# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Andrew Borovik' _publ_contact_author_email aborovik@uci.edu loop_ _publ_author_name N.Sickerman 'Young Jun Park' G.K.-Y.Ng J.Bates M.Hilkert J.Ziller F.Furche A.Borovik data_asb127 _database_code_depnum_ccdc_archive 'CCDC 855304' #TrackingRef '- DT-ART-11-2011-012244-CIF.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H47 B Cl Cr N7 O3' _chemical_formula_weight 760.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 11.4096(6) _cell_length_b 20.1336(10) _cell_length_c 15.8570(8) _cell_angle_alpha 90.00 _cell_angle_beta 96.1853(7) _cell_angle_gamma 90.00 _cell_volume 3621.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 98(2) _cell_measurement_reflns_used 9989 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 28.27 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 0.439 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8832 _exptl_absorpt_correction_T_max 0.9291 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 98(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX II CCD' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 41203 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0214 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.10 _reflns_number_total 7983 _reflns_number_gt 6816 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX2' _computing_cell_refinement 'Bruker SMART APEX2/SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0586P)^2^+4.3777P] 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 7983 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1228 _refine_ls_wR_factor_gt 0.1169 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 0.51127(3) 0.207750(16) 0.38917(2) 0.01791(10) Uani 1 1 d . . . Cl1 Cl 0.71746(4) 0.20313(2) 0.42723(3) 0.01999(12) Uani 1 1 d . . . O1 O 0.56748(13) 0.34042(8) 0.17510(10) 0.0243(3) Uani 1 1 d . . . O2 O 0.50387(14) -0.01229(8) 0.38687(11) 0.0296(4) Uani 1 1 d . . . O3 O 0.47007(13) 0.33727(8) 0.60921(9) 0.0244(3) Uani 1 1 d . . . N1 N 0.32709(15) 0.21068(9) 0.35483(12) 0.0205(4) Uani 1 1 d . . . N2 N 0.51026(15) 0.26680(9) 0.27410(11) 0.0203(4) Uani 1 1 d . . . N3 N 0.47782(15) 0.10186(9) 0.37506(12) 0.0213(4) Uani 1 1 d . . . N4 N 0.46080(15) 0.26114(9) 0.49778(11) 0.0227(4) Uani 1 1 d . . . N5 N 0.70664(16) 0.27906(9) 0.24411(12) 0.0223(4) Uani 1 1 d . . . H5 H 0.7380 0.2474 0.2775 0.027 Uiso 1 1 calc R . . N6 N 0.65796(16) 0.05073(9) 0.42295(15) 0.0319(5) Uani 1 1 d . . . H6 H 0.7009 0.0871 0.4276 0.038 Uiso 1 1 calc R . . N7 N 0.63763(16) 0.30686(9) 0.56241(12) 0.0244(4) Uani 1 1 d . . . H7 H 0.6871 0.2811 0.5387 0.029 Uiso 1 1 calc R . . C1 C 0.30600(18) 0.23155(11) 0.26398(14) 0.0225(4) Uani 1 1 d . . . H1A H 0.2234 0.2466 0.2514 0.027 Uiso 1 1 calc R . . H1B H 0.3180 0.1930 0.2271 0.027 Uiso 1 1 calc R . . C2 C 0.38870(18) 0.28738(11) 0.24462(14) 0.0228(4) Uani 1 1 d . . . H2A H 0.3811 0.2963 0.1829 0.027 Uiso 1 1 calc R . . H2B H 0.3686 0.3285 0.2741 0.027 Uiso 1 1 calc R . . C3 C 0.59158(19) 0.29378(10) 0.23500(13) 0.0193(4) Uani 1 1 d . . . C4 C 0.6768(2) 0.36192(11) 0.14398(15) 0.0265(5) Uani 1 1 d . . . H4A H 0.6898 0.4099 0.1546 0.032 Uiso 1 1 calc R . . H4B H 0.6743 0.3536 0.0823 0.032 Uiso 1 1 calc R . . C5 C 0.77404(19) 0.32133(11) 0.19248(14) 0.0241(4) Uani 1 1 d . . . H5B H 0.8179 0.2948 0.1537 0.029 Uiso 1 1 calc R . . H5C H 0.8300 0.3499 0.2281 0.029 Uiso 1 1 calc R . . C6 C 0.27677(19) 0.14325(11) 0.36575(15) 0.0251(5) Uani 1 1 d . . . H6A H 0.1983 0.1402 0.3326 0.030 Uiso 1 1 calc R . . H6B H 0.2664 0.1361 0.4263 0.030 Uiso 1 1 calc R . . C7 C 0.35700(19) 0.08979(11) 0.33640(15) 0.0247(5) Uani 1 1 d . . . H7B H 0.3301 0.0455 0.3534 0.030 Uiso 1 1 calc R . . H7C H 0.3545 0.0907 0.2738 0.030 Uiso 1 1 calc R . . C8 C 0.54407(18) 0.05044(10) 0.39394(13) 0.0197(4) Uani 1 1 d . . . C9 C 0.60080(19) -0.05821(11) 0.41145(15) 0.0238(4) Uani 1 1 d . . . H9A H 0.6209 -0.0841 0.3619 0.029 Uiso 1 1 calc R . . H9B H 0.5796 -0.0894 0.4556 0.029 Uiso 1 1 calc R . . C10 C 0.70428(19) -0.01385(10) 0.44597(15) 0.0243(4) Uani 1 1 d . . . H10A H 0.7220 -0.0184 0.5082 0.029 Uiso 1 1 calc R . . H10B H 0.7761 -0.0237 0.4184 0.029 Uiso 1 1 calc R . . C11 C 0.27397(19) 0.26046(12) 0.40949(15) 0.0266(5) Uani 1 1 d . . . H11A H 0.1886 0.2515 0.4091 0.032 Uiso 1 1 calc R . . H11B H 0.2833 0.3056 0.3863 0.032 Uiso 1 1 calc R . . C12 C 0.33257(19) 0.25751(13) 0.49976(15) 0.0290(5) Uani 1 1 d . . . H12A H 0.3055 0.2951 0.5330 0.035 Uiso 1 1 calc R . . H12B H 0.3114 0.2156 0.5270 0.035 Uiso 1 1 calc R . . C13 C 0.52040(19) 0.29902(10) 0.55273(13) 0.0213(4) Uani 1 1 d . . . C14 C 0.5627(2) 0.37304(11) 0.66084(15) 0.0282(5) Uani 1 1 d . . . H14A H 0.5735 0.3548 0.7191 0.034 Uiso 1 1 calc R . . H14B H 0.5428 0.4208 0.6639 0.034 Uiso 1 1 calc R . . C15 C 0.6735(2) 0.36352(11) 0.61740(14) 0.0255(5) Uani 1 1 d . . . H15A H 0.6914 0.4032 0.5841 0.031 Uiso 1 1 calc R . . H15B H 0.7423 0.3527 0.6585 0.031 Uiso 1 1 calc R . . B1 B 0.05709(19) 0.48047(11) 0.28879(14) 0.0156(4) Uani 1 1 d . . . C16 C 0.04252(16) 0.56124(10) 0.28014(13) 0.0176(4) Uani 1 1 d . . . C17 C 0.06865(17) 0.59878(10) 0.21021(13) 0.0193(4) Uani 1 1 d . . . H17A H 0.0965 0.5765 0.1635 0.023 Uiso 1 1 calc R . . C18 C 0.05542(18) 0.66774(11) 0.20643(14) 0.0228(4) Uani 1 1 d . . . H18A H 0.0726 0.6912 0.1573 0.027 Uiso 1 1 calc R . . C19 C 0.01726(19) 0.70205(11) 0.27427(15) 0.0250(5) Uani 1 1 d . . . H19A H 0.0064 0.7488 0.2716 0.030 Uiso 1 1 calc R . . C20 C -0.00467(19) 0.66702(11) 0.34589(15) 0.0261(5) Uani 1 1 d . . . H20A H -0.0284 0.6900 0.3935 0.031 Uiso 1 1 calc R . . C21 C 0.00779(19) 0.59840(11) 0.34865(14) 0.0228(4) Uani 1 1 d . . . H21A H -0.0077 0.5756 0.3987 0.027 Uiso 1 1 calc R . . C22 C -0.05373(17) 0.44982(10) 0.33386(13) 0.0187(4) Uani 1 1 d . . . C23 C -0.0471(2) 0.39187(12) 0.38276(14) 0.0262(5) Uani 1 1 d . . . H23A H 0.0273 0.3709 0.3955 0.031 Uiso 1 1 calc R . . C24 C -0.1459(2) 0.36375(13) 0.41348(15) 0.0328(5) Uani 1 1 d . . . H24A H -0.1380 0.3248 0.4474 0.039 Uiso 1 1 calc R . . C25 C -0.2556(2) 0.39284(13) 0.39442(15) 0.0324(5) Uani 1 1 d . . . H25A H -0.3232 0.3737 0.4148 0.039 Uiso 1 1 calc R . . C26 C -0.2658(2) 0.44954(12) 0.34579(16) 0.0305(5) Uani 1 1 d . . . H26A H -0.3410 0.4695 0.3321 0.037 Uiso 1 1 calc R . . C27 C -0.16681(19) 0.47767(11) 0.31677(15) 0.0251(5) Uani 1 1 d . . . H27A H -0.1757 0.5173 0.2841 0.030 Uiso 1 1 calc R . . C28 C 0.04822(16) 0.44102(10) 0.19730(12) 0.0154(4) Uani 1 1 d . . . C29 C -0.02595(17) 0.46099(10) 0.12515(13) 0.0186(4) Uani 1 1 d . . . H29A H -0.0691 0.5012 0.1276 0.022 Uiso 1 1 calc R . . C30 C -0.03873(19) 0.42434(11) 0.05024(14) 0.0227(4) Uani 1 1 d . . . H30A H -0.0895 0.4400 0.0030 0.027 Uiso 1 1 calc R . . C31 C 0.02197(19) 0.36521(10) 0.04401(14) 0.0223(4) Uani 1 1 d . . . H31A H 0.0141 0.3404 -0.0072 0.027 Uiso 1 1 calc R . . C32 C 0.09433(18) 0.34305(10) 0.11406(13) 0.0197(4) Uani 1 1 d . . . H32A H 0.1358 0.3023 0.1113 0.024 Uiso 1 1 calc R . . C33 C 0.10643(17) 0.38031(10) 0.18845(13) 0.0166(4) Uani 1 1 d . . . H33A H 0.1565 0.3639 0.2356 0.020 Uiso 1 1 calc R . . C34 C 0.18553(17) 0.46713(10) 0.34323(13) 0.0180(4) Uani 1 1 d . . . C35 C 0.20305(19) 0.46043(11) 0.43144(14) 0.0235(4) Uani 1 1 d . . . H35A H 0.1370 0.4638 0.4629 0.028 Uiso 1 1 calc R . . C36 C 0.3145(2) 0.44901(11) 0.47498(16) 0.0315(5) Uani 1 1 d . . . H36A H 0.3227 0.4447 0.5350 0.038 Uiso 1 1 calc R . . C37 C 0.4124(2) 0.44403(12) 0.43160(17) 0.0336(6) Uani 1 1 d . . . H37A H 0.4877 0.4348 0.4609 0.040 Uiso 1 1 calc R . . C38 C 0.3992(2) 0.45263(12) 0.34500(18) 0.0311(5) Uani 1 1 d . . . H38A H 0.4660 0.4502 0.3142 0.037 Uiso 1 1 calc R . . C39 C 0.28803(18) 0.46494(11) 0.30233(15) 0.0233(4) Uani 1 1 d . . . H39A H 0.2816 0.4722 0.2428 0.028 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 0.01364(16) 0.01965(17) 0.01960(17) 0.00152(12) -0.00201(12) 0.00063(12) Cl1 0.0165(2) 0.0192(2) 0.0235(2) 0.00247(18) -0.00095(18) -0.00069(17) O1 0.0229(8) 0.0236(8) 0.0261(8) 0.0081(6) 0.0019(6) 0.0023(6) O2 0.0239(8) 0.0174(7) 0.0453(10) -0.0030(7) -0.0070(7) -0.0025(6) O3 0.0246(8) 0.0269(8) 0.0220(8) -0.0018(6) 0.0035(6) 0.0014(6) N1 0.0167(8) 0.0201(9) 0.0239(9) -0.0006(7) -0.0013(7) 0.0003(7) N2 0.0187(8) 0.0197(8) 0.0214(9) 0.0007(7) -0.0025(7) 0.0018(7) N3 0.0156(8) 0.0216(9) 0.0257(9) -0.0026(7) -0.0015(7) -0.0019(7) N4 0.0185(8) 0.0268(9) 0.0224(9) -0.0007(7) 0.0011(7) -0.0016(7) N5 0.0210(9) 0.0228(9) 0.0232(9) 0.0055(7) 0.0026(7) 0.0020(7) N6 0.0166(9) 0.0164(9) 0.0611(14) -0.0013(9) -0.0031(9) -0.0009(7) N7 0.0233(9) 0.0248(9) 0.0249(9) -0.0052(8) 0.0014(7) -0.0031(7) C1 0.0196(10) 0.0225(10) 0.0237(11) 0.0006(8) -0.0055(8) 0.0010(8) C2 0.0185(10) 0.0210(10) 0.0279(11) 0.0032(8) -0.0015(8) 0.0030(8) C3 0.0230(10) 0.0156(9) 0.0185(10) -0.0019(7) -0.0019(8) 0.0022(8) C4 0.0292(11) 0.0258(11) 0.0256(11) 0.0052(9) 0.0074(9) 0.0015(9) C5 0.0238(11) 0.0235(11) 0.0258(11) 0.0025(9) 0.0058(9) -0.0013(9) C6 0.0164(10) 0.0265(11) 0.0316(12) 0.0034(9) -0.0019(8) -0.0019(8) C7 0.0199(10) 0.0223(11) 0.0304(11) -0.0005(9) -0.0038(9) -0.0040(8) C8 0.0195(10) 0.0182(10) 0.0216(10) -0.0035(8) 0.0039(8) -0.0032(8) C9 0.0224(10) 0.0181(10) 0.0309(12) -0.0014(8) 0.0030(9) 0.0000(8) C10 0.0235(11) 0.0178(10) 0.0308(11) -0.0022(9) -0.0011(9) 0.0001(8) C11 0.0186(10) 0.0303(12) 0.0309(12) -0.0050(9) 0.0026(9) 0.0014(9) C12 0.0209(11) 0.0389(13) 0.0277(12) -0.0042(10) 0.0056(9) -0.0031(9) C13 0.0249(10) 0.0201(10) 0.0190(10) 0.0039(8) 0.0025(8) 0.0023(8) C14 0.0378(13) 0.0212(11) 0.0254(11) -0.0036(9) 0.0029(9) -0.0053(9) C15 0.0288(11) 0.0215(10) 0.0257(11) -0.0019(9) 0.0005(9) -0.0062(9) B1 0.0118(9) 0.0174(10) 0.0174(10) -0.0007(8) 0.0002(8) 0.0007(8) C16 0.0109(8) 0.0190(9) 0.0219(10) -0.0026(8) -0.0024(7) 0.0011(7) C17 0.0146(9) 0.0202(10) 0.0226(10) -0.0033(8) -0.0003(7) -0.0013(7) C18 0.0175(10) 0.0201(10) 0.0296(11) 0.0015(9) -0.0023(8) -0.0031(8) C19 0.0193(10) 0.0179(10) 0.0361(12) -0.0053(9) -0.0048(9) 0.0009(8) C20 0.0238(11) 0.0229(11) 0.0308(12) -0.0088(9) -0.0001(9) 0.0041(9) C21 0.0227(10) 0.0224(10) 0.0230(10) -0.0021(8) 0.0014(8) 0.0027(8) C22 0.0164(9) 0.0227(10) 0.0170(9) -0.0044(8) 0.0018(7) -0.0038(8) C23 0.0260(11) 0.0275(11) 0.0245(11) 0.0001(9) 0.0001(9) -0.0056(9) C24 0.0439(14) 0.0316(13) 0.0227(11) 0.0028(9) 0.0032(10) -0.0141(11) C25 0.0301(12) 0.0416(14) 0.0272(12) -0.0096(10) 0.0114(10) -0.0151(10) C26 0.0198(11) 0.0345(13) 0.0383(13) -0.0076(10) 0.0078(9) -0.0029(9) C27 0.0211(10) 0.0258(11) 0.0285(11) -0.0023(9) 0.0031(8) -0.0015(9) C28 0.0108(8) 0.0166(9) 0.0189(9) 0.0011(7) 0.0024(7) -0.0022(7) C29 0.0157(9) 0.0169(9) 0.0225(10) 0.0014(8) -0.0020(8) 0.0014(7) C30 0.0218(10) 0.0238(10) 0.0209(10) 0.0016(8) -0.0051(8) -0.0011(8) C31 0.0264(11) 0.0208(10) 0.0195(10) -0.0044(8) 0.0016(8) -0.0043(8) C32 0.0191(9) 0.0152(9) 0.0250(10) -0.0010(8) 0.0031(8) -0.0003(8) C33 0.0139(9) 0.0167(9) 0.0187(9) 0.0026(7) -0.0001(7) 0.0001(7) C34 0.0159(9) 0.0133(9) 0.0236(10) -0.0026(8) -0.0024(8) 0.0006(7) C35 0.0235(11) 0.0214(10) 0.0240(11) -0.0029(8) -0.0045(8) 0.0010(8) C36 0.0360(13) 0.0229(11) 0.0312(12) -0.0043(9) -0.0163(10) 0.0034(9) C37 0.0234(11) 0.0224(11) 0.0501(16) -0.0097(10) -0.0179(10) 0.0038(9) C38 0.0145(10) 0.0261(12) 0.0514(15) -0.0122(11) -0.0022(10) 0.0006(9) C39 0.0162(10) 0.0235(10) 0.0295(11) -0.0054(9) -0.0010(8) -0.0011(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 Cr1 N1 2.1140(18) . ? Cr1 N4 2.1604(19) . ? Cr1 N3 2.1731(18) . ? Cr1 N2 2.1767(18) . ? Cr1 Cl1 2.3668(6) . ? O1 C3 1.343(2) . ? O1 C4 1.456(3) . ? O2 C8 1.344(3) . ? O2 C9 1.462(3) . ? O3 C13 1.355(3) . ? O3 C14 1.456(3) . ? N1 C6 1.491(3) . ? N1 C1 1.495(3) . ? N1 C11 1.495(3) . ? N2 C3 1.290(3) . ? N2 C2 1.474(3) . ? N3 C8 1.298(3) . ? N3 C7 1.467(3) . ? N4 C13 1.294(3) . ? N4 C12 1.469(3) . ? N5 C3 1.338(3) . ? N5 C5 1.457(3) . ? N6 C8 1.331(3) . ? N6 C10 1.436(3) . ? N7 C13 1.339(3) . ? N7 C15 1.467(3) . ? C1 C2 1.520(3) . ? C4 C5 1.519(3) . ? C6 C7 1.518(3) . ? C9 C10 1.534(3) . ? C11 C12 1.514(3) . ? C14 C15 1.515(3) . ? B1 C22 1.639(3) . ? B1 C16 1.639(3) . ? B1 C34 1.641(3) . ? B1 C28 1.647(3) . ? C16 C17 1.400(3) . ? C16 C21 1.411(3) . ? C17 C18 1.397(3) . ? C18 C19 1.387(3) . ? C19 C20 1.382(3) . ? C20 C21 1.389(3) . ? C22 C23 1.398(3) . ? C22 C27 1.406(3) . ? C23 C24 1.396(3) . ? C24 C25 1.385(4) . ? C25 C26 1.376(4) . ? C26 C27 1.386(3) . ? C28 C33 1.405(3) . ? C28 C29 1.406(3) . ? C29 C30 1.393(3) . ? C30 C31 1.386(3) . ? C31 C32 1.384(3) . ? C32 C33 1.392(3) . ? C34 C39 1.398(3) . ? C34 C35 1.398(3) . ? C35 C36 1.399(3) . ? C36 C37 1.377(4) . ? C37 C38 1.376(4) . ? C38 C39 1.394(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 N4 81.29(7) . . ? N1 Cr1 N3 80.92(7) . . ? N4 Cr1 N3 120.75(7) . . ? N1 Cr1 N2 81.58(7) . . ? N4 Cr1 N2 114.75(7) . . ? N3 Cr1 N2 117.68(7) . . ? N1 Cr1 Cl1 179.33(5) . . ? N4 Cr1 Cl1 99.16(5) . . ? N3 Cr1 Cl1 98.42(5) . . ? N2 Cr1 Cl1 98.66(5) . . ? C3 O1 C4 109.28(16) . . ? C8 O2 C9 109.30(16) . . ? C13 O3 C14 108.63(17) . . ? C6 N1 C1 110.10(17) . . ? C6 N1 C11 110.96(17) . . ? C1 N1 C11 109.69(17) . . ? C6 N1 Cr1 109.21(12) . . ? C1 N1 Cr1 107.96(13) . . ? C11 N1 Cr1 108.85(13) . . ? C3 N2 C2 115.46(17) . . ? C3 N2 Cr1 133.92(14) . . ? C2 N2 Cr1 109.82(13) . . ? C8 N3 C7 117.50(18) . . ? C8 N3 Cr1 131.87(14) . . ? C7 N3 Cr1 110.62(13) . . ? C13 N4 C12 117.86(19) . . ? C13 N4 Cr1 131.61(15) . . ? C12 N4 Cr1 110.12(14) . . ? C3 N5 C5 112.40(17) . . ? C8 N6 C10 113.75(18) . . ? C13 N7 C15 111.75(18) . . ? N1 C1 C2 111.31(17) . . ? N2 C2 C1 108.14(17) . . ? N2 C3 N5 127.07(19) . . ? N2 C3 O1 122.09(19) . . ? N5 C3 O1 110.79(18) . . ? O1 C4 C5 105.91(17) . . ? N5 C5 C4 101.41(17) . . ? N1 C6 C7 110.94(18) . . ? N3 C7 C6 108.95(17) . . ? N3 C8 N6 126.79(19) . . ? N3 C8 O2 123.04(19) . . ? N6 C8 O2 110.16(18) . . ? O2 C9 C10 104.95(17) . . ? N6 C10 C9 100.87(17) . . ? N1 C11 C12 110.88(18) . . ? N4 C12 C11 108.50(18) . . ? N4 C13 N7 126.3(2) . . ? N4 C13 O3 123.4(2) . . ? N7 C13 O3 110.28(18) . . ? O3 C14 C15 105.79(17) . . ? N7 C15 C14 100.13(17) . . ? C22 B1 C16 109.52(16) . . ? C22 B1 C34 113.34(16) . . ? C16 B1 C34 106.45(15) . . ? C22 B1 C28 103.03(15) . . ? C16 B1 C28 114.12(16) . . ? C34 B1 C28 110.55(16) . . ? C17 C16 C21 115.16(19) . . ? C17 C16 B1 124.99(18) . . ? C21 C16 B1 119.75(18) . . ? C18 C17 C16 122.6(2) . . ? C19 C18 C17 120.2(2) . . ? C20 C19 C18 118.9(2) . . ? C19 C20 C21 120.4(2) . . ? C20 C21 C16 122.6(2) . . ? C23 C22 C27 115.69(19) . . ? C23 C22 B1 123.90(18) . . ? C27 C22 B1 120.05(18) . . ? C24 C23 C22 122.3(2) . . ? C25 C24 C23 119.8(2) . . ? C26 C25 C24 119.6(2) . . ? C25 C26 C27 120.1(2) . . ? C26 C27 C22 122.5(2) . . ? C33 C28 C29 114.63(18) . . ? C33 C28 B1 121.50(17) . . ? C29 C28 B1 123.57(17) . . ? C30 C29 C28 122.74(19) . . ? C31 C30 C29 120.58(19) . . ? C32 C31 C30 118.62(19) . . ? C31 C32 C33 120.15(19) . . ? C32 C33 C28 123.26(18) . . ? C39 C34 C35 115.12(19) . . ? C39 C34 B1 120.37(18) . . ? C35 C34 B1 124.44(18) . . ? C34 C35 C36 122.3(2) . . ? C37 C36 C35 120.6(2) . . ? C38 C37 C36 118.8(2) . . ? C37 C38 C39 120.2(2) . . ? C38 C39 C34 122.9(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.917 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.068 #==END data_asb95 _database_code_depnum_ccdc_archive 'CCDC 855305' #TrackingRef '- DT-ART-11-2011-012244-CIF.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H47 B Cl Mn N7 O3' _chemical_formula_weight 763.