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_1555627
_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 ad
_chemical_formula_moiety         'C28 H38 O8, C H2 Cl2'
_chemical_formula_sum            'C29 H40 Cl2 O8'
_chemical_formula_weight         587.51
_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                 90.932(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.6253(10)
_cell_length_b                   11.8707(16)
_cell_length_c                   16.229(2)
_cell_measurement_reflns_used    8499
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.91
_cell_measurement_theta_min      2.51
_cell_volume                     1468.8(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.937
_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  0.0261
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16251
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.969
_diffrn_reflns_theta_min         2.126
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       plate
_exptl_crystal_F_000             624
_exptl_crystal_size_max          1.120
_exptl_crystal_size_mid          0.900
_exptl_crystal_size_min          0.060
_exptl_transmission_factor_max   0.7462
_exptl_transmission_factor_min   0.6452
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Flack x determined using 3280 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         8373
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.087
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+0.1086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0849
_reflns_Friedel_coverage         0.839
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.857
_reflns_number_gt                7750
_reflns_number_total             8373
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b01654_si_009.cif
_cod_data_source_block           mo_frj269_0m
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1555627
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.753
_shelx_estimated_absorpt_t_max   0.984
_shelx_res_checksum              55366
_shelx_hkl_checksum              53738