# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Silvio Biali' 'Kasim Agbaria' 'Samah Simaan' 'Iris Thondorf' _publ_contact_author_name 'Prof Silvio Biali' _publ_contact_author_address ; Organic Chemistry The Hebrew University of Jerusalem Givat Ram Jerusalem 91904 IVORY COAST ; _publ_contact_author_email SILVIO@VMS.HUJI.AC.IL _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Conformation of Syn and Anti Phenylquinazoline Calix[4]arene Diethers ; data_[N10]_Silvio_P-1 _database_code_CSD 187174 #------------------------------------------------------------------------------ _audit_creation_date 'Thu Jun 6 11:18:01 2002' _audit_creation_method 'from TEXRAY.INF file' #------------------------------------------------------------------------------ _computing_data_collection 'Philips PW1100 Diffractometer Control' _computing_cell_refinement 'Philips PW1100 Diffractometer Control' _computing_data_reduction teXsan _computing_structure_solution SHELXS86 _computing_structure_refinement teXsan _computing_publication_material teXsan #------------------------------------------------------------------------------ _cell_length_a 14.806(3) _cell_length_b 19.827(4) _cell_length_c 12.186(3) _cell_angle_alpha 92.49(1) _cell_angle_beta 113.65(2) _cell_angle_gamma 81.35(1) _cell_volume 3239(1) _cell_formula_units_Z 2 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 13.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description unknown _exptl_crystal_colour unknown _exptl_crystal_size_max 0.000 _exptl_crystal_size_mid 0.000 _exptl_crystal_size_min 0.000 _exptl_crystal_density_diffrn 1.205 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 1175.76 _chemical_formula_moiety 'C72 H72 N4 O4 C1 H1 Cl3' _exptl_crystal_F_000 1242.00 _exptl_absorpt_coefficient_mu 0.193 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector scintillation _diffrn_measurement_device 'Philips PW1100' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -7 2 3 _diffrn_reflns_number 9024 _reflns_number_total 9024 _reflns_number_observed 5157 _reflns_observed_criterion 2.50 _diffrn_reflns_av_R_equivalents 88.50 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2 _diffrn_reflns_theta_max 23.00 #------------------------------------------------------------------------------ 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 0 146 0.003 0.002 'International Tables' H 0 144 0.000 0.000 'International Tables' N 0 8 0.006 0.003 'International Tables' O 0 8 0.011 0.006 'International Tables' Cl 0 6 0.148 0.159 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type Cl(1) 0.9140(3) 0.5895(2) 0.2918(4) 0.179 Uij Cl(2) 0.7689(3) 0.6498(3) 0.0828(6) 0.328 Uij Cl(3) 0.8856(5) 0.5249(3) 0.0784(5) 0.265 Uij O(1) 0.5339(3) 0.7004(2) 0.3439(4) 0.053 Uij O(2) 0.3994(3) 0.6579(2) 0.5811(4) 0.042 Uij O(3) 0.6082(3) 0.7961(2) 0.6963(4) 0.052 Uij O(4) 0.3658(3) 0.8789(2) 0.3758(4) 0.044 Uij N(1) 0.4222(4) 0.5672(3) 0.7029(5) 0.045 Uij N(2) 0.2877(5) 0.5346(3) 0.7390(6) 0.061 Uij N(3) 0.3246(4) 0.9636(3) 0.2339(5) 0.043 Uij N(4) 0.1546(5) 1.0141(3) 0.1293(6) 0.063 Uij C(1) 0.4320(5) 0.7049(4) 0.2946(6) 0.042 Uij C(2) 0.3807(5) 0.7609(4) 0.2192(6) 0.041 Uij C(3) 0.2776(5) 0.7656(4) 0.1573(6) 0.048 Uij C(4) 0.2248(5) 0.7163(4) 0.1696(6) 0.050 Uij C(5) 0.2789(5) 0.6628(4) 0.2503(6) 0.048 Uij C(6) 0.3821(5) 0.6548(3) 0.3131(6) 0.038 Uij C(7) 0.4341(5) 0.5910(3) 0.3896(6) 0.044 Uij C(8) 0.5002(5) 0.6390(3) 0.5987(6) 0.035 Uij C(9) 0.5190(5) 0.6028(3) 0.5090(6) 0.035 Uij C(10) 0.6182(5) 0.5810(3) 0.5287(6) 0.044 Uij C(11) 0.6966(5) 0.5972(3) 0.6314(7) 0.043 Uij C(12) 0.6721(5) 0.6358(3) 0.7154(6) 0.042 Uij C(13) 0.5752(5) 0.6569(3) 0.7026(6) 0.038 Uij C(14) 0.5533(5) 0.6982(3) 0.7994(6) 0.045 Uij C(15) 0.5169(5) 0.8136(3) 0.7005(6) 0.038 Uij C(16) 0.4876(5) 0.7659(3) 0.7557(6) 0.039 Uij C(17) 0.3991(5) 0.7836(4) 0.7719(6) 0.046 Uij C(18) 0.3386(5) 0.8465(4) 0.7349(6) 0.044 Uij C(19) 0.3692(5) 0.8900(3) 0.6753(6) 0.042 Uij C(20) 0.4570(5) 0.8759(3) 0.6567(5) 0.036 Uij C(21) 