Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Jones, Cameron' 'Baker, Robert J.' 'Farley, Robert D.' 'Kloth, Marc' 'Murphy, Damien M.' _publ_contact_author_name 'Dr Cameron Jones' _publ_contact_author_address ; Department of Chemistry Cardiff University PO Box 912 Park Place Cardiff CF10 3TB UK ; _publ_contact_author_email 'JONESCA6@CARDIFF.AC.UK' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; The Reactivity of Diazabutadiences Toward Low Oxidation State Group 13 Iodides and the Synthesis of a new Gallium(I) Carbene Analogue ; data_compound9 _database_code_CSD 189504 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H36 Al I2 N2' _chemical_formula_weight 657.35 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' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 12.564(3) _cell_length_b 21.284(4) _cell_length_c 10.412(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2784.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1300 _exptl_absorpt_coefficient_mu 2.306 _exptl_absorpt_correction_type 'Sortav (Blessing)' _exptl_absorpt_correction_T_min 0.60 _exptl_absorpt_correction_T_max 0.72 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 Kappa CCD' _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 47890 _diffrn_reflns_av_R_equivalents 0.0803 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3273 _reflns_number_gt 2797 _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^)+(0.0299P)^2^+1.7133P] 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 3273 _refine_ls_number_parameters 149 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0643 _refine_ls_wR_factor_gt 0.0606 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 I1 I -0.366467(18) 0.2500 0.07385(2) 0.02743(8) Uani 1 2 d S . . I2 I -0.198339(18) 0.2500 0.41558(2) 0.02770(8) Uani 1 2 d S . . Al1 Al -0.18558(8) 0.2500 0.17290(10) 0.0191(2) Uani 1 2 d S . . N1 N -0.08916(15) 0.31133(9) 0.11240(18) 0.0181(4) Uani 1 1 d . . . C1 C 0.0017(2) 0.28309(12) 0.0787(2) 0.0202(5) Uani 1 1 d . . . H1 H 0.0620 0.3060 0.0564 0.024 Uiso 1 1 calc R . . C2 C -0.10389(19) 0.37770(11) 0.0892(2) 0.0190(5) Uani 1 1 d . . . C3 C -0.14616(19) 0.39613(11) -0.0305(2) 0.0209(5) Uani 1 1 d . . . C4 C -0.1650(2) 0.45978(13) -0.0499(2) 0.0266(6) Uani 1 1 d . . . H4 H -0.1934 0.4732 -0.1278 0.032 Uiso 1 1 calc R . . C5 C -0.1424(2) 0.50369(12) 0.0445(3) 0.0291(6) Uani 1 1 d . . . H5 H -0.1566 0.5460 0.0302 0.035 Uiso 1 1 calc R . . C6 C -0.0989(2) 0.48468(12) 0.1591(3) 0.0272(6) Uani 1 1 d . . . H6 H -0.0827 0.5147 0.2209 0.033 Uiso 1 1 calc R . . C7 C -0.07846(19) 0.42156(11) 0.1853(2) 0.0207(5) Uani 1 1 d . . . C8 C -0.1636(2) 0.34886(13) -0.1384(2) 0.0268(6) Uani 1 1 d . . . H8 H -0.1720 0.3073 -0.0993 0.032 Uiso 1 1 calc R . . C9 C -0.2634(3) 0.36241(16) -0.2171(3) 0.0426(7) Uani 1 1 d . . . H9A H -0.3235 0.3660 -0.1608 0.064 Uiso 1 1 calc R . . H9B H -0.2751 0.3287 -0.2768 0.064 Uiso 1 1 calc R . . H9C H -0.2542 0.4011 -0.2634 0.064 Uiso 1 1 calc R . . C10 C -0.0650(3) 0.34670(15) -0.2255(3) 0.0391(7) Uani 1 1 d . . . H10A H -0.0539 0.3873 -0.2634 0.059 Uiso 1 1 calc R . . H10B H -0.0758 0.3162 -0.2921 0.059 Uiso 1 1 calc R . . H10C H -0.0038 0.3353 -0.1755 0.059 Uiso 1 1 calc R . . C11 C -0.0266(2) 0.40265(13) 0.3109(2) 0.0267(6) Uani 1 1 d . . . H11 H -0.0257 0.3566 0.3150 0.032 Uiso 1 1 calc R . . C12 C -0.0892(3) 0.42685(15) 0.4271(2) 0.0437(8) Uani 1 1 d . . . H12A H -0.0877 0.4719 0.4279 0.066 Uiso 1 1 calc R . . H12B H -0.0574 0.4111 0.5046 0.066 Uiso 1 1 calc R . . H12C H -0.1615 0.4126 0.4216 0.066 Uiso 1 1 calc R . . C13 C 0.0886(2) 0.42565(15) 0.3155(3) 0.0413(8) Uani 1 1 d . . . H13A H 0.1274 0.4083 0.2444 0.062 Uiso 1 1 calc R . . H13B H 0.1209 0.4124 0.3946 0.062 Uiso 1 1 calc R . . H13C H 0.0898 0.4707 0.3104 0.062 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 I1 0.01554(12) 0.03259(15) 0.03416(15) 0.000 -0.00039(9) 0.000 I2 0.02070(13) 0.04092(16) 0.02148(13) 0.000 0.00395(9) 0.000 Al1 0.0156(5) 0.0201(5) 0.0216(5) 0.000 0.0023(4) 0.000 N1 0.0182(10) 0.0193(10) 0.0167(9) 0.0001(8) -0.0004(8) -0.0004(8) C1 0.0139(11) 0.0250(13) 0.0217(12) 0.0017(10) 0.0002(9) -0.0025(10) C2 0.0165(11) 0.0171(12) 0.0235(12) 0.0023(9) 0.0026(9) 0.0007(9) C3 0.0186(12) 0.0246(13) 0.0196(12) 0.0042(10) 0.0023(9) 0.0000(10) C4 0.0260(13) 0.0284(14) 0.0255(13) 0.0072(11) -0.0013(11) 0.0031(11) C5 0.0330(15) 0.0196(13) 0.0347(14) 0.0046(11) 0.0007(11) 0.0063(11) C6 0.0292(14) 0.0215(13) 0.0310(14) -0.0032(11) -0.0016(11) 0.0008(11) C7 0.0194(12) 0.0197(12) 0.0230(12) -0.0006(9) -0.0001(10) -0.0010(10) C8 0.0328(14) 0.0272(14) 0.0206(12) 0.0012(10) -0.0045(11) -0.0030(11) C9 0.0448(18) 0.0441(18) 0.0389(16) -0.0025(14) -0.0167(14) 0.0044(15) C10 0.0466(18) 0.0462(18) 0.0244(14) -0.0039(13) 0.0046(13) -0.0022(15) C11 0.0341(15) 0.0236(13) 0.0225(13) -0.0012(10) -0.0046(10) -0.0023(11) C12 0.070(2) 0.0366(17) 0.0244(15) -0.0018(12) 0.0028(14) 0.0041(16) C13 0.0410(18) 0.0388(18) 0.0440(17) 0.0085(13) -0.0208(14) -0.0093(14) _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 I1 Al1 2.4957(11) . ? I2 Al1 2.5318(11) . ? Al1 N1 1.889(2) . ? Al1 N1 1.889(2) 8_565 ? N1 C1 1.337(3) . ? N1 C2 1.445(3) . ? C1 C1 1.409(5) 8_565 ? C2 C7 1.405(3) . ? C2 C3 1.411(3) . ? C3 C4 1.390(4) . ? C3 C8 1.524(3) . ? C4 C5 1.386(4) . ? C5 C6 1.373(4) . ? C6 C7 1.395(3) . ? C7 C11 1.516(3) . ? C8 C9 1.525(4) . ? C8 C10 1.536(4) . ? C11 C13 1.529(4) . ? C11 C12 1.532(4) . ? 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 Al1 N1 87.42(13) . 8_565 ? N1 Al1 I1 116.50(7) . . ? N1 Al1 I1 116.50(7) 8_565 . ? N1 Al1 I2 111.93(7) . . ? N1 Al1 I2 111.93(7) 8_565 . ? I1 Al1 I2 110.78(4) . . ? C1 N1 C2 120.3(2) . . ? C1 N1 Al1 108.93(17) . . ? C2 N1 Al1 130.47(16) . . ? N1 C1 C1 116.71(14) . 8_565 ? C7 C2 C3 122.0(2) . . ? C7 C2 N1 120.1(2) . . ? C3 C2 N1 117.9(2) . . ? C4 C3 C2 117.6(2) . . ? C4 C3 C8 120.8(2) . . ? C2 C3 C8 121.5(2) . . ? C5 C4 C3 121.2(2) . . ? C6 C5 C4 120.0(2) . . ? C5 C6 C7 121.8(2) . . ? C6 C7 C2 117.3(2) . . ? C6 C7 C11 120.2(2) . . ? C2 C7 C11 122.4(2) . . ? C3 C8 C9 112.9(2) . . ? C3 C8 C10 109.8(2) . . ? C9 C8 C10 110.6(2) . . ? C7 C11 C13 110.4(2) . . ? C7 C11 C12 111.8(2) . . ? C13 C11 C12 110.7(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.929 _refine_diff_density_min -0.755 _refine_diff_density_rms 0.101 data_compound8 _database_code_CSD 189505 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H20 Ga I2 N2' _chemical_formula_weight 491.80 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' 'I' 'I' -0.4742 1.8119 '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)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.6790(15) _cell_length_b 10.583(2) _cell_length_c 10.653(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.95(3) _cell_angle_gamma 90.00 _cell_volume 823.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.983 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 462 _exptl_absorpt_coefficient_mu 5.397 _exptl_absorpt_correction_type 'Sortav (Blessing)' _exptl_absorpt_correction_T_min 0.06 _exptl_absorpt_correction_T_max 0.15 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 Kappa CCD' _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 12390 _diffrn_reflns_av_R_equivalents 0.0753 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 27.46 _reflns_number_total 1973 _reflns_number_gt 1805 _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^)+(0.0666P)^2^+2.6855P] 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 SHELXL _refine_ls_extinction_coef 0.0082(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1973 _refine_ls_number_parameters 87 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1281 _refine_ls_wR_factor_gt 0.1252 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 0.000 _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 I1 I 0.20273(6) 0.55489(4) 0.21425(4) 0.0532(2) Uani 1 1 d . . . Ga1 Ga 0.36931(10) 0.7500 0.17485(8) 0.0339(2) Uani 1 2 d S . . N1 N 0.6321(8) 0.7500 0.2725(6) 0.0369(13) Uani 1 2 d S . . N2 N 0.4375(8) 0.7500 0.0183(6) 0.0366(13) Uani 1 2 d S . . C1 C 0.7239(10) 0.7500 0.1866(8) 0.0448(18) Uani 1 2 d S . . H1 H 0.8512 0.7500 0.2148 0.054 Uiso 1 2 calc SR . . C2 C 0.6224(11) 0.7500 0.0471(7) 0.0455(19) Uani 1 2 d S . . H2 H 0.6800 0.7500 -0.0180 0.055 Uiso 1 2 calc SR . . C3 C 0.7288(11) 0.7500 0.4177(7) 0.0430(17) Uani 1 2 d S . . C4 C 0.5930(17) 0.7500 0.4924(12) 0.074(3) Uani 1 2 d SU . . H4A H 0.6549 0.7338 0.5840 0.110 Uiso 0.50 1 calc PR . . H4B H 0.5032 0.6854 0.4579 0.110 Uiso 0.50 1 calc PR . . H4C H 0.5337 0.8308 0.4833 0.110 Uiso 0.50 1 calc PR . . C5 C 0.8457(13) 0.8674(9) 0.4539(8) 0.079(2) Uani 1 1 d U . . H5A H 0.9383 0.8659 0.4106 0.118 Uiso 1 1 calc R . . H5B H 0.9027 0.8699 0.5477 0.118 Uiso 1 1 calc R . . H5C H 0.7702 0.9409 0.4265 0.118 Uiso 1 1 calc R . . C6 C 0.3182(11) 0.7500 -0.1205(7) 0.052(2) Uani 1 2 d SD . . C7 C 0.1201(14) 0.7500 -0.1266(12) 0.070(3) Uani 1 2 d SDU . . H7A H 0.0474 0.7154 -0.2095 0.106 Uiso 0.50 1 calc PR . . H7B H 0.0815 0.8350 -0.1183 0.106 Uiso 0.50 1 calc PR . . H7C H 0.1048 0.6996 -0.0558 0.106 Uiso 0.50 1 calc PR . . C8 C 0.348(3) 0.8707(13) -0.185(2) 0.180(8) Uani 1 1 d DU . . H8A H 0.3291 0.9413 -0.1338 0.271 Uiso 1 1 calc R . . H8B H 0.2639 0.8753 -0.2723 0.271 Uiso 1 1 calc R . . H8C H 0.4714 0.8728 -0.1888 0.271 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 I1 0.0507(3) 0.0449(3) 0.0715(4) 0.00730(17) 0.0300(2) -0.00863(15) Ga1 0.0249(4) 0.0360(4) 0.0422(4) 0.000 0.0126(3) 0.000 N1 0.028(3) 0.048(4) 0.034(3) 0.000 0.009(2) 0.000 N2 0.032(3) 0.048(4) 0.028(3) 0.000 0.006(2) 0.000 C1 0.027(3) 0.067(5) 0.039(4) 0.000 0.009(3) 0.000 C2 0.039(4) 0.070(6) 0.030(3) 0.000 0.013(3) 0.000 C3 0.037(4) 0.059(5) 0.030(3) 0.000 0.007(3) 0.000 C4 0.072(5) 0.091(5) 0.062(4) 0.000 0.027(4) 0.000 C5 0.090(4) 0.082(4) 0.060(3) -0.007(3) 0.019(3) -0.018(4) C6 0.042(4) 0.083(7) 0.026(3) 0.000 0.006(3) 0.000 C7 0.062(4) 0.081(5) 0.062(4) 0.000 0.009(3) 0.000 C8 0.179(8) 0.181(8) 0.176(8) 0.014(4) 0.046(4) -0.010(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 I1 Ga1 2.5312(7) . ? Ga1 N2 1.896(6) . ? Ga1 N1 1.965(6) . ? Ga1 I1 2.5312(7) 4_575 ? N1 C1 1.316(10) . ? N1 C3 1.495(9) . ? N2 C2 1.357(10) . ? N2 C6 1.479(9) . ? C1 C2 1.450(11) . ? C3 C4 1.495(14) . ? C3 C5 1.511(10) . ? C3 C5 1.511(10) 4_575 ? C6 C8 1.500(13) 4_575 ? C6 C8 1.500(13) . ? C6 C7 1.503(12) . ? 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 N2 Ga1 N1 87.1(3) . . ? N2 Ga1 I1 115.89(8) . . ? N1 Ga1 I1 113.66(9) . . ? N2 Ga1 I1 115.89(8) . 4_575 ? N1 Ga1 I1 113.66(9) . 4_575 ? I1 Ga1 I1 109.33(4) . 4_575 ? C1 N1 C3 121.1(6) . . ? C1 N1 Ga1 108.3(5) . . ? C3 N1 Ga1 130.5(5) . . ? C2 N2 C6 120.6(6) . . ? C2 N2 Ga1 110.8(5) . . ? C6 N2 Ga1 128.7(5) . . ? N1 C1 C2 118.6(7) . . ? N2 C2 C1 115.2(7) . . ? C4 C3 N1 110.2(7) . . ? C4 C3 C5 108.7(5) . . ? N1 C3 C5 109.3(5) . . ? C4 C3 C5 108.7(5) . 4_575 ? N1 C3 C5 109.3(5) . 4_575 ? C5 C3 C5 110.6(9) . 4_575 ? N2 C6 C8 108.7(9) . 4_575 ? N2 C6 C8 108.7(9) . . ? C8 C6 C8 116.8(15) 4_575 . ? N2 C6 C7 110.5(7) . . ? C8 C6 C7 106.1(9) 4_575 . ? C8 C6 C7 106.1(9) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.793 (near I1) _refine_diff_density_min -0.825 _refine_diff_density_rms 0.163 data_compound7 _database_code_CSD 189506 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H40 Ga2 I2 N4' _chemical_formula_weight 729.80 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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x+1/2, z+1/4' '-x, -y, z+1/2' 'y+1/2, -x+1/2, z+3/4' 'x+1/2, -y+1/2, -z+3/4' '-x+1/2, y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 10.7330(15) _cell_length_b 10.7330(15) _cell_length_c 24.880(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2866.