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8790(5) _cell_length_b 13.2995(7) _cell_length_c 15.3116(8) _cell_angle_alpha 71.1510(10) _cell_angle_beta 85.2050(10) _cell_angle_gamma 80.7250(10) _cell_volume 1877.88(17) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 9917 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 28.28 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 802 _exptl_absorpt_coefficient_mu 0.470 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8679 _exptl_absorpt_correction_T_max 0.9501 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX II CCD' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21352 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_av_sigmaI/netI 0.0241 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 27.10 _reflns_number_total 8194 _reflns_number_gt 7118 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX2' _computing_cell_refinement 'Bruker SMART APEX2/SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0469P)^2^+1.1764P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8194 _refine_ls_number_parameters 649 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0965 _refine_ls_wR_factor_gt 0.0922 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 Mn1 Mn -0.05030(2) 0.270877(19) 0.225998(16) 0.01732(8) Uani 1 1 d . . . Cl1 Cl 0.05879(5) 0.41829(3) 0.11793(3) 0.02734(11) Uani 1 1 d . . . N1 N -0.14773(14) 0.13386(11) 0.33316(10) 0.0199(3) Uani 1 1 d . . . N2 N -0.01186(15) 0.14436(11) 0.16355(10) 0.0206(3) Uani 1 1 d . . . N3 N -0.26615(15) 0.33490(12) 0.21740(10) 0.0235(3) Uani 1 1 d . . . N4 N 0.04573(14) 0.25936(11) 0.35192(9) 0.0190(3) Uani 1 1 d . . . N5 N 0.11072(16) 0.22567(13) 0.02759(10) 0.0245(3) Uani 1 1 d . . . N6 N -0.27570(18) 0.48280(12) 0.08103(11) 0.0282(3) Uani 1 1 d . . . N7 N 0.14736(17) 0.41659(13) 0.31701(12) 0.0279(3) Uani 1 1 d . . . O1 O 0.06510(13) 0.06103(10) 0.05399(9) 0.0269(3) Uani 1 1 d . . . O2 O -0.46042(13) 0.45954(10) 0.17358(9) 0.0296(3) Uani 1 1 d . . . O3 O 0.20308(12) 0.28311(10) 0.44436(8) 0.0239(3) Uani 1 1 d . . . C1 C -0.0856(2) 0.03308(14) 0.31579(12) 0.0246(4) Uani 1 1 d . . . C2 C -0.0731(2) 0.04656(14) 0.21311(12) 0.0262(4) Uani 1 1 d . . . C3 C 0.05098(17) 0.14504(13) 0.08631(12) 0.0210(3) Uani 1 1 d . . . C4 C 0.1928(3) 0.18997(19) -0.04165(17) 0.0441(6) Uani 1 1 d . . . H4A H 0.2911 0.1730 -0.0266 0.053 Uiso 1 1 calc R . . H4B H 0.1821 0.2444 -0.1034 0.053 Uiso 1 1 calc R . . C5 C 0.1344(2) 0.09133(17) -0.03689(14) 0.0329(4) Uani 1 1 d . . . C6 C -0.29707(19) 0.15616(15) 0.32032(14) 0.0273(4) Uani 1 1 d . . . C7 C -0.34808(19) 0.27595(16) 0.29702(14) 0.0292(4) Uani 1 1 d . . . C8 C -0.32844(18) 0.42073(14) 0.16034(13) 0.0237(4) Uani 1 1 d . . . C9 C -0.3641(2) 0.58512(16) 0.04724(16) 0.0344(4) Uani 1 1 d . . . C10 C -0.4986(2) 0.55666(16) 0.09600(14) 0.0326(4) Uani 1 1 d . . . C11 C -0.11374(18) 0.13366(14) 0.42536(12) 0.0216(3) Uani 1 1 d . . . C12 C 0.03177(18) 0.15653(14) 0.42445(12) 0.0219(3) Uani 1 1 d . . . C13 C 0.12731(17) 0.31685(13) 0.36847(11) 0.0199(3) Uani 1 1 d . . . C14 C 0.2621(2) 0.44965(17) 0.34988(14) 0.0304(4) Uani 1 1 d . . . C15 C 0.2710(3) 0.37118(18) 0.44713(15) 0.0373(5) Uani 1 1 d . . . H5 H 0.114(2) 0.2786(18) 0.0395(15) 0.026(6) Uiso 1 1 d . . . H7 H 0.127(2) 0.4383(19) 0.2637(17) 0.036(6) Uiso 1 1 d . . . H6 H -0.188(3) 0.477(2) 0.0739(19) 0.056(8) Uiso 1 1 d . . . H1A H -0.139(2) -0.0234(18) 0.3460(15) 0.033(6) Uiso 1 1 d . . . H1B H 0.007(2) 0.0126(15) 0.3393(13) 0.020(5) Uiso 1 1 d . . . H2A H -0.017(2) -0.0149(18) 0.2043(14) 0.028(5) Uiso 1 1 d . . . H2B H -0.164(2) 0.0514(16) 0.1877(14) 0.024(5) Uiso 1 1 d . . . H5A H 0.062(3) 0.103(2) -0.0810(18) 0.046(7) Uiso 1 1 d . . . H5B H 0.199(3) 0.033(2) -0.0411(16) 0.041(6) Uiso 1 1 d . . . H6A H -0.346(2) 0.1167(17) 0.3749(15) 0.028(5) Uiso 1 1 d . . . H6B H -0.316(2) 0.1325(16) 0.2693(14) 0.024(5) Uiso 1 1 d . . . H7A H -0.444(2) 0.2873(18) 0.2836(15) 0.035(6) Uiso 1 1 d . . . H7B H -0.339(2) 0.3025(17) 0.3504(15) 0.029(5) Uiso 1 1 d . . . H9A H -0.369(2) 0.6066(19) -0.0199(17) 0.040(6) Uiso 1 1 d . . . H9B H -0.331(2) 0.6375(18) 0.0683(15) 0.034(6) Uiso 1 1 d . . . H10A H -0.550(2) 0.6050(19) 0.1236(16) 0.039(6) Uiso 1 1 d . . . H10B H -0.560(2) 0.5385(17) 0.0595(15) 0.031(6) Uiso 1 1 d . . . H11A H -0.127(2) 0.0653(17) 0.4725(14) 0.025(5) Uiso 1 1 d . . . H11B H -0.177(2) 0.1885(16) 0.4417(14) 0.023(5) Uiso 1 1 d . . . H12A H 0.048(2) 0.1607(16) 0.4823(15) 0.025(5) Uiso 1 1 d . . . H12B H 0.095(2) 0.1010(16) 0.4147(13) 0.021(5) Uiso 1 1 d . . . H14A H 0.242(2) 0.5216(19) 0.3484(15) 0.034(6) Uiso 1 1 d . . . H14B H 0.343(3) 0.4422(19) 0.3137(17) 0.040(6) Uiso 1 1 d . . . H15A H 0.362(3) 0.339(2) 0.4667(19) 0.059(8) Uiso 1 1 d . . . H15B H 0.221(3) 0.402(2) 0.4919(18) 0.046(7) Uiso 1 1 d . . . B1 B 0.40609(19) 0.80421(15) 0.26848(13) 0.0184(4) Uani 1 1 d . . . C16 C 0.35555(17) 0.80174(13) 0.16939(11) 0.0207(3) Uani 1 1 d . . . C17 C 0.24774(19) 0.74974(15) 0.15834(13) 0.0270(4) Uani 1 1 d . . . C18 C 0.2164(2) 0.74388(17) 0.07288(14) 0.0335(4) Uani 1 1 d . . . C19 C 0.2920(2) 0.79032(17) -0.00548(14) 0.0359(5) Uani 1 1 d . . . C20 C 0.3979(2) 0.84349(16) 0.00159(14) 0.0343(5) Uani 1 1 d . . . C21 C 0.4281(2) 0.84860(15) 0.08736(13) 0.0273(4) Uani 1 1 d . . . C22 C 0.32290(16) 0.73043(13) 0.35730(11) 0.0183(3) Uani 1 1 d . . . C23 C 0.17906(17) 0.74840(14) 0.36524(12) 0.0219(3) Uani 1 1 d . . . C24 C 0.10417(18) 0.68848(15) 0.43895(12) 0.0242(4) Uani 1 1 d . . . C25 C 0.17153(19) 0.60902(14) 0.51163(12) 0.0242(4) Uani 1 1 d . . . C26 C 0.31389(19) 0.59137(14) 0.50831(12) 0.0228(3) Uani 1 1 d . . . C27 C 0.38690(17) 0.64986(13) 0.43218(11) 0.0199(3) Uani 1 1 d . . . C28 C 0.57089(16) 0.75687(13) 0.27320(11) 0.0188(3) Uani 1 1 d . . . C29 C 0.61545(17) 0.65260(14) 0.26899(11) 0.0200(3) Uani 1 1 d . . . C30 C 0.75247(18) 0.60657(14) 0.27420(12) 0.0221(3) Uani 1 1 d . . . C31 C 0.85234(18) 0.66425(15) 0.28388(13) 0.0252(4) Uani 1 1 d . . . C32 C 0.81298(18) 0.76794(15) 0.28683(13) 0.0258(4) Uani 1 1 d . . . C33 C 0.67512(18) 0.81313(14) 0.28139(12) 0.0221(3) Uani 1 1 d . . . C34 C 0.38186(16) 0.92619(13) 0.27728(12) 0.0205(3) Uani 1 1 d . . . C35 C 0.34991(19) 1.02051(15) 0.20448(14) 0.0273(4) Uani 1 1 d . . . C36 C 0.3375(2) 1.12210(16) 0.21470(16) 0.0332(4) Uani 1 1 d . . . C37 C 0.35563(18) 1.13242(16) 0.29970(16) 0.0324(4) Uani 1 1 d . . . C38 C 0.3850(2) 1.04077(17) 0.37425(15) 0.0322(4) Uani 1 1 d . . . C39 C 0.39776(19) 0.94030(15) 0.36288(13) 0.0276(4) Uani 1 1 d . . . H17A H 0.190(2) 0.7158(18) 0.2135(16) 0.033(6) Uiso 1 1 d . . . H18A H 0.138(3) 0.702(2) 0.0695(17) 0.047(7) Uiso 1 1 d . . . H19A H 0.276(2) 0.7843(19) -0.0650(17) 0.041(6) Uiso 1 1 d . . . H20A H 0.453(2) 0.8750(19) -0.0489(17) 0.039(6) Uiso 1 1 d . . . H21A H 0.499(2) 0.8822(16) 0.0917(14) 0.022(5) Uiso 1 1 d . . . H23A H 0.132(2) 0.8052(17) 0.3167(14) 0.025(5) Uiso 1 1 d . . . H24A H 0.009(2) 0.7021(16) 0.4399(14) 0.027(5) Uiso 1 1 d . . . H25A H 0.121(2) 0.5690(17) 0.5599(15) 0.032(6) Uiso 1 1 d . . . H26A H 0.361(2) 0.5405(17) 0.5557(14) 0.026(5) Uiso 1 1 d . . . H27A H 0.484(2) 0.6345(14) 0.4314(12) 0.014(4) Uiso 1 1 d . . . H29A H 0.547(2) 0.6099(15) 0.2637(13) 0.018(5) Uiso 1 1 d . . . H30A H 0.777(2) 0.5367(17) 0.2698(14) 0.027(5) Uiso 1 1 d . . . H31A H 0.944(2) 0.6345(17) 0.2887(14) 0.029(5) Uiso 1 1 d . . . H32A H 0.881(2) 0.8057(17) 0.2942(14) 0.029(5) Uiso 1 1 d . . . H33A H 0.6515(19) 0.8822(16) 0.2861(13) 0.018(5) Uiso 1 1 d . . . H35A H 0.335(2) 1.0159(17) 0.1463(15) 0.029(5) Uiso 1 1 d . . . H36A H 0.313(3) 1.183(2) 0.1630(17) 0.045(7) Uiso 1 1 d . . . H37A H 0.348(2) 1.2008(18) 0.3063(15) 0.034(6) Uiso 1 1 d . . . H38A H 0.396(2) 1.0461(19) 0.4315(17) 0.042(6) Uiso 1 1 d . . . H39A H 0.423(2) 0.8754(18) 0.4156(16) 0.034(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.01958(13) 0.01501(13) 0.01688(13) -0.00396(9) -0.00215(9) -0.00250(9) Cl1 0.0347(2) 0.0239(2) 0.0226(2) -0.00431(17) 0.00041(17) -0.00867(17) N1 0.0213(7) 0.0189(7) 0.0200(7) -0.0053(5) -0.0036(5) -0.0043(5) N2 0.0250(7) 0.0169(7) 0.0201(7) -0.0049(5) -0.0030(6) -0.0042(5) N3 0.0219(7) 0.0209(7) 0.0262(8) -0.0051(6) -0.0041(6) -0.0021(6) N4 0.0207(7) 0.0175(7) 0.0184(7) -0.0046(5) -0.0012(5) -0.0032(5) N5 0.0298(8) 0.0232(8) 0.0234(8) -0.0106(6) 0.0020(6) -0.0065(6) N6 0.0298(9) 0.0212(8) 0.0293(8) -0.0029(6) -0.0059(7) 0.0012(6) N7 0.0361(9) 0.0249(8) 0.0256(8) -0.0066(7) -0.0053(7) -0.0125(7) O1 0.0317(7) 0.0264(6) 0.0284(7) -0.0163(5) 0.0025(5) -0.0067(5) O2 0.0243(6) 0.0259(7) 0.0372(7) -0.0107(6) -0.0072(5) 0.0054(5) O3 0.0239(6) 0.0271(6) 0.0237(6) -0.0098(5) -0.0055(5) -0.0063(5) C1 0.0355(10) 0.0165(8) 0.0218(8) -0.0046(7) -0.0031(7) -0.0053(7) C2 0.0386(11) 0.0180(8) 0.0233(9) -0.0062(7) -0.0033(8) -0.0070(7) C3 0.0202(8) 0.0202(8) 0.0242(8) -0.0090(7) -0.0070(6) 0.0005(6) C4 0.0512(14) 0.0494(13) 0.0451(13) -0.0305(11) 0.0237(11) -0.0256(11) C5 0.0391(11) 0.0358(11) 0.0300(10) -0.0191(9) 0.0069(8) -0.0093(9) C6 0.0236(9) 0.0274(9) 0.0295(10) -0.0040(8) -0.0039(7) -0.0087(7) C7 0.0193(9) 0.0306(10) 0.0340(10) -0.0056(8) 0.0002(7) -0.0030(7) C8 0.0241(9) 0.0214(8) 0.0300(9) -0.0136(7) -0.0068(7) -0.0012(7) C9 0.0397(11) 0.0206(9) 0.0408(12) -0.0062(8) -0.0141(9) 0.0011(8) C10 0.0377(11) 0.0253(9) 0.0354(11) -0.0140(8) -0.0157(9) 0.0103(8) C11 0.0258(9) 0.0200(8) 0.0182(8) -0.0040(7) 0.0002(6) -0.0058(7) C12 0.0271(9) 0.0190(8) 0.0187(8) -0.0036(7) -0.0048(7) -0.0033(7) C13 0.0195(8) 0.0220(8) 0.0192(8) -0.0094(7) 0.0004(6) -0.0004(6) C14 0.0328(10) 0.0326(11) 0.0326(10) -0.0149(8) 0.0014(8) -0.0159(8) C15 0.0447(13) 0.0391(12) 0.0358(11) -0.0134(9) -0.0074(10) -0.0214(10) B1 0.0166(8) 0.0187(9) 0.0194(9) -0.0054(7) -0.0021(7) -0.0019(7) C16 0.0196(8) 0.0190(8) 0.0214(8) -0.0062(6) -0.0046(6) 0.0051(6) C17 0.0218(9) 0.0319(10) 0.0295(10) -0.0135(8) -0.0056(7) 0.0009(7) C18 0.0266(10) 0.0402(11) 0.0378(11) -0.0193(9) -0.0135(8) 0.0052(8) C19 0.0411(12) 0.0386(11) 0.0268(10) -0.0141(9) -0.0164(8) 0.0138(9) C20 0.0436(12) 0.0308(10) 0.0213(9) -0.0045(8) -0.0015(8) 0.0074(9) C21 0.0298(10) 0.0244(9) 0.0254(9) -0.0064(7) -0.0012(7) 0.0001(7) C22 0.0191(8) 0.0186(8) 0.0200(8) -0.0091(6) -0.0020(6) -0.0039(6) C23 0.0206(8) 0.0238(8) 0.0211(8) -0.0078(7) -0.0024(6) -0.0004(7) C24 0.0195(8) 0.0315(9) 0.0250(9) -0.0140(7) 0.0025(7) -0.0039(7) C25 0.0286(9) 0.0243(9) 0.0207(8) -0.0088(7) 0.0058(7) -0.0071(7) C26 0.0286(9) 0.0206(8) 0.0187(8) -0.0065(7) -0.0022(7) -0.0007(7) C27 0.0189(8) 0.0214(8) 0.0212(8) -0.0090(7) -0.0035(6) -0.0016(6) C28 0.0178(8) 0.0207(8) 0.0165(8) -0.0039(6) -0.0009(6) -0.0021(6) C29 0.0200(8) 0.0219(8) 0.0181(8) -0.0052(6) -0.0018(6) -0.0045(6) C30 0.0242(9) 0.0205(8) 0.0197(8) -0.0052(7) -0.0008(6) 0.0000(7) C31 0.0169(8) 0.0293(9) 0.0272(9) -0.0078(7) -0.0018(7) 0.0011(7) C32 0.0191(8) 0.0280(9) 0.0314(10) -0.0090(8) -0.0031(7) -0.0060(7) C33 0.0211(8) 0.0195(8) 0.0257(9) -0.0070(7) -0.0013(7) -0.0029(6) C34 0.0141(7) 0.0220(8) 0.0263(8) -0.0094(7) 0.0001(6) -0.0021(6) C35 0.0245(9) 0.0241(9) 0.0334(10) -0.0095(8) -0.0063(7) -0.0002(7) C36 0.0262(10) 0.0214(9) 0.0503(12) -0.0095(9) -0.0078(9) 0.0010(7) C37 0.0174(8) 0.0278(10) 0.0596(13) -0.0254(10) 0.0033(8) -0.0033(7) C38 0.0271(10) 0.0397(11) 0.0398(11) -0.0255(9) 0.0076(8) -0.0110(8) C39 0.0277(9) 0.0283(10) 0.0286(10) -0.0114(8) 0.0029(7) -0.0058(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 N2 2.1593(14) . ? Mn1 N3 2.1630(15) . ? Mn1 N4 2.1700(14) . ? Mn1 N1 2.3040(14) . ? Mn1 Cl1 2.4556(5) . ? N1 C6 1.474(2) . ? N1 C11 1.477(2) . ? N1 C1 1.477(2) . ? N2 C3 1.287(2) . ? N2 C2 1.474(2) . ? N3 C8 1.290(2) . ? N3 C7 1.476(2) . ? N4 C13 1.287(2) . ? N4 C12 1.475(2) . ? N5 C3 1.341(2) . ? N5 C4 1.437(3) . ? N6 C8 1.346(2) . ? N6 C9 1.456(2) . ? N7 C13 1.343(2) . ? N7 C14 1.459(2) . ? O1 C3 1.345(2) . ? O1 C5 1.461(2) . ? O2 C8 1.347(2) . ? O2 C10 1.466(2) . ? O3 C13 1.346(2) . ? O3 C15 1.454(2) . ? C1 C2 1.520(2) . ? C4 C5 1.495(3) . ? C6 C7 1.524(3) . ? C9 C10 1.510(3) . ? C11 C12 1.515(2) . ? C14 C15 1.517(3) . ? B1 C22 1.643(2) . ? B1 C28 1.647(2) . ? B1 C16 1.648(2) . ? B1 C34 1.649(2) . ? C16 C21 1.403(3) . ? C16 C17 1.409(3) . ? C17 C18 1.398(3) . ? C18 C19 1.378(3) . ? C19 C20 1.383(3) . ? C20 C21 1.396(3) . ? C22 C27 1.404(2) . ? C22 C23 1.404(2) . ? C23 C24 1.388(2) . ? C24 C25 1.391(3) . ? C25 C26 1.387(3) . ? C26 C27 1.392(2) . ? C28 C33 1.402(2) . ? C28 C29 1.406(2) . ? C29 C30 1.390(2) . ? C30 C31 1.388(3) . ? C31 C32 1.385(3) . ? C32 C33 1.395(2) . ? C34 C35 1.394(2) . ? C34 C39 1.407(3) . ? C35 C36 1.395(3) . ? C36 C37 1.381(3) . ? C37 C38 1.384(3) . ? C38 C39 1.387(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 N2 Mn1 N3 108.88(6) . . ? N2 Mn1 N4 122.35(5) . . ? N3 Mn1 N4 115.78(5) . . ? N2 Mn1 N1 77.45(5) . . ? N3 Mn1 N1 78.12(5) . . ? N4 Mn1 N1 78.07(5) . . ? N2 Mn1 Cl1 104.46(4) . . ? N3 Mn1 Cl1 102.97(4) . . ? N4 Mn1 Cl1 99.17(4) . . ? N1 Mn1 Cl1 177.23(4) . . ? C6 N1 C11 111.59(14) . . ? C6 N1 C1 112.12(14) . . ? C11 N1 C1 111.08(13) . . ? C6 N1 Mn1 107.67(10) . . ? C11 N1 Mn1 107.09(10) . . ? C1 N1 Mn1 106.99(10) . . ? C3 N2 C2 115.52(15) . . ? C3 N2 Mn1 128.67(12) . . ? C2 N2 Mn1 115.68(11) . . ? C8 N3 C7 117.05(15) . . ? C8 N3 Mn1 130.07(13) . . ? C7 N3 Mn1 112.41(11) . . ? C13 N4 C12 116.11(14) . . ? C13 N4 Mn1 131.40(11) . . ? C12 N4 Mn1 111.50(10) . . ? C3 N5 C4 110.50(16) . . ? C8 N6 C9 110.57(17) . . ? C13 N7 C14 111.09(16) . . ? C3 O1 C5 108.19(14) . . ? C8 O2 C10 108.44(15) . . ? C13 O3 C15 108.46(14) . . ? N1 C1 C2 111.61(14) . . ? N2 C2 C1 109.62(14) . . ? N2 C3 N5 126.64(16) . . ? N2 C3 O1 122.75(16) . . ? N5 C3 O1 110.61(15) . . ? N5 C4 C5 101.95(16) . . ? O1 C5 C4 104.22(15) . . ? N1 C6 C7 110.86(15) . . ? N3 C7 C6 108.93(15) . . ? N3 C8 N6 126.79(17) . . ? N3 C8 O2 122.64(17) . . ? N6 C8 O2 110.56(15) . . ? N6 C9 C10 100.90(16) . . ? O2 C10 C9 104.74(15) . . ? N1 C11 C12 110.57(14) . . ? N4 C12 C11 108.37(13) . . ? N4 C13 N7 126.84(16) . . ? N4 C13 O3 122.58(15) . . ? N7 C13 O3 110.56(15) . . ? N7 C14 C15 100.20(15) . . ? O3 C15 C14 104.81(15) . . ? C22 B1 C28 109.78(13) . . ? C22 B1 C16 112.21(13) . . ? C28 B1 C16 106.30(13) . . ? C22 B1 C34 106.19(13) . . ? C28 B1 C34 109.90(13) . . ? C16 B1 C34 112.49(13) . . ? C21 C16 C17 114.55(16) . . ? C21 C16 B1 119.60(15) . . ? C17 C16 B1 125.72(15) . . ? C18 C17 C16 122.92(19) . . ? C19 C18 C17 120.18(19) . . ? C18 C19 C20 119.09(18) . . ? C19 C20 C21 120.1(2) . . ? C20 C21 C16 123.15(19) . . ? C27 C22 C23 114.85(15) . . ? C27 C22 B1 124.06(14) . . ? C23 C22 B1 121.01(14) . . ? C24 C23 C22 123.18(16) . . ? C23 C24 C25 120.11(16) . . ? C26 C25 C24 118.59(16) . . ? C25 C26 C27 120.33(16) . . ? C26 C27 C22 122.84(16) . . ? C33 C28 C29 115.28(15) . . ? C33 C28 B1 124.91(15) . . ? C29 C28 B1 119.81(14) . . ? C30 C29 C28 123.06(16) . . ? C31 C30 C29 119.89(16) . . ? C32 C31 C30 118.87(16) . . ? C31 C32 C33 120.59(17) . . ? C32 C33 C28 122.29(16) . . ? C35 C34 C39 115.31(16) . . ? C35 C34 B1 125.01(16) . . ? C39 C34 B1 119.65(15) . . ? C34 C35 C36 122.67(19) . . ? C37 C36 C35 120.16(19) . . ? C36 C37 C38 119.05(18) . . ? C37 C38 C39 120.11(19) . . ? C38 C39 C34 122.67(18) . . ? 