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_4131274
_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            'C45 H41 Cl6 Ga2 N3 O1.5 P2'
_chemical_formula_weight         1061.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2ya'
_space_group_name_H-M_alt        'P 1 a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 106.315(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2505(6)
_cell_length_b                   18.0456(6)
_cell_length_c                   16.4190(8)
_cell_measurement_reflns_used    9138
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.7340
_cell_measurement_theta_min      2.5430
_cell_volume                     4621.0(3)
_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 0.997
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0834
_diffrn_reflns_av_unetI/netI     0.1076
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35225
_diffrn_reflns_point_group_measured_fraction_full 0.710
_diffrn_reflns_point_group_measured_fraction_max 0.671
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.257
_exptl_absorpt_coefficient_mu    1.622
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94239
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       prism
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details
;
 Flack x determined using 2374 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.517(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1072
_refine_ls_number_reflns         14266
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0680P)^2^+1.0417P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1285
_refine_ls_wR_factor_ref         0.1484
_reflns_Friedel_coverage         0.345
_reflns_Friedel_fraction_full    0.420
_reflns_Friedel_fraction_max     0.344
_reflns_number_gt                9877
_reflns_number_total             14266
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02553_si_002.cif
_cod_data_source_block           2b_PGaP
_cod_original_sg_symbol_H-M      Pa
_cod_original_formula_sum        'C45 H41 Cl6 Ga2 N3 O1.50 P2'
_cod_database_code               4131274
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.707
_shelx_estimated_absorpt_t_max   0.968
_shelx_res_checksum              14742
_shelx_hkl_checksum              1051