# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name G.P.A.Yap _publ_contact_author_email gpyap@udel.edu loop_ _publ_author_name 'Jingmei Shen' G.P.A.Yap 'Jan-Philipp Werner' 'Klaus H.Theopold' data_klat782 _database_code_depnum_ccdc_archive 'CCDC 839343' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H78 Cr2 N4' _chemical_formula_weight 911.22 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.627(3) _cell_length_b 19.352(4) _cell_length_c 20.122(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.097(4) _cell_angle_gamma 90.00 _cell_volume 5224.3(17) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 985 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 20.24 _exptl_crystal_description block _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.159 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 0.454 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9067 _exptl_absorpt_correction_T_max 0.9689 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _diffrn_ambient_temperature 200(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 AXS APEX diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 836.6 _diffrn_reflns_number 68941 _diffrn_reflns_av_R_equivalents 0.0997 _diffrn_reflns_av_sigmaI/netI 0.0805 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 28.38 _reflns_number_total 13006 _reflns_number_gt 7632 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2001)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _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^)+(0.0687P)^2^+1.2299P] 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 13006 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1250 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1659 _refine_ls_wR_factor_gt 0.1368 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 Cr1 Cr 0.10089(4) 0.81581(2) 0.22160(2) 0.03206(13) Uani 1 1 d . . . Cr2 Cr -0.03335(3) 0.82674(2) 0.23774(3) 0.03188(13) Uani 1 1 d . . . N1 N 0.13001(17) 0.71950(12) 0.23977(12) 0.0273(5) Uani 1 1 d . . . N2 N -0.06287(17) 0.74391(13) 0.28103(12) 0.0309(5) Uani 1 1 d . . . N3 N 0.16960(17) 0.89571(12) 0.26472(12) 0.0293(5) Uani 1 1 d . . . N4 N -0.04552(17) 0.92402(12) 0.24759(12) 0.0291(5) Uani 1 1 d . . . C1 C 0.0713(2) 0.66974(15) 0.26079(16) 0.0354(7) Uani 1 1 d . . . H1 H 0.0938 0.6233 0.2605 0.042 Uiso 1 1 calc R . . C2 C -0.0161(2) 0.68103(16) 0.28191(16) 0.0375(7) Uani 1 1 d . . . H2 H -0.0476 0.6425 0.2986 0.045 Uiso 1 1 calc R . . C3 C -0.1242(2) 0.73307(19) 0.38899(17) 0.0435(8) Uani 1 1 d . . . C4 C -0.2049(3) 0.7271(2) 0.42276(18) 0.0529(10) Uani 1 1 d . . . H4 H -0.1926 0.7200 0.4702 0.064 Uiso 1 1 calc R . . C5 C -0.3012(3) 0.7312(2) 0.38953(19) 0.0526(10) Uani 1 1 d . . . H5 H -0.3547 0.7267 0.4138 0.063 Uiso 1 1 calc R . . C6 C -0.3206(2) 0.74186(18) 0.32100(18) 0.0471(9) Uani 1 1 d . . . H6 H -0.3877 0.7457 0.2984 0.057 Uiso 1 1 calc R . . C7 C -0.2433(2) 0.74711(16) 0.28384(16) 0.0367(7) Uani 1 1 d . . . C8 C -0.1453(2) 0.74212(16) 0.31844(16) 0.0353(7) Uani 1 1 d . . . C9 C -0.0190(3) 0.7286(2) 0.42928(18) 0.0623(12) Uani 1 1 d . . . H9 H 0.0283 0.7401 0.3981 0.075 Uiso 1 1 calc R . . C10 C 0.0054(4) 0.6557(3) 0.4560(2) 0.0969(18) Uani 1 1 d . . . H10A H -0.0410 0.6426 0.4860 0.145 Uiso 1 1 calc R . . H10B H 0.0738 0.6545 0.4812 0.145 Uiso 1 1 calc R . . H10C H -0.0010 0.6233 0.4181 0.145 Uiso 1 1 calc R . . C11 C -0.0028(3) 0.7814(3) 0.4871(2) 0.0867(16) Uani 1 1 d . . . H11A H -0.0119 0.8282 0.4684 0.130 Uiso 1 1 calc R . . H11B H 0.0650 0.7766 0.5127 0.130 Uiso 1 1 calc R . . H11C H -0.0511 0.7731 0.5170 0.130 Uiso 1 1 calc R . . C12 C -0.2679(2) 0.75187(19) 0.20775(17) 0.0449(8) Uani 1 1 d . . . H12 H -0.2068 0.7689 0.1917 0.054 Uiso 1 1 calc R . . C13 C -0.2910(4) 0.6801(2) 0.1776(2) 0.0740(13) Uani 1 1 d . . . H13A H -0.2331 0.6500 0.1910 0.111 Uiso 1 1 calc R . . H13B H -0.3060 0.6835 0.1283 0.111 Uiso 1 1 calc R . . H13C H -0.3486 0.6608 0.1942 0.111 Uiso 1 1 calc R . . C14 C -0.3519(3) 0.8021(2) 0.1817(2) 0.0636(11) Uani 1 1 d . . . H14A H -0.4146 0.7847 0.1929 0.095 Uiso 1 1 calc R . . H14B H -0.3585 0.8066 0.1326 0.095 Uiso 1 1 calc R . . H14C H -0.3368 0.8474 0.2028 0.095 Uiso 1 1 calc R . . C15 C 0.3085(2) 0.68934(15) 0.25958(16) 0.0337(7) Uani 1 1 d . . . C16 C 0.3913(2) 0.66623(16) 0.23347(19) 0.0433(8) Uani 1 1 d . . . H16 H 0.4544 0.6642 0.2623 0.052 Uiso 1 1 calc R . . C17 C 0.3837(3) 0.64658(18) 0.1675(2) 0.0494(9) Uani 1 1 d . . . H17 H 0.4415 0.6323 0.1509 0.059 Uiso 1 1 calc R . . C18 C 0.2925(3) 0.64730(18) 0.12501(18) 0.0452(8) Uani 1 1 d . . . H18 H 0.2879 0.6328 0.0795 0.054 Uiso 1 1 calc R . . C19 C 0.2072(2) 0.66914(15) 0.14834(16) 0.0359(7) Uani 1 1 d . . . C20 C 0.2170(2) 0.69266(14) 0.21548(15) 0.0307(6) Uani 1 1 d . . . C21 C 0.3175(2) 0.70690(17) 0.33390(16) 0.0388(7) Uani 1 1 d . . . H21 H 0.2719 0.7466 0.3379 0.047 Uiso 1 1 calc R . . C22 C 0.2855(3) 0.6465(2) 0.37429(19) 0.0625(11) Uani 1 1 d . . . H22A H 0.2157 0.6349 0.3569 0.094 Uiso 1 1 calc R . . H22B H 0.2928 0.6595 0.4220 0.094 Uiso 1 1 calc R . . H22C H 0.3276 0.6062 0.3699 0.094 Uiso 1 1 calc R . . C23 C 0.4228(2) 0.72826(19) 0.36684(19) 0.0498(9) Uani 1 1 d . . . H23A H 0.4215 0.7467 0.4120 0.075 Uiso 1 1 calc R . . H23B H 0.4474 0.7638 0.3393 0.075 Uiso 1 1 calc R . . H23C H 0.4669 0.6879 0.3703 0.075 Uiso 1 1 calc R . . C24 C 0.1063(2) 0.66390(17) 0.10222(16) 0.0414(8) Uani 1 1 d . . . H24 H 0.0586 0.6940 0.1215 0.050 Uiso 1 1 calc R . . C25 C 0.1089(3) 0.6889(2) 0.03079(19) 0.0671(12) Uani 1 1 d . . . H25A H 0.1387 0.7351 0.0326 0.101 Uiso 1 1 calc R . . H25B H 0.0408 0.6908 0.0051 0.101 Uiso 1 1 calc R . . H25C H 0.1488 0.6569 0.0087 0.101 Uiso 1 1 calc R . . C26 C 0.0665(3) 0.5899(2) 0.1002(2) 0.0671(12) Uani 1 1 d . . . H26A H 0.1109 0.5594 0.0804 0.101 Uiso 1 1 calc R . . H26B H -0.0005 0.5884 0.0728 0.101 Uiso 1 1 calc R . . H26C H 0.0634 0.5746 0.1462 0.101 Uiso 1 1 calc R . . C27 C 0.1270(2) 0.95973(15) 0.26707(15) 0.0342(7) Uani 1 1 d . . . H27 H 0.1709 0.9981 0.2762 0.041 Uiso 1 1 calc R . . C28 C 0.0279(2) 0.97309(16) 0.25752(15) 0.0336(7) Uani 1 1 d . . . H28 H 0.0079 1.0201 0.2577 0.040 Uiso 1 1 calc R . . C29 C -0.1928(2) 0.95513(16) 0.29700(18) 0.0394(8) Uani 1 1 d . . . C30 C -0.2896(3) 0.98243(19) 0.2881(2) 0.0591(11) Uani 1 1 d . . . H30 H -0.3228 0.9847 0.3258 0.071 Uiso 1 1 calc R . . C31 C -0.3373(3) 1.0057(2) 0.2270(3) 0.0696(13) Uani 1 1 d . . . H31 H -0.4029 1.0239 0.2224 0.084 Uiso 1 1 calc R . . C32 C -0.2901(3) 1.00289(19) 0.1727(2) 0.0638(12) Uani 1 1 d . . . H32 H -0.3241 1.0193 0.1303 0.077 Uiso 1 1 calc R . . C33 C -0.1933(3) 0.97656(17) 0.17691(19) 0.0453(8) Uani 1 1 d . . . C34 C -0.1462(2) 0.95174(15) 0.24058(16) 0.0337(7) Uani 1 1 d . . . C35 C -0.1397(3) 0.9345(2) 0.36657(18) 0.0492(9) Uani 1 1 d . . . H35 H -0.0930 0.8959 0.3610 0.059 Uiso 1 1 calc R . . C36 C -0.2107(3) 0.9087(2) 0.4129(2) 0.0654(12) Uani 1 1 d . . . H36A H -0.2524 0.9470 0.4234 0.098 Uiso 1 1 calc R . . H36B H -0.1717 0.8906 0.4549 0.098 Uiso 1 1 calc R . . H36C H -0.2533 0.8719 0.3901 0.098 Uiso 1 1 calc R . . C37 C -0.0775(3) 0.9947(3) 0.4004(2) 0.0755(14) Uani 1 1 d . . . H37A H -0.0281 1.0082 0.3728 0.113 Uiso 1 1 calc R . . H37B H -0.0433 0.9805 0.4453 0.113 Uiso 1 1 calc R . . H37C H -0.1213 1.0340 0.4048 0.113 Uiso 1 1 calc R . . C38 C -0.1424(3) 0.9780(2) 0.11639(18) 0.0569(10) Uani 1 1 d . . . H38 H -0.0836 0.9464 0.1260 0.068 Uiso 1 1 calc R . . C39 C -0.1033(4) 1.0503(2) 0.1050(2) 0.0881(15) Uani 1 1 d . . . H39A H -0.1596 1.0823 0.0939 0.132 Uiso 1 1 calc R . . H39B H -0.0660 1.0489 0.0676 0.132 Uiso 1 1 calc R . . H39C H -0.0594 1.0659 0.1461 0.132 Uiso 1 1 calc R . . C40 C -0.2088(4) 0.9524(3) 0.0514(2) 0.1012(19) Uani 1 1 d . . . H40A H -0.2349 0.9065 0.0591 0.152 Uiso 1 1 calc R . . H40B H -0.1695 0.9499 0.0151 0.152 Uiso 1 1 calc R . . H40C H -0.2644 0.9846 0.0385 0.152 Uiso 1 1 calc R . . C41 C 0.3458(2) 0.89818(16) 0.24874(16) 0.0357(7) Uani 1 1 d . . . C42 C 0.4466(2) 0.90292(17) 0.27764(18) 0.0433(8) Uani 1 1 d . . . H42 H 0.4955 0.9040 0.2493 0.052 Uiso 1 1 calc R . . C43 C 0.4760(2) 0.90601(18) 0.34651(18) 0.0457(8) Uani 1 1 d . . . H43 H 0.5448 0.9100 0.3653 0.055 Uiso 1 1 calc R . . C44 C 0.4067(2) 0.90343(17) 0.38838(17) 0.0414(8) Uani 1 1 d . . . H44 H 0.4281 0.9057 0.4359 0.050 Uiso 1 1 calc R . . C45 C 0.3047(2) 0.89752(15) 0.36214(16) 0.0339(7) Uani 1 1 d . . . C46 C 0.2756(2) 0.89610(14) 0.29180(15) 0.0310(7) Uani 1 1 d . . . C47 C 0.3152(2) 0.9008(2) 0.17257(17) 0.0474(9) Uani 1 1 d . . . H47 H 0.2416 0.8932 0.1625 0.057 Uiso 1 1 calc R . . C48 C 0.3616(4) 0.8449(2) 0.1365(2) 0.0791(14) Uani 1 1 d . . . H48A H 0.3346 0.8471 0.0880 0.119 Uiso 1 1 calc R . . H48B H 0.3463 0.7997 0.1541 0.119 Uiso 1 1 calc R . . H48C H 0.4340 0.8515 0.1436 0.119 Uiso 1 1 calc R . . C49 C 0.3337(6) 0.9703(3) 0.1453(2) 0.132(3) Uani 1 1 d . . . H49A H 0.3050 1.0059 0.1707 0.197 Uiso 1 1 calc R . . H49B H 0.3026 0.9728 0.0976 0.197 Uiso 1 1 calc R . . H49C H 0.4056 0.9779 0.1496 0.197 Uiso 1 1 calc R . . C50 C 0.2295(2) 0.89395(17) 0.41002(16) 0.0398(8) Uani 1 1 d . . . H50 H 0.1635 0.8807 0.3828 0.048 Uiso 1 1 calc R . . C51 C 0.2573(3) 0.8397(2) 0.46479(19) 0.0615(11) Uani 1 1 d . . . H51A H 0.3239 0.8496 0.4902 0.092 Uiso 1 1 calc R . . H51B H 0.2572 0.7939 0.4440 0.092 Uiso 1 1 calc R . . H51C H 0.2088 0.8405 0.4954 0.092 Uiso 1 1 calc R . . C52 C 0.2173(3) 0.9638(2) 0.4418(2) 0.0649(11) Uani 1 1 d . . . H52A H 0.2794 0.9763 0.4718 0.097 Uiso 1 1 calc R . . H52B H 0.1630 0.9615 0.4678 0.097 Uiso 1 1 calc R . . H52C H 0.2016 0.9987 0.4062 0.097 Uiso 1 1 calc R . . C53 C -0.1105(3) 0.7706(2) 0.08642(19) 0.0594(11) Uani 1 1 d . . . H53A H -0.0878 0.7714 0.0428 0.089 Uiso 1 1 calc R . . H53B H -0.1758 0.7930 0.0819 0.089 Uiso 1 1 calc R . . H53C H -0.1157 0.7226 0.1009 0.089 Uiso 1 1 calc R . . C54 C -0.0376(2) 0.80830(17) 0.13750(16) 0.0383(7) Uani 1 1 d . . . C55 C 0.0429(2) 0.84325(17) 0.12899(16) 0.0382(7) Uani 1 1 d . . . C56 C 0.0722(3) 0.8746(2) 0.0673(2) 0.0653(11) Uani 1 1 d . . . H56A H 0.0222 0.8628 0.0277 0.098 Uiso 1 1 calc R . . H56B H 0.1372 0.8564 0.0614 0.098 Uiso 1 1 calc R . . H56C H 0.0762 0.9249 0.0724 0.098 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 Cr1 0.0352(3) 0.0285(3) 0.0356(3) -0.0008(2) 0.0149(2) 0.0000(2) Cr2 0.0275(3) 0.0293(3) 0.0376(3) -0.0015(2) 0.0023(2) 0.0003(2) N1 0.0255(12) 0.0288(13) 0.0280(13) 0.0006(10) 0.0059(10) 0.0025(10) N2 0.0257(12) 0.0382(14) 0.0298(13) 0.0035(11) 0.0076(10) 0.0018(11) N3 0.0243(12) 0.0350(14) 0.0291(13) -0.0021(11) 0.0061(10) -0.0003(10) N4 0.0273(13) 0.0299(13) 0.0301(13) -0.0020(10) 0.0054(10) 0.0021(10) C1 0.0356(16) 0.0275(15) 0.0442(19) 0.0039(14) 0.0103(14) 0.0035(13) C2 0.0364(17) 0.0347(17) 0.0433(19) 0.0078(14) 0.0122(14) -0.0024(14) C3 0.0351(18) 0.059(2) 0.0370(19) 0.0056(16) 0.0092(15) -0.0037(16) C4 0.050(2) 0.074(3) 0.038(2) 0.0006(18) 0.0175(17) -0.0146(19) C5 0.039(2) 0.072(3) 0.053(2) -0.0133(19) 0.0263(18) -0.0192(18) C6 0.0312(18) 0.059(2) 0.055(2) -0.0127(18) 0.0162(16) -0.0113(16) C7 0.0309(17) 0.0421(18) 0.0382(18) -0.0023(14) 0.0089(14) -0.0043(14) C8 0.0299(16) 0.0403(18) 0.0377(18) 0.0011(14) 0.0111(14) -0.0051(13) C9 0.041(2) 0.111(4) 0.036(2) 0.019(2) 0.0082(16) 0.000(2) C10 0.078(3) 0.144(5) 0.068(3) 0.043(3) 0.009(3) 0.028(3) C11 0.059(3) 0.154(5) 0.043(3) -0.001(3) 0.001(2) -0.030(3) C12 0.0276(17) 0.061(2) 0.044(2) -0.0051(17) 0.0024(14) 0.0008(16) C13 0.094(4) 0.070(3) 0.052(3) -0.015(2) -0.005(2) 0.013(2) C14 0.057(3) 0.070(3) 0.061(3) 0.003(2) 0.001(2) 0.007(2) C15 0.0298(16) 0.0278(15) 0.0440(19) 0.0021(13) 0.0075(13) 0.0021(12) C16 0.0323(17) 0.0407(19) 0.056(2) 0.0001(16) 0.0067(16) 0.0072(14) C17 0.039(2) 0.046(2) 0.068(3) -0.0042(18) 0.0225(18) 0.0092(16) C18 0.052(2) 0.046(2) 0.043(2) -0.0064(16) 0.0213(17) 0.0076(16) C19 0.0388(17) 0.0309(16) 0.0392(18) -0.0002(13) 0.0103(14) 0.0048(13) C20 0.0305(15) 0.0282(15) 0.0354(17) 0.0015(13) 0.0108(13) 0.0004(12) C21 0.0307(17) 0.0424(18) 0.0413(19) 0.0032(15) 0.0012(14) 0.0015(14) C22 0.063(3) 0.071(3) 0.048(2) 0.017(2) -0.0033(19) -0.017(2) C23 0.0372(19) 0.052(2) 0.056(2) -0.0011(18) -0.0045(16) 0.0043(16) C24 0.0439(19) 0.0441(19) 0.0360(19) -0.0111(15) 0.0059(15) 0.0067(15) C25 0.073(3) 0.087(3) 0.039(2) -0.003(2) 0.001(2) 0.007(2) C26 0.058(3) 0.064(3) 0.074(3) -0.016(2) -0.002(2) -0.007(2) C27 0.0340(17) 0.0300(16) 0.0396(18) -0.0017(14) 0.0087(14) -0.0057(13) C28 0.0309(16) 0.0303(15) 0.0401(18) -0.0018(14) 0.0072(13) 0.0020(13) C29 0.0308(16) 0.0314(16) 0.058(2) -0.0055(15) 0.0127(15) -0.0020(13) C30 0.041(2) 0.041(2) 0.101(3) -0.005(2) 0.031(2) -0.0003(17) C31 0.034(2) 0.049(2) 0.125(4) 0.007(3) 0.011(2) 0.0144(18) C32 0.046(2) 0.045(2) 0.090(3) 0.010(2) -0.015(2) 0.0087(18) C33 0.043(2) 0.0320(17) 0.057(2) 0.0013(16) -0.0029(17) 0.0063(15) C34 0.0263(15) 0.0279(15) 0.0462(19) -0.0036(14) 0.0045(14) -0.0001(12) C35 0.045(2) 0.059(2) 0.049(2) -0.0100(18) 0.0234(17) 0.0003(17) C36 0.075(3) 0.069(3) 0.063(3) -0.015(2) 0.041(2) -0.014(2) C37 0.066(3) 0.107(4) 0.058(3) -0.022(2) 0.022(2) -0.036(3) C38 0.071(3) 0.053(2) 0.043(2) 0.0067(18) -0.0024(19) 0.019(2) C39 0.126(4) 0.070(3) 0.074(3) 0.018(3) 0.034(3) -0.002(3) C40 0.136(5) 0.099(4) 0.054(3) -0.005(3) -0.024(3) 0.024(3) C41 0.0308(16) 0.0396(18) 0.0379(18) -0.0019(14) 0.0095(14) 0.0032(13) C42 0.0272(17) 0.051(2) 0.054(2) 0.0014(17) 0.0128(15) 0.0002(15) C43 0.0272(17) 0.052(2) 0.056(2) 0.0023(17) 0.0028(16) -0.0041(15) C44 0.0348(18) 0.0461(19) 0.0404(19) -0.0012(15) -0.0011(15) -0.0004(15) C45 0.0303(16) 0.0338(16) 0.0381(18) -0.0026(13) 0.0073(13) -0.0008(13) C46 0.0279(15) 0.0285(15) 0.0367(17) -0.0012(13) 0.0058(13) 0.0002(12) C47 0.0311(17) 0.072(3) 0.042(2) 0.0013(18) 0.0158(15) 0.0083(17) C48 0.115(4) 0.072(3) 0.049(3) -0.008(2) 0.014(3) 0.022(3) C49 0.266(8) 0.062(3) 0.058(3) 0.021(3) 0.002(4) 0.029(4) C50 0.0363(18) 0.053(2) 0.0305(17) -0.0017(15) 0.0052(14) -0.0018(15) C51 0.062(3) 0.076(3) 0.048(2) 0.013(2) 0.015(2) -0.004(2) C52 0.076(3) 0.067(3) 0.059(3) -0.010(2) 0.031(2) 0.004(2) C53 0.055(2) 0.074(3) 0.052(2) -0.019(2) 0.0156(19) -0.011(2) C54 0.0428(19) 0.0406(18) 0.0306(17) -0.0002(14) 0.0042(14) 0.0090(15) C55 0.0421(19) 0.0413(18) 0.0306(17) -0.0045(14) 0.0044(14) 0.0063(15) C56 0.065(3) 0.073(3) 0.056(3) 0.016(2) 0.005(2) -0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 Cr2 1.9248(7) . ? Cr1 N1 1.927(2) . ? Cr1 N3 1.933(2) . ? Cr1 C55 1.965(3) . ? Cr1 C54 2.308(3) . ? Cr2 N2 1.901(2) . ? Cr2 N4 1.903(2) . ? Cr2 C54 2.039(3) . ? N1 C1 1.366(4) . ? N1 C20 1.455(3) . ? N2 C2 1.372(4) . ? N2 C8 1.458(4) . ? N3 C27 1.372(4) . ? N3 C46 1.452(4) . ? N4 C28 1.368(4) . ? N4 C34 1.457(4) . ? C1 C2 1.351(4) . ? C3 C4 1.395(4) . ? C3 C8 1.409(4) . ? C3 C9 1.521(5) . ? C4 C5 1.366(5) . ? C5 C6 1.373(5) . ? C6 C7 1.398(4) . ? C7 C8 1.396(4) . ? C7 C12 1.512(4) . ? C9 C10 1.525(6) . ? C9 C11 1.535(6) . ? C12 C14 1.523(5) . ? C12 C13 1.525(5) . ? C15 C20 1.399(4) . ? C15 C16 1.399(4) . ? C15 C21 1.517(4) . ? C16 C17 1.367(5) . ? C17 C18 1.379(5) . ? C18 C19 1.393(4) . ? C19 C20 1.410(4) . ? C19 C24 1.521(4) . ? C21 C23 1.528(4) . ? C21 C22 1.531(5) . ? C24 C25 1.523(5) . ? C24 C26 1.529(5) . ? C27 C28 1.356(4) . ? C29 C34 1.396(4) . ? C29 C30 1.402(5) . ? C29 C35 1.513(5) . ? C30 C31 1.362(6) . ? C31 C32 1.363(6) . ? C32 C33 1.403(5) . ? C33 C34 1.413(4) . ? C33 C38 1.504(5) . ? C35 C37 1.530(5) . ? C35 C36 1.540(5) . ? C38 C39 1.528(6) . ? C38 C40 1.536(6) . ? C41 C42 1.398(4) . ? C41 C46 1.399(4) . ? C41 C47 1.517(5) . ? C42 C43 1.375(5) . ? C43 C44 1.372(5) . ? C44 C45 1.401(4) . ? C45 C46 1.402(4) . ? C45 C50 1.527(4) . ? C47 C49 1.490(6) . ? C47 C48 1.502(5) . ? C50 C52 1.517(5) . ? C50 C51 1.522(5) . ? C53 C54 1.489(5) . ? C54 C55 1.326(5) . ? C55 C56 1.497(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 Cr2 Cr1 N1 104.15(7) . . ? Cr2 Cr1 N3 103.67(7) . . ? N1 Cr1 N3 128.39(10) . . ? Cr2 Cr1 C55 83.94(10) . . ? N1 Cr1 C55 118.45(12) . . ? N3 Cr1 C55 106.98(12) . . ? Cr2 Cr1 C54 56.73(8) . . ? N1 Cr1 C54 101.13(11) . . ? N3 Cr1 C54 130.47(11) . . ? C55 Cr1 C54 35.00(12) . . ? N2 Cr2 N4 139.21(10) . . ? N2 Cr2 Cr1 105.57(8) . . ? N4 Cr2 Cr1 103.24(7) . . ? N2 Cr2 C54 109.52(12) . . ? N4 Cr2 C54 106.75(12) . . ? Cr1 Cr2 C54 71.16(9) . . ? C1 N1 C20 114.1(2) . . ? C1 N1 Cr1 128.9(2) . . ? C20 N1 Cr1 115.74(17) . . ? C2 N2 C8 111.7(2) . . ? C2 N2 Cr2 128.2(2) . . ? C8 N2 Cr2 120.05(19) . . ? C27 N3 C46 112.4(2) . . ? C27 N3 Cr1 124.28(19) . . ? C46 N3 Cr1 122.99(18) . . ? C28 N4 C34 114.2(2) . . ? C28 N4 Cr2 128.82(19) . . ? C34 N4 Cr2 116.87(18) . . ? C2 C1 N1 125.5(3) . . ? C1 C2 N2 124.9(3) . . ? C4 C3 C8 117.5(3) . . ? C4 C3 C9 119.1(3) . . ? C8 C3 C9 123.4(3) . . ? C5 C4 C3 121.9(3) . . ? C4 C5 C6 119.9(3) . . ? C5 C6 C7 121.2(3) . . ? C8 C7 C6 118.2(3) . . ? C8 C7 C12 122.2(3) . . ? C6 C7 C12 119.4(3) . . ? C7 C8 C3 121.3(3) . . ? C7 C8 N2 119.8(3) . . ? C3 C8 N2 118.9(3) . . ? C3 C9 C10 111.6(4) . . ? C3 C9 C11 111.3(4) . . ? C10 C9 C11 110.8(4) . . ? C7 C12 C14 114.1(3) . . ? C7 C12 C13 109.9(3) . . ? C14 C12 C13 110.8(3) . . ? C20 C15 C16 117.6(3) . . ? C20 C15 C21 121.6(3) . . ? C16 C15 C21 120.7(3) . . ? C17 C16 C15 121.6(3) . . ? C16 C17 C18 120.4(3) . . ? C17 C18 C19 120.5(3) . . ? C18 C19 C20 118.5(3) . . ? C18 C19 C24 119.5(3) . . ? C20 C19 C24 122.0(3) . . ? C15 C20 C19 121.1(3) . . ? C15 C20 N1 119.4(3) . . ? C19 C20 N1 119.4(3) . . ? C15 C21 C23 113.3(3) . . ? C15 C21 C22 111.8(3) . . ? C23 C21 C22 108.0(3) . . ? C19 C24 C25 112.7(3) . . ? C19 C24 C26 110.9(3) . . ? C25 C24 C26 109.9(3) . . ? C28 C27 N3 125.7(3) . . ? C27 C28 N4 125.0(3) . . ? C34 C29 C30 117.7(3) . . ? C34 C29 C35 121.9(3) . . ? C30 C29 C35 120.3(3) . . ? C31 C30 C29 121.9(4) . . ? C30 C31 C32 119.5(4) . . ? C31 C32 C33 122.4(4) . . ? C32 C33 C34 116.9(4) . . ? C32 C33 C38 120.4(3) . . ? C34 C33 C38 122.7(3) . . ? C29 C34 C33 121.5(3) . . ? C29 C34 N4 119.6(3) . . ? C33 C34 N4 118.9(3) . . ? C29 C35 C37 110.4(3) . . ? C29 C35 C36 113.4(3) . . ? C37 C35 C36 109.6(3) . . ? C33 C38 C39 111.2(3) . . ? C33 C38 C40 113.4(4) . . ? C39 C38 C40 109.6(4) . . ? C42 C41 C46 118.2(3) . . ? C42 C41 C47 119.6(3) . . ? C46 C41 C47 122.0(3) . . ? C43 C42 C41 120.9(3) . . ? C44 C43 C42 120.5(3) . . ? C43 C44 C45 121.0(3) . . ? C46 C45 C44 117.9(3) . . ? C46 C45 C50 122.3(3) . . ? C44 C45 C50 119.8(3) . . ? C41 C46 C45 121.5(3) . . ? C41 C46 N3 120.7(3) . . ? C45 C46 N3 117.8(3) . . ? C49 C47 C48 111.0(4) . . ? C49 C47 C41 111.6(3) . . ? C48 C47 C41 113.6(3) . . ? C52 C50 C51 110.0(3) . . ? C52 C50 C45 111.1(3) . . ? C51 C50 C45 112.2(3) . . ? C55 C54 C53 128.9(3) . . ? C55 C54 Cr2 99.1(2) . . ? C53 C54 Cr2 132.0(3) . . ? C55 C54 Cr1 58.22(18) . . ? C53 C54 Cr1 153.8(3) . . ? Cr2 C54 Cr1 52.11(8) . . ? C54 C55 C56 131.3(3) . . ? C54 C55 Cr1 86.8(2) . . ? C56 C55 Cr1 140.