0.4856(5) 0.9290(3) 0.5956(6) 0.045 Uij C(22) 0.4672(5) 0.8763(3) 0.3966(6) 0.038 Uij C(23) 0.5266(5) 0.9018(3) 0.5049(6) 0.038 Uij C(24) 0.6271(5) 0.8987(3) 0.5286(6) 0.043 Uij C(25) 0.6694(5) 0.8692(3) 0.4516(7) 0.045 Uij C(26) 0.6054(5) 0.8426(4) 0.3464(7) 0.048 Uij C(27) 0.5033(5) 0.8454(3) 0.3158(6) 0.041 Uij C(28) 0.4374(5) 0.8144(4) 0.2020(6) 0.046 Uij C(29) 0.3631(5) 0.6168(4) 0.6343(6) 0.040 Uij C(30) 0.3814(6) 0.5267(4) 0.7543(6) 0.048 Uij C(31) 0.2262(6) 0.5880(4) 0.6667(7) 0.058 Uij C(32) 0.1250(7) 0.5998(5) 0.6462(10) 0.089 Uij C(33) 0.0627(7) 0.6515(6) 0.572(1) 0.100 Uij C(34) 0.0965(6) 0.6933(5) 0.5153(9) 0.090 Uij C(35) 0.1954(6) 0.6838(4) 0.5325(7) 0.064 Uij C(36) 0.2602(5) 0.6312(4) 0.6090(7) 0.048 Uij C(37) 0.4538(7) 0.4713(4) 0.8343(7) 0.059 Uij C(38) 0.5535(8) 0.4772(4) 0.8879(7) 0.066 Uij C(39) 0.6213(8) 0.4269(6) 0.9623(8) 0.089 Uij C(40) 0.590(1) 0.3696(6) 0.9833(9) 0.105 Uij C(41) 0.493(1) 0.3612(5) 0.931(1) 0.094 Uij C(42) 0.4231(7) 0.4121(5) 0.8546(8) 0.079 Uij C(43) 0.2975(5) 0.9243(4) 0.2955(6) 0.040 Uij C(44) 0.2503(6) 1.0080(4) 0.1527(6) 0.052 Uij C(45) 0.1280(6) 0.9721(5) 0.1939(7) 0.060 Uij C(46) 0.0258(6) 0.9784(5) 0.1728(8) 0.081 Uij C(47) -0.0022(6) 0.9389(6) 0.2386(9) 0.085 Uij C(48) 0.0675(7) 0.8922(5) 0.3272(8) 0.077 Uij C(49) 0.1663(6) 0.8863(4) 0.3475(7) 0.064 Uij C(50) 0.1973(5) 0.9258(4) 0.2812(6) 0.049 Uij C(51) 0.2832(6) 1.0540(4) 0.0868(6) 0.057 Uij C(52) 0.3779(7) 1.0421(4) 0.0900(7) 0.064 Uij C(53) 0.4083(7) 1.0883(6) 0.0316(8) 0.086 Uij C(54) 0.343(1) 1.1443(6) -0.0307(9) 0.105 Uij C(55) 0.2497(10) 1.1536(6) -0.034(1) 0.109 Uij C(56) 0.2191(7) 1.1104(5) 0.0235(9) 0.084 Uij C(57) 0.1133(6) 0.7183(4) 0.0963(8) 0.067 Uij C(58) 0.0631(6) 0.7855(6) 0.0313(9) 0.102 Uij C(59) 0.0596(7) 0.7097(7) 0.176(1) 0.137 Uij C(60) 0.0971(8) 0.6626(7) 0.007(1) 0.205 Uij C(61) 0.8038(5) 0.5713(4) 0.6494(8) 0.058 Uij C(62) 0.8760(6) 0.6110(6) 0.737(1) 0.114 Uij C(63) 0.8260(8) 0.4974(6) 0.676(2) 0.202 Uij C(64) 0.8164(8) 0.5787(8) 0.531(1) 0.151 Uij C(65) 0.2473(5) 0.8668(4) 0.7637(7) 0.054 Uij C(66) 0.1582(7) 0.8903(6) 0.6538(9) 0.107 Uij C(67) 0.2670(7) 0.9226(6) 0.8534(10) 0.114 Uij C(68) 0.2222(8) 0.8082(6) 0.818(1) 0.118 Uij C(69) 0.7818(5) 0.8621(4) 0.4846(8) 0.060 Uij C(70) 0.8131(8) 0.9276(7) 0.497(2) 0.278 Uij C(71) 0.8161(8) 0.821(1) 0.403(2) 0.230 Uij C(72) 0.8388(8) 0.828(1) 0.604(2) 0.243 Uij C(73) 0.8223(8) 0.5735(7) 0.157(1) 0.135 Uij H(1O1) 0.577 0.668 0.407 0.065 Uij H(1O3) 0.644 0.832 0.718 0.063 Uij H(3) 0.242 0.804 0.105 0.057 Uij H(5) 0.244 0.630 0.263 0.057 Uij H(10) 0.633 0.554 0.470 0.053 Uij H(12) 0.725 0.648 0.785 0.050 Uij H(17) 0.379 0.751 0.810 0.055 Uij H(19) 0.328 0.932 0.645 0.051 Uij H(20) 0.219 0.713 0.493 0.077 Uij H(24) 0.669 0.917 0.601 0.052 Uij H(26) 0.632 0.821 0.292 0.058 Uij H(29) 0.214 0.855 0.407 0.077 Uij H(32) 0.100 0.571 0.684 0.107 Uij H(33) -0.006 0.659 0.560 0.120 Uij H(34) 0.051 0.729 0.464 0.108 Uij H(38) 0.576 0.517 0.873 0.079 Uij H(39) 0.690 0.432 0.999 0.107 Uij H(40) 0.637 0.335 1.035 0.127 Uij H(41) 0.472 0.321 0.946 0.114 Uij H(42) 0.355 0.406 0.817 0.095 Uij H(46) -0.022 1.009 0.114 0.098 Uij H(47) -0.071 0.943 0.225 0.102 Uij H(48) 0.046 0.865 0.372 0.092 Uij H(52) 0.423 1.003 0.131 0.077 Uij H(53) 0.474 1.081 0.035 0.103 Uij H(54) 0.363 1.175 -0.071 0.126 Uij H(55) 0.204 1.192 -0.077 0.132 Uij H(56) 0.153 1.119 0.020 0.101 Uij H(71) 0.386 0.572 0.406 0.052 Uij H(72) 0.461 0.560 0.345 0.052 Uij H(141) 0.521 0.672 0.832 0.054 Uij H(142) 0.615 0.707 0.860 0.054 Uij H(211) 0.428 0.961 0.556 0.054 Uij H(212) 0.535 0.951 0.656 0.054 Uij H(281) 0.478 0.794 0.163 0.056 Uij H(282) 0.390 0.850 0.153 0.056 Uij H(581) 0.070 0.821 0.088 0.121 Uij H(582) 0.093 0.795 -0.021 0.121 Uij H(583) -0.006 0.783 -0.014 0.121 Uij H(591) 0.065 0.747 0.229 0.163 Uij H(592) -0.009 0.708 0.129 0.163 Uij H(593) 0.089 0.668 0.222 0.163 Uij H(601) 0.028 0.663 -0.037 0.245 Uij H(602) 0.129 0.669 -0.045 0.245 Uij H(603) 0.125 0.620 0.049 0.245 Uij H(621) 0.941 0.592 