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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/7/25/02/7250246.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_7250246
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            'C20 H35 Co N10 O12 S4'
_chemical_formula_weight         794.75
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   geom
_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            8
_cell_length_a                   14.9159(12)
_cell_length_b                   18.4135(9)
_cell_length_c                   22.7514(13)
_cell_measurement_reflns_used    1241
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.1950
_cell_measurement_theta_min      3.7000
_cell_volume                     6248.8(7)
_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_R_equivalents  0.0222
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3991
_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         26.234
_diffrn_reflns_theta_min         3.210
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.893
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80893
_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    1.690
_exptl_crystal_description       block
_exptl_crystal_F_000             3296
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         1576
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0372
_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)+(0.0597P)²+4.8169P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1049
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1257
_reflns_number_total             1576
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5ce00184f2.cif
_cod_data_source_block           compound1_V_5396_NE67_n
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               7250246
_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   0.664
_shelx_estimated_absorpt_t_max   0.775
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'x, -y+1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'x, -y+3/4, -z+3/4'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'x+1/2, -y+1/4, -z+3/4'
'-x+3/4, y, -z+3/4'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'x+1/2, -y+3/4, -z+1/4'
'-x+3/4, y+1/2, -z+1/4'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'-x, y-1/4, z-1/4'
'x-1/4, -y, z-1/4'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'-x, y+1/4, z+1/4'
'x-1/4, -y+1/2, z+1/4'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'-x+1/2, y-1/4, z+1/4'
'x+1/4, -y, z+1/4'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'-x+1/2, y+1/4, z-1/4'
'x+1/4, -y+1/2, z-1/4'
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 0.125000 0.625000 0.625000 0.0270(2) Uani 1 4 d S T P . .
N1 N 0.21754(14) 0.70035(10) 0.62480(9) 0.0375(5) Uani 1 1 d . . . . .
H1A H 0.269734 0.680970 0.614160 0.056 Uiso 1 1 calc R U . . .
H1B H 0.222496 0.719225 0.660668 0.056 Uiso 1 1 calc R U . . .
H1C H 0.202468 0.735119 0.599489 0.056 Uiso 1 1 calc R U . . .
N2 N 0.125000 0.625000 0.71149(12) 0.0405(7) Uani 1 2 d S T P . .
H2A H 0.169797 0.652565 0.724530 0.061 Uiso 0.5 1 calc R U P . .
H2B H 0.132071 0.579791 0.724530 0.061 Uiso 0.5 1 calc R U P . .
H2C H 0.073132 0.642644 0.724530 0.061 Uiso 0.5 1 calc R U P . .
S1A S 0.6219(5) 0.3368(3) 0.5067(3) 0.0407(13) Uani 0.5 1 d D . P A 1
O1A O 0.7035(8) 0.3238(9) 0.5385(6) 0.053(3) Uani 0.5 1 d D . P A 1
O2A O 0.6366(10) 0.3646(10) 0.4480(5) 0.052(3) Uani 0.5 1 d D . P A 1
O3A O 0.5630(8) 0.2725(4) 0.5070(5) 0.052(2) Uani 0.5 1 d D . P A 1
C1 C 0.5597(4) 0.4042(3) 0.5450(4) 0.0294(12) Uani 0.5 1 d D . P A 1
C2 C 0.4812(4) 0.3881(3) 0.5747(3) 0.0446(14) Uani 0.5 1 d D . P A 1
H2 H 0.459434 0.340749 0.573598 0.053 Uiso 0.5 1 calc R U P A 1
N3A N 0.4352(4) 0.4386(3) 0.6051(3) 0.0605(14) Uani 0.5 1 d D . P A 1
C3 C 0.4691(8) 0.5068(5) 0.6057(7) 0.0505(19) Uani 0.5 1 d D . P A 1
H3 H 0.440211 0.542168 0.627911 0.061 Uiso 0.5 1 calc R U P A 1
C4 C 0.5430(5) 0.5251(3) 0.5754(3) 0.0460(17) Uani 0.5 1 d D . P A 1
H4 H 0.562783 0.573052 0.575910 0.055 Uiso 0.5 1 calc R U P A 1
C5 C 0.5890(5) 0.4752(4) 0.5444(4) 0.0367(12) Uani 0.5 1 d D . P A 1
H5 H 0.639522 0.488394 0.522941 0.044 Uiso 0.5 1 calc R U P A 1
S1B S 0.6321(5) 0.3498(4) 0.5144(3) 0.0333(8) Uani 0.5 1 d D . P B 2
O1B O 0.7083(10) 0.3331(10) 0.5521(7) 0.062(4) Uani 0.5 1 d D . P B 2
O2B O 0.6596(10) 0.3730(10) 0.4562(5) 0.044(3) Uani 0.5 1 d D . P B 2
O3B O 0.5656(8) 0.2947(4) 0.5152(6) 0.060(2) Uani 0.5 1 d D . P B 2
C6 C 0.5847(5) 0.4288(3) 0.5474(4) 0.0294(12) Uani 0.5 1 d D . P B 2
C10 C 0.6199(5) 0.4963(4) 0.5368(4) 0.0367(12) Uani 0.5 1 d D . P B 2
H10 H 0.668505 0.501468 0.511550 0.044 Uiso 0.5 1 calc R U P B 2
N3B N 0.5844(4) 0.5547(3) 0.5628(2) 0.0476(13) Uani 0.5 1 d D . P B 2
H3B H 0.605636 0.597246 0.555662 0.057 Uiso 0.25 1 calc R U P B 2
C9 C 0.5172(5) 0.5470(3) 0.5993(3) 0.0504(18) Uani 0.5 1 d D . P B 2
H9 H 0.494035 0.588127 0.617422 0.061 Uiso 0.5 1 calc R U P B 2
C8 C 0.4801(8) 0.4821(4) 0.6116(7) 0.0505(19) Uani 0.5 1 d D . P B 2
H8 H 0.432221 0.478542 0.637656 0.061 Uiso 0.5 1 calc R U P B 2
C7 C 0.5144(4) 0.4212(3) 0.5850(3) 0.0390(13) Uani 0.5 1 d D . P B 2
H7 H 0.490137 0.375653 0.592613 0.047 Uiso 0.5 1 calc R U P B 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'
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'
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
N1 Co1 N1 90.30(12) 2_565 4_556 ?
