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_1503927
_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 H20 O7'
_chemical_formula_sum            'C16 H20 O7'
_chemical_formula_weight         324.32
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      13
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 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                 90.832(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.269(3)
_cell_length_b                   5.3090(16)
_cell_length_c                   12.835(4)
_cell_measurement_reflns_used    1909
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.63
_cell_measurement_theta_min      3.196
_cell_volume                     767.8(4)
_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_max 0.997
_diffrn_measurement_device_type  'BRUKER AXS APEX II'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_source         'INCOATEC microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1435
_diffrn_reflns_theta_full        25.53
_diffrn_reflns_theta_max         25.74
_diffrn_reflns_theta_min         3.20
_exptl_absorpt_coefficient_mu    0.110
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS version 2008/1, Bruker AXS, 2008.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         1435
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0556
_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^)+(0.0440P)^2^+0.8152P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1408
_reflns_number_gt                1049
_reflns_number_total             1435
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol900694m_si_002.cif
_cod_data_source_block           3merester
_cod_database_code               1503927