# Copyright The Royal Society of Chemistry, 1998 data_8/02076K _audit_creation_date 98-04-13 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_sum C15_H30_N6_O3_S3_Cu2_Pb1 _chemical_formula_weight 772.93 _chemical_melting_point ? _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution xtal _computing_structure_refinement xtal_CRYLSQ _computing_molecular_graphics xtal _computing_publication_material xtal_BONDLA_CIFIO _cell_length_a 14.57860(10) _cell_length_b 17.4145(2) _cell_length_c 10.51940(10) _cell_angle_alpha 90.00000 _cell_angle_beta 105.108(10) _cell_angle_gamma 90.00000 _cell_volume 2578.35(13) _cell_formula_units_Z 4 _cell_measurement_temperature 203 _cell_measurement_reflns_used 16563 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.2 _cell_special_details ; _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _exptl_crystal_description fragment _exptl_crystal_preparation ? _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.991 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 1496 _exptl_absorpt_process_details ? _exptl_absorpt_coefficient_mu 9.22 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.236 _exptl_absorpt_correction_T_max 0.431 _exptl_special_details _diffrn_special_details ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'Siemens SMART' _diffrn_measurement_method 'Area detector' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 16056 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 28.23 _diffrn_reflns_reduction_process ? loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 60 .002 .002 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 120 0 0 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 N ? 0 24 .004 .003 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 O ? 0 12 .008 .006 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 S ? 0 12 .11 .124 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 Cu ? 0 8 .263 1.266 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 Pb ? 0 4 -4.133 10.102 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Cu1 .18465(10) .97588(7) .36106(12) .0297(6) Uani ? ? Cu2 .37626(12) .96311(8) .27094(13) .0370(7) Uani ? ? Pb .17397(3) 1.01823(2) .05273(3) .0289(2) Uani ? ? S1 -.1157(3) 1.12573(18) .1504(3) .0468(16) Uani ? ? S2 .2157(3) 1.09405(18) .7725(3) .0464(16) Uani ? ? S3 .4681(4) .9198(3) .7168(4) .079(3) Uani ? ? O1 .1958(6) .9140(4) .2128(7) .037(4) Uani ? ? O2 .2660(6) 1.0430(4) .2805(7) .035(4) Uani ? ? O3 .3300(6) .9926(5) .0781(7) .036(4) Uani ? ? N1 .0478(10) 1.0369(7) .2414(11) .060(7) Uani ? ? N2 .2003(8) 1.0293(6) .5260(9) .042(5) Uani ? ? N3 .4016(10) .9411(7) .4448(12) .068(8) Uani ? ? N4 .1167(7) .8834(5) .4109(9) .035(5) Uani ? ? N5 .2108(7) 1.1686(5) .0997(8) .034(5) Uani ? ? N6 .4413(10) .8789(8) .2041(14) .075(9) Uani ? ? C1 -.0184(8) 1.0754(6) .2020(10) .032(5) Uani ? ? C2 .2087(8) 1.0549(6) .6316(10) .030(5) Uani ? ? C3 .4303(11) .9321(9) .5623(13) .059(8) Uani ? ? C4 .1464(13) .8435(7) .2028(13) .061(8) Uani ? ? C5 .0735(10) .8475(7) .2832(12) .048(7) Uani ? ? C6 .1896(11) .8354(7) .5016(12) .051(7) Uani ? ? C7 .0429(12) .9039(11) .4772(13) .068(10) Uani ? ? C8 .2863(10) 1.1210(6) .3255(10) .042(6) Uani ? ? C9 .2200(10) 1.1749(6) .2411(11) .042(6) Uani ? ? C10 .1329(12) 1.2124(8) .0254(13) .057(8) Uani ? ? C11 .2976(10) 1.1947(7) .0713(11) .045(6) Uani ? ? C12 .3608(10) .9418(8) -.0052(13) .051(7) Uani ? ? C13 .456(3) .907(2) .083(2) .20(3) Uani ? ? C14 .387(2) .8077(13) .208(4) .16(2) Uani ? ? C15 .5398(16) .8733(14) .282(3) .14(2) Uani ? ? H4A .19010 .80286 .23492 .07400 Uiso ? ? H4B .11469 .83363 .11295 .07400 Uiso ? ? H5A .05313 .79678 .29787 .05900 Uiso ? ? H5B .02017 .87664 .23772 .05900 Uiso ? ? H6A .16976 .78957 .52347 .07500 Uiso ? ? H6B .21726 .86294 .57964 .07500 Uiso ? ? H6C .23776 .82119 .45967 .07500 Uiso ? ? H7A .07074 .93050 .55561 .10000 Uiso ? ? H7B .01319 .85815 .49648 .10000 Uiso ? ? H7C -.00360 .93529 .42017 .10000 Uiso ? ? H8A .35019 1.13346 .32411 .05400 Uiso ? ? H8B .28172 1.12508 .41411 .05400 Uiso ? ? H9A .24061 1.22585 .26723 .05300 Uiso ? ? H9B .15900 1.16693 .25535 .05300 Uiso ? ? H10A .12464 1.20413 -.06613 .08400 Uiso ? ? H10B .14329 1.26553 .04451 .08400 Uiso ? ? H10C .07571 1.19717 .04783 .08400 Uiso ? ? H11A .29186 1.19202 -.02031 .06900 Uiso ? ? H11B .34921 1.16213 .11622 .06900 Uiso ? ? H11C .31113 1.24574 .10154 .06900 Uiso ? ? H12A .37314 .96884 -.07726 .06400 Uiso ? ? H12B .31458 .90322 -.03670 .06400 Uiso ? ? H13A .50399 .94325 .10110 .21000 Uiso ? ? H13B .47379 .86364 .03780 .21000 Uiso ? ? H14A .38683 .80055 .29996 .22800 Uiso ? ? H14B .42010 .76644 .18323 .22800 Uiso ? ? H14C .32619 .81287 .15661 .22800 Uiso ? ? H15A .54093 .85422 .36871 .21000 Uiso ? ? H15B .56821 .92340 .29314 .21000 Uiso ? ? H15C .57503 .84044 .24265 .21000 Uiso ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu1 .0377(8) .0288(7) .0220(6) -.0027(5) .0068(5) -.0017(4) Cu2 .0519(10) .0357(7) .0301(7) -.0207(6) .0225(6) -.0085(5) Pb .0337(3) .0284(2) .0215(2) .00248(16) .00184(16) -.00009(13) S1 .051(2) .0417(16) .0412(15) .0103(14) .0002(14) -.0022(12) S2 .070(2) .0429(16) .0274(13) -.0055(15) .0143(14) -.0079(11) S3 .079(3) .111(4) .0368(18) -.001(3) -.003(2) .009(2) O1 .059(6) .025(4) .031(4) -.002(3) .019(4) -.003(3) O2 .047(5) .028(4) .026(3) -.011(3) .005(3) -.004(3) O3 .036(5) .045(4) .025(4) .004(3) .004(3) .005(3) N1 .059(9) .073(8) .037(6) .004(6) -.007(6) -.001(5) N2 .049(7) .049(6) .028(5) -.008(5) .008(5) -.015(4) N3 .073(10) .065(8) .059(7) .003(7) .003(7) .010(6) N4 .029(6) .039(5) .039(5) -.004(4) .009(4) -.001(4) N5 .043(6) .032(5) .026(4) .005(4) .005(4) -.002(3) N6 .052(9) .083(10) .087(10) .023(7) .013(7) .036(8) C1 .026(6) .035(6) .032(5) -.001(4) .002(5) -.002(4) C2 .027(6) .031(5) .032(5) -.004(4) .009(4) -.004(4) C3 .058(10) .071(10) .038(7) -.003(7) -.003(6) .001(6) C4 .114(14) .029(6) .051(7) -.022(7) .041(8) -.014(5) C5 .056(9) .045(7) .045(6) -.015(6) .019(6) -.003(5) C6 .078(11) .033(6) .041(6) .003(6) .015(7) .017(5) C7 .051(10) .114(14) .046(8) -.005(9) .023(7) -.001(8) C8 .076(10) .025(5) .028(5) -.011(5) .018(6) -.003(4) C9 .063(9) .033(6) .036(6) -.008(5) .020(6) -.012(5) C10 .077(11) .040(7) .048(7) .007(7) .003(7) -.002(6) C11 .058(9) .041(6) .034(6) -.007(6) .010(6) .001(5) C12 .041(8) .067(9) .049(7) .011(7) .018(6) -.001(6) C13 .30(5) .22(3) .099(17) .20(3) .09(2) .05(2) C14 .10(2) .069(14) .32(4) -.004(13) .08(2) .01(2) C15 .042(13) .112(18) .26(3) .022(12) .040(17) .03(2) _atom_sites_solution_primary direct _atom_sites_solution_secondary diff-map _atom_sites_solution_hydrogens geom _refine_special_details sfls__F_____calc_weight______full_matrix _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 395(279) _refine_ls_extinction_expression Eq22_p292_"Cryst._Comp."_Munksgaard_1970 _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack 0 _refine_ls_number_reflns 4798 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .075 _refine_ls_R_factor_obs .061 _refine_ls_wR_factor_all .089 _refine_ls_wR_factor_obs .086 _refine_ls_goodness_of_fit_all 2.538 _refine_ls_goodness_of_fit_obs 2.701 _refine_ls_shift/esd_max .046 _refine_ls_shift/esd_mean .001 _refine_diff_density_min -1.776 _refine_diff_density_max 5.147 _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 Cu2 3.183(2) . . ? Cu1 Pb 3.2901(13) . . ? Cu1 O1 1.937(8) . . ? Cu1 O2 2.004(8) . . ? Cu1 N1 2.321(12) . . ? Cu1 N2 1.929(10) . . ? Cu1 N4 2.029(10) . . ? Cu2 O2 2.148(8) . . ? Cu2 O3 