Metal-Metal Synergy in Well-Defined Surface Tantalum-Iridium Heterobimetallic Catalysts for H/D Exchange Reactions.
Lassalle, Sébastien; Jabbour, Ribal; Schiltz, Pauline; Berruyer, Pierrick; Todorova, Tanya K.; Veyre, Laurent; Gajan, David; Lesage, Anne; Thieuleux, Chloé; Camp, Clément; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b08311

data_4132336
_publ_section_title
;
 Metal-Metal Synergy in Well-Defined Surface Tantalum-Iridium
 Heterobimetallic Catalysts for H/D Exchange Reactions.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b08311
_journal_year                    2019
_chemical_formula_moiety         'C78 H158 Ir2 O16 Si4 Ta2'
_chemical_formula_sum            'C78 H158 Ir2 O16 Si4 Ta2'
_chemical_formula_weight         2210.78
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                94.585(5)
_cell_angle_beta                 95.530(6)
_cell_angle_gamma                105.728(7)
_cell_formula_units_Z            1
_cell_length_a                   9.8249(8)
_cell_length_b                   11.9731(9)
_cell_length_c                   21.9610(11)
_cell_measurement_reflns_used    12196
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      29.0140
_cell_measurement_theta_min      3.1680
_cell_volume                     2459.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4685
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.869
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       \w
_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  0.055
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            43235
_diffrn_reflns_theta_full        26.497
_diffrn_reflns_theta_max         29.687
_diffrn_reflns_theta_min         2.813
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.015
_exptl_absorpt_correction_T_max  0.786
_exptl_absorpt_correction_T_min  0.530
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            yellow
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       nedle
_exptl_crystal_F_000             1110
_exptl_crystal_size_max          0.365
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.117
_refine_diff_density_max         8.98
_refine_diff_density_min         -4.39
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0312
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         12123
_refine_ls_number_restraints     196
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0728
_refine_ls_shift/su_max          0.0013940
_refine_ls_shift/su_mean         0.0000231
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ +73.93P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1864
_refine_ls_wR_factor_gt          0.1659
_refine_ls_wR_factor_ref         0.1864
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                9373
_reflns_number_total             12148
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.28
_oxford_diffrn_Wilson_scale      0.19
_oxford_refine_ls_r_factor_ref   0.0947
_oxford_refine_ls_scale          2.341(19)
_oxford_reflns_number_all        12123
_cod_data_source_file            ja9b08311_si_003.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4132336
_oxdiff_exptl_absorpt_empirical_full_min 0.712
_oxdiff_exptl_absorpt_empirical_full_max 1.939
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxford_refine_reflns_threshold_expression_ref I>-10.0\s(I)