Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Charles Harding' _publ_contact_author_address ; Department of Chemistry Open University Walton Hall Milton Keynes BUCKS MK7 6AA UNITED KINGDOM ; _publ_contact_author_email C.J.HARDING@OPEN.AC.UK _publ_section_title ; N-methylation of macrobicycles reduces encapsulation ability ; loop_ _publ_author_name 'C. Harding' 'Sofia Derossi' 'David Farrell' 'V. McKee' 'Jane Nelson' data_Compound1(zof4) _database_code_depnum_ccdc_archive 'CCDC 630225' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H74 Cl2 N10 O8' _chemical_formula_weight 966.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 31.429(3) _cell_length_b 9.9882(8) _cell_length_c 16.6318(14) _cell_angle_alpha 90.00 _cell_angle_beta 103.333(2) _cell_angle_gamma 90.00 _cell_volume 5080.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3652 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 21.94 _exptl_crystal_description plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.263 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2072 _exptl_absorpt_coefficient_mu 0.188 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9528 _exptl_absorpt_correction_T_max 0.9833 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17969 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0487 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8681 _reflns_number_gt 5074 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure was initially solved in the space group C2/c, with a 2-fold axis bisecting both the N1-N2 and N3B-N4B vectors. While the centrosymmetric model can not be discounted, it was dropped in favour of refinement in space group Cc (with racemic twinning) In C2/c the cation must lie on either a C2 axis or a centre of symmetry and neither of these is consistent with the point symmetry of the cation. The structure can be solved in C2/c (although refinement is problematic), however the C2 axis only appears to be present by virtue of the disorder. Hence, the lower symmetry space group seems a more realistic description. ; __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^)+(0.0489P)^2^+2.6841P] 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' _refine_ls_abs_structure_Flack 0.42(13) _refine_ls_number_reflns 8681 _refine_ls_number_parameters 922 _refine_ls_number_restraints 1834 _refine_ls_R_factor_all 0.0965 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1233 _refine_ls_wR_factor_gt 0.0969 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.45907(16) -0.3952(6) 0.7634(3) 0.0510(14) Uani 1 1 d U . . H1N H 0.4304 -0.3950 0.7324 0.050 Uiso 1 1 calc R . . C1A C 0.4871(2) -0.3427(8) 0.7082(4) 0.0625(19) Uani 1 1 d U . . H1A1 H 0.5166 -0.3224 0.7423 0.075 Uiso 1 1 calc R . . H1A2 H 0.4903 -0.4133 0.6682 0.075 Uiso 1 1 calc R . . C2A C 0.4692(2) -0.2212(8) 0.6623(4) 0.065(2) Uani 1 1 d U A . H2A1 H 0.4692 -0.1470 0.7017 0.078 Uiso 1 1 calc R . . H2A2 H 0.4881 -0.1948 0.6249 0.078 Uiso 1 1 calc R . . N3A N 0.42521(17) -0.2425(7) 0.6144(4) 0.0671(16) Uani 1 1 d U . . C3A C 0.4224(4) -0.2858(12) 0.5436(8) 0.050(3) Uani 0.50 1 d PDU A 1 H3A1 H 0.4367 -0.3747 0.5478 0.060 Uiso 0.50 1 calc PR A 1 H3A2 H 0.4391 -0.2254 0.5150 0.060 Uiso 0.50 1 calc PR A 1 C4A C 0.3768(3) -0.2996(10) 0.4909(6) 0.041(3) Uani 0.50 1 d PDU A 1 C5A C 0.3617(3) -0.2152(12) 0.4223(6) 0.052(3) Uani 0.50 1 d PDU A 1 H5A H 0.3805 -0.1476 0.4101 0.063 Uiso 0.50 1 calc PR A 1 C6A C 0.3204(3) -0.2281(12) 0.3726(7) 0.057(3) Uani 0.50 1 d PDU A 1 H6A H 0.3120 -0.1741 0.3246 0.068 Uiso 0.50 1 calc PR A 1 C7A C 0.2908(3) -0.3197(12) 0.3920(6) 0.051(3) Uani 0.50 1 d PDU A 1 C8A C 0.3042(3) -0.3900(12) 0.4647(6) 0.050(3) Uani 0.50 1 d PDU A 1 H8A H 0.2840 -0.4486 0.4812 0.060 Uiso 0.50 1 calc PR A 1 C9A C 0.3457(3) -0.3789(11) 0.5147(7) 0.045(3) Uani 0.50 1 d PDU A 1 H9A H 0.3529 -0.4258 0.5657 0.053 Uiso 0.50 1 calc PR A 1 C10A C 0.2480(4) -0.3420(19) 0.3305(10) 0.084(5) Uani 0.50 1 d PDU A 1 H10A H 0.2469 -0.2850 0.2814 0.101 Uiso 0.50 1 calc PR A 1 H10B H 0.2461 -0.4367 0.3123 0.101 Uiso 0.50 1 calc PR A 1 C13A C 0.4077(5) -0.0838(12) 0.6096(10) 0.073(4) Uani 0.50 1 d PDU A 1 H13A H 0.4090 -0.0507 0.6656 0.109 Uiso 0.50 1 calc PR A 1 H13B H 0.3774 -0.0796 0.5771 0.109 Uiso 0.50 1 calc PR A 1 H13C H 0.4263 -0.0282 0.5834 0.109 Uiso 0.50 1 calc PR A 1 C14A C 0.2164(5) -0.1546(15) 0.3948(10) 0.078(5) Uani 0.50 1 d PDU A 1 H14A H 0.1919 -0.1296 0.4191 0.117 Uiso 0.50 1 calc PR A 1 H14B H 0.2164 -0.0975 0.3469 0.117 Uiso 0.50 1 calc PR A 1 H14C H 0.2440 -0.1426 0.4360 0.117 Uiso 0.50 1 calc PR A 1 C3Z C 0.4041(4) -0.1339(14) 0.5714(8) 0.058(3) Uani 0.50 1 d PDU A 2 H3Z1 H 0.4218 -0.1039 0.5325 0.069 Uiso 0.50 1 calc PR A 2 H3Z2 H 0.4046 -0.0604 0.6115 0.069 Uiso 0.50 1 calc PR A 2 C4Z C 0.3578(3) -0.1495(14) 0.5229(6) 0.054(3) Uani 0.50 1 d PDU A 2 C5Z C 0.3481(3) -0.1249(16) 0.4370(7) 0.069(4) Uani 0.50 1 d PDU A 2 H5Z H 0.3710 -0.0991 0.4115 0.083 Uiso 0.50 1 calc PR A 2 C6Z C 0.3062(3) -0.1376(17) 0.3894(8) 0.074(4) Uani 0.50 1 d PDU A 2 H6Z H 0.3005 -0.1204 0.3317 0.088 Uiso 0.50 1 calc PR A 2 C7Z C 0.2725(3) -0.1752(14) 0.4254(6) 0.053(3) Uani 0.50 1 d PDU A 2 C8Z C 0.2815(3) -0.2053(12) 0.5079(6) 0.049(3) Uani 0.50 1 d PDU A 2 H8Z H 0.2585 -0.2325 0.5327 0.059 Uiso 0.50 1 calc PR A 2 C9Z C 0.3242(3) -0.1962(11) 0.5558(6) 0.045(3) Uani 0.50 1 d PDU A 2 H9Z H 0.3302 -0.2228 0.6121 0.054 Uiso 0.50 1 calc PR A 2 C10Z C 0.2274(4) -0.187(2) 0.3687(10) 0.084(4) Uani 0.50 1 d PDU A 2 H10C H 0.2072 -0.1255 0.3880 0.101 Uiso 0.50 1 calc PR A 2 H10D H 0.2289 -0.1596 0.3123 0.101 Uiso 0.50 1 calc PR A 2 C13Z C 0.4235(4) -0.3513(13) 0.5409(8) 0.046(3) Uani 0.50 1 d PDU A 2 H13D H 0.4373 -0.4349 0.5646 0.069 Uiso 0.50 1 calc PR A 2 H13E H 0.4393 -0.3160 0.5011 0.069 Uiso 0.50 1 calc PR A 2 H13F H 0.3930 -0.3687 0.5130 0.069 Uiso 0.50 1 calc PR A 2 C14Z C 0.2416(5) -0.4105(19) 0.3257(10) 0.080(5) Uani 0.50 1 d PDU A 2 H14D H 0.2302 -0.5020 0.3247 0.120 Uiso 0.50 1 calc PR A 2 H14E H 0.2717 -0.4081 0.3589 0.120 Uiso 0.50 1 calc PR A 2 H14F H 0.2411 -0.3817 0.2692 0.120 Uiso 0.50 1 calc PR A 2 N4A N 0.21139(17) -0.3108(8) 0.3658(3) 0.0685(17) Uani 1 1 d U . . C11A C 0.16935(19) -0.3264(9) 0.3080(4) 0.073(2) Uani 1 1 d U A . H11A H 0.1672 -0.4175 0.2840 0.088 Uiso 1 1 calc R . . H11B H 0.1670 -0.2612 0.2624 0.088 Uiso 1 1 calc R . . C12A C 0.1311(2) -0.3040(8) 0.3512(4) 0.0626(19) Uani 1 1 d U . . H12A H 0.1317 -0.2104 0.3710 0.075 Uiso 1 1 calc R A . H12B H 0.1030 -0.3181 0.3106 0.075 Uiso 1 1 calc R . . N2 N 0.13378(16) -0.3983(6) 0.4233(3) 0.0506(14) Uani 1 1 d U A . H2N H 0.1624 -0.3977 0.4549 0.050 Uiso 1 1 calc R . . C1B C 0.4702(2) -0.5394(7) 0.7899(4) 0.0594(18) Uani 1 1 d U . . H1B1 H 0.4561 -0.5623 0.8355 0.071 Uiso 1 1 calc R . . H1B2 H 0.5022 -0.5475 0.8111 0.071 Uiso 1 1 calc R . . C2B C 0.4553(2) -0.6390(8) 0.7195(5) 0.068(2) Uani 1 1 d U B . H2B1 H 0.4720 -0.6228 0.6766 0.081 Uiso 1 1 calc R . . H2B2 H 0.4621 -0.7310 0.7409 0.081 Uiso 1 1 calc R . . N3B N 0.40877(18) -0.6293(6) 0.6820(4) 0.0687(18) Uani 1 1 d U . . C3B C 0.3869(3) -0.7116(13) 0.7198(8) 0.055(3) Uani 0.50 1 d PDU B 1 H3B1 H 0.3919 -0.6874 0.7789 0.066 Uiso 0.50 1 calc PR B 1 H3B2 H 0.3972 -0.8046 0.7160 0.066 Uiso 0.50 1 calc PR B 1 C4B C 0.3388(3) -0.7021(9) 0.6795(7) 0.042(3) Uani 0.50 1 d PDU B 1 C5B C 0.3148(3) -0.5849(11) 0.6706(7) 0.047(3) Uani 0.50 1 d PDU B 1 H5B H 0.3287 -0.5033 0.6912 0.056 Uiso 0.50 1 calc PR B 1 C6B C 0.2707(3) -0.5849(10) 0.6321(8) 0.053(3) Uani 0.50 1 d PDU B 1 H6B H 0.2554 -0.5022 0.6227 0.064 Uiso 0.50 1 calc PR B 1 C7B C 0.2484(3) -0.7032(10) 0.6069(8) 0.054(3) Uani 0.50 1 d PDU B 1 C8B C 0.2722(3) -0.8211(10) 0.6196(8) 0.058(3) Uani 0.50 1 d PDU B 1 H8B H 0.2577 -0.9043 0.6056 0.070 Uiso 0.50 1 calc PR B 1 C9B C 0.3168(3) -0.8193(11) 0.6527(9) 0.060(4) Uani 0.50 1 d PDU B 1 H9B H 0.3327 -0.9008 0.6570 0.072 Uiso 0.50 1 calc PR B 1 C10B C 0.1997(4) -0.7052(15) 0.5705(10) 0.075(4) Uani 0.50 1 d PDU B 1 H10C' H 0.1917 -0.7988 0.5542 0.090 Uiso 0.50 1 calc PR B 1 H10D' H 0.1852 -0.6830 0.6158 0.090 Uiso 0.50 1 calc PR B 1 C13B C 0.4096(4) -0.6958(18) 0.5942(7) 0.067(4) Uani 0.50 1 d PDU B 1 H13G H 0.4248 -0.6360 0.5635 0.100 Uiso 0.50 1 calc PR B 1 H13H H 0.3795 -0.7100 0.5625 0.100 Uiso 0.50 1 calc PR B 1 H13I H 0.4249 -0.7819 0.6033 0.100 Uiso 0.50 1 calc PR B 1 C14B C 0.2077(5) -0.6783(19) 0.4278(9) 0.088(5) Uani 0.50 1 d PDU B 1 H14G H 0.1955 -0.6284 0.3769 0.132 Uiso 0.50 1 calc PR B 1 H14H H 0.2030 -0.7744 0.4174 0.132 Uiso 0.50 1 calc PR B 1 H14I H 0.2391 -0.6602 0.4457 0.132 Uiso 0.50 1 calc PR B 1 C3Y C 0.3922(4) -0.7052(16) 0.6107(10) 0.068(4) Uani 0.50 1 d PDU B 2 H3Y1 H 0.4021 -0.7990 0.6216 0.081 Uiso 0.50 1 calc PR B 2 H3Y2 H 0.4050 -0.6710 0.5656 0.081 Uiso 0.50 1 calc PR B 2 C4Y C 0.3430(3) -0.7047(10) 0.5814(9) 0.056(3) Uani 0.50 1 d PDU B 2 C5Y C 0.3225(3) -0.5825(10) 0.5565(8) 0.050(3) Uani 0.50 1 d PDU B 2 H5Y H 0.3386 -0.5012 0.5642 0.060 Uiso 0.50 1 calc PR B 2 C6Y C 0.2787(3) -0.5829(10) 0.5209(7) 0.044(3) Uani 0.50 1 d PDU B 2 H6Y H 0.2645 -0.5001 0.5042 0.053 Uiso 0.50 1 calc PR B 2 C7Y C 0.2539(3) -0.7007(10) 0.5083(8) 0.051(3) Uani 0.50 1 d PDU B 2 C8Y C 0.2749(3) -0.8183(11) 0.5339(9) 0.060(4) Uani 0.50 1 d PDU B 2 H8Y H 0.2591 -0.9001 0.5246 0.072 Uiso 0.50 1 calc PR B 2 C9Y C 0.3190(3) -0.8205(12) 0.5732(11) 0.073(4) Uani 0.50 1 d PDU B 2 H9Y H 0.3325 -0.9022 0.5944 0.087 Uiso 0.50 1 calc PR B 2 C10Y C 0.2062(4) -0.6910(17) 0.4665(7) 0.055(3) Uani 0.50 1 d PDU B 2 H10E H 0.2037 -0.6464 0.4124 0.066 Uiso 0.50 1 calc PR B 2 H10F H 0.1947 -0.7830 0.4552 0.066 Uiso 0.50 1 calc PR B 2 C13Y C 0.3833(5) -0.6768(16) 0.7461(9) 0.064(4) Uani 0.50 1 d PDU B 2 H13J H 0.3924 -0.6240 0.7968 0.096 Uiso 0.50 1 calc PR B 2 H13K H 0.3895 -0.7717 0.7586 0.096 Uiso 0.50 1 calc PR B 2 H13L H 0.3519 -0.6648 0.7234 0.096 Uiso 0.50 1 calc PR B 2 C14Y C 0.1824(5) -0.6841(14) 0.5959(8) 0.051(3) Uani 0.50 1 d PDU B 2 H14J H 0.2125 -0.6833 0.6290 0.076 Uiso 0.50 1 calc PR B 2 H14K H 0.1712 -0.7760 0.5916 0.076 Uiso 0.50 1 calc PR B 2 H14L H 0.1641 -0.6277 0.6225 0.076 Uiso 0.50 1 calc PR B 2 N4B N 0.18129(19) -0.6276(6) 0.5060(4) 0.0689(18) Uani 1 1 d U . . C11B C 0.1344(2) -0.6326(8) 0.4664(5) 0.0626(19) Uani 1 1 d U A . H11C H 0.1266 -0.7245 0.4460 0.075 Uiso 1 1 calc R . . H11D H 0.1174 -0.6117 0.5081 0.075 Uiso 1 1 calc R . . C12B C 0.1221(2) -0.5381(7) 0.3971(4) 0.0617(19) Uani 1 1 d U . . H12C H 0.0902 -0.5439 0.3738 0.074 Uiso 1 1 calc R A . H12D H 0.1371 -0.5636 0.3532 0.074 Uiso 1 1 calc R . . C1C C 0.4604(2) -0.3070(8) 0.8365(4) 0.0612(19) Uani 1 1 d U . . H1C1 H 0.4883 -0.3219 0.8776 0.073 Uiso 1 1 calc R . . H1C2 H 0.4596 -0.2122 0.8187 0.073 Uiso 1 1 calc R . . C2C C 0.4240(2) -0.3322(7) 0.8751(4) 0.0595(17) Uani 1 1 d U C . H2C1 H 0.4262 -0.2705 0.9225 0.071 Uiso 1 1 calc R . . H2C2 H 0.4262 -0.4249 0.8968 0.071 Uiso 1 1 calc R . . N3C N 0.38102(19) -0.3140(8) 0.8173(4) 0.0708(18) Uani 1 1 d U . . C3C C 0.3666(4) -0.1931(15) 0.8100(9) 0.059(3) Uani 0.50 1 d PDU C 1 H3C1 H 0.3860 -0.1387 0.7839 0.071 Uiso 0.50 1 calc PR C 1 H3C2 H 0.3684 -0.1563 0.8659 0.071 Uiso 0.50 1 calc PR C 1 C4C C 0.3203(3) -0.1767(16) 0.7603(7) 0.062(3) Uani 0.50 1 d PDU C 1 C5C C 0.3099(3) -0.2102(12) 0.6763(6) 0.049(3) Uani 0.50 1 d PDU C 1 H5C H 0.3320 -0.2448 0.6515 0.058 Uiso 0.50 1 calc PR C 1 C6C C 0.2686(3) -0.1938(13) 0.6297(7) 0.054(3) Uani 0.50 1 d PDU C 1 H6C H 0.2628 -0.2109 0.5720 0.065 Uiso 0.50 1 calc PR C 1 C7C C 0.2342(3) -0.1523(13) 0.6647(6) 0.050(3) Uani 0.50 1 d PDU C 1 C8C C 0.2435(4) -0.1183(17) 0.7466(7) 0.072(4) Uani 0.50 1 d PDU C 1 H8C H 0.2212 -0.0856 0.7713 0.086 Uiso 0.50 1 calc PR C 1 C9C C 0.2865(4) -0.1324(18) 0.7936(8) 0.075(4) Uani 0.50 1 d PDU C 1 H9C H 0.2925 -0.1104 0.8507 0.090 Uiso 0.50 1 calc PR C 1 C10C C 0.1885(4) -0.1326(14) 0.6109(9) 0.057(3) Uani 0.50 1 d PDU C 1 H10E' H 0.1700 -0.0981 0.6470 0.068 Uiso 0.50 1 calc PR C 1 H10F' H 0.1903 -0.0608 0.5708 0.068 Uiso 0.50 1 calc PR C 1 C13C C 0.3488(5) -0.4069(14) 0.8576(10) 0.059(4) Uani 0.50 1 d PDU C 1 H13M H 0.3597 -0.4992 0.8625 0.089 Uiso 0.50 1 calc PR C 1 H13N H 0.3193 -0.4050 0.8220 0.089 Uiso 0.50 1 calc PR C 1 H13O H 0.3481 -0.3726 0.9124 0.089 Uiso 0.50 1 calc PR C 1 C14C C 0.1640(5) -0.3539(17) 0.6448(11) 0.070(5) Uani 0.50 1 d PDU C 1 H14M H 0.1934 -0.3720 0.6786 0.105 Uiso 0.50 1 calc PR C 1 H14N H 0.1514 -0.4369 0.6181 0.105 Uiso 0.50 1 calc PR C 1 H14O H 0.1455 -0.3193 0.6800 0.105 Uiso 0.50 1 calc PR C 1 C3X C 0.3452(4) -0.3305(14) 0.8478(7) 0.058(3) Uani 0.50 1 d PDU C 2 H3X1 H 0.3473 -0.2655 0.8935 0.069 Uiso 0.50 1 calc PR C 2 H3X2 H 0.3470 -0.4209 0.8726 0.069 Uiso 0.50 1 calc PR C 2 C4X C 0.3003(3) -0.3164(13) 0.7919(6) 0.052(3) Uani 0.50 1 d PDU C 2 C5X C 0.2887(3) -0.3947(12) 0.7194(6) 0.050(3) Uani 0.50 1 d PDU C 2 H5X H 0.3094 -0.4521 0.7034 0.060 Uiso 0.50 1 calc PR C 2 C6X C 0.2463(3) -0.3855(11) 0.6726(6) 0.044(3) Uani 0.50 1 d PDU C 2 H6X H 0.2376 -0.4417 0.6255 0.053 Uiso 0.50 1 calc PR C 2 C7X C 0.2158(3) -0.2969(12) 0.6919(6) 0.046(3) Uani 0.50 1 d PDU C 2 C8X C 0.2266(4) -0.2272(13) 0.7650(7) 0.055(3) Uani 0.50 1 d PDU C 2 H8X H 0.2053 -0.1741 