data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H48 Mo N6 O4' _chemical_formula_sum 'C38 H48 Mo N6 O4 ' _chemical_formula_weight 748.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 '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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.8445(8) _cell_length_b 13.5010(10) _cell_length_c 25.2225(18) _cell_angle_alpha 90.00 _cell_angle_beta 95.156(2) _cell_angle_gamma 90.00 _cell_volume 3677.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 31.3 _exptl_crystal_description block _exptl_crystal_colour Ink-blue _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568.0 _exptl_absorpt_coefficient_mu 0.404 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.930 _exptl_absorpt_correction_T_max 0.945 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56191 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 31.30 _reflns_number_total 11608 _reflns_number_gt 9021 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III' _computing_publication_material 'WinGX v1.70.01' _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^)+(0.0325P)^2^+2.1285P] 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 constrn _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11608 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0832 _refine_ls_wR_factor_gt 0.0759 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.005 _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 Mo1 Mo 0.521299(12) 0.440653(10) 0.792616(6) 0.01550(4) Uani 1 1 d . . . N5 N 0.82269(13) 0.44091(11) 0.82267(6) 0.0213(3) Uani 1 1 d . . . O1 O 0.58652(10) 0.31215(9) 0.83769(5) 0.0188(2) Uani 1 1 d . . . N3 N 0.35747(12) 0.36282(10) 0.83467(6) 0.0173(3) Uani 1 1 d . . . O2 O 0.50503(10) 0.51373(9) 0.86736(5) 0.0186(2) Uani 1 1 d . . . N1 N 0.33472(13) 0.52759(11) 0.78856(6) 0.0181(3) Uani 1 1 d . . . N4 N 0.68908(13) 0.37445(11) 0.75229(6) 0.0192(3) Uani 1 1 d . . . C2 C 0.21707(18) 0.67431(14) 0.76781(8) 0.0276(4) Uani 1 1 d . . . H2 H 0.2135 0.7381 0.7539 0.033 Uiso 1 1 calc R . . N6 N 0.71971(13) 0.46995(10) 0.83802(6) 0.0177(3) Uani 1 1 d . . . C29 C 0.58648(15) 0.62224(13) 0.93731(7) 0.0185(3) Uani 1 1 d . . . N2 N 0.24598(13) 0.39364(11) 0.83202(6) 0.0209(3) Uani 1 1 d . . . C30 C 0.59967(15) 0.55438(12) 0.89445(6) 0.0168(3) Uani 1 1 d . . . C26 C 0.82821(15) 0.57029(13) 0.90989(7) 0.0203(3) Uani 1 1 d . . . H26 H 0.9063 0.5517 0.9010 0.024 Uiso 1 1 calc R . . C27 C 0.81610(16) 0.63572(13) 0.95040(7) 0.0217(4) Uani 1 1 d . . . C8 C 0.33045(16) 0.10576(13) 0.88163(7) 0.0193(3) Uani 1 1 d . . . C25 C 0.72094(15) 0.53114(12) 0.88168(7) 0.0173(3) Uani 1 1 d . . . C5 C 0.23615(15) 0.48892(13) 0.81005(7) 0.0201(3) Uani 1 1 d . . . C23 C 0.90634(17) 0.33798(14) 0.75646(8) 0.0265(4) Uani 1 1 d . . . H23 H 0.9852 0.3446 0.7739 0.032 Uiso 1 1 calc R . . C6 C 0.38318(15) 0.26868(12) 0.85311(6) 0.0167(3) Uani 1 1 d . . . C11 C 0.51083(15) 0.24556(12) 0.85311(6) 0.0163(3) Uani 1 1 d . . . C16 C 0.24152(17) 0.02195(14) 0.89277(8) 0.0250(4) Uani 1 1 d . . . C24 C 0.80456(16) 0.38302(13) 0.77639(7) 0.0202(3) Uani 1 1 d . . . C9 C 0.45968(16) 0.08417(13) 0.88352(7) 0.0201(3) Uani 1 1 d . . . H9 H 0.4848 0.0213 0.8950 0.024 Uiso 1 1 calc R . . C10 C 0.55006(15) 0.14815(13) 0.86991(6) 0.0179(3) Uani 1 1 d . . . C7 C 0.29382(15) 0.19941(13) 0.86709(7) 0.0189(3) Uani 1 1 d . . . H7 H 0.2109 0.2175 0.8664 0.023 Uiso 1 1 calc R . . C35 C 0.92568(17) 0.68686(16) 0.98187(8) 0.0305(4) Uani 1 1 d . . . C4 C 0.12434(17) 0.53928(14) 0.81036(8) 0.0280(4) Uani 1 1 d . . . H4 H 0.0570 0.5102 0.8247 0.034 Uiso 1 1 calc R . . C12 C 0.68536(16) 0.11628(13) 0.86836(7) 0.0222(4) Uani 1 1 d . . . C3 C 0.11558(18) 0.63349(15) 0.78896(8) 0.0307(4) Uani 1 1 d . . . H3 H 0.0421 0.6690 0.7888 0.037 Uiso 1 1 calc R . . C1 C 0.32436(17) 0.61859(13) 0.76766(7) 0.0226(4) Uani 1 1 d . . . H1 H 0.3918 0.6455 0.7524 0.027 Uiso 1 1 calc R . . C28 C 0.69412(16) 0.65978(14) 0.96276(7) 0.0224(4) Uani 1 1 d . . . H28 H 0.6865 0.7045 0.9903 0.027 Uiso 1 1 calc R . . C21 C 0.76989(19) 0.27597(14) 0.68486(8) 0.0279(4) Uani 1 1 d . . . H21 H 0.7558 0.2404 0.6533 0.033 Uiso 1 1 calc R . . C22 C 0.88744(19) 0.28348(15) 0.71030(8) 0.0294(4) Uani 1 1 d . . . H22 H 0.9536 0.2519 0.6964 0.035 Uiso 1 1 calc R . . C31 C 0.45826(16) 0.65527(15) 0.95150(7) 0.0252(4) Uani 1 1 d . . . C20 C 0.67313(17) 0.32254(13) 0.70719(7) 0.0232(4) Uani 1 1 d . . . H20 H 0.5938 0.3174 0.6900 0.028 Uiso 1 1 calc R . . O3 O 0.56349(11) 0.54688(9) 0.76208(5) 0.0222(3) Uani 1 1 d . . . O4 O 0.44532(11) 0.37211(9) 0.74254(5) 0.0215(3) Uani 1 1 d . . . C17 C 0.2563(2) -0.06195(15) 0.85262(9) 0.0354(5) Uani 1 1 d . . . H17A H 0.2008 -0.1151 0.8592 0.053 Uiso 1 1 calc R . . H17B H 0.3400 -0.0858 0.8565 0.053 Uiso 1 1 calc