#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:29:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179181 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/29/4312913.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4312913
loop_
_publ_author_name
'W. G. Jackson'
'A. F. M. M. Rahman'
'D. C. Craig'
_publ_section_title
;
 The First Oxygen-Bonded Sulfenate Ion: Crystal and Molecular Structures
 of Bis(ethylenediamine)(2-pyridinesulfenato-O)cobalt(III) and
 Bis(ethylenediamine)(2-pyridinesulfinato-O)cobalt(III)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              383
_journal_page_last               388
_journal_paper_doi               10.1021/ic020207o
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C9 H20 Co N5 O1.21 S 2+,2(Cl O4 1-)'
_chemical_formula_sum            'C9 H20 Cl2 Co N5 O9.21 S'
_chemical_formula_weight         507.5
_chemical_name_systematic
;
2-rac-[Co(en)2(py-SO1.21-O](ClO4)2
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_type_scat_source
'International Tables for X-ray Crystallography, Vol. IV'
_audit_creation_method           'RAELSPUB and manual entry'
_cell_angle_alpha                75.83(3)
_cell_angle_beta                 85.15(2)
_cell_angle_gamma                85.21(2)
_cell_formula_units_Z            2
_cell_length_a                   9.216(3)
_cell_length_b                   9.374(3)
_cell_length_c                   11.283(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294
_cell_measurement_theta_max      20
_cell_measurement_theta_min      17
_cell_volume                     939.7(6)
_computing_cell_refinement       'CAD4 Version 5.0, 1989'
_computing_data_collection       'CAD4 Version 5.0, 1989'
_computing_data_reduction        'Local program'
_computing_molecular_graphics    'ORTEP-II, (Johnson, 1976)'
_computing_publication_material  'Local programs'
_computing_structure_refinement  'RAELS, (Rae, 1989)'
_computing_structure_solution    'SIR92 (Altomare et al, 1994)'
_diffrn_measurement_device_type  'Nonius CAD-4'
_diffrn_measurement_method       ω--2θ
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.010
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3518
_diffrn_reflns_theta_max         25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  30min
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    1.357
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(DeMeulenaer & Tompa, 1965)'
_exptl_crystal_colour            green-red
_exptl_crystal_density_diffrn    1.79
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             519.4
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.93
_refine_diff_density_min         -0.89
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.76
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     207
_refine_ls_number_reflns         2800
_refine_ls_R_factor_gt           0.051
_refine_ls_shift/su_max          0.008
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(F) + 0.0004F²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.082
_reflns_number_gt                2800
_reflns_number_total             3291
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic020207o_s2.cif
_cod_data_source_block           DDAN2(2)
_cod_database_code               4312913
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,-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_type_symbol
_atom_site_occupancy
Co 0.30240(6) 0.32723(6) 0.26265(5) 0.0287(2) Uani Co 1.0
S 0.4508(2) 0.1281(2) 0.1203(1) 0.0593(4) Uani S 1.0
O1 0.4469(4) 0.2860(4) 0.1432(3) 0.0498(9) Uani O 1.0
O2 0.5423(23) 0.0331(23) 0.2066(18) 0.071(8) Uani O 0.21
N1 0.1892(4) 0.1810(4) 0.2209(3) 0.0361(9) Uani N 1.0
C1 0.2656(6) 0.0959(5) 0.1531(4) 0.043(1) Uani C 1.0
C2 0.2031(8) -0.0087(6) 0.1113(5) 0.058(2) Uani C 1.0
C3 0.0594(8) -0.0325(7) 0.1430(6) 0.066(2) Uani C 1.0
C4 -0.0219(7) 0.0566(7) 0.2092(6) 0.064(2) Uani C 1.0
C5 0.0454(6) 0.1625(6) 0.2458(5) 0.051(1) Uani C 1.0
N2 0.3913(4) 0.1761(4) 0.3944(4) 0.0399(9) Uani N 1.0
