# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Kamil Wojciechowski' 'Gerald Bernardinelli' 'Anna Bitner' 'Marcin Brynda' _publ_contact_author_name 'Kamil Wojciechowski' _publ_contact_author_email KAMIL.WOJCIECHOWSKI@CH.PW.EDU.PL _publ_section_title ; Azacrown Ether-Copper(II)-Hexanoate Complexes. >From Monomer to 1-D Metal Organic Polymer ; # Attachment 'CCDC_689064.txt' data_WOJC _database_code_depnum_ccdc_archive 'CCDC 689064' _chemical_formula_moiety 'C12 H26 Cu1 N2 O4, 2(C6 H11 O2)' _chemical_formula_sum 'C24 H48 Cu1 N2 O8' _chemical_formula_weight 556.3 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 10.5343(9) _cell_length_b 16.7311(9) _cell_length_c 8.3453(5) _cell_angle_alpha 90.00000 _cell_angle_beta 91.272(9) _cell_angle_gamma 90.00000 _cell_volume 1470.50(18) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.256 _exptl_crystal_density_meas not_measured _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 4.8 _cell_measurement_theta_max 28.0 _cell_measurement_temperature 200 _exptl_crystal_F_000 598 _exptl_absorpt_coefficient_mu .79 _exptl_crystal_description prism _exptl_crystal_size_max .29 _exptl_crystal_size_mid .28 _exptl_crystal_size_min .11 _exptl_crystal_colour blue _diffrn_measurement_device_type 'Stoe Ipds' _diffrn_measurement_method \f _diffrn_detector_area_resol_mean 6 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'XRED; Stoe & Cie, 1999' _exptl_absorpt_correction_T_min .7953 _exptl_absorpt_correction_T_max .9114 _diffrn_reflns_number 19393 _reflns_number_total 3529 _reflns_number_gt 2026 _reflns_threshold_expression 'refl observed if Fo > 3.99 \s(Fo)' _diffrn_reflns_theta_max 28. _diffrn_reflns_theta_full 28. _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .066 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .045 _refine_ls_wR_factor_ref .045 _refine_ls_goodness_of_fit_ref 1.77(3) _refine_ls_number_reflns 2026 _refine_ls_number_parameters 163 _refine_ls_weighting_scheme calc _refine_ls_weighting_details \w=1/[\s^2^(Fo)+0.00015(Fo^2^)] _refine_ls_hydrogen_treatment mixed _refine_ls_shift/su_max .0001 _refine_diff_density_max 1.583 _refine_diff_density_min -1.075 _refine_ls_extinction_method none _refine_ls_abs_structure_details none _computing_data_collection 'EXPOSE (Stoe & Cie, 1999)' _computing_cell_refinement 'CELL (Stoe & Cie, 1999)' _computing_data_reduction 'XRED (Stoe & Cie, 1999)' _computing_structure_solution SIR97 _computing_structure_refinement xtal_CRYLSQ _computing_molecular_graphics xtal_gx3 _computing_publication_material xtal_CIFIO loop_ _atom_type_symbol _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag C Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .002 .002 H Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 0 0 N Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .004 .003 O Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .008 .006 Cu1 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .263 1.266 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Cu1 .00000 .50000 .50000 .0342(3) 1.00000 Uani O1 -.1535(4) .31065(13) .3769(3) .0554(16) 