# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Jason Love' _publ_contact_author_email jason.love@ed.ac.uk _publ_author_name J.Love data_[Pd(HL1)] _database_code_depnum_ccdc_archive 'CCDC 866705' #TrackingRef '- revised_combined.cif' # local name j11026 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H46 N6 Pd' _chemical_formula_sum 'C35 H46 N6 Pd' _chemical_formula_weight 657.18 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' Pd Pd -0.9988 1.0072 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6995(6) _cell_length_b 13.0619(7) _cell_length_c 13.1928(7) _cell_angle_alpha 115.965(5) _cell_angle_beta 113.289(5) _cell_angle_gamma 94.036(4) _cell_volume 1590.89(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8599 _cell_measurement_theta_min 2.9934 _cell_measurement_theta_max 29.1225 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.917 _exptl_crystal_size_mid 0.136 _exptl_crystal_size_min 0.082 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.617 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.81774 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro; Agilent Technologies, 2010 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1042 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35168 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 29.18 _reflns_number_total 7757 _reflns_number_gt 6644 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0222P)^2^+0.8003P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7757 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0444 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0659 _refine_ls_wR_factor_gt 0.0615 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 C1 C 0.3975(2) 0.8972(2) 0.7937(2) 0.0320(5) Uani 1 1 d . . . H1A H 0.4253 0.9845 0.8393 0.048 Uiso 1 1 calc R . . H1B H 0.4356 0.8701 0.8547 0.048 Uiso 1 1 calc R . . H1C H 0.3023 0.8680 0.7518 0.048 Uiso 1 1 calc R . . C2 C 0.44347(19) 0.84868(19) 0.69186(19) 0.0220(4) Uani 1 1 d . . . C3 C 0.39590(19) 0.90164(18) 0.60514(19) 0.0211(4) Uani 1 1 d . . . C4 C 0.3857(2) 1.01675(19) 0.6368(2) 0.0248(5) Uani 1 1 d . . . H4 H 0.4019 1.0782 0.7186 0.030 Uiso 1 1 calc R . . C5 C 0.3477(2) 1.02504(19) 0.5271(2) 0.0243(4) Uani 1 1 d . . . H5 H 0.3332 1.0927 0.5197 0.029 Uiso 1 1 calc R . . C6 C 0.33531(19) 0.91473(18) 0.43042(19) 0.0203(4) Uani 1 1 d . . . C7 C 0.29334(19) 0.85726(18) 0.29687(19) 0.0215(4) Uani 1 1 d . . . H7 H 0.2721 0.9003 0.2530 0.026 Uiso 1 1 calc R . . C8 C 0.2397(2) 0.68574(18) 0.09637(19) 0.0220(4) Uani 1 1 d . . . H8 H 0.2283 0.5987 0.0640 0.026 Uiso 1 1 calc R . . C9 C 0.1091(2) 0.6986(2) 0.0222(2) 0.0323(5) Uani 1 1 d . . . H9A H 0.1160 0.7841 0.0541 0.039 Uiso 1 1 calc R . . H9B H 0.0423 0.6644 0.0363 0.039 Uiso 1 1 calc R . . C10 C 0.0671(2) 0.6343(2) -0.1217(2) 0.0429(6) Uani 1 1 d . . . H10A H 0.0515 0.5476 -0.1553 0.051 Uiso 1 1 calc R . . H10B H -0.0155 0.6473 -0.1675 0.051 Uiso 1 1 calc R . . C11 C 0.1703(3) 0.6793(3) -0.1466(2) 0.0463(7) Uani 1 1 d . . . H11A H 0.1791 0.7640 -0.1216 0.056 Uiso 1 1 calc R . . H11B H 0.1429 0.6332 -0.2394 0.056 Uiso 1 1 calc R . . C12 C 0.3003(3) 0.6678(3) -0.0726(2) 0.0416(6) Uani 1 1 d . . . H12A H 0.3666 0.7027 -0.0865 0.050 Uiso 1 1 calc R . . H12B H 0.2942 0.5823 -0.1050 0.050 Uiso 1 1 calc R . . C13 C 0.3429(2) 0.7307(2) 0.0706(2) 0.0292(5) Uani 1 1 d . . . H13A H 0.4253 0.7168 0.1155 0.035 Uiso 1 1 calc R . . H13B H 0.3593 0.8176 0.1051 0.035 Uiso 1 1 calc R . . C14 C 0.40049(19) 0.71302(19) 0.62023(19) 0.0220(4) Uani 1 1 d . . . C15 C 0.3915(2) 0.6357(2) 0.6657(2) 0.0272(5) Uani 1 1 d . . . H15 H 0.4046 0.6584 0.7494 0.033 Uiso 1 1 calc R . . C16 C 0.3597(2) 0.5194(2) 0.5670(2) 0.0284(5) Uani 1 1 d . . . H16 H 0.3472 0.4485 0.5703 0.034 Uiso 1 1 calc R . . C17 C 0.3502(2) 0.52798(19) 0.4629(2) 0.0231(4) Uani 1 1 d . . . C18 C 0.31460(19) 0.44891(19) 0.3325(2) 0.0240(4) Uani 1 1 d . . . H18 H 0.2991 0.3656 0.2999 0.029 Uiso 1 1 calc R . . C19 C 0.2702(2) 0.41522(18) 0.1237(2) 0.0237(4) Uani 1 1 d . . . H19 H 0.1939 0.4322 0.0711 0.028 Uiso 1 1 calc R . . C20 C 0.3831(2) 0.4491(2) 0.1023(2) 0.0272(5) Uani 1 1 d . . . H20A H 0.4052 0.5353 0.1318 0.033 Uiso 1 1 calc R . . H20B H 0.4608 0.4337 0.1534 0.033 Uiso 1 1 calc R . . C21 C 0.3469(2) 0.3773(2) -0.0395(2) 0.0369(6) Uani 1 1 d . . . H21A H 0.2756 0.3997 -0.0890 0.044 Uiso 1 1 calc R . . H21B H 0.4231 0.3973 -0.0501 0.044 Uiso 1 1 calc R . . C22 C 0.3040(3) 0.2439(2) -0.0924(3) 0.0423(6) Uani 1 1 d . . . H22A H 0.3788 0.2194 -0.0511 0.051 Uiso 1 1 calc R . . H22B H 0.2745 0.2008 -0.1857 0.051 Uiso 1 1 calc R . . C23 C 0.1940(3) 0.2107(2) -0.0684(2) 0.0406(6) Uani 1 1 d . . . H23A H 0.1719 0.1245 -0.0984 0.049 Uiso 1 1 calc R . . H23B H 0.1158 0.2264 -0.1183 0.049 Uiso 1 1 calc R . . C24 C 0.2314(2) 0.28146(19) 0.0735(2) 0.0313(5) Uani 1 1 d . . . H24A H 0.3050 0.2609 0.1229 0.038 Uiso 1 1 calc R . . H24B H 0.1567 0.2599 0.0855 0.038 Uiso 1 1 calc R . . C25 C 0.5916(2) 0.88892(18) 0.75786(19) 0.0217(4) Uani 1 1 d . . . C26 C 0.6835(2) 0.96460(19) 0.8845(2) 0.0268(5) Uani 1 1 d . . . H26 H 0.6668 1.0048 0.9546 0.032 Uiso 1 1 calc R . . C27 C 0.8072(2) 0.97096(19) 0.8900(2) 0.0289(5) Uani 1 1 d . . . H27 H 0.8888 1.0168 0.9650 0.035 Uiso 1 1 calc R . . C28 C 0.7890(2) 0.89953(19) 0.7684(2) 0.0251(5) Uani 1 1 d . . . C29 C 0.8805(2) 0.8755(2) 0.7190(2) 0.0279(5) Uani 1 1 d . . . H29 H 0.9707 0.9140 0.7768 0.033 Uiso 1 1 calc R . . C30 C 0.9463(2) 0.7923(2) 0.5616(2) 0.0325(5) Uani 1 1 d . . . H30 H 1.0333 0.8418 0.6385 0.039 Uiso 1 1 calc R . . C31 C 0.9216(2) 0.8369(2) 0.4685(3) 0.0393(6) Uani 1 1 d . . . H31A H 0.9280 0.9226 0.5124 0.047 Uiso 1 1 calc R . . H31B H 0.8321 0.7934 0.3962 0.047 Uiso 1 1 calc R . . C32 C 1.0186(3) 0.8197(2) 0.4165(3) 0.0439(6) Uani 1 1 d . . . H32A H 0.9962 0.8452 0.3524 0.053 Uiso 1 1 calc R . . H32B H 1.1072 0.8702 0.4873 0.053 Uiso 1 1 calc R . . C33 C 1.0172(2) 0.6908(2) 0.3552(3) 0.0441(7) Uani 1 1 d . . . H33A H 0.9312 0.6414 0.2791 0.053 Uiso 1 1 calc R . . H33B H 1.0841 0.6826 0.3265 0.053 Uiso 1 1 calc R . . C34 C 1.0439(2) 0.6467(2) 0.4486(3) 0.0449(7) Uani 1 1 d . . . H34A H 1.1331 0.6913 0.5210 0.054 Uiso 1 1 calc R . . H34B H 1.0388 0.5613 0.4051 0.054 Uiso 1 1 calc R . . C35 C 0.9456(2) 0.6628(2) 0.4999(3) 0.0411(6) Uani 1 1 d . . . H35A H 0.8573 0.6121 0.4286 0.049 Uiso 1 1 calc R . . H35B H 0.9678 0.6370 0.5638 0.049 Uiso 1 1 calc R . . N1 N 0.36607(16) 0.84216(15) 0.48055(16) 0.0203(4) Uani 1 1 d . . . N2 N 0.28433(16) 0.74486(15) 0.23538(16) 0.0208(4) Uani 1 1 d . . . N3 N 0.37753(16) 0.64581(15) 0.49835(16) 0.0216(4) Uani 1 1 d . . . N4 N 0.30364(16) 0.49255(14) 0.25874(16) 0.0211(4) Uani 1 1 d . . . N5 N 0.65690(16) 0.85018(15) 0.68922(17) 0.0228(4) Uani 1 1 d . . . H5A H 0.6197 0.8006 0.6060 0.027 Uiso 1 1 calc R . . N6 N 0.84536(17) 0.80540(17) 0.60213(19) 0.0313(4) Uani 1 1 d . . . Pd1 Pd 0.335291(15) 0.676791(14) 0.358188(15) 0.01823(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0362(13) 0.0418(14) 0.0248(12) 0.0164(11) 0.0204(10) 0.0152(11) C2 0.0225(10) 0.0270(11) 0.0170(10) 0.0101(9) 0.0109(8) 0.0079(9) C3 0.0180(10) 0.0257(11) 0.0189(10) 0.0095(9) 0.0100(8) 0.0081(8) C4 0.0237(11) 0.0230(11) 0.0191(10) 0.0045(9) 0.0095(9) 0.0079(9) C5 0.0242(11) 0.0212(11) 0.0259(11) 0.0107(9) 0.0117(9) 0.0093(9) C6 0.0218(10) 0.0191(10) 0.0200(10) 0.0097(9) 0.0100(8) 0.0079(8) C7 0.0254(11) 0.0216(11) 0.0219(10) 0.0135(9) 0.0118(9) 0.0097(9) C8 0.0281(11) 0.0197(10) 0.0181(10) 0.0087(9) 0.0118(9) 0.0080(9) C9 0.0271(12) 0.0355(13) 0.0249(12) 0.0101(10) 0.0098(10) 0.0101(10) C10 0.0362(14) 0.0451(16) 0.0235(12) 0.0077(11) 0.0042(11) 0.0125(12) C11 0.0593(18) 0.0523(17) 0.0199(12) 0.0171(12) 0.0139(12) 0.0157(14) C12 0.0471(15) 0.0550(17) 0.0277(13) 0.0205(13) 0.0230(12) 0.0144(13) C13 0.0296(12) 0.0363(13) 0.0244(11) 0.0158(10) 0.0148(10) 0.0095(10) C14 0.0189(10) 0.0299(12) 0.0217(10) 0.0148(9) 0.0114(8) 0.0086(9) C15 0.0273(11) 0.0379(13) 0.0272(12) 0.0218(11) 0.0162(10) 0.0112(10) C16 0.0286(11) 0.0325(13) 0.0347(13) 0.0235(11) 0.0171(10) 0.0086(10) C17 0.0229(10) 0.0230(11) 0.0282(11) 0.0158(9) 0.0131(9) 0.0077(9) C18 0.0231(10) 0.0207(11) 0.0292(12) 0.0136(9) 0.0124(9) 0.0070(9) C19 0.0260(11) 0.0205(11) 0.0222(11) 0.0094(9) 0.0106(9) 0.0089(9) C20 0.0286(11) 0.0249(12) 0.0288(12) 0.0130(10) 0.0147(10) 0.0100(9) C21 0.0434(14) 0.0411(15) 0.0320(13) 0.0169(12) 0.0237(12) 0.0199(12) C22 0.0510(16) 0.0368(14) 0.0333(14) 0.0089(12) 0.0237(12) 0.0214(12) C23 0.0470(15) 0.0265(13) 0.0345(14) 0.0062(11) 0.0179(12) 0.0103(11) C24 0.0355(13) 0.0197(11) 0.0310(13) 0.0086(10) 0.0142(10) 0.0067(10) C25 0.0252(10) 0.0237(11) 0.0185(10) 0.0117(9) 0.0109(8) 0.0091(9) C26 0.0320(12) 0.0249(11) 0.0191(11) 0.0102(9) 0.0093(9) 0.0093(9) C27 0.0254(11) 0.0269(12) 0.0249(11) 0.0136(10) 0.0034(9) 0.0048(9) C28 0.0216(10) 0.0247(11) 0.0279(12) 0.0158(10) 0.0081(9) 0.0071(9) C29 0.0198(10) 0.0295(12) 0.0334(13) 0.0184(11) 0.0091(9) 0.0070(9) C30 0.0192(11) 0.0370(14) 0.0368(13) 0.0157(11) 0.0133(10) 0.0058(10) C31 0.0407(14) 0.0363(14) 0.0520(16) 0.0236(13) 0.0295(13) 0.0173(12) C32 0.0422(15) 0.0454(16) 0.0497(17) 0.0221(14) 0.0296(13) 0.0096(12) C33 0.0291(13) 0.0482(16) 0.0416(15) 0.0105(13) 0.0198(12) 0.0073(11) C34 0.0306(13) 0.0404(15) 0.0545(17) 0.0155(13) 0.0209(13) 0.0159(12) C35 0.0332(13) 0.0428(15) 0.0541(17) 0.0280(14) 0.0221(12) 0.0160(12) N1 0.0248(9) 0.0198(9) 0.0178(8) 0.0088(7) 0.0119(7) 0.0092(7) N2 0.0265(9) 0.0201(9) 0.0186(9) 0.0104(7) 0.0120(7) 0.0084(7) N3 0.0252(9) 0.0218(9) 0.0198(9) 0.0115(8) 0.0115(7) 0.0067(7) N4 0.0239(9) 0.0177(9) 0.0217(9) 0.0095(7) 0.0110(7) 0.0075(7) N5 0.0213(9) 0.0260(10) 0.0188(8) 0.0099(7) 0.0092(7) 0.0064(7) N6 0.0221(9) 0.0347(11) 0.0361(11) 0.0169(9) 0.0144(9) 0.0080(8) Pd1 0.02218(8) 0.01766(8) 0.01720(8) 0.00908(6) 0.01098(6) 0.00713(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C2 1.540(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C14 1.523(3) . ? C2 C25 1.521(3) . ? C2 C3 1.530(3) . ? C3 N1 1.348(2) . ? C3 C4 1.401(3) . ? C4 C5 1.393(3) . ? C4 H4 0.9500 . ? C5 C6 1.392(3) . ? C5 H5 0.9500 . ? C6 N1 1.369(2) . ? C6 C7 1.419(3) . ? C7 N2 1.301(3) . ? C7 H7 0.9500 . ? C8 N2 1.476(2) . ? C8 C13 1.522(3) . ? C8 C9 1.522(3) . ? C8 H8 1.0000 . ? C9 C10 1.536(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.515(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.509(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.527(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N3 1.348(3) . ? C14 C15 1.399(3) . ? C15 C16 1.396(3) . ? C15 H15 0.9500 . ? C16 C17 1.388(3) . ? C16 H16 0.9500 . ? C17 N3 1.368(3) . ? C17 C18 1.420(3) . ? C18 N4 1.299(3) . ? C18 H18 0.9500 . ? C19 N4 1.471(3) . ? C19 C24 1.528(3) . ? C19 C20 1.531(3) . ? C19 H19 1.0000 . ? C20 C21 1.529(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.520(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.519(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.528(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 N5 1.364(3) . ? C25 C26 1.381(3) . ? C26 C27 1.415(3) . ? C26 H26 0.9500 . ? C27 C28 1.371(3) . ? C27 H27 0.9500 . ? C28 N5 1.375(3) . ? C28 C29 1.445(3) . ? C29 N6 1.263(3) . ? C29 H29 0.9500 . ? C30 N6 1.468(3) . ? C30 C31 1.518(3) . ? C30 C35 1.520(3) . ? C30 H30 1.0000 . ? C31 C32 1.525(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.511(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.513(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.533(3) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? N1 Pd1 1.9439(16) . ? N2 Pd1 2.0841(16) . ? N3 Pd1 1.9462(16) . ? N4 Pd1 2.0918(16) . ? N5 H5A 0.8800 . ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C14 C2 C25 107.00(16) . . ? C14 C2 C3 113.97(17) . . ? C25 C2 C3 107.13(16) . . ? C14 C2 C1 109.87(17) . . ? C25 C2 C1 109.27(17) . . ? C3 C2 C1 109.45(17) . . ? N1 C3 C4 107.85(18) . . ? N1 C3 C2 122.66(18) . . ? C4 C3 C2 129.27(18) . . ? C5 C4 C3 107.80(18) . . ? C5 C4 H4 126.1 . . ? C3 C4 H4 126.1 . . ? C6 C5 C4 106.50(19) . . ? C6 C5 H5 126.8 . . ? C4 C5 H5 126.8 . . ? N1 C6 C5 108.48(18) . . ? N1 C6 C7 113.64(17) . . ? C5 C6 C7 137.75(19) . . ? N2 C7 C6 119.05(18) . . ? N2 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? N2 C8 C13 110.53(17) . . ? N2 C8 C9 113.05(17) . . ? C13 C8 C9 110.93(18) . . ? N2 C8 H8 107.4 . . ? C13 C8 H8 107.4 . . ? C9 C8 H8 107.4 . . ? C8 C9 C10 110.64(18) . . ? C8 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C11 C10 C9 111.2(2) . