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_1558071
_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 Cl Ir N3 O, F6 P'
_chemical_formula_sum            'C26 H26 Cl F6 Ir N3 O P'
_chemical_formula_weight         769.12
_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
_audit_creation_date             2016-01-14
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2019-06-08 deposited with the CCDC.	2020-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                89.3248(16)
_cell_angle_beta                 78.0376(16)
_cell_angle_gamma                88.7062(17)
_cell_formula_units_Z            2
_cell_length_a                   8.71914(18)
_cell_length_b                   9.9018(2)
_cell_length_c                   15.7288(3)
_cell_measurement_reflns_used    30461
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      37.2050
_cell_measurement_theta_min      3.1190
_cell_volume                     1328.09(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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 5.1417
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.966
_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    -44.00  54.00   1.00   20.50    --   29.88 -38.00 120.00   98
  2  \w     32.00 117.00   1.00   20.50    --   29.88-178.00 150.00   85
  3  \w      5.00 104.00   1.00   20.50    --   29.88  38.00 -60.00   99
  4  \w     12.00 101.00   1.00   20.50    --   29.88-149.00-108.00   89
  5  \w     -3.00 106.00   1.00   20.50    --   29.88  77.00   0.00  109
  6  \w      2.00 103.00   1.00   20.50    --   29.88  57.00 -60.00  101
  7  \w   -107.00   2.00   1.00   20.50    --  -30.82 -77.00 -30.00  109
  8  \w   -120.00 -57.00   1.00   20.50    --  -30.82-178.00 -30.00   63
  9  \w      5.00 104.00   1.00   20.50    --   29.88  38.00-180.00   99
 10  \w    -44.00  54.00   1.00   20.50    --   29.88 -38.00-120.00   98
 11  \w     -3.00 106.00   1.00   20.50    --   29.88  77.00-180.00  109
 12  \w   -118.00 -53.00   1.00   20.50    --  -30.82 178.00-120.00   65
 13  \w   -118.00 -93.00   1.00   20.50    --  -30.82 178.00 150.00   25
 14  \w   -104.00  -3.00   1.00   20.50    --  -30.82 -57.00  30.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0303335000
_diffrn_orient_matrix_UB_12      -0.0672244000
_diffrn_orient_matrix_UB_13      -0.0039708000
_diffrn_orient_matrix_UB_21      -0.0213268000
_diffrn_orient_matrix_UB_22      -0.0084284000
_diffrn_orient_matrix_UB_23      0.0457467000
_diffrn_orient_matrix_UB_31      -0.0744500000
_diffrn_orient_matrix_UB_32      -0.0233271000
_diffrn_orient_matrix_UB_33      -0.0040579000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            66113
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         37.686
_diffrn_reflns_theta_min         2.647
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.256
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48568
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.923
_exptl_crystal_description       block
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.627
_refine_diff_density_min         -1.153
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         13636
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0247P)^2^+0.7469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0618
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12253
_reflns_number_total             13636
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc00897d2.cif
_cod_data_source_block           gh3
_cod_depositor_comments
;Adding full bibliography for 1558064--1558071.cif.

 Adding full bibliography for 1558064--1558071.cif.
;
_cod_original_cell_volume        1328.08(5)
_cod_database_code               1558071
_chemical_oxdiff_formula         'C20 H20 N2 O2 F6 P Cl Ir'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.23
_olex2_refinement_description
;

The OH was located in a difference map but refined with AFIX 147 constraint.

1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C13(H13), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C19(H19)
2.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C)
2.c Idealised tetrahedral OH refined as rotating group:
 O12(H12)
;
_shelx_shelxl_version_number     2014/7
_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 1.773
_oxdiff_exptl_absorpt_empirical_full_min 0.756