2,2-Dimethyl-5-(<i>N</i>-methyl-<i>N</i>-methoxyaminomethylene)-1,3-dioxane-4,6-dione
Blake, Alexander J.; McNab, Hamish; Withell, Kirsti; Acta Crystallographica Section E 59 (2003) o841–o842; doi:10.1107/S1600536803010432

data_2201974
_publ_section_title
2,2-Dimethyl-5-(<i>N</i>-methyl-<i>N</i>-methoxyaminomethylene)-1,3-dioxane-4,6-dione
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o841
_journal_page_last               o842
_journal_paper_doi               10.1107/S1600536803010432
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C9 H13 N O5'
_chemical_formula_moiety         'C9 H13 N O5'
_chemical_formula_sum            'C9 H13 N O5'
_chemical_formula_weight         215.20
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.04(7)
_cell_angle_beta                 100.50(7)
_cell_angle_gamma                112.71(5)
_cell_formula_units_Z            2
_cell_length_a                   6.477(5)
_cell_length_b                   7.769(5)
_cell_length_c                   11.675(12)
_cell_measurement_reflns_used    14
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      12.3
_cell_measurement_theta_min      5.48
_cell_volume                     518.4(8)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1992)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1992)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  'SHELXL97 and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.864
_diffrn_measured_fraction_theta_max 0.864
_diffrn_measurement_device_type  'Stoe Stadi-4 four-circle'
_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  0.022
_diffrn_reflns_av_sigmaI/netI    0.026
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2066
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.92
_diffrn_standards_decay_%        +-12
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Cube
_exptl_crystal_F_000             228
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.238
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         1580
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0399P)^2^+0.537P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1193
_reflns_number_gt                1259
_reflns_number_total             1580
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn6072.cif
_cod_data_source_block           1
_cod_original_cell_volume        518.4(7)
_cod_database_code               2201974
_cod_database_fobs_code          2201974