R . . H17C H 0.2371 -0.0374 0.8171 0.053 Uiso 1 1 calc R . . C14 C 0.71631(19) 0.11674(16) 0.81019(8) 0.0315(4) Uani 1 1 d . . . H14A H 0.7027 0.1818 0.7955 0.047 Uiso 1 1 calc R . . H14B H 0.6641 0.0701 0.7901 0.047 Uiso 1 1 calc R . . H14C H 0.8015 0.0985 0.8086 0.047 Uiso 1 1 calc R . . C13 C 0.77312(17) 0.18601(16) 0.90165(8) 0.0314(4) Uani 1 1 d . . . H13A H 0.7610 0.2527 0.8890 0.047 Uiso 1 1 calc R . . H13B H 0.8573 0.1664 0.8985 0.047 Uiso 1 1 calc R . . H13C H 0.7560 0.1826 0.9383 0.047 Uiso 1 1 calc R . . C19 C 0.10610(18) 0.05633(16) 0.88703(10) 0.0377(5) Uani 1 1 d . . . H19A H 0.0532 0.0019 0.8943 0.057 Uiso 1 1 calc R . . H19B H 0.0850 0.0797 0.8514 0.057 Uiso 1 1 calc R . . H19C H 0.0954 0.1090 0.9118 0.057 Uiso 1 1 calc R . . C18 C 0.2722(2) -0.01708(17) 0.94960(8) 0.0350(5) Uani 1 1 d . . . H18A H 0.2162 -0.0697 0.9564 0.052 Uiso 1 1 calc R . . H18B H 0.2640 0.0356 0.9746 0.052 Uiso 1 1 calc R . . H18C H 0.3556 -0.0416 0.9533 0.052 Uiso 1 1 calc R . . C32 C 0.37509(19) 0.56599(18) 0.96160(10) 0.0420(6) Uani 1 1 d . . . H32A H 0.3688 0.5236 0.9309 0.063 Uiso 1 1 calc R . . H32B H 0.2941 0.5890 0.9682 0.063 Uiso 1 1 calc R . . H32C H 0.4105 0.5297 0.9920 0.063 Uiso 1 1 calc R . . C33 C 0.39694(19) 0.71451(16) 0.90455(9) 0.0351(5) Uani 1 1 d . . . H33A H 0.3906 0.6739 0.8732 0.053 Uiso 1 1 calc R . . H33B H 0.4460 0.7720 0.8987 0.053 Uiso 1 1 calc R . . H33C H 0.3157 0.7348 0.9124 0.053 Uiso 1 1 calc R . . C15 C 0.70828(19) 0.01148(15) 0.89011(9) 0.0329(5) Uani 1 1 d . . . H15A H 0.7938 -0.0056 0.8885 0.049 Uiso 1 1 calc R . . H15B H 0.6571 -0.0345 0.8691 0.049 Uiso 1 1 calc R . . H15C H 0.6884 0.0088 0.9264 0.049 Uiso 1 1 calc R . . C38 C 0.9157(2) 0.79882(17) 0.97242(11) 0.0456(6) Uani 1 1 d . . . H38A H 0.8378 0.8222 0.9828 0.068 Uiso 1 1 calc R . . H38B H 0.9211 0.8126 0.9354 0.068 Uiso 1 1 calc R . . H38C H 0.9820 0.8318 0.9932 0.068 Uiso 1 1 calc R . . C37 C 0.9218(2) 0.6643(2) 1.04170(9) 0.0449(6) Uani 1 1 d . . . H37A H 0.8441 0.6860 1.0531 0.067 Uiso 1 1 calc R . . H37B H 0.9882 0.6985 1.0617 0.067 Uiso 1 1 calc R . . H37C H 0.9306 0.5943 1.0475 0.067 Uiso 1 1 calc R . . C34 C 0.4670(2) 0.7215(3) 1.00064(11) 0.0657(10) Uani 1 1 d . . . H34A H 0.5053 0.6855 1.0306 0.099 Uiso 1 1 calc R . . H34B H 0.3855 0.7418 1.0080 0.099 Uiso 1 1 calc R . . H34C H 0.5158 0.7789 0.9943 0.099 Uiso 1 1 calc R . . C36 C 1.04950(19) 0.6516(2) 0.96519(11) 0.0547(8) Uani 1 1 d . . . H36A H 1.0571 0.5815 0.9709 0.082 Uiso 1 1 calc R . . H36B H 1.1153 0.6851 0.9860 0.082 Uiso 1 1 calc R . . H36C H 1.0544 0.6660 0.9282 0.082 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 Mo1 0.01379(7) 0.01349(7) 0.01933(7) -0.00078(6) 0.00199(5) -0.00076(5) N5 0.0153(7) 0.0209(7) 0.0284(8) -0.0049(6) 0.0059(5) 0.0006(6) O1 0.0138(5) 0.0175(6) 0.0251(6) 0.0008(5) 0.0021(4) -0.0003(4) N3 0.0144(6) 0.0161(7) 0.0212(7) -0.0013(5) 0.0011(5) 0.0002(5) O2 0.0127(5) 0.0206(6) 0.0227(6) -0.0038(5) 0.0023(4) -0.0011(4) N1 0.0179(7) 0.0153(7) 0.0205(7) -0.0011(5) -0.0012(5) 0.0009(5) N4 0.0211(7) 0.0161(7) 0.0209(7) -0.0005(6) 0.0054(5) -0.0004(5) C2 0.0338(10) 0.0192(9) 0.0286(10) 0.0024(7) -0.0047(8) 0.0067(8) N6 0.0164(7) 0.0152(7) 0.0219(7) -0.0018(5) 0.0045(5) 0.0000(5) C29 0.0163(8) 0.0213(9) 0.0183(8) 0.0003(6) 0.0030(6) 0.0036(6) N2 0.0147(7) 0.0184(8) 0.0297(8) 0.0001(6) 0.0026(6) 0.0012(5) C30 0.0155(7) 0.0155(8) 0.0196(8) 0.0017(6) 0.0023(6) -0.0005(6) C26 0.0142(7) 0.0200(9) 0.0266(9) -0.0030(7) 0.0020(6) 0.0011(6) C27 0.0173(8) 0.0209(9) 0.0264(9) -0.0043(7) -0.0005(6) 0.0000(6) C8 0.0213(8) 0.0182(9) 0.0183(8) 0.0012(6) 0.0013(6) -0.0022(6) C25 0.0158(8) 0.0143(8) 0.0220(8) -0.0014(6) 0.0032(6) 0.0004(6) C5 0.0162(8) 0.0174(8) 0.0259(9) -0.0015(7) -0.0016(6) 0.0009(6) C23 0.0215(9) 0.0269(10) 0.0324(10) -0.0027(8) 0.0087(7) 0.0044(7) C6 0.0163(8) 0.0136(8) 0.0199(8) -0.0009(6) 0.0009(6) 0.0000(6) C11 0.0166(8) 0.0164(8) 0.0159(7) -0.0021(6) 0.0014(6) 0.0009(6) C16 0.0246(9) 0.0200(9) 0.0301(10) 0.0069(7) -0.0002(7) -0.0041(7) C24 0.0207(8) 0.0159(8) 0.0251(9) -0.0015(7) 0.0070(7) -0.0010(6) C9 0.0246(9) 0.0149(8) 0.0207(8) 0.0018(6) 0.0012(6) 0.0026(6) C10 0.0186(8) 0.0180(8) 0.0171(8) -0.0016(6) 0.0006(6) 0.0030(6) C7 0.0158(8) 0.0185(8) 0.0224(8) -0.0013(6) 0.0022(6) -0.0010(6) C35 0.0199(9) 0.0319(11) 0.0388(11) -0.0153(9) -0.0026(8) -0.0011(8) C4 0.0183(9) 0.0253(10) 0.0402(11) -0.0007(8) 0.0017(7) 0.0036(7) C12 0.0194(8) 0.0204(9) 0.0269(9) 0.0005(7) 0.0030(7) 0.0060(7) C3 0.0240(9) 0.0269(10) 0.0401(11) -0.0007(8) -0.0035(8) 0.0112(8) C1 0.0255(9) 0.0200(9) 0.0215(8) 0.0015(7) -0.0030(7) 0.0014(7) C28 0.0226(9) 0.0231(9) 0.0212(8) -0.0054(7) 0.0008(7) 0.0034(7) C21 0.0394(11) 0.0217(10) 0.0236(9) -0.0043(7) 0.0082(8) 0.0019(8) C22 0.0329(10) 0.0261(10) 0.0313(10) -0.0020(8) 