Two <i>N</i>-aminoazolylmethylene derivatives of Meldrum's acid
Blake, Alexander J.; Gould, Robert O.; Irving, Iain; McNab, Hamish; Morrow, Mark; Acta Crystallographica Section C 50 (1994) 1935–1938; doi:10.1107/S0108270194007213

data_2010288
_publ_section_title
;
 Two <i>N</i>-aminoazolylmethylene derivatives of Meldrum's acid
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1935
_journal_page_last               1938
_journal_paper_doi               10.1107/S0108270194007213
_journal_volume                  50
_journal_year                    1994
_chemical_formula_moiety         'C11 H12 N2 O4'
_chemical_formula_sum            'C11 H12 N2 O4'
_chemical_formula_weight         236.23
_chemical_name_common            '5-(1-aminopyrrolylmethylene)-Meldrum's acid'
_chemical_name_systematic
;
 5-(1-aminopyrrolylmethylene)-2,2-dimethyl-1,3-dioxane-4,6-dione
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 94.31(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.7900(11)
_cell_length_b                   12.6423(8)
_cell_length_c                   11.1014(6)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      17
_cell_volume                     2349.8(3)
_computing_cell_refinement       '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, 1994)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Stoe Stadi-4'
_diffrn_measurement_method       '\w-2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3088
_diffrn_reflns_theta_max         59.33
_diffrn_reflns_theta_min         2.64
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.871
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       Needle
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.274
_refine_ls_extinction_coef       0.0013(2)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1994)'
_refine_ls_goodness_of_fit_all   1.079
_refine_ls_goodness_of_fit_obs   1.192
_refine_ls_hydrogen_treatment
' H atoms placed in calculated positions except for  H8 and H8''
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         3087
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_restrained_S_obs      1.192
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_obs          0.0563
_refine_ls_shift/esd_max         -0.086
_refine_ls_shift/esd_mean        0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
; calc w = 1/[\s^2^(F~o~^2^) + (0.0717P)^2^ + 1.7512P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1761
_refine_ls_wR_factor_obs         0.1475
_reflns_number_observed          1915
_reflns_number_total             3088
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ha1120.cif
_cod_data_source_block           morrow
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_original_cell_volume        2349.8(2)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2010288