0.7825 0.066 Uiso 0.50 1 calc PR C 2 C9X C 0.2695(4) -0.2356(15) 0.8136(8) 0.066(4) Uani 0.50 1 d PDU C 2 H9X H 0.2774 -0.1839 0.8627 0.079 Uiso 0.50 1 calc PR C 2 C10X C 0.1695(4) -0.2931(15) 0.6398(9) 0.053(3) Uani 0.50 1 d PDU C 2 H10G H 0.1582 -0.3857 0.6302 0.063 Uiso 0.50 1 calc PR C 2 H10H H 0.1507 -0.2445 0.6703 0.063 Uiso 0.50 1 calc PR C 2 C13X C 0.3798(5) -0.1518(15) 0.7953(10) 0.066(4) Uani 0.50 1 d PDU C 2 H13P H 0.4048 -0.1292 0.7718 0.099 Uiso 0.50 1 calc PR C 2 H13Q H 0.3814 -0.0999 0.8460 0.099 Uiso 0.50 1 calc PR C 2 H13R H 0.3525 -0.1306 0.7553 0.099 Uiso 0.50 1 calc PR C 2 C14X C 0.1829(5) -0.0793(12) 0.5812(8) 0.061(4) Uani 0.50 1 d PDU C 2 H14P H 0.2136 -0.0756 0.6114 0.092 Uiso 0.50 1 calc PR C 2 H14Q H 0.1647 -0.0322 0.6128 0.092 Uiso 0.50 1 calc PR C 2 H14R H 0.1797 -0.0364 0.5272 0.092 Uiso 0.50 1 calc PR C 2 N4C N 0.16737(19) -0.2342(7) 0.5685(4) 0.0712(18) Uani 1 1 d U . . C11C C 0.1219(2) -0.2219(8) 0.5238(5) 0.063(2) Uani 1 1 d U A . H11E H 0.1192 -0.1462 0.4845 0.075 Uiso 1 1 calc R . . H11F H 0.1038 -0.2007 0.5636 0.075 Uiso 1 1 calc R . . C12C C 0.10407(19) -0.3482(8) 0.4763(4) 0.0541(18) Uani 1 1 d U . . H12E H 0.1006 -0.4191 0.5160 0.065 Uiso 1 1 calc R A . H12F H 0.0748 -0.3292 0.4407 0.065 Uiso 1 1 calc R . . Cl1 Cl 0.10182(4) 0.05812(18) 0.29169(8) 0.0610(5) Uani 0.50 1 d PDU D 1 O11 O 0.08160(13) 0.0017(6) 0.3507(3) 0.1026(17) Uani 0.50 1 d PDU D 1 O12 O 0.1258(4) 0.1749(11) 0.2982(6) 0.139(4) Uani 0.50 1 d PDU D 1 O13 O 0.0641(3) 0.0806(11) 0.2240(5) 0.101(3) Uani 0.50 1 d PDU D 1 O14 O 0.1289(3) -0.0230(11) 0.2524(5) 0.106(3) Uani 0.50 1 d PDU D 1 Cl1' Cl 0.10182(4) 0.05812(18) 0.29169(8) 0.0610(5) Uani 0.50 1 d PDU E 2 O11' O 0.08160(13) 0.0017(6) 0.3507(3) 0.1026(17) Uani 0.50 1 d PDU E 2 O12' O 0.0901(5) 0.1906(9) 0.2849(8) 0.136(5) Uani 0.50 1 d PDU E 2 O13' O 0.0936(4) -0.0327(12) 0.2300(6) 0.133(5) Uani 0.50 1 d PDU E 2 O14' O 0.1449(2) 0.0463(9) 0.3453(8) 0.120(4) Uani 0.50 1 d PDU E 2 Cl2 Cl 0.49049(4) 0.05949(18) 0.89509(8) 0.0573(5) Uani 0.50 1 d PDU F 1 O21 O 0.5009(2) 0.0070(6) 0.8260(3) 0.138(2) Uani 0.50 1 d PDU F 1 O22 O 0.5269(3) 0.0422(12) 0.9617(6) 0.125(4) Uani 0.50 1 d PDU F 1 O23 O 0.4542(3) -0.0009(11) 0.9143(9) 0.140(5) Uani 0.50 1 d PDU F 1 O24 O 0.4845(3) 0.2041(7) 0.8948(6) 0.073(3) Uani 0.50 1 d PDU F 1 Cl2' Cl 0.49049(4) 0.05949(18) 0.89509(8) 0.0573(5) Uani 0.50 1 d PDU G 2 O21' O 0.5009(2) 0.0070(6) 0.8260(3) 0.138(2) Uani 0.50 1 d PDU G 2 O22' O 0.4901(4) -0.0377(10) 0.9554(5) 0.086(3) Uani 0.50 1 d PDU G 2 O23' O 0.4493(3) 0.0928(14) 0.8581(10) 0.174(6) Uani 0.50 1 d PDU G 2 O24' O 0.5189(4) 0.1647(12) 0.9249(10) 0.149(5) Uani 0.50 1 d PDU G 2 C1S C 0.5655(2) -0.3827(7) 0.5406(5) 0.064(2) Uani 1 1 d U . . H1S1 H 0.5772 -0.3822 0.4909 0.095 Uiso 1 1 calc R . . H1S2 H 0.5892 -0.3998 0.5892 0.095 Uiso 1 1 calc R . . H1S3 H 0.5521 -0.2957 0.5465 0.095 Uiso 1 1 calc R . . C2S C 0.5331(2) -0.4857(9) 0.5335(4) 0.062(2) Uani 1 1 d U . . N1S N 0.5080(2) -0.5676(8) 0.5241(4) 0.082(2) Uani 1 1 d U . . C3S C 0.0261(3) -0.3777(8) 0.6460(5) 0.078(3) Uani 1 1 d U . . H3S1 H 0.0390 -0.2983 0.6769 0.117 Uiso 1 1 calc R . . H3S2 H 0.0017 -0.4100 0.6680 0.117 Uiso 1 1 calc R . . H3S3 H 0.0156 -0.3545 0.5875 0.117 Uiso 1 1 calc R . . C4S C 0.0594(2) -0.4830(8) 0.6542(4) 0.059(2) Uani 1 1 d U . . N2S N 0.0853(2) -0.5634(8) 0.6563(5) 0.087(2) Uani 1 1 d U . . 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 N1 0.039(3) 0.066(3) 0.045(3) 0.003(2) 0.006(2) -0.004(3) C1A 0.045(3) 0.080(5) 0.061(4) 0.000(3) 0.010(3) -0.022(3) C2A 0.060(4) 0.077(5) 0.061(4) 0.008(3) 0.022(3) -0.015(3) N3A 0.045(3) 0.100(4) 0.059(3) 0.030(3) 0.017(2) -0.001(3) C3A 0.048(6) 0.037(6) 0.069(6) 0.010(5) 0.021(5) -0.004(5) C4A 0.046(5) 0.039(6) 0.042(5) -0.005(4) 0.020(4) -0.001(4) C5A 0.072(6) 0.048(7) 0.043(6) 0.011(5) 0.026(5) 0.005(5) C6A 0.067(6) 0.056(7) 0.051(7) 0.003(5) 0.022(5) 0.015(5) C7A 0.045(4) 0.066(7) 0.046(6) -0.007(5) 0.021(4) 0.021(5) C8A 0.037(5) 0.065(8) 0.056(6) 0.004(5) 0.025(4) -0.001(5) C9A 0.053(5) 0.037(6) 0.046(6) 0.006(5) 0.016(5) 0.000(5) C10A 0.043(5) 0.137(13) 0.075(8) 0.018(9) 0.020(5) 0.015(7) C13A 0.098(8) 0.036(6) 0.108(10) 0.023(6) 0.072(8) 0.008(6) C14A 0.082(10) 0.076(7) 0.073(9) 0.042(6) 0.013(7) -0.001(7) C3Z 0.058(5) 0.056(7) 0.066(8) 0.002(6) 0.028(5) -0.005(6) C4Z 0.052(5) 0.054(8) 0.060(6) 0.008(6) 0.019(4) -0.006(6) C5Z 0.052(5) 0.092(10) 0.068(6) 0.037(8) 0.023(5) -0.015(7) C6Z 0.052(5) 0.098(10) 0.074(7) 0.046(8) 0.018(5) 0.004(7) C7Z 0.047(5) 0.058(7) 0.056(6) 0.016(6) 0.013(4) 0.008(5) C8Z 0.051(5) 0.048(7) 0.053(5) 0.006(6) 0.023(5) 0.010(6) C9Z 0.059(5) 0.032(6) 0.047(6) 0.003(5) 0.020(4) 0.005(5) C10Z 0.051(6) 0.132(9) 0.066(8) 0.015(8) 0.011(6) -0.007(7) C13Z 0.049(7) 0.055(8) 0.037(6) 0.007(5) 0.013(5) 0.001(6) C14Z 0.041(7) 0.161(13) 0.042(8) 0.022(9) 0.021(6) 0.035(8) N4A 0.042(3) 0.116(4) 0.047(3) 0.023(3) 0.010(2) 0.007(3) C11A 0.040(3) 0.133(6) 0.047(4) 0.008(4) 0.011(3) 0.018(3) C12A 0.051(3) 0.092(5) 0.047(4) 0.009(3) 0.017(3) 0.024(4) N2 0.037(3) 0.067(3) 0.045(3) -0.001(3) 0.004(2) 0.013(3) C1B 0.048(4) 0.075(4) 0.053(4) 0.016(3) 0.008(3) 0.011(3) C2B 0.057(3) 0.060(4) 0.078(5) 0.011(3) -0.001(3) 0.008(3) N3B 0.055(3) 0.048(3) 0.086(4) 0.007(3) -0.018(3) 0.004(3) C3B 0.048(5) 0.043(7) 0.075(8) -0.021(5) 0.016(5) 0.004(4) C4B 0.049(5) 0.041(5) 0.037(6) 0.008(5) 0.010(5) -0.003(4) C5B 0.053(5) 0.055(6) 0.034(6) -0.005(5) 0.015(5) -0.013(5) C6B 0.059(6) 0.034(5) 0.065(8) 0.007(6) 0.012(6) 0.001(5) C7B 0.048(5) 0.048(6) 0.068(7) -0.011(6) 0.014(5) -0.006(4) C8B 0.063(6) 0.033(5) 0.073(8) -0.006(6) 0.002(6) -0.007(5) C9B 0.055(6) 0.050(6) 0.069(8) -0.006(7) 0.000(6) 0.002(5) C10B 0.053(6) 0.048(8) 0.115(8) 0.008(7) 0.001(6) -0.003(6) C13B 0.050(8) 0.106(11) 0.035(5) 0.018(6) -0.012(5) -0.007(8) C14B 0.055(7) 0.111(11) 0.083(8) -0.063(9) -0.013(6) 0.031(7) C3Y 0.049(6) 0.046(8) 0.104(9) -0.023(7) 0.009(6) 0.013(6) C4Y 0.047(5) 0.043(6) 0.076(8) -0.012(6) 0.009(6) 0.008(4) C5Y 0.041(5) 0.044(6) 0.070(8) -0.006(6) 0.026(6) 0.000(5) C6Y 0.048(5) 0.038(5) 0.048(6) -0.010(5) 0.019(5) 0.012(4) C7Y 0.040(5) 0.044(6) 0.073(8) -0.005(6) 0.022(5) -0.004(4) C8Y 0.053(5) 0.044(6) 0.089(10) -0.011(7) 0.028(6) -0.001(5) C9Y 0.056(6) 0.041(6) 0.121(12) 0.000(8) 0.020(7) 0.008(5) C10Y 0.058(5) 0.067(9) 0.035(6) -0.024(7) -0.003(5) -0.015(5) C13Y 0.064(7) 0.036(8) 0.084(9) 0.003(7) 0.001(7) 0.017(6) C14Y 0.062(8) 0.036(6) 0.058(6) 0.004(5) 0.022(5) 0.012(6) N4B 0.065(3) 0.061(4) 0.070(4) -0.009(3) -0.007(3) 0.003(3) C11B 0.053(3) 0.063(4) 0.069(4) -0.011(4) 0.007(3) -0.006(3) C12B 0.038(4) 0.070(4) 0.066(4) -0.018(3) -0.010(3) 0.012(3) C1C 0.056(4) 0.075(5) 0.044(4) -0.004(3) -0.006(3) -0.013(4) C2C 0.067(4) 0.063(4) 0.046(4) -0.012(3) 0.006(3) -0.019(3) N3C 0.052(3) 0.099(4) 0.059(4) -0.022(3) 0.008(3) -0.011(3) C3C 0.056(6) 0.072(7) 0.051(7) -0.032(6) 0.018(5) -0.027(5) C4C 0.063(6) 0.060(8) 0.062(6) -0.026(7) 0.012(5) -0.005(6) C5C 0.054(6) 0.033(7) 0.060(6) -0.001(6) 0.016(5) 0.011(6) C6C 0.064(6) 0.050(8) 0.050(7) -0.006(6) 0.017(5) 0.013(6) C7C 0.048(5) 0.039(7) 0.064(6) -0.008(6) 0.016(4) 0.006(5) C8C 0.070(6) 0.086(10) 0.062(6) -0.023(7) 0.020(5) 0.007(8) C9C 0.077(7) 0.093(11) 0.053(7) -0.024(8) 0.011(5) 0.021(8) C10C 0.057(6) 0.053(8) 0.065(9) -0.001(6) 0.021(5) 0.018(6) C13C 0.057(7) 0.075(9) 0.048(8) -0.012(7) 0.018(6) -0.010(7) C14C 0.039(7) 0.097(11) 0.067(9) 0.022(8) -0.003(6) -0.012(7) C3X 0.078(5) 0.069(8) 0.022(5) 0.005(6) 0.002(4) -0.028(6) C4X 0.059(5) 0.067(8) 0.031(5) 0.001(5) 0.010(5) -0.020(6) C5X 0.061(6) 0.056(7) 0.028(5) 0.000(5) 0.002(5) -0.012(6) C6X 0.054(5) 0.050(7) 0.030(6) 0.004(5) 0.015(4) -0.009(5) C7X 0.052(5) 0.057(7) 0.033(5) -0.003(5) 0.022(4) -0.019(5) C8X 0.065(6) 0.051(7) 0.054(6) -0.011(5) 0.024(5) -0.016(5) C9X 0.076(6) 0.083(9) 0.038(6) -0.026(6) 0.014(5) -0.025(6) C10X 0.045(6) 0.053(8) 0.067(7) -0.013(6) 0.028(5) -0.016(6) C13X 0.050(7) 0.083(8) 0.063(9) 0.013(7) 0.007(6) -0.020(6) C14X 0.078(8) 0.043(7) 0.052(7) 0.017(6) -0.004(6) -0.002(6) N4C 0.054(3) 0.093(4) 0.068(4) -0.023(3) 0.017(3) -0.002(3) C11C 0.053(4) 0.074(5) 0.064(4) -0.007(4) 0.019(3) 0.015(3) C12C 0.036(3) 0.073(4) 0.054(4) -0.007(3) 0.012(3) 0.006(3) Cl1 0.0549(10) 0.0601(11) 0.0659(11) -0.0031(9) 0.0096(8) -0.0005(9) O11 0.072(2) 0.149(4) 0.094(3) 0.043(3) 0.034(2) 0.031(3) O12 0.195(10) 0.158(8) 0.074(6) -0.043(6) 0.053(6) -0.135(7) O13 0.051(4) 0.152(9) 0.087(6) 0.066(6) -0.006(4) 0.010(5) O14 0.126(7) 0.139(8) 0.067(5) 0.034(5) 0.051(5) 0.080(7) Cl1' 0.0549(10) 0.0601(11) 0.0659(11) -0.0031(9) 0.0096(8) -0.0005(9) O11' 0.072(2) 0.149(4) 0.094(3) 0.043(3) 0.034(2) 0.031(3) O12' 0.184(12) 0.057(5) 0.130(9) 0.032(5) -0.042(8) 0.061(6) O13' 0.150(10) 0.155(9) 0.075(6) -0.059(7) -0.012(6) -0.007(9) O14' 0.055(4) 0.053(5) 0.214(10) -0.021(6) -0.048(5) -0.003(4) Cl2 0.0505(10) 0.0625(12) 0.0582(10) -0.0002(9) 0.0112(8) 0.0023(9) O21 0.266(6) 0.097(4) 0.086(3) -0.047(3) 0.116(4) -0.079(4) O22 0.091(6) 0.121(8) 0.130(7) 0.061(6) -0.039(6) 0.029(6) O23 0.074(5) 0.096(7) 0.293(13) -0.073(8) 0.132(7) -0.039(5) O24 0.108(7) 0.038(4) 0.069(5) 0.004(4) 0.011(5) -0.003(4) Cl2' 0.0505(10) 0.0625(12) 0.0582(10) -0.0002(9) 0.0112(8) 0.0023(9) O21' 0.266(6) 0.097(4) 0.086(3) -0.047(3) 0.116(4) -0.079(4) O22' 0.107(7) 0.112(7) 0.054(5) 0.027(5) 0.047(5) 0.045(6) O23' 0.034(4) 0.175(12) 0.298(16) 0.142(10) 0.010(6) 0.032(5) O24' 0.129(9) 0.120(9) 0.190(14) -0.060(8) 0.019(9) -0.059(8) C1S 0.053(4) 0.060(5) 0.081(5) 0.002(4) 0.022(4) 0.000(3) C2S 0.050(4) 0.074(5) 0.060(4) 0.001(4) 0.011(3) 0.012(3) N1S 0.084(4) 0.102(5) 0.056(3) -0.010(3) 0.011(3) -0.025(4) C3S 0.081(5) 0.063(5) 0.087(6) -0.004(5) 0.014(5) 0.015(4) C4S 0.057(4) 0.068(5) 0.054(4) 0.007(4) 0.016(3) 0.001(4) N2S 0.061(4) 0.092(5) 0.113(5) 0.011(4) 0.031(4) 0.014(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1C 1.494(9) . ? N1 C1A 1.507(8) . ? N1 C1B 1.523(9) . ? C1A C2A 1.475(10) . ? C2A N3A 1.443(8) . ? N3A C3A 1.238(14) . ? N3A C3Z 1.381(14) . ? N3A C13Z 1.627(14) . ? N3A C13A 1.674(13) . ? C3A C4A 1.505(11) . ? C4A C9A 1.385(10) . ? C4A C5A 1.410(11) . ? C5A C6A 1.373(11) . ? C6A C7A 1.395(11) . ? C7A C8A 1.378(11) . ? C7A C10A 1.505(12) . ? C8A C9A 1.380(10) . ? C10A N4A 1.443(17) . ? C14A N4A 1.630(17) . ? C3Z C4Z 1.502(12) . ? C4Z C9Z 1.376(11) . ? C4Z C5Z 1.413(11) . ? C5Z C6Z 1.376(11) . ? C6Z C7Z 1.385(11) . ? C7Z C8Z 1.369(11) . ? C7Z C10Z 1.516(12) . ? C8Z C9Z 1.397(10) . ? C10Z N4A 1.328(19) . ? C14Z N4A 1.622(17) . ? N4A C11A 1.452(8) . ? C11A C12A 1.552(9) . ? C12A N2 1.513(9) . ? N2 C12B 1.484(9) . ? N2 C12C 1.509(8) . ? C1B C2B 1.525(10) . ? C2B N3B 1.455(8) . ? N3B C3B 1.321(15) . ? N3B C3Y 1.402(15) . ? N3B C13Y 1.547(17) . ? N3B C13B 1.609(15) . ? C3B C4B 1.507(12) . ? C4B C9B 1.381(11) . ? C4B C5B 1.383(11) . ? C5B C6B 1.386(10) . ? C6B C7B 1.389(11) . ? C7B C8B 1.385(11) . ? C7B C10B 1.511(12) . ? C8B C9B 1.384(10) . ? C10B N4B 1.341(15) . ? C14B N4B 1.770(15) . ? C3Y C4Y 1.512(12) . ? C4Y C9Y 1.371(11) . ? C4Y C5Y 1.397(11) . ? C5Y C6Y 1.368(10) . ? C6Y C7Y 1.400(11) . ? C7Y C8Y 1.368(11) . ? C7Y C10Y 1.502(12) . ? C8Y C9Y 1.388(10) . ? C10Y N4B 1.297(14) . ? C14Y N4B 1.591(14) . ? N4B C11B 1.471(8) . ? C11B C12B 1.470(10) . ? C1C C2C 1.458(10) . ? C2C N3C 1.478(8) . ? N3C C3C 1.286(16) . ? N3C C3X 1.346(14) . ? N3C C13C 1.627(16) . ? N3C C13X 1.659(16) . ? C3C C4C 1.506(12) . ? C4C C9C 1.380(12) . ? C4C C5C 1.400(11) . ? C5C C6C 1.361(11) . ? C6C C7C 1.402(11) . ? C7C C8C 1.368(11) . ? C7C C10C 1.519(12) . ? C8C C9C 1.402(12) . ? C10C N4C 1.323(15) . ? C14C N4C 1.764(17) . ? C3X C4X 1.507(12) . ? C4X C9X 1.372(12) . ? C4X C5X 1.412(11) . ? C5X C6X 1.383(11) . ? C6X C7X 1.394(11) . ? C7X C8X 1.375(11) . ? C7X C10X 1.513(12) . ? C8X C9X 1.406(11) . ? C10X N4C 1.312(15) . ? C14X N4C 1.621(14) . ? N4C C11C 1.458(8) . ? C11C C12C 1.525(10) . ? Cl1 O12 1.379(8) . ? Cl1 O11 1.404(4) . ? Cl1 O14 1.436(8) . ? Cl1 O13 1.451(7) . ? Cl2 O21 1.369(4) . ? Cl2 O23 1.390(7) . ? Cl2 O22 1.407(7) . ? Cl2 O24 1.457(7) . ? C1S C2S 1.432(10) . ? C2S N1S 1.123(9) . ? C3S C4S 1.467(11) . ? C4S N2S 1.139(9) . ? 