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C10 C11 C12 111.4(2) . . ? C10 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? C10 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? C11 C12 C13 111.4(2) . . ? C11 C12 H12A 109.3 . . ? C13 C12 H12A 109.3 . . ? C11 C12 H12B 109.3 . . ? C13 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? C8 C13 C12 111.37(19) . . ? C8 C13 H13A 109.4 . . ? C12 C13 H13A 109.4 . . ? C8 C13 H13B 109.4 . . ? C12 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? N3 C14 C15 107.25(19) . . ? N3 C14 C2 122.89(17) . . ? C15 C14 C2 129.48(19) . . ? C16 C15 C14 108.22(19) . . ? C16 C15 H15 125.9 . . ? C14 C15 H15 125.9 . . ? C17 C16 C15 106.26(19) . . ? C17 C16 H16 126.9 . . ? C15 C16 H16 126.9 . . ? N3 C17 C16 108.46(19) . . ? N3 C17 C18 114.11(18) . . ? C16 C17 C18 137.3(2) . . ? N4 C18 C17 118.79(19) . . ? N4 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? N4 C19 C24 115.39(17) . . ? N4 C19 C20 109.50(17) . . ? C24 C19 C20 110.06(17) . . ? N4 C19 H19 107.2 . . ? C24 C19 H19 107.2 . . ? C20 C19 H19 107.2 . . ? C21 C20 C19 110.77(18) . . ? C21 C20 H20A 109.5 . . ? C19 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 108.1 . . ? C22 C21 C20 111.9(2) . . ? C22 C21 H21A 109.2 . . ? C20 C21 H21A 109.2 . . ? C22 C21 H21B 109.2 . . ? C20 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C21 C22 C23 110.9(2) . . ? C21 C22 H22A 109.5 . . ? C23 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 108.0 . . ? C22 C23 C24 111.5(2) . . ? C22 C23 H23A 109.3 . . ? C24 C23 H23A 109.3 . . ? C22 C23 H23B 109.3 . . ? C24 C23 H23B 109.3 . . ? H23A C23 H23B 108.0 . . ? C23 C24 C19 110.53(19) . . ? C23 C24 H24A 109.5 . . ? C19 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? N5 C25 C26 107.40(18) . . ? N5 C25 C2 120.77(18) . . ? C26 C25 C2 131.83(19) . . ? C25 C26 C27 107.09(19) . . ? C25 C26 H26 126.5 . . ? C27 C26 H26 126.5 . . ? C28 C27 C26 108.22(19) . . ? C28 C27 H27 125.9 . . ? C26 C27 H27 125.9 . . ? C27 C28 N5 106.85(19) . . ? C27 C28 C29 131.5(2) . . ? N5 C28 C29 121.6(2) . . ? N6 C29 C28 122.7(2) . . ? N6 C29 H29 118.6 . . ? C28 C29 H29 118.6 . . ? N6 C30 C31 108.84(18) . . ? N6 C30 C35 110.41(19) . . ? C31 C30 C35 110.7(2) . . ? N6 C30 H30 108.9 . . ? C31 C30 H30 109.0 . . ? C35 C30 H30 109.0 . . ? C30 C31 C32 111.8(2) . . ? C30 C31 H31A 109.3 . . ? C32 C31 H31A 109.3 . . ? C30 C31 H31B 109.3 . . ? C32 C31 H31B 109.3 . . ? H31A C31 H31B 107.9 . . ? C33 C32 C31 110.9(2) . . ? C33 C32 H32A 109.5 . . ? C31 C32 H32A 109.5 . . ? C33 C32 H32B 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 108.1 . . ? C34 C33 C32 111.0(2) . . ? C34 C33 H33A 109.4 . . ? C32 C33 H33A 109.4 . . ? C34 C33 H33B 109.4 . . ? C32 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C33 C34 C35 111.1(2) . . ? C33 C34 H34A 109.4 . . ? C35 C34 H34A 109.4 . . ? C33 C34 H34B 109.4 . . ? C35 C34 H34B 109.4 . . ? H34A C34 H34B 108.0 . . ? C30 C35 C34 110.8(2) . . ? C30 C35 H35A 109.5 . . ? C34 C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 108.1 . . ? C3 N1 C6 109.37(17) . . ? C3 N1 Pd1 134.12(14) . . ? C6 N1 Pd1 115.85(13) . . ? C7 N2 C8 118.62(17) . . ? C7 N2 Pd1 110.91(13) . . ? C8 N2 Pd1 130.45(13) . . ? C14 N3 C17 109.77(17) . . ? C14 N3 Pd1 133.06(14) . . ? C17 N3 Pd1 115.18(14) . . ? C18 N4 C19 121.15(17) . . ? C18 N4 Pd1 110.72(14) . . ? C19 N4 Pd1 128.12(13) . . ? C25 N5 C28 110.44(18) . . ? C25 N5 H5A 124.8 . . ? C28 N5 H5A 124.8 . . ? C29 N6 C30 117.98(19) . . ? N1 Pd1 N3 87.23(7) . . ? N1 Pd1 N2 80.43(7) . . ? N3 Pd1 N2 167.03(7) . . ? N1 Pd1 N4 167.34(7) . . ? N3 Pd1 N4 80.37(7) . . ? N2 Pd1 N4 111.73(7) . . ? 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 C14 C2 C3 N1 -25.0(3) . . . . ? C25 C2 C3 N1 93.1(2) . . . . ? C1 C2 C3 N1 -148.51(19) . . . . ? C14 C2 C3 C4 161.03(19) . . . . ? C25 C2 C3 C4 -80.8(2) . . . . ? C1 C2 C3 C4 37.6(3) . . . . ? N1 C3 C4 C5 0.4(2) . . . . ? C2 C3 C4 C5 175.07(19) . . . . ? C3 C4 C5 C6 0.1(2) . . . . ? C4 C5 C6 N1 -0.5(2) . . . . ? C4 C5 C6 C7 174.8(2) . . . . ? N1 C6 C7 N2 1.9(3) . . . . ? C5 C6 C7 N2 -173.3(2) . . . . ? N2 C8 C9 C10 -179.40(19) . . . . ? C13 C8 C9 C10 55.8(3) . . . . ? C8 C9 C10 C11 -56.0(3) . . . . ? C9 C10 C11 C12 55.8(3) . . . . ? C10 C11 C12 C13 -55.3(3) . . . . ? N2 C8 C13 C12 178.25(18) . . . . ? C9 C8 C13 C12 -55.5(2) . . . . ? C11 C12 C13 C8 55.2(3) . . . . ? C25 C2 C14 N3 -89.5(2) . . . . ? C3 C2 C14 N3 28.7(3) . . . . ? C1 C2 C14 N3 151.99(19) . . . . ? C25 C2 C14 C15 82.6(2) . . . . ? C3 C2 C14 C15 -159.2(2) . . . . ? C1 C2 C14 C15 -36.0(3) . . . . ? N3 C14 C15 C16 -1.2(2) . . . . ? C2 C14 C15 C16 -174.19(19) . . . . ? C14 C15 C16 C17 0.1(2) . . . . ? C15 C16 C17 N3 1.0(2) . . . . ? C15 C16 C17 C18 -175.2(2) . . . . ? N3 C17 C18 N4 -4.0(3) . . . . ? C16 C17 C18 N4 172.1(2) . . . . ? N4 C19 C20 C21 -175.32(17) . . . . ? C24 C19 C20 C21 56.8(2) . . . . ? C19 C20 C21 C22 -55.6(3) . . . . ? C20 C21 C22 C23 54.4(3) . . . . ? C21 C22 C23 C24 -55.2(3) . . . . ? C22 C23 C24 C19 57.2(3) . . . . ? N4 C19 C24 C23 177.85(18) . . . . ? C20 C19 C24 C23 -57.6(2) . . . . ? C14 C2 C25 N5 56.2(2) . . . . ? C3 C2 C25 N5 -66.4(2) . . . . ? C1 C2 C25 N5 175.09(18) . . . . ? C14 C2 C25 C26 -124.7(2) . . . . ? C3 C2 C25 C26 112.7(2) . . . . ? C1 C2 C25 C26 -5.8(3) . . . . ? N5 C25 C26 C27 0.4(2) . . . . ? C2 C25 C26 C27 -178.8(2) . . . . ? C25 C26 C27 C28 -0.3(2) . . . . ? C26 C27 C28 N5 0.1(2) . . . . ? C26 C27 C28 C29 178.3(2) . . . . ? C27 C28 C29 N6 179.6(2) . . . . ? N5 C28 C29 N6 -2.4(3) . . . . ? N6 C30 C31 C32 -176.9(2) . . . . ? C35 C30 C31 C32 -55.4(3) . . . . ? C30 C31 C32 C33 55.7(3) . . . . ? C31 C32 C33 C34 -56.1(3) . . . . ? C32 C33 C34 C35 56.7(3) . . . . ? N6 C30 C35 C34 175.9(2) . . . . ? C31 C30 C35 C34 55.3(3) . . . . ? C33 C34 C35 C30 -56.4(3) . . . . ? C4 C3 N1 C6 -0.8(2) . . . . ? C2 C3 N1 C6 -175.85(17) . . . . ? C4 C3 N1 Pd1 -170.70(14) . . . . ? C2 C3 N1 Pd1 14.2(3) . . . . ? C5 C6 N1 C3 0.8(2) . . . . ? C7 C6 N1 C3 -175.75(17) . . . . ? C5 C6 N1 Pd1 172.80(13) . . . . ? C7 C6 N1 Pd1 -3.8(2) . . . . ? C6 C7 N2 C8 179.56(17) . . . . ? C6 C7 N2 Pd1 0.7(2) . . . . ? C13 C8 N2 C7 70.1(2) . . . . ? C9 C8 N2 C7 -54.9(2) . . . . ? C13 C8 N2 Pd1 -111.31(18) . . . . ? C9 C8 N2 Pd1 123.67(18) . . . . ? C15 C14 N3 C17 1.9(2) . . . . ? C2 C14 N3 C17 175.43(17) . . . . ? C15 C14 N3 Pd1 164.52(15) . . . . ? C2 C14 N3 Pd1 -21.9(3) . . . . ? C16 C17 N3 C14 -1.8(2) . . . . ? C18 C17 N3 C14 175.37(17) . . . . ? C16 C17 N3 Pd1 -167.91(14) . . . . ? C18 C17 N3 Pd1 9.3(2) . . . . ? C17 C18 N4 C19 178.50(17) . . . . ? C17 C18 N4 Pd1 -2.8(2) . . . . ? C24 C19 N4 C18 8.2(3) . . . . ? C20 C19 N4 C18 -116.6(2) . . . . ? C24 C19 N4 Pd1 -170.30(14) . . . . ? C20 C19 N4 Pd1 64.9(2) . . . . ? C26 C25 N5 C28 -0.3(2) . . . . ? C2 C25 N5 C28 179.01(18) . . . . ? C27 C28 N5 C25 0.1(2) . . . . ? C29 C28 N5 C25 -178.29(19) . . . . ? C28 C29 N6 C30 177.0(2) . . . . ? C31 C30 N6 C29 -116.4(2) . . . . ? C35 C30 N6 C29 121.9(2) . . . . ? C3 N1 Pd1 N3 -3.33(19) . . . . ? C6 N1 Pd1 N3 -172.75(14) . . . . ? C3 N1 Pd1 N2 172.66(19) . . . . ? C6 N1 Pd1 N2 3.24(14) . . . . ? C3 N1 Pd1 N4 8.4(4) . . . . ? C6 N1 Pd1 N4 -161.0(3) . . . . ? C14 N3 Pd1 N1 7.14(19) . . . . ? C17 N3 Pd1 N1 169.09(15) . . . . ? C14 N3 Pd1 N2 -10.7(4) . . . . ? C17 N3 Pd1 N2 151.2(3) . . . . ? C14 N3 Pd1 N4 -170.27(19) . . . . ? C17 N3 Pd1 N4 -8.32(14) . . . . ? C7 N2 Pd1 N1 -2.12(14) . . . . ? C8 N2 Pd1 N1 179.22(17) . . . . ? C7 N2 Pd1 N3 16.0(4) . . . . ? C8 N2 Pd1 N3 -162.7(3) . . . . ? C7 N2 Pd1 N4 174.21(13) . . . . ? C8 N2 Pd1 N4 -4.46(18) . . . . ? C18 N4 Pd1 N1 -5.9(4) . . . . ? C19 N4 Pd1 N1 172.7(3) . . . . ? C18 N4 Pd1 N3 5.98(14) . . . . ? C19 N4 Pd1 N3 -175.41(17) . . . . ? C18 N4 Pd1 N2 -169.17(13) . . . . ? C19 N4 Pd1 N2 9.44(18) . . . . ? _diffrn_measured_fraction_theta_max 0.99 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.381 _refine_diff_density_min -0.639 _refine_diff_density_rms 0.073 _vrf_CELLV02_PdHL1 ; PROBLEM: The supplied cell volume s.u. differs from that RESPONSE: checkCIF does not use the full variance/covariance matrix when calculating these values. The value reported in the CIF is correct. ; _vrf_PLAT063_PdHL1 ; PROBLEM: Crystal Size Likely too Large for Beam Size .... 0.92 mm RESPONSE: Gorbitz has shown that this is not a problem. ; data_[Pd(ClH2L1)] _database_code_depnum_ccdc_archive 'CCDC 866706' #TrackingRef '- revised_combined.cif' # local name j11020b(1) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H47 N6 Pd, C H Cl3, Cl' _chemical_formula_sum 'C36 H48 Cl4 N6 Pd' _chemical_formula_weight 813.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' 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 17.130(2) _cell_length_b 11.0690(14) _cell_length_c 20.818(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.888(14) _cell_angle_gamma 90.00 _cell_volume 3734.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5169 _cell_measurement_theta_min 2.9403 _cell_measurement_theta_max 21.9202 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.2380 _exptl_crystal_size_mid 0.1240 _exptl_crystal_size_min 0.1075 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 0.818 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.977 _exptl_absorpt_correction_T_max 0.986 _exptl_absorpt_process_details 'CrysAlisPro, Agilent Technologies, 2010' _exptl_special_details ; The following A alert occurs in the Check CIF: THETM01_ALERT_3_A The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength = 0.5264 This is due to the data only being complete up to 0.95 Angstroms. It was therefore cut to that distance. CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type "Xcalibur, Eos'_diffrn_measurement_method" _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1042 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16832 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_sigmaI/netI 0.0628 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 21.97 _reflns_number_total 4554 _reflns_number_gt 3473 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0327P)^2^+4.2277P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4554 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.0910 _refine_ls_wR_factor_gt 0.0816 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.15205(2) 0.19269(3) 0.253665(19) 0.02133(15) Uani 1 1 d . . . N1 N 0.0605(2) 0.2902(3) 0.26124(19) 0.0228(10) Uani 1 1 d . . . N2 N 0.1966(2) 0.2344(4) 0.3581(2) 0.0231(10) Uani 1 1 d . . . N4 N 0.2354(2) 0.0852(3) 0.2224(2) 0.0219(10) Uani 1 1 d . . . N3 N 0.0905(2) 0.1785(4) 0.15686(19) 0.0218(10) Uani 1 1 d . . . N5 N -0.1025(2) 0.4127(4) 0.0339(2) 0.0244(10) Uani 1 1 d . . . H5N H -0.1320 0.3525 0.0107 0.029 Uiso 1 1 calc R . . N6 N -0.1822(2) 0.4943(4) -0.1084(2) 0.0234(10) Uani 1 1 d . . . H6N H -0.1951 0.4219 -0.0976 0.028 Uiso 1 1 calc R . . Cl1 Cl -0.22028(8) 0.23072(12) -0.07155(7) 0.0379(4) Uani 1 1 d . . . C1 C -0.1276(3) 0.2235(5) 0.1261(3) 0.0300(14) Uani 1 1 d . . . H1A H -0.1671 0.2749 0.1385 0.045 Uiso 1 1 calc R . . H1B H -0.1190 0.1487 0.1526 0.045 Uiso 1 1 calc R . . H1C H -0.1494 0.2041 0.0776 0.045 Uiso 1 1 calc R . . C2 C -0.0440(3) 0.2916(4) 0.1413(2) 0.0234(13) Uani 1 1 d . . . C3 C -0.0131(3) 0.3230(5) 0.2170(2) 0.0239(12) Uani 1 1 d . . . C4 C -0.0534(3) 0.3917(5) 0.2535(3) 0.0343(14) Uani 1 1 d . . . H4 H -0.1066 0.4270 0.2354 0.041 Uiso 1 1 calc R . . C5 C -0.0023(3) 0.3995(5) 0.3207(3) 0.0335(14) Uani 1 1 d . . . H5 H -0.0138 0.4405 0.3567 0.040 Uiso 1 1 calc R . . C6 C 0.0688(3) 0.3354(4) 0.3247(2) 0.0213(12) Uani 1 1 d . . . C7 C 0.1435(3) 0.3008(5) 0.3746(3) 0.0281(13) Uani 1 1 d . . . H7 H 0.1549 0.3262 0.4204 0.034 Uiso 1 1 calc R . . C8 C 0.2740(3) 0.1922(4) 0.4089(2) 0.0256(13) Uani 1 1 d . . . H8 H 0.3201 0.2081 0.3905 0.031 Uiso 1 1 calc R . . C9 C 0.2693(3) 0.0566(5) 0.4186(3) 0.0299(14) Uani 1 1 d . . . H9A H 0.2556 0.0157 0.3740 0.036 Uiso 1 1 calc R . . H9B H 0.2248 0.0385 0.4379 0.036 Uiso 1 1 calc R . . C10 C 0.3517(3) 0.0080(5) 0.4662(3) 0.0447(16) Uani 1 1 d . . . H10A H 0.3470 -0.0800 0.4726 0.054 Uiso 1 1 calc R . . H10B H 0.3954 0.0212 0.4454 0.054 Uiso 1 1 calc R . . C11 C 0.3756(4) 0.0708(5) 0.5348(3) 0.0478(17) Uani 1 1 d . . . H11A H 0.3353 0.0499 0.5580 0.057 Uiso 1 1 calc R . . H11B H 0.4306 0.0421 0.5635 0.057 Uiso 1 1 calc R . . C12 C 0.3777(3) 0.2052(5) 0.5267(3) 0.0455(16) Uani 1 1 d . . . H12A H 0.4226 0.2265 0.5085 0.055 Uiso 1 1 calc R . . H12B H 0.3900 0.2440 0.5718 0.055 Uiso 1 1 calc R . . C13 C 0.2957(3) 0.2539(5) 0.4790(3) 0.0356(14) Uani 1 1 d . . . H13A H 0.2999 0.3422 0.4737 0.043 Uiso 1 1 calc R . . H13B H 0.2513 0.2384 0.4988 0.043 Uiso 1 1 calc R . . C14 C 0.0145(3) 0.2121(4) 0.1171(2) 0.0195(12) Uani 1 1 d . . . C15 C 0.0014(3) 0.1656(4) 0.0520(3) 0.0238(13) Uani 1 1 d . . . H15 H -0.0467 0.1763 0.0137 0.029 Uiso 1 1 calc R . . C16 C 0.0716(3) 0.1009(4) 0.0534(3) 0.0228(12) Uani 1 1 d . . . H16 H 0.0805 0.0591 0.0165 0.027 Uiso 1 1 calc R . . C17 C 0.1259(3) 0.1096(4) 0.1190(3) 0.0215(12) Uani 1 1 d . . . C18 C 0.2038(3) 0.0605(4) 0.1575(3) 0.0255(13) Uani 1 1 d . . . H18 H 0.2328 0.0098 0.1361 0.031 Uiso 1 1 calc R . . C19 C 0.3170(3) 0.0306(4) 0.2607(2) 0.0243(13) Uani 1 1 d . . . H19 H 0.3356 0.0681 0.3069 0.029 Uiso 1 1 calc R . . C20 C 0.3828(3) 0.0567(5) 0.2282(3) 0.0291(14) Uani 1 1 d . . . H20A H 0.3654 0.0224 0.1818 0.035 Uiso 1 1 calc R . . H20B H 0.3885 0.1452 0.2244 0.035 Uiso 1 1 calc R . . C21 C 0.4654(3) 0.0038(5) 0.2688(3) 0.0354(15) Uani 1 1 d . . . H21A H 0.4854 0.0428 0.3140 0.042 Uiso 1 1 calc R . . H21B H 0.5061 0.0200 0.2452 0.042 Uiso 1 1 calc R . . C22 C 0.4580(3) -0.1330(5) 0.2774(3) 0.0402(16) Uani 1 1 d . . . H22A H 0.4431 -0.1729 0.2325 0.048 Uiso 1 1 calc R . . H22B H 0.5117 -0.1658 0.3061 0.048 Uiso 1 1 calc R . . C23 C 0.3924(3) -0.1596(5) 0.3102(3) 0.0371(15) Uani 1 1 d . . . H23A H 0.4105 -0.1266 0.3570 0.045 Uiso 1 1 calc R . . H23B H 0.3863 -0.2482 0.3133 0.045 Uiso 1 1 calc R . . C24 C 0.3095(3) -0.1049(4) 0.2703(3) 0.0269(13) Uani 1 1 d . . . H24A H 0.2695 -0.1198 0.2947 0.032 Uiso 1 1 calc R . . H24B H 0.2883 -0.1445 0.2253 0.032 Uiso 1 1 calc R . . C25 C -0.0559(3) 0.4089(5) 0.1005(2) 0.0201(12) Uani 1 1 d . . . C26 C -0.0208(3) 0.5219(5) 0.1188(3) 0.0260(13) Uani 1 1 d . . . H26 H 0.0136 0.5453 0.1627 0.031 Uiso 1 1 calc R . . C27 C -0.0449(3) 0.5952(5) 0.0612(2) 0.0233(13) Uani 1 1 d . . . H27 H -0.0293 0.6769 0.0585 0.028 Uiso 1 1 calc R . . C28 C -0.0962(3) 0.5262(4) 0.0082(2) 0.0204(12) Uani 1 1 d . . . C29 C -0.1336(3) 0.5603(5) -0.0599(3) 0.0217(12) Uani 1 1 d . . . H29 H -0.1224 0.6397 -0.0718 0.026 Uiso 1 1 calc R . . C30 C -0.2171(3) 0.5316(5) -0.1798(2) 0.0238(13) Uani 1 1 d . . . H30 H -0.1803 0.5948 -0.1890 0.029 Uiso 1 1 calc R . . C31 C -0.3031(3) 0.5867(5) -0.1931(2) 0.0258(13) Uani 1 1 d . . . H31A H -0.2991 0.6586 -0.1640 0.031 Uiso 1 1 calc R . . H31B H -0.3396 0.5271 -0.1816 0.031 Uiso 1 1 calc R . . C32 C -0.3402(3) 0.6231(5) -0.2684(2) 0.0277(13) Uani 1 1 d . . . H32A H -0.3972 0.6529 -0.2769 0.033 Uiso 