Comprehensive Picture of Functionalized Vinyl Monomers in Chain-Walking Polymerization
Zhang, Yuxing; Jian, Zhongbao; Macromolecules 53 (2020) 8858–8866; doi:10.1021/acs.macromol.0c01953

data_1559451
_publ_section_title
;
 Comprehensive Picture of Functionalized Vinyl Monomers in Chain-Walking
 Polymerization
;
_journal_issue                   20
_journal_name_full               Macromolecules
_journal_page_first              8858
_journal_page_last               8866
_journal_paper_doi               10.1021/acs.macromol.0c01953
_journal_volume                  53
_journal_year                    2020
_chemical_formula_moiety
'C92 H67 N2 O4 Pd, C32 H12 B F22.5, 4(C H Cl3)'
_chemical_formula_sum            'C128 H83 B Cl12 F22.5 N2 O4 Pd'
_chemical_formula_weight         2683.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-04-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 114.279(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.201(3)
_cell_length_b                   18.852(3)
_cell_length_c                   20.713(3)
_cell_measurement_reflns_used    9726
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      59.0868
_cell_measurement_theta_min      3.3128
_cell_volume                     6478.6(18)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'bruker apex ccd'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0628
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31034
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        59.083
_diffrn_reflns_theta_max         59.083
_diffrn_reflns_theta_min         2.728
_exptl_absorpt_coefficient_mu    4.151
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.3839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1551 before and 0.0830 after correction.
The Ratio of minimum to maximum transmission is 0.5108.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       block
_exptl_crystal_F_000             2709
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.035
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.094(10)
_refine_ls_extinction_coef       0.0014(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1607
_refine_ls_number_reflns         16008
_refine_ls_number_restraints     246
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0606
_refine_ls_shift/su_max          0.089
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1220P)^2^+7.0975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1689
_refine_ls_wR_factor_ref         0.1717
_reflns_Friedel_coverage         0.932
_reflns_Friedel_fraction_full    0.973
_reflns_Friedel_fraction_max     0.973
_reflns_number_gt                15591
_reflns_number_total             16008
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma0c01953_si_002.cif
_cod_data_source_block           1_sq
_cod_original_cell_volume        6478.4(16)
_cod_original_formula_sum        'C128 H83 B Cl12 F22.50 N2 O4 Pd'
_cod_database_code               1559451
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.906(10)
 0.094(10)
2. 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
3. Restrained distances
 C107-F1 = C107-F3 = C107-F1' = C107-F3' = C108-F4 = C108-F5 = C108-F6 = C117-F7
 1.34 with sigma of 0.01
 C118-F10 = C137-F20
 1.34 with sigma of 0.01
 C115-C118
 1.48 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C107 \\sim F1 \\sim F2 \\sim F3 \\sim F1' \\sim F2' \\sim F3': within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C108 \\sim F4 \\sim F5 \\sim F6: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002
C118 \\sim F10 \\sim F11 \\sim F12: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C137 \\sim F19 \\sim F20 \\sim F21 \\sim F19' \\sim F20' \\sim F21': within 2A
with sigma of 0.001 and sigma for terminal atoms of 0.002
C117 \\sim F7 \\sim F8 \\sim F9: within 2A with sigma of 0.015 and sigma for
terminal atoms of 0.03
5. Others
 Sof(F1')=Sof(F2')=Sof(F3')=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
 Sof(F19')=Sof(F20')=Sof(F21')=1-FVAR(2)
 Sof(F19)=Sof(F20)=Sof(F21)=FVAR(2)
 Fixed Sof: F4(0.5) F5(0.5) F6(0.5)
6.a Ternary CH refined with riding coordinates:
 C0(H0), C00(H00), C000(H000), C3(H3), C4(H4), C24(H24), C25(H25), C38(H38),
 C39(H39), C59(H59), C60(H60), C73(H73), C74(H74), C01(H01)
6.b Secondary CH2 refined with riding coordinates:
 C89(H89A,H89B)
6.c Me refined with riding coordinates:
 C23(H23A,H23B,H23C), C58(H58A,H58B,H58C), C90(H90A,H90B,H90C), C91(H91A,H91B,
 H91C), C92(H92A,H92B,H92C)
6.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14), C15(H15), C16(H16),
 C28(H28), C29(H29), C30(H30), C31(H31), C34(H34), C35(H35), C36(H36), C37(H37),
  C42(H42), C43(H43), C44(H44), C45(H45), C48(H48), C49(H49), C50(H50),
 C51(H51), C63(H63), C64(H64), C65(H65), C66(H66), C69(H69), C70(H70), C71(H71),
  C72(H72), C77(H77), C78(H78), C79(H79), C80(H80), C83(H83), C84(H84),
 C85(H85), C86(H86), C102(H102), C104(H104), C106(H106), C112(H112), C114(H114),
  C116(H116), C122(H122), C124(H124), C126(H126), C132(H132), C134(H134),
 C136(H136)
;
_shelx_res_checksum              30981
_shelx_hkl_checksum              55513
_shelx_fab_checksum              51267
_olex2_submission_special_instructions 'No special instructions were received'