1,6-Dimethyltetrahydroimidazo[4,5-<i>d</i>]-imidazole-2,5(1<i>H</i>,6<i>H</i>)-dione monohydrate
Dekaprilevich, Marina O.; Suvorova, Lyudmila I.; Khmelnitskii, Lenor I.; Struchkov, Yuri T.; Acta Crystallographica Section C 50 (1994) 2056–2058; doi:10.1107/S0108270194004555

data_2010324
_publ_contact_author
;
Dr. Marina O. Dekaprilevich
Institute of Organic Chemistry
47 Leninsky prosp.,
Moscow 117913
Russia
;
_publ_section_title
;1,6-Dimethyltetrahydroimidazo[4,5-<i>d</i>]-imidazole-2,5(1<i>H</i>,6<i>H</i>)-dione
 monohydrate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2056
_journal_page_last               2058
_journal_paper_doi               10.1107/S0108270194004555
_journal_volume                  50
_journal_year                    1994
_chemical_formula_moiety         'C6 H10 N4 O2,H2 O'
_chemical_formula_sum            'C6 H12 N4 O3'
_chemical_formula_weight         188.20
_chemical_name_systematic
;
1,6-Dimethyltetrahydroimidazo[4,5-d]imidazole-2,5(1H,6H)-dione 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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.5080(10)
_cell_length_b                   10.828(2)
_cell_length_c                   14.363(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      11.5
_cell_volume                     856.6(3)
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL-Plus (Sheldrick, 1987)'
_diffrn_ambient_temperature      153(2)
_diffrn_measurement_device       'Siemens P3/PC'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1347
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -2
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            1845
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         2.36
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.120
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       needle
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.260
_refine_ls_abs_structure_details
;
refinement according to Flack (1983)
yielded unconclusive results due to the lack of strong enough anomalous
scatterers
;
_refine_ls_abs_structure_Flack   -1.(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.080
_refine_ls_goodness_of_fit_obs   1.087
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         1746
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_restrained_S_obs      1.087
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_obs          0.0563
_refine_ls_shift/esd_max         0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
; calc w=1/[\s^2^(F~o~^2^)+(0.1131P)^2^ +0.0965P] where
P=(F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1675
_refine_ls_wR_factor_obs         0.1503
_reflns_number_observed          1427
_reflns_number_total             1751
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            na1080.cif
_cod_data_source_block           gela2
_cod_database_code               2010324