Electron Delocalization in Reduced Forms of 2-(BMes2)pyrene and 2,7-Bis(BMes2)pyrene.
Ji, Lei; Edkins, Robert M.; Lorbach, Andreas; Krummenacher, Ivo; Brückner, Charlotte; Eichhorn, Antonius; Braunschweig, Holger; Engels, Bernd; Low, Paul J.; Marder, Todd B.; Journal of the American Chemical Society 137 (2015) 6750–6753; doi:10.1021/jacs.5b03805

data_4123702
_publ_section_title
;
 Electron Delocalization in Reduced Forms of 2-(BMes2)pyrene and
 2,7-Bis(BMes2)pyrene.
;
_journal_issue                   21
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6750
_journal_page_last               6753
_journal_paper_doi               10.1021/jacs.5b03805
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C34 H31 B'
_chemical_formula_sum            'C34 H31 B'
_chemical_formula_weight         450.40
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-11-09
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.884(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.335(3)
_cell_length_b                   8.8033(18)
_cell_length_c                   23.422(5)
_cell_measurement_reflns_used    4427
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.54
_cell_measurement_theta_min      2.47
_cell_volume                     2537.5(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0581
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            22556
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.755
_diffrn_reflns_theta_min         1.743
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8343
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1374 before and 0.0594 after correction.
The Ratio of minimum to maximum transmission is 0.8343.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_description       plate
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.456
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.087
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         5389
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0558
_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^)+(0.0553P)^2^+1.2931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1236
_refine_ls_wR_factor_ref         0.1450
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3555
_reflns_number_total             5389
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b03805_si_002.cif
_cod_data_source_block           cmpd_B1
_cod_depositor_comments
'Adding full bibliography for 4123702--4123707.cif.'
_cod_original_cell_volume        2537.5(9)
_cod_database_code               4123702
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.971
_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.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C14(H14), C30(H30), C4(H4), C11(H11), C12(H12), C9(H9),
 C7(H7), C28(H28), C21(H21), C19(H19), C8(H8)
2.b Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C25(H25A,H25B,H25C), C33(H33A,H33B,H33C), C32(H32A,H32B,
 H32C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              62342
_shelx_hkl_checksum              19157
_olex2_submission_special_instructions 'No special instructions were received'