An unusual oligomerization/oxidation reaction of a 3-boron-substituted 1-phenylbuta-1,3-diene produces 6,9,16,19-tetraphenyl-5,15-distyryl-3,13,25,26-tetraoxa-2,12-diborapentacyclo[16.2.2.2^8,11^.1^2,5^.1^12,15^]hexacosa-1(20),7,10,17-tetraene
De, Subhasis; Day, Cynthia S.; Welker, Mark E.; Acta Crystallographica Section C 63 (2007) o729–o730; doi:10.1107/S0108270107050986

data_2016330
_publ_section_title
;An unusual oligomerization/oxidation reaction of a 3-boron-substituted
 1-phenylbuta-1,3-diene produces
 6,9,16,19-tetraphenyl-5,15-distyryl-3,13,25,26-tetraoxa-2,12-diborapentacyclo[16.2.2.2^8,11^.1^2,5^.1^12,15^]hexacosa-1(20),7,10,17-tetraene
;
_journal_coeditor_code           GG3111
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o729
_journal_page_last               o730
_journal_paper_doi               10.1107/S0108270107050986
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C60 H54 B2 O4'
_chemical_formula_moiety         'C60 H54 B2 O4'
_chemical_formula_sum            'C60 H54 B2 O4'
_chemical_formula_weight         860.65
_chemical_name_systematic
;6,9,16,19-tetraphenyl-5,15-distyryl-3,13,25,26-tetraoxa-2,12-
diborapentacyclo[16.2.2.2^8,11^.1^2,5^.1^12,15^]hexacosa-1(20),7,10,17-tetraene
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL-PC
_cell_angle_alpha                90.00
_cell_angle_beta                 101.764(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.212(3)
_cell_length_b                   6.0975(13)
_cell_length_c                   29.028(6)
_cell_measurement_reflns_used    1350
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      18.810
_cell_measurement_theta_min      3.824
_cell_volume                     2289.4(9)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  'SHELXTL (Bruker, 2001)'
_computing_structure_refinement  'SHELXTL (Bruker, 2001)'
_computing_structure_solution    'SHELXTL (Bruker, 2001)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0824
_diffrn_reflns_av_sigmaI/netI    0.0796
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            13447
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         3.82
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996))'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.16
_refine_diff_density_min         -0.15
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.850
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         3260
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.850
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0438P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1074
_reflns_number_gt                1769
_reflns_number_total             3260
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gg3111.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2016330
_cod_database_fobs_code          2016330