#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/20/00/2200030.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_2200030 loop_ _publ_author_name 'Ohba, Shigeru' 'Yamada, Naoki' 'Eishima, Makoto' _publ_section_title ;trans-Dinitro(1,4,8,11-tetraazacyclotetradecane-N,N',N'',N''')cobalt(III) perchlorate ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m12 _journal_page_last m13 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Co (N O2)2 (C10 H24 N4)] Cl O4' _chemical_formula_moiety 'C10 H24 Co N6 O4 1+, Cl O4 1-' _chemical_formula_structural '(Co (C10 H24 N4) (N O2)2) (Cl O4)' _chemical_formula_sum 'C10 H24 Cl Co N6 O8' _chemical_formula_weight 450.72 _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.299(3) _cell_length_b 19.8200(10) _cell_length_c 6.6531(7) _cell_measurement_reflns_used 25 _cell_measurement_temperature 297.0(10) _cell_measurement_theta_max 13.9 _cell_measurement_theta_min 10.3 _cell_volume 1753.7(4) _computing_cell_refinement WinAFC _computing_data_collection ; WinAFC (Rigaku Corporation, 1999) ; _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1999)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material TEXSAN _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _diffrn_measurement_device_type 'Rigaku AFC-7R' _diffrn_measurement_method \q-2\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .024 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_number 3312 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 2.5 _diffrn_standards_decay_% none _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.19 _exptl_absorpt_correction_T_max .942 _exptl_absorpt_correction_T_min .752 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(Coppens et al., 1965)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.707 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_size_max .40 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .05 _refine_diff_density_max .41 _refine_diff_density_min -.55 _refine_ls_abs_structure_details '(Flack, 1983), 225 Friedel pairs' _refine_ls_abs_structure_Flack -.05(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.08 _refine_ls_hydrogen_treatment constr _refine_ls_number_parameters 271 _refine_ls_number_reflns 2554 _refine_ls_R_factor_gt .035 _refine_ls_shift/su_max .001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.0410P)^2^+3.4475P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .108 _reflns_number_gt 2245 _reflns_number_total 2554 _reflns_threshold_expression I>2\s(I)' _[local]_cod_data_source_file cf6015.cif _[local]_cod_data_source_block I _[local]_cod_chemical_formula_sum_orig 'C10 H24 Cl Co N6 O8 ' _cod_original_cell_volume 1753.7(5) _cod_database_code 2200030 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Co1 -.02236(4) -.12630(3) .22719(9) .0289(2) Uani d . 