# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Holger Kleinke' _publ_contact_author_address ; Department of Chemistry University of Waterloo 200 University Ave W Waterloo Ontario N2L3G1 CANADA ; _publ_contact_author_email KLEINKE@UWATERLOO.CA _publ_section_title ; HfMoSb4, the first nonmetallic early transition metal antimonide ; loop_ _publ_author_name 'Holger Kleinke' 'Enkhtsetseg Dashjav' 'Shahab Derakhshan' 'Katja M. Kleinke' data_HfMoSb4 _database_code_depnum_ccdc_archive 'CCDC 242777' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Hf Mo Sb4' _chemical_formula_weight 761.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 10.321(3) _cell_length_b 3.6475(9) _cell_length_c 8.393(2) _cell_angle_alpha 90.00 _cell_angle_beta 119.895(5) _cell_angle_gamma 90.00 _cell_volume 273.91(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'prismatic shaped' _exptl_crystal_colour black _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.015 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 9.237 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 636 _exptl_absorpt_coefficient_mu 40.447 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.64 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1441 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0826 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 34.93 _reflns_number_total 645 _reflns_number_gt 429 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 645 _refine_ls_number_parameters 20 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.0913 _refine_ls_wR_factor_gt 0.0883 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.960 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hf Hf 0.15316(10) 0.0000 0.18998(13) 0.0094(3) Uani 0.501(5) 2 d SP . . Mo Mo 0.15316(10) 0.0000 0.18998(13) 0.0094(3) Uani 0.499(5) 2 d SP . . Sb1 Sb 0.40510(13) 0.0000 0.11280(17) 0.0128(3) Uani 1 2 d S . . Sb2 Sb 0.35328(13) 0.5000 0.46650(16) 0.0111(3) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hf 0.0131(5) 0.0090(4) 0.0071(5) 0.000 0.0058(4) 0.000 Mo 0.0131(5) 0.0090(4) 0.0071(5) 0.000 0.0058(4) 0.000 Sb1 0.0171(6) 0.0132(5) 0.0115(6) 0.000 0.0096(5) 0.000 Sb2 0.0144(5) 0.0104(5) 0.0103(6) 0.000 0.0075(4) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hf Sb2 2.8636(13) . ? Hf Sb2 2.8636(13) 1_545 ? Hf Sb2 2.9168(16) 7_556 ? Hf Sb1 2.9364(13) 7_545 ? Hf Sb1 2.9364(13) 7 ? Hf Sb1 2.9405(13) 3_445 ? Hf Sb1 2.9405(13) 3_455 ? Hf Sb1 2.9766(16) . ? Hf Hf 3.180(2) 5 ? Hf Mo 3.180(2) 5 ? Sb1 Mo 2.9364(13) 7_545 ? Sb1 Hf 2.9364(13) 7_545 ? Sb1 Mo 2.9364(13) 7 ? Sb1 Hf 2.9364(13) 7 ? Sb1 Mo 2.9405(13) 3 ? Sb1 Hf 2.9405(13) 3 ? Sb1 Hf 2.9405(13) 3_545 ? Sb1 Mo 2.9405(13) 3_545 ? Sb2 Sb2 2.791(2) 5_666 ? Sb2 Hf 2.8636(13) 1_565 ? Sb2 Mo 2.8636(13) 1_565 ? Sb2 Hf 2.9168(16) 7_556 ? Sb2 Mo 2.9168(16) 7_556 ? Sb2 Sb2 3.0629(19) 7_556 ? Sb2 Sb2 3.0629(19) 7_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Sb2 Hf Sb2 79.12(4) . 1_545 ? Sb2 Hf Sb2 63.99(4) . 7_556 ? Sb2 Hf Sb2 63.99(4) 1_545 7_556 ? Sb2 Hf Sb1 148.30(5) . 7_545 ? Sb2 Hf Sb1 93.42(3) 1_545 7_545 ? Sb2 Hf Sb1 139.44(3) 7_556 7_545 ? Sb2 Hf Sb1 93.42(3) . 7 ? Sb2 Hf Sb1 148.30(5) 1_545 7 ? Sb2 Hf Sb1 139.44(3) 7_556 7 ? Sb1 Hf Sb1 76.79(4) 7_545 7 ? Sb2 Hf Sb1 140.41(5) . 