#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2011655.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_2011655
loop_
_publ_author_name
'Ohba, Shigeru'
'Eishima, Makoto'
_publ_section_title
;
 <i>trans</i>-Chlorobis(ethylenediamine-<i>N</i>,<i>N</i>')nitrocobalt(III)
 nitrate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              e557
_journal_page_last               e558
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '[Co Cl (N O2) (C2 H8 N2)2] (N O3)'
_chemical_formula_moiety         'C4 H16 Cl Co N5 O2 1+, N O3 1-'
_chemical_formula_structural     '[Co Cl (N O2) (C2 H8 N2)2] (N O3)'
_chemical_formula_sum            'C4 H16 Cl Co N6 O5'
_chemical_formula_weight         322.59
_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
_cell_angle_beta                 97.060(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.601(2)
_cell_length_b                   12.721(2)
_cell_length_c                   14.0720(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298.0(10)
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      13.9
_cell_volume                     1172.7(4)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1993)
;
_computing_data_reduction
;TEXSAN
(Molecular Structure Corporation, 1999)
;
_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  .006
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            2930
_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    1.714
_exptl_absorpt_correction_T_max  .710
_exptl_absorpt_correction_T_min  .605
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            orange--red
_exptl_crystal_density_diffrn    1.827
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .5
_exptl_crystal_size_min          .2
_refine_diff_density_max         .75
_refine_diff_density_min         -.67
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.10
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     205
_refine_ls_number_reflns         2703
_refine_ls_R_factor_gt           .032
_refine_ls_shift/su_max          .001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.0406P)^2^+1.0531P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .082
_reflns_number_gt                2494
_reflns_number_total             2703
_reflns_threshold_expression     I>2\s(I)
_[local]_cod_data_source_file    qa0452.cif
_[local]_cod_data_source_block   I
_[local]_cod_cif_authors_sg_H-M  'P 21/c'
_[local]_cod_chemical_formula_sum_orig 'C4 H16 Cl Co N6 O5 '
_cod_original_cell_volume        1172.7(3)
_cod_database_code               2011655
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,1/2+y,1/2-z
-x,-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 .20504(4) .09122(2) .26611(2) .02170(10) Uani d . 1.00 Co
Cl2 -.06500(10) -.02185(6) .24844(6) .0405(2) Uani d P .84 Cl
Cl3 .483(2) .2025(9) .2854(9) .07987(4) Uiso d P .16 Cl
O4 -.162(3) .014(2) .192(2) .05302(7) Uiso d P .08 O
O5 -.017(3) -.080(2) .3100(10) .03871(6) Uiso d P .08 O
O6 -.058(3) -.063(2) .1830(10) .04049(6) Uiso d P .08 O
O7 -.145(4) -.008(2) .313(2) .05620(8) Uiso d P .08 O
O8 .4166(4) .2698(2) .2378(2) .0572(7) Uani d P .84 O
O9 .5902(3) .1581(2) .3292(2) .0594(7) Uani d P .84 O
O10 .7948(8) .2587(6) .5971(4) .088(2) Uani d P .55 O
O11 .5011(9) .2926(4) .5229(3) .0700(10) Uani d P .55 O
O12 .5938(8) .1350(3) .5507(3) .0580(10) Uani d P .55 O
