Crystal structure of natural phaeosphaeride A
Abzianidze, Victoria V.; Poluektova, Ekaterina V.; Bolshakova, Ksenia P.; Panikorovskii, Taras L.; Bogachenkov, Alexander S.; Berestetskiy, Alexander O.; Acta Crystallographica Section E 71 (2015) o625–o626; doi:10.1107/S205698901501395X

data_2240973
_publ_section_title
;
 Crystal structure of natural phaeosphaeride A
;
_journal_coeditor_code           PK2560
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o625
_journal_page_last               o626
_journal_paper_doi               10.1107/S205698901501395X
_journal_volume                  71
_journal_year                    2015
_chemical_formula_moiety         'C15 H23 N O5'
_chemical_formula_sum            'C15 H23 N O5'
_chemical_formula_weight         297.34
_chemical_name_common
;
Phaeosphaeride A
;
_chemical_name_systematic
3,4-Dihydroxy-6-methoxy-3-methyl-7-methylidene-2-pentyl-3,4-dihydro-2<i>H</i>,7<i>H</i>-pyrano[2,3-c]pyrrol-5(6<i>H</i>)-one
_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'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.1847(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.14078(18)
_cell_length_b                   9.10361(14)
_cell_length_c                   17.5991(3)
_cell_measurement_reflns_used    14376
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.9340
_cell_measurement_theta_min      4.3980
_cell_volume                     1599.11(5)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2012)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2012)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2012)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3829
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Agilent SuperNova Dual Source diffractometer with an Atlas detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            6054
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.982
_diffrn_reflns_theta_min         4.430
_exptl_absorpt_coefficient_mu    0.765
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2012)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       tabular
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.304
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2632 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   0.05(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         6054
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0289P)^2^+2.9758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.1504
_reflns_number_gt                5940
_reflns_number_total             6054
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pk2560sup1.cif
_cod_data_source_block           I
_cod_database_code               2240973
_cod_database_fobs_code          2240973
_shelx_hkl_checksum              1148
_shelx_res_checksum              2637