Highly Dispersed Silica-Supported Iridium and Iridium-Aluminium Catalysts for Methane Activation Prepared via Surface Organometallic Chemistry
Escomel, Léon; Abbott, Dan; Mougel, Victor; Veyre, Laurent; Thieuleux, Chloe; Camp, Clément; Chemical Communications  (2022) –; doi:10.1039/D2CC02139K

data_7130282
_publ_section_title
;
 Highly Dispersed Silica-Supported Iridium and Iridium-Aluminium Catalysts
 for Methane Activation Prepared via Surface Organometallic Chemistry
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02139K
_journal_year                    2022
_chemical_formula_moiety         'C32 H47 Al Ir2 O'
_chemical_formula_sum            'C32 H47 Al Ir2 O'
_chemical_formula_weight         859.07
_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
_audit_creation_date             2021-09-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-02-02 deposited with the CCDC.	2022-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.526(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8760(5)
_cell_length_b                   20.4157(9)
_cell_length_c                   18.4320(9)
_cell_measurement_reflns_used    19539
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.3130
_cell_measurement_theta_min      3.1050
_cell_volume                     3333.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4685
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.891
_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    -90.00  31.00   1.00   52.13    --  -10.24 -19.00 120.00  121
  2  \w    -43.00  39.00   1.00   52.13    --  -10.24  77.00-120.00   82
  3  \w    -85.00  14.00   1.00   52.13    --  -10.24 -37.00   0.00   99
  4  \w      1.00  52.00   1.00   52.13    --   11.26 -99.00-180.00   51
  5  \w    -85.00  14.00   1.00   52.13    --  -10.24 -37.00-120.00   99
  6  \w      1.00  39.00   1.00   52.13    --   11.26 -99.00  60.00   38
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0137783000
_diffrn_orient_matrix_UB_12      0.0148526000
_diffrn_orient_matrix_UB_13      -0.0337409000
_diffrn_orient_matrix_UB_21      0.0251174000
_diffrn_orient_matrix_UB_22      0.0289024000
_diffrn_orient_matrix_UB_23      0.0184718000
_diffrn_orient_matrix_UB_31      0.0747374000
_diffrn_orient_matrix_UB_32      -0.0123329000
_diffrn_orient_matrix_UB_33      0.0025552000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44351
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.817
_diffrn_reflns_theta_min         2.797
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.022
_exptl_absorpt_correction_T_max  0.640
_exptl_absorpt_correction_T_min  0.274
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_description       needle
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.058
_refine_diff_density_max         3.323
_refine_diff_density_min         -3.806
_refine_diff_density_rms         0.414
_refine_ls_extinction_coef       0.00236(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         8532
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0767
_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^)+(0.0544P)^2^+173.7456P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1824
_refine_ls_wR_factor_ref         0.2096
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6741
_reflns_number_total             8532
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02139k2.cif
_cod_data_source_block           les494
_cod_database_code               7130282
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C32 H47 Al1 Ir2 O1'
_shelx_estimated_absorpt_t_max   0.653
_shelx_estimated_absorpt_t_min   0.221
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim
C31 \\sim C32: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
3. Rigid body (RIGU) restrains
 C23, C24, C25, C26, C27, C28, C29, C30, C31, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5)
4.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              68972
_olex2_date_sample_data_collection 2021-08-31
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a nylon loop in perfluoroether oil'
_olex2_submission_original_sample_id LES494
_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 1.512
_oxdiff_exptl_absorpt_empirical_full_min 0.670