Rotaxane-branched Radical Dendrimers with TEMPO Termini
Peng, Zhiyong; Xu, Xiao-Qin; Wang, Xu-Qing; Shi, Xueliang; Wang, Wei; Yang, Hai-Bo; Chemical Communications  (2022) –; doi:10.1039/D1CC06158E

data_7129544
_publ_section_title
;
 Rotaxane-branched Radical Dendrimers with TEMPO Termini
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06158E
_journal_year                    2022
_chemical_formula_moiety         'C18 H23 N2 O2'
_chemical_formula_sum            'C18 H23 N2 O2'
_chemical_formula_weight         299.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-09-09 deposited with the CCDC.	2022-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.9640(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7806(2)
_cell_length_b                   10.9499(2)
_cell_length_c                   14.5775(2)
_cell_measurement_reflns_used    12304
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.8110
_cell_measurement_theta_min      4.6490
_cell_volume                     1676.96(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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     52.00  78.00   1.00    1.00    --    0.00  38.00   0.00   26
  2  \w    -19.00  41.00   1.00    1.00    --    0.00  38.00  90.00   60
  3  \w    -19.00  35.00   1.00    1.00    --    0.00  38.00 -60.00   54
  4  \w    -23.00  24.00   1.00    1.00    --    0.00  19.00 -90.00   47
  5  \w    -17.00   8.00   1.00    1.00    --    0.00  57.00 -90.00   25
  6  \w     40.00  66.00   1.00    1.00    --    0.00  38.00 -60.00   26
  7  \w     48.00  77.00   1.00    1.00    --    0.00  38.00  90.00   29
  8  \w    -30.00  77.00   1.00    1.00    --    0.00  77.00-180.00  107
  9  \w    -18.00  50.00   1.00    1.00    --    0.00  38.00   0.00   68
 10  \w     29.00  54.00   1.00    1.00    --    0.00  57.00 -90.00   25
 11  \w    -21.00  89.00   1.00    1.00    --    0.00  57.00 120.00  110
 12  \w    126.00 152.00   1.00    1.00    --   95.80  82.00-178.58   26
 13  \w     65.00  90.00   1.00    1.00    --   95.80  76.00  -0.59   25
 14  \w     48.00 119.00   1.00    1.00    --   95.80 -61.00  90.00   71
 15  \w     63.00  95.00   1.00    1.00    --   95.80  82.00-178.58   32
 16  \w     65.00  90.00   1.00    1.00    --   95.80  78.00-154.00   25
 17  \w    125.00 180.00   1.00    1.00    --   95.80  74.00 -98.52   55
 18  \w    134.00 160.00   1.00    1.00    --   95.80  50.00  83.84   26
 19  \w      6.00 128.00   1.00    1.00    --   95.80 -82.00   0.00  122
 20  \w     67.00 179.00   1.00    1.00    --   95.80  71.00  31.35  112
 21  \w      6.00 128.00   1.00    1.00    --   95.80 -82.00-120.00  122
 22  \w     67.00  95.00   1.00    1.00    --   95.80  77.00 -60.00   28
 23  \w    124.00 150.00   1.00    1.00    --   95.80  77.00 -60.00   26
 24  \w     64.00  90.00   1.00    1.00    --   95.80  82.00  30.00   26
 25  \w     94.00 119.00   1.00    1.00    --   95.80  82.00  30.00   25
 26  \w     63.00  89.00   1.00    1.00    --   95.80  82.00 -30.00   26
 27  \w     65.00  92.00   1.00    1.00    --   95.80  77.00 -30.00   27
 28  \w     67.00  93.00   1.00    1.00    --   95.80  82.00  90.00   26
 29  \w     63.00  89.00   1.00    1.00    --   95.80  82.00 120.00   26
 30  \w     65.00 125.00   1.00    1.00    --   95.80  77.00 -90.00   60
 31  \w     66.00  97.00   1.00    1.00    --   95.80  77.00-128.80   31
 32  \w     66.00 110.00   1.00    1.00    --   95.80  74.00 -98.52   44
 33  \w      7.00 119.00   1.00    1.00    --   95.80 -61.00   0.00  112
 34  \w     71.00 172.00   1.00    1.00    --   95.80  58.00 107.39  101
 35  \w     71.00 101.00   1.00    1.00    --   95.80  61.00  30.00   30
