Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 _publ_contact_author_name 'Geoffrey A. Lawrance' _publ_contact_author_address ; Discipline of Chemistry, School of Environmental and Life Sciences, The University of Newcastle, Callaghan, N.S.W. 2308, Australia ; _publ_contact_author_email geoffrey.lawrance@newcastle.edu.au _publ_contact_author_fax '+61 2 492 15472' _publ_contact_author_phone '+61 2 492 15474' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Geometrical Isomerism in Octahedral Complexes Arising from the Presence of a Fused ring on a Triaza Macrocycle ; loop_ _publ_author_name _publ_author_address 'Geoffrey A. Lawrance' ; Discipline of Chemistry, School of Environmental and Life Sciences, The University of Newcastle, Callaghan, N.S.W. 2308, Australia ; 'Peter Comba' ; Anorganisch-Chemisches Institut der Universität Heidelberg, Im Neuenheimer Feld 270, D-69120 Heidelberg, Germany ; 'Geoffry N. DeIuliis' ; Discipline of Chemistry, School of Environmental and Life Sciences, The University of Newcastle, Callaghan, N.S.W. 2308, Australia ; 'Stephan M. Luther' ; Discipline of Chemistry, School of Environmental and Life Sciences, The University of Newcastle, Callaghan, N.S.W. 2308, Australia ; 'Marcel Maeder' ; Discipline of Chemistry, School of Environmental and Life Sciences, The University of Newcastle, Callaghan, N.S.W. 2308, Australia ; 'Annette L. Nolan' ; Discipline of Chemistry, School of Environmental and Life Sciences, The University of Newcastle, Callaghan, N.S.W. 2308, Australia ; 'Mark J. Robertson' ; Discipline of Chemistry, School of Environmental and Life Sciences, The University of Newcastle, Callaghan, N.S.W. 2308, Australia ; 'Peter Turner' ; Crystal Structure Analysis Facility, School of Chemistry, The University of Sydney, N.S.W. 2006, Australia ; #======================================================== data_gal1 _database_code_CSD 195129 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H42 N8 Ni O6' _chemical_formula_weight 549.33 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' Ni Ni 0.3393 1.1124 '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' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.590(2) _cell_length_b 11.754(3) _cell_length_c 12.725(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.509(4) _cell_angle_gamma 90.00 _cell_volume 1249.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 986 _cell_measurement_theta_min 2.439 _cell_measurement_theta_max 25.774 _exptl_crystal_description prism _exptl_crystal_colour 'pale pink' _exptl_crystal_size_max 0.181 _exptl_crystal_size_mid 0.112 _exptl_crystal_size_min 0.074 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 0.829 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.886 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _diffrn_crystal_treatment ; attached to a thin glass fibre ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_standards_number 137 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 11997 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 26.41 _reflns_number_total 5026 _reflns_number_gt 4676 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker,1995)' _computing_cell_refinement 'SAINT (Bruker,1995)' _computing_data_reduction 'SAINT and XPREP (Bruker 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; teXsan for Windows (MSC, 1997) xtal 3.6 (Hall,du Boulay, D.J. & Olthof-Hazekamp, R. 1999) ORTEPII (Johnson,C.K., 1976). WinGX (Farrugia, 1999) ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0338P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.001(9) _refine_ls_number_reflns 5026 _refine_ls_number_parameters 316 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0634 _refine_ls_wR_factor_gt 0.0616 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 Ni1 Ni 0.26486(2) 0.16907(3) 0.748205(19) 0.02972(7) Uani 1 1 d . . . N1 N 0.06908(19) 0.08468(15) 0.64695(14) 0.0358(4) Uani 1 1 d . . . H1N H -0.0236 0.1200 0.6511 0.043 Uiso 1 1 calc R . . N2 N 0.32274(18) 0.00018(15) 0.80620(14) 0.0335(4) Uani 1 1 d . . . H2N H 0.3744 0.0031 0.8773 0.040 Uiso 1 1 calc R . . N3 N 0.38333(19) 0.11562(15) 0.62932(14) 0.0352(4) Uani 1 1 d . . . H3N H 0.4345 0.1761 0.6080 0.042 Uiso 1 1 calc R . . N4 N 0.45688(19) 0.25150(15) 0.85562(13) 0.0324(4) Uani 1 1 d . . . H4N H 0.5422 0.2034 0.8719 0.039 Uiso 1 1 calc R . . N5 N 0.21546(19) 0.33961(15) 0.69154(15) 0.0377(4) Uani 1 1 d . . . H5N H 0.2040 0.3417 0.6186 0.045 Uiso 1 1 calc R . . N6 N 0.1364(2) 0.22151(16) 0.86171(16) 0.0414(4) Uani 1 1 d . . . H6N H 0.0576 0.1704 0.8637 0.050 Uiso 1 1 calc R . . C1 C 0.0638(3) -0.0370(2) 0.68122(19) 0.0371(5) Uani 1 1 d . . . H10 H 0.1104 -0.0836 0.6325 0.044 Uiso 1 1 calc R . . C2 C -0.1067(3) -0.0790(2) 0.6732(2) 0.0539(7) Uani 1 1 d . . . H9A H -0.1568 -0.0326 0.7192 0.065 Uiso 1 1 calc R . . H9B H -0.1685 -0.0708 0.5994 0.065 Uiso 1 1 calc R . . C3 C -0.1083(3) -0.2030(3) 0.7072(3) 0.0678(8) Uani 1 1 d . . . H8A H -0.2172 -0.2253 0.7066 0.081 Uiso 1 1 calc R . . H8B H -0.0712 -0.2503 0.6556 0.081 Uiso 1 1 calc R . . C4 C -0.0031(3) -0.2229(3) 0.8189(2) 0.0644(8) Uani 1 1 d . . . H7A H -0.0007 -0.3036 0.8353 0.077 Uiso 1 1 calc R . . H7B H -0.0482 -0.1835 0.8719 0.077 Uiso 1 1 calc R . . C5 C 0.1673(3) -0.1807(2) 0.8269(2) 0.0508(6) Uani 1 1 d . . . H6A H 0.2165 -0.2248 0.7789 0.061 Uiso 1 1 calc R . . H6B H 0.2304 -0.1907 0.9001 0.061 Uiso 1 1 calc R . . C6 C 0.1644(2) -0.05484(18) 0.79582(17) 0.0357(5) Uani 1 1 d . . . H5 H 0.1103 -0.0141 0.8444 0.043 Uiso 1 1 calc R . . C7 C 0.0949(3) 0.0982(2) 0.53708(18) 0.0446(6) Uani 1 1 d . . . H1A H 0.0723 0.1762 0.5134 0.053 Uiso 1 1 calc R . . H1B H 0.0217 0.0491 0.4876 0.053 Uiso 1 1 calc R . . C8 C 0.2668(3) 0.0686(2) 0.53414(18) 0.0438(5) Uani 1 1 d . . . H2A H 0.2784 -0.0134 0.5329 0.053 Uiso 1 1 calc R . . H2B H 0.2899 0.0989 0.4685 0.053 Uiso 1 1 calc R . . C9 C 0.4287(2) -0.05592(19) 0.7437(2) 0.0386(5) Uani 1 1 d . . . H4A H 0.3666 -0.1095 0.6927 0.046 Uiso 1 1 calc R . . H4B H 0.5126 -0.0978 0.7928 0.046 Uiso 1 1 calc R . . C10 C 0.5031(2) 0.03180(19) 0.68339(18) 0.0400(5) Uani 1 1 d . . . H3A H 0.5888 0.0707 0.7337 0.048 Uiso 1 1 calc R . . H3B H 0.5489 -0.0060 0.6299 0.048 Uiso 1 1 calc R . . C11 C 0.4974(2) 0.34991(19) 0.79374(18) 0.0349(5) Uani 1 1 d . . . H20 H 0.5369 0.3186 0.7335 0.042 Uiso 1 1 calc R . . C12 C 0.6279(2) 0.4297(2) 0.85601(19) 0.0438(5) Uani 1 1 d . . . H19A H 0.5917 0.4654 0.9147 0.053 Uiso 1 1 calc R . . H19B H 0.7237 0.3862 0.8868 0.053 Uiso 1 1 calc R . . C13 C 0.6663(3) 0.5207(2) 0.7808(2) 0.0537(6) Uani 1 1 d . . . H18A H 0.7463 0.5722 0.8215 0.064 Uiso 1 1 calc R . . H18B H 0.7105 0.4851 0.7254 0.064 Uiso 1 1 calc R . . C14 C 0.5174(3) 0.5874(2) 0.7279(2) 0.0580(7) Uani 1 1 d . . . H17A H 0.5437 0.6413 0.6771 0.070 Uiso 1 1 calc R . . H17B H 0.4806 0.6300 0.7828 0.070 Uiso 1 1 calc R . . C15 C 0.3839(3) 0.5094(2) 0.6690(2) 0.0509(6) Uani 1 1 d . . . H16A H 0.4152 0.4741 0.6082 0.061 Uiso 1 1 calc R . . H16B H 0.2880 0.5539 0.6412 0.061 Uiso 1 1 