1.00000 Uani O2 .0073(3) .36290(12) .6515(3) .0462(14) 1.00000 Uani N1 -.1008(4) .47064(17) .2974(4) .0425(17) 1.00000 Uani C1 -.2299(4) .4407(3) .3143(5) .049(3) 1.00000 Uani C2 -.2356(5) .3730(3) .4317(5) .052(3) 1.00000 Uani C3 -.1038(5) .26024(19) .5028(5) .056(3) 1.00000 Uani C4 .0213(5) .28810(18) .5687(5) .053(3) 1.00000 Uani C5 .1162(5) .38208(19) .7481(5) .051(3) 1.00000 Uani C6 .0939(5) .4636(3) .8215(4) .048(3) 1.00000 Uani O1a .1611(3) .46360(14) .4078(3) .0464(14) 1.00000 Uani O2a .1136(4) .39222(15) .1870(4) .0615(18) 1.00000 Uani C1a .1907(5) .41963(18) .2889(5) .049(3) 1.00000 Uani C2a .3229(7) .4024(4) .2673(9) .095(5) 1.00000 Uani C3a .4080(7) .4723(4) .2863(9) .099(5) 1.00000 Uani C4a .3833(6) .5422(4) .1729(8) .091(4) 1.00000 Uani C5a .4753(8) .6113(5) .1982(11) .115(6) 1.00000 Uani C6a .4570(9) .6804(5) .0862(13) .141(7) 1.00000 Uani H101 -.046(4) .435(3) .273(5) .04000 1.00000 Uiso H11 -.28399 .48426 .35142 .05000 1.00000 Uiso H12 -.26143 .42181 .20962 .05000 1.00000 Uiso H21 -.20678 .39143 .53811 .05000 1.00000 Uiso H22 -.32277 .35314 .43763 .05000 1.00000 Uiso H31 -.16454 .25941 .59004 .05000 1.00000 Uiso H32 -.09353 .20616 .46034 .05000 1.00000 Uiso H41 .05545 .24795 .64320 .05000 1.00000 Uiso H42 .07995 .29532 .48019 .05000 1.00000 Uiso H51 .12781 .34207 .83301 .05000 1.00000 Uiso H52 .19178 .38336 .68183 .05000 1.00000 Uiso H61 .01000 .46389 .86934 .05000 1.00000 Uiso H62 .15924 .47297 .90462 .05000 1.00000 Uiso H21a .34919 .36164 .34512 .05000 1.00000 Uiso H22a .33247 .38087 .15800 .05000 1.00000 Uiso H31a .39939 .49235 .39553 .05000 1.00000 Uiso H32a .49505 .45425 .27029 .05000 1.00000 Uiso H41a .39094 .52274 .06237 .05000 1.00000 Uiso H42a .29659 .56139 .18854 .05000 1.00000 Uiso H51a .46519 .63167 .30772 .05000 1.00000 Uiso H52a .56163 .59158 .18592 .05000 1.00000 Uiso H61a .46642 .66048 -.02339 .05000 1.00000 Uiso H62a .36998 .70057 .09841 .05000 1.00000 Uiso H63a .51543 .72510 .10250 .05000 1.00000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu1 .0587(4) .0243(3) .0197(3) .0006(4) .0010(3) -.0016(3) O1 .098(3) .0326(12) .0359(14) -.0003(13) .0047(14) -.0034(10) O2 .0745(19) .0263(11) .0377(14) .0010(12) .0010(13) -.0006(10) N1 .072(3) .0290(12) .0265(15) .0010(14) -.0046(15) -.0026(11) C1 .064(3) .0421(18) .042(3) -.0060(18) -.0096(19) -.0033(15) C2 .070(3) .0383(18) .047(3) -.0090(18) .002(2) -.0065(16) C3 .098(4) .0239(15) .047(3) -.0043(18) .011(3) -.0011(15) C4 .087(4) .0228(15) .051(3) .0080(18) .013(3) .0031(14) C5 .079(3) .0346(17) .040(3) .0021(18) -.005(3) .0121(15) C6 .080(3) .0407(17) .0229(18) .0019(18) -.0049(18) .0040(14) O1a .0622(18) .0383(12) .0389(14) .0005(12) .0042(12) -.0057(10) O2a .108(3) .0392(13) .0375(15) .0036(15) .0151(17) -.0098(11) C1a .075(3) .0252(15) .047(3) .0017(17) .022(3) -.0033(15) C2a .096(5) .062(3) .128(6) .002(3) .036(4) -.030(3) C3a .081(4) .116(5) .100(5) .012(4) .001(4) -.002(4) C4a .085(5) .096(4) .093(5) .002(4) .016(4) .001(4) C5a .104(6) .099(5) .144(7) .002(4) .017(5) -.002(5) C6a .145(8) .091(5) .187(9) .009(5) -.004(7) -.005(6) 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 Cu1 O2 . . 