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 4.046 _exptl_absorpt_correction_type 'Sortav (Blessing)' _exptl_absorpt_correction_T_min 0.31 _exptl_absorpt_correction_T_max 0.46 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 Kappa CCD' _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 34327 _diffrn_reflns_av_R_equivalents 0.0626 _diffrn_reflns_av_sigmaI/netI 0.0221 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.51 _reflns_number_total 3280 _reflns_number_gt 3158 _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^)+(0.0125P)^2^+5.1519P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_number_reflns 3280 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0239 _refine_ls_wR_factor_ref 0.0524 _refine_ls_wR_factor_gt 0.0517 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 I1 I 0.53317(3) 0.21468(2) 0.049790(10) 0.03412(7) Uani 1 1 d . . . Ga1 Ga 0.54146(3) 0.45759(3) 0.041437(12) 0.01905(8) Uani 1 1 d . . . N1 N 0.7114(3) 0.5101(3) 0.06042(11) 0.0283(7) Uani 1 1 d . . . N2 N 0.4967(2) 0.5151(3) 0.11359(10) 0.0229(6) Uani 1 1 d . . . C1 C 0.7121(4) 0.5480(4) 0.11099(15) 0.0380(9) Uani 1 1 d . . . H1 H 0.7860 0.5726 0.1274 0.046 Uiso 1 1 calc R . . C2 C 0.5999(4) 0.5505(4) 0.13926(15) 0.0368(9) Uani 1 1 d . . . H2 H 0.5971 0.5760 0.1750 0.044 Uiso 1 1 calc R . . C3 C 0.8295(3) 0.5051(4) 0.02945(14) 0.0299(8) Uani 1 1 d . . . C6 C 0.7982(4) 0.4751(5) -0.02907(15) 0.0454(11) Uani 1 1 d . . . H6A H 0.7516 0.3989 -0.0307 0.068 Uiso 1 1 calc R . . H6B H 0.8740 0.4660 -0.0492 0.068 Uiso 1 1 calc R . . H6C H 0.7496 0.5416 -0.0441 0.068 Uiso 1 1 calc R . . C7 C 0.3768(3) 0.5112(4) 0.14319(14) 0.0276(8) Uani 1 1 d . . . C10 C 0.2746(3) 0.4856(4) 0.10253(15) 0.0380(9) Uani 1 1 d . . . H10A H 0.2715 0.5523 0.0769 0.057 Uiso 1 1 calc R . . H10B H 0.1960 0.4796 0.1207 0.057 Uiso 1 1 calc R . . H10C H 0.2917 0.4087 0.0843 0.057 Uiso 1 1 calc R . . C8 C 0.3526(4) 0.6363(4) 0.17029(17) 0.0418(10) Uani 1 1 d . . . H8A H 0.4134 0.6496 0.1980 0.063 Uiso 1 1 calc R . . H8B H 0.2707 0.6363 0.1858 0.063 Uiso 1 1 calc R . . H8C H 0.3586 0.7018 0.1441 0.063 Uiso 1 1 calc R . . C5 C 0.8954(4) 0.6303(4) 0.0316(2) 0.0475(11) Uani 1 1 d . . . H5A H 0.8421 0.6934 0.0168 0.071 Uiso 1 1 calc R . . H5B H 0.9711 0.6261 0.0112 0.071 Uiso 1 1 calc R . . H5C H 0.9146 0.6505 0.0683 0.071 Uiso 1 1 calc R . . C9 C 0.3823(4) 0.4061(4) 0.18427(16) 0.0419(10) Uani 1 1 d . . . H9A H 0.3921 0.3280 0.1660 0.063 Uiso 1 1 calc R . . H9B H 0.3065 0.4050 0.2048 0.063 Uiso 1 1 calc R . . H9C H 0.4517 0.4192 0.2079 0.063 Uiso 1 1 calc R . . C4 C 0.9126(4) 0.4040(5) 0.0528(2) 0.0497(11) Uani 1 1 d . . . H4A H 0.9345 0.4253 0.0891 0.074 Uiso 1 1 calc R . . H4B H 0.9869 0.3968 0.0315 0.074 Uiso 1 1 calc R . . H4C H 0.8688 0.3260 0.0526 0.074 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 I1 0.05103(16) 0.01995(11) 0.03138(11) 0.00142(9) -0.00955(12) 0.00474(11) Ga1 0.01875(16) 0.02019(16) 0.01822(15) -0.00191(14) -0.00127(13) 0.00055(14) N1 0.0182(13) 0.0409(18) 0.0258(14) -0.0080(12) -0.0018(11) -0.0023(12) N2 0.0219(14) 0.0260(14) 0.0208(12) -0.0058(11) 0.0036(10) -0.0001(11) C1 0.0247(17) 0.056(3) 0.0332(19) -0.0168(19) -0.0018(15) -0.0066(19) C2 0.033(2) 0.048(2) 0.0288(18) -0.0135(18) -0.0002(15) -0.0085(19) C3 0.0185(15) 0.041(2) 0.0298(17) -0.0079(15) 0.0012(14) 0.0000(14) C6 0.030(2) 0.071(3) 0.0350(19) -0.015(2) 0.0076(16) 0.004(2) C7 0.0248(16) 0.037(2) 0.0213(16) 0.0007(14) 0.0050(13) -0.0011(15) C10 0.0270(18) 0.055(3) 0.0323(18) -0.0007(18) 0.0056(16) -0.0003(18) C8 0.037(2) 0.048(3) 0.040(2) -0.0095(19) 0.0120(18) 0.0081(19) C5 0.036(2) 0.047(3) 0.059(3) -0.006(2) 0.013(2) -0.0090(19) C9 0.045(2) 0.047(3) 0.033(2) 0.0121(18) 0.0065(18) -0.003(2) C4 0.032(2) 0.064(3) 0.053(3) 0.009(3) 0.005(2) 0.0159(19) _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 I1 Ga1 2.6169(5) . ? Ga1 N2 1.958(3) . ? Ga1 N1 1.966(3) . ? Ga1 Ga1 2.4232(7) 7 ? N1 C1 1.322(4) . ? N1 C3 1.485(4) . ? N2 C2 1.333(4) . ? N2 C7 1.483(4) . ? C1 C2 1.395(5) . ? C3 C4 1.519(5) . ? C3 C5 1.520(5) . ? C3 C6 1.529(5) . ? C7 C10 1.518(5) . ? C7 C9 1.523(5) . ? C7 C8 1.524(5) . ? 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 N2 Ga1 N1 85.23(11) . . ? N2 Ga1 Ga1 124.87(8) . 7 ? N1 Ga1 Ga1 116.26(9) . 7 ? N2 Ga1 I1 103.47(8) . . ? N1 Ga1 I1 107.33(9) . . ? Ga1 Ga1 I1 115.153(14) 7 . ? C1 N1 C3 120.0(3) . . ? C1 N1 Ga1 108.8(2) . . ? C3 N1 Ga1 131.1(2) . . ? C2 N2 C7 119.4(3) . . ? C2 N2 Ga1 109.0(2) . . ? C7 N2 Ga1 131.2(2) . . ? N1 C1 C2 118.7(3) . . ? N2 C2 C1 118.0(3) . . ? N1 C3 C4 109.2(3) . . ? N1 C3 C5 110.3(3) . . ? C4 C3 C5 110.2(4) . . ? N1 C3 C6 108.3(3) . . ? C4 C3 C6 110.1(4) . . ? C5 C3 C6 108.8(4) . . ? N2 C7 C10 107.5(3) . . ? N2 C7 C9 108.7(3) . . ? C10 C7 C9 109.9(3) . . ? N2 C7 C8 110.0(3) . . ? C10 C7 C8 109.3(3) . . ? C9 C7 C8 111.2(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.880 _refine_diff_density_min -0.676 _refine_diff_density_rms 0.075 data_compound13 _database_code_CSD 189507 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H144 Ga2 K2 N4 O18' _chemical_formula_weight 1763.72 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 '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 20.844(4) _cell_length_b 26.080(5) _cell_length_c 17.719(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.70(3) _cell_angle_gamma 90.00 _cell_volume 9317(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3776 _exptl_absorpt_coefficient_mu 0.733 _exptl_absorpt_correction_type 'Sortav (Blessing 1995)' _exptl_absorpt_correction_T_min 0.8101 _exptl_absorpt_correction_T_max 0.9303 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 Kappa CCD' _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 137685 _diffrn_reflns_av_R_equivalents 0.0964 _diffrn_reflns_av_sigmaI/netI 0.0698 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.51 _reflns_number_total 21191 _reflns_number_gt 14543 _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 atom C2a refined using ISOR command of Shelx97 ; 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^)+(0.0369P)^2^+18.0496P] 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 21191 _refine_ls_number_parameters 1197 _refine_ls_number_restraints 92 _refine_ls_R_factor_all 0.1111 _refine_ls_R_factor_gt 0.0690 _refine_ls_wR_factor_ref 0.1565 _refine_ls_wR_factor_gt 0.1418 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.088 _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 Ga1 Ga 0.30790(3) 0.64826(2) 0.22587(3) 0.02633(18) Uani 0.8150(19) 1 d PD A 1 Ga1A Ga 0.3301(2) 0.71885(14) 0.3538(2) 0.0304(11) Uani 0.1850(19) 1 d PD A 2 Ga2 Ga 0.18566(3) 1.35660(2) 0.78550(3) 0.02526(17) Uani 0.7997(17) 1 d PD B 4 Ga2A Ga 0.17402(15) 1.28487(11) 0.66197(17) 0.0257(8) Uani 0.2003(17) 1 d PD B 3 K1 K 0.11534(4) 0.89617(3) 0.38833(4) 0.02821(17) Uani 1 1 d . . . K2 K 0.38726(4) 1.11839(3) 0.64114(4) 0.02750(17) Uani 1 1 d . . . O1 O 0.22061(13) 0.82329(9) 0.44157(15) 0.0351(6) Uani 1 1 d . . . O2 O 0.09296(13) 0.79744(9) 0.44869(15) 0.0355(6) Uani 1 1 d . . . O3 O -0.00751(12) 0.84655(10) 0.33677(15) 0.0348(6) Uani 1 1 d . . . O4 O 0.00913(13) 0.93750(10) 0.25895(14) 0.0363(6) Uani 1 1 d . . . O5 O 0.14247(13) 0.96004(9) 0.26901(15) 0.0367(6) Uani 1 1 d . . . O6 O 0.24814(12) 0.91903(9) 0.38426(14) 0.0331(6) Uani 1 1 d . . . O7 O 0.4130(2) 1.05127(14) 0.7676(2) 0.0354(9) Uani 0.70 1 d P . . O8 O 0.28395(19) 1.06807(15) 0.6796(2) 0.0308(8) Uani 0.70 1 d P . . O9 O 0.2613(2) 1.16397(15) 0.6033(2) 0.0332(9) Uani 0.70 1 d P . . O10 O 0.3636(2) 1.21091(15) 0.5538(2) 0.0322(8) Uani 0.70 1 d P . . O11 O 0.4911(2) 1.17510(16) 0.6202(3) 0.0354(9) Uani 0.70 1 d P . . O12 O 0.51809(19) 1.08519(15) 0.7090(2) 0.0342(8) Uani 0.70 1 d P . . O13 O 0.14183(14) 0.99704(10) 0.46277(17) 0.0415(7) Uani 1 1 d . . . O14 O 0.13229(14) 0.91005(10) 0.54980(15) 0.0391(6) Uani 1 1 d . . . O15 O 0.00013(14) 0.92106(10) 0.56382(15) 0.0415(7) Uani 1 1 d . . . O16 O 0.37647(14) 1.06458(10) 0.50921(15) 0.0433(7) Uani 1 1 d . . . O17 O 0.42007(15) 0.93256(10) 0.54359(16) 0.0471(7) Uani 1 1 d . . . O18 O 0.55233(15) 0.89552(11) 0.59391(16) 0.0458(7) Uani 1 1 d . . . N1 N 0.31037(15) 0.72308(10) 0.24647(16) 0.0307(7) Uani 1 1 d D . . N2 N 0.32313(15) 0.64389(10) 0.33923(16) 0.0301(7) Uani 1 1 d D . . N3 N 0.18990(15) 1.28183(10) 0.77006(15) 0.0273(6) Uani 1 1 d D . . N4 N 0.17422(14) 1.35836(10) 0.67205(15) 0.0253(6) Uani 1 1 d D . . C1 C 0.3210(4) 0.7324(3) 0.3278(3) 0.0272(17) Uani 0.8150(19) 1 d PD A 1 H1 H 0.3235 0.7664 0.3475 0.033 Uiso 0.8150(19) 1 calc PR A 1 C1A C 0.3009(11) 0.6764(6) 0.2051(12) 0.045(7) Uani 0.1850(19) 1 d PD A 2 H1A H 0.2874 0.6731 0.1499 0.053 Uiso 0.1850(19) 1 calc PR A 2 C2 C 0.3276(3) 0.6911(2) 0.3773(3) 0.0318(12) Uani 0.8150(19) 1 d PD A 1 H2 H 0.3345 0.6943 0.4322 0.038 Uiso 0.8150(19) 1 calc PR A 1 C2A C 0.3146(14) 0.6353(10) 0.2586(6) 0.048(8) Uani 0.1850(19) 1 d PDU A 2 H2A H 0.3182 0.6015 0.2402 0.057 Uiso 0.1850(19) 1 calc PR A 2 C3 C 0.30137(18) 0.76633(12) 0.1967(2) 0.0284(8) Uani 1 1 d . A . C4 C 0.24598(19) 0.79908(13) 0.1908(2) 0.0317(8) Uani 1 1 d . . . C5 C 0.2408(2) 0.84315(14) 0.1447(2) 0.0398(9) Uani 1 1 d . A . H5 H 0.2050 0.8662 0.1421 0.048 Uiso 1 1 calc R . . C6 C 0.2872(2) 0.85381(15) 0.1029(2) 0.0419(10) Uani 1 1 d . . . H6 H 0.2831 0.8841 0.0722 0.050 Uiso 1 1 calc R A . C7 C 0.3390(2) 0.82072(14) 0.1058(2) 0.0364(9) Uani 1 1 d . A . H7 H 0.3698 0.8281 0.0759 0.044 Uiso 1 1 calc R . . C8 C 0.34735(19) 0.77638(13) 0.1518(2) 0.0303(8) Uani 1 1 d . . . C9 C 0.19184(19) 0.78561(14) 0.2305(2) 0.0347(9) Uani 1 1 d . A . H9 H 0.2139 0.7758 0.2855 0.042 Uiso 1 1 calc R . . C10 C 0.1526(2) 0.73880(17) 0.1911(3) 0.0606(14) Uani 1 1 d . . . H10A H 0.1217 0.7277 0.2214 0.091 Uiso 1 1 calc R A . H10B H 0.1833 0.7108 0.1886 0.091 Uiso 1 1 calc R . . H10C H 0.1276 0.7480 0.1382 0.091 Uiso 1 1 calc R . . C11 C 0.1432(2) 0.82841(16) 0.2336(3) 0.0468(11) Uani 1 1 d . . . H11A H 0.1677 0.8590 0.2570 0.070 Uiso 1 1 calc R A . H11B H 0.1134 0.8175 0.2653 0.070 Uiso 1 1 calc R . . H11C H 0.1172 0.8364 0.1807 0.070 Uiso 1 1 calc R . . C12 C 0.40512(19) 0.73984(14) 0.1545(2) 0.0336(8) Uani 1 1 d . A . H12 H 0.3863 0.7044 0.1481 0.040 Uiso 1 1 calc R . . C13 C 0.4568(2) 0.74110(17) 0.2331(2) 0.0433(10) Uani 1 1 d . . . H13A H 0.4776 0.7750 0.2409 0.065 Uiso 1 1 calc R A . H13B H 0.4907 0.7150 0.2336 0.065 Uiso 1 1 calc R . . H13C H 0.4351 0.7341 0.2750 0.065 Uiso 1 1 calc R . . C14 C 0.4393(2) 0.74816(16) 0.0889(2) 0.0433(10) Uani 1 1 d . . . H14A H 0.4064 0.7462 0.0385 0.065 Uiso 1 1 calc R A . H14B H 0.4731 0.7216 0.0915 0.065 Uiso 1 1 calc R . . H14C H 0.4605 0.7820 0.0947 0.065 Uiso 1 1 calc R . . C15 C 0.33560(18) 0.59971(13) 0.38683(19) 0.0268(7) Uani 1 1 d . A . C16 C 0.28296(18) 0.56570(14) 0.3884(2) 0.0304(8) Uani 1 1 d . . . C17 C 0.2969(2) 0.52105(16) 0.4321(2) 0.0382(9) Uani 1 1 d . A . H17 H 0.2618 0.4979 0.4329 0.046 Uiso 1 1 calc R . . C18 C 0.3608(2) 0.50944(15) 0.4748(2) 0.0399(10) Uani 1 1 d . . . H18 H 0.3693 0.4784 0.5037 0.048 Uiso 1 1 calc R A . C19 C 0.4119(2) 0.54325(14) 0.4748(2) 0.0358(9) Uani 1 1 d . A . H19 H 0.4555 0.5355 0.5048 0.043 Uiso 1 1 calc R . . C20 C 0.40064(18) 0.58869(13) 0.43158(19) 0.0291(8) Uani 1 1 d . . . C21 C 0.21252(19) 0.57961(17) 0.3448(2) 0.0407(10) Uani 1 1 d . A . H21 H 0.2143 0.5938 0.2929 0.049 Uiso 1 1 calc R . . C22 C 0.1640(2) 0.53478(19) 0.3296(3) 0.0533(12) Uani 1 1 d . . . H22A H 0.1793 0.5089 0.2981 0.080 Uiso 1 1 calc R A . H22B H 0.1200 0.5470 0.3015 0.080 Uiso 1 1 calc R . . H22C H 0.1616 0.5196 0.3794 0.080 Uiso 1 1 calc R . . C23 C 0.1859(2) 0.6221(2) 0.3888(3) 0.0642(14) Uani 1 1 d . . . H23A H 0.1425 0.6336 0.3576 0.096 Uiso 1 1 calc R A . H23B H 0.2168 0.6511 0.3979 0.096 Uiso 1 1 calc R . . H23C H 0.1815 0.6088 0.4389 0.096 Uiso 1 1 calc R . . C24 C 0.45839(18) 0.62390(14) 0.4286(2) 0.0324(8) Uani 1 1 d . A . H24 H 0.4406 0.6596 0.4202 0.039 Uiso 1 1 calc R . . C25 C 0.5139(2) 0.62393(17) 0.5041(3) 0.0503(11) Uani 1 1 d . . . H25A H 0.4953 0.6324 0.5482 0.075 Uiso 1 1 calc R A . H25B H 0.5474 0.6495 0.5003 0.075 Uiso 1 1 calc R . . H25C H 0.5344 0.5899 0.5122 0.075 Uiso 1 1 calc R . . C26 C 0.4862(2) 0.61024(18) 0.3593(3) 0.0493(11) Uani 1 1 d . . . H26A H 0.5069 0.5763 0.3675 0.074 Uiso 1 1 calc R A . H26B H 0.5195 0.6358 0.3544 0.074 Uiso 1 1 calc R . . H26C H 0.4502 0.6099 0.3114 0.074 Uiso 1 1 calc R . . C27 C 0.1817(3) 1.2694(3) 0.6907(3) 0.0227(13) Uani 0.7997(17) 1 d PD B 4 H27 H 0.1815 1.2348 0.6739 0.027 Uiso 0.7997(17) 1 calc PR B 4 C28 C 0.1740(3) 1.3096(2) 0.6382(3) 0.0244(11) Uani 