Polymorphism ofN,N′′-Diacetylbiuret Studied by Solid-State13C and15N NMR Spectroscopy, DFT Calculations, and X-ray Diffraction
Macholl, Sven; Lentz, Dieter; Börner, Frank; Buntkowsky, Gerd; Chemistry - A European Journal 13 (2007) 6139–6149; doi:10.1002/chem.200601843

data_1560296
_publ_section_title
;
 Polymorphism ofN,N&#x2032;&#x2032;-Diacetylbiuret Studied by
 Solid-State13C and15N NMR Spectroscopy, DFT Calculations, and X-ray
 Diffraction
;
_journal_issue                   21
_journal_name_full               'Chemistry - A European Journal'
_journal_page_first              6139
_journal_page_last               6149
_journal_paper_doi               10.1002/chem.200601843
_journal_volume                  13
_journal_year                    2007
_chemical_formula_sum            'C6 H9 N3 O4'
_chemical_formula_weight         187.16
_chemical_name_common            alpha-N,N''-diacetylbiuret
_chemical_name_systematic
;
alpha-1,5-diacetyl biuret
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccnv17r
_audit_creation_method           SHELXL-97
_audit_update_record
;
2006-09-13 deposited with the CCDC.	2021-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 112.401(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.191(2)
_cell_length_b                   5.3440(9)
_cell_length_c                   13.545(2)
_cell_measurement_reflns_used    817
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      4.2
_cell_volume                     815.8(2)
_computing_cell_refinement       'BRUKER-AXS SAINT'
_computing_data_collection       'BRUKER-AXS SMART'
_computing_data_reduction        'BRUKER-AXS SAINT'
_computing_molecular_graphics    'ORTEP for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'CCD BRUKER-AXS SMART'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4948
_diffrn_reflns_theta_full        28.20
_diffrn_reflns_theta_max         28.20
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelett
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    isotropic
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         1969
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1295P)^2^+0.0584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1626
_refine_ls_wR_factor_ref         0.1779
_reflns_number_gt                1566
_reflns_number_total             1969
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            620844.cif
_cod_data_source_block           dabn
_cod_original_cell_volume        815.9(2)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               1560296