2.030(7) . . ? Cu2 N3 1.810(13) . . ? Cu2 N6 1.973(15) . . ? Pb O1 2.440(7) . . ? Pb O2 2.460(6) . . ? Pb O3 2.264(9) . . ? S1 C1 1.635(11) . . ? S2 C2 1.610(11) . . ? S3 C3 1.589(13) . . ? O1 C4 1.413(16) . . ? O2 C8 1.443(12) . . ? O3 C12 1.399(17) . . ? N1 C1 1.159(17) . . ? N2 C2 1.174(14) . . ? N3 C3 1.208(18) . . ? N4 C5 1.467(15) . . ? N4 C6 1.487(15) . . ? N4 C7 1.47(2) . . ? N5 C9 1.462(14) . . ? N5 C10 1.421(17) . . ? N5 C11 1.447(19) . . ? N6 C13 1.43(3) . . ? N6 C14 1.48(3) . . ? N6 C15 1.46(3) . . ? C4 C5 1.52(2) . . ? C4 H4A .953(14) . . ? C4 H4B .953(13) . . ? C5 H5A .957(13) . . ? C5 H5B .948(13) . . ? C6 H6A .899(13) . . ? C6 H6B .946(12) . . ? C6 H6C .954(16) . . ? C7 H7A .941(15) . . ? C7 H7B .954(18) . . ? C7 H7C .952(15) . . ? C8 C9 1.468(16) . . ? C8 H8A .960(15) . . ? C8 H8B .955(12) . . ? C9 H9A .954(11) . . ? C9 H9B .950(15) . . ? C10 H10A .950(13) . . ? C10 H10B .950(13) . . ? C10 H10C .961(18) . . ? C11 H11A .947(12) . . ? C11 H11B .962(12) . . ? C11 H11C .947(12) . . ? C12 C13 1.58(4) . . ? C12 H12A .948(15) . . ? C12 H12B .948(14) . . ? C13 H13A .93(4) . . ? C13 H13B .96(3) . . ? C14 H14A .98(4) . . ? C14 H14B .94(3) . . ? C14 H14C .92(3) . . ? C15 H15A .96(3) . . ? C15 H15B .96(2) . . ? C15 H15C .94(3) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cu1 N3 3.113(15) . . ? Cu1 C2 3.098(10) . . ? Cu1 C4 2.813(12) . . ? Cu1 C5 2.758(13) . . ? Cu1 C6 2.849(12) . . ? Cu1 C7 2.941(18) . . ? Cu1 C8 3.002(12) . . ? Cu1 H5B 2.9662(13) . . ? Cu1 H6B 2.9684(12) . . ? Cu1 H6C 2.9178(11) . . ? Cu1 H7A 3.0565(15) . . ? Cu1 H7C 3.0508(16) . . ? Cu1 H8B 2.9417(12) . . ? Cu2 Pb 3.3702(14) . . ? Cu2 S3 3.027(6) . 3_676 ? Cu2 O1 2.682(9) . . ? Cu2 C3 3.008(13) . . ? Cu2 C8 3.163(12) . . ? Cu2 C12 2.879(14) . . ? Cu2 C13 2.73(3) . . ? Cu2 C14 2.80(2) . . ? Cu2 C15 2.83(2) . . ? Cu2 H8A 3.0608(14) . . ? Cu2 H13A 2.9178(17) . . ? Cu2 H14A 2.8471(13) . . ? Cu2 H14C 2.8925(13) . . ? Cu2 H15A 3.0215(15) . . ? Cu2 H15B 2.8325(17) . . ? Pb S1 3.260(3) . 3_575 ? Pb S2 3.426(3) . 1_554 ? Pb N1 3.966(11) . 3_575 ? Pb N1 3.054(14) . . ? Pb N5 2.693(9) . . ? Pb C1 3.690(12) . . ? Pb C1 3.437(10) . 3_575 ? Pb C4 3.499(13) . . ? Pb C8 3.416(10) . . ? Pb C9 3.336(11) . . ? Pb C10 3.433(13) . . ? Pb C11 3.542(13) . . ? Pb C12 3.229(16) . . ? Pb H9B 3.3969(4) . . ? Pb H12B 3.1786(4) . . ? S1 S2 4.248(5) . 3_576 ? S1 O1 3.757(7) . 3_575 ? S1 O3 3.984(8) . 3_575 ? S1 N1 2.793(13) . . ? S1 N4 4.621(10) . 3_576 ? S1 N4 4.533(9) . 2 ? S1 C4 3.664(14) . 