3_445 ? Sb2 Hf Sb1 88.89(3) 1_545 3_445 ? Sb2 Hf Sb1 76.79(4) 7_556 3_445 ? Sb1 Hf Sb1 69.14(4) 7_545 3_445 ? Sb1 Hf Sb1 114.48(4) 7 3_445 ? Sb2 Hf Sb1 88.89(3) . 3_455 ? Sb2 Hf Sb1 140.41(5) 1_545 3_455 ? Sb2 Hf Sb1 76.79(4) 7_556 3_455 ? Sb1 Hf Sb1 114.48(4) 7_545 3_455 ? Sb1 Hf Sb1 69.14(4) 7 3_455 ? Sb1 Hf Sb1 76.66(4) 3_445 3_455 ? Sb2 Hf Sb1 79.69(4) . . ? Sb2 Hf Sb1 79.69(4) 1_545 . ? Sb2 Hf Sb1 131.90(5) 7_556 . ? Sb1 Hf Sb1 68.65(4) 7_545 . ? Sb1 Hf Sb1 68.65(4) 7 . ? Sb1 Hf Sb1 135.33(3) 3_445 . ? Sb1 Hf Sb1 135.33(3) 3_455 . ? Sb2 Hf Hf 140.14(2) . 5 ? Sb2 Hf Hf 140.14(2) 1_545 5 ? Sb2 Hf Hf 119.35(5) 7_556 5 ? Sb1 Hf Hf 57.30(3) 7_545 5 ? Sb1 Hf Hf 57.30(3) 7 5 ? Sb1 Hf Hf 57.18(3) 3_445 5 ? Sb1 Hf Hf 57.18(3) 3_455 5 ? Sb1 Hf Hf 108.75(5) . 5 ? Sb2 Hf Mo 140.14(2) . 5 ? Sb2 Hf Mo 140.14(2) 1_545 5 ? Sb2 Hf Mo 119.35(5) 7_556 5 ? Sb1 Hf Mo 57.30(3) 7_545 5 ? Sb1 Hf Mo 57.30(3) 7 5 ? Sb1 Hf Mo 57.18(3) 3_445 5 ? Sb1 Hf Mo 57.18(3) 3_455 5 ? Sb1 Hf Mo 108.75(5) . 5 ? Hf Hf Mo 0.00(4) 5 5 ? Mo Sb1 Hf 0.00(4) 7_545 7_545 ? Mo Sb1 Mo 76.79(4) 7_545 7 ? Hf Sb1 Mo 76.79(4) 7_545 7 ? Mo Sb1 Hf 76.79(4) 7_545 7 ? Hf Sb1 Hf 76.79(4) 7_545 7 ? Mo Sb1 Hf 0.00(4) 7 7 ? Mo Sb1 Mo 110.86(4) 7_545 3 ? Hf Sb1 Mo 110.86(4) 7_545 3 ? Mo Sb1 Mo 65.52(4) 7 3 ? Hf Sb1 Mo 65.52(4) 7 3 ? Mo Sb1 Hf 110.86(4) 7_545 3 ? Hf Sb1 Hf 110.86(4) 7_545 3 ? Mo Sb1 Hf 65.52(4) 7 3 ? Hf Sb1 Hf 65.52(4) 7 3 ? Mo Sb1 Hf 0.00(4) 3 3 ? Mo Sb1 Hf 65.52(4) 7_545 3_545 ? Hf Sb1 Hf 65.52(4) 7_545 3_545 ? Mo Sb1 Hf 110.86(4) 7 3_545 ? Hf Sb1 Hf 110.86(4) 7 3_545 ? Mo Sb1 Hf 76.66(4) 3 3_545 ? Hf Sb1 Hf 76.66(4) 3 3_545 ? Mo Sb1 Mo 65.52(4) 7_545 3_545 ? Hf Sb1 Mo 65.52(4) 7_545 3_545 ? Mo Sb1 Mo 110.86(4) 7 3_545 ? Hf Sb1 Mo 110.86(4) 7 3_545 ? Mo Sb1 Mo 76.66(4) 3 3_545 ? Hf Sb1 Mo 76.66(4) 3 3_545 ? Hf Sb1 Mo 0.00(4) 3_545 3_545 ? Mo Sb1 Hf 111.35(4) 7_545 . ? Hf Sb1 Hf 111.35(4) 7_545 . ? Mo Sb1 Hf 111.35(4) 7 . ? Hf Sb1 Hf 111.35(4) 7 . ? Mo Sb1 Hf 135.33(3) 3 . ? Hf Sb1 Hf 135.33(3) 3 . ? Hf Sb1 Hf 135.33(3) 3_545 . ? Mo Sb1 Hf 135.33(3) 3_545 . ? Sb2 Sb2 Hf 115.79(5) 5_666 . ? Sb2 Sb2 Hf 115.79(5) 5_666 1_565 ? Hf Sb2 Hf 79.12(4) . 1_565 ? Sb2 Sb2 Mo 115.79(5) 5_666 1_565 ? Hf Sb2 Mo 79.12(4) . 1_565 ? Hf Sb2 Mo 0.00(4) 1_565 1_565 ? Sb2 Sb2 Hf 110.97(6) 5_666 7_556 ? Hf Sb2 Hf 116.01(4) . 7_556 ? Hf Sb2 Hf 116.01(4) 1_565 7_556 ? Mo Sb2 Hf 116.01(4) 1_565 7_556 ? Sb2 Sb2 Mo 110.97(6) 5_666 7_556 ? Hf Sb2 Mo 116.01(4) . 7_556 ? Hf Sb2 Mo 116.01(4) 1_565 7_556 ? Mo Sb2 Mo 116.01(4) 1_565 7_556 ? Hf Sb2 Mo 0.00(4) 7_556 7_556 ? Sb2 Sb2 Sb2 138.38(5) 5_666 7_556 ? Hf Sb2 Sb2 58.85(4) . 7_556 ? Hf Sb2 Sb2 103.96(6) 1_565 7_556 ? Mo Sb2 Sb2 103.96(6) 1_565 7_556 ? Hf Sb2 Sb2 57.16(4) 7_556 7_556 ? Mo Sb2 Sb2 57.16(4) 7_556 7_556 ? Sb2 Sb2 Sb2 138.38(5) 5_666 7_566 ? Hf Sb2 Sb2 103.96(6) . 7_566 ? Hf Sb2 Sb2 58.85(4) 1_565 7_566 ? Mo Sb2 Sb2 58.85(4) 1_565 7_566 ? Hf Sb2 Sb2 57.16(4) 7_556 7_566 ? Mo Sb2 Sb2 57.16(4) 7_556 7_566 ? Sb2 Sb2 Sb2 73.09(5) 7_556 7_566 ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 34.93 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 4.539 _refine_diff_density_min -3.288 _refine_diff_density_rms 0.751