0.746 0.138 Uij H(622) 0.862 0.657 0.709 0.138 Uij H(623) 0.871 0.609 0.812 0.138 Uij H(631) 0.817 0.489 0.747 0.242 Uij H(632) 0.782 0.474 0.611 0.242 Uij H(633) 0.893 0.481 0.687 0.242 Uij H(641) 0.883 0.562 0.543 0.181 Uij H(642) 0.773 0.553 0.471 0.181 Uij H(643) 0.801 0.625 0.507 0.181 Uij H(661) 0.171 0.928 0.618 0.128 Uij H(662) 0.144 0.854 0.598 0.128 Uij H(663) 0.103 0.904 0.674 0.128 Uij H(671) 0.325 0.908 0.922 0.137 Uij H(672) 0.276 0.962 0.819 0.137 Uij H(673) 0.212 0.933 0.875 0.137 Uij H(681) 0.166 0.824 0.837 0.141 Uij H(682) 0.207 0.772 0.762 0.141 Uij H(683) 0.278 0.792 0.889 0.141 Uij H(701) 0.884 0.922 0.523 0.333 Uij H(702) 0.782 0.952 0.424 0.333 Uij H(703) 0.795 0.952 0.557 0.333 Uij H(711) 0.799 0.777 0.400 0.277 Uij H(712) 0.785 0.842 0.325 0.277 Uij H(713) 0.886 0.819 0.431 0.277 Uij H(721) 0.820 0.784 0.603 0.290 Uij H(722) 0.908 0.823 0.622 0.290 Uij H(723) 0.825 0.854 0.664 0.290 Uij 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 Cl(1) 0.164(4) 0.222(5) 0.149(3) -0.030(3) 0.055(3) 0.015(3) Cl(2) 0.141(4) 0.337(7) 0.449(10) 0.008(4) 0.037(5) 0.283(7) Cl(3) 0.329(8) 0.279(7) 0.221(6) -0.099(6) 0.126(6) -0.044(5) O(1) 0.036(3) 0.066(4) 0.054(3) -0.012(2) 0.009(2) 0.014(3) O(2) 0.039(3) 0.045(3) 0.047(3) -0.002(2) 0.021(2) 0.007(2) O(3) 0.042(3) 0.053(3) 0.066(3) -0.007(2) 0.025(3) 0.004(3) O(4) 0.036(3) 0.050(3) 0.047(3) -0.006(2) 0.017(2) 0.005(3) N(1) 0.054(4) 0.041(4) 0.047(4) -0.007(3) 0.027(3) 0.005(3) N(2) 0.070(5) 0.062(5) 0.066(5) -0.023(4) 0.037(4) -0.001(4) N(3) 0.044(4) 0.045(4) 0.040(4) -0.014(3) 0.012(3) -0.001(3) N(4) 0.050(5) 0.075(5) 0.051(4) 0.006(4) 0.012(4) 0.009(4) C(1) 0.037(5) 0.048(5) 0.040(4) -0.012(4) 0.013(4) -0.008(4) C(2) 0.048(5) 0.047(5) 0.033(4) -0.014(4) 0.018(4) -0.005(4) C(3) 0.046(5) 0.055(5) 0.036(4) -0.005(4) 0.010(4) 0.003(4) C(4) 0.049(5) 0.066(6) 0.037(5) -0.021(4) 0.013(4) -0.007(4) C(5) 0.046(5) 0.059(5) 0.041(5) -0.018(4) 0.016(4) -0.003(4) C(6) 0.041(4) 0.044(5) 0.033(4) -0.015(4) 0.015(4) -0.008(3) C(7) 0.051(5) 0.041(4) 0.044(5) -0.013(4) 0.022(4) 0.001(4) C(8) 0.032(4) 0.032(4) 0.040(5) 0.000(3) 0.013(4) 0.008(4) C(9) 0.039(4) 0.028(4) 0.044(5) -0.009(3) 0.019(4) 0.001(3) C(10) 0.052(5) 0.037(4) 0.047(5) -0.005(4) 0.024(4) -0.004(4) C(11) 0.035(4) 0.038(5) 0.057(5) -0.002(3) 0.020(4) 0.006(4) C(12) 0.040(5) 0.045(5) 0.038(4) -0.012(4) 0.011(4) -0.004(4) C(13) 0.044(5) 0.031(4) 0.043(5) -0.002(3) 0.021(4) 0.010(3) C(14) 0.057(5) 0.040(5) 0.040(4) 0.000(4) 0.022(4) 0.007(4) C(15) 0.040(4) 0.039(5) 0.036(4) -0.001(4) 0.017(3) -0.008(4) C(16) 0.043(4) 0.041(5) 0.034(4) -0.005(4) 0.016(4) -0.001(3) C(17) 0.058(5) 0.056(5) 0.035(4) -0.021(4) 0.025(4) -0.003(4) C(18) 0.057(5) 0.045(5) 0.036(4) -0.001(4) 0.026(4) 0.001(4) C(19) 0.048(5) 0.040(4) 0.040(4) 0.000(4) 0.019(4) 0.001(4) C(20) 0.045(4) 0.037(4) 0.031(4) -0.011(4) 0.019(4) -0.009(3) C(21) 0.050(5) 0.038(4) 0.051(5) -0.012(4) 0.021(4) 0.001(4) C(22) 0.041(5) 0.039(4) 0.040(5) -0.011(3) 0.018(4) 0.011(4) C(23) 0.039(4) 0.034(4) 0.042(5) -0.009(3) 0.017(4) 0.002(3) C(24) 0.047(5) 0.038(5) 0.051(5) -0.014(4) 0.022(4) 0.000(4) C(25) 0.047(5) 0.037(4) 0.053(5) -0.015(4) 0.018(4) 0.005(4) C(26) 0.057(5) 0.043(5) 0.055(5) -0.009(4) 0.033(4) -0.004(4) C(27) 0.044(5) 0.046(5) 0.040(5) -0.017(4) 0.018(4) 0.003(4) C(28) 0.053(5) 0.055(5) 0.037(4) -0.015(4) 0.020(4) -0.002(4) C(29) 0.050(5) 0.037(5) 0.041(4) -0.007(4) 0.027(4) -0.005(4) C(30) 0.064(6) 0.048(5) 0.040(5) -0.011(4) 0.028(4) -0.004(4) C(31) 0.053(6) 0.070(6) 0.067(6) -0.024(5) 0.038(5) -0.012(5) C(32) 0.070(7) 0.097(8) 0.123(9) -0.020(6) 0.055(6) 0.015(7) C(33) 0.051(6) 0.112(9) 0.16(1) -0.012(6) 0.057(7) 0.023(8) C(34) 0.049(6) 0.102(8) 0.120(9) 0.004(5) 0.035(6) 0.025(7) C(35) 0.052(6) 0.065(6) 0.079(6) -0.008(5) 0.028(5) 0.008(5) C(36) 0.039(5) 0.054(5) 0.054(5) -0.010(4) 0.021(4) -0.008(4) C(37) 0.089(7) 0.053(6) 0.053(5) -0.011(5) 0.046(5) -0.005(4) C(38) 0.098(7) 0.046(5) 0.057(6) 0.005(5) 0.040(5) 0.007(5) C(39) 0.121(9) 0.066(7) 0.067(7) 