(±)-1-{8'-(<i>tert</i>-Butyldiphenylsilyloxymethyl)-1',7'-dioxaspiro[5.5]undecan-2'-yl}uridine
Choi, Ka Wai; Brimble, Margaret A.; Groutso, Tania; Acta Crystallographica Section E 64 (2008) o715–; doi:10.1107/S1600536808006727

data_2218005
_publ_section_title
(+-)-1-{8'-(<i>tert</i>-Butyldiphenylsilyloxymethyl)-1',7'-dioxaspiro[5.5]undecan-2'-yl}uridine
_journal_coeditor_code           SI2075
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o715
_journal_paper_doi               10.1107/S1600536808006727
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C30 H38 N2 O5 Si'
_chemical_formula_moiety         'C30 H38 N2 O5 Si'
_chemical_formula_sum            'C30 H38 N2 O5 Si'
_chemical_formula_weight         534.71
_chemical_melting_point          482.4(9)
_chemical_name_systematic
;
(+-)-1-{8'-(<i>tert</i>-Butyldiphenylsilyloxymethyl)-1',7'-
dioxaspiro[5.5]undecan-2'-yl}uridine
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.4200(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.7960(2)
_cell_length_b                   12.5092(2)
_cell_length_c                   15.09350(10)
_cell_measurement_reflns_used    5612
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      1.79
_cell_volume                     2755.93(6)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996) and
Mercury (Macrae <i>et al.</i>,  2006)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and publCIF (Westrip, 2008)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       'area-detector \w'
_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  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15898
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  0.9848
_exptl_absorpt_correction_T_min  0.9603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.338
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5612
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0251P)^2^+2.8069P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1106
_reflns_number_gt                4327
_reflns_number_total             5612
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            si2075.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2218005
_cod_database_fobs_code          2218005