Efficient Enantioselective Syntheses of (+)-Dalesconol A and B.
Zhao, Guoqing; Xu, Guangqing; Qian, Chao; Tang, Wenjun; Journal of the American Chemical Society 139 (2017) 3360–3363; doi:10.1021/jacs.7b00783

data_4125453
_publ_section_title
;
 Efficient Enantioselective Syntheses of (+)-Dalesconol A and B.
;
_journal_issue                   9
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3360
_journal_page_last               3363
_journal_paper_doi               10.1021/jacs.7b00783
_journal_volume                  139
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C32 H27 Br O6'
_chemical_formula_sum            'C32 H27 Br O6'
_chemical_formula_weight         587.44
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4158(3)
_cell_length_b                   12.3181(4)
_cell_length_c                   20.3632(7)
_cell_measurement_reflns_used    5610
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      64.29
_cell_measurement_theta_min      4.19
_cell_volume                     2612.66(14)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 VENTURE CMOS photon 100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0753
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17180
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        65.069
_diffrn_reflns_theta_max         65.069
_diffrn_reflns_theta_min         4.194
_exptl_absorpt_coefficient_mu    2.529
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       block
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 1280 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.020(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         4401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0492P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0966
_reflns_Friedel_coverage         0.744
_reflns_Friedel_fraction_full    0.979
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                3548
_reflns_number_total             4401
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b00783_si_002.cif
_cod_data_source_block           t_a
_cod_depositor_comments          'Adding full bibliography for 4125453.cif.'
_cod_database_code               4125453
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.632
_shelx_estimated_absorpt_t_max   0.786
_shelx_res_checksum              22652
_shelx_hkl_checksum              97364