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_7246776
_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
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;
2023-03-29 deposited with the CCDC.	2023-05-11 downloaded from the CCDC.
;
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_cell_length_c                   14.6715(6)
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_cell_measurement_temperature    120(2)
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_cell_measurement_theta_min      6.03
_cell_volume                     862.58(6)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2021)'
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_diffrn_ambient_temperature      120(2)
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_diffrn_measurement_device_type  'Bruker PHOTON-II'
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_diffrn_radiation_monochromator  'MONTEL Multi-layer'
_diffrn_radiation_source         'Incoatec micro-focus'
_diffrn_radiation_type           CuK\a
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_diffrn_reflns_limit_k_min       -13
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_diffrn_reflns_point_group_measured_fraction_full 0.980
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_diffrn_reflns_theta_full        67.679
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_diffrn_reflns_theta_min         6.032
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_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.179
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_refine_diff_density_min         -0.263
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_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   0.01(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         1573
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0440P)^2^+0.1364P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0682
_reflns_Friedel_coverage         0.644
_reflns_Friedel_fraction_full    0.969
_reflns_Friedel_fraction_max     0.952
_reflns_number_gt                1553
_reflns_number_total             1573
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cp05363b2.cif
_cod_data_source_block           tt2202
_cod_depositor_comments
'Adding full bibliography for 7246773--7246779.cif.'
_cod_database_code               7246776
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.772
_shelx_estimated_absorpt_t_max   0.822
_shelx_res_checksum              9062