#------------------------------------------------------------------------------
#$Date: 2019-11-08 04:33:06 +0200 (Fri, 08 Nov 2019) $
#$Revision: 225377 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/27/1552779.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_1552779
loop_
_publ_author_name
'KUROGI, Chika'
'YONEMURA, Toshiaki'
_publ_section_title
;
 Crystal Structure of a Co(III) Complex with 2-Aminoethanethiol and
 Triethylenetetramine
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              43
_journal_paper_doi               10.2116/xraystruct.35.43
_journal_volume                  35
_journal_year                    2019
_chemical_formula_moiety         'C8 H24 Co N5 S, (C2 H5 O), Cl2'
_chemical_formula_sum            'C10 H29 Cl2 Co N5 O S'
_chemical_formula_weight         397.27
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                64.70(3)
_cell_angle_beta                 95.76(3)
_cell_angle_gamma                91.17(4)
_cell_formula_units_Z            2
_cell_length_a                   8.279(3)
_cell_length_b                   10.673(5)
_cell_length_c                   10.696(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296
_cell_measurement_theta_max      17.14
_cell_measurement_theta_min      15.02
_cell_volume                     849.9(6)
_computing_cell_refinement       WinAFC
_computing_data_collection       WinAFC
_computing_data_reduction        WinAFC
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku AFC7S'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4760
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         27.538
_diffrn_reflns_theta_min         3.089
_diffrn_standards_decay_%        -2.758
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.450
_exptl_absorpt_correction_T_max  0.602
_exptl_absorpt_correction_T_min  0.384
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             418.00
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.350
_refine_diff_density_max         0.69
_refine_diff_density_min         -0.79
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3913
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0644P)²+0.6283P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1145
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3710
_reflns_number_total             3913
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            35_43_1.txt
_cod_data_source_block           Co(aet)(trien)-EL2
_cod_database_code               1552779
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Co1 Co 0.20800(3) 0.29478(3) 0.85611(3) 0.03005(11) Uani 1 1 d . . .
Cl1 Cl 0.77660(9) 0.30050(8) 1.08389(9) 0.05228(18) Uani 1 1 d . . .
Cl2 Cl 0.19269(9) 0.43420(8) 0.40640(7) 0.05054(18) Uani 1 1 d . . .
S1 S 0.24023(8) 0.08623(6) 1.04226(7) 0.04150(16) Uani 1 1 d . . .
O1 O 0.6482(18) 0.1055(14) 0.5282(12) 0.175(4) Uani 0.5 1 d D U P
O2 O 0.534(4) 0.0546(19) 0.4605(15) 0.151(6) Uani 0.25 1 d . U P
O3 O 0.440(3) 0.122(2) 0.4716(19) 0.159(6) Uani 0.25 1 d . U P
N1 N 0.1631(3) 0.3691(2) 0.9901(3) 0.0455(5) Uani 1 1 d . . .
H1 H 0.196577 0.455946 0.959375 0.055 Uiso 1 1 calc R U .
H2 H 0.056247 0.370925 0.993680 0.055 Uiso 1 1 calc R U .
N2 N 0.1962(3) 0.4878(2) 0.7016(3) 0.0449(5) Uani 1 1 d . . .
H3 H 0.145772 0.486678 0.624614 0.054 Uiso 1 1 calc R U .
H4 H 0.139194 0.543159 0.724691 0.054 Uiso 1 1 calc R U .
N3 N 0.4431(2) 0.3215(2) 0.8670(2) 0.0367(4) Uani 1 1 d . . .
H5 H 0.486840 0.279800 0.965095 0.044 Uiso 1 1 calc R U .
N4 N 0.2481(2) 0.2151(2) 0.7293(2) 0.0373(4) Uani 1 1 d . . .
H6 H 0.248551 0.291436 0.636384 0.045 Uiso 1 1 calc R U .
N5 N -0.0232(2) 0.2602(2) 0.8195(2) 0.0398(4) Uani 1 1 d . . .
H7 H -0.059484 0.197588 0.897012 0.048 Uiso 1 1 calc R U .
