Highly efficient vinylic addition polymerization of 5-vinyl-2-norbornene using benzylic palladium complexes as precatalysts
Pérez-Ortega, Ignacio; Albéniz, Ana C.; Polymer Chemistry 12 (2021) 5963–5969; doi:10.1039/D1PY01165K

data_1564891
_publ_section_title
;
 Highly efficient vinylic addition polymerization of 5-vinyl-2-norbornene
 using benzylic palladium complexes as precatalysts
;
_journal_issue                   41
_journal_name_full               'Polymer Chemistry'
_journal_page_first              5963
_journal_page_last               5969
_journal_paper_doi               10.1039/D1PY01165K
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C32 H12 B F24, C34 H44 F5 N P Pd, C H2 Cl2'
_chemical_formula_sum            'C67 H58 B Cl2 F29 N P Pd'
_chemical_formula_weight         1647.22
_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             2021-08-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-27 deposited with the CCDC.	2021-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                84.761(4)
_cell_angle_beta                 70.245(4)
_cell_angle_gamma                89.960(4)
_cell_formula_units_Z            2
_cell_length_a                   13.4173(7)
_cell_length_b                   15.6707(7)
_cell_length_c                   18.5278(8)
_cell_measurement_reflns_used    7179
_cell_measurement_temperature    298
_cell_measurement_theta_max      25.6440
_cell_measurement_theta_min      3.9050
_cell_volume                     3649.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.0
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.814
_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    -35.00  62.00   1.00    6.66    --  -10.64  57.00 -90.00   97
  2  \w    -77.00  17.00   1.00    6.66    --  -10.64 -57.00 120.00   94
  3  \w     35.00 101.00   1.00    6.66    --   12.51 178.00 120.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0703
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.814
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25676
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.814
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.619
_diffrn_reflns_theta_min         3.416
_exptl_absorpt_coefficient_mu    0.463
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.256
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45g (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       block
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.89
_exptl_crystal_size_mid          0.772
_exptl_crystal_size_min          0.485
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1199
_refine_ls_number_reflns         16741
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0513P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1345
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10550
_reflns_number_total             16741
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1py01165k2.cif
_cod_data_source_block           4-BArF4
_cod_depositor_comments
'Adding full bibliography for 1564891--1564892.cif.'
_cod_database_code               1564891
_shelx_shelxl_version_number     2014/7
_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. Restrained distances
 C67B-Cl2
 1.6 with sigma of 0.02
3. Others
 Sof(F15A)=Sof(F16A)=Sof(F17A)=1-FVAR(1)
 Sof(F16)=Sof(F15)=Sof(F17)=FVAR(1)
 Sof(F9A)=Sof(F10A)=Sof(F11A)=1-FVAR(2)
 Sof(F9)=Sof(F10)=Sof(F11)=FVAR(2)
 Sof(F6A)=Sof(F7A)=Sof(F8A)=1-FVAR(3)
 Sof(F6)=Sof(F7)=Sof(F8)=FVAR(3)
 Sof(F27A)=Sof(F28A)=Sof(F29A)=1-FVAR(4)
 Sof(F27)=Sof(F28)=Sof(F29)=FVAR(4)
 Sof(F21A)=Sof(F22A)=Sof(F23A)=1-FVAR(5)
 Sof(F21)=Sof(F22)=Sof(F23)=FVAR(5)
 Sof(F18A)=Sof(F19A)=Sof(F20A)=1-FVAR(6)
 Sof(F18)=Sof(F19)=Sof(F20)=FVAR(6)
 Sof(F24A)=Sof(F25A)=Sof(F26A)=1-FVAR(7)
 Sof(F24)=Sof(F25)=Sof(F26)=FVAR(7)
 Sof(Cl1)=Sof(Cl2)=Sof(C67B)=Sof(H67A)=Sof(H67B)=1-FVAR(8)
 Sof(Cl1A)=Sof(Cl2A)=Sof(C67A)=Sof(H67C)=Sof(H67D)=FVAR(8)
 Fixed Sof: F12A(0.25) F13A(0.25) F14A(0.25) N1B(0.5) C33B(0.5) C34B(0.5)
 H34A(0.5) H34B(0.5) H34C(0.5) N1A(0.5) F12(0.75) F13(0.75) F14(0.75) C33A(0.5)
 C34A(0.5) H34D(0.5) H34E(0.5) H34F(0.5)
4.a Ternary CH refined with riding coordinates:
 C7(H7), C15(H15), C21(H21), C27(H27)
4.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B),
 C20(H20A,H20B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
  C26(H26A,H26B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,
 H31B), C32(H32A,H32B), C67B(H67A,H67B), C67A(H67C,H67D)
4.c Aromatic/amide H refined with riding coordinates:
 C36(H36), C39(H39), C42(H42), C44(H44), C47(H47), C50(H50), C52(H52),
 C55(H55), C58(H58), C60(H60), C63(H63), C66(H66), C2(H2), C3(H3), C4(H4),
 C5(H5), C6(H6)
4.d Idealised Me refined as rotating group:
 C34B(H34A,H34B,H34C), C34A(H34D,H34E,H34F)
;
_shelx_res_checksum              66108
_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
;