Redetermination of 1,13-diphenyl-2,4,6,8,10,12-hexaoxatridecane at 161K
Bats, Jan W.; Miculka, Christian; Noe, Christian R.; Acta Crystallographica Section E 63 (2007) o4757–o4757; doi:10.1107/S1600536807057741

data_2216805
_publ_section_title
;
 Redetermination of 1,13-diphenyl-2,4,6,8,10,12-hexaoxatridecane at
 161K
;
_journal_coeditor_code           SU2020
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4757
_journal_page_last               o4757
_journal_paper_doi               10.1107/S1600536807057741
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C19 H24 O6'
_chemical_formula_moiety         'C19 H24 O6'
_chemical_formula_sum            'C19 H24 O6'
_chemical_formula_weight         348.38
_chemical_name_systematic
;
1,13-diphenyl-2,4,6,8,10,12-hexaoxatridecane
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.34(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   40.733(9)
_cell_length_b                   5.4310(10)
_cell_length_c                   8.266(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    161(2)
_cell_measurement_theta_max      61
_cell_measurement_theta_min      39
_cell_volume                     1813.6(8)
_computing_cell_refinement       'CAD-4 Software (Enraf--Nonius, 1989)'
_computing_data_collection       'CAD-4 Software (Enraf--Nonius, 1989)'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1996)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      161(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Enraf--Nonius CAD4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0157
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3681
_diffrn_reflns_theta_full        70.01
_diffrn_reflns_theta_max         70.01
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_time  92
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.782
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.690
_exptl_absorpt_correction_type   'numerical using eight faces'
_exptl_absorpt_process_details   '(SHELXTL; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.131
_refine_diff_density_min         -0.117
_refine_ls_abs_structure_details 'Flack (1983), with 1519 Friedel pairs'
_refine_ls_abs_structure_Flack   0.23(15)
_refine_ls_extinction_coef       0.00125(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         3429
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.04P)^2^+0.46P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0815
_reflns_number_gt                3311
_reflns_number_total             3429
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su2020.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               2216805
_cod_database_fobs_code          2216805