# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1591 data_99255 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 99255/BL045 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H18 Ga2 N4' _chemical_formula_weight 261.66 _Chemical_compound_source 'Bing Luo' 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' 'N' 'N' 0.0061 0.0033 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 6.8583(5) _cell_length_b 19.607(2) _cell_length_c 8.0977(6) _cell_angle_alpha 90.000(2) _cell_angle_beta 95.323(2) _cell_angle_gamma 90.000(1) _cell_volume 1084.19(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2084 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 4.920 _exptl_absorpt_correction_type 'multi-scans' _exptl_absorpt_correction_T_min 0.5773 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; Absorption correction was carried out using the program SADABS, G. Sheldrick (1999). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart CCD, Siemens' _diffrn_measurement_method 'omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3964 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.02 _reflns_number_total 1718 _reflns_number_gt 1554 _reflns_threshold_expression 2sigma(I) _computing_data_collection 'Smart, Bruker' _computing_cell_refinement 'Saint, Bruker' _computing_data_reduction 'Saint, Bruker' _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^)+(0.0305P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0007(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(3) _refine_ls_number_reflns 1718 _refine_ls_number_parameters 132 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0635 _refine_ls_wR_factor_gt 0.0612 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.032 _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 0.87109(9) 0.87417(3) 0.09319(8) 0.02740(18) Uani 1 1 d D . . H1G H 0.970(14) 0.889(5) -0.061(8) 0.11(4) Uiso 1 1 d D . . H2G H 0.944(10) 0.848(3) 0.263(5) 0.054(19) Uiso 1 1 d D . . Ga2 Ga 0.46280(8) 0.91624(3) 0.06414(7) 0.02886(19) Uani 1 1 d D . . H3G H 0.344(9) 0.913(3) 0.212(6) 0.04(2) Uiso 1 1 d D . . H4G H 0.412(12) 0.953(4) -0.098(6) 0.09(3) Uiso 1 1 d D . . N1 N 0.7230(7) 0.9599(3) 0.1235(6) 0.0240(11) Uani 1 1 d . . . H1N H 0.720(8) 0.970(3) 0.220(7) 0.014(15) Uiso 1 1 d . . . N2 N 0.7708(8) 1.0174(3) 0.0212(6) 0.0287(12) Uani 1 1 d . . . N3 N 0.6099(8) 0.8276(3) 0.0445(7) 0.0292(12) Uani 1 1 d . . . H3N H 0.611(12) 0.810(4) -0.045(10) 0.06(3) Uiso 1 1 d . . . N4 N 0.5774(8) 0.7737(2) 0.1613(6) 