calc R . . C16 C 0.3484(2) 0.41724(19) 0.74479(18) 0.0374(5) Uani 1 1 d . . . H15 H 0.3147 0.4557 0.8041 0.045 Uiso 1 1 calc R . . C17 C 0.4076(3) 0.2817(2) 0.95669(17) 0.0423(5) Uani 1 1 d . . . H11A H 0.3899 0.3632 0.9582 0.051 Uiso 1 1 calc R . . H11B H 0.4931 0.2623 1.0185 0.051 Uiso 1 1 calc R . . C18 C 0.2562(3) 0.2200(2) 0.96501(19) 0.0466(6) Uani 1 1 d . . . H12A H 0.2820 0.1418 0.9866 0.056 Uiso 1 1 calc R . . H12B H 0.2118 0.2558 1.0202 0.056 Uiso 1 1 calc R . . C19 C 0.0615(3) 0.3676(2) 0.7176(2) 0.0511(7) Uani 1 1 d . . . H14A H -0.0242 0.3264 0.6694 0.061 Uiso 1 1 calc R . . H14B H 0.0404 0.4483 0.7069 0.061 Uiso 1 1 calc R . . C20 C 0.0649(3) 0.3367(2) 0.8329(2) 0.0535(7) Uani 1 1 d . . . H13A H 0.1268 0.3930 0.8807 0.064 Uiso 1 1 calc R . . H13B H -0.0434 0.3377 0.8433 0.064 Uiso 1 1 calc R . . N7 N 0.6846(2) 0.25354(17) 0.52810(16) 0.0423(4) Uani 1 1 d . . . O1 O 0.5430(2) 0.28635(18) 0.49988(16) 0.0655(5) Uani 1 1 d . . . O2 O 0.7806(2) 0.27163(18) 0.47125(16) 0.0686(6) Uani 1 1 d . . . O3 O 0.7294(2) 0.2023(2) 0.61414(17) 0.0775(8) Uani 1 1 d . . . N8 N -0.1918(2) 0.08146(18) 0.95295(18) 0.0496(5) Uani 1 1 d . . . O4 O -0.0609(3) 0.0350(2) 0.9871(2) 0.1025(9) Uani 1 1 d . . . O5 O -0.3128(2) 0.0563(2) 0.98624(18) 0.0794(6) Uani 1 1 d . . . O6 O -0.19897(19) 0.1578(2) 0.88658(17) 0.0782(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 Ni1 0.02518(11) 0.03061(11) 0.03479(12) -0.00170(11) 0.00992(8) -0.00103(13) N1 0.0265(8) 0.0410(10) 0.0401(11) -0.0022(8) 0.0079(7) 0.0027(7) N2 0.0297(8) 0.0368(10) 0.0339(10) -0.0025(8) 0.0073(7) -0.0026(7) N3 0.0340(8) 0.0337(9) 0.0422(11) -0.0015(8) 0.0173(7) -0.0044(7) N4 0.0285(8) 0.0341(9) 0.0365(10) 0.0009(8) 0.0112(7) -0.0003(7) N5 0.0339(9) 0.0375(10) 0.0392(11) 0.0020(8) 0.0035(7) -0.0002(8) N6 0.0350(9) 0.0384(10) 0.0565(12) -0.0056(9) 0.0224(8) -0.0046(8) C1 0.0301(11) 0.0406(12) 0.0419(13) -0.0080(10) 0.0114(9) -0.0060(9) C2 0.0312(11) 0.0650(17) 0.0662(17) -0.0098(14) 0.0129(10) -0.0114(11) C3 0.0522(15) 0.0642(18) 0.090(2) -0.0134(16) 0.0225(15) -0.0314(13) C4 0.0713(18) 0.0529(17) 0.077(2) -0.0002(14) 0.0336(15) -0.0239(13) C5 0.0556(14) 0.0422(14) 0.0569(16) 0.0060(12) 0.0176(12) -0.0086(11) C6 0.0342(10) 0.0376(11) 0.0384(12) -0.0009(10) 0.0149(9) -0.0053(9) C7 0.0435(12) 0.0501(15) 0.0371(13) -0.0007(10) 0.0035(9) 0.0001(10) C8 0.0487(12) 0.0484(14) 0.0370(13) 0.0001(10) 0.0156(10) 0.0011(10) C9 0.0265(10) 0.0366(12) 0.0523(14) -0.0021(11) 0.0084(9) 0.0042(9) C10 0.0280(10) 0.0433(12) 0.0517(14) -0.0070(10) 0.0155(9) 0.0014(9) C11 0.0300(10) 0.0374(11) 0.0397(12) -0.0007(10) 0.0129(8) -0.0034(8) C12 0.0351(11) 0.0451(13) 0.0522(14) -0.0042(11) 0.0122(10) -0.0074(10) C13 0.0465(13) 0.0513(14) 0.0679(17) -0.0044(13) 0.0224(12) -0.0176(11) C14 0.0610(15) 0.0429(14) 0.0743(19) 0.0059(13) 0.0238(14) -0.0146(12) C15 0.0525(13) 0.0420(14) 0.0574(16) 0.0103(12) 0.0114(11) -0.0020(11) C16 0.0335(11) 0.0361(12) 0.0425(13) -0.0016(10) 0.0083(9) -0.0046(9) C17 0.0475(12) 0.0456(14) 0.0357(12) -0.0038(10) 0.0134(10) -0.0041(10) C18 0.0543(13) 0.0516(13) 0.0413(13) -0.0056(10) 0.0261(11) -0.0065(11) C19 0.0314(12) 0.0372(13) 0.081(2) -0.0016(13) 0.0052(12) 0.0035(10) C20 0.0356(11) 0.0440(13) 0.088(2) -0.0112(13) 0.0287(12) 0.0033(10) N7 0.0381(10) 0.0382(10) 0.0515(12) 0.0063(9) 0.0123(8) -0.0047(8) O1 0.0455(10) 0.0706(13) 0.0805(13) 0.0165(11) 0.0148(9) 0.0075(9) O2 0.0589(11) 0.0777(15) 0.0803(13) 0.0263(11) 0.0387(10) 0.0074(10) O3 0.0490(9) 0.107(2) 0.0769(13) 0.0474(13) 0.0147(9) -0.0023(10) N8 0.0486(11) 0.0440(12) 0.0575(13) 0.0065(10) 0.0151(10) 0.0037(9) O4 0.0842(16) 0.103(2) 0.130(2) 0.0562(17) 0.0458(16) 0.0473(15) O5 0.0669(12) 0.0813(16) 0.0995(17) 0.0310(13) 0.0385(11) -0.0027(11) O6 0.0498(9) 0.0801(15) 0.1020(15) 0.0486(15) 0.0125(9) -0.0063(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N6 2.1043(18) . ? Ni1 N3 2.1067(17) . ? Ni1 N1 2.1119(18) . ? Ni1 N4 2.1153(17) . ? Ni1 N2 2.1356(19) . ? Ni1 N5 2.1390(19) . ? N1 C7 1.475(3) . ? N1 C1 1.499(3) . ? N1 H1N 0.9100 . ? N2 C6 1.484(2) . ? N2 C9 1.495(3) . ? N2 H2N 0.9100 . ? N3 C10 1.474(3) . ? N3 C8 1.486(3) . ? N3 H3N 0.9100 . ? N4 C11 1.486(3) . ? N4 C17 1.488(3) . ? N4 H4N 0.9100 . ? N5 C19 1.474(3) . ? N5 C16 1.495(3) . ? N5 H5N 0.9100 . ? N6 C18 1.468(3) . ? N6 C20 1.496(3) . ? N6 H6N 0.9100 . ? C1 C6 1.526(3) . ? C1 C2 1.526(3) . ? C1 H10 0.9800 . ? C2 C3 1.522(4) . ? C2 H9A 0.9700 . ? C2 H9B 0.9700 . ? C3 C4 1.514(4) . ? C3 H8A 0.9700 . ? C3 H8B 0.9700 . ? C4 C5 1.526(3) . ? C4 H7A 0.9700 . ? C4 H7B 0.9700 . ? C5 C6 1.530(3) . ? C5 H6A 0.9700 . ? C5 H6B 0.9700 . ? C6 H5 0.9800 . ? C7 C8 1.526(3) . ? C7 H1A 0.9700 . ? C7 H1B 0.9700 . ? C8 H2A 0.9700 . ? C8 H2B 0.9700 . ? C9 C10 1.513(3) . ? C9 H4A 0.9700 . ? C9 H4B 0.9700 . ? C10 H3A 0.9700 . ? C10 H3B 0.9700 . ? C11 C16 1.510(3) . ? C11 C12 1.532(3) . ? C11 H20 0.9800 . ? C12 C13 1.522(3) . ? C12 H19A 0.9700 . ? C12 H19B 0.9700 . ? C13 C14 1.517(4) . ? C13 H18A 0.9700 . ? C13 H18B 0.9700 . ? C14 C15 1.522(4) . ? C14 H17A 0.9700 . ? C14 H17B 0.9700 . ? C15 C16 1.528(3) . ? C15 H16A 0.9700 . ? C15 H16B 0.9700 . ? C16 H15 0.9800 . ? C17 C18 1.514(3) . ? C17 H11A 0.9700 . ? C17 H11B 0.9700 . ? C18 H12A 0.9700 . ? C18 H12B 0.9700 . ? C19 C20 1.504(4) . ? C19 H14A 0.9700 . ? C19 H14B 0.9700 . ? C20 H13A 0.9700 . ? C20 H13B 0.9700 . ? N7 O3 1.230(3) . ? N7 O2 1.236(2) . ? N7 O1 1.247(2) . ? N8 O6 1.224(3) . ? N8 O4 1.235(3) . ? N8 O5 1.245(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Ni1 N3 177.36(8) . . ? N6 Ni1 N1 94.93(7) . . ? N3 Ni1 N1 82.60(7) . . ? N6 Ni1 N4 82.93(7) . . ? N3 Ni1 N4 99.56(7) . . ? N1 Ni1 N4 177.44(7) . . ? N6 Ni1 N2 98.75(7) . . ? N3 Ni1 N2 81.86(7) . . ? N1 Ni1 N2 82.08(7) . . ? N4 Ni1 N2 96.83(7) . . ? N6 Ni1 N5 82.09(7) . . ? N3 Ni1 N5 97.38(7) . . ? N1 Ni1 N5 99.64(7) . . ? N4 Ni1 N5 81.48(7) . . ? N2 Ni1 N5 178.03(6) . . ? C7 N1 C1 113.59(17) . . ? C7 N1 Ni1 104.65(13) . . ? C1 N1 Ni1 110.15(13) . . ? C7 N1 H1N 109.4 . . ? C1 N1 H1N 109.4 . . ? Ni1 N1 H1N 109.4 . . ? C6 N2 C9 114.83(17) . . ? C6 N2 Ni1 103.87(12) . . ? C9 N2 Ni1 110.36(13) . . ? C6 N2 H2N 109.2 . . ? C9 N2 H2N 109.2 . . ? Ni1 N2 H2N 109.2 . . ? C10 N3 C8 113.32(17) . . ? C10 N3 Ni1 105.40(12) . . ? C8 N3 Ni1 110.48(12) . . ? C10 N3 H3N 109.2 . . ? C8 N3 H3N 109.2 . . ? Ni1 N3 H3N 109.2 . . ? C11 N4 C17 114.92(17) . . ? C11 N4 Ni1 104.96(12) . . ? C17 N4 Ni1 109.36(12) . . ? C11 N4 H4N 109.1 . . ? C17 N4 H4N 109.1 . . ? Ni1 N4 H4N 109.1 . . ? C19 N5 C16 113.11(18) . . ? C19 N5 Ni1 104.53(14) . . ? C16 N5 Ni1 110.42(13) . . ? C19 N5 H5N 109.5 . . ? C16 N5 H5N 109.5 . . ? Ni1 N5 H5N 109.5 . . ? C18 N6 C20 113.11(19) . . ? C18 N6 Ni1 103.93(12) . . ? C20 N6 Ni1 110.34(14) . . ? C18 N6 H6N 109.8 . . ? C20 N6 H6N 109.8 . . ? Ni1 N6 H6N 109.8 . . ? N1 C1 C6 111.10(17) . . ? N1 C1 C2 112.5(2) . . ? C6 C1 C2 109.9(2) . . ? N1 C1 H10 107.7 . . ? C6 C1 H10 107.7 . . ? C2 C1 H10 107.7 . . ? C3 C2 C1 111.3(2) . . ? C3 C2 H9A 109.4 . . ? C1 C2 H9A 109.4 . . ? C3 C2 H9B 109.4 . . ? C1 C2 H9B 109.4 . . ? H9A C2 H9B 108.0 . . ? C4 C3 C2 111.9(2) . . ? C4 C3 H8A 109.2 . . ? C2 C3 H8A 109.2 . . ? C4 C3 H8B 109.2 . . ? C2 C3 H8B 109.2 . . ? H8A C3 H8B 107.9 . . ? C3 C4 C5 111.4(2) . . ? C3 C4 H7A 109.3 . . ? C5 C4 H7A 109.3 . . ? C3 C4 H7B 109.3 . . ? C5 C4 H7B 109.3 . . ? H7A C4 H7B 108.0 . . ? C4 C5 C6 109.8(2) . . ? C4 C5 H6A 109.7 . . ? C6 C5 H6A 109.7 . . ? C4 C5 H6B 109.7 . . ? C6 C5 H6B 109.7 . . ? H6A C5 H6B 108.2 . . ? N2 C6 C1 109.14(16) . . ? N2 C6 C5 116.04(18) . . ? C1 C6 C5 110.55(18) . . ? N2 C6 H5 106.9 . . ? C1 C6 H5 106.9 . . ? C5 C6 H5 106.9 . . ? N1 C7 C8 111.07(18) . . ? N1 C7 H1A 109.4 . . ? C8 C7 H1A 109.4 . . ? N1 C7 H1B 109.4 . . ? C8 C7 H1B 109.4 . . ? H1A C7 H1B 108.0 . . ? N3 C8 C7 111.51(17) . . ? N3 C8 H2A 109.3 . . ? C7 C8 H2A 109.3 . . ? N3 C8 H2B 109.3 . . ? C7 C8 H2B 109.3 . . ? H2A C8 H2B 108.0 . . ? N2 C9 C10 110.55(18) . . ? N2 C9 H4A 109.5 . . ? C10 C9 H4A 109.5 . . ? N2 C9 H4B 109.5 . . ? C10 C9 H4B 109.5 . . ? H4A C9 H4B 108.1 . . ? N3 C10 C9 111.18(15) . . ? N3 C10 H3A 109.4 . . ? C9 C10 H3A 109.4 . . ? N3 C10 H3B 109.4 . . ? C9 C10 H3B 109.4 . . ? H3A C10 H3B 108.0 . . ? N4 C11 C16 110.21(16) . . ? N4 C11 C12 115.85(18) . . ? C16 C11 C12 109.86(18) . . ? N4 C11 H20 106.8 . . ? C16 C11 H20 106.8 . . ? C12 C11 H20 106.8 . . ? C13 C12 C11 110.16(19) . . ? C13 C12 H19A 109.6 . . ? C11 C12 H19A 109.6 . . ? C13 C12 H19B 109.6 . . ? C11 C12 H19B 109.6 . . ? H19A C12 H19B 108.1 . . ? C14 C13 C12 110.96(18) . . ? C14 C13 H18A 109.4 . . ? C12 C13 H18A 109.4 . . ? C14 C13 H18B 109.4 . . ? C12 C13 H18B 109.4 . . ? H18A C13 H18B 108.0 . . ? C13 C14 C15 111.6(2) . . ? C13 C14 H17A 109.3 . . ? C15 C14 H17A 109.3 . . ? C13 C14 H17B 109.3 . . ? C15 C14 H17B 109.3 . . ? H17A C14 H17B 108.0 . . ? C14 C15 C16 110.8(2) . . ? C14 C15 H16A 109.5 . . ? C16 C15 H16A 109.5 . . ? C14 C15 H16B 109.5 . . ? C16 C15 H16B 109.5 . . ? H16A C15 H16B 108.1 . . ? N5 C16 C11 110.57(17) . . ? N5 C16 C15 113.00(18) . . ? C11 C16 C15 110.91(18) . . ? N5 C16 H15 107.4 . . ? C11 C16 H15 107.4 . . ? C15 C16 H15 107.4 . . ? N4 C17 C18 111.61(17) . . ? N4 C17 H11A 109.3 . . ? C18 C17 H11A 109.3 . . ? N4 C17 H11B 109.3 . . ? C18 C17 H11B 109.3 . . ? H11A C17 H11B 108.0 . . ? N6 C18 C17 111.43(18) . . ? N6 C18 H12A 109.3 . . ? C17 C18 H12A 109.3 . . ? N6 C18 H12B 109.3 . . ? C17 C18 H12B 109.3 . . ? H12A C18 H12B 108.0 . . ? N5 C19 C20 110.6(2) . . ? N5 C19 H14A 109.5 . . ? C20 C19 H14A 109.5 . . ? N5 C19 H14B 109.5 . . ? C20 C19 H14B 109.5 . . ? H14A C19 H14B 108.1 . . ? N6 C20 C19 111.79(19) . . ? N6 C20 H13A 109.3 . . ? C19 C20 H13A 109.3 . . ? N6 C20 H13B 109.3 . . ? C19 C20 H13B 109.3 . . ? H13A C20 H13B 107.9 . . ? O3 N7 O2 119.52(19) . . ? O3 N7 O1 119.29(19) . . ? O2 N7 O1 121.2(2) . . ? O6 N8 O4 117.5(2) . . ? O6 N8 O5 119.8(2) . . ? O4 N8 O5 122.6(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Ni1 N1 C7 147.91(14) . . . . ? N3 Ni1 N1 C7 -31.15(13) . . . . ? N4 Ni1 N1 C7 -179(100) . . . . ? N2 Ni1 N1 C7 -113.91(14) . . . . ? N5 Ni1 N1 C7 65.12(14) . . . . ? N6 Ni1 N1 C1 -89.64(14) . . . . ? N3 Ni1 N1 C1 91.30(13) . . . . ? N4 Ni1 N1 C1 -56.5(17) . . . . ? N2 Ni1 N1 C1 8.54(13) . . . . ? N5 Ni1 N1 C1 -172.43(13) . . . . ? N6 Ni1 N2 C6 61.05(13) . . . . ? N3 Ni1 N2 C6 -116.35(13) . . . . ? N1 Ni1 N2 C6 -32.75(12) . . . . ? N4 Ni1 N2 C6 144.92(12) . . . . ? N5 Ni1 N2 C6 176(28) . . . . ? N6 Ni1 N2 C9 -175.37(13) . . . . ? N3 Ni1 N2 C9 7.23(13) . . . . ? N1 Ni1 N2 C9 90.83(14) . . . . ? N4 Ni1 N2 C9 -91.51(14) . . . . ? N5 Ni1 N2 C9 -60(2) . . . . ? N6 Ni1 N3 C10 -133.7(17) . . . . ? N1 Ni1 N3 C10 -113.07(13) . . . . ? N4 Ni1 N3 C10 65.55(13) . . . . ? N2 Ni1 N3 C10 -30.06(12) . . . . ? N5 Ni1 N3 C10 148.10(12) . . . . ? N6 Ni1 N3 C8 -10.9(18) . . . . ? N1 Ni1 N3 C8 9.70(14) . . . . ? N4 Ni1 N3 C8 -171.68(14) . . . . ? N2 Ni1 N3 C8 92.71(14) . . . . ? N5 Ni1 N3 C8 -89.13(14) . . . . ? N6 Ni1 N4 C11 -114.19(13) . . . . ? N3 Ni1 N4 C11 64.93(13) . . . . ? N1 Ni1 N4 C11 -147.5(17) . . . . ? N2 Ni1 N4 C11 147.78(12) . . . . ? N5 Ni1 N4 C11 -31.19(12) . . . . ? N6 Ni1 N4 C17 9.60(14) . . . . ? N3 Ni1 N4 C17 -171.28(14) . . . . ? N1 Ni1 N4 C17 -23.7(18) . . . . ? N2 Ni1 N4 C17 -88.42(14) . . . . ? N5 Ni1 N4 C17 92.61(14) . . . . ? N6 Ni1 N5 C19 -30.37(15) . . . . ? N3 Ni1 N5 C19 147.02(15) . . . . ? N1 Ni1 N5 C19 63.32(15) . . . . ? N4 Ni1 N5 C19 -114.36(15) . . . . ? N2 Ni1 N5 C19 -146(2) . . . . ? N6 Ni1 N5 C16 91.58(14) . . . . ? N3 Ni1 N5 C16 -91.03(14) . . . . ? N1 Ni1 N5 C16 -174.73(13) . . . . ? N4 Ni1 N5 C16 7.59(13) . . . . ? N2 Ni1 N5 C16 -24(2) . . . . ? N3 Ni1 N6 C18 167.6(17) . . . . ? N1 Ni1 N6 C18 147.07(14) . . . . ? N4 Ni1 N6 C18 -31.53(14) . . . . ? N2 Ni1 N6 C18 64.34(14) . . . . ? N5 Ni1 N6 C18 -113.86(14) . . . . ? N3 Ni1 N6 C20 -70.8(18) . . . . ? N1 Ni1 N6 C20 -91.38(15) . . . . ? N4 Ni1 N6 C20 90.03(15) . . . . ? N2 Ni1 N6 C20 -174.10(14) . . . . ? N5 Ni1 N6 C20 7.70(15) . . . . ? C7 N1 C1 C6 134.56(18) . . . . ? Ni1 N1 C1 C6 17.5(2) . . . . ? C7 N1 C1 C2 -101.8(2) . . . . ? Ni1 N1 C1 C2 141.17(17) . . . . ? N1 C1 C2 C3 179.4(2) . . . . ? C6 C1 C2 C3 -56.3(3) . . . . ? C1 C2 C3 C4 54.6(3) . . . . ? C2 C3 C4 C5 -54.6(3) . . . . ? C3 C4 C5 C6 56.3(3) . . . . ? C9 N2 C6 C1 -69.1(2) . . . . ? Ni1 N2 C6 C1 51.54(18) . . . . ? C9 N2 C6 C5 56.6(3) . . . . ? Ni1 N2 C6 C5 177.21(15) . . . . ? N1 C1 C6 N2 -47.3(2) . . . . ? C2 C1 C6 N2 -172.45(18) . . . . ? N1 C1 C6 C5 -176.13(17) . . . . ? C2 C1 C6 C5 58.8(2) . . . . ? C4 C5 C6 N2 176.39(19) . . . . ? C4 C5 C6 C1 -58.7(3) . . . . ? C1 N1 C7 C8 -72.3(2) . . . . ? Ni1 N1 C7 C8 47.8(2) . . . . ? C10 N3 C8 C7 131.83(19) . . . . ? Ni1 N3 C8 C7 13.8(2) . . . . ? N1 C7 C8 N3 -42.3(3) . . . . ? C6 N2 C9 C10 134.07(19) . . . . ? Ni1 N2 C9 C10 17.1(2) . . . . ? C8 N3 C10 C9 -71.9(2) . . . . ? Ni1 N3 C10 C9 49.1(2) . . . . ? N2 C9 C10 N3 -44.9(2) . . . . ? C17 N4 C11 C16 -69.4(2) . . . . ? Ni1 N4 C11 C16 50.76(18) . . . . ? C17 N4 C11 C12 56.1(2) . . . . ? Ni1 N4 C11 C12 176.25(14) . . . . ? N4 C11 C12 C13 175.52(18) . . . . ? C16 C11 C12 C13 -58.8(2) . . . . ? C11 C12 C13 C14 57.2(3) . . . . ? C12 C13 C14 C15 -55.3(3) . . . . ? C13 C14 C15 C16 54.5(3) . . . . ? C19 N5 C16 C11 134.63(19) . . . . ? Ni1 N5 C16 C11 17.9(2) . . . . ? C19 N5 C16 C15 -100.4(2) . . . . ? Ni1 N5 C16 C15 142.87(16) . . . . ? N4 C11 C16 N5 -46.5(2) . . . . ? C12 C11 C16 N5 -175.29(17) . . . . ? N4 C11 C16 C15 -172.63(18) . . . . ? C12 C11 C16 C15 58.5(2) . . . . ? C14 C15 C16 N5 178.77(19) . . . . ? C14 C15 C16 C11 -56.4(3) . . . . ? C11 N4 C17 C18 132.21(19) . . . . ? Ni1 N4 C17 C18 14.5(2) . . . . ? C20 N6 C18 C17 -70.6(2) . . . . ? Ni1 N6 C18 C17 49.1(2) . . . . ? N4 C17 C18 N6 -43.9(3) . . . . ? C16 N5 C19 C20 -71.6(2) . . . . ? Ni1 N5 C19 C20 48.5(2) . . . . ? C18 N6 C20 C19 132.8(2) . . . . ? Ni1 N6 C20 C19 16.8(2) . . . . ? N5 C19 C20 N6 -44.9(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N O3 0.91 2.28 3.167(3) 165.1 1_455 N3 H3N O1 0.91 2.24 3.111(3) 158.7 . N3 H3N O3 0.91 2.53 3.191(2) 129.4 . N4 H4N O6 0.91 2.25 3.092(3) 153.3 1_655 N4 H4N O5 0.91 2.41 3.226(3) 149.1 1_655 N4 H4N N8 0.91 2.69 3.590(3) 170.0 1_655 N6 H6N O6 0.91 2.29 3.064(2) 142.1 . N6 H6N O4 0.91 2.60 3.389(3) 144.9 . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.329 _refine_diff_density_min -0.208 _refine_diff_density_rms 0.037 #===END data_gal3 _database_code_CSD 195130 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H42 Cl3 Cr N6 O4.88' _chemical_formula_weight 602.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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 orthorhombic _symmetry_space_group_name_H-M 'P 21212' _symmetry_Int_Tables_number 18 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 18.936(4) _cell_length_b 29.495(5) _cell_length_c 11.545(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6448(2) _cell_formula_units_Z 8 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 978 _cell_measurement_theta_min 2.866 _cell_measurement_theta_max 22.125 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.169 _exptl_crystal_size_mid 0.134 _exptl_crystal_size_min 0.134 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 0.638 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.937 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _diffrn_crystal_treatment ; attached to a thin glass fibre ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 250 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 78427 _diffrn_reflns_av_R_equivalents 0.0605 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 28.30 _reflns_number_total 15616 _reflns_number_gt 10662 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker,1995)' _computing_cell_refinement 'SAINT (Bruker,1995)' _computing_data_reduction 'SAINT and XPREP (Bruker 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; teXsan for Windows (MSC, 1997) xtal 3.6 (Hall,du Boulay, D.J. & Olthof-Hazekamp, R. 1999) ORTEPII (Johnson,C.K., 1976). WinGX (Farrugia, 1999) ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.05P)^2^+5.0P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(3) _refine_ls_number_reflns 15650 _refine_ls_number_parameters 632 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1134 _refine_ls_R_factor_gt 0.0664 _refine_ls_wR_factor_ref 0.1943 _refine_ls_wR_factor_gt 0.1773 _refine_ls_goodness_of_fit_ref 1.568 _refine_ls_restrained_S_all 1.568 _refine_ls_shift/su_max 0.010 _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 Cr1 Cr 0.22030(5) 0.02234(3) 0.35894(7) 0.03247(19) Uani 1 1 d . . . N1 N 0.2136(3) -0.02049(16) 0.2151(4) 0.0409(11) Uani 1 1 d . . . H1N H 0.2217 -0.0496 0.2372 0.049 Uiso 1 1 calc R . . N2 N 0.2914(3) 0.05730(15) 0.2520(4) 0.0370(10) Uani 1 1 d . . . H2N H 0.3253 0.0704 0.2969 0.044 Uiso 1 1 calc R . . N3 N 0.1459(3) 0.05882(17) 0.2658(4) 0.0404(11) Uani 1 1 d . . . H3N H 0.1087 0.0649 0.3131 0.048 Uiso 1 1 calc R . . N4 N 0.2907(2) -0.01592(14) 0.4577(4) 0.0358(10) Uani 1 1 d . . . H4N H 0.3207 -0.0309 0.4095 0.043 Uiso 1 1 calc R . . N5 N 0.2243(2) 0.06549(14) 0.5040(4) 0.0326(9) Uani 1 1 d . . . H5N H 0.2347 0.0941 0.4800 0.039 Uiso 1 1 calc R . . N6 N 0.1453(3) -0.01114(16) 0.4580(4) 0.0430(12) Uani 1 1 d . . . H6N H 0.1057 -0.0154 0.4147 0.052 Uiso 1 1 calc R . . C1 C 0.2665(3) -0.00674(19) 0.1246(5) 0.0411(13) Uani 1 1 d . . . H1 H 0.2418 0.0124 0.0682 0.049 Uiso 1 1 calc R . . C2 C 0.2972(4) -0.0471(2) 0.0585(6) 0.0578(18) Uani 1 1 d . . . H2A H 0.2593 -0.0647 0.0242 0.069 Uiso 1 1 calc R . . H2B H 0.3230 -0.0665 0.1114 0.069 Uiso 1 1 calc R . . C3 C 0.3467(4) -0.0297(3) -0.0365(6) 0.065(2) Uani 1 1 d . . . H3A H 0.3682 -0.0553 -0.0760 0.078 Uiso 1 1 calc R . . H3B H 0.3198 -0.0126 -0.0930 0.078 Uiso 1 1 calc R . . C4 C 0.4035(4) -0.0001(3) 0.0142(6) 0.0650(19) Uani 1 1 d . . . H4A H 0.4323 0.0119 -0.0482 0.078 Uiso 1 1 calc R . . H4B H 0.4338 -0.0184 0.0632 0.078 Uiso 1 1 calc R . . C5 C 0.3743(3) 0.0390(3) 0.0849(6) 0.0558(17) Uani 1 1 d . . . H5A H 0.3492 0.0597 0.0343 0.067 Uiso 1 1 calc R . . H5B H 0.4130 0.0555 0.1203 0.067 Uiso 1 1 calc R . . C6 C 0.3244(3) 0.0219(2) 0.1792(5) 0.0405(13) Uani 1 1 d . . . H6 H 0.3518 0.0021 0.2304 0.049 Uiso 1 1 calc R . . C7 C 0.1403(3) -0.0160(2) 0.1714(5) 0.0493(16) Uani 1 1 d . . . H7A H 0.1082 -0.0318 0.2229 0.059 Uiso 1 1 calc R . . H7B H 0.1367 -0.0297 0.0953 0.059 Uiso 1 1 calc R . . C8 C 0.1199(3) 0.0335(2) 0.1644(5) 0.0497(17) Uani 1 1 d . . . H8A H 0.1395 0.0466 0.0943 0.060 Uiso 1 1 calc R . . H8B H 0.0689 0.0360 0.1603 0.060 Uiso 1 1 calc R . . C9 C 0.2537(3) 0.0937(2) 0.1850(5) 0.0444(14) Uani 1 1 d . . . H9A H 0.2487 0.0843 0.1049 0.053 Uiso 1 1 calc R . . H9B H 0.2815 0.1213 0.1864 0.053 Uiso 1 1 calc R . . C10 C 0.1819(4) 0.1027(2) 0.2359(6) 0.0488(15) Uani 1 1 d . . . H10A H 0.1867 0.1211 0.3050 0.059 Uiso 1 1 calc R . . H10B H 0.1534 0.1194 0.1805 0.059 Uiso 1 1 calc R . . C11 C 0.3320(3) 0.0184(2) 0.5273(5) 0.0376(12) Uani 1 1 d . . . H11 H 0.3589 0.0368 0.4721 0.045 Uiso 1 1 calc R . . C12 C 0.3853(3) -0.0015(2) 0.6140(5) 0.0473(14) Uani 1 1 d . . . H12A H 0.3609 -0.0199 0.6710 0.057 Uiso 1 1 calc R . . H12B H 0.4191 -0.0206 0.5737 0.057 Uiso 1 1 calc R . . C13 C 0.4234(4) 0.0376(2) 0.6736(6) 0.0584(18) Uani 1 1 d . . . H13A H 0.4523 0.0532 0.6169 0.070 Uiso 1 1 calc R . . H13B H 0.4547 0.0253 0.7323 0.070 Uiso 1 1 calc R . . C14 C 0.3736(4) 0.0718(2) 0.7303(6) 0.0543(17) Uani 1 1 d . . . H14A H 0.4008 0.0970 0.7603 0.065 Uiso 1 1 calc R . . H14B H 0.3495 0.0575 0.7948 0.065 Uiso 1 1 calc R . . C15 C 0.3187(3) 0.08943(19) 0.6424(6) 0.0463(14) Uani 1 1 d . . . H15A H 0.2851 0.1090 0.6815 0.056 Uiso 1 1 calc R . . H15B H 0.3422 0.1071 0.5829 0.056 Uiso 1 1 calc R . . C16 C 0.2802(3) 0.05005(18) 0.5874(4) 0.0343(11) Uani 1 1 d . . . H16 H 0.2569 0.0329 0.6493 0.041 Uiso 1 1 calc R . . C17 C 0.2514(3) -0.0500(2) 0.5311(5) 0.0431(14) Uani 1 1 d . . . H17A H 0.2498 -0.0396 0.6107 0.052 Uiso 1 1 calc R . . H17B H 0.2761 -0.0788 0.5296 0.052 Uiso 1 1 calc R . . C18 C 0.1771(3) -0.0563(2) 0.4860(6) 0.0467(15) Uani 1 1 d . . . H18A H 0.1780 -0.0750 0.4169 0.056 Uiso 1 1 calc R . . H18B H 0.1486 -0.0715 0.5439 0.056 Uiso 1 1 calc R . . C19 C 0.1528(3) 0.0651(2) 0.5539(5) 0.0395(13) Uani 1 1 d . . . H19A H 0.1211 0.0823 0.5047 0.047 Uiso 1 1 calc R . . H19B H 0.1535 0.0792 0.6297 0.047 Uiso 1 1 calc R . . C20 C 0.1267(3) 0.0163(2) 0.5644(5) 0.0456(15) Uani 1 1 d . . . H20A H 0.1477 0.0023 0.6322 0.055 Uiso 1 1 calc R . . H20B H 0.0758 0.0163 0.5748 0.055 Uiso 1 1 calc R . . Cr2 Cr 0.49511(4) 0.25671(3) 0.36995(7) 0.03067(18) Uani 1 1 d . . . N7 N 0.5603(2) 0.27169(14) 0.5109(4) 0.0326(10) Uani 1 1 d . . . H7N H 0.6050 0.2768 0.4847 0.039 Uiso 1 1 calc R . . N8 N 0.4707(2) 0.20022(15) 0.4699(4) 0.0365(10) Uani 1 1 d . . . H8N H 0.4609 0.1765 0.4221 0.044 Uiso 1 1 calc R . . N9 N 0.4201(2) 0.28795(16) 0.4730(4) 0.0368(11) Uani 1 1 d . . . H9N H 0.3974 0.3094 0.4302 0.044 Uiso 1 1 calc R . . N10 N 0.5721(2) 0.22966(15) 0.2617(4) 0.0364(10) Uani 1 1 d . . . H10N H 0.6062 0.2163 0.3055 0.044 Uiso 1 1 calc R . . N11 N 0.4296(2) 0.24052(16) 0.2320(4) 