A redox-switchable catalyst with an ‘unplugged’ redox tag
Gutiérrez-Peña, Cristian L.; Poyatos, Macarena; Peris, Eduardo; Chemical Communications  (2022) –; doi:10.1039/D2CC02497G

data_7130627
_publ_section_title
;
 A redox-switchable catalyst with an &#x2018;unplugged&#x2019; redox tag
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02497G
_journal_year                    2022
_chemical_formula_moiety         'C56 H54 Cl2 Ir2 N6 O4, 2(C H Cl3)'
_chemical_formula_sum            'C58 H56 Cl8 Ir2 N6 O4'
_chemical_formula_weight         1569.08
_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
_audit_creation_date             2022-02-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-03 deposited with the CCDC.	2022-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.392(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.1313(9)
_cell_length_b                   18.4166(6)
_cell_length_c                   16.7444(5)
_cell_measurement_reflns_used    14658
_cell_measurement_temperature    200.1(9)
_cell_measurement_theta_max      71.6000
_cell_measurement_theta_min      3.8400
_cell_volume                     8051.2(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.1(9)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4051
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     -5.00  39.00   0.40   10.00    --  -41.12  19.00-120.00  110
  2  \w    -22.00  33.20   0.40   10.00    --  -41.12  38.00 -90.00  138
  3  \w     -5.00  39.00   0.40   10.00    --  -41.12  19.00-180.00  110
  4  \w     -5.00  39.00   0.40   10.00    --  -41.12  19.00  60.00  110
  5  \w     -5.00  39.00   0.40   10.00    --  -41.12  19.00 120.00  110
  6  \w     -5.00  39.00   0.40   10.00    --  -41.12  19.00 150.00  110
  7  \w     -5.00  39.00   0.40   10.00    --  -41.12  19.00-150.00  110
  8  \w     -5.00  39.00   0.40   10.00    --  -41.12  19.00  90.00  110
  9  \w      8.00  42.00   0.40   10.00    --   41.12  81.00-156.46   85
 10  \w      6.00  32.00   0.40   10.00    --   41.12  85.00 -94.64   65
 11  \w      6.00  32.00   0.40   10.00    --   41.12  85.00-171.89   65
 12  \w     61.00 130.20   0.40   10.00    --   41.12 178.00 120.00  173
 13  \w     77.00 176.20   0.40   30.00    --  102.61  45.00   0.00  248
 14  \w     20.00 106.00   0.40   30.00    --  102.61 -94.00-120.00  215
 15  \w     30.00  72.00   0.40   30.00    --  102.61 -45.00-150.00  105
 16  \w    103.00 178.20   0.40   30.00    --  102.61  77.00-180.00  188
 17  \w     30.00  93.20   0.40   30.00    --  102.61 -61.00 120.00  158
 18  \w     30.00  72.00   0.40   30.00    --  102.61 -45.00 150.00  105
 19  \w     74.00 175.20   0.40   30.00    --  102.61  61.00 -60.00  253
 20  \w     30.00  93.20   0.40   30.00    --  102.61 -61.00   0.00  158
 21  \w     26.00  56.80   0.40   30.00    --  102.61 -30.00  30.00   77
 22  \w     72.00 176.00   0.40   30.00    --  102.61  68.00  35.27  260
 23  \w     20.00 106.00   0.40   30.00    --  102.61 -94.00-180.00  215
 24  \w     74.00 175.20   0.40   30.00    --  102.61  58.00-132.47  253
 25  \w     29.00 113.00   0.40   30.00    --  102.61-125.00 150.00  210
 26  \w     74.00 175.20   0.40   30.00    --  102.61  61.00 -80.14  253
 27  \w     -5.00  39.00   0.40   10.00    --  -41.12  19.00 -30.00  110
 28  \w      4.00  30.00   0.40   10.00    --   41.12  89.00  25.99   65
 29  \w      6.00  32.00   0.40   10.00    --   41.12  85.00 146.38   65
 30  \w      6.00  32.00   0.40   10.00    --   41.12  85.00  96.89   65
;
_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      0.0175534000
_diffrn_orient_matrix_UB_12      -0.0699896000
_diffrn_orient_matrix_UB_13      -0.0411485000
_diffrn_orient_matrix_UB_21      0.0182471000
_diffrn_orient_matrix_UB_22      -0.0310082000
_diffrn_orient_matrix_UB_23      0.0818119000
_diffrn_orient_matrix_UB_31      -0.0532699000
_diffrn_orient_matrix_UB_32      -0.0336764000
_diffrn_orient_matrix_UB_33      0.0102157000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            40535
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.599
_diffrn_reflns_theta_max         66.599
_diffrn_reflns_theta_min         3.903
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.053
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.809
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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 yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       prism
_exptl_crystal_F_000             3072
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.049
_refine_diff_density_max         1.779
_refine_diff_density_min         -1.314
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         7102
_refine_ls_number_restraints     351
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0577
_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^)+(0.1162P)^2^+51.5788P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1894
_refine_ls_wR_factor_ref         0.2028
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5431
_reflns_number_total             7102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02497g2.cif
_cod_data_source_block           str2206_sq
_cod_database_code               7130627
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C56 H58 Cl2 Ir2 N6 O4'
_shelx_estimated_absorpt_t_max   0.665
_shelx_estimated_absorpt_t_min   0.293
_diffrn_oxdiff_digest_frames
;
010782dd2459811f28ca789e70355d3d9a04734554f
;
_diffrn_oxdiff_digest_hkl
;
014326cf410436260da9c4d35814d57f06dcff
;
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: Cl2(0.5) Cl4(0.5) Cl3(0.5) C30(0.5) H30(0.5) Cl6(0.5) Cl5(0.5)
 Cl7(0.5) C29(0.5) H29(0.5)
4.a Ternary CH refined with riding coordinates:
 C3(H3), C7(H7), C2(H2), C6(H6), C30(H30), C29(H29)
4.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C21(H21A,H21B), C8(H8A,H8B), C12(H12A,H12B), C20(H20A,H20B),
 C5(H5A,H5B), C4(H4A,H4B), C9(H9A,H9B)
4.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C15(H15), C27(H27), C14(H14), C18(H18), C16(H16), C17(H17)
;
_shelx_res_checksum              58580
_shelx_hkl_checksum              83475
_shelx_fab_checksum              71973
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 6.366
_oxdiff_exptl_absorpt_empirical_full_min 0.489