#------------------------------------------------------------------------------
#$Date: 2025-04-09 01:47:09 +0300 (Wed, 09 Apr 2025) $
#$Revision: 299221 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/25/02/7250251.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_7250251
loop_
_publ_author_name
'Ecaterina, Beleaev'
'Kravtsov, Victor Ch.'
'Chumakov, Yuri'
'Baca, Svetlana G.'
_publ_section_title
;
 Multi-component supramolecular compounds containing hexaamminecobalt(III)
 cations and aromatic sulfonic acid derivatives
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D5CE00184F
_journal_year                    2025
_chemical_formula_sum            'C7 H22 Cl2 Co N6 Na O5.69 S'
_chemical_formula_weight         466.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 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                90
_cell_angle_beta                 97.903(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.489(3)
_cell_length_b                   6.8710(10)
_cell_length_c                   17.692(3)
_cell_measurement_reflns_used    636
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.9450
_cell_measurement_theta_min      3.5750
_cell_volume                     1744.6(5)
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9914
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1594
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            3869
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.242
_diffrn_reflns_theta_min         3.185
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.470
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69523
_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    1.775
_exptl_crystal_description       needle
_exptl_crystal_F_000             958
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.887
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         3869
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0130P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0902
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2089
_reflns_number_total             3869
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5ce00184f2.cif
_cod_data_source_block           V_5860_twin1_hklf5
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               7250251
_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+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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 0.06324(12) 0.250000 0.33233(9) 0.0158(4) Uani 1 2 d S T P . .
Co2 Co 0.37886(12) 0.750000 0.83879(9) 0.0188(5) Uani 1 2 d S T P . .
Na1 Na 0.2423(3) 0.250000 0.6070(3) 0.0244(13) Uani 1 2 d S T P . .
Na2 Na 0.7236(4) 1.250000 0.8880(3) 0.0326(14) Uani 1 2 d S T P . .
Cl1 Cl 0.0538(2) 0.250000 0.57909(16) 0.0284(9) Uani 1 2 d S T P . .
Cl2 Cl 0.2273(2) 0.250000 0.76242(16) 0.0336(9) Uani 1 2 d S T P . .
Cl3 Cl 0.8216(2) 1.250000 0.74435(17) 0.0291(9) Uani 1 2 d S T P . .
Cl4 Cl 0.5365(2) 1.250000 0.91200(19) 0.0351(9) Uani 1 2 d S T P . .
S1 S 0.7101(2) 0.250000 0.42318(18) 0.0221(9) Uani 1 2 d S T P . .
S2 S 0.7544(2) 0.750000 0.92027(18) 0.0211(8) Uani 1 2 d S T P . .
C1 C 0.3517(9) 0.250000 0.4472(7) 0.015(3) Uani 1 2 d S T P . .
C2 C 0.4530(9) 0.250000 0.4876(7) 0.020(3) Uani 1 2 d S T P . .
C3 C 0.5238(8) 0.250000 0.4422(6) 0.018(3) Uani 1 2 d S T P . .
H3 H 0.510496 0.250000 0.389249 0.021 Uiso 1 2 calc R U P . .
C4 C 0.6153(8) 0.250000 0.4783(6) 0.013(3) Uani 1 2 d S T P . .
C5 C 0.6397(9) 0.250000 0.5583(6) 0.023(3) Uani 1 2 d S T P . .
H5 H 0.701500 0.250000 0.581066 0.028 Uiso 1 2 calc R U P . .
C6 C 0.5655(9) 0.250000 0.6016(7) 0.025(3) Uani 1 2 d S TU P . .
H6 H 0.578487 0.250000 0.654544 0.030 Uiso 1 2 calc R U P . .
C7 C 0.4728(9) 0.250000 0.5673(6) 0.026(3) Uani 1 2 d S T P . .
H7 H 0.424706 0.250000 0.597089 0.031 Uiso 1 2 calc R U P . .
C8 C 1.1192(8) 0.750000 0.9425(6) 0.008(3) Uani 1 2 d S T P . .
C9 C 1.0321(8) 0.750000 0.9806(6) 0.010(3) Uani 1 2 d S TU P . .
C10 C 0.9450(8) 0.750000 0.9383(6) 0.008(3) Uani 1 2 d S TU P . .
H10 H 0.938302 0.750000 0.885251 0.009 Uiso 1 2 calc R U P . .
