Polymorphism in an unexpected caesium complex of 5-hydroxyhydurilic acid
Nichol, Gary S.; Clegg, William; Acta Crystallographica Section C 61 (2005) m459–m462; doi:10.1107/S0108270105029318

data_2015194
_publ_section_title
;
 Polymorphism in an unexpected caesium complex of 5-hydroxyhydurilic
 acid
;
_journal_coeditor_code           SK1870
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m459
_journal_page_last               m462
_journal_paper_doi               10.1107/S0108270105029318
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Cs (C8 H5 N4 O7)] , 0.5H2 O'
_chemical_formula_moiety         'Cs + , C8 H5 N4 O7 - , 0.5 H2 O'
_chemical_formula_sum            'C8 H6 Cs N4 O7.5'
_chemical_formula_weight         411.08
_chemical_name_common            'Caesium 5-hydroxyhydurilate hemihydrate'
_chemical_name_systematic
;
poly[[caesium-\m~5~-5-hydroxyhydurilato] hemihydrate]
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2bc 2n'
_symmetry_space_group_name_H-M   'P n a b'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.6671(8)
_cell_length_b                   7.0632(4)
_cell_length_c                   23.5991(17)
_cell_measurement_reflns_used    19019
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.5
_cell_volume                     2278.1(2)
_computing_cell_refinement       'EvalCCD (Duisenberg et al, 2003)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        EvalCCD
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2004) and MERCURY (Version 1.4; Bruno et
al., 2002)
;
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_sigmaI/netI    0.0238
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            49241
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         5.25
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.300
_exptl_absorpt_correction_T_max  0.723
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.449
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         2592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0248
_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^)+(0.0137P)^2^+4.4877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0439
_refine_ls_wR_factor_ref         0.0470
_reflns_number_gt                2146
_reflns_number_total             2592
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1870.cif
_cod_data_source_block           I
_cod_database_code               2015194
_cod_database_fobs_code          2015194