# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Craig Rice' _publ_contact_author_address ; Department of Chemical and Biological Sciences University of Huddersfield Queensgate Huddersfield West Yorkshire HD1 3DH UNITED KINGDOM ; _publ_contact_author_email C.R.RICE@HUD.AC.UK _publ_section_title ; Facile Interconversion of Dinuclear Double Helicates and Side-by-Side Species: A Reprogrammable Ligand with Potential Sensor Applications. ; loop_ _publ_author_name 'Craig Rice' 'Georgios Bokolinis' 'Lindsay P. Harding' 'J. Jeffery' 'Neil McLay' ; T.Riis-Johannessen ; #======================================================== data_craig19m _database_code_depnum_ccdc_archive 'CCDC 285237' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C104 H100 B2 Cu2 N8 O12 S2' _chemical_formula_weight 1866.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 14.3802(3) _cell_length_b 20.4058(4) _cell_length_c 37.9889(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.8080(10) _cell_angle_gamma 90.00 _cell_volume 11108.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4607 _cell_measurement_theta_min 4.669 _cell_measurement_theta_max 123.845 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.116 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3904 _exptl_absorpt_coefficient_mu 1.275 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.498516 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2001)' _exptl_special_details ; The structure contains extensive disorder within both the crown ether substituents (on the complex molecule) and the discreet, non-coordinating, tetraphenylborate counter ions. For the latter, of the expected two anions (per helicate/asymmetric unit), one was disordered over two partially overlapping positions (each component was refined at 0.5 site occupancy), whilst the other was refined at full site occupancy in one position. The geometries of the tetraphenylborate anions were modelled as follow; for each anion (component), the boron positions and isotropic displacement parameters were fixed and all rings were modelled using ring constraints. Furthermore, each tetrahedron described by the four ipso carbons located around the central boron atoms and all B-C bonds were restrained to an ideal geometry (DFIX). Finally, the Ph-B planes, for each phenyl ring attached to a boron atom, were restrained to approximate co-planarity using FLAT. The positional disorder present in the split occupancy tetraphenylborat ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source '4.8 kW rotating anode' _diffrn_radiation_monochromator 'Osmic ConFocal MaxFlux mirror optics' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Frames, each covering 0.3 \% in \w' _diffrn_detector_area_resol_mean 5.6 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52309 _diffrn_reflns_av_R_equivalents 0.0599 _diffrn_reflns_av_sigmaI/netI 0.0709 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 70.40 _reflns_number_total 18266 _reflns_number_gt 9000 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement 'SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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^)+(0.2000P)^2^+0.0000P] 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 18266 _refine_ls_number_parameters 741 _refine_ls_number_restraints 161 _refine_ls_R_factor_all 0.1946 _refine_ls_R_factor_gt 0.1439 _refine_ls_wR_factor_ref 0.4213 _refine_ls_wR_factor_gt 0.3838 _refine_ls_goodness_of_fit_ref 1.346 _refine_ls_restrained_S_all 1.393 _refine_ls_shift/su_max 0.162 _refine_ls_shift/su_mean 0.008 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 1.22706(8) 0.47457(6) 0.84206(3) 0.0608(4) Uani 1 1 d . . . Cu2 Cu 0.91600(9) 0.58533(6) 0.89726(3) 0.0600(4) Uani 1 1 d . . . N11 N 1.3414(5) 0.5363(3) 0.84788(17) 0.0544(16) Uani 1 1 d . . . C12 C 1.3433(6) 0.5755(4) 0.8765(2) 0.052(2) Uani 1 1 d . . . C13 C 1.4119(6) 0.6225(5) 0.8839(2) 0.066(2) Uani 1 1 d . . . H13 H 1.4101 0.6496 0.9035 0.079 Uiso 1 1 calc R . . C14 C 1.4819(7) 0.6286(5) 0.8620(3) 0.074(3) Uani 1 1 d . . . H14 H 1.5295 0.6590 0.8669 0.088 Uiso 1 1 calc R . . C15 C 1.4811(6) 0.5894(5) 0.8329(3) 0.069(3) Uani 1 1 d . . . H15 H 1.5274 0.5938 0.8173 0.082 Uiso 1 1 calc R . . C16 C 1.4124(7) 0.5437(5) 0.8265(3) 0.070(2) Uani 1 1 d . . . H16 H 1.4140 0.5166 0.8069 0.084 Uiso 1 1 calc R . . N21 N 1.2013(4) 0.5165(3) 0.88845(16) 0.0515(16) Uani 1 1 d . . . C22 C 1.1323(5) 0.5148(4) 0.9086(2) 0.0521(19) Uani 1 1 d . . . S23 S 1.13776(15) 0.57495(11) 0.94076(5) 0.0563(5) Uani 1 1 d . . . C24 C 1.2387(6) 0.6042(4) 0.9257(2) 0.057(2) Uani 1 1 d . . . H24 H 1.2719 0.6404 0.9349 0.068 Uiso 1 1 calc R . . C25 C 1.2635(6) 0.5662(4) 0.8981(2) 0.054(2) Uani 1 1 d . . . N31 N 0.9689(5) 0.4897(3) 0.91108(16) 0.0509(16) Uani 1 1 d . . . C32 C 0.8961(6) 0.4482(4) 0.9064(2) 0.053(2) Uani 1 1 d . . . C33 C 0.9066(6) 0.3867(5) 0.8927(2) 0.063(2) Uani 1 1 d . . . C34 C 0.9933(6) 0.3647(4) 0.8858(2) 0.060(2) Uani 1 1 d . . . H34 H 1.0003 0.3228 0.8768 0.072 Uiso 1 1 calc R . . C35 C 1.0697(6) 0.4043(4) 0.8923(2) 0.059(2) Uani 1 1 d . . . H35 H 1.1295 0.3895 0.8889 0.071 Uiso 1 1 calc R C . C36 C 1.0542(6) 0.4676(4) 0.9041(2) 0.055(2) Uani 1 1 d . . . N41 N 0.7943(5) 0.5411(4) 0.90255(18) 0.0637(19) Uani 1 1 d . . . C42 C 0.8062(6) 0.4781(5) 0.9132(2) 0.056(2) Uani 1 1 d . . . C43 C 0.7384(7) 0.4450(5) 0.9315(2) 0.065(2) Uani 1 1 d . C . C44 C 0.6541(7) 0.4780(5) 0.9343(2) 0.072(3) Uani 1 1 d . . . H44 H 0.6064 0.4576 0.9452 0.086 Uiso 1 1 calc R C . C45 C 0.6410(7) 0.5397(6) 0.9210(3) 0.087(3) Uani 1 1 d . . . H45 H 0.5836 0.5603 0.9219 0.105 Uiso 1 1 calc R . . C46 C 0.7133(7) 0.5716(5) 0.9063(2) 0.072(3) Uani 1 1 d . . . H46 H 0.7055 0.6148 0.8988 0.087 Uiso 1 1 calc R C . N51 N 1.2304(5) 0.3957(4) 0.81199(18) 0.0620(18) Uani 1 1 d . . . C52 C 1.1555(6) 0.3911(4) 0.7880(2) 0.058(2) Uani 1 1 d . . . C53 C 1.1626(6) 0.3566(5) 0.7555(2) 0.070(3) Uani 1 1 d . . . C54 C 1.2415(7) 0.3208(5) 0.7512(3) 0.078(3) Uani 1 1 d . . . H54 H 1.2467 0.2964 0.7308 0.093 Uiso 1 1 calc R . . C55 C 1.3151(8) 0.3217(6) 0.7786(3) 0.086(3) Uani 1 1 d . . . H55 H 1.3676 0.2956 0.7770 0.103 Uiso 1 1 calc R . . C56 C 1.3083(7) 0.3613(5) 0.8074(3) 0.075(3) Uani 1 1 d . . . H56 H 1.3589 0.3645 0.8242 0.090 Uiso 1 1 calc R . . N61 N 1.0916(5) 0.4875(3) 0.81079(16) 0.0552(17) Uani 1 1 d . . . C62 C 1.0729(6) 0.4266(4) 0.7967(2) 0.056(2) Uani 1 1 d . . . C63 C 0.9840(6) 0.4011(4) 0.7946(2) 0.060(2) Uani 1 1 d . . . C64 C 0.9094(6) 0.4385(5) 0.8048(2) 0.064(2) Uani 1 1 d . . . H64 H 0.8485 0.4227 0.8023 0.077 Uiso 1 1 calc R . . C65 C 0.9298(6) 0.5009(5) 0.8189(2) 0.056(2) Uani 1 1 d . . . H65 H 0.8825 0.5274 0.8262 0.067 Uiso 1 1 calc R . . C66 C 1.0205(5) 0.5223(4) 0.82170(19) 0.0492(18) Uani 1 1 d . . . N71 N 0.9985(5) 0.6162(3) 0.85963(16) 0.0543(16) Uani 1 1 d . . . C72 C 1.0431(6) 0.5879(4) 0.8357(2) 0.056(2) Uani 1 1 d . . . S73 S 1.12969(15) 0.63569(12) 0.81963(5) 0.0615(6) Uani 1 1 d . . . C74 C 1.1035(7) 0.6980(5) 0.8472(2) 0.067(2) Uani 1 1 d . . . H74 H 1.1326 0.7388 0.8486 0.081 Uiso 1 1 calc R . . C75 C 1.0327(7) 0.6785(4) 0.8670(2) 0.063(2) Uani 1 1 d . . . N81 N 0.9374(6) 0.6802(4) 0.91541(18) 0.066(2) Uani 1 1 d . . . C82 C 0.9908(8) 0.7149(5) 0.8949(2) 0.075(3) Uani 1 1 d . . . C83 C 1.0035(12) 0.7817(6) 0.9011(3) 0.119(5) Uani 1 1 d . . . H83 H 1.0401 0.8061 0.8869 0.143 Uiso 1 1 