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_7243375
_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         'C1 H1 O2, C3 H8 N2 O1'
_chemical_formula_sum            'C4 H9 N2 O3'
_chemical_formula_weight         133.128
_chemical_name_systematic        'N,N'-dimethylurea oxalic acid 2:1'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2020-06-04
_audit_creation_method
;
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                 94.614(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   3.81790(10)
_cell_length_b                   13.2171(2)
_cell_length_c                   12.4080(1)
_cell_measurement_reflns_used    23721
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      56.35681599534807
_cell_measurement_theta_min      2.1789248764459797
_cell_volume                     624.10(2)
_computing_cell_refinement
'DIALS 2theta refinement, DIALS 1.14.9-g0c59d74b8-release'
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction
;
DIALS 1.14.9-g0c59d74b8-release (Winter, G. et al., 2018)
;
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement
'olex2.refine 1.3-alpha (Bourhis et al., 2015)'
_computing_structure_solution    SHELXS-2014
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_measured_fraction_theta_full 0.9982
_diffrn_measured_fraction_theta_max 0.9773
_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'
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.9982
_diffrn_reflns_Laue_measured_fraction_max 0.9773
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9067
_diffrn_reflns_point_group_measured_fraction_full 0.9982
_diffrn_reflns_point_group_measured_fraction_max 0.9773
_diffrn_reflns_theta_full        24.4148
_diffrn_reflns_theta_max         56.50
_diffrn_reflns_theta_min         2.19
_diffrn_source                   Synchrotron
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  1.132
_exptl_absorpt_correction_T_min  0.884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             284
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: ethanol'
_exptl_crystal_size_max          0.057
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.028
_refine_diff_density_max         0.3540
_refine_diff_density_min         -0.3670
_refine_diff_density_rms         0.0566
_refine_ls_d_res_high            0.4130
_refine_ls_d_res_low             9.0307
_refine_ls_goodness_of_fit_ref   0.8748
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     163
_refine_ls_number_reflns         9065
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.8748
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0244P)^2^+0.0085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0678
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -9
_reflns_limit_k_max              31
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              -7
_reflns_number_gt                6439
_reflns_number_total             9065
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1ce00355k2.cif
_cod_data_source_block           system1_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.
;
_cod_original_cell_volume        624.098(11)
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7243375
_shelx_estimated_absorpt_t_min   0.996
_shelx_estimated_absorpt_t_max   0.998
_exptl_sortav_scale_factor_max   2.381
_exptl_sortav_scale_factor_min   0.119
_olex2_refinement_description
;
Initial refinement with olex2.refine G-N. 

;
_olex2_submission_special_instructions 'No special instructions were received'