Total synthesis of tetraacylated phosphatidylinositol hexamannoside and evaluation of its immunomodulatory activity
Pratap S. Patil; Ting-Jen Rachel Cheng; Medel Manuel L. Zulueta; Shih-Ting Yang; Larry S. Lico; Shang-Cheng Hung; Nature Communications 6 (2015) 7239–; doi:10.1038/ncomms8239

data_1548295
_publ_section_title
;
 Total synthesis of tetraacylated phosphatidylinositol hexamannoside and
 evaluation of its immunomodulatory activity
;
_journal_name_full               'Nature Communications'
_journal_page_first              7239
_journal_paper_doi               10.1038/ncomms8239
_journal_volume                  6
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C48 H50 O6 S'
_chemical_formula_sum            'C48 H50 O6 S'
_chemical_formula_weight         754.94
_space_group_IT_number           4
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 95.180(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.6730(11)
_cell_length_b                   7.8490(8)
_cell_length_c                   18.4910(18)
_cell_measurement_reflns_used    1111
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.0136
_cell_measurement_theta_min      2.9911
_cell_volume                     1976.3(3)
_computing_cell_refinement
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        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
        (compiled Aug 27 2010,11:50:40)
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_computing_data_collection
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        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
        (compiled Aug 27 2010,11:50:40)
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_computing_data_reduction
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        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
        (compiled Aug 27 2010,11:50:40)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.4875
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0303748
_diffrn_orient_matrix_UB_12      0.0598208
_diffrn_orient_matrix_UB_13      -0.0161607
_diffrn_orient_matrix_UB_21      -0.0108865
_diffrn_orient_matrix_UB_22      -0.040117
_diffrn_orient_matrix_UB_23      -0.0342859
_diffrn_orient_matrix_UB_31      -0.0410003
_diffrn_orient_matrix_UB_32      0.0550411
_diffrn_orient_matrix_UB_33      -0.0072735
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_av_unetI/netI     0.1166
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20728
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         30.12
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.98798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
        (compiled Aug 27 2010,11:50:40)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.934
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(9)
_refine_ls_extinction_coef       0.0066(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         9660
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0626
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+0.2016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1377
_reflns_number_gt                6466
_reflns_number_total             9660
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ncomms8239-s3.cif
_cod_data_source_block           i13957
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_sg_symbol_Hall     'p 2yb'
_cod_database_code               1548295