# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1817 data_global # 1. SUBMISSION DETAILS _publ_contact_autor ; Martin Nieger Institut f\"ur Anorganische Chemie Universit\"at Bonn Gerhard-Domagk-Str. 1 D-53121 Bonn Bundesrepublik Deutschland ; _publ_contact_author_phone '049 228 73-5823' _publ_contact_author_fax '049 228 73-5327' _publ_contact_author_email 'NIEGER@OC3062.CHEMIE.UNI-BONN.DE' _publ_requested_journal 'J. Chem. Soc. Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; enclosed you will fond the necessary data of our publication in J. Chem. Soc. Dalton Trans. ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and structural characterization of the first completely alkyl-substituted Ga-Sb Lewis acid-base adducts ; loop_ _publ_author_name _publ_author_address 'Schulz, Stephan' ; Institut f\"ur Anorganische Chemie Universit\"at Bonn Gerhard-Domagk-Str. 1 D-53121 Bonn Bundesrepublik Deutschland ; 'Nieger, Martin' ; Institut f\"ur Anorganische Chemie Universit\"at Bonn Gerhard-Domagk-Str. 1 D-53121 Bonn Bundesrepublik Deutschland ; #============================================================================== data_s36_mul_compound_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tri(tert.butyl)gallium-triethylantimon-adduct ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H42 Ga Sb' _chemical_formula_weight 449.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ga' 'Ga' 0.2307 1.6083 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P2(1)/c (No.14)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.1615(3) _cell_length_b 9.5735(2) _cell_length_c 16.0291(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.905(2) _cell_angle_gamma 90.00 _cell_volume 2172.88(8) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 41202 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blocks _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 2.477 _exptl_absorpt_correction_type 'empirical from multiple refl.' _exptl_absorpt_correction_T_min '0.4766 (0.4777; theor.)' _exptl_absorpt_correction_T_max '0.6789 (0.6372; theor.)' _exptl_absorpt_process_details 'MULABS (Platon98; cf Blessing, 1995)' _exptl_special_details ; dx = 39.733(4) mm; 2 x 90 sec., 2 deg., 384 frames, 9 sets; mos.= 0.738(1) deg. ; _diffrn_ambient_temperature 123(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 'Nonius KappaCCD' _diffrn_measurement_method 'rotation in phi and omega, 2 deg.