# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Fang Guo' _publ_contact_author_email fguo@lnu.edu.cn _publ_author_name 'Fang Guo' data_CRYSTAL1 _database_code_depnum_ccdc_archive 'CCDC 825594' #TrackingRef '- CRYSTAL1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H42 Cl4 Cu N2 O4' _chemical_formula_weight 748.04 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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.614(5) _cell_length_b 10.367(2) _cell_length_c 14.328(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.43(3) _cell_angle_gamma 90.00 _cell_volume 3565.1(12) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 5758 _cell_measurement_theta_min 2.140 _cell_measurement_theta_max 27.872 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1556 _exptl_absorpt_coefficient_mu 0.951 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8325 _exptl_absorpt_correction_T_max 0.8944 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'rigaku saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11515 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0217 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3132 _reflns_number_gt 2868 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalclear(Rigaku/MSC Inc., 2005)' _computing_cell_refinement crystalclear _computing_data_reduction crystalclear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+1.2159P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3132 _refine_ls_number_parameters 210 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0282 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0768 _refine_ls_wR_factor_gt 0.0754 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.135 _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 0.5000 0.12059(3) 0.2500 0.01892(11) Uani 1 2 d S . . Cl1 Cl 0.440489(17) 0.02551(4) 0.10868(3) 0.02061(12) Uani 1 1 d . . . Cl2 Cl 0.560971(18) 0.19200(4) 0.18410(3) 0.02596(13) Uani 1 1 d . . . O1 O 0.22179(5) 0.34903(13) 0.60677(10) 0.0331(3) Uani 1 1 d . . . O2 O 0.69030(6) 0.57965(14) 0.94248(11) 0.0382(3) Uani 1 1 d . . . N1 N 0.47764(6) 0.21933(13) 0.86248(10) 0.0164(3) Uani 1 1 d D . . C1 C 0.42600(7) 0.14822(17) 0.86682(13) 0.0222(4) Uani 1 1 d . . . H1A H 0.4277 0.0591 0.8475 0.027 Uiso 1 1 calc R . . H1B H 0.4269 0.1485 0.9351 0.027 Uiso 1 1 calc R . . C2 C 0.37180(7) 0.20556(16) 0.80120(13) 0.0196(4) Uani 1 1 d . . . C3 C 0.34495(7) 0.15361(16) 0.70697(13) 0.0219(4) Uani 1 1 d . . . H3 H 0.3609 0.0839 0.6860 0.026 Uiso 1 1 calc R . . C4 C 0.29531(7) 0.20331(17) 0.64418(13) 0.0242(4) Uani 1 1 d . . . H4 H 0.2783 0.1680 0.5811 0.029 Uiso 1 1 calc R . . C5 C 0.27058(7) 0.30669(17) 0.67521(13) 0.0240(4) Uani 1 1 d . . . C6 C 0.29583(8) 0.35781(17) 0.76951(14) 0.0266(4) Uani 1 1 d . . . H6 H 0.2792 0.4258 0.7910 0.032 Uiso 1 1 calc R . . C7 C 0.34624(7) 0.30687(17) 0.83204(13) 0.0242(4) Uani 1 1 d . . . H7 H 0.3630 0.3413 0.8955 0.029 Uiso 1 1 calc R . . C8 C 0.19416(8) 0.4538(2) 0.63486(17) 0.0393(5) Uani 1 1 d . . . H8A H 0.1838 0.4284 0.6904 0.059 Uiso 1 1 calc R . . H8B H 0.1614 0.4767 0.5798 0.059 Uiso 1 1 calc R . . H8C H 0.2188 0.5266 0.6533 0.059 Uiso 1 1 calc R . . C9 C 0.49177(7) 0.33279(17) 0.93295(12) 0.0215(4) Uani 1 1 d . . . H9A H 0.4609 0.3932 0.9129 0.026 Uiso 1 1 calc R . . H9B H 0.4964 0.3027 0.9995 0.026 Uiso 1 1 calc R . . C10 C 0.54369(7) 0.40147(17) 0.93565(11) 0.0197(4) Uani 1 1 d . . . C11 C 0.59633(7) 0.34824(17) 0.98654(12) 0.0238(4) Uani 1 1 d . . . H11 H 0.5990 0.2707 1.0205 0.029 Uiso 1 1 calc R . . C12 C 0.64385(8) 0.40903(18) 0.98686(13) 0.0270(4) Uani 1 1 d . . . H12 H 0.6785 0.3724 1.0208 0.032 Uiso 1 1 calc R . . C13 C 0.64061(8) 0.52568(17) 0.93648(13) 0.0263(4) Uani 1 1 d . . . C14 C 0.58889(8) 0.58043(17) 0.88647(13) 0.0250(4) Uani 1 1 d . . . H14 H 0.5863 0.6585 0.8532 0.030 Uiso 1 1 calc R . . C15 C 0.54116(7) 0.51768(16) 0.88662(12) 0.0214(4) Uani 1 1 d . . . H15 H 0.5066 0.5545 0.8530 0.026 Uiso 1 1 calc R . . C16 C 0.68791(10) 0.6965(2) 0.8881(2) 0.0528(6) Uani 1 1 d . . . H16A H 0.6680 0.6815 0.8186 0.079 Uiso 1 1 calc R . . H16B H 0.7251 0.7249 0.8971 0.079 Uiso 1 1 calc R . . H16C H 0.6691 0.7618 0.9120 0.079 Uiso 1 1 calc R . . C17 C 0.47187(6) 0.25465(15) 0.75745(11) 0.0158(3) Uani 1 1 d . . . H17A H 0.4552 0.3396 0.7421 0.019 Uiso 1 1 calc R . . H17B H 0.4472 0.1936 0.7117 0.019 Uiso 1 1 calc R . . H1 H 0.5061(6) 0.1641(16) 0.8845(14) 0.030(5) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02524(18) 0.01718(17) 0.01659(17) 0.000 0.01012(13) 0.000 Cl1 0.0253(2) 0.0198(2) 0.0153(2) 0.00175(15) 0.00515(17) 0.00202(16) Cl2 0.0326(3) 0.0241(2) 0.0268(2) 0.00066(17) 0.0175(2) -0.00387(17) O1 0.0214(7) 0.0364(7) 0.0357(8) -0.0107(6) 0.0029(6) 0.0075(6) O2 0.0281(7) 0.0380(8) 0.0462(9) 0.0037(7) 0.0099(6) -0.0032(6) N1 0.0196(7) 0.0184(7) 0.0127(7) 0.0033(6) 0.0073(6) 0.0047(6) C1 0.0274(9) 0.0201(8) 0.0245(9) 0.0063(7) 0.0158(8) 0.0010(7) C2 0.0208(9) 0.0201(8) 0.0225(9) 0.0033(7) 0.0132(7) -0.0011(7) C3 0.0221(9) 0.0187(8) 0.0306(10) -0.0048(7) 0.0166(8) -0.0028(7) C4 0.0217(9) 0.0273(9) 0.0256(9) -0.0079(7) 0.0107(7) -0.0041(7) C5 0.0181(9) 0.0254(9) 0.0294(10) -0.0031(8) 0.0095(7) -0.0002(7) C6 0.0250(9) 0.0265(9) 0.0314(10) -0.0078(8) 0.0138(8) 0.0038(8) C7 0.0260(9) 0.0282(10) 0.0213(9) -0.0035(7) 0.0120(7) 0.0009(7) C8 0.0232(10) 0.0376(11) 0.0510(13) -0.0124(10) 0.0053(9) 0.0095(9) C9 0.0265(9) 0.0252(9) 0.0139(8) -0.0024(7) 0.0083(7) 0.0058(7) C10 0.0263(9) 0.0229(8) 0.0098(8) -0.0054(7) 0.0060(7) 0.0042(7) C11 0.0301(10) 0.0221(9) 0.0168(9) 0.0014(7) 0.0052(7) 0.0067(8) C12 0.0241(9) 0.0283(9) 0.0239(9) -0.0004(8) 0.0023(7) 0.0066(8) C13 0.0265(10) 0.0276(10) 0.0232(9) -0.0064(8) 0.0068(8) -0.0008(8) C14 0.0331(10) 0.0205(9) 0.0198(9) -0.0013(7) 0.0074(8) 0.0029(8) C15 0.0255(9) 0.0208(9) 0.0154(8) -0.0033(7) 0.0040(7) 0.0079(7) C16 0.0399(13) 0.0482(14) 0.0687(17) 0.0123(12) 0.0172(12) -0.0104(11) C17 0.0199(8) 0.0181(8) 0.0099(8) 0.0015(6) 0.0060(6) 0.0007(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 Cl2 2.2154(6) . ? Cu1 Cl2 2.2155(6) 2_655 ? Cu1 Cl1 2.2890(8) . ? Cu1 Cl1 2.2891(8) 2_655 ? O1 C5 1.364(2) . ? O1 C8 1.428(2) . ? O2 C13 1.365(2) . ? O2 C16 1.431(3) . ? N1 C17 1.505(2) . ? N1 C9 1.510(2) . ? N1 C1 1.534(2) . ? N1 H1 0.893(9) . ? C1 C2 1.501(2) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C7 1.389(2) . ? C2 C3 1.392(3) . ? C3 C4 1.376(3) . ? C3 H3 0.9300 . ? C4 C5 1.394(3) . ? C4 H4 0.9300 . ? C5 C6 1.384(3) . ? C6 C7 1.393(3) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.497(2) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C15 1.385(2) . ? C10 C11 1.403(2) . ? C11 C12 1.369(3) . ? C11 H11 0.9300 . ? C12 C13 1.396(3) . ? C12 H12 0.9300 . ? C13 C14 1.388(3) . ? C14 C15 1.385(3) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C17 1.529(3) 2_656 ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 Cu1 Cl2 140.96(3) . 2_655 ? Cl2 Cu1 Cl1 96.76(2) . . ? Cl2 Cu1 Cl1 99.79(2) 2_655 . ? Cl2 Cu1 Cl1 99.79(2) . 2_655 ? Cl2 Cu1 Cl1 96.76(2) 2_655 2_655 ? Cl1 Cu1 Cl1 128.99(3) . 2_655 ? C5 O1 C8 117.50(14) . . ? C13 O2 C16 116.82(16) . . ? C17 N1 C9 113.34(13) . . ? C17 N1 C1 111.86(12) . . ? C9 N1 C1 110.86(13) . . ? C17 N1 H1 107.0(13) . . ? C9 N1 H1 106.7(13) . . ? C1 N1 H1 106.6(13) . . ? C2 C1 N1 113.96(13) . . ? C2 C1 H1A 108.8 . . ? N1 C1 H1A 108.8 . . ? C2 C1 H1B 108.8 . . ? N1 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? C7 C2 C3 118.23(16) . . ? C7 C2 C1 122.40(16) . . ? C3 C2 C1 119.34(15) . . ? C4 C3 C2 121.35(16) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 119.89(17) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? O1 C5 C6 125.26(16) . . ? O1 C5 C4 114.98(16) . . ? C6 C5 C4 119.76(17) . . ? C5 C6 C7 119.67(16) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C2 C7 C6 121.07(17) . . ? C2 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? O1 C8 H8A 109.5 . . ? O1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 N1 113.03(13) . . ? C10 C9 H9A 109.0 . . ? N1 C9 H9A 109.0 . . ? C10 C9 H9B 109.0 . . ? N1 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C15 C10 C11 118.17(17) . . ? C15 C10 C9 121.13(15) . . ? C11 C10 C9 120.69(16) . . ? C12 C11 C10 120.84(17) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C13 120.31(17) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? O2 C13 C14 124.43(17) . . ? O2 C13 C12 115.89(16) . . ? C14 C13 C12 119.67(17) . . ? C15 C14 C13 119.38(17) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C10 C15 C14 121.62(16) . . ? C10 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? O2 C16 H16A 109.5 . . ? O2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 C17 C17 111.80(16) . 2_656 ? N1 C17 H17A 109.3 . . ? C17 C17 H17A 109.3 2_656 . ? N1 C17 H17B 109.3 . . ? C17 C17 H17B 109.3 2_656 . ? H17A C17 H17B 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C17 N1 C1 C2 -43.00(19) . . . . ? C9 N1 C1 C2 84.56(17) . . . . ? N1 C1 C2 C7 -85.6(2) . . . . ? N1 C1 C2 C3 96.39(18) . . . . ? C7 C2 C3 C4 2.1(3) . . . . ? C1 C2 C3 C4 -179.78(16) . . . . ? C2 C3 C4 C5 -0.9(3) . . . . ? C8 O1 C5 C6 -0.6(3) . . . . ? C8 O1 C5 C4 179.23(17) . . . . ? C3 C4 C5 O1 179.41(16) . . . . ? C3 C4 C5 C6 -0.7(3) . . . . ? O1 C5 C6 C7 -179.08(17) . . . . ? C4 C5 C6 C7 1.1(3) . . . . ? C3 C2 C7 C6 -1.8(3) . . . . ? C1 C2 C7 C6 -179.80(16) . . . . ? C5 C6 C7 C2 0.2(3) . . . . ? C17 N1 C9 C10 -56.32(18) . . . . ? C1 N1 C9 C10 176.93(13) . . . . ? N1 C9 C10 C15 103.10(18) . . . . ? N1 C9 C10 C11 -75.65(19) . . . . ? C15 C10 C11 C12 -0.6(2) . . . . ? C9 C10 C11 C12 178.18(15) . . . . ? C10 C11 C12 C13 0.2(3) . . . . ? C16 O2 C13 C14 -3.9(3) . . . . ? C16 O2 C13 C12 177.54(19) . . . . ? C11 C12 C13 O2 179.04(16) . . . . ? C11 C12 C13 C14 0.4(3) . . . . ? O2 C13 C14 C15 -179.04(16) . . . . ? C12 C13 C14 C15 -0.6(3) . . . . ? C11 C10 C15 C14 0.5(2) . . . . ? C9 C10 C15 C14 -178.31(15) . . . . ? C13 C14 C15 C10 0.1(3) . . . . ? C9 N1 C17 C17 85.20(12) . . . 2_656 ? C1 N1 C17 C17 -148.58(10) . . . 2_656 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.243 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.048 # Attachment '- CRYSTAL2.cif' data_CRYSTAL2 _database_code_depnum_ccdc_archive 'CCDC 825595' #TrackingRef '- CRYSTAL2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H47 Cl4 Cu N2 O4' _chemical_formula_weight 837.