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_1567149
_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
'2(C23 H42 Ir N4 O P2), F, 0.5(F2 H4 O2), C2 H3 N'
_chemical_formula_sum            'C48 H89 F2 Ir2 N9 O3 P4'
_chemical_formula_weight         1386.56
_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   mixed
_atom_sites_solution_primary     dual
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_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                67.2030(10)
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_cell_angle_gamma                89.3060(10)
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_cell_length_c                   17.0807(2)
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_diffrn_measured_fraction_theta_max 0.999
_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    -95.00  11.00   0.50    5.00    --  -15.66 -34.00  30.00  212
  2  \w    -10.00  89.00   0.50    5.00    --   14.25  57.00 -90.00  198
  3  \w    -17.00  89.00   0.50    5.00    --   14.25  77.00-150.00  212
  4  \w    -17.00  89.00   0.50    5.00    --   14.25  77.00 -60.00  212
  5  \w    -42.00  64.00   0.50    5.00    --  -15.66  34.00-171.00  212
  6  \w    -40.00  61.00   0.50    5.00    --  -15.66  48.00 -14.74  202
  7  \w    -46.00  59.00   0.50    5.00    --  -15.66  77.00  60.00  210
  8  \w    -60.00 -20.00   0.50    5.00    --   14.25 -77.00-150.00   80
  9  \w    -60.00  39.00   0.50    5.00    --   14.25 -57.00 -90.00  198
 10  \w    -90.00  15.00   0.50    5.00    --  -15.66 -77.00  30.00  210
 11  \w    -90.00   9.00   0.50    5.00    --  -15.66 -57.00 -30.00  198
 12  \w    -97.00   2.00   0.50    5.00    --  -15.66 -19.00-150.00  198
;
_diffrn_measurement_device       '\k-geometry diffractometer'
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'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0557742000
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_diffrn_orient_matrix_UB_13      -0.0067342000
_diffrn_orient_matrix_UB_21      -0.0014857000
_diffrn_orient_matrix_UB_22      0.0322105000
_diffrn_orient_matrix_UB_23      0.0191354000
_diffrn_orient_matrix_UB_31      0.0269031000
_diffrn_orient_matrix_UB_32      0.0341667000
_diffrn_orient_matrix_UB_33      -0.0421810000
_diffrn_radiation_monochromator  mirror
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_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            87784
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         1.778
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.750
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_description       prism
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
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_refine_ls_extinction_method     none
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_refine_ls_restrained_S_all      1.358
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0461
_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^)+49.9701P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1246
_reflns_number_gt                13222
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_cod_data_source_file            d2sc00279e2.cif
_cod_data_source_block           8063
_cod_depositor_comments
'Adding full bibliography for 1567146--1567153.cif.'
_cod_database_code               1567149
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.732
_shelx_estimated_absorpt_t_min   0.600
_shelx_res_checksum              91597
_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 1.414
_oxdiff_exptl_absorpt_empirical_full_min 0.772