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_7157535
_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 syn
_chemical_formula_moiety         'C44 H46 Cl N3 O14'
_chemical_formula_sum            'C44 H46 Cl N3 O14'
_chemical_formula_weight         876.29
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_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-03-03 deposited with the CCDC.	2020-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1104(2)
_cell_length_b                   19.5548(6)
_cell_length_c                   27.2321(19)
_cell_measurement_reflns_used    17308
_cell_measurement_temperature    164(2)
_cell_measurement_theta_max      72.7
_cell_measurement_theta_min      6.7
_cell_volume                     4318.9(3)
_computing_cell_refinement       'FSProcess (Rigaku, 1998)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'FSProcess (Rigaku, 1998)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      164(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      '551 images in steps of 1\%'
_diffrn_measurement_device_details 'Curved image plate'
_diffrn_measurement_device_type
;  
Rigaku Spider 
;
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator
;
Rigaku VariMax-HF Confocal Optical System
;
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            34329
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        58.931
_diffrn_reflns_theta_max         58.931
_diffrn_reflns_theta_min         6.654
_diffrn_source
;
 Rigaku MM007 rotating anode
;
_exptl_absorpt_coefficient_mu    1.389
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR, Higashi (1995)'
_exptl_crystal_colour            colourless
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_exptl_crystal_description       needle
_exptl_crystal_F_000             1840
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene / Petroleum ether'
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 1487 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.101(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         6132
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0625
_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^)+(0.1173P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1705
_refine_ls_wR_factor_ref         0.1892
_reflns_Friedel_coverage         0.754
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                4550
_reflns_number_total             6132
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ob00671h2.cif
_cod_data_source_block           shelx_CCDC1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7157534--7157536.cif.
;
_cod_original_cell_volume        4318.9(4)
_cod_database_code               7157535
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              7460