O13 .7070(10) .3287(4) .5609(5) .079(2) Uani d P .45 O
O14 .7962(9) .1782(4) .6064(4) .0630(10) Uani d P .45 O
O15 .4860(10) .2030(10) .5463(6) .140(5) Uani d P .45 O
N16 -.017(3) -.005(2) .2540(10) .2271(3) Uiso d P .16 N
N17 .4299(6) .1841(3) .2794(3) .0401(8) Uani d P .84 N
N18 .0249(3) .20670(10) .29270(10) .0290(4) Uani d . 1.00 N
N19 .2387(3) .0660(2) .40400(10) .0338(4) Uani d . 1.00 N
N20 .1680(3) .1158(2) .12750(10) .0330(4) Uani d . 1.00 N
N21 .3870(3) -.0231(2) .23970(10) .0315(4) Uani d . 1.00 N
N22 .6410(4) .2319(2) .5622(2) .0445(5) Uani d . 1.00 N
C23 .0504(4) .2282(2) .3971(2) .0373(5) Uani d . 1.00 C
C24 .0768(4) .1237(2) .4472(2) .0384(5) Uani d . 1.00 C
C25 .2357(4) .0205(2) .0790(2) .0430(6) Uani d . 1.00 C
C26 .4247(4) -.0193(2) .1374(2) .0426(6) Uani d . 1.00 C
H18A .0595 .2678 .2594 .0347 Uiso calc . 1.00 H
H18B -.1124 .1878 .2723 .0347 Uiso calc . 1.00 H
H19A .3690 .0906 .4312 .0405 Uiso calc . 1.00 H
H19B .2275 -.0069 .4160 .0405 Uiso calc . 1.00 H
H20A .2473 .1744 .1129 .0395 Uiso calc . 1.00 H
H20B .0281 .1288 .1065 .0395 Uiso calc . 1.00 H
H21A .5130 -.0158 .2797 .0381 Uiso calc . 1.00 H
H21B .3260 -.0883 .2523 .0381 Uiso calc . 1.00 H
H23A .1670 .2712 .4141 .0446 Uiso calc . 1.00 H
H23B -.0674 .2631 .4143 .0446 Uiso calc . 1.00 H
H24A .1170 .1339 .5137 .0458 Uiso calc . 1.00 H
H24B -.0473 .0853 .4381 .0458 Uiso calc . 1.00 H
H25A .2644 .0381 .0164 .0513 Uiso calc . 1.00 H
H25B .1322 -.0317 .0750 .0513 Uiso calc . 1.00 H
H26A .5358 .0264 .1305 .0511 Uiso calc . 1.00 H
H26B .4558 -.0879 .1165 .0511 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 .02020(10) .0202(2) .0246(2) .00020(9) .00210(10) -.00016(9)
Cl2 .0338(3) .0332(3) .0543(4) -.0036(3) .0051(3) -.0042(3)
O8 .067(2) .0310(10) .078(2) -.0240(10) .0300(10) -.0060(10)
O9 .0211(10) .087(2) .069(2) -.0130(10) -.0010(10) -.0210(10)
O10 .052(3) .137(6) .073(3) -.042(4) .001(2) -.029(4)
O11 .098(4) .054(3) .059(3) .033(3) .020(2) .023(2)
O12 .079(3) .037(2) .055(2) .005(2) -.005(2) -.001(2)
O13 .094(5) .043(3) .100(5) .008(3) .016(4) .016(3)
O14 .072(3) .047(3) .074(3) .017(3) .024(3) .011(3)
O15 .048(4) .29(2) .081(5) -.067(7) .017(3) -.100(8)
N17 .035(2) .046(2) .043(2) -.0080(10) .0200(10) -.0210(10)
N18 .0301(9) .0230(8) .0348(9) .0031(7) .0077(7) .0014(7)
N19 .0331(9) .0384(10) .0290(9) .0045(8) .0010(7) .0026(8)
N20 .0374(10) .0331(9) .0287(9) .0039(8) .0041(8) .0037(7)
N21 .0302(9) .0300(9) .0343(9) .0075(7) .0033(7) -.0021(7)
N22 .0540(10) .0440(10) .0390(10) .0040(10) .0170(10) -.0012(9)
C23 .0410(10) .0340(10) .0390(10) .0010(10) .0121(10) -.0091(10)
C24 .0420(10) .0440(10) .0310(10) .0030(10) .0109(10) -.0008(10)
C25 .0520(10) .0470(10) .0300(10) .0060(10) .0050(10) -.0070(10)
C26 .0450(10) .0470(10) .0380(10) .0110(10) .0100(10) -.0080(10)
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
Cl2 Co1 N17 1_555 1_555 179.30(10) yes
Cl2 Co1 N18 1_555 1_555 90.53(6) no
Cl2 Co1 N19 1_555 1_555 89.82(6) no
Cl2 Co1 N20 1_555 1_555 89.53(6) no
Cl2 Co1 N21 1_555 1_555 90.03(6) no
Cl3 Co1 N16 1_555 1_555 177.3(7) no
Cl3 Co1 N18 1_555 1_555 90.6(3) no
Cl3 Co1 N19 1_555 1_555 89.5(3) no
Cl3 Co1 N20 1_555 1_555 91.1(3) no
Cl3 Co1 N21 1_555 1_555 88.8(3) no
N16 Co1 N18 1_555 1_555 91.1(6) no
N16 Co1 N19 1_555 1_555 88.5(6) no
N16 Co1 N20 1_555 1_555 90.8(6) no
N16 Co1 N21 1_555 1_555 89.5(6) no
N17 Co1 N18 1_555 1_555 90.00(10) no