0.7997(17) 1 d PD B 4 H28 H 0.1690 1.3046 0.5839 0.029 Uiso 0.7997(17) 1 calc PR B 4 C29 C 0.19872(17) 1.23978(12) 0.82234(19) 0.0255(7) Uani 1 1 d . B . C30 C 0.25526(17) 1.20808(13) 0.83365(19) 0.0259(7) Uani 1 1 d . . . C31 C 0.2591(2) 1.16473(13) 0.8805(2) 0.0334(8) Uani 1 1 d . B . H31 H 0.2963 1.1425 0.8871 0.040 Uiso 1 1 calc R . . C32 C 0.2099(2) 1.15329(14) 0.9178(2) 0.0352(9) Uani 1 1 d . . . H32 H 0.2128 1.1230 0.9483 0.042 Uiso 1 1 calc R B . C33 C 0.15690(19) 1.18592(13) 0.9104(2) 0.0314(8) Uani 1 1 d . B . H33 H 0.1240 1.1783 0.9374 0.038 Uiso 1 1 calc R . . C34 C 0.15017(17) 1.22990(13) 0.86452(18) 0.0252(7) Uani 1 1 d . . . C35 C 0.31208(17) 1.22285(13) 0.7980(2) 0.0273(7) Uani 1 1 d . B . H35 H 0.2922 1.2320 0.7421 0.033 Uiso 1 1 calc R . . C36 C 0.3483(2) 1.27056(15) 0.8386(3) 0.0486(11) Uani 1 1 d . . . H36A H 0.3162 1.2981 0.8379 0.073 Uiso 1 1 calc R B . H36B H 0.3811 1.2819 0.8110 0.073 Uiso 1 1 calc R . . H36C H 0.3709 1.2621 0.8927 0.073 Uiso 1 1 calc R . . C37 C 0.3631(2) 1.18082(15) 0.7994(2) 0.0400(9) Uani 1 1 d . . . H37A H 0.3853 1.1723 0.8536 0.060 Uiso 1 1 calc R B . H37B H 0.3960 1.1928 0.7725 0.060 Uiso 1 1 calc R . . H37C H 0.3408 1.1502 0.7730 0.060 Uiso 1 1 calc R . . C38 C 0.09128(18) 1.26571(14) 0.8571(2) 0.0310(8) Uani 1 1 d . B . H38 H 0.1093 1.3014 0.8599 0.037 Uiso 1 1 calc R . . C39 C 0.0419(2) 1.2615(2) 0.7810(3) 0.0590(13) Uani 1 1 d . . . H39A H 0.0643 1.2646 0.7388 0.088 Uiso 1 1 calc R B . H39B H 0.0089 1.2889 0.7763 0.088 Uiso 1 1 calc R . . H39C H 0.0197 1.2281 0.7774 0.088 Uiso 1 1 calc R . . C40 C 0.0579(3) 1.2606(2) 0.9243(3) 0.0625(14) Uani 1 1 d . . . H40A H 0.0261 1.2886 0.9216 0.094 Uiso 1 1 calc R B . H40B H 0.0917 1.2622 0.9741 0.094 Uiso 1 1 calc R . . H40C H 0.0347 1.2276 0.9202 0.094 Uiso 1 1 calc R . . C41 C 0.15892(17) 1.40027(12) 0.62044(19) 0.0243(7) Uani 1 1 d . B . C42 C 0.20923(17) 1.43633(13) 0.61731(19) 0.0262(7) Uani 1 1 d . . . C43 C 0.1916(2) 1.47976(14) 0.5700(2) 0.0365(9) Uani 1 1 d . B . H43 H 0.2246 1.5045 0.5684 0.044 Uiso 1 1 calc R . . C44 C 0.1278(2) 1.48767(15) 0.5258(2) 0.0394(10) Uani 1 1 d . . . H44 H 0.1170 1.5177 0.4948 0.047 Uiso 1 1 calc R B . C45 C 0.0796(2) 1.45166(14) 0.5269(2) 0.0343(8) Uani 1 1 d . B . H45 H 0.0360 1.4567 0.4950 0.041 Uiso 1 1 calc R . . C46 C 0.09363(17) 1.40782(13) 0.57395(19) 0.0270(7) Uani 1 1 d . . . C47 C 0.27989(18) 1.42677(14) 0.6635(2) 0.0328(8) Uani 1 1 d . B . H47 H 0.2783 1.4147 0.7165 0.039 Uiso 1 1 calc R . . C48 C 0.3119(2) 1.38395(17) 0.6257(3) 0.0488(11) Uani 1 1 d . . . H48A H 0.2833 1.3536 0.6179 0.073 Uiso 1 1 calc R B . H48B H 0.3553 1.3752 0.6600 0.073 Uiso 1 1 calc R . . H48C H 0.3175 1.3958 0.5753 0.073 Uiso 1 1 calc R . . C49 C 0.3243(2) 1.47447(16) 0.6743(2) 0.0437(10) Uani 1 1 d . . . H49A H 0.3278 1.4868 0.6232 0.066 Uiso 1 1 calc R B . H49B H 0.3685 1.4657 0.7064 0.066 Uiso 1 1 calc R . . H49C H 0.3049 1.5014 0.7002 0.066 Uiso 1 1 calc R . . C50 C 0.03852(18) 1.37094(13) 0.5785(2) 0.0334(8) Uani 1 1 d . B . H50 H 0.0584 1.3359 0.5886 0.040 Uiso 1 1 calc R . . C51 C -0.0173(2) 1.36825(16) 0.5035(3) 0.0489(11) Uani 1 1 d . . . H51A H -0.0402 1.4014 0.4944 0.073 Uiso 1 1 calc R B . H51B H -0.0489 1.3415 0.5087 0.073 Uiso 1 1 calc R . . H51C H 0.0013 1.3602 0.4594 0.073 Uiso 1 1 calc R . . C52 C 0.0103(2) 1.38504(17) 0.6479(3) 0.0459(10) Uani 1 1 d . . . H52A H 0.0464 1.3864 0.6957 0.069 Uiso 1 1 calc R B . H52B H -0.0222 1.3591 0.6537 0.069 Uiso 1 1 calc R . . H52C H -0.0114 1.4186 0.6386 0.069 Uiso 1 1 calc R . . C53 C 0.2090(2) 0.78620(15) 0.4959(2) 0.0434(10) Uani 1 1 d . . . H53A H 0.2069 0.8032 0.5452 0.052 Uiso 1 1 calc R . . H53B H 0.2454 0.7607 0.5077 0.052 Uiso 1 1 calc R . . C54 C 0.1451(2) 0.76045(15) 0.4603(3) 0.0455(10) Uani 1 1 d . . . H54A H 0.1464 0.7450 0.4098 0.055 Uiso 1 1 calc R . . H54B H 0.1371 0.7328 0.4951 0.055 Uiso 1 1 calc R . . C55 C 0.0297(2) 0.77468(15) 0.4185(3) 0.0440(10) Uani 1 1 d . . . H55A H 0.0191 0.7516 0.4580 0.053 Uiso 1 1 calc R . . H55B H 0.0300 0.7541 0.3717 0.053 Uiso 1 1 calc R . . C56 C -0.0214(2) 0.81599(15) 0.3976(3) 0.0411(10) Uani 1 1 d . . . H56A H -0.0661 0.8006 0.3799 0.049 Uiso 1 1 calc R . . H56B H -0.0203 0.8376 0.4439 0.049 Uiso 1 1 calc R . . C57 C -0.06174(19) 0.87794(17) 0.2986(3) 0.0450(10) Uani 1 1 d . . . H57A H -0.0705 0.9040 0.3353 0.054 Uiso 1 1 calc R . . H57B H -0.1021 0.8567 0.2804 0.054 Uiso 1 1 calc R . . C58 C -0.0452(2) 0.90376(17) 0.2305(3) 0.0456(10) Uani 1 1 d . . . H58A H -0.0334 0.8778 0.1956 0.055 Uiso 1 1 calc R . . H58B H -0.0841 0.9233 0.2004 0.055 Uiso 1 1 calc R . . C59 C 0.0312(2) 0.96072(15) 0.1967(2) 0.0405(10) Uani 1 1 d . . . H59A H -0.0048 0.9821 0.1645 0.049 Uiso 1 1 calc R . . H59B H 0.0425 0.9338 0.1629 0.049 Uiso 1 1 calc R . . C60 C 0.0902(2) 0.99300(14) 0.2293(2) 0.0360(9) Uani 1 1 d . . . H60A H 0.1034 1.0115 0.1868 0.043 Uiso 1 1 calc R . . H60B H 0.0801 1.0186 0.2660 0.043 Uiso 1 1 calc R . . C61 C 0.2028(2) 0.98742(15) 0.2985(2) 0.0400(10) Uani 1 1 d . . . H61A H 0.2003 1.0079 0.3447 0.048 Uiso 1 1 calc R . . H61B H 0.2111 1.0110 0.2582 0.048 Uiso 1 1 calc R . . C62 C 0.25702(19) 0.94899(15) 0.3203(2) 0.0373(9) Uani 1 1 d . . . H62A H 0.2565 0.9264 0.2752 0.045 Uiso 1 1 calc R . . H62B H 0.3005 0.9667 0.3351 0.045 Uiso 1 1 calc R . . C63 C 0.29617(18) 0.87912(15) 0.4044(2) 0.0376(9) Uani 1 1 d . . . H63A H 0.3411 0.8942 0.4209 0.045 Uiso 1 1 calc R . . H63B H 0.2942 0.8572 0.3582 0.045 Uiso 1 1 calc R . . C64 C 0.28306(19) 0.84737(15) 0.4691(2) 0.0376(9) Uani 1 1 d . . . H64A H 0.3182 0.8212 0.4855 0.045 Uiso 1 1 calc R . . H64B H 0.2828 0.8694 0.5145 0.045 Uiso 1 1 calc R . . C65 C 0.3637(4) 1.0126(2) 0.7644(4) 0.0419(15) Uani 0.70 1 d P . . C66 C 0.2974(3) 1.0355(2) 0.7464(3) 0.0720(17) Uani 1 1 d . . . C67 C 0.2221(3) 1.0955(3) 0.6685(4) 0.0396(15) Uani 0.70 1 d P . . C68 C 0.2102(2) 1.12690(18) 0.6006(4) 0.0657(15) Uani 1 1 d . . . C69 C 0.2483(3) 1.1996(2) 0.5388(3) 0.0382(14) Uani 0.70 1 d P . . C70 C 0.3000(3) 1.2349(2) 0.5486(3) 0.0683(16) Uani 1 1 d . . . C71 C 0.4192(3) 1.2444(2) 0.5674(4) 0.0426(14) Uani 0.70 1 d P . . C72 C 0.4757(2) 1.21600(19) 0.5625(3) 0.0534(12) Uani 1 1 d . . . C73 C 0.5461(3) 1.1437(3) 0.6176(4) 0.0481(15) Uani 0.70 1 d P . . C74 C 0.5680(2) 1.11893(17) 0.6947(3) 0.0476(11) Uani 1 1 d . . . C75 C 0.5288(3) 1.0715(2) 0.7896(3) 0.0406(14) Uani 0.70 1 d P . . C76 C 0.4793(2) 1.03335(18) 0.7979(3) 0.0501(11) Uani 1 1 d . . . C77 C 0.1951(2) 0.98131(16) 0.5273(3) 0.0473(11) Uani 1 1 d . . . H77A H 0.2190 1.0122 0.5522 0.057 Uiso 1 1 calc R . . H77B H 0.2267 0.9604 0.5072 0.057 Uiso 1 1 calc R . . C78 C 0.1728(2) 0.95098(15) 0.5879(2) 0.0456(10) Uani 1 1 d . . . H78A H 0.2118 0.9373 0.6269 0.055 Uiso 1 1 calc R . . H78B H 0.1474 0.9732 0.6152 0.055 Uiso 1 1 calc R . . C79 C 0.1056(2) 0.87963(16) 0.6010(2) 0.0455(10) Uani 1 1 d . . . H79A H 0.1418 0.8702 0.6469 0.055 Uiso 1 1 calc R . . H79B H 0.0877 0.8475 0.5739 0.055 Uiso 1 1 calc R . . C80 C 0.0517(2) 0.90582(16) 0.6288(2) 0.0454(10) Uani 1 1 d . . . H80A H 0.0338 0.8821 0.6621 0.055 Uiso 1 1 calc R . . H80B H 0.0700 0.9363 0.6604 0.055 Uiso 1 1 calc R . . C81 C -0.0497(2) 0.94979(16) 0.5864(2) 0.0430(10) Uani 1 1 d . . . H81A H -0.0294 0.9773 0.6233 0.052 Uiso 1 1 calc R . . H81B H -0.0758 0.9273 0.6124 0.052 Uiso 1 1 calc R . . C82 C -0.0936(2) 0.97246(16) 0.5139(2) 0.0430(10) Uani 1 1 d . . . H82A H -0.0672 0.9939 0.4867 0.052 Uiso 1 1 calc R . . H82B H -0.1154 0.9450 0.4779 0.052 Uiso 1 1 calc R . . C83 C 0.3810(2) 1.01189(15) 0.4916(2) 0.0436(10) Uani 1 1 d . . . H83A H 0.4098 1.0075 0.4554 0.052 Uiso 1 1 calc R . . H83B H 0.3364 0.9983 0.4660 0.052 Uiso 1 1 calc R . . C84 C 0.4092(2) 0.98340(16) 0.5649(2) 0.0489(11) Uani 1 1 d . . . H84A H 0.4514 0.9992 0.5939 0.059 Uiso 1 1 calc R . . H84B H 0.3779 0.9838 0.5986 0.059 Uiso 1 1 calc R . . C85 C 0.4429(3) 0.89854(17) 0.6075(3) 0.0549(12) Uani 1 1 d . . . H85A H 0.4359 0.8628 0.5884 0.066 Uiso 1 1 calc R . . H85B H 0.4160 0.9038 0.6457 0.066 Uiso 1 1 calc R . . C86 C 0.5136(2) 0.90558(18) 0.6474(2) 0.0515(12) Uani 1 1 d . . . H86A H 0.5214 0.9411 0.6672 0.062 Uiso 1 1 calc R . . H86B H 0.5264 0.8819 0.6924 0.062 Uiso 1 1 calc R . . C87 C 0.6194(2) 0.90835(16) 0.6227(2) 0.0467(11) Uani 1 1 d . . . H87A H 0.6406 0.8845 0.6653 0.056 Uiso 1 1 calc R . . H87B H 0.6233 0.9436 0.6441 0.056 Uiso 1 1 calc R . . C88 C 0.6535(2) 0.90503(16) 0.5586(2) 0.0444(10) Uani 1 1 d . . . H88A H 0.7001 0.9161 0.5789 0.053 Uiso 1 1 calc R . . H88B H 0.6541 0.8687 0.5424 0.053 Uiso 1 1 calc R . . C72A C 0.5181(7) 1.1782(5) 0.5843(8) 0.038(3) Uani 0.30 1 d PU . . C74A C 0.5526(8) 1.0959(6) 0.7613(10) 0.049(4) Uani 0.30 1 d PU . . C70A C 0.3556(8) 1.2457(7) 0.5541(9) 0.048(4) Uani 0.30 1 d PU . . C66A C 0.2471(7) 1.0594(5) 0.7072(8) 0.039(3) Uani 0.30 1 d PU . . C68A C 0.2163(7) 1.1617(5) 0.5575(8) 0.038(3) Uani 0.30 1 d PU . . C76A C 0.4176(8) 1.0108(5) 0.7829(8) 0.039(3) Uani 0.30 1 d PU . . O9A O 0.2813(5) 1.1843(4) 0.5804(6) 0.036(2) Uani 0.30 1 d PU . . O7A O 0.3634(5) 1.0453(4) 0.7501(5) 0.036(2) Uani 0.30 1 d PU . . O8A O 0.2537(6) 1.0905(3) 0.6437(6) 0.036(2) Uani 0.30 1 d P . . O11A O 0.5099(5) 1.1526(4) 0.6557(6) 0.036(2) Uani 0.30 1 d PU . . O12A O 0.4949(5) 1.0634(3) 0.7403(6) 0.037(2) Uani 0.30 1 d PU . . O10A O 0.4045(5) 1.2046(3) 0.5542(5) 0.030(2) Uani 0.30 1 d PU . . C27A C 0.1981(10) 1.3310(5) 0.8058(11) 0.032(5) Uiso 0.2003(17) 1 d PD B 3 H27A H 0.2111 1.3361 0.8607 0.039 Uiso 0.2003(17) 1 calc PR B 3 C28A C 0.1851(12) 1.3715(8) 0.7514(6) 0.049(7) Uiso 0.2003(17) 1 d PD B 3 H28A H 0.1836 1.4061 0.7675 0.058 Uiso 0.2003(17) 1 calc PR B 3 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 0.0317(3) 0.0249(3) 0.0231(3) -0.0034(3) 0.0083(2) -0.0025(3) Ga1A 0.0383(19) 0.033(3) 0.020(2) -0.0062(16) 0.0065(18) 0.0025(18) Ga2 0.0324(3) 0.0211(3) 0.0224(3) -0.0029(2) 0.0073(2) -0.0017(2) Ga2A 0.0321(14) 0.027(2) 0.0186(19) -0.0039(12) 0.0066(15) -0.0013(15) K1 0.0259(4) 0.0260(4) 0.0329(4) 0.0008(3) 0.0079(3) -0.0012(3) K2 0.0263(4) 0.0280(4) 0.0292(4) 0.0032(3) 0.0089(3) 0.0010(3) O1 0.0298(15) 0.0362(14) 0.0379(14) 0.0063(11) 0.0059(12) 0.0040(11) O2 0.0327(15) 0.0274(13) 0.0479(16) 0.0012(12) 0.0128(13) -0.0007(11) O3 0.0224(13) 0.0377(14) 0.0450(15) 0.0043(12) 0.0101(12) -0.0005(11) O4 0.0375(16) 0.0372(14) 0.0325(14) 0.0009(11) 0.0056(12) -0.0030(12) O5 0.0372(16) 0.0274(13) 0.0444(15) 0.0078(11) 0.0085(13) -0.0029(11) O6 0.0292(14) 0.0350(13) 0.0375(14) 0.0033(11) 0.0126(12) 0.0021(11) O7 0.039(2) 0.030(2) 0.039(2) 0.0064(17) 0.0140(19) 0.0076(18) O8 0.029(2) 0.033(2) 0.035(2) -0.0034(18) 0.0151(19) -0.0039(18) O9 0.031(2) 0.031(2) 0.037(2) 0.0034(17) 0.0076(19) 0.0053(17) O10 0.032(2) 0.026(2) 0.038(2) 0.0010(16) 0.0090(19) 0.0011(18) O11 0.032(2) 0.042(2) 0.036(2) -0.0033(19) 0.014(2) -0.0043(19) O12 0.027(2) 0.044(2) 0.034(2) -0.0025(18) 0.0104(18) 0.0022(17) O13 0.0394(17) 0.0347(14) 0.0534(17) -0.0078(13) 0.0174(14) 0.0020(12) O14 0.0415(17) 0.0334(14) 0.0393(15) -0.0060(12) 0.0045(13) 0.0048(12) O15 0.0443(17) 0.0431(15) 0.0372(15) -0.0021(12) 0.0106(13) 0.0100(13) O16 0.0501(18) 0.0395(15) 0.0383(15) -0.0078(12) 0.0074(14) 0.0092(13) O17 0.057(2) 0.0380(15) 0.0445(16) -0.0020(13) 0.0090(15) -0.0014(14) O18 0.0501(19) 0.0488(17) 0.0367(15) -0.0051(13) 0.0077(14) 0.0060(14) N1 0.0393(19) 0.0238(14) 0.0321(16) -0.0011(12) 0.0150(14) 0.0006(13) N2 0.0354(18) 0.0245(14) 0.0275(15) -0.0003(12) 0.0024(13) 0.0023(13) N3 0.0339(17) 0.0234(14) 0.0286(15) 0.0042(12) 0.0151(13) 0.0045(12) N4 0.0261(16) 0.0224(13) 0.0251(14) 0.0019(12) 0.0023(12) -0.0002(12) C1 0.032(4) 0.029(4) 0.020(4) -0.002(3) 0.006(3) -0.001(3) C1A 0.046(15) 0.041(13) 0.056(16) 0.030(13) 0.031(13) 0.018(12) C2 0.037(3) 0.029(3) 0.030(3) 0.002(2) 0.009(2) 0.001(2) C2A 0.047(9) 0.049(9) 0.049(9) 0.000(5) 0.015(5) -0.001(5) C3 0.035(2) 0.0212(16) 0.0280(18) -0.0049(14) 0.0064(16) -0.0028(15) C4 0.035(2) 0.0291(18) 0.0284(18) -0.0055(15) 0.0024(16) -0.0013(16) C5 0.047(3) 0.031(2) 0.037(2) 0.0007(17) 0.0035(19) 0.0045(18) C6 0.058(3) 0.032(2) 0.032(2) 0.0023(17) 0.0037(19) -0.002(2) C7 0.048(3) 0.038(2) 0.0238(18) -0.0032(16) 0.0090(17) -0.0104(19) C8 0.034(2) 0.0291(18) 