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 Mn1 N1 C6 -100.43(12) . . . . ? N3 Mn1 N1 C6 12.26(11) . . . . ? N4 Mn1 N1 C6 132.17(12) . . . . ? Cl1 Mn1 N1 C6 125.7(8) . . . . ? N2 Mn1 N1 C11 139.44(11) . . . . ? N3 Mn1 N1 C11 -107.87(11) . . . . ? N4 Mn1 N1 C11 12.04(10) . . . . ? Cl1 Mn1 N1 C11 5.6(9) . . . . ? N2 Mn1 N1 C1 20.27(10) . . . . ? N3 Mn1 N1 C1 132.95(11) . . . . ? N4 Mn1 N1 C1 -107.13(11) . . . . ? Cl1 Mn1 N1 C1 -113.6(8) . . . . ? N3 Mn1 N2 C3 108.05(15) . . . . ? N4 Mn1 N2 C3 -112.41(14) . . . . ? N1 Mn1 N2 C3 -179.35(15) . . . . ? Cl1 Mn1 N2 C3 -1.42(15) . . . . ? N3 Mn1 N2 C2 -67.75(13) . . . . ? N4 Mn1 N2 C2 71.78(13) . . . . ? N1 Mn1 N2 C2 4.85(12) . . . . ? Cl1 Mn1 N2 C2 -177.22(11) . . . . ? N2 Mn1 N3 C8 -100.23(16) . . . . ? N4 Mn1 N3 C8 117.28(16) . . . . ? N1 Mn1 N3 C8 -172.37(17) . . . . ? Cl1 Mn1 N3 C8 10.24(16) . . . . ? N2 Mn1 N3 C7 88.07(13) . . . . ? N4 Mn1 N3 C7 -54.42(13) . . . . ? N1 Mn1 N3 C7 15.93(12) . . . . ? Cl1 Mn1 N3 C7 -161.46(11) . . . . ? N2 Mn1 N4 C13 118.54(15) . . . . ? N3 Mn1 N4 C13 -104.45(15) . . . . ? N1 Mn1 N4 C13 -174.83(16) . . . . ? Cl1 Mn1 N4 C13 4.85(15) . . . . ? N2 Mn1 N4 C12 -49.38(13) . . . . ? N3 Mn1 N4 C12 87.63(12) . . . . ? N1 Mn1 N4 C12 17.25(11) . . . . ? Cl1 Mn1 N4 C12 -163.07(10) . . . . ? C6 N1 C1 C2 75.49(19) . . . . ? C11 N1 C1 C2 -158.89(15) . . . . ? Mn1 N1 C1 C2 -42.33(17) . . . . ? C3 N2 C2 C1 154.88(16) . . . . ? Mn1 N2 C2 C1 -28.75(18) . . . . ? N1 C1 C2 N2 47.9(2) . . . . ? C2 N2 C3 N5 177.70(16) . . . . ? Mn1 N2 C3 N5 1.9(3) . . . . ? C2 N2 C3 O1 -2.5(2) . . . . ? Mn1 N2 C3 O1 -178.28(11) . . . . ? C4 N5 C3 N2 168.80(19) . . . . ? C4 N5 C3 O1 -11.0(2) . . . . ? C5 O1 C3 N2 176.90(17) . . . . ? C5 O1 C3 N5 -3.24(19) . . . . ? C3 N5 C4 C5 19.7(2) . . . . ? C3 O1 C5 C4 15.3(2) . . . . ? N5 C4 C5 O1 -20.4(2) . . . . ? C11 N1 C6 C7 79.35(18) . . . . ? C1 N1 C6 C7 -155.31(15) . . . . ? Mn1 N1 C6 C7 -37.89(18) . . . . ? C8 N3 C7 C6 146.01(16) . . . . ? Mn1 N3 C7 C6 -41.12(18) . . . . ? N1 C6 C7 N3 53.3(2) . . . . ? C7 N3 C8 N6 -176.00(17) . . . . ? Mn1 N3 C8 N6 12.6(3) . . . . ? C7 N3 C8 O2 3.2(2) . . . . ? Mn1 N3 C8 O2 -168.15(12) . . . . ? C9 N6 C8 N3 -166.18(18) . . . . ? C9 N6 C8 O2 14.5(2) . . . . ? C10 O2 C8 N3 -179.60(16) . . . . ? C10 O2 C8 N6 -0.25(19) . . . . ? C8 N6 C9 C10 -21.4(2) . . . . ? C8 O2 C10 C9 -13.14(19) . . . . ? N6 C9 C10 O2 19.97(19) . . . . ? C6 N1 C11 C12 -156.72(14) . . . . ? C1 N1 C11 C12 77.37(17) . . . . ? Mn1 N1 C11 C12 -39.13(15) . . . . ? C13 N4 C12 C11 146.48(15) . . . . ? Mn1 N4 C12 C11 -43.59(16) . . . . ? N1 C11 C12 N4 55.99(18) . . . . ? C12 N4 C13 N7 -173.81(17) . . . . ? Mn1 N4 C13 N7 18.7(3) . . . . ? C12 N4 C13 O3 4.3(2) . . . . ? Mn1 N4 C13 O3 -163.21(11) . . . . ? C14 N7 C13 N4 -171.43(17) . . . . ? C14 N7 C13 O3 10.3(2) . . . . ? C15 O3 C13 N4 -173.56(17) . . . . ? C15 O3 C13 N7 4.8(2) . . . . ? C13 N7 C14 C15 -19.7(2) . . . . ? C13 O3 C15 C14 -17.0(2) . . . . ? N7 C14 C15 O3 21.2(2) . . . . ? C22 B1 C16 C21 -171.56(14) . . . . ? C28 B1 C16 C21 -51.55(19) . . . . ? C34 B1 C16 C21 68.77(19) . . . . ? C22 B1 C16 C17 4.2(2) . . . . ? C28 B1 C16 C17 124.17(17) . . . . ? C34 B1 C16 C17 -115.50(18) . . . . ? C21 C16 C17 C18 0.8(3) . . . . ? B1 C16 C17 C18 -175.10(17) . . . . ? C16 C17 C18 C19 -0.1(3) . . . . ? C17 C18 C19 C20 -0.6(3) . . . . ? C18 C19 C20 C21 0.7(3) . . . . ? C19 C20 C21 C16 0.0(3) . . . . ? C17 C16 C21 C20 -0.7(3) . . . . ? B1 C16 C21 C20 175.45(16) . . . . ? C28 B1 C22 C27 8.8(2) . . . . ? C16 B1 C22 C27 126.75(16) . . . . ? C34 B1 C22 C27 -109.96(17) . . . . ? C28 B1 C22 C23 -174.48(14) . . . . ? C16 B1 C22 C23 -56.5(2) . . . . ? C34 B1 C22 C23 66.76(19) . . . . ? C27 C22 C23 C24 -2.8(2) . . . . ? B1 C22 C23 C24 -179.86(16) . . . . ? C22 C23 C24 C25 2.8(3) . . . . ? C23 C24 C25 C26 -0.2(3) . . . . ? C24 C25 C26 C27 -2.1(3) . . . . ? C25 C26 C27 C22 1.9(3) . . . . ? C23 C22 C27 C26 0.5(2) . . . . ? B1 C22 C27 C26 177.41(15) . . . . ? C22 B1 C28 C33 -117.77(17) . . . . ? C16 B1 C28 C33 120.66(17) . . . . ? C34 B1 C28 C33 -1.3(2) . . . . ? C22 B1 C28 C29 62.21(19) . . . . ? C16 B1 C28 C29 -59.36(18) . . . . ? C34 B1 C28 C29 178.65(14) . . . . ? C33 C28 C29 C30 1.2(2) . . . . ? B1 C28 C29 C30 -178.83(15) . . . . ? C28 C29 C30 C31 -0.1(3) . . . . ? C29 C30 C31 C32 -0.9(3) . . . . ? C30 C31 C32 C33 0.8(3) . . . . ? C31 C32 C33 C28 0.3(3) . . . . ? C29 C28 C33 C32 -1.2(2) . . . . ? B1 C28 C33 C32 178.75(16) . . . . ? C22 B1 C34 C35 -135.84(17) . . . . ? C28 B1 C34 C35 105.49(18) . . . . ? C16 B1 C34 C35 -12.7(2) . . . . ? C22 B1 C34 C39 46.29(19) . . . . ? C28 B1 C34 C39 -72.39(19) . . . . ? C16 B1 C34 C39 169.39(15) . . . . ? C39 C34 C35 C36 1.4(3) . . . . ? B1 C34 C35 C36 -176.53(17) . . . . ? C34 C35 C36 C37 -0.7(3) . . . . ? C35 C36 C37 C38 -0.5(3) . . . . ? C36 C37 C38 C39 0.9(3) . . . . ? C37 C38 C39 C34 -0.1(3) . . . . ? C35 C34 C39 C38 -1.1(3) . . . . ? B1 C34 C39 C38 177.03(17) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.825 _refine_diff_density_min -0.500 _refine_diff_density_rms 0.052 #==END data_asb103 _database_code_depnum_ccdc_archive 'CCDC 855306' #TrackingRef '- DT-ART-11-2011-012244-CIF.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H47 B Cl Fe N7 O3' _chemical_formula_weight 763.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2339(5) _cell_length_b 12.5888(5) _cell_length_c 14.1351(6) _cell_angle_alpha 89.8857(5) _cell_angle_beta 75.3156(5) _cell_angle_gamma 72.3284(5) _cell_volume 1836.36(13) _cell_formula_units_Z 2 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used 9928 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 28.65 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 804 _exptl_absorpt_coefficient_mu 0.532 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8315 _exptl_absorpt_correction_T_max 0.9487 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX II CCD' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19949 _diffrn_reflns_av_R_equivalents 0.0164 _diffrn_reflns_av_sigmaI/netI 0.0189 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7480 _reflns_number_gt 6748 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX2' _computing_cell_refinement 'Bruker SMART APEX2/SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0355P)^2^+1.2217P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7480 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0786 _refine_ls_wR_factor_gt 0.0759 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 Fe1 Fe 1.01234(2) 0.302150(17) 0.697679(15) 0.01645(7) Uani 1 1 d . A . Cl1 Cl 1.14848(3) 0.20804(3) 0.53907(3) 0.02057(9) Uani 1 1 d . . . O1 O 1.29570(10) 0.12751(9) 0.84840(8) 0.0215(2) Uani 1 1 d . A . O2 O 0.77431(11) 0.08356(10) 0.72522(8) 0.0240(2) Uani 1 1 d . A . O3 O 1.05575(11) 0.62134(9) 0.60257(8) 0.0233(2) Uani 1 1 d . A . N1 N 0.87702(12) 0.39096(11) 0.83687(9) 0.0197(3) Uani 1 1 d . . . N2 N 1.12102(12) 0.23378(11) 0.79511(9) 0.0200(3) Uani 1 1 d . . . N3 N 0.86180(12) 0.22910(11) 0.71526(10) 0.0222(3) Uani 1 1 d . . . N4 N 1.00684(13) 0.46903(11) 0.67199(10) 0.0224(3) Uani 1 1 d . . . N5 N 1.31876(13) 0.12389(11) 0.68834(10) 0.0219(3) Uani 1 1 d . . . N6 N 0.97102(14) 0.05269(12) 0.62667(10) 0.0234(3) Uani 1 1 d . . . N7 N 1.17345(15) 0.45579(13) 0.52720(11) 0.0300(3) Uani 1 1 d . . . H5 H 1.2937(18) 0.1340(16) 0.6354(15) 0.025(5) Uiso 1 1 d . . . H6 H 1.039(2) 0.0664(16) 0.6100(14) 0.025(5) Uiso 1 1 d . . . H7 H 1.188(2) 0.3886(19) 0.5150(16) 0.037(6) Uiso 1 1 d . . . C1 C 0.9126(2) 0.3204(2) 0.91554(18) 0.0241(5) Uiso 0.65 1 d P A 1 H1A H 0.8761 0.2578 0.9184 0.029 Uiso 0.65 1 calc PR A 1 H1B H 0.8741 0.3655 0.9794 0.029 Uiso 0.65 1 calc PR A 1 C1B C 0.9515(5) 0.3887(4) 0.9060(4) 0.0277(10) Uiso 0.35 1 d P A 2 H1B1 H 0.8929 0.4047 0.9732 0.033 Uiso 0.35 1 calc PR A 2 H1B2 H 0.9932 0.4482 0.8937 0.033 Uiso 0.35 1 calc PR A 2 C2 C 1.05739(16) 0.27402(14) 0.89904(11) 0.0256(3) Uani 1 1 d . A . H2A H 1.0907 0.3329 0.9178 0.031 Uiso 1 1 calc R B 1 H2B H 1.0781 0.2115 0.9409 0.031 Uiso 1 1 calc R B 1 C3 C 1.23793(15) 0.16538(12) 0.77659(11) 0.0184(3) Uani 1 1 d . A . C4 C 1.43108(15) 0.06324(13) 0.80245(13) 0.0247(3) Uani 1 1 d . . . H4A H 1.4580 -0.0061 0.8354 0.030 Uiso 1 1 calc R A . H4B H 1.4891 0.1080 0.8052 0.030 Uiso 1 1 calc R . . C5 C 1.43424(15) 0.03616(13) 0.69686(12) 0.0233(3) Uani 1 1 d . A . H5A H 1.5136 0.0423 0.6501 0.028 Uiso 1 1 calc R . . H5B H 1.4272 -0.0393 0.6870 0.028 Uiso 1 1 calc R . . C6 C 0.7466(2) 0.4042(2) 0.82913(18) 0.0218(5) Uiso 0.65 1 d P A 1 H6A H 0.7226 0.4631 0.7847 0.026 Uiso 0.65 1 calc PR A 1 H6B H 0.6842 0.4277 0.8945 0.026 Uiso 0.65 1 calc PR A 1 C6B C 0.7765(4) 0.3309(4) 0.8707(3) 0.0238(9) Uiso 0.35 1 d P A 2 H6B1 H 0.8120 0.2663 0.9065 0.029 Uiso 0.35 1 calc PR A 2 H6B2 H 0.6984 0.3825 0.9166 0.029 Uiso 0.35 1 calc PR A 2 C7 C 0.74004(15) 0.29167(14) 0.78860(13) 0.0258(3) Uani 1 1 d . A . H7A H 0.7231 0.2449 0.8437 0.031 Uiso 1 1 calc R C 1 H7B H 0.6671 0.3072 0.7579 0.031 Uiso 1 1 calc R C 1 C8 C 0.87055(15) 0.12794(14) 0.68971(11) 0.0214(3) Uani 1 1 d . A . C9 C 0.81399(16) -0.03045(14) 0.68022(12) 0.0255(3) Uani 1 1 d . . . H9A H 0.7697 -0.0338 0.6285 0.031 Uiso 1 1 calc R A . H9B H 0.7939 -0.0824 0.7300 0.031 Uiso 1 1 calc R . . C10 C 0.95987(16) -0.05971(14) 0.63637(12) 0.0244(3) Uani 1 1 d . A . H10A H 1.0091 -0.1013 0.6811 0.029 Uiso 1 1 calc R . . H10B H 0.9888 -0.1034 0.5720 0.029 Uiso 1 1 calc R . . C11 C 0.8978(2) 0.5017(2) 0.84768(18) 0.0221(5) Uiso 0.65 1 d P A 1 H11A H 0.9769 0.4917 0.8700 0.027 Uiso 0.65 1 calc PR A 1 H11B H 0.8233 0.5522 0.8975 0.027 Uiso 0.65 1 calc PR A 1 C11B C 0.8095(5) 0.5038(4) 0.8145(4) 0.0266(10) Uiso 0.35 1 d P A 2 H11C H 0.7634 0.5522 0.8761 0.032 Uiso 0.35 1 calc PR A 2 H11D H 0.7450 0.5003 0.7791 0.032 Uiso 0.35 1 calc PR A 2 C12 C 0.91171(16) 0.55276(13) 0.74961(12) 0.0241(3) Uani 1 1 d . A . H12A H 0.8268 0.5775 0.7341 0.029 Uiso 1 1 calc R D 1 H12B H 0.9411 0.6189 0.7530 0.029 Uiso 1 1 calc R D 1 C13 C 1.07573(15) 0.51083(13) 0.60341(11) 0.0202(3) Uani 1 1 d . A . C14 C 1.15408(16) 0.64215(14) 0.52195(12) 0.0241(3) Uani 1 1 d . . . H14A H 1.2169 0.6669 0.5470 0.029 Uiso 1 1 calc R A . H14B H 1.1138 0.7002 0.4823 0.029 Uiso 1 1 calc R . . C15 C 1.22017(17) 0.53073(14) 0.46158(13) 0.0277(4) Uani 1 1 d . A . H15A H 1.1936 0.5310 0.3999 0.033 Uiso 1 1 calc R . . H15B H 1.3157 0.5110 0.4458 0.033 Uiso 1 1 calc R . . B1 B 0.68332(15) 0.26818(13) 0.21843(12) 0.0141(3) Uani 1 1 d . . . C16 C 0.64543(14) 0.25593(12) 0.33802(11) 0.0162(3) Uani 1 1 d . . . C17 C 0.70114(15) 0.15874(13) 0.38026(11) 0.0199(3) Uani 1 1 d . . . H17A H 0.7631 0.0971 0.3384 0.024 Uiso 1 1 calc R . . C18 C 0.66945(17) 0.14876(14) 0.48109(12) 0.0268(3) Uani 1 1 d . . . H18A H 0.7098 0.0812 0.5063 0.032 Uiso 1 1 calc R . . C19 C 0.57928(17) 0.23689(15) 0.54487(12) 0.0278(4) Uani 1 1 d . . . H19A H 0.5584 0.2308 0.6137 0.033 Uiso 1 1 calc R . . C20 C 0.52035(16) 0.33382(15) 0.50626(12) 0.0264(3) Uani 1 1 d . . . H20A H 0.4573 0.3945 0.5486 0.032 Uiso 1 1 calc R . . C21 C 0.55358(15) 0.34241(13) 0.40510(11) 0.0212(3) Uani 1 1 d . . . H21A H 0.5121 0.4100 0.3804 0.025 Uiso 1 1 calc R . . C22 C 0.59070(14) 0.22283(11) 0.16619(11) 0.0153(3) Uani 1 1 d . . . C23 C 0.45995(14) 0.23753(12) 0.21255(11) 0.0173(3) Uani 1 1 d . . . H23A H 0.4267 0.2656 0.2795 0.021 Uiso 1 1 calc R . . C24 C 0.37684(14) 0.21248(12) 0.16385(12) 0.0196(3) Uani 1 1 d . . . H24A H 0.2890 0.2237 0.1981 0.024 Uiso 1 1 calc R . . C25 C 0.42103(15) 0.17144(12) 0.06610(12) 0.0198(3) Uani 1 1 d . . . H25A H 0.3642 0.1551 0.0329 0.024 Uiso 1 1 calc R . . C26 C 0.55045(15) 0.15467(13) 0.01766(11) 0.0195(3) Uani 1 1 d . . . H26A H 0.5830 0.1263 -0.0493 0.023 Uiso 1 1 calc R . . C27 C 0.63248(14) 0.17960(12) 0.06757(11) 0.0176(3) Uani 1 1 d . . . H27A H 0.7207 0.1667 0.0332 0.021 Uiso 1 1 calc R . . C28 C 0.66010(13) 0.40044(12) 0.19584(10) 0.0147(3) Uani 1 1 d . . . C29 C 0.60617(14) 0.44856(12) 0.12047(11) 0.0181(3) Uani 1 1 d . . . H29A H 0.5744 0.4049 0.0843 0.022 Uiso 1 1 calc R . . C30 C 0.59718(15) 0.55766(13) 0.09632(12) 0.0213(3) Uani 1 1 d . . . H30A H 0.5608 0.5864 0.0442 0.026 Uiso 1 1 calc R . . C31 C 0.64108(15) 0.62426(13) 0.14805(12) 0.0232(3) Uani 1 1 d . . . H31A H 0.6365 0.6982 0.1312 0.028 Uiso 1 1 calc R . . C32 C 0.69205(16) 0.58111(13) 0.22511(12) 0.0235(3) Uani 1 1 d . . . H32A H 0.7208 0.6263 0.2623 0.028 Uiso 1 1 calc R . . C33 C 0.70090(14) 0.47206(12) 0.24770(11) 0.0192(3) Uani 1 1 d . . . H33A H 0.7361 0.4445 0.3006 0.023 Uiso 1 1 calc R . . C34 C 0.83760(13) 0.19628(12) 0.17267(10) 0.0146(3) Uani 1 1 d . . . C35 C 0.87909(14) 0.07961(12) 0.15130(11) 0.0184(3) Uani 1 1 d . . . H35A H 0.8157 0.0422 0.1604 0.022 Uiso 1 1 calc R . . C36 C 1.00967(15) 0.01669(13) 0.11729(11) 0.0223(3) Uani 1 1 d . . . H36A H 1.0334 -0.0620 0.1044 0.027 Uiso 1 1 calc R . . C37 C 1.10487(15) 0.06831(14) 0.10226(11) 0.0225(3) Uani 1 1 d . . . H37A H 1.1938 0.0259 0.0784 0.027 Uiso 1 1 calc R . . C38 C 1.06771(14) 0.18318(14) 0.12272(11) 0.0206(3) Uani 1 1 d . . . H38A H 1.1317 0.2199 0.1133 0.025 Uiso 1 1 calc R . . C39 C 0.93707(14) 0.24510(12) 0.15701(10) 0.0172(3) Uani 1 1 d . . . H39A H 0.9145 0.3237 0.1703 0.021 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 Fe1 0.01532(11) 0.01626(11) 0.01675(11) 0.00183(8) -0.00421(8) -0.00351(8) Cl1 0.01946(18) 0.02280(18) 0.01802(18) -0.00038(14) -0.00392(14) -0.00541(14) O1 0.0227(6) 0.0190(5) 0.0241(6) 0.0045(4) -0.0114(5) -0.0043(4) O2 0.0214(6) 0.0281(6) 0.0253(6) 0.0058(5) -0.0069(5) -0.0114(5) O3 0.0240(6) 0.0193(5) 0.0265(6) 0.0031(4) -0.0058(5) -0.0074(4) N1 0.0190(6) 0.0183(6) 0.0195(6) 0.0010(5) -0.0026(5) -0.0046(5) N2 0.0192(6) 0.0217(6) 0.0179(6) 0.0036(5) -0.0052(5) -0.0046(5) N3 0.0176(6) 0.0268(7) 0.0212(7) 0.0010(5) -0.0035(5) -0.0071(5) N4 0.0238(7) 0.0172(6) 0.0208(7) 0.0016(5) -0.0021(5) -0.0018(5) N5 0.0180(6) 0.0213(7) 0.0237(7) 0.0030(5) -0.0072(5) -0.0006(5) N6 0.0232(7) 0.0274(7) 0.0202(7) -0.0003(5) -0.0028(5) -0.0112(6) N7 0.0332(8) 0.0192(7) 0.0275(8) 0.0031(6) 0.0046(6) -0.0040(6) C2 0.0255(8) 0.0292(9) 0.0185(8) 0.0030(6) -0.0057(6) -0.0034(7) C3 0.0219(7) 0.0149(7) 0.0229(8) 0.0060(6) -0.0097(6) -0.0090(6) C4 0.0217(8) 0.0180(7) 0.0351(9) 0.0005(6) -0.0140(7) -0.0016(6) C5 0.0190(7) 0.0180(7) 0.0325(9) 0.0027(6) -0.0101(6) -0.0025(6) C7 0.0186(8) 0.0263(8) 0.0295(9) -0.0008(7) -0.0011(6) -0.0070(7) C8 0.0195(7) 0.0306(8) 0.0167(7) 0.0052(6) -0.0079(6) -0.0092(6) C9 0.0292(9) 0.0278(8) 0.0260(8) 0.0066(7) -0.0133(7) -0.0136(7) C10 0.0276(8) 0.0269(8) 0.0219(8) 0.0024(6) -0.0092(7) -0.0109(7) C12 0.0256(8) 0.0169(7) 0.0248(8) -0.0015(6) -0.0004(6) -0.0045(6) C13 0.0197(7) 0.0182(7) 0.0226(8) 0.0031(6) -0.0101(6) -0.0023(6) C14 0.0236(8) 0.0257(8) 0.0261(8) 0.0087(6) -0.0092(6) -0.0099(7) C15 0.0248(8) 0.0282(9) 0.0285(9) 0.0050(7) -0.0022(7) -0.0101(7) B1 0.0122(7) 0.0148(7) 0.0150(7) 0.0000(6) -0.0035(6) -0.0038(6) C16 0.0132(7) 0.0201(7) 0.0178(7) 0.0009(6) -0.0048(5) -0.0081(6) C17 0.0190(7) 0.0200(7) 0.0208(7) 0.0021(6) -0.0046(6) -0.0070(6) C18 0.0294(9) 0.0283(9) 0.0246(8) 0.0094(7) -0.0085(7) -0.0106(7) C19 0.0303(9) 0.0389(10) 0.0171(8) 0.0050(7) -0.0032(7) -0.0175(8) C20 0.0238(8) 0.0309(9) 0.0207(8) -0.0036(7) 0.0010(6) -0.0084(7) C21 0.0182(7) 0.0226(8) 0.0198(7) -0.0001(6) -0.0029(6) -0.0040(6) C22 0.0149(7) 0.0110(6) 0.0206(7) 0.0028(5) -0.0067(6) -0.0032(5) C23 0.0156(7) 0.0140(7) 0.0211(7) 0.0001(5) -0.0045(6) -0.0033(5) C24 0.0126(7) 0.0164(7) 0.0291(8) 0.0022(6) -0.0056(6) -0.0035(6) C25 0.0182(7) 0.0161(7) 0.0287(8) 0.0026(6) -0.0126(6) -0.0050(6) C26 0.0210(7) 0.0192(7) 0.0192(7) 0.0008(6) -0.0079(6) -0.0057(6) C27 0.0146(7) 0.0185(7) 0.0202(7) 0.0022(6) -0.0052(6) -0.0055(6) C28 0.0104(6) 0.0148(7) 0.0162(7) -0.0013(5) -0.0012(5) -0.0021(5) C29 0.0156(7) 0.0165(7) 0.0213(7) -0.0012(6) -0.0063(6) -0.0025(6) C30 0.0192(7) 0.0191(7) 0.0237(8) 0.0031(6) -0.0077(6) -0.0017(6) C31 0.0238(8) 0.0136(7) 0.0300(8) 0.0023(6) -0.0059(7) -0.0039(6) C32 0.0266(8) 0.0186(7) 0.0279(8) -0.0021(6) -0.0085(7) -0.0094(6) C33 0.0190(7) 0.0194(7) 0.0195(7) 0.0006(6) -0.0067(6) -0.0054(6) C34 0.0139(7) 0.0179(7) 0.0119(6) 0.0016(5) -0.0054(5) -0.0033(5) C35 0.0176(7) 0.0186(7) 0.0191(7) 0.0002(6) -0.0062(6) -0.0048(6) C36 0.0227(8) 0.0181(7) 0.0212(8) -0.0031(6) -0.0076(6) 0.0023(6) C37 0.0142(7) 0.0296(8) 0.0174(7) -0.0016(6) -0.0048(6) 0.0025(6) C38 0.0146(7) 0.0297(8) 0.0186(7) 0.0025(6) -0.0059(6) -0.0071(6) C39 0.0158(7) 0.0190(7) 0.0163(7) 0.0008(6) -0.0056(6) -0.0036(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 2.0828(13) . ? Fe1 N4 