H8 H -0.081740 0.338194 0.791575 0.048 Uiso 1 1 calc R U .
C1 C 0.1969(5) 0.1386(3) 1.1761(3) 0.0581(8) Uani 1 1 d . . .
H9 H 0.082368 0.128430 1.189322 0.070 Uiso 1 1 calc R U .
H10 H 0.258714 0.080408 1.263469 0.070 Uiso 1 1 calc R U .
C2 C 0.2425(4) 0.2877(3) 1.1321(3) 0.0567(7) Uani 1 1 d . . .
H11 H 0.206456 0.321895 1.195622 0.068 Uiso 1 1 calc R U .
H12 H 0.359498 0.295988 1.132794 0.068 Uiso 1 1 calc R U .
C3 C 0.3610(3) 0.5421(3) 0.6752(3) 0.0473(6) Uani 1 1 d . . .
H13 H 0.359079 0.641670 0.645106 0.057 Uiso 1 1 calc R U .
H14 H 0.399973 0.522807 0.602466 0.057 Uiso 1 1 calc R U .
C4 C 0.4718(3) 0.4727(3) 0.8079(3) 0.0421(5) Uani 1 1 d . . .
H15 H 0.584279 0.490237 0.788985 0.051 Uiso 1 1 calc R U .
H16 H 0.449212 0.509128 0.873493 0.051 Uiso 1 1 calc R U .
C5 C 0.5243(3) 0.2521(3) 0.7931(4) 0.0480(6) Uani 1 1 d . . .
H17 H 0.623396 0.204794 0.848222 0.058 Uiso 1 1 calc R U .
H18 H 0.552865 0.321332 0.704457 0.058 Uiso 1 1 calc R U .
C6 C 0.4121(3) 0.1486(3) 0.7696(3) 0.0467(6) Uani 1 1 d . . .
H19 H 0.445945 0.127576 0.696356 0.056 Uiso 1 1 calc R U .
H20 H 0.412677 0.063224 0.853938 0.056 Uiso 1 1 calc R U .
C7 C 0.1103(3) 0.1249(3) 0.7244(3) 0.0449(6) Uani 1 1 d . . .
H21 H 0.115984 0.039275 0.808829 0.054 Uiso 1 1 calc R U .
H22 H 0.111610 0.102684 0.645516 0.054 Uiso 1 1 calc R U .
C8 C -0.0408(3) 0.2087(3) 0.7103(3) 0.0447(6) Uani 1 1 d . . .
H23 H -0.054590 0.286211 0.619085 0.054 Uiso 1 1 calc R U .
H24 H -0.135573 0.151449 0.721115 0.054 Uiso 1 1 calc R U .
C9 C 0.7609(15) 0.0995(15) 0.4258(17) 0.358(14) Uani 1 1 d D U .
H25 H 0.698024 0.135986 0.335519 0.430 Uiso 1 1 calc R U .
H26 H 0.781330 0.001936 0.451529 0.430 Uiso 1 1 calc R U .
C10 C 0.9295(10) 0.1702(11) 0.4025(7) 0.164(3) Uani 1 1 d D U .
H27 H 0.926752 0.240567 0.308842 0.196 Uiso 1 1 calc R U .
H28 H 1.012288 0.101877 0.418231 0.196 Uiso 1 1 calc R U .
H29 H 0.952978 0.211435 0.466166 0.196 Uiso 1 1 calc R U .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Co Co 0.3494 0.9721
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
C C 0.0033 0.0016
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(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
N4 Co1 N3 85.00(9) . .
N4 Co1 N5 85.69(9) . .
N3 Co1 N5 170.54(9) . .
N4 Co1 N1 177.72(9) . .
N3 Co1 N1 96.25(10) . .
N5 Co1 N1 93.11(10) . .
N4 Co1 N2 91.63(11) . .
N3 Co1 N2 84.93(10) . .
N5 Co1 N2 93.65(10) . .
N1 Co1 N2 90.39(11) . .
N4 Co1 S1 92.12(8) . .
N3 Co1 S1 90.73(8) . .
N5 Co1 S1 91.30(8) . .
