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_1567150
_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         'C22 H42 Ir N4 P2, F6 P, 0.5(C6 H12 O2)'
_chemical_formula_sum            'C25 H48 F6 Ir N4 O P3'
_chemical_formula_weight         819.78
_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     dual
_audit_creation_date             2020-03-10
_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                77.4270(10)
_cell_angle_beta                 82.2190(10)
_cell_angle_gamma                84.3570(10)
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_cell_length_b                   16.1281(3)
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_computing_data_collection       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
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_diffrn_ambient_environment      N~2~
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_diffrn_detector                 'HPC area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'Dectris Pilatus3 R 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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     -9.00  83.00   0.50   15.00    --    5.23  37.00  30.00  184
  2  \w    -25.00  29.00   0.50   15.00    --    5.23 -77.00 -90.00  108
  3  \w    -25.00  18.00   0.50   15.00    --   -5.54 -77.00-180.00   86
  4  \w    -25.00  18.00   0.50   15.00    --   -5.54 -77.00-150.00   86
  5  \w    -20.00  74.00   0.50   15.00    --   -5.54  19.00 -30.00  188
  6  \w    -20.00  72.00   0.50   15.00    --   -5.54  37.00-150.00  184
  7  \w    -29.00  25.00   0.50   15.00    --   -5.54  77.00  30.00  108
  8  \w    -29.00  25.00   0.50   15.00    --   -5.54  77.00  90.00  108
  9  \w    -18.00  21.00   0.50   15.00    --    5.23  77.00 150.00   78
 10  \w    -29.00  25.00   0.50   15.00    --   -5.54  77.00 120.00  108
 11  \w    -59.00  11.00   0.50   15.00    --   -5.54 -57.00   0.00  140
 12  \w    -25.00  29.00   0.50   15.00    --    5.23 -77.00  30.00  108
 13  \w    -25.00  18.00   0.50   15.00    --   -5.54 -77.00  90.00   86
 14  \w    -59.00  11.00   0.50   15.00    --   -5.54 -57.00 120.00  140
;
_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      0.0232172000
_diffrn_orient_matrix_UB_12      0.0388570000
_diffrn_orient_matrix_UB_13      -0.0049195000
_diffrn_orient_matrix_UB_21      0.0209126000
_diffrn_orient_matrix_UB_22      -0.0031520000
_diffrn_orient_matrix_UB_23      -0.0418547000
_diffrn_orient_matrix_UB_31      -0.0442747000
_diffrn_orient_matrix_UB_32      0.0228245000
_diffrn_orient_matrix_UB_33      -0.0158804000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            96516
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.417
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.190
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71532
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_description       plate
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         5.162
_refine_diff_density_min         -1.951
_refine_diff_density_rms         0.268
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     785
_refine_ls_number_reflns         16564
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0649
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+81.8783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1615
_refine_ls_wR_factor_ref         0.1766
_reflns_number_gt                12539
_reflns_number_total             16564
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00279e2.cif
_cod_data_source_block           8034
_cod_depositor_comments
'Adding full bibliography for 1567146--1567153.cif.'
_cod_database_code               1567150
_shelx_shelxl_version_number     2018/3
_diffrn_oxdiff_digest_frames
;
016e6062668a447496d5494422f497552001712c12a
;
_diffrn_oxdiff_digest_hkl
;
0191b914601e4ff51f2a450c8e03fb30cf4976
;
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_shelx_res_checksum              92161
_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 1.467
_oxdiff_exptl_absorpt_empirical_full_min 0.795