0.0136(8) 0.0088(8) C31 0.0178(8) 0.0362(11) 0.0220(9) -0.0053(8) 0.0037(7) 0.0071(7) C20 0.0274(9) 0.0194(9) 0.0232(9) -0.0015(7) 0.0047(7) -0.0004(7) O3 0.0213(6) 0.0173(6) 0.0288(7) 0.0018(5) 0.0073(5) -0.0003(5) O4 0.0198(6) 0.0208(6) 0.0234(6) -0.0038(5) -0.0002(5) -0.0006(5) C17 0.0437(12) 0.0232(10) 0.0372(11) 0.0024(9) -0.0083(9) -0.0065(9) C14 0.0323(10) 0.0307(11) 0.0335(11) -0.0015(8) 0.0137(8) 0.0100(8) C13 0.0182(9) 0.0337(11) 0.0411(11) -0.0050(9) -0.0033(8) 0.0063(8) C19 0.0236(10) 0.0307(11) 0.0588(14) 0.0146(10) 0.0029(9) -0.0085(8) C18 0.0402(12) 0.0339(12) 0.0313(11) 0.0115(9) 0.0056(9) -0.0048(9) C32 0.0228(10) 0.0546(15) 0.0512(14) 0.0214(12) 0.0179(9) 0.0100(10) C33 0.0279(10) 0.0340(12) 0.0439(12) 0.0057(9) 0.0054(9) 0.0146(9) C15 0.0277(10) 0.0272(11) 0.0439(12) 0.0054(9) 0.0039(9) 0.0116(8) C38 0.0422(13) 0.0329(13) 0.0604(16) -0.0133(11) -0.0031(11) -0.0116(10) C37 0.0386(12) 0.0514(15) 0.0413(13) -0.0120(11) -0.0152(10) -0.0013(11) C34 0.0291(12) 0.117(3) 0.0509(15) -0.0511(17) 0.0012(11) 0.0217(14) C36 0.0183(10) 0.0653(18) 0.0799(19) -0.0430(15) 0.0005(11) -0.0056(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O3 1.7096(12) . ? Mo1 O4 1.7156(12) . ? Mo1 O2 2.1491(12) . ? Mo1 O1 2.1583(12) . ? Mo1 N1 2.3334(14) . ? Mo1 N4 2.3402(14) . ? Mo1 N6 2.3780(14) . ? Mo1 N3 2.3925(14) . ? N5 N6 1.2762(19) . ? N5 C24 1.404(2) . ? O1 C11 1.300(2) . ? N3 N2 1.2747(19) . ? N3 C6 1.373(2) . ? O2 C30 1.3021(19) . ? N1 C1 1.338(2) . ? N1 C5 1.347(2) . ? N4 C20 1.334(2) . ? N4 C24 1.347(2) . ? C2 C3 1.380(3) . ? C2 C1 1.386(3) . ? N6 C25 1.376(2) . ? C29 C28 1.377(2) . ? C29 C30 1.434(2) . ? C29 C31 1.533(2) . ? N2 C5 1.401(2) . ? C30 C25 1.417(2) . ? C26 C27 1.366(2) . ? C26 C25 1.411(2) . ? C27 C28 1.424(2) . ? C27 C35 1.533(2) . ? C8 C7 1.366(2) . ? C8 C9 1.428(2) . ? C8 C16 1.529(2) . ? C5 C4 1.391(2) . ? C23 C22 1.377(3) . ? C23 C24 1.393(2) . ? C6 C7 1.414(2) . ? C6 C11 1.419(2) . ? C11 C10 1.435(2) . ? C16 C19 1.535(3) . ? C16 C18 1.535(3) . ? C16 C17 1.537(3) . ? C9 C10 1.373(2) . ? C10 C12 1.533(2) . ? C35 C36 1.519(3) . ? C35 C38 1.533(3) . ? C35 C37 1.544(3) . ? C4 C3 1.382(3) . ? C12 C15 1.530(3) . ? C12 C14 1.534(3) . ? C12 C13 1.534(3) . ? C21 C22 1.378(3) . ? C21 C20 1.386(3) . ? C31 C34 1.524(3) . ? C31 C33 1.531(3) . ? C31 C32 1.540(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 O3 Mo1 O4 104.55(6) . . ? O3 Mo1 O2 93.24(5) . . ? O4 Mo1 O2 145.24(5) . . ? O3 Mo1 O1 145.42(5) . . ? O4 Mo1 O1 93.85(5) . . ? O2 Mo1 O1 87.47(5) . . ? O3 Mo1 N1 79.88(5) . . ? O4 Mo1 N1 83.22(5) . . ? O2 Mo1 N1 70.63(5) . . ? O1 Mo1 N1 132.01(5) . . ? O3 Mo1 N4 82.80(5) . . ? O4 Mo1 N4 79.33(5) . . ? O2 Mo1 N4 133.23(5) . . ? O1 Mo1 N4 72.01(5) . . ? N1 Mo1 N4 151.41(5) . . ? O3 Mo1 N6 79.06(6) . . ? O4 Mo1 N6 142.96(5) . . ? O2 Mo1 N6 69.10(4) . . ? O1 Mo1 N6 68.93(5) . . ? N1 Mo1 N6 132.92(5) . . ? N4 Mo1 N6 64.38(5) . . ? O3 Mo1 N3 143.86(5) . . ? O4 Mo1 N3 76.28(5) . . ? O2 Mo1 N3 71.94(5) . . ? O1 Mo1 N3 68.57(5) . . ? N1 Mo1 N3 64.21(5) . . ? N4 Mo1 N3 131.47(5) . . ? N6 Mo1 N3 122.37(5) . . ? N6 N5 C24 111.25(14) . . ? C11 O1 Mo1 121.84(10) . . ? N2 N3 C6 118.85(14) . . ? N2 N3 Mo1 124.89(11) . . ? C6 N3 Mo1 114.86(10) . . ? C30 O2 Mo1 122.06(10) . . ? C1 N1 C5 118.24(15) . . ? C1 N1 Mo1 121.41(12) . . ? C5 N1 Mo1 120.25(11) . . ? C20 N4 C24 118.29(15) . . ? C20 N4 Mo1 121.67(12) . . ? C24 N4 Mo1 119.91(11) . . ? C3 C2 C1 118.89(18) . . ? N5 N6 C25 118.79(14) . . ? N5 N6 Mo1 125.55(11) . . ? C25 N6 Mo1 115.38(10) . . ? C28 C29 C30 116.66(15) . . ? C28 C29 C31 122.18(16) . . ? C30 C29 C31 121.06(15) . . ? N3 N2 C5 111.01(14) . . ? O2 C30 C25 119.42(15) . . ? O2 C30 C29 122.52(15) . . ? C25 C30 C29 118.06(15) . . ? C27 C26 C25 119.29(16) . . ? C26 C27 C28 117.72(16) . . ? C26 C27 C35 123.81(16) . . ? C28 C27 C35 118.44(16) . . ? C7 C8 C9 117.32(16) . . ? C7 C8 C16 124.16(16) . . ? C9 C8 C16 118.43(16) . . ? N6 C25 C26 125.24(15) . . ? N6 C25 C30 111.87(14) . . ? C26 C25 C30 122.85(15) . . ? N1 C5 C4 122.46(17) . . ? N1 C5 N2 118.71(15) . . ? C4 C5 N2 118.82(16) . . ? C22 C23 C24 118.41(18) . . ? N3 C6 C7 125.01(15) . . ? N3 C6 C11 111.83(14) . . ? C7 C6 C11 123.02(15) . . ? O1 C11 C6 119.34(15) . . ? O1 C11 C10 122.94(14) . . ? C6 C11 C10 117.71(15) . . ? C8 C16 C19 111.89(15) . . ? C8 C16 C18 109.76(15) . . ? C19 C16 C18 108.49(17) . . ? C8 C16 C17 108.65(16) . . ? C19 C16 C17 108.42(17) . . ? C18 C16 C17 109.60(16) . . ? N4 C24 C23 122.30(16) . . ? N4 C24 N5 118.56(15) . . ? C23 C24 N5 119.13(16) . . ? C10 C9 C8 125.71(16) . . ? C9 C10 C11 116.82(15) . . ? C9 C10 C12 122.43(15) . . ? C11 C10 C12 120.60(15) . . ? C8 C7 C6 119.34(15) . . ? C36 C35 C38 108.5(2) . . ? C36 C35 C27 112.27(16) . . ? C38 C35 C27 108.86(17) . . ? C36 C35 C37 