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40096 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 28.36 _reflns_number_total 5368 _reflns_number_gt 5048 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0438P)^2^+10.0050P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5368 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.1140 _refine_ls_wR_factor_gt 0.1127 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.148 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Ga1 Ga 0.74826(3) 1.05010(4) 0.35700(2) 0.01734(11) Uani 1 1 d . . . Sb1 Sb 0.749721(16) 0.75844(2) 0.391983(15) 0.01753(9) Uani 1 1 d . . . C1 C 0.6297(3) 1.0684(4) 0.2819(3) 0.0246(8) Uani 1 1 d . . . C2 C 0.6357(4) 1.2121(6) 0.2394(3) 0.0379(11) Uani 1 1 d . . . H2A H 0.6945 1.2183 0.2082 0.057 Uiso 1 1 calc R . . H2B H 0.6348 1.2857 0.2819 0.057 Uiso 1 1 calc R . . H2C H 0.5817 1.2241 0.2011 0.057 Uiso 1 1 calc R . . C3 C 0.6262(3) 0.9574(6) 0.2127(3) 0.0387(11) Uani 1 1 d . . . H3A H 0.6846 0.9612 0.1808 0.058 Uiso 1 1 calc R . . H3B H 0.5720 0.9756 0.1754 0.058 Uiso 1 1 calc R . . H3C H 0.6197 0.8646 0.2378 0.058 Uiso 1 1 calc R . . C4 C 0.5386(3) 1.0579(6) 0.3298(3) 0.0372(11) Uani 1 1 d . . . H4A H 0.5350 0.9663 0.3568 0.056 Uiso 1 1 calc R . . H4B H 0.4848 1.0695 0.2913 0.056 Uiso 1 1 calc R . . H4C H 0.5372 1.1314 0.3724 0.056 Uiso 1 1 calc R . . C5 C 0.8752(3) 1.0727(4) 0.3007(3) 0.0237(8) Uani 1 1 d . . . C6 C 0.8758(3) 1.0188(6) 0.2114(3) 0.0372(11) Uani 1 1 d . . . H6A H 0.8253 1.0644 0.1789 0.056 Uiso 1 1 calc R . . H6B H 0.8654 0.9175 0.2113 0.056 Uiso 1 1 calc R . . H6C H 0.9369 1.0396 0.1864 0.056 Uiso 1 1 calc R . . C7 C 0.8979(4) 1.2311(5) 0.2996(3) 0.0351(10) Uani 1 1 d . . . H7A H 0.8480 1.2808 0.2686 0.053 Uiso 1 1 calc R . . H7B H 0.9586 1.2462 0.2725 0.053 Uiso 1 1 calc R . . H7C H 0.9014 1.2663 0.3570 0.053 Uiso 1 1 calc R . . C8 C 0.9552(3) 0.9998(6) 0.3491(3) 0.0334(10) Uani 1 1 d . . . H8A H 0.9563 1.0327 0.4070 0.050 Uiso 1 1 calc R . . H8B H 1.0157 1.0215 0.3231 0.050 Uiso 1 1 calc R . . H8C H 0.9449 0.8986 0.3480 0.050 Uiso 1 1 calc R . . C9 C 0.7374(3) 1.1294(4) 0.4745(2) 0.0246(8) Uani 1 1 d . . . C10 C 0.6624(3) 1.0534(5) 0.5260(3) 0.0301(9) Uani 1 1 d . . . H10A H 0.6023 1.0525 0.4949 0.045 Uiso 1 1 calc R . . H10B H 0.6543 1.1021 0.5792 0.045 Uiso 1 1 calc R . . H10C H 0.6829 0.9572 0.5367 0.045 Uiso 1 1 calc R . . C11 C 0.7048(4) 1.2827(5) 0.4656(3) 0.0348(10) Uani 1 1 d . . . H11A H 0.6453 1.2861 0.4336 0.052 Uiso 1 1 calc R . . H11B H 0.7531 1.3364 0.4364 0.052 Uiso 1 1 calc R . . H11C H 0.6954 1.3228 0.5211 0.052 Uiso 1 1 calc R . . C12 C 0.8295(3) 1.1254(6) 0.5240(3) 0.0366(10) Uani 1 1 d . . . H12A H 0.8787 1.1736 0.4928 0.055 Uiso 1 1 calc R . . H12B H 0.8482 1.0281 0.5335 0.055 Uiso 1 1 calc R . . H12C H 0.8210 1.1720 0.5778 0.055 Uiso 1 1 calc R . . C13 C 0.8129(3) 0.6793(5) 0.5058(3) 0.0340(10) Uani 1 1 d . . . H13A H 0.7895 0.7346 0.5534 0.041 Uiso 1 1 calc R . . H13B H 0.7925 0.5814 0.5138 0.041 Uiso 1 1 calc R . . C14 C 0.9204(4) 0.6848(7) 0.5061(4) 0.0516(15) Uani 1 1 d . . . H14A H 0.9450 0.6480 0.5592 0.077 Uiso 1 1 calc R . . H14B H 0.9411 0.7818 0.4994 0.077 