N1 Co1 N1 89.70(12) 2_565 3_566 ?
N1 Co1 N1 179.74(12) 4_556 3_566 ?
N1 Co1 N1 179.74(12) 2_565 . ?
N1 Co1 N1 89.70(12) 4_556 . ?
N1 Co1 N1 90.30(12) 3_566 . ?
N1 Co1 N2 89.87(6) 2_565 3_566 ?
N1 Co1 N2 90.13(6) 4_556 3_566 ?
N1 Co1 N2 90.13(6) 3_566 3_566 ?
N1 Co1 N2 89.87(6) . 3_566 ?
N1 Co1 N2 90.13(6) 2_565 . ?
N1 Co1 N2 89.87(6) 4_556 . ?
N1 Co1 N2 89.87(6) 3_566 . ?
N1 Co1 N2 90.13(6) . . ?
N2 Co1 N2 180.0 3_566 . ?
O1A S1A O2A 113.3(9) . . ?
O1A S1A O3A 111.6(9) . . ?
O2A S1A O3A 112.4(8) . . ?
O1A S1A C1 108.1(7) . . ?
O2A S1A C1 106.6(9) . . ?
O3A S1A C1 104.3(6) . . ?
C5 C1 C2 118.5(6) . . ?
C5 C1 S1A 119.4(6) . . ?
C2 C1 S1A 122.1(5) . . ?
N3A C2 C1 122.2(6) . . ?
C2 N3A C3 117.1(7) . . ?
C4 C3 N3A 122.3(9) . . ?
C3 C4 C5 121.0(7) . . ?
C4 C5 C1 118.7(7) . . ?
O3B S1B O2B 114.9(8) . . ?
O3B S1B O1B 112.8(10) . . ?
O2B S1B O1B 112.3(10) . . ?
O3B S1B C6 107.5(6) . . ?
O2B S1B C6 104.8(8) . . ?
O1B S1B C6 103.5(7) . . ?
C7 C6 C10 119.9(6) . . ?
C7 C6 S1B 119.1(5) . . ?
C10 C6 S1B 121.0(6) . . ?
N3B C10 C6 120.0(6) . . ?
C9 N3B C10 119.7(6) . . ?
N3B C9 C8 123.0(8) . . ?
C9 C8 C7 118.6(9) . . ?
C6 C7 C8 118.8(7) . . ?
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 N1 1.9571(19) 2_565 ?
Co1 N1 1.9571(19) 4_556 ?
Co1 N1 1.9571(19) 3_566 ?
Co1 N1 1.9571(19) . ?
Co1 N2 1.968(3) 3_566 ?
Co1 N2 1.968(3) . ?
S1A O1A 1.437(9) . ?
S1A O2A 1.445(9) . ?
S1A O3A 1.475(8) . ?
S1A C1 1.778(8) . ?
C1 C5 1.379(6) . ?
C1 C2 1.384(8) . ?
C2 N3A 1.348(7) . ?
N3A C3 1.353(11) . ?
C3 C4 1.344(11) . ?
C4 C5 1.347(10) . ?
S1B O3B 1.418(8) . ?
S1B O2B 1.451(9) . ?
S1B O1B 1.457(9) . ?
S1B C6 1.784(7) . ?
C6 C7 1.361(8) . ?
C6 C10 1.370(6) . ?
C10 N3B 1.338(8) . ?
N3B C9 1.308(9) . ?
C9 C8 1.347(10) . ?
C8 C7 1.372(11) . ?
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 O2A^a 0.89 2.16 2.985(17) 154.2 17_666 yes
N1 H1A O2B^b 0.89 2.16 2.929(16) 144.5 17_666 yes
N1 H1B O3A^a 0.89 2.18 3.033(12) 160.6 16_556 yes
N1 H1B O3B^b 0.89 2.26 3.086(13) 154.7 16_556 yes
N1 H1C O1A^a 0.89 2.14 3.012(16) 164.9 13_455 yes
N1 H1C O1B^b 0.89 2.10 2.955(19) 159.7 13_455 yes
N2 H2A O3A^a 0.89 2.26 2.957(9) 134.7 16_556 yes
N2 H2A O2B^b 0.89 2.64 3.216(15) 123.7 23_655 yes
N2 H2A O3B^b 0.89 2.64 3.291(10) 131.1 16_556 yes
N2 H2B O3A^a 0.89 2.19 2.957(9) 144.4 15_456 yes
N2 H2B O3B^b 0.89 2.51 3.291(10) 147.0 15_456 yes
N2 H2C O1A^a 0.89 2.38 3.240(17) 161.6 28_465 yes
N2 H2C S1B^b 0.89 2.99 3.846(8) 161.0 28_465 yes
N2 H2C O1B^b 0.89 2.50 3.32(2) 153.7 28_465 yes
N2 H2C O2B^b 0.89 2.49 3.216(15) 138.8 28_465 yes
C2^a H2^a N3A^a 0.93 2.34 2.938(9) 122.1 14 yes
N3B^b H3B^b N3B^b 0.86 2.02 2.857(11) 163.8 2_665 yes
