Anticancer Organorhodium and -iridium Complexes with Low Toxicity in vivo but High Potency in vitro: DNA Damage, Reactive Oxygen Species Formation, and Haemolytic Activity
Parveen, Shahida; Hanif, Muhammad; Leung, Euphemia; Tong, Kelvin; Yang, Annie; Astin, Jonathan; De Zoysa , Gayan Heruka; Steel , Tasha R.; Goodman, David; Movassaghi, Sanam; Soehnel, Tilo; Sarojini, Vijayalekshmi; Jamieson, Stephen; Hartinger, Christian; Chemical Communications  (2019) –; doi:10.1039/C9CC03822A

data_7124093
_publ_section_title
;
 Anticancer Organorhodium and -iridium Complexes with Low Toxicity in vivo
 but High Potency in vitro: DNA Damage, Reactive Oxygen Species Formation,
 and Haemolytic Activity
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC03822A
_journal_year                    2019
_chemical_formula_moiety         'C36 H48 Cl2 N2 O4 Rh2, 4(H2 O)'
_chemical_formula_sum            'C36 H56 Cl2 N2 O8 Rh2'
_chemical_formula_weight         921.54
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-03-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-13 deposited with the CCDC.    2019-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                75.400(2)
_cell_angle_beta                 76.174(2)
_cell_angle_gamma                76.504(2)
_cell_formula_units_Z            1
_cell_length_a                   8.3327(3)
_cell_length_b                   8.6240(4)
_cell_length_c                   14.4874(6)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.904
_cell_measurement_theta_min      2.483
_cell_volume                     961.52(7)
_computing_cell_refinement       'SAINT V8.32B (?, 2016)'
_computing_data_reduction        'SAINT V8.32B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'BRUKER APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22123
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.561
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.049
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.6293
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0796 before and 0.0577 after correction.
The Ratio of minimum to maximum transmission is 0.8429.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_description       irregular
_exptl_crystal_F_000             474
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.007
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         4737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0335
_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/[\s^2^(Fo^2^)+(0.0323P)^2^+1.6466P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0819
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4271
_reflns_number_total             4737
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03822a2.cif
_cod_data_source_block           d4rhp1_p-1
_cod_database_code               7124093
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.884
_shelx_estimated_absorpt_t_min   0.704
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Others
 Fixed Sof: H1(0.5) H3B(0.5)
3.a Riding coordinates:
 C1'(H1'A,H1'B), C2'(H2'A,H2'B), C6(H6)
3.b Free rotating group:
 O3(H3A,H3B), O4(H4A,H4B)
3.c Aromatic/amide H refined with riding coordinates:
 C5(H5)
3.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C),
 C15(H15A,H15B,H15C), C17(H17A,H17B,H17C)
;
_olex2_submission_special_instructions 'No special instructions were received'