A quantum crystallographic approach to short hydrogen bonds.
Saunders, Lucy K.; Pallipurath, Anuradha R.; Gutmann, Matthias J.; Nowell, Harriott; Zhang, Ningjin; Allan, David R.; CrystEngComm 23 (2021) 6180–6190; doi:10.1039/d1ce00355k

data_7243377
_publ_section_title
;
 A quantum crystallographic approach to short hydrogen bonds.
;
_journal_issue                   35
_journal_name_full               CrystEngComm
_journal_page_first              6180
_journal_page_last               6190
_journal_paper_doi               10.1039/d1ce00355k
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C10 H12 N4 O7'
_chemical_formula_sum            'C10 H12 N4 O7'
_chemical_formula_weight         300.229
_chemical_name_systematic
'N,N-dimethylurea 3,5-dinitrobenzoic acid 2:2'
_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_Int_Tables_number      15
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2020-06-04
_audit_creation_method
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Olex2 1.3-alpha
(compiled 2020.05.22 svn.r1d9e7f8d for OlexSys, GUI svn.r6115)
;
_audit_update_record
;
2021-03-05 deposited with the CCDC.	2021-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.5110(4)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   28.3783(1)
_cell_length_b                   6.0988(3)
_cell_length_c                   29.7998(1)
_cell_measurement_reflns_used    69509
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      46.27331728763817
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'olex2.refine 1.3-alpha (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.9890
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
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_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       62
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_diffrn_reflns_number            24743
_diffrn_reflns_point_group_measured_fraction_full 0.9998
_diffrn_reflns_point_group_measured_fraction_max 0.9890
_diffrn_reflns_theta_full        24.4148
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_diffrn_reflns_theta_min         1.33
_diffrn_source                   Synchrotron
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  1.069
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            colourless
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'Re-crystallisation from solvent: ethanol'
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_refine_diff_density_rms         0.0530
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_refine_ls_d_res_low             14.8856
_refine_ls_goodness_of_fit_ref   0.7239
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_refine_ls_shift/su_max          1.0669
_refine_ls_shift/su_mean         0.0789
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0746P)^2^+0.1103P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0963
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              59
_reflns_limit_h_min              -59
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              62
_reflns_limit_l_min              0
_reflns_number_gt                17697
_reflns_number_total             24742
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1ce00355k2.cif
_cod_data_source_block           system3_HAR
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7243373--7243378.cif.

2024-06-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C20 H24 N8 O14'
_cod_original_formula_weight         600.459
_cod_original_formula_moiety         '2(C10 H12 N4 O7)'
_cod_original_formula_units_Z            8
_cod_database_code               7243377
_shelx_estimated_absorpt_t_min   0.995
_shelx_estimated_absorpt_t_max   0.998
_exptl_sortav_scale_factor_max   1.952
_exptl_sortav_scale_factor_min   0.191
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
  Initial refinement with olex2.refine G-N. 
;
_olex2_submission_special_instructions 'No special instructions were received'