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_4135435
_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         'C61 H93 N3 O4 P4 Pt2, 3(C3 H6 O), 2(F6 P)'
_chemical_formula_sum            'C70 H111 F12 N3 O7 P6 Pt2'
_chemical_formula_weight         1910.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.1550(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5498(2)
_cell_length_b                   45.4250(5)
_cell_length_c                   13.8449(2)
_cell_measurement_reflns_used    80226
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.2130
_cell_measurement_theta_min      3.4470
_cell_volume                     8097.3(2)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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    -89.00  23.00   1.00    1.00    --    0.00 -57.00  30.00  112
  2  \w     48.00  89.00   1.00    1.00    --    0.00  57.00 -90.00   41
  3  \w    -34.00  21.00   1.00    1.00    --    0.00 -57.00-120.00   55
  4  \w    -43.00  21.00   1.00    1.00    --    0.00 -19.00 120.00   64
  5  \w    -18.00  19.00   1.00    1.00    --    0.00 -38.00 -30.00   37
  6  \w    -25.00  56.00   1.00    1.00    --    0.00  82.00  30.00   81
  7  \w    -11.00  16.00   1.00    1.00    --    0.00  57.00 -90.00   27
  8  \w    -88.00 -27.00   1.00    1.00    --    0.00 -38.00 -30.00   61
  9  \w     44.00  70.00   1.00    1.00    --    0.00  38.00  60.00   26
 10  \w    -19.00  19.00   1.00    1.00    --    0.00  38.00  60.00   38
 11  \w    -19.00  87.00   1.00    1.00    --    0.00  38.00 -90.00  106
 12  \w    -55.00  25.00   1.00    1.00    --    0.00 -77.00  90.00   80
 13  \w     68.00  94.00   1.00    1.00    --   95.80  69.00 126.82   26
 14  \w     70.00 185.00   1.00    1.00    --   95.80  63.00 162.23  115
 15  \w     73.00 184.00   1.00    1.00    --   95.80  53.00  53.35  111
 16  \w    117.00 184.00   1.00    1.00    --   95.80  76.00  78.76   67
 17  \w     65.00  95.00   1.00    1.00    --   95.80  76.00  78.76   30
 18  \w    106.00 137.00   1.00    1.00    --   95.80  36.00 146.35   31
 19  \w    133.00 159.00   1.00    1.00    --   95.80  58.00 -86.97   26
 20  \w     64.00  90.00   1.00    1.00    --   95.80  80.00-164.90   26
 21  \w     64.00  90.00   1.00    1.00    --   95.80  80.00  23.31   26
 22  \w     71.00 185.00   1.00    1.00    --   95.80  59.00 -38.57  114
 23  \w    128.00 155.00   1.00    1.00    --   95.80  80.00-164.90   27
 24  \w     65.00  91.00   1.00    1.00    --   95.80  78.00 -65.58   26
 25  \w     67.00  93.00   1.00    1.00    --   95.80  71.00 -27.34   26
 26  \w      7.00  81.00   1.00    1.00    --   95.80 -82.00 120.00   74
 27  \w     89.00 128.00   1.00    1.00    --   95.80 -82.00 120.00   39
 28  \w     23.00 127.00   1.00    1.00    --   95.80 -82.00 -60.00  104
 29  \w     65.00  91.00   1.00    1.00    --   95.80  77.00   0.00   26
 30  \w    124.00 177.00   1.00    1.00    --   95.80  77.00   0.00   53
 31  \w    157.00 183.00   1.00    1.00    --   95.80  82.00 165.19   26
 32  \w     63.00  90.00   1.00    1.00    --   95.80  82.00 165.19   27
 33  \w     70.00 185.00   1.00    1.00    --   95.80  64.00-140.78  115
 34  \w     76.00 102.00   1.00    1.00    --   95.80  36.00 146.35   26
 35  \w     64.00  89.00   1.00    1.00    --   95.80  82.00  60.00   25
 36  \w     63.00  89.00   1.00    1.00    --   95.80  82.00-180.00   26
 37  \w    141.00 167.00   1.00    1.00    --   95.80  74.00-122.40   26
 38  \w     63.00  89.00   1.00    1.00    --   95.80  82.00  90.00   26
 39  \w     72.00  97.00   1.00    1.00    --   95.80  61.00  30.00   25
 40  \w     63.00  88.00   1.00    1.00    --   95.80  82.00 -60.00   25
 41  \w     63.00  89.00   1.00    1.00    --   95.80  82.00  30.00   26
 42  \w     63.00  89.00   1.00    1.00    --   95.80  82.00-150.00   26
 43  \w     66.00  92.00   1.00    1.00    --   95.80  74.00-122.40   26
 44  \w     65.00  91.00   1.00    1.00    --   95.80  77.00 150.00   26
 45  \w     68.00  94.00   1.00    1.00    --   95.80  68.00 -63.71   26
 46  \w     65.00  91.00   1.00    1.00    --   95.80  77.00-120.00   26
 47  \w    147.00 183.00   1.00    1.00    --   95.80  52.00 142.93   36
 48  \w     63.00  89.00   1.00    1.00    --   95.80  82.00 120.00   26
 49  \w     75.00 185.00   1.00    1.00    --   95.80  45.00 -60.00  110
 50  \w     76.00 184.00   1.00    1.00    --   95.80  45.00  30.00  108
 51  \w     30.00 121.00   1.00    1.00    --   95.80 -82.00-180.00   91
 52  \w     73.00 175.00   1.00    1.00    --   95.80  61.00 150.00  102
 53  \w     65.00  90.00   1.00    1.00    --   95.80  77.00 -90.00   25
 54  \w     65.00 150.00   1.00    1.00    --   95.80  77.00  60.00   85
 55  \w     65.00  91.00   1.00    1.00    --   95.80  77.00  90.00   26
 56  \w     63.00  89.00   1.00    1.00    --   95.80  82.00   0.00   26
 57  \w     75.00 139.00   1.00    1.00    --   95.80  45.00 -90.00   64
 58  \w     66.00  92.00   1.00    1.00    --   95.80  75.00  53.11   26
 59  \w     63.00  89.00   1.00    1.00    --   95.80  82.00 -30.00   26
 60  \w     72.00  97.00   1.00    1.00    --   95.80  61.00-120.00   25
 61  \w     16.00  72.00   1.00    1.00    --   95.80 -61.00-120.00   56
 62  \w     79.00 104.00   1.00    1.00    --   95.80 -61.00-120.00   25
 63  \w     65.00 183.00   1.00    1.00    --   95.80  77.00-180.00  118
