#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:12:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179317 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/14/4321434.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_4321434
loop_
_publ_author_name
'Núria Duran'
'William Clegg'
'Lourdes Cucurull-Sánchez'
'Robert A. Coxall'
'Hermas R. Jiménez'
'José-María Moratal'
'Francesc Lloret'
'Pilar González-Duarte'
_publ_section_title
;
 Unprecedented Stabilization of Cobalt(II) in a Tetrahedral S2O2
 Environment: The Use of a Redox-Noninnocent Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4821
_journal_page_last               4832
_journal_paper_doi               10.1021/ic000223q
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C24 H21 Co O6 S3'
_chemical_formula_weight         560.52
_chemical_name_systematic
;
 ?
;
_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_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                103.105(5)
_cell_angle_beta                 99.194(5)
_cell_angle_gamma                104.501(4)
_cell_formula_units_Z            2
_cell_length_a                   7.7256(14)
_cell_length_b                   11.141(2)
_cell_length_c                   15.606(3)
_cell_measurement_reflns_used    3699
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      25.26
_cell_measurement_theta_min      1.96
_cell_volume                     1232.7(4)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_measurement_device       'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5323
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    0.988
_exptl_absorpt_correction_T_max  0.71679
_exptl_absorpt_correction_T_min  0.55479
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       Block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.0068(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.092
_refine_ls_goodness_of_fit_obs   1.094
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         3872
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_restrained_S_obs      1.094
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_obs          0.0403
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0367P)²+1.7674P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1022
_refine_ls_wR_factor_obs         0.0971
_reflns_number_observed          3513
_reflns_number_total             3873
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000223q_4.cif
_cod_data_source_block           compound7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+1.7674P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+1.7674P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1232.8(4)
_cod_database_code               4321434
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Co Co 0.72657(5) 0.58483(4) 0.77989(3) 0.0242(2) Uani 1 d . .
S1 S 0.94849(10) 0.73653(8) 0.76249(5) 0.0271(2) Uani 1 d . .
C11 C 0.8856(4) 0.7587(3) 0.6557(2) 0.0248(7) Uani 1 d . .
C12 C 1.0315(5) 0.8332(3) 0.6288(2) 0.0317(7) Uani 1 d . .
H12 H 1.1492(5) 0.8673(3) 0.6691(2) 0.038 Uiso 1 calc R .
C13 C 1.0095(5) 0.8583(3) 0.5462(2) 0.0345(8) Uani 1 d . .
H13 H 1.1111(5) 0.9097(3) 0.5305(2) 0.041 Uiso 1 calc R .
C14 C 0.8384(5) 0.8087(3) 0.4849(2) 0.0371(8) Uani 1 d . .
H14 H 0.8242(5) 0.8228(3) 0.4267(2) 0.045 Uiso 1 calc R .
C15 C 0.6915(5) 0.7393(3) 0.5101(2) 0.0326(8) Uani 1 d . .
H15 H 0.5742(5) 0.7075(3) 0.4695(2) 0.039 Uiso 1 calc R .
C16 C 0.7112(4) 0.7142(3) 0.5957(2) 0.0269(7) Uani 1 d . .
C17 C 0.5465(4) 0.6454(3) 0.6193(2) 0.0292(7) Uani 1 d . .
O11 O 0.5390(3) 0.5947(2) 0.68139(15) 0.0294(5) Uani 1 d . .
O12 O 0.3912(3) 0.6429(2) 0.5667(2) 0.0387(6) Uani 1 d . .
C18 C 0.2221(5) 0.5765(4) 0.5868(3) 0.0452(10) Uani 1 d . .
H18A H 0.1172(5) 0.5864(23) 0.5475(13) 0.068 Uiso 1 calc R .
H18B H 0.2230(17) 0.6137(18) 0.6501(6) 0.068 Uiso 1 calc R .
H18C H 0.2119(19) 0.4846(6) 0.5762(18) 0.068 Uiso 1 calc R .
S2 S 0.81849(11) 0.44590(8) 0.68973(6) 0.0297(2) Uani 1 d . .
C21 C 0.6930(4) 0.2890(3) 0.6837(2) 0.0288(7) Uani 1 d . .
C22 C 0.7633(5) 0.1937(3) 0.6401(2) 0.0374(8) Uani 1 d . .
