α-Glucosidase Inhibitors from Malbranchea flavorosea.
Verastegui-Omaña, Brisa; Rebollar-Ramos, Daniela; Pérez-Vásquez, Araceli; Martínez, Ana Laura; Madariaga-Mazón, Abraham; Flores-Bocanegra, Laura; Mata, Rachel; Journal of natural products 80 (2017) 190–195; doi:10.1021/acs.jnatprod.6b00977

data_1545009
_publ_section_title
;
 \a-Glucosidase Inhibitors from Malbranchea flavorosea.
;
_journal_issue                   1
_journal_name_full               'Journal of natural products'
_journal_page_first              190
_journal_page_last               195
_journal_paper_doi               10.1021/acs.jnatprod.6b00977
_journal_volume                  80
_journal_year                    2017
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C11 H12 O5, 0.5(H2 O)'
_chemical_formula_sum            'C11 H13 O5.5'
_chemical_formula_weight         233.21
_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'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 95.201(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.881(3)
_cell_length_b                   7.2139(11)
_cell_length_c                   7.1436(11)
_cell_measurement_reflns_used    6448
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      68.26
_cell_measurement_theta_min      4.25
_cell_volume                     1071.6(3)
_computing_cell_refinement       'APEX3 v2016.1 (Bruker, 2014)'
_computing_data_collection       'APEX3 v2016.1 (Bruker, 2014)'
_computing_data_reduction        'SAINT V8.37A  (Bruker, 2014)'
_computing_molecular_graphics    'XP V 5.1 (Bruker, 1998)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Bruker, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 52.0833
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Bruker D8 Venture \k-geometry diffractometer 208039-01'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1126
_diffrn_reflns_av_unetI/netI     0.0704
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6426
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.255
_diffrn_reflns_theta_min         4.252
_diffrn_source                   'micro-focus X-ray source'
_exptl_absorpt_coefficient_mu    0.996
_exptl_absorpt_correction_T_max  0.8612
_exptl_absorpt_correction_T_min  0.7801
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL (Sheldrick, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       Prism
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.403
_exptl_crystal_size_mid          0.256
_exptl_crystal_size_min          0.188
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
; 
 Classical Flack method preferred over Parsons because s.u. lower. 
;
_refine_ls_abs_structure_Flack   0.2(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         1971
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0501
_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^)+(0.0953P)^2^+0.2329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1293
_reflns_Friedel_coverage         0.839
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                1959
_reflns_number_total             1971
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np6b00977_si_003.cif
_cod_data_source_block           077XYZ16
_cod_depositor_comments
;
Adding full bibliography for 1545008--1545009.cif.

2019-03-26
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        1071.7(3)
_cod_original_formula_moiety     ' 2(C11 H12 O5), H2 O'
_cod_original_formula_sum        'C22 H26 O11'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     466.43
_cod_database_code               1545009
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.690
_shelx_estimated_absorpt_t_max   0.835
_shelx_res_checksum              77974
_shelx_hkl_checksum              21962