C11 C 0.8700(8) 0.750000 0.9752(6) 0.011(3) Uani 1 2 d S TU P . .
C12 C 0.8764(8) 0.750000 1.0535(6) 0.012(3) Uani 1 2 d S T P . .
H12 H 0.823114 0.750000 1.077438 0.014 Uiso 1 2 calc R U P . .
C13 C 0.9615(9) 0.750000 1.0945(6) 0.019(3) Uani 1 2 d S TU P . .
H13 H 0.967291 0.750000 1.147557 0.022 Uiso 1 2 calc R U P . .
C14 C 1.0414(8) 0.750000 1.0586(6) 0.016(3) Uani 1 2 d S T P . .
H14 H 1.100208 0.750000 1.087304 0.019 Uiso 1 2 calc R U P . .
N1 N -0.0012(4) 0.4554(8) 0.2666(3) 0.0251(19) Uani 1 1 d . . . . .
H1A H -0.034964 0.400863 0.226287 0.030 Uiso 1 1 calc R U . . .
H1B H 0.040858 0.534857 0.250864 0.030 Uiso 1 1 calc R U . . .
H1C H -0.038322 0.522901 0.292949 0.030 Uiso 1 1 calc R U . . .
N2 N -0.0367(6) 0.250000 0.3978(4) 0.024(3) Uani 1 2 d S T P . .
H2B H -0.084278 0.321611 0.376060 0.029 Uiso 0.5 1 d R U P A -1
H2C H -0.014976 0.299865 0.443164 0.029 Uiso 0.5 1 d R U P A -1
H2A H -0.055830 0.128524 0.403605 0.029 Uiso 0.5 1 d R U P A -1
N3 N 0.1294(4) 0.4523(8) 0.3965(3) 0.0210(18) Uani 1 1 d . . . . .
H3C H 0.162637 0.524841 0.368399 0.025 Uiso 1 1 calc R U . . .
H3A H 0.167282 0.396922 0.434236 0.025 Uiso 1 1 calc R U . . .
H3B H 0.088349 0.527163 0.415854 0.025 Uiso 1 1 calc R U . . .
N4 N 0.1675(6) 0.250000 0.2729(4) 0.020(3) Uani 1 2 d S T P . .
H4A H 0.220672 0.235422 0.304082 0.025 Uiso 0.5 1 calc R U P B -1
H4B H 0.168480 0.362294 0.247926 0.025 Uiso 0.5 1 calc R U P B -1
H4C H 0.160693 0.152284 0.239548 0.025 Uiso 0.5 1 calc R U P B -1
N5 N 0.4256(4) 0.9534(8) 0.7742(3) 0.031(2) Uani 1 1 d . . . . .
H5A H 0.397029 0.942105 0.726575 0.037 Uiso 1 1 calc R U . . .
H5B H 0.486724 0.938957 0.774790 0.037 Uiso 1 1 calc R U . . .
H5C H 0.414000 1.070409 0.792328 0.037 Uiso 1 1 calc R U . . .
N6 N 0.2549(6) 0.750000 0.7752(5) 0.030(3) Uani 1 2 d S T P . .
H6C H 0.213882 0.689310 0.800043 0.036 Uiso 0.5 1 calc R U P C -1
H6B H 0.258707 0.688568 0.731430 0.036 Uiso 0.5 1 calc R U P C -1
H6A H 0.236430 0.872122 0.765528 0.036 Uiso 0.5 1 calc R U P C -1
N7 N 0.3329(4) 0.9556(8) 0.9004(3) 0.031(2) Uani 1 1 d . . . . .
H7B H 0.302289 1.044057 0.869869 0.037 Uiso 1 1 calc R U . . .
H7C H 0.380782 1.012040 0.929101 0.037 Uiso 1 1 calc R U . . .
H7A H 0.294671 0.904375 0.930388 0.037 Uiso 1 1 calc R U . . .
N8 N 0.4983(7) 0.750000 0.9059(5) 0.038(3) Uani 1 2 d S T P . .
H8B H 0.492246 0.686398 0.948728 0.045 Uiso 0.5 1 calc R U P D -1
H8A H 0.515730 0.872087 0.916952 0.045 Uiso 0.5 1 calc R U P D -1
H8C H 0.541268 0.691515 0.882396 0.045 Uiso 0.5 1 calc R U P D -1
O1 O 0.3372(6) 0.250000 0.3767(4) 0.030(2) Uani 1 2 d S TU P . .
