(4<i>R</i>,9<i>S</i>)-4-Hydroxymethyl-3,8-dioxa-1,6-diazaspiro[4.4]nonane-2,7-dithione monohydrate
Cioci, Gianluca; Leconte, Nicolas; Tatibouët, Arnaud; Rollin, Patrick; Pérez, Serge; Imberty, Anne; Acta Crystallographica Section E 60 (2004) o2399–o2401; doi:10.1107/S1600536804029885

data_2204670
_publ_section_title
;(4<i>R</i>,9<i>S</i>)-4-Hydroxymethyl-3,8-dioxa-1,6-diazaspiro[4.4]nonane-2,7-dithione
 monohydrate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2399
_journal_page_last               o2401
_journal_paper_doi               10.1107/S1600536804029885
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C6 H8 N2 O3 S2 , H2 O'
_chemical_formula_moiety         'C6 H8 N2 O3 S2 , H2 O'
_chemical_formula_sum            'C6 H10 N2 O4 S2'
_chemical_formula_weight         238.28
_chemical_name_systematic
;
(4R,9S)-4-Hydroxymethyl-3,8-dioxa-1,6-diazaspiro[4.4]nonane-2,7-dithione
monohydrate
;
_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
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   7.036(2)
_cell_length_b                   10.336(3)
_cell_length_c                   13.814(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.5
_cell_measurement_theta_min      20.2
_cell_volume                     1004.6(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;MSC/AFC Diffractometer Control Software (Molecular Structure Corporation,
 1994)
;
_computing_data_reduction        'TEXSAN (MSC, 1992-1997)'
_computing_molecular_graphics    'PLATON (Spek, 2001)'
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.00000
_diffrn_reflns_av_sigmaI/netI    0.010
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1164
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        74.95
_diffrn_reflns_theta_max         74.95
_diffrn_reflns_theta_min         5.34
_diffrn_standards_decay_%        -3.10
_diffrn_standards_interval_count 120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.797
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       prism
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.372
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         1164
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0510
_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^)+(0.0629P)^2^+0.1989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1302
_reflns_number_gt                1150
_reflns_number_total             1164
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn6173.cif
_cod_data_source_block           I
_cod_database_code               2204670
_cod_database_fobs_code          2204670