108.15(19) . . ? C38 C35 C37 109.82(18) . . ? C27 C35 C37 109.21(17) . . ? C3 C4 C5 118.50(18) . . ? C15 C12 C10 112.06(15) . . ? C15 C12 C14 107.71(16) . . ? C10 C12 C14 108.38(14) . . ? C15 C12 C13 107.37(15) . . ? C10 C12 C13 111.22(14) . . ? C14 C12 C13 110.04(16) . . ? C2 C3 C4 119.30(18) . . ? N1 C1 C2 122.57(18) . . ? C29 C28 C27 125.40(16) . . ? C22 C21 C20 118.67(17) . . ? C23 C22 C21 119.61(17) . . ? C34 C31 C33 108.28(19) . . ? C34 C31 C29 111.65(16) . . ? C33 C31 C29 108.14(15) . . ? C34 C31 C32 108.6(2) . . ? C33 C31 C32 108.46(17) . . ? C29 C31 C32 111.59(16) . . ? N4 C20 C21 122.70(17) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 31.30 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.545 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.075 #END=== data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H48 Cr N6 O2' _chemical_formula_weight 672.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 18.210(3) _cell_length_b 15.258(2) _cell_length_c 17.196(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.908(4) _cell_angle_gamma 90.00 _cell_volume 4367.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 23.8 _exptl_crystal_description palate _exptl_crystal_colour green _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.023 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.296 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.9542 _exptl_absorpt_correction_T_max 0.9767 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22665 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.0273 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 23.77 _reflns_number_total 3330 _reflns_number_gt 2749 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX-2' _computing_cell_refinement 'Bruker APEX-2' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III' _computing_publication_material 'WinGX v1.70.01' _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^)+(0.0659P)^2^+0.8228P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3330 _refine_ls_number_parameters 213 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.1113 _refine_ls_wR_factor_gt 0.1050 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 0.0000 0.11100(3) 0.7500 0.04118(18) Uani 1 2 d S . . O1 O 0.01660(8) 0.20157(8) 0.67741(9) 0.0464(4) Uani 1 1 d . . . N1 N 0.03358(11) 0.01861(10) 0.84431(11) 0.0464(4) Uani 1 1 d . . . N3 N 0.11591(10) 0.09927(10) 0.78513(10) 0.0421(4) Uani 1 1 d . . . N2 N 0.16084(10) 0.04217(11) 0.84260(11) 0.0521(5) Uani 1 1 d . . . C10 C 0.11909(12) 0.27552(12) 0.64570(12) 0.0421(5) Uani 1 1 d . . . C6 C 0.14907(11) 0.15076(12) 0.74201(12) 0.0406(5) Uani 1 1 d . . . C7 C 0.22898(12) 0.14787(13) 0.75092(13) 0.0457(5) Uani 1 1 d . . . H7 H 0.2643 0.1065 0.7862 0.055 Uiso 1 1 calc R . . C11 C 0.09145(11) 0.20987(12) 0.68637(12) 0.0404(5) Uani 1 1 d . . . C5 C 0.11374(13) 0.00013(13) 0.87632(13) 0.0484(5) Uani 1 1 d . . . C8 C 0.25438(12) 0.20661(13) 0.70713(12) 0.0454(5) Uani 1 1 d . . . C16 C 0.06314(13) 0.34900(13) 0.59473(13) 0.0509(5) Uani 1 1 d . . . C9 C 0.19838(12) 0.27009(13) 0.65719(12) 0.0461(5) Uani 1 1 d . . . H9 H 0.2167 0.3117 0.6298 0.055 Uiso 1 1 calc R . . C2 C 0.02010(18) -0.08189(16) 0.94428(16) 0.0664(7) Uani 1 1 d . . . H2 H -0.0129 -0.1093 0.9664 0.080 Uiso 1 1 calc R . . C1 C -0.01156(15) -0.02326(14) 0.87852(15) 0.0576(6) Uani 1 1 d . . . H1 H -0.0664 -0.0119 0.8566 0.069 Uiso 1 1 calc R . . C4 C 0.14834(16) -0.05860(16) 0.94369(15) 0.0665(7) Uani 1 1 d . . . H4 H 0.2032 -0.0697 0.9656 0.080 Uiso 1 1 calc R . . C12 C 0.34033(12) 0.20770(16) 0.71193(14) 0.0566(6) Uani 1 1 d . . . C19 C 0.02864(16) 0.39635(14) 0.65138(16) 0.0655(7) Uani 1 1 d . . . H19A H -0.0065 0.4425 0.6196 0.098 Uiso 1 1 calc R . . H19B H 0.0718 0.4207 0.7000 0.098 Uiso 1 1 calc R . . H19C H -0.0009 0.3554 0.6700 0.098 Uiso 1 1 calc R . . C17 C 0.10773(17) 0.41722(17) 0.56404(18) 0.0802(8) Uani 1 1 d . . . H17A H 0.0709 0.4623 0.5325 0.120 Uiso 1 1 calc R . . H17B H 0.1296 0.3892 0.5282 0.120 Uiso 1 1 calc R . . H17C H 0.1505 0.4427 0.6123 0.120 Uiso 1 1 calc R . . C18 C -0.00582(15) 0.31113(16) 0.51656(15) 0.0716(7) Uani 1 1 d . . . H18A H -0.0406 0.3577 0.4852 0.107 Uiso 1 1 calc R . . H18B H -0.0357 0.2701 0.5346 0.107 Uiso 1 1 calc R . . H18C H 0.0157 0.2819 0.4810 0.107 Uiso 1 1 calc R . . C3 C 0.10095(18) -0.09976(16) 0.97722(16) 0.0716(7) Uani 1 1 d . . . H3 H 0.1232 -0.1393 1.0218 0.086 Uiso 1 1 calc R . . C14 C 0.33827(16) 0.1975(2) 0.62330(17) 0.0853(9) Uani 1 1 d . . . H14A H 0.3921 0.1976 0.6265 0.128 Uiso 1 1 calc R . . H14B H 0.3088 0.2453 0.5882 0.128 Uiso 1 1 calc R . . H14C H 0.3126 0.1432 0.5991 0.128 Uiso 1 1 calc R . . C13 C 0.39047(15) 0.1330(2) 0.7678(2) 0.0922(10) Uani 1 1 d . . . H13A H 0.4438 0.1350 0.7695 0.138 Uiso 