#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/31/7013143.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_7013143
loop_
_publ_author_name
'Clint A. Sharrad'
'Stefan R. Lüthi'
'Lawrence R. Gahan'
_publ_section_title
;
 Embracing ligands. A synthetic strategy towards new
 nitrogen--thioether multidentate ligands and characterization of the
 cobalt(III) complexes
;
_journal_issue                   19
_journal_name_full               'Dalton Trans.'
_journal_page_first              3693
_journal_page_last               3703
_journal_paper_doi               10.1039/b304914k
_journal_year                    2003
_chemical_formula_sum            'C12 H30 Cl2 Co F6 N3 O1.5 P S2'
_chemical_formula_weight         579.31
_chemical_name_common            endo-(Co(EtHON3S2amp)Cl)Cl(PF6).0.5H2O
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2003-07-25T10:15:30-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 102.07(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.357(5)
_cell_length_b                   6.908(1)
_cell_length_c                   21.547(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     4418.6(14)
_computing_cell_refinement       SET4
_computing_data_collection       CAD4
_computing_data_reduction        XTAL3.2
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       'omega-2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.1279
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            3971
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        'less than 5 %'
_exptl_absorpt_coefficient_mu    1.342
_exptl_absorpt_correction_type   psiscans
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         3892
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.1575
_refine_ls_R_factor_obs          0.0484
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0596P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1378
_refine_ls_wR_factor_obs         0.1029
_reflns_number_gt                1828
_reflns_number_total             3892
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b304914k.txt
_cod_data_source_block           1923cs32
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C12 H30 Cl2 Co F6 N3 O1.50 P S2'
_cod_database_code               7013143
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.59387(3) 0.17474(15) 0.07575(4) 0.0268(3) Uani 1 1 d . . .
Cl2 Cl 0.54864(6) 0.6566(3) -0.04261(9) 0.0455(5) Uani 1 1 d . . .
S2 S 0.64107(6) 0.1274(3) 0.16901(8) 0.0351(5) Uani 1 1 d . . .
Cl1 Cl 0.54653(6) -0.0502(3) 0.10371(8) 0.0408(5) Uani 1 1 d . . .
S1 S 0.64113(5) 0.3941(3) 0.05421(8) 0.0325(5) Uani 1 1 d . . .
N2 N 0.62344(17) -0.0412(8) 0.0410(2) 0.0312(14) Uani 1 1 d . . .
H2A H 0.6449 -0.0867 0.073 0.037 Uiso 1 1 calc R . .
H2B H 0.6027 -0.1356 0.0311 0.037 Uiso 1 1 calc R . .
N3 N 0.55767(16) 0.3798(9) 0.1061(2) 0.0354(16) Uani 1 1 d . . .
H3A H 0.571 0.4931 0.1006 0.043 Uiso 1 1 calc R . .
H3B H 0.5307 0.3806 0.079 0.043 Uiso 1 1 calc R . .
O1 O 0.5518(3) 0.2612(13) 0.3024(3) 0.100(3) Uani 1 1 d . . .
H1 H 0.5453 0.2732 0.3373 0.15 Uiso 1 1 calc R . .
N1 N 0.55631(16) 0.2072(9) -0.0101(2) 0.0346(15) Uani 1 1 d . . .
H1A H 0.5315 0.1341 -0.0122 0.042 Uiso 1 1 calc R . .
H1B H 0.5471 0.3314 -0.0137 0.042 Uiso 1 1 calc R . .
C4 C 0.6448(2) -0.0175(12) -0.0149(3) 0.0382(19) Uani 1 1 d . . .
H4A H 0.6395 -0.1331 -0.0409 0.046 Uiso 1 1 calc R . .
H4B H 0.6771 -0.0032 -0.0002 0.046 Uiso 1 1 calc R . .
C3 C 0.5747(2) 0.1617(12) -0.0671(3) 0.0369(18) Uani 1 1 d . . .
H3C H 0.5639 0.2577 -0.0995 0.044 Uiso 1 1 calc R . .
H3D H 0.5632 0.0368 -0.0835 0.044 Uiso 1 1 calc R . .
