#------------------------------------------------------------------------------
#$Date: 2022-03-18 01:36:57 +0200 (Fri, 18 Mar 2022) $
#$Revision: 273758 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/46/7244630.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_7244630
loop_
_publ_author_name
'Fonseca, Daniela'
'Perez, Adres Felipe'
'Cobo Domingo, Justo'
'Zapata Rivera, Jhon Enrique'
'Hurtado Belalcazar, John'
'Macías, Mario A.'
_publ_section_title
;
 Influence of the Lewis basicity hardness of crystallization solvents on
 the coordination sphere of the complex
 [Co(3,5-dinitrobenzoate-O,O’)2]: Crystallographic and Theoretical
 Analysis
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00177B
_journal_year                    2022
_chemical_formula_sum            'C18 H22 Co N4 O16 S2'
_chemical_formula_weight         673.44
_chemical_name_systematic
diaquabis(3,5-dinitrobenzoato)-bis[(methanesulfinyl)methane]-cobalt(II)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-01-21 deposited with the CCDC.	2022-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.788(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.3871(9)
_cell_length_b                   5.2909(4)
_cell_length_c                   22.6353(17)
_cell_measurement_reflns_used    9391
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.18
_cell_volume                     1243.36(17)
_computing.cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing.data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            20489
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.498
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.184
_diffrn_source
'INCOATEC high brilliance microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.948
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6699
_exptl.absorpt_correction_type   Multi--Scan
_exptl.absorpt_process_details
'SADABS--2016/2 -- Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_description       flake
_exptl_crystal_F_000             690
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DMSO'
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         2845
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0242P)²+0.9346P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0659
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2536
_reflns_number_total             2845
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ce00177b2.cif
_cod_data_source_block           190523_DFC5
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7244630
_shelx_shelxl_version_number     2018/3
_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   0.871
_shelx_estimated_absorpt_t_max   0.945
_computing_bruker_data_scaling
'SADABS--2016/2 -- Bruker AXS area detector scaling and absorption correction'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.500000 1.000000 0.500000 0.00865(8) Uani 1 2 d S . P . .
S2 S 0.22848(4) 1.21646(7) 0.55215(2) 0.01153(9) Uani 1 1 d . . . . .
O1 O 0.53112(11) 0.7937(2) 0.57759(5) 0.0142(2) Uani 1 1 d . . . . .
O11 O 0.65896(11) 1.0547(2) 0.63158(5) 0.0159(2) Uani 1 1 d . . . . .
O13 O 0.31706(11) 0.0985(2) 0.67695(5) 0.0159(2) Uani 1 1 d . . . . .
O14 O 0.33985(11) 0.0513(2) 0.77191(5) 0.0159(2) Uani 1 1 d . . . . .
O16 O 0.65783(12) 0.9916(2) 0.84468(5) 0.0196(3) Uani 1 1 d . . . . .
O15 O 0.56308(11) 0.6801(2) 0.88782(5) 0.0172(2) Uani 1 1 d . . . . .
O2 O 0.36968(11) 1.2525(2) 0.53807(5) 0.0156(2) Uani 1 1 d . . . . .
O3 O 0.35638(10) 0.7366(2) 0.47391(5) 0.0134(2) Uani 1 1 d . . . . .
H3A H 0.342843 0.766954 0.438257 0.020 Uiso 1 1 d R U . . .
H3B H 0.384020 0.594221 0.477928 0.020 Uiso 1 1 d R U . . .
C1 C 0.58757(14) 0.8660(3) 0.62499(7) 0.0108(3) Uani 1 1 d . . . . .
C11 C 0.56057(14) 0.7132(3) 0.67997(7) 0.0113(3) Uani 1 1 d . . . . .
C16 C 0.60459(14) 0.8018(3) 0.73477(7) 0.0116(3) Uani 1 1 d . . . . .
H16 H 0.659927 0.944532 0.737498 0.014 Uiso 1 1 calc R U . . .