1 1 calc R . . H13B H 0.3660 0.0778 0.7446 0.138 Uiso 1 1 calc R . . H13C H 0.3930 0.1393 0.8244 0.138 Uiso 1 1 calc R . . C15 C 0.37998(16) 0.2948(2) 0.7514(2) 0.0968(10) Uani 1 1 d . . . H15A H 0.4340 0.2961 0.7550 0.145 Uiso 1 1 calc R . . H15B H 0.3808 0.3003 0.8073 0.145 Uiso 1 1 calc R . . H15C H 0.3500 0.3425 0.7165 0.145 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 0.0416(3) 0.0355(3) 0.0506(3) 0.000 0.0229(2) 0.000 O1 0.0383(8) 0.0434(8) 0.0589(9) 0.0105(6) 0.0210(7) 0.0054(6) N1 0.0580(11) 0.0369(9) 0.0523(10) -0.0030(8) 0.0306(9) -0.0052(8) N3 0.0434(10) 0.0369(9) 0.0494(10) 0.0061(7) 0.0225(8) 0.0029(7) N2 0.0487(11) 0.0504(10) 0.0581(11) 0.0172(9) 0.0225(9) 0.0076(8) C10 0.0509(13) 0.0367(10) 0.0407(11) 0.0021(9) 0.0205(9) -0.0009(9) C6 0.0393(11) 0.0388(11) 0.0471(11) 0.0026(9) 0.0211(9) -0.0008(9) C7 0.0395(11) 0.0476(12) 0.0503(12) 0.0037(9) 0.0187(9) 0.0014(9) C11 0.0407(12) 0.0365(11) 0.0451(11) 0.0007(8) 0.0187(9) 0.0013(9) C5 0.0551(14) 0.0408(12) 0.0531(12) 0.0058(10) 0.0258(11) 0.0033(10) C8 0.0409(11) 0.0525(12) 0.0447(11) -0.0017(9) 0.0192(9) -0.0054(9) C16 0.0623(14) 0.0408(11) 0.0537(12) 0.0103(10) 0.0277(11) 0.0085(10) C9 0.0496(13) 0.0463(12) 0.0483(12) 0.0018(9) 0.0260(10) -0.0071(9) C2 0.093(2) 0.0522(14) 0.0722(16) 0.0057(12) 0.0527(16) -0.0086(13) C1 0.0677(15) 0.0509(13) 0.0660(14) -0.0040(11) 0.0392(13) -0.0095(11) C4 0.0732(17) 0.0592(15) 0.0686(16) 0.0192(12) 0.0304(13) 0.0067(12) C12 0.0404(12) 0.0749(16) 0.0577(13) 0.0001(11) 0.0230(11) -0.0086(11) C19 0.0870(19) 0.0441(13) 0.0732(16) 0.0042(11) 0.0405(14) 0.0157(12) C17 0.097(2) 0.0586(15) 0.098(2) 0.0325(14) 0.0530(17) 0.0152(14) C18 0.0816(18) 0.0667(16) 0.0545(14) 0.0089(12) 0.0152(13) 0.0211(13) C3 0.104(2) 0.0539(15) 0.0633(16) 0.0153(12) 0.0399(16) 0.0027(14) C14 0.0647(17) 0.127(3) 0.0769(18) -0.0017(17) 0.0415(15) -0.0015(16) C13 0.0435(14) 0.131(3) 0.104(2) 0.034(2) 0.0324(15) 0.0150(16) C15 0.0651(18) 0.116(2) 0.114(2) -0.026(2) 0.0415(17) -0.0407(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 N3 1.9541(16) 2_556 ? Cr1 N3 1.9541(16) . ? Cr1 O1 1.9659(13) 2_556 ? Cr1 O1 1.9659(13) . ? Cr1 N1 2.0463(17) 2_556 ? Cr1 N1 2.0463(17) . ? O1 C11 1.314(2) . ? N1 C1 1.350(3) . ? N1 C5 1.365(3) . ? N3 N2 1.323(2) . ? N3 C6 1.376(2) . ? N2 C5 1.373(3) . ? C10 C9 1.378(3) . ? C10 C11 1.425(3) . ? C10 C16 1.529(3) . ? C6 C7 1.401(3) . ? C6 C11 1.420(3) . ? C7 C8 1.366(3) . ? C7 H7 0.9300 . ? C5 C4 1.397(3) . ? C8 C9 1.416(3) . ? C8 C12 1.534(3) . ? C16 C18 1.533(3) . ? C16 C19 1.537(3) . ? C16 C17 1.539(3) . ? C9 H9 0.9300 . ? C2 C1 1.372(3) . ? C2 C3 1.374(4) . ? C2 H2 0.9300 . ? C1 H1 0.9300 . ? C4 C3 1.369(3) . ? C4 H4 0.9300 . ? C12 C14 1.517(3) . ? C12 C13 1.531(3) . ? C12 C15 1.533(4) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C3 H3 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cr1 N3 169.49(9) 2_556 . ? N3 Cr1 O1 80.55(6) 2_556 2_556 ? N3 Cr1 O1 107.03(6) . 2_556 ? N3 Cr1 O1 107.03(6) 2_556 . ? N3 Cr1 O1 80.55(6) . . ? O1 Cr1 O1 90.68(8) 2_556 . ? N3 Cr1 N1 75.73(7) 2_556 2_556 ? N3 Cr1 N1 96.91(7) . 2_556 ? O1 Cr1 N1 156.06(6) 2_556 2_556 ? O1 Cr1 N1 93.12(6) . 2_556 ? N3 Cr1 N1 96.91(7) 2_556 . ? N3 Cr1 N1 75.73(7) . . ? O1 Cr1 N1 93.12(6) 2_556 . ? O1 Cr1 N1 156.06(6) . . ? N1 Cr1 N1 92.92(9) 2_556 . ? C11 O1 Cr1 114.36(11) . . ? C1 N1 C5 117.86(19) . . ? C1 N1 Cr1 129.22(16) . . ? C5 N1 Cr1 112.91(13) . . ? N2 N3 C6 120.31(16) . . ? N2 N3 Cr1 123.70(13) . . ? C6 N3 Cr1 115.85(12) . . ? N3 N2 C5 108.66(16) . . ? C9 C10 C11 116.43(18) . . ? C9 C10 C16 122.83(17) . . ? C11 C10 C16 120.71(18) . . ? N3 C6 C7 125.90(17) . . ? N3 C6 C11 111.09(16) . . ? C7 C6 C11 123.01(18) . . ? C8 C7 C6 119.20(18) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? O1 C11 C6 117.76(17) . . ? O1 C11 C10 124.47(17) . . ? C6 C11 C10 117.75(17) . . ? N1 C5 N2 118.83(17) . . ? N1 C5 C4 121.1(2) . . ? N2 C5 C4 120.1(2) . . ? C7 C8 C9 117.48(18) . . ? C7 C8 C12 122.93(19) . . ? C9 C8 C12 119.57(18) . . ? C10 C16 C18 110.18(17) . . ? C10 C16 C19 109.26(17) . . ? C18 C16 C19 109.45(19) . . ? C10 C16 C17 111.76(18) . . ? C18 C16 C17 108.2(2) . . ? C19 C16 C17 107.91(19) . . ? C10 C9 C8 125.67(18) . . ? C10 C9 H9 117.2 . . ? C8 C9 H9 117.2 . . ? C1 C2 C3 119.4(2) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? N1 C1 C2 122.8(2) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C4 C5 119.6(2) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C14 C12 C13 108.7(2) . . ? C14 C12 C8 109.60(18) . . ? C13 C12 C8 111.19(18) . . ? C14 C12 C15 110.4(2) . . ? C13 C12 C15 108.3(2) . . ? C8 C12 C15 108.7(2) . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C4 C3 C2 119.2(2) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.77 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.180 _refine_diff_density_min -0.230 _refine_diff_density_rms 0.034 #END=== data_[2]I3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H48 Cr I3 N6 O2' _chemical_formula_weight 1053.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.983(6) _cell_length_b 10.545(3) _cell_length_c 20.782(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.786(9) _cell_angle_gamma 90.00 _cell_volume 4374(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description palate _exptl_crystal_colour green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2068 _exptl_absorpt_coefficient_mu 2.416 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.748 _exptl_absorpt_correction_T_max 0.824 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41341 _diffrn_reflns_av_R_equivalents 0.0982 _diffrn_reflns_av_sigmaI/netI 0.0594 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 22.76 _reflns_number_total 5803 _reflns_number_gt 3690 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX-2' _computing_cell_refinement 'Bruker APEX-2' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0887P)^2^+15.8265P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5803 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0920 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1589 _refine_ls_wR_factor_gt 0.1281 _refine_ls_goodness_of_fit_ref 0.896 _refine_ls_restrained_S_all 0.896 _refine_ls_shift/su_max 0.057 _refine_ls_shift/su_mean 0.005 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 I2 I 0.08802(4) 0.89463(6) 0.29496(4) 0.0717(3) Uani 1 1 d . . . I1 I 0.14220(5) 0.97412(7) 0.17285(4) 0.0900(3) Uani 1 1 d . . . I3 I 0.03643(4) 0.80690(8) 0.41555(4) 0.0929(3) Uani 1 1 d . . . Cr1 Cr 0.21848(7) 0.15024(12) 0.52958(6) 0.0426(4) Uani 1 1 d . . . O1 O 0.3043(3) 0.1499(5) 0.5767(3) 0.0458(14) Uani 1 1 d . . . O2 O 0.2589(3) 0.1417(5) 0.4470(2) 0.0455(14) Uani 1 1 d . . . N2 N 0.1865(4) 0.4187(7) 0.5202(3) 0.0484(18) Uani 1 1 d . . . N6 N 0.2097(3) -0.0365(6) 0.5141(3) 0.0415(17) Uani 1 1 d . . . N5 N 0.1827(3) -0.1127(6) 0.5544(3) 0.0468(18) Uani 1 1 d . . . N1 N 0.1334(4) 0.2271(7) 0.4859(3) 0.0516(19) Uani 1 1 d . . . C30 C 0.2619(4) 0.0272(7) 0.4234(4) 0.040(2) Uani 1 1 d . . . N3 N 0.2301(4) 0.3371(6) 0.5414(3) 0.0410(17) Uani 1 1 d . . . N4 N 0.1696(3) 0.0846(6) 0.6070(3) 0.0450(17) Uani 1 1 d . . . C27 C 0.2656(4) -0.2279(8) 0.3779(4) 0.046(2) Uani 1 1 d . . . C10 C 0.3980(4) 0.2845(7) 0.6068(4) 0.043(2) Uani 1 1 d . . . C29 C 0.2894(4) 0.0022(8) 0.3631(4) 0.042(2) Uani 1 1 d . . . C7 C 0.3151(5) 0.4976(8) 0.5738(4) 0.051(2) Uani 1 1 d . . . H7 H 0.2869 0.5655 0.5634 0.061 Uiso 1 1 calc R . . C23 C 0.1267(5) -0.1046(8) 0.6541(4) 0.053(2) Uani 1 1 d . . . H23 H 0.1213 -0.1922 0.6532 0.063 Uiso 1 1 calc R . . C28 C 0.2904(4) -0.1237(7) 0.3440(4) 0.047(2) Uani 1 1 d . . . H28 H 0.3094 -0.1410 0.3050 0.056 Uiso 1 1 calc R . . C9 C 0.4189(5) 0.4083(8) 0.6099(4) 0.050(2) Uani 1 1 d . . . H9 H 0.4635 0.4224 0.6225 0.060 Uiso 1 1 calc R . . C6 C 0.2921(4) 0.3710(7) 0.5670(4) 0.0362(19) Uani 1 1 d . . . C26 C 0.2384(4) -0.2021(8) 0.4349(4) 0.046(2) Uani 1 1 d . . . H26 H 0.2210 -0.2678 0.4589 0.055 Uiso 1 1 calc R . . C24 C 0.1593(4) -0.0423(7) 0.6063(4) 0.041(2) Uani 1 1 d . . . C16 C 0.4436(4) 0.1710(8) 0.6240(4) 0.048(2) Uani 1 1 d . . . C38 C 0.3725(5) 0.1802(9) 0.3604(5) 0.072(3) Uani 1 1 d . . . H38A H 0.3568 0.2112 0.4004 0.108 Uiso 1 1 calc R . . H38B H 0.3876 0.2500 0.3354 0.108 Uiso 1 1 calc R . . H38C H 0.4089 0.1222 0.3690 0.108 Uiso 1 1 calc R . . C25 C 0.2361(4) -0.0772(7) 0.4583(4) 0.039(2) Uani 1 1 d . . . C33 C 0.2045(6) -0.4341(10) 0.3608(6) 0.086(4) Uani 1 1 d . . . H33A H 0.2083 -0.5185 0.3441 0.130 Uiso 1 1 calc R . . H33B H 0.1684 -0.3908 0.3379 0.130 Uiso 1 1 calc R . . H33C H 0.1957 -0.4379 0.4057 0.130 Uiso 1 1 calc R . . C3 C 0.0289(6) 0.3646(15) 0.4270(7) 0.100(4) Uani 1 1 d . . . H3 H -0.0064 0.4096 0.4071 0.120 Uiso 1 1 calc R . . C11 C 0.3309(4) 0.2634(7) 0.5839(4) 0.037(2) Uani 1 1 d . . . C31 C 0.2688(5) -0.3635(8) 0.3522(4) 0.052(2) Uani 1 1 d . . . C19 C 0.4511(5) 0.0870(9) 0.5654(5) 0.072(3) Uani 1 1 d . . . H19A H 0.4800 0.0170 0.5768 0.109 Uiso 1 1 calc R . . H19B H 0.4701 0.1353 0.5317 0.109 Uiso 1 1 calc R . . H19C H 0.4079 0.0556 0.5508 0.109 Uiso 1 1 calc R . . C20 C 0.1467(5) 0.1522(9) 0.6567(4) 0.058(3) Uani 1 1 d . . . H20 H 0.1540 0.2392 0.6581 0.070 Uiso 1 1 calc R . . C35 C 0.3162(5) 0.1128(7) 0.3236(4) 0.048(2) Uani 1 1 d . . . C8 C 0.3790(5) 0.5171(8) 0.5957(4) 0.050(2) Uani 1 1 d . . . C37 C 0.2588(5) 0.2051(9) 0.3072(5) 0.071(3) Uani 1 1 d . . . H37A H 0.2415 0.2372 0.3462 0.107 Uiso 1 1 calc R . . H37B H 0.2239 0.1617 0.2827 0.107 Uiso 1 1 calc R . . H37C H 0.2751 0.2742 0.2823 0.107 Uiso 1 1 calc R . . C22 C 0.1023(5) -0.0321(10) 