1 1 calc R . . H32B H -0.3073 0.6900 -0.2781 0.033 Uiso 1 1 calc R . . C33 C -0.3417(3) 0.5187(5) -0.3157(3) 0.0317(14) Uani 1 1 d . . . H33A H -0.3613 0.5478 -0.3633 0.038 Uiso 1 1 calc R . . H33B H -0.3809 0.4565 -0.3108 0.038 Uiso 1 1 calc R . . C34 C -0.2563(3) 0.4626(5) -0.3005(3) 0.0318(14) Uani 1 1 d . . . H34A H -0.2602 0.3911 -0.3300 0.038 Uiso 1 1 calc R . . H34B H -0.2190 0.5217 -0.3113 0.038 Uiso 1 1 calc R . . C35 C -0.2200(3) 0.4245(5) -0.2264(2) 0.0298(14) Uani 1 1 d . . . H35A H -0.2541 0.3594 -0.2166 0.036 Uiso 1 1 calc R . . H35B H -0.1635 0.3926 -0.2179 0.036 Uiso 1 1 calc R . . C50 C -0.4020(3) 0.1537(5) -0.0467(3) 0.0444(16) Uani 1 1 d . . . H50 H -0.3494 0.1667 -0.0569 0.053 Uiso 1 1 calc R . . Cl51 Cl -0.38216(12) 0.17063(17) 0.04058(8) 0.0776(6) Uani 1 1 d . . . Cl52 Cl -0.47456(11) 0.26021(16) -0.09211(9) 0.0716(6) Uani 1 1 d . . . Cl53 Cl -0.43784(10) 0.00775(15) -0.07235(9) 0.0615(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0188(2) 0.0224(3) 0.0208(2) 0.0001(2) 0.00365(17) 0.00102(19) N1 0.025(2) 0.023(3) 0.020(3) 0.000(2) 0.007(2) 0.003(2) N2 0.025(2) 0.023(3) 0.021(2) -0.001(2) 0.007(2) 0.001(2) N4 0.023(2) 0.023(3) 0.020(3) -0.005(2) 0.008(2) -0.0019(19) N3 0.022(2) 0.025(3) 0.017(2) -0.007(2) 0.005(2) -0.005(2) N5 0.021(2) 0.024(3) 0.024(3) -0.004(2) 0.002(2) -0.002(2) N6 0.025(2) 0.019(2) 0.024(3) 0.004(2) 0.004(2) -0.001(2) Cl1 0.0405(8) 0.0331(9) 0.0338(9) -0.0007(7) 0.0035(7) -0.0127(7) C1 0.025(3) 0.030(4) 0.034(3) 0.005(3) 0.009(3) 0.000(2) C2 0.020(3) 0.025(3) 0.025(3) -0.001(3) 0.005(2) -0.002(2) C3 0.027(3) 0.023(3) 0.023(3) 0.004(3) 0.010(3) 0.002(2) C4 0.032(3) 0.033(4) 0.034(4) 0.004(3) 0.005(3) 0.015(3) C5 0.039(3) 0.036(4) 0.028(4) 0.001(3) 0.014(3) 0.013(3) C6 0.024(3) 0.020(3) 0.020(3) 0.002(3) 0.006(2) 0.000(2) C7 0.036(3) 0.025(3) 0.025(3) -0.003(3) 0.012(3) -0.005(3) C8 0.023(3) 0.029(3) 0.023(3) 0.004(3) 0.005(2) 0.003(3) C9 0.030(3) 0.033(4) 0.025(3) -0.004(3) 0.008(3) 0.000(3) C10 0.051(4) 0.048(4) 0.029(4) 0.003(3) 0.005(3) 0.015(3) C11 0.056(4) 0.048(5) 0.027(4) 0.004(3) -0.002(3) 0.019(3) C12 0.039(4) 0.056(5) 0.030(4) -0.007(3) -0.004(3) 0.002(3) C13 0.039(3) 0.035(3) 0.027(3) 0.002(3) 0.002(3) -0.001(3) C14 0.016(3) 0.015(3) 0.023(3) -0.001(3) 0.001(2) -0.004(2) C15 0.022(3) 0.018(3) 0.027(3) 0.004(3) 0.001(2) -0.004(2) C16 0.028(3) 0.015(3) 0.024(3) -0.003(3) 0.007(3) -0.002(2) C17 0.021(3) 0.017(3) 0.024(3) 0.000(3) 0.005(3) 0.002(2) C18 0.027(3) 0.018(3) 0.034(4) -0.007(3) 0.013(3) -0.002(2) C19 0.016(3) 0.032(3) 0.020(3) -0.004(3) 0.000(2) 0.003(2) C20 0.028(3) 0.026(3) 0.037(3) 0.002(3) 0.015(3) 0.005(2) C21 0.023(3) 0.049(4) 0.034(4) 0.005(3) 0.009(3) 0.005(3) C22 0.025(3) 0.061(5) 0.028(3) -0.007(3) 0.001(3) 0.017(3) C23 0.039(3) 0.033(4) 0.035(3) 0.004(3) 0.006(3) 0.011(3) C24 0.029(3) 0.020(3) 0.029(3) -0.002(3) 0.007(3) -0.004(2) C25 0.014(3) 0.026(3) 0.020(3) -0.003(3) 0.005(2) 0.003(2) C26 0.024(3) 0.030(4) 0.021(3) -0.003(3) 0.003(2) -0.001(3) C27 0.022(3) 0.021(3) 0.027(3) 0.000(3) 0.008(3) -0.002(2) C28 0.018(3) 0.017(3) 0.023(3) 0.002(3) 0.002(2) 0.004(2) C29 0.017(3) 0.022(3) 0.026(3) -0.001(3) 0.008(3) 0.000(2) C30 0.025(3) 0.028(3) 0.017(3) 0.005(3) 0.003(2) -0.004(2) C31 0.026(3) 0.024(3) 0.023(3) 0.002(3) 0.001(2) 0.001(2) C32 0.028(3) 0.024(3) 0.028(3) 0.007(3) 0.005(3) 0.007(2) C33 0.027(3) 0.034(4) 0.028(3) -0.001(3) 0.001(3) 0.001(3) C34 0.035(3) 0.031(3) 0.029(3) -0.006(3) 0.008(3) -0.001(3) C35 0.023(3) 0.031(3) 0.030(3) -0.004(3) 0.001(3) 0.003(2) C50 0.041(4) 0.054(4) 0.036(4) -0.001(3) 0.009(3) -0.007(3) Cl51 0.1160(16) 0.0686(13) 0.0286(10) 0.0049(10) -0.0034(10) -0.0272(11) Cl52 0.0855(13) 0.0558(12) 0.0519(11) 0.0062(10) -0.0075(10) 0.0141(10) Cl53 0.0730(12) 0.0484(11) 0.0623(12) -0.0099(10) 0.0208(10) -0.0050(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Pd1 N1 1.952(4) . ? Pd1 N3 1.955(4) . ? Pd1 N2 2.108(4) . ? Pd1 N4 2.116(4) . ? N1 C3 1.348(6) . ? N1 C6 1.377(6) . ? N2 C7 1.301(6) . ? N2 C8 1.478(6) . ? N4 C18 1.311(6) . ? N4 C19 1.495(6) . ? N3 C14 1.348(5) . ? N3 C17 1.370(6) . ? N5 C25 1.359(6) . ? N5 C28 1.383(6) . ? N5 H5N 0.8800 . ? N6 C29 1.305(6) . ? N6 C30 1.471(6) . ? N6 H6N 0.8800 . ? C1 C2 1.558(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C25 1.529(7) . ? C2 C3 1.531(7) . ? C2 C14 1.536(6) . ? C3 C4 1.405(7) . ? C4 C5 1.392(7) . ? C4 H4 0.9500 . ? C5 C6 1.389(6) . ? C5 H5 0.9500 . ? C6 C7 1.415(7) . ? C7 H7 0.9500 . ? C8 C9 1.520(7) . ? C8 C13 1.542(7) . ? C8 H8 1.0000 . ? C9 C10 1.537(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.520(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.499(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.533(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.399(6) . ? C15 C16 1.391(6) . ? C15 H15 0.9500 . ? C16 C17 1.386(6) . ? C16 H16 0.9500 . ? C17 C18 1.423(6) . ? C18 H18 0.9500 . ? C19 C20 1.519(6) . ? C19 C24 1.524(7) . ? C19 H19 1.0000 . ? C20 C21 1.512(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.535(7) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.520(7) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.521(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.388(7) . ? C26 C27 1.395(6) . ? C26 H26 0.9500 . ? C27 C28 1.394(6) . ? C27 H27 0.9500 . ? C28 C29 1.405(6) . ? C29 H29 0.9500 . ? C30 C35 1.523(7) . ? C30 C31 1.535(6) . ? C30 H30 1.0000 . ? C31 C32 1.541(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.514(7) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.525(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.524(7) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C50 Cl51 1.748(6) . ? C50 Cl53 1.749(6) . ? C50 Cl52 1.751(6) . ? C50 H50 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N3 87.03(16) . . ? N1 Pd1 N2 80.12(16) . . ? N3 Pd1 N2 167.10(16) . . ? N1 Pd1 N4 167.23(16) . . ? N3 Pd1 N4 80.20(16) . . ? N2 Pd1 N4 112.64(15) . . ? C3 N1 C6 109.9(4) . . ? C3 N1 Pd1 133.8(3) . . ? C6 N1 Pd1 116.3(3) . . ? C7 N2 C8 122.0(4) . . ? C7 N2 Pd1 110.3(3) . . ? C8 N2 Pd1 127.7(3) . . ? C18 N4 C19 117.9(4) . . ? C18 N4 Pd1 109.9(3) . . ? C19 N4 Pd1 132.1(3) . . ? C14 N3 C17 108.6(4) . . ? C14 N3 Pd1 134.5(3) . . ? C17 N3 Pd1 116.5(3) . . ? C25 N5 C28 109.2(4) . . ? C25 N5 H5N 125.4 . . ? C28 N5 H5N 125.4 . . ? C29 N6 C30 125.0(4) . . ? C29 N6 H6N 117.5 . . ? C30 N6 H6N 117.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C25 C2 C3 108.6(4) . . ? C25 C2 C14 106.8(4) . . ? C3 C2 C14 115.0(4) . . ? C25 C2 C1 110.4(4) . . ? C3 C2 C1 107.9(4) . . ? C14 C2 C1 108.1(4) . . ? N1 C3 C4 106.9(4) . . ? N1 C3 C2 125.2(4) . . ? C4 C3 C2 127.8(4) . . ? C5 C4 C3 108.5(5) . . ? C5 C4 H4 125.7 . . ? C3 C4 H4 125.7 . . ? C6 C5 C4 106.4(5) . . ? C6 C5 H5 126.8 . . ? C4 C5 H5 126.8 . . ? N1 C6 C5 108.2(4) . . ? N1 C6 C7 113.2(4) . . ? C5 C6 C7 138.6(5) . . ? N2 C7 C6 120.1(5) . . ? N2 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? N2 C8 C9 109.4(4) . . ? N2 C8 C13 115.1(4) . . ? C9 C8 C13 108.6(4) . . ? N2 C8 H8 107.8 . . ? C9 C8 H8 107.8 . . ? C13 C8 H8 107.8 . . ? C8 C9 C10 110.7(4) . . ? C8 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C11 C10 C9 111.0(5) . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C12 C11 C10 110.9(5) . . ? C12 C11 H11A 109.5 . . ? C10 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 108.0 . . ? C11 C12 C13 111.8(5) . . ? C11 C12 H12A 109.3 . . ? C13 C12 H12A 109.3 . . ? C11 C12 H12B 109.3 . . ? C13 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? C12 C13 C8 110.3(4) . . ? C12 C13 H13A 109.6 . . ? C8 C13 H13A 109.6 . . ? C12 C13 H13B 109.6 . . ? C8 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? N3 C14 C15 108.3(4) . . ? N3 C14 C2 124.0(4) . . ? C15 C14 C2 127.7(4) . . ? C16 C15 C14 107.6(4) . . ? C16 C15 H15 126.2 . . ? C14 C15 H15 126.2 . . ? C17 C16 C15 106.5(4) . . ? C17 C16 H16 126.7 . . ? C15 C16 H16 126.7 . . ? N3 C17 C16 108.9(4) . . ? N3 C17 C18 113.5(4) . . ? C16 C17 C18 137.4(5) . . ? N4 C18 C17 119.9(5) . . ? N4 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? N4 C19 C20 112.7(4) . . ? N4 C19 C24 111.3(4) . . ? C20 C19 C24 110.6(4) . . ? N4 C19 H19 107.3 . . ? C20 C19 H19 107.3 . . ? C24 C19 H19 107.3 . . ? C21 C20 C19 111.9(4) . . ? C21 C20 H20A 109.2 . . ? C19 C20 H20A 109.2 . . ? C21 C20 H20B 109.2 . . ? C19 C20 H20B 109.2 . . ? H20A C20 H20B 107.9 . . ? C20 C21 C22 110.4(4) . . ? C20 C21 H21A 109.6 . . ? C22 C21 H21A 109.6 . . ? C20 C21 H21B 109.6 . . ? C22 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C23 C22 C21 110.2(4) . . ? C23 C22 H22A 109.6 . . ? C21 C22 H22A 109.6 . . ? C23 C22 H22B 109.6 . . ? C21 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? C22 C23 C24 111.9(4) . . ? C22 C23 H23A 109.2 . . ? C24 C23 H23A 109.2 . . ? C22 C23 H23B 109.2 . . ? C24 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C23 C24 C19 111.1(4) . . ? C23 C24 H24A 109.4 . . ? C19 C24 H24A 109.4 . . ? C23 C24 H24B 109.4 . . ? C19 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? N5 C25 C26 108.1(4) . . ? N5 C25 C2 121.5(4) . . ? C26 C25 C2 130.2(4) . . ? C25 C26 C27 107.9(4) . . ? C25 C26 H26 126.1 . . ? C27 C26 H26 126.1 . . ? C28 C27 C26 107.3(4) . . ? C28 C27 H27 126.4 . . ? C26 C27 H27 126.4 . . ? N5 C28 C27 107.5(4) . . ? N5 C28 C29 124.5(5) . . ? C27 C28 C29 128.0(5) . . ? N6 C29 C28 126.8(5) . . ? N6 C29 H29 116.6 . . ? C28 C29 H29 116.6 . . ? N6 C30 C35 110.1(4) . . ? N6 C30 C31 110.3(4) . . ? C35 C30 C31 111.3(4) . . ? N6 C30 H30 108.4 . . ? C35 C30 H30 108.4 . . ? C31 C30 H30 108.4 . . ? C30 C31 C32 110.1(4) . . ? C30 C31 H31A 109.6 . . ? C32 C31 H31A 109.6 . . ? C30 C31 H31B 109.6 . . ? C32 C31 H31B 109.6 . . ? H31A C31 H31B 108.2 . . ? C33 C32 C31 112.1(4) . . ? C33 C32 H32A 109.2 . . ? C31 C32 H32A 109.2 . . ? C33 C32 H32B 109.2 . . ? C31 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? C32 C33 C34 111.3(4) . . ? C32 C33 H33A 109.4 . . ? C34 C33 H33A 109.4 . . ? C32 C33 H33B 109.4 . . ? C34 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C35 C34 C33 111.9(4) . . ? C35 C34 H34A 109.2 . . ? C33 C34 H34A 109.2 . . ? C35 C34 H34B 109.2 . . ? C33 C34 H34B 109.2 . . ? H34A C34 H34B 107.9 . . ? C30 C35 C34 110.3(4) . . ? C30 C35 H35A 109.6 . . ? C34 C35 H35A 109.6 . . ? C30 C35 H35B 109.6 . . ? C34 C35 H35B 109.6 . . ? H35A C35 H35B 108.1 . . ? Cl51 C50 Cl53 110.3(3) . . ? Cl51 C50 Cl52 110.7(3) . . ? Cl53 C50 Cl52 109.8(3) . . ? Cl51 C50 H50 108.6 . . ? Cl53 C50 H50 108.6 . . ? Cl52 C50 H50 108.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Pd1 N1 C3 3.3(5) . . . . ? N2 Pd1 N1 C3 -177.9(5) . . . . ? N4 Pd1 N1 C3 3.6(10) . . . . ? N3 Pd1 N1 C6 -178.4(3) . . . . ? N2 Pd1 N1 C6 0.5(3) . . . . ? N4 Pd1 N1 C6 -178.0(6) . . . . ? N1 Pd1 N2 C7 0.1(3) . . . . ? N3 Pd1 N2 C7 5.2(9) . . . . ? N4 Pd1 N2 C7 179.7(3) . . . . ? N1 Pd1 N2 C8 176.8(4) . . . . ? N3 Pd1 N2 C8 -178.0(6) . . . . ? N4 Pd1 N2 C8 -3.5(4) . . . . ? N1 Pd1 N4 C18 -2.7(9) . . . . ? N3 Pd1 N4 C18 -2.4(3) . . . . ? N2 Pd1 N4 C18 178.9(3) . . . . ? N1 Pd1 N4 C19 -178.8(6) . . . . ? N3 Pd1 N4 C19 -178.5(4) . . . . ? N2 Pd1 N4 C19 2.8(4) . . . . ? N1 Pd1 N3 C14 -6.1(4) . . . . ? N2 Pd1 N3 C14 -11.2(10) . . . . ? N4 Pd1 N3 C14 173.9(5) . . . . ? N1 Pd1 N3 C17 -178.3(3) . . . . ? N2 Pd1 N3 C17 176.6(6) . . . . ? N4 Pd1 N3 C17 1.7(3) . . . . ? C6 N1 C3 C4 0.0(5) . . . . ? Pd1 N1 C3 C4 178.4(3) . . . . ? C6 N1 C3 C2 178.9(4) . . . . ? Pd1 N1 C3 C2 -2.7(7) . . . . ? C25 C2 C3 N1 -117.1(5) . . . . ? C14 C2 C3 N1 2.5(7) . . . . ? C1 C2 C3 N1 123.3(5) . . . . ? C25 C2 C3 C4 61.6(6) . . . . ? C14 C2 C3 C4 -178.8(5) . . . . ? C1 C2 C3 C4 -58.0(6) . . . . ? N1 C3 C4 C5 0.0(6) . . . . ? C2 C3 C4 C5 -178.8(5) . . . . ? C3 C4 C5 C6 0.0(6) . . . . ? C3 N1 C6 C5 0.0(5) . . . . ? Pd1 N1 C6 C5 -178.7(3) . . . . ? C3 N1 C6 C7 177.8(4) . . . . ? Pd1 N1 C6 C7 -0.9(5) . . . . ? C4 C5 C6 N1 0.0(6) . . . . ? C4 C5 C6 C7 -176.9(6) . . . . ? C8 N2 C7 C6 -177.6(4) . . . . ? Pd1 N2 C7 C6 -0.6(6) . . . . ? N1 C6 C7 N2 1.0(7) . . . . ? C5 C6 C7 N2 177.8(6) . . . . ? C7 N2 C8 C9 110.2(5) . . . . ? Pd1 N2 C8 C9 -66.3(5) . . . . ? C7 N2 C8 C13 -12.4(7) . . . . ? Pd1 N2 C8 C13 171.2(3) . . . . ? N2 C8 C9 C10 174.8(4) . . . . ? C13 C8 C9 C10 -58.9(5) . . . . ? C8 C9 C10 C11 57.9(6) . . . . ? C9 C10 C11 C12 -55.3(7) . . . . ? C10 C11 C12 C13 55.4(7) . . . . ? C11 C12 C13 C8 -57.4(6) . . . . ? N2 C8 C13 C12 -178.7(4) . . . . ? C9 C8 C13 C12 58.3(6) . . . . ? C17 N3 C14 C15 -1.1(5) . . . . ? Pd1 N3 C14 C15 -173.7(3) . . . . ? C17 N3 C14 C2 -179.2(4) . . . . ? Pd1 N3 C14 C2 8.1(7) . . . . ? C25 C2 C14 N3 115.6(5) . . . . ? C3 C2 C14 N3 -5.0(6) . . . . ? C1 C2 C14 N3 -125.6(5) . . . . ? C25 C2 C14 C15 -62.2(6) . . . . ? C3 C2 C14 C15 177.3(4) . . . . ? C1 C2 C14 C15 56.6(6) . . . . ? N3 C14 C15 C16 0.8(5) . . . . ? C2 C14 C15 C16 178.8(4) . . . . ? C14 C15 C16 C17 -0.2(5) . . . . ? C14 N3 C17 C16 1.0(5) . . . . ? Pd1 N3 C17 C16 175.1(3) . . . . ? C14 N3 C17 C18 -175.0(4) . . . . ? Pd1 N3 C17 C18 -0.8(5) . . . . ? C15 C16 C17 N3 -0.5(5) . . . . ? C15 C16 C17 C18 174.1(6) . . . . ? C19 N4 C18 C17 179.5(4) . . . . ? Pd1 N4 C18 C17 2.7(5) . . . . ? N3 C17 C18 N4 -1.4(6) . . . . ? C16 C17 C18 N4 -175.8(5) . . . . ? C18 N4 C19 C20 53.8(6) . . . . ? Pd1 N4 C19 C20 -130.4(4) . . . . ? C18 N4 C19 C24 -71.2(5) . . . . ? Pd1 N4 C19 C24 104.7(4) . . . . ? N4 C19 C20 C21 178.4(4) . . . . ? C24 C19 C20 C21 -56.3(6) . . . . ? C19 C20 C21 C22 57.1(6) . . . . ? C20 C21 C22 C23 -56.3(6) . . . . ? C21 C22 C23 C24 56.0(6) . . . . ? C22 C23 C24 C19 -55.6(6) . . . . ? N4 C19 C24 C23 -179.2(4) . . . . ? C20 C19 C24 C23 54.7(5) . . . . ? C28 N5 C25 C26 1.6(5) . . . . ? C28 N5 C25 C2 -174.2(4) . . . . ? C3 C2 C25 N5 -162.4(4) . . . . ? C14 C2 C25 N5 73.0(5) . . . . ? C1 C2 C25 N5 -44.3(6) . . . . ? C3 C2 C25 C26 22.8(6) . . . . ? C14 C2 C25 C26 -101.8(5) . . . . ? C1 C2 C25 C26 140.9(5) . . . . ? N5 C25 C26 C27 -1.6(5) . . . . ? C2 C25 C26 C27 173.7(4) . . . . ? C25 C26 C27 C28 1.1(5) . . . . ? C25 N5 C28 C27 -0.9(5) . . . . ? C25 N5 C28 C29 177.2(4) . . . . ? C26 C27 C28 N5 -0.2(5) . . . . ? C26 C27 C28 C29 -178.1(4) . . . . ? C30 N6 C29 C28 -177.0(4) . . . . ? N5 C28 C29 N6 3.2(7) . . . . ? C27 C28 C29 N6 -179.2(4) . . . . ? C29 N6 C30 C35 142.8(4) . . . . ? C29 N6 C30 C31 -94.0(5) . . . . ? N6 C30 C31 C32 -178.8(4) . . . . ? C35 C30 C31 C32 -56.3(5) . . . . ? C30 C31 C32 C33 54.8(6) . . . . ? C31 C32 C33 C34 -54.1(6) . . . . ? C32 C33 C34 C35 54.8(6) . . . . ? N6 C30 C35 C34 179.8(4) . . . . ? C31 C30 C35 C34 57.3(5) . . . . ? C33 C34 C35 C30 -56.3(6) . . . . ? 