N17 Co1 N19 1_555 1_555 90.70(10) no
N17 Co1 N20 1_555 1_555 90.00(10) no
N17 Co1 N21 1_555 1_555 89.50(10) no
N18 Co1 N19 1_555 1_555 86.04(8) no
N18 Co1 N20 1_555 1_555 93.79(8) no
N18 Co1 N21 1_555 1_555 179.44(8) no
N19 Co1 N20 1_555 1_555 179.32(8) no
N19 Co1 N21 1_555 1_555 93.95(8) no
N20 Co1 N21 1_555 1_555 86.23(8) no
Co1 N16 O4 1_555 1_555 117.0(10) no
Co1 N16 O5 1_555 1_555 120.0(10) no
Co1 N16 O6 1_555 1_555 122.0(10) no
Co1 N16 O7 1_555 1_555 122.0(10) no
O4 N16 O5 1_555 1_555 122(2) no
O6 N16 O7 1_555 1_555 114(2) no
Co1 N17 O8 1_555 1_555 119.7(3) no
Co1 N17 O9 1_555 1_555 119.7(3) no
O8 N17 O9 1_555 1_555 120.6(4) yes
Co1 N18 C23 1_555 1_555 109.30(10) no
Co1 N18 H18A 1_555 1_555 109.4 no
Co1 N18 H18B 1_555 1_555 109.4 no
C23 N18 H18A 1_555 1_555 109.5 no
C23 N18 H18B 1_555 1_555 109.5 no
H18A N18 H18B 1_555 1_555 109.7 no
Co1 N19 C24 1_555 1_555 109.00(10) no
Co1 N19 H19A 1_555 1_555 109.5 no
Co1 N19 H19B 1_555 1_555 109.6 no
C24 N19 H19A 1_555 1_555 109.5 no
C24 N19 H19B 1_555 1_555 109.6 no
H19A N19 H19B 1_555 1_555 109.7 no
Co1 N20 C25 1_555 1_555 108.60(10) no
Co1 N20 H20A 1_555 1_555 109.6 no
Co1 N20 H20B 1_555 1_555 109.6 no
C25 N20 H20A 1_555 1_555 109.7 no
C25 N20 H20B 1_555 1_555 109.6 no
H20A N20 H20B 1_555 1_555 109.8 no
Co1 N21 C26 1_555 1_555 109.80(10) no
Co1 N21 H21A 1_555 1_555 109.2 no
Co1 N21 H21B 1_555 1_555 109.3 no
C26 N21 H21A 1_555 1_555 109.3 no
C26 N21 H21B 1_555 1_555 109.4 no
H21A N21 H21B 1_555 1_555 109.7 no
O10 N22 O11 1_555 1_555 124.9(5) no
O10 N22 O12 1_555 1_555 122.8(5) no
O11 N22 O12 1_555 1_555 112.1(4) no
O13 N22 O14 1_555 1_555 104.8(4) no
O13 N22 O15 1_555 1_555 128.8(8) no
O14 N22 O15 1_555 1_555 125.1(8) no
N18 C23 C24 1_555 1_555 107.1(2) no
N18 C23 H23A 1_555 1_555 110.2 no
N18 C23 H23B 1_555 1_555 109.9 no
C24 C23 H23A 1_555 1_555 110.3 no
C24 C23 H23B 1_555 1_555 110.1 no
H23A C23 H23B 1_555 1_555 109.2 no
N19 C24 C23 1_555 1_555 107.0(2) no
N19 C24 H24A 1_555 1_555 110.0 no
N19 C24 H24B 1_555 1_555 110.0 no
C23 C24 H24A 1_555 1_555 110.1 no
C23 C24 H24B 1_555 1_555 110.1 no
H24A C24 H24B 1_555 1_555 109.5 no
N20 C25 C26 1_555 1_555 107.5(2) no
N20 C25 H25A 1_555 1_555 109.8 no
N20 C25 H25B 1_555 1_555 110.1 no
C26 C25 H25A 1_555 1_555 110.0 no
C26 C25 H25B 1_555 1_555 110.0 no
H25A C25 H25B 1_555 1_555 109.5 no
N21 C26 C25 1_555 1_555 108.4(2) no
N21 C26 H26A 1_555 1_555 109.9 no
N21 C26 H26B 1_555 1_555 109.8 no
C25 C26 H26A 1_555 1_555 109.8 no
C25 C26 H26B 1_555 1_555 109.7 no
H26A C26 H26B 1_555 1_555 109.3 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 Cl2 2.2801(8) yes
Co1 Cl3 2.310(10) no
Co1 N16 1.90(2) no
Co1 N17 1.888(4) yes
Co1 N18 1.955(2) yes
Co1 N19 1.952(2) yes
Co1 N20 1.961(2) yes
Co1 N21 1.951(2) yes
O4 N16 1.24(3) no
O5 N16 1.24(3) no
O6 N16 1.25(3) no
O7 N16 1.25(3) no
O8 N17 1.235(5) yes
O9 N17 1.240(4) yes
O10 N22 1.125(6) no
O11 N22 1.276(6) no
O12 N22 1.276(5) no
O13 N22 1.306(6) no
O14 N22 1.321(6) no
O15 N22 1.085(8) no
N18 C23 1.484(3) no
N18 H18A .949 no
N18 H18B .948 no
N19 C24 1.487(3) no
N19 H19A .950 no
N19 H19B .947 no
N20 C25 1.486(3) no
N20 H20A .948 no
N20 H20B .948 no
N21 C26 1.491(3) no
N21 H21A .950 no
N21 H21B .948 no
C23 C24 1.504(4) no
C23 H23A .951 no
C23 H23B .952 no
C24 H24A .950 no
C24 H24B .949 no
C25 C26 1.496(4) no
C25 H25A .951 no
C25 H25B .949 no
C26 H26A .951 no
C26 H26B .951 no