Soluble mu-Fi bridged niobium clusters: synthesis and crystal structures of (Et4N)6[Nb6Fi6Bri6(NCS)a6]Br2 and Cs1.6K2.4[Nb6Fi6Ii6(NCS)a6].
Naumov, Nikolai G; Cordier, Stephane; Perrin, Christiane; Chemical communications (Cambridge, England)  (2004) 1126–1127; doi:10.1039/b400668b

data_7102610
_publ_section_title
;
 Soluble mu-Fi bridged niobium clusters: synthesis and crystal
 structures of (Et4N)6[Nb6Fi6Bri6(NCS)a6]Br2 and
 Cs1.6K2.4[Nb6Fi6Ii6(NCS)a6].
;
_journal_issue                   9
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1126
_journal_page_last               1127
_journal_paper_doi               10.1039/b400668b
_journal_year                    2004
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C54 H120 Br8 F6 N12 Nb6 S6'
_chemical_formula_sum            'C54 H120 Br8 F6 N12 Nb6 S6'
_chemical_formula_weight         2440.68
_chemical_name_common            (Et4N)6(Nb6F6Br6(NCS)6).2Br
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2003-11-18T09:40:02-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                120.000
_cell_formula_units_Z            3
_cell_length_a                   18.149(5)
_cell_length_b                   18.149(5)
_cell_length_c                   25.435(5)
_cell_measurement_reflns_used    23544
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_measurement_wavelength     0.71073
_cell_volume                     7256(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.86563E-2
_diffrn_orient_matrix_UB_12      0.117389E-1
_diffrn_orient_matrix_UB_13      -0.372246E-1
_diffrn_orient_matrix_UB_21      0.590192E-1
_diffrn_orient_matrix_UB_22      0.130885E-1
_diffrn_orient_matrix_UB_23      -0.88495E-2
_diffrn_orient_matrix_UB_31      -0.221289E-1
_diffrn_orient_matrix_UB_32      -0.611455E-1
_diffrn_orient_matrix_UB_33      -0.90407E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            30088
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         3.05
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    4.168
_exptl_absorpt_correction_T_max  0.9333
_exptl_absorpt_correction_T_min  0.767
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(see. N.W. Alcock (1970). Cryst. Computing, p271)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3612
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.56
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       0.00043(7)
_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   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         4703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.048
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0597P)^2^+20.0632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1139
_refine_ls_wR_factor_ref         0.1301
_reflns_number_gt                3187
_reflns_number_total             4703
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b400668b.txt
_cod_data_source_block           compound_1
_cod_original_sg_symbol_H-M      R_-3
_cod_database_code               7102610