Pd-Catalyzed CO/Vinyl Arene Copolymerization: when the Stereochemistry is Controlled by the Comonomer
Dall’Anese, Anna; Fiorindo, Mattia; Olivieri, Diego; Carfagna, Carla; Balducci, Gabriele; Alessio, Enzo; Durand, Jérôme; Milani, Barbara; Macromolecules 53 (2020) 7783–7794; doi:10.1021/acs.macromol.0c01461

data_1559045
_publ_section_title
;
 Pd-Catalyzed CO/Vinyl Arene Copolymerization: when the Stereochemistry is
 Controlled by the Comonomer
;
_journal_issue                   18
_journal_name_full               Macromolecules
_journal_page_first              7783
_journal_page_last               7794
_journal_paper_doi               10.1021/acs.macromol.0c01461
_journal_volume                  53
_journal_year                    2020
_chemical_formula_moiety         'C17 H15 Cl N2 Pd, C H2 Cl2'
_chemical_formula_sum            'C18 H17 Cl3 N2 Pd'
_chemical_formula_weight         474.08
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.516(10)
_cell_length_b                   12.357(4)
_cell_length_c                   19.840(5)
_cell_measurement_reflns_used    12139
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.649
_cell_measurement_theta_min      1.912
_cell_volume                     1843(3)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_data_reduction        'XDS - CCP4'
_computing_molecular_graphics    'Ortep3 for Windows'
_computing_publication_material  'private software'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.988
_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  0.0728
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            30973
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         28.649
_diffrn_reflns_theta_min         1.912
_diffrn_source                   'Elettra Synchrotron - XRD1 BL'
_exptl_absorpt_coefficient_mu    1.366
_exptl_absorpt_correction_T_max  1.147
_exptl_absorpt_correction_T_min  0.813
_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_density_diffrn    1.709
_exptl_crystal_description       needle
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.863
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details
;
 Flack x determined using 2006 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.059(15)
_refine_ls_extinction_coef       0.0081(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         4908
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0493P)^2^+0.8696P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0860
_reflns_Friedel_coverage         0.759
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                4710
_reflns_number_total             4908
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma0c01461_si_004.cif
_cod_data_source_block           hss7-05
_cod_depositor_comments
'Adding full bibliography for 1559040--1559045.cif.'
_cod_database_code               1559045
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.726
_shelx_estimated_absorpt_t_max   0.875
_shelx_res_checksum              6038
_shelx_hkl_checksum              28679