Crystal structure of 1,10-phenanthrolinium violurate violuric acid pentahydrate
Seidel, Rüdiger W.; Kolev, Tsonko M.; Acta Crystallographica Section E Crystallographic Communications 80 (2024) –; doi:10.1107/S205698902401065X

data_2023318
_publ_section_title
;
 Crystal structure of 1,10-phenanthrolinium violurate violuric acid
 pentahydrate
;
_journal_coeditor_code           WM5737
_journal_issue                   12
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S205698902401065X
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac
'C12 H9 N2 +, C4 H2 N3 O4 -, C4 H3 N3 O4, 5H2 O'
_chemical_formula_moiety
'C12 H9 N2 +, C4 H2 N3 O4 -, C4 H3 N3 O4, 5(H2 O)'
_chemical_formula_sum            'C20 H24 N8 O13'
_chemical_formula_weight         584.47
_chemical_name_common
;
1,10-Phenanthrolinium violurate violuric acid pentahydrate
;
_chemical_name_systematic
;
1,10-Phenanthrolinium 6-hydroxy-5-(oxidoimino)-1,3-diazinane-2,4-dione--\
6-hydroxy-5-(hydroxyimino)-1,3-diazinane-2,4-dione--water (1/1/5)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                90
_cell_angle_beta                 98.572(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.247(3)
_cell_length_b                   12.0714(16)
_cell_length_c                   25.771(4)
_cell_measurement_reflns_used    16
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      26.049
_cell_measurement_theta_min      11.971
_cell_volume                     2536.9(11)
_computing_cell_refinement
;
XSCANS (Siemens, 1994)
;
_computing_data_collection
;
XSCANS (Siemens, 1994)
;
_computing_data_reduction
;
XSCANS (Siemens, 1994)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2018)
;
_computing_publication_material
;
PLATON (Spek, 2020), enCIFer (Allen <i>et al.</i>,  2004) and
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2019/3</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0925
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            5990
_diffrn_reflns_theta_full        25.012
_diffrn_reflns_theta_max         25.012
_diffrn_reflns_theta_min         2.324
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  15
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_description       prism
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         4453
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1460
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0775P)^2^+0.7605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1873
_reflns_number_gt                2259
_reflns_number_total             4453
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5737.cif
_cod_data_source_block           I
_cod_original_cell_volume        2537.1(12)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2023318
_shelx_estimated_absorpt_t_min   0.963
_shelx_estimated_absorpt_t_max   0.972
_shelx_hkl_checksum              87735
_shelx_res_checksum              22541