O2 O 0.2885(6) 0.250000 0.4892(4) 0.025(2) Uani 1 2 d S T P . .
O3 O 0.6994(4) 0.4233(7) 0.3763(3) 0.0264(16) Uani 1 1 d . . . . .
O4 O 0.7963(6) 0.250000 0.4777(4) 0.029(2) Uani 1 2 d S T P . .
O5 O 0.6879(6) 0.750000 0.9740(4) 0.043(3) Uani 1 2 d S T P . .
O6 O 0.7502(4) 0.9232(7) 0.8733(3) 0.0302(17) Uani 1 1 d . . . . .
O7 O 1.1969(6) 0.750000 0.9820(4) 0.021(2) Uani 1 2 d S T P . .
O8 O 1.1082(5) 0.750000 0.8700(4) 0.022(2) Uani 1 2 d S T P . .
O9 O 0.4037(15) 0.250000 0.2483(10) 0.083(5) Uiso 0.624(14) 2 d S U P E 4
O10 O 0.4021(17) 0.391(3) 0.2521(12) 0.083(5) Uiso 0.376(14) 1 d . U P E 3
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'
Na Na 0.0362 0.0249 '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
N4 Co1 N3 87.6(3) . . ?
N4 Co1 N3 87.6(3) . 4_565 ?
N3 Co1 N3 90.4(4) . 4_565 ?
N4 Co1 N2 176.7(4) . . ?
N3 Co1 N2 90.0(3) . . ?
N3 Co1 N2 90.0(3) 4_565 . ?
N4 Co1 N1 91.2(3) . 4_565 ?
N3 Co1 N1 178.8(3) . 4_565 ?
N3 Co1 N1 89.3(2) 4_565 4_565 ?
N2 Co1 N1 91.2(3) . 4_565 ?
N4 Co1 N1 91.2(3) . . ?
N3 Co1 N1 89.3(2) . . ?
N3 Co1 N1 178.8(3) 4_565 . ?
N2 Co1 N1 91.2(3) . . ?
N1 Co1 N1 91.0(3) 4_565 . ?
N7 Co2 N7 92.4(4) . 4_575 ?
N7 Co2 N8 90.1(3) . . ?
N7 Co2 N8 90.1(3) 4_575 . ?
N7 Co2 N5 178.5(3) . 4_575 ?
N7 Co2 N5 88.9(3) 4_575 4_575 ?
N8 Co2 N5 90.3(3) . 4_575 ?
N7 Co2 N5 88.9(3) . . ?
N7 Co2 N5 178.5(3) 4_575 . ?
N8 Co2 N5 90.3(3) . . ?
N5 Co2 N5 89.7(4) 4_575 . ?
N7 Co2 N6 88.0(3) . . ?
N7 Co2 N6 88.0(3) 4_575 . ?
N8 Co2 N6 177.3(4) . . ?
N5 Co2 N6 91.6(3) 4_575 . ?
N5 Co2 N6 91.6(3) . . ?
O2 Na1 O3 88.26(17) . 3_666 ?
O2 Na1 O3 88.26(17) . 2_646 ?
O3 Na1 O3 138.2(3) 3_666 2_646 ?
O2 Na1 Cl1 104.5(3) . . ?
O3 Na1 Cl1 110.57(16) 3_666 . ?
O3 Na1 Cl1 110.57(16) 2_646 . ?
O2 Na1 Cl2 167.5(3) . . ?
O3 Na1 Cl2 87.28(15) 3_666 . ?
O3 Na1 Cl2 87.28(15) 2_646 . ?
Cl1 Na1 Cl2 88.09(16) . . ?
O6 Na2 O6 155.2(4) 4_585 . ?
O6 Na2 O7 92.40(17) 4_585 3_777 ?
O6 Na2 O7 92.40(17) . 3_777 ?
O6 Na2 Cl4 101.41(19) 4_585 . ?
O6 Na2 Cl4 101.41(19) . . ?
O7 Na2 Cl4 101.5(2) 3_777 . ?
O6 Na2 Cl3 78.65(17) 4_585 . ?
O6 Na2 Cl3 78.65(17) . . ?
O7 Na2 Cl3 124.7(3) 3_777 . ?
