Synthesis of Bishomoinositols and an Entry for Construction of a Substituted 3-Oxabicyclo[3.3.1]nonane Skeleton
Arif Baran; Merve Bekarlar; Gökay Aydin; Mehmet Nebioglu; Ertan Şahin; Metin Balci; Journal of Organic Chemistry 77 (2012) 1244–1250; doi:10.1021/jo202494v

data_4026939
_publ_contact_author_address
;
Department of Chemistry
University of Atat\"urk
25240-Erzurum
Turkey
;
_publ_contact_author_email       ertan@atauni.edu.tr
_publ_contact_author_fax         90(442)2314380
_publ_contact_author_name        'Ertan \,Sahin'
_publ_contact_author_phone       90(442)2360948
_publ_section_title
;
 Synthesis of Bishomoinositols and an Entry for Construction of a
 Substituted 3-Oxabicyclo[3.3.1]nonane Skeleton
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1244
_journal_page_last               1250
_journal_paper_doi               10.1021/jo202494v
_journal_volume                  77
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C16 H22 O9'
_chemical_formula_sum            'C16 H22 O9'
_chemical_formula_weight         358.34
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2011-11-23T11:42:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.0000(0)
_cell_angle_beta                 99.154(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   8.8325(4)
_cell_length_b                   14.1648(4)
_cell_length_c                   14.7778(5)
_cell_measurement_reflns_used    4574
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.3607
_cell_measurement_theta_min      2.3355
_cell_measurement_wavelength     0.71073
_cell_volume                     1825.31(12)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device
;
RAXIS conversion
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1182
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38440
_diffrn_reflns_theta_full        26.4
_diffrn_reflns_theta_max         26.4
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6703
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_description       needle
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_refine_diff_density_max         0.25
_refine_diff_density_min         -0.206
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.016(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3728
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1516
_refine_ls_R_factor_gt           0.0749
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1072P)^2^+0.3807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2018
_refine_ls_wR_factor_ref         0.223
_reflns_number_gt                1690
_reflns_number_total             3728
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            jo202494v_si_003.cif
_cod_data_source_block           shelxlmbalci-merve-4oac
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               4026939