Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data__Cu-dimer _database_code_CSD 168237 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Aratani, Naoki' 'Furuta, Hiroyuki' 'Nakano, Aiko' 'Osuka, Atsuhiro' _publ_contact_author_name 'Prof Atsuhiro Osuka' _publ_contact_author_address ; Department of Chemistry Kyoto University Graduate School of Science Sakyo-ku Kyoto 606-8502 JAPAN ; _publ_contact_author_email 'OSUKA@KUCHEM.KYOTO-U.AC.JP' _publ_section_title ; Directly linked dehydropurpurin - porphyrin dyads from Ag(I)-promoted oxidation of meso-phenylethynyl substituted zinc(II)-porphyrins ; #============================================================================== _audit_creation_date '2000-11-18' _audit_creation_method 'by teXsan for Windows v1.06' _audit_update_record ; ? ; #============================================================================== # SUBMISSION DETAILS _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1997-1999). teXsan for Windows. Single Crystal Structure Analysis Software. Version 1.06. MSC, 9009 New Trails Drive, The Woodlands, TX 77381, USA. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1994). J. Appl. Cryst., 26, 343. ; #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _computing_structure_refinement 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 13.204(1) _cell_length_b 24.665(1) _cell_length_c 11.0879(9) _cell_angle_alpha 99.737(2) _cell_angle_beta 106.210(3) _cell_angle_gamma 83.472(5) _cell_volume 3409.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 15197 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 27.4 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'prism' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1394.64 _chemical_formula_analytical ? _chemical_formula_sum 'C91 H62 Cu2 N8 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1444.00 _exptl_absorpt_coefficient_mu 0.681 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_max 1.165 _exptl_absorpt_correction_T_min 0.821 _exptl_special_details ; ? ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device 'Rigaku RAXIS-RAPID' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h ? _diffrn_standard_refln_index_k ? _diffrn_standard_refln_index_l ? _diffrn_reflns_number 14748 _reflns_number_total 14748 _reflns_number_gt 8332 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.04204 _diffrn_reflns_av_sigmaI/netI 0.056 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 