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_4131276
_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            'C39 H29 Al Cl3 N3 P2 Pd'
_chemical_formula_weight         841.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 104.8729(12)
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_cell_length_a                   23.6164(3)
_cell_length_b                   22.6680(3)
_cell_length_c                   36.3526(4)
_cell_measurement_reflns_used    82215
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.5140
_cell_measurement_theta_min      2.1460
_cell_volume                     18808.9(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       47
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_diffrn_reflns_number            230487
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.948
_exptl_absorpt_coefficient_mu    0.678
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97810
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       prism
_exptl_crystal_F_000             6784
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1765
_refine_ls_number_reflns         43233
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+4.5335P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1174
_reflns_Friedel_coverage         0.000
_reflns_number_gt                30824
_reflns_number_total             43233
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02553_si_002.cif
_cod_data_source_block           3a_PAlPPd
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               4131276
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.948
_shelx_estimated_absorpt_t_max   0.967
_shelx_res_checksum              52278
_shelx_hkl_checksum              86451
_shelx_fab_checksum              154