0.0362(10) Uani 1 1 d . . . H11N H 0.3930 0.2234 0.2581 0.043 Uiso 1 1 calc R . . N12 N 0.5138(3) 0.31460(16) 0.2733(4) 0.0423(12) Uani 1 1 d . . . H12N H 0.5070 0.3394 0.3187 0.051 Uiso 1 1 calc R . . C21 C 0.5617(3) 0.23271(19) 0.5959(5) 0.0375(12) Uani 1 1 d . . . H21 H 0.5280 0.2398 0.6578 0.045 Uiso 1 1 calc R . . C22 C 0.6340(3) 0.2254(2) 0.6527(5) 0.0430(13) Uani 1 1 d . . . H22A H 0.6690 0.2187 0.5937 0.052 Uiso 1 1 calc R . . H22B H 0.6484 0.2528 0.6928 0.052 Uiso 1 1 calc R . . C23 C 0.6295(4) 0.1863(2) 0.7378(6) 0.0570(18) Uani 1 1 d . . . H23A H 0.5978 0.1944 0.8004 0.068 Uiso 1 1 calc R . . H23B H 0.6758 0.1808 0.7709 0.068 Uiso 1 1 calc R . . C24 C 0.6031(4) 0.1431(2) 0.6799(6) 0.0590(19) Uani 1 1 d . . . H24A H 0.6371 0.1333 0.6224 0.071 Uiso 1 1 calc R . . H24B H 0.5988 0.1193 0.7375 0.071 Uiso 1 1 calc R . . C25 C 0.5320(3) 0.15058(19) 0.6221(6) 0.0482(14) Uani 1 1 d . . . H25A H 0.4966 0.1572 0.6804 0.058 Uiso 1 1 calc R . . H25B H 0.5179 0.1233 0.5815 0.058 Uiso 1 1 calc R . . C26 C 0.5367(3) 0.18980(18) 0.5370(5) 0.0357(12) Uani 1 1 d . . . H26 H 0.5730 0.1817 0.4801 0.043 Uiso 1 1 calc R . . C27 C 0.5325(3) 0.31369(18) 0.5609(5) 0.0390(13) Uani 1 1 d . . . H27A H 0.5436 0.3390 0.5104 0.047 Uiso 1 1 calc R . . H27B H 0.5546 0.3192 0.6354 0.047 Uiso 1 1 calc R . . C28 C 0.4530(3) 0.3104(2) 0.5763(5) 0.0416(14) Uani 1 1 d . . . H28A H 0.4424 0.2931 0.6455 0.050 Uiso 1 1 calc R . . H28B H 0.4334 0.3406 0.5858 0.050 Uiso 1 1 calc R . . C29 C 0.4074(3) 0.2095(2) 0.5447(5) 0.0419(14) Uani 1 1 d . . . H29A H 0.4224 0.2136 0.6244 0.050 Uiso 1 1 calc R . . H29B H 0.3756 0.1837 0.5420 0.050 Uiso 1 1 calc R . . C30 C 0.3686(3) 0.25175(19) 0.5039(5) 0.0413(13) Uani 1 1 d . . . H30A H 0.3399 0.2444 0.4369 0.050 Uiso 1 1 calc R . . H30B H 0.3376 0.2625 0.5648 0.050 Uiso 1 1 calc R . . C31 C 0.5346(3) 0.1939(2) 0.1916(5) 0.0396(13) Uani 1 1 d . . . H31 H 0.5193 0.1702 0.2454 0.048 Uiso 1 1 calc R . . C32 C 0.5812(4) 0.1711(2) 0.0981(6) 0.0515(16) Uani 1 1 d . . . H32A H 0.5972 0.1934 0.0422 0.062 Uiso 1 1 calc R . . H32B H 0.6222 0.1571 0.1336 0.062 Uiso 1 1 calc R . . C33 C 0.5359(5) 0.1352(2) 0.0387(6) 0.065(2) Uani 1 1 d . . . H33A H 0.5628 0.1213 -0.0235 0.078 Uiso 1 1 calc R . . H33B H 0.5242 0.1116 0.0941 0.078 Uiso 1 1 calc R . . C34 C 0.4680(4) 0.1550(3) -0.0107(6) 0.065(2) Uani 1 1 d . . . H34A H 0.4795 0.1767 -0.0710 0.077 Uiso 1 1 calc R . . H34B H 0.4402 0.1309 -0.0455 0.077 Uiso 1 1 calc R . . C35 C 0.4245(4) 0.1783(2) 0.0824(5) 0.0491(16) Uani 1 1 d . . . H35A H 0.3829 0.1921 0.0482 0.059 Uiso 1 1 calc R . . H35B H 0.4092 0.1563 0.1396 0.059 Uiso 1 1 calc R . . C36 C 0.4694(3) 0.21435(18) 0.1395(5) 0.0387(12) Uani 1 1 d . . . H36 H 0.4842 0.2359 0.0796 0.046 Uiso 1 1 calc R . . C37 C 0.6050(3) 0.2666(2) 0.1884(5) 0.0460(15) Uani 1 1 d . . . H37A H 0.6557 0.2621 0.1850 0.055 Uiso 1 1 calc R . . H37B H 0.5867 0.2647 0.1101 0.055 Uiso 1 1 calc R . . C38 C 0.5894(3) 0.3125(2) 0.2374(6) 0.0462(15) Uani 1 1 d . . . H38A H 0.6196 0.3182 0.3038 0.055 Uiso 1 1 calc R . . H38B H 0.5989 0.3356 0.1796 0.055 Uiso 1 1 calc R . . C39 C 0.4023(3) 0.2839(2) 0.1882(5) 0.0460(15) Uani 1 1 d . . . H39A H 0.3691 0.2967 0.2433 0.055 Uiso 1 1 calc R . . H39B H 0.3778 0.2792 0.1154 0.055 Uiso 1 1 calc R . . C40 C 0.4644(4) 0.3168(2) 0.1702(5) 0.0512(16) Uani 1 1 d . . . H40A H 0.4898 0.3088 0.1002 0.061 Uiso 1 1 calc R . . H40B H 0.4467 0.3475 0.1613 0.061 Uiso 1 1 calc R . . Cl1 Cl 0.00661(8) -0.06682(5) 0.37694(14) 0.0487(3) Uani 1 1 d . . . Cl2 Cl 0.03608(11) 0.21292(7) 0.11896(15) 0.0716(5) Uani 1 1 d . . . Cl3 Cl 0.17340(16) 0.05661(12) -0.1309(2) 0.1154(10) Uani 1 1 d . . . Cl4 Cl 0.21439(8) 0.17652(5) 0.50408(13) 0.0450(3) Uani 1 1 d . . . Cl5 Cl 0.44148(8) 0.09978(5) 0.35693(13) 0.0457(3) Uani 1 1 d . . . Cl6 Cl 0.70740(10) 0.17377(8) 0.37022(19) 0.0772(6) Uani 1 1 d . . . O1 O 0.2897(3) 0.20356(18) 0.2677(4) 0.0659(13) Uani 1 1 d . . . O2 O 0.4801(3) 0.40140(17) 0.3631(5) 0.0798(16) Uani 1 1 d . . . O3 O 0.3054(2) 0.34219(17) 0.3996(5) 0.0668(14) Uani 1 1 d . . . O4 O 0.3814(4) -0.0814(2) 0.3401(6) 0.100(2) Uani 1 1 d . . . O5 O 0.4594(5) 0.3796(2) 0.8533(7) 0.128(3) Uani 1 1 d . . . O6 O 0.2027(3) 0.2235(3) 0.0749(5) 0.101(2) Uani 1 1 d . . . O7 O 0.3072(4) 0.3803(2) -0.2130(7) 0.116(3) Uani 1 1 d . . . O8 O 0.2872(5) 0.2018(3) -0.2490(8) 0.061(2) Uiso 0.50 1 d P . . O9 O 0.2625(7) 0.3147(4) 0.0007(12) 0.092(4) Uiso 0.50 1 d P . . O10 O 0.2457(5) 0.1518(3) -0.0671(8) 0.056(2) Uiso 0.50 1 d P . . O11 O 0.2818(5) 0.3835(3) 0.1906(8) 0.060(2) Uiso 0.50 1 d P . . O12 O 0.3714(8) 0.2684(5) -0.1451(14) 0.039(3) Uiso 0.25 1 d P . . O13 O -0.0071(10) -0.0732(6) -0.0646(15) 0.050(4) Uiso 0.25 1 d P . . O14 O 0.1175(8) -0.0462(5) -0.1721(13) 0.043(4) Uiso 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0340(4) 0.0351(4) 0.0283(4) 0.0022(4) -0.0017(4) -0.0034(4) N1 0.048(3) 0.038(2) 0.036(2) 0.000(2) 0.004(2) -0.007(2) N2 0.040(3) 0.037(2) 0.034(2) -0.0015(19) -0.003(2) -0.004(2) N3 0.036(3) 0.049(3) 0.036(3) 0.002(2) -0.001(2) 0.003(2) N4 0.036(3) 0.032(2) 0.040(2) 0.0005(19) 0.001(2) 0.001(2) N5 0.035(2) 0.034(2) 0.029(2) 0.0018(18) -0.003(2) -0.0001(19) N6 0.039(3) 0.046(3) 0.043(3) 0.010(2) -0.006(2) -0.007(2) C1 0.044(3) 0.042(3) 0.037(3) -0.001(3) 0.001(3) -0.001(2) C2 0.072(5) 0.047(4) 0.054(4) -0.009(3) 0.007(3) 0.004(3) C3 0.078(5) 0.068(5) 0.049(4) -0.008(4) 0.015(4) 0.010(4) C4 0.055(4) 0.092(5) 0.047(4) 0.003(4) 0.015(3) 0.018(4) C5 0.037(4) 0.078(5) 0.052(4) -0.001(3) 0.005(3) -0.008(3) C6 0.038(3) 0.046(3) 0.038(3) -0.002(3) 0.002(2) 0.000(3) C7 0.043(3) 0.072(4) 0.033(3) -0.004(3) -0.003(3) -0.022(3) C8 0.039(3) 0.078(5) 0.032(3) 0.004(3) -0.006(2) -0.003(3) C9 0.055(4) 0.041(3) 0.037(3) 0.009(3) 0.001(3) -0.003(3) C10 0.059(4) 0.046(4) 0.042(3) 0.005(3) -0.005(3) 0.009(3) C11 0.040(3) 0.039(3) 0.034(3) 0.003(2) -0.003(2) -0.005(3) C12 0.045(3) 0.048(3) 0.049(3) 0.006(3) -0.005(3) 0.007(3) C13 0.047(4) 0.071(5) 0.056(4) 0.003(3) -0.015(3) 0.001(3) C14 0.056(4) 0.060(4) 0.047(4) -0.003(3) -0.021(3) -0.008(3) C15 0.052(4) 0.042(3) 0.045(3) -0.003(3) -0.010(3) 0.004(3) C16 0.036(3) 0.042(3) 0.025(2) 0.004(2) -0.006(2) -0.002(2) C17 0.047(3) 0.036(3) 0.046(3) 0.012(3) 0.001(3) -0.002(3) C18 0.044(3) 0.038(3) 0.057(4) 0.011(3) 0.000(3) -0.010(3) C19 0.039(3) 0.049(3) 0.031(3) 0.000(2) 0.001(2) 0.009(3) C20 0.038(3) 0.061(4) 0.038(3) 0.008(3) 0.005(3) 0.000(3) Cr2 0.0347(4) 0.0323(4) 0.0250(4) -0.0006(3) 0.0015(4) -0.0023(3) N7 0.038(2) 0.033(2) 0.026(2) -0.0015(18) 0.0035(19) -0.0037(19) N8 0.040(3) 0.035(2) 0.035(2) -0.0003(19) 0.001(2) -0.002(2) N9 0.040(3) 0.038(3) 0.033(2) -0.002(2) 0.003(2) 0.001(2) N10 0.033(2) 0.042(3) 0.034(2) -0.002(2) 0.002(2) -0.002(2) N11 0.037(3) 0.043(3) 0.029(2) -0.004(2) 0.0018(19) -0.002(2) N12 0.060(3) 0.037(2) 0.030(2) 0.0001(19) 0.001(2) -0.001(2) C21 0.041(3) 0.041(3) 0.031(3) -0.002(2) 0.001(2) -0.004(2) C22 0.042(3) 0.046(3) 0.040(3) 0.001(3) -0.003(3) 0.002(3) C23 0.065(4) 0.061(4) 0.046(4) 0.003(3) -0.010(3) 0.015(4) C24 