2.620(3) Cu1 N1 . . 2.037(4) Cu1 O1a . . 1.975(3) Cu1 O2 . 3_566 2.620(3) Cu1 N1 . 3_566 2.037(4) Cu1 O1a . 3_566 1.975(3) O1 C2 . . 1.437(5) O1 C3 . . 1.437(5) O2 C4 . . 1.439(4) O2 C5 . . 1.424(5) N1 C1 . . 1.459(6) N1 H101 . . .85(4) N1 C6 . 3_566 1.484(5) C1 C2 . . 1.500(6) C3 C4 . . 1.491(7) C5 C6 . . 1.515(5) O1a C1a . . 1.279(5) O2a C1a . . 1.250(5) C1a C2a . . 1.438(8) C2a C3a . . 1.480(9) C3a C4a . . 1.523(9) C4a C5a . . 1.521(10) C5a C6a . . 1.497(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 O2 Cu1 N1 . . . 101.46(10) O2 Cu1 O1a . . . 84.37(9) O2 Cu1 O2 . . 3_566 180.0000 O2 Cu1 N1 . . 3_566 78.54(10) O2 Cu1 O1a . . 3_566 95.63(9) N1 Cu1 O1a . . . 92.22(13) N1 Cu1 O2 . . 3_566 78.54(10) N1 Cu1 N1 . . 3_566 180.00(17) N1 Cu1 O1a . . 3_566 87.78(13) O1a Cu1 O2 . . 3_566 95.63(9) O1a Cu1 N1 . . 3_566 87.78(13) O1a Cu1 O1a . . 3_566 180.0(6) O2 Cu1 N1 3_566 . 3_566 101.46(10) O2 Cu1 O1a 3_566 . 3_566 84.37(9) N1 Cu1 O1a 3_566 . 3_566 92.22(13) C2 O1 C3 . . . 113.9(3) Cu1 O2 C4 . . . 122.1(2) Cu1 O2 C5 . . . 95.19(17) C4 O2 C5 . . . 112.2(3) Cu1 N1 C1 . . . 118.2(3) Cu1 N1 C6 . . 3_566 110.1(3) C1 N1 H101 . . . 115(3) C1 N1 C6 . . 3_566 112.2(4) H101 N1 C6 . . 3_566 108(3) N1 C1 C2 . . . 111.9(4) O1 C2 C1 . . . 107.9(4) O1 C3 C4 . . . 113.0(3) O2 C4 C3 . . . 110.4(4) O2 C5 C6 . . . 107.5(4) C5 C6 N1 . . 3_566 112.8(3) Cu1 O1a C1a . . . 134.9(3) O1a C1a O2a . . . 124.9(4) O1a C1a C2a . . . 117.8(5) O2a C1a C2a . . . 117.2(5) C1a C2a C3a . . . 114.4(5) C2a C3a C4a . . . 116.5(6) C3a C4a C5a . . . 113.5(6) C4a C5a C6a . . . 115.4(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 C3 O1 C2 C1 . . . . 153.3(4) C2 O1 C3 C4 . . . . -92.1(5) C5 O2 C4 C3 . . . . 165.9(3) C4 O2 C5 C6 . . . . 176.8(3) H101 N1 C1 C2 . . . . 54(3) C6 N1 C1 C2 3_566 . . . 178.7(3) N1 C1 C2 O1 . . . . -58.2(4) O1 C3 C4 O2 . . . . 67.2(5) O2 C5 C6 N1 . . . 3_566 -71.6(5) O1a C1a C2a C3a . . . . -44.7(7) O2a C1a C2a C3a . . . . 133.4(6) C1a C2a C3a C4a . . . . -59.5(8) C2a C3a C4a C5a . . . . -179.3(6) C3a C4a C5a C6a . . . . 178.3(7) #=END================================================= # Attachment 'polymeric_species_2.cif' data_KALM2 _database_code_depnum_ccdc_archive 'CCDC 706687' # Due to the poor resolution of this crystal structure, this file is # given for information # (see _refine_special_details) #-------------------------------------------------------------------- _audit_creation_date 2008-09-05 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record 2008-09-06 _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.0.1 #-------------------------------------------------------------------- _chemical_formula_moiety 'C72 H138 Cu4.5 N3 O24' _chemical_formula_sum 'C72 H138 Cu4.5 N3 O24' _chemical_formula_weight 1716.1 _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 13.2193(7) _cell_length_b 17.5953(14) _cell_length_c 22.5887(15) _cell_angle_alpha 106.272(9) _cell_angle_beta 91.889(7) _cell_angle_gamma 106.310(8) _cell_volume 4805.0(7) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.186 _exptl_crystal_density_meas not_measured _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 25.8 _cell_measurement_temperature 200 _exptl_absorpt_coefficient_mu .94 _exptl_crystal_description plate _exptl_crystal_colour green _diffrn_measurement_device_type 'Stoe Ipds' _diffrn_measurement_method \f _diffrn_detector_area_resol_mean 6 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'XRED; Stoe & Cie, 1999' _exptl_absorpt_correction_T_min .7689 _exptl_absorpt_correction_T_max .9344 _diffrn_reflns_number 51622 _reflns_number_total 17478 _reflns_number_gt 5560 _reflns_threshold_expression 'refl observed if Fo > 2.99 \s(Fo)' _diffrn_reflns_theta_max 25.8 _diffrn_reflns_theta_full 25.8 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .131 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .092 _refine_ls_wR_factor_ref .103 _refine_ls_goodness_of_fit_ref 1.50(1) _refine_ls_number_reflns 5950 _refine_ls_number_parameters 569 _refine_ls_weighting_scheme calc _refine_ls_weighting_details \w=1/[\s^2^(Fo)+0.0003(Fo^2^)] _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .674 _refine_diff_density_max 1.68 _refine_diff_density_min -1.35 _refine_ls_extinction_method none _refine_ls_abs_structure_details none _refine_special_details ; After several trial during a long time the best crystal obtained for this complex shows a very poor diffraction. Nevertheless the observed topology obtained for the complex (without taking into account the hydrogen atoms nor the unobserved solvant molecule) is unambiguous. ; _computing_data_collection 'EXPOSE (Stoe & Cie, 1999)' _computing_cell_refinement 'CELL (Stoe & Cie, 1999)' _computing_data_reduction 'XRED (Stoe & Cie, 1999)' _computing_structure_solution SIR97 _computing_structure_refinement xtal_CRYLSQ _computing_molecular_graphics xtal_gx3 _computing_publication_material xtal_CIFIO loop_ _atom_type_symbol _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag C Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .002 .002 H Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 0 0 N Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .004 .003 O Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .008 .006 Cu Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .263 1.266 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Cu1 .50000 1.00000 .50000 .05816 1.00000 Uani Cu2 .8970(2) .98394(18) .49020(11) .04446 1.00000 Uani Cu3 .6408(2) .93249(18) .15027(10) .03938 1.00000 Uani Cu4 1.0366(2) .90523(18) .13852(11) .04614 1.00000 Uani Cu5 1.24291(19) .95101(17) .13918(11) .04429 1.00000 Uani O1a .5563(16) .9892(18) .6276(8) .13991 1.00000 Uani O2a .322(3) .870(3) .5484(15) .22318 1.00000 Uiso N1a .6497(15) 1.0809(15) .5361(10) .08864 1.00000 Uani C1a .677(3) 1.1185(19) .6110(13) .09296 1.00000 Uiso C2a .666(4) 1.048(3) .6333(15) .13664 1.00000 Uiso C3a .548(4) .918(3) .6451(17) .14000 1.00000 Uiso C4a .428(6) .876(5) .648(3) .25200 1.00000 Uiso C5a .366(7) .831(5) .592(4) .33900 1.00000 Uiso C6a .323(3) .846(3) .4769(15) .12310 1.00000 Uiso O1b .5563(11) .9096(10) .4560(7) .07192 1.00000 