calc R . . C84 C 0.9624(13) 0.8112(6) 0.9279(4) 0.143(7) Uani 1 1 d . . . H84 H 0.9708 0.8558 0.9323 0.172 Uiso 1 1 calc R . . C85 C 0.9077(11) 0.7737(6) 0.9486(3) 0.117(5) Uani 1 1 d . . . H85 H 0.8795 0.7923 0.9674 0.140 Uiso 1 1 calc R . . C86 C 0.8963(8) 0.7089(5) 0.9408(2) 0.077(3) Uani 1 1 d . . . H86 H 0.8578 0.6840 0.9540 0.093 Uiso 1 1 calc R . . O400 O 1.0907(5) 0.3660(3) 0.73055(16) 0.0702(16) Uiso 1 1 d . . . C401 C 1.1062(8) 0.3506(5) 0.6947(3) 0.079(3) Uiso 1 1 d . . . H40A H 1.0905 0.3051 0.6897 0.095 Uiso 1 1 calc R . . H40B H 1.1714 0.3572 0.6908 0.095 Uiso 1 1 calc R . . C402 C 1.0462(9) 0.3943(6) 0.6711(3) 0.096(3) Uiso 1 1 d . . . H40C H 1.0536 0.4395 0.6788 0.115 Uiso 1 1 calc R . . H40D H 1.0636 0.3911 0.6470 0.115 Uiso 1 1 calc R . . O403 O 0.9514(6) 0.3736(4) 0.6729(2) 0.093(2) Uiso 1 1 d . . . C404 C 0.8893(10) 0.4155(7) 0.6507(4) 0.117(4) Uiso 1 1 d . . . H40E H 0.8962 0.4610 0.6578 0.141 Uiso 1 1 calc R . . H40F H 0.9018 0.4116 0.6261 0.141 Uiso 1 1 calc R . . C405 C 0.7970(11) 0.3913(7) 0.6562(4) 0.119(4) Uiso 1 1 d . . . H40G H 0.7507 0.4222 0.6462 0.143 Uiso 1 1 calc R . . H40H H 0.7905 0.3881 0.6813 0.143 Uiso 1 1 calc R . . O406 O 0.7798(7) 0.3272(5) 0.6399(3) 0.125(3) Uiso 1 1 d . . . C407 C 0.6842(14) 0.3009(9) 0.6405(5) 0.158(6) Uiso 1 1 d . . . H40I H 0.6425 0.3342 0.6300 0.190 Uiso 1 1 calc R . . H40J H 0.6799 0.2637 0.6246 0.190 Uiso 1 1 calc R . . C408 C 0.6502(14) 0.2827(8) 0.6684(5) 0.151(6) Uiso 1 1 d D . . H40K H 0.5858 0.2698 0.6625 0.181 Uiso 1 1 calc R . . H40L H 0.6500 0.3197 0.6844 0.181 Uiso 1 1 calc R . . O409 O 0.6946(9) 0.2336(6) 0.6849(3) 0.162(4) Uiso 1 1 d . . . C410 C 0.6708(11) 0.2061(7) 0.7159(3) 0.143(6) Uiso 1 1 d D B . H500 H 0.7027 0.1646 0.7200 0.171 Uiso 1 1 calc R . . H501 H 0.6041 0.1984 0.7148 0.171 Uiso 1 1 calc R . . C411 C 0.6972(9) 0.2494(9) 0.7428(4) 0.199(9) Uiso 1 1 d D . . H300 H 0.6537 0.2469 0.7609 0.238 Uiso 0.60 1 calc PR A 1 H301 H 0.6962 0.2938 0.7337 0.238 Uiso 0.60 1 calc PR A 1 H302 H 0.7159 0.2867 0.7292 0.238 Uiso 0.40 1 calc PR A 2 H303 H 0.6365 0.2617 0.7501 0.238 Uiso 0.40 1 calc PR A 2 O40A O 0.7968 0.2319 0.7587 0.100 Uiso 0.60 1 d PD B 1 C41A C 0.8655(11) 0.2679(8) 0.7425(4) 0.100 Uiso 0.60 1 d PD B 1 H304 H 0.8441 0.2738 0.7179 0.120 Uiso 0.60 1 calc PR B 1 H305 H 0.9217 0.2415 0.7434 0.120 Uiso 0.60 1 calc PR B 1 C42A C 0.8906(12) 0.3316(7) 0.7571(5) 0.094(5) Uiso 0.60 1 d PD B 1 H306 H 0.8376 0.3477 0.7688 0.112 Uiso 0.60 1 calc PR B 1 H307 H 0.8986 0.3608 0.7375 0.112 Uiso 0.60 1 calc PR B 1 O40B O 0.7488 0.2584 0.7721 0.100 Uiso 0.40 1 d PD B 2 C41B C 0.8267(13) 0.2992(13) 0.7649(7) 0.100 Uiso 0.40 1 d PD B 2 H308 H 0.8061 0.3444 0.7630 0.120 Uiso 0.40 1 calc PR B 2 H309 H 0.8483 0.2866 0.7423 0.120 Uiso 0.40 1 calc PR B 2 C42B C 0.9038(12) 0.2944(12) 0.7920(6) 0.091(8) Uiso 0.40 1 d PD B 2 H310 H 0.8835 0.3063 0.8148 0.109 Uiso 0.40 1 calc PR B 2 H311 H 0.9278 0.2499 0.7934 0.109 Uiso 0.40 1 calc PR B 2 O414 O 0.9738(5) 0.3383(3) 0.78224(16) 0.0764(17) Uiso 1 1 d D . . O50A O 0.7636(4) 0.3882(3) 0.94590(15) 0.0697(16) Uiso 0.50 1 d PD C 1 C51A C 0.6913(11) 0.3477(8) 0.9590(5) 0.061(5) Uiso 0.50 1 d PD C 1 H312 H 0.6455 0.3368 0.9396 0.073 Uiso 0.50 1 calc PR C 1 H313 H 0.6598 0.3720 0.9764 0.073 Uiso 0.50 1 calc PR C 1 C52A C 0.7304(15) 0.2875(8) 0.9749(5) 0.100 Uiso 0.50 1 d PD C 1 H314 H 0.6796 0.2584 0.9797 0.120 Uiso 0.50 1 calc PR C 1 H315 H 0.7669 0.2657 0.9580 0.120 Uiso 0.50 1 calc PR C 1 O53A O 0.7876(11) 0.2977(7) 1.0066(4) 0.100 Uiso 0.50 1 d PD C 1 C54A C 0.8469(12) 0.2464(9) 1.0185(6) 0.100 Uiso 0.50 1 d PD C 1 H316 H 0.9004 0.2648 1.0324 0.120 Uiso 0.50 1 calc PR C 1 H317 H 0.8698 0.2248 0.9982 0.120 Uiso 0.50 1 calc PR C 1 C55A C 0.8025(15) 0.1963(8) 1.0404(4) 0.100 Uiso 0.50 1 d PD C 1 H318 H 0.8503 0.1676 1.0514 0.120 Uiso 0.50 1 calc PR C 1 H319 H 0.7720 0.2181 1.0590 0.120 Uiso 0.50 1 calc PR C 1 O56A O 0.7364(11) 0.1587(7) 1.0196(4) 0.100 Uiso 0.50 1 d PD C 1 C57A C 0.7637(16) 0.1388(11) 0.9866(4) 0.100 Uiso 0.50 1 d PD C 1 H320 H 0.8282 0.1245 0.9898 0.120 Uiso 0.50 1 calc PR C 1 H321 H 0.7615 0.1766 0.9712 0.120 Uiso 0.50 1 calc PR C 1 C58A C 0.7090(17) 0.0865(10) 0.9688(4) 0.100 Uiso 0.50 1 d PD C 1 H322 H 0.7247 0.0457 0.9809 0.120 Uiso 0.50 1 calc PR C 1 H323 H 0.6436 0.0951 0.9713 0.120 Uiso 0.50 1 calc PR C 1 O59A O 0.7204(11) 0.0775(7) 0.9325(3) 0.100 Uiso 0.50 1 d PD C 1 C60A C 0.6681(14) 0.1105(9) 0.9076(5) 0.100 Uiso 0.50 1 d PD C 1 H324 H 0.6276 0.1402 0.9191 0.120 Uiso 0.50 1 calc PR C 1 H325 H 0.6287 0.0795 0.8939 0.120 Uiso 0.50 1 calc PR C 1 C61A C 0.7238(17) 0.1506(8) 0.8819(5) 0.100 Uiso 0.50 1 d PD C 1 H326 H 0.7891 0.1382 0.8849 0.120 Uiso 0.50 1 calc PR C 1 H327 H 0.7007 0.1409 0.8577 0.120 Uiso 0.50 1 calc PR C 1 O62A O 0.7156(11) 0.2141(7) 0.8878(4) 0.100 Uiso 0.50 1 d PD C 1 C63A C 0.7329(19) 0.2628(10) 0.8634(7) 0.151(14) Uiso 0.50 1 d PD C 1 H327' H 0.6878 0.2978 0.8648 0.181 Uiso 0.50 1 calc PR C 1 H328 H 0.7248 0.2445 0.8398 0.181 Uiso 0.50 1 calc PR C 1 C64A C 0.8296(14) 0.2907(8) 0.8695(7) 0.085(7) Uiso 0.50 1 d PD C 1 H329 H 0.8679 0.2619 0.8850 0.102 Uiso 0.50 1 calc PR C 1 H330 H 0.8577 0.2936 0.8472 0.102 Uiso 0.50 1 calc PR C 1 O65A O 0.8262(5) 0.3527(3) 0.88462(17) 0.0768(17) Uiso 0.50 1 d PD C 1 O50B O 0.8262(5) 0.3527(3) 0.88462(17) 0.0768(17) Uiso 0.50 1 d PD C 2 C51B C 0.8287(13) 0.2826(6) 0.8833(6) 0.078(7) Uiso 0.50 1 d PD C 2 H331 H 0.8446 0.2654 0.9068 0.094 Uiso 0.50 1 calc PR C 2 H332 H 0.8767 0.2687 0.8684 0.094 Uiso 0.50 1 calc PR C 2 C52B C 0.7370(13) 0.2556(8) 0.8691(7) 0.100 Uiso 0.50 1 d PD C 2 H333 H 0.7064 0.2352 0.8881 0.120 Uiso 0.50 1 calc PR C 2 H334 H 0.6975 0.2910 0.8596 0.120 Uiso 0.50 1 calc PR C 2 O53B O 0.7491(11) 0.2071(6) 0.8412(3) 0.100 Uiso 0.50 1 d PD C 2 C54B C 0.7763(15) 0.1465(7) 0.8559(5) 0.100 Uiso 0.50 1 d PD C 2 H335 H 0.8160 0.1563 0.8771 0.120 Uiso 0.50 1 calc PR C 2 H336 H 0.8163 0.1267 0.8395 0.120 Uiso 0.50 1 calc PR C 2 C55B C 0.7133(15) 0.0951(9) 0.8655(5) 0.100 Uiso 0.50 1 d PD C 2 H337 H 0.7109 0.0604 0.8480 0.120 Uiso 0.50 1 calc PR C 2 H338 H 0.6509 0.1126 0.8665 0.120 Uiso 0.50 1 calc PR C 2 O56B O 0.7477(11) 0.0687(7) 0.9004(3) 0.100 Uiso 0.50 1 d PD C 2 C57B C 0.8050(15) 0.1231(11) 0.9171(4) 0.100 Uiso 0.50 1 d PD C 2 H339 H 0.7933 0.1637 0.9043 0.120 Uiso 0.50 1 calc PR C 2 H340 H 0.8710 0.1129 0.9177 0.120 Uiso 0.50 1 calc PR C 2 C58B C 0.7740(14) 0.1282(11) 0.9543(4) 0.100 Uiso 0.50 1 d PD C 2 H341 H 0.7161 0.1526 0.9541 0.120 Uiso 0.50 1 calc PR C 2 H342 H 0.7640 0.0849 0.9638 0.120 Uiso 0.50 1 calc PR C 2 O59B O 0.8463(11) 0.1613(7) 0.9755(3) 0.100 Uiso 0.50 1 d PD C 2 C60B C 0.9040(12) 0.2004(9) 0.9552(6) 0.100 Uiso 0.50 1 d PD C 2 H343 H 0.9175 0.1779 0.9338 0.120 Uiso 0.50 1 calc PR C 2 H344 H 0.9625 0.2109 0.9687 0.120 Uiso 0.50 1 calc PR C 2 C61B C 0.8455(15) 0.2640(9) 0.9465(5) 0.100 Uiso 0.50 1 d PD C 2 H345 H 0.8818 0.3032 0.9521 0.120 Uiso 0.50 1 calc PR C 2 H346 H 0.8213 0.2652 0.9219 0.120 Uiso 0.50 1 calc PR C 2 O62B O 0.7699(10) 0.2562(7) 0.9702(4) 0.100 Uiso 0.50 1 d PD C 2 C63B C 0.7669(19) 0.3099(9) 0.9934(4) 0.118(10) Uiso 0.50 1 d PD C 2 H347 H 0.8287 0.3276 0.9996 0.142 Uiso 0.50 1 calc PR C 2 H348 H 0.7388 0.2978 1.0149 0.142 Uiso 0.50 1 calc PR C 2 C64B C 0.7031(13) 0.3603(8) 0.9703(5) 0.076(7) Uiso 0.50 1 d PD C 2 H349 H 0.6508 0.3380 0.9577 0.091 Uiso 0.50 1 calc PR C 2 H350 H 0.6792 