On the stereochemistry of acetylide additions to highly functionalized biphenylcarbaldehydes and multi-component cyclization of 1,n-diynes. Syntheses of dibenzocyclooctadiene lignans
Gong, Wei; Singidi, Ramakrishna Reddy; Gallucci, Judith C.; RajanBabu, T. V.; Chemical Science 3 (2012) 1221–; doi:10.1039/c2sc00920j

data_1514984
_publ_section_title
;
 On the stereochemistry of acetylide additions to highly functionalized
 biphenylcarbaldehydes and multi-component cyclization of 1,n-diynes.
 Syntheses of dibenzocyclooctadiene lignans
;
_journal_issue                   4
_journal_name_full               'Chemical Science'
_journal_page_first              1221
_journal_paper_doi               10.1039/c2sc00920j
_journal_volume                  3
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C35 H41 B1 O7'
_chemical_formula_sum            'C35 H41 B O7'
_chemical_formula_weight         584.49
_chemical_name_common            'RajanBabu 1635'
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_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     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2008-04-09T14:16:08-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                83.045(1)
_cell_angle_beta                 83.617(1)
_cell_angle_gamma                81.899(1)
_cell_formula_units_Z            2
_cell_length_a                   8.0671(1)
_cell_length_b                   12.5459(1)
_cell_length_c                   15.4229(2)
_cell_measurement_reflns_used    5345
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.037
_cell_measurement_wavelength     0.71073
_cell_volume                     1526.94(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_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, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_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 Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.106575
_diffrn_orient_matrix_UB_12      0.668118E-1
_diffrn_orient_matrix_UB_13      -0.7053E-3
_diffrn_orient_matrix_UB_21      -0.54026E-2
_diffrn_orient_matrix_UB_22      -0.275151E-1
_diffrn_orient_matrix_UB_23      0.759671E-1
_diffrn_orient_matrix_UB_31      0.391859E-1
_diffrn_orient_matrix_UB_32      0.508219E-1
_diffrn_orient_matrix_UB_33      0.0137
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            39388
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         2.23
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular plate'
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.165
_refine_diff_density_min         -0.184
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         5373
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+0.4503P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0954
_reflns_number_gt                4532
_reflns_number_total             5373
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2sc00920j.txt
_cod_data_source_block           RajanBabu1635
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1514984