Sterically very bulky aliphatic/aromatic phosphine-sulfonate palladium catalysts for ethylene polymerization and copolymerization with polar monomers
Xia, Jian; Zhang, Yixin; Hu, Xiaoqiang; Ma, Xin; Cui, Lei; Zhang, Jianfu; Jian, Zhongbao; Polymer Chemistry 10 (2019) 546–; doi:10.1039/C8PY01568F

data_1550338
_publ_section_title
;
 Sterically very bulky aliphatic/aromatic phosphine-sulfonate palladium
 catalysts for ethylene polymerization and copolymerization with polar
 monomers
;
_journal_issue                   4
_journal_name_full               'Polymer Chemistry'
_journal_page_first              546
_journal_paper_doi               10.1039/C8PY01568F
_journal_volume                  10
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_sum            'C34 H38 F2 N O3 P Pd S'
_chemical_formula_weight         716.08
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-09-29 deposited with the CCDC.
2018-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1697(6)
_cell_length_b                   9.5203(6)
_cell_length_c                   36.333(2)
_cell_measurement_reflns_used    2276
_cell_measurement_temperature    185(2)
_cell_measurement_theta_max      19.6671
_cell_measurement_theta_min      2.2114
_cell_volume                     3171.8(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      185(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0751
_diffrn_reflns_av_unetI/netI     0.0869
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            16352
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.211
_exptl_absorpt_coefficient_mu    0.749
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            transparent
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_description       plate
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Flack x determined using 1553 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    'riding mode'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5595
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0369P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0898
_reflns_Friedel_coverage         0.745
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4534
_reflns_number_total             5595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8py01568f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1550337--1550338.cif.'
_cod_original_cell_volume        3171.9(4)
_cod_database_code               1550338
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.801
_shelx_estimated_absorpt_t_max   0.964
_shelx_res_checksum              18972