0.3941 0.9851 0.091 Uiso 0.50 1 calc PR C 2 O65B O 0.7636(4) 0.3882(3) 0.94590(15) 0.0697(16) Uiso 0.50 1 d PD C 2 B1 B 0.3160 0.4043 0.2331 0.106 Uiso 1 1 d D . . C101 C 0.3794(5) 0.3748(3) 0.27291(15) 0.081(3) Uiso 1 1 d GD . . C102 C 0.3448(4) 0.3389(4) 0.30003(19) 0.096(3) Uiso 1 1 d GD . . H102 H 0.2812 0.3304 0.2997 0.115 Uiso 1 1 calc R . . C103 C 0.4053(6) 0.3156(4) 0.32767(17) 0.108(4) Uiso 1 1 d GD . . H103 H 0.3822 0.2916 0.3458 0.130 Uiso 1 1 calc R . . C104 C 0.5004(5) 0.3283(4) 0.32820(17) 0.114(4) Uiso 1 1 d GD . . H104 H 0.5409 0.3127 0.3467 0.137 Uiso 1 1 calc R . . C105 C 0.5350(4) 0.3642(4) 0.3011(2) 0.108(4) Uiso 1 1 d GD . . H105 H 0.5986 0.3727 0.3014 0.129 Uiso 1 1 calc R . . C106 C 0.4745(5) 0.3875(3) 0.27344(16) 0.086(3) Uiso 1 1 d GD . . H106 H 0.4976 0.4116 0.2553 0.103 Uiso 1 1 calc R . . C111 C 0.3132(4) 0.3400(2) 0.20732(14) 0.073(2) Uiso 1 1 d GD . . C112 C 0.3847(4) 0.2940(3) 0.20939(15) 0.076(3) Uiso 1 1 d GD . . H112 H 0.4328 0.2968 0.2273 0.092 Uiso 1 1 calc R . . C113 C 0.3843(5) 0.2437(3) 0.18470(19) 0.093(3) Uiso 1 1 d GD . . H113 H 0.4322 0.2129 0.1861 0.111 Uiso 1 1 calc R . . C114 C 0.3125(5) 0.2395(3) 0.15793(16) 0.099(3) Uiso 1 1 d GD . . H114 H 0.3123 0.2058 0.1414 0.118 Uiso 1 1 calc R . . C115 C 0.2411(5) 0.2855(3) 0.15586(16) 0.094(3) Uiso 1 1 d GD . . H115 H 0.1930 0.2827 0.1380 0.113 Uiso 1 1 calc R . . C116 C 0.2414(4) 0.3358(3) 0.18055(17) 0.081(3) Uiso 1 1 d GD . . H116 H 0.1936 0.3666 0.1792 0.097 Uiso 1 1 calc R . . C121 C 0.3400(4) 0.4721(3) 0.22286(16) 0.080(3) Uiso 1 1 d GD . . C122 C 0.3220(4) 0.4873(3) 0.18727(15) 0.067(2) Uiso 1 1 d GD . . H122 H 0.2946 0.4563 0.1717 0.081 Uiso 1 1 calc R . . C123 C 0.3448(5) 0.5489(3) 0.17492(13) 0.070(2) Uiso 1 1 d GD . . H123 H 0.3328 0.5591 0.1511 0.084 Uiso 1 1 calc R . . C124 C 0.3857(5) 0.5953(2) 0.19816(19) 0.099(3) Uiso 1 1 d GD . . H124 H 0.4010 0.6365 0.1899 0.119 Uiso 1 1 calc R . . C125 C 0.4037(6) 0.5801(3) 0.23374(18) 0.131(5) Uiso 1 1 d GD . . H125 H 0.4310 0.6111 0.2493 0.157 Uiso 1 1 calc R . . C126 C 0.3808(6) 0.5185(4) 0.24609(13) 0.114(4) Uiso 1 1 d GD . . H126 H 0.3929 0.5083 0.2699 0.137 Uiso 1 1 calc R . . C131 C 0.2005(4) 0.4053(4) 0.25004(17) 0.090(3) Uiso 1 1 d GD . . C132 C 0.1697(6) 0.4656(3) 0.2615(2) 0.108(4) Uiso 1 1 d GD . . H132 H 0.2087 0.5019 0.2617 0.130 Uiso 1 1 calc R . . C133 C 0.0806(7) 0.4715(4) 0.2729(3) 0.139(5) Uiso 1 1 d GD . . H133 H 0.0600 0.5118 0.2805 0.166 Uiso 1 1 calc R . . C134 C 0.0223(5) 0.4171(6) 0.2727(3) 0.144(6) Uiso 1 1 d GD . . H134 H -0.0373 0.4210 0.2802 0.173 Uiso 1 1 calc R . . C135 C 0.0532(6) 0.3568(5) 0.2612(3) 0.150(6) Uiso 1 1 d GD . . H135 H 0.0142 0.3204 0.2610 0.180 Uiso 1 1 calc R . . C136 C 0.1422(6) 0.3509(3) 0.2499(2) 0.116(4) Uiso 1 1 d GD . . H136 H 0.1629 0.3106 0.2422 0.139 Uiso 1 1 calc R . . B2 B 0.2339 0.2798 0.9491 0.069 Uiso 0.50 1 d PD D 1 C201 C 0.1632(7) 0.2420(4) 0.9167(2) 0.067(4) Uiso 0.50 1 d PGD D 1 C202 C 0.0873(9) 0.2038(6) 0.9242(2) 0.085(6) Uiso 0.50 1 d PGD D 1 H200 H 0.0746 0.1970 0.9476 0.102 Uiso 0.50 1 calc PR D 1 C203 C 0.0303(8) 0.1759(7) 0.8969(3) 0.109(8) Uiso 0.50 1 d PGD D 1 H201 H -0.0205 0.1503 0.9019 0.130 Uiso 0.50 1 calc PR D 1 C204 C 0.0492(8) 0.1861(6) 0.8620(3) 0.077(5) Uiso 0.50 1 d PGD D 1 H202 H 0.0111 0.1674 0.8437 0.093 Uiso 0.50 1 calc PR D 1 C205 C 0.1252(9) 0.2242(6) 0.8545(2) 0.088(6) Uiso 0.50 1 d PGD D 1 H203 H 0.1378 0.2311 0.8312 0.105 Uiso 0.50 1 calc PR D 1 C206 C 0.1821(7) 0.2522(5) 0.8818(3) 0.074(5) Uiso 0.50 1 d PGD D 1 H204 H 0.2329 0.2777 0.8768 0.088 Uiso 0.50 1 calc PR D 1 C211 C 0.1713(7) 0.3375(4) 0.9668(2) 0.061(4) Uiso 0.50 1 d PGD D 1 C212 C 0.0749(8) 0.3327(5) 0.9671(3) 0.066(5) Uiso 0.50 1 d PGD D 1 H205 H 0.0435 0.2968 0.9568 0.079 Uiso 0.50 1 calc PR D 1 C213 C 0.0254(6) 0.3817(6) 0.9829(3) 0.075(5) Uiso 0.50 1 d PGD D 1 H206 H -0.0390 0.3785 0.9831 0.090 Uiso 0.50 1 calc PR D 1 C214 C 0.0723(9) 0.4354(5) 0.9983(3) 0.077(5) Uiso 0.50 1 d PGD D 1 H207 H 0.0392 0.4681 1.0088 0.092 Uiso 0.50 1 calc PR D 1 C215 C 0.1687(9) 0.4401(5) 0.9980(3) 0.076(6) Uiso 0.50 1 d PGD D 1 H208 H 0.2000 0.4761 1.0083 0.091 Uiso 0.50 1 calc PR D 1 C216 C 0.2181(6) 0.3912(5) 0.9822(3) 0.058(4) Uiso 0.50 1 d PGD D 1 H209 H 0.2826 0.3944 0.9820 0.070 Uiso 0.50 1 calc PR D 1 C221 C 0.3262(5) 0.3031(4) 0.93124(19) 0.047(3) Uiso 0.50 1 d PGD D 1 C222 C 0.3282(6) 0.3652(4) 0.9163(2) 0.051(4) Uiso 0.50 1 d PGD D 1 H210 H 0.2775 0.3932 0.9173 0.061 Uiso 0.50 1 calc PR D 1 C223 C 0.4061(7) 0.3855(4) 0.8999(3) 0.056(4) Uiso 0.50 1 d PGD D 1 H211 H 0.4075 0.4270 0.8899 0.067 Uiso 0.50 1 calc PR D 1 C224 C 0.4820(6) 0.3437(5) 0.8984(2) 0.058(4) Uiso 0.50 1 d PGD D 1 H212 H 0.5341 0.3572 0.8874 0.070 Uiso 0.50 1 calc PR D 1 C225 C 0.4800(6) 0.2815(5) 0.9133(3) 0.055(4) Uiso 0.50 1 d PGD D 1 H213 H 0.5307 0.2536 0.9123 0.067 Uiso 0.50 1 calc PR D 1 C226 C 0.4021(7) 0.2613(4) 0.9297(3) 0.063(4) Uiso 0.50 1 d PGD D 1 H214 H 0.4007 0.2197 0.9397 0.075 Uiso 0.50 1 calc PR D 1 C231 C 0.2654(7) 0.2276(6) 0.9819(3) 0.089(6) Uiso 0.50 1 d PGD D 1 C232 C 0.2671(12) 0.1598(7) 0.9783(4) 0.123(9) Uiso 0.50 1 d PGD D 1 H215 H 0.2483 0.1406 0.9567 0.148 Uiso 0.50 1 calc PR D 1 C233 C 0.2969(14) 0.1208(6) 1.0070(5) 0.142(11) Uiso 0.50 1 d PGD D 1 H216 H 0.2980 0.0755 1.0046 0.171 Uiso 0.50 1 calc PR D 1 C234 C 0.3250(13) 0.1495(9) 1.0394(4) 0.169(14) Uiso 0.50 1 d PGD D 1 H217 H 0.3449 0.1234 1.0586 0.203 Uiso 0.50 1 calc PR D 1 C235 C 0.3232(13) 0.2173(10) 1.0430(3) 0.125(9) Uiso 0.50 1 d PGD D 1 H218 H 0.3420 0.2365 1.0646 0.150 Uiso 0.50 1 calc PR D 1 C236 C 0.2934(11) 0.2563(6) 1.0142(4) 0.099(7) Uiso 0.50 1 d PGD D 1 H219 H 0.2923 0.3017 1.0166 0.119 Uiso 0.50 1 calc PR D 1 B3 B 0.3812 0.3775 0.9840 0.111 Uiso 0.50 1 d PD . 2 C301 C 0.4619(7) 0.4333(4) 0.9942(2) 0.042(3) Uiso 0.50 1 d PGD . 2 C302 C 0.4304(6) 0.4898(5) 0.9766(2) 0.045(4) Uiso 0.50 1 d PGD . 2 H220 H 0.3762 0.4886 0.9614 0.054 Uiso 0.50 1 calc PR . 2 C303 C 0.4798(8) 0.5481(4) 0.9816(3) 0.052(4) Uiso 0.50 1 d PGD . 2 H221 H 0.4587 0.5858 0.9698 0.062 Uiso 0.50 1 calc PR . 2 C304 C 0.5608(8) 0.5498(4) 1.0043(3) 0.071(5) Uiso 0.50 1 d PGD . 2 H222 H 0.5939 0.5888 1.0077 0.085 Uiso 0.50 1 calc PR . 2 C305 C 0.5923(7) 0.4934(5) 1.0220(3) 0.077(6) Uiso 0.50 1 d PGD . 2 H223 H 0.6465 0.4946 1.0372 0.092 Uiso 0.50 1 calc PR . 2 C306 C 0.5429(7) 0.4351(4) 1.0169(3) 0.052(4) Uiso 0.50 1 d PGD . 2 H224 H 0.5640 0.3973 1.0288 0.062 Uiso 0.50 1 calc PR . 