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_1552720
_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         'C32 H28 N4 S, C12 H14 N2, 3(F6 P)'
_chemical_formula_sum            'C44 H42 F18 N6 P3 S'
_chemical_formula_weight         1121.80
_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             2017-12-08
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.8597(15)
_cell_length_b                   21.003(2)
_cell_length_c                   9.5902(9)
_cell_measurement_reflns_used    5573
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.666
_cell_measurement_theta_min      3.643
_cell_volume                     2993.1(5)
_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      99.95
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.919
_diffrn_measured_fraction_theta_max 0.960
_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  0.0833
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_Laue_measured_fraction_full 0.919
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12833
_diffrn_reflns_point_group_measured_fraction_full 0.919
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.662
_diffrn_reflns_theta_min         3.644
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    2.044
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.4849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1363 before and 0.0812 after correction. The Ratio of minimum to maximum transmission is 0.6443. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_description       needle
_exptl_crystal_F_000             1142
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.724
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.170
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2655
_refine_ls_number_restraints     325
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1497
_refine_ls_R_factor_gt           0.1358
_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^)+(0.1469P)^2^+25.6386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3484
_refine_ls_wR_factor_ref         0.3577
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2137
_reflns_number_total             2655
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc04860j2.cif
_cod_data_source_block           cx1122
_cod_depositor_comments
;Adding full bibliography for 1552713--1552722.cif.

 Adding full bibliography for 1552713--1552722.cif.
;
_cod_database_code               1552720
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.923
_shelx_estimated_absorpt_t_min   0.319
_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
 F9A-F7A \\sim F9A-F5A \\sim F7A-F8A \\sim F5A-F8A
 with sigma of 0.02
 P2-F9A \\sim P2-F7A \\sim P2-F5A \\sim P2-F6 \\sim P2-F4 \\sim P2-F8A
 with sigma of 0.01
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C9)=Sof(H9)=1-FVAR(1)
 Sof(S1A)=0.25*(1-FVAR(2))
 Sof(S1)=0.25*FVAR(2)
 Sof(C8)=Sof(H8)=FVAR(1)
 Sof(F5A)=Sof(F7A)=Sof(F8A)=Sof(F9A)=0.5*(1-FVAR(3))
 Sof(F5)=Sof(F7)=FVAR(2)
 Fixed Sof: H15A(0.5) H15B(0.5) H15C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13),
 C14(H14)
6.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
;
_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 = 754.1 Ang^3^ [25.6%]
Total electron count / cell = 197.6
;
_shelx_res_checksum              92695
_shelx_fab_checksum              44306
_olex2_date_sample_data_collection 2017-12-06
_olex2_date_sample_submission    2017-11-22
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id cx1122
_olex2_submission_special_instructions 'No special instructions were received'