#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2006661.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_2006661 loop_ _publ_author_name 'Sosa-Torres, M. E.' 'Toscano, R. A.' _publ_section_title ; trans-Dichloro(1,4,8,11-tetrazacyclotetradecane)cobalt(III) Chloride Tetrahydrate 0.47-Hydrochloride ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1585 _journal_page_last 1588 _journal_volume 53 _journal_year 1997 _chemical_formula_iupac '[Co Cl2 (C10 H24 N4)] Cl, 4H2 O1, 0.47H1 Cl1' _chemical_formula_moiety '(C10 H24 Cl2 Co N4 1+), Cl 1-, 4H2 O1, 0.47H1 Cl1' _chemical_formula_sum 'C10 H32.47 Cl3.47 Co N4 O4' _chemical_formula_weight 454.81 _chemical_name_common ; trans-Dichlorocyclamcobalt(III) chloride, tetrahydrate, 0.47(HCl) ; _chemical_name_systematic ; trans-Dichloro-(1,4,8,11-tetraazacyclotetradecane)cobalt(III) chloride, tetrahydrate, 0.47 HCl ; _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' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.97(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 6.393(2) _cell_length_b 7.4330(10) _cell_length_c 21.067(3) _cell_measurement_reflns_used 44 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 15.00 _cell_measurement_theta_min 4.00 _cell_volume 1000.9(4) _computing_cell_refinement XSCANS _computing_data_collection 'XSCANS (Siemens, 1993)' _computing_data_reduction XSCANS _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1990)' _computing_publication_material SHELXL93 _computing_structure_refinement SHELXL93 _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Siemens P4/PC diffractometer' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 3155 _diffrn_reflns_theta_max 30.00 _diffrn_reflns_theta_min 1.50 _diffrn_standards_decay_% 2.5 _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.340 _exptl_absorpt_correction_T_max 0.460 _exptl_absorpt_correction_T_min 0.346 _exptl_absorpt_correction_type '\y scans (XEMP; Siemens, 1990)' _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 477 _exptl_crystal_size_max 0.82 _exptl_crystal_size_mid 0.62 _exptl_crystal_size_min 0.58 _refine_diff_density_max 0.605 _refine_diff_density_min -0.975 _refine_ls_extinction_coef 0.084(4) _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)' _refine_ls_goodness_of_fit_all 1.072 _refine_ls_goodness_of_fit_obs 1.098 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 159 _refine_ls_number_reflns 2912 _refine_ls_number_restraints 5 _refine_ls_restrained_S_all 1.127 _refine_ls_restrained_S_obs 1.100 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_obs 0.0413 _refine_ls_shift/esd_max -0.040 _refine_ls_shift/esd_mean 0.004 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.0509P)^2^+0.2907P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.1101 _refine_ls_wR_factor_obs 0.0948 _reflns_number_observed 2297 _reflns_number_total 2914 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file fg1254.cif _[local]_cod_data_source_block cocyclam _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_database_code 2006661 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 0.0135(2) 0.0212(2) 0.0289(2) 0.00316(13) 