2 C311 C 0.4225(7) 0.3195(4) 1.0169(2) 0.058(4) Uiso 0.50 1 d PGD E 2 C312 C 0.5090(7) 0.2890(5) 1.0175(2) 0.064(4) Uiso 0.50 1 d PGD E 2 H225 H 0.5486 0.2980 0.9999 0.076 Uiso 0.50 1 calc PR E 2 C313 C 0.5366(6) 0.2452(5) 1.0444(3) 0.062(4) Uiso 0.50 1 d PGD E 2 H226 H 0.5945 0.2249 1.0448 0.075 Uiso 0.50 1 calc PR E 2 C314 C 0.4775(8) 0.2319(4) 1.0707(2) 0.066(4) Uiso 0.50 1 d PGD E 2 H227 H 0.4959 0.2026 1.0886 0.079 Uiso 0.50 1 calc PR E 2 C315 C 0.3909(7) 0.2623(5) 1.0700(2) 0.068(5) Uiso 0.50 1 d PGD E 2 H228 H 0.3514 0.2534 1.0876 0.081 Uiso 0.50 1 calc PR E 2 C316 C 0.3634(6) 0.3061(5) 1.0431(3) 0.060(4) Uiso 0.50 1 d PGD E 2 H229 H 0.3054 0.3265 1.0427 0.072 Uiso 0.50 1 calc PR E 2 C321 C 0.4205(6) 0.3486(5) 0.94584(18) 0.058(4) Uiso 0.50 1 d PGD F 2 C322 C 0.4391(8) 0.3947(4) 0.9205(2) 0.056(4) Uiso 0.50 1 d PGD F 2 H230 H 0.4298 0.4390 0.9247 0.068 Uiso 0.50 1 calc PR F 2 C323 C 0.4716(8) 0.3747(5) 0.8887(2) 0.054(4) Uiso 0.50 1 d PGD F 2 H231 H 0.4840 0.4056 0.8718 0.065 Uiso 0.50 1 calc PR F 2 C324 C 0.4855(8) 0.3084(6) 0.8824(2) 0.096(7) Uiso 0.50 1 d PGD F 2 H232 H 0.5072 0.2950 0.8612 0.115 Uiso 0.50 1 calc PR F 2 C325 C 0.4669(10) 0.2623(4) 0.9078(3) 0.081(6) Uiso 0.50 1 d PGD F 2 H233 H 0.4762 0.2180 0.9035 0.098 Uiso 0.50 1 calc PR F 2 C326 C 0.4344(9) 0.2823(4) 0.9395(2) 0.064(4) Uiso 0.50 1 d PGD F 2 H234 H 0.4219 0.2514 0.9565 0.077 Uiso 0.50 1 calc PR F 2 C331 C 0.2748(6) 0.3793(5) 0.9837(2) 0.061(4) Uiso 0.50 1 d PGD G 2 C332 C 0.2237(8) 0.3289(5) 0.9668(3) 0.085(6) Uiso 0.50 1 d PGD G 2 H235 H 0.2541 0.2959 0.9554 0.102 Uiso 0.50 1 calc PR G 2 C333 C 0.1271(8) 0.3280(6) 0.9669(4) 0.081(6) Uiso 0.50 1 d PGD G 2 H236 H 0.0928 0.2943 0.9555 0.098 Uiso 0.50 1 calc PR G 2 C334 C 0.0816(6) 0.3774(7) 0.9838(4) 0.098(7) Uiso 0.50 1 d PGD G 2 H237 H 0.0169 0.3768 0.9839 0.117 Uiso 0.50 1 calc PR G 2 C335 C 0.1327(7) 0.4278(6) 1.0008(3) 0.059(4) Uiso 0.50 1 d PGD G 2 H238 H 0.1023 0.4608 1.0121 0.071 Uiso 0.50 1 calc PR G 2 C336 C 0.2294(7) 0.4287(5) 1.0007(3) 0.064(4) Uiso 0.50 1 d PGD G 2 H239 H 0.2636 0.4624 1.0121 0.077 Uiso 0.50 1 calc PR G 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 0.0418(8) 0.0839(9) 0.0581(7) -0.0092(6) 0.0133(5) -0.0073(6) Cu2 0.0484(8) 0.0713(8) 0.0635(7) 0.0009(6) 0.0230(6) -0.0056(6) N11 0.030(4) 0.077(5) 0.058(4) -0.001(3) 0.014(3) -0.001(3) C12 0.033(5) 0.069(5) 0.056(5) 0.012(4) 0.005(3) -0.005(4) C13 0.036(5) 0.107(7) 0.056(5) 0.008(4) 0.007(4) 0.001(5) C14 0.047(6) 0.101(7) 0.073(6) 0.016(5) 0.002(5) -0.017(5) C15 0.037(6) 0.096(7) 0.076(6) 0.020(5) 0.021(4) 0.001(5) C16 0.046(6) 0.084(7) 0.083(6) 0.013(5) 0.016(5) -0.003(5) N21 0.026(4) 0.082(5) 0.047(3) 0.002(3) 0.008(3) -0.009(3) C22 0.029(5) 0.074(5) 0.053(4) -0.002(4) 0.005(3) -0.012(4) S23 0.0416(13) 0.0775(14) 0.0508(11) -0.0026(9) 0.0098(8) -0.0078(10) C24 0.048(6) 0.065(5) 0.059(5) 0.001(4) 0.009(4) -0.010(4) C25 0.037(5) 0.070(5) 0.057(5) 0.009(4) 0.003(4) -0.007(4) N31 0.032(4) 0.073(4) 0.050(4) -0.006(3) 0.018(3) -0.002(3) C32 0.047(6) 0.065(5) 0.049(4) -0.004(4) 0.016(3) -0.011(4) C33 0.040(6) 0.087(6) 0.064(5) -0.017(4) 0.012(4) -0.027(5) C34 0.057(6) 0.066(5) 0.060(5) -0.015(4) 0.012(4) -0.004(5) C35 0.049(6) 0.073(6) 0.058(5) -0.003(4) 0.022(4) -0.008(4) C36 0.051(6) 0.071(6) 0.045(4) -0.003(3) 0.010(3) -0.012(4) N41 0.049(5) 0.083(5) 0.060(4) -0.001(4) 0.015(3) -0.004(4) C42 0.036(5) 0.084(6) 0.052(4) -0.003(4) 0.019(3) -0.006(4) C43 0.045(6) 0.098(7) 0.053(5) 0.003(4) 0.008(4) -0.019(5) C44 0.038(6) 0.115(8) 0.065(5) 0.020(5) 0.019(4) -0.016(5) C45 0.047(6) 0.139(10) 0.079(6) 0.045(6) 0.020(5) 0.010(6) C46 0.052(7) 0.103(7) 0.066(5) 0.025(5) 0.027(4) 0.020(5) N51 0.047(5) 0.078(5) 0.062(4) -0.006(3) 0.011(3) 0.003(4) C52 0.043(5) 0.073(5) 0.058(5) -0.006(4) 0.015(4) 0.002(4) C53 0.046(6) 0.089(7) 0.075(6) -0.022(5) 0.006(4) -0.004(5) C54 0.065(7) 0.087(7) 0.080(6) -0.022(5) 0.005(5) 0.016(5) C55 0.061(7) 0.113(8) 0.084(7) -0.016(6) 0.014(5) 0.024(6) C56 0.051(6) 0.099(7) 0.076(6) -0.012(5) 0.012(5) 0.015(5) N61 0.043(4) 0.070(4) 0.051(4) -0.008(3) -0.003(3) -0.002(3) C62 0.042(5) 0.078(6) 0.049(4) -0.008(4) 0.012(3) 0.005(4) C63 0.056(6) 0.081(6) 0.045(4) -0.020(4) 0.010(4) -0.014(5) C64 0.045(6) 0.091(7) 0.058(5) -0.003(4) 0.018(4) -0.022(5) C65 0.032(5) 0.089(6) 0.049(4) -0.004(4) 0.013(3) 0.000(4) C66 0.032(5) 0.069(5) 0.048(4) -0.005(3) 0.010(3) 0.007(4) N71 0.041(4) 0.073(5) 0.050(4) 0.001(3) 0.015(3) -0.006(3) C72 0.038(5) 0.069(5) 0.061(5) 0.001(4) 0.008(4) -0.002(4) S73 0.0438(13) 0.0854(15) 0.0575(12) 0.0029(10) 0.0172(9) -0.0071(11) C74 0.065(6) 0.075(6) 0.064(5) -0.001(4) 0.012(4) -0.019(5) C75 0.063(6) 0.078(6) 0.051(5) -0.004(4) 0.013(4) -0.019(5) N81 0.069(5) 0.078(5) 0.054(4) 0.001(3) 0.029(4) -0.014(4) C82 0.090(8) 0.076(7) 0.061(5) -0.012(4) 0.026(5) -0.020(6) C83 0.189(15) 0.102(9) 0.076(7) -0.009(6) 0.073(9) -0.045(9) C84 0.24(2) 0.093(9) 0.110(10) -0.044(7) 0.101(12) -0.065(11) C85 0.184(15) 0.083(8) 0.094(8) -0.016(6) 0.076(9) -0.035(9) C86 0.082(8) 0.093(7) 0.060(5) -0.014(5) 0.031(5) -0.012(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N51 1.976(7) . ? Cu1 N21 2.021(6) . ? Cu1 N11 2.067(7) . ? Cu1 N61 2.211(6) . ? Cu2 N41 1.993(8) . ? Cu2 N71 2.032(6) . ? Cu2 N81 2.070(7) . ? Cu2 N31 2.143(7) . ? N11 C12 1.349(10) . ? N11 C16 1.365(11) . ? C12 C13 1.388(12) . ? C12 C25 1.476(12) . ? C13 C14 1.363(12) . ? C14 C15 1.366(14) . ? C15 C16 1.365(13) . ? N21 C22 1.305(10) . ? N21 C25 1.381(10) . ? C22 C36 1.478(11) . ? C22 S23 1.728(8) . ? S23 C24 1.712(9) . ? C24 C25 1.377(11) . ? N31 C32 1.346(10) . ? N31 C36 1.353(11) . ? C32 C33 1.374(12) . ? C32 C42 1.473(12) . ? C33 O65A 1.361(10) . ? C33 C34 1.370(12) . ? C34 C35 1.369(12) . ? C35 C36 1.392(12) . ? N41 C46 1.338(11) . ? N41 C42 1.354(11) . ? C42 C43 1.415(12) . ? C43 O50A 1.319(11) . ? C43 C44 1.397(14) . ? C44 C45 1.362(14) . ? C45 C46 1.385(13) . ? N51 C56 1.347(11) . ? N51 C52 1.353(11) . ? C52 C53 1.432(11) . ? C52 C62 1.453(12) . ? C53 O400 1.357(11) . ? C53 C54 1.371(13) . ? C54 C55 1.422(14) . ? C55 C56 1.369(13) . ? N61 C66 1.338(10) . ? N61 C62 1.371(11) . ? C62 C63 1.376(12) . ? C63 O414 1.369(10) . ? C63 C64 1.398(13) . ? C64 C65 1.402(12) . ? C65 C66 1.371(11) . ? C66 C72 1.467(12) . ? N71 C72 1.291(10) . ? N71 C75 1.383(11) . ? C72 S73 1.733(9) . ? S73 C74 1.709(10) . ? C74 C75 1.376(12) . ? C75 C82 1.463(12) . ? N81 C86 1.311(11) . ? N81 C82 1.342(11) . ? C82 C83 1.392(15) . ? C83 C84 1.360(15) . ? C84 C85 1.390(15) . ? C85 C86 1.361(15) . ? O400 C401 1.434(11) . ? C401 C402 1.488(15) . ? C402 O403 1.435(13) . ? O403 C404 1.453(15) . ? C404 C405 1.448(18) . ? C405 O406 1.460(16) . ? O406 C407 1.48(2) . ? C407 C408 1.26(2) . ? C408 O409 1.318(18) . ? O409 C410 1.373(16) . ? C410 C411 1.379(14) . ? C411 O40B 1.298(13) . ? C411 O40A 1.550(13) . ? O40A C41A 1.413(13) . ? C41A C42A 1.446(15) . ? C42A O414 1.473(14) . ? O40B C41B 1.441(15) . ? C41B C42B 1.452(17) . ? C42B O414 1.419(15) . ? O50A C51A 1.449(14) . ? C51A C52A 1.461(15) . ? C52A O53A 1.416(17) . ? O53A C54A 1.401(15) . ? C54A C55A 1.494(16) . ? C55A O56A 1.411(15) . ? O56A C57A 1.403(15) . ? C57A C58A 1.458(17) . ? C58A O59A 1.414(15) . ? O59A C60A 1.339(16) . ? C60A C61A 1.547(16) . ? C61A O62A 1.323(16) . ? O62A C63A 1.396(17) . ? C63A C64A 1.502(18) . ? C64A O65A 1.392(15) . ? C51B C52B 1.488(13) . ? C52B O53B 1.470(13) . ? O53B C54B 1.398(12) . ? C54B C55B 1.452(16) . ? C55B O56B 1.476(15) . ? O56B C57B 1.491(16) . ? C57B C58B 1.521(17) . ? C58B O59B 1.431(15) . ? O59B C60B 1.424(15) . ? C60B C61B 1.566(16) . ? C61B O62B 1.474(15) . ? O62B C63B 1.410(17) . ? C63B C64B 1.594(17) . ? B1 C121 1.487(5) . ? B1 C111 1.637(4) . ? B1 C101 1.801(5) . ? B1 C131 1.831(6) . ? C101 C102 1.3900 . ? C101 C106 1.3900 . ? C102 C103 1.3900 . ? C103 C104 1.3900 . ? C104 C105 1.3900 . ? C105 C106 1.3900 . ? C111 C112 1.3900 . ? C111 C116 1.3900 . ? C112 C113 1.3900 . ? C113 C114 1.3900 . ? C114 C115 1.3900 . ? C115 C116 1.3900 . ? C121 C122 1.3900 . ? C121 C126 1.3900 . ? C122 C123 1.3900 . ? C123 C124 1.3900 . ? C124 C125 1.3900 . ? C125 C126 1.3900 . ? C131 C132 1.3900 . ? C131 C136 1.3900 . ? C132 C133 1.3900 . ? C133 C134 1.3900 . ? C134 C135 1.3900 . ? C135 C136 1.3900 . ? B2 C221 1.612(7) . ? B2 C211 1.661(7) . ? B2 C231 1.673(9) . ? B2 C201 1.712(7) . ? C201 