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_7117376
_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            'C30 H58 P2 Pd'
_chemical_formula_weight         587.10
_chemical_name_common            '3 in manuscript'
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 101.0818(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1923(13)
_cell_length_b                   16.4379(19)
_cell_length_c                   16.7601(19)
_cell_measurement_reflns_used    3941
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.63
_cell_measurement_theta_min      2.23
_cell_volume                     3026.0(6)
_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 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0265
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11216
_diffrn_reflns_point_group_measured_fraction_full 0.930
_diffrn_reflns_point_group_measured_fraction_max 0.875
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.688
_diffrn_reflns_theta_min         2.230
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.735
_exptl_absorpt_correction_T_max  0.8672
_exptl_absorpt_correction_T_min  0.8082
_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    1.289
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
; 
 Flack x determined using 2558 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.002(15)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         6847
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0167P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0605
_reflns_Friedel_coverage         0.751
_reflns_friedel_fraction_full    0.860
_reflns_friedel_fraction_max     0.751
_reflns_number_gt                6422
_reflns_number_total             6847
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc01932j2.cif
_cod_data_source_block           cst18
_cod_database_code               7117376
_shelx_estimated_absorpt_t_min   0.832
_shelx_estimated_absorpt_t_max   0.910
_shelxl_version_number           2014-3
_shelx_res_checksum              8532
_shelx_hkl_checksum              11547