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_1550337
_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            'C31 H38 Cl2 O5 P S'
_chemical_formula_weight         624.54
_space_group_crystal_system      hexagonal
_space_group_IT_number           170
_space_group_name_Hall           'P 65'
_space_group_name_H-M_alt        'P 65'
_symmetry_space_group_name_Hall  'P 65'
_symmetry_space_group_name_H-M   'P 65'
_atom_sites_solution_hydrogens   mixed
_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                120
_cell_formula_units_Z            6
_cell_length_a                   22.6855(8)
_cell_length_b                   22.6855(8)
_cell_length_c                   10.7563(7)
_cell_measurement_reflns_used    4824
_cell_measurement_temperature    185(2)
_cell_measurement_theta_max      19.7500
_cell_measurement_theta_min      2.6096
_cell_volume                     4793.9(4)
_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  0.0598
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            24765
_diffrn_reflns_point_group_measured_fraction_full 0.890
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        24.987
_diffrn_reflns_theta_max         24.987
_diffrn_reflns_theta_min         1.795
_exptl_absorpt_coefficient_mu    0.356
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       block
_exptl_crystal_F_000             1974
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
;
 Flack x determined using 1463 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.05(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         5002
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.934
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          0.059
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1187P)^2^+2.4333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1592
_reflns_Friedel_coverage         0.682
_reflns_Friedel_fraction_full    0.766
_reflns_Friedel_fraction_max     0.766
_reflns_number_gt                4358
_reflns_number_total             5002
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8py01568f2.cif
_cod_data_source_block           1_sq
_cod_depositor_comments
'Adding full bibliography for 1550337--1550338.cif.'
_cod_original_cell_volume        4793.9(5)
_cod_database_code               1550337
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.895
_shelx_estimated_absorpt_t_max   0.972
_shelx_res_checksum              40568
_shelx_fab_checksum              78172