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cr1 Cr2 N2 11.58(11) . . . . ? N3 Cr1 Cr2 N2 -124.51(11) . . . . ? C55 Cr1 Cr2 N2 129.44(12) . . . . ? C54 Cr1 Cr2 N2 105.74(13) . . . . ? N1 Cr1 Cr2 N4 162.39(10) . . . . ? N3 Cr1 Cr2 N4 26.30(11) . . . . ? C55 Cr1 Cr2 N4 -79.75(12) . . . . ? C54 Cr1 Cr2 N4 -103.45(12) . . . . ? N1 Cr1 Cr2 C54 -94.16(12) . . . . ? N3 Cr1 Cr2 C54 129.75(12) . . . . ? C55 Cr1 Cr2 C54 23.70(13) . . . . ? Cr2 Cr1 N1 C1 -1.4(3) . . . . ? N3 Cr1 N1 C1 119.4(3) . . . . ? C55 Cr1 N1 C1 -92.1(3) . . . . ? C54 Cr1 N1 C1 -59.5(3) . . . . ? Cr2 Cr1 N1 C20 165.10(18) . . . . ? N3 Cr1 N1 C20 -74.2(2) . . . . ? C55 Cr1 N1 C20 74.4(2) . . . . ? C54 Cr1 N1 C20 106.9(2) . . . . ? N4 Cr2 N2 C2 -152.7(2) . . . . ? Cr1 Cr2 N2 C2 -19.3(3) . . . . ? C54 Cr2 N2 C2 55.8(3) . . . . ? N4 Cr2 N2 C8 28.2(3) . . . . ? Cr1 Cr2 N2 C8 161.57(19) . . . . ? C54 Cr2 N2 C8 -123.3(2) . . . . ? Cr2 Cr1 N3 C27 -35.0(2) . . . . ? N1 Cr1 N3 C27 -155.9(2) . . . . ? C55 Cr1 N3 C27 52.8(3) . . . . ? C54 Cr1 N3 C27 22.7(3) . . . . ? Cr2 Cr1 N3 C46 152.1(2) . . . . ? N1 Cr1 N3 C46 31.2(3) . . . . ? C55 Cr1 N3 C46 -120.2(2) . . . . ? C54 Cr1 N3 C46 -150.3(2) . . . . ? N2 Cr2 N4 C28 119.7(3) . . . . ? Cr1 Cr2 N4 C28 -14.4(3) . . . . ? C54 Cr2 N4 C28 -88.4(3) . . . . ? N2 Cr2 N4 C34 -63.6(3) . . . . ? Cr1 Cr2 N4 C34 162.34(19) . . . . ? C54 Cr2 N4 C34 88.3(2) . . . . ? C20 N1 C1 C2 -176.1(3) . . . . ? Cr1 N1 C1 C2 -9.5(5) . . . . ? N1 C1 C2 N2 4.8(5) . . . . ? C8 N2 C2 C1 -169.2(3) . . . . ? Cr2 N2 C2 C1 11.6(5) . . . . ? C8 C3 C4 C5 -1.3(6) . . . . ? C9 C3 C4 C5 179.5(4) . . . . ? C3 C4 C5 C6 -0.4(6) . . . . ? C4 C5 C6 C7 1.5(6) . . . . ? C5 C6 C7 C8 -0.8(5) . . . . ? C5 C6 C7 C12 174.1(3) . . . . ? C6 C7 C8 C3 -0.9(5) . . . . ? C12 C7 C8 C3 -175.7(3) . . . . ? C6 C7 C8 N2 177.0(3) . . . . ? C12 C7 C8 N2 2.2(5) . . . . ? C4 C3 C8 C7 1.9(5) . . . . ? C9 C3 C8 C7 -178.9(4) . . . . ? C4 C3 C8 N2 -176.0(3) . . . . ? C9 C3 C8 N2 3.2(5) . . . . ? C2 N2 C8 C7 -110.7(3) . . . . ? Cr2 N2 C8 C7 68.5(3) . . . . ? C2 N2 C8 C3 67.2(4) . . . . ? Cr2 N2 C8 C3 -113.5(3) . . . . ? C4 C3 C9 C10 69.5(5) . . . . ? C8 C3 C9 C10 -109.7(4) . . . . ? C4 C3 C9 C11 -54.8(5) . . . . ? C8 C3 C9 C11 126.0(4) . . . . ? C8 C7 C12 C14 -140.2(3) . . . . ? C6 C7 C12 C14 45.1(4) . . . . ? C8 C7 C12 C13 94.8(4) . . . . ? C6 C7 C12 C13 -79.9(4) . . . . ? C20 C15 C16 C17 -0.9(5) . . . . ? C21 C15 C16 C17 176.4(3) . . . . ? C15 C16 C17 C18 -1.7(5) . . . . ? C16 C17 C18 C19 1.1(5) . . . . ? C17 C18 C19 C20 2.2(5) . . . . ? C17 C18 C19 C24 -175.0(3) . . . . ? C16 C15 C20 C19 4.2(4) . . . . ? C21 C15 C20 C19 -173.0(3) . . . . ? C16 C15 C20 N1 -177.1(3) . . . . ? C21 C15 C20 N1 5.6(4) . . . . ? C18 C19 C20 C15 -4.9(4) . . . . ? C24 C19 C20 C15 172.2(3) . . . . ? C18 C19 C20 N1 176.4(3) . . . . ? C24 C19 C20 N1 -6.5(4) . . . . ? C1 N1 C20 C15 -95.5(3) . . . . ? Cr1 N1 C20 C15 96.0(3) . . . . ? C1 N1 C20 C19 83.2(3) . . . . ? Cr1 N1 C20 C19 -85.3(3) . . . . ? C20 C15 C21 C23 -156.9(3) . . . . ? C16 C15 C21 C23 25.9(4) . . . . ? C20 C15 C21 C22 80.7(4) . . . . ? C16 C15 C21 C22 -96.4(4) . . . . ? C18 C19 C24 C25 -44.7(4) . . . . ? C20 C19 C24 C25 138.2(3) . . . . ? C18 C19 C24 C26 79.0(4) . . . . ? C20 C19 C24 C26 -98.1(4) . . . . ? C46 N3 C27 C28 -166.9(3) . . . . ? Cr1 N3 C27 C28 19.5(4) . . . . ? N3 C27 C28 N4 3.8(5) . . . . ? C34 N4 C28 C27 178.3(3) . . . . ? Cr2 N4 C28 C27 -5.0(4) . . . . ? C34 C29 C30 C31 -0.6(5) . . . . ? C35 C29 C30 C31 175.7(3) . . . . ? C29 C30 C31 C32 -0.2(6) . . . . ? C30 C31 C32 C33 0.1(6) . . . . ? C31 C32 C33 C34 0.9(6) . . . . ? C31 C32 C33 C38 -176.7(4) . . . . ? C30 C29 C34 C33 1.7(5) . . . . ? C35 C29 C34 C33 -174.6(3) . . . . ? C30 C29 C34 N4 179.7(3) . . . . ? C35 C29 C34 N4 3.5(4) . . . . ? C32 C33 C34 C29 -1.8(5) . . . . ? C38 C33 C34 C29 175.8(3) . . . . ? C32 C33 C34 N4 -179.9(3) . . . . ? C38 C33 C34 N4 -2.3(5) . . . . ? C28 N4 C34 C29 -95.1(3) . . . . ? Cr2 N4 C34 C29 87.7(3) . . . . ? C28 N4 C34 C33 83.0(3) . . . . ? Cr2 N4 C34 C33 -94.2(3) . . . . ? C34 C29 C35 C37 84.1(4) . . . . ? C30 C29 C35 C37 -92.1(4) . . . . ? C34 C29 C35 C36 -152.5(3) . . . . ? C30 C29 C35 C36 31.3(4) . . . . ? C32 C33 C38 C39 77.4(5) . . . . ? C34 C33 C38 C39 -100.1(4) . . . . ? C32 C33 C38 C40 -46.6(5) . . . . ? C34 C33 C38 C40 135.9(4) . . . . ? C46 C41 C42 C43 -0.5(5) . . . . ? C47 C41 C42 C43 175.0(3) . . . . ? C41 C42 C43 C44 1.0(5) . . . . ? C42 C43 C44 C45 0.1(5) . . . . ? C43 C44 C45 C46 -1.6(5) . . . . ? C43 C44 C45 C50 179.3(3) . . . . ? C42 C41 C46 C45 -1.0(5) . . . . ? C47 C41 C46 C45 -176.4(3) . . . . ? C42 C41 C46 N3 176.0(3) . . . . ? C47 C41 C46 N3 0.6(5) . . . . ? C44 C45 C46 C41 2.1(4) . . . . ? C50 C45 C46 C41 -178.8(3) . . . . ? C44 C45 C46 N3 -175.0(3) . . . . ? C50 C45 C46 N3 4.0(4) . . . . ? C27 N3 C46 C41 -100.1(3) . . . . ? Cr1 N3 C46 C41 73.6(3) . . . . ? C27 N3 C46 C45 77.0(3) . . . . ? Cr1 N3 C46 C45 -109.2(3) . . . . ? C42 C41 C47 C49 -67.8(5) . . . . ? C46 C41 C47 C49 107.5(4) . . . . ? C42 C41 C47 C48 58.7(5) . . . . ? C46 C41 C47 C48 -126.0(4) . . . . ? C46 C45 C50 C52 -106.0(4) . . . . ? C44 C45 C50 C52 73.0(4) . . . . ? C46 C45 C50 C51 130.3(3) . . . . ? C44 C45 C50 C51 -50.6(4) . . . . ? N2 Cr2 C54 C55 -137.2(2) . . . . ? N4 Cr2 C54 C55 61.8(2) . . . . ? Cr1 Cr2 C54 C55 -36.86(19) . . . . ? N2 Cr2 C54 C53 45.7(4) . . . . ? N4 Cr2 C54 C53 -115.3(3) . . . . ? Cr1 Cr2 C54 C53 146.1(3) . . . . ? N2 Cr2 C54 Cr1 -100.37(9) . . . . ? N4 Cr2 C54 Cr1 98.63(8) . . . . ? Cr2 Cr1 C54 C55 135.8(2) . . . . ? N1 Cr1 C54 C55 -124.4(2) . . . . ? N3 Cr1 C54 C55 56.7(2) . . . . ? Cr2 Cr1 C54 C53 -109.8(6) . . . . ? N1 Cr1 C54 C53 -10.0(6) . . . . ? N3 Cr1 C54 C53 171.1(5) . . . . ? C55 Cr1 C54 C53 114.4(6) . . . . ? N1 Cr1 C54 Cr2 99.73(9) . . . . ? N3 Cr1 C54 Cr2 -79.14(13) . . . . ? C55 Cr1 C54 Cr2 -135.8(2) . . . . ? C53 C54 C55 C56 20.7(6) . . . . ? Cr2 C54 C55 C56 -156.5(4) . . . . ? Cr1 C54 C55 C56 169.7(4) . . . . ? C53 C54 C55 Cr1 -149.0(3) . . . . ? Cr2 C54 C55 Cr1 33.84(15) . . . . ? Cr2 Cr1 C55 C54 -35.86(19) . . . . ? N1 Cr1 C55 C54 67.0(2) . . . . ? N3 Cr1 C55 C54 -138.34(19) . . . . ? Cr2 Cr1 C55 C56 156.4(4) . . . . ? N1 Cr1 C55 C56 -100.8(4) . . . . ? N3 Cr1 C55 C56 53.9(4) . . . . ? C54 Cr1 C55 C56 -167.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.728 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.068 # start Validation Reply Form _vrf_PLAT220_klat782 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.3 Ratio RESPONSE: The isopropyl group including C49 has slight but unresolvable disorder causing a large Ueq range. ; data_klat811 _database_code_depnum_ccdc_archive 'CCDC 839344' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H82 Cr2 N4' _chemical_formula_weight 939.28 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.145(3) _cell_length_b 23.048(6) _cell_length_c 18.413(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.677(4) _cell_angle_gamma 90.00 _cell_volume 5371(2) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 960 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 24.15 _exptl_crystal_description block _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.162 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 0.444 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7782 _exptl_absorpt_correction_T_max 0.9545 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _diffrn_ambient_temperature 200(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 AXS APEX diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 836.6 _diffrn_reflns_number 56130 _diffrn_reflns_av_R_equivalents 0.0652 _diffrn_reflns_av_sigmaI/netI 0.0579 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 28.36 _reflns_number_total 13376 _reflns_number_gt 8861 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2001)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _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^)+(0.1033P)^2^+1.1286P] 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 13376 _refine_ls_number_parameters 595 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1023 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.1838 _refine_ls_wR_factor_gt 0.1576 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Cr1 Cr 0.08169(3) 0.226906(16) 0.39962(2) 0.02776(12) Uani 1 1 d . . . Cr2 Cr 0.11329(3) 0.305378(16) 0.37512(2) 0.02809(12) Uani 1 1 d . . . N1 N 0.20413(17) 0.19984(8) 0.47333(11) 0.0284(4) Uani 1 1 d . . . N2 N 0.24754(17) 0.32180(9) 0.44575(12) 0.0292(4) Uani 1 1 d . . . N3 N 0.08430(17) 0.30401(8) 0.26581(11) 0.0274(4) Uani 1 1 d . . . N4 N -0.02290(16) 0.20355(8) 0.31200(11) 0.0274(4) Uani 1 1 d . . . C1 C 0.2845(2) 0.23266(10) 0.51785(15) 0.0332(6) Uani 1 1 d . . . H1 H 0.3306 0.2144 0.5604 0.040 Uiso 1 1 calc R . . C2 C 0.3029(2) 0.28917(11) 0.50545(15) 0.0327(6) Uani 1 1 d . . . H2 H 0.3592 0.3077 0.5414 0.039 Uiso 1 1 calc R . . C3 C 0.3093(2) 0.11204(11) 0.46827(15) 0.0364(6) Uani 1 1 d . . . C4 C 0.3287(3) 0.05315(12) 0.48531(17) 0.0463(8) Uani 1 1 d . . . H4 H 0.3884 0.0351 0.4752 0.056 Uiso 1 1 calc R . . C5 C 0.2631(3) 0.02109(12) 0.51640(17) 0.0518(9) Uani 1 1 d . . . H5 H 0.2776 -0.0188 0.5274 0.062 Uiso 1 1 calc R . . C6 C 0.1766(3) 0.04647(12) 0.53163(16) 0.0477(8) Uani 1 1 d . . . H6 H 0.1315 0.0236 0.5526 0.057 Uiso 1 1 calc R . . C7 C 0.1534(2) 0.10512(11) 0.51696(15) 0.0371(6) Uani 1 1 d . . . C8 C 0.2225(2) 0.13804(10) 0.48576(14) 0.0314(6) Uani 1 1 d . . . C9 C 0.3843(2) 0.14516(13) 0.43278(17) 0.0420(7) Uani 1 1 d . . . H9 H 0.3557 0.1853 0.4208 0.050 Uiso 1 1 calc R . . C10 C 0.4941(3) 0.15010(17) 0.4880(2) 0.0613(9) Uani 1 1 d . . . H10A H 0.4888 0.1702 0.5337 0.092 Uiso 1 1 calc R . . H10B H 0.5405 0.1721 0.4644 0.092 Uiso 1 1 calc R . . H10C H 0.5233 0.1112 0.5012 0.092 Uiso 1 1 calc R . . C11 C 0.3931(3) 0.11725(16) 0.3598(2) 0.0611(9) Uani 1 1 d . . . H11A H 0.4187 0.0773 0.3698 0.092 Uiso 1 1 calc R . . H11B H 0.4429 0.1395 0.3395 0.092 Uiso 1 1 calc R . . H11C H 0.3236 0.1170 0.3230 0.092 Uiso 1 1 calc R . . C12 C 0.0636(3) 0.13218(13) 0.54125(16) 0.0438(7) Uani 1 1 d . . . H12 H 0.0448 0.1692 0.5125 0.053 Uiso 1 1 calc R . . C13 C 0.1002(3) 0.14789(19) 0.62501(19) 0.0705(11) Uani 1 1 d . . . H13A H 0.1232 0.1127 0.6548 0.106 Uiso 1 1 calc R . . H13B H 0.0417 0.1658 0.6404 0.106 Uiso 1 1 calc R . . H13C H 0.1593 0.1753 0.6335 0.106 Uiso 1 1 calc R . . C14 C -0.0365(3) 0.09475(16) 0.5241(2) 0.0619(9) Uani 1 1 d . . . H14A H -0.0565 0.0839 0.4707 0.093 Uiso 1 1 calc R . . H14B H -0.0941 0.1168 0.5355 0.093 Uiso 1 1 calc R . . H14C H -0.0228 0.0596 0.5553 0.093 Uiso 1 1 calc R . . C15 C 0.3617(2) 0.39264(13) 0.40366(18) 0.0457(7) Uani 1 1 d . . . C16 C 0.4023(3) 0.44879(16) 0.4063(2) 0.0666(11) Uani 1 1 d . . . H16 H 0.4504 0.4577 0.3777 0.080 Uiso 1 1 calc R . . C17 C 0.3742(4) 0.49158(16) 0.4494(3) 0.0789(13) Uani 1 1 d . . . H17 H 0.4026 0.5295 0.4497 0.095 Uiso 1 1 calc R . . C18 C 0.3057(3) 0.47965(14) 0.4916(2) 0.0665(11) Uani 1 1 d . . . H18 H 0.2876 0.5095 0.5214 0.080 Uiso 1 1 calc R . . C19 C 0.2611(3) 0.42394(12) 0.49191(17) 0.0463(8) Uani 1 1 d . . . C20 C 0.2888(2) 0.38089(11) 0.44657(16) 0.0376(6) Uani 1 1 d . . . C21 C 0.4012(2) 0.34612(15) 0.36007(18) 0.0494(8) Uani 1 1 d . . . H21 H 0.3410 0.3192 0.3384 0.059 Uiso 1 1 calc R . . C22 C 0.4392(3) 0.37008(18) 0.2947(2) 0.0660(10) Uani 1 1 d . . . H22A H 0.3850 0.3957 0.2639 0.099 Uiso 1 1 calc R . . H22B H 0.4523 0.3379 0.2637 0.099 Uiso 1 1 calc R . . H22C H 0.5047 0.3920 0.3147 0.099 Uiso 1 1 calc R . . C23 C 0.4892(3) 0.31067(19) 0.4116(2) 0.0728(12) Uani 1 1 d . . . H23A H 0.5492 0.3361 0.4341 0.109 Uiso 1 1 calc R . . H23B H 0.5118 0.2802 0.3822 0.109 Uiso 1 1 calc R . . H23C H 0.4634 0.2929 0.4516 0.109 Uiso 1 1 calc R . . C24 C 0.1889(3) 0.41212(13) 0.54020(18) 0.0502(8) Uani 1 1 d . . . H24 H 0.1458 0.3770 0.5200 0.060 Uiso 1 1 calc R . . C25 C 0.2485(4) 0.4004(2) 0.6214(2) 0.0871(14) Uani 1 1 d . . . H25A H 0.2977 0.3681 0.6234 0.131 Uiso 1 1 calc R . . H25B H 0.1984 0.3904 0.6503 0.131 Uiso 1 1 calc R . . H25C H 0.2882 0.4351 0.6431 0.131 Uiso 1 1 calc R . . C26 C 0.1130(4) 0.4631(2) 0.5387(3) 0.0929(15) Uani 1 1 d . . . H26A H 0.1527 0.4963 0.5655 0.139 Uiso 1 1 calc R . . H26B H 0.0588 0.4516 0.5633 0.139 Uiso 1 1 calc R . . H26C H 0.0793 0.4741 0.4862 0.139 Uiso 1 1 calc R . . C27 C -0.0010(2) 0.27480(11) 0.22139(14) 0.0328(6) Uani 1 1 d . . . H27 H -0.0268 0.2878 0.1708 0.039 Uiso 1 1 calc R . . C28 C -0.0519(2) 0.22960(11) 0.24196(14) 0.0330(6) Uani 1 1 d . . . H28 H -0.1120 0.2146 0.2057 0.040 Uiso 1 1 calc R . . C29 C 0.1968(2) 0.30965(12) 0.17934(15) 0.0387(6) Uani 1 1 d . . . C30 C 0.2414(3) 0.34246(14) 0.13236(17) 0.0468(7) Uani 1 1 d . . . H30 H 0.2809 0.3235 0.1031 0.056 Uiso 1 1 calc R . . C31 C 0.2295(3) 0.40143(15) 0.12736(18) 0.0521(8) Uani 1 1 d . . . H31 H 0.2608 0.4229 0.0950 0.063 Uiso 1 1 calc R . . C32 C 0.1728(3) 0.42944(13) 0.16893(17) 0.0476(8) Uani 1 1 d . . . H32 H 0.1653 0.4704 0.1650 0.057 Uiso 1 1 calc R . . C33 C 0.1251(2) 0.39911(12) 0.21733(16) 0.0388(6) Uani 1 1 d . . . C34 C 0.1377(2) 0.33844(11) 0.22141(14) 0.0309(5) Uani 1 1 d . . . C35 C 0.2115(3) 0.24396(13) 0.18172(17) 0.0460(7) Uani 1 1 d . . . H35 H 0.1762 0.2280 0.2192 0.055 Uiso 1 1 calc R . . C36 C 0.3280(3) 0.22728(18) 0.2075(2) 0.0709(11) Uani 1 1 d . . . H36A H 0.3657 0.2455 0.1743 0.106 Uiso 1 1 calc R . . H36B H 0.3348 0.1850 0.2053 0.106 Uiso 1 1 calc R . . H36C H 0.3582 0.2406 0.2594 0.106 Uiso 1 1 calc R . . C37 C 0.1584(4) 0.21693(16) 0.1050(2) 0.0669(11) Uani 1 1 d . . . H37A H 0.0827 0.2258 0.0911 0.100 Uiso 1 1 calc R . . H37B H 0.1684 0.1748 0.1078 0.100 Uiso 1 1 calc R . . H37C H 0.1902 0.2329 0.0668 0.100 Uiso 1 1 calc R . . C38 C 0.0566(3) 0.43094(13) 0.25782(18) 0.0469(7) Uani 1 1 d . . . H38 H 0.0445 0.4044 0.2976 0.056 Uiso 1 1 calc R . . C39 C 0.1079(4) 0.48600(15) 0.2970(2) 0.0700(11) Uani 1 1 d . . . H39A H 0.1774 0.4766 0.3307 0.105 Uiso 1 1 calc R . . H39B H 0.0631 0.5027 0.3265 0.105 Uiso 1 1 calc R . . H39C H 0.1162 0.5141 0.2591 0.105 Uiso 1 1 calc R . . C40 C -0.0507(3) 0.4438(2) 0.2033(3) 0.0920(15) Uani 1 1 d . . . H40A H -0.0412 0.4688 0.1625 0.138 Uiso 1 1 calc R . . H40B H -0.0956 0.4636 0.2302 0.138 Uiso 1 1 calc R . . H40C H -0.0842 0.4074 0.1820 0.138 Uiso 1 1 calc R . . C41 C -0.0391(2) 0.09655(11) 0.30306(15) 0.0386(7) Uani 1 1 d . . . C42 C -0.1002(3) 0.04749(13) 0.30503(18) 0.0533(9) Uani 1 1 d . . . H42 H -0.0733 0.0104 0.2972 0.064 Uiso 1 1 calc R . . C43 C -0.1979(3) 0.05109(16) 0.31792(19) 0.0618(10) Uani 1 1 d . . . H43 H -0.2380 0.0169 0.3184 0.074 Uiso 1 1 calc R . . C44 C -0.2375(3) 0.10368(17) 0.33006(19) 0.0580(9) Uani 1 1 d . . . H44 H -0.3052 0.1055 0.3392 0.070 Uiso 1 1 calc R . . C45 C -0.1812(2) 0.15519(14) 0.32951(16) 0.0428(7) Uani 1 1 d . . . C46 C -0.0814(2) 0.15099(11) 0.31599(14) 0.0316(6) Uani 1 1 d . . . C47 C 0.0652(3) 0.09155(12) 0.28373(19) 0.0473(7) Uani 1 1 d . . . H47 H 0.1106 0.1246 0.3087 0.057 Uiso 1 1 calc R . . C48 C 0.0508(3) 0.09701(17) 0.1990(2) 0.0722(11) Uani 1 1 d . . . H48A H 0.0062 0.0652 0.1729 0.108 Uiso 1 1 calc R . . H48B H 0.1199 0.0952 0.1885 0.108 Uiso 1 1 calc R . . H48C H 0.0169 0.1342 0.1813 0.108 Uiso 1 1 calc R . . C49 C 0.1243(3) 0.03575(14) 