Uani O2b .7278(13) .9609(10) .4726(7) .06557 1.00000 Uani C1b .6466(19) .9035(14) .4544(9) .04415 1.00000 Uiso C2b .6528(19) .8168(15) .4233(10) .06780 1.00000 Uiso C3b .609(4) .757(3) .4689(18) .17620 1.00000 Uiso C4b .669(5) .693(4) .467(4) .34495 1.00000 Uiso C5b .621(5) .638(4) .5081(19) .26681 1.00000 Uiso C6b .647(6) .554(3) .486(3) .29436 1.00000 Uiso O1c .8940(12) .8857(10) .5161(6) .06207 1.00000 Uani O2c 1.0707(12) .9119(10) .5311(6) .06074 1.00000 Uani C1c .978(3) .8669(14) .5279(9) .04847 1.00000 Uiso C2c .955(3) .7838(17) .5459(11) .08849 1.00000 Uiso C3c 1.043(3) .751(3) .5381(15) .13495 1.00000 Uiso C4c .998(5) .664(3) .559(2) .17546 1.00000 Uiso C5c 1.081(6) .662(5) .575(3) .28037 1.00000 Uiso C6c 1.093(6) .587(5) .596(3) .29695 1.00000 Uiso O1d .9179(10) .9287(9) .4055(6) .05026 1.00000 Uani O2d 1.0947(13) .9506(10) .4223(6) .06740 1.00000 Uani C1d 1.0069(19) .9212(13) .3901(9) .04023 1.00000 Uiso C2d 1.0016(19) .8698(15) .3226(10) .06800 1.00000 Uiso C3d .914(2) .7908(16) .3028(11) .08016 1.00000 Uiso C4d .923(3) .7245(19) .3414(13) .10708 1.00000 Uiso C5d .829(3) .646(3) .3148(16) .14632 1.00000 Uiso C6d .829(4) .583(3) .350(2) .20719 1.00000 Uiso O1e .6681(11) .9536(9) .2665(6) .05469 1.00000 Uani O2e .8740(12) 1.0710(11) .2598(7) .07390 1.00000 Uani O3e .6047(12) .9065(9) .0333(6) .05850 1.00000 Uani O4e .4085(12) .7791(10) .0369(7) .06639 1.00000 Uani N1e .4992(13) .8614(11) .1616(7) .05019 1.00000 Uani N2e .7822(12) 1.0073(10) .1382(6) .03692 1.00000 Uani C1e .4881(16) .8807(13) .2309(9) .05100 1.00000 Uiso C2e .5827(18) .8799(14) .2651(9) .05814 1.00000 Uiso C3e .7663(19) .9577(14) .2961(10) .06539 1.00000 Uiso C4e .8426(18) 1.0437(14) .3151(10) .06454 1.00000 Uiso C5e .8058(18) 1.1133(14) .2394(10) .05887 1.00000 Uiso C6e .8114(16) 1.0980(13) .1703(9) .04173 1.00000 Uiso C7e .7881(15) .9880(12) .0667(8) .04322 1.00000 Uiso C8e .6843(17) .9861(13) .0337(9) .04986 1.00000 Uiso C9e .5021(18) .8936(14) .0013(9) .05620 1.00000 Uiso C10e .4407(19) .8020(15) -.0175(10) .07379 1.00000 Uiso C11e .4783(18) .7481(14) .0648(9) .06107 1.00000 Uiso C12e .4715(16) .7672(14) .1333(9) .04987 1.00000 Uiso O1f .6986(10) .8380(8) .1419(5) .04441 1.00000 Uani O2f .8706(10) .8861(9) .1430(7) .05383 1.00000 Uani C1f .7928(18) .8302(13) .1389(9) .04037 1.00000 Uiso C2f .8030(17) .7428(14) .1252(9) .05828 1.00000 Uiso C3f .700(3) .6731(19) .1315(12) .10481 1.00000 Uiso C4f .727(3) .5908(19) .1228(12) .10708 1.00000 Uiso C5f .624(3) .523(3) .1209(16) .14326 1.00000 Uiso C6f .643(5) .446(4) .115(3) .24368 1.00000 Uiso O1g 1.0741(12) .9844(10) .2225(6) .05772 1.00000 Uani O2g 1.2488(11) 1.0213(10) .2261(6) .05716 1.00000 Uani C1g 1.169(3) 1.0263(15) .2487(10) .05651 1.00000 Uiso C2g 1.173(2) 1.0851(16) .3121(11) .07514 1.00000 Uiso C3g 1.230(3) 1.171(3) .3166(15) .13282 1.00000 Uiso C4g 1.172(4) 1.206(3) .2733(17) .14874 1.00000 Uiso C5g 1.182(7) 1.287(6) .288(4) .35905 1.00000 Uiso C6g 1.108(4) 1.304(3) .2440(19) .18235 1.00000 Uiso O1h 1.0414(11) .9972(10) .1051(7) .06072 1.00000 Uani O2h 1.2190(11) 1.0422(9) .1112(6) .05531 1.00000 Uani