5'-(2-Hydroxy-5-hydroxymethyl-3-methoxyphenyl)-6,9-bis(hydroxymethyl)-3',4,11-trimethoxydibenzo[<i>d</i>,<i>f</i>][1,3]dioxepine-2-spiro-4'-cyclohexa-2',5'-dienone
Pajunen, A.; Karhunen, P.; Brunow, G.; Acta Crystallographica Section C 52 (1996) 1815–1817; doi:10.1107/S0108270196003654

data_2005174
_publ_contact_author
;
     Prof. Aarne Pajunen
     Department of Chemistry
     University of Helsinki
     Box 55
     FIN-00014 UNIVERSITY OF HELSINKI
     FINLAND
;
_publ_section_title
5'-(2-Hydroxy-5-hydroxymethyl-3-methoxyphenyl)-6,9-bis(hydroxymethyl)-3',4,11-trimethoxydibenzo[<i>d</i>,<i>f</i>][1,3]dioxepine-2-spiro-4'-cyclohexa-2',5'-dienone
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1815
_journal_page_last               1817
_journal_paper_doi               10.1107/S0108270196003654
_journal_volume                  52
_journal_year                    1996
_chemical_formula_moiety         'C31 H30 O11'
_chemical_formula_structural     'C31 H30 O11'
_chemical_formula_sum            'C31 H30 O11'
_chemical_formula_weight         578.55
_chemical_name_systematic
;
6,9-Di(hydroxymethyl)-3',4,11-trimethoxy-5'-[2''-hydroxy-5''-
hydroxymethyl-3''-methoxyphenyl]dibenzo[d,f][1,3]dioxepin-2-spiro-
4'-cyclohexa-2',5'-dienone
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_audit_creation_method           'SHELXL-93 (Sheldrick, 1993)'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.934(5)
_cell_length_b                   21.728(4)
_cell_length_c                   11.217(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      10.67
_cell_measurement_theta_min      7.12
_cell_volume                     5589.5(19)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1993a)
;
_computing_data_reduction
'TEXSAN PROCESS (Molecular Structure Corporation, 1993b)'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL/PC (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measurement_device       'Rigaku AFC7S diffractometer'
_diffrn_measurement_method       2\q/\w
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0820
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4911
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.58
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_meas      1.37(2)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.323
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.861
_refine_ls_goodness_of_fit_obs   1.138
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         4911
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.861
_refine_ls_restrained_S_obs      1.138
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_obs          0.0547
_refine_ls_shift/esd_max         0.005
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0553P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1379
_refine_ls_wR_factor_obs         0.1259
_reflns_number_observed          2522
_reflns_number_total             4911
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            pa1229.cif
_cod_data_source_block           dioxepin
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '
calc w = 1/[\s^2^(Fo^2^)+(0.0553P)^2^] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0553P)^2^] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               2005174