#------------------------------------------------------------------------------ #$Date: 2008-01-26 17:25:03 +0000 (Sat, 26 Jan 2008) $ #$Revision: 20 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003341.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_2003341 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 738 _journal_page_last 741 _publ_section_title ; 1,4,7-Triazatricyclo[5.2.1.0^4.10^]decane at 100 K ; _chemical_formula_moiety 'C7 H13 N3' _chemical_formula_sum 'C7 H13 N3' _chemical_formula_structural 'C7 H13 N3' _chemical_formula_weight 139.20 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _symmetry_space_group_name_H-M 'P 21/n' _cell_length_a 6.027(3) _cell_length_b 11.177(3) _cell_length_c 10.715(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.03(4) _cell_angle_gamma 90.00 _cell_volume 716.3(5) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.291 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 15 _cell_measurement_theta_min 13 _cell_measurement_theta_max 16 _exptl_absorpt_coefficient_mu 0.082 _cell_measurement_temperature 100.0(2) _exptl_crystal_description Cylinder _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_colour Colourless _chemical_compound_source ; Reaction of 1,4,7-triazacyclononane with (MeO)~2~CHNMe~2~. A clear oil was obtained by vacuum distillation. ; _diffrn_measurement_device 'Stoe Stadi-4 four-circle diffractometer' _diffrn_measurement_method ; \w-2\q scans with on-line profile analysis (Clegg, 1981) ; _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 1262 _reflns_number_total 1262 _reflns_number_observed 927 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0607 _refine_ls_wR_factor_obs 0.1578 _refine_ls_wR_factor_all 0.1920 _refine_ls_goodness_of_fit_obs 1.044 _refine_ls_goodness_of_fit_all 1.029 _refine_ls_number_reflns 1253 _refine_ls_number_parameters 144 _refine_ls_hydrogen_treatment refall _refine_ls_weighting_scheme ;calc w = 1/[\s^2^(F~o~^2^) + (0.1173P)^2^ + 0.5530P] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_shift/esd_max 0.020 _refine_diff_density_max 0.302 _refine_diff_density_min -0.302 _refine_ls_extinction_method 'F~c~^*^ = kF~c~[1 + 0.001\xF~c~^2^\l^3^/sin(2\ _refine_ls_extinction_coef 0.0168(95) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0033 0.001 'N' 'N' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0061 0.003 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.000 loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv N(1) 1 0.0024(4) 0.7501(2) 0.7766(2) 0.0236(6) C(2) 1 -0.0625(5) 0.6394(2) 0.8383(3) 0.0261(7) H2A 1 -0.2322(55) 0.6350(26) 0.8301(29) 0.025(8) H2B 1 -0.0012(45) 0.6438(24) 0.9254(28) 0.016(7) C(3) 1 0.0472(4) 0.5392(2) 0.7706(3) 0.0227(7) H3A 1 0.0718(53) 0.4655(31) 0.8260(30) 0.034(8) H3B 1 -0.0422(46) 0.5227(23) 0.6900(25) 0.014(6) N(4) 1 0.2631(3) 0.5929(2) 0.7498(2) 0.0214(6) C(5) 1 0.3380(5) 0.5590(2) 0.6289(3) 0.0245(7) H5A 1 0.5047(51) 0.5662(26) 0.6323(27) 0.022(7) H5B 1 0.3084(51) 0.4760(29) 0.6068(28) 0.026(7) C(6) 1 0.2195(5) 0.6460(2) 0.5342(3) 0.0231(7) H6A 1 0.3035(61) 0.6535(31) 0.4593(34) 0.044(10) H6B 1 0.0601(49) 0.6258(24) 0.5021(26) 0.016(6) N(7) 1 0.2266(4) 0.7592(2) 0.6070(2) 0.0199(6) C(8) 1 0.0254(4) 0.8340(2) 0.5790(3) 0.0224(7) H8A 1 -0.0273(48) 0.8366(24) 0.4947(30) 0.018(7) H8B 1 0.0598(46) 0.9147(28) 0.6102(27) 0.020(7) C(9) 1 -0.1406(5) 0.7793(3) 0.6587(3) 0.0272(7) H9A 1 -0.2520(61) 0.8344(32) 0.6793(33) 0.039(9) H9B 1 -0.2033(46) 0.7051(27) 0.6197(26) 0.017(7) C(10) 1 0.2240(4) 0.7232(2) 0.7391(2) 0.0199(7) H10 1 0.3376(49) 0.7633(27) 0.7984(26) 0.022(7) 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 N(1) 0.0293(13) 0.0017(9) 0.0124(9) 0.0187(12) 0.0003(9) 0.0250(12) C(2) 0.032(2) 0.0000(11) 0.0139(12) 0.0212(15) 0.0005(11) 0.0273(15) C(3) 0.0251(14) -0.0025(11) 0.0071(11) 0.0178(13) 0.0013(11) 0.0261(14) N(4) 0.0239(11) -0.0006(9) 0.0077(9) 0.0139(12) 0.0012(8) 0.0275(12) C(5) 0.0263(15) -0.0005(11) 0.0126(11) 0.0155(13) -0.0014(11) 0.034(2) C(6) 0.0297(15) -0.0011(11) 0.0107(11) 0.0189(14) -0.0020(10) 0.0226(14) N(7) 0.0241(12) 0.0002(8) 0.0067(9) 0.0150(11) 0.0008(9) 0.0217(12) C(8) 0.0260(14) 0.0022(11) 0.0026(11) 0.0193(14) 0.0006(11) 0.0220(14) C(9) 0.0234(15) 0.0062(11) 0.0095(12) 0.024(2) -0.0011(12) 0.035(2) C(10) 0.0236(14) -0.0017(10) 0.0047(10) 0.0150(13) -0.0004(10) 0.0217(13)