0.0317(12) Uani 1 1 d . . . C1 C 0.9762(11) 1.0372(3) 0.0619(9) 0.0354(14) Uani 1 1 d . . . H1A H 1.0618 0.9995 0.0356 0.08(3) Uiso 1 1 calc R . . H1B H 0.9982 1.0479 0.1803 0.027(15) Uiso 1 1 calc R . . H1C H 1.0057 1.0774 -0.0032 0.036(18) Uiso 1 1 calc R . . C2 C 0.6422(10) 1.0749(4) 0.0517(8) 0.0356(16) Uani 1 1 d . . . H2A H 0.5056 1.0617 0.0225 0.013(14) Uiso 1 1 calc R . . H2B H 0.6749 1.1139 -0.0162 0.025(17) Uiso 1 1 calc R . . H2C H 0.6603 1.0875 0.1693 0.07(3) Uiso 1 1 calc R . . C3 C 0.7112(11) 0.7171(3) 0.1338(9) 0.0439(18) Uani 1 1 d . . . H3A H 0.8469 0.7331 0.1515 0.06(2) Uiso 1 1 calc R . . H3B H 0.6850 0.7003 0.0199 0.09(3) Uiso 1 1 calc R . . H3C H 0.6908 0.6801 0.2118 0.07(2) Uiso 1 1 calc R . . C4 C 0.3732(10) 0.7502(4) 0.1345(8) 0.0426(18) Uani 1 1 d . . . H4A H 0.2856 0.7864 0.1665 0.07(3) Uiso 1 1 calc R . . H4B H 0.3562 0.7096 0.2020 0.032(15) Uiso 1 1 calc R . . H4C H 0.3419 0.7391 0.0170 0.05(2) 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 0.0269(4) 0.0246(4) 0.0304(3) 0.0010(3) 0.0013(3) -0.0014(3) Ga2 0.0264(4) 0.0272(4) 0.0327(4) 0.0015(3) 0.0013(3) -0.0029(3) N1 0.030(3) 0.026(3) 0.016(3) 0.002(2) 0.003(2) -0.008(2) N2 0.040(3) 0.019(3) 0.027(3) 0.000(2) 0.002(2) -0.003(2) N3 0.035(3) 0.022(3) 0.031(3) 0.005(3) 0.004(2) -0.004(3) N4 0.040(3) 0.023(3) 0.031(3) 0.009(2) -0.002(2) -0.006(2) C1 0.039(4) 0.028(3) 0.037(3) 0.001(4) -0.006(3) -0.009(4) C2 0.041(4) 0.023(4) 0.043(4) -0.001(3) 0.003(3) 0.003(3) C3 0.050(5) 0.027(4) 0.053(4) 0.003(4) -0.006(4) 0.001(4) C4 0.043(4) 0.038(4) 0.048(4) 0.012(3) 0.008(4) -0.014(4) _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 N1 1.991(5) . ? Ga1 N3 2.017(5) . ? Ga1 Ga2 2.9076(9) . ? Ga1 H1G 1.51(3) . ? Ga1 H2G 1.51(3) . ? Ga2 N1 1.997(5) . ? Ga2 N3 2.024(6) . ? Ga2 H3G 1.51(3) . ? Ga2 H4G 1.51(3) . ? N1 N2 1.454(7) . ? N1 H1N 0.81(5) . ? N2 C2 1.466(8) . ? N2 C1 1.469(8) . ? N3 N4 1.449(7) . ? N3 H3N 0.80(8) . ? N4 C3 1.470(9) . ? N4 C4 1.471(8) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? 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 N1 Ga1 N3 87.3(2) . . ? N1 Ga1 Ga2 43.28(14) . . ? N3 Ga1 Ga2 44.07(16) . . ? N1 Ga1 H1G 102(4) . . ? N3 Ga1 H1G 113(4) . . ? Ga2 Ga1 H1G 113(4) . . ? N1 Ga1 H2G 108(2) . . ? N3 Ga1 H2G 104(3) . . ? Ga2 Ga1 H2G 114(3) . . ? H1G Ga1 H2G 133(5) . . ? N1 Ga2 N3 86.9(2) . . ? N1 Ga2 Ga1 43.10(16) . . ? N3 Ga2 Ga1 43.88(15) . . ? N1 Ga2 H3G 111(3) . . ? N3 Ga2 H3G 110(2) . . ? Ga1 Ga2 H3G 121(3) . . ? N1 Ga2 H4G 98(3) . . ? N3 