . ? N3 Mn02 N5 99.46(6) . . ? N6 Mn02 O1 88.94(5) . . ? N4 Mn02 O1 67.53(5) . . ? N3 Mn02 O1 146.45(5) . . ? N5 Mn02 O1 88.35(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C01 C02 N2 -0.9(3) . . . . ? N1 C01 C02 C03 173.60(19) . . . . ? N2 C02 C03 C04 0.1(2) . . . . ? C01 C02 C03 C04 -174.81(19) . . . . ? C02 C03 C04 C05 -0.7(2) . . . . ? C03 C04 C05 N2 1.1(2) . . . . ? C03 C04 C05 C06 -173.95(17) . . . . ? N2 C05 C06 C11 41.8(2) . . . . ? C04 C05 C06 C11 -143.49(18) . . . . ? N2 C05 C06 C07 162.11(16) . . . . ? C04 C05 C06 C07 -23.2(3) . . . . ? N2 C05 C06 C09 -77.40(19) . . . . ? C04 C05 C06 C09 97.3(2) . . . . ? C11 C06 C07 C08 -63.1(2) . . . . ? C05 C06 C07 C08 178.63(16) . . . . ? C09 C06 C07 C08 59.4(2) . . . . ? C11 C06 C09 C10 178.64(15) . . . . ? C05 C06 C09 C10 -63.72(19) . . . . ? C07 C06 C09 C10 55.8(2) . . . . ? C05 C06 C11 N3 -90.34(18) . . . . ? C07 C06 C11 N3 150.56(15) . . . . ? C09 C06 C11 N3 27.8(2) . . . . ? C05 C06 C11 C12 86.9(2) . . . . ? C07 C06 C11 C12 -32.2(2) . . . . ? C09 C06 C11 C12 -154.94(16) . . . . ? N3 C11 C12 C13 -0.7(2) . . . . ? C06 C11 C12 C13 -178.28(15) . . . . ? C11 C12 C13 C14 -0.6(2) . . . . ? C12 C13 C14 N3 1.65(19) . . . . ? C12 C13 C14 C15 -171.82(17) . . . . ? C13 C14 C15 N4 170.70(17) . . . . ? N3 C14 C15 N4 -2.2(2) . . . . ? C21 C16 C17 C18 -0.2(3) . . . . ? N4 C16 C17 C18 -178.67(18) . . . . ? C16 C17 C18 C19 1.5(3) . . . . ? C17 C18 C19 C20 -1.7(3) . . . . ? C18 C19 C20 C21 0.6(3) . . . . ? C19 C20 C21 O1 -179.18(19) . . . . ? C19 C20 C21 C16 0.7(3) . . . . ? C17 C16 C21 O1 179.00(17) . . . . ? N4 C16 C21 O1 -2.4(2) . . . . ? C17 C16 C21 C20 -0.9(3) . . . . ? N4 C16 C21 C20 177.69(17) . . . . ? O1 C22 C23 O2 -174.93(14) . . . . ? O2 C24 C25 O3 68.5(2) . . . . ? O3 C26 C27 O4 131.17(19) . . . . ? O4 C28 C29 O5 -78.2(2) . . . . ? O5 C30 C31 C32 179.64(18) . . . . ? C35 C30 C31 C32 1.3(3) . . . . ? C30 C31 C32 C33 -1.1(3) . . . . ? C31 C32 C33 C34 -0.5(3) . . . . ? C32 C33 C34 C35 2.0(3) . . . . ? C33 C34 C35 C30 -1.8(3) . . . . ? C33 C34 C35 N5 179.11(16) . . . . ? O5 C30 C35 C34 -178.32(16) . . . . ? C31 C30 C35 C34 0.2(3) . . . . ? O5 C30 C35 N5 0.7(3) . . . . ? C31 C30 C35 N5 179.23(17) . . . . ? N5 C36 C37 N6 0.1(2) . . . . ? N5 C36 C37 C38 -175.19(17) . . . . ? N6 C37 C38 C39 0.3(2) . . . . ? C36 C37 C38 C39 175.96(17) . . . . ? C37 C38 C39 C40 -1.0(2) . . . . ? C38 C39 C40 N6 1.4(2) . . . . ? C38 C39 C40 C41 -173.56(16) . . . . ? N6 C40 C41 C46 32.1(2) . . . . ? C39 C40 C41 C46 -153.57(17) . . . . ? N6 C40 C41 C42 152.67(15) . . . . ? C39 C40 C41 C42 -33.0(2) . . . . ? N6 C40 C41 C44 -86.71(19) . . . . ? C39 C40 C41 C44 87.6(2) . . . . ? C46 C41 C42 C43 -64.98(19) . . . . ? C40 C41 C42 C43 174.60(15) . . . . ? C44 C41 C42 C43 55.5(2) . . . . ? C46 C41 C44 C45 176.01(15) . . . . ? C40 C41 C44 C45 -64.33(19) . . . . ? C42 C41 C44 C45 54.5(2) . . . . ? C40 C41 C46 N7 -82.91(19) . . . . ? C42 C41 C46 N7 157.75(15) . . . . ? C44 C41 C46 N7 35.8(2) . . . . ? C40 C41 C46 C47 95.3(2) . . . . ? C42 C41 C46 C47 -24.1(2) . . . . ? C44 C41 C46 C47 -145.97(17) . . . . ? N7 C46 C47 C48 -0.2(2) . . . . ? C41 C46 C47 C48 -178.53(16) . . . . ? C46 C47 C48 C49 -0.7(2) . . . . ? C47 C48 C49 N7 1.3(2) . . . . ? C47 C48 C49 C50 -172.88(18) . . . . ? C48 C49 C50 N8 169.28(17) . . . . ? N7 C49 C50 N8 -4.4(3) . . . . ? C56 C51 C52 C53 -0.9(3) . . . . ? N8 C51 C52 C53 -178.48(17) . . . . ? C51 C52 C53 C54 1.0(3) . . . . ? C52 C53 C54 C55 0.0(3) . . . . ? C53 C54 C55 C56 -1.0(3) . . . . ? C54 C55 C56 O6 179.92(18) . . . . ? C54 C55 C56 C51 1.0(3) . . . . ? C52 C51 C56 O6 -179.08(16) . . . . ? N8 C51 C56 O6 -1.3(2) . . . . ? C52 C51 C56 C55 0.0(3) . . . . ? N8 C51 C56 C55 177.73(16) . . . . ? O6 C57 C58 O7 177.90(15) . . . . ? O7 C59 C60 O8 49.4(3) . . . . ? O8 C61 C62 O9 83.3(2) . . . . ? O9 C63 C64 O10 -62.0(2) . . . . ? O10 C65 C66 C67 176.07(19) . . . . ? C70 C65 C66 C67 -2.2(3) . . . . ? C65 C66 C67 C68 -2.6(3) . . . . ? C66 C67 C68 C69 4.0(3) . . . . ? C67 C68 C69 C70 -0.7(3) . . . . ? C68 C69 C70 N1 -179.54(18) . . . . ? C68 C69 C70 C65 -4.0(3) . . . . ? O10 C65 C70 C69 -172.96(17) . . . . ? C66 C65 C70 C69 5.5(3) . . . . ? O10 C65 C70 N1 2.4(3) . . . . ? C66 C65 C70 N1 -179.20(17) . . . . ? C02 C01 N1 C70 -173.50(16) . . . . ? C02 C01 N1 Mn01 0.5(2) . . . . ? C69 C70 N1 C01 -144.66(18) . . . . ? C65 C70 N1 C01 40.0(3) . . . . ? C69 C70 N1 Mn01 42.6(2) . . . . ? C65 C70 N1 Mn01 -132.76(15) . . . . ? C04 C05 N2 C02 -1.0(2) . . . . ? C06 C05 N2 C02 174.51(15) . . . . ? C04 C05 N2 Mn01 172.08(14) . . . . ? C06 C05 N2 Mn01 -12.4(3) . . . . ? C03 C02 N2 C05 0.6(2) . . . . ? C01 C02 N2 C05 176.16(16) . . . . ? C03 C02 N2 Mn01 -174.79(12) . . . . ? C01 C02 N2 Mn01 0.8(2) . . . . ? C12 C11 N3 C14 1.70(18) . . . . ? C06 C11 N3 C14 179.32(14) . . . . ? C12 C11 N3 Mn02 154.37(15) . . . . ? C06 C11 N3 Mn02 -28.0(3) . . . . ? C13 C14 N3 C11 -2.08(18) . . . . ? C15 C14 N3 C11 172.05(15) . . . . ? C13 C14 N3 Mn02 -165.26(11) . . . . ? C15 C14 N3 Mn02 8.88(18) . . . . ? C14 C15 N4 C16 175.81(15) . . . . ? C14 C15 N4 Mn02 -6.2(2) . . . . ? C17 C16 N4 C15 -12.8(3) . . . . ? C21 C16 N4 C15 168.75(16) . . . . ? C17 C16 N4 Mn02 169.54(14) . . . . ? C21 C16 N4 Mn02 -9.0(2) . . . . ? C37 C36 N5 C35 175.30(15) . . . . ? C37 C36 N5 Mn02 -0.18(19) . . . . ? C34 C35 N5 C36 -133.52(17) . . . . ? C30 C35 N5 C36 47.4(2) . . . . ? C34 C35 N5 Mn02 40.8(2) . . . . ? C30 C35 N5 Mn02 -138.30(15) . . . . ? C39 C40 N6 C37 -1.19(19) . . . . ? C41 C40 N6 C37 174.05(14) . . . . ? C39 C40 N6 Mn02 -174.59(14) . . . . ? C41 C40 N6 Mn02 0.7(3) . . . . ? C38 C37 N6 C40 0.57(19) . . . . ? C36 C37 N6 C40 -175.58(15) . . . . ? C38 C37 N6 Mn02 176.19(11) . . . . ? C36 C37 N6 Mn02 0.05(19) . . . . ? C47 C46 N7 C49 0.92(18) . . . . ? C41 C46 N7 C49 179.36(14) . . . . ? C47 C46 N7 Mn01 150.90(15) . . . . ? C41 C46 N7 Mn01 -30.7(3) . . . . ? C48 C49 N7 C46 -1.38(19) . . . . ? C50 C49 N7 C46 173.35(15) . . . . ? C48 C49 N7 Mn01 -163.21(12) . . . . ? C50 C49 N7 Mn01 11.52(19) . . . . ? C49 C50 N8 C51 176.36(15) . . . . ? C49 C50 N8 Mn01 -6.0(2) . . . . ? C52 C51 N8 C50 -14.4(3) . . . . ? C56 C51 N8 C50 168.05(16) . . . . ? C52 C51 N8 Mn01 168.36(14) . . . . ? C56 C51 N8 Mn01 -9.2(2) . . . . ? C20 C21 O1 C22 15.3(3) . . . . ? C16 C21 O1 C22 -164.65(17) . . . . ? C20 C21 O1 Mn02 -169.59(16) . . . . ? C16 C21 O1 Mn02 10.5(2) . . . . ? C23 C22 O1 C21 -92.9(2) . . . . ? C23 C22 O1 Mn02 92.47(18) . . . . ? C25 C24 O2 C23 -164.28(16) . . . . ? C22 C23 O2 C24 95.54(18) . . . . ? C27 C26 O3 C25 161.63(18) . . . . ? C24 C25 O3 C26 68.6(2) . . . . ? C26 C27 O4 C28 -78.7(2) . . . . ? C29 C28 O4 C27 165.59(16) . . . . ? C31 C30 O5 C29 -7.0(3) . . . . ? C35 C30 O5 C29 171.40(18) . . . . ? C28 C29 O5 C30 -175.25(17) . . . . ? C55 C56 O6 C57 25.2(3) . . . . ? C51 C56 O6 C57 -155.84(16) . . . . ? C55 C56 O6 Mn01 -170.07(15) . . . . ? C51 C56 O6 Mn01 8.91(19) . . . . ? C58 C57 O6 C56 -106.8(2) . . . . ? C58 C57 O6 Mn01 89.86(18) . . . . ? C60 C59 