An Ir(ppy)3 encapsulated metal–organic tetrahedral cage for photocatalytic dehydrogenation cross-couplings
Hao, Yang; Yang, Yang; Yang, Fengyu; Shi, Youpeng; Jing, Xu; Duan, Chunying; Chemical Communications 61 (2025) 8576–8579; doi:10.1039/D5CC01206F

data_7134490
_publ_section_title
;
 An Ir(ppy)3 encapsulated metal--organic tetrahedral cage for
 photocatalytic dehydrogenation cross-couplings
;
_journal_issue                   47
_journal_name_full               'Chemical Communications'
_journal_page_first              8576
_journal_page_last               8579
_journal_paper_doi               10.1039/D5CC01206F
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C168 H120 Fe4 N48 O12'
_chemical_formula_sum            'C168 H120 Fe4 N48 O12'
_chemical_formula_weight         3226.51
_space_group_crystal_system      cubic
_space_group_IT_number           218
_space_group_name_Hall           'P -4n 2 3'
_space_group_name_H-M_alt        'P -4 3 n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2024-11-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-01-11 deposited with the CCDC.	2025-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   26.4918(11)
_cell_length_b                   26.4918(11)
_cell_length_c                   26.4918(11)
_cell_measurement_reflns_used    9750
_cell_measurement_temperature    175.00
_cell_measurement_theta_max      53.03
_cell_measurement_theta_min      2.90
_cell_volume                     18592.4(13)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      175.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 VENTURE Metaljet PHOTON II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0922
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            181084
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        53.111
_diffrn_reflns_theta_max         53.111
_diffrn_reflns_theta_min         2.052
_exptl_absorpt_coefficient_mu    1.023
_exptl_absorpt_correction_T_max  0.6898
_exptl_absorpt_correction_T_min  0.5142
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1387 before and 0.1193 after correction.
The Ratio of minimum to maximum transmission is 0.7454.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    0.576
_exptl_crystal_description       block
_exptl_crystal_F_000             3328
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.889
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.46(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         5511
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.235
_refine_ls_R_factor_all          0.1079
_refine_ls_R_factor_gt           0.1063
_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^)+(0.1591P)^2^+25.3051P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2813
_refine_ls_wR_factor_ref         0.2829
_reflns_Friedel_coverage         0.860
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                5409
_reflns_number_total             5511
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01206f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7134490--7134491.cif.'
_cod_original_cell_volume        18592(2)
_cod_database_code               7134490
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.853
_shelx_estimated_absorpt_t_min   0.799
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.54(3)
 0.46(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
3. Restrained distances
 C4-C5
 1.39 with sigma of 0.01
 C4-C3
 1.39 with sigma of 0.01
4. Rigid bond restraints
 N1, C1
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.006
 C5, N1
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.006
 N4, C12
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.006
 C3, C2
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.006
 C8, C9
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.006
 C12, C13
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.006
 C14, C13
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.006
5. Uiso/Uaniso restraints and constraints
Uanis(C12) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C5) \\sim Ueq,
Uanis(C2) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C7) \\sim Ueq, Uanis(N3) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
6.a Aromatic/amide H refined with riding coordinates:
 N4(H4), C1(H1), C2(H2), C3(H3), C4(H4A), C7(H7), C8(H8), C14(H14), C10(H10),
 C11(H11)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              35827
_shelx_hkl_checksum              58601
_shelx_fab_checksum              62693
_olex2_submission_special_instructions 'No special instructions were received'