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_7110244
_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            'C46 H46 Cl2 O7 Rh2'
_chemical_formula_weight         987.55
_chemical_name_systematic
;
?
;
_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                 105.4680(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.3366(13)
_cell_length_b                   14.6059(12)
_cell_length_c                   17.7679(14)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      30.46
_cell_measurement_theta_min      2.38
_cell_volume                     4086.1(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            39041
_diffrn_reflns_theta_full        30.47
_diffrn_reflns_theta_max         30.47
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.991
_exptl_absorpt_correction_T_max  0.9614
_exptl_absorpt_correction_T_min  0.7554
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.356
_refine_diff_density_min         -0.992
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         12383
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+4.4825P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0827
_reflns_number_gt                9877
_reflns_number_total             12383
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc45286g.txt
_cod_data_source_block           mo_dm12338_0m
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7110244