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 C1C N1 C1A 112.3(5) . . ? C1C N1 C1B 111.2(5) . . ? C1A N1 C1B 112.2(5) . . ? C2A C1A N1 113.2(6) . . ? N3A C2A C1A 111.6(6) . . ? C3A N3A C3Z 82.1(9) . . ? C3A N3A C2A 115.1(7) . . ? C3Z N3A C2A 117.0(7) . . ? C3A N3A C13Z 21.5(7) . . ? C3Z N3A C13Z 102.0(8) . . ? C2A N3A C13Z 111.9(7) . . ? C3A N3A C13A 109.6(9) . . ? C3Z N3A C13A 28.2(7) . . ? C2A N3A C13A 98.6(7) . . ? C13Z N3A C13A 130.1(8) . . ? N3A C3A C4A 115.8(11) . . ? C9A C4A C5A 116.4(8) . . ? C9A C4A C3A 121.8(9) . . ? C5A C4A C3A 121.0(9) . . ? C6A C5A C4A 121.7(10) . . ? C5A C6A C7A 120.7(10) . . ? C8A C7A C6A 116.8(9) . . ? C8A C7A C10A 124.4(10) . . ? C6A C7A C10A 118.6(10) . . ? C7A C8A C9A 122.9(9) . . ? C8A C9A C4A 120.3(9) . . ? N4A C10A C7A 111.2(11) . . ? N3A C3Z C4Z 119.1(11) . . ? C9Z C4Z C5Z 117.1(9) . . ? C9Z C4Z C3Z 124.0(9) . . ? C5Z C4Z C3Z 118.7(9) . . ? C6Z C5Z C4Z 121.3(10) . . ? C5Z C6Z C7Z 120.1(10) . . ? C8Z C7Z C6Z 119.5(9) . . ? C8Z C7Z C10Z 123.6(10) . . ? C6Z C7Z C10Z 116.9(10) . . ? C7Z C8Z C9Z 120.4(9) . . ? C4Z C9Z C8Z 121.3(9) . . ? N4A C10Z C7Z 112.9(13) . . ? C10Z N4A C10A 83.3(11) . . ? C10Z N4A C11A 113.8(8) . . ? C10A N4A C11A 113.4(7) . . ? C10Z N4A C14Z 109.4(10) . . ? C10A N4A C14Z 26.1(10) . . ? C11A N4A C14Z 101.0(7) . . ? C10Z N4A C14A 24.6(10) . . ? C10A N4A C14A 107.2(10) . . ? C11A N4A C14A 108.1(7) . . ? C14Z N4A C14A 133.1(10) . . ? N4A C11A C12A 111.3(6) . . ? N2 C12A C11A 111.7(5) . . ? C12B N2 C12C 109.8(5) . . ? C12B N2 C12A 112.8(5) . . ? C12C N2 C12A 109.1(5) . . ? N1 C1B C2B 112.7(5) . . ? N3B C2B C1B 112.6(6) . . ? C3B N3B C3Y 86.1(9) . . ? C3B N3B C2B 109.7(7) . . ? C3Y N3B C2B 117.8(7) . . ? C3B N3B C13Y 21.9(8) . . ? C3Y N3B C13Y 105.4(9) . . ? C2B N3B C13Y 108.2(7) . . ? C3B N3B C13B 107.1(8) . . ? C3Y N3B C13B 24.5(7) . . ? C2B N3B C13B 97.8(7) . . ? C13Y N3B C13B 128.1(9) . . ? N3B C3B C4B 109.1(10) . . ? C9B C4B C5B 117.5(8) . . ? C9B C4B C3B 117.8(9) . . ? C5B C4B C3B 124.6(9) . . ? C4B C5B C6B 120.8(9) . . ? C5B C6B C7B 121.5(9) . . ? C8B C7B C6B 117.4(9) . . ? C8B C7B C10B 120.8(9) . . ? C6B C7B C10B 121.8(9) . . ? C9B C8B C7B 120.8(10) . . ? C4B C9B C8B 121.8(10) . . ? N4B C10B C7B 121.5(12) . . ? N3B C3Y C4Y 115.0(10) . . ? C9Y C4Y C5Y 120.1(9) . . ? C9Y C4Y C3Y 121.9(10) . . ? C5Y C4Y C3Y 117.8(10) . . ? C6Y C5Y C4Y 118.3(9) . . ? C5Y C6Y C7Y 122.5(9) . . ? C8Y C7Y C6Y 117.6(9) . . ? C8Y C7Y C10Y 124.0(10) . . ? C6Y C7Y C10Y 118.4(10) . . ? C7Y C8Y C9Y 121.2(11) . . ? C4Y C9Y C8Y 120.0(11) . . ? N4B C10Y C7Y 116.8(10) . . ? C10Y N4B C10B 85.7(10) . . ? C10Y N4B C11B 114.6(7) . . ? C10B N4B C11B 122.7(8) . . ? C10Y N4B C14Y 114.7(9) . . ? C10B N4B C14Y 29.7(7) . . ? C11B N4B C14Y 102.2(7) . . ? C10Y N4B C14B 17.9(9) . . ? C10B N4B C14B 103.6(9) . . ? C11B N4B C14B 104.6(6) . . ? C14Y N4B C14B 132.6(8) . . ? C12B C11B N4B 112.6(6) . . ? C11B C12B N2 111.8(6) . . ? C2C C1C N1 112.3(6) . . ? C1C C2C N3C 112.6(6) . . ? C3C N3C C3X 81.0(9) . . ? C3C N3C C2C 115.3(7) . . ? C3X N3C C2C 117.2(7) . . ? C3C N3C C13C 109.6(9) . . ? C3X N3C C13C 28.6(8) . . ? C2C N3C C13C 102.9(7) . . ? C3C N3C C13X 22.0(8) . . ? C3X N3C C13X 102.9(9) . . ? C2C N3C C13X 103.6(7) . . ? C13C N3C C13X 131.5(9) . . ? N3C C3C C4C 115.4(11) . . ? C9C C4C C5C 116.9(9) . . ? C9C C4C C3C 123.4(10) . . ? C5C C4C C3C 119.7(10) . . ? C6C C5C C4C 120.8(10) . . ? C5C C6C C7C 121.7(10) . . ? C8C C7C C6C 118.5(9) . . ? C8C C7C C10C 120.7(10) . . ? C6C C7C C10C 120.5(10) . . ? C7C C8C C9C 119.2(11) . . ? C4C C9C C8C 122.7(11) . . ? N4C C10C C7C 120.3(11) . . ? N3C C3X C4X 120.1(9) . . ? C9X C4X C5X 119.4(9) . . ? C9X C4X C3X 120.7(10) . . ? C5X C4X C3X 119.7(10) . . ? C6X C5X C4X 118.0(10) . . ? C5X C6X C7X 122.4(9) . . ? C8X C7X C6X 118.9(9) . . ? C8X C7X C10X 120.0(10) . . ? C6X C7X C10X 120.4(10) . . ? C7X C8X C9X 119.0(10) . . ? C4X C9X C8X 121.7(10) . . ? N4C C10X C7X 111.7(10) . . ? C10X N4C C10C 87.0(10) . . ? C10X N4C C11C 109.8(8) . . ? C10C N4C C11C 121.4(8) . . ? C10X N4C C14X 111.0(9) . . ? C10C N4C C14X 25.9(7) . . ? C11C N4C C14X 102.5(7) . . ? C10X N4C C14C 17.2(9) . . ? C10C N4C C14C 104.0(9) . . ? C11C N4C C14C 102.1(7) . . ? C14X N4C C14C 128.3(9) . . ? N4C C11C C12C 113.2(6) . . ? N2 C12C C11C 112.0(5) . . ? O12 Cl1 O11 127.7(5) . . ? O12 Cl1 O14 98.2(7) . . ? O11 Cl1 O14 120.2(5) . . ? O12 Cl1 O13 105.2(6) . . ? O11 Cl1 O13 100.6(4) . . ? O14 Cl1 O13 101.4(6) . . ? O21 Cl2 O23 113.2(5) . . ? O21 Cl2 O22 107.8(6) . . ? O23 Cl2 O22 109.0(8) . . ? O21 Cl2 O24 115.7(5) . . ? O23 Cl2 O24 108.6(6) . . ? O22 Cl2 O24 101.8(6) . . ? N1S C2S C1S 176.6(8) . . ? N2S C4S C3S 176.2(8) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.262 _refine_diff_density_min -0.273 _refine_diff_density_rms 0.033 data_Complex2(zof7) _database_code_depnum_ccdc_archive 'CCDC 630226' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H69 Cl2 Cu2 N10 O10.50' _chemical_formula_weight 1116.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.1316(11) _cell_length_b 18.2444(13) _cell_length_c 17.4585(12) _cell_angle_alpha 90.00 _cell_angle_beta 92.0860(10) _cell_angle_gamma 90.00 _cell_volume 5134.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11006 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 21.85 _exptl_crystal_description block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2340 _exptl_absorpt_coefficient_mu 0.998 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7674 _exptl_absorpt_correction_T_max 0.8178 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35937 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9023 _reflns_number_gt 6762 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0779P)^2^+6.6669P] 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 9023 _refine_ls_number_parameters 657 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.0732 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1494 _refine_ls_wR_factor_gt 0.1345 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.095 _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 0.46311(3) 0.57132(3) 0.86398(3) 0.02345(15) Uani 1 1 d . . . Cu2 Cu -0.03104(3) 0.69409(3) 0.59308(3) 0.02228(14) Uani 1 1 d . . . N1 N 0.4847(2) 0.55201(18) 0.75247(19) 0.0231(7) Uani 1 1 d . . . C1A C 0.4519(3) 0.4762(2) 0.7416(3) 0.0303(10) Uani 1 1 d . . . H1A1 H 0.4852 0.4414 0.7734 0.036 Uiso 1 1 calc R . . H1A2 H 0.4554 0.4615 0.6872 0.036 Uiso 1 1 calc R . . C2A C 0.3621(3) 0.4751(2) 0.7651(2) 0.0292(10) Uani 1 1 d . . . H2A1 H 0.3266 0.4986 0.7247 0.035 Uiso 1 1 calc R . . H2A2 H 0.3435 0.4237 0.7707 0.035 Uiso 1 1 calc R . . N3A N 0.3533(2) 0.51467(19) 0.83890(19) 0.0256(8) Uani 1 1 d . . . C3A C 0.2936(2) 0.5781(2) 0.8338(2) 0.0242(9) Uani 1 1 d . . . H3A1 H 0.3203 0.6176 0.8047 0.029 Uiso 1 1 calc R . . H3A2 H 0.2867 0.5967 0.8864 0.029 Uiso 1 1 calc R . . C4A C 0.2078(2) 0.5664(2) 0.7980(2) 0.0238(9) Uani 1 1 d . . . C5A C 0.1910(3) 0.5848(2) 0.7219(2) 0.0274(9) Uani 1 1 d . . . H5A H 0.2352 0.6000 0.6911 0.033 Uiso 1 1 calc R . . C6A C 0.1109(3) 0.5813(2) 0.6898(2) 0.0280(9) Uani 1 1 d . . . H6A H 0.1010 0.5929 0.6372 0.034 Uiso 1 1 calc R . . C7A C 0.0455(2) 0.5610(2) 0.7348(2) 0.0247(9) Uani 1 1 d . A . C8A C 0.0619(2) 0.5418(2) 0.8102(2) 0.0266(9) Uani 1 1 d . . . H8A H 0.0175 0.5273 0.8411 0.032 Uiso 1 1 calc R . . C9A C 0.1419(3) 0.5433(2) 0.8420(2) 0.0268(9) Uani 1 1 d . . . H9A H 0.1519 0.5285 0.8937 0.032 Uiso 1 1 calc R . . C10A C -0.0419(3) 0.5616(2) 0.7020(3) 0.0295(10) Uani 1 1 d . . . H10A H -0.0783 0.5370 0.7385 0.035 Uiso 1 1 calc R A . H10B H -0.0440 0.5329 0.6539 0.035 Uiso 1 1 calc R . . N4A N -0.0751(2) 0.63719(19) 0.6856(2) 0.0259(8) Uani 1 1 d . A . C11A C -0.0663(3) 0.6854(2) 0.7548(2) 0.0284(9) Uani 1 1 d . . . H11A H -0.0118 0.6767 0.7811 0.034 Uiso 1 1 calc R A . H11B H -0.1101 0.6735 0.7910 0.034 Uiso 1 1 calc R . . C12A C -0.0733(3) 0.7653(2) 0.7309(2) 0.0268(9) Uani 1 1 d . A . H12A H -0.1315 0.7768 0.7153 0.032 Uiso 1 1 calc R . . H12B H -0.0568 0.7973 0.7746 0.032 Uiso 1 1 calc R . . N2 N -0.0186(2) 0.77901(17) 0.66591(19) 0.0218(7) Uani 1 1 d . A . C13A C 0.3278(3) 0.4630(3) 0.8991(3) 0.0335(10) Uani 1 1 d . . . H13A H 0.3227 0.4895 0.9475 0.050 Uiso 1 1 calc R . . H13B H 0.3695 0.4243 0.9056 0.050 Uiso 1 1 calc R . . H13C H 0.2742 0.4411 0.8839 0.050 Uiso 1 1 calc R . . C14A C -0.1645(3) 0.6294(3) 0.6620(3) 0.0354(11) Uani 1 1 d . . . H14A H -0.1697 0.5982 0.6164 0.053 Uiso 1 1 calc R A . H14B H -0.1880 0.6778 0.6504 0.053 Uiso 1 1 calc R . . H14C H -0.1945 0.6069 0.7039 0.053 Uiso 1 1 calc R . . C1B C 0.4447(3) 0.6041(2) 0.6972(2) 0.0248(9) Uani 1 1 d . . . H1B1 H 0.4570 0.6546 0.7150 0.030 Uiso 1 1 calc R . . H1B2 H 0.3839 0.5973 0.6983 0.030 Uiso 1 1 calc R . . C2B C 0.4707(3) 0.5972(3) 0.6145(2) 0.0317(10) Uani 1 1 d . . . H2B1 H 0.5190 0.6293 0.6062 0.038 Uiso 1 1 calc R . . H2B2 H 0.4875 0.5460 0.6044 0.038 Uiso 1 1 calc R . . N3B N 0.4020(2) 0.6178(2) 0.5615(2) 0.0320(9) Uani 1 1 d . . . C3B C 0.3789(3) 0.6948(2) 0.5696(3) 0.0316(10) Uani 1 1 d . . . H3B1 H 0.4188 0.7255 0.5421 0.038 Uiso 1 1 calc R . . H3B2 H 0.3830 0.7084 0.6245 0.038 Uiso 1 1 calc R . . C4B C 0.2918(3) 0.7109(2) 0.5384(2) 0.0242(9) Uani 1 1 d . . . C5B C 0.2685(3) 0.7833(2) 0.5230(2) 0.0266(9) Uani 1 1 d . . . H5B H 0.3072 0.8219 0.5318 0.032 Uiso 1 1 calc R . . C6B C 0.1892(3) 0.7990(2) 0.4949(2) 0.0271(9) Uani 1 1 d . . . H6B H 0.1742 0.8484 0.4842 0.032 Uiso 1 1 calc R . . C7B C 0.1308(3) 0.7436(2) 0.4819(2) 0.0267(9) Uani 1 1 d . A . C8B C 0.1544(3) 0.6721(2) 0.4980(2) 0.0292(10) Uani 1 1 d . . . H8B H 0.1157 0.6334 0.4897 0.035 Uiso 1 1 calc R . . C9B C 0.2341(3) 0.6562(2) 0.5263(2) 0.0294(10) Uani 1 1 d . . . H9B H 0.2489 0.6069 0.5375 0.035 Uiso 1 1 calc R . . C10B C 0.0447(3) 0.7587(3) 0.4485(2) 0.0310(10) Uani 1 1 d . . . H10C H 0.0470 0.8022 0.4148 0.037 Uiso 1 1 calc R A . H10D H 0.0268 0.7165 0.4163 0.037 Uiso 1 1 calc R . . N4B N -0.0189(2) 0.77182(18) 0.50735(19) 0.0240(7) Uani 1 1 d . A . C11B C -0.0041(3) 0.8435(2) 0.5456(2) 0.0258(9) Uani 1 1 d . . . H11C H -0.0264 0.8835 0.5125 0.031 Uiso 1 1 calc R A . H11D H 0.0562 0.8515 0.5540 0.031 Uiso 1 1 calc R . . C12B C -0.0460(2) 0.8447(2) 0.6214(2) 0.0242(9) Uani 1 1 d . A . H12C H -0.0307 0.8898 0.6500 0.029 Uiso 1 1 calc R . . H12D H -0.1070 0.8439 0.6129 0.029 Uiso 1 1 calc R . . C13B C 0.4236(4) 0.6013(3) 0.4825(3) 0.0570(16) Uani 1 1 d . . . H13D H 0.4388 0.5494 0.4786 0.085 Uiso 1 1 calc R . . H13E H 0.4705 0.6318 0.4682 0.085 Uiso 1 1 calc R . . H13F H 0.3758 0.6114 0.4479 0.085 Uiso 1 1 calc R . . C14B C -0.1018(3) 0.7730(3) 0.4669(3) 0.0308(10) Uani 1 1 d . . . H14D H -0.1122 0.7256 0.4419 0.046 Uiso 1 1 calc R A . H14E H -0.1031 0.8120 0.4282 0.046 Uiso 1 1 calc R . . H14F H -0.1448 0.7823 0.5040 0.046 Uiso 1 1 calc R . . C1C C 0.5773(2) 0.5569(2) 0.7516(3) 0.0305(10) Uani 1 1 d . . . H1C1 H 0.5963 0.5527 0.6985 0.037 Uiso 1 1 calc R . . H1C2 H 0.6029 0.5168 0.7826 0.037 Uiso 1 1 calc R . . C2C C 0.6016(3) 0.6311(3) 0.7855(2) 0.0316(10) Uani 1 1 d . . . H2C1 H 0.6628 0.6353 0.7898 0.038 Uiso 1 1 calc R . . H2C2 H 0.5803 0.6709 0.7515 0.038 Uiso 1 1 calc R . . N3C N 0.5662(2) 0.63845(19) 0.8622(2) 0.0262(8) Uani 1 1 d . . . C3C C 0.5489(3) 0.7177(2) 0.8792(3) 0.0303(10) Uani 1 1 d . . . H3C1 H 0.5975 0.7472 0.8652 0.036 Uiso 1 1 calc R . . H3C2 H 0.5424 0.7232 0.9351 0.036 Uiso 1 1 calc R . . C4C C 0.4728(2) 0.7484(2) 0.8381(2) 0.0251(9) Uani 1 1 d . . . C5C C 0.4761(3) 0.7901(2) 0.7715(3) 0.0281(10) Uani 1 1 d . . . H5C H 0.5283 0.8006 0.7504 0.034 Uiso 1 1 calc R . . C6C C 0.4040(3) 0.8166(2) 0.7354(2) 0.0253(9) Uani 1 1 d . . . H6C H 0.4078 0.8449 0.6900 0.030 Uiso 1 1 calc R . . C7C C 0.3263(2) 0.8026(2) 0.7645(2) 0.0207(8) Uani 1 1 d . . . C8C C 0.3232(2) 0.7628(2) 0.8317(2) 0.0228(9) Uani 1 1 d . . . H8C H 0.2710 0.7535 0.8532 0.027 Uiso 1 1 calc R . . C9C C 0.3951(2) 0.7362(2) 0.8683(2) 0.0240(9) Uani 1 1 d . . . H9C H 0.3913 0.7093 0.9146 0.029 Uiso 1 1 calc R . . C10C C 0.2481(2) 0.8269(2) 0.7215(2) 0.0245(9) Uani 1 1 d . . . H10E H 0.2602 0.8715 0.6916 0.029 Uiso 1 1 calc R . . H10F H 0.2305 0.7881 0.6848 0.029 Uiso 1 1 calc R . . N4C N 0.1796(2) 0.84256(17) 0.77240(18) 0.0224(7) Uani 1 1 d . . . C11C C 0.1006(2) 0.8531(2) 0.7291(2) 0.0249(9) Uani 1 1 d . A . H11E H 0.1076 0.8912 0.6895 0.030 Uiso 1 1 calc R . . H11F H 0.0579 0.8703 0.7642 0.030 Uiso 1 1 calc R . . C12C C 0.0717(2) 0.7820(2) 0.6909(2) 0.0228(9) Uani 1 1 d . . . H12E H 0.1054 0.7736 0.6455 0.027 Uiso 1 1 calc R A . H12F H 0.0832 0.7411 0.7271 0.027 Uiso 1 1 calc R . . C13C C 0.6289(3) 0.6127(3) 0.9210(3) 0.0343(11) Uani 1 1 d . . . H13G H 0.6062 0.6171 0.9720 0.051 Uiso 1 1 calc R . . H13H H 0.6791 0.6428 0.9184 0.051 Uiso 1 1 calc R . . H13I H 0.6428 0.5614 0.9110 0.051 Uiso 1 1 calc R . . C14C C 0.1985(3) 0.9091(2) 0.8165(3) 0.0324(10) Uani 1 1 d . . . H14G H 0.1532 0.9194 0.8508 0.049 Uiso 1 1 calc R . . H14H H 0.2048 0.9504 0.7813 0.049 Uiso 1 1 calc R . . H14I H 0.2502 0.9021 0.8468 0.049 Uiso 1 1 calc R . . N31 N 0.4417(2) 0.5872(2) 0.9701(2) 0.0311(8) Uani 1 1 d . . . C32 C 0.4503(2) 0.5681(2) 1.0341(2) 0.0256(9) Uani 1 1 d . . . O33 O 0.4590(2) 0.54830(19) 1.09952(18) 0.0414(8) Uani 1 1 d . . . N41 N -0.0405(2) 0.6118(2) 0.5251(2) 0.0325(9) Uani 0.80 1 d P A 1 C42 C -0.0378(4) 0.5954(3) 0.4604(4) 0.0397(14) Uani 0.80 1 d P A 1 O43 O -0.0346(3) 0.5782(3) 0.3938(3) 0.0687(15) Uani 0.80 1 d P A 1 N41' N -0.0405(2) 0.6118(2) 0.5251(2) 0.0325(9) Uani 0.20 1 d P A 2 C42' C -0.0780(11) 0.5588(10) 0.5101(10) 0.016(4) Uiso 0.20 1 d P A 2 O43' O -0.1164(12) 0.5069(11) 0.4890(11) 0.057(5) Uiso 0.20 1 d P A 2 Cl1 Cl 0.33702(7) 0.24230(7) 0.38232(9) 0.0481(3) Uani 1 1 d . . . O11 O 0.4145(2) 0.2110(2) 0.4044(3) 0.0709(13) Uani 1 1 d . . . O12 O 0.3177(3) 0.2191(3) 0.3032(3) 0.0825(14) Uani 1 1 d . . . O13 O 0.2723(3) 0.2171(2) 0.4264(3) 0.0864(17) Uani 1 1 d . . . O14 O 0.3420(2) 0.3205(2) 0.3813(3) 0.0581(11) Uani 1 1 d . . . Cl2 Cl 0.17115(6) 0.48207(6) 0.07635(6) 0.0301(2) Uani 1 1 d . . . O21 O 0.2327(2) 0.53795(19) 0.0720(2) 0.0567(10) Uani 1 1 d . . . O22 O 0.1819(3) 0.4429(2) 0.1466(2) 0.0590(11) Uani 1 1 d . . . O23 O 0.0906(2) 0.5139(2) 