#------------------------------------------------------------------------------ #$Date: 2008-01-14 00:15:36 +0200 (Mon, 14 Jan 2008) $ #$Revision: 14 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2002946.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_2002946 _journal_name_full 'Acta Crystallographica, Section B' _journal_year 1999 _journal_volume B55 _journal_page_first 441 _journal_page_last 447 _publ_section_title ; 3(5),4-Dimethyl and 3,4,5-Trimethylpyrazoles at 200K ; loop_ _publ_author_name 'Infantes, L.' 'Foces-Foces, C.' 'Elguero,J.' _chemical_name_systematic '4,5-dimethylpyrazole' _chemical_formula_moiety 'C5 H8 N2' _chemical_formula_sum 'C5 H8 N2' _chemical_formula_weight 96.132 _chemical_melting_point 331 _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 14.4170(10) _cell_length_b 12.0200(10) _cell_length_c 12.0420(10) _cell_angle_alpha 119.990(7) _cell_angle_beta 105.991(7) _cell_angle_gamma 87.224(10) _cell_volume 1727.5(3) _cell_formula_units_Z 12 _cell_measurement_reflns_used 74 _cell_measurement_theta_min 4.2 _cell_measurement_theta_max 44.1 _cell_measurement_temperature 200 _exptl_crystal_description sheet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.17 _exptl_crystal_density_diffrn 1.109 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 0.556 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_ambient_temperature 200 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Philips PW1100 diffractometer' _diffrn_measurement_method '\w/2\q scans' _diffrn_reflns_number 5733 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_sigmaI/netI .000 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 64.84 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_reduction_process perpendicular_monochr_Lp _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 90 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 3 -3 0 -3 3 _reflns_number_total 5733 _reflns_number_observed 4543 _reflns_observed_criterion I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_R_factor_all .087 _refine_ls_R_factor_obs .075 _refine_ls_wR_factor_all .105 _refine_ls_wR_factor_obs .092 _refine_ls_goodness_of_fit_all .856 _refine_ls_goodness_of_fit_obs .848 _refine_ls_number_reflns 4543 _refine_ls_number_parameters 571 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_hydrogen_treatment refall _refine_ls_weighting_scheme 'w = k/[(A+B Fo)^2^(C+D(sin\q)/\l)]' _refine_ls_shift/esd_max .03 _refine_ls_shift/esd_mean .001 _refine_diff_density_max .30 _refine_diff_density_min -.42 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 84.E1(2) _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? .017 .009 IntTabIV H ? 0 0 IntTabIV N ? .029 .018 IntTabIV 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 _atom_site_calc_flag _atom_site_calc_attached_atom N11 .1263(2) .9490(2) .8749(2) .0450(10) Uani No No N12 .1136(2) .9932(2) .7889(2) .0506(10) Uani No No C13 .1079(2) 1.1196(3) .8621(3) .0491(12) Uani No No C14 .1158(2) 1.1562(3) .9940(3) .0451(11) Uani No No C15 .1278(2) 1.0442(3) .9983(3) .0427(10) Uani No No C16 .1128(3) 1.2893(3) 1.1064(4) .0668(15) Uani No No C17 .1391(3) 1.0208(4) 1.1120(3) .0616(16) Uani No No N21 .1299(2) .5914(2) .6354(2) .0452(10) Uani No No N22 .1363(2) .6765(2) .7654(2) .0484(10) Uani No No C23 .1340(2) .6044(3) .8202(3) .0505(12) Uani