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_1567507
_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         'C69 H48 Ir N3, C H2 Cl2'
_chemical_formula_sum            'C70 H50 Cl2 Ir N3'
_chemical_formula_weight         1196.23
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-07-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-13 deposited with the CCDC.	2022-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                100.2746(8)
_cell_angle_beta                 100.6552(8)
_cell_angle_gamma                105.2857(7)
_cell_formula_units_Z            2
_cell_length_a                   13.85396(12)
_cell_length_b                   14.21567(12)
_cell_length_c                   14.60645(14)
_cell_measurement_reflns_used    45783
_cell_measurement_temperature    139.99(10)
_cell_measurement_theta_max      75.9960
_cell_measurement_theta_min      3.1620
_cell_volume                     2647.62(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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      139.99(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 0.979
_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     49.00  84.00   0.50    0.05    --   46.00  73.00  65.85   70
  2  \w     55.00  85.00   0.50    0.05    --   50.00  69.00  13.24   60
  3  \w     57.00  88.00   0.50    0.05    --   50.00  64.00 -58.95   62
  4  \w     46.00  76.00   0.50    0.05    --   38.00  60.00-147.72   60
  5  \w     10.00  35.00   0.50    0.05    --   59.26 -30.00 -90.00   50
  6  \w     74.00 100.00   0.50    0.05    --   79.85-111.00-120.00   52
  7  \w     39.00 110.00   0.50    0.05    --   83.00-122.00  11.35  142
  8  \w     55.00 101.00   0.50    0.05    --   79.85-111.00  30.00   92
  9  \w     46.00 116.00   0.50    0.05    --   83.00-130.00 170.33  140
 10  \w     68.00 109.00   0.50    0.05    --   83.00-117.00  73.70   82
 11  \w     60.00  99.00   0.50    0.05    --   79.85-111.00  90.00   78
 12  \w     48.00  74.00   0.50    0.05    --   79.85-111.00 -30.00   52
 13  \w     48.00 103.00   0.50    0.05    --   79.85-111.00 -90.00  110
 14  \w     53.00 102.00   0.50    0.05    --   79.85-111.00-150.00   98
 15  \w     69.00 103.00   0.50    0.05    --   79.85-111.00-180.00   68
 16  \w     40.00  87.00   0.50    0.05    --   79.85 -95.00-180.00   94
 17  \w     59.00  86.00   0.50    0.05    --   79.85-111.00 -60.00   54
 18  \w     53.00  78.00   0.50    0.05    --   79.85 -95.00   0.00   50
 19  \w     40.00  78.00   0.50    0.05    --   79.85 -95.00  60.00   76
 20  \w     45.00  82.00   0.50    0.05    --   83.00-108.00 123.11   74
 21  \w     41.00  67.00   0.50    0.05    --   79.85 -95.00 150.00   52
 22  \w     46.00  73.00   0.50    0.05    --   79.85 -95.00  90.00   54
 23  \w     41.00  82.00   0.50    0.05    --   73.26 -95.00  60.00   82
 24  \w     51.00  79.00   0.50    0.05    --   73.26 -93.00 124.00   56
 25  \w     41.00  71.00   0.50    0.05    --   79.85 -95.00  30.00   60
 26  \w     41.00  66.00   0.50    0.05    --   79.85 -93.00 124.00   50
 27  \w     20.00  61.00   0.50    0.05    --   59.26 -93.00 124.00   82
 28  \w     43.00  84.00   0.50    0.05    --   79.85 -95.00 -60.00   82
 29  \w     42.00  79.00   0.50    0.05    --   79.85 -95.00-120.00   74
 30  \w     48.00  74.00   0.50    0.05    --   79.85 -95.00-150.00   52
 31  \w     68.00  94.00   0.50    0.05    --   79.85   0.00-180.00   52
 32  \w     90.00 116.00   0.50    0.05    --   83.00  80.00 -70.18   52
 33  \w     97.00 126.00   0.50    0.05    --   83.00  58.00  -9.51   58
 34  \w     81.00 125.00   0.50    0.05    --   79.85  30.00-120.00   88
 35  \w     82.00 108.00   0.50    0.05    --   70.00  73.00  43.37   52
 36  \w     75.00 101.00   0.50    0.05    --   66.00  74.00 135.62   52
 37  \w     90.00 127.00   0.50    0.05    --   83.00  59.00 165.70   74
 38  \w     83.00 108.00   0.50    0.05    --   79.85  30.00  60.00   50
 39  \w     96.00 121.00   0.50    0.05    --   79.85  30.00  30.00   50
 40  \w     82.00 107.00   0.50    0.05    --   79.85  30.00 -30.00   50
 41  \w     81.00 128.00   0.50    0.05    --   79.85  30.00 -60.00   94
 42  \w     68.00 127.00   0.50    0.05    --   83.00  24.00 -88.72  118
 43  \w     49.00 106.00   0.50    0.05    --   83.00   7.00-143.92  114
 44  \w     83.00 114.00   0.50    0.05    --   79.85   0.00-120.00   62
 45  \w     86.00 115.00   0.50    0.05    --   79.85  15.00 -60.00   58
 46  \w     55.00 102.00   0.50    0.05    --   83.00   6.00  39.13   94
