# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2308 ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_global _audit_creation_method Xtal3.6 _audit_creation_date 00-08-09 _audit_update_record ? #============================================================================== # (Publishing Staff Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia Nedlands Western Australia 6907 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal ? _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Skelton, Brian W.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Pogram for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_yk08 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C18 H48 Cl4 Cu2 N8 O16' _chemical_formula_moiety ? _chemical_formula_weight 901.53 _chemical_melting_point ? _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 _cell_length_a 13.7910(10) _cell_length_b 9.1815(8) _cell_length_c 27.573(2) _cell_angle_alpha 90.00000 _cell_angle_beta 90.524(2) _cell_angle_gamma 90.00000 _cell_volume 3491.2(5) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 28.4 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu 1.602 _exptl_crystal_description pyramid _exptl_crystal_size_max .45 _exptl_crystal_size_mid .4 _exptl_crystal_size_min .16 _exptl_crystal_size_rad ? _exptl_crystal_colour red _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .51 _exptl_absorpt_correction_T_max .75 _diffrn_reflns_number 51632 _reflns_number_total 13588 _reflns_Friedel_coverage 0 _reflns_number_gt 10597 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 34.05 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .040 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 43 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .049 _refine_ls_wR_factor_ref .059 _refine_ls_goodness_of_fit_ref 1.341 _refine_ls_number_reflns 10597 _refine_ls_number_parameters 680 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .095 _refine_diff_density_min -1.019 _refine_diff_density_max 1.552 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 337(221) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ 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 72 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 192 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 16 .132 .159 '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' N ? 0 32 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 64 .008 .006 '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_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 .60491(2) .73398(3) .624844(10) .01715(13) Uani ? ? 1.00000 ? ? Cu2 1.10691(2) .73833(3) .627658(11) .01807(13) Uani ? ? 1.00000 ? ? C11 .6761(2) .7918(3) .50815(9) .0268(12) Uani ? ? 1.00000 ? ? C111 .6515(3) .8244(5) .45458(12) .0394(17) Uani ? ? 1.00000 ? ? C12 .6227(2) .6502(3) .52031(9) .0264(12) Uani ? ? 1.00000 ? ? N13 .63914(16) .5974(2) .57058(8) .0215(9) Uani ? ? 1.00000 ? ? C14 .5873(2) .4589(3) .57976(11) .0303(13) Uani ? ? 1.00000 ? ? C15 .5963(2) .4260(3) .63337(11) .0308(14) Uani ? ? 1.00000 ? ? N16 .56008(17) .5545(2) .65991(8) .0244(10) Uani ? ? 1.00000 ? ? C111' .7862(2) .7750(5) .51427(13) .0388(17) Uani ? ? 1.00000 ? ? C12' .6389(2) .9211(3) .53753(10) .0251(12) Uani ? ? 1.00000 ? ? N13' .65887(15) .9096(2) .59029(8) .0201(9) Uani ? ? 1.00000 ? ? C14' .6250(2) 1.0403(3) .61660(11) .0273(12) Uani ? ? 1.00000 ? ? C15' .6268(2) 1.0089(3) .67036(11) .0293(13) Uani ? ? 1.00000 ? ? N16' .57127(19) .8735(3) .67849(8) .0271(11) Uani ? ? 1.00000 ? ? C21 1.1691(2) .7829(3) .74689(10) .0276(12) Uani ? ? 1.00000 ? ? C211 1.1451(4) .7875(4) .80101(12) .043(2) Uani ? ? 1.00000 ? ? C22 1.1098(2) .9032(3) .72225(9) .0241(12) Uani ? ? 1.00000 ? ? N23 1.12705(14) .9165(2) .66957(8) .0188(9) Uani ? ? 1.00000 ? ? C24 1.06918(19) 1.0370(3) .64755(10) .0239(11) Uani ? ? 1.00000 ? ? C25 1.0783(2) 1.0262(3) .59342(11) .0281(13) Uani ? ? 1.00000 ? ? N26 1.04861(18) .8769(3) .57925(9) .0272(11) Uani ? ? 1.00000 ? ? C211' 1.2775(2) .8097(4) .74047(14) .0397(17) Uani ? ? 1.00000 ? ? C22' 1.1392(2) .6315(3) .72903(10) .0238(11) Uani ? ? 1.00000 ? ? N23' 1.16205(14) .6018(2) .67774(8) .0196(9) Uani ? ? 1.00000 ? ? C24' 1.1314(2) .4526(3) .66322(11) .0254(12) Uani ? ? 1.00000 ? ? C25' 1.1478(2) .4385(3) .60944(12) .0334(14) Uani ? ? 1.00000 ? ? N26' 1.0971(2) .5607(3) .58518(10) .0332(14) Uani ? ? 1.00000 ? ? Cl1 .3579(7) .7370(11) .5844(5) .025(2) Uani ? ? .50000 ? ? O11 .44078(16) .8179(3) .58968(12) .0568(16) Uani ? ? 1.00000 ? ? O12 .27062(15) .8221(3) .59170(10) .0443(13) Uani ? ? 1.00000 ? ? O13 .3537(5) .6094(7) .6135(4) .065(5) Uani ? ? .50000 ? ? O14 .3633(7) .6986(12) .5342(3) .089(6) Uani ? ? .50000 ? ? Cl1' .3533(8) .7344(12) .5924(5) .030(2) Uani ? ? .50000 ? ? O13' .3643(5) .6659(11) .6397(3) .070(5) Uani ? ? .50000 ? ? O14' .3459(6) .6219(10) .5598(4) .091(6) Uani ? ? .50000 ? ? Cl2 .85576(4) .74420(6) .66953(2) .0218(2) Uani ? ? 1.00000 ? ? O21 .94100(14) .6618(2) .65887(9) .0371(11) Uani ? ? 1.00000 ? ? O22 .77087(14) .6575(2) .66017(9) .0352(11) Uani ? ? 1.00000 ? ? O23 .85348(15) .8722(3) .63906(11) .0463(13) Uani ? ? 1.00000 ? ? O24 .8590(2) .7869(4) .71909(10) .0587(17) Uani ? ? 1.00000 ? ? Cl3 .63373(4) .70874(8) .80571(2) .0259(3) Uani ? ? 1.00000 ? ? O31 .5888(2) .6450(4) .76404(10) .071(2) Uani ? ? 1.00000 ? ? O32 .6380(3) .8614(3) .79892(19) .099(3) Uani ? ? 1.00000 ? ? O33 .5751(2) .6751(6) .84506(11) .101(3) Uani ? ? 1.00000 ? ? O34 .72812(16) .6520(3) .81431(11) .0481(14) Uani ? ? 1.00000 ? ? Cl4 .86954(5) .30346(9) .55171(3) .0329(3) Uani ? ? 1.00000 ? ? O41 .9318(3) .3397(5) .59094(12) .097(3) Uani ? ? 1.00000 ? ? O42 .8933(17) .385(3) .5159(5) .28(2) Uani ? ? .50000 ? ? O43 .7793(5) .3360(15) .5695(4) .127(8) Uani ? ? .50000 ? ? O44 .8734(11) .1711(13) .5303(6) .161(11) Uani ? ? .50000 ? ? O42' .8150(6) .4132(10) .5258(3) .099(6) Uani ? ? .50000 ? ? O43' .8251(7) .1786(11) .5676(3) .097(6) Uani ? ? .50000 ? ? O44' .9452(6) .2739(10) .5178(2) .070(4) Uani ? ? .50000 ? ? H111a .683(3) .910(5) .4457(16) .060(13) Uiso ? ? 1.00000 ? ? H111b .589(3) .831(4) .4501(11) .023(8) Uiso ? ? 1.00000 ? ? H111c .667(3) .744(5) .4371(15) .047(12) Uiso ? ? 1.00000 ? ? H12a .647(3) .575(4) .4991(13) .037(10) Uiso ? ? 1.00000 ? ? H12b .551(2) .660(4) .5162(12) .029(8) Uiso ? ? 1.00000 ? ? H13 .701(2) .577(3) .5774(11) .021(8) Uiso ? ? 1.00000 ? ? H14a .614(3) .381(4) .5609(12) .032(9) Uiso ? ? 1.00000 ? ? H14b .520(3) .472(4) .5718(13) .040(10) Uiso ? ? 1.00000 ? ? H15a .666(3) .411(4) .6415(12) .031(9) Uiso ? ? 1.00000 ? ? H15b .566(3) .343(4) .6440(13) .043(10) Uiso ? ? 1.00000 ? ? H16a .575(2) .558(4) .6895(12) .027(8) Uiso ? ? 1.00000 ? ? H16b .494(3) .551(4) .6582(12) .035(9) Uiso ? ? 1.00000 ? ? H111'a .807(3) .757(4) .5462(14) .036(10) Uiso ? ? 1.00000 ? ? H111'b .815(4) .868(6) .5076(18) .080(16) Uiso ? ? 1.00000 ? ? H111'c .806(3) .703(5) .4946(15) .050(12) Uiso ? ? 1.00000 ? ? H12'a .567(2) .932(4) .5342(11) .026(8) Uiso ? ? 1.00000 ? ? H12'b .669(2) 1.010(3) .5258(10) .015(7) Uiso ? ? 1.00000 ? ? H13' .723(2) .908(3) .5957(11) .020(7) Uiso ? ? 1.00000 ? ? H14'a .561(2) 1.060(3) .6032(11) .020(7) Uiso ? ? 1.00000 ? ? H14'b .668(2) 1.119(4) .6080(11) .025(8) Uiso ? ? 1.00000 ? ? H15'a .600(2) 1.092(4) .6869(11) .022(8) Uiso ? ? 1.00000 ? ? H15'b .691(2) .992(4) .6824(12) .028(8) Uiso ? ? 1.00000 ? ? H16'a .506(3) .899(4) .6766(13) .038(10) Uiso ? ? 1.00000 ? ? H16'b .579(2) .833(4) .7081(12) .028(8) Uiso ? ? 1.00000 ? ? H211a 1.185(3) .717(4) .8209(14) .045(11) Uiso ? ? 1.00000 ? ? H211b 1.088(3) .775(5) .8032(15) .046(13) Uiso ? ? 1.00000 ? ? H211c 1.166(3) .874(4) .8147(14) .042(10) Uiso ? ? 1.00000 ? ? H22a 1.129(3) 1.001(4) .7390(13) .039(10) Uiso ? ? 1.00000 ? ? H22b 1.041(3) .883(4) .7264(12) .038(10) Uiso ? ? 1.00000 ? ? H23 1.189(2) .938(3) .6650(10) .011(6) Uiso ? ? 1.00000 ? ? H24a 1.092(2) 1.131(4) .6584(12) .031(9) Uiso ? ? 1.00000 ? ? H24b 1.007(2) 1.022(4) .6543(11) .023(8) Uiso ? ? 1.00000 ? ? H25a 1.144(3) 1.039(4) .5858(12) .035(9) Uiso ? ? 1.00000 ? ? H25b 1.034(3) 1.099(4) .5782(13) .040(10) Uiso ? ? 1.00000 ? ? H26a .986(3) .873(5) .5784(15) .053(12) Uiso ? ? 1.00000 ? ? H26b 1.059(3) .858(4) .5511(14) .036(10) Uiso ? ? 1.00000 ? ? H211'a 1.294(2) .811(4) .7093(13) .026(8) Uiso ? ? 1.00000 ? ? H211'b 1.314(3) .741(5) .7552(16) .056(13) Uiso ? ? 1.00000 ? ? H211'c 1.301(3) .908(5) .7528(15) .059(13) Uiso ? ? 1.00000 ? ? H22'a 1.068(2) .619(4) .7343(11) .026(8) Uiso ? ? 1.00000 ? ? H22'b 1.173(2) .559(4) .7488(11) .026(8) Uiso ? ? 1.00000 ? ? H23' 1.219(2) .605(4) .6745(11) .022(8) Uiso ? ? 1.00000 ? ? H24'a 1.059(2) .452(3) .6665(10) .015(7) Uiso ? ? 1.00000 ? ? H24'b 1.163(3) .373(4) .6803(14) .047(11) Uiso ? ? 1.00000 ? ? H25'a 1.124(2) .347(4) .5985(12) .028(8) Uiso ? ? 1.00000 ? ? H25'b 1.221(3) .452(4) .6009(14) .049(11) Uiso ? ? 1.00000 ? ? H26'a 1.119(3) .572(5) .5598(15) .047(12) Uiso ? ? 1.00000 ? ? H26'b 1.043(3) .550(4) .5804(13) .029(10) Uiso ? ? 1.00000 ? ? 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 .01835(13) .01395(13) .01908(13) .00083(10) -.00301(9) -.00085(10) Cu2 .01805(13) .01390(13) .02228(14) .00065(10) .00087(10) .00068(10) C11 .0262(12) .0323(14) .0221(11) .0082(10) .0034(9) .0038(10) C111 .0434(18) .049(2) .0260(14) .0150(16) .0033(12) .0083(13) C12 .0322(13) .0267(13) .0202(11) .0077(10) -.0043(9) -.0028(9) N13 .0257(10) .0173(9) .0214(9) .0049(8) -.0043(8) -.0024(7) C14 .0407(16) .0165(11) .0335(14) -.0003(10) -.0078(12) -.0045(10) C15 .0399(16) .0171(11) .0353(14) -.0004(11) -.0075(12) .0048(10) N16 .0268(11) .0238(11) .0227(10) -.0024(8) -.0035(8) .0034(8) C111' .0272(14) .054(2) .0359(16) .0121(14) .0087(12) .0063(15) C12' .0238(11) .0230(12) .0286(12) .0043(9) .0007(9) .0061(9) N13' .0153(8) .0176(9) .0273(10) .0014(7) -.0006(7) -.0003(7) C14' .0291(13) .0147(11) .0382(14) .0023(9) -.0005(10) -.0022(9) C15' .0289(13) .0224(12) .0364(14) .0050(10) -.0119(11) -.0111(10) N16' .0331(12) .0268(11) .0214(10) .0057(9) -.0006(9) -.0030(8) C21 .0323(13) .0221(12) .0281(12) -.0076(10) -.0120(10) .0045(9) C211 .067(3) .0358(18) .0267(14) -.0136(17) -.0103(15) -.0006(12) C22 .0269(12) .0197(11) .0257(12) -.0021(9) -.0034(9) -.0026(9) N23 .0132(8) .0151(9) .0282(10) .0005(7) -.0036(7) .0021(7) C24 .0194(11) .0156(10) .0367(13) .0034(8) -.0042(9) .0032(9) C25 .0227(12) .0247(12) .0368(14) .0018(10) -.0032(10) .0119(11) N26 .0271(11) .0295(12) .0251(11) .0023(9) -.0012(9) .0039(9) C211' .0293(14) .0372(17) .052(2) -.0110(12) -.0232(14) .0163(15) C22' .0245(11) .0195(11) .0274(12) -.0041(9) -.0038(9) .0045(9) N23' .0113(8) .0150(9) .0323(11) .0008(6) -.0003(7) .0026(7) C24' .0253(12) .0126(10) .0382(14) .0007(8) .0012(10) .0015(9) C25' .0392(16) .0179(12) .0434(16) .0010(11) .0145(13) -.0074(11) N26' .0480(17) .0242(12) .0276(12) -.0041(11) .0074(11) -.0041(9) Cl1 .0118(14) .0199(13) .043(3) .0020(11) .0032(17) -.0035(13) O11 .0205(10) .0433(14) .106(2) -.0101(10) -.0139(12) .0176(15) O12 .0202(9) .0420(13) .0708(17) .0079(9) .0105(10) .0124(12) O13 .023(3) .034(3) .136(9) .002(2) .009(4) .041(4) O14 .089(7) .128(9) .050(4) .045(6) -.019(4) -.050(5) Cl1' .0145(10) .0298(14) .046(4) -.0051(9) .0096(15) -.0030(16) O13' .022(3) .109(8) .080(5) .014(4) .015(3) .061(5) O14' .070(5) .080(6) .123(8) -.019(5) .022(6) -.078(6) Cl2 .0123(2) .0209(3) .0321(3) .00101(18) -.00203(19) .0003(2) O21 .0178(9) .0332(11) .0603(14) .0069(8) .0058(9) .0019(10) O22 .0175(8) .0282(10) .0598(14) -.0062(7) -.0114(9) .0082(9) O23 .0213(10) .0343(12) .0830(18) -.0044(8) -.0135(10) .0285(12) O24 .0615(18) .072(2) .0431(14) -.0177(15) .0119(13) -.0253(14) Cl3 .0201(3) .0335(3) .0240(3) .0038(2) .0002(2) -.0023(2) O31 .080(2) .086(2) .0444(15) .0226(19) -.0289(15) -.0267(16) O32 .062(2) .0282(15) .205(5) .0129(14) -.041(3) .001(2) O33 .0364(15) .227(5) .0388(15) -.005(2) .0096(12) .028(2) O34 .0209(10) .0297(11) .094(2) .0070(8) -.0055(11) .0013(12) Cl4 .0254(3) .0408(4) .0326(3) .0039(3) -.0013(2) -.0084(3) O41 .101(3) .139(4) .0499(18) -.055(3) -.0147(18) -.021(2) O42 .29(3) .44(4) .097(10) -.09(2) .002(13) .150(17) O43 .029(3) .230(13) .121(7) .019(5) .008(4) -.081(8) O44 .177(12) .100(8) .203(13) .079(8) -.132(11) -.101(9) O42' .091(6) .099(6) .107(6) .080(5) .039(5) .056(5) O43' .133(7) .105(6) .052(4) -.099(6) .012(4) .002(4) O44' .083(5) .093(6) .033(3) .046(4) .020(3) .008(3) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Cu1 N13 . . 2.011(2) ? Cu1 N16 . . 2.011(2) ? Cu1 N13' . . 2.018(2) ? Cu1 N16' . . 2.014(2) ? Cu1 O11 . . 2.572(3) ? Cu1 O22 . . 2.577(2) ? Cu2 N23 . . 2.020(2) ? Cu2 N26 . . 2.007(3) ? Cu2 N23' . . 2.009(2) ? Cu2 N26' . . 2.012(3) ? Cu2 O21 . . 2.551(2) ? Cu2 O12 . '1 655' 2.591(2) ? C11 C111 . . 1.542(4) ? C11 C12 . . 1.533(4) ? C11 C111' . . 1.535(4) ? C11 C12' . . 1.528(4) ? C111 H111a . . .93(5) ? C111 H111b . . .87(4) ? C111 H111c . . .91(4) ? C12 N13 . . 1.484(3) ? C12 H12a . . .96(4) ? C12 H12b . . .99(3) ? N13 C14 . . 1.482(4) ? N13 H13 . . .90(3) ? C14 C15 . . 1.513(4) ? C14 H14a . . .96(4) ? C14 H14b . . .95(4) ? C15 N16 . . 1.478(4) ? C15 H15a . . .99(4) ? C15 H15b . . .92(4) ? N16 H16a . . .84(3) ? N16 H16b . . .91(4) ? C111' H111'a . . .94(4) ? C111' H111'b . . .96(5) ? C111' H111'c . . .90(4) ? C12' N13' . . 1.482(3) ? C12' H12'a . . 1.00(3) ? C12' H12'b . . .97(3) ? N13' C14' . . 1.481(3) ? N13' H13' . . .90(3) ? C14' C15' . . 1.510(4) ? C14' H14'a . . .96(3) ? C14' H14'b . . .96(3) ? C15' N16' . . 1.478(4) ? C15' H15'a . . .96(3) ? C15' H15'b . . .96(3) ? N16' H16'a . . .93(4) ? N16' H16'b . . .90(3) ? C21 C211 . . 1.532(4) ? C21 C22 . . 1.530(4) ? C21 C211' . . 1.527(4) ? C21 C22' . . 1.530(4) ? C211 H211a . . 1.01(4) ? C211 H211b . . .80(5) ? C211 H211c . . .93(4) ? C22 N23 . . 1.479(3) ? C22 H22a . . 1.04(4) ? C22 H22b . . .97(4) ? N23 C24 . . 1.490(3) ? N23 H23 . . .88(3) ? C24 C25 . . 1.502(4) ? C24 H24a . . .97(4) ? C24 H24b . . .89(3) ? C25 N26 . . 1.482(4) ? C25 H25a . . .94(4) ? C25 H25b . . .99(4) ? N26 H26a . . .87(4) ? N26 H26b . . .81(4) ? C211' H211'a . . .89(4) ? C211' H211'b . . .91(4) ? C211' H211'c . . 1.01(5) ? C22' N23' . . 1.477(3) ? C22' H22'a . . .99(3) ? C22' H22'b . . .98(3) ? N23' C24' . . 1.488(3) ? N23' H23' . . .79(3) ? C24' C25' . . 1.508(4) ? C24' H24'a . . 1.00(3) ? C24' H24'b . . .97(4) ? C25' N26' . . 1.479(4) ? C25' H25'a . . .95(3) ? C25' H25'b . . 1.05(4) ? N26' H26'a . . .77(4) ? N26' H26'b . . .76(4) ? Cl1 O11 . . 1.369(10) ? Cl1 O12 . . 1.451(10) ? Cl1 O13 . . 1.420(14) ? Cl1 O14 . . 1.432(15) ? Cl1 Cl1' . . .230(19) ? Cl1 O13' . . 1.659(15) ? Cl1 O14' . . 1.266(15) ? O11 Cl1' . . 1.432(12) ? O12 Cl1' . . 1.395(12) ? O13 Cl1' . . 1.287(14) ? O13 O13' . . .901(13) ? O13 O14' . . 1.487(15) ? O14 Cl1' . . 1.644(16) ? O14 O14' . . 1.027(14) ? Cl1' O13' . . 1.455(16) ? Cl1' O14' . . 1.372(16) ? Cl2 O21 . . 1.431(2) ? Cl2 O22 . . 1.437(2) ? Cl2 O23 . . 1.445(3) ? Cl2 O24 . . 1.422(3) ? Cl3 O31 . . 1.426(3) ? Cl3 O32 . . 1.415(3) ? Cl3 O33 . . 1.394(3) ? Cl3 O34 . . 1.420(2) ? Cl4 O41 . . 1.415(4) ? Cl4 O42 . . 1.28(2) ? Cl4 O43 . . 1.375(8) ? Cl4 O44 . . 1.352(13) ? Cl4 O42' . . 1.443(9) ? Cl4 O43' . . 1.373(10) ? Cl4 O44' . . 1.434(8) ? O42 O42' . . 1.15(2) ? O42 O44' . . 1.24(3) ? O43 O42' . . 1.486(14) ? O43 O43' . . 1.579(16) ? O44 O43' . . 1.232(18) ? O44 O44' . . 1.413(16) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published N13 Cu1 N16 . . . 85.54(9) ? N13 Cu1 N13' . . . 93.25(9) ? N13 Cu1 N16' . . . 179.07(10) ? N13 Cu1 O11 . . . 96.78(10) ? N13 Cu1 O22 . . . 84.13(8) ? N16 Cu1 N13' . . . 176.26(9) ? N16 Cu1 N16' . . . 95.39(10) ? N16 Cu1 O11 . . . 98.82(9) ? N16 Cu1 O22 . . . 82.58(8) ? N13' Cu1 N16' . . . 85.83(9) ? N13' Cu1 O11 . . . 84.82(9) ? N13' Cu1 O22 . . . 93.78(7) ? N16' Cu1 O11 . . . 83.03(10) ? N16' Cu1 O22 . . . 96.05(9) ? O11 Cu1 O22 . . . 178.37(8) ? N23 Cu2 N26 . . . 85.36(9) ? N23 Cu2 N23' . . . 93.60(8) ? N23 Cu2 N26' . . . 175.92(11) ? N23 Cu2 O21 . . . 98.58(8) ? N23 Cu2 O12 . . '1 655' 82.12(8) ? N26 Cu2 N23' . . . 178.10(9) ? N26 Cu2 N26' . . . 95.88(11) ? N26 Cu2 O21 . . . 92.52(9) ? N26 Cu2 O12 . . '1 655' 84.41(9) ? N23' Cu2 N26' . . . 85.26(10) ? N23' Cu2 O21 . . . 86.06(8) ? N23' Cu2 O12 . . '1 655' 97.03(8) ? N26' Cu2 O21 . . . 85.26(11) ? N26' Cu2 O12 . . '1 655' 94.12(11) ? O21 Cu2 O12 . . '1 655' 176.79(8) ? C111 C11 C12 . . . 105.8(2) ? C111 C11 C111' . . . 109.5(3) ? C111 C11 C12' . . . 106.6(2) ? C12 C11 C111' . . . 111.6(3) ? C12 C11 C12' . . . 112.3(2) ? C111' C11 C12' . . . 110.9(2) ? C11 C111 H111a . . . 108(3) ? C11 C111 H111b . . . 111(2) ? C11 C111 H111c . . . 108(3) ? H111a C111 H111b . . . 111(4) ? H111a C111 H111c . . . 116(4) ? H111b C111 H111c . . . 102(3) ? C11 C12 N13 . . . 114.3(2) ? C11 C12 H12a . . . 108(2) ? C11 C12 H12b . . . 112(2) ? N13 C12 H12a . . . 106(2) ? N13 C12 H12b . . . 106.3(19) ? H12a C12 H12b . . . 110(3) ? Cu1 N13 C12 . . . 117.15(16) ? Cu1 N13 C14 . . . 106.93(17) ? Cu1 N13 H13 . . . 102(2) ? C12 N13 C14 . . . 111.7(2) ? C12 N13 H13 . . . 114(2) ? C14 N13 H13 . . . 104(2) ? N13 C14 C15 . . . 107.6(2) ? N13 C14 H14a . . . 111(2) ? N13 C14 H14b . . . 108(2) ? C15 C14 H14a . . . 111(2) ? C15 C14 H14b . . . 109(2) ? H14a C14 H14b . . . 110(3) ? C14 C15 N16 . . . 107.4(2) ? C14 C15 H15a . . . 109(2) ? C14 C15 H15b . . . 116(2) ? N16 C15 H15a . . . 109(2) ? N16 C15 H15b . . . 111(2) ? H15a C15 H15b . . . 104(3) ? Cu1 N16 C15 . . . 108.02(17) ? Cu1 N16 H16a . . . 111(2) ? Cu1 N16 H16b . . . 109(2) ? C15 N16 H16a . . . 116(2) ? C15 N16 H16b . . . 107(2) ? H16a N16 H16b . . . 107(3) ? C11 C111' H111'a . . . 115(2) ? C11 C111' H111'b . . . 107(3) ? C11 C111' H111'c . . . 109(3) ? H111'a C111' H111'b . . . 103(4) ? H111'a C111' H111'c . . . 110(3) ? H111'b C111' H111'c . . . 114(4) ? C11 C12' N13' . . . 113.9(2) ? C11 C12' H12'a . . . 111.5(18) ? C11 C12' H12'b . . . 109.3(17) ? N13' C12' H12'a . . . 105.8(18) ? N13' C12' H12'b . . . 108.1(16) ? H12'a C12' H12'b . . . 108(3) ? Cu1 N13' C12' . . . 117.02(16) ? Cu1 N13' C14' . . . 107.27(16) ? Cu1 N13' H13' . . . 106(2) ? C12' N13' C14' . . . 111.5(2) ? C12' N13' H13' . . . 109.9(19) ? C14' N13' H13' . . . 104(2) ? N13' C14' C15' . . . 108.9(2) ? N13' C14' H14'a . . . 104.6(18) ? N13' C14' H14'b . . . 107(2) ? C15' C14' H14'a . . . 114.7(18) ? C15' C14' H14'b . . . 112.4(19) ? H14'a C14' H14'b . . . 109(3) ? C14' C15' N16' . . . 107.8(2) ? C14' C15' H15'a . . . 108.0(18) ? C14' C15' H15'b . . . 112(2) ? N16' C15' H15'a . . . 113.1(19) ? N16' C15' H15'b . . . 107(2) ? H15'a C15' H15'b . . . 109(3) ? Cu1 N16' C15' . . . 107.47(17) ? Cu1 N16' H16'a . . . 110(2) ? Cu1 N16' H16'b . . . 112(2) ? C15' N16' H16'a . . . 106(2) ? C15' N16' H16'b . . . 115(2) ? H16'a N16' H16'b . . . 105(3) ? C211 C21 C22 . . . 107.1(3) ? C211 C21 C211' . . . 109.2(3) ? C211 C21 C22' . . . 106.2(2) ? C22 C21 C211' . . . 110.6(2) ? C22 C21 C22' . . . 111.8(2) ? C211' C21 C22' . . . 111.7(2) ? C21 C211 H211a . . . 113(2) ? C21 C211 H211b . . . 107(3) ? C21 C211 H211c . . . 110(2) ? H211a C211 H211b . . . 114(4) ? H211a C211 H211c . . . 99(3) ? H211b C211 H211c . . . 114(4) ? C21 C22 N23 . . . 113.9(2) ? C21 C22 H22a . . . 107(2) ? C21 C22 H22b . . . 109(2) ? N23 C22 H22a . . . 109(2) ? N23 C22 H22b . . . 107(2) ? H22a C22 H22b . . . 111(3) ? Cu2 N23 C22 . . . 118.18(15) ? Cu2 N23 C24 . . . 107.32(15) ? Cu2 N23 H23 . . . 102.9(18) ? C22 N23 C24 . . . 111.8(2) ? C22 N23 H23 . . . 108.9(17) ? C24 N23 H23 . . . 106.9(18) ? N23 C24 C25 . . . 107.8(2) ? N23 C24 H24a . . . 112(2) ? N23 C24 H24b . . . 108(2) ? C25 C24 H24a . . . 110(2) ? C25 C24 H24b . . . 107(2) ? H24a C24 H24b . . . 112(3) ? C24 C25 N26 . . . 107.3(2) ? C24 C25 H25a . . . 108(2) ? C24 C25 H25b . . . 109(2) ? N26 C25 H25a . . . 109(2) ? N26 C25 H25b . . . 110(2) ? H25a C25 H25b . . . 114(3) ? Cu2 N26 C25 . . . 107.64(17) ? Cu2 N26 H26a . . . 113(3) ? Cu2 N26 H26b . . . 115(3) ? C25 N26 H26a . . . 108(3) ? C25 N26 H26b . . . 114(3) ? H26a N26 H26b . . . 98(4) ? C21 C211' H211'a . . . 112(2) ? C21 C211' H211'b . . . 112(3) ? C21 C211' H211'c . . . 115(2) ? H211'a C211' H211'b . . . 107(4) ? H211'a C211' H211'c . . . 103(3) ? H211'b C211' H211'c . . . 107(4) ? C21 C22' N23' . . . 114.6(2) ? C21 C22' H22'a . . . 108.6(19) ? C21 C22' H22'b . . . 108.3(19) ? N23' C22' H22'a . . . 109.7(18) ? N23' C22' H22'b . . . 107.5(19) ? H22'a C22' H22'b . . . 108(3) ? Cu2 N23' C22' . . . 117.39(15) ? Cu2 N23' C24' . . . 106.53(16) ? Cu2 N23' H23' . . . 106(2) ? C22' N23' C24' . . . 111.4(2) ? C22' N23' H23' . . . 109(2) ? C24' N23' H23' . . . 107(2) ? N23' C24' C25' . . . 107.4(2) ? N23' C24' H24'a . . . 105.4(17) ? N23' C24' H24'b . . . 116(2) ? C25' C24' H24'a . . . 104.3(16) ? C25' C24' H24'b . . . 110(2) ? H24'a C24' H24'b . . . 113(3) ? C24' C25' N26' . . . 107.8(2) ? C24' C25' H25'a . . . 110(2) ? C24' C25' H25'b . . . 111(2) ? N26' C25' H25'a . . . 112(2) ? N26' C25' H25'b . . . 105(2) ? H25'a C25' H25'b . . . 111(3) ? Cu2 N26' C25' . . . 108.8(2) ? Cu2 N26' H26'a . . . 113(3) ? Cu2 N26' H26'b . . . 105(3) ? C25' N26' H26'a . . . 109(3) ? C25' N26' H26'b . . . 116(3) ? H26'a N26' H26'b . . . 105(4) ? O11 Cl1 O12 . . . 112.7(7) ? O11 Cl1 O13 . . . 115.3(9) ? O11 Cl1 O14 . . . 100.7(9) ? O11 Cl1 Cl1' . . . 101(4) ? O11 Cl1 O13' . . . 94.6(8) ? O11 Cl1 O14' . . . 127.9(10) ? O12 Cl1 O13 . . . 109.2(8) ? O12 Cl1 O14 . . . 108.4(9) ? O12 Cl1 Cl1' . . . 72(4) ? O12 Cl1 O13' . . . 97.0(8) ? O12 Cl1 O14' . . . 114.7(9) ? O13 Cl1 O14 . . . 110.2(9) ? O13 Cl1 Cl1' . . . 51(4) ? O13 Cl1 O13' . . . 32.9(6) ? O13 Cl1 O14' . . . 66.9(8) ? O14 Cl1 Cl1' . . . 156(4) ? O14 Cl1 O13' . . . 142.1(9) ? O14 Cl1 O14' . . . 44.2(8) ? Cl1' Cl1 O13' . . . 26(4) ? Cl1' Cl1 O14' . . . 113(4) ? O13' Cl1 O14' . . . 99.8(9) ? Cu1 O11 Cl1 . . . 127.4(5) ? Cu1 O11 Cl1' . . . 124.0(5) ? Cl1 O11 Cl1' . . . 9.1(8) ? Cl1 O12 Cl1' . . . 9.0(8) ? Cl1 O12 Cu2 . . '1 455' 128.3(4) ? Cl1' O12 Cu2 . . '1 455' 122.6(5) ? Cl1 O13 Cl1' . . . 7.9(8) ? Cl1 O13 O13' . . . 88.3(9) ? Cl1 O13 O14' . . . 51.6(7) ? Cl1' O13 O13' . . . 81.3(10) ? Cl1' O13 O14' . . . 58.8(8) ? O13' O13 O14' . . . 139.8(10) ? Cl1 O14 Cl1' . . . 3.3(6) ? Cl1 O14 O14' . . . 59.3(8) ? Cl1' O14 O14' . . . 56.2(8) ? Cl1 Cl1' O11 . . . 70(4) ? Cl1 Cl1' O12 . . . 99(4) ? Cl1 Cl1' O13 . . . 121(4) ? Cl1 Cl1' O14 . . . 21(4) ? Cl1 Cl1' O13' . . . 151(4) ? Cl1 Cl1' O14' . . . 58(4) ? O11 Cl1' O12 . . . 112.3(8) ? O11 Cl1' O13 . . . 120.1(9) ? O11 Cl1' O14 . . . 88.7(8) ? O11 Cl1' O13' . . . 101.4(8) ? O11 Cl1' O14' . . . 115.3(9) ? O12 Cl1' O13 . . . 121.4(9) ? O12 Cl1' O14 . . . 100.2(8) ? O12 Cl1' O13' . . . 109.9(9) ? O12 Cl1' O14' . . . 111.7(9) ? O13 Cl1' O14 . . . 105.2(10) ? O13 Cl1' O13' . . . 37.8(7) ? O13 Cl1' O14' . . . 67.9(8) ? O14 Cl1' O13' . . . 141.2(10) ? O14 Cl1' O14' . . . 38.5(7) ? O13' Cl1' O14' . . . 105.6(9) ? Cl1 O13' O13 . . . 58.8(8) ? Cl1 O13' Cl1' . . . 3.9(6) ? O13 O13' Cl1' . . . 60.9(8) ? Cl1 O14' O13 . . . 61.5(8) ? Cl1 O14' O14 . . . 76.5(10) ? Cl1 O14' Cl1' . . . 8.9(8) ? O13 O14' O14 . . . 136.2(10) ? O13 O14' Cl1' . . . 53.3(7) ? O14 O14' Cl1' . . . 85.3(10) ? O21 Cl2 O22 . . . 109.86(13) ? O21 Cl2 O23 . . . 108.93(14) ? O21 Cl2 O24 . . . 108.95(16) ? O22 Cl2 O23 . . . 109.42(13) ? O22 Cl2 O24 . . . 110.09(16) ? O23 Cl2 O24 . . . 109.56(17) ? Cu2 O21 Cl2 . . . 131.66(13) ? Cu1 O22 Cl2 . . . 129.53(12) ? O31 Cl3 O32 . . . 108.5(2) ? O31 Cl3 O33 . . . 106.6(2) ? O31 Cl3 O34 . . . 112.01(19) ? O32 Cl3 O33 . . . 110.3(3) ? O32 Cl3 O34 . . . 110.26(17) ? O33 Cl3 O34 . . . 109.0(2) ? O41 Cl4 O42 . . . 107.1(10) ? O41 Cl4 O43 . . . 102.8(4) ? O41 Cl4 O44 . . . 121.3(7) ? O41 Cl4 O42' . . . 121.6(4) ? O41 Cl4 O43' . . . 102.9(4) ? O41 Cl4 O44' . . . 95.9(3) ? O42 Cl4 O43 . . . 112.8(12) ? O42 Cl4 O44 . . . 100.1(13) ? O42 Cl4 O42' . . . 49.3(11) ? O42 Cl4 O43' . . . 148.0(11) ? O42 Cl4 O44' . . . 54.2(12) ? O43 Cl4 O44 . . . 113.0(8) ? O43 Cl4 O42' . . . 63.6(6) ? O43 Cl4 O43' . . . 70.1(7) ? O43 Cl4 O44' . . . 160.1(5) ? O44 Cl4 O42' . . . 115.7(7) ? O44 Cl4 O43' . . . 53.7(7) ? O44 Cl4 O44' . . . 60.9(7) ? O42' Cl4 O43' . . . 120.6(5) ? O42' Cl4 O44' . . . 100.8(5) ? O43' Cl4 O44' . . . 112.3(5) ? Cl4 O42 O42' . . . 72.6(12) ? Cl4 O42 O44' . . . 69.1(13) ? O42' O42 O44' . . . 136(2) ? Cl4 O43 O42' . . . 60.4(5) ? Cl4 O43 O43' . . . 54.9(5) ? O42' O43 O43' . . . 105.9(7) ? Cl4 O44 O43' . . . 64.0(8) ? Cl4 O44 O44' . . . 62.4(6) ? O43' O44 O44' . . . 123.5(12) ? Cl4 O42' O42 . . . 58.0(12) ? Cl4 O42' O43 . . . 56.0(5) ? O42 O42' O43 . . . 113.8(13) ? Cl4 O43' O43 . . . 55.0(5) ? Cl4 O43' O44 . . . 62.3(7) ? O43 O43' O44 . . . 107.4(9) ? Cl4 O44' O42 . . . 56.7(9) ? Cl4 O44' O44 . . . 56.7(7) ? O42 O44' O44 . . . 98.8(14) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- 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 C11 3.414(3) . . ? Cu1 C12 2.995(3) . . ? Cu1 C14 2.825(3) . . ? Cu1 C15 2.840(3) . . ? Cu1 C12' 2.998(3) . . ? Cu1 C14' 2.835(3) . . ? Cu1 C15' 2.834(3) . . ? Cu1 Cl1 3.574(10) . . ? Cu1 O13 3.659(7) . . ? Cu1 Cl1' 3.576(11) . . ? Cu1 O13' 3.406(7) . . ? Cu1 Cl2 3.6630(7) . . ? Cu1 O23 3.673(2) . . ? Cu1 H12b 3.15(3) . . ? Cu1 H13 2.36(3) . . ? Cu1 H14b 3.04(4) . . ? Cu1 H15a 3.12(3) . . ? Cu1 H16a 2.44(3) . . ? Cu1 H16b 2.46(4) . . ? Cu1 H12'a 3.13(3) . . ? Cu1 H13' 2.43(3) . . ? Cu1 H14'a 3.11(3) . . ? Cu1 H15'b 3.08(3) . . ? Cu1 H16'a 2.49(4) . . ? Cu1 H16'b 2.50(3) . . ? Cu2 C21 3.415(3) . . ? Cu2 C22 3.015(3) . . ? Cu2 C24 2.845(3) . . ? Cu2 C25 2.833(3) . . ? Cu2 C22' 2.992(3) . . ? Cu2 C24' 2.820(3) . . ? Cu2 C25' 2.856(3) . . ? Cu2 Cl1 3.671(11) . '1 655' ? Cu2 O13 3.628(7) . '1 655' ? Cu2 Cl1' 3.543(12) . '1 655' ? Cu2 O13' 3.623(7) . '1 655' ? Cu2 Cl2 3.6613(7) . . ? Cu2 O23 3.721(2) . . ? Cu2 H22b 3.17(4) . . ? Cu2 H23 2.38(3) . . ? Cu2 H24b 3.04(3) . . ? Cu2 H25a 3.04(4) . . ? Cu2 H26a 2.48(4) . . ? Cu2 H26b 2.46(4) . . ? Cu2 H22'a 3.19(3) . . ? Cu2 H23' 2.35(3) . . ? Cu2 H24'a 2.92(3) . . ? Cu2 H25'b 3.16(4) . . ? Cu2 H26'a 2.42(4) . . ? Cu2 H26'b 2.33(4) . . ? C11 N13 2.535(3) . . ? C11 N13' 2.522(3) . . ? C11 H111a 2.04(4) . . ? C11 H111b 2.03(3) . . ? C11 H111c 2.01(4) . . ? C11 H12a 2.04(4) . . ? C11 H12b 2.11(3) . . ? C11 H111'a 2.11(4) . . ? C11 H111'b 2.03(5) . . ? C11 H111'c 2.01(4) . . ? C11 H12'a 2.11(3) . . ? C11 H12'b 2.06(3) . . ? C111 C12 2.452(5) . . ? C111 C111' 2.512(5) . . ? C111 C12' 2.461(4) . . ? C111 H12a 2.60(4) . . ? C111 H12b 2.67(3) . . ? C111 H111'c 2.64(4) . . ? C111 H12'a 2.68(3) . . ? C111 H12'b 2.61(3) . . ? C12 C14 2.455(4) . . ? C12 C111' 2.537(4) . . ? C12 C12' 2.541(4) . . ? C12 H111b 2.59(3) . . ? C12 H111c 2.53(4) . . ? C12 H13 2.02(3) . . ? C12 H14b 2.59(4) . . ? C12 H111'c 2.68(4) . . ? N13 C15 2.417(4) . . ? N13 N16 2.731(3) . . ? N13 C111' 3.040(4) . . ? N13 N13' 2.929(3) . . ? N13 O22 3.102(3) . . ? N13 O43 3.082(12) . . ? N13 H12a 1.98(3) . . ? N13 H12b 2.00(3) . . ? N13 H14a 2.04(4) . . ? N13 H14b 2.00(4) . . ? N13 H15a 2.62(3) . . ? C14 N16 2.411(4) . . ? C14 O43 2.894(9) . . ? C14 H12a 2.61(4) . . ? C14 H12b 2.59(3) . . ? C14 H13 1.91(3) . . ? C14 H15a 2.06(3) . . ? C14 H15b 2.09(4) . . ? C14 H16b 2.66(4) . . ? C15 H13 2.54(3) . . ? C15 H14a 2.06(3) . . ? C15 H14b 2.03(4) . . ? C15 H16a 1.99(3) . . ? C15 H16b 1.95(4) . . ? N16 N16' 2.977(3) . . ? N16 O13 3.151(8) . . ? N16 O13' 2.936(8) . . ? N16 O22 3.057(3) . . ? N16 O31 3.012(4) . . ? N16 H14b 2.60(4) . . ? N16 H15a 2.04(4) . . ? N16 H15b 1.99(4) . . ? C111' C12' 2.522(4) . . ? C111' N13' 3.012(4) . . ? C111' H111a 2.66(4) . . ? C111' H111c 2.70(4) . . ? C111' H12a 2.69(4) . . ? C12' C14' 2.449(4) . . ? C12' H111a 2.61(4) . . ? C12' H111b 2.64(3) . . ? C12' H111'b 2.61(5) . . ? C12' H13' 1.98(3) . . ? C12' H14'a 2.46(3) . . ? C12' H14'b 2.69(3) . . ? N13' C15' 2.433(4) . . ? N13' N16' 2.746(3) . . ? N13' O11 3.123(3) . . ? N13' O23 3.011(3) . . ? N13' H111'a 2.77(4) . . ? N13' H12'a 2.00(3) . . ? N13' H12'b 2.01(3) . . ? N13' H14'a 1.96(3) . . ? N13' H14'b 1.99(3) . . ? N13' H15'b 2.68(3) . . ? C14' N16' 2.415(4) . . ? C14' H12'a 2.60(3) . . ? C14' H12'b 2.59(3) . . ? C14' H13' 1.92(3) . . ? C14' H15'a 2.03(3) . . ? C14' H15'b 2.07(3) . . ? C14' H16'a 2.68(4) . . ? C15' H13' 2.63(3) . . ? C15' H14'a 2.10(3) . . ? C15' H14'b 2.08(3) . . ? C15' H16'a 1.96(4) . . ? C15' H16'b 2.03(3) . . ? N16' O11 3.068(4) . . ? N16' O31 3.164(4) . . ? N16' H14'a 2.69(3) . . ? N16' H15'a 2.06(3) . . ? N16' H15'b 1.98(3) . . ? C21 N23 2.523(3) . . ? C21 N23' 2.531(3) . . ? C21 H211a 2.14(4) . . ? C21 H211b 1.92(4) . . ? C21 H211c 2.05(4) . . ? C21 H22a 2.09(4) . . ? C21 H22b 2.07(4) . . ? C21 H23 2.68(3) . . ? C21 H211'a 2.04(3) . . ? C21 H211'b 2.05(5) . . ? C21 H211'c 2.16(4) . . ? C21 H22'a 2.07(3) . . ? C21 H22'b 2.06(3) . . ? C21 H23' 2.67(3) . . ? C211 C22 2.462(4) . . ? C211 C211' 2.493(6) . . ? C211 C22' 2.448(4) . . ? C211 H22a 2.61(4) . . ? C211 H22b 2.65(4) . . ? C211 H211'b 2.70(5) . . ? C211 H22'a 2.62(3) . . ? C211 H22'b 2.58(3) . . ? C22 C24 2.458(4) . . ? C22 C211' 2.514(4) . . ? C22 C22' 2.534(4) . . ? C22 H211b 2.54(4) . . ? C22 H211c 2.67(4) . . ? C22 H23 1.95(3) . . ? C22 H24b 2.58(3) . . ? C22 H22'a 2.69(3) . . ? N23 C25 2.418(4) . . ? N23 N26 2.730(3) . . ? N23 C211' 3.002(4) . . ? N23 C22' 3.091(3) . . ? N23 N23' 2.937(3) . . ? N23 O12 3.059(3) . '1 655' ? N23 O34 2.974(3) . '2 756' ? N23 H22a 2.07(4) . . ? N23 H22b 2.00(4) . . ? N23 H24a 2.05(4) . . ? N23 H24b 1.96(3) . . ? N23 H25a 2.58(3) . . ? N23 H211'a 2.72(3) . . ? C24 N26 2.403(4) . . ? C24 H22a 2.67(4) . . ? C24 H22b 2.62(4) . . ? C24 H23 1.94(3) . . ? C24 H25a 2.00(4) . . ? C24 H25b 2.05(4) . . ? C24 H26a 2.68(4) . . ? C25 H23 2.61(3) . . ? C25 H24a 2.04(3) . . ? C25 H24b 1.95(3) . . ? C25 H26a 1.94(4) . . ? C25 H26b 1.96(4) . . ? N26 N26' 2.984(4) . . ? N26 O12 3.119(3) . '1 655' ? N26 O23 3.169(3) . . ? N26 O44' 3.014(7) . '3 766' ? N26 H24b 2.53(3) . . ? N26 H25a 1.99(4) . . ? N26 H25b 2.05(4) . . ? C211' C22' 2.530(4) . . ? C211' N23' 3.020(4) . . ? C211' H211c 2.63(4) . . ? C211' H22a 2.70(4) . . ? C211' H23 2.68(3) . . ? C22' C24' 2.449(4) . . ? C22' H211b 2.54(4) . . ? C22' H22b 2.68(4) . . ? C22' H23' 1.88(3) . . ? C22' H24'a 2.62(3) . . ? N23' C25' 2.414(4) . . ? N23' N26' 2.723(4) . . ? N23' O13 3.196(8) . '1 655' ? N23' O13' 3.046(7) . '1 655' ? N23' O21 3.137(3) . . ? N23' H211'a 2.78(3) . . ? N23' H22'a 2.04(3) . . ? N23' H22'b 2.00(3) . . ? N23' H24'a 2.00(3) . . ? N23' H24'b 2.10(4) . . ? N23' H25'b 2.66(4) . . ? C24' N26' 2.412(4) . . ? C24' H22'a 2.64(3) . . ? C24' H22'b 2.61(3) . . ? C24' H23' 1.87(3) . . ? C24' H25'a 2.03(3) . . ? C24' H25'b 2.13(4) . . ? C25' H23' 2.55(3) . . ? C25' H24'a 2.00(3) . . ? C25' H24'b 2.05(4) . . ? C25' H26'a 1.88(4) . . ? C25' H26'b 1.94(4) . . ? N26' O21 3.115(4) . . ? N26' O41 3.057(5) . . ? N26' O42 2.836(15) . '3 766' ? N26' H24'a 2.52(3) . . ? N26' H25'a 2.03(3) . . ? N26' H25'b 2.02(4) . . ? O11 O12 2.348(3) . . ? O11 O13 2.356(8) . . ? O11 O14 2.157(10) . . ? O11 O13' 2.234(9) . . ? O11 O14' 2.368(10) . . ? O11 H12'a 2.55(3) . . ? O11 H14'a 2.80(3) . . ? O11 H16'a 2.66(4) . . ? O12 O13 2.340(8) . . ? O12 O14 2.338(9) . . ? O12 O13' 2.333(9) . . ? O12 O14' 2.290(10) . . ? O12 H111a 2.74(5) . '3 676' ? O12 H23 2.56(3) . '1 455' ? O12 H25a 2.65(4) . '1 455' ? O13 O14 2.338(13) . . ? O13 H16b 2.35(4) . . ? O13 H23' 2.52(3) . '1 455' ? O13 H25'b 2.35(4) . '1 455' ? O14 O13' 2.924(11) . . ? O14 O42' 3.124(13) . '3 666' ? O14 H12a 2.68(4) . '3 666' ? O14 H12b 2.67(4) . . ? O14 H14a 2.74(3) . '3 666' ? O13' O14' 2.252(14) . . ? O13' H16b 2.14(4) . . ? O13' H211'a 2.53(4) . '1 455' ? O13' H23' 2.30(3) . '1 455' ? O14' H12a 2.44(4) . '3 666' ? O14' H14b 2.79(4) . . ? O14' H25'b 2.59(4) . '1 455' ? O21 O22 2.347(3) . . ? O21 O23 2.340(3) . . ? O21 O24 2.322(4) . . ? O21 H22'a 2.74(3) . . ? O21 H24'a 2.53(3) . . ? O21 H26'b 2.79(4) . . ? O22 O23 2.352(3) . . ? O22 O24 2.343(4) . . ? O22 H13 2.58(3) . . ? O22 H15a 2.74(3) . . ? O23 O24 2.342(4) . . ? O23 H13' 2.17(3) . . ? O23 H15'b 2.77(3) . . ? O23 H24b 2.56(3) . . ? O23 H26a 2.48(4) . . ? O24 H22b 2.67(4) . . ? O24 H22'b 2.69(3) . '2 756' ? O31 O32 2.306(5) . . ? O31 O33 2.260(4) . . ? O31 O34 2.360(4) . . ? O31 H16a 2.21(3) . . ? O31 H16'b 2.32(3) . . ? O31 H211'c 2.70(5) . '2 746' ? O32 O33 2.306(6) . . ? O32 O34 2.326(4) . . ? O32 H16b 2.79(4) . '2 656' ? O32 H16'b 2.64(3) . . ? O32 H24'b 2.79(4) . '2 756' ? O33 O34 2.291(4) . . ? O33 H15b 2.51(4) . '2 656' ? O33 H14'a 2.60(3) . '2 646' ? O33 H15'a 2.67(3) . '2 646' ? O34 H23 2.35(3) . '2 746' ? O34 H24a 2.60(3) . '2 746' ? O34 H24'b 2.53(4) . '2 756' ? O41 O42 2.171(16) . . ? O41 O43 2.180(8) . . ? O41 O44 2.412(15) . . ? O41 O42' 2.495(10) . . ? O41 O43' 2.180(11) . . ? O41 O44' 2.116(7) . . ? O41 H25b 2.65(4) . '1 545' ? O41 H25'a 2.66(3) . . ? O41 H26'b 2.48(4) . . ? O42 O43 2.21(2) . . ? O42 O44 2.02(3) . . ? O42 O43' 2.55(3) . . ? O42 H26'a 2.13(4) . '3 766' ? O43 O44 2.274(18) . . ? O43 O44' 2.766(11) . . ? O43 H13 2.47(3) . . ? O43 H14a 2.33(4) . . ? O43 H15a 2.63(4) . . ? O43 H14'b 2.74(3) . '1 545' ? O44 O42' 2.367(15) . . ? O44 H25b 2.66(4) . '1 545' ? O44 H26b 2.45(4) . '3 766' ? O42' O43' 2.446(13) . . ? O42' O44' 2.216(12) . . ? O42' H13 2.60(3) . . ? O42' H111'c 2.80(4) . . ? O42' H26'a 2.54(4) . '3 766' ? O43' O44' 2.331(12) . . ? O43' H14'b 2.51(3) . '1 545' ? O44' H25b 2.61(4) . '1 545' ? O44' H26b 2.25(4) . '3 766' ? O44' H26'a 2.71(4) . '3 766' ? H111a H111b 1.49(6) . . ? H111a H111c 1.56(6) . . ? H111a H12'b 2.40(5) . . ? H111b H111c 1.39(5) . . ? H111c H12a 2.32(5) . . ? H12a H12b 1.61(5) . . ? H12a H13 2.28(5) . . ? H12b H14b 2.35(5) . . ? H13 H14a 2.21(5) . . ? H13 H15a 2.39(5) . . ? H13 H111'a 2.37(5) . . ? H14a H14b 1.57(5) . . ? H14a H15a 2.34(5) . . ? H14b H15b 2.40(5) . . ? H15a H15b 1.51(5) . . ? H15a H16a 2.28(5) . . ? H15b H16a 2.35(5) . . ? H15b H16b 2.19(5) . . ? H16a H16b 1.41(5) . . ? H111'a H111'b 1.48(6) . . ? H111'a H111'c 1.51(6) . . ? H111'a H13' 2.27(5) . . ? H111'b H111'c 1.56(7) . . ? H12'a H12'b 1.59(4) . . ? H12'a H14'a 2.24(4) . . ? H12'b H13' 2.27(4) . . ? H13' H14'b 2.12(5) . . ? H14'a H14'b 1.57(4) . . ? H14'a H15'a 2.38(4) . . ? H14'b H15'a 2.39(4) . . ? H14'b H15'b 2.38(5) . . ? H15'a H15'b 1.56(5) . . ? H15'a H16'a 2.21(5) . . ? H15'b H16'b 2.25(5) . . ? H16'a H16'b 1.45(5) . . ? H211a H211b 1.52(6) . . ? H211a H211c 1.47(6) . . ? H211b H211c 1.45(6) . . ? H211b H22'a 2.39(5) . . ? H22a H22b 1.66(5) . . ? H22a H23 2.28(4) . . ? H23 H24a 2.23(4) . . ? H23 H211'a 2.22(4) . . ? H24a H24b 1.54(5) . . ? H24a H25a 2.30(5) . . ? H24a H25b 2.36(5) . . ? H24b H25b 2.25(5) . . ? H25a H25b 1.62(5) . . ? H25a H26b 2.25(5) . . ? H25b H26a 2.18(6) . . ? H25b H26b 2.37(5) . . ? H26a H26b 1.27(6) . . ? H211'a H211'b 1.44(6) . . ? H211'a H211'c 1.49(6) . . ? H211'a H23' 2.36(5) . . ? H211'b H211'c 1.54(6) . . ? H22'a H22'b 1.60(5) . . ? H22'b H23' 2.19(4) . . ? H23' H24'b 2.27(5) . . ? H24'a H24'b 1.65(5) . . ? H24'a H25'a 2.30(4) . . ? H24'b H25'a 2.33(5) . . ? H25'a H25'b 1.64(5) . . ? H25'a H26'a 2.32(5) . . ? H25'a H26'b 2.23(5) . . ? H25'b H26'a 2.11(6) . . ? H26'a H26'b 1.21(6) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1864 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 21 _reflns_limit_k_min 0 _reflns_limit_k_max 14 _reflns_limit_l_min -43 _reflns_limit_l_max 43 _reflns_number_observed ? _reflns_d_resolution_high .635 _reflns_d_resolution_low 9.775 _diffrn_reflns_av_sigmaI/netI .056 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970' _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .067 _refine_ls_wR_factor_all .063 _refine_ls_goodness_of_fit_all 1.252 _refine_ls_shift/su_mean .006 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_global _audit_creation_method Xtal3.6 _audit_creation_date 99-11-15 _audit_update_record ? #============================================================================== # (Publishing Staff Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia Nedlands Western Australia 6907 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal ? _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Skelton, Brian W.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; 'White, Allan H.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Pogram for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_ykcun4 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C18 H48 Cl4 Cu2 N8 O16' _chemical_formula_moiety ? _chemical_formula_weight 901.53 _chemical_melting_point ? _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 _cell_length_a 13.8870(10) _cell_length_b 9.2532(9) _cell_length_c 27.778(3) _cell_angle_alpha 90.00000 _cell_angle_beta 90.634(2) _cell_angle_gamma 90.00000 _cell_volume 3569.2(6) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.678 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 6602 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 1.567 _exptl_crystal_description rhomboid _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_size_rad ? _exptl_crystal_colour red-purple _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .631 _exptl_absorpt_correction_T_max .901 _diffrn_reflns_number 40411 _reflns_number_total 8745 _reflns_Friedel_coverage 0 _reflns_number_gt 6577 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 28.98 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .0233 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 37 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .052 _refine_ls_wR_factor_ref .069 _refine_ls_goodness_of_fit_ref 2.256 _refine_ls_number_reflns 6577 _refine_ls_number_parameters 653 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .057 _refine_diff_density_min -.67 _refine_diff_density_max .876 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 2379(522) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ 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 72 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 192 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 16 .132 .159 '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' N ? 0 32 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 64 .008 .006 '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_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 .60656(3) .73229(4) .624316(14) .0343(3) Uani ? ? 1.00000 ? ? Cu2 1.10854(3) .73595(4) .627211(15) .0352(3) Uani ? ? 1.00000 ? ? C11 .6769(3) .7886(5) .50872(14) .052(2) Uani ? ? 1.00000 ? ? C111 .6495(5) .8200(8) .4552(2) .081(4) Uani ? ? 1.00000 ? ? C12 .6244(3) .6467(5) .52076(14) .048(2) Uani ? ? 1.00000 ? ? N13 .6410(2) .5956(3) .57094(11) .0381(18) Uani ? ? 1.00000 ? ? C14 .5903(4) .4583(4) .58073(18) .053(3) Uani ? ? 1.00000 ? ? C15 .6000(4) .4273(5) .63378(18) .058(3) Uani ? ? 1.00000 ? ? N16 .5636(3) .5542(4) .65937(14) .048(2) Uani ? ? 1.00000 ? ? C111' .7844(4) .7741(7) .5140(2) .070(4) Uani ? ? 1.00000 ? ? C12' .6387(3) .9155(4) .53717(15) .047(2) Uani ? ? 1.00000 ? ? N13' .6576(2) .9063(3) .58959(12) .0391(18) Uani ? ? 1.00000 ? ? C14' .6239(4) 1.0360(4) .61535(18) .054(3) Uani ? ? 1.00000 ? ? C15' .6261(4) 1.0058(5) .66869(19) .059(3) Uani ? ? 1.00000 ? ? N16' .5727(3) .8717(4) .67712(14) .055(2) Uani ? ? 1.00000 ? ? C21 1.1705(3) .7774(4) .74528(14) .050(2) Uani ? ? 1.00000 ? ? C211 1.1474(7) .7793(9) .8000(2) .082(5) Uani ? ? 1.00000 ? ? C22 1.1141(3) .8976(4) .72127(14) .047(2) Uani ? ? 1.00000 ? ? N23 1.1317(2) .9117(3) .66895(11) .0367(17) Uani ? ? 1.00000 ? ? C24 1.0752(4) 1.0319(4) .64706(18) .050(3) Uani ? ? 1.00000 ? ? C25 1.0841(4) 1.0230(5) .59362(17) .054(3) Uani ? ? 1.00000 ? ? N26 1.0537(3) .8769(4) .57959(14) .053(2) Uani ? ? 1.00000 ? ? C211' 1.2785(4) .7993(7) .7403(2) .064(3) Uani ? ? 1.00000 ? ? C22' 1.1396(3) .6285(4) .72792(14) .045(2) Uani ? ? 1.00000 ? ? N23' 1.1614(2) .5986(3) .67647(12) .0379(18) Uani ? ? 1.00000 ? ? C24' 1.1300(3) .4505(4) .66179(17) .050(3) Uani ? ? 1.00000 ? ? C25' 1.1451(4) .4385(5) .60915(19) .060(3) Uani ? ? 1.00000 ? ? N26' 1.0957(4) .5598(5) .58502(17) .061(3) Uani ? ? 1.00000 ? ? Cl1 .35680(7) .73539(11) .58748(5) .0570(6) Uani ? ? 1.00000 ? ? O11 .4410(3) .8093(5) .5892(2) .120(3) Uani ? ? 1.00000 ? ? O12 .2720(2) .8128(4) .59028(16) .106(3) Uani ? ? 1.00000 ? ? O13 .3598(3) .6287(8) .6226(3) .249(8) Uani ? ? 1.00000 ? ? O14 .3566(5) .6691(12) .5455(3) .314(11) Uani ? ? 1.00000 ? ? Cl2 .85744(7) .74291(10) .66815(4) .0468(6) Uani ? ? 1.00000 ? ? O21 .9411(2) .6650(4) .65815(15) .087(3) Uani ? ? 1.00000 ? ? O22 .7725(2) .6602(3) .66104(13) .077(2) Uani ? ? 1.00000 ? ? O23 .8546(2) .8695(4) .63992(17) .111(3) Uani ? ? 1.00000 ? ? O24 .8648(4) .7836(6) .71733(17) .137(4) Uani ? ? 1.00000 ? ? Cl3 .63209(8) .71043(13) .80434(4) .0540(6) Uani ? ? 1.00000 ? ? O31 .5863(4) .6453(6) .76550(15) .136(4) Uani ? ? 1.00000 ? ? O32 .6384(4) .8569(5) .7966(2) .164(5) Uani ? ? 1.00000 ? ? O33 .5744(4) .6895(8) .84388(16) .176(5) Uani ? ? 1.00000 ? ? O34 .7235(3) .6536(4) .8149(2) .118(3) Uani ? ? 1.00000 ? ? Cl4 .87074(8) .29589(14) .55120(4) .0580(7) Uani ? ? 1.00000 ? ? O41 .9311(4) .3260(7) .58970(18) .158(5) Uani ? ? 1.00000 ? ? O42 .878(4) .383(3) .5162(7) .38(4) Uani ? ? .50000 ? ? O43 .7831(8) .319(3) .5700(6) .224(16) Uani ? ? .50000 ? ? O44 .8807(14) .1761(18) .5242(5) .158(13) Uani ? ? .50000 ? ? O42' .8191(12) .410(2) .5307(7) .180(15) Uani ? ? .50000 ? ? O43' .8336(13) .1669(15) .5658(6) .165(12) Uani ? ? .50000 ? ? O44' .9486(9) .280(2) .5214(4) .129(10) Uani ? ? .50000 ? ? H111a .656(4) .719(6) .4337(19) .088(18) Uiso ? ? 1.00000 ? ? H111b .589(3) .822(4) .4478(14) .038(12) Uiso ? ? 1.00000 ? ? H111c .679(4) .908(5) .4455(17) .077(17) Uiso ? ? 1.00000 ? ? H12a .555(3) .651(4) .5197(12) .041(10) Uiso ? ? 1.00000 ? ? H12b .653(3) .571(5) .4954(16) .091(16) Uiso ? ? 1.00000 ? ? H13 .697(3) .579(4) .5764(13) .040(11) Uiso ? ? 1.00000 ? ? H14a .528(3) .460(5) .5724(15) .065(15) Uiso ? ? 1.00000 ? ? H14b .614(3) .394(5) .5639(14) .052(12) Uiso ? ? 1.00000 ? ? H15a .570(3) .355(5) .6432(14) .050(12) Uiso ? ? 1.00000 ? ? H15b .669(3) .415(5) .6403(15) .064(14) Uiso ? ? 1.00000 ? ? H16a .508(3) .558(5) .6554(14) .051(14) Uiso ? ? 1.00000 ? ? H16 .585(3) .548(4) .6865(14) .046(13) Uiso ? ? 1.00000 ? ? H111'a .813(3) .755(4) .5462(15) .047(12) Uiso ? ? 1.00000 ? ? H111'b .813(4) .708(6) .4967(18) .088(18) Uiso ? ? 1.00000 ? ? H111'c .824(4) .874(7) .513(2) .13(2) Uiso ? ? 1.00000 ? ? H12'a .668(3) 1.010(4) .5269(13) .054(11) Uiso ? ? 1.00000 ? ? H12'b .571(3) .926(3) .5339(11) .028(9) Uiso ? ? 1.00000 ? ? H13' .713(3) .897(4) .5966(12) .033(10) Uiso ? ? 1.00000 ? ? H14'a .664(3) 1.114(5) .6028(15) .075(14) Uiso ? ? 1.00000 ? ? H14'b .558(3) 1.054(4) .6059(13) .050(12) Uiso ? ? 1.00000 ? ? H15'a .686(3) .991(5) .6792(15) .069(15) Uiso ? ? 1.00000 ? ? H15'b .602(2) 1.081(4) .6839(12) .038(10) Uiso ? ? 1.00000 ? ? H16'a .579(3) .818(5) .7031(16) .061(14) Uiso ? ? 1.00000 ? ? H16'b .506(4) .873(5) .6751(16) .078(17) Uiso ? ? 1.00000 ? ? H211a 1.100(3) .784(5) .8004(16) .022(13) Uiso ? ? 1.00000 ? ? H211b 1.199(4) .705(5) .8156(18) .083(17) Uiso ? ? 1.00000 ? ? H211c 1.170(4) .882(6) .8141(18) .096(18) Uiso ? ? 1.00000 ? ? H22a 1.051(3) .884(4) .7222(13) .051(12) Uiso ? ? 1.00000 ? ? H22b 1.129(2) .991(4) .7389(12) .041(10) Uiso ? ? 1.00000 ? ? H23 1.193(3) .930(4) .6633(11) .032(10) Uiso ? ? 1.00000 ? ? H24a 1.018(3) 1.021(4) .6528(14) .050(13) Uiso ? ? 1.00000 ? ? H24b 1.101(3) 1.117(5) .6570(15) .061(13) Uiso ? ? 1.00000 ? ? H25a 1.037(3) 1.109(4) .5777(13) .053(11) Uiso ? ? 1.00000 ? ? H25b 1.148(3) 1.028(5) .5899(15) .067(15) Uiso ? ? 1.00000 ? ? H26a .996(4) .868(5) .5760(17) .078(19) Uiso ? ? 1.00000 ? ? H26b 1.078(3) .840(5) .5553(15) .059(15) Uiso ? ? 1.00000 ? ? H211'a 1.302(3) .811(5) .7096(16) .065(15) Uiso ? ? 1.00000 ? ? H211'b 1.294(4) .877(6) .7529(18) .087(19) Uiso ? ? 1.00000 ? ? H211'c 1.327(4) .735(5) .754(2) .093(18) Uiso ? ? 1.00000 ? ? H22'a 1.165(3) .549(5) .7481(14) .063(12) Uiso ? ? 1.00000 ? ? H22'b 1.070(3) .609(4) .7327(12) .049(11) Uiso ? ? 1.00000 ? ? H23' 1.215(3) .599(4) .6738(12) .029(10) Uiso ? ? 1.00000 ? ? H24'a 1.171(4) .378(7) .679(2) .13(2) Uiso ? ? 1.00000 ? ? H24'b 1.065(3) .446(4) .6665(12) .034(10) Uiso ? ? 1.00000 ? ? H25'a 1.220(3) .446(5) .6030(15) .076(14) Uiso ? ? 1.00000 ? ? H25'b 1.121(3) .368(4) .5966(13) .043(11) Uiso ? ? 1.00000 ? ? H26'a 1.118(5) .586(7) .559(2) .13(3) Uiso ? ? 1.00000 ? ? H26'b 1.047(3) .547(5) .5840(17) .053(19) Uiso ? ? 1.00000 ? ? 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 .0387(3) .0289(2) .0351(3) .00095(17) -.00128(18) -.00168(17) Cu2 .0387(3) .0279(2) .0390(3) .00037(17) .00284(19) .00074(17) C11 .055(3) .063(3) .037(2) .009(2) .0104(19) .0066(18) C111 .088(5) .108(5) .047(3) .025(4) .004(3) .027(3) C12 .055(3) .050(2) .038(2) .011(2) -.0015(19) -.0061(17) N13 .040(2) .0346(16) .0395(18) .0036(13) -.0025(14) -.0038(12) C14 .061(3) .030(2) .067(3) -.0030(19) -.003(2) -.012(2) C15 .064(3) .032(2) .079(3) -.006(2) -.002(3) .014(2) N16 .047(2) .050(2) .047(2) -.0051(17) -.0021(18) .0101(16) C111' .055(3) .090(4) .065(3) .014(3) .018(3) .006(3) C12' .048(3) .042(2) .052(3) .0057(18) .006(2) .0121(18) N13' .0313(18) .0331(16) .053(2) .0004(13) -.0004(15) -.0033(13) C14' .064(3) .029(2) .071(3) .0024(19) .006(2) -.0064(19) C15' .056(3) .048(3) .074(3) .013(2) -.013(2) -.027(2) N16' .071(3) .050(2) .044(2) .011(2) .003(2) -.0076(17) C21 .062(3) .049(2) .041(2) -.0105(19) -.011(2) .0040(17) C211 .095(6) .105(6) .045(3) -.003(5) -.001(4) -.003(3) C22 .050(3) .044(2) .046(2) -.0022(18) .000(2) -.0094(17) N23 .0347(18) .0276(15) .0478(18) -.0006(12) -.0051(14) .0029(12) C24 .046(3) .028(2) .075(3) .0026(17) -.007(2) .0049(19) C25 .052(3) .044(2) .068(3) .008(2) -.002(2) .021(2) N26 .052(3) .058(2) .049(2) .0057(19) -.000(2) .0094(17) C211' .054(3) .067(3) .069(4) -.012(3) -.021(3) .012(3) C22' .048(2) .043(2) .043(2) -.0035(18) .0021(18) .0104(17) N23' .0272(17) .0279(15) .059(2) .0009(12) .0010(15) .0011(13) C24' .047(3) .0272(19) .076(3) -.0022(17) -.002(2) -.0002(18) C25' .064(3) .034(2) .082(4) -.002(2) .014(3) -.021(2) N26' .078(4) .046(2) .058(3) -.011(2) .006(2) -.0103(18) Cl1 .0301(5) .0521(6) .0890(8) -.0000(4) .0046(5) -.0067(6) O11 .052(2) .098(3) .210(5) -.021(2) -.009(3) .032(3) O12 .050(2) .105(3) .162(4) .029(2) .033(2) .039(3) O13 .067(3) .205(7) .476(13) .029(4) .061(5) .234(8) O14 .172(7) .428(14) .339(11) .096(8) -.062(7) -.312(11) Cl2 .0287(5) .0478(5) .0639(6) .0012(4) -.0011(4) .0003(4) O21 .046(2) .068(2) .148(3) .0115(16) .018(2) .006(2) O22 .0399(18) .064(2) .128(3) -.0133(15) -.0181(18) .016(2) O23 .054(2) .080(3) .199(4) -.0063(18) -.017(2) .064(3) O24 .124(4) .185(5) .103(4) -.048(4) .023(3) -.063(3) Cl3 .0468(6) .0684(7) .0470(6) .0074(5) .0037(5) -.0037(5) O31 .172(5) .156(5) .079(3) .008(4) -.043(3) -.027(3) O32 .137(5) .074(3) .278(7) .022(3) -.055(5) -.001(4) O33 .095(4) .357(9) .075(3) .008(5) .028(3) .036(4) O34 .055(2) .078(3) .219(5) .011(2) -.015(3) -.008(3) Cl4 .0522(7) .0694(7) .0524(6) .0063(5) -.0013(5) -.0060(5) O41 .167(5) .197(6) .109(4) -.038(5) -.036(4) -.029(4) O42 .79(7) .28(4) .084(10) -.08(4) .02(3) .101(16) O43 .063(7) .43(3) .179(13) .013(11) .053(8) -.099(16) O44 .214(16) .149(12) .112(9) .065(11) -.003(10) -.052(9) O42' .151(11) .170(13) .22(2) .124(11) .048(12) .073(13) O43' .207(15) .122(10) .167(12) -.097(10) .011(11) .033(9) O44' .116(9) .175(14) .098(8) .049(8) .054(7) .039(8) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Cu1 N13 . . 