0.023(7) 0.036(6) 0.008(6) C(40) 0.17(1) 0.075(9) 0.056(7) 0.041(9) 0.055(8) 0.015(6) C(41) 0.18(1) 0.040(6) 0.085(8) 0.002(8) 0.085(9) 0.011(6) C(42) 0.121(8) 0.058(6) 0.084(7) -0.008(6) 0.068(7) -0.003(5) C(43) 0.042(5) 0.041(5) 0.040(5) -0.015(4) 0.017(4) -0.011(4) C(44) 0.054(5) 0.055(5) 0.040(5) -0.005(4) 0.013(4) -0.005(4) C(45) 0.054(6) 0.082(7) 0.043(5) -0.011(5) 0.019(4) -0.008(5) C(46) 0.051(6) 0.114(8) 0.068(7) -0.006(5) 0.013(5) 0.006(6) C(47) 0.040(6) 0.128(9) 0.086(8) -0.006(6) 0.024(6) -0.006(7) C(48) 0.054(6) 0.110(8) 0.083(7) -0.028(5) 0.036(5) -0.006(6) C(49) 0.053(6) 0.086(7) 0.059(6) -0.019(5) 0.025(5) -0.004(5) C(50) 0.045(5) 0.063(5) 0.040(5) -0.011(4) 0.018(4) -0.010(4) C(51) 0.069(6) 0.053(6) 0.040(5) -0.010(5) 0.010(4) 0.000(4) C(52) 0.075(6) 0.070(6) 0.049(5) -0.027(5) 0.020(5) -0.003(4) C(53) 0.094(7) 0.108(8) 0.066(6) -0.044(7) 0.028(6) 0.002(6) C(54) 0.14(1) 0.096(9) 0.072(7) -0.045(9) 0.025(8) 0.026(6) C(55) 0.13(1) 0.085(8) 0.111(9) -0.014(8) 0.039(8) 0.048(7) C(56) 0.078(7) 0.078(7) 0.088(7) -0.004(6) 0.025(6) 0.026(6) C(57) 0.040(5) 0.073(6) 0.076(6) -0.006(5) 0.008(5) 0.006(5) C(58) 0.049(6) 0.125(9) 0.110(8) -0.009(6) 0.006(6) 0.013(7) C(59) 0.043(6) 0.19(1) 0.17(1) -0.021(7) 0.024(7) 0.055(10) C(60) 0.073(8) 0.18(1) 0.24(2) 0.008(8) -0.057(9) -0.12(1) C(61) 0.044(5) 0.055(6) 0.080(6) -0.006(4) 0.030(5) -0.007(5) C(62) 0.049(6) 0.15(1) 0.146(10) -0.027(6) 0.039(6) -0.067(8) C(63) 0.065(8) 0.083(9) 0.45(3) 0.021(7) 0.09(1) 0.05(1) C(64) 0.077(8) 0.28(2) 0.13(1) -0.051(9) 0.068(7) -0.06(1) C(65) 0.056(5) 0.067(6) 0.050(5) 0.001(4) 0.036(4) 0.005(4) C(66) 0.064(6) 0.17(1) 0.088(8) 0.011(6) 0.039(6) 0.032(7) C(67) 0.093(8) 0.15(1) 0.125(9) -0.018(7) 0.074(7) -0.060(8) C(68) 0.111(8) 0.127(9) 0.16(1) 0.009(7) 0.106(8) 0.036(8) C(69) 0.035(5) 0.076(6) 0.076(6) -0.008(4) 0.027(5) 0.006(5) C(70) 0.069(8) 0.10(1) 0.70(4) -0.026(8) 0.17(2) 0.03(2) C(71) 0.065(8) 0.39(2) 0.26(2) -0.07(1) 0.09(1) -0.20(2) C(72) 0.055(8) 0.43(3) 0.22(2) 0.04(1) 0.033(9) 0.17(2) C(73) 0.083(8) 0.15(1) 0.13(1) 0.022(8) 0.002(8) 0.025(9) #------------------------------------------------------------------------------ _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_number_reflns 5157 _refine_ls_number_parameters 757 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.0950 _refine_ls_wR_factor_obs 0.1080 _refine_ls_goodness_of_fit_obs 3.110 _refine_ls_shift/esd_max 0.0000 _refine_diff_density_min 0.64 _refine_diff_density_max -0.62 #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Cl(1) C(73) 1.72(1) Cl(2) C(73) 1.71(1) Cl(3) C(73) 1.76(2) O(1) C(1) 1.373(8) O(2) C(8) 1.412(8) O(2) C(29) 1.35(1) O(3) C(15) 1.365(9) O(4) C(22) 1.413(9) O(4) C(43) 1.341(7) N(1) C(29) 1.288(8) N(1) C(30) 1.38(1) N(2) C(30) 1.31(1) N(2) C(31) 1.370(10) N(3) C(43) 1.31(1) N(3) C(44) 1.370(8) N(4) C(44) 1.32(1) N(4) C(45) 1.37(1) C(1) C(2) 1.389(9) C(1) C(6) 1.40(1) C(2) C(3) 1.396(9) C(2) C(28) 1.52(1) C(3) C(4) 1.39(1) C(4) C(5) 1.391(10) C(4) C(57) 1.524(10) C(5) C(6) 1.394(9) C(6) C(7) 1.515(9) C(7) C(9) 1.532(8) C(8) C(9) 1.38(1) C(8) C(13) 1.383(8) C(9) C(10) 1.39(1) C(10) C(11) 1.389(9) C(11) C(12) 1.38(1) C(11) C(61) 1.52(1) C(12) C(13) 1.38(1) C(13) C(14) 1.52(1) C(14) C(16) 1.511(9) C(15) C(16) 1.39(1) C(15) C(20) 1.395(9) C(16) C(17) 1.39(1) C(17) C(18) 1.396(10) C(18) C(19) 1.38(1) C(18) C(65) 1.52(1) C(19) C(20) 1.39(1) C(20) C(21) 1.52(1) C(21) C(23) 1.51(1) C(22) C(23) 1.383(9) C(22) C(27) 1.38(1) C(23) C(24) 1.39(1) C(24) C(25) 1.39(1) C(25) C(26) 1.392(9) C(25) C(69) 1.53(1) C(26) C(27) 1.40(1) C(27) C(28) 1.507(9) C(29) C(36) 1.41(1) C(30) C(37) 1.485(10) C(31) C(32) 1.40(1) C(31) C(36) 1.39(1) C(32) C(33) 1.36(1) C(33) C(34) 1.37(2) C(34) C(35) 1.38(1) C(35) C(36) 1.394(10) C(37) C(38) 1.38(1) C(37) C(42) 1.38(1) C(38) C(39) 1.37(1) C(39) C(40) 1.36(2) C(40) C(41) 1.35(2) C(41) C(42) 1.40(1) C(43) C(50) 1.42(1) C(44) C(51) 1.49(1) C(45) C(46) 1.42(1) C(45) C(50) 1.397(10) C(46) C(47) 1.36(2) C(47) C(48) 1.41(1) C(48) C(49) 