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_1567151
_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         'C23 H42 Ir N4 O P2, Br'
_chemical_formula_sum            'C23 H42 Br Ir N4 O P2'
_chemical_formula_weight         724.65
_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             2020-07-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-11-23 deposited with the CCDC.	2022-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.189(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7005(4)
_cell_length_b                   8.11750(10)
_cell_length_c                   21.3840(4)
_cell_measurement_reflns_used    20097
_cell_measurement_temperature    100
_cell_measurement_theta_max      74.1100
_cell_measurement_theta_min      4.2200
_cell_volume                     2864.81(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2019)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'HPC area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            HyPix-6000HE
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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    -35.00  25.00   0.50    3.00    --  -48.77  26.00 -52.00  120
  2  \w    -50.00  23.00   0.50    3.00    --  -48.77  57.00-120.00  146
  3  \w    -50.00 -24.00   0.50   12.00    --  -84.25  45.00 -90.00   52
  4  \w    -61.00  23.00   0.50    3.00    --  -48.77  57.00   0.00  168
  5  \w    -26.00  25.00   0.50    3.00    --  -48.77  19.00 120.00  102
  6  \w    -21.00   7.00   0.50    3.00    --  -48.77  77.00 120.00   56
  7  \w    -69.00 -27.00   0.50    3.00    --  -48.77  77.00 120.00   84
  8  \w    -64.00 -38.00   0.50   12.00    --  -84.25  61.00 120.00   52
  9  \w   -122.00 -41.00   0.50    3.00    --  -48.77 -26.00 143.00  162
 10  \w    -24.00  29.00   0.50    3.00    --   48.77 -26.00 143.00  106
 11  \w     38.00  68.00   0.50   12.00    --  105.75 -61.00 150.00   60
 12  \w     79.00 122.00   0.50   12.00    --  105.75 -80.00 126.86   86
 13  \w    100.00 169.00   0.50   12.00    --  105.75  15.00  60.00  138
 14  \w    129.00 171.00   0.50   12.00    --  105.75  61.00 120.00   84
 15  \w    107.00 173.00   0.50   12.00    --  105.75  48.00 142.20  132
 16  \w    103.00 178.00   0.50   12.00    --  105.75  15.00 120.00  150
 17  \w     97.00 164.00   0.50   12.00    --  105.75  45.00   0.00  134
 18  \w     98.00 161.00   0.50   12.00    --  105.75  26.00 -52.00  126
 19  \w    110.00 147.00   0.50   12.00    --  105.75  15.00-150.00   74
 20  \w    150.00 176.00   0.50   12.00    --  105.75  15.00-150.00   52
 21  \w    125.00 175.00   0.50   12.00    --  105.75  61.00-150.00  100
 22  \w    102.00 165.00   0.50   12.00    --  105.75  30.00 -90.00  126
 23  \w     87.00 113.00   0.50   12.00    --  105.75 -80.00 -63.60   52
 24  \w     92.00 118.00   0.50   12.00    --  105.75 -80.00  -6.50   52
 25  \w     73.00 117.00   0.50   12.00    --  105.75 -80.00 -99.92   88
 26  \w     82.00 126.00   0.50   12.00    --  105.75 -80.00-155.00   88
 27  \w     53.00  89.00   0.50   12.00    --  105.75 -77.00-120.00   72
 28  \w     35.00  63.00   0.50   12.00    --  105.75 -61.00 -60.00   56
 29  \w     37.00 101.00   0.50   12.00    --  105.75 -77.00 -60.00  128
 30  \w     54.00  80.00   0.50   12.00    --  105.75 -80.00  -6.50   52
 31  \w     37.00  68.00   0.50   12.00    --  105.75 -61.00  30.00   62
 32  \w     60.00 123.00   0.50   12.00    --  105.75 -80.00  60.27  126
 33  \w     41.00 122.00   0.50    3.00    --   48.77  26.00 -52.00  162
 34  \w     39.00  64.00   0.50   12.00    --  105.75 -61.00  60.00   50
 35  \w     45.00  73.00   0.50   12.00    --  105.75 -77.00  30.00   56
 36  \w     43.00  95.00   0.50   12.00    --  105.75 -77.00   0.00  104
 37  \w     38.00  68.00   0.50   12.00    --  105.75 -61.00  90.00   60
 38  \w     37.00  63.00   0.50   12.00    --  105.75 -80.00 126.86   52
 39  \w     40.00  88.00   0.50   12.00    --  105.75 -77.00 150.00   96
 40  \w     40.00  83.00   0.50   12.00    --  105.75 -77.00  90.00   86
 41  \w     37.00 124.00   0.50   12.00    --  105.75 -80.00  23.69  174
 42  \w     34.00  60.00   0.50   12.00    --  105.75 -61.00-150.00   52
 43  \w     42.00  78.00   0.50   12.00    --  105.75 -80.00-155.00   72
 44  \w     37.00  80.00   0.50   12.00    --  105.75 -77.00-150.00   86
 45  \w     40.00  74.00   0.50   12.00    --  105.75 -80.00 -63.60   68
 46  \w     34.00  59.00   0.50   12.00    --  105.75 -61.00-180.00   50
 47  \w    -10.00  17.00   0.50    3.00    --   48.77 -19.00   0.00   54
 48  \w     36.00  66.00   0.50   12.00    --  105.75 -61.00 120.00   60
 49  \w   -158.00 -92.00   0.50   12.00    --  -84.25 -26.00 143.00  132
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-S'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0925882000
_diffrn_orient_matrix_UB_12      0.0021706000
_diffrn_orient_matrix_UB_13      -0.0184073000
_diffrn_orient_matrix_UB_21      -0.0019573000
_diffrn_orient_matrix_UB_22      0.1837770000
_diffrn_orient_matrix_UB_23      -0.0184985000
_diffrn_orient_matrix_UB_31      -0.0118891000
_diffrn_orient_matrix_UB_32      -0.0474049000
_diffrn_orient_matrix_UB_33      -0.0726888000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0770
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            44440
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.501
_diffrn_reflns_theta_min         2.677
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.875
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_description       needle
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.044
_refine_diff_density_min         -2.374
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         5853
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0671P)^2^+6.1235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1145
_reflns_number_gt                5235
_reflns_number_total             5853
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00279e2.cif
_cod_data_source_block           8044
_cod_depositor_comments
'Adding full bibliography for 1567146--1567153.cif.'
_cod_database_code               1567151
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.237
_shelx_res_checksum              51775
_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 3.089
_oxdiff_exptl_absorpt_empirical_full_min 0.500