0.84 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.07573 _diffrn_orient_matrix_UB_12 0.00096 _diffrn_orient_matrix_UB_13 0.00094 _diffrn_orient_matrix_UB_21 -0.00313 _diffrn_orient_matrix_UB_22 0.04049 _diffrn_orient_matrix_UB_23 0.03110 _diffrn_orient_matrix_UB_31 0.02251 _diffrn_orient_matrix_UB_32 -0.00777 _diffrn_orient_matrix_UB_33 0.08967 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 182 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 124 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 16 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cu 0 4 0.263 1.266 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Cu(1) 0.97355(8) 0.08828(4) 0.4428(1) 0.0435(3) 1.000 . Uani d ? Cu(2) 0.57639(8) 0.40937(4) 0.3421(1) 0.0418(3) 1.000 . Uani d ? N(1) 0.9624(5) 0.1579(3) 0.5612(7) 0.046(2) 1.000 . Uani d ? N(2) 1.1193(5) 0.0721(3) 0.5521(7) 0.047(2) 1.000 . Uani d ? N(3) 0.9864(5) 0.0196(3) 0.3218(7) 0.046(2) 1.000 . Uani d ? N(4) 0.8284(5) 0.1052(3) 0.3311(7) 0.043(2) 1.000 . Uani d ? N(5) 0.5333(5) 0.3603(3) 0.4349(6) 0.041(2) 1.000 . Uani d ? N(6) 0.4445(5) 0.4575(3) 0.3548(6) 0.041(2) 1.000 . Uani d ? N(7) 0.6143(5) 0.4573(3) 0.2398(7) 0.046(2) 1.000 . Uani d ? N(8) 0.7073(5) 0.3570(3) 0.3282(7) 0.044(2) 1.000 . Uani d ? C(1) 0.8723(6) 0.1930(3) 0.5584(8) 0.045(2) 1.000 . Uani d ? C(2) 0.8947(7) 0.2375(4) 0.660(1) 0.060(3) 1.000 . Uani d ? C(3) 0.9966(8) 0.2297(4) 0.726(1) 0.065(3) 1.000 . Uani d ? C(4) 1.0382(7) 0.1802(4) 0.6641(9) 0.053(3) 1.000 . Uani d ? C(5) 1.1421(7) 0.1570(4) 0.7085(9) 0.056(3) 1.000 . Uani d ? C(6) 1.1774(7) 0.1057(4) 0.655(1) 0.056(3) 1.000 . Uani d ? C(7) 1.2796(7) 0.0782(5) 0.703(1) 0.068(3) 1.000 . Uani d ? C(8) 1.2810(7) 0.0279(4) 0.631(1) 0.070(3) 1.000 . Uani d ? C(9) 1.1821(7) 0.0244(4) 0.5362(9) 0.054(3) 1.000 . Uani d ? C(10) 1.1555(7) -0.0194(4) 0.443(1) 0.055(3) 1.000 . Uani d ? C(11) 1.0657(7) -0.0218(3) 0.3414(9) 0.051(3) 1.000 . Uani d ? C(12) 1.0449(7) -0.0662(4) 0.239(1) 0.058(3) 1.000 . Uani d ? C(13) 0.9546(7) -0.0523(4) 0.1565(9) 0.057(3) 1.000 . Uani d ? C(14) 0.9181(7) 0.0018(3) 0.2092(9) 0.050(3) 1.000 . Uani d ? C(15) 0.8215(7) 0.0299(3) 0.1524(9) 0.049(3) 1.000 . Uani d ? C(16) 0.7810(6) 0.0783(3) 0.2143(9) 0.048(2) 1.000 . Uani d ? C(17) 0.6799(7) 0.1063(4) 0.1632(9) 0.056(3) 1.000 . Uani d ? C(18) 0.6658(7) 0.1485(4) 0.2537(9) 0.053(3) 1.000 . Uani d ? C(19) 0.7574(6) 0.1485(3) 0.3578(8) 