2.1163(13) . ? Fe1 N3 2.1208(13) . ? Fe1 N1 2.2119(13) . ? Fe1 Cl1 2.4375(4) . ? O1 C3 1.3501(18) . ? O1 C4 1.4642(19) . ? O2 C8 1.3504(19) . ? O2 C9 1.461(2) . ? O3 C13 1.3407(18) . ? O3 C14 1.4572(19) . ? N1 C1B 1.434(5) . ? N1 C6 1.456(3) . ? N1 C11B 1.469(5) . ? N1 C1 1.480(3) . ? N1 C11 1.495(3) . ? N1 C6B 1.522(5) . ? N2 C3 1.294(2) . ? N2 C2 1.475(2) . ? N3 C8 1.292(2) . ? N3 C7 1.482(2) . ? N4 C13 1.296(2) . ? N4 C12 1.4775(19) . ? N5 C3 1.339(2) . ? N5 C5 1.4581(19) . ? N6 C8 1.345(2) . ? N6 C10 1.461(2) . ? N7 C13 1.337(2) . ? N7 C15 1.441(2) . ? C1 C2 1.508(3) . ? C1B C2 1.552(5) . ? C4 C5 1.521(2) . ? C6 C7 1.559(3) . ? C6B C7 1.458(5) . ? C9 C10 1.525(2) . ? C11 C12 1.519(3) . ? C11B C12 1.560(5) . ? C14 C15 1.516(2) . ? B1 C22 1.645(2) . ? B1 C28 1.649(2) . ? B1 C34 1.650(2) . ? B1 C16 1.654(2) . ? C16 C17 1.402(2) . ? C16 C21 1.405(2) . ? C17 C18 1.394(2) . ? C18 C19 1.389(2) . ? C19 C20 1.384(2) . ? C20 C21 1.396(2) . ? C22 C23 1.403(2) . ? C22 C27 1.406(2) . ? C23 C24 1.396(2) . ? C24 C25 1.386(2) . ? C25 C26 1.392(2) . ? C26 C27 1.397(2) . ? C28 C29 1.404(2) . ? C28 C33 1.409(2) . ? C29 C30 1.394(2) . ? C30 C31 1.385(2) . ? C31 C32 1.391(2) . ? C32 C33 1.388(2) . ? C34 C39 1.402(2) . ? C34 C35 1.407(2) . ? C35 C36 1.396(2) . ? C36 C37 1.385(2) . ? C37 C38 1.387(2) . ? C38 C39 1.394(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N4 112.92(5) . . ? N2 Fe1 N3 107.75(5) . . ? N4 Fe1 N3 129.02(5) . . ? N2 Fe1 N1 80.24(5) . . ? N4 Fe1 N1 79.48(5) . . ? N3 Fe1 N1 78.44(5) . . ? N2 Fe1 Cl1 103.66(4) . . ? N4 Fe1 Cl1 99.89(4) . . ? N3 Fe1 Cl1 99.03(4) . . ? N1 Fe1 Cl1 175.91(4) . . ? C3 O1 C4 108.20(12) . . ? C8 O2 C9 108.51(12) . . ? C13 O3 C14 109.03(12) . . ? C1B N1 C6 143.1(2) . . ? C1B N1 C11B 114.4(3) . . ? C6 N1 C11B 66.5(2) . . ? C1B N1 C1 43.1(2) . . ? C6 N1 C1 113.63(16) . . ? C11B N1 C1 145.0(2) . . ? C1B N1 C11 69.5(2) . . ? C6 N1 C11 111.47(16) . . ? C11B N1 C11 47.5(2) . . ? C1 N1 C11 110.75(16) . . ? C1B N1 C6B 112.0(3) . . ? C6 N1 C6B 43.5(2) . . ? C11B N1 C6B 107.7(3) . . ? C1 N1 C6B 72.1(2) . . ? C11 N1 C6B 141.8(2) . . ? C1B N1 Fe1 107.6(2) . . ? C6 N1 Fe1 106.90(12) . . ? C11B N1 Fe1 107.1(2) . . ? C1 N1 Fe1 106.01(12) . . ? C11 N1 Fe1 107.67(11) . . ? C6B N1 Fe1 107.78(19) . . ? C3 N2 C2 116.00(13) . . ? C3 N2 Fe1 129.03(11) . . ? C2 N2 Fe1 114.88(10) . . ? C8 N3 C7 115.08(13) . . ? C8 N3 Fe1 128.41(11) . . ? C7 N3 Fe1 114.27(10) . . ? C13 N4 C12 114.10(13) . . ? C13 N4 Fe1 131.92(11) . . ? C12 N4 Fe1 113.88(10) . . ? C3 N5 C5 111.47(13) . . ? C8 N6 C10 110.80(14) . . ? C13 N7 C15 112.06(14) . . ? N1 C1 C2 111.94(18) . . ? N1 C1B C2 112.0(3) . . ? N2 C2 C1 110.49(15) . . ? N2 C2 C1B 109.8(2) . . ? C1 C2 C1B 40.9(2) . . ? N2 C3 N5 127.29(14) . . ? N2 C3 O1 122.19(14) . . ? N5 C3 O1 110.51(13) . . ? O1 C4 C5 104.42(12) . . ? N5 C5 C4 100.13(12) . . ? N1 C6 C7 109.99(17) . . ? C7 C6B N1 111.9(3) . . ? C6B C7 N3 107.0(2) . . ? C6B C7 C6 42.8(2) . . ? N3 C7 C6 111.93(14) . . ? N3 C8 N6 127.25(15) . . ? N3 C8 O2 122.44(14) . . ? N6 C8 O2 110.32(14) . . ? O2 C9 C10 104.49(12) . . ? N6 C10 C9 99.84(13) . . ? N1 C11 C12 109.38(17) . . ? N1 C11B C12 108.6(3) . . ? N4 C12 C11 109.56(14) . . ? N4 C12 C11B 111.6(2) . . ? C11 C12 C11B 45.6(2) . . ? N4 C13 N7 127.75(15) . . ? N4 C13 O3 121.61(14) . . ? N7 C13 O3 110.64(14) . . ? O3 C14 C15 104.77(12) . . ? N7 C15 C14 101.62(13) . . ? C22 B1 C28 107.00(11) . . ? C22 B1 C34 111.06(11) . . ? C28 B1 C34 109.41(11) . . ? C22 B1 C16 110.72(11) . . ? C28 B1 C16 110.61(11) . . ? C34 B1 C16 108.05(11) . . ? C17 C16 C21 114.85(14) . . ? C17 C16 B1 122.89(13) . . ? C21 C16 B1 122.25(13) . . ? C18 C17 C16 122.80(15) . . ? C19 C18 C17 120.44(15) . . ? C20 C19 C18 118.73(15) . . ? C19 C20 C21 120.02(15) . . ? C20 C21 C16 123.15(15) . . ? C23 C22 C27 115.17(13) . . ? C23 C22 B1 122.38(13) . . ? C27 C22 B1 121.98(12) . . ? C24 C23 C22 122.42(14) . . ? C25 C24 C23 120.81(14) . . ? C24 C25 C26 118.58(14) . . ? C25 C26 C27 119.90(14) . . ? C26 C27 C22 123.11(14) . . ? C29 C28 C33 114.86(13) . . ? C29 C28 B1 123.22(12) . . ? C33 C28 B1 121.81(13) . . ? C30 C29 C28 122.86(14) . . ? C31 C30 C29 120.23(14) . . ? C30 C31 C32 118.92(14) . . ? C33 C32 C31 120.02(14) . . ? C32 C33 C28 123.09(14) . . ? C39 C34 C35 115.12(13) . . ? C39 C34 B1 122.96(12) . . ? C35 C34 B1 121.84(12) . . ? C36 C35 C34 122.62(14) . . ? C37 C36 C35 120.42(14) . . ? C36 C37 C38 118.62(14) . . ? C37 C38 C39 120.46(14) . . ? C38 C39 C34 122.76(14) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.379 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.047 #==END data_asb123 _database_code_depnum_ccdc_archive 'CCDC 855307' #TrackingRef '- DT-ART-11-2011-012244-CIF.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H47 B Cl Co N7 O3' _chemical_formula_weight 767.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 11.4693(6) _cell_length_b 20.0855(10) _cell_length_c 15.7222(8) _cell_angle_alpha 90.00 _cell_angle_beta 96.2667(7) _cell_angle_gamma 90.00 _cell_volume 3600.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 9848 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 28.10 _exptl_crystal_description cut_cube _exptl_crystal_colour pink _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1612 _exptl_absorpt_coefficient_mu 0.601 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9153 _exptl_absorpt_correction_T_max 0.9507 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX II CCD' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 41337 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.88 _reflns_number_total 8426 _reflns_number_gt 6487 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX2' _computing_cell_refinement 'Bruker SMART APEX2/SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0488P)^2^+1.0754P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8426 _refine_ls_number_parameters 657 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0952 _refine_ls_wR_factor_gt 0.0867 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 Co1 Co 0.51107(2) 0.206959(11) 0.890737(15) 0.01792(7) Uani 1 1 d . . . Cl1 Cl 0.71864(4) 0.20244(2) 0.92754(3) 0.02085(10) Uani 1 1 d . . . N1 N 0.31889(13) 0.20862(7) 0.85771(10) 0.0214(3) Uani 1 1 d . . . N2 N 0.47853(13) 0.10532(7) 0.87661(10) 0.0219(3) Uani 1 1 d . . . N3 N 0.46240(13) 0.25442(8) 0.99760(10) 0.0228(3) Uani 1 1 d . . . N4 N 0.50284(13) 0.26575(7) 0.78301(9) 0.0206(3) Uani 1 1 d . . . N5 N 0.65513(15) 0.05436(9) 0.93319(13) 0.0345(4) Uani 1 1 d . . . N6 N 0.63634(15) 0.30728(8) 1.05522(11) 0.0266(4) Uani 1 1 d . . . N7 N 0.69682(14) 0.27456(8) 0.74630(10) 0.0236(3) Uani 1 1 d . . . O1 O 0.50891(12) -0.00836(7) 0.88040(10) 0.0347(4) Uani 1 1 d . . . O2 O 0.47279(12) 0.33015(7) 1.10978(8) 0.0278(3) Uani 1 1 d . . . O3 O 0.55932(12) 0.34012(6) 0.68381(8) 0.0259(3) Uani 1 1 d . . . C1 C 0.27404(17) 0.14029(10) 0.86374(14) 0.0264(4) Uani 1 1 d . . . C2 C 0.36042(17) 0.09072(10) 0.83299(14) 0.0259(4) Uani 1 1 d . . . C3 C 0.54583(16) 0.05429(9) 0.89547(11) 0.0213(4) Uani 1 1 d . . . C4 C 0.60251(17) -0.05456(10) 0.90986(14) 0.0260(4) Uani 1 1 d . . . C5 C 0.70502(19) -0.01067(10) 0.94479(15) 0.0287(4) Uani 1 1 d . . . C6 C 0.26880(17) 0.25376(11) 0.91821(14) 0.0287(4) Uani 1 1 d . . . C7 C 0.33624(17) 0.24747(11) 1.00633(13) 0.0295(4) Uani 1 1 d . . . C8 C 0.52238(17) 0.29449(9) 1.05051(11) 0.0218(4) Uani 1 1 d . . . C9 C 0.5629(2) 0.37115(10) 1.15781(14) 0.0303(4) Uani 1 1 d . . . C10 C 0.67262(19) 0.36220(10) 1.11248(13) 0.0278(4) Uani 1 1 d . . . C11 C 0.29834(17) 0.23367(10) 0.76890(13) 0.0245(4) Uani 1 1 d . . . C12 C 0.38285(16) 0.28917(10) 0.75561(13) 0.0247(4) Uani 1 1 d . . . C13 C 0.58429(16) 0.29161(8) 0.74191(11) 0.0200(4) Uani 1 1 d . . . C14 C 0.66576(18) 0.35849(11) 0.64646(13) 0.0275(4) Uani 1 1 d . . . C15 C 0.76337(18) 0.31842(10) 0.69541(13) 0.0260(4) Uani 1 1 d . . . H5 H 0.688(2) 0.0909(12) 0.9347(15) 0.035(6) Uiso 1 1 d . . . H6 H 0.678(2) 0.2877(13) 1.0253(18) 0.052(8) Uiso 1 1 d . . . H7 H 0.725(2) 0.2519(12) 0.7901(15) 0.033(6) Uiso 1 1 d . . . H1A H 0.2637(18) 0.1313(10) 0.9249(14) 0.025(5) Uiso 1 1 d . . . H1B H 0.1992(19) 0.1362(10) 0.8303(13) 0.025(5) Uiso 1 1 d . . . H2A H 0.3390(19) 0.0486(11) 0.8438(13) 0.030(6) Uiso 1 1 d . . . H2B H 0.3628(17) 0.0944(10) 0.7693(13) 0.022(5) Uiso 1 1 d . . . H4A H 0.6191(19) -0.0798(11) 0.8623(14) 0.032(6) Uiso 1 1 d . . . H4B H 0.5732(19) -0.0831(11) 0.9518(14) 0.030(6) Uiso 1 1 d . . . H5A H 0.771(2) -0.0164(11) 0.9158(14) 0.033(6) Uiso 1 1 d . . . H5B H 0.725(2) -0.0184(12) 1.0011(17) 0.049(7) Uiso 1 1 d . . . H6A H 0.2759(19) 0.2984(11) 0.8989(13) 0.027(6) Uiso 1 1 d . . . H6B H 0.1840(18) 0.2451(10) 0.9193(12) 0.022(5) Uiso 1 1 d . . . H7A H 0.3238(18) 0.2006(10) 1.0305(13) 0.025(5) Uiso 1 1 d . . . H7B H 0.3099(19) 0.2826(10) 1.0408(14) 0.027(5) Uiso 1 1 d . . . H9A H 0.5779(18) 0.3569(10) 1.2179(14) 0.026(5) Uiso 1 1 d . . . H9B H 0.5310(19) 0.4154(12) 1.1579(14) 0.034(6) Uiso 1 1 d . . . H10A H 0.736(2) 0.3500(11) 1.1502(15) 0.032(6) Uiso 1 1 d . . . H10B H 0.692(2) 0.4015(12) 1.0817(15) 0.038(6) Uiso 1 1 d . . . H11A H 0.3097(17) 0.1955(10) 0.7276(13) 0.021(5) Uiso 1 1 d . . . H11B H 0.2181(19) 0.2499(10) 0.7574(13) 0.025(5) Uiso 1 1 d . . . H12A H 0.3700(17) 0.3287(10) 0.7888(12) 0.019(5) Uiso 1 1 d . . . H12B H 0.3757(18) 0.3012(10) 0.6972(14) 0.022(5) Uiso 1 1 d . . . H14A H 0.6740(18) 0.4053(11) 0.6514(13) 0.025(5) Uiso 1 1 d . . . H14B H 0.6558(18) 0.3477(10) 0.5855(14) 0.028(6) Uiso 1 1 d . . . H15A H 0.804(2) 0.2920(10) 0.6571(14) 0.032(6) Uiso 1 1 d . . . H15B H 0.8172(19) 0.3452(11) 0.7292(14) 0.027(6) Uiso 1 1 d . . . B1 B 0.94229(17) -0.01793(10) 0.70968(13) 0.0190(4) Uani 1 1 d . . . C16 C 0.81567(16) -0.03194(9) 0.65375(12) 0.0217(4) Uani 1 1 d . . . C17 C 0.71242(17) -0.03166(10) 0.69368(14) 0.0276(4) Uani 1 1 d . . . C18 C 0.60266(18) -0.04449(11) 0.65092(17) 0.0357(5) Uani 1 1 d . . . C19 C 0.59094(19) -0.05680(10) 0.56373(16) 0.0381(6) Uani 1 1 d . . . C20 C 0.6893(2) -0.05403(11) 0.52107(15) 0.0378(5) Uani 1 1 d . . . C21 C 0.79937(19) -0.04174(10) 0.56500(13) 0.0286(4) Uani 1 1 d . . . C22 C 0.95021(15) -0.05695(9) 0.80220(11) 0.0189(4) Uani 1 1 d . . . C23 C 0.89045(16) -0.11736(9) 0.81108(12) 0.0214(4) Uani 1 1 d . . . C24 C 0.90246(17) -0.15484(10) 0.88595(13) 0.0254(4) Uani 1 1 d . . . C25 C 0.97599(18) -0.13372(10) 0.95579(13) 0.0288(4) Uani 1 1 d . . . C26 C 1.03782(18) -0.07516(10) 0.94938(13) 0.0303(4) Uani 1 1 d . . . C27 C 1.02518(17) -0.03807(10) 0.87417(12) 0.0247(4) Uani 1 1 d . . . C28 C 1.05489(16) -0.04842(9) 0.66623(11) 0.0209(4) Uani 1 1 d . . . C29 C 1.05073(18) -0.10676(10) 0.61762(13) 0.0276(4) Uani 1 1 d . . . C30 C 1.1507(2) -0.13441(11) 0.58834(14) 0.0353(5) Uani 1 1 d . . . C31 C 1.2594(2) -0.10478(12) 0.60890(14) 0.0353(5) Uani 1 1 d . . . C32 C 1.26632(19) -0.04795(11) 0.65782(15) 0.0332(5) Uani 1 1 d . . . C33 C 1.16609(17) -0.02028(10) 0.68490(13) 0.0279(4) Uani 1 1 d . . . C34 C 0.95580(15) 0.06321(9) 0.71780(12) 0.0197(4) Uani 1 1 d . . . C35 C 0.93081(16) 0.10103(9) 0.78816(12) 0.0229(4) Uani 1 1 d . . . C36 C 0.94436(16) 0.17011(10) 0.79138(13) 0.0256(4) Uani 1 1 d . . . C37 C 0.98117(16) 0.20397(10) 0.72296(14) 0.0275(4) Uani 1 1 d . . . C38 C 1.00199(18) 0.16876(10) 0.65031(14) 0.0293(4) Uani 1 1 d . . . C39 C 0.98920(17) 0.10021(10) 0.64837(13) 0.0255(4) Uani 1 1 d . . . H17A H 0.7169(19) -0.0225(11) 0.7521(14) 0.030(6) Uiso 1 1 d . . . H18A H 0.540(2) -0.0434(12) 0.6820(16) 0.045(7) Uiso 1 1 d . . . H19A H 0.516(2) -0.0648(12) 0.5359(15) 0.045(7) Uiso 1 1 d . . . H20A H 0.681(2) -0.0626(13) 0.4599(18) 0.054(8) Uiso 1 1 d . . . H21A H 0.865(2) -0.0398(11) 0.5345(15) 0.039(6) Uiso 1 1 d . . . H23A H 0.8408(18) -0.1340(10) 0.7619(13) 0.025(5) Uiso 1 1 d . . . H24A H 0.8631(19) -0.1937(11) 0.8888(13) 0.025(5) Uiso 1 1 d . . . H25A H 0.9876(19) -0.1581(11) 1.0057(14) 0.028(6) Uiso 1 1 d . . . H26A H 1.087(2) -0.0595(11) 0.9970(15) 0.039(6) Uiso 1 1 d . . . H27A H 1.0683(18) 0.0000(10) 0.8715(12) 0.021(5) Uiso 1 1 d . . . H29A H 0.9810(19) -0.1297(11) 0.6025(13) 0.028(6) Uiso 1 1 d . . . H30A H 1.141(2) -0.1747(12) 0.5561(15) 0.041(7) Uiso 1 1 d . . . H31A H 1.329(2) -0.1252(12) 0.5906(15) 0.045(7) Uiso 1 1 d . . . H32A H 1.338(2) -0.0277(12) 0.6741(15) 0.046(7) Uiso 1 1 d . . . H33A H 1.1734(19) 0.0205(11) 0.7174(14) 0.034(6) Uiso 1 1 d . . . H35A H 0.9076(17) 0.0804(10) 0.8371(13) 0.021(5) Uiso 1 1 d . . . H36A H 0.9305(19) 0.1928(11) 0.8395(14) 0.030(6) Uiso 1 1 d . . . H37A H 0.9918(18) 0.2514(11) 0.7242(13) 0.031(6) Uiso 1 1 d . . . H38A H 1.0280(19) 0.1904(11) 0.6020(14) 0.030(6) Uiso 1 1 d . . . H39A H 1.0052(18) 0.0790(11) 0.6023(13) 0.027(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01668(13) 0.01708(13) 0.01962(13) 0.00046(9) 0.00032(9) -0.00017(9) Cl1 0.0176(2) 0.0201(2) 0.0244(2) 0.00206(16) 0.00055(16) -0.00070(16) N1 0.0187(7) 0.0204(8) 0.0248(8) 0.0006(6) 0.0008(6) 0.0015(6) N2 0.0181(7) 0.0196(8) 0.0274(8) 0.0009(6) -0.0005(6) -0.0002(6) N3 0.0191(8) 0.0262(8) 0.0230(8) -0.0011(6) 0.0024(6) -0.0007(6) N4 0.0181(7) 0.0205(8) 0.0223(8) 0.0016(6) -0.0017(6) 0.0016(6) N5 0.0219(9) 0.0176(9) 0.0614(13) -0.0018(8) -0.0076(8) 0.0003(7) N6 0.0258(9) 0.0277(9) 0.0266(9) -0.0078(7) 0.0042(7) -0.0043(7) N7 0.0223(8) 0.0249(8) 0.0239(8) 0.0067(7) 0.0035(7) 0.0030(7) O1 0.0287(8) 0.0168(7) 0.0548(10) -0.0013(6) -0.0118(7) -0.0001(6) O2 0.0286(7) 0.0295(8) 0.0254(7) -0.0055(6) 0.0039(6) 0.0008(6) O3 0.0257(7) 0.0258(7) 0.0262(7) 0.0097(5) 0.0026(6) 0.0025(6) C1 0.0179(9) 0.0251(10) 0.0355(11) 0.0045(8) -0.0006(8) -0.0018(8) C2 0.0211(9) 0.0208(10) 0.0344(11) -0.0002(8) -0.0028(8) -0.0039(8) C3 0.0230(9) 0.0191(9) 0.0221(9) -0.0017(7) 0.0032(7) -0.0028(7) C4 0.0257(10) 0.0191(9) 0.0330(11) 0.0003(8) 0.0025(8) 0.0022(8) C5 0.0284(11) 0.0210(10) 0.0353(12) -0.0027(8) -0.0028(9) 0.0025(8) C6 0.0180(10) 0.0308(11) 0.0374(12) -0.0043(9) 0.0033(8) 0.0027(8) C7 0.0213(10) 0.0366(12) 0.0316(11) -0.0040(9) 0.0080(8) -0.0013(8) C8 0.0254(9) 0.0204(9) 0.0198(9) 0.0043(7) 0.0038(7) 0.0040(7) C9 0.0390(12) 0.0235(10) 0.0289(11) -0.0041(8) 0.0063(9) -0.0056(9) C10 0.0307(11) 0.0262(10) 0.0254(10) -0.0023(8) -0.0015(9) -0.0050(9) C11 0.0203(9) 0.0234(10) 0.0284(10) 0.0026(8) -0.0040(8) 0.0009(8) C12 0.0196(9) 0.0241(10) 0.0294(11) 0.0049(8) -0.0021(8) 0.0029(7) C13 0.0245(9) 0.0164(8) 0.0181(8) -0.0009(7) -0.0021(7) 0.0016(7) C14 0.0297(11) 0.0274(11) 0.0265(11) 0.0064(8) 0.0072(8) 0.0025(8) C15 0.0250(10) 0.0264(10) 0.0274(10) 0.0031(8) 0.0068(8) 0.0001(8) B1 0.0149(9) 0.0210(10) 0.0210(10) 0.0007(8) 0.0016(8) -0.0001(8) C16 0.0198(9) 0.0168(8) 0.0275(10) 0.0044(7) -0.0019(7) -0.0008(7) C17 0.0198(9) 0.0290(10) 0.0330(11) 0.0065(8) -0.0013(8) 0.0024(8) C18 0.0172(10) 0.0296(11) 0.0592(15) 0.0133(10) -0.0001(10) 0.0008(8) C19 0.0270(11) 0.0258(11) 0.0561(15) 0.0119(10) -0.0198(11) -0.0050(9) C20 0.0423(13) 0.0316(12) 0.0347(12) 0.0033(9) -0.0169(10) -0.0024(10) C21 0.0287(11) 0.0263(10) 0.0295(11) 0.0032(8) -0.0031(9) -0.0008(8) C22 0.0141(8) 0.0209(9) 0.0218(9) -0.0001(7) 0.0029(7) 0.0025(7) C23 0.0189(9) 0.0208(9) 0.0240(9) -0.0008(7) 0.0009(7) 0.0008(7) C24 0.0245(10) 0.0202(9) 0.0320(11) 0.0015(8) 0.0055(8) -0.0012(8) C25 0.0339(11) 0.0291(10) 0.0228(10) 0.0058(8) 0.0008(8) 0.0021(9) C26 0.0319(11) 0.0324(11) 0.0241(10) -0.0018(8) -0.0079(9) -0.0015(9) C27 0.0228(10) 0.0225(10) 0.0280(10) 0.0002(8) -0.0015(8) -0.0041(8) C28 0.0203(9) 0.0223(9) 0.0199(9) 0.0037(7) 0.0021(7) 0.0026(7) C29 0.0263(10) 0.0282(10) 0.0273(10) -0.0014(8) -0.0011(8) 0.0038(8) C30 0.0441(13) 0.0329(12) 0.0285(11) -0.0041(9) 0.0016(9) 0.0154(10) C31 0.0311(11) 0.0456(13) 0.0312(11) 0.0070(10) 0.0127(9) 0.0159(10) C32 0.0214(10) 0.0353(12) 0.0438(13) 0.0075(10) 0.0075(9) 