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_7246774
_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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_chemical_formula_moiety         'C7 H14 O6, H2 O'
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_space_group_name_Hall           'P 2ac 2ab'
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;
2023-03-29 deposited with the CCDC.	2023-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_angle_gamma                90
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_cell_length_c                   21.1354(6)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      69.71
_cell_measurement_theta_min      6.32
_cell_volume                     956.87(5)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2010)'
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_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      120(2)
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_diffrn_measured_fraction_theta_full 0.994
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_diffrn_radiation_type           CuK\a
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_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0121
_diffrn_reflns_Laue_measured_fraction_full 0.994
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_diffrn_reflns_limit_l_max       25
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_diffrn_reflns_point_group_measured_fraction_full 0.997
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_diffrn_source                   'Incoatec micro-focus'
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_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.102
_refine_diff_density_max         0.210
_refine_diff_density_min         -0.167
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Flack x determined using 709 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         1790
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0208
_refine_ls_R_factor_gt           0.0206
_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^)+(0.0308P)^2^+0.1737P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0548
_reflns_Friedel_coverage         0.664
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                1777
_reflns_number_total             1790
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cp05363b2.cif
_cod_data_source_block           tt2102
_cod_depositor_comments
'Adding full bibliography for 7246773--7246779.cif.'
_cod_database_code               7246774
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.787
_shelx_estimated_absorpt_t_max   0.891
_diffrn_source_monochromator     'MONTEL Multi-layer'
_shelx_res_checksum              10786