Tunable “In-Chain” and “At the End of the Branches” Methyl Acrylate Incorporation in the Polyolefin Skeleton through Pd(II) Catalysis
Alberoni, Chiara; D’Alterio, Massimo C.; Balducci, Gabriele; Immirzi, Barbara; Polentarutti, Maurizio; Pellecchia, Claudio; Milani, Barbara; ACS Catalysis 12 (2022) 3430–3443; doi:10.1021/acscatal.1c05326

data_4519376
_publ_section_title
;
 Tunable &#x201C;In-Chain&#x201D; and &#x201C;At the End of the
 Branches&#x201D; Methyl Acrylate Incorporation in the Polyolefin Skeleton
 through Pd(II) Catalysis
;
_journal_issue                   6
_journal_name_full               'ACS Catalysis'
_journal_page_first              3430
_journal_page_last               3443
_journal_paper_doi               10.1021/acscatal.1c05326
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C32 H36 N3 Pd S, F6 P'
_chemical_formula_sum            'C32 H36 F6 N3 P Pd S'
_chemical_formula_weight         746.07
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 109.5400(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.3000(19)
_cell_length_b                   10.543(3)
_cell_length_c                   15.816(2)
_cell_measurement_reflns_used    23027
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.227
_cell_measurement_theta_min      2.097
_cell_volume                     3190.0(10)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_data_reduction        'XDS - CCP4'
_computing_molecular_graphics
;
ShelXle (Hubschle et al. 2011)
Coot (Emsley et al., 2010) 
Ortep3 for Windows (Farrugia, 2012)
;
_computing_publication_material  'private software, PLATON (Spek, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution
'SHELXT (Sheldrick, 2015), Sir2014 (Burla, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
;
Huber 4-circles Kappa Goniometer, Pilatus 2M detector
;
_diffrn_measurement_method       'Rotating crystal'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            75730
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         28.227
_diffrn_reflns_theta_min         2.097
_diffrn_source                   'Elettra Synchrotron - XRD1 BL'
_exptl_absorpt_coefficient_mu    0.720
_exptl_absorpt_correction_T_max  1.138
_exptl_absorpt_correction_T_min  0.848
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
        Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
        Cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       thin_plate
_exptl_crystal_F_000             1520
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CD2Cl2/hexane'
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.894
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details
;
 Flack x determined using 4072 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.057(2)
_refine_ls_extinction_coef       0.0091(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         8238
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0238
_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^)+(0.0483P)^2^+1.6952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0649
_reflns_Friedel_coverage         0.996
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                8217
_reflns_number_total             8238
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c05326_si_003.cif
_cod_data_source_block           dmr5-05
_cod_original_cell_volume        3190.0(11)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4519376
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.813
_shelx_estimated_absorpt_t_max   0.869
_shelx_res_checksum              17216
_shelx_hkl_checksum              41666