Stoichiometry-dependent structures: an X-ray and neutron single-crystal diffraction study of the effect of reaction stoichiometry on the crystalline products formed in the potassium‒cyanurate system
G. S. Nichol; W. Clegg; M. J. Gutmann; D. M. Tooke; Acta Crystallographica Section B 62 (2006) 798–807; doi:10.1107/S0108768106025171

data_2100599
_publ_section_title
;
 Stoichiometry-dependent structures: an X-ray and neutron
 single-crystal diffraction study of the effect of reaction
 stoichiometry on the crystalline products formed in the
 potassium--cyanurate system
;
_journal_coeditor_code           BS5033
_journal_date_accepted           2006-06-29
_journal_date_recd_electronic    2006-03-31
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              798
_journal_page_last               807
_journal_paper_category          FA
_journal_paper_doi               10.1107/S0108768106025171
_journal_volume                  62
_journal_year                    2006
_chemical_formula_moiety         'C12 D17 K3 N12 O16'
_chemical_formula_sum            'C12 D17 K3 N12 O16'
_chemical_formula_weight         719.71
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     'using coords of known structure'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.514(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.824(2)
_cell_length_b                   16.332(3)
_cell_length_c                   23.713(4)
_cell_measurement_reflns_used    11000
_cell_measurement_temperature    150(2)
_cell_volume                     4923.8(14)
_computing_cell_refinement       SXD2001
_computing_data_collection       SXD2001
_computing_data_reduction        SXD2001
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'using coords of known structure'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.045
_diffrn_measured_fraction_theta_max 0.045
_diffrn_measurement_device_type  'SXD at ISIS neutron source'
_diffrn_measurement_method       'time-of-flight Laue diffraction'
_diffrn_radiation_monochromator  none
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'ISIS spallation neutron source'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     0.5-7.0
_diffrn_reflns_av_R_equivalents  0.0908
_diffrn_reflns_av_sigmaI/netI    0.0585
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -62
_diffrn_reflns_number            8194
_diffrn_reflns_theta_full        83.23
_diffrn_reflns_theta_max         83.23
_diffrn_reflns_theta_min         8.65
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.0652+0.00475
_exptl_absorpt_correction_T_max  0.497
_exptl_absorpt_correction_T_min  0.123
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Mu = 0.7cm^-1^ at 1.8\A calculated using custom ISIS
software program SXD-2001.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3275
_exptl_crystal_size_max          2.00
_exptl_crystal_size_mid          2.00
_exptl_crystal_size_min          1.00
_refine_diff_density_max         2.011
_refine_diff_density_min         -2.199
_refine_ls_extinction_coef       0.000083(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   1.033
_refine_ls_hydrogen_treatment    anisotropic
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         8194
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0678
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1144P)^2^+438.2559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1820
_refine_ls_wR_factor_ref         0.1820
_reflns_number_gt                2535
_reflns_number_total             2545
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bs5033.cif
_cod_data_source_block           3_neutron
_cod_original_cell_volume        4923.8(15)
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               2100599