TEMPO Radical-Functionalized Supramolecular Coordination Complexes with Controllable Spin-Spin Interactions.
Jiang, Wei-Ling; Peng, Zhiyong; Huang, Bin; Zhao, Xiao-Li; Sun, Di; Shi, Xueliang; Yang, Hai-Bo; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c11738

data_4135434
_publ_section_title
;
 TEMPO Radical-Functionalized Supramolecular Coordination Complexes with
 Controllable Spin-Spin Interactions.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c11738
_journal_year                    2020
_chemical_formula_moiety         'C134 H194 N6 O8 P8 Pt4, 4(B F4)'
_chemical_formula_sum            'C134 H194 B4 F16 N6 O8 P8 Pt4'
_chemical_formula_weight         3392.30
_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             2020-09-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                107.001(3)
_cell_angle_beta                 90.638(3)
_cell_angle_gamma                94.110(4)
_cell_formula_units_Z            1
_cell_length_a                   12.0853(5)
_cell_length_b                   18.1737(9)
_cell_length_c                   19.8820(6)
_cell_measurement_reflns_used    11542
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.9180
_cell_measurement_theta_min      3.7010
_cell_volume                     4162.8(3)
_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 0.983
_diffrn_measured_fraction_theta_max 0.983
_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    -26.00  13.00   1.00    3.00    --    0.00 -38.00  30.00   39
  2  \w    -26.00  22.00   1.00    3.00    --    0.00 -57.00-180.00   48
  3  \w    -56.00 -29.00   1.00    3.00    --    0.00 -57.00-180.00   27
  4  \w    -83.00 -36.00   1.00    3.00    --    0.00 -57.00 120.00   47
  5  \w    -88.00 -26.00   1.00    3.00    --    0.00 -38.00   0.00   62
  6  \w    -17.00  69.00   1.00    3.00    --    0.00  38.00   0.00   86
  7  \w    -22.00  36.00   1.00    3.00    --    0.00  57.00-120.00   58
  8  \w     69.00 127.00   1.00    3.00    --   95.80 -82.00 150.00   58
  9  \w     76.00 180.00   1.00    3.00    --   95.80  30.00 -90.00  104
 10  \w      6.00 116.00   1.00    3.00    --   95.80 -45.00  90.00  110
 11  \w     13.00 119.00   1.00    3.00    --   95.80 -61.00 -60.00  106
 12  \w     77.00 104.00   1.00    3.00    --   95.80 -82.00 -90.00   27
 13  \w     24.00 122.00   1.00    3.00    --   95.80 -82.00-120.00   98
 14  \w     18.00 104.00   1.00    3.00    --   95.80 -61.00  60.00   86
 15  \w     38.00 105.00   1.00    3.00    --   95.80 -30.00-180.00   67
 16  \w    100.00 127.00   1.00    3.00    --   95.80 -82.00  90.00   27
 17  \w     11.00  37.00   1.00    3.00    --   95.80 -82.00   0.00   26
 18  \w     58.00  89.00   1.00    3.00    --   95.80 -82.00-150.00   31
 19  \w     95.00 122.00   1.00    3.00    --   95.80 -82.00-150.00   27
 20  \w     14.00 127.00   1.00    3.00    --   95.80 -82.00  60.00  113
 21  \w    139.00 177.00   1.00    3.00    --   95.80  30.00-180.00   38
 22  \w     90.00 126.00   1.00    3.00    --   95.80  30.00-180.00   36
 23  \w     86.00 113.00   1.00    3.00    --   95.80 -82.00 -30.00   27
 24  \w      6.00  92.00   1.00    3.00    --   95.80 -45.00 -60.00   86
 25  \w     82.00 164.00   1.00    3.00    --   95.80  30.00-150.00   82
 26  \w     74.00  99.00   1.00    3.00    --   95.80 -82.00  30.00   25
 27  \w     50.00  75.00   1.00    3.00    --   95.80 -77.00 -90.00   25
;
_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      0.0283981000
_diffrn_orient_matrix_UB_12      -0.0205349000
_diffrn_orient_matrix_UB_13      0.0677470000
_diffrn_orient_matrix_UB_21      0.0039031000
_diffrn_orient_matrix_UB_22      0.0860284000
_diffrn_orient_matrix_UB_23      0.0422853000
_diffrn_orient_matrix_UB_31      -0.1246204000
_diffrn_orient_matrix_UB_32      -0.0091335000
_diffrn_orient_matrix_UB_33      0.0139632000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0893
_diffrn_reflns_av_unetI/netI     0.0924
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43305
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.075
_diffrn_reflns_theta_max         67.075
_diffrn_reflns_theta_min         4.279
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.409
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21480
_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    1.353
_exptl_crystal_description       block
