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_1559044
_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         'C22 H19 Cl N2 Pd'
_chemical_formula_sum            'C22 H19 Cl N2 Pd'
_chemical_formula_weight         853.24
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.939(4)
_cell_length_b                   10.6180(17)
_cell_length_c                   38.547(5)
_cell_measurement_reflns_used    35056
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.083
_cell_measurement_theta_min      1.041
_cell_volume                     3658.7(18)
_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'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution
'SHELXT (Sheldrick, 2015), Sir2014 (Burla, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.980
_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  0.0896
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            61073
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         29.083
_diffrn_reflns_theta_min         1.041
_diffrn_source                   'Elettra Synchrotron - XRD1 BL'
_exptl_absorpt_coefficient_mu    1.106
_exptl_absorpt_correction_T_max  1.622
_exptl_absorpt_correction_T_min  0.724
_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            orange
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_description       plate
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.563
_refine_diff_density_min         -1.031
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       0.0153(5)
_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   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         5031
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0668P)^2^+3.0864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1053
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5004
_reflns_number_total             5031
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma0c01461_si_005.cif
_cod_data_source_block           mf10-05
_cod_depositor_comments
;
Adding full bibliography for 1559040--1559045.cif.

2022-09-17
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C176 H152 Cl8 N16 Pd8'
_cod_original_formula_weight         3625.93
_cod_original_formula_units_Z            1
_cod_database_code               1559044
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.769
_shelx_estimated_absorpt_t_max   0.897
_shelx_res_checksum              54146
_shelx_hkl_checksum              35997