(1β,2α,3α,7α,11α,13β)-1,3,7,11-Tetraacetoxy-2,13-bis(benzyloxy)-21-methyl-19,21-secohetisan-19-al hemihydrate
Chen, Feng-Zheng; Xiang, Qing-Xiang; Zhang, Yuan-Qin; Xiong, Jun-Ru; Acta Crystallographica Section E 65 (2009) o1432–; doi:10.1107/S1600536809018315

data_2222179
_publ_section_title
;(1\b,2\a,3\a,7\a,11\a,13\b)-1,3,7,11-Tetraacetoxy-2,13-bis(benzyloxy)-21-methyl-19,21-secohetisan-19-al
 hemihydrate
;
_journal_coeditor_code           XU2510
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1432
_journal_paper_doi               10.1107/S1600536809018315
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C43 H46 N O13, 0.5H2 O'
_chemical_formula_moiety         'C43 H46 N O13, 0.5(H2 O)'
_chemical_formula_sum            'C43 H47 N O13.5'
_chemical_formula_weight         793.82
_chemical_name_systematic
;
(1\b,2\a,3\a,7\a,11\a,13\b)-1,3,7,11-Tetraacetoxy-2,13-bis(benzyloxy)-
21-dimethyl-19,21-secohetisan-19-al hemihydrate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.517(3)
_cell_length_b                   18.045(4)
_cell_length_c                   19.241(4)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      9.56
_cell_measurement_theta_min      4.59
_cell_volume                     3998.7(16)
_computing_cell_refinement       'DIFRAC (Gabe & White, 1993)'
_computing_data_collection       'DIFRAC (Gabe & White, 1993)'
_computing_data_reduction        'NRCVAX (Gabe <i>et al.</i>,  1989)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      292(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_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  0.0074
_diffrn_reflns_av_sigmaI/netI    0.0633
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            4333
_diffrn_reflns_theta_full        25.48
_diffrn_reflns_theta_max         25.48
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        1.963
_diffrn_standards_interval_count 250
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.42
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         4092
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1332
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0817P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1501
_reflns_number_gt                2220
_reflns_number_total             4092
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            xu2510.cif
_cod_data_source_block           I
_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 
;
_cod_original_formula_sum        'C43 H47 N O13.50'
_cod_database_code               2222179
_cod_database_fobs_code          2222179