#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2011852.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_2011852 loop_ _publ_author_name 'Hubin, Timothy J.' 'Tyryshkin, Nickolay' 'Alcock, Nathaniel W.' 'Busch, Daryle H.' _publ_section_title ; trans-Dioxocyclam (1,4,8,11-tetraazacyclotetradecane-2,9-dione) dihydrate and its Ni^II^ complex ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 359 _journal_page_last 362 _journal_volume 57 _journal_year 2001 _chemical_formula_moiety 'C10 H20 N4 O2 , 2H2 O' _chemical_formula_sum 'C10 H24 N4 O4' _chemical_formula_weight 264.33 _chemical_name_systematic ; 1,4,8,11-tetraazacyclotetradecane-2,9-dione dihydrate ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _audit_creation_method SHELXTL _cell_angle_alpha 83.037(10) _cell_angle_beta 88.727(15) _cell_angle_gamma 79.806(10) _cell_formula_units_Z 1 _cell_length_a 4.869(3) _cell_length_b 7.530(5) _cell_length_c 9.150(5) _cell_measurement_reflns_used 1077 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 20 _cell_measurement_theta_min 3 _cell_volume 327.7(3) _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_collection 'SMART (Siemens, 1994)' _computing_data_reduction SAINT _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997b)' _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997a)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997a)' _diffrn_ambient_temperature 200(2) _diffrn_detector_area_resol_mean 8.192 _diffrn_measured_fraction_theta_full .970 _diffrn_measured_fraction_theta_max .970 _diffrn_measurement_device_type 'Siemens SMART CCD area-detector' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .018 _diffrn_reflns_av_sigmaI/netI .047 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 1627 _diffrn_reflns_theta_full 24.99 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_theta_min 2.24 _diffrn_standards_decay_% none _exptl_absorpt_coefficient_mu .103 _exptl_absorpt_correction_T_max .96 _exptl_absorpt_correction_T_min .58 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'prism AUTHOR: please specify what kind' _exptl_crystal_F_000 144 _exptl_crystal_size_max .48 _exptl_crystal_size_mid .10 _exptl_crystal_size_min .10 _refine_diff_density_max .18 _refine_diff_density_min -.24 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref .967 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 102 _refine_ls_number_reflns 1118 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all .967 _refine_ls_R_factor_all .066 _refine_ls_R_factor_gt .046 _refine_ls_shift/su_max .025 _refine_ls_shift/su_mean .002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.073P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .118 _reflns_number_gt 825 _reflns_number_total 1118 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bm1440.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M P-1 _cod_database_code 2011852 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 O1 .5423(3) .2685(2) .44403(15) .0340(4) Uani d . 1 O C1 .3047(4) .2498(3) .4106(2) .0238(5) Uani d . 1 C N2 .1230(4) .1947(2) .51042(19) .0254(4) Uani d . 1 N H2 -.054(5) .202(3) .479(3) .036(6) Uiso d . 1 H C3 .1882(4) .1570(3) .6668(2) .0271(5) Uani d . 1 C H3A .3912 .1129 .6793 .033 Uiso calc R 1 H H3B .0898 .0596 .7118 .033 Uiso calc R 1 H C4 .1038(4) .3241(3) .7458(2) .0269(5) Uani d . 1 C H4A .1868 .3005 .8456 .032 Uiso calc R 1 H H4B .1782 .4273 .6915 .032 Uiso calc R 1 H N5 -.2007(4) .3733(2) .7581(2) .0251(4) Uani d . 1 N H5A -.274(4) .384(3) .672(2) .028(6) Uiso d . 1 H C6 -.2931(4) .5413(3) .8254(2) .0261(5) Uani d . 1 C H6A -.2202 .5223 .9273 .031 Uiso calc R 1 H H6B -.4993 .5618 .8319 .031 Uiso calc R 1 H C7 -.2066(4) .7140(3) .7471(2) .0268(5) Uani d . 1 C H7A -.2868 .8185 .7998 .032 Uiso calc R 1 H H7B -.0009 .7013 .7495 .032 Uiso calc R 1 H O2 -.2756(5) .0943(3) .9866(2) .0480(5) Uani d . 1 O H2A -.291(6) .173(4) .909(3) .064(9) Uiso d . 1 H H2B -.43(2) .059(13) .988(12) .15(5) Uiso d P .50 H H2C -.120(9) .033(6) 1.002(5) .030(14) Uiso d P .50 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 O1 .0201(8) .0440(9) .0370(9) -.0073(6) -.0037(6) .0017(7) C1 .0202(11) .0197(10) .0297(12) .0012(8) .0000(8) -.0024(9) N2 .0221(9) .0266(10) .0276(10) -.0052(7) -.0010(7) -.0023(7) C3 .0274(11) .0236(11) .0287(12) -.0028(9) -.0005(9) .0012(9) C4 .0244(11) .0281(11) .0279(12) -.0055(8) -.0023(8) -.0005(9) N5 .0241(9) .0261(10) .0253(10) -.0056(7) -.0012(7) -.0014(8) C6 .0238(11) .0299(11) .0241(11) -.0036(9) .0023(8) -.0033(9) C7 .0268(11) .0239(11) .0301(12) -.0033(8) .0015(9) -.0066(9) O2 .0498(14) .0418(11) .0459(12) -.0043(10) .0047(10) .0144(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 '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_site_symmetry_3 _geom_angle O1 C1 N2 . . 122.49(19) O1 C1 C7 . 2_566 121.17(18) N2 C1 C7 . 2_566 116.33(17) C1 N2 C3 . . 122.27(18) N2 C3 C4 . . 111.94(16) N5 C4 C3 . . 111.71(16) C4 N5 C6 . . 113.66(15) N5 C6 C7 . . 116.61(16) C1 C7 C6 2_566 . 111.41(16) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance O1 C1 . 1.239(2) C1 N2 . 1.339(3) C1 C7 2_566 1.507(3) N2 C3 . 1.456(3) C3 C4 . 1.516(3) C4 N5 . 1.469(3) N5 C6 . 1.469(3) C6 C7 . 1.528(3) C7 C1 2_566 1.507(3) N2 H2A . .905(10) N5 H5A . .864(10) O2 H2A . .860(10) O2 H2B . .85(2) O2 H2C . .82(2)