O7 C58 -174.76(17) . . . . ? C57 C58 O7 C59 159.56(17) . . . . ? C62 C61 O8 C60 -176.96(16) . . . . ? C59 C60 O8 C61 63.2(2) . . . . ? C64 C63 O9 C62 -172.12(16) . . . . ? C61 C62 O9 C63 -72.8(3) . . . . ? C66 C65 O10 C64 -0.2(3) . . . . ? C70 C65 O10 C64 178.13(16) . . . . ? C63 C64 O10 C65 176.86(16) . . . . ? C05 N2 Mn01 N8 -66.5(2) . . . . ? C02 N2 Mn01 N8 106.38(15) . . . . ? C05 N2 Mn01 N7 86.2(2) . . . . ? C02 N2 Mn01 N7 -100.91(12) . . . . ? C05 N2 Mn01 N1 -173.27(19) . . . . ? C02 N2 Mn01 N1 -0.38(12) . . . . ? C05 N2 Mn01 O6 -90.22(19) . . . . ? C02 N2 Mn01 O6 82.67(12) . . . . ? C50 N8 Mn01 N2 166.51(12) . . . . ? C51 N8 Mn01 N2 -16.0(2) . . . . ? C50 N8 Mn01 N7 9.12(11) . . . . ? C51 N8 Mn01 N7 -173.38(14) . . . . ? C50 N8 Mn01 N1 -93.46(12) . . . . ? C51 N8 Mn01 N1 84.05(14) . . . . ? C50 N8 Mn01 O6 -167.53(13) . . . . ? C51 N8 Mn01 O6 9.98(12) . . . . ? C46 N7 Mn01 N2 31.5(2) . . . . ? C49 N7 Mn01 N2 -178.77(10) . . . . ? C46 N7 Mn01 N8 -160.2(2) . . . . ? C49 N7 Mn01 N8 -10.47(10) . . . . ? C46 N7 Mn01 N1 -54.6(2) . . . . ? C49 N7 Mn01 N1 95.15(11) . . . . ? C46 N7 Mn01 O6 -154.83(17) . . . . ? C49 N7 Mn01 O6 -5.06(16) . . . . ? C01 N1 Mn01 N2 -0.06(12) . . . . ? C70 N1 Mn01 N2 173.23(16) . . . . ? C01 N1 Mn01 N8 -154.19(12) . . . . ? C70 N1 Mn01 N8 19.10(16) . . . . ? C01 N1 Mn01 N7 123.02(12) . . . . ? C70 N1 Mn01 N7 -63.69(16) . . . . ? C01 N1 Mn01 O6 -91.36(12) . . . . ? C70 N1 Mn01 O6 81.93(15) . . . . ? C56 O6 Mn01 N2 159.27(13) . . . . ? C57 O6 Mn01 N2 -36.95(14) . . . . ? C56 O6 Mn01 N8 -9.78(12) . . . . ? C57 O6 Mn01 N8 153.99(15) . . . . ? C56 O6 Mn01 N7 -15.56(17) . . . . ? C57 O6 Mn01 N7 148.21(13) . . . . ? C56 O6 Mn01 N1 -122.57(13) . . . . ? C57 O6 Mn01 N1 41.20(14) . . . . ? C40 N6 Mn02 N4 -73.4(2) . . . . ? C37 N6 Mn02 N4 113.37(14) . . . . ? C40 N6 Mn02 N3 78.95(19) . . . . ? C37 N6 Mn02 N3 -94.27(11) . . . . ? C40 N6 Mn02 N5 173.12(19) . . . . ? C37 N6 Mn02 N5 -0.10(10) . . . . ? C40 N6 Mn02 O1 -98.36(18) . . . . ? C37 N6 Mn02 O1 88.42(11) . . . . ? C15 N4 Mn02 N6 165.35(12) . . . . ? C16 N4 Mn02 N6 -16.7(2) . . . . ? C15 N4 Mn02 N3 8.25(11) . . . . ? C16 N4 Mn02 N3 -173.83(14) . . . . ? C15 N4 Mn02 N5 -88.00(12) . . . . ? C16 N4 Mn02 N5 89.92(14) . . . . ? C15 N4 Mn02 O1 -167.49(13) . . . . ? C16 N4 Mn02 O1 10.42(12) . . . . ? C11 N3 Mn02 N6 30.8(2) . . . . ? C14 N3 Mn02 N6 -176.71(10) . . . . ? C11 N3 Mn02 N4 -161.17(19) . . . . ? C14 N3 Mn02 N4 -8.70(10) . . . . ? C11 N3 Mn02 N5 -52.60(19) . . . . ? C14 N3 Mn02 N5 99.87(11) . . . . ? C11 N3 Mn02 O1 -154.04(16) . . . . ? C14 N3 Mn02 O1 -1.58(16) . . . . ? C36 N5 Mn02 N6 0.15(11) . . . . ? C35 N5 Mn02 N6 -174.55(15) . . . . ? C36 N5 Mn02 N4 -154.44(11) . . . . ? C35 N5 Mn02 N4 30.85(15) . . . . ? C36 N5 Mn02 N3 123.74(11) . . . . ? C35 N5 Mn02 N3 -50.97(15) . . . . ? C36 N5 Mn02 O1 -89.08(11) . . . . ? C35 N5 Mn02 O1 96.22(14) . . . . ? C21 O1 Mn02 N6 157.49(13) . . . . ? C22 O1 Mn02 N6 -27.70(15) . . . . ? C21 O1 Mn02 N4 -10.92(12) . . . . ? C22 O1 Mn02 N4 163.89(16) . . . . ? C21 O1 Mn02 N3 -18.50(18) . . . . ? C22 O1 Mn02 N3 156.31(13) . . . . ? C21 O1 Mn02 N5 -123.22(13) . . . . ? C22 O1 Mn02 N5 51.59(15) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 73.41 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.714 _refine_diff_density_min -0.233 _refine_diff_density_rms 0.047 data_jl0035_Co(2+2LNMe) _database_code_depnum_ccdc_archive 'CCDC 895827' #TrackingRef 'combined_CIF.cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H70 Co2 N10 O4' _chemical_formula_sum 'C64 H70 Co2 N10 O4' _chemical_formula_weight 1161.