2.011(3) ? Cu1 N16 . . 2.008(4) ? Cu1 N13' . . 2.010(3) ? Cu1 N16' . . 2.013(4) ? Cu1 O11 . . 2.588(4) ? Cu1 O22 . . 2.596(3) ? Cu2 N23 . . 2.021(3) ? Cu2 N26 . . 2.002(4) ? Cu2 N23' . . 2.001(3) ? Cu2 N26' . . 2.014(4) ? Cu2 O21 . . 2.573(3) ? Cu2 O12 . '1 655' 2.600(4) ? C11 C111 . . 1.557(7) ? C11 C12 . . 1.540(6) ? C11 C111' . . 1.505(7) ? C11 C12' . . 1.515(6) ? C111 H111a . . 1.12(5) ? C111 H111b . . .87(4) ? C111 H111c . . .95(5) ? C12 N13 . . 1.487(5) ? C12 H12a . . .96(4) ? C12 H12b . . 1.07(5) ? N13 C14 . . 1.480(5) ? N13 H13 . . .81(4) ? C14 C15 . . 1.506(7) ? C14 H14a . . .90(5) ? C14 H14b . . .83(4) ? C15 N16 . . 1.465(6) ? C15 H15a . . .83(4) ? C15 H15b . . .99(5) ? N16 H16a . . .78(4) ? N16 H16 . . .81(4) ? C111' H111'a . . .99(4) ? C111' H111'b . . .88(5) ? C111' H111'c . . 1.07(6) ? C12' N13' . . 1.479(5) ? C12' H12'a . . 1.00(4) ? C12' H12'b . . .95(4) ? N13' C14' . . 1.476(5) ? N13' H13' . . .79(4) ? C14' C15' . . 1.508(7) ? C14' H14'a . . .98(5) ? C14' H14'b . . .97(4) ? C15' N16' . . 1.466(6) ? C15' H15'a . . .89(5) ? C15' H15'b . . .89(4) ? N16' H16'a . . .88(4) ? N16' H16'b . . .93(5) ? C21 C211 . . 1.557(8) ? C21 C22 . . 1.511(6) ? C21 C211' . . 1.522(7) ? C21 C22' . . 1.519(6) ? C211 H211a . . .66(4) ? C211 H211b . . 1.08(5) ? C211 H211c . . 1.07(5) ? C22 N23 . . 1.482(5) ? C22 H22a . . .88(4) ? C22 H22b . . 1.02(4) ? N23 C24 . . 1.487(5) ? N23 H23 . . .89(4) ? C24 C25 . . 1.493(7) ? C24 H24a . . .81(4) ? C24 H24b . . .91(4) ? C25 N26 . . 1.468(6) ? C25 H25a . . 1.12(4) ? C25 H25b . . .89(5) ? N26 H26a . . .80(5) ? N26 H26b . . .83(4) ? C211' H211'a . . .92(5) ? C211' H211'b . . .83(5) ? C211' H211'c . . .97(6) ? C22' N23' . . 1.490(5) ? C22' H22'a . . .99(4) ? C22' H22'b . . 1.00(4) ? N23' C24' . . 1.493(5) ? N23' H23' . . .75(4) ? C24' C25' . . 1.484(7) ? C24' H24'a . . 1.00(6) ? C24' H24'b . . .92(4) ? C25' N26' . . 1.473(7) ? C25' H25'a . . 1.06(5) ? C25' H25'b . . .82(4) ? N26' H26'a . . .83(6) ? N26' H26'b . . .69(4) ? Cl1 O11 . . 1.355(4) ? Cl1 O12 . . 1.382(4) ? Cl1 O13 . . 1.388(8) ? Cl1 O14 . . 1.319(10) ? Cl2 O21 . . 1.398(3) ? Cl2 O22 . . 1.419(3) ? Cl2 O23 . . 1.410(4) ? Cl2 O24 . . 1.420(5) ? Cl3 O31 . . 1.384(5) ? Cl3 O32 . . 1.375(5) ? Cl3 O33 . . 1.380(5) ? Cl3 O34 . . 1.403(4) ? Cl4 O41 . . 1.380(6) ? Cl4 O42 . . 1.27(2) ? Cl4 O43 . . 1.348(13) ? Cl4 O44 . . 1.346(16) ? Cl4 O42' . . 1.395(19) ? Cl4 O43' . . 1.364(15) ? Cl4 O44' . . 1.377(13) ? O41 O44' . . 1.962(14) ? O42 O44 . . 1.93(3) ? O42 O42' . . .94(5) ? O42 O44' . . 1.38(4) ? O43 O42' . . 1.47(3) ? O43 O43' . . 1.58(3) ? O44 O43' . . 1.34(2) ? O44 O44' . . 1.35(2) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published N13 Cu1 N16 . . . 85.17(14) ? N13 Cu1 N13' . . . 93.55(13) ? N13 Cu1 N16' . . . 179.12(15) ? N13 Cu1 O11 . . . 96.47(15) ? N13 Cu1 O22 . . . 84.87(12) ? N16 Cu1 N13' . . . 176.62(15) ? N16 Cu1 N16' . . . 95.71(16) ? N16 Cu1 O11 . . . 98.13(16) ? N16 Cu1 O22 . . . 82.28(14) ? N13' Cu1 N16' . . . 85.57(14) ? N13' Cu1 O11 . . . 85.11(14) ? N13' Cu1 O22 . . . 94.50(12) ? N16' Cu1 O11 . . . 83.39(17) ? N16' Cu1 O22 . . . 95.27(15) ? O11 Cu1 O22 . . . 178.62(14) ? N23 Cu2 N26 . . . 84.94(14) ? N23 Cu2 N23' . . . 93.68(12) ? N23 Cu2 N26' . . . 176.0(2) ? N23 Cu2 O21 . . . 98.75(12) ? N23 Cu2 O12 . . '1 655' 82.69(13) ? N26 Cu2 N23' . . . 178.20(15) ? N26 Cu2 N26' . . . 96.42(18) ? N26 Cu2 O21 . . . 92.77(15) ? N26 Cu2 O12 . . '1 655' 83.61(16) ? N23' Cu2 N26' . . . 85.03(16) ? N23' Cu2 O21 . . . 86.29(13) ? N23' Cu2 O12 . . '1 655' 97.38(13) ? N26' Cu2 O21 . . . 85.00(19) ? N26' Cu2 O12 . . '1 655' 93.7(2) ? O21 Cu2 O12 . . '1 655' 175.99(13) ? C111 C11 C12 . . . 104.8(4) ? C111 C11 C111' . . . 109.9(4) ? C111 C11 C12' . . . 105.7(4) ? C12 C11 C111' . . . 112.0(4) ? C12 C11 C12' . . . 112.2(3) ? C111' C11 C12' . . . 111.8(4) ? C11 C111 H111a . . . 110(3) ? C11 C111 H111b . . . 117(3) ? C11 C111 H111c . . . 109(3) ? H111a C111 H111b . . . 88(4) ? H111a C111 H111c . . . 122(4) ? H111b C111 H111c . . . 110(4) ? C11 C12 N13 . . . 113.9(3) ? C11 C12 H12a . . . 116(2) ? C11 C12 H12b . . . 104(3) ? N13 C12 H12a . . . 101(2) ? N13 C12 H12b . . . 111(3) ? H12a C12 H12b . . . 113(3) ? Cu1 N13 C12 . . . 117.1(2) ? Cu1 N13 C14 . . . 106.7(3) ? Cu1 N13 H13 . . . 103(3) ? C12 N13 C14 . . . 112.1(3) ? C12 N13 H13 . . . 112(3) ? C14 N13 H13 . . . 105(3) ? N13 C14 C15 . . . 107.8(4) ? N13 C14 H14a . . . 114(3) ? N13 C14 H14b . . . 109(3) ? C15 C14 H14a . . . 109(3) ? C15 C14 H14b . . . 112(3) ? H14a C14 H14b . . . 105(4) ? C14 C15 N16 . . . 107.1(4) ? C14 C15 H15a . . . 115(3) ? C14 C15 H15b . . . 106(2) ? N16 C15 H15a . . . 108(3) ? N16 C15 H15b . . . 110(2) ? H15a C15 H15b . . . 110(4) ? Cu1 N16 C15 . . . 108.5(3) ? Cu1 N16 H16a . . . 101(3) ? Cu1 N16 H16 . . . 114(3) ? C15 N16 H16a . . . 108(3) ? C15 N16 H16 . . . 106(3) ? H16a N16 H16 . . . 119(4) ? C11 C111' H111'a . . . 120(3) ? C11 C111' H111'b . . . 118(4) ? C11 C111' H111'c . . . 115(3) ? H111'a C111' H111'b . . . 101(4) ? H111'a C111' H111'c . . . 88(4) ? H111'b C111' H111'c . . . 110(5) ? C11 C12' N13' . . . 114.2(3) ? C11 C12' H12'a . . . 112(2) ? C11 C12' H12'b . . . 112.6(19) ? N13' C12' H12'a . . . 105(2) ? N13' C12' H12'b . . . 105.4(18) ? H12'a C12' H12'b . . . 107(3) ? Cu1 N13' C12' . . . 117.3(2) ? Cu1 N13' C14' . . . 107.7(3) ? Cu1 N13' H13' . . . 98(2) ? C12' N13' C14' . . . 112.1(3) ? C12' N13' H13' . . . 114(2) ? C14' N13' H13' . . . 106(2) ? N13' C14' C15' . . . 108.8(3) ? N13' C14' H14'a . . . 104(3) ? N13' C14' H14'b . . . 108(2) ? C15' C14' H14'a . . . 119(3) ? C15' C14' H14'b . . . 108(2) ? H14'a C14' H14'b . . . 109(4) ? C14' C15' N16' . . . 108.0(4) ? C14' C15' H15'a . . . 111(3) ? C14' C15' H15'b . . . 109(2) ? N16' C15' H15'a . . . 107(3) ? N16' C15' H15'b . . . 113(2) ? H15'a C15' H15'b . . . 109(4) ? Cu1 N16' C15' . . . 107.7(3) ? Cu1 N16' H16'a . . . 102(3) ? Cu1 N16' H16'b . . . 102(3) ? C15' N16' H16'a . . . 124(3) ? C15' N16' H16'b . . . 119(3) ? H16'a N16' H16'b . . . 98(4) ? C211 C21 C22 . . . 108.1(4) ? C211 C21 C211' . . . 107.5(5) ? C211 C21 C22' . . . 105.0(4) ? C22 C21 C211' . . . 111.6(4) ? C22 C21 C22' . . . 112.6(3) ? C211' C21 C22' . . . 111.5(4) ? C21 C211 H211a . . . 103(4) ? C21 C211 H211b . . . 104(3) ? C21 C211 H211c . . . 108(3) ? H211a C211 H211b . . . 134(5) ? H211a C211 H211c . . . 103(5) ? H211b C211 H211c . . . 103(4) ? C21 C22 N23 . . . 114.0(3) ? C21 C22 H22a . . . 113(3) ? C21 C22 H22b . . . 108(2) ? N23 C22 H22a . . . 102(2) ? N23 C22 H22b . . . 111(2) ? H22a C22 H22b . . . 108(3) ? Cu2 N23 C22 . . . 117.7(2) ? Cu2 N23 C24 . . . 106.7(2) ? Cu2 N23 H23 . . . 102(2) ? C22 N23 C24 . . . 112.0(3) ? C22 N23 H23 . . . 111(2) ? C24 N23 H23 . . . 107(2) ? N23 C24 C25 . . . 108.4(3) ? N23 C24 H24a . . . 109(3) ? N23 C24 H24b . . . 109(3) ? C25 C24 H24a . . . 106(3) ? C25 C24 H24b . . . 108(3) ? H24a C24 H24b . . . 116(4) ? C24 C25 N26 . . . 106.7(4) ? C24 C25 H25a . . . 107.4(19) ? C24 C25 H25b . . . 102(3) ? N26 C25 H25a . . . 112(2) ? N26 C25 H25b . . . 108(3) ? H25a C25 H25b . . . 120(4) ? Cu2 N26 C25 . . . 108.6(3) ? Cu2 N26 H26a . . . 113(4) ? Cu2 N26 H26b . . . 97(3) ? C25 N26 H26a . . . 114(4) ? C25 N26 H26b . . . 118(3) ? H26a N26 H26b . . . 106(5) ? C21 C211' H211'a . . . 117(3) ? C21 C211' H211'b . . . 109(4) ? C21 C211' H211'c . . . 124(3) ? H211'a C211' H211'b . . . 101(4) ? H211'a C211' H211'c . . . 101(4) ? H211'b C211' H211'c . . . 101(5) ? C21 C22' N23' . . . 114.4(3) ? C21 C22' H22'a . . . 113(2) ? C21 C22' H22'b . . . 113(2) ? N23' C22' H22'a . . . 109(2) ? N23' C22' H22'b . . . 108(2) ? H22'a C22' H22'b . . . 98(3) ? Cu2 N23' C22' . . . 117.4(2) ? Cu2 N23' C24' . . . 107.0(3) ? Cu2 N23' H23' . . . 107(3) ? C22' N23' C24' . . . 111.8(3) ? C22' N23' H23' . . . 108(3) ? C24' N23' H23' . . . 105(3) ? N23' C24' C25' . . . 107.1(3) ? N23' C24' H24'a . . . 109(4) ? N23' C24' H24'b . . . 107(2) ? C25' C24' H24'a . . . 110(3) ? C25' C24' H24'b . . . 107(2) ? H24'a C24' H24'b . . . 117(4) ? C24' C25' N26' . . . 108.7(4) ? C24' C25' H25'a . . . 108(2) ? C24' C25' H25'b . . . 115(3) ? N26' C25' H25'a . . . 109(2) ? N26' C25' H25'b . . . 103(3) ? H25'a C25' H25'b . . . 113(4) ? Cu2 N26' C25' . . . 108.3(3) ? Cu2 N26' H26'a . . . 104(5) ? Cu2 N26' H26'b . . . 104(4) ? C25' N26' H26'a . . . 116(5) ? C25' N26' H26'b . . . 110(4) ? H26'a N26' H26'b . . . 113(6) ? O11 Cl1 O12 . . . 118.2(3) ? O11 Cl1 O13 . . . 108.4(3) ? O11 Cl1 O14 . . . 105.0(4) ? O12 Cl1 O13 . . . 110.3(3) ? O12 Cl1 O14 . . . 107.3(4) ? O13 Cl1 O14 . . . 106.9(6) ? Cu1 O11 Cl1 . . . 129.6(3) ? Cl1 O12 Cu2 . . '1 455' 129.0(2) ? O21 Cl2 O22 . . . 112.7(2) ? O21 Cl2 O23 . . . 109.6(2) ? O21 Cl2 O24 . . . 106.1(3) ? O22 Cl2 O23 . . . 110.7(2) ? O22 Cl2 O24 . . . 109.1(3) ? O23 Cl2 O24 . . . 108.5(3) ? Cu2 O21 Cl2 . . . 133.7(2) ? Cu1 O22 Cl2 . . . 130.49(19) ? O31 Cl3 O32 . . . 109.6(4) ? O31 Cl3 O33 . . . 107.1(3) ? O31 Cl3 O34 . . . 114.0(3) ? O32 Cl3 O33 . . . 107.6(4) ? O32 Cl3 O34 . . . 110.1(3) ? O33 Cl3 O34 . . . 108.2(3) ? O41 Cl4 O42 . . . 114.5(17) ? O41 Cl4 O43 . . . 102.1(7) ? O41 Cl4 O44 . . . 122.2(8) ? O41 Cl4 O42' . . . 117.9(8) ? O41 Cl4 O43' . . . 100.0(7) ? O41 Cl4 O44' . . . 90.7(6) ? O42 Cl4 O43 . . . 106(2) ? O42 Cl4 O44 . . . 95.2(13) ? O42 Cl4 O42' . . . 41(2) ? O42 Cl4 O43' . . . 144.9(17) ? O42 Cl4 O44' . . . 63(2) ? O43 Cl4 O44 . . . 116.6(14) ? O43 Cl4 O42' . . . 64.8(13) ? O43 Cl4 O43' . . . 71.3(14) ? O43 Cl4 O44' . . . 165.7(9) ? O44 Cl4 O42' . . . 116.9(11) ? O44 Cl4 O43' . . . 59.1(10) ? O44 Cl4 O44' . . . 59.5(11) ? O42' Cl4 O43' . . . 126.2(10) ? O42' Cl4 O44' . . . 103.8(10) ? O43' Cl4 O44' . . . 112.8(10) ? Cl4 O41 O44' . . . 44.6(4) ? Cl4 O42 O44 . . . 43.9(10) ? Cl4 O42 O42' . . . 77(2) ? Cl4 O42 O44' . . . 62.5(15) ? O44 O42 O42' . . . 103(3) ? O44 O42 O44' . . . 44.4(12) ? O42' O42 O44' . . . 139(3) ? Cl4 O43 O42' . . . 59.1(9) ? Cl4 O43 O43' . . . 54.8(10) ? O42' O43 O43' . . . 107.4(13) ? Cl4 O44 O42 . . . 40.9(7) ? Cl4 O44 O43' . . . 61.1(9) ? Cl4 O44 O44' . . . 61.4(10) ? O42 O44 O43' . . . 98.7(14) ? O42 O44 O44' . . . 45.6(17) ? O43' O44 O44' . . . 116.4(14) ? Cl4 O42' O42 . . . 62.3(18) ? Cl4 O42' O43 . . . 56.1(10) ? O42 O42' O43 . . . 118(2) ? Cl4 O43' O43 . . . 53.9(8) ? Cl4 O43' O44 . . . 59.8(10) ? O43 O43' O44 . . . 103.3(13) ? Cl4 O44' O41 . . . 44.7(4) ? Cl4 O44' O42 . . . 54.8(13) ? Cl4 O44' O44 . . . 59.1(9) ? O41 O44' O42 . . . 81.6(10) ? O41 O44' O44 . . . 90.2(9) ? O42 O44' O44 . . . 90(2) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- 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 C11 3.407(4) . . ? Cu1 C12 2.997(4) . . ? Cu1 C14 2.817(4) . . ? Cu1 C15 2.836(4) . . ? Cu1 C12' 2.993(4) . . ? Cu1 C14' 2.831(4) . . ? Cu1 C15' 2.827(5) . . ? Cu1 Cl1 3.6054(11) . . ? Cu1 O13 3.559(5) . . ? Cu1 Cl2 3.6792(10) . . ? Cu1 O23 3.692(4) . . ? Cu1 H12a 3.08(3) . . ? Cu1 H13 2.32(4) . . ? Cu1 H14a 3.10(4) . . ? Cu1 H15b 3.09(4) . . ? Cu1 H16a 2.29(4) . . ? Cu1 H16 2.45(4) . . ? Cu1 H12'b 3.12(3) . . ? Cu1 H13' 2.26(4) . . ? Cu1 H14'b 3.09(4) . . ? Cu1 H15'a 3.04(4) . . ? Cu1 H16'a 2.36(4) . . ? Cu1 H16'b 2.38(5) . . ? Cu2 C21 3.403(4) . . ? Cu2 C22 3.011(4) . . ? Cu2 C24 2.833(4) . . ? Cu2 C25 2.835(4) . . ? Cu2 C22' 2.996(4) . . ? Cu2 C24' 2.825(4) . . ? Cu2 C25' 2.844(4) . . ? Cu2 Cl1 3.6316(11) . '1 655' ? Cu2 O13 3.631(5) . '1 655' ? Cu2 Cl2 3.6804(11) . . ? Cu2 H22a 3.08(4) . . ? Cu2 H23 2.37(3) . . ? Cu2 H24a 3.01(4) . . ? Cu2 H25b 2.95(5) . . ? Cu2 H26a 2.43(5) . . ? Cu2 H26b 2.25(4) . . ? Cu2 H22'b 3.21(3) . . ? Cu2 H23' 2.33(3) . . ? Cu2 H24'b 2.96(3) . . ? Cu2 H25'a 3.18(5) . . ? Cu2 H26'a 2.36(6) . . ? Cu2 H26'b 2.28(5) . . ? C11 N13 2.538(5) . . ? C11 N13' 2.514(5) . . ? C11 H111a 2.20(5) . . ? C11 H111b 2.10(4) . . ? C11 H111c 2.08(5) . . ? C11 H12a 2.14(4) . . ? C11 H12b 2.08(5) . . ? C11 H111'a 2.17(4) . . ? C11 H111'b 2.07(6) . . ? C11 H111'c 2.19(6) . . ? C11 H12'a 2.11(4) . . ? C11 H12'b 2.07(3) . . ? C11 H13' 2.68(3) . . ? C111 C12 2.454(8) . . ? C111 C111' 2.507(9) . . ? C111 C12' 2.448(7) . . ? C111 H12b 2.56(5) . . ? C111 H12'a 2.66(4) . . ? C111 H12'b 2.64(3) . . ? C12 C14 2.461(6) . . ? C12 C111' 2.524(7) . . ? C12 C12' 2.536(6) . . ? C12 H111a 2.55(5) . . ? C12 H111b 2.64(4) . . ? C12 H13 1.94(4) . . ? C12 H14a 2.63(4) . . ? C12 H14b 2.63(4) . . ? N13 C15 2.412(6) . . ? N13 N16 2.719(5) . . ? N13 C111' 3.044(7) . . ? N13 N13' 2.930(4) . . ? N13 O22 3.139(5) . . ? N13 H12a 1.91(4) . . ? N13 H12b 2.12(5) . . ? N13 H14a 2.02(5) . . ? N13 H14b 1.92(4) . . ? N13 H15b 2.58(4) . . ? C14 N16 2.390(6) . . ? C14 O43 2.988(17) . . ? C14 H12a 2.50(3) . . ? C14 H13 1.86(4) . . ? C14 H15a 2.00(4) . . ? C14 H15b 2.02(4) . . ? C14 H16a 2.55(4) . . ? C15 H13 2.53(4) . . ? C15 H14a 1.99(4) . . ? C15 H14b 1.98(4) . . ? C15 H16a 1.87(4) . . ? C15 H16 1.86(4) . . ? N16 N16' 2.981(5) . . ? N16 O13 3.078(7) . . ? N16 O22 3.061(5) . . ? N16 O31 3.079(6) . . ? N16 H14a 2.61(4) . . ? N16 H15a 1.90(4) . . ? N16 H15b 2.03(4) . . ? N16 H16'a 2.73(4) . . ? C111' C12' 2.500(7) . . ? C111' N13' 3.015(7) . . ? C111' H111c 2.69(5) . . ? C111' H12b 2.67(5) . . ? C12' C14' 2.452(6) . . ? C12' H111c 2.62(5) . . ? C12' H111'c 2.70(6) . . ? C12' H13' 1.94(3) . . ? C12' H14'a 2.61(5) . . ? C12' H14'b 2.57(4) . . ? N13' C15' 2.427(6) . . ? N13' N16' 2.733(5) . . ? N13' O11 3.139(5) . . ? N13' O23 3.078(5) . . ? N13' H12'a 1.99(4) . . ? N13' H12'b 1.96(3) . . ? N13' H14'a 1.96(5) . . ? N13' H14'b 2.00(4) . . ? N13' H15'a 2.64(4) . . ? C14' N16' 2.406(6) . . ? C14' H12'a 2.55(4) . . ? C14' H12'b 2.58(3) . . ? C14' H13' 1.86(4) . . ? C14' H15'a 2.01(4) . . ? C14' H15'b 1.98(3) . . ? C15' H13' 2.55(3) . . ? C15' H14'a 2.16(4) . . ? C15' H14'b 2.03(4) . . ? C15' H16'a 2.09(4) . . ? C15' H16'b 2.09(5) . . ? N16' O11 3.090(6) . . ? N16' H14'b 2.61(4) . . ? N16' H15'a 1.92(5) . . ? N16' H15'b 1.99(4) . . ? C21 N23 2.511(5) . . ? C21 N23' 2.530(5) . . ? C21 H211a 1.83(4) . . ? C21 H211b 2.10(5) . . ? C21 H211c 2.14(5) . . ? C21 H22a 2.02(4) . . ? C21 H22b 2.07(4) . . ? C21 H211'a 2.11(5) . . ? C21 H211'b 1.96(5) . . ? C21 H211'c 2.22(6) . . ? C21 H22'a 2.12(4) . . ? C21 H22'b 2.12(4) . . ? C21 H23' 2.66(3) . . ? C211 C22 2.485(8) . . ? C211 C211' 2.483(10) . . ? C211 C22' 2.441(8) . . ? C211 H22b 2.60(4) . . ? C211 H211'b 2.60(5) . . ? C211 H22'a 2.59(4) . . ? C211 H22'b 2.67(4) . . ? C22 C24 2.462(6) . . ? C22 C211' 2.509(7) . . ? C22 C22' 2.521(6) . . ? C22 H211a 2.44(4) . . ? C22 H211c 2.69(5) . . ? C22 H23 1.98(3) . . ? C22 H24a 2.57(4) . . ? C22 H211'b 2.65(5) . . ? N23 C25 2.418(6) . . ? N23 N26 2.716(5) . . ? N23 C211' 3.013(6) . . ? N23 C22' 3.091(5) . . ? N23 N23' 2.934(4) . . ? N23 O12 3.083(5) . '1 655' ? N23 O34 3.039(5) . '2 756' ? N23 H22a 1.88(4) . . ? N23 H22b 2.08(3) . . ? N23 H24a 1.92(4) . . ? N23 H24b 1.98(5) . . ? N23 H25b 2.46(4) . . ? N23 H211'a 2.77(5) . . ? C24 N26 2.377(6) . . ? C24 H22a 2.52(4) . . ? C24 H22b 2.68(3) . . ? C24 H23 1.94(3) . . ? C24 H25a 2.12(4) . . ? C24 H25b 1.89(4) . . ? C25 H23 2.59(3) . . ? C25 H24a 1.89(4) . . ? C25 H24b 1.98(4) . . ? C25 H26a 1.94(5) . . ? C25 H26b 2.00(4) . . ? N26 N26' 2.994(6) . . ? N26 O12 3.100(6) . '1 655' ? N26 O44 3.073(16) . '3 766' ? N26 O44' 3.158(14) . '3 766' ? N26 H24a 2.48(4) . . ? N26 H25a 2.16(4) . . ? N26 H25b 1.93(5) . . ? C211' C22' 2.514(7) . . ? C211' N23' 3.029(7) . . ? C211' H211b 2.53(5) . . ? C211' H211c 2.67(5) . . ? C22' C24' 2.470(6) . . ? C22' H211a 2.54(4) . . ? C22' H211b 2.66(5) . . ? C22' H22a 2.67(4) . . ? C22' H23' 1.86(3) . . ? C22' H24'b 2.61(3) . . ? N23' C25' 2.394(6) . . ? N23' N26' 2.714(6) . . ? N23' O13 3.162(7) . '1 655' ? N23' O21 3.156(5) . . ? N23' H22'a 2.04(4) . . ? N23' H22'b 2.03(4) . . ? N23' H24'a 2.04(6) . . ? N23' H24'b 1.96(4) . . ? N23' H25'a 2.62(4) . . ? C24' N26' 2.403(7) . . ? C24' H22'a 2.61(4) . . ? C24' H22'b 2.60(4) . . ? C24' H23' 1.84(3) . . ? C24' H25'a 2.07(4) . . ? C24' H25'b 1.97(4) . . ? C24' H26'b 2.60(5) . . ? C25' H23' 2.51(3) . . ? C25' H24'a 2.05(6) . . ? C25' H24'b 1.96(3) . . ? C25' H26'a 1.98(6) . . ? C25' H26'b 1.83(5) . . ? N26' O21 3.127(7) . . ? N26' O41 3.150(8) . . ? N26' O42 2.89(2) . '3 766' ? N26' H26b 2.73(5) . . ? N26' H24'b 2.54(3) . . ? N26' H25'a 2.08(5) . . ? N26' H25'b 1.84(4) . . ? O11 O12 2.348(5) . . ? O11 O13 2.224(8) . . ? O11 O14 2.121(11) . . ? O11 H12'b 2.62(3) . . ? O11 H16'b 2.61(5) . . ? O12 O13 2.273(8) . . ? O12 O14 2.175(11) . . ? O12 H23 2.56(3) . '1 455' ? O12 H25b 2.64(5) . '1 455' ? O13 O14 2.175(13) . . ? O13 H16a 2.33(4) . . ? O13 H23' 2.49(4) . '1 455' ? O13 H25'a 2.63(5) . '1 455' ? O14 H12b 2.50(5) . '3 666' ? O21 O22 2.345(4) . . ? O21 O23 2.295(5) . . ? O21 O24 2.251(6) . . ? O21 H22'b 2.77(4) . . ? O21 H24'b 2.66(4) . . ? O21 H26'b 2.77(5) . . ? O22 O23 2.326(5) . . ? O22 O24 2.313(6) . . ? O22 H13 2.67(4) . . ? O22 H15b 2.74(4) . . ? O22 H211c 2.78(5) . '2 746' ? O23 O24 2.296(7) . . ? O23 H13' 2.31(4) . . ? O23 H24a 2.69(4) . . ? O23 H26a 2.67(5) . . ? O24 H22a 2.76(4) . . ? O24 H22'a 2.67(4) . '2 756' ? O31 O32 2.255(7) . . ? O31 O33 2.223(6) . . ? O31 O34 2.337(7) . . ? O31 H16 2.37(4) . . ? O31 H16'a 2.36(4) . . ? O32 O33 2.223(9) . . ? O32 O34 2.276(6) . . ? O32 H16'a 2.74(4) . . ? O32 H24'a 2.73(6) . '2 756' ? O33 O34 2.255(6) . . ? O33 H15a 2.55(4) . '2 656' ? O33 H14'b 2.63(4) . '2 646' ? O33 H15'b 2.74(4) . '2 646' ? O34 H23 2.44(3) . '2 746' ? O34 H24b 2.57(4) . '2 746' ? O34 H24'a 2.55(6) . '2 756' ? O41 O42 2.23(2) . . ? O41 O43 2.123(13) . . ? O41 O44 2.387(17) . . ? O41 O42' 2.38(2) . . ? O41 O43' 2.103(17) . . ? O41 H25a 2.51(4) . '1 545' ? O41 H25'b 2.67(4) . . ? O41 H26'b 2.61(5) . . ? O42 O43 2.09(4) . . ? O42 O43' 2.51(3) . . ? O42 H26'a 2.11(6) . '3 766' ? O43 O44 2.29(3) . . ? O43 O44' 2.704(18) . . ? O43 H13 2.69(5) . . ? O43 H14b 2.45(4) . . ? O43 H15b 2.67(5) . . ? O43 H14'a 2.68(5) . '1 545' ? O44 O42' 2.34(3) . . ? O44 H25a 2.69(4) . '1 545' ? O44 H26b 2.29(5) . '3 766' ? O42' O43' 2.46(2) . . ? O42' O44' 2.18(2) . . ? O42' H13 2.64(4) . . ? O42' H26'a 2.65(7) . '3 766' ? O43' O44' 2.28(2) . . ? O43' H14'a 2.62(5) . '1 545' ? O44' H25a 2.53(4) . '1 545' ? O44' H26b 2.43(5) . '3 766' ? O44' H26'a 2.71(6) . '3 766' ? H111a H111b 1.39(7) . . ? H111a H111c 1.81(7) . . ? H111a H12b 2.19(7) . . ? H111b H111c 1.49(6) . . ? H12a H12b 1.69(6) . . ? H12a H14a 2.33(6) . . ? H12b H13 2.32(6) . . ? H13 H14b 2.09(6) . . ? H13 H15b 2.37(5) . . ? H14a H14b 1.37(6) . . ? H14a H15a 2.26(6) . . ? H14b H15a 2.32(5) . . ? H14b H15b 2.26(6) . . ? H15a H15b 1.49(6) . . ? H15a H16a 2.09(6) . . ? H15a H16 2.16(6) . . ? H15b H16 2.14(6) . . ? H16a H16 1.37(6) . . ? H111'a H111'b 1.44(7) . . ? H111'a H111'c 1.44(7) . . ? H111'a H13' 2.39(5) . . ? H111'b H111'c 1.61(8) . . ? H12'a H12'b 1.57(5) . . ? H12'a H13' 2.28(5) . . ? H12'a H14'a 2.32(6) . . ? H12'b H14'b 2.33(5) . . ? H13' H14'a 2.12(6) . . ? H14'a H14'b 1.59(6) . . ? H14'b H15'b 2.26(5) . . ? H15'a H15'b 1.45(6) . . ? H15'a H16'a 2.29(6) . . ? H15'b H16'b 2.36(6) . . ? H16'a H16'b 1.37(7) . . ? H211a H211b 1.61(7) . . ? H211a H211c 1.38(7) . . ? H211b H211c 1.69(7) . . ? H211c H22b 2.38(6) . . ? H22a H22b 1.53(5) . . ? H22a H24a 2.35(5) . . ? H22b H23 2.36(5) . . ? H23 H24b 2.16(6) . . ? H23 H25b 2.31(5) . . ? H23 H211'a 2.26(6) . . ? H24a H24b 1.46(6) . . ? H24a H25a 2.26(5) . . ? H24b H25a 2.37(5) . . ? H24b H25b 2.14(6) . . ? H25a H25b 1.74(6) . . ? H25a H26a 2.30(6) . . ? H25b H26b 2.21(6) . . ? H26a H26b 1.30(7) . . ? H211'a H211'b 1.35(7) . . ? H211'a H211'c 1.47(7) . . ? H211'b H211'c 1.39(7) . . ? H22'a H22'b 1.50(6) . . ? H22'a H23' 2.23(5) . . ? H22'b H24'b 2.38(5) . . ? H23' H24'a 2.13(7) . . ? H24'a H24'b 1.64(7) . . ? H24'a H25'a 2.32(7) . . ? H24'a H25'b 2.39(7) . . ? H24'b H25'b 2.22(5) . . ? H25'a H25'b 1.57(6) . . ? H25'a H26'a 2.27(8) . . ? H25'b H26'a 2.27(8) . . ? H25'b H26'b 1.98(6) . . ? H26'a H26'b 1.27(8) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1864 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min -36 _reflns_limit_l_max 37 _reflns_number_observed ? _reflns_d_resolution_high .734 _reflns_d_resolution_low 13.85 _diffrn_reflns_av_sigmaI/netI .055 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970' _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .071 _refine_ls_wR_factor_all .072 _refine_ls_goodness_of_fit_all 2.004 _refine_ls_shift/su_mean .002 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_global _audit_creation_method Xtal3.6 _audit_creation_date 00-09-14 _audit_update_record ? #============================================================================== # (Publishing Staff Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia Nedlands Western Australia 6907 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal ? _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Skelton, Brian W.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_cuyk2 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C8 H22 Cl2 Cu1 N4 O8' _chemical_formula_moiety ? _chemical_formula_weight 436.74 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 9.5674(19) _cell_length_b 13.745(3) _cell_length_c 12.562(3) _cell_angle_alpha 90.00000 _cell_angle_beta 91.26(3) _cell_angle_gamma 90.00000 _cell_volume 1651.6(6) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71069 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.5 _cell_measurement_theta_max 10.5 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 1.691 _exptl_crystal_description plate _exptl_crystal_size_max .3 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .2 _exptl_crystal_size_rad ? _exptl_crystal_colour blue _diffrn_measurement_device_type 'STOE STADI4 4-circle-diffractometer' _diffrn_measurement_method '2\q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type Numerical _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min .59 _exptl_absorpt_correction_T_max .8144 _diffrn_reflns_number 3821 _reflns_number_total 3780 _reflns_Friedel_coverage ? _reflns_number_gt 2774 _reflns_threshold_expression 'I > 2.00 sig(I )' _diffrn_reflns_theta_max 27.52 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .075 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 6.8 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt .0584 _refine_ls_wR_factor_ref .1411 _refine_ls_goodness_of_fit_ref 1.184 _refine_ls_number_reflns 3780 _refine_ls_number_parameters 236 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ' calc w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+4.2473P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .005 _refine_diff_density_min -.445 _refine_diff_density_max .536 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'STADI4 (STOE, 1996)' _computing_cell_refinement 'STADI4 (STOE, 1996)' _computing_data_reduction 'X-RED (STOE, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'xtal ORTEP PLOTX' _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ 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 Cu ? 0 4 .320129 1.2651 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 16 .006104 .003296 'Int Tables Vol IV Tables 2.2B and 2.3.1' C ? 0 32 .003296 .001587 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 8 .148376 .158508 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 32 .01062 .005981 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 88 0 0 '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_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu .24118(6) .38979(4) .73361(5) .0416(3) Uani ? ? 1.00000 ? ? C1 .2873(9) .3051(6) .4857(5) .088(6) Uani ? ? 1.00000 ? ? H1 .29740 .31130 .40860 .10600 Uiso ? ? 1.00000 ? ? C11 .3006(10) .1975(5) .5104(6) .103(6) Uani ? ? 1.00000 ? ? H11a .22440 .16290 .47680 .12400 Uiso ? ? 1.00000 ? ? H11b .29840 .18780 .58600 .12400 Uiso ? ? 1.00000 ? ? H11c .38750 .17350 .48390 .12400 Uiso ? ? 1.00000 ? ? C2 .1433(7) .3471(5) .5106(5) .072(4) Uani ? ? 1.00000 ? ? H2a .14190 .41560 .49220 .08700 Uiso ? ? 1.00000 ? ? H2b .07310 .31460 .46650 .08700 Uiso ? ? 1.00000 ? ? N3 .1062(4) .3363(3) .6236(4) .050(2) Uani ? ? 1.00000 ? ? H3 .10000 .27130 .63620 .06000 Uiso ? ? 1.00000 ? ? C4 -.0314(6) .3777(4) .6474(6) .067(4) Uani ? ? 1.00000 ? ? H4a -.10460 .34180 .61000 .08000 Uiso ? ? 1.00000 ? ? H4b -.03590 .44510 .62480 .08000 Uiso ? ? 1.00000 ? ? C5 -.0503(6) .3708(5) .7641(6) .075(4) Uani ? ? 1.00000 ? ? H5a -.13730 .40150 .78380 .09000 Uiso ? ? 1.00000 ? ? H5b -.05250 .30320 .78620 .09000 Uiso ? ? 1.00000 ? ? N6 .0697(5) .4214(4) .8155(4) .071(3) Uani ? ? 1.00000 ? ? H6a .08050 .40160 .88350 .08600 Uiso ? ? 1.00000 ? ? H6b .05500 .48610 .81530 .08600 Uiso ? ? 1.00000 ? ? N3' .4117(4) .3549(3) .6516(4) .054(2) Uani ? ? 1.00000 ? ? H3' .43130 .29150 .66670 .06500 Uiso ? ? 1.00000 ? ? C2' .4016(8) .3630(5) .5348(6) .086(5) Uani ? ? 1.00000 ? ? H2'a .48950 .34220 .50520 .10300 Uiso ? ? 1.00000 ? ? H2'b .38790 .43080 .51600 .10300 Uiso ? ? 1.00000 ? ? C4' .5267(6) .4132(5) .6988(7) .083(5) Uani ? ? 1.00000 ? ? H4'a .51810 .48060 .67660 .10000 Uiso ? ? 1.00000 ? ? H4'b .61620 .38860 .67600 .10000 Uiso ? ? 1.00000 ? ? C5' .5163(7) .4054(5) .8162(8) .096(6) Uani ? ? 1.00000 ? ? H5'a .53070 .33860 .83860 .11500 Uiso ? ? 1.00000 ? ? H5'b .58720 .44560 .85090 .11500 Uiso ? ? 1.00000 ? ? N6' .3773(6) .4382(4) .8456(4) .069(3) Uani ? ? 1.00000 ? ? H6'a .37480 .50360 .84890 .08400 Uiso ? ? 1.00000 ? ? H6'b .35540 .41420 .90980 .08400 Uiso ? ? 1.00000 ? ? Cl1 .25865(14) .14400(8) .83373(11) .0506(7) Uani ? ? 1.00000 ? ? O11 .1439(6) .1447(4) .7617(5) .115(4) Uani ? ? 1.00000 ? ? O12 .3904(7) .1490(5) .7765(6) .085(5) Uani ? ? .721(14) ? ? O13 .2463(13) .2274(7) .8929(10) .134(9) Uani ? ? .721(14) ? ? O14 .2566(8) .0568(5) .8876(7) .079(5) Uani ? ? .721(14) ? ? O12' .324(3) .2259(13) .834(2) .11(2) Uani ? ? .279(14) ? ? O13' .235(3) .119(2) .9496(14) .115(17) Uani ? ? .279(14) ? ? O14' .321(3) .0622(16) .808(3) .13(2) Uani ? ? .279(14) ? ? Cl2 .76661(17) .62722(10) .86621(13) .0621(9) Uani ? ? 1.00000 ? ? O21 .7669(7) .5752(4) .7682(4) .108(4) Uani ? ? 1.00000 ? ? O22 .6292(6) .6375(4) .9051(5) .106(4) Uani ? ? 1.00000 ? ? O23 .8240(7) .7194(4) .8501(6) .132(5) Uani ? ? 1.00000 ? ? O24 .8430(8) .5736(5) .9405(5) .138(6) Uani ? ? 1.00000 ? ? 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 Cu .0349(3) .0356(3) .0540(4) .0001(2) -.0036(2) .0015(3) C1 .122(7) .097(6) .045(4) .054(5) .000(4) .002(4) C11 .138(7) .083(5) .087(5) .041(5) -.031(5) -.039(4) C2 .091(5) .071(4) .053(4) .019(4) -.023(3) .004(3) N3 .047(2) .036(2) .066(3) .0003(18) -.014(2) .0024(19) C4 .037(3) .060(4) .102(5) -.001(3) -.011(3) .004(3) C5 .040(3) .073(4) .111(6) .004(3) .010(3) .010(4) N6 .068(3) .074(3) .073(3) .019(3) .013(3) -.008(3) N3' .039(2) .038(2) .085(3) .0067(18) .004(2) .006(2) C2' .094(5) .083(5) .082(5) .027(4) .043(4) .025(4) C4' .032(3) .056(4) .161(8) -.004(3) .004(4) .001(4) C5' .063(4) .050(4) .172(9) -.016(3) -.067(5) .015(5) N6' .083(4) .051(3) .073(3) -.015(3) -.027(3) .006(2) Cl1 .0544(7) .0291(5) .0680(9) -.0005(5) -.0044(6) .0003(5) O11 .103(4) .074(3) .164(6) -.009(3) -.069(4) .028(3) O12 .064(4) .070(6) .122(6) .002(3) .025(4) .017(4) O13 .161(10) .061(6) .181(11) -.011(6) .052(8) -.060(6) O14 .087(5) .054(4) .095(7) -.011(4) .001(4) .028(4) O12' .15(3) .034(11) .15(2) -.048(14) -.042(19) .026(13) O13' .18(2) .12(2) .045(11) -.048(17) .015(12) .008(12) O14' .108(19) .067(16) .23(3) .017(13) .02(2) -.050(19) Cl2 .0727(10) .0417(7) .0713(9) -.0083(6) -.0109(7) -.0025(6) O21 .148(5) .107(4) .070(3) -.028(4) .000(3) -.019(3) O22 .082(4) .102(4) .134(5) -.015(3) .007(3) -.010(3) O23 .134(5) .055(3) .209(7) -.032(3) .048(5) -.014(4) O24 .178(7) .146(6) .089(4) .057(5) -.032(4) .006(4) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Cu N3 . . 2.010(4) ? Cu N6 . . 2.003(5) ? Cu N3' . . 2.007(4) ? Cu N6' . . 2.009(5) ? Cu O13 . . 2.997(11) ? Cu O12' . . 2.69(2) ? Cu O14 . '2 556' 2.755(8) ? Cu O14' . '2 556' 2.50(2) ? C1 H1 . . .979(6) ? C1 C11 . . 1.516(11) ? C1 C2 . . 1.532(11) ? C1 C2' . . 1.476(11) ? C11 H11a . . .960(9) ? C11 H11b . . .960(8) ? C11 H11c . . .961(9) ? C2 H2a . . .970(7) ? C2 H2b . . .970(7) ? C2 N3 . . 1.478(8) ? N3 H3 . . .910(4) ? N3 C4 . . 1.471(7) ? C4 H4a . . .970(6) ? C4 H4b . . .970(6) ? C4 C5 . . 1.484(11) ? C5 H5a . . .970(6) ? C5 H5b . . .970(7) ? C5 N6 . . 1.479(8) ? N6 H6a . . .900(5) ? N6 H6b . . .900(5) ? N3' H3' . . .910(4) ? N3' C2' . . 1.473(9) ? N3' C4' . . 1.475(8) ? C2' H2'a . . .970(8) ? C2' H2'b . . .970(7) ? C4' H4'a . . .970(7) ? C4' H4'b . . .970(6) ? C4' C5' . . 1.484(13) ? C5' H5'a . . .969(7) ? C5' H5'b . . .971(7) ? C5' N6' . . 1.459(9) ? N6' H6'a . . .900(6) ? N6' H6'b . . .900(5) ? Cl1 O11 . . 1.407(6) ? Cl1 O12 . . 1.466(7) ? Cl1 O13 . . 1.373(11) ? Cl1 O14 . . 1.377(7) ? Cl1 O12' . . 1.29(2) ? Cl1 O13' . . 1.517(19) ? Cl1 O14' . . 1.32(2) ? O11 O12 . . 2.362(9) ? O11 O13 . . 2.213(13) ? O11 O14 . . 2.247(10) ? O11 O12' . . 2.23(3) ? O11 O14' . . 2.11(3) ? O12 O13 . . 2.300(14) ? O12 O14 . . 2.296(11) ? O12 O12' . . 1.44(2) ? O12 O14' . . 1.43(3) ? O13 O14 . . 2.348(12) ? O13 O12' . . 1.06(3) ? O13 O13' . . 1.66(3) ? O14 O13' . . 1.18(3) ? O14 O14' . . 1.19(4) ? O12' O13' . . 2.25(3) ? O12' O14' . . 2.27(3) ? O13' O14' . . 2.12(4) ? Cl2 O21 . . 1.424(5) ? Cl2 O22 . . 1.420(6) ? Cl2 O23 . . 1.397(6) ? Cl2 O24 . . 1.385(7) ? O21 O22 . . 2.351(8) ? O21 O23 . . 2.294(8) ? O21 O24 . . 2.268(8) ? O22 O23 . . 2.297(9) ? O22 O24 . . 2.261(9) ? O23 O24 . . 2.309(9) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published N3 Cu N6 . . . 84.9(2) ? N3 Cu N3' . . . 94.41(18) ? N3 Cu N6' . . . 177.9(2) ? N3 Cu O13 . . . 100.8(3) ? N3 Cu O12' . . . 101.2(5) ? N3 Cu O14 . . '2 556' 86.4(2) ? N3 Cu O14' . . '2 556' 93.3(8) ? N6 Cu N3' . . . 178.7(2) ? N6 Cu N6' . . . 95.4(2) ? N6 Cu O13 . . . 79.6(3) ? N6 Cu O12' . . . 100.2(6) ? N6 Cu O14 . . '2 556' 96.9(2) ? N6 Cu O14' . . '2 556' 73.0(8) ? N3' Cu N6' . . . 85.2(2) ? N3' Cu O13 . . . 99.4(3) ? N3' Cu O12' . . . 78.8(6) ? N3' Cu O14 . . '2 556' 84.2(2) ? N3' Cu O14' . . '2 556' 108.2(8) ? N6' Cu O13 . . . 77.2(3) ? N6' Cu O12' . . . 76.7(5) ? N6' Cu O14 . . '2 556' 95.6(2) ? N6' Cu O14' . . '2 556' 88.9(8) ? O13 Cu O12' . . . 20.6(6) ? O13 Cu O14 . . '2 556' 171.6(3) ? O13 Cu O14' . . '2 556' 147.9(9) ? O12' Cu O14 . . '2 556' 161.9(6) ? O12' Cu O14' . . '2 556' 163.5(10) ? O14 Cu O14' '2 556' . '2 556' 25.6(8) ? H1 C1 C11 . . . 106.1(7) ? H1 C1 C2 . . . 106.1(7) ? H1 C1 C2' . . . 106.1(7) ? C11 C1 C2 . . . 113.4(7) ? C11 C1 C2' . . . 112.5(7) ? C2 C1 C2' . . . 111.9(6) ? C1 C11 H11a . . . 109.5(7) ? C1 C11 H11b . . . 109.5(6) ? C1 C11 H11c . . . 109.5(7) ? H11a C11 H11b . . . 109.5(8) ? H11a C11 H11c . . . 109.4(7) ? H11b C11 H11c . . . 109.5(8) ? C1 C2 H2a . . . 109.0(6) ? C1 C2 H2b . . . 108.9(6) ? C1 C2 N3 . . . 113.2(5) ? H2a C2 H2b . . . 107.8(6) ? H2a C2 N3 . . . 108.9(6) ? H2b C2 N3 . . . 108.9(6) ? Cu N3 C2 . . . 117.3(3) ? Cu N3 H3 . . . 106.4(3) ? Cu N3 C4 . . . 106.4(4) ? C2 N3 H3 . . . 106.5(5) ? C2 N3 C4 . . . 113.0(5) ? H3 N3 C4 . . . 106.4(4) ? N3 C4 H4a . . . 110.2(5) ? N3 C4 H4b . . . 110.1(5) ? N3 C4 C5 . . . 107.8(5) ? H4a C4 H4b . . . 108.5(6) ? H4a C4 C5 . . . 110.1(6) ? H4b C4 C5 . . . 110.2(6) ? C4 C5 H5a . . . 110.4(6) ? C4 C5 H5b . . . 110.4(6) ? C4 C5 N6 . . . 106.9(5) ? H5a C5 H5b . . . 108.6(6) ? H5a C5 N6 . . . 110.3(6) ? H5b C5 N6 . . . 110.3(6) ? Cu N6 C5 . . . 108.1(4) ? Cu N6 H6a . . . 110.1(4) ? Cu N6 H6b . . . 110.0(4) ? C5 N6 H6a . . . 110.1(5) ? C5 N6 H6b . . . 110.1(5) ? H6a N6 H6b . . . 108.4(5) ? Cu N3' H3' . . . 106.7(3) ? Cu N3' C2' . . . 117.2(4) ? Cu N3' C4' . . . 105.8(4) ? H3' N3' C2' . . . 106.8(5) ? H3' N3' C4' . . . 106.7(4) ? C2' N3' C4' . . . 113.0(5) ? C1 C2' N3' . . . 114.0(6) ? C1 C2' H2'a . . . 108.7(7) ? C1 C2' H2'b . . . 108.7(7) ? N3' C2' H2'a . . . 108.7(6) ? N3' C2' H2'b . . . 108.7(6) ? H2'a C2' H2'b . . . 107.7(7) ? N3' C4' H4'a . . . 110.2(6) ? N3' C4' H4'b . . . 110.3(6) ? N3' C4' C5' . . . 107.1(5) ? H4'a C4' H4'b . . . 108.5(7) ? H4'a C4' C5' . . . 110.3(7) ? H4'b C4' C5' . . . 110.3(7) ? C4' C5' H5'a . . . 110.2(8) ? C4' C5' H5'b . . . 110.1(7) ? C4' C5' N6' . . . 108.1(6) ? H5'a C5' H5'b . . . 108.4(8) ? H5'a C5' N6' . . . 110.1(7) ? H5'b C5' N6' . . . 110.0(7) ? Cu N6' C5' . . . 107.5(5) ? Cu N6' H6'a . . . 110.2(4) ? Cu N6' H6'b . . . 110.2(4) ? C5' N6' H6'a . . . 110.2(6) ? C5' N6' H6'b . . . 110.2(6) ? H6'a N6' H6'b . . . 108.5(5) ? O11 Cl1 O12 . . . 110.6(4) ? O11 Cl1 O13 . . . 105.5(6) ? O11 Cl1 O14 . . . 107.6(4) ? O11 Cl1 O12' . . . 111.6(12) ? O11 Cl1 O13' . . . 119.2(11) ? O11 Cl1 O14' . . . 101.5(15) ? O12 Cl1 O13 . . . 108.1(6) ? O12 Cl1 O14 . . . 107.7(4) ? O12 Cl1 O12' . . . 62.5(12) ? O12 Cl1 O13' . . . 129.0(11) ? O12 Cl1 O14' . . . 61.4(13) ? O13 Cl1 O14 . . . 117.3(6) ? O13 Cl1 O12' . . . 46.9(13) ? O13 Cl1 O13' . . . 69.7(11) ? O13 Cl1 O14' . . . 153.0(15) ? O14 Cl1 O12' . . . 140.5(12) ? O14 Cl1 O13' . . . 47.7(11) ? O14 Cl1 O14' . . . 52.3(15) ? O12' Cl1 O13' . . . 106.1(15) ? O12' Cl1 O14' . . . 121.6(17) ? O13' Cl1 O14' . . . 96.9(19) ? Cl1 O11 O12 . . . 35.5(2) ? Cl1 O11 O13 . . . 36.7(3) ? Cl1 O11 O14 . . . 35.7(2) ? Cl1 O11 O12' . . . 32.5(6) ? Cl1 O11 O14' . . . 37.7(8) ? O12 O11 O13 . . . 60.2(4) ? O12 O11 O14 . . . 59.7(3) ? O12 O11 O12' . . . 36.3(7) ? O12 O11 O14' . . . 36.6(7) ? O13 O11 O14 . . . 63.5(4) ? O13 O11 O12' . . . 27.6(8) ? O13 O11 O14' . . . 74.4(9) ? O14 O11 O12' . . . 68.2(6) ? O14 O11 O14' . . . 31.5(10) ? O12' O11 O14' . . . 63.1(9) ? Cl1 O12 O11 . . . 33.9(2) ? Cl1 O12 O13 . . . 34.6(3) ? Cl1 O12 O14 . . . 34.8(3) ? Cl1 O12 O12' . . . 52.7(10) ? Cl1 O12 O14' . . . 54.1(12) ? O11 O12 O13 . . . 56.7(4) ? O11 O12 O14 . . . 57.7(3) ? O11 O12 O12' . . . 66.8(11) ? O11 O12 O14' . . . 62.0(12) ? O13 O12 O14 . . . 61.4(4) ? O13 O12 O12' . . . 19.5(10) ? O13 O12 O14' . . . 85.8(13) ? O14 O12 O12' . . . 80.9(10) ? O14 O12 O14' . . . 25.8(14) ? O12' O12 O14' . . . 105.2(16) ? Cu O13 Cl1 . . . 105.1(6) ? Cu O13 O11 . . . 83.4(4) ? Cu O13 O12 . . . 85.7(4) ? Cu O13 O14 . . . 136.5(5) ? Cu O13 O12' . . . 63.3(12) ? Cu O13 O13' . . . 163.1(9) ? Cl1 O13 O11 . . . 37.8(4) ? Cl1 O13 O12 . . . 37.3(4) ? Cl1 O13 O14 . . . 31.4(3) ? Cl1 O13 O12' . . . 62.4(12) ? Cl1 O13 O13' . . . 59.3(8) ? O11 O13 O12 . . . 63.1(4) ? O11 O13 O14 . . . 58.9(4) ? O11 O13 O12' . . . 77.1(15) ? O11 O13 O13' . . . 80.0(9) ? O12 O13 O14 . . . 59.2(4) ? O12 O13 O12' . . . 26.9(10) ? O12 O13 O13' . . . 84.1(10) ? O14 O13 O12' . . . 86.0(11) ? O14 O13 O13' . . . 28.0(8) ? O12' O13 O13' . . . 109.6(15) ? Cl1 O14 O11 . . . 36.7(3) ? Cl1 O14 O12 . . . 37.5(3) ? Cl1 O14 O13 . . . 31.3(4) ? Cl1 O14 O13' . . . 72.4(12) ? Cl1 O14 O14' . . . 61.2(12) ? Cl1 O14 Cu . . '2 546' 117.0(5) ? O11 O14 O12 . . . 62.7(3) ? O11 O14 O13 . . . 57.5(4) ? O11 O14 O13' . . . 89.2(12) ? O11 O14 O14' . . . 67.9(14) ? O11 O14 Cu . . '2 546' 93.9(3) ? O12 O14 O13 . . . 59.4(4) ? O12 O14 O13' . . . 96.3(13) ? O12 O14 O14' . . . 31.5(12) ? O12 O14 Cu . . '2 546' 96.5(3) ? O13 O14 O13' . . . 41.3(12) ? O13 O14 O14' . . . 89.1(12) ? O13 O14 Cu . . '2 546' 148.1(5) ? O13' O14 O14' . . . 127.8(18) ? O13' O14 Cu . . '2 546' 166.9(14) ? O14' O14 Cu . . '2 546' 64.9(12) ? Cu O12' Cl1 . . . 126.3(16) ? Cu O12' O11 . . . 90.6(9) ? Cu O12' O12 . . . 120.6(14) ? Cu O12' O13 . . . 96.1(15) ? Cu O12' O13' . . . 137.6(14) ? Cu O12' O14' . . . 139.3(14) ? Cl1 O12' O11 . . . 35.9(8) ? Cl1 O12' O12 . . . 64.9(9) ? Cl1 O12' O13 . . . 70.8(15) ? Cl1 O12' O13' . . . 40.4(9) ? Cl1 O12' O14' . . . 29.5(9) ? O11 O12' O12 . . . 76.9(10) ? O11 O12' O13 . . . 75.3(16) ? O11 O12' O13' . . . 68.6(9) ? O11 O12' O14' . . . 55.9(9) ? O12 O12' O13 . . . 133.6(18) ? O12 O12' O13' . . . 91.3(11) ? O12 O12' O14' . . . 37.2(10) ? O13 O12' O13' . . . 44.0(12) ? O13 O12' O14' . . . 96.5(16) ? O13' O12' O14' . . . 56.1(12) ? Cl1 O13' O13 . . . 51.0(8) ? Cl1 O13' O14 . . . 59.9(9) ? Cl1 O13' O12' . . . 33.4(8) ? Cl1 O13' O14' . . . 38.0(9) ? O13 O13' O14 . . . 110.8(14) ? O13 O13' O12' . . . 26.4(8) ? O13 O13' O14' . . . 86.6(12) ? O14 O13' O12' . . . 88.4(13) ? O14 O13' O14' . . . 26.2(10) ? O12' O13' O14' . . . 62.6(10) ? Cl1 O14' O11 . . . 40.8(9) ? Cl1 O14' O12 . . . 64.5(10) ? Cl1 O14' O14 . . . 66.5(16) ? Cl1 O14' O12' . . . 28.8(9) ? Cl1 O14' O13' . . . 45.1(13) ? Cl1 O14' Cu . . '2 546' 139.0(18) ? O11 O14' O12 . . . 81.4(12) ? O11 O14' O14 . . . 80.6(15) ? O11 O14' O12' . . . 61.0(10) ? O11 O14' O13' . . . 73.1(12) ? O11 O14' Cu . . '2 546' 105.4(12) ? O12 O14' O14 . . . 123(2) ? O12 O14' O12' . . . 37.6(10) ? O12 O14' O13' . . . 96.7(16) ? O12 O14' Cu . . '2 546' 148(2) ? O14 O14' O12' . . . 86.9(16) ? O14 O14' O13' . . . 26.0(11) ? O14 O14' Cu . . '2 546' 89.5(13) ? O12' O14' O13' . . . 61.3(12) ? O12' O14' Cu . . '2 546' 166.4(16) ? O13' O14' Cu . . '2 546' 115.4(15) ? O21 Cl2 O22 . . . 111.5(4) ? O21 Cl2 O23 . . . 108.8(4) ? O21 Cl2 O24 . . . 107.7(4) ? O22 Cl2 O23 . . . 109.2(4) ? O22 Cl2 O24 . . . 107.5(4) ? O23 Cl2 O24 . . . 112.1(4) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- 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 Cu C1 3.363(7) . . ? Cu H11b 3.3898(8) . . ? Cu C2 2.992(6) . . ? Cu H2a 3.1777(9) . . ? Cu H3 2.4293(7) . . ? Cu C4 2.807(6) . . ? Cu H4b 3.0519(7) . . ? Cu C5 2.835(6) . . ? Cu H5b 3.1352(8) . . ? Cu H6a 2.4622(7) . . ? Cu H6b 2.4614(7) . . ? Cu H3' 2.4305(7) . . ? Cu C2' 2.983(8) . . ? Cu H2'b 3.1511(9) . . ? Cu C4' 2.795(6) . . ? Cu H4'a 3.0288(7) . . ? Cu C5' 2.816(7) . . ? Cu H5'a 3.1219(8) . . ? Cu H6'a 2.4693(7) . . ? Cu H6'b 2.4696(8) . . ? Cu Cl1 3.5951(15) . '2 556' ? Cu Cl1 3.6075(14) . . ? Cu O11 3.672(6) . '2 556' ? Cu O11 3.515(6) . . ? Cu O12 3.780(7) . '2 556' ? Cu O12 3.640(7) . . ? C1 H11a 2.047(8) . . ? C1 H11b 2.048(8) . . ? C1 H11c 2.048(8) . . ? C1 H2a 2.062(8) . . ? C1 H2b 2.062(9) . . ? C1 N3 2.514(9) . . ? C1 H3 2.674(8) . . ? C1 N3' 2.474(8) . . ? C1 H3' 2.639(7) . . ? C1 H2'a 2.010(9) . . ? C1 H2'b 2.010(8) . . ? H1 C11 2.020(7) . . ? H1 H11a 2.3257(4) . . ? H1 H11c 2.2780(4) . . ? H1 C2 2.035(7) . . ? H1 H2a 2.3324(3) . . ? H1 H2b 2.2814(4) . . ? H1 N3 3.313(5) . . ? H1 N3' 3.275(5) . . ? H1 C2' 1.986(7) . . ? H1 H2'a 2.2210(3) . . ? H1 H2'b 2.2840(3) . . ? C11 C2 2.548(10) . . ? C11 N3 3.039(9) . . ? C11 N3' 2.979(9) . . ? C11 H3' 2.642(8) . . ? C11 C2' 2.488(10) . . ? C11 H2'a 2.689(8) . . ? H11a H11b 1.5676(3) . . ? H11a H11c 1.5678(3) . . ? H11a C2 2.685(7) . . ? H11a N3 3.233(4) . . ? H11b H11c 1.5679(3) . . ? H11b N3 2.794(4) . . ? H11b H3 2.3175(3) . . ? H11b N3' 2.663(4) . . ? H11b H3' 2.1493(3) . . ? H11b C2' 2.686(7) . . ? H11b O12 2.587(7) . . ? H11c N6 3.062(5) . '4 554' ? H11c N3' 3.269(5) . . ? H11c C2' 2.685(7) . . ? C2 H3 1.943(7) . . ? C2 C4 2.460(9) . . ? C2 H4b 2.631(7) . . ? C2 N3' 3.089(8) . . ? C2 C2' 2.493(10) . . ? C2 H2'b 2.607(7) . . ? H2a H2b 1.5670(3) . . ? H2a N3 2.013(5) . . ? H2a C4 2.639(7) . . ? H2a N3' 3.338(4) . . ? H2a C2' 2.631(8) . . ? H2a H2'b 2.3752(5) . . ? H2a O14 2.632(8) . '2 556' ? H2b N3 2.014(5) . . ? H2b H3 2.2228(5) . . ? H2b C4 2.649(7) . . ? N3 H4a 2.022(4) . . ? N3 H4b 2.021(4) . . ? N3 C5 2.387(8) . . ? N3 H5a 3.238(4) . . ? N3 H5b 2.612(5) . . ? N3 N6 2.709(7) . . ? N3 H6b 3.214(5) . . ? N3 N3' 2.947(5) . . ? N3 H3' 3.205(4) . . ? N3 C2' 3.083(9) . . ? N3 H2'b 3.307(4) . . ? N3 N6' 4.018(7) . . ? N3 O11 3.170(7) . . ? N3 O14 3.307(8) . '2 556' ? N3 O12' 3.66(3) . . ? N3 O14' 3.29(2) . '2 556' ? N3 O22 3.554(7) . '2 546' ? H3 C4 1.936(6) . . ? H3 H4a 2.2024(4) . . ? H3 C5 2.573(7) . . ? H3 N6 3.073(5) . . ? H3 N3' 3.198(4) . . ? H3 O11 2.379(6) . . ? C4 H5a 2.036(7) . . ? C4 H5b 2.036(7) . . ? C4 N6 2.380(9) . . ? C4 H6b 2.697(7) . . ? H4a H4b 1.5739(3) . . ? H4a C5 2.033(7) . . ? H4a H5a 2.3597(5) . . ? H4a H5b 2.3196(5) . . ? H4a N6 3.233(5) . . ? H4a O13' 2.56(2) . '4 454' ? H4b C5 2.033(7) . . ? H4b H5a 2.3184(4) . . ? H4b N6 2.600(5) . . ? C5 H6a 1.978(7) . . ? C5 H6b 1.978(7) . . ? H5a H5b 1.5760(3) . . ? H5a N6 2.030(5) . . ? H5a H6b 2.2049(3) . . ? H5a O21 2.563(6) . '1 455' ? H5b N6 2.031(5) . . ? H5b H6a 2.2077(3) . . ? N6 N3' 4.010(7) . . ? N6 N6' 2.968(7) . . ? N6 H6'a 3.150(5) . . ? N6 H6'b 2.957(5) . . ? N6 O12 3.360(9) . '2 556' ? N6 O13 3.292(12) . . ? N6 O14 3.595(10) . '2 556' ? N6 O12' 3.63(2) . . ? N6 O14' 2.71(3) . '2 556' ? N6 O21 3.625(8) . '1 455' ? N6 O24 3.420(9) . '1 455' ? N6 O24 3.160(8) . '3 667' ? H6a H6b 1.4606(2) . . ? H6a N6' 2.933(6) . . ? H6a O24 2.339(6) . '3 667' ? H6b N6' 3.168(6) . . ? H6b O12 2.577(7) . '2 556' ? H6b O14' 2.23(3) . '2 556' ? N3' H2'a 2.007(5) . . ? N3' H2'b 2.006(5) . . ? N3' H4'a 2.026(4) . . ? N3' H4'b 2.027(4) . . ? N3' C5' 2.381(10) . . ? N3' H5'a 2.598(5) . . ? N3' H5'b 3.234(5) . . ? N3' N6' 2.719(7) . . ? N3' H6'a 3.238(5) . . ? N3' O12 3.244(8) . . ? N3' O14 3.241(8) . '2 556' ? N3' O12' 3.03(2) . . ? N3' O14' 3.66(3) . '2 556' ? N3' O23 3.141(7) . '2 646' ? H3' C2' 1.942(7) . . ? H3' H2'a 2.2274(4) . . ? H3' C4' 1.944(7) . . ? H3' H4'b 2.2170(3) . . ? H3' C5' 2.564(9) . . ? H3' N6' 3.072(5) . . ? H3' O12 2.432(7) . . ? H3' O12' 2.53(3) . . ? H3' O23 2.555(7) . '2 646' ? C2' C4' 2.459(11) . . ? C2' H4'a 2.635(7) . . ? H2'a H2'b 1.5659(2) . . ? H2'a C4' 2.637(9) . . ? H2'a O13' 2.52(3) . '4 554' ? H2'b C4' 2.638(8) . . ? H2'b O14 2.540(8) . '2 556' ? C4' H5'a 2.033(8) . . ? C4' H5'b 2.034(8) . . ? C4' N6' 2.383(10) . . ? H4'a H4'b 1.5749(2) . . ? H4'a C5' 2.036(9) . . ? H4'a H5'b 2.3236(5) . . ? H4'a N6' 2.605(5) . . ? H4'b C5' 2.035(9) . . ? H4'b H5'a 2.3210(4) . . ? H4'b H5'b 2.3547(5) . . ? H4'b N6' 3.231(5) . . ? H4'b O23 2.419(6) . '2 646' ? C5' H6'a 1.962(7) . . ? C5' H6'b 1.961(8) . . ? H5'a H5'b 1.5733(3) . . ? H5'a N6' 2.010(6) . . ? H5'a H6'b 2.1814(3) . . ? H5'a O12' 2.51(3) . . ? H5'b N6' 2.010(6) . . ? H5'b H6'a 2.1825(4) . . ? H5'b H6'b 2.3925(4) . . ? H5'b O21 2.699(6) . . ? N6' O11 3.147(8) . '2 556' ? N6' O13 3.217(12) . . ? N6' O14 3.566(10) . '2 556' ? N6' O12' 2.97(2) . . ? N6' O14' 3.17(3) . '2 556' ? N6' O22 3.302(8) . '3 667' ? N6' O24 3.455(9) . '3 667' ? H6'a H6'b 1.4615(2) . . ? H6'a O11 2.390(6) . '2 556' ? H6'b O22 2.433(6) . '3 667' ? O11 O13' 2.52(2) . . ? O12 O13' 2.69(2) . . ? O13 O14' 2.61(3) . . ? O14 O12' 2.51(2) . . ? _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 900 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _reflns_number_observed ? _reflns_d_resolution_high ? _reflns_d_resolution_low ? _diffrn_reflns_av_sigmaI/netI .033 _diffrn_reflns_theta_min 2.2 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'planar graphite' _diffrn_radiation_detector 'scintillation counter' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .0907 _refine_ls_wR_factor_all .1219 _refine_ls_goodness_of_fit_all 1.184 _refine_ls_shift/su_mean .0001 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_global _audit_creation_method Xtal3.6 _audit_creation_date 00-09-14 _audit_update_record ? #============================================================================== # (Publishing Staff Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia Nedlands Western Australia 6907 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal ? _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Skelton, Brian W.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Pogram for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_17yk # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C8 H22 Cl2 Cu1 N4 O8' _chemical_formula_moiety ? _chemical_formula_weight 436.74 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21_1 _symmetry_space_group_name_Hall p_2yb loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,-z _cell_length_a 8.3680(10) _cell_length_b 24.884(4) _cell_length_c 8.5080(10) _cell_angle_alpha 90.00000 _cell_angle_beta 114.917(3) _cell_angle_gamma 90.00000 _cell_volume 1606.7(4) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.805 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 1927 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 24.4 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu 1.738 _exptl_crystal_description prism _exptl_crystal_size_max .12 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .06 _exptl_crystal_size_rad ? _exptl_crystal_colour dark_blue _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .738 _exptl_absorpt_correction_T_max .894 _diffrn_reflns_number 16230 _reflns_number_total 4227 _reflns_Friedel_coverage 0 _reflns_number_gt 3150 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.32 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .047 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .042 _refine_ls_wR_factor_ref .041 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_number_reflns 3150 _refine_ls_number_parameters 414 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .011 _refine_diff_density_min -.542 _refine_diff_density_max .574 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ 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 32 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 88 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 8 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cu ? 