3_575 ? S1 C5 3.943(13) . 2 ? S1 C7 3.817(14) . 3_576 ? S1 C12 3.693(14) . 3_575 ? S1 H4A 3.582(3) . 2 ? S1 H4B 2.863(3) . 3_575 ? S1 H5A 3.121(3) . 2 ? S1 H6A 3.370(3) . 2 ? S1 H6B 3.534(4) . 3_576 ? S1 H7A 3.146(3) . 3_576 ? S1 H7B 3.636(3) . 3_576 ? S1 H10C 3.474(4) . . ? S1 H12B 2.878(4) . 3_575 ? S2 S3 4.921(7) . . ? S2 O3 3.667(8) . 1_556 ? S2 N1 4.436(15) . 3_576 ? S2 N2 2.782(10) . . ? S2 N5 4.508(9) . 4_575 ? S2 N5 3.697(9) . 1_556 ? S2 C10 3.803(16) . 1_556 ? S2 C11 3.525(11) . 1_556 ? S2 C12 3.793(14) . 1_556 ? S2 C15 3.80(3) . 3_676 ? S2 H5B 3.450(4) . 3_576 ? S2 H7C 3.265(3) . 3_576 ? S2 H9A 3.159(3) . 4_575 ? S2 H10A 3.081(4) . 1_556 ? S2 H10B 3.395(3) . 4_575 ? S2 H11A 2.763(3) . 1_556 ? S2 H12A 3.261(3) . 1_556 ? S2 H15B 3.410(4) . 3_676 ? S2 H15C 3.300(4) . 3_676 ? S3 O2 3.922(10) . 3_676 ? S3 O3 3.511(9) . 3_676 ? S3 N2 4.339(12) . . ? S3 N3 3.748(16) . 3_676 ? S3 N3 2.797(13) . . ? S3 N6 3.762(15) . 3_676 ? S3 C8 3.788(16) . 3_676 ? S3 C12 3.678(16) . 1_556 ? S3 C13 3.69(3) . 3_676 ? S3 C13 3.91(3) . 1_556 ? S3 C15 3.60(2) . 3_676 ? S3 H8A 2.942(6) . 3_676 ? S3 H11B 3.126(5) . 3_676 ? S3 H12A 2.984(5) . 1_556 ? S3 H13A 3.019(5) . 3_676 ? S3 H13B 3.496(4) . 1_556 ? S3 H14B 3.318(5) . 4_565 ? S3 H15B 2.778(5) . 3_676 ? O1 O2 2.495(10) . . ? O1 N1 3.109(16) . . ? O1 N3 3.371(15) . . ? O1 N4 2.684(14) . . ? O1 N6 3.656(18) . . ? O1 C5 2.398(18) . . ? O1 H4A 1.953(7) . . ? O1 H4B 1.952(7) . . ? O2 O3 2.684(12) . . ? O2 N1 3.102(17) . . ? O2 N2 2.989(14) . . ? O2 N3 2.874(14) . . ? O2 N5 2.872(11) . . ? O2 C9 2.398(13) . . ? O2 H8A 1.976(7) . . ? O2 H8B 1.976(7) . . ? O2 H9B 2.635(8) . . ? O3 N5 3.559(12) . . ? O3 N6 2.681(15) . . ? O3 C13 2.36(4) . . ? O3 H12A 1.943(8) . . ? O3 H12B 1.947(8) . . ? O3 H13A 2.629(9) . . ? N1 N2 3.234(14) . . ? N1 N4 3.225(15) . . ? N1 N5 3.870(17) . . ? N1 C5 3.336(18) . . ? N1 C7 3.41(2) . . ? N1 C7 3.69(2) . 3_576 ? N1 C8 3.66(2) . . ? N1 C9 3.476(19) . . ? N1 H5B 2.818(13) . . ? N1 H7A 3.129(14) . 3_576 ? N1 H7C 2.822(13) . . ? N1 H9B 2.767(13) . . ? N2 N3 3.61(2) . . ? N2 N4 2.939(13) . . ? N2 C3 3.69(2) . . ? N2 C6 3.388(15) . . ? N2 C7 3.11(2) . . ? N2 C8 3.154(17) . . ? N2 H6B 2.950(10) . . ? N2 H7A 2.634(11) . . ? N2 H7C 3.126(12) . 3_576 ? N2 H7C 3.322(11) . . ? N2 H8B 2.510(11) . . ? N3 N3 3.47(2) . 3_676 ? N3 N4 4.196(18) . . ? N3 N6 2.95(2) . . ? N3 C3 3.31(2) . 