X-ray Crystallographic and Mass Spectrometric Probing of the Conformational and Ionophoric Properties of Stereoisomeric Hexatetrahydrofuranylhexane Segments
David G. Hilmey; Barry D. Davis; Judith C. Gallucci; Jennifer S. Brodbelt; Leo A. Paquette; Journal of Organic Chemistry 72 (2007) 9088–9101; doi:10.1021/jo7016229

data_4023066
_publ_section_title
;
 X-ray Crystallographic and Mass Spectrometric Probing of
 the Conformational and Ionophoric Properties of Stereoisomeric
 Hexatetrahydrofuranylhexane Segments
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              9088
_journal_page_last               9101
_journal_paper_doi               10.1021/jo7016229
_journal_volume                  72
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C24 H38 O6'
_chemical_formula_sum            'C24 H38 O6'
_chemical_formula_weight         422.54
_chemical_name_common            'Paquette 1438'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2006-07-18T11:51:14-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 110.603(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9610(10)
_cell_length_b                   14.4933(10)
_cell_length_c                   13.1231(10)
_cell_measurement_reflns_used    5085
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.037
_cell_measurement_wavelength     0.71073
_cell_volume                     2129.4(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.173223E-1
_diffrn_orient_matrix_UB_12      -0.676665E-1
_diffrn_orient_matrix_UB_13      -0.74133E-2
_diffrn_orient_matrix_UB_21      -0.786614E-1
_diffrn_orient_matrix_UB_22      0.127645E-1
_diffrn_orient_matrix_UB_23      -0.584585E-1
_diffrn_orient_matrix_UB_31      0.386004E-1
_diffrn_orient_matrix_UB_32      -0.43541E-2
_diffrn_orient_matrix_UB_33      -0.561691E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            45150
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.86
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.24
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4893
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.05
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0664P)^2^+0.2746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1164
_reflns_number_gt                3759
_reflns_number_total             4893
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo7016229-File007.cif
_cod_data_source_block           Paquette1438
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4023066