0 4 .263 1.266 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 16 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 32 .008 .006 '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_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 .52065(10) .00000 .92683(9) .0164(3) Uani ? ? 1.00000 ? ? Cl1 .7861(2) -.03813(8) .7110(2) .0229(8) Uani ? ? 1.00000 ? ? O11 .6954(6) .0066(2) .7453(6) .029(2) Uani ? ? 1.00000 ? ? O12 .6609(7) -.0803(2) .6268(7) .044(3) Uani ? ? 1.00000 ? ? O13 .9156(7) -.0586(2) .8720(7) .041(3) Uani ? ? 1.00000 ? ? O14 .8709(7) -.0199(2) .6060(7) .044(3) Uani ? ? 1.00000 ? ? Cl1' .2420(2) .03224(7) 1.1240(2) .0228(8) Uani ? ? 1.00000 ? ? O11' .3441(6) -.01193(18) 1.1016(6) .028(2) Uani ? ? 1.00000 ? ? O12' .1285(7) .0537(2) .9561(6) .033(3) Uani ? ? 1.00000 ? ? O13' .3622(7) .0733(2) 1.2255(7) .044(3) Uani ? ? 1.00000 ? ? O14' .1394(6) .0129(2) 1.2112(6) .031(2) Uani ? ? 1.00000 ? ? C11 .3469(9) .1160(3) .7057(9) .021(3) Uani ? ? 1.00000 ? ? C111 .3149(9) .1618(3) .5793(9) .026(3) Uani ? ? 1.00000 ? ? C12 .5387(9) .1163(3) .8382(8) .019(3) Uani ? ? 1.00000 ? ? N13 .5740(7) .0795(2) .9874(7) .018(2) Uani ? ? 1.00000 ? ? C14 .7590(9) .0823(3) 1.1172(8) .022(3) Uani ? ? 1.00000 ? ? C15 .7873(8) .0382(3) 1.2453(8) .020(3) Uani ? ? 1.00000 ? ? N16 .7381(7) -.0129(2) 1.1476(7) .024(3) Uani ? ? 1.00000 ? ? C12' .2978(8) .0634(3) .6075(8) .019(3) Uani ? ? 1.00000 ? ? N13' .2975(7) .0164(2) .7132(6) .019(2) Uani ? ? 1.00000 ? ? C14' .2490(8) -.0332(3) .6097(8) .020(3) Uani ? ? 1.00000 ? ? C15' .2805(9) -.0802(3) .7330(8) .020(3) Uani ? ? 1.00000 ? ? N16' .4673(7) -.0765(2) .8642(7) .021(2) Uani ? ? 1.00000 ? ? Cu2 .94595(10) .29789(4) .93339(10) .0166(3) Uani ? ? 1.00000 ? ? Cl2 .6765(2) .25163(7) 1.1355(2) .0218(8) Uani ? ? 1.00000 ? ? O21 .7180(6) .2449(2) .9882(6) .028(2) Uani ? ? 1.00000 ? ? O22 .8343(7) .2455(3) 1.2898(7) .061(4) Uani ? ? 1.00000 ? ? O23 .6077(7) .3048(2) 1.1307(7) .044(3) Uani ? ? 1.00000 ? ? O24 .5498(7) .2126(2) 1.1313(7) .038(3) Uani ? ? 1.00000 ? ? Cl2' 1.2256(2) .34085(7) .7395(2) .0208(7) Uani ? ? 1.00000 ? ? O21' 1.1790(6) .3522(2) .8823(6) .030(2) Uani ? ? 1.00000 ? ? O22' 1.2694(7) .2854(2) .7424(8) .043(3) Uani ? ? 1.00000 ? ? O23' 1.0770(6) .3540(2) .5799(6) .041(3) Uani ? ? 1.00000 ? ? O24' 1.3752(6) .37365(18) .7609(6) .025(2) Uani ? ? 1.00000 ? ? C21 .9107(9) .1912(3) .6758(9) .023(3) Uani ? ? 1.00000 ? ? C211 .8475(10) .1371(3) .5833(9) .031(4) Uani ? ? 1.00000 ? ? C22 1.0018(9) .1821(3) .8717(9) .025(3) Uani ? ? 1.00000 ? ? N23 1.0904(7) .2317(2) .9687(7) .019(3) Uani ? ? 1.00000 ? ? C24 1.1766(8) .2207(3) 1.1584(8) .021(3) Uani ? ? 1.00000 ? ? C25 1.2415(9) .2744(3) 1.2508(9) .027(3) Uani ? ? 1.00000 ? ? N26 1.0913(7) .3119(2) 1.1897(7) .024(3) Uani ? ? 1.00000 ? ? C22' .7525(9) .2296(3) .6245(8) .020(3) Uani ? ? 1.00000 ? ? N23' .8093(7) .2855(2) .6766(7) .017(2) Uani ? ? 1.00000 ? ? C24' .6581(9) .3237(3) .6138(8) .022(3) Uani ? ? 1.00000 ? ? C25' .7175(9) .3764(3) .7036(9) .022(3) Uani ? ? 1.00000 ? ? N26' .7982(7) .3652(2) .8930(7) .019(2) Uani ? ? 1.00000 ? ? H11 .27253 .11963 .76609 .02800 Uiso ? ? 1.00000 ? ? H111a .19555 .16234 .49639 .04100 Uiso ? ? 1.00000 ? ? H111b .38913 .15726 .51996 .04100 Uiso ? ? 1.00000 ? ? H111c .34307 .19499 .64009 .04100 Uiso ? ? 1.00000 ? ? H12a .61013 .10487 .77970 .02500 Uiso ? ? 1.00000 ? ? H12b .57164 .15169 .87915 .02500 Uiso ? ? 1.00000 ? ? H13 .50213 .08589 1.05667 .02400 Uiso ? ? 1.00000 ? ? H14a .78257 .11688 1.17467 .02800 Uiso ? ? 1.00000 ? ? H14b .83822 .07838 1.06318 .02800 Uiso ? ? 1.00000 ? ? H15a .90564 .03700 1.32988 .02400 Uiso ? ? 1.00000 ? ? H15b .71184 .04363 1.30423 .02400 Uiso ? ? 1.00000 ? ? H16a .83113 -.02362 1.12340 .03300 Uiso ? ? 1.00000 ? ? H16b .71774 -.03881 1.21418 .03300 Uiso ? ? 1.00000 ? ? H12'a .37935 .05675 .55774 .02900 Uiso ? ? 1.00000 ? ? H12'b .18199 .06699 .51281 .02900 Uiso ? ? 1.00000 ? ? H13' .20789 .02214 .74921 .02400 Uiso ? ? 1.00000 ? ? H14'a .12880 -.03236 .52723 .02500 Uiso ? ? 1.00000 ? ? H14'b .32155 -.03737 .54818 .02500 Uiso ? ? 1.00000 ? ? H15'a .20050 -.07843 .78608 .02500 Uiso ? ? 1.00000 ? ? H15'b .25908 -.11369 .66935 .02500 Uiso ? ? 1.00000 ? ? H16'a .54326 -.08986 .81901 .02900 Uiso ? ? 1.00000 ? ? H16'b .48419 -.09649 .96196 .02900 Uiso ? ? 1.00000 ? ? H21 .99779 .20707 .64190 .03200 Uiso ? ? 1.00000 ? ? H211a .94256 .11283 .60987 .04400 Uiso ? ? 1.00000 ? ? H211b .79322 .14260 .45899 .04400 Uiso ? ? 1.00000 ? ? H211c .76175 .12197 .61570 .04400 Uiso ? ? 1.00000 ? ? H22a 1.08545 .15400 .89711 .03200 Uiso ? ? 1.00000 ? ? H22b .91305 .17146 .90931 .03200 Uiso ? ? 1.00000 ? ? H23b 1.17618 .23728 .92851 .02400 Uiso ? ? 1.00000 ? ? H24a 1.09298 .20503 1.19585 .03000 Uiso ? ? 1.00000 ? ? H24b 1.27180 .19570 1.18592 .03000 Uiso ? ? 1.00000 ? ? H25a 1.29049 .27019 1.37352 .03500 Uiso ? ? 1.00000 ? ? H25b 1.33429 .28820 1.22154 .03500 Uiso ? ? 1.00000 ? ? H26a 1.02501 .30690 1.25211 .03200 Uiso ? ? 1.00000 ? ? H26b 1.13185 .34762 1.20741 .03200 Uiso ? ? 1.00000 ? ? H22'a .68355 .22885 .50219 .02400 Uiso ? ? 1.00000 ? ? H22'b .68019 .21868 .68066 .02400 Uiso ? ? 1.00000 ? ? H23' .88147 .29220 .62061 .02300 Uiso ? ? 1.00000 ? ? H24'a .61648 .32897 .49192 .02600 Uiso ? ? 1.00000 ? ? H24'b .56511 .30982 .63799 .02600 Uiso ? ? 1.00000 ? ? H25'a .79803 .39272 .66850 .02700 Uiso ? ? 1.00000 ? ? H25'b .61597 .39952 .67355 .02700 Uiso ? ? 1.00000 ? ? H26'a .86877 .39451 .95190 .02600 Uiso ? ? 1.00000 ? ? H26'b .71238 .36116 .93408 .02600 Uiso ? ? 1.00000 ? ? 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 .0178(4) .0148(4) .0149(4) .0000(3) .0050(3) -.0002(3) Cl1 .0206(9) .0264(9) .0245(9) .0043(7) .0121(7) .0017(7) O11 .027(3) .031(3) .035(3) .009(2) .018(2) .003(3) O12 .030(3) .053(4) .050(4) -.012(3) .018(3) -.026(3) O13 .039(3) .035(3) .037(3) .009(3) .004(3) .014(3) O14 .051(4) .051(4) .046(3) .009(3) .037(3) .013(3) Cl1' .0254(9) .0270(9) .0201(9) -.0008(7) .0136(7) -.0011(7) O11' .036(3) .024(3) .030(3) .010(2) .021(2) .005(2) O12' .046(3) .029(3) .027(3) .013(3) .020(2) .008(2) O13' .048(3) .044(4) .048(3) -.018(3) .027(3) -.022(3) O14' .031(3) .039(3) .028(3) -.003(2) .019(2) .005(2) C11 .022(4) .019(3) .022(3) -.000(3) .011(3) .001(3) C111 .031(4) .016(4) .022(4) .002(3) .001(3) .001(3) C12 .026(4) .012(3) .020(3) -.005(3) .009(3) -.004(3) N13 .018(3) .018(3) .016(3) -.003(2) .005(2) .007(2) C14 .026(4) .018(3) .021(4) .003(3) .007(3) .003(3) C15 .013(3) .024(4) .018(3) -.003(3) .002(3) -.004(3) N16 .025(3) .020(3) .026(3) -.001(2) .010(3) .001(2) C12' .018(3) .019(4) .016(3) -.003(3) .003(3) -.003(3) N13' .022(3) .019(3) .015(3) -.001(2) .007(2) .001(2) C14' .020(4) .016(3) .019(3) -.004(3) .003(3) .002(3) C15' .021(4) .016(3) .022(4) .001(3) .008(3) .002(3) N16' .020(3) .022(3) .022(3) .002(2) .011(2) .003(2) Cu2 .0193(4) .0156(4) .0144(4) -.0004(3) .0066(3) -.0002(3) Cl2 .0256(9) .0224(9) .0230(9) -.0012(7) .0156(7) -.0003(7) O21 .033(3) .030(3) .032(3) -.012(2) .024(2) -.008(2) O22 .033(3) .114(6) .037(3) .009(4) .017(3) .038(4) O23 .068(4) .020(3) .058(4) .004(3) .039(3) -.007(3) O24 .041(3) .033(3) .053(3) -.015(3) .034(3) -.007(3) Cl2' .0202(8) .0201(9) .0241(9) -.0044(7) .0112(7) -.0016(7) O21' .034(3) .034(3) .031(3) -.009(2) .022(2) -.008(2) O22' .054(4) .022(3) .064(4) .001(3) .036(3) -.010(3) O23' .025(3) .060(4) .031(3) -.008(3) .006(2) .010(3) O24' .026(3) .028(3) .029(3) -.002(2) .018(2) .001(2) C21 .025(4) .020(4) .032(4) -.007(3) .019(3) -.004(3) C211 .044(5) .025(4) .028(4) -.005(3) .019(4) -.008(3) C22 .027(4) .022(4) .030(4) -.004(3) .017(3) -.005(3) N23 .023(3) .021(3) .016(3) .004(2) .012(2) .005(2) C24 .014(3) .028(4) .019(3) .006(3) .004(3) .010(3) C25 .025(4) .033(4) .020(4) -.003(3) .006(3) -.005(3) N26 .030(3) .022(3) .017(3) -.003(3) .009(2) -.002(2) C22' .024(4) .022(3) .012(3) -.011(3) .006(3) -.009(3) N23' .020(3) .015(3) .019(3) -.003(2) .012(2) -.002(2) C24' .020(3) .026(4) .019(3) -.001(3) .008(3) .002(3) C25' .021(4) .020(4) .025(4) .005(3) .009(3) .009(3) N26' .021(3) .014(3) .022(3) -.005(2) .010(2) -.000(2) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Cu1 O11 . . 2.540(6) ? Cu1 O11' . . 2.517(6) ? Cu1 N13 . . 2.045(5) ? Cu1 N16 . . 2.016(5) ? Cu1 N13' . . 2.024(4) ? Cu1 N16' . . 1.978(5) ? Cl1 O11 . . 1.445(6) ? Cl1 O12 . . 1.442(6) ? Cl1 O13 . . 1.435(5) ? Cl1 O14 . . 1.430(7) ? Cl1' O11' . . 1.453(6) ? Cl1' O12' . . 1.444(5) ? Cl1' O13' . . 1.439(5) ? Cl1' O14' . . 1.433(6) ? C11 C111 . . 1.511(10) ? C11 C12 . . 1.524(8) ? C11 C12' . . 1.515(9) ? C11 H11 . . .964(9) ? C111 H111a . . .950(6) ? C111 H111b . . .958(9) ? C111 H111c . . .950(7) ? C12 N13 . . 1.491(9) ? C12 H12a . . .968(8) ? C12 H12b . . .944(6) ? N13 C14 . . 1.477(7) ? N13 H13 . . 1.017(7) ? C14 C15 . . 1.494(10) ? C14 H14a . . .968(7) ? C14 H14b . . .957(9) ? C15 N16 . . 1.478(9) ? C15 H15a . . .948(5) ? C15 H15b . . .967(8) ? N16 H16a . . .925(7) ? N16 H16b . . .921(6) ? C12' N13' . . 1.476(9) ? C12' H12'a . . .957(8) ? C12' H12'b . . .969(5) ? N13' C14' . . 1.470(8) ? N13' H13' . . .933(7) ? C14' C15' . . 1.519(10) ? C14' H14'a . . .954(6) ? C14' H14'b . . .959(8) ? C15' N16' . . 1.492(7) ? C15' H15'a . . .953(8) ? C15' H15'b . . .969(7) ? N16' H16'a . . .931(7) ? N16' H16'b . . .927(6) ? Cu2 O21 . . 2.518(6) ? Cu2 O21' . . 2.556(6) ? Cu2 N23 . . 1.991(6) ? Cu2 N26 . . 2.031(5) ? Cu2 N23' . . 2.018(5) ? Cu2 N26' . . 2.024(5) ? Cl2 O21 . . 1.445(6) ? Cl2 O22 . . 1.425(5) ? Cl2 O23 . . 1.437(6) ? Cl2 O24 . . 1.427(6) ? Cl2' O21' . . 1.451(6) ? Cl2' O22' . . 1.426(6) ? Cl2' O23' . . 1.439(4) ? Cl2' O24' . . 1.440(5) ? C21 C211 . . 1.536(10) ? C21 C22 . . 1.530(10) ? C21 C22' . . 1.539(10) ? C21 H21 . . .974(8) ? C211 H211a . . .946(8) ? C211 H211b . . .969(7) ? C211 H211c . . .948(9) ? C22 N23 . . 1.495(8) ? C22 H22a . . .947(7) ? C22 H22b . . .961(9) ? N23 C24 . . 1.489(8) ? N23 H23b . . .927(7) ? C24 C25 . . 1.530(10) ? C24 H24a . . .965(8) ? C24 H24b . . .958(7) ? C25 N26 . . 1.474(9) ? C25 H25a . . .953(7) ? C25 H25b . . .973(9) ? N26 H26a . . .924(7) ? N26 H26b . . .940(6) ? C22' N23' . . 1.478(8) ? C22' H22'a . . .954(6) ? C22' H22'b . . .954(8) ? N23' C24' . . 1.489(8) ? N23' H23' . . .928(7) ? C24' C25' . . 1.494(9) ? C24' H24'a . . .954(7) ? C24' H24'b . . .950(8) ? C25' N26' . . 1.488(8) ? C25' H25'a . . .937(8) ? C25' H25'b . . .967(7) ? N26' H26'a . . .939(5) ? N26' H26'b . . .927(7) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published O11 Cu1 O11' . . . 176.82(15) ? O11 Cu1 N13 . . . 88.3(2) ? O11 Cu1 N16 . . . 93.0(2) ? O11 Cu1 N13' . . . 89.5(2) ? O11 Cu1 N16' . . . 91.2(2) ? O11' Cu1 N13 . . . 94.9(2) ? O11' Cu1 N16 . . . 87.4(2) ? O11' Cu1 N13' . . . 90.3(2) ? O11' Cu1 N16' . . . 85.6(2) ? N13 Cu1 N16 . . . 84.4(2) ? N13 Cu1 N13' . . . 93.0(2) ? N13 Cu1 N16' . . . 179.0(2) ? N16 Cu1 N13' . . . 176.4(3) ? N16 Cu1 N16' . . . 96.4(2) ? N13' Cu1 N16' . . . 86.2(2) ? O11 Cl1 O12 . . . 109.1(3) ? O11 Cl1 O13 . . . 109.3(3) ? O11 Cl1 O14 . . . 108.9(3) ? O12 Cl1 O13 . . . 108.4(3) ? O12 Cl1 O14 . . . 111.6(4) ? O13 Cl1 O14 . . . 109.6(3) ? Cu1 O11 Cl1 . . . 124.0(3) ? O11' Cl1' O12' . . . 109.2(3) ? O11' Cl1' O13' . . . 108.4(3) ? O11' Cl1' O14' . . . 109.1(3) ? O12' Cl1' O13' . . . 109.4(3) ? O12' Cl1' O14' . . . 110.4(3) ? O13' Cl1' O14' . . . 110.3(4) ? Cu1 O11' Cl1' . . . 120.8(3) ? C111 C11 C12 . . . 109.8(6) ? C111 C11 C12' . . . 109.5(6) ? C111 C11 H11 . . . 110.4(6) ? C12 C11 C12' . . . 111.6(5) ? C12 C11 H11 . . . 108.7(6) ? C12' C11 H11 . . . 106.7(6) ? C11 C111 H111a . . . 110.8(7) ? C11 C111 H111b . . . 109.0(6) ? C11 C111 H111c . . . 109.8(6) ? H111a C111 H111b . . . 108.8(7) ? H111a C111 H111c . . . 109.6(7) ? H111b C111 H111c . . . 108.8(8) ? C11 C12 N13 . . . 113.3(6) ? C11 C12 H12a . . . 107.7(6) ? C11 C12 H12b . . . 109.3(6) ? N13 C12 H12a . . . 108.2(5) ? N13 C12 H12b . . . 109.7(6) ? H12a C12 H12b . . . 108.5(7) ? Cu1 N13 C12 . . . 115.9(4) ? Cu1 N13 C14 . . . 106.4(4) ? Cu1 N13 H13 . . . 100.3(4) ? C12 N13 C14 . . . 112.1(5) ? C12 N13 H13 . . . 116.3(5) ? C14 N13 H13 . . . 104.4(5) ? N13 C14 C15 . . . 107.7(6) ? N13 C14 H14a . . . 110.3(6) ? N13 C14 H14b . . . 110.8(6) ? C15 C14 H14a . . . 110.4(6) ? C15 C14 H14b . . . 110.3(6) ? H14a C14 H14b . . . 107.3(7) ? C14 C15 N16 . . . 107.5(5) ? C14 C15 H15a . . . 111.8(7) ? C14 C15 H15b . . . 109.8(6) ? N16 C15 H15a . . . 110.7(6) ? N16 C15 H15b . . . 108.9(6) ? H15a C15 H15b . . . 108.2(7) ? Cu1 N16 C15 . . . 108.4(4) ? Cu1 N16 H16a . . . 110.6(5) ? Cu1 N16 H16b . . . 110.9(4) ? C15 N16 H16a . . . 108.2(5) ? C15 N16 H16b . . . 109.7(6) ? H16a N16 H16b . . . 109.0(5) ? C11 C12' N13' . . . 114.8(6) ? C11 C12' H12'a . . . 108.3(6) ? C11 C12' H12'b . . . 108.8(6) ? N13' C12' H12'a . . . 108.5(6) ? N13' C12' H12'b . . . 108.8(6) ? H12'a C12' H12'b . . . 107.3(7) ? Cu1 N13' C12' . . . 118.0(4) ? Cu1 N13' C14' . . . 106.7(4) ? Cu1 N13' H13' . . . 107.5(4) ? C12' N13' C14' . . . 111.8(5) ? C12' N13' H13' . . . 106.6(5) ? C14' N13' H13' . . . 105.6(5) ? N13' C14' C15' . . . 108.0(5) ? N13' C14' H14'a . . . 111.2(6) ? N13' C14' H14'b . . . 109.9(6) ? C15' C14' H14'a . . . 110.3(6) ? C15' C14' H14'b . . . 109.1(6) ? H14'a C14' H14'b . . . 108.3(7) ? C14' C15' N16' . . . 106.9(5) ? C14' C15' H15'a . . . 109.9(6) ? C14' C15' H15'b . . . 109.8(6) ? N16' C15' H15'a . . . 111.5(6) ? N16' C15' H15'b . . . 111.1(6) ? H15'a C15' H15'b . . . 107.7(7) ? Cu1 N16' C15' . . . 107.9(4) ? Cu1 N16' H16'a . . . 109.8(5) ? Cu1 N16' H16'b . . . 110.0(4) ? C15' N16' H16'a . . . 110.6(5) ? C15' N16' H16'b . . . 110.7(6) ? H16'a N16' H16'b . . . 107.9(5) ? O21 Cu2 O21' . . . 179.17(15) ? O21 Cu2 N23 . . . 89.9(2) ? O21 Cu2 N26 . . . 92.8(2) ? O21 Cu2 N23' . . . 89.6(2) ? O21 Cu2 N26' . . . 90.5(2) ? O21' Cu2 N23 . . . 90.3(2) ? O21' Cu2 N26 . . . 86.4(2) ? O21' Cu2 N23' . . . 91.2(2) ? O21' Cu2 N26' . . . 89.4(2) ? N23 Cu2 N26 . . . 85.9(2) ? N23 Cu2 N23' . . . 93.9(2) ? N23 Cu2 N26' . . . 179.0(2) ? N26 Cu2 N23' . . . 177.6(3) ? N26 Cu2 N26' . . . 95.0(2) ? N23' Cu2 N26' . . . 85.2(2) ? O21 Cl2 O22 . . . 108.6(4) ? O21 Cl2 O23 . . . 108.7(4) ? O21 Cl2 O24 . . . 110.3(3) ? O22 Cl2 O23 . . . 109.2(4) ? O22 Cl2 O24 . . . 109.9(4) ? O23 Cl2 O24 . . . 110.0(4) ? Cu2 O21 Cl2 . . . 125.3(3) ? O21' Cl2' O22' . . . 109.4(4) ? O21' Cl2' O23' . . . 108.4(3) ? O21' Cl2' O24' . . . 108.0(3) ? O22' Cl2' O23' . . . 110.4(3) ? O22' Cl2' O24' . . . 110.1(3) ? O23' Cl2' O24' . . . 110.5(3) ? Cu2 O21' Cl2' . . . 122.2(3) ? C211 C21 C22 . . . 109.5(6) ? C211 C21 C22' . . . 109.3(5) ? C211 C21 H21 . . . 110.1(8) ? C22 C21 C22' . . . 112.0(7) ? C22 C21 H21 . . . 106.9(5) ? C22' C21 H21 . . . 109.0(6) ? C21 C211 H211a . . . 111.3(6) ? C21 C211 H211b . . . 109.6(6) ? C21 C211 H211c . . . 109.7(8) ? H211a C211 H211b . . . 108.1(9) ? H211a C211 H211c . . . 110.0(7) ? H211b C211 H211c . . . 108.0(7) ? C21 C22 N23 . . . 112.5(6) ? C21 C22 H22a . . . 109.8(7) ? C21 C22 H22b . . . 107.6(6) ? N23 C22 H22a . . . 109.6(5) ? N23 C22 H22b . . . 108.4(7) ? H22a C22 H22b . . . 108.8(7) ? Cu2 N23 C22 . . . 118.1(4) ? Cu2 N23 C24 . . . 107.6(4) ? Cu2 N23 H23b . . . 109.5(4) ? C22 N23 C24 . . . 110.4(5) ? C22 N23 H23b . . . 101.6(6) ? C24 N23 H23b . . . 109.3(5) ? N23 C24 C25 . . . 107.5(5) ? N23 C24 H24a . . . 110.1(5) ? N23 C24 H24b . . . 110.9(7) ? C25 C24 H24a . . . 109.4(7) ? C25 C24 H24b . . . 111.3(5) ? H24a C24 H24b . . . 107.6(7) ? C24 C25 N26 . . . 107.9(5) ? C24 C25 H25a . . . 111.2(7) ? C24 C25 H25b . . . 109.0(7) ? N26 C25 H25a . . . 111.4(7) ? N26 C25 H25b . . . 109.9(7) ? H25a C25 H25b . . . 107.3(6) ? Cu2 N26 C25 . . . 107.8(4) ? Cu2 N26 H26a . . . 111.1(4) ? Cu2 N26 H26b . . . 110.3(4) ? C25 N26 H26a . . . 109.9(6) ? C25 N26 H26b . . . 110.2(5) ? H26a N26 H26b . . . 107.5(6) ? C21 C22' N23' . . . 111.7(5) ? C21 C22' H22'a . . . 110.5(7) ? C21 C22' H22'b . . . 109.4(6) ? N23' C22' H22'a . . . 108.3(6) ? N23' C22' H22'b . . . 108.0(7) ? H22'a C22' H22'b . . . 108.8(6) ? Cu2 N23' C22' . . . 115.6(4) ? Cu2 N23' C24' . . . 107.4(4) ? Cu2 N23' H23' . . . 109.5(3) ? C22' N23' C24' . . . 112.1(5) ? C22' N23' H23' . . . 102.2(6) ? C24' N23' H23' . . . 109.9(5) ? N23' C24' C25' . . . 109.1(5) ? N23' C24' H24'a . . . 110.1(7) ? N23' C24' H24'b . . . 109.9(6) ? C25' C24' H24'a . . . 109.0(6) ? C25' C24' H24'b . . . 109.5(7) ? H24'a C24' H24'b . . . 109.2(6) ? C24' C25' N26' . . . 106.9(5) ? C24' C25' H25'a . . . 110.3(7) ? C24' C25' H25'b . . . 108.8(5) ? N26' C25' H25'a . . . 111.5(5) ? N26' C25' H25'b . . . 110.2(7) ? H25'a C25' H25'b . . . 109.1(7) ? Cu2 N26' C25' . . . 107.8(4) ? Cu2 N26' H26'a . . . 110.5(4) ? Cu2 N26' H26'b . . . 111.1(4) ? C25' N26' H26'a . . . 109.2(5) ? C25' N26' H26'b . . . 111.0(5) ? H26'a N26' H26'b . . . 107.2(6) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- 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 Cl1 3.555(2) . . ? Cu1 O12 3.796(7) . . ? Cu1 Cl1' 3.492(2) . . ? Cu1 O12' 3.648(6) . . ? Cu1 O13' 3.793(7) . . ? Cu1 C11 3.419(7) . . ? Cu1 C12 3.011(6) . . ? Cu1 C14 2.841(6) . . ? Cu1 C15 2.851(6) . . ? Cu1 C12' 3.013(6) . . ? Cu1 C14' 2.821(6) . . ? Cu1 C15' 2.819(6) . . ? Cu1 H12a 3.1189(6) . . ? Cu1 H13 2.4406(5) . . ? Cu1 H14b 3.1007(7) . . ? Cu1 H15b 3.1176(7) . . ? Cu1 H16a 2.4963(7) . . ? Cu1 H16b 2.4964(6) . . ? Cu1 H12'a 3.1820(7) . . ? Cu1 H13' 2.4707(7) . . ? Cu1 H14'b 3.0816(7) . . ? Cu1 H15'a 3.1172(7) . . ? Cu1 H16'a 2.4543(5) . . ? Cu1 H16'b 2.4544(4) . . ? Cl1 H16'a 2.864(2) . . ? O11 O12 2.352(8) . . ? O11 O13 2.349(7) . . ? O11 O14 2.338(9) . . ? O11 H12a 2.598(5) . . ? O11 H12'a 2.746(4) . . ? O12 O13 2.333(6) . . ? O12 O14 2.375(9) . . ? O12 N16' 3.077(10) . . ? O12 H16'a 2.248(7) . . ? O12 H26b 2.481(5) . '2 747' ? O12 H25'b 2.676(5) . '2 646' ? O13 O14 2.340(8) . . ? O13 N26' 3.048(7) . '2 747' ? O13 H16a 2.665(6) . . ? O13 H26b 2.416(6) . '2 747' ? O13 H26'a 2.141(5) . '2 747' ? O14 H13' 2.763(5) . '1 655' ? O14 H14'a 2.534(7) . '1 655' ? Cl1' H13 2.811(2) . . ? O11' O12' 2.361(6) . . ? O11' O13' 2.345(8) . . ? O11' O14' 2.351(8) . . ? O11' N16 3.152(8) . . ? O11' N16' 3.080(9) . . ? O12' O13' 2.353(6) . . ? O12' O14' 2.363(8) . . ? O12' N13' 3.098(9) . . ? O12' H13' 2.268(6) . . ? O12' H22a 2.541(5) . '1 455' ? O13' O14' 2.357(8) . . ? O13' H13 2.225(7) . . ? O13' H12'a 2.800(6) . '1 556' ? O14' H15a 2.621(6) . '1 455' ? O14' H16a 2.533(5) . '1 455' ? O14' H12'b 2.785(5) . '1 556' ? C11 N13 2.519(7) . . ? C11 N13' 2.520(9) . . ? C11 H111a 2.050(6) . . ? C11 H111b 2.035(8) . . ? C11 H111c 2.039(7) . . ? C11 H12a 2.039(7) . . ? C11 H12b 2.040(6) . . ? C11 H12'a 2.030(8) . . ? C11 H12'b 2.044(6) . . ? C111 C12 2.482(8) . . ? C111 C12' 2.471(9) . . ? C111 H11 2.056(8) . . ? C111 H12b 2.563(6) . . ? C111 H12'a 2.691(7) . . ? C111 H12'b 2.568(7) . . ? C12 C14 2.463(8) . . ? C12 C12' 2.514(8) . . ? C12 N13' 3.095(8) . . ? C12 H11 2.047(7) . . ? C12 H111b 2.660(6) . . ? C12 H111c 2.650(6) . . ? C12 H13 2.145(8) . . ? C12 H14b 2.607(6) . . ? C12 H12'a 2.644(6) . . ? N13 C15 2.399(7) . . ? N13 N16 2.729(7) . . ? N13 N13' 2.952(7) . . ? N13 H11 2.628(5) . . ? N13 H12a 2.016(6) . . ? N13 H12b 2.015(6) . . ? N13 H14a 2.027(5) . . ? N13 H14b 2.026(5) . . ? N13 H15b 2.603(5) . . ? C14 N16 2.396(9) . . ? C14 H12a 2.664(7) . . ? C14 H12b 2.620(6) . . ? C14 H13 1.990(7) . . ? C14 H15a 2.044(6) . . ? C14 H15b 2.035(8) . . ? C14 H16a 2.700(7) . . ? C15 H13 2.540(6) . . ? C15 H14a 2.044(7) . . ? C15 H14b 2.034(8) . . ? C15 H16a 1.974(7) . . ? C15 H16b 1.988(7) . . ? N16 N16' 2.976(7) . . ? N16 O24' 3.178(8) . '2 747' ? N16 H14b 2.623(6) . . ? N16 H15a 2.019(5) . . ? N16 H15b 2.012(6) . . ? C12' C14' 2.439(9) . . ? C12' H11 2.016(7) . . ? C12' H111a 2.647(6) . . ? C12' H111b 2.660(7) . . ? C12' H12a 2.611(6) . . ? C12' H13' 1.959(8) . . ? C12' H14'b 2.581(7) . . ? N13' C15' 2.418(9) . . ? N13' N16' 2.734(7) . . ? N13' H11 2.632(6) . . ? N13' H12'a 1.998(6) . . ? N13' H12'b 2.010(5) . . ? N13' H14'a 2.021(5) . . ? N13' H14'b 2.009(6) . . ? N13' H15'a 2.652(6) . . ? C14' N16' 2.420(7) . . ? C14' H12'a 2.607(7) . . ? C14' H12'b 2.611(7) . . ? C14' H13' 1.941(7) . . ? C14' H15'a 2.049(8) . . ? C14' H15'b 2.060(7) . . ? C15' O23 3.080(8) . '2 647' ? C15' H13' 2.635(7) . . ? C15' H14'a 2.055(6) . . ? C15' H14'b 2.045(8) . . ? C15' H16'a 2.018(7) . . ? C15' H16'b 2.016(6) . . ? N16' O23 3.022(8) . '2 647' ? N16' O24' 3.147(7) . '2 747' ? N16' H14'b 2.627(5) . . ? N16' H15'a 2.044(6) . . ? N16' H15'b 2.050(5) . . ? Cu2 Cl2 3.555(2) . . ? Cu2 O22 3.762(7) . . ? Cu2 Cl2' 3.549(2) . . ? Cu2 O22' 3.711(8) . . ? Cu2 C21 3.376(7) . . ? Cu2 C22 3.001(7) . . ? Cu2 C24 2.823(6) . . ? Cu2 C25 2.850(6) . . ? Cu2 C22' 2.972(6) . . ? Cu2 C24' 2.844(6) . . ? Cu2 C25' 2.854(6) . . ? Cu2 H22b 3.1573(11) . . ? Cu2 H23b 2.4609(10) . . ? Cu2 H24a 3.0862(9) . . ? Cu2 H25b 3.1489(7) . . ? Cu2 H26a 2.5158(9) . . ? Cu2 H26b 2.5161(8) . . ? Cu2 H22'b 3.0700(9) . . ? Cu2 H23' 2.4866(9) . . ? Cu2 H24'b 3.1324(7) . . ? Cu2 H25'a 3.1351(9) . . ? Cu2 H26'a 2.5116(11) . . ? Cu2 H26'b 2.5116(10) . . ? O21 O22 2.330(8) . . ? O21 O23 2.342(9) . . ? O21 O24 2.357(9) . . ? O21 H12b 2.605(5) . . ? O21 H22b 2.717(6) . . ? O21 H22'b 2.583(5) . . ? O22 O23 2.333(8) . . ? O22 O24 2.335(7) . . ? O22 N26 3.103(10) . . ? O22 H24a 2.792(7) . . ? O22 H26a 2.327(7) . . ? O22 H22'a 2.636(7) . '1 556' ? O23 O24 2.347(7) . . ? O23 H15'b 2.578(5) . '2 657' ? O23 H16'b 2.594(5) . '2 657' ? O23 H25b 2.738(7) . '1 455' ? O23 H26'b 2.601(7) . . ? O24 H12b 2.695(6) . . ? O24 H24b 2.591(6) . '1 455' ? Cl2' H23' 2.8853(17) . . ? O21' O22' 2.348(9) . . ? O21' O23' 2.344(7) . . ? O21' O24' 2.339(8) . . ? O21' N26 3.163(9) . . ? O22' O23' 2.353(7) . . ? O22' O24' 2.349(7) . . ? O22' N23 3.189(10) . . ? O22' H111c 2.578(6) . '1 655' ? O22' H23b 2.364(7) . . ? O23' O24' 2.366(6) . . ? O23' N23' 3.185(9) . . ? O23' H23' 2.374(6) . . ? O24' H16b 2.352(5) . '2 757' ? O24' H16'b 2.271(4) . '2 757' ? O24' H24'b 2.747(5) . '1 655' ? O24' H25'b 2.508(6) . '1 655' ? O24' H26'b 2.594(4) . '1 655' ? C21 N23 2.516(8) . . ? C21 N23' 2.498(9) . . ? C21 H211a 2.076(7) . . ? C21 H211b 2.074(7) . . ? C21 H211c 2.060(7) . . ? C21 H22a 2.054(6) . . ? C21 H22b 2.039(8) . . ? C21 H23b 2.618(6) . . ? C21 H22'a 2.075(6) . . ? C21 H22'b 2.063(8) . . ? C21 H23' 2.550(7) . . ? C211 C22 2.505(10) . . ? C211 C22' 2.508(10) . . ? C211 H21 2.082(7) . . ? C211 H22a 2.606(6) . . ? C211 H22'a 2.604(7) . . ? C22 C24 2.450(9) . . ? C22 C22' 2.545(8) . . ? C22 H21 2.039(8) . . ? C22 H211a 2.692(8) . . ? C22 H23b 1.912(7) . . ? C22 H24a 2.596(8) . . ? C22 H24b 2.697(6) . . ? C22 H22'b 2.651(6) . . ? N23 C25 2.436(8) . . ? N23 N26 2.741(8) . . ? N23 C22' 3.098(7) . . ? N23 N23' 2.930(6) . . ? N23 H21 2.625(6) . . ? N23 H22a 2.021(5) . . ? N23 H22b 2.017(5) . . ? N23 H24a 2.034(6) . . ? N23 H24b 2.038(5) . . ? N23 H25b 2.659(5) . . ? C24 N26 2.429(9) . . ? C24 H22a 2.617(7) . . ? C24 H22b 2.630(6) . . ? C24 H23b 1.998(8) . . ? C24 H25a 2.075(7) . . ? C24 H25b 2.063(7) . . ? C25 H24a 2.062(8) . . ? C25 H24b 2.079(8) . . ? C25 H26a 1.988(8) . . ? C25 H26b 2.003(8) . . ? N26 N26' 2.988(6) . . ? N26 H24a 2.661(6) . . ? N26 H25a 2.026(5) . . ? N26 H25b 2.023(6) . . ? C22' C24' 2.461(10) . . ? C22' H21 2.072(8) . . ? C22' H211b 2.681(7) . . ? C22' H211c 2.680(7) . . ? C22' H22b 2.650(6) . . ? C22' H23' 1.904(7) . . ? C22' H24'b 2.571(7) . . ? N23' C25' 2.430(9) . . ? N23' N26' 2.734(8) . . ? N23' H21 2.604(6) . . ? N23' H22'a 1.995(5) . . ? N23' H22'b 1.992(5) . . ? N23' H24'a 2.026(4) . . ? N23' H24'b 2.021(6) . . ? N23' H25'a 2.669(5) . . ? C24' N26' 2.396(8) . . ? C24' H22'a 2.586(7) . . ? C24' H22'b 2.664(7) . . ? C24' H23' 2.005(8) . . ? C24' H25'a 2.020(7) . . ? C24' H25'b 2.024(7) . . ? C25' H24'a 2.017(7) . . ? C25' H24'b 2.021(7) . . ? C25' H26'a 2.004(6) . . ? C25' H26'b 2.015(8) . . ? N26' H24'b 2.617(5) . . ? N26' H25'a 2.028(6) . . ? N26' H25'b 2.035(5) . . ? H11 H111a 2.3589(2) . . ? H11 H111c 2.3553(3) . . ? H11 H12'b 2.3575(2) . . ? H111a H111b 1.5513(2) . . ? H111a H111c 1.55145(12) . . ? H111a H12'b 2.3823(4) . . ? H111b H111c 1.55132(13) . . ? H111c H12b 2.38289(18) . . ? H12a H12b 1.55135(16) . . ? H12a H12'a 2.37834(18) . . ? H12a H211c 2.28678(19) . . ? H13 H14a 2.2637(2) . . ? H13 H15b 2.34674(18) . . ? H14a H14b 1.55134(13) . . ? H14a H15a 2.3685(3) . . ? H14a H15b 2.3319(2) . . ? H14b H15a 2.3342(2) . . ? H15a H15b 1.5513(2) . . ? H15a H16a 2.1971(2) . . ? H15a H16b 2.3866(3) . . ? H15a H12'b 2.3009(2) . '1 656' ? H15b H16b 2.1977(3) . . ? H16a H16b 1.50241(12) . . ? H12'a H12'b 1.5513(2) . . ? H12'a H14'b 2.3859(4) . . ? H12'b H13' 2.2295(2) . . ? H13' H14'a 2.1888(2) . . ? H14'a H14'b 1.5513(2) . . ? H14'a H15'a 2.3261(2) . . ? H14'a H15'b 2.3740(3) . . ? H14'b H15'b 2.3231(3) . . ? H15'a H15'b 1.55135(13) . . ? H15'a H16'b 2.2546(2) . . ? H15'b H16'a 2.2531(2) . . ? H16'a H16'b 1.50243(14) . . ? H21 H211a 2.3835(4) . . ? H21 H211b 2.3835(2) . . ? H21 H22a 2.3779(2) . . ? H21 H23b 2.3817(2) . . ? H21 H23' 2.3063(3) . . ? H211a H211b 1.55133(12) . . ? H211a H211c 1.55134(18) . . ? H211b H211c 1.55125(15) . . ? H22a H22b 1.55143(17) . . ? H22a H23b 2.1844(3) . . ? H23b H24b 2.2429(2) . . ? H24a H24b 1.55135(18) . . ? H24a H25a 2.3538(2) . . ? H24b H25b 2.3516(4) . . ? H25a H25b 1.55129(15) . . ? H25a H26a 2.2143(2) . . ? H25b H26b 2.2133(2) . . ? H26a H26b 1.50239(13) . . ? H22'a H22'b 1.55126(18) . . ? H22'a H23' 2.1993(2) . . ? H23' H24'a 2.2152(2) . . ? H24'a H24'b 1.55128(14) . . ? H24'a H25'a 2.2712(2) . . ? H24'a H25'b 2.3400(2) . . ? H24'b H25'b 2.2686(4) . . ? H25'a H25'b 1.55133(18) . . ? H25'a H26'a 2.2279(3) . . ? H25'b H26'b 2.2290(2) . . ? H26'a H26'b 1.50237(15) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 900 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 34 _reflns_limit_l_min -11 _reflns_limit_l_max 10 _reflns_number_observed ? _reflns_d_resolution_high .726 _reflns_d_resolution_low 12.411 _diffrn_reflns_av_sigmaI/netI .103 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .069 _refine_ls_wR_factor_all .045 _refine_ls_goodness_of_fit_all .941 _refine_ls_shift/su_mean .001 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_global _audit_creation_method Xtal3.6 _audit_creation_date 99-11-15 _audit_update_record ? #============================================================================== # (Publishing Staff Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia Nedlands Western Australia 6907 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal ? _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Skelton, Brian W.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; 'White, Allan H.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Pogram for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_ykn4cu # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C9 H24 Cl2 Cu1 N4 O4' _chemical_formula_moiety ? _chemical_formula_weight 386.77 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M p_n_m_a _symmetry_space_group_name_Hall -p_2ac_2n loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,-y,1/2+z 1/2+x,1/2-y,1/2-z -x,1/2+y,-z -x,-y,-z 1/2+x,+y,1/2-z 1/2-x,1/2+y,1/2+z +x,1/2-y,+z _cell_length_a 11.2460(10) _cell_length_b 9.373(2) _cell_length_c 15.291(2) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 1611.8(4) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 3507 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 1.703 _exptl_crystal_description bar _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_size_rad ? _exptl_crystal_colour blue #<< use NfA code _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .748 _exptl_absorpt_correction_T_max .913 _diffrn_reflns_number 19214 _reflns_number_total 2235 _reflns_Friedel_coverage 0 _reflns_number_gt 1847 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.35 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .0263 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .031 _refine_ls_wR_factor_ref .04 _refine_ls_goodness_of_fit_ref 1.448 _refine_ls_number_reflns 1847 _refine_ls_number_parameters 170 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .094 _refine_diff_density_min -.328 _refine_diff_density_max .439 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 76(231) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ 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 36 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 96 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 8 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cu ? 0 4 .263 1.266 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 16 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 16 .008 .006 '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_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu .38962(3) .75000 .23676(2) .0351(2) Uani ? ? 1.00000 ? ? C1 .3612(2) .75000 .45953(16) .0348(13) Uani ? ? 1.00000 ? ? C11 .4166(3) .75000 .5514(2) .052(2) Uani ? ? 1.00000 ? ? C11' .2260(3) .75000 .4675(2) .0484(18) Uani ? ? 1.00000 ? ? C2 .40624(18) .6146(2) .41409(11) .0351(10) Uani ? ? 1.00000 ? ? N3 .35951(14) .59406(15) .32454(10) .0307(7) Uani ? ? 1.00000 ? ? C4 .4016(2) .4609(2) .28358(14) .0427(11) Uani ? ? 1.00000 ? ? C5 .3569(2) .4591(2) .19031(14) .0469(12) Uani ? ? 1.00000 ? ? N6 .3972(2) .5903(2) .14795(12) .0493(11) Uani ? ? 1.00000 ? ? Cl1 .62472(5) .75000 .26866(5) .0454(4) Uani ? ? 1.00000 ? ? Cl2 .14041(6) .25000 .41596(5) .0484(4) Uani ? ? 1.00000 ? ? O21 .2430(2) .25000 .4683(2) .116(3) Uani ? ? 1.00000 ? ? O22 .0367(4) .25000 .4648(3) .086(4) Uani ? ? .723(14) ? ? O23 .1437(3) .3716(7) .3633(5) .162(6) Uani ? ? .723(14) ? ? O22' .0771(19) .356(2) .4435(10) .23(2) Uani ? ? .277(14) ? ? O23' .1409(11) .25000 .3278(6) .091(10) Uani ? ? .277(14) ? ? H11a .497(3) .75000 .545(2) .061(10) Uiso ? ? 1.00000 ? ? H11b .3839(17) .692(2) .5866(13) .045(7) Uiso ? ? 1.00000 ? ? H11'a .185(2) .75000 .4104(18) .043(7) Uiso ? ? 1.00000 ? ? H11'b .197(2) .665(2) .4985(14) .053(6) Uiso ? ? 1.00000 ? ? H2a .3870(15) .540(2) .4479(14) .042(5) Uiso ? ? 1.00000 ? ? H2b .4921(16) .6169(17) .4083(10) .029(4) Uiso ? ? 1.00000 ? ? H3 .2910(19) .589(2) .3262(12) .034(5) Uiso ? ? 1.00000 ? ? H4a .3795(19) .380(3) .3104(17) .060(7) Uiso ? ? 1.00000 ? ? H4b .486(2) .464(2) .2822(12) .045(6) Uiso ? ? 1.00000 ? ? H5a .274(2) .458(2) .1895(16) .064(7) Uiso ? ? 1.00000 ? ? H5b .3870(18) .376(3) .1605(14) .055(7) Uiso ? ? 1.00000 ? ? H6a .358(2) .611(4) .105(2) .090(10) Uiso ? ? 1.00000 ? ? H6b .467(2) .578(2) .1321(16) .068(9) Uiso ? ? 1.00000 ? ? 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 Cu .0533(2) .02488(18) .02717(18) .00000 -.00331(13) .00000 C1 .0321(12) .0454(14) .0269(12) .00000 -.0002(9) .00000 C11 .054(2) .076(2) .0270(14) .00000 -.0055(13) .00000 C11' .0377(15) .068(2) .0392(16) .00000 .0089(12) .00000 C2 .0364(10) .0366(10) .0323(9) -.0002(7) -.0032(7) .0072(7) N3 .0288(8) .0284(7) .0350(7) -.0005(6) -.0020(6) -.0001(6) C4 .0549(13) .0246(9) .0486(11) .0018(8) -.0008(9) .0001(8) C5 .0588(14) .0313(10) .0505(12) -.0015(9) -.0045(10) -.0118(9) N6 .0735(14) .0388(9) .0356(9) .0018(9) -.0018(9) -.0061(7) Cl1 .0285(3) .0551(5) .0527(4) .00000 .0100(3) .00000 Cl2 .0378(4) .0640(5) .0434(4) .00000 .0022(3) .00000 O21 .0521(18) .203(4) .092(2) .00000 -.0201(14) .00000 O22 .037(2) .160(6) .062(3) .00000 .0169(16) .00000 O23 .090(3) .165(7) .231(9) -.026(3) -.015(3) .137(7) O22' .34(3) .22(3) .128(13) .20(2) -.082(17) -.061(15) O23' .105(9) .137(17) .030(5) .00000 .020(5) .00000 # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Cu N3 . . 2.0131(15) ? Cu N6 . . 2.0226(19) ? Cu Cl1 . . 2.6885(7) ? Cu N3 . '8 565' 2.0131(15) ? Cu N6 . '8 565' 2.0226(19) ? C1 C11 . . 1.537(4) ? C1 C11' . . 1.526(4) ? C1 C2 . . 1.533(2) ? C1 C2 . '8 565' 1.533(2) ? C11 H11a . . .90(4) ? C11 H11b . . .85(2) ? C11 H11b . '8 565' .85(2) ? C11' H11'a . . .99(3) ? C11' H11'b . . .98(2) ? C11' H11'b . '8 565' .98(2) ? C2 N3 . . 1.479(2) ? C2 H2a . . .90(2) ? C2 H2b . . .970(19) ? N3 C4 . . 1.474(2) ? N3 H3 . . .77(2) ? C4 C5 . . 1.512(3) ? C4 H4a . . .89(3) ? C4 H4b . . .95(2) ? C5 N6 . . 1.462(3) ? C5 H5a . . .94(2) ? C5 H5b . . .97(3) ? N6 H6a . . .82(3) ? N6 H6b . . .83(3) ? Cl2 O21 . . 1.404(3) ? Cl2 O22 . . 1.385(5) ? Cl2 O23 . . 1.396(7) ? Cl2 O22' . . 1.292(19) ? Cl2 O23' . . 1.348(10) ? Cl2 O23 . 8 1.396(7) ? Cl2 O22' . 8 1.292(19) ? O22 O22' . . 1.139(19) ? O22 O22' . 8 1.139(19) ? O23 O22' . . 1.444(18) ? O23 O23' . . 1.263(8) ? O22' O22' . 8 1.99(3) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published N3 Cu N6 . . . 85.27(7) ? N3 Cu Cl1 . . . 92.55(5) ? N3 Cu N3 . . '8 565' 93.11(6) ? N3 Cu N6 . . '8 565' 172.71(8) ? N6 Cu Cl1 . . . 94.62(7) ? N6 Cu N3 . . '8 565' 172.71(8) ? N6 Cu N6 . . '8 565' 95.45(8) ? Cl1 Cu N3 . . '8 565' 92.55(5) ? Cl1 Cu N6 . . '8 565' 94.62(7) ? N3 Cu N6 '8 565' . '8 565' 85.27(7) ? C11 C1 C11' . . . 109.3(2) ? C11 C1 C2 . . . 106.30(14) ? C11 C1 C2 . . '8 565' 106.30(14) ? C11' C1 C2 . . . 111.44(14) ? C11' C1 C2 . . '8 565' 111.44(14) ? C2 C1 C2 . . '8 565' 111.77(18) ? C1 C11 H11a . . . 107(2) ? C1 C11 H11b . . . 113.8(13) ? C1 C11 H11b . . '8 565' 113.8(13) ? H11a C11 H11b . . . 120.1(19) ? H11a C11 H11b . . '8 565' 120.1(19) ? H11b C11 H11b . . '8 565' 80(2) ? C1 C11' H11'a . . . 113.2(16) ? C1 C11' H11'b . . . 111.6(13) ? C1 C11' H11'b . . '8 565' 111.6(13) ? H11'a C11' H11'b . . . 105.8(15) ? H11'a C11' H11'b . . '8 565' 105.8(15) ? H11'b C11' H11'b . . '8 565' 108.5(17) ? C1 C2 N3 . . . 114.21(16) ? C1 C2 H2a . . . 107.8(13) ? C1 C2 H2b . . . 110.6(9) ? N3 C2 H2a . . . 110.2(13) ? N3 C2 H2b . . . 105.8(9) ? H2a C2 H2b . . . 108.1(15) ? Cu N3 C2 . . . 117.57(11) ? Cu N3 C4 . . . 106.10(12) ? Cu N3 H3 . . . 103.8(13) ? C2 N3 C4 . . . 112.92(15) ? C2 N3 H3 . . . 109.4(13) ? C4 N3 H3 . . . 106.1(13) ? N3 C4 C5 . . . 107.66(16) ? N3 C4 H4a . . . 115.4(17) ? N3 C4 H4b . . . 107.7(12) ? C5 C4 H4a . . . 109.4(17) ? C5 C4 H4b . . . 108.2(12) ? H4a C4 H4b . . . 108.2(18) ? C4 C5 N6 . . . 107.77(17) ? C4 C5 H5a . . . 110.2(15) ? C4 C5 H5b . . . 109.7(13) ? N6 C5 H5a . . . 108.2(14) ? N6 C5 H5b . . . 111.3(14) ? H5a C5 H5b . . . 109.6(19) ? Cu N6 C5 . . . 108.19(13) ? Cu N6 H6a . . . 110(2) ? Cu N6 H6b . . . 109.7(17) ? C5 N6 H6a . . . 113(2) ? C5 N6 H6b . . . 108.0(16) ? H6a N6 H6b . . . 108(3) ? O21 Cl2 O22 . . . 112.6(2) ? O21 Cl2 O23 . . . 107.9(2) ? O21 Cl2 O22' . . . 105.5(8) ? O21 Cl2 O23' . . . 124.5(5) ? O21 Cl2 O23 . . 8 107.9(2) ? O21 Cl2 O22' . . 8 105.5(8) ? O22 Cl2 O23 . . . 109.4(2) ? O22 Cl2 O22' . . . 50.2(8) ? O22 Cl2 O23' . . . 122.9(6) ? O22 Cl2 O23 . . 8 109.4(2) ? O22 Cl2 O22' . . 8 50.2(8) ? O23 Cl2 O22' . . . 64.8(8) ? O23 Cl2 O23' . . . 54.8(3) ? O23 Cl2 O23 . . 8 109.5(4) ? O23 Cl2 O22' . . 8 146.1(9) ? O22' Cl2 O23' . . . 109.2(8) ? O22' Cl2 O23 . . 8 146.1(9) ? O22' Cl2 O22' . . 8 100.4(12) ? O23' Cl2 O23 . . 8 54.8(3) ? O23' Cl2 O22' . . 8 109.2(8) ? O23 Cl2 O22' 8 . 8 64.8(8) ? Cl2 O22 O22' . . . 60.7(10) ? Cl2 O22 O22' . . 8 60.7(10) ? O22' O22 O22' . . 8 121.3(14) ? Cl2 O23 O22' . . . 54.1(8) ? Cl2 O23 O23' . . . 60.7(5) ? O22' O23 O23' . . . 105.1(9) ? Cl2 O22' O22 . . . 69.1(10) ? Cl2 O22' O23 . . . 61.0(8) ? Cl2 O22' O22' . . 8 39.8(8) ? O22 O22' O23 . . . 122.5(14) ? O22 O22' O22' . . 8 29.4(8) ? O23 O22' O22' . . 8 95.8(11) ? Cl2 O23' O23 . . . 64.5(5) ? Cl2 O23' O23 . . 8 64.5(5) ? O23 O23' O23 . . 8 128.9(9) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- 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 Cu C1 3.421(3) . . ? Cu C2 2.9995(18) . . ? Cu C2 2.9995(18) . '8 565' ? Cu C4 2.806(2) . . ? Cu C4 2.806(2) . '8 565' ? Cu C5 2.842(2) . . ? Cu C5 2.842(2) . '8 565' ? Cu Cl1 2.9803(8) . '3 465' ? Cu H2b 3.125(16) . '8 565' ? Cu H2b 3.125(16) . . ? Cu H3 2.321(19) . . ? Cu H3 2.321(19) . '8 565' ? Cu H4b 2.97(2) . . ? Cu H4b 2.97(2) . '8 565' ? Cu H5a 3.12(2) . . ? Cu H5a 3.12(2) . '8 565' ? Cu H6a 2.42(3) . '8 565' ? Cu H6a 2.42(3) . . ? Cu H6b 2.43(2) . '8 565' ? Cu H6b 2.43(2) . . ? C1 N3 2.529(2) . '8 565' ? C1 N3 2.529(2) . . ? C1 H11a 2.00(3) . . ? C1 H11b 2.03(2) . '8 565' ? C1 H11b 2.03(2) . . ? C1 H11'a 2.12(3) . . ? C1 H11'b 2.10(2) . '8 565' ? C1 H11'b 2.10(2) . . ? C1 H2a 2.00(2) . . ? C1 H2a 2.00(2) . '8 565' ? C1 H2b 2.083(17) . '8 565' ? C1 H2b 2.083(17) . . ? C1 H3 2.659(18) . . ? C1 H3 2.659(18) . '8 565' ? C11 C11' 2.498(5) . . ? C11 C2 2.457(3) . . ? C11 C2 2.457(3) . '8 565' ? C11 H2a 2.55(2) . . ? C11 H2a 2.55(2) . '8 565' ? C11 H2b 2.659(16) . . ? C11 H2b 2.659(16) . '8 565' ? C11' C2 2.527(3) . '8 565' ? C11' C2 2.527(3) . . ? C11' N3 3.028(3) . . ? C11' N3 3.028(3) . '8 565' ? C11' H11b 2.60(2) . '8 565' ? C11' H11b 2.60(2) . . ? C11' H2a 2.69(2) . '8 565' ? C11' H2a 2.69(2) . . ? C2 C2 2.538(3) . '8 565' ? C2 N3 3.100(2) . '8 565' ? C2 C4 2.462(3) . . ? C2 H11a 2.58(3) . . ? C2 H2b 2.697(16) . '8 565' ? C2 H3 1.88(2) . . ? C2 H4b 2.62(2) . . ? N3 N3 2.923(2) . '8 565' ? N3 C5 2.411(3) . . ? N3 N6 2.733(2) . . ? N3 H11'a 2.78(2) . . ? N3 H2a 1.98(2) . . ? N3 H2b 1.977(17) . . ? N3 H4a 2.03(3) . . ? N3 H4b 1.98(2) . . ? N3 H5a 2.61(2) . . ? C4 N6 2.403(3) . . ? C4 H2a 2.62(2) . . ? C4 H2b 2.610(16) . . ? C4 H3 1.85(2) . . ? C4 H5a 2.03(2) . . ? C4 H5b 2.05(2) . . ? C4 H6b 2.67(2) . . ? C5 H3 2.518(18) . . ? C5 H4a 2.00(3) . . ? C5 H4b 2.02(2) . . ? C5 H6a 1.93(3) . . ? C5 H6b 1.89(3) . . ? N6 N6 2.993(3) . '8 565' ? N6 O22' 3.180(16) . '2 564' ? N6 H4b 2.57(2) . . ? N6 H5a 1.97(2) . . ? N6 H5b 2.02(3) . . ? Cl1 H11'a 2.82(3) . '3 565' ? Cl1 H2b 2.888(16) . '8 565' ? Cl1 H2b 2.888(16) . . ? Cl1 H3 2.81(2) . 6 ? Cl1 H3 2.81(2) . '3 565' ? O21 O22 2.320(5) . . ? O21 O23 2.264(7) . 8 ? O21 O23 2.264(7) . . ? O21 O22' 2.15(2) . . ? O21 O22' 2.15(2) . 8 ? O21 O23' 2.437(11) . . ? O21 H6a 2.71(3) . '7 545' ? O21 H6a 2.71(3) . '2 565' ? O22 O23 2.270(7) . 8 ? O22 O23 2.270(7) . . ? O22 O23' 2.400(12) . . ? O22 H6a 2.77(3) . '7 545' ? O22 H6a 2.77(3) . '2 565' ? O23 O23 2.280(9) . 8 ? O23 O22' 2.571(19) . 8 ? O23 H3 2.68(2) . . ? O23 H4a 2.77(2) . . ? O23 H6b 2.78(3) . '6 455' ? O22' O23' 2.152(19) . . ? O22' H5b 2.67(3) . '6 455' ? O22' H6a 2.59(4) . '2 565' ? O22' H6b 2.69(3) . '6 455' ? H11a H11b 1.52(4) . '8 565' ? H11a H11b 1.52(4) . . ? H11b H11b 1.09(3) . '8 565' ? H11'a H11'b 1.57(3) . '8 565' ? H11'a H11'b 1.57(3) . . ? H11'a H3 2.32(3) . . ? H11'a H3 2.32(3) . '8 565' ? H11'b H11'b 1.59(3) . '8 565' ? H2a H2b 1.51(3) . . ? H2a H3 2.20(3) . . ? H3 H4a 2.20(3) . . ? H4a H4b 1.49(3) . . ? H4a H5a 2.32(3) . . ? H4a H5b 2.29(3) . . ? H4b H5b 2.32(3) . . ? H5a H5b 1.55(3) . . ? H5a H6a 2.15(4) . . ? H5b H5b 2.36(4) . 8 ? H5b H6a 2.39(4) . . ? H5b H6b 2.15(4) . . ? H6a H6b 1.33(4) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 804 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _reflns_number_observed ? _reflns_d_resolution_high .725 _reflns_d_resolution_low 9.043 _diffrn_reflns_av_sigmaI/netI .036 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970' _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .041 _refine_ls_wR_factor_all .041 _refine_ls_goodness_of_fit_all 1.351 _refine_ls_shift/su_mean .012 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_global _audit_creation_method Xtal3.6 _audit_creation_date 99-11-15 _audit_update_record ? #============================================================================== # (Publishing Staff Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia Nedlands Western Australia 6907 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal ? _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Skelton, Brian W.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; 'White, Allan H.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Pogram for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_ykbase # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C16 H50 Cl6 N6 O2' _chemical_formula_moiety ? _chemical_formula_weight 571.33 _chemical_melting_point ? _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 _cell_length_a 7.0501(8) _cell_length_b 18.946(2) _cell_length_c 11.0050(12) _cell_angle_alpha 90.00000 _cell_angle_beta 105.3830(10) _cell_angle_gamma 90.00000 _cell_volume 1417.3(3) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu .63 _exptl_crystal_description prism _exptl_crystal_size_max .45 _exptl_crystal_size_mid .35 _exptl_crystal_size_min .30 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .653 _exptl_absorpt_correction_T_max .962 _diffrn_reflns_number 15638 _reflns_number_total 3519 _reflns_Friedel_coverage 0 _reflns_number_gt 3181 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 28.85 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .029 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .026 _refine_ls_wR_factor_ref .037 _refine_ls_goodness_of_fit_ref 1.476 _refine_ls_number_reflns 3181 _refine_ls_number_parameters 237 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .056 _refine_diff_density_min -.285 _refine_diff_density_max .468 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 575(529) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ 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 32 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 100 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 12 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 12 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 4 .008 .006 '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_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cl1 .14081(4) .187209(15) .53877(3) .01915(14) Uani ? ? 1.00000 ? ? Cl2 -.30400(4) .152099(15) .19209(3) .02033(15) Uani ? ? 1.00000 ? ? Cl3 -.38615(4) .033366(14) .66092(3) .01864(14) Uani ? ? 1.00000 ? ? C11 .2536(2) .05797(7) 1.01699(12) .0225(6) Uani ? ? 1.00000 ? ? C12 .00716(18) .13373(7) .86679(13) .0214(6) Uani ? ? 1.00000 ? ? C1 .19493(16) .08961(6) .88342(10) .0150(5) Uani ? ? 1.00000 ? ? C2a .36571(17) .13351(6) .86011(11) .0151(5) Uani ? ? 1.00000 ? ? N3a .40901(15) .19878(5) .93910(10) .0150(4) Uani ? ? 1.00000 ? ? C4a .57577(17) .23977(6) .91356(12) .0172(5) Uani ? ? 1.00000 ? ? C5a .61051(18) .30943(6) .98339(12) .0185(5) Uani ? ? 1.00000 ? ? N6a .48523(17) .36725(5) .91271(11) .0196(5) Uani ? ? 1.00000 ? ? C2b .16285(18) .02706(6) .79055(10) .0157(5) Uani ? ? 1.00000 ? ? N3b .04916(15) .04575(5) .65830(9) .0144(4) Uani ? ? 1.00000 ? ? C4b .06852(17) -.00916(6) .56441(10) .0165(5) Uani ? ? 1.00000 ? ? O01 .15140(15) .29863(6) .75020(10) .0298(5) Uani ? ? 1.00000 ? ? H11A .370(2) .0306(8) 1.0348(14) .032(4) Uiso ? ? 1.00000 ? ? H11B .155(3) .0290(9) 1.0310(16) .036(4) Uiso ? ? 1.00000 ? ? H11C .280(2) .0943(8) 1.0853(14) .028(4) Uiso ? ? 1.00000 ? ? H12A .024(2) .1668(8) .9286(15) .026(4) Uiso ? ? 1.00000 ? ? H12B -.105(2) .1032(8) .8692(13) .023(4) Uiso ? ? 1.00000 ? ? H12c -.024(3) .1594(9) .7873(17) .034(4) Uiso ? ? 1.00000 ? ? H2aA .335(2) .1472(7) .7710(14) .018(3) Uiso ? ? 1.00000 ? ? H2aB .486(2) .1061(7) .8789(12) .014(3) Uiso ? ? 1.00000 ? ? H3aA .440(2) .1890(8) 1.0154(17) .027(4) Uiso ? ? 1.00000 ? ? H3aB .314(2) .2254(8) .9268(14) .024(4) Uiso ? ? 1.00000 ? ? H4aA .550(2) .2468(8) .8319(15) .023(4) Uiso ? ? 1.00000 ? ? H4aB .692(2) .2101(7) .9429(12) .013(3) Uiso ? ? 1.00000 ? ? H5aA .743(2) .3234(7) .9928(14) .020(3) Uiso ? ? 1.00000 ? ? H5aB .589(2) .3037(7) 1.0650(14) .021(4) Uiso ? ? 1.00000 ? ? H6aA .519(3) .3743(9) .8422(18) .038(5) Uiso ? ? 1.00000 ? ? H6aB .488(2) .4050(9) .9605(14) .028(4) Uiso ? ? 1.00000 ? ? H6aC .360(3) .3542(9) .8871(17) .038(5) Uiso ? ? 1.00000 ? ? H2bA .288(2) .0076(7) .7849(12) .014(3) Uiso ? ? 1.00000 ? ? H2bB .088(2) -.0093(7) .8178(12) .012(3) Uiso ? ? 1.00000 ? ? H3bA -.078(3) .0505(8) .6517(15) .032(4) Uiso ? ? 1.00000 ? ? H3bB .090(2) .0860(8) .6371(12) .018(3) Uiso ? ? 1.00000 ? ? H4bA .202(2) -.0108(7) .5642(12) .016(3) Uiso ? ? 1.00000 ? ? H4bB .035(2) -.0519(7) .5929(13) .018(3) Uiso ? ? 1.00000 ? ? H01A .140(3) .2749(10) .6867(18) .039(5) Uiso ? ? 1.00000 ? ? H01B .050(3) .3111(11) .742(2) .052(7) Uiso ? ? 1.00000 ? ? 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 Cl1 .02080(16) .01764(15) .02040(15) -.00096(10) .00791(11) .00248(10) Cl2 .02064(17) .02021(16) .01939(16) .00069(11) .00398(12) .00073(10) Cl3 .01779(16) .01843(15) .01961(16) -.00228(10) .00480(11) -.00088(10) C11 .0264(7) .0239(6) .0167(6) -.0077(5) .0050(5) .0006(5) C12 .0175(6) .0207(6) .0258(7) -.0012(5) .0055(5) -.0095(5) C1 .0156(5) .0146(5) .0147(5) -.0023(4) .0040(4) -.0024(4) C2a .0170(6) .0139(5) .0150(5) -.0012(4) .0050(4) -.0032(4) N3a .0156(5) .0127(4) .0172(5) -.0000(4) .0052(4) -.0008(4) C4a .0164(6) .0145(5) .0224(6) -.0010(4) .0083(5) -.0001(4) C5a .0159(6) .0159(6) .0227(6) -.0017(4) .0032(5) -.0004(4) N6a .0205(6) .0132(5) .0255(6) -.0010(4) .0068(4) -.0017(4) C2b .0188(6) .0133(5) .0139(5) -.0004(4) .0023(4) -.0008(4) N3b .0162(5) .0119(4) .0151(5) -.0011(4) .0041(4) -.0011(3) C4b .0187(6) .0145(5) .0163(5) .0010(4) .0046(5) -.0036(4) O01 .0207(5) .0388(6) .0282(5) .0023(4) .0032(4) -.0116(4) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published C11 C1 . . 1.5391(17) ? C11 H11A . . .944(16) ? C11 H11B . . .931(19) ? C11 H11C . . .999(15) ? C12 C1 . . 1.5350(17) ? C12 H12A . . .910(16) ? C12 H12B . . .988(15) ? C12 H12c . . .974(18) ? C1 C2a . . 1.5398(17) ? C1 C2b . . 1.5419(16) ? C2a N3a . . 1.4957(15) ? C2a H2aA . . .981(15) ? C2a H2aB . . .967(13) ? N3a C4a . . 1.4966(17) ? N3a H3aA . . .831(18) ? N3a H3aB . . .821(16) ? C4a C5a . . 1.5140(17) ? C4a H4aA . . .879(16) ? C4a H4aB . . .976(13) ? C5a N6a . . 1.4902(15) ? C5a H5aA . . .949(16) ? C5a H5aB . . .955(16) ? N6a H6aA . . .88(2) ? N6a H6aB . . .885(16) ? N6a H6aC . . .886(19) ? C2b N3b . . 1.5057(14) ? C2b H2bA . . .974(15) ? C2b H2bB . . .964(14) ? N3b C4b . . 1.4978(16) ? N3b H3bA . . .883(19) ? N3b H3bB . . .869(15) ? C4b H4bA . . .945(16) ? C4b H4bB . . .921(15) ? C4b C4b . '3 556' 1.5289(14) ? O01 H01A . . .82(2) ? O01 H01B . . .73(2) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published C1 C11 H11A . . . 114.2(10) ? C1 C11 H11B . . . 111.4(10) ? C1 C11 H11C . . . 113.6(9) ? H11A C11 H11B . . . 106.7(15) ? H11A C11 H11C . . . 