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 N5 H5N Cl1 0.88 2.32 3.175(4) 165.5 . N6 H6N Cl1 0.88 2.26 3.138(4) 175.9 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 21.97 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.639 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.082 _vrf_THETM01_PdClH2L1 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: The data for [Pd(ClH2L1)] was complete up to 0.95 A and were cut at this resolution. ; _vrf_PLAT023_PdClH2L1 ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 21.97 Deg. RESPONSE: The data for [Pd(ClH2L1)] was complete up to 0.95 A and were cut at this resolution. ; data_CuClH2L1 _database_code_depnum_ccdc_archive 'CCDC 866707' #TrackingRef '- revised_combined.cif' # local name jl1006 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2 C35 H47 Cl Cu N6, C4 H10 O, 0.6 C2 H3 N' _chemical_formula_sum 'C75.20 H105.80 Cl2 Cu2 N12.60 O' _chemical_formula_weight 1400.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 16.9395(3) _cell_length_b 16.1910(3) _cell_length_c 26.7675(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7341.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 28634 _cell_measurement_theta_min 2.6063 _cell_measurement_theta_max 75.7261 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2981 _exptl_absorpt_coefficient_mu 1.783 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.6130 _exptl_absorpt_correction_T_max 0.8949 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator 'mirror optics' _diffrn_measurement_device_type 'Agilent Technologies SuperNova' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 5.1574 _diffrn_reflns_number 57040 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 75.91 _reflns_number_total 14997 _reflns_number_gt 14290 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrysAlisPro (Agilent Technologies, 2011)' _computing_cell_refinement 'CrysAlisPro (Agilent Technologies, 2011)' _computing_data_reduction 'CrysAlisPro (Agilent Technologies, 2011)' _computing_structure_solution 'SIR92 (Altomare et al., 1992)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury 2.0 (Bruno et al, 2002)' _computing_publication_material 'SHELXTL (Sheldrick, 2008) and local programs' _refine_special_details ; The acetonitrile molecule has a partial occupancy of 60% and was refined as such. The ether molecule of crystallisation was handled using an isotropic whole molecule disorder model, The refined occupancy ratio is 0.670(5):0.330(5). 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^)+(0.0622P)^2^+7.9680P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 7243 Friedel pairs' _refine_ls_abs_structure_Flack 0.488(15) _refine_ls_number_reflns 14997 _refine_ls_number_parameters 838 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0483 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1268 _refine_ls_wR_factor_gt 0.1250 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.075 _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 0.44404(3) 0.87610(3) 0.236104(17) 0.02004(10) Uani 1 1 d . . . Cl1 Cl 0.56287(5) 0.96665(5) 0.21051(3) 0.02989(17) Uani 1 1 d . . . N1 N 0.39316(16) 0.94956(17) 0.28376(10) 0.0212(5) Uani 1 1 d . . . N2 N 0.37218(16) 0.94204(18) 0.18699(10) 0.0214(5) Uani 1 1 d . . . N3 N 0.47340(17) 0.81214(17) 0.29468(11) 0.0232(5) Uani 1 1 d . . . N4 N 0.48055(16) 0.76968(17) 0.20044(11) 0.0219(5) Uani 1 1 d . . . N5 N 0.55082(18) 0.99222(18) 0.33147(11) 0.0246(6) Uani 1 1 d . . . H5N H 0.5338 0.9880 0.3005 0.029 Uiso 1 1 calc R . . N6 N 0.65350(17) 1.10280(18) 0.26826(13) 0.0301(6) Uani 1 1 d . . . H6 H 0.6184 1.0731 0.2520 0.036 Uiso 1 1 calc R . . C1 C 0.4075(3) 0.8921(3) 0.41941(13) 0.0347(8) Uani 1 1 d . . . H1A H 0.3974 0.9464 0.4342 0.052 Uiso 1 1 calc R . . H1B H 0.4448 0.8615 0.4404 0.052 Uiso 1 1 calc R . . H1C H 0.3579 0.8613 0.4170 0.052 Uiso 1 1 calc R . . C2 C 0.4426(2) 0.9031(2) 0.36720(13) 0.0250(7) Uani 1 1 d . . . C3 C 0.3861(2) 0.9519(2) 0.33429(12) 0.0222(6) Uani 1 1 d . . . C4 C 0.3267(2) 1.0083(2) 0.34670(14) 0.0251(7) Uani 1 1 d . . . H4 H 0.3097 1.0220 0.3795 0.030 Uiso 1 1 calc R . . C5 C 0.2968(2) 1.0410(2) 0.30225(14) 0.0261(7) Uani 1 1 d . . . H5 H 0.2563 1.0812 0.2990 0.031 Uiso 1 1 calc R . . C6 C 0.33827(19) 1.0026(2) 0.26363(13) 0.0231(7) Uani 1 1 d . . . C7 C 0.33216(19) 0.9985(2) 0.21008(14) 0.0234(7) Uani 1 1 d . . . H7 H 0.2997 1.0362 0.1922 0.028 Uiso 1 1 calc R . . C8 C 0.3689(2) 0.9343(2) 0.13229(12) 0.0255(7) Uani 1 1 d . . . H8 H 0.4242 0.9251 0.1205 0.031 Uiso 1 1 calc R . . C9 C 0.3374(3) 1.0069(3) 0.10400(15) 0.0376(9) Uani 1 1 d . . . H9A H 0.3684 1.0569 0.1124 0.045 Uiso 1 1 calc R . . H9B H 0.2817 1.0170 0.1135 0.045 Uiso 1 1 calc R . . C10 C 0.3428(3) 0.9899(3) 0.04760(17) 0.0513(12) Uani 1 1 d . . . H10A H 0.3209 1.0375 0.0290 0.062 Uiso 1 1 calc R . . H10B H 0.3989 0.9837 0.0380 0.062 Uiso 1 1 calc R . . C11 C 0.2984(3) 0.9131(4) 0.03339(16) 0.0562(13) Uani 1 1 d . . . H11A H 0.2414 0.9217 0.0394 0.067 Uiso 1 1 calc R . . H11B H 0.3059 0.9023 -0.0027 0.067 Uiso 1 1 calc R . . C12 C 0.3257(3) 0.8402(3) 0.06245(15) 0.0434(10) Uani 1 1 d . . . H12A H 0.3808 0.8269 0.0530 0.052 Uiso 1 1 calc R . . H12B H 0.2923 0.7920 0.0541 0.052 Uiso 1 1 calc R . . C13 C 0.3217(2) 0.8565(2) 0.11875(13) 0.0295(7) Uani 1 1 d . . . H13A H 0.3434 0.8084 0.1370 0.035 Uiso 1 1 calc R . . H13B H 0.2660 0.8637 0.1290 0.035 Uiso 1 1 calc R . . C14 C 0.4592(2) 0.8192(2) 0.34412(13) 0.0237(6) Uani 1 1 d . . . C15 C 0.4628(2) 0.7406(2) 0.36608(14) 0.0287(7) Uani 1 1 d . . . H15 H 0.4559 0.7284 0.4005 0.034 Uiso 1 1 calc R . . C16 C 0.4784(2) 0.6834(2) 0.32822(14) 0.0281(7) Uani 1 1 d . . . H16 H 0.4838 0.6252 0.3315 0.034 Uiso 1 1 calc R . . C17 C 0.48450(19) 0.7298(2) 0.28472(12) 0.0229(7) Uani 1 1 d . . . C18 C 0.49325(18) 0.7109(2) 0.23290(14) 0.0240(7) Uani 1 1 d . . . H18 H 0.5079 0.6571 0.2223 0.029 Uiso 1 1 calc R . . C19 C 0.5036(2) 0.7576(2) 0.14808(12) 0.0227(6) Uani 1 1 d . . . H19 H 0.4778 0.8023 0.1281 0.027 Uiso 1 1 calc R . . C20 C 0.5924(2) 0.7690(3) 0.14287(15) 0.0316(8) Uani 1 1 d . . . H20A H 0.6200 0.7253 0.1620 0.038 Uiso 1 1 calc R . . H20B H 0.6078 0.8231 0.1570 0.038 Uiso 1 1 calc R . . C21 C 0.6175(3) 0.7647(3) 0.08777(16) 0.0389(9) Uani 1 1 d . . . H21A H 0.5927 0.8107 0.0691 0.047 Uiso 1 1 calc R . . H21B H 0.6755 0.7709 0.0853 0.047 Uiso 1 1 calc R . . C22 C 0.5930(3) 0.6832(3) 0.06486(15) 0.0389(9) Uani 1 1 d . . . H22A H 0.6218 0.6376 0.0814 0.047 Uiso 1 1 calc R . . H22B H 0.6069 0.6828 0.0289 0.047 Uiso 1 1 calc R . . C23 C 0.5044(3) 0.6700(3) 0.07078(14) 0.0368(9) Uani 1 1 d . . . H23A H 0.4901 0.6150 0.0573 0.044 Uiso 1 1 calc R . . H23B H 0.4758 0.7122 0.0510 0.044 Uiso 1 1 calc R . . C24 C 0.4783(2) 0.6755(2) 0.12547(14) 0.0298(8) Uani 1 1 d . . . H24A H 0.4202 0.6702 0.1275 0.036 Uiso 1 1 calc R . . H24B H 0.5021 0.6296 0.1447 0.036 Uiso 1 1 calc R . . C25 C 0.5179(2) 0.9543(2) 0.37130(13) 0.0266(7) Uani 1 1 d . . . C26 C 0.5623(2) 0.9758(3) 0.41330(15) 0.0356(9) Uani 1 1 d . . . H26 H 0.5532 0.9579 0.4466 0.043 Uiso 1 1 calc R . . C27 C 0.6223(3) 1.0283(3) 0.39746(16) 0.0376(9) Uani 1 1 d . . . H27 H 0.6614 1.0529 0.4181 0.045 Uiso 1 1 calc R . . C28 C 0.6149(2) 1.0385(2) 0.34640(15) 0.0287(7) Uani 1 1 d . . . C29 C 0.6610(2) 1.0909(2) 0.31552(15) 0.0312(8) Uani 1 1 d . . . H29 H 0.7022 1.1206 0.3316 0.037 Uiso 1 1 calc R . . C30 C 0.7004(2) 1.1634(2) 0.23973(17) 0.0310(7) Uani 1 1 d . . . H30 H 0.7563 1.1615 0.2517 0.037 Uiso 1 1 calc R . . C31 C 0.6678(2) 1.2502(2) 0.24771(15) 0.0311(8) Uani 1 1 d . . . H31A H 0.6115 1.2517 0.2380 0.037 Uiso 1 1 calc R . . H31B H 0.6716 1.2649 0.2835 0.037 Uiso 1 1 calc R . . C32 C 0.7138(2) 1.3123(2) 0.21681(16) 0.0323(8) Uani 1 1 d . . . H32A H 0.7688 1.3149 0.2291 0.039 Uiso 1 1 calc R . . H32B H 0.6899 1.3677 0.2209 0.039 Uiso 1 1 calc R . . C33 C 0.7138(3) 1.2892(3) 0.16183(17) 0.0390(9) Uani 1 1 d . . . H33A H 0.7466 1.3292 0.1431 0.047 Uiso 1 1 calc R . . H33B H 0.6593 1.2924 0.1487 0.047 Uiso 1 1 calc R . . C34 C 0.7459(3) 1.2025(3) 0.15383(18) 0.0440(10) Uani 1 1 d . . . H34A H 0.8021 1.2005 0.1638 0.053 Uiso 1 1 calc R . . H34B H 0.7423 1.1879 0.1180 0.053 Uiso 1 1 calc R . . C35 C 0.6984(3) 1.1403(3) 0.18498(18) 0.0418(10) Uani 1 1 d . . . H35A H 0.6431 1.1393 0.1732 0.050 Uiso 1 1 calc R . . H35B H 0.7209 1.0844 0.1805 0.050 Uiso 1 1 calc R . . Cu2 Cu 0.98947(3) 0.12229(3) 0.274051(17) 0.01929(10) Uani 1 1 d . . . Cl2 Cl 0.87048(5) 0.03281(5) 0.29835(3) 0.02820(17) Uani 1 1 d . . . N101 N 0.95888(17) 0.18988(17) 0.21699(11) 0.0215(5) Uani 1 1 d . . . N102 N 0.95349(16) 0.22691(18) 0.31190(11) 0.0209(5) Uani 1 1 d . . . N103 N 1.04000(16) 0.05156(17) 0.22466(10) 0.0218(6) Uani 1 1 d . . . N104 N 1.06328(16) 0.05486(17) 0.32092(10) 0.0205(5) Uani 1 1 d . . . N105 N 0.88081(18) 0.01141(18) 0.17810(11) 0.0242(6) Uani 1 1 d . . . H105 H 0.8977 0.0152 0.2091 0.029 Uiso 1 1 calc R . . N106 N 0.77944(17) -0.10207(17) 0.23996(12) 0.0273(6) Uani 1 1 d . . . H106 H 0.8146 -0.0730 0.2566 0.033 Uiso 1 1 calc R . . C51 C 1.0226(2) 0.1139(2) 0.08983(13) 0.0317(8) Uani 1 1 d . . . H51A H 0.9844 0.1445 0.0695 0.048 Uiso 1 1 calc R . . H51B H 1.0327 0.0600 0.0745 0.048 Uiso 1 1 calc R . . H51C H 1.0721 0.1452 0.0918 0.048 Uiso 1 1 calc R . . C52 C 0.9890(2) 0.1016(2) 0.14273(13) 0.0243(7) Uani 1 1 d . . . C53 C 0.9712(2) 0.1850(2) 0.16733(12) 0.0213(6) Uani 1 1 d . . . C54 C 0.9668(2) 0.2637(2) 0.14619(14) 0.0280(7) Uani 1 1 d . . . H54 H 0.9726 0.2772 0.1118 0.034 Uiso 1 1 calc R . . C55 C 0.9521(2) 0.3190(2) 0.18538(15) 0.0280(7) Uani 1 1 d . . . H55 H 0.9461 0.3772 0.1828 0.034 Uiso 1 1 calc R . . C56 C 0.94786(18) 0.2714(2) 0.22911(14) 0.0235(7) Uani 1 1 d . . . C57 C 0.93989(18) 0.2866(2) 0.28115(13) 0.0231(7) Uani 1 1 d . . . H57 H 0.9249 0.3396 0.2930 0.028 Uiso 1 1 calc R . . C58 C 0.9306(2) 0.2357(2) 0.36429(12) 0.0225(6) Uani 1 1 d . . . H58 H 0.9549 0.1886 0.3829 0.027 Uiso 1 1 calc R . . C59 C 0.8400(2) 0.2266(3) 0.36904(14) 0.0313(8) Uani 1 1 d . . . H59A H 0.8138 0.2723 0.3509 0.038 Uiso 1 1 calc R . . H59B H 0.8231 0.1739 0.3536 0.038 Uiso 1 1 calc R . . C60 C 0.8150(3) 0.2282(3) 0.42390(16) 0.0392(9) Uani 1 1 d . . . H60A H 0.7568 0.2240 0.4262 0.047 Uiso 1 1 calc R . . H60B H 0.8381 0.1801 0.4415 0.047 Uiso 1 1 calc R . . C61 C 0.8422(3) 0.3072(3) 0.44894(16) 0.0418(10) Uani 1 1 d . . . H61A H 0.8271 0.3060 0.4847 0.050 Uiso 1 1 calc R . . H61B H 0.8154 0.3549 0.4332 0.050 Uiso 1 1 calc R . . C62 C 0.9316(3) 0.3182(3) 0.44459(15) 0.0386(9) Uani 1 1 d . . . H62A H 0.9586 0.2737 0.4634 0.046 Uiso 1 1 calc R . . H62B H 0.9471 0.3718 0.4594 0.046 Uiso 1 1 calc R . . C63 C 0.9578(2) 0.3154(2) 0.38992(14) 0.0312(8) Uani 1 1 d . . . H63A H 1.0160 0.3192 0.3882 0.037 Uiso 1 1 calc R . . H63B H 0.9355 0.3635 0.3720 0.037 Uiso 1 1 calc R . . C64 C 1.0464(2) 0.0524(2) 0.17424(12) 0.0217(6) Uani 1 1 d . . . C65 C 1.1071(2) -0.0017(2) 0.15965(13) 0.0259(7) Uani 1 1 d . . . H65 H 1.1242 -0.0126 0.1265 0.031 Uiso 1 1 calc R . . C66 C 1.13802(19) -0.0369(2) 0.20404(13) 0.0245(6) Uani 1 1 d . . . H66 H 1.1793 -0.0764 0.2066 0.029 Uiso 1 1 calc R . . C67 C 1.09527(18) -0.00152(19) 0.24315(12) 0.0197(6) Uani 1 1 d . . . C68 C 1.10294(18) 0.0002(2) 0.29640(13) 0.0202(6) Uani 1 1 d . . . H68 H 1.1363 -0.0379 0.3132 0.024 Uiso 1 1 calc R . . C69 C 1.06850(19) 0.0611(2) 0.37544(12) 0.0216(6) Uani 1 1 d . . . H69 H 1.0135 0.0684 0.3882 0.026 Uiso 1 1 calc R . . C70 C 1.1037(2) -0.0137(2) 0.40264(13) 0.0275(7) Uani 1 1 d . . . H70A H 1.0733 -0.0639 0.3939 0.033 Uiso 1 1 calc R . . H70B H 1.1590 -0.0220 0.3917 0.033 Uiso 1 1 calc R . . C71 C 1.1016(3) -0.0006(2) 0.45923(14) 0.0338(8) Uani 1 1 d . . . H71A H 1.1258 -0.0488 0.4761 0.041 Uiso 1 1 calc R . . H71B H 1.0461 0.0038 0.4705 0.041 Uiso 1 1 calc R . . C72 C 1.1465(2) 0.0780(3) 0.47387(14) 0.0351(8) Uani 1 1 d . . . H72A H 1.2032 0.0715 0.4656 0.042 Uiso 1 1 calc R . . H72B H 1.1420 0.0869 0.5103 0.042 Uiso 1 1 calc R . . C73 C 1.1131(2) 0.1533(2) 0.44600(14) 0.0311(7) Uani 1 1 d . . . H73A H 1.0581 0.1633 0.4570 0.037 Uiso 1 1 calc R . . H73B H 1.1447 0.2028 0.4543 0.037 Uiso 1 1 calc R . . C74 C 1.1146(2) 0.1391(2) 0.38964(13) 0.0258(7) Uani 1 1 d . . . H74A H 1.1700 0.1335 0.3783 0.031 Uiso 1 1 calc R . . H74B H 1.0912 0.1874 0.3725 0.031 Uiso 1 1 calc R . . C75 C 0.9136(2) 0.0499(2) 0.13866(13) 0.0248(7) Uani 1 1 d . . . C76 C 0.8690(2) 0.0296(2) 0.09627(14) 0.0308(8) Uani 1 1 d . . . H76 H 0.8781 0.0488 0.0632 0.037 Uiso 1 1 calc R . . C77 C 0.8093(2) -0.0233(2) 0.11128(14) 0.0308(8) Uani 1 1 d . . . H77 H 0.7703 -0.0474 0.0903 0.037 Uiso 1 1 calc R . . C78 C 0.8165(2) -0.0351(2) 0.16273(14) 0.0264(7) Uani 1 1 d . . . C79 C 0.7714(2) -0.0892(2) 0.19238(14) 0.0267(7) Uani 1 1 d . . . H79 H 0.7310 -0.1193 0.1759 0.032 Uiso 1 1 calc R . . C80 C 0.73199(19) -0.1636(2) 0.26728(14) 0.0274(7) Uani 1 1 d . . . H80 H 0.6771 -0.1636 0.2536 0.033 Uiso 1 1 calc R . . C81 C 0.7676(2) -0.2496(2) 0.26074(15) 0.0311(8) Uani 1 1 d . . . H81A H 0.8232 -0.2493 0.2722 0.037 Uiso 1 1 calc R . . H81B H 0.7671 -0.2649 0.2249 0.037 Uiso 1 1 calc R . . C82 C 0.7204(2) -0.3130(2) 0.29085(16) 0.0330(8) Uani 1 1 d . . . H82A H 0.6663 -0.3170 0.2772 0.040 Uiso 1 1 calc R . . H82B H 0.7456 -0.3680 0.2877 0.040 Uiso 1 1 calc R . . C83 C 0.7164(3) -0.2890(2) 0.34567(16) 0.0381(9) Uani 1 1 d . . . H83A H 0.6840 -0.3298 0.3641 0.046 Uiso 1 1 calc R . . H83B H 0.7702 -0.2893 0.3602 0.046 Uiso 1 1 calc R . . C84 C 0.6806(3) -0.2039(3) 0.35115(16) 0.0378(9) Uani 1 1 d . . . H84A H 0.6791 -0.1884 0.3869 0.045 Uiso 1 1 calc R . . H84B H 0.6257 -0.2045 0.3384 0.045 Uiso 1 1 calc R . . C85 C 0.7292(2) -0.1402(2) 0.32194(15) 0.0330(8) Uani 1 1 d . . . H85A H 0.7051 -0.0849 0.3256 0.040 Uiso 1 1 calc R . . H85B H 0.7834 -0.1379 0.3356 0.040 Uiso 1 1 calc R . . N400 N 0.8503(7) -0.5234(6) 0.5277(4) 0.089(3) Uani 0.60 1 d P . . C401 C 0.8909(7) -0.4816(6) 0.5528(3) 0.064(3) Uani 0.60 1 d P . . C402 C 0.9351(6) -0.4332(7) 0.5824(4) 0.070(3) Uani 0.60 1 d P . . H40A H 0.9439 -0.4610 0.6144 0.104 Uiso 0.60 1 calc PR . . H40B H 0.9076 -0.3808 0.5881 0.104 Uiso 0.60 1 calc PR . . H40C H 0.9859 -0.4225 0.5662 0.104 Uiso 0.60 1 calc PR . . C311 C 0.8609(6) -0.0218(6) 0.4373(4) 0.0738(9) Uiso 0.670(5) 1 d PD A 1 H31C H 0.9014 0.0194 0.4449 0.089 Uiso 0.670(5) 1 calc PR A 1 H31D H 0.8092 0.0051 0.4353 0.089 Uiso 0.670(5) 1 calc PR A 1 H31E H 0.8729 -0.0481 0.4052 0.089 Uiso 0.670(5) 1 calc PR A 1 C312 C 0.8594(8) -0.0887(9) 0.4793(5) 0.0738(9) Uiso 0.670(5) 1 d PD A 1 H31F H 0.8468 -0.0627 0.5118 0.089 Uiso 0.670(5) 1 calc PR A 1 H31G H 0.9118 -0.1155 0.4820 0.089 Uiso 0.670(5) 1 calc PR A 1 O311 O 0.7947(4) -0.1548(4) 0.4656(3) 0.0738(9) Uiso 0.670(5) 1 d PD A 1 C313 C 0.7935(7) -0.2283(7) 0.5072(4) 0.0738(9) Uiso 0.670(5) 1 d PD A 1 H31H H 0.8419 -0.2623 0.5043 0.089 Uiso 0.670(5) 1 calc PR A 1 H31I H 0.7917 -0.2043 0.5412 0.089 Uiso 0.670(5) 1 calc PR A 1 C314 C 0.7216(6) -0.2810(6) 0.4982(4) 0.0738(9) Uiso 0.670(5) 1 d PD A 1 H31J H 0.7181 -0.3234 0.5242 0.089 Uiso 0.670(5) 1 calc PR A 1 H31K H 0.7257 -0.3076 0.4654 0.089 Uiso 0.670(5) 1 calc PR A 1 H31L H 0.6742 -0.2463 0.4991 0.089 Uiso 0.670(5) 1 calc PR A 1 C321 C 0.8454(14) -0.0940(19) 0.4730(11) 0.0738(9) Uiso 0.330(5) 1 d PD A 2 H32C H 0.8491 -0.0500 0.4480 0.089 Uiso 0.330(5) 1 calc PR A 2 H32D H 0.8782 -0.1408 0.4627 0.089 Uiso 0.330(5) 1 calc PR A 2 H32E H 0.8639 -0.0731 0.5054 0.089 Uiso 0.330(5) 1 calc PR A 2 C322 C 0.7518(11) -0.1244(11) 0.4782(8) 0.0738(9) Uiso 0.330(5) 1 d PD A 2 H32F H 0.7195 -0.0834 0.4964 0.089 Uiso 0.330(5) 1 calc PR A 2 H32G H 0.7279 -0.1352 0.4451 0.089 Uiso 0.330(5) 1 calc PR A 2 O321 O 0.7625(8) -0.2097(8) 0.5103(5) 0.0738(9) Uiso 0.330(5) 1 d PD A 2 C323 C 0.6771(10) -0.2581(12) 0.5155(8) 0.0738(9) Uiso 0.330(5) 1 d PD A 2 H32H H 0.6869 -0.3153 0.5040 0.089 Uiso 0.330(5) 1 calc PR A 2 H32I H 0.6666 -0.2620 0.5518 0.089 Uiso 0.330(5) 1 calc PR A 2 C324 C 0.6132(10) -0.2371(13) 0.4961(8) 0.0738(9) Uiso 0.330(5) 1 d PD A 2 H32J H 0.5784 -0.2853 0.4936 0.089 Uiso 0.330(5) 1 calc PR A 2 H32K H 0.6231 -0.2148 0.4626 0.089 Uiso 0.330(5) 1 calc PR A 2 H32L H 0.5880 -0.1947 0.5168 0.089 Uiso 0.330(5) 1 calc PR A 2 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 0.0214(2) 0.0184(2) 0.0203(2) 0.00000(18) -0.00190(18) 0.00128(17) Cl1 0.0274(4) 0.0253(4) 0.0369(4) -0.0024(3) -0.0001(3) -0.0066(3) N1 0.0234(13) 0.0221(13) 0.0182(13) 0.0015(10) -0.0037(10) 0.0019(10) N2 0.0194(12) 0.0237(14) 0.0210(13) 0.0022(11) -0.0052(10) 0.0015(11) N3 0.0239(13) 0.0179(13) 0.0277(14) -0.0001(11) -0.0022(11) -0.0006(10) N4 0.0228(12) 0.0207(13) 0.0223(13) -0.0010(11) -0.0021(11) -0.0006(10) N5 0.0225(13) 0.0228(14) 0.0284(14) -0.0013(11) -0.0058(11) -0.0018(11) N6 0.0226(13) 0.0227(13) 0.0451(18) -0.0002(13) -0.0072(13) -0.0050(11) C1 0.043(2) 0.041(2) 0.0204(16) -0.0027(15) 0.0013(15) -0.0003(17) C2 0.0252(16) 0.0266(17) 0.0231(16) -0.0022(13) -0.0004(12) -0.0002(13) C3 0.0256(16) 0.0214(15) 0.0196(15) -0.0009(12) -0.0021(12) -0.0007(13) C4 0.0245(15) 0.0242(16) 0.0265(16) -0.0056(13) 0.0019(13) -0.0041(13) C5 0.0212(14) 0.0207(15) 0.0365(19) -0.0043(13) 0.0010(14) -0.0005(12) C6 0.0207(14) 0.0156(14) 0.0329(18) 0.0023(13) -0.0006(13) 0.0004(12) C7 0.0226(15) 0.0177(14) 0.0298(17) 0.0040(13) -0.0009(13) -0.0005(12) C8 0.0255(16) 0.0325(18) 0.0185(15) 0.0026(13) -0.0040(12) -0.0016(14) C9 0.041(2) 0.039(2) 0.033(2) 0.0088(16) -0.0032(16) 0.0045(17) C10 0.064(3) 0.058(3) 0.031(2) 0.020(2) -0.001(2) 0.001(2) C11 0.054(3) 0.089(4) 0.026(2) 0.000(2) -0.0063(19) -0.006(3) C12 0.043(2) 0.064(3) 0.0231(18) -0.0078(18) 0.0020(16) -0.015(2) C13 0.0279(17) 0.0373(19) 0.0232(17) -0.0008(14) -0.0019(13) -0.0074(15) C14 0.0227(15) 0.0256(17) 0.0228(15) -0.0003(13) -0.0026(13) -0.0010(13) C15 0.0305(17) 0.0293(18) 0.0262(16) 0.0026(14) -0.0013(14) 0.0020(15) C16 0.0320(18) 0.0225(17) 0.0296(18) 0.0073(14) -0.0029(14) 0.0001(14) C17 0.0211(14) 0.0213(15) 0.0264(18) 0.0028(12) -0.0010(12) 0.0009(12) C18 0.0218(14) 0.0192(15) 0.0310(18) 0.0029(13) -0.0032(13) 0.0023(11) C19 0.0236(15) 0.0219(15) 0.0226(15) -0.0014(12) -0.0025(12) 0.0029(12) C20 0.0282(17) 0.0335(19) 0.0332(19) -0.0057(15) 0.0034(15) -0.0060(15) C21 0.042(2) 0.036(2) 0.039(2) 0.0034(17) 0.0141(18) 0.0029(17) C22 0.056(3) 0.035(2) 0.0266(18) 0.0018(16) 0.0127(17) 0.0105(19) C23 0.053(2) 0.0310(19) 0.0261(18) -0.0088(14) -0.0047(16) -0.0010(17) C24 0.0366(18) 0.0284(18) 0.0245(17) -0.0079(14) -0.0012(14) -0.0064(15) C25 0.0300(17) 0.0256(17) 0.0242(17) -0.0043(13) -0.0072(14) 0.0024(14) C26 0.041(2) 0.036(2) 0.0304(19) -0.0040(16) -0.0111(16) -0.0020(16) C27 0.038(2) 0.0318(19) 0.043(2) -0.0078(16) -0.0177(17) -0.0029(17) C28 0.0249(16) 0.0237(16) 0.0374(19) -0.0055(14) -0.0093(14) 0.0014(13) C29 0.0241(16) 0.0214(16) 0.048(2) -0.0052(15) -0.0129(15) -0.0009(13) C30 0.0204(14) 0.0208(15) 0.052(2) 0.0008(16) 0.0011(16) -0.0022(12) C31 0.0302(17) 0.0216(16) 0.042(2) -0.0054(14) 0.0027(15) 0.0010(14) C32 0.0306(17) 0.0204(16) 0.046(2) -0.0018(15) -0.0003(16) -0.0007(13) C33 0.037(2) 0.033(2) 0.048(2) 0.0058(17) 0.0048(18) -0.0056(17) C34 0.044(2) 0.036(2) 0.053(3) -0.0088(19) 0.013(2) -0.0069(18) C35 0.040(2) 0.0267(19) 0.059(3) -0.0157(18) 0.0140(19) -0.0038(17) Cu2 0.0206(2) 0.0170(2) 0.0202(2) 0.00031(18) -0.00042(18) 0.00175(16) Cl2 0.0285(4) 0.0263(4) 0.0298(4) 0.0005(3) 0.0001(3) -0.0071(3) N101 0.0241(12) 0.0196(13) 0.0206(12) 0.0001(10) -0.0026(10) 0.0002(10) N102 0.0211(12) 0.0187(13) 0.0228(13) -0.0020(10) 0.0007(10) 0.0004(10) N103 0.0214(12) 0.0214(13) 0.0226(14) -0.0011(10) -0.0008(10) -0.0001(10) N104 0.0218(13) 0.0188(13) 0.0210(13) 0.0026(10) -0.0012(10) 0.0008(10) N105 0.0265(14) 0.0237(14) 0.0226(13) 0.0029(11) -0.0072(11) -0.0041(12) N106 0.0246(13) 0.0218(13) 0.0354(15) -0.0002(13) -0.0023(13) -0.0050(11) C51 0.040(2) 0.0336(19) 0.0218(16) 0.0028(14) 0.0026(15) -0.0010(16) C52 0.0280(17) 0.0252(16) 0.0197(15) -0.0002(13) 0.0000(12) -0.0034(13) C53 0.0234(15) 0.0200(15) 0.0205(15) 0.0015(12) -0.0015(12) -0.0012(12) C54 0.0330(18) 0.0242(17) 0.0268(17) 0.0054(14) -0.0019(15) -0.0024(14) C55 0.0289(17) 0.0206(16) 0.0346(19) 0.0056(14) -0.0003(14) 0.0048(13) C56 0.0204(14) 0.0183(15) 0.0318(19) 0.0021(13) -0.0020(12) 0.0019(11) C57 0.0206(14) 0.0198(15) 0.0289(17) -0.0007(13) -0.0006(12) 0.0013(11) C58 0.0262(16) 0.0191(15) 0.0222(15) 0.0003(12) 0.0030(13) 0.0011(13) C59 0.0272(17) 0.0351(19) 0.0317(18) -0.0005(15) 0.0061(14) 0.0031(14) C60 0.035(2) 0.047(2) 0.035(2) 0.0050(18) 0.0104(17) 0.0060(18) C61 0.052(2) 0.042(2) 0.0314(19) 0.0047(17) 0.0120(18) 0.021(2) C62 0.056(3) 0.033(2) 0.0267(18) -0.0065(15) 0.0020(17) 0.0064(18) C63 0.0397(19) 0.0227(17) 0.0312(19) -0.0020(14) -0.0007(15) -0.0005(15) C64 0.0235(15) 0.0214(15) 0.0201(16) -0.0010(12) -0.0005(12) -0.0030(13) C65 0.0280(17) 0.0237(16) 0.0259(17) -0.0027(13) 0.0037(13) -0.0041(14) C66 0.0222(14) 0.0221(15) 0.0292(17) -0.0033(13) -0.0004(13) -0.0009(12) C67 0.0217(14) 0.0184(14) 0.0190(15) -0.0001(12) -0.0002(12) -0.0013(11) C68 0.0188(14) 0.0186(14) 0.0232(15) 0.0009(12) -0.0020(12) 0.0013(12) C69 0.0196(14) 0.0243(16) 0.0209(15) 0.0024(12) 0.0008(12) 0.0004(12) C70 0.0337(18) 0.0240(16) 0.0248(17) 0.0036(13) -0.0023(14) 0.0056(14) C71 0.041(2) 0.0356(19) 0.0245(17) 0.0053(15) -0.0041(15) 0.0072(16) C72 0.0314(18) 0.050(2) 0.0238(17) 0.0031(15) -0.0031(14) 0.0005(17) C73 0.0329(18) 0.0327(19) 0.0277(17) -0.0047(15) 0.0007(14) -0.0047(15) C74 0.0266(16) 0.0270(17) 0.0236(16) -0.0008(13) 0.0015(13) -0.0014(14) C75 0.0266(16) 0.0210(15) 0.0269(17) -0.0017(13) -0.0050(13) -0.0011(13) C76 0.0377(19) 0.0320(19) 0.0228(16) -0.0029(14) -0.0049(14) 0.0006(15) C77 0.0319(18) 0.0311(18) 0.0295(18) -0.0049(14) -0.0091(14) -0.0005(15) C78 0.0282(16) 0.0230(16) 0.0280(17) -0.0029(13) -0.0042(13) -0.0006(13) C79 0.0211(15) 0.0218(15) 0.0373(19) -0.0033(13) -0.0050(14) -0.0025(12) C80 0.0196(14) 0.0229(16) 0.040(2) 0.0016(14) -0.0010(14) -0.0022(12) C81 0.0294(17) 0.0221(16) 0.042(2) -0.0049(14) 0.0039(15) -0.0019(14) C82 0.0306(17) 0.0204(16) 0.048(2) 0.0005(15) 0.0030(16) -0.0014(14) C83 0.041(2) 0.0316(19) 0.042(2) 0.0041(17) -0.0006(18) -0.0066(17) C84 0.040(2) 0.034(2) 0.040(2) -0.0050(16) 0.0120(17) -0.0081(17) C85 0.0368(19) 0.0214(16) 0.041(2) -0.0043(15) 0.0089(16) -0.0016(15) N400 0.106(8) 0.078(6) 0.084(6) -0.028(5) 0.032(6) -0.036(6) C401 0.096(7) 0.044(4) 0.052(5) -0.006(4) 0.026(5) -0.011(5) C402 0.060(5) 0.095(8) 0.054(5) -0.024(5) -0.002(4) 0.003(5) _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 2.5827(9) . ? Cu1 N1 1.946(3) . ? Cu1 N2 2.086(3) . ? Cu1 N3 1.944(3) . ? Cu1 N4 2.065(3) . ? N1 C3 1.358(4) . ? N1 C6 1.376(4) . ? N2 C7 1.295(5) . ? N2 C8 1.471(4) . ? N3 C14 1.350(5) . ? N3 C17 1.372(4) . ? N4 C18 1.306(4) . ? N4 C19 1.468(4) . ? N5 H5N 0.880 . ? N5 C25 1.351(5) . ? N5 C28 1.378(5) . ? N6 H6 0.880 . ? N6 C29 1.286(5) . ? N6 C30 1.475(5) . ? C1 H1A 0.980 . ? C1 H1B 0.980 . ? C1 H1C 0.980 . ? C1 C2 1.529(5) . ? C2 C3 1.521(5) . ? C2 C14 1.518(5) . ? C2 C25 1.526(5) . ? C3 C4 1.399(5) . ? C4 H4 0.950 . ? C4 C5 1.397(5) . ? C5 H5 0.950 . ? C5 C6 1.396(5) . ? C6 C7 1.439(5) . ? C7 H7 0.950 . ? C8 H8 1.000 . ? C8 C9 1.497(5) . ? C8 C13 1.535(5) . ? C9 H9A 0.990 . ? C9 H9B 0.990 . ? C9 C10 1.538(6) . ? C10 H10A 0.990 . ? C10 H10B 0.990 . ? C10 C11 1.501(8) . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C11 C12 1.487(8) . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C12 C13 1.531(5) . ? C13 H13A 0.990 . ? C13 H13B 0.990 . ? C14 C15 1.404(5) . ? C15 H15 0.950 . ? C15 C16 1.398(5) . ? C16 H16 0.950 . ? C16 C17 1.390(5) . ? C17 C18 1.428(5) . ? C18 H18 0.950 . ? C19 H19 1.000 . ? C19 C20 1.521(5) . ? C19 C24 1.522(5) . ? C20 H20A 0.990 . ? C20 H20B 0.990 . ? C20 C21 1.537(5) . ? C21 H21A 0.990 . ? C21 H21B 0.990 . ? C21 C22 1.513(6) . ? C22 H22A 0.990 . ? C22 H22B 0.990 . ? C22 C23 1.524(7) . ? C23 H23A 0.990 . ? C23 H23B 0.990 . ? C23 C24 1.532(5) . ? C24 H24A 0.990 . ? C24 H24B 0.990 . ? C25 C26 1.397(5) . ? C26 H26 0.950 . ? C26 C27 1.391(6) . ? C27 H27 0.950 . ? C27 C28 1.382(6) . ? C28 C29 1.418(6) . ? C29 H29 0.950 . ? C30 H30 1.000 . ? C30 C31 1.525(5) . ? C30 C35 1.513(6) . ? C31 H31A 0.990 . ? C31 H31B 0.990 . ? C31 C32 1.517(5) . ? C32 H32A 0.990 . ? C32 H32B 0.990 . ? C32 C33 1.518(6) . ? C33 H33A 0.990 . ? C33 H33B 0.990 . ? C33 C34 1.520(6) . ? C34 H34A 0.990 . ? C34 H34B 0.990 . ? C34 C35 1.535(6) . ? C35 H35A 0.990 . ? C35 H35B 0.990 . ? Cu2 Cl2 2.5661(9) . ? Cu2 N101 1.949(3) . ? Cu2 N102 2.066(3) . ? Cu2 N103 1.947(3) . ? Cu2 N104 2.081(3) . ? N101 C53 1.348(4) . ? N101 C56 1.372(4) . ? N102 C57 1.291(5) . ? N102 C58 1.462(4) . ? N103 C64 1.354(4) . ? N103 C67 1.364(4) . ? N104 C68 1.291(4) . ? N104 C69 1.466(4) . ? N105 H105 0.880 . ? N105 C75 1.346(5) . ? N105 C78 1.387(4) . ? N106 H106 0.880 . ? N106 C79 1.298(5) . ? N106 C80 1.474(4) . ? C51 H51A 0.980 . ? C51 H51B 0.980 . ? C51 H51C 0.980 . ? C51 C52 1.539(5) . ? C52 C53 1.531(5) . ? C52 C64 1.514(5) . ? C52 C75 1.532(5) . ? C53 C54 1.397(5) . ? C54 H54 0.950 . ? C54 C55 1.402(5) . ? C55 H55 0.950 . ? C55 C56 1.403(5) . ? C56 C57 1.421(5) . ? C57 H57 0.950 . ? C58 H58 1.000 . ? C58 C59 1.546(5) . ? C58 C63 1.533(5) . ? C59 H59A 0.990 . ? C59 H59B 0.990 . ? C59 C60 1.529(5) . ? C60 H60A 0.990 . ? C60 H60B 0.990 . ? C60 C61 1.517(7) . ? C61 H61A 0.990 . ? C61 H61B 0.990 . ? C61 C62 1.530(7) . ? C62 H62A 0.990 . ? C62 H62B 0.990 . ? C62 C63 1.530(5) . ? C63 H63A 0.990 . ? C63 H63B 0.990 . ? C64 C65 1.407(5) . ? C65 H65 0.950 . ? C65 C66 1.418(5) . ? C66 H66 0.950 . ? C66 C67 1.396(5) . ? C67 C68 1.432(4) . ? C68 H68 0.950 . ? C69 H69 1.000 . ? C69 C70 1.534(5) . ? C69 C74 1.532(5) . ? C70 H70A 0.990 . ? C70 H70B 0.990 . ? C70 C71 1.530(5) . ? C71 H71A 0.990 . ? C71 H71B 0.990 . ? C71 C72 1.534(6) . ? C72 H72A 0.990 . ? C72 H72B 0.990 . ? C72 C73 1.537(6) . ? C73 H73A 0.990 . ? C73 H73B 0.990 . ? C73 C74 1.526(5) . ? C74 H74A 0.990 . ? C74 H74B 0.990 . ? C75 C76 1.401(5) . ? C76 H76 0.950 . ? C76 C77 1.386(6) . ? C77 H77 0.950 . ? C77 C78 1.395(5) . ? C78 C79 1.407(5) . ? C79 H79 0.950 . ? C80 H80 1.000 . ? C80 C81 1.528(5) . ? C80 C85 1.512(5) . ? C81 H81A 0.990 . ? C81 H81B 0.990 . ? C81 C82 1.531(5) . ? C82 H82A 0.990 . ? C82 H82B 0.990 . ? C82 C83 1.520(6) . ? C83 H83A 0.990 . ? C83 H83B 0.990 . ? C83 C84 1.513(6) . ? C84 H84A 0.990 . ? C84 H84B 0.990 . ? C84 C85 1.533(5) . ? C85 H85A 0.990 . ? C85 H85B 0.990 . ? N40 C401 1.175(14) . ? C401 C402 1.342(14) . ? C402 H40A 0.980 . ? C402 H40B 0.980 . ? C402 H40C 0.980 . ? C311 H31C 0.980 . ? C311 H31D 0.980 . ? C311 H31E 0.980 . ? C311 C312 1.561(17) . ? C312 H31F 0.990 . ? C312 H31G 0.990 . ? C312 O311 1.576(13) . ? O311 C313 1.630(12) . ? C313 H31H 0.990 . ? C313 H31I 0.990 . ? C313 C314 1.507(15) . ? C314 H31J 0.980 . ? C314 H31K 0.980 . ? C314 H31L 0.980 . ? C321 H32C 0.980 . ? C321 H32D 0.980 . ? C321 H32E 0.980 . ? C321 C322 1.67(2) . ? C322 H32F 0.990 . ? C322 H32G 0.990 . ? C322 O321 1.636(18) . ? O321 C323 1.651(18) . ? C323 H32H 0.990 . ? C323 H32I 0.990 . ? C323 C324 1.248(19) . ? C324 H32J 0.980 . ? C324 H32K 0.980 . ? C324 H32L 0.980 . ? 