Gas storage in soft 1D nano-tunnels by the induced fit of a serration structure
Katagiri, Toshimasa; Takahashi, Satoshi; Tanaka, Yasuhiro; Kawabata, Kouji; Hattori, Yoshiyuki; Kaneko, Katsumi; Uneyama, Kenji; CrystEngComm 11 (2009) 347–; doi:10.1039/b814508c

data_7200402
_publ_section_title
;
 Gas storage in soft 1D nano-tunnels by the induced fit of a serration
 structure
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              347
_journal_paper_doi               10.1039/b814508c
_journal_volume                  11
_journal_year                    2009
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C16 H24 F6 O6, (C6H14)0.30, (C4H10O)0.08'
_chemical_formula_sum            'C18.12 H29 F6 O6.08'
_chemical_formula_weight         458.13
_chemical_melting_point          339
_chemical_name_common
;(S,S)-(-)-decamethylene bis(3,3,3-trifluorolactate) hexane
ether mixed solvate
;
_chemical_optical_rotation       '[\a]^25^~D~= -3.78 (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                   28.6832(8)
_cell_length_b                   5.0572(1)
_cell_length_c                   7.9245(3)
_cell_measurement_reflns_used    13317
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.1
_cell_volume                     1149.50(6)
_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    'SAPI91 (Rigaku, 1991)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.936
_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  0.0086
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2511
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(HIGASHI, T. (1995). Abscor - Empirical Absorption Correction
based on Fourier Series Approximation. Rigaku Corporation, Tokyo, Japan.)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             481
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_platon_squeeze_details
;
Although there were four peaks within the void from Fourier difference map,
the highly disordered solvents within the void were not crystallographically
well defined.

The SQUEEZE routine of the program PLATON was used
in order to eliminate the contribution of disordered solvents molecules,
thereby a final model based only on the ordered part of the crystal structure
was obtained.

The SQUEEZE routine suggested that
a total potential solvent area volume of 206.9 Ang^3^[18.0% of cell volume],
and a void electron population of 73 per cell.

Refinement after the SQUEEZE routine gave significantly improved R values.
[R values before SQUEEZE]
R1 = 0.121 for >2sigma(I) data
R1 = 0.142 , wR2 = 0.360, GooF = S = 1.83 for all data
( 1496 data and 0 restraint / 128 parameters)

;
_refine_diff_density_max         0.191
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.054
_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_coef       0.046(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1274
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0616P)^2^+0.1844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.0949
_reflns_number_gt                1200
_reflns_number_total             1274
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b814508c.txt
_cod_data_source_block           3g_hexane_ether_mixed_solvate
_cod_original_sg_symbol_H-M      'P 21 21 2 '
_cod_database_code               7200402