103.9(12) ? H11B C11 H11C . . . 106.4(15) ? C1 C12 H12A . . . 110.3(10) ? C1 C12 H12B . . . 110.6(9) ? C1 C12 H12c . . . 111.2(12) ? H12A C12 H12B . . . 109.4(15) ? H12A C12 H12c . . . 106.4(14) ? H12B C12 H12c . . . 108.9(13) ? C11 C1 C12 . . . 109.31(11) ? C11 C1 C2a . . . 110.23(9) ? C11 C1 C2b . . . 106.78(9) ? C12 C1 C2a . . . 111.95(9) ? C12 C1 C2b . . . 111.67(9) ? C2a C1 C2b . . . 106.76(10) ? C1 C2a N3a . . . 113.44(10) ? C1 C2a H2aA . . . 109.7(9) ? C1 C2a H2aB . . . 110.7(9) ? N3a C2a H2aA . . . 108.6(8) ? N3a C2a H2aB . . . 106.7(8) ? H2aA C2a H2aB . . . 107.6(12) ? C2a N3a C4a . . . 111.67(10) ? C2a N3a H3aA . . . 111.2(10) ? C2a N3a H3aB . . . 112.4(10) ? C4a N3a H3aA . . . 107.2(11) ? C4a N3a H3aB . . . 107.3(12) ? H3aA N3a H3aB . . . 106.8(16) ? N3a C4a C5a . . . 112.73(11) ? N3a C4a H4aA . . . 108.1(10) ? N3a C4a H4aB . . . 105.7(9) ? C5a C4a H4aA . . . 110.4(10) ? C5a C4a H4aB . . . 109.0(7) ? H4aA C4a H4aB . . . 110.8(14) ? C4a C5a N6a . . . 112.47(9) ? C4a C5a H5aA . . . 108.7(9) ? C4a C5a H5aB . . . 109.4(8) ? N6a C5a H5aA . . . 106.3(8) ? N6a C5a H5aB . . . 110.8(8) ? H5aA C5a H5aB . . . 109.0(12) ? C5a N6a H6aA . . . 107.9(11) ? C5a N6a H6aB . . . 111.5(9) ? C5a N6a H6aC . . . 111.3(11) ? H6aA N6a H6aB . . . 115.6(16) ? H6aA N6a H6aC . . . 104.0(16) ? H6aB N6a H6aC . . . 106.2(16) ? C1 C2b N3b . . . 114.01(9) ? C1 C2b H2bA . . . 111.0(7) ? C1 C2b H2bB . . . 109.8(8) ? N3b C2b H2bA . . . 106.6(7) ? N3b C2b H2bB . . . 105.9(7) ? H2bA C2b H2bB . . . 109.3(12) ? C2b N3b C4b . . . 112.39(9) ? C2b N3b H3bA . . . 111.8(11) ? C2b N3b H3bB . . . 109.7(8) ? C4b N3b H3bA . . . 106.9(10) ? C4b N3b H3bB . . . 109.2(10) ? H3bA N3b H3bB . . . 106.6(14) ? N3b C4b H4bA . . . 107.4(8) ? N3b C4b H4bB . . . 107.2(9) ? N3b C4b C4b . . '3 556' 109.34(9) ? H4bA C4b H4bB . . . 108.6(12) ? H4bA C4b C4b . . '3 556' 113.0(8) ? H4bB C4b C4b . . '3 556' 111.0(7) ? H01A O01 H01B . . . 102(2) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- 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 Cl1 N3a 3.2472(12) . '4 554' ? Cl1 N6a 3.2669(13) . '4 554' ? Cl1 N3b 3.1276(11) . . ? Cl1 O01 3.2076(12) . '4 554' ? Cl1 O01 3.1278(12) . . ? Cl1 H2aA 2.670(14) . . ? Cl1 H3aB 2.558(17) . '4 554' ? Cl1 H5aA 2.723(16) . '4 454' ? Cl1 H6aC 2.68(2) . '4 554' ? Cl1 H3bB 2.276(15) . . ? Cl1 H01A 2.33(2) . . ? Cl2 N3a 3.1047(10) . '1 454' ? Cl2 N6a 3.1861(14) . '4 454' ? Cl2 O01 3.2403(12) . '4 554' ? Cl2 H3aA 2.379(15) . '1 454' ? Cl2 H4aA 2.817(17) . '4 454' ? Cl2 H6aA 2.37(2) . '4 454' ? Cl2 H01B 2.51(2) . '4 554' ? Cl3 N6a 3.2427(12) . '4 454' ? Cl3 N6a 3.2786(11) . '2 546' ? Cl3 N3b 3.0857(12) . . ? Cl3 H6aB 2.777(16) . '2 546' ? Cl3 H6aB 2.444(15) . '4 454' ? Cl3 H3bA 2.23(2) . . ? C11 C12 2.5074(17) . . ? C11 C2a 2.526(2) . . ? C11 N3a 3.0905(17) . . ? C11 C2b 2.4731(17) . . ? C11 H12A 2.641(16) . . ? C11 H2aB 2.672(15) . . ? C11 H2bB 2.537(12) . . ? C12 C2a 2.5483(19) . . ? C12 N3a 2.9970(16) . . ? C12 C2b 2.5459(18) . . ? C12 N3b 2.9140(18) . . ? C12 H11B 2.700(17) . . ? C1 N3a 2.5378(15) . . ? C1 N3b 2.5561(14) . . ? C1 H11A 2.110(15) . . ? C1 H11B 2.069(19) . . ? C1 H11C 2.144(15) . . ? C1 H12A 2.037(17) . . ? C1 H12B 2.098(15) . . ? C1 H12c 2.094(16) . . ? C1 H2aA 2.086(16) . . ? C1 H2aB 2.087(14) . . ? C1 H2bA 2.098(14) . . ? C1 H2bB 2.077(13) . . ? C1 H3bB 2.615(13) . . ? C2a C4a 2.4759(16) . . ? C2a C2b 2.4735(16) . . ? C2a H12c 2.696(18) . . ? C2a H3aA 1.956(17) . . ? C2a H3aB 1.961(16) . . ? C2a H4aA 2.570(16) . . ? C2a H4aB 2.667(13) . . ? C2a H2bA 2.537(13) . . ? N3a C5a 2.5066(15) . . ? N3a O01 3.0324(14) . . ? N3a H12A 2.750(17) . . ? N3a H2aA 2.034(14) . . ? N3a H2aB 2.001(14) . . ? N3a H4aA 1.956(18) . . ? N3a H4aB 1.996(15) . . ? N3a H5aB 2.559(13) . . ? C4a N6a 2.4975(16) . . ? C4a H2aA 2.646(13) . . ? C4a H2aB 2.614(14) . . ? C4a H3aA 1.914(19) . . ? C4a H3aB 1.909(17) . . ? C4a H5aA 2.028(14) . . ? C4a H5aB 2.041(15) . . ? C4a H6aA 2.665(17) . . ? C4a H6aC 2.620(18) . . ? C5a H3aA 2.645(16) . . ? C5a H3aB 2.570(16) . . ? C5a H4aA 1.998(16) . . ? C5a H4aB 2.051(13) . . ? C5a H6aA 1.951(18) . . ? C5a H6aB 1.992(16) . . ? C5a H6aC 1.991(17) . . ? N6a O01 2.8626(14) . . ? N6a H4aA 2.533(16) . . ? N6a H5aA 1.979(15) . . ? N6a H5aB 2.036(14) . . ? C2b C4b 2.4957(16) . . ? C2b H11A 2.697(14) . . ? C2b H11B 2.662(18) . . ? C2b H12B 2.698(16) . . ? C2b H2aA 2.616(14) . . ? C2b H2aB 2.682(13) . . ? C2b H3bA 2.009(15) . . ? C2b H3bB 1.976(14) . . ? C2b H4bA 2.677(15) . . ? C2b H4bB 2.596(13) . . ? N3b C4b 2.4693(14) . '3 556' ? N3b H12c 2.702(18) . . ? N3b H2bA 2.014(12) . . ? N3b H2bB 1.998(13) . . ? N3b H4bA 2.697(12) . '3 556' ? N3b H4bA 1.996(16) . . ? N3b H4bB 1.977(14) . . ? N3b H4bB 2.671(14) . '3 556' ? C4b H2bA 2.528(12) . . ? C4b H3bA 2.521(18) . '3 556' ? C4b H3bA 1.947(19) . . ? C4b H3bB 1.963(15) . . ? C4b H3bB 2.640(13) . '3 556' ? C4b H4bA 2.088(13) . '3 556' ? C4b H4bB 2.048(13) . '3 556' ? O01 H3aB 2.415(14) . . ? O01 H6aC 2.090(17) . . ? H11A H11B 1.50(3) . . ? H11A H11C 1.53(2) . . ? H11B H11B 2.38(2) . '3 557' ? H11B H11C 1.55(2) . . ? H11B H2bB 2.38(2) . . ? H11C H3aA 2.35(2) . . ? H12A H12B 1.55(2) . . ? H12A H12c 1.51(2) . . ? H12A H3aB 2.33(2) . . ? H12B H12c 1.60(2) . . ? H2aA H2aB 1.572(18) . . ? H2aA H3aB 2.30(2) . . ? H2aA H4aA 2.40(2) . . ? H2aA H3bB 2.271(18) . . ? H2aB H3aA 2.25(2) . . ? H2aB H2bA 2.394(18) . . ? H3aA H3aB 1.33(2) . . ? H3aA H4aB 2.17(2) . . ? H3aB H4aA 2.22(3) . . ? H4aA H4aB 1.528(19) . . ? H4aB H5aA 2.221(19) . . ? H5aA H5aB 1.55(2) . . ? H5aA H6aA 2.18(2) . . ? H5aA H6aB 2.32(2) . . ? H5aB H6aB 2.25(2) . . ? H5aB H6aC 2.38(2) . . ? H6aA H6aB 1.50(3) . . ? H6aA H6aC 1.39(3) . . ? H6aB H6aC 1.42(2) . . ? H2bA H2bB 1.58(2) . . ? H2bA H3bB 2.367(18) . . ? H2bA H4bA 2.368(18) . . ? H2bB H3bA 2.20(2) . . ? H3bA H3bB 1.40(2) . . ? H3bA H4bB 2.25(2) . . ? H3bB H4bA 2.23(2) . . ? H4bA H4bB 2.379(18) . '3 556' ? H4bA H4bB 1.52(2) . . ? H01A H01B 1.20(3) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 612 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 9 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min -14 _reflns_limit_l_max 14 _reflns_number_observed ? _reflns_d_resolution_high .736 _reflns_d_resolution_low 9.455 _diffrn_reflns_av_sigmaI/netI .018 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 153 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970' _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .029 _refine_ls_wR_factor_all .038 _refine_ls_goodness_of_fit_all 1.427 _refine_ls_shift/su_mean .002 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_global _audit_creation_method Xtal3.6 _audit_creation_date 99-11-15 _audit_update_record ? #============================================================================== # (Publishing Staff Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia Nedlands Western Australia 6907 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal ? _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Skelton, Brian W.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; 'White, Allan H.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Pogram for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_n4ykcu # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C44 H112 Cl8 Cu4 N16 O26' _chemical_formula_moiety ? _chemical_formula_weight 1819.27 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M c_1_2/c_1 _symmetry_space_group_name_Hall -c_2yc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,+y,1/2-z -x,-y,-z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 42.632(3) _cell_length_b 9.9729(8) _cell_length_c 18.6590(10) _cell_angle_alpha 90.00000 _cell_angle_beta 101.3650(10) _cell_angle_gamma 90.00000 _cell_volume 7777.6(9) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 7309 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 1.434 _exptl_crystal_description block _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_size_rad ? _exptl_crystal_colour ? #<< use NfA code _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min 0.698 _exptl_absorpt_correction_T_max 0.914 _diffrn_reflns_number 34329 _reflns_number_total 9754 _reflns_Friedel_coverage 0 _reflns_number_gt 5964 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.2 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .0353 _diffrn_reflns_limit_h_min -57 _diffrn_reflns_limit_h_max 54 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .043 _refine_ls_wR_factor_ref .047 _refine_ls_goodness_of_fit_ref 1.397 _refine_ls_number_reflns 5964 _refine_ls_number_parameters 694 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .09 _refine_diff_density_min -.501 _refine_diff_density_max .651 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction xtal _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ 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 ? 0 176 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 464 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 32 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cu ? 0 16 .263 1.266 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 64 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 104 .008 .006 '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_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 .442472(10) .75175(4) .26973(2) .0409(2) Uani ? ? 1.00000 ? ? Cu2 .305232(9) .30995(4) .07886(2) .0380(2) Uani ? ? 1.00000 ? ? C11 .44459(8) 1.0138(4) .38874(18) .044(2) Uani ? ? 1.00000 ? ? C111 .45805(15) 1.1342(6) .4362(3) .066(3) Uani ? ? 1.00000 ? ? C12 .46576(10) .8946(4) .4156(2) .049(2) Uani ? ? 1.00000 ? ? N13 .45587(8) .7621(3) .38216(16) .0428(17) Uani ? ? 1.00000 ? ? C14 .48012(11) .6626(4) .4172(3) .058(3) Uani ? ? 1.00000 ? ? C15 .47137(14) .5190(5) .3988(3) .065(3) Uani ? ? 1.00000 ? ? C16 .47302(13) .4813(5) .3232(3) .064(3) Uani ? ? 1.00000 ? ? N17 .44798(10) .5507(4) .2699(2) .058(2) Uani ? ? 1.00000 ? ? C111' .40997(11) .9911(6) .3959(3) .060(3) Uani ? ? 1.00000 ? ? C12' .44738(10) 1.0477(4) .3112(2) .048(2) Uani ? ? 1.00000 ? ? N13' .43154(8) .9530(3) .25485(15) .0436(18) Uani ? ? 1.00000 ? ? C14' .43611(12) 1.0054(5) .1829(2) .061(3) Uani ? ? 1.00000 ? ? C15' .41419(13) .9439(6) .1183(2) .074(3) Uani ? ? 1.00000 ? ? C16' .41965(12) .7997(6) .1075(2) .068(3) Uani ? ? 1.00000 ? ? N17' .41234(11) .7221(5) .1700(2) .065(3) Uani ? ? 1.00000 ? ? C21 .30744(9) .6121(4) -.0055(2) .049(2) Uani ? ? 1.00000 ? ? C211 .29523(14) .7270(5) -.0598(3) .071(3) Uani ? ? 1.00000 ? ? C22 .30805(11) .4876(4) -.0522(2) .050(2) Uani ? ? 1.00000 ? ? N23 .32210(7) .3668(3) -.01292(16) .0408(16) Uani ? ? 1.00000 ? ? C24 .32035(10) .2569(4) -.0687(2) .052(2) Uani ? ? 1.00000 ? ? C25 .34170(11) .1384(5) -.0423(3) .061(3) Uani ? ? 1.00000 ? ? C26 .33301(12) .0672(5) .0211(3) .060(3) Uani ? ? 1.00000 ? ? N27 .33735(10) .1543(4) .0860(2) .054(2) Uani ? ? 1.00000 ? ? C211' .34098(12) .6457(6) .0360(4) .069(3) Uani ? ? 1.00000 ? ? C22' .28351(10) .5967(4) .0438(2) .050(2) Uani ? ? 1.00000 ? ? N23' .29160(7) .4990(3) .10492(17) .0424(17) Uani ? ? 1.00000 ? ? C24' .26530(10) .5046(5) .1474(2) .055(3) Uani ? ? 1.00000 ? ? C25' .27205(13) .4276(5) .2171(3) .063(3) Uani ? ? 1.00000 ? ? C26' .26865(11) .2795(5) .2063(3) .062(3) Uani ? ? 1.00000 ? ? N27' .29322(9) .2253(4) .1690(2) .050(2) Uani ? ? 1.00000 ? ? Cl1 .50000 .79115(14) .25000 .0529(7) Uani ? ? 1.00000 ? ? Cl2 .25000 .25000 .00000 .0497(7) Uani ? ? 1.00000 ? ? Cl3 .68082(3) .86589(11) .28638(6) .0642(6) Uani ? ? 1.00000 ? ? O31 .65084(10) .9080(5) .2957(3) .130(3) Uani ? ? 1.00000 ? ? O32 .68234(13) .7280(4) .2764(2) .142(3) Uani ? ? 1.00000 ? ? O33 .68820(10) .9328(5) .2256(2) .122(3) Uani ? ? 1.00000 ? ? O34 .70351(10) .9053(4) .34933(19) .107(3) Uani ? ? 1.00000 ? ? Cl4 .57723(3) .37671(13) .43612(7) .0718(7) Uani ? ? 1.00000 ? ? O41 .60276(12) .3541(7) .4051(3) .187(5) Uani ? ? 1.00000 ? ? O42 .55858(13) .4766(6) .4047(4) .137(5) Uani ? ? .791(11) ? ? O43 .5587(3) .2643(8) .4412(6) .186(8) Uani ? ? .791(11) ? ? O44 .5924(2) .4203(11) .5090(3) .201(7) Uani ? ? .791(11) ? ? O42' .5574(6) .357(3) .3631(14) .132(11) Uiso ? ? .209(11) ? ? O43' .5721(6) .288(3) .4781(14) .096(8) Uiso ? ? .209(11) ? ? O44' .5707(7) .491(3) .463(2) .145(11) Uiso ? ? .209(11) ? ? Cl5 .62939(3) .33212(14) .22475(7) .0761(8) Uani ? ? 1.00000 ? ? O51 .64006(10) .4296(4) .2802(2) .125(3) Uani ? ? 1.00000 ? ? O52 .62679(14) .2055(5) .2596(3) .129(4) Uani ? ? .813(10) ? ? O53 .65194(17) .3246(12) .1821(4) .174(7) Uani ? ? .813(10) ? ? O54 .59994(13) .3622(6) .1800(4) .109(4) Uani ? ? .813(10) ? ? O52' .5981(7) .330(3) .2143(13) .080(8) Uiso ? ? .187(10) ? ? O53' .6505(5) .246(2) .2093(12) .079(7) Uiso ? ? .187(10) ? ? O54' .6302(11) .422(4) .160(2) .197(17) Uiso ? ? .187(10) ? ? O01 .38465(9) .6725(4) .3276(3) .130(3) Uani ? ? 1.00000 ? ? H111a .4466(12) 1.206(5) .424(3) .09(2) Uiso ? ? 1.00000 ? ? H111b .4775(9) 1.154(3) .4268(18) .034(10) Uiso ? ? 1.00000 ? ? H111c .4617(9) 1.107(4) .489(2) .061(12) Uiso ? ? 1.00000 ? ? H12a .4680(8) .883(4) .464(2) .050(11) Uiso ? ? 1.00000 ? ? H12b .4885(8) .908(3) .4065(17) .044(10) Uiso ? ? 1.00000 ? ? H13a .4401(8) .743(3) .3957(18) .034(10) Uiso ? ? 1.00000 ? ? H14a .4814(9) .680(4) .467(2) .062(12) Uiso ? ? 1.00000 ? ? H14b .4986(9) .685(4) .401(2) .054(12) Uiso ? ? 1.00000 ? ? H15a .4504(9) .498(4) .413(2) .055(12) Uiso ? ? 1.00000 ? ? H15b .4847(9) .478(4) .427(2) .059(13) Uiso ? ? 1.00000 ? ? H16a .4727(9) .394(4) .314(2) .055(12) Uiso ? ? 1.00000 ? ? H16b .4931(10) .501(4) .313(2) .069(14) Uiso ? ? 1.00000 ? ? H17a .4308(9) .522(4) .276(2) .048(13) Uiso ? ? 1.00000 ? ? H17b .4494(11) .525(5) .233(3) .073(19) Uiso ? ? 1.00000 ? ? H111'a .4112(10) .976(4) .444(3) .079(15) Uiso ? ? 1.00000 ? ? H111'b .3998(9) .910(4) .366(2) .058(11) Uiso ? ? 1.00000 ? ? H111'c .3972(11) 1.059(5) .383(2) .085(18) Uiso ? ? 1.00000 ? ? H12'a .4708(9) 1.056(4) .3055(19) .058(11) Uiso ? ? 1.00000 ? ? H12'b .4369(9) 1.133(4) .299(2) .066(12) Uiso ? ? 1.00000 ? ? H13'b .4136(7) .953(3) .2545(16) .027(10) Uiso ? ? 1.00000 ? ? H14'a .4592(9) .981(4) .179(2) .060(12) Uiso ? ? 1.00000 ? ? H14'b .4308(8) 1.089(4) .1816(18) .041(11) Uiso ? ? 1.00000 ? ? H15'a .4209(9) .986(4) .078(2) .069(13) Uiso ? ? 1.00000 ? ? H15'b .3923(10) .960(4) .121(2) .078(14) Uiso ? ? 1.00000 ? ? H16'a .4421(11) .792(4) .102(2) .070(13) Uiso ? ? 1.00000 ? ? H16'b .4085(10) .767(4) .059(2) .074(13) Uiso ? ? 1.00000 ? ? H17'a .4129(11) .635(5) .158(2) .078(17) Uiso ? ? 1.00000 ? ? H17'b .3957(14) .732(6) .184(3) .11(3) Uiso ? ? 1.00000 ? ? H211a .2917(11) .808(5) -.033(3) .091(16) Uiso ? ? 1.00000 ? ? H211b .3121(14) .732(5) -.091(3) .13(2) Uiso ? ? 1.00000 ? ? H211c .2716(11) .702(4) -.088(2) .078(14) Uiso ? ? 1.00000 ? ? H211'a .3585(11) .656(4) -.000(2) .084(14) Uiso ? ? 1.00000 ? ? H211'b .3406(10) .715(5) .062(3) .072(16) Uiso ? ? 1.00000 ? ? H211'c .3510(10) .583(4) .067(2) .066(14) Uiso ? ? 1.00000 ? ? H22a .2872(9) .463(4) -.0711(18) .049(11) Uiso ? ? 1.00000 ? ? H22b .3203(7) .513(3) -.0894(18) .040(9) Uiso ? ? 1.00000 ? ? H23b .3408(9) .379(4) .003(2) .046(11) Uiso ? ? 1.00000 ? ? H24a .2977(9) .222(3) -.077(2) .052(11) Uiso ? ? 1.00000 ? ? H24b .3285(11) .298(4) -.117(3) .089(14) Uiso ? ? 1.00000 ? ? H25a .3386(9) .076(4) -.084(2) .072(13) Uiso ? ? 1.00000 ? ? H25b .3624(11) .170(4) -.036(2) .073(14) Uiso ? ? 1.00000 ? ? H26a .3096(9) .036(4) .012(2) .061(12) Uiso ? ? 1.00000 ? ? H26b .3447(8) -.002(4) .0339(17) .040(10) Uiso ? ? 1.00000 ? ? H27a .3333(11) .107(5) .128(3) .097(18) Uiso ? ? 1.00000 ? ? H27b .3536(8) .184(4) .0887(19) .031(11) Uiso ? ? 1.00000 ? ? H22'a .2801(9) .677(4) .062(2) .058(12) Uiso ? ? 1.00000 ? ? H22'b .2621(10) .566(4) .013(2) .074(13) Uiso ? ? 1.00000 ? ? H23'a .3055(8) .522(3) .1321(18) .033(10) Uiso ? ? 1.00000 ? ? H24'a .2637(9) .603(4) .152(2) .069(13) Uiso ? ? 1.00000 ? ? H24'b .2471(9) .469(4) .111(2) .057(11) Uiso ? ? 1.00000 ? ? H25'a .2951(10) .448(4) .245(2) .073(13) Uiso ? ? 1.00000 ? ? H25'b .2593(9) .452(4) .238(2) .061(14) Uiso ? ? 1.00000 ? ? H26'a .2726(9) .236(4) .251(2) .065(13) Uiso ? ? 1.00000 ? ? H26'b .2489(11) .260(4) .174(2) .075(14) Uiso ? ? 1.00000 ? ? H27'a .3095(10) .224(4) .195(2) .044(12) Uiso ? ? 1.00000 ? ? H27'b .2890(8) .143(4) .154(2) .049(12) Uiso ? ? 1.00000 ? ? 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 .0354(2) .0497(3) .0354(2) -.0018(2) .00156(17) .0028(2) Cu2 .0342(2) .0380(2) .0408(2) .00293(19) .00477(17) -.0008(2) C11 .046(2) .049(2) .037(2) -.0049(17) .0055(16) -.0002(17) C111 .072(4) .060(3) .064(3) -.010(3) .008(3) -.011(3) C12 .050(3) .056(3) .038(2) -.0109(19) -.0024(18) .0038(18) N13 .0370(18) .049(2) .0405(17) -.0022(14) .0036(14) .0060(14) C14 .060(3) .058(3) .049(3) .004(2) -.006(2) .012(2) C15 .075(4) .053(3) .062(3) .008(2) .003(3) .020(2) C16 .072(3) .049(3) .070(3) .009(2) .013(3) .006(2) N17 .056(3) .061(3) .057(3) -.007(2) .008(2) .000(2) C111' .053(3) .077(4) .052(3) -.005(3) .020(2) -.006(3) C12' .048(2) .047(3) .048(2) .0003(19) .0092(18) .0064(19) N13' .039(2) .056(2) .0358(17) .0050(15) .0074(14) .0065(14) C14' .078(3) .060(3) .045(2) .015(3) .014(2) .017(2) C15' .072(3) .112(5) .037(2) .024(3) .008(2) .019(3) C16' .056(3) .107(4) .037(2) .000(3) .001(2) -.009(2) N17' .062(3) .078(3) .048(2) -.005(2) -.0067(19) -.003(2) C21 .050(2) .036(2) .059(2) .0013(17) .0064(19) .0050(18) C211 .076(4) .050(3) .089(4) .006(2) .024(3) .018(3) C22 .050(3) .051(3) .051(2) .000(2) .013(2) .007(2) N23 .0308(17) .0439(18) .0481(18) -.0012(14) .0084(14) -.0026(14) C24 .049(2) .057(3) .051(2) .004(2) .0124(19) -.010(2) C25 .049(3) .062(3) .069(3) .013(2) .011(2) -.022(2) C26 .060(3) .041(3) .074(3) .016(2) .002(2) -.004(2) N27 .048(2) .052(2) .060(2) .0112(18) .0057(19) .0045(18) C211' .050(3) .057(3) .097(4) -.009(2) .007(3) -.009(3) C22' .049(2) .039(2) .060(3) .0072(19) .006(2) .000(2) N23' .0354(18) .046(2) .0437(18) -.0005(14) .0015(15) -.0080(15) C24' .051(3) .059(3) .057(3) .009(2) .017(2) -.006(2) C25' .061(3) .078(4) .055(3) .008(3) .025(2) -.009(2) C26' .050(3) .084(4) .055(3) -.000(2) .014(2) .009(2) N27' .046(2) .055(3) .045(2) .0004(17) .0011(16) .0025(17) Cl1 .0340(7) .0581(9) .0701(9) .00000 .0188(6) .00000 Cl2 .0314(6) .0668(9) .0481(7) -.0106(6) .0014(5) -.0094(7) Cl3 .0866(8) .0512(7) .0534(6) .0073(6) .0104(6) -.0025(5) O31 .097(3) .142(4) .162(4) .026(3) .050(3) -.015(3) O32 .211(5) .059(3) .127(4) .027(3) -.037(3) -.022(2) O33 .148(4) .146(4) .079(3) -.010(3) .038(2) .015(3) O34 .143(3) .080(3) .081(2) -.010(2) -.018(2) -.006(2) Cl4 .0788(8) .0715(8) .0725(8) .0114(7) .0327(7) .0176(7) O41 .112(4) .274(8) .196(5) .041(4) .085(4) -.012(5) O42 .129(5) .113(5) .153(7) .050(4) -.010(4) .059(5) O43 .260(11) .115(6) .216(11) -.081(6) .123(9) -.008(6) O44 .216(8) .296(11) .071(4) .049(8) -.020(4) -.044(5) Cl5 .0503(7) .0874(10) .0855(8) .0077(6) .0012(6) .0003(7) O51 .128(3) .102(3) .138(4) -.046(3) .005(3) -.035(3) O52 .177(6) .074(4) .106(4) -.020(3) -.040(4) .039(3) O53 .131(6) .286(12) .128(6) -.011(7) .084(5) -.000(6) O54 .076(4) .103(4) .129(5) .025(3) -.028(4) .013(4) O01 .078(2) .106(3) .205(5) -.011(2) .024(3) -.046(3) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Cu1 N13 . . 2.065(3) ? Cu1 N17 . . 2.018(4) ? Cu1 N13' . . 2.067(3) ? Cu1 N17' . . 2.064(4) ? Cu1 Cl1 . . 2.5808(5) ? Cu1 O01 . . 2.986(5) ? Cu2 N23 . . 2.063(3) ? Cu2 N27 . . 2.057(4) ? Cu2 N23' . . 2.060(3) ? Cu2 N27' . . 2.036(4) ? Cu2 Cl2 . . 2.5887(4) ? C11 C111 . . 1.535(6) ? C11 C12 . . 1.517(5) ? C11 C111' . . 1.525(6) ? C11 C12' . . 1.514(5) ? C111 H111a . . .88(5) ? C111 H111b . . .90(4) ? C111 H111c . . 1.01(4) ? C12 N13 . . 1.486(5) ? C12 H12a . . .91(4) ? C12 H12b . . 1.03(4) ? N13 C14 . . 1.488(5) ? N13 H13a . . .79(4) ? C14 C15 . . 1.502(6) ? C14 H14a . . .94(4) ? C14 H14b . . .93(4) ? C15 C16 . . 1.474(7) ? C15 H15a . . 1.01(4) ? C15 H15b . . .81(4) ? C16 N17 . . 1.480(6) ? C16 H16a . . .88(4) ? C16 H16b . . .93(4) ? N17 H17a . . .82(4) ? N17 H17b . . .75(5) ? C111' H111'a . . .89(5) ? C111' H111'b . . 1.03(4) ? C111' H111'c . . .87(5) ? C12' N13' . . 1.474(5) ? C12' H12'a . . 1.03(4) ? C12' H12'b . . .97(4) ? N13' C14' . . 1.489(6) ? N13' H13'b . . .76(3) ? C14' C15' . . 1.502(6) ? C14' H14'a . . 1.03(4) ? C14' H14'b . . .87(4) ? C15' C16' . . 1.477(8) ? C15' H15'a . . .96(4) ? C15' H15'b . . .96(5) ? C16' N17' . . 1.482(7) ? C16' H16'a . . .98(5) ? C16' H16'b . . .99(4) ? N17' H17'a . . .90(5) ? N17' H17'b . . .81(6) ? C21 C211 . . 1.550(6) ? C21 C22 . . 1.520(6) ? C21 C211' . . 1.523(6) ? C21 C22' . . 1.510(6) ? C211 H211a . . .97(5) ? C211 H211b . . 1.02(7) ? C211 H211c . . 1.07(4) ? C22 N23 . . 1.474(5) ? C22 H22a . . .92(4) ? C22 H22b . . .98(4) ? N23 C24 . . 1.503(5) ? N23 H23b . . .80(4) ? C24 C25 . . 1.513(6) ? C24 H24a . . 1.01(4) ? C24 H24b . . 1.11(5) ? C25 C26 . . 1.489(7) ? C25 H25a . . .99(4) ? C25 H25b . . .92(5) ? C26 N27 . . 1.471(6) ? C26 H26a . . 1.03(4) ? C26 H26b . . .85(3) ? N27 H27a . . .96(5) ? N27 H27b . . .75(4) ? C211' H211'a . . 1.10(5) ? C211' H211'b . . .84(5) ? C211' H211'c . . .91(4) ? C22' N23' . . 1.488(5) ? C22' H22'a . . .89(4) ? C22' H22'b . . 1.02(4) ? N23' C24' . . 1.496(6) ? N23' H23'a . . .74(3) ? C24' C25' . . 1.489(7) ? C24' H24'a . . .99(4) ? C24' H24'b . . .99(3) ? C25' C26' . . 1.493(7) ? C25' H25'a . . 1.04(4) ? C25' H25'b . . .76(4) ? C26' N27' . . 1.471(7) ? C26' H26'a . . .92(4) ? C26' H26'b . . .96(4) ? N27' H27'a . . .76(4) ? N27' H27'b . . .87(4) ? Cl3 O31 . . 1.388(5) ? Cl3 O32 . . 1.391(4) ? Cl3 O33 . . 1.405(4) ? Cl3 O34 . . 1.422(4) ? Cl4 O41 . . 1.348(6) ? Cl4 O42 . . 1.336(6) ? Cl4 O43 . . 1.385(9) ? Cl4 O44 . . 1.452(7) ? Cl4 O42' . . 1.47(2) ? Cl4 O43' . . 1.23(3) ? Cl4 O44' . . 1.30(3) ? O41 O44 . . 2.174(10) ? O41 O42' . . 1.94(2) ? O41 O43' . . 2.17(3) ? O42 O42' . . 1.42(3) ? O42 O44' . . 1.12(3) ? O43 O42' . . 1.72(3) ? O43 O43' . . .84(3) ? O44 O43' . . 1.62(3) ? O44 O44' . . 1.33(3) ? O43' O44' . . 2.04(4) ? Cl5 O51 . . 1.428(4) ? Cl5 O52 . . 1.435(5) ? Cl5 O53 . . 1.366(8) ? Cl5 O54 . . 1.396(6) ? Cl5 O52' . . 1.31(3) ? Cl5 O53' . . 1.32(2) ? Cl5 O54' . . 1.51(4) ? O51 O52' . . 2.20(3) ? O52 O52' . . 1.83(3) ? O52 O53' . . 1.56(3) ? O53 O53' . . .95(2) ? O53 O54' . . 1.35(4) ? O54 O52' . . .74(3) ? O54 O54' . . 1.53(5) ? O52' O54' . . 2.07(5) ? O53' O54' . . 2.09(5) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published N13 Cu1 N17 . . . 92.26(15) ? N13 Cu1 N13' . . . 95.61(12) ? N13 Cu1 N17' . . . 157.16(17) ? N13 Cu1 Cl1 . . . 93.26(9) ? N13 Cu1 O01 . . . 74.26(13) ? N17 Cu1 N13' . . . 171.06(14) ? N17 Cu1 N17' . . . 84.89(18) ? N17 Cu1 Cl1 . . . 92.17(13) ? N17 Cu1 O01 . . . 80.83(16) ? N13' Cu1 N17' . . . 86.22(16) ? N13' Cu1 Cl1 . . . 91.63(10) ? N13' Cu1 O01 . . . 97.20(13) ? N17' Cu1 Cl1 . . . 109.47(14) ? N17' Cu1 O01 . . . 82.92(16) ? Cl1 Cu1 O01 . . . 165.31(9) ? N23 Cu2 N27 . . . 85.66(15) ? N23 Cu2 N23' . . . 96.03(13) ? N23 Cu2 N27' . . . 170.21(14) ? N23 Cu2 Cl2 . . . 91.06(8) ? N27 Cu2 N23' . . . 153.00(13) ? N27 Cu2 N27' . . . 84.63(16) ? N27 Cu2 Cl2 . . . 112.45(11) ? N23' Cu2 N27' . . . 93.22(14) ? N23' Cu2 Cl2 . . . 94.49(8) ? N27' Cu2 Cl2 . . . 91.44(10) ? C111 C11 C12 . . . 107.0(3) ? C111 C11 C111' . . . 108.9(4) ? C111 C11 C12' . . . 106.6(4) ? C12 C11 C111' . . . 112.2(4) ? C12 C11 C12' . . . 109.7(3) ? C111' C11 C12' . . . 112.1(3) ? C11 C111 H111a . . . 112(3) ? C11 C111 H111b . . . 108(2) ? C11 C111 H111c . . . 109(2) ? H111a C111 H111b . . . 105(4) ? H111a C111 H111c . . . 116(4) ? H111b C111 H111c . . . 106(3) ? C11 C12 N13 . . . 117.2(3) ? C11 C12 H12a . . . 112(2) ? C11 C12 H12b . . . 111.3(18) ? N13 C12 H12a . . . 106(2) ? N13 C12 H12b . . . 104.3(18) ? H12a C12 H12b . . . 106(3) ? Cu1 N13 C12 . . . 118.0(2) ? Cu1 N13 C14 . . . 116.2(3) ? Cu1 N13 H13a . . . 103(2) ? C12 N13 C14 . . . 107.1(3) ? C12 N13 H13a . . . 105(2) ? C14 N13 H13a . . . 105(2) ? N13 C14 C15 . . . 114.6(4) ? N13 C14 H14a . . . 102(2) ? N13 C14 H14b . . . 105(2) ? C15 C14 H14a . . . 111(2) ? C15 C14 H14b . . . 110(2) ? H14a C14 H14b . . . 113(3) ? C14 C15 C16 . . . 113.9(4) ? C14 C15 H15a . . . 110(2) ? C14 C15 H15b . . . 103(3) ? C16 C15 H15a . . . 114(2) ? C16 C15 H15b . . . 110(3) ? H15a C15 H15b . . . 105(4) ? C15 C16 N17 . . . 111.1(4) ? C15 C16 H16a . . . 116(3) ? C15 C16 H16b . . . 112(2) ? N17 C16 H16a . . . 110(2) ? N17 C16 H16b . . . 109(2) ? H16a C16 H16b . . . 98(4) ? Cu1 N17 C16 . . . 122.3(3) ? Cu1 N17 H17a . . . 104(3) ? Cu1 N17 H17b . . . 112(4) ? C16 N17 H17a . . . 107(3) ? C16 N17 H17b . . . 106(3) ? H17a N17 H17b . . . 104(4) ? C11 C111' H111'a . . . 104(3) ? C11 C111' H111'b . . . 112(2) ? C11 C111' H111'c . . . 115(3) ? H111'a C111' H111'b . . . 110(4) ? H111'a C111' H111'c . . . 108(4) ? H111'b C111' H111'c . . . 107(4) ? C11 C12' N13' . . . 115.3(3) ? C11 C12' H12'a . . . 112(2) ? C11 C12' H12'b . . . 108(3) ? N13' C12' H12'a . . . 107(2) ? N13' C12' H12'b . . . 106(2) ? H12'a C12' H12'b . . . 109(3) ? Cu1 N13' C12' . . . 117.8(2) ? Cu1 N13' C14' . . . 113.3(3) ? Cu1 N13' H13'b . . . 101(2) ? C12' N13' C14' . . . 107.2(3) ? C12' N13' H13'b . . . 109(2) ? C14' N13' H13'b . . . 108(2) ? N13' C14' C15' . . . 114.2(4) ? N13' C14' H14'a . . . 106(2) ? N13' C14' H14'b . . . 106(2) ? C15' C14' H14'a . . . 107(2) ? C15' C14' H14'b . . . 105(2) ? H14'a C14' H14'b . . . 118(3) ? C14' C15' C16' . . . 114.6(4) ? C14' C15' H15'a . . . 103(2) ? C14' C15' H15'b . . . 110(2) ? C16' C15' H15'a . . . 104(3) ? C16' C15' H15'b . . . 111(3) ? H15'a C15' H15'b . . . 115(3) ? C15' C16' N17' . . . 109.8(4) ? C15' C16' H16'a . . . 106(2) ? C15' C16' H16'b . . . 113(2) ? N17' C16' H16'a . . . 114(2) ? N17' C16' H16'b . . . 114(3) ? H16'a C16' H16'b . . . 100(4) ? Cu1 N17' C16' . . . 116.4(3) ? Cu1 N17' H17'a . . . 109(3) ? Cu1 N17' H17'b . . . 97(4) ? C16' N17' H17'a . . . 107(3) ? C16' N17' H17'b . . . 121(4) ? H17'a N17' H17'b . . . 106(5) ? C211 C21 C22 . . . 105.7(3) ? C211 C21 C211' . . . 109.3(4) ? C211 C21 C22' . . . 107.1(4) ? C22 C21 C211' . . . 110.5(4) ? C22 C21 C22' . . . 110.8(3) ? C211' C21 C22' . . . 113.1(4) ? C21 C211 H211a . . . 110(3) ? C21 C211 H211b . . . 103(3) ? C21 C211 H211c . . . 108(2) ? H211a C211 H211b . . . 117(4) ? H211a C211 H211c . . . 103(4) ? H211b C211 H211c . . . 115(4) ? C21 C22 N23 . . . 115.7(3) ? C21 C22 H22a . . . 108(2) ? C21 C22 H22b . . . 105.3(19) ? N23 C22 H22a . . . 104(2) ? N23 C22 H22b . . . 110.2(19) ? H22a C22 H22b . . . 114(3) ? Cu2 N23 C22 . . . 117.6(3) ? Cu2 N23 C24 . . . 113.3(2) ? Cu2 N23 H23b . . . 103(3) ? C22 N23 C24 . . . 107.0(3) ? C22 N23 H23b . . . 110(3) ? C24 N23 H23b . . . 106(3) ? N23 C24 C25 . . . 113.6(3) ? N23 C24 H24a . . . 106(2) ? N23 C24 H24b . . . 109(2) ? C25 C24 H24a . . . 106(2) ? C25 C24 H24b . . . 107(2) ? H24a C24 H24b . . . 116(3) ? C24 C25 C26 . . . 113.8(4) ? C24 C25 H25a . . . 105(2) ? C24 C25 H25b . . . 106(3) ? C26 C25 H25a . . . 108(3) ? C26 C25 H25b . . . 116(3) ? H25a C25 H25b . . . 107(4) ? C25 C26 N27 . . . 111.2(4) ? C25 C26 H26a . . . 113(2) ? C25 C26 H26b . . . 113(2) ? N27 C26 H26a . . . 106(2) ? N27 C26 H26b . . . 106(2) ? H26a C26 H26b . . . 107(3) ? Cu2 N27 C26 . . . 114.8(3) ? Cu2 N27 H27a . . . 102(3) ? Cu2 N27 H27b . . . 108(3) ? C26 N27 H27a . . . 111(3) ? C26 N27 H27b . . . 105(3) ? H27a N27 H27b . . . 117(4) ? C21 C211' H211'a . . . 113(2) ? C21 C211' H211'b . . . 110(3) ? C21 C211' H211'c . . . 117(3) ? H211'a C211' H211'b . . . 111(4) ? H211'a C211' H211'c . . . 99(4) ? H211'b C211' H211'c . . . 105(4) ? C21 C22' N23' . . . 116.8(3) ? C21 C22' H22'a . . . 108(3) ? C21 C22' H22'b . . . 109(2) ? N23' C22' H22'a . . . 109(2) ? N23' C22' H22'b . . . 106(2) ? H22'a C22' H22'b . . . 107(3) ? Cu2 N23' C22' . . . 116.9(3) ? Cu2 N23' C24' . . . 115.8(3) ? Cu2 N23' H23'a . . . 103(3) ? C22' N23' C24' . . . 107.3(3) ? C22' N23' H23'a . . . 111(3) ? C24' N23' H23'a . . . 102(3) ? N23' C24' C25' . . . 114.0(4) ? N23' C24' H24'a . . . 99(2) ? N23' C24' H24'b . . . 101(2) ? C25' C24' H24'a . . . 116(2) ? C25' C24' H24'b . . . 114(2) ? H24'a C24' H24'b . . . 111(3) ? C24' C25' C26' . . . 113.3(4) ? C24' C25' H25'a . . . 110(2) ? C24' C25' H25'b . . . 104(3) ? C26' C25' H25'a . . . 109(2) ? C26' C25' H25'b . . . 109(3) ? H25'a C25' H25'b . . . 112(4) ? C25' C26' N27' . . . 111.6(4) ? C25' C26' H26'a . . . 111(3) ? C25' C26' H26'b . . . 110(3) ? N27' C26' H26'a . . . 103(3) ? N27' C26' H26'b . . . 104(3) ? H26'a C26' H26'b . . . 117(4) ? Cu2 N27' C26' . . . 123.9(3) ? Cu2 N27' H27'a . . . 101(3) ? Cu2 N27' H27'b . . . 101(3) ? C26' N27' H27'a . . . 110(3) ? C26' N27' H27'b . . . 112(3) ? H27'a N27' H27'b . . . 107(4) ? Cu1 Cl1 Cu1 . . '2 655' 162.49(6) ? Cu2 Cl2 Cu2 . . 7 180.0000 ? O31 Cl3 O32 . . . 112.6(3) ? O31 Cl3 O33 . . . 108.4(3) ? O31 Cl3 O34 . . . 107.9(3) ? O32 Cl3 O33 . . . 109.8(3) ? O32 Cl3 O34 . . . 110.0(2) ? O33 Cl3 O34 . . . 108.2(2) ? O41 Cl4 O42 . . . 113.4(4) ? O41 Cl4 O43 . . . 114.4(6) ? O41 Cl4 O44 . . . 101.8(4) ? O41 Cl4 O42' . . . 86.8(11) ? O41 Cl4 O43' . . . 114.4(13) ? O41 Cl4 O44' . . . 124.5(15) ? O42 Cl4 O43 . . . 109.6(5) ? O42 Cl4 O44 . . . 107.7(5) ? O42 Cl4 O42' . . . 60.7(11) ? O42 Cl4 O43' . . . 130.6(12) ? O42 Cl4 O44' . . . 50.5(14) ? O43 Cl4 O44 . . . 109.4(6) ? O43 Cl4 O42' . . . 73.9(12) ? O43 Cl4 O43' . . . 36.7(12) ? O43 Cl4 O44' . . . 121.0(16) ? O44 Cl4 O42' . . . 167.9(11) ? O44 Cl4 O43' . . . 73.9(12) ? O44 Cl4 O44' . . . 57.4(14) ? O42' Cl4 O43' . . . 110.6(15) ? O42' Cl4 O44' . . . 110.7(17) ? O43' Cl4 O44' . . . 108(2) ? Cl4 O41 O44 . . . 40.8(3) ? Cl4 O41 O42' . . . 49.2(8) ? Cl4 O41 O43' . . . 31.2(7) ? O44 O41 O42' . . . 89.7(9) ? O44 O41 O43' . . . 43.9(8) ? O42' O41 O43' . . . 65.3(10) ? Cl4 O42 O42' . . . 64.2(10) ? Cl4 O42 O44' . . . 63.1(16) ? O42' O42 O44' . . . 126.8(19) ? Cl4 O43 O42' . . . 55.2(9) ? Cl4 O43 O43' . . . 62(2) ? O42' O43 O43' . . . 117(2) ? Cl4 O44 O41 . . . 37.4(2) ? Cl4 O44 O43' . . . 46.8(10) ? Cl4 O44 O44' . . . 55.5(14) ? O41 O44 O43' . . . 67.9(10) ? O41 O44 O44' . . . 80.1(16) ? O43' O44 O44' . . . 87.2(16) ? Cl4 O42' O41 . . . 44.0(6) ? Cl4 O42' O42 . . . 55.1(10) ? Cl4 O42' O43 . . . 50.8(9) ? O41 O42' O42 . . . 82.3(11) ? O41 O42' O43 . . . 77.7(10) ? O42 O42' O43 . . . 89.8(14) ? Cl4 O43' O41 . . . 34.5(8) ? Cl4 O43' O43 . . . 82(2) ? Cl4 O43' O44 . . . 59.3(12) ? Cl4 O43' O44' . . . 37.3(13) ? O41 O43' O43 . . . 88(2) ? O41 O43' O44 . . . 68.2(10) ? O41 O43' O44' . . . 67.5(14) ? O43 O43' O44 . . . 139(3) ? O43 O43' O44' . . . 100(2) ? O44 O43' O44' . . . 40.4(11) ? Cl4 O44' O42 . . . 66.4(18) ? Cl4 O44' O44 . . . 67.1(15) ? Cl4 O44' O43' . . . 35.0(11) ? O42 O44' O44 . . . 133(3) ? O42 O44' O43' . . . 90(2) ? O44 O44' O43' . . . 52.4(13) ? O51 Cl5 O52 . . . 108.2(3) ? O51 Cl5 O53 . . . 107.5(4) ? O51 Cl5 O54 . . . 114.1(3) ? O51 Cl5 O52' . . . 106.8(12) ? O51 Cl5 O53' . . . 118.1(9) ? O51 Cl5 O54' . . . 97.1(15) ? O52 Cl5 O53 . . . 110.0(5) ? O52 Cl5 O54 . . . 108.6(3) ? O52 Cl5 O52' . . . 83.3(12) ? O52 Cl5 O53' . . . 68.9(10) ? O52 Cl5 O54' . . . 154.2(16) ? O53 Cl5 O54 . . . 108.5(4) ? O53 Cl5 O52' . . . 136.5(11) ? O53 Cl5 O53' . . . 41.2(11) ? O53 Cl5 O54' . . . 55.6(18) ? O54 Cl5 O52' . . . 31.3(12) ? O54 Cl5 O53' . . . 125.5(10) ? O54 Cl5 O54' . . . 63.5(17) ? O52' Cl5 O53' . . . 132.4(15) ? O52' Cl5 O54' . . . 94(2) ? O53' Cl5 O54' . . . 95(2) ? Cl5 O51 O52' . . . 34.8(8) ? Cl5 O52 O52' . . . 45.4(9) ? Cl5 O52 O53' . . . 52.0(8) ? O52' O52 O53' . . . 90.1(12) ? Cl5 O53 O53' . . . 66.7(16) ? Cl5 O53 O54' . . . 68(2) ? O53' O53 O54' . . . 130(3) ? Cl5 O54 O52' . . . 68(2) ? Cl5 O54 O54' . . . 61.8(14) ? O52' O54 O54' . . . 128(3) ? Cl5 O52' O51 . . . 38.4(7) ? Cl5 O52' O52 . . . 51.3(9) ? Cl5 O52' O54 . . . 81(2) ? Cl5 O52' O54' . . . 46.6(14) ? O51 O52' O52 . . . 69.6(8) ? O51 O52' O54 . . . 94(2) ? O51 O52' O54' . . . 62.0(13) ? O52 O52' O54 . . . 122(3) ? O52 O52' O54' . . . 94.6(17) ? O54 O52' O54' . . . 35(2) ? Cl5 O53' O52 . . . 59.1(10) ? Cl5 O53' O53 . . . 72.1(15) ? Cl5 O53' O54' . . . 46.0(14) ? O52 O53' O53 . . . 131(2) ? O52 O53' O54' . . . 102.7(17) ? O53 O53' O54' . . . 29.4(16) ? Cl5 O54' O53 . . . 56.9(16) ? Cl5 O54' O54 . . . 54.7(16) ? Cl5 O54' O52' . . . 39.1(13) ? Cl5 O54' O53' . . . 39.0(12) ? O53 O54' O54 . . . 102(3) ? O53 O54' O52' . . . 91(2) ? O53 O54' O53' . . . 20.2(11) ? O54 O54' O52' . . . 16.1(9) ? O54 O54' O53' . . . 82(2) ? O52' O54' O53' . . . 70.7(17) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- 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 C11 3.419(4) . . ? Cu1 C12 3.059(4) . . ? Cu1 C14 3.033(4) . . ? Cu1 C15 3.396(5) . . ? Cu1 C16 3.075(5) . . ? Cu1 C111' 3.800(6) . . ? Cu1 C12' 3.048(4) . . ? Cu1 C14' 2.987(5) . . ? Cu1 C15' 3.430(5) . . ? Cu1 C16' 3.029(4) . . ? Cu1 H12b 3.29(3) . . ? Cu1 H13a 2.37(3) . . ? Cu1 H14b 3.14(3) . . ? Cu1 H15a 3.65(4) . . ? Cu1 H16b 3.30(4) . . ? Cu1 H17a 2.35(4) . . ? Cu1 H17b 2.40(5) . . ? Cu1 H111'b 3.21(4) . . ? Cu1 H12'a 3.28(4) . . ? Cu1 H13'b 2.34(3) . . ? Cu1 H14'a 3.02(4) . . ? Cu1 H16'a 3.15(4) . . ? Cu1 H17'a 2.50(4) . . ? Cu1 H17'b 2.31(5) . . ? Cu2 C21 3.410(4) . . ? Cu2 C22 3.041(4) . . ? Cu2 C24 2.996(4) . . ? Cu2 C25 3.441(5) . . ? Cu2 C26 2.988(5) . . ? Cu2 C211' 3.828(6) . . ? Cu2 C22' 3.037(4) . . ? Cu2 C24' 3.027(5) . . ? Cu2 C25' 3.386(5) . . ? Cu2 C26' 3.105(5) . . ? Cu2 O41 3.900(5) . '2 655' ? Cu2 Cl5 4.1497(12) . '2 655' ? Cu2 O51 3.370(4) . '2 655' ? Cu2 O52 3.889(5) . '2 655' ? Cu2 O53' 4.08(2) . '2 655' ? Cu2 H211'c 3.38(4) . . ? Cu2 H22a 3.15(3) . . ? Cu2 H23b 2.37(4) . . ? Cu2 H24a 3.00(4) . . ? Cu2 H26a 3.03(4) . . ? Cu2 H27a 2.44(5) . . ? Cu2 H27b 2.39(4) . . ? Cu2 H22'b 3.25(4) . . ? Cu2 H23'a 2.33(3) . . ? Cu2 H24'b 3.10(4) . . ? Cu2 H25'a 3.50(4) . . ? Cu2 H26'b 3.29(5) . . ? Cu2 H27'a 2.31(4) . . ? Cu2 H27'b 2.37(4) . . ? C11 N13 2.563(5) . . ? C11 N13' 2.524(4) . . ? C11 H111a 2.03(5) . . ? C11 H111b 2.01(3) . . ? C11 H111c 2.09(4) . . ? C11 H12a 2.03(3) . . ? C11 H12b 2.12(3) . . ? C11 H111'a 1.95(5) . . ? C11 H111'b 2.14(4) . . ? C11 H111'c 2.05(5) . . ? C11 H12'a 2.13(4) . . ? C11 H12'b 2.03(4) . . ? C11 H13'b 2.66(3) . . ? C111 C12 2.453(7) . . ? C111 C111' 2.489(8) . . ? C111 C12' 2.445(7) . . ? C111 H12a 2.58(4) . . ? C111 H111'a 2.57(4) . . ? C111 H111'c 2.69(5) . . ? C111 H12'b 2.54(4) . . ? C12 C14 2.392(6) . . ? C12 C111' 2.525(6) . . ? C12 C12' 2.478(6) . . ? C12 H111b 2.64(3) . . ? C12 H111c 2.55(4) . . ? C12 H13a 1.86(3) . . ? C12 H14a 2.39(4) . . ? C12 H14b 2.56(4) . . ? C12 H111'a 2.61(5) . . ? C12 H12'a 2.65(4) . . ? N13 C15 2.516(6) . . ? N13 N17 2.944(5) . . ? N13 C111' 3.051(6) . . ? N13 N13' 3.062(4) . . ? N13 O43' 3.11(3) . '3 666' ? N13 O01 3.136(5) . . ? N13 H12a 1.94(4) . . ? N13 H12b 2.00(3) . . ? N13 H14a 1.93(4) . . ? N13 H14b 1.94(4) . . ? N13 H15a 2.72(4) . . ? N13 H111'b 2.77(4) . . ? C14 C16 2.495(7) . . ? C14 N17 3.032(6) . . ? C14 H12a 2.46(4) . . ? C14 H12b 2.49(3) . . ? C14 H13a 1.86(3) . . ? C14 H15a 2.07(4) . . ? C14 H15b 1.86(4) . . ? C14 H16b 2.67(4) . . ? C15 N17 2.436(6) . . ? C15 H13a 2.60(3) . . ? C15 H14a 2.04(4) . . ? C15 H14b 2.02(4) . . ? C15 H16a 2.02(4) . . ? C15 H16b 2.01(4) . . ? C15 H17a 2.58(3) . . ? C16 H14b 2.61(4) . . ? C16 H15a 2.10(4) . . ? C16 H15b 1.91(4) . . ? C16 H17a 1.88(4) . . ? C16 H17b 1.83(4) . . ? N17 N17' 2.755(6) . . ? N17 O42' 3.12(3) . '2 655' ? N17 O54 3.056(8) . '2 655' ? N17 O52' 3.01(3) . '2 655' ? N17 H15a 2.71(4) . . ? N17 H16a 1.97(4) . . ? N17 H16b 1.99(4) . . ? N17 H17'a 2.46(4) . . ? C111' C12' 2.521(7) . . ? C111' N13' 2.978(6) . . ? C111' H111a 2.65(5) . . ? C111' H13'b 2.70(3) . . ? C12' C14' 2.385(6) . . ? C12' H111a 2.64(5) . . ? C12' H111b 2.52(3) . . ? C12' H12b 2.64(3) . . ? C12' H13'b 1.87(3) . . ? C12' H14'b 2.42(3) . . ? N13' C15' 2.511(5) . . ? N13' C16' 3.099(6) . . ? N13' N17' 2.823(6) . . ? N13' H111'b 2.72(4) . . ? N13' H12'a 2.03(4) . . ? N13' H12'b 1.97(4) . . ? N13' H14'a 2.04(4) . . ? N13' H14'b 1.92(4) . . ? N13' H15'b 2.72(4) . . ? C14' C16' 2.507(7) . . ? C14' N17' 2.994(7) . . ? C14' H12'a 2.52(3) . . ? C14' H12'b 2.51(4) . . ? C14' H13'b 1.87(3) . . ? C14' H15'a 1.95(4) . . ? C14' H15'b 2.04(4) . . ? C14' H16'a 2.65(4) . . ? C15' N17' 2.420(8) . . ? C15' H13'b 2.55(3) . . ? C15' H14'a 2.06(4) . . ? C15' H14'b 1.91(4) . . ? C15' H16'a 1.99(4) . . ? C15' H16'b 2.07(4) . . ? C15' H17'b 2.64(6) . . ? C16' H14'a 2.64(4) . . ? C16' H15'a 1.95(4) . . ? C16' H15'b 2.02(5) . . ? C16' H17'a 1.94(5) . . ? C16' H17'b 2.02(6) . . ? N17' O42 3.187(8) . '2 655' ? N17' H17b 2.65(5) . . ? N17' H13'b 2.78(3) . . ? N17' H15'b 2.62(4) . . ? N17' H16'a 2.08(5) . . ? N17' H16'b 2.09(5) . . ? C21 N23 2.535(5) . . ? C21 N23' 2.554(5) . . ? C21 H211a 2.10(5) . . ? C21 H211b 2.04(6) . . ? C21 H211c 2.15(4) . . ? C21 H211'a 2.20(5) . . ? C21 H211'b 1.98(4) . . ? C21 H211'c 2.10(4) . . ? C21 H22a 2.01(3) . . ? C21 H22b 2.02(3) . . ? C21 H22'a 1.98(4) . . ? C21 H22'b 2.08(4) . . ? C211 C22 2.446(7) . . ? C211 C211' 2.506(7) . . ? C211 C22' 2.461(8) . . ? C211 H211'b 2.68(4) . . ? C211 H22a 2.66(4) . . ? C211 H22b 2.49(3) . . ? C211 H22'a 2.53(4) . . ? C211 H22'b 2.68(4) . . ? C22 C24 2.393(6) . . ? C22 C211' 2.500(7) . . ? C22 C22' 2.495(6) . . ? C22 H211b 2.56(6) . . ? C22 H211c 2.65(4) . . ? C22 H23b 1.90(3) . . ? C22 H24b 2.50(5) . . ? C22 H22'b 2.62(4) . . ? N23 C25 2.524(6) . . ? N23 C26 3.072(5) . . ? N23 N27 2.801(5) . . ? N23 C211' 2.987(7) . . ? N23 N23' 3.064(5) . . ? N23 H211'c 2.77(4) . . ? N23 H22a 1.92(3) . . ? N23 H22b 2.03(3) . . ? N23 H24a 2.03(3) . . ? N23 H24b 2.13(5) . . ? N23 H25b 2.70(4) . . ? N23 H27b 2.78(3) . . ? C24 C26 2.515(6) . . ? C24 N27 3.012(6) . . ? C24 H22a 2.49(4) . . ? C24 H22b 2.59(3) . . ? C24 H23b 1.89(3) . . ? C24 H25a 2.01(4) . . ? C24 H25b 1.98(4) . . ? C25 N27 2.442(7) . . ? C25 H23b 2.55(4) . . ? C25 H24a 2.04(4) . . ? C25 H24b 2.12(5) . . ? C25 H26a 2.12(4) . . ? C25 H26b 1.98(3) . . ? C25 H27b 2.44(3) . . ? C26 H24a 2.64(3) . . ? C26 H25a 2.02(4) . . ? C26 H25b 2.07(5) . . ? C26 H27a 2.03(5) . . ? C26 H27b 1.81(3) . . ? N27 N27' 2.755(6) . . ? N27 O52 3.027(6) . '2 655' ? N27 H23b 2.75(4) . . ? N27 H25b 2.70(5) . . ? N27 H26a 2.02(4) . . ? N27 H26b 1.89(4) . . ? N27 H27'a 2.64(4) . . ? N27 H27'b 2.63(4) . . ? C211' C22' 2.531(7) . . ? C211' N23' 3.049(7) . . ? C211' H211b 2.60(6) . . ? C211' H22b 2.68(3) . . ? C22' C24' 2.402(7) . . ? C22' H211a 2.61(5) . . ? C22' H211c 2.64(4) . . ? C22' H211'b 2.67(4) . . ? C22' H22a 2.56(4) . . ? C22' H23'a 1.88(3) . . ? C22' H24'a 2.34(4) . . ? C22' H24'b 2.53(4) . . ? N23' C25' 2.504(6) . . ? N23' N27' 2.976(5) . . ? N23' H22'a 1.97(4) . . ? N23' H22'b 2.03(4) . . ? N23' H24'a 1.92(4) . . ? N23' H24'b 1.95(4) . . ? N23' H25'a 2.64(4) . . ? C24' C26' 2.492(7) . . ? C24' N27' 3.026(6) . . ? C24' H22'a 2.51(4) . . ? C24' H22'b 2.56(4) . . ? C24' H23'a 1.80(3) . . ? C24' H25'a 2.09(4) . . ? C24' H25'b 1.83(4) . . ? C24' H26'b 2.61(4) . . ? C25' N27' 2.451(7) . . ? C25' H23'a 2.52(4) . . ? C25' H24'a 2.13(4) . . ? C25' H24'b 2.09(3) . . ? C25' H26'a 2.01(4) . . ? C25' H26'b 2.03(4) . . ? C25' H27'a 2.67(4) . . ? C26' H24'b 2.63(4) . . ? C26' H25'a 2.07(4) . . ? C26' H25'b 1.88(4) . . ? C26' H27'a 1.88(4) . . ? C26' H27'b 1.97(4) . . ? N27' O53' 2.97(2) . '2 655' ? N27' H27a 2.33(5) . . ? N27' H25'a 2.63(4) . . ? N27' H26'a 1.91(5) . . ? N27' H26'b 1.94(5) . . ? Cl1 H14'a 2.73(4) . '2 655' ? Cl1 H14'a 2.73(4) . . ? Cl2 H24a 2.73(4) . 7 ? Cl2 H24a 2.73(4) . . ? O31 O32 2.312(6) . . ? O31 O33 2.265(7) . . ? O31 O34 2.272(6) . . ? O31 O52 3.167(7) . '1 565' ? O31 H13'b 2.76(3) . '2 655' ? O31 H15'b 2.68(5) . '2 655' ? O31 H17'b 2.73(6) . '2 655' ? O31 H27a 2.46(5) . '2 665' ? O32 O33 2.287(6) . . ? O32 O34 2.304(5) . . ? O32 O01 3.169(6) . '2 655' ? O32 H23'a 2.66(3) . '2 655' ? O32 H24'a 2.72(4) . '2 655' ? O33 O34 2.289(5) . . ? O33 H25a 2.67(4) . '3 665' ? O34 H27a 2.64(5) . '2 665' ? O34 H27'b 2.40(4) . '2 665' ? O41 O42 2.244(8) . . ? O41 O43 2.297(13) . . ? O41 O44' 2.34(4) . . ? O41 O51 3.160(8) . . ? O41 H23b 2.68(3) . '2 655' ? O41 H27b 2.50(4) . '2 655' ? O42 O43 2.224(10) . . ? O42 O44 2.252(9) . . ? O42 O43' 2.33(3) . . ? O42 H17b 2.57(5) . '2 655' ? O42 H17'a 2.43(5) . '2 655' ? O43 O44 2.316(13) . . ? O43 O44' 2.34(3) . . ? O43 H12a 2.71(4) . '3 666' ? O43 H14a 2.70(5) . '3 666' ? O44 O42' 2.90(2) . . ? O44 O01 3.153(8) . '3 666' ? O44 H15a 2.67(4) . '3 666' ? O42' O43' 2.22(4) . . ? O42' O44' 2.28(4) . . ? O42' H17b 2.43(5) . '2 655' ? O43' H12a 2.77(5) . '3 666' ? O43' H13a 2.53(5) . '3 666' ? O43' H14a 2.69(5) . '3 666' ? O44' H15a 2.64(5) . '3 666' ? O51 O52 2.319(6) . . ? O51 O53 2.253(10) . . ? O51 O54 2.369(7) . . ? O51 O53' 2.36(2) . . ? O51 O54' 2.20(4) . . ? O51 O01 3.192(6) . '2 655' ? O51 H23'a 2.72(3) . '2 655' ? O52 O53 2.295(11) . . ? O52 O54 2.299(8) . . ? O52 O54' 2.87(4) . . ? O52 H27a 2.62(5) . '2 655' ? O52 H27b 2.80(3) . '2 655' ? O52 H27'a 2.69(4) . '2 655' ? O53 O54 2.241(10) . . ? O53 O52' 2.49(3) . . ? O53 H211b 2.56(7) . '3 665' ? O53 H22b 2.79(4) . '3 665' ? O53 H25'a 2.69(4) . '2 655' ? O53 H27'a 2.74(4) . '2 655' ? O54 O53' 2.41(2) . . ? O54 O01 3.173(7) . '2 655' ? O54 H17a 2.31(4) . '2 655' ? O52' O53' 2.40(4) . . ? O52' H17a 2.30(5) . '2 655' ? O52' H12'b 2.45(5) . '2 645' ? O53' H27'a 2.22(4) . '2 655' ? O54' O01 2.60(4) . '2 655' ? O54' H22b 2.78(6) . '3 665' ? O01 H13a 2.55(3) . . ? O01 H17a 2.79(4) . . ? O01 H111'b 2.52(4) . . ? H111a H111b 1.41(6) . . ? H111a H111c 1.60(6) . . ? H111b H111c 1.53(6) . . ? H111c H12a 2.31(5) . . ? H12a H12b 1.54(5) . . ? H12a H13a 2.10(5) . . ? H12a H14a 2.11(5) . . ? H12b H14b 2.27(5) . . ? H12b H12'a 2.39(5) . . ? H13a H14a 2.09(5) . . ? H13a H111'b 2.37(5) . . ? H14a H14b 1.56(6) . . ? H14a H15a 2.36(5) . . ? H14a H15b 2.16(6) . . ? H14b H15b 2.24(6) . . ? H15a H15b 1.45(5) . . ? H15b H16a 2.24(5) . . ? H15b H16b 2.25(6) . . ? H16a H16b 1.37(6) . . ? H16a H17a 2.19(5) . . ? H16a H17b 2.09(6) . . ? H16b H17b 2.15(6) . . ? H17a H17b 1.24(7) . . ? H17b H17'a 2.18(6) . . ? H111'a H111'b 1.58(6) . . ? H111'a H111'c 1.43(6) . . ? H111'b H111'c 1.54(6) . . ? H111'b H13'b 2.31(5) . . ? H12'a H12'b 1.62(6) . . ? H12'b H13'b 2.14(5) . . ? H12'b H14'b 2.20(5) . . ? H13'b H14'b 2.15(5) . . ? H14'a H14'b 1.63(5) . . ? H14'a H15'a 2.24(5) . . ? H14'a H16'a 2.39(5) . . ? H14'b H15'a 2.16(5) . . ? H14'b H15'b 2.21(5) . . ? H15'a H15'b 1.62(6) . . ? H15'a H16'a 2.15(6) . . ? H15'a H16'b 2.26(6) . . ? H15'b H26b 2.37(5) . '1 565' ? H16'a H16'b 1.52(6) . . ? H16'a H17'a 2.36(7) . . ? H16'b H17'a 2.24(6) . . ? H17'a H17'b 1.36(8) . . ? H211a H211b 1.69(8) . . ? H211a H211c 1.60(6) . . ? H211a H22'a 2.33(7) . . ? H211b H211c 1.77(8) . . ? H211b H22b 2.21(6) . . ? H211'a H211'b 1.61(7) . . ? H211'a H211'c 1.54(6) . . ? H211'b H211'c 1.39(6) . . ? H211'c H23b 2.35(5) . . ? H22a H22b 1.60(5) . . ? H22a H22'b 2.31(6) . . ? H22b H23b 2.22(5) . . ? H22b H24b 2.26(6) . . ? H23b H24b 2.34(6) . . ? H24a H24b 1.80(6) . . ? H24a H25a 2.30(6) . . ? H24b H25a 2.32(6) . . ? H24b H25b 2.27(6) . . ? H25a H25b 1.53(6) . . ? H25a H26a 2.39(6) . . ? H25a H26b 2.30(5) . . ? H25b H26b 2.37(6) . . ? H26a H26b 1.51(5) . . ? H26a H27a 2.31(6) . . ? H26b H27a 2.20(6) . . ? H26b H27b 2.12(5) . . ? H27a H27b 1.46(6) . . ? H27a H27'a 2.11(7) . . ? H27a H27'b 2.08(6) . . ? H22'a H22'b 1.54(5) . . ? H22'a H23'a 2.18(5) . . ? H22'a H24'a 2.08(6) . . ? H22'b H24'b 2.27(6) . . ? H23'a H24'a 2.06(5) . . ? H23'a H25'a 2.36(5) . . ? H24'a H24'b 1.63(5) . . ? H24'a H25'b 2.24(6) . . ? H24'b H25'b 2.32(5) . . ? H24'b H26'b 2.38(6) . . ? H25'a H25'b 1.50(6) . . ? H25'a H26'a 2.33(6) . . ? H25'b H26'a 2.22(6) . . ? H25'b H26'b 2.25(6) . . ? H26'a H26'b 1.60(6) . . ? H26'a H27'a 2.05(6) . . ? H26'a H27'b 2.26(6) . . ? H26'b H27'b 2.16(6) . . ? H27'a H27'b 1.32(5) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 3808 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 57 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min -25 _reflns_limit_l_max 24 _reflns_number_observed ? _reflns_d_resolution_high .728 _reflns_d_resolution_low 20.811 _diffrn_reflns_av_sigmaI/netI .116 _diffrn_reflns_theta_min .97 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .084 _refine_ls_wR_factor_all .053 _refine_ls_goodness_of_fit_all 1.201 _refine_ls_shift/su_mean .004 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_global _audit_creation_method Xtal3.6 _audit_creation_date 99-11-15 _audit_update_record ? #============================================================================== # (Publishing Staff Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia Nedlands Western Australia 6907 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal ? _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Skelton, Brian W.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; 'White, Allan H.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Pogram for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_ykon # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C9 H29 Cl4 Co1 N6 O1' _chemical_formula_moiety ? _chemical_formula_weight 438.12 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 11.265(4) _cell_length_b 10.177(2) _cell_length_c 8.382(2) _cell_angle_alpha 97.91(2) _cell_angle_beta 97.51(3) _cell_angle_gamma 107.01(2) _cell_volume 895.2(4) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8 _cell_measurement_theta_min 26.5 _cell_measurement_theta_max 30 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 1.562 _exptl_crystal_description prism _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.26 _exptl_crystal_size_rad ? _exptl_crystal_colour orange _diffrn_measurement_device_type ; CAD4 diffractometer ; _diffrn_measurement_method '2\q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; XTAl absorb ; _exptl_absorpt_correction_T_min .52 _exptl_absorpt_correction_T_max .69 _diffrn_reflns_number 6056 _reflns_number_total 6056 _reflns_Friedel_coverage ? _reflns_number_gt 5347 _reflns_threshold_expression 'I > 3.00 sig(I )' _diffrn_reflns_theta_max 32.5 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_standards_number 8 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F #<< use NfA code _refine_ls_R_factor_gt .031 _refine_ls_wR_factor_ref .041 _refine_ls_goodness_of_fit_ref 1.273 _refine_ls_number_reflns 5347 _refine_ls_number_parameters 306 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall #<< use NfA code _refine_ls_shift/su_max .074 _refine_diff_density_min -1.03 _refine_diff_density_max 1.24 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Enraf Nonius software' _computing_cell_refinement 'Enraf Nonius software' _computing_data_reduction xtal _computing_structure_solution xtal _computing_structure_refinement xtal _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ 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 18 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 8 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' Co ? 