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_4135422
_publ_section_title
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 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         'C40 H40 N4 O4, 2(F6 P)'
_chemical_formula_sum            'C40 H40 F12 N4 O4 P2'
_chemical_formula_weight         930.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                90
_cell_angle_beta                 90.006(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.155(2)
_cell_length_b                   23.664(5)
_cell_length_c                   20.711(4)
_cell_measurement_reflns_used    9360
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.78
_cell_measurement_theta_min      2.61
_cell_volume                     5957(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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0451
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36620
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.023
_diffrn_reflns_theta_max         25.023
_diffrn_reflns_theta_min         1.884
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0558 before and 0.0464 after correction.
The Ratio of minimum to maximum transmission is 0.8898.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.038
_exptl_crystal_description       block
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.503
_exptl_crystal_size_mid          0.279
_exptl_crystal_size_min          0.158
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.524
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         5188
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.524
_refine_ls_R_factor_all          0.1895
_refine_ls_R_factor_gt           0.1412
_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          0.3842
_refine_ls_wR_factor_ref         0.4331
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2739
_reflns_number_total             5188
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c07148_si_006.cif
_cod_data_source_block           b
_cod_database_code               4135422
_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. Uiso/Uaniso restraints and constraints
Uanis(C9) = Uanis(C7)
Uanis(C16) = Uanis(C13) = Uanis(C10) = Uanis(C7)
3. Others
 Fixed Sof: P2(0.5) P1(0.5) H12(0.5) H9(0.5) H10(0.5) H13(0.5) O1A(0.5)
 O1(0.5) O2(0.5) O2A(0.5) F2(0.5) F8(0.5) F9(0.5) F3(0.5) F4(0.5) F7(0.5)
 F5(0.5) F10(0.5) F6(0.5) C17(0.5) H17A(0.5) H17B(0.5) H17C(0.5) C20A(0.5)
 H20A(0.5) H20B(0.5) H20C(0.5) C20(0.5) H20D(0.5) H20E(0.5) H20F(0.5) C17A(0.5)
 H17D(0.5) H17E(0.5) H17F(0.5) F11(0.5) F1(0.5) F12(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C4(H4A,H4B)
4.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C6(H6), C18(H18), C5(H5), C2(H2), C12(H12), C9(H9), C15(H15),
 C3(H3), C10(H10), C1(H1), C13(H13)
4.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C20A(H20A,H20B,H20C), C20(H20D,H20E,H20F), C17A(H17D,
 H17E,H17F)
;
_shelx_res_checksum              80819
_shelx_hkl_checksum              84396
_shelx_fab_checksum              24177
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'