0.076(5) 0.045(4) 0.056(4) 0.010(3) -0.009(4) 0.015(3) C25 0.066(4) 0.036(3) 0.043(3) 0.004(3) -0.001(3) 0.001(3) C26 0.038(3) 0.034(3) 0.035(3) 0.000(2) 0.002(2) -0.001(2) C27 0.047(3) 0.034(3) 0.036(3) -0.004(2) -0.005(3) -0.009(2) C28 0.052(4) 0.043(3) 0.030(3) -0.010(2) 0.004(3) 0.005(3) C29 0.042(3) 0.040(3) 0.044(3) 0.001(3) 0.009(3) -0.005(3) C30 0.035(3) 0.045(3) 0.044(3) -0.006(3) 0.008(3) -0.005(2) C31 0.049(4) 0.037(3) 0.033(3) -0.006(2) 0.009(3) 0.001(3) C32 0.058(4) 0.052(4) 0.045(4) -0.008(3) 0.015(3) 0.003(3) C33 0.091(6) 0.053(4) 0.052(4) -0.018(3) 0.016(4) -0.001(4) C34 0.084(5) 0.060(4) 0.050(4) -0.023(3) 0.003(4) -0.016(4) C35 0.057(4) 0.056(4) 0.035(3) -0.010(3) 0.003(3) -0.013(3) C36 0.047(3) 0.041(3) 0.028(3) -0.006(2) 0.003(3) -0.003(2) C37 0.045(4) 0.055(4) 0.038(3) 0.004(3) 0.011(3) -0.008(3) C38 0.051(4) 0.043(3) 0.045(3) 0.009(3) 0.005(3) -0.018(3) C39 0.048(4) 0.050(4) 0.039(3) -0.005(3) -0.007(3) 0.012(3) C40 0.074(5) 0.043(3) 0.037(3) 0.006(3) -0.004(3) 0.007(3) Cl1 0.0398(7) 0.0505(8) 0.0559(9) 0.0043(7) -0.0037(8) -0.0058(6) Cl2 0.0883(13) 0.0873(13) 0.0393(9) 0.0056(9) -0.0078(9) -0.0291(11) Cl3 0.118(2) 0.183(3) 0.0443(11) 0.0286(16) 0.0060(13) 0.0004(19) Cl4 0.0422(8) 0.0429(7) 0.0500(8) 0.0044(6) 0.0003(7) 0.0063(6) Cl5 0.0524(8) 0.0413(7) 0.0434(8) -0.0009(7) -0.0020(7) -0.0177(6) Cl6 0.0540(10) 0.1050(15) 0.0725(12) -0.0105(12) -0.0094(10) 0.0136(10) O1 0.044(3) 0.093(4) 0.060(3) -0.002(3) -0.001(2) -0.014(3) O2 0.102(4) 0.062(3) 0.076(3) -0.015(3) -0.008(3) 0.015(3) O3 0.055(3) 0.065(3) 0.080(4) 0.004(3) -0.001(3) 0.013(2) O4 0.111(5) 0.082(4) 0.107(5) -0.008(4) 0.018(4) 0.036(4) O5 0.150(7) 0.095(5) 0.139(7) 0.042(5) 0.042(6) 0.026(5) O6 0.092(5) 0.150(6) 0.061(4) -0.008(4) -0.014(3) 0.015(4) O7 0.125(6) 0.090(5) 0.135(6) -0.023(4) -0.030(5) -0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 N3 2.073(5) . ? Cr1 N6 2.074(5) . ? Cr1 N4 2.086(4) . ? Cr1 N1 2.091(5) . ? Cr1 N2 2.098(5) . ? Cr1 N5 2.105(4) . ? N1 C7 1.483(8) . ? N1 C1 1.502(7) . ? N1 H1N 0.9100 . ? N2 C6 1.478(7) . ? N2 C9 1.503(7) . ? N2 H2N 0.9100 . ? N3 C8 1.474(8) . ? N3 C10 1.504(8) . ? N3 H3N 0.9100 . ? N4 C11 1.511(7) . ? N4 C17 1.511(7) . ? N4 H4N 0.9100 . ? N5 C19 1.471(7) . ? N5 C16 1.501(7) . ? N5 H5N 0.9100 . ? N6 C18 1.496(8) . ? N6 C20 1.513(8) . ? N6 H6N 0.9100 . ? C1 C6 1.522(8) . ? C1 C2 1.528(8) . ? C1 H1 0.9800 . ? C2 C3 1.532(10) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.504(11) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.518(10) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.527(8) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6 0.9800 . ? C7 C8 1.512(10) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.505(9) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C16 1.521(8) . ? C11 C12 1.539(8) . ? C11 H11 0.9800 . ? C12 C13 1.524(9) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.527(10) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.544(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.511(8) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16 0.9800 . ? C17 C18 1.512(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.526(9) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? Cr2 N9 2.070(5) . ? Cr2 N12 2.070(5) . ? Cr2 N11 2.074(4) . ? Cr2 N8 2.079(4) . ? Cr2 N10 2.079(5) . ? Cr2 N7 2.090(4) . ? N7 C27 1.465(7) . ? N7 C21 1.512(7) . ? N7 H7N 0.9100 . ? N8 C26 1.503(7) . ? N8 C29 1.503(7) . ? N8 H8N 0.9100 . ? N9 C30 1.489(7) . ? N9 C28 1.501(7) . ? N9 H9N 0.9100 . ? N10 C31 1.506(7) . ? N10 C37 1.514(7) . ? N10 H10N 0.9100 . ? N11 C39 1.471(7) . ? N11 C36 1.518(7) . ? N11 H11N 0.9100 . ? N12 C38 1.492(8) . ? N12 C40 1.515(8) . ? N12 H12N 0.9100 . ? C21 C26 1.513(8) . ? C21 C22 1.534(8) . ? C21 H21 0.9800 . ? C22 C23 1.518(9) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.523(10) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.518(9) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.520(8) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26 0.9800 . ? C27 C28 1.517(8) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.521(8) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C36 1.499(8) . ? C31 C32 1.549(8) . ? C31 H31 0.9800 . ? C32 C33 1.526(10) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.524(11) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.518(9) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.512(8) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36 0.9800 . ? C37 C38 1.497(9) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.539(9) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cr1 N6 93.90(19) . . ? N3 Cr1 N4 176.92(19) . . ? N6 Cr1 N4 83.02(18) . . ? N3 Cr1 N1 82.0(2) . . ? N6 Cr1 N1 96.26(19) . . ? N4 Cr1 N1 98.40(19) . . ? N3 Cr1 N2 82.88(18) . . ? N6 Cr1 N2 176.66(19) . . ? N4 Cr1 N2 100.20(18) . . ? N1 Cr1 N2 82.44(18) . . ? N3 Cr1 N5 97.11(18) . . ? N6 Cr1 N5 82.76(19) . . ? N4 Cr1 N5 82.46(17) . . ? N1 Cr1 N5 178.6(2) . . ? N2 Cr1 N5 98.49(17) . . ? C7 N1 C1 111.3(4) . . ? C7 N1 Cr1 105.8(4) . . ? C1 N1 Cr1 110.4(3) . . ? C7 N1 H1N 109.8 . . ? C1 N1 H1N 109.8 . . ? Cr1 N1 H1N 109.8 . . ? C6 N2 C9 114.3(4) . . ? C6 N2 Cr1 105.0(3) . . ? C9 N2 Cr1 110.4(4) . . ? C6 N2 H2N 109.0 . . ? C9 N2 H2N 109.0 . . ? Cr1 N2 H2N 109.0 . . ? C8 N3 C10 113.9(5) . . ? C8 N3 Cr1 112.1(4) . . ? C10 N3 Cr1 105.0(4) . . ? C8 N3 H3N 108.5 . . ? C10 N3 H3N 108.5 . . ? Cr1 N3 H3N 108.5 . . ? C11 N4 C17 113.8(4) . . ? C11 N4 Cr1 105.0(3) . . ? C17 N4 Cr1 110.6(3) . . ? C11 N4 H4N 109.1 . . ? C17 N4 H4N 109.1 . . ? Cr1 N4 H4N 109.1 . . ? C19 N5 C16 113.3(4) . . ? C19 N5 Cr1 105.8(3) . . ? C16 N5 Cr1 110.7(3) . . ? C19 N5 H5N 109.0 . . ? C16 N5 H5N 109.0 . . ? Cr1 N5 H5N 109.0 . . ? C18 N6 C20 113.3(5) . . ? C18 N6 Cr1 105.5(4) . . ? C20 N6 Cr1 110.6(3) . . ? C18 N6 H6N 109.1 . . ? C20 N6 H6N 109.1 . . ? Cr1 N6 H6N 109.1 . . ? N1 C1 C6 110.0(4) . . ? N1 C1 C2 113.0(5) . . ? C6 C1 C2 111.4(5) . . ? N1 C1 H1 107.4 . . ? C6 C1 H1 107.4 . . ? C2 C1 H1 107.4 . . ? C1 C2 C3 109.3(5) . . ? C1 C2 H2A 109.8 . . ? C3 C2 H2A 109.8 . . ? C1 C2 H2B 109.8 . . ? C3 C2 H2B 109.8 . . ? H2A C2 H2B 108.3 . . ? C4 C3 C2 110.7(6) . . ? C4 C3 H3A 109.5 . . ? C2 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? C3 C4 C5 113.0(6) . . ? C3 C4 H4A 109.0 . . ? C5 C4 H4A 109.0 . . ? C3 C4 H4B 109.0 . . ? C5 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? C4 C5 C6 110.9(6) . . ? C4 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.0 . . ? N2 C6 C1 108.9(5) . . ? N2 C6 C5 115.7(5) . . ? C1 C6 C5 109.6(5) . . ? N2 C6 H6 107.5 . . ? C1 C6 H6 107.5 . . ? C5 C6 H6 107.5 . . ? N1 C7 C8 110.2(5) . . ? N1 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? N1 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? N3 C8 C7 111.1(5) . . ? N3 C8 H8A 109.4 . . ? C7 C8 H8A 109.4 . . ? N3 C8 H8B 109.4 . . ? C7 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? N2 C9 C10 110.8(5) . . ? N2 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? N2 