#------------------------------------------------------------------------------ #$Date: 2025-08-19 07:12:48 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301798 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/14/2011499.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_2011499 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_paper_doi 10.1107/S0108270100011793 _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-(3-aminopropyl)-1,3-propanediamine]cobalt(III)' _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _cell_angle_alpha 90.00 _cell_angle_beta 94.267(14) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.8040(12) _cell_length_b 9.286(2) _cell_length_c 14.209(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293 _cell_measurement_theta_max 12.80 _cell_measurement_theta_min 7.94 _cell_volume 1290.0(4) _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 .0273 _diffrn_reflns_av_sigmaI/netI .0421 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2777 _diffrn_reflns_theta_max 26.46 _diffrn_reflns_theta_min 2.08 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 240 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.341 _exptl_absorpt_correction_T_max .625 _exptl_absorpt_correction_T_min .570 _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 1.628 _exptl_crystal_density_method 'not measured' _exptl_crystal_description brick _exptl_crystal_F_000 656 _exptl_crystal_size_max .65 _exptl_crystal_size_mid .45 _exptl_crystal_size_min .35 _refine_diff_density_max .311 _refine_diff_density_min -.227 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.025 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 240 _refine_ls_number_reflns 2664 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.025 _refine_ls_restrained_S_obs 1.139 _refine_ls_R_factor_all .0534 _refine_ls_R_factor_gt .0253 _refine_ls_shift/esd_mean .001 _refine_ls_shift/su_max .004 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0326P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all .0652 _refine_ls_wR_factor_ref .0603 _reflns_number_gt 1918 _reflns_number_total 2664 _reflns_threshold_expression I>2\s(I) _cod_data_source_file da1147.cif _cod_data_source_block III _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 1290.1(3) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2011499 _cod_database_fobs_code 2011499 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 .02707(14) .02442(14) .01605(13) -.00219(13) .00052(9) .00144(12) N1 .0342(11) .0297(10) .0243(9) -.0019(8) .0018(8) -.0006(8) N2 .0279(9) .0368(10) .0238(9) -.0026(8) -.0005(7) .0033(8) N3 .0447(11) .0282(10) .0210(9) .0010(9) .0013(9) .0021(8) N4 .0356(10) .0337(10) .0199(8) .0028(8) -.0019(7) .0005(8) N5 .0337(10) .0429(11) .0312(9) -.0028(9) .0109(8) -.0015(9) N6 .0643(14) .0354(11) .0255(9) -.0081(10) -.0101(9) .0058(9) N7 .0285(9) .0349(9) .0219(8) -.0042(8) -.0007(7) .0076(9) N8 .0724(15) .0455(12) .0253(10) -.0143(11) -.0028(9) -.0042(10) N9 .0338(11) .0466(12) .0478(12) .0004(10) .0128(9) .0178(10) N10 .0350(13) .138(3) .085(2) -.006(2) -.0066(12) .055(2) N11 .0325(9) .0391(10) .0226(8) .0100(9) .0021(7) .0050(9) N12 .0491(13) .0683(15) .0316(11) .0012(11) -.0114(9) -.0090(10) C1 .050(2) .0286(13) .0413(14) .0038(11) .0019(11) -.0007(11) C2 .0435(14) .0440(14) .0428(14) .0120(12) .0086(11) -.0066(12) C3 .0302(13) .052(2) .0480(15) .0071(12) .0030(11) .0036(13) C4 .0332(12) .054(2) .0392(13) -.0175(12) .0010(10) .0010(12) C5 .057(2) .0398(15) .047(2) -.0232(13) -.0003(13) .0062(12) C6 .057(2) .0289(13) .0400(14) -.0077(11) -.0054(12) -.0032(11) 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 .64854(3) .19033(3) .90649(2) .02257(9) Uani d . 1 . Co N1 .6185(2) -.0139(2) .87042(14) .0294(4) Uani d . 1 . N H1N .572(2) -.038(3) .9124(16) .033(7) Uiso d . 1 . H H2N .564(3) -.019(3) .8199(19) .053(8) Uiso d . 1 . H N2 .8349(2) .2054(2) .85703(12) .0296(4) Uani d . 1 . N H3N .811(2) .224(2) .7985(17) .033(6) Uiso d . 1 . H N3 .6433(2) .3906(2) .95173(14) .0314(4) Uani d . 1 . N H4N .587(3) .428(3) .9133(18) .040(7) Uiso d . 