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_1552715
_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         'C36 H32 N4, 0.5(C24 H28 N4), 3(F6 P)'
_chemical_formula_sum            'C48 H46 F18 N6 P3'
_chemical_formula_weight         1141.82
_space_group_crystal_system      orthorhombic
_space_group_IT_number           55
_space_group_name_Hall           '-P 2 2ab'
_space_group_name_H-M_alt        'P b a m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-07-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2019-09-24 deposited with the CCDC.	2019-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.1423(6)
_cell_length_b                   21.9108(7)
_cell_length_c                   9.5937(3)
_cell_measurement_reflns_used    2877
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      54.353
_cell_measurement_theta_min      3.720
_cell_volume                     2972.79(18)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14176
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        65.061
_diffrn_reflns_theta_max         65.061
_diffrn_reflns_theta_min         3.720
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    1.748
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0860 before and 0.0504 after correction. The Ratio of minimum to maximum transmission is 0.8754. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_description       plate
_exptl_crystal_F_000             1166
_exptl_crystal_size_max          0.141
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.028
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         2679
_refine_ls_number_restraints     342
_refine_ls_restrained_S_all      1.392
_refine_ls_R_factor_all          0.1427
_refine_ls_R_factor_gt           0.1009
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3140
_refine_ls_wR_factor_ref         0.3523
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1433
_reflns_number_total             2679
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc04860j2.cif
_cod_data_source_block           cx1022
_cod_depositor_comments
;Adding full bibliography for 1552713--1552722.cif.

 Adding full bibliography for 1552713--1552722.cif.
;
_cod_database_code               1552715
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.791
_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
 C9_$1-C8_$1 \\sim C7_$1-C8 \\sim C12-C7 \\sim C11-C10
 with sigma of 0.01
 C9_$1-C7_$1 \\sim C9-C9_$1 \\sim C9-C7 \\sim C8-C7 \\sim C8-C8_$1 \\sim
C8_$1-C7_$1 \\sim C7_$1-C10 ~
 C7-C10 \\sim C11-C7 \\sim C12-C11 \\sim C12-C11_$1 \\sim C11_$1-C7_$1
 with sigma of 0.01
 C12-C7 \\sim C10-C11
 with sigma of 0.01
 F1A-F1A_$3 \\sim F1A-F1A_$4 \\sim F1A_$3-F1A_$2 \\sim F1A_$2-F1A_$4
 with sigma of 0.04
 P1-F3 \\sim P1-F3_$3 \\sim P1-F1A \\sim P1-F1A_$3 \\sim P1-F1A_$2 \\sim
P1-F1A_$4
 with sigma of 0.02
3. Restrained planarity
 C7, C7_$1, C8_$1, C8, C9, C9_$1
 with sigma of 0.1
4. 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
5. Others
 Sof(F7A)=1-FVAR(1)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(F8A)=Sof(P2A)=0.5*(1-FVAR(2))
 Sof(F4)=Sof(F5)=Sof(F6)=Sof(F8)=Sof(P2)=0.5*FVAR(2)
 Sof(F7)=FVAR(1)
 Fixed Sof: C8(0.5) H8(0.5) C9(0.5) H9(0.5) C10(0.25) H10(0.25) C11(0.5)
 H11(0.5) C12(0.25) H12(0.25) H18B(0.5) H18C(0.5) F1(0.25) F1A(0.5) F2(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
6.b Me refined with riding coordinates:
 C18(H18A,H18B,H18C)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C16(H16), C17(H17)
;
_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 = 626.7 Ang^3^ [21.0%]
Total electron count / cell = 171.6
;
_shelx_res_checksum              35507
_shelx_fab_checksum              45095
_olex2_date_sample_data_collection 2017-07-17
_olex2_date_sample_submission    2017-07-07
_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 cx1022
_olex2_submission_special_instructions 'No special instructions were received'