Uiso 1 1 calc R . . H14C H 0.9441 0.6283 0.4600 0.077 Uiso 1 1 calc R . . C15 C 0.8195(3) 0.6196(5) 0.3074(3) 0.0321(9) Uani 1 1 d . . . H15A H 0.8829 0.6576 0.2953 0.038 Uiso 1 1 calc R . . H15B H 0.8284 0.5278 0.3350 0.038 Uiso 1 1 calc R . . C16 C 0.7651(4) 0.5983(6) 0.2251(3) 0.0403(11) Uani 1 1 d . . . H16A H 0.8009 0.5358 0.1889 0.060 Uiso 1 1 calc R . . H16B H 0.7562 0.6886 0.1973 0.060 Uiso 1 1 calc R . . H16C H 0.7033 0.5569 0.2364 0.060 Uiso 1 1 calc R . . C17 C 0.6181(3) 0.6478(5) 0.3980(3) 0.0338(9) Uani 1 1 d . . . H17A H 0.5794 0.6710 0.3479 0.041 Uiso 1 1 calc R . . H17B H 0.6310 0.5462 0.3967 0.041 Uiso 1 1 calc R . . C18 C 0.5617(4) 0.6813(6) 0.4755(4) 0.0422(12) Uani 1 1 d . . . H18A H 0.5026 0.6280 0.4743 0.063 Uiso 1 1 calc R . . H18B H 0.5474 0.7815 0.4767 0.063 Uiso 1 1 calc R . . H18C H 0.5987 0.6561 0.5254 0.063 Uiso 1 1 calc R . . 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 Ga1 0.01572(19) 0.0162(2) 0.0202(2) 0.00105(14) 0.00136(14) 0.00047(13) Sb1 0.01654(13) 0.01567(13) 0.02038(14) -0.00035(8) 0.00031(9) 0.00002(8) C1 0.0193(17) 0.0283(19) 0.0260(19) 0.0060(15) -0.0036(14) 0.0007(15) C2 0.036(2) 0.044(3) 0.033(2) 0.013(2) -0.0048(19) 0.004(2) C3 0.030(2) 0.059(3) 0.026(2) -0.002(2) -0.0060(17) -0.001(2) C4 0.022(2) 0.060(3) 0.030(2) 0.001(2) -0.0007(16) -0.002(2) C5 0.0184(17) 0.0252(18) 0.0278(19) 0.0032(15) 0.0058(14) -0.0016(14) C6 0.030(2) 0.055(3) 0.027(2) 0.000(2) 0.0091(17) 0.001(2) C7 0.034(2) 0.032(2) 0.039(3) 0.0041(19) 0.0103(19) -0.0043(18) C8 0.0215(19) 0.046(3) 0.033(2) -0.003(2) 0.0032(16) 0.0008(18) C9 0.033(2) 0.0222(18) 0.0186(17) -0.0006(14) 0.0033(15) 0.0009(16) C10 0.031(2) 0.038(2) 0.0221(19) -0.0030(17) 0.0037(16) -0.0005(18) C11 0.044(3) 0.028(2) 0.033(2) -0.0021(18) 0.0094(19) -0.0002(19) C12 0.027(2) 0.059(3) 0.024(2) -0.005(2) 0.0001(16) -0.005(2) C13 0.041(3) 0.039(2) 0.022(2) 0.0028(18) -0.0029(17) 0.000(2) C14 0.037(3) 0.068(4) 0.049(3) 0.021(3) -0.018(2) 0.000(3) C15 0.035(2) 0.033(2) 0.029(2) -0.0073(18) 0.0039(17) 0.0083(18) C16 0.056(3) 0.039(3) 0.025(2) -0.010(2) 0.002(2) 0.007(2) C17 0.030(2) 0.033(2) 0.038(2) -0.0007(19) 0.0021(18) -0.0041(18) C18 0.036(3) 0.043(3) 0.049(3) 0.003(2) 0.019(2) -0.003(2) _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 Ga1 C5 2.035(4) . ? Ga1 C9 2.039(4) . ? Ga1 C1 2.058(4) . ? Ga1 Sb1 2.8479(5) . ? Sb1 C17 2.148(5) . ? Sb1 C15 2.150(4) . ? Sb1 C13 2.156(4) . ? C1 C4 1.515(6) . ? C1 C3 1.536(7) . ? C1 C2 1.539(6) . ? C5 C6 1.522(6) . ? C5 C8 1.531(6) . ? C5 C7 1.550(6) . ? C9 C12 1.516(6) . ? C9 C10 1.539(6) . ? C9 C11 1.544(6) . ? C13 C14 1.523(7) . ? C15 C16 1.532(6) . ? C17 C18 1.522(7) . ? 