Cl4 Na2 Cl3 133.73(18) . . ?
O3 S1 O3 110.7(5) 4_565 . ?
O3 S1 O4 113.0(3) 4_565 . ?
O3 S1 O4 113.0(3) . . ?
O3 S1 C4 106.4(3) 4_565 . ?
O3 S1 C4 106.4(3) . . ?
O4 S1 C4 106.8(5) . . ?
O5 S2 O6 113.5(3) . 4_575 ?
O5 S2 O6 113.5(3) . . ?
O6 S2 O6 110.6(5) 4_575 . ?
O5 S2 C11 107.3(5) . . ?
O6 S2 C11 105.6(3) 4_575 . ?
O6 S2 C11 105.6(3) . . ?
O1 C1 O2 124.1(12) . . ?
O1 C1 C2 119.0(12) . . ?
O2 C1 C2 116.8(11) . . ?
C7 C2 C3 121.1(12) . . ?
C7 C2 C1 121.1(12) . . ?
C3 C2 C1 117.7(11) . . ?
C2 C3 C4 118.0(11) . . ?
C3 C4 C5 123.5(11) . . ?
C3 C4 S1 120.3(9) . . ?
C5 C4 S1 116.2(9) . . ?
C4 C5 C6 116.3(12) . . ?
C7 C6 C5 121.8(11) . . ?
C2 C7 C6 119.3(12) . . ?
O7 C8 O8 123.1(11) . . ?
O7 C8 C9 119.8(10) . . ?
O8 C8 C9 117.0(11) . . ?
C10 C9 C14 120.3(11) . . ?
C10 C9 C8 121.1(10) . . ?
C14 C9 C8 118.6(11) . . ?
C11 C10 C9 118.6(11) . . ?
C10 C11 C12 122.8(12) . . ?
C10 C11 S2 119.3(9) . . ?
C12 C11 S2 117.9(9) . . ?
C13 C12 C11 118.3(11) . . ?
C12 C13 C14 120.8(11) . . ?
C9 C14 C13 119.2(11) . . ?
C1 O2 Na1 150.8(8) . . ?
S1 O3 Na1 133.7(4) . 3_666 ?
S2 O6 Na2 137.1(3) . . ?
C8 O7 Na2 144.1(8) . 3_777 ?
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 N4 1.956(8) . ?
Co1 N3 1.960(6) . ?
Co1 N3 1.960(6) 4_565 ?
Co1 N2 1.974(8) . ?
Co1 N1 1.979(6) 4_565 ?
Co1 N1 1.979(6) . ?
Co2 N7 1.957(6) . ?
Co2 N7 1.957(6) 4_575 ?
Co2 N8 1.960(9) . ?
Co2 N5 1.982(5) 4_575 ?
Co2 N5 1.982(6) . ?
Co2 N6 1.984(9) . ?
Na1 O2 2.275(9) . ?
Na1 O3 2.402(5) 3_666 ?
Na1 O3 2.402(5) 2_646 ?
Na1 Cl1 2.707(6) . ?
Na1 Cl2 2.788(5) . ?
Na2 O6 2.299(5) 4_585 ?
Na2 O6 2.299(5) . ?
Na2 O7 2.426(9) 3_777 ?
Na2 Cl4 2.801(6) . ?
Na2 Cl3 3.077(5) . ?
S1 O3 1.448(5) 4_565 ?
S1 O3 1.448(5) . ?
S1 O4 1.470(8) . ?
S1 C4 1.790(11) . ?
S2 O5 1.443(8) . ?
S2 O6 1.447(5) 4_575 ?
S2 O6 1.448(5) . ?
S2 C11 1.817(12) . ?
C1 O1 1.236(12) . ?
C1 O2 1.256(13) . ?
C1 C2 1.542(16) . ?
C2 C7 1.400(13) . ?
C2 C3 1.387(14) . ?
C3 C4 1.390(14) . ?
C4 C5 1.411(14) . ?
C5 C6 1.403(14) . ?
C6 C7 1.396(15) . ?
C8 O7 1.240(12) . ?
C8 O8 1.272(11) . ?
C8 C9 1.510(14) . ?
C9 C10 1.376(14) . ?
C9 C14 1.367(13) . ?
C10 C11 1.342(13) . ?
C11 C12 1.377(13) . ?
C12 C13 1.342(15) . ?
C13 C14 1.395(14) . ?
