Lagoden dimethylformamide hemisolvate dihydrate: absolute configuration, dipolar interactions and~hydrogen-bonding interactions
Wicher, Barbara; Gdaniec, Maria; Dalimov, Davran N.; Zainutdinov, Umardjon N.; Acta Crystallographica Section C 65 (2009) m367–m370; doi:10.1107/S010827010903354X

data_2017369
_publ_section_title
;
 Lagoden dimethylformamide hemisolvate dihydrate: absolute
 configuration, dipolar interactions and~hydrogen-bonding interactions
;
_journal_coeditor_code           SU3037
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m367
_journal_page_last               m370
_journal_paper_doi               10.1107/S010827010903354X
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'Na + , C20 H33 O6 - , 0.5C3 H7 N O , 2H2 O'
_chemical_formula_moiety         'Na + , C20 H33 O6 - , 0.5C3 H7 N O , 2H2 O'
_chemical_formula_sum            'C21.5 H40.5 N0.5 Na O8.5'
_chemical_formula_weight         465.04
_chemical_name_common            lagoden
_chemical_name_systematic
;
sodium 3\b,16,18-trihydroxy-8,13-<i>epi</i>-9,13-epoxylabdan-15-oate
dimethylformamide hemisolvate dihydrate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 110.948(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.7614(2)
_cell_length_b                   31.0703(5)
_cell_length_c                   14.7131(3)
_cell_measurement_reflns_used    58666
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      76.30
_cell_measurement_theta_min      4.26
_cell_volume                     4594.32(16)
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlisPro (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction, 2009)'
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 1997) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla <i>et al.</i>,  2005)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Nova Cu X-ray source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            70056
_diffrn_reflns_theta_full        76.46
_diffrn_reflns_theta_max         76.46
_diffrn_reflns_theta_min         4.40
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.005
_exptl_absorpt_correction_T_max  0.818
_exptl_absorpt_correction_T_min  0.655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlisPro; Oxford Diffraction, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.286
_refine_ls_abs_structure_details 'Flack (1983), with 8192 Friedel pairs'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_coef       0.00094(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1143
_refine_ls_number_reflns         18050
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0545P)^2^+1.3939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0863
_reflns_number_gt                17865
_reflns_number_total             18050
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su3037.cif
_cod_data_source_block           I
_cod_original_cell_volume        4594.32(15)
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C21.5 H40.5 N0.5 Na1 O8.5'
_cod_database_code               2017369
_cod_database_fobs_code          2017369