C5 C 0.6464(2) 0.3483(11) -0.0266(3) 0.0384(19) Uani 1 1 d . . .
H5A H 0.6316 0.4527 -0.0532 0.046 Uiso 1 1 calc R . .
H5B H 0.6781 0.3516 -0.0281 0.046 Uiso 1 1 calc R . .
C9 C 0.5482(2) 0.3853(11) 0.1713(3) 0.0389(19) Uani 1 1 d . . .
H9A H 0.5318 0.2689 0.1776 0.047 Uiso 1 1 calc R . .
H9B H 0.5286 0.4947 0.174 0.047 Uiso 1 1 calc R . .
C2 C 0.6266(2) 0.1566(11) -0.0547(3) 0.0360(17) Uani 1 1 d . . .
C11 C 0.5894(2) 0.4009(12) 0.2250(3) 0.039(2) Uani 1 1 d . . .
C7 C 0.6897(2) 0.2832(12) 0.1688(3) 0.044(2) Uani 1 1 d . . .
H7A H 0.6853 0.4079 0.1873 0.053 Uiso 1 1 calc R . .
H7B H 0.7167 0.2246 0.1937 0.053 Uiso 1 1 calc R . .
C8 C 0.6179(2) 0.2143(12) 0.2338(3) 0.038(2) Uani 1 1 d . . .
H8A H 0.5993 0.1118 0.2455 0.045 Uiso 1 1 calc R . .
H8B H 0.6427 0.2342 0.2697 0.045 Uiso 1 1 calc R . .
C12 C 0.6157(3) 0.5859(12) 0.2173(4) 0.049(2) Uani 1 1 d . . .
H12A H 0.6419 0.5938 0.2509 0.074 Uiso 1 1 calc R . .
H12B H 0.5969 0.6967 0.2189 0.074 Uiso 1 1 calc R . .
H12C H 0.6248 0.583 0.1772 0.074 Uiso 1 1 calc R . .
C6 C 0.6947(2) 0.3094(13) 0.1009(3) 0.042(2) Uani 1 1 d . . .
H6A H 0.7029 0.1874 0.0841 0.051 Uiso 1 1 calc R . .
H6B H 0.7182 0.403 0.0991 0.051 Uiso 1 1 calc R . .
C1 C 0.6391(3) 0.1349(12) -0.1201(3) 0.056(2) Uani 1 1 d . . .
H1C H 0.6275 0.2432 -0.1464 0.085 Uiso 1 1 calc R . .
H1D H 0.6263 0.0173 -0.1399 0.085 Uiso 1 1 calc R . .
H1E H 0.6713 0.1305 -0.1148 0.085 Uiso 1 1 calc R . .
C10 C 0.5731(3) 0.4320(15) 0.2874(4) 0.063(3) Uani 1 1 d . . .
H10A H 0.5985 0.4628 0.3214 0.076 Uiso 1 1 calc R . .
H10B H 0.552 0.5393 0.2827 0.076 Uiso 1 1 calc R . .
P1 P 0.76727(6) -0.1822(4) 0.12302(9) 0.0419(5) Uani 1 1 d . . .
F4 F 0.75981(14) -0.0166(7) 0.0712(2) 0.0630(14) Uani 1 1 d . . .
F3 F 0.71422(13) -0.1852(9) 0.1207(2) 0.0716(16) Uani 1 1 d . . .
F6 F 0.81992(13) -0.1774(8) 0.1246(2) 0.0671(14) Uani 1 1 d . . .
F1 F 0.77458(14) -0.3474(8) 0.1748(2) 0.0634(14) Uani 1 1 d . . .
F5 F 0.76099(16) -0.3423(8) 0.0694(2) 0.0695(15) Uani 1 1 d . . .
F2 F 0.77377(17) -0.0254(9) 0.1775(2) 0.0838(17) Uani 1 1 d . . .
O2 O 0.5 0.874(3) 0.25 0.224(8) Uani 1 2 d S . .
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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'
Cl Cl 0.1484 0.1585 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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
N2 Co1 N1 87.1(2) . . ?
N2 Co1 N3 173.7(2) . . ?
N1 Co1 N3 88.7(2) . . ?
N2 Co1 S1 94.15(17) . . ?