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 C5 Ga1 C9 116.72(17) . . ? C5 Ga1 C1 116.71(17) . . ? C9 Ga1 C1 115.88(17) . . ? C5 Ga1 Sb1 100.83(12) . . ? C9 Ga1 Sb1 100.57(12) . . ? C1 Ga1 Sb1 101.64(12) . . ? C17 Sb1 C15 97.55(19) . . ? C17 Sb1 C13 97.91(19) . . ? C15 Sb1 C13 97.32(18) . . ? C17 Sb1 Ga1 119.26(13) . . ? C15 Sb1 Ga1 118.95(13) . . ? C13 Sb1 Ga1 120.84(14) . . ? C4 C1 C3 107.6(4) . . ? C4 C1 C2 109.7(4) . . ? C3 C1 C2 107.5(4) . . ? C4 C1 Ga1 113.0(3) . . ? C3 C1 Ga1 112.4(3) . . ? C2 C1 Ga1 106.5(3) . . ? C6 C5 C8 107.8(4) . . ? C6 C5 C7 108.5(4) . . ? C8 C5 C7 107.4(4) . . ? C6 C5 Ga1 113.5(3) . . ? C8 C5 Ga1 112.3(3) . . ? C7 C5 Ga1 107.1(3) . . ? C12 C9 C10 107.6(3) . . ? C12 C9 C11 109.0(4) . . ? C10 C9 C11 106.9(4) . . ? C12 C9 Ga1 113.4(3) . . ? C10 C9 Ga1 112.5(3) . . ? C11 C9 Ga1 107.1(3) . . ? C14 C13 Sb1 113.1(3) . . ? C16 C15 Sb1 113.3(3) . . ? C18 C17 Sb1 113.5(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 Ga1 Sb1 C17 -151.60(19) . . . . ? C9 Ga1 Sb1 C17 88.30(19) . . . . ? C1 Ga1 Sb1 C17 -31.15(19) . . . . ? C5 Ga1 Sb1 C15 -32.79(19) . . . . ? C9 Ga1 Sb1 C15 -152.89(19) . . . . ? C1 Ga1 Sb1 C15 87.66(19) . . . . ? C5 Ga1 Sb1 C13 87.2(2) . . . . ? C9 Ga1 Sb1 C13 -32.9(2) . . . . ? C1 Ga1 Sb1 C13 -152.4(2) . . . . ? C5 Ga1 C1 C4 -176.8(3) . . . . ? C9 Ga1 C1 C4 -33.4(4) . . . . ? Sb1 Ga1 C1 C4 74.6(3) . . . . ? C5 Ga1 C1 C3 61.2(4) . . . . ? C9 Ga1 C1 C3 -155.4(3) . . . . ? Sb1 Ga1 C1 C3 -47.4(3) . . . . ? C5 Ga1 C1 C2 -56.3(3) . . . . ? C9 Ga1 C1 C2 87.1(3) . . . . ? Sb1 Ga1 C1 C2 -164.9(3) . . . . ? C9 Ga1 C5 C6 -176.5(3) . . . . ? C1 Ga1 C5 C6 -33.3(4) . . . . ? Sb1 Ga1 C5 C6 75.7(3) . . . . ? C9 Ga1 C5 C8 60.9(4) . . . . ? C1 Ga1 C5 C8 -156.0(3) . . . . ? Sb1 Ga1 C5 C8 -46.9(3) . . . . ? C9 Ga1 C5 C7 -56.8(3) . . . . ? C1 Ga1 C5 C7 86.3(3) . . . . ? Sb1 Ga1 C5 C7 -164.6(3) . . . . ? C5 Ga1 C9 C12 -31.0(4) . . . . ? C1 Ga1 C9 C12 -174.5(3) . . . . ? Sb1 Ga1 C9 C12 76.9(3) . . . . ? C5 Ga1 C9 C10 -153.5(3) . . . . ? C1 Ga1 C9 C10 63.1(3) . . . . ? Sb1 Ga1 C9 C10 -45.5(3) . . . . ? C5 Ga1 C9 C11 89.3(3) . . . . ? C1 Ga1 C9 C11 -54.2(3) . . . . ? Sb1 Ga1 C9 C11 -162.7(3) . . . . ? C17 Sb1 C13 C14 155.8(4) . . . . ? C15 Sb1 C13 C14 57.1(4) . . . . ? Ga1 Sb1 C13 C14 -73.1(4) . . . . ? C17 Sb1 C15 C16 56.4(4) . . . . ? C13 Sb1 C15 C16 155.4(4) . . . . ? Ga1 Sb1 C15 C16 -73.2(4) . . . . ? C15 Sb1 C17 C18 158.4(4) . . . . ? C13 Sb1 C17 C18 59.9(4) . . . . ? Ga1 Sb1 C17 C18 -72.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max '1.601 (near Sb)' _refine_diff_density_min -0.956 _refine_diff_density_rms 0.145 #============================================================================== data_schulz20_compound_7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tri(tert.butyl)gallium-tri(isopropyl)antimon-adduct ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H48 Ga Sb' _chemical_formula_weight 492.