#------------------------------------------------------------------------------
#$Date: 2025-07-06 17:02:57 +0200 (Sun 06 de Jul de 2025) $
#$Revision: 300696 $
#$URL: svn://www.crystallography.net/cod/cif/7/25/02/7250249.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_7250249
loop_
_publ_author_name
'Beleaev, Ecaterina S.'
'Kravtsov, Victor Ch.'
'Chumakov, Yurii'
'Baca, Svetlana G.'
_publ_section_title
;
 Multi-component supramolecular compounds containing hexaamminecobalt(iii)
 cations and aromatic sulfonic acid derivatives
;
_journal_issue                   19
_journal_name_full               CrystEngComm
_journal_page_first              3018
_journal_page_last               3031
_journal_paper_doi               10.1039/D5CE00184F
_journal_volume                  27
_journal_year                    2025
_chemical_formula_sum            'C7 H53 Cl2 Co2 N12 O16 S2'
_chemical_formula_weight         814.49
_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   mixed
_audit_creation_method           SHELXL-2019/1
_audit_update_record
;
2025-01-09 deposited with the CCDC.	2025-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                100.100(6)
_cell_angle_beta                 98.038(6)
_cell_angle_gamma                91.656(6)
_cell_formula_units_Z            2
_cell_length_a                   7.4383(5)
_cell_length_b                   12.0736(9)
_cell_length_c                   19.2979(12)
_cell_measurement_reflns_used    1613
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.1250
_cell_measurement_theta_min      3.3330
_cell_volume                     1686.9(2)
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.1082
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10656
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.049
_diffrn_reflns_theta_max         25.049
_diffrn_reflns_theta_min         2.999
_exptl_absorpt_coefficient_mu    1.341
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97310
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_description       needle
_exptl_crystal_F_000             854
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.851
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         5962
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1016
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0900P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1598
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3855
_reflns_number_total             5962
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5ce00184f2.cif
_cod_data_source_block           V_5731_NE
_cod_depositor_comments
'Adding full bibliography for 7250246--7250252.cif.'
_cod_database_code               7250249
_shelx_shelxl_version_number     2019/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_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_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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 1.000000 0.500000 1.000000 0.0222(3) Uani 1 2 d S . P . .
Co2 Co 0.41254(9) 0.46685(6) 0.67278(4) 0.0231(2) Uani 1 1 d . . . . .
Co3 Co 0.500000 1.000000 0.000000 0.0269(3) Uani 1 2 d S . P . .
C1 C 0.6226(7) -0.0598(5) 0.3892(3) 0.0339(14) Uani 1 1 d . . . . .
C2 C 0.7067(7) 0.0158(5) 0.4581(3) 0.0282(13) Uani 1 1 d . . . . .
C3 C 0.7619(7) -0.0304(5) 0.5180(3) 0.0375(15) Uani 1 1 d . . . . .
H3 H 0.748039 -0.107767 0.515778 0.045 Uiso 1 1 calc R U . . .
C4 C 0.8374(8) 0.0381(6) 0.5809(3) 0.0434(17) Uani 1 1 d . . . . .
H4 H 0.874833 0.006680 0.620826 0.052 Uiso 1 1 calc R U . . .
C5 C 0.8575(7) 0.1532(5) 0.5848(3) 0.0365(15) Uani 1 1 d . . . . .
H5 H 0.905503 0.199347 0.627587 0.044 Uiso 1 1 calc R U . . .
C6 C 0.8060(7) 0.2000(5) 0.5246(3) 0.0282(13) Uani 1 1 d . . . . .
C7 C 0.7268(7) 0.1311(5) 0.4628(3) 0.0297(14) Uani 1 1 d . . . . .
H7 H 0.685897 0.162805 0.423246 0.036 Uiso 1 1 calc R U . . .
N1 N 0.8302(5) 0.4300(4) 1.0509(2) 0.0290(11) Uani 1 1 d . . . . .
H1A H 0.721538 0.417638 1.024057 0.035 Uiso 1 1 calc R U . . .
H1B H 0.820616 0.475685 1.091549 0.035 Uiso 1 1 calc R U . . .
H1C H 0.871398 0.364802 1.060062 0.035 Uiso 1 1 calc R U . . .
N2 N 0.9681(6) 0.3628(4) 0.9269(2) 0.0323(12) Uani 1 1 d . . . . .
H2A H 1.052873 0.363680 0.898686 0.039 Uiso 1 1 calc R U . . .
H2B H 0.858435 0.359976 0.901152 0.039 Uiso 1 1 calc R U . . .
H2C H 0.978408 0.302661 0.947716 0.039 Uiso 1 1 calc R U . . .