 47  \w     46.00 104.00   0.50    0.05    --   83.00   5.00 123.85  116
 48  \w     63.00 132.00   0.50    0.05    --   83.00  22.00 122.45  138
 49  \w     67.00 120.00   0.50    0.05    --   79.85 178.00 120.00  106
 50  \w     55.00 110.00   0.50    0.05    --   83.00 161.00-120.20  110
 51  \w     94.00 119.00   0.50    0.05    --   79.85 178.00 -60.00   50
 52  \w     16.00  41.00   0.50    0.05    --   18.00  82.00 168.72   50
 53  \w    -66.00 -27.00   0.50    0.05    --  -62.07  93.00-124.00   78
 54  \w    -68.00 -42.00   0.50    0.05    --  -74.55  93.00-124.00   52
 55  \w   -113.00 -63.00   0.50    0.05    --  -79.25 130.00-176.35  100
 56  \w   -114.00 -87.00   0.50    0.05    --  -79.25 132.00-144.94   54
 57  \w   -113.00 -66.00   0.50    0.05    --  -79.25 130.00-114.41   94
 58  \w    -75.00 -32.00   0.50    0.05    --  -75.95 125.00 -90.00   86
 59  \w    -85.00 -60.00   0.50    0.05    --  -75.95  93.00-124.00   50
 60  \w   -106.00 -75.00   0.50    0.05    --  -70.00 -72.00-148.94   62
 61  \w   -122.00 -87.00   0.50    0.05    --  -75.95-125.00-120.00   70
 62  \w   -120.00 -89.00   0.50    0.05    --  -79.25 -58.00-125.26   62
 63  \w   -121.00 -76.00   0.50    0.05    --  -75.95-125.00  30.00   90
 64  \w   -119.00 -89.00   0.50    0.05    --  -79.25 -58.00 133.46   60
 65  \w   -119.00 -80.00   0.50    0.05    --  -79.25-118.00 144.03   78
;
_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      -0.0090127000
_diffrn_orient_matrix_UB_12      -0.0076410000
_diffrn_orient_matrix_UB_13      0.1021539000
_diffrn_orient_matrix_UB_21      0.0676525000
_diffrn_orient_matrix_UB_22      -0.0703629000
_diffrn_orient_matrix_UB_23      0.0003048000
_diffrn_orient_matrix_UB_31      0.0973385000
_diffrn_orient_matrix_UB_32      0.0915457000
_diffrn_orient_matrix_UB_33      0.0422348000
_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  0.0184
_diffrn_reflns_av_unetI/netI     0.0128
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            56071
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.166
_diffrn_reflns_theta_min         3.171
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.173
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.218
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.110a (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 dark orange'
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_description       prism
_exptl_crystal_F_000             1204
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         10852
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0163
_refine_ls_R_factor_gt           0.0161
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0166P)^2^+1.9752P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0401
_refine_ls_wR_factor_ref         0.0402
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10760
_reflns_number_total             10852
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02808e3.cif
_cod_data_source_block           ag281p-2
_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               1567507
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C70 H50 Cl2 Ir N3'
_shelx_estimated_absorpt_t_max   0.790
_shelx_estimated_absorpt_t_min   0.297
_reflns_odcompleteness_completeness 99.36
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
2. Restrained distances
 Cl2A-C70 \\sim Cl2B-C70 \\sim Cl1A-C70 \\sim Cl1B-C70
 with sigma of 0.02
 Cl2A-Cl1A \\sim Cl2B-Cl1B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1A \\sim Cl1B \\sim Cl2A \\sim Cl2B \\sim C70: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01 within 2A
4. Others
 Sof(Cl1B)=Sof(Cl2B)=Sof(H70C)=Sof(H70D)=1-FVAR(1)
 Sof(Cl1A)=Sof(Cl2A)=Sof(H70A)=Sof(H70B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C70(H70C,H70D), C70(H70A,H70B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C10(H10), C11(H11), C13(H13),
 C14(H14), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23),
  C24(H24), C25(H25), C26(H26), C27(H27), C31(H31), C33(H33), C34(H34),
 C36(H36), C37(H37), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44), C45(H45),
  C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C54(H54), C56(H56),
 C57(H57), C59(H59), C60(H60), C62(H62), C63(H63), C65(H65), C66(H66), C67(H67),
  C68(H68), C69(H69)
;
_shelx_res_checksum              66030
_shelx_hkl_checksum              90407
_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 1.487
_oxdiff_exptl_absorpt_empirical_full_min 0.780