[Ni5Sb17]4-Transition-Metal Zintl Ion Complex: Crossing the Zintl Border in Molecular Intermetalloid Clusters
Melanie J. Moses; James C. Fettinger; Bryan W. Eichhorn; Inorganic Chemistry 46 (2007) 1036–1038; doi:10.1021/ic0616535

data_4307140
_publ_section_title
;
[Ni5Sb17]4-Transition-Metal Zintl Ion Complex: Crossing the Zintl Border
in Molecular Intermetalloid Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1036
_journal_page_last               1038
_journal_paper_doi               10.1021/ic0616535
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C74 H152 K4 N10 Ni5 O24 Sb17'
_chemical_formula_sum            'C74 H152 K4 N10 Ni5 O24 Sb17'
_chemical_formula_weight         4085.76
_chemical_name_systematic
; 
 ? 
;
_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                86.253(4)
_cell_angle_beta                 81.860(4)
_cell_angle_gamma                66.513(3)
_cell_formula_units_Z            2
_cell_length_a                   15.510(3)
_cell_length_b                   16.661(3)
_cell_length_c                   25.943(5)
_cell_measurement_reflns_used    7961
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      54.242
_cell_measurement_theta_min      4.681
_cell_volume                     6086(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      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0481
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            42595
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.650
_exptl_absorpt_correction_T_max  0.8358
_exptl_absorpt_correction_T_min  0.4505
_exptl_absorpt_correction_type   'Empirical, SADABS (multi-scan)'
_exptl_absorpt_process_details   'Blessing,R.H.(1995).Acta Cryst.,A51,33-38.'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    2.229
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             3882
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.147
_refine_diff_density_min         -1.147
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       0.000014(13)
_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   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1390
_refine_ls_number_reflns         21436
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0491P)^2^+22.2174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1168
_reflns_number_gt                15133
_reflns_number_total             21436
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0616535si20060831_025309.cif
_cod_data_source_block           991ffmi
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_original_cell_volume        6086.3(19)
_cod_database_code               4307140