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 12.40470(10) _cell_length_b 18.6551(2) _cell_length_c 24.0651(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5568.93(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10691 _cell_measurement_theta_min 2.3665 _cell_measurement_theta_max 73.1194 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2440 _exptl_absorpt_coefficient_mu 5.139 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.60922 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 5.1574 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 27037 _diffrn_reflns_av_R_equivalents 0.0589 _diffrn_reflns_av_sigmaI/netI 0.0401 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.67 _diffrn_reflns_theta_max 73.27 _reflns_number_total 5502 _reflns_number_gt 4591 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP (Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen et al., 2004)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0706P)^2^+2.8946P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5502 _refine_ls_number_parameters 364 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1252 _refine_ls_wR_factor_gt 0.1164 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4098(2) 0.06633(12) 0.21043(10) 0.0234(5) Uani 1 1 d . . . H1 H 0.4614 0.0323 0.2228 0.028 Uiso 1 1 calc R . . C2 C 0.3103(2) 0.07538(12) 0.23860(10) 0.0230(5) Uani 1 1 d . . . C3 C 0.2622(2) 0.04045(13) 0.28338(10) 0.0280(5) Uani 1 1 d . . . H3 H 0.2928 0.0035 0.3055 0.034 Uiso 1 1 calc R . . C4 C 0.1600(2) 0.07085(13) 0.28917(10) 0.0279(5) Uani 1 1 d . . . H4 H 0.1073 0.0582 0.3161 0.033 Uiso 1 1 calc R . . C5 C 0.14955(19) 0.12356(12) 0.24797(9) 0.0217(5) Uani 1 1 d . . . C6 C 0.0575(2) 0.17471(12) 0.23614(10) 0.0224(5) Uani 1 1 d . . . C7 C -0.0479(2) 0.14141(13) 0.25888(10) 0.0265(5) Uani 1 1 d . . . H7A H -0.0628 0.0968 0.2380 0.032 Uiso 1 1 calc R . . H7B H -0.0362 0.1280 0.2982 0.032 Uiso 1 1 calc R . . C8 C -0.1474(2) 0.18916(15) 0.25570(13) 0.0353(6) Uani 1 1 d . . . H8A H -0.1392 0.2296 0.2814 0.053 Uiso 1 1 calc R . . H8B H -0.2114 0.1613 0.2660 0.053 Uiso 1 1 calc R . . H8C H -0.1557 0.2073 0.2177 0.053 Uiso 1 1 calc R . . C9 C 0.0813(2) 0.24759(13) 0.26476(10) 0.0274(5) Uani 1 1 d . . . H9A H 0.1504 0.2663 0.2502 0.033 Uiso 1 1 calc R . . H9B H 0.0241 0.2820 0.2542 0.033 Uiso 1 1 calc R . . C10 C 0.0879(3) 0.24489(15) 0.32791(11) 0.0378(6) Uani 1 1 d . . . H10A H 0.0178 0.2307 0.3431 0.057 Uiso 1 1 calc R . . H10B H 0.1074 0.2923 0.3422 0.057 Uiso 1 1 calc R . . H10C H 0.1427 0.2099 0.3391 0.057 Uiso 1 1 calc R . . C11 C 0.04762(19) 0.18577(12) 0.17370(10) 0.0213(5) Uani 1 1 d . . . C12 C -0.0268(2) 0.15218(13) 0.13864(10) 0.0247(5) Uani 1 1 d . . . H12 H -0.0794 0.1179 0.1494 0.030 Uiso 1 1 calc R . . C13 C -0.0097(2) 0.17802(12) 0.08512(10) 0.0240(5) Uani 1 1 d . . . H13 H -0.0483 0.1652 0.0525 0.029 Uiso 1 1 calc R . . C14 C 0.07501(19) 0.22633(12) 0.08913(9) 0.0208(5) Uani 1 1 d . . . C15 C 0.11614(19) 0.27347(12) 0.04834(10) 0.0217(5) Uani 1 1 d . . . H15 H 0.0929 0.2695 0.0108 0.026 Uiso 1 1 calc R . . C16 C 0.23982(19) 0.36473(12) 0.02295(10) 0.0216(5) Uani 1 1 d . . . C17 C 0.2449(2) 0.34941(13) -0.03353(10) 0.0253(5) Uani 1 1 d . . . H17 H 0.2055 0.3099 -0.0480 0.030 Uiso 1 1 calc R . . C18 C 0.3069(2) 0.39118(14) -0.06916(11) 0.0290(5) Uani 1 1 d . . . H18 H 0.3093 0.3806 -0.1078 0.035 Uiso 