Two new "onium" fluorosilicates, the products of interaction of fluorosilicic acid with 12-membered macrocycles: structures and spectroscopic properties.
Gelmboldt, Vladimir O.; Ganin, Eduard V.; Fonari, Marina S.; Simonov, Yurii A.; Koroeva, Larisa V.; Ennan, Alim A.; Basok, Stepan S.; Shova, Sergiu; Kählig, Hanspeter; Arion, Vladimir B.; Keppler, Bernhard K.; Dalton transactions (Cambridge, England : 2003)  (2007) 2915–2924; doi:10.1039/B703645K

data_7005616
_publ_section_title
;
 Two new "onium" fluorosilicates, the products of interaction of
 fluorosilicic acid with 12-membered macrocycles: structures and
 spectroscopic properties.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2915
_journal_page_last               2924
_journal_paper_doi               10.1039/B703645K
_journal_year                    2007
_chemical_formula_moiety
'2(C8 H18 N O3), 2(F5 H2 O1 Si1), 2(H2 O1), O1'
_chemical_formula_sum            'C16 H46 F10 N2 O11 Si2'
_chemical_formula_weight         688.73
_chemical_melting_point          383.15
_chemical_name_common
;bis(1,4,7-trioxa-10-azoniacyclododecane)
bis(aquapentafluorosilicate) trihydrate
;
_chemical_name_systematic
;
bis(1,4,7-trioxa-10-azoniacyclododecane)
bis(aquapentafluorosilicate) trihydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 93.900(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8889(7)
_cell_length_b                   9.3635(5)
_cell_length_c                   20.3291(9)
_cell_measurement_temperature    100(2)
_cell_volume                     2827.6(2)
_computing_molecular_graphics    'ORTEP for windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'X8APEX II CCD diffractometer'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0178
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            88034
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    0.247
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         6465
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0554P)^2^+3.3768P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1199
_reflns_number_gt                5432
_reflns_number_total             6465
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            B703645K.txt
_cod_data_source_block           sesh037
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '110/oC' was changed to '383.15' - it
was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               7005616