0.3121(2) 0.0667(11) Uani 1 1 d . . . H49A H 0.1337 0.0322 0.3666 0.100 Uiso 1 1 calc R . . H49B H 0.1936 0.0366 0.3018 0.100 Uiso 1 1 calc R . . H49C H 0.0837 0.0025 0.2862 0.100 Uiso 1 1 calc R . . C50 C -0.2292(3) 0.21288(16) 0.34137(19) 0.0520(8) Uani 1 1 d . . . H50 H -0.1766 0.2438 0.3396 0.062 Uiso 1 1 calc R . . C51 C -0.2512(4) 0.2159(2) 0.4191(3) 0.0968(16) Uani 1 1 d . . . H51A H -0.3013 0.1853 0.4229 0.145 Uiso 1 1 calc R . . H51B H -0.2814 0.2539 0.4253 0.145 Uiso 1 1 calc R . . H51C H -0.1850 0.2105 0.4586 0.145 Uiso 1 1 calc R . . C52 C -0.3296(3) 0.22517(19) 0.2782(3) 0.0786(12) Uani 1 1 d . . . H52A H -0.3123 0.2265 0.2297 0.118 Uiso 1 1 calc R . . H52B H -0.3594 0.2625 0.2875 0.118 Uiso 1 1 calc R . . H52C H -0.3813 0.1943 0.2770 0.118 Uiso 1 1 calc R . . C53 C -0.1905(4) 0.3734(2) 0.3295(4) 0.113(2) Uani 1 1 d . . . H53A H -0.1767 0.3577 0.2836 0.170 Uiso 1 1 calc R . . H53B H -0.2284 0.4104 0.3178 0.170 Uiso 1 1 calc R . . H53C H -0.2337 0.3459 0.3488 0.170 Uiso 1 1 calc R . . C54 C -0.0869(3) 0.38323(15) 0.3885(2) 0.0575(9) Uani 1 1 d . . . H54A H -0.1015 0.3938 0.4368 0.069 Uiso 1 1 calc R . . H54B H -0.0494 0.4162 0.3728 0.069 Uiso 1 1 calc R . . C55 C -0.0159(2) 0.33004(12) 0.40051(16) 0.0390(6) Uani 1 1 d . . . C56 C 0.0126(2) 0.28931(13) 0.45200(17) 0.0417(7) Uani 1 1 d . . . C57 C 0.0093(4) 0.28534(17) 0.5332(2) 0.0670(11) Uani 1 1 d . . . H57A H 0.0830 0.2834 0.5652 0.080 Uiso 1 1 calc R . . H57B H -0.0252 0.2482 0.5396 0.080 Uiso 1 1 calc R . . C58 C -0.0463(4) 0.3335(2) 0.5634(3) 0.0958(16) Uani 1 1 d . . . H58A H -0.0181 0.3711 0.5532 0.144 Uiso 1 1 calc R . . H58B H -0.0345 0.3287 0.6179 0.144 Uiso 1 1 calc R . . H58C H -0.1223 0.3320 0.5385 0.144 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 Cr1 0.0311(2) 0.0260(2) 0.0237(2) 0.00162(15) 0.00324(16) -0.00193(16) Cr2 0.0333(2) 0.0243(2) 0.0242(2) 0.00058(15) 0.00346(16) -0.00036(16) N1 0.0337(12) 0.0235(10) 0.0257(10) 0.0024(8) 0.0043(9) -0.0019(8) N2 0.0324(11) 0.0228(10) 0.0293(10) 0.0004(8) 0.0029(9) 0.0011(8) N3 0.0318(11) 0.0254(10) 0.0238(10) 0.0030(8) 0.0056(8) -0.0025(8) N4 0.0303(11) 0.0265(10) 0.0243(10) 0.0015(8) 0.0055(8) -0.0031(8) C1 0.0383(15) 0.0283(12) 0.0272(12) 0.0007(10) -0.0013(11) 0.0016(11) C2 0.0326(14) 0.0293(12) 0.0308(13) -0.0039(10) -0.0007(11) 0.0010(10) C3 0.0455(16) 0.0259(12) 0.0314(13) 0.0007(10) -0.0005(12) 0.0010(11) C4 0.058(2) 0.0310(14) 0.0401(16) -0.0015(12) -0.0025(14) 0.0114(13) C5 0.079(2) 0.0247(13) 0.0423(17) 0.0062(12) 0.0004(16) -0.0012(15) C6 0.071(2) 0.0313(14) 0.0368(15) 0.0053(12) 0.0069(15) -0.0090(14) C7 0.0494(17) 0.0294(13) 0.0277(13) 0.0036(10) 0.0025(12) -0.0076(12) C8 0.0383(15) 0.0241(12) 0.0253(12) 0.0026(9) -0.0025(10) -0.0022(10) C9 0.0414(17) 0.0378(15) 0.0465(17) -0.0028(12) 0.0113(13) 0.0032(12) C10 0.0423(19) 0.070(2) 0.067(2) -0.0042(19) 0.0067(17) -0.0032(17) C11 0.076(3) 0.057(2) 0.054(2) -0.0059(16) 0.0234(19) 0.0016(18) C12 0.059(2) 0.0392(15) 0.0357(15) 0.0044(12) 0.0163(14) -0.0073(14) C13 0.087(3) 0.085(3) 0.0403(19) -0.0130(18) 0.0193(19) -0.008(2) C14 0.064(2) 0.062(2) 0.062(2) 0.0084(18) 0.0212(19) -0.0160(18) C15 0.0439(17) 0.0384(15) 0.0461(17) 0.0089(13) -0.0025(14) -0.0110(13) C16 0.072(3) 0.051(2) 0.069(2) 0.0121(18) 0.005(2) -0.0244(18) C17 0.109(4) 0.040(2) 0.078(3) 0.0016(19) 0.008(3) -0.031(2) C18 0.094(3) 0.0295(16) 0.061(2) -0.0089(15) -0.005(2) -0.0043(17) C19 0.058(2) 0.0282(14) 0.0404(16) -0.0020(11) -0.0075(14) 0.0045(13) C20 0.0424(16) 0.0245(12) 0.0358(14) 0.0006(10) -0.0067(12) -0.0014(11) C21 0.0387(17) 0.059(2) 0.0501(18) 0.0116(15) 0.0108(14) -0.0071(15) C22 0.055(2) 0.086(3) 0.057(2) 0.015(2) 0.0170(18) -0.017(2) C23 0.057(2) 0.098(3) 0.067(2) 0.031(2) 0.023(2) 0.022(2) C24 0.060(2) 0.0362(15) 0.0462(17) -0.0150(13) 0.0004(15) 0.0098(14) C25 0.098(3) 0.112(4) 0.043(2) 0.002(2) 0.005(2) 0.022(3) C26 0.098(3) 0.072(3) 0.110(4) -0.005(3) 0.028(3) 0.037(3) C27 0.0366(14) 0.0357(14) 0.0225(12) 0.0035(10) 0.0017(10) -0.0047(11) C28 0.0336(14) 0.0365(14) 0.0252(12) 0.0012(10) 0.0017(10) -0.0064(11) C29 0.0407(16) 0.0433(15) 0.0308(14) 0.0062(11) 0.0072(12) -0.0075(12) C30 0.0487(18) 0.0553(19) 0.0391(16) 0.0079(14) 0.0164(14) -0.0061(15) C31 0.0508(19) 0.060(2) 0.0435(17) 0.0177(15) 0.0099(15) -0.0176(16) C32 0.0517(19) 0.0381(15) 0.0464(17) 0.0142(13) 0.0019(15) -0.0131(14) C33 0.0405(16) 0.0341(14) 0.0357(14) 0.0081(11) 0.0001(12) -0.0049(12) C34 0.0318(14) 0.0315(13) 0.0265(12) 0.0055(10) 0.0033(10) -0.0067(10) C35 0.059(2) 0.0457(17) 0.0398(16) 0.0054(13) 0.0246(15) 0.0049(15) C36 0.076(3) 0.073(3) 0.068(3) 0.008(2) 0.027(2) 0.026(2) C37 0.102(3) 0.054(2) 0.050(2) -0.0073(16) 0.028(2) -0.008(2) C38 0.056(2) 0.0326(14) 0.0494(18) 0.0100(13) 0.0105(15) 0.0057(13) C39 0.106(3) 0.0386(18) 0.061(2) -0.0016(16) 0.015(2) 0.0036(19) C40 0.069(3) 0.100(4) 0.095(3) -0.015(3) 0.002(3) 0.031(3) C41 0.0473(17) 0.0293(13) 0.0317(14) 0.0039(11) -0.0021(12) -0.0075(12) C42 0.071(2) 0.0341(15) 0.0434(17) 0.0076(13) -0.0046(16) -0.0144(15) C43 0.066(2) 0.063(2) 0.0463(19) 0.0210(16) -0.0036(17) -0.0354(19) C44 0.049(2) 0.075(3) 0.0489(19) 0.0172(17) 0.0115(16) -0.0254(18) C45 0.0390(16) 0.0574(18) 0.0309(14) 0.0083(13) 0.0074(12) -0.0128(14) C46 0.0329(14) 0.0342(13) 0.0248(12) 0.0045(10) 0.0028(10) -0.0095(11) C47 0.0481(18) 0.0286(14) 0.060(2) -0.0097(13) 0.0059(15) -0.0007(13) C48 0.084(3) 0.062(2) 0.084(3) 0.014(2) 0.045(2) 0.020(2) C49 0.071(2) 0.0398(18) 0.075(3) -0.0114(17) -0.004(2) 0.0130(17) C50 0.0374(17) 0.072(2) 0.0522(19) 0.0026(16) 0.0210(15) -0.0005(16) C51 0.088(3) 0.145(5) 0.076(3) 0.011(3) 0.053(3) 0.033(3) C52 0.061(3) 0.083(3) 0.085(3) 0.015(2) 0.008(2) 0.006(2) C53 0.071(3) 0.075(3) 0.161(6) -0.012(3) -0.025(3) 0.032(2) C54 0.056(2) 0.056(2) 0.064(2) 0.0036(17) 0.0212(18) 0.0211(16) C55 0.0391(16) 0.0398(15) 0.0377(15) -0.0045(12) 0.0095(12) 0.0039(12) C56 0.0393(16) 0.0443(16) 0.0425(16) -0.0065(13) 0.0131(13) 0.0027(13) C57 0.101(3) 0.061(2) 0.048(2) 0.0027(16) 0.035(2) 0.021(2) C58 0.140(5) 0.083(3) 0.088(3) -0.010(3) 0.071(3) -0.001(3) _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 N4 1.893(2) . ? Cr1 N1 1.908(2) . ? Cr1 Cr2 1.9361(7) . ? Cr1 C56 2.073(3) . ? Cr2 N2 1.926(2) . ? Cr2 N3 1.945(2) . ? Cr2 C55 1.963(3) . ? Cr2 C56 2.215(3) . ? N1 C1 1.376(3) . ? N1 C8 1.453(3) . ? N2 C2 1.368(3) . ? N2 C20 1.465(3) . ? N3 C27 1.372(3) . ? N3 C34 1.449(3) . ? N4 C28 1.380(3) . ? N4 C46 1.447(3) . ? C1 C2 1.355(4) . ? C3 C4 1.401(4) . ? C3 C8 1.401(4) . ? C3 C9 1.526(4) . ? C4 C5 1.373(5) . ? C5 C6 1.373(5) . ? C6 C7 1.396(4) . ? C7 C8 1.418(4) . ? C7 C12 1.507(4) . ? C9 C11 1.523(4) . ? C9 C10 1.528(4) . ? C12 C13 1.530(4) . ? C12 C14 1.533(4) . ? C15 C16 1.395(4) . ? C15 C20 1.423(4) . ? C15 C21 1.513(5) . ? C16 C17 1.376(6) . ? C17 C18 1.368(6) . ? C18 C19 1.412(4) . ? C19 C20 1.407(4) . ? C19 C24 1.491(5) . ? C21 C23 1.521(5) . ? C21 C22 1.525(4) . ? C24 C25 1.514(5) . ? C24 C26 1.537(5) . ? C27 C28 1.347(4) . ? C29 C30 1.392(4) . ? C29 C34 1.403(4) . ? C29 C35 1.525(4) . ? C30 C31 1.368(5) . ? C31 C32 1.367(5) . ? C32 C33 1.406(4) . ? C33 C34 1.408(4) . ? C33 C38 1.506(4) . ? C35 C36 1.525(5) . ? C35 C37 1.530(5) . ? C38 C39 1.524(5) . ? C38 C40 1.524(5) . ? C41 C42 1.393(4) . ? C41 C46 1.419(4) . ? C41 C47 1.510(4) . ? C42 C43 1.370(5) . ? C43 C44 1.361(5) . ? C44 C45 1.400(4) . ? C45 C46 1.404(4) . ? C45 C50 1.512(5) . ? C47 C49 1.521(4) . ? C47 C48 1.525(5) . ? C50 C52 1.532(5) . ? C50 C51 1.536(5) . ? C53 C54 1.512(6) . ? C54 C55 1.520(4) . ? C55 C56 1.315(4) . ? C56 C57 1.510(4) . ? C57 C58 1.516(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 N4 Cr1 N1 142.37(9) . . ? N4 Cr1 Cr2 102.66(6) . . ? N1 Cr1 Cr2 106.16(6) . . ? N4 Cr1 C56 106.57(11) . . ? N1 Cr1 C56 106.69(11) . . ? Cr2 Cr1 C56 66.97(9) . . ? N2 Cr2 Cr1 103.96(6) . . ? N2 Cr2 N3 126.13(9) . . ? Cr1 Cr2 N3 103.39(6) . . ? N2 Cr2 C55 118.42(11) . . ? Cr1 Cr2 C55 87.78(9) . . ? N3 Cr2 C55 108.12(11) . . ? N2 Cr2 C56 101.42(11) . . ? Cr1 Cr2 C56 59.47(8) . . ? N3 Cr2 C56 132.45(10) . . ? C55 Cr2 C56 36.05(11) . . ? C1 N1 C8 112.2(2) . . ? C1 N1 Cr1 127.48(16) . . ? C8 N1 Cr1 120.34(16) . . ? C2 N2 C20 112.8(2) . . ? C2 N2 Cr2 128.77(18) . . ? C20 N2 Cr2 117.32(16) . . ? C27 N3 C34 112.0(2) . . ? C27 N3 Cr2 121.65(17) . . ? C34 N3 Cr2 125.84(16) . . ? C28 N4 C46 113.3(2) . . ? C28 N4 Cr1 128.80(17) . . ? C46 N4 Cr1 117.91(15) . . ? C2 C1 N1 124.8(2) . . ? C1 C2 N2 125.7(2) . . ? C4 C3 C8 118.2(3) . . ? C4 C3 C9 118.8(3) . . ? C8 C3 C9 123.0(2) . . ? C5 C4 C3 121.2(3) . . ? C4 C5 C6 120.3(3) . . ? C5 C6 C7 121.5(3) . . ? C6 C7 C8 117.8(3) . . ? C6 C7 C12 119.4(3) . . ? C8 C7 C12 122.5(2) . . ? C3 C8 C7 121.0(2) . . ? C3 C8 N1 119.6(2) . . ? C7 C8 N1 119.4(2) . . ? C11 C9 C3 112.3(3) . . ? C11 C9 C10 109.6(3) . . ? C3 C9 C10 110.8(3) . . ? C7 C12 C13 109.8(3) . . ? C7 C12 C14 113.8(3) . . ? C13 C12 C14 111.1(3) . . ? C16 C15 C20 117.7(3) . . ? C16 C15 C21 119.6(3) . . ? C20 C15 C21 122.6(3) . . ? C17 C16 C15 121.7(4) . . ? C18 C17 C16 120.2(3) . . ? C17 C18 C19 121.5(3) . . ? C20 C19 C18 117.7(3) . . ? C20 C19 C24 122.3(3) . . ? C18 C19 C24 120.0(3) . . ? C19 C20 C15 121.1(3) . . ? C19 C20 N2 120.5(3) . . ? C15 C20 N2 118.3(2) . . ? C15 C21 C23 111.2(3) . . ? C15 C21 C22 113.2(3) . . ? C23 C21 C22 109.3(3) . . ? C19 C24 C25 112.2(3) . . ? C19 C24 C26 111.3(3) . . ? C25 C24 C26 108.4(3) . . ? C28 C27 N3 126.9(2) . . ? C27 C28 N4 124.5(2) . . ? C30 C29 C34 118.4(3) . . ? C30 C29 C35 119.1(3) . . ? C34 C29 C35 122.6(2) . . ? C31 C30 C29 121.5(3) . . ? C32 C31 C30 120.1(3) . . ? C31 C32 C33 121.6(3) . . ? C32 C33 C34 117.5(3) . . ? C32 C33 C38 120.0(3) . . ? C34 C33 C38 122.3(3) . . ? C29 C34 C33 121.0(2) . . ? C29 C34 N3 118.5(2) . . ? C33 C34 N3 120.4(2) . . ? C29 C35 C36 111.6(3) . . ? C29 C35 C37 110.8(3) . . ? C36 C35 C37 110.7(3) . . ? C33 C38 C39 113.2(3) . . ? C33 C38 C40 109.8(3) . . ? C39 C38 C40 111.2(3) . . ? C42 C41 C46 117.3(3) . . ? C42 C41 C47 120.7(3) . . ? C46 C41 C47 121.9(2) . . ? C43 C42 C41 122.0(3) . . ? C44 C43 C42 120.0(3) . . ? C43 C44 C45 121.8(3) . . ? C44 C45 C46 117.6(3) . . ? C44 C45 C50 120.2(3) . . ? C46 C45 C50 122.2(3) . . ? C45 C46 C41 121.2(2) . . ? C45 C46 N4 119.1(2) . . ? C41 C46 N4 119.6(2) . . ? C41 C47 C49 113.3(3) . . ? C41 C47 C48 111.4(3) . . ? C49 C47 C48 109.4(3) . . ? C45 C50 C52 111.1(3) . . ? C45 C50 C51 111.4(3) . . ? C52 C50 C51 111.0(3) . . ? C53 C54 C55 112.5(3) . . ? C56 C55 C54 136.5(3) . . ? C56 C55 Cr2 82.46(19) . . ? C54 C55 Cr2 137.3(2) . . ? C55 C56 C57 132.7(3) . . ? C55 C56 Cr1 103.6(2) . . ? C57 C56 Cr1 123.5(2) . . ? C55 C56 Cr2 61.48(17) . . ? C57 C56 Cr2 145.6(3) . . ? Cr1 C56 Cr2 53.56(7) . . ? C56 C57 C58 117.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Cr1 Cr2 N2 -161.99(10) . . . . ? N1 Cr1 Cr2 N2 -6.47(10) . . . . ? C56 Cr1 Cr2 N2 95.17(12) . . . . ? N4 Cr1 Cr2 N3 -28.85(10) . . . . ? N1 Cr1 Cr2 N3 126.67(9) . . . . ? C56 Cr1 Cr2 N3 -131.69(12) . . . . ? N4 Cr1 Cr2 C55 79.25(11) . . . . ? N1 Cr1 Cr2 C55 -125.23(11) . . . . ? C56 Cr1 Cr2 C55 -23.59(12) . . . . ? N4 Cr1 Cr2 C56 102.83(11) . . . . ? N1 Cr1 Cr2 C56 -101.64(12) . . . . ? N4 Cr1 N1 C1 157.1(2) . . . . ? Cr2 Cr1 N1 C1 18.5(2) . . . . ? C56 Cr1 N1 C1 -51.7(2) . . . . ? N4 Cr1 N1 C8 -20.7(3) . . . . ? Cr2 Cr1 N1 C8 -159.25(18) . . . . ? C56 Cr1 N1 C8 130.5(2) . . . . ? Cr1 Cr2 N2 C2 -7.1(2) . . . . ? N3 Cr2 N2 C2 -125.6(2) . . . . ? C55 Cr2 N2 C2 88.0(2) . . . . ? C56 Cr2 N2 C2 54.0(2) . . . . ? Cr1 Cr2 N2 C20 -174.16(18) . . . . ? N3 Cr2 N2 C20 67.3(2) . . . . ? C55 Cr2 N2 C20 -79.1(2) . . . . ? C56 Cr2 N2 C20 -113.1(2) . . . . ? N2 Cr2 N3 C27 158.89(18) . . . . ? Cr1 Cr2 N3 C27 40.1(2) . . . . ? C55 Cr2 N3 C27 -51.9(2) . . . . ? C56 Cr2 N3 C27 -20.5(3) . . . . ? N2 Cr2 N3 C34 -30.0(2) . . . . ? Cr1 Cr2 N3 C34 -148.77(19) . . . . ? C55 Cr2 N3 C34 119.2(2) . . . . ? C56 Cr2 N3 C34 150.6(2) . . . . ? N1 Cr1 N4 C28 -125.8(2) . . . . ? Cr2 Cr1 N4 C28 13.6(2) . . . . ? C56 Cr1 N4 C28 83.0(2) . . . . ? N1 Cr1 N4 C46 53.2(3) . . . . ? Cr2 Cr1 N4 C46 -167.44(17) . . . . ? C56 Cr1 N4 C46 -98.0(2) . . . . ? C8 N1 C1 C2 162.2(3) . . . . ? Cr1 N1 C1 C2 -15.7(4) . . . . ? N1 C1 C2 N2 -2.6(5) . . . . ? C20 N2 C2 C1 -177.9(3) . . . . ? Cr2 N2 C2 C1 14.6(4) . . . . ? C8 C3 C4 C5 1.8(4) . . . . ? C9 C3 C4 C5 -179.2(3) . . . . ? C3 C4 C5 C6 -0.1(5) . . . . ? C4 C5 C6 C7 -0.7(5) . . . . ? C5 C6 C7 C8 -0.1(4) . . . . ? C5 C6 C7 C12 -174.4(3) . . . . ? C4 C3 C8 C7 -2.6(4) . . . . ? C9 C3 C8 C7 178.4(2) . . . . ? C4 C3 C8 N1 176.0(2) . . . . ? C9 C3 C8 N1 -3.0(4) . . . . ? C6 C7 C8 C3 1.8(4) . . . . ? C12 C7 C8 C3 175.9(2) . . . . ? C6 C7 C8 N1 -176.8(2) . . . . ? C12 C7 C8 N1 -2.8(4) . . . . ? C1 N1 C8 C3 -63.7(3) . . . . ? Cr1 N1 C8 C3 114.4(2) . . . . ? C1 N1 C8 C7 114.9(3) . . . . ? Cr1 N1 C8 C7 -67.0(3) . . . . ? C4 C3 C9 C11 56.6(4) . . . . ? C8 C3 C9 C11 -124.4(3) . . . . ? C4 C3 C9 C10 -66.3(3) . . . . ? C8 C3 C9 C10 112.7(3) . . . . ? C6 C7 C12 C13 81.2(3) . . . . ? C8 C7 C12 C13 -92.7(3) . . . . ? C6 C7 C12 C14 -44.0(4) . . . . ? C8 C7 C12 C14 142.0(3) . . . . ? C20 C15 C16 C17 0.7(5) . . . . ? C21 C15 C16 C17 -175.5(3) . . . . ? C15 C16 C17 C18 0.5(6) . . . . ? C16 C17 C18 C19 -0.6(6) . . . . ? C17 C18 C19 C20 -0.6(5) . . . . ? C17 C18 C19 C24 178.4(3) . . . . ? C18 C19 C20 C15 1.9(4) . . . . ? C24 C19 C20 C15 -177.1(3) . . . . ? C18 C19 C20 N2 178.4(3) . . . . ? C24 C19 C20 N2 -0.5(4) . . . . ? C16 C15 C20 C19 -1.9(4) . . . . ? C21 C15 C20 C19 174.2(3) . . . . ? C16 C15 C20 N2 -178.6(3) . . . . ? C21 C15 C20 N2 -2.5(4) . . . . ? C2 N2 C20 C19 -81.4(3) . . . . ? Cr2 N2 C20 C19 87.7(3) . . . . ? C2 N2 C20 C15 95.3(3) . . . . ? Cr2 N2 C20 C15 -95.6(3) . . . . ? C16 C15 C21 C23 95.6(4) . . . . ? C20 C15 C21 C23 -80.4(4) . . . . ? C16 C15 C21 C22 -28.0(4) . . . . ? C20 C15 C21 C22 156.0(3) . . . . ? C20 C19 C24 C25 98.1(4) . . . . ? C18 C19 C24 C25 -80.8(4) . . . . ? C20 C19 C24 C26 -140.2(3) . . . . ? C18 C19 C24 C26 40.9(4) . . . . ? C34 N3 C27 C28 163.4(3) . . . . ? Cr2 N3 C27 C28 -24.4(4) . . . . ? N3 C27 C28 N4 -2.7(5) . . . . ? C46 N4 C28 C27 -171.7(3) . . . . ? Cr1 N4 C28 C27 7.3(4) . . . . ? C34 C29 C30 C31 0.7(4) . . . . ? C35 C29 C30 C31 179.2(3) . . . . ? C29 C30 C31 C32 -0.1(5) . . . . ? C30 C31 C32 C33 -0.2(5) . . . . ? C31 C32 C33 C34 -0.2(4) . . . . ? C31 C32 C33 C38 -175.5(3) . . . . ? C30 C29 C34 C33 -1.1(4) . . . . ? C35 C29 C34 C33 -179.5(3) . . . . ? C30 C29 C34 N3 175.2(2) . . . . ? C35 C29 C34 N3 -3.2(4) . . . . ? C32 C33 C34 C29 0.8(4) . . . . ? C38 C33 C34 C29 176.0(3) . . . . ? C32 C33 C34 N3 -175.4(2) . . . . ? C38 C33 C34 N3 -0.2(4) . . . . ? C27 N3 C34 C29 -71.8(3) . . . . ? Cr2 N3 C34 C29 116.4(2) . . . . ? C27 N3 C34 C33 104.5(3) . . . . ? Cr2 N3 C34 C33 -67.3(3) . . . . ? C30 C29 C35 C36 60.1(4) . . . . ? C34 C29 C35 C36 -121.5(3) . . . . ? C30 C29 C35 C37 -63.7(4) . . . . ? C34 C29 C35 C37 114.7(3) . . . . ? C32 C33 C38 C39 -48.7(4) . . . . ? C34 C33 C38 C39 136.2(3) . . . . ? C32 C33 C38 C40 76.3(4) . . . . ? C34 C33 C38 C40 -98.8(4) . . . . ? C46 C41 C42 C43 0.8(4) . . . . ? C47 C41 C42 C43 -176.0(3) . . . . ? C41 C42 C43 C44 -0.7(5) . . . . ? C42 C43 C44 C45 0.3(5) . . . . ? C43 C44 C45 C46 -0.1(5) . . . . ? C43 C44 C45 C50 178.5(3) . . . . ? C44 C45 C46 C41 0.2(4) . . . . ? C50 C45 C46 C41 -178.3(3) . . . . ? C44 C45 C46 N4 177.5(2) . . . . ? C50 C45 C46 N4 -1.0(4) . . . . ? C42 C41 C46 C45 -0.6(4) . . . . ? C47 C41 C46 C45 176.2(3) . . . . ? C42 C41 C46 N4 -177.9(2) . . . . ? C47 C41 C46 N4 -1.1(4) . . . . ? C28 N4 C46 C45 -83.4(3) . . . . ? Cr1 N4 C46 C45 97.5(2) . . . . ? C28 N4 C46 C41 93.9(3) . . . . ? Cr1 N4 C46 C41 -85.2(3) . . . . ? C42 C41 C47 C49 -34.3(4) . . . . ? C46 C41 C47 C49 149.1(3) . . . . ? C42 C41 C47 C48 89.6(3) . . . . ? C46 C41 C47 C48 -87.1(3) . . . . ? C44 C45 C50 C52 -62.9(4) . . . . ? C46 C45 C50 C52 115.6(3) . . . . ? C44 C45 C50 C51 61.4(4) . . . . ? C46 C45 C50 C51 -120.0(4) . . . . ? C53 C54 C55 C56 -104.6(5) . . . . ? C53 C54 C55 Cr2 106.1(4) . . . . ? N2 Cr2 C55 C56 -68.8(2) . . . . ? Cr1 Cr2 C55 C56 35.85(17) . . . . ? N3 Cr2 C55 C56 139.22(18) . . . . ? N2 Cr2 C55 C54 90.4(3) . . . . ? Cr1 Cr2 C55 C54 -164.9(3) . . . . ? N3 Cr2 C55 C54 -61.5(3) . . . . ? C56 Cr2 C55 C54 159.3(4) . . . . ? C54 C55 C56 C57 -18.7(7) . . . . ? Cr2 C55 C56 C57 140.9(4) . . . . ? C54 C55 C56 Cr1 166.2(3) . . . . ? Cr2 C55 C56 Cr1 -34.22(14) . . . . ? C54 C55 C56 Cr2 -159.6(4) . . . . ? N4 Cr1 C56 C55 -59.1(2) . . . . ? N1 Cr1 C56 C55 138.8(2) . . . . ? Cr2 Cr1 C56 C55 37.90(19) . . . . ? N4 Cr1 C56 C57 125.2(3) . . . . ? N1 Cr1 C56 C57 -37.0(3) . . . . ? Cr2 Cr1 C56 C57 -137.8(3) . . . . ? N4 Cr1 C56 Cr2 -97.00(8) . . . . ? N1 Cr1 C56 Cr2 100.86(8) . . . . ? N2 Cr2 C56 C55 123.21(18) . . . . ? Cr1 Cr2 C56 C55 -137.2(2) . . . . ? N3 Cr2 C56 C55 -57.3(2) . . . . ? N2 Cr2 C56 C57 -1.7(4) . . . . ? Cr1 Cr2 C56 C57 97.9(4) . . . . ? N3 Cr2 C56 C57 177.8(4) . . . . ? C55 Cr2 C56 C57 -125.0(5) . . . . ? N2 Cr2 C56 Cr1 -99.59(8) . . . . ? N3 Cr2 C56 Cr1 79.92(12) . . . . ? C55 Cr2 C56 Cr1 137.2(2) . . . . ? C55 C56 C57 C58 7.2(7) . . . . ? Cr1 C56 C57 C58 -178.5(3) . . . . ? Cr2 C56 C57 C58 108.