N1 Co1 S1 89.90(18) . . ?
N3 Co1 S1 90.47(18) . . ?
N2 Co1 S2 88.47(16) . . ?
N1 Co1 S2 175.00(17) . . ?
N3 Co1 S2 95.92(15) . . ?
S1 Co1 S2 88.10(7) . . ?
N2 Co1 Cl1 86.96(17) . . ?
N1 Co1 Cl1 93.03(17) . . ?
N3 Co1 Cl1 88.65(17) . . ?
S1 Co1 Cl1 176.92(8) . . ?
S2 Co1 Cl1 89.06(7) . . ?
C8 S2 C7 104.7(4) . . ?
C8 S2 Co1 111.6(2) . . ?
C7 S2 Co1 106.1(2) . . ?
C5 S1 C6 103.2(3) . . ?
C5 S1 Co1 105.9(2) . . ?
C6 S1 Co1 102.0(3) . . ?
C4 N2 Co1 122.3(4) . . ?
C9 N3 Co1 123.9(4) . . ?
C3 N1 Co1 120.5(4) . . ?
N2 C4 C2 112.1(6) . . ?
N1 C3 C2 114.2(5) . . ?
C2 C5 S1 115.3(5) . . ?
N3 C9 C11 115.3(5) . . ?
C4 C2 C5 113.4(6) . . ?
C4 C2 C1 108.1(6) . . ?
C5 C2 C1 107.3(6) . . ?
C4 C2 C3 110.8(6) . . ?
C5 C2 C3 110.5(6) . . ?
C1 C2 C3 106.4(6) . . ?
C9 C11 C12 109.9(6) . . ?
C9 C11 C8 112.7(6) . . ?
C12 C11 C8 114.8(6) . . ?
C9 C11 C10 108.0(6) . . ?
C12 C11 C10 104.4(7) . . ?
C8 C11 C10 106.4(6) . . ?
C6 C7 S2 108.5(5) . . ?
C11 C8 S2 119.0(5) . . ?
C7 C6 S1 108.3(5) . . ?
O1 C10 C11 109.2(8) . . ?
F2 P1 F1 89.6(3) . . ?
F2 P1 F5 179.0(4) . . ?
F1 P1 F5 89.4(3) . . ?
F2 P1 F4 90.3(3) . . ?
F1 P1 F4 179.8(3) . . ?
F5 P1 F4 90.7(3) . . ?
F2 P1 F6 90.0(3) . . ?
F1 P1 F6 90.4(3) . . ?
F5 P1 F6 89.9(3) . . ?
F4 P1 F6 89.7(3) . . ?
F2 P1 F3 90.0(3) . . ?
F1 P1 F3 90.3(3) . . ?
F5 P1 F3 90.1(3) . . ?
F4 P1 F3 89.6(3) . . ?
F6 P1 F3 179.3(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
Co1 N2 1.968(6) . ?
Co1 N1 1.973(5) . ?
Co1 N3 1.986(6) . ?
Co1 S1 2.202(2) . ?
Co1 S2 2.2348(19) . ?
Co1 Cl1 2.281(2) . ?
S2 C8 1.793(7) . ?
S2 C7 1.827(7) . ?
S1 C5 1.809(7) . ?
S1 C6 1.821(6) . ?
N2 C4 1.492(8) . ?
N3 C9 1.492(8) . ?
O1 C10 1.415(11) . ?
N1 C3 1.485(8) . ?
C4 C2 1.514(10) . ?
C3 C2 1.542(8) . ?
C5 C2 1.526(10) . ?
C9 C11 1.520(9) . ?
C2 C1 1.541(9) . ?
C11 C12 1.534(10) . ?
C11 C8 1.542(10) . ?
C11 C10 1.544(10) . ?
C7 C6 1.512(10) . ?
P1 F2 1.579(6) . ?
P1 F1 1.579(5) . ?
P1 F5 1.582(5) . ?
P1 F4 1.582(5) . ?
P1 F6 1.592(4) . ?
P1 F3 1.601(4) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Co1 S2 C8 -155.3(3) . . . . ?
N1 Co1 S2 C8 177(2) . . . . ?
