Synthesis and Structure of Cyclic Trisaccharide with Expanded Glycosidic Linkages.
Maiti, Krishnagopal; Jayaraman, Narayanaswamy; The Journal of organic chemistry 81 (2016) 4616–4622; doi:10.1021/acs.joc.6b00462

data_4036766
_publ_section_title
;
 Synthesis and Structure of Cyclic Trisaccharide with Expanded Glycosidic
 Linkages.
;
_journal_issue                   11
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              4616
_journal_page_last               4622
_journal_paper_doi               10.1021/acs.joc.6b00462
_journal_volume                  81
_journal_year                    2016
_chemical_formula_sum            'C21.67 H36 Ho0 O17.67'
_chemical_formula_weight         579.17
_space_group_crystal_system      trigonal
_space_group_IT_number           143
_space_group_name_Hall           'P 3'
_space_group_name_H-M_alt        'P 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   11.0527(15)
_cell_length_b                   11.0527(15)
_cell_length_c                   18.729(3)
_cell_measurement_reflns_used    9865
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      24.56
_cell_measurement_theta_min      3.04
_cell_volume                     1981.4(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0801
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            65772
_diffrn_reflns_theta_full        27.63
_diffrn_reflns_theta_max         27.63
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.128
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             922
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         6145
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1307
_refine_ls_R_factor_gt           0.1054
_refine_ls_shift/su_max          0.128
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1689P)^2^+3.1983P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2822
_refine_ls_wR_factor_ref         0.3010
_reflns_number_gt                4648
_reflns_number_total             6145
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo6b00462_si_002.cif
_cod_data_source_block           kghcd_0m
_cod_database_code               4036766