# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address G.Linti ;Anorganisch-Chemisches Institut Im Neuenheimer Feld 270 D-69120 Heidelberg Germany ; T.Zessin ;Anorganisch-Chemisches Institut Im Neuenheimer Feld 270 D-69120 Heidelberg Germany ; _publ_contact_author_address ;Anorganisch-Chemisches Institut Im Neuenheimer Feld 270 D-69120 Heidelberg Germany ; _publ_contact_author_email gerald.linti@aci.uni-heidelberg.de _publ_contact_author_fax +49-(0)6221-546617 _publ_contact_author_phone +49-(0)6221-548468 _publ_contact_author_name 'Gerald Linti' # Attachment '- 2 - TZE40.CIF' data_2 _database_code_depnum_ccdc_archive 'CCDC 811974' #TrackingRef '- 2 - TZE40.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; diiodo-bis(N,N'-bis(2,6-diisopropylphenyl)ethylamidinato)-di-gallium(II) ; _chemical_name_common ;diiodo-bis(N,N'-bis(2,6-diisopropylphenyl)ethylamidinato)-di- gallium(ii) ; _chemical_melting_point '513 (dec)' _chemical_formula_moiety 'C26 H37 Ga I N2' _chemical_formula_sum 'C26 H37 Ga I N2' _chemical_formula_weight 574.20 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' 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 'P 21/c' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.364(2) _cell_length_b 17.629(4) _cell_length_c 15.399(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.90(3) _cell_angle_gamma 90.00 _cell_volume 2677.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cuboid _exptl_crystal_colour colourless _exptl_crystal_size_max 0.330 _exptl_crystal_size_mid 0.222 _exptl_crystal_size_min 0.185 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1164 _exptl_absorpt_coefficient_mu 2.195 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.5928 _exptl_absorpt_correction_T_max 0.6829 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21208 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_sigmaI/netI 0.0499 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 26.07 _reflns_number_total 5269 _reflns_number_gt 3806 _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^)+(0.0355P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5269 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.0650 _refine_ls_wR_factor_gt 0.0621 _refine_ls_goodness_of_fit_ref 0.880 _refine_ls_restrained_S_all 0.880 _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 0.39928(3) 0.970039(17) 0.94939(2) 0.02127(9) Uani 1 1 d . . . I1 I 0.16546(2) 1.007109(13) 0.954327(15) 0.03942(8) Uani 1 1 d . . . N1 N 0.3964(2) 0.86010(12) 0.92310(15) 0.0206(5) Uani 1 1 d . . . N2 N 0.3914(2) 0.94665(12) 0.82168(14) 0.0196(5) Uani 1 1 d . . . C1 C 0.3939(3) 0.87342(15) 0.83833(19) 0.0214(6) Uani 1 1 d . . . C2 C 0.3988(4) 0.81328(17) 0.7721(2) 0.0331(7) Uani 1 1 d . . . H2A H 0.3086 0.8029 0.7332 0.050 Uiso 1 1 calc R . . H2B H 0.4372 0.7680 0.8045 0.050 Uiso 1 1 calc R . . H2C H 0.4538 0.8300 0.7357 0.050 Uiso 1 1 calc R . . C3 C 0.3946(3) 0.78635(15) 0.95980(19) 0.0232(6) Uani 1 1 d . . . C4 C 0.2726(3) 0.74550(17) 0.9364(2) 0.0311(7) Uani 1 1 d . . . C5 C 0.2768(4) 0.67288(18) 0.9717(2) 0.0383(8) Uani 1 1 d . . . H5A H 0.1983 0.6437 0.9556 0.046 Uiso 1 1 calc R . . C6 C 0.3931(4) 0.64314(17) 1.0296(2) 0.0376(8) Uani 1 1 d . . . H6A H 0.3936 0.5939 1.0515 0.045 Uiso 1 1 calc R . . C7 C 0.5087(4) 0.68566(17) 1.0554(2) 0.0342(8) Uani 1 1 d . . . H7A H 0.5865 0.6656 1.0968 0.041 Uiso 1 1 calc R . . C8 C 0.5129(3) 0.75778(16) 1.02148(18) 0.0261(7) Uani 1 1 d . . . C9 C 0.1394(4) 0.7781(2) 0.8800(3) 0.0432(9) Uani 1 1 d . . . H9A H 0.1579 0.8275 0.8571 0.052 Uiso 1 1 calc R . . C10 C 0.0486(5) 0.7916(3) 0.9389(4) 0.0692(13) Uani 1 1 d . . . H10A H 0.0952 0.8229 0.9899 0.104 Uiso 1 1 calc R . . H10B H 0.0260 0.7439 0.9605 0.104 Uiso 1 1 calc R . . H10C H -0.0328 0.8167 0.9035 0.104 Uiso 1 1 calc R . . C11 C 0.0663(5) 0.7292(3) 0.7970(3) 0.0729(14) Uani 1 1 d . . . H11A H 0.1247 0.7216 0.7599 0.109 Uiso 1 1 calc R . . H11B H -0.0150 0.7544 0.7617 0.109 Uiso 1 1 calc R . . H11C H 0.0435 0.6810 0.8173 0.109 Uiso 1 1 calc R . . C12 C 0.6412(3) 0.80418(18) 1.0539(2) 0.0330(8) Uani 1 1 d . . . H12A H 0.6286 0.8497 1.0158 0.040 Uiso 1 1 calc R . . C13 C 0.6647(6) 0.8296(3) 1.1517(3) 0.0815(16) Uani 1 1 d . . . H13A H 0.5860 0.8562 1.1561 0.122 Uiso 1 1 calc R . . H13B H 0.7419 0.8627 1.1699 0.122 Uiso 1 1 calc R . . H13C H 0.6809 0.7861 1.1911 0.122 Uiso 1 1 calc R . . C14 C 0.7633(5) 0.7638(3) 1.0460(4) 0.0874(18) Uani 1 1 d . . . H14A H 0.7479 0.7481 0.9840 0.131 Uiso 1 1 calc R . . H14B H 0.7806 0.7200 1.0850 0.131 Uiso 1 1 calc R . . H14C H 0.8402 0.7971 1.0640 0.131 Uiso 1 1 calc R . . C15 C 0.3723(3) 0.98176(14) 0.73609(18) 0.0223(6) Uani 1 1 d . . . C16 C 0.2430(3) 0.98409(16) 0.6727(2) 0.0289(7) Uani 1 1 d . . . C17 C 0.2275(4) 1.02236(18) 0.5912(2) 0.0390(8) Uani 1 1 d . . . H17A H 0.1424 1.0241 0.5476 0.047 Uiso 1 1 calc R . . C18 C 0.3338(4) 1.0573(2) 0.5738(2) 0.0460(10) Uani 1 1 d . . . H18A H 0.3212 1.0821 0.5185 0.055 Uiso 1 1 calc R . . C19 C 0.4589(4) 1.05610(19) 0.6373(2) 0.0420(9) Uani 1 1 d . . . H19A H 0.5301 1.0814 0.6251 0.050 Uiso 1 1 calc R . . C20 C 0.4827(3) 1.01803(16) 0.7196(2) 0.0305(7) Uani 1 1 d . . . C21 C 0.1207(3) 0.9489(2) 0.6893(2) 0.0367(8) Uani 1 1 d . . . H21A H 0.1487 0.9278 0.7512 0.044 Uiso 1 1 calc R . . C22 C 0.0113(4) 1.0083(3) 0.6837(3) 0.0607(11) Uani 1 1 d . . . H22A H 0.0482 1.0484 0.7263 0.091 Uiso 1 1 calc R . . H22B H -0.0634 0.9852 0.6983 0.091 Uiso 1 1 calc R . . H22C H -0.0198 1.0288 0.6230 0.091 Uiso 1 1 calc R . . C23 C 0.0630(4) 0.8847(2) 0.6230(3) 0.0533(10) Uani 1 1 d . . . H23A H 0.1322 0.8475 0.6271 0.080 Uiso 1 1 calc R . . H23B H 0.0316 0.9044 0.5620 0.080 Uiso 1 1 calc R . . H23C H -0.0114 0.8616 0.6380 0.080 Uiso 1 1 calc R . . C24 C 0.6224(3) 1.01498(19) 0.7880(2) 0.0371(8) Uani 1 1 d . . . H24A H 0.6108 1.0085 0.8484 0.045 Uiso 1 1 calc R . . C25 C 0.7056(5) 1.0859(3) 0.7917(3) 0.0710(14) Uani 1 1 d . . . H25A H 0.6564 1.1290 0.8031 0.106 Uiso 1 1 calc R . . H25B H 0.7233 1.0925 0.7345 0.106 Uiso 1 1 calc R . . H25C H 0.7899 1.0814 0.8398 0.106 Uiso 1 1 calc R . . C26 C 0.6993(4) 0.9464(3) 0.7711(3) 0.0631(12) Uani 1 1 d . . . H26A H 0.6461 0.9015 0.7696 0.095 Uiso 1 1 calc R . . H26B H 0.7837 0.9420 0.8191 0.095 Uiso 1 1 calc R . . H26C H 0.7167 0.9520 0.7137 0.095 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 0.02058(18) 0.02236(16) 0.01954(15) -0.00253(12) 0.00421(12) -0.00145(13) I1 0.02507(12) 0.05047(15) 0.04328(13) -0.00810(10) 0.01131(9) 0.00245(10) N1 0.0216(14) 0.0168(11) 0.0226(13) 0.0007(9) 0.0059(10) -0.0010(9) N2 0.0237(14) 0.0177(12) 0.0167(11) 0.0001(9) 0.0050(10) -0.0002(10) C1 0.0150(16) 0.0242(15) 