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ga' 'Ga' 0.2307 1.6083 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P2(1)/c (No.14)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.6128(2) _cell_length_b 9.0089(2) _cell_length_c 20.0307(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.750(1) _cell_angle_gamma 90.00 _cell_volume 2455.35(7) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 32772 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blocks _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.55 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 2.198 _exptl_absorpt_correction_type 'empirical from multiple refl' _exptl_absorpt_correction_T_min '0.3988 (0.3522, theor.)' _exptl_absorpt_correction_T_max '0.4383 (0.4062, theor.)' _exptl_absorpt_process_details 'MULABS (cf. Blessing, 1995) in PLATON98' _exptl_special_details ; dx = 39.785(3) mm; 2 x 30 sec., 1 deg., 551 frames; mos.= 0.579(1) ; _diffrn_ambient_temperature 123(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 'Nonius KappaCCD' _diffrn_measurement_method 'rotation in phi and omega, 1 deg.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31295 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 28.27 _reflns_number_total 5802 _reflns_number_gt 5523 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0206P)^2^+1.4385P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5802 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0214 _refine_ls_R_factor_gt 0.0198 _refine_ls_wR_factor_ref 0.0488 _refine_ls_wR_factor_gt 0.0482 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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 Sb1 Sb 0.731685(7) 0.871680(11) 0.222643(5) 0.01408(4) Uani 1 1 d . . . C1 C 0.58366(11) 0.81161(18) 0.25236(8) 0.0182(3) Uani 1 1 d . . . H1 H 0.5671 0.7159 0.2294 0.022 Uiso 1 1 calc R . . C2 C 0.50877(13) 0.9252(2) 0.22669(10) 0.0295(4) Uani 1 1 d . . . H2A H 0.5169 0.9409 0.1788 0.044 Uiso 1 1 calc R . . H2B H 0.5189 1.0192 0.2505 0.044 Uiso 1 1 calc R . . H2C H 0.4423 0.8885 0.2343 0.044 Uiso 1 1 calc R . . C3 C 0.57302(13) 0.7842(2) 0.32683(9) 0.0269(4) Uani 1 1 d . . . H3A H 0.6220 0.7111 0.3422 0.040 Uiso 1 1 calc R . . H3B H 0.5069 0.7464 0.3349 0.040 Uiso 1 1 calc R . . H3C H 0.5833 0.8775 0.3512 0.040 Uiso 1 1 calc R . . C4 C 0.81432(12) 0.76116(19) 0.30328(8) 0.0199(3) Uani 1 1 d . . . H4 H 0.7841 0.7893 0.3464 0.024 Uiso 1 1 calc R . . C5 C 0.80591(14) 0.5929(2) 0.29563(9) 0.0267(4) Uani 1 1 d . . . H5A H 0.7364 0.5643 0.2940 0.040 Uiso 1 1 calc R . . H5B H 0.8394 0.5443 0.3337 0.040 Uiso 1 1 calc R . . H5C H 0.8365 0.5621 0.2542 0.040 Uiso 1 1 calc R . . C6 C 0.92197(13) 0.8087(2) 0.30698(10) 0.0312(4) Uani 1 1 d . . . H6A H 0.9259 0.9168 0.3120 0.047 Uiso 1 1 calc R . . H6B H 0.9540 0.7790 0.2659 0.047 Uiso 1 1 calc R . . H6C H 0.9551 0.7609 0.3454 0.047 Uiso 1 1 calc R . . C7 C 0.73920(13) 1.10296(19) 0.25514(9) 0.0236(3) Uani 1 1 d . . . H7 H 0.6844 1.1567 0.2311 0.028 Uiso 1 1 calc R . . C8 C 0.72509(18) 1.1258(2) 0.32979(11) 0.0374(5) Uani 1 1 d . . . H8A H 0.6633 1.0796 0.3426 0.056 Uiso 1 1 calc R . . H8B H 0.7230 1.2323 0.3396 0.056 Uiso 1 1 calc R . . H8C H 0.7799 1.0802 0.3551 0.056 Uiso 1 1 calc R . . C9 C 0.83498(16) 1.1741(2) 0.23352(11) 0.0346(4) Uani 1 1 d . . . H9A H 0.8423 1.1588 0.1855 0.052 Uiso 1 1 calc R . . H9B H 0.8905 1.1283 0.2581 0.052 Uiso 1 1 calc R . . H9C H 0.8336 1.2807 0.2431 0.052 Uiso 1 1 calc R . . Ga1 Ga 0.760868(12) 0.802808(18) 0.080033(8) 0.01425(5) Uani 1 1 d . . . C10 C 0.90800(11) 0.76438(19) 0.07437(8) 0.0197(3) Uani 1 1 d . . . C11 C 0.97056(13) 0.8856(2) 0.10824(10) 0.0273(4) Uani 1 1 d . . . H11A H 0.9519 0.9825 0.0897 0.041 Uiso 1 1 calc R . . H11B H 1.0402 0.8668 0.1004 0.041 Uiso 1 1 calc R . . H11C H 0.9597 0.8850 0.1564 0.041 Uiso 1 1 calc R . . C12 C 0.93988(13) 0.6155(2) 0.10452(10) 0.0272(4) Uani 1 1 d . . . H12A H 0.9015 0.5354 0.0833 0.041 Uiso 1 1 calc R . . H12B H 0.9287 0.6160 0.1526 0.041 Uiso 1 1 calc R . . H12C H 1.0099 0.5995 0.0970 0.041 Uiso 1 1 calc R . . C13 C 0.93142(13) 0.7603(2) -0.00040(9) 0.0269(4) Uani 1 1 d . . . H13A H 0.8924 0.6823 -0.0226 0.040 Uiso 1 1 calc R . . H13B H 1.0015 0.7395 -0.0053 0.040 Uiso 1 1 calc R . . H13C H 0.9153 0.8565 -0.0208 0.040 Uiso 1 1 calc R . . C14 C 0.67261(12) 0.62004(18) 0.07109(8) 0.0187(3) Uani 1 1 d . . . C15 C 0.69671(13) 0.5454(2) 0.00441(8) 0.0251(4) Uani 1 1 d . . . H15A H 0.6859 0.6163 -0.0322 0.038 Uiso 1 1 calc R . . H15B H 0.6540 0.4589 -0.0028 0.038 Uiso 1 1 calc R . . H15C H 0.7656 0.5135 0.0058 0.038 Uiso 1 1 calc R . . C16 C 0.56286(12) 0.6583(2) 0.06922(9) 0.0256(4) Uani 1 1 d . . . H16A H 0.5492 0.7322 0.0343 0.038 Uiso 1 1 calc R . . H16B H 0.5448 0.6987 0.1126 0.038 Uiso 1 1 calc R . . H16C H 0.5244 0.5684 0.0596 0.038 Uiso 1 1 calc R . . C17 C 0.69071(13) 0.50546(19) 0.12670(9) 0.0234(3) Uani 1 1 d . . . H17A H 0.7607 0.4798 0.1294 0.035 Uiso 1 1 calc R . . H17B H 0.6520 0.4160 0.1168 0.035 Uiso 1 1 calc R . . H17C H 0.6710 0.5473 0.1694 0.035 Uiso 1 1 calc R . . C18 C 0.71029(12) 0.99155(18) 0.03386(8) 0.0197(3) Uani 1 1 d . . . C19 C 0.78817(15) 1.1136(2) 0.03010(10) 0.0295(4) Uani 1 1 d . . . H19A H 0.8469 1.0738 0.0093 0.044 Uiso 1 1 calc R . . H19B H 0.8055 1.1486 0.0753 0.044 Uiso 1 1 calc R . . H19C H 0.7620 1.1964 0.0033 0.044 Uiso 1 1 calc R . . C20 C 0.62005(13) 1.0581(2) 0.06617(9) 0.0260(4) Uani 1 1 d . . . H20A H 0.5690 0.9819 0.0694 0.039 Uiso 1 1 calc R . . H20B H 0.5949 1.1409 0.0389 0.039 Uiso 1 1 calc R . . H20C H 0.6383 1.0942 0.1110 0.039 Uiso 1 1 calc R . . C21 C 0.68026(14) 0.9478(2) -0.03827(8) 0.0277(4) Uani 1 1 d . . . H21A H 0.7369 0.9047 -0.0603 0.042 Uiso 1 1 calc R . . H21B H 0.6578 1.0362 -0.0629 0.042 Uiso 1 1 calc R . . H21C H 0.6270 0.8747 -0.0376 0.042 Uiso 1 1 calc R . . 