Ga2 H4G 115(3) . . ? Ga1 Ga2 H4G 111(3) . . ? H3G Ga2 H4G 128(4) . . ? N2 N1 Ga1 116.1(4) . . ? N2 N1 Ga2 116.0(4) . . ? Ga1 N1 Ga2 93.6(2) . . ? N2 N1 H1N 113(4) . . ? Ga1 N1 H1N 113(4) . . ? Ga2 N1 H1N 103(4) . . ? N1 N2 C2 109.2(5) . . ? N1 N2 C1 109.8(5) . . ? C2 N2 C1 109.8(5) . . ? N4 N3 Ga1 113.0(4) . . ? N4 N3 Ga2 117.8(4) . . ? Ga1 N3 Ga2 92.1(2) . . ? N4 N3 H3N 108(6) . . ? Ga1 N3 H3N 107(6) . . ? Ga2 N3 H3N 119(6) . . ? N3 N4 C3 108.4(6) . . ? N3 N4 C4 109.5(5) . . ? C3 N4 C4 109.9(5) . . ? N2 C1 H1A 109.5 . . ? N2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N2 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N4 C3 H3A 109.5 . . ? N4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N4 C4 H4A 109.5 . . ? N4 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N4 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? 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 N3 Ga1 Ga2 N1 176.0(3) . . . . ? N1 Ga1 Ga2 N3 -176.0(3) . . . . ? N3 Ga1 N1 N2 -124.2(4) . . . . ? Ga2 Ga1 N1 N2 -121.4(4) . . . . ? N3 Ga1 N1 Ga2 -2.8(2) . . . . ? N3 Ga2 N1 N2 124.2(4) . . . . ? Ga1 Ga2 N1 N2 121.4(5) . . . . ? N3 Ga2 N1 Ga1 2.8(2) . . . . ? Ga1 N1 N2 C2 176.9(4) . . . . ? Ga2 N1 N2 C2 68.4(5) . . . . ? Ga1 N1 N2 C1 -62.7(5) . . . . ? Ga2 N1 N2 C1 -171.2(4) . . . . ? N1 Ga1 N3 N4 -118.8(4) . . . . ? Ga2 Ga1 N3 N4 -121.5(5) . . . . ? N1 Ga1 N3 Ga2 2.8(2) . . . . ? N1 Ga2 N3 N4 114.7(4) . . . . ? Ga1 Ga2 N3 N4 117.4(5) . . . . ? N1 Ga2 N3 Ga1 -2.7(2) . . . . ? Ga1 N3 N4 C3 -69.4(5) . . . . ? Ga2 N3 N4 C3 -175.0(4) . . . . ? Ga1 N3 N4 C4 170.7(4) . . . . ? Ga2 N3 N4 C4 65.1(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N N2 0.81(5) 2.45(5) 3.238(7) 167(5) 2_575 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.385 _refine_diff_density_min -0.430 _refine_diff_density_rms 0.088 #===END data_99343a _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 99343/BL046 _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20 H68 Ga4 N20' _chemical_formula_weight 867.82 _chemical_melting_point ? _chemical_compound_source 'Bing Luo' 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' 'N' 'N' 0.0061 0.0033 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 9.8972(7) _cell_length_b 22.489(2) _cell_length_c 10.0230(7) _cell_angle_alpha 90.000(1) _cell_angle_beta 112.824(1) _cell_angle_gamma 90.000(1) _cell_volume 2056.