N1 Co1 S1 85.96(8) . .
N2 Co1 S1 174.00(7) . .
C1 S1 Co1 98.96(12) . .
O2 O1 C9 84.7(13) . .
O2 O1 O3 39.6(13) . .
C9 O1 O3 115.7(12) . .
O3 O2 O2 91(3) . 2_656
O3 O2 O1 88.9(14) . .
O2 O2 O1 114.6(19) 2_656 .
O3 O2 O3 132(2) . 2_656
O2 O2 O3 40.8(18) 2_656 2_656
O1 O2 O3 108.7(17) . 2_656
O2 O3 O2 48(2) . 2_656
O2 O3 O1 51.5(16) . .
O2 O3 O1 79.8(18) 2_656 .
C2 N1 Co1 113.60(19) . .
C2 N1 H1 108.8 . .
Co1 N1 H1 108.8 . .
C2 N1 H2 108.8 . .
Co1 N1 H2 108.8 . .
H1 N1 H2 107.7 . .
C3 N2 Co1 110.41(18) . .
C3 N2 H3 109.6 . .
Co1 N2 H3 109.6 . .
C3 N2 H4 109.6 . .
Co1 N2 H4 109.6 . .
H3 N2 H4 108.1 . .
C4 N3 C5 112.1(2) . .
C4 N3 Co1 108.18(16) . .
C5 N3 Co1 110.76(16) . .
C4 N3 H5 108.6 . .
C5 N3 H5 108.6 . .
Co1 N3 H5 108.6 . .
C6 N4 C7 116.5(2) . .
C6 N4 Co1 108.74(17) . .
C7 N4 Co1 108.60(16) . .
C6 N4 H6 107.6 . .
C7 N4 H6 107.6 . .
Co1 N4 H6 107.6 . .
C8 N5 Co1 109.20(16) . .
C8 N5 H7 109.8 . .
Co1 N5 H7 109.8 . .
C8 N5 H8 109.8 . .
Co1 N5 H8 109.8 . .
H7 N5 H8 108.3 . .
C2 C1 S1 108.7(2) . .
C2 C1 H9 109.9 . .
S1 C1 H9 109.9 . .
C2 C1 H10 109.9 . .
S1 C1 H10 109.9 . .
H9 C1 H10 108.3 . .
N1 C2 C1 107.8(2) . .
N1 C2 H11 110.1 . .
C1 C2 H11 110.1 . .
N1 C2 H12 110.1 . .
C1 C2 H12 110.1 . .
H11 C2 H12 108.5 . .
N2 C3 C4 108.4(2) . .
N2 C3 H13 110.0 . .
C4 C3 H13 110.0 . .
N2 C3 H14 110.0 . .
C4 C3 H14 110.0 . .
H13 C3 H14 108.4 . .
N3 C4 C3 108.2(2) . .
N3 C4 H15 110.1 . .
C3 C4 H15 110.1 . .
N3 C4 H16 110.1 . .
C3 C4 H16 110.1 . .
H15 C4 H16 108.4 . .
N3 C5 C6 110.3(2) . .
N3 C5 H17 109.6 . .
C6 C5 H17 109.6 . .
N3 C5 H18 109.6 . .
C6 C5 H18 109.6 . .
H17 C5 H18 108.1 . .
N4 C6 C5 106.1(2) . .
N4 C6 H19 110.5 . .
C5 C6 H19 110.5 . .
N4 C6 H20 110.5 . .
C5 C6 H20 110.5 . .
H19 C6 H20 108.7 . .
N4 C7 C8 105.2(2) . .
N4 C7 H21 110.7 . .
C8 C7 H21 110.7 . .
N4 C7 H22 110.7 . .
C8 C7 H22 110.7 . .
H21 C7 H22 108.8 . .
N5 C8 C7 108.4(2) . .
N5 C8 H23 110.0 . .
C7 C8 H23 110.0 . .
N5 C8 H24 110.0 . .
C7 C8 H24 110.0 . .
H23 C8 H24 108.4 . .
O1 C9 C10 124.2(11) . .