C202 1.3900 . ? C201 C206 1.3900 . ? C202 C203 1.3900 . ? C203 C204 1.3900 . ? C204 C205 1.3900 . ? C205 C206 1.3900 . ? C211 C212 1.3900 . ? C211 C216 1.3900 . ? C212 C213 1.3900 . ? C213 C214 1.3900 . ? C214 C215 1.3900 . ? C215 C216 1.3900 . ? C221 C222 1.3900 . ? C221 C226 1.3900 . ? C222 C223 1.3900 . ? C223 C224 1.3900 . ? C224 C225 1.3900 . ? C225 C226 1.3900 . ? C231 C232 1.3900 . ? C231 C236 1.3900 . ? C232 C233 1.3900 . ? C233 C234 1.3900 . ? C234 C235 1.3900 . ? C235 C236 1.3900 . ? B3 C331 1.529(8) . ? B3 C301 1.650(8) . ? B3 C321 1.705(7) . ? B3 C304 1.740(8) 3_667 ? B3 C311 1.785(6) . ? C301 C304 0.480(18) 3_667 ? C301 C303 1.248(18) 3_667 ? C301 C302 1.3900 . ? C301 C306 1.3900 . ? C301 C305 1.773(18) 3_667 ? C302 C303 1.3900 . ? C303 C304 1.3900 . ? C304 C305 1.3900 . ? C304 B3 1.740(8) 3_667 ? C305 C306 1.3900 . ? C311 C312 1.3900 . ? C311 C316 1.3900 . ? C312 C313 1.3900 . ? C313 C314 1.3900 . ? C314 C315 1.3900 . ? C315 C316 1.3900 . ? C321 C322 1.3900 . ? C321 C326 1.3900 . ? C322 C323 1.3900 . ? C323 C324 1.3900 . ? C324 C325 1.3900 . ? C325 C326 1.3900 . ? C331 C332 1.3900 . ? C331 C336 1.3900 . ? C332 C333 1.3900 . ? C333 C334 1.3900 . ? C334 C335 1.3900 . ? C335 C336 1.3900 . ? 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 N51 Cu1 N21 149.7(3) . . ? N51 Cu1 N11 120.0(3) . . ? N21 Cu1 N11 81.4(3) . . ? N51 Cu1 N61 81.3(3) . . ? N21 Cu1 N61 101.6(3) . . ? N11 Cu1 N61 129.9(3) . . ? N41 Cu2 N71 141.3(3) . . ? N41 Cu2 N81 119.8(3) . . ? N71 Cu2 N81 82.3(3) . . ? N41 Cu2 N31 81.9(3) . . ? N71 Cu2 N31 103.8(3) . . ? N81 Cu2 N31 136.9(3) . . ? C12 N11 C16 116.6(7) . . ? C12 N11 Cu1 114.2(5) . . ? C16 N11 Cu1 129.2(6) . . ? N11 C12 C13 122.6(8) . . ? N11 C12 C25 114.0(7) . . ? C13 C12 C25 123.3(8) . . ? C14 C13 C12 119.3(9) . . ? C15 C14 C13 118.9(9) . . ? C14 C15 C16 120.0(9) . . ? N11 C16 C15 122.5(10) . . ? C22 N21 C25 111.8(7) . . ? C22 N21 Cu1 134.8(5) . . ? C25 N21 Cu1 112.3(5) . . ? N21 C22 C36 123.9(7) . . ? N21 C22 S23 113.8(6) . . ? C36 C22 S23 122.3(6) . . ? C24 S23 C22 90.1(4) . . ? C25 C24 S23 109.8(6) . . ? N21 C25 C24 114.4(7) . . ? N21 C25 C12 117.6(7) . . ? C24 C25 C12 127.9(8) . . ? C32 N31 C36 118.2(7) . . ? C32 N31 Cu2 106.5(5) . . ? C36 N31 Cu2 124.4(5) . . ? N31 C32 C33 121.1(8) . . ? N31 C32 C42 113.6(7) . . ? C33 C32 C42 124.8(8) . . ? O65A C33 C34 124.1(8) . . ? O65A C33 C32 115.7(8) . . ? C34 C33 C32 120.1(8) . . ? C33 C34 C35 120.2(8) . . ? C34 C35 C36 117.3(8) . . ? N31 C36 C35 123.0(8) . . ? N31 C36 C22 116.9(7) . . ? C35 C36 C22 120.1(8) . . ? C46 N41 C42 119.9(8) . . ? C46 N41 Cu2 125.4(7) . . ? C42 N41 Cu2 111.7(6) . . ? N41 C42 C43 121.7(8) . . ? N41 C42 C32 115.5(7) . . ? C43 C42 C32 122.7(8) . . ? O50A C43 C44 127.1(8) . . ? O50A C43 C42 116.4(9) . . ? C44 C43 C42 116.4(9) . . ? C45 C44 C43 120.7(9) . . ? C44 C45 C46 119.9(10) . . ? N41 C46 C45 120.9(9) . . ? C56 N51 C52 119.9(7) . . ? C56 N51 Cu1 124.1(6) . . ? C52 N51 Cu1 112.9(6) . . ? N51 C52 C53 120.3(8) . . ? N51 C52 C62 115.5(7) . . ? C53 C52 C62 124.1(8) . . ? O400 C53 C54 125.4(8) . . ? O400 C53 C52 115.4(8) . . ? C54 C53 C52 119.0(8) . . ? C53 C54 C55 118.5(9) . . ? C56 C55 C54 119.6(9) . . ? N51 C56 C55 121.9(9) . . ? C66 N61 C62 118.1(7) . . ? C66 N61 Cu1 123.9(5) . . ? C62 N61 Cu1 103.6(5) . . ? N61 C62 C63 121.0(7) . . ? N61 C62 C52 113.8(7) . . ? C63 C62 C52 124.9(8) . . ? O414 C63 C62 116.5(8) . . ? O414 C63 C64 122.9(8) . . ? C62 C63 C64 120.6(8) . . ? C63 C64 C65 117.4(8) . . ? C66 C65 C64 119.1(8) . . ? N61 C66 C65 123.6(8) . . ? N61 C66 C72 116.4(7) . . ? C65 C66 C72 119.9(7) . . ? C72 N71 C75 111.4(7) . . ? C72 N71 Cu2 135.3(6) . . ? C75 N71 Cu2 111.1(5) . . ? N71 C72 C66 123.7(8) . . ? N71 C72 S73 114.3(6) . . ? C66 C72 S73 122.0(6) . . ? C74 S73 C72 90.1(4) . . ? C75 C74 S73 109.3(7) . . ? C74 C75 N71 114.9(8) . . ? C74 C75 C82 128.1(8) . . ? N71 C75 C82 117.0(8) . . ? C86 N81 C82 120.5(8) . . ? C86 N81 Cu2 126.9(6) . . ? C82 N81 Cu2 112.1(6) . . ? N81 C82 C83 119.4(9) . . ? N81 C82 C75 116.2(8) . . ? C83 C82 C75 124.3(9) . . ? C84 C83 C82 120.1(10) . . ? C83 C84 C85 118.8(11) . . ? C86 C85 C84 118.3(10) . . ? N81 C86 C85 122.8(10) . . ? C53 O400 C401 117.7(8) . . ? O400 C401 C402 108.2(9) . . ? O403 C402 C401 107.5(9) . . ? C402 O403 C404 109.8(9) . . ? C405 C404 O403 104.0(11) . . ? C404 C405 O406 111.5(12) . . ? C405 O406 C407 116.2(12) . . ? C408 C407 O406 123.3(19) . . ? C407 C408 O409 114.7(19) . . ? C408 O409 C410 124.9(14) . . ? O409 C410 C411 107.5(15) . . ? O40B C411 C410 145.8(16) . . ? O40B C411 O40A 41.7(4) . . ? C410 C411 O40A 109.2(13) . . ? C41A O40A C411 111.6(10) . . ? O40A C41A C42A 117.5(13) . . ? C41A C42A O414 119.6(13) . . ? C411 O40B C41B 108.4(12) . . ? O40B C41B C42B 112.7(15) . . ? O414 C42B C41B 106.8(14) . . ? C63 O414 C42B 124.0(13) . . ? C63 O414 C42A 111.6(8) . . ? C42B O414 C42A 63.6(10) . . ? C43 O50A C51A 117.6(8) . . ? O50A C51A C52A 111.1(13) . . ? O53A C52A C51A 113.8(15) . . ? C54A O53A C52A 117.4(14) . . ? O53A C54A C55A 114.4(15) . . ? O56A C55A C54A 111.1(13) . . ? C57A O56A C55A 115.6(14) . . ? O56A C57A C58A 116.6(16) . . ? O59A C58A C57A 116.5(15) . . ? C60A O59A C58A 121.3(16) . . ? O59A C60A C61A 115.0(16) . . ? O62A C61A C60A 110.6(15) . . ? C61A O62A C63A 124.0(16) . . ? O62A C63A C64A 112.4(17) . . ? O65A C64A C63A 110.1(15) . . ? C33 O65A C64A 119.8(10) . . ? O53B C52B C51B 110.8(12) . . ? C54B O53B C52B 110.8(12) . . ? O53B C54B C55B 125.4(17) . . ? C54B C55B O56B 108.7(13) . . ? C55B O56B C57B 104.1(11) . . ? O56B C57B C58B 104.6(13) . . ? O59B C58B C57B 107.5(12) . . ? C60B O59B C58B 112.9(13) . . ? O59B C60B C61B 104.5(11) . . ? O62B C61B C60B 101.2(11) . . ? C63B O62B C61B 111.2(14) . . ? O62B C63B C64B 101.7(14) . . ? C121 B1 C111 125.7(3) . . ? C121 B1 C101 114.8(3) . . ? C111 B1 C101 102.8(3) . . ? C121 B1 C131 108.6(3) . . ? C111 B1 C131 104.0(3) . . ? C101 B1 C131 96.9(3) . . ? C102 C101 C106 120.0 . . ? C102 C101 B1 127.6(4) . . ? C106 C101 B1 112.2(4) . . ? C101 C102 C103 120.0 . . ? C104 C103 C102 120.0 . . ? C103 C104 C105 120.0 . . ? C106 C105 C104 120.0 . . ? C105 C106 C101 120.0 . . ? C112 C111 C116 120.0 . . ? C112 C111 B1 121.8(4) . . ? C116 C111 B1 117.9(4) . . ? C113 C112 C111 120.0 . . ? C112 C113 C114 120.0 . . ? C115 C114 C113 120.0 . . ? C114 C115 C116 120.0 . . ? C115 C116 C111 120.0 . . ? C122 C121 C126 120.0 . . ? C122 C121 B1 115.8(4) . . ? C126 C121 B1 124.2(4) . . ? C121 C122 C123 120.0 . . ? C124 C123 C122 120.0 . . ? C123 C124 C125 120.0 . . ? C126 C125 C124 120.0 . . ? C125 C126 C121 120.0 . . ? C132 C131 C136 120.0 . . ? C132 C131 B1 116.3(5) . . ? C136 C131 B1 123.6(5) . . ? C131 C132 C133 120.0 . . ? C132 C133 C134 120.0 . . ? C133 C134 C135 120.0 . . ? C136 C135 C134 120.0 . . ? C135 C136 C131 120.0 . . ? C221 B2 C211 117.0(5) . . ? C221 B2 C231 108.7(4) . . ? C211 B2 C231 105.7(5) . . ? C221 B2 C201 107.0(5) . . ? C211 B2 C201 107.6(5) . . ? C231 B2 C201 110.9(6) . . ? C202 C201 C206 120.0 . . ? C202 C201 B2 122.3(7) . . ? C206 C201 B2 117.7(7) . . ? C201 C202 C203 120.0 . . ? C204 C203 C202 120.0 . . ? C205 C204 C203 120.0 . . ? C204 C205 C206 120.0 . . ? C205 C206 C201 120.0 . . ? C212 C211 C216 120.0 . . ? C212 C211 B2 121.9(7) . . ? C216 C211 B2 118.1(7) . . ? C213 C212 C211 120.0 . . ? C212 C213 C214 120.0 . . ? C215 C214 C213 120.0 . . ? C214 C215 C216 120.0 . . ? C215 C216 C211 120.0 . . ? C222 C221 C226 120.0 . . ? C222 C221 B2 119.1(6) . . ? C226 C221 B2 120.8(6) . . ? C223 C222 C221 120.0 . . ? C222 C223 C224 120.0 . . ? C223 C224 C225 120.0 . . ? C226 C225 C224 120.0 . . ? C225 C226 C221 120.0 . . ? C232 C231 C236 120.0 . . ? C232 C231 B2 124.5(9) . . ? C236 C231 B2 115.5(9) . . ? C231 C232 C233 120.0 . . ? C234 C233 C232 120.0 . . ? C233 C234 C235 120.0 . . ? C236 C235 C234 120.0 . . ? C235 C236 C231 120.0 . . ? C331 B3 C301 131.9(5) . . ? C331 B3 C321 113.9(5) . . ? C301 B3 C321 99.4(4) . . ? C331 B3 C304 116.0(5) . 