Hydrogen-bonded network in the trichloroacetate salts of 2-amino-5-chloropyridinium and 2-methyl-5-nitroanilinium monohydrate
Janczak, Jan; Perpétuo, Genivaldo Julio; Acta Crystallographica Section C 65 (2009) o339–o341; doi:10.1107/S0108270109021490

data_2017196
_publ_section_title
;
 Hydrogen-bonded network in the trichloroacetate salts of
 2-amino-5-chloropyridinium and 2-methyl-5-nitroanilinium monohydrate
;
_journal_coeditor_code           SK3318
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o339
_journal_page_last               o341
_journal_paper_doi               10.1107/S0108270109021490
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C7 H9 N2 O2 +, C2 Cl3 O2 -, H2 O'
_chemical_formula_moiety         'C7 H9 N2 O2 +, C2 Cl3 O2 -, H2 O'
_chemical_formula_sum            'C9 H11 Cl3 N2 O5'
_chemical_formula_weight         333.55
_chemical_name_systematic
;
2-methyl-5-nitroanilinium trichloroacetate monohydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.740(10)
_cell_angle_beta                 92.290(10)
_cell_angle_gamma                94.770(10)
_cell_formula_units_Z            2
_cell_length_a                   6.9810(14)
_cell_length_b                   8.3611(17)
_cell_length_c                   12.229(2)
_cell_measurement_reflns_used    2229
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      3.31
_cell_volume                     689.6(2)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction Poland, 2008)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction Poland, 2008)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction Poland, 2008)
;
_computing_molecular_graphics
;
Diamond (Brandenburg & Putz, 2006)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean '1024x1024 with blocks 2x2'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
'KUMA KM-4 diffractometer with CCD area detector'
_diffrn_measurement_method       \w-scan
_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  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7531
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         3.31
_exptl_absorpt_coefficient_mu    0.680
_exptl_absorpt_correction_T_max  0.9081
_exptl_absorpt_correction_T_min  0.8106
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction Poland, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_meas      1.60
_exptl_crystal_density_method    flotation
_exptl_crystal_description       paralellepiped
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.456
_refine_ls_extinction_coef       0.368(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         3305
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0576
_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^)+(0.0360P)^2^+1.1800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1313
_reflns_number_gt                2306
_reflns_number_total             3305
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3318.cif
_cod_data_source_block           II
_cod_database_code               2017196
_cod_database_fobs_code          2017196