 64  \w     65.00  91.00   1.00    1.00    --   95.80  77.00 -30.00   26
 65  \w     22.00 126.00   1.00    1.00    --   95.80 -82.00  90.00  104
 66  \w     64.00  89.00   1.00    1.00    --   95.80  79.00 160.78   25
 67  \w     75.00 101.00   1.00    1.00    --   95.80  45.00   0.00   26
 68  \w      6.00 110.00   1.00    1.00    --   95.80 -82.00   0.00  104
 69  \w     73.00  99.00   1.00    1.00    --   95.80  52.00 142.93   26
 70  \w     75.00 102.00   1.00    1.00    --   95.80  51.00 -20.85   27
 71  \w     72.00  97.00   1.00    1.00    --   95.80  58.00 -86.97   25
 72  \w     75.00 101.00   1.00    1.00    --   95.80  42.00  12.60   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      -0.0246176000
_diffrn_orient_matrix_UB_12      0.0318457000
_diffrn_orient_matrix_UB_13      0.0230810000
_diffrn_orient_matrix_UB_21      -0.0645714000
_diffrn_orient_matrix_UB_22      0.0042540000
_diffrn_orient_matrix_UB_23      -0.1123070000
_diffrn_orient_matrix_UB_31      -0.0976884000
_diffrn_orient_matrix_UB_32      -0.0108650000
_diffrn_orient_matrix_UB_33      0.0237421000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1891
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            202952
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.078
_diffrn_reflns_theta_max         67.078
_diffrn_reflns_theta_min         3.433
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.154
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.03969
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_description       block
_exptl_crystal_F_000             3848
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.32
_refine_diff_density_max         7.084
_refine_diff_density_min         -3.719
_refine_diff_density_rms         0.283
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     905
_refine_ls_number_reflns         14378
_refine_ls_number_restraints     119
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.1154
_refine_ls_R_factor_gt           0.1125
_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^)+(0.0684P)^2^+338.8987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2632
_refine_ls_wR_factor_ref         0.2647
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13559
_reflns_number_total             14378
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11738_si_003.cif
_cod_data_source_block           exp_1303
_cod_original_cell_volume        8097.30(19)
_cod_database_code               4135435
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.180
_shelx_estimated_absorpt_t_min   0.111
_reflns_odcompleteness_completeness 99.98
_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
 C47-C48
 1.52 with sigma of 0.01
 C43-C44
 1.52 with sigma of 0.01
 C45-C46
 1.52 with sigma of 0.01
 C39-C40
 1.52 with sigma of 0.01
 C37-C38
 1.52 with sigma of 0.01
 C41-C42
 1.52 with sigma of 0.01
 C55-C56
 1.52 with sigma of 0.01
 C57-C58
 1.52 with sigma of 0.01
 C51-C52
 1.52 with sigma of 0.01
 C54-C53
 1.52 with sigma of 0.01
 C59-C60
 1.52 with sigma of 0.01
3. Rigid bond restraints
 C47, C48
 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
 C45, C46
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C37, C38
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C39, C40
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C41, C42
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C53, C54
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C49, C50
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C51, C52
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C57, C58
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C55, C56
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C59, C60
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C47 \\sim C48: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim
C45 \\sim C46: 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
C51 \\sim C52: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C53 \\sim C54: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C57 \\sim C58 \\sim C59 \\sim C60: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C26) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of
0.002 and sigma for terminal atoms of 0.004
Uanis(F12) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C7) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C48) = Uanis(C47) = Uanis(C44) = Uanis(C43)
5.a Ternary CH refined with riding coordinates:
 C28(H28)
5.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C32(H32A,H32B), C37(H37A,H37B), C39(H39A,H39B), C41(H41A,
 H41B), 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)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C5(H5), C10(H10), C11(H11), C12(H12), C013(H013), C15(H15),
 C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C24(H24), C25(H25), C26(H26)
5.d Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), 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), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C), C64(H64A,
 H64B,H64C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C69(H69A,H69B,H69C)
;
_shelx_res_checksum              80633
_shelx_hkl_checksum              25010
_shelx_fab_checksum              89391
_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 14.559
_oxdiff_exptl_absorpt_empirical_full_min 0.460