Tuning radical interactions in trisradical tricationic complexes by varying host-cavity sizes.
Cai, Kang; Shi, Yi; Cao, Changsu; Vemuri, Suneal; Cui, Binbin; Shen, Dengke; Wu, Huang; Zhang, Long; Qiu, Yunyan; Chen, Hongliang; Jiao, Yang; Stern, Charlotte L.; Alsubaie, Fehaid M.; Xiao, Hai; Li, Jun; Stoddart, J. Fraser; Chemical science 11 (2020) 107–112; doi:10.1039/c9sc04860j

data_1552718
_publ_section_title
;
 Tuning radical interactions in trisradical tricationic complexes by
 varying host-cavity sizes.
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              107
_journal_page_last               112
_journal_paper_doi               10.1039/c9sc04860j
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C35 H31 N5, 4(F6 P)'
_chemical_formula_sum            'C35 H31 F24 N5 P4'
_chemical_formula_weight         1101.53
_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             2017-09-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-09-24 deposited with the CCDC.	2019-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                75.157(10)
_cell_angle_beta                 86.061(11)
_cell_angle_gamma                86.580(9)
_cell_formula_units_Z            4
_cell_length_a                   11.2904(11)
_cell_length_b                   16.9439(18)
_cell_length_c                   24.966(3)
_cell_measurement_reflns_used    4665
_cell_measurement_temperature    99.98
_cell_measurement_theta_max      64.6830
_cell_measurement_theta_min      2.7680
_cell_volume                     4601.4(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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      99.98
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f   -360.00   9.50   0.50   30.00 -55.02 -97.50  33.00    --   739
  2  \f   -328.39   9.11   0.50   30.00-152.20 -97.50-164.56    --   675
  3  \f     20.88 270.38   0.50   29.99 163.25  90.00 105.51    --   499
  4  \f    114.12 287.62   0.50   10.00  13.41 -35.00  58.00    --   347
  5  \f    182.41 312.91   0.50   29.99-113.97 -87.50-107.00    --   261
  6  \f    155.10 295.60   0.50   29.99-150.75 -97.50-119.51    --   281
  7  \w    -73.97  -4.47   0.50   10.00    --  -52.50  78.01-127.50  139
  8  \f      7.42 129.92   0.50   10.00  52.90  27.50-129.52    --   245
  9  \w   -126.86 -18.36   0.50   30.00    --  -90.00 143.03  64.98  217
 10  \w    180.33 272.83   0.50   30.00    --  -95.00-109.52  80.02  185
 11  \w     70.50 105.50   0.50   10.00    --   20.00 133.01 169.99   70
 12  \w    246.92 280.92   0.50   10.00    --  -52.50-104.50-172.50   68
 13  \w   -123.60 -20.10   0.50   30.00    --  -97.50 140.52-157.52  207
 14  \w   -108.99  -7.49   0.50   30.00    --  -92.50 100.50 120.00  203
 15  \w    109.76 145.76   0.50   30.00    --   87.50-169.60 107.58   72
 16  \w    224.43 265.43   0.50   30.00    -- -100.00 -52.01  15.00   82
 17  \w    247.00 285.50   0.50   30.00    --  -92.50-119.51  10.01   77
 18  \w    236.01 345.51   0.50   30.00    -- -100.00  25.50 -90.01  219
 19  \f     18.91 117.91   0.50   10.00  43.34 -40.00-174.63    --   198
 20  \w    218.63 258.63   0.50   30.00    --  -92.50 -52.01 122.50   80
 21  \w     55.88  97.38   0.50   30.00    --   90.00 -32.00  87.50   83
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0273204000
_diffrn_orient_matrix_UB_12      -0.0011751000
_diffrn_orient_matrix_UB_13      -0.0611086000
_diffrn_orient_matrix_UB_21      0.0841168000
_diffrn_orient_matrix_UB_22      -0.0757481000
_diffrn_orient_matrix_UB_23      0.0184631000
_diffrn_orient_matrix_UB_31      -0.1045001000
_diffrn_orient_matrix_UB_32      -0.0559018000
_diffrn_orient_matrix_UB_33      0.0035222000
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1817
_diffrn_reflns_av_unetI/netI     0.1636
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            34289
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        60.000
_diffrn_reflns_theta_max         60.000
_diffrn_reflns_theta_min         1.833
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.739
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_description       plate
_exptl_crystal_F_000             2208
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.305
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.026
_refine_diff_density_max         0.783
_refine_diff_density_min         -0.947
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.535
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1276
_refine_ls_number_reflns         13418
_refine_ls_number_restraints     1402
_refine_ls_restrained_S_all      1.476
_refine_ls_R_factor_all          0.3412
_refine_ls_R_factor_gt           0.2375
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5158
_refine_ls_wR_factor_ref         0.6050
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4387
_reflns_number_total             13418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc04860j2.cif
_cod_data_source_block           cx1045
_cod_depositor_comments
;Adding full bibliography for 1552713--1552722.cif.

