Spin Frustration in the Triradical Trianion of a Naphthalenediimide Molecular Triangle.
Wu, Yilei; Krzyaniak, Matthew D.; Stoddart, J. Fraser; Wasielewski, Michael R.; Journal of the American Chemical Society 139 (2017) 2948–2951; doi:10.1021/jacs.7b00515

data_4125548
_publ_section_title
;
 Spin Frustration in the Triradical Trianion of a Naphthalenediimide
 Molecular Triangle.
;
_journal_issue                   8
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2948
_journal_page_last               2951
_journal_paper_doi               10.1021/jacs.7b00515
_journal_volume                  139
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C60 H42 N6 O12, 3(C10 H10 Co), 8(C2 H3 N)'
_chemical_formula_sum            'C106 H96 Co3 N14 O12'
_chemical_formula_weight         1934.75
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-12-17
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.753(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.489(3)
_cell_length_b                   27.457(5)
_cell_length_c                   14.100(2)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.145
_cell_measurement_theta_min      3.232
_cell_volume                     4675.6(16)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.998
_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  0.0321
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_Laue_measured_fraction_full 0.934
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            35421
_diffrn_reflns_point_group_measured_fraction_full 0.922
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         64.666
_diffrn_reflns_theta_min         3.219
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    4.699
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.5633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0738 before and 0.0407 after correction.
The Ratio of minimum to maximum transmission is 0.7485.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_description       block
_exptl_crystal_F_000             2014
_exptl_crystal_size_max          0.361
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.087
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 6602 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.0169(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1223
_refine_ls_number_reflns         15584
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0341
_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^)+(0.0563P)^2^+1.2603P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0899
_reflns_Friedel_coverage         0.931
_reflns_Friedel_fraction_full    0.910
_reflns_Friedel_fraction_max     0.974
_reflns_number_gt                14765
_reflns_number_total             15584
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b00515_si_002.cif
_cod_data_source_block           cx0197
_cod_depositor_comments          'Adding full bibliography for 4125548.cif.'
_cod_database_code               4125548
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.685
_shelx_estimated_absorpt_t_min   0.282
_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 Ternary CH refined with riding coordinates:
 C15(H15), C20(H20), C35(H35), C40(H40), C55(H55), C60(H60)
2.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C36(H36A,
 H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C56(H56A,H56B),
 C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B)
2.c Me refined with riding coordinates:
 C74(H74A,H74B,H74C)
2.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C9(H9), C10(H10), C23(H23), C24(H24), C29(H29), C30(H30),
 C43(H43), C44(H44), C49(H49), C50(H50), C77(H77), C78(H78), C79(H79), C80(H80),
  C81(H81), C82(H82), C83(H83), C84(H84), C85(H85), C86(H86), C87(H87),
 C88(H88), C89(H89), C90(H90), C91(H91), C92(H92), C93(H93), C94(H94), C95(H95),
  C96(H96), C97(H97), C98(H98), C99(H99), C100(H100), C101(H101), C102(H102),
 C103(H103), C104(H104), C105(H105), C106(H106)
2.e Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C), C64(H64A,H64B,H64C), C66(H66A,H66B,H66C), C68(H68A,H68B,
 H68C), C70(H70A,H70B,H70C), C72(H72A,H72B,H72C), C76(H76A,H76B,H76C)
;
_shelx_res_checksum              35739
_shelx_hkl_checksum              48621
_olex2_date_sample_data_collection 12/16/2014
_olex2_date_sample_submission    12/16/2014
_olex2_submission_original_sample_id cx0197
_olex2_submission_special_instructions 'No special instructions were received'