2,9,10-Trimethoxydibenzo[<i>b</i>,<i>d</i>]oxepin-7(6<i>H</i>)-one
Hou, Yan-Jun; Song, Shu-Lin; Chu, Wen-Yi; Sun, Zhi-Zhong; Acta Crystallographica Section E 68 (2012) o204–; doi:10.1107/S1600536811053803

data_2233281
_publ_section_title
;
 2,9,10-Trimethoxydibenzo[<i>b</i>,<i>d</i>]oxepin-7(6<i>H</i>)-one
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o204
_journal_paper_doi               10.1107/S1600536811053803
_journal_volume                  68
_journal_year                    2012
_chemical_formula_moiety         'C17 H16 O5'
_chemical_formula_sum            'C17 H16 O5'
_chemical_formula_weight         300.30
_chemical_name_systematic
;
 2,9,10--trimethoxydibenzo[<i>b,d</i>]oxepin--7(6<i>H</i>)--one
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.6070(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5474(10)
_cell_length_b                   8.3776(7)
_cell_length_c                   14.8801(13)
_cell_measurement_reflns_used    3123
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.0205
_cell_measurement_theta_min      2.7431
_cell_volume                     1436.6(2)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2004)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2004)'
_computing_data_reduction        '<i>SAINT</i> (Bruker, 2004)'
_computing_molecular_graphics    '<i>SHELXTL</i>  (Sheldrick, 2008)'
_computing_publication_material  '<i>publCIF</i>  (Westrip, 2010)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_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  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11231
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_T_max  0.9758
_exptl_absorpt_correction_T_min  0.9680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '<i>SADABS</i> (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3517
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+0.2417P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1269
_reflns_number_gt                2517
_reflns_number_total             3517
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            rk2322.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2233281
_cod_database_fobs_code          2233281