1.00 . . Co Cl2 .04200(10) .11990(8) .5995(2) .0561(4) Uani d . 1.00 . . Cl O3 -.0563(7) -.0715(6) .6010(10) .091(3) Uani d P .65 . . O O4 -.1886(7) -.1029(7) .484(2) .111(4) Uani d P .65 . . O O5 -.115(2) -.1351(10) .602(2) .094(6) Uani d P .35 . . O O6 -.122(2) -.0389(7) .490(3) .083(5) Uani d P .35 . . O O7 .0728(8) -.2147(4) -.035(2) .082(3) Uani d P .65 . . O O8 .0746(9) -.1180(5) -.1410(10) .086(3) Uani d P .65 . . O O9 .1360(10) -.1390(10) -.063(3) .097(8) Uani d P .35 . . O O10 .012(2) -.1886(10) -.141(2) .094(6) Uani d P .35 . . O O11 -.0280(6) .1258(3) .7629(9) .121(2) Uani d . 1.00 . . O O12 .1098(5) .1723(4) .6130(10) .147(3) Uani d . 1.00 . . O O13 -.0134(4) .1254(3) .4198(8) .098(2) Uani d . 1.00 . . O O14 .0907(5) .0566(3) .6113(9) .091(2) Uani d . 1.00 . . O N15 -.0993(4) -.0967(3) .4640(7) .0400(10) Uani d . 1.00 . . N N16 .0528(4) -.1568(2) -.0097(7) .0380(10) Uani d . 1.00 . . N N17 .0690(3) -.1740(2) .4135(7) .0360(10) Uani d . 1.00 . . N N18 .0546(3) -.0406(2) .2455(7) .0389(9) Uani d . 1.00 . . N N19 -.1121(4) -.0776(3) .0406(7) .0420(10) Uani d . 1.00 . . N N20 -.0977(3) -.2124(2) .2146(7) .0389(10) Uani d . 1.00 . . N C21 .1780(5) -.1618(4) .3980(10) .055(2) Uani d . 1.00 . . C C22 .2027(5) -.0879(4) .4230(10) .055(2) Uani d . 1.00 . . C C23 .1662(4) -.0437(3) .2570(10) .056(2) Uani d . 1.00 . . C C24 .0189(6) .0057(3) .0850(10) .057(2) Uani d . 1.00 . . C C25 -.0924(6) -.0033(3) .0640(10) .061(2) Uani d . 1.00 . . C C26 -.2200(6) -.0942(4) .0310(10) .064(2) Uani d . 1.00 . . C C27 -.2376(5) -.1691(4) .0080(10) .068(2) Uani d . 1.00 . . C C28 -.2083(4) -.2118(4) .1840(10) .058(2) Uani d . 1.00 . . C C29 -.0667(5) -.2544(3) .3890(10) .050(2) Uani d . 1.00 . . C C30 .0446(5) -.2484(3) .4090(10) .053(2) Uani d . 1.00 . . C H17 .0505 -.1590 .5441 .0438 Uiso calc . 1.00 . . H H18 .0338 -.0204 .3682 .0467 Uiso calc . 1.00 . . H H19 -.0872 -.0884 -.0894 .0508 Uiso calc . 1.00 . . H H20 -.0716 -.2351 .1003 .0466 Uiso calc . 1.00 . . H H21A .2008 -.1765 .2704 .0661 Uiso calc . 1.00 . . H H21B .2113 -.1867 .5006 .0661 Uiso calc . 1.00 . . H H22A .2738 -.0835 .4311 .0659 Uiso calc . 1.00 . . H H22B .1733 -.0726 .5450 .0659 Uiso calc . 1.00 . . H H23A .1913 -.0606 .1332 .0670 Uiso calc . 1.00 . . H H23B .1912 .0007 .2781 .0670 Uiso calc . 1.00 . . H H24A .0513 -.0049 -.0380 .0683 Uiso calc . 1.00 . . H H24B .0335 .0510 .1213 .0683 Uiso calc . 1.00 . . H H25A -.1158 .0202 -.0516 .0736 Uiso calc . 1.00 . . H H25B -.1258 .0133 .1797 .0736 Uiso calc . 1.00 . . H H26A -.2491 -.0715 -.0801 .0773 Uiso calc . 1.00 . . H H26B -.2514 -.0794 .1518 .0773 Uiso calc . 