Total Synthesis of Rubriflordilactone A.
Li, Jian; Yang, Peng; Yao, Ming; Deng, Jun; Li, Ang; Journal of the American Chemical Society  (2014) 141113160240003–; doi:10.1021/ja5092563

data_4122934
_publ_section_title
;
 Total Synthesis of Rubriflordilactone A.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              141113160240003
_journal_paper_doi               10.1021/ja5092563
_journal_year                    2014
_chemical_formula_sum            'C17 H17 Br O3'
_chemical_formula_weight         349.21
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                104.136(4)
_cell_angle_beta                 94.884(5)
_cell_angle_gamma                93.828(5)
_cell_formula_units_Z            2
_cell_length_a                   6.7558(15)
_cell_length_b                   8.971(2)
_cell_length_c                   12.667(3)
_cell_measurement_reflns_used    1300
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      44.318
_cell_measurement_theta_min      6.077
_cell_volume                     738.7(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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.009
_diffrn_measured_fraction_theta_max 1.011
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_Laue_measured_fraction_full 1.009
_diffrn_reflns_Laue_measured_fraction_max 1.011
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4252
_diffrn_reflns_point_group_measured_fraction_full 1.009
_diffrn_reflns_point_group_measured_fraction_max 1.011
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         2.351
_exptl_absorpt_coefficient_mu    2.790
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6047
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.113
_refine_diff_density_max         1.109
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2711
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0961P)^2^+2.0348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1748
_refine_ls_wR_factor_ref         0.1835
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2184
_reflns_number_total             2711
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5092563_si_002.cif
_cod_data_source_block           cd214602
_cod_database_code               4122934
_shelxl_version_number           2013-4
_shelx_res_checksum              72053
_shelx_hkl_checksum              55533