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 Sb1 0.01530(6) 0.01318(6) 0.01381(6) -0.00050(3) 0.00135(4) 0.00007(3) C1 0.0165(7) 0.0187(8) 0.0195(8) 0.0002(6) 0.0038(6) -0.0008(6) C2 0.0211(8) 0.0339(10) 0.0338(10) 0.0074(8) 0.0063(7) 0.0086(7) C3 0.0253(8) 0.0342(10) 0.0216(8) 0.0024(7) 0.0058(7) -0.0029(7) C4 0.0222(8) 0.0230(8) 0.0142(7) 0.0001(6) -0.0013(6) 0.0047(6) C5 0.0347(9) 0.0224(9) 0.0229(8) 0.0035(7) -0.0005(7) 0.0066(7) C6 0.0232(8) 0.0399(11) 0.0300(10) -0.0005(8) -0.0059(7) 0.0025(8) C7 0.0304(9) 0.0137(7) 0.0267(9) -0.0033(6) 0.0017(7) -0.0010(6) C8 0.0543(13) 0.0269(10) 0.0318(11) -0.0133(8) 0.0129(9) -0.0080(9) C9 0.0447(11) 0.0219(9) 0.0377(11) -0.0040(8) 0.0084(9) -0.0129(8) Ga1 0.01440(8) 0.01382(8) 0.01454(8) 0.00048(6) 0.00075(6) -0.00021(6) C10 0.0155(7) 0.0228(8) 0.0208(8) 0.0012(6) 0.0029(6) 0.0003(6) C11 0.0197(8) 0.0336(10) 0.0285(9) -0.0020(7) 0.0019(7) -0.0049(7) C12 0.0204(8) 0.0296(10) 0.0317(10) 0.0041(7) 0.0021(7) 0.0066(7) C13 0.0249(8) 0.0318(10) 0.0245(9) -0.0011(7) 0.0080(7) -0.0015(7) C14 0.0193(7) 0.0179(8) 0.0190(8) -0.0012(6) -0.0004(6) -0.0029(6) C15 0.0317(9) 0.0220(8) 0.0214(8) -0.0058(7) -0.0013(7) -0.0035(7) C16 0.0196(8) 0.0293(9) 0.0277(9) -0.0031(7) -0.0019(7) -0.0046(7) C17 0.0276(8) 0.0174(8) 0.0252(8) 0.0013(7) 0.0007(7) -0.0047(6) C18 0.0242(8) 0.0176(8) 0.0174(7) 0.0027(6) 0.0012(6) 0.0025(6) C19 0.0350(10) 0.0192(9) 0.0343(10) 0.0062(7) 0.0038(8) -0.0014(7) C20 0.0299(9) 0.0244(9) 0.0238(8) 0.0031(7) 0.0012(7) 0.0089(7) C21 0.0351(9) 0.0307(10) 0.0172(8) 0.0040(7) -0.0007(7) 0.0054(8) _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 Sb1 C4 2.1805(15) . ? Sb1 C7 2.1843(17) . ? Sb1 C1 2.1866(15) . ? Sb1 Ga1 2.96178(19) . ? C1 C2 1.523(2) . ? C1 C3 1.523(2) . ? C4 C6 1.526(2) . ? C4 C5 1.528(2) . ? C7 C9 1.527(3) . ? C7 C8 1.527(3) . ? Ga1 C10 2.0392(15) . ? Ga1 C14 2.0429(16) . ? Ga1 C18 2.0450(16) . ? C10 C12 1.529(2) . ? C10 C11 1.530(2) . ? C10 C13 1.541(2) . ? C14 C16 1.533(2) . ? C14 C17 1.533(2) . ? C14 C15 1.540(2) . ? C18 C20 1.528(2) . ? C18 C19 1.531(2) . ? C18 C21 1.541(2) . ? 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 C4 Sb1 C7 101.33(7) . . ? C4 Sb1 C1 98.29(6) . . ? C7 Sb1 C1 100.96(6) . . ? C4 Sb1 Ga1 122.51(4) . . ? C7 Sb1 Ga1 118.74(5) . . ? C1 Sb1 Ga1 111.26(4) . . ? C2 C1 C3 110.91(14) . . ? C2 C1 Sb1 110.78(11) . . ? C3 C1 Sb1 115.01(11) . . ? C6 C4 C5 110.63(15) . . ? C6 C4 Sb1 112.37(12) . . ? C5 C4 Sb1 110.09(11) . . ? C9 C7 C8 110.79(16) . . ? C9 C7 Sb1 110.38(12) . . ? C8 C7 Sb1 114.47(12) . . ? C10 Ga1 C14 115.74(7) . . ? C10 Ga1 C18 115.70(7) . . ? C14 Ga1 C18 