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_4132339
_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         'C40 H76 Ir2 Ta2'
_chemical_formula_sum            'C40 H76 Ir2 Ta2'
_chemical_formula_weight         1303.38
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 94.102(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4502(10)
_cell_length_b                   18.8905(9)
_cell_length_c                   15.8769(9)
_cell_measurement_reflns_used    12391
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      32.7640
_cell_measurement_theta_min      3.5920
_cell_volume                     4322.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.924
_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  0.048
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35405
_diffrn_reflns_theta_full        30.830
_diffrn_reflns_theta_max         33.036
_diffrn_reflns_theta_min         3.043
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.206
_exptl_absorpt_correction_T_max  0.172
_exptl_absorpt_correction_T_min  0.076
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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    2.003
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.374
_exptl_crystal_size_mid          0.281
_exptl_crystal_size_min          0.245
_refine_diff_density_max         3.06
_refine_diff_density_min         -3.34
_refine_ls_extinction_coef       51(2)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0174
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         7539
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.0016613
_refine_ls_shift/su_mean         0.0000324
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.276E+04 0.431E+04 0.260E+04 0.109E+04 164. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0986
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0986
_reflns_limit_h_max              21
_reflns_limit_h_min              -22
_reflns_limit_k_max              28
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                6616
_reflns_number_total             7549
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.27
_oxford_diffrn_Wilson_scale      1.37
_oxford_refine_ls_r_factor_ref   0.0474
_oxford_refine_ls_scale          1.133(4)
_oxford_reflns_number_all        7539
_cod_data_source_file            ja9b08311_si_005.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               4132339
_oxdiff_exptl_absorpt_empirical_full_min 0.892
_oxdiff_exptl_absorpt_empirical_full_max 1.134
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)