Crystal structure of 4-aminopyridinium 4-acetyl-(pyridin-4-yl)-1H-1,2,3-triazol-5-olate monohydrate, C14H16N6O3
Cisterna, Jonathan; Cárdenas, Alejandro; Brito, Iván; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 571–573; doi:10.1515/ncrs-2017-0326

data_8106220
_publ_section_title
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 Crystal structure of 4-aminopyridinium
 4-acetyl-(pyridin-4-yl)-1H-1,2,3-triazol-5-olate monohydrate, C14H16N6O3
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_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              571
_journal_page_last               573
_journal_paper_doi               10.1515/ncrs-2017-0326
_journal_volume                  233
_journal_year                    2018
_chemical_formula_moiety         'C9 H7 N4 O2, H2 O, C5 H7 N2'
_chemical_formula_sum            'C14 H16 N6 O3'
_chemical_formula_weight         316.33
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                77.064(4)
_cell_angle_beta                 72.754(3)
_cell_angle_gamma                67.148(3)
_cell_formula_units_Z            2
_cell_length_a                   7.7890(5)
_cell_length_b                   8.6069(6)
_cell_length_c                   12.4753(8)
_cell_measurement_reflns_used    9399
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      59.023
_cell_measurement_theta_min      3.738
_cell_volume                     730.40(9)
_computing_cell_refinement       'APEX3 (Bruker, 2007)'
_computing_data_collection       'APEX3 (Bruker, 2007)'
_computing_data_reduction        'APEX3 (Bruker, 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      297.16
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker AXS D8-Venture,Triumph-I\m-Cu'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0591
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10456
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        59.023
_diffrn_reflns_theta_max         59.023
_diffrn_reflns_theta_min         3.738
_exptl_absorpt_coefficient_mu    0.881
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       plate
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0045(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2104
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0594
_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^)+(0.0614P)^2^+0.7808P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1465
_refine_ls_wR_factor_ref         0.1542
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1774
_reflns_number_total             2104
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2017-0326_suppl.cif
_cod_data_source_block           jc_4pta
_cod_database_code               8106220
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C2'(H2'), C2*(H2*), C3'(H3'), C3*(H3*), C5'(H5'), C5*(H5*), C6'(H6'), C6*(H6*)
2.c X=CH2 refined with riding coordinates:
 N1*(H1*A,H1*B)
2.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
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_shelx_res_checksum              62355
_shelx_hkl_checksum              90089
_shelx_shelxl_version_number     2017/1
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n
_publcif_funding_html
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