Anticancer Cyclometalated Iridium(III) Complexes with Planar Ligands: Mitochondrial DNA Damage and Metabolism Disturbance.
Cao, Jian-Jun; Zheng, Yue; Wu, Xiao-Wen; Tan, Cai-Ping; Chen, Mu-He; Wu, Na; Ji, Liang-Nian; Mao, Zong-Wan; Journal of medicinal chemistry 62 (2019) 3311–3322; doi:10.1021/acs.jmedchem.8b01704

data_1552563
_publ_section_title
;
 Anticancer Cyclometalated Iridium(III) Complexes with Planar Ligands:
 Mitochondrial DNA Damage and Metabolism Disturbance.
;
_journal_issue                   7
_journal_name_full               'Journal of medicinal chemistry'
_journal_page_first              3311
_journal_page_last               3322
_journal_paper_doi               10.1021/acs.jmedchem.8b01704
_journal_volume                  62
_journal_year                    2019
_chemical_formula_moiety         'C36 H22 Ir N6 S2, F6 P'
_chemical_formula_sum            'C36 H22 F6 Ir N6 P S2'
_chemical_formula_weight         1880.78
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-10-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                111.899(2)
_cell_angle_beta                 93.037(2)
_cell_angle_gamma                111.657(2)
_cell_formula_units_Z            4
_cell_length_a                   13.4535(8)
_cell_length_b                   16.0914(11)
_cell_length_c                   19.2715(11)
_cell_measurement_reflns_used    22038
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.01
_cell_volume                     3508.7(4)
_computing_cell_refinement       'Rigaku R-AXIS SPIDE IP'
_computing_data_collection       'Rigaku R-AXIS SPIDE IP'
_computing_data_reduction        'Rigaku R-AXIS SPIDE IP'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDE IP'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_av_unetI/netI     0.1081
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29512
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.456
_diffrn_reflns_theta_min         3.006
_exptl_absorpt_coefficient_mu    4.039
_exptl_absorpt_correction_T_max  0.587
_exptl_absorpt_correction_T_min  0.442
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_description       block
_exptl_crystal_F_000             1834
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.132
_refine_diff_density_max         3.227
_refine_diff_density_min         -1.698
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     937
_refine_ls_number_reflns         15271
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0681
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1012P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1699
_refine_ls_wR_factor_ref         0.1937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10004
_reflns_number_total             15271
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jm8b01704_si_002.cif
_cod_data_source_block           a
_cod_depositor_comments
;

2022-03-31
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C72 H45 F12 Ir2 N12 P2 S4'
_cod_original_formula_weight         1880.78
_cod_original_formula_moiety         '2(C36 H22 Ir N6 S2), 2(F6 P)'
_cod_original_formula_units_Z            2
_cod_database_code               1552563
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.618
_shelx_estimated_absorpt_t_min   0.481
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 P2-F7 = P2-F8 = P2-F9 = P2-F10 = P2-F11 = P2-F12
 1.55 with sigma of 0.02
 F9-F7 \\sim F9-F8 \\sim F9-F10 \\sim F9-F12
 with sigma of 0.02
 F11-F7 \\sim F11-F8 \\sim F11-F10 \\sim F11-F12
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F3) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F8) \\sim
Ueq, Uanis(F9) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F11) \\sim Ueq,
Uanis(F12) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C9) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C68) \\sim Ueq,
Uanis(C69) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C71)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(P2) \\sim Ueq, Uanis(F1) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C15(H15),
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C24(H24), C25(H25),
  C26(H26), C32(H32), C33(H33), C34(H34), C35(H35), C38(H38), C39(H39),
 C42(H42), C43(H43), C44(H44), C45(H45), C47(H47), C48(H48), C51(H51), C52(H52),
  C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C60(H60), C61(H61),
 C62(H62), C69(H69), C70(H70), C71(H71), C72(H72)
;
_shelx_res_checksum              97134
_shelx_hkl_checksum              23722
_shelx_fab_checksum              4617
_olex2_submission_special_instructions
'No special instructions were received PROBLEM: Large Average Ueq of Residue Including P1 0.206 Check RESPONSE: The atoms flagging this alert are from Ir atoms as part of the [Ir(ptz)2(dppz)]- anions. For these, residual electron density issues could be from slight positional disorder (static or dynamic), but potentially also from X-ray absorption or weakly diffracting supercell peaks, as opposed to wrongly assigned atom types or twinning. PROBLEM: Large Average Ueq of Residue Including P2 0.269 Check RESPONSE: The atoms flagging this alert are from Ir atoms as part of the [Ir(ptz)2(dppz)]- anions. For these, residual electron density issues could be from slight positional disorder (static or dynamic), but potentially also from X-ray absorption or weakly diffracting supercell peaks, as opposed to wrongly assigned atom types or twinning.'