Asymmetric Annulation of Donor-Acceptor Cyclopropanes with Dienes.
Xu, Hao; Hu, Jiang-Lin; Wang, Lijia; Liao, Saihu; Tang, Yong; Journal of the American Chemical Society 137 (2015) 8006–8009; doi:10.1021/jacs.5b04429

data_4123837
_publ_section_title
;
 Asymmetric Annulation of Donor-Acceptor Cyclopropanes with Dienes.
;
_journal_issue                   25
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8006
_journal_page_last               8009
_journal_paper_doi               10.1021/jacs.5b04429
_journal_volume                  137
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_sum            'C40 H52 O6'
_chemical_formula_weight         628.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 91.6640(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0266(2)
_cell_length_b                   13.4830(2)
_cell_length_c                   11.3181(2)
_cell_measurement_reflns_used    5364
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      69.22
_cell_measurement_theta_min      3.91
_cell_volume                     1681.97(5)
_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-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8967
_diffrn_reflns_point_group_measured_fraction_full 0.856
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.769
_diffrn_reflns_theta_min         3.907
_exptl_absorpt_coefficient_mu    0.649
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_correction_T_min  0.569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
; 
 Flack x determined using 2005 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.02(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         5321
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1018P)^2^+0.1760P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1422
_refine_ls_wR_factor_ref         0.1439
_reflns_Friedel_coverage         0.658
_reflns_Friedel_fraction_full    0.720
_reflns_Friedel_fraction_max     0.696
_reflns_number_gt                5191
_reflns_number_total             5321
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b04429_si_004.cif
_cod_data_source_block           cu_dm14241_0m
_cod_depositor_comments
'Adding full bibliography for 4123835--4123839.cif.'
_cod_database_code               4123837
_shelx_estimated_absorpt_t_min   0.819
_shelx_estimated_absorpt_t_max   0.870
_shelxl_version_number           2014-3
_shelx_res_checksum              77900
_shelx_hkl_checksum              47576