0.00015(12) -0.00136(15) Cl1 0.0198(2) 0.0282(3) 0.0483(3) 0.0076(2) 0.0001(2) -0.0016(2) Cl2 0.0530(7) 0.0737(9) 0.0734(8) -0.0007(5) 0.0046(5) -0.0164(6) N1 0.0191(7) 0.0271(9) 0.0427(11) 0.0018(7) 0.0018(7) -0.0019(8) C2 0.0295(11) 0.0365(13) 0.055(2) 0.0003(10) -0.0075(10) -0.0153(11) C3 0.0325(11) 0.0479(14) 0.0395(13) 0.0040(11) -0.0077(10) -0.0115(11) N4 0.0247(8) 0.0360(10) 0.0313(9) 0.0068(7) -0.0005(7) -0.0022(8) C5 0.0429(13) 0.051(2) 0.0353(13) 0.0086(12) 0.0021(11) 0.0088(11) C6 0.0404(13) 0.050(2) 0.052(2) -0.0009(12) 0.0136(12) 0.0180(13) C7 0.0315(11) 0.0272(11) 0.063(2) -0.0001(9) 0.0055(11) 0.0088(11) O1 0.0537(15) 0.080(2) 0.078(2) 0.0112(14) 0.0087(13) 0.001(2) O2 0.075(2) 0.080(2) 0.096(2) -0.014(2) 0.007(2) 0.004(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_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Co 0.5000 0.0000 0.5000 0.02120(10) Uani d S 1 Co Cl1 0.23878(7) 0.20309(7) 0.49486(3) 0.0321(2) Uani d . 1 Cl Cl2 0.1763(2) 0.2511(2) 0.68061(6) 0.0666(5) Uani d P 0.734(4) Cl N1 0.7152(3) 0.1904(3) 0.50221(10) 0.0296(4) Uani d . 1 N H1 0.825(5) 0.132(4) 0.4972(13) 0.036 Uiso d . 1 H C2 0.7181(4) 0.2728(4) 0.56615(14) 0.0403(6) Uani d . 1 C H2A 0.605(5) 0.352(5) 0.5683(14) 0.048 Uiso d . 1 H H2B 0.843(5) 0.336(5) 0.5735(15) 0.048 Uiso d . 1 H C3 0.6882(4) 0.1251(4) 0.61340(13) 0.0400(6) Uani d . 1 C H3A 0.802(5) 0.034(4) 0.6154(15) 0.048 Uiso d . 1 H H3B 0.664(5) 0.177(4) 0.6582(15) 0.048 Uiso d . 1 H N4 0.4982(3) 0.0222(3) 0.59369(9) 0.0307(4) Uani d . 1 N H4 0.392(5) 0.094(4) 0.6011(13) 0.037 Uiso d . 1 H C5 0.4729(4) -0.1408(4) 0.63270(13) 0.0430(6) Uani d . 1 C H5A 0.596(5) -0.216(5) 0.6286(15) 0.052 Uiso d . 1 H H5B 0.481(5) -0.104(5) 0.6762(16) 0.052 Uiso d . 1 H C6 0.2774(5) -0.2452(4) 0.61388(15) 0.0473(7) Uani d . 1 C H6A 0.151(6) -0.169(5) 0.6171(16) 0.057 Uiso d . 1 H H6B 0.262(6) -0.338(5) 0.6468(16) 0.057 Uiso d . 1 H C7 0.2843(4) -0.3275(3) 0.54865(14) 0.0405(6) Uani d . 1 C H7A 0.400(5) -0.393(5) 0.5456(14) 0.049 Uiso d . 1 H H7B 0.165(5) -0.414(5) 0.5411(15) 0.049 Uiso d . 1 H O1 -0.0108(4) -0.0838(5) 0.7420(2) 0.0704(8) Uani d D 1 O H1A 0.031(10) 0.023(7) 0.727(3) 0.084 Uiso d PD 0.74 H H1B -0.093(9) -0.046(9) 0.759(3) 0.084 Uiso d PD 0.74 H H1C 0.068(9) -0.116(9) 0.763(3) 0.084 Uiso d PD 0.74 H O2 0.8588(5) -0.4502(5) 0.6962(2) 0.0836(9) Uani d D 1 O H2C 0.942(8) -0.525(6) 0.691(3) 0.100 Uiso d D 1 H H2D 0.909(9) -0.370(7) 0.710(3) 0.100 Uiso d 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 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 Co N1 3_656 . 180.0 no N1 Co N4 3_656 . 93.86(8) no N1 Co N4 . . 86.14(8) yes N1 Co N4 3_656 3_656 86.14(8) no N1 Co N4 . 3_656 93.86(8) yes N4 Co N4 . 3_656 180.0 no N1 Co Cl1 3_656 . 87.92(6) no N1 Co Cl1 . . 92.08(6) yes N4 Co Cl1 . . 88.58(6) yes N4 Co Cl1 3_656 . 91.42(6) no N1 Co Cl1 3_656 3_656 92.08(6) no N1 Co Cl1 . 3_656 87.92(6) yes N4 Co Cl1 . 3_656 91.42(6) yes N4 Co Cl1 3_656 3_656 88.58(6) no Cl1 Co Cl1 . 3_656 180.0 no C7 N1 C2 3_656 . 112.0(2) no C7 N1 Co 3_656 . 119.2(2) no C2 N1 Co . . 108.4(2) no C7 N1 H1 3_656 . 105(2) no C2 N1 H1 . . 109(2) no Co N1 H1 . . 