0.7035(4) 0.060(3) Uani 1 1 d . . . H22 H 0.0785 -0.0709 0.7354 0.072 Uiso 1 1 calc R . . C14 C 0.4403(7) 0.6737(10) 0.6678(5) 0.099(4) Uani 1 1 d . . . H14A H 0.4053 0.6688 0.6978 0.148 Uiso 1 1 calc R . . H14B H 0.4601 0.7567 0.6697 0.148 Uiso 1 1 calc R . . H14C H 0.4739 0.6112 0.6787 0.148 Uiso 1 1 calc R . . C12 C 0.4112(5) 0.6491(9) 0.6003(5) 0.064(3) Uani 1 1 d . . . C4 C 0.0798(5) 0.4264(11) 0.4615(5) 0.077(3) Uani 1 1 d . . . H4 H 0.0791 0.5141 0.4661 0.093 Uiso 1 1 calc R . . C36 C 0.3424(6) 0.0652(9) 0.2603(5) 0.078(3) Uani 1 1 d . . . H36A H 0.3587 0.1356 0.2363 0.117 Uiso 1 1 calc R . . H36B H 0.3069 0.0240 0.2356 0.117 Uiso 1 1 calc R . . H36C H 0.3782 0.0061 0.2691 0.117 Uiso 1 1 calc R . . C15 C 0.4647(8) 0.6606(13) 0.5544(6) 0.137(6) Uani 1 1 d . . . H15A H 0.4844 0.7435 0.5580 0.206 Uiso 1 1 calc R . . H15B H 0.4462 0.6482 0.5114 0.206 Uiso 1 1 calc R . . H15C H 0.4984 0.5976 0.5640 0.206 Uiso 1 1 calc R . . C18 C 0.4140(5) 0.0931(9) 0.6781(5) 0.066(3) Uani 1 1 d . . . H18A H 0.4430 0.0228 0.6888 0.099 Uiso 1 1 calc R . . H18B H 0.3706 0.0621 0.6640 0.099 Uiso 1 1 calc R . . H18C H 0.4099 0.1457 0.7154 0.099 Uiso 1 1 calc R . . C17 C 0.5137(5) 0.2141(11) 0.6475(6) 0.092(4) Uani 1 1 d . . . H17A H 0.5409 0.1412 0.6578 0.137 Uiso 1 1 calc R . . H17B H 0.5105 0.2659 0.6853 0.137 Uiso 1 1 calc R . . H17C H 0.5337 0.2623 0.6143 0.137 Uiso 1 1 calc R . . C21 C 0.1127(5) 0.0954(10) 0.7055(4) 0.061(3) Uani 1 1 d . . . H21 H 0.0972 0.1436 0.7392 0.073 Uiso 1 1 calc R . . C5 C 0.1317(5) 0.3557(9) 0.4890(4) 0.053(2) Uani 1 1 d . . . C1 C 0.0844(6) 0.1675(11) 0.4534(5) 0.077(3) Uani 1 1 d . . . H1 H 0.0852 0.0794 0.4510 0.093 Uiso 1 1 calc R . . C13 C 0.3588(7) 0.7505(10) 0.5858(8) 0.150(7) Uani 1 1 d . . . H13A H 0.3236 0.7430 0.6155 0.225 Uiso 1 1 calc R . . H13B H 0.3404 0.7400 0.5426 0.225 Uiso 1 1 calc R . . H13C H 0.3790 0.8328 0.5901 0.225 Uiso 1 1 calc R . . C2 C 0.0319(6) 0.2331(15) 0.4228(6) 0.102(4) Uani 1 1 d . . . H2 H -0.0015 0.1890 0.3994 0.122 Uiso 1 1 calc R . . C34 C 0.2798(9) -0.3660(11) 0.2808(6) 0.138(7) Uani 1 1 d . . . H34A H 0.2817 -0.4523 0.2664 0.208 Uiso 1 1 calc R . . H34B H 0.3213 -0.3242 0.2727 0.208 Uiso 1 1 calc R . . H34C H 0.2435 -0.3231 0.2581 0.208 Uiso 1 1 calc R . . C32 C 0.3242(7) -0.4351(12) 0.3873(7) 0.128(6) Uani 1 1 d . . . H32A H 0.3259 -0.5199 0.3707 0.192 Uiso 1 1 calc R . . H32B H 0.3160 -0.4378 0.4324 0.192 Uiso 1 1 calc R . . H32C H 0.3661 -0.3933 0.3812 0.192 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 I2 0.0652(5) 0.0533(4) 0.0959(6) 0.0046(4) -0.0021(4) 0.0005(3) I1 0.1174(8) 0.0631(5) 0.0892(6) 0.0048(4) 0.0024(5) -0.0264(4) I3 0.0823(6) 0.0901(6) 0.1072(7) 0.0189(5) 0.0156(5) -0.0030(5) Cr1 0.0485(9) 0.0316(7) 0.0480(8) -0.0054(6) 0.0047(6) -0.0073(6) O1 0.044(4) 0.033(3) 0.060(4) -0.001(3) 0.000(3) -0.005(3) O2 0.064(4) 0.030(3) 0.043(3) -0.007(3) 0.014(3) -0.009(3) N2 0.043(5) 0.044(4) 0.058(5) 0.001(4) 0.004(4) -0.007(4) N6 0.040(4) 0.035(4) 0.049(4) -0.005(3) 0.000(3) -0.008(3) N5 0.048(5) 0.040(4) 0.052(4) 0.001(4) 0.002(4) -0.014(4) N1 0.040(5) 0.063(5) 0.052(4) -0.001(4) 0.002(4) -0.010(4) C30 0.031(5) 0.037(5) 0.052(5) -0.014(4) 0.000(4) 0.005(4) N3 0.045(5) 0.037(4) 0.042(4) -0.001(3) 0.005(3) 0.001(4) N4 0.051(5) 0.042(4) 0.043(4) -0.003(3) 0.001(3) -0.008(3) C27 0.052(6) 0.038(5) 0.046(5) -0.010(4) -0.001(4) -0.003(4) C10 0.047(6) 0.034(5) 0.047(5) 0.004(4) 0.005(4) -0.001(4) C29 0.039(5) 0.041(5) 0.046(5) -0.007(4) 0.004(4) -0.003(4) C7 0.070(7) 0.033(5) 0.048(5) 0.003(4) -0.004(5) -0.008(5) C23 0.063(7) 0.040(5) 0.055(6) 0.009(5) 0.000(5) -0.007(5) C28 0.060(6) 0.027(5) 0.054(5) -0.002(4) 0.006(4) 0.003(4) C9 0.056(6) 0.048(6) 0.046(5) -0.007(4) -0.001(4) -0.011(5) C6 0.040(5) 0.026(4) 0.043(5) -0.006(3) 0.000(4) -0.005(4) C26 0.049(6) 0.034(5) 0.055(6) 0.002(4) 0.002(4) -0.008(4) C24 0.039(5) 0.033(5) 0.052(5) -0.002(4) -0.005(4) -0.004(4) C16 0.045(6) 0.038(5) 0.061(6) -0.001(4) 0.003(4) 0.002(4) C38 0.075(8) 0.053(6) 0.090(8) 0.007(5) 0.022(6) -0.015(6) C25 0.049(6) 0.030(5) 0.039(5) -0.003(4) 0.003(4) -0.003(4) C33 0.092(9) 0.060(7) 0.109(9) -0.033(6) 0.023(7) -0.021(6) C3 0.045(8) 0.121(12) 0.131(11) 0.035(9) -0.024(7) -0.007(8) C11 0.045(6) 0.028(5) 0.040(5) -0.002(4) 0.012(4) -0.006(4) C31 0.068(7) 0.040(5) 0.049(5) -0.009(4) 0.008(5) 0.000(5) C19 0.079(8) 0.054(6) 0.086(8) 0.001(5) 0.020(6) 0.012(5) C20 0.074(7) 0.050(6) 0.052(6) -0.001(5) 0.007(5) -0.007(5) C35 0.065(7) 0.028(4) 0.052(5) 0.003(4) 0.012(5) -0.011(4) C8 0.070(7) 0.035(5) 0.044(5) 0.007(4) -0.003(5) -0.010(5) C37 0.099(9) 0.042(5) 0.072(7) 0.012(5) 0.002(6) 0.007(6) C22 0.051(6) 0.073(7) 0.057(6) 0.005(5) 0.011(5) -0.004(5) C14 0.146(12) 0.066(7) 0.082(8) -0.012(6) -0.016(8) -0.053(8) C12 0.075(8) 0.049(6) 