1 1 calc R . . C19 C 0.3649(2) 0.44804(14) -0.04804(11) 0.0288(5) Uani 1 1 d . . . H19 H 0.4081 0.4762 -0.0723 0.035 Uiso 1 1 calc R . . C20 C 0.3611(2) 0.46483(13) 0.00818(10) 0.0264(5) Uani 1 1 d . . . H20 H 0.4010 0.5044 0.0222 0.032 Uiso 1 1 calc R . . C21 C 0.20139(19) 0.07648(13) 0.04392(10) 0.0228(5) Uani 1 1 d . . . C22 C 0.1556(2) 0.00855(12) 0.12732(10) 0.0244(5) Uani 1 1 d . . . H22A H 0.0922 -0.0059 0.1050 0.029 Uiso 1 1 calc R . . H22B H 0.1295 0.0245 0.1642 0.029 Uiso 1 1 calc R . . C23 C 0.2298(2) -0.05505(13) 0.13449(11) 0.0264(5) Uani 1 1 d . . . H23A H 0.2975 -0.0385 0.1521 0.032 Uiso 1 1 calc R . . H23B H 0.1954 -0.0897 0.1601 0.032 Uiso 1 1 calc R . . C24 C 0.1741(2) -0.14602(14) 0.07000(12) 0.0330(6) Uani 1 1 d . . . H24A H 0.1887 -0.1676 0.0336 0.049 Uiso 1 1 calc R . . H24B H 0.1029 -0.1232 0.0695 0.049 Uiso 1 1 calc R . . H24C H 0.1755 -0.1833 0.0986 0.049 Uiso 1 1 calc R . . C25 C 0.3635(2) -0.12492(13) 0.08393(12) 0.0302(6) Uani 1 1 d . . . H25A H 0.3652 -0.1649 0.0569 0.036 Uiso 1 1 calc R . . H25B H 0.3750 -0.1456 0.1214 0.036 Uiso 1 1 calc R . . C26 C 0.4560(2) -0.07481(13) 0.07113(11) 0.0285(5) Uani 1 1 d . . . H26A H 0.5244 -0.1021 0.0705 0.034 Uiso 1 1 calc R . . H26B H 0.4453 -0.0532 0.0340 0.034 Uiso 1 1 calc R . . C27 C 0.53756(19) 0.03389(12) 0.10399(10) 0.0231(5) Uani 1 1 d . . . C28 C 0.6254(2) 0.02868(13) 0.06872(11) 0.0279(5) Uani 1 1 d . . . H28 H 0.6360 -0.0135 0.0473 0.033 Uiso 1 1 calc R . . C29 C 0.6980(2) 0.08522(14) 0.06461(12) 0.0313(6) Uani 1 1 d . . . H29 H 0.7579 0.0814 0.0402 0.038 Uiso 1 1 calc R . . C30 C 0.6842(2) 0.14671(14) 0.09545(12) 0.0294(5) Uani 1 1 d . . . H30 H 0.7347 0.1848 0.0928 0.035 Uiso 1 1 calc R . . C31 C 0.5957(2) 0.15246(13) 0.13036(11) 0.0266(5) Uani 1 1 d . . . H31 H 0.5853 0.1951 0.1513 0.032 Uiso 1 1 calc R . . C32 C 0.52228(19) 0.09699(12) 0.13505(10) 0.0223(5) Uani 1 1 d . . . N1 N 0.24074(16) 0.12617(10) 0.21758(8) 0.0206(4) Uani 1 1 d . . . N2 N 0.42776(16) 0.10609(10) 0.16725(8) 0.0210(4) Uani 1 1 d . . . N3 N 0.11357(16) 0.23009(10) 0.14354(8) 0.0198(4) Uani 1 1 d . . . N4 N 0.18587(16) 0.32231(10) 0.06233(8) 0.0197(4) Uani 1 1 d . . . N5 N 0.25652(18) -0.09207(11) 0.08233(9) 0.0260(4) Uani 1 1 d . . . O1 O 0.21009(13) 0.06726(9) 0.10008(7) 0.0233(4) Uani 1 1 d . . . O2 O 0.46244(14) -0.01933(9) 0.11204(7) 0.0261(4) Uani 1 1 d . . . Co1 Co 0.29331(3) 0.171947(19) 0.147652(15) 0.01919(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0280(12) 0.0185(10) 0.0237(11) -0.0013(9) -0.0028(10) -0.0024(9) C2 0.0282(12) 0.0193(11) 0.0215(12) 0.0006(9) -0.0025(10) -0.0013(9) C3 0.0349(14) 0.0263(12) 0.0228(12) 0.0065(10) -0.0029(10) 0.0002(10) C4 0.0332(13) 0.0292(12) 0.0212(12) 0.0067(10) 0.0013(10) -0.0042(10) C5 0.0258(12) 0.0218(11) 0.0174(10) -0.0002(9) 0.0013(9) -0.0058(9) C6 0.0239(12) 0.0206(11) 0.0226(12) 0.0011(9) 0.0028(9) -0.0047(9) C7 0.0268(12) 0.0277(12) 0.0250(12) 0.0042(10) 0.0040(10) -0.0041(10) C8 0.0285(14) 0.0383(15) 0.0392(15) 0.0098(12) 0.0083(12) 0.0000(11) C9 0.0348(14) 0.0226(11) 0.0249(12) -0.0008(9) 0.0030(10) -0.0044(10) C10 0.0519(18) 0.0358(14) 0.0258(14) -0.0044(11) 0.0060(12) -0.0095(13) C11 0.0229(11) 0.0184(10) 0.0226(12) 0.0013(9) 0.0005(9) -0.0003(9) C12 0.0232(12) 0.0224(11) 0.0285(12) 0.0008(10) -0.0012(10) -0.0050(9) C13 0.0252(12) 0.0218(11) 0.0249(12) -0.0014(9) -0.0041(10) -0.0021(9) C14 0.0235(11) 0.0198(10) 0.0191(11) 0.0001(9) -0.0023(9) 0.0006(9) C15 0.0222(11) 0.0213(11) 0.0216(11) 