0.0235(15) 0.0007(11) 0.0036(12) -0.0018(11) C2 0.045(2) 0.0267(16) 0.0283(17) -0.0046(12) 0.0132(15) 0.0007(14) C3 0.0328(18) 0.0199(14) 0.0194(14) 0.0011(11) 0.0115(13) 0.0003(13) C4 0.035(2) 0.0272(17) 0.0336(18) 0.0046(13) 0.0135(15) -0.0037(14) C5 0.045(2) 0.0306(18) 0.041(2) 0.0061(15) 0.0166(17) -0.0117(16) C6 0.062(3) 0.0214(16) 0.0354(18) 0.0089(13) 0.0239(18) 0.0009(16) C7 0.044(2) 0.0319(18) 0.0293(18) 0.0091(13) 0.0158(16) 0.0123(15) C8 0.034(2) 0.0229(15) 0.0228(16) 0.0020(11) 0.0106(14) 0.0056(13) C9 0.029(2) 0.038(2) 0.056(2) 0.0126(16) 0.0032(17) -0.0106(15) C10 0.042(3) 0.068(3) 0.104(4) 0.025(3) 0.032(3) 0.006(2) C11 0.057(3) 0.060(3) 0.077(3) 0.003(2) -0.016(2) -0.017(2) C12 0.0272(19) 0.0298(17) 0.0370(18) 0.0062(13) 0.0027(15) 0.0066(13) C13 0.097(4) 0.089(4) 0.049(3) -0.018(2) 0.008(3) -0.037(3) C14 0.042(3) 0.058(3) 0.162(6) -0.022(3) 0.030(3) -0.001(2) C15 0.0305(17) 0.0166(14) 0.0189(13) 0.0016(10) 0.0061(12) 0.0023(12) C16 0.0361(19) 0.0230(16) 0.0251(15) -0.0010(12) 0.0056(13) 0.0056(13) C17 0.048(2) 0.0373(19) 0.0239(16) 0.0066(13) -0.0004(15) 0.0105(16) C18 0.071(3) 0.0358(19) 0.0273(18) 0.0134(14) 0.0099(19) 0.0032(18) C19 0.059(3) 0.0348(18) 0.0342(19) 0.0065(14) 0.0169(18) -0.0124(17) C20 0.043(2) 0.0236(16) 0.0268(15) -0.0018(12) 0.0132(14) -0.0053(13) C21 0.0264(19) 0.049(2) 0.0287(17) 0.0053(14) 0.0002(14) 0.0006(15) C22 0.039(2) 0.086(3) 0.053(2) -0.001(2) 0.0095(18) 0.019(2) C23 0.041(2) 0.056(2) 0.051(2) 0.0012(18) -0.0035(18) -0.0093(19) C24 0.034(2) 0.044(2) 0.0337(17) 0.0007(14) 0.0115(14) -0.0141(15) C25 0.067(3) 0.066(3) 0.073(3) 0.002(2) 0.011(2) -0.035(2) C26 0.038(3) 0.074(3) 0.073(3) -0.010(2) 0.012(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 N1 1.978(2) . ? Ga1 N2 1.986(2) . ? Ga1 C1 2.402(3) . ? Ga1 Ga1 2.4298(10) 3_677 ? Ga1 I1 2.5334(6) . ? N1 C1 1.319(3) . ? N1 C3 1.420(3) . ? N2 C1 1.315(3) . ? N2 C15 1.414(3) . ? C1 C2 1.483(4) . ? C3 C8 1.394(4) . ? C3 C4 1.403(4) . ? C4 C5 1.387(4) . ? C4 C9 1.501(5) . ? C5 C6 1.365(5) . ? C6 C7 1.365(5) . ? C7 C8 1.381(4) . ? C8 C12 1.509(5) . ? C9 C10 1.513(6) . ? C9 C11 1.535(6) . ? C12 C14 1.489(6) . ? C12 C13 1.518(5) . ? C15 C16 1.395(4) . ? C15 C20 1.400(4) . ? C16 C17 1.390(4) . ? C16 C21 1.502(5) . ? C17 C18 1.359(5) . ? C18 C19 1.363(5) . ? C19 C20 1.388(4) . ? C20 C24 1.507(5) . ? C21 C23 1.519(5) . ? C21 C22 1.526(5) . ? C24 C25 1.511(5) . ? C24 C26 1.515(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 N1 Ga1 N2 66.45(9) . . ? N1 Ga1 C1 33.29(9) . . ? N2 Ga1 C1 33.18(9) . . ? N1 Ga1 Ga1 120.87(7) . 3_677 ? N2 Ga1 Ga1 119.43(7) . 3_677 ? C1 Ga1 Ga1 126.32(7) . 3_677 ? N1 Ga1 I1 107.73(7) . . ? N2 Ga1 I1 109.54(8) . . ? C1 Ga1 I1 113.03(7) . . ? Ga1 Ga1 I1 120.65(2) 3_677 . ? C1 N1 C3 123.9(2) . . ? C1 N1 Ga1 91.29(16) . . ? C3 N1 Ga1 144.75(19) . . ? C1 N2 C15 126.9(2) . . ? C1 N2 Ga1 91.06(16) . . ? C15 N2 Ga1 141.58(18) . . ? N2 C1 N1 111.2(2) . . ? N2 C1 C2 124.8(3) . . ? N1 C1 C2 124.0(2) . . ? N2 C1 Ga1 55.77(13) . . ? N1 C1 Ga1 55.42(14) . . ? C2 C1 Ga1 176.8(2) . . ? C8 C3 C4 121.6(3) . . ? C8 C3 N1 119.0(3) . . ? C4 C3 N1 119.3(3) . . ? C5 C4 C3 117.1(3) . . ? C5 C4 C9 119.5(3) . . ? C3 C4 C9 123.3(3) . . ? C6 C5 C4 121.7(3) . . ? C5 C6 C7 120.0(3) . . ? C6 C7 C8 121.5(3) . . ? C7 C8 C3 117.9(3) . . ? C7 C8 C12 120.0(3) . . ? C3 C8 C12 122.0(3) . . ? C4 C9 C10 110.1(3) . . ? C4 C9 C11 113.4(3) . . ? C10 C9 C11 110.5(4) . . ? C14 C12 C8 113.4(3) . . ? C14 C12 C13 110.0(4) . . ? C8 C12 C13 110.2(3) . . ? C16 C15 C20 121.5(3) . . ? C16 C15 N2 119.6(3) . . ? C20 C15 N2 118.7(3) . . ? C17 C16 C15 117.8(3) . . ? C17 C16 C21 119.0(3) . . ? C15 C16 C21 123.3(3) . . ? C18 C17 C16 121.5(3) . . ? C17 C18 C19 120.1(3) . . ? C18 C19 C20 121.8(3) . . ? C19 C20 C15 117.4(3) . . ? C19 C20 C24 121.3(3) . . ? C15 C20 C24 121.3(3) . . ? C16 C21 C23 111.8(3) . . ? C16 C21 C22 111.0(3) . . ? C23 C21 C22 110.0(3) . . ? C20 C24 C25 114.3(3) . . ? C20 C24 C26 110.6(3) . . ? C25 C24 C26 110.1(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.07 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.531 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.084 _exptl_crystal_recrystallization_method 'from tetrahydrofurane' data_2a _database_code_depnum_ccdc_archive 'CCDC 811975' _audit_creation_method SHELXL-97 _chemical_name_systematic ; diiodo-bis(N,N'-bis(2,6-diisopropylphenyl)ethylamidinato) -di-gallium(II) tetrahydrofurane solvate ; _chemical_name_common ; diiodo-bis(N,N'-bis(2,6-diisopropylphenyl)ethylamidinato) -di- gallium(ii) tetrahydrofurane solvate ; _chemical_melting_point '513 (dec)' _chemical_formula_moiety ;C52 H74 Ga2 I2 N4, 2(C4 H8 O) ; _chemical_formula_sum 'C60 H90 Ga2 I2 N4 O2' _chemical_formula_weight 1292.60 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' O O 0.0106 0.0060 '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' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.847(2) _cell_length_b 12.842(3) _cell_length_c 22.349(5) _cell_angle_alpha 96.71(3) _cell_angle_beta 91.80(3) _cell_angle_gamma 101.27(3) _cell_volume 3027.5(11) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needles _exptl_crystal_colour colourless _exptl_crystal_size_max 0.434 _exptl_crystal_size_mid 0.076 _exptl_crystal_size_min 0.044 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1324 _exptl_absorpt_coefficient_mu 1.952 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.6121 _exptl_absorpt_correction_T_max 0.9182 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23545 _diffrn_reflns_av_R_equivalents 0.1181 _diffrn_reflns_av_sigmaI/netI 0.2590 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 26.01 _reflns_number_total 11042 _reflns_number_gt 3830 _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^)+(0.0176P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11042 _refine_ls_number_parameters 631 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1546 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.0912 _refine_ls_wR_factor_gt 0.0737 _refine_ls_goodness_of_fit_ref 0.648 _refine_ls_restrained_S_all 0.649 _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 -0.05925(6) 0.01922(6) 0.28200(4) 0.0411(2) Uani 1 1 d . . . I2 I 0.55165(6) 0.06487(5) 0.29052(3) 0.0410(2) Uani 1 1 d . . . Ga2 Ga 0.31819(8) -0.01725(7) 0.27029(4) 0.0269(3) Uani 1 1 d . . . Ga1 Ga 0.17388(8) 0.10473(7) 0.28389(4) 0.0263(2) Uani 1 1 d . . . N4 N 0.3078(5) -0.1157(4) 0.1913(3) 0.0221(15) Uani 1 1 d . . . N1 N 0.2050(5) 0.2489(4) 0.3324(3) 0.0193(14) Uani 1 1 d . . . N3 N 0.2886(5) -0.1702(4) 0.2796(3) 0.0195(14) Uani 1 1 d . . . C29 C 0.2842(7) -0.2446(5) 0.3234(3) 