Comparison of hydrogen bonds and diverse weak interactions of the nitro group in 2-methyl-4-nitroanilinium nitrate, bisulfate and two hexafluoridosilicates: elementary graph-set approach
Daszkiewicz, Marek; Mielcarek, Agnieszka; Acta Crystallographica Section B 72 (2016) 916–926; doi:10.1107/S2052520616016139

data_2108025
_publ_section_title
;
 Comparison of hydrogen bonds and diverse weak interactions of the nitro
 group in 2-methyl-4-nitroanilinium nitrate, bisulfate and two
 hexafluoridosilicates: elementary graph-set approach
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              916
_journal_page_last               926
_journal_paper_doi               10.1107/S2052520616016139
_journal_volume                  72
_journal_year                    2016
_chemical_formula_moiety         '2(C7 H9 N2 O2), F6 Si, 2(H2 O'
_chemical_formula_sum            'C14 H22 F6 N4 O6 Si'
_chemical_formula_weight         484.44
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 104.638(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.0445(8)
_cell_length_b                   8.8682(4)
_cell_length_c                   8.1133(4)
_cell_measurement_reflns_used    1555
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      23.531
_cell_measurement_theta_min      2.689
_cell_volume                     1047.32(9)
_computing_cell_refinement       'CrysAlis 1.171.38.34a'
_computing_data_collection       'CrysAlis 1.171.38.34a'
_computing_data_reduction        'CrysAlis 1.171.38.34a'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'KUMA KM-4 with area CCD detector'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            8200
_diffrn_reflns_theta_full        23.531
_diffrn_reflns_theta_max         23.531
_diffrn_reflns_theta_min         2.689
_exptl_absorpt_coefficient_mu    0.204
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68144
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.34a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_description       plate
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.319
_exptl_crystal_size_mid          0.292
_exptl_crystal_size_min          0.012
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         1555
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+0.4536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1128
_reflns_number_gt                1117
_reflns_number_total             1555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            eb5052sup1.cif
_cod_data_source_block           1652
_cod_depositor_comments
;

2019-10-27
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum        'C7 H11 F3 N2 O3 Si0.50'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     242.22
_cod_database_code               2108025
_cod_database_fobs_code          2108025
_shelx_hkl_checksum              12993
_shelx_res_checksum              11534