#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:29:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179181 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/29/4312912.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_4312912
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 O S 2+,2(Cl O4 1-)'
_chemical_formula_sum            'C9 H20 Cl2 Co N5 O9 S'
_chemical_formula_weight         504.2
_chemical_name_systematic
;
1-rac-[Co(en)2(py-SO1.00-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                75.73(2)
_cell_angle_beta                 84.80(2)
_cell_angle_gamma                84.92(2)
_cell_formula_units_Z            2
_cell_length_a                   9.231(2)
_cell_length_b                   9.383(2)
_cell_length_c                   11.253(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294
_cell_measurement_theta_max      23
_cell_measurement_theta_min      20
_cell_volume                     938.5(4)
_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  0.007
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3504
_diffrn_reflns_theta_max         25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  30min
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    1.358
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(DeMeulenaer & Tompa, 1965)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.78
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             516.0
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.04
_refine_diff_density_min         -0.91
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.90
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     197
_refine_ls_number_reflns         2952
_refine_ls_R_factor_gt           0.049
_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         0.093
_reflns_number_gt                2952
_reflns_number_total             3284
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic020207o_s1.cif
_cod_data_source_block           DDAN3(1)
_cod_database_code               4312912
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 0.30201(5) 0.32748(5) 0.26205(4) 0.0282(3) Uani Co 1.0
S 0.4498(2) 0.1258(1) 0.1210(1) 0.0542(4) Uani S 1.0
O1 0.4473(3) 0.2866(3) 0.1434(3) 0.0437(7) Uani O 1.0
N1 0.1898(4) 0.1810(4) 0.2202(3) 0.0354(8) Uani N 1.0
C1 0.2661(5) 0.0953(5) 0.1529(4) 0.041(1) Uani C 1.0
C2 0.2026(7) -0.0108(5) 0.1119(4) 0.055(1) Uani C 1.0
C3 0.0586(7) -0.0305(6) 0.1438(5) 0.064(2) Uani C 1.0
C4 -0.0230(6) 0.0588(6) 0.2099(5) 0.060(1) Uani C 1.0
C5 0.0452(5) 0.1652(6) 0.2451(4) 0.050(1) Uani C 1.0
N2 0.3904(4) 0.1760(4) 0.3940(3) 0.0386(8) Uani N 1.0
N3 0.1625(4) 0.3695(4) 0.3950(3) 0.0369(8) Uani N 1.0
C6 0.3211(8) 0.1847(7) 0.5148(5) 0.076(2) Uani C 1.0
C7 0.1790(7) 0.2470(9) 0.5068(5) 0.084(2) Uani C 1.0
N4 0.2150(4) 0.4794(4) 0.1320(3) 0.0360(8) Uani N 1.0
N5 0.4278(4) 0.4792(4) 0.2765(3) 0.0352(8) Uani N 1.0
C8 0.3104(7) 0.6019(6) 0.0946(5) 0.064(2) Uani C 1.0
C9 0.3780(7) 0.6234(6) 0.1968(6) 0.070(2) Uani C 1.0
Cl1A 0.82577(10) 0.62192(11) 0.16892(8) 0.044(1) Uani Cl 1.0
O1A 0.7418(3) 0.7416(3) 0.2029(3) 0.091(2) Uani O 1.0
O2A 0.9188(3) 0.5527(3) 0.2632(2) 0.075(2) Uani O 1.0
O3A 0.9111(3) 0.6748(3) 0.0579(2) 0.062(1) Uani O 1.0