0.0251(19) Uani 1 1 d . . . C15 C 0.1723(7) 0.2556(5) 0.1749(3) 0.0254(19) Uani 1 1 d . . . C34 C 0.3925(7) -0.2819(6) 0.3388(4) 0.029(2) Uani 1 1 d . . . C4 C 0.1068(7) 0.3296(6) 0.4188(4) 0.030(2) Uani 1 1 d . . . C3 C 0.2113(6) 0.3038(5) 0.3932(3) 0.0213(18) Uani 1 1 d . . . C42 C 0.2133(7) -0.1015(5) 0.0945(4) 0.028(2) Uani 1 1 d . . . C1 C 0.2005(6) 0.2964(5) 0.2845(3) 0.0196(18) Uani 1 1 d . . . C41 C 0.3182(7) -0.1188(6) 0.1280(3) 0.031(2) Uani 1 1 d . . . C28 C 0.2748(7) -0.3134(5) 0.1919(4) 0.031(2) Uani 1 1 d . . . H28A H 0.2642 -0.3617 0.2230 0.046 Uiso 1 1 calc R . . H28B H 0.3494 -0.3221 0.1697 0.046 Uiso 1 1 calc R . . H28C H 0.2002 -0.3306 0.1639 0.046 Uiso 1 1 calc R . . N2 N 0.1810(5) 0.2275(4) 0.2356(3) 0.0198(14) Uani 1 1 d . . . C33 C 0.3841(8) -0.3497(6) 0.3815(4) 0.037(2) Uani 1 1 d . . . H33A H 0.4558 -0.3778 0.3914 0.044 Uiso 1 1 calc R . . C43 C 0.2275(8) -0.1006(7) 0.0326(4) 0.046(2) Uani 1 1 d . . . H43A H 0.1588 -0.0910 0.0078 0.055 Uiso 1 1 calc R . . C30 C 0.1720(7) -0.2734(5) 0.3520(3) 0.028(2) Uani 1 1 d . . . C5 C 0.1170(7) 0.3828(6) 0.4778(4) 0.0293(19) Uani 1 1 d . . . H5A H 0.0450 0.4030 0.4952 0.035 Uiso 1 1 calc R . . C9 C 0.4440(7) 0.2930(6) 0.3991(4) 0.028(2) Uani 1 1 d . . . H9A H 0.4134 0.2280 0.3692 0.033 Uiso 1 1 calc R . . C45 C 0.4345(8) -0.1303(6) 0.0415(4) 0.038(2) Uani 1 1 d . . . H45A H 0.5094 -0.1404 0.0228 0.045 Uiso 1 1 calc R . . C46 C 0.4299(7) -0.1338(6) 0.1024(4) 0.030(2) Uani 1 1 d . . . C16 C 0.0611(8) 0.2823(6) 0.1546(4) 0.037(2) Uani 1 1 d . . . C20 C 0.2716(8) 0.2506(7) 0.1390(4) 0.041(2) Uani 1 1 d . . . C8 C 0.3306(7) 0.3255(6) 0.4259(4) 0.029(2) Uani 1 1 d . . . C6 C 0.2294(8) 0.4055(6) 0.5103(4) 0.038(2) Uani 1 1 d . . . H6A H 0.2362 0.4404 0.5506 0.046 Uiso 1 1 calc R . . C27 C 0.2911(6) -0.2008(6) 0.2208(3) 0.0230(18) Uani 1 1 d . . . C12 C -0.0229(7) 0.3016(6) 0.3854(4) 0.033(2) Uani 1 1 d U . . H12A H -0.0135 0.2665 0.3438 0.040 Uiso 1 1 calc R . . C24 C -0.0496(8) 0.2889(7) 0.1933(5) 0.048(3) Uani 1 1 d . . . H24A H -0.0269 0.2737 0.2346 0.058 Uiso 1 1 calc R . . C7 C 0.3343(7) 0.3767(6) 0.4835(4) 0.032(2) Uani 1 1 d . . . H7A H 0.4125 0.3933 0.5064 0.039 Uiso 1 1 calc R . . C44 C 0.3377(8) -0.1130(6) 0.0064(4) 0.042(2) Uani 1 1 d . . . H44A H 0.3460 -0.1097 -0.0356 0.050 Uiso 1 1 calc R . . C32 C 0.2757(9) -0.3793(6) 0.4110(4) 0.039(2) Uani 1 1 d . . . H32A H 0.2730 -0.4253 0.4415 0.047 Uiso 1 1 calc R . . C17 C 0.0524(10) 0.2973(7) 0.0951(5) 0.052(3) Uani 1 1 d . . . H17A H -0.0237 0.3115 0.0789 0.063 Uiso 1 1 calc R . . C2 C 0.2128(7) 0.4159(6) 0.2857(4) 0.039(2) Uani 1 1 d . . . H2A H 0.2260 0.4503 0.3275 0.058 Uiso 1 1 calc R . . H2B H 0.1358 0.4309 0.2675 0.058 Uiso 1 1 calc R . . H2C H 0.2848 0.4439 0.2627 0.058 Uiso 1 1 calc R . . C31 C 0.1714(8) -0.3407(6) 0.3952(4) 0.043(2) Uani 1 1 d . . . H31A H 0.0960 -0.3615 0.4150 0.052 Uiso 1 1 calc R . . C19 C 0.2573(10) 0.2679(8) 0.0805(4) 0.060(3) Uani 1 1 d . . . H19A H 0.3236 0.2629 0.0542 0.072 Uiso 1 1 calc R . . C18 C 0.1477(13) 0.2927(9) 0.0593(5) 0.084(4) Uani 1 1 d . . . H18A H 0.1397 0.3066 0.0187 0.101 Uiso 1 1 calc R . . C47 C 0.5425(7) -0.1513(7) 0.1392(4) 0.035(2) Uani 1 1 d . . . H47A H 0.5205 -0.1529 0.1822 0.042 Uiso 1 1 calc R . . C21 C 0.3938(8) 0.2266(7) 0.1643(4) 0.039(2) Uani 1 1 d . . . H21A H 0.3727 0.1810 0.1973 0.047 Uiso 1 1 calc R . . C38 C 0.0566(8) -0.2325(7) 0.3357(4) 0.031(2) Uani 1 1 d . . . H38A H 0.0851 -0.1597 0.3233 0.037 Uiso 1 1 calc R . . C11 C 0.5342(9) 0.2636(8) 0.4441(5) 0.060(3) Uani 1 1 d . . . H11A H 0.4891 0.2073 0.4660 0.090 Uiso 1 1 calc R . . H11B H 0.5702 0.3268 0.4727 0.090 Uiso 1 1 calc R . . H11C H 0.6020 0.2375 0.4227 0.090 Uiso 1 1 calc R . . C37 C 0.6155(9) -0.1860(8) 0.3576(5) 0.060(3) Uani 1 1 d . . . H37A H 0.5847 -0.1238 0.3764 0.090 Uiso 1 1 calc R . . H37B H 0.6931 -0.1618 0.3376 0.090 Uiso 1 1 calc R . . H37C H 0.6325 -0.2300 0.3887 0.090 Uiso 1 1 calc R . . C23 C 0.4613(8) 0.1660(7) 0.1173(5) 0.060(3) Uani 1 1 d . . . H23A H 0.5381 0.1516 0.1361 0.090 Uiso 1 1 calc R . . H23B H 0.4835 0.2092 0.0844 0.090 Uiso 1 1 calc R . . H23C H 0.4058 0.0981 0.1011 0.090 Uiso 1 1 calc R . . C35 C 0.5164(8) -0.2518(7) 0.3115(4) 0.047(3) Uani 1 1 d . . . H35A H 0.5041 -0.2051 0.2799 0.056 Uiso 1 1 calc R . . C48 C 0.6549(8) -0.0616(7) 0.1359(5) 0.052(3) Uani 1 1 d . . . H48A H 0.6334 0.0069 0.1513 0.078 Uiso 1 1 calc R . . H48B H 0.6779 -0.0602 0.0939 0.078 Uiso 1 1 calc R . . H48C H 0.7261 -0.0734 0.1605 0.078 Uiso 1 1 calc R . . C14 C -0.1122(8) 0.2217(8) 0.4178(5) 0.066(3) Uani 1 1 d . . . H14A H -0.0768 0.1576 0.4201 0.099 Uiso 1 1 calc R . . H14B H -0.1942 0.2018 0.3953 0.099 Uiso 1 1 calc R . . H14C H -0.1228 0.2546 0.4586 0.099 Uiso 1 1 calc R . . C39 C -0.0293(9) -0.2231(9) 0.3836(5) 0.065(3) Uani 1 1 d . . . H39A H 0.0157 -0.1769 0.4187 0.097 Uiso 1 1 calc R . . H39B H -0.0630 -0.2941 0.3950 0.097 Uiso 1 1 calc R . . H39C H -0.0987 -0.1918 0.3695 0.097 Uiso 1 1 calc R . . C13 C -0.0801(9) 0.3990(7) 0.3796(5) 0.067(3) Uani 1 1 d . . . H13A H -0.0236 0.4496 0.3583 0.100 Uiso 1 1 calc R . . H13B H -0.0922 0.4334 0.4199 0.100 Uiso 1 1 calc R . . H13C H -0.1616 0.3768 0.3568 0.100 Uiso 1 1 calc R . . C51 C 0.0256(8) -0.0155(7) 0.0918(5) 0.054(3) Uani 1 1 d . . . H51A H 0.0829 0.0537 0.0919 0.081 Uiso 1 1 calc R . . H51B H -0.0486 -0.0052 0.1139 0.081 Uiso 1 1 calc R . . H51C H -0.0008 -0.0466 0.0501 0.081 Uiso 1 1 calc R . . C10 C 0.5158(8) 0.3792(7) 0.3647(5) 0.058(3) Uani 1 1 d . . . H10A H 0.4583 0.3977 0.3348 0.087 Uiso 1 1 calc R . . H10B H 0.5840 0.3524 0.3441 0.087 Uiso 1 1 calc R . . H10C H 0.5514 0.4430 0.3930 0.087 Uiso 1 1 calc R . . C50 C 0.0918(8) -0.0897(7) 0.1218(4) 0.036(2) Uani 1 1 d . . . H50A H 0.1135 -0.0561 0.1644 0.043 Uiso 1 1 calc R . . C40 C -0.0183(8) -0.3043(7) 0.2813(4) 0.054(3) Uani 1 1 d . . . H40A H -0.0927 -0.2759 0.2710 0.080 Uiso 1 1 calc R . . H40B H -0.0448 -0.3772 0.2916 0.080 Uiso 1 1 calc R . . H40C H 0.0349 -0.3055 0.2467 0.080 Uiso 1 1 calc R . . C26 C -0.1665(8) 0.2090(8) 0.1688(5) 0.072(4) Uani 1 1 d . . . H26A H -0.1488 0.1366 0.1651 0.108 Uiso 1 1 calc R . . H26B H -0.1925 0.2249 0.1291 0.108 Uiso 1 1 calc R . . H26C H -0.2343 0.2135 0.1964 0.108 Uiso 1 1 calc R . . C25 C -0.0789(10) 0.4007(7) 0.1982(5) 0.069(3) Uani 1 1 d . . . H25A H -0.0039 0.4533 0.2146 0.104 Uiso 1 1 calc R . . H25B H -0.1479 0.4046 0.2251 0.104 Uiso 1 1 calc R . . H25C H -0.1036 0.4161 0.1581 0.104 Uiso 1 1 calc R . . C49 C 0.5815(9) -0.2583(7) 0.1156(5) 0.063(3) Uani 1 1 d . . . H49A H 0.6532 -0.2678 0.1407 0.095 Uiso 1 1 calc R . . H49B H 0.6053 -0.2567 0.0737 0.095 Uiso 1 1 calc R . . H49C H 0.5105 -0.3180 0.1175 0.095 Uiso 1 1 calc R . . C36 C 0.5636(9) -0.3485(8) 0.2797(5) 0.068(3) Uani 1 1 d . . . H36A H 0.4991 -0.3891 0.2496 0.102 Uiso 1 1 calc R . . H36B H 0.5807 -0.3947 0.3096 0.102 Uiso 1 1 calc R . . H36C H 0.6410 -0.3233 0.2597 0.102 Uiso 1 1 calc R . . C52 C 0.0077(8) -0.1936(8) 0.1247(5) 0.071(4) Uani 1 1 d . . . H52A H 0.0537 -0.2403 0.1441 0.106 Uiso 1 1 calc R . . H52B H -0.0219 -0.2270 0.0837 0.106 Uiso 1 1 calc R . . H52C H -0.0646 -0.1828 0.1481 0.106 Uiso 1 1 calc R . . C22 C 0.4775(9) 0.3280(9) 0.1909(5) 0.080(4) Uani 1 1 d . . . H22A H 0.5554 0.3126 0.2079 0.120 Uiso 1 1 calc R . . H22B H 0.4349 0.3635 0.2229 0.120 Uiso 1 1 calc R . . H22C H 0.4975 0.3750 0.1595 0.120 Uiso 1 1 calc R . . O1 O 0.1432(11) -0.4971(10) -0.0481(5) 0.139(4) Uani 1 1 d . . . C53 C 0.1776(18) -0.4304(12) 0.0054(8) 0.160(9) Uani 1 1 d . . . H53A H 0.1713 -0.3564 -0.0008 0.193 Uiso 1 1 calc R . . H53B H 0.1186 -0.4535 0.0364 0.193 Uiso 1 1 calc R . . C54 C 0.2973(17) -0.4312(13) 0.0254(8) 0.133(7) Uani 1 1 d . . . H54A H 0.2992 -0.4853 0.0534 0.160 Uiso 1 1 calc R . . H54B H 0.3412 -0.3600 0.0452 0.160 Uiso 1 1 calc R . . C56 C 0.2578(19) -0.5082(17) -0.0767(7) 0.163(9) Uani 1 1 d . . . H56A H 0.2594 -0.5847 -0.0882 0.196 Uiso 1 1 calc R . . H56B H 0.2651 -0.4716 -0.1134 0.196 Uiso 1 1 calc R . . C55 C 0.3531(19) -0.4624(19) -0.0354(10) 0.193(11) Uani 1 1 d . . . H55A H 0.4033 -0.3978 -0.0496 0.231 Uiso 1 1 calc R . . H55B H 0.4092 -0.5132 -0.0301 0.231 Uiso 1 1 calc R . . O2 O 0.2634(13) 0.0081(11) 0.3969(4) 0.160(7) Uani 1 1 d . . . C60 C 0.1779(15) 0.0457(10) 0.4334(7) 0.098(5) Uani 1 1 d . . . H60A H 0.0916 0.0067 0.4200 0.118 Uiso 1 1 calc R . . H60B H 0.1824 0.1226 0.4305 0.118 Uiso 1 1 calc R . . C59 C 0.2055(12) 0.0304(10) 0.4963(6) 0.099(5) Uani 1 1 d . . . H59A H 0.2275 0.0998 0.5225 0.118 Uiso 1 1 calc R . . H59B H 0.1334 -0.0157 0.5124 0.118 Uiso 1 1 calc R . . C58 C 0.3103(13) -0.0205(12) 0.4908(6) 0.107(5) Uani 1 1 d . . . H58A H 0.3806 0.0193 0.5190 0.129 Uiso 1 1 calc R . . H58B H 0.2870 -0.0942 0.5014 0.129 Uiso 1 1 calc R . . C57 C 0.3479(14) -0.0232(12) 0.4321(6) 0.128(7) Uani 1 1 d . . . H57A H 0.4311 0.0247 0.4312 0.154 Uiso 1 1 calc R . . H57B H 0.3562 -0.0968 0.4166 0.154 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 0.0234(4) 0.0395(4) 0.0574(4) 0.0038(3) -0.0002(3) 0.0008(3) I2 0.0234(4) 0.0409(5) 0.0540(5) -0.0052(3) -0.0030(3) 0.0021(3) Ga2 0.0216(5) 0.0236(5) 0.0346(6) -0.0008(4) -0.0027(5) 0.0054(4) Ga1 0.0206(5) 0.0242(5) 0.0338(6) 0.0005(4) 0.0012(5) 0.0059(4) N4 0.019(3) 0.022(3) 0.025(4) 0.003(3) -0.004(3) 0.003(2) N1 0.018(3) 0.028(3) 0.013(4) 0.004(3) 0.003(3) 0.006(3) N3 0.016(3) 0.024(3) 0.017(4) 0.000(3) 0.007(3) 0.002(2) C29 0.028(4) 0.024(4) 0.019(5) -0.005(3) 0.000(4) 0.001(3) C15 0.035(5) 0.023(4) 0.021(5) 0.006(3) -0.004(4) 0.011(3) C34 0.028(5) 0.032(5) 0.026(5) -0.002(4) -0.008(4) 0.004(4) C4 0.023(4) 0.026(5) 0.040(6) -0.007(4) 0.001(4) 0.005(4) C3 0.024(4) 0.024(4) 0.017(4) 0.003(3) 0.001(4) 0.008(3) C42 0.037(5) 0.019(4) 0.024(5) -0.001(3) -0.007(4) 0.001(3) C1 0.011(3) 0.018(4) 0.027(5) -0.003(3) 0.000(3) -0.001(3) C41 0.027(4) 0.035(5) 0.022(5) 0.002(4) -0.004(4) -0.009(4) C28 0.039(5) 0.021(4) 0.033(5) 0.003(4) 0.000(4) 0.006(3) N2 0.013(3) 0.029(3) 0.015(4) -0.002(3) -0.001(3) 0.003(2) C33 0.052(6) 0.023(4) 0.036(6) 0.003(4) -0.016(5) 0.014(4) C43 0.042(5) 0.061(6) 0.033(6) 0.014(5) -0.010(5) 0.006(5) C30 0.041(5) 0.017(4) 0.022(5) 0.003(3) -0.001(4) -0.002(3) C5 0.035(5) 0.032(5) 0.024(5) 0.006(4) 0.023(4) 0.011(4) C9 0.034(5) 0.029(5) 0.017(5) -0.006(4) 0.003(4) 0.003(4) C45 0.042(5) 0.039(5) 0.031(6) 0.001(4) 0.018(5) 0.005(4) C46 0.030(5) 0.027(5) 0.034(6) 0.001(4) 0.002(4) 0.008(4) C16 0.043(5) 0.035(5) 0.036(6) 0.004(4) -0.010(5) 0.014(4) C20 0.037(5) 0.047(6) 0.033(6) -0.009(4) 0.002(5) 0.004(4) C8 0.027(4) 0.034(5) 0.026(5) 0.006(4) -0.001(4) 0.007(3) C6 0.061(6) 0.029(5) 0.019(5) 0.000(4) -0.008(5) -0.001(4) C27 0.022(4) 0.026(4) 0.019(5) 0.004(3) -0.001(4) 0.000(3) C12 0.024(4) 0.045(5) 0.029(5) -0.017(4) 0.012(4) 0.014(4) C24 0.037(5) 0.051(6) 0.059(7) 0.010(5) -0.011(5) 0.014(5) C7 0.029(4) 0.042(5) 0.025(5) -0.010(4) 0.009(4) 0.012(4) C44 0.054(6) 0.041(5) 0.026(5) 0.003(4) -0.012(5) 0.000(4) C32 0.066(6) 0.024(4) 0.022(5) 0.007(4) -0.004(5) -0.006(4) C17 0.056(6) 0.071(7) 0.033(6) 0.015(5) -0.019(6) 0.017(5) C2 0.043(5) 0.035(5) 0.030(5) -0.006(4) -0.016(4) -0.006(4) C31 0.049(5) 0.039(5) 0.036(6) 0.015(4) -0.002(5) -0.010(4) C19 0.062(7) 0.084(8) 0.032(6) 0.015(5) 0.018(6) 0.002(6) C18 0.102(10) 0.106(10) 0.044(8) 0.047(7) -0.017(8) 0.000(8) C47 0.015(4) 0.061(6) 0.033(6) 0.009(4) 0.011(4) 0.018(4) C21 0.037(6) 0.059(6) 0.027(6) 0.015(5) 0.010(5) 0.018(5) C38 0.023(5) 0.029(5) 0.042(6) 0.011(4) 0.012(5) 0.005(4) C11 0.036(6) 0.072(7) 0.072(8) 0.005(6) -0.020(6) 0.015(5) C37 0.046(6) 0.075(8) 0.061(8) 0.028(6) -0.003(6) 0.005(6) C23 0.046(6) 0.055(7) 0.079(9) 0.003(6) 0.016(6) 0.013(5) C35 0.036(5) 0.058(6) 0.043(6) 0.016(5) -0.017(5) 0.000(5) C48 0.031(5) 0.059(7) 0.066(8) -0.002(5) -0.004(5) 0.014(5) C14 0.033(6) 0.073(8) 0.072(8) -0.015(6) 0.006(6) -0.024(5) C39 0.035(6) 0.084(8) 0.077(9) 0.016(7) 0.005(6) 0.011(5) C13 0.044(6) 0.066(7) 0.093(9) 0.004(6) -0.017(6) 0.024(5) C51 0.037(5) 0.050(6) 0.075(8) -0.003(5) 0.002(5) 0.016(4) C10 0.034(5) 0.065(7) 0.077(8) 0.021(6) 0.001(5) 0.007(5) C50 0.033(5) 0.055(6) 0.021(5) 0.000(4) -0.007(4) 0.013(5) C40 0.048(6) 0.060(7) 0.054(7) 0.001(5) -0.005(5) 0.021(5) C26 0.036(6) 0.079(8) 0.092(10) 0.003(7) -0.025(6) 0.001(6) C25 0.077(7) 0.066(7) 0.068(8) -0.005(6) -0.023(7) 0.032(6) C49 0.057(6) 0.052(6) 0.084(9) 0.002(6) -0.013(6) 0.026(5) C36 0.054(6) 0.069(7) 0.093(10) 0.009(6) 0.019(6) 0.038(6) C52 0.037(6) 0.083(8) 0.096(10) 0.043(7) 0.006(6) 0.005(6) C22 0.055(7) 0.101(9) 0.066(9) -0.030(7) 0.003(7) -0.002(7) O1 0.130(9) 0.205(12) 0.090(8) -0.003(8) -0.017(8) 0.063(8) C53 0.21(2) 0.120(13) 0.146(17) -0.070(12) -0.092(16) 0.093(13) C54 0.149(16) 0.108(12) 0.106(14) -0.033(10) -0.033(13) -0.029(11) C56 0.175(18) 0.29(2) 0.084(13) 0.015(14) 0.012(14) 0.189(19) C55 0.138(18) 0.29(3) 0.119(19) 0.03(2) 0.010(16) -0.041(18) O2 0.157(11) 0.216(13) 0.052(7) 0.041(8) -0.042(8) -0.107(10) C60 0.132(14) 0.055(8) 0.108(14) 0.039(8) -0.035(11) 0.010(8) C59 0.097(10) 0.136(12) 0.060(9) -0.007(9) -0.011(8) 0.031(10) C58 0.086(9) 0.205(17) 0.056(10) 0.053(10) 0.020(8) 0.069(11) C57 0.119(12) 0.164(14) 0.047(9) -0.068(9) 0.023(9) -0.060(11) _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 2.5495(13) . ? I2 Ga2 2.5501(13) . ? Ga2 N3 1.964(5) . ? Ga2 N4 2.034(6) . ? Ga2 Ga1 