1.37(1) C(49) C(50) 1.39(1) C(51) C(52) 1.37(1) C(51) C(56) 1.38(1) C(52) C(53) 1.41(2) C(53) C(54) 1.38(1) C(54) C(55) 1.35(2) C(55) C(56) 1.36(2) C(57) C(58) 1.51(1) C(57) C(59) 1.51(2) C(57) C(60) 1.49(2) C(61) C(62) 1.47(1) C(61) C(63) 1.47(1) C(61) C(64) 1.54(2) C(65) C(66) 1.48(1) C(65) C(67) 1.50(1) C(65) C(68) 1.52(2) C(69) C(70) 1.42(2) C(69) C(71) 1.45(2) C(69) C(72) 1.49(2) #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C(8) O(2) C(29) 115.9(5) C(22) O(4) C(43) 119.1(6) C(29) N(1) C(30) 117.1(7) C(30) N(2) C(31) 116.8(8) C(43) N(3) C(44) 116.5(7) C(44) N(4) C(45) 116.0(6) O(1) C(1) C(2) 115.8(7) O(1) C(1) C(6) 122.7(6) C(2) C(1) C(6) 121.5(6) C(1) C(2) C(3) 118.9(7) C(1) C(2) C(28) 119.9(6) C(3) C(2) C(28) 121.1(6) C(2) C(3) C(4) 121.9(6) C(3) C(4) C(5) 116.9(6) C(3) C(4) C(57) 122.4(6) C(5) C(4) C(57) 120.7(8) C(4) C(5) C(6) 123.7(8) C(1) C(6) C(5) 116.9(6) C(1) C(6) C(7) 123.9(6) C(5) C(6) C(7) 119.0(7) C(6) C(7) C(9) 114.6(5) O(2) C(8) C(9) 117.2(5) O(2) C(8) C(13) 120.0(7) C(9) C(8) C(13) 122.8(7) C(7) C(9) C(8) 121.1(6) C(7) C(9) C(10) 121.4(7) C(8) C(9) C(10) 117.4(5) C(9) C(10) C(11) 122.2(7) C(10) C(11) C(12) 117.0(7) C(10) C(11) C(61) 120.2(7) C(12) C(11) C(61) 122.8(6) C(11) C(12) C(13) 123.3(6) C(8) C(13) C(12) 117.1(7) C(8) C(13) C(14) 122.2(7) C(12) C(13) C(14) 120.7(5) C(13) C(14) C(16) 114.2(6) O(3) C(15) C(16) 115.7(6) O(3) C(15) C(20) 123.0(7) C(16) C(15) C(20) 121.2(7) C(14) C(16) C(15) 119.8(7) C(14) C(16) C(17) 122.0(7) C(15) C(16) C(17) 118.2(6) C(16) C(17) C(18) 123.0(8) C(17) C(18) C(19) 115.8(7) C(17) C(18) C(65) 121.7(8) C(19) C(18) C(65) 122.4(6) C(18) C(19) C(20) 124.1(6) C(15) C(20) C(19) 117.5(7) C(15) C(20) C(21) 123.0(7) C(19) C(20) C(21) 119.5(6) C(20) C(21) C(23) 115.3(6) O(4) C(22) C(23) 115.8(7) O(4) C(22) C(27) 120.3(5) C(23) C(22) C(27) 123.7(7) C(21) C(23) C(22) 121.9(7) C(21) C(23) C(24) 121.1(6) C(22) C(23) C(24) 116.9(7) C(23) C(24) C(25) 123.0(6) C(24) C(25) C(26) 116.5(7) C(24) C(25) C(69) 121.6(6) C(26) C(25) C(69) 121.7(8) C(25) C(26) C(27) 123.3(8) C(22) C(27) C(26) 116.3(6) C(22) C(27) C(28) 122.3(7) C(26) C(27) C(28) 121.4(7) C(2) C(28) C(27) 115.1(6) O(2) C(29) N(1) 119.4(7) O(2) C(29) C(36) 116.8(6) N(1) C(29) C(36) 123.8(8) N(1) C(30) N(2) 125.3(6) N(1) C(30) C(37) 114.5(8) N(2) C(30) C(37) 120.2(9) N(2) C(31) C(32) 120.1(10) N(2) C(31) C(36) 122.2(8) C(32) C(31) C(36) 117.7(8) C(31) C(32) C(33) 120(1) C(32) C(33) C(34) 121.3(10) C(33) C(34) C(35) 120.2(8) C(34) C(35) C(36) 119.0(9) C(29) C(36) C(31) 114.8(6) C(29) C(36) C(35) 124.1(8) C(31) C(36) C(35) 121.1(8) C(30) C(37) C(38) 120.3(8) C(30) C(37) C(42) 121.1(8) C(38) C(37) C(42) 118.6(7) C(37) C(38) C(39) 121.3(10) C(38) C(39) C(40) 119(1) C(39) C(40) C(41) 120(1) C(40) C(41) C(42) 119(1) C(37) C(42) C(41) 119.5(10) O(4) C(43) N(3) 120.1(7) O(4) C(43) C(50) 116.4(7) N(3) C(43) C(50) 123.5(6) N(3) C(44) N(4) 126.3(8) N(3) C(44) C(51) 115.6(7) N(4) C(44) C(51) 118.0(6) N(4) C(45) C(46) 117.5(7) N(4) C(45) C(50) 122.9(8) C(46) C(45) C(50) 119.6(9) C(45) C(46) C(47) 118.7(8) C(46) C(47) C(48) 122.0(9) C(47) C(48) C(49) 119(1) C(48) C(49) C(50) 120.2(7) C(43) C(50) C(45) 114.7(8) C(43) C(50) C(49) 124.9(6) C(45) C(50) C(49) 120.3(8) C(44) C(51) C(52) 120.7(7) C(44) C(51) C(56) 120.3(9) C(52) C(51) C(56) 119.0(9) C(51) C(52) C(53) 119.3(7) C(52) C(53) C(54) 120(1) C(53) C(54) C(55) 118(1) C(54) C(55) C(56) 122.2(10) C(51) C(56) C(55) 120(1) C(4) C(57) C(58) 113.5(8) C(4) C(57) C(59) 110.9(7) C(4) C(57) C(60) 109.2(7) C(58) C(57) C(59) 104.6(8) C(58) C(57) C(60) 109.0(8) C(59) C(57) C(60) 109(1) C(11) C(61) C(62) 112.9(7) C(11) C(61) C(63) 109.8(8) C(11) C(61) C(64) 109.8(6) C(62) C(61) C(63) 114.0(8) C(62) C(61) C(64) 105.3(9) C(63) C(61) C(64) 104(1) C(18) C(65) C(66) 110.8(8) C(18) C(65) C(67) 109.0(7) C(18) C(65) C(68) 112.7(7) C(66) C(65) C(67) 109.8(7) C(66) C(65) C(68) 107.0(8) C(67) C(65) C(68) 107.4(9) C(25) C(69) C(70) 110.6(7) C(25) C(69) C(71) 114.9(7) C(25) C(69) C(72) 110.8(9) C(70) C(69) C(71) 