#------------------------------------------------------------------------------
#$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/2200030.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_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_
_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
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_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