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 10.471(2) _cell_length_b 14.032(3) _cell_length_c 27.239(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.80(3) _cell_angle_gamma 90.00 _cell_volume 3988.4(14) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 11741 _cell_measurement_theta_min 1.634 _cell_measurement_theta_max 27.910 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 0.859 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7827 _exptl_absorpt_correction_T_max 0.8748 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'rigaku saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 28834 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7051 _reflns_number_gt 6201 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalclear(Rigaku/MSC Inc., 2005)' _computing_cell_refinement crystalclear _computing_data_reduction crystalclear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+0.7373P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0088(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7051 _refine_ls_number_parameters 482 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0840 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.003 _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 0.14700(2) 0.389641(17) 0.244082(9) 0.01753(9) Uani 1 1 d . . . Cl1 Cl 0.05312(5) 0.52579(3) 0.212823(18) 0.02092(13) Uani 1 1 d . . . Cl2 Cl 0.15288(6) 0.31492(4) 0.17240(2) 0.03202(15) Uani 1 1 d . . . Cl3 Cl 0.07372(5) 0.26465(4) 0.28671(2) 0.02415(13) Uani 1 1 d . . . Cl4 Cl 0.26084(5) 0.45681(4) 0.30724(2) 0.02510(14) Uani 1 1 d . . . O1 O 0.60195(14) 0.32626(11) 0.45273(5) 0.0280(4) Uani 1 1 d . . . O2 O 0.44728(15) 0.28818(11) 0.03408(5) 0.0306(4) Uani 1 1 d . . . O3 O 0.43686(14) 0.51259(11) 0.09389(5) 0.0277(4) Uani 1 1 d . . . O4 O 0.77389(15) 0.49596(11) 0.51970(5) 0.0302(4) Uani 1 1 d . . . N1 N 0.79204(15) 0.25859(11) 0.24076(6) 0.0155(4) Uani 1 1 d D . . N2 N 0.83228(15) 0.51622(11) 0.28418(6) 0.0152(4) Uani 1 1 d D . . C1 C 0.68238(19) 0.20360(14) 0.26025(7) 0.0190(4) Uani 1 1 d . . . H1A H 0.6040 0.2135 0.2379 0.023 Uiso 1 1 calc R . . H1B H 0.7029 0.1347 0.2603 0.023 Uiso 1 1 calc R . . C2 C 0.65608(19) 0.23310(14) 0.31140(7) 0.0173(4) Uani 1 1 d . . . C3 C 0.54718(19) 0.28440(14) 0.31943(8) 0.0206(5) Uani 1 1 d . . . H3 H 0.4864 0.2979 0.2924 0.025 Uiso 1 1 calc R . . C4 C 0.5246(2) 0.31672(14) 0.36605(8) 0.0215(5) Uani 1 1 d . . . H4 H 0.4493 0.3521 0.3709 0.026 Uiso 1 1 calc R . . C5 C 0.6129(2) 0.29679(15) 0.40545(8) 0.0214(5) Uani 1 1 d . . . C6 C 0.7216(2) 0.24301(15) 0.39825(8) 0.0221(5) Uani 1 1 d . . . H6 H 0.7810 0.2278 0.4254 0.026 Uiso 1 1 calc R . . C7 C 0.74281(19) 0.21176(14) 0.35146(7) 0.0193(4) Uani 1 1 d . . . H7 H 0.8172 0.1754 0.3466 0.023 Uiso 1 1 calc R . . C8 C 0.4968(2) 0.38724(17) 0.46090(9) 0.0340(6) Uani 1 1 d . . . H8A H 0.4999 0.4440 0.4400 0.051 Uiso 1 1 calc R . . H8B H 0.5021 0.4065 0.4956 0.051 Uiso 1 1 calc R . . H8C H 0.4162 0.3532 0.4527 0.051 Uiso 1 1 calc R . . C9 C 0.82423(19) 0.21868(15) 0.19122(7) 0.0187(4) Uani 1 1 d . . . H9A H 0.9074 0.2454 0.1831 0.022 Uiso 1 1 calc R . . H9B H 0.8344 0.1487 0.1942 0.022 Uiso 1 1 calc R . . C10 C 0.72511(19) 0.23992(14) 0.14953(7) 0.0182(4) Uani 1 1 d . . . C11 C 0.61673(19) 0.18220(14) 0.14111(7) 0.0195(4) Uani 1 1 d . . . H11 H 0.6050 0.1296 0.1622 0.023 Uiso 1 1 calc R . . C12 C 0.5269(2) 0.20100(15) 0.10251(7) 0.0235(5) Uani 1 1 d . . . H12 H 0.4529 0.1618 0.0975 0.028 Uiso 1 1 calc R . . C13 C 0.5433(2) 0.27685(15) 0.07064(8) 0.0239(5) Uani 1 1 d . . . C14 C 0.6517(2) 0.33320(16) 0.07771(8) 0.0277(5) Uani 1 1 d . . . H14 H 0.6649 0.3843 0.0558 0.033 Uiso 1 1 calc R . . C15 C 0.7411(2) 0.31436(15) 0.11708(8) 0.0232(5) Uani 1 1 d . . . H15 H 0.8151 0.3535 0.1219 0.028 Uiso 1 1 calc R . . C16 C 0.4641(3) 0.35960(18) -0.00228(9) 0.0392(6) Uani 1 1 d . . . H16A H 0.4721 0.4222 0.0136 0.059 Uiso 1 1 calc R . . H16B H 0.3899 0.3596 -0.0267 0.059 Uiso 1 1 calc R . . H16C H 0.5419 0.3459 -0.0187 0.059 Uiso 1 1 calc R . . C17 C 0.77245(19) 0.36484(14) 0.23807(7) 0.0174(4) Uani 1 1 d . . . H17A H 0.6828 0.3785 0.2256 0.021 Uiso 1 1 calc R . . H17B H 0.8295 0.3923 0.2146 0.021 Uiso 1 1 calc R . . C18 C 0.8007(2) 0.41208(14) 0.28853(7) 0.0178(4) Uani 1 1 d . . . H18A H 0.7251 0.4051 0.3078 0.021 Uiso 1 1 calc R . . H18B H 0.8737 0.3790 0.3067 0.021 Uiso 1 1 calc R . . C19 C 0.71533(18) 0.57950(14) 0.27712(7) 0.0193(4) Uani 1 1 d . . . H19A H 0.6610 0.5691 0.3047 0.023 Uiso 1 1 calc R . . H19B H 0.7428 0.6470 0.2780 0.023 Uiso 1 1 calc R . . C20 C 0.63775(18) 0.56032(14) 0.22925(7) 0.0173(4) Uani 1 1 d . . . C21 C 0.52008(19) 0.51589(14) 0.22765(8) 0.0198(5) Uani 1 1 d . . . H21 H 0.4868 0.4974 0.2576 0.024 Uiso 1 1 calc R . . C22 C 0.44876(19) 0.49739(14) 0.18318(8) 0.0200(4) Uani 1 1 d . . . H22 H 0.3678 0.4668 0.1828 0.024 Uiso 1 1 calc R . . C23 C 0.49772(19) 0.52438(14) 0.13950(8) 0.0202(4) Uani 1 1 d . . . C24 C 0.6178(2) 0.56769(15) 0.14057(8) 0.0222(5) Uani 1 1 d . . . H24 H 0.6523 0.5849 0.1106 0.027 Uiso 1 1 calc R . . C25 C 0.68661(19) 0.58554(14) 0.18498(8) 0.0204(5) Uani 1 1 d . . . H25 H 0.7682 0.6153 0.1854 0.024 Uiso 1 1 calc R . . C26 C 0.3101(2) 0.47358(19) 0.09089(9) 0.0354(6) Uani 1 1 d . . . H26A H 0.3135 0.4079 0.1031 0.053 Uiso 1 1 calc R . . H26B H 0.2739 0.4743 0.0565 0.053 Uiso 1 1 calc R . . H26C H 0.2561 0.5119 0.1110 0.053 Uiso 1 1 calc R . . C27 C 0.92465(18) 0.54909(15) 0.32691(7) 0.0174(4) Uani 1 1 d . . . H27A H 1.0078 0.5165 0.3246 0.021 Uiso 1 1 calc R . . H27B H 0.9394 0.6183 0.3234 0.021 Uiso 1 1 calc R . . C28 C 0.88071(18) 0.53089(14) 0.37740(7) 0.0159(4) Uani 1 1 d . . . C29 C 0.80632(18) 0.59807(14) 0.39979(7) 0.0183(4) Uani 1 1 d . . . H29 H 0.7792 0.6542 0.3824 0.022 Uiso 1 1 calc R . . C30 C 0.77177(19) 0.58372(15) 0.44707(7) 0.0210(5) Uani 1 1 d . . . H30 H 0.7204 0.6296 0.4619 0.025 Uiso 1 1 calc R . . C31 C 0.81203(19) 0.50231(15) 0.47304(7) 0.0213(5) Uani 1 1 d . . . C32 C 0.8863(2) 0.43522(15) 0.45129(8) 0.0230(5) Uani 1 1 d . . . H32 H 0.9135 0.3792 0.4688 0.028 Uiso 1 1 calc R . . C33 C 0.92043(19) 0.45034(15) 0.40390(7) 0.0198(4) Uani 1 1 d . . . H33 H 0.9722 0.4045 0.3892 0.024 Uiso 1 1 calc R . . C34 C 0.8123(2) 0.41318(18) 0.54791(8) 0.0356(6) Uani 1 1 d . . . H34A H 0.7737 0.3564 0.5318 0.053 Uiso 1 1 calc R . . H34B H 0.7837 0.4190 0.5811 0.053 Uiso 1 1 calc R . . H34C H 0.9059 0.4075 0.5501 0.053 Uiso 1 1 calc R . . C35 C 0.0814(2) 0.19346(19) 0.50595(9) 0.0371(6) Uani 1 1 d . . . H35 H 0.0870 0.2263 0.5366 0.045 Uiso 1 1 calc R . . C36 C 0.1132(2) 0.2395(2) 0.46529(9) 0.0395(6) Uani 1 1 d . . . H36 H 0.1419 0.3037 0.4676 0.047 Uiso 1 1 calc R . . C37 C 0.1038(2) 0.1922(2) 0.41888(9) 0.0381(6) Uani 1 1 d . . . H37 H 0.1251 0.2255 0.3903 0.046 Uiso 1 1 calc R . . C38 C 0.0651(2) 0.1008(2) 0.41514(9) 0.0359(6) Uani 1 1 d . . . H38 H 0.0594 0.0705 0.3838 0.043 Uiso 1 1 calc R . . C39 C 0.0322(2) 0.04831(18) 0.45719(8) 0.0308(6) Uani 1 1 d . . . C40 C 0.0395(2) 0.09633(18) 0.50409(8) 0.0311(6) Uani 1 1 d . . . C41 C 0.0069(2) 0.04694(19) 0.54554(9) 0.0336(6) Uani 1 1 d . . . H41 H 0.0113 0.0787 0.5764 0.040 Uiso 1 1 calc R . . H1 H 0.8648(13) 0.2467(16) 0.2599(6) 0.021(6) Uiso 1 1 d D . . H2 H 0.8770(18) 0.5243(16) 0.2577(6) 0.027(6) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01888(15) 0.01198(14) 0.02202(15) 0.00054(10) 0.00347(10) -0.00033(10) Cl1 0.0240(3) 0.0179(3) 0.0215(3) 0.0053(2) 0.0058(2) 0.0044(2) Cl2 0.0486(4) 0.0194(3) 0.0300(3) -0.0061(2) 0.0146(3) -0.0047(2) Cl3 0.0199(3) 0.0197(3) 0.0322(3) 0.0105(2) -0.0015(2) -0.0027(2) Cl4 0.0237(3) 0.0207(3) 0.0298(3) -0.0005(2) -0.0042(2) -0.0012(2) O1 0.0322(9) 0.0318(9) 0.0208(8) -0.0049(7) 0.0082(6) 0.0018(7) O2 0.0397(10) 0.0308(9) 0.0196(8) 0.0045(7) -0.0075(7) 0.0015(7) O3 0.0232(8) 0.0358(9) 0.0231(8) -0.0007(7) -0.0041(6) -0.0073(7) O4 0.0340(9) 0.0394(10) 0.0176(8) 0.0091(7) 0.0046(7) -0.0015(7) N1 0.0143(9) 0.0139(9) 0.0184(9) -0.0018(7) 0.0014(7) 0.0014(7) N2 0.0167(9) 0.0132(8) 0.0161(9) -0.0021(7) 0.0030(7) -0.0015(7) C1 0.0186(11) 0.0162(10) 0.0226(11) -0.0023(8) 0.0040(8) -0.0048(8) C2 0.0188(11) 0.0122(10) 0.0216(11) -0.0011(8) 0.0046(8) -0.0042(8) C3 0.0179(11) 0.0191(11) 0.0247(12) 0.0025(9) 0.0012(8) -0.0032(9) C4 0.0190(11) 0.0186(11) 0.0276(12) -0.0007(9) 0.0064(9) 0.0009(9) C5 0.0255(12) 0.0185(11) 0.0213(11) -0.0029(9) 0.0081(9) -0.0042(9) C6 0.0226(11) 0.0211(11) 0.0223(11) 0.0026(9) 0.0006(9) -0.0013(9) C7 0.0204(11) 0.0143(10) 0.0239(11) 0.0008(8) 0.0049(9) 0.0010(8) C8 0.0434(15) 0.0297(13) 0.0312(14) -0.0064(10) 0.0163(11) 0.0072(11) C9 0.0191(11) 0.0186(10) 0.0190(11) -0.0061(8) 0.0050(8) 0.0021(9) C10 0.0187(11) 0.0181(10) 0.0186(11) -0.0056(8) 0.0061(8) -0.0004(8) C11 0.0222(11) 0.0172(10) 0.0194(11) -0.0017(8) 0.0037(8) -0.0014(9) C12 0.0243(12) 0.0239(12) 0.0222(12) -0.0014(9) 0.0014(9) -0.0036(9) C13 0.0310(13) 0.0233(11) 0.0172(11) -0.0023(9) 0.0004(9) 0.0039(10) C14 0.0422(14) 0.0209(12) 0.0203(12) 0.0018(9) 0.0054(10) -0.0018(10) C15 0.0277(12) 0.0214(11) 0.0207(11) -0.0033(9) 0.0040(9) -0.0064(9) C16 0.0630(18) 0.0307(14) 0.0222(13) 0.0068(11) -0.0075(11) 0.0049(13) C17 0.0216(11) 0.0128(10) 0.0179(10) -0.0016(8) 0.0015(8) 0.0005(8) C18 0.0214(11) 0.0121(10) 0.0199(11) -0.0015(8) 0.0019(8) -0.0020(8) C19 0.0212(11) 0.0162(10) 0.0203(11) -0.0006(8) 0.0008(8) 0.0042(9) C20 0.0193(11) 0.0121(10) 0.0200(11) -0.0006(8) -0.0010(8) 0.0040(8) C21 0.0183(11) 0.0183(11) 0.0234(11) 0.0033(9) 0.0059(9) 0.0044(9) C22 0.0129(10) 0.0192(11) 0.0280(12) 0.0011(9) 0.0018(8) -0.0004(8) C23 0.0184(11) 0.0183(11) 0.0228(11) -0.0007(9) -0.0038(8) 0.0019(9) C24 0.0235(12) 0.0240(11) 0.0192(11) 0.0029(9) 0.0026(9) -0.0053(9) C25 0.0176(11) 0.0177(10) 0.0257(12) 0.0030(9) 0.0007(9) -0.0043(9) C26 0.0225(13) 0.0484(16) 0.0341(14) -0.0105(12) -0.0050(10) -0.0097(11) C27 0.0144(10) 0.0204(11) 0.0172(10) -0.0030(8) -0.0002(8) -0.0023(8) C28 0.0132(10) 0.0173(10) 0.0169(10) -0.0022(8) 0.0000(8) -0.0052(8) C29 0.0189(11) 0.0172(10) 0.0182(11) 0.0006(8) -0.0012(8) -0.0004(8) C30 0.0205(11) 0.0240(11) 0.0184(11) -0.0007(9) 0.0016(8) 0.0046(9) C31 0.0183(11) 0.0285(12) 0.0167(11) 0.0026(9) -0.0002(8) -0.0061(9) C32 0.0256(12) 0.0186(11) 0.0239(12) 0.0050(9) -0.0041(9) -0.0014(9) C33 0.0190(11) 0.0190(11) 0.0208(11) -0.0035(9) -0.0021(8) 0.0003(9) C34 0.0394(14) 0.0433(15) 0.0231(13) 0.0137(11) -0.0034(10) -0.0098(12) C35 0.0321(14) 0.0453(16) 0.0328(14) -0.0155(12) -0.0040(11) 0.0120(12) C36 0.0319(14) 0.0445(16) 0.0409(16) -0.0048(12) -0.0046(11) 0.0133(12) C37 0.0310(14) 0.0517(17) 0.0305(14) -0.0001(12) -0.0034(10) 0.0125(12) C38 0.0287(13) 0.0563(18) 0.0219(13) -0.0085(11) -0.0029(10) 0.0118(12) C39 0.0179(12) 0.0436(15) 0.0297(13) -0.0107(11) -0.0049(9) 0.0123(10) C40 0.0204(12) 0.0462(15) 0.0255(13) -0.0083(11) -0.0049(9) 0.0116(11) C41 0.0220(12) 0.0494(16) 0.0285(13) -0.0159(11) -0.0033(10) 0.0119(11) _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 Cl4 2.2194(8) . ? Cu1 Cl2 2.2215(7) . ? Cu1 Cl3 2.2720(6) . ? Cu1 Cl1 2.2806(7) . ? O1 C5 1.367(2) . ? O1 C8 1.427(3) . ? O2 C13 1.364(3) . ? O2 C16 1.430(3) . ? O3 C23 1.358(2) . ? O3 C26 1.432(3) . ? O4 C31 1.367(2) . ? O4 C34 1.432(3) . ? N1 C17 1.506(2) . ? N1 C1 1.516(2) . ? N1 C9 1.525(2) . ? N1 H1 0.902(9) . ? N2 C18 1.505(2) . ? N2 C19 1.512(2) . ? N2 C27 1.521(2) . ? N2 H2 0.899(9) . ? C1 C2 1.501(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.381(3) . ? C2 C7 1.393(3) . ? C3 C4 1.387(3) . ? C3 H3 0.9500 . ? C4 C5 1.385(3) . ? C4 H4 0.9500 . ? C5 C6 1.393(3) . ? C6 C7 1.383(3) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.503(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C15 1.387(3) . ? C10 C11 1.398(3) . ? C11 C12 1.376(3) . ? C11 H11 0.9500 . ? C12 C13 1.393(3) . ? C12 H12 0.9500 . ? C13 C14 1.384(3) . ? C14 C15 1.388(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.532(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.502(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.378(3) . ? C20 C25 1.395(3) . ? C21 C22 1.393(3) . ? C21 H21 0.9500 . ? C22 C23 1.387(3) . ? C22 H22 0.9500 . ? C23 C24 1.395(3) . ? C24 C25 1.378(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.508(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C33 1.386(3) . ? C28 C29 1.395(3) . ? C29 C30 1.381(3) . ? C29 H29 0.9500 . ? C30 C31 1.390(3) . ? C30 H30 0.9500 . ? C31 C32 1.385(3) . ? C32 C33 