Acid-base-induced fac → mer isomerization of luminescent iridium(iii) complexes
Yu. Gitlina, Anastasia; Fadaei-Tirani, Farzaneh; Ruggi, Albert; Plaice, Carolina; Severin, Kay; Chemical Science  (2022) –; doi:10.1039/D2SC02808E

data_1567509
_publ_section_title
;
 Acid-base-induced fac \\rightarrow mer isomerization of luminescent
 iridium(iii) complexes
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC02808E
_journal_year                    2022
_chemical_formula_moiety         'C34 H22 F4 Ir N3'
_chemical_formula_sum            'C34 H22 F4 Ir N3'
_chemical_formula_weight         740.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-11-17
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2021-11-17 deposited with the CCDC.	2022-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.8980(14)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.9701(5)
_cell_length_b                   8.77822(19)
_cell_length_c                   18.0310(3)
_cell_measurement_reflns_used    20871
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      75.2040
_cell_measurement_theta_min      2.6010
_cell_volume                     5312.08(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.980
_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     44.00  79.00   0.50    0.50    --   40.00  72.00 -70.70   70
  2  \w     46.00  82.00   0.50    0.50    --   44.00  75.00  68.51   72
  3  \w     48.00  83.00   0.50    0.50    --   44.00  72.00-151.78   70
  4  \w     59.00  94.00   0.50    0.50    --   52.00  64.00 151.95   70
  5  \w     10.00  37.00   0.50    0.50    --   59.56 -30.00  90.00   54
  6  \w   -110.00 -73.00   0.50    0.50    --  -64.00 -50.00 -15.19   74
  7  \w   -115.00 -77.00   0.50    0.50    --  -68.00 -44.00   7.42   76
  8  \w   -116.00 -78.00   0.50    0.50    --  -68.00 -42.00  59.71   76
  9  \w   -114.00 -77.00   0.50    0.50    --  -68.00 -52.00-166.72   74
 10  \w   -115.00 -77.00   0.50    0.50    --  -68.00 -45.00 -55.23   76
 11  \w     32.00  83.00   0.50    1.00    --   71.88 -95.00 -30.00  102
 12  \w     32.00  83.00   0.50    1.00    --   71.88 -95.00 150.00  102
 13  \w   -114.00 -78.00   0.50    0.50    --  -72.00 -65.00 -79.01   72
 14  \w     34.00  84.00   0.50    1.00    --   73.45 -95.00 -60.00  100
 15  \w     34.00  84.00   0.50    1.00    --   73.45 -95.00   0.00  100
 16  \w   -107.00 -30.00   0.50    1.00    --  -75.95 125.00  60.00  154
 17  \w   -107.00 -30.00   0.50    1.00    --  -75.95 125.00-150.00  154
 18  \w   -115.00 -79.00   0.50    1.00    --  -76.55 -74.00-120.21   72
 19  \w   -114.00 -79.00   0.50    1.00    --  -76.55 -75.00  57.11   70
 20  \w   -118.00 -83.00   0.50    1.00    --  -76.55 -66.00 145.35   70
 21  \w   -123.00 -86.00   0.50    1.00    --  -76.55 -49.00 158.90   74
 22  \w   -122.00 -85.00   0.50    1.00    --  -76.55 -52.00 105.73   74
 23  \w     41.00  92.00   0.50    1.00    --   81.22 -95.00-150.00  102
 24  \w     79.00 127.00   0.50    1.00    --   81.22 125.00 150.00   96
 25  \w     79.00 127.00   0.50    1.00    --   81.22 125.00 -60.00   96
 26  \w     41.00  92.00   0.50    1.00    --   81.22 -95.00  90.00  102
 27  \w     35.00 112.00   0.50    1.00    --   81.22-125.00-150.00  154
 28  \w     79.00 127.00   0.50    1.00    --   81.22 125.00-120.00   96
 29  \w     35.00 112.00   0.50    1.00    --   81.22-125.00 120.00  154
 30  \w     79.00 127.00   0.50    1.00    --   81.22 125.00  30.00   96
 31  \w     79.00 127.00   0.50    1.00    --   81.22 125.00   0.00   96
 32  \w     35.00 112.00   0.50    1.00    --   81.22-125.00  30.00  154
 33  \w     35.00 112.00   0.50    1.00    --   81.22-125.00  60.00  154
 34  \w     35.00 112.00   0.50    1.00    --   81.22-125.00 -60.00  154
 35  \w     35.00 112.00   0.50    1.00    --   81.22-125.00 -90.00  154
 36  \w     79.00 127.00   0.50    1.00    --   81.22 125.00  90.00   96
 37  \w     -6.00  21.00   0.50    0.50    --    8.00 100.00 -57.06   54
 38  \w     11.00  40.00   0.50    0.50    --   20.00  92.00  63.14   58
 39  \w     12.00  41.00   0.50    0.50    --   20.00  91.00 159.62   58
 40  \w     15.00  42.00   0.50    0.50    --   20.00  87.00-151.50   54
 41  \w     34.00  70.00   0.50    0.50    --   32.00  76.00 -13.71   72
 42  \w     47.00  83.00   0.50    0.50    --   44.00  74.00 111.77   72
 43  \w     10.00  37.00   0.50    0.50    --   59.56 -30.00  30.00   54
 44  \w   -116.00 -79.00   0.50    0.50    --  -68.00 -40.00-133.38   74
 45  \w   -122.00 -74.00   0.50    1.00    --  -75.95-125.00 -90.00   96
 46  \w   -122.00 -74.00   0.50    1.00    --  -75.95-125.00  60.00   96
 47  \w   -114.00 -78.00   0.50    1.00    --  -76.55 -77.00 -37.17   72
 48  \w     79.00 127.00   0.50    1.00    --   81.22 125.00  60.00   96
;
_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      -0.0259823000
_diffrn_orient_matrix_UB_12      -0.0055018000
_diffrn_orient_matrix_UB_13      0.0628654000
_diffrn_orient_matrix_UB_21      -0.0016694000
_diffrn_orient_matrix_UB_22      -0.1749517000
_diffrn_orient_matrix_UB_23      -0.0058015000
_diffrn_orient_matrix_UB_31      0.0378090000
_diffrn_orient_matrix_UB_32      -0.0114618000
_diffrn_orient_matrix_UB_33      0.0591457000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45625
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.533
_diffrn_reflns_theta_min         2.633
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.238
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.218
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021)
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    1.852
_exptl_crystal_description       plate
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.376
_refine_diff_density_min         -2.012
_refine_diff_density_rms         0.152
_refine_ls_extinction_coef       0.000052(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         5386
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0582P)^2^+46.2447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4613
_reflns_number_total             5386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02808e3.cif
_cod_data_source_block           ag360
_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_original_cell_volume        5312.07(16)
_cod_database_code               1567509
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C34 H22 F4 Ir N3'
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.291
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15), C19(H19), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26),
  C29(H29), C30(H30), C32(H32)
2.b Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C)
;
_shelx_res_checksum              48983
_shelx_hkl_checksum              63175
_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 2.682
_oxdiff_exptl_absorpt_empirical_full_min 0.383