Comparison of disaccharide donors for heparan sulfate synthesis: uronic acids vs. their pyranose equivalents.
Sheppard, Daniel J.; Cameron, Scott A.; Tyler, Peter C.; Schwörer, Ralf; Organic & biomolecular chemistry 18 (2020) 4728–4733; doi:10.1039/d0ob00671h

data_7157534
_publ_section_title
;
 Comparison of disaccharide donors for heparan sulfate synthesis: uronic
 acids vs. their pyranose equivalents.
;
_journal_issue                   25
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              4728
_journal_page_last               4733
_journal_paper_doi               10.1039/d0ob00671h
_journal_volume                  18
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C59 H56 Cl N3 O14 S'
_chemical_formula_sum            'C59 H56 Cl N3 O14 S'
_chemical_formula_weight         1098.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2020-03-03 deposited with the CCDC.	2020-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.5220(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
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_cell_length_b                   35.3229(3)
_cell_length_c                   14.56840(10)
_cell_measurement_reflns_used    26240
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.2940
_cell_measurement_theta_min      3.9400
_cell_volume                     2682.24(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0856
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            48369
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.534
_diffrn_reflns_theta_min         3.944
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.590
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       rod
_exptl_crystal_F_000             1152
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.484
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Flack x determined using 4408 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     914
_refine_ls_number_reflns         10328
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0396
_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^+1.3455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1051
_reflns_Friedel_coverage         0.906
_reflns_Friedel_fraction_full    0.954
_reflns_Friedel_fraction_max     0.922
_reflns_number_gt                9914
_reflns_number_total             10328
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ob00671h2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7157534--7157536.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7157534
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.513
_shelx_estimated_absorpt_t_max   0.918
_shelx_res_checksum              54420