102(2) no N1 C2 C3 . . 107.6(2) no N1 C2 H2A . . 108(2) no C3 C2 H2A . . 109(2) no N1 C2 H2B . . 111(2) no C3 C2 H2B . . 112(2) no H2A C2 H2B . . 110(3) no N4 C3 C2 . . 107.7(2) no N4 C3 H3A . . 105(2) no C2 C3 H3A . . 115(2) no N4 C3 H3B . . 108(2) no C2 C3 H3B . . 111(2) no H3A C3 H3B . . 110(3) no C5 N4 C3 . . 111.3(2) no C5 N4 Co . . 119.3(2) no C3 N4 Co . . 107.6(2) no C5 N4 H4 . . 108(2) no C3 N4 H4 . . 105(2) no Co N4 H4 . . 104(2) no N4 C5 C6 . . 111.8(2) no N4 C5 H5A . . 109(2) no C6 C5 H5A . . 110(2) no N4 C5 H5B . . 107(2) no C6 C5 H5B . . 115(2) no H5A C5 H5B . . 103(3) no C7 C6 C5 . . 114.2(2) no C7 C6 H6A . . 109(2) no C5 C6 H6A . . 111(2) no C7 C6 H6B . . 111(2) no C5 C6 H6B . . 105(2) no H6A C6 H6B . . 105(3) no N1 C7 C6 3_656 . 112.5(2) no N1 C7 H7A 3_656 . 108(2) no C6 C7 H7A . . 109(2) no N1 C7 H7B 3_656 . 110(2) no C6 C7 H7B . . 112(2) no H7A C7 H7B . . 106(3) no H1A O1 H1B . . 93(6) yes H1A O1 H1C . . 108(7) yes H1B O1 H1C . . 111(8) yes H2C O2 H2D . . 110(6) yes 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 N1 3_656 1.974(2) no Co N1 . 1.974(2) yes Co N4 . 1.981(2) yes Co N4 3_656 1.981(2) no Co Cl1 . 2.2524(6) yes Co Cl1 3_656 2.2524(6) no N1 C7 3_656 1.478(3) no N1 C2 . 1.479(3) no N1 H1 . 0.84(3) no C2 C3 . 1.497(4) no C2 H2A . 0.93(3) no C2 H2B . 0.94(3) no C3 N4 . 1.489(3) no C3 H3A . 0.99(3) no C3 H3B . 1.03(3) no N4 C5 . 1.474(3) no N4 H4 . 0.88(3) no C5 C6 . 1.518(4) no C5 H5A . 0.97(3) no C5 H5B . 0.96(3) no C6 C7 . 1.506(5) no C6 H6A . 0.99(4) no C6 H6B . 0.98(3) no C7 N1 3_656 1.478(3) no C7 H7A . 0.89(3) no C7 H7B . 1.01(3) no O1 H1A . 0.89(5) no O1 H1B . 0.69(5) no O1 H1C . 0.70(5) no O2 H2C . 0.78(4) no O2 H2D . 0.73(4) no 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 _geom_hbond_publ_flag N1 H1 Cl1 1_655 0.84(3) 2.70(3) 3.355(2) 137(2) yes O1 H1A Cl2 . 0.89(5) 2.18(5) 3.058(4) 169(6) yes O1 H1B O2 2_556 0.69(5) 2.08(6) 2.779(5) 174(6) yes O1 H1C Cl2 2_546 0.70(5) 2.24(5) 2.936(3) 172(6) yes O2 H2C Cl2 1_645 0.78(4) 2.25(4) 3.030(4) 176(6) yes O2 H2D O1 1_655 0.73(4) 2.29(5) 3.002(5) 165(6) yes N4 H4 Cl2 . 0.88(3) 2.48(3) 3.257(2) 148(2) yes 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_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag N4 Co N1 C7 . . . 3_656 -143.2(2) no Cl1 Co N1 C7 . . . 3_656 -54.8(2) no Cl1 Co N1 C7 3_656 . . 3_656 125.2(2) no N4 Co N1 C2 . . . . -13.6(2) yes N4 Co N1 C2 3_656 . . . 166.4(2) no Cl1 Co N1 C2 . . . . 74.88(15) no Cl1 Co N1 C2 3_656 . . . -105.12(15) no C7 N1 C2 C3 3_656 . . . 172.5(2) no Co N1 C2 C3 . . . . 39.0(2) yes N1 C2 C3 N4 . . . . -52.2(3) yes C2 C3 N4 C5 . . . . 172.3(2) no C2 C3 N4 Co . . . . 39.9(2) yes N1 Co N4 C3 . . . . -14.7(2) yes N1 Co N4 C5 3_656 . . . 37.3(2) yes N1 Co N4 C5 . . . . -142.7(2) no Cl1 Co N4 C5 . . . . 125.1(2) no Cl1 Co N4 C5 3_656 . . . -54.9(2) no N1 Co N4 C3 3_656 . . . 165.3(2) no Cl1 Co N4 C3 . . . . -106.9(2) no Cl1 Co N4 C3 3_656 . . . 73.1(2) no C3 N4 C5 C6 . . . . 178.9(2) no Co N4 C5 C6 . . . . -54.9(3) yes N4 C5 C6 C7 . . . . 66.9(3) yes C5 C6 C7 N1 . . . 3_656 -66.9(3) yes Co N1 C7 C6 . 3_656 . . 54.6(3) yes N4 Co N1 C7 . . 3_656 . -36.8(2) yes