1.384(3) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.347(4) . ? C35 C40 1.432(4) . ? C35 H35 0.9500 . ? C36 C37 1.424(3) . ? C36 H36 0.9500 . ? C37 C38 1.347(4) . ? C37 H37 0.9500 . ? C38 C39 1.427(3) . ? C38 H38 0.9500 . ? C39 C41 1.398(4) 3_556 ? C39 C40 1.441(3) . ? C40 C41 1.391(3) . ? C41 C39 1.398(4) 3_556 ? C41 H41 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl4 Cu1 Cl2 146.01(3) . . ? Cl4 Cu1 Cl3 96.55(2) . . ? Cl2 Cu1 Cl3 96.90(3) . . ? Cl4 Cu1 Cl1 96.92(3) . . ? Cl2 Cu1 Cl1 96.31(3) . . ? Cl3 Cu1 Cl1 133.16(2) . . ? C5 O1 C8 117.08(18) . . ? C13 O2 C16 117.46(18) . . ? C23 O3 C26 117.42(17) . . ? C31 O4 C34 117.46(18) . . ? C17 N1 C1 114.64(15) . . ? C17 N1 C9 111.11(15) . . ? C1 N1 C9 110.68(15) . . ? C17 N1 H1 108.4(14) . . ? C1 N1 H1 109.3(13) . . ? C9 N1 H1 101.8(13) . . ? C18 N2 C19 113.53(15) . . ? C18 N2 C27 111.33(15) . . ? C19 N2 C27 112.07(15) . . ? C18 N2 H2 108.5(15) . . ? C19 N2 H2 107.1(14) . . ? C27 N2 H2 103.6(14) . . ? C2 C1 N1 112.84(16) . . ? C2 C1 H1A 109.0 . . ? N1 C1 H1A 109.0 . . ? C2 C1 H1B 109.0 . . ? N1 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? C3 C2 C7 118.74(18) . . ? C3 C2 C1 120.58(19) . . ? C7 C2 C1 120.65(18) . . ? C2 C3 C4 121.4(2) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C5 C4 C3 119.27(19) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? O1 C5 C4 124.43(18) . . ? O1 C5 C6 115.50(19) . . ? C4 C5 C6 120.06(19) . . ? C7 C6 C5 119.8(2) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C2 120.63(19) . . ? C6 C7 H7 119.7 . . ? C2 C7 H7 119.7 . . ? O1 C8 H8A 109.5 . . ? O1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 N1 113.95(15) . . ? C10 C9 H9A 108.8 . . ? N1 C9 H9A 108.8 . . ? C10 C9 H9B 108.8 . . ? N1 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C15 C10 C11 118.1(2) . . ? C15 C10 C9 121.21(18) . . ? C11 C10 C9 120.60(18) . . ? C12 C11 C10 120.53(19) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C13 120.7(2) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? O2 C13 C14 125.5(2) . . ? O2 C13 C12 114.98(19) . . ? C14 C13 C12 119.5(2) . . ? C13 C14 C15 119.4(2) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C10 C15 C14 121.7(2) . . ? C10 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? O2 C16 H16A 109.5 . . ? O2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 C17 C18 111.68(16) . . ? N1 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? N1 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 107.9 . . ? N2 C18 C17 112.12(16) . . ? N2 C18 H18A 109.2 . . ? C17 C18 H18A 109.2 . . ? N2 C18 H18B 109.2 . . ? C17 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? C20 C19 N2 112.26(16) . . ? C20 C19 H19A 109.2 . . ? N2 C19 H19A 109.2 . . ? C20 C19 H19B 109.2 . . ? N2 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? C21 C20 C25 118.63(19) . . ? C21 C20 C19 121.72(18) . . ? C25 C20 C19 119.63(18) . . ? C20 C21 C22 121.63(19) . . ? C20 C21 H21 119.2 . . ? C22 C21 H21 119.2 . . ? C23 C22 C21 119.03(19) . . ? C23 C22 H22 120.5 . . ? C21 C22 H22 120.5 . . ? O3 C23 C22 124.93(19) . . ? O3 C23 C24 115.16(18) . . ? C22 C23 C24 119.90(19) . . ? C25 C24 C23 120.09(19) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C20 120.70(19) . . ? C24 C25 H25 119.7 . . ? C20 C25 H25 119.7 . . ? O3 C26 H26A 109.5 . . ? O3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 N2 115.05(15) . . ? C28 C27 H27A 108.5 . . ? N2 C27 H27A 108.5 . . ? C28 C27 H27B 108.5 . . ? N2 C27 H27B 108.5 . . ? H27A C27 H27B 107.5 . . ? C33 C28 C29 118.52(18) . . ? C33 C28 C27 120.79(18) . . ? C29 C28 C27 120.55(18) . . ? C30 C29 C28 120.56(19) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C31 120.14(19) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? O4 C31 C32 124.86(19) . . ? O4 C31 C30 115.28(19) . . ? C32 C31 C30 119.86(18) . . ? C33 C32 C31 119.5(2) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C32 C33 C28 121.39(19) . . ? C32 C33 H33 119.3 . . ? C28 C33 H33 119.3 . . ? O4 C34 H34A 109.5 . . ? O4 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O4 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C40 121.5(2) . . ? C36 C35 H35 119.2 . . ? C40 C35 H35 119.2 . . ? C35 C36 C37 120.2(3) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C38 C37 C36 120.6(2) . . ? C38 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? C37 C38 C39 121.5(2) . . ? C37 C38 H38 119.3 . . ? C39 C38 H38 119.3 . . ? C41 C39 C38 122.7(2) 3_556 . ? C41 C39 C40 119.2(2) 3_556 . ? C38 C39 C40 118.2(2) . . ? C41 C40 C35 122.7(2) . . ? C41 C40 C39 119.2(2) . . ? C35 C40 C39 118.0(2) . . ? C40 C41 C39 121.6(2) . 3_556 ? C40 C41 H41 119.2 . . ? C39 C41 H41 119.2 3_556 . ? 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 C17 N1 C1 C2 -59.5(2) . . . . ? C9 N1 C1 C2 173.83(16) . . . . ? N1 C1 C2 C3 108.5(2) . . . . ? N1 C1 C2 C7 -69.5(2) . . . . ? C7 C2 C3 C4 1.6(3) . . . . ? C1 C2 C3 C4 -176.50(18) . . . . ? C2 C3 C4 C5 -0.2(3) . . . . ? C8 O1 C5 C4 -4.7(3) . . . . ? C8 O1 C5 C6 175.57(19) . . . . ? C3 C4 C5 O1 178.82(19) . . . . ? C3 C4 C5 C6 -1.4(3) . . . . ? O1 C5 C6 C7 -178.50(18) . . . . ? C4 C5 C6 C7 1.7(3) . . . . ? C5 C6 C7 C2 -0.4(3) . . . . ? C3 C2 C7 C6 -1.3(3) . . . . ? C1 C2 C7 C6 176.80(18) . . . . ? C17 N1 C9 C10 -57.2(2) . . . . ? C1 N1 C9 C10 71.4(2) . . . . ? N1 C9 C10 C15 99.2(2) . . . . ? N1 C9 C10 C11 -83.8(2) . . . . ? C15 C10 C11 C12 -2.0(3) . . . . ? C9 C10 C11 C12 -179.12(17) . . . . ? C10 C11 C12 C13 1.1(3) . . . . ? C16 O2 C13 C14 5.0(3) . . . . ? C16 O2 C13 C12 -174.68(19) . . . . ? C11 C12 C13 O2 -179.67(18) . . . . ? C11 C12 C13 C14 0.6(3) . . . . ? O2 C13 C14 C15 178.97(19) . . . . ? C12 C13 C14 C15 -1.3(3) . . . . ? C11 C10 C15 C14 1.2(3) . . . . ? C9 C10 C15 C14 178.36(18) . . . . ? C13 C14 C15 C10 0.4(3) . . . . ? C1 N1 C17 C18 79.6(2) . . . . ? C9 N1 C17 C18 -154.03(16) . . . . ? C19 N2 C18 C17 82.97(19) . . . . ? C27 N2 C18 C17 -149.44(16) . . . . ? N1 C17 C18 N2 157.62(16) . . . . ? C18 N2 C19 C20 -64.7(2) . . . . ? C27 N2 C19 C20 168.14(15) . . . . ? N2 C19 C20 C21 108.7(2) . . . . ? N2 C19 C20 C25 -69.6(2) . . . . ? C25 C20 C21 C22 -1.1(3) . . . . ? C19 C20 C21 C22 -179.42(18) . . . . ? C20 C21 C22 C23 0.1(3) . . . . ? C26 O3 C23 C22 3.2(3) . . . . ? C26 O3 C23 C24 -176.44(19) . . . . ? C21 C22 C23 O3 -178.38(19) . . . . ? C21 C22 C23 C24 1.2(3) . . . . ? O3 C23 C24 C25 178.23(19) . . . . ? C22 C23 C24 C25 -1.4(3) . . . . ? C23 C24 C25 C20 0.3(3) . . . . ? C21 C20 C25 C24 0.9(3) . . . . ? C19 C20 C25 C24 179.26(19) . . . . ? C18 N2 C27 C28 -55.6(2) . . . . ? C19 N2 C27 C28 72.7(2) . . . . ? N2 C27 C28 C33 95.8(2) . . . . ? N2 C27 C28 C29 -88.6(2) . . . . ? C33 C28 C29 C30 -0.9(3) . . . . ? C27 C28 C29 C30 -176.55(18) . . . . ? C28 C29 C30 C31 0.6(3) . . . . ? C34 O4 C31 C32 -0.8(3) . . . . ? C34 O4 C31 C30 179.68(19) . . . . ? C29 C30 C31 O4 179.13(18) . . . . ? C29 C30 C31 C32 -0.4(3) . . . . ? O4 C31 C32 C33 -179.03(19) . . . . ? C30 C31 C32 C33 0.5(3) . . . . ? C31 C32 C33 C28 -0.7(3) . . . . ? C29 C28 C33 C32 0.9(3) . . . . ? C27 C28 C33 C32 176.60(18) . . . . ? C40 C35 C36 C37 0.9(4) . . . . ? C35 C36 C37 C38 -1.0(4) . . . . ? C36 C37 C38 C39 0.0(4) . . . . ? C37 C38 C39 C41 -179.3(2) . . . 3_556 ? C37 C38 C39 C40 1.1(3) . . . . ? C36 C35 C40 C41 179.6(2) . . . . ? C36 C35 C40 C39 0.1(3) . . . . ? C41 C39 C40 C41 -0.2(3) 3_556 . . . ? C38 C39 C40 C41 179.44(19) . . . . ? C41 C39 C40 C35 179.2(2) 3_556 . . . ? C38 C39 C40 C35 -1.1(3) . . . . ? C35 C40 C41 C39 -179.2(2) . . . 3_556 ? C39 C40 C41 C39 0.3(4) . . . 3_556 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 Cl3 0.902(9) 2.262(12) 3.1075(19) 156.0(18) 1_655 N2 H2 Cl1 0.899(9) 2.297(12) 3.1457(18) 157.4(19) 1_655 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.325 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.063 # Attachment '- CRYSTAL3.CIF' data_CRYSTAL3 _database_code_depnum_ccdc_archive 'CCDC 825596' #TrackingRef '- CRYSTAL3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H47 Cl4 Cu N2 O4' _chemical_formula_weight 837.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 10.467(2) _cell_length_b 14.108(3) _cell_length_c 27.330(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.29(3) _cell_angle_gamma 90.00 _cell_volume 4018.6(14) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 0.852 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8480 _exptl_absorpt_correction_T_max 0.9046 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'rigaku saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 29666 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7075 _reflns_number_gt 6457 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0466P)^2^+3.1118P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0165(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7075 _refine_ls_number_parameters 490 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0835 _refine_ls_wR_factor_gt 0.0810 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _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 0.64770(2) 0.387969(15) 0.249184(9) 0.02116(10) Uani 1 1 d U . . Cl1 Cl 0.66125(6) 0.31033(4) 0.17917(2) 0.03902(16) Uani 1 1 d . . . Cl2 Cl 0.55084(5) 0.52100(3) 0.215194(17) 0.02434(13) Uani 1 1 d . . . Cl3 Cl 0.75976(5) 0.45907(3) 0.31156(2) 0.03008(13) Uani 1 1 d . . . Cl4 Cl 0.57243(5) 0.26628(3) 0.29323(2) 0.03090(14) Uani 1 1 d . . . O1 O 0.89952(15) 0.82429(11) 0.04710(5) 0.0326(3) Uani 1 1 d . . . O2 O 1.05418(17) 0.78851(12) 0.46561(6) 0.0397(4) Uani 1 1 d . . . O3 O 1.06679(14) 1.01159(11) 0.40540(5) 0.0319(3) Uani 1 1 d . . . O4 O 0.72621(16) 0.99339(12) -0.02066(5) 0.0386(4) Uani 1 1 d . . . N1 N 0.70752(15) 0.75848(11) 0.25781(6) 0.0182(3) Uani 1 1 d D . . N2 N 0.67057(14) 1.01492(10) 0.21426(6) 0.0166(3) Uani 1 1 d D . . C1 C 1.0044(3) 0.88595(17) 0.03956(9) 0.0412(6) Uani 1 1 d . . . H1D H 1.0024 0.9020 0.0046 0.062 Uiso 1 1 calc R . . H1B H 1.0854 0.8541 0.0502 0.062 Uiso 1 1 calc R . . H1C H 0.9971 0.9441 0.0588 0.062 Uiso 1 1 calc R . . C2 C 0.8882(2) 0.79496(14) 0.09420(7) 0.0250(4) Uani 1 1 d . . . C3 C 0.7794(2) 0.74092(14) 0.10083(8) 0.0256(4) Uani 1 1 d . . . H3A H 0.7204 0.7255 0.0735 0.031 Uiso 1 1 calc R . . C4 C 0.75757(19) 0.70991(13) 0.14722(7) 0.0238(4) Uani 1 1 d . . . H4A H 0.6833 0.6734 0.1516 0.029 Uiso 1 1 calc R . . C5 C 0.84362(18) 0.73168(13) 0.18784(7) 0.0209(4) Uani 1 1 d . . . C6 C 0.95327(19) 0.78277(13) 0.18052(7) 0.0230(4) Uani 1 1 d . . . H6A H 1.0138 0.7961 0.2077 0.028 Uiso 1 1 calc R . . C7 C 0.97625(19) 0.81501(14) 0.13393(8) 0.0254(4) Uani 1 1 d . . . H7A H 1.0515 0.8504 0.1294 0.031 Uiso 1 1 calc R . . C8 C 0.81606(19) 0.70254(13) 0.23865(7) 0.0227(4) Uani 1 1 d . . . H8A H 0.8946 0.7112 0.2613 0.027 Uiso 1 1 calc R . . H8B H 0.7938 0.6343 0.2384 0.027 Uiso 1 1 calc R . . C9 C 0.67587(18) 0.71969(13) 0.30747(7) 0.0220(4) Uani 1 1 d . . . H9A H 0.5930 0.7468 0.3154 0.026 Uiso 1 1 calc R . . H9B H 0.6651 0.6501 0.3048 0.026 Uiso 1 1 calc R . . C10 C 0.77589(18) 0.74094(13) 0.34915(7) 0.0211(4) Uani 1 1 d . . . C11 C 0.88428(19) 0.68308(14) 0.35822(7) 0.0234(4) Uani 1 1 d . . . H11A H 0.8958 0.6305 0.3374 0.028 Uiso 1 1 calc R . . C12 C 0.9743(2) 0.70168(15) 0.39704(7) 0.0284(5) Uani 1 1 d . . . H12A H 1.0480 0.6624 0.4024 0.034 Uiso 1 1 calc R . . C13 C 0.9585(2) 0.77751(15) 0.42849(8) 0.0294(5) Uani 1 1 d . . . C14 C 0.8509(2) 0.83438(15) 0.42073(8) 