Crystal packing in three related disaccharides: precursors to heparan sulfate oligosaccharides
Gainsford, Graeme J.; Schwörer, Ralf; Tyler, Peter C.; Zubkova, Olga V.; Acta Crystallographica Section E 71 (2015) 582–587; doi:10.1107/S2056989015008518

data_2240639
_publ_section_title
;
 Crystal packing in three related disaccharides: precursors to heparan
 sulfate oligosaccharides
;
_journal_coeditor_code           SJ5456
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              582
_journal_page_last               587
_journal_paper_doi               10.1107/S2056989015008518
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C59 H56 Cl N3 O16'
_chemical_formula_moiety         'C59 H56 Cl N3 O16'
_chemical_formula_sum            'C59 H56 Cl N3 O16'
_chemical_formula_weight         1098.51
_chemical_name_systematic
;4-Methoxyphenyl
4-<i>O</i>-[6-<i>O</i>-acetyl-2-azido-3-<i>O</i>-benzyl-2-deoxy-4-<i>O</i>-(9-fluorenylmethyloxycarbonyl)-\a-<i>D</i>-glucopyranosyl]-2-<i>O</i>-benzoyl-3-<i>O</i>-benzyl-6-<i>O</i>-chloroacetyl-\a-<i>L</i>-iodopyranoside
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
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_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90.00
_cell_angle_beta                 91.780(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.8343(11)
_cell_length_b                   8.4771(6)
_cell_length_c                   21.8112(17)
_cell_measurement_temperature    123(2)
_cell_volume                     2741.5(4)
_computing_cell_refinement
;
<i>FSProcess</i> (Rigaku, 1998)
;
_computing_data_collection
;
CrystalClear (Rigaku, 2005)
;
_computing_data_reduction
;
<i>FSProcess</i> (Rigaku, 1998)
;
_computing_molecular_graphics
;
ORTEP-3 in WinGX (Farrugia, 2012)
;
_computing_publication_material
;
SHELXL2012 (Sheldrick, 2015) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2012 (Sheldrick, 2015)
;
_computing_structure_solution
;
<i>SHELX-D</i> (Sheldrick, 2008)
;
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.421
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
;
Rigaku Spider
;
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator
;
Rigaku VariMax-HF Confocal Optical System
;
_diffrn_radiation_source
;
 Rigaku MM007 rotating anode
;
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1013
_diffrn_reflns_av_sigmaI/netI    0.1073
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19701
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         43.49
_diffrn_reflns_theta_min         6.62
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.238
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.247
_refine_ls_abs_structure_details
;
Parsons & Flack (2004), 1721 Friedel pairs
;
_refine_ls_abs_structure_Flack   0.01(8)
_refine_ls_extinction_coef       0.0110(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2012 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     666
_refine_ls_number_reflns         3962
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1479
_refine_ls_R_factor_gt           0.0880
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1736P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2135
_refine_ls_wR_factor_ref         0.2800
_reflns_number_gt                2294
_reflns_number_total             3962
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj5456sup1.cif
_cod_data_source_block           OZTF
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2240639
_cod_database_fobs_code          2240639
_shelx_hkl_checksum              590
_shelx_res_checksum              26536
_shelxl_version_number           .000002012