3_676 ? N3 C8 3.621(17) . . ? N3 C14 3.37(3) . . ? N3 C15 3.19(4) . . ? N3 H6C 3.207(15) . . ? N3 H14A 2.861(13) . . ? N3 H15A 2.812(15) . . ? N3 H15B 3.250(16) . . ? N4 C4 2.441(18) . . ? N4 H4A 2.752(10) . . ? N4 H4B 3.245(10) . . ? N4 H5A 1.994(9) . . ? N4 H5B 1.994(8) . . ? N4 H6A 2.048(9) . . ? N4 H6B 2.017(8) . . ? N4 H6C 2.020(10) . . ? N4 H7A 1.992(10) . . ? N4 H7B 1.997(11) . . ? N4 H7C 1.998(10) . . ? N5 C8 2.486(13) . . ? N5 H8A 2.753(8) . . ? N5 H8B 3.287(8) . . ? N5 H9A 1.972(8) . . ? N5 H9B 1.974(10) . . ? N5 H10A 1.965(8) . . ? N5 H10B 1.964(9) . . ? N5 H10C 1.966(10) . . ? N5 H11A 1.983(11) . . ? N5 H11B 1.983(11) . . ? N5 H11C 1.982(10) . . ? N6 C12 2.466(19) . . ? N6 H12A 3.266(14) . . ? N6 H12B 2.751(13) . . ? N6 H13A 1.945(16) . . ? N6 H13B 1.946(16) . . ? N6 H14A 1.981(15) . . ? N6 H14B 1.985(14) . . ? N6 H14C 1.987(14) . . ? N6 H15A 1.995(13) . . ? N6 H15B 2.000(13) . . ? N6 H15C 2.001(14) . . ? C4 H5A 2.054(18) . . ? C4 H5B 2.051(19) . . ? C5 C6 2.481(17) . . ? C5 C7 2.41(2) . . ? C5 H4A 2.049(16) . . ? C5 H4B 2.046(15) . . ? C5 H6C 2.659(13) . . ? C5 H7B 2.621(15) . . ? C5 H7C 2.555(14) . . ? C6 C7 2.40(2) . . ? C6 H5A 2.604(12) . . ? C6 H7A 2.566(15) . . ? C6 H7B 2.589(17) . . ? C7 H5A 2.685(17) . . ? C7 H5B 2.499(14) . . ? C7 H6A 2.675(18) . . ? C7 H6B 2.589(16) . . ? C8 H9A 1.985(10) . . ? C8 H9B 1.979(13) . . ? C8 H11B 2.693(13) . . ? C9 C10 2.384(16) . . ? C9 C11 2.37(2) . . ? C9 H8A 2.005(13) . . ? C9 H8B 2.006(11) . . ? C9 H10B 2.610(11) . . ? C9 H10C 2.545(11) . . ? C9 H11B 2.571(15) . . ? C9 H11C 2.541(14) . . ? C10 C11 2.34(2) . . ? C10 H9A 2.628(12) . . ? C10 H9B 2.478(13) . . ? C10 H11A 2.512(18) . . ? C10 H11C 2.578(17) . . ? C11 H9A 2.475(14) . . ? C11 H10A 2.565(13) . . ? C11 H10B 2.516(14) . . ? C12 H13A 2.096(13) . . ? C12 H13B 2.094(14) . . ? C13 C14 2.53(5) . . ? C13 C15 2.21(4) . . ? C13 H12A 2.10(3) . . ? C13 H12B 2.12(3) . . ? C13 H15B 2.40(3) . . ? C13 H15C 2.38(3) . . ? C14 C15 2.44(3) . . ? C14 H13B 2.63(4) . . ? C14 H15A 2.56(3) . . ? C15 H13A 2.21(3) . . ? C15 H13B 2.51(3) . . ? C15 H14A 2.61(3) . . ? C15 H14B 2.58(2) . . ? H4A H4B 1.55135(6) . . ? H4A H5A 2.26414(4) . . ? H4A H6C 2.30607(5) . . ? H4A H14C 2.34461(4) . . ? H4B H5B 2.26390(5) . . ? H5A H5B 1.551410(19) . . ? H5B H7C 2.27893(2) . . ? H6A H6B 1.49930(2) . . ? H6A H6C 1.44334(3) . . ? H6B H6C 1.551519(19) . . ? H6B H7A 2.39361(2) . . ? H7A H7B 1.55120(2) . . ? H7A H7C 1.55130(6) . . ? H7B H7C 1.551281(16) . . ? H8A H8B 1.55134(4) . . ? H8A H9A 2.23617(3) . . ? H8A H11B 2.23956(2) . . ? H8B H9A 2.31156(3) . . ? H8B H9B 2.22790(8) . . ? H9A H9B 1.551272(11) . . ? H9A H11C 