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.356 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.098 data_klat844 _database_code_depnum_ccdc_archive 'CCDC 839345' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H92 Cr2 N4 O' _chemical_formula_weight 1013.40 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' 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 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 18.701(3) _cell_length_b 13.666(2) _cell_length_c 23.540(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.455(3) _cell_angle_gamma 90.00 _cell_volume 5896.2(16) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 1002 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 17.75 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.142 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 0.410 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9244 _exptl_absorpt_correction_T_max 0.9594 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _diffrn_ambient_temperature 200(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 AXS APEX diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 836.6 _diffrn_reflns_number 74695 _diffrn_reflns_av_R_equivalents 0.1052 _diffrn_reflns_av_sigmaI/netI 0.0777 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.50 _reflns_number_total 13530 _reflns_number_gt 7691 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2001)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _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^)+(0.0853P)^2^+23.2289P] 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 13530 _refine_ls_number_parameters 642 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1473 _refine_ls_R_factor_gt 0.0903 _refine_ls_wR_factor_ref 0.2696 _refine_ls_wR_factor_gt 0.2374 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Cr1 Cr 0.25863(4) 0.14104(6) 0.26796(4) 0.0347(2) Uani 1 1 d . . . Cr2 Cr 0.25181(4) 0.28213(6) 0.26521(4) 0.0317(2) Uani 1 1 d . . . N1 N 0.3465(2) 0.3260(3) 0.3071(2) 0.0355(10) Uani 1 1 d . . . N2 N 0.3603(2) 0.1179(3) 0.27723(18) 0.0308(9) Uani 1 1 d . . . N3 N 0.1568(2) 0.3098(3) 0.2811(2) 0.0350(10) Uani 1 1 d . . . N4 N 0.1776(2) 0.0976(3) 0.29888(18) 0.0325(9) Uani 1 1 d . . . O1 O 0.1918(5) 0.7196(7) 0.0435(3) 0.126(3) Uani 1 1 d D . . C1 C 0.4102(3) 0.2783(4) 0.3044(2) 0.0372(12) Uani 1 1 d . . . H1 H 0.4538 0.3156 0.3136 0.045 Uiso 1 1 calc R . . C2 C 0.4172(3) 0.1837(4) 0.2899(2) 0.0397(12) Uani 1 1 d . . . H2 H 0.4648 0.1607 0.2884 0.048 Uiso 1 1 calc R . . C3 C 0.3853(3) 0.4114(4) 0.3998(3) 0.0476(14) Uani 1 1 d . . . C4 C 0.3980(4) 0.4987(5) 0.4313(3) 0.0611(18) Uani 1 1 d . . . H4 H 0.4185 0.4966 0.4716 0.073 Uiso 1 1 calc R . . C5 C 0.3810(4) 0.5883(5) 0.4044(4) 0.070(2) Uani 1 1 d . . . H5 H 0.3886 0.6469 0.4265 0.084 Uiso 1 1 calc R . . C6 C 0.3533(4) 0.5927(4) 0.3463(4) 0.064(2) Uani 1 1 d . . . H6 H 0.3417 0.6545 0.3283 0.077 Uiso 1 1 calc R . . C7 C 0.3417(3) 0.5068(4) 0.3123(3) 0.0513(16) Uani 1 1 d . . . C8 C 0.3578(3) 0.4160(4) 0.3404(3) 0.0425(13) Uani 1 1 d . . . C9 C 0.3202(3) 0.5137(4) 0.2471(3) 0.0577(18) Uani 1 1 d . . . H9 H 0.2946 0.4515 0.2328 0.069 Uiso 1 1 calc R . . C10 C 0.3881(4) 0.5204(5) 0.2213(3) 0.0659(19) Uani 1 1 d . . . H10A H 0.4133 0.5821 0.2331 0.099 Uiso 1 1 calc R . . H10B H 0.3743 0.5179 0.1789 0.099 Uiso 1 1 calc R . . H10C H 0.4205 0.4654 0.2352 0.099 Uiso 1 1 calc R . . C11 C 0.2658(4) 0.6007(5) 0.2263(4) 0.075(2) Uani 1 1 d . . . H11A H 0.2901 0.6631 0.2379 0.113 Uiso 1 1 calc R . . H11B H 0.2228 0.5943 0.2441 0.113 Uiso 1 1 calc R . . H11C H 0.2505 0.5987 0.1840 0.113 Uiso 1 1 calc R . . C12 C 0.4040(4) 0.3153(5) 0.4320(3) 0.0562(16) Uani 1 1 d . . . H12 H 0.3898 0.2610 0.4036 0.067 Uiso 1 1 calc R . . C13 C 0.4858(5) 0.3065(6) 0.4560(4) 0.094(3) Uani 1 1 d . . . H13A H 0.5123 0.3109 0.4240 0.141 Uiso 1 1 calc R . . H13B H 0.4962 0.2434 0.4756 0.141 Uiso 1 1 calc R . . H13C H 0.5016 0.3596 0.4836 0.141 Uiso 1 1 calc R . . C14 C 0.3615(6) 0.3018(7) 0.4809(4) 0.105(3) Uani 1 1 d . . . H14A H 0.3732 0.3554 0.5088 0.158 Uiso 1 1 calc R . . H14B H 0.3750 0.2393 0.5005 0.158 Uiso 1 1 calc R . . H14C H 0.3090 0.3021 0.4646 0.158 Uiso 1 1 calc R . . C15 C 0.4016(3) -0.0437(4) 0.3197(3) 0.0447(14) Uani 1 1 d . . . C16 C 0.4229(4) -0.1393(5) 0.3111(4) 0.0618(19) Uani 1 1 d . . . H16 H 0.4360 -0.1814 0.3436 0.074 Uiso 1 1 calc R . . C17 C 0.4254(4) -0.1742(4) 0.2570(4) 0.0613(19) Uani 1 1 d . . . H17 H 0.4387 -0.2403 0.2521 0.074 Uiso 1 1 calc R . . C18 C 0.4086(3) -0.1133(4) 0.2096(3) 0.0536(16) Uani 1 1 d . . . H18 H 0.4111 -0.1379 0.1723 0.064 Uiso 1 1 calc R . . C19 C 0.3878(3) -0.0160(4) 0.2153(3) 0.0406(13) Uani 1 1 d . . . C20 C 0.3827(3) 0.0176(4) 0.2703(2) 0.0360(12) Uani 1 1 d . . . C21 C 0.4040(4) -0.0069(5) 0.3809(3) 0.0600(18) Uani 1 1 d . . . H21 H 0.3688 0.0488 0.3784 0.072 Uiso 1 1 calc R . . C22 C 0.4785(5) 0.0317(6) 0.4081(3) 0.083(3) Uani 1 1 d . . . H22A H 0.5142 -0.0215 0.4115 0.125 Uiso 1 1 calc R . . H22B H 0.4775 0.0579 0.4466 0.125 Uiso 1 1 calc R . . H22C H 0.4922 0.0838 0.3837 0.125 Uiso 1 1 calc R . . C23 C 0.3813(4) -0.0835(7) 0.4205(3) 0.081(2) Uani 1 1 d . . . H23A H 0.4201 -0.1324 0.4304 0.121 Uiso 1 1 calc R . . H23B H 0.3364 -0.1155 0.4007 0.121 Uiso 1 1 calc R . . H23C H 0.3729 -0.0521 0.4560 0.121 Uiso 1 1 calc R . . C24 C 0.3769(3) 0.0501(5) 0.1625(3) 0.0459(14) Uani 1 1 d . . . H24 H 0.3516 0.1108 0.1717 0.055 Uiso 1 1 calc R . . C25 C 0.4505(4) 0.0798(6) 0.1497(3) 0.0666(19) Uani 1 1 d . . . H25A H 0.4792 0.0210 0.1458 0.100 Uiso 1 1 calc R . . H25B H 0.4767 0.1201 0.1816 0.100 Uiso 1 1 calc R . . H25C H 0.4431 0.1174 0.1136 0.100 Uiso 1 1 calc R . . C26 C 0.3298(5) 0.0029(7) 0.1095(3) 0.090(3) Uani 1 1 d . . . H26A H 0.3550 -0.0543 0.0980 0.135 Uiso 1 1 calc R . . H26B H 0.3207 0.0502 0.0776 0.135 Uiso 1 1 calc R . . H26C H 0.2832 -0.0175 0.1189 0.135 Uiso 1 1 calc R . . C27 C 0.1041(3) 0.2439(4) 0.2910(2) 0.0393(12) Uani 1 1 d . . . H27 H 0.0569 0.2690 0.2916 0.047 Uiso 1 1 calc R . . C28 C 0.1147(3) 0.1465(4) 0.2999(2) 0.0400(12) Uani 1 1 d . . . H28 H 0.0747 0.1094 0.3075 0.048 Uiso 1 1 calc R . . C29 C 0.1000(3) 0.4521(4) 0.2237(3) 0.0456(14) Uani 1 1 d . . . C30 C 0.0748(3) 0.5486(4) 0.2226(4) 0.0591(18) Uani 1 1 d . . . H30 H 0.0544 0.5784 0.1865 0.071 Uiso 1 1 calc R . . C31 C 0.0792(3) 0.6006(5) 0.2731(4) 0.066(2) Uani 1 1 d . . . H31 H 0.0614 0.6658 0.2716 0.080 Uiso 1 1 calc R . . C32 C 0.1092(4) 0.5594(5) 0.3257(4) 0.063(2) Uani 1 1 d . . . H32 H 0.1116 0.5965 0.3602 0.076 Uiso 1 1 calc R . . C33 C 0.1361(3) 0.4638(4) 0.3291(3) 0.0480(15) Uani 1 1 d . . . C34 C 0.1307(3) 0.4105(4) 0.2778(3) 0.0390(12) Uani 1 1 d . . . C35 C 0.0863(3) 0.3937(5) 0.1679(3) 0.0537(16) Uani 1 1 d . . . H35 H 0.1218 0.3382 0.1728 0.064 Uiso 1 1 calc R . . C36 C 0.0975(4) 0.4539(6) 0.1154(3) 0.076(2) Uani 1 1 d . . . H36A H 0.0571 0.5001 0.1045 0.114 Uiso 1 1 calc R . . H36B H 0.0991 0.4099 0.0828 0.114 Uiso 1 1 calc R . . H36C H 0.1436 0.4900 0.1252 0.114 Uiso 1 1 calc R . . C37 C 0.0093(4) 0.3504(6) 0.1569(3) 0.070(2) Uani 1 1 d . . . H37A H 0.0030 0.3113 0.1904 0.105 Uiso 1 1 calc R . . H37B H 0.0023 0.3086 0.1223 0.105 Uiso 1 1 calc R . . H37C H -0.0266 0.4034 0.1507 0.105 Uiso 1 1 calc R . . C38 C 0.1654(4) 0.4201(5) 0.3886(3) 0.0582(17) Uani 1 1 d . . . H38 H 0.1995 0.3660 0.3833 0.070 Uiso 1 1 calc R . . C39 C 0.2084(4) 0.4930(6) 0.4311(4) 0.083(3) Uani 1 1 d . . . H39A H 0.2453 0.5249 0.4132 0.125 Uiso 1 1 calc R . . H39B H 0.2325 0.4584 0.4662 0.125 Uiso 1 1 calc R . . H39C H 0.1752 0.5424 0.4413 0.125 Uiso 1 1 calc R . . C40 C 0.1043(5) 0.3751(6) 0.4147(3) 0.085(3) Uani 1 1 d . . . H40A H 0.0709 0.4268 0.4220 0.127 Uiso 1 1 calc R . . H40B H 0.1255 0.3425 0.4513 0.127 Uiso 1 1 calc R . . H40C H 0.0775 0.3272 0.3876 0.127 Uiso 1 1 calc R . . C41 C 0.1815(3) -0.0830(4) 0.2917(3) 0.0401(13) Uani 1 1 d . . . C42 C 0.1857(3) -0.1737(4) 0.3192(3) 0.0520(15) Uani 1 1 d . . . H42 H 0.1871 -0.2316 0.2972 0.062 Uiso 1 1 calc R . . C43 C 0.1880(4) -0.1805(5) 0.3778(3) 0.0575(17) Uani 1 1 d . . . H43 H 0.1908 -0.2431 0.3957 0.069 Uiso 1 1 calc R . . C44 C 0.1864(3) -0.0984(5) 0.4105(3) 0.0532(16) Uani 1 1 d . . . H44 H 0.1866 -0.1047 0.4507 0.064 Uiso 1 1 calc R . . C45 C 0.1846(3) -0.0054(4) 0.3857(3) 0.0446(13) Uani 1 1 d . . . C46 C 0.1810(3) 0.0021(4) 0.3259(2) 0.0370(12) Uani 1 1 d . . . C47 C 0.1684(3) -0.0776(4) 0.2263(3) 0.0422(13) Uani 1 1 d . . . H47 H 0.1883 -0.0134 0.2162 0.051 Uiso 1 1 calc R . . C48 C 0.2067(4) -0.1566(5) 0.1982(3) 0.0609(18) Uani 1 1 d . . . H48A H 0.2582 -0.1596 0.2175 0.091 Uiso 1 1 calc R . . H48B H 0.2033 -0.1412 0.1570 0.091 Uiso 1 1 calc R . . H48C H 0.1835 -0.2199 0.2018 0.091 Uiso 1 1 calc R . . C49 C 0.0874(4) -0.0768(6) 0.2007(3) 0.0651(19) Uani 1 1 d . . . H49A H 0.0657 -0.1389 0.2095 0.098 Uiso 1 1 calc R . . H49B H 0.0799 -0.0684 0.1586 0.098 Uiso 1 1 calc R . . H49C H 0.0641 -0.0226 0.2175 0.098 Uiso 1 1 calc R . . C50 C 0.1832(4) 0.0835(5) 0.4246(3) 0.0533(16) Uani 1 1 d . . . H50 H 0.1882 0.1431 0.4011 0.064 Uiso 1 1 calc R . . C51 C 0.2480(5) 0.0828(6) 0.4770(3) 0.080(2) Uani 1 1 d . . . H51A H 0.2444 0.0253 0.5011 0.119 Uiso 1 1 calc R . . H51B H 0.2467 0.1423 0.5000 0.119 Uiso 1 1 calc R . . H51C H 0.2940 0.0803 0.4631 0.119 Uiso 1 1 calc R . . C52 C 0.1118(5) 0.0923(6) 0.4462(4) 0.078(2) Uani 1 1 d . . . H52A H 0.0710 0.0961 0.4129 0.117 Uiso 1 1 calc R . . H52B H 0.1129 0.1515 0.4697 0.117 Uiso 1 1 calc R . . H52C H 0.1057 0.0348 0.4696 0.117 Uiso 1 1 calc R . . C53 C 0.3507(4) 0.3161(5) 0.1267(4) 0.072(2) Uani 1 1 d . . . H53A H 0.3848 0.3174 0.1641 0.108 Uiso 1 1 calc R . . H53B H 0.3634 0.3683 0.1019 0.108 Uiso 1 1 calc R . . H53C H 0.3539 0.2527 0.1079 0.108 Uiso 1 1 calc R . . C54 C 0.2752(4) 0.3313(5) 0.1358(3) 0.0573(16) Uani 1 1 d . . . H54A H 0.2404 0.3180 0.0991 0.069 Uiso 1 1 calc R . . H54B H 0.2693 0.4006 0.1464 0.069 Uiso 1 1 calc R . . C55 C 0.2575(3) 0.2661(4) 0.1829(3) 0.0460(14) Uani 1 1 d . . . C56 C 0.2181(3) 0.1859(5) 0.1845(3) 0.0491(15) Uani 1 1 d . . . C57 C 0.1584(4) 0.1404(6) 0.1422(4) 0.086(3) Uani 1 1 d . . . H57A H 0.1711 0.0703 0.1401 0.103 Uiso 1 1 calc R . . H57B H 0.1144 0.1432 0.1595 0.103 Uiso 1 1 calc R . . C58 C 0.1378(8) 0.1723(9) 0.0862(5) 0.153(5) Uani 1 1 d . . . H58A H 0.1343 0.2438 0.0857 0.229 Uiso 1 1 calc R . . H58B H 0.0902 0.1442 0.0690 0.229 Uiso 1 1 calc R . . H58C H 0.1740 0.1516 0.0638 0.229 Uiso 1 1 calc R . . C59 C 0.0649(8) 0.7292(16) 0.0313(8) 0.224(10) Uani 1 1 d D . . H59A H 0.0541 0.6728 0.0053 0.336 Uiso 1 1 calc R . . H59B H 0.0300 0.7818 0.0178 0.336 Uiso 1 1 calc R . . H59C H 0.0609 0.7099 0.0706 0.336 Uiso 1 1 calc R . . C60 C 0.1285(9) 0.7588(11) 0.0315(6) 0.162(6) Uani 1 1 d D . . H60A H 0.1333 0.8173 0.0568 0.194 Uiso 1 1 calc R . . H60B H 0.1255 0.7845 -0.0083 0.194 Uiso 1 1 calc R . . C61 C 0.2568(8) 0.7452(12) 0.0477(7) 0.180(8) Uani 1 1 d D . . H61A H 0.2615 0.8022 0.0742 0.216 Uiso 1 1 calc R . . H61B H 0.2580 0.7727 0.0090 0.216 Uiso 1 1 calc R . . C62 C 0.3186(8) 0.7022(13) 0.0621(8) 0.193(9) Uani 1 1 d D . . H62A H 0.3367 0.7092 0.1039 0.290 Uiso 1 1 calc R . . H62B H 0.3535 0.7319 0.0412 0.290 Uiso 1 1 calc R . . H62C H 0.3130 0.6326 0.0522 0.290 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 Cr1 0.0288(4) 0.0255(4) 0.0508(5) -0.0058(4) 0.0107(4) -0.0012(3) Cr2 0.0290(4) 0.0252(4) 0.0412(5) 0.0015(4) 0.0077(3) 0.0005(3) N1 0.032(2) 0.023(2) 0.050(3) 0.0001(19) 0.0043(19) -0.0022(17) N2 0.028(2) 0.028(2) 0.037(2) 0.0015(17) 0.0059(17) 0.0005(16) N3 0.032(2) 0.026(2) 0.049(3) -0.0010(18) 0.0117(19) -0.0003(17) N4 0.033(2) 0.025(2) 0.040(2) -0.0016(18) 0.0083(18) -0.0008(17) O1 0.092(5) 0.170(8) 0.124(6) -0.070(6) 0.040(5) -0.027(5) C1 0.028(2) 0.034(3) 0.049(3) 0.001(2) 0.006(2) -0.004(2) C2 0.031(3) 0.036(3) 0.052(3) 0.002(2) 0.010(2) 0.002(2) C3 0.041(3) 0.045(3) 0.058(4) -0.010(3) 0.013(3) -0.010(3) C4 0.057(4) 0.053(4) 0.074(5) -0.025(4) 0.014(3) -0.017(3) C5 0.060(4) 0.048(4) 0.103(6) -0.033(4) 0.019(4) -0.014(3) C6 0.052(4) 0.025(3) 0.113(7) -0.015(3) 0.010(4) -0.005(3) C7 0.035(3) 0.035(3) 0.083(5) -0.008(3) 0.009(3) -0.004(2) C8 0.030(3) 0.033(3) 0.064(4) -0.010(3) 0.008(3) -0.004(2) C9 0.045(3) 0.025(3) 0.097(5) 0.009(3) 0.000(3) -0.003(2) C10 0.058(4) 0.056(4) 0.082(5) -0.001(4) 0.010(4) 0.001(3) C11 0.065(5) 0.063(5) 0.091(6) 0.025(4) -0.002(4) -0.022(4) C12 0.064(4) 0.054(4) 0.047(4) -0.010(3) 0.004(3) -0.013(3) C13 0.083(6) 0.067(5) 0.115(7) -0.001(5) -0.023(5) -0.002(4) C14 0.156(10) 0.091(7) 0.074(6) 0.000(5) 0.038(6) -0.019(7) C15 0.036(3) 0.036(3) 0.063(4) 0.010(3) 0.012(3) 0.004(2) C16 0.052(4) 0.036(3) 0.101(6) 0.020(4) 0.023(4) 0.009(3) C17 0.050(4) 0.027(3) 0.110(6) -0.008(4) 0.024(4) 0.005(3) C18 0.045(3) 0.039(3) 0.079(5) -0.020(3) 0.016(3) 0.004(3) C19 0.034(3) 0.036(3) 0.052(3) -0.008(3) 0.009(2) 0.005(2) C20 0.031(3) 0.029(3) 0.051(3) 0.001(2) 0.014(2) 0.003(2) C21 0.072(5) 0.058(4) 0.053(4) 0.019(3) 0.021(3) 0.024(4) C22 0.109(7) 0.075(5) 0.058(5) 0.008(4) -0.001(5) -0.014(5) C23 0.069(5) 0.108(7) 0.066(5) 0.039(5) 0.016(4) 0.015(5) C24 0.043(3) 0.053(3) 0.045(3) -0.005(3) 0.016(3) 0.008(3) C25 0.049(4) 0.075(5) 0.078(5) 0.017(4) 0.019(4) 0.006(3) C26 0.096(6) 0.120(8) 0.047(4) -0.009(5) 0.000(4) -0.033(6) C27 0.029(3) 0.038(3) 0.053(3) 0.000(2) 0.010(2) -0.001(2) C28 0.031(3) 0.036(3) 0.054(3) 0.001(3) 0.012(2) -0.002(2) C29 0.030(3) 0.036(3) 0.073(4) 0.016(3) 0.013(3) 0.007(2) C30 0.043(3) 0.035(3) 0.098(6) 0.013(3) 0.011(3) 0.010(3) C31 0.039(3) 0.038(3) 0.118(7) -0.004(4) 0.005(4) 0.011(3) C32 0.050(4) 0.038(3) 0.104(6) -0.028(4) 0.022(4) -0.004(3) C33 0.035(3) 0.038(3) 0.071(4) -0.016(3) 0.010(3) 0.001(2) C34 0.029(3) 0.028(3) 0.060(4) 0.000(2) 0.010(2) 0.003(2) C35 0.047(3) 0.055(4) 0.058(4) 0.020(3) 0.008(3) 0.019(3) C36 0.069(5) 0.094(6) 0.067(5) 0.032(4) 0.018(4) 0.015(4) C37 0.060(4) 0.072(5) 0.075(5) -0.005(4) 0.008(4) -0.006(4) C38 0.057(4) 0.059(4) 0.059(4) -0.021(3) 0.012(3) 0.006(3) C39 0.070(5) 0.094(6) 0.083(6) -0.049(5) 0.012(4) -0.007(4) C40 0.108(7) 0.080(6) 0.064(5) -0.004(4) 0.012(5) -0.024(5) C41 0.035(3) 0.029(3) 0.057(4) 0.003(2) 0.012(3) -0.003(2) C42 0.056(4) 0.030(3) 0.071(4) 0.003(3) 0.012(3) -0.006(3) C43 0.063(4) 0.035(3) 0.072(5) 0.019(3) 0.006(3) 0.001(3) C44 0.054(4) 0.052(4) 0.052(4) 0.014(3) 0.008(3) -0.006(3) C45 0.046(3) 0.042(3) 0.047(3) 0.006(3) 0.011(3) -0.004(3) C46 0.034(3) 0.027(2) 0.051(3) 0.006(2) 0.010(2) -0.005(2) C47 0.048(3) 0.026(3) 0.054(3) -0.006(2) 0.014(3) -0.001(2) C48 0.069(4) 0.045(4) 0.072(5) -0.013(3) 0.023(4) 0.006(3) C49 0.052(4) 0.076(5) 0.064(4) -0.004(4) 0.004(3) 0.002(4) C50 0.065(4) 0.050(4) 0.046(3) 0.001(3) 0.013(3) -0.009(3) C51 0.095(6) 0.068(5) 0.065(5) -0.014(4) -0.009(4) -0.009(4) C52 0.089(6) 0.073(5) 0.082(6) -0.011(4) 0.045(5) -0.009(4) C53 0.082(5) 0.059(4) 0.086(6) 0.000(4) 0.043(5) 0.000(4) C54 0.063(4) 0.062(4) 0.047(4) 0.006(3) 0.010(3) -0.002(3) C55 0.047(3) 0.046(3) 0.044(3) 0.007(3) 0.009(3) 0.012(3) C56 0.046(3) 0.054(4) 0.051(4) 0.013(3) 0.018(3) 0.014(3) C57 0.070(5) 0.086(6) 0.083(6) 0.038(5) -0.030(4) -0.030(4) C58 0.197(14) 0.137(10) 0.092(8) -0.018(7) -0.048(8) 0.000(10) C59 0.105(11) 0.38(3) 0.193(18) -0.077(18) 0.039(12) -0.024(15) C60 0.143(13) 0.197(16) 0.141(12) -0.095(11) 0.018(11) 0.011(13) C61 0.134(13) 0.227(18) 0.183(15) -0.137(14) 0.042(12) -0.047(13) C62 0.105(11) 0.24(2) 0.238(19) -0.127(16) 0.038(12) -0.021(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 Cr1 N2 1.897(4) . ? Cr1 N4 1.902(4) . ? Cr1 Cr2 1.9325(11) . ? Cr1 C56 2.055(6) . ? Cr2 N3 1.924(4) . ? Cr2 N1 1.943(4) . ? Cr2 C55 1.975(6) . ? Cr2 C56 2.294(7) . ? N1 C1 1.370(6) . ? N1 C8 1.451(7) . ? N2 C2 1.379(6) . ? N2 C20 1.452(6) . ? N3 C27 1.389(6) . ? N3 C34 1.457(6) . ? N4 C28 1.357(6) . ? N4 C46 1.447(6) . ? O1 C61 1.250(13) . ? O1 C60 1.280(13) . ? C1 C2 1.350(7) . ? C3 C8 1.392(8) . ? C3 C4 1.400(8) . ? C3 C12 1.522(9) . ? C4 C5 1.386(10) . ? C5 C6 1.364(11) . ? C6 C7 1.412(8) . ? C7 C8 1.411(8) . ? C7 C9 1.512(10) . ? C9 C10 1.514(10) . ? C9 C11 1.578(9) . ? C12 C13 1.526(10) . ? C12 C14 1.534(11) . ? C15 C16 1.392(8) . ? C15 C20 1.419(8) . ? C15 C21 1.519(9) . ? C16 C17 1.371(10) . ? C17 C18 1.376(10) . ? C18 C19 1.399(7) . ? C19 C20 1.395(8) . ? C19 C24 1.518(8) . ? C21 C22 1.508(11) . ? C21 C23 1.517(9) . ? C24 C26 1.520(9) . ? C24 C25 1.521(8) . ? C27 C28 1.355(7) . ? C29 C30 1.399(8) . ? C29 C34 1.407(8) . ? C29 C35 1.515(9) . ? C30 C31 1.373(10) . ? C31 C32 1.375(11) . ? C32 C33 1.397(8) . ? C33 C34 1.398(8) . ? C33 C38 1.520(9) . ? C35 C36 1.534(9) . ? C35 C37 1.530(9) . ? C38 C39 1.523(9) . ? C38 C40 1.530(10) . ? C41 C42 1.394(8) . ? C41 C46 1.415(7) . ? C41 C47 1.513(8) . ? C42 C43 1.374(9) . ? C43 C44 1.364(9) . ? C44 C45 1.396(8) . ? C45 C46 1.401(8) . ? C45 C50 1.525(8) . ? C47 C49 1.515(8) . ? C47 C48 1.518(8) . ? C50 C52 1.524(9) . ? C50 C51 1.547(9) . ? C53 C54 1.485(9) . ? C54 C55 1.509(8) . ? C55 C56 1.324(8) . ? C56 C57 