0 2 .299 .973 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 2 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 12 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 58 0 0 '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_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Co .16045(2) .86794(2) .76449(2) .01840(8) Uani ? ? 1.00000 ? ? Cl1 -.00227(4) .95515(4) .72530(5) .02751(15) Uani ? ? 1.00000 ? ? Cl2 .36192(6) 1.45145(6) .29317(7) .0529(2) Uani ? ? 1.00000 ? ? Cl3 .10681(4) 1.38398(5) .65952(6) .03663(18) Uani ? ? 1.00000 ? ? Cl4 .56626(4) 1.04277(6) .81176(6) .0418(2) Uani ? ? 1.00000 ? ? N1 .15561(14) .89424(16) .99911(17) .0254(5) Uani ? ? 1.00000 ? ? C1 .0850(2) .7609(2) 1.0433(2) .0355(8) Uani ? ? 1.00000 ? ? C2 -.0196(2) .6819(2) .9023(3) .0384(8) Uani ? ? 1.00000 ? ? N2 .03368(15) .68439(16) .7489(2) .0290(6) Uani ? ? 1.00000 ? ? N11 .29740(15) .78598(18) .79360(19) .0277(6) Uani ? ? 1.00000 ? ? C12 .32697(19) .7316(2) .6331(2) .0344(7) Uani ? ? 1.00000 ? ? C13 .21598(19) .7104(2) .4990(2) .0326(7) Uani ? ? 1.00000 ? ? N14 .16805(14) .83185(15) .53100(17) .0248(5) Uani ? ? 1.00000 ? ? C15 .24968(18) .9578(2) .4815(2) .0295(7) Uani ? ? 1.00000 ? ? C16 .25911(15) 1.08655(17) .6006(2) .0250(6) Uani ? ? 1.00000 ? ? N17 .28345(12) 1.05441(14) .76821(16) .0222(5) Uani ? ? 1.00000 ? ? C18 .29259(18) 1.17827(19) .8924(2) .0330(7) Uani ? ? 1.00000 ? ? C19 .3970(2) 1.3058(2) .8715(3) .0420(8) Uani ? ? 1.00000 ? ? N110 .37646(17) 1.33559(18) .7023(3) .0421(7) Uani ? ? 1.00000 ? ? C111 .3634(2) 1.2119(2) .5759(3) .0364(8) Uani ? ? 1.00000 ? ? O01 .2752(2) .5658(2) .9872(3) .0663(10) Uani ? ? 1.00000 ? ? H11a .282(3) .727(3) .838(3) .050(8) Uiso ? ? 1.00000 ? ? H11b .365(3) .855(3) .842(3) .051(7) Uiso ? ? 1.00000 ? ? H12a .398(2) .803(2) .620(3) .034(6) Uiso ? ? 1.00000 ? ? H12b .341(2) .638(3) .636(3) .052(7) Uiso ? ? 1.00000 ? ? H13a .241(2) .709(2) .398(3) .034(6) Uiso ? ? 1.00000 ? ? H13b .141(2) .622(2) .498(3) .032(5) Uiso ? ? 1.00000 ? ? H14 .090(2) .805(2) .476(3) .032(6) Uiso ? ? 1.00000 ? ? H15a .333(2) .951(2) .496(3) .042(6) Uiso ? ? 1.00000 ? ? H15b .215(2) .959(2) .374(3) .037(6) Uiso ? ? 1.00000 ? ? H16 .1833(18) 1.103(2) .589(2) .018(4) Uiso ? ? 1.00000 ? ? H17 .354(2) 1.044(2) .775(2) .021(5) Uiso ? ? 1.00000 ? ? H18a .214(2) 1.190(2) .885(2) .028(5) Uiso ? ? 1.00000 ? ? H18b .309(2) 1.156(2) .998(3) .038(6) Uiso ? ? 1.00000 ? ? H19a .479(3) 1.295(3) .890(3) .055(7) Uiso ? ? 1.00000 ? ? H19b .398(3) 1.382(3) .942(3) .056(8) Uiso ? ? 1.00000 ? ? H110a .450(3) 1.407(3) .687(3) .047(7) Uiso ? ? 1.00000 ? ? H110b .302(3) 1.366(3) .682(3) .063(8) Uiso ? ? 1.00000 ? ? H111a .437(2) 1.194(2) .590(2) .025(5) Uiso ? ? 1.00000 ? ? H111b .339(3) 1.236(3) .475(4) .066(9) Uiso ? ? 1.00000 ? ? H1aN .116(2) .955(2) 1.021(3) .041(6) Uiso ? ? 1.00000 ? ? H1bN .233(2) .925(2) 1.052(3) .036(6) Uiso ? ? 1.00000 ? ? H1aC .056(2) .781(2) 1.140(3) .035(6) Uiso ? ? 1.00000 ? ? H1bC .137(2) .705(2) 1.061(3) .038(6) Uiso ? ? 1.00000 ? ? H2aC -.084(3) .726(3) .890(3) .049(7) Uiso ? ? 1.00000 ? ? H2bC -.063(3) .584(3) .911(3) .054(7) Uiso ? ? 1.00000 ? ? H2aN .062(3) .615(3) .731(3) .058(8) Uiso ? ? 1.00000 ? ? H2bN -.024(2) .666(3) .662(3) .041(6) Uiso ? ? 1.00000 ? ? H01a .204(3) .477(3) .914(3) .058(6) Uiso ? ? 1.00000 ? ? H01b .302(3) .602(3) 1.095(4) .070(7) Uiso ? ? 1.00000 ? ? 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 Co .01673(10) .02149(10) .01839(11) .00708(7) .00424(7) .00507(7) Cl1 .02142(17) .0342(2) .0301(2) .01344(15) .00359(14) .00738(15) Cl2 .0460(3) .0503(3) .0511(3) -.0049(2) .0032(2) .0216(3) Cl3 .0302(2) .0352(2) .0411(3) .00728(17) .00199(17) .00660(18) Cl4 .02181(19) .0686(3) .0345(2) .0150(2) .00436(16) .0064(2) N1 .0227(6) .0348(7) .0216(7) .0116(6) .0057(5) .0078(5) C1 .0396(10) .0429(10) .0308(9) .0145(8) .0153(8) .0179(8) C2 .0341(9) .0368(10) .0448(11) .0043(8) .0186(8) .0136(8) N2 .0287(7) .0235(7) .0333(8) .0055(6) .0073(6) .0050(6) N11 .0260(7) .0321(8) .0322(8) .0153(6) .0085(6) .0130(6) C12 .0350(9) .0374(10) .0386(10) .0202(8) .0140(8) .0065(8) C13 .0369(9) .0314(9) .0308(9) .0144(7) .0098(7) -.0014(7) N14 .0234(6) .0296(7) .0211(6) .0089(5) .0042(5) .0019(5) C15 .0317(8) .0375(9) .0239(8) .0127(7) .0108(6) .0112(6) C16 .0223(7) .0278(8) .0274(8) .0080(6) .0055(6) .0122(6) N17 .0185(6) .0250(6) .0231(6) .0068(5) .0030(5) .0060(5) C18 .0320(9) .0273(8) .0333(9) .0032(7) .0050(7) -.0009(7) C19 .0347(10) .0280(9) .0537(13) -.0004(8) .0049(9) .0012(8) N110 .0310(8) .0261(8) .0689(13) .0042(6) .0116(8) .0160(8) C111 .0331(9) .0353(10) .0448(11) .0078(8) .0137(8) .0212(8) O01 .0688(13) .0513(11) .0769(14) .0139(10) .0034(11) .0264(10) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Co Cl1 . . 2.2650(8) ? Co N1 . . 1.9580(15) ? Co N2 . . 1.9670(15) ? Co N11 . . 1.961(2) ? Co N14 . . 1.9588(15) ? Co N17 . . 1.9890(13) ? N1 C1 . . 1.482(3) ? N1 H1aN . . .88(3) ? N1 H1bN . . .87(2) ? C1 C2 . . 1.501(3) ? C1 H1aC . . .94(2) ? C1 H1bC . . .94(3) ? C2 N2 . . 1.489(3) ? C2 H2aC . . .96(3) ? C2 H2bC . . .99(3) ? N2 H2aN . . .85(3) ? N2 H2bN . . .87(2) ? N11 C12 . . 1.499(3) ? N11 H11a . . .74(3) ? N11 H11b . . .87(2) ? C12 C13 . . 1.511(3) ? C12 H12a . . .94(2) ? C12 H12b . . 1.01(3) ? C13 N14 . . 1.493(3) ? C13 H13a . . .92(2) ? C13 H13b . . 1.04(2) ? N14 C15 . . 1.489(2) ? N14 H14 . . .88(2) ? C15 C16 . . 1.502(3) ? C15 H15a . . .95(3) ? C15 H15b . . .93(2) ? C16 N17 . . 1.495(2) ? C16 C111 . . 1.520(3) ? C16 H16 . . .91(2) ? N17 C18 . . 1.489(2) ? N17 H17 . . .83(2) ? C18 C19 . . 1.523(3) ? C18 H18a . . .92(3) ? C18 H18b . . .95(3) ? C19 N110 . . 1.493(3) ? C19 H19a . . .95(3) ? C19 H19b . . .90(3) ? N110 C111 . . 1.487(3) ? N110 H110a . . .97(2) ? N110 H110b . . .98(4) ? C111 H111a . . .89(2) ? C111 H111b . . .94(3) ? O01 H01a . . 1.06(2) ? O01 H01b . . .90(3) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published Cl1 Co N1 . . . 88.84(6) ? Cl1 Co N2 . . . 87.29(6) ? Cl1 Co N11 . . . 177.93(5) ? Cl1 Co N14 . . . 93.90(5) ? Cl1 Co N17 . . . 90.75(5) ? N1 Co N2 . . . 85.84(7) ? N1 Co N11 . . . 92.08(7) ? N1 Co N14 . . . 176.67(8) ? N1 Co N17 . . . 96.71(6) ? N2 Co N11 . . . 90.93(8) ? N2 Co N14 . . . 92.39(7) ? N2 Co N17 . . . 176.76(7) ? N11 Co N14 . . . 85.11(7) ? N11 Co N17 . . . 90.98(7) ? N14 Co N17 . . . 85.16(6) ? Co N1 C1 . . . 110.37(11) ? Co N1 H1aN . . . 108.4(16) ? Co N1 H1bN . . . 107.9(16) ? C1 N1 H1aN . . . 108.5(16) ? C1 N1 H1bN . . . 111.1(17) ? H1aN N1 H1bN . . . 111(2) ? N1 C1 C2 . . . 108.09(17) ? N1 C1 H1aC . . . 108.4(14) ? N1 C1 H1bC . . . 111.4(14) ? C2 C1 H1aC . . . 113.1(13) ? C2 C1 H1bC . . . 107.7(12) ? H1aC C1 H1bC . . . 108(2) ? C1 C2 N2 . . . 108.21(17) ? C1 C2 H2aC . . . 111.7(13) ? C1 C2 H2bC . . . 114.7(15) ? N2 C2 H2aC . . . 106.4(16) ? N2 C2 H2bC . . . 109.8(16) ? H2aC C2 H2bC . . . 106(2) ? Co N2 C2 . . . 109.10(11) ? Co N2 H2aN . . . 114.1(18) ? Co N2 H2bN . . . 110.9(16) ? C2 N2 H2aN . . . 109(2) ? C2 N2 H2bN . . . 112.3(18) ? H2aN N2 H2bN . . . 101(2) ? Co N11 C12 . . . 112.04(13) ? Co N11 H11a . . . 112(2) ? Co N11 H11b . . . 106(2) ? C12 N11 H11a . . . 107(2) ? C12 N11 H11b . . . 105(2) ? H11a N11 H11b . . . 114(3) ? N11 C12 C13 . . . 109.01(18) ? N11 C12 H12a . . . 104.2(14) ? N11 C12 H12b . . . 109.9(15) ? C13 C12 H12a . . . 111.1(14) ? C13 C12 H12b . . . 108.2(13) ? H12a C12 H12b . . . 114(2) ? C12 C13 N14 . . . 107.77(15) ? C12 C13 H13a . . . 110.2(14) ? C12 C13 H13b . . . 113.0(13) ? N14 C13 H13a . . . 108.4(16) ? N14 C13 H13b . . . 106.3(15) ? H13a C13 H13b . . . 111.0(17) ? Co N14 C13 . . . 108.11(12) ? Co N14 C15 . . . 111.14(10) ? Co N14 H14 . . . 107.9(16) ? C13 N14 C15 . . . 111.31(16) ? C13 N14 H14 . . . 106.2(16) ? C15 N14 H14 . . . 112.0(16) ? N14 C15 C16 . . . 109.72(15) ? N14 C15 H15a . . . 106.5(15) ? N14 C15 H15b . . . 107.7(13) ? C16 C15 H15a . . . 104.6(13) ? C16 C15 H15b . . . 113.0(16) ? H15a C15 H15b . . . 115(2) ? C15 C16 N17 . . . 106.68(15) ? C15 C16 C111 . . . 110.83(16) ? C15 C16 H16 . . . 109.6(10) ? N17 C16 C111 . . . 111.70(13) ? N17 C16 H16 . . . 106.9(12) ? C111 C16 H16 . . . 110.9(12) ? Co N17 C16 . . . 106.36(8) ? Co N17 C18 . . . 121.17(11) ? Co N17 H17 . . . 107.1(13) ? C16 N17 C18 . . . 109.25(14) ? C16 N17 H17 . . . 103.6(14) ? C18 N17 H17 . . . 108.0(12) ? N17 C18 C19 . . . 110.34(17) ? N17 C18 H18a . . . 108.2(12) ? N17 C18 H18b . . . 107.6(15) ? C19 C18 H18a . . . 114.3(13) ? C19 C18 H18b . . . 111.0(12) ? H18a C18 H18b . . . 105(2) ? C18 C19 N110 . . . 111.32(16) ? C18 C19 H19a . . . 113.3(17) ? C18 C19 H19b . . . 109.9(18) ? N110 C19 H19a . . . 106.4(17) ? N110 C19 H19b . . . 108(2) ? H19a C19 H19b . . . 108(2) ? C19 N110 C111 . . . 111.72(18) ? C19 N110 H110a . . . 109.9(15) ? C19 N110 H110b . . . 111.3(18) ? C111 N110 H110a . . . 104.9(16) ? C111 N110 H110b . . . 109.5(15) ? H110a N110 H110b . . . 109(3) ? C16 C111 N110 . . . 109.72(18) ? C16 C111 H111a . . . 109.0(13) ? C16 C111 H111b . . . 108.9(16) ? N110 C111 H111a . . . 107.3(12) ? N110 C111 H111b . . . 105.4(19) ? H111a C111 H111b . . . 116(2) ? H01a O01 H01b . . . 137(3) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- 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 Co Cl3 4.2951(9) . '2 576' ? Co Cl4 4.3353(16) . . ? Co Cl4 4.1876(10) . '2 677' ? Co C1 2.837(2) . . ? Co C2 2.829(2) . . ? Co C12 2.881(2) . . ? Co C13 2.808(2) . . ? Co C15 2.856(2) . . ? Co C16 2.8047(18) . . ? Co C18 3.0397(18) . . ? Co H11a 2.34(3) . . ? Co H11b 2.36(3) . . ? Co H12a 3.28(3) . . ? Co H13b 3.05(2) . . ? Co H14 2.38(2) . . ? Co H15a 3.20(3) . . ? Co H16 2.94(2) . . ? Co H17 2.370(19) . . ? Co H18a 3.14(2) . . ? Co H18b 3.15(2) . . ? Co H1aN 2.38(2) . . ? Co H1bN 2.37(2) . . ? Co H1bC 3.17(3) . . ? Co H2aC 3.11(3) . . ? Co H2aN 2.44(3) . . ? Co H2bN 2.42(2) . . ? Cl1 N1 2.9638(17) . . ? Cl1 C2 3.296(3) . . ? Cl1 N2 2.929(2) . . ? Cl1 N14 3.0937(19) . . ? Cl1 C15 3.487(2) . '2 576' ? Cl1 C16 3.231(2) . . ? Cl1 N17 3.0339(17) . . ? Cl1 C18 3.413(2) . . ? Cl1 H14 2.90(2) . . ? Cl1 H15b 2.85(3) . '2 576' ? Cl1 H16 2.68(2) . . ? Cl1 H16 2.985(18) . '2 576' ? Cl1 H18a 2.882(18) . . ? Cl1 H1aN 2.66(2) . . ? Cl1 H1aN 2.80(3) . '2 577' ? Cl1 H1aC 3.02(3) . '2 577' ? Cl1 H2aC 2.86(3) . . ? Cl1 H2bN 2.85(3) . . ? Cl2 O01 3.118(3) . '1 564' ? Cl2 H19b 3.04(3) . '1 554' ? Cl2 H111b 2.81(3) . . ? Cl2 H2aC 3.18(2) . '2 576' ? Cl2 H01b 2.56(4) . '1 564' ? Cl3 N2 3.405(2) . '1 565' ? Cl3 N2 3.4631(18) . '2 576' ? Cl3 N14 3.2749(15) . '2 576' ? Cl3 N110 3.200(2) . . ? Cl3 O01 3.123(2) . '1 565' ? Cl3 H12b 3.16(2) . '1 565' ? Cl3 H13b 2.88(2) . '1 565' ? Cl3 H13b 2.91(2) . '2 576' ? Cl3 H14 2.48(2) . '2 576' ? Cl3 H110b 2.24(4) . . ? Cl3 H1aC 2.96(2) . '2 577' ? Cl3 H2aN 2.56(3) . '1 565' ? Cl3 H2bN 2.66(2) . '2 576' ? Cl3 H01a 2.21(2) . '1 565' ? Cl4 Cl4 3.7645(10) . '2 677' ? Cl4 N1 3.1603(18) . '2 677' ? Cl4 N11 3.4435(16) . '2 677' ? Cl4 N11 3.3414(18) . . ? Cl4 C12 3.490(2) . . ? Cl4 C15 3.417(2) . '2 676' ? Cl4 N17 3.1978(19) . . ? Cl4 H11b 2.57(3) . . ? Cl4 H11b 2.87(3) . '2 677' ? Cl4 H12a 2.75(2) . . ? Cl4 H15a 2.95(3) . '2 676' ? Cl4 H15b 3.08(3) . '2 676' ? Cl4 H17 2.37(2) . . ? Cl4 H19a 3.03(3) . . ? Cl4 H111a 3.06(2) . . ? Cl4 H1bN 2.30(2) . '2 677' ? N1 C2 2.414(2) . . ? N1 N2 2.673(2) . . ? N1 N11 2.821(3) . . ? N1 N17 2.950(2) . . ? N1 H1aC 1.99(2) . . ? N1 H1bC 2.02(3) . . ? N1 H2aC 2.70(2) . . ? C1 N2 2.422(3) . . ? C1 H1aN 1.95(3) . . ? C1 H1bN 1.97(2) . . ? C1 H2aC 2.06(3) . . ? C1 H2bC 2.11(2) . . ? C2 H1aC 2.06(2) . . ? C2 H1bC 2.00(2) . . ? C2 H2aN 1.95(3) . . ? C2 H2bN 1.99(3) . . ? N2 N11 2.800(2) . . ? N2 N14 2.833(2) . . ? N2 H11a 2.69(3) . . ? N2 H13b 2.65(2) . . ? N2 H1bC 2.68(2) . . ? N2 H2aC 1.99(3) . . ? N2 H2bC 2.05(3) . . ? N11 C13 2.450(2) . . ? N11 N14 2.651(2) . . ? N11 N17 2.817(3) . . ? N11 O01 2.915(3) . . ? N11 H12a 1.95(2) . . ? N11 H12b 2.07(3) . . ? N11 H17 2.55(2) . . ? N11 H2aN 2.65(3) . . ? C12 N14 2.426(3) . . ? C12 H11a 1.85(3) . . ? C12 H11b 1.93(3) . . ? C12 H13a 2.03(2) . . ? C12 H13b 2.14(2) . . ? C12 H15a 2.64(3) . . ? C13 C15 2.462(3) . . ? C13 H12a 2.05(2) . . ? C13 H12b 2.06(3) . . ? C13 H14 1.93(3) . . ? C13 H15a 2.42(2) . . ? N14 C16 2.446(2) . . ? N14 N17 2.6712(17) . . ? N14 H13a 1.99(3) . . ? N14 H13b 2.05(2) . . ? N14 H15a 1.98(2) . . ? N14 H15b 1.98(3) . . ? N14 H16 2.68(2) . . ? C15 N17 2.404(2) . . ? C15 C111 2.488(3) . . ? C15 H13a 2.51(2) . . ? C15 H14 1.99(2) . . ? C15 H16 2.00(2) . . ? C15 H17 2.502(18) . . ? C15 H111a 2.639(18) . . ? C16 C18 2.433(3) . . ? C16 C19 2.864(2) . . ? C16 N110 2.459(2) . . ? C16 H15a 1.97(3) . . ? C16 H15b 2.05(2) . . ? C16 H17 1.87(2) . . ? C16 H18a 2.64(2) . . ? C16 H111a 2.00(2) . . ? C16 H111b 2.03(3) . . ? N17 C19 2.473(2) . . ? N17 N110 2.902(2) . . ? N17 C111 2.495(3) . . ? N17 H11b 2.58(3) . . ? N17 H15a 2.58(3) . . ? N17 H16 1.96(2) . . ? N17 H18a 1.98(2) . . ? N17 H18b 2.00(2) . . ? N17 H111a 2.66(2) . . ? C18 N110 2.491(3) . . ? C18 C111 2.904(3) . . ? C18 H16 2.581(17) . . ? C18 H17 1.92(2) . . ? C18 H19a 2.09(3) . . ? C18 H19b 2.02(3) . . ? C19 C111 2.467(3) . . ? C19 H17 2.55(2) . . ? C19 H18a 2.08(2) . . ? C19 H18b 2.07(3) . . ? C19 H110a 2.04(3) . . ? C19 H110b 2.07(3) . . ? C19 H111a 2.63(2) . . ? N110 H16 2.659(16) . . ? N110 H19a 1.98(3) . . ? N110 H19b 1.96(3) . . ? N110 H111a 1.95(2) . . ? N110 H111b 1.96(3) . . ? C111 H15a 2.55(3) . . ? C111 H16 2.034(19) . . ? C111 H17 2.54(2) . . ? C111 H19a 2.68(3) . . ? C111 H110a 1.97(2) . . ? C111 H110b 2.04(3) . . ? O01 H11a 2.19(3) . . ? O01 H19a 2.70(3) . '2 677' ? O01 H19b 2.65(3) . '1 545' ? O01 H1bC 2.47(3) . . ? O01 H2bC 2.74(3) . '2 567' ? H11a H11b 1.35(4) . . ? H11a H12b 2.08(4) . . ? H11a H2aN 2.39(4) . . ? H11b H12a 1.98(4) . . ? H11b H17 2.11(4) . . ? H12a H12b 1.64(4) . . ? H12a H13a 2.27(3) . . ? H12a H15a 2.19(4) . . ? H12b H13b 2.34(4) . . ? H13a H13b 1.62(3) . . ? H13a H14 2.31(4) . . ? H13a H15a 2.36(3) . . ? H13b H14 2.13(4) . . ? H13b H2aN 2.25(4) . . ? H14 H15b 2.14(3) . . ? H15a H15b 1.59(4) . . ? H15a H17 2.35(3) . . ? H15a H111a 2.37(3) . . ? H15b H16 2.29(3) . . ? H16 H111b 2.29(4) . . ? H17 H18b 2.24(3) . . ? H18a H18b 1.49(4) . . ? H18a H19b 2.34(3) . . ? H18b H19a 2.39(4) . . ? H18b H19b 2.37(4) . . ? H18b H1bN 2.38(3) . . ? H19a H19b 1.50(5) . . ? H19a H110a 2.21(4) . . ? H19a H01b 2.37(4) . '2 677' ? H19b H110a 2.32(4) . . ? H19b H110b 2.27(4) . . ? H110a H110b 1.59(4) . . ? H110a H111a 2.17(3) . . ? H110a H111b 2.24(3) . . ? H110b H111b 2.20(4) . . ? H111a H111b 1.56(4) . . ? H1aN H1bN 1.44(4) . . ? H1aN H1aC 2.13(3) . . ? H1bN H1aC 2.37(3) . . ? H1bN H1bC 2.20(3) . . ? H1aC H1bC 1.52(4) . . ? H1aC H2aC 2.34(3) . . ? H1bC H2bC 2.32(3) . . ? H1bC H01b 2.39(5) . . ? H2aC H2bC 1.55(4) . . ? H2aC H2bN 2.18(4) . . ? H2bC H2aN 2.19(4) . . ? H2bC H2bN 2.39(4) . . ? H2bC H01a 2.32(4) . '2 567' ? H2aN H2bN 1.33(4) . . ? H01a H01b 1.83(4) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 456 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 7 6 6 -7 -6 -6 15 0 0 -15 0 0 0 12 0 0 -12 0 0 0 8 0 0 -8 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 15 _reflns_limit_k_min -14 _reflns_limit_k_max 14 _reflns_limit_l_min -10 _reflns_limit_l_max 10 _reflns_number_observed 6056 _reflns_d_resolution_high ? _reflns_d_resolution_low ? _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_theta_min ? _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'single counter' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .035 _refine_ls_wR_factor_all .041 _refine_ls_goodness_of_fit_all 1.159 _refine_ls_shift/su_mean .0058 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_global _audit_creation_method Xtal3.6 _audit_creation_date 99-11-16 _audit_update_record ? #============================================================================== # (Publishing Staff Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia Nedlands Western Australia 6907 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal ? _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Skelton, Brian W.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; 'White, Allan H.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Pogram for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_yklig # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C17 H67 Cl8 N8 O7.5' _chemical_formula_moiety ? _chemical_formula_weight 787.40 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C_1_2/c_1 _symmetry_space_group_name_Hall -c_2yc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,+y,1/2-z -x,-y,-z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 21.636(6) _cell_length_b 17.446(5) _cell_length_c 10.360(4) _cell_angle_alpha 90.00000 _cell_angle_beta 94.82(3) _cell_angle_gamma 90.00000 _cell_volume 3897(2) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.342 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 19.8 _cell_measurement_theta_max 21.5 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu .62 _exptl_crystal_description block _exptl_crystal_size_max .65 _exptl_crystal_size_mid .55 _exptl_crystal_size_min .33 _exptl_crystal_size_rad ? _exptl_crystal_colour blue _diffrn_measurement_device_type ; CAD4 diffractomter ; _diffrn_measurement_method '2\q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; XTAL absorb ; _exptl_absorpt_correction_T_min .77 _exptl_absorpt_correction_T_max .83 _diffrn_reflns_number 9154 _reflns_number_total 4439 _reflns_Friedel_coverage ? _reflns_number_gt 3142 _reflns_threshold_expression 'I > 3.00 sig(I )' _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .033 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_standards_number 6 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F #<< use NfA code _refine_ls_R_factor_gt .057 _refine_ls_wR_factor_ref .060 _refine_ls_goodness_of_fit_ref 1.945 _refine_ls_number_reflns 3142 _refine_ls_number_parameters 310 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment mixed #<< use NfA code _refine_ls_shift/su_max .0835 _refine_diff_density_min -.69 _refine_diff_density_max .58 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Enraf Nonius software' _computing_cell_refinement 'Enraf Nonius software' _computing_data_reduction xtal _computing_structure_solution xtal _computing_structure_refinement xtal _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ 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 68 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 32 .132019 .158997 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 30 .007996 .005981 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 32 .004028 .002991 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 268 0 0 '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_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C0 .50000 .6751(3) .25000 .040(2) Uani ? ? 1.00000 ? ? C11 .55659(15) .6262(2) .2194(4) .0403(18) Uani ? ? 1.00000 ? ? N12 .57993(15) .5710(2) .3201(4) .0423(18) Uani ? ? 1.00000 ? ? C13 .63285(16) .5242(2) .2806(4) .0415(18) Uani ? ? 1.00000 ? ? C14 .65396(18) .4671(2) .3847(4) .044(2) Uani ? ? 1.00000 ? ? C15 .7057(2) .4172(2) .3417(4) .048(2) Uani ? ? 1.00000 ? ? N16 .7183(2) .3532(2) .4316(5) .059(2) Uani ? ? 1.00000 ? ? C21 .51231(16) .7239(2) .3735(4) .046(2) Uani ? ? 1.00000 ? ? N22 .56363(14) .7812(2) .3761(4) .0485(19) Uani ? ? 1.00000 ? ? C23 .5695(2) .8239(3) .5027(6) .064(3) Uani ? ? 1.00000 ? ? C24 .6148(2) .8898(3) .5033(7) .066(3) Uani ? ? 1.00000 ? ? C25 .68190(19) .8691(3) .4961(5) .055(2) Uani ? ? 1.00000 ? ? N26 .70904(18) .8292(2) .6129(4) .056(2) Uani ? ? 1.00000 ? ? Cl1 .65965(4) .66422(5) .52103(9) .0476(5) Uani ? ? 1.00000 ? ? Cl2 .68177(5) .75159(6) .18749(11) .0583(6) Uani ? ? 1.00000 ? ? Cl3 .78973(6) .55196(7) .16073(11) .0711(7) Uani ? ? 1.00000 ? ? Cl4 .50000 .96177(18) .75000 .149(2) Uani ? ? 1.00000 ? ? Cl5 .50977(18) .5402(4) .5644(6) .176(7) Uani ? ? .50000 ? ? O01 .5560(2) .8898(2) .1730(4) .108(3) Uani ? ? 1.00000 ? ? O02 .4102(2) .8814(3) .5743(5) .128(4) Uani ? ? 1.00000 ? ? O03 .6097(3) .7353(4) .8441(7) .178(5) Uani ? ? 1.00000 ? ? O04 .50000 .6753(9) .75000 .24(2) Uani ? ? .50000 ? ? O05 .5107(9) .5660(10) .6395(14) .047(9) Uani ? ? .25000 ? ? O06 .5054(6) .5910(8) .7006(15) .052(9) Uani ? ? .25000 ? ? H11a .5893(16) .657(2) .211(3) .037(9) Uiso ? ? 1.00000 ? ? H11b .5503(16) .601(2) .149(3) .036(10) Uiso ? ? 1.00000 ? ? H12a .592(2) .596(3) .389(4) .062(14) Uiso ? ? 1.00000 ? ? H12b .5620(17) .546(2) .337(4) .026(12) Uiso ? ? 1.00000 ? ? H13a .6631(18) .561(2) .271(4) .051(11) Uiso ? ? 1.00000 ? ? H13b .6193(19) .499(2) .201(4) .062(12) Uiso ? ? 1.00000 ? ? H14a .6691(18) .494(2) .456(4) .056(12) Uiso ? ? 1.00000 ? ? H14b .618(2) .436(3) .404(4) .077(14) Uiso ? ? 1.00000 ? ? H15a .697(2) .403(3) .273(5) .071(16) Uiso ? ? 1.00000 ? ? H15b .750(2) .431(2) .341(4) .050(11) Uiso ? ? 1.00000 ? ? H16a .732(3) .369(4) .503(6) .11(3) Uiso ? ? 1.00000 ? ? H16b .684(3) .323(4) .429(6) .12(2) Uiso ? ? 1.00000 ? ? H16c .753(3) .322(3) .414(5) .097(18) Uiso ? ? 1.00000 ? ? H21a .5193(18) .692(2) .445(4) .052(12) Uiso ? ? 1.00000 ? ? H21b .4753(17) .752(2) .386(3) .046(10) Uiso ? ? 1.00000 ? ? H22a .5615(19) .814(2) .311(4) .054(13) Uiso ? ? 1.00000 ? ? H22b .5954(18) .760(2) .364(4) .046(11) Uiso ? ? 1.00000 ? ? H23a .536(2) .837(3) .509(4) .061(13) Uiso ? ? 1.00000 ? ? H23b .5789(19) .780(3) .577(4) .063(13) Uiso ? ? 1.00000 ? ? H25a .703(2) .913(3) .497(4) .060(12) Uiso ? ? 1.00000 ? ? H25b .6866(18) .833(2) .415(4) .058(11) Uiso ? ? 1.00000 ? ? H24a .612(2) .913(3) .572(5) .077(17) Uiso ? ? 1.00000 ? ? H24b .607(2) .921(3) .438(5) .086(18) Uiso ? ? 1.00000 ? ? H26a .759(3) .824(3) .608(5) .11(2) Uiso ? ? 1.00000 ? ? H26b .6894(19) .787(3) .632(4) .053(12) Uiso ? ? 1.00000 ? ? H26c .700(2) .852(3) .679(4) .060(14) Uiso ? ? 1.00000 ? ? H01a .52992 .93374 .18744 .16500 Uiso ? ? 1.00000 ? ? H01b .59753 .91413 .20317 .16500 Uiso ? ? 1.00000 ? ? H02a .44319 .91227 .61168 .18000 Uiso ? ? 1.00000 ? ? H02b .36818 .90872 .60360 .18000 Uiso ? ? 1.00000 ? ? H03a .59278 .70267 .91587 .27000 Uiso ? ? 1.00000 ? ? H03b .57954 .70956 .78450 .27000 Uiso ? ? 1.00000 ? ? 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 C0 .022(2) .031(2) .065(3) .00000 -.007(2) .00000 C11 .0228(15) .0341(17) .063(2) -.0012(13) -.0027(15) .0001(17) N12 .0269(15) .0409(18) .058(2) .0044(14) -.0039(15) -.0041(17) C13 .0342(17) .043(2) .045(2) .0112(15) -.0065(15) -.0065(16) C14 .0404(19) .042(2) .050(2) .0118(16) .0023(16) -.0014(17) C15 .052(2) .050(2) .042(2) .0200(18) .0039(18) -.0006(18) N16 .064(2) .049(2) .067(3) .022(2) .014(2) .0083(19) C21 .0287(17) .0362(19) .072(3) .0022(14) -.0042(17) -.0072(18) N22 .0292(16) .0362(17) .078(3) .0020(13) -.0059(15) -.0102(17) C23 .034(2) .054(3) .103(4) .0037(18) -.001(2) -.037(3) C24 .055(3) .044(2) .096(4) .003(2) -.020(3) -.018(3) C25 .047(2) .050(2) .067(3) -.0096(18) -.005(2) -.008(2) N26 .046(2) .051(2) .068(2) -.0015(17) -.0126(17) -.014(2) Cl1 .0477(5) .0426(5) .0502(5) .0004(4) -.0099(4) -.0007(4) Cl2 .0524(6) .0589(6) .0656(6) -.0181(5) .0161(5) -.0013(5) Cl3 .0898(9) .0680(7) .0564(7) -.0091(6) .0124(6) -.0116(5) Cl4 .128(2) .106(2) .209(3) .00000 -.009(2) .00000 Cl5 .054(3) .214(8) .268(10) .045(4) .059(5) .207(8) O01 .167(4) .067(2) .093(3) -.013(3) .021(3) -.001(2) O02 .099(3) .139(4) .149(4) .013(3) .041(3) -.028(3) O03 .145(5) .180(6) .197(6) .065(4) -.055(4) -.063(5) O04 .21(2) .088(10) .38(3) .00000 -.20(2) .00000 O05 .037(9) .047(9) .052(11) -.032(8) -.024(9) .040(8) O06 .015(6) .036(6) .103(18) -.013(5) -.014(11) .006(6) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published C0 C11 . . 1.547(4) ? C0 C21 . . 1.542(5) ? C0 C11 . '2 655' 1.547(4) ? C0 C21 . '2 655' 1.542(5) ? C11 N12 . . 1.477(5) ? C11 H11a . . .90(3) ? C11 H11b . . .85(4) ? N12 C13 . . 1.492(5) ? N12 H12a . . .86(4) ? N12 H12b . . .62(4) ? C13 C14 . . 1.511(5) ? C13 H13a . . .93(4) ? C13 H13b . . .95(4) ? C14 C15 . . 1.514(6) ? C14 H14a . . .91(4) ? C14 H14b . . .99(5) ? C15 N16 . . 1.466(6) ? C15 H15a . . .77(5) ? C15 H15b . . 1.00(4) ? N16 H16a . . .82(6) ? N16 H16b . . .91(6) ? N16 H16c . . .95(6) ? C21 N22 . . 1.492(5) ? C21 H21a . . .93(4) ? C21 H21b . . .96(4) ? N22 C23 . . 1.505(7) ? N22 H22a . . .88(4) ? N22 H22b . . .80(4) ? C23 C24 . . 1.511(7) ? C23 H23a . . .77(5) ? C23 H23b . . 1.10(4) ? C24 C25 . . 1.504(6) ? C24 H24a . . .83(5) ? C24 H24b . . .87(5) ? C25 N26 . . 1.474(6) ? C25 H25a . . .90(4) ? C25 H25b . . 1.06(4) ? N26 H26a . . 1.08(6) ? N26 H26b . . .88(4) ? N26 H26c . . .83(5) ? Cl5 O05 . . .897(16) ? Cl5 O06 . . 1.676(16) ? Cl5 Cl5 . '3 666' 1.957(8) ? O01 H01a . . .971(4) ? O01 H01b . . 1.020(5) ? O02 H02a . . .950(5) ? O02 H02b . . 1.093(5) ? O03 H03a . . 1.028(7) ? O03 H03b . . .970(6) ? O04 O06 . . 1.56(2) ? O04 O06 . '2 656' 1.56(2) ? O05 O06 . . .79(2) ? O05 O06 . '2 656' 1.78(2) ? O06 O06 . '2 656' 1.07(2) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published C11 C0 C21 . . . 113.0(2) ? C11 C0 C11 . . '2 655' 113.1(3) ? C11 C0 C21 . . '2 655' 102.7(2) ? C21 C0 C11 . . '2 655' 102.7(2) ? C21 C0 C21 . . '2 655' 112.9(4) ? C11 C0 C21 '2 655' . '2 655' 113.0(2) ? C0 C11 N12 . . . 116.4(3) ? C0 C11 H11a . . . 109(2) ? C0 C11 H11b . . . 113(2) ? N12 C11 H11a . . . 104(2) ? N12 C11 H11b . . . 107(2) ? H11a C11 H11b . . . 107(3) ? C11 N12 C13 . . . 112.8(3) ? C11 N12 H12a . . . 109(3) ? C11 N12 H12b . . . 118(3) ? C13 N12 H12a . . . 109(3) ? C13 N12 H12b . . . 102(3) ? H12a N12 H12b . . . 106(5) ? N12 C13 C14 . . . 111.0(3) ? N12 C13 H13a . . . 102(2) ? N12 C13 H13b . . . 107(2) ? C14 C13 H13a . . . 111(2) ? C14 C13 H13b . . . 111(3) ? H13a C13 H13b . . . 113(3) ? C13 C14 C15 . . . 110.8(3) ? C13 C14 H14a . . . 108(3) ? C13 C14 H14b . . . 108(3) ? C15 C14 H14a . . . 108(3) ? C15 C14 H14b . . . 111(3) ? H14a C14 H14b . . . 111(4) ? C14 C15 N16 . . . 110.7(4) ? C14 C15 H15a . . . 110(4) ? C14 C15 H15b . . . 127(2) ? N16 C15 H15a . . . 111(4) ? N16 C15 H15b . . . 93(2) ? H15a C15 H15b . . . 103(4) ? C15 N16 H16a . . . 110(4) ? C15 N16 H16b . . . 108(4) ? C15 N16 H16c . . . 115(3) ? H16a N16 H16b . . . 117(6) ? H16a N16 H16c . . . 98(5) ? H16b N16 H16c . . . 109(5) ? C0 C21 N22 . . . 117.5(3) ? C0 C21 H21a . . . 109(2) ? C0 C21 H21b . . . 108(2) ? N22 C21 H21a . . . 109(2) ? N22 C21 H21b . . . 106(2) ? H21a C21 H21b . . . 106(3) ? C21 N22 C23 . . . 110.8(3) ? C21 N22 H22a . . . 115(3) ? C21 N22 H22b . . . 110(3) ? C23 N22 H22a . . . 110(3) ? C23 N22 H22b . . . 111(3) ? H22a N22 H22b . . . 100(4) ? N22 C23 C24 . . . 112.8(5) ? N22 C23 H23a . . . 102(3) ? N22 C23 H23b . . . 105(2) ? C24 C23 H23a . . . 113(3) ? C24 C23 H23b . . . 117(2) ? H23a C23 H23b . . . 105(4) ? C23 C24 C25 . . . 116.5(4) ? C23 C24 H24a . . . 107(4) ? C23 C24 H24b . . . 113(3) ? C25 C24 H24a . . . 107(3) ? C25 C24 H24b . . . 103(4) ? H24a C24 H24b . . . 110(5) ? C24 C25 N26 . . . 113.1(4) ? C24 C25 H25a . . . 107(3) ? C24 C25 H25b . . . 110(2) ? N26 C25 H25a . . . 103(3) ? N26 C25 H25b . . . 108(2) ? H25a C25 H25b . . . 116(4) ? C25 N26 H26a . . . 109(3) ? C25 N26 H26b . . . 114(3) ? C25 N26 H26c . . . 110(3) ? H26a N26 H26b . . . 117(4) ? H26a N26 H26c . . . 112(4) ? H26b N26 H26c . . . 94(4) ? O05 Cl5 O06 . . . 4.9(13) ? O05 Cl5 Cl5 . . '3 666' 159.7(13) ? O06 Cl5 Cl5 . . '3 666' 158.3(6) ? H01a O01 H01b . . . 97.6(3) ? H02a O02 H02b . . . 104.6(5) ? H03a O03 H03b . . . 86.7(5) ? O06 O04 O06 . . '2 656' 40.0(9) ? Cl5 O05 O06 . . . 170(3) ? Cl5 O05 O06 . . '2 656' 160.1(19) ? O06 O05 O06 . . '2 656' 19.6(13) ? Cl5 O06 O04 . . . 141.6(10) ? Cl5 O06 O05 . . . 5.6(15) ? Cl5 O06 O05 . . '2 656' 133.2(10) ? Cl5 O06 O06 . . '2 656' 147.0(14) ? O04 O06 O05 . . . 144(2) ? O04 O06 O05 . . '2 656' 84.2(9) ? O04 O06 O06 . . '2 656' 70.0(11) ? O05 O06 O05 . . '2 656' 132(2) ? O05 O06 O06 . . '2 656' 146(2) ? O05 O06 O06 '2 656' . '2 656' 14.3(10) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- 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 C0 N12 2.569(5) . . ? C0 N12 2.569(5) . '2 655' ? C0 N22 2.593(5) . . ? C0 N22 2.593(5) . '2 655' ? C0 H11a 2.03(3) . . ? C0 H11a 2.03(3) . '2 655' ? C0 H11b 2.03(4) . '2 655' ? C0 H11b 2.03(4) . . ? C0 H21a 2.05(4) . '2 655' ? C0 H21a 2.05(4) . . ? C0 H21b 2.06(4) . '2 655' ? C0 H21b 2.06(4) . . ? C11 C11 2.580(5) . '2 655' ? C11 C13 2.473(5) . . ? C11 C21 2.575(6) . . ? C11 C21 2.411(5) . '2 655' ? C11 Cl5 3.430(7) . '4 564' ? C11 Cl5 3.500(7) . '2 655' ? C11 H12a 1.93(4) . . ? C11 H12b 1.85(4) . . ? C11 H13a 2.58(4) . . ? C11 H13b 2.61(4) . . ? C11 H21a 2.53(4) . '2 655' ? C11 H21b 2.53(4) . '2 655' ? N12 C14 2.475(5) . . ? N12 Cl1 3.057(4) . . ? N12 Cl5 3.059(7) . '3 666' ? N12 Cl5 3.106(7) . . ? N12 H11a 1.91(3) . . ? N12 H11b 1.91(4) . . ? N12 H13a 1.92(4) . . ? N12 H13b 2.00(4) . . ? N12 H14a 2.65(4) . . ? N12 H14b 2.62(5) . . ? C13 C15 2.490(6) . . ? C13 H11a 2.59(3) . . ? C13 H11b 2.54(3) . . ? C13 H12a 1.94(5) . . ? C13 H12b 1.73(4) . . ? C13 H14a 1.99(4) . . ? C13 H14b 2.05(5) . . ? C13 H15a 2.54(5) . . ? C14 N16 2.451(6) . . ? C14 H12a 2.62(4) . . ? C14 H12b 2.44(4) . . ? C14 H13a 2.04(4) . . ? C14 H13b 2.06(4) . . ? C14 H15a 1.92(5) . . ? C14 H15b 2.26(4) . . ? C14 H16a 2.63(6) . . ? C14 H16b 2.63(6) . . ? C15 H13b 2.68(4) . . ? C15 H14a 1.99(4) . . ? C15 H14b 2.09(5) . . ? C15 H16a 1.91(6) . . ? C15 H16b 1.96(6) . . ? C15 H16c 2.05(5) . . ? N16 Cl2 3.368(5) . '4 565' ? N16 Cl2 3.128(5) . '6 645' ? N16 Cl3 3.186(5) . '4 565' ? N16 O03 2.893(8) . '4 564' ? N16 H14a 2.70(4) . . ? N16 H14b 2.61(5) . . ? N16 H15a 1.88(5) . . ? N16 H15b 1.82(4) . . ? C21 C21 2.570(6) . '2 655' ? C21 C23 2.467(6) . . ? C21 H11a 2.57(3) . '2 655' ? C21 H11b 2.53(4) . '2 655' ? C21 H22a 2.03(4) . . ? C21 H22b 1.92(4) . . ? C21 H23a 2.45(4) . . ? C21 H23b 2.64(4) . . ? N22 C24 2.511(6) . . ? N22 Cl1 3.195(4) . . ? N22 Cl2 3.385(4) . . ? N22 O01 2.826(6) . . ? N22 H21a 1.99(4) . . ? N22 H21b 1.99(4) . . ? N22 H23a 1.83(4) . . ? N22 H23b 2.08(4) . . ? N22 H24b 2.67(5) . . ? C23 C25 2.563(6) . . ? C23 Cl1 3.397(5) . . ? C23 H21a 2.60(4) . . ? C23 H21b 2.60(4) . . ? C23 H22a 1.98(4) . . ? C23 H22b 1.93(4) . . ? C23 H24a 1.92(5) . . ? C23 H24b 2.02(5) . . ? C24 N26 2.485(6) . . ? C24 H22a 2.58(4) . . ? C24 H22b 2.69(4) . . ? C24 H23a 1.95(5) . . ? C24 H23b 2.23(4) . . ? C24 H25a 1.96(4) . . ? C24 H25b 2.11(4) . . ? C24 H26b 2.69(4) . . ? C24 H26c 2.57(4) . . ? C25 Cl1 3.496(4) . '7 666' ? C25 H24a 1.92(5) . . ? C25 H24b 1.90(5) . . ? C25 H26a 2.09(6) . . ? C25 H26b 2.00(4) . . ? C25 H26c 1.92(4) . . ? N26 Cl1 3.187(4) . . ? N26 Cl1 3.267(4) . '7 666' ? N26 Cl2 3.320(4) . '7 666' ? N26 Cl3 3.129(4) . '7 666' ? N26 H25a 1.89(4) . . ? N26 H25b 2.07(4) . . ? N26 H24a 2.56(5) . . ? Cl1 Cl2 3.843(2) . . ? Cl1 Cl5 3.955(5) . . ? Cl1 H12a 2.26(4) . . ? Cl1 H13a 3.16(4) . . ? Cl1 H14a 3.05(4) . . ? Cl1 H15a 2.91(5) . '4 565' ? Cl1 H21a 3.11(4) . . ? Cl1 H22b 2.65(4) . . ? Cl1 H23b 2.76(4) . . ? Cl1 H26a 2.31(6) . '7 666' ? Cl1 H26b 2.49(4) . . ? Cl2 H11a 2.62(3) . . ? Cl2 H16a 3.10(6) . '4 564' ? Cl2 H16b 2.98(6) . '4 564' ? Cl2 H16c 2.21(6) . '6 655' ? Cl2 H22a 3.19(4) . . ? Cl2 H22b 2.73(4) . . ? Cl2 H25b 2.75(4) . . ? Cl2 H26a 2.73(6) . '7 666' ? Cl3 O02 3.057(5) . '8 564' ? Cl3 H13a 3.06(4) . . ? Cl3 H15b 2.99(4) . . ? Cl3 H16a 2.41(6) . '4 564' ? Cl3 H25a 2.93(4) . '6 645' ? Cl3 H26c 2.36(4) . '7 666' ? Cl3 H02b 1.9674(14) . '8 564' ? Cl4 O01 2.996(5) . '3 676' ? Cl4 O01 2.996(5) . '4 575' ? Cl4 O02 2.908(5) . . ? Cl4 O02 2.908(5) . '2 656' ? Cl4 H01a 2.057(3) . '4 575' ? Cl4 H01a 2.057(3) . '3 676' ? Cl4 H01b 3.090(2) . '3 676' ? Cl4 H01b 3.090(2) . '4 575' ? Cl4 H02a 2.0035(14) . . ? Cl4 H02a 2.0035(14) . '2 656' ? Cl5 Cl5 3.905(8) . '2 656' ? Cl5 O04 3.060(13) . . ? Cl5 O05 2.816(17) . '3 666' ? Cl5 O05 3.169(16) . '2 656' ? Cl5 O06 2.638(16) . '2 656' ? Cl5 O06 3.568(16) . '3 666' ? Cl5 H11b 2.74(4) . '4 565' ? Cl5 H11b 2.69(3) . '2 655' ? Cl5 H12a 2.81(5) . . ? Cl5 H12b 2.45(4) . '3 666' ? Cl5 H12b 2.70(4) . . ? Cl5 H13b 2.75(4) . '4 565' ? Cl5 H14b 2.83(5) . '3 666' ? Cl5 H21a 2.93(4) . . ? O01 O01 3.010(7) . '2 655' ? O01 O02 2.726(7) . '2 655' ? O01 H21b 2.55(4) . '2 655' ? O01 H22a 1.95(4) . . ? O01 H23a 2.78(4) . '2 655' ? O01 H01a 2.566(5) . '2 655' ? O02 O03 2.731(8) . '2 656' ? O03 O04 2.700(9) . . ? O03 H16b 2.04(6) . '4 565' ? O04 O05 2.25(2) . '2 656' ? O04 O05 2.25(2) . . ? O04 H03a 2.575(3) . . ? O04 H03a 2.575(3) . '2 656' ? O04 H03b 1.829(5) . '2 656' ? O04 H03b 1.829(5) . . ? O05 O05 2.37(2) . '2 656' ? O05 H12b 2.54(4) . '3 666' ? O05 H13b 2.64(4) . '4 565' ? O05 H14b 2.78(5) . '3 666' ? O06 H03b 2.714(13) . . ? O06 H03b 2.780(14) . '2 656' ? H11a H11b 1.41(5) . . ? H11a H12a 2.13(6) . . ? H11a H13a 2.36(5) . . ? H11a H21b 2.34(5) . '2 655' ? H11a H22b 2.39(5) . . ? H11b H12b 2.17(5) . . ? H11b H13b 2.36(5) . . ? H11b H21a 2.33(5) . '2 655' ? H12a H12b 1.18(6) . . ? H12a H13a 2.14(6) . . ? H12a H21a 2.40(6) . . ? H12b H13a 2.36(6) . . ? H12b H13b 2.11(6) . . ? H12b H14b 2.35(6) . . ? H13a H13b 1.57(6) . . ? H13a H14a 2.24(6) . . ? H13b H14b 2.38(6) . . ? H14a H14b 1.57(6) . . ? H14b H15a 2.36(7) . . ? H15a H15b 1.39(6) . . ? H15a H16b 2.18(8) . . ? H15a H16c 2.30(7) . . ? H15b H16a 2.06(7) . . ? H15b H16c 2.04(7) . . ? H16a H16b 1.48(9) . . ? H16a H16c 1.34(9) . . ? H16b H16c 1.52(9) . . ? H16b H03a 2.01(6) . '4 564' ? H21a H21b 1.51(5) . . ? H21a H22b 2.25(6) . . ? H21a H23b 2.36(6) . . ? H21b H22a 2.39(5) . '2 655' ? H21b H22a 2.34(6) . . ? H21b H23a 2.29(6) . . ? H22a H22b 1.28(6) . . ? H22a H23a 2.20(6) . . ? H22a H01b 2.25(4) . . ? H22b H23b 2.29(6) . . ? H22b H25b 2.37(5) . . ? H23a H23b 1.50(6) . . ? H23a H24a 2.18(7) . . ? H23a H24b 2.30(7) . . ? H25a H25b 1.66(6) . . ? H25a H24a 2.17(7) . . ? H25a H24b 2.11(7) . . ? H25a H26a 2.22(7) . . ? H25a H26c 2.17(6) . . ? H25b H24b 2.33(7) . . ? H25b H26b 2.39(6) . . ? H24a H24b 1.39(7) . . ? H24a H26c 2.38(6) . . ? H26a H26b 1.67(7) . . ? H26a H26c 1.59(8) . . ? H26b H26c 1.25(6) . . ? H01a H01a 1.9075(5) . '2 655' ? H01a H01b 1.4978(4) . . ? H02a H02b 1.6192(4) . . ? H03a H03b 1.3723(5) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1684 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 11 9 6 11 -9 6 -11 9 6 11 9 -6 -11 -9 -6 -11 9 -6 -11 -9 6 11 -9 -6 0 18 0 0 -18 0 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 28 _reflns_limit_k_min -22 _reflns_limit_k_max 22 _reflns_limit_l_min -13 _reflns_limit_l_max 13 _reflns_d_resolution_high ? _reflns_d_resolution_low ? _diffrn_reflns_av_sigmaI/netI .038 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_reduction_process perpendicular_monochr_Lp _diffrn_ambient_temperature 293 _diffrn_radiation_source 'totating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'single counter' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .0769 _refine_ls_wR_factor_all .0690 _refine_ls_goodness_of_fit_all 1.856 _refine_ls_shift/su_mean .00439 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END data_ykcua _audit_creation_date 98-01-27 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? #ActaC _chemical_name_systematic ? #ActaC _chemical_name_common ? #ActaC _chemical_formula_analytical ? #ActaC _chemical_formula_moiety ? #ActaC _chemical_formula_structural ? #ActaC _chemical_formula_sum 'C17 H48 Cl4 Cu2 N8 O2' #ActaC _chemical_formula_weight 665.53 #ActaC _chemical_melting_point ? #ActaC _computing_data_collection 'Enraf Nonius software' #ActaC _computing_cell_refinement 'Enraf Nonius software' #ActaC _computing_data_reduction xtal_DIFDAT_ABSORB_SORTRF_ADDREF #ActaC _computing_structure_solution xtal #ActaC _computing_structure_refinement xtal_CRYLSQ #ActaC _computing_molecular_graphics xtal #ActaC _computing_publication_material xtal_BONDLA_CIFIO #ActaC _cell_length_a 12.531(4) #ActaC _cell_length_b 12.271(2) #ActaC _cell_length_c 10.075(2) #ActaC _cell_angle_alpha 99.220(10) #ActaC _cell_angle_beta 112.61(2) #ActaC _cell_angle_gamma 90.64(2) #ActaC _cell_volume 1407.2(6) #ActaC _cell_formula_units_Z 2 #ActaC _cell_measurement_temperature 293 #ActaC _cell_measurement_reflns_used 18 #ActaC _cell_measurement_theta_min 16.1 #ActaC _cell_measurement_theta_max 25.1 #ActaC _cell_special_details #ActaC ; ? ; _symmetry_cell_setting triclinic #ActaC _symmetry_space_group_name_H-M p_-1 #ActaC _symmetry_space_group_name_Hall -p_1 #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +x,+y,+z -x,-y,-z _exptl_crystal_description block #ActaC _exptl_crystal_preparation ? _exptl_crystal_colour blue #ActaC _exptl_crystal_size_max 0.75 #ActaC _exptl_crystal_size_mid 0.65 #ActaC _exptl_crystal_size_min 0.48 #ActaC _exptl_crystal_density_diffrn 1.571 #ActaC _exptl_crystal_density_meas ? #ActaC _exptl_crystal_density_method ? #ActaC _exptl_crystal_F_000 696 #ActaC _exptl_absorpt_process_details 'XTAL absorb' _exptl_absorpt_coefficient_mu 1.92 #ActaC _exptl_absorpt_correction_type gaussian #ActaC _exptl_absorpt_correction_T_min 0.28 #ActaC _exptl_absorpt_correction_T_max 0.47 #ActaC _exptl_special_details #ActaC ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 #ActaC _diffrn_radiation_wavelength 0.71073 #ActaC _diffrn_radiation_type Mo-K\a #ActaC _diffrn_radiation_source 'rotating anode' #ActaC _diffrn_radiation_monochromator graphite #ActaC _diffrn_radiation_detector 'single counter' #ActaC _diffrn_measurement_device CAD4 #ActaC _diffrn_measurement_method '2\q-\w scans' #ActaC _diffrn_standards_number 8 #ActaC _diffrn_standards_interval_count ? #ActaC _diffrn_standards_interval_time 60 #ActaC _diffrn_standards_decay_% 0 #ActaC loop_ _diffrn_standard_refln_index_h #ActaC _diffrn_standard_refln_index_k #ActaC _diffrn_standard_refln_index_l #ActaC 7 7 5 -7 -7 -5 9 0 0 -9 0 0 0 14 0 0 -14 0 0 0 8 0 0 -8 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 7815 #ActaC _diffrn_reflns_av_R_equivalents .026 #ActaC _diffrn_reflns_av_sigmaI/netI .031 #ActaC _diffrn_reflns_limit_h_min -16 #ActaC _diffrn_reflns_limit_h_max 2 #ActaC _diffrn_reflns_limit_k_min -16 #ActaC _diffrn_reflns_limit_k_max 16 #ActaC _diffrn_reflns_limit_l_min -12 #ActaC _diffrn_reflns_limit_l_max 13 #ActaC _diffrn_reflns_theta_min 1.69 #ActaC _diffrn_reflns_theta_max 27.98 #ActaC _diffrn_reflns_reduction_process perpendicular_monochr_Lp #ActaC loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC C ? 0 34 .002 .002 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 96 0 0 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 Cl ? 0 8 .132 .159 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 Cu ? 0 4 .263 1.266 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 N ? 0 16 .004 .003 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 O ? 0 4 .008 .006 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC Cu1 1.25830(4) .81649(3) .90877(5) .0325(2) Uani ? ? Cu2 .70616(3) .66903(3) .88641(5) .03088(19) Uani ? ? Cl1 1.34251(8) .62153(8) .85537(13) .0494(5) Uani ? ? Cl2 .60788(9) .86175(7) .91212(12) .0445(4) Uani ? ? Cl3 .92380(11) .95269(9) 1.23887(13) .0572(5) Uani ? ? Cl4 .75045(10) .41169(10) .77352(14) .0656(6) Uani ? ? C0 .9839(3) .7471(3) .9029(4) .0303(13) Uani ? ? C11 1.0663(3) .8422(3) 1.0108(4) .0314(14) Uani ? ? N12 1.1907(2) .8176(2) 1.0686(3) .0289(12) Uani ? ? C13 1.2560(3) .9051(3) 1.1971(4) .0393(17) Uani ? ? C14 1.3767(4) .8768(4) 1.2869(5) .047(2) Uani ? ? C15 1.4427(4) .8270(5) 1.1971(6) .059(3) Uani ? ? N16 1.4147(3) .8685(4) 1.0629(4) .0497(18) Uani ? ? C21 1.0355(3) .6900(3) .7962(5) .0369(16) Uani ? ? N22 1.0989(3) .7682(3) .7500(3) .0347(13) Uani ? ? C23 1.0991(4) .7199(4) .6056(5) .051(2) Uani ? ? C24 1.1450(5) .8017(5) .5400(6) .059(3) Uani ? ? C25 1.2734(5) .8373(6) .6206(6) .066(3) Uani ? ? N26 1.3004(4) .8953(4) .7705(5) .055(2) Uani ? ? C31 .9595(3) .6582(3) .9804(5) .0342(15) Uani ? ? N32 .8733(2) .6870(2) 1.0462(3) .0328(12) Uani ? ? C33 .8827(3) .6140(3) 1.1535(5) .0419(17) Uani ? ? C34 .8240(4) .6559(4) 1.2551(5) .0443(18) Uani ? ? C35 .7021(4) .6876(4) 1.1792(5) .050(2) Uani ? ? N36 .6443(3) .6238(3) 1.0295(4) .0390(15) Uani ? ? C41 .8720(3) .7980(3) .8209(4) .0314(14) Uani ? ? N42 .7705(2) .7148(2) .7425(3) .0314(12) Uani ? ? C43 .6855(4) .7549(4) .6131(5) .0440(18) Uani ? ? C44 .5867(4) .6695(4) .5214(5) .050(2) Uani ? ? C45 .5043(3) .6500(4) .5923(5) .0461(19) Uani ? ? N46 .5590(3) .5962(3) .7211(4) .0411(16) Uani ? ? O01 .8547(4) .9140(3) .5036(4) .092(2) Uani ? ? O02 .8020(4) .5054(3) .5357(5) .102(3) Uani ? ? H11a 1.046(3) .869(3) 1.094(4) .035(10) Uiso ? ? H11b 1.062(3) .910(3) .961(4) .035(10) Uiso ? ? H12 1.201(3) .754(3) 1.104(4) .028(9) Uiso ? ? H13a 1.203(3) .919(3) 1.259(4) .046(11) Uiso ? ? H13b 1.249(3) .973(3) 1.162(4) .048(12) Uiso ? ? H14a 1.370(4) .815(4) 1.337(5) .071(15) Uiso ? ? H14b 1.414(4) .939(4) 1.337(5) .057(14) Uiso ? ? H15a 1.513(4) .841(3) 1.250(4) .076(17) Uiso ? ? H15b 1.426(3) .746(5) 1.167(4) .13(3) Uiso ? ? H16a 1.452(4) .835(4) 1.015(5) .061(15) Uiso ? ? H16b 1.419(5) .954(5) 1.094(7) .13(2) Uiso ? ? H21a .976(3) .644(3) .705(4) .045(11) Uiso ? ? H21b 1.086(3) .637(3) .839(4) .036(10) Uiso ? ? H22 1.061(3) .830(3) .736(4) .046(12) Uiso ? ? H23a 1.014(4) .699(4) .533(5) .067(14) Uiso ? ? H23b 1.135(3) .662(3) .614(4) .039(11) Uiso ? ? H24a 1.090(4) .868(4) .533(5) .074(15) Uiso ? ? H24b 1.128(4) .771(4) .454(5) .070(16) Uiso ? ? H25a 1.293(4) .890(4) .579(6) .081(17) Uiso ? ? H25b 1.300(4) .774(4) .623(5) .060(15) Uiso ? ? H26a 1.262(4) .960(4) .762(5) .072(16) Uiso ? ? H26b 1.366(4) .914(4) .820(5) .069(18) Uiso ? ? H31a 1.028(3) .645(3) 1.054(4) .036(10) Uiso ? ? H31b .933(3) .600(3) .921(4) .018(9) Uiso ? ? H32 .888(3) .763(3) 1.104(3) .021(8) Uiso ? ? H33a .963(4) .616(3) 1.212(4) .052(12) Uiso ? ? H33b .843(3) .534(3) 1.083(4) .043(11) Uiso ? ? H34a .871(4) .724(3) 1.329(5) .054(12) Uiso ? ? H34b .825(3) .605(3) 1.301(4) .044(12) Uiso ? ? H35a .707(4) .764(4) 1.168(5) .066(14) Uiso ? ? H35b .665(3) .673(3) 1.240(4) .040(11) Uiso ? ? H36a .580(4) .639(3) .994(4) .042(12) Uiso ? ? H36b .650(3) .552(3) 1.027(4) .034(10) Uiso ? ? H41a .889(3) .839(3) .751(4) .037(10) Uiso ? ? H41b .857(3) .849(3) .895(4) .035(10) Uiso ? ? H42 .798(3) .656(3) .714(4) .047(12) Uiso ? ? H43a .729(4) .769(3) .555(5) .063(14) Uiso ? ? H43b .659(3) .821(3) .649(4) .034(10) Uiso ? ? H44a .622(3) .594(3) .493(4) .048(11) Uiso ? ? H44b .545(4) .689(4) .433(6) .078(16) Uiso ? ? H45a .439(4) .606(3) .522(5) .065(14) Uiso ? ? H45b .484(3) .720(3) .630(4) .036(10) Uiso ? ? H46a .578(4) .527(4) .693(5) .075(17) Uiso ? ? H46b .521(3) .589(3) .755(4) .027(11) Uiso ? ? loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC Cu1 .0239(2) .0385(2) .0404(3) .00184(17) .0174(2) .0093(2) Cu2 .0199(2) .0394(2) .0355(3) .00137(17) .01025(18) .01440(19) Cl1 .0339(5) .0479(5) .0736(7) .0072(4) .0232(5) .0249(5) Cl2 .0443(5) .0380(5) .0631(7) .0068(4) .0320(5) .0132(4) Cl3 .0738(8) .0528(6) .0599(7) .0144(5) .0420(6) .0100(5) Cl4 .0502(7) .0568(7) .0710(8) .0090(5) -.0007(6) .0218(6) C0 .0190(15) .0310(16) .043(2) .0041(13) .0135(15) .0102(15) C11 .0216(17) .0325(17) .046(2) .0039(14) .0191(16) .0076(16) N12 .0221(14) .0303(14) .0387(17) .0023(11) .0155(13) .0090(13) C13 .031(2) .045(2) .043(2) .0013(16) .0173(18) .0023(18) C14 .036(2) .060(3) .041(2) -.002(2) .013(2) .000(2) C15 .030(2) .090(4) .062(3) .016(2) .017(2) .027(3) N16 .035(2) .065(3) .055(2) .0006(17) .0268(18) .004(2) C21 .0251(18) .0359(19) .052(2) .0029(15) .0182(18) .0056(18) N22 .0282(16) .0406(17) .0408(18) .0091(13) .0177(14) .0109(14) C23 .047(3) .063(3) .043(3) .014(2) .020(2) .005(2) C24 .062(3) .085(4) .043(3) .022(3) .030(3) .021(3) C25 .059(3) .091(4) .077(4) .028(3) .048(3) .042(3) N26 .040(2) .069(3) .066(3) .004(2) .026(2) .031(2) C31 .0222(17) .0310(19) .052(2) .0055(15) .0146(17) .0124(18) N32 .0229(14) .0365(16) .0416(18) .0038(12) .0120(13) .0157(14) C33 .030(2) .049(2) .048(2) .0052(17) .0104(18) .026(2) C34 .043(2) .054(3) .036(2) -.001(2) .0114(19) .020(2) C35 .054(3) .063(3) .044(2) .015(2) .027(2) .022(2) N36 .0276(17) .049(2) .046(2) .0057(15) .0137(16) .0228(16) C41 .0239(17) .0312(17) .044(2) .0061(14) .0164(16) .0140(16) N42 .0232(14) .0344(16) .0387(17) .0053(12) .0126(13) .0109(13) C43 .033(2) .059(3) .043(2) .0050(19) .0127(19) .022(2) C44 .036(2) .074(3) .035(2) .005(2) .0076(19) .013(2) C45 .025(2) .059(3) .045(2) .0037(19) .0052(18) .005(2) N46 .0284(18) .052(2) .042(2) -.0048(15) .0141(16) .0053(16) O01 .112(3) .087(3) .104(3) -.012(2) .071(3) .023(2) O02 .105(3) .075(3) .143(4) .006(2) .076(3) .001(3) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_special_details sfls__F____sigma_weight______full_matrix _refine_ls_structure_factor_coef F #ActaC _refine_ls_matrix_type full #ActaC _refine_ls_weighting_scheme sigma #ActaC _refine_ls_hydrogen_treatment mixed #ActaC _refine_ls_extinction_method Zachariasen #ActaC _refine_ls_extinction_coef 1846(245) #ActaC _refine_ls_extinction_expression Eq22_p292_"Cryst._Comp."