2,2-Dimethyl-5-(2-methyl-4-phenyl-3,4-diaza-2-butenylidene)-1,3-dioxane-4,6-dione
Blake, A. J.; McNab, H.; Acta Crystallographica Section C 51 (1995) 527–529; doi:10.1107/S0108270194008371

data_2003257
_publ_section_title
2,2-Dimethyl-5-(2-methyl-4-phenyl-3,4-diaza-2-butenylidene)-1,3-dioxane-4,6-dione
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              527
_journal_page_last               529
_journal_paper_doi               10.1107/S0108270194008371
_journal_volume                  51
_journal_year                    1995
_chemical_compound_source
;
The title compound was obtained by the reaction of PhNHN=C(Me)CHO
with 2,2-dimethyl-1,3-dioxane-4,6-dione.
Crystals were grown from ethanol (McNab & Stobie, 1982).
;
_chemical_formula_structural     'C15 H16 N2 O4'
_chemical_formula_sum            'C15 H16 N2 O4'
_chemical_formula_weight         288.30
_chemical_melting_point          412.6(5)
_chemical_name_common
;
5-(1,2-Diaza-3-methyl-1-phenylbutadien-4-ylidene)-Meldrum's acid
;
_chemical_name_systematic
;
5-(1,2-Diaza-3-methyl-1-phenylbutadien-4-ylidene)-2,2-dimethyl-1,3-dioxane
-4,6-dione
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                78.01(3)
_cell_angle_beta                 83.36(3)
_cell_angle_gamma                71.41(3)
_cell_formula_units_Z            2
_cell_length_a                   7.544(3)
_cell_length_b                   8.576(3)
_cell_length_c                   12.014(7)
_cell_measurement_reflns_used    12
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      15
_cell_volume                     719.6(6)
_computing_cell_refinement       'Stoe DIF4 (Stoe & Cie, 1988a)'
_computing_data_collection       'DIF4 (Stoe & Cie, 1988a)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1988b)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1992)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Stoe Stadi-4'
_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  0.0116
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1858
_diffrn_reflns_theta_max         22.52
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        2.0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       Lath
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.216
_refine_diff_density_min         -0.200
_refine_ls_extinction_coef       0.0458(87)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.056
_refine_ls_goodness_of_fit_obs   1.124
_refine_ls_hydrogen_treatment
;
 H10 was constrained to lie 1.00\%A from N10, other H atoms
were placed in calculated positions.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         1845
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.085
_refine_ls_restrained_S_obs      1.124
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_obs          0.0397
_refine_ls_shift/esd_max         0.367
_refine_ls_shift/esd_mean        0.021
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
; calc w = 1/[\s^2^(F~o~^2^) + (0.1000P)^2^ + 0.0000P]
 where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1394
_refine_ls_wR_factor_obs         0.1285
_reflns_number_observed          1499
_reflns_number_total             1847
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ha1123.cif
_cod_data_source_block           melphme
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '139-140\%C' was changed to
'412.6(5)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was
estimated.

'_symmetry_cell_setting' value 'Triclinic' changed to
'triclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2003257