C1h 1.1264(19) 1.0452(13) .0987(9) .04637 1.00000 Uiso C2h 1.1183(17) 1.1184(13) .0785(9) .05317 1.00000 Uiso C3h 1.2309(19) 1.1868(15) .0855(10) .07070 1.00000 Uiso C4h 1.212(3) 1.2633(17) .0662(11) .08954 1.00000 Uiso C5h 1.323(3) 1.328(3) .0732(14) .12908 1.00000 Uiso C6h 1.296(4) 1.399(3) .0590(19) .19488 1.00000 Uiso O1i 1.0337(14) .8335(10) .0546(7) .07359 1.00000 Uani O2i 1.2092(12) .8792(10) .0523(6) .06209 1.00000 Uani C1i 1.122(3) .8367(15) .0314(10) .05516 1.00000 Uiso C2i 1.113(3) .779(3) -.0421(13) .11459 1.00000 Uiso C3i 1.098(4) .701(3) -.0441(16) .20586 1.00000 Uiso C4i 1.047(3) .638(3) -.1089(19) .27870 1.00000 Uiso C5i 1.124(4) .646(3) -.1546(17) .24568 1.00000 Uiso C6i 1.089(4) .566(3) -.2123(16) .18619 1.00000 Uiso O1j 1.0638(11) .8191(10) .1722(6) .05750 1.00000 Uani O2j 1.2350(12) .8539(10) .1704(7) .06578 1.00000 Uani C1j 1.1496(18) .8072(13) .1792(9) .04165 1.00000 Uiso C2j 1.1596(18) .7367(14) .2024(10) .06416 1.00000 Uiso C3j 1.072(3) .6640(17) .1798(12) .09155 1.00000 Uiso C4j 1.067(4) .631(3) .115(3) .19711 1.00000 Uiso C5j 1.161(5) .604(4) .097(3) .23406 1.00000 Uiso C6j 1.171(5) .552(4) .024(3) .27341 1.00000 Uiso O1k .5850(10) 1.0316(9) .1667(6) .04696 1.00000 Uani O2k 1.4114(11) .9749(9) .1372(6) .04516 1.00000 Uani C1k .4898(18) 1.0358(14) .1597(9) .04060 1.00000 Uiso C2k .4747(17) 1.1207(14) .1784(9) .05624 1.00000 Uiso C3k .580(3) 1.1922(19) .1973(12) .11626 1.00000 Uiso C4k .546(4) 1.271(3) .2089(14) .19730 1.00000 Uiso C5k .559(5) 1.314(3) .2770(16) .26942 1.00000 Uiso C6k .545(9) 1.400(4) .288(3) .52115 1.00000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu1 .03005 .08001 .06284 .02308 .00589 .01261 Cu2 .02727 .06836 .04048 .02086 .00733 .01390 Cu3 .02707 .05552 .04024 .01635 .00713 .01753 Cu4 .03024 .06331 .05347 .02140 .01155 .02297 Cu5 .03021 .06696 .04516 .02198 .00806 .02395 O1a .07294 .27519 .06300 .06940 .01974 .01951 N1a .05064 .11249 .11016 .01158 .00914 .05825 O1b .03212 .09405 .09139 .03287 .01707 .01585 O2b .06176 .06358 .06682 .03008 .01505 .00060 O1c .05298 .07696 .06625 .02597 .01060 .03040 O2c .03968 .07523 .06757 .01480 .00094 .02514 O1d .03028 .08349 .04064 .02423 .00204 .01758 O2d .05190 .10317 .04099 .02086 .01735 .01345 O1e .04286 .08385 .04566 .02492 -.00138 .02744 O2e .05058 .10913 .06612 .02448 .01426 .03172 O3e .05397 .07315 .05309 .01963 .00206 .02646 O4e .04784 .07146 .07362 .00676 -.00892 .02532 N1e .04931 .05563 .05384 .02290 .02340 .02032 N2e .02902 .04504 .03525 .00958 .00420 .01142 O1f .02508 .06427 .03902 .01106 -.00040 .01096 O2f .01691 .04688 .09933 .00784 .00520 .02662 O1g .06206 .08021 .04739 .04316 .02274 .02140 O2g .03745 .09936 .03963 .03117 .01180 .01737 O1h .02915 .08171 .08833 .01939 .01333 .04880 O2h .03991 .08297 .06228 .02517 .00856 .04495 O1i .06746 .07254 .06395 .01283 -.01700 .00560 O2i .04948 .08361 .04291 .02162 .01592 .00046 O1j .03335 .08621 .06532 .02250 .00638 .03765 O2j .04912 .07027 .09486 .02626 .01798 .04194 O1k .02083 .07738 .04841 .02384 .00990 .01824 O2k .03362 .05371 .05503 .02228 .00872 .01763 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 Cu1 N1a . . 