The underappreciated influence of ancillary halide on metal-ligand proton tautomerism.
Jain, Anant Kumar; Gau, Michael R.; Carroll, Patrick J.; Goldberg, Karen I.; Chemical science 13 (2022) 7837–7845; doi:10.1039/d2sc00279e

data_1567148
_publ_section_title
;
 The underappreciated influence of ancillary halide on metal-ligand proton
 tautomerism.
;
_journal_issue                   26
_journal_name_full               'Chemical science'
_journal_page_first              7837
_journal_page_last               7845
_journal_paper_doi               10.1039/d2sc00279e
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C24 H42 Cl Ir N4 O P2, C H2 Cl2'
_chemical_formula_sum            'C25 H44 Cl3 Ir N4 O P2'
_chemical_formula_weight         777.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
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Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
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_audit_update_record
;
2021-11-23 deposited with the CCDC.	2022-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.0160(10)
_cell_angle_gamma                90
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_cell_length_c                   25.8721(3)
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_diffrn_ambient_environment      N~2~
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_diffrn_detector                 'HPC area detector'
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_diffrn_measured_fraction_theta_max 1.000
_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    -26.00   1.00   0.50    1.00    --   -9.89  77.00 -90.00   54
  2  \w    -32.00  17.00   0.50    1.00    --   -9.89  80.00 -54.24   98
  3  \w     34.00  63.00   0.50    1.00    --   -9.89  77.00 -90.00   58
  4  \w    -21.00  59.00   0.50    1.00    --   -9.89  57.00-120.00  160
  5  \w    -27.00  -1.00   0.50    1.00    --   -9.89  79.00 102.84   52
  6  \w    -31.00  12.00   0.50    1.00    --   -9.89  78.00 143.80   86
  7  \w     17.00  52.00   0.50    1.00    --   -9.89  31.00  81.00   70
  8  \w    -58.00   3.00   0.50    1.00    --   -9.89 -31.00 -78.00  122
  9  \w    -75.00 -12.00   0.50    1.00    --   -9.89 -57.00-150.00  126
 10  \w    -68.00   5.00   0.50    1.00    --   -9.89 -57.00 -90.00  146
 11  \w    -69.00 -23.00   0.50    1.00    --   -9.89 -77.00 -30.00   92
 12  \w    -64.00 -10.00   0.50    1.00    --   -9.89 -77.00   0.00  108
 13  \w    -80.00  13.00   0.50    1.00    --   -9.89 -77.00  90.00  186
;
_diffrn_measurement_device       '\k-geometry diffractometer'
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'CrysAlisPro convention (1999,Acta A55,543-557)'
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_diffrn_orient_matrix_UB_21      0.0592215000
_diffrn_orient_matrix_UB_22      -0.0057022000
_diffrn_orient_matrix_UB_23      0.0002053000
_diffrn_orient_matrix_UB_31      -0.0014843000
_diffrn_orient_matrix_UB_32      0.0277712000
_diffrn_orient_matrix_UB_33      -0.0251613000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            67574
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         1.832
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.629
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76064
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_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_description       block
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_exptl_crystal_size_min          0.2
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_refine_ls_extinction_method     none
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_refine_ls_number_reflns         7805
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_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0182
_refine_ls_R_factor_gt           0.0163
_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^)+(0.0061P)^2^+3.6611P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0335
_refine_ls_wR_factor_ref         0.0340
_reflns_number_gt                7369
_reflns_number_total             7805
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00279e2.cif
_cod_data_source_block           8111
_cod_depositor_comments
'Adding full bibliography for 1567146--1567153.cif.'
_cod_database_code               1567148
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              35044
_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 1.186
_oxdiff_exptl_absorpt_empirical_full_min 0.862