Stabilising small clusters: synthesis and characterisation of thermolabile [Gd4F7(15-crown-5)4][AsF6]5.6 SO2.
Deacon, Glen B.; Evans, David J.; Junk, Peter C.; Lork, Enno; Mews, Rüdiger; Zemva, Boris; Dalton transactions (Cambridge, England : 2003)  (2005) 2237–2238; doi:10.1039/b504819b

data_7008589
_publ_section_title
;
 Stabilising small clusters: synthesis and characterisation of
 thermolabile [Gd4F7(15-crown-5)4][AsF6]5.6 SO2.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2237
_journal_page_last               2238
_journal_paper_doi               10.1039/b504819b
_journal_year                    2005
_chemical_formula_moiety         '[Gd4C40H80F7][AsF6]5(SO2)6'
_chemical_formula_sum            'C40 H80 As5 F37 Gd4 O32 S6'
_chemical_formula_weight         2972.00
_chemical_name_systematic
;
tetra(15-crown-5)heptakis(mu-fluoro)tetrakisgadolinium(III)
pentakis(hexafluoroarsenate) sulphur dioxide solvate
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.32(3)
_cell_angle_beta                 84.45(3)
_cell_angle_gamma                73.91(3)
_cell_formula_units_Z            2
_cell_length_a                   13.712(3)
_cell_length_b                   13.783(3)
_cell_length_c                   24.527(5)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.49
_cell_measurement_theta_min      2.66
_cell_volume                     4429.6(18)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_sigmaI/netI    0.1030
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            17526
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        'random variation +/-2.0'
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.100
_exptl_absorpt_correction_T_max  0.6858
_exptl_absorpt_correction_T_min  0.2611
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'Stuart & Walker, Acta Cryst A, 1983'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.228
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2852
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.729
_refine_diff_density_min         -1.899
_refine_diff_density_rms         0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1137
_refine_ls_number_reflns         15207
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1261
_refine_ls_R_factor_gt           0.0768
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0843P)^2^+91.5980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1760
_refine_ls_wR_factor_ref         0.2033
_reflns_number_gt                10025
_reflns_number_total             15207
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b504819b.txt
_cod_data_source_block           david2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'refdelF' changed to
'refdelf' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               7008589