N3 N 0.7971(5) 0.5661(4) 0.9488(2) 0.0294(11) Uani 1 1 d . . . . .
H3A H 0.739507 0.513947 0.913673 0.035 Uiso 1 1 calc R U . . .
H3B H 0.839175 0.622913 0.930709 0.035 Uiso 1 1 calc R U . . .
H3C H 0.720256 0.591467 0.978583 0.035 Uiso 1 1 calc R U . . .
N4 N 0.2339(5) 0.3664(4) 0.7002(2) 0.0315(12) Uani 1 1 d . . . . .
H4C H 0.123175 0.377308 0.679126 0.038 Uiso 1 1 calc R U . . .
H4A H 0.237120 0.381249 0.747233 0.038 Uiso 1 1 calc R U . . .
H4B H 0.260168 0.295133 0.686780 0.038 Uiso 1 1 calc R U . . .
N5 N 0.3570(6) 0.3818(4) 0.5750(2) 0.0317(12) Uani 1 1 d . . . . .
H5A H 0.254898 0.404943 0.553530 0.038 Uiso 1 1 calc R U . . .
H5B H 0.342988 0.308647 0.576083 0.038 Uiso 1 1 calc R U . . .
H5C H 0.447962 0.393157 0.551192 0.038 Uiso 1 1 calc R U . . .
N6 N 0.2241(6) 0.5727(4) 0.6532(3) 0.0357(12) Uani 1 1 d . . . . .
H6A H 0.157562 0.546862 0.611148 0.043 Uiso 1 1 calc R U . . .
H6B H 0.276595 0.639690 0.652717 0.043 Uiso 1 1 calc R U . . .
H6C H 0.152942 0.579504 0.687010 0.043 Uiso 1 1 calc R U . . .
N7 N 0.5957(6) 0.5628(4) 0.6438(3) 0.0358(12) Uani 1 1 d . . . . .
H7A H 0.612190 0.535184 0.599363 0.043 Uiso 1 1 calc R U . . .
H7B H 0.700259 0.564373 0.672772 0.043 Uiso 1 1 calc R U . . .
H7C H 0.557673 0.632416 0.646023 0.043 Uiso 1 1 calc R U . . .
N8 N 0.4719(6) 0.5488(4) 0.7705(2) 0.0378(13) Uani 1 1 d . . . . .
H8A H 0.401351 0.606900 0.776981 0.045 Uiso 1 1 calc R U . . .
H8B H 0.587989 0.573811 0.778577 0.045 Uiso 1 1 calc R U . . .
H8C H 0.453377 0.502940 0.800596 0.045 Uiso 1 1 calc R U . . .
N9 N 0.5978(5) 0.3616(4) 0.6943(2) 0.0294(11) Uani 1 1 d . . . . .
H9A H 0.565199 0.293833 0.668283 0.035 Uiso 1 1 calc R U . . .
H9B H 0.608938 0.357409 0.740317 0.035 Uiso 1 1 calc R U . . .
H9C H 0.703660 0.385742 0.684269 0.035 Uiso 1 1 calc R U . . .
N10 N 0.4824(7) 0.8396(4) -0.0411(3) 0.0452(14) Uani 1 1 d . . . . .
H10A H 0.373377 0.821537 -0.066971 0.068 Uiso 1 1 calc R U . . .
H10B H 0.497644 0.799535 -0.006399 0.068 Uiso 1 1 calc R U . . .
H10C H 0.568104 0.824654 -0.068802 0.068 Uiso 1 1 calc R U . . .
N11 N 0.3462(6) 0.9700(4) 0.0700(3) 0.0363(13) Uani 1 1 d . . . . .
H11A H 0.317802 0.896409 0.063408 0.054 Uiso 1 1 calc R U . . .
H11B H 0.244906 1.007024 0.064693 0.054 Uiso 1 1 calc R U . . .
H11C H 0.406099 0.992929 0.113705 0.054 Uiso 1 1 calc R U . . .
N12 N 0.7161(6) 0.9769(5) 0.0653(3) 0.0399(13) Uani 1 1 d . . . . .
H12A H 0.686511 0.930615 0.093551 0.048 Uiso 1 1 calc R U . . .
H12B H 0.759550 1.042773 0.091534 0.048 Uiso 1 1 calc R U . . .
H12C H 0.800366 0.946807 0.040376 0.048 Uiso 1 1 calc R U . . .
O1 O 0.6234(6) -0.1626(4) 0.3850(2) 0.0499(12) Uani 1 1 d . . . . .
O2 O 0.5566(6) -0.0110(4) 0.3388(2) 0.0446(11) Uani 1 1 d . . . . .
O3 O 0.9882(5) 0.3541(4) 0.4847(2) 0.0358(10) Uani 1 1 d . . . . .
