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_1552716
_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, 4(F6 P)'
_chemical_formula_sum            'C36 H32 F24 N4 P4'
_chemical_formula_weight         1100.53
_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             2017-09-19
_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                 91.831(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.4563(11)
_cell_length_b                   20.125(3)
_cell_length_c                   13.948(2)
_cell_measurement_reflns_used    6342
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.030
_cell_measurement_theta_min      4.394
_cell_volume                     2091.9(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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0346
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12508
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        65.074
_diffrn_reflns_theta_max         65.074
_diffrn_reflns_theta_min         3.857
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    3.004
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6070
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1298 before and 0.0465 after correction. The Ratio of minimum to maximum transmission is 0.8065. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_description       needle
_exptl_crystal_F_000             1104
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.473
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.019
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         3544
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0447P)^2^+2.8834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1248
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2993
_reflns_number_total             3544
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc04860j2.cif
_cod_data_source_block           cx1072
_cod_depositor_comments
;Adding full bibliography for 1552713--1552722.cif.

 Adding full bibliography for 1552713--1552722.cif.
;
_cod_original_cell_volume        2092.0(5)
_cod_database_code               1552716
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.331
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
2. Rigid bond restraints
 C13, C19, F3, F3A, F4, F4A, F5, F5A, F6, F6A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C13 \\sim C19 \\sim F3 \\sim F3A \\sim F4 \\sim F4A \\sim F5 \\sim F5A \\sim F6
\\sim F6A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
 Fixed Sof: H1BC(0.5) H1BD(0.5) H1AA(0.5) H1AB(0.5) H12C(0.5) H12D(0.5)
 H12A(0.5) H12B(0.5) C13(0.5) C14(0.5) H14(0.5) C15(0.5) H15(0.5) C16(0.5)
 H16(0.5) C17(0.5) C18(0.5) H18(0.5) C19(0.5) C20(0.5) H20(0.5) C21(0.5)
 H21(0.5) C22(0.5) C23(0.5) H23(0.5) C24(0.5) H24(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1BC,H1BD), C1(H1AA,H1AB), C12(H12C,H12D), C12(H12A,H12B)
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), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24)
;
_shelx_res_checksum              61283
_olex2_date_sample_data_collection 2017-09-18
_olex2_date_sample_submission    2017-09-18
_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 cx1072
_olex2_submission_special_instructions 'No special instructions were received'