Bis(μ-trifluoromethanesulfonato-κ^2^<i>O</i>:<i>O</i>')bis[aqua(1,4,7,10,13,16-hexaoxacyclooctadecane-κ^6^<i>O</i>)barium(II)] bis(trifluoromethanesulfonate)
C. Arnal-Hérault; A. van der Lee; M. Barboiu; Y. M. Legrand; Acta Crystallographica Section E 63 (2007) m3151–m3152; doi:10.1107/S1600536807060564

data_2216688
_publ_section_title
;Bis(\m-trifluoromethanesulfonato-\k^2^<i>O</i>:<i>O</i>')bis[aqua(1,4,7,10,13,16-hexaoxacyclooctadecane-\k^6^<i>O</i>)barium(II)]
 bis(trifluoromethanesulfonate)
;
_journal_coeditor_code           NG2370
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m3151
_journal_page_last               m3152
_journal_paper_doi               10.1107/S1600536807060564
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac
'[Ba2 (C F3 O3 S)2 (C12 H24 O6)2 (H2 O)2] (C F3 O3 S)2'
_chemical_formula_moiety         'C26 H52 Ba2 F6 O20 S2 2+, 2(C F3 O3 S -)'
_chemical_formula_sum            'C28 H52 Ba2 F12 O26 S4'
_chemical_formula_weight         1465.34
_chemical_name_systematic
;
Bis(\m-trifluoromethanesulfonato-\k^2^<i>O</i>:<i>O</i>')bis[aqua\
(1,4,7,10,13,16-hexaoxacyclooctadecane-\k^6^<i>O</i>)barium(II)]
bis(trifluoromethanesulfonate)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                68.629(12)
_cell_angle_beta                 87.576(10)
_cell_angle_gamma                83.212(10)
_cell_formula_units_Z            1
_cell_length_a                   8.9420(10)
_cell_length_b                   12.3257(16)
_cell_length_c                   12.7431(14)
_cell_measurement_reflns_used    23806
_cell_measurement_temperature    175
_cell_measurement_theta_max      33
_cell_measurement_theta_min      4
_cell_volume                     1298.8(3)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2007)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2007)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2007)
;
_computing_molecular_graphics
;
CAMERON (Watkin <i>et al.</i>,  1996),
Mercury (Macrae <i>et al.</i>,  2006) and
DrawXtl (Finger <i>et al.</i>,  2007)
;
_computing_publication_material  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_solution    'SIR2004 (Burla <i>et al.</i>,  2003)'
_diffrn_ambient_temperature      175
_diffrn_detector_area_resol_mean 16.0143
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  'Oxford Diffraction GEMINI'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.022
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23806
_diffrn_reflns_theta_full        29.492
_diffrn_reflns_theta_max         33.514
_diffrn_reflns_theta_min         3.813
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count '50 frames'
_diffrn_standards_number         '2 frames'
_exptl_absorpt_coefficient_mu    1.790
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2007);
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.45
_refine_diff_density_min         -0.48
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         6364
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0234
_refine_ls_shift/su_max          0.001353
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
 Method = Robust Weighting (Prince, 1982)
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
 A~i~ are:
 19.2 -26.3 13.3 -3.95
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0268
_refine_ls_wR_factor_gt          0.0220
_refine_ls_wR_factor_ref         0.0220
_reflns_number_gt                6364
_reflns_number_total             9409
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ng2370.cif
_cod_data_source_block           I
_cod_database_code               2216688
_cod_database_fobs_code          2216688