2.26912(5) . . ? H9B H10C 2.26614(7) . . ? H10A H10B 1.551402(17) . . ? H10A H10C 1.55126(4) . . ? H10A H11A 2.36798(3) . . ? H10B H10C 1.551451(11) . . ? H10B H11C 2.38761(4) . . ? H11A H11B 1.55137(5) . . ? H11A H11C 1.552214(18) . . ? H11B H11C 1.551570(16) . . ? H12A H12B 1.551328(18) . . ? H12A H13A 2.34353(9) . . ? H12B H13B 2.35125(5) . . ? H13A H13B 1.551267(18) . . ? H13A H15B 2.02265(6) . . ? H13A H15C 2.38566(4) . . ? H13B H15C 2.30809(9) . . ? H14A H14B 1.55125(3) . . ? H14A H14C 1.55132(5) . . ? H14A H15A 2.36573(4) . . ? H14B H14C 1.551355(18) . . ? H15A H15B 1.551228(17) . . ? H15A H15C 1.55140(3) . . ? H15B H15C 1.551349(16) . . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu2 Cu1 Pb 62.73(4) . . . ? Cu2 Cu1 O1 57.1(3) . . . ? Cu2 Cu1 O2 41.6(2) . . . ? Cu2 Cu1 N1 124.6(3) . . . ? Cu2 Cu1 N2 113.2(4) . . . ? Cu2 Cu1 N4 123.1(3) . . . ? Pb Cu1 O1 47.4(2) . . . ? Pb Cu1 O2 48.19(18) . . . ? Pb Cu1 N1 63.2(3) . . . ? Pb Cu1 N2 137.9(3) . . . ? Pb Cu1 N4 122.1(3) . . . ? O1 Cu1 O2 78.5(3) . . . ? O1 Cu1 N1 93.4(4) . . . ? O1 Cu1 N2 167.8(4) . . . ? O1 Cu1 N4 85.1(4) . . . ? O2 Cu1 N1 91.3(4) . . . ? O2 Cu1 N2 98.9(4) . . . ? O2 Cu1 N4 162.7(4) . . . ? N1 Cu1 N2 98.7(4) . . . ? N1 Cu1 N4 95.4(4) . . . ? N2 Cu1 N4 95.8(4) . . . ? Cu1 Cu2 O2 38.3(2) . . . ? Cu1 Cu2 O3 101.0(3) . . . ? Cu1 Cu2 N3 71.2(5) . . . ? Cu1 Cu2 N6 134.3(4) . . . ? O2 Cu2 O3 79.9(3) . . . ? O2 Cu2 N3 92.8(5) . . . ? O2 Cu2 N6 158.9(4) . . . ? O3 Cu2 N3 172.1(6) . . . ? O3 Cu2 N6 84.1(5) . . . ? N3 Cu2 N6 102.3(6) . . . ? Cu1 Pb O1 35.78(18) . . . ? Cu1 Pb O2 37.4(2) . . . ? Cu1 Pb O3 92.95(19) . . . ? O1 Pb O2 61.2(2) . . . ? O1 Pb O3 80.0(3) . . . ? O2 Pb O3 69.1(3) . . . ? Cu1 O1 Pb 96.8(3) . . . ? Cu1 O1 C4 113.3(8) . . . ? Pb O1 C4 128.5(6) . . . ? Cu1 O2 Cu2 100.0(3) . . . ? Cu1 O2 Pb 94.4(3) . . . ? Cu1 O2 C8 120.2(7) . . . ? Cu2 O2 Pb 93.8(3) . . . ? Cu2 O2 C8 122.2(7) . . . ? Pb O2 C8 119.9(5) . . . ? Cu2 O3 Pb 103.3(4) . . . ? Cu2 O3 C12 112.9(7) . . . ? Pb O3 C12 121.8(7) . . . ? Cu1 N1 C1 167.6(10) . . . ? Cu1 N2 C2 173.3(9) . . . ? Cu2 N3 C3 170.7(14) . . . ? Cu1 N4 C5 102.9(8) . . . ? Cu1 N4 C6 107.3(8) . . . ? Cu1 N4 C7 113.4(9) . . . ? C5 N4 C6 114.3(9) . . . ? C5 N4 C7 110.2(10) . . . ? C6 N4 C7 108.7(10) . . . ? C9 N5 C10 111.5(10) . . . ? C9 N5 C11 109.4(9) . . . ? C10 N5 C11 109.6(10) . . . ? Cu2 N6 C13 105.3(16) . . . ? Cu2 N6 C14 107.8(16) . . . ? Cu2 N6 C15 110.0(14) . . . ? C13 N6 C14 121(2) . . . ? C13 N6 C15 100(2) . . . ? C14 N6 C15 