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? N3 C10 C9 110.2(5) . . ? N3 C10 H10A 109.6 . . ? C9 C10 H10A 109.6 . . ? N3 C10 H10B 109.6 . . ? C9 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? N4 C11 C16 108.7(4) . . ? N4 C11 C12 115.4(5) . . ? C16 C11 C12 111.2(5) . . ? N4 C11 H11 107.1 . . ? C16 C11 H11 107.1 . . ? C12 C11 H11 107.1 . . ? C13 C12 C11 108.3(5) . . ? C13 C12 H12A 110.0 . . ? C11 C12 H12A 110.0 . . ? C13 C12 H12B 110.0 . . ? C11 C12 H12B 110.0 . . ? H12A C12 H12B 108.4 . . ? C12 C13 C14 113.7(6) . . ? C12 C13 H13A 108.8 . . ? C14 C13 H13A 108.8 . . ? C12 C13 H13B 108.8 . . ? C14 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? C13 C14 C15 110.9(5) . . ? C13 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C16 C15 C14 110.0(5) . . ? C16 C15 H15A 109.7 . . ? C14 C15 H15A 109.7 . . ? C16 C15 H15B 109.7 . . ? C14 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? N5 C16 C15 112.1(4) . . ? N5 C16 C11 110.3(4) . . ? C15 C16 C11 110.6(5) . . ? N5 C16 H16 107.9 . . ? C15 C16 H16 107.9 . . ? C11 C16 H16 107.9 . . ? N4 C17 C18 110.2(5) . . ? N4 C17 H17A 109.6 . . ? C18 C17 H17A 109.6 . . ? N4 C17 H17B 109.6 . . ? C18 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? N6 C18 C17 109.9(5) . . ? N6 C18 H18A 109.7 . . ? C17 C18 H18A 109.7 . . ? N6 C18 H18B 109.7 . . ? C17 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? N5 C19 C20 109.7(5) . . ? N5 C19 H19A 109.7 . . ? C20 C19 H19A 109.7 . . ? N5 C19 H19B 109.7 . . ? C20 C19 H19B 109.7 . . ? H19A C19 H19B 108.2 . . ? N6 C20 C19 111.3(5) . . ? N6 C20 H20A 109.4 . . ? C19 C20 H20A 109.4 . . ? N6 C20 H20B 109.4 . . ? C19 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? N9 Cr2 N12 93.43(19) . . ? N9 Cr2 N11 97.68(18) . . ? N12 Cr2 N11 83.00(19) . . ? N9 Cr2 N8 83.40(18) . . ? N12 Cr2 N8 176.6(2) . . ? N11 Cr2 N8 96.24(19) . . ? N9 Cr2 N10 176.08(19) . . ? N12 Cr2 N10 82.70(19) . . ? N11 Cr2 N10 82.48(18) . . ? N8 Cr2 N10 100.49(18) . . ? N9 Cr2 N7 82.19(18) . . ? N12 Cr2 N7 98.29(18) . . ? N11 Cr2 N7 178.71(18) . . ? N8 Cr2 N7 82.46(18) . . ? N10 Cr2 N7 97.75(18) . . ? C27 N7 C21 113.1(4) . . ? C27 N7 Cr2 105.8(3) . . ? C21 N7 Cr2 110.8(3) . . ? C27 N7 H7N 109.0 . . ? C21 N7 H7N 109.0 . . ? Cr2 N7 H7N 109.0 . . ? C26 N8 C29 113.9(4) . . ? C26 N8 Cr2 105.4(3) . . ? C29 N8 Cr2 110.5(3) . . ? C26 N8 H8N 109.0 . . ? C29 N8 H8N 109.0 . . ? Cr2 N8 H8N 109.0 . . ? C30 N9 C28 113.5(5) . . ? C30 N9 Cr2 105.5(3) . . ? C28 N9 Cr2 111.6(3) . . ? C30 N9 H9N 108.7 . . ? C28 N9 H9N 108.7 . . ? Cr2 N9 H9N 108.7 . . ? C31 N10 C37 113.4(4) . . ? C31 N10 Cr2 105.1(3) . . ? C37 N10 Cr2 110.4(3) . . ? C31 N10 H10N 109.3 . . ? C37 N10 H10N 109.3 . . ? Cr2 N10 H10N 109.3 . . ? C39 N11 C36 112.1(4) . . ? C39 N11 Cr2 105.9(3) . . ? C36 N11 Cr2 111.1(3) . . ? C39 N11 H11N 109.2 . . ? C36 N11 H11N 109.2 . . ? Cr2 N11 H11N 109.2 . . ? C38 N12 C40 112.1(5) . . ? C38 N12 Cr2 106.2(4) . . ? C40 N12 Cr2 110.7(4) . . ? C38 N12 H12N 109.2 . . ? C40 N12 H12N 109.2 . . ? Cr2 N12 H12N 109.2 . . ? N7 C21 C26 109.8(4) . . ? N7 C21 C22 113.5(5) . . ? C26 C21 C22 110.8(5) . . ? N7 C21 H21 107.5 . . ? C26 C21 H21 107.5 . . ? C22 C21 H21 107.5 . . ? C23 C22 C21 109.4(5) . . ? C23 C22 H22A 109.8 . . ? C21 C22 H22A 109.8 . . ? C23 C22 H22B 109.8 . . ? C21 C22 H22B 109.8 . . ? H22A C22 H22B 108.2 . . ? C22 C23 C24 111.7(5) . . ? C22 C23 H23A 109.3 . . ? C24 C23 H23A 109.3 . . ? C22 C23 H23B 109.3 . . ? C24 C23 H23B 109.3 . . ? H23A C23 H23B 107.9 . . ? C25 C24 C23 111.3(5) . . ? C25 C24 H24A 109.4 . . ? C23 C24 H24A 109.4 . . ? C25 C24 H24B 109.4 . . ? C23 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? C24 C25 C26 110.0(5) . . ? C24 C25 H25A 109.7 . . ? C26 C25 H25A 109.7 . . ? C24 C25 H25B 109.7 . . ? C26 C25 H25B 109.7 . . ? H25A C25 H25B 108.2 . . ? N8 C26 C21 108.7(4) . . ? N8 C26 C25 116.1(5) . . ? C21 C26 C25 111.4(5) . . ? N8 C26 H26 106.7 . . ? C21 C26 H26 106.7 . . ? C25 C26 H26 106.7 . . ? N7 C27 C28 110.5(5) . . ? N7 C27 H27A 109.6 . . ? C28 C27 H27A 109.6 . . ? N7 C27 H27B 109.6 . . ? C28 C27 H27B 109.6 . . ? H27A C27 H27B 108.1 . . ? N9 C28 C27 110.3(5) . . ? N9 C28 H28A 109.6 . . ? C27 C28 H28A 109.6 . . ? N9 C28 H28B 109.6 . . ? C27 C28 H28B 109.6 . . ? H28A C28 H28B 108.1 . . ? N8 C29 C30 110.8(5) . . ? N8 C29 H29A 109.5 . . ? C30 C29 H29A 109.5 . . ? N8 C29 H29B 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 108.1 . . ? N9 C30 C29 110.3(4) . . ? N9 C30 H30A 109.6 . . ? C29 C30 H30A 109.6 . . ? N9 C30 H30B 109.6 . . ? C29 C30 H30B 109.6 . . ? H30A C30 H30B 108.1 . . ? C36 C31 N10 108.8(4) . . ? C36 C31 C32 111.3(5) . . ? N10 C31 C32 114.3(5) . . ? C36 C31 H31 107.4 . . ? N10 C31 H31 107.4 . . ? C32 C31 H31 107.4 . . ? C33 C32 C31 107.2(5) . . ? C33 C32 H32A 110.3 . . ? C31 C32 H32A 110.3 . . ? C33 C32 H32B 110.3 . . ? C31 C32 H32B 110.3 . . ? H32A C32 H32B 108.5 . . ? C34 C33 C32 112.1(6) . . ? C34 C33 H33A 109.2 . . ? C32 C33 H33A 109.2 . . ? C34 C33 H33B 109.2 . . ? C32 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? C35 C34 C33 111.5(6) . . ? C35 C34 H34A 109.3 . . ? C33 C34 H34A 109.3 . . ? C35 C34 H34B 109.3 . . ? C33 C34 H34B 109.3 . . ? H34A C34 H34B 108.0 . . ? C36 C35 C34 108.8(5) . . ? C36 C35 H35A 109.9 . . ? C34 C35 H35A 109.9 . . ? C36 C35 H35B 109.9 . . ? C34 C35 H35B 109.9 . . ? H35A C35 H35B 108.3 . . ? C31 C36 C35 110.8(5) . . ? C31 C36 N11 109.3(4) . . ? C35 C36 N11 112.6(5) . . ? C31 C36 H36 108.0 . . ? C35 C36 H36 108.0 . . ? N11 C36 H36 108.0 . . ? C38 C37 N10 111.0(5) . . ? C38 C37 H37A 109.4 . . ? N10 C37 H37A 109.4 . . ? C38 C37 H37B 109.4 . . ? N10 C37 H37B 109.4 . . ? H37A C37 H37B 108.0 . . ? N12 C38 C37 109.4(5) . . ? N12 C38 H38A 109.8 . . ? C37 C38 H38A 109.8 . . ? N12 C38 H38B 109.8 . . ? C37 C38 H38B 109.8 . . ? H38A C38 H38B 108.2 . . ? N11 C39 C40 109.0(5) . . ? N11 C39 H39A 109.9 . . ? C40 C39 H39A 109.9 . . ? N11 C39 H39B 109.9 . . ? C40 C39 H39B 109.9 . . ? H39A C39 H39B 108.3 . . ? N12 C40 C39 109.8(5) . . ? N12 C40 H40A 109.7 . . ? C39 C40 H40A 109.7 . . ? N12 C40 H40B 109.7 . . ? C39 C40 H40B 109.7 . . ? H40A C40 H40B 108.2 . . ? 