Nanoporous organic layered crystals of double-headed bis(trifluorolactate)s. Hydrogen-bonded systematic crystal structures controlled by the symmetries of molecular components
Takahashi, Satoshi; Katagiri, Toshimasa; Uneyama, Kenji; CrystEngComm 8 (2006) 132–; doi:10.1039/b512051a

data_7203129
_publ_section_title
;
 Nanoporous organic layered crystals of double-headed
 bis(trifluorolactate)s. Hydrogen-bonded systematic crystal structures
 controlled by the symmetries of molecular components
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              132
_journal_paper_doi               10.1039/b512051a
_journal_volume                  8
_journal_year                    2006
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C12 H16 F6 O6 '
_chemical_formula_sum            'C12 H16 F6 O6'
_chemical_formula_weight         370.25
_chemical_melting_point          387
_chemical_name_common
'(S,S)-(-)-hexamethylene bis(3,3,3-trifluorolactate)'
_chemical_optical_rotation       '[\a]^25^~D~= -5.80 (c = 1.1, acetone)'
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      18
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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            2
_cell_length_a                   19.7519(12)
_cell_length_b                   5.0738(2)
_cell_length_c                   7.8915(5)
_cell_measurement_reflns_used    5322
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      4.0
_cell_volume                     790.86(8)
_computing_cell_refinement       'PAPID-AUTO (Rigaku)'
_computing_data_collection       'RAPID-AUTO (Rigaku)'
_computing_data_reduction        'teXsan Ver. 1.11 (MSC)'
_computing_molecular_graphics    'Mercury Ver. 1.3 (Bruno et al., 2002)'
_computing_publication_material  'WinGX Ver. 1.7 (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Rigaku RAXIS-IV Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5550
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.30
_exptl_absorpt_coefficient_mu    0.165
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             380
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.225
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
; The absolute configuration was assigned to agree with
that of its precursor (S)-trifluorolactic acid at the chiral centre C2.
This compound has no atom heavier than Si and analyzed by
Mo radiation so that Flack parameter is not listed.
Friedel pairs were merged before refinement.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1040
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0532P)^2^+0.2184P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.0931
_reflns_number_gt                1015
_reflns_number_total             1040
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b512051a.txt
_cod_data_source_block           3c
_cod_original_sg_symbol_H-M      'P 21 21 2 '
_cod_original_formula_sum        'C12 H16 F6 O6 '
_cod_database_code               7203129