0.0017(9) C33 0.0214(10) 0.0284(10) 0.0345(11) -0.0009(9) 0.0054(8) 0.0022(8) C34 0.0121(8) 0.0213(9) 0.0253(9) 0.0010(7) -0.0003(7) 0.0002(7) C35 0.0182(9) 0.0245(10) 0.0261(10) 0.0021(8) 0.0036(7) 0.0014(7) C36 0.0188(9) 0.0254(10) 0.0320(11) -0.0041(8) 0.0005(8) 0.0034(8) C37 0.0187(9) 0.0187(9) 0.0440(12) 0.0027(8) -0.0017(8) 0.0000(7) C38 0.0271(10) 0.0261(10) 0.0347(11) 0.0096(9) 0.0040(9) -0.0042(8) C39 0.0260(10) 0.0259(10) 0.0251(10) 0.0015(8) 0.0047(8) -0.0004(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 Co1 N4 2.0584(15) . ? Co1 N3 2.0610(15) . ? Co1 N2 2.0829(15) . ? Co1 N1 2.2089(15) . ? Co1 Cl1 2.3895(5) . ? N1 C1 1.472(2) . ? N1 C6 1.475(2) . ? N1 C11 1.479(2) . ? N2 C3 1.298(2) . ? N2 C2 1.479(2) . ? N3 C8 1.299(2) . ? N3 C7 1.475(2) . ? N4 C13 1.301(2) . ? N4 C12 1.474(2) . ? N5 C3 1.327(3) . ? N5 C5 1.430(3) . ? N5 H5 0.82(2) . ? N6 C8 1.326(3) . ? N6 C10 1.456(2) . ? N6 H6 0.81(3) . ? N7 C13 1.330(2) . ? N7 C15 1.460(2) . ? N7 H7 0.86(2) . ? O1 C3 1.340(2) . ? O1 C4 1.456(2) . ? O2 C8 1.349(2) . ? O2 C9 1.465(2) . ? O3 C13 1.345(2) . ? O3 C14 1.459(2) . ? C1 C2 1.520(3) . ? C1 H1A 1.00(2) . ? C1 H1B 0.96(2) . ? C2 H2A 0.90(2) . ? C2 H2B 1.01(2) . ? C4 C5 1.523(3) . ? C4 H4A 0.94(2) . ? C4 H4B 0.96(2) . ? C5 H5A 0.94(2) . ? C5 H5B 0.90(3) . ? C6 C7 1.516(3) . ? C6 H6A 0.95(2) . ? C6 H6B 0.99(2) . ? C7 H7A 1.03(2) . ? C7 H7B 0.96(2) . ? C9 C10 1.523(3) . ? C9 H9A 0.98(2) . ? C9 H9B 0.96(2) . ? C10 H10A 0.92(2) . ? C10 H10B 0.97(2) . ? C11 C12 1.507(3) . ? C11 H11A 1.02(2) . ? C11 H11B 0.97(2) . ? C12 H12A 0.97(2) . ? C12 H12B 0.94(2) . ? C14 C15 1.518(3) . ? C14 H14A 0.95(2) . ? C14 H14B 0.98(2) . ? C15 H15A 0.96(2) . ? C15 H15B 0.94(2) . ? B1 C16 1.638(3) . ? B1 C34 1.641(3) . ? B1 C28 1.644(3) . ? B1 C22 1.646(3) . ? C16 C17 1.400(3) . ? C16 C21 1.401(3) . ? C17 C18 1.385(3) . ? C17 H17A 0.93(2) . ? C18 C19 1.385(4) . ? C18 H18A 0.91(2) . ? C19 C20 1.375(4) . ? C19 H19A 0.93(3) . ? C20 C21 1.393(3) . ? C20 H20A 0.97(3) . ? C21 H21A 0.94(2) . ? C22 C27 1.397(3) . ? C22 C23 1.408(2) . ? C23 C24 1.391(3) . ? C23 H23A 0.97(2) . ? C24 C25 1.377(3) . ? C24 H24A 0.90(2) . ? C25 C26 1.383(3) . ? C25 H25A 0.92(2) . ? C26 C27 1.392(3) . ? C26 H26A 0.94(2) . ? C27 H27A 0.91(2) . ? C28 C33 1.397(3) . ? C28 C29 1.397(3) . ? C29 C30 1.397(3) . ? C29 H29A 0.93(2) . ? C30 C31 1.388(3) . ? C30 H30A 0.96(2) . ? C31 C32 1.374(3) . ? C31 H31A 0.97(3) . ? C32 C33 1.385(3) . ? C32 H32A 0.93(3) . ? C33 H33A 0.96(2) . ? C34 C35 1.397(3) . ? C34 C39 1.408(3) . ? C35 C36 1.397(3) . ? C35 H35A 0.94(2) . ? C36 C37 1.377(3) . ? C36 H36A 0.91(2) . ? C37 C38 1.386(3) . ? C37 H37A 0.96(2) . ? C38 C39 1.385(3) . ? C38 H38A 0.95(2) . ? C39 H39A 0.88(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Co1 N3 114.41(6) . . ? N4 Co1 N2 118.88(6) . . ? N3 Co1 N2 118.62(6) . . ? N4 Co1 N1 80.97(6) . . ? N3 Co1 N1 80.36(6) . . ? N2 Co1 N1 80.05(6) . . ? N4 Co1 Cl1 100.14(4) . . ? N3 Co1 Cl1 99.87(4) . . ? N2 Co1 Cl1 98.67(4) . . ? N1 Co1 Cl1 178.62(4) . . ? C1 N1 C6 111.59(16) . . ? C1 N1 C11 110.93(15) . . ? C6 N1 C11 111.50(15) . . ? C1 N1 Co1 108.51(11) . . ? C6 N1 Co1 107.85(11) . . ? C11 N1 Co1 106.21(11) . . ? C3 N2 C2 116.18(15) . . ? C3 N2 Co1 130.89(13) . . ? C2 N2 Co1 112.83(11) . . ? C8 N3 C7 117.08(16) . . ? C8 N3 Co1 129.56(13) . . ? C7 N3 Co1 112.82(12) . . ? C13 N4 C12 115.20(15) . . ? C13 N4 Co1 131.84(12) . . ? C12 N4 Co1 112.40(12) . . ? C3 N5 C5 113.68(17) . . ? C3 N5 H5 114.8(16) . . ? C5 N5 H5 129.5(17) . . ? C8 N6 C10 113.26(17) . . ? C8 N6 H6 121(2) . . ? C10 N6 H6 126(2) . . ? C13 N7 C15 112.25(16) . . ? C13 N7 H7 117.2(15) . . ? C15 N7 H7 125.8(15) . . ? C3 O1 C4 109.54(14) . . ? C8 O2 C9 109.12(15) . . ? C13 O3 C14 109.34(14) . . ? N1 C1 C2 110.21(16) . . ? N1 C1 H1A 108.0(12) . . ? C2 C1 H1A 109.8(12) . . ? N1 C1 H1B 110.0(12) . . ? C2 C1 H1B 110.2(12) . . ? H1A C1 H1B 108.6(17) . . ? N2 C2 C1 108.56(16) . . ? N2 C2 H2A 110.6(14) . . ? C1 C2 H2A 110.8(14) . . ? N2 C2 H2B 108.9(12) . . ? C1 C2 H2B 111.0(11) . . ? H2A C2 H2B 107.0(17) . . ? N2 C3 N5 127.64(17) . . ? N2 C3 O1 122.17(17) . . ? N5 C3 O1 110.16(16) . . ? O1 C4 C5 105.02(15) . . ? O1 C4 H4A 107.3(13) . . ? C5 C4 H4A 112.6(14) . . ? O1 C4 H4B 107.3(13) . . ? C5 C4 H4B 114.3(13) . . ? H4A C4 H4B 109.8(19) . . ? N5 C5 C4 101.55(16) . . ? N5 C5 H5A 112.7(14) . . ? C4 C5 H5A 112.9(14) . . ? N5 C5 H5B 109.7(16) . . ? C4 C5 H5B 110.8(16) . . ? H5A C5 H5B 109(2) . . ? N1 C6 C7 110.01(16) . . ? N1 C6 H6A 108.6(13) . . ? C7 C6 H6A 108.5(13) . . ? N1 C6 H6B 110.9(11) . . ? C7 C6 H6B 111.9(11) . . ? H6A C6 H6B 106.8(17) . . ? N3 C7 C6 108.35(16) . . ? N3 C7 H7A 107.3(11) . . ? C6 C7 H7A 109.6(12) . . ? N3 C7 H7B 110.9(13) . . ? C6 C7 H7B 107.1(13) . . ? H7A C7 H7B 113.5(17) . . ? N3 C8 N6 127.26(17) . . ? N3 C8 O2 122.51(17) . . ? N6 C8 O2 110.22(16) . . ? O2 C9 C10 105.37(16) . . ? O2 C9 H9A 111.8(12) . . ? C10 C9 H9A 110.4(12) . . ? O2 C9 H9B 105.8(13) . . ? C10 C9 H9B 116.3(13) . . ? H9A C9 H9B 107.1(18) . . ? N6 C10 C9 100.59(16) . . ? N6 C10 H10A 110.5(14) . . ? C9 C10 H10A 111.5(14) . . ? N6 C10 H10B 112.2(14) . . ? C9 C10 H10B 112.8(14) . . ? H10A C10 H10B 109.2(19) . . ? N1 C11 C12 110.13(15) . . ? N1 C11 H11A 109.0(11) . . ? C12 C11 H11A 109.8(11) . . ? N1 C11 H11B 109.8(12) . . ? C12 C11 H11B 109.6(12) . . ? H11A C11 H11B 108.5(16) . . ? N4 C12 C11 108.52(15) . . ? N4 C12 H12A 107.2(12) . . ? C11 C12 H12A 113.2(11) . . ? N4 C12 H12B 110.2(13) . . ? C11 C12 H12B 109.6(12) . . ? H12A C12 H12B 108.2(16) . . ? N4 C13 N7 128.09(17) . . ? N4 C13 O3 121.04(16) . . ? N7 C13 O3 110.81(16) . . ? O3 C14 C15 105.37(15) . . ? O3 C14 H14A 107.3(13) . . ? C15 C14 H14A 115.0(13) . . ? O3 C14 H14B 109.0(13) . . ? C15 C14 H14B 112.4(12) . . ? H14A C14 H14B 107.5(17) . . ? N7 C15 C14 101.36(16) . . ? N7 C15 H15A 109.0(13) . . ? C14 C15 H15A 110.7(13) . . ? N7 C15 H15B 112.8(13) . . ? C14 C15 H15B 112.7(13) . . ? H15A C15 H15B 110.0(19) . . ? C16 B1 C34 106.44(14) . . ? C16 B1 C28 113.80(15) . . ? C34 B1 C28 109.30(14) . . ? C16 B1 C22 110.66(14) . . ? C34 B1 C22 114.11(15) . . ? C28 B1 C22 102.70(14) . . ? C17 C16 C21 114.82(18) . . ? C17 C16 B1 120.17(17) . . ? C21 C16 B1 124.95(17) . . ? C18 C17 C16 123.4(2) . . ? C18 C17 H17A 117.7(14) . . ? C16 C17 H17A 118.9(14) . . ? C19 C18 C17 119.9(2) . . ? C19 C18 H18A 122.6(16) . . ? C17 C18 H18A 117.5(16) . . ? C20 C19 C18 118.6(2) . . ? C20 C19 H19A 122.6(15) . . ? C18 C19 H19A 118.7(15) . . ? C19 C20 C21 120.8(2) . . ? C19 C20 H20A 118.7(16) . . ? C21 C20 H20A 120.4(16) . . ? C20 C21 C16 122.3(2) . . ? C20 C21 H21A 119.3(15) . . ? C16 C21 H21A 118.4(15) . . ? C27 C22 C23 114.64(17) . . ? C27 C22 B1 123.80(16) . . ? C23 C22 B1 121.16(16) . . ? C24 C23 C22 123.08(17) . . ? C24 C23 H23A 119.0(12) . . ? C22 C23 H23A 117.9(12) . . ? C25 C24 C23 120.24(18) . . ? C25 C24 H24A 119.4(13) . . ? C23 C24 H24A 120.3(13) . . ? C24 C25 C26 118.58(19) . . ? C24 C25 H25A 122.3(14) . . ? C26 C25 H25A 119.1(14) . . ? C25 C26 C27 120.70(19) . . ? C25 C26 H26A 119.6(14) . . ? C27 C26 H26A 119.6(14) . . ? C26 C27 C22 122.74(18) . . ? C26 C27 H27A 118.7(13) . . ? C22 C27 H27A 118.6(13) . . ? C33 C28 C29 115.48(17) . . ? C33 C28 B1 120.18(17) . . ? C29 C28 B1 123.95(17) . . ? C30 C29 C28 122.3(2) . . ? C30 C29 H29A 115.6(13) . . ? C28 C29 H29A 122.1(13) . . ? C31 C30 C29 120.1(2) . . ? C31 C30 H30A 122.6(14) . . ? C29 C30 H30A 117.2(14) . . ? C32 C31 C30 118.8(2) . . ? C32 C31 H31A 121.4(15) . . ? C30 C31 H31A 119.7(15) . . ? C31 C32 C33 120.4(2) . . ? C31 C32 H32A 120.9(15) . . ? C33 C32 H32A 118.6(15) . . ? C32 C33 C28 122.9(2) . . ? C32 C33 H33A 118.5(13) . . ? C28 C33 H33A 118.7(13) . . ? C35 C34 C39 115.07(17) . . ? C35 C34 B1 125.16(16) . . ? C39 C34 B1 119.69(16) . . ? C36 C35 C34 122.50(18) . . ? C36 C35 H35A 116.7(12) . . ? C34 C35 H35A 120.7(13) . . ? C37 C36 C35 120.31(19) . . ? C37 C36 H36A 119.9(14) . . ? C35 C36 H36A 119.8(14) . . ? C36 C37 C38 119.12(18) . . ? C36 C37 H37A 121.5(13) . . ? C38 C37 H37A 119.3(13) . . ? C39 C38 C37 119.88(19) . . ? C39 C38 H38A 118.6(13) . . ? C37 C38 H38A 121.4(13) . . ? C38 C39 C34 123.02(19) . . ? C38 C39 H39A 118.1(15) . . ? C34 C39 H39A 118.9(15) . . ? 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 Co1 N1 C1 134.18(13) . . . . ? N3 Co1 N1 C1 -108.99(13) . . . . ? N2 Co1 N1 C1 12.55(12) . . . . ? Cl1 Co1 N1 C1 -9.1(19) . . . . ? N4 Co1 N1 C6 -104.79(13) . . . . ? N3 Co1 N1 C6 12.05(12) . . . . ? N2 Co1 N1 C6 133.58(13) . . . . ? Cl1 Co1 N1 C6 112.0(18) . . . . ? N4 Co1 N1 C11 14.86(11) . . . . ? N3 Co1 N1 C11 131.69(12) . . . . ? N2 Co1 N1 C11 -106.77(12) . . . . ? Cl1 Co1 N1 C11 -128.4(18) . . . . ? N4 Co1 N2 C3 116.71(17) . . . . ? N3 Co1 N2 C3 -96.30(17) . . . . ? N1 Co1 N2 C3 -169.48(18) . . . . ? Cl1 Co1 N2 C3 10.00(17) . . . . ? N4 Co1 N2 C2 -59.25(14) . . . . ? N3 Co1 N2 C2 87.73(14) . . . . ? N1 Co1 N2 C2 14.56(13) . . . . ? Cl1 Co1 N2 C2 -165.96(12) . . . . ? N4 Co1 N3 C8 -80.31(17) . . . . ? N2 Co1 N3 C8 131.28(16) . . . . ? N1 Co1 N3 C8 -155.72(17) . . . . ? Cl1 Co1 N3 C8 25.66(17) . . . . ? N4 Co1 N3 C7 90.91(14) . . . . ? N2 Co1 N3 C7 -57.50(15) . . . . ? N1 Co1 N3 C7 15.50(13) . . . . ? Cl1 Co1 N3 C7 -163.12(12) . . . . ? N3 Co1 N4 C13 108.72(17) . . . . ? N2 Co1 N4 C13 -102.96(17) . . . . ? N1 Co1 N4 C13 -176.25(17) . . . . ? Cl1 Co1 N4 C13 2.91(17) . . . . ? N3 Co1 N4 C12 -62.08(14) . . . . ? N2 Co1 N4 C12 86.24(13) . . . . ? N1 Co1 N4 C12 12.95(12) . . . . ? Cl1 Co1 N4 C12 -167.89(12) . . . . ? C6 N1 C1 C2 -155.44(16) . . . . ? C11 N1 C1 C2 79.57(19) . . . . ? Co1 N1 C1 C2 -36.75(18) . . . . ? C3 N2 C2 C1 144.91(17) . . . . ? Co1 N2 C2 C1 -38.49(19) . . . . ? N1 C1 C2 N2 49.9(2) . . . . ? C2 N2 C3 N5 179.0(2) . . . . ? Co1 N2 C3 N5 3.1(3) . . . . ? C2 N2 C3 O1 -3.3(3) . . . . ? Co1 N2 C3 O1 -179.14(13) . . . . ? C5 N5 C3 N2 -180.0(2) . . . . ? C5 N5 C3 O1 2.1(3) . . . . ? C4 O1 C3 N2 -178.78(17) . . . . ? C4 O1 C3 N5 -0.7(2) . . . . ? C3 O1 C4 C5 -0.8(2) . . . . ? C3 N5 C5 C4 -2.4(3) . . . . ? O1 C4 C5 N5 1.8(2) . . . . ? C1 N1 C6 C7 82.4(2) . . . . ? C11 N1 C6 C7 -152.92(17) . . . . ? Co1 N1 C6 C7 -36.69(19) . . . . ? C8 N3 C7 C6 132.57(18) . . . . ? Co1 N3 C7 C6 -39.8(2) . . . . ? N1 C6 C7 N3 50.7(2) . . . . ? C7 N3 C8 N6 178.68(18) . . . . ? Co1 N3 C8 N6 -10.4(3) . . . . ? C7 N3 C8 O2 -1.8(3) . . . . ? Co1 N3 C8 O2 169.06(12) . . . . ? C10 N6 C8 N3 170.91(18) . . . . ? C10 N6 C8 O2 -8.6(2) . . . . ? C9 O2 C8 N3 -178.87(17) . . . . ? C9 O2 C8 N6 0.7(2) . . . . ? C8 O2 C9 C10 6.8(2) . . . . ? C8 N6 C10 C9 12.0(2) . . . . ? O2 C9 C10 N6 -10.7(2) . . . . ? C1 N1 C11 C12 -157.51(16) . . . . ? C6 N1 C11 C12 77.4(2) . . . . ? Co1 N1 C11 C12 -39.79(17) . . . . ? C13 N4 C12 C11 149.19(17) . . . . ? Co1 N4 C12 C11 -38.38(19) . . . . ? N1 C11 C12 N4 52.5(2) . . . . ? C12 N4 C13 N7 -171.84(18) . . . . ? Co1 N4 C13 N7 17.6(3) . . . . ? C12 N4 C13 O3 5.2(2) . . . . ? Co1 N4 C13 O3 -165.43(12) . . . . ? C15 N7 C13 N4 -175.64(18) . . . . ? C15 N7 C13 O3 7.1(2) . . . . ? C14 O3 C13 N4 -178.64(17) . . . . ? C14 O3 C13 N7 -1.2(2) . . . . ? C13 O3 C14 C15 -4.8(2) . . . . ? C13 N7 C15 C14 -9.4(2) . . . . ? O3 C14 C15 N7 8.1(2) . . . . ? C34 B1 C16 C17 -82.8(2) . . . . ? C28 B1 C16 C17 156.73(16) . . . . ? C22 B1 C16 C17 41.7(2) . . . . ? C34 B1 C16 C21 94.1(2) . . . . ? C28 B1 C16 C21 -26.4(3) . . . . ? C22 B1 C16 C21 -141.40(18) . . . . ? C21 C16 C17 C18 4.2(3) . . . . ? B1 C16 C17 C18 -178.56(18) . . . . ? C16 C17 C18 C19 -1.7(3) . . . . ? C17 C18 C19 C20 -1.8(3) . . . . ? C18 C19 C20 C21 2.5(3) . . . . ? C19 C20 C21 C16 0.3(3) . . . . ? C17 C16 C21 C20 -3.5(3) . . . . ? B1 C16 C21 C20 179.44(18) . . . . ? C16 B1 C22 C27 -157.17(17) . . . . ? C34 B1 C22 C27 -37.2(2) . . . . ? C28 B1 C22 C27 81.0(2) . . . . ? C16 B1 C22 C23 30.5(2) . . . . ? C34 B1 C22 C23 150.50(16) . . . . ? C28 B1 C22 C23 -91.33(18) . . . . ? C27 C22 C23 C24 1.4(3) . . . . ? B1 C22 C23 C24 174.42(17) . . . . ? C22 C23 C24 C25 -0.4(3) . . . . ? C23 C24 C25 C26 -0.6(3) . . . . ? C24 C25 C26 C27 0.6(3) . . . . ? C25 C26 C27 C22 0.5(3) . . . . ? C23 C22 C27 C26 -1.4(3) . . . . ? B1 C22 C27 C26 -174.23(18) . . . . ? C16 B1 C28 C33 154.74(17) . . . . ? C34 B1 C28 C33 35.9(2) . . . . ? C22 B1 C28 C33 -85.61(19) . . . . ? C16 B1 C28 C29 -32.7(2) . . . . ? C34 B1 C28 C29 -151.56(17) . . . . ? C22 B1 C28 C29 86.9(2) . . . . ? C33 C28 C29 C30 -1.1(3) . . . . ? B1 C28 C29 C30 -173.97(18) . . . . ? C28 C29 C30 C31 1.5(3) . . . . ? C29 C30 C31 C32 -0.4(3) . . . . ? C30 C31 C32 C33 -1.0(3) . . . . ? C31 C32 C33 C28 1.4(3) . . . . ? C29 C28 C33 C32 -0.3(3) . . . . ? B1 C28 C33 C32 172.85(19) . . . . ? C16 B1 C34 C35 98.0(2) . . . . ? C28 B1 C34 C35 -138.69(17) . . . . ? C22 B1 C34 C35 -24.4(2) . . . . ? C16 B1 C34 C39 -78.5(2) . . . . ? C28 B1 C34 C39 44.8(2) . . . . ? C22 B1 C34 C39 159.11(16) . . . . ? C39 C34 C35 C36 -3.5(3) . . . . ? B1 C34 C35 C36 179.85(17) . . . . ? C34 C35 C36 C37 1.4(3) . . . . ? C35 C36 C37 C38 1.4(3) . . . . ? C36 C37 C38 C39 -2.0(3) . . . . ? C37 C38 C39 C34 -0.2(3) . . . . ? C35 C34 C39 C38 2.9(3) . . . . ? B1 C34 C39 C38 179.76(18) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.424 _refine_diff_density_min -0.306 _refine_diff_density_rms 0.058 #==END data_asb137 _database_code_depnum_ccdc_archive 'CCDC 855308' #TrackingRef '- DT-ART-11-2011-012244-CIF.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H47 B Cl N7 Ni O3' _chemical_formula_weight 766.