C15 C 0.56643(15) 0.6784(3) 0.78552(6) 0.0118(3) Uani 1 1 d . . . . .
C14 C 0.48799(14) 0.4676(3) 0.78393(7) 0.0120(3) Uani 1 1 d . . . . .
H14 H 0.462345 0.385852 0.819033 0.014 Uiso 1 1 calc R U . . .
C13 C 0.44870(14) 0.3817(3) 0.72848(7) 0.0110(3) Uani 1 1 d . . . . .
N13 N 0.36213(12) 0.1620(3) 0.72550(6) 0.0118(3) Uani 1 1 d . . . . .
C12 C 0.48306(14) 0.4988(3) 0.67633(7) 0.0111(3) Uani 1 1 d . . . . .
H12 H 0.454315 0.434057 0.639060 0.013 Uiso 1 1 calc R U . . .
N15 N 0.59972(13) 0.7908(3) 0.84348(6) 0.0133(3) Uani 1 1 d . . . . .
C21 C 0.14040(16) 1.2473(3) 0.48347(7) 0.0181(3) Uani 1 1 d . . . . .
H21A H 0.160211 1.410691 0.465496 0.027 Uiso 1 1 calc R U . . .
H21B H 0.047886 1.237451 0.490430 0.027 Uiso 1 1 calc R U . . .
H21C H 0.164781 1.110684 0.456807 0.027 Uiso 1 1 calc R U . . .
C22 C 0.18552(16) 1.5133(3) 0.58383(7) 0.0146(3) Uani 1 1 d . . . . .
H22A H 0.223377 1.526010 0.623919 0.022 Uiso 1 1 calc R U . . .
H22B H 0.091546 1.525509 0.585393 0.022 Uiso 1 1 calc R U . . .
H22C H 0.218111 1.651138 0.559522 0.022 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
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'
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 Co1 O1 180.00(5) . 3_676 ?
O1 Co1 O2 94.14(5) . . ?
O1 Co1 O2 85.86(5) 3_676 . ?
O1 Co1 O2 85.86(5) . 3_676 ?
O1 Co1 O2 94.14(5) 3_676 3_676 ?
O2 Co1 O2 180.0 . 3_676 ?
O1 Co1 O3 91.16(4) . 3_676 ?
O1 Co1 O3 88.84(4) 3_676 3_676 ?
O2 Co1 O3 85.67(4) . 3_676 ?
O2 Co1 O3 94.33(4) 3_676 3_676 ?
O1 Co1 O3 88.84(4) . . ?
O1 Co1 O3 91.17(4) 3_676 . ?
O2 Co1 O3 94.33(4) . . ?
O2 Co1 O3 85.67(4) 3_676 . ?
O3 Co1 O3 180.0 3_676 . ?
O2 S2 C21 106.08(8) . . ?
O2 S2 C22 103.17(7) . . ?
C21 S2 C22 98.12(8) . . ?
C1 O1 Co1 127.70(10) . . ?
S2 O2 Co1 129.95(7) . . ?
Co1 O3 H3A 103.9 . . ?
Co1 O3 H3B 109.7 . . ?
H3A O3 H3B 109.7 . . ?
O11 C1 O1 126.86(14) . . ?
O11 C1 C11 116.87(13) . . ?
O1 C1 C11 116.21(14) . . ?
C16 C11 C12 120.08(14) . . ?
C16 C11 C1 119.22(14) . . ?
C12 C11 C1 120.46(14) . . ?
C15 C16 C11 119.00(15) . . ?
C15 C16 H16 120.5 . . ?
C11 C16 H16 120.5 . . ?
C14 C15 C16 122.76(14) . . ?
C14 C15 N15 118.14(14) . . ?
C16 C15 N15 118.80(14) . . ?
C15 C14 C13 116.46(14) . . ?
C15 C14 H14 121.8 . . ?