0.0334(5) Uani 1 1 d . . . H14A H 0.8385 0.8858 0.4422 0.040 Uiso 1 1 calc R . . C15 C 0.7610(2) 0.81567(14) 0.38115(8) 0.0292(5) Uani 1 1 d . . . H15A H 0.6874 0.8551 0.3759 0.035 Uiso 1 1 calc R . . C16 C 1.0377(3) 0.85988(18) 0.50173(9) 0.0492(7) Uani 1 1 d . . . H16A H 1.1126 0.8604 0.5261 0.074 Uiso 1 1 calc R . . H16B H 0.9604 0.8461 0.5181 0.074 Uiso 1 1 calc R . . H16C H 1.0289 0.9220 0.4857 0.074 Uiso 1 1 calc R . . C17 C 0.72941(18) 0.86398(12) 0.26036(7) 0.0195(4) Uani 1 1 d . . . H17A H 0.8197 0.8766 0.2728 0.023 Uiso 1 1 calc R . . H17B H 0.6735 0.8921 0.2838 0.023 Uiso 1 1 calc R . . C18 C 0.70081(19) 0.91125(13) 0.20978(7) 0.0202(4) Uani 1 1 d . . . H18A H 0.7761 0.9038 0.1907 0.024 Uiso 1 1 calc R . . H18B H 0.6271 0.8789 0.1916 0.024 Uiso 1 1 calc R . . C19 C 1.1931(2) 0.97156(18) 0.40851(9) 0.0396(6) Uani 1 1 d . . . H19A H 1.2268 0.9665 0.4431 0.059 Uiso 1 1 calc R . . H19B H 1.2495 1.0124 0.3910 0.059 Uiso 1 1 calc R . . H19C H 1.1895 0.9084 0.3935 0.059 Uiso 1 1 calc R . . C20 C 1.00558(19) 1.02310(14) 0.35951(7) 0.0241(4) Uani 1 1 d . . . C21 C 0.8867(2) 1.06792(15) 0.35780(8) 0.0270(4) Uani 1 1 d . . . H21A H 0.8527 1.0863 0.3874 0.032 Uiso 1 1 calc R . . C22 C 0.81851(19) 1.08566(14) 0.31320(8) 0.0242(4) Uani 1 1 d . . . H22A H 0.7379 1.1169 0.3123 0.029 Uiso 1 1 calc R . . C23 C 0.86606(18) 1.05843(13) 0.26923(7) 0.0199(4) Uani 1 1 d . . . C24 C 0.98399(18) 1.01252(13) 0.27132(7) 0.0218(4) Uani 1 1 d . . . H24A H 1.0174 0.9932 0.2417 0.026 Uiso 1 1 calc R . . C25 C 1.05395(18) 0.99439(13) 0.31624(8) 0.0235(4) Uani 1 1 d . . . H25A H 1.1342 0.9626 0.3173 0.028 Uiso 1 1 calc R . . C26 C 0.78863(18) 1.07712(13) 0.22116(7) 0.0229(4) Uani 1 1 d . . . H26A H 0.8428 1.0656 0.1939 0.027 Uiso 1 1 calc R . . H26B H 0.7621 1.1445 0.2198 0.027 Uiso 1 1 calc R . . C27 C 0.57732(17) 1.04865(13) 0.17128(7) 0.0202(4) Uani 1 1 d . . . H27A H 0.4937 1.0169 0.1734 0.024 Uiso 1 1 calc R . . H27B H 0.5635 1.1176 0.1748 0.024 Uiso 1 1 calc R . . C28 C 0.62058(17) 1.03030(13) 0.12131(7) 0.0185(4) Uani 1 1 d . . . C29 C 0.69422(18) 1.09684(14) 0.09844(7) 0.0220(4) Uani 1 1 d . . . H29A H 0.7215 1.1530 0.1155 0.026 Uiso 1 1 calc R . . C30 C 0.72785(19) 1.08214(15) 0.05134(7) 0.0261(4) Uani 1 1 d . . . H30A H 0.7782 1.1280 0.0364 0.031 Uiso 1 1 calc R . . C31 C 0.68815(19) 1.00026(15) 0.02562(7) 0.0268(4) Uani 1 1 d . . . C32 C 0.6141(2) 0.93415(15) 0.04759(8) 0.0291(5) Uani 1 1 d . . . H32A H 0.5864 0.8783 0.0303 0.035 Uiso 1 1 calc R . . C33 C 0.58029(19) 0.94952(14) 0.09487(7) 0.0249(4) Uani 1 1 d . . . H33A H 0.5287 0.9041 0.1095 0.030 Uiso 1 1 calc R . . C34 C 0.6878(3) 0.9103(2) -0.04870(9) 0.0468(7) Uani 1 1 d . . . H34A H 0.7213 0.9139 -0.0810 0.070 Uiso 1 1 calc R . . H34B H 0.5940 0.9067 -0.0529 0.070 Uiso 1 1 calc R . . H34C H 0.7222 0.8538 -0.0313 0.070 Uiso 1 1 calc R . . C35 C 0.5035(5) 0.9559(4) 0.41981(17) 0.0420(13) Uani 0.50 1 d P . . H35A H 0.510(6) 0.955(5) 0.394(2) 0.063 Uiso 0.50 1 d P . . C36 C 0.4688(4) 0.8765(3) 0.44456(18) 0.0354(11) Uani 0.50 1 d P . . H36A H 0.4531 0.8200 0.4260 0.043 Uiso 0.50 1 calc PR . . C37 C 0.4567(3) 0.8728(2) 0.48817(14) 0.0601(9) Uani 1 1 d . . . C38 C 0.4177(3) 0.7916(2) 0.51472(17) 0.0728(11) Uani 1 1 d . . . H38A H 0.3994 0.7338 0.4977 0.087 Uiso 1 1 calc R . . C39 C 0.4064(3) 0.7965(3) 0.56449(16) 0.0707(10) Uani 1 1 d . . . H39A H 0.3805 0.7422 0.5816 0.085 Uiso 1 1 calc R . . C40 C 0.4324(3) 0.8789(2) 0.58897(15) 0.0687(10) Uani 1 1 d . . . H40A H 0.4254 0.8813 0.6234 0.082 Uiso 1 1 calc R . . C41 C 0.4687(3) 0.9592(2) 0.56503(16) 0.0664(9) Uani 1 1 d . . . C42 C 0.4811(2) 0.95775(19) 0.51380(16) 0.0634(10) Uani 1 1 d . . . H1A H 0.6354(14) 0.7490(17) 0.2379(7) 0.031(6) Uiso 1 1 d D . . H2A H 0.6236(17) 1.0232(14) 0.2395(5) 0.016(5) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01967(14) 0.01283(13) 0.03144(16) 0.00073(9) 0.00480(10) -0.00040(9) Cl1 0.0558(4) 0.0210(3) 0.0430(3) -0.0087(2) 0.0190(3) -0.0044(2) Cl2 0.0277(3) 0.0197(2) 0.0266(3) 0.00569(18) 0.0077(2) 0.00528(19) Cl3 0.0258(3) 0.0243(3) 0.0388(3) -0.0001(2) -0.0043(2) -0.0013(2) Cl4 0.0207(2) 0.0230(2) 0.0479(3) 0.0158(2) -0.0026(2) -0.00321(19) O1 0.0360(8) 0.0369(8) 0.0258(8) 0.0053(6) 0.0084(6) -0.0010(7) O2 0.0503(10) 0.0413(9) 0.0253(8) -0.0041(7) -0.0087(7) -0.0039(8) O3 0.0266(8) 0.0428(9) 0.0251(8) 0.0011(6) -0.0046(6) 0.0057(7) O4 0.0380(9) 0.0564(10) 0.0215(8) -0.0120(7) 0.0039(7) 0.0039(8) N1 0.0162(8) 0.0162(7) 0.0220(8) 0.0040(6) 0.0008(7) -0.0014(6) N2 0.0169(8) 0.0162(7) 0.0170(8) 0.0026(6) 0.0024(6) 0.0019(6) C1 0.0484(15) 0.0392(13) 0.0388(14) 0.0083(10) 0.0184(12) -0.0051(11) C2 0.0284(11) 0.0221(10) 0.0255(10) -0.0003(8) 0.0077(9) 0.0042(8) C3 0.0254(10) 0.0241(10) 0.0271(11) -0.0034(8) 0.0013(8) -0.0005(8) C4 0.0212(10) 0.0189(9) 0.0317(11) -0.0007(8) 0.0053(8) -0.0017(8) C5 0.0212(10) 0.0154(9) 0.0265(10) 0.0005(7) 0.0036(8) 0.0038(7) C6 0.0195(10) 0.0228(10) 0.0267(10) -0.0022(8) 0.0011(8) 0.0029(8) C7 0.0201(10) 0.0232(10) 0.0339(12) 0.0010(8) 0.0079(8) -0.0012(8) C8 0.0214(10) 0.0184(9) 0.0288(11) 0.0032(8) 0.0051(8) 0.0047(8) C9 0.0189(9) 0.0215(9) 0.0264(10) 0.0093(8) 0.0058(8) -0.0013(8) C10 0.0221(10) 0.0210(9) 0.0207(10) 0.0073(7) 0.0042(8) -0.0005(8) C11 0.0266(10) 0.0208(9) 0.0228(10) 0.0010(8) 0.0027(8) 0.0022(8) C12 0.0275(11) 0.0308(11) 0.0267(11) 0.0023(9) 0.0014(9) 0.0054(9) C13 0.0377(12) 0.0279(11) 0.0221(10) 0.0033(8) 0.0001(9) -0.0042(9) C14 0.0511(14) 0.0251(11) 0.0246(11) -0.0025(9) 0.0057(10) 0.0036(10) C15 0.0352(12) 0.0254(10) 0.0281(11) 0.0041(8) 0.0082(9) 0.0089(9) C16 0.077(2) 0.0410(14) 0.0276(13) -0.0069(11) -0.0079(12) -0.0086(14) C17 0.0212(10) 0.0136(8) 0.0233(10) 0.0031(7) 0.0006(8) 0.0001(7) C18 0.0240(10) 0.0145(9) 0.0222(10) 0.0017(7) 0.0014(8) 0.0003(8) C19 0.0260(11) 0.0521(15) 0.0385(13) 0.0070(11) -0.0088(10) 0.0072(11) C20 0.0228(10) 0.0215(9) 0.0271(11) 0.0006(8) -0.0030(8) -0.0012(8) C21 0.0263(11) 0.0291(11) 0.0257(11) -0.0063(8) 0.0034(8) 0.0049(9) C22 0.0203(10) 0.0207(9) 0.0316(11) -0.0032(8) 0.0014(8) 0.0043(8) C23 0.0197(9) 0.0154(9) 0.0243(10) 0.0013(7) 0.0002(8) -0.0032(7) C24 0.0199(10) 0.0199(9) 0.0262(10) -0.0027(8) 0.0053(8) -0.0051(8) C25 0.0159(9) 0.0224(10) 0.0322(11) 0.0001(8) 0.0018(8) 0.0007(8) C26 0.0232(10) 0.0187(9) 0.0265(11) 0.0041(8) 0.0005(8) -0.0048(8) C27 0.0158(9) 0.0224(9) 0.0221(10) 0.0058(8) -0.0001(8) 0.0044(8) C28 0.0153(9) 0.0205(9) 0.0193(9) 0.0021(7) -0.0012(7) 0.0036(7) C29 0.0223(10) 0.0219(9) 0.0215(10) -0.0010(8) 0.0002(8) -0.0017(8) C30 0.0227(10) 0.0329(11) 0.0228(10) 0.0018(8) 0.0025(8) -0.0032(9) C31 0.0223(10) 0.0380(12) 0.0198(10) -0.0044(9) -0.0008(8) 0.0069(9) C32 0.0339(12) 0.0242(10) 0.0274(11) -0.0055(8) -0.0077(9) 0.0029(9) C33 0.0241(10) 0.0223(9) 0.0271(11) 0.0034(8) -0.0049(8) -0.0025(8) C34 0.0483(15) 0.0617(16) 0.0288(13) -0.0212(12) -0.0054(11) 0.0160(13) C35 0.034(3) 0.071(4) 0.020(2) -0.009(2) 0.001(2) 0.028(3) C36 0.031(2) 0.041(3) 0.031(3) -0.019(2) -0.012(2) 0.017(2) C37 0.0297(14) 0.0474(16) 0.099(3) 0.0176(16) -0.0135(15) 0.0050(12) C38 0.0364(16) 0.0378(15) 0.138(4) 0.0066(18) -0.0266(19) 0.0031(12) C39 0.0374(16) 0.070(2) 0.101(3) 0.038(2) -0.0099(17) 0.0025(15) C40 0.0311(15) 0.068(2) 0.106(3) 0.0225(19) 0.0011(16) 0.0138(14) C41 0.0261(14) 0.059(2) 0.112(3) 0.013(2) -0.0048(16) 0.0139(13) C42 0.0165(12) 0.0382(14) 0.132(3) 0.0190(17) -0.0115(15) 0.0078(11) _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 Cl3 2.2181(8) . ? Cu1 Cl1 2.2207(7) . ? Cu1 Cl4 2.2787(6) . ? Cu1 Cl2 2.2890(6) . ? O1 C2 1.368(2) . ? O1 C1 1.430(3) . ? O2 C13 1.367(3) . ? O2 C16 1.432(3) . ? O3 C20 1.365(2) . ? O3 C19 1.433(3) . ? O4 C31 1.364(2) . ? O4 C34 1.437(3) . ? N1 C17 1.507(2) . ? N1 C8 1.516(2) . ? N1 C9 1.528(2) . ? N1 H1A 0.900(10) . ? N2 C18 1.504(2) . ? N2 C26 1.513(2) . ? N2 C27 1.532(2) . ? N2 H2A 0.890(9) . ? C1 H1D 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C7 1.387(3) . ? C2 C3 1.397(3) . ? C3 C4 1.380(3) . ? C3 H3A 0.9500 . ? C4 C5 1.398(3) . ? C4 H4A 0.9500 . ? C5 C6 1.385(3) . ? C5 C8 1.501(3) . ? C6 C7 1.394(3) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.504(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C15 1.388(3) . ? C10 C11 1.401(3) . ? C11 C12 1.378(3) . ? C11 H11A 0.9500 . ? C12 C13 1.392(3) . ? C12 H12A 0.9500 . ? C13 C14 1.383(3) . ? C14 C15 1.392(3) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.539(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C25 1.389(3) . ? C20 C21 1.392(3) . ? C21 C22 1.378(3) . ? C21 H21A 0.9500 . ? C22 C23 1.396(3) . ? C22 H22A 0.9500 . ? C23 C24 1.391(3) . ? C23 C26 1.502(3) . ? C24 C25 1.394(3) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.500(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C33 1.394(3) . ? C28 C29 1.398(3) . ? C29 C30 1.381(3) . ? C29 H29A 0.9500 . ? C30 C31 1.396(3) . ? C30 H30A 0.9500 . ? C31 C32 1.385(3) . ? C32 C33 1.388(3) . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C41 1.292(7) 3_676 ? C35 C36 1.375(8) . ? C35 H35A 0.71(6) . ? C36 C37 1.211(6) . ? C36 H36A 0.9500 . ? C37 C42 1.400(5) . ? C37 C38 1.435(5) . ? C38 C39 1.378(5) . ? C38 H38A 0.9500 . ? C39 C40 1.357(5) . ? C39 H39A 0.9500 . ? C40 C41 1.380(5) . ? C40 H40A 0.9500 . ? C41 C35 1.292(7) 3_676 ? C41 C42 1.418(5) . ? C42 C42 1.484(6) 3_676 ? 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 Cl3 Cu1 Cl1 144.50(3) . . ? Cl3 Cu1 Cl4 96.82(3) . . ? Cl1 Cu1 Cl4 97.83(3) . . ? Cl3 Cu1 Cl2 97.13(3) . . ? Cl1 Cu1 Cl2 96.65(3) . . ? Cl4 Cu1 Cl2 132.10(2) . . ? C2 O1 C1 116.98(17) . . ? C13 O2 C16 117.71(19) . . ? C20 O3 C19 116.99(17) . . ? C31 O4 C34 117.47(19) . . ? C17 N1 C8 114.50(14) . . ? C17 N1 C9 110.93(14) . . ? C8 N1 C9 110.57(14) . . ? C17 N1 H1A 106.8(15) . . ? C8 N1 H1A 109.1(15) . . ? C9 N1 H1A 104.3(15) . . ? C18 N2 C26 113.49(14) . . ? C18 N2 C27 111.33(14) . . ? C26 N2 C27 111.76(14) . . ? C18 N2 H2A 109.0(13) . . ? C26 N2 H2A 109.3(13) . . ? C27 N2 H2A 101.2(13) . . ? O1 C1 H1D 109.5 . . ? O1 C1 H1B 109.5 . . ? H1D C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1D C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C7 124.51(18) . . ? O1 C2 C3 115.45(18) . . ? C7 C2 C3 120.05(18) . . ? C4 C3 C2 119.89(19) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? C3 C4 C5 120.74(18) . . ? C3 C4 H4A 119.6 . . ? C5 C4 H4A 119.6 . . ? C6 C5 C4 118.78(18) . . ? C6 C5 C8 120.55(18) . . ? C4 C5 C8 120.64(17) . . ? C5 C6 C7 121.11(19) . . ? C5 C6 H6A 119.4 . . ? C7 C6 H6A 119.4 . . ? C2 C7 C6 119.39(18) . . ? C2 C7 H7A 120.3 . . ? C6 C7 H7A 120.3 . . ? C5 C8 N1 113.02(15) . . ? C5 C8 H8A 109.0 . . ? N1 C8 H8A 109.0 . . ? C5 C8 H8B 109.0 . . ? N1 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C10 C9 N1 114.11(15) . . ? C10 C9 H9A 108.7 . . ? N1 C9 H9A 108.7 . . ? C10 C9 H9B 108.7 . . ? N1 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? C15 C10 C11 117.86(19) . . ? C15 C10 C9 121.17(18) . . ? C11 C10 C9 120.90(18) . . ? C12 C11 C10 120.71(19) . . ? C12 C11 H11A 119.6 . . ? C10 C11 H11A 119.6 . . ? C11 C12 C13 120.7(2) . . ? C11 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? O2 C13 C14 125.3(2) . . ? O2 C13 C12 115.14(19) . . ? C14 C13 C12 119.5(2) . . ? C13 C14 C15 119.47(19) . . ? C13 C14 H14A 120.3 . . ? C15 C14 H14A 120.3 . . ? C10 C15 C14 121.8(2) . . ? C10 C15 H15A 119.1 . . ? C14 C15 H15A 119.1 . . ? O2 C16 H16A 109.5 . . ? O2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 C17 C18 111.74(15) . . ? N1 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? N1 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 107.9 . . ? N2 C18 C17 111.92(15) . . ? N2 C18 H18A 109.2 . . ? C17 C18 H18A 109.2 . . ? N2 C18 H18B 109.2 . . ? C17 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? O3 C19 H19A 109.5 . . ? O3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O3 C20 C25 124.81(18) . . ? O3 C20 C21 115.29(18) . . ? C25 C20 C21 119.90(19) . . ? C22 C21 C20 120.05(19) . . ? C22 C21 H21A 120.0 . . ? C20 C21 H21A 120.0 . . ? C21 C22 C23 120.98(18) . . ? C21 C22 H22A 119.5 . . ? C23 C22 H22A 119.5 . . ? C24 C23 C22 118.57(18) . . ? C24 C23 C26 121.54(18) . . ? C22 C23 C26 119.88(17) . . ? C23 C24 C25 120.93(18) . . ? C23 C24 H24A 119.5 . . ? C25 C24 H24A 119.5 . . ? C20 C25 C24 119.55(18) . . ? C20 C25 H25A 120.2 . . ? C24 C25 H25A 120.2 . . ? C23 C26 N2 112.08(15) . . ? C23 C26 H26A 109.2 . . ? N2 C26 H26A 109.2 . . ? C23 C26 H26B 109.2 . . ? N2 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? C28 C27 N2 114.83(14) . . ? C28 C27 H27A 108.6 . . ? N2 C27 H27A 108.6 . . ? C28 C27 H27B 108.6 . . ? N2 C27 H27B 108.6 . . ? H27A C27 H27B 107.5 . . ? C33 C28 C29 118.04(18) . . ? C33 C28 C27 120.71(17) . . ? C29 C28 C27 121.08(17) . . ? C30 C29 C28 120.95(18) . . ? C30 C29 H29A 119.5 . . ? C28 C29 H29A 119.5 . . ? C29 C30 C31 120.28(19) . . ? C29 C30 H30A 119.9 . . ? C31 C30 H30A 119.9 . . ? O4 C31 C32 125.26(19) . . ? O4 C31 C30 115.29(19) . . ? C32 C31 C30 119.45(18) . . ? C31 C32 C33 119.97(19) . . ? C31 C32 H32A 120.0 . . ? C33 C32 H32A 120.0 . . ? C32 C33 C28 121.31(19) . . ? C32 C33 H33A 119.3 . . ? C28 C33 H33A 119.3 . . ? O4 C34 H34A 109.5 . . ? O4 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O4 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C41 C35 C36 131.3(4) 3_676 . ? C41 C35 H35A 107(6) 3_676 . ? C36 C35 H35A 122(6) . . ? C37 C36 C35 125.1(4) . . ? C37 C36 H36A 117.4 . . ? C35 C36 H36A 117.4 . . ? C36 C37 C42 115.2(4) . . ? C36 C37 C38 126.3(4) . . ? C42 C37 C38 118.5(4) . . ? C39 C38 C37 120.9(3) . . ? C39 C38 H38A 119.5 . . ? C37 C38 H38A 119.5 . . ? C40 C39 C38 119.8(3) . . ? C40 C39 H39A 120.1 . . ? C38 C39 H39A 120.1 . . ? C39 C40 C41 121.5(4) . . ? C39 C40 H40A 119.3 . . ? C41 C40 H40A 119.3 . . ? C35 C41 C40 132.3(5) 3_676 . ? C35 C41 C42 107.0(4) 3_676 . ? C40 C41 C42 120.7(4) . . ? C37 C42 C41 118.5(3) . . ? C37 C42 C42 118.6(5) . 3_676 ? C41 C42 C42 122.9(4) . 3_676 ? 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 C1 O1 C2 C7 -5.1(3) . . . . ? C1 O1 C2 C3 175.22(18) . . . . ? O1 C2 C3 C4 -178.39(17) . . . . ? C7 C2 C3 C4 1.9(3) . . . . ? C2 C3 C4 C5 -0.2(3) . . . . ? C3 C4 C5 C6 -1.8(3) . . . . ? C3 C4 C5 C8 176.57(17) . . . . ? C4 C5 C6 C7 2.2(3) . . . . ? C8 C5 C6 C7 -176.22(17) . . . . ? O1 C2 C7 C6 178.78(18) . . . . ? C3 C2 C7 C6 -1.6(3) . . . . ? C5 C6 C7 C2 -0.5(3) . . . . ? C6 C5 C8 N1 107.4(2) . . . . ? C4 C5 C8 N1 -70.9(2) . . . . ? C17 N1 C8 C5 -59.0(2) . . . . ? C9 N1 C8 C5 174.81(15) . . . . ? C17 N1 C9 C10 -56.5(2) . . . . ? C8 N1 C9 C10 71.6(2) . . . . ? N1 C9 C10 C15 99.0(2) . . . . ? N1 C9 C10 C11 -84.0(2) . . . . ? C15 C10 C11 C12 -1.6(3) . . . . ? C9 C10 C11 C12 -178.66(18) . . . . ? C10 C11 C12 C13 1.0(3) . . . . ? C16 O2 C13 C14 5.1(3) . . . . ? C16 O2 C13 C12 -174.5(2) . . . . ? C11 C12 C13 O2 179.90(18) . . . . ? C11 C12 C13 C14 0.3(3) . . . . ? O2 C13 C14 C15 179.5(2) . . . . ? C12 C13 C14 C15 -0.9(3) . . . . ? C11 C10 C15 C14 1.0(3) . . . . ? C9 C10 C15 C14 178.05(18) . . . . ? C13 C14 C15 C10 0.3(3) . . . . ? C8 N1 C17 C18 79.89(19) . . . . ? C9 N1 C17 C18 -154.12(15) . . . . ? C26 N2 C18 C17 83.35(19) . . . . ? C27 N2 C18 C17 -149.52(15) . . . . ? N1 C17 C18 N2 157.15(15) . . . . ? C19 O3 C20 C25 3.6(3) . . . . ? C19 O3 C20 C21 -175.91(19) . . . . ? O3 C20 C21 C22 178.06(18) . . . . ? C25 C20 C21 C22 -1.4(3) . . . . ? C20 C21 C22 C23 0.7(3) . . . . ? C21 C22 C23 C24 0.2(3) . . . . ? C21 C22 C23 C26 178.92(18) . . . . ? C22 C23 C24 C25 -0.4(3) . . . . ? C26 C23 C24 C25 -179.04(17) . . . . ? O3 C20 C25 C24 -178.15(18) . . . . ? C21 C20 C25 C24 1.3(3) . . . . ? C23 C24 C25 C20 -0.4(3) . . . . ? C24 C23 C26 N2 108.5(2) . . . . ? C22 C23 C26 N2 -70.2(2) . . . . ? C18 N2 C26 C23 -65.7(2) . . . . ? C27 N2 C26 C23 167.42(15) . . . . ? C18 N2 C27 C28 -55.6(2) . . . . ? C26 N2 C27 C28 72.5(2) . . . . ? N2 C27 C28 C33 95.1(2) . . . . ? N2 C27 C28 C29 -89.7(2) . . . . ? C33 C28 C29 C30 -1.1(3) . . . . ? C27 C28 C29 C30 -176.35(17) . . . . ? C28 C29 C30 C31 0.3(3) . . . . ? C34 O4 C31 C32 -0.9(3) . . . . ? C34 O4 C31 C30 179.96(19) . . . . ? C29 C30 C31 O4 179.63(18) . . . . ? C29 C30 C31 C32 0.4(3) . . . . ? O4 C31 C32 C33 -179.34(19) . . . . ? C30 C31 C32 C33 -0.2(3) . . . . ? C31 C32 C33 C28 -0.7(3) . . . . ? C29 C28 C33 C32 1.3(3) . . . . ? C27 C28 C33 C32 176.59(18) . . . . ? C41 C35 C36 C37 0.6(8) 3_676 . . . ? C35 C36 C37 C42 -0.1(6) . . . . ? C35 C36 C37 C38 178.4(4) . . . . ? C36 C37 C38 C39 -179.5(4) . . . . ? C42 C37 C38 C39 -1.0(4) . . . . ? C37 C38 C39 C40 0.0(4) . . . . ? C38 C39 C40 C41 0.8(5) . . . . ? C39 C40 C41 C35 179.3(4) . . . 3_676 ? C39 C40 C41 C42 -0.5(4) . . . . ? C36 C37 C42 C41 179.9(3) . . . . ? C38 C37 C42 C41 1.2(4) . . . . ? C36 C37 C42 C42 -0.1(5) . . . 3_676 ? C38 C37 C42 C42 -178.8(3) . . . 3_676 ? C35 C41 C42 C37 179.7(3) 3_676 . . . ? C40 C41 C42 C37 -0.5(4) . . . . ? C35 C41 C42 C42 -0.3(5) 3_676 . . 3_676 ? C40 C41 C42 C42 179.5(3) . . . 3_676 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.392 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.058 # Attachment '- CRYSTAL4.cif' data_CRYSTAL4 _database_code_depnum_ccdc_archive 'CCDC 825597' #TrackingRef '- CRYSTAL4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H98.50 Cl7 Cu N4 O10.50' _chemical_formula_weight 1643.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 15.823(3) _cell_length_b 17.165(3) _cell_length_c 18.838(4) _cell_angle_alpha 64.88(3) _cell_angle_beta 72.07(3) _cell_angle_gamma 63.17(3) _cell_volume 4090.8(14) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 12030 _cell_measurement_theta_min 1.458 _cell_measurement_theta_max 27.847 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1725 _exptl_absorpt_coefficient_mu 0.556 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8969 _exptl_absorpt_correction_T_max 0.9363 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'rigaku saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 29816 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0622 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.02 _reflns_number_total 14347 _reflns_number_gt 10901 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalclear(Rigaku/MSC Inc., 2005)' _computing_cell_refinement crystalclear _computing_data_reduction crystalclear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0736P)^2^+6.7853P] 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 SHELXL _refine_ls_extinction_coef 0.0152(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 14347 _refine_ls_number_parameters 977 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0716 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1633 _refine_ls_wR_factor_gt 0.1557 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.003 _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 0.44836(3) 0.62499(3) 0.15966(3) 0.02614(15) Uani 1 1 d . . . Cl1 Cl 0.46960(7) 0.57684(7) 0.06033(5) 0.0306(2) Uani 1 1 d . . . Cl2 Cl 0.58951(7) 0.52547(7) 0.20848(6) 0.0312(2) Uani 1 1 d . . . Cl3 Cl 0.34343(7) 0.60819(8) 0.27059(5) 0.0335(3) Uani 1 1 d . . . Cl4 Cl 0.39772(8) 0.78041(8) 0.10377(6) 0.0402(3) Uani 1 1 d . . . Cl5 Cl 0.04589(6) 0.48451(6) 0.61328(5) 0.0231(2) Uani 1 1 d . . . Cl6 Cl 0.02887(7) 0.52254(7) 0.11004(5) 0.0299(2) Uani 1 1 d . . . O1 O -0.0536(2) 0.8526(2) 0.28603(18) 0.0384(7) Uani 1 1 d . . . O2 O 0.3369(2) 0.13214(19) 0.3678(2) 0.0429(8) Uani 1 1 d . . . O3 O 0.3706(3) 0.1058(2) 0.1986(2) 0.0497(9) Uani 1 1 d . . . O4 O -0.0127(2) 0.9497(2) -0.0639(2) 0.0511(9) Uani 1 1 d . . . O5 O -0.0510(2) 0.8415(2) 0.71750(19) 0.0375(7) Uani 1 1 d . . . O6 O 0.2940(3) 0.1288(3) 0.9406(2) 0.0607(11) Uani 1 1 d . . . O7 O 0.3800(3) 0.0929(2) 0.5836(2) 0.0721(13) Uani 1 1 d . . . O8 O 0.0714(2) 0.90586(18) 0.51554(17) 0.0320(7) Uani 1 1 d . . . N1 N 0.2078(2) 0.5512(2) 0.11269(17) 0.0216(7) Uani 1 1 d . . . H1 H 0.1515 0.5415 0.1221 0.026 Uiso 1 1 calc R . . N2 N 0.1809(2) 0.5221(2) -0.03732(18) 0.0262(7) Uani 1 1 d . . . H2 H 0.1356 0.5232 0.0079 0.031 Uiso 1 1 calc R . . N3 N 0.2392(2) 0.4802(2) 0.62397(16) 0.0175(6) Uani 1 1 d . . . H3 H 0.1782 0.4794 0.6342 0.021 Uiso 1 1 calc R . . N4 N 0.1716(2) 0.53532(19) 0.45312(17) 0.0171(6) Uani 1 1 d . . . H4 H 0.1332 0.5178 0.5007 0.021 Uiso 1 1 calc R . . C1 C 0.1855(3) 0.6549(3) 0.0755(2) 0.0272(9) Uani 1 1 d . . . H1A H 0.2464 0.6655 0.0568 0.033 Uiso 1 1 calc R . . H1B H 0.1533 0.6796 0.0288 0.033 Uiso 1 1 calc R . . C2 C 0.1228(3) 0.7080(3) 0.1316(2) 0.0241(8) Uani 1 1 d . . . C3 C 0.1515(3) 0.7659(3) 0.1436(3) 0.0328(10) Uani 1 1 d . . . H3A H 0.2116 0.7706 0.1173 0.039 Uiso 1 1 calc R . . C4 C 0.0941(3) 0.8179(3) 0.1932(3) 0.0341(10) Uani 1 1 d . . . H4A H 0.1136 0.8595 0.1991 0.041 Uiso 1 1 calc R . . C5 C 0.0087(3) 0.8077(3) 0.2337(2) 0.0293(9) Uani 1 1 d . . . C6 C -0.0191(3) 0.7473(3) 0.2246(3) 0.0401(11) Uani 1 1 d . . . H6 H -0.0767 0.7388 0.2543 0.048 Uiso 1 1 calc R . . C7 C 0.0356(3) 0.6994(3) 0.1731(3) 0.0376(10) Uani 1 1 d . . . H7 H 0.0142 0.6602 0.1656 0.045 Uiso 1 1 calc R . . C8 C -0.0368(4) 0.9259(3) 0.2888(3) 0.0418(11) Uani 1 1 d . . . H8A H 0.0249 0.9011 0.3071 0.063 Uiso 1 1 calc R . . H8B H -0.0879 0.9546 0.3255 0.063 Uiso 1 1 calc R . . H8C H -0.0358 0.9724 0.2358 0.063 Uiso 1 1 calc R . . C9 C 0.2430(3) 0.5138(3) 0.1918(2) 0.0261(9) Uani 1 1 d . . . H9A H 0.3022 0.5252 0.1825 0.031 Uiso 1 1 calc R . . H9B H 0.1942 0.5488 0.2262 0.031 Uiso 1 1 calc R . . C10 C 0.2634(3) 0.4121(3) 0.2349(2) 0.0218(8) Uani 1 1 d . . . C11 C 0.1914(3) 0.3797(3) 0.2800(2) 0.0233(8) Uani 1 1 d . . . H11 H 0.1266 0.4215 0.2807 0.028 Uiso 1 1 calc R . . C12 C 0.2129(3) 0.2860(3) 0.3247(2) 0.0283(9) Uani 1 1 d . . . H12 H 0.1632 0.2638 0.3556 0.034 Uiso 1 1 calc R . . C13 C 0.3079(3) 0.2254(3) 0.3236(2) 0.0293(9) Uani 1 1 d . . . C14 C 0.3802(3) 0.2567(3) 0.2786(2) 0.0322(10) Uani 1 1 d . . . H14 H 0.4449 0.2147 0.2779 0.039 Uiso 1 1 calc R . . C15 C 0.3584(3) 0.3491(3) 0.2347(2) 0.0309(9) Uani 1 1 d . . . H15 H 0.4086 0.3706 0.2037 0.037 Uiso 1 1 calc R . . C16 C 0.2634(4) 0.0959(3) 0.4118(4) 0.0637(17) Uani 1 1 d . . . H16A H 0.2256 0.1252 0.4521 0.096 Uiso 1 1 calc R . . H16B H 0.2926 0.0287 0.4376 0.096 Uiso 1 1 calc R . . H16C H 0.2216 0.1090 0.3758 0.096 Uiso 1 1 calc R . . C17 C 0.2815(3) 0.4970(3) 0.0598(2) 0.0239(8) Uani 1 1 d . . . H17A H 0.3450 0.4955 0.0595 0.029 Uiso 1 1 calc R . . H17B H 0.2845 0.4323 0.0839 0.029 Uiso 1 1 calc R . . C18 C 0.2643(3) 0.5335(3) -0.0252(2) 0.0255(8) Uani 1 1 d . . . H18A H 0.2538 0.6003 -0.0473 0.031 Uiso 1 1 calc R . . H18B H 0.3231 0.5016 -0.0560 0.031 Uiso 1 1 calc R . . C19 C 0.2083(3) 0.4311(3) -0.0500(2) 0.0331(10) Uani 1 1 d . . . H19A H 0.1501 0.4281 -0.0563 0.040 Uiso 1 1 calc R . . H19B H 0.2532 0.4309 -0.1000 0.040 Uiso 1 1 calc R . . C20 C 0.2536(3) 0.3464(3) 