Boosting photocatalytic efficiency of iridium polypyridyl complex in coupling reaction through the induction of ferrocene: insights into bimetallic catalysis
Gayen, Firdaus Rahaman; Chawla, Sakshi; Bora, Debashree; Borkotoky, Lodsna; Gazi, Sarifuddin; Mallick, Dibyendu; Maurya, Ram Awatar; De, Arijit Kumar; Saha, Biswajit; Catalysis Science & Technology 14 (2024) 3618–3628; doi:10.1039/D3CY01418E

data_1571723
_publ_section_title
;
 Boosting photocatalytic efficiency of iridium polypyridyl complex in
 coupling reaction through the induction of ferrocene: insights into
 bimetallic catalysis
;
_journal_issue                   13
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              3618
_journal_page_last               3628
_journal_paper_doi               10.1039/D3CY01418E
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C42 H32 Fe Ir N4, F6 P'
_chemical_formula_sum            'C42 H32 F6 Fe Ir N4 P'
_chemical_formula_weight         985.73
_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     iterative
_audit_creation_date             2022-08-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-10-18 deposited with the CCDC.	2024-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.0980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.71160(10)
_cell_length_b                   14.07180(10)
_cell_length_c                   15.44540(10)
_cell_measurement_reflns_used    29528
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      68.1100
_cell_measurement_theta_min      2.6460
_cell_volume                     3611.62(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.115a (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 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_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     14.00 109.00   0.50    0.20    --   40.33  77.00-150.00  190
  2  \w     14.00 109.00   0.50    0.20    --   40.33  77.00  60.00  190
  3  \w     14.00 109.00   0.50    0.20    --   40.33  77.00  90.00  190
  4  \w     14.00 109.00   0.50    0.20    --   40.33  77.00 120.00  190
  5  \w     14.00 109.00   0.50    0.20    --   40.33  77.00 150.00  190
  6  \w     25.00 111.00   0.50    0.20    --   40.33  25.00  60.00  172
  7  \w     82.00 167.00   0.50    0.55    --   96.67  25.00-150.00  170
  8  \w     99.00 164.00   0.50    0.55    --   96.67 117.00 -67.00  130
  9  \w     99.00 164.00   0.50    0.55    --   96.67 117.00 -30.00  130
 10  \w    105.00 170.00   0.50    0.55    --   96.67  96.00   0.00  130
 11  \w     81.00 164.00   0.50    0.55    --   96.67 145.00 120.00  166
 12  \w     80.00 163.00   0.50    0.55    --   96.67  42.00  90.00  166
 13  \w    -35.00  24.00   0.50    0.20    --   40.33 -12.00  90.00  118
 14  \w     29.00  68.00   0.50    0.55    --   96.67 -59.00  30.00   78
 15  \w     29.00  68.00   0.50    0.55    --   96.67 -59.00-120.00   78
 16  \w     30.00  57.00   0.50    0.55    --   96.67 -50.00-150.00   54
 17  \w     29.00  68.00   0.50    0.55    --   96.67 -59.00-150.00   78
 18  \w     28.00 105.00   0.50    0.55    --   96.67 -77.00-180.00  154
 19  \w     29.00  68.00   0.50    0.55    --   96.67 -59.00 -90.00   78
 20  \w     30.00  57.00   0.50    0.55    --   96.67 -50.00   0.00   54
 21  \w     30.00  57.00   0.50    0.55    --   96.67 -50.00  30.00   54
 22  \w     30.00  57.00   0.50    0.55    --   96.67 -50.00  60.00   54
 23  \w     30.00  57.00   0.50    0.55    --   96.67 -50.00  90.00   54
 24  \w     52.00 137.00   0.50    0.55    --   96.67-162.00  55.00  170
 25  \w     30.00 109.00   0.50    0.55    --   96.67-117.00  30.00  158
 26  \w     44.00 127.00   0.50    0.55    --   96.67-145.00 -30.00  166
 27  \w     30.00 109.00   0.50    0.55    --   96.67-117.00-154.00  158
 28  \w     30.00 109.00   0.50    0.55    --   96.67-117.00-180.00  158
 29  \w     52.00 113.00   0.50    0.20    --   40.33-162.00  55.00  122
 30  \w    -47.00 -15.00   0.50    0.55    --  -82.50  42.00-180.00   64
 31  \w     28.00  86.00   0.50    0.20    --   40.33-117.00-154.00  116
 32  \w     18.00  79.00   0.50    0.20    --   40.33-104.00  60.00  122
 33  \w    -47.00 -15.00   0.50    0.55    --  -82.50  42.00 -60.00   64
 34  \w    -47.00 -15.00   0.50    0.55    --  -82.50  42.00 -30.00   64
 35  \w    -24.00  35.00   0.50    0.20    --  -40.33  12.00 -60.00  118
 36  \w    -56.00  26.00   0.50    0.20    --  -40.33  50.00-120.00  164
 37  \w    -43.00  26.00   0.50    0.20    --  -40.33  38.00 -30.00  138
 38  \w    -31.00  30.00   0.50    0.20    --  -40.33  25.00  60.00  122
 39  \w    -63.00  27.00   0.50    0.20    --  -40.33  64.00  90.00  180
 40  \w   -112.00 -31.00   0.50    0.20    --  -40.33 162.00  83.00  162
 41  \w    -84.00  -6.00   0.50    0.20    --  -40.33 117.00 -67.00  156
 42  \w   -109.00 -13.00   0.50    0.20    --  -40.33 -77.00 -60.00  192
 43  \w   -107.00 -21.00   0.50    0.20    --  -40.33 -50.00 -60.00  172
 44  \w   -108.00 -17.00   0.50    0.20    --  -40.33 -64.00-150.00  182
 45  \w   -109.00 -13.00   0.50    0.20    --  -40.33 -77.00 -90.00  192
 46  \w   -109.00 -13.00   0.50    0.20    --  -40.33 -77.00   0.00  192
 47  \w   -108.00 -17.00   0.50    0.20    --  -40.33 -64.00 150.00  182
 48  \w   -150.00 -69.00   0.50    0.55    --  -82.50 -33.00  30.00  162
 49  \w   -149.00 -78.00   0.50    0.55    --  -82.50-117.00-154.00  142
 50  \w   -110.00 -48.00   0.50    0.20    --  -40.33-162.00  55.00  124
 51  \w   -141.00 -48.00   0.50    0.55    --  -82.50-162.00  55.00  186
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0947
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            42163
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.354
_diffrn_reflns_theta_min         2.659
_exptl_absorpt_coefficient_mu    11.270
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25041
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.115a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark brown'
_exptl_crystal_density_diffrn    1.813
_exptl_crystal_description       block
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.961
_refine_diff_density_min         -1.567
_refine_diff_density_rms         0.127
_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     496
_refine_ls_number_reflns         6569
_refine_ls_number_restraints     538
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+4.8854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0925
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6003
_reflns_number_total             6569
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cy01418e2.cif
_cod_data_source_block           frg4_128
_cod_depositor_comments          'Adding full bibliography for 1571723.cif.'
_cod_database_code               1571723
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.430
_shelx_estimated_absorpt_t_min   0.103
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12),
 C13(H13), C14(H14), C15(H15), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23),
  C24(H24), C25(H25), C26(H26), C29(H29), C30(H30), C32(H32), C34(H34),
 C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42)
;
_shelx_res_checksum              75564
_shelx_hkl_checksum              15028
_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
;