0.0720(2) 0.0617(11) Uani 1 1 d . . . O24 O 0.1799(2) 0.43289(17) 0.01382(19) 0.0393(8) Uani 1 1 d . . . O51 O 0.3340(9) 0.4840(8) 0.5853(8) 0.051(4) Uani 0.25 1 d PU B 1 H51 H 0.3496 0.5161 0.5546 0.050 Uiso 0.25 1 calc PR B 1 C52 C 0.2959(9) 0.4323(7) 0.5477(8) 0.068(3) Uani 0.25 1 d PU B 1 H52A H 0.3345 0.4124 0.5101 0.040 Uiso 0.25 1 calc PR B 1 H52B H 0.2488 0.4546 0.5181 0.040 Uiso 0.25 1 calc PR B 1 C53 C 0.2668(8) 0.3765(7) 0.5870(9) 0.080(4) Uani 0.25 1 d PU B 1 H53A H 0.2399 0.3413 0.5516 0.050 Uiso 0.25 1 calc PR B 1 H53B H 0.2262 0.3944 0.6230 0.050 Uiso 0.25 1 calc PR B 1 H53C H 0.3125 0.3523 0.6155 0.050 Uiso 0.25 1 calc PR B 1 O51' O 0.3665(12) 0.4104(10) 0.5384(11) 0.078(5) Uani 0.25 1 d PU C 2 H51' H 0.3647 0.3715 0.5128 0.050 Uiso 0.25 1 calc PR C 2 C52' C 0.2959(9) 0.4323(7) 0.5477(8) 0.068(3) Uani 0.25 1 d PU C 2 H52C H 0.2648 0.4393 0.4983 0.040 Uiso 0.25 1 calc PR C 2 H52D H 0.2955 0.4784 0.5775 0.040 Uiso 0.25 1 calc PR C 2 C53' C 0.2668(8) 0.3765(7) 0.5870(9) 0.080(4) Uani 0.25 1 d PU C 2 H53D H 0.2094 0.3866 0.6002 0.050 Uiso 0.25 1 calc PR C 2 H53E H 0.3009 0.3696 0.6340 0.050 Uiso 0.25 1 calc PR C 2 H53F H 0.2684 0.3319 0.5558 0.050 Uiso 0.25 1 calc PR C 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 0.0178(3) 0.0292(3) 0.0232(3) 0.0044(2) -0.00143(19) 0.0015(2) Cu2 0.0205(3) 0.0214(3) 0.0246(3) -0.0016(2) -0.00346(19) -0.0001(2) N1 0.0184(17) 0.0262(18) 0.0245(18) 0.0032(14) -0.0005(14) 0.0071(14) C1A 0.030(2) 0.028(2) 0.032(2) 0.0017(18) -0.0003(19) 0.0103(19) C2A 0.032(2) 0.026(2) 0.030(2) 0.0030(18) -0.0061(19) 0.0021(18) N3A 0.0215(18) 0.0285(19) 0.0267(18) 0.0066(15) -0.0005(14) 0.0011(15) C3A 0.018(2) 0.026(2) 0.028(2) 0.0001(17) -0.0021(17) -0.0013(17) C4A 0.019(2) 0.023(2) 0.029(2) 0.0018(17) -0.0025(17) 0.0019(17) C5A 0.019(2) 0.032(2) 0.031(2) 0.0044(18) 0.0039(17) -0.0009(18) C6A 0.026(2) 0.030(2) 0.027(2) 0.0043(18) -0.0067(18) 0.0009(18) C7A 0.023(2) 0.018(2) 0.034(2) 0.0021(17) -0.0031(18) -0.0026(16) C8A 0.018(2) 0.026(2) 0.036(2) 0.0048(18) 0.0048(17) -0.0021(17) C9A 0.025(2) 0.028(2) 0.027(2) 0.0038(18) -0.0003(17) 0.0018(18) C10A 0.023(2) 0.025(2) 0.040(3) 0.0061(19) -0.0047(19) -0.0037(18) N4A 0.0211(18) 0.0255(18) 0.0308(19) 0.0014(15) -0.0026(15) -0.0023(14) C11A 0.025(2) 0.033(2) 0.027(2) 0.0028(18) 0.0018(18) -0.0004(19) C12A 0.023(2) 0.031(2) 0.027(2) -0.0012(18) 0.0037(17) 0.0030(18) N2 0.0176(17) 0.0202(17) 0.0274(18) -0.0016(14) -0.0016(14) 0.0024(14) C13A 0.029(2) 0.036(3) 0.035(3) 0.013(2) -0.0038(19) -0.004(2) C14A 0.015(2) 0.042(3) 0.049(3) 0.007(2) -0.0068(19) -0.0026(19) C1B 0.021(2) 0.028(2) 0.025(2) 0.0050(17) -0.0004(17) 0.0060(17) C2B 0.024(2) 0.040(3) 0.031(2) 0.006(2) 0.0008(18) 0.0117(19) N3B 0.032(2) 0.041(2) 0.0223(19) -0.0006(16) -0.0030(15) 0.0142(17) C3B 0.029(2) 0.035(2) 0.031(2) 0.0060(19) -0.0038(19) 0.0045(19) C4B 0.026(2) 0.029(2) 0.017(2) 0.0033(17) 0.0030(16) 0.0047(18) C5B 0.026(2) 0.030(2) 0.024(2) 0.0015(17) 0.0045(17) 0.0048(18) C6B 0.030(2) 0.029(2) 0.022(2) 0.0068(17) 0.0069(17) 0.0068(19) C7B 0.026(2) 0.036(2) 0.018(2) 0.0003(17) 0.0032(17) 0.0079(19) C8B 0.028(2) 0.033(2) 0.027(2) -0.0051(18) 0.0020(18) 0.0018(19) C9B 0.033(2) 0.028(2) 0.027(2) 0.0026(18) 0.0004(18) 0.0079(19) C10B 0.029(2) 0.037(3) 0.026(2) 0.0018(19) -0.0008(18) 0.005(2) N4B 0.0203(18) 0.0254(18) 0.0258(18) 0.0015(14) -0.0045(14) 0.0019(14) C11B 0.022(2) 0.024(2) 0.031(2) 0.0028(18) -0.0034(17) 0.0027(17) C12B 0.021(2) 0.019(2) 0.032(2) -0.0020(17) -0.0049(17) 0.0049(16) C13B 0.067(4) 0.073(4) 0.031(3) 0.000(3) -0.002(3) 0.041(3) C14B 0.025(2) 0.035(2) 0.032(2) 0.0000(19) -0.0095(18) 0.0030(19) C1C 0.020(2) 0.041(3) 0.031(2) 0.006(2) 0.0038(18) 0.0117(19) C2C 0.018(2) 0.042(3) 0.034(2) 0.008(2) 0.0034(18) 0.0016(19) N3C 0.0190(18) 0.0294(19) 0.0299(19) 0.0074(15) -0.0039(14) 0.0045(15) C3C 0.018(2) 0.034(2) 0.039(3) 0.001(2) -0.0044(18) -0.0030(18) C4C 0.020(2) 0.027(2) 0.029(2) -0.0021(18) -0.0026(17) -0.0023(17) C5C 0.019(2) 0.028(2) 0.038(3) 0.0038(19) 0.0034(18) -0.0062(17) C6C 0.027(2) 0.021(2) 0.028(2) 0.0044(17) 0.0025(18) -0.0009(17) C7C 0.022(2) 0.0189(19) 0.021(2) -0.0016(16) -0.0021(16) 0.0004(16) C8C 0.018(2) 0.026(2) 0.025(2) -0.0011(17) 0.0035(16) -0.0012(16) C9C 0.025(2) 0.026(2) 0.021(2) 0.0026(16) -0.0002(17) 0.0009(17) C10C 0.023(2) 0.027(2) 0.023(2) 0.0007(17) -0.0028(17) 0.0015(17) N4C 0.0202(17) 0.0222(17) 0.0243(18) -0.0046(14) -0.0049(14) 0.0039(14) C11C 0.021(2) 0.024(2) 0.029(2) -0.0024(17) -0.0063(17) 0.0040(17) C12C 0.016(2) 0.025(2) 0.027(2) -0.0014(17) -0.0060(16) 0.0027(16) C13C 0.019(2) 0.043(3) 0.040(3) 0.008(2) -0.0106(19) 0.0064(19) C14C 0.030(2) 0.028(2) 0.038(3) -0.010(2) -0.008(2) 0.0040(19) N31 0.027(2) 0.042(2) 0.024(2) -0.0002(17) 0.0019(15) -0.0026(16) C32 0.022(2) 0.029(2) 0.026(3) -0.0054(19) 0.0019(17) -0.0025(18) O33 0.043(2) 0.046(2) 0.0344(19) 0.0076(16) -0.0046(15) 0.0029(16) N41 0.034(2) 0.027(2) 0.036(2) -0.0062(17) -0.0033(17) -0.0035(16) C42 0.037(3) 0.037(3) 0.045(4) -0.012(3) -0.005(3) -0.004(3) O43 0.078(4) 0.076(4) 0.052(3) -0.027(3) 0.003(3) 0.004(3) N41' 0.034(2) 0.027(2) 0.036(2) -0.0062(17) -0.0033(17) -0.0035(16) Cl1 0.0259(6) 0.0467(7) 0.0723(9) 0.0228(7) 0.0075(6) 0.0047(5) O11 0.031(2) 0.077(3) 0.105(4) 0.030(3) 0.004(2) 0.018(2) O12 0.079(3) 0.079(3) 0.089(4) 0.005(3) -0.001(3) -0.006(3) O13 0.054(3) 0.067(3) 0.142(5) 0.039(3) 0.056(3) 0.013(2) O14 0.034(2) 0.048(2) 0.092(3) 0.020(2) 0.003(2) -0.0027(17) Cl2 0.0276(6) 0.0270(5) 0.0360(6) 0.0021(4) 0.0074(4) 0.0026(4) O21 0.061(3) 0.035(2) 0.074(3) -0.0092(18) 0.009(2) -0.0189(18) O22 0.065(3) 0.075(3) 0.038(2) 0.0200(19) 0.0123(18) 0.012(2) O23 0.043(2) 0.061(3) 0.083(3) 0.009(2) 0.017(2) 0.0263(19) O24 0.0350(18) 0.0385(19) 0.045(2) -0.0109(15) 0.0047(15) -0.0044(15) O51 0.063(8) 0.052(7) 0.037(7) 0.013(6) -0.017(6) -0.016(6) C52 0.072(6) 0.055(6) 0.077(7) -0.036(5) -0.016(6) -0.006(5) C53 0.058(6) 0.057(6) 0.121(8) -0.016(6) -0.041(6) -0.009(5) O51' 0.070(8) 0.071(10) 0.092(10) -0.045(8) 0.000(8) -0.021(7) C52' 0.072(6) 0.055(6) 0.077(7) -0.036(5) -0.016(6) -0.006(5) C53' 0.058(6) 0.057(6) 0.121(8) -0.016(6) -0.041(6) -0.009(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 N31 1.918(4) . y Cu1 N1 2.021(3) . y Cu1 N3C 2.067(3) . y Cu1 N3A 2.083(3) . y Cu1 O33 2.586(3) 3_667 y Cu2 N41 1.916(4) . y Cu2 N2 2.010(3) . y Cu2 N4A 2.067(3) . y Cu2 N4B 2.076(3) . y N1 C1B 1.485(5) . ? N1 C1A 1.490(5) . ? N1 C1C 1.497(5) . ? C1A C2A 1.520(6) . ? C2A N3A 1.488(5) . ? N3A C13A 1.481(5) . ? N3A C3A 1.507(5) . ? C3A C4A 1.512(5) . ? C4A C5A 1.387(6) . ? C4A C9A 1.400(6) . ? C5A C6A 1.391(6) . ? C6A C7A 1.390(6) . ? C7A C8A 1.379(6) . ? C7A C10A 1.501(5) . ? C8A C9A 1.385(6) . ? C10A N4A 1.504(5) . ? N4A C14A 1.492(5) . ? N4A C11A 1.497(5) . ? C11A C12A 1.518(6) . ? C12A N2 1.484(5) . ? N2 C12B 1.487(5) . ? N2 C12C 1.507(5) . ? C1B C2B 1.524(6) . ? C2B N3B 1.467(5) . ? N3B C3B 1.460(6) . ? N3B C13B 1.467(6) . ? C3B C4B 1.518(6) . ? C4B C9B 1.376(6) . ? C4B C5B 1.397(6) . ? C5B C6B 1.384(6) . ? C6B C7B 1.394(6) . ? C7B C8B 1.385(6) . ? C7B C10B 1.512(6) . ? C8B C9B 1.390(6) . ? C10B N4B 1.498(5) . ? N4B C11B 1.484(5) . ? N4B C14B 1.490(5) . ? C11B C12B 1.508(6) . ? C1C C2C 1.524(6) . ? C2C N3C 1.482(5) . ? N3C C13C 1.490(5) . ? N3C C3C 1.504(6) . ? C3C C4C 1.507(6) . ? C4C C5C 1.393(6) . ? C4C C9C 1.395(6) . ? C5C C6C 1.388(6) . ? C6C C7C 1.393(6) . ? C7C C8C 1.381(5) . ? C7C C10C 1.512(5) . ? C8C C9C 1.393(6) . ? C10C N4C 1.471(5) . ? N4C C14C 1.464(5) . ? N4C C11C 1.470(5) . ? C11C C12C 1.524(6) . ? N31 C32 1.175(5) . ? C32 O33 1.201(5) . ? N41 C42 1.170(7) . ? C42 O43 1.208(8) . ? C42' O43' 1.18(3) . ? Cl1 O13 1.397(4) . ? Cl1 O11 1.415(4) . ? Cl1 O14 1.430(4) . ? Cl1 O12 1.467(5) . ? Cl2 O23 1.423(4) . ? Cl2 O24 1.424(3) . ? Cl2 O22 1.425(4) . ? Cl2 O21 1.427(4) . ? O51 C52 1.292(17) . ? C52 C53 1.324(19) . ? 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 N31 Cu1 N1 178.60(15) . . y N31 Cu1 N3C 95.61(15) . . y N1 Cu1 N3C 85.52(14) . . y N31 Cu1 N3A 95.54(14) . . y N1 Cu1 N3A 83.47(13) . . y N3C Cu1 N3A 165.79(13) . . y N31 Cu1 O33 89.57(14) . 3_667 y N1 Cu1 O33 89.48(12) . 3_667 y N3C Cu1 O33 96.88(12) . 3_667 y N3A Cu1 O33 91.99(12) . 3_667 y N41 Cu2 N2 178.47(15) . . y N41 Cu2 N4A 93.93(15) . . y N2 Cu2 N4A 85.54(13) . . y N41 Cu2 N4B 95.50(15) . . y N2 Cu2 N4B 85.40(13) . . y N4A Cu2 N4B 161.83(13) . . y C1B N1 C1A 111.6(3) . . ? C1B N1 C1C 111.5(3) . . ? C1A N1 C1C 113.8(3) . . ? C1B N1 Cu1 115.3(2) . . ? C1A N1 Cu1 102.2(2) . . ? C1C N1 Cu1 101.9(2) . . ? N1 C1A C2A 108.4(3) . . ? N3A C2A C1A 110.4(3) . . ? C13A N3A C2A 110.1(3) . . ? C13A N3A C3A 109.7(3) . . ? C2A N3A C3A 113.7(3) . . ? C13A N3A Cu1 115.0(3) . . ? C2A N3A Cu1 108.4(2) . . ? C3A N3A Cu1 99.7(2) . . ? N3A C3A C4A 119.4(3) . . ? C5A C4A C9A 118.2(4) . . ? C5A C4A C3A 120.3(4) . . ? C9A C4A C3A 121.2(4) . . ? C4A C5A C6A 121.4(4) . . ? C7A C6A C5A 119.9(4) . . ? C8A C7A C6A 118.9(4) . . ? C8A C7A C10A 120.8(4) . . ? C6A C7A C10A 120.3(4) . . ? C7A C8A C9A 121.4(4) . . ? C8A C9A C4A 120.1(4) . . ? C7A C10A N4A 113.7(3) . . ? C14A N4A C11A 110.0(3) . . ? C14A N4A C10A 107.4(3) . . ? C11A N4A C10A 111.2(3) . . ? C14A N4A Cu2 100.9(3) . . ? C11A N4A Cu2 108.0(2) . . ? C10A N4A Cu2 118.7(3) . . ? N4A C11A C12A 109.8(3) . . ? N2 C12A C11A 109.3(3) . . ? C12A N2 C12B 111.2(3) . . ? C12A N2 C12C 112.3(3) . . ? C12B N2 C12C 112.9(3) . . ? C12A N2 Cu2 107.8(2) . . ? C12B N2 Cu2 105.6(2) . . ? C12C N2 Cu2 106.5(2) . . ? N1 C1B C2B 115.7(3) . . ? N3B C2B C1B 110.4(3) . . ? C3B N3B C2B 112.1(4) . . ? C3B N3B C13B 111.0(4) . . ? C2B N3B C13B 109.9(3) . . ? N3B C3B C4B 112.9(4) . . ? C9B C4B C5B 118.8(4) . . ? C9B C4B C3B 121.8(4) . . ? C5B C4B C3B 119.4(4) . . ? C6B C5B C4B 120.1(4) . . ? C5B C6B C7B 121.3(4) . . ? C8B C7B C6B 118.0(4) . . ? C8B C7B C10B 119.5(4) . . ? C6B C7B C10B 122.4(4) . . ? C7B C8B C9B 120.8(4) . . ? C4B C9B C8B 121.0(4) . . ? N4B C10B C7B 114.0(3) . . ? C11B N4B C14B 109.1(3) . . ? C11B N4B C10B 110.3(3) . . ? C14B N4B C10B 107.7(3) . . ? C11B N4B Cu2 107.2(2) . . ? C14B N4B Cu2 104.2(2) . . ? C10B N4B Cu2 118.0(3) . . ? N4B C11B C12B 109.7(3) . . ? N2 C12B C11B 108.2(3) . . ? N1 C1C C2C 106.9(3) . . ? N3C C2C C1C 109.2(3) . . ? C2C N3C C13C 108.6(3) . . ? C2C N3C C3C 110.2(3) . . ? C13C N3C C3C 107.1(3) . . ? C2C N3C Cu1 107.3(3) . . ? C13C N3C Cu1 109.3(3) . . ? C3C N3C Cu1 114.3(2) . . ? N3C C3C C4C 114.7(3) . . ? C5C C4C C9C 117.7(4) . . ? C5C C4C C3C 123.1(4) . . ? C9C C4C C3C 119.2(4) . . ? C6C C5C C4C 120.8(4) . . ? C5C C6C C7C 121.3(4) . . ? C8C C7C C6C 117.9(4) . . ? C8C C7C C10C 121.3(3) . . ? C6C C7C C10C 120.7(4) . . ? C7C C8C C9C 121.1(4) . . ? C8C C9C C4C 121.1(4) . . ? N4C C10C C7C 112.9(3) . . ? C14C N4C C11C 108.8(3) . . ? C14C N4C C10C 109.4(3) . . ? C11C N4C C10C 111.7(3) . . ? N4C C11C C12C 111.1(3) . . ? N2 C12C C11C 115.7(3) . . ? C32 N31 Cu1 148.7(4) . . y N31 C32 O33 179.8(6) . . y C42 N41 Cu2 142.4(4) . . y N41 C42 O43 179.6(8) . . y O13 Cl1 O11 112.8(3) . . ? O13 Cl1 O14 112.2(3) . . ? O11 Cl1 O14 110.9(3) . . ? O13 Cl1 O12 106.6(3) . . ? O11 Cl1 O12 107.2(3) . . ? O14 Cl1 O12 106.6(3) . . ? O23 Cl2 O24 109.4(2) . . ? O23 Cl2 O22 109.4(2) . . ? O24 Cl2 O22 109.4(2) . . ? O23 Cl2 O21 110.0(2) . . ? O24 Cl2 O21 108.7(2) . . ? O22 Cl2 O21 110.0(3) . . ? O51 C52 C53 118.0(14) . . ? 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 O51 H51 N3B 0.84 2.04 2.716(15) 136.9 . O51' H51' O14 0.84 2.49 3.207(17) 143.9 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.950 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.101 data_Complex3(me6n3) _database_code_depnum_ccdc_archive 'CCDC 630227' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H69 Cl2 Cu2 N14 O8.50' _chemical_formula_weight 1116.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.1365(7) _cell_length_b 18.2403(8) _cell_length_c 17.3928(8) _cell_angle_alpha 90.00 _cell_angle_beta 92.2190(10) _cell_angle_gamma 90.00 _cell_volume 5115.