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_1555630
_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         'C28 H38 O8, H2 O'
_chemical_formula_sum            'C28 H40 O9'
_chemical_formula_weight         520.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 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                 91.171(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.073(6)
_cell_length_b                   7.8003(19)
_cell_length_c                   29.094(7)
_cell_measurement_reflns_used    9166
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.59
_cell_volume                     5916(2)
_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 0.992
_diffrn_measured_fraction_theta_max 0.964
_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  0.0613
_diffrn_reflns_av_unetI/netI     0.0899
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            31206
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.963
_diffrn_reflns_theta_min         0.700
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_description       prism
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.670
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.280
_exptl_transmission_factor_max   0.7460
_exptl_transmission_factor_min   0.5378
_platon_squeeze_details
;
;
_refine_diff_density_max         1.004
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details
;
 Flack x determined using 4215 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.5(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     684
_refine_ls_number_reflns         15773
_refine_ls_number_restraints     693
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1352
_refine_ls_R_factor_gt           0.1209
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1499P)^2^+40.1750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3218
_refine_ls_wR_factor_ref         0.3308
_reflns_Friedel_coverage         0.781
_reflns_Friedel_fraction_full    0.940
_reflns_Friedel_fraction_max     0.865
_reflns_number_gt                13002
_reflns_number_total             15773
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b01654_si_010.cif
_cod_data_source_block           mo_frj165_0m-sr
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               1555630
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.944
_shelx_estimated_absorpt_t_max   0.976
_shelx_res_checksum              29627
_shelx_hkl_checksum              81758