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4494 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 2.632 _exptl_absorpt_correction_type 'multi-scans' _exptl_absorpt_correction_T_min 0.7756 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; Absorption correction was carried out using the program SADABS, G. Sheldrick (1999). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Smart CCD, Siemens' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12953 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0500 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4622 _reflns_number_observed 3239 _reflns_observed_criterion 2sigma(I) _computing_data_collection 'Smart, Bruker' _computing_cell_refinement 'Saint, Bruker' _computing_data_reduction 'Saint, Bruker' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0507P)^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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_number_reflns 4622 _refine_ls_number_parameters 209 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_obs 0.0384 _refine_ls_wR_factor_all 0.0957 _refine_ls_wR_factor_obs 0.0887 _refine_ls_goodness_of_fit_all 0.975 _refine_ls_goodness_of_fit_obs 1.089 _refine_ls_restrained_S_all 0.976 _refine_ls_restrained_S_obs 1.090 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ga1 Ga 0.83536(4) 0.06007(2) 0.84505(4) 0.02915(11) Uani 1 d . . Ga2 Ga 1.10966(4) 0.08665(2) 1.09817(4) 0.02878(11) Uani 1 d . . N1 N 1.0405(3) 0.08415(14) 0.8834(3) 0.0376(7) Uani 1 d . . H1N H 1.0344(3) 0.12371(14) 0.8546(3) 0.045 Uiso 1 calc R . N2 N 1.1201(3) 0.0556(2) 0.8128(3) 0.0484(8) Uani 1 d . . N3 N 0.8942(3) 0.07435(13) 1.0601(3) 0.0394(7) Uani 1 d . . H3N H 0.8875(3) 0.03786(13) 1.1008(3) 0.047 Uiso 1 calc R . N4 N 0.8160(3) 0.1162(2) 1.1103(4) 0.0499(8) Uani 1 d . . N5 N 0.7907(3) -0.01938(12) 0.8050(3) 0.0305(6) Uani 1 d . . N6 N 0.6572(3) -0.02378(13) 0.6739(3) 0.0316(6) Uani 1 d . . N7 N 1.1873(3) 0.16200(13) 1.1508(3) 0.0460(8) Uani 1 d . . H7N H 1.2547(3) 0.16905(13) 1.2374(3) 0.055 Uiso 1 calc R . N8 N 1.1347(4) 0.2075(2) 1.0476(4) 0.0718(12) Uani 1 d D . N9 N 0.7059(3) 0.11202(14) 0.7181(4) 0.0597(10) Uani 1 d . . H9N H 0.6208(3) 0.09881(14) 0.6565(4) 0.072 Uiso 1 calc R . N10 N 0.7405(4) 0.17277(15) 0.7176(4) 0.0673(12) Uani 1 d D . C1 C 1.0440(5) 0.0632(2) 0.6540(4) 0.0536(11) Uani 1 d . . H1A H 0.9446(12) 0.0469(12) 0.6222(6) 0.080 Uiso 1 calc R . H1B H 1.0984(17) 0.0422(11) 0.6049(4) 0.080 Uiso 1 calc R . H1C H 1.0386(28) 0.1056(2) 0.6298(5) 0.080 Uiso 1 calc R . C2 C 1.2685(4) 0.0816(2) 0.8568(5) 0.0556(11) Uani 1 d . . H2A H 1.3187(13) 0.0797(12) 