3_667 ? C301 B3 C304 16.0(6) . 3_667 ? C321 B3 C304 109.0(4) . 3_667 ? C331 B3 C311 107.1(4) . . ? C301 B3 C311 96.1(4) . . ? C321 B3 C311 104.5(4) . . ? C304 B3 C311 105.2(4) 3_667 . ? C304 C301 C303 97(2) 3_667 3_667 ? C304 C301 C302 43(2) 3_667 . ? C303 C301 C302 105.9(8) 3_667 . ? C304 C301 C306 117(2) 3_667 . ? C303 C301 C306 20.0(8) 3_667 . ? C302 C301 C306 120.0 . . ? C304 C301 B3 93(2) 3_667 . ? C303 C301 B3 143.1(10) 3_667 . ? C302 C301 B3 105.3(5) . . ? C306 C301 B3 134.5(5) . . ? C304 C301 C305 32.0(16) 3_667 3_667 ? C303 C301 C305 104.3(10) 3_667 3_667 ? C302 C301 C305 10.5(7) . 3_667 ? C306 C301 C305 121.0(7) . 3_667 ? B3 C301 C305 102.7(7) . 3_667 ? C303 C302 C301 120.0 . . ? C302 C303 C304 120.0 . . ? C305 C304 C303 120.0 . . ? C305 C304 B3 117.0(6) . 3_667 ? C303 C304 B3 122.6(6) . 3_667 ? C306 C305 C304 120.0 . . ? C305 C306 C301 120.0 . . ? C312 C311 C316 120.0 . . ? C312 C311 B3 123.6(6) . . ? C316 C311 B3 116.4(6) . . ? C311 C312 C313 120.0 . . ? C314 C313 C312 120.0 . . ? C313 C314 C315 120.0 . . ? C316 C315 C314 120.0 . . ? C315 C316 C311 120.0 . . ? C322 C321 C326 120.0 . . ? C322 C321 B3 116.9(6) . . ? C326 C321 B3 123.1(6) . . ? C323 C322 C321 120.0 . . ? C322 C323 C324 120.0 . . ? C325 C324 C323 120.0 . . ? C324 C325 C326 120.0 . . ? C325 C326 C321 120.0 . . ? C332 C331 C336 120.0 . . ? C332 C331 B3 118.4(7) . . ? C336 C331 B3 121.6(7) . . ? C331 C332 C333 120.0 . . ? C334 C333 C332 120.0 . . ? C333 C334 C335 120.0 . . ? C336 C335 C334 120.0 . . ? C335 C336 C331 120.0 . . ? _diffrn_measured_fraction_theta_max 0.860 _diffrn_reflns_theta_full 70.40 _diffrn_measured_fraction_theta_full 0.860 _refine_diff_density_max 1.630 _refine_diff_density_min -1.519 _refine_diff_density_rms 0.144 # Attachment 'Cu2L2Ba2.cif' data_sad _database_code_depnum_ccdc_archive 'CCDC 285238' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H84 Ba2 Cl6 Cu2 N12 O38 S2' _chemical_formula_weight 2380.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -1.0456 8.4617 '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 11.5874(7) _cell_length_b 12.9425(8) _cell_length_c 16.1980(10) _cell_angle_alpha 86.496(2) _cell_angle_beta 88.891(2) _cell_angle_gamma 66.515(2) _cell_volume 2223.8(2) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5412 _cell_measurement_theta_min 7.458 _cell_measurement_theta_max 140.002 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.777 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1196 _exptl_absorpt_coefficient_mu 10.266 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.282579 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2001)' _exptl_special_details ; Disorder was identified in two perchlorate anions [ClO4(1) and (2)]. Whilst attempts to model disoreder in ClO4(1) were deemed unecessary, the latter, more severely disordered anion ClO4(2) was modelled by treating the anion as two components (a) and (b), with 0.6 and 0.4 site occupancies respectively. In addition, the anisotropic displacement parameters on the oxygen atoms of ClO4(2) were restrained (ISOR and DELU). No geometric restraints were applied. Attempts at modelling an extensively disordered acetone/solvent molecule were unsuccessful and a diffuse solvent correction was employed using the SQUEEZE routine in PLATON (Spek, A. L. Acta. Cryst. 1990, A46, C-34). The empirical formula is thus necessarily an estimate and includes one additional acetone moiety per asymmetric unit. The given/calculated molecular weight is thus also spurious. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source '4.8 kW rotating anode' _diffrn_radiation_monochromator 'Osmic ConFocal MaxFlux mirror optics' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Frames, each covering 0.3 \% in \w' _diffrn_detector_area_resol_mean 5.6 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17363 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0522 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 70.15 _reflns_number_total 7570 _reflns_number_gt 6354 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement 'SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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^)+(0.0754P)^2^+2.4310P] 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 7570 _refine_ls_number_parameters 588 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1151 _refine_ls_wR_factor_gt 0.1082 _refine_ls_goodness_of_fit_ref 0.916 _refine_ls_restrained_S_all 0.913 _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 -0.10384(6) 0.73215(5) 0.82085(3) 0.03245(16) Uani 1 1 d . . . Ba1 Ba 0.48395(2) 0.41793(2) 0.697399(16) 0.03753(10) Uani 1 1 d . . . N11 N -0.0166(3) 0.8414(3) 0.7820(2) 0.0362(8) Uani 1 1 d . . . C12 C 0.0434(4) 0.8662(4) 0.8424(3) 0.0348(10) Uani 1 1 d . . . C13 C 0.1117(4) 0.9323(4) 0.8271(3) 0.0401(10) Uani 1 1 d . . . H1 H 0.1523 0.9487 0.8702 0.048 Uiso 1 1 calc R . . C14 C 0.1189(4) 0.9733(4) 0.7476(3) 0.0434(12) Uani 1 1 d . . . H2 H 0.1639 1.0181 0.7364 0.052 Uiso 1 1 calc R . . C15 C 0.0579(5) 0.9470(4) 0.6845(3) 0.0415(11) Uani 1 1 d . . . H3 H 0.0627 0.9725 0.6301 0.050 Uiso 1 1 calc R . . C16 C -0.0101(4) 0.8819(4) 0.7041(3) 0.0391(10) Uani 1 1 d . . . H4 H -0.0528 0.8656 0.6622 0.047 Uiso 1 1 calc R . . N21 N -0.0303(3) 0.7449(3) 0.9318(2) 0.0294(7) Uani 1 1 d . . . C22 C -0.0262(4) 0.7028(4) 1.0087(2) 0.0312(9) Uani 1 1 d . . . S23 S 0.05933(12) 0.74507(11) 1.07553(7) 0.0419(3) Uani 1 1 d . . . C24 C 0.0886(5) 0.8248(4) 0.9968(3) 0.0418(11) Uani 1 1 d . . . H5 H 0.1347 0.8687 1.0021 0.050 Uiso 1 1 calc R . . C25 C 0.0351(4) 0.8152(4) 0.9254(3) 0.0339(9) Uani 1 1 d . . . N31 N 0.0592(3) 0.4100(3) 0.88089(19) 0.0291(7) Uani 1 1 d . . . C32 C 0.1167(4) 0.4715(4) 0.8458(2) 0.0294(9) Uani 1 1 d . . . C33 C 0.2088(4) 0.4941(4) 0.8868(3) 0.0325(9) Uani 1 1 d . . . C34 C 0.2360(4) 0.4545(4) 0.9687(3) 0.0365(10) Uani 1 1 d . . . H6 H 0.2946 0.4700 0.9983 0.044 Uiso 1 1 calc R . . C35 C -0.1747(4) 0.6085(4) 0.9944(2) 0.0348(10) Uani 1 1 d . . . H7 H -0.1912 0.6354 0.9395 0.042 Uiso 1 1 calc R . . C36 C -0.0885(4) 0.6310(3) 1.0401(2) 0.0298(9) Uani 1 1 d . . . N41 N -0.0261(3) 0.6035(3) 0.7425(2) 0.0294(7) Uani 1 1 d . . . C42 C 0.0797(4) 0.5119(4) 0.7575(2) 0.0292(9) Uani 1 1 d . A . C43 C 0.1521(4) 0.4507(4) 0.6946(3) 0.0323(9) Uani 1 1 d . . . C44 C 0.1102(4) 0.4783(4) 0.6134(3) 0.0367(10) Uani 1 1 d . A . H8 H 0.1555 0.4356 0.5705 0.044 Uiso 1 1 calc R . . C45 C -0.0005(4) 0.5709(4) 0.5982(3) 0.0384(10) Uani 1 1 d . . . H9 H -0.0314 0.5918 0.5445 0.046 Uiso 1 1 calc R A . C46 C -0.0652(4) 0.6328(4) 0.6632(2) 0.0329(9) Uani 1 1 d . A . H10 H -0.1383 0.6968 0.6520 0.039 Uiso 1 1 calc R . . O100 O 0.2654(3) 0.5525(3) 0.84195(17) 0.0369(7) Uani 1 1 d . . . C101 C 0.3346(4) 0.6000(4) 0.8891(3) 0.0362(10) Uani 1 1 d . A . H11A H 0.4042 0.5403 0.9180 0.043 Uiso 