H22 H 0.8750(5) 0.2194(3) 0.6216(2) 0.045 Uiso 1 calc R .
C23 C 0.6760(5) 0.0645(4) 0.6233(3) 0.0447(9) Uani 1 d . .
H23 H 0.7269(5) 0.0026(4) 0.5930(3) 0.054 Uiso 1 calc R .
C24 C 0.5133(5) 0.0235(3) 0.6503(3) 0.0386(8) Uani 1 d . .
H24 H 0.4519(5) -0.0659(3) 0.6382(3) 0.046 Uiso 1 calc R .
C25 C 0.4434(5) 0.1144(3) 0.6947(2) 0.0322(8) Uani 1 d . .
H25 H 0.3325(5) 0.0869(3) 0.7134(2) 0.039 Uiso 1 calc R .
C26 C 0.5313(4) 0.2478(3) 0.7134(2) 0.0261(7) Uani 1 d . .
C27 C 0.4515(4) 0.3384(3) 0.7645(2) 0.0263(7) Uani 1 d . .
O21 O 0.5204(3) 0.4559(2) 0.79569(15) 0.0288(5) Uani 1 d . .
O22 O 0.2898(3) 0.2825(2) 0.7787(2) 0.0370(6) Uani 1 d . .
C28 C 0.2046(5) 0.3678(4) 0.8295(3) 0.0428(9) Uani 1 d . .
H28A H 0.0841(16) 0.3176(5) 0.8337(16) 0.064 Uiso 1 calc R .
H28B H 0.1895(33) 0.4333(16) 0.7986(10) 0.064 Uiso 1 calc R .
H28C H 0.2827(18) 0.4103(19) 0.8904(6) 0.064 Uiso 1 calc R .
S3 S 0.91926(12) 0.57249(8) 0.89503(5) 0.0300(2) Uani 1 d . .
C31 C 0.9732(4) 0.7167(3) 0.9810(2) 0.0265(7) Uani 1 d . .
C32 C 1.1388(5) 0.7450(3) 1.0446(2) 0.0351(8) Uani 1 d . .
H32 H 1.2120(5) 0.6881(3) 1.0368(2) 0.042 Uiso 1 calc R .
C33 C 1.1983(5) 0.8527(3) 1.1179(2) 0.0405(9) Uani 1 d . .
H33 H 1.3109(5) 0.8689(3) 1.1597(2) 0.049 Uiso 1 calc R .
C34 C 1.0950(5) 0.9376(3) 1.1311(3) 0.0427(9) Uani 1 d . .
H34 H 1.1365(5) 1.0122(3) 1.1816(3) 0.051 Uiso 1 calc R .
C35 C 0.9322(5) 0.9129(3) 1.0706(2) 0.0368(8) Uani 1 d . .
H35 H 0.8611(5) 0.9710(3) 1.0797(2) 0.044 Uiso 1 calc R .
C36 C 0.8680(4) 0.8032(3) 0.9951(2) 0.0281(7) Uani 1 d . .
C37 C 0.6938(4) 0.7834(3) 0.9325(2) 0.0277(7) Uani 1 d . .
O31 O 0.6331(3) 0.7077(2) 0.85615(14) 0.0271(5) Uani 1 d . .
O32 O 0.5929(3) 0.8562(2) 0.9646(2) 0.0380(6) Uani 1 d . .
C38 C 0.4231(5) 0.8438(4) 0.9024(3) 0.0442(9) Uani 1 d . .
H38A H 0.3609(19) 0.9026(20) 0.9315(7) 0.066 Uiso 1 calc R .
H38B H 0.3428(16) 0.7547(8) 0.8860(15) 0.066 Uiso 1 calc R .
H38C H 0.4515(6) 0.8656(25) 0.8478(8) 0.066 Uiso 1 calc R .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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_3
_geom_angle_publ_flag
O21 Co O31 83.90(9) . . ?
O21 Co O11 83.26(9) . . ?
O31 Co O11 83.64(9) . . ?
O21 Co S2 95.05(7) . . ?
O31 Co S2 177.17(7) . . ?
O11 Co S2 93.63(7) . . ?
O21 Co S1 176.87(7) . . ?
O31 Co S1 93.47(7) . . ?
O11 Co S1 94.78(7) . . ?
