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_1564892
_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         'C34 H44 F5 N P Pd, B F4'
_chemical_formula_sum            'C34 H44 B F9 N P Pd'
_chemical_formula_weight         785.88
_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   mixed
_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                109.041(6)
_cell_angle_beta                 91.911(6)
_cell_angle_gamma                107.037(5)
_cell_formula_units_Z            2
_cell_length_a                   10.3004(6)
_cell_length_b                   13.2588(7)
_cell_length_c                   16.2684(14)
_cell_measurement_reflns_used    3209
_cell_measurement_temperature    298
_cell_measurement_theta_max      23.4530
_cell_measurement_theta_min      3.6960
_cell_volume                     1987.5(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 0.992
_diffrn_measured_fraction_theta_max 0.818
_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  63.00   1.00   26.45    --  -10.48  57.00 -90.00   98
  2  \w    -75.00  15.00   1.00   26.45    --  -10.48 -57.00 120.00   90
  3  \w     34.00 100.00   1.00   26.45    --   12.36-178.00 120.00   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  0.0374
_diffrn_reflns_av_unetI/netI     0.0892
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.818
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13942
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.818
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.534
_diffrn_reflns_theta_min         3.433
_exptl_absorpt_coefficient_mu    0.571
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.367
_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    1.313
_exptl_crystal_description       block
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.362
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.111
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         9092
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0547
_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^)+(0.0383P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1218
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5689
_reflns_number_total             9092
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1py01165k2.cif
_cod_data_source_block           4-BF4
_cod_depositor_comments
'Adding full bibliography for 1564891--1564892.cif.'
_cod_original_cell_volume        1987.5(2)
_cod_database_code               1564892
_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
 F13A-F12A
 2 with sigma of 0.02
3. Others
 Fixed Sof: F11A(0.5) F11B(0.5) F12A(0.5) F12B(0.5) F13A(0.5) F13B(0.5)
4.a Ternary CH refined with riding coordinates:
 C7(H7), C17(H17), C23(H23), C29(H29)
4.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B),
 C22(H22A,H22B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B),
  C28(H28A,H28B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,
 H33B), C34(H34A,H34B)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
4.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C)
;
_shelx_res_checksum              97845
_shelx_fab_checksum              73651
_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
;