#------------------------------------------------------------------------------ #$Date: 2011-09-28 17:24:46 +0300 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/00/29/2002947.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_2002947 _journal_name_full 'Acta Crystallographica, Section B' _journal_volume 55 _journal_year 1999 _journal_page_first 441 _journal_page_last 447 _publ_section_title ; 3(5),4-Dimethyl and 3,4,5-Trimethylpyrazoles at 200K ; _space_group_IT_number 15 _symmetry_space_group_name_Hall '-I 2ya' _symmetry_space_group_name_H-M 'I 1 2/a 1' _[local]_cod_cif_authors_sg_H-M 'I 2/a' loop_ _publ_author_name 'Infantes, L.' 'Foces-Foces, C.' 'Elguero,J.' _chemical_name_systematic '3,4,5-trimethylpyrazole' _chemical_formula_moiety 'C6 H10 N2' _chemical_formula_sum 'C6 H10 N2' _chemical_formula_weight 110.2 _chemical_melting_point .411E-305 _symmetry_cell_setting monoclinic loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,+y,-z -x,-y,-z 1/2+x,-y,+z 1/2+x,1/2+y,1/2+z -x,1/2+y,1/2-z 1/2-x,1/2-y,1/2-z +x,1/2-y,1/2+z _cell_length_a 14.1911(9) _cell_length_b 8.2520(6) _cell_length_c 16.7382(19) _cell_angle_alpha 90.00000 _cell_angle_beta 90.696(9) _cell_angle_gamma 90.00000 _cell_volume 1960.0(3) _cell_formula_units_Z 12 _cell_measurement_reflns_used 43 _cell_measurement_theta_min 5.2 _cell_measurement_theta_max 45.0 _cell_measurement_temperature 200 _exptl_crystal_description 'Rectangular prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.67 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.17 _exptl_crystal_density_diffrn 1.12 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 0.546 _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 1863 _diffrn_reflns_av_R_equivalents .024 _diffrn_reflns_av_sigmaI/netI .013 _diffrn_reflns_theta_min 5.29 _diffrn_reflns_theta_max 65.08 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _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 1 2 1 -1 -2 -1 _reflns_number_total 1680 _reflns_number_observed 1372 _reflns_observed_criterion I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_R_factor_all .059 _refine_ls_R_factor_obs .048 _refine_ls_wR_factor_all .063 _refine_ls_wR_factor_obs .054 _refine_ls_goodness_of_fit_all .913 _refine_ls_goodness_of_fit_obs .887 _refine_ls_number_reflns 1366 _refine_ls_number_parameters 182 _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 .07 _refine_ls_shift/esd_mean .006 _refine_diff_density_max 0.22 _refine_diff_density_min -0.20 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 390.(10) _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 N21 .35536(12) .7225(2) .13030(10) .0433(8) Uani No No N22 .33361(11) .7844(2) .20287(9) .0415(8) Uani No No C23 .40460(13) .8798(2) .22683(11) .0410(9) Uani No No C24 .47360(13) .8813(2) .16877(11) .0407(9) Uani No No C25 .43939(13) .7802(2) .10908(11) .0428(9) Uani No No C26 .40211(19) .9656(3) .30554(14) .0586(13) Uani No No C27 .56448(16) .9731(3) .16994(15) .0577(13) Uani No No C28 .48383(19) .7345(3) .03184(14) .0594(13) Uani No No N12 .26997(11) .4612(2) .03667(10) .0414(8) Uani No No C13 .28248(12) .3071(2) .05999(11) .0410(9) Uani No No C14 .25000 .2043(3) .00000 .0398(12) Uani No No C16 .32655(19) .2663(4) .13847(14) .0605(13) Uani No No C17 .25000 .0223(4) .00000 .064(2) Uani No No H21 .324(3) .655(6) .107(3) .010(9) Uiso No No H22 .281(3) .761(5) .230(3) .016(10) Uiso No No H26a .400(3) 1.080(7) .300(3) .094(15) Uiso No No H26b .344(4) .951(6) .330(3) .090(14) Uiso No No H26c .448(4) .936(7) .341(3) .096(15) Uiso No No H27a .584(3) 1.026(6) .220(3) .076(11) Uiso No No H27b .570(3) 1.058(6) .127(3) .077(12) Uiso No No H27c .619(3) .912(6) .160(3) .088(13) Uiso No No H28a .448(3) .664(6) .000(3) .084(13) Uiso No No H28b .494(3) .827(6) -.003(3) .075(11) Uiso No No H28c .544(3) .682(5) .036(2) .072(11) Uiso No No H12 .284(2) .543(6) .061(2) .002(8) Uiso No No H16a .388(3) .237(5) .136(3) .074(12) Uiso No No H16b .319(4) .348(7) .177(3) .103(17) Uiso No No H16c .288(4) .196(6) .169(3) .092(14) Uiso No No H17a .177(5) -.023(8) -.008(4) .045(15) Uiso No No H17b .287(6) -.021(10) -.040(5) .06(2) Uiso No No H17c .266(4) -.023(7) .057(4) .030(13) 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 N21 .0495(9) .0359(8) .0444(8) -.0024(7) -.0017(7) -.0055(7) N22 .0419(8) .0401(8) .0425(8) -.0021(6) .0040(6) -.0026(6) C23 .0449(9) .0334(8) .0446(9) .0014(7) .0005(7) -.0006(7) C24 .0410(9) .0354(8) .0456(9) .0022(7) -.0008(7) .0003(7) C25 .0470(9) .0371(9) .0443(9) .0051(7) -.0004(7) -.0006(8) C26 .0663(14) .0570(13) .0527(12) -.0027(11) .0049(10) -.0141(10) C27 .0463(11) .0640(14) .0628(13) -.0108(10) -.0014(9) .0024(11) C28 .0696(14) .0606(13) .0484(11) .0056(11) .0102(10) -.0073(10) N12 .0486(8) .0382(9) .0374(7) -.0027(7) -.0017(6) -.0019(7) C13 .0385(8) .0437(10) .0408(9) .0019(7) .0030(7) .0033(7) C14 .0359(11) .0355(13) .0481(13) .00000 .0055(10) .00000 C16 .0635(14) .0688(15) .0490(12) .0089(11) -.0086(10) .0082(11) C17 .073(2) .0382(16) .080(2) .00000 .017(2) .00000 _cod_database_code 2002947