Discrete Open-Shell Tris(bipyridinium radical cationic) Inclusion Complexes in the Solid State
Anamimoghadam, Ommid; Jones, Leighton O.; Cooper, James A.; Beldjoudi, Yassine; Nguyen, Minh T.; Liu, Wenqi; Krzyaniak, Matthew D.; Pezzato, Cristian; Stern, Charlotte L.; Patel, Hasmukh A.; Wasielewski, Michael R.; Schatz, George C.; Stoddart, J. Fraser; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c07148

data_4135420
_publ_section_title
;
 Discrete Open-Shell Tris(bipyridinium radical cationic) Inclusion
 Complexes in the Solid State
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c07148
_journal_year                    2020
_chemical_formula_moiety         '4(F6 P), C40 H40 N4 O4, 6(C2 H3 N)'
_chemical_formula_sum            'C52 H58 F24 N10 O4 P4'
_chemical_formula_weight         1466.96
_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             2020-06-27
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                112.990(2)
_cell_angle_beta                 93.419(2)
_cell_angle_gamma                105.009(2)
_cell_formula_units_Z            1
_cell_length_a                   10.9093(8)
_cell_length_b                   11.8788(9)
_cell_length_c                   14.0160(11)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.69
_cell_measurement_theta_min      2.75
_cell_volume                     1588.4(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            57137
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.692
_diffrn_reflns_theta_min         1.605
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.242
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6955
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0478 before and 0.0426 after correction.
The Ratio of minimum to maximum transmission is 0.9324.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_description       block
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.538
_exptl_crystal_size_mid          0.361
_exptl_crystal_size_min          0.224
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         8832
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+0.7061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.0977
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7728
_reflns_number_total             8832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c07148_si_003.cif
_cod_data_source_block           mo_meobb_0m
_cod_database_code               4135420
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.881
_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.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C18(H18), C16(H16), C7(H7), C10(H10), C17(H17), C19(H19), C11(H11),
 C12(H12), C13(H13)
2.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C9(H9A,H9B,H9C), C3(H3A,H3B,H3C), C23(H23A,H23B,H23C),
 C25(H25A,H25B,H25C)
;
_shelx_res_checksum              21270
_shelx_hkl_checksum              67694
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'