0.9624(5) 0.083 Uiso 1 calc R . H2B H 1.2605(4) 0.1232(4) 0.8254(28) 0.083 Uiso 1 calc R . H2C H 1.3246(11) 0.0592(8) 0.8119(26) 0.083 Uiso 1 calc R . C3 C 0.8828(5) 0.1178(2) 1.2674(4) 0.0578(11) Uani 1 d . . H3A H 0.9875(8) 0.1269(13) 1.2988(4) 0.087 Uiso 1 calc R . H3B H 0.8708(27) 0.0791(4) 1.3062(4) 0.087 Uiso 1 calc R . H3C H 0.8353(21) 0.1486(9) 1.3032(4) 0.087 Uiso 1 calc R . C4 C 0.6631(4) 0.0979(2) 1.0610(5) 0.0611(12) Uani 1 d . . H4A H 0.6215(10) 0.0946(13) 0.9552(6) 0.092 Uiso 1 calc R . H4B H 0.6079(8) 0.1276(7) 1.0909(29) 0.092 Uiso 1 calc R . H4C H 0.6569(5) 0.0593(6) 1.1038(26) 0.092 Uiso 1 calc R . C5 C 0.5391(4) -0.0503(2) 0.7049(4) 0.0447(10) Uani 1 d . . H5A H 0.5179(19) -0.0255(6) 0.7748(21) 0.067 Uiso 1 calc R . H5B H 0.5682(11) -0.0901(5) 0.7455(26) 0.067 Uiso 1 calc R . H5C H 0.4513(9) -0.0532(10) 0.6153(6) 0.067 Uiso 1 calc R . C6 C 0.6837(4) -0.0569(2) 0.5625(4) 0.0431(9) Uani 1 d . . H6A H 0.7660(18) -0.0390(7) 0.5457(19) 0.065 Uiso 1 calc R . H6B H 0.5957(10) -0.0558(9) 0.4727(8) 0.065 Uiso 1 calc R . H6C H 0.7072(26) -0.0982(3) 0.5937(12) 0.065 Uiso 1 calc R . C7 C 1.2565(8) 0.2440(3) 1.0525(8) 0.120(2) Uani 1 d D . H7A H 1.3296(27) 0.2191(5) 1.0356(57) 0.179 Uiso 1 calc R . H7B H 1.3010(37) 0.2628(19) 1.1478(21) 0.179 Uiso 1 calc R . H7C H 1.2216(12) 0.2747(15) 0.9775(38) 0.179 Uiso 1 calc R . C8 C 1.0318(7) 0.2440(3) 1.0746(9) 0.135(3) Uani 1 d D . H8A H 0.9458(29) 0.2203(7) 1.0661(65) 0.202 Uiso 1 calc R . H8B H 1.0018(50) 0.2765(16) 1.0039(41) 0.202 Uiso 1 calc R . H8C H 1.0765(22) 0.2606(21) 1.1725(25) 0.202 Uiso 1 calc R . C9 C 0.6526(10) 0.2069(3) 0.7716(8) 0.147(3) Uani 1 d D . H9A H 0.6739(53) 0.1956(21) 0.8721(24) 0.220 Uiso 1 calc R . H9B H 0.5488(10) 0.1995(22) 0.7126(44) 0.220 Uiso 1 calc R . H9C H 0.6741(52) 0.2492(3) 0.7673(67) 0.220 Uiso 1 calc R . C10 C 0.7080(8) 0.1912(3) 0.5719(7) 0.124(3) Uani 1 d D . H10A H 0.7505(49) 0.1628(13) 0.5249(19) 0.187 Uiso 1 calc R . H10B H 0.7498(49) 0.2307(10) 0.5721(8) 0.187 Uiso 1 calc R . H10C H 0.6015(8) 0.1927(22) 0.5188(17) 0.187 Uiso 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 0.0253(2) 0.0283(2) 0.0267(2) 0.00053(15) 0.00230(15) -0.0013(2) Ga2 0.0269(2) 0.0269(2) 0.0259(2) -0.00175(15) 0.00305(15) -0.0034(2) N1 0.033(2) 0.054(2) 0.0248(15) 0.0045(13) 0.0098(12) -0.0109(14) N2 0.041(2) 0.065(2) 0.039(2) -0.009(2) 0.0146(15) -0.004(2) N3 0.032(2) 0.042(2) 0.037(2) -0.0133(13) 0.0057(13) 0.0035(13) N4 0.038(2) 0.066(2) 0.049(2) -0.009(2) 0.021(2) 0.001(2) N5 