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_2100600
_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 H16 N12 O16 Rb3'
_chemical_formula_sum            'C12 H16 N12 O16 Rb3'
_chemical_formula_weight         840.78
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.584(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1499(15)
_cell_length_b                   16.6185(19)
_cell_length_c                   11.8444(13)
_cell_measurement_reflns_used    4184
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.08
_cell_measurement_theta_min      2.45
_cell_volume                     2552.2(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9291
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.81
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.831
_exptl_absorpt_correction_T_max  0.759
_exptl_absorpt_correction_T_min  0.388
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.188
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.970
_refine_diff_density_min         -0.980
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         2324
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0253P)^2^+9.2128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0774
_reflns_number_gt                1898
_reflns_number_total             2324
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bs5033.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               2100600