Synthesis, Structure, and Catalysis of Palladium Complexes Bearing a Group 13 Metalloligand: Remarkable Effect of an Aluminum-Metalloligand in Hydrosilylation of CO<sub>2</sub>.
Takaya, Jun; Iwasawa, Nobuharu; Journal of the American Chemical Society 139 (2017) 6074–6077; doi:10.1021/jacs.7b02553

data_4131273
_publ_section_title
;
 Synthesis, Structure, and Catalysis of Palladium Complexes Bearing a
 Group 13 Metalloligand: Remarkable Effect of an Aluminum-Metalloligand in
 Hydrosilylation of CO<sub>2</sub>.
;
_journal_issue                   17
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6074
_journal_page_last               6077
_journal_paper_doi               10.1021/jacs.7b02553
_journal_volume                  139
_journal_year                    2017
_chemical_formula_sum            'C43 H37 Al2 Cl6 N3 O P2'
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_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
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_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
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_cell_angle_beta                 111.526(6)
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_cell_formula_units_Z            4
_cell_length_a                   15.9914(9)
_cell_length_b                   17.7499(7)
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_cell_measurement_reflns_used    12138
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.3190
_cell_measurement_theta_min      1.9310
_cell_volume                     4310.6(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0806
_diffrn_reflns_av_unetI/netI     0.0666
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
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_diffrn_reflns_limit_k_min       -21
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_diffrn_reflns_number            44110
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
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_exptl_absorpt_coefficient_mu    0.553
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84863
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       prism
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.703
_refine_diff_density_min         -1.264
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         7592
_refine_ls_number_restraints     24
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_refine_ls_R_factor_all          0.1553
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1634P)^2^+22.9022P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2686
_refine_ls_wR_factor_ref         0.3170
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4904
_reflns_number_total             7592
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02553_si_002.cif
_cod_data_source_block           2a_PAlP
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4131273
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.942
_shelx_estimated_absorpt_t_max   0.994
_shelx_res_checksum              69295
_shelx_hkl_checksum              13985