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16546 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 28.64 _exptl_crystal_description block _exptl_crystal_colour brown-green _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2340 _exptl_absorpt_coefficient_mu 1.001 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6559 _exptl_absorpt_correction_T_max 0.7951 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39002 _diffrn_reflns_av_R_equivalents 0.0225 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10047 _reflns_number_gt 8214 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0721P)^2^+5.4468P] 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 10047 _refine_ls_number_parameters 667 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.1272 _refine_ls_wR_factor_gt 0.1160 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.070 _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 -0.46378(2) 0.574473(19) 0.133758(18) 0.02409(10) Uani 1 1 d . . . Cu2 Cu 0.03006(2) 0.692746(18) 0.412205(18) 0.02216(10) Uani 1 1 d . . . N1 N -0.48542(14) 0.55214(13) 0.24589(13) 0.0240(5) Uani 1 1 d . . . C1A C -0.44483(17) 0.60341(16) 0.30240(15) 0.0252(6) Uani 1 1 d . . . H1A1 H -0.4567 0.6543 0.2854 0.030 Uiso 1 1 calc R . . H1A2 H -0.3841 0.5962 0.3015 0.030 Uiso 1 1 calc R . . C2A C -0.47154(19) 0.59509(19) 0.38548(17) 0.0331(7) Uani 1 1 d . . . H2A1 H -0.5199 0.6271 0.3941 0.040 Uiso 1 1 calc R . . H2A2 H -0.4883 0.5437 0.3948 0.040 Uiso 1 1 calc R . . N3A N -0.40257(16) 0.61525(15) 0.43937(13) 0.0318(6) Uani 1 1 d . . . C3A C -0.37989(19) 0.69250(17) 0.43224(17) 0.0301(6) Uani 1 1 d . . . H3A1 H -0.4204 0.7228 0.4595 0.036 Uiso 1 1 calc R . . H3A2 H -0.3834 0.7065 0.3772 0.036 Uiso 1 1 calc R . . C4A C -0.29338(18) 0.70910(16) 0.46469(15) 0.0258(6) Uani 1 1 d . . . C5A C -0.27013(18) 0.78128(16) 0.47997(16) 0.0268(6) Uani 1 1 d . . . H5A H -0.3090 0.8197 0.4705 0.032 Uiso 1 1 calc R . . C6A C -0.19110(18) 0.79797(16) 0.50881(16) 0.0265(6) Uani 1 1 d . . . H6A H -0.1765 0.8476 0.5192 0.032 Uiso 1 1 calc R . . C7A C -0.13262(17) 0.74257(16) 0.52278(15) 0.0257(6) Uani 1 1 d . . . C8A C -0.15549(18) 0.67023(16) 0.50671(16) 0.0282(6) Uani 1 1 d . . . H8A H -0.1165 0.6318 0.5157 0.034 Uiso 1 1 calc R . . C9A C -0.23473(19) 0.65398(16) 0.47769(16) 0.0290(6) Uani 1 1 d . . . H9A H -0.2492 0.6045 0.4665 0.035 Uiso 1 1 calc R . . C10A C -0.04717(18) 0.75895(17) 0.55682(16) 0.0282(6) Uani 1 1 d . . . H10A H -0.0501 0.8037 0.5888 0.034 Uiso 1 1 calc R . . H10B H -0.0298 0.7180 0.5911 0.034 Uiso 1 1 calc R . . N4A N 0.01769(14) 0.76994(13) 0.49835(13) 0.0232(5) Uani 1 1 d . . . C11A C 0.00331(17) 0.84256(15) 0.46003(16) 0.0245(6) Uani 1 1 d . . . H11A H 0.0252 0.8824 0.4938 0.029 Uiso 1 1 calc R . . H11B H -0.0569 0.8507 0.4507 0.029 Uiso 1 1 calc R . . C12A C 0.04655(17) 0.84368(15) 0.38445(16) 0.0240(6) Uani 1 1 d . . . H12A H 0.0322 0.8891 0.3558 0.029 Uiso 1 1 calc R . . H12B H 0.1074 0.8424 0.3940 0.029 Uiso 1 1 calc R . . C13A C -0.4248(3) 0.5983(2) 0.51828(19) 0.0567(11) Uani 1 1 d . . . H13A H -0.3791 0.6123 0.5540 0.085 Uiso 1 1 calc R . . H13B H -0.4354 0.5456 0.5229 0.085 Uiso 1 1 calc R . . H13C H -0.4748 0.6256 0.5307 0.085 Uiso 1 1 calc R . . C14A C 0.10049(18) 0.77028(17) 0.53970(16) 0.0295(6) Uani 1 1 d . . . H14A H 0.1100 0.7228 0.5648 0.044 Uiso 1 1 calc R . . H14B H 0.1020 0.8092 0.5786 0.044 Uiso 1 1 calc R . . H14C H 0.1438 0.7791 0.5028 0.044 Uiso 1 1 calc R . . N2 N 0.01930(14) 0.77867(12) 0.33896(12) 0.0217(5) Uani 1 1 d . . . C1B C -0.57768(17) 0.55706(17) 0.24621(17) 0.0294(6) Uani 1 1 d . . . H1B1 H -0.5969 0.5510 0.2992 0.035 Uiso 1 1 calc R . . H1B2 H -0.6031 0.5181 0.2134 0.035 Uiso 1 1 calc R . . C2B C -0.60226(17) 0.63231(17) 0.21504(17) 0.0303(6) Uani 1 1 d . . . H2B1 H -0.6634 0.6363 0.2107 0.036 Uiso 1 1 calc R . . H2B2 H -0.5812 0.6709 0.2507 0.036 Uiso 1 1 calc R . . N3B N -0.56664(14) 0.64278(13) 0.13770(13) 0.0260(5) Uani 1 1 d . . . C3B C -0.54925(18) 0.72267(16) 0.12360(18) 0.0296(6) Uani 1 1 d . . . H3B1 H -0.5978 0.7517 0.1388 0.035 Uiso 1 1 calc R . . H3B2 H -0.5429 0.7301 0.0677 0.035 Uiso 1 1 calc R . . C4B C -0.47275(16) 0.75217(15) 0.16616(16) 0.0245(6) Uani 1 1 d . . . C5B C -0.47573(18) 0.79167(16) 0.23416(17) 0.0281(6) Uani 1 1 d . . . H5B H -0.5279 0.8008 0.2559 0.034 Uiso 1 1 calc R . . C6B C -0.40389(18) 0.81812(15) 0.27114(16) 0.0258(6) Uani 1 1 d . . . H6B H -0.4076 0.8454 0.3174 0.031 Uiso 1 1 calc R . . C7B C -0.32606(17) 0.80505(14) 0.24092(15) 0.0214(5) Uani 1 1 d . . . C8B C -0.32309(17) 0.76669(15) 0.17199(15) 0.0231(5) Uani 1 1 d . . . H8B H -0.2711 0.7579 0.1499 0.028 Uiso 1 1 calc R . . C9B C -0.39524(17) 0.74118(15) 0.13510(15) 0.0248(6) Uani 1 1 d . . . H9B H -0.3918 0.7157 0.0877 0.030 Uiso 1 1 calc R . . C10B C -0.24758(17) 0.82909(16) 0.28379(16) 0.0261(6) Uani 1 1 d . . . H10C H -0.2593 0.8738 0.3137 0.031 Uiso 1 1 calc R . . H10D H -0.2301 0.7902 0.3207 0.031 Uiso 1 1 calc R . . N4B N -0.17890(14) 0.84442(12) 0.23264(13) 0.0226(5) Uani 1 1 d . . . C11B C -0.09951(17) 0.85375(15) 0.27569(16) 0.0246(6) Uani 1 1 d . . . H11C H -0.1056 0.8916 0.3158 0.030 Uiso 1 1 calc R . . H11D H -0.0569 0.8708 0.2403 0.030 Uiso 1 1 calc R . . C12B C -0.07099(16) 0.78163(15) 0.31353(16) 0.0229(5) Uani 1 1 d . . . H12C H -0.1048 0.7728 0.3589 0.027 Uiso 1 1 calc R . . H12D H -0.0824 0.7412 0.2767 0.027 Uiso 1 1 calc R . . C13B C -0.62967(18) 0.61926(18) 0.07755(17) 0.0334(7) Uani 1 1 d . . . H13D H -0.6070 0.6256 0.0265 0.050 Uiso 1 1 calc R . . H13E H -0.6798 0.6492 0.0814 0.050 Uiso 1 1 calc R . . H13F H -0.6436 0.5676 0.0853 0.050 Uiso 1 1 calc R . . C14B C -0.19792(19) 0.91136(17) 0.18848(18) 0.0313(7) Uani 1 1 d . . . H14D H -0.2507 0.9052 0.1595 0.047 Uiso 1 1 calc R . . H14E H -0.1537 0.9206 0.1527 0.047 Uiso 1 1 calc R . . H14F H -0.2020 0.9529 0.2238 0.047 Uiso 1 1 calc R . . C1C C -0.45232(19) 0.47655(16) 0.25470(17) 0.0288(6) Uani 1 1 d . . . H1C1 H -0.4856 0.4424 0.2219 0.035 Uiso 1 1 calc R . . H1C2 H -0.4557 0.4605 0.3089 0.035 Uiso 1 1 calc R . . C2C C -0.36237(18) 0.47563(16) 0.23117(16) 0.0281(6) Uani 1 1 d . . . H2C1 H -0.3266 0.4974 0.2727 0.034 Uiso 1 1 calc R . . H2C2 H -0.3443 0.4244 0.2235 0.034 Uiso 1 1 calc R . . N3C N -0.35301(15) 0.51835(13) 0.15795(13) 0.0258(5) Uani 1 1 d . . . C3C C -0.29352(17) 0.58142(15) 0.16607(16) 0.0254(6) Uani 1 1 d . . . H3C1 H -0.3203 0.6198 0.1968 0.030 Uiso 1 1 calc R . . H3C2 H -0.2864 0.6020 0.1141 0.030 Uiso 1 1 calc R . . C4C C -0.20816(17) 0.56822(15) 0.20187(16) 0.0240(6) Uani 1 1 d . . . C5C C -0.19165(18) 0.58587(16) 0.27937(16) 0.0277(6) Uani 1 1 d . . . H5C H -0.2358 0.6012 0.3101 0.033 Uiso 1 1 calc R . . C6C C -0.11189(18) 0.58141(16) 0.31205(16) 0.0270(6) Uani 1 1 d . . . H6C H -0.1023 0.5924 0.3650 0.032 Uiso 1 1 calc R . . C7C C -0.04614(17) 0.56096(15) 0.26753(16) 0.0241(6) Uani 1 1 d . . . C8C C -0.06211(18) 0.54258(15) 0.19090(17) 0.0267(6) Uani 1 1 d . . . H8C H -0.0176 0.5278 0.1602 0.032 Uiso 1 1 calc R . . C9C C -0.14220(18) 0.54540(16) 0.15828(16) 0.0263(6) Uani 1 1 d . . . H9C H -0.1520 0.5317 0.1060 0.032 Uiso 1 1 calc R . . C10C C 0.04143(17) 0.56091(15) 0.30061(17) 0.0262(6) Uani 1 1 d . . . H10E H 0.0436 0.5312 0.3483 0.031 Uiso 1 1 calc R . . H10F H 0.0778 0.5370 0.2635 0.031 Uiso 1 1 calc R . . N4C N 0.07489(14) 0.63616(13) 0.31888(13) 0.0237(5) Uani 1 1 d . . . C11C C 0.06715(19) 0.68480(16) 0.25003(16) 0.0273(6) Uani 1 1 d . . . H11E H 0.0127 0.6767 0.2231 0.033 Uiso 1 1 calc R . . H11F H 0.1111 0.6726 0.2140 0.033 Uiso 1 1 calc R . . C12C C 0.07493(18) 0.76470(16) 0.27408(16) 0.0264(6) Uani 1 1 d . . . H12E H 0.1331 0.7757 0.2904 0.032 Uiso 1 1 calc R . . H12F H 0.0592 0.7969 0.2301 0.032 Uiso 1 1 calc R . . C13C C -0.3271(2) 0.46814(18) 0.09601(18) 0.0347(7) Uani 1 1 d . . . H13G H -0.3215 0.4959 0.0483 0.052 Uiso 1 1 calc R . . H13H H -0.3690 0.4297 0.0879 0.052 Uiso 1 1 calc R . . H13I H -0.2737 0.4457 0.1110 0.052 Uiso 1 1 calc R . . C14C C 0.16392(18) 0.62747(18) 0.34282(18) 0.0320(7) Uani 1 1 d . . . H14G H 0.1878 0.6756 0.3554 0.048 Uiso 1 1 calc R . . H14H H 0.1939 0.6055 0.3007 0.048 Uiso 1 1 calc R . . H14I H 0.1687 0.5956 0.3881 0.048 Uiso 1 1 calc R . . N11 N -0.43674(16) 0.60238(14) 0.02841(13) 0.0299(5) Uani 1 1 d . . . N12 N -0.45182(14) 0.56821(13) -0.02798(13) 0.0249(5) Uani 1 1 d . . . N13 N -0.46601(17) 0.53606(15) -0.08473(14) 0.0349(6) Uani 1 1 d . . . N21 N 0.03909(16) 0.60370(14) 0.47636(14) 0.0312(6) Uani 1 1 d . . . N22 N 0.03595(18) 0.59878(16) 0.54163(18) 0.0422(7) Uani 1 1 d . . . N23 N 0.0336(2) 0.59096(19) 0.60902(18) 0.0545(8) Uani 1 1 d . . . Cl1 Cl 0.17029(4) 0.51965(4) 0.07559(4) 0.02965(16) Uani 1 1 d . . . O11 O 0.17961(14) 0.57010(12) 0.01365(13) 0.0380(5) Uani 1 1 d . . . O12 O 0.23216(18) 0.46347(14) 0.07075(16) 0.0573(7) Uani 1 1 d . . . O13 O 0.18032(19) 0.55756(17) 0.14723(14) 0.0574(7) Uani 1 1 d . . . O14 O 0.08914(17) 0.48776(16) 0.06954(18) 0.0615(8) Uani 1 1 d . . . Cl2 Cl 0.33497(5) 0.76006(5) 0.38047(6) 0.0464(2) Uani 1 1 d . . . O21 O 0.26935(18) 0.78336(17) 0.42696(19) 0.0678(9) Uani 1 1 d . . . O22 O 0.3141(2) 0.78057(19) 0.30152(19) 0.0696(8) Uani 1 1 d . . . O23 O 0.34294(17) 0.68164(16) 0.38286(18) 0.0581(7) Uani 1 1 d . . . O24 O 0.41192(17) 0.79337(19) 0.40382(19) 0.0686(9) Uani 1 1 d . . . O1S O -0.3310(6) 0.4833(5) 0.4128(4) 0.053(2) Uani 0.30 1 d PDU A 1 H1S H -0.3491 0.5197 0.4366 0.050 Uiso 0.30 1 calc PR A 1 C1S C -0.2925(12) 0.4412(8) 0.4598(12) 0.060(5) Uani 0.30 1 d PDU A 1 H1S1 H -0.3251 0.4369 0.5066 0.050 Uiso 0.30 1 calc PR A 1 H1S2 H -0.2390 0.4645 0.4751 0.050 Uiso 0.30 1 calc PR A 1 C2S C -0.2771(10) 0.3739(7) 0.4343(9) 0.050(4) Uani 0.30 1 d PDU A 1 H2S1 H -0.2610 0.3422 0.4779 0.050 Uiso 0.30 1 calc PR A 1 H2S2 H -0.2319 0.3758 0.3983 0.050 Uiso 0.30 1 calc PR A 1 H2S3 H -0.3270 0.3542 0.4079 0.050 Uiso 0.30 1 calc PR A 1 O1S' O -0.3707(8) 0.4011(9) 0.4597(8) 0.061(4) Uani 0.20 1 d PDU B 2 H1S' H -0.3677 0.3605 0.4824 0.050 Uiso 0.20 1 calc PR B 2 C1S' C -0.3002(13) 0.4211(15) 0.4429(15) 0.050(6) Uani 0.20 1 d PDU B 2 H1S3 H -0.2663 0.4286 0.4908 0.050 Uiso 0.20 1 calc PR B 2 H1S4 H -0.3044 0.4687 0.4157 0.050 Uiso 0.20 1 calc PR B 2 C2S' C -0.2619(11) 0.3730(11) 0.3984(13) 0.043(4) Uani 0.20 1 d PDU B 2 H2S4 H -0.2062 0.3911 0.3880 0.050 Uiso 0.20 1 calc PR B 2 H2S5 H -0.2938 0.3670 0.3497 0.050 Uiso 0.20 1 calc PR B 2 H2S6 H -0.2575 0.3256 0.4249 0.050 Uiso 0.20 1 calc PR B 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 0.02279(18) 0.0298(2) 0.01962(18) -0.00204(13) 0.00040(13) -0.00339(13) Cu2 0.02476(18) 0.02187(18) 0.01970(17) 0.00095(12) -0.00106(13) 0.00078(13) N1 0.0246(12) 0.0274(12) 0.0201(11) -0.0025(9) 0.0008(9) -0.0069(10) C1A 0.0252(14) 0.0287(15) 0.0218(13) -0.0048(11) 0.0014(11) -0.0066(11) C2A 0.0310(16) 0.0445(18) 0.0243(15) -0.0049(13) 0.0046(12) -0.0120(14) N3A 0.0366(14) 0.0400(15) 0.0187(11) 0.0011(10) -0.0019(10) -0.0151(12) C3A 0.0295(15) 0.0334(16) 0.0273(15) -0.0045(12) -0.0024(12) -0.0025(12) C4A 0.0283(14) 0.0324(15) 0.0168(13) -0.0017(11) 0.0021(11) -0.0054(12) C5A 0.0270(14) 0.0309(15) 0.0228(14) -0.0027(11) 0.0062(11) 0.0024(12) C6A 0.0290(15) 0.0285(15) 0.0225(13) -0.0048(11) 0.0070(11) -0.0043(12) C7A 0.0262(14) 0.0329(15) 0.0182(13) -0.0018(11) 0.0032(11) -0.0041(12) C8A 0.0298(15) 0.0292(15) 0.0258(14) 0.0008(12) 0.0020(12) 0.0021(12) C9A 0.0351(16) 0.0267(15) 0.0253(14) -0.0013(11) 0.0013(12) -0.0049(12) C10A 0.0292(15) 0.0349(16) 0.0204(13) -0.0026(11) 0.0002(11) -0.0027(12) N4A 0.0234(11) 0.0248(12) 0.0210(11) 0.0003(9) -0.0024(9) -0.0009(9) C11A 0.0258(14) 0.0210(13) 0.0263(14) -0.0011(11) -0.0037(11) 0.0011(11) C12A 0.0240(13) 0.0217(13) 0.0259(14) 0.0020(11) -0.0030(11) -0.0050(11) C13A 0.072(3) 0.075(3) 0.0230(16) 0.0013(17) 0.0002(16) -0.043(2) C14A 0.0277(15) 0.0341(16) 0.0264(14) 0.0000(12) -0.0033(12) -0.0025(12) N2 0.0218(11) 0.0234(11) 0.0199(11) 0.0002(9) -0.0004(9) -0.0026(9) C1B 0.0240(14) 0.0388(17) 0.0255(14) -0.0049(12) 0.0043(11) -0.0102(12) C2B 0.0204(13) 0.0404(17) 0.0304(15) -0.0070(13) 0.0048(11) -0.0030(12) N3B 0.0211(11) 0.0319(13) 0.0249(12) -0.0034(10) -0.0010(9) -0.0052(10) C3B 0.0225(14) 0.0304(15) 0.0352(16) -0.0010(12) -0.0053(12) -0.0019(12) C4B 0.0219(13) 0.0238(14) 0.0275(14) 0.0008(11) -0.0016(11) -0.0007(11) C5B 0.0222(14) 0.0269(15) 0.0353(16) -0.0028(12) 0.0022(12) 0.0028(11) C6B 0.0278(14) 0.0234(14) 0.0261(14) -0.0050(11) 0.0010(11) 0.0020(11) C7B 0.0244(13) 0.0190(13) 0.0206(13) 0.0022(10) -0.0018(10) -0.0012(10) C8B 0.0221(13) 0.0243(14) 0.0228(13) 0.0005(11) 0.0014(10) -0.0010(11) C9B 0.0262(14) 0.0270(14) 0.0210(13) -0.0018(11) -0.0011(11) -0.0027(11) C10B 0.0254(14) 0.0304(15) 0.0223(13) -0.0006(11) -0.0020(11) -0.0040(12) N4B 0.0238(11) 0.0220(11) 0.0218(11) 0.0032(9) -0.0028(9) -0.0041(9) C11B 0.0243(14) 0.0237(14) 0.0254(14) 0.0021(11) -0.0047(11) -0.0036(11) C12B 0.0205(13) 0.0235(13) 0.0244(13) 0.0006(11) -0.0028(10) -0.0035(11) C13B 0.0247(14) 0.0418(18) 0.0328(16) -0.0046(13) -0.0082(12) -0.0074(13) C14B 0.0317(16) 0.0296(15) 0.0320(16) 0.0062(12) -0.0069(12) -0.0049(12) C1C 0.0357(16) 0.0249(14) 0.0255(14) 0.0008(11) -0.0003(12) -0.0090(12) C2C 0.0330(15) 0.0250(14) 0.0260(14) -0.0008(11) -0.0031(12) -0.0020(12) N3C 0.0267(12) 0.0285(13) 0.0221(11) -0.0037(9) 0.0008(9) -0.0026(10) C3C 0.0229(14) 0.0269(14) 0.0260(14) 0.0010(11) -0.0011(11) -0.0020(11) C4C 0.0235(13) 0.0228(13) 0.0255(14) -0.0007(11) -0.0021(11) -0.0030(11) C5C 0.0257(14) 0.0314(15) 0.0264(14) -0.0055(12) 0.0055(11) -0.0015(12) C6C 0.0268(14) 0.0311(15) 0.0227(14) -0.0036(11) -0.0028(11) -0.0020(12) C7C 0.0264(14) 0.0180(13) 0.0278(14) -0.0008(11) -0.0007(11) 0.0000(11) C8C 0.0259(14) 0.0237(14) 0.0308(15) -0.0061(11) 0.0036(11) 0.0007(11) C9C 0.0289(14) 0.0270(14) 0.0229(13) -0.0040(11) 0.0009(11) -0.0018(12) C10C 0.0268(14) 0.0222(14) 0.0296(14) -0.0025(11) -0.0010(11) 0.0039(11) N4C 0.0242(12) 0.0237(12) 0.0230(11) -0.0004(9) -0.0015(9) 0.0012(9) C11C 0.0315(15) 0.0293(15) 0.0211(13) -0.0001(11) 0.0030(11) 0.0001(12) C12C 0.0279(14) 0.0294(15) 0.0222(13) 0.0031(11) 0.0036(11) -0.0019(12) C13C 0.0338(16) 0.0386(17) 0.0318(16) -0.0134(13) 0.0021(13) 0.0002(13) C14C 0.0227(14) 0.0379(17) 0.0352(16) -0.0031(13) -0.0028(12) 0.0015(12) N11 0.0347(14) 0.0345(14) 0.0206(12) -0.0020(10) 0.0010(10) -0.0105(11) N12 0.0218(11) 