2.4235(13) . ? Ga2 O2 2.904(11) . ? Ga1 N1 1.995(6) . ? Ga1 N2 2.003(6) . ? Ga1 O2 3.148(12) . ? N4 C27 1.326(8) . ? N4 C41 1.420(10) . ? N1 C1 1.297(9) . ? N1 C3 1.450(9) . ? N3 C27 1.330(9) . ? N3 C29 1.440(9) . ? C29 C30 1.399(10) . ? C29 C34 1.400(10) . ? C15 C20 1.370(11) . ? C15 C16 1.392(10) . ? C15 N2 1.449(9) . ? C34 C33 1.359(11) . ? C34 C35 1.495(12) . ? C4 C3 1.365(11) . ? C4 C5 1.404(11) . ? C4 C12 1.530(9) . ? C3 C8 1.428(9) . ? C42 C43 1.398(12) . ? C42 C41 1.409(9) . ? C42 C50 1.497(12) . ? C1 N2 1.308(8) . ? C1 C2 1.510(9) . ? C41 C46 1.393(11) . ? C28 C27 1.488(9) . ? C33 C32 1.376(12) . ? C43 C44 1.377(12) . ? C30 C31 1.367(10) . ? C30 C38 1.499(11) . ? C5 C6 1.363(10) . ? C9 C8 1.495(11) . ? C9 C11 1.510(10) . ? C9 C10 1.524(11) . ? C45 C44 1.359(10) . ? C45 C46 1.369(11) . ? C46 C47 1.519(10) . ? C16 C17 1.369(12) . ? C16 C24 1.511(13) . ? C20 C19 1.361(12) . ? C20 C21 1.525(11) . ? C8 C7 1.371(11) . ? C6 C7 1.395(11) . ? C12 C13 1.517(11) . ? C12 C14 1.531(12) . ? C24 C26 1.509(11) . ? C24 C25 1.522(12) . ? C32 C31 1.373(11) . ? C17 C18 1.333(15) . ? C19 C18 1.374(14) . ? C47 C48 1.515(11) . ? C47 C49 1.555(12) . ? C21 C22 1.483(11) . ? C21 C23 1.524(13) . ? C38 C39 1.452(13) . ? C38 C40 1.539(11) . ? C37 C35 1.517(11) . ? C35 C36 1.541(13) . ? C51 C50 1.502(11) . ? C50 C52 1.471(11) . ? O1 C53 1.382(16) . ? O1 C56 1.438(17) . ? C53 C54 1.36(2) . ? C54 C55 1.55(2) . ? C56 C55 1.36(2) . ? O2 C57 1.339(18) . ? O2 C60 1.375(18) . ? C60 C59 1.470(17) . ? C59 C58 1.419(16) . ? C58 C57 1.386(17) . ? 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 N3 Ga2 N4 65.8(2) . . ? N3 Ga2 Ga1 128.60(17) . . ? N4 Ga2 Ga1 119.28(15) . . ? N3 Ga2 I2 109.65(16) . . ? N4 Ga2 I2 105.00(16) . . ? Ga1 Ga2 I2 116.42(4) . . ? N3 Ga2 O2 83.9(3) . . ? N4 Ga2 O2 148.1(3) . . ? Ga1 Ga2 O2 71.8(4) . . ? I2 Ga2 O2 93.9(2) . . ? N1 Ga1 N2 65.1(2) . . ? N1 Ga1 Ga2 127.57(15) . . ? N2 Ga1 Ga2 121.93(18) . . ? N1 Ga1 I1 109.66(17) . . ? N2 Ga1 I1 104.76(15) . . ? Ga2 Ga1 I1 116.25(4) . . ? N1 Ga1 O2 89.5(3) . . ? N2 Ga1 O2 150.4(2) . . ? Ga2 Ga1 O2 61.2(3) . . ? I1 Ga1 O2 97.8(2) . . ? C27 N4 C41 124.8(6) . . ? C27 N4 Ga2 90.7(5) . . ? C41 N4 Ga2 144.3(5) . . ? C1 N1 C3 123.3(6) . . ? C1 N1 Ga1 92.2(4) . . ? C3 N1 Ga1 143.7(5) . . ? C27 N3 C29 122.0(6) . . ? C27 N3 Ga2 93.7(4) . . ? C29 N3 Ga2 143.5(5) . . ? C30 C29 C34 121.3(7) . . ? C30 C29 N3 118.5(6) . . ? C34 C29 N3 120.1(7) . . ? C20 C15 C16 122.7(8) . . ? C20 C15 N2 118.7(6) . . ? C16 C15 N2 118.6(8) . . ? C33 C34 C29 117.8(8) . . ? C33 C34 C35 118.0(7) . . ? C29 C34 C35 124.2(8) . . ? C3 C4 C5 119.6(7) . . ? C3 C4 C12 122.2(7) . . ? C5 C4 C12 118.2(7) . . ? C4 C3 C8 121.7(7) . . ? C4 C3 N1 121.4(6) . . ? C8 C3 N1 116.8(7) . . ? C43 C42 C41 115.5(8) . . ? C43 C42 C50 121.1(7) . . ? C41 C42 C50 123.3(7) . . ? N1 C1 N2 111.3(6) . . ? N1 C1 C2 124.1(7) . . ? N2 C1 C2 124.6(7) . . ? C46 C41 C42 123.5(7) . . ? C46 C41 N4 120.0(6) . . ? C42 C41 N4 116.5(7) . . ? C1 N2 C15 124.6(6) . . ? C1 N2 Ga1 91.4(4) . . ? C15 N2 Ga1 143.9(4) . . ? C34 C33 C32 122.5(8) . . ? C44 C43 C42 122.1(7) . . ? C31 C30 C29 117.5(7) . . ? C31 C30 C38 121.4(8) . . ? C29 C30 C38 121.1(7) . . ? C6 C5 C4 120.4(8) . . ? C8 C9 C11 114.4(7) . . ? C8 C9 C10 111.6(7) . . ? C11 C9 C10 108.9(7) . . ? C44 C45 C46 123.5(9) . . ? C45 C46 C41 116.4(7) . . ? C45 C46 C47 120.8(8) . . ? C41 C46 C47 122.8(8) . . ? C17 C16 C15 116.4(9) . . ? C17 C16 C24 119.7(8) . . ? C15 C16 C24 123.8(8) . . ? C19 C20 C15 117.8(8) . . ? C19 C20 C21 121.5(9) . . ? C15 C20 C21 120.7(8) . . ? C7 C8 C3 116.0(7) . . ? C7 C8 C9 122.2(6) . . ? C3 C8 C9 121.9(7) . . ? C5 C6 C7 118.8(7) . . ? N4 C27 N3 109.8(6) . . ? N4 C27 C28 124.8(7) . . ? N3 C27 C28 125.4(7) . . ? C13 C12 C4 112.9(6) . . ? C13 C12 C14 109.5(8) . . ? C4 C12 C14 109.8(7) . . ? C26 C24 C16 112.4(8) . . ? C26 C24 C25 108.6(8) . . ? C16 C24 C25 110.6(8) . . ? C8 C7 C6 123.5(7) . . ? C45 C44 C43 119.0(8) . . ? C31 C32 C33 118.3(7) . . ? C18 C17 C16 121.9(9) . . ? C30 C31 C32 122.6(9) . . ? C20 C19 C18 120.4(11) . . ? C17 C18 C19 120.6(10) . . ? C48 C47 C46 110.6(7) . . ? C48 C47 C49 107.7(7) . . ? C46 C47 C49 111.5(7) . . ? C22 C21 C23 110.5(8) . . ? C22 C21 C20 109.3(8) . . ? C23 C21 C20 113.0(7) . . ? C39 C38 C30 115.4(8) . . ? C39 C38 C40 107.7(8) . . ? C30 C38 C40 110.6(7) . . ? C34 C35 C37 111.4(8) . . ? C34 C35 C36 113.4(8) . . ? C37 C35 C36 110.7(8) . . ? C52 C50 C42 112.3(8) . . ? C52 C50 C51 111.4(7) . . ? C42 C50 C51 113.1(8) . . ? C53 O1 C56 106.8(13) . . ? C54 C53 O1 111.7(16) . . ? C53 C54 C55 99.5(15) . . ? C55 C56 O1 106.1(15) . . ? C56 C55 C54 109.2(17) . . ? C57 O2 C60 108.0(11) . . ? C57 O2 Ga2 112.3(11) . . ? C60 O2 Ga2 139.6(11) . . ? C57 O2 Ga1 154.6(10) . . ? C60 O2 Ga1 93.6(11) . . ? Ga2 O2 Ga1 46.99(15) . . ? O2 C60 C59 109.7(12) . . ? C58 C59 C60 102.1(12) . . ? C57 C58 C59 109.4(12) . . ? O2 C57 C58 110.0(14) . . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 0.733 _refine_diff_density_min -0.843 _refine_diff_density_rms 0.103 _exptl_crystal_recrystallization_method 'from tetrahydrofurane' # Attachment '- 3 - TZE67A.CIF' data_3 _database_code_depnum_ccdc_archive 'CCDC 811976' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis-(N,N'-dicyclohexylneopentylamidinato-iodo-gallium(II)) -N,N'-dicyclohexylneopentylamidinato-gallium(I) ; _chemical_name_common ; bis-(N,N'-dicyclohexylneopentylamidinato-iodo-gallium(ii)) - N,N'-dicyclohexylneopentylamidinato-gallium(i) ; _chemical_melting_point '603 (dec)' _chemical_formula_moiety 'C51 H93 Ga3 I2 N6' _chemical_formula_sum 'C51 H93 Ga3 I2 N6' _chemical_formula_weight 1253.27 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.293(3) _cell_length_b 13.507(3) _cell_length_c 18.197(4) _cell_angle_alpha 81.06(3) _cell_angle_beta 77.42(3) _cell_angle_gamma 69.29(3) _cell_volume 2748.2(10) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plates _exptl_crystal_colour colourless _exptl_crystal_size_max 0.437 _exptl_crystal_size_mid 0.345 _exptl_crystal_size_min 0.074 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 2.622 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.3697 _exptl_absorpt_correction_T_max 0.7698 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26791 _diffrn_reflns_av_R_equivalents 0.0802 _diffrn_reflns_av_sigmaI/netI 0.1954 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 28.16 _reflns_number_total 12307 _reflns_number_gt 5380 _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^)+(0.0232P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12307 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1079 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0765 _refine_ls_wR_factor_gt 0.0672 _refine_ls_goodness_of_fit_ref 0.656 _refine_ls_restrained_S_all 0.656 _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 -0.06368(3) 0.69167(3) 0.34855(2) 0.03831(12) Uani 1 1 d . . . I2 I 0.51092(4) 0.58403(3) 0.39204(2) 0.03956(12) Uani 1 1 d . . . Ga1 Ga 0.14076(5) 0.61491(4) 0.26398(3) 0.02273(14) Uani 1 1 d . . . Ga2 Ga 0.26559(5) 0.72290(4) 0.25107(3) 0.02086(14) Uani 1 1 d . . . Ga3 Ga 0.33999(5) 0.74776(4) 0.35678(3) 0.02254(14) Uani 1 1 d . . . N1 N 0.1117(4) 0.5501(3) 0.1847(2) 0.0244(10) Uani 1 1 d . . . N2 N 0.1860(4) 0.4595(3) 0.2795(2) 0.0245(11) Uani 1 1 d . . . N3 N 0.2273(4) 0.8493(3) 0.1781(2) 0.0223(10) Uani 1 1 d . . . N4 N 0.3809(4) 0.7133(3) 0.1556(2) 0.0245(10) Uani 1 1 d . . . N5 N 0.3695(4) 0.8755(3) 0.3712(2) 0.0268(11) Uani 1 1 d . . . N6 N 0.2451(4) 0.8144(3) 0.4498(2) 0.0247(11) Uani 1 1 d . . . C1 C 0.1540(4) 0.4524(4) 0.2159(3) 0.0211(12) Uani 1 1 d . . . C2 C 0.1592(5) 0.3537(4) 0.1820(3) 0.0267(13) Uani 1 1 d . . . C3 C 0.0366(5) 0.3634(4) 0.1692(3) 0.0343(15) Uani 1 1 d . . . H3A H -0.0182 0.3706 0.2175 0.051 Uiso 1 1 calc R . . H3B H 0.0415 0.2997 0.1473 0.051 Uiso 1 1 calc R . . H3C H 0.0081 0.4261 0.1344 0.051 Uiso 1 1 calc R . . C4 C 0.1988(5) 0.2493(4) 0.2312(3) 0.0341(15) Uani 1 1 d . . . H4A H 0.1438 0.2535 0.2794 0.051 Uiso 1 1 calc R . . H4B H 0.2783 0.2368 0.2407 0.051 Uiso 1 1 calc R . . H4C H 0.1998 0.1906 0.2051 0.051 Uiso 1 1 calc R . . C5 C 0.2482(5) 0.3427(5) 0.1078(3) 0.0374(15) Uani 1 1 d . . . H5A H 0.3255 0.3366 0.1180 0.056 Uiso 1 1 calc R . . H5B H 0.2213 0.4055 0.0728 0.056 Uiso 1 1 calc R . . H5C H 0.2548 0.2791 0.0853 0.056 Uiso 1 1 calc R . . C6 C 0.0608(5) 0.5906(4) 0.1155(3) 0.0259(13) Uani 1 1 d . . . H6A H 0.0708 0.5295 0.0870 0.031 Uiso 1 1 calc R . . C7 C 0.1228(5) 0.6611(4) 0.0673(3) 0.0345(15) Uani 1 1 d . . . H7A H 0.2073 0.6196 0.0523 0.041 Uiso 1 1 calc R . . H7B H 0.1177 0.7189 0.0967 0.041 Uiso 1 1 calc R . . C8 C 0.0681(5) 0.7091(5) -0.0036(3) 0.0392(16) Uani 1 1 d . . . H8A H 0.1085 0.7579 -0.0335 0.047 Uiso 1 1 calc R . . H8B H 0.0798 0.6516 -0.0354 0.047 Uiso 1 1 calc R . . C9 C -0.0633(6) 0.7694(5) 0.0172(3) 0.0430(17) Uani 1 1 d . . . H9A H -0.0748 0.8313 0.0444 0.052 Uiso 1 1 calc R . . H9B H -0.0977 0.7961 -0.0294 0.052 Uiso 1 1 calc R . . C10 C -0.1252(5) 0.6988(5) 0.0659(3) 0.0467(18) Uani 1 1 d . . . H10A H -0.1194 0.6403 0.0370 0.056 Uiso 1 1 calc R . . H10B H -0.2100 0.7400 0.0804 0.056 Uiso 1 1 calc R . . C11 C -0.0716(5) 0.6518(5) 0.1378(3) 0.0380(15) Uani 1 1 d . . . H11A H -0.0825 0.7097 0.1690 0.046 Uiso 1 1 calc R . . H11B H -0.1122 0.6034 0.1681 0.046 Uiso 1 1 calc R . . C12 C 0.2504(4) 0.3790(4) 0.3328(3) 0.0213(12) Uani 1 1 d . . . H12A H 0.2204 0.3175 0.3419 0.026 Uiso 1 1 calc R . . C13 C 0.3834(4) 0.3393(4) 0.3032(3) 0.0291(14) Uani 1 1 d . . . H13A H 0.3990 0.3077 0.2548 0.035 Uiso 1 1 calc R . . H13B H 0.4136 0.3999 0.2936 0.035 Uiso 1 1 calc R . . C14 C 0.4476(5) 0.2569(4) 0.3599(3) 0.0360(15) Uani 1 1 d . . . H14A H 0.4213 0.1942 0.3669 0.043 Uiso 1 1 calc R . . H14B H 0.5336 0.2334 0.3403 0.043 Uiso 1 1 calc R . . C15 C 0.4236(5) 0.3014(4) 0.4345(3) 0.0355(15) Uani 1 1 d . . . H15A H 0.4590 0.3582 0.4286 0.043 Uiso 1 1 calc R . . H15B H 0.4616 0.2447 0.4714 0.043 Uiso 1 1 calc R . . C16 C 0.2909(5) 0.3468(4) 0.4650(3) 0.0345(15) Uani 1 1 d . . . H16A H 0.2573 0.2883 0.4779 0.041 Uiso 1 1 calc R . . H16B H 0.2785 0.3815 0.5116 0.041 Uiso 1 1 calc R . . C17 C 0.2276(5) 0.4273(4) 0.4067(3) 0.0275(13) Uani 1 1 d . . . H17A H 0.1416 0.4525 0.4264 0.033 Uiso 1 1 calc R . . H17B H 0.2553 0.4893 0.3978 0.033 Uiso 1 1 calc R . . C18 C 0.3225(5) 0.8107(4) 0.1263(3) 0.0227(12) Uani 1 1 d . . . C19 C 0.3633(5) 0.8609(4) 0.0487(3) 0.0285(13) Uani 1 1 d . . . C20 C 0.3443(6) 0.8042(5) -0.0107(3) 0.0454(17) Uani 1 1 d . . . H20A H 0.3857 0.7277 -0.0029 0.068 Uiso 1 1 calc R . . H20B H 0.3752 0.8310 -0.0611 0.068 Uiso 1 1 calc R . . H20C H 0.2596 0.8171 -0.0064 0.068 Uiso 1 1 calc R . . C21 C 0.2974(5) 0.9793(4) 0.0343(3) 0.0414(16) Uani 1 1 d . . . H21A H 0.3072 1.0181 0.0724 0.062 Uiso 1 1 calc R . . H21B H 0.2132 0.9908 0.0376 0.062 Uiso 1 1 calc R . . H21C H 0.3294 1.0052 -0.0162 0.062 Uiso 1 1 calc R . . C22 C 0.4917(5) 0.8506(5) 0.0394(3) 0.0402(16) Uani 1 1 d . . . H22A H 0.5390 0.7757 0.0479 0.060 Uiso 1 1 calc R . . H22B H 0.5012 0.8915 0.0762 0.060 Uiso 1 1 calc R . . H22C H 0.5185 0.8780 -0.0118 0.060 Uiso 1 1 calc R . . C23 C 0.1296(4) 0.9506(4) 0.1814(3) 0.0232(12) Uani 1 1 d . . . H23A H 0.1590 1.0088 0.1538 0.028 Uiso 1 1 calc R . . C24 C 0.0827(5) 0.9727(4) 0.2642(3) 0.0318(14) Uani 1 1 d . . . H24A H 0.0540 0.9149 0.2918 0.038 Uiso 1 1 calc R . . H24B H 0.1469 0.9751 0.2879 0.038 Uiso 1 1 calc R . . C25 C -0.0178(5) 1.0781(5) 0.2694(4) 0.0468(17) Uani 1 1 d . . . H25A H -0.0469 1.0929 0.3231 0.056 Uiso 1 1 calc R . . H25B H 0.0118 1.1358 0.2427 0.056 Uiso 1 1 calc R . . C26 C -0.1158(6) 1.0766(5) 0.2357(4) 0.057(2) Uani 1 1 d . . . H26A H -0.1789 1.1468 0.2386 0.068 Uiso 1 1 calc R . . H26B H -0.1495 1.0227 0.2649 0.068 Uiso 1 1 calc R . . C27 C -0.0743(5) 1.0512(5) 0.1539(4) 0.056(2) Uani 1 1 d . . . H27A H -0.0498 1.1096 0.1235 0.067 Uiso 1 1 calc R . . H27B H -0.1404 1.0455 0.1339 0.067 Uiso 1 1 calc R . . C28 C 0.0305(5) 0.9458(5) 0.1464(3) 0.0383(15) Uani 1 1 d . . . H28A H 0.0038 0.8861 0.1721 0.046 Uiso 1 1 calc R . . H28B H 0.0596 0.9332 0.0924 0.046 Uiso 1 1 calc R . . C29 C 0.4835(5) 0.6279(4) 0.1229(3) 0.0270(13) Uani 1 1 d . . . H29A H 0.5045 0.6471 0.0676 0.032 Uiso 1 1 calc R . . C30 C 0.4501(5) 0.5292(4) 0.1340(3) 0.0375(15) Uani 1 1 d . . . H30A H 0.3876 0.5398 0.1043 0.045 Uiso 1 1 calc R . . H30B H 0.4173 0.5168 0.1880 0.045 Uiso 1 1 calc R . . C31 C 0.5540(6) 0.4324(5) 0.1100(4) 0.0513(18) Uani 1 1 d . . . H31A H 0.5290 0.3688 0.1214 0.062 Uiso 1 1 calc R . . H31B H 0.5810 0.4409 0.0548 0.062 Uiso 1 1 calc R . . C32 C 0.6539(6) 0.4168(5) 0.1500(4) 0.060(2) Uani 1 1 d . . . H32A H 0.7218 0.3548 0.1316 0.072 Uiso 1 1 calc R . . H32B H 0.6291 0.4018 0.2049 0.072 Uiso 1 1 calc R . . C33 C 0.6911(5) 0.5136(5) 0.1366(4) 0.057(2) Uani 1 1 d . . . H33A H 0.7232 0.5246 0.0823 0.069 Uiso 1 1 calc R . . H33B H 0.7544 0.5027 0.1657 0.069 Uiso 1 1 calc R . . C34 C 0.5879(5) 0.6106(5) 0.1604(4) 0.0442(17) Uani 1 1 d . . . H34A H 0.6135 0.6738 0.1477 0.053 Uiso 1 1 calc R . . H34B H 0.5630 0.6030 0.2160 0.053 Uiso 1 1 calc R . . C35 C 0.2898(4) 0.8943(4) 0.4339(3) 0.0226(12) Uani 1 1 d . . . C36 C 0.2510(5) 0.9935(4) 0.4761(3) 0.0254(13) Uani 1 1 d . . . C37 C 0.1992(5) 1.0908(4) 0.4212(3) 0.0362(15) Uani 1 1 d . . . H37A H 0.2577 