#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:29:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179181 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/29/4312915.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_4312915
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 O2 S 2+,2(Cl O4 1-)'
_chemical_formula_sum            'C9 H20 Cl2 Co N5 O10 S'
_chemical_formula_weight         520.2
_chemical_name_systematic
;
4-rac-[Co(en)2(py-SO2.00-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                96.57(2)
_cell_angle_beta                 98.44(2)
_cell_angle_gamma                94.23(2)
_cell_formula_units_Z            2
_cell_length_a                   8.611(3)
_cell_length_b                   9.370(3)
_cell_length_c                   11.786(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294
_cell_measurement_theta_max      24
_cell_measurement_theta_min      20
_cell_volume                     930.5(5)
_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       -10
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3467
_diffrn_reflns_theta_max         25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  30min
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    1.376
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(DeMeulenaer & Tompa, 1965)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.86
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             532.0
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.51
_refine_diff_density_min         -0.56
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.58
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     206
_refine_ls_number_reflns         2919
_refine_ls_R_factor_gt           0.032
_refine_ls_shift/su_max          0.007
_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         0.056
_reflns_number_gt                2919
_reflns_number_total             3248
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic020207o_s4.cif
_cod_data_source_block           DDAN4(4)
_cod_database_code               4312915
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 0.17037(4) 0.18091(3) 0.28350(3) 0.0218(2) Uani Co 1.0
S -0.00802(8) -0.10526(7) 0.19826(6) 0.0307(2) Uani S 1.0
O1 0.0157(2) 0.0280(2) 0.2913(2) 0.0301(4) Uani O 1.0
O2 -0.1014(2) -0.0724(2) 0.0893(2) 0.0399(5) Uani O 1.0
N1 0.2800(3) 0.0324(3) 0.2050(2) 0.0270(5) Uani N 1.0
C1 0.1935(3) -0.0953(3) 0.1686(2) 0.0294(6) Uani C 1.0
C2 0.2535(4) -0.2129(3) 0.1158(3) 0.0380(7) Uani C 1.0
C3 0.4103(4) -0.2020(4) 0.1003(3) 0.0468(8) Uani C 1.0
C4 0.5013(4) -0.0721(4) 0.1396(3) 0.0458(8) Uani C 1.0
C5 0.4327(4) 0.0419(4) 0.1900(3) 0.0376(7) Uani C 1.0
N2 0.0569(3) 0.2270(3) 0.1369(2) 0.0284(5) Uani N 1.0
N3 0.3226(3) 0.3420(2) 0.2701(2) 0.0290(5) Uani N 1.0
C6 0.1295(4) 0.3618(3) 0.1048(3) 0.0376(7) Uani C 1.0
C7 0.3027(4) 0.3703(3) 0.1471(3) 0.0384(7) Uani C 1.0
N4 0.2767(3) 0.1408(3) 0.4328(2) 0.0305(5) Uani N 1.0
N5 0.0514(3) 0.3073(3) 0.3734(2) 0.0311(5) Uani N 1.0
C8 0.1879(4) 0.1927(3) 0.5255(3) 0.0358(7) Uani C 1.0
C9 0.1305(4) 0.3345(3) 0.4958(2) 0.0363(7) Uani C 1.0
Cl1A 0.72485(7) 0.47371(7) 0.19478(5) 0.0332(9) Uani Cl 1.0
O1A 0.6798(3) 0.5093(2) 0.0810(1) 0.075(1) Uani O 1.0
O2A 0.7131(2) 0.3210(1) 0.1922(2) 0.078(2) Uani O 1.0
O3A 0.6232(2) 0.5336(2) 0.2689(2) 0.0758(6) Uani O 1.0
