(<i>E</i>)-2,4,7-Trichloro-3-hydroxy-8-methoxy-1,9-dimethyl-6-(1-methyl-1-propenyl)-11<i>H</i>-dibenzo[<i>b</i>,<i>e</i>][1,4]dioxepin-11-one monohydrate (nidulin monohydrate)
Aree, Thammarat; Surerum, Sanya; Ngamrojanavanich, Nattaya; Kittakoop, Prasat; Acta Crystallographica Section E 65 (2009) o2470–o2471; doi:10.1107/S1600536809036277

data_2223557
_publ_section_title
;(<i>E</i>)-2,4,7-Trichloro-3-hydroxy-8-methoxy-1,9-dimethyl-6-(1-methyl-1-propenyl)-11<i>H</i>-dibenzo[<i>b</i>,<i>e</i>][1,4]dioxepin-11-one
 monohydrate (nidulin monohydrate)
;
_journal_coeditor_code           SJ2646
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2470
_journal_page_last               o2471
_journal_paper_doi               10.1107/S1600536809036277
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C20 H17 Cl3 O5, H2 O'
_chemical_formula_moiety         'C20 H17 Cl3 O5, H2 O'
_chemical_formula_sum            'C20 H19 Cl3 O6'
_chemical_formula_weight         461.70
_chemical_name_common            'nidulin monohydrate'
_chemical_name_systematic
;(<i>E</i>)-2,4,7-trichloro-3-hydroxy-8-methoxy-1,9-dimethyl-6-(1-methyl-1-propenyl)-11<i>H</i>-dibenzo[<i>b</i>,<i>e</i>]
[1,4]dioxepin-11-one
 monohydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.707(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7706(4)
_cell_length_b                   11.0374(5)
_cell_length_c                   23.9428(10)
_cell_measurement_reflns_used    4256
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      30.14
_cell_measurement_theta_min      2.64
_cell_volume                     2039.45(16)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics
;
ORTEP3 for Windows (Farrugia, 1997) and <i>Mercury</i> (Macrae <i>et
al.</i>
2006)
;
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            11735
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         1.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.485
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.341
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         5969
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max_lt       0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+0.8010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1184
_reflns_number_gt                4193
_reflns_number_total             5969
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            sj2646.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2223557
_cod_database_fobs_code          2223557