_Munksgaard_1970 _refine_ls_abs_structure_details none #ActaC _refine_ls_abs_structure_Flack ? #ActaC _refine_ls_number_reflns 5569 #ActaC _refine_ls_number_parameters 475 #ActaC _refine_ls_number_restraints 5 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all .059 #ActaC _refine_ls_R_factor_gt .047 #ActaC _refine_ls_wR_factor_all .053 #ActaC _refine_ls_wR_factor_ref .052 #ActaC _refine_ls_goodness_of_fit_all 2.085 #ActaC _refine_ls_goodness_of_fit_ref 2.262 #ActaC _refine_ls_shift/su_max .097 #ActaC _refine_ls_shift/su_mean .005 #ActaC _refine_diff_density_min -.535 #ActaC _refine_diff_density_max .912 #ActaC _geom_special_details ? #ActaC loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC Cu1 Cl1 2.6846(12) . . ? Cu1 N12 2.086(4) . . ? Cu1 N16 1.994(3) . . ? Cu1 N22 2.028(3) . . ? Cu1 N26 2.035(6) . . ? Cu2 Cl2 2.7001(11) . . ? Cu2 N32 2.076(3) . . ? Cu2 N36 2.023(5) . . ? Cu2 N42 2.054(4) . . ? Cu2 N46 2.025(3) . . ? C0 C11 1.521(4) . . ? C0 C21 1.539(6) . . ? C0 C31 1.531(6) . . ? C0 C41 1.527(5) . . ? C11 N12 1.494(4) . . ? C11 H11a .98(4) . . ? C11 H11b 1.03(4) . . ? N12 C13 1.490(4) . . ? N12 H12 .90(4) . . ? C13 C14 1.512(6) . . ? C13 H13a 1.06(5) . . ? C13 H13b .94(4) . . ? C14 C15 1.512(8) . . ? C14 H14a 1.00(5) . . ? C14 H14b .87(4) . . ? C15 N16 1.439(7) . . ? C15 H15a .83(5) . . ? C15 H15b .99(6) . . ? N16 H16a .86(6) . . ? N16 H16b 1.05(6) . . ? C21 N22 1.476(6) . . ? C21 H21a 1.01(3) . . ? C21 H21b .94(4) . . ? N22 C23 1.482(6) . . ? N22 H22 .91(4) . . ? C23 C24 1.505(9) . . ? C23 H23a 1.04(4) . . ? C23 H23b .84(4) . . ? C24 C25 1.519(7) . . ? C24 H24a 1.06(5) . . ? C24 H24b .83(5) . . ? C25 N26 1.470(8) . . ? C25 H25a .91(6) . . ? C25 H25b .85(5) . . ? N26 H26a .94(5) . . ? N26 H26b .78(5) . . ? C31 N32 1.488(6) . . ? C31 H31a .92(3) . . ? C31 H31b .83(3) . . ? N32 C33 1.484(6) . . ? N32 H32 .99(3) . . ? C33 C34 1.508(7) . . ? C33 H33a .95(4) . . ? C33 H33b 1.10(3) . . ? C34 C35 1.510(6) . . ? C34 H34a 1.03(4) . . ? C34 H34b .83(5) . . ? C35 N36 1.477(5) . . ? C35 H35a .96(5) . . ? C35 H35b .94(5) . . ? N36 H36a .78(4) . . ? N36 H36b .88(4) . . ? C41 N42 1.491(4) . . ? C41 H41a 1.01(4) . . ? C41 H41b .97(4) . . ? N42 C43 1.491(5) . . ? N42 H42 .86(4) . . ? C43 C44 1.506(6) . . ? C43 H43a .97(6) . . ? C43 H43b .95(4) . . ? C44 C45 1.500(8) . . ? C44 H44a 1.07(4) . . ? C44 H44b .92(5) . . ? C45 N46 1.479(6) . . ? C45 H45a .94(4) . . ? C45 H45b .96(4) . . ? N46 H46a .92(5) . . ? N46 H46b .70(5) . . ? loop_ _geom_contact_atom_site_label_1 #ActaC _geom_contact_atom_site_label_2 #ActaC _geom_contact_distance #ActaC _geom_contact_site_symmetry_1 #ActaC _geom_contact_site_symmetry_2 #ActaC _geom_contact_publ_flag #ActaC Cu1 Cl2 4.1109(11) . 2_777 ? Cu1 Cl2 4.3960(19) . 1_655 ? Cu1 Cl3 3.7850(14) . 2_777 ? Cu1 C0 3.509(4) . . ? Cu1 C11 2.960(4) . . ? Cu1 C13 2.945(5) . . ? Cu1 C14 3.463(4) . . ? Cu1 C15 2.917(4) . . ? Cu1 C21 2.897(4) . . ? Cu1 C23 2.969(4) . . ? Cu1 C24 3.402(5) . . ? Cu1 C25 3.031(7) . . ? Cu1 H11b 2.92(4) . . ? Cu1 H12 2.56(4) . . ? Cu1 H13b 2.97(4) . . ? Cu1 H15b 2.91(4) . . ? Cu1 H16a 2.24(5) . . ? Cu1 H16b 2.53(5) . . ? Cu1 H21b 2.87(4) . . ? Cu1 H22 2.44(4) . . ? Cu1 H23b 3.07(3) . . ? Cu1 H25b 3.08(6) . . ? Cu1 H26a 2.49(6) . . ? Cu1 H26b 2.30(6) . . ? Cu2 Cl4 3.3086(13) . . ? Cu2 C0 3.534(4) . . ? Cu2 C31 2.955(4) . . ? Cu2 C33 2.938(4) . . ? Cu2 C34 3.462(4) . . ? Cu2 C35 2.942(5) . . ? Cu2 C41 2.928(4) . . ? Cu2 C43 3.025(5) . . ? Cu2 C44 3.397(5) . . ? Cu2 C45 3.039(4) . . ? Cu2 H31b 2.88(4) . . ? Cu2 H32 2.57(3) . . ? Cu2 H33b 2.84(4) . . ? Cu2 H35a 2.89(5) . . ? Cu2 H36a 2.29(5) . . ? Cu2 H36b 2.44(4) . . ? Cu2 H41b 2.86(4) . . ? Cu2 H42 2.41(5) . . ? Cu2 H43b 3.15(4) . . ? Cu2 H45b 3.14(3) . . ? Cu2 H46a 2.42(4) . . ? Cu2 H46b 2.30(4) . . ? Cl1 N16 3.290(4) . . ? Cl1 N22 3.454(3) . . ? Cl1 C23 3.500(5) . . ? Cl1 N36 3.379(4) . 2_767 ? Cl1 N46 3.463(5) . 1_655 ? Cl1 H15b 3.03(4) . . ? Cl1 H16a 2.86(4) . . ? Cl1 H21b 3.17(4) . . ? Cl1 H23b 2.91(4) . . ? Cl1 H25b 3.12(5) . . ? Cl1 H36a 2.75(4) . 1_655 ? Cl1 H36b 2.59(4) . 2_767 ? Cl1 H46b 2.79(5) . 1_655 ? Cl2 N16 3.311(5) . 1_455 ? Cl2 N16 3.303(4) . 2_777 ? Cl2 N36 3.294(4) . . ? Cl2 N42 3.478(4) . . ? Cl2 N46 3.426(4) . . ? Cl2 H13b 3.05(5) . 2_777 ? Cl2 H16a 2.57(6) . 1_455 ? Cl2 H16b 2.29(7) . 2_777 ? Cl2 H26b 2.93(5) . 1_455 ? Cl2 H35a 2.86(5) . . ? Cl2 H36a 3.04(4) . . ? Cl2 H41b 3.20(4) . . ? Cl2 H43b 2.93(4) . . ? Cl2 H45b 2.91(3) . . ? Cl3 N22 3.427(3) . 2_777 ? Cl3 N26 3.369(5) . 2_777 ? Cl3 N32 3.432(3) . . ? Cl3 O01 3.204(5) . 1_556 ? Cl3 O01 3.180(4) . 2_777 ? Cl3 H11a 2.60(4) . . ? Cl3 H11b 2.88(4) . 2_777 ? Cl3 H22 2.63(4) . 2_777 ? Cl3 H24a 2.98(5) . 2_777 ? Cl3 H26a 2.57(6) . 2_777 ? Cl3 H32 2.45(3) . . ? Cl4 N12 3.401(3) . 2_767 ? Cl4 N46 3.270(4) . . ? Cl4 O02 3.088(6) . . ? Cl4 H12 2.51(4) . 2_767 ? Cl4 H14a 2.98(5) . 2_767 ? Cl4 H15b 3.20(6) . 2_767 ? Cl4 H31a 2.82(4) . 2_767 ? Cl4 H31b 2.99(3) . . ? Cl4 H33b 3.00(4) . . ? Cl4 H45a 2.98(4) . 2_666 ? Cl4 H46a 2.53(5) . . ? C0 N12 2.532(4) . . ? C0 N22 2.519(6) . . ? C0 N32 2.531(6) . . ? C0 N42 2.524(4) . . ? C0 H11a 2.11(3) . . ? C0 H11b 2.11(3) . . ? C0 H12 2.68(3) . . ? C0 H21a 2.15(4) . . ? C0 H21b 2.06(4) . . ? C0 H22 2.56(5) . . ? C0 H31a 2.04(4) . . ? C0 H31b 1.97(3) . . ? C0 H41a 2.05(4) . . ? C0 H41b 2.02(4) . . ? C0 H42 2.48(3) . . ? C11 C13 2.415(4) . . ? C11 C21 2.522(5) . . ? C11 N22 2.823(6) . . ? C11 C31 2.526(5) . . ? C11 C41 2.437(4) . . ? C11 H12 2.01(3) . . ? C11 H13a 2.45(3) . . ? C11 H13b 2.56(4) . . ? C11 H31a 2.59(4) . . ? C11 H41a 2.70(3) . . ? C11 H41b 2.44(3) . . ? N12 C14 2.511(4) . . ? N12 C15 2.909(5) . . ? N12 N16 2.893(5) . . ? N12 C21 2.866(4) . . ? N12 N22 2.919(4) . . ? N12 H11a 2.03(4) . . ? N12 H11b 2.04(3) . . ? N12 H13a 2.06(4) . . ? N12 H13b 1.97(4) . . ? C13 C15 2.539(7) . . ? C13 N16 2.807(7) . . ? C13 H11a 2.44(4) . . ? C13 H11b 2.67(3) . . ? C13 H12 1.93(3) . . ? C13 H14a 2.06(5) . . ? C13 H14b 1.93(4) . . ? C14 N16 2.467(7) . . ? C14 H12 2.54(3) . . ? C14 H13a 2.16(4) . . ? C14 H13b 2.12(4) . . ? C14 H15a 1.92(6) . . ? C14 H15b 2.10(6) . . ? C14 H16b 2.52(8) . . ? C15 H14a 1.97(6) . . ? C15 H14b 1.94(5) . . ? C15 H16a 1.91(6) . . ? C15 H16b 1.98(7) . . ? N16 N26 2.814(6) . . ? N16 H15a 1.90(4) . . ? N16 H15b 1.95(6) . . ? N16 H26b 2.45(6) . . ? C21 C23 2.420(8) . . ? C21 C31 2.467(7) . . ? C21 C41 2.523(6) . . ? C21 H22 1.97(4) . . ? C21 H23a 2.58(5) . . ? C21 H23b 2.57(5) . . ? C21 H31b 2.47(4) . . ? C21 H41a 2.57(4) . . ? N22 C24 2.487(8) . . ? N22 N26 2.874(6) . . ? N22 H21a 2.02(4) . . ? N22 H21b 1.99(4) . . ? N22 H23a 2.06(4) . . ? N22 H23b 1.92(4) . . ? N22 H24a 2.64(6) . . ? C23 C25 2.544(9) . . ? C23 H21a 2.39(5) . . ? C23 H22 1.93(4) . . ? C23 H24a 2.05(5) . . ? C23 H24b 1.90(6) . . ? C23 H25b 2.53(5) . . ? C24 N26 2.475(6) . . ? C24 H22 2.56(5) . . ? C24 H23a 2.03(5) . . ? C24 H23b 2.00(4) . . ? C24 H25a 2.01(5) . . ? C24 H25b 1.86(5) . . ? C24 H26a 2.64(4) . . ? C25 H24a 2.18(5) . . ? C25 H24b 1.99(4) . . ? C25 H26a 1.95(5) . . ? C25 H26b 1.96(4) . . ? N26 H16a 2.69(4) . . ? N26 H25a 1.89(6) . . ? N26 H25b 1.92(5) . . ? C31 C33 2.418(8) . . ? C31 C41 2.510(6) . . ? C31 N42 2.836(5) . . ? C31 H11a 2.69(3) . . ? C31 H21b 2.50(5) . . ? C31 H32 2.09(4) . . ? C31 H33a 2.46(5) . . ? C31 H33b 2.67(5) . . ? C31 H42 2.66(4) . . ? N32 C34 2.492(7) . . ? N32 C35 2.934(7) . . ? N32 N36 2.899(5) . . ? N32 C41 2.823(6) . . ? N32 N42 2.908(5) . . ? N32 H31a 1.98(4) . . ? N32 H31b 1.90(4) . . ? N32 H33a 1.97(4) . . ? N32 H33b 2.03(4) . . ? N32 H41b 2.66(4) . . ? C33 C35 2.536(7) . . ? C33 N36 2.773(5) . . ? C33 H31a 2.44(5) . . ? C33 H31b 2.63(4) . . ? C33 H32 1.98(3) . . ? C33 H34a 2.10(4) . . ? C33 H34b 1.91(5) . . ? C34 N36 2.480(5) . . ? C34 H32 2.50(4) . . ? C34 H33a 2.00(5) . . ? C34 H33b 2.19(4) . . ? C34 H35a 2.02(4) . . ? C34 H35b 1.96(4) . . ? C34 H36b 2.61(3) . . ? C35 H34a 2.07(4) . . ? C35 H34b 1.97(4) . . ? C35 H36a 1.90(3) . . ? C35 H36b 1.99(3) . . ? N36 N46 2.831(5) . . ? N36 H33b 2.63(4) . . ? N36 H35a 1.97(4) . . ? N36 H35b 2.02(4) . . ? N36 H46b 2.55(4) . . ? C41 C43 2.445(5) . . ? C41 H11b 2.51(3) . . ? C41 H21a 2.68(4) . . ? C41 H42 1.91(4) . . ? C41 H43a 2.55(4) . . ? C41 H43b 2.61(3) . . ? N42 C44 2.491(4) . . ? N42 N46 2.927(5) . . ? N42 H41a 2.08(4) . . ? N42 H41b 2.03(3) . . ? N42 H43a 1.99(5) . . ? N42 H43b 1.99(4) . . ? N42 H44a 2.66(3) . . ? C43 C45 2.519(7) . . ? C43 H41a 2.50(3) . . ? C43 H42 1.96(4) . . ? C43 H44a 2.11(4) . . ? C43 H44b 2.02(4) . . ? C43 H45b 2.64(4) . . ? C44 N46 2.467(7) . . ? C44 H42 2.64(4) . . ? C44 H43a 2.03(5) . . ? C44 H43b 2.06(3) . . ? C44 H45a 2.00(5) . . ? C44 H45b 2.03(5) . . ? C44 H46a 2.68(6) . . ? C45 H43b 2.68(4) . . ? C45 H44a 2.14(5) . . ? C45 H44b 1.99(6) . . ? C45 H46a 2.00(5) . . ? C45 H46b 1.85(4) . . ? N46 H36a 2.63(5) . . ? N46 H44a 2.69(5) . . ? N46 H45a 2.01(4) . . ? N46 H45b 1.96(4) . . ? O01 H41a 2.68(4) . . ? O01 H43a 2.61(5) . . ? O02 H21a 2.59(3) . . ? O02 H23b 2.66(4) . 2_766 ? O02 H42 2.38(4) . . ? O02 H44a 2.43(4) . . ? H11a H11b 1.59(6) . . ? H11a H12 2.40(5) . . ? H11a H13a 2.04(4) . . ? H11a H32 2.39(6) . . ? H11b H22 2.32(6) . . ? H12 H13a 2.35(5) . . ? H12 H31a 2.37(5) . . ? H13a H13b 1.53(7) . . ? H13a H14a 2.39(6) . . ? H13b H14b 2.24(5) . . ? H14a H14b 1.62(7) . . ? H14a H15a 2.32(8) . . ? H14a H15b 2.15(7) . . ? H14b H15a 2.07(7) . . ? H15a H15b 1.49(6) . . ? H15a H16a 2.18(6) . . ? H15a H16b 2.26(7) . . ? H15b H16a 2.14(8) . . ? H16a H16b 1.69(8) . . ? H16a H26b 2.23(7) . . ? H21a H21b 1.52(5) . . ? H21a H23a 2.17(8) . . ? H21a H42 2.28(7) . . ? H22 H23a 2.26(6) . . ? H22 H24a 2.33(8) . . ? H22 H41a 2.22(6) . . ? H23a H23b 1.54(6) . . ? H23a H24a 2.27(7) . . ? H23a H24b 2.13(8) . . ? H23a H34a 2.21(6) . 1_554 ? H23b H24b 2.24(7) . . ? H24a H24b 1.51(7) . . ? H24b H25a 2.31(6) . . ? H24b H25b 2.17(6) . . ? H25a H25b 1.56(7) . . ? H25a H26a 2.09(8) . . ? H25a H26b 2.21(7) . . ? H25b H26b 2.27(6) . . ? H25b H45b 2.38(7) . 1_655 ? H26a H26b 1.37(7) . . ? H31a H31b 1.43(4) . . ? H31a H33a 2.12(7) . . ? H31b H42 2.33(5) . . ? H32 H33a 2.28(5) . . ? H33a H33b 1.74(5) . . ? H33a H34a 2.25(7) . . ? H33a H34b 2.25(7) . . ? H33b H34b 2.33(6) . . ? H33b H36b 2.28(6) . . ? H34a H34b 1.50(6) . . ? H34a H35a 2.20(6) . . ? H34b H35b 2.09(6) . . ? H35a H35b 1.60(7) . . ? H35a H36a 2.21(5) . . ? H35b H36a 2.25(5) . . ? H35b H36b 2.35(5) . . ? H36a H36b 1.39(6) . . ? H36a H46b 2.21(6) . . ? H41a H41b 1.63(6) . . ? H41a H43a 2.25(5) . . ? H42 H43a 2.22(6) . . ? H43a H43b 1.59(7) . . ? H43a H44a 2.37(6) . . ? H43a H44b 2.27(6) . . ? H44a H44b 1.57(6) . . ? H44b H45a 2.19(8) . . ? H44b H45b 2.38(8) . . ? H45a H45b 1.58(5) . . ? H45a H46a 2.28(6) . . ? H45a H46b 2.22(6) . . ? H45b H46b 2.14(6) . . ? H46a H46b 1.31(7) . . ? loop_ _geom_angle_atom_site_label_1 #ActaC _geom_angle_atom_site_label_2 #ActaC _geom_angle_atom_site_label_3 #ActaC _geom_angle #ActaC _geom_angle_site_symmetry_1 #ActaC _geom_angle_site_symmetry_2 #ActaC _geom_angle_site_symmetry_3 #ActaC _geom_angle_publ_flag #ActaC Cl1 Cu1 N12 111.19(9) . . . ? Cl1 Cu1 N16 88.10(13) . . . ? Cl1 Cu1 N22 93.21(9) . . . ? Cl1 Cu1 N26 98.23(14) . . . ? N12 Cu1 N16 90.29(16) . . . ? N12 Cu1 N22 90.35(13) . . . ? N12 Cu1 N26 150.51(16) . . . ? N16 Cu1 N22 178.23(17) . . . ? N16 Cu1 N26 88.60(18) . . . ? N22 Cu1 N26 90.03(15) . . . ? Cl2 Cu2 N32 108.28(9) . . . ? Cl2 Cu2 N36 87.22(11) . . . ? Cl2 Cu2 N42 93.03(9) . . . ? Cl2 Cu2 N46 91.82(11) . . . ? N32 Cu2 N36 90.02(14) . . . ? N32 Cu2 N42 89.48(13) . . . ? N32 Cu2 N46 159.78(14) . . . ? N36 Cu2 N42 179.48(12) . . . ? N36 Cu2 N46 88.75(16) . . . ? N42 Cu2 N46 91.70(15) . . . ? C11 C0 C21 111.0(3) . . . ? C11 C0 C31 111.7(3) . . . ? C11 C0 C41 106.2(3) . . . ? C21 C0 C31 106.9(3) . . . ? C21 C0 C41 110.7(3) . . . ? C31 C0 C41 110.3(3) . . . ? C0 C11 N12 114.3(3) . . . ? C0 C11 H11a 113(2) . . . ? C0 C11 H11b 110.2(16) . . . ? N12 C11 H11a 108(2) . . . ? N12 C11 H11b 106(2) . . . ? H11a C11 H11b 104(3) . . . ? Cu1 N12 C11 110.5(2) . . . ? Cu1 N12 C13 109.8(3) . . . ? Cu1 N12 H12 111(3) . . . ? C11 N12 C13 108.1(3) . . . ? C11 N12 H12 112(2) . . . ? C13 N12 H12 105.1(18) . . . ? N12 C13 C14 113.5(3) . . . ? N12 C13 H13a 106.4(17) . . . ? N12 C13 H13b 106(2) . . . ? C14 C13 H13a 112.7(19) . . . ? C14 C13 H13b 117(2) . . . ? H13a C13 H13b 99(4) . . . ? C13 C14 C15 114.1(4) . . . ? C13 C14 H14a 109(3) . . . ? C13 C14 H14b 106(3) . . . ? C15 C14 H14a 102(3) . . . ? C15 C14 H14b 106(4) . . . ? H14a C14 H14b 121(4) . . . ? C14 C15 N16 113.4(4) . . . ? C14 C15 H15a 107(3) . . . ? C14 C15 H15b 112(3) . . . ? N16 C15 H15a 111(3) . . . ? N16 C15 H15b 105(3) . . . ? H15a C15 H15b 109(3) . . . ? Cu1 N16 C15 115.4(3) . . . ? Cu1 N16 H16a 95(3) . . . ? Cu1 N16 H16b 109(3) . . . ? C15 N16 H16a 109(3) . . . ? C15 N16 H16b 104(4) . . . ? H16a N16 H16b 125(5) . . . ? C0 C21 N22 113.3(3) . . . ? C0 C21 H21a 114(3) . . . ? C0 C21 H21b 110(3) . . . ? N22 C21 H21a 108(3) . . . ? N22 C21 H21b 109(3) . . . ? H21a C21 H21b 103(3) . . . ? Cu1 N22 C21 110.5(2) . . . ? Cu1 N22 C23 114.7(3) . . . ? Cu1 N22 H22 106(2) . . . ? C21 N22 C23 109.8(3) . . . ? C21 N22 H22 110(3) . . . ? C23 N22 H22 106(3) . . . ? N22 C23 C24 112.8(4) . . . ? N22 C23 H23a 108(3) . . . ? N22 C23 H23b 109(3) . . . ? C24 C23 H23a 104(3) . . . ? C24 C23 H23b 114(3) . . . ? H23a C23 H23b 109(3) . . . ? C23 C24 C25 114.6(5) . . . ? C23 C24 H24a 105(3) . . . ? C23 C24 H24b 105(4) . . . ? C25 C24 H24a 114(2) . . . ? C25 C24 H24b 113(4) . . . ? H24a C24 H24b 105(4) . . . ? C24 C25 N26 111.8(5) . . . ? C24 C25 H25a 109(3) . . . ? C24 C25 H25b 99(3) . . . ? N26 C25 H25a 103(3) . . . ? N26 C25 H25b 109(3) . . . ? H25a C25 H25b 125(5) . . . ? Cu1 N26 C25 118.9(4) . . . ? Cu1 N26 H26a 108(4) . . . ? Cu1 N26 H26b 99(4) . . . ? C25 N26 H26a 106(3) . . . ? C25 N26 H26b 117(4) . . . ? H26a N26 H26b 106(5) . . . ? C0 C31 N32 113.9(3) . . . ? C0 C31 H31a 110(3) . . . ? C0 C31 H31b 109(3) . . . ? N32 C31 H31a 108(3) . . . ? N32 C31 H31b 107(3) . . . ? H31a C31 H31b 109(3) . . . ? Cu2 N32 C31 110.9(2) . . . ? Cu2 N32 C33 110.1(2) . . . ? Cu2 N32 H32 109.0(17) . . . ? C31 N32 C33 108.9(3) . . . ? C31 N32 H32 113(2) . . . ? C33 N32 H32 105(2) . . . ? N32 C33 C34 112.8(4) . . . ? N32 C33 H33a 106(3) . . . ? N32 C33 H33b 102(2) . . . ? C34 C33 H33a 107(3) . . . ? C34 C33 H33b 113(3) . . . ? H33a C33 H33b 116(3) . . . ? C33 C34 C35 114.3(4) . . . ? C33 C34 H34a 110(3) . . . ? C33 C34 H34b 106(3) . . . ? C35 C34 H34a 108(2) . . . ? C35 C34 H34b 111(3) . . . ? H34a C34 H34b 107(4) . . . ? C34 C35 N36 112.3(4) . . . ? C34 C35 H35a 108(3) . . . ? C34 C35 H35b 104(2) . . . ? N36 C35 H35a 106(3) . . . ? N36 C35 H35b 112(2) . . . ? H35a C35 H35b 115(4) . . . ? Cu2 N36 C35 113.5(3) . . . ? Cu2 N36 H36a 100(4) . . . ? Cu2 N36 H36b 107(3) . . . ? C35 N36 H36a 110(3) . . . ? C35 N36 H36b 112(2) . . . ? H36a N36 H36b 113(4) . . . ? C0 C41 N42 113.5(3) . . . ? C0 C41 H41a 106(2) . . . ? C0 C41 H41b 106(2) . . . ? N42 C41 H41a 111.5(17) . . . ? N42 C41 H41b 109(2) . . . ? H41a C41 H41b 111(3) . . . ? Cu2 N42 C41 110.4(3) . . . ? Cu2 N42 C43 116.2(3) . . . ? Cu2 N42 H42 104(3) . . . ? C41 N42 C43 110.1(3) . . . ? C41 N42 H42 106(3) . . . ? C43 N42 H42 110(3) . . . ? N42 C43 C44 112.4(4) . . . ? N42 C43 H43a 106(2) . . . ? N42 C43 H43b 107(2) . . . ? C44 C43 H43a 108(2) . . . ? C44 C43 H43b 112(2) . . . ? H43a C43 H43b 111(4) . . . ? C43 C44 C45 113.9(4) . . . ? C43 C44 H44a 108(2) . . . ? C43 C44 H44b 111(3) . . . ? C45 C44 H44a 111(3) . . . ? C45 C44 H44b 108(4) . . . ? H44a C44 H44b 104(4) . . . ? C44 C45 N46 111.8(4) . . . ? C44 C45 H45a 108(3) . . . ? C44 C45 H45b 110(3) . . . ? N46 C45 H45a 111(3) . . . ? N46 C45 H45b 105(2) . . . ? H45a C45 H45b 112(4) . . . ? Cu2 N46 C45 119.5(3) . . . ? Cu2 N46 H46a 104(3) . . . ? Cu2 N46 H46b 104(3) . . . ? C45 N46 H46a 110(3) . . . ? C45 N46 H46b 111(3) . . . ? H46a N46 H46b 107(5) . . . ? loop_ _geom_torsion_atom_site_label_1 #ActaC _geom_torsion_atom_site_label_2 #ActaC _geom_torsion_atom_site_label_3 #ActaC _geom_torsion_atom_site_label_4 #ActaC _geom_torsion #ActaC _geom_torsion_site_symmetry_1 #ActaC _geom_torsion_site_symmetry_2 #ActaC _geom_torsion_site_symmetry_3 #ActaC _geom_torsion_site_symmetry_4 #ActaC _geom_torsion_publ_flag #ActaC ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 16 _reflns_limit_k_min -16 _reflns_limit_k_max 16 _reflns_limit_l_min -13 _reflns_limit_l_max 12 _reflns_number_total 6779 #ActaC _reflns_number_gt 5569 #ActaC _reflns_threshold_expression refl_observed_if_I____>2.000_sigma(I___) _reflns_d_resolution_high .757 _reflns_d_resolution_low 12.074 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? .851731 #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia Nedlands Western Australia 6907 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal ? _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Skelton, Brian W.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; #============================================================================== # (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_global _audit_creation_method Xtal3.6 _audit_creation_date 99-12-14 _audit_update_record ? #============================================================================== # (Publishing Staff Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia Nedlands Western Australia 6907 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal ? _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Skelton, Brian W.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; 'White, Allan H.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_cuykno # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C17 H50 Cu2 N12 O15' _chemical_formula_moiety ? _chemical_formula_weight 789.75 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P_b_c_a _symmetry_space_group_name_Hall -p_2ac_2ab loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z -x,-y,-z 1/2+x,+y,1/2-z 1/2-x,1/2+y,+z +x,1/2-y,1/2+z _cell_length_a 22.843(9) _cell_length_b 18.422(6) _cell_length_c 15.489(5) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 6518(4) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8 _cell_measurement_theta_min 17.65 _cell_measurement_theta_max 17.65 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 1.39 _exptl_crystal_description block _exptl_crystal_size_max .95 _exptl_crystal_size_mid .35 _exptl_crystal_size_min .23 _exptl_crystal_size_rad ? _exptl_crystal_colour blue _diffrn_measurement_device_type ; CAD4 diffractometer ; _diffrn_measurement_method '2\q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; XTAL absorb ; _exptl_absorpt_correction_T_min .53 _exptl_absorpt_correction_T_max .69 _diffrn_reflns_number 9636 _reflns_number_total 5735 _reflns_Friedel_coverage ? _reflns_number_gt 3810 _reflns_threshold_expression 'I > 2.00 sig(I )' _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .082 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_standards_number 8 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F #<< use NfA code _refine_ls_R_factor_gt .0494 _refine_ls_wR_factor_ref .0611 _refine_ls_goodness_of_fit_ref 1.486 _refine_ls_number_reflns 3810 _refine_ls_number_parameters 601 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment mixed #<< use NfA code _refine_ls_shift/su_max .084 _refine_diff_density_min -.53 _refine_diff_density_max .79 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Enraf Nonius software' _computing_cell_refinement 'Enraf Nonius software' _computing_data_reduction xtal _computing_structure_solution xtal _computing_structure_refinement xtal _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ 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 ? 0 136 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 400 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cu ? 0 16 .263001 1.266 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 96 .004028 .002991 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 120 .007996 .005981 '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_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 .56828(2) .33244(3) .72808(4) .0356(3) Uani ? ? 1.00000 ? ? Cu2 .68118(3) .59068(4) 1.00875(4) .0518(4) Uani ? ? 1.00000 ? ? C0 .6158(2) .4572(3) .8812(3) .041(3) Uani ? ? 1.00000 ? ? C11 .5603(2) .4714(3) .8284(4) .042(3) Uani ? ? 1.00000 ? ? N12 .5602(2) .4438(2) .7398(3) .038(2) Uani ? ? 1.00000 ? ? C13 .5025(3) .4642(3) .6997(4) .053(3) Uani ? ? 1.00000 ? ? C14 .5014(4) .4546(4) .6027(4) .057(4) Uani ? ? 1.00000 ? ? C15 .5021(3) .3780(4) .5726(4) .056(4) Uani ? ? 1.00000 ? ? N16 .5562(2) .3405(3) .6018(3) .046(3) Uani ? ? 1.00000 ? ? C21 .6380(3) .3787(3) .8730(5) .048(3) Uani ? ? 1.00000 ? ? N22 .5924(2) .3247(2) .8532(3) .038(2) Uani ? ? 1.00000 ? ? C23 .6126(3) .2513(3) .8793(5) .050(4) Uani ? ? 1.00000 ? ? C24 .5665(3) .1934(3) .8670(4) .060(4) Uani ? ? 1.00000 ? ? C25 .5541(4) .1761(3) .7735(5) .064(4) Uani ? ? 1.00000 ? ? N26 .5261(3) .2364(3) .7291(4) .069(4) Uani ? ? 1.00000 ? ? C31 .6675(2) .5043(3) .8505(4) .047(3) Uani ? ? 1.00000 ? ? N32 .6653(2) .5804(2) .8803(3) .042(2) Uani ? ? 1.00000 ? ? C33 .7067(3) .6247(4) .8259(5) .063(4) Uani ? ? 1.00000 ? ? C34 .7008(4) .7051(4) .8416(5) .074(5) Uani ? ? 1.00000 ? ? C35 .7200(4) .7294(5) .9292(6) .077(5) Uani ? ? 1.00000 ? ? N36 .6832(3) .6995(3) .9957(4) .066(4) Uani ? ? 1.00000 ? ? C41 .5970(2) .4728(3) .9748(3) .042(3) Uani ? ? 1.00000 ? ? N42 .6453(2) .4913(2) 1.0353(3) .043(2) Uani ? ? 1.00000 ? ? C43 .6219(3) .4878(4) 1.1243(4) .054(4) Uani ? ? 1.00000 ? ? C44 .6653(4) .4924(5) 1.1948(5) .073(5) Uani ? ? 1.00000 ? ? C45 .7021(7) .5562(8) 1.1938(9) .203(13) Uani ? ? 1.00000 ? ? N46 .7094(5) .6008(5) 1.1295(4) .116(6) Uani ? ? 1.00000 ? ? N1 .6826(2) .2555(3) .6492(3) .055(3) Uani ? ? 1.00000 ? ? O11 .6677(2) .3065(3) .6970(3) .067(2) Uani ? ? 1.00000 ? ? O12 .6456(2) .2180(2) .6122(4) .079(3) Uani ? ? 1.00000 ? ? O13 .7363(2) .2436(2) .6379(3) .067(3) Uani ? ? 1.00000 ? ? N2 .8244(3) .5617(4) .9776(5) .080(4) Uani ? ? 1.00000 ? ? O21 .7768(2) .5346(3) .9659(4) .097(4) Uani ? ? 1.00000 ? ? O22 .8286(3) .6153(5) 1.0234(6) .147(6) Uani ? ? 1.00000 ? ? O23 .8694(3) .5395(3) .9461(6) .133(6) Uani ? ? 1.00000 ? ? N3 .5253(2) .6672(2) .9779(3) .049(3) Uani ? ? 1.00000 ? ? O31 .5446(3) .6363(3) 1.0405(3) .091(3) Uani ? ? 1.00000 ? ? O32 .5554(2) .6754(4) .9158(4) .134(5) Uani ? ? 1.00000 ? ? O33 .4753(2) .6885(3) .9751(4) .081(3) Uani ? ? 1.00000 ? ? N4 .6089(6) .6262(9) .6500(10) .177(13) Uani ? ? 1.00000 ? ? O41 .5850(4) .6248(7) .7110(8) .171(8) Uani ? ? 1.00000 ? ? O42 .6192(5) .6707(6) .5960(7) .221(10) Uani ? ? 1.00000 ? ? O43 .6337(5) .5592(7) .6311(6) .185(8) Uani ? ? 1.00000 ? ? O01 .7408(2) .3891(3) 1.0403(4) .096(4) Uani ? ? 1.00000 ? ? O02 .8524(4) .3863(5) .9190(10) .249(12) Uani ? ? 1.00000 ? ? O03 .5840(10) .7830(10) .6800(10) .150(13) Uani ? ? .50000 ? ? O03' .5960(10) .8160(10) .727(2) .18(2) Uani ? ? .50000 ? ? H11a .556(2) .526(3) .825(3) .040(10) Uiso ? ? 1.00000 ? ? H11b .524(2) .443(3) .855(3) .040(10) Uiso ? ? 1.00000 ? ? H12 .585(2) .465(3) .714(4) .05(2) Uiso ? ? 1.00000 ? ? H13a .496(2) .516(3) .710(3) .040(10) Uiso ? ? 1.00000 ? ? H13b .471(2) .423(3) .726(4) .05(2) Uiso ? ? 1.00000 ? ? H14a .530(2) .479(3) .584(3) .04(2) Uiso ? ? 1.00000 ? ? H14b .466(3) .475(3) .591(5) .08(2) Uiso ? ? 1.00000 ? ? H15a .497(3) .379(4) .505(5) .08(2) Uiso ? ? 1.00000 ? ? H15b .468(3) .346(4) .591(6) .11(3) Uiso ? ? 1.00000 ? ? H16a .584(2) .362(3) .594(3) .020(10) Uiso ? ? 1.00000 ? ? H16b .551(2) .297(3) .590(4) .04(2) Uiso ? ? 1.00000 ? ? H21a .659(2) .364(3) .926(4) .050(10) Uiso ? ? 1.00000 ? ? H21b .665(2) .376(3) .832(4) .05(2) Uiso ? ? 1.00000 ? ? H22 .565(2) .329(3) .872(4) .03(2) Uiso ? ? 1.00000 ? ? H23a .623(3) .253(4) .931(5) .09(3) Uiso ? ? 1.00000 ? ? H23b .644(2) .246(2) .843(3) .030(10) Uiso ? ? 1.00000 ? ? H24a .531(2) .215(3) .892(4) .06(2) Uiso ? ? 1.00000 ? ? H24b .583(2) .154(3) .901(4) .06(2) Uiso ? ? 1.00000 ? ? H25a .533(3) .137(4) .766(5) .09(2) Uiso ? ? 1.00000 ? ? H25b .585(3) .164(3) .753(4) .05(2) Uiso ? ? 1.00000 ? ? H26a .490(4) .248(5) .758(6) .14(4) Uiso ? ? 1.00000 ? ? H26b .529(3) .212(4) .667(6) .11(3) Uiso ? ? 1.00000 ? ? H31a .665(2) .504(3) .782(4) .05(2) Uiso ? ? 1.00000 ? ? H31b .700(2) .481(3) .878(3) .040(10) Uiso ? ? 1.00000 ? ? H32 .629(2) .605(3) .871(3) .040(10) Uiso ? ? 1.00000 ? ? H33a .699(3) .616(4) .768(6) .09(2) Uiso ? ? 1.00000 ? ? H33b .742(2) .611(3) .841(4) .04(2) Uiso ? ? 1.00000 ? ? H34a .660(3) .725(3) .837(4) .07(2) Uiso ? ? 1.00000 ? ? H34b .719(3) .735(4) .800(5) .08(2) Uiso ? ? 1.00000 ? ? H35a .719(4) .777(6) .932(8) .15(4) Uiso ? ? 1.00000 ? ? H35b .756(3) .714(4) .933(5) .09(3) Uiso ? ? 1.00000 ? ? H36a .639(4) .724(5) .977(6) .14(4) Uiso ? ? 1.00000 ? ? H36b .682(3) .714(4) 1.045(6) .08(3) Uiso ? ? 1.00000 ? ? H41a .578(2) .422(3) 1.004(3) .050(10) Uiso ? ? 1.00000 ? ? H41b .566(2) .521(3) .978(4) .06(2) Uiso ? ? 1.00000 ? ? H42 .674(3) .453(4) 1.044(5) .08(2) Uiso ? ? 1.00000 ? ? H43a .608(3) .438(4) 1.133(5) .09(2) Uiso ? ? 1.00000 ? ? H43b .600(2) .523(3) 1.127(4) .04(2) Uiso ? ? 1.00000 ? ? H44a .686(3) .466(4) 1.182(6) .07(3) Uiso ? ? 1.00000 ? ? H44b .646(4) .491(4) 1.258(7) .12(3) Uiso ? ? 1.00000 ? ? H45a .735(2) .538(2) 1.194(4) .08(3) Uiso ? ? 1.00000 ? ? H45b .709(3) .576(3) 1.246(3) .09(3) Uiso ? ? 1.00000 ? ? H46a .741(2) .567(2) 1.119(3) .020(10) Uiso ? ? 1.00000 ? ? H46b .731(3) .645(3) 1.137(4) .15(4) Uiso ? ? 1.00000 ? ? H01a .72310 .33780 1.04070 .15000 Uiso ? ? 1.00000 ? ? H01b .76620 .40440 1.03580 .15000 Uiso ? ? 1.00000 ? ? 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 .0447(4) .0311(3) .0309(3) -.0003(3) -.0024(3) -.0010(2) Cu2 .0652(5) .0549(4) .0354(4) -.0228(3) -.0003(3) -.0057(3) C0 .040(3) .039(3) .043(3) .001(2) .000(2) -.009(2) C11 .045(3) .034(3) .047(3) .007(2) -.002(3) -.016(2) N12 .043(3) .032(2) .040(2) .002(2) .000(2) -.001(2) C13 .059(3) .044(3) .055(3) .018(3) -.017(3) -.008(3) C14 .065(4) .055(4) .052(4) .013(3) -.014(4) .001(3) C15 .059(4) .074(4) .035(3) .015(3) -.007(3) -.006(3) N16 .056(3) .045(3) .038(2) -.003(3) .007(2) -.005(2) C21 .043(3) .049(3) .052(4) .003(3) -.007(3) -.014(3) N22 .042(3) .039(2) .034(2) .003(2) .002(2) .001(2) C23 .057(4) .045(3) .048(4) .010(3) .001(3) .011(3) C24 .082(5) .043(3) .055(4) .006(3) .001(4) .014(3) C25 .089(5) .044(4) .058(4) -.019(4) .003(4) -.005(3) N26 .095(5) .053(3) .060(4) -.029(3) -.018(3) .010(3) C31 .041(3) .053(3) .046(3) -.002(2) .006(3) -.011(3) N32 .044(3) .045(2) .037(2) -.004(2) .011(2) -.007(2) C33 .061(4) .075(4) .053(4) -.014(4) .011(4) .008(4) C34 .094(6) .062(4) .065(5) -.026(4) .008(4) .003(4) C35 .088(6) .062(5) .081(5) -.029(4) .010(5) -.004(4) N36 .078(4) .060(3) .059(4) -.020(3) .004(3) -.020(3) C41 .040(3) .045(3) .042(3) -.006(2) -.002(2) -.011(3) N42 .045(2) .045(2) .038(2) .001(2) -.001(2) -.003(2) C43 .065(4) .053(4) .045(3) -.009(3) .004(3) .004(3) C44 .086(6) .080(6) .052(4) -.004(5) -.012(4) .011(4) C45 .230(10) .25(2) .130(10) -.160(10) -.130(10) .120(10) N46 .179(8) .121(7) .047(4) -.083(7) -.039(5) .010(4) N1 .051(3) .066(3) .048(3) .004(2) .007(2) .014(3) O11 .059(2) .089(3) .053(2) .002(2) .004(2) -.017(3) O12 .059(3) .068(3) .109(4) -.009(2) -.005(3) -.016(3) O13 .047(2) .081(3) .072(3) .003(2) .010(2) .005(3) N2 .073(4) .066(4) .100(5) -.019(3) -.022(4) .014(4) O21 .066(3) .098(4) .127(5) -.026(3) -.029(3) .004(4) O22 .118(5) .143(6) .179(8) -.042(4) -.008(5) -.063(6) O23 .070(4) .103(5) .226(9) .001(3) .026(5) .046(5) N3 .055(3) .050(3) .041(3) .012(2) .000(2) .007(2) O31 .135(4) .069(3) .070(3) .006(3) -.027(3) .018(3) O32 .088(4) .223(8) .090(4) .066(4) .036(4) .054(5) O33 .067(3) .080(3) .096(4) .022(2) .027(3) .028(3) N4 .130(10) .23(2) .170(10) -.070(10) -.030(10) .060(10) O41 .101(5) .230(10) .181(9) -.011(6) .021(6) .102(9) O42 .250(10) .240(10) .172(9) -.107(9) -.020(8) .130(9) O43 .200(10) .270(10) .085(5) -.120(10) .000(6) .013(8) O01 .078(3) .062(3) .148(5) .012(2) .003(3) .022(3) O02 .161(8) .145(7) .44(2) -.021(6) -.030(10) .010(10) O03 .160(10) .18(2) .110(10) -.060(10) -.040(10) .020(10) O03' .15(2) .19(2) .21(3) .05(2) .05(2) .13(2) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Cu1 N12 . . 2.068(4) ? Cu1 N16 . . 1.981(5) ? Cu1 N22 . . 2.020(5) ? Cu1 N26 . . 2.015(6) ? Cu1 O11 . . 2.370(5) ? Cu2 N32 . . 2.031(5) ? Cu2 N36 . . 2.015(6) ? Cu2 N42 . . 2.048(4) ? Cu2 N46 . . 1.987(7) ? Cu2 O21 . . 2.506(5) ? C0 C11 . . 1.531(7) ? C0 C21 . . 1.538(8) ? C0 C31 . . 1.541(7) ? C0 C41 . . 1.539(7) ? C11 N12 . . 1.463(8) ? C11 H11a . . 1.01(6) ? C11 H11b . . 1.06(5) ? N12 C13 . . 1.505(8) ? N12 H12 . . .80(5) ? C13 C14 . . 1.513(9) ? C13 H13a . . .98(6) ? C13 H13b . . 1.12(5) ? C14 C15 . . 1.486(10) ? C14 H14a . . .84(5) ? C14 H14b . . .91(7) ? C15 N16 . . 1.486(8) ? C15 H15a . . 1.05(8) ? C15 H15b . . 1.02(7) ? N16 H16a . . .76(5) ? N16 H16b . . .83(6) ? C21 N22 . . 1.473(8) ? C21 H21a . . .99(6) ? C21 H21b . . .89(6) ? N22 C23 . . 1.485(7) ? N22 H22 . . .69(5) ? C23 C24 . . 1.511(9) ? C23 H23a . . .84(8) ? C23 H23b . . .92(5) ? C24 C25 . . 1.510(10) ? C24 H24a . . .98(5) ? C24 H24b . . .97(6) ? C25 N26 . . 1.455(9) ? C25 H25a . . .87(7) ? C25 H25b . . .81(7) ? N26 H26a . . .96(9) ? N26 H26b . . 1.06(9) ? C31 N32 . . 1.477(7) ? C31 H31a . . 1.06(6) ? C31 H31b . . .96(5) ? N32 C33 . . 1.507(8) ? N32 H32 . . .96(5) ? C33 C34 . . 1.507(10) ? C33 H33a . . .93(9) ? C33 H33b . . .88(5) ? C34 C35 . . 1.495(12) ? C34 H34a . . 1.00(7) ? C34 H34b . . .94(7) ? C35 N36 . . 1.439(11) ? C35 H35a . . .88(11) ? C35 H35b . . .87(7) ? N36 H36a . . 1.14(9) ? N36 H36b . . .81(9) ? C41 N42 . . 1.487(7) ? C41 H41a . . 1.13(5) ? C41 H41b . . 1.14(5) ? N42 C43 . . 1.480(8) ? N42 H42 . . .97(7) ? C43 C44 . . 1.477(11) ? C43 H43a . . .98(7) ? C43 H43b . . .82(5) ? C44 C45 . . 1.445(18) ? C44 H44a . . .71(7) ? C44 H44b . . 1.07(11) ? C45 N46 . . 1.302(16) ? C45 H45a . . .82(5) ? C45 H45b . . .90(5) ? N46 H46a . . .97(4) ? N46 H46b . . .96(6) ? N1 O11 . . 1.244(7) ? N1 O12 . . 1.233(7) ? N1 O13 . . 1.258(6) ? N2 O21 . . 1.210(8) ? N2 O22 . . 1.220(12) ? N2 O23 . . 1.209(10) ? N3 O31 . . 1.208(7) ? N3 O32 . . 1.192(7) ? N3 O33 . . 1.208(6) ? N4 O41 . . 1.09(2) ? N4 O42 . . 1.19(2) ? N4 O43 . . 1.39(2) ? O01 H01a . . 1.028(5) ? O01 H01b . . .649(5) ? O03 O03' . . .99(3) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published N12 Cu1 N16 . . . 90.0(2) ? N12 Cu1 N22 . . . 90.58(17) ? N12 Cu1 N26 . . . 145.9(2) ? N12 Cu1 O11 . . . 107.66(19) ? N16 Cu1 N22 . . . 172.18(19) ? N16 Cu1 N26 . . . 90.4(2) ? N16 Cu1 O11 . . . 87.02(18) ? N22 Cu1 N26 . . . 93.5(2) ? N22 Cu1 O11 . . . 85.37(17) ? N26 Cu1 O11 . . . 106.4(2) ? N32 Cu2 N36 . . . 89.9(2) ? N32 Cu2 N42 . . . 92.40(17) ? N32 Cu2 N46 . . . 171.4(3) ? N32 Cu2 O21 . . . 81.82(19) ? N36 Cu2 N42 . . . 156.7(2) ? N36 Cu2 N46 . . . 89.6(3) ? N36 Cu2 O21 . . . 111.3(2) ? N42 Cu2 N46 . . . 91.4(3) ? N42 Cu2 O21 . . . 91.92(18) ? N46 Cu2 O21 . . . 90.3(3) ? C11 C0 C21 . . . 112.9(5) ? C11 C0 C31 . . . 111.9(4) ? C11 C0 C41 . . . 103.9(4) ? C21 C0 C31 . . . 104.6(4) ? C21 C0 C41 . . . 110.2(5) ? C31 C0 C41 . . . 113.5(4) ? C0 C11 N12 . . . 116.3(4) ? C0 C11 H11a . . . 106(3) ? C0 C11 H11b . . . 111(3) ? N12 C11 H11a . . . 107(3) ? N12 C11 H11b . . . 101(3) ? H11a C11 H11b . . . 116(4) ? Cu1 N12 C11 . . . 115.3(3) ? Cu1 N12 C13 . . . 106.8(3) ? Cu1 N12 H12 . . . 112(4) ? C11 N12 C13 . . . 107.6(4) ? C11 N12 H12 . . . 107(4) ? C13 N12 H12 . . . 107(4) ? N12 C13 C14 . . . 113.3(6) ? N12 C13 H13a . . . 108(3) ? N12 C13 H13b . . . 104(3) ? C14 C13 H13a . . . 106(3) ? C14 C13 H13b . . . 106(3) ? H13a C13 H13b . . . 120(4) ? C13 C14 C15 . . . 115.0(5) ? C13 C14 H14a . . . 105(3) ? C13 C14 H14b . . . 99(5) ? C15 C14 H14a . . . 113(4) ? C15 C14 H14b . . . 110(4) ? H14a C14 H14b . . . 114(5) ? C14 C15 N16 . . . 110.8(6) ? C14 C15 H15a . . . 107(4) ? C14 C15 H15b . . . 117(4) ? N16 C15 H15a . . . 114(4) ? N16 C15 H15b . . . 106(4) ? H15a C15 H15b . . . 102(6) ? Cu1 N16 C15 . . . 116.8(4) ? Cu1 N16 H16a . . . 95(4) ? Cu1 N16 H16b . . . 99(4) ? C15 N16 H16a . . . 114(4) ? C15 N16 H16b . . . 105(3) ? H16a N16 H16b . . . 126(5) ? C0 C21 N22 . . . 114.8(5) ? C0 C21 H21a . . . 110(3) ? C0 C21 H21b . . . 110(4) ? N22 C21 H21a . . . 109(3) ? N22 C21 H21b . . . 108(4) ? H21a C21 H21b . . . 104(5) ? Cu1 N22 C21 . . . 110.2(4) ? Cu1 N22 C23 . . . 114.2(4) ? Cu1 N22 H22 . . . 99(5) ? C21 N22 C23 . . . 109.8(5) ? C21 N22 H22 . . . 118(5) ? C23 N22 H22 . . . 106(5) ? N22 C23 C24 . . . 113.1(5) ? N22 C23 H23a . . . 108(5) ? N22 C23 H23b . . . 100(2) ? C24 C23 H23a . . . 110(5) ? C24 C23 H23b . . . 113(3) ? H23a C23 H23b . . . 112(6) ? C23 C24 C25 . . . 113.6(6) ? C23 C24 H24a . . . 104(3) ? C23 C24 H24b . . . 101(3) ? C25 C24 H24a . . . 108(3) ? C25 C24 H24b . . . 116(4) ? H24a C24 H24b . . . 114(5) ? C24 C25 N26 . . . 112.0(5) ? C24 C25 H25a . . . 114(5) ? C24 C25 H25b . . . 106(5) ? N26 C25 H25a . . . 109(5) ? N26 C25 H25b . . . 114(4) ? H25a C25 H25b . . . 102(6) ? Cu1 N26 C25 . . . 117.6(5) ? Cu1 N26 H26a . . . 103(5) ? Cu1 N26 H26b . . . 110(4) ? C25 N26 H26a . . . 109(6) ? C25 N26 H26b . . . 94(4) ? H26a N26 H26b . . . 125(7) ? C0 C31 N32 . . . 114.3(4) ? C0 C31 H31a . . . 105(3) ? C0 C31 H31b . . . 102(3) ? N32 C31 H31a . . . 108(3) ? N32 C31 H31b . . . 108(3) ? H31a C31 H31b . . . 119(4) ? Cu2 N32 C31 . . . 112.9(3) ? Cu2 N32 C33 . . . 112.7(4) ? Cu2 N32 H32 . . . 105(3) ? C31 N32 C33 . . . 108.5(5) ? C31 N32 H32 . . . 116(3) ? C33 N32 H32 . . . 102(3) ? N32 C33 C34 . . . 112.7(6) ? N32 C33 H33a . . . 109(5) ? N32 C33 H33b . . . 106(4) ? C34 C33 H33a . . . 108(5) ? C34 C33 H33b . . . 109(4) ? H33a C33 H33b . . . 112(6) ? C33 C34 C35 . . . 114.5(7) ? C33 C34 H34a . . . 115(3) ? C33 C34 H34b . . . 115(5) ? C35 C34 H34a . . . 103(4) ? C35 C34 H34b . . . 108(5) ? H34a C34 H34b . . . 98(5) ? C34 C35 N36 . . . 111.3(7) ? C34 C35 H35a . . . 110(8) ? C34 C35 H35b . . . 104(5) ? N36 C35 H35a . . . 109(7) ? N36 C35 H35b . . . 112(5) ? H35a C35 H35b . . . 110(8) ? Cu2 N36 C35 . . . 117.8(5) ? Cu2 N36 H36a . . . 113(5) ? Cu2 N36 H36b . . . 103(5) ? C35 N36 H36a . . . 101(5) ? C35 N36 H36b . . . 125(5) ? H36a N36 H36b . . . 95(7) ? C0 C41 N42 . . . 115.4(4) ? C0 C41 H41a . . . 109(3) ? C0 C41 H41b . . . 111(3) ? N42 C41 H41a . . . 103(2) ? N42 C41 H41b . . . 105(3) ? H41a C41 H41b . . . 113(4) ? Cu2 N42 C41 . . . 112.0(3) ? Cu2 N42 C43 . . . 111.8(4) ? Cu2 N42 H42 . . . 114(4) ? C41 N42 C43 . . . 108.0(4) ? C41 N42 H42 . . . 115(4) ? C43 N42 H42 . . . 95(5) ? N42 C43 C44 . . . 116.3(6) ? N42 C43 H43a . . . 107(5) ? N42 C43 H43b . . . 103(4) ? C44 C43 H43a . . . 100(4) ? C44 C43 H43b . . . 109(4) ? H43a C43 H43b . . . 122(5) ? C43 C44 C45 . . . 115.4(9) ? C43 C44 H44a . . . 102(7) ? C43 C44 H44b . . . 113(5) ? C45 C44 H44a . . . 100(6) ? C45 C44 H44b . . . 106(4) ? H44a C44 H44b . . . 121(8) ? C44 C45 N46 . . . 126.6(12) ? C44 C45 H45a . . . 102(3) ? C44 C45 H45b . . . 115(4) ? N46 C45 H45a . . . 98(4) ? N46 C45 H45b . . . 114(4) ? H45a C45 H45b . . . 90(6) ? Cu2 N46 C45 . . . 128.3(9) ? Cu2 N46 H46a . . . 91(3) ? Cu2 N46 H46b . . . 111(4) ? C45 N46 H46a . . . 80(3) ? C45 N46 H46b . . . 121(4) ? H46a N46 H46b . . . 101(5) ? O11 N1 O12 . . . 120.8(5) ? O11 N1 O13 . . . 118.8(5) ? O12 N1 O13 . . . 120.4(5) ? Cu1 O11 N1 . . . 122.4(4) ? O21 N2 O22 . . . 119.5(7) ? O21 N2 O23 . . . 124.3(8) ? O22 N2 O23 . . . 116.2(7) ? Cu2 O21 N2 . . . 125.0(5) ? O31 N3 O32 . . . 119.8(6) ? O31 N3 O33 . . . 121.8(6) ? O32 N3 O33 . . . 118.4(5) ? O41 N4 O42 . . . 136.1(17) ? O41 N4 O43 . . . 111.4(15) ? O42 N4 O43 . . . 112.4(13) ? H01a O01 H01b . . . 138.7(7) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- 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 C0 3.476(5) . . ? Cu1 C11 3.000(6) . . ? Cu1 C13 2.888(6) . . ? Cu1 C14 3.342(7) . . ? Cu1 C15 2.965(7) . . ? Cu1 C21 2.881(7) . . ? Cu1 C23 2.957(7) . . ? Cu1 C24 3.345(6) . . ? Cu1 C25 2.982(6) . . ? Cu1 N1 3.213(5) . . ? Cu1 O12 3.284(5) . . ? Cu1 O03 3.87(2) . '4 646' ? Cu1 O03' 3.83(2) . '4 646' ? Cu1 H11b 3.01(5) . . ? Cu1 H12 2.48(6) . . ? Cu1 H13b 2.78(5) . . ? Cu1 H15b 3.13(8) . . ? Cu1 H16a 2.18(5) . . ? Cu1 H16b 2.27(6) . . ? Cu1 H21b 2.85(5) . . ? Cu1 H22 2.23(6) . . ? Cu1 H23b 2.95(4) . . ? Cu1 H24a 3.44(6) . . ? Cu1 H25b 3.15(6) . . ? Cu1 H26a 2.41(9) . . ? Cu1 H26b 2.57(8) . . ? Cu2 C0 3.490(5) . . ? Cu2 C31 2.939(6) . . ? Cu2 C33 2.959(8) . . ? Cu2 C34 3.368(8) . . ? Cu2 C35 2.972(9) . . ? Cu2 C41 2.948(5) . . ? Cu2 C43 2.937(7) . . ? Cu2 C44 3.423(8) . . ? Cu2 C45 2.974(14) . . ? Cu2 N2 3.350(7) . . ? Cu2 O22 3.405(7) . . ? Cu2 N3 3.859(5) . . ? Cu2 O31 3.268(7) . . ? Cu2 O32 3.573(6) . . ? Cu2 O01 3.985(6) . . ? Cu2 H31b 2.89(5) . . ? Cu2 H32 2.46(5) . . ? Cu2 H33b 2.97(6) . . ? Cu2 H35b 3.08(7) . . ? Cu2 H36a 2.68(9) . . ? Cu2 H36b 2.34(7) . . ? Cu2 H41b 2.97(5) . . ? Cu2 H42 2.60(7) . . ? Cu2 H43b 2.89(5) . . ? Cu2 H44a 3.53(9) . . ? Cu2 H45a 3.27(6) . . ? Cu2 H46a 2.23(5) . . ? Cu2 H46b 2.50(6) . . ? C0 N12 2.544(7) . . ? C0 N22 2.536(7) . . ? C0 N32 2.536(7) . . ? C0 N42 2.558(7) . . ? C0 H11a 2.06(5) . . ? C0 H11b 2.15(5) . . ? C0 H12 2.69(6) . . ? C0 H21a 2.10(5) . . ? C0 H21b 2.02(5) . . ? C0 H22 2.64(5) . . ? C0 H31a 2.09(6) . . ? C0 H31b 1.97(5) . . ? C0 H41a 2.19(5) . . ? C0 H41b 2.22(6) . . ? C11 C13 2.395(9) . . ? C11 C21 2.558(8) . . ? C11 N22 2.826(7) . . ? C11 C31 2.546(7) . . ? C11 C41 2.418(8) . . ? C11 H12 1.86(6) . . ? C11 H13a 2.49(5) . . ? C11 H31a 2.57(5) . . ? C11 H41b 2.49(6) . . ? N12 C14 2.521(9) . . ? N12 N16 2.863(7) . . ? N12 C21 2.975(8) . . ? N12 N22 2.905(6) . . ? N12 H11a 2.01(5) . . ? N12 H11b 1.97(5) . . ? N12 H13a 2.03(5) . . ? N12 H13b 2.08(5) . . ? N12 H14a 2.59(5) . . ? C13 C15 2.529(9) . . ? C13 N16 3.000(8) . . ? C13 H11a 2.56(5) . . ? C13 H11b 2.49(5) . . ? C13 H12 1.90(5) . . ? C13 H14a 1.92(5) . . ? C13 H14b 1.89(8) . . ? C14 N16 2.447(10) . . ? C14 H12 2.58(5) . . ? C14 H13a 2.01(5) . . ? C14 H13b 2.11(6) . . ? C14 H15a 2.06(8) . . ? C14 H15b 2.15(7) . . ? C14 H16a 2.55(5) . . ? C15 H13b 2.61(6) . . ? C15 H14a 1.97(5) . . ? C15 H14b 1.99(6) . . ? C15 H16a 1.92(5) . . ? C15 H16b 1.88(5) . . ? N16 N26 2.835(8) . . ? N16 O11 3.009(7) . . ? N16 O12 3.048(7) . . ? N16 O22 3.010(9) . '2 664' ? N16 H14a 2.64(6) . . ? N16 H15a 2.14(7) . . ? N16 H15b 2.02(7) . . ? N16 H26b 2.65(8) . . ? C21 C23 2.420(8) . . ? C21 C31 2.435(8) . . ? C21 C41 2.524(8) . . ? C21 H22 1.90(5) . . ? C21 H23a 2.51(7) . . ? C21 H23b 2.49(4) . . ? C21 H31b 2.36(5) . . ? C21 H41a 2.58(5) . . ? N22 C24 2.499(7) . . ? N22 N26 2.938(8) . . ? N22 O11 2.987(7) . . ? N22 O33 3.086(7) . '5 667' ? N22 H11b 2.68(5) . . ? N22 H21a 2.03(5) . . ? N22 H21b 1.94(5) . . ? N22 H23a 1.92(7) . . ? N22 H23b 1.88(4) . . ? N22 H24a 2.53(5) . . ? C23 C25 2.528(10) . . ? C23 H21a 2.44(5) . . ? C23 H21b 2.69(5) . . ? C23 H22 1.80(5) . . ? C23 H24a 1.99(5) . . ? C23 H24b 1.95(5) . . ? C23 H25b 2.61(6) . . ? C24 N26 2.458(9) . . ? C24 H22 2.50(6) . . ? C24 H23a 1.96(7) . . ? C24 H23b 2.05(4) . . ? C24 H25a 2.03(8) . . ? C24 H25b 1.89(6) . . ? C24 H26a 2.63(9) . . ? C25 H23b 2.65(4) . . ? C25 H24a 2.04(6) . . ? C25 H24b 2.12(6) . . ? C25 H26a 1.99(9) . . ? C25 H26b 1.87(9) . . ? N26 O03 3.01(2) . '4 646' ? N26 H16b 2.49(6) . . ? N26 H24a 2.56(6) . . ? N26 H25a 1.92(7) . . ? N26 H25b 1.93(6) . . ? C31 C33 2.422(9) . . ? C31 C41 2.576(7) . . ? C31 N42 2.917(8) . . ? C31 H11a 2.61(5) . . ? C31 H21b 2.38(6) . . ? C31 H32 2.08(5) . . ? C31 H33a 2.53(8) . . ? C31 H33b 2.60(5) . . ? N32 C34 2.509(9) . . ? N32 N36 2.859(7) . . ? N32 C41 2.916(7) . . ? N32 N42 2.944(6) . . ? N32 O21 2.993(7) . . ? N32 H31a 2.07(6) . . ? N32 H31b 2.00(5) . . ? N32 H33a 2.01(9) . . ? N32 H33b 1.94(5) . . ? C33 C35 2.524(12) . . ? C33 H31a 2.51(6) . . ? C33 H32 1.94(5) . . ? C33 H34a 2.14(6) . . ? C33 H34b 2.09(7) . . ? C33 H35b 2.59(7) . . ? C34 N36 2.423(10) . . ? C34 H32 2.51(5) . . ? C34 H33a 2.00(8) . . ? C34 H33b 1.97(5) . . ? C34 H35a 1.97(12) . . ? C34 H35b 1.90(7) . . ? C34 H36a 2.55(9) . . ? C35 H33b 2.62(6) . . ? C35 H34a 1.98(7) . . ? C35 H34b 2.00(8) . . ? C35 H36a 2.00(9) . . ? C35 H36b 2.01(9) . . ? N36 N46 2.821(10) . . ? N36 O13 3.055(8) . '2 665' ? N36 H34a 2.56(6) . . ? N36 H35a 1.92(11) . . ? N36 H35b 1.94(7) . . ? N36 H46b 2.64(6) . . ? C41 C43 2.400(8) . . ? C41 H11a 2.69(5) . . ? C41 H11b 2.55(5) . . ? C41 H21a 2.57(5) . . ? C41 H42 2.09(7) . . ? C41 H43a 2.55(8) . . ? C41 H43b 2.53(6) . . ? N42 C44 2.512(9) . . ? N42 N46 2.888(10) . . ? N42 O01 2.883(7) . . ? N42 H41a 2.06(5) . . ? N42 H41b 2.09(5) . . ? N42 H43a 2.00(8) . . ? N42 H43b 1.85(6) . . ? N42 H44a 2.50(9) . . ? C43 C45 2.470(17) . . ? C43 N46 2.887(13) . . ? C43 H41a 2.44(5) . . ? C43 H41b 2.67(6) . . ? C43 H42 1.84(7) . . ? C43 H44a 1.76(8) . . ? C43 H44b 2.14(11) . . ? C44 N46 2.455(13) . . ? C44 H42 2.45(8) . . ? C44 H43a 1.91(7) . . ? C44 H43b 1.91(5) . . ? C44 H45a 1.80(4) . . ? C44 H45b 2.00(6) . . ? C44 H46a 2.50(4) . . ? C45 H43b 2.62(5) . . ? C45 H44a 1.71(8) . . ? C45 H44b 2.02(9) . . ? C45 H46a 1.47(5) . . ? C45 H46b 1.97(6) . . ? N46 H36b 2.54(8) . . ? N46 H44a 2.67(8) . . ? N46 H45a 1.64(5) . . ? N46 H45b 1.86(5) . . ? N1 O22 3.087(11) . '2 664' ? N1 H01a 2.576(5) . '8 554' ? O11 O12 2.154(7) . . ? O11 O13 2.153(7) . . ? O11 O22 3.052(10) . '2 664' ? O11 H16a 2.69(5) . . ? O11 H21b 2.45(6) . . ? O11 H23b 2.58(5) . . ? O11 H46b 2.65(7) . '2 664' ? O12 O13 2.162(7) . . ? O12 O33 3.123(7) . '4 646' ? O12 O01 3.140(7) . '8 554' ? O12 H16b 2.63(5) . . ? O12 H25b 2.77(6) . . ? O12 H26b 2.80(7) . . ? O12 H01a 2.327(5) . '8 554' ? O13 O01 2.876(7) . '8 554' ? O13 H34b 2.72(8) . '7 645' ? O13 H36b 2.48(8) . '2 664' ? O13 H46b 2.18(6) . '2 664' ? O13 H01a 2.146(4) . '8 554' ? O21 O22 2.098(10) . . ? O21 O23 2.139(8) . . ? O21 O01 3.031(8) . . ? O21 H31b 2.43(5) . . ? O21 H33b 2.52(6) . . ? O21 H46a 2.58(5) . . ? O21 H01b 2.643(6) . . ? O22 O23 2.062(11) . . ? O22 H16a 2.31(5) . '2 665' ? O22 H46a 2.64(5) . . ? O23 O02 2.880(11) . . ? O23 H14b 2.57(7) . '6 556' ? O23 H24b 2.47(5) . '7 655' ? N3 H26b 2.69(9) . '4 656' ? O31 O32 2.076(8) . . ? O31 O33 2.111(8) . . ? O31 O03 2.773(18) . '8 565' ? O31 H11b 2.69(5) . '5 667' ? O31 H41b 2.38(6) . . ? O31 H43b 2.78(6) . . ? O32 O33 2.061(7) . . ? O32 H26b 2.41(8) . '4 656' ? O32 H32 2.23(5) . . ? O32 H36a 2.31(9) . . ? O33 H16b 2.32(6) . '4 656' ? O33 H22 2.56(6) . '5 667' ? O33 H24a 2.72(6) . '5 667' ? O33 H26b 2.25(9) . '4 656' ? O33 H41a 2.39(5) . '5 667' ? N4 O03 2.98(2) . . ? O41 O42 2.121(16) . . ? O41 O43 2.057(16) . . ? O41 O03 2.95(2) . . ? O41 H11a 2.62(5) . . ? O41 H25a 2.73(7) . '4 656' ? O41 H32 2.70(5) . . ? O41 H33a 2.75(7) . . ? O42 O43 2.150(17) . . ? O42 O02 3.007(18) . '2 664' ? O42 O03 2.57(2) . . ? O42 H36a 2.71(9) . '8 564' ? O42 H36b 2.68(7) . '8 564' ? O43 H12 2.43(6) . . ? O43 H31a 2.65(6) . . ? O43 H33a 2.80(8) . . ? O01 O02 3.167(13) . . ? O01 H21a 2.62(5) . . ? O01 H42 1.93(7) . . ? O02 H15b 2.75(7) . '6 556' ? O02 H35a 2.60(10) . '7 645' ? O02 H01b 2.695(12) . . ? O03 H26a 2.05(9) . '4 656' ? O03' H13b 2.60(6) . '4 656' ? O03' H26a 2.34(9) . '4 656' ? H11a H11b 1.76(8) . . ? H11a H12 2.16(8) . . ? H11a H13a 2.26(7) . . ? H11a H32 2.33(7) . . ? H11a H41b 2.38(8) . . ? H11b H13b 2.37(7) . . ? H11b H22 2.31(8) . . ? H12 H13a 2.24(7) . . ? H12 H14a 2.39(7) . . ? H12 H31a 2.23(7) . . ? H13a H13b 1.82(8) . . ? H13a H14a 2.21(7) . . ? H13a H14b 2.11(9) . . ? H13a H25a 2.35(9) . '4 656' ? H13b H14b 2.30(10) . . ? H14a H14b 1.47(8) . . ? H14a H15a 2.34(9) . . ? H14b H15a 2.32(10) . . ? H14b H15b 2.38(9) . . ? H15a H15b 1.61(11) . . ? H15a H16b 2.35(9) . . ? H15b H16b 2.10(8) . . ? H16a H16b 1.42(7) . . ? H16b H26b 2.03(10) . . ? H21a H21b 1.48(9) . . ? H21a H22 2.39(7) . . ? H21a H23a 2.21(9) . . ? H21a H01a 2.35(6) . . ? H21b H31b 2.21(8) . . ? H22 H23a 2.13(9) . . ? H22 H24a 2.26(8) . . ? H23a H23b 1.45(9) . . ? H23a H24a 2.30(8) . . ? H23a H24b 2.09(9) . . ? H23b H24b 2.37(7) . . ? H24a H24b 1.64(7) . . ? H24a H26a 2.36(11) . . ? H24b H25b 2.30(9) . . ? H25a H25b 1.30(10) . . ? H25a H26a 2.27(12) . . ? H25a H26b 2.07(11) . . ? H25b H26b 2.05(10) . . ? H26a H26b 1.79(13) . . ? H31a H31b 1.74(7) . . ? H31a H33a 2.22(9) . . ? H32 H33a 2.27(9) . . ? H32 H34a 2.38(8) . . ? H33a H33b 1.50(10) . . ? H33a H34b 2.29(10) . . ? H33b H35b 2.39(9) . . ? H34a H34b 1.48(10) . . ? H34a H35a 2.21(13) . . ? H34a H36a 2.22(11) . . ? H34b H35a 2.19(14) . . ? H34b H35b 2.26(11) . . ? H35a H35b 1.44(13) . . ? H35a H36a 2.19(14) . . ? H35a H36b 2.26(14) . . ? H36a H36b 1.45(12) . . ? H36b H46b 2.21(10) . . ? H41a H41b 1.89(8) . . ? H41a H42 2.35(8) . . ? H41a H43a 2.13(9) . . ? H42 H43a 2.06(10) . . ? H42 H44a 2.17(12) . . ? H42 H01b 2.29(7) . . ? H43a H43b 1.58(9) . . ? H43a H44a 2.00(10) . . ? H43a H44b 2.34(13) . . ? H43b H44a 2.38(9) . . ? H43b H44b 2.36(12) . . ? H44a H44b 1.56(13) . . ? H44a H45a 1.75(8) . . ? H44a H45b 2.32(9) . . ? H44b H45b 2.13(10) . . ? H45a H45b 1.22(8) . . ? H45a H46a 1.29(7) . . ? H45a H46b 2.16(7) . . ? H45b H46a 2.11(7) . . ? H45b H46b 2.17(8) . . ? H46a H46b 1.48(7) . . ? H01a H01b 1.5749(4) . . ? _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier' _atom_sites_solution_hydrogens 'difference Fourier' _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 3312 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 11 10 7 -11 10 7 11 -10 7 11 10 -7 11 -10 -7 -11 10 -7 -11 -10 7 -11 -10 -7 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 27 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _reflns_number_observed 3810 _reflns_d_resolution_high ? _reflns_d_resolution_low ? _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_theta_min ? _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'single counter' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .0789 _refine_ls_wR_factor_all .0715 _refine_ls_goodness_of_fit_all 1.383 _refine_ls_shift/su_mean .0019 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_global _audit_creation_method Xtal3.6 _audit_creation_date 00-02-28 _audit_update_record ? #============================================================================== # (Publishing Staff Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia Nedlands Western Australia 6907 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal test _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Skelton, Brian W.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; 'White, Allan H.