O4A 0.8833(1) 0.5310(2) 0.2370(2) 0.060(1) Uani O 1.0
Cl1B 0.68636(7) 0.26456(7) 0.55083(6) 0.0340(7) Uani Cl 1.0
O1B 0.7823(2) 0.3676(2) 0.6353(1) 0.063(1) Uani O 1.0
O2B 0.5961(2) 0.1690(2) 0.6070(1) 0.053(1) Uani O 1.0
O3B 0.7840(2) 0.1843(2) 0.4849(2) 0.0971(6) Uani O 1.0
O4B 0.5830(2) 0.3372(2) 0.4761(2) 0.081(1) Uani O 1.0
HC2 0.1851 -0.3050 0.0890 0.038 Uani H 1.0
HC3 0.4569 -0.2856 0.0618 0.047 Uani H 1.0
HC4 0.6154 -0.0617 0.1314 0.046 Uani H 1.0
HC5 0.4986 0.1355 0.2165 0.038 Uani H 1.0
H1N2 -0.0554 0.2392 0.1455 0.028 Uani H 1.0
H2N2 0.0606 0.1460 0.0745 0.028 Uani H 1.0
H1N3 0.4322 0.3164 0.2944 0.029 Uani H 1.0
H2N3 0.3029 0.4300 0.3206 0.029 Uani H 1.0
H1C6 0.0836 0.4469 0.1418 0.038 Uani H 1.0
H2C6 0.1101 0.3602 0.0188 0.038 Uani H 1.0
H1C7 0.3528 0.4685 0.1417 0.038 Uani H 1.0
H2C7 0.3522 0.2962 0.0999 0.038 Uani H 1.0
H1N4 0.3856 0.1912 0.4485 0.031 Uani H 1.0
H2N4 0.2830 0.0345 0.4311 0.031 Uani H 1.0
H1N5 -0.0577 0.2604 0.3699 0.031 Uani H 1.0
H2N5 0.0456 0.4009 0.3406 0.031 Uani H 1.0
H1C8 0.2583 0.2073 0.6021 0.036 Uani H 1.0
H2C8 0.0965 0.1216 0.5280 0.036 Uani H 1.0
H1C9 0.2215 0.4098 0.5044 0.036 Uani H 1.0
H2C9 0.0542 0.3671 0.5474 0.036 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 85.63(9) 1_555 1_555 1_555 no
O1 Co N2 92.30(9) 1_555 1_555 1_555 no
O1 Co N3 177.32(8) 1_555 1_555 1_555 no
O1 Co N4 87.44(9) 1_555 1_555 1_555 no
O1 Co N5 87.58(9) 1_555 1_555 1_555 no
N1 Co N2 92.6(1) 1_555 1_555 1_555 no
N1 Co N3 95.3(1) 1_555 1_555 1_555 no
N1 Co N4 90.0(1) 1_555 1_555 1_555 no
N1 Co N5 172.0(1) 1_555 1_555 1_555 no
N2 Co N3 85.14(9) 1_555 1_555 1_555 no
N2 Co N4 177.3(1) 1_555 1_555 1_555 no
N2 Co N5 91.9(1) 1_555 1_555 1_555 no
N3 Co N4 95.07(9) 1_555 1_555 1_555 no
N3 Co N5 91.7(1) 1_555 1_555 1_555 no
N4 Co N5 85.4(1) 1_555 1_555 1_555 no
O1 S O2 110.5(1) 1_555 1_555 1_555 no
O1 S C1 96.2(1) 1_555 1_555 1_555 no
O2 S C1 103.7(1) 1_555 1_555 1_555 no
Co O1 S 119.3(1) 1_555 1_555 1_555 no
Co N1 C1 115.2(2) 1_555 1_555 1_555 no
Co N1 C5 127.1(2) 1_555 1_555 1_555 no
C1 N1 C5 117.6(3) 1_555 1_555 1_555 no
S C1 N1 115.8(2) 1_555 1_555 1_555 no
S C1 C2 121.3(2) 1_555 1_555 1_555 no
N1 C1 C2 122.9(3) 1_555 1_555 1_555 no
C1 C2 C3 119.1(3) 1_555 1_555 1_555 no
C2 C3 C4 118.5(3) 1_555 1_555 1_555 no
C3 C4 C5 119.3(3) 1_555 1_555 1_555 no
N1 C5 C4 122.6(3) 1_555 1_555 1_555 no
Co N2 C6 110.8(2) 1_555 1_555 1_555 no
Co N3 C7 108.5(2) 1_555 1_555 1_555 no
N2 C6 C7 107.6(2) 1_555 1_555 1_555 no
N3 C7 C6 107.2(2) 1_555 1_555 1_555 no
Co N4 C8 109.9(2) 1_555 1_555 1_555 no
Co N5 C9 109.7(2) 1_555 1_555 1_555 no
N4 C8 C9 106.3(2) 1_555 1_555 1_555 no
N5 C9 C8 106.3(2) 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 1.902(2) 1_555 1_555 no
Co N1 1.959(2) 1_555 1_555 no
Co N2 1.966(2) 1_555 1_555 no
Co N3 1.961(2) 1_555 1_555 no
Co N4 1.951(2) 1_555 1_555 no
Co N5 1.945(2) 1_555 1_555 no
S O1 1.545(2) 1_555 1_555 no
S O2 1.488(2) 1_555 1_555 no
S C1 1.817(3) 1_555 1_555 no
N1 C1 1.352(4) 1_555 1_555 no
N1 C5 1.351(4) 1_555 1_555 no
C1 C2 1.375(4) 1_555 1_555 no
C2 C3 1.387(5) 1_555 1_555 no
C3 C4 1.390(5) 1_555 1_555 no
C4 C5 1.376(5) 1_555 1_555 no
N2 C6 1.481(4) 1_555 1_555 no
N3 C7 1.491(4) 1_555 1_555 no
C6 C7 1.495(4) 1_555 1_555 no
N4 C8 1.481(4) 1_555 1_555 no
N5 C9 1.488(4) 1_555 1_555 no
C8 C9 1.512(4) 1_555 1_555 no
Cl1A O1A 1.424(1) 1_555 1_555 no
