NMR-guided refinement of crystal structures using 15N chemical shift tensors
Toomey, Ryan; Wang, Luther; Heider, Emily C.; Hartman, Joshua D.; Nichols, Alexander J.; Myles, Dean A. A.; Gardberg, Anna S.; McIntyre, Garry J.; Zeller, Matthias; Mehta, Manish A.; Harper, James K.; CrystEngComm 26 (2024) 3289–3302; doi:10.1039/D4CE00237G

data_7248795
_publ_section_title
;
 NMR-guided refinement of crystal structures using 15N chemical shift
 tensors
;
_journal_issue                   25
_journal_name_full               CrystEngComm
_journal_page_first              3289
_journal_page_last               3302
_journal_paper_doi               10.1039/D4CE00237G
_journal_volume                  26
_journal_year                    2024
_chemical_absolute_configuration syn
_chemical_formula_sum            'C7 H15 N3 O5'
_chemical_formula_weight         221.22
_chemical_name_systematic        'L-Analyl-glycyl-glycine monohydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   'isomorphic replacement from X-ray data'
_atom_sites_solution_primary     'isomorphic replacement from X-ray data'
_atom_sites_solution_secondary   'isomorphic replacement from X-ray data'
_audit_creation_method           SHELXL-2019/1
_audit_update_record
;
2024-03-05 deposited with the CCDC.	2024-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.7243(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.8012(3)
_cell_length_b                   5.3813(2)
_cell_length_c                   12.1746(4)
_cell_measurement_temperature    150(2)
_cell_volume                     498.55(3)
_computing_cell_refinement       LaueGEN
_computing_data_collection       LaueGEN
_computing_data_reduction        'LaueGEN, ARGONNE_BOXES and LSCALE'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_solution    'isomorphic replacement from X-ray data'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.747
_diffrn_measured_fraction_theta_max 0.732
_diffrn_measurement_device_type
;
cylindrical image-plate detector, 
Very-Intense Vertical-Axis Laue Diffractometer (VIVALDI) at 
the Institut Laue-Langevin
;
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     1.500
_diffrn_reflns_av_R_equivalents  0.1022
_diffrn_reflns_av_unetI/netI     0.0639
_diffrn_reflns_Laue_measured_fraction_full 0.747
_diffrn_reflns_Laue_measured_fraction_max 0.732
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3459
_diffrn_reflns_point_group_measured_fraction_full 0.417
_diffrn_reflns_point_group_measured_fraction_max 0.404
_diffrn_reflns_theta_full        64.158
_diffrn_reflns_theta_max         87.426
_diffrn_reflns_theta_min         8.802
_diffrn_source                   'white neutron beam'
_exptl_absorpt_coefficient_mu    4.873
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       block
_exptl_crystal_F_000             236
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Water'
_refine_diff_density_max         1.102
_refine_diff_density_min         -1.030
_refine_diff_density_rms         0.269
_refine_ls_abs_structure_details
;
 All f" are zero, so absolute structure could not be determined
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         1001
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0549
_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^)+(0.1277P)^2^+0.0471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1355
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.000
_reflns_Friedel_fraction_max     0.000
_reflns_number_gt                987
_reflns_number_total             1001
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00237g2.cif
_cod_data_source_block           agg-150K-neutron-MZ
_cod_depositor_comments          'Adding full bibliography for 7248795.cif.'
_cod_original_cell_volume        498.54(3)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7248795
_shelx_shelxl_version_number     2019/1
_shelx_res_checksum              84515
_shelx_hkl_checksum              44704