Acrylate formation from CO2 and ethylene: catalysis with palladium and mechanistic insight
S. Chantal E. Stieber; Nuria Huguet; Takeharu Kageyama; Ivana Jevtovikj; Piyal Ariyananda; Alvaro Gordillo; Stephan A. Schunk; Frank Rominger; Peter Hofmann; Michael Limbach; Chem.Commun. 51 (2015) 10907–; doi:10.1039/C5cc01932J

data_7117378
_publ_section_title
;
 Acrylate formation from CO2 and ethylene: catalysis with palladium and
 mechanistic insight
;
_journal_name_full               Chem.Commun.
_journal_page_first              10907
_journal_paper_doi               10.1039/C5cc01932J
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C39 H56 F2 O4 P2 Pd'
_chemical_formula_weight         795.17
_chemical_name_common            'additional structure'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-02-20 deposited with the CCDC.
2015-06-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.717(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.3557(15)
_cell_length_b                   17.2752(14)
_cell_length_c                   27.490(2)
_cell_measurement_reflns_used    3138
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      23.96
_cell_measurement_theta_min      2.29
_cell_volume                     7893.8(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.584
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1229
_diffrn_reflns_av_unetI/netI     0.0962
_diffrn_reflns_Laue_measured_fraction_full 0.584
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            44695
_diffrn_reflns_point_group_measured_fraction_full 0.584
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         20.905
_diffrn_reflns_theta_min         1.410
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.598
_exptl_absorpt_correction_T_max  0.9705
_exptl_absorpt_correction_T_min  0.8244
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2008). <i>SADABS</i>. University of G\"ottingen, Germany.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       plate
_exptl_crystal_F_000             3328
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.940
_refine_diff_density_min         -1.033
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         8348
_refine_ls_number_restraints     1460
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1376
_refine_ls_R_factor_gt           0.0936
_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^)+(0.0543P)^2^+94.8364P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1907
_refine_ls_wR_factor_ref         0.2158
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5631
_reflns_number_total             8348
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc01932j2.cif
_cod_data_source_block           cst17
_cod_original_cell_volume        7893.7(11)
_cod_database_code               7117378
_shelx_estimated_absorpt_t_min   0.860
_shelx_estimated_absorpt_t_max   0.976
_shelxl_version_number           2014-1
_shelx_res_checksum              72773
_shelx_hkl_checksum              75563