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_4323402
_publ_section_title
;
 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            'C52 H96 Ag4 N8 O Sb4'
_chemical_formula_weight         1767.85
_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
_cell_angle_alpha                103.50(3)
_cell_angle_beta                 95.89(3)
_cell_angle_gamma                96.71(3)
_cell_formula_units_Z            2
_cell_length_a                   11.501(2)
_cell_length_b                   13.752(3)
_cell_length_c                   22.868(5)
_cell_measurement_temperature    293(2)
_cell_volume                     3461.1(14)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'siemens stoe AED'
_diffrn_measurement_method       omega/2theta
_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  0.0871
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            12163
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.50
_exptl_absorpt_coefficient_mu    2.679
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_correction_T_min  0.277
_exptl_absorpt_correction_type   'semi-empirical with psi-scans'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_description       cubes
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         2.807
_refine_diff_density_min         -2.871
_refine_diff_density_rms         0.472
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.109
_refine_ls_goodness_of_fit_obs   0.795
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         12107
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.183
_refine_ls_restrained_S_obs      0.795
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_obs          0.0513
_refine_ls_shift/esd_max         0.374
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1764P)^2^+49.1187P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2832
_refine_ls_wR_factor_obs         0.1740
_reflns_number_observed          10106
_reflns_number_total             12163
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961108b_1.cif
_cod_data_source_block           wmb01
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1764P)^2^+49.1187P] 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^)+(0.1764P)^2^+49.1187P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3461.1(12)
_cod_database_code               4323402