0.0272(14) 0.030(2) 0.0240(15) -0.0001(11) -0.0013(11) -0.0028(12) N6 0.0232(14) 0.038(2) 0.0244(15) 0.0008(12) -0.0011(11) -0.0033(12) N7 0.048(2) 0.034(2) 0.038(2) 0.0002(13) -0.0043(15) -0.0078(15) N8 0.078(3) 0.033(2) 0.071(3) 0.009(2) -0.007(2) -0.014(2) N9 0.043(2) 0.034(2) 0.065(2) 0.010(2) -0.019(2) -0.002(2) N10 0.063(2) 0.032(2) 0.067(3) 0.009(2) -0.018(2) 0.001(2) C1 0.061(3) 0.074(3) 0.034(2) -0.012(2) 0.027(2) -0.009(2) C2 0.033(2) 0.083(3) 0.055(3) -0.007(2) 0.021(2) -0.007(2) C3 0.065(3) 0.071(3) 0.041(2) -0.012(2) 0.024(2) 0.001(2) C4 0.037(2) 0.085(4) 0.068(3) 0.001(2) 0.029(2) -0.003(2) C5 0.023(2) 0.057(3) 0.049(2) 0.001(2) 0.007(2) -0.003(2) C6 0.044(2) 0.052(2) 0.025(2) -0.003(2) 0.005(2) -0.003(2) C7 0.166(7) 0.067(4) 0.140(6) 0.006(4) 0.075(5) -0.040(4) C8 0.106(5) 0.062(4) 0.224(9) 0.052(5) 0.050(6) 0.022(4) C9 0.259(10) 0.067(4) 0.142(7) 0.003(4) 0.109(7) 0.049(5) C10 0.160(7) 0.081(5) 0.144(7) 0.044(4) 0.072(6) 0.007(5) _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 N9 1.833(3) . ? Ga1 N5 1.847(3) . ? Ga1 N1 1.989(3) . ? Ga1 N3 2.029(3) . ? Ga1 Ga2 2.9699(5) . ? Ga2 N7 1.851(3) . ? Ga2 N5 1.860(3) 3_757 ? Ga2 N1 1.990(3) . ? Ga2 N3 2.034(3) . ? N1 N2 1.402(4) . ? N1 H1N 0.93 . ? N2 C2 1.480(5) . ? N2 C1 1.483(5) . ? N3 N4 1.427(4) . ? N3 H3N 0.93 . ? N4 C3 1.453(5) . ? N4 C4 1.457(5) . ? N5 N6 1.461(3) . ? N5 Ga2 1.860(3) 3_757 ? N6 C6 1.448(4) . ? N6 C5 1.449(4) . ? N7 N8 1.403(4) . ? N7 H7N 0.88 . ? N8 C8 1.413(6) . ? N8 C7 1.442(6) . ? N9 N10 1.409(4) . ? N9 H9N 0.88 . ? N10 C9 1.416(6) . ? N10 C10 1.429(6) . ? C1 H1A 0.98 . ? C1 H1B 0.98 . ? C1 H1C 0.98 . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? 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 N9 Ga1 N5 114.94(13) . . ? N9 Ga1 N1 110.30(14) . . ? N5 Ga1 N1 116.46(13) . . ? N9 Ga1 N3 118.16(15) . . ? N5 Ga1 N3 109.27(12) . . ? N1 Ga1 N3 84.30(11) . . ? N9 Ga1 Ga2 128.75(10) . . ? N5 Ga1 Ga2 116.28(8) . . ? N1 Ga1 Ga2 41.75(8) . . ? N3 Ga1 Ga2 43.10(8) . . ? N7 Ga2 N5 121.23(12) . 3_757 ? N7 Ga2 N1 105.34(13) . . ? N5 Ga2 N1 115.56(12) 3_757 . ? N7 Ga2 N3 117.83(13) . . ? N5 Ga2 N3 107.00(12) 3_757 . ? N1 Ga2 N3 84.13(11) . . ? N7 Ga2 Ga1 124.64(9) . . ? N5 Ga2 Ga1 113.95(8) 3_757 . ? N1 Ga2 Ga1 41.72(8) . . ? N3 Ga2 Ga1 42.96(8) . . ? N2 N1 Ga1 120.6(2) . . ? N2 N1 Ga2 122.3(2) . . ? Ga1 N1 Ga2 96.53(12) . . ? N2 N1 H1N 105.2(2) . . ? Ga1 N1 H1N 105.19(9) . . ? Ga2 N1 H1N 105.19(9) . . ? N1 N2 C2 110.8(3) . . ? N1 N2 C1 109.8(3) . . ? C2 N2 C1 107.9(3) . . ? N4 N3 Ga1 120.5(2) . . ? N4 N3 Ga2 121.1(2) . . ? Ga1 N3 Ga2 93.94(12) . . ? N4 N3 H3N 106.6(2) . . ? Ga1 N3 H3N 106.61(9) . . ? Ga2 N3 H3N 106.61(9) . . ? N3 N4 C3 108.5(3) . . ? N3 N4 C4 109.2(3) . . ? C3 N4 C4 110.5(3) . . ? N6 N5 Ga1 108.5(2) . . ? N6 N5 Ga2 121.7(2) . 