Crystal structures of ecdysteroids: the role of solvent molecules in hydrogen bonding and isostructurality
Fábián, László; Argay, Gyula; Kálmán, Alajos; Báthori, Mária; Acta Crystallographica Section B 58 (2002) 710–720; doi:10.1107/S0108768102005608

data_2103321
_publ_section_title
;
 Crystal structures of ecdysteroids: the role of solvent molecules in
 hydrogen bonding and isostructurality
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              710
_journal_page_last               720
_journal_paper_doi               10.1107/S0108768102005608
_journal_volume                  58
_journal_year                    2002
_chemical_formula_moiety         'C27 H44 O8, H2 O1'
_chemical_formula_sum            'C27 H46 O9'
_chemical_formula_weight         514.64
_chemical_name_common            'polypodine B hydrate'
_chemical_name_systematic
;
 2\b,3\b,5\b,14\a,20R,22R,25-heptahydroxy-5\b-cholest-7-en-6-one hydrate
;
_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                   7.1630(10)
_cell_length_b                   10.3030(10)
_cell_length_c                   37.254(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.01
_cell_measurement_theta_min      25.00
_cell_volume                     2749.4(5)
_computing_cell_refinement       'CAD4 Express'
_computing_data_collection       'CAD4 Express'
_computing_data_reduction        'XCAD4 (Harms, 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0087
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            6667
_diffrn_reflns_theta_full        74.85
_diffrn_reflns_theta_max         74.85
_diffrn_reflns_theta_min         2.37
_diffrn_standards_decay_%        6
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.756
_exptl_absorpt_correction_T_max  0.927
_exptl_absorpt_correction_T_min  0.896
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
'North A.C., Philips, D.C. & Mathews, F. (1968) Acta Cryst. A24 350-359'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.184
_refine_diff_density_min         -0.201
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         5553
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0701P)^2^+0.1608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1042
_reflns_number_gt                4972
_reflns_number_total             5553
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            de0015.cif
_cod_data_source_block           V
_cod_database_code               2103321
_cod_database_fobs_code          2103321