1.0910 0.3751 0.054 Uiso 1 1 calc R . . H37B H 0.1795 1.1563 0.4455 0.054 Uiso 1 1 calc R . . H37C H 0.1277 1.0865 0.4084 0.054 Uiso 1 1 calc R . . C38 C 0.3559(5) 1.0025(4) 0.5029(3) 0.0381(16) Uani 1 1 d . . . H38A H 0.3870 0.9403 0.5375 0.057 Uiso 1 1 calc R . . H38B H 0.3304 1.0671 0.5292 0.057 Uiso 1 1 calc R . . H38C H 0.4176 1.0059 0.4593 0.057 Uiso 1 1 calc R . . C39 C 0.1540(5) 0.9987(4) 0.5452(3) 0.0375(15) Uani 1 1 d . . . H39A H 0.1820 0.9388 0.5822 0.056 Uiso 1 1 calc R . . H39B H 0.0840 0.9949 0.5300 0.056 Uiso 1 1 calc R . . H39C H 0.1337 1.0656 0.5679 0.056 Uiso 1 1 calc R . . C40 C 0.4421(4) 0.9359(4) 0.3285(3) 0.0219(12) Uani 1 1 d . . . H40A H 0.4220 1.0031 0.3527 0.026 Uiso 1 1 calc R . . C41 C 0.5720(5) 0.8728(5) 0.3279(3) 0.0370(15) Uani 1 1 d . . . H41A H 0.5871 0.8581 0.3804 0.044 Uiso 1 1 calc R . . H41B H 0.5909 0.8038 0.3073 0.044 Uiso 1 1 calc R . . C42 C 0.6521(5) 0.9311(5) 0.2810(4) 0.0504(18) Uani 1 1 d . . . H42A H 0.6386 0.9971 0.3041 0.060 Uiso 1 1 calc R . . H42B H 0.7356 0.8861 0.2807 0.060 Uiso 1 1 calc R . . C43 C 0.6294(6) 0.9584(6) 0.2008(4) 0.0522(18) Uani 1 1 d . . . H43A H 0.6512 0.8923 0.1759 0.063 Uiso 1 1 calc R . . H43B H 0.6791 1.0004 0.1722 0.063 Uiso 1 1 calc R . . C44 C 0.5007(5) 1.0216(5) 0.1998(3) 0.0400(16) Uani 1 1 d . . . H44A H 0.4814 1.0912 0.2196 0.048 Uiso 1 1 calc R . . H44B H 0.4867 1.0349 0.1470 0.048 Uiso 1 1 calc R . . C45 C 0.4210(5) 0.9636(5) 0.2469(3) 0.0340(14) Uani 1 1 d . . . H45A H 0.4347 0.8975 0.2239 0.041 Uiso 1 1 calc R . . H45B H 0.3376 1.0086 0.2467 0.041 Uiso 1 1 calc R . . C46 C 0.1800(4) 0.7740(4) 0.5179(3) 0.0207(12) Uani 1 1 d . . . H46A H 0.1122 0.8342 0.5405 0.025 Uiso 1 1 calc R . . C47 C 0.2586(5) 0.7174(4) 0.5759(3) 0.0273(13) Uani 1 1 d . . . H47A H 0.3300 0.6630 0.5516 0.033 Uiso 1 1 calc R . . H47B H 0.2844 0.7693 0.5943 0.033 Uiso 1 1 calc R . . C48 C 0.1957(5) 0.6643(4) 0.6424(3) 0.0362(15) Uani 1 1 d . . . H48A H 0.2511 0.6250 0.6775 0.043 Uiso 1 1 calc R . . H48B H 0.1292 0.7192 0.6702 0.043 Uiso 1 1 calc R . . C49 C 0.1494(5) 0.5885(4) 0.6163(3) 0.0392(16) Uani 1 1 d . . . H49A H 0.2166 0.5298 0.5929 0.047 Uiso 1 1 calc R . . H49B H 0.1053 0.5575 0.6604 0.047 Uiso 1 1 calc R . . C50 C 0.0701(5) 0.6442(5) 0.5604(3) 0.0384(15) Uani 1 1 d . . . H50A H -0.0007 0.6987 0.5851 0.046 Uiso 1 1 calc R . . H50C H 0.0436 0.5925 0.5424 0.046 Uiso 1 1 calc R . . C51 C 0.1338(5) 0.6974(4) 0.4930(3) 0.0311(14) Uani 1 1 d . . . H51C H 0.2005 0.6422 0.4656 0.037 Uiso 1 1 calc R . . H51A H 0.0786 0.7359 0.4577 0.037 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 0.0254(2) 0.0448(3) 0.0417(2) -0.01042(19) -0.00414(19) -0.00630(19) I2 0.0399(2) 0.0282(2) 0.0403(2) 0.00116(18) -0.0143(2) 0.00385(18) Ga1 0.0244(3) 0.0197(3) 0.0255(3) 0.0000(2) -0.0082(3) -0.0076(3) Ga2 0.0222(3) 0.0192(3) 0.0203(3) -0.0002(2) -0.0041(3) -0.0062(3) Ga3 0.0261(3) 0.0194(3) 0.0224(3) -0.0004(2) -0.0065(3) -0.0073(3) N1 0.029(3) 0.014(2) 0.026(2) 0.0091(18) -0.013(2) -0.0027(19) N2 0.026(2) 0.026(3) 0.022(2) -0.0043(19) -0.011(2) -0.004(2) N3 0.021(2) 0.019(2) 0.024(2) -0.0025(19) 0.002(2) -0.005(2) N4 0.028(3) 0.017(2) 0.023(2) 0.0008(19) -0.004(2) -0.003(2) N5 0.025(2) 0.031(3) 0.020(2) -0.005(2) 0.000(2) -0.005(2) N6 0.031(3) 0.021(2) 0.024(2) 0.0014(19) -0.008(2) -0.011(2) C1 0.019(3) 0.021(3) 0.024(3) 0.000(2) -0.001(2) -0.010(2) C2 0.033(3) 0.021(3) 0.030(3) -0.004(2) -0.008(3) -0.012(3) C3 0.042(4) 0.033(3) 0.038(3) 0.000(3) -0.015(3) -0.022(3) C4 0.043(4) 0.023(3) 0.038(3) 0.002(3) -0.017(3) -0.010(3) C5 0.043(4) 0.041(4) 0.030(3) -0.012(3) -0.001(3) -0.017(3) C6 0.030(3) 0.030(3) 0.020(3) -0.001(2) -0.011(3) -0.010(3) C7 0.029(3) 0.035(3) 0.040(3) 0.009(3) -0.018(3) -0.010(3) C8 0.044(4) 0.040(4) 0.036(3) 0.018(3) -0.018(3) -0.020(3) C9 0.053(4) 0.033(4) 0.041(4) 0.003(3) -0.028(4) -0.003(3) C10 0.030(3) 0.067(5) 0.039(4) 0.000(3) -0.018(3) -0.005(3) C11 0.026(3) 0.050(4) 0.035(3) 0.005(3) -0.010(3) -0.010(3) C12 0.026(3) 0.016(3) 0.025(3) 0.006(2) -0.011(3) -0.010(2) C13 0.029(3) 0.032(3) 0.027(3) -0.001(2) -0.009(3) -0.010(3) C14 0.031(3) 0.034(3) 0.036(3) 0.004(3) -0.015(3) -0.001(3) C15 0.036(4) 0.030(3) 0.037(3) 0.011(3) -0.021(3) -0.004(3) C16 0.046(4) 0.029(3) 0.029(3) 0.002(3) -0.016(3) -0.010(3) C17 0.030(3) 0.029(3) 0.025(3) 0.001(2) -0.008(3) -0.011(3) C18 0.025(3) 0.020(3) 0.025(3) -0.006(2) -0.003(3) -0.009(2) C19 0.032(3) 0.023(3) 0.028(3) 0.001(2) -0.002(3) -0.009(3) C20 0.070(5) 0.046(4) 0.024(3) 0.002(3) -0.009(3) -0.025(4) C21 0.045(4) 0.030(4) 0.038(4) 0.008(3) 0.002(3) -0.009(3) C22 0.047(4) 0.037(4) 0.029(3) 0.005(3) 0.009(3) -0.016(3) C23 0.021(3) 0.012(3) 0.030(3) 0.007(2) -0.003(3) -0.004(2) C24 0.031(3) 0.022(3) 0.038(3) -0.006(3) -0.002(3) -0.005(3) C25 0.038(4) 0.025(3) 0.060(4) -0.006(3) 0.016(3) -0.005(3) C26 0.031(4) 0.038(4) 0.080(5) 0.003(4) 0.006(4) 0.002(3) C27 0.028(4) 0.049(4) 0.076(5) 0.023(4) -0.021(4) 0.000(3) C28 0.033(3) 0.038(4) 0.045(4) 0.001(3) -0.016(3) -0.010(3) C29 0.029(3) 0.021(3) 0.022(3) -0.002(2) 0.005(3) -0.003(2) C30 0.035(3) 0.029(3) 0.039(4) -0.005(3) 0.000(3) -0.002(3) C31 0.053(4) 0.029(4) 0.059(4) -0.013(3) 0.013(4) -0.008(3) C32 0.038(4) 0.035(4) 0.073(5) 0.003(4) 0.008(4) 0.015(3) C33 0.028(4) 0.047(5) 0.079(5) -0.002(4) 0.002(4) 0.002(3) C34 0.030(3) 0.043(4) 0.057(4) -0.011(3) -0.013(3) -0.003(3) C35 0.021(3) 0.020(3) 0.028(3) 0.007(2) -0.012(3) -0.008(2) C36 0.031(3) 0.018(3) 0.030(3) 0.003(2) -0.009(3) -0.011(2) C37 0.036(3) 0.017(3) 0.054(4) -0.006(3) -0.016(3) -0.001(3) C38 0.047(4) 0.033(3) 0.041(4) -0.007(3) -0.020(3) -0.012(3) C39 0.044(4) 0.022(3) 0.042(4) -0.016(3) -0.004(3) -0.003(3) C40 0.021(3) 0.018(3) 0.028(3) 0.006(2) -0.002(3) -0.012(2) C41 0.023(3) 0.038(4) 0.045(4) 0.010(3) -0.008(3) -0.010(3) C42 0.027(4) 0.054(4) 0.069(5) 0.008(4) -0.011(4) -0.016(3) C43 0.039(4) 0.057(5) 0.059(5) 0.002(4) 0.008(4) -0.026(4) C44 0.042(4) 0.043(4) 0.037(4) 0.013(3) -0.008(3) -0.022(3) C45 0.036(3) 0.039(4) 0.033(3) 0.007(3) -0.011(3) -0.020(3) C46 0.022(3) 0.014(3) 0.020(3) -0.004(2) -0.001(2) 0.001(2) C47 0.033(3) 0.023(3) 0.025(3) 0.001(2) -0.013(3) -0.005(3) C48 0.050(4) 0.025(3) 0.027(3) 0.004(3) -0.005(3) -0.008(3) C49 0.042(4) 0.025(3) 0.038(4) -0.002(3) 0.010(3) -0.005(3) C50 0.030(3) 0.036(4) 0.048(4) -0.005(3) 0.004(3) -0.016(3) C51 0.029(3) 0.036(3) 0.032(3) 0.000(3) -0.002(3) -0.018(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 I1 Ga1 2.5939(13) . ? I2 Ga3 2.5646(12) . ? Ga1 N1 1.953(4) . ? Ga1 N2 1.963(4) . ? Ga1 Ga2 2.4202(10) . ? Ga1 C1 2.428(5) . ? Ga2 N3 1.975(4) . ? Ga2 N4 1.978(4) . ? Ga2 Ga3 2.4154(9) . ? Ga2 C18 2.472(5) . ? Ga3 N5 