Endophytic <i>Akanthomyces</i> sp. LN303 from Edelweiss Produces Emestrin and Two New 2-Hydroxy-4 Pyridone Alkaloids.
Oberhofer, Martina; Wackerlig, Judith; Zehl, Martin; Büyük, Havva; Cao, Jia Jian; Prado-Roller, Alexander; Urban, Ernst; Zotchev, Sergey B.; ACS omega 6 (2021) 2184–2191; doi:10.1021/acsomega.0c05472

data_4518480
_publ_section_title
;
 Endophytic <i>Akanthomyces</i> sp. LN303 from Edelweiss Produces Emestrin
 and Two New 2-Hydroxy-4 Pyridone Alkaloids.
;
_journal_issue                   3
_journal_name_full               'ACS omega'
_journal_page_first              2184
_journal_page_last               2191
_journal_paper_doi               10.1021/acsomega.0c05472
_journal_volume                  6
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C27 H22 N2 O10 S2, 2(C H4 O)'
_chemical_formula_sum            'C29 H30 N2 O12 S2'
_chemical_formula_weight         662.67
_chemical_name_systematic
;
(13R,15aS,16S,111R,111aR,2S)-111,34,2-trihydroxy-56-methoxy-12-
methyl-11,12,13,14,15a,16-hexahydro-111H-4,7-dioxa-1(3,6)-3,11a-
epidithiooxepino[3',4':4,5]pyrrolo[1,2-a]pyrazina-3,5(1,3)-
dibenzenacycloheptaphane-11,14,6-trione
;
_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
_audit_creation_date             2020-03-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.357(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0970(12)
_cell_length_b                   7.7388(8)
_cell_length_c                   15.2512(15)
_cell_measurement_reflns_used    7082
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      29.75
_cell_measurement_theta_min      2.96
_cell_volume                     1412.6(2)
_computing_cell_refinement       'SAINT V8.38A (2016)'
_computing_data_collection       APEX3
_computing_data_reduction        'SAINT V8.38A (2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1639
_diffrn_reflns_av_unetI/netI     0.0994
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            73456
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.114
_diffrn_reflns_theta_min         2.321
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.261
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1036 before and 0.0873 after correction. 
The Ratio of minimum to maximum transmission is 0.8641. 
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       block
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
;
 Flack x determined using 2073 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.07(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         8218
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1094
_refine_ls_R_factor_gt           0.0609
_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^)+(0.0456P)^2^+1.4457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1403
_reflns_Friedel_coverage         0.858
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                5816
_reflns_number_total             8218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c05472_si_002.cif
_cod_data_source_block           mo_mo_emestrin_a1_p21
_cod_database_code               4518480
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.979