0.0256(17) -0.0060(15) 0.0037(16) -0.0074(16) C9 0.032(2) 0.0318(19) 0.040(2) -0.0053(16) 0.0081(18) 0.0024(16) C10 0.046(3) 0.045(3) 0.102(4) -0.030(3) 0.039(3) -0.013(2) C11 0.043(3) 0.038(2) 0.060(3) -0.009(2) 0.015(2) 0.0055(19) C12 0.040(2) 0.0304(18) 0.035(2) -0.0065(16) 0.0167(18) -0.0089(17) C13 0.036(2) 0.056(3) 0.037(2) -0.0046(19) 0.0077(19) 0.007(2) C14 0.044(3) 0.047(2) 0.043(2) -0.0029(19) 0.020(2) -0.007(2) C15 0.033(2) 0.0282(17) 0.0206(16) -0.0033(14) 0.0092(15) 0.0041(15) C16 0.031(2) 0.0372(19) 0.0258(18) -0.0029(15) 0.0119(16) 0.0017(16) C17 0.043(2) 0.047(2) 0.031(2) 0.0029(17) 0.0208(19) -0.0045(19) C18 0.053(3) 0.038(2) 0.032(2) 0.0117(17) 0.016(2) 0.0049(19) C19 0.038(2) 0.040(2) 0.0287(19) 0.0058(16) 0.0077(17) 0.0097(18) C20 0.033(2) 0.0318(18) 0.0233(17) -0.0015(15) 0.0082(15) 0.0042(16) C21 0.027(2) 0.059(3) 0.035(2) 0.0062(19) 0.0077(17) 0.0000(19) C22 0.038(3) 0.084(3) 0.040(2) -0.010(2) 0.013(2) -0.012(2) C23 0.030(3) 0.069(3) 0.095(4) -0.014(3) 0.019(3) 0.006(2) C24 0.031(2) 0.0288(18) 0.036(2) -0.0020(16) 0.0048(17) 0.0036(16) C25 0.047(3) 0.049(2) 0.047(2) -0.005(2) -0.002(2) -0.006(2) C26 0.039(2) 0.060(3) 0.053(3) -0.011(2) 0.019(2) -0.017(2) C27 0.026(3) 0.023(3) 0.019(3) -0.002(2) 0.005(3) -0.001(2) C28 0.026(3) 0.028(3) 0.019(3) 0.004(2) 0.005(2) 0.000(2) C29 0.031(2) 0.0217(16) 0.0219(16) -0.0022(13) 0.0039(15) -0.0019(14) C30 0.0285(19) 0.0266(17) 0.0201(16) -0.0026(13) 0.0013(14) -0.0007(14) C31 0.040(2) 0.0266(17) 0.0281(18) -0.0007(15) -0.0009(17) 0.0058(16) C32 0.049(2) 0.0285(18) 0.0256(18) 0.0047(15) 0.0043(17) -0.0042(17) C33 0.038(2) 0.0330(19) 0.0234(17) -0.0006(15) 0.0093(16) -0.0126(17) C34 0.0258(19) 0.0274(17) 0.0208(16) -0.0020(14) 0.0026(14) -0.0053(14) C35 0.0230(18) 0.0313(18) 0.0258(17) -0.0007(14) 0.0030(15) 0.0010(15) C36 0.039(3) 0.038(2) 0.071(3) -0.014(2) 0.018(2) -0.0086(19) C37 0.034(2) 0.039(2) 0.047(2) -0.0052(18) 0.0100(19) 0.0065(18) C38 0.030(2) 0.0320(18) 0.0331(19) 0.0030(16) 0.0115(16) -0.0016(16) C39 0.050(3) 0.073(3) 0.053(3) -0.006(2) 0.011(2) 0.005(3) C40 0.055(3) 0.083(4) 0.052(3) -0.002(3) 0.019(3) 0.007(3) C41 0.0298(19) 0.0215(15) 0.0226(16) -0.0006(13) 0.0085(15) 0.0019(14) C42 0.029(2) 0.0257(17) 0.0255(17) -0.0020(14) 0.0105(15) -0.0007(15) C43 0.049(3) 0.0316(19) 0.035(2) 0.0059(16) 0.0222(19) -0.0025(18) C44 0.052(3) 0.033(2) 0.036(2) 0.0158(17) 0.015(2) 0.0076(19) C45 0.040(2) 0.0320(19) 0.0287(19) 0.0046(16) 0.0040(17) 0.0081(17) C46 0.028(2) 0.0264(17) 0.0260(17) -0.0010(14) 0.0059(15) 0.0036(15) C47 0.031(2) 0.039(2) 0.0308(19) -0.0030(16) 0.0111(16) -0.0085(17) C48 0.026(2) 0.052(3) 0.071(3) -0.007(2) 0.017(2) 0.0013(19) C49 0.040(2) 0.056(3) 0.038(2) -0.006(2) 0.0145(19) -0.016(2) C50 0.026(2) 0.0252(17) 0.044(2) 0.0007(16) 0.0009(17) 0.0036(15) C51 0.044(3) 0.039(2) 0.053(3) -0.006(2) -0.007(2) -0.0002(19) C52 0.030(2) 0.050(2) 0.061(3) -0.004(2) 0.017(2) -0.0061(19) C53 0.044(3) 0.037(2) 0.048(2) 0.0155(19) 0.010(2) 0.0079(19) C54 0.050(3) 0.0274(19) 0.062(3) 0.0093(19) 0.019(2) 0.0063(18) C55 0.044(3) 0.035(2) 0.054(3) 0.0042(19) 0.015(2) -0.0105(19) C56 0.031(2) 0.044(2) 0.053(2) 0.0008(19) 0.020(2) -0.0112(18) C57 0.023(2) 0.049(2) 0.061(3) -0.001(2) 0.007(2) 0.0024(18) C58 0.029(2) 0.050(2) 0.051(3) 0.003(2) -0.0040(19) -0.0002(19) C59 0.047(3) 0.041(2) 0.031(2) 0.0072(17) 0.0048(18) 0.0093(19) C60 0.048(2) 0.0297(19) 0.032(2) 0.0086(16) 0.0136(18) 0.0021(18) C61 0.045(3) 0.033(2) 0.045(2) 0.0041(17) 0.017(2) -0.0124(18) C62 0.034(2) 0.043(2) 0.038(2) -0.0034(18) 0.0152(18) -0.0137(18) C63 0.022(2) 0.046(2) 0.045(2) -0.0070(19) 0.0096(17) 0.0008(17) C64 0.028(2) 0.042(2) 0.040(2) -0.0008(18) 0.0040(17) 0.0049(17) C65 0.064(5) 0.024(3) 0.046(4) 0.014(3) 0.029(3) 0.000(3) C66 0.045(3) 0.086(4) 0.083(4) 0.056(3) 0.013(3) -0.008(3) C67 0.017(3) 0.054(4) 0.051(4) -0.001(3) 0.015(3) 0.001(3) C68 0.032(3) 0.041(2) 0.113(4) 0.016(3) -0.002(3) -0.004(2) C69 0.038(4) 0.043(3) 0.031(3) 0.008(3) 0.004(3) 0.018(3) C70 0.065(4) 0.059(3) 0.096(4) 0.045(3) 0.047(3) 0.034(3) C71 0.048(4) 0.028(3) 0.051(4) 0.005(3) 0.012(3) -0.008(3) C72 0.045(3) 0.067(3) 0.044(2) 0.021(2) 0.005(2) -0.024(2) C73 0.029(3) 0.061(4) 0.060(4) 0.005(3) 0.021(3) 0.001(3) C74 0.027(2) 0.048(2) 0.071(3) 0.005(2) 0.018(2) 0.0033(19) C75 0.038(4) 0.047(4) 0.032(3) 0.002(3) -0.001(3) 0.006(3) C76 0.040(3) 0.061(3) 0.046(2) 0.022(2) 0.004(2) 0.016(2) C77 0.035(2) 0.041(2) 0.066(3) -0.020(2) 0.012(2) -0.0030(19) C78 0.042(3) 0.040(2) 0.048(2) -0.0157(19) 0.000(2) 0.0073(19) C79 0.055(3) 0.037(2) 0.040(2) 0.0054(18) 0.003(2) 0.012(2) C80 0.062(3) 0.042(2) 0.032(2) 0.0057(18) 0.011(2) 0.010(2) C81 0.048(3) 0.038(2) 0.048(2) -0.0034(19) 0.022(2) 0.0044(19) C82 0.036(2) 0.041(2) 0.052(2) -0.0139(19) 0.012(2) 0.0031(18) C83 0.052(3) 0.040(2) 0.038(2) -0.0050(18) 0.010(2) 0.004(2) C84 0.060(3) 0.048(2) 0.038(2) -0.0054(19) 0.011(2) 0.007(2) C85 0.065(3) 0.043(2) 0.062(3) 0.010(2) 0.027(3) 0.004(2) C86 0.070(3) 0.049(3) 0.037(2) 0.009(2) 0.017(2) 0.006(2) C87 0.055(3) 0.042(2) 0.037(2) 0.0000(18) 0.000(2) 0.009(2) C88 0.046(3) 0.044(2) 0.037(2) -0.0037(18) -0.0011(19) 0.014(2) C72A 0.038(5) 0.041(5) 0.039(5) 0.000(4) 0.016(4) -0.003(4) C74A 0.047(5) 0.048(5) 0.049(5) 0.004(4) 0.004(4) -0.001(4) C70A 0.048(5) 0.047(5) 0.049(5) -0.001(4) 0.015(4) 0.004(4) C66A 0.039(5) 0.040(5) 0.041(5) 0.000(4) 0.014(4) -0.004(4) C68A 0.038(5) 0.036(5) 0.040(5) -0.006(4) 0.007(4) 0.000(4) C76A 0.043(5) 0.036(5) 0.038(5) 0.006(4) 0.009(4) 0.004(4) O9A 0.039(4) 0.035(4) 0.038(4) 0.002(3) 0.017(4) -0.003(3) O7A 0.034(4) 0.038(4) 0.035(4) 0.003(3) 0.010(3) -0.003(3) O8A 0.042(7) 0.021(4) 0.038(6) 0.000(4) 0.000(5) 0.003(4) O11A 0.032(4) 0.037(4) 0.039(4) 0.006(3) 0.010(3) 0.001(3) O12A 0.040(4) 0.035(4) 0.039(4) 0.001(3) 0.014(4) -0.001(3) O10A 0.033(4) 0.030(4) 0.028(4) 0.001(3) 0.007(3) 0.005(3) _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 N2 1.956(3) . ? Ga1 N1 1.983(3) . ? Ga1A N1 1.845(4) . ? Ga1A N2 1.972(4) . ? Ga2 N4 1.964(3) . ? Ga2 N3 1.974(3) . ? Ga2A N3 1.861(4) . ? Ga2A N4 1.925(4) . ? K1 O3 2.807(3) . ? K1 O14 2.816(3) . ? K1 O6 2.850(3) . ? K1 O5 2.859(3) . ? K1 O2 2.871(3) . ? K1 O1 2.875(3) . ? K1 O13 2.932(3) . ? K1 O4 2.957(3) . ? K2 O11A 2.659(9) . ? K2 O16 2.687(3) . ? K2 O11 2.723(4) . ? K2 O8 2.751(4) . ? K2 O7 2.786(4) . ? K2 O9A 2.790(11) . ? K2 O10A 2.799(9) . ? K2 O9 2.803(4) . ? K2 O12 2.823(4) . ? K2 O10 2.842(4) . ? K2 O7A 2.845(10) . ? K2 O12A 2.860(10) . ? O1 C64 1.416(5) . ? O1 C53 1.429(4) . ? O2 C55 1.422(5) . ? O2 C54 1.428(5) . ? O3 C57 1.420(5) . ? O3 C56 1.429(4) . ? O4 C58 1.422(5) . ? O4 C59 1.432(5) . ? O5 C60 1.425(4) . ? O5 C61 1.426(5) . ? O6 C63 1.425(4) . ? O6 C62 1.427(4) . ? O7 O7A 1.013(10) . ? O7 C76A 1.088(14) . ? O7 C76 1.428(6) . ? O7 C65 1.431(7) . ? O8 O8A 0.970(9) . ? O8 C66A 1.034(14) . ? O8 C66 1.427(6) . ? O8 C67 1.443(7) . ? O9 O9A 0.840(9) . ? O9 C68A 1.076(14) . ? O9 C68 1.430(6) . ? O9 C69 1.445(7) . ? O10 O10A 0.866(9) . ? O10 C70A 0.924(16) . ? O10 C71 1.423(7) . ? O10 C70 1.448(6) . ? O11 O11A 0.877(9) . ? O11 C72A 0.953(14) . ? O11 C73 1.420(7) . ? O11 C72 1.456(6) . ? O12 O12A 1.000(9) . ? O12 C74A 1.056(16) . ? O12 C75 1.434(7) . ? O12 C74 1.434(6) . ? O13 C82 1.424(4) 3_576 ? O13 C77 1.436(5) . ? O14 C78 1.421(5) . ? O14 C79 1.421(5) . ? O15 C80 1.418(5) . ? O15 C81 1.419(5) . ? O16 C83 1.418(5) . ? O16 C88 1.442(5) 3_676 ? O17 C84 1.413(5) . ? O17 C85 1.422(5) . ? O18 C87 1.402(5) . ? O18 C86 1.417(5) . ? N1 C1A 1.409(10) . ? N1 C3 1.414(4) . ? N1 C1 1.423(6) . ? N2 C2 1.395(5) . ? N2 C2A 1.412(10) . ? N2 C15 1.413(4) . ? N3 C27 1.411(5) . ? N3 C29 1.417(4) . ? N3 C27A 1.422(9) . ? N4 C28 1.406(5) . ? N4 C28A 1.408(10) . ? N4 C41 1.409(4) . ? C1 C2 1.374(6) . ? C1A C2A 1.411(10) . ? C3 C8 1.418(5) . ? C3 C4 1.418(5) . ? C4 C5 1.398(5) . ? C4 C9 1.515(5) . ? C5 C6 1.387(6) . ? C6 C7 1.373(6) . ? C7 C8 1.400(5) . ? C8 C12 1.527(5) . ? C9 C11 1.518(5) . ? C9 C10 1.536(5) . ? C12 C14 1.526(5) . ? C12 C13 1.528(5) . ? C15 C20 1.415(5) . ? C15 C16 1.417(5) . ? C16 C17 1.388(5) . ? C16 C21 1.520(5) . ? C17 C18 1.388(6) . ? C18 C19 1.384(6) . ? C19 C20 1.398(5) . ? C20 C24 1.526(5) . ? C21 C22 1.524(6) . ? C21 C23 1.538(6) . ? C24 C26 1.528(5) . ? C24 C25 1.530(5) . ? C27 C28 1.383(6) . ? C29 C30 1.411(5) . ? C29 C34 1.426(5) . ? C30 C31 1.393(5) . ? C30 C35 1.527(5) . ? C31 C32 1.386(5) . ? C32 C33 1.375(5) . ? C33 C34 1.393(5) . ? C34 C38 1.521(5) . ? C35 C37 1.522(5) . ? C35 C36 1.537(5) . ? C38 C39 1.479(6) . ? C38 C40 1.529(5) . ? C41 C46 1.414(5) . ? C41 C42 1.420(5) . ? C42 C43 1.401(5) . ? C42 C47 1.513(5) . ? C43 C44 1.377(6) . ? C44 C45 1.378(5) . ? C45 C46 1.402(5) . ? C46 C50 1.516(5) . ? C47 C49 1.533(5) . ? C47 C48 1.538(5) . ? C50 C51 1.530(5) . ? C50 C52 1.536(5) . ? C53 C54 1.482(6) . ? C55 C56 1.493(6) . ? C57 C58 1.495(6) . ? C59 C60 1.482(6) . ? C61 C62 1.486(6) . ? C63 C64 1.494(5) . ? C65 O7A 0.889(10) . ? C65 C76A 1.089(16) . ? C65 C66 1.464(9) . ? C66 C66A 1.266(15) . ? C66 O7A 1.385(11) . ? C67 O8A 0.889(10) . ? C67 C66A 1.201(15) . ? C67 C68 1.424(9) . ? C68 C68A 1.213(14) . ? C68 O8A 1.397(12) . ? C69 O9A 0.959(11) . ? C69 C68A 1.284(15) . ? C69 C70 1.394(8) . ? C70 C70A 1.173(17) . ? C70 O9A 1.524(12) . ? C71 O10A 1.091(10) . ? C71 C70A 1.287(17) . ? C71 C72 1.412(8) . ? C72 C72A 1.315(15) . ? C72 O10A 1.485(11) . ? C73 C72A 1.150(15) . ? C73 O11A 1.157(10) . ? C73 C74 1.475(8) . ? C74 C74A 1.431(18) . ? C74 O11A 1.513(11) . ? C75 O12A 0.996(10) . ? C75 C74A 1.016(16) . ? C75 C76 1.467(8) . ? C76 C76A 1.377(16) . ? C76 O12A 1.390(11) . ? C77 C78 1.499(6) . ? C79 C80 1.501(6) . ? C81 C82 1.497(6) . ? C82 O13 1.424(4) 3_576 ? C83 C84 1.483(6) . ? C85 C86 1.476(7) . ? C87 C88 1.488(6) . ? C88 O16 1.442(5) 3_676 ? C88 K2 3.477(4) 3_676 ? C72A O11A 1.477(17) . ? C74A O12A 1.441(19) . ? C70A O10A 1.479(18) . ? C66A O8A 1.421(17) . ? C68A O9A 1.440(17) . ? C76A O7A 1.446(17) . ? C27A C28A 1.408(10) . ? 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 N2 Ga1 N1 83.02(11) . . ? N1 Ga1A N2 86.23(18) . . ? N4 Ga2 N3 83.07(11) . . ? N3 Ga2A N4 87.21(15) . . ? O3 K1 O14 105.01(8) . . ? O3 K1 O6 154.13(8) . . ? O14 K1 O6 97.27(8) . . ? O3 K1 O5 111.30(8) . . ? O14 K1 O5 132.78(8) . . ? O6 K1 O5 58.92(8) . . ? O3 K1 O2 59.13(8) . . ? O14 K1 O2 74.17(8) . . ? O6 K1 O2 116.59(8) . . ? O5 K1 O2 151.57(8) . . ? O3 K1 O1 111.06(8) . . ? O14 K1 O1 82.13(8) . . ? O6 K1 O1 58.76(7) . . ? O5 K1 O1 110.50(8) . . ? O2 K1 O1 57.83(7) . . ? O3 K1 O13 127.75(8) . . ? O14 K1 O13 57.77(8) . . ? O6 K1 O13 75.55(8) . . ? O5 K1 O13 76.10(8) . . ? O2 K1 O13 131.83(8) . . ? O1 K1 O13 113.86(8) . . ? O3 K1 O4 58.26(7) . . ? O14 K1 O4 128.11(8) . . ? O6 K1 O4 116.42(8) . . ? O5 K1 O4 57.57(8) . . ? O2 K1 O4 117.08(8) . . ? O1 K1 O4 148.68(8) . . ? O13 K1 O4 92.30(8) . . ? O11A K2 O16 97.3(2) . . ? O11A K2 O11 18.70(19) . . ? O16 K2 O11 93.38(11) . . ? O11A K2 O8 158.5(2) . . ? O16 K2 O8 93.93(10) . . ? O11 K2 O8 172.69(11) . . ? O11A K2 O7 98.5(2) . . ? O16 K2 O7 109.16(10) . . ? O11 K2 O7 116.96(14) . . ? O8 K2 O7 60.28(13) . . ? O11A K2 O9A 118.5(3) . . ? O16 K2 O9A 95.9(2) . . ? O11 K2 O9A 101.0(2) . . ? O8 K2 O9A 78.3(2) . . ? O7 K2 O9A 132.0(2) . . ? O11A K2 O10A 61.9(3) . . ? O16 K2 O10A 86.27(19) . . ? O11 K2 O10A 43.2(2) . . ? O8 K2 O10A 137.5(2) . . ? O7 K2 O10A 157.2(2) . . ? O9A K2 O10A 59.5(3) . . ? O11A K2 O9 134.4(2) . . ? O16 K2 O9 98.44(11) . . ? O11 K2 O9 117.72(13) . . ? O8 K2 O9 61.14(13) . . ? O7 K2 O9 115.88(13) . . ? O9A K2 O9 17.28(19) . . ? O10A K2 O9 76.7(2) . . ? O11A K2 O12 42.3(2) . . ? O16 K2 O12 93.95(10) . . ? O11 K2 O12 60.63(13) . . ? O8 K2 O12 118.72(13) . . ? O7 K2 O12 59.77(12) . . ? O9A K2 O12 159.7(2) . . ? O10A K2 O12 103.6(2) . . ? O9 K2 O12 167.59(11) . . ? O11A K2 O10 78.3(2) . . ? O16 K2 O10 90.28(10) . . ? O11 K2 O10 59.90(13) . . ? O8 K2 O10 120.09(13) . . ? O7 K2 O10 160.56(11) . . ? O9A K2 O10 41.9(2) . . ? O10A K2 O10 17.64(18) . . ? O9 K2 O10 59.13(13) . . ? O12 K2 O10 120.53(13) . . ? O11A K2 O7A 119.2(3) . . ? O16 K2 O7A 104.5(2) . . ? O11 K2 O7A 137.6(2) . . ? O8 K2 O7A 39.6(2) . . ? O7 K2 O7A 20.70(19) . . ? O9A K2 O7A 114.7(3) . . ? O10A K2 O7A 168.6(3) . . ? O9 