#------------------------------------------------------------------------------ #$Date: 2009-11-14 13:09:05 +0000 (Sat, 14 Nov 2009) $ #$Revision: 846 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003715.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003715 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 1352 _journal_page_last 1355 _publ_section_title ; 1,7-Bis(\'ethoxycarbonyl)-3a-m\'ethyl-4a-ph\'enyl- 3,5-bis(p-nitroph\'enyl)-3a,4,4a,5-t\'etrahydro-3H-bis [1,2,4] triazolo[4,3-a:3',4'-d][1,5]benzodiaz\'epine, C~36~H~32~N~8~O~8~.CHCl~3~ ; _chemical_formula_moiety ' C36 H32 N8 O8,C1 H1 Cl3 ' _chemical_formula_sum ' C37 H33 Cl3 N8 O8' _chemical_formula_weight 824.08 loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' '-x,-y,-z' _symmetry_space_group_name_H-M 'P -1' _cell_length_a 12.044(7) _cell_length_b 12.461(7) _cell_length_c 13.730(8) _cell_angle_alpha 104.33(3) _cell_angle_beta 94.47(3) _cell_angle_gamma 101.00(3) _cell_volume 1942.8(19) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.41 _exptl_crystal_density_meas ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6.0 _cell_measurement_theta_max 10.7 _exptl_absorpt_coefficient_mu 0.29 _cell_measurement_temperature 293 _exptl_crystal_description prism _exptl_crystal_size_max 0.92 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.20 _exptl_crystal_colour orange _chemical_compound_source ; synth\`ese ; _diffrn_measurement_device 'Philips PW100 diffractometer' _diffrn_measurement_method \q/2\q _exptl_absorpt_correction_type none _diffrn_reflns_number 5736 _reflns_number_total 5736 _reflns_number_observed 3655 _reflns_observed_criterion refl_observed_if_I_>_3.0_sigma(I) _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_max 23.52 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_standards_number 3 _diffrn_standards_interval_time 180 _diffrn_standards_decay_% 3 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.088 _refine_ls_wR_factor_obs 0.111 _refine_ls_goodness_of_fit_obs 1.34 _refine_ls_number_reflns 3630 _refine_ls_number_parameters 280 _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme 'calc w = 1/(\s^2^(F) + 0.0005F^2^)' _refine_ls_shift/esd_max 0.01 _refine_diff_density_max 0.71 _refine_diff_density_min -0.59 _refine_ls_extinction_method none _atom_type_scat_source 'IntTabIV' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv C1 0.0477(5) 0.4819(5) 0.2087(4) 0.043(7) N2 -0.0040(4) 0.3838(4) 0.1535(4) 0.049(6) N3 0.0624(4) 0.3589(4) 