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2415(4) _cell_length_b 12.4842(5) _cell_length_c 14.1654(5) _cell_angle_alpha 89.1512(5) _cell_angle_beta 75.4318(5) _cell_angle_gamma 71.8214(5) _cell_volume 1823.65(12) _cell_formula_units_Z 2 _cell_measurement_temperature 98(2) _cell_measurement_reflns_used 9935 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 28.27 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.654 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8694 _exptl_absorpt_correction_T_max 0.9680 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 98(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22128 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 28.29 _reflns_number_total 8694 _reflns_number_gt 7304 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0346P)^2^+0.8088P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8694 _refine_ls_number_parameters 481 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0785 _refine_ls_wR_factor_gt 0.0743 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 Ni1 Ni 1.001372(19) 0.304927(16) 0.700969(14) 0.01307(6) Uani 1 1 d . . . Cl1 Cl 1.12967(4) 0.21579(3) 0.54448(3) 0.01641(8) Uani 1 1 d . . . O1 O 1.29297(11) 0.12235(9) 0.83972(8) 0.0175(2) Uani 1 1 d . . . O2 O 0.77057(11) 0.08300(9) 0.72335(8) 0.0190(2) Uani 1 1 d . . . O3 O 1.05865(11) 0.61970(9) 0.60227(8) 0.0174(2) Uani 1 1 d . . . N1 N 0.87450(12) 0.38677(11) 0.83162(9) 0.0151(3) Uani 1 1 d . . . N2 N 1.11358(13) 0.22479(11) 0.78864(9) 0.0158(3) Uani 1 1 d . . . N3 N 0.85781(12) 0.22897(11) 0.71497(10) 0.0166(3) Uani 1 1 d . . . N4 N 1.01510(12) 0.46577(11) 0.67664(9) 0.0152(3) Uani 1 1 d . . . N5 N 1.31399(13) 0.12218(12) 0.68029(11) 0.0188(3) Uani 1 1 d . . . N6 N 0.96965(14) 0.05054(11) 0.62914(10) 0.0183(3) Uani 1 1 d . . . N7 N 1.18338(13) 0.45067(12) 0.53321(10) 0.0192(3) Uani 1 1 d . . . H5 H 1.2874(19) 0.1330(16) 0.6282(15) 0.023(5) Uiso 1 1 d . . . H6 H 1.039(2) 0.0644(17) 0.6109(15) 0.027(5) Uiso 1 1 d . . . H7 H 1.194(2) 0.3840(19) 0.5200(16) 0.032(6) Uiso 1 1 d . . . C1 C 0.90609(16) 0.31011(14) 0.90926(12) 0.0204(3) Uani 1 1 d . . . H1A H 0.8690 0.2480 0.9085 0.024 Uiso 1 1 calc R . . H1B H 0.8670 0.3525 0.9740 0.024 Uiso 1 1 calc R . . C2 C 1.05229(16) 0.26107(15) 0.89332(12) 0.0205(3) Uani 1 1 d . . . H2A H 1.0863 0.3188 0.9135 0.025 Uiso 1 1 calc R . . H2B H 1.0730 0.1956 0.9335 0.025 Uiso 1 1 calc R . . C3 C 1.23242(15) 0.16010(13) 0.76881(11) 0.0156(3) Uani 1 1 d . . . C4 C 1.42940(16) 0.06153(14) 0.79360(13) 0.0202(3) Uani 1 1 d . . . H4A H 1.4599 -0.0090 0.8259 0.024 Uiso 1 1 calc R . . H4B H 1.4845 0.1090 0.7966 0.024 Uiso 1 1 calc R . . C5 C 1.43232(16) 0.03556(14) 0.68805(13) 0.0201(3) Uani 1 1 d . . . H5A H 1.5100 0.0445 0.6414 0.024 Uiso 1 1 calc R . . H5B H 1.4286 -0.0415 0.6778 0.024 Uiso 1 1 calc R . . C6 C 0.74210(15) 0.40236(13) 0.82179(12) 0.0180(3) Uani 1 1 d . . . H6A H 0.7205 0.4611 0.7755 0.022 Uiso 1 1 calc R . . H6B H 0.6786 0.4283 0.8860 0.022 Uiso 1 1 calc R . . C7 C 0.73318(16) 0.29159(14) 0.78465(12) 0.0203(3) Uani 1 1 d . . . H7A H 0.7141 0.2453 0.8403 0.024 Uiso 1 1 calc R . . H7B H 0.6621 0.3076 0.7518 0.024 Uiso 1 1 calc R . . C8 C 0.86804(15) 0.12674(14) 0.68954(11) 0.0164(3) Uani 1 1 d . . . C9 C 0.81164(17) -0.03225(14) 0.67953(12) 0.0204(3) Uani 1 1 d . . . H9A H 0.7687 -0.0356 0.6271 0.024 Uiso 1 1 calc R . . H9B H 0.7905 -0.0845 0.7294 0.024 Uiso 1 1 calc R . . C10 C 0.95776(17) -0.06266(14) 0.63801(12) 0.0200(3) Uani 1 1 d . . . H10A H 1.0058 -0.1059 0.6835 0.024 Uiso 1 1 calc R . . H10B H 0.9877 -0.1059 0.5738 0.024 Uiso 1 1 calc R . . C11 C 0.89403(16) 0.49604(13) 0.84687(12) 0.0188(3) Uani 1 1 d . . . H11A H 0.9700 0.4840 0.8739 0.023 Uiso 1 1 calc R . . H11B H 0.8168 0.5464 0.8944 0.023 Uiso 1 1 calc R . . C12 C 0.91597(16) 0.55063(13) 0.75071(11) 0.0173(3) Uani 1 1 d . . . H12A H 0.8341 0.5778 0.7304 0.021 Uiso 1 1 calc R . . H12B H 0.9457 0.6161 0.7578 0.021 Uiso 1 1 calc R . . C13 C 1.08281(15) 0.50733(13) 0.60721(11) 0.0153(3) Uani 1 1 d . . . C14 C 1.15994(16) 0.63872(14) 0.52310(12) 0.0193(3) Uani 1 1 d . . . H14A H 1.2269 0.6553 0.5488 0.023 Uiso 1 1 calc R . . H14B H 1.1232 0.7022 0.4852 0.023 Uiso 1 1 calc R . . C15 C 1.21607(16) 0.52774(14) 0.46049(12) 0.0200(3) Uani 1 1 d . . . H15A H 1.1741 0.5294 0.4066 0.024 Uiso 1 1 calc R . . H15B H 1.3110 0.5082 0.4332 0.024 Uiso 1 1 calc R . . B1 B 0.68536(16) 0.27357(14) 0.21392(12) 0.0122(3) Uani 1 1 d . . . C16 C 0.64776(14) 0.26047(13) 0.33311(11) 0.0140(3) Uani 1 1 d . . . C17 C 0.70527(16) 0.16224(13) 0.37559(12) 0.0177(3) Uani 1 1 d . . . H17A H 0.7687 0.1008 0.3342 0.021 Uiso 1 1 calc R . . C18 C 0.67310(17) 0.15107(15) 0.47612(13) 0.0234(4) Uani 1 1 d . . . H18A H 0.7148 0.0829 0.5017 0.028 Uiso 1 1 calc R . . C19 C 0.58079(17) 0.23854(15) 0.53898(12) 0.0236(4) Uani 1 1 d . . . H19A H 0.5592 0.2313 0.6075 0.028 Uiso 1 1 calc R . . C20 C 0.52046(16) 0.33683(15) 0.49991(12) 0.0223(4) Uani 1 1 d . . . H20A H 0.4561 0.3975 0.5417 0.027 Uiso 1 1 calc R . . C21 C 0.55430(15) 0.34659(14) 0.39916(12) 0.0181(3) Uani 1 1 d . . . H21A H 0.5120 0.4149 0.3741 0.022 Uiso 1 1 calc R . . C22 C 0.59241(14) 0.22739(12) 0.16284(11) 0.0133(3) Uani 1 1 d . . . C23 C 0.46146(15) 0.24423(12) 0.20932(12) 0.0149(3) Uani 1 1 d . . . H23A H 0.4283 0.2752 0.2751 0.018 Uiso 1 1 calc R . . C24 C 0.37811(15) 0.21716(13) 0.16260(12) 0.0166(3) Uani 1 1 d . . . H24A H 0.2900 0.2302 0.1969 0.020 Uiso 1 1 calc R . . C25 C 0.42215(15) 0.17159(13) 0.06689(12) 0.0166(3) Uani 1 1 d . . . H25A H 0.3652 0.1535 0.0351 0.020 Uiso 1 1 calc R . . C26 C 0.55179(15) 0.15287(13) 0.01826(11) 0.0162(3) Uani 1 1 d . . . H26A H 0.5842 0.1214 -0.0474 0.019 Uiso 1 1 calc R . . C27 C 0.63392(15) 0.18029(13) 0.06587(11) 0.0153(3) Uani 1 1 d . . . H27A H 0.7220 0.1666 0.0313 0.018 Uiso 1 1 calc R . . C28 C 0.66116(14) 0.40726(12) 0.18999(11) 0.0127(3) Uani 1 1 d . . . C29 C 0.61240(14) 0.45419(13) 0.11147(11) 0.0144(3) Uani 1 1 d . . . H29A H 0.5836 0.4093 0.0744 0.017 Uiso 1 1 calc R . . C30 C 0.60436(15) 0.56371(13) 0.08552(12) 0.0171(3) Uani 1 1 d . . . H30A H 0.5713 0.5917 0.0314 0.021 Uiso 1 1 calc R . . C31 C 0.64438(16) 0.63215(13) 0.13839(12) 0.0193(3) Uani 1 1 d . . . H31A H 0.6403 0.7065 0.1203 0.023 Uiso 1 1 calc R . . C32 C 0.69051(16) 0.59015(14) 0.21822(12) 0.0204(3) Uani 1 1 d . . . H32A H 0.7168 0.6365 0.2559 0.024 Uiso 1 1 calc R . . C33 C 0.69824(15) 0.48037(13) 0.24297(12) 0.0169(3) Uani 1 1 d . . . H33A H 0.7299 0.4536 0.2980 0.020 Uiso 1 1 calc R . . C34 C 0.83980(14) 0.20228(13) 0.16895(11) 0.0129(3) Uani 1 1 d . . . C35 C 0.88401(15) 0.08424(13) 0.14856(11) 0.0164(3) Uani 1 1 d . . . H35A H 0.8219 0.0455 0.1577 0.020 Uiso 1 1 calc R . . C36 C 1.01484(16) 0.02206(13) 0.11559(12) 0.0189(3) Uani 1 1 d . . . H36A H 1.0400 -0.0575 0.1031 0.023 Uiso 1 1 calc R . . C37 C 1.10858(15) 0.07528(14) 0.10082(11) 0.0185(3) Uani 1 1 d . . . H37A H 1.1980 0.0331 0.0781 0.022 Uiso 1 1 calc R . . C38 C 1.06930(15) 0.19144(14) 0.11987(11) 0.0168(3) Uani 1 1 d . . . H38A H 1.1321 0.2295 0.1102 0.020 Uiso 1 1 calc R . . C39 C 0.93792(15) 0.25253(13) 0.15314(11) 0.0142(3) Uani 1 1 d . . . H39A H 0.9137 0.3320 0.1657 0.017 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 Ni1 0.01292(10) 0.01279(10) 0.01323(10) 0.00035(7) -0.00324(7) -0.00383(7) Cl1 0.01683(18) 0.01667(18) 0.01489(18) -0.00103(14) -0.00304(14) -0.00493(14) O1 0.0165(6) 0.0164(5) 0.0201(6) 0.0025(4) -0.0077(5) -0.0037(4) O2 0.0193(6) 0.0175(6) 0.0223(6) 0.0014(5) -0.0049(5) -0.0093(5) O3 0.0193(6) 0.0147(5) 0.0187(6) 0.0028(4) -0.0043(5) -0.0068(5) N1 0.0150(6) 0.0138(6) 0.0161(6) 0.0016(5) -0.0036(5) -0.0042(5) N2 0.0155(6) 0.0167(6) 0.0139(6) 0.0020(5) -0.0032(5) -0.0041(5) N3 0.0142(6) 0.0166(7) 0.0176(7) -0.0009(5) -0.0018(5) -0.0049(5) N4 0.0148(6) 0.0143(6) 0.0154(6) -0.0012(5) -0.0031(5) -0.0036(5) N5 0.0153(7) 0.0193(7) 0.0186(7) 0.0010(6) -0.0051(6) -0.0004(5) N6 0.0195(7) 0.0161(7) 0.0190(7) -0.0011(5) -0.0019(6) -0.0074(6) N7 0.0179(7) 0.0162(7) 0.0207(7) 0.0013(6) -0.0003(6) -0.0052(6) C1 0.0196(8) 0.0222(8) 0.0163(8) 0.0033(6) -0.0026(6) -0.0040(7) C2 0.0198(8) 0.0234(8) 0.0149(8) 0.0010(6) -0.0033(6) -0.0030(7) C3 0.0194(8) 0.0126(7) 0.0181(8) 0.0039(6) -0.0072(6) -0.0081(6) C4 0.0161(8) 0.0151(8) 0.0292(9) 0.0004(7) -0.0086(7) -0.0023(6) C5 0.0153(8) 0.0169(8) 0.0269(9) 0.0002(7) -0.0069(7) -0.0024(6) C6 0.0142(7) 0.0182(8) 0.0201(8) 0.0001(6) -0.0028(6) -0.0046(6) C7 0.0157(8) 0.0204(8) 0.0232(8) -0.0018(7) -0.0011(7) -0.0066(6) C8 0.0182(8) 0.0199(8) 0.0144(7) 0.0044(6) -0.0070(6) -0.0084(6) C9 0.0274(9) 0.0165(8) 0.0226(8) 0.0027(6) -0.0117(7) -0.0104(7) C10 0.0266(9) 0.0160(8) 0.0203(8) 0.0018(6) -0.0089(7) -0.0086(7) C11 0.0209(8) 0.0177(8) 0.0172(8) -0.0028(6) -0.0034(6) -0.0065(6) C12 0.0189(8) 0.0143(7) 0.0170(8) -0.0014(6) -0.0022(6) -0.0049(6) C13 0.0152(7) 0.0153(7) 0.0184(8) 0.0015(6) -0.0088(6) -0.0054(6) C14 0.0186(8) 0.0218(8) 0.0198(8) 0.0066(6) -0.0053(7) -0.0097(7) C15 0.0175(8) 0.0227(8) 0.0192(8) 0.0046(7) -0.0031(6) -0.0070(7) B1 0.0116(8) 0.0129(8) 0.0124(8) 0.0005(6) -0.0038(6) -0.0039(6) C16 0.0123(7) 0.0169(7) 0.0159(7) 0.0008(6) -0.0045(6) -0.0081(6) C17 0.0176(8) 0.0166(8) 0.0189(8) 0.0006(6) -0.0033(6) -0.0068(6) C18 0.0287(9) 0.0220(9) 0.0223(9) 0.0093(7) -0.0084(7) -0.0111(7) C19 0.0260(9) 0.0332(10) 0.0160(8) 0.0047(7) -0.0042(7) -0.0165(8) C20 0.0176(8) 0.0278(9) 0.0190(8) -0.0027(7) -0.0003(7) -0.0071(7) C21 0.0138(7) 0.0208(8) 0.0180(8) 0.0010(6) -0.0035(6) -0.0039(6) C22 0.0141(7) 0.0089(7) 0.0177(7) 0.0031(6) -0.0053(6) -0.0039(6) C23 0.0146(7) 0.0113(7) 0.0184(8) 0.0006(6) -0.0042(6) -0.0036(6) C24 0.0108(7) 0.0136(7) 0.0255(8) 0.0032(6) -0.0051(6) -0.0036(6) C25 0.0163(8) 0.0133(7) 0.0241(8) 0.0034(6) -0.0107(6) -0.0061(6) C26 0.0181(8) 0.0156(7) 0.0161(8) 0.0006(6) -0.0061(6) -0.0054(6) C27 0.0134(7) 0.0149(7) 0.0180(8) 0.0015(6) -0.0034(6) -0.0055(6) C28 0.0087(7) 0.0122(7) 0.0146(7) -0.0025(6) -0.0004(6) -0.0016(6) C29 0.0119(7) 0.0140(7) 0.0171(7) -0.0022(6) -0.0036(6) -0.0038(6) C30 0.0155(8) 0.0163(8) 0.0185(8) 0.0018(6) -0.0049(6) -0.0031(6) C31 0.0210(8) 0.0119(7) 0.0240(8) 0.0016(6) -0.0052(7) -0.0041(6) C32 0.0230(8) 0.0167(8) 0.0239(9) -0.0026(6) -0.0082(7) -0.0080(7) C33 0.0171(8) 0.0172(8) 0.0172(8) -0.0001(6) -0.0065(6) -0.0050(6) C34 0.0134(7) 0.0145(7) 0.0111(7) 0.0006(6) -0.0046(6) -0.0037(6) C35 0.0167(8) 0.0157(7) 0.0181(8) -0.0001(6) -0.0057(6) -0.0058(6) C36 0.0204(8) 0.0133(7) 0.0202(8) -0.0028(6) -0.0068(7) 0.0001(6) C37 0.0138(7) 0.0227(8) 0.0149(8) -0.0019(6) -0.0052(6) 0.0013(6) C38 0.0134(7) 0.0245(8) 0.0143(7) 0.0008(6) -0.0048(6) -0.0073(6) C39 0.0148(7) 0.0152(7) 0.0124(7) -0.0007(6) -0.0046(6) -0.0039(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 2.0245(13) . ? Ni1 N4 2.0786(13) . ? Ni1 N1 2.0790(13) . ? Ni1 N3 2.0812(13) . ? Ni1 Cl1 2.3866(4) . ? O1 C3 1.3505(18) . ? O1 C4 1.4627(19) . ? O2 C8 1.3526(19) . ? O2 C9 1.4616(19) . ? O3 C13 1.3474(18) . ? O3 C14 1.4592(19) . ? N1 C11 1.475(2) . ? N1 C6 1.482(2) . ? N1 C1 1.485(2) . ? N2 C3 1.289(2) . ? N2 C2 1.480(2) . ? N3 C8 1.294(2) . ? N3 C7 1.481(2) . ? N4 C13 1.292(2) . ? N4 C12 1.474(2) . ? N5 C3 1.344(2) . ? N5 C5 1.457(2) . ? N6 C8 1.340(2) . ? N6 C10 1.461(2) . ? N7 C13 1.343(2) . ? N7 C15 1.457(2) . ? C1 C2 1.522(2) . ? C4 C5 1.525(2) . ? C6 C7 1.528(2) . ? C9 C10 1.523(2) . ? C11 C12 1.513(2) . ? C14 C15 1.521(2) . ? B1 C34 1.646(2) . ? B1 C22 1.648(2) . ? B1 C28 1.650(2) . ? B1 C16 1.653(2) . ? C16 C17 1.401(2) . ? C16 C21 1.402(2) . ? C17 C18 1.394(2) . ? C18 C19 1.385(3) . ? C19 C20 1.386(3) . ? C20 C21 1.395(2) . ? C22 C23 1.403(2) . ? C22 C27 1.407(2) . ? C23 C24 1.395(2) . ? C24 C25 1.384(2) . ? C25 C26 1.393(2) . ? C26 C27 1.393(2) . ? C28 C29 1.403(2) . ? C28 C33 1.409(2) . ? C29 C30 1.392(2) . ? C30 C31 1.386(2) . ? C31 C32 1.389(2) . ? C32 C33 1.391(2) . ? C34 C39 1.401(2) . ? C34 C35 1.409(2) . ? C35 C36 1.392(2) . ? C36 C37 1.385(2) . ? C37 C38 1.387(2) . ? C38 C39 1.394(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni1 N4 111.16(5) . . ? N2 Ni1 N1 83.76(5) . . ? N4 Ni1 N1 82.09(5) . . ? N2 Ni1 N3 106.15(5) . . ? N4 Ni1 N3 136.15(5) . . ? N1 Ni1 N3 79.86(5) . . ? N2 Ni1 Cl1 101.33(4) . . ? N4 Ni1 Cl1 97.76(4) . . ? N1 Ni1 Cl1 174.54(4) . . ? N3 Ni1 Cl1 96.69(4) . . ? C3 O1 C4 108.53(12) . . ? C8 O2 C9 108.19(12) . . ? C13 O3 C14 108.19(12) . . ? C11 N1 C6 111.54(12) . . ? C11 N1 C1 111.57(12) . . ? C6 N1 C1 111.92(12) . . ? C11 N1 Ni1 109.21(9) . . ? C6 N1 Ni1 106.27(9) . . ? C1 N1 Ni1 106.01(9) . . ? C3 N2 C2 115.24(13) . . ? C3 N2 Ni1 131.45(11) . . ? C2 N2 Ni1 112.66(10) . . ? C8 N3 C7 114.55(13) . . ? C8 N3 Ni1 129.58(11) . . ? C7 N3 Ni1 114.02(10) . . ? C13 N4 C12 114.50(13) . . ? C13 N4 Ni1 133.93(11) . . ? C12 N4 Ni1 111.23(9) . . ? C3 N5 C5 111.36(14) . . ? C8 N6 C10 110.98(14) . . ? C13 N7 C15 110.30(13) . . ? N1 C1 C2 110.48(13) . . ? N2 C2 C1 109.28(13) . . ? N2 C3 N5 127.83(15) . . ? N2 C3 O1 121.88(14) . . ? N5 C3 O1 110.28(13) . . ? O1 C4 C5 104.23(12) . . ? N5 C5 C4 100.15(13) . . ? N1 C6 C7 110.46(13) . . ? N3 C7 C6 109.25(13) . . ? N3 C8 N6 127.59(15) . . ? N3 C8 O2 121.81(15) . . ? N6 C8 O2 110.60(14) . . ? O2 C9 C10 104.81(12) . . ? N6 C10 C9 99.88(13) . . ? N1 C11 C12 109.75(13) . . ? N4 C12 C11 108.33(13) . . ? N4 C13 N7 127.69(14) . . ? N4 C13 O3 121.58(14) . . ? N7 C13 O3 110.73(13) . . ? O3 C14 C15 103.72(12) . . ? N7 C15 C14 100.24(13) . . ? C34 B1 C22 111.54(12) . . ? C34 B1 C28 108.87(12) . . ? C22 B1 C28 107.20(12) . . ? C34 B1 C16 108.23(12) . . ? C22 B1 C16 110.10(12) . . ? C28 B1 C16 110.92(12) . . ? C17 C16 C21 115.00(14) . . ? C17 C16 B1 122.68(14) . . ? C21 C16 B1 122.31(14) . . ? C18 C17 C16 122.65(15) . . ? C19 C18 C17 120.54(16) . . ? C18 C19 C20 118.71(16) . . ? C19 C20 C21 119.92(16) . . ? C20 C21 C16 123.18(16) . . ? C23 C22 C27 115.13(14) . . ? C23 C22 B1 121.96(13) . . ? C27 C22 B1 122.53(13) . . ? C24 C23 C22 122.47(15) . . ? C25 C24 C23 120.81(15) . . ? C24 C25 C26 118.55(14) . . ? C25 C26 C27 120.01(15) . . ? C26 C27 C22 123.03(14) . . ? C29 C28 C33 115.05(14) . . ? C29 C28 B1 123.03(13) . . ? C33 C28 B1 121.73(13) . . ? C30 C29 C28 122.85(14) . . ? C31 C30 C29 120.25(15) . . ? C30 C31 C32 118.91(15) . . ? C31 C32 C33 120.08(15) . . ? C32 C33 C28 122.82(15) . . ? C39 C34 C35 114.78(14) . . ? C39 C34 B1 122.98(13) . . ? C35 C34 B1 122.15(13) . . ? C36 C35 C34 122.77(15) . . ? C37 C36 C35 120.50(15) . . ? C36 C37 C38 118.62(15) . . ? C37 C38 C39 120.22(15) . . ? C38 C39 C34 123.11(15) . . ? 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 Ni1 N1 C11 96.12(10) . . . . ? N4 Ni1 N1 C11 -16.32(10) . . . . ? N3 Ni1 N1 C11 -156.19(11) . . . . ? Cl1 Ni1 N1 C11 -105.1(4) . . . . ? N2 Ni1 N1 C6 -143.43(10) . . . . ? N4 Ni1 N1 C6 104.12(10) . . . . ? N3 Ni1 N1 C6 -35.75(9) . . . . ? Cl1 Ni1 N1 C6 15.4(5) . . . . ? N2 Ni1 N1 C1 -24.21(10) . . . . ? N4 Ni1 N1 C1 -136.66(10) . . . . ? N3 Ni1 N1 C1 83.48(10) . . . . ? Cl1 Ni1 N1 C1 134.6(4) . . . . ? N4 Ni1 N2 C3 -90.35(15) . . . . ? N1 Ni1 N2 C3 -169.35(15) . . . . ? N3 Ni1 N2 C3 113.13(14) . . . . ? Cl1 Ni1 N2 C3 12.66(15) . . . . ? N4 Ni1 N2 C2 79.79(11) . . . . ? N1 Ni1 N2 C2 0.79(10) . . . . ? N3 Ni1 N2 C2 -76.73(11) . . . . ? Cl1 Ni1 N2 C2 -177.20(10) . . . . ? N2 Ni1 N3 C8 -65.50(15) . . . . ? N4 Ni1 N3 C8 146.94(13) . . . . ? N1 Ni1 N3 C8 -145.90(15) . . . . ? Cl1 Ni1 N3 C8 38.38(14) . . . . ? N2 Ni1 N3 C7 97.95(11) . . . . ? N4 Ni1 N3 C7 -49.61(14) . . . . ? N1 Ni1 N3 C7 17.55(11) . . . . ? Cl1 Ni1 N3 C7 -158.17(10) . . . . ? N2 Ni1 N4 C13 96.82(15) . . . . ? N1 Ni1 N4 C13 176.94(16) . . . . ? N3 Ni1 N4 C13 -116.72(15) . . . . ? Cl1 Ni1 N4 C13 -8.57(15) . . . . ? N2 Ni1 N4 C12 -90.42(11) . . . . ? N1 Ni1 N4 C12 -10.30(10) . . . . ? N3 Ni1 N4 C12 56.04(13) . . . . ? Cl1 Ni1 N4 C12 164.20(9) . . . . ? C11 N1 C1 C2 -75.39(16) . . . . ? C6 N1 C1 C2 158.84(13) . . . . ? Ni1 N1 C1 C2 43.39(15) . . . . ? C3 N2 C2 C1 -165.52(14) . . . . ? Ni1 N2 C2 C1 22.64(16) . . . . ? N1 C1 C2 N2 -44.31(18) . . . . ? C2 N2 C3 N5 -174.36(15) . . . . ? Ni1 N2 C3 N5 -4.4(3) . . . . ? C2 N2 C3 O1 4.3(2) . . . . ? Ni1 N2 C3 O1 174.26(10) . . . . ? C5 N5 C3 N2 -170.02(15) . . . . ? C5 N5 C3 O1 11.18(18) . . . . ? C4 O1 C3 N2 -174.07(14) . . . . ? C4 O1 C3 N5 4.82(16) . . . . ? C3 O1 C4 C5 -17.67(16) . . . . ? C3 N5 C5 C4 -20.98(17) . . . . ? O1 C4 C5 N5 22.25(15) . . . . ? C11 N1 C6 C7 167.90(13) . . . . ? C1 N1 C6 C7 -66.31(17) . . . . ? Ni1 N1 C6 C7 48.97(14) . . . . ? C8 N3 C7 C6 170.53(14) . . . . ? Ni1 N3 C7 C6 4.50(16) . . . . ? N1 C6 C7 N3 -35.21(18) . . . . ? C7 N3 C8 N6 -178.96(15) . . . . ? Ni1 N3 C8 N6 -15.6(3) . . . . ? C7 N3 C8 O2 1.2(2) . . . . ? Ni1 N3 C8 O2 164.56(11) . . . . ? C10 N6 C8 N3 165.49(16) . . . . ? C10 N6 C8 O2 -14.64(18) . . . . ? C9 O2 C8 N3 178.85(14) . . . . ? C9 O2 C8 N6 -1.03(17) . . . . ? C8 O2 C9 C10 15.14(16) . . . . ? C8 N6 C10 C9 22.56(17) . . . . ? O2 C9 C10 N6 -21.73(15) . . . . ? C6 N1 C11 C12 -77.40(16) . . . . ? C1 N1 C11 C12 156.62(13) . . . . ? Ni1 N1 C11 C12 39.76(15) . . . . ? C13 N4 C12 C11 -151.57(14) . . . . ? Ni1 N4 C12 C11 34.15(15) . . . . ? N1 C11 C12 N4 -48.84(17) . . . . ? C12 N4 C13 N7 176.25(15) . . . . ? Ni1 N4 C13 N7 -11.2(3) . . . . ? C12 N4 C13 O3 -2.9(2) . . . . ? Ni1 N4 C13 O3 169.66(10) . . . . ? C15 N7 C13 N4 168.69(16) . . . . ? C15 N7 C13 O3 -12.06(18) . . . . ? C14 O3 C13 N4 173.60(14) . . . . ? C14 O3 C13 N7 -5.70(17) . . . . ? C13 O3 C14 C15 19.90(16) . . . . ? C13 N7 C15 C14 23.18(17) . . . . ? O3 C14 C15 N7 -24.96(15) . . . . ? C34 B1 C16 C17 -33.40(18) . . . . ? C22 B1 C16 C17 88.75(17) . . . . ? C28 B1 C16 C17 -152.77(14) . . . . ? C34 B1 C16 C21 147.53(14) . . . . ? C22 B1 C16 C21 -90.32(17) . . . . ? C28 B1 C16 C21 28.17(19) . . . . ? C21 C16 C17 C18 -0.6(2) . . . . ? B1 C16 C17 C18 -179.72(14) . . . . ? C16 C17 C18 C19 0.2(3) . . . . ? C17 C18 C19 C20 0.5(3) . . . . ? C18 C19 C20 C21 -0.7(2) . . . . ? C19 C20 C21 C16 0.3(3) . . . . ? C17 C16 C21 C20 0.3(2) . . . . ? B1 C16 C21 C20 179.47(14) . . . . ? C34 B1 C22 C23 157.08(13) . . . . ? C28 B1 C22 C23 -83.83(16) . . . . ? C16 B1 C22 C23 36.92(19) . . . . ? C34 B1 C22 C27 -30.39(19) . . . . ? C28 B1 C22 C27 88.70(16) . . . . ? C16 B1 C22 C27 -150.55(14) . . . . ? C27 C22 C23 C24 -0.5(2) . . . . ? B1 C22 C23 C24 172.52(14) . . . . ? C22 C23 C24 C25 0.1(2) . . . . ? C23 C24 C25 C26 0.3(2) . . . . ? C24 C25 C26 C27 -0.2(2) . . . . ? C25 C26 C27 C22 -0.2(2) . . . . ? C23 C22 C27 C26 0.5(2) . . . . ? B1 C22 C27 C26 -172.46(14) . . . . ? C34 B1 C28 C29 98.69(16) . . . . ? C22 B1 C28 C29 -22.11(19) . . . . ? C16 B1 C28 C29 -142.33(14) . . . . ? C34 B1 C28 C33 -76.09(17) . . . . ? C22 B1 C28 C33 163.11(13) . . . . ? C16 B1 C28 C33 42.89(18) . . . . ? C33 C28 C29 C30 1.8(2) . . . . ? B1 C28 C29 C30 -173.32(14) . . . . ? C28 C29 C30 C31 -0.6(2) . . . . ? C29 C30 C31 C32 -1.0(2) . . . . ? C30 C31 C32 C33 1.2(2) . . . . ? C31 C32 C33 C28 0.2(3) . . . . ? C29 C28 C33 C32 -1.6(2) . . . . ? B1 C28 C33 C32 173.59(15) . . . . ? C22 B1 C34 C39 143.05(14) . . . . ? C28 B1 C34 C39 24.96(19) . . . . ? C16 B1 C34 C39 -95.69(16) . . . . ? C22 B1 C34 C35 -40.65(19) . . . . ? C28 B1 C34 C35 -158.74(13) . . . . ? C16 B1 C34 C35 80.61(17) . . . . ? C39 C34 C35 C36 0.2(2) . . . . ? B1 C34 C35 C36 -176.39(14) . . . . ? C34 C35 C36 C37 -0.3(2) . . . . ? C35 C36 C37 C38 0.2(2) . . . . ? C36 C37 C38 C39 0.0(2) . . . . ? C37 C38 C39 C34 -0.1(2) . . . . ? C35 C34 C39 C38 0.0(2) . . . . ? B1 C34 C39 C38 176.56(14) . . