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_1560297
_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            beta-N,N''-diacetylbiuret
_chemical_name_systematic
;
beta-1,5-diacteyl biuret
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccnv16q
_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                 93.496(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.4215(12)
_cell_length_b                   20.224(6)
_cell_length_c                   9.300(3)
_cell_measurement_reflns_used    827
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     830.1(4)
_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      223(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART CCD'
_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  0.0950
_diffrn_reflns_av_sigmaI/netI    0.0626
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6743
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.127
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.194
_refine_diff_density_min         -0.178
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.008(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    isotropic
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         1582
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1085
_reflns_number_gt                1074
_reflns_number_total             1582
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            620843.cif
_cod_data_source_block           dabm
_cod_original_cell_volume        830.0(4)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1560297