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_4333173
_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 Be Br18)'
_chemical_formula_sum            'C24 H44 Be Br18 N8 Zr6'
_chemical_formula_weight         2439.38
_chemical_name_systematic
;
Tetrakis-1-ethyl-3-methyl-imidazolium dodecakis-\m-bromo-
hexa bromo-beryillido-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                 111.31(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.574(2)
_cell_length_b                   22.681(4)
_cell_length_c                   13.041(2)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34.97
_cell_measurement_theta_min      3.81
_cell_volume                     2913.8(10)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_publication_material  'ct.exe (M. K\"ockerling, 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w 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  0.0345
_diffrn_reflns_av_sigmaI/netI    0.1417
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6904
_diffrn_reflns_theta_full        26.98
_diffrn_reflns_theta_max         26.98
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    13.404
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.483
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'Platon, A.L. Spec, 2001'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    2.780
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             2236
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.156
_refine_diff_density_min         -0.932
_refine_diff_density_rms         0.181
_refine_ls_extinction_coef       0.00021(3)
_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   0.721
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         6273
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.721
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0288P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0855
_reflns_number_gt                3059
_reflns_number_total             6273
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061624usup1.cif
_cod_data_source_block           Zr6Br18Be
_cod_depositor_comments
'Adding full bibliography for 4333173--4333174.cif.'
_cod_original_cell_volume        2913.8(9)
_cod_database_code               4333173