3_757 ? Ga1 N5 Ga2 129.76(14) . 3_757 ? C6 N6 C5 110.9(3) . . ? C6 N6 N5 110.9(3) . . ? C5 N6 N5 111.0(3) . . ? N8 N7 Ga2 117.6(2) . . ? N8 N7 H7N 121.2(2) . . ? Ga2 N7 H7N 121.19(9) . . ? N7 N8 C8 111.8(4) . . ? N7 N8 C7 108.9(4) . . ? C8 N8 C7 108.5(4) . . ? N10 N9 Ga1 121.0(2) . . ? N10 N9 H9N 119.5(2) . . ? Ga1 N9 H9N 119.51(10) . . ? N9 N10 C9 109.7(4) . . ? N9 N10 C10 109.0(4) . . ? C9 N10 C10 107.8(5) . . ? N2 C1 H1A 109.5(2) . . ? N2 C1 H1B 109.5(2) . . ? H1A C1 H1B 109.5 . . ? N2 C1 H1C 109.5(2) . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N2 C2 H2A 109.5(2) . . ? N2 C2 H2B 109.5(2) . . ? H2A C2 H2B 109.5 . . ? N2 C2 H2C 109.5(2) . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N4 C3 H3A 109.5(2) . . ? N4 C3 H3B 109.5(2) . . ? H3A C3 H3B 109.5 . . ? N4 C3 H3C 109.5(2) . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N4 C4 H4A 109.5(2) . . ? N4 C4 H4B 109.5(2) . . ? H4A C4 H4B 109.5 . . ? N4 C4 H4C 109.5(2) . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N6 C5 H5A 109.5(2) . . ? N6 C5 H5B 109.5(2) . . ? H5A C5 H5B 109.5 . . ? N6 C5 H5C 109.5(2) . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N6 C6 H6A 109.5(2) . . ? N6 C6 H6B 109.5(2) . . ? H6A C6 H6B 109.5 . . ? N6 C6 H6C 109.5(2) . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N8 C7 H7A 109.5(3) . . ? N8 C7 H7B 109.5(3) . . ? H7A C7 H7B 109.5 . . ? N8 C7 H7C 109.5(3) . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N8 C8 H8A 109.5(3) . . ? N8 C8 H8B 109.5(3) . . ? H8A C8 H8B 109.5 . . ? N8 C8 H8C 109.5(4) . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N10 C9 H9A 109.5(3) . . ? N10 C9 H9B 109.5(4) . . ? H9A C9 H9B 109.5 . . ? N10 C9 H9C 109.5(3) . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N10 C10 H10A 109.5(3) . . ? N10 C10 H10B 109.5(3) . . ? H10A C10 H10B 109.5 . . ? N10 C10 H10C 109.5(3) . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? 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 N9 Ga1 Ga2 N7 -3.6(2) . . . . ? N5 Ga1 Ga2 N7 174.2(2) . . . . ? N1 Ga1 Ga2 N7 73.0(2) . . . . ? N3 Ga1 Ga2 N7 -95.2(2) . . . . ? N9 Ga1 Ga2 N5 -178.8(2) . . . 3_757 ? N5 Ga1 Ga2 N5 -1.1(2) . . . 3_757 ? N1 Ga1 Ga2 N5 -102.2(2) . . . 3_757 ? N3 Ga1 Ga2 N5 89.6(2) . . . 