K2 O7A 97.6(2) . . ? O12 K2 O7A 79.7(2) . . ? O10 K2 O7A 154.5(2) . . ? O11A K2 O12A 61.5(3) . . ? O16 K2 O12A 98.8(2) . . ? O11 K2 O12A 80.2(2) . . ? O8 K2 O12A 98.6(2) . . ? O7 K2 O12A 39.6(2) . . ? O9A K2 O12A 165.2(3) . . ? O10A K2 O12A 123.4(3) . . ? O9 K2 O12A 154.2(2) . . ? O12 K2 O12A 20.25(18) . . ? O10 K2 O12A 139.6(2) . . ? O7A K2 O12A 59.5(3) . . ? C64 O1 C53 111.5(3) . . ? C64 O1 K1 112.2(2) . . ? C53 O1 K1 115.0(2) . . ? C55 O2 C54 111.8(3) . . ? C55 O2 K1 117.2(2) . . ? C54 O2 K1 118.1(2) . . ? C57 O3 C56 113.1(3) . . ? C57 O3 K1 116.1(2) . . ? C56 O3 K1 110.7(2) . . ? C58 O4 C59 111.8(3) . . ? C58 O4 K1 114.9(2) . . ? C59 O4 K1 115.3(2) . . ? C60 O5 C61 111.8(3) . . ? C60 O5 K1 116.5(2) . . ? C61 O5 K1 110.0(2) . . ? C63 O6 C62 112.0(3) . . ? C63 O6 K1 117.8(2) . . ? C62 O6 K1 117.2(2) . . ? O7A O7 C76A 86.9(10) . . ? O7A O7 C76 151.6(7) . . ? C76A O7 C76 64.7(9) . . ? O7A O7 C65 38.1(6) . . ? C76A O7 C65 48.9(8) . . ? C76 O7 C65 113.6(4) . . ? O7A O7 K2 82.9(6) . . ? C76A O7 K2 142.8(8) . . ? C76 O7 K2 118.6(3) . . ? C65 O7 K2 114.9(4) . . ? O8A O8 C66A 90.3(11) . . ? O8A O8 C66 149.5(8) . . ? C66A O8 C66 59.4(9) . . ? O8A O8 C67 37.1(7) . . ? C66A O8 C67 55.1(8) . . ? C66 O8 C67 112.9(4) . . ? O8A O8 K2 88.2(7) . . ? C66A O8 K2 160.5(8) . . ? C66 O8 K2 119.3(3) . . ? C67 O8 K2 117.3(4) . . ? O9A O9 C68A 96.6(11) . . ? O9A O9 C68 150.1(9) . . ? C68A O9 C68 55.7(8) . . ? O9A O9 C69 39.5(8) . . ? C68A O9 C69 59.1(8) . . ? C68 O9 C69 114.8(4) . . ? O9A O9 K2 80.5(8) . . ? C68A O9 K2 137.9(7) . . ? C68 O9 K2 111.4(3) . . ? C69 O9 K2 116.1(3) . . ? O10A O10 C70A 111.4(14) . . ? O10A O10 C71 50.0(7) . . ? C70A O10 C71 62.3(11) . . ? O10A O10 C70 165.0(8) . . ? C70A O10 C70 54.0(11) . . ? C71 O10 C70 116.1(4) . . ? O10A O10 K2 78.4(7) . . ? C70A O10 K2 146.9(10) . . ? C71 O10 K2 114.0(3) . . ? C70 O10 K2 115.6(3) . . ? O11A O11 C72A 107.6(12) . . ? O11A O11 C73 54.5(7) . . ? C72A O11 C73 53.7(9) . . ? O11A O11 C72 166.5(8) . . ? C72A O11 C72 62.1(10) . . ? C73 O11 C72 115.8(5) . . ? O11A O11 K2 76.5(7) . . ? C72A O11 K2 139.6(9) . . ? C73 O11 K2 111.6(3) . . ? C72 O11 K2 116.9(3) . . ? O12A O12 C74A 88.9(11) . . ? O12A O12 C75 44.0(6) . . ? C74A O12 C75 45.1(9) . . ? O12A O12 C74 157.1(8) . . ? C74A O12 C74 68.2(10) . . ? C75 O12 C74 113.2(5) . . ? O12A O12 K2 82.0(6) . . ? C74A O12 K2 131.5(9) . . ? C75 O12 K2 112.9(3) . . ? C74 O12 K2 113.7(3) . . ? C82 O13 C77 112.9(3) 3_576 . ? C82 O13 K1 124.4(2) 3_576 . ? C77 O13 K1 97.0(2) . . ? C78 O14 C79 113.5(3) . . ? C78 O14 K1 119.0(2) . . ? C79 O14 K1 127.5(2) . . ? C80 O15 C81 112.2(3) . . ? C83 O16 C88 112.8(3) . 3_676 ? C83 O16 K2 134.6(2) . . ? C88 O16 K2 111.1(2) 3_676 . ? C84 O17 C85 114.6(3) . . ? C87 O18 C86 113.4(3) . . ? C1A N1 C3 112.7(10) . . ? C1A N1 C1 129.8(10) . . ? C3 N1 C1 117.2(4) . . ? C1A N1 Ga1A 116.7(10) . . ? C3 N1 Ga1A 130.5(3) . . ? C1 N1 Ga1A 13.8(3) . . ? C1A N1 Ga1 20.0(9) . . ? C3 N1 Ga1 132.6(2) . . ? C1 N1 Ga1 110.2(4) . . ? Ga1A N1 Ga1 96.86(16) . . ? C2 N2 C2A 127.2(11) . . ? C2 N2 C15 116.8(3) . . ? C2A N2 C15 115.6(11) . . ? C2 N2 Ga1 114.7(3) . . ? C2A N2 Ga1 12.6(10) . . ? C15 N2 Ga1 128.2(2) . . ? C2 N2 Ga1A 21.3(2) . . ? C2A N2 Ga1A 106.0(11) . . ? C15 N2 Ga1A 137.2(2) . . ? Ga1 N2 Ga1A 93.69(16) . . ? C27 N3 C29 115.9(3) . . ? C27 N3 C27A 128.5(9) . . ? C29 N3 C27A 115.2(8) . . ? C27 N3 Ga2A 16.0(3) . . ? C29 N3 Ga2A 131.7(2) . . ? C27A N3 Ga2A 112.9(8) . . ? C27 N3 Ga2 111.5(3) . . ? C29 N3 Ga2 132.6(2) . . ? C27A N3 Ga2 18.5(8) . . ? Ga2A N3 Ga2 95.62(14) . . ? C28 N4 C28A 128.9(9) . . ? C28 N4 C41 116.7(3) . . ? C28A N4 C41 114.3(9) . . ? C28 N4 Ga2A 19.9(2) . . ? C28A N4 Ga2A 109.3(9) . . ? C41 N4 Ga2A 135.9(2) . . ? C28 N4 Ga2 113.7(3) . . ? C28A N4 Ga2 15.6(9) . . ? C41 N4 Ga2 129.1(2) . . ? Ga2A N4 Ga2 93.93(14) . . ? C2 C1 N1 118.5(6) . . ? N1 C1A C2A 109.2(18) . . ? C1 C2 N2 113.6(6) . . ? C1A C2A N2 120.8(19) . . ? N1 C3 C8 119.7(3) . . ? N1 C3 C4 120.2(3) . . ? C8 C3 C4 120.0(3) . . ? C5 C4 C3 118.6(3) . . ? C5 C4 C9 120.4(3) . . ? C3 C4 C9 120.9(3) . . ? C6 C5 C4 121.1(4) . . ? C7 C6 C5 120.1(4) . . ? C6 C7 C8 121.4(4) . . ? C7 C8 C3 118.5(3) . . ? C7 C8 C12 121.0(3) . . ? C3 C8 C12 120.5(3) . . ? C4 C9 C11 115.4(3) . . ? C4 C9 C10 110.3(3) . . ? C11 C9 C10 108.5(3) . . ? C14 C12 C8 113.8(3) . . ? C14 C12 C13 109.5(3) . . ? C8 C12 C13 112.5(3) . . ? N2 C15 C20 120.3(3) . . ? N2 C15 C16 119.8(3) . . ? C20 C15 C16 119.9(3) . . ? C17 C16 C15 118.9(3) . . ? C17 C16 C21 121.5(3) . . ? C15 C16 C21 119.6(3) . . ? C18 C17 C16 121.5(4) . . ? C19 C18 C17 119.7(4) . . ? C18 C19 C20 121.1(4) . . ? C19 C20 C15 118.9(3) . . ? C19 C20 C24 120.3(3) . . ? C15 C20 C24 120.7(3) . . ? C16 C21 C22 114.7(4) . . ? C16 C21 C23 109.9(3) . . ? C22 C21 C23 109.5(3) . . ? C20 C24 C26 110.6(3) . . ? C20 C24 C25 113.4(3) . . ? C26 C24 C25 110.3(3) . . ? C28 C27 N3 117.4(6) . . ? C27 C28 N4 114.3(5) . . ? C30 C29 N3 120.8(3) . . ? C30 C29 C34 119.8(3) . . ? N3 C29 C34 119.4(3) . . ? C31 C30 C29 118.7(3) . . ? C31 C30 C35 121.2(3) . . ? C29 C30 C35 120.1(3) . . ? C32 C31 C30 121.4(3) . . ? C33 C32 C31 119.7(3) . . ? C32 C33 C34 121.6(3) . . ? C33 C34 C29 118.4(3) . . ? C33 C34 C38 121.0(3) . . ? C29 C34 C38 120.5(3) . . ? C37 C35 C30 115.0(3) . . ? C37 C35 C36 108.5(3) . . ? C30 C35 C36 110.6(3) . . ? C39 C38 C34 113.1(3) . . ? C39 C38 C40 110.8(4) . . ? C34 C38 C40 113.3(3) . . ? N4 C41 C46 120.8(3) . . ? N4 C41 C42 119.4(3) . . ? C46 C41 C42 119.7(3) . . ? C43 C42 C41 118.3(3) . . ? C43 C42 C47 121.9(3) . . ? C41 C42 C47 119.8(3) . . ? C44 C43 C42 122.0(4) . . ? C43 C44 C45 119.4(3) . . ? C44 C45 C46 121.4(4) . . ? C45 C46 C41 119.0(3) . . ? C45 C46 C50 120.2(3) . . ? C41 C46 C50 120.7(3) . . ? C42 C47 C49 114.1(3) . . ? C42 C47 C48 110.8(3) . . ? C49 C47 C48 109.2(3) . . ? C46 C50 C51 113.7(3) . . ? C46 C50 C52 109.9(3) . . ? C51 C50 C52 110.1(3) . . ? O1 C53 C54 108.0(3) . . ? O2 C54 C53 108.9(3) . . ? O2 C55 C56 109.1(3) . . ? O3 C56 C55 108.7(3) . . ? O3 C57 C58 109.0(3) . . ? O4 C58 C57 108.6(3) . . ? O4 C59 C60 109.7(3) . . ? O5 C60 C59 107.7(3) . . ? O5 C61 C62 107.4(3) . . ? O6 C62 C61 109.4(3) . . ? O6 C63 C64 110.1(3) . . ? O1 C64 C63 108.2(3) . . ? O7A C65 C76A 93.4(11) . . ? O7A C65 O7 44.6(7) . . ? C76A C65 O7 48.9(8) . . ? O7A C65 C66 67.0(9) . . ? C76A C65 C66 158.1(10) . . ? O7 C65 C66 110.5(5) . . ? C66A C66 O7A 127.5(8) . . ? C66A C66 O8 44.7(7) . . ? O7A C66 O8 85.0(5) . . ? C66A C66 C65 157.6(8) . . ? O7A C66 C65 36.3(4) . . ? O8 C66 C65 113.5(4) . . ? O8A C67 C66A 84.2(11) . . ? O8A C67 C68 70.0(9) . . ? C66A C67 C68 152.7(10) . . ? O8A C67 O8 41.2(7) . . ? C66A C67 O8 44.9(7) . . ? C68 C67 O8 110.9(5) . . ? C68A C68 O8A 134.1(9) . . ? C68A C68 C67 159.9(9) . . ? O8A C68 C67 36.7(4) . . ? C68A C68 O9 47.2(7) . . ? O8A C68 O9 93.8(5) . . ? C67 C68 O9 113.2(5) . . ? O9A C69 C68A 78.4(10) . . ? O9A C69 C70 78.3(8) . . ? C68A C69 C70 156.0(9) . . ? O9A C69 O9 33.9(6) . . ? C68A C69 O9 46.0(7) . . ? C70 C69 O9 110.0(5) . . ? C70A C70 C69 152.4(10) . . ? C70A C70 O10 39.5(8) . . ? C69 C70 O10 112.9(4) . . ? C70A C70 O9A 121.1(10) . . ? C69 C70 O9A 38.0(4) . . ? O10 C70 O9A 85.3(5) . . ? O10A C71 C70A 76.4(9) . . ? O10A C71 C72 71.4(7) . . ? C70A C71 C72 147.0(9) . . ? O10A C71 O10 37.5(5) . . ? C70A C71 O10 39.4(7) . . ? C72 C71 O10 108.9(5) . . ? C72A C72 C71 152.0(8) . . ? C72A C72 O11 39.8(6) . . ? C71 C72 O11 112.2(4) . . ? C72A C72 O10A 117.3(8) . . ? C71 C72 O10A 44.2(4) . . ? O11 C72 O10A 87.6(4) . . ? C72A C73 O11A 79.6(9) . . ? C72A C73 O11 41.9(7) . . ? O11A C73 O11 38.1(5) . . ? C72A C73 C74 144.5(10) . . ? O11A C73 C74 69.0(7) . . ? O11 C73 C74 106.6(5) . . ? C72A C73 K2 80.6(8) . . ? O11A C73 K2 36.2(5) . . ? O11 C73 K2 46.3(3) . . ? C74 C73 K2 83.5(3) . . ? C74A C74 O12 43.3(7) . . ? C74A C74 C73 150.0(8) . . ? O12 C74 C73 111.4(4) . . ? C74A C74 O11A 107.4(8) . . ? O12 C74 O11A 84.5(4) . . ? C73 C74 O11A 45.5(4) . . ? O12A C75 C74A 91.5(12) . . ? O12A C75 O12 44.2(6) . . ? C74A C75 O12 47.4(10) . . ? O12A C75 C76 65.5(8) . . ? C74A C75 C76 156.9(12) . . ? O12 C75 C76 109.5(5) . . ? C76A C76 O12A 118.7(8) . . ? C76A C76 O7 45.6(6) . . ? O12A C76 O7 85.6(5) . . ? C76A C76 C75 156.3(7) . . ? O12A C76 C75 40.7(4) . . ? O7 C76 C75 112.2(4) . . ? O13 C77 C78 113.8(3) . . ? O14 C78 C77 108.1(3) . . ? O14 C79 C80 113.8(3) . . ? O15 C80 C79 109.7(3) . . ? O15 C81 C82 107.3(3) . . ? O13 C82 C81 107.1(3) 3_576 . ? O16 C83 C84 109.1(3) . . ? O17 C84 C83 106.9(3) . . ? O17 C85 C86 113.3(4) . . ? O18 C86 C85 109.0(4) . . ? O18 C87 C88 109.5(3) . . ? O16 C88 C87 114.5(3) 3_676 . ? O16 C88 K2 46.11(16) 3_676 3_676 ? C87 C88 K2 138.3(3) . 3_676 ? O11 C72A C73 84.4(12) . . ? O11 C72A C72 78.1(11) . . ? C73 C72A C72 162.5(15) . . ? O11 C72A O11A 34.5(7) . . ? C73 C72A O11A 50.4(7) . . ? C72 C72A O11A 112.1(12) . . ? O11 C72A K2 30.3(7) . . ? C73 C72A K2 80.5(8) . . ? C72 C72A K2 84.5(7) . . ? O11A C72A K2 44.5(6) . . ? C75 C74A O12 87.5(14) . . ? C75 C74A C74 155.6(17) . . ? O12 C74A C74 68.5(10) . . ? C75 C74A O12A 43.7(8) . . ? O12 C74A O12A 43.9(8) . . ? C74 C74A O12A 112.4(13) . . ? O10 C70A C70 86.5(14) . . ? O10 C70A C71 78.2(12) . . ? C70 C70A C71 163.6(17) . . ? O10 C70A O10A 33.0(8) . . ? C70 C70A O10A 119.4(14) . . ? C71 C70A O10A 45.8(7) . . ? O8 C66A C67 80.1(10) . . ? O8 C66A C66 75.9(10) . . ? C67 C66A C66 151.5(13) . . ? O8 C66A O8A 43.1(7) . . ? C67 C66A O8A 38.5(6) . . ? C66 C66A O8A 119.0(13) . . ? O9 C68A C68 77.1(10) . . ? O9 C68A C69 74.9(9) . . ? C68 C68A C69 152.0(14) . . ? O9 C68A O9A 35.4(6) . . ? C68 C68A O9A 111.7(13) . . ? C69 C68A O9A 40.7(6) . . ? O7 C76A C65 82.2(11) . . ? O7 C76A C76 69.7(9) . . ? C65 C76A C76 151.8(13) . . ? O7 C76A O7A 44.4(7) . . ? C65 C76A O7A 37.9(7) . . ? C76 C76A O7A 114.1(11) . . ? O9 O9A C69 106.7(12) . . ? O9 O9A C68A 47.9(8) . . ? C69 O9A C68A 60.9(9) . . ? O9 O9A C70 158.4(11) . . ? C69 O9A C70 63.6(8) . . ? C68A O9A C70 124.2(10) . . ? O9 O9A K2 82.2(8) . . ? C69 O9A K2 153.8(8) . . ? C68A O9A K2 116.9(8) . . ? C70 O9A K2 115.2(6) . . ? C65 O7A O7 97.3(11) . . ? C65 O7A C66 76.7(9) . . ? O7 O7A C66 165.3(9) . . ? C65 O7A C76A 48.7(9) . . ? O7 O7A C76A 48.7(7) . . ? C66 O7A C76A 124.7(10) . . ? C65 O7A K2 147.7(9) . . ? O7 O7A K2 76.4(6) . . ? C66 O7A K2 115.8(6) . . ? C76A O7A K2 115.9(8) . . ? C67 O8A O8 101.7(12) . . ? C67 O8A C68 73.3(10) . . ? O8 O8A C68 172.4(10) . . ? C67 O8A C66A 57.3(9) . . ? O8 O8A C66A 46.7(8) . . ? C68 O8A C66A 129.8(12) . . ? C67 O8A K2 144.0(9) . . ? O8 O8A K2 72.2(7) . . ? C68 O8A K2 108.3(6) . . ? C66A O8A K2 116.3(9) . . ? O11 O11A C73 87.4(9) . . ? O11 O11A C72A 37.9(8) . . ? C73 O11A C72A 50.0(7) . . ? O11 O11A C74 151.2(10) . . ? C73 O11A C74 65.5(6) . . ? C72A O11A C74 113.6(9) . . ? O11 O11A K2 84.8(7) . . ? C73 O11A K2 128.9(7) . . ? C72A O11A K2 112.6(8) . . ? C74 O11A K2 119.2(5) . . ? C75 O12A O12 91.8(10) . . ? C75 O12A C76 73.8(8) . . ? O12 O12A C76 164.7(11) . . ? C75 O12A C74A 44.8(8) . . ? O12 O12A C74A 47.1(8) . . ? C76 O12A C74A 118.6(11) . . ? C75 O12A K2 134.7(8) . . ? O12 O12A K2 77.8(6) . . ? C76 O12A K2 116.1(6) . . ? C74A O12A K2 109.7(8) . . ? O10 O10A C71 92.5(9) . . ? O10 O10A C70A 35.5(8) . . ? C71 O10A C70A 57.8(8) . . ? O10 O10A C72 156.9(10) . . ? C71 O10A C72 64.4(7) . . ? C70A O10A C72 121.7(9) . . ? O10 O10A K2 84.0(7) . . ? C71 O10A K2 135.6(7) . . ? C70A O10A K2 113.5(8) . . ? C72 O10A K2 111.8(5) . . ? C28A C27A N3 113.0(15) . . ? N4 C28A C27A 117.1(16) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.063 _refine_diff_density_min -0.419 _refine_diff_density_rms 0.072 data_compound12 _database_code_CSD 189508 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H104 Ga2 K2 N8' _chemical_formula_weight 1203.20 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' 'K' 'K' 0.2009 0.2494 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.615(3) _cell_length_b 12.650(3) _cell_length_c 12.727(3) _cell_angle_alpha 82.22(3) _cell_angle_beta 62.52(3) _cell_angle_gamma 66.93(3) _cell_volume 1655.1(6) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.207 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 644 _exptl_absorpt_coefficient_mu 0.982 _exptl_absorpt_correction_type 