0.045(2) 1.000 . Uani d ? C(20) 0.7755(6) 0.1875(3) 0.4657(8) 0.043(2) 1.000 . Uani d ? C(21) 1.2137(7) 0.1879(4) 0.822(1) 0.063(3) 1.000 . Uani d ? C(22) 1.2470(8) 0.2395(4) 0.818(1) 0.072(4) 1.000 . Uani d ? C(23) 1.3076(9) 0.2691(5) 0.925(1) 0.084(4) 1.000 . Uani d ? C(24) 1.3362(9) 0.2502(6) 1.040(1) 0.086(4) 1.000 . Uani d ? C(25) 1.307(1) 0.1992(6) 1.045(1) 0.094(5) 1.000 . Uani d ? C(26) 1.2462(9) 0.1683(5) 0.938(1) 0.081(4) 1.000 . Uani d ? C(27) 1.395(1) 0.2846(7) 1.158(1) 0.123(6) 1.000 . Uani d ? C(28) 0.7591(7) 0.0045(4) 0.0251(9) 0.053(3) 1.000 . Uani d ? C(29) 0.6606(8) -0.0158(4) 0.007(1) 0.062(3) 1.000 . Uani d ? C(30) 0.6062(8) -0.0418(5) -0.110(1) 0.074(4) 1.000 . Uani d ? C(31) 0.649(1) -0.0489(5) -0.213(1) 0.078(4) 1.000 . Uani d ? C(32) 0.746(1) -0.0293(5) -0.195(1) 0.077(4) 1.000 . Uani d ? C(33) 0.7997(8) -0.0029(4) -0.079(1) 0.065(3) 1.000 . Uani d ? C(34) 0.589(1) -0.0775(7) -0.340(1) 0.134(7) 1.000 . Uani d ? C(35) 0.6875(6) 0.2306(3) 0.4793(8) 0.044(2) 1.000 . Uani d ? C(36) 0.6057(6) 0.2270(3) 0.5314(8) 0.043(2) 1.000 . Uani d ? C(37) 0.5853(6) 0.1848(3) 0.5967(9) 0.050(3) 1.000 . Uani d ? C(38) 0.5157(9) 0.1963(5) 0.673(1) 0.092(5) 1.000 . Uani d ? C(39) 0.500(1) 0.1587(5) 0.745(2) 0.113(6) 1.000 . Uani d ? C(40) 0.5519(9) 0.1071(5) 0.739(1) 0.089(5) 1.000 . Uani d ? C(41) 0.619(1) 0.0943(5) 0.666(1) 0.097(5) 1.000 . Uani d ? C(42) 0.6361(9) 0.1329(4) 0.595(1) 0.085(4) 1.000 . Uani d ? C(43) 0.5870(6) 0.3120(3) 0.4576(8) 0.040(2) 1.000 . Uani d ? C(44) 0.5374(6) 0.2793(3) 0.5160(8) 0.042(2) 1.000 . Uani d ? C(45) 0.4472(6) 0.3092(3) 0.5300(8) 0.044(2) 1.000 . Uani d ? C(46) 0.4446(6) 0.3609(3) 0.4799(8) 0.039(2) 1.000 . Uani d ? C(47) 0.3671(6) 0.4039(3) 0.4733(8) 0.043(2) 1.000 . Uani d ? C(48) 0.3716(6) 0.4511(3) 0.4191(8) 0.044(2) 1.000 . Uani d ? C(49) 0.2996(6) 0.4992(3) 0.4197(9) 0.050(3) 1.000 . Uani d ? C(50) 0.3285(7) 0.5342(3) 0.3550(9) 0.052(3) 1.000 . Uani d ? C(51) 0.4168(6) 0.5078(3) 0.3127(8) 0.045(2) 1.000 . Uani d ? C(52) 0.4664(6) 0.5289(3) 0.2369(8) 0.045(2) 1.000 . Uani d ? C(53) 0.5545(6) 0.5035(3) 0.1977(8) 0.047(2) 1.000 . Uani d ? C(54) 0.6006(7) 0.5240(4) 0.1118(8) 0.052(3) 1.000 . Uani d ? C(55) 0.6883(7) 0.4915(4) 0.1067(9) 0.054(3) 1.000 . Uani d ? C(56) 0.6985(7) 0.4503(4) 0.1878(8) 0.049(3) 1.000 . Uani d ? C(57) 0.7833(6) 0.4101(3) 0.2100(8) 0.048(3) 1.000 . Uani d ? C(58) 0.7855(6) 0.3667(3) 0.2741(9) 0.048(3) 1.000 . Uani d ? C(59) 