C13 C14 H14 121.8 . . ?
C14 C13 C12 123.21(15) . . ?
C14 C13 N13 117.63(14) . . ?
C12 C13 N13 119.11(13) . . ?
O13 N13 O14 123.86(14) . . ?
O13 N13 C13 118.23(13) . . ?
O14 N13 C13 117.91(13) . . ?
C13 C12 C11 118.45(14) . . ?
C13 C12 H12 120.8 . . ?
C11 C12 H12 120.8 . . ?
O16 N15 O15 124.04(14) . . ?
O16 N15 C15 118.26(13) . . ?
O15 N15 C15 117.65(14) . . ?
S2 C21 H21A 109.5 . . ?
S2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
S2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
S2 C22 H22A 109.5 . . ?
S2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
S2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
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 O1 2.0845(11) . ?
Co1 O1 2.0845(11) 3_676 ?
Co1 O2 2.1053(11) . ?
Co1 O2 2.1053(11) 3_676 ?
Co1 O3 2.1121(11) 3_676 ?
Co1 O3 2.1121(11) . ?
S2 O2 1.5226(12) . ?
S2 C21 1.7865(16) . ?
S2 C22 1.7890(17) . ?
O1 C1 1.2658(19) . ?
O11 C1 1.250(2) . ?
O13 N13 1.2278(17) . ?
O14 N13 1.2309(17) . ?
O16 N15 1.2220(19) . ?
O15 N15 1.2325(18) . ?
O3 H3A 0.8305 . ?
O3 H3B 0.8104 . ?
C1 C11 1.517(2) . ?
C11 C16 1.390(2) . ?
C11 C12 1.392(2) . ?
C16 C15 1.390(2) . ?
C16 H16 0.9500 . ?
C15 C14 1.381(2) . ?
C15 N15 1.4718(19) . ?
C14 C13 1.384(2) . ?
C14 H14 0.9500 . ?
C13 C12 1.390(2) . ?
C13 N13 1.470(2) . ?
C12 H12 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
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
O3 H3A O11 0.83 1.84 2.6310(16) 158.5 3_676 yes
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C21 S2 O2 Co1 -77.63(11) . . . . ?
C22 S2 O2 Co1 179.75(9) . . . . ?
Co1 O1 C1 O11 -15.9(2) . . . . ?
Co1 O1 C1 C11 161.22(10) . . . . ?
O11 C1 C11 C16 6.3(2) . . . . ?
O1 C1 C11 C16 -171.10(14) . . . . ?
O11 C1 C11 C12 -179.35(14) . . . . ?
O1 C1 C11 C12 3.3(2) . . . . ?
C12 C11 C16 C15 -2.2(2) . . . . ?
C1 C11 C16 C15 172.21(14) . . . . ?
C11 C16 C15 C14 1.2(2) . . . . ?
C11 C16 C15 N15 -172.45(13) . . . . ?
C16 C15 C14 C13 0.4(2) . . . . ?
N15 C15 C14 C13 173.99(13) . . . . ?
C15 C14 C13 C12 -0.9(2) . . . . ?
C15 C14 C13 N13 -178.30(13) . . . . ?
C14 C13 N13 O13 173.33(14) . . . . ?
C12 C13 N13 O13 -4.2(2) . . . . ?
C14 C13 N13 O14 -7.2(2) . . . . ?
C12 C13 N13 O14 175.30(14) . . . . ?
C14 C13 C12 C11 -0.1(2) . . . . ?
N13 C13 C12 C11 177.26(13) . . . . ?
C16 C11 C12 C13 1.7(2) . . . . ?
C1 C11 C12 C13 -172.63(14) . . . . ?
C14 C15 N15 O16 -172.57(14) . . . . ?
C16 C15 N15 O16 1.3(2) . . . . ?
C14 C15 N15 O15 5.0(2) . . . . ?
C16 C15 N15 O15 178.86(14) . . . . ?
