4,7-Phenanthrolinium perchlorate–5-methyl-1,2,4-triazolo[1,5-<i>a</i>]pyrimidin-7(4<i>H</i>)-one–water (1/1/2)
Caballero, Ana B.; Quirós, Miguel; Salas, Juan M.; Acta Crystallographica Section E 66 (2010) o459–o460; doi:10.1107/S1600536810002564

data_2225054
_publ_section_title
;4,7-Phenanthrolinium
 perchlorate--5-methyl-1,2,4-triazolo[1,5-<i>a</i>]pyrimidin-7(4<i>H</i>)-one--water
 (1/1/2)
;
_journal_coeditor_code           LH2981
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o459
_journal_page_last               o460
_journal_paper_doi               10.1107/S1600536810002564
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C12 H9 N2 +, Cl O4 -, C6 H6 N4 O, 2H2 O'
_chemical_formula_moiety         'C12 H9 N2 +, Cl O4 -, C6 H6 N4 O, 2(H2 O)'
_chemical_formula_sum            'C18 H19 Cl N6 O7'
_chemical_formula_weight         466.84
_chemical_name_systematic
;4,7-Phenanthrolinium
perchlorate--5-methyl-1,2,4-triazolo[1,5-<i>a</i>]pyrimidin-7(4<i>H</i>)-one--
water
 (1/1/2)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.609(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6082(8)
_cell_length_b                   14.7723(14)
_cell_length_c                   16.8079(17)
_cell_measurement_reflns_used    3841
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.6
_cell_measurement_theta_min      2.4
_cell_volume                     2068.2(3)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12883
_diffrn_reflns_theta_full        26.70
_diffrn_reflns_theta_max         28.3
_diffrn_reflns_theta_min         1.9
_diffrn_standards_decay_%        -0.6
_diffrn_standards_number         257
_exptl_absorpt_coefficient_mu    0.24
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1999)'
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.366
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         4653
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.068
_refine_ls_R_factor_gt           0.054
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.7000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.142
_refine_ls_wR_factor_ref         0.152
_reflns_number_gt                3687
_reflns_number_total             4653
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh2981.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2225054
_cod_database_fobs_code          2225054