Fast and Regioselective Polymerization of para-Alkoxystyrene by Palladium Catalysts for Precision Production of High-Molecular-Weight Polystyrene Derivatives
Liao, Guangfu; Xiao, Zefan; Chen, Xiaolin; Du, Cheng; Zhong, Liu; Cheung, Chi Shing; Gao, Haiyang; Macromolecules  (2019) –; doi:10.1021/acs.macromol.9b02274

data_1556732
_publ_section_title
;
 Fast and Regioselective Polymerization of para-Alkoxystyrene by Palladium
 Catalysts for Precision Production of High-Molecular-Weight Polystyrene
 Derivatives
;
_journal_name_full               Macromolecules
_journal_paper_doi               10.1021/acs.macromol.9b02274
_journal_year                    2019
_chemical_formula_moiety         'C29 H23 Cl N2 Pd, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C29.5 H24 Cl2 N2 Pd'
_chemical_formula_weight         583.81
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-23
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                95.854(2)
_cell_angle_beta                 90.584(2)
_cell_angle_gamma                110.370(2)
_cell_formula_units_Z            4
_cell_length_a                   12.1104(3)
_cell_length_b                   13.4886(3)
_cell_length_c                   16.6398(4)
_cell_measurement_reflns_used    11831
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.6340
_cell_measurement_theta_min      3.8680
_cell_volume                     2531.84(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXD (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -82.00  -2.00   1.00   12.50    --  -40.84 125.00 -30.00   80
  2  \w   -115.00 -18.00   1.00   12.50    --  -40.84 -73.00 -78.00   97
  3  \w   -109.00 -15.00   1.00   12.50    --  -40.84 -37.00 150.00   94
  4  \w    -94.00 -21.00   1.00   12.50    --  -40.84 -37.00  60.00   73
  5  \w     52.00  88.00   1.00   12.50    --   40.84-125.00-120.00   36
  6  \w    141.00 168.00   1.00   40.00    --  108.22  45.00-180.00   27
  7  \w     35.00 135.00   1.00   40.00    --  108.22 -61.00 -90.00  100
  8  \w     57.00 137.00   1.00   40.00    --  108.22 -77.00  30.00   80
  9  \w     49.00 106.00   1.00   40.00    --  108.22 -94.00   0.00   57
 10  \w     34.00  71.00   1.00   40.00    --  108.22 -45.00 150.00   37
 11  \w     86.00 139.00   1.00   40.00    --  108.22  45.00-120.00   53
 12  \w     83.00 118.00   1.00   40.00    --  108.22  45.00-180.00   35
 13  \w     31.00 135.00   1.00   40.00    --  108.22 -30.00   0.00  104
 14  \w     24.00  64.00   1.00   40.00    --  108.22 -94.00 -90.00   40
 15  \w     72.00 108.00   1.00   40.00    --  108.22 -94.00 -90.00   36
 16  \w     49.00 122.00   1.00   40.00    --  108.22-125.00-150.00   73
 17  \w     50.00  89.00   1.00   40.00    --  108.22 -94.00-120.00   39
 18  \w     25.00 161.00   1.00   40.00    --  108.22 -15.00-150.00  136
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0413289000
_diffrn_orient_matrix_UB_12      0.0857398000
_diffrn_orient_matrix_UB_13      0.0733215000
_diffrn_orient_matrix_UB_21      0.1294088000
_diffrn_orient_matrix_UB_22      0.0166719000
_diffrn_orient_matrix_UB_23      -0.0179112000
_diffrn_orient_matrix_UB_31      0.0016878000
_diffrn_orient_matrix_UB_32      0.0860462000
_diffrn_orient_matrix_UB_33      -0.0546415000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17864
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.879
_diffrn_reflns_theta_min         3.518
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.009
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            bronze
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_description       block
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.528
_refine_diff_density_min         -1.767
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         9958
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+2.0527P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1032
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9097
_reflns_number_total             9958
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma9b02274_si_002.cif
_cod_data_source_block           18031902
_cod_original_cell_volume        2531.83(11)
_cod_original_formula_sum        'C29.50 H24 Cl2 N2 Pd'
_cod_database_code               1556732
_chemical_oxdiff_formula         'C H N Pd'
_chemical_oxdiff_usercomment     dbb-h-Ca
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C32(H1AA), C3(H8AA), C39(H3BA), C10(H1DA)
2.b Secondary CH2 refined with riding coordinates:
 C59(H8FA,H8FB)
2.c Aromatic/amide H refined with riding coordinates:
 C34(H9AA), C37(H4BA), C27(H1CA), C44(H2CA), C57(H3CA), C53(H4CA), C47(H6CA),
 C24(H8CA), C41(H9CA), C28(H0DA), C51(H2DA), C25(H3DA), C13(H4DA), C18(H5DA),
 C42(H6DA), C12(H7DA), C7(H8DA), C15(H9DA), C35(H0EA), C8(H1EA), C43(H2EA),
 C5(H3EA), C56(H4EA), C14(H5EA), C36(H6EA), C26(H7EA), C6(H8EA), C55(H9EA),
 C50(H0FA), C54(H1FA), C22(H2FA), C49(H3FA), C48(H4FA), C19(H5FA), C21(H6FA),
 C20(H7FA)
2.d Idealised Me refined as rotating group:
 C58(H6AA,H6AB,H6AC), C29(H7CA,H7CB,H7CC)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 7.732
_oxdiff_exptl_absorpt_empirical_full_min 0.486