Stereospecific Furanosylations Catalyzed by Bis-thiourea Hydrogen-Bond Donors.
Mayfield, Andrew B.; Metternich, Jan B.; Trotta, Adam H.; Jacobsen, Eric N.; Journal of the American Chemical Society 142 (2020) 4061–4069; doi:10.1021/jacs.0c00335

data_4134197
_publ_section_title
;
 Stereospecific Furanosylations Catalyzed by Bis-thiourea Hydrogen-Bond
 Donors.
;
_journal_issue                   8
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4061
_journal_page_last               4069
_journal_paper_doi               10.1021/jacs.0c00335
_journal_volume                  142
_journal_year                    2020
_chemical_absolute_configuration ad
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_cell_measurement_temperature    100(2)
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_computing_cell_refinement       'SAINT 8.37A (Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT 8.37A (Bruker-AXS, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2015)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
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_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
;
Bruker D8 goniometer with CCD area detector  
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
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_diffrn_reflns_av_unetI/netI     0.0322
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_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38199
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.964
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_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.279
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_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.080
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_refine_diff_density_min         -0.197
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_refine_ls_abs_structure_details
;
 Flack x determined using 2442 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.13(11)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         5734
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_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0341
_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^)+(0.0605P)^2^+0.2072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.0913
_reflns_Friedel_coverage         0.816
_reflns_Friedel_fraction_full    0.929
_reflns_Friedel_fraction_max     0.929
_reflns_number_gt                5541
_reflns_number_total             5734
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00335_si_001.cif
_cod_data_source_block           JBM-5-118
_cod_depositor_comments
;
         Adding full bibliography for 4134197.cif.

2020-11-05
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        1682.48(4)
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C74 H90 N2 O18'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     1295.47
_cod_database_code               4134197
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.878
_shelx_estimated_absorpt_t_max   0.971
_refine_ls_abs_structure_hooft   -0.13(9)
_shelx_res_checksum              24626
_shelx_hkl_checksum              917