Heteroatomic Deltahedral Clusters: Synthesis and Structures of closo-[Bi3Ni4(CO)6]3-, closo-[Bi4Ni4(CO)6]2-, the Open Cluster [Bi3Ni6(CO)9]3-, and the Intermetalloid closo-[Nix@{Bi6Ni6(CO)8}]4-
Jose M. Goicoechea; Michael W. Hull; Slavi C. Sevov; Journal of the American Chemical Society 129 (2007) 7885–7893; doi:10.1021/ja071044b

data_4109561
_publ_section_title
;
 Heteroatomic Deltahedral Clusters: Synthesis and Structures of
 closo-[Bi3Ni4(CO)6]3-, closo-[Bi4Ni4(CO)6]2-, the Open Cluster
 [Bi3Ni6(CO)9]3-, and the Intermetalloid closo-[Nix@{Bi6Ni6(CO)8}]4-
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7885
_journal_page_last               7893
_journal_paper_doi               10.1021/ja071044b
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety
'3(C12 H24 K O6), (C9 Bi3 Ni6 O9), (C2 N2 H8), 0.5(C7 H8)'
_chemical_formula_sum            'C50.5 H84 Bi3 K3 N2 Ni6 O27'
_chemical_formula_weight         2247.70
_chemical_name_systematic
; 
 (K-18crown6)3(Bi3Ni6(CO)9)*en*0.5tol
;
_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                86.716(2)
_cell_angle_beta                 89.544(2)
_cell_angle_gamma                82.269(2)
_cell_formula_units_Z            2
_cell_length_a                   12.4407(7)
_cell_length_b                   12.7175(7)
_cell_length_c                   22.9792(13)
_cell_measurement_temperature    100(2)
_cell_volume                     3596.7(3)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full .961
_diffrn_measured_fraction_theta_max .961
_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  0.0603
_diffrn_reflns_av_sigmaI/netI    0.0684
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            63169
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.89
_exptl_absorpt_coefficient_mu    9.093
_exptl_absorpt_correction_T_max  0.7214
_exptl_absorpt_correction_T_min  0.1923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Blessing, R.H. (1995) Acta Cryst. A51, 33-38'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.075
_exptl_crystal_description       needle
_exptl_crystal_F_000             2182
_exptl_crystal_size_max          0.83
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.866
_refine_diff_density_min         -2.812
_refine_diff_density_rms         .230
_refine_ls_extinction_coef       0.00009(2)
_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   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     830
_refine_ls_number_reflns         12170
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0151P)^2^+87.7992P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1229
_reflns_number_gt                8450
_reflns_number_total             12170
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja071044bsi20070213_043014_5.cif
_cod_data_source_block           4
_cod_original_formula_sum        'C50.50 H84 Bi3 K3 N2 Ni6 O27'
_cod_database_code               4109561