On the anomeric preference of the isothiocyanato group
Sosa-Gil, Concepción; Babiano, Reyes; Cintas, Pedro; Light, Mark E.; Palacios, Juan C.; New Journal of Chemistry 45 (2021) 14111–14125; doi:10.1039/D1NJ00852H

data_7060856
_publ_section_title
;
 On the anomeric preference of the isothiocyanato group
;
_journal_issue                   31
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14111
_journal_page_last               14125
_journal_paper_doi               10.1039/D1NJ00852H
_journal_volume                  45
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C12 H15 N O7 S'
_chemical_formula_sum            'C12 H15 N O7 S'
_chemical_formula_weight         317.31
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-03-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-03-29 deposited with the CCDC.	2021-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                92.663(7)
_cell_angle_beta                 99.327(7)
_cell_angle_gamma                90.796(6)
_cell_formula_units_Z            2
_cell_length_a                   7.6274(4)
_cell_length_b                   9.1304(5)
_cell_length_c                   10.6185(7)
_cell_measurement_reflns_used    11964
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     728.75(7)
_computing_cell_refinement
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_collection
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 FRE-HF'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_orient_matrix_type       XPlain
_diffrn_orient_matrix_UB_11      -0.055744
_diffrn_orient_matrix_UB_12      0.016399
_diffrn_orient_matrix_UB_13      -0.090009
_diffrn_orient_matrix_UB_21      -0.063787
_diffrn_orient_matrix_UB_22      -0.097026
_diffrn_orient_matrix_UB_23      -0.004710
_diffrn_orient_matrix_UB_31      -0.102395
_diffrn_orient_matrix_UB_32      0.048421
_diffrn_orient_matrix_UB_33      0.031732
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12109
_diffrn_reflns_point_group_measured_fraction_full 0.781
_diffrn_reflns_point_group_measured_fraction_max 0.754
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.035
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FR-E+ SuperBright'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.254
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       Chunk
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 1554 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         5042
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0400P)^2^+0.1390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0905
_reflns_Friedel_coverage         0.510
_reflns_Friedel_fraction_full    0.564
_reflns_Friedel_fraction_max     0.510
_reflns_number_gt                4803
_reflns_number_total             5042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj00852h2.cif
_cod_data_source_block           2013acc0123
_cod_depositor_comments
'Adding full bibliography for 7060855--7060856.cif.'
_cod_database_code               7060856
_shelx_shelxl_version_number     2018/3
_diffrn_measurement_device_type2 'Rigaku AFC12 (Right)'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C2B(H2B), C3B(H3B), C4B(H4B), C5B(H5B)
2.b Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C1B(H1BA,H1BB)
2.c Idealised Me refined as rotating group:
 C7A(H7AA,H7AB,H7AC), C9A(H9AA,H9AB,H9AC), C11A(H11A,H11B,H11C), C7B(H7BA,H7BB,
 H7BC), C9B(H9BA,H9BB,H9BC), C11B(H11D,H11E,H11F)
;
_shelx_res_checksum              5607
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_special_instructions 'No special instructions were received'