0.8670(7) 0.3223(4) 0.289(1) 0.059(3) 1.000 . Uani d ? C(60) 0.8378(7) 0.2852(4) 0.347(1) 0.059(3) 1.000 . Uani d ? C(61) 0.7384(6) 0.3069(3) 0.3727(8) 0.047(2) 1.000 . Uani d ? C(62) 0.6782(6) 0.2843(3) 0.4311(8) 0.041(2) 1.000 . Uani d ? C(63) 0.2735(6) 0.3996(3) 0.5210(8) 0.042(2) 1.000 . Uani d ? C(64) 0.1714(7) 0.4050(4) 0.4420(9) 0.058(3) 1.000 . Uani d ? C(65) 0.0845(7) 0.4004(4) 0.486(1) 0.068(3) 1.000 . Uani d ? C(66) 0.0955(8) 0.3883(4) 0.605(1) 0.062(3) 1.000 . Uani d ? C(67) 0.1960(8) 0.3827(4) 0.6824(9) 0.061(3) 1.000 . Uani d ? C(68) 0.2837(7) 0.3881(4) 0.6410(9) 0.054(3) 1.000 . Uani d ? C(69) -0.0014(9) 0.3819(5) 0.649(1) 0.092(5) 1.000 . Uani d ? C(70) 0.4251(7) 0.5800(4) 0.1923(9) 0.052(3) 1.000 . Uani d ? C(71) 0.3966(7) 0.6225(4) 0.1530(9) 0.056(3) 1.000 . Uani d ? C(72) 0.3611(7) 0.6740(4) 0.1048(9) 0.054(3) 1.000 . Uani d ? C(73) 0.2921(9) 0.7108(4) 0.154(1) 0.072(4) 1.000 . Uani d ? C(74) 0.255(1) 0.7596(5) 0.107(1) 0.088(4) 1.000 . Uani d ? C(75) 0.288(1) 0.7721(5) 0.010(1) 0.094(5) 1.000 . Uani d ? C(76) 0.356(1) 0.7362(6) -0.041(1) 0.096(5) 1.000 . Uani d ? C(77) 0.3936(9) 0.6867(5) 0.006(1) 0.078(4) 1.000 . Uani d ? C(78) 0.8763(7) 0.4156(4) 0.1606(9) 0.053(3) 1.000 . Uani d ? C(79) 0.9350(7) 0.4616(4) 0.208(1) 0.059(3) 1.000 . Uani d ? C(80) 1.0240(8) 0.4660(4) 0.167(1) 0.068(3) 1.000 . Uani d ? C(81) 1.0572(8) 0.4257(5) 0.082(1) 0.071(4) 1.000 . Uani d ? C(82) 0.997(1) 0.3805(5) 0.034(1) 0.081(4) 1.000 . Uani d ? C(83) 0.9073(8) 0.3756(4) 0.072(1) 0.072(4) 1.000 . Uani d ? C(84) 1.158(1) 0.4297(6) 0.046(1) 0.105(5) 1.000 . Uani d ? C(85) 0.0950(8) 0.1613(4) 0.2892(9) 0.159(7) 1.000 G Uiso d ? C(86) 0.0271(7) 0.1428(3) 0.172(1) 0.159(6) 1.000 G Uiso d ? C(87) -0.0016(6) 0.1763(5) 0.0764(7) 0.159 1.000 G Uiso d ? C(88) 0.0376(8) 0.2283(4) 0.0984(9) 0.159 1.000 G Uiso d ? C(89) 0.1056(8) 0.2468(3) 0.216(1) 0.159(7) 1.000 G Uiso d ? C(90) 0.1343(6) 0.2133(5) 0.3112(7) 0.159(6) 1.000 G Uiso d ? C(91) 0.196(2) 0.232(1) 0.425(3) 0.237(6) 1.000 . Uiso d ? H(1) 0.8465 0.2673 0.6786 0.072 1.000 . Uiso c ? H(2) 1.0335 0.2527 0.7986 0.078 1.000 . Uiso c ? H(3) 1.3353 0.0926 0.7720 0.082 1.000 . Uiso c ? H(4) 1.3374 -0.0000 0.6416 0.083 1.000 . Uiso c ? H(5) 1.2034 -0.0513 0.4475 0.066 1.000 . Uiso c ? H(6) 1.0877 -0.0996 0.2311 0.070 1.000 . Uiso c ? H(7) 0.9209 -0.0736 0.0787 0.068 1.000 . Uiso c ? H(8) 0.6325 0.0969 0.0820 0.067 1.000 . Uiso c ? H(9) 0.6053 0.1737 0.2484 