Double gamma-alkylation of allylic phosphorus ylides: a unique access to oxa-bicyclic[3.3.0] diene skeletons
Peng Wang; Saihu Liao; Jian-Bo Zhu; Yong Tang; Chem.Commun. 50 (2014) 808–; doi:10.1039/c3cc45286g

data_7110243
_publ_section_title
;
 Double gamma-alkylation of allylic phosphorus ylides: a unique access to
 oxa-bicyclic[3.3.0] diene skeletons
;
_journal_name_full               Chem.Commun.
_journal_page_first              808
_journal_paper_doi               10.1039/c3cc45286g
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C39 H35 Br O4.5 P'
_chemical_formula_weight         686.55
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.2700(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5869(5)
_cell_length_b                   35.5331(19)
_cell_length_c                   10.4715(6)
_cell_measurement_reflns_used    3994
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      44.974
_cell_measurement_theta_min      4.522
_cell_volume                     3457.1(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            20978
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    1.276
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74833
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1420
_exptl_crystal_size_max          0.342
_exptl_crystal_size_mid          0.223
_exptl_crystal_size_min          0.113
_refine_diff_density_max         0.730
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         6778
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+1.2662P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1241
_reflns_number_gt                4782
_reflns_number_total             6778
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc45286g.txt
_cod_data_source_block           cd211552
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C39 H35 Br O4.50 P'
_cod_database_code               7110243