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 N3 Cr1 N1 C7 -30.5(4) . . . . ? N6 Cr1 N1 C7 62.6(4) . . . . ? N4 Cr1 N1 C7 146.4(4) . . . . ? N2 Cr1 N1 C7 -114.3(4) . . . . ? N5 Cr1 N1 C7 18(8) . . . . ? N3 Cr1 N1 C1 90.0(4) . . . . ? N6 Cr1 N1 C1 -176.9(4) . . . . ? N4 Cr1 N1 C1 -93.1(4) . . . . ? N2 Cr1 N1 C1 6.2(4) . . . . ? N5 Cr1 N1 C1 138(7) . . . . ? N3 Cr1 N2 C6 -114.0(4) . . . . ? N6 Cr1 N2 C6 -98(3) . . . . ? N4 Cr1 N2 C6 66.0(4) . . . . ? N1 Cr1 N2 C6 -31.2(3) . . . . ? N5 Cr1 N2 C6 149.8(3) . . . . ? N3 Cr1 N2 C9 9.6(4) . . . . ? N6 Cr1 N2 C9 25(3) . . . . ? N4 Cr1 N2 C9 -170.4(4) . . . . ? N1 Cr1 N2 C9 92.4(4) . . . . ? N5 Cr1 N2 C9 -86.5(4) . . . . ? N6 Cr1 N3 C8 -86.4(4) . . . . ? N4 Cr1 N3 C8 -88(4) . . . . ? N1 Cr1 N3 C8 9.4(4) . . . . ? N2 Cr1 N3 C8 92.7(4) . . . . ? N5 Cr1 N3 C8 -169.6(4) . . . . ? N6 Cr1 N3 C10 149.4(4) . . . . ? N4 Cr1 N3 C10 148(4) . . . . ? N1 Cr1 N3 C10 -114.8(4) . . . . ? N2 Cr1 N3 C10 -31.5(4) . . . . ? N5 Cr1 N3 C10 66.2(4) . . . . ? N3 Cr1 N4 C11 -114(4) . . . . ? N6 Cr1 N4 C11 -115.4(4) . . . . ? N1 Cr1 N4 C11 149.2(3) . . . . ? N2 Cr1 N4 C11 65.5(3) . . . . ? N5 Cr1 N4 C11 -31.9(3) . . . . ? N3 Cr1 N4 C17 9(4) . . . . ? N6 Cr1 N4 C17 7.7(4) . . . . ? N1 Cr1 N4 C17 -87.7(4) . . . . ? N2 Cr1 N4 C17 -171.4(4) . . . . ? N5 Cr1 N4 C17 91.2(4) . . . . ? N3 Cr1 N5 C19 61.7(3) . . . . ? N6 Cr1 N5 C19 -31.3(3) . . . . ? N4 Cr1 N5 C19 -115.2(3) . . . . ? N1 Cr1 N5 C19 13(8) . . . . ? N2 Cr1 N5 C19 145.6(3) . . . . ? N3 Cr1 N5 C16 -175.2(3) . . . . ? N6 Cr1 N5 C16 91.8(3) . . . . ? N4 Cr1 N5 C16 7.9(3) . . . . ? N1 Cr1 N5 C16 137(7) . . . . ? N2 Cr1 N5 C16 -91.4(3) . . . . ? N3 Cr1 N6 C18 149.6(4) . . . . ? N4 Cr1 N6 C18 -30.5(4) . . . . ? N1 Cr1 N6 C18 67.2(4) . . . . ? N2 Cr1 N6 C18 134(3) . . . . ? N5 Cr1 N6 C18 -113.8(4) . . . . ? N3 Cr1 N6 C20 -87.6(4) . . . . ? N4 Cr1 N6 C20 92.3(4) . . . . ? N1 Cr1 N6 C20 -169.9(4) . . . . ? N2 Cr1 N6 C20 -103(3) . . . . ? N5 Cr1 N6 C20 9.1(4) . . . . ? C7 N1 C1 C6 137.1(5) . . . . ? Cr1 N1 C1 C6 19.9(5) . . . . ? C7 N1 C1 C2 -97.7(6) . . . . ? Cr1 N1 C1 C2 145.1(4) . . . . ? N1 C1 C2 C3 176.4(5) . . . . ? C6 C1 C2 C3 -59.1(7) . . . . ? C1 C2 C3 C4 56.2(8) . . . . ? C2 C3 C4 C5 -55.1(9) . . . . ? C3 C4 C5 C6 54.7(8) . . . . ? C9 N2 C6 C1 -70.2(6) . . . . ? Cr1 N2 C6 C1 50.9(5) . . . . ? C9 N2 C6 C5 53.7(7) . . . . ? Cr1 N2 C6 C5 174.8(4) . . . . ? N1 C1 C6 N2 -47.8(6) . . . . ? C2 C1 C6 N2 -173.9(5) . . . . ? N1 C1 C6 C5 -175.2(5) . . . . ? C2 C1 C6 C5 58.7(7) . . . . ? C4 C5 C6 N2 -178.7(5) . . . . ? C4 C5 C6 C1 -55.2(7) . . . . ? C1 N1 C7 C8 -73.2(6) . . . . ? Cr1 N1 C7 C8 46.8(5) . . . . ? C10 N3 C8 C7 133.0(5) . . . . ? Cr1 N3 C8 C7 14.0(6) . . . . ? N1 C7 C8 N3 -40.9(7) . . . . ? C6 N2 C9 C10 133.1(5) . . . . ? Cr1 N2 C9 C10 15.1(6) . . . . ? C8 N3 C10 C9 -73.9(6) . . . . ? Cr1 N3 C10 C9 49.1(5) . . . . ? N2 C9 C10 N3 -43.1(7) . . . . ? C17 N4 C11 C16 -70.1(6) . . . . ? Cr1 N4 C11 C16 50.9(4) . . . . ? C17 N4 C11 C12 55.5(6) . . . . ? Cr1 N4 C11 C12 176.5(4) . . . . ? N4 C11 C12 C13 178.4(5) . . . . ? C16 C11 C12 C13 -57.3(7) . . . . ? C11 C12 C13 C14 54.5(7) . . . . ? C12 C13 C14 C15 -54.0(8) . . . . ? C13 C14 C15 C16 54.3(7) . . . . ? C19 N5 C16 C15 -99.3(6) . . . . ? Cr1 N5 C16 C15 142.0(4) . . . . ? C19 N5 C16 C11 137.0(5) . . . . ? Cr1 N5 C16 C11 18.3(5) . . . . ? C14 C15 C16 N5 178.1(5) . . . . ? C14 C15 C16 C11 -58.3(7) . . . . ? N4 C11 C16 N5 -46.3(6) . . . . ? C12 C11 C16 N5 -174.4(5) . . . . ? N4 C11 C16 C15 -170.9(4) . . . . ? C12 C11 C16 C15 61.0(6) . . . . ? C11 N4 C17 C18 135.0(5) . . . . ? Cr1 N4 C17 C18 17.1(6) . . . . ? C20 N6 C18 C17 -72.3(6) . . . . ? Cr1 N6 C18 C17 48.9(6) . . . . ? N4 C17 C18 N6 -44.2(7) . . . . ? C16 N5 C19 C20 -73.8(6) . . . . ? Cr1 N5 C19 C20 47.6(5) . . . . ? C18 N6 C20 C19 132.8(5) . . . . ? Cr1 N6 C20 C19 14.6(6) . . . . ? N5 C19 C20 N6 -42.1(6) . . . . ? N9 Cr2 N7 C27 -31.4(3) . . . . ? N12 Cr2 N7 C27 60.9(4) . . . . ? N11 Cr2 N7 C27 -116(8) . . . . ? N8 Cr2 N7 C27 -115.8(3) . . . . ? N10 Cr2 N7 C27 144.6(3) . . . . ? N9 Cr2 N7 C21 91.5(4) . . . . ? N12 Cr2 N7 C21 -176.1(3) . . . . ? N11 Cr2 N7 C21 7(9) . . . . ? N8 Cr2 N7 C21 7.2(3) . . . . ? N10 Cr2 N7 C21 -92.4(4) . . . . ? N9 Cr2 N8 C26 -114.4(3) . . . . ? N12 Cr2 N8 C26 -135(3) . . . . ? N11 Cr2 N8 C26 148.5(3) . . . . ? N10 Cr2 N8 C26 65.1(3) . . . . ? N7 Cr2 N8 C26 -31.5(3) . . . . ? N9 Cr2 N8 C29 9.0(4) . . . . ? N12 Cr2 N8 C29 -11(3) . . . . ? N11 Cr2 N8 C29 -88.0(4) . . . . ? N10 Cr2 N8 C29 -171.5(4) . . . . ? N7 Cr2 N8 C29 92.0(4) . . . . ? N12 Cr2 N9 C30 148.1(4) . . . . ? N11 Cr2 N9 C30 64.7(4) . . . . ? N8 Cr2 N9 C30 -30.7(4) . . . . ? N10 Cr2 N9 C30 157(3) . . . . ? N7 Cr2 N9 C30 -114.0(4) . . . . ? N12 Cr2 N9 C28 -88.2(4) . . . . ? N11 Cr2 N9 C28 -171.6(4) . . . . ? N8 Cr2 N9 C28 93.0(4) . . . . ? N10 Cr2 N9 C28 -80(3) . . . . ? N7 Cr2 N9 C28 9.7(4) . . . . ? N9 Cr2 N10 C31 -123(3) . . . . ? N12 Cr2 N10 C31 -114.8(4) . . . . ? N11 Cr2 N10 C31 -30.9(3) . . . . ? N8 Cr2 N10 C31 64.1(4) . . . . ? N7 Cr2 N10 C31 147.8(3) . . . . ? N9 Cr2 N10 C37 -1(3) . . . . ? N12 Cr2 N10 C37 7.9(4) . . . . ? N11 Cr2 N10 C37 91.7(4) . . . . ? N8 Cr2 N10 C37 -173.3(4) . . . . ? N7 Cr2 N10 C37 -89.5(4) . . . . ? N9 Cr2 N11 C39 60.6(4) . . . . ? N12 Cr2 N11 C39 -32.0(4) . . . . ? N8 Cr2 N11 C39 144.7(4) . . . . ? N10 Cr2 N11 C39 -115.5(4) . . . . ? N7 Cr2 N11 C39 145(8) . . . . ? N9 Cr2 N11 C36 -177.5(3) . . . . ? N12 Cr2 N11 C36 90.0(4) . . . . ? N8 Cr2 N11 C36 -93.4(4) . . . . ? N10 Cr2 N11 C36 6.4(3) . . . . ? N7 Cr2 N11 C36 -94(8) . . . . ? N9 Cr2 N12 C38 148.9(4) . . . . ? N11 Cr2 N12 C38 -113.8(4) . . . . ? N8 Cr2 N12 C38 169(3) . . . . ? N10 Cr2 N12 C38 -30.6(4) . . . . ? N7 Cr2 N12 C38 66.3(4) . . . . ? N9 Cr2 N12 C40 -89.2(4) . . . . ? N11 Cr2 N12 C40 8.1(4) . . . . ? N8 Cr2 N12 C40 -69(3) . . . . ? N10 Cr2 N12 C40 91.4(4) . . . . ? N7 Cr2 N12 C40 -171.8(4) . . . . ? C27 N7 C21 C26 137.6(5) . . . . ? Cr2 N7 C21 C26 19.0(5) . . . . ? C27 N7 C21 C22 -97.9(5) . . . . ? Cr2 N7 C21 C22 143.5(4) . . . . ? N7 C21 C22 C23 178.9(5) . . . . ? C26 C21 C22 C23 -57.0(6) . . . . ? C21 C22 C23 C24 56.3(7) . . . . ? C22 C23 C24 C25 -56.4(8) . . . . ? C23 C24 C25 C26 55.4(7) . . . . ? C29 N8 C26 C21 -70.4(6) . . . . ? Cr2 N8 C26 C21 50.9(5) . . . . ? C29 N8 C26 C25 56.1(6) . . . . ? Cr2 N8 C26 C25 177.4(4) . . . . ? N7 C21 C26 N8 -46.5(6) . . . . ? C22 C21 C26 N8 -172.6(4) . . . . ? N7 C21 C26 C25 -175.7(5) . . . . ? C22 C21 C26 C25 58.1(6) . . . . ? C24 C25 C26 N8 178.0(5) . . . . ? C24 C25 C26 C21 -56.8(7) . . . . ? C21 N7 C27 C28 -73.5(6) . . . . ? Cr2 N7 C27 C28 48.0(5) . . . . ? C30 N9 C28 C27 132.7(5) . . . . ? Cr2 N9 C28 C27 13.6(6) . . . . ? N7 C27 C28 N9 -41.4(7) . . . . ? C26 N8 C29 C30 133.2(5) . . . . ? Cr2 N8 C29 C30 14.8(6) . . . . ? C28 N9 C30 C29 -75.0(6) . . . . ? Cr2 N9 C30 C29 47.5(5) . . . . ? N8 C29 C30 N9 -41.9(7) . . . . ? C37 N10 C31 C36 -69.6(6) . . . . ? Cr2 N10 C31 C36 51.1(5) . . . . ? C37 N10 C31 C32 55.5(7) . . . . ? Cr2 N10 C31 C32 176.2(4) . . . . ? C36 C31 C32 C33 -58.0(7) . . . . ? N10 C31 C32 C33 178.3(5) . . . . ? C31 C32 C33 C34 55.7(7) . . . . ? C32 C33 C34 C35 -57.2(8) . . . . ? C33 C34 C35 C36 56.5(8) . . . . ? N10 C31 C36 C35 -172.0(5) . . . . ? C32 C31 C36 C35 61.2(6) . . . . ? N10 C31 C36 N11 -47.3(6) . . . . ? C32 C31 C36 N11 -174.1(5) . . . . ? C34 C35 C36 C31 -58.8(7) . . . . ? C34 C35 C36 N11 178.4(5) . . . . ? C39 N11 C36 C31 138.3(5) . . . . ? Cr2 N11 C36 C31 20.1(5) . . . . ? C39 N11 C36 C35 -98.0(6) . . . . ? Cr2 N11 C36 C35 143.7(4) . . . . ? C31 N10 C37 C38 134.5(5) . . . . ? Cr2 N10 C37 C38 16.8(6) . . . . ? C40 N12 C38 C37 -72.6(6) . . . . ? Cr2 N12 C38 C37 48.4(5) . . . . ? N10 C37 C38 N12 -43.4(7) . . . . ? C36 N11 C39 C40 -71.6(6) . . . . ? Cr2 N11 C39 C40 49.7(5) . . . . ? C38 N12 C40 C39 135.1(5) . . . . ? Cr2 N12 C40 C39 16.7(6) . . . . ? N11 C39 C40 N12 -44.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.261 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.130