Reversible bromide-chloride exchange in zirconium cluster compounds: synthesis by means of ionic liquids, structures, and some spectral data of (EMIm)(4)[(Zr(6)Z)Br(18)] cluster phases (Z = Be, Fe).
Willems, Johannes B.; Rohm, Henning W.; Geers, Christine; Köckerling, Martin; Inorganic chemistry 46 (2007) 6197–6203; doi:10.1021/ic061624u

data_4333174
_publ_section_title
;
 Reversible bromide-chloride exchange in zirconium cluster compounds:
 synthesis by means of ionic liquids, structures, and some spectral data
 of (EMIm)(4)[(Zr(6)Z)Br(18)] cluster phases (Z = Be, Fe).
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6197
_journal_page_last               6203
_journal_paper_doi               10.1021/ic061624u
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         '(C2H5-C3N2-CH3)4 (Zr6 Fe Br18)'
_chemical_formula_sum            'C24 H44 Br18 Fe N8 Zr6'
_chemical_formula_weight         2486.22
_chemical_name_systematic
;
Tetrakis-1-ethyl-3-methyl-imidazolium dodecakis-\m-bromo-
hexa bromo-ferro-hexa-zirconium
;
_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           'ct.exe (M. K\"ockerling, 1996)'
_cell_angle_alpha                90.00
_cell_angle_beta                 111.279(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.5746(4)
_cell_length_b                   22.6567(9)
_cell_length_c                   13.0260(5)
_cell_measurement_reflns_used    9659
_cell_measurement_temperature    566(2)
_cell_measurement_theta_max      30.73
_cell_measurement_theta_min      2.74
_cell_volume                     2908.1(2)
_computing_cell_refinement       'bruker smart'
_computing_data_collection       'bruker smart'
_computing_data_reduction        'bruker saint'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'ccd area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0597
_diffrn_reflns_av_sigmaI/netI    0.0479
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            69913
_diffrn_reflns_theta_full        30.78
_diffrn_reflns_theta_max         30.78
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    13.670
_exptl_absorpt_correction_T_max  0.1096
_exptl_absorpt_correction_T_min  0.0758
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            violet-blue
_exptl_crystal_density_diffrn    2.839
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.555
_refine_diff_density_min         -1.453
_refine_diff_density_rms         0.210
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         9067
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(fo^2^)+(0.0523p)^2^+17.1066p] where p=(fo^2^+2fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1261
_reflns_number_gt                6251
_reflns_number_total             9067
_reflns_threshold_expression     >2sigma(i)
_cod_data_source_file            ic061624usup2.cif
_cod_data_source_block           Zr6Br18Be
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_structure_factor_coef' value 'fsqd' changed to 'Fsqd'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_atom_site_adp_type' value 'uani' changed to 'Uani'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26 (29
times).

'_atom_site_adp_type' value 'uiso' changed to 'Uiso'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26 (22
times).

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

 Adding full bibliography for 4333173--4333174.cif.
;
_cod_original_cell_volume        2908.07(19)
_cod_database_code               4333174