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 N1 99.91(9) . . ? Cl1 Cu1 N2 89.83(8) . . ? Cl1 Cu1 N3 108.48(9) . . ? Cl1 Cu1 N4 96.76(8) . . ? N1 Cu1 N2 80.89(11) . . ? N1 Cu1 N3 84.85(12) . . ? N1 Cu1 N4 161.11(12) . . ? N2 Cu1 N3 158.51(12) . . ? N2 Cu1 N4 108.10(11) . . ? N3 Cu1 N4 81.48(12) . . ? Cu1 N1 C3 135.1(2) . . ? Cu1 N1 C6 115.1(2) . . ? C3 N1 C6 108.3(3) . . ? Cu1 N2 C7 111.5(2) . . ? Cu1 N2 C8 127.3(2) . . ? C7 N2 C8 121.0(3) . . ? Cu1 N3 C14 134.4(2) . . ? Cu1 N3 C17 113.3(2) . . ? C14 N3 C17 107.3(3) . . ? Cu1 N4 C18 110.4(2) . . ? Cu1 N4 C19 129.2(2) . . ? C18 N4 C19 119.6(3) . . ? H5N N5 C25 125.0 . . ? H5N N5 C28 125.0 . . ? C25 N5 C28 110.1(3) . . ? H6 N6 C29 118.1 . . ? H6 N6 C30 118.1 . . ? C29 N6 C30 123.8(3) . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1A C1 C2 109.5 . . ? H1B C1 H1C 109.5 . . ? H1B C1 C2 109.5 . . ? H1C C1 C2 109.5 . . ? C1 C2 C3 110.2(3) . . ? C1 C2 C14 109.9(3) . . ? C1 C2 C25 108.8(3) . . ? C3 C2 C14 110.2(3) . . ? C3 C2 C25 106.6(3) . . ? C14 C2 C25 111.1(3) . . ? N1 C3 C2 120.5(3) . . ? N1 C3 C4 108.5(3) . . ? C2 C3 C4 130.8(3) . . ? C3 C4 H4 126.1 . . ? C3 C4 C5 107.8(3) . . ? H4 C4 C5 126.1 . . ? C4 C5 H5 126.9 . . ? C4 C5 C6 106.2(3) . . ? H5 C5 C6 126.9 . . ? N1 C6 C5 109.2(3) . . ? N1 C6 C7 114.2(3) . . ? C5 C6 C7 136.2(3) . . ? N2 C7 C6 118.1(3) . . ? N2 C7 H7 121.0 . . ? C6 C7 H7 121.0 . . ? N2 C8 H8 106.9 . . ? N2 C8 C9 116.7(3) . . ? N2 C8 C13 109.0(3) . . ? H8 C8 C9 106.9 . . ? H8 C8 C13 106.9 . . ? C9 C8 C13 109.9(3) . . ? C8 C9 H9A 109.8 . . ? C8 C9 H9B 109.8 . . ? C8 C9 C10 109.5(4) . . ? H9A C9 H9B 108.2 . . ? H9A C9 C10 109.8 . . ? H9B C9 C10 109.8 . . ? C9 C10 H10A 109.3 . . ? C9 C10 H10B 109.3 . . ? C9 C10 C11 111.6(4) . . ? H10A C10 H10B 108.0 . . ? H10A C10 C11 109.3 . . ? H10B C10 C11 109.3 . . ? C10 C11 H11A 109.3 . . ? C10 C11 H11B 109.3 . . ? C10 C11 C12 111.7(4) . . ? H11A C11 H11B 107.9 . . ? H11A C11 C12 109.3 . . ? H11B C11 C12 109.3 . . ? C11 C12 H12A 109.4 . . ? C11 C12 H12B 109.4 . . ? C11 C12 C13 111.4(4) . . ? H12A C12 H12B 108.0 . . ? H12A C12 C13 109.4 . . ? H12B C12 C13 109.4 . . ? C8 C13 C12 110.5(3) . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? N3 C14 C2 120.5(3) . . ? N3 C14 C15 109.0(3) . . ? C2 C14 C15 130.5(3) . . ? C14 C15 H15 126.1 . . ? C14 C15 C16 107.8(3) . . ? H15 C15 C16 126.1 . . ? C15 C16 H16 127.4 . . ? C15 C16 C17 105.2(3) . . ? H16 C16 C17 127.4 . . ? N3 C17 C16 110.7(3) . . ? N3 C17 C18 114.2(3) . . ? C16 C17 C18 134.9(3) . . ? N4 C18 C17 118.3(3) . . ? N4 C18 H18 120.9 . . ? C17 C18 H18 120.9 . . ? N4 C19 H19 107.2 . . ? N4 C19 C20 109.5(3) . . ? N4 C19 C24 114.9(3) . . ? H19 C19 C20 107.2 . . ? H19 C19 C24 107.2 . . ? C20 C19 C24 110.4(3) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 C21 110.9(3) . . ? H20A C20 H20B 108.1 . . ? H20A C20 C21 109.5 . . ? H20B C20 C21 109.5 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? C20 C21 C22 110.6(3) . . ? H21A C21 H21B 108.1 . . ? H21A C21 C22 109.5 . . ? H21B C21 C22 109.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C21 C22 C23 110.5(3) . . ? H22A C22 H22B 108.1 . . ? H22A C22 C23 109.5 . . ? H22B C22 C23 109.5 . . ? C22 C23 H23A 109.2 . . ? C22 C23 H23B 109.2 . . ? C22 C23 C24 112.0(3) . . ? H23A C23 H23B 107.9 . . ? H23A C23 C24 109.2 . . ? H23B C23 C24 109.2 . . ? C19 C24 C23 110.5(3) . . ? C19 C24 H24A 109.6 . . ? C19 C24 H24B 109.6 . . ? C23 C24 H24A 109.6 . . ? C23 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? N5 C25 C2 122.4(3) . . ? N5 C25 C26 107.4(3) . . ? C2 C25 C26 130.1(4) . . ? C25 C26 H26 126.3 . . ? C25 C26 C27 107.5(4) . . ? H26 C26 C27 126.3 . . ? C26 C27 H27 126.0 . . ? C26 C27 C28 108.0(3) . . ? H27 C27 C28 126.0 . . ? N5 C28 C27 107.0(3) . . ? N5 C28 C29 126.1(3) . . ? C27 C28 C29 126.7(3) . . ? N6 C29 C28 127.5(3) . . ? N6 C29 H29 116.3 . . ? C28 C29 H29 116.3 . . ? N6 C30 H30 108.9 . . ? N6 C30 C31 110.2(3) . . ? N6 C30 C35 109.0(3) . . ? H30 C30 C31 108.9 . . ? H30 C30 C35 108.9 . . ? C31 C30 C35 110.8(3) . . ? C30 C31 H31A 109.6 . . ? C30 C31 H31B 109.6 . . ? C30 C31 C32 110.4(3) . . ? H31A C31 H31B 108.1 . . ? H31A C31 C32 109.6 . . ? H31B C31 C32 109.6 . . ? C31 C32 H32A 109.3 . . ? C31 C32 H32B 109.3 . . ? C31 C32 C33 111.5(3) . . ? H32A C32 H32B 108.0 . . ? H32A C32 C33 109.3 . . ? H32B C32 C33 109.3 . . ? C32 C33 H33A 109.4 . . ? C32 C33 H33B 109.4 . . ? C32 C33 C34 111.3(4) . . ? H33A C33 H33B 108.0 . . ? H33A C33 C34 109.4 . . ? H33B C33 C34 109.4 . . ? C33 C34 H34A 109.7 . . ? C33 C34 H34B 109.7 . . ? C33 C34 C35 110.0(3) . . ? H34A C34 H34B 108.2 . . ? H34A C34 C35 109.7 . . ? H34B C34 C35 109.7 . . ? C30 C35 C34 110.7(3) . . ? C30 C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 108.1 . . ? Cl2 Cu2 N101 107.86(9) . . ? Cl2 Cu2 N102 96.14(8) . . ? Cl2 Cu2 N103 100.68(9) . . ? Cl2 Cu2 N104 91.31(8) . . ? N101 Cu2 N102 81.11(12) . . ? N101 Cu2 N103 85.12(12) . . ? N101 Cu2 N104 157.95(12) . . ? N102 Cu2 N103 160.89(12) . . ? N102 Cu2 N104 108.17(11) . . ? N103 Cu2 N104 80.60(11) . . ? Cu2 N101 C53 134.3(2) . . ? Cu2 N101 C56 113.0(2) . . ? C53 N101 C56 108.1(3) . . ? Cu2 N102 C57 110.7(2) . . ? Cu2 N102 C58 128.9(2) . . ? C57 N102 C58 119.5(3) . . ? Cu2 N103 C64 134.9(2) . . ? Cu2 N103 C67 115.2(2) . . ? C64 N103 C67 108.3(3) . . ? Cu2 N104 C68 111.5(2) . . ? Cu2 N104 C69 126.9(2) . . ? C68 N104 C69 121.5(3) . . ? H105 N105 C75 125.0 . . ? H105 N105 C78 125.0 . . ? C75 N105 C78 110.0(3) . . ? H106 N106 C79 118.7 . . ? H106 N106 C80 118.7 . . ? C79 N106 C80 122.6(3) . . ? H51A C51 H51B 109.5 . . ? H51A C51 H51C 109.5 . . ? H51A C51 C52 109.5 . . ? H51B C51 H51C 109.5 . . ? H51B C51 C52 109.5 . . ? H51C C51 C52 109.5 . . ? C51 C52 C53 110.8(3) . . ? C51 C52 C64 110.0(3) . . ? C51 C52 C75 108.3(3) . . ? C53 C52 C64 110.5(3) . . ? C53 C52 C75 110.4(3) . . ? C64 C52 C75 106.7(3) . . ? N101 C53 C52 120.4(3) . . ? N101 C53 C54 109.7(3) . . ? C52 C53 C54 129.8(3) . . ? C53 C54 H54 126.6 . . ? C53 C54 C55 106.8(3) . . ? H54 C54 C55 126.6 . . ? C54 C55 H55 126.8 . . ? C54 C55 C56 106.4(3) . . ? H55 C55 C56 126.8 . . ? N101 C56 C55 108.9(3) . . ? N101 C56 C57 114.3(3) . . ? C55 C56 C57 136.7(3) . . ? N102 C57 C56 118.6(3) . . ? N102 C57 H57 120.7 . . ? C56 C57 H57 120.7 . . ? N102 C58 H58 107.2 . . ? N102 C58 C59 109.5(3) . . ? N102 C58 C63 115.5(3) . . ? H58 C58 C59 107.2 . . ? H58 C58 C63 107.2 . . ? C59 C58 C63 110.0(3) . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? C58 C59 C60 110.6(3) . . ? H59A C59 H59B 108.1 . . ? H59A C59 C60 109.5 . . ? H59B C59 C60 109.5 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? C59 C60 C61 110.7(3) . . ? H60A C60 H60B 108.1 . . ? H60A C60 C61 109.5 . . ? H60B C60 C61 109.5 . . ? C60 C61 H61A 109.3 . . ? C60 C61 H61B 109.3 . . ? C60 C61 C62 111.4(3) . . ? H61A C61 H61B 108.0 . . ? H61A C61 C62 109.3 . . ? H61B C61 C62 109.3 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? C61 C62 C63 110.8(4) . . ? H62A C62 H62B 108.1 . . ? H62A C62 C63 109.5 . . ? H62B C62 C63 109.5 . . ? C58 C63 C62 111.4(3) . . ? C58 C63 H63A 109.3 . . ? C58 C63 H63B 109.3 . . ? C62 C63 H63A 109.3 . . ? C62 C63 H63B 109.3 . . ? H63A C63 H63B 108.0 . . ? N103 C64 C52 120.6(3) . . ? N103 C64 C65 109.2(3) . . ? C52 C64 C65 130.0(3) . . ? C64 C65 H65 126.6 . . ? C64 C65 C66 106.7(3) . . ? H65 C65 C66 126.6 . . ? C65 C66 H66 127.1 . . ? C65 C66 C67 105.8(3) . . ? H66 C66 C67 127.1 . . ? N103 C67 C66 110.0(3) . . ? N103 C67 C68 114.3(3) . . ? C66 C67 C68 135.0(3) . . ? N104 C68 C67 118.2(3) . . ? N104 C68 H68 120.9 . . ? C67 C68 H68 120.9 . . ? N104 C69 H69 107.0 . . ? N104 C69 C70 116.2(3) . . ? N104 C69 C74 109.6(3) . . ? H69 C69 C70 107.0 . . ? H69 C69 C74 107.0 . . ? C70 C69 C74 109.5(3) . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? C69 C70 C71 110.6(3) . . ? H70A C70 H70B 108.1 . . ? H70A C70 C71 109.5 . . ? H70B C70 C71 109.5 . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? C70 C71 C72 110.9(3) . . ? H71A C71 H71B 108.1 . . ? H71A C71 C72 109.5 . . ? H71B C71 C72 109.5 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? C71 C72 C73 110.6(3) . . ? H72A C72 H72B 108.1 . . ? H72A C72 C73 109.5 . . ? H72B C72 C73 109.5 . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? C72 C73 C74 110.7(3) . . ? H73A C73 H73B 108.1 . . ? H73A C73 C74 109.5 . . ? H73B C73 C74 109.5 . . ? C69 C74 C73 111.1(3) . . ? C69 C74 H74A 109.4 . . ? C69 C74 H74B 109.4 . . ? C73 C74 H74A 109.4 . . ? C73 C74 H74B 109.4 . . ? H74A C74 H74B 108.0 . . ? N105 C75 C52 122.8(3) . . ? N105 C75 C76 107.8(3) . . ? C52 C75 C76 129.4(3) . . ? C75 C76 H76 126.2 . . ? C75 C76 C77 107.6(3) . . ? H76 C76 C77 126.2 . . ? C76 C77 H77 126.1 . . ? C76 C77 C78 107.8(3) . . ? H77 C77 C78 126.1 . . ? N105 C78 C77 106.7(3) . . ? N105 C78 C79 126.6(3) . . ? C77 C78 C79 126.4(3) . . ? N106 C79 C78 126.7(3) . . ? N106 C79 H79 116.7 . . ? C78 C79 H79 116.7 . . ? N106 C80 H80 109.0 . . ? N106 C80 C81 110.1(3) . . ? N106 C80 C85 109.2(3) . . ? H80 C80 C81 109.0 . . ? H80 C80 C85 109.0 . . ? C81 C80 C85 110.6(3) . . ? C80 C81 H81A 109.6 . . ? C80 C81 H81B 109.6 . . ? C80 C81 C82 110.2(3) . . ? H81A C81 H81B 108.1 . . ? H81A C81 C82 109.6 . . ? H81B C81 C82 109.6 . . ? C81 C82 H82A 109.4 . . ? C81 C82 H82B 109.4 . . ? C81 C82 C83 111.1(3) . . ? H82A C82 H82B 108.0 . . ? H82A C82 C83 109.4 . . ? H82B C82 C83 109.4 . . ? C82 C83 H83A 109.6 . . ? C82 C83 H83B 109.6 . . ? C82 C83 C84 110.2(3) . . ? H83A C83 H83B 108.1 . . ? H83A C83 C84 109.6 . . ? H83B C83 C84 109.6 . . ? C83 C84 H84A 109.6 . . ? C83 C84 H84B 109.6 . . ? C83 C84 C85 110.3(3) . . ? H84A C84 H84B 108.1 . . ? H84A C84 C85 109.6 . . ? H84B C84 C85 109.6 . . ? C80 C85 C84 110.0(3) . . ? C80 C85 H85A 109.7 . . ? C80 C85 H85B 109.7 . . ? C84 C85 H85A 109.7 . . ? C84 C85 H85B 109.7 . . ? H85A C85 H85B 108.2 . . ? N400 C401 C402 178.1(12) . . ? C401 C402 H40A 109.5 . . ? C401 C402 H40B 109.5 . . ? C401 C402 H40C 109.5 . . ? H40A C402 H40B 109.5 . . ? H40A C402 H40C 109.5 . . ? H40B C402 H40C 109.5 . . ? H31C C311 H31D 109.5 . . ? H31C C311 H31E 109.5 . . ? H31C C311 C312 109.5 . . ? H31D C311 H31E 109.5 . . ? H31D C311 C312 109.5 . . ? H31E C311 C312 109.5 . . ? C311 C312 H31F 110.0 . . ? C311 C312 H31G 110.0 . . ? C311 C312 O311 108.3(8) . . ? H31F C312 H31G 108.4 . . ? H31F C312 O311 110.0 . . ? H31G C312 O311 110.0 . . ? C312 O311 C313 110.2(7) . . ? O311 C313 H31H 110.0 . . ? O311 C313 H31I 110.0 . . ? O311 C313 C314 108.3(8) . . ? H31H C313 H31I 108.4 . . ? H31H C313 C314 110.0 . . ? H31I C313 C314 110.0 . . ? C313 C314 H31J 109.5 . . ? C313 C314 H31K 109.5 . . ? C313 C314 H31L 109.5 . . ? H31J C314 H31K 109.5 . . ? H31J C314 H31L 109.5 . . ? H31K C314 H31L 109.5 . . ? H32C C321 H32D 109.5 . . ? H32C C321 H32E 109.5 . . ? H32C C321 C322 109.5 . . ? H32D C321 H32E 109.5 . . ? H32D C321 C322 109.5 . . ? H32E C321 C322 109.5 . . ? C321 C322 H32F 111.6 . . ? C321 C322 H32G 111.6 . . ? C321 C322 O321 100.9(14) . . ? H32F C322 H32G 109.4 . . ? H32F C322 O321 111.6 . . ? H32G C322 O321 111.6 . . ? C322 O321 C323 110.4(12) . . ? O321 C323 H32H 105.7 . . ? O321 C323 H32I 105.7 . . ? O321 C323 C324 126.5(16) . . ? H32H C323 H32I 106.1 . . ? H32H C323 C324 105.7 . . ? H32I C323 C324 105.7 . . ? C323 C324 H32J 109.5 . . ? C323 C324 H32K 109.5 . . ? C323 C324 H32L 109.5 . . ? H32J C324 H32K 109.5 . . ? H32J C324 H32L 109.5 . . ? H32K C324 H32L 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 Cl1 Cu1 N1 C3 -106.3(3) . . . . ? Cl1 Cu1 N1 C6 89.7(2) . . . . ? N2 Cu1 N1 C3 165.5(3) . . . . ? N2 Cu1 N1 C6 1.5(2) . . . . ? N3 Cu1 N1 C3 1.6(3) . . . . ? N3 Cu1 N1 C6 -162.4(2) . . . . ? N4 Cu1 N1 C3 45.3(5) . . . . ? N4 Cu1 N1 C6 -118.7(4) . . . . ? Cl1 Cu1 N2 C7 -98.3(2) . . . . ? Cl1 Cu1 N2 C8 76.6(3) . . . . ? N1 Cu1 N2 C7 1.7(2) . . . . ? N1 Cu1 N2 C8 176.7(3) . . . . ? N3 Cu1 N2 C7 50.8(4) . . . . ? N3 Cu1 N2 C8 -134.3(3) . . . . ? N4 Cu1 N2 C7 164.6(2) . . . . ? N4 Cu1 N2 C8 -20.4(3) . . . . ? Cl1 Cu1 N3 C14 100.9(3) . . . . ? Cl1 Cu1 N3 C17 -107.9(2) . . . . ? N1 Cu1 N3 C14 2.2(3) . . . . ? N1 Cu1 N3 C17 153.4(2) . . . . ? N2 Cu1 N3 C14 -46.3(5) . . . . ? N2 Cu1 N3 C17 104.9(4) . . . . ? N4 Cu1 N3 C14 -164.7(3) . . . . ? N4 Cu1 N3 C17 -13.6(2) . . . . ? Cl1 Cu1 N4 C18 116.9(2) . . . . ? Cl1 Cu1 N4 C19 -53.3(3) . . . . ? N1 Cu1 N4 C18 -35.0(5) . . . . ? N1 Cu1 N4 C19 154.9(3) . . . . ? N2 Cu1 N4 C18 -151.1(2) . . . . ? N2 Cu1 N4 C19 38.7(3) . . . . ? N3 Cu1 N4 C18 9.1(2) . . . . ? N3 Cu1 N4 C19 -161.1(3) . . . . ? Cu1 N1 C3 C2 18.8(5) . . . . ? Cu1 N1 C3 C4 -165.8(3) . . . . ? C6 N1 C3 C2 -176.4(3) . . . . ? C6 N1 C3 C4 -1.0(4) . . . . ? C1 C2 C3 N1 -161.2(3) . . . . ? C1 C2 C3 C4 24.5(5) . . . . ? C14 C2 C3 N1 -39.8(4) . . . . ? C14 C2 C3 C4 145.9(4) . . . . ? C25 C2 C3 N1 80.9(4) . . . . ? C25 C2 C3 C4 -93.4(4) . . . . ? N1 C3 C4 C5 0.1(4) . . . . ? C2 C3 C4 C5 174.9(3) . . . . ? C3 C4 C5 C6 0.8(4) . . . . ? Cu1 N1 C6 C5 169.7(2) . . . . ? Cu1 N1 C6 C7 -4.3(4) . . . . ? C3 N1 C6 C5 1.5(4) . . . . ? C3 N1 C6 C7 -172.5(3) . . . . ? C4 C5 C6 N1 -1.4(4) . . . . ? C4 C5 C6 C7 170.6(4) . . . . ? Cu1 N2 C7 C6 -4.6(4) . . . . ? C8 N2 C7 C6 -179.9(3) . . . . ? N1 C6 C7 N2 6.0(5) . . . . ? C5 C6 C7 N2 -165.7(4) . . . . ? Cu1 N2 C8 C9 -157.5(3) . . . . ? Cu1 N2 C8 C13 77.4(3) . . . . ? C7 N2 C8 C9 17.1(5) . . . . ? C7 N2 C8 C13 -108.1(4) . . . . ? N2 C8 C9 C10 176.7(3) . . . . ? C13 C8 C9 C10 -58.6(4) . . . . ? C8 