#------------------------------------------------------------------------------ #$Date: 2013-08-29 16:37:19 +0100 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/14/2011498.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_2011498 loop_ _publ_author_name 'Chun, Hyungphil' 'Bernal, Ivan' _publ_section_title ; Triazidocobalt(III) complexes with tridentate amine ligands ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1326 _journal_page_last 1329 _journal_volume 56 _journal_year 2000 _chemical_formula_iupac '[Co(C6 H17 N3 )(N3 )3 ]' _chemical_formula_moiety 'C6 H17 Co N12' _chemical_formula_sum 'C6 H17 Co N12' _chemical_formula_weight 316.25 _chemical_name_systematic ' Triazido[N,N-(2-aminoethyl)-methyl-1,3-propanediamine]cobalt(III)' _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _cell_angle_alpha 90.00 _cell_angle_beta 91.65(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.560(3) _cell_length_b 9.404(2) _cell_length_c 16.149(4) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293 _cell_measurement_theta_max 12.65 _cell_measurement_theta_min 8.14 _cell_volume 1299.4(6) _computing_cell_refinement CAD-4-PC _computing_data_collection 'CAD-4-PC (Enraf-Nonius, 1989)' _computing_data_reduction 'NRCVAX DATRD2 (Le Page & Gabe, 1979)' _computing_molecular_graphics 'ORTEPIII (Burnett & Johnson, 1996)' _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 293 _diffrn_measurement_device_type 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .0191 _diffrn_reflns_av_sigmaI/netI .0230 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2357 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_min 2.51 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 240 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.331 _exptl_absorpt_correction_T_max .756 _exptl_absorpt_correction_T_min .654 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(NRCVAX ABSORP; Gabe et al., 1989)' _exptl_crystal_colour 'dark green' _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_description brick _exptl_crystal_F_000 656 _exptl_crystal_size_max .50 _exptl_crystal_size_mid .48 _exptl_crystal_size_min .21 _refine_diff_density_max .340 _refine_diff_density_min -.218 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.045 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 240 _refine_ls_number_reflns 2278 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.045 _refine_ls_restrained_S_obs 1.118 _refine_ls_R_factor_all .0341 _refine_ls_R_factor_gt .0221 _refine_ls_shift/esd_mean .001 _refine_ls_shift/su_max -.009 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0364P)^2^+0.0998P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all .0599 _refine_ls_wR_factor_ref .0569 _reflns_number_gt 1851 _reflns_number_total 2278 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file da1147.cif _[local]_cod_data_source_block II _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 1299.5(7) _cod_database_code 2011498 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' 