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_1567508
_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         'C23 H17 N'
_chemical_formula_sum            'C23 H17 N'
_chemical_formula_weight         307.38
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-06-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-10 deposited with the CCDC.	2022-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.986(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.7468(11)
_cell_length_b                   5.5397(4)
_cell_length_c                   7.8676(5)
_cell_measurement_reflns_used    1539
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.8520
_cell_measurement_theta_min      4.8760
_cell_volume                     769.26(9)
_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      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_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   -113.00 -21.00   1.00   10.00    --  -43.01 -36.00   4.00   92
  2  \w     20.00 118.00   1.00   10.00    --   43.01  36.00 160.00   98
  3  \w     17.00  44.00   1.00   10.00    --   43.01 -36.00   4.00   27
  4  \w     89.00 128.00   1.00   40.00    --  107.38 -36.00   4.00   39
  5  \w    100.00 175.00   1.00   40.00    --  107.38  36.00 160.00   75
  6  \w     54.00  81.00   1.00   40.00    --  107.38 -36.00   4.00   27
  7  \w    -64.00 -39.00   1.00   10.00    --  -43.01  36.00 160.00   25
  8  \w    -16.00   9.00   1.00   10.00    --  -43.01  36.00 160.00   25
  9  \w    -61.00  -7.00   1.00   10.00    --  -43.01 125.00-150.00   54
 10  \w     29.00  98.00   1.00   10.00    --   43.01-125.00 -30.00   69
 11  \w     53.00  80.00   1.00   10.00    --   43.01-125.00-180.00   27
 12  \w     51.00 108.00   1.00   40.00    --  107.38-111.00 -60.00   57
 13  \w     94.00 123.00   1.00   40.00    --  107.38 178.00 -60.00   29
 14  \w     26.00  90.00   1.00   40.00    --  107.38 -94.00-120.00   64
 15  \w     39.00  66.00   1.00   40.00    --  107.38 -94.00  60.00   27
 16  \w    108.00 170.00   1.00   40.00    --  107.38 111.00  90.00   62
 17  \w     81.00 106.00   1.00   40.00    --  107.38 -94.00  60.00   25
 18  \w     31.00 105.00   1.00   40.00    --  107.38 -94.00   0.00   74
 19  \w     44.00 109.00   1.00   40.00    --  107.38-111.00-180.00   65
 20  \w    105.00 145.00   1.00   40.00    --  107.38 111.00 -30.00   40
 21  \w    105.00 178.00   1.00   40.00    --  107.38 111.00-150.00   73
 22  \w     80.00 177.00   1.00   40.00    --  107.38  61.00  30.00   97
 23  \w    116.00 149.00   1.00   40.00    --  107.38 111.00  60.00   33
 24  \w    112.00 153.00   1.00   40.00    --  107.38  77.00  60.00   41
;
_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      -0.0686389000
_diffrn_orient_matrix_UB_12      -0.0218379000
_diffrn_orient_matrix_UB_13      -0.1362539000
_diffrn_orient_matrix_UB_21      0.0263889000
_diffrn_orient_matrix_UB_22      -0.2542220000
_diffrn_orient_matrix_UB_23      -0.0466164000
_diffrn_orient_matrix_UB_31      -0.0470689000
_diffrn_orient_matrix_UB_32      -0.1105051000
_diffrn_orient_matrix_UB_33      0.1342285000
_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  0.0430
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            5478
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.999
_diffrn_reflns_theta_min         5.012
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.585
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.635
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_description       plate
_exptl_crystal_F_000             324
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1527
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1139P)^2^+0.1838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1775
_refine_ls_wR_factor_ref         0.2065
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1032
_reflns_number_total             1527
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02808e3.cif
_cod_data_source_block           ag239ae
_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        769.26(8)
_cod_database_code               1567508
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C23 H17 N'
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.835
_reflns_odcompleteness_completeness 99.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{N1, C1}
3. Uiso/Uaniso restraints and constraints
Uanis(N1) = Uanis(C1)
4. Others
 Fixed Sof: N1(0.5) C1(0.5) H1(0.5) H2A(0.5) H2B(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2A), C2(H2B), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C11(H11),
 C12(H12)
;
_shelx_res_checksum              66146
_shelx_hkl_checksum              37532
_olex2_date_sample_data_collection 2021-06-11
_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 1.745
_oxdiff_exptl_absorpt_empirical_full_min 0.654