1.478(9) . ? C57 C58 1.369(12) . ? C59 C60 1.255(15) . ? C61 C62 1.281(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 N2 Cr1 N4 139.54(18) . . ? N2 Cr1 Cr2 103.17(12) . . ? N4 Cr1 Cr2 105.77(13) . . ? N2 Cr1 C56 109.3(2) . . ? N4 Cr1 C56 106.8(2) . . ? Cr2 Cr1 C56 70.16(19) . . ? N3 Cr2 Cr1 104.30(13) . . ? N3 Cr2 N1 128.62(19) . . ? Cr1 Cr2 N1 104.10(13) . . ? N3 Cr2 C55 116.4(2) . . ? Cr1 Cr2 C55 84.61(18) . . ? N1 Cr2 C55 108.2(2) . . ? N3 Cr2 C56 99.3(2) . . ? Cr1 Cr2 C56 57.42(15) . . ? N1 Cr2 C56 132.1(2) . . ? C55 Cr2 C56 35.1(2) . . ? C1 N1 C8 113.3(4) . . ? C1 N1 Cr2 122.8(3) . . ? C8 N1 Cr2 123.8(3) . . ? C2 N2 C20 114.3(4) . . ? C2 N2 Cr1 129.0(3) . . ? C20 N2 Cr1 116.7(3) . . ? C27 N3 C34 112.3(4) . . ? C27 N3 Cr2 128.2(3) . . ? C34 N3 Cr2 119.2(3) . . ? C28 N4 C46 113.6(4) . . ? C28 N4 Cr1 127.7(4) . . ? C46 N4 Cr1 118.7(3) . . ? C61 O1 C60 138.0(15) . . ? C2 C1 N1 126.6(5) . . ? C1 C2 N2 124.7(5) . . ? C8 C3 C4 119.0(6) . . ? C8 C3 C12 122.8(5) . . ? C4 C3 C12 118.2(6) . . ? C5 C4 C3 120.7(7) . . ? C6 C5 C4 120.3(6) . . ? C5 C6 C7 121.0(7) . . ? C8 C7 C6 118.1(7) . . ? C8 C7 C9 121.3(5) . . ? C6 C7 C9 120.2(6) . . ? C3 C8 C7 120.8(5) . . ? C3 C8 N1 119.3(5) . . ? C7 C8 N1 119.9(5) . . ? C10 C9 C7 109.6(5) . . ? C10 C9 C11 111.8(6) . . ? C7 C9 C11 112.8(6) . . ? C3 C12 C13 111.5(6) . . ? C3 C12 C14 112.1(6) . . ? C13 C12 C14 110.2(7) . . ? C16 C15 C20 117.8(6) . . ? C16 C15 C21 119.6(6) . . ? C20 C15 C21 122.5(5) . . ? C17 C16 C15 121.7(6) . . ? C16 C17 C18 119.8(6) . . ? C17 C18 C19 121.4(6) . . ? C20 C19 C18 118.2(6) . . ? C20 C19 C24 122.8(5) . . ? C18 C19 C24 118.8(5) . . ? C19 C20 C15 121.0(5) . . ? C19 C20 N2 119.3(5) . . ? C15 C20 N2 119.7(5) . . ? C22 C21 C15 111.5(6) . . ? C22 C21 C23 109.2(6) . . ? C15 C21 C23 113.3(6) . . ? C26 C24 C19 112.4(6) . . ? C26 C24 C25 110.6(6) . . ? C19 C24 C25 109.9(5) . . ? C28 C27 N3 125.2(5) . . ? C27 C28 N4 125.5(5) . . ? C30 C29 C34 118.3(6) . . ? C30 C29 C35 118.7(6) . . ? C34 C29 C35 122.6(5) . . ? C31 C30 C29 120.6(7) . . ? C32 C31 C30 120.8(6) . . ? C31 C32 C33 120.8(7) . . ? C32 C33 C34 118.3(6) . . ? C32 C33 C38 118.7(6) . . ? C34 C33 C38 122.8(5) . . ? C33 C34 C29 121.1(5) . . ? C33 C34 N3 118.7(5) . . ? C29 C34 N3 120.2(5) . . ? C29 C35 C36 113.0(6) . . ? C29 C35 C37 110.1(5) . . ? C36 C35 C37 110.2(6) . . ? C33 C38 C39 113.3(6) . . ? C33 C38 C40 111.5(6) . . ? C39 C38 C40 109.7(6) . . ? C42 C41 C46 118.2(6) . . ? C42 C41 C47 120.0(5) . . ? C46 C41 C47 121.4(5) . . ? C43 C42 C41 121.0(6) . . ? C44 C43 C42 120.7(6) . . ? C43 C44 C45 121.0(6) . . ? C44 C45 C46 118.7(6) . . ? C44 C45 C50 118.5(6) . . ? C46 C45 C50 122.8(5) . . ? C45 C46 C41 120.4(5) . . ? C45 C46 N4 119.8(5) . . ? C41 C46 N4 119.7(5) . . ? C41 C47 C49 110.6(5) . . ? C41 C47 C48 114.4(5) . . ? C49 C47 C48 110.7(5) . . ? C45 C50 C52 112.5(5) . . ? C45 C50 C51 111.7(6) . . ? C52 C50 C51 109.6(6) . . ? C53 C54 C55 112.2(6) . . ? C56 C55 C54 135.6(6) . . ? C56 C55 Cr2 85.7(4) . . ? C54 C55 Cr2 135.8(5) . . ? C55 C56 C57 132.7(6) . . ? C55 C56 Cr1 100.0(5) . . ? C57 C56 Cr1 127.2(5) . . ? C55 C56 Cr2 59.1(4) . . ? C57 C56 Cr2 147.8(6) . . ? Cr1 C56 Cr2 52.42(16) . . ? C58 C57 C56 123.1(8) . . ? C59 C60 O1 134.4(19) . . ? O1 C61 C62 134.8(19) . . ? 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 Cr2 N3 -161.97(19) . . . . ? N4 Cr1 Cr2 N3 -10.6(2) . . . . ? C56 Cr1 Cr2 N3 92.0(2) . . . . ? N2 Cr1 Cr2 N1 -25.2(2) . . . . ? N4 Cr1 Cr2 N1 126.2(2) . . . . ? C56 Cr1 Cr2 N1 -131.3(2) . . . . ? N2 Cr1 Cr2 C55 82.2(2) . . . . ? N4 Cr1 Cr2 C55 -126.4(2) . . . . ? C56 Cr1 Cr2 C55 -23.9(2) . . . . ? N2 Cr1 Cr2 C56 106.1(2) . . . . ? N4 Cr1 Cr2 C56 -102.5(2) . . . . ? N3 Cr2 N1 C1 158.0(4) . . . . ? Cr1 Cr2 N1 C1 36.3(4) . . . . ? C55 Cr2 N1 C1 -52.6(5) . . . . ? C56 Cr2 N1 C1 -22.3(5) . . . . ? N3 Cr2 N1 C8 -27.1(5) . . . . ? Cr1 Cr2 N1 C8 -148.9(4) . . . . ? C55 Cr2 N1 C8 122.2(4) . . . . ? C56 Cr2 N1 C8 152.5(4) . . . . ? N4 Cr1 N2 C2 -123.8(4) . . . . ? Cr2 Cr1 N2 C2 11.0(5) . . . . ? C56 Cr1 N2 C2 84.3(5) . . . . ? N4 Cr1 N2 C20 56.0(5) . . . . ? Cr2 Cr1 N2 C20 -169.2(3) . . . . ? C56 Cr1 N2 C20 -95.9(4) . . . . ? Cr1 Cr2 N3 C27 -1.3(5) . . . . ? N1 Cr2 N3 C27 -123.0(5) . . . . ? C55 Cr2 N3 C27 89.7(5) . . . . ? C56 Cr2 N3 C27 57.3(5) . . . . ? Cr1 Cr2 N3 C34 -175.0(4) . . . . ? N1 Cr2 N3 C34 63.3(5) . . . . ? C55 Cr2 N3 C34 -84.0(4) . . . . ? C56 Cr2 N3 C34 -116.5(4) . . . . ? N2 Cr1 N4 C28 155.4(4) . . . . ? Cr2 Cr1 N4 C28 21.3(5) . . . . ? C56 Cr1 N4 C28 -52.3(5) . . . . ? N2 Cr1 N4 C46 -23.5(5) . . . . ? Cr2 Cr1 N4 C46 -157.6(3) . . . . ? C56 Cr1 N4 C46 128.8(4) . . . . ? C8 N1 C1 C2 162.0(6) . . . . ? Cr2 N1 C1 C2 -22.7(8) . . . . ? N1 C1 C2 N2 -2.3(9) . . . . ? C20 N2 C2 C1 -172.4(5) . . . . ? Cr1 N2 C2 C1 7.5(8) . . . . ? C8 C3 C4 C5 2.3(9) . . . . ? C12 C3 C4 C5 -179.0(6) . . . . ? C3 C4 C5 C6 -1.7(11) . . . . ? C4 C5 C6 C7 -0.2(11) . . . . ? C5 C6 C7 C8 1.6(10) . . . . ? C5 C6 C7 C9 -172.2(6) . . . . ? C4 C3 C8 C7 -1.0(9) . . . . ? C12 C3 C8 C7 -179.5(5) . . . . ? C4 C3 C8 N1 178.2(5) . . . . ? C12 C3 C8 N1 -0.4(8) . . . . ? C6 C7 C8 C3 -0.9(9) . . . . ? C9 C7 C8 C3 172.8(5) . . . . ? C6 C7 C8 N1 179.9(5) . . . . ? C9 C7 C8 N1 -6.4(8) . . . . ? C1 N1 C8 C3 -66.6(7) . . . . ? Cr2 N1 C8 C3 118.2(5) . . . . ? C1 N1 C8 C7 112.6(6) . . . . ? Cr2 N1 C8 C7 -62.7(6) . . . . ? C8 C7 C9 C10 -86.4(7) . . . . ? C6 C7 C9 C10 87.2(7) . . . . ? C8 C7 C9 C11 148.5(5) . . . . ? C6 C7 C9 C11 -38.0(8) . . . . ? C8 C3 C12 C13 114.1(7) . . . . ? C4 C3 C12 C13 -64.5(8) . . . . ? C8 C3 C12 C14 -121.8(7) . . . . ? C4 C3 C12 C14 59.6(8) . . . . ? C20 C15 C16 C17 -0.3(9) . . . . ? C21 C15 C16 C17 -176.5(6) . . . . ? C15 C16 C17 C18 1.9(10) . . . . ? C16 C17 C18 C19 -0.9(10) . . . . ? C17 C18 C19 C20 -1.6(9) . . . . ? C17 C18 C19 C24 174.3(6) . . . . ? C18 C19 C20 C15 3.2(8) . . . . ? C24 C19 C20 C15 -172.6(5) . . . . ? C18 C19 C20 N2 -179.2(5) . . . . ? C24 C19 C20 N2 5.1(8) . . . . ? C16 C15 C20 C19 -2.2(8) . . . . ? C21 C15 C20 C19 173.8(5) . . . . ? C16 C15 C20 N2 -179.9(5) . . . . ? C21 C15 C20 N2 -3.8(8) . . . . ? C2 N2 C20 C19 -91.6(6) . . . . ? Cr1 N2 C20 C19 88.6(5) . . . . ? C2 N2 C20 C15 86.2(6) . . . . ? Cr1 N2 C20 C15 -93.7(5) . . . . ? C16 C15 C21 C22 85.9(7) . . . . ? C20 C15 C21 C22 -90.1(7) . . . . ? C16 C15 C21 C23 -37.8(8) . . . . ? C20 C15 C21 C23 146.2(6) . . . . ? C20 C19 C24 C26 -136.0(6) . . . . ? C18 C19 C24 C26 48.3(8) . . . . ? C20 C19 C24 C25 100.4(6) . . . . ? C18 C19 C24 C25 -75.3(7) . . . . ? C34 N3 C27 C28 -175.4(6) . . . . ? Cr2 N3 C27 C28 10.5(8) . . . . ? N3 C27 C28 N4 -2.0(10) . . . . ? C46 N4 C28 C27 162.9(6) . . . . ? Cr1 N4 C28 C27 -16.0(8) . . . . ? C34 C29 C30 C31 -0.8(9) . . . . ? C35 C29 C30 C31 173.1(6) . . . . ? C29 C30 C31 C32 0.7(10) . . . . ? C30 C31 C32 C33 0.2(10) . . . . ? C31 C32 C33 C34 -1.1(9) . . . . ? C31 C32 C33 C38 -177.2(6) . . . . ? C32 C33 C34 C29 1.0(8) . . . . ? C38 C33 C34 C29 176.9(5) . . . . ? C32 C33 C34 N3 -178.4(5) . . . . ? C38 C33 C34 N3 -2.4(8) . . . . ? C30 C29 C34 C33 -0.1(8) . . . . ? C35 C29 C34 C33 -173.7(5) . . . . ? C30 C29 C34 N3 179.3(5) . . . . ? C35 C29 C34 N3 5.6(8) . . . . ? C27 N3 C34 C33 85.9(6) . . . . ? Cr2 N3 C34 C33 -99.4(5) . . . . ? C27 N3 C34 C29 -93.5(6) . . . . ? Cr2 N3 C34 C29 81.2(5) . . . . ? C30 C29 C35 C36 41.0(8) . . . . ? C34 C29 C35 C36 -145.4(6) . . . . ? C30 C29 C35 C37 -82.7(7) . . . . ? C34 C29 C35 C37 91.0(7) . . . . ? C32 C33 C38 C39 -39.0(8) . . . . ? C34 C33 C38 C39 145.1(6) . . . . ? C32 C33 C38 C40 85.3(7) . . . . ? C34 C33 C38 C40 -90.6(7) . . . . ? C46 C41 C42 C43 1.2(9) . . . . ? C47 C41 C42 C43 -171.4(6) . . . . ? C41 C42 C43 C44 -0.2(10) . . . . ? C42 C43 C44 C45 -1.9(10) . . . . ? C43 C44 C45 C46 2.9(9) . . . . ? C43 C44 C45 C50 -179.7(6) . . . . ? C44 C45 C46 C41 -1.8(8) . . . . ? C50 C45 C46 C41 -179.1(5) . . . . ? C44 C45 C46 N4 178.8(5) . . . . ? C50 C45 C46 N4 1.4(8) . . . . ? C42 C41 C46 C45 -0.2(8) . . . . ? C47 C41 C46 C45 172.3(5) . . . . ? C42 C41 C46 N4 179.2(5) . . . . ? C47 C41 C46 N4 -8.2(7) . . . . ? C28 N4 C46 C45 -66.9(6) . . . . ? Cr1 N4 C46 C45 112.2(5) . . . . ? C28 N4 C46 C41 113.7(5) . . . . ? Cr1 N4 C46 C41 -67.3(6) . . . . ? C42 C41 C47 C49 88.3(7) . . . . ? C46 C41 C47 C49 -84.2(6) . . . . ? C42 C41 C47 C48 -37.6(8) . . . . ? C46 C41 C47 C48 150.0(5) . . . . ? C44 C45 C50 C52 -68.4(8) . . . . ? C46 C45 C50 C52 108.9(7) . . . . ? C44 C45 C50 C51 55.2(8) . . . . ? C46 C45 C50 C51 -127.4(6) . . . . ? C53 C54 C55 C56 -105.0(9) . . . . ? C53 C54 C55 Cr2 101.2(7) . . . . ? N3 Cr2 C55 C56 -67.0(4) . . . . ? Cr1 Cr2 C55 C56 36.3(3) . . . . ? N1 Cr2 C55 C56 139.4(3) . . . . ? N3 Cr2 C55 C54 95.0(6) . . . . ? Cr1 Cr2 C55 C54 -161.7(6) . . . . ? N1 Cr2 C55 C54 -58.6(7) . . . . ? C56 Cr2 C55 C54 161.9(8) . . . . ? C54 C55 C56 C57 -19.8(13) . . . . ? Cr2 C55 C56 C57 142.2(8) . . . . ? C54 C55 C56 Cr1 163.7(6) . . . . ? Cr2 C55 C56 Cr1 -34.3(3) . . . . ? C54 C55 C56 Cr2 -162.0(8) . . . . ? N2 Cr1 C56 C55 -59.9(4) . . . . ? N4 Cr1 C56 C55 138.7(4) . . . . ? Cr2 Cr1 C56 C55 37.6(4) . . . . ? N2 Cr1 C56 C57 123.3(7) . . . . ? N4 Cr1 C56 C57 -38.0(7) . . . . ? Cr2 Cr1 C56 C57 -139.2(7) . . . . ? N2 Cr1 C56 Cr2 -97.49(15) . . . . ? N4 Cr1 C56 Cr2 101.13(15) . . . . ? N3 Cr2 C56 C55 123.3(4) . . . . ? Cr1 Cr2 C56 C55 -135.6(4) . . . . ? N1 Cr2 C56 C55 -56.4(4) . . . . ? N3 Cr2 C56 C57 1.0(9) . . . . ? Cr1 Cr2 C56 C57 102.1(9) . . . . ? N1 Cr2 C56 C57 -178.7(8) . . . . ? C55 Cr2 C56 C57 -122.3(10) . . . . ? N3 Cr2 C56 Cr1 -101.10(16) . . . . ? N1 Cr2 C56 Cr1 79.2(3) . . . . ? C55 Cr2 C56 Cr1 135.6(4) . . . . ? C55 C56 C57 C58 8.2(16) . . . . ? Cr1 C56 C57 C58 -176.2(9) . . . . ? Cr2 C56 C57 C58 107.2(13) . . . . ? C61 O1 C60 C59 -175.0(19) . . . . ? C60 O1 C61 C62 177.1(18) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.957 _refine_diff_density_min -0.774 _refine_diff_density_rms 0.087 # start Validation Reply Form _vrf_PLAT220_klat844 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.2 Ratio RESPONSE: The isopropyl groups have slight but unresolvable disorder causing a large Ueq range. ; _vrf_PLAT360_klat844 ; PROBLEM: Short C(sp3)-C(sp3) Bond C59 -C60 ... 1.26 Ang. RESPONSE: The diethyl ether molecule of solvation is unresolvably disordered along its length. ; data_klat827s _database_code_depnum_ccdc_archive 'CCDC 839346' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C73 H90 Cr2 N4' _chemical_formula_weight 1127.49 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.399(4) _cell_length_b 13.333(3) _cell_length_c 27.223(6) _cell_angle_alpha 90.00 _cell_angle_beta 106.668(4) _cell_angle_gamma 90.00 _cell_volume 6397(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 931 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 22.11 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.171 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 0.384 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8823 _exptl_absorpt_correction_T_max 0.9373 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _diffrn_ambient_temperature 200(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 AXS APEX diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 836.6 _diffrn_reflns_number 80891 _diffrn_reflns_av_R_equivalents 0.0980 _diffrn_reflns_av_sigmaI/netI 0.0862 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 28.34 _reflns_number_total 15966 _reflns_number_gt 10194 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2001)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _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^)+(0.0735P)^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 15966 _refine_ls_number_parameters 665 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1147 _refine_ls_R_factor_gt 0.0696 _refine_ls_wR_factor_ref 0.1737 _refine_ls_wR_factor_gt 0.1532 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 Cr1 Cr 0.85304(2) 0.35536(3) 0.114810(16) 0.03091(12) Uani 1 1 d . . . Cr2 Cr 0.78457(3) 0.24991(3) 0.083240(16) 0.02877(12) Uani 1 1 d . . . N1 N 0.83462(12) 0.37413(15) 0.18070(8) 0.0263(5) Uani 1 1 d . . . N2 N 0.71377(12) 0.23684(14) 0.12249(8) 0.0246(5) Uani 1 1 d . . . N3 N 0.84797(12) 0.45205(15) 0.06128(8) 0.0267(5) Uani 1 1 d . . . N4 N 0.77503(12) 0.26533(14) 0.01190(8) 0.0246(5) Uani 1 1 d . . . C1 C 0.78230(15) 0.32670(19) 0.19940(10) 0.0288(6) Uani 1 1 d . . . H1 H 0.7858 0.3378 0.2345 0.035 Uiso 1 1 calc R . . C2 C 0.72598(15) 0.26534(18) 0.17287(10) 0.0276(6) Uani 1 1 d . . . H2 H 0.6921 0.2399 0.1904 0.033 Uiso 1 1 calc R . . C3 C 0.62939(15) 0.09272(19) 0.08910(10) 0.0300(6) Uani 1 1 d . . . C4 C 0.55555(17) 0.0558(2) 0.06981(11) 0.0392(7) Uani 1 1 d . . . H4 H 0.5482 -0.0131 0.0608 0.047 Uiso 1 1 calc R . . C5 C 0.49324(17) 0.1168(2) 0.06360(11) 0.0397(7) Uani 1 1 d . . . H5 H 0.4435 0.0901 0.0505 0.048 Uiso 1 1 calc R . . C6 C 0.50330(16) 0.2163(2) 0.07638(11) 0.0362(6) Uani 1 1 d . . . H6 H 0.4601 0.2579 0.0725 0.043 Uiso 1 1 calc R . . C7 C 0.57523(15) 0.25779(19) 0.09487(10) 0.0296(6) Uani 1 1 d . . . C8 C 0.63864(14) 0.19508(18) 0.10116(10) 0.0262(5) Uani 1 1 d . . . C9 C 0.58200(16) 0.36915(19) 0.10799(11) 0.0345(6) Uani 1 1 d . . . H9 H 0.6371 0.3864 0.1207 0.041 Uiso 1 1 calc R . . C10 C 0.54594(19) 0.4349(2) 0.06132(13) 0.0466(8) Uani 1 1 d . . . H10A H 0.5710 0.4223 0.0346 0.070 Uiso 1 1 calc R . . H10B H 0.5519 0.5057 0.0713 0.070 Uiso 1 1 calc R . . H10C H 0.4918 0.4188 0.0481 0.070 Uiso 1 1 calc R . . C11 C 0.5457(2) 0.3923(3) 0.15071(14) 0.0597(10) Uani 1 1 d . . . H11A H 0.4911 0.3795 0.1384 0.090 Uiso 1 1 calc R . . H11B H 0.5545 0.4629 0.1607 0.090 Uiso 1 1 calc R . . H11C H 0.5684 0.3495 0.1804 0.090 Uiso 1 1 calc R . . C12 C 0.69532(18) 0.0205(2) 0.10032(12) 0.0411(7) Uani 1 1 d . . . H12 H 0.7431 0.0609 0.1107 0.049 Uiso 1 1 calc R . . C13 C 0.6940(2) -0.0465(3) 0.14539(15) 0.0623(10) Uani 1 1 d . . . H13A H 0.6953 -0.0047 0.1753 0.093 Uiso 1 1 calc R . . H13B H 0.7383 -0.0909 0.1536 0.093 Uiso 1 1 calc R . . H13C H 0.6476 -0.0869 0.1363 0.093 Uiso 1 1 calc R . . C14 C 0.6967(2) -0.0418(3) 0.05366(16) 0.0665(11) Uani 1 1 d . . . H14A H 0.6525 -0.0863 0.0444 0.100 Uiso 1 1 calc R . . H14B H 0.7432 -0.0821 0.0618 0.100 Uiso 1 1 calc R . . H14C H 0.6954 0.0029 0.0248 0.100 Uiso 1 1 calc R . . C15 C 0.86438(18) 0.5415(2) 0.21965(11) 0.0371(7) Uani 1 1 d . . . C16 C 0.9113(2) 0.6019(3) 0.25817(13) 0.0512(9) Uani 1 1 d . . . H16 H 0.8997 0.6711 0.2596 0.061 Uiso 1 1 calc R . . C17 C 0.9734(2) 0.5629(3) 0.29372(13) 0.0583(10) Uani 1 1 d . . . H17 H 1.0038 0.6050 0.3198 0.070 Uiso 1 1 calc R . . C18 C 0.9920(2) 0.4640(3) 0.29196(12) 0.0521(9) Uani 1 1 d . . . H18 H 1.0356 0.4386 0.3167 0.063 Uiso 1 1 calc R . . C19 C 0.94859(17) 0.3998(2) 0.25481(11) 0.0380(7) Uani 1 1 d . . . C20 C 0.88446(16) 0.4393(2) 0.21858(10) 0.0310(6) Uani 1 1 d . . . C21 C 0.79382(18) 0.5853(2) 0.18311(12) 0.0400(7) Uani 1 1 d . . . H21 H 0.7867 0.5526 0.1490 0.048 Uiso 1 1 calc R . . C22 C 0.7230(2) 0.5631(2) 0.20038(14) 0.0534(9) Uani 1 1 d . . . H22A H 0.7163 0.4904 0.2020 0.080 Uiso 1 1 calc R . . H22B H 0.6783 0.5923 0.1758 0.080 Uiso 1 1 calc R . . H22C H 0.7291 0.5924 0.2343 0.080 Uiso 1 1 calc R . . C23 C 0.7990(2) 0.6988(2) 0.17564(14) 0.0579(10) Uani 1 1 d . . . H23A H 0.7961 0.7337 0.2067 0.087 Uiso 1 1 calc R . . H23B H 0.7570 0.7204 0.1464 0.087 Uiso 1 1 calc R . . H23C H 0.8473 0.7147 0.1690 0.087 Uiso 1 1 calc R . . C24 C 0.96929(18) 0.2895(2) 0.25608(11) 0.0452(8) Uani 1 1 d . . . H24 H 0.9461 0.2608 0.2211 0.054 Uiso 1 1 calc R . . C25 C 0.9375(2) 0.2329(3) 0.29390(15) 0.0623(10) Uani 1 1 d . . . H25A H 0.9532 0.1624 0.2952 0.093 Uiso 1 1 calc R . . H25B H 0.8820 0.2370 0.2829 0.093 Uiso 1 1 calc R . . H25C H 0.9570 0.2628 0.3280 0.093 Uiso 1 1 calc R . . C26 C 1.0554(2) 0.2726(3) 0.27037(15) 0.0677(11) Uani 1 1 d . . . H26A H 1.0771 0.3145 0.2486 0.102 Uiso 1 1 calc R . . H26B H 1.0657 0.2019 0.2653 0.102 Uiso 1 1 calc R . . H26C H 1.0783 0.2907 0.3064 0.102 Uiso 1 1 calc R . . C27 C 0.83488(15) 0.42667(19) 0.01071(10) 0.0288(6) Uani 1 1 d . . . H27 H 0.8498 0.4742 -0.0105 0.035 Uiso 1 1 calc R . . C28 C 0.80311(15) 0.34131(19) -0.01192(10) 0.0291(6) Uani 1 1 d . . . H28 H 0.7997 0.3326 -0.0471 0.035 Uiso 1 1 calc R . . C29 C 0.93678(16) 0.5915(2) 0.09768(10) 0.0327(6) Uani 1 1 d . . . C30 C 0.94905(18) 0.6948(2) 0.10328(12) 0.0418(7) Uani 1 1 d . . . H30 H 0.9973 0.7189 0.1227 0.050 Uiso 1 1 calc R . . C31 C 0.8923(2) 0.7627(2) 0.08115(13) 0.0465(8) Uani 1 1 d . . . H31 H 0.9020 0.8327 0.0848 0.056 Uiso 1 1 calc R . . C32 C 0.82170(19) 0.7287(2) 0.05392(13) 0.0419(7) Uani 1 1 d . . . H32 H 0.7834 0.7760 0.0384 0.050 Uiso 1 1 calc R . . C33 C 0.80496(17) 0.62672(19) 0.04851(11) 0.0338(6) Uani 1 1 d . . . C34 C 0.86374(16) 0.55775(18) 0.07023(10) 0.0288(6) Uani 1 1 d . . . C35 C 1.00304(16) 0.5211(2) 0.11768(11) 0.0389(7) Uani 1 1 d . . . H35 H 0.9828 0.4511 0.1149 0.047 Uiso 1 1 calc R . . C36 C 1.0465(2) 0.5400(3) 0.17377(13) 0.0593(10) Uani 1 1 d . . . H36A H 1.0714 0.6056 0.1770 0.089 Uiso 1 1 calc R . . H36B H 1.0849 0.4876 0.1857 0.089 