O4 O 0.8928(5) 0.3983(3) 0.60060(19) 0.0360(10) Uani 1 1 d . . . . .
O5 O 0.6734(5) 0.3850(4) 0.4942(2) 0.0359(10) Uani 1 1 d . . . . .
O6 O 0.4298(8) 0.1982(4) 0.8645(3) 0.0828(19) Uani 1 1 d . . . . .
O7 O 0.2792(5) 0.3644(5) 0.8515(2) 0.0629(16) Uani 1 1 d . . . . .
O8 O 0.5963(5) 0.3599(4) 0.8508(2) 0.0503(14) Uani 1 1 d . . . . .
O9 O 0.4778(5) 0.3548(5) 0.9598(2) 0.0538(14) Uani 1 1 d . . . . .
O10 O 0.6984(7) 0.1355(7) 0.7648(4) 0.081(2) Uani 1 1 d . . . . .
H10W H 0.641(15) 0.149(11) 0.785(7) 0.121 Uiso 1 1 d . U . . .
H9W H 0.632(14) 0.093(9) 0.732(5) 0.121 Uiso 1 1 d . U . . .
O11 O 0.9244(7) 0.7775(6) 0.6428(3) 0.0746(16) Uani 1 1 d D . . . .
H11W H 0.964(10) 0.730(6) 0.614(4) 0.112 Uiso 1 1 d D U . . .
H12W H 1.008(8) 0.821(6) 0.666(4) 0.112 Uiso 1 1 d D U . . .
O12 O 0.5926(7) 0.8120(5) 0.6813(3) 0.0588(14) Uani 1 1 d . . . . .
H13W H 0.636(11) 0.813(7) 0.7196(15) 0.088 Uiso 1 1 d D U . . .
H14W H 0.544(10) 0.876(8) 0.669(4) 0.088 Uiso 1 1 d . U . . .
O13 O 0.1869(5) 0.9266(4) 0.7337(3) 0.0793(17) Uani 1 1 d G . . . .
H15W H 0.145129 0.980285 0.760518 0.119 Uiso 1 1 d G U . . .
H16W H 0.263163 0.953208 0.711155 0.119 Uiso 1 1 d G U . . .
O14 O 0.6792(4) 0.8052(4) 0.8273(3) 0.0753(17) Uani 1 1 d DG . . . .
H17W H 0.736750 0.868839 0.833489 0.113 Uiso 1 1 d DG U . . .
H18W H 0.740707 0.761819 0.850490 0.113 Uiso 1 1 d DG U . . .
O15 O 0.0531(8) 0.1383(4) 0.7601(7) 0.089(7) Uani 0.466(19) 1 d DG . P A 2
H19W H 0.120002 0.173938 0.794976 0.133 Uiso 0.466(19) 1 d DG U P A 2
H20W H -0.026434 0.101511 0.773280 0.133 Uiso 0.466(19) 1 d DG U P A 2
O16 O 0.0489(8) 0.1039(4) 0.8054(7) 0.075(5) Uani 0.534(19) 1 d G . P A 1
O17 O 0.2448(6) 0.7544(6) 0.8111(3) 0.0694(16) Uani 1 1 d G . . B 1
H21W H 0.219582 0.805318 0.786586 0.104 Uiso 1 1 d G U . B 1
H22W H 0.153929 0.707597 0.805307 0.104 Uiso 1 1 d G U . B 1
Cl1 Cl 0.9337(2) 0.55857(16) 0.78339(8) 0.0460(4) Uani 1 1 d D . . . .
Cl2 Cl 0.98940(19) 0.82512(14) 0.96518(9) 0.0446(4) Uani 1 1 d D . . . .
S1 S 0.84191(18) 0.34515(13) 0.52635(7) 0.0279(3) Uani 1 1 d . . . . .
S2 S 0.44612(17) 0.31942(13) 0.88229(7) 0.0261(3) Uani 1 1 d . . . . .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
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'
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
N3 Co1 N3 180.0(2) 2_767 . ?
N3 Co1 N1 90.03(18) 2_767 . ?
N3 Co1 N1 89.97(18) . . ?
N3 Co1 N1 89.97(18) 2_767 2_767 ?
N3 Co1 N1 90.03(18) . 2_767 ?
N1 Co1 N1 180.0(3) . 2_767 ?
N3 Co1 N2 89.18(19) 2_767 . ?
N3 Co1 N2 90.82(19) . . ?
N1 Co1 N2 88.4(2) . . ?
N1 Co1 N2 91.6(2) 2_767 . ?
N3 Co1 N2 90.82(19) 2_767 2_767 ?
N3 Co1 N2 89.18(19) . 2_767 ?