0.0761(4) 0.049(6) C3a 0.1714(4) 0.4439(5) 0.0907(4) 0.038(6) C4 0.2749(4) 0.3954(5) 0.1179(4) 0.040(6) C4a 0.3622(4) 0.4753(4) 0.2060(4) 0.035(6) N5 0.4792(4) 0.4510(4) 0.1935(4) 0.043(5) N6 0.5441(4) 0.5258(4) 0.1519(3) 0.042(5) C7 0.4894(5) 0.6066(5) 0.1525(4) 0.039(6) N8 0.3876(4) 0.5896(4) 0.1906(3) 0.038(5) C8a 0.3248(5) 0.6749(5) 0.2254(4) 0.040(6) C9 0.3802(5) 0.7857(5) 0.2715(4) 0.046(7) C10 0.3185(6) 0.8698(5) 0.2991(5) 0.060(8) C11 0.2017(6) 0.8408(6) 0.2811(5) 0.065(9) C12 0.1458(5) 0.7307(5) 0.2380(5) 0.056(8) C12a 0.2046(5) 0.6430(5) 0.2124(4) 0.041(6) N13 0.1472(4) 0.5290(4) 0.1797(3) 0.039(5) C14 0.1830(5) 0.4942(6) 0.0013(5) 0.056(8) C15 0.3347(4) 0.4752(5) 0.3127(4) 0.037(6) C16 0.2478(5) 0.4005(5) 0.3331(5) 0.049(7) C17 0.2307(6) 0.4026(7) 0.4311(6) 0.077(10) C18 0.2976(8) 0.4835(8) 0.5090(6) 0.083(11) C19 0.3822(7) 0.5607(7) 0.4924(5) 0.071(10) C20 0.4038(5) 0.5601(5) 0.3938(5) 0.054(8) C21 0.5200(4) 0.3599(5) 0.2135(4) 0.037(6) C22 0.6385(5) 0.3618(5) 0.2101(4) 0.045(7) C23 0.6809(5) 0.2721(6) 0.2267(5) 0.056(8) C24 0.6101(5) 0.1832(5) 0.2467(5) 0.050(7) C25 0.4963(5) 0.1805(5) 0.2537(4) 0.049(7) C26 0.4507(5) 0.2700(5) 0.2359(4) 0.041(6) N27 0.6536(6) 0.0857(5) 0.2615(5) 0.075(9) O28 0.7487(5) 0.0782(5) 0.2366(5) 0.116(9) O29 0.5967(5) 0.0155(5) 0.2944(5) 0.118(10) C30 0.5331(6) 0.6963(5) 0.1044(4) 0.048(7) O31 0.6332(4) 0.7293(4) 0.0994(4) 0.081(7) O32 0.4508(3) 0.7386(3) 0.0693(3) 0.054(5) C33 0.4827(6) 0.8402(6) 0.0362(5) 0.063(8) C34 0.3826(7) 0.8935(7) 0.0350(6) 0.086(10) C35 0.0005(6) 0.5311(6) 0.3045(5) 0.060(8) O36 -0.0979(4) 0.5159(5) 0.3109(4) 0.105(8) O37 0.0824(4) 0.5925(4) 0.3761(3) 0.063(5) C38 0.0481(8) 0.6528(8) 0.4703(6) 0.096(12) C39 0.1370(11) 0.7366(11) 0.5284(8) 0.147(18) C40 0.0319(5) 0.2496(5) 0.0107(4) 0.046(7) C41 0.0992(5) 0.2134(5) -0.0655(5) 0.055(8) C42 0.0629(5) 0.1055(6) -0.1314(5) 0.058(8) C43 -0.0359(6) 0.0364(5) -0.1239(5) 0.058(8) C44 -0.1015(5) 0.0699(6) -0.0477(6) 0.062(8) C45 -0.0672(5) 0.1754(5) 0.0177(5) 0.057(8) N46 -0.0771(6) -0.0752(5) -0.1956(5) 0.076(9) O47 -0.0192(6) -0.1043(5) -0.2616(5) 0.119(9) O48 -0.1668(6) -0.1332(5) -0.1860(5) 0.110(9) C53 0.2568(11) 0.1258(10) 0.5844(15) 0.21(3) Cl1 0.2571(5) 0.2549(4) 0.6647(3) 0.211(8) Cl2 0.3673(5) 0.1507(4) 0.5146(4) 0.232(9) Cl3 0.1364(4) 0.0707(5) 0.5141(6) 0.355(15) H4a 0.31478 0.37799 0.05660 0.044 H4b 0.24608 0.32359 0.13690 0.044 H9 0.46535 0.80597 0.28507 0.051 H10 0.35884 0.95024 0.33176 0.065 H11 0.15721 0.90105 0.29972 0.071 