#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2204367.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_2204367 _space_group_IT_number 12 _symmetry_space_group_name_Hall '-C 2y' _symmetry_space_group_name_H-M 'C 1 2/m 1' _[local]_cod_cif_authors_sg_H-M 'C 2/m' loop_ _publ_author_name 'S\"anger, Inge' 'Lerner, Hans-Wolfram' 'Bolte, Michael' _publ_section_title ; Redetermination of trans-2,5,7,10-tetraazabicyclo[4.4.0]decane ; _journal_issue 10 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first o1847 _journal_page_last o1848 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac 'C6 H14 N4' _chemical_formula_moiety 'C6 H14 N4' _chemical_formula_sum 'C6 H14 N4' _chemical_formula_weight 142.21 _chemical_name_systematic ; trans-2,5,7,10-tetraazabicyclo[4.4.0]decane ; _symmetry_cell_setting monoclinic _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 108.78(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 5.283(2) _cell_length_b 15.937(4) _cell_length_c 4.6205(18) _cell_measurement_reflns_used 2510 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.7 _cell_measurement_theta_min 4.2 _cell_volume 368.3(2) _computing_cell_refinement X-AREA _computing_data_collection 'X-AREA (Stoe & Cie, 2001)' _computing_data_reduction X-AREA _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997) ' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990) ' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Stoe IPDS-II two-circle' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0685 _diffrn_reflns_av_sigmaI/netI 0.0802 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_number 2406 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 27.81 _diffrn_reflns_theta_min 4.27 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_description rod _exptl_crystal_F_000 156 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _refine_diff_density_max 0.261 _refine_diff_density_min -0.272 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 45 _refine_ls_number_reflns 449 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.994 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0499 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0894P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1387 _refine_ls_wR_factor_ref 0.1444 _reflns_number_gt 362 _reflns_number_total 449 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file lh6274.cif loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' 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 0.0000 0.0000 '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' 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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol N1 0.1960(3) 0.42558(6) 0.8009(2) 0.0312(5) Uani d . 1 . . N H1' 0.356(8) 0.4282(14) 0.877(7) 0.030(10) Uiso d P 0.54(4) A 1 H H1'' 0.062(6) 0.4260(13) 0.890(6) 0.013(9) Uiso d P 0.46(4) A 2 H C1 0.1446(3) 0.5000 0.6067(3) 0.0277(5) Uani d S 1 . . C H1 0.268(4) 0.5000 0.479(4) 0.023(4) Uiso d S 1 . . H C2 0.1424(2) 0.34970(8) 0.6111(3) 0.0341(5) Uani d . 1 . . C H2A 0.168(4) 0.2997(10) 0.740(4) 0.039(4) Uiso d . 1 . . H H2B 0.283(3) 0.3459(9) 0.500(4) 0.035(4) Uiso d . 1 . . H 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 N1 0.0308(8) 0.0329(7) 0.0247(7) 0.0010(3) 0.0018(5) 0.0016(3) C1 0.0259(9) 0.0318(9) 0.0222(9) 0.000 0.0035(7) 0.000 C2 0.0353(8) 0.0311(7) 0.0310(8) 0.0030(4) 0.0041(5) 0.0011(4) 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 N1 C1 . 1.4591(13) y N1 C2 . 1.4669(14) y N1 H1' . 0.80(4) ? N1 H1'' . 0.93(3) ? C1 N1 6_565 1.4590(13) ? C1 C1 5_566 1.528(3) ? C1 H1 . 1.011(19) ? C2 C2 2_556 1.524(2) ? C2 H2A . 0.977(17) ? C2 H2B . 1.031(16) ? 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_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 N1 C2 . . 109.91(10) y C1 N1 H1' . . 100.8(18) ? C2 N1 H1' . . 106.0(18) ? C1 N1 H1'' . . 104.5(14) ? C2 N1 H1'' . . 104.1(14) ? H1' N1 H1'' . . 131(3) ? N1 C1 N1 6_565 . 108.77(13) y N1 C1 C1 6_565 5_566 110.26(10) ? N1 C1 C1 . 5_566 110.25(10) y N1 C1 H1 6_565 . 109.3(5) ? N1 C1 H1 . . 109.3(5) ? C1 C1 H1 5_566 . 108.9(10) ? N1 C2 C2 . 2_556 111.18(9) y N1 C2 H2A . . 110.3(9) ? C2 C2 H2A 2_556 . 108.8(11) ? N1 C2 H2B . . 108.3(9) ? C2 C2 H2B 2_556 . 112.2(8) ? H2A C2 H2B . . 105.9(13) ? 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 N1 C1 N1 6_565 179.27(7) C2 N1 C1 C1 5_566 58.26(19) C1 N1 C2 C2 2_556 -56.40(18) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N1 H1' N1 2_657 0.80(4) 2.36(4) 3.146(3) 167(3) N1 H1'' N1 2_557 0.93(3) 2.27(3) 3.182(3) 168(2)