Design, synthesis, and structural evaluation of metal complexes of azepane-1-carbodithioate for targeting human breast cancer: investigating cytotoxic activity against the MDA-MB-231 cell line
Jaiswal, Shubham; Rai, Nilesh; Chandra, Suryansh; Verma, Ashish; Gautam, Vibhav; Adhikari, Manu; Singh, Sanjay; Bharty, M. K.; New Journal of Chemistry 48 (2024) 13589–13601; doi:10.1039/D4NJ01878H

data_7063313
_publ_section_title
;
 Design, synthesis, and structural evaluation of metal complexes of
 azepane-1-carbodithioate for targeting human breast cancer: investigating
 cytotoxic activity against the MDA-MB-231 cell line
;
_journal_issue                   30
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              13589
_journal_page_last               13601
_journal_paper_doi               10.1039/D4NJ01878H
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C21 H35 Co1 N3 S6, 1[CH2Cl2]'
_chemical_formula_sum            'C22 H37 Cl2 Co N3 S6'
_chemical_formula_weight         665.794
_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'
_symmetry_Int_Tables_number      14
_audit_creation_date             2024-05-21
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2024.05.14 svn.rc2abdb5a for OlexSys, GUI svn.r6697)
;
_audit_update_record
;
2024-06-25 deposited with the CCDC.	2024-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.005(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0012(12)
_cell_length_b                   15.8404(16)
_cell_length_c                   16.6915(16)
_cell_measurement_reflns_used    2599
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      21.8970
_cell_measurement_theta_min      2.8320
_cell_volume                     3172.6(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      290(2)
_diffrn_measured_fraction_theta_full 0.9924
_diffrn_measured_fraction_theta_max 0.9924
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -69.00 118.20   0.30   15.00    --   29.89  54.00  30.00  624
  2  \w    -68.00  50.20   0.30   15.00    --   29.89  54.00  30.00  394
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.9924
_diffrn_reflns_Laue_measured_fraction_max 0.9924
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15246
_diffrn_reflns_point_group_measured_fraction_full 0.9924
_diffrn_reflns_point_group_measured_fraction_max 0.9924
_diffrn_reflns_theta_full        25.0515
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    1.121
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark blue'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1394.063
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.4632
_refine_diff_density_min         -0.4081
_refine_diff_density_rms         0.0828
_refine_ls_d_res_high            0.8392
_refine_ls_d_res_low             7.9202
_refine_ls_goodness_of_fit_ref   1.0836
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    105
_refine_ls_number_parameters     407
_refine_ls_number_reflns         5578
_refine_ls_number_restraints     522
_refine_ls_restrained_S_all      1.0327
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          -0.0010
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+1.5013P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1470
_refine_ls_wR_factor_ref         0.1772
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -14
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              -10
_reflns_number_gt                3816
_reflns_number_total             5578
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4nj01878h2.cif
_cod_data_source_block           j3
_cod_depositor_comments
'Adding full bibliography for 7063310--7063313.cif.'
_cod_original_formula_sum        'C22 H37 Cl2 Co1 N3 S6'
_cod_database_code               7063313
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
2. Rigid body (RIGU) restrains
 Co01, S007, S004, S006, S002, S005, S003, C8, C15, C7, N00B, N009, N00C, C14,
 C9, C16, C21, C1, C6, C13, C10, C17, C20, C2, C5, C12, C11, C18, C19, C3, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S005, Co01, S007, S004, S006, S002, S003, C8, C15, C7, N00B, N009, N00C, C14,
 C9, C16, C21, C1A, C6A, C13A, C10A, C17a, C20a, C2A, C5A, C12A, C11A, C18a,
 C19a, C3A, C4A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: H14(0.5) H14c(0.5) H14d(0.5) H9aa(0.5) H9ab(0.5) H9bc(0.5)
 H9bd(0.5) H16(0.5) C1(0.5) H1a(0.5) H1b(0.5) C2(0.5) H2a(0.5) H2b(0.5) C3(0.5)
 H3a(0.5) H3b(0.5) C4(0.5) H4a(0.5) H4b(0.5) C5(0.5) H5a(0.5) H5b(0.5) C6(0.5)
 H6a(0.5) H6b(0.5) C1A(0.5) H1Aa(0.5) H1Ab(0.5) C2A(0.5) C3A(0.5) H3Aa(0.5)
 H3Ab(0.5) C4A(0.5) H4Aa(0.5) H4Ab(0.5) C10(0.5) H10a(0.5) H10b(0.5) C13(0.5)
 H13(0.5) C12(0.5) H12a(0.5) H12b(0.5) C11(0.5) H11a(0.5) H11b(0.5) C10A(0.5)
 H10c(0.5) H10d(0.5) C13A(0.5) H13c(0.5) H13d(0.5) C11A(0.5) H11c(0.5)
 C12A(0.5) H12c(0.5) C5A(0.5) H5Aa(0.5) H5Ab(0.5) C6A(0.5) H6Aa(0.5) H6Ab(0.5)
 H17c(0.5) H16a(0.5) H16b(0.5) H16c(0.5) H16d(0.5) H21a(0.5) H21b(0.5)
 H21c(0.5) H21d(0.5) C17(0.5) H17a(0.5) H17b(0.5) C18(0.5) H18a(0.5) H18b(0.5)
 C19(0.5) H19a(0.5) H19b(0.5) C20(0.5) H20a(0.5) H20b(0.5) C17a(0.5) H17c(0.5)
 H17d(0.5) C18a(0.5) H18c(0.5) H18d(0.5) C19a(0.5) H19c(0.5) H19d(0.5)
 C20a(0.5) H20c(0.5) H20d(0.5) H14a(0.5) H14b(0.5) H13a(0.5) H13b(0.5)
 H11c(0.5) H11d(0.5) H12c(0.5) H12d(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C14(H14c,H14d), C9(H9aa,H9ab), C9(H9bc,H9bd), C1(H1a,H1b), C2(H2a,H2b),
 C3(H3a,H3b), C4(H4a,H4b), C5(H5a,H5b), C6(H6a,H6b), C1A(H1Aa,H1Ab), C3A(H3Aa,
 H3Ab), C4A(H4Aa,H4Ab), C10(H10a,H10b), C12(H12a,H12b), C11(H11a,H11b),
 C10A(H10c,H10d), C13A(H13c,H13d), C5A(H5Aa,H5Ab), C6A(H6Aa,H6Ab), C16(H16a,
 H16b), C16(H16c,H16d), C21(H21a,H21b), C21(H21c,H21d), C17(H17a,H17b),
 C18(H18a,H18b), C19(H19a,H19b), C20(H20a,H20b), C17a(H17c,H17d), C18a(H18c,
 H18d), C19a(H19c,H19d), C20a(H20c,H20d), C14(H14a,H14b), C13(H13a,H13b),
 C11A(H11c,H11d), C12A(H12c,H12d)
;
_smtbx_masks_void_probe_radius   1.1
_smtbx_masks_void_truncation_radius 1.1
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.828
_oxdiff_exptl_absorpt_empirical_full_min 0.670