2.066(18) Cu1 O1b . . 1.974(17) Cu1 N1a . 2_676 2.066(18) Cu1 O1b . 2_676 1.974(17) Cu2 O1c . . 1.965(19) Cu2 O1d . . 1.956(12) Cu2 O2c . 2_776 1.961(18) Cu2 O2d . 2_776 1.971(13) Cu3 N1e . . 2.008(16) Cu3 N2e . . 2.038(14) Cu3 O1f . . 1.982(16) Cu3 O1k . . 2.024(16) Cu4 O1g . . 1.964(12) Cu4 O1h . . 1.955(18) Cu4 O1i . . 1.953(14) Cu4 O1j . . 1.983(18) Cu5 O2g . . 1.992(13) Cu5 O2h . . 1.977(18) Cu5 O2i . . 1.970(12) Cu5 O2j . . 2.003(19) O1a C2a . . 1.50(5) O1a C3a . . 1.39(6) O2a C5a . . 1.53(11) O2a C6a . . 1.55(5) N1a C1a . . 1.62(4) N1a C6a . 2_676 1.36(5) C1a C2a . . 1.44(6) C3a C4a . . 1.56(9) C4a C5a . . 1.38(10) O1b C1b . . 1.23(4) O2b C1b . . 1.21(3) C1b C2b . . 1.52(4) C2b C3b . . 1.67(6) C3b C4b . . 1.54(8) C4b C5b . . 1.57(9) C5b C6b . . 1.55(9) O1c C1c . . 1.28(4) O2c C1c . . 1.25(3) C1c C2c . . 1.58(4) C2c C3c . . 1.44(6) C3c C4c . . 1.67(7) C4c C5c . . 1.15(10) C5c C6c . . 1.57(13) O1d C1d . . 1.27(3) O2d C1d . . 1.24(3) C1d C2d . . 1.53(3) C2d C3d . . 1.48(3) C3d C4d . . 1.67(5) C4d C5d . . 1.53(5) C5d C6d . . 1.53(8) O1e C2e . . 1.45(3) O1e C3e . . 1.41(3) O2e C4e . . 1.49(3) O2e C5e . . 1.46(4) O3e C8e . . 1.49(3) O3e C9e . . 1.44(3) O4e C10e . . 1.44(3) O4e C11e . . 1.41(4) N1e C1e . . 1.53(3) N1e C12e . . 1.53(3) N2e C6e . . 1.49(3) N2e C7e . . 1.56(3) C1e C2e . . 1.45(4) C3e C4e . . 1.50(3) C5e C6e . . 1.52(3) C7e C8e . . 1.53(4) C9e C10e . . 1.51(4) C11e C12e . . 1.50(3) O1f C1f . . 1.29(3) O2f C1f . . 1.19(3) C1f C2f . . 1.53(4) C2f C3f . . 1.60(4) C3f C4f . . 1.55(5) C4f C5f . . 1.53(5) C5f C6f . . 1.42(9) O1g C1g . . 1.29(3) O2g C1g . . 1.20(4) C1g C2g . . 1.50(3) C2g C3g . . 1.46(5) C3g C4g . . 1.57(7) C4g C5g . . 1.34(11) C5g C6g . . 1.51(12) O1h C1h . . 1.24(3) O2h C1h . . 1.27(4) C1h C2h . . 1.51(4) C2h C3h . . 1.60(3) C3h C4h . . 1.61(5) C4h C5h . . 1.55(4) C5h C6h . . 1.51(7) O1i C1i . . 1.29(4) O2i C1i . . 1.18(3) C1i C2i . . 1.67(4) C2i C3i . . 1.31(7) C3i C4i . . 1.56(5) C4i C5i . . 1.48(6) C5i C6i . . 1.57(5) O1j C1j . . 1.22(3) O2j C1j . . 1.25(3) C1j C2j . . 1.51(4) C2j C3j . . 1.42(4) C3j C4j . . 1.42(6) C4j C5j . . 1.48(9) C5j C6j . . 1.66(8) O1k C1k . . 1.29(3) O2k C1k . 1_655 1.23(3) C1k C2k . . 1.51(4) C2k C3k . . 1.54(4) C3k C4k . . 1.53(6) C4k C5k . . 1.49(5) C5k C6k . . 1.54(10) 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 N1a Cu1 O1b . . . 93.0(8) N1a Cu1 N1a . . 2_676 180.0(9) N1a Cu1 O1b . . 2_676 87.0(8) O1b Cu1 N1a . . 2_676 87.0(8) O1b Cu1 O1b . . 2_676 180.0(6) N1a Cu1 O1b 2_676 . 2_676 93.0(8) O1c Cu2 O1d . . . 91.5(7) O1c Cu2 O2c . . 2_776 169.1(7) O1c Cu2 O2d . . 2_776 90.0(7) O1d Cu2 O2c . . 2_776 88.3(7) O1d Cu2 O2d . . 2_776 169.2(6) O2c Cu2 O2d 2_776 . 2_776 88.1(7) N1e Cu3 N2e . . . 178.2(8) N1e Cu3 O1f . . . 89.5(7) N1e Cu3 O1k . . . 90.2(7) N2e Cu3 O1f . . . 92.2(7) N2e Cu3 O1k . . . 88.1(7) O1f Cu3 O1k . . . 175.2(5) O1g Cu4 O1h . . . 89.3(7) O1g Cu4 O1i . . . 167.2(7) O1g Cu4 O1j . . . 89.2(7) O1h Cu4 O1i . . . 89.7(7) O1h Cu4 O1j . . . 168.2(6) O1i Cu4 O1j . . . 89.2(7) O2g Cu5 O2h . . . 87.8(7) O2g Cu5 O2i . . . 169.5(7) O2g Cu5 O2j . . . 