0.0156(2) 0.0312(9) Uani 1 1 d . . . C21 C 0.1975(3) 0.3075(3) 0.0830(2) 0.0319(10) Uani 1 1 d . . . H21 H 0.1298 0.3366 0.0876 0.038 Uiso 1 1 calc R . . C22 C 0.2386(3) 0.2284(3) 0.1425(3) 0.0365(11) Uani 1 1 d . . . H22 H 0.1992 0.2032 0.1875 0.044 Uiso 1 1 calc R . . C23 C 0.3376(3) 0.1851(3) 0.1371(3) 0.0363(10) Uani 1 1 d . . . C24 C 0.3953(3) 0.2226(3) 0.0714(3) 0.0383(11) Uani 1 1 d . . . H24 H 0.4630 0.1948 0.0681 0.046 Uiso 1 1 calc R . . C25 C 0.3522(3) 0.3015(3) 0.0108(3) 0.0359(10) Uani 1 1 d . . . H25 H 0.3915 0.3253 -0.0353 0.043 Uiso 1 1 calc R . . C26 C 0.4726(4) 0.0609(4) 0.1968(4) 0.0615(15) Uani 1 1 d . . . H26A H 0.5017 0.0449 0.1484 0.092 Uiso 1 1 calc R . . H26B H 0.4875 0.0044 0.2432 0.092 Uiso 1 1 calc R . . H26C H 0.4981 0.1029 0.1978 0.092 Uiso 1 1 calc R . . C27 C 0.1338(3) 0.6023(3) -0.1077(2) 0.0355(10) Uani 1 1 d . . . H27A H 0.1821 0.6039 -0.1559 0.043 Uiso 1 1 calc R . . H27B H 0.0824 0.5906 -0.1160 0.043 Uiso 1 1 calc R . . C28 C 0.0919(3) 0.6955(3) -0.0972(2) 0.0328(10) Uani 1 1 d . . . C29 C 0.1407(3) 0.7563(3) -0.1320(2) 0.0343(10) Uani 1 1 d . . . H29 H 0.2003 0.7395 -0.1649 0.041 Uiso 1 1 calc R . . C30 C 0.1048(3) 0.8397(3) -0.1200(2) 0.0386(11) Uani 1 1 d . . . H30 H 0.1400 0.8793 -0.1436 0.046 Uiso 1 1 calc R . . C31 C 0.0168(3) 0.8661(3) -0.0731(3) 0.0381(11) Uani 1 1 d . . . C32 C -0.0343(3) 0.8081(3) -0.0398(3) 0.0391(11) Uani 1 1 d . . . H32 H -0.0950 0.8262 -0.0087 0.047 Uiso 1 1 calc R . . C33 C 0.0027(3) 0.7251(3) -0.0516(2) 0.0360(10) Uani 1 1 d . . . H33 H -0.0331 0.6861 -0.0282 0.043 Uiso 1 1 calc R . . C34 C -0.0982(4) 0.9765(4) -0.0100(4) 0.0636(16) Uani 1 1 d . . . H34A H -0.1527 0.9812 -0.0281 0.095 Uiso 1 1 calc R . . H34B H -0.1097 1.0367 -0.0081 0.095 Uiso 1 1 calc R . . H34C H -0.0907 0.9299 0.0430 0.095 Uiso 1 1 calc R . . C35 C 0.2483(3) 0.5089(3) 0.6866(2) 0.0220(8) Uani 1 1 d . . . H35A H 0.2457 0.4600 0.7388 0.026 Uiso 1 1 calc R . . H35B H 0.3114 0.5142 0.6742 0.026 Uiso 1 1 calc R . . C36 C 0.1707(3) 0.5998(3) 0.6915(2) 0.0210(8) Uani 1 1 d . . . C37 C 0.0766(3) 0.6053(3) 0.7201(2) 0.0231(8) Uani 1 1 d . . . H37 H 0.0614 0.5526 0.7339 0.028 Uiso 1 1 calc R . . C38 C 0.0050(3) 0.6867(3) 0.7287(2) 0.0271(9) Uani 1 1 d . . . H38 H -0.0590 0.6898 0.7483 0.033 Uiso 1 1 calc R . . C39 C 0.0265(3) 0.7630(3) 0.7090(2) 0.0262(9) Uani 1 1 d . . . C40 C 0.1201(3) 0.7596(3) 0.6819(2) 0.0277(9) Uani 1 1 d . . . H40 H 0.1349 0.8121 0.6697 0.033 Uiso 1 1 calc R . . C41 C 0.1923(3) 0.6765(3) 0.6730(2) 0.0245(8) Uani 1 1 d . . . H41 H 0.2565 0.6731 0.6542 0.029 Uiso 1 1 calc R . . C42 C -0.0312(4) 0.9196(3) 0.7072(3) 0.0452(12) Uani 1 1 d . . . H42A H 0.0135 0.9006 0.7430 0.068 Uiso 1 1 calc R . . H42B H -0.0909 0.9684 0.7192 0.068 Uiso 1 1 calc R . . H42C H -0.0027 0.9432 0.6522 0.068 Uiso 1 1 calc R . . C43 C 0.3115(3) 0.3832(2) 0.6281(2) 0.0232(8) Uani 1 1 d . . . H43A H 0.2975 0.3623 0.5930 0.028 Uiso 1 1 calc R . . H43B H 0.3764 0.3853 0.6082 0.028 Uiso 1 1 calc R . . C44 C 0.3103(3) 0.3142(3) 0.7110(2) 0.0256(9) Uani 1 1 d . . . C45 C 0.3857(3) 0.2738(3) 0.7517(3) 0.0394(11) Uani 1 1 d . . . H45 H 0.4409 0.2892 0.7268 0.047 Uiso 1 1 calc R . . C46 C 0.3846(3) 0.2105(3) 0.8290(3) 0.0402(11) Uani 1 1 d . . . H46 H 0.4385 0.1826 0.8558 0.048 Uiso 1 1 calc R . . C47 C 0.3050(4) 0.1897(3) 0.8651(3) 0.0399(11) Uani 1 1 d . . . C48 C 0.2264(4) 0.2339(5) 0.8267(4) 0.087(3) Uani 1 1 d . . . H48 H 0.1691 0.2231 0.8534 0.105 Uiso 1 1 calc R . . C49 C 0.2301(4) 0.2942(4) 0.7492(3) 0.072(2) Uani 1 1 d . . . H49 H 0.1762 0.3219 0.7225 0.086 Uiso 1 1 calc R . . C50 C 0.3752(5) 0.0792(4) 0.9813(3) 0.0636(17) Uani 1 1 d . . . H50A H 0.4251 0.0357 0.9553 0.095 Uiso 1 1 calc R . . H50B H 0.3566 0.0448 1.0363 0.095 Uiso 1 1 calc R . . H50C H 0.3997 0.1230 0.9802 0.095 Uiso 1 1 calc R . . C51 C 0.2492(3) 0.5531(2) 0.54421(19) 0.0179(7) Uani 1 1 d . . . H51A H 0.3053 0.5668 0.5401 0.022 Uiso 1 1 calc R . . H51B H 0.1919 0.6106 0.5428 0.022 Uiso 1 1 calc R . . C52 C 0.2607(2) 0.5299(2) 0.4714(2) 0.0169(7) Uani 1 1 d . . . H52A H 0.2868 0.5725 0.4248 0.020 Uiso 1 1 calc R . . H52B H 0.3089 0.4662 0.4782 0.020 Uiso 1 1 calc R . . C53 C 0.1963(3) 0.4694(2) 0.4090(2) 0.0206(8) Uani 1 1 d . . . H53A H 0.1366 0.4766 0.3959 0.025 Uiso 1 1 calc R . . H53B H 0.2379 0.4871 0.3585 0.025 Uiso 1 1 calc R . . C54 C 0.2459(3) 0.3698(2) 0.4549(2) 0.0211(8) Uani 1 1 d . . . C55 C 0.3439(3) 0.3271(3) 0.4376(2) 0.0254(8) Uani 1 1 d . . . H55 H 0.3790 0.3616 0.3963 0.030 Uiso 1 1 calc R . . C56 C 0.3925(3) 0.2338(3) 0.4798(3) 0.0359(10) Uani 1 1 d . . . H56 H 0.4599 0.2050 0.4676 0.043 Uiso 1 1 calc R . . C57 C 0.3401(4) 0.1848(3) 0.5396(3) 0.0427(12) Uani 1 1 d . . . C58 C 0.2416(3) 0.2264(3) 0.5564(3) 0.0391(11) Uani 1 1 d . . . H58 H 0.2062 0.1915 0.5965 0.047 Uiso 1 1 calc R . . C59 C 0.1952(3) 0.3177(3) 0.5153(2) 0.0274(9) Uani 1 1 d . . . H59 H 0.1279 0.3461 0.5280 0.033 Uiso 1 1 calc R . . C60 C 0.4822(5) 0.0518(5) 0.5764(5) 0.106(3) Uani 1 1 d . . . H60A H 0.5086 0.0422 0.5251 0.160 Uiso 1 1 calc R . . H60B H 0.5015 -0.0079 0.6191 0.160 Uiso 1 1 calc R . . H60C H 0.5066 0.0931 0.5800 0.160 Uiso 1 1 calc R . . C61 C 0.1132(3) 0.6317(2) 0.4022(2) 0.0205(8) Uani 1 1 d . . . H61A H 0.1456 0.6433 0.3468 0.025 Uiso 1 1 calc R . . H61B H 0.0495 0.6332 0.4032 0.025 Uiso 1 1 calc R . . C62 C 0.0996(3) 0.7083(2) 0.4289(2) 0.0211(8) Uani 1 1 d . . . C63 C 0.0256(3) 0.7324(2) 0.4891(2) 0.0224(8) Uani 1 1 d . . . H63 H -0.0193 0.7027 0.5117 0.027 Uiso 1 1 calc R . . C64 C 0.0181(3) 0.7995(3) 0.5155(2) 0.0250(8) Uani 1 1 d . . . H64 H -0.0325 0.8163 0.5557 0.030 Uiso 1 1 calc R . . C65 C 0.0842(3) 0.8424(2) 0.4837(2) 0.0237(8) Uani 1 1 d . . . C66 C 0.1568(3) 0.8207(3) 0.4220(2) 0.0263(9) Uani 1 1 d . . . H66 H 0.2009 0.8513 0.3985 0.032 Uiso 1 1 calc R . . C67 C 0.1628(3) 0.7537(3) 0.3960(2) 0.0234(8) Uani 1 1 d . . . H67 H 0.2119 0.7386 0.3543 0.028 Uiso 1 1 calc R . . C68 C 0.1417(3) 0.9462(3) 0.4887(3) 0.0379(10) Uani 1 1 d . . . H68A H 0.2052 0.8970 0.4959 0.057 Uiso 1 1 calc R . . H68B H 0.1280 0.9857 0.5193 0.057 Uiso 1 1 calc R . . H68C H 0.1404 0.9837 0.4325 0.057 Uiso 1 1 calc R . . O9 O 0.3912(4) 0.7707(4) 0.4071(4) 0.0409(15) Uani 0.50 1 d P . . H9 H 0.3982 0.7812 0.3582 0.061 Uiso 0.50 1 calc PR . . C69 C 0.4268(3) 0.6759(3) 0.4462(3) 0.0357(10) Uani 1 1 d . . . C70 C 0.4499(3) 0.6078(3) 0.4157(2) 0.0308(9) Uani 1 1 d . . . H70 H 0.4380 0.6248 0.3637 0.037 Uiso 1 1 calc R . . C71 C 0.4911(3) 0.5125(3) 0.4605(2) 0.0296(9) Uani 1 1 d . . . C72 C 0.5156(3) 0.4410(3) 0.4314(2) 0.0319(10) Uani 1 1 d . . . H72 H 0.5045 0.4564 0.3795 0.038 Uiso 1 1 calc R . . C73 C 0.5552(3) 0.3492(3) 0.4760(3) 0.0364(10) Uani 1 1 d . . . H73 H 0.5706 0.3023 0.4548 0.044 Uiso 1 1 calc R . . Cl7 Cl 0.67170(11) 0.13025(10) 0.37925(7) 0.0578(4) Uani 1 1 d . . . O10 O 0.5907(3) 0.3276(2) 0.30364(19) 0.0482(8) Uani 1 1 d . . . H10 H 0.5893 0.3817 0.2771 0.072 Uiso 1 1 calc R . . C74 C 0.6122(3) 0.2803(3) 0.2533(3) 0.0384(11) Uani 1 1 d . . . C75 C 0.6493(3) 0.1852(3) 0.2808(3) 0.0399(11) Uani 1 1 d . . . C76 C 0.6717(3) 0.1308(3) 0.2334(2) 0.0356(10) Uani 1 1 d . . . C77 C 0.7089(4) 0.0337(4) 0.2599(3) 0.0533(14) Uani 1 1 d . . . H77 H 0.7211 0.0003 0.3131 0.064 Uiso 1 1 calc R . . C78 C 0.7276(4) -0.0126(4) 0.2118(4) 0.0663(17) Uani 1 1 d . . . H78 H 0.7528 -0.0784 0.2314 0.080 Uiso 1 1 calc R . . C79 C 0.7108(4) 0.0343(4) 0.1325(3) 0.0553(14) Uani 1 1 d . . . H79 H 0.7244 -0.0001 0.0993 0.066 Uiso 1 1 calc R . . C80 C 0.6746(4) 0.1298(4) 0.1027(3) 0.0507(13) Uani 1 1 d . . . H80 H 0.6641 0.1615 0.0490 0.061 Uiso 1 1 calc R . . C81 C 0.6530(3) 0.1806(3) 0.1537(3) 0.0406(11) Uani 1 1 d . . . C82 C 0.6158(3) 0.2779(3) 0.1255(3) 0.0415(12) Uani 1 1 d . . . H82 H 0.6048 0.3101 0.0719 0.050 Uiso 1 1 calc R . . C83 C 0.5952(3) 0.3269(3) 0.1735(3) 0.0388(11) Uani 1 1 d . . . H83 H 0.5693 0.3928 0.1535 0.047 Uiso 1 1 calc R . . O11 O 0.3361(4) 0.8290(3) 0.2646(3) 0.0872(15) Uani 1 1 d . . . H11A H 0.3531 0.8030 0.2307 0.131 Uiso 1 1 calc R . . C84 C 0.3252(6) 0.9213(4) 0.2266(4) 0.096(3) Uani 1 1 d . . . H84A H 0.3113 0.9501 0.2661 0.144 Uiso 1 1 calc R . . H84B H 0.2722 0.9536 0.1955 0.144 Uiso 1 1 calc R . . H84C H 0.3844 0.9255 0.1913 0.144 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0230(3) 0.0399(3) 0.0175(2) -0.0090(2) -0.00084(19) -0.0152(2) Cl1 0.0306(5) 0.0458(6) 0.0207(5) -0.0122(4) -0.0060(4) -0.0162(5) Cl2 0.0255(5) 0.0481(6) 0.0228(5) -0.0109(4) -0.0058(4) -0.0153(5) Cl3 0.0276(5) 0.0582(7) 0.0184(5) -0.0138(4) 0.0040(4) -0.0228(5) Cl4 0.0402(6) 0.0382(6) 0.0359(6) -0.0066(5) -0.0027(5) -0.0166(5) Cl5 0.0168(5) 0.0351(5) 0.0210(4) -0.0094(4) 0.0002(3) -0.0144(4) Cl6 0.0281(5) 0.0497(6) 0.0211(5) -0.0120(4) 0.0032(4) -0.0263(5) O1 0.0405(18) 0.0378(17) 0.0450(18) -0.0220(14) -0.0058(14) -0.0141(14) O2 0.0390(18) 0.0226(15) 0.057(2) -0.0017(14) -0.0145(16) -0.0095(14) O3 0.046(2) 0.0397(19) 0.057(2) -0.0132(16) -0.0056(17) -0.0152(16) O4 0.042(2) 0.048(2) 0.051(2) -0.0123(16) 0.0046(16) -0.0185(17) O5 0.0324(17) 0.0333(16) 0.0527(19) -0.0221(14) -0.0050(14) -0.0106(14) O6 0.067(3) 0.058(2) 0.0351(19) 0.0191(16) -0.0181(17) -0.031(2) O7 0.063(3) 0.0305(19) 0.074(3) 0.0087(18) -0.010(2) -0.0023(18) O8 0.0347(17) 0.0273(15) 0.0401(17) -0.0148(13) -0.0062(13) -0.0127(13) N1 0.0244(17) 0.0311(17) 0.0144(15) -0.0032(13) -0.0052(13) -0.0170(14) N2 0.0210(17) 0.048(2) 0.0151(15) -0.0112(14) 0.0018(13) -0.0196(16) N3 0.0138(15) 0.0239(16) 0.0148(14) -0.0046(12) -0.0033(12) -0.0081(13) N4 0.0161(15) 0.0228(16) 0.0141(14) -0.0050(12) -0.0028(12) -0.0093(13) C1 0.029(2) 0.027(2) 0.0211(19) -0.0005(16) -0.0079(16) -0.0115(18) C2 0.024(2) 0.0241(19) 0.0233(19) -0.0005(15) -0.0092(16) -0.0110(17) C3 0.027(2) 0.028(2) 0.040(2) -0.0025(18) -0.0058(19) -0.0143(18) C4 0.034(2) 0.022(2) 0.049(3) -0.0090(19) -0.011(2) -0.0131(19) C5 0.032(2) 0.023(2) 0.030(2) -0.0034(17) -0.0132(18) -0.0072(18) C6 0.037(3) 0.053(3) 0.045(3) -0.022(2) 0.001(2) -0.028(2) C7 0.036(3) 0.049(3) 0.043(3) -0.022(2) -0.002(2) -0.024(2) C8 0.047(3) 0.029(2) 0.054(3) -0.015(2) -0.021(2) -0.009(2) C9 0.038(2) 0.028(2) 0.0187(19) -0.0028(16) -0.0112(17) -0.0181(18) C10 0.025(2) 0.0252(19) 0.0189(18) -0.0071(15) -0.0080(15) -0.0097(17) C11 0.021(2) 0.027(2) 0.0239(19) -0.0089(16) -0.0060(16) -0.0084(16) C12 0.028(2) 0.036(2) 0.026(2) -0.0115(17) -0.0008(17) -0.0172(19) C13 0.032(2) 0.026(2) 0.033(2) -0.0097(17) -0.0111(18) -0.0088(18) C14 0.020(2) 0.035(2) 0.038(2) -0.0157(19) -0.0063(18) -0.0026(18) C15 0.027(2) 0.041(2) 0.026(2) -0.0089(18) -0.0010(17) -0.018(2) C16 0.054(3) 0.034(3) 0.086(4) 0.011(3) -0.018(3) -0.026(3) C17 0.021(2) 0.034(2) 0.0195(19) -0.0074(16) -0.0026(15) -0.0142(17) C18 0.021(2) 0.040(2) 0.0203(19) -0.0077(17) -0.0031(16) -0.0172(18) C19 0.035(2) 0.058(3) 0.024(2) -0.021(2) 0.0045(18) -0.031(2) C20 0.030(2) 0.048(3) 0.032(2) -0.023(2) 0.0042(18) -0.024(2) C21 0.027(2) 0.047(3) 0.033(2) -0.019(2) 0.0052(18) -0.024(2) C22 0.034(3) 0.043(3) 0.042(3) -0.025(2) 0.012(2) -0.024(2) C23 0.039(3) 0.036(2) 0.043(3) -0.021(2) 0.001(2) -0.020(2) C24 0.028(2) 0.044(3) 0.053(3) -0.027(2) 0.004(2) -0.018(2) C25 0.035(3) 0.045(3) 0.036(2) -0.020(2) 0.012(2) -0.027(2) C26 0.059(4) 0.050(3) 0.070(4) -0.017(3) -0.018(3) -0.013(3) C27 0.029(2) 0.060(3) 0.018(2) -0.0073(19) -0.0073(17) -0.020(2) C28 0.023(2) 0.052(3) 