1 1 calc R . . H12B H 0.2802 0.6483 0.9297 0.043 Uiso 1 1 calc R . . C102 C 0.3835(4) 0.6679(4) 0.8295(3) 0.0338(9) Uani 1 1 d . . . H13A H 0.3181 0.7109 0.7897 0.041 Uiso 1 1 calc R A . H14B H 0.4036 0.7209 0.8600 0.041 Uiso 1 1 calc R . . O103 O 0.4939(3) 0.5972(2) 0.78622(17) 0.0325(6) Uani 1 1 d . A . C104 C 0.6066(4) 0.5667(4) 0.8348(3) 0.0347(9) Uani 1 1 d . . . H15A H 0.6071 0.5146 0.8806 0.042 Uiso 1 1 calc R A . H16B H 0.6093 0.6335 0.8573 0.042 Uiso 1 1 calc R . . C105 C 0.7183(4) 0.5129(4) 0.7814(3) 0.0368(10) Uani 1 1 d . A . H17A H 0.7144 0.5622 0.7331 0.044 Uiso 1 1 calc R . . H18B H 0.7950 0.4989 0.8118 0.044 Uiso 1 1 calc R . . O106 O 0.7175(3) 0.4091(3) 0.75703(19) 0.0372(7) Uani 1 1 d . A . C107 C 0.8248(4) 0.3463(4) 0.7086(3) 0.0418(11) Uani 1 1 d . . . H19A H 0.9012 0.3431 0.7342 0.050 Uiso 1 1 calc R A . H20B H 0.8178 0.3822 0.6535 0.050 Uiso 1 1 calc R . . C108 C 0.8287(4) 0.2301(4) 0.7038(3) 0.0443(12) Uani 1 1 d . A . H21A H 0.8988 0.1862 0.6697 0.053 Uiso 1 1 calc R . . H22B H 0.8408 0.1930 0.7588 0.053 Uiso 1 1 calc R . . O109 O 0.7126(3) 0.2364(3) 0.66895(19) 0.0399(7) Uani 1 1 d . A . C110 C 0.7133(5) 0.1257(4) 0.6634(3) 0.0458(12) Uani 1 1 d . . . H23A H 0.7227 0.0887 0.7182 0.055 Uiso 1 1 calc R A . H24B H 0.7841 0.0807 0.6303 0.055 Uiso 1 1 calc R . . C111 C 0.5957(5) 0.1339(4) 0.6256(3) 0.0476(12) Uani 1 1 d . A . H25A H 0.5857 0.1711 0.5708 0.057 Uiso 1 1 calc R . . H26B H 0.5973 0.0590 0.6206 0.057 Uiso 1 1 calc R . . O112 O 0.4933(3) 0.1976(3) 0.67732(19) 0.0403(7) Uani 1 1 d . A . C113 C 0.3768(5) 0.1914(4) 0.6531(3) 0.0495(12) Uani 1 1 d . . . H27A H 0.3876 0.1132 0.6522 0.059 Uiso 1 1 calc R A . H28B H 0.3521 0.2268 0.5981 0.059 Uiso 1 1 calc R . . C114 C 0.2789(5) 0.2504(4) 0.7135(3) 0.0474(12) Uani 1 1 d . A . H29A H 0.1992 0.2492 0.6978 0.057 Uiso 1 1 calc R . . H30B H 0.3020 0.2128 0.7680 0.057 Uiso 1 1 calc R . . O115 O 0.2671(3) 0.3669(3) 0.71511(18) 0.0378(7) Uani 1 1 d . A . Cl1 Cl 0.60638(11) 0.59266(11) 0.54342(6) 0.0443(3) Uani 1 1 d . . . O1A O 0.6068(6) 0.4896(5) 0.5731(3) 0.107(2) Uani 1 1 d . A . O1B O 0.5014(5) 0.6788(7) 0.5766(4) 0.130(3) Uani 1 1 d . A . O1C O 0.5937(4) 0.6047(3) 0.4568(2) 0.0537(9) Uani 1 1 d . . . O1D O 0.7194(4) 0.6019(4) 0.5666(2) 0.0589(10) Uani 1 1 d . A . Cl2 Cl 0.56285(12) 0.25555(11) 0.91699(7) 0.0479(3) Uani 1 1 d . . . O2A O 0.6824(4) 0.1749(4) 0.8909(3) 0.0604(10) Uani 1 1 d . A . O2B O 0.4860(10) 0.3099(11) 0.8535(5) 0.056(3) Uani 0.60 1 d PU A 1 O2C O 0.5880(11) 0.3436(8) 0.9589(6) 0.075(3) Uani 0.60 1 d PU A 1 O2D O 0.5069(8) 0.2086(7) 0.9788(6) 0.073(2) Uani 0.60 1 d PU A 1 O2E O 0.512(2) 0.3413(17) 0.8470(12) 0.069(5) Uani 0.40 1 d PU A 2 O2F O 0.5600(16) 0.292(2) 0.9904(9) 0.118(9) Uani 0.40 1 d PU A 2 O2G O 0.4793(10) 0.1913(10) 0.9114(10) 0.081(4) Uani 0.40 1 d PU A 2 Cl3 Cl 0.18703(11) 0.10060(10) 0.51852(7) 0.0425(3) Uani 1 1 d . . . O3A O 0.1019(4) 0.0557(3) 0.4883(2) 0.0514(9) Uani 1 1 d . . . O3B O 0.1188(4) 0.1950(4) 0.5644(3) 0.0752(13) Uani 1 1 d . . . O3C O 0.2466(4) 0.1329(4) 0.4498(3) 0.0660(12) Uani 1 1 d . . . O3D O 0.2795(4) 0.0140(4) 0.5699(2) 0.0635(11) Uani 1 1 d . . . N1 N -0.2835(4) 0.7939(3) 0.7886(2) 0.0397(9) Uani 1 1 d . . . C2 C -0.3744(5) 0.8226(4) 0.7520(3) 0.0430(11) Uani 1 1 d . . . C3 C -0.4902(6) 0.8580(5) 0.7039(4) 0.0645(16) Uani 1 1 d . . . H31A H -0.4808 0.8937 0.6520 0.097 Uiso 1 1 calc R . . H32B H -0.5586 0.9102 0.7340 0.097 Uiso 1 1 calc R . . H33C H -0.5076 0.7932 0.6939 0.097 Uiso 1 1 calc R . . N4 N 0.2766(4) 0.6246(4) 0.6518(3) 0.0458(10) Uani 1 1 d . A . C5 C 0.2420(4) 0.6877(4) 0.5965(3) 0.0401(11) Uani 1 1 d . . . C6 C 0.1997(5) 0.7664(5) 0.5257(3) 0.0636(17) Uani 1 1 d . A . H34A H 0.2182 0.8310 0.5339 0.095 Uiso 1 1 calc R . . H35B H 0.1106 0.7898 0.5187 0.095 Uiso 1 1 calc R . . H36C H 0.2422 0.7307 0.4771 0.095 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0333(3) 0.0394(4) 0.0245(3) 0.0024(2) -0.0029(2) -0.0148(3) Ba1 0.03032(15) 0.03945(17) 0.03910(16) -0.00862(10) -0.00876(10) -0.00869(11) N11 0.036(2) 0.043(2) 0.0287(19) 0.0036(14) -0.0017(15) -0.0147(16) C12 0.034(2) 0.034(2) 0.033(2) 0.0047(17) -0.0019(17) -0.0107(18) C13 0.041(3) 0.041(3) 0.040(3) 0.0041(18) -0.0047(19) -0.019(2) C14 0.036(2) 0.042(3) 0.049(3) 0.009(2) 0.004(2) -0.015(2) C15 0.047(3) 0.041(3) 0.032(2) 0.0084(18) 0.0050(19) -0.016(2) C16 0.044(3) 0.040(3) 0.029(2) 0.0064(17) -0.0002(18) -0.014(2) N21 0.0290(18) 0.0350(19) 0.0230(17) 0.0016(13) -0.0027(13) -0.0117(14) C22 0.033(2) 0.035(2) 0.023(2) 0.0022(15) -0.0037(15) -0.0110(17) S23 0.0523(7) 0.0556(7) 0.0266(5) 0.0040(4) -0.0090(4) -0.0312(6) C24 0.051(3) 0.051(3) 0.033(2) 0.0052(19) -0.006(2) -0.030(2) C25 0.032(2) 0.038(2) 0.031(2) 0.0026(16) -0.0011(16) -0.0139(18) N31 0.0322(18) 0.0339(19) 0.0202(16) 0.0008(12) -0.0005(13) -0.0124(14) C32 0.028(2) 0.036(2) 0.023(2) 0.0001(15) -0.0003(15) -0.0115(17) C33 0.035(2) 0.036(2) 0.026(2) 0.0036(16) -0.0039(16) -0.0146(18) C34 0.036(2) 0.052(3) 0.027(2) 0.0027(18) -0.0113(17) -0.024(2) C35 0.035(2) 0.047(3) 0.022(2) 0.0050(16) -0.0028(16) -0.0161(19) C36 0.026(2) 0.033(2) 0.026(2) -0.0011(15) 0.0003(15) -0.0074(16) N41 0.0282(18) 0.0355(19) 0.0249(17) 0.0022(13) -0.0031(13) -0.0133(14) C42 0.032(2) 0.038(2) 0.0215(19) 0.0022(15) -0.0027(15) -0.0186(18) C43 0.030(2) 0.040(2) 0.028(2) 0.0003(16) -0.0023(16) -0.0159(18) C44 0.033(2) 0.056(3) 0.026(2) -0.0071(18) -0.0022(16) -0.022(2) C45 0.037(2) 0.057(3) 0.024(2) 0.0013(18) -0.0060(17) -0.022(2) C46 0.033(2) 0.045(3) 0.025(2) 0.0049(17) -0.0073(16) -0.0200(19) O100 0.0383(17) 0.0522(19) 0.0282(15) 0.0053(12) -0.0076(12) -0.0272(14) C101 0.036(2) 0.048(3) 0.027(2) 0.0004(17) -0.0025(17) -0.018(2) C102 0.029(2) 0.038(2) 0.033(2) -0.0023(17) -0.0037(16) -0.0122(18) O103 0.0320(15) 0.0387(17) 0.0279(15) -0.0007(11) -0.0044(11) -0.0152(12) C104 0.037(2) 0.043(3) 0.030(2) 0.0026(17) -0.0092(17) -0.023(2) C105 0.034(2) 0.045(3) 0.032(2) 0.0056(18) -0.0087(17) -0.0179(19) O106 0.0301(16) 0.0424(18) 0.0386(17) -0.0027(13) -0.0048(12) -0.0134(13) C107 0.034(2) 0.051(3) 0.035(2) 0.0013(19) -0.0041(18) -0.012(2) C108 0.035(2) 0.048(3) 0.040(3) -0.001(2) -0.0079(19) -0.006(2) O109 0.0336(17) 0.0424(18) 0.0404(17) -0.0032(13) -0.0065(13) -0.0113(13) C110 0.043(3) 0.038(3) 0.049(3) -0.002(2) -0.002(2) -0.009(2) C111 0.047(3) 0.044(3) 0.051(3) -0.008(2) 0.008(2) -0.016(2) O112 0.0367(17) 0.0383(18) 0.0413(18) -0.0052(13) -0.0035(13) -0.0097(13) C113 0.045(3) 0.043(3) 0.060(3) -0.005(2) -0.006(2) -0.016(2) C114 0.042(3) 0.051(3) 0.047(3) 0.009(2) -0.003(2) -0.019(2) O115 0.0337(16) 0.0450(19) 0.0304(16) -0.0073(12) -0.0036(12) -0.0102(13) Cl1 0.0387(6) 0.0703(8) 0.0298(5) 0.0037(5) -0.0043(4) -0.0286(5) O1A 0.114(4) 0.141(5) 0.104(4) 0.086(4) -0.071(3) -0.100(4) O1B 0.059(3) 0.214(8) 0.121(5) -0.098(5) 0.035(3) -0.046(4) O1C 0.068(2) 0.075(3) 0.0320(18) 0.0051(16) -0.0091(16) -0.045(2) O1D 0.050(2) 0.096(3) 0.045(2) 0.0061(19) -0.0086(16) -0.045(2) Cl2 0.0486(7) 0.0527(7) 0.0398(6) 0.0099(5) -0.0070(5) -0.0188(5) O2A 0.046(2) 0.064(3) 0.066(3) -0.0003(18) -0.0066(18) -0.0166(18) O2B 0.051(5) 0.081(8) 0.025(4) 0.009(4) -0.008(3) -0.014(4) O2C 0.094(7) 0.069(5) 0.064(6) -0.014(4) -0.031(5) -0.029(4) O2D 0.075(5) 0.061(5) 0.072(5) 0.016(4) 0.020(4) -0.021(4) O2E 0.074(11) 0.051(9) 0.076(9) 0.033(6) 0.010(7) -0.024(6) O2F 0.079(10) 0.21(3) 0.035(8) -0.043(10) -0.015(7) -0.023(13) O2G 