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_7117377
_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            'C31.5 H56 O2 P2 Pd'
_chemical_formula_weight         635.10
_chemical_name_common            '5 in manuscript'
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 118.016(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.266(2)
_cell_length_b                   13.8216(11)
_cell_length_c                   18.2436(14)
_cell_measurement_reflns_used    2712
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.99
_cell_measurement_theta_min      2.28
_cell_volume                     6292.2(8)
_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 0.952
_diffrn_measured_fraction_theta_max 0.986
_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  0.0800
_diffrn_reflns_av_unetI/netI     0.0737
_diffrn_reflns_Laue_measured_fraction_full 0.952
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24383
_diffrn_reflns_point_group_measured_fraction_full 0.952
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.908
_diffrn_reflns_theta_min         1.862
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.717
_exptl_absorpt_correction_T_max  0.9437
_exptl_absorpt_correction_T_min  0.8593
_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    1.341
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5417
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0135P)^2^+27.2464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0956
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3960
_reflns_number_total             5417
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc01932j2.cif
_cod_data_source_block           cst23
_cod_original_cell_volume        6292.2(9)
_cod_original_formula_sum        'C31.50 H56 O2 P2 Pd'
_cod_database_code               7117377
_shelx_estimated_absorpt_t_min   0.888
_shelx_estimated_absorpt_t_max   0.932
_shelxl_version_number           2014-3
_shelx_res_checksum              58570
_shelx_hkl_checksum              37127