 36  \w     65.00  90.00   1.00    1.00    --   95.80  77.00-180.00   25
 37  \w     63.00  88.00   1.00    1.00    --   95.80  82.00-150.00   25
 38  \w     65.00  90.00   1.00    1.00    --   95.80  77.00  60.00   25
 39  \w     71.00 100.00   1.00    1.00    --   95.80  61.00  90.00   29
 40  \w    111.00 163.00   1.00    1.00    --   95.80  61.00  90.00   52
 41  \w     71.00  97.00   1.00    1.00    --   95.80  61.00 150.00   26
 42  \w     65.00  91.00   1.00    1.00    --   95.80  77.00  30.00   26
 43  \w     66.00  92.00   1.00    1.00    --   95.80  77.00  90.00   26
 44  \w     65.00  90.00   1.00    1.00    --   95.80  77.00 120.00   25
 45  \w     65.00  91.00   1.00    1.00    --   95.80  82.00 -90.00   26
 46  \w     64.00  95.00   1.00    1.00    --   95.80  82.00 -60.00   31
 47  \w     63.00  89.00   1.00    1.00    --   95.80  82.00 150.00   26
 48  \w     76.00 185.00   1.00    1.00    --   95.80  45.00 -30.00  109
 49  \w     75.00 169.00   1.00    1.00    --   95.80  45.00   0.00   94
 50  \w     75.00 100.00   1.00    1.00    --   95.80  45.00  30.00   25
 51  \w     71.00 144.00   1.00    1.00    --   95.80  61.00 120.00   73
 52  \w     21.00 100.00   1.00    1.00    --   95.80 -61.00-120.00   79
 53  \w     63.00  95.00   1.00    1.00    --   95.80  82.00-120.00   32
 54  \w     79.00 128.00   1.00    1.00    --   95.80 -82.00  90.00   49
 55  \w     74.00 135.00   1.00    1.00    --   95.80  48.00 152.07   61
 56  \w     73.00 185.00   1.00    1.00    --   95.80  53.00-127.45  112
 57  \w     75.00 185.00   1.00    1.00    --   95.80  45.00-150.00  110
 58  \w     74.00 100.00   1.00    1.00    --   95.80  50.00  83.84   26
 59  \w     79.00 104.00   1.00    1.00    --   95.80  30.00-150.00   25
 60  \w     59.00  99.00   1.00    1.00    --   95.80 -82.00-180.00   40
 61  \w     67.00  93.00   1.00    1.00    --   95.80  72.00 148.40   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0441985000
_diffrn_orient_matrix_UB_12      0.0325393000
_diffrn_orient_matrix_UB_13      0.1051075000
_diffrn_orient_matrix_UB_21      0.1357811000
_diffrn_orient_matrix_UB_22      0.0226129000
_diffrn_orient_matrix_UB_23      -0.0135669000
_diffrn_orient_matrix_UB_31      -0.0332386000
_diffrn_orient_matrix_UB_32      0.1350224000
_diffrn_orient_matrix_UB_33      -0.0230130000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35256
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.061
_diffrn_reflns_theta_max         67.061
_diffrn_reflns_theta_min         5.100
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.617
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28500
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
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    1.186
_exptl_crystal_description       block
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.189
_refine_diff_density_min         -0.187
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         2975
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+0.6568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0854
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2678
_reflns_number_total             2975
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06158e2.cif
_cod_data_source_block           exp_1289
_cod_database_code               7129544
_shelx_shelxl_version_number     2017/1
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C9(H9A,H9B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C1(H1A), C2(H2), C5(H5), C4(H4)
2.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C)
;
_shelx_res_checksum              85222
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.355
_oxdiff_exptl_absorpt_empirical_full_min 0.567