0.063 1.000 . Uiso c ? H(10) 1.2275 0.2541 0.7404 0.087 1.000 . Uiso c ? H(11) 1.3300 0.3037 0.9193 0.100 1.000 . Uiso c ? H(12) 1.3293 0.1847 1.1232 0.113 1.000 . Uiso c ? H(13) 1.2266 0.1332 0.9447 0.097 1.000 . Uiso c ? H(14) 1.3791 0.2745 1.2296 0.147 1.000 . Uiso c ? H(15) 1.4685 0.2788 1.1666 0.147 1.000 . Uiso c ? H(16) 1.3734 0.3225 1.1533 0.147 1.000 . Uiso c ? H(17) 0.6303 -0.0116 0.0767 0.075 1.000 . Uiso c ? H(18) 0.5391 -0.0550 -0.1196 0.089 1.000 . Uiso c ? H(19) 0.7764 -0.0341 -0.2647 0.092 1.000 . Uiso c ? H(20) 0.8664 0.0105 -0.0709 0.079 1.000 . Uiso c ? H(21) 0.5410 -0.1008 -0.3275 0.160 1.000 . Uiso c ? H(22) 0.5520 -0.0514 -0.3918 0.160 1.000 . Uiso c ? H(23) 0.6382 -0.0999 -0.3796 0.160 1.000 . Uiso c ? H(24) 0.4773 0.2313 0.6757 0.111 1.000 . Uiso c ? H(25) 0.4537 0.1686 0.7981 0.135 1.000 . Uiso c ? H(26) 0.5399 0.0808 0.7861 0.107 1.000 . Uiso c ? H(27) 0.6560 0.0589 0.6628 0.116 1.000 . Uiso c ? H(28) 0.6842 0.1227 0.5442 0.103 1.000 . Uiso c ? H(29) 0.3959 0.2987 0.5653 0.053 1.000 . Uiso c ? H(30) 0.2426 0.5053 0.4581 0.060 1.000 . Uiso c ? H(31) 0.2958 0.5697 0.3405 0.062 1.000 . Uiso c ? H(32) 0.5739 0.5546 0.0675 0.062 1.000 . Uiso c ? H(33) 0.7355 0.4950 0.0580 0.065 1.000 . Uiso c ? H(34) 0.9302 0.3197 0.2628 0.070 1.000 . Uiso c ? H(35) 0.8753 0.2512 0.3667 0.070 1.000 . Uiso c ? H(36) 0.1613 0.4119 0.3576 0.070 1.000 . Uiso c ? H(37) 0.0155 0.4057 0.4312 0.081 1.000 . Uiso c ? H(38) 0.2058 0.3749 0.7660 0.073 1.000 . Uiso c ? H(39) 0.3523 0.3838 0.6969 0.065 1.000 . Uiso c ? H(40) 0.0183 0.3838 0.7392 0.110 1.000 . Uiso c ? H(41) -0.0538 0.4105 0.6252 0.110 1.000 . Uiso c ? H(42) -0.0286 0.3472 0.6117 0.110 1.000 . Uiso c ? H(43) 0.2691 0.7024 0.2227 0.087 1.000 . Uiso c ? H(44) 0.2069 0.7844 0.1417 0.106 1.000 . Uiso c ? H(45) 0.2637 0.8060 -0.0217 0.113 1.000 . Uiso c ? H(46) 0.3786 0.7449 -0.1091 0.115 1.000 . Uiso c ? H(47) 0.4414 0.6619 -0.0302 0.094 1.000 . Uiso c ? H(48) 0.9147 0.4899 0.2680 0.071 1.000 . Uiso c ? H(49) 1.0627 0.4979 0.1979 0.082 1.000 . Uiso c ? H(50) 1.0176 0.3524 -0.0261 0.097 1.000 . Uiso c ? H(51) 0.8669 0.3444 0.0375 0.086 1.000 . Uiso c ? H(52) 1.2161 0.4311 0.1200 0.126 1.000 . Uiso c ? H(53) 1.1691 0.3981 -0.0124 0.126 1.000 . Uiso c ? H(54) 1.1527 0.4619 0.0082 0.126 1.000 . Uiso c ? H(55) 0.1150 0.1387 0.3547 0.191 1.000 . Uiso c ? H(56) 0.0008 0.1074 0.1577 0.191 1.000 . Uiso c ? H(57) -0.0479 0.1635 -0.0032 0.191 1.000 . Uiso c ? H(58) 0.0177 0.2509 0.0331 0.191 1.000 . Uiso c ? H(59) 0.1319 0.2822 0.2301 0.191 1.000 . Uiso c ? H(60) 0.1647 0.2206 0.4887 0.280 1.000 . Uiso c ? H(61) 0.2636 0.2107 0.4361 0.280 1.000 . Uiso c ? H(62) 0.2014 0.2680 0.4386 0.280 1.000 . Uiso c ? 