N3 0.1638(4) 0.3707(4) 0.3946(3) 0.0368(8) Uani N 1.0
C6 0.3228(8) 0.1842(9) 0.5148(5) 0.082(2) Uani C 1.0
C7 0.1829(9) 0.2537(11) 0.5071(5) 0.103(3) Uani C 1.0
N4 0.2156(4) 0.4790(4) 0.1322(3) 0.0362(8) Uani N 1.0
N5 0.4291(4) 0.4796(4) 0.2767(4) 0.0365(8) Uani N 1.0
C8 0.3098(8) 0.6028(7) 0.0955(6) 0.069(2) Uani C 1.0
C9 0.3790(8) 0.6224(6) 0.1985(6) 0.069(2) Uani C 1.0
Cl1A 0.82656(11) 0.62027(13) 0.16803(9) 0.045(1) Uani Cl 1.0
O1A 0.7421(3) 0.7393(3) 0.2017(3) 0.095(2) Uani O 1.0
O2A 0.9202(3) 0.5523(4) 0.2620(2) 0.076(2) Uani O 1.0
O3A 0.9112(3) 0.6736(4) 0.0576(2) 0.066(1) Uani O 1.0
O4A 0.7328(3) 0.5158(4) 0.1508(3) 0.090(2) Uani O 1.0
Cl1B 0.7273(1) 0.2596(1) 0.5052(1) 0.047(1) Uani Cl 1.0
O1B 0.7286(4) 0.2180(4) 0.3926(2) 0.086(2) Uani O 1.0
O2B 0.6807(5) 0.1421(3) 0.6023(3) 0.095(2) Uani O 1.0
O3B 0.6302(4) 0.3856(3) 0.5023(4) 0.104(3) Uani O 1.0
O4B 0.8697(3) 0.2928(5) 0.5236(4) 0.122(1) Uani O 1.0
HC2 0.2619 -0.0666 0.0584 0.058 Uani H 1.0
HC3 0.0133 -0.1131 0.1188 0.066 Uani H 1.0
HC4 -0.1284 0.0438 0.2301 0.064 Uani H 1.0
HC5 -0.0140 0.2277 0.2922 0.051 Uani H 1.0
H1N2 0.4976 0.1915 0.3924 0.040 Uani H 1.0
H2N2 0.3790 0.0764 0.3808 0.040 Uani H 1.0
H1N3 0.0617 0.3746 0.3698 0.037 Uani H 1.0
H2N3 0.1832 0.4679 0.4099 0.037 Uani H 1.0
H1C6 0.3848 0.2406 0.5533 0.082 Uani H 1.0
H2C6 0.3162 0.0818 0.5672 0.082 Uani H 1.0
H1C7 0.1613 0.2985 0.5791 0.103 Uani H 1.0
H2C7 0.1119 0.1776 0.5105 0.103 Uani H 1.0
H1N4 0.1173 0.5142 0.1625 0.036 Uani H 1.0
H2N4 0.2052 0.4369 0.0602 0.036 Uani H 1.0
H1N5 0.5318 0.4529 0.2497 0.036 Uani H 1.0
H2N5 0.4248 0.4870 0.3638 0.036 Uani H 1.0
H1C8 0.2496 0.6948 0.0601 0.069 Uani H 1.0
H2C8 0.3863 0.5825 0.0322 0.069 Uani H 1.0
H1C9 0.3078 0.6748 0.2478 0.069 Uani H 1.0
H2C9 0.4649 0.6831 0.1686 0.069 Uani H 1.0
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co N1 86.6(2) 1_555 1_555 1_555 no
O1 Co N2 92.3(2) 1_555 1_555 1_555 no
O1 Co N3 175.8(2) 1_555 1_555 1_555 no
O1 Co N4 87.7(2) 1_555 1_555 1_555 no
O1 Co N5 85.2(2) 1_555 1_555 1_555 no
N1 Co N2 91.2(2) 1_555 1_555 1_555 no
N1 Co N3 96.6(2) 1_555 1_555 1_555 no
N1 Co N4 89.4(2) 1_555 1_555 1_555 no
N1 Co N5 170.6(2) 1_555 1_555 1_555 no
N2 Co N3 84.9(2) 1_555 1_555 1_555 no
N2 Co N4 179.3(2) 1_555 1_555 1_555 no
N2 Co N5 93.7(2) 1_555 1_555 1_555 no
N3 Co N4 95.0(2) 1_555 1_555 1_555 no
N3 Co N5 91.8(2) 1_555 1_555 1_555 no
N4 Co N5 85.6(2) 1_555 1_555 1_555 no
O1 S O2 107.8(9) 1_555 1_555 1_555 no
O1 S C1 98.9(2) 1_555 1_555 1_555 no
O2 S C1 112.8(9) 1_555 1_555 1_555 no
Co O1 S 115.6(2) 1_555 1_555 1_555 no
Co N1 C1 114.4(3) 1_555 1_555 1_555 no
Co N1 C5 127.6(3) 1_555 1_555 1_555 no
C1 N1 C5 117.8(4) 1_555 1_555 1_555 no
S C1 N1 115.8(3) 1_555 1_555 1_555 no
S C1 C2 121.5(4) 1_555 1_555 1_555 no
N1 C1 C2 122.7(5) 1_555 1_555 1_555 no
C1 C2 C3 119.0(5) 1_555 1_555 1_555 no
C2 C3 C4 119.1(5) 1_555 1_555 1_555 no
C3 C4 C5 119.3(6) 1_555 1_555 1_555 no
N1 C5 C4 121.9(5) 1_555 1_555 1_555 no
Co N2 C6 111.3(3) 1_555 1_555 1_555 no
Co N3 C7 109.1(3) 1_555 1_555 1_555 no
N2 C6 C7 112.3(5) 1_555 1_555 1_555 no
N3 C7 C6 114.1(6) 1_555 1_555 1_555 no
Co N4 C8 109.4(3) 1_555 1_555 1_555 no
Co N5 C9 109.4(3) 1_555 1_555 1_555 no
N4 C8 C9 110.6(5) 1_555 1_555 1_555 no
N5 C9 C8 111.2(5) 1_555 1_555 1_555 no
O1A Cl1A O2A 109.47 1_555 1_555 1_555 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co O1 1.898(3) 1_555 1_555 no
Co N1 1.956(4) 1_555 1_555 no
Co N2 1.967(4) 1_555 1_555 no
Co N3 1.976(4) 1_555 1_555 no
Co N4 1.953(4) 1_555 1_555 no
Co N5 1.962(4) 1_555 1_555 no
S O1 1.561(4) 1_555 1_555 no
S O2 1.429(19) 1_555 1_555 no
S C1 1.751(6) 1_555 1_555 no
N1 C1 1.353(6) 1_555 1_555 no
N1 C5 1.348(6) 1_555 1_555 no
C1 C2 1.372(7) 1_555 1_555 no
C2 C3 1.365(10) 1_555 1_555 no
C3 C4 1.386(10) 1_555 1_555 no
C4 C5 1.374(8) 1_555 1_555 no
N2 C6 1.466(7) 1_555 1_555 no
N3 C7 1.473(7) 1_555 1_555 no
C6 C7 1.395(10) 1_555 1_555 no
N4 C8 1.465(7) 1_555 1_555 no
N5 C9 1.473(7) 1_555 1_555 no
C8 C9 1.429(9) 1_555 1_555 no
Cl1A O1A 1.417(2) 1_555 1_555 no
