Crystal structural analysis of methyl-substituted pyrazines with anilic acids: a combined diffraction, inelastic neutron scattering, 1H-NMR study and theoretical approach
Rok, M.; Bator, G.; Sawka-Dobrowolska, W.; Durlak, P.; Moskwa, M.; Medycki, W.; Sobczyk, L.; Zamponi, M.; CrystEngComm 20 (2018) 2016–; doi:10.1039/C8CE00040A

data_7230254
_publ_section_title
;
 Crystal structural analysis of methyl-substituted pyrazines with anilic
 acids: a combined diffraction, inelastic neutron scattering, 1H-NMR study
 and theoretical approach
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2016
_journal_paper_doi               10.1039/C8CE00040A
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C6 H Cl2 O4, C7 H11 N2'
_chemical_formula_sum            'C13 H12 Cl2 N2 O4'
_chemical_formula_weight         331.15
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
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_audit_update_record
;
2018-01-06 deposited with the CCDC.
2018-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                113.90(4)
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_cell_angle_gamma                98.24(2)
_cell_formula_units_Z            8
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_cell_length_b                   14.992(3)
_cell_length_c                   16.043(4)
_cell_measurement_reflns_used    7338
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.4210
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_cell_volume                     2753(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3359
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25077
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.499
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         2.938
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.489
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.799
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.720
_exptl_crystal_size_mid          0.370
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     773
_refine_ls_number_reflns         10236
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0564
_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^)+(0.0771P)^2^+0.7576P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1414
_refine_ls_wR_factor_ref         0.1562
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6857
_reflns_number_total             10236
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00040a2.cif
_cod_data_source_block           3ba
_cod_depositor_comments
'Adding full bibliography for 7230250--7230254.cif.'
_cod_original_cell_volume        2752(4)
_cod_database_code               7230254
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.720
_shelx_estimated_absorpt_t_max   0.962
_shelx_res_checksum              61561