O4A 0.7314(3) 0.5186(3) 0.1516(3) 0.089(2) Uani O 1.0
Cl1B 0.72490(11) 0.25909(11) 0.50476(9) 0.046(1) Uani Cl 1.0
O1B 0.7263(4) 0.2177(3) 0.3916(2) 0.081(2) Uani O 1.0
O2B 0.6772(4) 0.1419(3) 0.6024(2) 0.090(2) Uani O 1.0
O3B 0.6286(4) 0.3861(3) 0.5019(3) 0.097(2) Uani O 1.0
O4B 0.8675(2) 0.2907(4) 0.5231(3) 0.1149(9) Uani O 1.0
HC2 0.2610 -0.0713 0.0604 0.055 Uani H 1.0
HC3 0.0115 -0.1099 0.1193 0.064 Uani H 1.0
HC4 -0.1293 0.0464 0.2317 0.060 Uani H 1.0
HC5 -0.0139 0.2324 0.2902 0.050 Uani H 1.0
H1N2 0.4966 0.1909 0.3919 0.039 Uani H 1.0
H2N2 0.3781 0.0764 0.3806 0.039 Uani H 1.0
H1N3 0.0608 0.3771 0.3691 0.037 Uani H 1.0
H2N3 0.1834 0.4644 0.4132 0.037 Uani H 1.0
H1C6 0.3793 0.2463 0.5511 0.076 Uani H 1.0
H2C6 0.3197 0.0830 0.5694 0.076 Uani H 1.0
H1C7 0.1502 0.2863 0.5811 0.084 Uani H 1.0
H2C7 0.1130 0.1689 0.5043 0.084 Uani H 1.0
H1N4 0.1172 0.5156 0.1631 0.036 Uani H 1.0
H2N4 0.2038 0.4376 0.0601 0.036 Uani H 1.0
H1N5 0.5307 0.4522 0.2500 0.035 Uani H 1.0
H2N5 0.4223 0.4868 0.3639 0.035 Uani H 1.0
H1C8 0.2512 0.6940 0.0576 0.064 Uani H 1.0
H2C8 0.3876 0.5796 0.0322 0.064 Uani H 1.0
H1C9 0.3063 0.6766 0.2457 0.070 Uani H 1.0
H2C9 0.4639 0.6837 0.1665 0.070 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 86.8(1) 1_555 1_555 1_555 no
O1 Co N2 92.0(1) 1_555 1_555 1_555 no
O1 Co N3 175.4(1) 1_555 1_555 1_555 no
O1 Co N4 88.2(1) 1_555 1_555 1_555 no
O1 Co N5 85.1(1) 1_555 1_555 1_555 no
N1 Co N2 91.1(2) 1_555 1_555 1_555 no
N1 Co N3 96.4(1) 1_555 1_555 1_555 no
N1 Co N4 89.6(1) 1_555 1_555 1_555 no
N1 Co N5 170.8(1) 1_555 1_555 1_555 no
N2 Co N3 84.7(1) 1_555 1_555 1_555 no
N2 Co N4 179.4(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(1) 1_555 1_555 1_555 no
N3 Co N5 91.9(1) 1_555 1_555 1_555 no
N4 Co N5 85.8(1) 1_555 1_555 1_555 no
O1 S C1 99.4(2) 1_555 1_555 1_555 no
Co O1 S 114.7(2) 1_555 1_555 1_555 no
Co N1 C1 114.9(3) 1_555 1_555 1_555 no
Co N1 C5 126.7(3) 1_555 1_555 1_555 no
C1 N1 C5 118.3(4) 1_555 1_555 1_555 no
S C1 N1 115.6(3) 1_555 1_555 1_555 no
S C1 C2 121.9(4) 1_555 1_555 1_555 no
N1 C1 C2 122.5(5) 1_555 1_555 1_555 no
C1 C2 C3 118.2(5) 1_555 1_555 1_555 no
C2 C3 C4 120.4(4) 1_555 1_555 1_555 no
C3 C4 C5 118.7(5) 1_555 1_555 1_555 no
N1 C5 C4 121.7(5) 1_555 1_555 1_555 no
Co N2 C6 111.1(3) 1_555 1_555 1_555 no
Co N3 C7 108.7(3) 1_555 1_555 1_555 no
N2 C6 C7 111.9(5) 1_555 1_555 1_555 no
N3 C7 C6 112.4(5) 1_555 1_555 1_555 no
Co N4 C8 109.0(3) 1_555 1_555 1_555 no
Co N5 C9 109.3(3) 1_555 1_555 1_555 no
N4 C8 C9 111.1(4) 1_555 1_555 1_555 no
N5 C9 C8 110.4(4) 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 1.888(3) 1_555 1_555 no
Co N1 1.961(3) 1_555 1_555 no
Co N2 1.966(3) 1_555 1_555 no
Co N3 1.976(3) 1_555 1_555 no
Co N4 1.949(3) 1_555 1_555 no
Co N5 1.960(3) 1_555 1_555 no
S O1 1.588(3) 1_555 1_555 no
S C1 1.735(5) 1_555 1_555 no
N1 C1 1.348(6) 1_555 1_555 no
N1 C5 1.353(6) 1_555 1_555 no
C1 C2 1.388(6) 1_555 1_555 no
C2 C3 1.362(9) 1_555 1_555 no
C3 C4 1.384(9) 1_555 1_555 no
C4 C5 1.379(7) 1_555 1_555 no
N2 C6 1.466(6) 1_555 1_555 no
N3 C7 1.489(7) 1_555 1_555 no
C6 C7 1.390(9) 1_555 1_555 no
N4 C8 1.465(6) 1_555 1_555 no
N5 C9 1.488(6) 1_555 1_555 no
C8 C9 1.421(8) 1_555 1_555 no
Cl1A O1A 1.418(1) 1_555 1_555 no