0.055(6) 0.076(8) 0.123(11) 0.044(7) -0.014(7) -0.044(6) Cl3 0.0461(6) 0.0451(6) 0.0372(6) 0.0059(4) -0.0069(4) -0.0199(5) O3A 0.056(2) 0.060(2) 0.044(2) 0.0001(16) -0.0118(16) -0.0293(18) O3B 0.068(3) 0.080(3) 0.081(3) -0.033(2) -0.002(2) -0.030(2) O3C 0.062(2) 0.066(3) 0.067(3) 0.024(2) 0.0045(19) -0.027(2) O3D 0.061(2) 0.072(3) 0.057(2) 0.0267(19) -0.0299(19) -0.029(2) N1 0.035(2) 0.042(2) 0.042(2) 0.0049(16) -0.0040(17) -0.0170(17) C2 0.039(3) 0.038(3) 0.051(3) 0.005(2) -0.007(2) -0.015(2) C3 0.052(3) 0.055(4) 0.085(4) 0.013(3) -0.031(3) -0.021(3) N4 0.045(2) 0.052(3) 0.040(2) 0.0013(18) -0.0049(17) -0.0189(19) C5 0.036(2) 0.041(3) 0.040(3) -0.004(2) 0.0027(19) -0.012(2) C6 0.050(3) 0.068(4) 0.050(3) 0.017(3) 0.001(2) -0.002(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 Cu1 N1 1.978(4) . ? Cu1 N21 2.047(3) . ? Cu1 N41 2.053(4) . ? Cu1 N11 2.103(4) . ? Ba1 O2E 2.537(18) . ? Ba1 O1C 2.743(3) 2_666 ? Ba1 O1A 2.767(5) . ? Ba1 O109 2.807(3) . ? Ba1 O2B 2.810(9) . ? Ba1 O103 2.845(3) . ? Ba1 O115 2.846(3) . ? Ba1 O106 2.847(3) . ? Ba1 O112 2.849(3) . ? Ba1 N4 2.860(4) . ? N11 C12 1.338(6) . ? N11 C16 1.349(5) . ? C12 C13 1.387(7) . ? C12 C25 1.480(6) . ? C13 C14 1.376(6) . ? C14 C15 1.386(8) . ? C15 C16 1.385(7) . ? N21 C22 1.323(5) . ? N21 C25 1.396(6) . ? C22 C36 1.452(6) . ? C22 S23 1.731(5) . ? S23 C24 1.705(5) . ? C24 C25 1.358(7) . ? N31 C32 1.324(5) . ? N31 C36 1.352(5) 2_567 ? C32 C33 1.402(7) . ? C32 C42 1.502(5) . ? C33 O100 1.356(5) . ? C33 C34 1.388(6) . ? C34 C35 1.382(6) 2_567 ? C35 C34 1.382(6) 2_567 ? C35 C36 1.384(7) . ? C36 N31 1.352(5) 2_567 ? N41 C42 1.336(5) . ? N41 C46 1.351(5) . ? C42 C43 1.380(6) . ? C43 O115 1.372(5) . ? C43 C44 1.387(6) . ? C44 C45 1.376(7) . ? C45 C46 1.380(6) . ? O100 C101 1.442(6) . ? C101 C102 1.515(6) . ? C102 O103 1.441(5) . ? O103 C104 1.439(5) . ? C104 C105 1.490(6) . ? C105 O106 1.428(6) . ? O106 C107 1.435(5) . ? C107 C108 1.492(8) . ? C108 O109 1.440(6) . ? O109 C110 1.437(6) . ? C110 C111 1.467(8) . ? C111 O112 1.434(6) . ? O112 C113 1.446(6) . ? C113 C114 1.478(7) . ? C114 O115 1.461(6) . ? Cl1 O1A 1.388(5) . ? Cl1 O1C 1.406(4) . ? Cl1 O1B 1.406(5) . ? Cl1 O1D 1.421(4) . ? O1C Ba1 2.743(3) 2_666 ? Cl2 O2F 1.301(15) . ? Cl2 O2B 1.339(9) . ? Cl2 O2D 1.416(7) . ? Cl2 O2A 1.437(4) . ? Cl2 O2C 1.487(10) . ? Cl2 O2E 1.489(18) . ? Cl2 O2G 1.514(12) . ? Cl3 O3B 1.411(4) . ? Cl3 O3C 1.426(4) . ? Cl3 O3D 1.436(4) . ? Cl3 O3A 1.436(4) . ? N1 C2 1.133(6) . ? C2 C3 1.458(7) . ? N4 C5 1.137(6) . ? C5 C6 1.441(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N21 127.15(15) . . ? N1 Cu1 N41 101.98(16) . . ? N21 Cu1 N41 126.16(13) . . ? N1 Cu1 N11 112.00(15) . . ? N21 Cu1 N11 80.85(14) . . ? N41 Cu1 N11 101.89(14) . . ? O2E Ba1 O1C 144.8(4) . 2_666 ? O2E Ba1 O1A 141.1(4) . . ? O1C Ba1 O1A 68.03(13) 2_666 . ? O2E Ba1 O109 85.8(5) . . ? O1C Ba1 O109 88.25(11) 2_666 . ? O1A Ba1 O109 72.66(15) . . ? O2E Ba1 O2B 11.5(5) . . ? O1C Ba1 O2B 133.5(3) 2_666 . ? O1A Ba1 O2B 150.4(2) . . ? O109 Ba1 O2B 86.4(3) . . ? O2E Ba1 O103 76.0(5) . . ? O1C Ba1 O103 136.23(10) 2_666 . ? O1A Ba1 O103 85.57(15) . . ? O109 Ba1 O103 117.33(9) . . ? O2B Ba1 O103 85.7(3) . . ? O2E Ba1 O115 80.4(4) . . ? O1C Ba1 O115 71.47(10) 2_666 . ? O1A Ba1 O115 138.15(11) . . ? O109 Ba1 O115 116.53(9) . . ? O2B Ba1 O115 70.0(2) . . ? O103 Ba1 O115 118.38(8) . . ? O2E Ba1 O106 71.3(4) . . ? O1C Ba1 O106 132.12(10) 2_666 . ? O1A Ba1 O106 69.77(11) . . ? O109 Ba1 O106 58.05(9) . . ? O2B Ba1 O106 81.4(2) . . ? O103 Ba1 O106 59.29(9) . . ? O115 Ba1 O106 151.40(9) . . ? O2E Ba1 O112 80.0(5) . . ? O1C Ba1 O112 67.39(10) 2_666 . ? O1A Ba1 O112 113.11(16) . . ? O109 Ba1 O112 58.87(10) . . ? O2B Ba1 O112 70.5(3) . . ? O103 Ba1 O112 155.88(9) . . ? O115 Ba1 O112 57.77(9) . . ? O106 Ba1 O112 111.37(9) . . ? O2E Ba1 N4 119.8(5) . . ? O1C Ba1 N4 73.11(12) 2_666 . ? O1A Ba1 N4 83.62(15) . . ? O109 Ba1 N4 154.14(11) . . ? O2B Ba1 N4 119.4(3) . . ? O103 Ba1 N4 69.66(11) . . ? O115 Ba1 N4 74.95(11) . . ? O106 Ba1 N4 123.11(11) . . ? O112 Ba1 N4 125.33(11) . . ? C12 N11 C16 118.7(4) . . ? C12 N11 Cu1 114.1(3) . . ? C16 N11 Cu1 127.1(3) . . ? N11 C12 C13 121.8(4) . . ? N11 C12 C25 115.2(4) . . ? C13 C12 C25 122.9(4) . . ? C14 C13 C12 119.5(5) . . ? C13 C14 C15 119.0(5) . . ? C16 C15 C14 118.6(4) . . ? N11 C16 C15 122.3(5) . . ? C22 N21 C25 110.4(4) . . ? C22 N21 Cu1 137.1(3) . . ? C25 N21 Cu1 112.5(3) . . ? N21 C22 C36 126.4(4) . . ? N21 C22 S23 113.8(3) . . ? C36 C22 S23 119.8(3) . . ? C24 S23 C22 90.2(2) . . ? C25 C24 S23 110.5(4) . . ? C24 C25 N21 115.1(4) . . ? C24 C25 C12 127.5(4) . . ? N21 C25 C12 117.3(4) . . ? C32 N31 C36 118.9(4) . 2_567 ? N31 C32 C33 122.6(4) . . ? N31 C32 C42 115.1(4) . . ? C33 C32 C42 122.2(4) . . ? O100 C33 C34 125.3(4) . . ? O100 C33 C32 116.5(3) . . ? C34 C33 C32 118.2(4) . . ? C35 C34 C33 119.0(4) 2_567 . ? C34 C35 C36 119.3(4) 2_567 . ? N31 C36 C35 121.9(4) 2_567 . ? N31 C36 C22 114.7(4) 2_567 . ? C35 C36 C22 123.4(4) . . ? C42 N41 C46 118.2(4) . . ? C42 N41 Cu1 125.0(3) . . ? C46 N41 Cu1 113.8(3) . . ? N41 C42 C43 122.1(4) . . ? N41 C42 C32 118.6(3) . . ? C43 C42 C32 119.3(4) . . ? O115 C43 C42 117.9(4) . . ? O115 C43 C44 122.2(4) . . ? C42 C43 C44 119.8(4) . . ? C45 C44 C43 117.9(4) . . ? C44 C45 C46 119.6(4) . . ? N41 C46 C45 122.2(4) . . ? C33 O100 C101 115.6(3) . . ? O100 C101 C102 108.1(3) . . ? O103 C102 C101 112.2(4) . . ? C104 O103 C102 112.0(3) . . ? C104 O103 Ba1 114.1(2) . . ? C102 O103 Ba1 119.0(2) . . ? O103 C104 C105 109.1(3) . . ? O106 C105 C104 107.9(4) . . ? C105 O106 C107 113.1(4) . . ? C105 O106 Ba1 116.3(2) . . ? C107 O106 Ba1 114.7(3) . . ? O106 C107 C108 107.7(4) . . ? O109 C108 C107 109.6(4) . . ? C110 O109 C108 111.1(3) . . ? C110 O109 Ba1 119.0(3) . . ? C108 O109 Ba1 121.1(3) . . ? O109 C110 C111 110.2(4) . . ? O112 C111 C110 108.4(4) . . ? C111 O112 C113 111.6(4) . . ? C111 O112 Ba1 111.8(3) . . ? C113 O112 Ba1 116.2(3) . . ? O112 C113 C114 108.3(4) . . ? O115 C114 C113 108.9(4) . . ? C43 O115 C114 117.3(4) . . ? C43 O115 Ba1 118.2(3) . . ? C114 O115 Ba1 120.3(3) . . ? O1A Cl1 O1C 110.6(3) . . ? O1A Cl1 O1B 108.2(5) . . ? O1C Cl1 O1B 107.7(4) . . ? O1A Cl1 O1D 110.3(3) . . ? O1C Cl1 O1D 109.6(2) . . ? O1B Cl1 O1D 110.5(3) . . ? Cl1 O1A Ba1 135.7(5) . . ? Cl1 O1C Ba1 158.3(2) . 2_666 ? O2F Cl2 O2B 126.6(11) . . ? O2F Cl2 O2D 64.9(12) . . ? O2B Cl2 O2D 113.9(6) . . ? O2F Cl2 O2A 116.0(8) . . ? O2B Cl2 O2A 112.9(5) . . ? O2D Cl2 O2A 112.2(4) . . ? O2F Cl2 O2C 40.0(11) . . ? O2B Cl2 O2C 105.7(7) . . ? O2D Cl2 O2C 104.5(6) . . ? O2A Cl2 O2C 106.9(5) . . ? O2F Cl2 O2E 117.6(15) . . ? O2B Cl2 O2E 23.8(8) . . ? O2D Cl2 O2E 133.9(8) . . ? O2A Cl2 O2E 106.8(8) . . ? O2C Cl2 O2E 86.4(9) . . ? O2F Cl2 O2G 111.5(13) . . ? O2B Cl2 O2G 76.7(7) . . ? O2D Cl2 O2G 48.3(6) . . ? O2A Cl2 O2G 102.2(6) . . ? O2C Cl2 O2G 146.7(8) . . ? O2E Cl2 O2G 100.5(9) . . ? Cl2 O2B Ba1 141.6(6) . . ? Cl2 O2E Ba1 156.5(14) . . ? O3B Cl3 O3C 110.2(3) . . ? O3B Cl3 O3D 110.5(3) . . ? O3C Cl3 O3D 110.0(3) . . ? O3B Cl3 O3A 109.0(3) . . ? O3C Cl3 O3A 108.9(3) . . ? O3D Cl3 O3A 108.2(2) . . ? C2 N1 Cu1 163.5(4) . . ? N1 C2 C3 179.0(6) . . ? C5 N4 Ba1 139.3(4) . . ? N4 C5 C6 179.1(6) . . ? _diffrn_measured_fraction_theta_max 0.895 _diffrn_reflns_theta_full 70.15 _diffrn_measured_fraction_theta_full 0.895 _refine_diff_density_max 1.342 _refine_diff_density_min -0.849 _refine_diff_density_rms 0.090