#------------------------------------------------------------------------------ #$Date: 2015-01-23 14:30:19 +0200 (Fri, 23 Jan 2015) $ #$Revision: 130086 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/00/80/2008094.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_2008094 loop_ _publ_author_name 'Marzotto, Armando' 'Clemente, Dore Augusto' 'Valle, Giovanni' _publ_section_title ; Cobalt(II) complexes of piperazine and derivatives: 1-methylpiperazin-4-ium trichloro(1-methylpiperazine-N^4^)cobaltate(II) ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 43 _journal_page_last 46 _journal_paper_doi 10.1107/S0108270198009603 _journal_volume 55 _journal_year 1999 _chemical_formula_iupac (C~5~H~13~N~2~)[CoCl~3~(C~5~H~12~N~2~)] _chemical_formula_moiety 'C5 H13 N2 1+ , C5 H12 Cl3 Co N2 1-' _chemical_formula_structural '(C5 H13 N2) (Co Cl3 (C5 H12 N2) )' _chemical_formula_sum 'C10 H25 Cl3 Co N4' _chemical_formula_weight 366.62 _chemical_name_systematic ; N-Methylpiperazinium Trichloro(N-methylpiperazine-N^1^)cobaltate(II) ; _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 'SHELXL and manual form' _cell_angle_alpha 103.20(3) _cell_angle_beta 108.60(4) _cell_angle_gamma 91.40(3) _cell_formula_units_Z 2 _cell_length_a 8.956(2) _cell_length_b 11.760(3) _cell_length_c 8.781(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 20 _cell_measurement_theta_min 14 _cell_volume 848.6(4) _computing_cell_refinement 'Pavia University Philips PW1100/20 software' _computing_data_collection 'Philips PW1100/20 software' _computing_data_reduction 'RIFLUP80 (Biagini Cingi et al., 1980)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'PARST (Nardelli, 1995)' _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1985)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Philips PW1100/20 diffractometer' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed X-ray tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI 0.026 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 4102 _diffrn_reflns_theta_max 28.01 _diffrn_reflns_theta_min 2.41 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.474 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_type 'semi-empirical via \y scans (North et al., 1968)' _exptl_crystal_colour 'light blue' _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_meas ? _exptl_crystal_description parallelepiped _exptl_crystal_F_000 382 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.679 _refine_diff_density_min -0.432 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.073 _refine_ls_goodness_of_fit_obs 1.097 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 163 _refine_ls_number_reflns 4102 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.073 _refine_ls_restrained_S_obs 1.097 _refine_ls_R_factor_all 0.055 _refine_ls_R_factor_obs 0.033 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.0554P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.097 _refine_ls_wR_factor_obs 0.086 _reflns_number_observed 3096 _reflns_number_total 4102 _reflns_observed_criterion I>2\s(I) _[local]_cod_data_source_file na1379.cif _[local]_cod_data_source_block car1 _cod_depositor_comments ; The following automatic conversions were performed: '_chemical_melting_point' value 'not measured' was changed to '?' - the value is undefined or not given. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_original_cell_volume 848.6(3) _cod_database_code 2008094 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 0.0338(2) 0.0350(2) 0.0359(2) 0.00507(11) 0.01161(12) 0.00604(12) Cl1 0.0513(3) 0.0411(3) 0.0365(3) 0.0085(2) 0.0127(2) 0.0035(2) Cl2 0.0495(4) 0.0376(3) 0.0787(5) 0.0122(3) 0.0127(3) 0.0100(3) Cl3 0.0672(4) 0.0610(4) 0.0577(4) -0.0002(3) 0.0385(3) 0.0128(3) N1 0.0348(9) 0.0337(9) 0.0278(8) 0.0040(7) 0.0107(7) 0.0054(7) N2 0.0328(9) 0.0413(10) 0.0312(9) 0.0064(7) 0.0091(7) 0.0089(8) N3 0.0436(10) 0.0354(9) 0.0417(10) 0.0040(8) 0.0182(8) 0.0085(8) N4 0.0424(10) 0.0361(9) 0.0377(10) 0.0015(8) 0.0173(8) 0.0084(8) C1 0.0428(12) 0.0319(10) 0.0350(11) 0.0092(9) 0.0113(9) 0.0030(9) C2 0.0429(12) 0.0339(11) 0.0367(11) 0.0008(9) 0.0073(9) 0.0029(9) C3 0.0432(12) 0.0373(11) 0.0378(12) 0.0117(9) 0.0162(10) 0.0074(9) C4 0.0407(11) 0.0302(10) 0.0333(11) 0.0043(8) 0.0120(9) 0.0020(8) C5 0.0343(12) 0.070(2) 0.0465(14) 0.0037(11) 0.0064(10) 0.0132(13) C6 0.0356(11) 0.0418(12) 0.0415(12) -0.0013(9) 0.0116(9) 0.0087(10) C7 0.0399(12) 0.0419(12) 0.0417(12) 0.0067(9) 0.0152(10) 0.0136(10) C8 0.0393(12) 0.0490(13) 0.0443(13) -0.0046(10) 0.0146(10) 0.0089(11) C9 0.0371(12) 0.0577(15) 0.0413(13) 0.0085(10) 0.0135(10) 0.0149(11) C10 0.078(2) 0.0403(13) 0.053(2) 0.0025(13) 0.0280(14) 0.0063(12) 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 0.85428(3) 0.71353(3) 0.23134(4) 0.03537(10) Uani d . 1 . Co Cl1 0.78880(7) 0.58350(5) -0.01739(7) 0.04444(15) Uani d . 1 . Cl Cl2 0.78474(8) 0.89181(5) 0.20455(10) 0.0580(2) Uani d . 1 . Cl Cl3 0.76149(9) 0.62545(6) 0.39317(9) 0.0581(2) Uani d . 1 . Cl N1 1.0967(2) 0.73520(15) 0.3388(2) 0.0324(4) Uani d . 1 . N H1 1.1384(2) 0.75688(15) 0.2665(2) 0.039 Uiso calc PR 0.85 . H N2 1.3787(2) 0.7321(2) 0.6171(2) 0.0355(4) Uani d . 1 . N H2 1.3296(2) 0.7104(2) 0.6838(2) 0.043 Uiso calc PR 0.25 . H N3 1.2706(2) 0.6459(2) 0.8474(2) 0.0394(4) Uani d . 1 . N HN3A 1.2753(2) 0.5683(2) 0.8129(2) 0.047 Uiso calc R 1 . H HN3B 1.2944(2) 0.6813(2) 0.7761(2) 0.047 Uiso calc PR 0.75 . H N4 1.2117(2) 0.8328(2) 1.0893(2) 0.0380(4) Uani d . 1 . N H4 1.1907(2) 0.7879(2) 1.1532(2) 0.046 Uiso calc PR 0.15 . H C1 1.1476(3) 0.8296(2) 0.4936(3) 0.0378(5) Uani d . 1 . C H1A 1.0941(3) 0.8127(2) 0.5674(3) 0.057 Uiso calc R 1 . H H1B 1.1161(3) 0.9032(2) 0.4680(3) 0.057 Uiso calc R 1 . H C2 1.3249(3) 0.8428(2) 0.5814(3) 0.0404(5) Uani d . 