(1<i>R</i>,4<i>R</i>,7<i>R</i>,8<i>R</i>,9<i>R</i>)-8-Benzyloxy-7-benzyloxymethyl-2,5,10-trioxatricyclo[5.2.1.0^4,8^]decan-9-ol
Sharma, Pawan K.; Nielsen, Poul; Bond, Andrew D.; Acta Crystallographica Section E 63 (2007) o4537–o4537; doi:10.1107/S1600536807053536

data_2216606
_publ_section_title
(1<i>R</i>,4<i>R</i>,7<i>R</i>,8<i>R</i>,9<i>R</i>)-8-Benzyloxy-7-benzyloxymethyl-2,5,10-trioxatricyclo[5.2.1.0^4,8^]decan-9-ol
_journal_coeditor_code           KP2133
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4537
_journal_page_last               o4537
_journal_paper_doi               10.1107/S1600536807053536
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C22 H24 O6'
_chemical_formula_moiety         'C22 H24 O6'
_chemical_formula_sum            'C22 H24 O6'
_chemical_formula_weight         384.41
_chemical_name_systematic
;
(1<i>R</i>,4<i>R</i>,7<i>R</i>,8<i>R</i>,9<i>R</i>)-8-(Benzyloxy)-7-
(benzyloxymethyl)-2,5,10-trioxatricyclo[5.2.1.0^4,8^]decan-9-ol
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4559(3)
_cell_length_b                   10.8048(4)
_cell_length_c                   18.0620(6)
_cell_measurement_reflns_used    4020
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      21.11
_cell_measurement_theta_min      2.43
_cell_volume                     1845.38(11)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'APEX2 (Bruker--Nonius, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2000)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2000)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker--Nonius X8 APEXII CCD'
_diffrn_measurement_method       'thin-slice \w and \f'
_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  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0369
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16553
_diffrn_reflns_theta_full        25.61
_diffrn_reflns_theta_max         25.61
_diffrn_reflns_theta_min         3.65
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.111
_refine_diff_density_min         -0.175
_refine_ls_abs_structure_details
;
In the absence of significant anomalous scattering effects,
Friedel opposites (1570 measured) have been merged.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         1975
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0389P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0607
_refine_ls_wR_factor_ref         0.0629
_reflns_number_gt                1554
_reflns_number_total             1975
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            kp2133.cif
_cod_data_source_block           I
_cod_database_code               2216606
_cod_database_fobs_code          2216606