112.5(17) . . . ? S1 C1 N1 176.3(12) . . . ? S2 C2 N2 176.5(10) . . . ? S3 C3 N3 179.7(16) . . . ? O1 C4 C5 109.6(11) . . . ? O1 C4 H4A 109.8(15) . . . ? O1 C4 H4B 109.6(12) . . . ? C5 C4 H4A 109.6(13) . . . ? C5 C4 H4B 109.3(15) . . . ? H4A C4 H4B 108.9(13) . . . ? N4 C5 C4 109.5(11) . . . ? N4 C5 H5A 108.9(11) . . . ? N4 C5 H5B 109.4(11) . . . ? C4 C5 H5A 109.8(12) . . . ? C4 C5 H5B 110.1(12) . . . ? H5A C5 H5B 109.1(14) . . . ? N4 C6 H6A 116.1(14) . . . ? N4 C6 H6B 110.1(11) . . . ? N4 C6 H6C 109.8(11) . . . ? H6A C6 H6B 108.7(13) . . . ? H6A C6 H6C 102.3(12) . . . ? H6B C6 H6C 109.5(15) . . . ? N4 C7 H7A 109.5(14) . . . ? N4 C7 H7B 109.1(15) . . . ? N4 C7 H7C 109.2(13) . . . ? H7A C7 H7B 109.9(15) . . . ? H7A C7 H7C 110.1(18) . . . ? H7B C7 H7C 109.0(16) . . . ? O2 C8 C9 110.9(9) . . . ? O2 C8 H8A 108.9(11) . . . ? O2 C8 H8B 109.3(10) . . . ? C9 C8 H8A 109.6(11) . . . ? C9 C8 H8B 109.9(12) . . . ? H8A C8 H8B 108.2(10) . . . ? N5 C9 C8 116.0(11) . . . ? N5 C9 H9A 107.6(10) . . . ? N5 C9 H9B 108.0(10) . . . ? C8 C9 H9A 108.2(10) . . . ? C8 C9 H9B 107.9(11) . . . ? H9A C9 H9B 109.1(13) . . . ? N5 C10 H10A 110.3(14) . . . ? N5 C10 H10B 110.2(12) . . . ? N5 C10 H10C 109.7(12) . . . ? H10A C10 H10B 109.4(13) . . . ? H10A C10 H10C 108.5(14) . . . ? H10B C10 H10C 108.6(16) . . . ? N5 C11 H11A 110.1(11) . . . ? N5 C11 H11B 109.1(11) . . . ? N5 C11 H11C 110.0(13) . . . ? H11A C11 H11B 108.7(14) . . . ? H11A C11 H11C 110.1(12) . . . ? H11B C11 H11C 108.7(12) . . . ? O3 C12 C13 104.8(14) . . . ? O3 C12 H12A 110.3(13) . . . ? O3 C12 H12B 110.6(14) . . . ? C13 C12 H12A 109.9(18) . . . ? C13 C12 H12B 111.4(17) . . . ? H12A C12 H12B 109.8(13) . . . ? N6 C13 C12 110(3) . . . ? N6 C13 H13A 109(2) . . . ? N6 C13 H13B 107(3) . . . ? C12 C13 H13A 111(3) . . . ? C12 C13 H13B 109(2) . . . ? H13A C13 H13B 111(4) . . . ? N6 C14 H14A 106(2) . . . ? N6 C14 H14B 109(3) . . . ? N6 C14 H14C 110(2) . . . ? H14A C14 H14B 108(3) . . . ? H14A C14 H14C 110(3) . . . ? H14B C14 H14C 114(3) . . . ? N6 C15 H15A 109(2) . . . ? N6 C15 H15B 110(2) . . . ? N6 C15 H15C 111(3) . . . ? H15A C15 H15B 108(3) . . . ? H15A C15 H15C 109(2) . . . ? H15B C15 H15C 110(3) . . . ? _reflns_limit_h_min -19 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 13 _reflns_number_total 5799 _reflns_number_observed 4798 _reflns_observed_criterion refl_observed_if_F____>_6.00_sigma(F___) _reflns_d_resolution_high .751 _reflns_d_resolution_low 10.923 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? 14.4347