Redetermination of 3,3,6,6-tetramethyl-4a-hydroxy-9-(<i>ortho</i>-methoxyphenyl)-2,3,4,4a,5,6,7,8,9,9a-decahydro-1<i>H</i>-xanthene-1,8-dione at 173K
Bolte, Michael; Degen, Alexander; Rühl, Stephan; Acta Crystallographica Section E 57 (2001) o172–o173; doi:10.1107/S160053680100160X

data_2200178
_publ_section_title
;Redetermination of
 3,3,6,6-tetramethyl-4a-hydroxy-9-(<i>ortho</i>-methoxyphenyl)-2,3,4,4a,5,6,7,8,9,9a-decahydro-1<i>H</i>-xanthene-1,8-dione
 at 173K
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o172
_journal_page_last               o173
_journal_paper_doi               10.1107/S160053680100160X
_journal_volume                  57
_journal_year                    2001
_chemical_formula_moiety         'C24 H30 O5'
_chemical_formula_sum            'C24 H30 O5'
_chemical_formula_weight         398.48
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 128.820(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   33.845(4)
_cell_length_b                   7.2140(10)
_cell_length_c                   22.605(3)
_cell_measurement_reflns_used    7436
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      0
_cell_volume                     4300.1(11)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 1991)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens CCD three-circle'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0240
_diffrn_reflns_av_sigmaI/netI    .0134
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            39326
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.54
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  1500
_diffrn_standards_number         623
_exptl_absorpt_coefficient_mu    .085
_exptl_absorpt_correction_T_max  .959
_exptl_absorpt_correction_T_min  .951
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          .60
_exptl_crystal_size_mid          .50
_exptl_crystal_size_min          .50
_refine_diff_density_max         .336
_refine_diff_density_min         -.232
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         4750
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          .0470
_refine_ls_R_factor_gt           .0407
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0558P)^2^+3.6403P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1110
_reflns_number_gt                4193
_reflns_number_total             4750
_reflns_threshold_expression     I>2\ss(I)
_cod_data_source_file            na6041.cif
_cod_data_source_block           rd8
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_cell_volume        4300.1(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2200178