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#$Date: 2025-08-19 20:55:00 +0200 (Tue 19 de Aug de 2025) $
#$Revision: 301808 $
#$URL: svn://www.crystallography.net/cod/cif/2/30/05/2300563.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2300563
loop_
_publ_author_name
'Krause, Lennard'
'Herbst-Irmer, Regine'
'Stalke, Dietmar'
_publ_section_title
;
 An empirical correction for the influence of low-energy contamination
;
_journal_coeditor_code           KS5494
_journal_issue                   6
_journal_name_full               'Journal of Applied Crystallography'
_journal_page_first              1907
_journal_page_last               1913
_journal_paper_doi               10.1107/S1600576715020440
_journal_volume                  48
_journal_year                    2015
_chemical_formula_moiety         'C12 H4 N4'
_chemical_formula_sum            'C12 H4 N4'
_chemical_formula_weight         204.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 98.241(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8840(12)
_cell_length_b                   6.9036(9)
_cell_length_c                   16.421(2)
_cell_measurement_reflns_used    6067
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.723
_cell_measurement_theta_min      2.5065
_cell_volume                     996.7(2)
_computing_cell_refinement       'SAINT V8.30C'
_computing_data_collection       'APEX2 v2012.2'
_computing_data_reduction        'SAINT V8.30C'
_computing_molecular_graphics    'Mercury CSD 3.3 (Build RC5)'
_computing_publication_material  'Mercury CSD 3.3 (Build RC5)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution
'SHELXT (G.M.Sheldrick,Acta Cryst.(2015)A71,3-8)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0155
_diffrn_reflns_av_unetI/netI     0.0093
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10375
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.728
_diffrn_reflns_theta_min         2.507
_diffrn_source                   'INCOATEC Microsource'
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7184
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2015/1
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       plate
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         1545
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0338
_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/[σ²(Fo²)+(0.0567P)²+0.4831P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.0992
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1432
_reflns_number_total             1545
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ks5494sup1.cif
_cod_data_source_block           2_filter
_cod_database_code               2300563
_cod_database_fobs_code          2300563
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.984
_shelx_estimated_absorpt_t_max   0.995
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
N1 N 0.30687(8) 0.24383(11) 0.23988(4) 0.02160(18) Uani 1 1 d . .
C1 C 0.65123(8) 0.47404(11) 0.48395(4) 0.01331(16) Uani 1 1 d . .
H1 H 0.7533 0.4578 0.4742 0.016 Uiso 1 1 calc R U
N2 N -0.02033(8) 0.43413(11) 0.40011(5) 0.02135(18) Uani 1 1 d . .
C2 C 0.53546(8) 0.42002(11) 0.42555(4) 0.01347(16) Uani 1 1 d . .
H2 H 0.5572 0.3661 0.3753 0.016 Uiso 1 1 calc R U
C4 C 0.26078(8) 0.38973(11) 0.37923(4) 0.01353(16) Uani 1 1 d . .
C3 C 0.37905(8) 0.44364(10) 0.43889(4) 0.01239(16) Uani 1 1 d . .
C6 C 0.10468(9) 0.41472(11) 0.39038(5) 0.01544(17) Uani 1 1 d . .
C5 C 0.28653(8) 0.30871(11) 0.30187(5) 0.01573(17) Uani 1 1 d . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C2 C1 C3 120.67(6) . 5_666
C2 C1 H1 119.7 . .
C3 C1 H1 119.7 5_666 .
C1 C2 C3 120.68(6) . .
C1 C2 H2 119.7 . .
C3 C2 H2 119.7 . .
C3 C4 C6 121.87(7) . .
C3 C4 C5 122.07(7) . .
C6 C4 C5 116.04(6) . .
C4 C3 C2 120.79(7) . .
C4 C3 C1 120.56(7) . 5_666
C2 C3 C1 118.65(6) . 5_666
N2 C6 C4 179.33(8) . .
N1 C5 C4 179.88(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 C5 1.1499(11) .
C1 C2 1.3541(10) .
C1 C3 1.4486(10) 5_666
C1 H1 0.9500 .
N2 C6 1.1522(11) .
C2 C3 1.4466(10) .
C2 H2 0.9500 .
C4 C3 1.3809(10) .
C4 C6 1.4350(10) .
C4 C5 1.4360(10) .
C3 C1 1.4486(10) 5_666
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 73697
