Ligand-centred redox activation of inert organoiridium anticancer catalysts
Zhang, Wen-Ying; Banerjee, Samya; Hughes, George M.; Bridgewater, Hannah E.; Song, Ji-Inn; Breeze, Ben G.; Clarkson, Guy J.; Coverdale, James P. C.; Sanchez-Cano, Carlos; Ponte, Fortuna; Sicilia, Emilia; Sadler, Peter J.; Chemical Science 11 (2020) 5466–5480; doi:10.1039/D0SC00897D

data_1558068
_publ_section_title
;
 Ligand-centred redox activation of inert organoiridium anticancer
 catalysts
;
_journal_issue                   21
_journal_name_full               'Chemical Science'
_journal_page_first              5466
_journal_page_last               5480
_journal_paper_doi               10.1039/D0SC00897D
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C26 H26 I Ir N3, I'
_chemical_formula_sum            'C26 H26 I2 Ir N3'
_chemical_formula_weight         826.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2018-08-08 deposited with the CCDC.	2020-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.7830(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.19420(10)
_cell_length_b                   8.21580(10)
_cell_length_c                   33.7933(3)
_cell_measurement_reflns_used    28319
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.4240
_cell_measurement_theta_min      4.8160
_cell_volume                     2539.68(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3046
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_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   -113.00 -16.00   1.00    1.00    --  -42.36 -57.00-180.00   97
  2  \w   -115.00 -20.00   1.00    1.00    --  -42.36 -37.00 -30.00   95
  3  \w    -96.00  -2.00   1.00    1.00    --  -42.36 125.00 -30.00   94
  4  \w      1.00  82.00   1.00    1.00    --   42.36 -99.00-150.00   81
  5  \w     82.00 178.00   1.00    4.00    --  106.00  30.00  30.00   96
  6  \w     34.00 121.00   1.00    4.00    --  106.00-125.00 -90.00   87
  7  \w     25.00 109.00   1.00    4.00    --  106.00 -94.00  30.00   84
  8  \w     32.00 137.00   1.00    4.00    --  106.00 -77.00  90.00  105
  9  \w     31.00 130.00   1.00    4.00    --  106.00 -30.00   0.00   99
 10  \w     82.00 178.00   1.00    4.00    --  106.00  30.00-180.00   96
 11  \w     31.00 130.00   1.00    4.00    --  106.00 -30.00-150.00   99
 12  \w     31.00 130.00   1.00    4.00    --  106.00 -30.00  90.00   99
 13  \w     32.00 137.00   1.00    4.00    --  106.00 -77.00-120.00  105
 14  \w   -113.00 -16.00   1.00    1.00    --  -42.36 -57.00 -90.00   97
 15  \w    -65.00  31.00   1.00    1.00    --  -42.36  37.00 -30.00   96
 16  \w   -113.00 -16.00   1.00    1.00    --  -42.36 -57.00  90.00   97
 17  \w   -116.00 -11.00   1.00    1.00    --  -42.36 -77.00  30.00  105
 18  \w     78.00 176.00   1.00    4.00    --  106.00  61.00-180.00   98
 19  \w     78.00 176.00   1.00    4.00    --  106.00  61.00 -30.00   98
 20  \w     82.00 177.00   1.00    4.00    --  106.00  45.00  90.00   95
 21  \w     75.00 178.00   1.00    4.00    --  106.00  77.00  30.00  103
 22  \w     61.00 178.00   1.00    4.00    --  106.00  15.00 -60.00  117
 23  \w     75.00 178.00   1.00    4.00    --  106.00  77.00 -90.00  103
 24  \w     78.00 176.00   1.00    4.00    --  106.00  61.00-150.00   98
 25  \w     78.00 176.00   1.00    4.00    --  106.00  61.00 120.00   98
 26  \w   -116.00 -11.00   1.00    1.00    --  -42.36 -77.00  90.00  105
 27  \w   -116.00 -11.00   1.00    1.00    --  -42.36 -77.00 -60.00  105
 28  \w      1.00  82.00   1.00    1.00    --   42.36 -99.00 120.00   81
 29  \w     11.00 116.00   1.00    1.00    --   42.36  77.00-150.00  105
 30  \w     75.00 178.00   1.00    4.00    --  106.00  77.00   0.00  103
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0157583000
_diffrn_orient_matrix_UB_12      -0.1565496000
_diffrn_orient_matrix_UB_13      -0.0251490000
_diffrn_orient_matrix_UB_21      -0.0604828000
_diffrn_orient_matrix_UB_22      0.1006682000
_diffrn_orient_matrix_UB_23      -0.0364798000
_diffrn_orient_matrix_UB_31      0.1563379000
_diffrn_orient_matrix_UB_32      0.0231431000
_diffrn_orient_matrix_UB_33      -0.0116793000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            43995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.554
_diffrn_reflns_theta_min         4.834
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    29.401
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.162
_exptl_crystal_description       block
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.259
_refine_diff_density_min         -1.291
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         5081
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0255
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+5.2482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0613
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5010
_reflns_number_total             5081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc00897d2.cif
_cod_data_source_block           wz3
_cod_depositor_comments
;Adding full bibliography for 1558064--1558071.cif.

 Adding full bibliography for 1558064--1558071.cif.
;
_cod_database_code               1558068
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C20 H20 N2 O2 F6 P I Ir'
_shelx_estimated_absorpt_t_max   0.591
_shelx_estimated_absorpt_t_min   0.067
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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 Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C11(H11), C18(H18), C5(H5), C4(H4), C10(H10), C19(H19),
 C14(H14), C15(H15), C13(H13), C16(H16), C17(H17), C12(H12)
2.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C27(H27A,H27B,H27C), C26(H26A,H26B,
 H26C)
;
_shelx_res_checksum              40283
_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 4.914
_oxdiff_exptl_absorpt_empirical_full_min 0.540