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 Co .02504(14) .02436(14) .02689(14) -.00089(10) .00001(9) -.00342(10) N1 .0338(10) .0421(11) .0343(9) .0041(8) -.0069(7) -.0096(8) N2 .0327(8) .0248(8) .0294(8) -.0012(6) .0032(6) -.0019(6) N3 .0347(9) .0322(9) .0298(8) .0014(8) .0008(7) .0004(8) N4 .0326(9) .0377(9) .0398(9) .0072(7) -.0064(7) -.0110(7) N5 .0408(10) .0514(11) .0492(11) -.0148(9) .0145(8) -.0162(9) N6 .0357(9) .0255(9) .0443(10) -.0027(7) .0060(7) -.0057(7) N7 .0350(9) .0293(8) .0312(8) -.0012(7) .0031(7) -.0039(7) N8 .0413(10) .0504(12) .0546(12) .0118(9) -.0110(9) .0011(9) N9 .0295(8) .0369(10) .0515(12) -.0027(7) .0027(8) .0025(8) N10 .073(2) .094(2) .0488(13) -.0159(14) .0152(12) .0076(12) N11 .0346(8) .0304(10) .0315(8) .0036(7) -.0007(7) -.0005(7) N12 .0548(12) .0282(10) .0680(13) -.0064(8) .0031(10) .0067(9) C1 .0572(14) .0503(14) .0294(11) .0084(11) -.0047(10) .0048(10) C2 .0505(12) .0415(12) .0298(10) -.0007(10) .0058(9) .0022(9) C3 .0277(10) .0456(12) .0450(12) -.0029(9) .0056(9) -.0022(10) C4 .0304(11) .064(2) .0483(13) .0036(11) -.0063(9) -.0027(11) C5 .0434(12) .0474(14) .0388(12) .0116(10) -.0084(9) .0036(10) C6 .0558(15) .0285(11) .0484(13) -.0102(10) .0112(11) -.0049(10) 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_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol Co .03654(3) .21659(3) .129815(14) .02545(9) Uani d . 1 . Co N1 .1369(2) .1907(2) .23898(11) .0369(4) Uani d . 1 . N H1N .228(3) .171(3) .2373(15) .047(7) Uiso d . 1 . H H2N .125(3) .270(3) .2643(16) .054(7) Uiso d . 1 . H N2 -.1460(2) .1064(2) .17558(9) .0289(3) Uani d . 1 . N N3 -.0723(2) .2358(2) .02167(10) .0322(4) Uani d . 1 . N H3N -.022(3) .290(3) -.0076(15) .049(7) Uiso d . 1 . H H4N -.066(3) .157(3) .0010(14) .045(7) Uiso d . 1 . H N4 .1332(2) .0445(2) .08478(10) .0368(4) Uani d . 1 . N N5 .2200(2) .3255(2) .09835(12) .0469(5) Uani d . 1 . N N6 -.0586(2) .3906(2) .17103(10) .0351(4) Uani d . 1 . N N7 .2525(2) .0014(2) .11699(10) .0318(4) Uani d . 1 . N N8 .3665(2) -.0440(2) .14558(12) .0490(5) Uani d . 1 . N N9 .2622(2) .3255(2) .02904(12) .0393(4) Uani d . 1 . N N10 .3094(3) .3287(3) -.03648(14) .0718(7) Uani d . 1 . N N11 .0008(2) .5048(2) .16284(10) .0322(4) Uani d . 1 . N N12 .0501(2) .6180(2) .15798(13) .0503(5) Uani d . 1 . N C1 .0519(3) .0842(3) .28720(14) .0457(5) Uani d . 1 . C H1C .087(3) -.011(3) .2670(15) .052(7) Uiso d . 1 . H H2C .067(3) .095(3) .3452(16) .065(8) Uiso d . 1 . H C2 -.1194(3) .1086(3) .26746(12) .0405(5) Uani d . 1 . C H3C -.151(2) .207(2) .2868(12) .034(5) Uiso d . 1 . H H4C -.183(3) .037(3) .2936(14) .045(6) Uiso d . 1 . H C3 -.3013(2) .1745(3) .15721(14) .0393(5) Uani d . 1 . C H5C -.301(2) .271(2) .1814(13) .035(5) Uiso d . 1 . H H6C -.379(3) .122(3) .1851(14) .049(6) Uiso d . 1 . H C4 -.3417(3) .1866(3) .06548(15) .0479(6) Uani d . 1 . C H7C -.339(2) .091(3) .0421(13) .037(6) Uiso d . 1 . H H8C -.443(4) .225(3) .0593(17) .068(8) Uiso d . 1 . H C5 -.2376(3) .2839(3) .01880(14) .0433(5) Uani d . 