Uiso 1 1 calc R . . H36C H 1.0111 0.5389 0.1947 0.089 Uiso 1 1 calc R . . C37 C 1.0563(2) 0.5287(3) 0.08436(14) 0.0601(10) Uani 1 1 d . . . H37A H 1.0281 0.5153 0.0486 0.090 Uiso 1 1 calc R . . H37B H 1.0972 0.4795 0.0958 0.090 Uiso 1 1 calc R . . H37C H 1.0780 0.5963 0.0872 0.090 Uiso 1 1 calc R . . C38 C 0.72470(17) 0.5946(2) 0.01990(12) 0.0388(7) Uani 1 1 d . . . H38 H 0.7217 0.5201 0.0228 0.047 Uiso 1 1 calc R . . C39 C 0.7052(2) 0.6210(3) -0.03676(13) 0.0522(9) Uani 1 1 d . . . H39A H 0.7054 0.6940 -0.0407 0.078 Uiso 1 1 calc R . . H39B H 0.6547 0.5948 -0.0545 0.078 Uiso 1 1 calc R . . H39C H 0.7428 0.5911 -0.0515 0.078 Uiso 1 1 calc R . . C40 C 0.66639(19) 0.6409(3) 0.04323(15) 0.0526(9) Uani 1 1 d . . . H40A H 0.6774 0.6202 0.0792 0.079 Uiso 1 1 calc R . . H40B H 0.6155 0.6180 0.0242 0.079 Uiso 1 1 calc R . . H40C H 0.6688 0.7142 0.0413 0.079 Uiso 1 1 calc R . . C41 C 0.78412(16) 0.11019(19) -0.03549(10) 0.0304(6) Uani 1 1 d . . . C42 C 0.74842(17) 0.0340(2) -0.06886(11) 0.0384(7) Uani 1 1 d . . . H42 H 0.7781 -0.0176 -0.0776 0.046 Uiso 1 1 calc R . . C43 C 0.67047(18) 0.0326(2) -0.08938(12) 0.0437(8) Uani 1 1 d . . . H43 H 0.6468 -0.0206 -0.1115 0.052 Uiso 1 1 calc R . . C44 C 0.62708(17) 0.1081(2) -0.07778(11) 0.0383(7) Uani 1 1 d . . . H44 H 0.5736 0.1066 -0.0923 0.046 Uiso 1 1 calc R . . C45 C 0.65983(15) 0.1867(2) -0.04524(10) 0.0306(6) Uani 1 1 d . . . C46 C 0.73915(15) 0.18556(18) -0.02295(9) 0.0256(5) Uani 1 1 d . . . C47 C 0.86955(16) 0.1103(2) -0.01529(12) 0.0361(7) Uani 1 1 d . . . H47 H 0.8845 0.1646 0.0111 0.043 Uiso 1 1 calc R . . C48 C 0.8999(2) 0.0114(2) 0.01061(14) 0.0545(9) Uani 1 1 d . . . H48A H 0.8748 -0.0039 0.0370 0.082 Uiso 1 1 calc R . . H48B H 0.9547 0.0168 0.0265 0.082 Uiso 1 1 calc R . . H48C H 0.8895 -0.0424 -0.0150 0.082 Uiso 1 1 calc R . . C49 C 0.9053(2) 0.1345(3) -0.05832(14) 0.0552(9) Uani 1 1 d . . . H49A H 0.8939 0.0804 -0.0837 0.083 Uiso 1 1 calc R . . H49B H 0.9604 0.1409 -0.0439 0.083 Uiso 1 1 calc R . . H49C H 0.8844 0.1977 -0.0748 0.083 Uiso 1 1 calc R . . C50 C 0.61092(16) 0.2726(2) -0.03690(11) 0.0359(7) Uani 1 1 d . . . H50 H 0.6328 0.2972 -0.0010 0.043 Uiso 1 1 calc R . . C51 C 0.61334(19) 0.3594(2) -0.07319(14) 0.0534(9) Uani 1 1 d . . . H51A H 0.5930 0.3370 -0.1088 0.080 Uiso 1 1 calc R . . H51B H 0.6659 0.3817 -0.0673 0.080 Uiso 1 1 calc R . . H51C H 0.5827 0.4152 -0.0667 0.080 Uiso 1 1 calc R . . C52 C 0.52850(17) 0.2435(3) -0.04341(12) 0.0468(8) Uani 1 1 d . . . H52A H 0.5024 0.2988 -0.0319 0.070 Uiso 1 1 calc R . . H52B H 0.5268 0.1836 -0.0229 0.070 Uiso 1 1 calc R . . H52C H 0.5033 0.2294 -0.0796 0.070 Uiso 1 1 calc R . . C53 C 0.92858(16) 0.2541(2) 0.10699(11) 0.0355(6) Uani 1 1 d . . . C54 C 0.88633(16) 0.1849(2) 0.12166(11) 0.0345(6) Uani 1 1 d . . . C55 C 1.0678(2) 0.2329(3) 0.14236(16) 0.0639(11) Uani 1 1 d . . . H55 H 1.0611 0.2169 0.1748 0.077 Uiso 1 1 calc R . . C56 C 1.1393(3) 0.2324(4) 0.1365(2) 0.0968(17) Uani 1 1 d . . . H56 H 1.1817 0.2181 0.1651 0.116 Uiso 1 1 calc R . . C57 C 1.1502(3) 0.2525(3) 0.0895(3) 0.0939(17) Uani 1 1 d . . . H57 H 1.1996 0.2487 0.0853 0.113 Uiso 1 1 calc R . . C58 C 1.0902(3) 0.2777(3) 0.0495(2) 0.0804(15) Uani 1 1 d . . . H58 H 1.0977 0.2945 0.0174 0.096 Uiso 1 1 calc R . . C59 C 1.0183(2) 0.2791(3) 0.05525(14) 0.0574(10) Uani 1 1 d . . . H59 H 0.9766 0.2961 0.0267 0.069 Uiso 1 1 calc R . . C60 C 1.00514(18) 0.2563(2) 0.10177(12) 0.0387(7) Uani 1 1 d . . . C61 C 0.87372(18) 0.0607(3) 0.18628(12) 0.0452(8) Uani 1 1 d . . . H61 H 0.8330 0.0994 0.1912 0.054 Uiso 1 1 calc R . . C62 C 0.8965(2) -0.0252(3) 0.21504(13) 0.0570(9) Uani 1 1 d . . . H62 H 0.8709 -0.0454 0.2392 0.068 Uiso 1 1 calc R . . C63 C 0.9558(2) -0.0814(3) 0.20890(14) 0.0590(10) Uani 1 1 d . . . H63 H 0.9716 -0.1398 0.2291 0.071 Uiso 1 1 calc R . . C64 C 0.9924(2) -0.0527(2) 0.17320(13) 0.0524(9) Uani 1 1 d . . . H64 H 1.0332 -0.0918 0.1686 0.063 Uiso 1 1 calc R . . C65 C 0.96940(18) 0.0331(2) 0.14422(12) 0.0425(7) Uani 1 1 d . . . H65 H 0.9947 0.0526 0.1198 0.051 Uiso 1 1 calc R . . C66 C 0.90955(15) 0.0911(2) 0.15045(11) 0.0329(6) 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 Cr1 0.0279(2) 0.0423(3) 0.0227(2) -0.00116(19) 0.00755(17) -0.00813(19) Cr2 0.0430(3) 0.0211(2) 0.0249(2) -0.00048(17) 0.01401(19) -0.00070(18) N1 0.0296(12) 0.0254(11) 0.0226(11) -0.0037(8) 0.0054(9) -0.0027(9) N2 0.0251(11) 0.0198(10) 0.0272(11) 0.0005(8) 0.0049(9) 0.0015(8) N3 0.0290(12) 0.0207(10) 0.0309(12) -0.0024(9) 0.0094(10) -0.0006(9) N4 0.0263(11) 0.0224(10) 0.0249(11) 0.0002(8) 0.0070(9) 0.0011(8) C1 0.0313(14) 0.0321(13) 0.0230(13) 0.0001(11) 0.0079(11) -0.0001(11) C2 0.0281(14) 0.0279(13) 0.0270(14) 0.0011(10) 0.0084(11) -0.0001(10) C3 0.0307(15) 0.0271(13) 0.0306(14) -0.0021(11) 0.0065(12) -0.0029(11) C4 0.0406(17) 0.0304(14) 0.0441(17) -0.0039(13) 0.0082(14) -0.0111(13) C5 0.0279(15) 0.0475(17) 0.0403(17) 0.0002(14) 0.0041(13) -0.0106(13) C6 0.0286(15) 0.0418(16) 0.0381(16) 0.0019(13) 0.0095(13) 0.0021(12) C7 0.0264(14) 0.0335(14) 0.0279(14) -0.0004(11) 0.0059(11) 0.0031(11) C8 0.0226(13) 0.0288(13) 0.0256(13) -0.0010(10) 0.0042(11) -0.0021(10) C9 0.0330(15) 0.0282(14) 0.0397(16) -0.0064(12) 0.0065(13) 0.0051(11) C10 0.051(2) 0.0361(16) 0.052(2) 0.0026(14) 0.0136(16) 0.0108(14) C11 0.073(3) 0.055(2) 0.055(2) -0.0142(18) 0.025(2) 0.0073(19) C12 0.0386(17) 0.0233(13) 0.059(2) -0.0037(13) 0.0099(15) -0.0015(12) C13 0.061(2) 0.045(2) 0.075(3) 0.0127(18) 0.009(2) 0.0053(17) C14 0.075(3) 0.043(2) 0.090(3) -0.013(2) 0.035(2) 0.0086(18) C15 0.0476(18) 0.0357(15) 0.0337(16) -0.0088(12) 0.0209(14) -0.0109(13) C16 0.070(2) 0.0430(18) 0.047(2) -0.0186(15) 0.0260(19) -0.0200(17) C17 0.069(3) 0.066(2) 0.0397(19) -0.0222(17) 0.0141(18) -0.034(2) C18 0.052(2) 0.068(2) 0.0286(17) -0.0035(16) 0.0001(15) -0.0203(17) C19 0.0411(17) 0.0447(17) 0.0273(15) -0.0002(13) 0.0084(13) -0.0124(13) C20 0.0371(16) 0.0353(14) 0.0235(13) -0.0053(11) 0.0132(12) -0.0105(12) C21 0.0489(19) 0.0327(15) 0.0432(18) -0.0108(13) 0.0210(15) 0.0020(13) C22 0.053(2) 0.0447(18) 0.070(2) -0.0029(17) 0.0300(19) 0.0049(16) C23 0.086(3) 0.0376(18) 0.057(2) -0.0045(16) 0.031(2) -0.0020(18) C24 0.0472(19) 0.0540(19) 0.0260(15) -0.0002(14) -0.0029(14) -0.0026(15) C25 0.067(3) 0.059(2) 0.055(2) 0.0190(18) 0.0081(19) -0.0051(18) C26 0.057(2) 0.086(3) 0.055(2) 0.006(2) 0.0073(19) 0.008(2) C27 0.0326(15) 0.0266(13) 0.0320(14) 0.0017(11) 0.0168(12) -0.0012(11) C28 0.0344(15) 0.0307(14) 0.0246(13) -0.0009(11) 0.0125(11) 0.0017(11) C29 0.0391(16) 0.0308(14) 0.0304(15) -0.0025(11) 0.0135(12) -0.0064(12) C30 0.0477(19) 0.0348(16) 0.0441(18) -0.0080(13) 0.0150(15) -0.0145(14) C31 0.063(2) 0.0259(15) 0.054(2) -0.0042(13) 0.0218(17) -0.0078(14) C32 0.052(2) 0.0247(14) 0.0521(19) 0.0002(13) 0.0189(16) 0.0016(13) C33 0.0405(16) 0.0263(13) 0.0393(16) -0.0002(12) 0.0190(13) -0.0003(12) C34 0.0363(15) 0.0243(12) 0.0291(14) -0.0026(11) 0.0146(12) -0.0038(11) C35 0.0342(16) 0.0361(15) 0.0437(18) 0.0022(13) 0.0067(14) -0.0102(12) C36 0.050(2) 0.076(3) 0.047(2) 0.0093(19) 0.0072(17) -0.0067(18) C37 0.054(2) 0.070(2) 0.057(2) 0.0019(19) 0.0171(18) 0.0097(19) C38 0.0359(16) 0.0289(14) 0.0520(19) 0.0030(13) 0.0135(14) 0.0009(12) C39 0.047(2) 0.051(2) 0.055(2) 0.0065(16) 0.0098(16) 0.0014(16) C40 0.0389(18) 0.051(2) 0.072(2) 0.0014(18) 0.0228(17) 0.0050(15) C41 0.0323(15) 0.0294(13) 0.0301(14) -0.0025(11) 0.0100(12) -0.0003(11) C42 0.0404(17) 0.0315(14) 0.0442(17) -0.0124(13) 0.0135(14) 0.0017(12) C43 0.0467(19) 0.0392(16) 0.0412(18) -0.0195(14) 0.0061(15) -0.0073(14) C44 0.0303(15) 0.0473(17) 0.0326(15) -0.0120(13) 0.0015(12) -0.0034(13) C45 0.0314(15) 0.0334(14) 0.0263(14) -0.0007(11) 0.0072(11) 0.0012(11) C46 0.0288(14) 0.0269(12) 0.0204(12) -0.0002(10) 0.0057(11) -0.0013(10) C47 0.0305(15) 0.0366(15) 0.0420(17) -0.0098(13) 0.0117(13) 0.0048(12) C48 0.054(2) 0.0494(19) 0.058(2) -0.0003(17) 0.0116(18) 0.0167(16) C49 0.042(2) 0.065(2) 0.064(2) 0.0015(18) 0.0237(17) -0.0007(16) C50 0.0286(15) 0.0410(16) 0.0333(15) -0.0054(12) 0.0013(12) 0.0081(12) C51 0.0415(19) 0.0441(18) 0.072(2) 0.0071(17) 0.0118(17) 0.0145(15) C52 0.0340(17) 0.065(2) 0.0383(17) -0.0047(16) 0.0061(14) 0.0096(15) C53 0.0338(15) 0.0331(14) 0.0313(15) -0.0031(12) -0.0037(12) 0.0009(12) C54 0.0321(15) 0.0328(14) 0.0397(16) -0.0129(12) 0.0118(13) 0.0056(12) C55 0.038(2) 0.091(3) 0.063(2) 0.022(2) 0.0144(18) 0.0018(18) C56 0.049(3) 0.117(4) 0.126(5) 0.048(3) 0.028(3) 0.006(2) C57 0.071(3) 0.082(3) 0.155(6) 0.012(3) 0.075(4) 0.002(3) C58 0.106(4) 0.068(3) 0.094(4) -0.025(3) 0.070(3) -0.032(3) C59 0.077(3) 0.053(2) 0.043(2) -0.0066(16) 0.0194(19) -0.0200(19) C60 0.0417(17) 0.0327(15) 0.0423(17) 0.0003(13) 0.0128(14) -0.0008(13) C61 0.0374(18) 0.058(2) 0.0388(18) -0.0020(15) 0.0094(14) 0.0012(15) C62 0.051(2) 0.075(2) 0.046(2) 0.0147(18) 0.0152(17) 0.0047(19) C63 0.064(2) 0.056(2) 0.049(2) 0.0143(17) 0.0034(18) 0.0043(18) C64 0.052(2) 0.0461(19) 0.054(2) 0.0008(16) 0.0084(17) 0.0104(16) C65 0.0479(19) 0.0393(16) 0.0407(18) -0.0016(14) 0.0135(15) 0.0022(14) C66 0.0269(14) 0.0372(15) 0.0325(15) -0.0051(12) 0.0049(12) 0.0005(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 Cr1 Cr2 1.9186(7) . ? Cr1 N3 1.928(2) . ? Cr1 N1 1.935(2) . ? Cr1 C53 1.992(3) . ? Cr1 C54 2.347(3) . ? Cr2 N4 1.910(2) . ? Cr2 N2 1.915(2) . ? Cr2 C54 2.056(3) . ? N1 C1 1.366(3) . ? N1 C20 1.455(3) . ? N2 C2 1.378(3) . ? N2 C8 1.448(3) . ? N3 C27 1.370(3) . ? N3 C34 1.445(3) . ? N4 C28 1.380(3) . ? N4 C46 1.452(3) . ? C1 C2 1.355(4) . ? C3 C4 1.398(4) . ? C3 C8 1.403(3) . ? C3 C12 1.510(4) . ? C4 C5 1.376(4) . ? C5 C6 1.371(4) . ? C6 C7 1.389(4) . ? C7 C8 1.405(3) . ? C7 C9 1.524(4) . ? C9 C11 1.529(4) . ? C9 C10 1.529(4) . ? C12 C13 1.523(5) . ? C12 C14 1.524(5) . ? C15 C16 1.405(4) . ? C15 C20 1.414(4) . ? C15 C21 1.508(4) . ? C16 C17 1.371(5) . ? C17 C18 1.367(5) . ? C18 C19 1.389(4) . ? C19 C20 1.406(4) . ? C19 C24 1.517(4) . ? C21 C23 1.533(4) . ? C21 C22 1.536(4) . ? C24 C25 1.521(5) . ? C24 C26 1.535(5) . ? C27 C28 1.345(4) . ? C29 C30 1.397(4) . ? C29 C34 1.411(4) . ? C29 C35 1.511(4) . ? C30 C31 1.383(4) . ? C31 C32 1.374(5) . ? C32 C33 1.393(4) . ? C33 C34 1.414(4) . ? C33 C38 1.520(4) . ? C35 C37 1.518(5) . ? C35 C36 1.528(4) . ? C38 C39 1.521(4) . ? C38 C40 1.525(4) . ? C41 C42 1.395(4) . ? C41 C46 1.405(4) . ? C41 C47 1.509(4) . ? C42 C43 1.382(4) . ? C43 C44 1.377(4) . ? C44 C45 1.392(4) . ? C45 C46 1.411(4) . ? C45 C50 1.514(4) . ? C47 C48 1.524(4) . ? C47 C49 1.533(4) . ? C50 C52 1.526(4) . ? C50 C51 1.531(4) . ? C53 C54 1.339(4) . ? C53 C60 1.456(4) . ? C54 C66 1.473(4) . ? C55 C56 1.369(6) . ? C55 C60 1.385(5) . ? C56 C57 1.377(7) . ? C57 C58 1.352(7) . ? C58 C59 1.377(6) . ? C59 C60 1.389(4) . ? C61 C62 1.382(5) . ? C61 C66 1.385(4) . ? C62 C63 1.373(5) . ? C63 C64 1.386(5) . ? C64 C65 1.385(4) . ? C65 C66 1.396(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cr2 Cr1 N3 105.56(7) . . ? Cr2 Cr1 N1 104.06(7) . . ? N3 Cr1 N1 129.12(9) . . ? Cr2 Cr1 C53 81.04(8) . . ? N3 Cr1 C53 104.85(11) . . ? N1 Cr1 C53 119.99(11) . . ? Cr2 Cr1 C54 56.56(7) . . ? N3 Cr1 C54 131.49(10) . . ? N1 Cr1 C54 99.36(9) . . ? C53 Cr1 C54 34.75(11) . . ? N4 Cr2 N2 134.28(9) . . ? N4 Cr2 Cr1 103.51(6) . . ? N2 Cr2 Cr1 106.32(6) . . ? N4 Cr2 C54 111.55(10) . . ? N2 Cr2 C54 110.11(11) . . ? Cr1 Cr2 C54 72.29(8) . . ? C1 N1 C20 112.4(2) . . ? C1 N1 Cr1 127.96(17) . . ? C20 N1 Cr1 119.46(16) . . ? C2 N2 C8 111.7(2) . . ? C2 N2 Cr2 125.98(17) . . ? C8 N2 Cr2 122.35(16) . . ? C27 N3 C34 112.3(2) . . ? C27 N3 Cr1 123.43(16) . . ? C34 N3 Cr1 124.10(17) . . ? C28 N4 C46 113.1(2) . . ? C28 N4 Cr2 128.23(17) . . ? C46 N4 Cr2 118.52(15) . . ? C2 C1 N1 126.4(2) . . ? C1 C2 N2 125.3(2) . . ? C4 C3 C8 118.0(2) . . ? C4 C3 C12 119.3(2) . . ? C8 C3 C12 122.4(2) . . ? C5 C4 C3 121.6(3) . . ? C6 C5 C4 119.6(3) . . ? C5 C6 C7 121.5(3) . . ? C6 C7 C8 118.6(2) . . ? C6 C7 C9 118.6(2) . . ? C8 C7 C9 122.8(2) . . ? C3 C8 C7 120.6(2) . . ? C3 C8 N2 120.4(2) . . ? C7 C8 N2 118.9(2) . . ? C7 C9 C11 110.6(2) . . ? C7 C9 C10 112.1(2) . . ? C11 C9 C10 109.6(3) . . ? C3 C12 C13 109.8(3) . . ? C3 C12 C14 112.6(3) . . ? C13 C12 C14 111.1(3) . . ? C16 C15 C20 117.4(3) . . ? C16 C15 C21 119.9(3) . . ? C20 C15 C21 122.7(2) . . ? C17 C16 C15 121.2(3) . . ? C18 C17 C16 120.5(3) . . ? C17 C18 C19 121.5(3) . . ? C18 C19 C20 118.1(3) . . ? C18 C19 C24 119.5(3) . . ? C20 C19 C24 122.3(3) . . ? C19 C20 C15 121.2(3) . . ? C19 C20 N1 120.3(2) . . ? C15 C20 N1 118.4(3) . . ? C15 C21 C23 113.2(3) . . ? C15 C21 C22 111.6(3) . . ? C23 C21 C22 108.8(3) . . ? C19 C24 C25 110.7(3) . . ? C19 C24 C26 112.4(3) . . ? C25 C24 C26 108.9(3) . . ? C28 C27 N3 126.6(2) . . ? C27 C28 N4 125.3(2) . . ? C30 C29 C34 118.1(3) . . ? C30 C29 C35 119.0(3) . . ? C34 C29 C35 122.7(2) . . ? C31 C30 C29 121.3(3) . . ? C32 C31 C30 119.8(3) . . ? C31 C32 C33 121.7(3) . . ? C32 C33 C34 118.1(3) . . ? C32 C33 C38 118.8(3) . . ? C34 C33 C38 123.1(2) . . ? C29 C34 C33 120.8(2) . . ? C29 C34 N3 121.0(2) . . ? C33 C34 N3 118.1(2) . . ? C29 C35 C37 109.6(2) . . ? C29 C35 C36 113.2(3) . . ? C37 C35 C36 110.1(3) . . ? C39 C38 C33 111.5(2) . . ? C39 C38 C40 109.8(3) . . ? C33 C38 C40 111.6(3) . . ? C42 C41 C46 118.6(3) . . ? C42 C41 C47 119.0(2) . . ? C46 C41 C47 122.4(2) . . ? C43 C42 C41 120.9(3) . . ? C44 C43 C42 120.0(3) . . ? C43 C44 C45 121.5(3) . . ? C44 C45 C46 118.1(2) . . ? C44 C45 C50 119.8(2) . . ? C46 C45 C50 122.0(2) . . ? C41 C46 C45 120.8(2) . . ? C41 C46 N4 119.6(2) . . ? C45 C46 N4 119.6(2) . . ? C41 C47 C48 111.9(2) . . ? C41 C47 C49 110.6(3) . . ? C48 C47 C49 110.8(3) . . ? C45 C50 C52 113.8(2) . . ? C45 C50 C51 110.3(2) . . ? C52 C50 C51 109.2(2) . . ? C54 C53 C60 134.7(3) . . ? C54 C53 Cr1 87.29(19) . . ? C60 C53 Cr1 136.2(2) . . ? C53 C54 C66 129.8(3) . . ? C53 C54 Cr2 94.6(2) . . ? C66 C54 Cr2 135.4(2) . . ? C53 C54 Cr1 57.97(16) . . ? C66 C54 Cr1 153.3(2) . . ? Cr2 C54 Cr1 51.15(6) . . ? C56 C55 C60 121.1(4) . . ? C55 C56 C57 120.5(5) . . ? C58 C57 C56 119.6(4) . . ? C57 C58 C59 120.1(4) . . ? C58 C59 C60 121.7(4) . . ? C55 C60 C59 117.0(3) . . ? C55 C60 C53 121.7(3) . . ? C59 C60 C53 121.3(3) . . ? C62 C61 C66 120.9(3) . . ? C63 C62 C61 120.3(3) . . ? C62 C63 C64 119.9(3) . . ? C65 C64 C63 119.7(3) . . ? C64 C65 C66 120.8(3) . . ? C61 C66 C65 118.3(3) . . ? C61 C66 C54 120.0(3) . . ? C65 C66 C54 121.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Cr1 Cr2 N4 21.16(9) . . . . ? N1 Cr1 Cr2 N4 159.31(9) . . . . ? C53 Cr1 Cr2 N4 -81.87(11) . . . . ? C54 Cr1 Cr2 N4 -108.65(11) . . . . ? N3 Cr1 Cr2 N2 -123.78(9) . . . . ? N1 Cr1 Cr2 N2 14.37(9) . . . . ? C53 Cr1 Cr2 N2 133.19(11) . . . . ? C54 Cr1 Cr2 N2 106.41(11) . . . . ? N3 Cr1 Cr2 C54 129.81(11) . . . . ? N1 Cr1 Cr2 C54 -92.04(11) . . . . ? C53 Cr1 Cr2 C54 26.78(12) . . . . ? Cr2 Cr1 N1 C1 -2.9(2) . . . . ? N3 Cr1 N1 C1 121.2(2) . . . . ? C53 Cr1 N1 C1 -90.6(2) . . . . ? C54 Cr1 N1 C1 -60.6(2) . . . . ? Cr2 Cr1 N1 C20 171.38(17) . . . . ? N3 Cr1 N1 C20 -64.6(2) . . . . ? C53 Cr1 N1 C20 83.7(2) . . . . ? C54 Cr1 N1 C20 113.69(19) . . . . ? N4 Cr2 N2 C2 -152.34(18) . . . . ? Cr1 Cr2 N2 C2 -23.6(2) . . . . ? C54 Cr2 N2 C2 53.1(2) . . . . ? N4 Cr2 N2 C8 27.1(2) . . . . ? Cr1 Cr2 N2 C8 155.79(16) . . . . ? C54 Cr2 N2 C8 -127.52(18) . . . . ? Cr2 Cr1 N3 C27 -31.9(2) . . . . ? N1 Cr1 N3 C27 -155.41(19) . . . . ? C53 Cr1 N3 C27 52.7(2) . . . . ? C54 Cr1 N3 C27 26.9(3) . . . . ? Cr2 Cr1 N3 C34 153.51(18) . . . . ? N1 Cr1 N3 C34 30.0(2) . . . . ? C53 Cr1 N3 C34 -121.9(2) . . . . ? C54 Cr1 N3 C34 -147.65(19) . . . . ? N2 Cr2 N4 C28 122.6(2) . . . . ? Cr1 Cr2 N4 C28 -7.1(2) . . . . ? C54 Cr2 N4 C28 -83.1(2) . . . . ? N2 Cr2 N4 C46 -62.6(2) . . . . ? Cr1 Cr2 N4 C46 167.80(16) . . . . ? C54 Cr2 N4 C46 91.77(19) . . . . ? C20 N1 C1 C2 176.5(3) . . . . ? Cr1 N1 C1 C2 -8.9(4) . . . . ? N1 C1 C2 N2 2.9(4) . . . . ? C8 N2 C2 C1 -163.9(2) . . . . ? Cr2 N2 C2 C1 15.5(4) . . . . ? C8 C3 C4 C5 -1.3(4) . . . . ? C12 C3 C4 C5 173.6(3) . . . . ? C3 C4 C5 C6 0.2(5) . . . . ? C4 C5 C6 C7 0.9(5) . . . . ? C5 C6 C7 C8 -1.0(4) . . . . ? C5 C6 C7 C9 179.7(3) . . . . ? C4 C3 C8 C7 1.2(4) . . . . ? C12 C3 C8 C7 -173.5(3) . . . . ? C4 C3 C8 N2 178.4(2) . . . . ? C12 C3 C8 N2 3.7(4) . . . . ? C6 C7 C8 C3 -0.1(4) . . . . ? C9 C7 C8 C3 179.2(2) . . . . ? C6 C7 C8 N2 -177.4(2) . . . . ? C9 C7 C8 N2 2.0(4) . . . . ? C2 N2 C8 C3 -111.1(3) . . . . ? Cr2 N2 C8 C3 69.4(3) . . . . ? C2 N2 C8 C7 66.2(3) . . . . ? Cr2 N2 C8 C7 -113.3(2) . . . . ? C6 C7 C9 C11 61.7(3) . . . . ? C8 C7 C9 C11 -117.7(3) . . . . ? C6 C7 C9 C10 -61.0(3) . . . . ? C8 C7 C9 C10 119.7(3) . . . . ? C4 C3 C12 C13 -67.9(4) . . . . ? C8 C3 C12 C13 106.7(3) . . . . ? C4 C3 C12 C14 56.4(4) . . . . ? C8 C3 C12 C14 -128.9(3) . . . . ? C20 C15 C16 C17 -0.9(5) . . . . ? C21 C15 C16 C17 176.3(3) . . . . ? C15 C16 C17 C18 1.1(5) . . . . ? C16 C17 C18 C19 -0.7(5) . . . . ? C17 C18 C19 C20 0.2(5) . . . . ? C17 C18 C19 C24 -176.9(3) . . . . ? C18 C19 C20 C15 0.0(4) . . . . ? C24 C19 C20 C15 177.0(3) . . . . ? C18 C19 C20 N1 -176.5(3) . . . . ? C24 C19 C20 N1 0.5(4) . . . . ? C16 C15 C20 C19 0.3(4) . . . . ? C21 C15 