Extraordinary Redox Activities in Ladder-Type Conjugated Molecules Enabled by B ←N Coordination-Promoted Delocalization and Hyperconjugation.
Zhu, Congzhi; Ji, Xiaozhou; You, Di; Chen, Teresa L.; Mu, Anthony U.; Barker, Kayla P.; Klivansky, Liana M.; Liu, Yi; Fang, Lei; Journal of the American Chemical Society 140 (2018) 18173–18182; doi:10.1021/jacs.8b11337

data_4133577
_publ_section_title
;
 Extraordinary Redox Activities in Ladder-Type Conjugated Molecules
 Enabled by B \\leftarrow N Coordination-Promoted Delocalization and
 Hyperconjugation.
;
_journal_issue                   51
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18173
_journal_page_last               18182
_journal_paper_doi               10.1021/jacs.8b11337
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         '2(C20 H30 Co), C64 H52 B2 N4 S2'
_chemical_formula_sum            'C104 H112 B2 Co2 N4 S2'
_chemical_formula_weight         1621.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.245(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.8118(9)
_cell_length_b                   14.5805(8)
_cell_length_c                   17.8689(10)
_cell_measurement_reflns_used    9845
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      65.055
_cell_measurement_theta_min      3.925
_cell_volume                     4086.7(4)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0926
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25877
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        49.998
_diffrn_reflns_theta_max         49.998
_diffrn_reflns_theta_min         3.519
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.059
_exptl_absorpt_correction_T_max  0.5192
_exptl_absorpt_correction_T_min  0.3036
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1443 before and 0.0852 after correction. The Ratio of minimum to maximum transmission is 0.5847. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       needle
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.402
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         4125
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.383
_refine_ls_R_factor_all          0.1268
_refine_ls_R_factor_gt           0.1008
_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^)+29.4971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1696
_refine_ls_wR_factor_ref         0.1850
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3295
_reflns_number_total             4125
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b11337_si_003.cif
_cod_data_source_block           bph2cco
_cod_database_code               4133577
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.845
_shelx_estimated_absorpt_t_min   0.631
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C34 \\sim C35 \\sim C36 \\sim C40 \\sim C1 \\sim C2 \\sim C3 \\sim C10 \\sim
C11 \\sim C12 \\sim C16: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
3. Rigid body (RIGU) restrains
 C34, C35, C36, C40, C1, C2, C3, C10, C11, C12, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C14(H14), C15(H15), C22(H22),
 C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31),
  C32(H32)
4.b Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,
 H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              62002
_shelx_hkl_checksum              6499
_olex2_submission_special_instructions 'No special instructions were received'