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(1) 0.0353(5) 0.0386(5) 0.0595(7) 0.0030(4) 0.0179(5) 0.0095(5) Cu(2) 0.0385(5) 0.0391(5) 0.0504(6) 0.0004(4) 0.0161(5) 0.0087(5) N(1) 0.037(4) 0.041(4) 0.061(5) 0.002(3) 0.015(3) 0.007(3) N(2) 0.040(4) 0.044(4) 0.061(5) 0.005(3) 0.018(3) 0.013(4) N(3) 0.039(4) 0.041(4) 0.063(5) -0.002(3) 0.021(4) 0.005(3) N(4) 0.039(4) 0.036(4) 0.056(5) 0.004(3) 0.015(3) 0.010(3) N(5) 0.035(3) 0.038(4) 0.053(4) 0.002(3) 0.018(3) 0.008(3) N(6) 0.040(4) 0.033(3) 0.051(4) 0.004(3) 0.013(3) 0.008(3) N(7) 0.046(4) 0.044(4) 0.052(4) 0.001(3) 0.018(3) 0.012(3) N(8) 0.041(4) 0.039(4) 0.059(5) 0.006(3) 0.022(3) 0.014(3) C(1) 0.041(4) 0.041(5) 0.058(5) 0.003(4) 0.019(4) 0.010(4) C(2) 0.051(6) 0.054(6) 0.071(7) 0.004(4) 0.017(5) -0.000(5) C(3) 0.054(6) 0.056(6) 0.075(7) 0.001(5) 0.014(5) -0.005(5) C(4) 0.046(5) 0.049(5) 0.063(6) -0.001(4) 0.013(5) 0.010(5) C(5) 0.042(5) 0.055(6) 0.071(7) -0.002(4) 0.013(5) 0.017(5) C(6) 0.039(5) 0.058(6) 0.072(7) 0.001(4) 0.015(5) 0.018(5) C(7) 0.037(5) 0.076(7) 0.086(8) 0.003(5) 0.006(5) 0.018(6) C(8) 0.045(5) 0.074(7) 0.088(8) 0.018(5) 0.018(5) 0.020(6) C(9) 0.039(5) 0.060(6) 0.071(6) 0.008(4) 0.025(5) 0.021(5) C(10) 0.047(5) 0.048(5) 0.077(7) 0.013(4) 0.030(5) 0.020(5) C(11) 0.050(5) 0.043(5) 0.072(6) 0.005(4) 0.034(5) 0.012(4) C(12) 0.056(6) 0.045(5) 0.083(7) 0.005(4) 0.036(5) 0.008(5) C(13) 0.054(6) 0.048(5) 0.072(7) -0.001(4) 0.029(5) 0.001(5) C(14) 0.049(5) 0.038(4) 0.072(6) 0.001(4) 0.034(5) 0.010(4) C(15) 0.046(5) 0.043(5) 0.063(6) -0.003(4) 0.022(4) 0.009(4) C(16) 0.039(4) 0.046(5) 0.060(6) -0.002(4) 0.015(4) 0.010(4) C(17) 0.052(5) 0.049(5) 0.062(6) 0.002(4) 0.009(5) 0.011(5) C(18) 0.047(5) 0.044(5) 0.064(6) 0.005(4) 0.013(4) 0.010(4) C(19) 0.039(4) 0.042(5) 0.060(6) 0.000(4) 0.018(4) 0.012(4) C(20) 0.040(4) 0.035(4) 0.060(5) 0.005(3) 0.021(4) 0.016(4) C(21) 0.040(5) 0.064(6) 0.076(7) 0.003(4) 0.007(5) 0.005(5) C(22) 0.065(7) 0.063(7) 0.084(8) -0.005(5) 0.010(6) 0.009(6) C(23) 0.075(8) 0.080(8) 0.084(9) -0.020(6) 0.006(7) -0.004(7) C(24) 0.062(7) 0.11(1) 0.077(9) -0.010(7) 0.004(6) -0.006(8) C(25) 0.073(8) 0.12(1) 0.074(8) -0.008(8) 0.002(7) 0.016(8) C(26) 0.066(7) 