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_1567510
_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         'C33 H25 Ir N3, C2 F6 N O4 S2, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C35.5 H26 Cl F6 Ir N4 O4 S2'
_chemical_formula_weight         978.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-06 deposited with the CCDC.	2022-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.6080(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.8756(2)
_cell_length_b                   12.70840(9)
_cell_length_c                   20.40752(14)
_cell_measurement_reflns_used    57568
_cell_measurement_temperature    140.01(10)
_cell_measurement_theta_max      76.5360
_cell_measurement_theta_min      3.2230
_cell_volume                     6995.75(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.105a (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, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_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    -83.00  -1.00   1.00    1.00    --  -43.01 119.00 136.00   82
  2  \w    -87.00 -62.00   1.00    1.00    --  -43.01-156.00-104.00   25
  3  \w     58.00  90.00   1.00    1.00    --   43.01-119.00  51.00   32
  4  \w     58.00  83.00   1.00    1.00    --   43.01-156.00-104.00   25
  5  \w     50.00  75.00   1.00    4.00    --  112.00-119.00  51.00   25
  6  \w    134.00 160.00   1.00    4.00    --  112.00 156.00 -68.00   26
  7  \w     64.00  89.00   1.00    4.00    --  112.00-156.00-104.00   25
  8  \w     86.00 117.00   1.00    4.00    --  112.00 156.00 -68.00   31
  9  \w    119.00 145.00   1.00    4.00    --  112.00 119.00 136.00   26
 10  \w   -117.00 -24.00   1.00    1.00    --  -43.01 -37.00  90.00   93
 11  \w   -117.00 -20.00   1.00    1.00    --  -43.01 -37.00   0.00   97
 12  \w    -89.00 -64.00   1.00    1.00    --  -43.01 156.00 -68.00   25
 13  \w      6.00  63.00   1.00    1.00    --   43.01 -99.00 -30.00   57
 14  \w     75.00 101.00   1.00    1.00    --   43.01  37.00 -60.00   26
 15  \w     21.00  63.00   1.00    1.00    --   43.01  37.00 -60.00   42
 16  \w     37.00 109.00   1.00    4.00    --  112.00-111.00   0.00   72
 17  \w    105.00 177.00   1.00    4.00    --  112.00  77.00 120.00   72
 18  \w    106.00 155.00   1.00    4.00    --  112.00 111.00  60.00   49
 19  \w    110.00 139.00   1.00    4.00    --  112.00 111.00 120.00   29
 20  \w     29.00  75.00   1.00    4.00    --  112.00 -94.00  90.00   46
 21  \w     80.00 107.00   1.00    4.00    --  112.00 -94.00  90.00   27
 22  \w     82.00 107.00   1.00    4.00    --  112.00 -94.00 -30.00   25
 23  \w    110.00 177.00   1.00    4.00    --  112.00 111.00 -90.00   67
 24  \w     84.00 177.00   1.00    4.00    --  112.00  30.00-150.00   93
 25  \w     95.00 137.00   1.00    4.00    --  112.00 -45.00   0.00   42
 26  \w     36.00  88.00   1.00    4.00    --  112.00-111.00  60.00   52
 27  \w     65.00 109.00   1.00    4.00    --  112.00-111.00 -90.00   44
 28  \w    112.00 156.00   1.00    4.00    --  112.00  77.00  90.00   44
 29  \w     64.00 107.00   1.00    4.00    --  112.00-111.00 150.00   43
 30  \w     37.00  94.00   1.00    4.00    --  112.00-111.00-120.00   57
 31  \w    148.00 173.00   1.00    4.00    --  112.00 111.00 120.00   25
 32  \w     59.00 109.00   1.00    4.00    --  112.00-111.00  90.00   50
 33  \w     39.00 138.00   1.00    4.00    --  112.00 -45.00 120.00   99
 34  \w    118.00 144.00   1.00    4.00    --  112.00 111.00 150.00   26
 35  \w     40.00  65.00   1.00    4.00    --  112.00 -94.00 -30.00   25
 36  \w     84.00 109.00   1.00    4.00    --  112.00-111.00-150.00   25
 37  \w     95.00 120.00   1.00    4.00    --  112.00  45.00  60.00   25
 38  \w    129.00 169.00   1.00    4.00    --  112.00  45.00  60.00   40
 39  \w     40.00  96.00   1.00    4.00    --  112.00 -94.00 -60.00   56
 40  \w     37.00 107.00   1.00    4.00    --  112.00-111.00 -60.00   70
 41  \w     41.00  66.00   1.00    4.00    --  112.00 -45.00   0.00   25
 42  \w     84.00 135.00   1.00    4.00    --  112.00 178.00-150.00   51
 43  \w    105.00 177.00   1.00    4.00    --  112.00  45.00-120.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0036851000
_diffrn_orient_matrix_UB_12      0.1145602000
_diffrn_orient_matrix_UB_13      0.0253637000
_diffrn_orient_matrix_UB_21      -0.0565242000
_diffrn_orient_matrix_UB_22      0.0024408000
_diffrn_orient_matrix_UB_23      -0.0087581000
_diffrn_orient_matrix_UB_31      0.0073237000
_diffrn_orient_matrix_UB_32      -0.0394056000
_diffrn_orient_matrix_UB_33      0.0732863000
_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  0.0383
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            81444
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.610
_diffrn_reflns_theta_min         3.845
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.913
_exptl_absorpt_correction_T_max  0.661
_exptl_absorpt_correction_T_min  0.083
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.105a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear intense yellow'
_exptl_crystal_density_diffrn    1.858
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             3832
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.564
_refine_diff_density_min         -1.299
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     964
_refine_ls_number_reflns         14600
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+6.6529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0761
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14192
_reflns_number_total             14600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02808e3.cif
_cod_data_source_block           ag163
_cod_original_formula_sum        'C35.50 H26 Cl F6 Ir N4 O4 S2'
_cod_database_code               1567510
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C35.50 H26 Cl F6 Ir N4 O4 S2'
_shelx_estimated_absorpt_t_max   0.383
_shelx_estimated_absorpt_t_min   0.103
_reflns_odcompleteness_completeness 99.81
_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) groups
2.a Secondary CH2 refined with riding coordinates:
 C60(HY,HZ)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H), C2(HA), C3(HB), C4(HC), C7(HD), C8(HE), C9(HF), C10(HG), C12(HH),
 C13(HI), C14(HJ), C15(HK), C18(HL), C19(HM), C20(HN), C21(HO), C22(HP),
 C23(HQ), C24(HR), C25(HS), C26(HT), C29(HU), C30(HV), C31(HW), C32(HX),
 C34(H34), C35(H35), C36(H36), C37(H37), C40(H40), C41(H41), C42(H42), C43(H43),
  C45(H45), C46(H46), C47(H47), C48(H48), C51(H51), C52(H52), C53(H53),
 C54(H54), C55(H55), C62(H62), C63(H63), C64(H64), C65(H65), C67(H67), C68(H68),
  C69(H69), C70(H70)
;
_shelx_res_checksum              60664
_shelx_hkl_checksum              46900
_olex2_date_sample_data_collection 2021-04-26
_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 3.093
_oxdiff_exptl_absorpt_empirical_full_min 0.523