0.0173(19) -0.0045(18) -0.0065(16) -0.013(2) C29 0.022(2) 0.052(3) 0.017(2) 0.0000(18) -0.0034(16) -0.014(2) C30 0.025(2) 0.048(3) 0.026(2) 0.0081(19) -0.0055(18) -0.018(2) C31 0.030(2) 0.045(3) 0.029(2) -0.0031(19) -0.0067(19) -0.012(2) C32 0.025(2) 0.057(3) 0.028(2) -0.009(2) 0.0025(18) -0.018(2) C33 0.026(2) 0.060(3) 0.025(2) -0.007(2) -0.0044(17) -0.024(2) C34 0.048(3) 0.068(4) 0.068(4) -0.028(3) 0.014(3) -0.025(3) C35 0.025(2) 0.028(2) 0.0166(18) -0.0078(15) -0.0081(15) -0.0091(17) C36 0.023(2) 0.032(2) 0.0099(16) -0.0058(15) -0.0025(14) -0.0131(17) C37 0.026(2) 0.033(2) 0.0150(18) -0.0100(15) 0.0026(15) -0.0165(18) C38 0.023(2) 0.039(2) 0.025(2) -0.0129(17) 0.0007(16) -0.0161(19) C39 0.024(2) 0.032(2) 0.0216(19) -0.0131(16) -0.0054(16) -0.0044(18) C40 0.037(2) 0.030(2) 0.0216(19) -0.0061(16) -0.0074(17) -0.0173(19) C41 0.025(2) 0.032(2) 0.0195(19) -0.0069(16) -0.0038(16) -0.0141(18) C42 0.054(3) 0.037(3) 0.054(3) -0.020(2) -0.021(2) -0.011(2) C43 0.023(2) 0.0212(19) 0.0224(19) -0.0051(15) -0.0033(16) -0.0081(16) C44 0.029(2) 0.025(2) 0.0221(19) -0.0038(16) -0.0081(16) -0.0109(17) C45 0.026(2) 0.044(3) 0.034(2) 0.002(2) -0.0074(19) -0.013(2) C46 0.040(3) 0.039(3) 0.035(2) 0.0012(19) -0.019(2) -0.013(2) C47 0.050(3) 0.037(2) 0.028(2) 0.0035(19) -0.013(2) -0.021(2) C48 0.054(4) 0.097(5) 0.071(4) 0.053(4) -0.035(3) -0.054(4) C49 0.061(4) 0.083(4) 0.062(4) 0.041(3) -0.043(3) -0.058(3) C50 0.103(5) 0.050(3) 0.032(3) 0.011(2) -0.035(3) -0.031(3) C51 0.0158(18) 0.0229(18) 0.0146(17) -0.0012(14) -0.0038(14) -0.0105(15) C52 0.0115(17) 0.0259(19) 0.0160(17) -0.0061(14) -0.0029(14) -0.0095(15) C53 0.0189(19) 0.0257(19) 0.0209(18) -0.0105(15) -0.0039(15) -0.0081(16) C54 0.023(2) 0.0256(19) 0.0207(18) -0.0099(15) -0.0041(15) -0.0118(16) C55 0.026(2) 0.034(2) 0.0228(19) -0.0134(17) 0.0015(16) -0.0162(18) C56 0.025(2) 0.035(2) 0.041(3) -0.011(2) -0.0064(19) -0.0051(19) C57 0.047(3) 0.023(2) 0.043(3) -0.0006(19) -0.011(2) -0.007(2) C58 0.043(3) 0.032(2) 0.036(2) -0.0076(19) 0.008(2) -0.020(2) C59 0.024(2) 0.030(2) 0.032(2) -0.0161(17) 0.0026(17) -0.0130(18) C60 0.074(5) 0.049(4) 0.111(6) 0.013(4) -0.030(4) 0.020(4) C61 0.0189(19) 0.0233(19) 0.0185(18) -0.0062(15) -0.0068(15) -0.0053(16) C62 0.021(2) 0.0209(18) 0.0191(18) -0.0005(14) -0.0091(15) -0.0077(16) C63 0.0150(19) 0.0249(19) 0.026(2) -0.0054(15) -0.0046(15) -0.0082(16) C64 0.020(2) 0.0231(19) 0.028(2) -0.0086(16) -0.0042(16) -0.0041(16) C65 0.025(2) 0.0181(18) 0.027(2) -0.0036(15) -0.0100(16) -0.0064(16) C66 0.025(2) 0.0225(19) 0.029(2) -0.0007(16) -0.0087(17) -0.0111(17) C67 0.023(2) 0.025(2) 0.0201(19) -0.0030(15) -0.0068(15) -0.0089(17) C68 0.042(3) 0.036(2) 0.047(3) -0.014(2) -0.013(2) -0.020(2) O9 0.031(3) 0.052(4) 0.043(4) -0.019(3) 0.000(3) -0.019(3) C69 0.020(2) 0.047(3) 0.035(2) -0.008(2) -0.0010(18) -0.015(2) C70 0.019(2) 0.055(3) 0.021(2) -0.0074(19) -0.0016(16) -0.021(2) C71 0.0156(19) 0.051(3) 0.0232(19) -0.0095(18) 0.0025(15) -0.0198(19) C72 0.021(2) 0.054(3) 0.024(2) -0.014(2) -0.0007(17) -0.017(2) C73 0.025(2) 0.060(3) 0.034(2) -0.022(2) 0.0050(18) -0.023(2) Cl7 0.0638(9) 0.0702(9) 0.0324(6) -0.0012(6) -0.0151(6) -0.0288(7) O10 0.052(2) 0.055(2) 0.0429(19) -0.0152(16) -0.0047(16) -0.0271(19) C74 0.021(2) 0.049(3) 0.044(3) -0.015(2) -0.0001(19) -0.016(2) C75 0.030(2) 0.052(3) 0.027(2) -0.001(2) -0.0048(19) -0.018(2) C76 0.022(2) 0.049(3) 0.028(2) -0.0050(19) -0.0024(17) -0.014(2) C77 0.040(3) 0.047(3) 0.057(3) -0.010(3) -0.008(3) -0.011(2) C78 0.055(4) 0.056(4) 0.069(4) -0.019(3) -0.006(3) -0.009(3) C79 0.038(3) 0.063(4) 0.060(3) -0.033(3) 0.006(3) -0.012(3) C80 0.036(3) 0.081(4) 0.040(3) -0.026(3) 0.001(2) -0.025(3) C81 0.022(2) 0.046(3) 0.045(3) -0.011(2) -0.005(2) -0.011(2) C82 0.028(2) 0.060(3) 0.027(2) -0.001(2) -0.0071(18) -0.018(2) C83 0.022(2) 0.050(3) 0.039(3) -0.007(2) -0.0043(19) -0.016(2) O11 0.129(4) 0.083(3) 0.060(3) -0.024(2) 0.008(3) -0.063(3) C84 0.126(7) 0.052(4) 0.084(5) -0.015(4) 0.016(5) -0.040(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 Cl1 2.2298(12) . ? Cu1 Cl3 2.2340(13) . ? Cu1 Cl4 2.2524(15) . ? Cu1 Cl2 2.2887(15) . ? O1 C5 1.378(5) . ? O1 C8 1.423(5) . ? O2 C13 1.382(5) . ? O2 C16 1.431(6) . ? O3 C23 1.363(6) . ? O3 C26 1.437(7) . ? O4 C31 1.365(6) . ? O4 C34 1.436(6) . ? O5 C39 1.384(5) . ? O5 C42 1.433(5) . ? O6 C47 1.377(5) . ? O6 C50 1.424(7) . ? O7 C57 1.374(5) . ? O7 C60 1.432(8) . ? O8 C65 1.367(5) . ? O8 C68 1.422(5) . ? N1 C17 1.519(5) . ? N1 C1 1.521(5) . ? N1 C9 1.523(5) . ? N1 H1 0.9300 . ? N2 C18 1.514(5) . ? N2 C19 1.526(5) . ? N2 C27 1.530(5) . ? N2 H2 0.9300 . ? N3 C51 1.512(4) . ? N3 C43 1.520(5) . ? N3 C35 1.522(4) . ? N3 H3 0.9300 . ? N4 C52 1.505(4) . ? N4 C53 1.524(4) . ? N4 C61 1.527(4) . ? N4 H4 0.9300 . ? C1 C2 1.512(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.380(6) . ? C2 C7 1.399(6) . ? C3 C4 1.397(6) . ? C3 H3A 0.9500 . ? C4 C5 1.380(6) . ? C4 H4A 0.9500 . ? C5 C6 1.380(6) . ? C6 C7 1.373(6) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.503(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.381(5) . ? C10 C15 1.401(6) . ? C11 C12 1.394(5) . ? C11 H11 0.9500 . ? C12 C13 1.389(6) . ? C12 H12 0.9500 . ? C13 C14 1.373(6) . ? C14 C15 1.373(6) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.514(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.495(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C25 1.387(6) . ? C20 C21 1.403(6) . ? C21 C22 1.372(6) . ? C21 H21 0.9500 . ? C22 C23 1.389(6) . ? C22 H22 0.9500 . ? C23 C24 1.392(6) . ? C24 C25 1.392(7) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.507(7) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.397(6) . ? C28 C33 1.402(6) . ? C29 C30 1.373(7) . ? C29 H29 0.9500 . ? C30 C31 1.393(6) . ? C30 H30 0.9500 . ? C31 C32 1.386(7) . ? C32 C33 1.363(7) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.508(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C41 1.385(5) . ? C36 C37 1.393(5) . ? C37 C38 1.383(6) . ? C37 H37 0.9500 . ? C38 C39 1.371(6) . ? C38 H38 0.9500 . ? C39 C40 1.392(6) . ? C40 C41 1.407(6) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.509(5) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.363(6) . ? C44 C49 1.367(6) . ? C45 C46 1.401(6) . ? C45 H45 0.9500 . ? C46 C47 1.360(7) . ? C46 H46 0.9500 . ? C47 C48 1.370(7) . ? C48 C49 1.387(7) . ? C48 H48 0.9500 . ? C49 H49 0.9500 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.523(5) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.496(5) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.383(5) . ? C54 C59 1.400(5) . ? C55 C56 1.404(6) . ? C55 H55 0.9500 . ? C56 C57 1.384(6) . ? C56 H56 0.9500 . ? C57 C58 1.386(7) . ? C58 C59 1.370(6) . ? C58 H58 0.9500 . ? C59 H59 0.9500 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.504(5) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C67 1.379(5) . ? C62 C63 1.404(5) . ? C63 C64 1.385(5) . ? C63 H63 0.9500 . ? C64 C65 1.388(5) . ? C64 H64 0.9500 . ? C65 C66 1.403(6) . ? C66 C67 1.388(5) . ? C66 H66 0.9500 . ? C67 H67 0.9500 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? O9 C69 1.384(8) . ? O9 H9 0.8400 . ? C69 C70 1.374(6) . ? C69 C73 1.422(6) 2_666 ? C70 C71 1.419(6) . ? C70 H70 0.9500 . ? C71 C72 1.402(6) . ? C71 C71 1.446(8) 2_666 ? C72 C73 1.375(6) . ? C72 H72 0.9500 . ? C73 C69 1.422(6) 2_666 ? C73 H73 0.9500 . ? Cl7 C75 1.752(4) . ? O10 C74 1.372(6) . ? O10 H10 0.8400 . ? C74 C75 1.372(7) . ? C74 C83 1.415(7) . ? C75 C76 1.418(7) . ? C76 C77 1.400(7) . ? C76 C81 1.424(6) . ? C77 C78 1.332(8) . ? C77 H77 0.9500 . ? C78 C79 1.407(8) . ? C78 H78 0.9500 . ? C79 C80 1.378(8) . ? C79 H79 0.9500 . ? C80 C81 1.429(7) . ? C80 H80 0.9500 . ? C81 C82 1.404(7) . ? C82 C83 1.360(7) . ? C82 H82 0.9500 . ? C83 H83 0.9500 . ? O11 C84 1.386(7) . ? O11 H11A 0.8400 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? 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 Cl1 Cu1 Cl3 126.83(5) . . ? Cl1 Cu1 Cl4 103.79(5) . . ? Cl3 Cu1 Cl4 101.65(6) . . ? Cl1 Cu1 Cl2 99.10(5) . . ? Cl3 Cu1 Cl2 100.88(5) . . ? Cl4 Cu1 Cl2 127.71(5) . . ? C5 O1 C8 117.3(4) . . ? C13 O2 C16 117.1(4) . . ? C23 O3 C26 117.0(4) . . ? C31 O4 C34 118.3(4) . . ? C39 O5 C42 117.3(4) . . ? C47 O6 C50 116.8(4) . . ? C57 O7 C60 117.1(5) . . ? C65 O8 C68 117.2(3) . . ? C17 N1 C1 113.1(3) . . ? C17 N1 C9 109.2(3) . . ? C1 N1 C9 110.1(3) . . ? C17 N1 H1 108.1 . . ? C1 N1 H1 108.1 . . ? C9 N1 H1 108.1 . . ? C18 N2 C19 113.5(3) . . ? C18 N2 C27 111.0(3) . . ? C19 N2 C27 108.6(3) . . ? C18 N2 H2 107.9 . . ? C19 N2 H2 107.9 . . ? C27 N2 H2 107.9 . . ? C51 N3 C43 113.4(3) . . ? C51 N3 C35 108.0(3) . . ? C43 N3 C35 110.7(3) . . ? C51 N3 H3 108.2 . . ? C43 N3 H3 108.2 . . ? C35 N3 H3 108.2 . . ? C52 N4 C53 110.9(3) . . ? C52 N4 C61 113.9(3) . . ? C53 N4 C61 106.9(3) . . ? C52 N4 H4 108.4 . . ? C53 N4 H4 108.4 . . ? C61 N4 H4 108.4 . . ? C2 C1 N1 113.5(3) . . ? C2 C1 H1A 108.9 . . ? N1 C1 H1A 108.9 . . ? C2 C1 H1B 108.9 . . ? N1 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? C3 C2 C7 118.3(4) . . ? C3 C2 C1 120.1(4) . . ? C7 C2 C1 121.6(4) . . ? C2 C3 C4 121.6(4) . . ? C2 C3 H3A 119.2 . . ? C4 C3 H3A 119.2 . . ? C5 C4 C3 118.7(4) . . ? C5 C4 H4A 120.7 . . ? C3 C4 H4A 120.7 . . ? O1 C5 C6 114.7(4) . . ? O1 C5 C4 125.0(4) . . ? C6 C5 C4 120.2(4) . . ? C7 C6 C5 120.8(4) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C7 C2 120.2(4) . . ? C6 C7 H7 119.9 . . ? C2 C7 H7 119.9 . . ? O1 C8 H8A 109.5 . . ? O1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 N1 114.2(3) . . ? C10 C9 H9A 108.7 . . ? N1 C9 H9A 108.7 . . ? C10 C9 H9B 108.7 . . ? N1 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? C11 C10 C15 118.7(3) . . ? C11 C10 C9 121.7(3) . . ? C15 C10 C9 119.4(4) . . ? C10 C11 C12 120.6(4) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C13 C12 C11 119.2(4) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C14 C13 O2 115.5(4) . . ? C14 C13 C12 120.8(4) . . ? O2 C13 C12 123.6(4) . . ? C13 C14 C15 119.7(4) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C14 C15 C10 121.0(4) . . ? C14 C15 H15 119.5 . . ? C10 C15 H15 119.5 . . ? O2 C16 H16A 109.5 . . ? O2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 N1 116.1(3) . . ? C18 C17 H17A 108.2 . . ? N1 C17 H17A 108.2 . . ? C18 C17 H17B 108.2 . . ? N1 C17 H17B 108.2 . . ? H17A C17 H17B 107.4 . . ? N2 C18 C17 115.8(3) . . ? N2 C18 H18A 108.3 . . ? C17 C18 H18A 108.3 . . ? N2 C18 H18B 108.3 . . ? C17 C18 H18B 108.3 . . ? H18A C18 H18B 107.4 . . ? C20 C19 N2 114.3(3) . . ? C20 C19 H19A 108.7 . . ? N2 C19 H19A 108.7 . . ? C20 C19 H19B 108.7 . . ? N2 C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? C25 C20 C21 117.6(4) . . ? C25 C20 C19 121.4(4) . . ? C21 C20 C19 121.0(4) . . ? C22 C21 C20 121.3(4) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C23 120.3(4) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? O3 C23 C22 115.3(4) . . ? O3 C23 C24 124.8(4) . . ? C22 C23 C24 119.9(4) . . ? C25 C24 C23 118.9(4) . . ? C25 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? C20 C25 C24 122.0(4) . . ? C20 C25 H25 119.0 . . ? C24 C25 H25 119.0 . . ? O3 C26 H26A 109.5 . . ? O3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 N2 113.6(3) . . ? C28 C27 H27A 108.8 . . ? N2 C27 H27A 108.8 . . ? C28 C27 H27B 108.8 . . ? N2 C27 H27B 108.8 . . ? H27A C27 H27B 107.7 . . ? C29 C28 C33 116.8(4) . . ? C29 C28 C27 121.4(4) . . ? C33 C28 C27 121.8(4) . . ? C30 