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.378 _refine_diff_density_min -0.249 _refine_diff_density_rms 0.055 #==END data_asb120 _database_code_depnum_ccdc_archive 'CCDC 855309' #TrackingRef '- DT-ART-11-2011-012244-CIF.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H47 B Cl Cu N7 O3' _chemical_formula_weight 771.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 11.4375(5) _cell_length_b 20.0606(8) _cell_length_c 15.7480(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.2570(10) _cell_angle_gamma 90.00 _cell_volume 3591.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 98(2) _cell_measurement_reflns_used 9862 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 28.28 _exptl_crystal_description irregular _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1620 _exptl_absorpt_coefficient_mu 0.732 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7582 _exptl_absorpt_correction_T_max 0.9044 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 98(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX II CCD' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 42713 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0219 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 28.30 _reflns_number_total 8788 _reflns_number_gt 7539 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX2' _computing_cell_refinement 'Bruker SMART APEX2/SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0404P)^2^+2.0894P] 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 8788 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0827 _refine_ls_wR_factor_gt 0.0789 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 Cu1 Cu 0.505012(15) 0.207709(9) 0.387858(11) 0.01292(6) Uani 1 1 d . . . Cl1 Cl 0.70521(3) 0.203539(16) 0.42197(2) 0.01430(8) Uani 1 1 d . . . O1 O 0.56213(9) 0.34170(5) 0.18010(7) 0.0182(2) Uani 1 1 d . . . O2 O 0.50938(10) -0.01022(6) 0.38076(8) 0.0277(3) Uani 1 1 d . . . O3 O 0.47234(9) 0.33233(5) 0.60987(7) 0.0188(2) Uani 1 1 d . . . N1 N 0.32533(11) 0.20952(6) 0.35628(8) 0.0143(2) Uani 1 1 d . . . N2 N 0.50564(11) 0.26663(6) 0.27839(8) 0.0147(2) Uani 1 1 d . . . N3 N 0.47883(11) 0.10373(6) 0.37544(8) 0.0162(2) Uani 1 1 d . . . N4 N 0.46265(11) 0.25626(6) 0.49822(8) 0.0163(3) Uani 1 1 d . . . N5 N 0.70030(11) 0.27524(6) 0.24218(8) 0.0164(3) Uani 1 1 d . . . H5 H 0.7310 0.2410 0.2717 0.020 Uiso 1 1 calc R . . N6 N 0.65621(12) 0.05319(7) 0.43211(11) 0.0312(4) Uani 1 1 d . . . H6 H 0.6947 0.0900 0.4472 0.037 Uiso 1 1 calc R . . N7 N 0.63806(11) 0.30719(7) 0.55722(8) 0.0185(3) Uani 1 1 d . . . H7 H 0.6875 0.2833 0.5307 0.022 Uiso 1 1 calc R . . C1 C 0.30270(13) 0.23310(7) 0.26629(10) 0.0172(3) Uani 1 1 d . . . H1A H 0.2203 0.2486 0.2549 0.021 Uiso 1 1 calc R . . H1B H 0.3141 0.1958 0.2269 0.021 Uiso 1 1 calc R . . C2 C 0.38529(13) 0.28937(7) 0.25065(10) 0.0176(3) Uani 1 1 d . . . H2A H 0.3775 0.3011 0.1892 0.021 Uiso 1 1 calc R . . H2B H 0.3665 0.3293 0.2835 0.021 Uiso 1 1 calc R . . C3 C 0.58704(13) 0.29266(7) 0.23783(9) 0.0141(3) Uani 1 1 d . . . C4 C 0.66836(14) 0.35909(8) 0.14176(10) 0.0198(3) Uani 1 1 d . . . H4A H 0.6837 0.4076 0.1465 0.024 Uiso 1 1 calc R . . H4B H 0.6608 0.3464 0.0806 0.024 Uiso 1 1 calc R . . C5 C 0.76716(13) 0.31978(8) 0.19202(10) 0.0187(3) Uani 1 1 d . . . H5B H 0.8140 0.2945 0.1536 0.022 Uiso 1 1 calc R . . H5C H 0.8199 0.3493 0.2292 0.022 Uiso 1 1 calc R . . C6 C 0.27713(13) 0.14128(8) 0.36410(10) 0.0188(3) Uani 1 1 d . . . H6A H 0.1996 0.1379 0.3296 0.023 Uiso 1 1 calc R . . H6B H 0.2658 0.1323 0.4245 0.023 Uiso 1 1 calc R . . C7 C 0.36050(13) 0.08993(8) 0.33344(10) 0.0185(3) Uani 1 1 d . . . H7B H 0.3356 0.0445 0.3481 0.022 Uiso 1 1 calc R . . H7C H 0.3601 0.0928 0.2706 0.022 Uiso 1 1 calc R . . C8 C 0.54628(13) 0.05285(7) 0.39492(9) 0.0147(3) Uani 1 1 d . . . C9 C 0.60341(13) -0.05617(7) 0.41070(10) 0.0183(3) Uani 1 1 d . . . H9A H 0.6252 -0.0843 0.3632 0.022 Uiso 1 1 calc R . . H9B H 0.5790 -0.0855 0.4562 0.022 Uiso 1 1 calc R . . C10 C 0.70640(14) -0.01180(7) 0.44544(11) 0.0206(3) Uani 1 1 d . . . H10A H 0.7302 -0.0205 0.5068 0.025 Uiso 1 1 calc R . . H10B H 0.7751 -0.0180 0.4131 0.025 Uiso 1 1 calc R . . C11 C 0.27294(13) 0.25659(8) 0.41468(10) 0.0207(3) Uani 1 1 d . . . H11A H 0.1884 0.2464 0.4155 0.025 Uiso 1 1 calc R . . H11B H 0.2800 0.3028 0.3938 0.025 Uiso 1 1 calc R . . C12 C 0.33601(13) 0.25044(9) 0.50438(10) 0.0213(3) Uani 1 1 d . . . H12A H 0.3099 0.2862 0.5413 0.026 Uiso 1 1 calc R . . H12B H 0.3182 0.2068 0.5294 0.026 Uiso 1 1 calc R . . C13 C 0.52220(13) 0.29593(7) 0.55113(9) 0.0150(3) Uani 1 1 d . . . C14 C 0.56382(14) 0.37150(8) 0.65935(10) 0.0207(3) Uani 1 1 d . . . H14A H 0.5784 0.3544 0.7185 0.025 Uiso 1 1 calc R . . H14B H 0.5405 0.4189 0.6613 0.025 Uiso 1 1 calc R . . C15 C 0.67335(14) 0.36359(8) 0.61293(10) 0.0197(3) Uani 1 1 d . . . H15A H 0.6887 0.4040 0.5797 0.024 Uiso 1 1 calc R . . H15B H 0.7437 0.3531 0.6530 0.024 Uiso 1 1 calc R . . B1 B 0.05616(14) 0.48117(8) 0.28965(10) 0.0131(3) Uani 1 1 d . . . C16 C 0.04282(12) 0.56242(7) 0.28041(9) 0.0143(3) Uani 1 1 d . . . C17 C 0.06928(13) 0.59974(7) 0.20955(10) 0.0164(3) Uani 1 1 d . . . H17A H 0.0969 0.5771 0.1627 0.020 Uiso 1 1 calc R . . C18 C 0.05645(13) 0.66892(8) 0.20544(10) 0.0179(3) Uani 1 1 d . . . H18A H 0.0741 0.6922 0.1559 0.022 Uiso 1 1 calc R . . C19 C 0.01813(13) 0.70379(7) 0.27305(11) 0.0196(3) Uani 1 1 d . . . H19A H 0.0077 0.7507 0.2699 0.024 Uiso 1 1 calc R . . C20 C -0.00478(14) 0.66885(8) 0.34582(10) 0.0206(3) Uani 1 1 d . . . H20A H -0.0288 0.6921 0.3935 0.025 Uiso 1 1 calc R . . C21 C 0.00753(13) 0.59987(8) 0.34881(10) 0.0180(3) Uani 1 1 d . . . H21A H -0.0086 0.5771 0.3991 0.022 Uiso 1 1 calc R . . C22 C -0.05666(13) 0.45090(7) 0.33292(9) 0.0148(3) Uani 1 1 d . . . C23 C -0.05260(14) 0.39242(8) 0.38225(10) 0.0200(3) Uani 1 1 d . . . H23A H 0.0211 0.3711 0.3966 0.024 Uiso 1 1 calc R . . C24 C -0.15286(15) 0.36463(9) 0.41085(10) 0.0249(3) Uani 1 1 d . . . H24A H -0.1463 0.3256 0.4451 0.030 Uiso 1 1 calc R . . C25 C -0.26226(15) 0.39377(9) 0.38952(11) 0.0249(4) Uani 1 1 d . . . H25A H -0.3309 0.3748 0.4086 0.030 Uiso 1 1 calc R . . C26 C -0.26954(14) 0.45076(8) 0.34020(11) 0.0237(3) Uani 1 1 d . . . H26A H -0.3439 0.4710 0.3244 0.028 Uiso 1 1 calc R . . C27 C -0.16854(13) 0.47876(8) 0.31350(10) 0.0193(3) Uani 1 1 d . . . H27A H -0.1758 0.5185 0.2806 0.023 Uiso 1 1 calc R . . C28 C 0.04901(12) 0.44160(7) 0.19754(9) 0.0133(3) Uani 1 1 d . . . C29 C -0.02551(13) 0.46089(8) 0.12480(10) 0.0173(3) Uani 1 1 d . . . H29A H -0.0698 0.5008 0.1270 0.021 Uiso 1 1 calc R . . C30 C -0.03698(14) 0.42374(8) 0.04955(10) 0.0209(3) Uani 1 1 d . . . H30A H -0.0878 0.4390 0.0018 0.025 Uiso 1 1 calc R . . C31 C 0.02507(14) 0.36469(8) 0.04368(10) 0.0203(3) Uani 1 1 d . . . H31A H 0.0177 0.3395 -0.0078 0.024 Uiso 1 1 calc R . . C32 C 0.09794(13) 0.34326(7) 0.11458(10) 0.0175(3) Uani 1 1 d . . . H32A H 0.1406 0.3028 0.1121 0.021 Uiso 1 1 calc R . . C33 C 0.10871(13) 0.38096(7) 0.18953(9) 0.0154(3) Uani 1 1 d . . . H33A H 0.1586 0.3649 0.2373 0.018 Uiso 1 1 calc R . . C34 C 0.18291(13) 0.46759(7) 0.34626(10) 0.0155(3) Uani 1 1 d . . . C35 C 0.19799(14) 0.45881(8) 0.43524(10) 0.0205(3) Uani 1 1 d . . . H35A H 0.1310 0.4613 0.4659 0.025 Uiso 1 1 calc R . . C36 C 0.30810(16) 0.44652(8) 0.48028(11) 0.0271(4) Uani 1 1 d . . . H36A H 0.3146 0.4407 0.5405 0.032 Uiso 1 1 calc R . . C37 C 0.40733(15) 0.44285(8) 0.43799(12) 0.0285(4) Uani 1 1 d . . . H37A H 0.4817 0.4330 0.4683 0.034 Uiso 1 1 calc R . . C38 C 0.39686(14) 0.45366(8) 0.35065(12) 0.0259(4) Uani 1 1 d . . . H38A H 0.4647 0.4524 0.3208 0.031 Uiso 1 1 calc R . . C39 C 0.28676(13) 0.46643(8) 0.30659(11) 0.0200(3) Uani 1 1 d . . . H39A H 0.2819 0.4747 0.2469 0.024 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 Cu1 0.01010(9) 0.01340(9) 0.01490(9) 0.00038(6) -0.00036(6) -0.00005(6) Cl1 0.01163(15) 0.01406(16) 0.01694(16) 0.00163(12) 0.00029(12) -0.00050(12) O1 0.0169(5) 0.0175(5) 0.0203(5) 0.0068(4) 0.0023(4) 0.0019(4) O2 0.0218(6) 0.0109(5) 0.0465(8) -0.0008(5) -0.0128(5) -0.0004(4) O3 0.0193(5) 0.0202(6) 0.0171(5) -0.0039(4) 0.0030(4) -0.0003(4) N1 0.0124(6) 0.0140(6) 0.0160(6) 0.0002(5) -0.0003(5) 0.0002(4) N2 0.0136(6) 0.0138(6) 0.0161(6) 0.0008(5) -0.0013(5) 0.0012(5) N3 0.0128(6) 0.0144(6) 0.0209(6) -0.0008(5) -0.0006(5) -0.0007(5) N4 0.0130(6) 0.0199(6) 0.0162(6) -0.0007(5) 0.0023(5) -0.0003(5) N5 0.0156(6) 0.0159(6) 0.0182(6) 0.0046(5) 0.0029(5) 0.0025(5) N6 0.0162(7) 0.0118(6) 0.0625(11) -0.0025(6) -0.0101(7) 0.0008(5) N7 0.0172(6) 0.0189(6) 0.0198(6) -0.0059(5) 0.0030(5) -0.0028(5) C1 0.0148(7) 0.0164(7) 0.0192(7) 0.0010(6) -0.0031(6) 0.0004(5) C2 0.0145(7) 0.0165(7) 0.0212(7) 0.0034(6) -0.0009(6) 0.0019(5) C3 0.0177(7) 0.0112(6) 0.0128(6) -0.0009(5) -0.0010(5) 0.0016(5) C4 0.0214(8) 0.0197(8) 0.0191(7) 0.0053(6) 0.0059(6) 0.0012(6) C5 0.0190(7) 0.0184(7) 0.0194(7) 0.0032(6) 0.0051(6) 0.0004(6) C6 0.0133(7) 0.0178(7) 0.0247(8) 0.0026(6) -0.0006(6) -0.0022(5) C7 0.0156(7) 0.0148(7) 0.0240(8) -0.0001(6) -0.0025(6) -0.0022(5) C8 0.0164(7) 0.0132(7) 0.0150(7) -0.0018(5) 0.0034(5) -0.0025(5) C9 0.0177(7) 0.0127(7) 0.0239(8) 0.0008(6) -0.0003(6) 0.0015(5) C10 0.0190(7) 0.0132(7) 0.0281(8) -0.0008(6) -0.0037(6) 0.0013(6) C11 0.0141(7) 0.0230(8) 0.0249(8) -0.0043(6) 0.0018(6) 0.0025(6) C12 0.0151(7) 0.0293(9) 0.0199(7) -0.0048(6) 0.0045(6) -0.0015(6) C13 0.0180(7) 0.0141(7) 0.0132(6) 0.0028(5) 0.0033(5) 0.0023(5) C14 0.0273(8) 0.0147(7) 0.0202(7) -0.0037(6) 0.0037(6) -0.0046(6) C15 0.0220(8) 0.0181(7) 0.0189(7) -0.0028(6) 0.0018(6) -0.0043(6) B1 0.0110(7) 0.0134(7) 0.0150(7) -0.0004(6) 0.0014(6) 0.0000(6) C16 0.0093(6) 0.0155(7) 0.0175(7) -0.0011(5) -0.0009(5) -0.0001(5) C17 0.0136(7) 0.0172(7) 0.0185(7) -0.0018(6) 0.0021(5) -0.0015(5) C18 0.0136(7) 0.0167(7) 0.0231(8) 0.0028(6) 0.0002(6) -0.0033(5) C19 0.0129(7) 0.0136(7) 0.0314(8) -0.0017(6) -0.0017(6) -0.0007(5) C20 0.0183(7) 0.0188(8) 0.0249(8) -0.0073(6) 0.0029(6) 0.0014(6) C21 0.0171(7) 0.0178(7) 0.0194(7) -0.0010(6) 0.0031(6) -0.0004(6) C22 0.0149(7) 0.0154(7) 0.0141(6) -0.0023(5) 0.0018(5) -0.0016(5) C23 0.0196(7) 0.0200(8) 0.0199(7) 0.0013(6) 0.0001(6) -0.0027(6) C24 0.0310(9) 0.0241(8) 0.0196(8) 0.0037(6) 0.0023(7) -0.0103(7) C25 0.0217(8) 0.0320(9) 0.0227(8) -0.0058(7) 0.0096(6) -0.0115(7) C26 0.0144(7) 0.0262(8) 0.0311(9) -0.0052(7) 0.0054(6) -0.0015(6) C27 0.0162(7) 0.0175(7) 0.0244(8) -0.0003(6) 0.0036(6) -0.0004(6) C28 0.0103(6) 0.0134(7) 0.0163(7) 0.0004(5) 0.0022(5) -0.0023(5) C29 0.0152(7) 0.0153(7) 0.0208(7) 0.0008(6) -0.0011(6) 0.0016(5) C30 0.0223(8) 0.0215(8) 0.0173(7) 0.0016(6) -0.0055(6) -0.0005(6) C31 0.0238(8) 0.0199(8) 0.0170(7) -0.0044(6) 0.0019(6) -0.0028(6) C32 0.0172(7) 0.0143(7) 0.0214(7) -0.0016(6) 0.0041(6) 0.0000(5) C33 0.0134(6) 0.0154(7) 0.0172(7) 0.0018(5) 0.0009(5) -0.0006(5) C34 0.0144(7) 0.0107(6) 0.0206(7) -0.0025(5) -0.0014(6) 0.0000(5) C35 0.0216(8) 0.0177(7) 0.0211(7) -0.0027(6) -0.0024(6) 0.0005(6) C36 0.0326(9) 0.0202(8) 0.0249(8) -0.0028(6) -0.0125(7) 0.0016(7) C37 0.0208(8) 0.0163(8) 0.0441(10) -0.0076(7) -0.0165(7) 0.0032(6) C38 0.0129(7) 0.0189(8) 0.0452(10) -0.0108(7) -0.0005(7) -0.0006(6) C39 0.0154(7) 0.0181(7) 0.0260(8) -0.0052(6) 0.0006(6) -0.0014(6) _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 Cu1 N1 2.0614(12) . ? Cu1 N2 2.0909(12) . ? Cu1 N4 2.0947(12) . ? Cu1 N3 2.1133(13) . ? Cu1 Cl1 2.2957(4) . ? O1 C3 1.3486(17) . ? O1 C4 1.4569(18) . ? O2 C8 1.3446(18) . ? O2 C9 1.4553(18) . ? O3 C13 1.3526(17) . ? O3 C14 1.4634(18) . ? N1 C6 1.4859(19) . ? N1 C11 1.4887(19) . ? N1 C1 1.4897(19) . ? N2 C3 1.2950(19) . ? N2 C2 1.4706(18) . ? N3 C8 1.2959(19) . ? N3 C7 1.4666(19) . ? N4 C13 1.2914(19) . ? N4 C12 1.4668(19) . ? N5 C3 1.3363(19) . ? N5 C5 1.4624(19) . ? N6 C8 1.328(2) . ? N6 C10 1.431(2) . ? N7 C13 1.337(2) . ? N7 C15 1.4614(19) . ? C1 C2 1.509(2) . ? C4 C5 1.526(2) . ? C6 C7 1.518(2) . ? C9 C10 1.529(2) . ? C11 C12 1.520(2) . ? C14 C15 1.526(2) . ? B1 C34 1.640(2) . ? B1 C22 1.640(2) . ? B1 C16 1.642(2) . ? B1 C28 1.648(2) . ? C16 C17 1.404(2) . ? C16 C21 1.408(2) . ? C17 C18 1.396(2) . ? C18 C19 1.384(2) . ? C19 C20 1.392(2) . ? C20 C21 1.391(2) . ? C22 C27 1.399(2) . ? C22 C23 1.405(2) . ? C23 C24 1.393(2) . ? C24 C25 1.389(3) . ? C25 C26 1.380(2) . ? C26 C27 1.390(2) . ? C28 C29 1.406(2) . ? C28 C33 1.407(2) . ? C29 C30 1.394(2) . ? C30 C31 1.389(2) . ? C31 C32 1.387(2) . ? C32 C33 1.396(2) . ? C34 C39 1.401(2) . ? C34 C35 1.404(2) . ? C35 C36 1.398(2) . ? C36 C37 1.379(3) . ? C37 C38 1.385(3) . ? C38 C39 1.394(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N2 83.34(5) . . ? N1 Cu1 N4 82.95(5) . . ? N2 Cu1 N4 116.31(5) . . ? N1 Cu1 N3 82.39(5) . . ? N2 Cu1 N3 119.66(5) . . ? N4 Cu1 N3 119.50(5) . . ? N1 Cu1 Cl1 178.85(4) . . ? N2 Cu1 Cl1 96.92(3) . . ? N4 Cu1 Cl1 97.92(4) . . ? N3 Cu1 Cl1 96.51(3) . . ? C3 O1 C4 109.24(11) . . ? C8 O2 C9 109.56(11) . . ? C13 O3 C14 108.89(12) . . ? C6 N1 C11 110.81(12) . . ? C6 N1 C1 110.11(11) . . ? C11 N1 C1 110.27(11) . . ? C6 N1 Cu1 109.44(9) . . ? C11 N1 Cu1 108.66(9) . . ? C1 N1 Cu1 107.48(9) . . ? C3 N2 C2 115.36(12) . . ? C3 N2 Cu1 134.58(10) . . ? C2 N2 Cu1 109.45(9) . . ? C8 N3 C7 117.02(12) . . ? C8 N3 Cu1 132.91(10) . . ? C7 N3 Cu1 110.03(9) . . ? C13 N4 C12 117.49(13) . . ? C13 N4 Cu1 131.94(10) . . ? C12 N4 Cu1 109.71(9) . . ? C3 N5 C5 111.94(12) . . ? C8 N6 C10 113.93(13) . . ? C13 N7 C15 112.37(13) . . ? N1 C1 C2 110.23(12) . . ? N2 C2 C1 107.56(12) . . ? N2 C3 N5 127.90(13) . . ? N2 C3 O1 121.08(13) . . ? N5 C3 O1 110.96(13) . . ? O1 C4 C5 105.38(11) . . ? N5 C5 C4 101.22(12) . . ? N1 C6 C7 110.32(12) . . ? N3 C7 C6 108.02(12) . . ? N3 C8 N6 127.66(14) . . ? N3 C8 O2 122.27(13) . . ? N6 C8 O2 110.05(13) . . ? O2 C9 C10 105.10(12) . . ? N6 C10 C9 101.35(12) . . ? N1 C11 C12 109.90(12) . . ? N4 C12 C11 107.71(12) . . ? N4 C13 N7 126.82(14) . . ? N4 C13 O3 122.81(13) . . ? N7 C13 O3 110.37(13) . . ? O3 C14 C15 105.42(12) . . ? N7 C15 C14 100.40(12) . . ? C34 B1 C22 113.68(12) . . ? C34 B1 C16 106.33(11) . . ? C22 B1 C16 109.55(11) . . ? C34 B1 C28 110.77(12) . . ? C22 B1 C28 102.80(11) . . ? C16 B1 C28 113.89(12) . . ? C17 C16 C21 115.36(13) . . ? C17 C16 B1 125.01(13) . . ? C21 C16 B1 119.56(13) . . ? C18 C17 C16 122.42(14) . . ? C19 C18 C17 120.46(14) . . ? C18 C19 C20 118.84(14) . . ? C21 C20 C19 120.08(14) . . ? C20 C21 C16 122.76(14) . . ? C27 C22 C23 115.37(14) . . ? C27 C22 B1 120.23(13) . . ? C23 C22 B1 123.98(13) . . ? C24 C23 C22 122.28(15) . . ? C25 C24 C23 120.33(15) . . ? C26 C25 C24 118.85(15) . . ? C25 C26 C27 120.26(15) . . ? C26 C27 C22 122.88(15) . . ? C29 C28 C33 114.96(13) . . ? C29 C28 B1 123.52(13) . . ? C33 C28 B1 121.16(12) . . ? C30 C29 C28 122.56(14) . . ? C31 C30 C29 120.74(14) . . ? C32 C31 C30 118.50(14) . . ? C31 C32 C33 120.18(14) . . ? C32 C33 C28 123.04(14) . . ? C39 C34 C35 115.15(14) . . ? C39 C34 B1 120.17(13) . . ? C35 C34 B1 124.65(13) . . ? C36 C35 C34 122.29(16) . . ? C37 C36 C35 120.51(16) . . ? C36 C37 C38 118.99(15) . . ? C37 C38 C39 119.94(16) . . ? C38 C39 C34 123.01(16) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.401 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.057 #==END data_asb113 _database_code_depnum_ccdc_archive 'CCDC 855310' #TrackingRef '- DT-ART-11-2011-012244-CIF.