Conformation and reactivity in dibenzocyclooctadienes (DBCOD). A general approach to the total synthesis of fully substituted DBCOD lignans via borostannylative cyclization of α,ω-diynes
Gong, Wei; RajanBabu, T. V.; Chemical Science 4 (2013) 3979–; doi:10.1039/c3sc51751a

data_1514551
_publ_section_title
;
 Conformation and reactivity in dibenzocyclooctadienes (DBCOD). A general
 approach to the total synthesis of fully substituted DBCOD lignans via
 borostannylative cyclization of \a,\w-diynes
;
_journal_issue                   10
_journal_name_full               'Chemical Science'
_journal_page_first              3979
_journal_paper_doi               10.1039/c3sc51751a
_journal_volume                  4
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C45 H63 B1 O10 Si1 Sn1'
_chemical_formula_sum            'C45 H63 B O10 Si Sn'
_chemical_formula_weight         921.54
_chemical_name_common            'RajanBabu 1872'
_chemical_name_systematic
;
?
;
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_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
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_audit_creation_date             2011-12-30T14:04:54-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                96.233(1)
_cell_angle_beta                 98.572(1)
_cell_angle_gamma                100.371(1)
_cell_formula_units_Z            2
_cell_length_a                   11.9576(1)
_cell_length_b                   12.6539(1)
_cell_length_c                   16.2477(1)
_cell_measurement_reflns_used    10832
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.018
_cell_measurement_wavelength     0.71073
_cell_volume                     2367.98(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.231171E-1
_diffrn_orient_matrix_UB_12      0.70505E-2
_diffrn_orient_matrix_UB_13      0.566999E-1
_diffrn_orient_matrix_UB_21      0.781066E-1
_diffrn_orient_matrix_UB_22      -0.93512E-2
_diffrn_orient_matrix_UB_23      0.262286E-1
_diffrn_orient_matrix_UB_31      0.28538E-1
_diffrn_orient_matrix_UB_32      0.802797E-1
_diffrn_orient_matrix_UB_33      0.69178E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            71828
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.76
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.617
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'trapezoidal plate'
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.246
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         10850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+1.7606P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1099
_reflns_number_gt                8712
_reflns_number_total             10850
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3sc51751a.txt
_cod_data_source_block           RajanBabu1872
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1514551