1<small>D</small>-1-<i>O</i>-<i>tert</i>-Butyldiphenylsilyl-2,3,6-<i>O</i>-tris(methoxymethylene)-<i>myo</i>-inositol 4,5-bis(dibenzylphosphate)
Anderson, Regan J.; Gainsford, Graeme J.; Acta Crystallographica Section E 68 (2012) o900–; doi:10.1107/S1600536812008069

data_2233811
_publ_section_title
;
 1<small>D</small>-1-<i>O</i>-<i>tert</i>-Butyldiphenylsilyl-2,3,6-<i>O</i>-tris(methoxymethylene)-<i>myo</i>-inositol
 4,5-bis(dibenzylphosphate)
;
_journal_coeditor_code           GK2443
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o900
_journal_paper_doi               10.1107/S1600536812008069
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C56 H68 O15 P2 Si'
_chemical_formula_moiety         'C56 H68 O15 P2 Si'
_chemical_formula_sum            'C56 H68 O15 P2 Si'
_chemical_formula_weight         1071.13
_chemical_name_common
;
1D-1-<i>O</i>-<i>tert</i>-Butyldiphenylsilyl-2,3,6-<i>O</i>-
tris(methoxymethylene)-<i>myo</i>-inositol 4,5-bis(dibenzylphosphate)
;
_chemical_name_systematic
;tetrabenzyl
(1<i>R</i>,2<i>R</i>,3<i>S</i>,4<i>R</i>,5<i>R</i>,6<i>S</i>)-4-(<i>tert</i>-
butyldiphenylsilyloxy)-3,5,6-tris(methoxymethoxy)cyclohexane-1,2-diyl
bisphosphate
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4052(7)
_cell_length_b                   53.019(3)
_cell_length_c                   10.0786(6)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    118(2)
_cell_measurement_theta_max      24.9
_cell_measurement_theta_min      2.26
_cell_volume                     5560.1(6)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction
;
SAINT (Bruker, 2005) and SADABS (Bruker, 2005)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 1997) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      118(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.821
_diffrn_measured_fraction_theta_max 0.821
_diffrn_measurement_device_type  'Bruker APEXII 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  0.081
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       62
_diffrn_reflns_limit_k_min       -63
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            68347
_diffrn_reflns_theta_full        25.29
_diffrn_reflns_theta_max         25.29
_diffrn_reflns_theta_min         2.54
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[SADABS (Bruker, 2005); Blessing (1995)]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       triangular
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.427
_refine_ls_abs_structure_details 'Flack (1983), 2324 Friedel pairs'
_refine_ls_abs_structure_Flack   0.12(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         8042
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0707
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1107P)^2^+10.0351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1754
_refine_ls_wR_factor_ref         0.1809
_reflns_number_gt                7297
_reflns_number_total             8042
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            gk2443.cif
_cod_data_source_block           I
_cod_database_code               2233811
_cod_database_fobs_code          2233811