H12 0.06086 0.71250 0.22423 0.061 H14a 0.25680 0.55086 0.01376 0.061 H14b 0.11825 0.53220 -0.00731 0.061 H14c 0.18110 0.43229 -0.06151 0.061 H16 0.19514 0.34314 0.27586 0.054 H17 0.16868 0.34460 0.44497 0.084 H18 0.28275 0.48541 0.58015 0.091 H19 0.43081 0.61886 0.55149 0.078 H20 0.46706 0.61784 0.38118 0.059 H22 0.68995 0.42756 0.19544 0.050 H23 0.76343 0.27227 0.22431 0.061 H25 0.44707 0.11550 0.27118 0.054 H26 0.36758 0.26891 0.23919 0.045 H33a 0.50556 0.82009 -0.03340 0.069 H33b 0.54816 0.89359 0.08390 0.069 H34a 0.40327 0.96402 0.01206 0.095 H34b 0.31769 0.83929 -0.01286 0.095 H34c 0.36035 0.91289 0.10463 0.095 H38a 0.02178 0.59751 0.50992 0.105 H38b -0.01649 0.68812 0.45370 0.105 H39a 0.11004 0.77610 0.59237 0.162 H39b 0.20120 0.70204 0.54610 0.162 H39c 0.16288 0.79279 0.48980 0.162 H41 0.17119 0.26471 -0.07198 0.060 H42 0.11011 0.07869 -0.18535 0.064 H44 -0.17265 0.01740 -0.04120 0.068 H45 -0.11465 0.20016 0.07207 0.063 H53 0.26586 0.06875 0.62596 0.221 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 C1 0.0320(32) 0.0136(29) 0.0029(28) 0.0425(37) 0.0048(30) 0.0463(37) N2 0.0294(26) 0.0078(25) 0.0019(24) 0.0567(35) -0.0025(27) 0.0493(32) N3 0.0315(26) 0.0089(24) 0.0048(23) 0.0591(35) -0.0034(26) 0.0451(31) C3a 0.0326(30) 0.0070(25) -0.0021(25) 0.0380(33) -0.0079(26) 0.0326(33) C4 0.0293(30) 0.0086(26) -0.0025(25) 0.0439(34) -0.0047(27) 0.0374(34) C4a 0.0245(28) 0.0095(24) 0.0024(24) 0.0322(32) -0.0003(25) 0.0405(34) N5 0.0282(25) 0.0115(22) 0.0056(22) 0.0404(28) 0.0070(24) 0.0518(31) N6 0.0362(26) 0.0053(24) 0.0043(22) 0.0401(29) 0.0062(23) 0.0416(30) C7 0.0371(33) 0.0077(28) 0.0011(26) 0.0367(33) 0.0044(26) 0.0362(34) N8 0.0329(25) 0.0119(21) 0.0090(21) 0.0322(27) 0.0036(21) 0.0420(29) C8a 0.0427(34) 0.0115(28) 0.0050(26) 0.0375(34) 0.0044(27) 0.0323(33) C9 0.0467(35) 0.0079(30) 0.0034(29) 0.0391(36) 0.0012(29) 0.0436(37) C10 0.0660(46) 0.0124(35) 0.0107(36) 0.0407(39) 0.0007(32) 0.0605(45) C11 0.0778(52) 0.0306(38) 0.0171(38) 0.0478(42) 0.0042(34) 0.0572(44) C12 0.0537(39) 0.0255(33) 0.0090(32) 0.0463(40) 0.0081(32) 0.0572(42) C12a 0.0407(34) 0.0106(28) 0.0055(26) 0.0378(34) 0.0034(26) 0.0350(34) N13 0.0272(25) 0.0081(21) 0.0038(21) 0.0370(28) -0.0029(22) 0.0432(29) C14 0.0445(37) 0.0137(33) -0.0038(30) 0.0704(46) 0.0065(33) 0.0415(39) C15 0.0333(31) 0.0139(26) 0.0008(25) 0.0351(31) 0.0008(26) 0.0361(33) C16 0.0436(35) 0.0196(30) 0.0128(30) 0.0456(37) 0.0075(30) 0.0490(40) C17 0.0695(49) 0.0283(42) 0.0376(44) 0.0786(54) 0.0285(46) 