0.068(7) 0.006(5) -0.007(6) -0.026(5) C4 0.056(8) 0.082(8) 0.094(8) 0.029(7) 0.013(6) 0.011(6) C36 0.128(10) 0.042(5) 0.069(7) 0.002(5) 0.046(7) -0.003(6) C15 0.201(17) 0.109(11) 0.105(10) -0.010(9) 0.036(11) -0.101(12) C18 0.070(7) 0.052(6) 0.075(7) 0.012(5) 0.003(5) 0.005(5) C17 0.054(7) 0.086(8) 0.131(10) 0.014(7) -0.030(7) -0.002(6) C21 0.061(7) 0.074(7) 0.050(6) -0.015(5) 0.013(5) -0.004(5) C5 0.049(6) 0.054(6) 0.057(6) 0.011(5) 0.011(5) 0.005(5) C1 0.061(8) 0.085(8) 0.084(8) 0.002(6) -0.016(6) -0.026(7) C13 0.142(14) 0.034(7) 0.26(2) 0.015(9) -0.096(13) -0.027(8) C2 0.067(9) 0.124(12) 0.110(10) -0.007(9) -0.033(7) -0.016(9) C34 0.27(2) 0.052(7) 0.098(10) -0.036(7) 0.061(11) -0.038(10) C32 0.112(11) 0.075(8) 0.188(15) -0.058(9) -0.078(11) 0.034(8) _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 I2 I3 2.9070(13) . ? I2 I1 2.9295(13) . ? Cr1 O1 1.933(6) . ? Cr1 O2 1.935(5) . ? Cr1 N3 1.997(7) . ? Cr1 N6 2.002(6) . ? Cr1 N4 2.043(7) . ? Cr1 N1 2.055(7) . ? O1 C11 1.315(9) . ? O2 C30 1.306(9) . ? N2 N3 1.287(9) . ? N2 C5 1.413(11) . ? N6 N5 1.297(9) . ? N6 C25 1.366(10) . ? N5 C24 1.408(10) . ? N1 C1 1.321(11) . ? N1 C5 1.358(11) . ? C30 C25 1.428(11) . ? C30 C29 1.417(11) . ? N3 C6 1.372(10) . ? N4 C24 1.353(10) . ? N4 C20 1.353(11) . ? C27 C26 1.356(11) . ? C27 C28 1.409(11) . ? C27 C31 1.528(11) . ? C10 C9 1.371(11) . ? C10 C11 1.419(11) . ? C10 C16 1.536(11) . ? C29 C28 1.386(11) . ? C29 C35 1.537(11) . ? C7 C8 1.351(12) . ? C7 C6 1.416(11) . ? C23 C24 1.380(11) . ? C23 C22 1.387(12) . ? C9 C8 1.419(12) . ? C6 C11 1.409(11) . ? C26 C25 1.405(11) . ? C16 C17 1.530(13) . ? C16 C19 1.519(12) . ? C16 C18 1.535(12) . ? C38 C35 1.507(12) . ? C33 C31 1.504(13) . ? C3 C4 1.379(16) . ? C3 C2 1.391(18) . ? C31 C34 1.511(14) . ? C31 C32 1.498(14) . ? C20 C21 1.384(13) . ? C35 C36 1.525(12) . ? C35 C37 1.530(12) . ? C8 C12 1.536(12) . ? C22 C21 1.361(13) . ? C14 C12 1.515(13) . ? C12 C15 1.471(16) . ? C12 C13 1.518(16) . ? C4 C5 1.378(13) . ? C1 C2 1.386(16) . ? 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 I3 I2 I1 177.95(4) . . ? O1 Cr1 O2 92.9(2) . . ? O1 Cr1 N3 81.1(3) . . ? O2 Cr1 N3 95.9(2) . . ? O1 Cr1 N6 98.5(2) . . ? O2 Cr1 N6 81.3(2) . . ? N3 Cr1 N6 177.2(3) . . ? O1 Cr1 N4 92.7(3) . . ? O2 Cr1 N4 156.8(2) . . ? N3 Cr1 N4 107.2(3) . . ? N6 Cr1 N4 75.6(3) . . ? O1 Cr1 N1 156.8(3) . . ? O2 Cr1 N1 89.9(3) . . ? N3 Cr1 N1 75.8(3) . . ? N6 Cr1 N1 104.6(3) . . ? N4 Cr1 N1 93.7(3) . . ? C11 O1 Cr1 113.5(5) . . ? C30 O2 Cr1 113.9(5) . . ? N3 N2 C5 109.8(7) . . ? N5 N6 C25 123.0(6) . . ? N5 N6 Cr1 122.8(5) . . ? C25 N6 Cr1 114.3(5) . . ? N6 N5 C24 109.4(6) . . ? C1 N1 C5 118.7(9) . . ? C1 N1 Cr1 127.9(7) . . ? C5 N1 Cr1 113.3(6) . . ? O2 C30 C25 119.9(7) . . ? O2 C30 C29 122.0(7) . . ? C25 C30 C29 118.1(7) . . ? N2 N3 C6 122.8(7) . . ? N2 N3 Cr1 123.0(5) . . ? C6 N3 Cr1 113.7(5) . . ? C24 N4 C20 118.2(7) . . ? C24 N4 Cr1 113.9(6) . . ? C20 N4 Cr1 127.9(6) . . ? C26 C27 C28 116.5(7) . . ? C26 C27 C31 121.3(8) . . ? C28 C27 C31 122.2(7) . . ? C9 C10 C11 116.5(8) . . ? C9 C10 C16 123.8(8) . . ? C11 C10 C16 119.7(7) . . ? C28 C29 C30 116.3(7) . . ? C28 C29 C35 124.3(7) . . ? C30 C29 C35 119.4(7) . . ? C8 C7 C6 118.3(8) . . ? C24 C23 C22 117.7(8) . . ? C29 C28 C27 126.4(8) . . ? C10 C9 C8 126.4(9) . . ? N3 C6 C11 111.2(7) . . ? N3 C6 C7 124.5(8) . . ? C11 C6 C7 124.2(8) . . ? C27 C26 C25 120.8(8) . . ? N4 C24 C23 122.7(8) . . ? N4 C24 N5 118.2(7) . . ? C23 C24 N5 119.1(7) . . ? C10 C16 C17 111.5(7) . . ? C10 C16 C19 110.4(7) . . ? C17 C16 C19 107.8(8) . . ? C10 C16 C18 110.0(7) . . ? C17 C16 C18 107.7(8) . . ? C19 C16 C18 109.4(7) . . ? N6 C25 C26 127.4(7) . . ? N6 C25 C30 110.7(6) . . ? C26 C25 C30 121.9(7) . . ? C4 C3 C2 118.1(11) . . ? O1 C11 C6 119.4(7) . . ? O1 C11 C10 123.4(7) . . ? C6 C11 C10 117.2(7) . . ? C27 C31 C34 111.7(8) . . ? C27 C31 C33 111.7(8) . . ? C34 C31 C33 105.9(9) . . ? C27 C31 C32 110.1(8) . . ? C34 C31 C32 109.2(10) . . ? C33 C31 C32 108.0(10) . . ? N4 C20 C21 121.9(9) . . ? C36 C35 C29 110.8(7) . . ? C36 C35 C38 108.3(8) . . ? C29 C35 C38 110.9(7) . . ? C36 C35 C37 107.6(8) . . ? C29 C35 C37 109.0(7) . . ? C38 C35 C37 110.3(7) . . ? C7 C8 C9 117.3(8) . . ? C7 C8 C12 123.1(8) . . ? C9 C8 C12 119.3(9) . . ? C21 C22 C23 120.6(9) . . ? C15 C12 C8 110.5(9) . . ? C15 C12 C14 109.2(10) . . ? C8 C12 C14 110.7(8) . . ? C15 C12 C13 109.3(11) . . ? C8 C12 C13 110.0(8) . . ? C14 C12 C13 107.1(10) . . ? C3 C4 C5 118.8(11) . . ? C22 C21 C20 118.9(9) . . ? N1 C5 C4 122.7(10) . . ? N1 C5 N2 118.1(8) . . ? C4 C5 N2 119.2(9) . . ? N1 C1 C2 121.5(11) . . ? C1 C2 C3 120.2(11) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 22.76 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.285 _refine_diff_density_min -0.803 _refine_diff_density_rms 0.095