Synthesis of a Small-Molecule Library with Skeletal Diversity from Hemslecin A via the Reaction-Discovery Strategy.
Ren, Jian; Shi, Xin; Li, Xiao-Nian; Li, Lai-Wei; Su, Jia; Shao, Li-Dong; Zhao, Qin-Shi; Organic letters 18 (2016) 3948–3951; doi:10.1021/acs.orglett.6b01654

data_1555631
_publ_section_title
;
 Synthesis of a Small-Molecule Library with Skeletal Diversity from
 Hemslecin A via the Reaction-Discovery Strategy.
;
_journal_issue                   16
_journal_name_full               'Organic letters'
_journal_page_first              3948
_journal_page_last               3951
_journal_paper_doi               10.1021/acs.orglett.6b01654
_journal_volume                  18
_journal_year                    2016
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C24 H30 O3'
_chemical_formula_sum            'C24 H30 O3'
_chemical_formula_weight         366.48
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 99.799(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.2298(14)
_cell_length_b                   12.745(3)
_cell_length_c                   12.605(3)
_cell_measurement_reflns_used    3729
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.98
_cell_measurement_theta_min      2.29
_cell_volume                     986.2(4)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10207
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.119
_diffrn_reflns_theta_min         1.639
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       plate
_exptl_crystal_F_000             396
_exptl_crystal_size_max          1.000
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.070
_exptl_transmission_factor_max   0.7458
_exptl_transmission_factor_min   0.6681
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.195
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 1899 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.2(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         5191
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0673P)^2^+0.0090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1118
_reflns_Friedel_coverage         0.882
_reflns_Friedel_fraction_full    0.974
_reflns_Friedel_fraction_max     0.956
_reflns_number_gt                4580
_reflns_number_total             5191
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b01654_si_007.cif
_cod_data_source_block           mo_frj247_0m
_cod_original_cell_volume        986.3(4)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1555631
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.925
_shelx_estimated_absorpt_t_max   0.994
_shelx_res_checksum              19112
_shelx_hkl_checksum              73973