3_757 ? N9 Ga1 Ga2 N1 -76.6(2) . . . . ? N5 Ga1 Ga2 N1 101.1(2) . . . . ? N1 Ga1 Ga2 N1 0.0 . . . . ? N3 Ga1 Ga2 N1 -168.2(2) . . . . ? N9 Ga1 Ga2 N3 91.6(2) . . . . ? N5 Ga1 Ga2 N3 -90.6(2) . . . . ? N1 Ga1 Ga2 N3 168.2(2) . . . . ? N3 Ga1 Ga2 N3 0.0 . . . . ? N9 Ga1 N1 N2 -100.2(3) . . . . ? N5 Ga1 N1 N2 33.2(3) . . . . ? N3 Ga1 N1 N2 141.9(3) . . . . ? Ga2 Ga1 N1 N2 133.8(3) . . . . ? N9 Ga1 N1 Ga2 126.0(2) . . . . ? N5 Ga1 N1 Ga2 -100.66(14) . . . . ? N3 Ga1 N1 Ga2 8.04(13) . . . . ? Ga2 Ga1 N1 Ga2 0.0 . . . . ? N7 Ga2 N1 N2 101.9(3) . . . . ? N5 Ga2 N1 N2 -34.7(3) 3_757 . . . ? N3 Ga2 N1 N2 -140.8(3) . . . . ? Ga1 Ga2 N1 N2 -132.8(3) . . . . ? N7 Ga2 N1 Ga1 -125.31(14) . . . . ? N5 Ga2 N1 Ga1 98.04(14) 3_757 . . . ? N3 Ga2 N1 Ga1 -8.02(13) . . . . ? Ga1 Ga2 N1 Ga1 0.0 . . . . ? Ga1 N1 N2 C2 179.2(2) . . . . ? Ga2 N1 N2 C2 -58.8(4) . . . . ? Ga1 N1 N2 C1 60.1(4) . . . . ? Ga2 N1 N2 C1 -177.9(2) . . . . ? N9 Ga1 N3 N4 12.1(3) . . . . ? N5 Ga1 N3 N4 -121.9(3) . . . . ? N1 Ga1 N3 N4 122.1(3) . . . . ? Ga2 Ga1 N3 N4 129.9(3) . . . . ? N9 Ga1 N3 Ga2 -117.84(14) . . . . ? N5 Ga1 N3 Ga2 108.23(13) . . . . ? N1 Ga1 N3 Ga2 -7.84(13) . . . . ? Ga2 Ga1 N3 Ga2 0.0 . . . . ? N7 Ga2 N3 N4 -17.3(3) . . . . ? N5 Ga2 N3 N4 123.4(3) 3_757 . . . ? N1 Ga2 N3 N4 -121.6(3) . . . . ? Ga1 Ga2 N3 N4 -129.5(3) . . . . ? N7 Ga2 N3 Ga1 112.10(13) . . . . ? N5 Ga2 N3 Ga1 -107.14(13) 3_757 . . . ? N1 Ga2 N3 Ga1 7.84(13) . . . . ? Ga1 Ga2 N3 Ga1 0.0 . . . . ? Ga1 N3 N4 C3 -179.2(3) . . . . ? Ga2 N3 N4 C3 -62.6(4) . . . . ? Ga1 N3 N4 C4 60.2(4) . . . . ? Ga2 N3 N4 C4 176.9(3) . . . . ? N9 Ga1 N5 N6 0.8(3) . . . . ? N1 Ga1 N5 N6 -130.4(2) . . . . ? N3 Ga1 N5 N6 136.4(2) . . . . ? Ga2 Ga1 N5 N6 -177.2(2) . . . . ? N9 Ga1 N5 Ga2 179.3(2) . . . 3_757 ? N1 Ga1 N5 Ga2 48.1(2) . . . 3_757 ? N3 Ga1 N5 Ga2 -45.1(2) . . . 3_757 ? Ga2 Ga1 N5 Ga2 1.3(2) . . . 3_757 ? Ga1 N5 N6 C6 120.7(3) . . . . ? Ga2 N5 N6 C6 -58.0(3) 3_757 . . . ? Ga1 N5 N6 C5 -115.6(3) . . . . ? Ga2 N5 N6 C5 65.8(3) 3_757 . . . ? N5 Ga2 N7 N8 158.9(3) 3_757 . . . ? N1 Ga2 N7 N8 25.3(3) . . . . ? N3 Ga2 N7 N8 -66.1(3) . . . . ? Ga1 Ga2 N7 N8 -16.0(4) . . . . ? Ga2 N7 N8 C8 101.5(4) . . . . ? Ga2 N7 N8 C7 -138.6(4) . . . . ? N5 Ga1 N9 N10 -167.2(3) . . . . ? N1 Ga1 N9 N10 -33.1(4) . . . . ? N3 Ga1 N9 N10 61.3(4) . . . . ? Ga2 Ga1 N9 N10 10.5(4) . . . . ? Ga1 N9 N10 C9 -109.9(5) . . . . ? Ga1 N9 N10 C10 132.3(4) . . . . ? _refine_diff_density_max 1.055 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.083