0.0724(55) C18 0.0920(60) 0.0410(51) 0.0284(46) 0.0906(61) 0.0229(47) 0.0529(50) C19 0.0891(56) 0.0273(45) -0.0136(38) 0.0731(52) -0.0002(36) 0.0356(43) C20 0.0514(38) 0.0127(32) -0.0067(32) 0.0488(39) -0.0010(32) 0.0493(42) C21 0.0302(30) 0.0068(26) -0.0047(24) 0.0360(33) -0.0081(25) 0.0341(33) C22 0.0328(32) 0.0086(28) -0.0001(27) 0.0427(36) -0.0008(29) 0.0503(39) C23 0.0380(35) 0.0222(35) -0.0074(30) 0.0643(46) -0.0045(34) 0.0519(42) C24 0.0475(39) 0.0167(31) -0.0079(30) 0.0396(37) -0.0010(30) 0.0521(41) C25 0.0476(38) 0.0087(30) 0.0012(30) 0.0412(36) 0.0060(30) 0.0487(39) C26 0.0351(31) 0.0103(27) 0.0010(27) 0.0339(33) 0.0033(27) 0.0453(36) N27 0.0602(43) 0.0195(35) -0.0144(37) 0.0510(41) 0.0054(36) 0.0979(52) O28 0.0791(40) 0.0506(34) 0.0034(39) 0.0867(43) 0.0190(39) 0.1608(61) O29 0.0893(44) 0.0356(36) 0.0004(41) 0.0780(43) 0.0491(44) 0.1697(66) C30 0.0496(40) 0.0094(31) 0.0109(31) 0.0396(36) 0.0015(29) 0.0444(38) O31 0.0428(28) 0.0162(25) 0.0279(26) 0.0877(36) 0.0384(31) 0.0991(40) O32 0.0493(25) 0.0130(21) 0.0016(20) 0.0544(27) 0.0187(22) 0.0502(27) C33 0.0672(45) 0.0129(35) 0.0106(34) 0.0557(42) 0.0225(35) 0.0550(43) C34 0.0899(56) 0.0369(45) 0.0153(44) 0.0757(52) 0.0319(43) 0.0790(55) C35 0.0403(40) 0.0102(33) 0.0146(36) 0.0577(44) -0.0054(37) 0.0689(49) O36 0.0462(32) -0.0069(31) 0.0342(30) 0.1263(50) -0.0382(37) 0.1108(46) O37 0.0532(27) 0.0187(24) 0.0109(22) 0.0746(32) -0.0119(23) 0.0452(27) C38 0.0935(61) 0.0129(53) 0.0317(48) 0.1075(68) -0.0262(49) 0.0610(53) C39 0.1530 0.0325(87) 0.0079(69) 0.1680 -0.0441(72) 0.0827(72) C40 0.0321(32) 0.0091(29) -0.0088(28) 0.0494(39) -0.0059(31) 0.0446(37) C41 0.0401(36) 0.0080(31) -0.0005(31) 0.0586(43) -0.0097(34) 0.0515(41) C42 0.0499(41) 0.0134(34) -0.0059(33) 0.0519(42) -0.0119(34) 0.0582(44) C43 0.0500(41) 0.0097(34) -0.0109(35) 0.0489(41) -0.0072(34) 0.0608(46) C44 0.0411(37) 0.0000(32) -0.0085(35) 0.0541(44) -0.0062(37) 0.0738(50) C45 0.0384(36) 0.0036(31) 0.0067(32) 0.0519(41) -0.0020(35) 0.0679(46) N46 0.0683(45) 0.0086(36) -0.0129(39) 0.0536(42) -0.0141(37) 0.0865(51) O47 0.1073(48) 0.0060(38) 0.0113(41) 0.1032(50) -0.0632(40) 0.1093(50) O48 0.0917(44) -0.0174(35) 0.0070(40) 0.0657(39) -0.0324(36) 0.1409(57) C53 0.1024(87) -0.0152(72) -0.095(12) 0.1043(94) 0.126(13) 0.399(23) Cl1 0.3197(58) -0.0207(35) -0.0325(29) 0.1607(34) -0.0058(22) 0.1045(25) Cl2 0.2373(52) -0.0036(38) -0.0449(41) 0.1739(40) -0.0055(34) 0.2282(49) Cl3 0.1751(42) 0.0383(36) -0.1465(58) 0.2031(50) -0.1917(65) 0.576(12)