0.0296(13) 0.0234(12) 0.0039(10) 0.0015(9) -0.0015(10) N13 0.0412(15) 0.0386(15) 0.0247(13) -0.0053(11) -0.0008(11) -0.0080(12) N21 0.0391(15) 0.0330(14) 0.0217(13) -0.0039(10) 0.0027(10) 0.0001(11) N22 0.0415(16) 0.0342(15) 0.051(2) 0.0093(13) 0.0019(13) 0.0029(12) N23 0.074(2) 0.053(2) 0.0361(17) 0.0108(14) 0.0050(15) 0.0010(17) Cl1 0.0315(4) 0.0265(4) 0.0313(4) -0.0012(3) 0.0062(3) -0.0014(3) O11 0.0396(13) 0.0369(12) 0.0380(12) 0.0103(10) 0.0069(10) 0.0061(10) O12 0.0693(18) 0.0402(14) 0.0635(17) 0.0128(13) 0.0174(14) 0.0227(13) O13 0.0718(19) 0.0682(18) 0.0331(13) -0.0139(12) 0.0118(13) -0.0098(15) O14 0.0476(16) 0.0625(18) 0.075(2) -0.0009(15) 0.0119(14) -0.0246(14) Cl2 0.0296(4) 0.0498(5) 0.0603(6) -0.0201(4) 0.0091(4) -0.0041(3) O21 0.0490(16) 0.0642(18) 0.093(2) -0.0317(17) 0.0341(16) -0.0086(14) O22 0.070(2) 0.071(2) 0.067(2) -0.0039(16) 0.0015(16) 0.0075(16) O23 0.0427(15) 0.0534(16) 0.078(2) -0.0125(14) 0.0076(14) 0.0045(12) O24 0.0381(15) 0.085(2) 0.084(2) -0.0334(18) 0.0111(14) -0.0171(14) O1S 0.084(6) 0.041(4) 0.032(4) -0.011(3) -0.018(4) 0.024(4) C1S 0.101(10) 0.011(7) 0.065(10) 0.004(6) -0.046(8) 0.012(6) C2S 0.063(8) 0.032(6) 0.057(8) 0.003(6) 0.021(7) -0.005(5) O1S' 0.046(6) 0.076(8) 0.061(8) 0.027(7) 0.012(6) 0.024(6) C1S' 0.083(10) 0.024(11) 0.040(10) 0.010(8) -0.013(9) -0.004(8) C2S' 0.026(7) 0.050(9) 0.054(10) 0.026(8) 0.000(7) 0.011(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N11 1.967(2) . y Cu1 N1 2.036(2) . y Cu1 N3B 2.079(2) . y Cu1 N3C 2.089(2) . y Cu1 N13 2.450(3) 3_465 y Cu2 N21 1.973(3) . y Cu2 N2 2.023(2) . y Cu2 N4A 2.071(2) . y Cu2 N4C 2.077(2) . y N1 C1C 1.484(4) . ? N1 C1A 1.490(3) . ? N1 C1B 1.492(4) . ? C1A C2A 1.531(4) . ? C2A N3A 1.474(4) . ? N3A C3A 1.462(4) . ? N3A C13A 1.465(4) . ? C3A C4A 1.516(4) . ? C4A C5A 1.392(4) . ? C4A C9A 1.393(4) . ? C5A C6A 1.386(4) . ? C6A C7A 1.398(4) . ? C7A C8A 1.395(4) . ? C7A C10A 1.509(4) . ? C8A C9A 1.388(4) . ? C10A N4A 1.501(4) . ? N4A C14A 1.493(3) . ? N4A C11A 1.497(3) . ? C11A C12A 1.512(4) . ? C12A N2 1.483(3) . ? N2 C12C 1.491(3) . ? N2 C12B 1.507(3) . ? C1B C2B 1.523(4) . ? C2B N3B 1.495(4) . ? N3B C13B 1.494(3) . ? N3B C3B 1.506(4) . ? C3B C4B 1.513(4) . ? C4B C5B 1.387(4) . ? C4B C9B 1.396(4) . ? C5B C6B 1.390(4) . ? C6B C7B 1.400(4) . ? C7B C8B 1.391(4) . ? C7B C10B 1.510(4) . ? C8B C9B 1.388(4) . ? C10B N4B 1.474(3) . ? N4B C14B 1.469(4) . ? N4B C11B 1.469(3) . ? C11B C12B 1.534(4) . ? C1C C2C 1.523(4) . ? C2C N3C 1.506(4) . ? N3C C13C 1.486(4) . ? N3C C3C 1.502(4) . ? C3C C4C 1.509(4) . ? C4C C9C 1.394(4) . ? C4C C5C 1.401(4) . ? C5C C6C 1.389(4) . ? C6C C7C 1.389(4) . ? C7C C8C 1.389(4) . ? C7C C10C 1.505(4) . ? C8C C9C 1.392(4) . ? C10C N4C 1.504(4) . ? N4C C14C 1.489(4) . ? N4C C11C 1.492(4) . ? C11C C12C 1.520(4) . ? N11 N12 1.179(3) . ? N12 N13 1.163(3) . ? N13 Cu1 2.450(3) 3_465 ? N21 N22 1.142(4) . ? N22 N23 1.183(4) . ? Cl1 O13 1.429(3) . ? Cl1 O11 1.429(2) . ? Cl1 O14 1.433(3) . ? Cl1 O12 1.435(3) . ? Cl2 O21 1.422(3) . ? Cl2 O24 1.427(3) . ? Cl2 O23 1.437(3) . ? Cl2 O22 1.450(3) . ? O1S C1S 1.267(16) . ? C1S C2S 1.331(16) . ? O1S' C1S' 1.24(2) . ? C1S' C2S' 1.34(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Cu1 N1 175.35(10) . . y N11 Cu1 N3B 94.69(10) . . y N1 Cu1 N3B 85.50(9) . . y N11 Cu1 N3C 95.48(10) . . y N1 Cu1 N3C 83.46(9) . . y N3B Cu1 N3C 164.89(9) . . y N11 Cu1 N13 90.29(9) . 3_465 y N1 Cu1 N13 94.28(9) . 3_465 y N3B Cu1 N13 98.38(9) . 3_465 y N3C Cu1 N13 92.72(9) . 3_465 y N21 Cu2 N2 175.36(10) . . y N21 Cu2 N4A 99.07(9) . . y N2 Cu2 N4A 85.44(9) . . y N21 Cu2 N4C 90.72(10) . . y N2 Cu2 N4C 85.23(9) . . y N4A Cu2 N4C 161.68(9) . . y C1C N1 C1A 111.6(2) . . ? C1C N1 C1B 114.2(2) . . ? C1A N1 C1B 111.9(2) . . ? C1C N1 Cu1 102.14(16) . . ? C1A N1 Cu1 114.78(17) . . ? C1B N1 Cu1 101.52(16) . . ? N1 C1A C2A 115.3(2) . . ? N3A C2A C1A 110.0(2) . . ? C3A N3A C13A 110.8(3) . . ? C3A N3A C2A 111.8(2) . . ? C13A N3A C2A 109.7(2) . . ? N3A C3A C4A 113.0(3) . . ? C5A C4A C9A 118.4(3) . . ? C5A C4A C3A 119.8(3) . . ? C9A C4A C3A 121.7(3) . . ? C6A C5A C4A 121.0(3) . . ? C5A C6A C7A 120.6(3) . . ? C8A C7A C6A 118.5(3) . . ? C8A C7A C10A 119.8(3) . . ? C6A C7A C10A 121.7(3) . . ? C9A C8A C7A 120.5(3) . . ? C8A C9A C4A 121.0(3) . . ? N4A C10A C7A 114.3(2) . . ? C14A N4A C11A 109.4(2) . . ? C14A N4A C10A 108.0(2) . . ? C11A N4A C10A 108.7(2) . . ? C14A N4A Cu2 103.99(17) . . ? C11A N4A Cu2 107.28(16) . . ? C10A N4A Cu2 119.26(17) . . ? N4A C11A C12A 109.3(2) . . ? N2 C12A C11A 108.4(2) . . ? C12A N2 C12C 111.5(2) . . ? C12A N2 C12B 113.0(2) . . ? C12C N2 C12B 112.8(2) . . ? C12A N2 Cu2 105.50(16) . . ? C12C N2 Cu2 107.74(17) . . ? C12B N2 Cu2 105.72(15) . . ? N1 C1B C2B 107.4(2) . . ? N3B C2B C1B 109.4(2) . . ? C13B N3B C2B 108.6(2) . . ? C13B N3B C3B 106.9(2) . . ? C2B N3B C3B 110.5(2) . . ? C13B N3B Cu1 109.13(18) . . ? C2B N3B Cu1 106.76(18) . . ? C3B N3B Cu1 114.87(17) . . ? N3B C3B C4B 114.7(2) . . ? C5B C4B C9B 117.7(2) . . ? C5B C4B C3B 123.2(3) . . ? C9B C4B C3B 119.1(3) . . ? C4B C5B C6B 121.3(3) . . ? C5B C6B C7B 120.7(3) . . ? C8B C7B C6B 118.1(2) . . ? C8B C7B C10B 121.0(2) . . ? C6B C7B C10B 120.8(2) . . ? C9B C8B C7B 120.7(3) . . ? C8B C9B C4B 121.4(3) . . ? N4B C10B C7B 113.1(2) . . ? C14B N4B C11B 109.3(2) . . ? C14B N4B C10B 109.1(2) . . ? C11B N4B C10B 112.1(2) . . ? N4B C11B C12B 111.1(2) . . ? N2 C12B C11B 115.3(2) . . ? N1 C1C C2C 109.0(2) . . ? N3C C2C C1C 110.5(2) . . ? C13C N3C C3C 110.1(2) . . ? C13C N3C C2C 109.5(2) . . ? C3C N3C C2C 113.7(2) . . ? C13C N3C Cu1 114.75(18) . . ? C3C N3C Cu1 100.51(16) . . ? C2C N3C Cu1 108.12(17) . . ? N3C C3C C4C 119.1(2) . . ? C9C C4C C5C 118.1(3) . . ? C9C C4C C3C 121.8(2) . . ? C5C C4C C3C 119.8(3) . . ? C6C C5C C4C 121.2(3) . . ? C7C C6C C5C 120.2(3) . . ? C6C C7C C8C 118.9(3) . . ? C6C C7C C10C 120.9(2) . . ? C8C C7C C10C 120.2(3) . . ? C7C C8C C9C 121.1(3) . . ? C8C C9C C4C 120.4(3) . . ? N4C C10C C7C 113.8(2) . . ? C14C N4C C11C 109.7(2) . . ? C14C N4C C10C 107.2(2) . . ? C11C N4C C10C 110.8(2) . . ? C14C N4C Cu2 101.29(17) . . ? C11C N4C Cu2 108.11(17) . . ? C10C N4C Cu2 119.04(17) . . ? N4C C11C C12C 110.2(2) . . ? N2 C12C C11C 109.1(2) . . ? N12 N11 Cu1 126.3(2) . . y N13 N12 N11 178.2(3) . . y N12 N13 Cu1 141.6(2) . 3_465 y N22 N21 Cu2 128.5(2) . . y N21 N22 N23 177.5(4) . . ?y O13 Cl1 O11 109.52(16) . . ? O13 Cl1 O14 109.44(17) . . ? O11 Cl1 O14 109.18(16) . . ? O13 Cl1 O12 109.94(18) . . ? O11 Cl1 O12 108.77(15) . . ? O14 Cl1 O12 109.97(18) . . ? O21 Cl2 O24 111.70(18) . . ? O21 Cl2 O23 110.42(18) . . ? O24 Cl2 O23 109.85(19) . . ? O21 Cl2 O22 108.1(2) . . ? O24 Cl2 O22 109.1(2) . . ? O23 Cl2 O22 107.55(19) . . ? O1S C1S C2S 116.0(16) . . ? O1S' C1S' C2S' 113(2) . . ? 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 O1S H1S N3A 0.84 1.95 2.717(8) 152.0 . O1S' H1S' O23 0.84 2.48 3.143(14) 136.0 3_566 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.975 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.090 data_Complex4(cumenco) _database_code_depnum_ccdc_archive 'CCDC 630228' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H74 Cl2 Cu2 N12 O11' _chemical_formula_weight 1193.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Aba2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/2, -y+1, z+1/2' '-x+1/2, y+1, z+1/2' _cell_length_a 22.370(3) _cell_length_b 15.246(2) _cell_length_c 17.260(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5886.4(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4706 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 23.37 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2504 _exptl_absorpt_coefficient_mu 0.877 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7547 _exptl_absorpt_correction_T_max 0.9412 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19817 _diffrn_reflns_av_R_equivalents 0.0928 _diffrn_reflns_av_sigmaI/netI 0.0989 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5130 _reflns_number_gt 3543 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1225P)^2^+18.6866P] 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' _refine_ls_abs_structure_Flack 0.06(4) _refine_ls_number_reflns 5130 _refine_ls_number_parameters 381 _refine_ls_number_restraints 691 _refine_ls_R_factor_all 0.1375 _refine_ls_R_factor_gt 0.0944 _refine_ls_wR_factor_ref 0.2450 _refine_ls_wR_factor_gt 0.2214 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.100 _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 0.87865(4) 0.73776(6) 0.60404(11) 0.0368(3) Uani 1 1 d U A . N1 N 0.8309(3) 0.6331(5) 0.5733(4) 0.0270(15) Uani 1 1 d U . . C1A C 0.7811(4) 0.6709(6) 0.5227(6) 0.035(2) Uani 1 1 d U . . H1A1 H 0.7589 0.6229 0.4969 0.042 Uiso 1 1 calc R . . H1A2 H 0.7526 0.7046 0.5551 0.042 Uiso 1 1 calc R . . C2A C 0.8092(4) 0.7301(6) 0.4630(6) 0.0346(19) Uani 1 1 d U . . H2A1 H 0.8319 0.6946 0.4250 0.042 Uiso 1 1 calc R . . H2A2 H 0.7776 0.7625 0.4347 0.042 Uiso 1 1 calc R . . N3A N 0.8505(3) 0.7940(5) 0.5025(5) 0.0374(17) Uani 1 1 d U . . C3A C 0.9014(4) 0.8230(7) 0.4500(6) 0.042(2) Uani 1 1 d U . . H3A1 H 0.8846 0.8516 0.4033 0.051 Uiso 1 1 calc R . . H3A2 H 0.9261 0.8669 0.4776 0.051 Uiso 1 1 calc R . . C4A C 0.9407(4) 0.7472(5) 0.4251(6) 0.0321(19) Uani 1 1 d U . . C5A C 0.9352(4) 0.7126(7) 0.3523(6) 0.039(2) Uani 1 1 d U . . H5A H 0.9065 0.7363 0.3175 0.047 Uiso 1 1 calc R . . C6A C 0.9711(4) 0.6432(7) 0.3287(6) 0.041(2) Uani 1 1 d U . . H6A H 0.9659 0.6184 0.2787 0.049 Uiso 1 1 calc R . . C7A C 1.0144(4) 0.6101(6) 0.3782(5) 0.0309(19) Uani 1 1 d U . . H7A H 1.0399 0.5641 0.3613 0.037 Uiso 1 1 calc R . . C8A C 1.0207(4) 0.6445(6) 0.4533(5) 0.0286(19) Uani 1 1 d U . . C9A C 0.9844(4) 0.7149(6) 0.4756(5) 0.0304(19) Uani 1 1 d U . . H9A H 0.9894 0.7409 0.5253 0.036 Uiso 1 1 calc R . . C10A C 1.0646(4) 0.6052(6) 0.5075(5) 0.031(2) Uani 1 1 d U . . H10A H 1.0457 0.5548 0.5341 0.037 Uiso 1 1 calc R . . H10B H 1.0751 0.6492 0.5474 0.037 Uiso 1 1 calc R . . N4A N 1.1204(3) 0.5748(5) 0.4688(4) 0.0267(16) Uani 1 1 d U . . C11A C 1.1568(4) 0.5229(5) 0.5219(5) 0.0267(18) Uani 1 1 d U . . H11A H 1.1582 0.5519 0.5732 0.032 Uiso 1 1 calc R . . H11B H 1.1982 0.5188 0.5019 0.032 Uiso 1 1 calc R . . C12A C 1.1304(3) 0.4305(6) 0.5304(6) 0.028(2) Uani 1 1 d U . . H12A H 1.0916 0.4351 0.5577 0.034 Uiso 1 1 calc R . . H12B H 1.1224 0.4067 0.4781 0.034 Uiso 1 1 calc R . . C13A C 0.8160(5) 0.8775(6) 0.5241(7) 0.045(2) Uani 1 1 d U . . H13A H 0.7830 0.8623 0.5590 0.050 Uiso 1 1 calc R . . H13B H 0.7999 0.9046 0.4770 0.050 Uiso 1 1 calc R . . H13C H 0.8430 0.9187 0.5501 0.050 Uiso 1 1 calc R . . C14A C 1.1550(4) 0.6547(6) 0.4451(6) 0.038(2) Uani 1 1 d U . . H14A H 1.1310 0.6897 0.4090 0.050 Uiso 1 1 calc R . . H14B H 1.1922 0.6367 0.4197 0.050 Uiso 1 1 calc R . . H14C H 1.1643 0.6899 0.4910 0.050 Uiso 1 1 calc R . . C1B C 0.8078(4) 0.5981(7) 0.6468(5) 0.034(2) Uani 1 1 d U . . H1B1 H 0.7861 0.5425 0.6376 0.041 Uiso 1 1 calc R . . H1B2 H 0.7798 0.6406 0.6706 0.041 Uiso 1 1 calc R . . C2B C 0.8608(4) 0.5826(7) 0.6998(5) 0.0300(19) Uani 1 1 d U . . H2B1 H 0.8468 0.5645 0.7518 0.036 Uiso 1 1 calc R . . H2B2 H 0.8866 0.5356 0.6785 0.036 Uiso 1 1 calc R . . N3B N 0.8953(3) 0.6676(5) 0.7051(4) 0.0306(16) Uani 1 1 d U . . C3B C 0.9613(4) 0.6520(6) 0.7103(5) 0.035(2) Uani 1 1 d U . . H3B1 H 0.9800 0.7052 0.7325 0.042 Uiso 1 1 calc R . . H3B2 H 0.9770 0.6449 0.6571 0.042 Uiso 1 1 calc R . . C4B C 0.9813(4) 0.5741(6) 0.7575(5) 0.0295(18) Uani 1 1 d U . . C5B C 0.9827(4) 0.5753(7) 0.8384(5) 0.039(2) Uani 1 1 d U . . H5B H 0.9720 0.6263 0.8667 0.047 Uiso 1 1 calc R . . C6B C 1.0000 0.5000 0.8751(8) 0.046(3) Uani 1 2 d SU . . H6B H 1.0000 0.5000 0.9301 0.055 Uiso 1 2 calc SR . . C9B C 1.0000 0.5000 0.7197(7) 0.029(3) Uani 1 2 d SU . . H9B H 1.0000 0.5000 0.6647 0.035 Uiso 1 2 calc SR . . C13B C 0.8738(5) 0.7156(8) 0.7731(7) 0.054(3) Uani 1 1 d U . . H13D H 0.8305 0.7246 0.7688 0.050 Uiso 1 1 calc R . . H13E H 0.8939 0.7726 0.7760 0.050 Uiso 1 1 calc R . . H13F H 0.8825 0.6817 0.8200 0.050 Uiso 1 1 calc R . . N21 N 0.9293(4) 0.8375(6) 0.6357(5) 0.046(2) Uani 1 1 d DU . . C22 C 0.9405(16) 0.8985(17) 0.653(2) 0.070(8) Uani 0.50 1 d PDU A 1 O23 O 0.9590(12) 0.9636(14) 0.6914(15) 0.104(7) Uani 0.50 1 d PDU A 1 C22' C 0.9258(14) 0.8880(14) 0.6732(13) 0.046(6) Uani 0.50 1 d PDU A 2 O23' O 0.9231(12) 0.9607(14) 0.7078(14) 0.103(7) Uani 0.50 1 d PDU A 2 Cl1 Cl 0.79476(14) 1.3206(2) 0.72506(17) 0.0594(8) Uani 1 1 d DU . . O11 O 0.7839(6) 1.3490(11) 0.7997(6) 0.158(5) Uani 1 1 d DU . . O12 O 0.8024(7) 1.2315(7) 0.7348(13) 0.203(8) Uani 1 1 d DU . . O13 O 0.8505(6) 1.3509(11) 0.7070(9) 0.173(7) Uani 1 1 d DU . . O14 O 0.7465(7) 1.3244(13) 0.6805(8) 0.208(8) Uani 1 1 d DU . . N31 N 0.7299(9) 1.0525(13) 0.8690(9) 0.117(5) Uani 1 1 d DU . . C32 C 0.769(2) 1.030(5) 0.829(4) 0.107(12) Uani 0.50 1 d PDU B 1 C33 C 0.8199(12) 1.013(3) 0.786(2) 0.084(8) Uani 0.50 1 d PDU B 1 H33A H 0.8296 1.0641 0.7540 0.050 Uiso 0.50 1 calc PR B 1 H33B H 0.8133 0.9619 0.7531 0.050 Uiso 0.50 1 calc PR B 1 H33C H 0.8532 1.0013 0.8217 0.050 Uiso 0.50 1 calc PR B 1 C32' C 0.7731(16) 1.050(4) 0.832(3) 0.081(8) Uani 0.50 1 d PDU B 2 C33' C 0.8264(17) 1.038(4) 0.794(3) 0.139(13) Uani 