C9 C10 C11 57.8(5) . . . . ? C9 C10 C11 C12 -55.6(6) . . . . ? C10 C11 C12 C13 54.4(5) . . . . ? C11 C12 C13 C8 -55.5(5) . . . . ? N2 C8 C13 C12 -172.9(3) . . . . ? C9 C8 C13 C12 58.1(4) . . . . ? Cu1 N3 C14 C2 -26.3(5) . . . . ? Cu1 N3 C14 C15 153.5(3) . . . . ? C17 N3 C14 C2 -178.7(3) . . . . ? C17 N3 C14 C15 1.1(4) . . . . ? C1 C2 C14 N3 165.1(3) . . . . ? C1 C2 C14 C15 -14.7(5) . . . . ? C3 C2 C14 N3 43.4(4) . . . . ? C3 C2 C14 C15 -136.4(4) . . . . ? C25 C2 C14 N3 -74.5(4) . . . . ? C25 C2 C14 C15 105.7(4) . . . . ? N3 C14 C15 C16 -1.1(4) . . . . ? C2 C14 C15 C16 178.7(3) . . . . ? C14 C15 C16 C17 0.6(4) . . . . ? Cu1 N3 C17 C16 -159.6(2) . . . . ? Cu1 N3 C17 C18 15.8(4) . . . . ? C14 N3 C17 C16 -0.8(4) . . . . ? C14 N3 C17 C18 174.7(3) . . . . ? C15 C16 C17 N3 0.1(4) . . . . ? C15 C16 C17 C18 -174.0(4) . . . . ? Cu1 N4 C18 C17 -3.1(4) . . . . ? C19 N4 C18 C17 168.1(3) . . . . ? N3 C17 C18 N4 -8.1(4) . . . . ? C16 C17 C18 N4 165.8(4) . . . . ? Cu1 N4 C19 C20 92.1(3) . . . . ? Cu1 N4 C19 C24 -143.1(3) . . . . ? C18 N4 C19 C20 -77.4(4) . . . . ? C18 N4 C19 C24 47.5(4) . . . . ? N4 C19 C20 C21 -174.7(3) . . . . ? C24 C19 C20 C21 57.8(4) . . . . ? C19 C20 C21 C22 -57.9(5) . . . . ? C20 C21 C22 C23 56.1(5) . . . . ? C21 C22 C23 C24 -55.6(5) . . . . ? N4 C19 C24 C23 179.3(3) . . . . ? C20 C19 C24 C23 -56.3(4) . . . . ? C22 C23 C24 C19 55.6(4) . . . . ? C28 N5 C25 C2 175.9(3) . . . . ? C28 N5 C25 C26 -0.6(4) . . . . ? C1 C2 C25 N5 -162.4(3) . . . . ? C1 C2 C25 C26 13.2(5) . . . . ? C3 C2 C25 N5 -43.6(4) . . . . ? C3 C2 C25 C26 132.0(4) . . . . ? C14 C2 C25 N5 76.5(4) . . . . ? C14 C2 C25 C26 -107.9(4) . . . . ? N5 C25 C26 C27 0.5(4) . . . . ? C2 C25 C26 C27 -175.6(4) . . . . ? C25 C26 C27 C28 -0.3(5) . . . . ? C25 N5 C28 C27 0.4(4) . . . . ? C25 N5 C28 C29 -175.7(3) . . . . ? C26 C27 C28 N5 -0.1(5) . . . . ? C26 C27 C28 C29 176.0(4) . . . . ? C30 N6 C29 C28 175.2(3) . . . . ? N5 C28 C29 N6 -2.5(6) . . . . ? C27 C28 C29 N6 -177.9(4) . . . . ? C29 N6 C30 C31 -78.5(4) . . . . ? C29 N6 C30 C35 159.7(4) . . . . ? N6 C30 C31 C32 -177.7(3) . . . . ? C35 C30 C31 C32 -56.9(4) . . . . ? C30 C31 C32 C33 55.8(4) . . . . ? C31 C32 C33 C34 -56.0(4) . . . . ? C32 C33 C34 C35 55.9(5) . . . . ? N6 C30 C35 C34 179.4(3) . . . . ? C31 C30 C35 C34 57.9(4) . . . . ? C33 C34 C35 C30 -57.1(5) . . . . ? Cl2 Cu2 N101 C53 -100.4(3) . . . . ? Cl2 Cu2 N101 C56 107.0(2) . . . . ? N102 Cu2 N101 C53 165.9(3) . . . . ? N102 Cu2 N101 C56 13.4(2) . . . . ? N103 Cu2 N101 C53 -0.8(3) . . . . ? N103 Cu2 N101 C56 -153.3(2) . . . . ? N104 Cu2 N101 C53 48.9(5) . . . . ? N104 Cu2 N101 C56 -103.7(4) . . . . ? Cl2 Cu2 N102 C57 -115.9(2) . . . . ? Cl2 Cu2 N102 C58 53.1(3) . . . . ? N101 Cu2 N102 C57 -8.7(2) . . . . ? N101 Cu2 N102 C58 160.3(3) . . . . ? N103 Cu2 N102 C57 35.7(5) . . . . ? N103 Cu2 N102 C58 -155.3(3) . . . . ? N104 Cu2 N102 C57 150.7(2) . . . . ? N104 Cu2 N102 C58 -40.3(3) . . . . ? Cl2 Cu2 N103 C64 105.9(3) . . . . ? Cl2 Cu2 N103 C67 -90.8(2) . . . . ? N101 Cu2 N103 C64 -1.4(3) . . . . ? N101 Cu2 N103 C67 161.9(2) . . . . ? N102 Cu2 N103 C64 -45.3(5) . . . . ? N102 Cu2 N103 C67 117.9(4) . . . . ? N104 Cu2 N103 C64 -164.5(3) . . . . ? N104 Cu2 N103 C67 -1.2(2) . . . . ? Cl2 Cu2 N104 C68 98.8(2) . . . . ? Cl2 Cu2 N104 C69 -77.0(3) . . . . ? N101 Cu2 N104 C68 -52.2(4) . . . . ? N101 Cu2 N104 C69 132.0(3) . . . . ? N102 Cu2 N104 C68 -164.3(2) . . . . ? N102 Cu2 N104 C69 19.9(3) . . . . ? N103 Cu2 N104 C68 -1.8(2) . . . . ? N103 Cu2 N104 C69 -177.6(3) . . . . ? Cu2 N101 C53 C52 23.9(5) . . . . ? Cu2 N101 C53 C54 -154.6(3) . . . . ? C56 N101 C53 C52 177.3(3) . . . . ? C56 N101 C53 C54 -1.1(4) . . . . ? C51 C52 C53 N101 -164.6(3) . . . . ? C51 C52 C53 C54 13.6(5) . . . . ? C64 C52 C53 N101 -42.4(4) . . . . ? C64 C52 C53 C54 135.8(4) . . . . ? C75 C52 C53 N101 75.5(4) . . . . ? C75 C52 C53 C54 -106.4(4) . . . . ? N101 C53 C54 C55 0.8(4) . . . . ? C52 C53 C54 C55 -177.5(3) . . . . ? C53 C54 C55 C56 -0.2(4) . . . . ? Cu2 N101 C56 C55 160.7(2) . . . . ? Cu2 N101 C56 C57 -16.0(3) . . . . ? C53 N101 C56 C55 1.0(4) . . . . ? C53 N101 C56 C57 -175.6(3) . . . . ? C54 C55 C56 N101 -0.5(4) . . . . ? C54 C55 C56 C57 175.1(4) . . . . ? Cu2 N102 C57 C56 2.5(4) . . . . ? C58 N102 C57 C56 -167.7(3) . . . . ? N101 C56 C57 N102 8.7(4) . . . . ? C55 C56 C57 N102 -166.7(4) . . . . ? Cu2 N102 C58 C59 -93.6(3) . . . . ? Cu2 N102 C58 C63 141.7(3) . . . . ? C57 N102 C58 C59 74.6(4) . . . . ? C57 N102 C58 C63 -50.1(4) . . . . ? N102 C58 C59 C60 175.2(3) . . . . ? C63 C58 C59 C60 -56.9(4) . . . . ? C58 C59 C60 C61 57.5(4) . . . . ? C59 C60 C61 C62 -56.9(5) . . . . ? C60 C61 C62 C63 55.8(5) . . . . ? C61 C62 C63 C58 -55.6(4) . . . . ? N102 C58 C63 C62 -179.4(3) . . . . ? C59 C58 C63 C62 56.1(4) . . . . ? Cu2 N103 C64 C52 -20.0(5) . . . . ? Cu2 N103 C64 C65 164.4(3) . . . . ? C67 N103 C64 C52 175.9(3) . . . . ? C67 N103 C64 C65 0.3(4) . . . . ? C51 C52 C64 N103 163.1(3) . . . . ? C51 C52 C64 C65 -22.3(5) . . . . ? C53 C52 C64 N103 40.4(4) . . . . ? C53 C52 C64 C65 -144.9(4) . . . . ? C75 C52 C64 N103 -79.6(4) . . . . ? C75 C52 C64 C65 95.0(4) . . . . ? N103 C64 C65 C66 0.3(4) . . . . ? C52 C64 C65 C66 -174.8(3) . . . . ? C64 C65 C66 C67 -0.8(4) . . . . ? Cu2 N103 C67 C66 -168.4(2) . . . . ? Cu2 N103 C67 C68 3.9(4) . . . . ? C64 N103 C67 C66 -0.8(4) . . . . ? C64 N103 C67 C68 171.5(3) . . . . ? C65 C66 C67 N103 1.0(4) . . . . ? C65 C66 C67 C68 -169.1(4) . . . . ? Cu2 N104 C68 C67 4.5(4) . . . . ? C69 N104 C68 C67 -179.4(3) . . . . ? N103 C67 C68 N104 -5.7(5) . . . . ? C66 C67 C68 N104 164.0(3) . . . . ? Cu2 N104 C69 C70 158.8(2) . . . . ? Cu2 N104 C69 C74 -76.4(3) . . . . ? C68 N104 C69 C70 -16.6(5) . . . . ? C68 N104 C69 C74 108.2(3) . . . . ? N104 C69 C70 C71 -177.1(3) . . . . ? C74 C69 C70 C71 58.1(4) . . . . ? C69 C70 C71 C72 -57.7(4) . . . . ? C70 C71 C72 C73 56.1(4) . . . . ? C71 C72 C73 C74 -55.7(4) . . . . ? C72 C73 C74 C69 57.2(4) . . . . ? N104 C69 C74 C73 173.3(3) . . . . ? C70 C69 C74 C73 -58.1(4) . . . . ? C78 N105 C75 C52 -176.0(3) . . . . ? C78 N105 C75 C76 1.1(4) . . . . ? C51 C52 C75 N105 163.2(3) . . . . ? C51 C52 C75 C76 -13.2(5) . . . . ? C53 C52 C75 N105 -75.3(4) . . . . ? C53 C52 C75 C76 108.3(4) . . . . ? C64 C52 C75 N105 44.8(4) . . . . ? C64 C52 C75 C76 -131.6(4) . . . . ? N105 C75 C76 C77 -1.0(4) . . . . ? C52 C75 C76 C77 175.8(4) . . . . ? C75 C76 C77 C78 0.5(4) . . . . ? C75 N105 C78 C77 -0.8(4) . . . . ? C75 N105 C78 C79 174.3(3) . . . . ? C76 C77 C78 N105 0.1(4) . . . . ? C76 C77 C78 C79 -175.0(4) . . . . ? C80 N106 C79 C78 -176.5(3) . . . . ? N105 C78 C79 N106 3.7(6) . . . . ? C77 C78 C79 N106 177.8(4) . . . . ? C79 N106 C80 C81 82.1(4) . . . . ? C79 N106 C80 C85 -156.4(3) . . . . ? N106 C80 C81 C82 177.7(3) . . . . ? C85 C80 C81 C82 57.0(4) . . . . ? C80 C81 C82 C83 -56.3(4) . . . . ? C81 C82 C83 C84 57.2(4) . . . . ? C82 C83 C84 C85 -58.2(5) . . . . ? N106 C80 C85 C84 -179.5(3) . . . . ? C81 C80 C85 C84 -58.3(4) . . . . ? C83 C84 C85 C80 59.0(5) . . . . ? C311 C312 O311 C313 177.5(9) . . . . ? C312 O311 C313 C314 169.5(9) . . . . ? C321 C322 O321 C323 -174.0(17) . . . . ? C322 O321 C323 C324 4(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N5 H5N Cl1 0.88 2.48 3.271(3) 149.3 . N5 H5N N1 0.88 2.50 3.040(4) 120.0 . N6 H6 Cl1 0.88 2.26 3.099(3) 160.5 . N105 H105 Cl2 0.88 2.45 3.242(3) 150.0 . N105 H105 N103 0.88 2.52 3.041(4) 119.0 . N106 H106 Cl2 0.88 2.25 3.097(3) 160.4 . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 75.91 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.090 _refine_diff_density_min -0.666 _refine_diff_density_rms 0.072 _vrf_PLAT411_CuClH2L1 ; PROBLEM: Short Inter H...H Contact H10A .. H32F .. 1.33 Ang. RESPONSE: This apparent short distance is an artefact of disorder modelling of the ether of crystallization. It is not significant. ; _vrf_STRVA01_CuClH2L1 ; PROBLEM: Flack test results are ambiguous. RESPONSE: We comment on this in the Supplementary Information ; _vrf_PLAT202_CuClH2L1 ; PROBLEM: Isotropic non-H Atoms in Anion/Solvent ......... 5 RESPONSE: The ether of crystallization was refined using an isotropic disorder model. ; data_[Ti(OiPr)2(H4L2b)] _database_code_depnum_ccdc_archive 'CCDC 866708' #TrackingRef '- revised_combined.cif' # local name john_ti _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H45 N9 O5 Ti' _chemical_formula_weight 683.67 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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.704(10) _cell_length_b 35.30(3) _cell_length_c 9.483(12) _cell_angle_alpha 90.00 _cell_angle_beta 112.407(12) _cell_angle_gamma 90.00 _cell_volume 3622(7) _cell_formula_units_Z 4 _cell_measurement_temperature 160 _cell_measurement_reflns_used 5234 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.254 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 0.287 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9449 _exptl_absorpt_correction_T_max 0.9449 _exptl_absorpt_process_details 'CrystalClear, Rigaku 2010' _exptl_special_details ; ? ; _diffrn_ambient_temperature 160 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'XtaLABmini: Fixed Chi 2 circle' _diffrn_measurement_device_type 'Rigaku Mercury375R (2x2 bin mode)' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 19852 _diffrn_reflns_av_R_equivalents 0.1237 _diffrn_reflns_av_sigmaI/netI 0.1103 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6022 _reflns_number_gt 4080 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 rc12 (Rigaku, 2009)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 rc12 (Rigaku, 2009)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 rc12 (Rigaku, 2009)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0700P)^2^+2.6439P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6022 _refine_ls_number_parameters 435 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1287 _refine_ls_R_factor_gt 0.0871 _refine_ls_wR_factor_ref 0.2089 _refine_ls_wR_factor_gt 0.1850 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.115 _refine_ls_shift/su_max 0.014 _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 Ti1 Ti 0.37538(8) 0.08647(2) 0.84008(10) 0.0289(2) Uani 1 1 d . . . O1 O 0.2403(3) 0.06462(9) 0.6393(4) 0.0369(8) Uani 1 1 d . . . O3 O -0.0319(3) 0.26949(9) 0.7631(4) 0.0361(8) Uani 1 1 d . . . O2 O 0.5052(3) 0.05635(8) 1.0224(4) 0.0351(8) Uani 1 1 d . . . O4 O 0.4845(3) 0.07580(9) 0.7530(4) 0.0356(8) Uani 1 1 d . . . O5 O 0.2721(3) 0.07107(9) 0.9279(4) 0.0381(8) Uani 1 1 d . . . N2 N 0.1003(4) 0.07720(12) 0.4058(5) 0.0395(10) Uani 1 1 d . . . H1 H 0.0678 0.0938 0.3356 0.047 Uiso 1 1 calc R . . N1 N 0.2917(3) 0.13405(10) 0.7188(4) 0.0285(9) Uani 1 1 d . . . N5 N 0.1759(4) 0.22467(10) 0.8719(4) 0.0286(9) Uani 1 1 d . . . H3 H 0.1689 0.2369 0.7907 0.034 Uiso 1 1 calc R . . N6 N -0.0718(4) 0.25935(11) 0.9739(5) 0.0372(10) Uani 1 1 d . . . H4 H -0.0506 0.2482 1.0608 0.045 Uiso 1 1 calc R . . N3 N 0.4686(3) 0.12854(10) 0.9916(4) 0.0281(9) Uani 1 1 d . . . N4 N 0.6642(4) 0.05972(11) 1.2496(5) 0.0382(10) Uani 1 1 d . . . H6 H 0.7128 0.0738 1.3212 0.046 Uiso 1 1 calc R . . N7 N 0.8539(5) 0.09613(17) 0.5326(7) 0.0687(16) Uani 1 1 d . . . N8 N 0.9430(6) 0.12527(17) 0.1543(7) 0.0808(19) Uani 1 1 d . . . N9 N 0.6491(8) 0.1971(3) 0.6397(8) 0.124(3) Uani 1 1 d . . . C1 C 0.1832(4) 0.08839(14) 0.5372(5) 0.0334(11) Uani 1 1 d . . . C2 C 0.2128(5) 0.12724(13) 0.5721(5) 0.0324(11) Uani 1 1 d . . . C3 C 0.1785(5) 0.16117(14) 0.4948(6) 0.0399(12) Uani 1 1 d . . . H3A H 0.1250 0.1645 0.3939 0.048 Uiso 1 1 calc R . . C4 C 0.2401(5) 0.18920(14) 0.5986(6) 0.0409(13) Uani 1 1 d . . . H4A H 0.2370 0.2151 0.5791 0.049 Uiso 1 1 calc R . . C5 C 0.3063(4) 0.17200(12) 0.7345(5) 0.0297(10) Uani 1 1 d . . . C6 C 0.3690(4) 0.19130(12) 0.8876(5) 0.0302(10) Uani 1 1 d . . . C7 C 0.4627(4) 0.16682(12) 1.0047(5) 0.0292(10) Uani 1 1 d . . . C8 C 0.5484(5) 0.17789(14) 1.1434(6) 0.0399(12) Uani 1 1 d . . . H8 H 0.5622 0.2026 1.1799 0.048 Uiso 1 1 calc R . . C9 C 0.6106(5) 0.14611(13) 1.2197(6) 0.0364(11) Uani 1 1 d . . . H9 H 0.6736 0.1452 1.3160 0.044 Uiso 1 1 calc R . . C10 C 0.5601(4) 0.11602(13) 1.1238(5) 0.0313(11) Uani 1 1 d . . . C11 C 0.5767(4) 0.07577(13) 1.1318(6) 0.0304(11) Uani 1 1 d . . . C12 C 0.2682(4) 0.19989(12) 0.9472(5) 0.0301(10) Uani 1 1 d . . . C13 C 0.2470(5) 0.18664(13) 1.0689(6) 0.0349(11) Uani 1 1 d . . . H13 H 0.2960 0.1693 1.1403 0.042 Uiso 1 1 calc R . . C14 C 0.1381(5) 0.20356(12) 1.0693(6) 0.0343(11) Uani 1 1 d . . . H14 H 0.1023 0.1995 1.1402 0.041 Uiso 1 1 calc R . . C15 C 0.0952(4) 0.22699(12) 0.9463(5) 0.0265(10) Uani 1 1 d . . . C16 C -0.0072(4) 0.25327(13) 0.8872(5) 0.0296(10) Uani 1 1 d . . . C17 C 0.0615(6) 0.03841(15) 0.3743(7) 0.0507(14) Uani 1 1 d . . . H17A H 0.1310 0.0230 0.3815 0.061 Uiso 1 1 calc R . . H17B H -0.0010 0.0365 0.2734 0.061 Uiso 1 1 calc R . . H17C H 0.0284 0.0298 0.4471 0.061 Uiso 1 1 calc R . . C18 C -0.1771(6) 0.2845(2) 0.9240(7) 0.066(2) Uani 1 1 d . . . H18A H -0.2023 0.2895 1.0074 0.079 Uiso 1 1 calc R . . H18B H -0.2440 0.2729 0.8419 0.079 Uiso 1 1 calc R . . H18C H -0.1549 0.3079 0.8894 0.079 Uiso 1 1 calc R . . C19 C 0.6807(5) 0.01910(14) 1.2615(6) 0.0431(13) Uani 1 1 d . . . H19A H 0.6940 0.0098 1.1739 0.052 Uiso 1 1 calc R . . H19B H 0.6080 0.0075 1.2662 0.052 Uiso 1 1 calc R . . H19C H 0.7508 0.0131 1.3522 0.052 Uiso 1 1 calc R . . C20 C 0.5876(5) 0.05433(15) 0.7617(7) 0.0476(14) Uani 1 1 d . . . H20 H 0.5884 0.0312 0.8193 0.057 Uiso 1 1 calc R . . C21 C 0.5772(7) 0.0430(2) 0.6054(8) 0.081(2) Uani 1 1 d . . . H21A H 0.5800 0.0651 0.5483 0.098 Uiso 1 1 calc R . . H21B H 0.5003 0.0300 0.5545 0.098 Uiso 1 1 calc R . . H21C H 0.6445 0.0265 0.6131 0.098 Uiso 1 1 calc R . . C22 C 0.7051(5) 0.0755(2) 0.8452(8) 0.0650(18) Uani 1 1 d . . . H22A H 0.7107 0.0813 