Improved Synthesis and Determination of the Biologically Active Diastereomer of YK11
Kanno, Yuichiro; Kusakabe, Taichi; Saito, Nao; Kikkawa, Shoko; Takahashi, Keisuke; Azumaya, Isao; Nemoto, Kiyomitsu; Kato, Keisuke; Molbank 2020 (2020) M1125–; doi:10.3390/M1125

data_1558005
_publ_section_title
;
 Improved Synthesis and Determination of the Biologically Active
 Diastereomer of YK11
;
_journal_issue                   2
_journal_name_full               Molbank
_journal_page_first              M1125
_journal_paper_doi               10.3390/M1125
_journal_volume                  2020
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C25 H34 O6'
_chemical_formula_sum            'C25 H34 O6'
_chemical_formula_weight         430.54
_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 97.4360(13)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   15.7937(3)
_cell_length_b                   7.49440(10)
_cell_length_c                   20.8812(2)
_cell_measurement_reflns_used    26467
_cell_measurement_temperature    93
_cell_measurement_theta_max      73.10
_cell_measurement_theta_min      2.80
_cell_volume                     2450.80(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            29206
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.249
_diffrn_reflns_theta_min         2.822
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.670
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             928.00
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.070
_platon_squeeze_details
;
Highly disordered solvent, which located in channels along [010], was unable to be modeled. 
As the identification of disordered solvent molecules riding on the center of symmetry was 
failed in the refinement of void space, PLATON/SQUEEZE program was applied.
PLATON/SQUEEZE shows the total potential solvent accessible void 
volume is 270 A^3^ and residual electrons count 76 in the unit cell.
;
_refine_diff_density_max         0.32
_refine_diff_density_min         -0.31
_refine_ls_abs_structure_details
;
 Flack x determined using 3806 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     798
_refine_ls_number_reflns         8612
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0908P)^2^+0.2519P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1136
_reflns_Friedel_coverage         0.828
_reflns_Friedel_fraction_full    0.955
_reflns_Friedel_fraction_max     0.954
_reflns_number_gt                8505
_reflns_number_total             8612
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            CrystalStructure_200418.cif
_cod_data_source_block           YK-11
_cod_database_code               1558005
_shelx_res_checksum              93569
_shelx_hkl_checksum              71518