 Adding full bibliography for 1552713--1552722.cif.
;
_cod_original_cell_volume        4601.5(8)
_cod_database_code               1552718
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.489
_reflns_odcompleteness_completeness 91.11
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.36
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 F33-F32 \\sim F33-F34 \\sim F33-F36 \\sim F32-F35 \\sim F32-F34 \\sim F32-F36
\\sim F35-F34 \\sim F35-F36
 with sigma of 0.04
 P6-F33 \\sim P6-F32 \\sim P6-F35 \\sim P6-F31 \\sim P6-F34 \\sim P6-F36
 with sigma of 0.02
 F30-F26 \\sim F30-F25 \\sim F30-F29 \\sim F28-F26 \\sim F28-F25 \\sim F28-F29
\\sim F27-F26 \\sim F27-F25
 \\sim F25-F29
 with sigma of 0.02
 P5-F30 \\sim P5-F28 \\sim P5-F27 \\sim P5-F26 \\sim P5-F25 \\sim P5-F29
 with sigma of 0.01
 F22-F23 \\sim F22-F20 \\sim F22-F19 \\sim F22-F21 \\sim F24-F23 \\sim F24-F20
\\sim F24-F19 \\sim F24-F21
 \\sim F23-F20 \\sim F23-F19 \\sim F20-F21 \\sim F19-F21
 with sigma of 0.02
 P4-F22 \\sim P4-F24 \\sim P4-F23 \\sim P4-F20 \\sim P4-F19 \\sim P4-F21
 with sigma of 0.01
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: P4(0.5) F19(0.5) F20(0.5) F21(0.5) F22(0.5) F23(0.5) F24(0.5)
 P6(0.5) F31(0.5) F32(0.5) F33(0.5) F34(0.5) F35(0.5) F36(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C12(H12A,H12B), C18(H18A,H18B), C29(H29A,H29B), C1A(H1AA,H1AB),
 C12A(H12C,H12D), C18A(H18C,H18D), C29A(H29C,H29D)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
 C15(H15), C16(H16), C19(H19), C20(H20), C22(H22), C23(H23), C25(H25), C26(H26),
  C27(H27), C28(H28), C34(H34), C35(H35), C31(H31), C32(H32), C2A(H2A),
 C3A(H3A), C5A(H5A), C6A(H6A), C8A(H8A), C9A(H9A), C10A(H10A), C11A(H11A),
 C14A(H14A), C15A(H15A), C16A(H16A), C19A(H19A), C20A(H20A), C22A(H22A),
 C23A(H23A), C25A(H25A), C26A(H26A), C27A(H27A), C28A(H28A), C31A(H31A),
 C32A(H32A), C34A(H34A), C35A(H35A)
5.c Fitted hexagon refined as free rotating group:
 C33(C34,C35,C30,C31,C32)
;
_smtbx_masks_special_details
;
The solvent masking procedure as implemented in Olex2 was used to remove the
electronic contribution of solvent molecules from the refinement.  As the exact
solvent content is not known, only the atoms used in the refinement model are
reported in the formula here.

Total solvent accessible volume / cell = 319.1 Ang^3^ [6.9%]
Total electron count / cell = 117.5
;
_shelx_res_checksum              63955
_shelx_fab_checksum              53714
_olex2_date_sample_data_collection 2017-09-22
_olex2_date_sample_submission    2017-08-07
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a glass fibre in Paratone oil'
_olex2_submission_original_sample_id cx1045
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.277
_oxdiff_exptl_absorpt_empirical_full_min 0.377