1 . H H5N .603(2) .383(2) 1.0023(17) .028(6) Uiso d . 1 . H N4 .5737(2) .2661(2) .78332(11) .0299(4) Uani d . 1 . N N5 .4639(2) .1808(2) .95258(13) .0355(4) Uani d . 1 . N N6 .7240(2) .1169(2) 1.02741(13) .0424(5) Uani d . 1 . N N7 .5558(2) .1866(2) .71736(11) .0286(4) Uani d . 1 . N N8 .5375(2) .1133(2) .65197(14) .0481(5) Uani d . 1 . N N9 .3671(2) .1827(2) .89611(14) .0422(5) Uani d . 1 . N N10 .2706(2) .1827(3) .8456(2) .0866(10) Uani d . 1 . N N11 .7901(2) .1813(2) 1.08625(12) .0314(4) Uani d . 1 . N N12 .8560(2) .2381(3) 1.14651(13) .0504(6) Uani d . 1 . N C1 .7341(3) -.1141(3) .8650(2) .0402(6) Uani d . 1 . C H1C .698(3) -.201(3) .8419(18) .049(7) Uiso d . 1 . H H2C .774(2) -.124(3) .9300(18) .043(7) Uiso d . 1 . H C2 .8431(3) -.0524(3) .8073(2) .0432(6) Uani d . 1 . C H3C .807(3) -.022(3) .7460(18) .043(7) Uiso d . 1 . H H4C .905(3) -.128(3) .7946(19) .062(8) Uiso d . 1 . H C3 .9177(2) .0714(3) .8548(2) .0435(6) Uani d . 1 . C H5C 1.002(3) .092(3) .8274(17) .047(7) Uiso d . 1 . H H6C .946(2) .048(3) .9159(18) .046(7) Uiso d . 1 . H C4 .9253(2) .3245(3) .8945(2) .0422(6) Uani d . 1 . C H7C 1.003(3) .321(3) .8579(18) .047(7) Uiso d . 1 . H H8C .954(3) .297(3) .9576(18) .046(7) Uiso d . 1 . H C5 .8581(3) .4699(3) .8899(2) .0483(7) Uani d . 1 . C H9C .925(3) .541(3) .8974(18) .052(7) Uiso d . 1 . H H10C .809(3) .482(3) .8319(19) .048(7) Uiso d . 1 . H C6 .7608(3) .4896(3) .9660(2) .0423(6) Uani d . 1 . C H11C .807(2) .467(3) 1.0262(17) .046(7) Uiso d . 1 . H H12C .723(2) .584(3) .9692(16) .044(7) Uiso d . 1 . H 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 N3 93.46(8) no N6 Co N5 89.37(8) yes N3 Co N5 83.53(8) no N6 Co N4 179.40(8) yes N3 Co N4 86.32(8) no N5 Co N4 91.16(8) yes N6 Co N1 86.11(8) no N3 Co N1 168.96(8) yes N5 Co N1 85.44(8) no N4 Co N1 94.22(8) no N6 Co N2 92.16(8) no N3 Co N2 95.43(8) no N5 Co N2 178.20(8) yes N4 Co N2 87.31(7) no N1 Co N2 95.61(7) no C1 N1 Co 121.23(15) no C1 N1 H1N 110.0(16) no Co N1 H1N 98.9(17) no C1 N1 H2N 110.8(18) no Co N1 H2N 109.7(18) no H1N N1 H2N 104(2) no C3 N2 C4 108.5(2) no C3 N2 Co 117.47(14) no C4 N2 Co 117.26(14) no C3 N2 H3N 104.9(15) no C4 N2 H3N 107.8(15) no Co N2 H3N 99.2(14) no C6 N3 Co 126.4(2) no C6 N3 H4N 107.9(17) no Co N3 H4N 102.1(17) no C6 N3 H5N 110.0(15) no Co N3 H5N 103.1(15) no H4N N3 H5N 105(2) no N7 N4 Co 119.82(14) yes N9 N5 Co 118.57(14) yes N11 N6 Co 126.9(2) yes N8 N7 N4 178.0(2) yes N10 N9 N5 176.6(2) yes N12 N11 N6 176.5(2) yes N1 C1 C2 111.6(2) no N1 C1 H1C 107.0(15) no C2 C1 H1C 113.9(16) no N1 C1 H2C 105.5(14) no C2 C1 H2C 107.3(14) no H1C C1 H2C 111(2) no C3 C2 C1 112.9(2) no C3 C2 H3C 108.6(15) no C1 C2 H3C 112.0(15) no C3 C2 H4C 110.9(17) no C1 C2 H4C 107.9(17) no H3C C2 H4C 104(2) no N2 C3 C2 113.7(2) no N2 C3 H5C 109.3(15) no C2 C3 H5C 112.1(14) no N2 C3 H6C 108.0(16) no C2 C3 H6C 110.2(16) no H5C C3 H6C 103(2) no N2 C4 C5 113.9(2) no N2 C4 H7C 104.8(15) no C5 C4 H7C 112.1(14) no N2 C4 H8C 105.2(15) no C5 C4 H8C 112.2(15) no H7C C4 H8C 108(2) no C4 C5 C6 112.2(2) no C4 C5 H9C 109.5(16) no C6 C5 H9C 108.0(16) no C4 C5 H10C 110.1(15) no C6 C5 H10C 107.7(16) no H9C C5 H10C 109(2) no N3 C6 C5 110.9(2) no N3 C6 H11C 107.5(15) no C5 C6 H11C 109.4(14) no N3 C6 H12C 106.1(14) no C5 C6 H12C 114.6(15) no H11C C6 H12C 108(2) no 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 . 1.943(2) yes Co N3 . 1.970(2) yes Co N5 . 1.973(2) yes Co N4 . 1.976(2) yes Co N1 . 1.981(2) yes Co N2 . 2.010(2) yes N1 C1 . 1.473(3) no N1 H1N . .81(2) no N1 H2N . .86(3) no N2 C3 . 1.487(3) no N2 C4 . 1.491(3) no N2 H3N . .86(2) no N3 C6 . 1.476(3) no N3 H4N . .82(3) no N3 H5N . .85(2) no N4 N7 . 1.196(2) yes N5 N9 . 1.196(3) yes N6 N11 . 1.182(2) yes N7 N8 . 1.155(2) yes N9 N10 . 1.145(3) yes N11 N12 . 1.160(3) yes C1 C2 . 1.508(3) no C1 H1C . .93(3) no C1 H2C . .98(2) no C2 C3 . 1.497(4) no C2 H3C . .96(2) no C2 H4C . .95(3) no C3 H5C . .96(3) no C3 H6C . .92(3) no C4 C5 . 1.501(4) no C4 H7C . .96(3) no C4 H8C . .95(3) no C5 C6 . 1.505(4) no C5 H9C . .93(3) no C5 H10C . .93(3) no C6 H11C . .96(2) no C6 H12C . .95(2) no loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 168307741