S2 Co S1 87.50(4) . . ?
O21 Co S3 93.47(7) . . ?
O31 Co S3 93.40(7) . . ?
O11 Co S3 175.79(7) . . ?
S2 Co S3 89.28(4) . . ?
S1 Co S3 88.37(4) . . ?
C11 S1 Co 108.69(11) . . ?
C12 C11 C16 117.3(3) . . ?
C12 C11 S1 113.8(2) . . ?
C16 C11 S1 128.9(2) . . ?
C13 C12 C11 122.2(3) . . ?
C12 C13 C14 120.4(3) . . ?
C15 C14 C13 119.0(3) . . ?
C14 C15 C16 121.3(3) . . ?
C11 C16 C15 119.8(3) . . ?
C11 C16 C17 122.2(3) . . ?
C15 C16 C17 118.0(3) . . ?
O11 C17 O12 119.3(3) . . ?
O11 C17 C16 127.4(3) . . ?
O12 C17 C16 113.3(3) . . ?
C17 O11 Co 133.7(2) . . ?
C17 O12 C18 116.2(3) . . ?
C21 S2 Co 109.73(11) . . ?
C22 C21 C26 117.6(3) . . ?
C22 C21 S2 113.7(2) . . ?
C26 C21 S2 128.7(3) . . ?
C23 C22 C21 122.0(3) . . ?
C22 C23 C24 120.5(3) . . ?
C25 C24 C23 118.7(3) . . ?
C24 C25 C26 121.9(3) . . ?
C21 C26 C25 119.2(3) . . ?
C21 C26 C27 122.4(3) . . ?
C25 C26 C27 118.3(3) . . ?
O21 C27 O22 119.3(3) . . ?
O21 C27 C26 126.9(3) . . ?
O22 C27 C26 113.8(3) . . ?
C27 O21 Co 135.3(2) . . ?
C27 O22 C28 116.1(3) . . ?
C31 S3 Co 107.80(11) . . ?
C32 C31 C36 117.4(3) . . ?
C32 C31 S3 114.7(2) . . ?
C36 C31 S3 127.9(2) . . ?
C33 C32 C31 121.9(3) . . ?
C32 C33 C34 120.5(3) . . ?
C35 C34 C33 119.2(3) . . ?
C34 C35 C36 121.5(3) . . ?
C35 C36 C31 119.5(3) . . ?
C35 C36 C37 118.6(3) . . ?
C31 C36 C37 121.8(3) . . ?
O31 C37 O32 118.4(3) . . ?
O31 C37 C36 127.3(3) . . ?
O32 C37 C36 114.2(3) . . ?
C37 O31 Co 134.0(2) . . ?
C37 O32 C38 115.7(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co O21 1.950(2) . ?
Co O31 1.960(2) . ?
Co O11 1.980(2) . ?
Co S2 2.1822(9) . ?
Co S1 2.1853(9) . ?
Co S3 2.1962(9) . ?
S1 C11 1.750(3) . ?
C11 C12 1.406(5) . ?
C11 C16 1.411(4) . ?
C12 C13 1.375(5) . ?
C13 C14 1.399(5) . ?
C14 C15 1.372(5) . ?
C15 C16 1.417(5) . ?
C16 C17 1.461(5) . ?
C17 O11 1.229(4) . ?
C17 O12 1.332(4) . ?
O12 C18 1.451(4) . ?
S2 C21 1.747(3) . ?
C21 C22 1.402(5) . ?
C21 C26 1.407(5) . ?
C22 C23 1.372(5) . ?
C23 C24 1.391(5) . ?
C24 C25 1.368(5) . ?
C25 C26 1.410(5) . ?
C26 C27 1.462(5) . ?
C27 O21 1.230(4) . ?
C27 O22 1.327(4) . ?
O22 C28 1.450(4) . ?
S3 C31 1.751(3) . ?
C31 C32 1.404(5) . ?
C31 C36 1.411(4) . ?
C32 C33 1.375(5) . ?
C33 C34 1.384(5) . ?
C34 C35 1.371(5) . ?
C35 C36 1.408(5) . ?
C36 C37 1.466(5) . ?
C37 O31 1.232(4) . ?
C37 O32 1.332(4) . ?
O32 C38 1.457(4) . ?
