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_4135419
_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         '2(F6 P), C3 H2 S2, C20 H20 N2 O2, C2 H3 N'
_chemical_formula_sum            'C25 H25 F12 N3 O2 P2 S2'
_chemical_formula_weight         753.54
_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     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                64.875(2)
_cell_angle_beta                 77.838(2)
_cell_angle_gamma                65.854(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4509(4)
_cell_length_b                   12.2972(4)
_cell_length_c                   13.7176(5)
_cell_measurement_reflns_used    9755
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.09
_cell_measurement_theta_min      2.32
_cell_volume                     1455.03(10)
_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      100.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_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  0.0423
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23652
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.195
_diffrn_reflns_theta_min         1.641
_exptl_absorpt_coefficient_mu    0.403
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0657 before and 0.0488 after correction.
The Ratio of minimum to maximum transmission is 0.8898.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.720
_exptl_crystal_description       block
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.107
_exptl_crystal_size_mid          0.039
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         7081
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0425P)^2^+1.0168P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1064
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5420
_reflns_number_total             7081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c07148_si_004.cif
_cod_data_source_block           meobb_ttf
_cod_database_code               4135419
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.958
_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), C10(H10), C16(H16), C19(H19), C5(H5), C18(H18), C17(H17), C11(H11),
 C12(H12), C13(H13), C25(H25), C24(H24)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C21(H21A,H21B,H21C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              54358
_shelx_hkl_checksum              14583
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'