Catalytic Chain Transfer Polymerization to Functional Reactive End Groups for Controlled Free Radical Growth
Stadler, Sonja M.; Göttker-Schnetmann, Inigo; Fuchs, Amelie S.; Fischer, Stephan R. R.; Mecking, Stefan; Macromolecules  (2020) –; doi:10.1021/acs.macromol.0c00241

data_1557694
_publ_section_title
;
 Catalytic Chain Transfer Polymerization to Functional Reactive End Groups
 for Controlled Free Radical Growth
;
_journal_name_full               Macromolecules
_journal_paper_doi               10.1021/acs.macromol.0c00241
_journal_year                    2020
_chemical_formula_moiety         'C31 H46 N3 Pd, C32 H12 B F24'
_chemical_formula_sum            'C63 H58 B F24 N3 Pd'
_chemical_formula_weight         1430.33
_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             2019-11-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                93.278(3)
_cell_angle_beta                 98.104(3)
_cell_angle_gamma                98.439(3)
_cell_formula_units_Z            2
_cell_length_a                   12.7207(5)
_cell_length_b                   15.1193(7)
_cell_length_c                   16.6268(6)
_cell_measurement_reflns_used    20349
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.21
_cell_measurement_theta_min      1.77
_cell_volume                     3121.7(2)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 1.74.2.0 (STOE, 2018)
X-Area LANA 1.75.3.0 (STOE, 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      100.15
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
 246 frames, detector distance = 120 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27373
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.825
_diffrn_reflns_theta_min         1.899
_diffrn_source
'Sealed Mo X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.411
_exptl_absorpt_correction_T_max  0.9398
_exptl_absorpt_correction_T_min  0.7210
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.837
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     862
_refine_ls_number_reflns         13210
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0381P)^2^+4.8170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0946
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11223
_reflns_number_total             13210
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma0c00241_si_003.cif
_cod_data_source_block           ssp196
_cod_database_code               1557694
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H1A,H1B,H1C} of C1, {H11A,H11B,H11C} of C11, {H27A,H27B,
  H27C} of C27, {H26A,H26B,H26C} of C26, {H29A,H29B,H29C} of C29, {H14A,H14B,
  H14C} of C14, {H13A,H13B,H13C} of C13, {H17A,H17B,H17C} of C17, {H24A,H24B,
  H24C} of C24
 At 1.5 times of:
  {H64A,H64B,H64C} of C64, {H66A,H66B,H66C} of C66, {H31A,H31B,H31C} of C31,
  {H8A,H8B,H8C} of C8, {H10A,H10B,H10C} of C10
2. Shared sites
{C9, C65}
3. Uiso/Uaniso restraints and constraints
Uanis(C9) = Uanis(C65)
4. Others
 Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=Sof(C65)=Sof(H65)=Sof(C66)=Sof(H66A)=
 Sof(H66B)=Sof(H66C)=1-FVAR(1)
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10A)=
 Sof(H10B)=Sof(H10C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12), C25(H25), C28(H28), C65(H65)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C20(H20), C21(H21), C22(H22), C33(H33), C35(H35),
 C37(H37), C41(H41), C43(H43), C45(H45), C49(H49), C51(H51), C53(H53), C57(H57),
  C59(H59), C61(H61)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C31(H31A,
 H31B,H31C), C64(H64A,H64B,H64C), C66(H66A,H66B,H66C)
;
_shelx_res_checksum              24951
_shelx_hkl_checksum              24365
_olex2_submission_special_instructions 'No special instructions were received'