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_1557693
_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         'C33 H49 N2 O2 Pd, C32 H12 B F24'
_chemical_formula_sum            'C65 H61 B F24 N2 O2 Pd'
_chemical_formula_weight         1475.36
_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
_audit_creation_date             2019-11-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                74.958(3)
_cell_angle_beta                 70.373(3)
_cell_angle_gamma                83.080(3)
_cell_formula_units_Z            2
_cell_length_a                   12.4860(5)
_cell_length_b                   15.7992(7)
_cell_length_c                   18.2813(8)
_cell_measurement_reflns_used    37690
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.13
_cell_measurement_theta_min      1.73
_cell_volume                     3278.2(3)
_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_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 2018/3 (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 0.998
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
 309 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  0.0343
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32280
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.907
_diffrn_reflns_theta_min         1.733
_diffrn_source
'Sealed Mo X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.396
_exptl_absorpt_correction_T_max  0.8363
_exptl_absorpt_correction_T_min  0.5079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.225
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       0.0024(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     935
_refine_ls_number_reflns         13902
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1098
_refine_ls_R_factor_gt           0.0711
_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^)+(0.0508P)^2^+10.3203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1521
_refine_ls_wR_factor_ref         0.1769
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9782
_reflns_number_total             13902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma0c00241_si_002.cif
_cod_data_source_block           gs19_022
_cod_database_code               1557693
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H) groups
2. Others
 Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(C69)=Sof(H69A)=
 Sof(H69B)=Sof(C70)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=Sof(O3)=Sof(O4)=
 Sof(Pd2)=1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(H3A)=Sof(H3B)=
 Sof(C4)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(O1)=Sof(O2)=Sof(Pd1)=FVAR(1)
 Sof(F25)=Sof(F26)=Sof(F27)=1-FVAR(2)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(2)
3.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C29(H29), C32(H32)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C67(H67A,H67B), C68(H68A,H68B),
 C69(H69A,H69B)
3.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C25(H25), C26(H26), C27(H27), C36(H36), C38(H38),
 C40(H40), C44(H44), C46(H46), C48(H48), C52(H52), C54(H54), C56(H56), C60(H60),
  C62(H62), C64(H64)
3.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C30(H30A,
 H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C),
 C71(H71A,H71B,H71C)
;
_shelx_res_checksum              10324
_shelx_hkl_checksum              43527
_olex2_submission_special_instructions 'No special instructions were received'