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_1567512
_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_absolute_configuration rmad
_chemical_formula_moiety         'C33 H24 Ir N3, 1[CH2Cl2]'
_chemical_formula_sum            'C33 H24 Ir N3'
_chemical_formula_weight         654.75
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-10-26
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2021-10-27 deposited with the CCDC.	2022-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.72023(11)
_cell_length_b                   9.72023(11)
_cell_length_c                   30.5949(5)
_cell_measurement_reflns_used    42711
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      40.8350
_cell_measurement_theta_min      2.1820
_cell_volume                     2890.69(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.118a (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 0.935
_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    -11.00  30.00   0.50    2.00    --   -0.80  19.00   0.00   82
  2  \w    -34.00  32.00   0.50    2.00    --   12.00 -22.00  95.25  132
  3  \w      2.00  40.00   0.50    2.00    --   -0.80  19.00 150.00   76
  4  \w    -13.00  26.00   0.50    2.00    --  -12.00  29.00 -41.51   78
  5  \w     -5.00  48.00   0.50    2.00    --   -0.80  26.00 -65.61  106
  6  \w    -18.00  32.00   0.50    2.00    --   -0.80  23.00-156.07  100
  7  \w      8.00  33.00   0.50    2.00    --   -0.80  87.00 -89.66   50
  8  \w    -16.00   9.00   0.50    2.00    --   -0.80 102.00-178.94   50
  9  \w     -6.00  33.00   0.50    2.00    --   -0.80  93.00 -53.80   78
 10  \w     -9.00  32.00   0.50    2.00    --   -0.80  93.00  59.24   82
 11  \w    -42.00  38.00   0.50    2.00    --   -0.80  -2.00 -71.15  160
 12  \w    -23.00  12.00   0.50    2.00    --   -0.80 -10.00-159.84   70
;
_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      -0.0129113000
_diffrn_orient_matrix_UB_12      -0.0716444000
_diffrn_orient_matrix_UB_13      0.0007547000
_diffrn_orient_matrix_UB_21      0.0444254000
_diffrn_orient_matrix_UB_22      -0.0060184000
_diffrn_orient_matrix_UB_23      0.0183327000
_diffrn_orient_matrix_UB_31      -0.0566026000
_diffrn_orient_matrix_UB_32      0.0116150000
_diffrn_orient_matrix_UB_33      0.0141768000
_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  0.0786
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            99418
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         41.261
_diffrn_reflns_theta_min         2.198
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.643
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.593
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.118a (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 orange'
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_description       plate
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.032
_refine_diff_density_max         1.810
_refine_diff_density_min         -2.757
_refine_diff_density_rms         0.133
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.070(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         8678
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0257P)^2^+3.0334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0720
_reflns_Friedel_coverage         0.668
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.845
_reflns_number_gt                6667
_reflns_number_total             8678
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02808e3.cif
_cod_data_source_block           ag347
_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        2890.70(8)
_cod_database_code               1567512
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C33 H24 Ir N3'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.930(11)
 0.070(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Shared sites
{N2, C2}
4. Restrained distances
 Ir1-N2 \\sim Ir1-C2
 with sigma of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(N2) = Uanis(C2)
6. Others
 Fixed Sof: N2(0.5) C2(0.5) H14(0.5) H14A(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C14(H14A), C15(H15), C16(H16), C17(H17)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              4308
_shelx_hkl_checksum              67958
_shelx_fab_checksum              52308
_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 1.590
_oxdiff_exptl_absorpt_empirical_full_min 0.751