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_2240640
_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          'C60 H59 N3 O17'
_chemical_formula_moiety         'C60 H59 N3 O17'
_chemical_formula_sum            'C60 H59 N3 O17'
_chemical_formula_weight         1094.10
_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>-methoxyacetal-\a-<i>L</i>-iodopyranoside
;
_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'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 90.939(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.8595(17)
_cell_length_b                   8.3873(6)
_cell_length_c                   22.0138(18)
_cell_measurement_reflns_used    3418
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      71.55
_cell_measurement_theta_min      3.57
_cell_volume                     2743.2(4)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2013)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2013)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2013)
;
_computing_molecular_graphics
;
ORTEP-3 in WinGX (Farrugia, 2012) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
SHELXL2012 (Sheldrick, 2015) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2012 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.3250
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Agilent SuperNova (Dual, Cu at zero, Atlas)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1012
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17226
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.106
_diffrn_reflns_theta_min         4.962
_exptl_absorpt_coefficient_mu    0.811
_exptl_absorpt_correction_T_max  1.638
_exptl_absorpt_correction_T_min  1.080
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2013)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.359
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.323
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 810 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons & Flack, 2004)
;
_refine_ls_abs_structure_Flack   -0.3(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     730
_refine_ls_number_reflns         7922
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1218
_refine_ls_R_factor_gt           0.0834
_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^)+(0.0552P)^2^+2.9735P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1802
_refine_ls_wR_factor_ref         0.2011
_reflns_number_gt                4977
_reflns_number_total             7922
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj5456sup1.cif
_cod_data_source_block           RNSB
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2240640
_cod_database_fobs_code          2240640
_shelx_estimated_absorpt_t_min   0.760
_shelx_estimated_absorpt_t_max   0.996
_shelx_hkl_checksum              74862
_shelx_res_checksum              46088
_shelxl_version_number           .000002012