Enhanced mechanical properties of acrylate and 5-vinyl-2-norbornene-based ethylene terpolymers: rational design and synthesis using remotely modulated phosphine–sulfonate palladium complexes
Li, Yong-Qing; Cao, Gui-Ping; Cao, Yu-Cai; Polymer Chemistry 15 (2024) 4662–4672; doi:10.1039/D4PY00722K

data_1572946
_publ_section_title
;
 Enhanced mechanical properties of acrylate and 5-vinyl-2-norbornene-based
 ethylene terpolymers: rational design and synthesis using remotely
 modulated phosphine--sulfonate palladium complexes
;
_journal_issue                   45
_journal_name_full               'Polymer Chemistry'
_journal_page_first              4662
_journal_page_last               4672
_journal_paper_doi               10.1039/D4PY00722K
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C38 H34 N O5 P Pd S'
_chemical_formula_sum            'C38 H34 N O5 P Pd S'
_chemical_formula_weight         754.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-03-01
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-03-21 deposited with the CCDC.	2024-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.00(3)
_cell_angle_beta                 91.10(3)
_cell_angle_gamma                90.00(3)
_cell_formula_units_Z            8
_cell_length_a                   17.077(3)
_cell_length_b                   19.687(4)
_cell_length_c                   20.582(4)
_cell_measurement_reflns_used    6108
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      22.53
_cell_measurement_theta_min      2.24
_cell_volume                     6918(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      193.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1963
_diffrn_reflns_av_unetI/netI     0.1011
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            129338
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.017
_diffrn_reflns_theta_min         1.851
_diffrn_source_current           40.0
_diffrn_source_power             1.8
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.687
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6224
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1287 before and 0.0904 after correction.
The Ratio of minimum to maximum transmission is 0.8349.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_F_000             3092
_refine_diff_density_max         13.877
_refine_diff_density_min         -1.597
_refine_diff_density_rms         0.521
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.438
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     853
_refine_ls_number_reflns         15116
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.438
_refine_ls_R_factor_all          0.3259
_refine_ls_R_factor_gt           0.1906
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3829
_refine_ls_wR_factor_ref         0.4786
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6014
_reflns_number_total             15116
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4py00722k2.cif
_cod_data_source_block           1_a
_cod_depositor_comments
;
Adding full bibliography for 1572945--1572946.cif.

2025-06-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C76 H69 N2 O10 P2 Pd2 S2'
_cod_original_formula_weight         1509.19
_cod_original_formula_moiety         '2(C38 H34 N O5 P Pd S)'
_cod_original_formula_units_Z            4
_cod_database_code               1572946
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00J(H00J), C00K(H00K), C00P(H00P), C00Q(H00Q), C00T(H00T), C00W(H00W),
 C00Y(H00Y), C00Z(H00Z), C010(H010), C011(H011), C013(H013), C014(H014),
 C015(H015), C017(H017), C018(H018), C01B(H01D), C01C(H01E), C01D(H01F),
 C01G(H01O), C01H(H01H), C01I(H01P), C01J(H01R), C01L(H01S), C01M(H01M),
 C01O(H01T), C01P(H01W), C01Q(H01Q), C01T(H01X), C01U(H01U), C01V(H01V),
 C01Z(H01Z), C020(H020), C022(H022), C023(H023), C024(H024), C025(H025),
 C026(H026), C027(H027), C028(H028), C02A(H02J), C02B(H02K), C02C(H02C),
 C02D(H02L), C02E(H02N), C02F(H02F), C02H(H02H), C02I(H02R), C02J(H02S),
 C02K(H02T), C02M(H02M)
2.b Idealised Me refined as rotating group:
 C012(H01A,H01B,H01C), C01A(H01K,H01L,H01N), C01Y(H01G,H01I,H01J), C029(H02E,
 H02G,H02I), C02G(H02O,H02P,H02Q), C02L(H02A,H02B,H02D)
;
_shelx_res_checksum              14657
_shelx_hkl_checksum              52415
_olex2_submission_special_instructions 'No special instructions were received'