Phenalenyl based platinum anticancer compounds with superior efficacy: design, synthesis, characterization, and interaction with nuclear DNA
Dutta, Pradip; Kumari, Smita; Paulraj, Justin; Sharma, Rupali; Vijaykumar, Gonela; Sankar Das, Hari; P, Sreejyothi; Sil, Swagata; Mandal, Swadhin K.; Sengupta, Aniruddha; Sarkar, Arindam; New Journal of Chemistry 45 (2021) 10524–10533; doi:10.1039/D0NJ06229D

data_7060609
_publ_section_title
;
 Phenalenyl based platinum anticancer compounds with superior efficacy:
 design, synthesis, characterization, and interaction with nuclear DNA
;
_journal_issue                   23
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10524
_journal_page_last               10533
_journal_paper_doi               10.1039/D0NJ06229D
_journal_volume                  45
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C15 H13 Cl O3 Pt S, 0.5(C H Cl3)'
_chemical_formula_sum            'C15.5 H13.5 Cl2.5 O3 Pt S'
_chemical_formula_weight         563.54
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-11-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-12 deposited with the CCDC.	2021-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.4285(7)
_cell_length_b                   15.7599(9)
_cell_length_c                   16.4621(9)
_cell_measurement_reflns_used    4334
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.9960
_cell_measurement_theta_min      2.3560
_cell_volume                     3483.9(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0612
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22167
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.35
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    8.568
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51186
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.149
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.636
_refine_diff_density_min         -1.400
_refine_diff_density_rms         0.240
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.007(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         7112
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0897
_reflns_number_gt                5339
_reflns_number_total             7112
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0nj06229d2.cif
_cod_data_source_block           sample2
_cod_depositor_comments
;
          Adding full bibliography for 7060609.cif.

2024-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C31 H27 Cl5 O6 Pt2 S2'
_cod_original_formula_weight         1127.08
_cod_original_formula_moiety         '2(C15 H13 Cl O3 Pt S), C H Cl3'
_cod_original_formula_units_Z            4
_cod_database_code               7060609
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C16(H16)
2.b Aromatic/amide H refined with riding coordinates:
 C10A(H10A), C9A(H9A), C3A(H3A), C2B(H2B), C2A(H2A), C9B(H9B), C10B(H10B),
 C5A(H5A), C3B(H3B), C6B(H6B), C5B(H5B), C7A(H7A), C7B(H7B), C6A(H6A)
2.c Idealised Me refined as rotating group:
 C14A(H14A,H14B,H14C), C15A(H15A,H15B,H15C), C15B(H15D,H15E,H15F), C14B(H14D,
 H14E,H14F)
;
_olex2_submission_special_instructions 'No special instructions were received'