'Sortav (Blessing)' _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 Kappa CCD' _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 18217 _diffrn_reflns_av_R_equivalents 0.0895 _diffrn_reflns_av_sigmaI/netI 0.0785 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5715 _reflns_number_gt 4578 _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^)+(0.0691P)^2^+3.7586P] 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 5715 _refine_ls_number_parameters 355 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0863 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.1710 _refine_ls_wR_factor_gt 0.1593 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.000 _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 0.12320(5) 0.42427(4) -0.00727(4) 0.03342(19) Uani 1 1 d . . . K1 K -0.14247(10) 0.35466(9) 0.19929(9) 0.0392(3) Uani 1 1 d . . . N1 N 0.2539(3) 0.3880(3) -0.1789(3) 0.0271(8) Uani 1 1 d . . . N2 N 0.2235(4) 0.5171(3) -0.0128(3) 0.0329(9) Uani 1 1 d . . . N3 N -0.3069(6) 0.2309(5) 0.3714(5) 0.0700(15) Uani 1 1 d . . . N4 N -0.0398(6) 0.1730(6) 0.3487(6) 0.0824(18) Uani 1 1 d . . . C1 C 0.3542(4) 0.4237(4) -0.2025(4) 0.0306(10) Uani 1 1 d . . . H1 H 0.4288 0.4033 -0.2741 0.037 Uiso 1 1 calc R . . C2 C 0.3381(5) 0.4892(4) -0.1169(4) 0.0341(10) Uani 1 1 d . . . H2 H 0.4019 0.5149 -0.1273 0.041 Uiso 1 1 calc R . . C3 C 0.2855(4) 0.2956(4) -0.2538(4) 0.0304(10) Uani 1 1 d . . . C4 C 0.3682(5) 0.1841(4) -0.2475(4) 0.0370(11) Uani 1 1 d . . . C5 C 0.3994(5) 0.0955(4) -0.3248(5) 0.0459(13) Uani 1 1 d . . . H5 H 0.4536 0.0215 -0.3207 0.055 Uiso 1 1 calc R . . C6 C 0.3517(5) 0.1157(5) -0.4065(5) 0.0505(14) Uani 1 1 d . . . H6 H 0.3751 0.0563 -0.4581 0.061 Uiso 1 1 calc R . . C7 C 0.2694(5) 0.2241(5) -0.4111(5) 0.0481(14) Uani 1 1 d . . . H7 H 0.2362 0.2372 -0.4656 0.058 Uiso 1 1 calc R . . C8 C 0.2342(5) 0.3152(4) -0.3357(4) 0.0373(11) Uani 1 1 d . . . C9 C 0.4205(5) 0.1557(4) -0.1570(5) 0.0447(12) Uani 1 1 d . . . H9 H 0.3901 0.2277 -0.1127 0.054 Uiso 1 1 calc R . . C10 C 0.3677(7) 0.0733(6) -0.0675(6) 0.0715(19) Uani 1 1 d . . . H10A H 0.2753 0.1041 -0.0336 0.107 Uiso 1 1 calc R . . H10B H 0.3937 0.0645 -0.0058 0.107 Uiso 1 1 calc R . . H10C H 0.4011 -0.0003 -0.1071 0.107 Uiso 1 1 calc R . . C11 C 0.5681(6) 0.1076(5) -0.2142(5) 0.0569(15) Uani 1 1 d . . . H11A H 0.6012 0.0368 -0.2586 0.085 Uiso 1 1 calc R . . H11B H 0.5962 0.0935 -0.1534 0.085 Uiso 1 1 calc R . . H11C H 0.5994 0.1622 -0.2663 0.085 Uiso 1 1 calc R . . C12 C 0.1494(5) 0.4361(5) -0.3465(4) 0.0441(13) Uani 1 1 d . . . H12 H 0.0993 0.4756 -0.2676 0.053 Uiso 1 1 calc R . . C13 C 0.0546(6) 0.4418(6) -0.3921(6) 0.072(2) Uani 1 1 d . . . H13A H 0.1014 0.4112 -0.4728 0.107 Uiso 1 1 calc R . . H13B H -0.0015 0.5203 -0.3882 0.107 Uiso 1 1 calc R . . H13C H 0.0044 0.3972 -0.3439 0.107 Uiso 1 1 calc R . . C14 C 0.2369(6) 0.5003(5) -0.4278(5) 0.0581(16) Uani 1 1 d . . . H14A H 0.2954 0.4969 -0.3979 0.087 Uiso 1 1 calc R . . H14B H 0.1849 0.5793 -0.4296 0.087 Uiso 1 1 calc R . . H14C H 0.2849 0.4649 -0.5066 0.087 Uiso 1 1 calc R . . C15 C 0.2269(5) 0.5570(4) 0.0849(4) 0.0374(11) Uani 1 1 d . . . C16 C 0.1599(6) 0.6746(5) 0.1236(5) 0.0520(14) Uani 1 1 d . . . C17 C 0.1726(7) 0.7123(5) 0.2142(6) 0.0668(18) Uani 1 1 d . . . H17 H 0.1303 0.7896 0.2398 0.080 Uiso 1 1 calc R . . C18 C 0.2460(7) 0.6378(6) 0.2662(5) 0.0640(17) Uani 1 1 d . . . H18 H 0.2552 0.6654 0.3244 0.077 Uiso 1 1 calc R . . C19 C 0.3053(6) 0.5231(5) 0.2318(5) 0.0509(14) Uani 1 1 d . . . H19 H 0.3525 0.4727 0.2690 0.061 Uiso 1 1 calc R . . C20 C 0.2962(5) 0.4808(4) 0.1424(4) 0.0402(12) Uani 1 1 d . . . C21 C 0.0759(8) 0.7576(5) 0.0662(5) 0.0666(19) Uani 1 1 d . . . H21 H 0.0451 0.7128 0.0377 0.080 Uiso 1 1 calc R . . C22 C -0.0411(7) 0.8575(6) 0.1479(7) 0.080(2) Uani 1 1 d . . . H22A H -0.0128 0.9062 0.1715 0.120 Uiso 1 1 calc R . . H22B H -0.0938 0.8278 0.2169 0.120 Uiso 1 1 calc R . . H22C H -0.0904 0.9011 0.1066 0.120 Uiso 1 1 calc R . . C23 C 0.1624(7) 0.8010(6) -0.0380(7) 0.0731(19) Uani 1 1 d . . . H23A H 0.1841 0.8539 -0.0118 0.110 Uiso 1 1 calc R . . H23B H 0.1196 0.8397 -0.0861 0.110 Uiso 1 1 calc R . . H23C H 0.2396 0.7376 -0.0838 0.110 Uiso 1 1 calc R . . C24 C 0.3621(5) 0.3521(4) 0.1090(5) 0.0438(12) Uani 1 1 d . . . H24 H 0.3385 0.3377 0.0505 0.053 Uiso 1 1 calc R . . C25 C 0.3146(8) 0.2817(6) 0.2156(7) 0.085(2) Uani 1 1 d . . . H25A H 0.3375 0.2930 0.2743 0.128 Uiso 1 1 calc R . . H25B H 0.3539 0.2016 0.1906 0.128 Uiso 1 1 calc R . . H25C H 0.2227 0.3062 0.2490 0.128 Uiso 1 1 calc R . . C26 C 0.5067(6) 0.3107(5) 0.0525(6) 0.0604(16) Uani 1 1 d . . . H26A H 0.5357 0.3564 -0.0133 0.091 Uiso 1 1 calc R . . H26B H 0.5433 0.2315 0.0251 0.091 Uiso 1 1 calc R . . H26C H 0.5335 0.3178 0.1098 0.091 Uiso 1 1 calc R . . C27 C -0.3772(9) 0.2014(9) 0.3236(8) 0.100(3) Uani 1 1 d . . . H27A H -0.3186 0.1395 0.2642 0.150 Uiso 1 1 calc R . . H27B H -0.4171 0.2673 0.2888 0.150 Uiso 1 1 calc R . . H27C H -0.4423 0.1779 0.3863 0.150 Uiso 1 1 calc R . . C28 C -0.3978(9) 0.3117(8) 0.4682(8) 0.105(3) Uani 1 1 d . . . H28A H -0.4473 0.2751 0.5320 0.158 Uiso 1 1 calc R . . H28B H -0.4543 0.3741 0.4439 0.158 Uiso 1 1 calc R . . H28C H -0.3536 0.3408 0.4942 0.158 Uiso 1 1 calc R . . C29 C -0.2347(9) 0.1294(8) 0.4078(9) 0.095(2) Uani 1 1 d U . . H29A H -0.1976 0.0687 0.3477 0.114 Uiso 1 1 calc R . . H29B H -0.2950 0.1082 0.4799 0.114 Uiso 1 1 calc R . . C30 C -0.1311(9) 0.1285(8) 0.4302(9) 0.100(3) Uani 1 1 d U . . H30A H -0.1709 0.1701 0.5058 0.120 Uiso 1 1 calc R . . H30B H -0.0842 0.0492 0.4400 0.120 Uiso 1 1 calc R . . C31 C 0.0543(8) 0.1008(7) 0.2489(8) 0.100(3) Uani 1 1 d . . . H31A H 0.0888 0.0248 0.2728 0.151 Uiso 1 1 calc R . . H31B H 0.1222 0.1295 0.2060 0.151 Uiso 1 1 calc R . . H33 H 0.0170 0.0982 0.1989 0.151 Uiso 1 1 calc R . . C32 C 0.0258(9) 0.1958(9) 0.4083(9) 0.106(3) Uani 1 1 d . . . H32A H 0.0806 0.1241 0.4235 0.159 Uiso 1 1 calc R . . H32B H -0.0372 0.2392 0.4820 0.159 Uiso 1 1 calc R . . H32C H 0.0769 0.2389 0.3583 0.159 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 0.0351(3) 0.0347(3) 0.0277(3) -0.0012(2) -0.0118(2) -0.0122(2) K1 0.0383(6) 0.0341(6) 0.0380(6) 0.0039(4) -0.0140(5) -0.0109(5) N1 0.032(2) 0.0256(19) 0.0245(18) 0.0003(14) -0.0143(16) -0.0085(16) N2 0.038(2) 0.034(2) 0.029(2) -0.0016(16) -0.0167(18) -0.0123(18) N3 0.080(4) 0.062(3) 0.071(4) 0.002(3) -0.037(3) -0.026(3) N4 0.065(4) 0.081(4) 0.102(5) 0.017(4) -0.043(4) -0.025(3) C1 0.026(2) 0.032(2) 0.026(2) 0.0001(18) -0.0073(19) -0.0073(19) C2 0.036(3) 0.033(2) 0.036(3) 0.003(2) -0.018(2) -0.014(2) C3 0.029(2) 0.031(2) 0.024(2) -0.0017(18) -0.0058(19) -0.0097(19) C4 0.035(3) 0.035(3) 0.035(3) -0.002(2) -0.011(2) -0.011(2) C5 0.038(3) 0.029(3) 0.054(3) -0.011(2) -0.010(3) -0.004(2) C6 0.040(3) 0.049(3) 0.053(3) -0.023(3) -0.009(3) -0.014(3) C7 0.039(3) 0.064(4) 0.041(3) -0.016(3) -0.014(2) -0.016(3) C8 0.035(3) 0.047(3) 0.027(2) -0.006(2) -0.010(2) -0.015(2) C9 0.044(3) 0.035(3) 0.044(3) 0.002(2) -0.021(2) -0.001(2) C10 0.061(4) 0.076(5) 0.063(4) 0.028(3) -0.028(3) -0.020(4) C11 0.048(3) 0.059(4) 0.058(4) 0.005(3) -0.027(3) -0.012(3) C12 0.037(3) 0.055(3) 0.031(3) -0.007(2) -0.018(2) -0.002(2) C13 0.060(4) 0.087(5) 0.059(4) -0.019(3) -0.041(3) 0.006(4) C14 0.062(4) 0.055(4) 0.036(3) 0.008(3) -0.023(3) -0.003(3) C15 0.048(3) 0.038(3) 0.033(2) -0.002(2) -0.021(2) -0.017(2) C16 0.075(4) 0.041(3) 0.039(3) -0.006(2) -0.030(3) -0.014(3) C17 0.103(5) 0.049(4) 0.056(4) -0.012(3) -0.043(4) -0.021(4) C18 0.088(5) 0.073(4) 0.047(3) -0.007(3) -0.038(3) -0.033(4) C19 0.060(4) 0.062(4) 0.040(3) 0.004(3) -0.030(3) -0.024(3) C20 0.046(3) 0.045(3) 0.036(3) 0.004(2) -0.021(2) -0.020(2) C21 0.114(6) 0.030(3) 0.045(3) -0.005(2) -0.038(4) -0.012(3) C22 0.068(5) 0.066(5) 0.078(5) -0.014(4) -0.017(4) -0.011(4) C23 0.062(4) 0.070(4) 0.086(5) -0.011(4) -0.035(4) -0.015(4) C24 0.051(3) 0.044(3) 0.050(3) 0.008(2) -0.035(3) -0.017(3) C25 0.081(5) 0.064(5) 0.080(5) 0.026(4) -0.016(4) -0.028(4) C26 0.058(4) 0.051(4) 0.068(4) -0.002(3) -0.030(3) -0.013(3) C27 0.088(6) 0.131(8) 0.106(7) 0.021(6) -0.053(5) -0.059(6) C28 0.083(6) 0.091(6) 0.096(6) -0.019(5) 0.007(5) -0.037(5) C29 0.093(4) 0.102(4) 0.100(4) 0.024(3) -0.052(3) -0.042(3) C30 0.098(4) 0.092(4) 0.119(5) 0.028(4) -0.050(4) -0.049(4) C31 0.077(6) 0.077(6) 0.114(7) -0.004(5) -0.038(5) 0.002(4) C32 0.096(7) 0.115(7) 0.126(8) 0.024(6) -0.068(6) -0.042(6) _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 N2 2.011(4) . ? Ga1 N1 2.014(4) . ? Ga1 Ga1 2.8746(15) 2_565 ? Ga1 K1 3.4620(16) 2_565 ? Ga1 K1 3.5318(18) . ? K1 N3 2.996(6) . ? K1 C1 3.009(5) 2_565 ? K1 C2 3.016(5) 2_565 ? K1 N1 3.027(4) 2_565 ? K1 N2 3.034(4) 2_565 ? K1 N4 3.055(7) . ? K1 Ga1 3.4620(16) 2_565 ? N1 C1 1.399(6) . ? N1 C3 1.420(5) . ? N1 K1 3.027(4) 2_565 ? N2 C2 1.389(6) . ? N2 C15 1.428(6) . ? N2 K1 3.034(4) 2_565 ? N3 C28 1.412(9) . ? N3 C29 1.416(10) . ? N3 C27 1.455(9) . ? N4 C31 1.389(10) . ? N4 C30 1.402(10) . ? N4 C32 1.472(10) . ? C1 C2 1.350(6) . ? C1 K1 3.009(5) 2_565 ? C2 K1 3.016(5) 2_565 ? C3 C4 1.407(7) . ? C3 C8 1.412(7) . ? C4 C5 1.405(7) . ? C4 C9 1.515(7) . ? C5 C6 1.376(8) . ? C6 C7 1.371(8) . ? C7 C8 1.398(7) . ? C8 C12 1.517(7) . ? C9 C11 1.532(8) . ? C9 C10 1.533(8) . ? C12 C13 1.526(8) . ? C12 C14 1.539(8) . ? C15 C20 1.403(7) . ? C15 C16 1.413(7) . ? C16 C17 1.400(8) . ? C16 C21 1.547(9) . ? C17 C18 1.377(9) . ? C18 C19 1.370(9) . ? C19 C20 1.389(7) . ? C20 C24 1.523(7) . ? C21 C23 1.479(10) . ? C21 C22 1.528(9) . ? C24 C26 1.504(8) . ? C24 C25 1.528(8) . ? C29 C30 1.456(11) . ? 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 N2 Ga1 N1 82.05(15) . . ? N2 Ga1 Ga1 109.79(12) . 2_565 ? N1 Ga1 Ga1 109.32(11) . 2_565 ? N2 Ga1 K1 60.66(11) . 2_565 ? N1 Ga1 K1 60.44(11) . 2_565 ? Ga1 Ga1 K1 67.01(4) 2_565 2_565 ? N2 Ga1 K1 139.09(11) . . ? N1 Ga1 K1 138.84(10) . . ? Ga1 Ga1 K1 64.47(4) 2_565 . ? K1 Ga1 K1 131.47(3) 2_565 . ? N3 K1 C1 98.39(15) . 2_565 ? N3 K1 C2 96.64(15) . 2_565 ? C1 K1 C2 25.90(12) 2_565 2_565 ? N3 K1 N1 121.11(14) . 2_565 ? C1 K1 N1 26.79(11) 2_565 2_565 ? C2 K1 N1 45.69(11) 2_565 2_565 ? N3 K1 N2 116.73(14) . 2_565 ? C1 K1 N2 45.73(11) 2_565 2_565 ? C2 K1 N2 26.54(12) 2_565 2_565 ? N1 K1 N2 51.68(10) 2_565 2_565 ? N3 K1 N4 60.15(17) . . ? C1 K1 N4 145.83(16) 2_565 . ? C2 K1 N4 156.68(16) 2_565 . ? N1 K1 N4 142.60(15) 2_565 . ? N2 K1 N4 165.68(16) 2_565 . ? N3 K1 Ga1 147.28(12) . 2_565 ? C1 K1 Ga1 51.15(9) 2_565 2_565 ? C2 K1 Ga1 50.92(9) 2_565 2_565 ? N1 K1 Ga1 35.36(7) 2_565 2_565 ? N2 K1 Ga1 35.29(7) 2_565 2_565 ? N4 K1 Ga1 151.85(12) . 2_565 ? N3 K1 Ga1 163.38(12) . . ? C1 K1 Ga1 98.22(10) 2_565 . ? C2 K1 Ga1 98.03(10) 2_565 . ? N1 K1 Ga1 75.14(8) 2_565 . ? N2 K1 Ga1 75.24(8) 2_565 . ? N4 K1 Ga1 105.25(13) . . ? Ga1 K1 Ga1 48.53(3) 2_565 . ? C1 N1 C3 116.0(4) . . ? C1 N1 Ga1 110.4(3) . . ? C3 N1 Ga1 127.1(3) . . ? C1 N1 K1 75.9(2) . 2_565 ? C3 N1 K1 130.2(3) . 2_565 ? Ga1 N1 K1 84.20(12) . 2_565 ? C2 N2 C15 114.7(4) . . ? C2 N2 Ga1 110.4(3) . . ? C15 N2 Ga1 127.5(3) . . ? C2 N2 K1 76.0(2) . 2_565 ? C15 N2 K1 131.5(3) . 2_565 ? Ga1 N2 K1 84.05(12) . 2_565 ? C28 N3 C29 111.2(7) . . ? C28 N3 C27 107.8(7) . . ? C29 N3 C27 108.7(6) . . ? C28 N3 K1 104.4(4) . . ? C29 N3 K1 112.4(5) . . ? C27 N3 K1 112.1(5) . . ? C31 N4 C30 114.5(8) . . ? C31 N4 C32 107.6(7) . . ? C30 N4 C32 108.8(7) . . ? C31 N4 K1 91.8(5) . . ? C30 N4 K1 112.9(5) . . ? C32 N4 K1 120.3(5) . . ? C2 C1 N1 117.2(4) . . ? C2 C1 K1 77.3(3) . 2_565 ? N1 C1 K1 77.3(2) . 2_565 ? C1 C2 N2 118.0(4) . . ? C1 C2 K1 76.8(3) . 2_565 ? N2 C2 K1 77.5(3) . 