110(1) C(70) C(69) C(72) 105(1) C(71) C(69) C(72) 104(1) Cl(1) C(73) Cl(2) 107.7(8) Cl(1) C(73) Cl(3) 104.9(6) Cl(2) C(73) Cl(3) 108.4(9) #------------------------------------------------------------------------------ data_[N11]_Silvio_P-1 _database_code_CSD 187175 #------------------------------------------------------------------------------ _audit_creation_date 'Thu May 9 11:45:24 2002' _audit_creation_method 'from TEXRAY.INF file' #------------------------------------------------------------------------------ _computing_data_collection 'Philips PW1100 Diffractometer Control' _computing_cell_refinement 'Philips PW1100 Diffractometer Control' _computing_data_reduction teXsan _computing_structure_solution SHELXS86 _computing_structure_refinement teXsan _computing_publication_material teXsan #------------------------------------------------------------------------------ _cell_length_a 13.031(5) _cell_length_b 13.368(5) _cell_length_c 11.333(4) _cell_angle_alpha 108.68(2) _cell_angle_beta 111.11(2) _cell_angle_gamma 61.57(2) _cell_volume 1592(1) _cell_formula_units_Z 2 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description unknown _exptl_crystal_colour unknown _exptl_crystal_size_max 0.000 _exptl_crystal_size_mid 0.000 _exptl_crystal_size_min 0.000 _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 588.89 _chemical_formula_moiety 'C72 H72 N4 O4 C1 H1 Cl3' _exptl_crystal_F_000 623.00 _exptl_absorpt_coefficient_mu 0.196 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details Walker&Stuart_DIFABS _exptl_absorpt_correction_T_max 1.115 _exptl_absorpt_correction_T_min 0.757 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector scintillation _diffrn_measurement_device 'Philips PW1100' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 4436 _reflns_number_total 4436 _reflns_number_observed 2545 _reflns_observed_criterion 2.00 _diffrn_reflns_av_R_equivalents 30.24 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2 _diffrn_reflns_theta_max 23.00 _diffrn_orient_matrix_UB_11 -0.02990 _diffrn_orient_matrix_UB_12 0.02903 _diffrn_orient_matrix_UB_13 -0.05338 _diffrn_orient_matrix_UB_21 0.05352 _diffrn_orient_matrix_UB_22 0.00488 _diffrn_orient_matrix_UB_23 0.00527 _diffrn_orient_matrix_UB_31 0.01855 _diffrn_orient_matrix_UB_32 -0.05397 _diffrn_orient_matrix_UB_33 -0.04237 #------------------------------------------------------------------------------ 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 73 0.003 0.002 'International Tables' H 0 74 0.000 0.000 'International Tables' O 0 4 0.011 0.006 'International Tables' N 0 4 0.006 0.003 'International Tables' Cl 0 3 0.148 0.159 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type Cl(1) 1.0174(5) 0.6057(4) 0.5409(5) 0.187 Uij Cl(2) 0.8746(6) 0.5638(6) 0.3181(7) 0.128 Uij O(1) 0.6770(5) 0.4249(4) 0.4590(5) 0.051 Uij O(2) 0.4363(4) 0.5540(4) 0.3141(4) 0.039 Uij N(1) 0.3444(5) 0.6224(5) 0.1263(6) 0.040 Uij N(2) 0.3515(6) 0.4977(6) -0.0778(6) 0.048 Uij C(1) 0.7088(6) 0.5005(6) 0.5644(7) 0.036 Uij C(2) 0.7784(6) 0.4539(6) 0.6768(7) 0.040 Uij C(3) 0.8126(7) 0.5278(7) 0.7834(7) 0.048 Uij C(4) 0.7847(6) 0.6427(6) 0.7864(7) 0.042 Uij C(5) 0.7169(7) 0.6814(6) 0.6696(8) 0.045 Uij C(6) 0.6772(6) 0.6134(6) 0.5585(7) 0.034 Uij C(7) 0.6025(7) 0.6622(6) 0.4357(7) 0.043 Uij C(8) 0.3914(7) 0.6715(6) 0.3771(7) 0.040 Uij C(9) 0.4700(6) 0.7246(6) 0.4347(6) 0.036 Uij C(10) 0.4223(7) 0.8393(6) 0.4934(7) 0.044 Uij C(11) 0.3034(7) 0.9016(6) 0.4974(7) 0.041 Uij C(12) 0.2301(7) 0.8415(6) 0.4420(7) 0.044 Uij C(13) 0.2712(7) 0.7263(6) 0.3819(7) 0.040 Uij C(14) 0.1813(6) 0.6711(6) 0.3177(7) 0.046 Uij C(15) 0.4053(6) 0.5340(7) 0.1829(7) 0.039 Uij C(16) 0.3187(6) 0.5991(7) -0.0058(8) 0.042 Uij C(17) 0.4134(7) 0.4051(6) -0.0151(8) 0.044 Uij C(18) 0.4531(8) 0.2917(8) -0.0866(8) 0.055 Uij C(19) 0.5129(8) 0.1977(7) -0.0297(10) 0.064 Uij C(20) 0.5381(8) 0.2125(7) 0.1050(9) 0.058 Uij C(21) 0.5040(7) 0.3207(7) 0.1793(8) 0.049 Uij C(22) 0.4423(6) 0.4171(6) 0.1199(7) 0.038 Uij C(23) 