N1 Co1 N2 91.6(2) . 2_767 ?
N1 Co1 N2 88.4(2) 2_767 2_767 ?
N2 Co1 N2 180.0 . 2_767 ?
N9 Co2 N8 88.9(2) . . ?
N9 Co2 N4 88.35(19) . . ?
N8 Co2 N4 91.6(2) . . ?
N9 Co2 N7 90.1(2) . . ?
N8 Co2 N7 89.6(2) . . ?
N4 Co2 N7 178.0(2) . . ?
N9 Co2 N6 178.66(19) . . ?
N8 Co2 N6 90.1(2) . . ?
N4 Co2 N6 90.77(19) . . ?
N7 Co2 N6 90.8(2) . . ?
N9 Co2 N5 89.7(2) . . ?
N8 Co2 N5 178.6(2) . . ?
N4 Co2 N5 88.3(2) . . ?
N7 Co2 N5 90.5(2) . . ?
N6 Co2 N5 91.3(2) . . ?
N10 Co3 N10 180.0(3) 2_675 . ?
N10 Co3 N12 90.1(2) 2_675 . ?
N10 Co3 N12 89.9(2) . . ?
N10 Co3 N12 89.9(2) 2_675 2_675 ?
N10 Co3 N12 90.1(2) . 2_675 ?
N12 Co3 N12 180.0 . 2_675 ?
N10 Co3 N11 89.7(2) 2_675 2_675 ?
N10 Co3 N11 90.3(2) . 2_675 ?
N12 Co3 N11 90.23(19) . 2_675 ?
N12 Co3 N11 89.77(19) 2_675 2_675 ?
N10 Co3 N11 90.3(2) 2_675 . ?
N10 Co3 N11 89.7(2) . . ?
N12 Co3 N11 89.77(19) . . ?
N12 Co3 N11 90.23(19) 2_675 . ?
N11 Co3 N11 180.0 2_675 . ?
O1 C1 O2 124.4(6) . . ?
O1 C1 C2 119.0(5) . . ?
O2 C1 C2 116.7(5) . . ?
C7 C2 C3 119.0(5) . . ?
C7 C2 C1 121.0(5) . . ?
C3 C2 C1 120.1(6) . . ?
C4 C3 C2 120.2(6) . . ?
C3 C4 C5 120.3(5) . . ?
C4 C5 C6 119.9(6) . . ?
C7 C6 C5 119.2(6) . . ?
C7 C6 S1 119.8(4) . . ?
C5 C6 S1 121.1(5) . . ?
C6 C7 C2 121.4(5) . . ?
O3 S1 O5 112.0(2) . . ?
O3 S1 O4 112.3(2) . . ?
O5 S1 O4 112.3(3) . . ?
O3 S1 C6 105.2(3) . . ?
O5 S1 C6 107.4(2) . . ?
O4 S1 C6 107.0(2) . . ?
O6 S2 O8 108.9(3) . . ?
O6 S2 O7 108.9(3) . . ?
O8 S2 O7 108.2(3) . . ?
O6 S2 O9 109.6(3) . . ?
O8 S2 O9 110.6(3) . . ?
O7 S2 O9 110.7(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
Co1 N3 1.955(4) 2_767 ?
Co1 N3 1.955(4) . ?
Co1 N1 1.962(4) . ?
Co1 N1 1.962(4) 2_767 ?
Co1 N2 1.963(5) . ?
Co1 N2 1.963(5) 2_767 ?
Co2 N9 1.952(4) . ?
Co2 N8 1.954(5) . ?
Co2 N4 1.961(4) . ?
Co2 N7 1.965(4) . ?
Co2 N6 1.966(5) . ?
Co2 N5 1.965(5) . ?
Co3 N10 1.953(5) 2_675 ?
Co3 N10 1.953(5) . ?
Co3 N12 1.957(4) . ?
Co3 N12 1.957(4) 2_675 ?
Co3 N11 1.961(4) 2_675 ?
Co3 N11 1.961(4) . ?
C1 O1 1.231(7) . ?
C1 O2 1.271(7) . ?
C1 C2 1.518(8) . ?
C2 C7 1.382(8) . ?
C2 C3 1.386(8) . ?
C3 C4 1.379(9) . ?
C4 C5 1.381(9) . ?
C5 C6 1.390(7) . ?
C6 C7 1.374(8) . ?
C6 S1 1.759(6) . ?
O3 S1 1.452(4) . ?
O4 S1 1.456(4) . ?
O5 S1 1.453(4) . ?
O6 S2 1.441(5) . ?
O7 S2 1.461(4) . ?
O8 S2 1.455(4) . ?
O9 S2 1.465(4) . ?