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_yk5grn # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C23 H57 Cl5 Co1 N6 O4.5' _chemical_formula_moiety ? _chemical_formula_weight 725.95 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P_21_21_21 _symmetry_space_group_name_Hall p_2ac_2ab loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z _cell_length_a 17.339(7) _cell_length_b 15.529(4) _cell_length_c 12.625(4) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 3399(2) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 21.4 _cell_measurement_theta_max 23.2 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu .937 _exptl_crystal_description prism _exptl_crystal_size_max .75 _exptl_crystal_size_mid .42 _exptl_crystal_size_min .32 _exptl_crystal_size_rad ? _exptl_crystal_colour green _diffrn_measurement_device_type ; CAD4 diffractometer ; _diffrn_measurement_method '2\q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; XTAL absorb ; _exptl_absorpt_correction_T_min .68 _exptl_absorpt_correction_T_max .76 _diffrn_reflns_number 5459 _reflns_number_total 5459 _reflns_Friedel_coverage ? _reflns_number_gt 4124 _reflns_threshold_expression 'I > 3.00 sig(I )' _diffrn_reflns_theta_max 30 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_standards_number 10 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 #<< do not append units _diffrn_standards_decay_% ? #<< do not append % _refine_ls_structure_factor_coef F #<< use NfA code _refine_ls_R_factor_gt .046 _refine_ls_wR_factor_ref .048 _refine_ls_goodness_of_fit_ref 1.967 _refine_ls_number_reflns 4124 _refine_ls_number_parameters 362 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref #<< use NfA code _refine_ls_shift/su_max .074 _refine_diff_density_min -.695 _refine_diff_density_max .703 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Enraf Nonius software' _computing_cell_refinement 'Enraf Nonius software' _computing_data_reduction xtal _computing_structure_solution xtal _computing_structure_refinement xtal _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ 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 92 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 20 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' Co ? 0 4 .299 .973 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 18 .008 .006 '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' H ? 0 228 0 0 '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_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Co .64107(3) .41028(4) .17120(5) .0289(3) Uani ? ? 1.00000 ? ? Cl1 .69584(7) .53828(7) .21149(10) .0353(6) Uani ? ? 1.00000 ? ? Cl2 .58590(8) .28563(9) .12124(12) .0485(8) Uani ? ? 1.00000 ? ? Cl3 .42400(8) .18269(12) .49079(16) .0698(10) Uani ? ? 1.00000 ? ? Cl4 .81628(9) .03493(12) .08665(16) .0747(11) Uani ? ? 1.00000 ? ? Cl5 .56176(8) .43325(9) .67121(13) .0551(8) Uani ? ? 1.00000 ? ? C11 .7110(3) .2850(3) .3179(4) .032(2) Uani ? ? 1.00000 ? ? N12 .7298(2) .3518(2) .2399(3) .028(2) Uani ? ? 1.00000 ? ? C13 .7811(2) .3175(3) .1526(4) .030(2) Uani ? ? 1.00000 ? ? C14 .7822(3) .3855(3) .0661(4) .034(2) Uani ? ? 1.00000 ? ? N14 .7001(2) .4064(3) .0406(3) .037(2) Uani ? ? 1.00000 ? ? C15 .8274(3) .3533(3) -.0291(4) .044(3) Uani ? ? 1.00000 ? ? C16 .9099(3) .3316(4) .0036(5) .054(4) Uani ? ? 1.00000 ? ? C17 .9092(3) .2648(4) .0894(5) .049(3) Uani ? ? 1.00000 ? ? C18 .8633(3) .2952(3) .1856(4) .044(3) Uani ? ? 1.00000 ? ? C0 .6693(2) .3196(3) .4184(3) .027(2) Uani ? ? 1.00000 ? ? C21 .6273(3) .4054(3) .3995(3) .032(2) Uani ? ? 1.00000 ? ? N22 .58070(19) .4058(2) .3016(3) .0291(18) Uani ? ? 1.00000 ? ? C23 .5215(3) .4765(3) .2976(4) .034(2) Uani ? ? 1.00000 ? ? C24 .4885(3) .4725(3) .1873(4) .037(3) Uani ? ? 1.00000 ? ? N24 .5549(2) .4740(3) .1109(3) .036(2) Uani ? ? 1.00000 ? ? C25 .4300(3) .5435(3) .1704(5) .046(3) Uani ? ? 1.00000 ? ? C26 .3665(3) .5378(4) .2521(5) .053(3) Uani ? ? 1.00000 ? ? C27 .3975(3) .5381(4) .3632(5) .052(3) Uani ? ? 1.00000 ? ? C28 .4571(3) .4683(4) .3810(5) .046(3) Uani ? ? 1.00000 ? ? C31 .6124(2) .2482(3) .4498(4) .029(2) Uani ? ? 1.00000 ? ? N32 .5815(2) .2538(3) .5609(3) .032(2) Uani ? ? 1.00000 ? ? C33 .6267(3) .2028(3) .6401(4) .035(3) Uani ? ? 1.00000 ? ? C34 .5779(3) .1906(4) .7394(5) .056(4) Uani ? ? 1.00000 ? ? C35 .6203(4) .1369(4) .8218(5) .068(4) Uani ? ? 1.00000 ? ? C41 .7264(2) .3409(3) .5077(4) .030(2) Uani ? ? 1.00000 ? ? N42 .7522(2) .2661(3) .5739(3) .033(2) Uani ? ? 1.00000 ? ? C43 .7030(3) .2478(3) .6698(4) .034(2) Uani ? ? 1.00000 ? ? C44 .7464(3) .1915(4) .7472(5) .052(3) Uani ? ? 1.00000 ? ? C45 .6985(4) .1756(5) .8474(5) .069(4) Uani ? ? 1.00000 ? ? O01 .84249(19) .4685(2) .3672(3) .046(2) Uani ? ? 1.00000 ? ? O02 .7640(2) .1139(2) .4719(3) .064(3) Uani ? ? 1.00000 ? ? O03 .8692(3) .0951(3) .3180(4) .083(3) Uani ? ? 1.00000 ? ? O04 .4933(3) .4576(5) .9023(4) .123(5) Uani ? ? 1.00000 ? ? O05 .4402(7) .2500(9) .2920(14) .170(13) Uani ? ? .50500 ? ? H11a .75640 .25461 .33754 .04200 Uiso ? ? 1.00000 ? ? H11b .67686 .24347 .28299 .04200 Uiso ? ? 1.00000 ? ? H12 .75908 .39467 .27767 .03600 Uiso ? ? 1.00000 ? ? H13 .75865 .26552 .12597 .03600 Uiso ? ? 1.00000 ? ? H14 .80901 .43536 .09043 .04200 Uiso ? ? 1.00000 ? ? H14a .69825 .46235 .00634 .04400 Uiso ? ? 1.00000 ? ? H14b .67959 .36521 -.00647 .04400 Uiso ? ? 1.00000 ? ? H15a .80297 .30208 -.05681 .05800 Uiso ? ? 1.00000 ? ? H15b .82648 .39581 -.08449 .05800 Uiso ? ? 1.00000 ? ? H16a .93718 .31236 -.05928 .06500 Uiso ? ? 1.00000 ? ? H16b .93371 .38393 .02631 .06500 Uiso ? ? 1.00000 ? ? H17a .88381 .21239 .06376 .05900 Uiso ? ? 1.00000 ? ? H17b .96011 .24917 .10930 .05900 Uiso ? ? 1.00000 ? ? H18a .86369 .25547 .24230 .05600 Uiso ? ? 1.00000 ? ? H18b .88800 .34863 .21309 .05600 Uiso ? ? 1.00000 ? ? H21a .59500 .41873 .45917 .04100 Uiso ? ? 1.00000 ? ? H21b .66524 .45119 .39436 .04100 Uiso ? ? 1.00000 ? ? H22 .55438 .35193 .30727 .03600 Uiso ? ? 1.00000 ? ? H23 .54618 .53127 .31112 .04400 Uiso ? ? 1.00000 ? ? H24 .46276 .41774 .17844 .04600 Uiso ? ? 1.00000 ? ? H24a .54021 .44966 .04457 .04600 Uiso ? ? 1.00000 ? ? H24b .56986 .53296 .09883 .04600 Uiso ? ? 1.00000 ? ? H25a .45472 .59888 .17103 .05300 Uiso ? ? 1.00000 ? ? H25b .40843 .53856 .09652 .05300 Uiso ? ? 1.00000 ? ? H26a .33135 .58425 .24072 .06500 Uiso ? ? 1.00000 ? ? H26b .33901 .48473 .23866 .06500 Uiso ? ? 1.00000 ? ? H27a .42216 .59305 .37532 .06400 Uiso ? ? 1.00000 ? ? H27b .35687 .53142 .41154 .06400 Uiso ? ? 1.00000 ? ? H28a .47917 .47239 .45128 .05900 Uiso ? ? 1.00000 ? ? H28b .43434 .41240 .37471 .05900 Uiso ? ? 1.00000 ? ? H31a .57028 .25025 .40080 .03900 Uiso ? ? 1.00000 ? ? H31b .63823 .19419 .44125 .03900 Uiso ? ? 1.00000 ? ? H32a .52982 .23359 .56091 .03800 Uiso ? ? 1.00000 ? ? H32b .58195 .31285 .58258 .03800 Uiso ? ? 1.00000 ? ? H33 .63991 .14655 .61000 .04400 Uiso ? ? 1.00000 ? ? H34a .56567 .24544 .76857 .07000 Uiso ? ? 1.00000 ? ? H34b .52966 .16290 .72016 .07000 Uiso ? ? 1.00000 ? ? H35a .59348 .12652 .88126 .08900 Uiso ? ? 1.00000 ? ? H35b .63336 .07961 .78761 .08900 Uiso ? ? 1.00000 ? ? H41a .77104 .36624 .47652 .04000 Uiso ? ? 1.00000 ? ? H41b .70286 .38187 .55374 .04000 Uiso ? ? 1.00000 ? ? H42a .80328 .27617 .59628 .04000 Uiso ? ? 1.00000 ? ? H42b .75135 .21551 .52963 .04000 Uiso ? ? 1.00000 ? ? H43 .68914 .30148 .70301 .04200 Uiso ? ? 1.00000 ? ? H44a .79407 .21737 .76424 .07400 Uiso ? ? 1.00000 ? ? H44b .75623 .13673 .71363 .07400 Uiso ? ? 1.00000 ? ? H45a .69003 .22963 .88207 .09100 Uiso ? ? 1.00000 ? ? H45b .72724 .13938 .89492 .09100 Uiso ? ? 1.00000 ? ? H01a .85700 .48706 .29212 .05700 Uiso ? ? 1.00000 ? ? H01b .88040 .42482 .37101 .05700 Uiso ? ? 1.00000 ? ? H02a .75000 .06868 .50399 .12400 Uiso ? ? 1.00000 ? ? H02b .78973 .08958 .42205 .12400 Uiso ? ? 1.00000 ? ? 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 Co .0267(3) .0292(3) .0309(3) .0006(3) -.0031(3) .0009(3) Cl1 .0361(6) .0315(6) .0381(6) -.0039(5) .0003(5) .0019(5) Cl2 .0436(7) .0385(7) .0633(9) -.0063(6) -.0107(7) -.0098(7) Cl3 .0278(6) .0735(10) .1081(14) -.0079(7) -.0021(8) -.0207(10) Cl4 .0540(9) .0791(12) .0909(13) -.0148(9) -.0047(9) -.0135(11) Cl5 .0543(8) .0600(9) .0509(8) .0028(7) .0070(7) -.0119(8) C11 .034(2) .030(2) .033(2) .0050(19) .005(2) .005(2) N12 .0232(18) .033(2) .029(2) -.0005(16) -.0025(16) .0039(17) C13 .029(2) .032(2) .030(3) -.0023(19) .005(2) -.003(2) C14 .033(2) .035(3) .033(3) .002(2) .003(2) .002(2) N14 .043(2) .038(2) .029(2) .005(2) -.0021(19) .001(2) C15 .050(3) .047(3) .035(3) .004(3) .010(3) .005(2) C16 .048(3) .062(4) .052(4) .003(3) .023(3) -.005(3) C17 .037(3) .055(3) .055(3) .012(3) .001(3) -.011(3) C18 .034(2) .054(3) .044(3) .007(2) -.001(3) -.002(3) C0 .025(2) .031(2) .026(2) .0009(18) -.0040(18) .0038(19) C21 .032(2) .034(2) .030(2) .001(2) -.0002(19) -.002(2) N22 .0244(17) .0292(18) .034(2) .0004(16) -.0038(15) .0051(17) C23 .025(2) .033(2) .043(3) .005(2) -.001(2) -.000(2) C24 .031(2) .031(2) .051(3) .001(2) -.005(2) .006(2) N24 .034(2) .039(2) .036(2) -.0000(18) -.0059(18) .003(2) C25 .033(2) .042(3) .062(3) .006(2) -.010(3) .013(3) C26 .031(3) .048(3) .080(4) .011(3) .002(3) .008(3) C27 .033(3) .047(3) .078(4) .010(2) .008(3) .011(3) C28 .035(3) .044(3) .058(4) .003(2) .011(3) .007(3) C31 .027(2) .029(2) .032(2) -.004(2) -.004(2) .003(2) N32 .0207(17) .036(2) .039(2) -.0056(17) -.0008(17) .0036(19) C33 .032(2) .037(3) .037(3) -.003(2) .002(2) .005(2) C34 .054(3) .069(4) .043(3) -.013(3) .012(3) .005(3) C35 .080(5) .073(4) .050(4) -.011(4) .016(4) .020(4) C41 .026(2) .030(2) .035(3) -.0058(18) .001(2) .005(2) N42 .0228(18) .040(2) .037(2) .0003(17) -.0017(17) .0029(19) C43 .032(2) .040(2) .031(2) .001(2) .002(2) .003(2) C44 .053(3) .062(4) .041(3) .006(3) -.012(3) .011(3) C45 .095(5) .076(4) .035(3) .004(4) -.007(3) .013(3) O01 .0413(19) .050(2) .047(2) -.0018(17) .0025(17) -.0049(18) O02 .079(3) .045(2) .069(3) .013(2) .021(3) .000(2) O03 .089(3) .089(3) .071(3) -.001(3) .027(3) -.015(3) O04 .064(3) .258(8) .047(3) -.039(4) -.005(3) -.026(4) O05 .109(9) .145(12) .258(19) .053(9) -.100(12) -.100(13) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Co Cl1 . . 2.2609(14) ? Co Cl2 . . 2.2494(16) ? Co N12 . . 1.986(4) ? Co N14 . . 1.941(4) ? Co N22 . . 1.953(4) ? Co N24 . . 1.947(4) ? C11 N12 . . 1.468(6) ? C11 C0 . . 1.555(6) ? C11 H11a . . .951(4) ? C11 H11b . . .979(5) ? N12 C13 . . 1.513(6) ? N12 H12 . . .964(4) ? C13 C14 . . 1.519(7) ? C13 C18 . . 1.526(6) ? C13 H13 . . .956(4) ? C14 N14 . . 1.496(6) ? C14 C15 . . 1.520(7) ? C14 H14 . . .953(5) ? N14 H14a . . .971(4) ? N14 H14b . . .943(4) ? C15 C16 . . 1.525(8) ? C15 H15a . . .966(5) ? C15 H15b . . .962(5) ? C16 C17 . . 1.500(8) ? C16 H16a . . .972(6) ? C16 H16b . . .956(6) ? C17 C18 . . 1.525(8) ? C17 H17a . . .981(6) ? C17 H17b . . .950(5) ? C18 H18a . . .945(5) ? C18 H18b . . .997(5) ? C0 C21 . . 1.537(6) ? C0 C31 . . 1.537(6) ? C0 C41 . . 1.537(6) ? C21 N22 . . 1.476(6) ? C21 H21a . . .961(4) ? C21 H21b . . .971(5) ? N22 C23 . . 1.503(6) ? N22 H22 . . .956(4) ? C23 C24 . . 1.506(7) ? C23 C28 . . 1.541(7) ? C23 H23 . . .967(4) ? C24 N24 . . 1.501(6) ? C24 C25 . . 1.514(7) ? C24 H24 . . .967(5) ? N24 H24a . . .954(4) ? N24 H24b . . .964(4) ? C25 C26 . . 1.511(8) ? C25 H25a . . .961(5) ? C25 H25b . . 1.008(6) ? C26 C27 . . 1.502(9) ? C26 H26a . . .955(5) ? C26 H26b . . .967(6) ? C27 C28 . . 1.515(8) ? C27 H27a . . .966(6) ? C27 H27b . . .938(6) ? C28 H28a . . .968(6) ? C28 H28b . . .957(6) ? C31 N32 . . 1.504(6) ? C31 H31a . . .958(4) ? C31 H31b . . .957(4) ? N32 C33 . . 1.497(6) ? N32 H32a . . .950(4) ? N32 H32b . . .956(4) ? C33 C34 . . 1.524(8) ? C33 C43 . . 1.542(6) ? C33 H33 . . .981(5) ? C34 C35 . . 1.522(9) ? C34 H34a . . .952(6) ? C34 H34b . . .971(6) ? C35 C45 . . 1.518(10) ? C35 H35a . . .898(7) ? C35 H35b . . 1.014(7) ? C41 N42 . . 1.500(6) ? C41 H41a . . .953(4) ? C41 H41b . . .953(4) ? N42 C43 . . 1.507(6) ? N42 H42a . . .943(4) ? N42 H42b . . .964(4) ? C43 C44 . . 1.512(8) ? C43 H43 . . .963(5) ? C44 C45 . . 1.534(9) ? C44 H44a . . .944(6) ? C44 H44b . . .966(6) ? C45 H45a . . .958(7) ? C45 H45b . . .962(7) ? O01 H01a . . 1.022(4) ? O01 H01b . . .945(3) ? O02 H02a . . .847(4) ? O02 H02b . . .859(4) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published Cl1 Co Cl2 . . . 176.64(6) ? Cl1 Co N12 . . . 88.78(11) ? Cl1 Co N14 . . . 89.82(13) ? Cl1 Co N22 . . . 93.82(11) ? Cl1 Co N24 . . . 87.90(13) ? Cl2 Co N12 . . . 93.33(11) ? Cl2 Co N14 . . . 87.67(13) ? Cl2 Co N22 . . . 88.74(11) ? Cl2 Co N24 . . . 90.08(13) ? N12 Co N14 . . . 87.03(16) ? N12 Co N22 . . . 91.76(15) ? N12 Co N24 . . . 176.06(16) ? N14 Co N22 . . . 176.14(16) ? N14 Co N24 . . . 95.08(17) ? N22 Co N24 . . . 86.34(16) ? N12 C11 C0 . . . 114.0(4) ? N12 C11 H11a . . . 109.9(4) ? N12 C11 H11b . . . 107.3(4) ? C0 C11 H11a . . . 110.1(4) ? C0 C11 H11b . . . 108.3(4) ? H11a C11 H11b . . . 106.9(4) ? Co N12 C11 . . . 116.4(3) ? Co N12 C13 . . . 107.3(3) ? Co N12 H12 . . . 107.9(3) ? C11 N12 C13 . . . 111.8(3) ? C11 N12 H12 . . . 105.9(4) ? C13 N12 H12 . . . 107.1(3) ? N12 C13 C14 . . . 106.6(3) ? N12 C13 C18 . . . 115.5(4) ? N12 C13 H13 . . . 108.3(4) ? C14 C13 C18 . . . 110.0(4) ? C14 C13 H13 . . . 109.9(4) ? C18 C13 H13 . . . 106.5(4) ? C13 C14 N14 . . . 107.0(4) ? C13 C14 C15 . . . 110.2(4) ? C13 C14 H14 . . . 109.8(4) ? N14 C14 C15 . . . 113.1(4) ? N14 C14 H14 . . . 110.9(4) ? C15 C14 H14 . . . 105.7(4) ? Co N14 C14 . . . 109.0(3) ? Co N14 H14a . . . 109.5(3) ? Co N14 H14b . . . 111.0(3) ? C14 N14 H14a . . . 108.7(4) ? C14 N14 H14b . . . 110.3(4) ? H14a N14 H14b . . . 108.3(4) ? C14 C15 C16 . . . 110.0(4) ? C14 C15 H15a . . . 109.4(5) ? C14 C15 H15b . . . 109.9(5) ? C16 C15 H15a . . . 109.1(5) ? C16 C15 H15b . . . 111.3(5) ? H15a C15 H15b . . . 107.1(5) ? C15 C16 C17 . . . 109.9(5) ? C15 C16 H16a . . . 107.7(5) ? C15 C16 H16b . . . 107.4(5) ? C17 C16 H16a . . . 112.4(5) ? C17 C16 H16b . . . 112.0(5) ? H16a C16 H16b . . . 107.2(6) ? C16 C17 C18 . . . 111.5(5) ? C16 C17 H17a . . . 109.8(5) ? C16 C17 H17b . . . 111.1(5) ? C18 C17 H17a . . . 106.6(5) ? C18 C17 H17b . . . 110.7(5) ? H17a C17 H17b . . . 106.9(6) ? C13 C18 C17 . . . 109.9(4) ? C13 C18 H18a . . . 111.2(4) ? C13 C18 H18b . . . 107.9(4) ? C17 C18 H18a . . . 113.5(5) ? C17 C18 H18b . . . 108.1(4) ? H18a C18 H18b . . . 106.0(5) ? C11 C0 C21 . . . 113.2(4) ? C11 C0 C31 . . . 105.0(3) ? C11 C0 C41 . . . 112.0(3) ? C21 C0 C31 . . . 111.2(3) ? C21 C0 C41 . . . 103.4(3) ? C31 C0 C41 . . . 112.3(4) ? C0 C21 N22 . . . 113.2(4) ? C0 C21 H21a . . . 110.0(4) ? C0 C21 H21b . . . 108.9(4) ? N22 C21 H21a . . . 109.6(4) ? N22 C21 H21b . . . 108.1(4) ? H21a C21 H21b . . . 106.8(4) ? Co N22 C21 . . . 114.4(3) ? Co N22 C23 . . . 108.1(3) ? Co N22 H22 . . . 110.5(3) ? C21 N22 C23 . . . 113.9(3) ? C21 N22 H22 . . . 101.2(3) ? C23 N22 H22 . . . 108.4(3) ? N22 C23 C24 . . . 105.1(4) ? N22 C23 C28 . . . 114.3(4) ? N22 C23 H23 . . . 109.5(4) ? C24 C23 C28 . . . 110.7(4) ? C24 C23 H23 . . . 111.6(4) ? C28 C23 H23 . . . 105.8(4) ? C23 C24 N24 . . . 107.5(4) ? C23 C24 C25 . . . 110.8(4) ? C23 C24 H24 . . . 108.6(4) ? N24 C24 C25 . . . 114.4(4) ? N24 C24 H24 . . . 107.1(4) ? C25 C24 H24 . . . 108.3(4) ? Co N24 C24 . . . 109.2(3) ? Co N24 H24a . . . 110.3(3) ? Co N24 H24b . . . 109.8(3) ? C24 N24 H24a . . . 110.7(4) ? C24 N24 H24b . . . 108.8(4) ? H24a N24 H24b . . . 108.0(4) ? C24 C25 C26 . . . 110.5(5) ? C24 C25 H25a . . . 110.5(4) ? C24 C25 H25b . . . 108.8(5) ? C26 C25 H25a . . . 111.9(5) ? C26 C25 H25b . . . 110.9(4) ? H25a C25 H25b . . . 103.9(5) ? C25 C26 C27 . . . 112.1(4) ? C25 C26 H26a . . . 108.5(5) ? C25 C26 H26b . . . 106.8(5) ? C27 C26 H26a . . . 111.5(6) ? C27 C26 H26b . . . 110.1(5) ? H26a C26 H26b . . . 107.7(5) ? C26 C27 C28 . . . 112.4(5) ? C26 C27 H27a . . . 108.0(5) ? C26 C27 H27b . . . 109.8(5) ? C28 C27 H27a . . . 107.9(5) ? C28 C27 H27b . . . 109.7(5) ? H27a C27 H27b . . . 109.1(6) ? C23 C28 C27 . . . 109.5(5) ? C23 C28 H28a . . . 109.5(4) ? C23 C28 H28b . . . 108.5(5) ? C27 C28 H28a . . . 111.0(5) ? C27 C28 H28b . . . 110.8(5) ? H28a C28 H28b . . . 107.4(6) ? C0 C31 N32 . . . 115.3(4) ? C0 C31 H31a . . . 107.4(4) ? C0 C31 H31b . . . 107.6(4) ? N32 C31 H31a . . . 109.2(4) ? N32 C31 H31b . . . 108.9(4) ? H31a C31 H31b . . . 108.3(4) ? C31 N32 C33 . . . 114.0(3) ? C31 N32 H32a . . . 108.5(4) ? C31 N32 H32b . . . 108.7(4) ? C33 N32 H32a . . . 108.6(4) ? C33 N32 H32b . . . 108.2(4) ? H32a N32 H32b . . . 108.9(4) ? N32 C33 C34 . . . 109.0(4) ? N32 C33 C43 . . . 111.8(4) ? N32 C33 H33 . . . 109.5(4) ? C34 C33 C43 . . . 109.5(4) ? C34 C33 H33 . . . 109.7(4) ? C43 C33 H33 . . . 107.3(4) ? C33 C34 C35 . . . 111.2(5) ? C33 C34 H34a . . . 109.2(5) ? C33 C34 H34b . . . 109.1(5) ? C35 C34 H34a . . . 109.4(5) ? C35 C34 H34b . . . 110.1(6) ? H34a C34 H34b . . . 107.5(6) ? C34 C35 C45 . . . 111.1(5) ? C34 C35 H35a . . . 114.9(6) ? C34 C35 H35b . . . 107.3(6) ? C45 C35 H35a . . . 110.8(6) ? C45 C35 H35b . . . 103.7(6) ? H35a C35 H35b . . . 108.3(7) ? C0 C41 N42 . . . 115.7(4) ? C0 C41 H41a . . . 107.9(4) ? C0 C41 H41b . . . 108.3(4) ? N42 C41 H41a . . . 108.0(4) ? N42 C41 H41b . . . 107.8(4) ? H41a C41 H41b . . . 109.0(4) ? C41 N42 C43 . . . 115.1(3) ? C41 N42 H42a . . . 108.5(4) ? C41 N42 H42b . . . 107.7(4) ? C43 N42 H42a . . . 108.8(4) ? C43 N42 H42b . . . 107.7(4) ? H42a N42 H42b . . . 108.8(4) ? C33 C43 N42 . . . 112.1(4) ? C33 C43 C44 . . . 108.8(4) ? C33 C43 H43 . . . 106.5(4) ? N42 C43 C44 . . . 110.2(4) ? N42 C43 H43 . . . 109.2(4) ? C44 C43 H43 . . . 110.0(5) ? C43 C44 C45 . . . 110.9(5) ? C43 C44 H44a . . . 109.7(5) ? C43 C44 H44b . . . 108.3(5) ? C45 C44 H44a . . . 110.8(5) ? C45 C44 H44b . . . 108.4(5) ? H44a C44 H44b . . . 108.6(6) ? C35 C45 C44 . . . 111.8(5) ? C35 C45 H45a . . . 107.9(6) ? C35 C45 H45b . . . 111.4(6) ? C44 C45 H45a . . . 108.5(6) ? C44 C45 H45b . . . 109.1(6) ? H45a C45 H45b . . . 107.9(6) ? H01a O01 H01b . . . 94.5(3) ? H02a O02 H02b . . . 97.7(4) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- 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 Co C11 2.947(5) . . ? Co C13 2.833(4) . . ? Co C14 2.810(5) . . ? Co C0 3.459(5) . . ? Co C21 2.893(5) . . ? Co C23 2.810(5) . . ? Co C24 2.823(5) . . ? Co H11b 3.0145(9) . . ? Co H12 2.4602(9) . . ? Co H13 3.0880(9) . . ? Co H14 3.1098(12) . . ? Co H14a 2.4431(9) . . ? Co H14b 2.4428(9) . . ? Co H21b 2.9184(11) . . ? Co H22 2.4559(8) . . ? Co H23 3.0590(8) . . ? Co H24 3.0952(14) . . ? Co H24a 2.4471(8) . . ? Co H24b 2.4472(8) . . ? Cl1 Cl3 3.984(2) . '4 655' ? Cl1 N12 2.977(4) . . ? Cl1 C14 3.352(5) . . ? Cl1 N14 2.975(4) . . ? Cl1 C21 3.362(5) . . ? Cl1 N22 3.084(4) . . ? Cl1 C23 3.352(5) . . ? Cl1 N24 2.929(4) . . ? Cl1 C41 3.457(5) . '2 664' ? Cl1 O01 3.392(4) . . ? Cl1 H12 2.6218(12) . . ? Cl1 H14 2.9565(13) . . ? Cl1 H14a 2.8461(14) . . ? Cl1 H15b 2.7985(15) . '2 665' ? Cl1 H21b 2.7278(14) . . ? Cl1 H23 2.8858(16) . . ? Cl1 H24b 2.6079(15) . . ? Cl1 H41b 2.9307(14) . '2 664' ? Cl1 H43 3.1907(13) . '2 664' ? Cl1 H01a 3.0785(16) . . ? Cl2 C11 3.297(5) . . ? Cl2 N12 3.086(4) . . ? Cl2 C13 3.443(5) . . ? Cl2 N14 2.911(4) . . ? Cl2 N22 2.946(4) . . ? Cl2 C24 3.459(5) . . ? Cl2 N24 2.977(4) . . ? Cl2 O05 3.366(15) . . ? Cl2 H11b 2.6620(16) . . ? Cl2 H13 3.0121(18) . . ? Cl2 H14b 2.6011(15) . . ? Cl2 H16a 3.0947(17) . '3 455' ? Cl2 H22 2.6220(16) . . ? Cl2 H24 3.0478(16) . . ? Cl2 H24a 2.8378(15) . . ? Cl2 H27a 2.9942(16) . '4 645' ? Cl3 C31 3.460(5) . . ? Cl3 N32 3.076(4) . . ? Cl3 C41 3.445(5) . '3 456' ? Cl3 N42 3.190(4) . '3 456' ? Cl3 O01 3.274(4) . '3 456' ? Cl3 O05 2.734(18) . . ? Cl3 H24b 2.588(2) . '4 645' ? Cl3 H31a 2.9706(18) . . ? Cl3 H32a 2.1852(17) . . ? Cl3 H41a 2.7896(18) . '3 456' ? Cl3 H42a 2.4491(17) . '3 456' ? Cl3 H01b 2.530(2) . '3 456' ? Cl4 O02 3.063(4) . '2 654' ? Cl4 O03 3.201(5) . . ? Cl4 O04 3.075(5) . '3 556' ? Cl4 H17a 3.008(2) . . ? Cl4 H25b 3.034(2) . 3 ? Cl4 H27b 3.003(2) . '4 645' ? Cl4 H33 2.934(2) . '2 654' ? Cl4 H02a 2.2357(19) . '2 654' ? Cl5 N32 3.134(4) . . ? Cl5 O01 3.348(4) . '2 665' ? Cl5 O03 3.371(5) . '3 456' ? Cl5 O04 3.172(5) . . ? Cl5 H14 3.1975(16) . '2 665' ? Cl5 H21a 2.7476(18) . . ? Cl5 H28a 3.1827(18) . . ? Cl5 H32b 2.2069(15) . . ? Cl5 H34a 3.1657(16) . . ? Cl5 H41b 2.9701(17) . . ? Cl5 H43 3.0375(16) . . ? Cl5 H01a 2.4178(16) . '2 665' ? C11 C13 2.468(7) . . ? C11 C21 2.581(6) . . ? C11 N22 2.944(6) . . ? C11 C31 2.454(6) . . ? C11 C41 2.563(7) . . ? C11 H12 1.964(4) . . ? C11 H13 2.578(5) . . ? C11 H31b 2.450(5) . . ? C11 H41a 2.586(5) . . ? N12 C14 2.432(6) . . ? N12 N14 2.704(5) . . ? N12 C18 2.569(6) . . ? N12 C0 2.535(6) . . ? N12 C21 2.813(6) . . ? N12 N22 2.828(5) . . ? N12 H11a 2.002(4) . . ? N12 H11b 1.992(4) . . ? N12 H13 2.028(4) . . ? N12 H14 2.671(4) . . ? C13 N14 2.424(6) . . ? C13 C15 2.493(7) . . ? C13 C16 2.928(7) . . ? C13 C17 2.497(7) . . ? C13 H11a 2.567(5) . . ? C13 H12 2.019(5) . . ? C13 H14 2.050(5) . . ? C13 H15a 2.681(5) . . ? C13 H17a 2.663(4) . . ? C13 H18a 2.065(4) . . ? C13 H18b 2.063(4) . . ? C14 C16 2.494(7) . . ? C14 C17 2.906(7) . . ? C14 C18 2.494(7) . . ? C14 H13 2.052(5) . . ? C14 H14a 2.028(5) . . ? C14 H14b 2.026(5) . . ? C14 H15a 2.053(5) . . ? C14 H15b 2.056(5) . . ? C14 H16b 2.674(5) . . ? C14 H18b 2.671(5) . . ? N14 C15 2.516(7) . . ? N14 N24 2.868(6) . . ? N14 O01 3.020(5) . '2 664' ? N14 H13 2.642(4) . . ? N14 H14 2.041(4) . . ? C15 C17 2.477(8) . . ? C15 C18 2.923(7) . . ? C15 H13 2.667(5) . . ? C15 H14 2.001(5) . . ? C15 H14b 2.585(5) . . ? C15 H16a 2.042(5) . . ? C15 H16b 2.028(5) . . ? C15 H17a 2.668(5) . . ? C16 C18 2.500(8) . . ? C16 H14 2.618(6) . . ? C16 H15a 2.056(6) . . ? C16 H15b 2.078(6) . . ? C16 H17a 2.052(6) . . ? C16 H17b 2.044(6) . . ? C16 H18b 2.685(6) . . ? C17 H13 2.650(5) . . ? C17 H15a 2.671(6) . . ? C17 H16a 2.075(6) . . ? C17 H16b 2.058(6) . . ? C17 H18a 2.090(6) . . ? C17 H18b 2.065(6) . . ? C18 H12 2.647(5) . . ? C18 H13 2.017(5) . . ? C18 H14 2.659(5) . . ? C18 H17a 2.035(5) . . ? C18 H17b 2.063(5) . . ? C0 N22 2.515(6) . . ? C0 N32 2.569(6) . . ? C0 N42 2.571(6) . . ? C0 H11a 2.083(4) . . ? C0 H11b 2.082(4) . . ? C0 H12 2.634(4) . . ? C0 H21a 2.073(4) . . ? C0 H21b 2.067(4) . . ? C0 H22 2.488(4) . . ? C0 H31a 2.039(4) . . ? C0 H31b 2.041(4) . . ? C0 H32b 2.570(4) . . ? C0 H41a 2.043(4) . . ? C0 H41b 2.048(4) . . ? C0 H42b 2.571(4) . . ? C21 C23 2.498(6) . . ? C21 C31 2.536(7) . . ? C21 C41 2.413(6) . . ? C21 H22 1.909(4) . . ? C21 H23 2.654(5) . . ? C21 H31a 2.604(5) . . ? C21 H41b 2.375(4) . . ? N22 C24 2.390(6) . . ? N22 N24 2.668(5) . . ? N22 C28 2.557(6) . . ? N22 H21a 2.014(4) . . ? N22 H21b 2.004(3) . . ? N22 H23 2.042(4) . . ? N22 H24 2.576(3) . . ? C23 N24 2.426(7) . . ? C23 C25 2.486(7) . . ? C23 C26 2.910(7) . . ? C23 C27 2.496(7) . . ? C23 H21a 2.567(5) . . ? C23 H22 2.020(5) . . ? C23 H24 2.033(5) . . ? C23 H27a 2.685(5) . . ? C23 H28a 2.076(5) . . ? C23 H28b 2.056(5) . . ? C24 C26 2.486(7) . . ? C24 C27 2.909(8) . . ? C24 C28 2.507(8) . . ? C24 H22 2.665(5) . . ? C24 H23 2.068(5) . . ? C24 H24a 2.043(5) . . ? C24 H24b 2.029(5) . . ? C24 H25a 2.058(5) . . ? C24 H25b 2.072(5) . . ? C24 H26b 2.679(5) . . ? N24 C25 2.534(6) . . ? N24 O04 2.854(6) . '1 554' ? N24 H23 2.683(4) . . ? N24 H24 2.010(4) . . ? C25 C27 2.499(9) . . ? C25 C28 2.942(8) . . ? C25 H23 2.693(5) . . ? C25 H24 2.037(5) . . ? C25 H24b 2.594(5) . . ? C25 H26a 2.027(5) . . ? C25 H26b 2.015(5) . . ? C26 C28 2.507(8) . . ? C26 H24 2.670(6) . . ? C26 H25a 2.071(6) . . ? C26 H25b 2.095(6) . . ? C26 H27a 2.022(6) . . ? C26 H27b 2.022(7) . . ? C27 H23 2.663(5) . . ? C27 H26a 2.054(6) . . ? C27 H26b 2.046(6) . . ? C27 H28a 2.070(6) . . ? C27 H28b 2.059(6) . . ? C28 H21a 2.699(5) . . ? C28 H22 2.642(5) . . ? C28 H23 2.030(5) . . ? C28 H24 2.677(6) . . ? C28 H27a 2.031(6) . . ? C28 H27b 2.032(5) . . ? C31 C33 2.516(7) . . ? C31 C41 2.553(6) . . ? C31 N42 2.899(6) . . ? C31 H11b 2.386(5) . . ? C31 H21a 2.668(5) . . ? C31 H22 2.617(5) . . ? C31 H32a 2.017(4) . . ? C31 H32b 2.024(5) . . ? C31 H33 2.609(5) . . ? C31 H42b 2.660(4) . . ? N32 C34 2.459(7) . . ? N32 C41 2.931(6) . . ? N32 N42 2.969(5) . . ? N32 C43 2.516(6) . . ? N32 H31a 2.031(4) . . ? N32 H31b 2.027(4) . . ? N32 H33 2.046(4) . . ? N32 H34a 2.639(4) . . ? N32 H34b 2.616(4) . . ? N32 H43 2.692(4) . . ? C33 C35 2.514(8) . . ? C33 N42 2.529(6) . . ? C33 C44 2.483(7) . . ? C33 C45 2.929(8) . . ? C33 H31b 2.523(5) . . ? C33 H32a 2.012(5) . . ? C33 H32b 2.012(5) . . ? C33 H34a 2.046(5) . . ? C33 H34b 2.058(5) . . ? C33 H35b 2.672(5) . . ? C33 H42b 2.580(5) . . ? C33 H43 2.037(5) . . ? C33 H44b 2.638(5) . . ? C34 C43 2.504(7) . . ? C34 C44 2.923(8) . . ? C34 C45 2.507(9) . . ? C34 H32a 2.494(6) . . ? C34 H33 2.072(6) . . ? C34 H35a 2.066(6) . . ? C34 H35b 2.065(6) . . ? C34 H43 2.627(6) . . ? C35 C43 2.951(8) . . ? C35 C44 2.527(9) . . ? C35 H33 2.699(7) . . ? C35 H34a 2.046(7) . . ? C35 H34b 2.068(7) . . ? C35 H45a 2.029(7) . . ? C35 H45b 2.073(7) . . ? C41 C43 2.538(7) . . ? C41 H11a 2.586(5) . . ? C41 H21a 2.651(4) . . ? C41 H21b 2.471(4) . . ? C41 H42a 2.009(4) . . ? C41 H42b 2.014(4) . . ? C41 H43 2.621(5) . . ? N42 C44 2.477(7) . . ? N42 O02 2.699(6) . . ? N42 H41a 2.010(4) . . ? N42 H41b 2.007(4) . . ? N42 H43 2.038(4) . . ? N42 H44a 2.621(4) . . ? N42 H44b 2.674(4) . . ? C43 C45 2.509(8) . . ? C43 H32b 2.576(5) . . ? C43 H33 2.059(5) . . ? C43 H34a 2.688(5) . . ? C43 H41b 2.545(5) . . ? C43 H42a 2.020(5) . . ? C43 H42b 2.021(5) . . ? C43 H44a 2.035(5) . . ? C43 H44b 2.034(5) . . ? C44 H33 2.626(6) . . ? C44 H35b 2.668(6) . . ? C44 H42a 2.517(6) . . ? C44 H43 2.052(6) . . ? C44 H45a 2.050(6) . . ? C44 H45b 2.060(6) . . ? C45 H35a 2.019(7) . . ? C45 H35b 2.016(7) . . ? C45 H43 2.678(7) . . ? C45 H44a 2.067(7) . . ? C45 H44b 2.054(6) . . ? O01 O04 3.102(6) . '2 664' ? O01 H12 2.164(3) . . ? O01 H14a 2.177(4) . '2 665' ? O01 H41a 2.441(4) . . ? O02 O03 2.681(6) . . ? O02 H11a 2.769(4) . . ? O02 H31b 2.541(4) . . ? O02 H42b 1.752(4) . . ? O03 H18a 2.668(5) . . ? O03 H35b 2.741(5) . '2 654' ? O03 H02b 1.906(5) . . ? O04 H24a 1.975(5) . '1 556' ? O05 H22 2.542(13) . . ? O05 H28b 2.731(15) . . ? O05 H31a 2.641(14) . . ? O05 H42a 2.792(14) . '3 456' ? O05 H44a 2.680(12) . '3 456' ? H11a H11b 1.5512(5) . . ? H11a H12 2.3031(5) . . ? H11a H18a 2.2151(7) . . ? H11b H31a 2.3745(7) . . ? H11b H31b 2.2420(6) . . ? H12 H21b 2.3639(5) . . ? H12 H01a 2.2303(6) . . ? H13 H18a 2.3449(6) . . ? H14 H14a 2.2340(7) . . ? H14 H15b 2.3121(7) . . ? H14a H14b 1.5512(4) . . ? H15a H15b 1.5514(4) . . ? H15a H16a 2.3327(9) . . ? H15a H45a 2.3866(7) . '1 554' ? H15b H16a 2.3377(7) . . ? H15b H16b 2.3340(7) . . ? H15b H21b 2.3952(6) . '2 664' ? H16a H16b 1.5513(3) . . ? H16a H17a 2.3831(4) . . ? H16a H17b 2.3771(6) . . ? H16b H17b 2.3847(5) . . ? H17a H17b 1.5515(5) . . ? H17a H18a 2.3770(7) . . ? H17b H18a 2.3715(6) . . ? H17b H18b 2.3803(4) . . ? H17b H34a 2.3947(6) . '3 556' ? H18a H18b 1.5513(4) . . ? H18b H01b 2.3221(6) . . ? H21a H21b 1.5514(4) . . ? H21a H22 2.2913(5) . . ? H21a H28a 2.1767(8) . . ? H21a H32b 2.2764(5) . . ? H21a H41b 2.2914(6) . . ? H21b H41b 2.3734(6) . . ? H22 H31a 1.9909(4) . . ? H23 H28a 2.3059(5) . . ? H24 H24a 2.2149(5) . . ? H24 H25b 2.3404(4) . . ? H24a H24b 1.5514(3) . . ? H25a H25b 1.5513(3) . . ? H25a H26a 2.3241(8) . . ? H25b H26a 2.3673(5) . . ? H25b H26b 2.3169(5) . . ? H26a H26b 1.5514(4) . . ? H26a H27a 2.3207(6) . . ? H26a H27b 2.3494(6) . . ? H26b H27b 2.3206(7) . . ? H27a H27b 1.5513(4) . . ? H27a H28a 2.3254(4) . . ? H27b H28a 2.3641(8) . . ? H27b H28b 2.3317(5) . . ? H28a H28b 1.5513(3) . . ? H31a H31b 1.5514(4) . . ? H31a H32a 2.1552(6) . . ? H31b H33 2.2554(6) . . ? H31b H42b 2.2807(7) . . ? H32a H32b 1.5514(3) . . ? H32a H34b 2.2907(6) . . ? H32b H41b 2.3825(8) . . ? H33 H34b 2.3776(7) . . ? H34a H34b 1.5512(3) . . ? H34a H35a 2.3805(5) . . ? H34b H35a 2.3834(6) . . ? H34b H35b 2.3730(6) . . ? H35a H35b 1.5514(3) . . ? H35a H45a 2.3166(6) . . ? H35a H45b 2.3342(9) . . ? H35b H45b 2.3123(5) . . ? H41a H41b 1.5514(4) . . ? H41a H42a 2.1342(4) . . ? H41b H43 2.2730(5) . . ? H42a H42b 1.5512(3) . . ? H42a H44a 2.3143(6) . . ? H42b H02a 2.3031(6) . . ? H43 H44a 2.3693(6) . . ? H44a H44b 1.5514(3) . . ? H44a H45a 2.3459(6) . . ? H44a H45b 2.3519(5) . . ? H44b H45b 2.3437(7) . . ? H45a H45b 1.5514(3) . . ? H01a H01b 1.4460(3) . . ? H02a H02b 1.2845(3) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1540 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 10 9 9 10 -9 9 -10 9 -9 -10 -9 -9 18 0 0 -18 0 0 0 16 0 0 -16 0 0 0 14 0 0 -14 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 24 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 17 _reflns_number_observed ? _reflns_d_resolution_high ? _reflns_d_resolution_low ? _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_theta_min ? _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type Full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .060 _refine_ls_wR_factor_all .050 _refine_ls_goodness_of_fit_all 1.945 _refine_ls_shift/su_mean .0054 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_global _audit_creation_method Xtal3.6 _audit_creation_date 00-09-15 _audit_update_record ? #============================================================================== # (Publishing Staff Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia Nedlands Western Australia 6907 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal ? _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Skelton, Brian W.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Pogram for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_yk24pf # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C13 H32 Cl1 Cu1 F6 N5 O3.5 P1' _chemical_formula_moiety ? _chemical_formula_weight 558.39 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 6.5904(8) _cell_length_b 17.471(2) _cell_length_c 19.014(2) _cell_angle_alpha 90.00000 _cell_angle_beta 96.038(2) _cell_angle_gamma 90.00000 _cell_volume 2177.1(4) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.704 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 2975 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 22.4 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu 1.278 _exptl_crystal_description frames _exptl_crystal_size_max .15 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .06 _exptl_crystal_size_rad ? _exptl_crystal_colour purple _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .757 _exptl_absorpt_correction_T_max .928 _diffrn_reflns_number 21705 _reflns_number_total 5523 _reflns_Friedel_coverage 0 _reflns_number_gt 3592 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.25 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .055 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .051 _refine_ls_wR_factor_ref .056 _refine_ls_goodness_of_fit_ref 1.35 _refine_ls_number_reflns 3592 _refine_ls_number_parameters 325 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .062 _refine_diff_density_min -.614 _refine_diff_density_max .731 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ 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 52 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 128 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 4 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cu ? 0 4 .263 1.266 'Int Tables Vol IV Tables 2.2B and 2.3.1' F ? 0 24 .014 .01 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 20 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 14 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 4 .09 .095 '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_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu .64225(8) .75790(3) .06457(2) .0210(3) Uani ? ? 1.00000 ? ? Cl .27950(16) .82813(6) .06741(6) .0301(6) Uani ? ? 1.00000 ? ? O0 .9926(5) .6882(2) .05898(19) .054(2) Uani ? ? 1.00000 ? ? C1 .7009(6) .8865(2) -.0670(2) .023(2) Uani ? ? 1.00000 ? ? C11 .6260(7) .9517(3) -.1174(2) .032(2) Uani ? ? 1.00000 ? ? N1 .9218(5) .8711(2) -.08143(18) .028(2) Uani ? ? 1.00000 ? ? O11 1.0421(5) .92661(19) -.07453(18) .044(2) Uani ? ? 1.00000 ? ? O12 .9709(5) .80898(19) -.09938(18) .044(2) Uani ? ? 1.00000 ? ? C2 .5660(6) .8168(2) -.0850(2) .023(2) Uani ? ? 1.00000 ? ? N3 .6145(5) .74737(18) -.04185(16) .0197(16) Uani ? ? 1.00000 ? ? C4 .4601(6) .6866(2) -.0595(2) .024(2) Uani ? ? 1.00000 ? ? C5 .5038(7) .6221(2) -.0074(2) .028(2) Uani ? ? 1.00000 ? ? N6 .5041(5) .65480(19) .06532(16) .0227(18) Uani ? ? 1.00000 ? ? C7 .5797(7) .5994(2) .1212(2) .027(2) Uani ? ? 1.00000 ? ? C8 .5778(6) .6310(2) .1964(2) .027(2) Uani ? ? 1.00000 ? ? C81 .3624(7) .6576(2) .2097(2) .030(2) Uani ? ? 1.00000 ? ? C82 .6415(8) .5651(3) .2477(2) .037(3) Uani ? ? 1.00000 ? ? C2' .7060(6) .9146(2) .0095(2) .024(2) Uani ? ? 1.00000 ? ? N3' .7914(5) .85881(19) .06264(16) .0213(17) Uani ? ? 1.00000 ? ? C4' .8021(6) .8906(2) .1358(2) .025(2) Uani ? ? 1.00000 ? ? C5' .8481(6) .8254(2) .1868(2) .026(2) Uani ? ? 1.00000 ? ? N6' .6892(5) .76617(19) .17053(17) .0217(17) Uani ? ? 1.00000 ? ? C7' .7334(6) .6950(2) .2120(2) .027(2) Uani ? ? 1.00000 ? ? P1 .4173(2) .90168(10) .32826(7) .0498(9) Uani ? ? 1.00000 ? ? F1 .4301(4) .86414(17) .40518(14) .0507(18) Uani ? ? 1.00000 ? ? F2 .4078(19) .9596(7) .2616(7) .094(8) Uani ? ? .50000 ? ? F3 .2476(11) .8274(5) .3101(4) .062(5) Uani ? ? .50000 ? ? F4 .5815(12) .8287(6) .3147(4) .069(5) Uani ? ? .50000 ? ? F5 .584(2) .9524(9) .3507(8) .127(12) Uani ? ? .50000 ? ? F6 .244(2) .9476(8) .3454(7) .110(10) Uani ? ? .50000 ? ? F2' .408(3) .9150(6) .2467(7) .100(8) Uani ? ? .50000 ? ? F3' .1815(14) .9061(8) .3206(6) .087(8) Uani ? ? .50000 ? ? F4' .439(3) .8351(6) .2874(5) .126(10) Uani ? ? .50000 ? ? F5' .6574(15) .9217(8) .3410(7) .074(7) Uani ? ? .50000 ? ? F6' .3983(18) .9858(5) .3748(7) .110(8) Uani ? ? .50000 ? ? O01 1.0650(12) .5429(4) .0273(4) .067(5) Uani ? ? .50000 ? ? H11a .62046 .93575 -.16568 .04900 Uiso ? ? 1.00000 ? ? H11b .71389 .99511 -.11084 .04900 Uiso ? ? 1.00000 ? ? H11c .49063 .96775 -.10885 .04900 Uiso ? ? 1.00000 ? ? H2a .57419 .80404 -.13351 .02900 Uiso ? ? 1.00000 ? ? H2b .42766 .83082 -.07969 .02900 Uiso ? ? 1.00000 ? ? H3 .74369 .73190 -.05229 .02500 Uiso ? ? 1.00000 ? ? H4a .46672 .66919 -.10714 .03000 Uiso ? ? 1.00000 ? ? H4b .32615 .70665 -.05637 .03000 Uiso ? ? 1.00000 ? ? H5a .63433 .59989 -.01326 .03500 Uiso ? ? 1.00000 ? ? H5b .40274 .58280 -.01553 .03500 Uiso ? ? 1.00000 ? ? H6 .35828 .66939 .07500 .02800 Uiso ? ? 1.00000 ? ? H7a .71611 .58497 .11387 .03500 Uiso ? ? 1.00000 ? ? H7b .49605 .55432 .11634 .03500 Uiso ? ? 1.00000 ? ? H81a .26600 .61670 .19924 .04500 Uiso ? ? 1.00000 ? ? H81b .32027 .70019 .18065 .04500 Uiso ? ? 1.00000 ? ? H81c .35904 .67161 .25815 .04500 Uiso ? ? 1.00000 ? ? H82a .55008 .52321 .24045 .05700 Uiso ? ? 1.00000 ? ? H82b .64342 .58206 .29580 .05700 Uiso ? ? 1.00000 ? ? H82c .77656 .54767 .24105 .05700 Uiso ? ? 1.00000 ? ? H2'a .56862 .92620 .01955 .03200 Uiso ? ? 1.00000 ? ? H2'b .78389 .96061 .01509 .03200 Uiso ? ? 1.00000 ? ? H3' .91885 .84774 .04999 .02600 Uiso ? ? 1.00000 ? ? H4'a .67475 .91347 .14377 .03100 Uiso ? ? 1.00000 ? ? H4'b .90620 .92893 .14268 .03100 Uiso ? ? 1.00000 ? ? H5'a .84954 .84261 .23473 .03200 Uiso ? ? 1.00000 ? ? H5'b .98064 .80444 .18133 .03200 Uiso ? ? 1.00000 ? ? H6' .56808 .76974 .18588 .02700 Uiso ? ? 1.00000 ? ? H7'a .74076 .70761 .26158 .03400 Uiso ? ? 1.00000 ? ? H7'b .86557 .67685 .20283 .03400 Uiso ? ? 1.00000 ? ? 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 Cu .0202(3) .0233(3) .0190(2) -.0007(2) .00049(18) -.0018(2) Cl .0188(5) .0352(6) .0362(6) .0032(5) .0025(4) -.0015(5) O0 .043(2) .057(2) .057(2) .0004(19) -.0120(18) .010(2) C1 .021(2) .023(2) .023(2) .0010(18) .0028(17) -.0011(18) C11 .037(3) .029(2) .029(2) .002(2) .002(2) .003(2) N1 .026(2) .035(2) .025(2) -.0026(18) .0062(16) -.0008(17) O11 .038(2) .041(2) .055(2) -.0105(17) .0122(17) -.0016(17) O12 .038(2) .036(2) .061(2) .0003(16) .0126(17) -.0098(17) C2 .018(2) .027(2) .024(2) .0003(18) .0003(17) -.0007(18) N3 .0143(16) .0232(19) .0214(17) -.0005(14) .0010(13) -.0022(14) C4 .022(2) .027(2) .023(2) -.0060(19) .0009(17) -.0026(18) C5 .034(3) .025(2) .026(2) -.006(2) .004(2) -.0085(19) N6 .024(2) .025(2) .0192(17) .0009(15) .0028(15) -.0002(15) C7 .029(3) .025(2) .029(2) .0033(19) .003(2) .0012(19) C8 .028(3) .026(2) .025(2) .001(2) .0010(19) .0035(18) C81 .028(3) .031(3) .031(2) .001(2) .006(2) .006(2) C82 .049(3) .034(3) .028(2) .008(2) .002(2) .008(2) C2' .025(2) .022(2) .025(2) -.0015(18) .0048(18) -.0015(18) N3' .0147(18) .030(2) .0196(17) .0004(15) .0023(14) -.0033(15) C4' .026(2) .026(2) .022(2) -.0034(18) .0031(18) -.0080(18) C5' .020(2) .036(3) .021(2) -.001(2) -.0027(17) -.005(2) N6' .0191(18) .0250(18) .0208(17) -.0008(15) .0017(14) -.0007(15) C7' .026(2) .028(2) .026(2) .006(2) -.0020(19) .0032(19) P1 .0405(9) .0731(11) .0370(8) .0005(8) .0087(7) .0148(7) F1 .052(2) .061(2) .0408(17) -.0049(15) .0109(14) .0122(15) F2 .061(6) .130(11) .090(10) -.009(7) -.005(5) .080(9) F3 .038(4) .097(6) .050(4) -.016(4) .005(3) -.008(4) F4 .043(5) .121(8) .043(5) .021(5) .009(3) -.014(5) F5 .180(18) .120(13) .087(7) -.123(12) .039(12) -.019(9) F6 .119(13) .088(10) .122(11) .077(8) .004(9) .016(8) F2' .157(11) .100(9) .042(5) -.000(9) .008(5) .036(7) F3' .035(5) .145(12) .079(7) -.035(7) -.005(4) .039(7) F4' .233(17) .091(7) .055(6) .032(10) .028(8) -.032(6) F5' .023(4) .116(11) .084(8) .007(5) .008(4) .063(8) F6' .097(9) .048(5) .186(12) .027(5) .015(8) -.004(6) O01 .074(6) .057(5) .075(6) .020(4) .033(5) .014(4) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Cu Cl . . 2.6928(12) ? Cu O0 . . 2.622(4) ? Cu N3 . . 2.021(3) ? Cu N6 . . 2.019(3) ? Cu N3' . . 2.021(3) ? Cu N6' . . 2.011(3) ? C1 C11 . . 1.536(6) ? C1 N1 . . 1.533(6) ? C1 C2 . . 1.525(6) ? C1 C2' . . 1.532(6) ? C11 H11a . . .957(4) ? C11 H11b . . .954(4) ? C11 H11c . . .965(5) ? N1 O11 . . 1.251(5) ? N1 O12 . . 1.192(5) ? C2 N3 . . 1.480(5) ? C2 H2a . . .956(4) ? C2 H2b . . .960(4) ? N3 C4 . . 1.484(5) ? N3 H3 . . .934(3) ? C4 C5 . . 1.508(6) ? C4 H4a . . .962(4) ? C4 H4b . . .957(4) ? C5 N6 . . 1.496(5) ? C5 H5a . . .961(4) ? C5 H5b . . .957(4) ? N6 C7 . . 1.485(5) ? N6 H6 . . 1.029(3) ? C7 C8 . . 1.533(6) ? C7 H7a . . .958(4) ? C7 H7b . . .960(4) ? C8 C81 . . 1.540(6) ? C8 C82 . . 1.538(6) ? C8 C7' . . 1.525(6) ? C81 H81a . . .963(4) ? C81 H81b . . .951(4) ? C81 H81c . . .955(4) ? C82 H82a . . .949(5) ? C82 H82b . . .960(4) ? C82 H82c . . .962(5) ? C2' N3' . . 1.472(5) ? C2' H2'a . . .966(4) ? C2' H2'b . . .954(4) ? N3' C4' . . 1.493(5) ? N3' H3' . . .918(3) ? C4' C5' . . 1.506(6) ? C4' H4'a . . .956(4) ? C4' H4'b . . .957(4) ? C5' N6' . . 1.482(5) ? C5' H5'a . . .960(4) ? C5' H5'b . . .962(4) ? N6' C7' . . 1.485(5) ? N6' H6' . . .881(3) ? C7' H7'a . . .965(4) ? C7' H7'b . . .960(4) ? P1 F1 . . 1.597(3) ? P1 F2 . . 1.618(13) ? P1 F3 . . 1.725(8) ? P1 F4 . . 1.710(9) ? P1 F5 . . 1.441(16) ? P1 F6 . . 1.461(15) ? P1 F2' . . 1.563(13) ? P1 F3' . . 1.548(9) ? P1 F4' . . 1.415(10) ? P1 F5' . . 1.613(10) ? P1 F6' . . 1.727(10) ? F2 F2' . . .828(17) ? F3 F3' . . 1.463(16) ? F3 F4' . . 1.380(18) ? F4 F4' . . 1.031(16) ? F5 F5' . . .76(2) ? F5 F6' . . 1.47(2) ? F6 F3' . . .936(18) ? F6 F6' . . 1.293(18) ? F2' F4' . . 1.599(15) ? O01 O01 . '3 765' 1.966(11) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published Cl Cu O0 . . . 178.70(10) ? Cl Cu N3 . . . 94.27(9) ? Cl Cu N6 . . . 90.25(10) ? Cl Cu N3' . . . 92.15(9) ? Cl Cu N6' . . . 89.46(10) ? O0 Cu N3 . . . 84.52(12) ? O0 Cu N6 . . . 89.18(12) ? O0 Cu N3' . . . 88.41(12) ? O0 Cu N6' . . . 91.75(12) ? N3 Cu N6 . . . 86.13(13) ? N3 Cu N3' . . . 93.11(13) ? N3 Cu N6' . . . 176.21(13) ? N6 Cu N3' . . . 177.53(14) ? N6 Cu N6' . . . 94.53(13) ? N3' Cu N6' . . . 86.08(13) ? C11 C1 N1 . . . 105.5(3) ? C11 C1 C2 . . . 108.1(3) ? C11 C1 C2' . . . 109.2(3) ? N1 C1 C2 . . . 111.2(3) ? N1 C1 C2' . . . 107.5(3) ? C2 C1 C2' . . . 115.0(3) ? C1 C11 H11a . . . 111.1(4) ? C1 C11 H11b . . . 110.9(4) ? C1 C11 H11c . . . 110.6(4) ? H11a C11 H11b . . . 108.6(4) ? H11a C11 H11c . . . 107.7(4) ? H11b C11 H11c . . . 107.9(4) ? C1 N1 O11 . . . 116.6(3) ? C1 N1 O12 . . . 120.2(4) ? O11 N1 O12 . . . 123.2(4) ? C1 C2 N3 . . . 116.3(3) ? C1 C2 H2a . . . 108.2(4) ? C1 C2 H2b . . . 108.1(4) ? N3 C2 H2a . . . 108.2(4) ? N3 C2 H2b . . . 107.6(4) ? H2a C2 H2b . . . 108.2(4) ? Cu N3 C2 . . . 118.2(2) ? Cu N3 C4 . . . 106.2(2) ? Cu N3 H3 . . . 104.5(2) ? C2 N3 C4 . . . 111.0(3) ? C2 N3 H3 . . . 105.5(3) ? C4 N3 H3 . . . 111.3(3) ? N3 C4 C5 . . . 107.9(3) ? N3 C4 H4a . . . 109.9(4) ? N3 C4 H4b . . . 109.9(4) ? C5 C4 H4a . . . 110.9(4) ? C5 C4 H4b . . . 110.3(4) ? H4a C4 H4b . . . 107.9(4) ? C4 C5 N6 . . . 107.6(3) ? C4 C5 H5a . . . 109.7(4) ? C4 C5 H5b . . . 110.4(4) ? N6 C5 H5a . . . 110.3(4) ? N6 C5 H5b . . . 110.8(4) ? H5a C5 H5b . . . 107.9(4) ? Cu N6 C5 . . . 106.9(2) ? Cu N6 C7 . . . 118.0(2) ? Cu N6 H6 . . . 102.2(2) ? C5 N6 C7 . . . 112.4(3) ? C5 N6 H6 . . . 110.4(3) ? C7 N6 H6 . . . 106.4(3) ? N6 C7 C8 . . . 113.4(3) ? N6 C7 H7a . . . 108.4(4) ? N6 C7 H7b . . . 108.6(3) ? C8 C7 H7a . . . 109.3(4) ? C8 C7 H7b . . . 109.0(4) ? H7a C7 H7b . . . 108.0(4) ? C7 C8 C81 . . . 111.1(3) ? C7 C8 C82 . . . 107.1(3) ? C7 C8 C7' . . . 112.0(4) ? C81 C8 C82 . . . 108.4(4) ? C81 C8 C7' . . . 111.0(3) ? C82 C8 C7' . . . 107.0(3) ? C8 C81 H81a . . . 109.9(4) ? C8 C81 H81b . . . 111.0(4) ? C8 C81 H81c . . . 110.6(4) ? H81a C81 H81b . . . 108.3(4) ? H81a C81 H81c . . . 107.9(4) ? H81b C81 H81c . . . 109.0(4) ? C8 C82 H82a . . . 111.0(4) ? C8 C82 H82b . . . 110.5(4) ? C8 C82 H82c . . . 110.4(4) ? H82a C82 H82b . . . 108.7(5) ? H82a C82 H82c . . . 108.5(5) ? H82b C82 H82c . . . 107.7(4) ? C1 C2' N3' . . . 114.1(3) ? C1 C2' H2'a . . . 109.1(3) ? C1 C2' H2'b . . . 109.4(4) ? N3' C2' H2'a . . . 107.6(4) ? N3' C2' H2'b . . . 108.6(3) ? H2'a C2' H2'b . . . 107.8(4) ? Cu N3' C2' . . . 116.0(2) ? Cu N3' C4' . . . 106.5(2) ? Cu N3' H3' . . . 106.3(3) ? C2' N3' C4' . . . 111.7(3) ? C2' N3' H3' . . . 104.7(3) ? C4' N3' H3' . . . 111.6(3) ? N3' C4' C5' . . . 107.7(3) ? N3' C4' H4'a . . . 110.3(3) ? N3' C4' H4'b . . . 110.5(4) ? C5' C4' H4'a . . . 109.6(4) ? C5' C4' H4'b . . . 110.4(4) ? H4'a C4' H4'b . . . 108.4(4) ? C4' C5' N6' . . . 107.7(3) ? C4' C5' H5'a . . . 110.8(4) ? C4' C5' H5'b . . . 110.0(4) ? N6' C5' H5'a . . . 110.7(4) ? N6' C5' H5'b . . . 110.0(4) ? H5'a C5' H5'b . . . 107.6(4) ? Cu N6' C5' . . . 106.8(2) ? Cu N6' C7' . . . 118.2(2) ? Cu N6' H6' . . . 106.7(2) ? C5' N6' C7' . . . 112.3(3) ? C5' N6' H6' . . . 121.8(3) ? C7' N6' H6' . . . 91.0(3) ? C8 C7' N6' . . . 114.9(3) ? C8 C7' H7'a . . . 108.7(4) ? C8 C7' H7'b . . . 109.1(4) ? N6' C7' H7'a . . . 108.3(4) ? N6' C7' H7'b . . . 108.1(4) ? H7'a C7' H7'b . . . 107.4(4) ? F1 P1 F2 . . . 165.5(5) ? F1 P1 F3 . . . 81.1(3) ? F1 P1 F4 . . . 81.9(3) ? F1 P1 F5 . . . 90.9(6) ? F1 P1 F6 . . . 89.3(5) ? F1 P1 F2' . . . 164.3(4) ? F1 P1 F3' . . . 93.6(5) ? F1 P1 F4' . . . 99.6(4) ? F1 P1 F5' . . . 89.7(5) ? F1 P1 F6' . . . 83.1(4) ? F2 P1 F3 . . . 110.0(5) ? F2 P1 F4 . . . 108.8(5) ? F2 P1 F5 . . . 79.2(7) ? F2 P1 F6 . . . 82.2(7) ? F2 P1 F2' . . . 30.1(6) ? F2 P1 F3' . . . 86.5(6) ? F2 P1 F4' . . . 94.7(6) ? F2 P1 F5' . . . 86.5(7) ? F2 P1 F6' . . . 82.6(6) ? F3 P1 F4 . . . 79.4(4) ? F3 P1 F5 . . . 168.7(7) ? F3 P1 F6 . . . 87.3(6) ? F3 P1 F2' . . . 87.6(6) ? F3 P1 F3' . . . 52.8(6) ? F3 P1 F4' . . . 51.0(7) ? F3 P1 F5' . . . 142.9(6) ? F3 P1 F6' . . . 131.5(5) ? F4 P1 F5 . . . 91.6(7) ? F4 P1 F6 . . . 165.0(6) ? F4 P1 F2' . . . 85.4(6) ? F4 P1 F3' . . . 131.9(6) ? F4 P1 F4' . . . 37.0(7) ? F4 P1 F5' . . . 63.8(6) ? F4 P1 F6' . . . 142.5(5) ? F5 P1 F6 . . . 100.7(9) ? F5 P1 F2' . . . 98.6(8) ? F5 P1 F3' . . . 136.4(8) ? F5 P1 F4' . . . 123.5(9) ? F5 P1 F5' . . . 28.0(8) ? F5 P1 F6' . . . 54.5(8) ? F6 P1 F2' . . . 101.0(7) ? F6 P1 F3' . . . 36.1(7) ? F6 P1 F4' . . . 134.4(8) ? F6 P1 F5' . . . 128.7(7) ? F6 P1 F6' . . . 47.0(7) ? F2' P1 F3' . . . 88.1(8) ? F2' P1 F4' . . . 64.7(6) ? F2' P1 F5' . . . 92.9(8) ? F2' P1 F6' . . . 112.6(6) ? F3' P1 F4' . . . 98.4(8) ? F3' P1 F5' . . . 164.3(7) ? F3' P1 F6' . . . 83.1(6) ? F4' P1 F5' . . . 96.2(8) ? F4' P1 F6' . . . 176.8(7) ? F5' P1 F6' . . . 82.1(6) ? P1 F2 F2' . . . 71.2(12) ? P1 F3 F3' . . . 57.4(5) ? P1 F3 F4' . . . 52.8(5) ? F3' F3 F4' . . . 104.2(8) ? P1 F4 F4' . . . 55.7(7) ? P1 F5 F5' . . . 88.8(16) ? P1 F5 F6' . . . 72.7(9) ? F5' F5 F6' . . . 158(2) ? P1 F6 F3' . . . 77.0(11) ? P1 F6 F6' . . . 77.4(9) ? F3' F6 F6' . . . 154.3(17) ? P1 F2' F2 . . . 78.6(13) ? P1 F2' F4' . . . 53.1(5) ? F2 F2' F4' . . . 131.4(16) ? P1 F3' F3 . . . 69.8(6) ? P1 F3' F6 . . . 66.9(11) ? F3 F3' F6 . . . 132.5(13) ? P1 F4' F3 . . . 76.2(8) ? P1 F4' F4 . . . 87.2(9) ? P1 F4' F2' . . . 62.1(6) ? F3 F4' F4 . . . 130.2(10) ? F3 F4' F2' . . . 99.5(11) ? F4 F4' F2' . . . 113.6(13) ? P1 F5' F5 . . . 63.2(14) ? P1 F6' F5 . . . 52.8(7) ? P1 F6' F6 . . . 55.6(7) ? F5 F6' F6 . . . 