Assembly of Mixed-Metal Cages Using Polyimido Antimony(III) Anions. Syntheses and Structures of [Sb3(NCy)4(HNCy)2]K.2(toluene), [Sb2(NCy)4]2M4 (M = Cu, Ag), and [Sb(NCy)3]2Pb3 (Cy = Cyclohexyl, C6H11)
Michael A. Beswick; Natalie L. Cromhout; Christopher N. Harmer; Michael A. Paver; Paul R. Raithby; Moira-Ann Rennie; Alexander Steiner; Dominic S. Wright; Inorganic Chemistry 36 (1997) 1740–1744; doi:10.1021/ic961108b

data_4323393
_publ_section_title
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 Assembly of Mixed-Metal Cages Using Polyimido Antimony(III) Anions.
 Syntheses and Structures of [Sb3(NCy)4(HNCy)2]K.2(toluene),
 [Sb2(NCy)4]2M4 (M = Cu, Ag), and [Sb(NCy)3]2Pb3 (Cy = Cyclohexyl, C6H11)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1740
_journal_page_last               1744
_journal_paper_doi               10.1021/ic961108b
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C50 H84 K N6 Sb3'
_chemical_formula_weight         1173.58
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.24(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.418(3)
_cell_length_b                   11.457(2)
_cell_length_c                   24.798(6)
_cell_measurement_temperature    153(2)
_cell_volume                     5232.7(18)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_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  0.0160
_diffrn_reflns_av_sigmaI/netI    0.0161
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            5852
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         4.10
_exptl_absorpt_coefficient_mu    1.655
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.378
_exptl_absorpt_correction_type   'semi-empirical with psi-scans'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.409
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.041
_refine_ls_goodness_of_fit_obs   1.050
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         3409
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.038
_refine_ls_restrained_S_obs      1.046
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_obs          0.0265
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+24.2550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0659
_refine_ls_wR_factor_obs         0.0634
_reflns_number_observed          3119
_reflns_number_total             3409
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961108b_3.cif
_cod_data_source_block           la
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+24.2550P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+24.2550P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4323393