anti-Oligoannelated THF moieties: synthesis via push-pull-substituted cyclopropanes.
Schneider, Tobias F.; Kaschel, Johannes; Dittrich, Birger; Werz, Daniel B.; Organic letters 11 (2009) 2317–2320; doi:10.1021/ol900694m

data_1503929
_publ_contact_author
;
Dittrich, Birger, Institute for inorganic chemistry,
Georg-August-University Goettingen, Tammannstr. 4,
D-37077 Goettingen, Germany.
;
_publ_section_title
;
 anti-Oligoannelated THF moieties: synthesis via push-pull-substituted
 cyclopropanes.
;
_journal_issue                   11
_journal_name_full               'Organic letters'
_journal_page_first              2317
_journal_page_last               2320
_journal_paper_doi               10.1021/ol900694m
_journal_volume                  11
_journal_year                    2009
_chemical_formula_moiety         'C16 H16 O7'
_chemical_formula_sum            'C16 H16 O7'
_chemical_formula_weight         320.29
_chemical_name_common            all-anti-Heptatetrahydrofuran
_chemical_name_systematic
; 
all-anti-2,3,4-5-Hexakis(tetrahydrofuro)furan 
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      43
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 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            8
_cell_length_a                   42.329(8)
_cell_length_b                   5.8139(13)
_cell_length_c                   11.242(2)
_cell_measurement_reflns_used    5013
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      140.406
_cell_measurement_theta_min      8.356
_cell_volume                     2766.6(9)
_computing_cell_refinement       'SATIN ,Bruker AXS'
_computing_data_collection       'Bruker AXS Apex II suite'
_computing_data_reduction        'SADABS, Bruker AXS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'BRUKER AXS SMART 6000'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_UB_11      -0.1424873
_diffrn_orient_matrix_UB_12      -0.0118960
_diffrn_orient_matrix_UB_13      0.0128501
_diffrn_orient_matrix_UB_21      0.0946658
_diffrn_orient_matrix_UB_22      -0.0012365
_diffrn_orient_matrix_UB_23      0.0197217
_diffrn_orient_matrix_UB_31      -0.0179027
_diffrn_orient_matrix_UB_32      0.0881416
_diffrn_orient_matrix_UB_33      0.0020110
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         'rotating anode with mirror optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            677
_diffrn_reflns_theta_full        70.54
_diffrn_reflns_theta_max         70.54
_diffrn_reflns_theta_min         4.18
_exptl_absorpt_coefficient_mu    1.034
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.725
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS version 2008/1, Bruker AXS, 2008.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.5379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
Flack parameter Flack H D (1983), Acta Cryst. A39, 876-881,
is inconclusive, data were therefore merged. 
The chirality of the molecule was verified.
;
_refine_ls_extinction_coef       0.0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         677
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0612
_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^)+(0.0687P)^2^+20.0539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1711
_refine_ls_wR_factor_ref         0.1720
_reflns_number_gt                643
_reflns_number_total             677
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol900694m_si_002.cif
_cod_data_source_block           hepta
_cod_database_code               1503929