1.00 . . H H27A -.2002 -.1841 -.1048 .0813 Uiso calc . 1.00 . . H H27B -.3073 -.1759 -.0158 .0813 Uiso calc . 1.00 . . H H28A -.2307 -.2567 .1616 .0698 Uiso calc . 1.00 . . H H28B -.2396 -.1945 .3017 .0698 Uiso calc . 1.00 . . H H29A -.0848 -.3002 .3665 .0599 Uiso calc . 1.00 . . H H29B -.0987 -.2387 .5079 .0599 Uiso calc . 1.00 . . H H30A .0770 -.2693 .2985 .0632 Uiso calc . 1.00 . . H H30B .0663 -.2692 .5307 .0632 Uiso calc . 1.00 . . 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 Co1 .0312(3) .0309(3) .0246(3) .0012(3) .0035(3) .0001(3) Cl2 .0669(10) .0504(8) .0509(8) .0029(8) -.0089(7) .0043(8) O3 .090(7) .141(9) .042(4) -.036(7) .019(5) -.037(5) O4 .060(6) .190(10) .085(7) .000(7) .027(5) -.063(8) O5 .120(10) .110(10) .049(8) .010(10) .049(10) .026(10) O6 .12(2) .046(8) .080(10) .029(10) .050(10) -.001(8) O7 .110(8) .053(5) .084(7) .031(5) .051(6) -.003(5) O8 .147(10) .064(5) .048(5) -.003(7) .045(6) .003(4) O9 .070(10) .16(2) .060(10) -.030(10) .019(9) -.050(10) O10 .12(2) .110(10) .052(8) -.050(10) .030(10) -.040(9) O11 .206(7) .075(3) .082(4) .036(5) .052(5) -.001(4) O12 .107(5) .114(5) .222(9) -.049(4) -.058(6) .062(6) O13 .106(4) .120(5) .069(3) .027(5) -.028(3) .000(3) O14 .109(4) .074(3) .091(4) .037(3) -.009(4) -.005(3) N15 .044(3) .042(3) .034(2) -.001(2) .010(2) .001(2) N16 .039(2) .044(3) .030(2) .000(2) .005(2) -.003(2) N17 .037(2) .039(2) .033(2) -.003(2) .002(2) .002(2) N18 .047(2) .040(2) .030(2) -.005(2) .009(2) .000(2) N19 .042(3) .052(3) .033(2) .013(2) .002(2) .001(2) N20 .034(2) .048(2) .034(2) -.005(2) .005(2) -.007(2) C21 .034(3) .078(4) .053(4) .006(3) -.008(3) .005(4) C22 .036(3) .076(4) .053(4) -.012(3) -.002(3) .000(4) C23 .050(3) .069(4) .048(4) -.023(3) .010(4) -.004(4) C24 .084(4) .036(3) .051(3) -.004(3) .010(4) .009(3) C25 .085(5) .042(3) .056(4) .022(3) .003(4) .011(3) C26 .043(4) .084(5) .067(5) .021(4) -.009(3) -.003(4) C27 .039(3) .087(5) .077(5) -.001(4) -.016(4) -.007(5) C28 .038(3) .075(4) .061(4) -.017(3) .005(3) -.009(4) C29 .061(4) .035(3) .054(4) -.012(3) -.002(3) .009(3) C30 .060(4) .043(3) .055(4) .006(3) -.005(3) .013(3) 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 Co1 N15 . . 1.968(5) no Co1 N16 . . 1.962(5) no Co1 N17 . . 1.976(4) no Co1 N18 . . 1.986(4) no Co1 N19 . . 1.974(5) no Co1 N20 . . 1.981(4) no Cl2 O11 . . 1.436(7) no Cl2 O12 . . 1.379(7) no Cl2 O13 . . 1.409(6) no Cl2 O14 . . 1.414(6) no O3 N15 . . 1.180(10) no O4 N15 . . 1.200(10) no O5 N15 . . 1.21(2) no O6 N15 . . 1.20(2) no O7 N16 . . 1.189(10) no O8 N16 . . 1.200(10) no O9 N16 . . 1.21(2) no O10 N16 . . 1.21(2) no N17 C21 . . 1.473(8) no N17 C30 . . 1.511(8) no N17 H17 . . .950 no N18 C23 . . 1.487(7) no N18 C24 . . 