107.6(11) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- 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 Cu C1 3.415(4) . . ? Cu N1 4.011(4) . . ? Cu C2 3.017(4) . . ? Cu C4 2.821(4) . . ? Cu C5 2.841(4) . . ? Cu C7 3.016(4) . . ? Cu C8 3.407(4) . . ? Cu C81 3.894(5) . . ? Cu C2' 2.976(4) . . ? Cu C4' 2.833(4) . . ? Cu C5' 2.822(4) . . ? Cu C7' 3.012(4) . . ? Cu F1 4.306(3) . '4 564' ? Cu H2b 3.2142(5) . . ? Cu H3 2.4296(5) . . ? Cu H4a 3.6885(6) . . ? Cu H4b 3.0695(5) . . ? Cu H5a 3.1300(6) . . ? Cu H5b 3.6964(6) . . ? Cu H6 2.4517(5) . . ? Cu H7a 3.1855(6) . . ? Cu H81b 3.3728(6) . . ? Cu H2'a 3.0866(6) . . ? Cu H3' 2.4434(5) . . ? Cu H4'a 3.1038(5) . . ? Cu H4'b 3.6901(6) . . ? Cu H5'a 3.6871(5) . . ? Cu H5'b 3.0857(5) . . ? Cu H6' 2.4165(5) . . ? Cu H7'b 3.2044(5) . . ? Cl O0 3.085(4) . '1 455' ? Cl N1 3.568(4) . '1 455' ? Cl N3 3.485(3) . . ? Cl N6 3.373(3) . . ? Cl N3' 3.427(3) . . ? Cl N3' 3.253(3) . '1 455' ? Cl N6' 3.346(3) . . ? Cl F2' 3.747(13) . . ? Cl H2'a 2.7855(11) . . ? Cl H3' 2.3897(11) . '1 455' ? O0 N3 3.154(4) . . ? O0 N6 3.286(5) . . ? O0 N6 3.411(5) . '1 655' ? O0 N3' 3.266(5) . . ? O0 N6' 3.353(5) . . ? O0 F1 3.050(4) . '4 564' ? O0 O01 2.665(8) . . ? O0 H3 2.649(3) . . ? O0 H6 2.420(3) . '1 655' ? C1 O11 2.374(5) . . ? C1 O12 2.369(5) . . ? C1 N3 2.553(5) . . ? C1 N3' 2.521(5) . . ? C1 H11a 2.082(4) . . ? C1 H11b 2.078(4) . . ? C1 H11c 2.083(4) . . ? C1 H2a 2.037(4) . . ? C1 H2b 2.039(4) . . ? C1 H2'a 2.062(4) . . ? C1 H2'b 2.057(4) . . ? C1 H3' 2.607(4) . . ? C11 N1 2.444(6) . . ? C11 O11 2.811(6) . . ? C11 C2 2.478(6) . . ? C11 C2' 2.501(6) . . ? C11 F2 3.137(14) . '3 675' ? C11 F2' 3.377(13) . '3 675' ? C11 H2a 2.616(4) . . ? C11 H2b 2.623(5) . . ? C11 H2'b 2.627(4) . . ? N1 C2 2.523(5) . . ? N1 N3 3.108(5) . . ? N1 C2' 2.471(6) . . ? N1 N3' 2.964(5) . . ? N1 F1 4.118(5) . '4 564' ? N1 F3 4.134(9) . '4 564' ? N1 F4 4.198(10) . '4 564' ? N1 H11a 2.668(3) . . ? N1 H11b 2.593(4) . . ? N1 H11c 3.299(4) . . ? N1 H2a 2.669(4) . . ? N1 H2b 3.335(4) . . ? N1 H3 2.781(4) . . ? N1 H81c 3.125(3) . '4 564' ? N1 H82b 2.995(4) . '4 564' ? N1 H2'a 3.312(4) . . ? N1 H2'b 2.644(4) . . ? N1 H3' 2.534(3) . . ? O11 O12 2.149(5) . . ? O11 C2' 2.872(6) . . ? O11 N3' 3.441(5) . . ? O11 H11b 2.504(3) . . ? O11 H82b 2.626(4) . '4 564' ? O11 H2'b 2.491(3) . '3 775' ? O11 H2'b 2.600(4) . . ? O12 C2 2.714(5) . . ? O12 N3 2.901(5) . . ? O12 N3' 3.523(5) . . ? O12 P1 3.932(4) . '4 564' ? O12 F1 3.039(4) . '4 564' ? O12 F3 3.205(9) . '4 564' ? O12 F4 3.039(10) . '4 564' ? O12 F4' 3.304(10) . '4 564' ? O12 H2a 2.628(3) . . ? O12 H3 2.267(3) . . ? C2 C4 2.443(6) . . ? C2 C2' 2.579(6) . . ? C2 N3' 3.123(5) . . ? C2 F3 3.501(9) . '4 564' ? C2 H11a 2.630(4) . . ? C2 H3 1.951(4) . . ? C2 H4a 2.683(4) . . ? C2 H4b 2.585(4) . . ? N3 C5 2.419(5) . . ? N3 N6 2.759(5) . . ? N3 C2' 3.118(5) . . ? N3 N3' 2.934(4) . . ? N3 N6' 4.030(4) . . ? N3 P1 4.231(4) . '4 564' ? N3 F1 3.095(4) . '4 564' ? N3 F3 3.305(8) . '4 564' ? N3 F6 4.161(14) . '4 564' ? N3 F3' 3.803(13) . '4 564' ? N3 F4' 4.318(13) . '4 564' ? N3 H2a 1.998(3) . . ? N3 H2b 1.993(3) . . ? N3 H4a 2.025(3) . . ? N3 H4b 2.021(3) . . ? N3 H5a 2.634(3) . . ? N3 H5b 3.258(3) . . ? N3 H6 3.230(3) . . ? N3 H2'a 3.360(3) . . ? N3 H3' 3.068(3) . . ? C4 N6 2.424(5) . . ? C4 F1 3.597(5) . '4 464' ? C4 F1 3.358(5) . '4 564' ? C4 F3 3.286(8) . '4 564' ? C4 F4 3.281(8) . '4 464' ? C4 F6 3.604(15) . '4 564' ? C4 F3' 3.264(12) . '4 564' ? C4 F5' 3.217(13) . '4 464' ? C4 H2a 2.642(4) . . ? C4 H2b 2.554(4) . . ? C4 H3 2.021(4) . . ? C4 H5a 2.043(4) . . ? C4 H5b 2.049(4) . . ? C5 C7 2.477(6) . . ? C5 F1 3.420(5) . '4 564' ? C5 F6 3.571(15) . '4 564' ? C5 F3' 3.621(12) . '4 564' ? C5 F5' 3.567(12) . '4 464' ? C5 H3 2.682(4) . . ? C5 H4a 2.058(4) . . ? C5 H4b 2.047(4) . . ? C5 H6 2.092(4) . . ? C5 H7a 2.649(4) . . ? C5 H7b 2.640(4) . . ? N6 C8 2.523(5) . . ? N6 C81 2.992(6) . . ? N6 N3' 4.039(5) . . ? N6 N6' 2.960(4) . . ? N6 C7' 3.109(5) . . ? N6 F6' 4.205(12) . '2 545' ? N6 O01 3.505(9) . '1 455' ? N6 H3 3.170(3) . . ? N6 H4a 3.272(3) . . ? N6 H4b 2.642(3) . . ? N6 H5a 2.039(3) . . ? N6 H5b 2.043(3) . . ? N6 H7a 2.005(3) . . ? N6 H7b 2.009(3) . . ? N6 H81a 3.198(3) . . ? N6 H81b 2.732(3) . . ? N6 H6' 3.043(3) . . ? N6 H7'b 3.369(3) . . ? C7 C81 2.535(6) . . ? C7 C82 2.470(6) . . ? C7 N6' 3.122(5) . . ? C7 C7' 2.535(6) . . ? C7 F5 3.397(16) . '2 645' ? C7 F6 3.502(15) . '2 545' ? C7 F5' 3.590(14) . '2 645' ? C7 H5a 2.620(4) . . ? C7 H6 2.032(4) . . ? C7 H81a 2.685(4) . . ? C7 H82a 2.653(4) . . ? C7 H82c 2.658(4) . . ? C7 H7'b 2.679(4) . . ? C8 N6' 2.537(5) . . ? C8 H6 2.677(4) . . ? C8 H7a 2.059(4) . . ? C8 H7b 2.056(4) . . ? C8 H81a 2.076(4) . . ? C8 H81b 2.080(4) . . ? C8 H81c 2.078(4) . . ? C8 H82a 2.076(4) . . ? C8 H82b 2.078(4) . . ? C8 H82c 2.079(4) . . ? C8 H6' 2.433(4) . . ? C8 H7'a 2.050(4) . . ? C8 H7'b 2.051(4) . . ? C81 C82 2.497(6) . . ? C81 N6' 3.021(6) . . ? C81 C7' 2.527(6) . . ? C81 F3 3.648(10) . . ? C81 F4' 3.448(11) . . ? C81 H6 2.567(4) . . ? C81 H82a 2.690(4) . . ? C81 H82b 2.686(4) . . ? C81 H6' 2.451(4) . . ? C82 C7' 2.462(6) . . ? C82 F2 3.517(13) . '2 645' ? C82 F5 3.371(17) . '2 645' ? C82 F6 3.586(14) . '2 545' ? C82 F3' 3.655(13) . '2 545' ? C82 F5' 3.369(14) . '2 645' ? C82 H7a 2.665(5) . . ? C82 H7b 2.587(4) . . ? C82 H81c 2.654(5) . . ? C82 H7'a 2.580(5) . . ? C82 H7'b 2.643(5) . . ? C2' C4' 2.454(6) . . ? C2' H11b 2.692(4) . . ? C2' H11c 2.697(4) . . ? C2' H3' 1.923(4) . . ? C2' H4'a 2.583(4) . . ? N3' C5' 2.422(5) . . ? N3' N6' 2.752(5) . . ? N3' H3 3.106(3) . . ? N3' H2'a 1.990(3) . . ? N3' H2'b 1.993(3) . . ? N3' H4'a 2.033(3) . . ? N3' H4'b 2.036(3) . . ? N3' H5'a 3.266(3) . . ? N3' H5'b 2.638(3) . . ? N3' H6' 3.287(3) . . ? C4' N6' 2.413(5) . . ? C4' F2' 3.537(17) . . ? C4' H2'a 2.632(4) . . ? C4' H2'b 2.592(4) . . ? C4' H3' 2.020(4) . . ? C4' H5'a 2.053(4) . . ? C4' H5'b 2.046(4) . . ? C5' C7' 2.464(6) . . ? C5' F3 3.336(8) . '1 655' ? C5' F4 3.148(9) . . ? C5' F2' 3.584(17) . . ? C5' F3' 3.481(11) . '1 655' ? C5' F4' 3.472(16) . . ? C5' H4'a 2.036(4) . . ? C5' H4'b 2.047(4) . . ? C5' H6' 2.085(4) . . ? C5' H7'a 2.640(4) . . ? C5' H7'b 2.614(4) . . ? N6' P1 4.352(4) . . ? N6' F2 4.305(13) . . ? N6' F3 4.275(8) . . ? N6' F4 3.101(9) . . ? N6' F2' 3.585(14) . . ? N6' F4' 3.144(13) . . ? N6' F5' 4.252(14) . . ? N6' H6 3.175(3) . . ? N6' H7a 3.355(3) . . ? N6' H81b 2.716(3) . . ? N6' H81c 3.317(3) . . ? N6' H3' 3.210(3) . . ? N6' H4'a 2.623(3) . . ? N6' H4'b 3.251(3) . . ? N6' H5'a 2.030(3) . . ? N6' H5'b 2.024(3) . . ? N6' H7'a 2.009(3) . . ? N6' H7'b 2.003(3) . . ? C7' F4 3.268(10) . . ? C7' F4' 3.522(14) . . ? C7' H7a 2.672(4) . . ? C7' H82b 2.643(4) . . ? C7' H82c 2.641(4) . . ? C7' H5'b 2.617(4) . . ? C7' H6' 1.739(4) . . ? P1 O01 3.928(8) . '4 465' ? P1 O01 3.685(8) . '2 655' ? P1 H3 3.5302(16) . '4 465' ? P1 H4a 3.5537(16) . '4 465' ? P1 H5a 3.7071(15) . '4 465' ? P1 H82c 3.5876(16) . '2 655' ? P1 H5'a 3.6615(16) . . ? F1 F2 3.189(14) . . ? F1 F3 2.162(7) . . ? F1 F4 2.168(9) . . ? F1 F5 2.169(16) . . ? F1 F6 2.152(14) . . ? F1 F2' 3.130(14) . . ? F1 F3' 2.292(10) . . ? F1 F4' 2.303(10) . . ? F1 F5' 2.265(13) . . ? F1 F6' 2.206(10) . . ? F1 O01 3.375(8) . '2 655' ? F1 O01 2.896(8) . '4 465' ? F1 H3 2.278(3) . '4 465' ? F1 H4a 3.094(3) . '4 465' ? F1 H4b 2.911(3) . '4 565' ? F1 H5a 2.690(3) . '4 465' ? F2 F3 2.740(15) . . ? F2 F4 2.706(15) . . ? F2 F5 1.95(2) . . ? F2 F6 2.03(2) . . ? F2 F3' 2.170(17) . . ? F2 F4' 2.235(16) . . ? F2 F5' 2.214(17) . . ? F2 F6' 2.209(19) . . ? F2 H11a 2.575(13) . '3 675' ? F2 H11b 3.000(13) . '3 675' ? F2 H11c 3.302(14) . '3 675' ? F2 H81a 3.095(12) . 2 ? F2 H82a 3.212(12) . 2 ? F2 H82c 2.592(12) . '2 655' ? F2 H4'a 3.097(14) . . ? F3 F4 2.193(10) . . ? F3 F5 3.151(18) . . ? F3 F6 2.207(16) . . ? F3 F2' 2.278(16) . . ? F3 F5' 3.166(13) . . ? F3 F5' 4.321(13) . '1 455' ? F3 F6' 3.147(13) . . ? F3 H2a 2.826(9) . '4 465' ? F3 H3 2.817(7) . '4 465' ? F3 H4a 2.554(7) . '4 465' ? F3 H81c 3.012(9) . . ? F3 H5'a 2.866(7) . '1 455' ? F3 H5'b 2.888(6) . '1 455' ? F4 F5 2.267(19) . . ? F4 F6 3.143(17) . . ? F4 F2' 2.222(16) . . ? F4 F3' 4.169(12) . '1 655' ? F4 F3' 2.976(13) . . ? F4 F5' 1.758(17) . . ? F4 F6' 3.254(14) . . ? F4 H4a 2.804(7) . '4 565' ? F4 H4b 2.856(7) . '4 565' ? F4 H81c 3.241(10) . . ? F4 H5'a 2.461(8) . . ? F4 H6' 2.650(8) . . ? F4 H7'a 2.611(10) . . ? F5 F6 2.23(2) . . ? F5 F2' 2.28(2) . . ? F5 F3' 4.118(19) . '1 655' ? F5 F3' 2.776(18) . . ? F5 F4' 2.515(19) . . ? F5 O01 3.054(18) . '2 655' ? F5 O01 3.374(17) . '4 465' ? F5 H4a 3.330(16) . '4 565' ? F5 H5b 3.184(15) . '4 565' ? F5 H7a 2.714(16) . '2 655' ? F5 H7b 3.295(16) . '2 655' ? F5 H82a 3.350(16) . '2 655' ? F5 H82c 2.644(16) . '2 655' ? F6 F2' 2.33(2) . . ? F6 F4' 2.651(19) . . ? F6 F5' 3.884(18) . '1 455' ? F6 F5' 2.772(18) . . ? F6 O01 3.094(15) . '2 655' ? F6 H4a 2.943(14) . '4 465' ? F6 H5a 2.974(13) . '4 465' ? F6 H7b 2.598(14) . 2 ? F6 H81a 3.073(14) . 2 ? F6 H82a 2.738(13) . 2 ? F2' F3' 2.16(2) . . ? F2' F5' 2.302(18) . . ? F2' F6' 2.739(18) . . ? F2' H11a 3.024(12) . '3 675' ? F2' H11b 3.058(13) . '3 675' ? F2' H82c 3.104(14) . '2 655' ? F2' H4'a 2.764(16) . . ? F2' H5'a 3.201(16) . . ? F2' H6' 3.024(13) . . ? F3' F4' 2.245(18) . . ? F3' F5' 3.526(14) . '1 455' ? F3' F5' 3.132(13) . . ? F3' F6' 2.175(16) . . ? F3' H4a 2.455(12) . '4 465' ? F3' H5a 3.208(11) . '4 465' ? F3' H7b 3.132(13) . 2 ? F3' H82a 2.737(12) . 2 ? F3' H5'a 2.816(10) . '1 455' ? F3' H5'b 3.344(11) . '1 455' ? F4' F5' 2.257(17) . . ? F4' F6' 3.140(15) . . ? F4' H81b 3.154(10) . . ? F4' H81c 2.946(11) . . ? F4' H5'a 2.986(16) . . ? F4' H6' 2.470(11) . . ? F4' H7'a 3.060(14) . . ? F5' F6' 2.194(17) . . ? F5' H4a 2.688(11) . '4 565' ? F5' H4b 3.101(13) . '4 565' ? F5' H5b 3.023(12) . '4 565' ? F5' H7a 3.069(14) . '2 655' ? F5' H7b 3.294(12) . '2 655' ? F5' H82a 3.144(13) . '2 655' ? F5' H82c 2.758(14) . '2 655' ? F5' H5'a 2.852(13) . . ? F6' O01 3.031(15) . '4 465' ? F6' O01 2.103(14) . '2 655' ? F6' H5a 3.251(13) . '4 465' ? F6' H7a 3.065(11) . '2 655' ? F6' H7b 2.882(12) . 2 ? F6' H81a 2.840(10) . 2 ? O01 H5b 2.546(8) . '1 655' ? H11a H11b 1.55141(11) . . ? H11a H11c 1.55139(11) . . ? H11b H11c 1.55131(17) . . ? H2a H2b 1.55131(11) . . ? H2a H3 2.20417(15) . . ? H2b H4b 2.3265(2) . . ? H3 H4a 2.28460(18) . . ? H4a H4b 1.55132(11) . . ? H4a H5a 2.33615(16) . . ? H4a H5b 2.37581(18) . . ? H4b H5b 2.3361(2) . . ? H5a H5b 1.55134(18) . . ? H5b H6 2.33315(18) . . ? H6 H7b 2.3095(2) . . ? H6 H81b 2.1198(2) . . ? H7a H7b 1.55132(17) . . ? H81a H81b 1.55149(16) . . ? H81a H81c 1.55128(11) . . ? H81b H81c 1.55140(15) . . ? H81b H6' 2.02964(18) . . ? H82a H82b 1.55143(11) . . ? H82a H82c 1.55145(17) . . ? H82b H82c 1.55138(11) . . ? H82b H7'a 2.3946(2) . . ? H2'a H2'b 1.55134(16) . . ? H2'b H3' 2.2351(2) . . ? H3' H4'b 2.27068(18) . . ? H4'a H4'b 1.55136(18) . . ? H4'a H5'a 2.33060(16) . . ? H4'b H5'a 2.36952(18) . . ? H4'b H5'b 2.3314(2) . . ? H5'a H5'b 1.55135(11) . . ? H5'a H6' 2.35836(19) . . ? H6' H7'a 2.04952(14) . . ? H7'a H7'b 1.55130(11) . . ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1152 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 8 _reflns_limit_k_min 0 _reflns_limit_k_max 24 _reflns_limit_l_min -25 _reflns_limit_l_max 25 _reflns_number_observed ? _reflns_d_resolution_high .727 _reflns_d_resolution_low 12.799 _diffrn_reflns_av_sigmaI/netI .125 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 153 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .092 _refine_ls_wR_factor_all .062 _refine_ls_goodness_of_fit_all 1.183 _refine_ls_shift/su_mean .003 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_global _audit_creation_method Xtal3.6 _audit_creation_date 00-09-15 _audit_update_record ? #============================================================================== # (Publishing Staff Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia Nedlands Western Australia 6907 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal ? _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Skelton, Brian W.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Pogram for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_yk24 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C13 H31 Cu1 N7 O9' _chemical_formula_moiety ? _chemical_formula_weight 492.98 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C_1_2/c_1 _symmetry_space_group_name_Hall -c_2yc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,+y,1/2-z -x,-y,-z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 19.018(3) _cell_length_b 9.015(2) _cell_length_c 12.256(2) _cell_angle_alpha 90.00000 _cell_angle_beta 97.504(2) _cell_angle_gamma 90.00000 _cell_volume 2083.3(7) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 5169 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 24.4 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu 1.11 _exptl_crystal_description plate _exptl_crystal_size_max .45 _exptl_crystal_size_mid .4 _exptl_crystal_size_min .05 _exptl_crystal_size_rad ? _exptl_crystal_colour pink _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .604 _exptl_absorpt_correction_T_max .862 _diffrn_reflns_number 9784 _reflns_number_total 2559 _reflns_Friedel_coverage 0 _reflns_number_gt 2227 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 28.85 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .029 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .032 _refine_ls_wR_factor_ref .042 _refine_ls_goodness_of_fit_ref 1.352 _refine_ls_number_reflns 2227 _refine_ls_number_parameters 203 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment mixed _refine_ls_shift/su_max .011 _refine_diff_density_min -.649 _refine_diff_density_max .505 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ 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 52 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 124 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cu ? 0 4 .263 1.266 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 28 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 36 .008 .006 '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_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu .25000 .75000 .00000 .01966(16) Uani ? ? 1.00000 ? ? C1 .08551(10) .7326(2) .08270(15) .0251(9) Uani ? ? 1.00000 ? ? C11 .00466(12) .7131(3) .0640(2) .0346(11) Uani ? ? 1.00000 ? ? N12 .10600(11) .7612(2) .20575(15) .0328(10) Uani ? ? .50000 ? ? C12 .10600(11) .7612(2) .20575(15) .0328(10) Uani ? ? .50000 ? ? O11 .1297(2) .6704(5) .2632(3) .055(2) Uani ? ? .50000 ? ? O12 .0838(2) .8861(4) .2364(3) .052(2) Uani ? ? .50000 ? ? C2 .10376(10) .8685(2) .01734(15) .0249(9) Uani ? ? 1.00000 ? ? N3 .18025(8) .90753(16) .03293(13) .0213(7) Uani ? ? 1.00000 ? ? C4 .19423(11) 1.0387(2) -.03425(15) .0245(9) Uani ? ? 1.00000 ? ? C5 .27354(11) 1.0551(2) -.02865(16) .0263(9) Uani ? ? 1.00000 ? ? N6 .30275(8) .91337(16) -.06556(13) .0214(7) Uani ? ? 1.00000 ? ? C7 .38119(10) .9107(2) -.04777(16) .0254(9) Uani ? ? 1.00000 ? ? N .16717(9) .7887(2) -.26214(12) .0258(8) Uani ? ? 1.00000 ? ? O1 .17836(9) .69858(18) -.18510(12) .0373(8) Uani ? ? 1.00000 ? ? O2 .21468(7) .88008(16) -.28016(11) .0308(7) Uani ? ? 1.00000 ? ? O3 .10997(9) .7868(2) -.32349(15) .0493(10) Uani ? ? 1.00000 ? ? O01 .00000 .5947(3) -.25000 .069(2) Uani ? ? 1.00000 ? ? H3 .1886(12) .931(3) .103(2) .033(6) Uiso ? ? 1.00000 ? ? H6 .2901(13) .911(3) -.134(2) .034(6) Uiso ? ? 1.00000 ? ? H11a -.0098(12) .625(3) .102(2) .035(6) Uiso ? ? 1.00000 ? ? H11b -.0104(16) .691(3) -.003(3) .055(8) Uiso ? ? 1.00000 ? ? H11c -.0166(12) .800(3) .0829(18) .026(5) Uiso ? ? 1.00000 ? ? H12a .15597 .77389 .22130 .05000 Uiso ? ? .50000 ? ? H12b .09204 .67888 .24660 .05000 Uiso ? ? .50000 ? ? H12c .08291 .84813 .22669 .05000 Uiso ? ? .50000 ? ? H2a .0752(11) .950(2) .0399(16) .021(5) Uiso ? ? 1.00000 ? ? H2b .0890(11) .845(2) -.0603(17) .022(5) Uiso ? ? 1.00000 ? ? H4a .1740(10) 1.122(2) -.0033(16) .018(5) Uiso ? ? 1.00000 ? ? H4b .1720(12) 1.022(2) -.110(2) .028(6) Uiso ? ? 1.00000 ? ? H5a .2975(12) 1.069(2) .0486(18) .026(5) Uiso ? ? 1.00000 ? ? H5b .2862(12) 1.133(3) -.0723(19) .036(6) Uiso ? ? 1.00000 ? ? H7a .3940(12) .927(3) .029(2) .033(6) Uiso ? ? 1.00000 ? ? H7b .3979(11) .989(2) -.0863(17) .025(5) Uiso ? ? 1.00000 ? ? H01a .0288(17) .646(4) -.265(3) .072(11) Uiso ? ? 1.00000 ? ? 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 Cu .02181(17) .01527(16) .02155(17) -.00357(11) .00153(11) .00176(11) C1 .0246(9) .0301(10) .0206(9) -.0062(7) .0033(7) -.0020(7) C11 .0260(11) .0445(13) .0331(12) -.0056(9) .0029(8) -.0024(10) N12 .0350(10) .0430(12) .0212(9) -.0112(8) .0069(7) -.0033(8) C12 .0350(10) .0430(12) .0212(9) -.0112(8) .0069(7) -.0033(8) O11 .051(2) .088(3) .0248(16) .029(2) .0042(14) .0076(17) O12 .082(3) .042(2) .0327(17) -.0170(18) .0089(17) -.0090(15) C2 .0248(9) .0263(9) .0229(9) .0007(7) .0002(7) .0010(7) N3 .0255(8) .0187(7) .0194(7) -.0026(6) .0014(6) .0007(6) C4 .0334(10) .0183(9) .0220(9) -.0001(7) .0038(8) .0013(7) C5 .0374(11) .0162(8) .0256(9) -.0059(8) .0058(8) .0011(7) N6 .0266(8) .0180(7) .0192(7) -.0055(6) .0015(6) .0004(6) C7 .0270(10) .0240(9) .0244(9) -.0091(7) .0007(7) .0005(7) N .0292(9) .0307(8) .0173(7) .0007(7) .0023(6) -.0039(6) O1 .0474(9) .0333(8) .0282(8) -.0118(7) -.0069(6) .0079(6) O2 .0329(8) .0363(8) .0224(7) -.0064(6) .0005(5) .0047(6) O3 .0310(9) .0669(11) .0454(10) -.0089(8) -.0117(7) .0179(8) O01 .057(2) .0419(16) .118(3) .00000 .043(2) .00000 # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Cu N3 . . 2.0196(16) ? Cu N6 . . 2.0079(16) ? Cu O1 . . 2.5318(15) ? Cu N3 . '7 565' 2.0196(16) ? Cu N6 . '7 565' 2.0079(16) ? Cu O1 . '7 565' 2.5318(15) ? C1 C11 . . 1.535(3) ? C1 N12 . . 1.529(3) ? C1 C12 . . 1.529(3) ? C1 C2 . . 1.528(3) ? C1 C7 . '7 565' 1.524(3) ? C11 H11a . . .98(2) ? C11 H11b . . .85(3) ? C11 H11c . . .92(2) ? N12 O11 . . 1.134(4) ? N12 O12 . . 1.276(4) ? N12 H12a . . .951(2) ? N12 H12b . . .952(2) ? N12 H12c . . .950(2) ? C12 O11 . . 1.134(4) ? C12 O12 . . 1.276(4) ? C12 H12a . . .951(2) ? C12 H12b . . .952(2) ? C12 H12c . . .950(2) ? O11 H12a . . 1.205(4) ? O11 H12b . . .722(4) ? O12 H12c . . .362(3) ? C2 N3 . . 1.485(2) ? C2 H2a . . .97(2) ? C2 H2b . . .98(2) ? N3 C4 . . 1.485(2) ? N3 H3 . . .88(2) ? C4 C5 . . 1.508(3) ? C4 H4a . . .95(2) ? C4 H4b . . .98(2) ? C5 N6 . . 1.487(2) ? C5 H5a . . 1.00(2) ? C5 H5b . . .93(2) ? N6 C7 . . 1.479(3) ? N6 H6 . . .84(2) ? C7 H7a . . .95(2) ? C7 H7b . . .93(2) ? N O1 . . 1.243(2) ? N O2 . . 1.263(2) ? N O3 . . 1.239(2) ? O01 H01a . . .76(3) ? O01 H01a . '2 554' .76(3) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published N3 Cu N6 . . . 86.54(6) ? N3 Cu O1 . . . 90.98(6) ? N3 Cu N3 . . '7 565' 180.0000 ? N3 Cu N6 . . '7 565' 93.46(6) ? N3 Cu O1 . . '7 565' 89.02(6) ? N6 Cu O1 . . . 90.82(6) ? N6 Cu N3 . . '7 565' 93.46(7) ? N6 Cu N6 . . '7 565' 180.0000 ? N6 Cu O1 . . '7 565' 89.18(6) ? O1 Cu N3 . . '7 565' 89.02(6) ? O1 Cu N6 . . '7 565' 89.18(6) ? O1 Cu O1 . . '7 565' 180.0000 ? N3 Cu N6 '7 565' . '7 565' 86.54(6) ? N3 Cu O1 '7 565' . '7 565' 90.98(6) ? N6 Cu O1 '7 565' . '7 565' 90.82(6) ? C11 C1 N12 . . . 106.72(18) ? C11 C1 C12 . . . 106.72(18) ? C11 C1 C2 . . . 107.78(16) ? C11 C1 C7 . . '7 565' 107.80(16) ? N12 C1 C12 . . . .00(18) ? N12 C1 C2 . . . 109.63(15) ? N12 C1 C7 . . '7 565' 110.97(15) ? C12 C1 C2 . . . 109.63(15) ? C12 C1 C7 . . '7 565' 110.97(15) ? C2 C1 C7 . . '7 565' 113.64(17) ? C1 C11 H11a . . . 111.2(13) ? C1 C11 H11b . . . 112(2) ? C1 C11 H11c . . . 109.1(14) ? H11a C11 H11b . . . 101(2) ? H11a C11 H11c . . . 114(2) ? H11b C11 H11c . . . 109(2) ? C1 N12 O11 . . . 121.3(3) ? C1 N12 O12 . . . 112.8(2) ? C1 N12 H12a . . . 109.69(18) ? C1 N12 H12b . . . 109.55(17) ? C1 N12 H12c . . . 109.77(17) ? O11 N12 O12 . . . 125.0(3) ? O11 N12 H12a . . . 70.0(2) ? O11 N12 H12b . . . 39.3(2) ? O11 N12 H12c . . . 126.0(3) ? O12 N12 H12a . . . 101.2(2) ? O12 N12 H12b . . . 114.0(3) ? O12 N12 H12c . . . 8.19(19) ? H12a N12 H12b . . . 109.15(19) ? H12a N12 H12c . . . 109.38(19) ? H12b N12 H12c . . . 109.3(2) ? C1 C12 O11 . . . 121.3(3) ? C1 C12 O12 . . . 112.8(2) ? C1 C12 H12a . . . 109.69(18) ? C1 C12 H12b . . . 109.55(17) ? C1 C12 H12c . . . 109.77(17) ? O11 C12 O12 . . . 125.0(3) ? O11 C12 H12a . . . 70.0(2) ? O11 C12 H12b . . . 39.3(2) ? O11 C12 H12c . . . 126.0(3) ? O12 C12 H12a . . . 101.2(2) ? O12 C12 H12b . . . 114.0(3) ? O12 C12 H12c . . . 8.19(19) ? H12a C12 H12b . . . 109.15(19) ? H12a C12 H12c . . . 109.38(19) ? H12b C12 H12c . . . 109.3(2) ? N12 O11 C12 . . . .00(13) ? N12 O11 H12a . . . 47.9(2) ? N12 O11 H12b . . . 56.6(3) ? C12 O11 H12a . . . 47.9(2) ? C12 O11 H12b . . . 56.6(3) ? H12a O11 H12b . . . 104.4(4) ? N12 O12 C12 . . . .00(12) ? N12 O12 H12c . . . 22.0(5) ? C12 O12 H12c . . . 22.0(5) ? C1 C2 N3 . . . 114.09(15) ? C1 C2 H2a . . . 106.3(13) ? C1 C2 H2b . . . 106.3(13) ? N3 C2 H2a . . . 111.0(12) ? N3 C2 H2b . . . 109.2(13) ? H2a C2 H2b . . . 109.8(17) ? Cu N3 C2 . . . 117.77(11) ? Cu N3 C4 . . . 106.23(12) ? Cu N3 H3 . . . 108.9(15) ? C2 N3 C4 . . . 111.14(14) ? C2 N3 H3 . . . 103.4(16) ? C4 N3 H3 . . . 109.2(16) ? N3 C4 C5 . . . 107.64(15) ? N3 C4 H4a . . . 107.4(13) ? N3 C4 H4b . . . 108.5(13) ? C5 C4 H4a . . . 111.1(12) ? C5 C4 H4b . . . 111.4(14) ? H4a C4 H4b . . . 110.6(17) ? C4 C5 N6 . . . 108.26(15) ? C4 C5 H5a . . . 112.5(13) ? C4 C5 H5b . . . 112.3(14) ? N6 C5 H5a . . . 104.6(13) ? N6 C5 H5b . . . 109.6(15) ? H5a C5 H5b . . . 109.3(19) ? Cu N6 C5 . . . 106.40(12) ? Cu N6 C7 . . . 118.41(11) ? Cu N6 H6 . . . 106.8(17) ? C5 N6 C7 . . . 112.27(14) ? C5 N6 H6 . . . 104.7(16) ? C7 N6 H6 . . . 107.3(17) ? N6 C7 H7a . . . 105.5(14) ? N6 C7 H7b . . . 108.5(13) ? N6 C7 C1 . . '7 565' 114.86(15) ? H7a C7 H7b . . . 109(2) ? H7a C7 C1 . . '7 565' 110.3(14) ? H7b C7 C1 . . '7 565' 108.8(14) ? O1 N O2 . . . 120.24(15) ? O1 N O3 . . . 120.13(18) ? O2 N O3 . . . 119.60(17) ? Cu O1 N . . . 125.44(12) ? H01a O01 H01a . . '2 554' 105(4) ? N12 H12a C12 . . . .00000 ? N12 H12a O11 . . . 62.2(2) ? C12 H12a O11 . . . 62.2(2) ? N12 H12b C12 . . . .00000 ? N12 H12b O11 . . . 84.1(4) ? C12 H12b O11 . . . 84.1(4) ? N12 H12c C12 . . . .00000 ? N12 H12c O12 . . . 149.8(7) ? C12 H12c O12 . . . 149.8(7) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- 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 Cu C1 3.415(2) . . ? Cu C1 3.415(2) . '7 565' ? Cu N12 3.959(2) . . ? Cu N12 3.959(2) . '7 565' ? Cu C12 3.959(2) . . ? Cu C12 3.959(2) . '7 565' ? Cu C2 3.013(2) . '7 565' ? Cu C2 3.013(2) . . ? Cu C4 2.821(2) . . ? Cu C4 2.821(2) . '7 565' ? Cu C5 2.816(2) . '7 565' ? Cu C5 2.816(2) . . ? Cu C7 3.008(2) . . ? Cu C7 3.008(2) . '7 565' ? Cu N 3.4063(15) . . ? Cu N 3.4063(15) . '7 565' ? Cu O2 3.6074(14) . '7 565' ? Cu O2 3.6074(14) . . ? Cu H3 2.45(2) . '7 565' ? Cu H3 2.45(2) . . ? Cu H6 2.39(3) . . ? Cu H6 2.39(3) . '7 565' ? Cu H12a 3.4449(4) . . ? Cu H12a 3.4449(4) . '7 565' ? Cu H2b 3.17(2) . '7 565' ? Cu H2b 3.17(2) . . ? Cu H4a 3.65(2) . '7 565' ? Cu H4a 3.65(2) . . ? Cu H4b 3.08(2) . '7 565' ? Cu H4b 3.08(2) . . ? Cu H5a 3.05(2) . '7 565' ? Cu H5a 3.05(2) . . ? Cu H5b 3.65(2) . '7 565' ? Cu H5b 3.65(2) . . ? Cu H7a 3.15(2) . . ? Cu H7a 3.15(2) . '7 565' ? C1 O11 2.330(4) . . ? C1 O12 2.341(4) . . ? C1 N3 2.528(3) . . ? C1 N6 2.532(3) . '7 565' ? C1 H3 2.64(2) . . ? C1 H6 2.70(2) . '7 565' ? C1 H11a 2.10(2) . . ? C1 H11b 2.01(3) . . ? C1 H11c 2.03(2) . . ? C1 H12a 2.0554(18) . . ? C1 H12b 2.054(2) . . ? C1 H12c 2.055(2) . . ? C1 H2a 2.03(2) . . ? C1 H2b 2.03(2) . . ? C1 H7a 2.06(2) . '7 565' ? C1 H7b 2.03(2) . '7 565' ? C11 N12 2.459(3) . . ? C11 C12 2.459(3) . . ? C11 O12 2.887(4) . . ? C11 C2 2.475(3) . . ? C11 C7 2.472(3) . '7 565' ? C11 H12b 2.625(2) . . ? C11 H12c 2.626(2) . . ? C11 H2a 2.56(2) . . ? C11 H2b 2.64(2) . . ? C11 H7a 2.68(2) . '7 565' ? C11 H7b 2.59(2) . '7 565' ? N12 N12 4.310(3) . 2 ? N12 C2 2.499(3) . . ? N12 N3 3.000(3) . . ? N12 N6 3.036(3) . '7 565' ? N12 C7 2.516(3) . '7 565' ? N12 N 4.302(3) . '7 565' ? N12 N 4.225(3) . '4 575' ? N12 O2 3.643(3) . '7 565' ? N12 H3 2.63(2) . . ? N12 H6 2.75(2) . '7 565' ? N12 H11a 2.69(2) . . ? N12 H11b 3.21(3) . . ? N12 H11c 2.63(2) . . ? N12 H11c 3.30(2) . 2 ? N12 H2a 2.66(2) . . ? N12 H2b 3.32(2) . . ? N12 H4b 3.12(2) . '4 575' ? N12 H7a 3.34(2) . '7 565' ? N12 H7b 2.69(2) . '7 565' ? C12 C2 2.499(3) . . ? C12 N3 3.000(3) . . ? C12 N6 3.036(3) . '7 565' ? C12 C7 2.516(3) . '7 565' ? C12 H3 2.63(2) . . ? C12 H11a 2.69(2) . . ? C12 H11c 2.63(2) . . ? C12 H2a 2.66(2) . . ? C12 H7b 2.69(2) . '7 565' ? O11 O12 2.139(6) . . ? O11 N6 2.984(4) . '7 565' ? O11 C7 2.721(4) . '7 565' ? O11 O2 2.975(4) . '7 565' ? O11 H6 2.45(3) . '7 565' ? O11 H12c 1.859(4) . . ? O11 H5a 2.69(2) . '6 545' ? O11 H7b 2.60(2) . '7 565' ? O12 C2 2.765(4) . . ? O12 N3 3.289(4) . . ? O12 N 3.332(4) . '4 575' ? O12 H11c 2.62(2) . . ? O12 H12a 1.734(4) . . ? O12 H12b 1.877(4) . . ? O12 H2a 2.46(2) . . ? O12 H4b 2.49(2) . '4 575' ? C2 C4 2.449(3) . . ? C2 N6 3.114(2) . '7 565' ? C2 C7 2.555(3) . '7 565' ? C2 H3 1.89(2) . . ? C2 H11b 2.68(3) . . ? C2 H11c 2.60(2) . . ? C2 H12c 2.653(2) . . ? C2 H4a 2.68(2) . . ? C2 H4b 2.56(2) . . ? N3 N3 4.039(2) . '7 565' ? N3 C5 2.416(3) . . ? N3 N6 2.761(2) . . ? N3 N6 2.933(2) . '7 565' ? N3 C7 3.112(2) . '7 565' ? N3 N 3.746(2) . '4 575' ? N3 N 4.161(2) . '7 565' ? N3 N 3.749(2) . . ? N3 O1 3.211(2) . '7 565' ? N3 O1 3.266(2) . . ? N3 O2 2.992(2) . '4 575' ? N3 O3 3.618(3) . '4 575' ? N3 H6 3.15(2) . '7 565' ? N3 H6 3.11(3) . . ? N3 H12a 2.6969(16) . . ? N3 H12c 3.2406(17) . . ? N3 H2a 2.05(2) . . ? N3 H2b 2.03(2) . . ? N3 H4a 1.99(2) . . ? N3 H4b 2.02(2) . . ? N3 H5a 2.65(2) . . ? N3 H5b 3.24(2) . . ? N3 H7a 3.37(2) . '7 565' ? C4 N6 2.427(3) . . ? C4 N 3.574(2) . . ? C4 H3 1.96(2) . . ? C4 H6 2.59(3) . . ? C4 H2a 2.67(2) . . ? C4 H2b 2.64(2) . . ? C4 H5a 2.11(2) . . ? C4 H5b 2.05(2) . . ? C5 C7 2.463(3) . . ? C5 N 3.611(3) . '6 554' ? C5 H3 2.67(3) . . ? C5 H6 1.88(3) . . ? C5 H4a 2.05(2) . . ? C5 H4b 2.07(2) . . ? C5 H7a 2.58(2) . . ? C5 H7b 2.62(2) . . ? N6 N6 4.016(2) . '7 565' ? N6 N 3.478(2) . . ? N6 N 4.379(2) . '7 565' ? N6 N 4.068(2) . '6 554' ? N6 O1 3.254(2) . . ? N6 O1 3.209(2) . '7 565' ? N6 O2 2.943(2) . . ? N6 H3 3.19(3) . . ? N6 H3 3.14(2) . '7 565' ? N6 H12a 2.7388(16) . '7 565' ? N6 H12b 3.2829(17) . '7 565' ? N6 H2b 3.35(2) . '7 565' ? N6 H4a 3.26(2) . . ? N6 H4b 2.66(2) . . ? N6 H5a 1.99(2) . . ? N6 H5b 2.00(2) . . ? N6 H7a 1.96(2) . . ? N6 H7b 1.98(2) . . ? C7 H6 1.91(2) . . ? C7 H11a 2.64(2) . '7 565' ? C7 H11b 2.62(3) . '7 565' ? C7 H12b 2.678(2) . '7 565' ? C7 H2b 2.68(2) . '7 565' ? C7 H5a 2.54(2) . . ? C7 H5b 2.69(2) . . ? N O01 3.649(2) . . ? N H3 3.08(2) . '4 574' ? N H6 2.86(2) . . ? N H12a 3.3826(17) . '7 565' ? N H2b 3.09(2) . . ? N H4a 3.08(2) . '4 574' ? N H4b 2.81(2) . . ? N H5b 2.71(2) . '6 544' ? N H01a 2.93(3) . . ? O1 O2 2.173(2) . . ? O1 O3 2.151(2) . . ? O2 O3 2.163(2) . . ? O2 H3 2.24(2) . '4 574' ? O2 H6 2.16(2) . . ? O2 H4b 2.67(2) . . ? O3 O01 2.946(3) . . ? O3 H01a 2.19(3) . . ? O01 H11a 2.68(2) . '4 564' ? O01 H11a 2.68(2) . '3 565' ? H3 H12a 2.17(2) . . ? H3 H2a 2.20(3) . . ? H3 H4a 2.16(3) . . ? H6 H12a 2.30(2) . '7 565' ? H6 H5b 2.14(3) . . ? H6 H7b 2.17(3) . . ? H11a H11b 1.41(4) . . ? H11a H11c 1.60(3) . . ? H11a H7b 2.39(3) . '7 565' ? H11b H11c 1.45(4) . . ? H11c H2a 2.32(3) . . ? H12a H12b 1.55128(19) . . ? H12a H12c 1.5514(2) . . ? H12b H12c 1.5513(3) . . ? H2a H2b 1.60(3) . . ? H2b H4b 2.38(3) . . ? H4a H4b 1.58(3) . . ? H4a H5b 2.40(3) . . ? H4b H5b 2.38(3) . . ? H5a H5b 1.58(3) . . ? H5a H7a 2.28(3) . . ? H7a H7b 1.53(3) . . ? H01a H01a 1.20(5) . '2 554' ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1036 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 25 _reflns_limit_k_min 0 _reflns_limit_k_max 11 _reflns_limit_l_min -16 _reflns_limit_l_max 16 _reflns_number_observed ? _reflns_d_resolution_high .737 _reflns_d_resolution_low 9.41 _diffrn_reflns_av_sigmaI/netI .026 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 153 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .038 _refine_ls_wR_factor_all .044 _refine_ls_goodness_of_fit_all 1.298 _refine_ls_shift/su_mean .001 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_global _audit_creation_method Xtal3.6 _audit_creation_date 00-09-27 _audit_update_record ? #============================================================================== # (Publishing Staff Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia Nedlands Western Australia 6907 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal ? _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Skelton, Brian W.' . ; Department of Chemistry, University of Western Australia, Nedlands, WA 6907 Australia. ; _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Sheldrick, G.M. (1997). SHELXL97, Program for the Refinement of Crystal Structures. Univ. of G\"ottingen, Germany. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_cuyk3 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C12 H27 Cl4 Cu2 N5 O2' _chemical_formula_moiety ? _chemical_formula_weight 542.28 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C_1_c_1 _symmetry_space_group_name_Hall c_-2yc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2+x,1/2-y,1/2+z _cell_length_a 17.439(4) _cell_length_b 8.0368(16) _cell_length_c 15.946(3) _cell_angle_alpha 90.00000 _cell_angle_beta 112.59(3) _cell_angle_gamma 90.00000 _cell_volume 2063.4(9) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.2 _cell_measurement_theta_max 11.8 _cell_measurement_temperature 298 _exptl_absorpt_coefficient_mu 2.596 _exptl_crystal_description 'square column' _exptl_crystal_size_max .5 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .2 _exptl_crystal_size_rad ? _exptl_crystal_colour violet _diffrn_measurement_device_type 'STOE STADI4 4-circle-diffractometer' _diffrn_measurement_method '2\q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; ? ; _exptl_absorpt_correction_T_min .6217 _exptl_absorpt_correction_T_max .7407 _diffrn_reflns_number 2383 _reflns_number_total 2094 _reflns_Friedel_coverage ? _reflns_number_gt 2094 _reflns_threshold_expression 'I > 2.00 sig(I )' _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max 1.00 _diffrn_measured_fraction_theta_full 1.00 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 3 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt .0394 _refine_ls_wR_factor_ref .103 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_number_reflns 2383 _refine_ls_number_parameters 228 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+6.6204P] where P=(Fo^2^+2Fc^2^)/3' ; _refine_ls_hydrogen_treatment mixed _refine_ls_shift/su_max 0.0 _refine_diff_density_min -0.451 _refine_diff_density_max .482 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.58(7) # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'STADI4 (STOE, 1996)' _computing_cell_refinement 'STADI4 (STOE, 1996)' _computing_data_reduction 'X-RED (STOE, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XTAL ortep' _computing_publication_material 'XTAL bondla atable' _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. ; # 4. Supplementary data for validation and tables #------------------------------------------------ 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 48 .003296 .001587 'Int Tables Vol C Tables 4.2,6,8 and 6.1.1.4' H ? 0 108 0 0 'Int Tables Vol C Tables 4.2,6,8 and 6.1.1.4' N ? 0 20 .006104 .003296 'Int Tables Vol C Tables 4.2,6,8 and 6.1.1.4' O ? 0 8 .01062 .005981 'Int Tables Vol C Tables 4.2,6,8 and 6.1.1.4' Cl ? 0 16 .148376 .158508 'Int Tables Vol C Tables 4.2,6,8 and 6.1.1.4' Cu ? 0 8 .320129 1.2651 'Int Tables Vol C Tables 4.2,6,8 and 6.1.1.4' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 .02974(16) .99188(17) .31273(16) .0276(3) Uani ? ? 1.00000 ? ? Cu2 .03018(16) 1.28862(9) .06306(16) .0309(3) Uani ? ? 1.00000 ? ? Cl1 -.08119(18) 1.3826(4) -.05238(18) .0453(14) Uani ? ? 1.00000 ? ? Cl2 .13976(18) 1.3817(4) .18308(17) .0430(14) Uani ? ? 1.00000 ? ? Cl3 -.04119(19) 1.1761(4) .1423(2) .0443(14) Uani ? ? 1.00000 ? ? Cl4 .09990(19) 1.1974(4) -.0223(2) .0457(14) Uani ? ? 1.00000 ? ? C1 -.0997(8) .6992(12) .1742(8) .034(4) Uani ? ? 1.00000 ? ? C11 -.1639(9) .6513(18) .0813(9) .057(6) Uani ? ? 1.00000 ? ? H11a -.14280 .56100 .05690 .06900 Uiso ? ? 1.00000 ? ? H11b -.17490 .74520 .04120 .06900 Uiso ? ? 1.00000 ? ? H11c -.21430 .61740 .08730 .06900 Uiso ? ? 1.00000 ? ? N1 -.0886(4) .5484(8) .2341(5) .038(3) Uani ? ? 1.00000 ? ? O1 -.0174(4) .5086(8) .2831(5) .053(3) Uani ? ? 1.00000 ? ? O2 -.1501(5) .4726(9) .2314(6) .062(4) Uani ? ? 1.00000 ? ? C2 -.1362(7) .8375(12) .2094(7) .030(4) Uani ? ? 1.00000 ? ? H2a -.15110 .92660 .16490 .03700 Uiso ? ? 1.00000 ? ? H2b -.18720 .79720 .21320 .03700 Uiso ? ? 1.00000 ? ? N3 -.0842(6) .9092(9) .2985(6) .032(4) Uani ? ? 1.00000 ? ? H3 -.07600 .82690 .34030 .03800 Uiso ? ? 1.00000 ? ? C4 -.1241(7) 1.0517(15) .3280(8) .037(5) Uani ? ? 1.00000 ? ? H4a -.14960 1.12700 .27740 .04500 Uiso ? ? 1.00000 ? ? H4b -.16730 1.00930 .34650 .04500 Uiso ? ? 1.00000 ? ? C5 -.0638(9) 1.1397(15) .4018(9) .046(6) Uani ? ? 1.00000 ? ? H5a -.04710 1.07130 .45600 .05500 Uiso ? ? 1.00000 ? ? H5b -.08890 1.24040 .41340 .05500 Uiso ? ? 1.00000 ? ? N6 .0095(6) 1.1839(10) .3838(6) .030(4) Uani ? ? 1.00000 ? ? H6 -.00730 1.26930 .34330 .03700 Uiso ? ? 1.00000 ? ? C7 .0814(8) 1.2494(15) .4597(8) .041(6) Uani ? ? 1.00000 ? ? H7a .09920 1.16580 .50720 .05000 Uiso ? ? 1.00000 ? ? H7b .06340 1.34580 .48400 .05000 Uiso ? ? 1.00000 ? ? C8 .1547(8) 1.2986(14) .4388(9) .039(5) Uani ? ? 1.00000 ? ? H8 .13670 1.37970 .38910 .04800 Uiso ? ? 1.00000 ? ? C81 .2206(10) 1.3827(19) .5248(11) .077(8) Uani ? ? 1.00000 ? ? H81a .26780 1.41580 .51190 .09200 Uiso ? ? 1.00000 ? ? H81b .23790 1.30510 .57440 .09200 Uiso ? ? 1.00000 ? ? H81c .19660 1.47890 .54100 .09200 Uiso ? ? 1.00000 ? ? C2' -.0189(6) .7380(13) .1604(7) .029(4) Uani ? ? 1.00000 ? ? H2'a -.00080 .63820 .13910 .03400 Uiso ? ? 1.00000 ? ? H2'b -.03040 .82200 .11350 .03400 Uiso ? ? 1.00000 ? ? N3' .0509(6) .7989(9) .2454(6) .027(4) Uani ? ? 1.00000 ? ? H3' .06840 .71180 .28470 .03200 Uiso ? ? 1.00000 ? ? C4' .1212(7) .8491(14) .2181(7) .033(4) Uani ? ? 1.00000 ? ? H4'a .10210 .92620 .16740 .04000 Uiso ? ? 1.00000 ? ? H4'b .14520 .75250 .20090 .04000 Uiso ? ? 1.00000 ? ? C5' .1862(8) .9343(16) .3045(8) .042(6) Uani ? ? 1.00000 ? ? H5'a .20560 .85670 .35490 .05000 Uiso ? ? 1.00000 ? ? H5'b .23350 .97400 .29250 .05000 Uiso ? ? 1.00000 ? ? N6' .1414(5) 1.0750(10) .3250(5) .028(4) Uani ? ? 1.00000 ? ? H6' .13300 1.15280 .28090 .03300 Uiso ? ? 1.00000 ? ? C7' .1963(8) 1.1496(14) .4108(8) .038(5) Uani ? ? 1.00000 ? ? H7'a .24680 1.18740 .40480 .04600 Uiso ? ? 1.00000 ? ? H7'b .21150 1.06580 .45820 .04600 Uiso ? ? 1.00000 ? ? 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 .0245(3) .0307(4) .0294(3) -.0016(3) .0125(3) -.0051(3) Cu2 .0322(4) .0315(4) .0293(3) .0003(7) .0123(3) -.0006(6) Cl1 .0382(17) .0616(17) .0327(14) .0175(13) .0098(13) .0022(12) Cl2 .0428(18) .0486(15) .0350(15) -.0129(12) .0120(13) .0013(11) Cl3 .0354(16) .0529(15) .0456(16) -.0045(11) .0166(13) .0171(12) Cl4 .0370(16) .0572(16) .0446(16) .0004(12) .0174(13) -.0204(13) C1 .038(6) .028(5) .040(5) -.003(4) .019(5) -.007(4) C11 .037(6) .072(7) .060(7) -.014(6) .015(5) -.029(6) N1 .041(4) .033(3) .045(4) -.007(3) .021(3) -.006(3) O1 .052(4) .038(3) .062(4) .003(3) .015(3) .017(3) O2 .061(4) .049(4) .093(5) -.007(3) .047(4) .004(4) C2 .021(5) .029(4) .033(5) .002(3) .001(4) .001(4) N3 .033(5) .025(4) .043(5) .001(3) .020(4) .003(3) C4 .023(5) .034(5) .061(7) .001(4) .023(5) -.003(5) C5 .057(8) .041(6) .057(7) -.003(5) .040(7) -.013(5) N6 .030(5) .032(4) .023(4) .003(3) .003(4) .005(3) C7 .051(8) .042(6) .037(6) .002(5) .024(5) -.012(5) C8 .026(6) .040(5) .043(6) .000(4) .003(4) -.002(4) C81 .045(7) .080(9) .094(10) -.018(7) .013(7) -.052(9) C2' .023(5) .032(4) .028(5) -.001(4) .007(4) -.006(4) N3' .026(5) .028(4) .033(5) -.003(3) .018(4) -.003(3) C4' .028(5) .041(5) .033(5) -.001(4) .014(4) -.017(4) C5' .028(6) .060(7) .038(6) .001(5) .014(4) -.014(5) N6' .022(4) .036(4) .023(4) -.002(3) .006(3) -.002(3) C7' .030(6) .043(5) .040(6) .004(4) .012(5) -.014(5) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Cu1 Cl3 . . 2.920(4) ? Cu1 N3 . . 2.024(11) ? Cu1 N6 . . 2.024(10) ? Cu1 N3' . . 2.000(9) ? Cu1 N6' . . 1.996(9) ? Cu1 Cl4 . '2 575' 2.874(4) ? Cu2 Cl1 . . 2.233(3) ? Cu2 Cl2 . . 2.250(3) ? Cu2 Cl3 . . 2.274(5) ? Cu2 Cl4 . . 2.267(5) ? C1 C11 . . 1.524(16) ? C1 N1 . . 1.509(13) ? C1 C2 . . 1.493(17) ? C1 C2' . . 1.54(2) ? C11 H11a . . .961(16) ? C11 H11b . . .960(14) ? C11 H11c . . .959(17) ? N1 O1 . . 1.228(8) ? N1 O2 . . 1.220(11) ? C2 H2a . . .971(10) ? C2 H2b . . .970(13) ? C2 N3 . . 1.478(12) ? N3 H3 . . .910(8) ? N3 C4 . . 1.506(16) ? C4 H4a . . .969(11) ? C4 H4b . . .970(14) ? C4 C5 . . 1.428(16) ? C5 H5a . . .970(13) ? C5 H5b . . .971(14) ? C5 N6 . . 1.46(2) ? N6 H6 . . .910(8) ? N6 C7 . . 1.466(13) ? C7 H7a . . .970(12) ? C7 H7b . . .971(13) ? C7 C8 . . 1.49(2) ? C8 H8 . . .980(12) ? C8 C81 . . 1.564(18) ? C8 C7' . . 1.55(2) ? C81 H81a . . .96(2) ? C81 H81b . . .960(16) ? C81 H81c . . .961(17) ? C2' H2'a . . .970(11) ? C2' H2'b . . .970(11) ? C2' N3' . . 1.514(12) ? N3' H3' . . .910(8) ? N3' C4' . . 1.505(18) ? C4' H4'a . . .970(11) ? C4' H4'b . . .970(12) ? C4' C5' . . 1.566(15) ? C5' H5'a . . .970(12) ? C5' H5'b . . .970(15) ? C5' N6' . . 1.481(17) ? N6' H6' . . .910(8) ? N6' C7' . . 1.463(13) ? C7' H7'a . . .970(15) ? C7' H7'b . . .970(12) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published Cl3 Cu1 N3 . . . 90.9(3) ? Cl3 Cu1 N6 . . . 91.8(3) ? Cl3 Cu1 N3' . . . 89.6(3) ? Cl3 Cu1 N6' . . . 88.3(2) ? Cl3 Cu1 Cl4 . . '2 575' 178.42(16) ? N3 Cu1 N6 . . . 86.5(4) ? N3 Cu1 N3' . . . 93.5(4) ? N3 Cu1 N6' . . . 179.2(3) ? N3 Cu1 Cl4 . . '2 575' 89.0(3) ? N6 Cu1 N3' . . . 178.6(4) ? N6 Cu1 N6' . . . 93.6(4) ? N6 Cu1 Cl4 . . '2 575' 89.7(3) ? N3' Cu1 N6' . . . 86.4(4) ? N3' Cu1 Cl4 . . '2 575' 88.8(3) ? N6' Cu1 Cl4 . . '2 575' 91.8(2) ? Cl1 Cu2 Cl2 . . . 140.74(12) ? Cl1 Cu2 Cl3 . . . 95.98(16) ? Cl1 Cu2 Cl4 . . . 96.41(15) ? Cl2 Cu2 Cl3 . . . 97.29(15) ? Cl2 Cu2 Cl4 . . . 98.17(16) ? Cl3 Cu2 Cl4 . . . 137.66(13) ? Cu1 Cl3 Cu2 . . . 126.31(14) ? Cu2 Cl4 Cu1 . . '2 574' 125.65(15) ? C11 C1 N1 . . . 106.3(9) ? C11 C1 C2 . . . 107.1(10) ? C11 C1 C2' . . . 106.5(12) ? N1 C1 C2 . . . 109.2(11) ? N1 C1 C2' . . . 110.6(9) ? C2 C1 C2' . . . 116.7(9) ? C1 C11 H11a . . . 109.4(12) ? C1 C11 H11b . . . 109.5(12) ? C1 C11 H11c . . . 109.5(14) ? H11a C11 H11b . . . 109.5(16) ? H11a C11 H11c . . . 109.5(14) ? H11b C11 H11c . . . 109.5(13) ? C1 N1 O1 . . . 117.7(8) ? C1 N1 O2 . . . 118.8(7) ? O1 N1 O2 . . . 123.5(8) ? C1 C2 H2a . . . 107.9(11) ? C1 C2 H2b . . . 108.0(9) ? C1 C2 N3 . . . 117.3(9) ? H2a C2 H2b . . . 107.3(10) ? H2a C2 N3 . . . 108.0(8) ? H2b C2 N3 . . . 108.0(11) ? Cu1 N3 C2 . . . 116.7(9) ? Cu1 N3 H3 . . . 106.6(7) ? Cu1 N3 C4 . . . 105.5(6) ? C2 N3 H3 . . . 106.6(7) ? C2 N3 C4 . . . 114.2(8) ? H3 N3 C4 . . . 106.6(10) ? N3 C4 H4a . . . 109.5(12) ? N3 C4 H4b . . . 109.5(10) ? N3 C4 C5 . . . 110.6(10) ? H4a C4 H4b . . . 108.1(11) ? H4a C4 C5 . . . 109.5(11) ? H4b C4 C5 . . . 109.6(13) ? C4 C5 H5a . . . 109.1(12) ? C4 C5 H5b . . . 109.1(12) ? C4 C5 N6 . . . 112.5(13) ? H5a C5 H5b . . . 107.8(15) ? H5a C5 N6 . . . 109.1(12) ? H5b C5 N6 . . . 109.1(11) ? Cu1 N6 C5 . . . 106.2(7) ? Cu1 N6 H6 . . . 104.8(8) ? Cu1 N6 C7 . . . 117.3(8) ? C5 N6 H6 . . . 104.8(9) ? C5 N6 C7 . . . 117.5(11) ? H6 N6 C7 . . . 104.8(8) ? N6 C7 H7a . . . 108.2(11) ? N6 C7 H7b . . . 108.1(11) ? N6 C7 C8 . . . 116.4(11) ? H7a C7 H7b . . . 107.3(13) ? H7a C7 C8 . . . 108.3(11) ? H7b C7 C8 . . . 108.3(11) ? C7 C8 H8 . . . 108.7(11) ? C7 C8 C81 . . . 108.8(13) ? C7 C8 C7' . . . 113.3(10) ? H8 C8 C81 . . . 108.7(11) ? H8 C8 C7' . . . 108.7(13) ? C81 C8 C7' . . . 108.6(10) ? C8 C81 H81a . . . 109.5(16) ? C8 C81 H81b . . . 109.5(13) ? C8 C81 H81c . . . 109.5(13) ? H81a C81 H81b . . . 109.4(15) ? H81a C81 H81c . . . 109.4(15) ? H81b C81 H81c . . . 109.4(19) ? C1 C2' H2'a . . . 108.8(9) ? C1 C2' H2'b . . . 108.8(8) ? C1 C2' N3' . . . 113.8(10) ? H2'a C2' H2'b . . . 107.7(12) ? H2'a C2' N3' . . . 108.8(8) ? H2'b C2' N3' . . . 108.8(9) ? Cu1 N3' C2' . . . 118.7(7) ? Cu1 N3' H3' . . . 108.0(8) ? Cu1 N3' C4' . . . 106.6(6) ? C2' N3' H3' . . . 108.0(7) ? C2' N3' C4' . . . 107.0(9) ? H3' N3' C4' . . . 108.1(9) ? N3' C4' H4'a . . . 110.8(10) ? N3' C4' H4'b . . . 110.8(10) ? N3' C4' C5' . . . 104.9(10) ? H4'a C4' H4'b . . . 108.8(12) ? H4'a C4' C5' . . . 110.8(10) ? H4'b C4' C5' . . . 110.7(10) ? C4' C5' H5'a . . . 110.6(11) ? C4' C5' H5'b . . . 110.7(12) ? C4' C5' N6' . . . 105.3(9) ? H5'a C5' H5'b . . . 108.8(12) ? H5'a C5' N6' . . . 110.7(12) ? H5'b C5' N6' . . . 110.7(11) ? Cu1 N6' C5' . . . 107.5(7) ? Cu1 N6' H6' . . . 107.0(6) ? Cu1 N6' C7' . . . 119.5(8) ? C5' N6' H6' . . . 107.2(9) ? C5' N6' C7' . . . 107.9(8) ? H6' N6' C7' . . . 107.1(8) ? C8 C7' N6' . . . 112.0(9) ? C8 C7' H7'a . . . 109.2(10) ? C8 C7' H7'b . . . 109.2(13) ? N6' C7' H7'a . . . 109.2(12) ? N6' C7' H7'b . . . 109.2(10) ? H7'a C7' H7'b . . . 107.9(11) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- 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 Cu2 4.582(4) . '2 575' ? Cu1 Cu2 4.643(4) . . ? Cu1 C1 3.417(10) . . ? Cu1 N1 4.068(7) . . ? Cu1 C2 2.994(11) . . ? Cu1 H2a 3.173(2) . . ? Cu1 H3 2.444(3) . . ? Cu1 C4 2.827(14) . . ? Cu1 H4a 3.150(3) . . ? Cu1 C5 2.805(17) . . ? Cu1 H5a 3.126(3) . . ? Cu1 H6 2.4223(18) . . ? Cu1 C7 2.994(12) . . ? Cu1 H7a 3.186(2) . . ? Cu1 C8 3.391(11) . . ? Cu1 H8 3.5961(17) . . ? Cu1 C2' 3.033(11) . . ? Cu1 H2'b 3.240(2) . . ? Cu1 H3' 2.4398(18) . . ? Cu1 C4' 2.826(14) . . ? Cu1 H4'a 3.080(3) . . ? Cu1 C5' 2.820(15) . . ? Cu1 H5'a 3.075(3) . . ? Cu1 H6' 2.424(3) . . ? Cu1 C7' 3.000(12) . . ? Cu1 H7'b 3.183(2) . . ? Cu2 N1 4.520(9) . '1 565' ? Cu2 N3 4.224(9) . '2 574' ? Cu2 H3 3.443(2) . '2 574' ? Cu2 H5a 3.3661(13) . '2 574' ? Cu2 H2'a 3.1873(17) . '1 565' ? Cu2 H4'a 3.3499(13) . . ? Cu2 N6' 4.235(8) . . ? Cu2 H6' 3.419(2) . . ? Cl1 H11a 2.772(3) . '1 565' ? Cl1 N1 3.403(9) . '2 574' ? Cl1 N3 3.326(9) . '2 574' ? Cl1 H3 2.427(3) . '2 574' ? Cl2 N6' 3.339(9) . . ? Cl2 H6' 2.444(3) . . ? Cl3 N1 3.565(8) . '1 565' ? Cl3 N3 3.578(11) . . ? Cl3 N6 3.606(10) . . ? Cl3 N3' 3.528(8) . . ? Cl3 N6' 3.487(7) . . ? Cl4 N3 3.487(8) . '2 574' ? Cl4 N6 3.508(9) . '2 574' ? Cl4 N3' 3.467(10) . '2 574' ? Cl4 N6' 3.550(10) . '2 574' ? C1 H11a 2.054(11) . . ? C1 H11b 2.054(11) . . ? C1 H11c 2.054(11) . . ? C1 O1 2.347(12) . . ? C1 O2 2.353(15) . . ? C1 H2a 2.016(11) . . ? C1 H2b 2.016(15) . . ? C1 N3 2.537(15) . . ? C1 H2'a 2.066(15) . . ? C1 H2'b 2.066(15) . . ? C1 N3' 2.557(15) . . ? C11 N1 2.426(14) . . ? C11 O2 2.722(17) . . ? C11 C2 2.426(18) . . ? C11 H2a 2.548(15) . . ? C11 H2b 2.573(16) . . ? C11 C2' 2.454(17) . . ? C11 H2'a 2.634(15) . . ? C11 H2'b 2.578(15) . . ? H11a H11b 1.5684(3) . . ? H11a H11c 1.5683(3) . . ? H11a N1 2.615(8) . . ? H11a C2' 2.584(9) . . ? H11a H2'a 2.3962(5) . . ? H11b H11c 1.5670(2) . . ? H11b N1 3.267(7) . . ? H11b C2 2.609(11) . . ? H11b H2a 2.3579(3) . . ? H11b C2' 2.654(9) . . ? H11c N1 2.579(6) . . ? H11c O2 2.431(8) . . ? H11c C2 2.596(9) . . ? H11c H2b 2.3692(3) . . ? N1 C2 2.448(12) . . ? N1 H2a 3.274(6) . . ? N1 H2b 2.574(7) . . ? N1 N3 3.067(10) . . ? N1 H3 2.764(7) . . ? N1 N6 3.751(10) . '1 545' ? N1 H6 2.860(6) . '1 545' ? N1 C2' 2.506(14) . . ? N1 H2'a 2.635(9) . . ? N1 H2'b 3.326(8) . . ? N1 N3' 3.109(12) . . ? N1 H3' 2.859(7) . . ? O1 O2 2.157(10) . . ? O1 N3 3.464(10) . . ? O1 N6 3.005(11) . '1 545' ? O1 H6 2.126(7) . '1 545' ? O1 C2' 2.681(13) . . ? O1 H2'a 2.637(8) . . ? O1 N3' 2.788(11) . . ? O1 H3' 2.208(7) . . ? O2 C2 2.974(12) . . ? O2 H2b 2.677(7) . . ? O2 H5'b 2.567(10) . '3 445' ? C2 H3 1.945(10) . . ? C2 C4 2.506(17) . . ? C2 H4a 2.615(10) . . ? C2 C2' 2.581(18) . . ? C2 N3' 3.104(16) . . ? H2a H2b 1.5632(2) . . ? H2a N3 2.002(8) . . ? H2a C4 2.656(13) . . ? H2b N3 2.002(8) . . ? H2b H3 2.2149(5) . . ? H2b C4 2.683(12) . . ? N3 H4a 2.045(8) . . ? N3 H4b 2.046(11) . . ? N3 C5 2.413(15) . . ? N3 H5a 2.679(9) . . ? N3 H5b 3.250(8) . . ? N3 N6 2.772(11) . . ? N3 H6 3.154(8) . . ? N3 C2' 3.157(16) . . ? N3 N3' 2.930(16) . . ? N3 H3' 3.178(10) . . ? N3 N6' 4.019(14) . . ? H3 C4 1.970(12) . . ? H3 H4b 2.1942(3) . . ? H3 C5 2.677(12) . . ? H3 N6 3.185(8) . . ? H3 N3' 3.132(12) . . ? C4 H5a 1.972(11) . . ? C4 H5b 1.972(12) . . ? C4 N6 2.399(15) . . ? C4 H6 2.624(12) . . ? H4a H4b 1.5702(2) . . ? H4a C5 1.976(12) . . ? H4a H5b 2.2115(4) . . ? H4a N6 2.678(9) . . ? H4b C5 1.978(13) . . ? H4b H5a 2.2089(5) . . ? H4b H5b 2.3101(4) . . ? H4b N6 3.228(10) . . ? C5 H6 1.906(16) . . ? C5 C7 2.50(2) . . ? C5 H7a 2.698(13) . . ? C5 H7b 2.674(13) . . ? H5a H5b 1.5682(3) . . ? H5a N6 1.998(11) . . ? H5a C7 2.641(14) . . ? H5b N6 1.999(11) . . ? H5b H6 2.1332(4) . . ? N6 H7a 1.994(8) . . ? N6 H7b 1.994(8) . . ? N6 C8 2.515(16) . . ? N6 H8 2.694(10) . . ? N6 N3' 4.024(13) . . ? N6 N6' 2.931(15) . . ? N6 H6' 3.179(12) . . ? N6 C7' 3.130(18) . . ? H6 C7 1.913(10) . . ? H6 H7b 2.1924(4) . . ? H6 C8 2.655(12) . . ? H6 N6' 3.135(9) . . ? C7 H8 2.032(15) . . ? C7 C81 2.49(2) . . ? C7 H81b 2.676(11) . . ? C7 H81c 2.668(12) . . ? C7 N6' 3.066(17) . . ? C7 C7' 2.54(2) . . ? H7a H7b 1.5627(3) . . ? H7a C8 2.019(15) . . ? H7a C81 2.673(17) . . ? H7a N6' 3.340(9) . . ? H7a C7' 2.692(16) . . ? H7b C8 2.020(16) . . ? H7b H8 2.3419(4) . . ? H7b C81 2.580(17) . . ? H7b H81c 2.3967(5) . . ? C8 H81a 2.090(12) . . ? C8 H81b 2.091(12) . . ? C8 H81c 2.092(12) . . ? C8 N6' 2.501(15) . . ? C8 H6' 2.669(14) . . ? C8 H7'a 2.084(15) . . ? C8 H7'b 2.084(12) . . ? H8 C81 2.096(14) . . ? H8 H81a 2.3887(5) . . ? H8 H81c 2.3770(4) . . ? H8 N6' 2.667(8) . . ? H8 C7' 2.084(12) . . ? C81 C7' 2.53(2) . . ? C81 H7'a 2.647(18) . . ? H81a H81b 1.5671(2) . . ? H81a H81c 1.5674(3) . . ? H81a C7' 2.681(11) . . ? H81b H81c 1.5680(3) . . ? C2' H3' 1.993(9) . . ? C2' C4' 2.426(15) . . ? C2' H4'a 2.564(11) . . ? C2' H4'b 2.683(10) . . ? H2'a H2'b 1.5663(3) . . ? H2'a N3' 2.045(8) . . ? H2'a H3' 2.2459(4) . . ? H2'a C4' 2.632(11) . . ? H2'b N3' 2.044(8) . . ? H2'b C4' 2.536(10) . . ? H2'b H4'a 2.2920(5) . . ? N3' H4'a 2.060(11) . . ? N3' H4'b 2.060(12) . . ? N3' C5' 2.435(16) . . ? N3' H5'a 2.631(9) . . ? N3' H5'b 3.294(10) . . ? N3' N6' 2.736(11) . . ? N3' H6' 3.136(8) . . ? H3' C4' 1.986(13) . . ? H3' H4'b 2.2497(4) . . ? H3' C5' 2.649(14) . . ? H3' N6' 3.150(8) . . ? C4' H5'a 2.112(9) . . ? C4' H5'b 2.113(10) . . ? C4' N6' 2.422(14) . . ? C4' H6' 2.616(11) . . ? H4'a H4'b 1.5782(3) . . ? H4'a C5' 2.115(11) . . ? H4'a N6' 2.625(8) . . ? H4'b C5' 2.114(12) . . ? H4'b N6' 3.277(8) . . ? C5' H6' 1.954(13) . . ? C5' C7' 2.381(18) . . ? C5' H7'a 2.552(12) . . ? C5' H7'b 2.547(13) . . ? H5'a H5'b 1.5772(2) . . ? H5'a N6' 2.037(8) . . ? H5'a C7' 2.544(12) . . ? H5'a H7'b 2.3276(3) . . ? H5'b N6' 2.036(9) . . ? H5'b H6' 2.2185(4) . . ? H5'b C7' 2.629(14) . . ? N6' H7'a 2.004(7) . . ? N6' H7'b 2.004(7) . . ? H6' C7' 1.937(11) . . ? H6' H7'a 2.2152(5) . . ? H7'a H7'b 1.5690(2) . . ? _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _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. ; _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1104 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min -22 _reflns_limit_h_max 17 _reflns_limit_k_min -10 _reflns_limit_k_max 0 _reflns_limit_l_min -20 _reflns_limit_l_max 17 _reflns_number_observed ? _reflns_d_resolution_high ? _reflns_d_resolution_low ? _diffrn_reflns_av_sigmaI/netI .026 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 298 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'planar graphite' _diffrn_radiation_detector 'scintillation counter' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 2 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0498 _refine_ls_wR_factor_all 0.095 _refine_ls_goodness_of_fit_all 1.158 _refine_ls_shift/su_mean 0.00 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #===END