0.0007(9) -0.0031(9) 0.0029(9) C16 0.0227(11) 0.0192(10) 0.0230(11) 0.0019(9) 0.0021(9) 0.0031(9) C17 0.0286(12) 0.0218(11) 0.0256(12) 0.0001(9) -0.0006(10) 0.0022(10) C18 0.0375(14) 0.0284(12) 0.0211(11) 0.0015(10) 0.0053(10) 0.0049(11) C19 0.0282(13) 0.0306(13) 0.0275(12) 0.0071(10) 0.0078(10) -0.0002(10) C20 0.0262(12) 0.0254(12) 0.0276(12) 0.0034(10) 0.0031(10) -0.0037(10) C21 0.0252(12) 0.0229(11) 0.0203(11) -0.0002(9) -0.0028(9) 0.0003(9) C22 0.0287(12) 0.0210(11) 0.0235(12) 0.0032(9) 0.0002(10) -0.0048(9) C23 0.0308(13) 0.0242(12) 0.0242(12) 0.0018(10) -0.0028(10) -0.0048(10) C24 0.0370(15) 0.0247(13) 0.0372(14) -0.0048(11) -0.0071(12) -0.0040(11) C25 0.0331(14) 0.0229(12) 0.0346(14) -0.0044(10) -0.0079(11) -0.0006(10) C26 0.0300(13) 0.0262(12) 0.0292(13) -0.0066(10) -0.0006(11) 0.0015(10) C27 0.0244(12) 0.0214(11) 0.0236(11) 0.0019(9) -0.0040(10) -0.0003(9) C28 0.0296(13) 0.0245(12) 0.0295(13) -0.0020(10) 0.0001(11) 0.0026(10) C29 0.0293(13) 0.0310(13) 0.0336(14) 0.0020(11) 0.0068(11) 0.0016(10) C30 0.0266(13) 0.0235(12) 0.0380(14) 0.0006(11) 0.0016(11) -0.0027(10) C31 0.0269(12) 0.0218(12) 0.0311(13) -0.0008(10) -0.0016(10) -0.0010(10) C32 0.0242(12) 0.0216(11) 0.0211(11) 0.0011(9) -0.0040(9) 0.0001(9) N1 0.0245(10) 0.0182(9) 0.0192(9) 0.0005(7) -0.0012(8) -0.0040(7) N2 0.0221(10) 0.0194(9) 0.0216(9) 0.0000(8) -0.0026(8) -0.0010(7) N3 0.0212(9) 0.0172(9) 0.0209(9) -0.0001(7) -0.0016(8) -0.0047(7) N4 0.0235(10) 0.0183(9) 0.0174(9) 0.0012(7) 0.0003(8) 0.0015(7) N5 0.0263(10) 0.0230(10) 0.0286(11) -0.0040(8) -0.0044(9) -0.0022(8) O1 0.0267(9) 0.0226(8) 0.0205(8) 0.0007(6) -0.0025(7) -0.0065(7) O2 0.0282(9) 0.0216(8) 0.0284(9) -0.0023(7) -0.0022(7) -0.0039(7) Co1 0.0228(2) 0.0175(2) 0.0173(2) 0.00139(14) -0.00029(15) -0.00285(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.296(3) . ? C1 C2 1.418(3) . ? C1 H1 0.9500 . ? C2 N1 1.378(3) . ? C2 C3 1.394(3) . ? C3 C4 1.396(4) . ? C3 H3 0.9500 . ? C4 C5 1.402(3) . ? C4 H4 0.9500 . ? C5 N1 1.348(3) . ? C5 C6 1.515(3) . ? C6 C11 1.522(3) . ? C6 C7 1.548(3) . ? C6 C9 1.552(3) . ? C7 C8 1.524(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.523(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N3 1.371(3) . ? C11 C12 1.399(3) . ? C12 C13 1.391(3) . ? C12 H12 0.9500 . ? C13 C14 1.388(3) . ? C13 H13 0.9500 . ? C14 N3 1.396(3) . ? C14 C15 1.413(3) . ? C15 N4 1.301(3) . ? C15 H15 0.9500 . ? C16 C17 1.390(3) . ? C16 N4 1.404(3) . ? C16 C21 1.410(3) 2 ? C17 C18 1.391(4) . ? C17 H17 0.9500 . ? C18 C19 1.379(4) . ? C18 H18 0.9500 . ? C19 C20 1.389(4) . ? C19 H19 0.9500 . ? C20 C21 1.391(3) 2 ? C20 H20 0.9500 . ? C21 O1 1.366(3) . ? C21 C20 1.391(3) 2 ? C21 C16 1.410(3) 2 ? C22 O1 1.444(3) . ? C22 C23 1.512(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 N5 1.470(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 N5 1.465(3) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 N5 1.463(3) . ? C25 C26 1.511(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O2 1.431(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 O2 1.375(3) . ? C27 C28 1.385(4) . ? C27 C32 1.407(3) . ? C28 C29 1.391(4) . ? C28 H28 0.9500 . ? C29 C30 1.377(4) . ? C29 H29 0.9500 . ? C30 C31 1.387(4) . ? C30 H30 0.9500 . ? C31 C32 1.383(3) . ? C31 H31 0.9500 . ? C32 N2 1.415(3) . ? N1 Co1 1.997(2) . ? N2 Co1 2.125(2) . ? N3 Co1 2.1642(19) 2 ? N4 Co1 2.072(2) 2 ? Co1 N4 2.072(2) 2 ? Co1 N3 2.1642(19) 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 N2 C1 C2 117.7(2) . . ? N2 C1 H1 