N3 Co1 S2 C8 20.2(3) . . . . ?
S1 Co1 S2 C8 110.5(3) . . . . ?
Cl1 Co1 S2 C8 -68.3(3) . . . . ?
N2 Co1 S2 C7 91.2(3) . . . . ?
N1 Co1 S2 C7 63(2) . . . . ?
N3 Co1 S2 C7 -93.3(3) . . . . ?
S1 Co1 S2 C7 -3.0(3) . . . . ?
Cl1 Co1 S2 C7 178.2(3) . . . . ?
N2 Co1 S1 C5 46.7(3) . . . . ?
N1 Co1 S1 C5 -40.4(3) . . . . ?
N3 Co1 S1 C5 -129.0(3) . . . . ?
S2 Co1 S1 C5 135.1(3) . . . . ?
Cl1 Co1 S1 C5 157.7(16) . . . . ?
N2 Co1 S1 C6 -60.9(3) . . . . ?
N1 Co1 S1 C6 -148.0(3) . . . . ?
N3 Co1 S1 C6 123.3(3) . . . . ?
S2 Co1 S1 C6 27.4(3) . . . . ?
Cl1 Co1 S1 C6 50.1(17) . . . . ?
N1 Co1 N2 C4 55.5(5) . . . . ?
N3 Co1 N2 C4 103(2) . . . . ?
S1 Co1 N2 C4 -34.2(5) . . . . ?
S2 Co1 N2 C4 -122.2(5) . . . . ?
Cl1 Co1 N2 C4 148.6(5) . . . . ?
N2 Co1 N3 C9 101(2) . . . . ?
N1 Co1 N3 C9 148.2(5) . . . . ?
S1 Co1 N3 C9 -121.9(5) . . . . ?
S2 Co1 N3 C9 -33.8(5) . . . . ?
Cl1 Co1 N3 C9 55.2(5) . . . . ?
N2 Co1 N1 C3 -32.0(6) . . . . ?
N3 Co1 N1 C3 152.7(6) . . . . ?
S1 Co1 N1 C3 62.2(5) . . . . ?
S2 Co1 N1 C3 -4(3) . . . . ?
Cl1 Co1 N1 C3 -118.8(5) . . . . ?
Co1 N2 C4 C2 -21.5(7) . . . . ?
Co1 N1 C3 C2 -19.4(9) . . . . ?
C6 S1 C5 C2 94.8(6) . . . . ?
Co1 S1 C5 C2 -12.0(6) . . . . ?
Co1 N3 C9 C11 61.2(8) . . . . ?
N2 C4 C2 C5 78.2(7) . . . . ?
N2 C4 C2 C1 -163.0(6) . . . . ?
N2 C4 C2 C3 -46.8(8) . . . . ?
S1 C5 C2 C4 -54.4(7) . . . . ?
S1 C5 C2 C1 -173.7(5) . . . . ?
S1 C5 C2 C3 70.7(6) . . . . ?
N1 C3 C2 C4 70.1(8) . . . . ?
N1 C3 C2 C5 -56.5(8) . . . . ?
N1 C3 C2 C1 -172.6(6) . . . . ?
N3 C9 C11 C12 59.3(8) . . . . ?
N3 C9 C11 C8 -70.1(8) . . . . ?
N3 C9 C11 C10 172.6(7) . . . . ?
C8 S2 C7 C6 -146.8(5) . . . . ?
Co1 S2 C7 C6 -28.6(6) . . . . ?
C9 C11 C8 S2 59.6(8) . . . . ?
C12 C11 C8 S2 -67.3(7) . . . . ?
C10 C11 C8 S2 177.8(6) . . . . ?
C7 S2 C8 C11 77.4(6) . . . . ?
Co1 S2 C8 C11 -36.9(6) . . . . ?
S2 C7 C6 S1 53.4(7) . . . . ?
C5 S1 C6 C7 -163.2(5) . . . . ?
Co1 S1 C6 C7 -53.4(6) . . . . ?
C9 C11 C10 O1 68.4(9) . . . . ?
C12 C11 C10 O1 -174.6(7) . . . . ?
C8 C11 C10 O1 -52.8(9) . . . . ?