_exptl_crystal_F_000             1700
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         6.202
_refine_diff_density_min         -1.823
_refine_diff_density_rms         0.277
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     779
_refine_ls_number_reflns         14620
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.1296
_refine_ls_R_factor_gt           0.0998
_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^)+(0.1988P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2524
_refine_ls_wR_factor_ref         0.2742
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9648
_reflns_number_total             14620
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11738_si_006.cif
_cod_data_source_block           exp_1427
_cod_database_code               4135434
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.269
_shelx_estimated_absorpt_t_min   0.200
_reflns_odcompleteness_completeness 99.50
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C57-C58
 1.52 with sigma of 0.01
 C55-C56
 1.52 with sigma of 0.01
 C59-C60
 1.52 with sigma of 0.01
 C61-C62
 1.52 with sigma of 0.01
 C49-C50
 1.52 with sigma of 0.01
 C54-C53
 1.52 with sigma of 0.01
 C51-C52
 1.52 with sigma of 0.01
 C63-C64
 1.52 with sigma of 0.01
 C65-C66
 1.52 with sigma of 0.01
 C33-O1
 1.4 with sigma of 0.02
 C33-C67
 1.52 with sigma of 0.02
 C41-C37
 1.52 with sigma of 0.01
 C36-C39
 1.52 with sigma of 0.01
 C36-C40
 1.52 with sigma of 0.01
3. Rigid bond restraints
 C40, C36, C39
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C33, C67, O3, C34, C38
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C42, C37
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 P3, C55
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 P3, C59
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 P3, C57
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 P4, C63
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C41, C37
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C43, C44
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O1, C13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C33, O1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C22 \\sim C21 \\sim C26 \\sim C25 \\sim C24 \\sim C23: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C55 \\sim C56: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C57 \\sim C58: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C60 \\sim C59: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C36 \\sim C35 \\sim C34 \\sim C38 \\sim C37 \\sim N3: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C64 \\sim C63: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C65 \\sim C66: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C3 \\sim C2 \\sim C1 \\sim N1 \\sim C5 \\sim C4: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
C40 \\sim C36 \\sim C39: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C33 \\sim C67 \\sim O3 \\sim C34 \\sim C38: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C37 \\sim C42: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C65) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O1) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C64) = Uanis(C63) = Uanis(C65) = Uanis(C66)
Uanis(C57) = Uanis(C58) = Uanis(C55) = Uanis(C56)
Uanis(C59) = Uanis(C60) = Uanis(C57) = Uanis(C58)
5.a Ternary CH refined with riding coordinates:
 C34(H34)
5.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C35(H35A,H35B), C38(H38A,H38B), C43(H43A,H43B), C45(H45A,
 H45B), C47(H47A,H47B), C49(H49A,H49B), C51(H51A,H51B), C53(H53A,H53B),
 C55(H55A,H55B), C57(H57A,H57B), C59(H59A,H59B), C61(H61A,H61B), C63(H63A,H63B),
  C65(H65A,H65B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C17(H17), C18(H18),
 C19(H19), C20(H20), C22(H22), C23(H23), C25(H25), C26(H26), C28(H28), C29(H29),
  C31(H31), C32(H32)
5.d Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C50(H50A,
 H50B,H50C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C),
 C58(H58A,H58B,H58C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C), C64(H64A,H64B,
 H64C), C66(H66A,H66B,H66C)
;
_shelx_res_checksum              37083
_shelx_hkl_checksum              85298
_shelx_fab_checksum              67216
_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 4.562
_oxdiff_exptl_absorpt_empirical_full_min 0.301