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_4132337
_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         'C38 H50 Ir O Ta'
_chemical_formula_sum            'C38 H50 Ir O Ta'
_chemical_formula_weight         895.93
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                63.368(2)
_cell_angle_beta                 83.6700(10)
_cell_angle_gamma                85.9320(10)
_cell_formula_units_Z            4
_cell_length_a                   11.3629(2)
_cell_length_b                   18.5429(4)
_cell_length_c                   18.9187(3)
_cell_measurement_reflns_used    34438
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      37.6740
_cell_measurement_theta_min      3.6100
_cell_volume                     3540.51(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9897
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.951
_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     25.00  76.00   1.00    5.00    --   36.98 -99.00  60.00   51
  2  \w     10.00  86.00   1.00    5.00    --   36.98  77.00-180.00   76
  3  \w     11.00  65.00   1.00    5.00    --   36.98 -99.00 -30.00   54
  4  \w     62.00 102.00   1.00    5.00    --   36.98 178.00-150.00   40
  5  \w     -6.00  76.00   1.00    5.00    --   36.98 -99.00 -90.00   82
  6  \w     10.00 108.00   1.00    5.00    --   36.98  19.00  90.00   98
  7  \w     -2.00  86.00   1.00    5.00    --   36.98   0.00  30.00   88
  8  \w     20.00 102.00   1.00    5.00    --   36.98  57.00 -90.00   82
  9  \w     45.00  71.00   1.00    5.00    --   36.98 178.00  30.00   26
 10  \w      1.00  26.00   1.00    5.00    --   36.98  93.00 141.96   25
 11  \w     10.00  67.00   1.00    5.00    --   36.98  77.00 -30.00   57
 12  \w      2.00  28.00   1.00    5.00    --   36.98  92.00-101.39   26
 13  \w    -33.00  59.00   1.00    5.00    --   36.98 -19.00 -30.00   92
 14  \w      6.00  68.00   1.00    5.00    --   36.98 -99.00-180.00   62
 15  \w     17.00  99.00   1.00    5.00    --   36.98  19.00-180.00   82
 16  \w     52.00  78.00   1.00    5.00    --   36.98 178.00 -60.00   26
 17  \w     10.00  60.00   1.00    5.00    --   36.98  77.00  60.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0434335000
_diffrn_orient_matrix_UB_12      -0.0168310000
_diffrn_orient_matrix_UB_13      0.0325739000
_diffrn_orient_matrix_UB_21      0.0160905000
_diffrn_orient_matrix_UB_22      -0.0391617000
_diffrn_orient_matrix_UB_23      0.0038085000
_diffrn_orient_matrix_UB_31      0.0424434000
_diffrn_orient_matrix_UB_32      -0.0039112000
_diffrn_orient_matrix_UB_33      0.0264060000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            130323
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.822
_diffrn_reflns_theta_min         3.395
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.869
_exptl_absorpt_correction_T_max  0.386
_exptl_absorpt_correction_T_min  0.061
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_description       plate
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.276
_exptl_crystal_size_mid          0.242
_exptl_crystal_size_min          0.099
_refine_diff_density_max         2.643
_refine_diff_density_min         -1.782
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     761
_refine_ls_number_reflns         36218
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0197P)^2^+4.8936P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0808
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27488
_reflns_number_total             36218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08311_si_004.cif
_cod_data_source_block           psc49
_cod_database_code               4132337
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C38 H48 Ir1 O1 Ta1'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.23
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C29 \\sim C33: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
3. Rigid body (RIGU) restrains
 C29, C33
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C24(H24A,H24B), C57(H57A,H57B), C62(H62A,H62B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C41(H41), C42(H42), C43(H43),
  C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C52(H52), C53(H53),
 C54(H54), C55(H55), C56(H56)
4.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C),
 C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C64(H64A,H64B,
 H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C72(H72A,H72B,H72C), C73(H73A,
 H73B,H73C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C)
;
_shelx_res_checksum              81965
_shelx_hkl_checksum              15492
_olex2_date_sample_data_collection 2019-06-12
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a nylon loop oil'
_olex2_submission_original_sample_id PSC49
_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 1.315
_oxdiff_exptl_absorpt_empirical_full_min 0.675