0.088(8) 0.084(8) -0.011(6) 0.005(6) 0.020(7) C(27) 0.11(1) 0.15(1) 0.09(1) -0.03(1) 0.005(8) -0.03(1) C(28) 0.050(5) 0.047(5) 0.062(6) -0.003(4) 0.015(5) 0.005(4) C(29) 0.060(6) 0.056(6) 0.074(7) -0.004(5) 0.022(5) 0.006(5) C(30) 0.058(6) 0.072(7) 0.085(8) -0.013(5) 0.007(6) 0.009(6) C(31) 0.089(9) 0.069(7) 0.064(7) -0.007(6) 0.004(6) 0.004(6) C(32) 0.098(9) 0.079(8) 0.060(7) -0.007(7) 0.031(6) 0.010(6) C(33) 0.071(7) 0.071(7) 0.063(7) -0.015(5) 0.026(5) 0.012(5) C(34) 0.14(1) 0.15(1) 0.09(1) -0.04(1) -0.01(1) -0.01(1) C(35) 0.037(4) 0.041(4) 0.057(5) 0.002(3) 0.017(4) 0.007(4) C(36) 0.038(4) 0.037(4) 0.057(5) 0.003(3) 0.014(4) 0.011(4) C(37) 0.041(5) 0.045(5) 0.068(6) 0.003(4) 0.021(4) 0.014(4) C(38) 0.085(8) 0.064(7) 0.16(1) 0.020(6) 0.077(9) 0.053(8) C(39) 0.10(1) 0.087(9) 0.19(2) 0.013(8) 0.10(1) 0.06(1) C(40) 0.083(8) 0.068(7) 0.14(1) 0.014(6) 0.063(8) 0.055(8) C(41) 0.096(9) 0.074(8) 0.15(1) 0.031(7) 0.075(9) 0.061(8) C(42) 0.084(8) 0.067(7) 0.14(1) 0.032(6) 0.075(8) 0.053(7) C(43) 0.036(4) 0.037(4) 0.047(5) 0.000(3) 0.013(4) 0.006(4) C(44) 0.038(4) 0.041(4) 0.049(5) 0.001(3) 0.016(4) 0.006(4) C(45) 0.041(4) 0.043(5) 0.057(5) -0.002(4) 0.024(4) 0.010(4) C(46) 0.033(4) 0.039(4) 0.047(5) 0.002(3) 0.013(4) 0.007(4) C(47) 0.036(4) 0.041(4) 0.051(5) 0.002(3) 0.012(4) 0.006(4) C(48) 0.035(4) 0.045(5) 0.052(5) 0.001(3) 0.012(4) 0.009(4) C(49) 0.041(5) 0.046(5) 0.065(6) 0.007(4) 0.020(4) 0.010(4) C(50) 0.048(5) 0.039(5) 0.068(6) 0.006(4) 0.017(5) 0.010(4) C(51) 0.041(5) 0.041(5) 0.051(5) -0.001(4) 0.009(4) 0.003(4) C(52) 0.047(5) 0.038(4) 0.048(5) 0.001(4) 0.009(4) 0.011(4) C(53) 0.046(5) 0.044(5) 0.048(5) -0.004(4) 0.009(4) 0.009(4) C(54) 0.058(6) 0.051(5) 0.050(5) -0.004(4) 0.015(4) 0.015(4) C(55) 0.055(5) 0.058(6) 0.055(6) -0.010(4) 0.020(5) 0.013(5) C(56) 0.051(5) 0.050(5) 0.052(5) -0.007(4) 0.021(4) 0.008(4) C(57) 0.045(5) 0.048(5) 0.059(6) -0.005(4) 0.025(4) 0.010(4) C(58) 0.042(5) 0.047(5) 0.060(6) -0.005(4) 0.023(4) 0.006(4) C(59) 0.048(5) 0.054(5) 0.086(7) 0.007(4) 0.036(5) 0.017(5) C(60) 0.048(5) 0.050(5) 0.087(7) 0.012(4) 0.035(5) 0.016(5) C(61) 0.041(5) 0.045(5) 0.058(6) -0.001(4) 0.021(4) 0.005(4) C(62) 0.039(4) 0.032(4) 0.057(5) 0.002(3) 0.018(4) 0.012(4) C(63) 0.035(4) 0.041(4) 0.053(5) 0.005(3) 0.018(4) 0.010(4) C(64) 0.043(5) 0.068(6) 0.069(6) 0.001(4) 0.015(5) 0.022(5) C(65) 0.039(5) 0.073(7) 0.093(8) 0.003(5) 0.017(5) 0.023(6) C(66) 0.052(6) 0.058(6) 0.084(8) -0.009(5) 0.033(5) 