116.20(7) . . ? C10 Ga1 Sb1 104.48(5) . . ? C14 Ga1 Sb1 99.07(5) . . ? C18 Ga1 Sb1 102.05(5) . . ? C12 C10 C11 107.67(14) . . ? C12 C10 C13 107.36(14) . . ? C11 C10 C13 108.60(14) . . ? C12 C10 Ga1 113.23(11) . . ? C11 C10 Ga1 112.85(11) . . ? C13 C10 Ga1 106.90(11) . . ? C16 C14 C17 107.70(14) . . ? C16 C14 C15 108.08(14) . . ? C17 C14 C15 107.60(14) . . ? C16 C14 Ga1 113.03(11) . . ? C17 C14 Ga1 113.45(11) . . ? C15 C14 Ga1 106.73(11) . . ? C20 C18 C19 107.82(15) . . ? C20 C18 C21 107.69(14) . . ? C19 C18 C21 107.56(14) . . ? C20 C18 Ga1 113.48(11) . . ? C19 C18 Ga1 113.28(11) . . ? C21 C18 Ga1 106.71(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 Sb1 C1 C2 153.89(12) . . . . ? C7 Sb1 C1 C2 50.57(13) . . . . ? Ga1 Sb1 C1 C2 -76.36(12) . . . . ? C4 Sb1 C1 C3 27.15(13) . . . . ? C7 Sb1 C1 C3 -76.17(13) . . . . ? Ga1 Sb1 C1 C3 156.90(11) . . . . ? C7 Sb1 C4 C6 -64.30(13) . . . . ? C1 Sb1 C4 C6 -167.32(13) . . . . ? Ga1 Sb1 C4 C6 70.86(13) . . . . ? C7 Sb1 C4 C5 171.90(12) . . . . ? C1 Sb1 C4 C5 68.89(12) . . . . ? Ga1 Sb1 C4 C5 -52.94(13) . . . . ? C4 Sb1 C7 C9 84.23(14) . . . . ? C1 Sb1 C7 C9 -174.90(13) . . . . ? Ga1 Sb1 C7 C9 -53.07(14) . . . . ? C4 Sb1 C7 C8 -41.59(15) . . . . ? C1 Sb1 C7 C8 59.28(15) . . . . ? Ga1 Sb1 C7 C8 -178.89(13) . . . . ? C4 Sb1 Ga1 C10 -36.53(7) . . . . ? C7 Sb1 Ga1 C10 91.42(7) . . . . ? C1 Sb1 Ga1 C10 -152.09(7) . . . . ? C4 Sb1 Ga1 C14 83.17(7) . . . . ? C7 Sb1 Ga1 C14 -148.88(7) . . . . ? C1 Sb1 Ga1 C14 -32.39(7) . . . . ? C4 Sb1 Ga1 C18 -157.41(7) . . . . ? C7 Sb1 Ga1 C18 -29.45(7) . . . . ? C1 Sb1 Ga1 C18 87.04(7) . . . . ? C14 Ga1 C10 C12 -34.16(14) . . . . ? C18 Ga1 C10 C12 -175.07(12) . . . . ? Sb1 Ga1 C10 C12 73.61(12) . . . . ? C14 Ga1 C10 C11 -156.81(12) . . . . ? C18 Ga1 C10 C11 62.29(14) . . . . ? Sb1 Ga1 C10 C11 -49.04(12) . . . . ? C14 Ga1 C10 C13 83.86(13) . . . . ? C18 Ga1 C10 C13 -57.04(13) . . . . ? Sb1 Ga1 C10 C13 -168.37(10) . . . . ? C10 Ga1 C14 C16 -174.63(11) . . . . ? C18 Ga1 C14 C16 -33.92(14) . . . . ? Sb1 Ga1 C14 C16 74.39(12) . . . . ? C10 Ga1 C14 C17 62.39(14) . . . . ? C18 Ga1 C14 C17 -156.91(11) . . . . ? Sb1 Ga1 C14 C17 -48.60(12) . . . . ? C10 Ga1 C14 C15 -55.94(13) . . . . ? C18 Ga1 C14 C15 84.76(12) . . . . ? Sb1 Ga1 C14 C15 -166.93(10) . . . . ? C10 Ga1 C18 C20 -150.72(12) . . . . ? C14 Ga1 C18 C20 68.56(14) . . . . ? Sb1 Ga1 C18 C20 -37.98(12) . . . . ? C10 Ga1 C18 C19 -27.34(14) . . . . ? C14 Ga1 C18 C19 -168.05(12) . . . . ? Sb1 Ga1 C18 C19 85.41(12) . . . . ? C10 Ga1 C18 C21 90.84(12) . . . . ? C14 Ga1 C18 C21 -49.88(13) . . . . ? Sb1 Ga1 C18 C21 -156.42(10) . . . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 0.446 _refine_diff_density_min -0.704 _refine_diff_density_rms 0.070 #==============================================================================