0.9466 0.078 Uiso 1 1 calc R . . H22B H 0.7055 0.0986 0.7921 0.078 Uiso 1 1 calc R . . H22C H 0.7744 0.0602 0.8505 0.078 Uiso 1 1 calc R . . C23 C 0.2610(5) 0.04932(15) 1.0463(6) 0.0452(13) Uani 1 1 d . . . H23 H 0.3228 0.0291 1.0735 0.054 Uiso 1 1 calc R . . C24 C 0.1342(7) 0.0319(2) 0.9911(9) 0.077(2) Uani 1 1 d . . . H24A H 0.1276 0.0158 1.0692 0.093 Uiso 1 1 calc R . . H24B H 0.1211 0.0171 0.9011 0.093 Uiso 1 1 calc R . . H24C H 0.0731 0.0515 0.9677 0.093 Uiso 1 1 calc R . . C25 C 0.2849(6) 0.0743(2) 1.1836(7) 0.0664(18) Uani 1 1 d . . . H25A H 0.2241 0.0941 1.1582 0.080 Uiso 1 1 calc R . . H25B H 0.3658 0.0853 1.2140 0.080 Uiso 1 1 calc R . . H25C H 0.2800 0.0595 1.2659 0.080 Uiso 1 1 calc R . . C26 C 0.9219(5) 0.11227(18) 0.6308(7) 0.0499(14) Uani 1 1 d . . . C27 C 1.0080(6) 0.1332(2) 0.7555(8) 0.070(2) Uani 1 1 d . . . H27A H 1.0241 0.1573 0.7193 0.084 Uiso 1 1 calc R . . H27B H 1.0838 0.1193 0.7990 0.084 Uiso 1 1 calc R . . H27C H 0.9739 0.1372 0.8317 0.084 Uiso 1 1 calc R . . C28 C 0.8711(6) 0.14681(18) 0.0884(7) 0.0549(16) Uani 1 1 d . . . C29 C 0.7798(6) 0.17365(16) 0.0014(7) 0.0545(15) Uani 1 1 d . . . H29A H 0.7838 0.1957 0.0625 0.065 Uiso 1 1 calc R . . H29B H 0.6992 0.1624 -0.0293 0.065 Uiso 1 1 calc R . . H29C H 0.7950 0.1808 -0.0875 0.065 Uiso 1 1 calc R . . C30 C 0.5756(7) 0.1759(2) 0.5797(8) 0.069(2) Uani 1 1 d . . . C31 C 0.4794(6) 0.1499(2) 0.5053(8) 0.0690(19) Uani 1 1 d . . . H31A H 0.4016 0.1630 0.4686 0.083 Uiso 1 1 calc R . . H31B H 0.4782 0.1306 0.5759 0.083 Uiso 1 1 calc R . . H31C H 0.4929 0.1386 0.4210 0.083 Uiso 1 1 calc R . . C41 C 0.4312(5) 0.22848(13) 0.8679(6) 0.0396(12) Uani 1 1 d . . . H41A H 0.4650 0.2415 0.9640 0.048 Uiso 1 1 calc R . . H41B H 0.3710 0.2443 0.7944 0.048 Uiso 1 1 calc R . . H41C H 0.4963 0.2227 0.8332 0.048 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 Ti1 0.0299(5) 0.0291(4) 0.0267(5) -0.0005(3) 0.0096(4) -0.0003(4) O1 0.038(2) 0.0401(18) 0.0263(19) -0.0013(14) 0.0050(17) -0.0026(15) O3 0.036(2) 0.0493(19) 0.023(2) 0.0038(14) 0.0114(17) 0.0079(16) O2 0.0334(19) 0.0332(17) 0.031(2) -0.0019(14) 0.0041(17) -0.0020(15) O4 0.036(2) 0.0396(17) 0.035(2) -0.0015(14) 0.0169(17) 0.0079(15) O5 0.036(2) 0.0442(19) 0.036(2) 0.0035(14) 0.0148(17) -0.0050(15) N2 0.039(3) 0.053(3) 0.022(2) -0.0010(17) 0.006(2) -0.004(2) N1 0.026(2) 0.035(2) 0.025(2) 0.0034(15) 0.0103(19) 0.0028(16) N5 0.031(2) 0.034(2) 0.021(2) 0.0004(14) 0.0106(19) 0.0026(17) N6 0.036(2) 0.052(2) 0.026(2) 0.0082(18) 0.016(2) 0.013(2) N3 0.027(2) 0.0322(19) 0.026(2) -0.0015(15) 0.0110(19) -0.0021(16) N4 0.040(3) 0.036(2) 0.032(3) 0.0014(17) 0.007(2) 0.0008(19) N7 0.059(4) 0.087(4) 0.051(4) -0.009(3) 0.011(3) -0.017(3) N8 0.064(4) 0.082(4) 0.064(4) 0.014(3) -0.012(3) 0.006(3) N9 0.114(7) 0.200(9) 0.053(5) 0.013(5) 0.028(5) -0.078(7) C1 0.029(3) 0.045(3) 0.028(3) 0.005(2) 0.013(2) 0.003(2) C2 0.033(3) 0.042(3) 0.023(3) -0.0007(19) 0.011(2) 0.002(2) C3 0.047(3) 0.044(3) 0.027(3) 0.004(2) 0.013(3) 0.011(2) C4 0.055(4) 0.035(3) 0.037(3) 0.009(2) 0.022(3) 0.007(2) C5 0.031(3) 0.030(2) 0.032(3) -0.0016(18) 0.017(2) 0.004(2) C6 0.031(3) 0.028(2) 0.031(3) -0.0004(18) 0.011(2) 0.002(2) C7 0.028(3) 0.032(2) 0.030(3) -0.0017(18) 0.014(2) 0.0025(19) C8 0.034(3) 0.037(3) 0.042(3) -0.012(2) 0.007(3) 0.002(2) C9 0.029(3) 0.040(3) 0.032(3) -0.008(2) 0.003(2) -0.003(2) C10 0.029(3) 0.036(2) 0.030(3) 0.0019(19) 0.012(2) 0.003(2) C11 0.026(3) 0.034(2) 0.034(3) 0.001(2) 0.015(2) -0.002(2) C12 0.030(3) 0.029(2) 0.029(3) -0.0010(18) 0.010(2) -0.0002(19) C13 0.034(3) 0.039(3) 0.032(3) 0.001(2) 0.012(2) 0.005(2) C14 0.041(3) 0.032(2) 0.034(3) 0.0008(19) 0.019(3) -0.002(2) C15 0.025(2) 0.032(2) 0.022(3) -0.0046(17) 0.009(2) 0.0001(19) C16 0.028(3) 0.039(2) 0.022(3) -0.0013(19) 0.010(2) 0.001(2) C17 0.051(4) 0.057(3) 0.037(3) -0.007(2) 0.008(3) -0.010(3) C18 0.066(4) 0.091(5) 0.053(4) 0.021(3) 0.038(4) 0.044(4) C19 0.043(3) 0.042(3) 0.035(3) 0.006(2) 0.004(3) -0.001(2) C20 0.040(3) 0.043(3) 0.063(4) 0.000(2) 0.023(3) 0.006(2) C21 0.064(5) 0.103(6) 0.085(6) -0.052(4) 0.037(4) 0.001(4) C22 0.037(4) 0.090(5) 0.064(5) -0.011(3) 0.015(3) -0.006(3) C23 0.055(4) 0.045(3) 0.042(3) 0.003(2) 0.026(3) -0.008(3) C24 0.082(5) 0.087(5) 0.078(5) -0.010(4) 0.047(5) -0.041(4) C25 0.065(4) 0.098(5) 0.044(4) -0.007(3) 0.029(4) -0.009(4) C26 0.035(3) 0.072(4) 0.044(4) -0.002(3) 0.017(3) -0.004(3) C27 0.050(4) 0.097(5) 0.064(5) -0.037(4) 0.023(4) -0.019(4) C28 0.052(4) 0.071(4) 0.031(3) 0.002(3) 0.004(3) -0.018(3) C29 0.054(4) 0.058(3) 0.049(4) 0.000(3) 0.018(3) -0.002(3) C30 0.054(4) 0.118(6) 0.041(4) 0.025(4) 0.023(4) -0.008(4) C31 0.069(5) 0.086(5) 0.064(5) 0.011(4) 0.038(4) 0.004(4) C41 0.039(3) 0.032(2) 0.052(4) 0.004(2) 0.021(3) 0.000(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Ti1 O5 1.794(3) . ? Ti1 O4 1.806(3) . ? Ti1 N1 2.060(4) . ? Ti1 N3 2.065(4) . ? Ti1 O2 2.104(4) . ? Ti1 O1 2.104(4) . ? O1 C1 1.263(6) . ? O3 C16 1.241(6) . ? O2 C11 1.259(6) . ? O4 C20 1.400(6) . ? O5 C23 1.406(6) . ? N2 C1 1.315(6) . ? N2 C17 1.438(7) . ? N2 H1 0.8600 . ? N1 C5 1.352(6) . ? N1 C2 1.366(6) . ? N5 C12 1.362(6) . ? N5 C15 1.381(5) . ? N5 H3 0.8600 . ? N6 C16 1.329(6) . ? N6 C18 1.446(7) . ? N6 H4 0.8600 . ? N3 C7 1.361(6) . ? N3 C10 1.375(6) . ? N4 C11 1.321(6) . ? N4 C19 1.445(6) . ? N4 H6 0.8600 . ? N7 C26 1.123(7) . ? N8 C28 1.129(8) . ? N9 C30 1.119(10) . ? C1 C2 1.422(7) . ? C2 C3 1.382(7) . ? C3 C4 1.388(7) . ? C3 H3A 0.9300 . ? C4 C5 1.367(7) . ? C4 H4A 0.9300 . ? C5 C6 1.516(7) . ? C6 C7 1.501(6) . ? C6 C12 1.520(6) . ? C6 C41 1.546(6) . ? C7 C8 1.372(7) . ? C8 C9 1.383(7) . ? C8 H8 0.9300 . ? C9 C10 1.376(7) . ? C9 H9 0.9300 . ? C10 C11 1.432(7) . ? C12 C13 1.354(7) . ? C13 C14 1.409(7) . ? C13 H13 0.9300 . ? C14 C15 1.360(6) . ? C14 H14 0.9300 . ? C15 C16 1.448(6) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.495(8) . ? C20 C22 1.499(8) . ? C20 H20 0.9800 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.504(8) . ? C23 C25 1.508(8) . ? C23 H23 0.9800 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.433(8) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.431(9) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C31 1.414(10) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Ti1 O4 150.29(15) . . ? O5 Ti1 N1 104.19(16) . . ? O4 Ti1 N1 100.57(15) . . ? O5 Ti1 N3 99.53(16) . . ? O4 Ti1 N3 100.96(16) . . ? N1 Ti1 N3 79.33(16) . . ? O5 Ti1 O2 82.43(16) . . ? O4 Ti1 O2 81.69(16) . . ? N1 Ti1 O2 155.73(14) . . ? N3 Ti1 O2 76.53(15) . . ? O5 Ti1 O1 84.38(17) . . ? O4 Ti1 O1 85.88(17) . . ? N1 Ti1 O1 76.14(15) . . ? N3 Ti1 O1 155.36(14) . . ? O2 Ti1 O1 128.07(14) . . ? C1 O1 Ti1 116.5(3) . . ? C11 O2 Ti1 116.6(3) . . ? C20 O4 Ti1 146.1(3) . . ? C23 O5 Ti1 145.1(3) . . ? C1 N2 C17 122.9(5) . . ? C1 N2 H1 118.5 . . ? C17 N2 H1 118.5 . . ? C5 N1 C2 107.1(4) . . ? C5 N1 Ti1 137.2(3) . . ? C2 N1 Ti1 114.7(3) . . ? C12 N5 C15 109.3(4) . . ? C12 N5 H3 125.3 . . ? C15 N5 H3 125.3 . . ? C16 N6 C18 120.8(4) . . ? C16 N6 H4 119.6 . . ? C18 N6 H4 119.6 . . ? C7 N3 C10 106.5(4) . . ? C7 N3 Ti1 138.2(3) . . ? C10 N3 Ti1 115.1(3) . . ? C11 N4 C19 121.9(4) . . ? C11 N4 H6 119.0 . . ? C19 N4 H6 119.0 . . ? O1 C1 N2 120.7(5) . . ? O1 C1 C2 116.8(5) . . ? N2 C1 C2 122.4(4) . . ? N1 C2 C3 109.6(4) . . ? N1 C2 C1 114.6(4) . . ? C3 C2 C1 135.8(5) . . ? C2 C3 C4 105.9(5) . . ? C2 C3 H3A 127.0 . . ? C4 C3 H3A 127.0 . . ? C5 C4 C3 107.8(4) . . ? C5 C4 H4A 126.1 . . ? C3 C4 H4A 126.1 . . ? N1 C5 C4 109.5(4) . . ? N1 C5 C6 123.1(4) . . ? C4 C5 C6 126.7(4) . . ? C7 C6 C5 113.6(4) . . ? C7 C6 C12 106.9(4) . . ? C5 C6 C12 106.5(4) . . ? C7 C6 C41 109.5(4) . . ? C5 C6 C41 110.1(4) . . ? C12 C6 C41 110.1(4) . . ? N3 C7 C8 109.0(4) . . ? N3 C7 C6 123.5(4) . . ? C8 C7 C6 127.3(4) . . ? C7 C8 C9 108.5(4) . . ? C7 C8 H8 125.7 . . ? C9 C8 H8 125.7 . . ? C10 C9 C8 105.8(5) . . ? C10 C9 H9 127.1 . . ? C8 C9 H9 127.1 . . ? N3 C10 C9 110.1(4) . . ? N3 C10 C11 114.2(4) . . ? C9 C10 C11 135.6(5) . . ? O2 C11 N4 121.4(4) . . ? O2 C11 C10 117.5(4) . . ? N4 C11 C10 121.1(4) . . ? C13 C12 N5 107.6(4) . . ? C13 C12 C6 132.0(4) . . ? N5 C12 C6 120.4(4) . . ? C12 C13 C14 108.4(4) . . ? C12 C13 H13 125.8 . . ? C14 C13 H13 125.8 . . ? C15 C14 C13 107.2(4) . . ? C15 C14 H14 126.4 . . ? C13 C14 H14 126.4 . . ? C14 C15 N5 107.5(4) . . ? C14 C15 C16 134.6(4) . . ? N5 C15 C16 117.8(4) . . ? O3 C16 N6 122.1(4) . . ? O3 C16 C15 121.4(4) . . ? N6 C16 C15 116.5(4) . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N6 C18 H18A 109.5 . . ? N6 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N6 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N4 C19 H19A 109.5 . . ? N4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O4 C20 C21 110.1(5) . . ? O4 C20 C22 111.0(5) . . ? C21 C20 C22 111.7(5) . . ? O4 C20 H20 108.0 . . ? C21 C20 H20 108.0 . . ? C22 C20 H20 108.0 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O5 C23 C24 109.0(5) . . ? O5 C23 C25 109.1(5) . . ? C24 C23 C25 112.0(5) . . ? O5 C23 H23 108.9 . . ? C24 C23 H23 108.9 . . ? C25 C23 H23 108.9 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N7 C26 C27 179.4(8) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N8 C28 C29 178.5(8) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N9 C30 C31 177.8(10) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C6 C41 H41A 109.5 . . ? C6 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C6 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 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 O5 Ti1 O1 C1 113.0(3) . . . . ? O4 Ti1 O1 C1 -95.1(3) . . . . ? N1 Ti1 O1 C1 6.9(3) . . . . ? N3 Ti1 O1 C1 12.4(5) . . . . ? O2 Ti1 O1 C1 -171.2(3) . . . . ? O5 Ti1 O2 C11 -102.7(3) . . . . ? O4 Ti1 O2 C11 102.5(3) . . . . ? N1 Ti1 O2 C11 5.1(5) . . . . ? N3 Ti1 O2 C11 -1.0(3) . . . . ? O1 Ti1 O2 C11 -179.5(3) . . . . ? O5 Ti1 O4 C20 -45.4(7) . . . . ? N1 Ti1 O4 C20 168.5(6) . . . . ? N3 Ti1 O4 C20 87.4(6) . . . . ? O2 Ti1 O4 C20 13.0(6) . . . . ? O1 Ti1 O4 C20 -116.5(6) . . . . ? O4 Ti1 O5 C23 54.7(7) . . . . ? N1 Ti1 O5 C23 -159.7(5) . . . . ? N3 Ti1 O5 C23 -78.4(6) . . . . ? O2 Ti1 O5 C23 -3.5(5) . . . . ? O1 Ti1 O5 C23 126.1(6) . . . . ? O5 Ti1 N1 C5 103.1(4) . . . . ? O4 Ti1 N1 C5 -93.5(4) . . . . ? N3 Ti1 N1 C5 5.8(4) . . . . ? O2 Ti1 N1 C5 -0.2(7) . . . . ? O1 Ti1 N1 C5 -176.5(5) . . . . ? O5 Ti1 N1 C2 -90.2(3) . . . . ? O4 Ti1 N1 C2 73.2(3) . . . . ? N3 Ti1 N1 C2 172.5(3) . . . . ? O2 Ti1 N1 C2 166.4(3) . . . . ? O1 Ti1 N1 C2 -9.8(3) . . . . ? O5 Ti1 N3 C7 -96.0(5) . . . . ? O4 Ti1 N3 C7 105.7(5) . . . . ? N2 Ti1 N3 C7 6.8(4) . . . . ? O2 Ti1 N3 C7 -175.7(5) . . . . ? O1 Ti1 N3 C7 1.4(7) . . . . ? O5 Ti1 N3 C10 79.5(3) . . . . ? O4 Ti1 N3 C10 -78.9(3) . . . . ? N1 Ti1 N3 C10 -177.7(3) . . . . ? O2 Ti1 N3 C10 -0.3(3) . . . . ? O1 Ti1 N3 C10 176.8(3) . . . . ? Ti1 O1 C1 N2 177.6(3) . . . . ? Ti1 O1 C1 C2 -2.7(5) . . . . ? C17 N2 C1 O1 5.5(7) . . . . ? C17 N2 C1 C2 -174.2(5) . . . . ? C5 N1 C2 C3 0.5(5) . . . . ? Ti1 N1 C2 C3 -170.1(3) . . . . ? C5 N1 C2 C1 -177.7(4) . . . . ? Ti1 N1 C2 C1 11.7(5) . . . . ? O1 C1 C2 N1 -6.0(6) . . . . ? N2 C1 C2 N1 173.7(4) . . . . ? O1 C1 C2 C3 176.5(5) . . . . ? N2 C1 C2 C3 -3.8(9) . . . . ? N1 C2 C3 C4 0.7(6) . . . . ? C1 C2 C3 C4 178.3(5) . . . . ? C2 C3 C4 C5 -1.6(6) . . . . ? C2 N1 C5 C4 -1.5(5) . . . . ? Ti1 N1 C5 C4 165.9(3) . . . . ? C2 N1 C5 C6 169.0(4) . . . . ? Ti1 N1 C5 C6 -23.6(7) . . . . ? C3 C4 C5 N1 1.9(6) . . . . ? C3 C4 C5 C6 -168.1(4) . . . . ? N1 C5 C6 C7 27.5(6) . . . . ? C4 C5 C6 C7 -163.7(5) . . . . ? N1 C5 C6 C12 -90.0(5) . . . . ? C4 C5 C6 C12 78.8(6) . . . . ? N1 C5 C6 C41 150.7(4) . . . . ? C4 C5 C6 C41 -40.5(7) . . . . ? C10 N3 C7 C8 -0.5(5) . . . . ? Ti1 N3 C7 C8 175.2(3) . . . . ? C10 N3 C7 C6 -176.4(4) . . . . ? Ti1 N3 C7 C6 -0.7(7) . . . . ? C5 C6 C7 N3 -16.7(6) . . . . ? C12 C6 C7 N3 100.5(5) . . . . ? C41 C6 C7 N3 -140.3(4) . . . . ? C5 C6 C7 C8 168.2(5) . . . . ? C12 C6 C7 C8 -74.6(6) . . . . ? C41 C6 C7 C8 44.6(6) . . . . ? N3 C7 C8 C9 0.4(6) . . . . ? C6 C7 C8 C9 176.0(4) . . . . ? C7 C8 C9 C10 -0.1(6) . . . . ? C7 N3 C10 C9 0.5(5) . . . . ? Ti1 N3 C10 C9 -176.4(3) . . . . ? C7 N3 C10 C11 178.2(4) . . . . ? Ti1 N3 C10 C11 1.3(5) . . . . ? C8 C9 C10 N3 -0.2(6) . . . . ? C8 C9 C10 C11 -177.3(5) . . . . ? Ti1 O2 C11 N4 -177.7(3) . . . . ? Ti1 O2 C11 C10 2.1(5) . . . . ? C19 N4 C11 O2 -1.7(7) . . . . ? C19 N4 C11 C10 178.5(4) . . . . ? N3 C10 C11 O2 -2.3(6) . . . . ? C9 C10 C11 O2 174.7(5) . . . . ? N3 C10 C11 N4 177.5(4) . . . . ? C9 C10 C11 N4 -5.5(9) . . . . ? C15 N5 C12 C13 -0.3(5) . . . . ? C15 N5 C12 C6 178.8(4) . . . . ? C7 C6 C12 C13 -7.6(7) . . . . ? C5 C6 C12 C13 114.2(6) . . . . ? C41 C6 C12 C13 -126.4(6) . . . . ? C7 C6 C12 N5 173.7(4) . . . . ? C5 C6 C12 N5 -64.5(5) . . . . ? C41 C6 C12 N5 54.8(6) . . . . ? N5 C12 C13 C14 0.2(5) . . . . ? C6 C12 C13 C14 -178.7(5) . . . . ? C12 C13 C14 C15 0.0(6) . . . . ? C13 C14 C15 N5 -0.1(5) . . . . ? C13 C14 C15 C16 -176.6(5) . . . . ? C12 N5 C15 C14 0.2(5) . . . . ? C12 N5 C15 C16 177.4(4) . . . . ? C18 N6 C16 O3 2.0(8) . . . . ? C18 N6 C16 C15 -178.9(5) . . . . ? C14 C15 C16 O3 -174.4(5) . . . . ? N5 C15 C16 O3 9.4(7) . . . . ? C14 C15 C16 N6 6.5(8) . . . . ? N5 C15 C16 N6 -169.8(4) . . . . ? Ti1 O4 C20 C21 143.2(5) . . . . ? Ti1 O4 C20 C22 -92.6(7) . . . . ? Ti1 O5 C23 C24 -145.4(5) . . . . ? Ti1 O5 C23 C25 92.1(6) . . . . ? 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 N2 H1 N8 0.86 2.10 2.938(7) 163.6 1_455 N6 H4 O3 0.86 1.95 2.792(6) 166.7 4_566 N4 H6 N7 0.86 2.20 3.038(7) 165.5 1_556 _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.322 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.069 _vrf_PLAT029_TiOiPr2H4L2b ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.945 RESPONSE: This small amount of missing data is unlikely to affect the refinement. ;