The acid-mediated isomerization of iridium(III) complexes with cyclometalated NHC ligands: kinetic <i>vs.</i> thermodynamic control.
Gitlina, Anastasia Yu; Fadaei-Tirani, Farzaneh; Severin, Kay; Dalton transactions (Cambridge, England : 2003) 52 (2023) 2833–2837; doi:10.1039/d2dt04039e

data_7712442
_publ_section_title
;
 The acid-mediated isomerization of iridium(III) complexes with
 cyclometalated NHC ligands: kinetic <i>vs.</i> thermodynamic control.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2833
_journal_page_last               2837
_journal_paper_doi               10.1039/d2dt04039e
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C60 H46 Ir N6, C2 F6 N O4 S2'
_chemical_formula_sum            'C62 H46 F6 Ir N7 O4 S2'
_chemical_formula_weight         1323.38
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-09-29
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-09-29 deposited with the CCDC.	2023-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                85.2923(6)
_cell_angle_beta                 87.1337(7)
_cell_angle_gamma                85.6362(7)
_cell_formula_units_Z            2
_cell_length_a                   11.63227(10)
_cell_length_b                   13.80526(10)
_cell_length_c                   16.19706(13)
_cell_measurement_reflns_used    36919
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      44.6840
_cell_measurement_theta_min      2.0290
_cell_volume                     2582.23(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_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    -10.00  17.00   0.50    3.00    --   -0.82 101.00 166.12   54
  2  \w    -51.00 -23.00   0.50    3.00    --  -18.00 135.00  91.43   56
  3  \w    -13.00  12.00   0.50    3.00    --   -0.82 102.00  83.16   50
  4  \w    -11.00  15.00   0.50    3.00    --   -0.82 101.00 110.48   52
  5  \w    -11.00  23.00   0.50    3.00    --   -0.82  99.00 158.90   68
  6  \w    -12.00  13.00   0.50    3.00    --   -0.82 102.00  43.89   50
  7  \w      2.00  28.00   0.50    3.00    --   -0.82  96.00 -48.96   52
  8  \w      0.00  27.00   0.50    3.00    --   -0.82  98.00 -79.13   54
  9  \w    -12.00  13.00   0.50    3.00    --   -0.82 102.00-110.84   50
 10  \w      8.00  34.00   0.50    3.00    --   -0.82  68.00 -99.71   52
 11  \w     -6.00  23.00   0.50    3.00    --  -18.00  29.00-153.66   58
 12  \w    -33.00  13.00   0.50    3.00    --   10.00 -25.00-126.25   92
 13  \w    -12.00  18.00   0.50    3.00    --  -18.00  31.00 -39.95   60
 14  \w    -14.00  25.00   0.50    3.00    --  -18.00  29.00  68.72   78
 15  \w    -16.00  28.00   0.50    3.00    --   -6.00  21.00 110.70   88
 16  \w    -24.00   5.00   0.50    3.00    --   -0.82 -94.00 154.15   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0595176000
_diffrn_orient_matrix_UB_12      0.0038132000
_diffrn_orient_matrix_UB_13      0.0056439000
_diffrn_orient_matrix_UB_21      -0.0103240000
_diffrn_orient_matrix_UB_22      -0.0050848000
_diffrn_orient_matrix_UB_23      0.0436172000
_diffrn_orient_matrix_UB_31      0.0099085000
_diffrn_orient_matrix_UB_32      -0.0512960000
_diffrn_orient_matrix_UB_33      -0.0004209000
_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  0.0345
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            80489
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.319
_diffrn_reflns_theta_min         2.023
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.748
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.70a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on Gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics
as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            'clear intense yellow'
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_description       prism
_exptl_crystal_F_000             1324
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.568
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     743
_refine_ls_number_reflns         24306
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+0.1736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21440
_reflns_number_total             24306
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04039e2.cif
_cod_data_source_block           ag560
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Gaussian' was
changed to 'gaussian' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7712442
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C62 H45 F6 Ir N7 O4 S2'
_shelx_estimated_absorpt_t_max   0.898
_shelx_estimated_absorpt_t_min   0.668
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C34(H34A,H34B), C54(H54A,H54B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12),
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24),
  C25(H25), C29(H29), C30(H30), C31(H31), C32(H32), C36(H36), C37(H37),
 C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44), C45(H45), C49(H49),
  C50(H50), C51(H51), C52(H52), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60)
;
_shelx_res_checksum              39217
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.542
_oxdiff_exptl_absorpt_empirical_full_min 0.711