121.1 . . ? C2 C1 H1 121.1 . . ? N1 C2 C3 109.7(2) . . ? N1 C2 C1 116.8(2) . . ? C3 C2 C1 133.4(2) . . ? C2 C3 C4 106.0(2) . . ? C2 C3 H3 127.0 . . ? C4 C3 H3 127.0 . . ? C3 C4 C5 107.4(2) . . ? C3 C4 H4 126.3 . . ? C5 C4 H4 126.3 . . ? N1 C5 C4 109.3(2) . . ? N1 C5 C6 120.5(2) . . ? C4 C5 C6 130.1(2) . . ? C5 C6 C11 109.38(19) . . ? C5 C6 C7 108.51(19) . . ? C11 C6 C7 109.6(2) . . ? C5 C6 C9 109.0(2) . . ? C11 C6 C9 109.56(18) . . ? C7 C6 C9 110.8(2) . . ? C8 C7 C6 115.6(2) . . ? C8 C7 H7A 108.4 . . ? C6 C7 H7A 108.4 . . ? C8 C7 H7B 108.4 . . ? C6 C7 H7B 108.4 . . ? H7A C7 H7B 107.4 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C6 115.1(2) . . ? C10 C9 H9A 108.5 . . ? C6 C9 H9A 108.5 . . ? C10 C9 H9B 108.5 . . ? C6 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 C12 110.2(2) . . ? N3 C11 C6 123.8(2) . . ? C12 C11 C6 126.0(2) . . ? C13 C12 C11 107.6(2) . . ? C13 C12 H12 126.2 . . ? C11 C12 H12 126.2 . . ? C14 C13 C12 106.0(2) . . ? C14 C13 H13 127.0 . . ? C12 C13 H13 127.0 . . ? C13 C14 N3 110.9(2) . . ? C13 C14 C15 129.0(2) . . ? N3 C14 C15 119.8(2) . . ? N4 C15 C14 119.7(2) . . ? N4 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C17 C16 N4 124.4(2) . . ? C17 C16 C21 119.1(2) . 2 ? N4 C16 C21 116.3(2) . 2 ? C16 C17 C18 120.8(2) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C19 C18 C17 119.5(2) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 121.0(2) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C19 C20 C21 119.8(2) . 2 ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 2 . ? O1 C21 C20 125.9(2) . 2 ? O1 C21 C16 114.3(2) . 2 ? C20 C21 C16 119.8(2) 2 2 ? O1 C22 C23 111.2(2) . . ? O1 C22 H22A 109.4 . . ? C23 C22 H22A 109.4 . . ? O1 C22 H22B 109.4 . . ? C23 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? N5 C23 C22 114.1(2) . . ? N5 C23 H23A 108.7 . . ? C22 C23 H23A 108.7 . . ? N5 C23 H23B 108.7 . . ? C22 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? N5 C24 H24A 109.5 . . ? N5 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N5 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N5 C25 C26 115.1(2) . . ? N5 C25 H25A 108.5 . . ? C26 C25 H25A 108.5 . . ? N5 C25 H25B 108.5 . . ? C26 C25 H25B 108.5 . . ? H25A C25 H25B 107.5 . . ? O2 C26 C25 110.5(2) . . ? O2 C26 H26A 109.6 . . ? C25 C26 H26A 109.6 . . ? O2 C26 H26B 109.6 . . ? C25 C26 H26B 109.6 . . ? H26A C26 H26B 108.1 . . ? O2 C27 C28 124.7(2) . . ? O2 C27 C32 116.0(2) . . ? C28 C27 C32 119.4(2) . . ? C27 C28 C29 120.0(2) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 120.9(2) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C29 C30 C31 119.3(2) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? C32 C31 C30 120.8(2) . . ? C32 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? C31 C32 C27 119.6(2) . . ? C31 C32 N2 120.0(2) . . ? C27 C32 N2 120.2(2) . . ? C5 N1 C2 107.56(19) . . ? C5 N1 Co1 138.32(17) . . ? C2 N1 Co1 113.51(16) . . ? C1 N2 C32 120.9(2) . . ? C1 N2 Co1 111.94(16) . . ? C32 N2 Co1 126.73(15) . . ? C11 N3 C14 105.17(18) . . ? C11 N3 Co1 143.47(16) . 2 ? C14 N3 Co1 105.57(14) . 2 ? C15 N4 C16 122.5(2) . . ? C15 N4 Co1 112.07(16) . 2 ? C16 N4 Co1 125.46(16) . 2 ? C25 N5 C24 110.5(2) . . ? C25 N5 C23 112.2(2) . . ? C24 N5 C23 109.8(2) . . ? C21 O1 C22 120.49(18) . . ? C27 O2 C26 117.59(19) . . ? N1 Co1 N4 153.89(8) . 2 ? N1 Co1 N2 79.75(8) . . ? N4 Co1 N2 98.74(8) 2 . ? N1 Co1 N3 125.04(7) . 2 ? N4 Co1 N3 81.05(7) 2 2 ? N2 Co1 N3 94.56(7) . 