Controlling Selectivity in the Hydroboration of Carbon Dioxide to the Formic Acid, Formaldehyde, and Methanol Oxidation Levels
Espinosa, Matthew R.; Charboneau, David J.; Garcia de Oliveira, André; Hazari, Nilay; ACS Catalysis 9 (2018) 301–; doi:10.1021/acscatal.8b03894

data_4515463
_publ_section_title
;
 Controlling Selectivity in the Hydroboration of Carbon Dioxide to the
 Formic Acid, Formaldehyde, and Methanol Oxidation Levels
;
_journal_issue                   1
_journal_name_full               'ACS Catalysis'
_journal_page_first              301
_journal_paper_doi               10.1021/acscatal.8b03894
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C28 H47 B O8 P2 Pd'
_chemical_formula_sum            'C28 H47 B O8 P2 Pd'
_chemical_formula_weight         690.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     SHELXT
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 108.358(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.0162(11)
_cell_length_b                   11.1134(4)
_cell_length_c                   23.2857(10)
_cell_measurement_reflns_used    24414
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.9060
_cell_measurement_theta_min      1.7410
_cell_volume                     6389.9(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9d (Rigaku OD, 2015)'
_computing_molecular_graphics
; 
 'Rigaku SCX Mini, Rigaku Mercury275R CCD' 
;
_computing_publication_material  'CIFTAB-2014/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 6.8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Mercury275R CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            54827
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_min         2.898
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.726
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76230
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.39.9d (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         7341
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0339P)^2^+13.0295P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0773
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6177
_reflns_number_total             7341
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b03894_si_002.cif
_cod_data_source_block           mini-17066
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4515463
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              15229
_shelx_hkl_checksum              90621