0.006(5) C(67) 0.071(7) 0.062(6) 0.059(6) -0.003(5) 0.030(5) 0.011(5) C(68) 0.042(5) 0.056(5) 0.063(6) 0.001(4) 0.017(4) 0.004(5) C(69) 0.071(7) 0.102(9) 0.12(1) -0.016(7) 0.054(7) 0.007(8) C(70) 0.049(5) 0.052(5) 0.054(6) -0.001(4) 0.015(4) 0.007(4) C(71) 0.055(6) 0.052(6) 0.060(6) 0.002(4) 0.015(5) 0.013(5) C(72) 0.056(5) 0.048(5) 0.058(6) 0.004(4) 0.012(5) 0.017(4) C(73) 0.079(7) 0.061(6) 0.083(8) 0.011(5) 0.030(6) 0.023(6) C(74) 0.087(9) 0.070(8) 0.11(1) 0.024(6) 0.029(8) 0.027(7) C(75) 0.11(1) 0.065(8) 0.11(1) 0.011(7) 0.023(9) 0.042(8) C(76) 0.12(1) 0.089(9) 0.10(1) 0.007(8) 0.042(9) 0.050(8) C(77) 0.087(8) 0.073(7) 0.088(8) 0.007(6) 0.039(7) 0.027(6) C(78) 0.049(5) 0.054(5) 0.067(6) -0.001(4) 0.026(5) 0.020(5) C(79) 0.055(6) 0.056(6) 0.071(7) -0.003(4) 0.023(5) 0.015(5) C(80) 0.057(6) 0.071(7) 0.088(8) -0.010(5) 0.023(6) 0.029(6) C(81) 0.059(6) 0.088(8) 0.084(8) 0.004(6) 0.038(6) 0.036(7) C(82) 0.086(8) 0.093(9) 0.081(8) -0.010(7) 0.053(7) 0.004(7) C(83) 0.069(7) 0.074(7) 0.085(8) -0.011(5) 0.044(6) 0.004(6) C(84) 0.076(8) 0.15(1) 0.12(1) -0.007(8) 0.056(8) 0.05(1) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details unit _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 8332 _refine_ls_number_parameters 858 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_all 0.0660 _refine_ls_wR_factor_ref 0.0660 _refine_ls_goodness_of_fit_all 0.488 _refine_ls_goodness_of_fit_ref 0.490 _refine_ls_shift/su_max 0.0100 _refine_ls_shift/su_mean 0.0001 _refine_diff_density_min -0.55 _refine_diff_density_max 0.75 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag ? ? ? ? ? ? # -- ENTER BONDS HERE, ONE PER LINE -- # e.g. C1 C2 1.541(1) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag # -- ENTER ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 109.4(3) . . . yes ? ? ? ? ? ? ? ? #------------------------------------------------------------------------------ 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 ? ? ? ? ? ? # -- ENTER NON-BONDED CONTACTS HERE, ONE PER LINE -- # e.g. O1 N1 2.841(1) . . yes #------------------------------------------------------------------------------ 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 TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 52.8(1) . . . . yes #------------------------------------------------------------------------------ # End of CIF #==============================================================================