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#$Date: 2025-04-09 01:47:09 +0300 (Wed, 09 Apr 2025) $
#$Revision: 299221 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/25/02/7250250.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_7250250
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_moiety         'C7 H24 Cl Co N6 O9 S'
_chemical_formula_sum            'C7 H24 Cl Co N6 O9 S'
_chemical_formula_weight         462.76
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.0699(10)
_cell_length_b                   7.2512(4)
_cell_length_c                   10.8265(6)
_cell_measurement_reflns_used    1379
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.3030
_cell_measurement_theta_min      3.7330
_cell_volume                     1968.12(17)
_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 0.995
_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_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4450
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         3.079
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.164
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90399
_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            orange
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_description       Block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         1978
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0485
_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)+(0.1100P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1559
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1643
_reflns_number_total             1978
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5ce00184f2.cif
_cod_data_source_block           V_5528_NE127
_cod_database_code               7250250
_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.
;
_shelx_estimated_absorpt_t_min   0.594
_shelx_estimated_absorpt_t_max   0.760
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'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
S1 S 0.65506(5) 0.750000 0.90909(11) 0.0367(3) Uani 1 2 d S T P . .
O1 O 0.67730(10) 0.5849(4) 0.9641(2) 0.0504(7) Uani 1 1 d . . . . .
O2 O 0.66042(15) 0.750000 0.7757(3) 0.0513(10) Uani 1 2 d S T P . .
O3 O 0.45033(16) 0.750000 1.2486(4) 0.0706(13) Uani 1 2 d S T P . .
O4 O 0.53497(18) 0.750000 1.3075(4) 0.0952(19) Uani 1 2 d S T P . .
C1 C 0.58566(19) 0.750000 0.9414(4) 0.0377(11) Uani 1 2 d S T P . .
C2 C 0.5489(2) 0.750000 0.8479(5) 0.0564(16) Uani 1 2 d S T P . .
H7 H 0.559672 0.750000 0.765665 0.068 Uiso 1 2 calc R U P . .
C3 C 0.4953(2) 0.750000 0.8789(5) 0.073(2) Uani 1 2 d S T P . .
H8 H 0.469796 0.750000 0.816524 0.087 Uiso 1 2 calc R U P . .
C4 C 0.4792(2) 0.750000 0.9990(5) 0.0641(18) Uani 1 2 d S T P . .
H9 H 0.443011 0.750000 1.017923 0.077 Uiso 1 2 calc R U P . .
C5 C 0.51698(19) 0.750000 1.0939(5) 0.0511(14) Uani 1 2 d S T P . .
C6 C 0.5706(2) 0.750000 1.0630(5) 0.0458(12) Uani 1 2 d S T P . .
H10 H 0.596327 0.750000 1.124851 0.055 Uiso 1 2 calc R U P . .
C7 C 0.4994(2) 0.750000 1.2260(5) 0.0654(18) Uani 1 2 d S T P . .
Co1 Co 0.31748(2) 0.750000 0.36718(5) 0.0310(3) Uani 1 2 d S T P . .
N1 N 0.33855(17) 0.750000 0.1940(4) 0.0390(9) Uani 1 2 d S T P . .
H1A H 0.336013 0.863840 0.163850 0.047 Uiso 0.5 1 d R U P A -1
H1B H 0.317273 0.675070 0.151460 0.047 Uiso 0.5 1 d R U P A -1
H1C H 0.372113 0.711090 0.187710 0.047 Uiso 0.5 1 d R U P A -1
N2 N 0.29705(17) 0.750000 0.5438(4) 0.0441(10) Uani 1 2 d S T P . .
H2A H 0.294787 0.865690 0.570710 0.053 Uiso 0.5 1 d R U P B -1
H2B H 0.321687 0.689840 0.587120 0.053 Uiso 0.5 1 d R U P B -1
H2C H 0.265636 0.694480 0.552940 0.053 Uiso 0.5 1 d R U P B -1
N3 N 0.26331(11) 0.5617(4) 0.3323(3) 0.0404(7) Uani 1 1 d . . . . .
H3A H 0.247863 0.585457 0.260044 0.049 Uiso 1 1 d R U . . .
H3B H 0.238783 0.562828 0.391755 0.049 Uiso 1 1 d R U . . .
H3C H 0.278733 0.451219 0.329505 0.049 Uiso 1 1 d R U . . .
N4 N 0.37082(12) 0.5600(4) 0.3990(3) 0.0475(8) Uani 1 1 d . . . . .
H4A H 0.402310 0.597208 0.370370 0.057 Uiso 1 1 d R U . . .
H4B H 0.361360 0.456018 0.361158 0.057 Uiso 1 1 d R U . . .
H4C H 0.373160 0.540117 0.479910 0.057 Uiso 1 1 d R U . . .
Cl1 Cl 0.71394(6) 0.750000 0.43492(12) 0.0503(4) Uani 1 2 d S T P . .
O5 O 0.3385(3) 0.750000 0.8329(8) 0.157(3) Uani 1 2 d S TU P . .
