2-[(2<i>R</i>,3<i>S</i>,4<i>S</i>,5<i>S</i>)-3,4-Benzyloxy-2,5-bis(trityloxymethyl)tetrahydrofuran-2-yloxy]-3,4,5-tribenzyloxy-6-(trityloxymethyl)tetrahydropyran‒methanol‒2-butanone (1/1/0.75)
Zi-Sheng Wu; Chong-Bo Liu; Zhi-Jie Fang; Yuan-Xing Wang; Hui-Liang Wen; Acta Crystallographica Section E 63 (2007) o1471–o1472; doi:10.1107/S1600536807007362

data_2212637
_publ_section_title
;2-[(2<i>R</i>,3<i>S</i>,4<i>S</i>,5<i>S</i>)-3,4-Benzyloxy-2,5-bis(trityloxymethyl)tetrahydrofuran-2-yloxy]-3,4,5-tribenzyloxy-6-(trityloxymethyl)tetrahydropyran--methanol--2-butanone
 (1/1/0.75)
;
_journal_coeditor_code           LH2308
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1471
_journal_page_last               o1472
_journal_paper_doi               10.1107/S1600536807007362
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C104 H94 O11, C H4 O, 0.75C4 H8 O'
_chemical_formula_moiety         'C104 H94 O11, C H4 O, 0.75(C4 H8 O)'
_chemical_formula_sum            'C108 H104 O12.75'
_chemical_formula_weight         1605.91
_chemical_name_systematic
;
2-[(2R,3S,4S,5S)-3,4-Benzyloxy-2,5-bis-trityloxymethyl-tetrahydrofuran-2-
yloxy]-3,4,5-tribenzyloxy-6-(trityloxymethyl)tetrahydropyran--methanol--
2-butanone (1/1/0.75)
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.322(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.9897(10)
_cell_length_b                   24.0016(15)
_cell_length_c                   15.9688(11)
_cell_measurement_reflns_used    10202
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      1.6
_cell_volume                     4605.6(6)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC, 2005)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'DIAMOND (Brandenburg & Berndt, 2005)'
_computing_publication_material  'CrystalStructure (Rigaku/MSC, 2005)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            38013
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  0.9852
_exptl_absorpt_correction_T_min  0.9623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1708
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.286
_refine_ls_abs_structure_details 'None, Friedel Pairs merged'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1217
_refine_ls_number_reflns         9165
_refine_ls_number_restraints     337
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1092P)^2^+0.4583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1624
_refine_ls_wR_factor_ref         0.1690
_reflns_number_gt                8198
_reflns_number_total             9165
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh2308.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2212637
_cod_database_fobs_code          2212637