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H47 B Cl N7 O3 Zn' _chemical_formula_weight 773.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 11.4509(6) _cell_length_b 20.1051(10) _cell_length_c 15.7239(8) _cell_angle_alpha 90.00 _cell_angle_beta 96.1007(7) _cell_angle_gamma 90.00 _cell_volume 3599.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 9955 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 28.19 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 0.806 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7998 _exptl_absorpt_correction_T_max 0.9457 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX II CCD' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 38564 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7355 _reflns_number_gt 6067 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX2' _computing_cell_refinement 'Bruker SMART APEX2/SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0483P)^2^+2.2808P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7355 _refine_ls_number_parameters 481 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0930 _refine_ls_wR_factor_gt 0.0868 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.988326(19) 0.206966(11) 0.108955(14) 0.01807(8) Uani 1 1 d . . . Cl1 Cl 0.78077(4) 0.20204(2) 0.07225(3) 0.02402(12) Uani 1 1 d . . . O1 O 0.94067(13) 0.34092(7) 0.31558(9) 0.0268(3) Uani 1 1 d . . . O2 O 0.99033(13) -0.00849(7) 0.12121(11) 0.0342(4) Uani 1 1 d . . . O3 O 1.02740(13) 0.32991(8) -0.11033(9) 0.0279(3) Uani 1 1 d . . . N1 N 1.18415(15) 0.20845(8) 0.14175(11) 0.0216(4) Uani 1 1 d . . . N2 N 0.99687(14) 0.26605(8) 0.21685(10) 0.0207(4) Uani 1 1 d . . . N3 N 1.02159(15) 0.10501(8) 0.12398(11) 0.0213(4) Uani 1 1 d . . . N4 N 1.03735(15) 0.25375(9) 0.00101(11) 0.0226(4) Uani 1 1 d . . . N5 N 0.80345(16) 0.27414(9) 0.25503(12) 0.0248(4) Uani 1 1 d . . . N6 N 0.84653(18) 0.05400(10) 0.06519(15) 0.0344(5) Uani 1 1 d . . . N7 N 0.86404(17) 0.30798(10) -0.05421(12) 0.0281(4) Uani 1 1 d . . . H5 H 0.773(2) 0.2546(14) 0.2141(17) 0.037(8) Uiso 1 1 d . . . H6 H 0.818(2) 0.0859(14) 0.0606(17) 0.032(8) Uiso 1 1 d . . . H7 H 0.825(2) 0.2898(13) -0.0208(18) 0.041(8) Uiso 1 1 d . . . C1 C 1.20305(18) 0.23482(11) 0.22968(13) 0.0246(4) Uani 1 1 d . . . H1A H 1.2843 0.2519 0.2410 0.030 Uiso 1 1 calc R . . H1B H 1.1930 0.1986 0.2709 0.030 Uiso 1 1 calc R . . C2 C 1.11708(18) 0.29014(10) 0.24196(14) 0.0258(5) Uani 1 1 d . . . H2A H 1.1250 0.3043 0.3026 0.031 Uiso 1 1 calc R . . H2B H 1.1339 0.3289 0.2065 0.031 Uiso 1 1 calc R . . C3 C 0.91573(18) 0.29187(10) 0.25799(12) 0.0211(4) Uani 1 1 d . . . C4 C 0.8345(2) 0.35828(12) 0.35371(14) 0.0295(5) Uani 1 1 d . . . H4A H 0.8183 0.4065 0.3477 0.035 Uiso 1 1 calc R . . H4B H 0.8425 0.3467 0.4153 0.035 Uiso 1 1 calc R . . C5 C 0.73647(19) 0.31818(11) 0.30537(14) 0.0269(5) Uani 1 1 d . . . H5A H 0.6912 0.2928 0.3448 0.032 Uiso 1 1 calc R . . H5B H 0.6823 0.3469 0.2684 0.032 Uiso 1 1 calc R . . C6 C 1.22674(18) 0.13972(10) 0.13716(15) 0.0259(5) Uani 1 1 d . . . H6A H 1.3030 0.1353 0.1728 0.031 Uiso 1 1 calc R . . H6B H 1.2393 0.1290 0.0773 0.031 Uiso 1 1 calc R . . C7 C 1.13934(18) 0.09119(11) 0.16820(14) 0.0255(5) Uani 1 1 d . . . H7A H 1.1628 0.0450 0.1561 0.031 Uiso 1 1 calc R . . H7B H 1.1379 0.0959 0.2308 0.031 Uiso 1 1 calc R . . C8 C 0.95451(18) 0.05410(10) 0.10473(12) 0.0202(4) Uani 1 1 d . . . C9 C 0.89725(19) -0.05445(11) 0.09042(14) 0.0273(5) Uani 1 1 d . . . H9A H 0.8743 -0.0824 0.1378 0.033 Uiso 1 1 calc R . . H9B H 0.9230 -0.0838 0.0454 0.033 Uiso 1 1 calc R . . C10 C 0.7955(2) -0.01061(11) 0.05442(15) 0.0299(5) Uani 1 1 d . . . H10A H 0.7715 -0.0205 -0.0066 0.036 Uiso 1 1 calc R . . H10B H 0.7269 -0.0155 0.0873 0.036 Uiso 1 1 calc R . . C11 C 1.23232(18) 0.25251(12) 0.07936(14) 0.0287(5) Uani 1 1 d . . . H11A H 1.3156 0.2410 0.0752 0.034 Uiso 1 1 calc R . . H11B H 1.2290 0.2992 0.0989 0.034 Uiso 1 1 calc R . . C12 C 1.16288(18) 0.24548(12) -0.00774(14) 0.0295(5) Uani 1 1 d . . . H12A H 1.1886 0.2796 -0.0472 0.035 Uiso 1 1 calc R . . H12B H 1.1770 0.2011 -0.0319 0.035 Uiso 1 1 calc R . . C13 C 0.97808(19) 0.29443(10) -0.05093(13) 0.0220(4) Uani 1 1 d . . . C14 C 0.9377(2) 0.37124(11) -0.15718(15) 0.0321(5) Uani 1 1 d . . . H14A H 0.9230 0.3565 -0.2175 0.039 Uiso 1 1 calc R . . H14B H 0.9625 0.4184 -0.1562 0.039 Uiso 1 1 calc R . . C15 C 0.8279(2) 0.36266(11) -0.11171(14) 0.0300(5) Uani 1 1 d . . . H15A H 0.8100 0.4033 -0.0799 0.036 Uiso 1 1 calc R . . H15B H 0.7589 0.3506 -0.1521 0.036 Uiso 1 1 calc R . . B1 B 1.4425(2) 0.48253(11) 0.20975(15) 0.0206(5) Uani 1 1 d . . . C16 C 1.31569(18) 0.46853(10) 0.15385(13) 0.0224(4) Uani 1 1 d . . . C17 C 1.2995(2) 0.45817(11) 0.06532(14) 0.0294(5) Uani 1 1 d . . . H17A H 1.3660 0.4596 0.0340 0.035 Uiso 1 1 calc R . . C18 C 1.1897(2) 0.44587(12) 0.02159(16) 0.0391(6) Uani 1 1 d . . . H18A H 1.1828 0.4388 -0.0385 0.047 Uiso 1 1 calc R . . C19 C 1.0909(2) 0.44383(12) 0.06429(18) 0.0400(6) Uani 1 1 d . . . H19A H 1.0163 0.4340 0.0346 0.048 Uiso 1 1 calc R . . C20 C 1.1022(2) 0.45641(12) 0.15111(18) 0.0372(6) Uani 1 1 d . . . H20A H 1.0348 0.4563 0.1815 0.045 Uiso 1 1 calc R . . C21 C 1.21207(18) 0.46916(11) 0.19400(15) 0.0282(5) Uani 1 1 d . . . H21A H 1.2174 0.4788 0.2534 0.034 Uiso 1 1 calc R . . C22 C 1.45005(17) 0.44317(10) 0.30220(13) 0.0197(4) Uani 1 1 d . . . C23 C 1.39018(18) 0.38326(10) 0.31111(13) 0.0225(4) Uani 1 1 d . . . H23A H 1.3388 0.3676 0.2640 0.027 Uiso 1 1 calc R . . C24 C 1.40243(19) 0.34568(11) 0.38582(14) 0.0255(4) Uani 1 1 d . . . H24A H 1.3597 0.3054 0.3887 0.031 Uiso 1 1 calc R . . C25 C 1.4761(2) 0.36657(11) 0.45569(14) 0.0291(5) Uani 1 1 d . . . H25A H 1.4844 0.3413 0.5070 0.035 Uiso 1 1 calc R . . C26 C 1.5376(2) 0.42510(12) 0.44930(14) 0.0322(5) Uani 1 1 d . . . H26A H 1.5890 0.4402 0.4967 0.039 Uiso 1 1 calc R . . C27 C 1.52506(18) 0.46217(11) 0.37425(13) 0.0252(4) Uani 1 1 d . . . H27A H 1.5692 0.5020 0.3717 0.030 Uiso 1 1 calc R . . C28 C 1.55537(18) 0.45177(10) 0.16648(12) 0.0219(4) Uani 1 1 d . . . C29 C 1.5513(2) 0.39326(11) 0.11815(14) 0.0289(5) Uani 1 1 d . . . H29A H 1.4778 0.3718 0.1046 0.035 Uiso 1 1 calc R . . C30 C 1.6512(2) 0.36533(13) 0.08919(15) 0.0363(6) Uani 1 1 d . . . H30A H 1.6449 0.3260 0.0556 0.044 Uiso 1 1 calc R . . C31 C 1.7596(2) 0.39499(13) 0.10943(15) 0.0360(6) Uani 1 1 d . . . H31A H 1.8281 0.3762 0.0900 0.043 Uiso 1 1 calc R . . C32 C 1.7670(2) 0.45202(12) 0.15799(16) 0.0344(5) Uani 1 1 d . . . H32A H 1.8412 0.4723 0.1732 0.041 Uiso 1 1 calc R . . C33 C 1.66657(19) 0.47999(11) 0.18477(14) 0.0279(5) Uani 1 1 d . . . H33A H 1.6737 0.5201 0.2169 0.033 Uiso 1 1 calc R . . C34 C 1.45608(17) 0.56355(10) 0.21768(13) 0.0211(4) Uani 1 1 d . . . C35 C 1.43064(18) 0.60130(11) 0.28814(13) 0.0239(4) Uani 1 1 d . . . H35A H 1.4035 0.5792 0.3357 0.029 Uiso 1 1 calc R . . C36 C 1.44376(18) 0.67034(11) 0.29115(15) 0.0277(5) Uani 1 1 d . . . H36A H 1.4270 0.6942 0.3406 0.033 Uiso 1 1 calc R . . C37 C 1.48101(19) 0.70405(11) 0.22236(15) 0.0299(5) Uani 1 1 d . . . H37A H 1.4917 0.7509 0.2246 0.036 Uiso 1 1 calc R . . C38 C 1.5025(2) 0.66860(11) 0.15018(15) 0.0313(5) Uani 1 1 d . . . H38A H 1.5259 0.6913 0.1018 0.038 Uiso 1 1 calc R . . C39 C 1.49009(19) 0.60019(11) 0.14852(14) 0.0276(5) Uani 1 1 d . . . H39A H 1.5053 0.5770 0.0983 0.033 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 Zn1 0.01597(12) 0.01754(12) 0.02033(13) -0.00052(9) 0.00018(8) 0.00019(9) Cl1 0.0212(2) 0.0236(3) 0.0271(3) -0.00201(19) 0.00189(19) 0.00030(19) O1 0.0258(8) 0.0262(8) 0.0280(8) -0.0090(6) 0.0012(6) -0.0013(6) O2 0.0277(8) 0.0173(8) 0.0544(10) 0.0018(7) -0.0111(7) -0.0002(6) O3 0.0298(8) 0.0297(8) 0.0247(8) 0.0052(6) 0.0054(6) 0.0004(6) N1 0.0180(8) 0.0202(9) 0.0261(9) -0.0006(7) -0.0004(7) -0.0002(7) N2 0.0187(8) 0.0201(9) 0.0223(9) -0.0025(7) -0.0023(7) -0.0015(7) N3 0.0181(8) 0.0192(9) 0.0260(9) 0.0019(7) 0.0000(7) 0.0020(7) N4 0.0191(9) 0.0259(9) 0.0230(9) 0.0009(7) 0.0033(7) 0.0010(7) N5 0.0237(9) 0.0264(10) 0.0243(10) -0.0057(8) 0.0024(7) -0.0028(8) N6 0.0222(10) 0.0183(10) 0.0603(14) 0.0029(9) -0.0073(9) -0.0002(8) N7 0.0255(10) 0.0307(10) 0.0287(10) 0.0074(8) 0.0052(8) 0.0053(8) C1 0.0196(10) 0.0228(11) 0.0295(11) -0.0017(8) -0.0060(8) -0.0004(8) C2 0.0195(10) 0.0236(11) 0.0328(12) -0.0056(9) -0.0036(9) -0.0031(8) C3 0.0259(11) 0.0179(10) 0.0185(10) 0.0011(8) -0.0022(8) -0.0025(8) C4 0.0333(12) 0.0296(12) 0.0266(11) -0.0057(9) 0.0075(9) 0.0007(10) C5 0.0275(11) 0.0286(11) 0.0252(11) -0.0039(9) 0.0057(9) 0.0006(9) C6 0.0171(10) 0.0235(11) 0.0363(12) -0.0031(9) -0.0002(9) 0.0029(8) C7 0.0203(10) 0.0207(10) 0.0346(12) 0.0006(9) -0.0017(9) 0.0043(8) C8 0.0213(10) 0.0178(10) 0.0218(10) 0.0014(7) 0.0041(8) 0.0024(8) C9 0.0276(11) 0.0191(11) 0.0346(12) -0.0007(9) 0.0006(9) -0.0056(9) C10 0.0279(12) 0.0233(11) 0.0372(12) 0.0008(9) -0.0023(9) -0.0025(9) C11 0.0175(10) 0.0315(12) 0.0371(12) 0.0049(10) 0.0026(9) -0.0027(9) C12 0.0222(11) 0.0363(13) 0.0312(12) 0.0054(10) 0.0075(9) 0.0015(9) C13 0.0259(11) 0.0196(10) 0.0208(10) -0.0057(8) 0.0038(8) -0.0031(8) C14 0.0428(14) 0.0230(11) 0.0309(12) 0.0050(9) 0.0055(10) 0.0072(10) C15 0.0345(13) 0.0282(12) 0.0265(11) 0.0035(9) 0.0000(9) 0.0073(10) B1 0.0178(11) 0.0204(11) 0.0235(11) 0.0005(9) 0.0022(9) -0.0008(9) C16 0.0203(10) 0.0166(10) 0.0294(11) 0.0040(8) -0.0012(8) -0.0012(8) C17 0.0288(12) 0.0265(11) 0.0314(12) 0.0030(9) -0.0035(9) -0.0015(9) C18 0.0445(15) 0.0320(13) 0.0358(13) 0.0038(10) -0.0177(11) -0.0033(11) C19 0.0285(13) 0.0270(12) 0.0591(17) 0.0109(11) -0.0200(12) -0.0057(10) C20 0.0188(11) 0.0297(13) 0.0622(17) 0.0151(12) -0.0007(11) -0.0004(9) C21 0.0212(11) 0.0286(12) 0.0341(12) 0.0064(9) -0.0006(9) 0.0003(9) C22 0.0149(9) 0.0209(10) 0.0236(10) -0.0013(8) 0.0031(8) 0.0030(8) C23 0.0202(10) 0.0218(10) 0.0251(10) -0.0022(8) 0.0008(8) 0.0006(8) C24 0.0256(11) 0.0208(11) 0.0306(11) 0.0017(9) 0.0052(9) -0.0004(9) C25 0.0335(12) 0.0292(12) 0.0245(11) 0.0051(9) 0.0020(9) 0.0024(10) C26 0.0332(12) 0.0350(13) 0.0260(11) -0.0005(9) -0.0072(9) -0.0019(10) C27 0.0231(11) 0.0241(11) 0.0273(11) 0.0003(9) -0.0023(8) -0.0029(9) C28 0.0226(10) 0.0236(10) 0.0197(10) 0.0035(8) 0.0030(8) 0.0021(8) C29 0.0271(12) 0.0294(12) 0.0292(12) -0.0013(9) -0.0018(9) 0.0042(9) C30 0.0452(15) 0.0359(13) 0.0277(12) -0.0043(10) 0.0031(10) 0.0160(11) C31 0.0316(13) 0.0468(15) 0.0312(12) 0.0086(11) 0.0113(10) 0.0166(11) C32 0.0218(11) 0.0398(14) 0.0425(14) 0.0060(11) 0.0074(10) 0.0003(10) C33 0.0218(11) 0.0285(12) 0.0334(12) -0.0006(9) 0.0030(9) 0.0008(9) C34 0.0146(9) 0.0221(10) 0.0258(10) 0.0017(8) -0.0010(8) 0.0012(8) C35 0.0187(10) 0.0270(11) 0.0261(11) 0.0031(9) 0.0024(8) 0.0004(8) C36 0.0194(10) 0.0268(12) 0.0360(12) -0.0049(9) -0.0003(9) 0.0037(9) C37 0.0209(11) 0.0208(11) 0.0467(14) 0.0033(9) -0.0023(9) -0.0006(8) C38 0.0288(12) 0.0289(12) 0.0362(13) 0.0091(10) 0.0036(10) -0.0044(10) C39 0.0274(11) 0.0278(12) 0.0280(11) 0.0021(9) 0.0041(9) 0.0002(9) _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 Zn1 N2 2.0649(16) . ? Zn1 N4 2.0696(17) . ? Zn1 N3 2.0938(17) . ? Zn1 N1 2.2470(17) . ? Zn1 Cl1 2.3875(5) . ? O1 C3 1.349(2) . ? O1 C4 1.454(3) . ? O2 C8 1.340(2) . ? O2 C9 1.454(2) . ? O3 C13 1.346(2) . ? O3 C14 1.459(3) . ? N1 C6 1.470(3) . ? N1 C11 1.472(3) . ? N1 C1 1.475(3) . ? N2 C3 1.296(3) . ? N2 C2 1.473(3) . ? N3 C8 1.296(3) . ? N3 C7 1.476(3) . ? N4 C13 1.296(3) . ? N4 C12 1.468(3) . ? N5 C3 1.330(3) . ? N5 C5 1.459(3) . ? N6 C8 1.324(3) . ? N6 C10 1.427(3) . ? N7 C13 1.330(3) . ? N7 C15 1.455(3) . ? C1 C2 1.511(3) . ? C4 C5 1.519(3) . ? C6 C7 1.515(3) . ? C9 C10 1.521(3) . ? C11 C12 1.516(3) . ? C14 C15 1.521(3) . ? B1 C34 1.640(3) . ? B1 C16 1.640(3) . ? B1 C28 1.644(3) . ? B1 C22 1.649(3) . ? C16 C17 1.400(3) . ? C16 C21 1.402(3) . ? C17 C18 1.389(3) . ? C18 C19 1.377(4) . ? C19 C20 1.381(4) . ? C20 C21 1.386(3) . ? C22 C27 1.400(3) . ? C22 C23 1.400(3) . ? C23 C24 1.391(3) . ? C24 C25 1.378(3) . ? C25 C26 1.380(3) . ? C26 C27 1.390(3) . ? C28 C33 1.396(3) . ? C28 C29 1.399(3) . ? C29 C30 1.393(3) . ? C30 C31 1.383(4) . ? C31 C32 1.375(4) . ? C32 C33 1.385(3) . ? C34 C35 1.399(3) . ? C34 C39 1.402(3) . ? C35 C36 1.397(3) . ? C36 C37 1.382(3) . ? C37 C38 1.384(3) . ? C38 C39 1.383(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 N2 Zn1 N4 114.77(7) . . ? N2 Zn1 N3 118.58(7) . . ? N4 Zn1 N3 118.40(7) . . ? N2 Zn1 N1 81.07(6) . . ? N4 Zn1 N1 80.28(6) . . ? N3 Zn1 N1 79.75(6) . . ? N2 Zn1 Cl1 100.46(5) . . ? N4 Zn1 Cl1 99.81(5) . . ? N3 Zn1 Cl1 98.69(5) . . ? N1 Zn1 Cl1 178.22(5) . . ? C3 O1 C4 109.00(16) . . ? C8 O2 C9 109.50(16) . . ? C13 O3 C14 109.10(16) . . ? C6 N1 C11 112.54(17) . . ? C6 N1 C1 111.56(16) . . ? C11 N1 C1 112.36(17) . . ? C6 N1 Zn1 107.73(12) . . ? C11 N1 Zn1 106.89(12) . . ? C1 N1 Zn1 105.27(12) . . ? C3 N2 C2 115.71(17) . . ? C3 N2 Zn1 131.81(14) . . ? C2 N2 Zn1 111.76(13) . . ? C8 N3 C7 116.77(17) . . ? C8 N3 Zn1 130.59(14) . . ? C7 N3 Zn1 112.55(12) . . ? C13 N4 C12 117.70(18) . . ? C13 N4 Zn1 129.37(14) . . ? C12 N4 Zn1 112.28(13) . . ? C3 N5 C5 112.35(18) . . ? C8 N6 C10 114.04(19) . . ? C13 N7 C15 113.10(19) . . ? N1 C1 C2 110.58(17) . . ? N2 C2 C1 109.07(16) . . ? N2 C3 N5 128.09(19) . . ? N2 C3 O1 121.08(18) . . ? N5 C3 O1 110.75(18) . . ? O1 C4 C5 105.79(16) . . ? N5 C5 C4 100.99(17) . . ? N1 C6 C7 110.83(17) . . ? N3 C7 C6 109.18(17) . . ? N3 C8 N6 127.72(19) . . ? N3 C8 O2 122.32(18) . . ? N6 C8 O2 109.93(18) . . ? O2 C9 C10 105.12(17) . . ? N6 C10 C9 101.28(17) . . ? N1 C11 C12 110.39(17) . . ? N4 C12 C11 109.24(17) . . ? N4 C13 N7 126.9(2) . . ? N4 C13 O3 122.79(19) . . ? N7 C13 O3 110.32(18) . . ? O3 C14 C15 105.73(17) . . ? N7 C15 C14 100.54(17) . . ? C34 B1 C16 106.40(16) . . ? C34 B1 C28 109.46(16) . . ? C16 B1 C28 113.82(17) . . ? C34 B1 C22 114.46(17) . . ? C16 B1 C22 110.50(16) . . ? C28 B1 C22 102.40(16) . . ? C17 C16 C21 114.82(19) . . ? C17 C16 B1 125.07(19) . . ? C21 C16 B1 120.05(19) . . ? C18 C17 C16 122.4(2) . . ? C19 C18 C17 120.8(2) . . ? C18 C19 C20 118.7(2) . . ? C19 C20 C21 120.0(2) . . ? C20 C21 C16 123.1(2) . . ? C27 C22 C23 114.75(18) . . ? C27 C22 B1 123.52(18) . . ? C23 C22 B1 121.38(17) . . ? C24 C23 C22 123.03(19) . . ? C25 C24 C23 120.4(2) . . ? C24 C25 C26 118.4(2) . . ? C25 C26 C27 120.8(2) . . ? C26 C27 C22 122.6(2) . . ? C33 C28 C29 115.51(19) . . ? C33 C28 B1 120.12(18) . . ? C29 C28 B1 124.02(19) . . ? C30 C29 C28 122.4(2) . . ? C31 C30 C29 119.9(2) . . ? C32 C31 C30 119.2(2) . . ? C31 C32 C33 120.2(2) . . ? C32 C33 C28 122.7(2) . . ? C35 C34 C39 115.30(19) . . ? C35 C34 B1 124.97(18) . . ? C39 C34 B1 119.65(18) . . ? C36 C35 C34 122.4(2) . . ? C37 C36 C35 120.1(2) . . ? C36 C37 C38 119.1(2) . . ? C39 C38 C37 120.0(2) . . ? C38 C39 C34 123.0(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.978 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.059