1 . C H2A 1.3788(3) 0.8670(2) 0.5123(3) 0.061 Uiso calc R 1 . H H2B 1.3520(3) 0.9033(2) 0.6844(3) 0.061 Uiso calc R 1 . H C3 1.3375(3) 0.6407(2) 0.4609(3) 0.0390(5) Uani d . 1 . C H3A 1.3722(3) 0.5671(2) 0.4840(3) 0.058 Uiso calc R 1 . H H3B 1.3918(3) 0.6625(2) 0.3906(3) 0.058 Uiso calc R 1 . H C4 1.1606(3) 0.6249(2) 0.3713(3) 0.0358(5) Uani d . 1 . C H4A 1.1371(3) 0.5667(2) 0.2665(3) 0.054 Uiso calc R 1 . H H4B 1.1079(3) 0.5953(2) 0.4374(3) 0.054 Uiso calc R 1 . H C5 1.5510(3) 0.7470(3) 0.7018(3) 0.0521(6) Uani d . 1 . C H5A 1.5854(3) 0.6739(3) 0.7237(3) 0.078 Uiso calc R 1 . H H5B 1.5769(3) 0.8060(3) 0.8045(3) 0.078 Uiso calc R 1 . H H5C 1.6031(3) 0.7708(3) 0.6323(3) 0.078 Uiso calc R 1 . H C6 1.1063(3) 0.6671(2) 0.8460(3) 0.0403(5) Uani d . 1 . C H6A 1.0740(3) 0.6188(2) 0.9083(3) 0.060 Uiso calc R 1 . H H6B 1.0337(3) 0.6446(2) 0.7327(3) 0.060 Uiso calc R 1 . H C7 1.0977(3) 0.7943(2) 0.9209(3) 0.0402(5) Uani d . 1 . C H7A 1.1199(3) 0.8420(2) 0.8525(3) 0.060 Uiso calc R 1 . H H7B 0.9915(3) 0.8051(2) 0.9239(3) 0.060 Uiso calc R 1 . H C8 1.3710(3) 0.8184(2) 1.0825(3) 0.0447(5) Uani d . 1 . C H8A 1.4477(3) 0.8470(2) 1.1930(3) 0.067 Uiso calc R 1 . H H8B 1.3926(3) 0.8648(2) 1.0122(3) 0.067 Uiso calc R 1 . H C9 1.3886(3) 0.6915(2) 1.0154(3) 0.0448(5) Uani d . 1 . C H9A 1.4947(3) 0.6843(2) 1.0102(3) 0.067 Uiso calc R 1 . H H9B 1.3733(3) 0.6455(2) 1.0890(3) 0.067 Uiso calc R 1 . H C10 1.1984(4) 0.9562(2) 1.1603(4) 0.0565(7) Uani d . 1 . C H10A 1.0947(4) 0.9638(2) 1.1689(4) 0.085 Uiso calc R 1 . H H10B 1.2149(4) 1.0033(2) 1.0899(4) 0.085 Uiso calc R 1 . H H10C 1.2768(4) 0.9824(2) 1.2686(4) 0.085 Uiso calc R 1 . H loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Co Co 0.3494 0.9721 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -3 1 1 2 2 2 -2 3 2 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 N1 Co Cl2 105.53(6) yes N1 Co Cl1 108.83(7) yes Cl2 Co Cl1 111.30(4) yes N1 Co Cl3 105.66(6) yes Cl2 Co Cl3 119.06(4) yes Cl1 Co Cl3 106.02(4) yes C1 N1 C4 110.1(2) no C1 N1 Co 111.20(13) no C4 N1 Co 112.01(13) no C2 N2 C3 109.2(2) no C2 N2 C5 109.9(2) no C3 N2 C5 109.9(2) no C9 N3 C6 111.5(2) no C8 N4 C7 108.9(2) no C8 N4 C10 110.4(2) no C7 N4 C10 109.6(2) no N1 C1 C2 112.5(2) no N2 C2 C1 111.0(2) no N2 C3 C4 110.7(2) no N1 C4 C3 112.9(2) no N3 C6 C7 111.0(2) no N4 C7 C6 110.8(2) no N4 C8 C9 111.2(2) no N3 C9 C8 110.1(2) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co N1 . . 2.055(2) yes Co Cl2 . . 2.2438(9) yes Co Cl1 . . 2.2509(11) yes Co Cl3 . . 2.2730(9) yes N1 C1 . . 1.476(3) no N1 C4 . . 1.480(3) no N2 C2 . . 1.464(3) no N2 C3 . . 1.469(3) no N2 C5 . . 1.470(3) no N3 C9 . . 1.483(3) no N3 C6 . . 1.495(3) no N4 C8 . . 1.459(3) no N4 C7 . . 1.463(3) no N4 C10 . . 1.467(3) no C1 C2 . . 1.514(3) no C3 C4 . . 1.512(3) no C6 C7 . . 1.505(3) no C8 C9 . . 1.506(4) no 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 _geom_torsion_publ_flag N1 C1 C2 N2 -56.7(2) yes N2 C3 C4 N1 56.3(2) yes N3 C6 C7 N4 -56.2(3) yes N4 C8 C9 N3 58.3(3) yes