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_1567153
_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 H41 Ir N4 O P2, 1.5(C2 H3 N)'
_chemical_formula_sum            'C26 H45.5 Ir N5.5 O P2'
_chemical_formula_weight         705.32
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-12
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   26.01830(10)
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_cell_length_c                   31.3406(2)
_cell_measurement_reflns_used    217240
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.35
_cell_measurement_theta_min      1.73
_cell_volume                     19107.95(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
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_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'HPC area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            HyPix-6000HE
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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    -11.00  96.00   0.50   10.00    --   19.17  57.00 -58.00  214
  2  \w    -11.00  96.00   0.50   10.00    --   19.17  57.00-120.00  214
  3  \w    -11.00  96.00   0.50   10.00    --   19.17  57.00 -30.00  214
  4  \w    -19.00  98.00   0.50   10.00    --   19.17  77.00  90.00  234
  5  \w    -20.00 103.00   0.50   10.00    --   19.17  37.00  60.00  246
  6  \w    -51.00  57.00   0.50   10.00    --  -20.58  57.00 -58.00  216
  7  \w    -58.00  41.00   0.50   10.00    --   19.17 -57.00 159.00  198
  8  \w    -64.00  18.00   0.50   10.00    --   19.17 -37.00   0.00  164
  9  \w    -60.00  34.00   0.50   10.00    --   19.17 -77.00-120.00  188
 10  \w    -58.00  41.00   0.50   10.00    --   19.17 -57.00  60.00  198
 11  \w    -98.00  10.00   0.50   10.00    --  -20.58 -57.00 159.00  216
 12  \w    -99.00  18.00   0.50   10.00    --  -20.58 -77.00 120.00  234
 13  \w    -99.00  18.00   0.50   10.00    --  -20.58 -77.00   0.00  234
;
_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      -0.0182505000
_diffrn_orient_matrix_UB_12      -0.0182525000
_diffrn_orient_matrix_UB_13      -0.0098404000
_diffrn_orient_matrix_UB_21      -0.0096014000
_diffrn_orient_matrix_UB_22      0.0233858000
_diffrn_orient_matrix_UB_23      -0.0119710000
_diffrn_orient_matrix_UB_31      0.0178400000
_diffrn_orient_matrix_UB_32      -0.0060879000
_diffrn_orient_matrix_UB_33      -0.0164930000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            563209
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.327
_diffrn_reflns_theta_min         1.738
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.319
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6046
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       prism
_exptl_crystal_F_000             8520
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.502
_refine_diff_density_min         -1.298
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     994
_refine_ls_number_reflns         23761
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.264
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0299P)^2^+118.6224P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.0996
_reflns_number_gt                21647
_reflns_number_total             23761
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00279e2.cif
_cod_data_source_block           8062
_cod_depositor_comments
'Adding full bibliography for 1567146--1567153.cif.'
_cod_original_formula_sum        'C26 H45.50 Ir N5.50 O P2'
_cod_database_code               1567153
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C79 H138 N12 O3 P6 Ir3'
_shelx_estimated_absorpt_t_max   0.782
_shelx_estimated_absorpt_t_min   0.510
_shelx_res_checksum              99969
_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 1.480
_oxdiff_exptl_absorpt_empirical_full_min 0.820