1 . C H9C -.236(3) .378(3) .0381(15) .051(7) Uiso d . 1 . H H10C -.270(3) .290(3) -.0402(16) .053(7) Uiso d . 1 . H C6 -.1569(3) -.0446(2) .1478(2) .0440(5) Uani d . 1 . C H11C -.160(2) -.047(2) .0870(13) .037(6) Uiso d . 1 . H H12C -.063(3) -.099(3) .1724(14) .053(7) Uiso d . 1 . H H13C -.257(3) -.080(3) .1675(15) .061(7) Uiso d . 1 . H 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 Co N6 . 1.953(2) yes Co N1 . 1.954(2) yes Co N5 . 1.955(2) yes Co N3 . 1.964(2) yes Co N4 . 1.966(2) yes Co N2 . 2.032(2) yes N1 C1 . 1.474(3) no N1 H1N . .81(3) no N1 H2N . .86(3) no N2 C6 . 1.492(3) no N2 C2 . 1.495(2) no N2 C3 . 1.497(3) no N3 C5 . 1.485(3) no N3 H3N . .83(3) no N3 H4N . .82(3) no N4 N7 . 1.203(2) yes N5 N9 . 1.186(3) yes N6 N11 . 1.196(2) yes N7 N8 . 1.150(2) yes N9 N10 . 1.144(3) yes N11 N12 . 1.149(2) yes C1 C2 . 1.509(3) no C1 H1C . 1.00(3) no C1 H2C . .95(3) no C2 H3C . 1.01(2) no C2 H4C . .97(2) no C3 C4 . 1.516(3) no C3 H5C . .99(2) no C3 H6C . .96(2) no C4 C5 . 1.496(3) no C4 H7C . .98(2) no C4 H8C . .94(3) no C5 H9C . .94(3) no C5 H10C . .99(3) no C6 H11C . .98(2) no C6 H12C . 1.02(2) no C6 H13C . .98(3) no 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' Co Co .3494 .9721 '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 _geom_angle_publ_flag N6 Co N1 88.50(8) no N6 Co N5 89.73(7) yes N1 Co N5 87.94(9) no N6 Co N3 91.97(7) no N1 Co N3 177.15(8) yes N5 Co N3 94.87(8) no N6 Co N4 178.11(7) yes N1 Co N4 93.00(8) no N5 Co N4 89.17(8) yes N3 Co N4 86.59(7) no N6 Co N2 88.32(7) no N1 Co N2 86.06(7) no N5 Co N2 173.73(7) yes N3 Co N2 91.15(7) no N4 Co N2 92.94(7) no C1 N1 Co 110.50(13) no C1 N1 H1N 110.6(18) no Co N1 H1N 113.6(17) no C1 N1 H2N 105.7(17) no Co N1 H2N 105.4(17) no H1N N1 H2N 111(2) no C6 N2 C2 108.5(2) no C6 N2 C3 107.4(2) no C2 N2 C3 107.5(2) no C6 N2 Co 114.70(13) no C2 N2 Co 104.92(12) no C3 N2 Co 113.44(12) no C5 N3 Co 118.88(14) no C5 N3 H3N 107.8(17) no Co N3 H3N 108.9(17) no C5 N3 H4N 109.9(17) no Co N3 H4N 104.2(16) no H3N N3 H4N 107(2) no N7 N4 Co 118.58(13) yes N9 N5 Co 120.93(15) yes N11 N6 Co 122.11(13) yes N8 N7 N4 177.4(2) yes N10 N9 N5 176.7(2) yes N12 N11 N6 175.5(2) yes N1 C1 C2 106.1(2) no N1 C1 H1C 105.9(14) no C2 C1 H1C 111.6(13) no N1 C1 H2C 112.9(17) no C2 C1 H2C 107.4(16) no H1C C1 H2C 113(2) no N2 C2 C1 109.1(2) no N2 C2 H3C 106.5(11) no C1 C2 H3C 109.7(12) no N2 C2 H4C 110.7(13) no C1 C2 H4C 110.9(13) no H3C C2 H4C 109.9(17) no N2 C3 C4 113.7(2) no N2 C3 H5C 108.9(12) no C4 C3 H5C 108.3(12) no N2 C3 H6C 108.1(14) no C4 C3 H6C 111.0(13) no H5C C3 H6C 106.6(19) no C5 C4 C3 114.6(2) no C5 C4 H7C 110.3(13) no C3 C4 H7C 107.5(12) no C5 C4 H8C 105.9(17) no C3 C4 H8C 108.4(17) no H7C C4 H8C 110(2) no N3 C5 C4 112.2(2) no N3 C5 H9C 105.6(15) no C4 C5 H9C 114.5(15) no N3 C5 H10C 106.7(14) no C4 C5 H10C 111.6(14) no H9C C5 H10C 105.7(19) no N2 C6 H11C 108.8(13) no N2 C6 H12C 108.3(14) no H11C C6 H12C 111.8(18) no N2 C6 H13C 105.8(15) no H11C C6 H13C 108.8(19) no H12C C6 H13C 113(2) no _cod_database_fobs_code 2011498