H5W H 0.353223 0.661703 0.798081 0.236 Uiso 1 1 d R U . . .
O6 O 0.3803(3) 0.4787(10) 0.6780(8) 0.109(2) Uiso 0.564 1 d . . P C 1
O8 O 0.4979(5) 0.6785(17) 0.5412(10) 0.125(4) Uiso 0.436 1 d . . P D 1
O7 O 0.4149(4) 0.5909(13) 0.6433(8) 0.088(3) Uiso 0.404(7) 1 d . . P E 2
O9 O 0.5201(11) 0.750000 0.551(2) 0.058(8) Uiso 0.191(13) 2 d S . P E 2
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'
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'
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'
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
O1 S1 O1 111.5(2) 8_575 . ?
O1 S1 O2 111.93(14) 8_575 . ?
O1 S1 O2 111.93(14) . . ?
O1 S1 C1 107.24(14) 8_575 . ?
O1 S1 C1 107.24(14) . . ?
O2 S1 C1 106.7(2) . . ?
C2 C1 C6 121.7(5) . . ?
C2 C1 S1 120.9(4) . . ?
C6 C1 S1 117.4(4) . . ?
C1 C2 C3 118.3(5) . . ?
C4 C3 C2 121.3(5) . . ?
C3 C4 C5 120.1(5) . . ?
C6 C5 C4 118.7(5) . . ?
C6 C5 C7 121.2(5) . . ?
C4 C5 C7 120.2(5) . . ?
C1 C6 C5 120.0(5) . . ?
O3 C7 O4 124.1(5) . . ?
O3 C7 C5 118.4(5) . . ?
O4 C7 C5 117.5(5) . . ?
N1 Co1 N4 89.08(13) . . ?
N1 Co1 N4 89.08(13) . 8_575 ?
N4 Co1 N4 89.88(19) . 8_575 ?
N1 Co1 N3 90.15(12) . . ?
N4 Co1 N3 90.96(13) . . ?
N4 Co1 N3 178.85(13) 8_575 . ?
N1 Co1 N3 90.15(12) . 8_575 ?
N4 Co1 N3 178.85(12) . 8_575 ?
N4 Co1 N3 90.96(13) 8_575 8_575 ?
N3 Co1 N3 88.19(17) . 8_575 ?
N1 Co1 N2 179.26(17) . . ?
N4 Co1 N2 90.40(13) . . ?
N4 Co1 N2 90.40(13) 8_575 . ?
N3 Co1 N2 90.38(13) . . ?
N3 Co1 N2 90.38(13) 8_575 . ?
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
S1 O1 1.449(3) 8_575 ?
S1 O1 1.449(3) . ?
S1 O2 1.451(4) . ?
S1 C1 1.775(5) . ?
O3 C7 1.253(7) . ?
O4 C7 1.255(7) . ?
C1 C2 1.368(7) . ?
C1 C6 1.371(7) . ?
C2 C3 1.386(8) . ?
C3 C4 1.361(8) . ?
C4 C5 1.398(7) . ?
C5 C6 1.385(7) . ?
C5 C7 1.497(7) . ?
Co1 N1 1.948(4) . ?
Co1 N4 1.951(3) . ?
Co1 N4 1.951(3) 8_575 ?
Co1 N3 1.962(3) . ?
Co1 N3 1.962(3) 8_575 ?
Co1 N2 1.979(4) . ?
O8 O8 1.04(2) 8_575 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1A^a S1 0.89 2.92 3.7969(12) 169.7 5_676 yes
N1 H1A^a O1 0.89 2.14 2.997(4) 160.3 4_656 yes
N1 H1B^a O1 0.89 2.27 2.997(4) 139.2 5_666 yes
N1 H1B^a Cl1 0.89 2.81 3.422(4) 127.4 6_556 yes
N1 H1C^a O3 0.89 2.09 2.864(6) 145.2 1_554 yes
N2 H2A^a Cl1 0.89 2.80 3.6434(5) 159.6 5_676 yes
N2 H2C^a S1 0.89 2.83 3.596(4) 144.9 6_557 yes
N2 H2C^a O1 0.89 2.36 3.233(5) 166.9 6_557 yes
N3 H3A Cl1 0.89 2.57 3.430(3) 163.0 6_556 yes
N3 H3B O1 0.89 2.20 3.088(4) 176.3 6_557 yes
N3 H3C O2 0.89 2.40 3.183(4) 147.2 5_666 yes
N3 H3C Cl1 0.89 2.94 3.433(3) 116.3 5_666 yes
N4 H4A O3 0.89 2.10 2.919(5) 152.4 1_554 yes
N4 H4B O2 0.89 2.17 3.040(4) 164.3 5_666 yes
N4 H4C O6^a 0.89 2.20 3.087(9) 177.4 . yes
N4 H4C O7^b 0.89 2.09 2.875(9) 147.0 . yes
O5 H5W O6^a 0.83 1.98 2.790(10) 165.7 . yes
O5 H5W O7^b 0.83 2.34 3.036(11) 142.2 . yes