No No C24 .1265(2) .4734(3) .7272(3) .0439(11) Uani No No C25 .1241(2) .4697(2) .6105(3) .0420(10) Uani No No C26 .1226(3) .3620(4) .7502(5) .0667(17) Uani No No C27 .1155(3) .3567(3) .4732(3) .0626(15) Uani No No N31 .1239(2) .8333(2) .5196(2) .0442(9) Uani No No N32 .1331(2) .7061(2) .4767(2) .0512(11) Uani No No C33 .1394(3) .6544(3) .3524(3) .0505(12) Uani No No C34 .1343(2) .7467(3) .3136(3) .0441(11) Uani No No C35 .1249(2) .8601(2) .4235(3) .0408(10) Uani No No C36 .1388(4) .7278(4) .1823(4) .0657(18) Uani No No C37 .1167(3) .9936(3) .4459(4) .0554(13) Uani No No N41 .3811(2) -.0505(2) .1160(2) .0446(10) Uani No No N42 .3864(2) -.0946(2) .2009(2) .0483(10) Uani No No C43 .3902(2) -.2224(3) .1292(3) .0494(12) Uani No No C44 .3875(2) -.2608(2) -.0010(3) .0452(10) Uani No No C45 .3816(2) -.1483(3) -.0062(3) .0439(11) Uani No No C46 .3901(3) -.3945(3) -.1122(4) .0696(15) Uani No No C47 .3755(3) -.1264(4) -.1193(4) .0640(16) Uani No No N51 .3696(2) .3030(2) .3534(2) .0463(10) Uani No No N52 .3767(2) .2238(2) .2280(2) .0519(11) Uani No No C53 .3812(3) .2986(3) .1774(3) .0524(13) Uani No No C54 .3778(2) .4279(3) .2703(3) .0446(11) Uani No No C55 .3703(2) .4253(2) .3809(3) .0412(10) Uani No No C56 .3819(4) .5420(4) .2518(5) .0706(19) Uani No No C57 .3642(3) .5338(3) .5135(3) .0578(13) Uani No No N61 .3736(2) .0632(2) .4689(2) .0459(10) Uani No No N62 .3595(2) .1887(2) .5099(2) .0520(11) Uani No No C63 .3517(2) .2405(3) .6341(3) .0487(12) Uani No No C64 .3602(2) .1496(3) .6739(3) .0432(11) Uani No No C65 .3740(2) .0374(3) .5654(3) .0415(10) Uani No No C66 .3551(3) .1666(4) .8041(3) .0612(16) Uani No No C67 .3876(3) -.0944(3) .5478(4) .0599(14) Uani No No H11 .122(3) .866(4) .842(4) .031(9) Uiso No No H13 .103(4) 1.170(6) .821(6) .069(16) Uiso No No H161 .112(4) 1.354(6) 1.068(6) .074(17) Uiso No No H162 .058(5) 1.294(6) 1.146(7) .081(18) Uiso No No H163 .169(5) 1.318(6) 1.182(6) .073(17) Uiso No No H171 .166(5) .943(7) 1.097(7) .082(19) Uiso No No H172 .199(5) 1.090(7) 1.196(7) .09(2) Uiso No No H173 .092(5) 1.032(7) 1.140(7) .09(2) Uiso No No H21 .137(4) .631(5) .582(5) .057(13) Uiso No No H23 .132(4) .663(5) .916(6) .062(14) Uiso No No H261 .117(7) .404(10) .851(11) .15(4) Uiso No No H262 .062(6) .294(8) .686(8) .10(2) Uiso No No H263 .173(4) .308(6) .736(5) .062(14) Uiso No No H271 .085(4) .366(6) .395(7) .075(17) Uiso No No H272 .183(6) .322(7) .463(7) .10(2) Uiso No No H273 .077(5) .293(7) .461(7) .09(2) Uiso No No H31 .119(6) .892(8) .629(8) .12(3) Uiso No No H33 .148(3) .574(4) .306(4) .025(8) Uiso No No H361 .127(6) .627(8) .118(8) .12(3) Uiso No No H362 .087(5) .759(6) .139(7) .079(18) Uiso No No H363 .190(5) .778(7) .195(7) .08(2) Uiso No No H371 .128(7) 1.065(9) .549(10) .13(3) Uiso No No H372 .166(7) 1.005(9) .400(10) .14(3) Uiso No No H373 .049(6) .999(7) .381(8) .10(2) Uiso No No H41 .375(4) .040(5) .140(5) .060(14) Uiso No No H43 .394(4) -.272(5) .174(5) .058(13) Uiso No No H461 .406(7) -.452(9) -.071(10) .14(3) Uiso No No H462 .334(7) -.443(9) -.195(10) .13(3) Uiso No No H463 .432(6) -.406(8) -.169(8) .11(3) Uiso No No H471 .355(7) -.033(10) -.090(10) .14(3) Uiso No No H472 .425(6) -.158(8) -.158(8) .11(3) Uiso No No H473 .316(5) -.181(6) -.204(7) .082(18) Uiso No No H51 .366(4) .244(6) .393(6) .072(16) Uiso No No H53 .393(4) .266(5) .089(5) .057(13) Uiso No No H561 .383(5) .517(7) .148(8) .10(2) Uiso No No H562 .338(4) .594(6) .284(6) .067(15) Uiso No No H563 .447(6) .603(7) .327(8) .10(2) Uiso No No H571 .339(6) .502(8) .567(9) .12(3) Uiso No No H572 .420(5) .602(6) .566(7) .080(18) Uiso No No H573 .317(6) .602(8) .504(8) .12(3) Uiso No No H61 .364(5) -.004(7) .359(7) .09(2) Uiso No No H63 .344(3) .329(4) .683(4) .030(9) Uiso No No H661 .350(7) .260(9) .865(9) .13(3) Uiso No No H662 .305(4) .116(6) .787(6) .063(15) Uiso No No H663 .413(4) .132(5) .845(5) .054(12) Uiso No No H671 .408(6) -.139(9) .469(10) .12(3) Uiso No No H672 .451(5) -.097(6) .617(7) .09(2) Uiso No No H673 .328(5) -.132(7) .556(7) .09(2) Uiso No No 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 N11 .0693(15) .0294(11) .0338(11) .0081(9) .0138(10) .0151(9) N12 .0784(17) .0406(12) .0329(11) .0112(11) .0187(11) .0179(10) C13 .0732(19) .0384(13) .0377(14) .0113(12) .0178(12) .0202(12) C14 .0559(16) .0357(13) .0321(13) .0040(11) .0108(11) .0097(11) C15 .0528(15) .0420(13) .0306(12) .0048(10) .0111(10) .0169(11) C16 .080(2) .0439(17) .0446(17) .0103(15) .0133(16) .0025(14) C17 .075(2) .075(2) .0440(17) .0092(18) .0147(15) .0381(17) N21 .0673(15) .0388(11) .0335(11) .0105(10) .0162(10) .0209(9) N22 .0743(16) .0358(11) .0356(12) .0107(10) .0171(11) .0183(9) C23 .0706(19) .0480(15) .0386(14) .0116(13) .0200(12) .0244(12) C24 .0567(15) .0384(13) .0453(14) .0089(11) .0162(11) .0269(11) C25 .0534(15) .0337(12) .0388(14) .0078(10) .0125(11) .0189(11) C26 .087(3) .0548(18) .087(3) .0163(18) .034(2) .053(2) C27 .085(2) .0431(16) .0434(17) .0108(16) .0168(15) .0112(13) N31 .0658(14) .0368(11) .0312(11) .0114(9) .0143(9) .0185(9) N32 .0848(18) .0414(12) .0359(12) .0159(11) .0240(11) .0231(10) C33 .078(2) .0404(15) .0325(13) .0156(13) .0195(12) .0175(12) C34 .0622(16) .0479(14) .0270(12) .0104(11) .0156(11) .0213(11) C35 .0525(15) .0372(13) .0346(12) .0059(10) .0100(10) .0209(10) C36 .095(3) .079(2) .0421(17) .027(2) .0316(17) .0405(17) C37 .067(2) .0422(15) .0602(19) .0080(13) .0095(15) .0331(14) N41 .0658(15) .0315(11) .0370(11) .0091(9) .0164(10) .0174(9) N42 .0720(16) .0382(11) .0343(11) .0067(10) .0179(10) .0170(9) C43 .0708(19) .0379(13) .0448(15) .0076(12) .0196(13) .0234(12) C44 .0555(15) .0333(13) .0377(13) .0032(10) .0148(11) .0107(11) C45 .0551(15) .0419(13) .0309(12) .0066(11) .0121(11) .0161(11) C46 .089(3) .0362(15) .057(2) .0056(15) .0272(18) .0014(14) C47 .086(2) .071(2) .0455(17) .0121(18) .0215(17) .0360(16) N51 .0706(15) .0370(11) .0370(12) .0114(10) .0190(10) .0216(9) N52 .0848(18) .0375(11) .0393(12) .0095(11) .0249(12) .0204(10) C53 .084(2) .0417(14) .0391(15) .0122(13) .0255(14) .0226(12) C54 .0612(16) .0361(13) .0469(15) .0115(11) .0214(12) .0261(12) C55 .0520(14) .0348(12) .0353(13) .0076(10) .0119(10) .0173(10) C56 .105(3) .0540(18) .086(3) .028(2) .048(2) .051(2) C57 .073(2) .0449(15) .0411(15) .0133(14) .0173(14) .0115(13) N61 .0649(15) .0404(11) .0330(11) .0068(10) .0161(10) .0181(9) N62 .0822(18) .0438(12) .0379(12) .0103(11) .0242(11) .0232(10) C63 .0709(19) .0384(14) .0334(13) .0078(12) .0172(12) .0151(11) C64 .0560(15) .0456(14) .0285(12) .0034(11) .0109(10) .0197(10) C65 .0503(14) .0386(13) .0361(13) .0042(10) .0096(10) .0207(11) C66 .077(2) .079(2) .0377(15) .0099(18) .0182(14) .0364(16) C67 .071(2) .0473(16) .067(2) .0093(14) .0145(16) .0363(16)