1.484(8) no N18 H18 . . .950 no N19 C25 . . 1.504(9) no N19 C26 . . 1.474(9) no N19 H19 . . .950 no N20 C28 . . 1.485(7) no N20 C29 . . 1.487(8) no N20 H20 . . .950 no C21 C22 . . 1.510(10) no C21 H21A . . .950 no C21 H21B . . .950 no C22 C23 . . 1.492(10) no C22 H22A . . .950 no C22 H22B . . .950 no C23 H23A . . .950 no C23 H23B . . .950 no C24 C25 . . 1.500(10) no C24 H24A . . .950 no C24 H24B . . .950 no C25 H25A . . .950 no C25 H25B . . .950 no C26 C27 . . 1.510(10) no C26 H26A . . .950 no C26 H26B . . .950 no C27 C28 . . 1.500(10) no C27 H27A . . .950 no C27 H27B . . .950 no C28 H28A . . .951 no C28 H28B . . .950 no C29 C30 . . 1.492(10) no C29 H29A . . .950 no C29 H29B . . .950 no C30 H30A . . .950 no C30 H30B . . .951 no loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .003 .002 ;International Tables for Crystallography (1992, Vol. C) ; H H .000 .000 ;International Tables for Crystallography (1992, Vol. C) ; Cl Cl .148 .159 ;International Tables for Crystallography (1992, Vol. C) ; Co Co .349 .972 ;International Tables for Crystallography (1992, Vol. C) ; N N .006 .003 ;International Tables for Crystallography (1992, Vol. C) ; O O .011 .006 ;International Tables for Crystallography (1992, Vol. C) ; loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N15 Co1 N16 1_555 1_555 179.1(2) no N15 Co1 N17 1_555 1_555 87.7(2) no N15 Co1 N18 1_555 1_555 87.9(2) no N15 Co1 N19 1_555 1_555 92.5(2) no N15 Co1 N20 1_555 1_555 91.6(2) no N16 Co1 N17 1_555 1_555 92.5(2) no N16 Co1 N18 1_555 1_555 92.9(2) no N16 Co1 N19 1_555 1_555 87.3(2) no N16 Co1 N20 1_555 1_555 87.6(2) no N17 Co1 N18 1_555 1_555 93.1(2) no N17 Co1 N19 1_555 1_555 179.1(2) no N17 Co1 N20 1_555 1_555 85.7(2) no N18 Co1 N19 1_555 1_555 86.1(2) no N18 Co1 N20 1_555 1_555 178.7(2) no N19 Co1 N20 1_555 1_555 95.1(2) no O11 Cl2 O12 1_555 1_555 108.3(5) no O11 Cl2 O13 1_555 1_555 107.3(4) no O11 Cl2 O14 1_555 1_555 109.1(4) no O12 Cl2 O13 1_555 1_555 109.8(5) no O12 Cl2 O14 1_555 1_555 111.4(4) no O13 Cl2 O14 1_555 1_555 110.8(4) no Co1 N15 O3 1_555 1_555 119.3(6) no Co1 N15 O4 1_555 1_555 124.8(7) no Co1 N15 O5 1_555 1_555 120.7(10) no Co1 N15 O6 1_555 1_555 122.3(10) no O3 N15 O4 1_555 1_555 115.9(8) no O5 N15 O6 1_555 1_555 116.0(10) no Co1 N16 O7 1_555 1_555 121.7(6) no Co1 N16 O8 1_555 1_555 120.6(6) no Co1 N16 O9 1_555 1_555 127.0(10) no Co1 N16 O10 1_555 1_555 120.8(10) no O7 N16 O8 1_555 1_555 117.5(8) no O9 N16 O10 1_555 1_555 110.0(10) no Co1 N17 C21 1_555 1_555 118.9(4) no Co1 N17 C30 1_555 1_555 108.9(4) no Co1 N17 H17 1_555 1_555 105.4 no C21 N17 C30 1_555 1_555 111.7(5) no C21 N17 H17 1_555 1_555 105.4 no C30 N17 H17 1_555 1_555 105.4 no Co1 N18 C23 1_555 1_555 118.9(3) no Co1 N18 C24 1_555 