C20 C19 -176.8(3) . . . . ? C16 C15 C20 N1 176.9(3) . . . . ? C21 C15 C20 N1 -0.2(4) . . . . ? C1 N1 C20 C19 83.7(3) . . . . ? Cr1 N1 C20 C19 -91.4(3) . . . . ? C1 N1 C20 C15 -92.9(3) . . . . ? Cr1 N1 C20 C15 92.0(3) . . . . ? C16 C15 C21 C23 26.7(4) . . . . ? C20 C15 C21 C23 -156.3(3) . . . . ? C16 C15 C21 C22 -96.5(3) . . . . ? C20 C15 C21 C22 80.5(3) . . . . ? C18 C19 C24 C25 82.3(4) . . . . ? C20 C19 C24 C25 -94.7(3) . . . . ? C18 C19 C24 C26 -39.8(4) . . . . ? C20 C19 C24 C26 143.3(3) . . . . ? C34 N3 C27 C28 -164.6(3) . . . . ? Cr1 N3 C27 C28 20.3(4) . . . . ? N3 C27 C28 N4 2.8(4) . . . . ? C46 N4 C28 C27 175.8(3) . . . . ? Cr2 N4 C28 C27 -9.1(4) . . . . ? C34 C29 C30 C31 -2.2(4) . . . . ? C35 C29 C30 C31 173.4(3) . . . . ? C29 C30 C31 C32 1.4(5) . . . . ? C30 C31 C32 C33 1.0(5) . . . . ? C31 C32 C33 C34 -2.4(5) . . . . ? C31 C32 C33 C38 177.3(3) . . . . ? C30 C29 C34 C33 0.8(4) . . . . ? C35 C29 C34 C33 -174.7(3) . . . . ? C30 C29 C34 N3 177.5(2) . . . . ? C35 C29 C34 N3 2.1(4) . . . . ? C32 C33 C34 C29 1.5(4) . . . . ? C38 C33 C34 C29 -178.2(3) . . . . ? C32 C33 C34 N3 -175.4(2) . . . . ? C38 C33 C34 N3 4.9(4) . . . . ? C27 N3 C34 C29 -110.8(3) . . . . ? Cr1 N3 C34 C29 64.3(3) . . . . ? C27 N3 C34 C33 66.1(3) . . . . ? Cr1 N3 C34 C33 -118.9(2) . . . . ? C30 C29 C35 C37 -70.5(3) . . . . ? C34 C29 C35 C37 104.9(3) . . . . ? C30 C29 C35 C36 52.9(4) . . . . ? C34 C29 C35 C36 -131.7(3) . . . . ? C32 C33 C38 C39 67.3(4) . . . . ? C34 C33 C38 C39 -113.0(3) . . . . ? C32 C33 C38 C40 -55.9(4) . . . . ? C34 C33 C38 C40 123.8(3) . . . . ? C46 C41 C42 C43 0.2(4) . . . . ? C47 C41 C42 C43 -178.2(3) . . . . ? C41 C42 C43 C44 1.3(5) . . . . ? C42 C43 C44 C45 -0.5(5) . . . . ? C43 C44 C45 C46 -1.9(4) . . . . ? C43 C44 C45 C50 175.0(3) . . . . ? C42 C41 C46 C45 -2.6(4) . . . . ? C47 C41 C46 C45 175.7(2) . . . . ? C42 C41 C46 N4 179.7(2) . . . . ? C47 C41 C46 N4 -2.0(4) . . . . ? C44 C45 C46 C41 3.4(4) . . . . ? C50 C45 C46 C41 -173.4(3) . . . . ? C44 C45 C46 N4 -178.9(2) . . . . ? C50 C45 C46 N4 4.3(4) . . . . ? C28 N4 C46 C41 82.2(3) . . . . ? Cr2 N4 C46 C41 -93.4(3) . . . . ? C28 N4 C46 C45 -95.5(3) . . . . ? Cr2 N4 C46 C45 88.9(2) . . . . ? C42 C41 C47 C48 -54.8(4) . . . . ? C46 C41 C47 C48 126.9(3) . . . . ? C42 C41 C47 C49 69.2(3) . . . . ? C46 C41 C47 C49 -109.1(3) . . . . ? C44 C45 C50 C52 28.0(4) . . . . ? C46 C45 C50 C52 -155.2(3) . . . . ? C44 C45 C50 C51 -95.2(3) . . . . ? C46 C45 C50 C51 81.6(3) . . . . ? Cr2 Cr1 C53 C54 -41.28(17) . . . . ? N3 Cr1 C53 C54 -145.11(17) . . . . ? N1 Cr1 C53 C54 59.8(2) . . . . ? Cr2 Cr1 C53 C60 153.5(3) . . . . ? N3 Cr1 C53 C60 49.7(3) . . . . ? N1 Cr1 C53 C60 -105.4(3) . . . . ? C54 Cr1 C53 C60 -165.2(4) . . . . ? C60 C53 C54 C66 17.3(6) . . . . ? Cr1 C53 C54 C66 -148.3(3) . . . . ? C60 C53 C54 Cr2 -156.8(3) . . . . ? Cr1 C53 C54 Cr2 37.59(12) . . . . ? C60 C53 C54 Cr1 165.6(4) . . . . ? N4 Cr2 C54 C53 56.3(2) . . . . ? N2 Cr2 C54 C53 -142.99(17) . . . . ? Cr1 Cr2 C54 C53 -41.61(16) . . . . ? N4 Cr2 C54 C66 -117.3(3) . . . . ? N2 Cr2 C54 C66 43.5(3) . . . . ? Cr1 Cr2 C54 C66 144.8(3) . . . . ? N4 Cr2 C54 Cr1 97.91(8) . . . . ? N2 Cr2 C54 Cr1 -101.38(8) . . . . ? Cr2 Cr1 C54 C53 128.7(2) . . . . ? N3 Cr1 C54 C53 47.6(2) . . . . ? N1 Cr1 C54 C53 -130.62(18) . . . . ? Cr2 Cr1 C54 C66 -115.6(5) . . . . ? N3 Cr1 C54 C66 163.4(4) . . . . ? N1 Cr1 C54 C66 -14.8(5) . . . . ? C53 Cr1 C54 C66 115.8(5) . . . . ? N3 Cr1 C54 Cr2 -81.08(12) . . . . ? N1 Cr1 C54 Cr2 100.73(8) . . . . ? C53 Cr1 C54 Cr2 -128.7(2) . . . . ? C60 C55 C56 C57 -1.9(7) . . . . ? C55 C56 C57 C58 3.2(8) . . . . ? C56 C57 C58 C59 -2.7(7) . . . . ? C57 C58 C59 C60 0.8(6) . . . . ? C56 C55 C60 C59 0.0(6) . . . . ? C56 C55 C60 C53 178.1(4) . . . . ? C58 C59 C60 C55 0.6(5) . . . . ? C58 C59 C60 C53 -177.6(3) . . . . ? C54 C53 C60 C55 -55.7(5) . . . . ? Cr1 C53 C60 C55 103.3(4) . . . . ? C54 C53 C60 C59 122.3(4) . . . . ? Cr1 C53 C60 C59 -78.6(4) . . . . ? C66 C61 C62 C63 0.7(5) . . . . ? C61 C62 C63 C64 -0.9(6) . . . . ? C62 C63 C64 C65 0.6(5) . . . . ? C63 C64 C65 C66 -0.1(5) . . . . ? C62 C61 C66 C65 -0.2(5) . . . . ? C62 C61 C66 C54 -177.6(3) . . . . ? C64 C65 C66 C61 -0.1(4) . . . . ? C64 C65 C66 C54 177.3(3) . . . . ? C53 C54 C66 C61 142.2(3) . . . . ? Cr2 C54 C66 C61 -46.2(4) . . . . ? Cr1 C54 C66 C61 45.4(6) . . . . ? C53 C54 C66 C65 -35.1(5) . . . . ? Cr2 C54 C66 C65 136.5(3) . . . . ? Cr1 C54 C66 C65 -132.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.543 _refine_diff_density_min -0.408 _refine_diff_density_rms 0.068 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 _platon_squeeze_void_content 1 0.250 -0.054 0.250 552 140 '2 toluene' 2 0.750 -0.043 0.750 552 140 '2 toluene' _platon_squeeze_details ; PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13 Void space analysis consistent with initial solutions showing one molecule of severely disordered toluene molecule of solvation per compound molecule. ; # start Validation Reply Form _vrf_CHEMW03_klat827s ; PROBLEM: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.95 <> 1.05 RESPONSE: Data-set was treated with SQUEEZE to model one toluene molecule of solvation per compound molecule as diffused contributions. ; _vrf_PLAT043_klat827s ; PROBLEM: Check Reported Molecular Weight .............. 1127.49 RESPONSE: See response to CHEMW03 ; data_klat839s _database_code_depnum_ccdc_archive 'CCDC 839347' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H72 Cr2 F6 N4, 2.5(C7 H8)' _chemical_formula_sum 'C73.50 H92 Cr2 F6 N4' _chemical_formula_weight 1249.51 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' F F 0.0171 0.0103 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.416(5) _cell_length_b 23.911(4) _cell_length_c 21.946(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.553(4) _cell_angle_gamma 90.00 _cell_volume 14433(5) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 997 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 22.63 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.150 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5304 _exptl_absorpt_coefficient_mu 0.358 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9310 _exptl_absorpt_correction_T_max 0.9778 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _diffrn_ambient_temperature 200(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 AXS APEX diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 836.6 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 1 _diffrn_reflns_number 98135 _diffrn_reflns_av_R_equivalents 0.0966 _diffrn_reflns_av_sigmaI/netI 0.0795 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 28.31 _reflns_number_total 17963 _reflns_number_gt 11453 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2001)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _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^)+(0.0488P)^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 17963 _refine_ls_number_parameters 629 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1010 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1377 _refine_ls_wR_factor_gt 0.1256 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 Cr1 Cr 0.177901(12) 0.034894(15) 0.720522(15) 0.02647(9) Uani 1 1 d . . . Cr2 Cr 0.245744(13) 0.059199(16) 0.750207(16) 0.03068(10) Uani 1 1 d . . . N1 N 0.17906(6) -0.04297(7) 0.70040(8) 0.0289(4) Uani 1 1 d . . . N4 N 0.14500(6) 0.10069(7) 0.66275(8) 0.0271(4) Uani 1 1 d . . . N3 N 0.23587(7) 0.13738(8) 0.75556(8) 0.0321(4) Uani 1 1 d . . . N2 N 0.28115(7) -0.00754(9) 0.74592(9) 0.0356(5) Uani 1 1 d . . . F1 F 0.23531(6) -0.02784(6) 0.86892(6) 0.0497(4) Uani 1 1 d . . . F2 F 0.17230(6) 0.00873(7) 0.88982(6) 0.0514(4) Uani 1 1 d . . . F3 F 0.24161(6) 0.04921(7) 0.92078(6) 0.0581(4) Uani 1 1 d . . . F4 F 0.13218(6) 0.11844(7) 0.87058(6) 0.0540(4) Uani 1 1 d . . . F5 F 0.09522(5) 0.05666(6) 0.80437(7) 0.0477(4) Uani 1 1 d . . . F6 F 0.09512(5) 0.14291(6) 0.77643(7) 0.0484(4) Uani 1 1 d . . . C3 C 0.12054(8) -0.08540(9) 0.61022(10) 0.0331(5) Uani 1 1 d . . . C4 C 0.08011(9) -0.11957(10) 0.58771(12) 0.0414(6) Uani 1 1 d . . . H4 H 0.0704 -0.1281 0.5440 0.050 Uiso 1 1 calc R . . C5 C 0.05387(9) -0.14131(11) 0.62700(13) 0.0440(6) Uani 1 1 d . . . H5 H 0.0270 -0.1652 0.6106 0.053 Uiso 1 1 calc R . . C6 C 0.06670(9) -0.12827(11) 0.69005(13) 0.0429(6) Uani 1 1 d . . . H6 H 0.0478 -0.1424 0.7166 0.051 Uiso 1 1 calc R . . C7 C 0.10695(8) -0.09470(10) 0.71579(11) 0.0343(5) Uani 1 1 d . . . C8 C 0.13423(8) -0.07373(9) 0.67522(10) 0.0299(5) Uani 1 1 d . . . C9 C 0.14857(9) -0.06281(11) 0.56512(11) 0.0397(6) Uani 1 1 d . . . H9 H 0.1677 -0.0298 0.5858 0.048 Uiso 1 1 calc R . . C11 C 0.11507(11) -0.04260(12) 0.50332(12) 0.0534(7) Uani 1 1 d . . . H11A H 0.0998 -0.0749 0.4786 0.080 Uiso 1 1 calc R . . H11B H 0.1341 -0.0217 0.4794 0.080 Uiso 1 1 calc R . . H11C H 0.0899 -0.0183 0.5123 0.080 Uiso 1 1 calc R . . C10 C 0.18444(11) -0.10536(14) 0.55174(14) 0.0620(8) Uani 1 1 d . . . H10A H 0.2065 -0.1173 0.5915 0.093 Uiso 1 1 calc R . . H10B H 0.2033 -0.0884 0.5248 0.093 Uiso 1 1 calc R . . H10C H 0.1667 -0.1379 0.5303 0.093 Uiso 1 1 calc R . . C12 C 0.12080(9) -0.08189(11) 0.78574(11) 0.0378(5) Uani 1 1 d . . . H12 H 0.1410 -0.0471 0.7920 0.045 Uiso 1 1 calc R . . C13 C 0.15184(11) -0.12864(13) 0.82262(13) 0.0577(8) Uani 1 1 d . . . H13A H 0.1324 -0.1629 0.8192 0.087 Uiso 1 1 calc R . . H13B H 0.1630 -0.1178 0.8670 0.087 Uiso 1 1 calc R . . H13C H 0.1800 -0.1353 0.8054 0.087 Uiso 1 1 calc R . . C14 C 0.07664(10) -0.07093(12) 0.81199(13) 0.0509(7) Uani 1 1 d . . . H14A H 0.0545 -0.0450 0.7841 0.076 Uiso 1 1 calc R . . H14B H 0.0874 -0.0545 0.8541 0.076 Uiso 1 1 calc R . . H14C H 0.0598 -0.1063 0.8145 0.076 Uiso 1 1 calc R . . C19 C 0.36359(10) 0.01668(14) 0.80856(13) 0.0554(7) Uani 1 1 d . . . C18 C 0.41324(11) 0.01913(19) 0.81283(17) 0.0861(12) Uani 1 1 d . . . H18 H 0.4348 0.0306 0.8512 0.103 Uiso 1 1 calc R . . C17 C 0.43126(12) 0.0056(2) 0.7639(2) 0.1168(18) Uani 1 1 d . . . H17 H 0.4653 0.0076 0.7681 0.140 Uiso 1 1 calc R . . C16 C 0.40087(11) -0.0112(2) 0.70737(18) 0.0979(14) Uani 1 1 d . . . H16 H 0.4144 -0.0201 0.6731 0.117 Uiso 1 1 calc R . . C15 C 0.35090(10) -0.01524(15) 0.69958(14) 0.0605(8) Uani 1 1 d . . . C20 C 0.33267(9) -0.00149(12) 0.75153(12) 0.0462(7) Uani 1 1 d . . . C24 C 0.34545(10) 0.02950(14) 0.86608(13) 0.0611(8) Uani 1 1 d . . . H24 H 0.3098 0.0372 0.8516 0.073 Uiso 1 1 calc R . . C25 C 0.35213(14) -0.02186(19) 0.90850(17) 0.0948(13) Uani 1 1 d . . . H25A H 0.3366 -0.0542 0.8842 0.142 Uiso 1 1 calc R . . H25B H 0.3372 -0.0151 0.9435 0.142 Uiso 1 1 calc R . . H25C H 0.3869 -0.0293 0.9251 0.142 Uiso 1 1 calc R . . C26 C 0.36970(14) 0.08118(19) 0.9020(2) 0.1076(15) Uani 1 1 d . . . H26A H 0.4033 0.0722 0.9240 0.161 Uiso 1 1 calc R . . H26B H 0.3518 0.0926 0.9327 0.161 Uiso 1 1 calc R . . H26C H 0.3695 0.1118 0.8722 0.161 Uiso 1 1 calc R . . C21 C 0.31952(11) -0.03310(16) 0.63568(14) 0.0684(10) Uani 1 1 d . . . H21 H 0.2848 -0.0281 0.6366 0.082 Uiso 1 1 calc R . . C23 C 0.32684(13) -0.09507(18) 0.62252(18) 0.0961(14) Uani 1 1 d . . . H23A H 0.3613 -0.1020 0.6251 0.144 Uiso 1 1 calc R . . H23B H 0.3074 -0.1047 0.5803 0.144 Uiso 1 1 calc R . . H23C H 0.3166 -0.1181 0.6538 0.144 Uiso 1 1 calc R . . C22 C 0.32849(13) 0.0034(2) 0.58207(16) 0.0947(14) Uani 1 1 d . . . H22A H 0.3219 0.0426 0.5899 0.142 Uiso 1 1 calc R . . H22B H 0.3069 -0.0086 0.5420 0.142 Uiso 1 1 calc R . . H22C H 0.3624 -0.0006 0.5801 0.142 Uiso 1 1 calc R . . C29 C 0.30552(9) 0.19478(12) 0.74888(12) 0.0472(7) Uani 1 1 d . . . C30 C 0.33748(11) 0.23836(12) 0.77156(14) 0.0569(8) Uani 1 1 d . . . H30 H 0.3613 0.2480 0.7498 0.068 Uiso 1 1 calc R . . C31 C 0.33563(11) 0.26795(13) 0.82473(14) 0.0625(9) Uani 1 1 d . . . H31 H 0.3565 0.2990 0.8382 0.075 Uiso 1 1 calc R . . C32 C 0.30323(11) 0.25156(12) 0.85745(13) 0.0577(8) Uani 1 1 d . . . H32 H 0.3028 0.2713 0.8949 0.069 Uiso 1 1 calc R . . C33 C 0.27071(10) 0.20759(11) 0.83923(11) 0.0442(6) Uani 1 1 d . . . C34 C 0.27031(9) 0.17989(10) 0.78135(11) 0.0379(6) Uani 1 1 d . . . C35 C 0.31064(12) 0.16447(16) 0.68977(15) 0.0722(10) Uani 1 1 d . . . H35 H 0.2862 0.1336 0.6794 0.087 Uiso 1 1 calc R . . C37 C 0.36345(15) 0.13946(19) 0.7008(2) 0.1058(14) Uani 1 1 d . . . H37A H 0.3652 0.1158 0.6649 0.159 Uiso 1 1 calc R . . H37B H 0.3710 0.1170 0.7393 0.159 Uiso 1 1 calc R . . H37C H 0.3870 0.1700 0.7049 0.159 Uiso 1 1 calc R . . C36 C 0.30311(15) 0.20453(18) 0.63489(16) 0.0945(13) Uani 1 1 d . . . H36A H 0.2699 0.2192 0.6254 0.142 Uiso 1 1 calc R . . H36B H 0.3083 0.1848 0.5980 0.142 Uiso 1 1 calc R . . H36C H 0.3263 0.2355 0.6458 0.142 Uiso 1 1 calc R . . C38 C 0.24064(11) 0.19016(12) 0.88440(11) 0.0490(7) Uani 1 1 d . . . H38 H 0.2224 0.1554 0.8674 0.059 Uiso 1 1 calc R . . C39 C 0.27342(12) 0.17641(14) 0.94989(12) 0.0649(9) Uani 1 1 d . . . H39A H 0.2990 0.1504 0.9455 0.097 Uiso 1 1 calc R . . H39B H 0.2539 0.1592 0.9758 0.097 Uiso 1 1 calc R . . H39C H 0.2883 0.2109 0.9701 0.097 Uiso 1 1 calc R . . C40 C 0.20350(12) 0.23449(13) 0.89123(14) 0.0655(9) Uani 1 1 d . . . H40A H 0.2204 0.2694 0.9068 0.098 Uiso 1 1 calc R . . H40B H 0.1854 0.2213 0.9211 0.098 Uiso 1 1 calc R . . H40C H 0.1808 0.2412 0.8502 0.098 Uiso 1 1 calc R . . C41 C 0.13483(9) 0.11179(10) 0.54762(10) 0.0370(5) Uani 1 1 d . . . C42 C 0.10428(9) 0.10793(11) 0.48730(11) 0.0419(6) Uani 1 1 d . . . H42 H 0.1166 0.1168 0.4521 0.050 Uiso 1 1 calc R . . C43 C 0.05632(9) 0.09143(11) 0.47750(11) 0.0426(6) Uani 1 1 d . . . H43 H 0.0361 0.0890 0.4359 0.051 Uiso 1 1 calc R . . C44 C 0.03810(9) 0.07856(11) 0.52799(11) 0.0401(6) Uani 1 1 d . . . H44 H 0.0051 0.0675 0.5209 0.048 Uiso 1 1 calc R . . C45 C 0.06675(8) 0.08133(10) 0.58930(10) 0.0321(5) Uani 1 1 d . . . C46 C 0.11525(8) 0.09813(9) 0.59818(10) 0.0293(5) Uani 1 1 d . . . C47 C 0.18711(9) 0.13023(12) 0.55504(11) 0.0462(7) Uani 1 1 d . . . H47 H 0.2021 0.1373 0.6007 0.055 Uiso 1 1 calc R . . C48 C 0.21585(11) 0.08418(16) 0.53302(18) 0.0771(10) Uani 1 1 d . . . H48A H 0.2006 0.0752 0.4889 0.116 Uiso 1 1 calc R . . H48B H 0.2162 0.0508 0.5590 0.116 Uiso 1 1 calc R . . H48C H 0.2493 0.0969 0.5370 0.116 Uiso 1 1 calc R . . C49 C 0.18941(12) 0.18375(14) 0.51922(16) 0.0702(9) Uani 1 1 d . . . H49A H 0.1764 0.1771 0.4741 0.105 Uiso 1 1 calc R . . H49B H 0.2233 0.1962 0.5272 0.105 Uiso 1 1 calc R . . H49C H 0.1700 0.2127 0.5332 0.105 Uiso 1 1 calc R . . C50 C 0.04441(9) 0.06926(11) 0.64378(12) 0.0418(6) Uani 1 1 d . . . H50 H 0.0716 0.0654 0.6826 0.050 Uiso 1 1 calc R . . C52 C 0.01333(11) 0.11910(13) 0.65366(15) 0.0609(8) Uani 1 1 d . . . H52A H 0.0331 0.1532 0.6593 0.091 Uiso 1 1 calc R . . H52B H 0.0013 0.1127 0.6912 0.091 Uiso 1 1 calc R . . H52C H -0.0143 0.1233 0.6168 0.091 Uiso 1 1 calc R . . C51 C 0.01535(10) 0.01527(13) 0.63560(14) 0.0560(8) Uani 1 1 d . . . H51A H -0.0143 0.0199 0.6018 0.084 Uiso 1 1 calc R . . H51B H 0.0067 0.0062 0.6750 0.084 Uiso 1 1 calc R . . H51C H 0.0350 -0.0151 0.6248 0.084 Uiso 1 1 calc R . . C1 C 0.21859(9) -0.07794(10) 0.71524(11) 0.0367(5) Uani 1 1 d . . . H1 H 0.2124 -0.1170 0.7107 0.044 Uiso 1 1 calc R . . C2 C 0.26555(9) -0.06182(11) 0.73572(11) 0.0405(6) Uani 1 1 d . . . H2 H 0.2896 -0.0903 0.7437 0.049 Uiso 1 1 calc R . . C27 C 0.18479(8) 0.14729(9) 0.75647(10) 0.0305(5) Uani 1 1 d . . . H27 H 0.1809 0.1824 0.7796 0.037 Uiso 1 1 calc R . . C28 C 0.15514(8) 0.14845(10) 0.68941(10) 0.0304(5) Uani 1 1 d . . . H28 H 0.1445 0.1825 0.6680 0.036 Uiso 1 1 calc R . . C53 C 0.21310(9) 0.02129(11) 0.87125(11) 0.0410(6) Uani 1 1 d . . . C54 C 0.20532(8) 0.05334(10) 0.81184(10) 0.0311(5) Uani 1 1 d . . . C55 C 0.16875(8) 0.09462(9) 0.78748(10) 0.0307(5) Uani 1 1 d . . . C56 C 0.12359(9) 0.10221(11) 0.80966(11) 0.0391(6) 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 Cr1 0.02690(18) 0.0316(2) 0.02127(17) -0.00218(14) 0.00664(14) -0.00038(15) Cr2 0.02737(19) 0.0391(2) 0.02497(18) -0.00411(15) 0.00556(14) -0.00282(16) N1 0.0275(9) 0.0306(10) 0.0282(9) -0.0025(7) 0.0066(8) 0.0002(8) N4 0.0254(9) 0.0327(10) 0.0231(9) -0.0024(7) 0.0058(7) -0.0033(8) N3 0.0329(10) 0.0358(11) 0.0270(10) -0.0050(8) 0.0066(8) -0.0093(8) N2 0.0265(10) 0.0474(13) 0.0321(10) -0.0033(9) 0.0059(8) 0.0012(9) F1 0.0592(10) 0.0497(10) 0.0408(8) 0.0101(7) 0.0134(7) 0.0110(7) F2 0.0604(10) 0.0653(10) 0.0339(8) 0.0104(7) 0.0222(7) 0.0034(8) F3 0.0728(11) 0.0686(11) 0.0249(7) -0.0018(7) -0.0023(7) -0.0072(8) F4 0.0675(10) 0.0664(11) 0.0358(8) -0.0098(7) 0.0273(7) 0.0057(8) F5 0.0431(8) 0.0500(9) 0.0570(9) 0.0011(7) 0.0258(7) -0.0046(7) F6 0.0464(9) 0.0500(9) 0.0535(9) 0.0041(7) 0.0213(7) 0.0136(7) C3 0.0354(12) 0.0304(12) 0.0304(12) 0.0009(9) 0.0024(10) 0.0054(10) C4 0.0406(14) 0.0399(15) 0.0354(13) -0.0012(11) -0.0062(11) 0.0025(11) C5 0.0320(13) 0.0389(15) 0.0539(17) 0.0019(12) -0.0029(12) -0.0047(11) C6 0.0340(13) 0.0417(15) 0.0545(17) 0.0073(12) 0.0142(12) -0.0006(11) C7 0.0321(12) 0.0337(13) 0.0370(13) 0.0038(10) 0.0085(10) 0.0077(10) C8 0.0316(12) 0.0273(12) 0.0294(11) 0.0011(9) 0.0051(9) 0.0058(9) C9 0.0462(15) 0.0448(15) 0.0276(12) -0.0043(10) 