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_1552713
_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 S2, C12 H14 N2, 3(F6 P)'
_chemical_formula_sum            'C44 H42 F18 N6 P3 S2'
_chemical_formula_weight         1153.86
_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             2017-12-12
_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                   14.8195(8)
_cell_length_b                   20.8662(12)
_cell_length_c                   9.5394(7)
_cell_measurement_reflns_used    4318
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      63.810
_cell_measurement_theta_min      3.659
_cell_volume                     2949.8(3)
_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      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.915
_diffrn_measured_fraction_theta_max 0.996
_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  0.0471
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_Laue_measured_fraction_full 0.915
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9385
_diffrn_reflns_point_group_measured_fraction_full 0.915
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         63.824
_diffrn_reflns_theta_min         3.658
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    2.411
_exptl_absorpt_correction_T_max  0.7524
_exptl_absorpt_correction_T_min  0.5422
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1137 before and 0.0766 after correction. The Ratio of minimum to maximum transmission is 0.7206. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       plate
_exptl_crystal_F_000             1174
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         2597
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1185
_refine_ls_R_factor_gt           0.1123
_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^)+(0.1249P)^2^+17.7906P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2975
_refine_ls_wR_factor_ref         0.3018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2309
_reflns_number_total             2597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc04860j2.cif
_cod_data_source_block           cx1132
_cod_depositor_comments
;Adding full bibliography for 1552713--1552722.cif.

 Adding full bibliography for 1552713--1552722.cif.
;
_cod_database_code               1552713
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.573
_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. Others
 Fixed Sof: H9A(0.5) H9B(0.5) H9C(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C8(H8), C10(H10), C11(H11), C13(H13), C14(H14)
3.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C)
;
_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 = 812.6 Ang^3^ [27.5%]
Total electron count / cell = 206.4
;
_shelx_res_checksum              80867
_shelx_fab_checksum              13563
_olex2_date_sample_data_collection 2017-12-11
_olex2_date_sample_submission    2017-12-06
_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 cx1132
_olex2_submission_special_instructions 'No special instructions were received'