2_565 ? C4 C3 C8 119.3(4) . . ? C4 C3 N1 120.6(4) . . ? C8 C3 N1 120.1(4) . . ? C5 C4 C3 118.9(5) . . ? C5 C4 C9 119.1(5) . . ? C3 C4 C9 122.0(4) . . ? C6 C5 C4 121.5(5) . . ? C7 C6 C5 119.5(5) . . ? C6 C7 C8 121.4(5) . . ? C7 C8 C3 119.4(5) . . ? C7 C8 C12 120.9(5) . . ? C3 C8 C12 119.7(4) . . ? C4 C9 C11 112.8(4) . . ? C4 C9 C10 111.3(5) . . ? C11 C9 C10 110.6(5) . . ? C8 C12 C13 114.6(5) . . ? C8 C12 C14 108.4(4) . . ? C13 C12 C14 110.2(5) . . ? C20 C15 C16 119.9(4) . . ? C20 C15 N2 120.6(4) . . ? C16 C15 N2 119.5(4) . . ? C17 C16 C15 118.0(5) . . ? C17 C16 C21 121.9(5) . . ? C15 C16 C21 120.2(4) . . ? C18 C17 C16 121.7(6) . . ? C19 C18 C17 119.8(5) . . ? C18 C19 C20 121.1(5) . . ? C19 C20 C15 119.5(5) . . ? C19 C20 C24 119.0(5) . . ? C15 C20 C24 121.5(4) . . ? C23 C21 C22 110.6(5) . . ? C23 C21 C16 106.5(6) . . ? C22 C21 C16 115.3(5) . . ? C26 C24 C20 113.0(5) . . ? C26 C24 C25 109.9(5) . . ? C20 C24 C25 111.6(5) . . ? N3 C29 C30 119.8(8) . . ? N4 C30 C29 120.5(8) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.628 (near Ga1) _refine_diff_density_min -0.556 _refine_diff_density_rms 0.085 data_compound11 _database_code_CSD 189509 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H102 Ga2 K2 N4 O3' _chemical_formula_weight 1193.14 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.559(3) _cell_length_b 12.623(3) _cell_length_c 12.931(3) _cell_angle_alpha 67.45(3) _cell_angle_beta 77.15(3) _cell_angle_gamma 62.55(3) _cell_volume 1677.5(6) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.181 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 638 _exptl_absorpt_coefficient_mu 0.970 _exptl_absorpt_correction_type 'Sortav (Blessing)' _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.84 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 Kappa CCD' _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 26246 _diffrn_reflns_av_R_equivalents 0.0734 _diffrn_reflns_av_sigmaI/netI 0.0544 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 25.34 _reflns_number_total 6082 _reflns_number_gt 5028 _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^)+(0.0347P)^2^+1.6322P] 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 6082 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1003 _refine_ls_wR_factor_gt 0.0942 _refine_ls_goodness_of_fit_ref 1.032 _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 -0.02989(3) -0.08530(3) 0.59949(3) 0.02401(11) Uani 1 1 d . . . K1 K 0.17686(5) 0.00683(6) 0.62640(5) 0.02903(16) Uani 1 1 d . . . O1 O 0.28925(18) -0.06970(19) 0.81576(17) 0.0335(5) Uani 1 1 d . . . O2 O 0.5000 -0.5000 1.0000 0.0645(11) Uani 1 2 d S . . N1 N -0.03433(19) -0.22011(19) 0.55691(19) 0.0235(5) Uani 1 1 d . . . N2 N -0.20869(18) -0.03104(19) 0.61632(19) 0.0225(5) Uani 1 1 d . . . C1 C -0.1474(2) -0.2234(3) 0.5848(2) 0.0256(6) Uani 1 1 d . . . H1 H -0.1602 -0.2895 0.5827 0.031 Uiso 1 1 calc R . . C2 C -0.2373(2) -0.1257(2) 0.6151(2) 0.0250(6) Uani 1 1 d . . . H2 H -0.3147 -0.1216 0.6343 0.030 Uiso 1 1 calc R . . C3 C 0.0642(2) -0.3379(2) 0.5548(2) 0.0246(6) Uani 1 1 d . . . C4 C 0.1194(2) -0.3544(3) 0.4515(2) 0.0270(6) Uani 1 1 d . . . C5 C 0.2108(3) -0.4725(3) 0.4517(3) 0.0335(7) Uani 1 1 d . . . H5 H 0.2474 -0.4851 0.3840 0.040 Uiso 1 1 calc R . . C6 C 0.2476(3) -0.5708(3) 0.5509(3) 0.0354(7) Uani 1 1 d . . . H6 H 0.3067 -0.6494 0.5494 0.042 Uiso 1 1 calc R . . C7 C 0.1967(3) -0.5521(3) 0.6515(3) 0.0343(7) Uani 1 1 d . . . H7 H 0.2237 -0.6179 0.7179 0.041 Uiso 1 1 calc R . . C8 C 0.1050(2) -0.4361(3) 0.6563(2) 0.0285(6) Uani 1 1 d . . . C9 C 0.0762(3) -0.2485(3) 0.3420(2) 0.0306(7) Uani 1 1 d . . . H9 H 0.0482 -0.1685 0.3561 0.037 Uiso 1 1 calc R . . C10 C -0.0315(3) -0.2505(3) 0.3072(3) 0.0395(8) Uani 1 1 d . . . H10A H -0.0057 -0.3257 0.2885 0.059 Uiso 1 1 calc R . . H10B H -0.0649 -0.1778 0.2432 0.059 Uiso 1 1 calc R . . H10C H -0.0913 -0.2495 0.3682 0.059 Uiso 1 1 calc R . . C11 C 0.1726(3) -0.2509(3) 0.2458(3) 0.0412(8) Uani 1 1 d . . . H11A H 0.2422 -0.2560 0.2702 0.062 Uiso 1 1 calc R . . H11B H 0.1418 -0.1753 0.1833 0.062 Uiso 1 1 calc R . . H11C H 0.1944 -0.3230 0.2236 0.062 Uiso 1 1 calc R . . C12 C 0.0542(3) -0.4182(3) 0.7689(3) 0.0349(7) Uani 1 1 d . . . H12 H -0.0069 -0.3312 0.7546 0.042 Uiso 1 1 calc R . . C13 C -0.0077(3) -0.5047(4) 0.8380(3) 0.0526(9) Uani 1 1 d . . . H13A H -0.0697 -0.4910 0.7961 0.079 Uiso 1 1 calc R . . H13B H -0.0425 -0.4866 0.9066 0.079 Uiso 1 1 calc R . . H13C H 0.0502 -0.5911 0.8548 0.079 Uiso 1 1 calc R . . C14 C 0.1509(3) -0.4340(3) 0.8344(3) 0.0497(9) Uani 1 1 d . . . H14A H 0.2116 -0.5191 0.8513 0.075 Uiso 1 1 calc R . . H14B H 0.1152 -0.4161 0.9030 0.075 Uiso 1 1 calc R . . H14C H 0.1867 -0.3766 0.7901 0.075 Uiso 1 1 calc R . . C15 C -0.2947(2) 0.0529(2) 0.6743(2) 0.0233(6) Uani 1 1 d . . . C16 C -0.3639(2) 0.1799(2) 0.6131(2) 0.0242(6) Uani 1 1 d . . . C17 C -0.4482(2) 0.2595(3) 0.6708(3) 0.0280(6) Uani 1 1 d . . . H17 H -0.4936 0.3431 0.6309 0.034 Uiso 1 1 calc R . . C18 C -0.4662(2) 0.2174(3) 0.7861(3) 0.0316(7) Uani 1 1 d . . . H18 H -0.5239 0.2717 0.8232 0.038 Uiso 1 1 calc R . . C19 C -0.3972(3) 0.0933(3) 0.8458(3) 0.0313(7) Uani 1 1 d . . . H19 H -0.4091 0.0648 0.9234 0.038 Uiso 1 1 calc R . . C20 C -0.3104(2) 0.0102(3) 0.7919(2) 0.0283(6) Uani 1 1 d . . . C21 C -0.3514(2) 0.2251(2) 0.4857(2) 0.0269(6) Uani 1 1 d . . . H21 H -0.2666 0.1829 0.4634 0.032 Uiso 1 1 calc R . . C22 C -0.4239(2) 0.1856(3) 0.4381(3) 0.0319(7) Uani 1 1 d . . . H22A H -0.4020 0.0966 0.4729 0.048 Uiso 1 1 calc R . . H22B H -0.4068 0.2041 0.3586 0.048 Uiso 1 1 calc R . . H22C H -0.5082 0.2312 0.4530 0.048 Uiso 1 1 calc R . . C23 C -0.3893(3) 0.3681(3) 0.4318(3) 0.0366(7) Uani 1 1 d . . . H23A H -0.4742 0.4118 0.4458 0.055 Uiso 1 1 calc R . . H23B H -0.3706 0.3880 0.3524 0.055 Uiso 1 1 calc R . . H23C H -0.3467 0.3939 0.4636 0.055 Uiso 1 1 calc R . . C24 C -0.2315(3) -0.1230(3) 0.8625(3) 0.0354(7) Uani 1 1 d . . . H24 H -0.1832 -0.1702 0.8108 0.042 Uiso 1 1 calc R . . C25 C -0.3029(3) -0.1934(3) 0.9424(4) 0.0650(12) Uani 1 1 d . . . H25A H -0.2489 -0.2772 0.9823 0.098 Uiso 1 1 calc R . . H25B H -0.3545 -0.1978 0.9008 0.098 Uiso 1 1 calc R . . H25C H -0.3508 -0.1498 0.9947 0.098 Uiso 1 1 calc R . . C26 C -0.1458(4) -0.1206(4) 0.9258(4) 0.0744(14) Uani 1 1 d . . . H26A H -0.1903 -0.0794 0.9805 0.112 Uiso 1 1 calc R . . H26B H -0.1011 -0.0753 0.8743 0.112 Uiso 1 1 calc R . . H26C H -0.0913 -0.2054 0.9628 0.112 Uiso 1 1 calc R . . C27 C 0.3912(3) 0.0598(3) 0.7023(3) 0.0488(9) Uani 1 1 d . . . H27A H 0.4030 0.0311 0.6401 0.073 Uiso 1 1 calc R . . H27B H 0.4568 0.0791 0.7021 0.073 Uiso 1 1 calc R . . H27C H 0.3173 0.1341 0.6960 0.073 Uiso 1 1 calc R . . C28 C 0.3861(4) -0.0390(5) 0.8070(3) 0.0673(12) Uani 1 1 d . . . H28A H 0.4606 -0.1142 0.8122 0.081 Uiso 1 1 calc R . . H28B H 0.3792 -0.0113 0.8695 0.081 Uiso 1 1 calc R . . C29 C 0.2765(4) -0.1605(4) 0.9178(3) 0.0607(11) Uani 1 1 d . . . H29A H 0.2718 -0.1328 0.9797 0.073 Uiso 1 1 calc R . . H29B H 0.3470 -0.2398 0.9257 0.073 Uiso 1 1 calc R . . C30 C 0.1708(5) -0.1803(5) 0.9237(4) 0.0855(17) Uani 1 1 d . . . H30A H 0.1004 -0.1037 0.9221 0.128 Uiso 1 1 calc R . . H30B H 0.1681 -0.2461 0.9920 0.128 Uiso 1 1 calc R . . H30C H 0.1735 -0.2043 0.8608 0.128 Uiso 1 1 calc R . . C31 C 0.3749(6) -0.5701(5) 1.1479(5) 0.106(2) Uani 1 1 d . . . H31A H 0.3188 -0.6080 1.1703 0.160 Uiso 1 1 calc R A 1 H31B H 0.3367 -0.4884 1.1571 0.160 Uiso 1 1 calc R A 1 H31C H 0.4430 -0.6226 1.1937 0.160 Uiso 1 1 calc R A 1 C32 C 0.4161(8) -0.5568(9) 1.0267(8) 0.074(3) Uani 0.50 1 d P B 1 H32A H 0.4549 -0.6387 1.0160 0.088 Uiso 0.50 1 calc PR B 1 H32B H 0.3484 -0.5034 0.9791 0.088 Uiso 0.50 1 calc PR B 1 C32A C 0.4575(8) -0.5118(9) 1.1212(8) 0.073(3) Uani 0.50 1 d P B 2 H32C H 0.5247 -0.5638 1.1693 0.087 Uiso 0.50 1 calc PR B 2 H32D H 0.4174 -0.4293 1.1308 0.087 Uiso 0.50 1 calc PR B 2 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 0.01962(16) 0.02155(16) 0.02745(18) -0.00868(13) -0.00029(12) -0.00570(12) K1 0.0256(3) 0.0302(3) 0.0283(4) -0.0081(3) -0.0044(3) -0.0091(3) O1 0.0355(11) 0.0381(11) 0.0287(11) -0.0058(9) -0.0069(9) -0.0185(9) O2 0.059(2) 0.063(2) 0.068(3) -0.024(2) -0.012(2) -0.017(2) N1 0.0193(11) 0.0194(11) 0.0283(13) -0.0096(10) 0.0022(10) -0.0053(9) N2 0.0186(11) 0.0208(11) 0.0265(13) -0.0097(10) 0.0016(9) -0.0065(9) C1 0.0239(14) 0.0239(14) 0.0291(16) -0.0076(12) -0.0005(12) -0.0112(11) C2 0.0196(13) 0.0249(14) 0.0291(15) -0.0082(12) 0.0031(11) -0.0106(11) C3 0.0195(13) 0.0191(13) 0.0333(16) -0.0093(12) -0.0009(12) -0.0060(11) C4 0.0216(14) 0.0278(14) 0.0338(17) -0.0141(13) 0.0013(12) -0.0100(12) C5 0.0288(15) 0.0305(16) 0.0402(18) -0.0189(14) 0.0047(13) -0.0084(13) C6 0.0259(15) 0.0215(14) 0.051(2) -0.0151(14) 0.0021(14) -0.0029(12) C7 0.0290(15) 0.0206(14) 0.0419(19) -0.0032(13) -0.0047(14) -0.0055(12) C8 0.0235(14) 0.0241(14) 0.0320(16) -0.0074(12) 0.0025(12) -0.0082(12) C9 0.0292(15) 0.0313(15) 0.0304(16) -0.0139(13) 0.0003(13) -0.0097(12) C10 0.0376(17) 0.0407(18) 0.0417(19) -0.0174(15) -0.0050(15) -0.0131(14) C11 0.0403(18) 0.0446(19) 0.0367(19) -0.0168(15) 0.0054(15) -0.0164(15) C12 0.0361(17) 0.0241(15) 0.0313(17) -0.0028(13) -0.0008(14) -0.0074(13) C13 0.059(2) 0.060(2) 0.038(2) -0.0143(18) 0.0112(17) -0.0326(19) C14 0.059(2) 0.051(2) 0.038(2) -0.0092(17) -0.0043(17) -0.0253(18) C15 0.0146(12) 0.0220(13) 0.0320(16) -0.0108(12) 0.0008(11) -0.0059(10) C16 0.0188(13) 0.0239(14) 0.0314(16) -0.0105(12) -0.0003(11) -0.0095(11) C17 0.0222(14) 0.0214(14) 0.0386(18) -0.0133(13) 0.0001(12) -0.0054(11) C18 0.0234(14) 0.0296(15) 0.0423(19) -0.0220(14) 0.0052(13) -0.0063(12) C19 0.0287(15) 0.0385(17) 0.0260(16) -0.0135(13) 0.0034(12) -0.0132(13) C20 0.0208(14) 0.0284(15) 0.0304(16) -0.0098(13) 0.0002(12) -0.0066(12) C21 0.0218(14) 0.0215(13) 0.0304(16) -0.0076(12) -0.0004(12) -0.0045(11) C22 0.0262(15) 0.0294(15) 0.0329(17) -0.0093(13) -0.0038(13) -0.0055(12) C23 0.0386(17) 0.0244(15) 0.0363(18) -0.0032(13) -0.0003(14) -0.0108(13) C24 0.0318(16) 0.0311(16) 0.0290(17) -0.0062(13) 0.0008(13) -0.0055(13) C25 0.046(2) 0.0374(19) 0.086(3) 0.010(2) -0.011(2) -0.0174(17) C26 0.058(3) 0.058(3) 0.089(3) 0.011(2) -0.044(2) -0.020(2) C27 0.0417(19) 0.054(2) 0.059(2) -0.0137(18) -0.0057(17) -0.0295(17) C28 0.068(3) 0.104(3) 0.050(2) -0.010(2) -0.014(2) -0.060(3) C29 0.075(3) 0.070(3) 0.038(2) -0.0015(19) -0.010(2) -0.041(2) C30 0.117(4) 0.119(4) 0.050(3) 0.007(3) -0.015(3) -0.097(4) C31 0.112(5) 0.092(4) 0.119(5) -0.054(4) 0.035(4) -0.048(4) C32 0.056(5) 0.070(6) 0.082(7) -0.026(5) -0.015(5) -0.010(4) C32A 0.075(6) 0.063(5) 0.073(7) -0.030(5) -0.014(5) -0.012(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 N1 2.005(2) . ? Ga1 N2 2.009(2) . ? Ga1 Ga1 2.8640(13) 2_556 ? Ga1 K1 3.3784(13) 2_556 ? Ga1 K1 3.4223(10) . ? K1 O1 2.718(2) . ? K1 N1 2.936(3) 2_556 ? K1 C1 2.977(3) 2_556 ? K1 N2 2.987(2) 2_556 ? K1 C2 2.997(3) 2_556 ? K1 C9 3.318(3) 2_556 ? K1 C21 3.377(3) 2_556 ? K1 Ga1 3.3784(13) 2_556 ? O1 C28 1.408(4) . ? O1 C29 1.413(4) . ? O2 C32 1.445(10) 2_647 ? O2 C32 1.445(10) . ? O2 C32A 1.512(9) 2_647 ? O2 C32A 1.512(9) . ? N1 C1 1.402(3) . ? N1 C3 1.436(3) . ? N1 K1 2.936(3) 2_556 ? N2 C2 1.403(3) . ? N2 C15 1.430(3) . ? N2 K1 2.987(2) 2_556 ? C1 C2 1.356(4) . ? C1 K1 2.977(3) 2_556 ? C2 K1 2.997(3) 2_556 ? C3 C4 1.407(4) . ? C3 C8 1.409(4) . ? C4 C5 1.400(4) . ? C4 C9 1.519(4) . ? C5 C6 1.382(4) . ? C6 C7 1.373(4) . ? C7 C8 1.399(4) . ? C8 C12 1.512(4) . ? C9 C11 1.530(4) . ? C9 C10 1.531(4) . ? C9 K1 3.318(3) 2_556 ? C12 C13 1.523(5) . ? C12 C14 1.529(5) . ? C15 C20 1.407(4) . ? C15 C16 1.414(4) . ? C16 C17 1.389(4) . ? C16 C21 1.520(4) . ? C17 C18 1.382(4) . ? C18 C19 1.385(4) . ? C19 C20 1.393(4) . ? C20 C24 1.527(4) . ? C21 C23 1.536(4) . ? C21 C22 1.537(4) . ? C21 K1 3.377(3) 2_556 ? C24 C26 1.507(5) . ? C24 C25 1.510(5) . ? C27 C28 1.460(5) . ? C29 C30 1.442(6) . ? C31 C32A 1.444(11) . ? C31 C32 1.507(11) . ? 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 N2 81.88(9) . . ? N1 Ga1 Ga1 107.95(7) . 2_556 ? N2 Ga1 Ga1 109.68(7) . 2_556 ? N1 Ga1 K1 59.81(7) . 2_556 ? N2 Ga1 K1 61.26(7) . 2_556 ? Ga1 Ga1 K1 65.89(3) 2_556 2_556 ? N1 Ga1 K1 138.96(6) . . ? N2 Ga1 K1 139.15(6) . . ? Ga1 Ga1 K1 64.30(3) 2_556 . ? K1 Ga1 K1 130.19(2) 2_556 . ? O1 K1 N1 147.04(7) . 2_556 ? O1 K1 C1 131.75(7) . 2_556 ? N1 K1 C1 27.41(7) 2_556 2_556 ? O1 K1 N2 145.78(6) . 2_556 ? N1 K1 N2 52.73(6) 2_556 2_556 ? C1 K1 N2 46.54(7) 2_556 2_556 ? O1 K1 C2 131.42(7) . 2_556 ? N1 K1 C2 46.63(7) 2_556 2_556 ? C1 K1 C2 26.24(7) 2_556 2_556 ? N2 K1 C2 27.13(7) 2_556 2_556 ? O1 K1 C9 102.31(8) . 2_556 ? N1 K1 C9 54.67(7) 2_556 2_556 ? C1 K1 C9 72.29(8) 2_556 2_556 ? N2 K1 C9 106.85(8) 2_556 2_556 ? C2 K1 C9 97.99(8) 2_556 2_556 ? O1 K1 C21 102.46(7) . 2_556 ? N1 K1 C21 105.50(7) 2_556 2_556 ? C1 K1 C21 97.21(8) 2_556 2_556 ? N2 K1 C21 53.54(7) 2_556 2_556 ? C2 K1 C21 71.61(8) 2_556 2_556 ? C9 K1 C21 153.73(7) 2_556 2_556 ? O1 K1 Ga1 175.82(5) . 