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_4109559
_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         '4(C18 H36 K N2 O6), 2(C6 Bi4 Ni4 O6), C7 H8'
_chemical_formula_sum            'C91 H152 Bi8 K4 N8 Ni8 O36'
_chemical_formula_weight         4232.13
_chemical_name_systematic
;
 (K-crypt)4(Bi4Ni4(CO)6)2*tol
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.448(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7566(18)
_cell_length_b                   48.054(7)
_cell_length_c                   22.508(3)
_cell_measurement_temperature    100(2)
_cell_volume                     12716(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL-V5.1'
_computing_molecular_graphics    'Bruker SHELXTL-V5.1'
_computing_publication_material  'Bruker SHELXTL-V5.1'
_computing_structure_refinement  'Bruker SHELXTL-V5.1'
_computing_structure_solution    'Bruker SHELXTL-V5.1'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0562
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       -57
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            74808
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.69
_exptl_absorpt_coefficient_mu    12.383
_exptl_absorpt_correction_T_max  0.2420
_exptl_absorpt_correction_T_min  0.1551
_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    2.211
_exptl_crystal_description       cube
_exptl_crystal_F_000             8024
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.997
_refine_diff_density_min         -1.925
_refine_diff_density_rms         0.247
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1391
_refine_ls_number_reflns         22189
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+117.8895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1005
_reflns_number_gt                18275
_reflns_number_total             22189
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja071044bsi20070213_043014_3.cif
_cod_data_source_block           2
_cod_original_cell_volume        12715(3)
_cod_database_code               4109559