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_4323392
_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            'C43 H74 N6 Pb3 Sb2'
_chemical_formula_weight         1540.15
_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
_cell_angle_alpha                65.36(3)
_cell_angle_beta                 74.21(3)
_cell_angle_gamma                70.70(3)
_cell_formula_units_Z            2
_cell_length_a                   11.071(2)
_cell_length_b                   14.892(3)
_cell_length_c                   17.262(3)
_cell_measurement_temperature    153(2)
_cell_volume                     2411.3(10)
_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  0.1341
_diffrn_reflns_av_sigmaI/netI    0.1120
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9039
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         4.00
_exptl_absorpt_coefficient_mu    11.578
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.236
_exptl_absorpt_correction_type   'semi-empirical with psi-scans'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.121
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1444
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         4.538
_refine_diff_density_min         -5.777
_refine_diff_density_rms         0.533
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.063
_refine_ls_goodness_of_fit_obs   1.024
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         6233
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_restrained_S_obs      1.024
_refine_ls_R_factor_all          0.1337
_refine_ls_R_factor_obs          0.0909
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1503P)^2^+215.5831P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2961
_refine_ls_wR_factor_obs         0.2370
_reflns_number_observed          4360
_reflns_number_total             6242
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961108b_2.cif
_cod_data_source_block           mb10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1503P)^2^+215.5831P] 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^)+(0.1503P)^2^+215.5831P] 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        2411.3(8)
_cod_database_code               4323392