2_556 ? N1 K1 Ga1 36.18(5) 2_556 2_556 ? C1 K1 Ga1 52.41(6) 2_556 2_556 ? N2 K1 Ga1 36.15(4) 2_556 2_556 ? C2 K1 Ga1 52.25(6) 2_556 2_556 ? C9 K1 Ga1 78.24(6) 2_556 2_556 ? C21 K1 Ga1 76.42(6) 2_556 2_556 ? O1 K1 Ga1 126.10(5) . . ? N1 K1 Ga1 76.86(5) 2_556 . ? C1 K1 Ga1 100.66(6) 2_556 . ? N2 K1 Ga1 77.23(5) 2_556 . ? C2 K1 Ga1 100.64(6) 2_556 . ? C9 K1 Ga1 79.66(6) 2_556 . ? C21 K1 Ga1 78.77(5) 2_556 . ? Ga1 K1 Ga1 49.81(2) 2_556 . ? C28 O1 C29 115.4(3) . . ? C28 O1 K1 118.2(2) . . ? C29 O1 K1 125.0(2) . . ? C32 O2 C32 180.0(6) 2_647 . ? C32 O2 C32A 74.1(5) 2_647 2_647 ? C32 O2 C32A 105.9(5) . 2_647 ? C32 O2 C32A 105.9(5) 2_647 . ? C32 O2 C32A 74.1(5) . . ? C32A O2 C32A 180.000(1) 2_647 . ? C1 N1 C3 115.0(2) . . ? C1 N1 Ga1 111.05(17) . . ? C3 N1 Ga1 126.79(17) . . ? C1 N1 K1 77.91(15) . 2_556 ? C3 N1 K1 129.99(17) . 2_556 ? Ga1 N1 K1 84.01(7) . 2_556 ? C2 N2 C15 115.9(2) . . ? C2 N2 Ga1 110.65(16) . . ? C15 N2 Ga1 127.14(17) . . ? C2 N2 K1 76.83(15) . 2_556 ? C15 N2 K1 130.69(16) . 2_556 ? Ga1 N2 K1 82.60(8) . 2_556 ? C2 C1 N1 116.8(2) . . ? C2 C1 K1 77.71(17) . 2_556 ? N1 C1 K1 74.68(15) . 2_556 ? C1 C2 N2 117.3(2) . . ? C1 C2 K1 76.05(17) . 2_556 ? N2 C2 K1 76.04(14) . 2_556 ? C4 C3 C8 120.5(2) . . ? C4 C3 N1 119.7(2) . . ? C8 C3 N1 119.8(2) . . ? C5 C4 C3 118.4(3) . . ? C5 C4 C9 120.9(3) . . ? C3 C4 C9 120.6(2) . . ? C6 C5 C4 121.3(3) . . ? C7 C6 C5 119.8(3) . . ? C6 C7 C8 121.4(3) . . ? C7 C8 C3 118.5(3) . . ? C7 C8 C12 119.6(3) . . ? C3 C8 C12 121.8(2) . . ? C4 C9 C11 114.5(2) . . ? C4 C9 C10 109.4(2) . . ? C11 C9 C10 110.0(3) . . ? C4 C9 K1 113.50(17) . 2_556 ? C11 C9 K1 128.7(2) . 2_556 ? C10 C9 K1 68.82(16) . 2_556 ? C8 C12 C13 112.4(3) . . ? C8 C12 C14 111.2(3) . . ? C13 C12 C14 111.1(3) . . ? C20 C15 C16 119.7(2) . . ? C20 C15 N2 120.5(2) . . ? C16 C15 N2 119.8(2) . . ? C17 C16 C15 118.9(3) . . ? C17 C16 C21 120.9(2) . . ? C15 C16 C21 120.0(2) . . ? C18 C17 C16 121.6(3) . . ? C17 C18 C19 119.2(3) . . ? C18 C19 C20 121.4(3) . . ? C19 C20 C15 119.1(3) . . ? C19 C20 C24 119.1(3) . . ? C15 C20 C24 121.7(2) . . ? C16 C21 C23 114.4(2) . . ? C16 C21 C22 110.1(2) . . ? C23 C21 C22 109.2(2) . . ? C16 C21 K1 114.17(16) . 2_556 ? C23 C21 K1 128.91(19) . 2_556 ? C22 C21 K1 66.79(14) . 2_556 ? C26 C24 C25 110.1(3) . . ? C26 C24 C20 110.9(3) . . ? C25 C24 C20 113.1(3) . . ? O1 C28 C27 113.0(3) . . ? O1 C29 C30 112.1(3) . . ? C32A C31 C32 74.2(6) . . ? O2 C32 C31 106.0(7) . . ? C31 C32A O2 105.8(6) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.534 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.066 data_compound10 _database_code_CSD 189510 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H36 Al I3 N2' _chemical_formula_weight 784.25 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' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.389(2) _cell_length_b 21.162(4) _cell_length_c 13.452(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.61(3) _cell_angle_gamma 90.00 _cell_volume 2943.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.770 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 3.232 _exptl_absorpt_correction_type 'Sortav (Blessing)' _exptl_absorpt_correction_T_min 0.67 _exptl_absorpt_correction_T_max 0.84 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 Kappa CCD' _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 24508 _diffrn_reflns_av_R_equivalents 0.1593 _diffrn_reflns_av_sigmaI/netI 0.1177 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.96 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5120 _reflns_number_gt 3446 _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^)+(0.0507P)^2^+6.3631P] 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 5120 _refine_ls_number_parameters 297 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1079 _refine_ls_R_factor_gt 0.0601 _refine_ls_wR_factor_ref 0.1355 _refine_ls_wR_factor_gt 0.1180 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.000 _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 I1 I 0.71881(7) 0.26969(3) 1.27233(5) 0.0317(2) Uani 1 1 d . . . I2 I 0.97704(6) 0.13025(4) 1.37401(5) 0.0319(2) Uani 1 1 d . . . I3 I 0.66717(7) -0.04249(3) 1.38293(5) 0.0333(2) Uani 1 1 d . . . Al1 Al 0.7459(3) 0.15817(14) 1.3298(2) 0.0211(6) Uani 1 1 d . . . N1 N 0.6415(7) 0.1310(4) 1.4332(5) 0.0187(17) Uani 1 1 d . . . N2 N 0.6464(7) 0.1003(4) 1.2458(5) 0.0211(18) Uani 1 1 d . . . C1 C 0.5684(8) 0.0846(4) 1.4013(7) 0.017(2) Uani 1 1 d . . . H1 H 0.5163 0.0638 1.4433 0.021 Uiso 1 1 calc R . . C2 C 0.5704(9) 0.0660(5) 1.2983(7) 0.025(2) Uani 1 1 d . . . H2 H 0.5217 0.0324 1.2707 0.030 Uiso 1 1 calc R . . C3 C 0.6302(9) 0.1559(5) 1.5336(7) 0.021(2) Uani 1 1 d . . . C4 C 0.7037(8) 0.1294(5) 1.6162(7) 0.021(2) Uani 1 1 d . . . C5 C 0.6866(9) 0.1536(5) 1.7096(7) 0.027(2) Uani 1 1 d . . . H5 H 0.7319 0.1363 1.7662 0.032 Uiso 1 1 calc R . . C6 C 0.6023(9) 0.2034(5) 1.7194(7) 0.029(2) Uani 1 1 d . . . H6 H 0.5938 0.2204 1.7822 0.034 Uiso 1 1 calc R . . C7 C 0.5307(9) 0.2280(5) 1.6365(7) 0.027(2) Uani 1 1 d . . . H7 H 0.4723 0.2605 1.6446 0.033 Uiso 1 1 calc R . . C8 C 0.5441(8) 0.2054(4) 1.5420(7) 0.019(2) Uani 1 1 d . . . C9 C 0.7949(9) 0.0738(5) 1.6065(7) 0.025(2) Uani 1 1 d . . . H9 H 0.7972 0.0635 1.5357 0.030 Uiso 1 1 calc R . . C10 C 0.9331(10) 0.0894(6) 1.6526(8) 0.039(3) Uani 1 1 d . . . H10A H 0.9318 0.0980 1.7226 0.058 Uiso 1 1 calc R . . H10B H 0.9645 0.1259 1.6201 0.058 Uiso 1 1 calc R . . H10C H 0.9889 0.0541 1.6439 0.058 Uiso 1 1 calc R . . C11 C 0.7446(10) 0.0172(5) 1.6601(8) 0.034(3) Uani 1 1 d . . . H11A H 0.7409 0.0274 1.7293 0.051 Uiso 1 1 calc R . . H11B H 0.8016 -0.0181 1.6546 0.051 Uiso 1 1 calc R . . H11C H 0.6596 0.0066 1.6304 0.051 Uiso 1 1 calc R . . C12 C 0.4572(9) 0.2321(5) 1.4539(7) 0.023(2) Uani 1 1 d . . . H12 H 0.4983 0.2217 1.3935 0.028 Uiso 1 1 calc R . . C13 C 0.4426(12) 0.3031(5) 1.4553(9) 0.044(3) Uani 1 1 d . . . H13A H 0.3906 0.3149 1.5075 0.067 Uiso 1 1 calc R . . H13B H 0.4016 0.3171 1.3921 0.067 Uiso 1 1 calc R . . H13C H 0.5264 0.3223 1.4672 0.067 Uiso 1 1 calc R . . C14 C 0.3240(10) 0.1991(6) 1.4441(9) 0.045(3) Uani 1 1 d . . . H14A H 0.2779 0.2102 1.5000 0.067 Uiso 1 1 calc R . . H14B H 0.3360 0.1541 1.4429 0.067 Uiso 1 1 calc R . . H14C H 0.2753 0.2123 1.3833 0.067 Uiso 1 1 calc R . . C15 C 0.6249(9) 0.0936(5) 1.1362(6) 0.022(2) Uani 1 1 d . . . C16 C 0.5214(9) 0.1248(5) 1.0844(7) 0.021(2) Uani 1 1 d . . . C17 C 0.5046(10) 0.1168(5) 0.9822(7) 0.031(2) Uani 1 1 d . . . H17 H 0.4360 0.1372 0.9458 0.037 Uiso 1 1 calc R . . C18 C 0.5856(10) 0.0798(5) 0.9328(7) 0.029(2) Uani 1 1 d . . . H18 H 0.5695 0.0740 0.8642 0.035 Uiso 1 1 calc R . . C19 C 0.6913(10) 0.0511(5) 0.9846(7) 0.032(3) Uani 1 1 d . . . H19 H 0.7483 0.0276 0.9502 0.039 Uiso 1 1 calc R . . C20 C 0.7132(9) 0.0572(5) 1.0890(7) 0.025(2) Uani 1 1 d . . . C21 C 0.4267(9) 0.1659(5) 1.1372(8) 0.030(2) Uani 1 1 d . . . H21 H 0.4665 0.1746 1.2049 0.036 Uiso 1 1 calc R . . C22 C 0.4024(12) 0.2288(6) 1.0846(9) 0.043(3) Uani 1 1 d . . . H22A H 0.3579 0.2218 1.0196 0.064 Uiso 1 1 calc R . . H22B H 0.4835 0.2493 1.0779 0.064 Uiso 1 1 calc R . . H22C H 0.3505 0.2551 1.1230 0.064 Uiso 1 1 calc R . . C23 C 0.2987(10) 0.1312(6) 1.1465(9) 0.041(3) Uani 1 1 d . . . H23A H 0.2403 0.1586 1.1769 0.062 Uiso 1 1 calc R . . H23B H 0.3147 0.0942 1.1871 0.062 Uiso 1 1 calc R . . H23C H 0.2610 0.1190 1.0813 0.062 Uiso 1 1 calc R . . C24 C 0.8285(9) 0.0231(4) 1.1439(6) 0.019(2) Uani 1 1 d . . . H24 H 0.8252 0.0301 1.2157 0.023 Uiso 1 1 calc R . . C25 C 0.8197(12) -0.0476(5) 1.1254(8) 0.039(3) Uani 1 1 d . . . H25A H 0.7402 -0.0634 1.1466 0.059 Uiso 1 1 calc R . . H25B H 0.8913 -0.0684 1.1623 0.059 Uiso 1 1 calc R . . H25C H 0.8219 -0.0559 1.0554 0.059 Uiso 1 1 calc R . . C26 C 0.9563(10) 0.0499(6) 1.1158(8) 0.036(3) Uani 1 1 d . . . H26A H 0.9573 0.0488 1.0445 0.054 Uiso 1 1 calc R . . H26B H 1.0266 0.0250 1.1464 0.054 Uiso 1 1 calc R . . H26C H 0.9655 0.0928 1.1388 0.054 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 I1 0.0348(4) 0.0223(4) 0.0387(4) 0.0045(3) 0.0073(3) -0.0026(3) I2 0.0194(3) 0.0384(4) 0.0377(4) -0.0046(3) 0.0021(3) -0.0002(3) I3 0.0401(4) 0.0232(4) 0.0381(4) 0.0051(3) 0.0123(3) 0.0024(3) Al1 0.0214(14) 0.0200(15) 0.0223(15) -0.0014(12) 0.0038(12) -0.0028(12) N1 0.023(4) 0.015(4) 0.017(4) -0.001(3) -0.003(3) 0.007(4) N2 0.022(4) 0.025(5) 0.017(4) -0.003(4) 0.005(3) -0.004(4) C1 0.016(4) 0.012(5) 0.022(5) 0.012(4) -0.004(4) 0.001(4) C2 0.026(5) 0.027(6) 0.022(5) 0.000(4) 0.003(4) 0.007(5) C3 0.023(5) 0.016(5) 0.025(5) -0.002(4) 0.006(4) -0.007(4) C4 0.016(4) 0.022(5) 0.025(5) 0.001(4) -0.008(4) 0.001(4) C5 0.027(5) 0.030(6) 0.021(5) 0.001(4) 0.000(4) -0.003(5) C6 0.034(6) 0.036(6) 0.017(5) -0.002(5) 0.004(4) -0.004(5) C7 0.024(5) 0.033(6) 0.026(5) 0.000(5) 0.013(4) 0.004(5) C8 0.015(4) 0.019(5) 0.023(5) 0.009(4) -0.003(4) -0.002(4) C9 0.023(5) 0.029(6) 0.022(5) 0.003(4) -0.003(4) 0.004(4) C10 0.026(6) 0.047(8) 0.040(6) -0.001(6) -0.006(5) 0.009(5) C11 0.036(6) 0.028(6) 0.037(6) 0.001(5) -0.002(5) 0.005(5) C12 0.025(5) 0.024(5) 0.023(5) 0.003(4) 0.008(4) 0.010(5) C13 0.053(7) 0.026(7) 0.052(7) 0.008(6) -0.004(6) 0.008(6) C14 0.028(6) 0.054(8) 0.051(7) 0.022(6) -0.006(5) 0.008(6) C15 0.029(5) 0.024(6) 0.014(5) 0.000(4) 0.006(4) -0.003(5) C16 0.021(5) 0.016(5) 0.026(5) 0.005(4) -0.001(4) 0.001(4) C17 0.039(6) 0.026(6) 0.027(5) 0.012(5) -0.003(5) 0.004(5) C18 0.037(6) 0.033(6) 0.018(5) -0.009(5) 0.003(4) -0.007(5) C19 0.029(5) 0.038(7) 0.031(6) -0.005(5) 0.010(5) 0.008(5) C20 0.033(5) 0.024(6) 0.019(5) -0.001(4) 0.002(4) -0.008(5) C21 0.027(5) 0.032(6) 0.031(6) -0.013(5) -0.004(4) 0.013(5) C22 0.048(7) 0.034(7) 0.046(7) -0.001(6) 0.002(6) 0.011(6) C23 0.030(6) 0.048(8) 0.044(7) -0.005(6) -0.002(5) 0.008(6) C24 0.023(5) 0.020(5) 0.014(4) -0.005(4) 0.005(4) 0.004(4) C25 0.057(7) 0.028(6) 0.033(6) -0.007(5) 0.001(5) 0.010(6) C26 0.036(6) 0.041(7) 0.031(6) 0.001(5) 0.003(5) 0.008(6) _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 I1 Al1 2.491(3) . ? I2 Al1 2.487(3) . ? Al1 N2 1.903(8) . ? Al1 N1 1.933(8) . ? N1 C1 1.289(11) . ? N1 C3 1.465(12) . ? N2 C2 1.325(12) . ? N2 C15 1.476(11) . ? C1 C2 1.442(13) . ? C3 C8 1.389(13) . ? C3 C4 1.402(13) . ? C4 C5 1.384(13) . ? C4 C9 1.525(13) . ? C5 C6 1.385(15) . ? C6 C7 1.380(14) . ? C7 C8 1.378(13) . ? C8 C12 1.527(13) . ? C9 C11 1.516(15) . ? C9 C10 1.543(14) . ? C12 C13 1.509(15) . ? C12 C14 1.544(15) . ? C15 C16 1.390(13) . ? C15 C20 1.397(13) . ? C16 C17 1.379(14) . ? C16 C21 1.538(13) . ? C17 C18 1.368(14) . ? C18 C19 1.383(15) . ? C19 C20 1.407(14) . ? C20 C24 1.525(14) . ? C21 C22 1.517(16) . ? C21 C23 1.535(15) . ? C24 C25 1.519(15) . ? C24 C26 1.525(14) . ? 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 N2 Al1 N1 85.7(3) . . ? N2 Al1 I2 116.4(3) . . ? N1 Al1 I2 110.7(2) . . ? N2 Al1 I1 112.8(3) . . ? N1 Al1 I1 116.8(3) . . ? I2 Al1 I1 112.12(11) . . ? C1 N1 C3 118.9(8) . . ? C1 N1 Al1 109.9(6) . . ? C3 N1 Al1 131.1(6) . . ? C2 N2 C15 116.1(8) . . ? C2 N2 Al1 110.7(6) . . ? C15 N2 Al1 132.5(6) . . ? N1 C1 C2 117.7(8) . . ? N2 C2 C1 115.4(9) . . ? C8 C3 C4 122.8(8) . . ? C8 C3 N1 117.2(8) . . ? C4 C3 N1 120.0(8) . . ? C5 C4 C3 117.6(9) . . ? C5 C4 C9 119.9(8) . . ? C3 C4 C9 122.4(8) . . ? C4 C5 C6 120.4(9) . . ? C7 C6 C5 120.4(9) . . ? C8 C7 C6 121.3(9) . . ? C7 C8 C3 117.5(8) . . ? C7 C8 C12 118.8(8) . . ? C3 C8 C12 123.6(8) . . ? C11 C9 C4 108.8(8) . . ? C11 C9 C10 109.2(9) . . ? C4 C9 C10 111.2(9) . . ? C13 C12 C8 114.2(9) . . ? C13 C12 C14 111.2(9) . . ? C8 C12 C14 110.8(8) . . ? C16 C15 C20 123.0(8) . . ? C16 C15 N2 119.3(8) . . ? C20 C15 N2 117.7(8) . . ? C17 C16 C15 117.3(9) . . ? C17 C16 C21 120.4(8) . . ? C15 C16 C21 122.4(8) . . ? C18 C17 C16 122.0(10) . . ? C17 C18 C19 120.2(9) . . ? C18 C19 C20 120.4(9) . . ? C15 C20 C19 117.0(9) . . ? C15 C20 C24 124.1(8) . . ? C19 C20 C24 118.9(8) . . ? C22 C21 C23 110.6(9) . . ? C22 C21 C16 111.4(9) . . ? C23 C21 C16 111.5(9) . . ? C25 C24 C26 111.5(8) . . ? C25 C24 C20 110.7(8) . . ? C26 C24 C20 111.4(8) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.466 (near I2) _refine_diff_density_min -0.925 _refine_diff_density_rms 0.237