0.2454(6) 0.7062(6) -0.0641(8) 0.040 Uij C(24) 0.2039(8) 0.8140(8) 0.0101(8) 0.058 Uij C(25) 0.1391(9) 0.9118(8) -0.044(1) 0.069 Uij C(26) 0.1144(9) 0.9016(9) -0.176(1) 0.077 Uij C(27) 0.1544(9) 0.7953(9) -0.2529(10) 0.079 Uij C(28) 0.2186(8) 0.6973(7) -0.1976(8) 0.060 Uij C(29) 0.8280(7) 0.7217(7) 0.9038(8) 0.053 Uij C(30) 0.844(1) 0.6865(9) 1.0294(9) 0.089 Uij C(31) 0.949(1) 0.710(1) 0.903(1) 0.117 Uij C(32) 0.736(1) 0.8480(8) 0.911(1) 0.098 Uij C(33) 0.2548(8) 1.0302(7) 0.5539(8) 0.056 Uij C(34) 0.338(1) 1.059(1) 0.675(1) 0.169 Uij C(35) 0.131(1) 1.0785(9) 0.575(1) 0.114 Uij C(36) 0.244(1) 1.0943(9) 0.455(1) 0.135 Uij C(37) 0.999(2) 0.514(2) 0.428(2) 0.070 Uij H(1O1) 0.618 0.448 0.408 0.070 Uij H(3) 0.859 0.498 0.861 0.058 Uij H(5) 0.697 0.759 0.666 0.055 Uij H(10) 0.475 0.877 0.534 0.053 Uij H(12) 0.148 0.881 0.445 0.053 Uij H(18) 0.437 0.281 -0.177 0.066 Uij H(19) 0.538 0.122 -0.080 0.077 Uij H(20) 0.579 0.146 0.145 0.069 Uij H(21) 0.522 0.330 0.270 0.059 Uij H(24) 0.220 0.821 0.100 0.070 Uij H(25) 0.111 0.986 0.008 0.082 Uij H(26) 0.069 0.969 -0.213 0.093 Uij H(27) 0.138 0.789 -0.343 0.094 Uij H(28) 0.245 0.623 -0.251 0.072 Uij H(71) 0.629 0.715 0.430 0.052 Uij H(72) 0.613 0.601 0.364 0.052 Uij H(141) 0.155 0.677 0.229 0.055 Uij H(142) 0.115 0.715 0.357 0.055 Uij H(301) 0.768 0.695 1.033 0.107 Uij H(302) 0.900 0.608 1.030 0.107 Uij H(303) 0.873 0.735 1.102 0.107 Uij H(311) 1.005 0.632 0.904 0.141 Uij H(312) 0.941 0.733 0.828 0.141 Uij H(313) 0.976 0.759 0.977 0.141 Uij H(321) 0.767 0.894 0.985 0.118 Uij H(322) 0.723 0.874 0.836 0.118 Uij H(323) 0.663 0.854 0.917 0.118 Uij H(341) 0.347 1.021 0.738 0.204 Uij H(342) 0.415 1.033 0.659 0.204 Uij H(343) 0.307 1.140 0.704 0.204 Uij H(351) 0.105 1.159 0.606 0.139 Uij H(352) 0.076 1.064 0.496 0.139 Uij H(353) 0.133 1.042 0.636 0.139 Uij H(361) 0.321 1.067 0.440 0.163 Uij H(362) 0.189 1.080 0.377 0.163 Uij H(363) 0.216 1.175 0.489 0.163 Uij 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 Cl(1) 0.191(5) 0.144(4) 0.233(6) -0.054(4) 0.081(4) 0.030(4) Cl(2) 0.096(5) 0.140(6) 0.109(5) -0.024(4) 0.020(4) 0.016(4) O(1) 0.061(4) 0.046(3) 0.040(3) -0.022(3) 0.005(3) 0.006(3) O(2) 0.039(3) 0.038(3) 0.035(3) -0.013(2) 0.007(2) 0.005(2) N(1) 0.036(4) 0.052(4) 0.033(4) -0.015(3) 0.010(3) 0.011(3) N(2) 0.059(4) 0.047(4) 0.043(4) -0.024(4) 0.020(3) 0.000(4) C(1) 0.024(4) 0.047(5) 0.041(5) -0.019(4) 0.011(4) -0.001(4) C(2) 0.030(4) 0.038(5) 0.048(5) -0.013(4) 0.003(4) 0.011(4) C(3) 0.044(5) 0.051(5) 0.048(5) -0.021(4) -0.001(4) 0.017(4) C(4) 0.034(4) 0.047(5) 0.048(5) -0.015(4) 0.012(4) 0.009(4) C(5) 0.048(5) 0.042(5) 0.059(6) -0.022(4) 0.020(4) 0.009(4) C(6) 0.027(4) 0.040(5) 0.037(5) -0.019(3) 0.009(3) 0.002(4) C(7) 0.043(5) 0.050(5) 0.046(5) -0.019(4) 0.010(4) 0.020(4) C(8) 0.039(5) 0.044(5) 0.037(5) -0.016(4) 0.005(4) 0.012(4) C(9) 0.035(4) 0.047(5) 0.029(4) -0.020(4) 0.001(3) 0.013(3) C(10) 0.045(5) 0.037(5) 0.056(5) -0.017(4) 0.013(4) 0.014(4) C(11) 0.045(5) 0.045(5) 0.038(5) -0.019(4) 0.013(4) 0.008(4) C(12) 0.043(5) 0.049(5) 0.046(5) -0.016(4) 0.013(4) 0.015(4) C(13) 0.046(5) 0.035(5) 0.036(5) -0.015(4) 0.007(4) 0.010(4) C(14) 0.032(4) 0.049(5) 0.049(5) -0.010(4) 0.002(4) 0.016(4) C(15) 0.038(5) 0.051(5) 0.032(5) -0.021(4) 0.005(4) 0.012(4) C(16) 0.031(4) 0.045(5) 0.046(5) -0.013(4) 0.004(4) 0.015(4) C(17) 0.046(5) 0.041(5) 0.050(6) -0.018(4) 0.023(4) 0.002(4) C(18) 0.057(6) 0.064(6) 0.048(5) -0.034(5) 0.020(5) -0.010(5) C(19) 0.072(6) 0.042(5) 0.079(7) -0.022(5) 0.025(5) 0.003(5) C(20) 0.059(6) 0.035(5) 0.078(7) -0.018(4) 0.024(5) 0.001(5) C(21) 0.054(5) 0.049(5) 0.050(5) -0.023(4) 0.009(4) 0.015(4) C(22) 0.036(4) 0.037(5) 0.046(5) -0.014(4) 0.014(4) 0.007(4) C(23) 0.029(4) 0.045(5) 0.050(5) -0.014(4) 0.014(4) 0.007(4) C(24) 0.065(6) 0.060(6) 0.057(6) -0.023(5) 0.022(5) 0.014(5) C(25) 0.080(7) 0.057(6) 0.078(8) -0.025(5) 0.029(6) 0.017(5) C(26) 0.067(7) 0.074(8) 0.090(9) -0.009(6) 0.021(6) 0.042(7) C(27) 0.086(8) 0.076(7) 0.067(7) -0.013(6) 0.014(6) 0.043(6) C(28) 0.060(6) 0.069(6) 