#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2205087.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2205087 loop_ _publ_author_name 'Battle, Andrew R.' 'Johnson, Daniel L.' 'Martin, Lisandra L.' _publ_section_title ; 1,4,7-Triazacyclononane hemihydrate ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o330 _journal_page_last o332 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac 'C6 H15 N3, 0.5H2 O' _chemical_formula_moiety 'C6 H15 N3, 0.5H2 O' _chemical_formula_sum 'C6 H16 N3 O0.5' _chemical_formula_weight 138.22 _chemical_name_systematic '1,4,7-triazacyclononane hemihydrate' _space_group_IT_number 165 _symmetry_cell_setting trigonal _symmetry_space_group_name_Hall '-P 3 2"c' _symmetry_space_group_name_H-M 'P -3 c 1' _audit_creation_method 'WinGX routine CIF_UPDATE' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 4 _cell_length_a 7.2980(10) _cell_length_b 7.2980(10) _cell_length_c 16.560(3) _cell_measurement_reflns_used 7794 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 27.86 _cell_measurement_theta_min 4.06 _cell_volume 763.8(2) _computing_cell_refinement 'SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_collection 'COLLECT (Hooft, 2000)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) and SCALEPACK' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 123 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 7794 _diffrn_reflns_theta_full 27.5 _diffrn_reflns_theta_max 27.86 _diffrn_reflns_theta_min 4.06 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.202 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 308 _exptl_crystal_size_max 0.87 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _refine_diff_density_max 0.317 _refine_diff_density_min -0.189 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 50 _refine_ls_number_reflns 610 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.118 _refine_ls_R_factor_gt 0.0485 _refine_ls_shift/su_max 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0781P)^2^+0.2454P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.1398 _reflns_number_gt 523 _reflns_number_total 610 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file is6022.cif _[local]_cod_data_source_block I _[local]_cod_chemical_formula_sum_orig 'C6 H16 N3 O0.50' _cod_database_code 2205087 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'y, x, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-y, -x, z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol C1 0.1191(2) 0.4022(2) 0.14760(8) 0.0280(4) Uani d . 1 C N1 0.27316(19) 0.41635(19) 0.08734(6) 0.0254(4) Uani d . 1 N C2 0.0008(2) 0.5138(2) 0.11820(8) 0.0273(4) Uani d . 1 C H4 -0.090(3) 0.517(3) 0.1643(11) 0.034(4) Uiso d . 1 H H5 -0.097(3) 0.431(3) 0.0739(10) 0.033(4) Uiso d . 1 H H3 0.189(3) 0.463(3) 0.2011(9) 0.029(4) Uiso d . 1 H H2 0.011(3) 0.249(3) 0.1587(12) 0.037(5) Uiso d . 1 H H1 0.218(5) 0.282(6) 0.0559(18) 0.089(9) Uiso d . 1 H O1 0 0 0 0.0944(16) Uani d SP 1 O 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 C1 0.0268(7) 0.0289(7) 0.0257(7) 0.0120(6) 0.0054(5) 0.0044(5) N1 0.0260(7) 0.0272(6) 0.0231(6) 0.0134(5) 0.0015(4) -0.0003(4) C2 0.0230(7) 0.0297(8) 0.0275(7) 0.0119(6) 0.0014(5) -0.0012(6) O1 0.120(3) 0.120(3) 0.0433(19) 0.0600(13) 0 0 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle _geom_angle_publ_flag N1 C1 C2 . 111.22(11) y N1 C1 H3 . 111.4(10) n C2 C1 H3 . 109.9(10) n N1 C1 H2 . 110.4(11) n C2 C1 H2 . 107.9(11) n H3 C1 H2 . 105.7(14) n C2 N1 C1 2_665 115.40(11) y C2 N1 H1 2_665 111.2(19) n C1 N1 H1 . 111.6(18) n N1 C2 C1 3_565 112.70(11) y N1 C2 H4 3_565 111.2(10) n C1 C2 H4 . 108.8(10) n N1 C2 H5 3_565 107.5(11) n C1 C2 H5 . 109.8(12) n H4 C2 H5 . 106.7(16) n loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 N1 . 1.4681(18) y C1 C2 . 1.533(2) y C1 H3 . 1.009(16) n C1 H2 . 1.01(2) n N1 C2 2_665 1.4636(19) y N1 H1 . 1.00(4) n C2 N1 3_565 1.4636(19) n C2 H4 . 1.021(18) n C2 H5 . 0.992(17) n loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_4 _geom_torsion C2 C1 N1 C2 2_665 130.77(12) N1 C1 C2 N1 3_565 -49.02(15)