1_555 108.6(4) no Co1 N18 H18 1_555 1_555 105.2 no C23 N18 C24 1_555 1_555 112.4(5) no C23 N18 H18 1_555 1_555 105.3 no C24 N18 H18 1_555 1_555 105.2 no Co1 N19 C25 1_555 1_555 108.0(4) no Co1 N19 C26 1_555 1_555 120.4(4) no Co1 N19 H19 1_555 1_555 104.6 no C25 N19 C26 1_555 1_555 113.1(5) no C25 N19 H19 1_555 1_555 104.6 no C26 N19 H19 1_555 1_555 104.6 no Co1 N20 C28 1_555 1_555 120.0(4) no Co1 N20 C29 1_555 1_555 108.0(3) no Co1 N20 H20 1_555 1_555 104.9 no C28 N20 C29 1_555 1_555 112.7(5) no C28 N20 H20 1_555 1_555 104.9 no C29 N20 H20 1_555 1_555 104.9 no N17 C21 C22 1_555 1_555 111.4(5) no N17 C21 H21A 1_555 1_555 109.0 no N17 C21 H21B 1_555 1_555 108.9 no C22 C21 H21A 1_555 1_555 109.0 no C22 C21 H21B 1_555 1_555 109.0 no H21A C21 H21B 1_555 1_555 109.5 no C21 C22 C23 1_555 1_555 114.7(6) no C21 C22 H22A 1_555 1_555 108.1 no C21 C22 H22B 1_555 1_555 108.2 no C23 C22 H22A 1_555 1_555 108.1 no C23 C22 H22B 1_555 1_555 108.2 no H22A C22 H22B 1_555 1_555 109.4 no N18 C23 C22 1_555 1_555 112.7(5) no N18 C23 H23A 1_555 1_555 108.7 no N18 C23 H23B 1_555 1_555 108.7 no C22 C23 H23A 1_555 1_555 108.6 no C22 C23 H23B 1_555 1_555 108.6 no H23A C23 H23B 1_555 1_555 109.5 no N18 C24 C25 1_555 1_555 108.2(5) no N18 C24 H24A 1_555 1_555 109.8 no N18 C24 H24B 1_555 1_555 109.8 no C25 C24 H24A 1_555 1_555 109.8 no C25 C24 H24B 1_555 1_555 109.8 no H24A C24 H24B 1_555 1_555 109.4 no N19 C25 C24 1_555 1_555 107.3(5) no N19 C25 H25A 1_555 1_555 110.0 no N19 C25 H25B 1_555 1_555 110.0 no C24 C25 H25A 1_555 1_555 110.0 no C24 C25 H25B 1_555 1_555 110.0 no H25A C25 H25B 1_555 1_555 109.4 no N19 C26 C27 1_555 1_555 112.0(6) no N19 C26 H26A 1_555 1_555 108.9 no N19 C26 H26B 1_555 1_555 108.9 no C27 C26 H26A 1_555 1_555 108.8 no C27 C26 H26B 1_555 1_555 108.8 no H26A C26 H26B 1_555 1_555 109.5 no C26 C27 C28 1_555 1_555 115.8(7) no C26 C27 H27A 1_555 1_555 107.9 no C26 C27 H27B 1_555 1_555 107.9 no C28 C27 H27A 1_555 1_555 107.8 no C28 C27 H27B 1_555 1_555 107.8 no H27A C27 H27B 1_555 1_555 109.5 no N20 C28 C27 1_555 1_555 111.6(5) no N20 C28 H28A 1_555 1_555 108.9 no N20 C28 H28B 1_555 1_555 108.9 no C27 C28 H28A 1_555 1_555 109.0 no C27 C28 H28B 1_555 1_555 109.0 no H28A C28 H28B 1_555 1_555 109.4 no N20 C29 C30 1_555 1_555 107.6(5) no N20 C29 H29A 1_555 1_555 109.9 no N20 C29 H29B 1_555 1_555 110.0 no C30 C29 H29A 1_555 1_555 110.0 no C30 C29 H29B 1_555 1_555 110.0 no H29A C29 H29B 1_555 1_555 109.4 no N17 C30 C29 1_555 1_555 107.0(5) no N17 C30 H30A 1_555 1_555 110.1 no N17 C30 H30B 1_555 1_555 110.1 no C29 C30 H30A 1_555 1_555 110.2 no C29 C30 H30B 1_555 1_555 110.1 no H30A C30 H30B 1_555 1_555 109.4 no _cod_database_fobs_code 2200030 _journal_paper_doi 10.1107/S1600536800018778