89.4(7) O2h Cu5 O2i . . . 89.0(7) O2h Cu5 O2j . . . 168.0(7) O2i Cu5 O2j . . . 91.7(7) C2a O1a C3a . . . 117(3) C5a O2a C6a . . . 125(5) Cu1 N1a C1a . . . 118.1(16) Cu1 N1a C6a . . 2_676 117(3) C1a N1a C6a . . 2_676 97(3) N1a C1a C2a . . . 106(3) O1a C2a C1a . . . 118(4) O1a C3a C4a . . . 108(5) C3a C4a C5a . . . 117(6) O2a C5a C4a . . . 124(7) O2a C6a N1a . . 2_676 104(3) Cu1 O1b C1b . . . 132.7(13) O1b C1b O2b . . . 125(3) O1b C1b C2b . . . 115.2(18) O2b C1b C2b . . . 120(3) C1b C2b C3b . . . 109(3) C2b C3b C4b . . . 113(4) C3b C4b C5b . . . 110(5) C4b C5b C6b . . . 109(5) Cu2 O1c C1c . . . 123.3(14) C1c O2c Cu2 . . 2_776 122.1(18) O1c C1c O2c . . . 125(3) O1c C1c C2c . . . 114(3) O2c C1c C2c . . . 121(3) C1c C2c C3c . . . 112(3) C2c C3c C4c . . . 102(4) C3c C4c C5c . . . 95(5) C4c C5c C6c . . . 120(7) Cu2 O1d C1d . . . 123.3(11) C1d O2d Cu2 . . 2_776 118.6(15) O1d C1d O2d . . . 128.3(18) O1d C1d C2d . . . 113.7(18) O2d C1d C2d . . . 118(3) C1d C2d C3d . . . 114(2) C2d C3d C4d . . . 113(3) C3d C4d C5d . . . 107(3) C4d C5d C6d . . . 111(4) C2e O1e C3e . . . 113.4(18) C4e O2e C5e . . . 114.0(17) C8e O3e C9e . . . 113.0(18) C10e O4e C11e . . . 115.4(18) Cu3 N1e C1e . . . 109.0(10) Cu3 N1e C12e . . . 118.3(13) C1e N1e C12e . . . 108.5(16) Cu3 N2e C6e . . . 118.8(12) Cu3 N2e C7e . . . 107.5(9) C6e N2e C7e . . . 112.0(16) N1e C1e C2e . . . 110.3(18) O1e C2e C1e . . . 108(2) O1e C3e C4e . . . 112(3) O2e C4e C3e . . . 111.1(16) O2e C5e C6e . . . 106.1(19) N2e C6e C5e . . . 109.9(18) N2e C7e C8e . . . 110.1(16) O3e C8e C7e . . . 106.0(19) O3e C9e C10e . . . 109(3) O4e C10e C9e . . . 109.4(16) O4e C11e C12e . . . 110(2) N1e C12e C11e . . . 108.5(18) Cu3 O1f C1f . . . 133.8(13) O1f C1f O2f . . . 124(3) O1f C1f C2f . . . 117.6(17) O2f C1f C2f . . . 118(3) C1f C2f C3f . . . 116(3) C2f C3f C4f . . . 109(3) C3f C4f C5f . . . 108(3) C4f C5f C6f . . . 111(4) Cu4 O1g C1g . . . 125.4(15) Cu5 O2g C1g . . . 121.2(13) O1g C1g O2g . . . 125.1(19) O1g C1g C2g . . . 113(3) O2g C1g C2g . . . 121(2) C1g C2g C3g . . . 112(3) C2g C3g C4g . . . 112(3) C3g C4g C5g . . . 121(5) C4g C5g C6g . . . 111(6) Cu4 O1h C1h . . . 122.2(17) Cu5 O2h C1h . . . 121.7(14) O1h C1h O2h . . . 127(3) O1h C1h C2h . . . 116(3) O2h C1h C2h . . . 116.8(19) C1h C2h C3h . . . 113(2) C2h C3h C4h . . . 108(2) C3h C4h C5h . . . 107(3) C4h C5h C6h . . . 103(4) Cu4 O1i C1i . . . 118.6(12) Cu5 O2i C1i . . . 121.8(16) O1i C1i O2i . . . 130(2) O1i C1i C2i . . . 116(2) O2i C1i C2i . . . 114(3) C1i C2i C3i . . . 110(3) C2i C3i C4i . . . 114(4) C3i C4i C5i . . . 109(3) C4i C5i C6i . . . 109(3) Cu4 O1j C1j . . . 126.1(14) Cu5 O2j C1j . . . 123.3(17) O1j C1j O2j . . . 123(3) O1j C1j C2j . . . 121(2) O2j C1j C2j . . . 116(3) C1j C2j C3j . . . 113(3) C2j C3j C4j . . . 110(3) C3j C4j C5j . . . 112(5) C4j C5j C6j . . . 123(5) Cu3 O1k C1k . . . 131.0(13) O1k C1k C2k . . . 117.7(17) O1k C1k O2k . . 1_455 124(3) C2k C1k O2k . . 1_455 118(3) C1k C2k C3k . . . 114(3) C2k C3k C4k . . . 104(3) C3k C4k C5k . . . 109(4) C4k C5k C6k . . . 109(5) #=END========================================================