0.50 1 d PDU B 2 H33D H 0.8554 1.0122 0.8301 0.050 Uiso 0.50 1 calc PR B 2 H33E H 0.8415 1.0945 0.7755 0.050 Uiso 0.50 1 calc PR B 2 H33F H 0.8205 0.9983 0.7502 0.050 Uiso 0.50 1 calc PR B 2 O1W O 0.8994(13) 1.1422(19) 0.610(2) 0.080(8) Uiso 0.30 1 d PU C 1 O1W' O 0.8983(17) 1.111(2) 0.534(2) 0.052(9) Uiso 0.20 1 d PU D 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 0.0337(5) 0.0314(6) 0.0452(6) -0.0104(8) -0.0070(6) 0.0071(4) N1 0.017(3) 0.043(4) 0.021(3) -0.007(3) 0.002(3) 0.011(3) C1A 0.017(4) 0.048(5) 0.038(5) -0.007(4) 0.000(3) 0.013(3) C2A 0.021(4) 0.048(5) 0.034(5) -0.005(4) -0.003(3) 0.014(4) N3A 0.027(4) 0.034(4) 0.051(5) -0.007(3) -0.008(3) 0.015(3) C3A 0.041(5) 0.042(5) 0.043(5) 0.008(4) -0.006(4) 0.010(4) C4A 0.030(4) 0.026(5) 0.040(5) 0.011(4) 0.001(4) 0.002(3) C5A 0.022(4) 0.049(6) 0.047(5) 0.009(4) -0.004(4) 0.002(4) C6A 0.035(5) 0.065(7) 0.023(5) 0.000(4) -0.002(4) -0.002(4) C7A 0.026(5) 0.035(5) 0.032(4) 0.009(4) 0.006(4) 0.005(4) C8A 0.018(4) 0.033(5) 0.035(4) 0.013(4) -0.001(3) -0.002(3) C9A 0.028(4) 0.036(5) 0.027(5) 0.004(4) 0.002(3) 0.000(3) C10A 0.026(4) 0.036(5) 0.031(5) 0.016(4) 0.006(3) 0.004(3) N4A 0.021(3) 0.033(4) 0.026(4) 0.008(3) -0.004(3) -0.002(3) C11A 0.025(4) 0.031(4) 0.024(4) 0.002(4) -0.003(4) 0.003(4) C12A 0.013(4) 0.039(5) 0.032(5) 0.004(4) 0.006(4) 0.003(4) C13A 0.039(5) 0.035(5) 0.062(7) -0.005(5) -0.004(5) 0.010(4) C14A 0.025(5) 0.042(5) 0.046(6) 0.021(5) -0.007(4) -0.012(4) C1B 0.023(4) 0.048(5) 0.032(5) -0.013(4) 0.002(4) 0.010(4) C2B 0.030(4) 0.040(5) 0.020(4) -0.009(4) 0.007(4) 0.000(4) N3B 0.034(4) 0.036(4) 0.022(4) -0.016(3) 0.001(3) 0.004(3) C3B 0.036(4) 0.045(5) 0.022(5) -0.004(4) 0.001(4) -0.004(4) C4B 0.028(4) 0.039(5) 0.021(4) -0.006(4) -0.001(4) -0.010(4) C5B 0.055(6) 0.040(6) 0.023(4) 0.000(4) -0.002(4) -0.009(5) C6B 0.070(8) 0.050(7) 0.018(6) 0.000 0.000 -0.017(6) C9B 0.027(6) 0.045(6) 0.014(6) 0.000 0.000 -0.001(5) C13B 0.055(7) 0.058(7) 0.050(6) -0.027(5) 0.009(5) 0.006(5) N21 0.057(5) 0.041(4) 0.038(5) -0.003(4) -0.010(4) 0.007(4) C22 0.067(13) 0.065(9) 0.076(13) -0.007(10) 0.006(10) -0.025(9) O23 0.108(12) 0.096(10) 0.109(13) -0.031(9) -0.004(11) -0.033(10) C22' 0.062(12) 0.051(9) 0.024(10) 0.009(7) -0.004(9) -0.014(8) O23' 0.118(13) 0.090(10) 0.099(12) -0.036(9) -0.007(11) 0.006(10) Cl1 0.073(2) 0.0625(19) 0.0426(15) 0.0076(15) -0.0192(15) 0.0038(15) O11 0.148(12) 0.263(15) 0.061(6) -0.023(9) -0.008(6) 0.005(12) O12 0.167(13) 0.070(6) 0.37(2) -0.011(9) -0.127(14) -0.017(7) O13 0.172(10) 0.214(16) 0.132(11) 0.051(12) 0.039(8) -0.069(12) O14 0.204(12) 0.30(2) 0.117(11) 0.036(13) -0.117(11) 0.027(15) N31 0.150(13) 0.128(12) 0.075(10) 0.019(10) -0.022(8) -0.002(12) C32 0.118(18) 0.12(3) 0.080(19) 0.019(19) -0.023(14) -0.02(2) C33 0.080(11) 0.089(14) 0.083(13) 0.031(11) -0.034(9) -0.053(10) C32' 0.100(13) 0.09(2) 0.056(15) 0.010(16) -0.065(10) -0.030(17) C33' 0.137(15) 0.141(19) 0.139(17) 0.006(13) -0.009(12) -0.016(13) _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 N21 1.973(10) . ? Cu1 N1 1.993(8) . ? Cu1 N3A 2.051(8) . ? Cu1 N3B 2.079(8) . ? N1 C1B 1.470(11) . ? N1 C12A 1.495(11) 2_765 ? N1 C1A 1.528(11) . ? C1A C2A 1.509(14) . ? C2A N3A 1.506(12) . ? N3A C3A 1.521(13) . ? N3A C13A 1.534(12) . ? C3A C4A 1.514(13) . ? C4A C5A 1.369(14) . ? C4A C9A 1.398(12) . ? C5A C6A 1.389(14) . ? C6A C7A 1.388(12) . ? C7A C8A 1.405(13) . ? C8A C9A 1.401(12) . ? C8A C10A 1.482(12) . ? C10A N4A 1.489(10) . ? N4A C11A 1.461(10) . ? N4A C14A 1.500(11) . ? C11A C12A 1.534(13) . ? C12A N1 1.495(11) 2_765 ? C1B C2B 1.516(13) . ? C2B N3B 1.511(13) . ? N3B C13B 1.465(13) . ? N3B C3B 1.498(12) . ? C3B C4B 1.507(13) . ? C4B C9B 1.370(11) . ? C4B C5B 1.397(12) . ? C5B C6B 1.367(11) . ? C6B C5B 1.367(11) 2_765 ? C9B C4B 1.370(11) 2_765 ? N21 C22 1.009(18) . ? N21 C22' 1.009(17) . ? C22 O23 1.26(2) . ? C22' O23' 1.26(2) . ? Cl1 O14 1.328(10) . ? Cl1 O13 1.365(11) . ? Cl1 O12 1.379(11) . ? Cl1 O11 1.381(10) . ? N31 C32' 1.16(3) . ? N31 C32 1.17(3) . ? C32 C33 1.38(3) . ? C32' C33' 1.37(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N21 Cu1 N1 177.2(3) . . ? N21 Cu1 N3A 95.2(3) . . ? N1 Cu1 N3A 86.7(3) . . ? N21 Cu1 N3B 93.5(3) . . ? N1 Cu1 N3B 84.7(3) . . ? N3A Cu1 N3B 170.8(3) . . ? C1B N1 C12A 113.3(7) . 2_765 ? C1B N1 C1A 111.9(6) . . ? C12A N1 C1A 112.6(6) 2_765 . ? C1B N1 Cu1 104.4(5) . . ? C12A N1 Cu1 109.9(5) 2_765 . ? C1A N1 Cu1 103.9(6) . . ? C2A C1A N1 108.2(7) . . ? N3A C2A C1A 109.4(8) . . ? C2A N3A C3A 112.1(8) . . ? C2A N3A C13A 109.7(7) . . ? C3A N3A C13A 106.3(8) . . ? C2A N3A Cu1 107.8(6) . . ? C3A N3A Cu1 113.6(6) . . ? C13A N3A Cu1 107.1(6) . . ? C4A C3A N3A 112.5(8) . . ? C5A C4A C9A 120.1(8) . . ? C5A C4A C3A 120.0(8) . . ? C9A C4A C3A 119.8(9) . . ? C4A C5A C6A 120.6(9) . . ? C7A C6A C5A 120.1(9) . . ? C6A C7A C8A 120.1(8) . . ? C9A C8A C7A 118.9(8) . . ? C9A C8A C10A 121.3(8) . . ? C7A C8A C10A 119.8(8) . . ? C4A C9A C8A 120.2(9) . . ? C8A C10A N4A 113.5(7) . . ? C11A N4A C10A 110.8(7) . . ? C11A N4A C14A 108.9(6) . . ? C10A N4A C14A 107.6(7) . . ? N4A C11A C12A 110.0(7) . . ? N1 C12A C11A 114.8(7) 2_765 . ? N1 C1B C2B 107.6(7) . . ? N3B C2B C1B 107.6(8) . . ? C13B N3B C3B 110.8(7) . . ? C13B N3B C2B 108.0(8) . . ? C3B N3B C2B 111.8(7) . . ? C13B N3B Cu1 110.9(7) . . ? C3B N3B Cu1 108.0(5) . . ? C2B N3B Cu1 107.4(5) . . ? N3B C3B C4B 116.8(7) . . ? C9B C4B C5B 118.7(9) . . ? C9B C4B C3B 118.9(8) . . ? C5B C4B C3B 122.4(9) . . ? C6B C5B C4B 117.3(10) . . ? C5B C6B C5B 124.8(12) 2_765 . ? C4B C9B C4B 123.2(12) . 2_765 ? C22 N21 C22' 29(2) . . ? C22 N21 Cu1 159(2) . . ? C22' N21 Cu1 136.2(19) . . ? N21 C22 O23 164(4) . . ? N21 C22' O23' 168(3) . . ? O14 Cl1 O13 126.6(10) . . ? O14 Cl1 O12 102.3(10) . . ? O13 Cl1 O12 104.4(10) . . ? O14 Cl1 O11 112.6(10) . . ? O13 Cl1 O11 105.5(10) . . ? O12 Cl1 O11 102.6(11) . . ? C32' N31 C32 16(6) . . ? N31 C32 C33 172(7) . . ? N31 C32' C33' 172(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.764 _refine_diff_density_min -0.438 _refine_diff_density_rms 0.122 data_complex5(me6cusq) _database_code_depnum_ccdc_archive 'CCDC 630229' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H72 Cl2 Cu2 N10 O11' _chemical_formula_weight 1151.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9441(5) _cell_length_b 13.3353(6) _cell_length_c 18.3828(8) _cell_angle_alpha 106.3320(10) _cell_angle_beta 104.3400(10) _cell_angle_gamma 102.9450(10) _cell_volume 2582.92(19) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10393 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 23.23 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 0.995 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.851559 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22146 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 28.71 _reflns_number_total 11629 _reflns_number_gt 9407 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+0.4382P] 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 11629 _refine_ls_number_parameters 628 _refine_ls_number_restraints 245 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0898 _refine_ls_wR_factor_gt 0.0855 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.069 _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 0.40189(2) 0.779419(17) 0.329682(12) 0.02167(6) Uani 1 1 d U . . Cu2 Cu 0.59016(2) 1.090762(17) 0.298589(13) 0.02154(6) Uani 1 1 d U . . N1 N 0.39337(14) 0.64175(12) 0.24635(9) 0.0233(3) Uani 1 1 d U . . C1A C 0.48217(19) 0.67631(15) 0.20639(11) 0.0270(4) Uani 1 1 d U . . H1A1 H 0.5647 0.7072 0.2471 0.032 Uiso 1 1 calc R . . H1A2 H 0.4641 0.7366 0.1891 0.032 Uiso 1 1 calc R . . C2A C 0.4856(2) 0.58832(16) 0.13402(12) 0.0314(4) Uani 1 1 d U . . H2A1 H 0.4009 0.5467 0.0980 0.038 Uiso 1 1 calc R . . H2A2 H 0.5279 0.6253 0.1041 0.038 Uiso 1 1 calc R . . N3A N 0.54578(18) 0.50969(14) 0.15277(11) 0.0372(4) Uani 1 1 d U . . C13A C 0.5130(3) 0.41346(17) 0.07968(14) 0.0462(6) Uani 1 1 d U . . H13A H 0.4249 0.3766 0.0601 0.069 Uiso 1 1 calc R . . H13B H 0.5556 0.3622 0.0917 0.069 Uiso 1 1 calc R . . H13C H 0.5367 0.4372 0.0383 0.069 Uiso 1 1 calc R . . C3A C 0.6785(2) 0.55813(18) 0.19249(13) 0.0391(5) Uani 1 1 d U . . H3A1 H 0.7114 0.4992 0.2017 0.047 Uiso 1 1 calc R . . H3A2 H 0.6943 0.6133 0.2459 0.047 Uiso 1 1 calc R . . C4A C 0.7495(2) 0.61330(17) 0.14828(12) 0.0332(4) Uani 1 1 d U . . C5A C 0.7886(2) 0.55233(18) 0.08968(13) 0.0372(5) Uani 1 1 d U . . H5A H 0.7725 0.4754 0.0779 0.045 Uiso 1 1 calc R . . C6A C 0.8505(2) 0.60374(18) 0.04895(13) 0.0370(5) Uani 1 1 d U . . H6A H 0.8760 0.5616 0.0090 0.044 Uiso 1 1 calc R . . C7A C 0.87570(18) 0.71597(18) 0.06578(12) 0.0321(4) Uani 1 1 d U . . H7A H 0.9187 0.7502 0.0375 0.039 Uiso 1 1 calc R . . C8A C 0.83836(17) 0.77937(16) 0.12415(11) 0.0279(4) Uani 1 1 d U . . C9A C 0.77620(18) 0.72587(17) 0.16444(11) 0.0295(4) Uani 1 1 d U . . H9A H 0.7510 0.7680 0.2046 0.035 Uiso 1 1 calc R . . C10A C 0.86685(18) 0.90268(16) 0.14483(11) 0.0285(4) Uani 1 1 d U . . H10A H 0.8691 0.9354 0.2009 0.034 Uiso 1 1 calc R . . H10B H 0.9497 0.9324 0.1434 0.034 Uiso 1 1 calc R . . N4A N 0.78364(15) 0.94090(14) 0.09378(9) 0.0281(3) Uani 1 1 d U . . C14A C 0.7909(2) 0.9133(2) 0.01224(13) 0.0412(5) Uani 1 1 d U . . H14A H 0.8765 0.9347 0.0154 0.062 Uiso 1 1 calc R . . H14B H 0.7479 0.9529 -0.0162 0.062 Uiso 1 1 calc R . . H14C H 0.7532 0.8338 -0.0169 0.062 Uiso 1 1 calc R . . C11A C 0.65642(18) 0.90480(17) 0.08955(11) 0.0286(4) Uani 1 1 d U . . H11A H 0.6273 0.8233 0.0692 0.034 Uiso 1 1 calc R . . H11B H 0.6078 0.9285 0.0495 0.034 Uiso 1 1 calc R . . C12A C 0.63000(17) 0.94631(15) 0.16783(11) 0.0247(4) Uani 1 1 d U . . H12A H 0.5445 0.9056 0.1587 0.030 Uiso 1 1 calc R . . H12B H 0.6825 0.9264 0.2087 0.030 Uiso 1 1 calc R . . N2 N 0.64746(14) 1.06681(12) 0.20287(9) 0.0235(3) Uani 1 1 d U . . C1B C 0.26655(18) 0.59222(15) 0.18863(11) 0.0277(4) Uani 1 1 d U . . H1B1 H 0.2507 0.5130 0.1595 0.033 Uiso 1 1 calc R . . H1B2 H 0.2556 0.6291 0.1488 0.033 Uiso 1 1 calc R . . C2B C 0.17829(18) 0.60583(15) 0.23421(12) 0.0291(4) Uani 1 1 d U . . H2B1 H 0.0938 0.5755 0.1961 0.035 Uiso 1 1 calc R . . H2B2 H 0.1856 0.5649 0.2716 0.035 Uiso 1 1 calc R . . N3B N 0.20588(14) 0.72504(13) 0.28021(9) 0.0246(3) Uani 1 1 d U . . C13B C 0.1581(2) 0.73991(18) 0.34816(12) 0.0332(4) Uani 1 1 d U . . H13D H 0.0689 0.7125 0.3273 0.050 Uiso 1 1 calc R . . H13E H 0.1854 0.8183 0.3812 0.050 Uiso 1 1 calc R . . H13F H 0.1883 0.6988 0.3809 0.050 Uiso 1 1 calc R . . C3B C 0.14292(18) 0.77288(16) 0.22378(11) 0.0278(4) Uani 1 1 d U . . H3B1 H 0.0540 0.7421 0.2112 0.033 Uiso 1 1 calc R . . H3B2 H 0.1604 0.7480 0.1730 0.033 Uiso 1 1 calc R . . C4B C 0.17675(17) 0.89611(16) 0.25327(11) 0.0254(4) Uani 1 1 d U . . C5B C 0.12824(18) 0.95528(17) 0.30610(12) 0.0296(4) Uani 1 1 d U . . H5B H 0.0753 0.9175 0.3276 0.035 Uiso 1 1 calc R . . C6B C 0.15667(17) 1.06844(16) 0.32740(12) 0.0294(4) Uani 1 1 d U . . H6B H 0.1248 1.1079 0.3645 0.035 Uiso 1 1 calc R . . C7B C 0.23122(17) 1.12444(16) 0.29502(11) 0.0279(4) Uani 1 1 d U . . H7B H 0.2487 1.2018 0.3088 0.033 Uiso 1 1 calc R . . C8B C 0.28042(17) 1.06710(16) 0.24215(11) 0.0260(4) Uani 1 1 d U . . C9B C 0.25249(17) 0.95400(15) 0.22206(11) 0.0252(4) Uani 1 1 d U . . H9B H 0.2860 0.9149 0.1860 0.030 Uiso 1 1 calc R . . C10B C 0.35510(18) 1.12111(16) 0.20030(11) 0.0285(4) Uani 1 1 d U . . H10C H 0.3497 1.0638 0.1505 0.034 Uiso 1 1 calc R . . H10D H 0.3180 1.1742 0.1841 0.034 Uiso 1 1 calc R . . N4B N 0.48702(15) 1.18050(13) 0.24810(9) 0.0256(3) Uani 1 1 d U . . C14B C 0.4975(2) 1.28303(16) 0.31159(13) 0.0349(5) Uani 1 1 d U . . H14D H 0.4517 1.3247 0.2874 0.052 Uiso 1 1 calc R . . H14E H 0.5834 1.3279 0.3378 0.052 Uiso 1 1 calc R . . H14F H 0.4643 1.2643 0.3515 0.052 Uiso 1 1 calc R . . C11B C 0.5484(2) 1.20667(17) 0.19113(13) 0.0320(4) Uani 1 1 d U . . H11C H 0.6257 1.2678 0.2213 0.038 Uiso 1 1 calc R . . H11D H 0.4955 1.2303 0.1532 0.038 Uiso 1 1 calc R . . C12B C 0.57406(18) 1.10586(16) 0.14497(11) 0.0281(4) Uani 1 1 d U . . H12C H 0.4964 1.0469 0.1108 0.034 Uiso 1 1 calc R . . H12D H 0.6194 1.1243 0.1096 0.034 Uiso 1 1 calc R . . C1C C 0.42491(18) 0.56480(15) 0.28808(11) 0.0266(4) Uani 1 1 d U . . H1C1 H 0.4488 0.5081 0.2531 0.032 Uiso 1 1 calc R . . H1C2 H 0.3530 0.5271 0.2991 0.032 Uiso 1 1 calc R . . C2C C 0.52882(19) 0.62931(16) 0.36604(11) 0.0280(4) Uani 1 1 d U . . H2C1 H 0.5424 0.5807 0.3970 0.034 Uiso 1 1 calc R . . H2C2 H 0.6043 0.6560 0.3544 0.034 Uiso 1 1 calc R . . N3C N 0.50178(14) 0.72458(12) 0.41472(9) 0.0227(3) Uani 1 1 d U . . C13C C 0.41579(18) 0.68474(16) 0.45440(11) 0.0281(4) Uani 1 1 d U . . H13G H 0.4541 0.6517 0.4909 0.042 Uiso 1 1 calc R . . H13H H 0.3415 0.6295 0.4135 0.042 Uiso 1 1 calc R . . H13I H 0.3951 0.7468 0.4849 0.042 Uiso 1 1 calc R . . C3C C 0.61509(17) 0.80279(15) 0.48198(11) 0.0250(4) Uani 1 1 d U . . H3C1 H 0.5923 0.8595 0.5178 0.030 Uiso 1 1 calc R . . H3C2 H 0.6495 0.7615 0.5139 0.030 Uiso 1 1 calc R . . C4C C 0.71226(17) 0.85957(16) 0.45531(11) 0.0248(4) Uani 1 1 d U . . C5C C 0.79624(17) 0.81014(16) 0.43292(11) 0.0290(4) Uani 1 1 d U . . H5C H 0.7916 0.7382 0.4332 0.035 Uiso 1 1 calc R . . C6C C 0.88594(18) 0.86590(17) 0.41032(12) 