Crystal structure of 3,4-diacetyl-15,21-dioxatetracyclo[23.4.0.02,7.06,11]nonacosa-1(29),2,4,6,8,10,25,27-octaene-14,22-dione — water (1:2), C31H32O6 · 2H2O
Pablo Wessig; Annika Matthes; Uwe Schilde; Zeitschrift für Kristallographie - New Crystal Structures 225 (2010) 744–; doi:

data_8102821
_publ_section_title
;
 Crystal structure of
 3,4-diacetyl-15,21-dioxatetracyclo[23.4.0.02,7.06,11]nonacosa-1(29),2,4,6,8,10,25,27-octaene-14,22-dione
 --- water (1:2), C31H32O6 &#x00B7; 2H2O
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              744
_journal_volume                  225
_journal_year                    2010
_chemical_formula_moiety         'C31 H32 O6, 2(H2O)'
_chemical_formula_sum            'C31 H36 O8'
_chemical_formula_weight         536.60
_chemical_melting_point          392.5(5)
_chemical_name_systematic
; 
 3,4-Diacetyl-15,21-dioxatetracyclo[23.4.0.02,7.06,11]nonacosa-
 1(29),2,4,6,8,10,25,27-octaene-14,22-dione solvate hydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 105.120(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9563(12)
_cell_length_b                   15.0540(18)
_cell_length_c                   15.4461(15)
_cell_measurement_reflns_used    14717
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      27.3
_cell_measurement_theta_min      1.36
_cell_volume                     2908.4(5)
_computing_cell_refinement       'X-AREA (Stoe, 2004)'
_computing_data_collection       'X-AREA (Stoe, 2004)'
_computing_data_reduction        'X-RED (Stoe, 2004)'
_computing_molecular_graphics
;
 ORTEP-3 for Windows (Farrugia, 2005) based on ORTEP-III
 (Burnett & Johnson, 2000)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      210(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_details
;
 180 frames, detector distance = 140 mm
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       '\w scan, 1.0 \%'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21850
_diffrn_reflns_theta_full        55.00
_diffrn_reflns_theta_max         55.00
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bloc
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.038
_refine_ls_extinction_coef       0.0054(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         5888
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0574
_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^)+(0.1033P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1512
_refine_ls_wR_factor_ref         0.1681
_reflns_number_gt                3506
_reflns_number_total             5888
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-3146.cff
_cod_data_source_block           wes2
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' value '392-393' was changed to '392.5(5)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               8102821