Zr11Sb18: A New Binary Antimonide Exhibiting an Unusual Sb Atom Network with Nonclassical Sb-Sb Bonding
Ingrid Elder; Chi-Shen Lee; Holger Kleinke; Inorganic Chemistry 41 (2002) 538–545; doi:10.1021/ic0108235

data_4317500
_publ_section_title
;
 Zr11Sb18: A New Binary Antimonide Exhibiting an Unusual Sb Atom Network
 with Nonclassical Sb-Sb Bonding
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              538
_journal_page_last               545
_journal_paper_doi               10.1021/ic0108235
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'Sb18 V0.63 Zr10.37'
_chemical_formula_weight         3169.34
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           122
_symmetry_cell_setting           1
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.7648(8)
_cell_length_b                   6.7648(8)
_cell_length_c                   60.056(9)
_cell_measurement_temperature    293(2)
_cell_volume                     2748.3(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       96
_diffrn_reflns_limit_l_min       -65
_diffrn_reflns_number            21277
_diffrn_reflns_theta_full        34.96
_diffrn_reflns_theta_max         34.96
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    21.272
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.37
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    7.660
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             5389
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.710
_refine_diff_density_min         -2.280
_refine_diff_density_rms         0.386
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.6(2)
_refine_ls_extinction_coef       0.000053(3)
_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   1.306
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         3018
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.306
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.158
_refine_ls_shift/su_mean         0.047
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0701
_reflns_number_gt                2420
_reflns_number_total             3018
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0108235_2.cif
_cod_data_source_block           zr10.4v0.6sb18
_cod_database_code               4317500