0.0325(4) Uani 1 1 d U . . H6C H 0.9413 0.8312 0.3936 0.039 Uiso 1 1 calc R . . C7C C 0.89579(18) 0.97218(17) 0.41184(12) 0.0309(4) Uani 1 1 d U . . H7C H 0.9586 1.0101 0.3970 0.037 Uiso 1 1 calc R . . C8C C 0.81413(17) 1.02380(16) 0.43506(11) 0.0259(4) Uani 1 1 d U . . C9C C 0.72342(16) 0.96627(15) 0.45692(11) 0.0244(4) Uani 1 1 d U . . H9C H 0.6678 1.0008 0.4733 0.029 Uiso 1 1 calc R . . C10C C 0.82928(18) 1.14250(16) 0.44478(11) 0.0278(4) Uani 1 1 d U . . H10E H 0.7897 1.1718 0.4837 0.033 Uiso 1 1 calc R . . H10F H 0.9173 1.1842 0.4689 0.033 Uiso 1 1 calc R . . N4C N 0.77964(14) 1.16568(12) 0.37044(9) 0.0239(3) Uani 1 1 d U . . C14C C 0.80413(19) 1.28717(15) 0.39782(12) 0.0322(4) Uani 1 1 d U . . H14G H 0.7605 1.3085 0.4353 0.048 Uiso 1 1 calc R . . H14H H 0.7762 1.3084 0.3513 0.048 Uiso 1 1 calc R . . H14I H 0.8918 1.3245 0.4249 0.048 Uiso 1 1 calc R . . C11C C 0.84402(17) 1.13242(16) 0.31275(11) 0.0274(4) Uani 1 1 d U . . H11E H 0.8474 1.0571 0.3066 0.033 Uiso 1 1 calc R . . H11F H 0.9286 1.1831 0.3338 0.033 Uiso 1 1 calc R . . C12C C 0.77865(17) 1.13528(16) 0.23186(11) 0.0275(4) Uani 1 1 d U . . H12E H 0.7845 1.2122 0.2366 0.033 Uiso 1 1 calc R . . H12F H 0.8178 1.1066 0.1925 0.033 Uiso 1 1 calc R . . C1 C 0.48204(15) 0.97866(14) 0.36023(10) 0.0197(3) Uani 1 1 d U . . O1 O 0.49959(11) 0.92211(10) 0.29656(7) 0.0229(3) Uani 1 1 d U . . O2 O 0.42701(11) 0.92824(10) 0.39725(7) 0.0227(3) Uani 1 1 d U . . O3 O 0.52344(11) 1.08456(10) 0.38379(7) 0.0226(3) Uani 1 1 d U . . Cl1 Cl 0.26077(5) 0.77441(4) 0.00506(3) 0.03673(12) Uani 1 1 d DU . . O11 O 0.24665(18) 0.72213(14) -0.07752(9) 0.0522(4) Uani 1 1 d DU . . O12 O 0.3292(2) 0.88691(15) 0.03116(12) 0.0734(6) Uani 1 1 d DU . . O13 O 0.3261(3) 0.7276(2) 0.05443(13) 0.1058(10) Uani 1 1 d DU . . O14 O 0.1477(2) 0.7652(3) 0.01395(15) 0.1429(15) Uani 1 1 d DU . . Cl2 Cl 0.21357(5) 0.41744(4) 0.43046(4) 0.04181(13) Uani 0.60 1 d PDU A 1 O21 O 0.13270(18) 0.31524(14) 0.42177(13) 0.0637(5) Uani 0.60 1 d PDU A 1 O22 O 0.2827(7) 0.4706(5) 0.5133(3) 0.126(3) Uani 0.60 1 d PDU A 1 O23 O 0.2826(9) 0.4062(4) 0.3832(6) 0.151(4) Uani 0.60 1 d PDU A 1 O24 O 0.1529(4) 0.4939(4) 0.4179(5) 0.1035(19) Uani 0.60 1 d PDU A 1 Cl2' Cl 0.21357(5) 0.41744(4) 0.43046(4) 0.04181(13) Uani 0.40 1 d PDU B 2 O21' O 0.13270(18) 0.31524(14) 0.42177(13) 0.0637(5) Uani 0.40 1 d PDU B 2 O22' O 0.2258(13) 0.5004(5) 0.4914(7) 0.148(5) Uani 0.40 1 d PDU B 2 O23' O 0.3286(6) 0.4048(7) 0.4337(7) 0.099(4) Uani 0.40 1 d PDU B 2 O24' O 0.1795(9) 0.4372(9) 0.3586(5) 0.120(3) Uani 0.40 1 d PDU B 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 0.02922(12) 0.01783(11) 0.01821(11) 0.00535(8) 0.00932(9) 0.00765(9) Cu2 0.02723(12) 0.02017(11) 0.02036(11) 0.00792(9) 0.01129(9) 0.00868(9) N1 0.0315(8) 0.0196(7) 0.0187(7) 0.0059(6) 0.0099(6) 0.0078(6) C1A 0.0384(11) 0.0211(9) 0.0238(9) 0.0080(7) 0.0149(8) 0.0088(8) C2A 0.0450(12) 0.0268(10) 0.0244(10) 0.0063(8) 0.0175(9) 0.0119(9) N3A 0.0610(12) 0.0243(8) 0.0345(10) 0.0104(7) 0.0275(9) 0.0162(8) C13A 0.0785(18) 0.0239(10) 0.0415(13) 0.0063(9) 0.0356(13) 0.0158(11) C3A 0.0618(15) 0.0358(11) 0.0341(11) 0.0174(9) 0.0239(11) 0.0275(11) C4A 0.0433(12) 0.0346(11) 0.0286(10) 0.0125(9) 0.0145(9) 0.0209(10) C5A 0.0485(13) 0.0336(11) 0.0344(11) 0.0097(9) 0.0163(10) 0.0220(10) C6A 0.0421(12) 0.0414(12) 0.0282(11) 0.0049(9) 0.0145(9) 0.0210(10) C7A 0.0321(10) 0.0419(11) 0.0257(10) 0.0106(9) 0.0127(8) 0.0163(9) C8A 0.0281(10) 0.0324(10) 0.0230(9) 0.0072(8) 0.0073(8) 0.0141(8) C9A 0.0361(11) 0.0353(10) 0.0212(9) 0.0083(8) 0.0109(8) 0.0195(9) C10A 0.0274(10) 0.0338(10) 0.0243(9) 0.0080(8) 0.0095(8) 0.0117(8) N4A 0.0341(9) 0.0353(9) 0.0220(8) 0.0132(7) 0.0138(7) 0.0151(7) C14A 0.0584(14) 0.0502(14) 0.0294(11) 0.0178(10) 0.0249(10) 0.0279(12) C11A 0.0314(10) 0.0326(10) 0.0199(9) 0.0058(8) 0.0069(8) 0.0128(8) C12A 0.0264(9) 0.0232(9) 0.0245(9) 0.0068(7) 0.0106(7) 0.0076(7) N2 0.0264(8) 0.0233(8) 0.0218(7) 0.0086(6) 0.0102(6) 0.0064(6) C1B 0.0344(10) 0.0207(9) 0.0227(9) 0.0051(7) 0.0059(8) 0.0061(8) C2B 0.0310(10) 0.0216(9) 0.0287(10) 0.0069(8) 0.0065(8) 0.0033(8) N3B 0.0282(8) 0.0238(8) 0.0217(8) 0.0083(6) 0.0085(6) 0.0074(6) C13B 0.0381(11) 0.0369(11) 0.0295(10) 0.0132(9) 0.0156(9) 0.0144(9) C3B 0.0278(10) 0.0283(10) 0.0239(9) 0.0068(8) 0.0048(8) 0.0100(8) C4B 0.0254(9) 0.0275(9) 0.0209(9) 0.0074(7) 0.0028(7) 0.0111(8) C5B 0.0264(10) 0.0352(11) 0.0285(10) 0.0114(8) 0.0097(8) 0.0113(8) C6B 0.0281(10) 0.0331(10) 0.0274(10) 0.0065(8) 0.0097(8) 0.0154(8) C7B 0.0280(10) 0.0259(9) 0.0279(10) 0.0071(8) 0.0062(8) 0.0117(8) C8B 0.0265(9) 0.0277(9) 0.0234(9) 0.0091(8) 0.0057(7) 0.0107(8) C9B 0.0276(9) 0.0297(10) 0.0198(9) 0.0077(7) 0.0069(7) 0.0146(8) C10B 0.0335(10) 0.0323(10) 0.0257(10) 0.0136(8) 0.0108(8) 0.0164(8) N4B 0.0327(8) 0.0220(8) 0.0268(8) 0.0111(6) 0.0130(7) 0.0110(7) C14B 0.0437(12) 0.0247(10) 0.0383(12) 0.0088(9) 0.0156(10) 0.0152(9) C11B 0.0414(12) 0.0304(10) 0.0360(11) 0.0212(9) 0.0193(9) 0.0142(9) C12B 0.0353(10) 0.0315(10) 0.0254(9) 0.0158(8) 0.0143(8) 0.0131(8) C1C 0.0411(11) 0.0194(8) 0.0227(9) 0.0088(7) 0.0127(8) 0.0120(8) C2C 0.0391(11) 0.0255(9) 0.0236(9) 0.0083(8) 0.0122(8) 0.0165(8) N3C 0.0294(8) 0.0204(7) 0.0198(7) 0.0073(6) 0.0107(6) 0.0075(6) C13C 0.0354(11) 0.0268(9) 0.0246(9) 0.0117(8) 0.0130(8) 0.0077(8) C3C 0.0287(9) 0.0271(9) 0.0186(9) 0.0070(7) 0.0073(7) 0.0100(8) C4C 0.0248(9) 0.0286(9) 0.0187(8) 0.0064(7) 0.0051(7) 0.0089(8) C5C 0.0287(10) 0.0308(10) 0.0283(10) 0.0105(8) 0.0079(8) 0.0127(8) C6C 0.0296(10) 0.0363(11) 0.0347(11) 0.0100(9) 0.0134(9) 0.0169(9) C7C 0.0246(10) 0.0379(11) 0.0311(10) 0.0131(9) 0.0110(8) 0.0090(8) C8C 0.0259(9) 0.0283(10) 0.0203(9) 0.0067(8) 0.0045(7) 0.0088(8) C9C 0.0239(9) 0.0290(9) 0.0202(9) 0.0065(7) 0.0074(7) 0.0110(8) C10C 0.0290(10) 0.0271(9) 0.0210(9) 0.0044(8) 0.0059(7) 0.0052(8) N4C 0.0277(8) 0.0212(7) 0.0222(8) 0.0056(6) 0.0107(6) 0.0064(6) C14C 0.0399(11) 0.0230(9) 0.0301(10) 0.0055(8) 0.0138(9) 0.0059(8) C11C 0.0246(9) 0.0282(10) 0.0263(9) 0.0051(8) 0.0110(8) 0.0056(8) C12C 0.0292(10) 0.0253(9) 0.0272(10) 0.0075(8) 0.0150(8) 0.0036(8) C1 0.0195(8) 0.0220(8) 0.0182(8) 0.0071(7) 0.0056(7) 0.0086(7) O1 0.0291(7) 0.0213(6) 0.0198(6) 0.0059(5) 0.0110(5) 0.0092(5) O2 0.0284(7) 0.0198(6) 0.0212(6) 0.0065(5) 0.0118(5) 0.0075(5) O3 0.0289(7) 0.0179(6) 0.0215(6) 0.0049(5) 0.0116(5) 0.0072(5) Cl1 0.0481(3) 0.0324(3) 0.0289(3) 0.0107(2) 0.0142(2) 0.0101(2) O11 0.0848(13) 0.0429(9) 0.0333(9) 0.0137(7) 0.0245(9) 0.0226(9) O12 0.1010(17) 0.0367(10) 0.0576(12) 0.0088(9) 0.0084(12) 0.0058(10) O13 0.195(3) 0.0713(15) 0.0531(13) 0.0347(12) 0.0116(16) 0.0622(18) O14 0.0521(14) 0.255(4) 0.0617(15) -0.002(2) 0.0321(12) -0.0043(18) Cl2 0.0482(3) 0.0271(2) 0.0504(3) 0.0163(2) 0.0174(3) 0.0081(2) O21 0.0641(12) 0.0341(9) 0.0855(14) 0.0197(9) 0.0303(11) -0.0023(8) O22 0.148(5) 0.082(4) 0.074(3) 0.028(3) -0.035(3) -0.020(3) O23 0.248(9) 0.033(2) 0.207(8) 0.006(4) 0.208(8) 0.010(5) O24 0.078(3) 0.070(3) 0.184(6) 0.075(4) 0.032(4) 0.036(2) Cl2' 0.0482(3) 0.0271(2) 0.0504(3) 0.0163(2) 0.0174(3) 0.0081(2) O21' 0.0641(12) 0.0341(9) 0.0855(14) 0.0197(9) 0.0303(11) -0.0023(8) O22' 0.256(14) 0.029(3) 0.169(8) -0.017(5) 0.190(10) -0.002(6) O23' 0.033(3) 0.057(4) 0.203(11) 0.048(6) 0.030(4) 0.015(2) O24' 0.112(7) 0.130(8) 0.084(5) 0.079(5) -0.021(5) -0.014(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 O2 1.9323(12) . y Cu1 N1 1.9962(15) . y Cu1 N3C 2.1241(15) . y Cu1 N3B 2.1558(16) . y Cu1 O1 2.3156(12) . y Cu2 O3 1.9382(12) . y Cu2 N2 2.0111(15) . y Cu2 N4B 2.1284(16) . y Cu2 N4C 2.1515(16) . y Cu2 O1 2.2522(12) . y N1 C1B 1.489(2) . ? N1 C1A 1.495(2) . ? N1 C1C 1.502(2) . ? C1A C2A 1.523(2) . ? C2A N3A 1.468(3) . ? N3A C13A 1.466(3) . ? N3A C3A 1.472(3) . ? C3A C4A 1.523(3) . ? C4A C9A 1.390(3) . ? C4A C5A 1.402(3) . ? C5A C6A 1.383(3) . ? C6A C7A 1.385(3) . ? C7A C8A 1.400(3) . ? C8A C9A 1.393(3) . ? C8A C10A 1.516(3) . ? C10A N4A 1.470(2) . ? N4A C11A 1.463(2) . ? N4A C14A 1.469(2) . ? C11A C12A 1.527(2) . ? C12A N2 1.497(2) . ? N2 C12B 1.492(2) . ? N2 C12C 1.498(2) . ? C1B C2B 1.511(3) . ? C2B N3B 1.491(2) . ? N3B C13B 1.480(2) . ? N3B C3B 1.500(2) . ? C3B C4B 1.500(3) . ? C4B C9B 1.392(3) . ? C4B C5B 1.398(3) . ? C5B C6B 1.385(3) . ? C6B C7B 1.385(3) . ? C7B C8B 1.393(3) . ? C8B C9B 1.387(3) . ? C8B C10B 1.507(3) . ? C10B N4B 1.499(3) . ? N4B C14B 1.484(2) . ? N4B C11B 1.493(2) . ? C11B C12B 1.514(3) . ? C1C C2C 1.511(3) . ? C2C N3C 1.486(2) . ? N3C C13C 1.488(2) . ? N3C C3C 1.504(2) . ? C3C C4C 1.503(3) . ? C4C C9C 1.390(3) . ? C4C C5C 1.399(3) . ? C5C C6C 1.382(3) . ? C6C C7C 1.387(3) . ? C7C C8C 1.396(3) . ? C8C C9C 1.393(3) . ? C8C C10C 1.505(3) . ? C10C N4C 1.494(2) . ? N4C C11C 1.485(2) . ? N4C C14C 1.490(2) . ? C11C C12C 1.514(3) . ? C1 O2 1.276(2) . ? C1 O3 1.290(2) . ? C1 O1 1.296(2) . ? Cl1 O14 1.383(2) . ? Cl1 O12 1.4142(19) . ? Cl1 O13 1.418(2) . ? Cl1 O11 1.4297(16) . ? Cl2 O23 1.340(4) . ? Cl2 O24 1.413(4) . ? Cl2 O22 1.419(5) . ? Cl2 O21 1.4238(17) . ? 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 O2 Cu1 N1 167.57(6) . . y O2 Cu1 N3C 100.29(5) . . y N1 Cu1 N3C 86.15(6) . . y O2 Cu1 N3B 98.74(6) . . y N1 Cu1 N3B 86.13(6) . . y N3C Cu1 N3B 124.10(6) . . y O2 Cu1 O1 62.23(5) . . y N1 Cu1 O1 105.34(5) . . y N3C Cu1 O1 120.58(5) . . y N3B Cu1 O1 114.86(5) . . y O3 Cu2 N2 169.46(6) . . y O3 Cu2 N4B 98.84(6) . . y N2 Cu2 N4B 86.45(6) . . y O3 Cu2 N4C 98.60(5) . . y N2 Cu2 N4C 86.16(6) . . y N4B Cu2 N4C 121.75(6) . . y O3 Cu2 O1 63.17(5) . . y N2 Cu2 O1 106.28(5) . . y N4B Cu2 O1 121.28(5) . . y N4C Cu2 O1 116.23(5) . . y C1B N1 C1A 111.45(14) . . ? C1B N1 C1C 110.30(14) . . ? C1A N1 C1C 112.97(14) . . ? C1B N1 Cu1 108.03(11) . . ? C1A N1 Cu1 105.98(10) . . ? C1C N1 Cu1 107.84(11) . . ? N1 C1A C2A 117.23(15) . . ? N3A C2A C1A 115.28(17) . . ? C13A N3A C2A 109.45(18) . . ? C13A N3A C3A 112.09(18) . . ? C2A N3A C3A 113.75(16) . . ? N3A C3A C4A 116.63(18) . . ? C9A C4A C5A 118.1(2) . . ? C9A C4A C3A 120.65(18) . . ? C5A C4A C3A 121.25(19) . . ? C6A C5A C4A 120.3(2) . . ? C5A C6A C7A 120.69(19) . . ? C6A C7A C8A 120.5(2) . . ? C9A C8A C7A 117.82(19) . . ? C9A C8A C10A 120.60(17) . . ? C7A C8A C10A 121.56(18) . . ? C4A C9A C8A 122.62(18) . . ? N4A C10A C8A 117.31(16) . . ? C11A N4A C14A 109.79(16) . . ? C11A N4A C10A 115.20(15) . . ? C14A N4A C10A 112.01(16) . . ? N4A C11A C12A 116.54(16) . . ? N2 C12A C11A 117.74(15) . . ? C12B N2 C12A 112.11(14) . . ? C12B N2 C12C 109.46(14) . . ? C12A N2 C12C 112.18(14) . . ? C12B N2 Cu2 107.94(11) . . ? C12A N2 Cu2 107.41(10) . . ? C12C N2 Cu2 107.53(11) . . ? N1 C1B C2B 109.21(15) . . ? N3B C2B C1B 109.34(15) . . ? C13B N3B C2B 110.82(15) . . ? C13B N3B C3B 108.53(15) . . ? C2B N3B C3B 107.28(14) . . ? C13B N3B Cu1 107.68(12) . . ? C2B N3B Cu1 101.90(11) . . ? C3B N3B Cu1 120.37(11) . . ? N3B C3B C4B 116.05(15) . . ? C9B C4B C5B 118.07(18) . . ? C9B C4B C3B 118.74(17) . . ? C5B C4B C3B 123.01(18) . . ? C6B C5B C4B 120.60(19) . . ? C5B C6B C7B 120.46(18) . . ? C6B C7B C8B 119.89(18) . . ? C9B C8B C7B 119.10(18) . . ? C9B C8B C10B 117.92(17) . . ? C7B C8B C10B 122.80(17) . . ? C8B C9B C4B 121.87(17) . . ? N4B C10B C8B 115.92(15) . . ? C14B N4B C11B 110.61(15) . . ? C14B N4B C10B 108.91(15) . . ? C11B N4B C10B 107.02(15) . . ? C14B N4B Cu2 110.22(12) . . ? C11B N4B Cu2 102.33(11) . . ? C10B N4B Cu2 117.47(11) . . ? N4B C11B C12B 109.71(15) . . ? N2 C12B C11B 109.29(15) . . ? N1 C1C C2C 109.44(15) . . ? N3C C2C C1C 110.74(15) . . ? C2C N3C C13C 109.08(14) . . ? C2C N3C C3C 110.42(14) . . ? C13C N3C C3C 105.56(14) . . ? C2C N3C Cu1 105.10(11) . . ? C13C N3C Cu1 105.47(11) . . ? C3C N3C Cu1 120.77(11) . . ? C4C C3C N3C 114.66(14) . . ? C9C C4C C5C 118.90(18) . . ? C9C C4C C3C 119.31(16) . . ? C5C C4C C3C 121.70(17) . . ? C6C C5C C4C 120.03(19) . . ? C5C C6C C7C 120.49(18) . . ? C6C C7C C8C 120.51(18) . . ? C9C C8C C7C 118.41(18) . . ? C9C C8C C10C 119.53(17) . . ? C7C C8C C10C 121.77(18) . . ? C4C C9C C8C 121.63(17) . . ? N4C C10C C8C 116.84(15) . . ? C11C N4C C14C 109.83(15) . . ? C11C N4C C10C 110.31(15) . . ? C14C N4C C10C 105.27(14) . . ? C11C N4C Cu2 103.66(11) . . ? C14C N4C Cu2 107.01(12) . . ? C10C N4C Cu2 120.53(11) . . ? N4C C11C C12C 110.29(15) . . ? N2 C12C C11C 110.07(15) . . ? O2 C1 O3 123.09(15) . . ? O2 C1 O1 119.33(15) . . ? O3 C1 O1 117.57(15) . . ? C1 O1 Cu2 82.60(10) . . ? C1 O1 Cu1 80.46(10) . . ? Cu2 O1 Cu1 163.01(6) . . y C1 O2 Cu1 97.97(10) . . ? C1 O3 Cu2 96.65(10) . . ? O14 Cl1 O12 109.7(2) . . ? O14 Cl1 O13 109.8(2) . . ? O12 Cl1 O13 107.04(15) . . ? O14 Cl1 O11 109.86(13) . . ? O12 Cl1 O11 109.23(12) . . ? O13 Cl1 O11 111.20(13) . . ? O23 Cl2 O24 109.5(4) . . ? O23 Cl2 O22 113.2(5) . . ? O24 Cl2 O22 100.6(4) . . ? O23 Cl2 O21 113.2(2) . . ? O24 Cl2 O21 112.8(2) . . ? O22 Cl2 O21 107.0(3) . . ? _diffrn_measured_fraction_theta_max 0.871 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.569 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.057 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.005 0.365 0.229 153.1 42.5 2 -0.006 0.635 0.771 152.5 42.6 3 0.103 0.942 0.068 5.3 -0.1 4 0.897 0.057 0.932 5.6 -0.1 _platon_squeeze_details ; interpereted as 2CH3CN per asymmetric unit. ; # END