One-bond <sup>13</sup>C-<sup>13</sup>C spin-coupling constants in saccharides: a comparison of experimental and calculated values by density functional theory using solid-state <sup>13</sup>C NMR and X-ray crystallography.
Tetrault, Timothy; Meredith, Reagan J.; Yoon, Mi-Kyung; Canizares, Christopher; Oliver, Allen G.; Carmichael, Ian; Serianni, Anthony S.; Physical chemistry chemical physics : PCCP 25 (2023) 16048–16059; doi:10.1039/d2cp05363b

data_7246778
_publ_section_title
;
 One-bond <sup>13</sup>C-<sup>13</sup>C spin-coupling constants in
 saccharides: a comparison of experimental and calculated values by
 density functional theory using solid-state <sup>13</sup>C NMR and X-ray
 crystallography.
;
_journal_issue                   23
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              16048
_journal_page_last               16059
_journal_paper_doi               10.1039/d2cp05363b
_journal_volume                  25
_journal_year                    2023
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C7 H14 O6, 0.5(H2 O)'
_chemical_formula_sum            'C7 H15 O6.5'
_chemical_formula_weight         203.19
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-03-29 deposited with the CCDC.	2023-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.3472(2)
_cell_length_b                   7.3472(2)
_cell_length_c                   34.1458(12)
_cell_measurement_reflns_used    9615
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      69.81
_cell_measurement_theta_min      6.16
_cell_volume                     1843.24(10)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2021)'
_computing_data_collection       'Bruker APEX-4 (Bruker, 2021)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2021)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2020)'
_computing_publication_material  'CIFTAB (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker PHOTON-II'
_diffrn_measurement_method       'combination of \w and \f-scans '
_diffrn_radiation_monochromator  'MONTEL Multi-layer'
_diffrn_radiation_source         'Incoatec micro-focus'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            43262
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.733
_diffrn_reflns_theta_min         6.161
_exptl_absorpt_coefficient_mu    1.135
_exptl_absorpt_correction_T_max  0.9904
_exptl_absorpt_correction_T_min  0.8394
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Krause et al., 2015)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_description       tablet
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.084
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
;
 Flack x determined using 611 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         1727
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0217
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+0.3452P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0586
_reflns_Friedel_coverage         0.556
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                1703
_reflns_number_total             1727
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cp05363b2.cif
_cod_data_source_block           tt2203
_cod_depositor_comments
'Adding full bibliography for 7246773--7246779.cif.'
_cod_original_cell_volume        1843.24(12)
_cod_original_formula_sum        'C7 H15 O6.50'
_cod_database_code               7246778
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.805
_shelx_estimated_absorpt_t_max   0.911
_shelx_res_checksum              95383