0.050(6) -0.024(5) 0.012(5) 0.015(5) C(29) 0.059(6) 0.058(6) 0.048(5) -0.037(5) 0.006(4) 0.001(4) C(30) 0.121(9) 0.102(8) 0.054(7) -0.074(7) 0.011(6) -0.008(6) C(31) 0.103(9) 0.18(1) 0.101(9) -0.113(9) 0.027(7) -0.033(8) C(32) 0.114(9) 0.058(7) 0.100(8) -0.045(7) 0.009(7) -0.012(6) C(33) 0.059(6) 0.039(5) 0.067(6) -0.020(4) 0.019(5) -0.001(4) C(34) 0.13(1) 0.085(9) 0.15(1) -0.017(8) -0.030(10) -0.050(9) C(35) 0.110(10) 0.057(7) 0.19(1) -0.031(7) 0.091(10) -0.020(7) C(36) 0.19(1) 0.047(7) 0.19(1) -0.011(8) 0.11(1) 0.038(8) C(37) 0.09(1) 0.08(1) 0.05(1) -0.05(1) 0.02(1) -0.01(1) #------------------------------------------------------------------------------ _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 3.48344 _refine_ls_number_reflns 2545 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.0890 _refine_ls_wR_factor_obs 0.1160 _refine_ls_goodness_of_fit_obs 2.110 _refine_ls_shift/esd_max 0.0000 _refine_diff_density_min 0.18 _refine_diff_density_max -0.17 #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Cl(1) C(37) 1.50(2) Cl(1)' C(37) 1.86(2) Cl(2) C(37) 1.64(2) O(1) C(1) 1.374(8) O(2) C(8) 1.424(8) O(2) C(15) 1.364(8) N(1) C(15) 1.290(9) N(1) C(16) 1.375(9) N(2) C(16) 1.295(9) N(2) C(17) 1.374(9) C(1) C(2) 1.404(10) C(1) C(6) 1.381(9) C(2) C(3) 1.378(10) C(2) C(14) 1.511(10) C(3) C(4) 1.391(10) C(4) C(5) 1.40(1) C(4) C(29) 1.53(1) C(5) C(6) 1.386(9) C(6) C(7) 1.520(10) C(7) C(9) 1.516(10) C(8) C(9) 1.375(9) C(8) C(13) 1.391(10) C(9) C(10) 1.385(10) C(10) C(11) 1.376(10) C(11) C(12) 1.389(10) C(11) C(33) 1.52(1) C(12) C(13) 1.388(10) C(13) C(14) 1.520(10) C(15) C(22) 1.414(10) C(16) C(23) 1.50(1) C(17) C(18) 1.41(1) C(17) C(22) 1.412(10) C(18) C(19) 1.35(1) C(19) C(20) 1.41(1) C(20) C(21) 1.37(1) C(21) C(22) 1.39(1) C(23) C(24) 1.37(1) C(23) C(28) 1.40(1) C(24) C(25) 1.38(1) C(25) C(26) 1.38(1) C(26) C(27) 1.37(1) C(27) C(28) 1.38(1) C(29) C(30) 1.55(1) C(29) C(31) 1.51(1) C(29) C(32) 1.53(1) C(33) C(34) 1.48(1) C(33) C(35) 1.51(1) C(33) C(36) 1.54(1) #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C(8) O(2) C(15) 116.7(5) C(15) N(1) C(16) 116.2(6) C(16) N(2) C(17) 116.1(7) O(1) C(1) C(2) 115.4(6) O(1) C(1) C(6) 122.0(7) C(2) C(1) C(6) 122.5(6) C(1) C(2) C(3) 116.4(6) C(1) C(2) C(14) 122.9(6) C(3) C(2) C(14) 120.7(7) C(2) C(3) C(4) 125.0(7) C(3) C(4) C(5) 114.8(7) C(3) C(4) C(29) 124.2(7) C(5) C(4) C(29) 121.0(7) C(4) C(5) C(6) 123.9(7) C(1) C(6) C(5) 117.3(7) C(1) C(6) C(7) 121.8(6) C(5) C(6) C(7) 120.9(6) C(6) C(7) C(9) 111.0(6) O(2) C(8) C(9) 118.4(6) O(2) C(8) C(13) 118.7(6) C(9) C(8) C(13) 122.8(7) C(7) C(9) C(8) 122.6(6) C(7) C(9) C(10) 120.9(6) C(8) C(9) C(10) 116.6(7) C(9) C(10) C(11) 124.3(7) C(10) C(11) C(12) 116.1(7) C(10) C(11) C(33) 121.5(7) C(12) C(11) C(33) 122.4(7) C(11) C(12) C(13) 123.0(7) C(8) C(13) C(12) 117.0(7) C(8) C(13) C(14) 124.3(6) C(12) C(13) C(14) 118.5(7) C(2) C(14) C(13) 118.9(6) O(2) C(15) N(1) 117.8(6) O(2) C(15) C(22) 116.9(7) N(1) C(15) C(22) 125.3(7) N(1) C(16) N(2) 126.3(7) N(1) C(16) C(23) 112.9(7) N(2) C(16) C(23) 120.8(7) N(2) C(17) C(18) 119.6(8) N(2) C(17) C(22) 123.1(7) C(18) C(17) C(22) 117.2(8) C(17) C(18) C(19) 121.9(8) C(18) C(19) C(20) 119.5(8) C(19) C(20) C(21) 121.0(8) C(20) C(21) C(22) 119.1(7) C(15) C(22) C(17) 112.8(7) C(15) C(22) C(21) 126.0(7) C(17) C(22) C(21) 121.2(7) C(16) C(23) C(24) 121.6(7) C(16) C(23) C(28) 119.8(7) C(24) C(23) C(28) 118.6(8) C(23) C(24) C(25) 121.1(8) C(24) C(25) C(26) 119.5(9) C(25) C(26) C(27) 120.9(9) C(26) C(27) C(28) 119.1(9) C(23) C(28) C(27) 120.7(8) C(4) C(29) C(30) 110.3(7) C(4) C(29) C(31) 109.7(7) C(4) C(29) C(32) 112.2(7) C(30) C(29) C(31) 107.9(8) C(30) C(29) C(32) 105.7(8) C(31) C(29) C(32) 111.0(8) C(11) C(33) C(34) 112.1(8) C(11) C(33) C(35) 114.0(7) C(11) C(33) C(36) 107.1(7) C(34) C(33) C(35) 109.9(10) C(34) C(33) C(36) 106(1) C(35) C(33) C(36) 106.4(9) Cl(1) C(37) Cl(1)' 117(1) Cl(1) C(37) Cl(2) 113(1) Cl(1)' C(37) Cl(2) 101(1) #------------------------------------------------------------------------------