2 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C1 C2 N1 -0.1(3) . . . . ? N2 C1 C2 C3 176.0(3) . . . . ? N1 C2 C3 C4 0.5(3) . . . . ? C1 C2 C3 C4 -175.8(3) . . . . ? C2 C3 C4 C5 -0.3(3) . . . . ? C3 C4 C5 N1 0.1(3) . . . . ? C3 C4 C5 C6 -177.8(2) . . . . ? N1 C5 C6 C11 37.9(3) . . . . ? C4 C5 C6 C11 -144.4(3) . . . . ? N1 C5 C6 C7 157.4(2) . . . . ? C4 C5 C6 C7 -24.9(3) . . . . ? N1 C5 C6 C9 -81.9(3) . . . . ? C4 C5 C6 C9 95.8(3) . . . . ? C5 C6 C7 C8 174.1(2) . . . . ? C11 C6 C7 C8 -66.5(3) . . . . ? C9 C6 C7 C8 54.5(3) . . . . ? C5 C6 C9 C10 -63.1(3) . . . . ? C11 C6 C9 C10 177.2(2) . . . . ? C7 C6 C9 C10 56.2(3) . . . . ? C5 C6 C11 N3 -78.6(3) . . . . ? C7 C6 C11 N3 162.5(2) . . . . ? C9 C6 C11 N3 40.8(3) . . . . ? C5 C6 C11 C12 100.1(3) . . . . ? C7 C6 C11 C12 -18.8(3) . . . . ? C9 C6 C11 C12 -140.5(2) . . . . ? N3 C11 C12 C13 -2.1(3) . . . . ? C6 C11 C12 C13 179.0(2) . . . . ? C11 C12 C13 C14 0.3(3) . . . . ? C12 C13 C14 N3 1.6(3) . . . . ? C12 C13 C14 C15 -172.0(2) . . . . ? C13 C14 C15 N4 169.9(2) . . . . ? N3 C14 C15 N4 -3.3(3) . . . . ? N4 C16 C17 C18 -175.0(2) . . . . ? C21 C16 C17 C18 0.0(4) 2 . . . ? C16 C17 C18 C19 0.7(4) . . . . ? C17 C18 C19 C20 -0.9(4) . . . . ? C18 C19 C20 C21 0.5(4) . . . 2 ? O1 C22 C23 N5 -70.5(3) . . . . ? N5 C25 C26 O2 63.2(3) . . . . ? O2 C27 C28 C29 -178.5(2) . . . . ? C32 C27 C28 C29 0.6(4) . . . . ? C27 C28 C29 C30 0.3(4) . . . . ? C28 C29 C30 C31 -1.0(4) . . . . ? C29 C30 C31 C32 0.8(4) . . . . ? C30 C31 C32 C27 0.0(4) . . . . ? C30 C31 C32 N2 -174.7(2) . . . . ? O2 C27 C32 C31 178.5(2) . . . . ? C28 C27 C32 C31 -0.7(3) . . . . ? O2 C27 C32 N2 -6.9(3) . . . . ? C28 C27 C32 N2 174.0(2) . . . . ? C4 C5 N1 C2 0.2(3) . . . . ? C6 C5 N1 C2 178.3(2) . . . . ? C4 C5 N1 Co1 170.14(18) . . . . ? C6 C5 N1 Co1 -11.8(4) . . . . ? C3 C2 N1 C5 -0.4(3) . . . . ? C1 C2 N1 C5 176.6(2) . . . . ? C3 C2 N1 Co1 -173.14(16) . . . . ? C1 C2 N1 Co1 3.8(3) . . . . ? C2 C1 N2 C32 -176.1(2) . . . . ? C2 C1 N2 Co1 -3.4(3) . . . . ? C31 C32 N2 C1 -118.1(3) . . . . ? C27 C32 N2 C1 67.2(3) . . . . ? C31 C32 N2 Co1 70.4(3) . . . . ? C27 C32 N2 Co1 -104.3(2) . . . . ? C12 C11 N3 C14 3.0(3) . . . . ? C6 C11 N3 C14 -178.1(2) . . . . ? C12 C11 N3 Co1 149.4(2) . . . 2 ? C6 C11 N3 Co1 -31.7(4) . . . 2 ? C13 C14 N3 C11 -2.8(3) . . . . ? C15 C14 N3 C11 171.4(2) . . . . ? C13 C14 N3 Co1 -162.87(16) . . . 2 ? C15 C14 N3 Co1 11.4(2) . . . 2 ? C14 C15 N4 C16 171.8(2) . . . . ? C14 C15 N4 Co1 -7.7(3) . . . 2 ? C17 C16 N4 C15 -15.5(4) . . . . ? C21 C16 N4 C15 169.4(2) 2 . . . ? C17 C16 N4 Co1 163.95(19) . . . 2 ? C21 C16 N4 Co1 -11.2(3) 2 . . 2 ? C26 C25 N5 C24 154.3(2) . . . . ? C26 C25 N5 C23 -82.7(3) . . . . ? C22 C23 N5 C25 149.8(2) . . . . ? C22 C23 N5 C24 -86.8(3) . . . . ? C20 C21 O1 C22 3.0(4) 2 . . . ? C16 C21 O1 C22 -179.1(2) 2 . . . ? C23 C22 O1 C21 95.5(2) . . . . ? C28 C27 O2 C26 -18.3(3) . . . . ? C32 C27 O2 C26 162.6(2) . . . . ? C25 C26 O2 C27 -175.2(2) . . . . ? C5 N1 Co1 N4 -84.8(3) . . . 2 ? C2 N1 Co1 N4 84.7(2) . . . 2 ? C5 N1 Co1 N2 -173.8(2) . . . . ? C2 N1 Co1 N2 -4.21(15) . . . . ? C5 N1 Co1 N3 97.9(2) . . . 2 ? C2 N1 Co1 N3 -92.59(17) . . . 2 ? C1 N2 Co1 N1 4.21(16) . . . . ? C32 N2 Co1 N1 176.35(19) . . . . ? C1 N2 Co1 N4 -149.35(16) . . . 2 ? C32 N2 Co1 N4 22.79(19) . . . 2 ? C1 N2 Co1 N3 129.02(16) . . . 2 ? C32 N2 Co1 N3 -58.84(19) . . . 2 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 73.27 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.457 _refine_diff_density_min -0.430 _refine_diff_density_rms 0.063