C29 C28 121.7(4) . . ? C30 C29 H29 119.1 . . ? C28 C29 H29 119.1 . . ? C29 C30 C31 119.9(4) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? O4 C31 C32 124.8(4) . . ? O4 C31 C30 115.7(4) . . ? C32 C31 C30 119.4(5) . . ? C33 C32 C31 120.0(4) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C28 122.1(4) . . ? C32 C33 H33 119.0 . . ? C28 C33 H33 119.0 . . ? O4 C34 H34A 109.5 . . ? O4 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O4 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 N3 112.8(3) . . ? C36 C35 H35A 109.0 . . ? N3 C35 H35A 109.0 . . ? C36 C35 H35B 109.0 . . ? N3 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? C41 C36 C37 119.1(4) . . ? C41 C36 C35 121.0(3) . . ? C37 C36 C35 119.7(3) . . ? C38 C37 C36 120.7(4) . . ? C38 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? C39 C38 C37 119.9(4) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 O5 115.0(4) . . ? C38 C39 C40 121.1(4) . . ? O5 C39 C40 123.9(4) . . ? C39 C40 C41 118.5(4) . . ? C39 C40 H40 120.7 . . ? C41 C40 H40 120.7 . . ? C36 C41 C40 120.7(4) . . ? C36 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? O5 C42 H42A 109.5 . . ? O5 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? O5 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 N3 112.6(3) . . ? C44 C43 H43A 109.1 . . ? N3 C43 H43A 109.1 . . ? C44 C43 H43B 109.1 . . ? N3 C43 H43B 109.1 . . ? H43A C43 H43B 107.8 . . ? C45 C44 C49 117.9(4) . . ? C45 C44 C43 121.9(4) . . ? C49 C44 C43 120.1(4) . . ? C44 C45 C46 122.2(4) . . ? C44 C45 H45 118.9 . . ? C46 C45 H45 118.9 . . ? C47 C46 C45 118.8(4) . . ? C47 C46 H46 120.6 . . ? C45 C46 H46 120.6 . . ? C46 C47 C48 119.6(4) . . ? C46 C47 O6 125.1(4) . . ? C48 C47 O6 115.3(4) . . ? C47 C48 C49 120.5(5) . . ? C47 C48 H48 119.7 . . ? C49 C48 H48 119.7 . . ? C44 C49 C48 120.8(5) . . ? C44 C49 H49 119.6 . . ? C48 C49 H49 119.6 . . ? O6 C50 H50A 109.5 . . ? O6 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? O6 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N3 C51 C52 116.8(3) . . ? N3 C51 H51A 108.1 . . ? C52 C51 H51A 108.1 . . ? N3 C51 H51B 108.1 . . ? C52 C51 H51B 108.1 . . ? H51A C51 H51B 107.3 . . ? N4 C52 C51 116.4(3) . . ? N4 C52 H52A 108.2 . . ? C51 C52 H52A 108.2 . . ? N4 C52 H52B 108.2 . . ? C51 C52 H52B 108.2 . . ? H52A C52 H52B 107.3 . . ? C54 C53 N4 113.6(3) . . ? C54 C53 H53A 108.9 . . ? N4 C53 H53A 108.9 . . ? C54 C53 H53B 108.9 . . ? N4 C53 H53B 108.9 . . ? H53A C53 H53B 107.7 . . ? C55 C54 C59 118.6(4) . . ? C55 C54 C53 119.9(3) . . ? C59 C54 C53 121.4(3) . . ? C54 C55 C56 121.2(4) . . ? C54 C55 H55 119.4 . . ? C56 C55 H55 119.4 . . ? C57 C56 C55 118.5(4) . . ? C57 C56 H56 120.8 . . ? C55 C56 H56 120.8 . . ? O7 C57 C56 123.4(4) . . ? O7 C57 C58 115.9(4) . . ? C56 C57 C58 120.7(4) . . ? C59 C58 C57 120.2(4) . . ? C59 C58 H58 119.9 . . ? C57 C58 H58 119.9 . . ? C58 C59 C54 120.7(4) . . ? C58 C59 H59 119.6 . . ? C54 C59 H59 119.6 . . ? O7 C60 H60A 109.5 . . ? O7 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? O7 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C62 C61 N4 113.7(3) . . ? C62 C61 H61A 108.8 . . ? N4 C61 H61A 108.8 . . ? C62 C61 H61B 108.8 . . ? N4 C61 H61B 108.8 . . ? H61A C61 H61B 107.7 . . ? C67 C62 C63 118.9(3) . . ? C67 C62 C61 119.8(3) . . ? C63 C62 C61 121.2(3) . . ? C64 C63 C62 119.9(4) . . ? C64 C63 H63 120.0 . . ? C62 C63 H63 120.0 . . ? C63 C64 C65 120.5(4) . . ? C63 C64 H64 119.8 . . ? C65 C64 H64 119.8 . . ? O8 C65 C64 115.6(3) . . ? O8 C65 C66 124.4(3) . . ? C64 C65 C66 120.1(3) . . ? C67 C66 C65 118.6(4) . . ? C67 C66 H66 120.7 . . ? C65 C66 H66 120.7 . . ? C62 C67 C66 122.0(4) . . ? C62 C67 H67 119.0 . . ? C66 C67 H67 119.0 . . ? O8 C68 H68A 109.5 . . ? O8 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? O8 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C69 O9 H9 109.5 . . ? C70 C69 O9 126.5(5) . . ? C70 C69 C73 119.5(4) . 2_666 ? O9 C69 C73 113.8(5) . 2_666 ? C69 C70 C71 121.3(4) . . ? C69 C70 H70 119.4 . . ? C71 C70 H70 119.4 . . ? C72 C71 C70 123.0(4) . . ? C72 C71 C71 118.1(5) . 2_666 ? C70 C71 C71 118.9(5) . 2_666 ? C73 C72 C71 121.9(4) . . ? C73 C72 H72 119.1 . . ? C71 C72 H72 119.1 . . ? C72 C73 C69 120.3(4) . 2_666 ? C72 C73 H73 119.9 . . ? C69 C73 H73 119.9 2_666 . ? C74 O10 H10 109.5 . . ? C75 C74 O10 119.6(4) . . ? C75 C74 C83 118.7(4) . . ? O10 C74 C83 121.7(4) . . ? C74 C75 C76 123.3(4) . . ? C74 C75 Cl7 117.2(4) . . ? C76 C75 Cl7 119.4(3) . . ? C77 C76 C75 124.8(4) . . ? C77 C76 C81 119.2(5) . . ? C75 C76 C81 116.0(4) . . ? C78 C77 C76 121.2(5) . . ? C78 C77 H77 119.4 . . ? C76 C77 H77 119.4 . . ? C77 C78 C79 121.2(6) . . ? C77 C78 H78 119.4 . . ? C79 C78 H78 119.4 . . ? C80 C79 C78 120.4(5) . . ? C80 C79 H79 119.8 . . ? C78 C79 H79 119.8 . . ? C79 C80 C81 119.1(5) . . ? C79 C80 H80 120.4 . . ? C81 C80 H80 120.4 . . ? C82 C81 C76 120.5(4) . . ? C82 C81 C80 120.7(5) . . ? C76 C81 C80 118.8(4) . . ? C83 C82 C81 121.2(4) . . ? C83 C82 H82 119.4 . . ? C81 C82 H82 119.4 . . ? C82 C83 C74 120.3(4) . . ? C82 C83 H83 119.9 . . ? C74 C83 H83 119.9 . . ? C84 O11 H11A 109.5 . . ? O11 C84 H84A 109.5 . . ? O11 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? O11 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C17 N1 C1 C2 -172.1(3) . . . . ? C9 N1 C1 C2 -49.7(4) . . . . ? N1 C1 C2 C3 126.6(4) . . . . ? N1 C1 C2 C7 -52.7(5) . . . . ? C7 C2 C3 C4 -2.4(6) . . . . ? C1 C2 C3 C4 178.2(4) . . . . ? C2 C3 C4 C5 2.8(6) . . . . ? C8 O1 C5 C6 -170.5(4) . . . . ? C8 O1 C5 C4 10.8(6) . . . . ? C3 C4 C5 O1 178.3(4) . . . . ? C3 C4 C5 C6 -0.2(6) . . . . ? O1 C5 C6 C7 178.8(4) . . . . ? C4 C5 C6 C7 -2.5(7) . . . . ? C5 C6 C7 C2 2.9(7) . . . . ? C3 C2 C7 C6 -0.4(6) . . . . ? C1 C2 C7 C6 178.9(4) . . . . ? C17 N1 C9 C10 -57.6(4) . . . . ? C1 N1 C9 C10 177.7(3) . . . . ? N1 C9 C10 C11 -81.8(4) . . . . ? N1 C9 C10 C15 103.5(4) . . . . ? C15 C10 C11 C12 0.1(6) . . . . ? C9 C10 C11 C12 -174.6(3) . . . . ? C10 C11 C12 C13 0.2(6) . . . . ? C16 O2 C13 C14 -176.4(5) . . . . ? C16 O2 C13 C12 5.3(6) . . . . ? C11 C12 C13 C14 -0.5(6) . . . . ? C11 C12 C13 O2 177.7(4) . . . . ? O2 C13 C14 C15 -177.8(4) . . . . ? C12 C13 C14 C15 0.4(6) . . . . ? C13 C14 C15 C10 -0.1(6) . . . . ? C11 C10 C15 C14 -0.2(6) . . . . ? C9 C10 C15 C14 174.7(4) . . . . ? C1 N1 C17 C18 -49.0(4) . . . . ? C9 N1 C17 C18 -172.0(3) . . . . ? C19 N2 C18 C17 -90.2(4) . . . . ? C27 N2 C18 C17 147.2(3) . . . . ? N1 C17 C18 N2 -70.4(4) . . . . ? C18 N2 C19 C20 57.2(4) . . . . ? C27 N2 C19 C20 -178.9(3) . . . . ? N2 C19 C20 C25 -97.3(4) . . . . ? N2 C19 C20 C21 85.1(5) . . . . ? C25 C20 C21 C22 0.6(6) . . . . ? C19 C20 C21 C22 178.3(4) . . . . ? C20 C21 C22 C23 0.3(6) . . . . ? C26 O3 C23 C22 -177.5(4) . . . . ? C26 O3 C23 C24 3.5(7) . . . . ? C21 C22 C23 O3 -178.4(4) . . . . ? C21 C22 C23 C24 0.6(6) . . . . ? O3 C23 C24 C25 176.7(4) . . . . ? C22 C23 C24 C25 -2.3(6) . . . . ? C21 C20 C25 C24 -2.3(6) . . . . ? C19 C20 C25 C24 179.9(4) . . . . ? C23 C24 C25 C20 3.2(7) . . . . ? C18 N2 C27 C28 -62.1(4) . . . . ? C19 N2 C27 C28 172.5(3) . . . . ? N2 C27 C28 C29 99.6(4) . . . . ? N2 C27 C28 C33 -79.9(5) . . . . ? C33 C28 C29 C30 2.3(6) . . . . ? C27 C28 C29 C30 -177.2(4) . . . . ? C28 C29 C30 C31 -1.2(6) . . . . ? C34 O4 C31 C32 6.2(7) . . . . ? C34 O4 C31 C30 -173.9(4) . . . . ? C29 C30 C31 O4 179.4(4) . . . . ? C29 C30 C31 C32 -0.7(7) . . . . ? O4 C31 C32 C33 -178.7(4) . . . . ? C30 C31 C32 C33 1.4(7) . . . . ? C31 C32 C33 C28 -0.2(7) . . . . ? C29 C28 C33 C32 -1.6(6) . . . . ? C27 C28 C33 C32 177.9(4) . . . . ? C51 N3 C35 C36 62.0(4) . . . . ? C43 N3 C35 C36 -173.2(3) . . . . ? N3 C35 C36 C41 -115.9(4) . . . . ? N3 C35 C36 C37 68.6(4) . . . . ? C41 C36 C37 C38 1.3(5) . . . . ? C35 C36 C37 C38 176.9(3) . . . . ? C36 C37 C38 C39 0.0(6) . . . . ? C37 C38 C39 O5 178.0(3) . . . . ? C37 C38 C39 C40 -1.5(6) . . . . ? C42 O5 C39 C38 172.5(4) . . . . ? C42 O5 C39 C40 -8.0(6) . . . . ? C38 C39 C40 C41 1.8(6) . . . . ? O5 C39 C40 C41 -177.7(3) . . . . ? C37 C36 C41 C40 -1.0(5) . . . . ? C35 C36 C41 C40 -176.5(3) . . . . ? C39 C40 C41 C36 -0.5(5) . . . . ? C51 N3 C43 C44 171.4(3) . . . . ? C35 N3 C43 C44 49.8(4) . . . . ? N3 C43 C44 C45 -113.1(4) . . . . ? N3 C43 C44 C49 63.3(6) . . . . ? C49 C44 C45 C46 2.8(7) . . . . ? C43 C44 C45 C46 179.2(4) . . . . ? C44 C45 C46 C47 -1.0(7) . . . . ? C45 C46 C47 C48 -2.9(8) . . . . ? C45 C46 C47 O6 179.8(5) . . . . ? C50 O6 C47 C46 -4.7(7) . . . . ? C50 O6 C47 C48 177.9(6) . . . . ? C46 C47 C48 C49 5.0(11) . . . . ? O6 C47 C48 C49 -177.5(7) . . . . ? C45 C44 C49 C48 -0.7(10) . . . . ? C43 C44 C49 C48 -177.2(6) . . . . ? C47 C48 C49 C44 -3.2(12) . . . . ? C43 N3 C51 C52 46.0(4) . . . . ? C35 N3 C51 C52 169.1(3) . . . . ? C53 N4 C52 C51 -152.3(3) . . . . ? C61 N4 C52 C51 87.2(4) . . . . ? N3 C51 C52 N4 76.0(4) . . . . ? C52 N4 C53 C54 60.9(4) . . . . ? C61 N4 C53 C54 -174.4(3) . . . . ? N4 C53 C54 C55 -101.8(4) . . . . ? N4 C53 C54 C59 78.5(4) . . . . ? C59 C54 C55 C56 -0.6(6) . . . . ? C53 C54 C55 C56 179.7(4) . . . . ? C54 C55 C56 C57 0.1(6) . . . . ? C60 O7 C57 C56 11.7(9) . . . . ? C60 O7 C57 C58 -170.6(6) . . . . ? C55 C56 C57 O7 178.7(5) . . . . ? C55 C56 C57 C58 1.1(7) . . . . ? O7 C57 C58 C59 -179.6(4) . . . . ? C56 C57 C58 C59 -1.9(8) . . . . ? C57 C58 C59 C54 1.4(7) . . . . ? C55 C54 C59 C58 -0.1(6) . . . . ? C53 C54 C59 C58 179.5(4) . . . . ? C52 N4 C61 C62 -45.6(4) . . . . ? C53 N4 C61 C62 -168.4(3) . . . . ? N4 C61 C62 C67 93.0(4) . . . . ? N4 C61 C62 C63 -84.4(4) . . . . ? C67 C62 C63 C64 -1.2(5) . . . . ? C61 C62 C63 C64 176.3(3) . . . . ? C62 C63 C64 C65 -0.9(6) . . . . ? C68 O8 C65 C64 175.4(3) . . . . ? C68 O8 C65 C66 -5.8(5) . . . . ? C63 C64 C65 O8 -178.4(3) . . . . ? C63 C64 C65 C66 2.7(6) . . . . ? O8 C65 C66 C67 178.9(3) . . . . ? C64 C65 C66 C67 -2.3(5) . . . . ? C63 C62 C67 C66 1.6(6) . . . . ? C61 C62 C67 C66 -175.9(3) . . . . ? C65 C66 C67 C62 0.2(6) . . . . ? O9 C69 C70 C71 176.4(5) . . . . ? C73 C69 C70 C71 0.2(6) 2_666 . . . ? C69 C70 C71 C72 -180.0(4) . . . . ? C69 C70 C71 C71 -0.1(7) . . . 2_666 ? C70 C71 C72 C73 -179.8(4) . . . . ? C71 C71 C72 C73 0.3(7) 2_666 . . . ? C71 C72 C73 C69 -0.4(6) . . . 2_666 ? O10 C74 C75 C76 178.7(4) . . . . ? C83 C74 C75 C76 0.0(7) . . . . ? O10 C74 C75 Cl7 -2.7(6) . . . . ? C83 C74 C75 Cl7 178.6(3) . . . . ? C74 C75 C76 C77 -179.5(5) . . . . ? Cl7 C75 C76 C77 2.0(6) . . . . ? C74 C75 C76 C81 -0.3(7) . . . . ? Cl7 C75 C76 C81 -178.9(3) . . . . ? C75 C76 C77 C78 179.6(5) . . . . ? C81 C76 C77 C78 0.4(8) . . . . ? C76 C77 C78 C79 0.1(9) . . . . ? C77 C78 C79 C80 0.2(9) . . . . ? C78 C79 C80 C81 -0.9(8) . . . . ? C77 C76 C81 C82 -179.9(4) . . . . ? C75 C76 C81 C82 0.9(6) . . . . ? C77 C76 C81 C80 -1.1(7) . . . . ? C75 C76 C81 C80 179.6(4) . . . . ? C79 C80 C81 C82 -179.8(5) . . . . ? C79 C80 C81 C76 1.4(7) . . . . ? C76 C81 C82 C83 -1.1(7) . . . . ? C80 C81 C82 C83 -179.9(4) . . . . ? C81 C82 C83 C74 0.8(7) . . . . ? C75 C74 C83 C82 -0.2(7) . . . . ? O10 C74 C83 C82 -178.9(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 Cl6 0.93 2.20 3.103(3) 164.3 . N2 H2 Cl6 0.93 2.13 3.063(3) 177.3 . N3 H3 Cl5 0.93 2.20 3.093(3) 159.6 . N4 H4 Cl5 0.93 2.15 3.076(3) 175.7 . O9 H9 O11 0.84 1.97 2.709(8) 147.1 . O10 H10 Cl2 0.84 2.25 3.089(4) 177.9 . O11 H11A Cl4 0.84 2.42 3.227(5) 160.7 . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.799 _refine_diff_density_min -0.531 _refine_diff_density_rms 0.085