0.0083(10) -0.0012(12) C11 0.0666(19) 0.0625(19) 0.0323(14) 0.0059(12) 0.0144(13) 0.0159(15) C10 0.0554(18) 0.079(2) 0.0562(18) 0.0124(16) 0.0224(15) 0.0208(16) C12 0.0411(14) 0.0417(14) 0.0345(13) 0.0007(11) 0.0170(11) 0.0002(11) C13 0.0601(19) 0.073(2) 0.0400(15) 0.0066(14) 0.0133(13) 0.0208(16) C14 0.0527(17) 0.0586(18) 0.0500(16) 0.0069(13) 0.0288(13) 0.0029(13) C19 0.0329(14) 0.078(2) 0.0505(17) -0.0044(15) 0.0017(12) 0.0002(14) C18 0.0335(17) 0.156(4) 0.062(2) -0.015(2) -0.0007(15) -0.006(2) C17 0.0263(17) 0.228(6) 0.094(3) -0.027(3) 0.0124(19) -0.002(2) C16 0.0330(17) 0.191(5) 0.073(2) -0.018(3) 0.0192(17) 0.010(2) C15 0.0325(15) 0.098(3) 0.0516(18) -0.0044(16) 0.0122(13) 0.0071(15) C20 0.0256(12) 0.0674(19) 0.0446(15) -0.0002(13) 0.0069(11) 0.0008(12) C24 0.0341(15) 0.094(3) 0.0465(17) -0.0175(16) -0.0058(12) 0.0052(15) C25 0.082(3) 0.139(4) 0.062(2) 0.024(2) 0.015(2) 0.018(3) C26 0.080(3) 0.123(4) 0.103(3) -0.057(3) -0.009(2) 0.004(3) C21 0.0410(16) 0.120(3) 0.0448(17) -0.0171(18) 0.0119(13) 0.0119(17) C23 0.075(3) 0.129(4) 0.082(3) -0.046(2) 0.016(2) 0.023(2) C22 0.060(2) 0.174(4) 0.056(2) 0.002(2) 0.0258(18) 0.008(2) C29 0.0420(15) 0.0535(17) 0.0441(15) -0.0078(12) 0.0074(12) -0.0140(12) C30 0.0542(17) 0.0583(19) 0.0552(18) -0.0012(14) 0.0083(14) -0.0254(15) C31 0.069(2) 0.0525(19) 0.0556(19) -0.0026(15) -0.0046(15) -0.0293(16) C32 0.076(2) 0.0508(18) 0.0384(15) -0.0099(13) 0.0003(14) -0.0215(15) C33 0.0540(16) 0.0413(15) 0.0298(13) -0.0057(11) -0.0035(11) -0.0088(12) C34 0.0403(14) 0.0369(14) 0.0328(13) 0.0000(10) 0.0023(11) -0.0066(11) C35 0.063(2) 0.097(3) 0.066(2) -0.0223(19) 0.0334(17) -0.0449(19) C37 0.088(3) 0.117(4) 0.128(4) -0.012(3) 0.055(3) -0.005(3) C36 0.105(3) 0.127(4) 0.049(2) -0.010(2) 0.014(2) -0.013(3) C38 0.0691(19) 0.0502(17) 0.0257(12) -0.0102(11) 0.0085(12) -0.0139(14) C39 0.089(2) 0.070(2) 0.0290(14) -0.0053(13) 0.0038(15) -0.0220(18) C40 0.089(2) 0.064(2) 0.0440(17) -0.0190(15) 0.0181(16) -0.0039(18) C41 0.0378(13) 0.0450(15) 0.0270(12) -0.0027(10) 0.0062(10) -0.0040(11) C42 0.0453(15) 0.0555(16) 0.0234(12) -0.0003(11) 0.0060(10) -0.0062(12) C43 0.0402(14) 0.0538(17) 0.0262(12) -0.0034(11) -0.0060(10) 0.0019(12) C44 0.0290(12) 0.0474(15) 0.0397(14) -0.0030(11) 0.0006(10) 0.0010(11) C45 0.0278(11) 0.0350(13) 0.0324(12) -0.0008(10) 0.0052(9) 0.0008(9) C46 0.0319(12) 0.0312(12) 0.0226(11) 0.0008(9) 0.0030(9) 0.0010(9) C47 0.0389(14) 0.076(2) 0.0243(12) -0.0023(12) 0.0083(10) -0.0152(13) C48 0.0421(18) 0.090(3) 0.103(3) 0.006(2) 0.0266(18) -0.0034(17) C49 0.066(2) 0.071(2) 0.072(2) -0.0002(17) 0.0152(17) -0.0279(17) C50 0.0304(13) 0.0557(17) 0.0394(14) 0.0008(11) 0.0092(11) -0.0053(11) C52 0.0512(18) 0.074(2) 0.065(2) -0.0069(16) 0.0279(15) 0.0061(15) C51 0.0401(15) 0.065(2) 0.0611(19) 0.0133(15) 0.0089(13) -0.0122(14) C1 0.0372(13) 0.0350(13) 0.0374(13) -0.0038(10) 0.0084(10) 0.0033(10) C2 0.0346(13) 0.0443(15) 0.0412(14) -0.0026(11) 0.0069(11) 0.0113(11) C27 0.0346(12) 0.0330(13) 0.0239(11) -0.0066(9) 0.0073(9) -0.0036(10) C28 0.0312(12) 0.0331(12) 0.0271(11) 0.0012(9) 0.0078(9) -0.0025(10) C53 0.0460(15) 0.0470(16) 0.0297(13) 0.0003(11) 0.0089(11) 0.0035(12) C54 0.0341(12) 0.0381(13) 0.0207(11) -0.0042(9) 0.0064(9) -0.0013(10) C55 0.0342(12) 0.0357(13) 0.0234(11) -0.0050(9) 0.0095(9) -0.0037(10) C56 0.0464(15) 0.0412(15) 0.0335(13) -0.0013(11) 0.0170(11) 0.0058(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 Cr1 N1 1.9157(19) . ? Cr1 Cr2 1.9615(6) . ? Cr1 C54 2.008(2) . ? Cr1 N4 2.0883(18) . ? Cr1 C55 2.112(2) . ? Cr2 N3 1.898(2) . ? Cr2 N2 1.901(2) . ? Cr2 C54 1.987(2) . ? N1 C1 1.372(3) . ? N1 C8 1.454(3) . ? N4 C28 1.282(3) . ? N4 C46 1.458(3) . ? N3 C34 1.426(3) . ? N3 C27 1.476(3) . ? N2 C2 1.371(3) . ? N2 C20 1.445(3) . ? F1 C53 1.341(3) . ? F2 C53 1.356(3) . ? F3 C53 1.357(3) . ? F4 C56 1.354(3) . ? F5 C56 1.343(3) . ? F6 C56 1.355(3) . ? C3 C4 1.395(3) . ? C3 C8 1.409(3) . ? C3 C9 1.517(3) . ? C4 C5 1.376(4) . ? C5 C6 1.375(4) . ? C6 C7 1.395(3) . ? C7 C8 1.411(3) . ? C7 C12 1.517(3) . ? C9 C10 1.520(4) . ? C9 C11 1.526(3) . ? C12 C13 1.524(4) . ? C12 C14 1.529(3) . ? C19 C18 1.391(4) . ? C19 C20 1.405(4) . ? C19 C24 1.510(4) . ? C18 C17 1.341(5) . ? C17 C16 1.381(5) . ? C16 C15 1.390(4) . ? C15 C20 1.405(4) . ? C15 C21 1.522(4) . ? C24 C25 1.524(5) . ? C24 C26 1.533(5) . ? C21 C23 1.534(5) . ? C21 C22 1.536(5) . ? C29 C30 1.390(4) . ? C29 C34 1.412(3) . ? C29 C35 1.524(4) . ? C30 C31 1.377(4) . ? C31 C32 1.360(4) . ? C32 C33 1.390(4) . ? C33 C34 1.430(3) . ? C33 C38 1.521(4) . ? C35 C36 1.511(5) . ? C35 C37 1.577(5) . ? C38 C40 1.530(4) . ? C38 C39 1.539(4) . ? C41 C42 1.392(3) . ? C41 C46 1.399(3) . ? C41 C47 1.518(3) . ? C42 C43 1.383(3) . ? C43 C44 1.371(3) . ? C44 C45 1.388(3) . ? C45 C46 1.401(3) . ? C45 C50 1.516(3) . ? C47 C49 1.512(4) . ? C47 C48 1.520(4) . ? C50 C51 1.519(4) . ? C50 C52 1.531(4) . ? C1 C2 1.353(3) . ? C27 C28 1.501(3) . ? C27 C55 1.553(3) . ? C53 C54 1.480(3) . ? C54 C55 1.436(3) . ? C55 C56 1.494(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 N1 Cr1 Cr2 106.99(6) . . ? N1 Cr1 C54 114.75(9) . . ? Cr2 Cr1 C54 60.07(6) . . ? N1 Cr1 N4 128.55(7) . . ? Cr2 Cr1 N4 103.36(5) . . ? C54 Cr1 N4 116.28(8) . . ? N1 Cr1 C55 146.10(8) . . ? Cr2 Cr1 C55 81.44(6) . . ? C54 Cr1 C55 40.69(9) . . ? N4 Cr1 C55 78.37(8) . . ? N3 Cr2 N2 156.62(8) . . ? N3 Cr2 Cr1 99.44(6) . . ? N2 Cr2 Cr1 102.88(6) . . ? N3 Cr2 C54 84.70(9) . . ? N2 Cr2 C54 112.21(9) . . ? Cr1 Cr2 C54 61.14(6) . . ? C1 N1 C8 111.64(18) . . ? C1 N1 Cr1 126.72(16) . . ? C8 N1 Cr1 120.99(14) . . ? C28 N4 C46 119.34(18) . . ? C28 N4 Cr1 112.26(14) . . ? C46 N4 Cr1 128.34(14) . . ? C34 N3 C27 117.35(19) . . ? C34 N3 Cr2 128.99(16) . . ? C27 N3 Cr2 108.68(13) . . ? C2 N2 C20 112.8(2) . . ? C2 N2 Cr2 130.46(16) . . ? C20 N2 Cr2 116.67(17) . . ? C4 C3 C8 117.9(2) . . ? C4 C3 C9 119.9(2) . . ? C8 C3 C9 122.2(2) . . ? C5 C4 C3 121.8(2) . . ? C6 C5 C4 119.8(2) . . ? C5 C6 C7 121.4(2) . . ? C6 C7 C8 118.3(2) . . ? C6 C7 C12 120.2(2) . . ? C8 C7 C12 121.5(2) . . ? C3 C8 C7 120.8(2) . . ? C3 C8 N1 118.52(19) . . ? C7 C8 N1 120.49(19) . . ? C3 C9 C10 112.0(2) . . ? C3 C9 C11 112.3(2) . . ? C10 C9 C11 109.8(2) . . ? C7 C12 C13 110.9(2) . . ? C7 C12 C14 112.8(2) . . ? C13 C12 C14 110.2(2) . . ? C18 C19 C20 118.0(3) . . ? C18 C19 C24 119.2(3) . . ? C20 C19 C24 122.6(2) . . ? C17 C18 C19 121.4(3) . . ? C18 C17 C16 120.7(3) . . ? C17 C16 C15 121.3(3) . . ? C16 C15 C20 117.2(3) . . ? C16 C15 C21 118.5(3) . . ? C20 C15 C21 124.3(2) . . ? C15 C20 C19 121.3(2) . . ? C15 C20 N2 118.7(2) . . ? C19 C20 N2 120.0(2) . . ? C19 C24 C25 109.3(3) . . ? C19 C24 C26 112.9(3) . . ? C25 C24 C26 111.4(3) . . ? C15 C21 C23 111.6(3) . . ? C15 C21 C22 112.0(3) . . ? C23 C21 C22 110.3(3) . . ? C30 C29 C34 119.4(2) . . ? C30 C29 C35 117.9(2) . . ? C34 C29 C35 122.7(2) . . ? C31 C30 C29 121.9(3) . . ? C32 C31 C30 118.3(3) . . ? C31 C32 C33 123.7(3) . . ? C32 C33 C34 117.5(3) . . ? C32 C33 C38 117.5(2) . . ? C34 C33 C38 124.9(2) . . ? C29 C34 N3 118.8(2) . . ? C29 C34 C33 118.9(2) . . ? N3 C34 C33 122.3(2) . . ? C36 C35 C29 110.6(3) . . ? C36 C35 C37 107.5(3) . . ? C29 C35 C37 109.9(3) . . ? C33 C38 C40 112.9(2) . . ? C33 C38 C39 111.1(2) . . ? C40 C38 C39 109.1(2) . . ? C42 C41 C46 117.5(2) . . ? C42 C41 C47 118.7(2) . . ? C46 C41 C47 123.8(2) . . ? C43 C42 C41 121.4(2) . . ? C44 C43 C42 119.7(2) . . ? C43 C44 C45 121.6(2) . . ? C44 C45 C46 117.7(2) . . ? C44 C45 C50 119.7(2) . . ? C46 C45 C50 122.5(2) . . ? C41 C46 C45 122.0(2) . . ? C41 C46 N4 120.80(19) . . ? C45 C46 N4 117.21(18) . . ? C49 C47 C41 111.0(2) . . ? C49 C47 C48 110.5(2) . . ? C41 C47 C48 110.2(2) . . ? C45 C50 C51 113.1(2) . . ? C45 C50 C52 109.5(2) . . ? C51 C50 C52 111.3(2) . . ? C2 C1 N1 125.8(2) . . ? C1 C2 N2 125.1(2) . . ? N3 C27 C28 107.53(16) . . ? N3 C27 C55 105.87(18) . . ? C28 C27 C55 106.88(17) . . ? N4 C28 C27 115.9(2) . . ? F1 C53 F2 105.3(2) . . ? F1 C53 F3 105.6(2) . . ? F2 C53 F3 104.57(19) . . ? F1 C53 C54 112.80(19) . . ? F2 C53 C54 115.5(2) . . ? F3 C53 C54 112.2(2) . . ? C55 C54 C53 128.2(2) . . ? C55 C54 Cr2 100.73(14) . . ? C53 C54 Cr2 130.70(17) . . ? C55 C54 Cr1 73.52(12) . . ? C53 C54 Cr1 134.42(17) . . ? Cr2 C54 Cr1 58.80(6) . . ? C54 C55 C56 124.3(2) . . ? C54 C55 C27 117.13(19) . . ? C56 C55 C27 114.51(19) . . ? C54 C55 Cr1 65.79(12) . . ? C56 C55 Cr1 125.11(16) . . ? C27 C55 Cr1 98.19(13) . . ? F5 C56 F4 105.85(19) . . ? F5 C56 F6 105.8(2) . . ? F4 C56 F6 105.11(19) . . ? F5 C56 C55 114.82(19) . . ? F4 C56 C55 113.6(2) . . ? F6 C56 C55 110.96(19) . . ? 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 Cr1 Cr2 N3 172.24(8) . . . . ? C54 Cr1 Cr2 N3 -78.55(9) . . . . ? N4 Cr1 Cr2 N3 34.30(7) . . . . ? C55 Cr1 Cr2 N3 -41.50(8) . . . . ? N1 Cr1 Cr2 N2 -0.76(8) . . . . ? C54 Cr1 Cr2 N2 108.46(10) . . . . ? N4 Cr1 Cr2 N2 -138.70(8) . . . . ? C55 Cr1 Cr2 N2 145.51(9) . . . . ? N1 Cr1 Cr2 C54 -109.22(10) . . . . ? N4 Cr1 Cr2 C54 112.85(9) . . . . ? C55 Cr1 Cr2 C54 37.05(10) . . . . ? Cr2 Cr1 N1 C1 11.73(19) . . . . ? C54 Cr1 N1 C1 -52.6(2) . . . . ? N4 Cr1 N1 C1 135.27(17) . . . . ? C55 Cr1 N1 C1 -88.4(2) . . . . ? Cr2 Cr1 N1 C8 -178.34(14) . . . . ? C54 Cr1 N1 C8 117.37(16) . . . . ? N4 Cr1 N1 C8 -54.80(18) . . . . ? C55 Cr1 N1 C8 81.6(2) . . . . ? N1 Cr1 N4 C28 -173.84(14) . . . . ? Cr2 Cr1 N4 C28 -48.86(15) . . . . ? C54 Cr1 N4 C28 14.09(17) . . . . ? C55 Cr1 N4 C28 29.30(15) . . . . ? N1 Cr1 N4 C46 3.4(2) . . . . ? Cr2 Cr1 N4 C46 128.36(16) . . . . ? C54 Cr1 N4 C46 -168.69(16) . . . . ? C55 Cr1 N4 C46 -153.48(18) . . . . ? N2 Cr2 N3 C34 -25.5(3) . . . . ? Cr1 Cr2 N3 C34 171.93(18) . . . . ? C54 Cr2 N3 C34 112.4(2) . . . . ? N2 Cr2 N3 C27 -179.34(18) . . . . ? Cr1 Cr2 N3 C27 18.09(13) . . . . ? C54 Cr2 N3 C27 -41.46(13) . . . . ? N3 Cr2 N2 C2 -172.7(2) . . . . ? Cr1 Cr2 N2 C2 -10.3(2) . . . . ? C54 Cr2 N2 C2 53.5(2) . . . . ? N3 Cr2 N2 C20 4.4(3) . . . . ? Cr1 Cr2 N2 C20 166.74(15) . . . . ? C54 Cr2 N2 C20 -129.46(17) . . . . ? C8 C3 C4 C5 0.3(3) . . . . ? C9 C3 C4 C5 179.5(2) . . . . ? C3 C4 C5 C6 1.6(4) . . . . ? C4 C5 C6 C7 -2.1(4) . . . . ? C5 C6 C7 C8 0.6(4) . . . . ? C5 C6 C7 C12 -178.9(2) . . . . ? C4 C3 C8 C7 -1.8(3) . . . . ? C9 C3 C8 C7 179.0(2) . . . . ? C4 C3 C8 N1 173.8(2) . . . . ? C9 C3 C8 N1 -5.3(3) . . . . ? C6 C7 C8 C3 1.3(3) . . . . ? C12 C7 C8 C3 -179.2(2) . . . . ? C6 C7 C8 N1 -174.2(2) . . . . ? C12 C7 C8 N1 5.3(3) . . . . ? C1 N1 C8 C3 -86.1(2) . . . . ? Cr1 N1 C8 C3 102.6(2) . . . . ? C1 N1 C8 C7 89.5(2) . . . . ? Cr1 N1 C8 C7 -81.8(2) . . . . ? C4 C3 C9 C10 -81.8(3) . . . . ? C8 C3 C9 C10 97.4(3) . . . . ? C4 C3 C9 C11 42.4(3) . . . . ? C8 C3 C9 C11 -138.5(2) . . . . ? C6 C7 C12 C13 84.3(3) . . . . ? C8 C7 C12 C13 -95.2(3) . . . . ? C6 C7 C12 C14 -40.0(3) . . . . ? C8 C7 C12 C14 140.6(2) . . . . ? C20 C19 C18 C17 1.2(6) . . . . ? C24 C19 C18 C17 176.9(4) . . . . ? C19 C18 C17 C16 0.1(8) . . . . ? C18 C17 C16 C15 -0.8(8) . . . . ? C17 C16 C15 C20 0.1(7) . . . . ? C17 C16 C15 C21 179.0(4) . . . . ? C16 C15 C20 C19 1.2(5) . . . . ? C21 C15 C20 C19 -177.6(3) . . . . ? C16 C15 C20 N2 -177.4(3) . . . . ? C21 C15 C20 N2 3.8(5) . . . . ? C18 C19 C20 C15 -1.9(5) . . . . ? C24 C19 C20 C15 -177.4(3) . . . . ? C18 C19 C20 N2 176.7(3) . . . . ? C24 C19 C20 N2 1.2(4) . . . . ? C2 N2 C20 C15 62.8(3) . . . . ? Cr2 N2 C20 C15 -114.8(3) . . . . ? C2 N2 C20 C19 -115.9(3) . . . . ? Cr2 N2 C20 C19 66.6(3) . . . . ? C18 C19 C24 C25 -80.4(4) . . . . ? C20 C19 C24 C25 95.1(4) . . . . ? C18 C19 C24 C26 44.2(5) . . . . ? C20 C19 C24 C26 -140.3(3) . . . . ? C16 C15 C21 C23 70.9(4) . . . . ? C20 C15 C21 C23 -110.3(4) . . . . ? C16 C15 C21 C22 -53.4(5) . . . . ? C20 C15 C21 C22 125.4(3) . . . . ? C34 C29 C30 C31 -0.5(5) . . . . ? C35 C29 C30 C31 -179.8(3) . . . . ? C29 C30 C31 C32 3.8(5) . . . . ? C30 C31 C32 C33 -2.1(5) . . . . ? C31 C32 C33 C34 -2.7(4) . . . . ? C31 C32 C33 C38 173.4(3) . . . . ? C30 C29 C34 N3 176.3(2) . . . . ? C35 C29 C34 N3 -4.5(4) . . . . ? C30 C29 C34 C33 -4.3(4) . . . . ? C35 C29 C34 C33 174.9(3) . . . . ? C27 N3 C34 C29 -137.0(2) . . . . ? Cr2 N3 C34 C29 71.1(3) . . . . ? C27 N3 C34 C33 43.6(3) . . . . ? Cr2 N3 C34 C33 -108.3(2) . . . . ? C32 C33 C34 C29 5.8(4) . . . . ? C38 C33 C34 C29 -170.0(3) . . . . ? C32 C33 C34 N3 -174.8(2) . . . . ? C38 C33 C34 N3 9.4(4) . . . . ? C30 C29 C35 C36 -60.6(4) . . . . ? C34 C29 C35 C36 120.1(3) . . . . ? C30 C29 C35 C37 57.9(4) . . . . ? C34 C29 C35 C37 -121.3(3) . . . . ? C32 C33 C38 C40 68.0(3) . . . . ? C34 C33 C38 C40 -116.2(3) . . . . ? C32 C33 C38 C39 -54.9(3) . . . . ? C34 C33 C38 C39 120.9(3) . . . . ? C46 C41 C42 C43 0.2(4) . . . . ? C47 C41 C42 C43 -180.0(2) . . . . ? C41 C42 C43 C44 0.1(4) . . . . ? C42 C43 C44 C45 -0.4(4) . . . . ? C43 C44 C45 C46 0.4(4) . . . . ? C43 C44 C45 C50 177.2(2) . . . . ? C42 C41 C46 C45 -0.2(4) . . . . ? C47 C41 C46 C45 179.9(2) . . . . ? C42 C41 C46 N4 179.5(2) . . . . ? C47 C41 C46 N4 -0.3(4) . . . . ? C44 C45 C46 C41 0.0(3) . . . . ? C50 C45 C46 C41 -176.8(2) . . . . ? C44 C45 C46 N4 -179.8(2) . . . . ? C50 C45 C46 N4 3.4(3) . . . . ? C28 N4 C46 C41 75.7(3) . . . . ? Cr1 N4 C46 C41 -101.4(2) . . . . ? C28 N4 C46 C45 -104.6(2) . . . . ? Cr1 N4 C46 C45 78.4(2) . . . . ? C42 C41 C47 C49 51.2(3) . . . . ? C46 C41 C47 C49 -129.0(3) . . . . ? C42 C41 C47 C48 -71.6(3) . . . . ? C46 C41 C47 C48 108.2(3) . . . . ? C44 C45 C50 C51 49.6(3) . . . . ? C46 C45 C50 C51 -133.7(2) . . . . ? C44 C45 C50 C52 -75.1(3) . . . . ? C46 C45 C50 C52 101.6(3) . . . . ? C8 N1 C1 C2 175.5(2) . . . . ? Cr1 N1 C1 C2 -13.8(3) . . . . ? N1 C1 C2 N2 1.1(4) . . . . ? C20 N2 C2 C1 -164.7(2) . . . . ? Cr2 N2 C2 C1 12.4(4) . . . . ? C34 N3 C27 C28 118.0(2) . . . . ? Cr2 N3 C27 C28 -84.68(17) . . . . ? C34 N3 C27 C55 -128.01(19) . . . . ? Cr2 N3 C27 C55 29.29(18) . . . . ? C46 N4 C28 C27 178.38(17) . . . . ? Cr1 N4 C28 C27 -4.1(2) . . . . ? N3 C27 C28 N4 78.4(2) . . . . ? C55 C27 C28 N4 -34.9(2) . . . . ? F1 C53 C54 C55 154.2(2) . . . . ? F2 C53 C54 C55 33.1(3) . . . . ? F3 C53 C54 C55 -86.6(3) . . . . ? F1 C53 C54 Cr2 -34.6(3) . . . . ? F2 C53 C54 Cr2 -155.76(17) . . . . ? F3 C53 C54 Cr2 84.6(3) . . . . ? F1 C53 C54 Cr1 48.8(3) . . . . ? F2 C53 C54 Cr1 -72.3(3) . . . . ? F3 C53 C54 Cr1 168.02(17) . . . . ? N3 Cr2 C54 C55 40.73(14) . . . . ? N2 Cr2 C54 C55 -155.97(13) . . . . ? Cr1 Cr2 C54 C55 -63.11(13) . . . . ? N3 Cr2 C54 C53 -132.2(2) . . . . ? N2 Cr2 C54 C53 31.1(2) . . . . ? Cr1 Cr2 C54 C53 123.9(2) . . . . ? N3 Cr2 C54 Cr1 103.84(7) . . . . ? N2 Cr2 C54 Cr1 -92.87(8) . . . . ? N1 Cr1 C54 C55 -149.97(12) . . . . ? Cr2 Cr1 C54 C55 113.96(13) . . . . ? N4 Cr1 C54 C55 23.21(15) . . . . ? N1 Cr1 C54 C53 -22.2(3) . . . . ? Cr2 Cr1 C54 C53 -118.3(2) . . . . ? N4 Cr1 C54 C53 151.0(2) . . . . ? C55 Cr1 C54 C53 127.7(3) . . . . ? N1 Cr1 C54 Cr2 96.07(8) . . . . ? N4 Cr1 C54 Cr2 -90.76(7) . . . . ? C55 Cr1 C54 Cr2 -113.96(13) . . . . ? C53 C54 C55 C56 -16.9(4) . . . . ? Cr2 C54 C55 C56 169.88(18) . . . . ? Cr1 C54 C55 C56 117.2(2) . . . . ? C53 C54 C55 C27 139.1(2) . . . . ? Cr2 C54 C55 C27 -34.1(2) . . . . ? Cr1 C54 C55 C27 -86.86(17) . . . . ? C53 C54 C55 Cr1 -134.1(3) . . . . ? Cr2 C54 C55 Cr1 52.71(7) . . . . ? N3 C27 C55 C54 5.2(2) . . . . ? C28 C27 C55 C54 119.6(2) . . . . ? N3 C27 C55 C56 163.48(18) . . . . ? C28 C27 C55 C56 -82.1(2) . . . . ? N3 C27 C55 Cr1 -61.75(16) . . . . ? C28 C27 C55 Cr1 52.67(17) . . . . ? N1 Cr1 C55 C54 54.6(2) . . . . ? Cr2 Cr1 C55 C54 -53.21(12) . . . . ? N4 Cr1 C55 C54 -158.85(14) . . . . ? N1 Cr1 C55 C56 -61.4(3) . . . . ? Cr2 Cr1 C55 C56 -169.2(2) . . . . ? C54 Cr1 C55 C56 -116.0(2) . . . . ? N4 Cr1 C55 C56 85.13(19) . . . . ? N1 Cr1 C55 C27 170.72(13) . . . . ? Cr2 Cr1 C55 C27 62.92(12) . . . . ? C54 Cr1 C55 C27 116.13(19) . . . . ? N4 Cr1 C55 C27 -42.72(13) . . . . ? C54 C55 C56 F5 -57.8(3) . . . . ? C27 C55 C56 F5 145.63(19) . . . . ? Cr1 C55 C56 F5 24.8(3) . . . . ? C54 C55 C56 F4 64.2(3) . . . . ? C27 C55 C56 F4 -92.4(2) . . . . ? Cr1 C55 C56 F4 146.84(17) . . . . ? C54 C55 C56 F6 -177.7(2) . . . . ? C27 C55 C56 F6 25.8(3) . . . . ? Cr1 C55 C56 F6 -95.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.568 _refine_diff_density_min -0.260 _refine_diff_density_rms 0.066 # SQUEEZE RESULTS (APPEND TO CIF) 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 0.000 0.500 -0.037 2605.3 494.2 2 0.500 1.000 0.036 2605.3 494.2 _platon_squeeze_details ; - PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13 Void space analysis consistent with initial solutions displaying 2.5 severely disordered toluene molecules of solvation per compound molecule. ; # start Validation Reply Form _vrf_CHEMW03_klat839s ; PROBLEM: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.95 <> 1.05 RESPONSE: Data-set was treated with SQUEEZE to model 2.5 toluene molecule of solvation per compound molecule as diffused contributions. ; _vrf_PLAT043_klat839s ; PROBLEM: Check Reported Molecular Weight .............. 1249.51 RESPONSE: See response to CHEMW03 ; _vrf_PLAT049_klat839s ; PROBLEM: Calculated Density less than 1.0 gcm-3 ........ 0.9381 RESPONSE: See response to CHEMW03 ;