O1 C9 H25 106.3 . .
C10 C9 H25 106.3 . .
O1 C9 H26 106.3 . .
C10 C9 H26 106.3 . .
H25 C9 H26 106.4 . .
C9 C10 H27 109.5 . .
C9 C10 H28 109.5 . .
H27 C10 H28 109.5 . .
C9 C10 H29 109.5 . .
H27 C10 H29 109.5 . .
H28 C10 H29 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N4 1.939(2) .
Co1 N3 1.961(2) .
Co1 N5 1.975(2) .
Co1 N1 1.977(2) .
Co1 N2 2.013(2) .
Co1 S1 2.2627(14) .
S1 C1 1.813(3) .
O1 O2 1.38(2) .
O1 C9 1.530(13) .
O1 O3 1.76(3) .
O2 O3 1.12(4) .
O2 O2 1.27(3) 2_656
O2 O3 1.72(3) 2_656
N1 C2 1.480(4) .
N1 H1 0.8900 .
N1 H2 0.8900 .
N2 C3 1.477(3) .
N2 H3 0.8900 .
N2 H4 0.8900 .
N3 C4 1.484(3) .
N3 C5 1.501(3) .
N3 H5 0.9800 .
N4 C6 1.480(3) .
N4 C7 1.489(3) .
N4 H6 0.9800 .
N5 C8 1.482(4) .
N5 H7 0.8900 .
N5 H8 0.8900 .
C1 C2 1.506(4) .
C1 H9 0.9700 .
C1 H10 0.9700 .
C2 H11 0.9700 .
C2 H12 0.9700 .
C3 C4 1.508(4) .
C3 H13 0.9700 .
C3 H14 0.9700 .
C4 H15 0.9700 .
C4 H16 0.9700 .
C5 C6 1.514(4) .
C5 H17 0.9700 .
C5 H18 0.9700 .
C6 H19 0.9700 .
C6 H20 0.9700 .
C7 C8 1.511(4) .
C7 H21 0.9700 .
C7 H22 0.9700 .
C8 H23 0.9700 .
C8 H24 0.9700 .
C9 C10 1.564(9) .
C9 H25 0.9700 .
C9 H26 0.9700 .
C10 H27 0.9600 .
C10 H28 0.9600 .
C10 H29 0.9600 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N4 H6 Cl2 3.230(3) 0.980 2.277 163.9 no
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_4
C9 O1 O2 O3 -142.4(15) . .
C9 O1 O2 O2 127(4) . 2_656
O3 O1 O2 O2 -91(4) . 2_656
C9 O1 O2 O3 82.9(19) . 2_656
O3 O1 O2 O3 -135(2) . 2_656
O1 O2 O3 O2 -114.6(19) . 2_656
O3 O2 O3 O2 0.001(4) 2_656 2_656
O2 O2 O3 O1 114.6(19) 2_656 .
O3 O2 O3 O1 114.6(19) 2_656 .
C9 O1 O3 O2 42.3(17) . .
O2 O1 O3 O2 43.2(18) . 2_656
C9 O1 O3 O2 85.5(13) . 2_656
Co1 S1 C1 C2 -28.5(3) . .
Co1 N1 C2 C1 -53.1(3) . .
S1 C1 C2 N1 51.8(3) . .
Co1 N2 C3 C4 -27.4(3) . .
C5 N3 C4 C3 77.8(3) . .
Co1 N3 C4 C3 -44.6(2) . .
N2 C3 C4 N3 47.0(3) . .
C4 N3 C5 C6 -137.6(2) . .
Co1 N3 C5 C6 -16.7(3) . .
C7 N4 C6 C5 -169.6(2) . .
Co1 N4 C6 C5 -46.5(3) . .
N3 C5 C6 N4 40.5(3) . .
C6 N4 C7 C8 168.7(2) . .
Co1 N4 C7 C8 45.6(2) . .
Co1 N5 C8 C7 32.5(2) . .
N4 C7 C8 N5 -50.7(3) . .
O2 O1 C9 C10 167.2(16) . .
O3 O1 C9 C10 141.7(15) . .