1.950(4) . ? Ga3 N6 1.976(4) . ? Ga3 C35 2.427(5) . ? N1 C1 1.322(6) . ? N1 C6 1.470(5) . ? N2 C1 1.329(5) . ? N2 C12 1.464(6) . ? N3 C18 1.331(6) . ? N3 C23 1.465(6) . ? N4 C18 1.346(6) . ? N4 C29 1.460(6) . ? N5 C35 1.324(6) . ? N5 C40 1.442(7) . ? N6 C35 1.342(6) . ? N6 C46 1.463(7) . ? C1 C2 1.530(7) . ? C2 C4 1.530(7) . ? C2 C5 1.531(8) . ? C2 C3 1.531(7) . ? C6 C7 1.489(8) . ? C6 C11 1.537(7) . ? C7 C8 1.533(6) . ? C8 C9 1.522(8) . ? C9 C10 1.494(9) . ? C10 C11 1.539(7) . ? C12 C17 1.514(6) . ? C12 C13 1.529(7) . ? C13 C14 1.519(7) . ? C14 C15 1.498(7) . ? C15 C16 1.532(8) . ? C16 C17 1.521(6) . ? C18 C19 1.529(7) . ? C19 C22 1.509(8) . ? C19 C20 1.518(7) . ? C19 C21 1.527(7) . ? C23 C28 1.517(7) . ? C23 C24 1.527(7) . ? C24 C25 1.519(7) . ? C25 C26 1.474(8) . ? C26 C27 1.517(9) . ? C27 C28 1.546(8) . ? C29 C30 1.502(8) . ? C29 C34 1.512(7) . ? C30 C31 1.511(8) . ? C31 C32 1.496(8) . ? C32 C33 1.501(9) . ? C33 C34 1.508(8) . ? C35 C36 1.524(7) . ? C36 C38 1.522(7) . ? C36 C39 1.524(8) . ? C36 C37 1.551(7) . ? C40 C41 1.519(7) . ? C40 C45 1.530(7) . ? C41 C42 1.514(8) . ? C42 C43 1.510(8) . ? C43 C44 1.511(8) . ? C44 C45 1.509(8) . ? C46 C51 1.508(7) . ? C46 C47 1.519(6) . ? C47 C48 1.513(8) . ? C48 C49 1.511(8) . ? C49 C50 1.493(7) . ? C50 C51 1.529(8) . ? 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 66.02(15) . . ? N1 Ga1 Ga2 127.91(14) . . ? N2 Ga1 Ga2 127.93(12) . . ? N1 Ga1 C1 32.90(15) . . ? N2 Ga1 C1 33.12(14) . . ? Ga2 Ga1 C1 136.66(13) . . ? N1 Ga1 I1 105.52(13) . . ? N2 Ga1 I1 107.06(14) . . ? Ga2 Ga1 I1 113.32(3) . . ? C1 Ga1 I1 110.00(13) . . ? N3 Ga2 N4 65.34(16) . . ? N3 Ga2 Ga3 113.95(12) . . ? N4 Ga2 Ga3 112.73(11) . . ? N3 Ga2 Ga1 114.48(12) . . ? N4 Ga2 Ga1 114.85(12) . . ? Ga3 Ga2 Ga1 122.20(4) . . ? N3 Ga2 C18 32.44(16) . . ? N4 Ga2 C18 32.90(15) . . ? Ga3 Ga2 C18 117.82(11) . . ? Ga1 Ga2 C18 119.97(11) . . ? N5 Ga3 N6 66.51(18) . . ? N5 Ga3 Ga2 125.74(12) . . ? N6 Ga3 Ga2 126.66(12) . . ? N5 Ga3 C35 32.99(17) . . ? N6 Ga3 C35 33.56(18) . . ? Ga2 Ga3 C35 133.75(10) . . ? N5 Ga3 I2 109.06(11) . . ? N6 Ga3 I2 109.06(11) . . ? Ga2 Ga3 I2 112.07(4) . . ? C35 Ga3 I2 114.16(10) . . ? C1 N1 C6 131.3(4) . . ? C1 N1 Ga1 93.7(3) . . ? C6 N1 Ga1 135.0(3) . . ? C1 N2 C12 132.2(4) . . ? C1 N2 Ga1 93.0(3) . . ? C12 N2 Ga1 134.0(3) . . ? C18 N3 C23 133.0(4) . . ? C18 N3 Ga2 94.8(3) . . ? C23 N3 Ga2 132.2(3) . . ? C18 N4 C29 131.7(4) . . ? C18 N4 Ga2 94.1(3) . . ? C29 N4 Ga2 133.7(3) . . ? C35 N5 C40 131.1(4) . . ? C35 N5 Ga3 93.7(3) . . ? C40 N5 Ga3 135.0(3) . . ? C35 N6 C46 134.1(4) . . ? C35 N6 Ga3 92.0(3) . . ? C46 N6 Ga3 131.9(3) . . ? N1 C1 N2 107.2(4) . . ? N1 C1 C2 123.5(4) . . ? N2 C1 C2 129.3(4) . . ? N1 C1 Ga1 53.4(2) . . ? N2 C1 Ga1 53.9(2) . . ? C2 C1 Ga1 176.8(3) . . ? C1 C2 C4 115.1(4) . . ? C1 C2 C5 107.6(4) . . ? C4 C2 C5 107.2(4) . . ? C1 C2 C3 110.5(4) . . ? C4 C2 C3 104.9(4) . . ? C5 C2 C3 111.5(4) . . ? N1 C6 C7 109.5(4) . . ? N1 C6 C11 108.8(4) . . ? C7 C6 C11 110.7(5) . . ? C6 C7 C8 111.1(4) . . ? C9 C8 C7 111.0(5) . . ? C10 C9 C8 110.5(5) . . ? C9 C10 C11 111.5(5) . . ? C6 C11 C10 109.4(5) . . ? N2 C12 C17 108.6(4) . . ? N2 C12 C13 112.0(4) . . ? C17 C12 C13 109.1(4) . . ? C14 C13 C12 110.6(5) . . ? C15 C14 C13 110.9(4) . . ? C14 C15 C16 111.9(4) . . ? C17 C16 C15 110.8(5) . . ? C12 C17 C16 111.1(4) . . ? N3 C18 N4 105.7(4) . . ? N3 C18 C19 129.9(4) . . ? N4 C18 C19 124.4(5) . . ? N3 C18 Ga2 52.7(3) . . ? N4 C18 Ga2 53.0(3) . . ? C19 C18 Ga2 177.3(4) . . ? C22 C19 C20 110.9(5) . . ? C22 C19 C21 105.7(5) . . ? C20 C19 C21 107.6(4) . . ? C22 C19 C18 110.3(4) . . ? C20 C19 C18 107.7(4) . . ? C21 C19 C18 114.8(4) . . ? N3 C23 C28 110.8(4) . . ? N3 C23 C24 108.5(4) . . ? C28 C23 C24 109.0(5) . . ? C25 C24 C23 109.6(4) . . ? C26 C25 C24 111.2(5) . . ? C25 C26 C27 111.2(6) . . ? C26 C27 C28 111.0(5) . . ? C23 C28 C27 110.2(5) . . ? N4 C29 C30 107.7(5) . . ? N4 C29 C34 110.6(4) . . ? C30 C29 C34 110.7(4) . . ? C29 C30 C31 112.3(5) . . ? C32 C31 C30 111.2(5) . . ? C31 C32 C33 111.0(5) . . ? C32 C33 C34 110.7(6) . . ? C33 C34 C29 112.8(5) . . ? N5 C35 N6 107.7(4) . . ? N5 C35 C36 125.2(5) . . ? N6 C35 C36 127.0(5) . . ? N5 C35 Ga3 53.3(3) . . ? N6 C35 Ga3 54.5(3) . . ? C36 C35 Ga3 174.0(3) . . ? C38 C36 C39 107.1(4) . . ? C38 C36 C35 110.0(4) . . ? C39 C36 C35 115.3(4) . . ? C38 C36 C37 110.9(5) . . ? C39 C36 C37 105.8(4) . . ? C35 C36 C37 107.7(4) . . ? N5 C40 C41 110.3(4) . . ? N5 C40 C45 111.1(4) . . ? C41 C40 C45 108.8(5) . . ? C42 C41 C40 112.3(5) . . ? C43 C42 C41 111.1(5) . . ? C42 C43 C44 110.6(5) . . ? C45 C44 C43 111.4(5) . . ? C44 C45 C40 112.1(4) . . ? N6 C46 C51 106.5(4) . . ? N6 C46 C47 111.8(4) . . ? C51 C46 C47 109.8(4) . . ? C48 C47 C46 112.0(4) . . ? C49 C48 C47 110.8(4) . . ? C50 C49 C48 110.9(5) . . ? C49 C50 C51 110.9(5) . . ? C46 C51 C50 111.4(4) . . ? _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 28.16 _diffrn_measured_fraction_theta_full 0.912 _refine_diff_density_max 0.946 _refine_diff_density_min -0.878 _refine_diff_density_rms 0.112 _exptl_crystal_recrystallization_method 'from toluene' # Attachment '- 3a - tze49a.CIF' data_3a _database_code_depnum_ccdc_archive 'CCDC 811977' #TrackingRef '- 3a - tze49a.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis-(N,N'-dicyclohexylneopentylamidinato-iodo-gallium(II))-N,N' -dicyclohexylneopentylamidinato-gallium(I) n-hexane solvate ; _chemical_name_common ; bis-(N,N'-dicyclohexylneopentylamidinato-iodo-gallium(ii))- N,N' -dicyclohexylneopentylamidinato-gallium(i) n-hexane solvate ; _chemical_melting_point '603 (dec)' _chemical_formula_moiety 'C51 H93 Ga3 I2 N6, C6 H14' _chemical_formula_sum 'C57 H107 Ga3 I2 N6' _chemical_formula_weight 1339.45 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.831(3) _cell_length_b 13.914(3) _cell_length_c 20.005(4) _cell_angle_alpha 83.48(3) _cell_angle_beta 83.11(3) _cell_angle_gamma 64.33(3) _cell_volume 3188.5(11) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plates _exptl_crystal_colour colourless _exptl_crystal_size_max 0.227 _exptl_crystal_size_mid 0.193 _exptl_crystal_size_min 0.071 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1380 _exptl_absorpt_coefficient_mu 2.264 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.5944 _exptl_absorpt_correction_T_max 0.8348 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25396 _diffrn_reflns_av_R_equivalents 0.1203 _diffrn_reflns_av_sigmaI/netI 0.2354 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 26.06 _reflns_number_total 11664 _reflns_number_gt 4596 _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^)+(0.0550P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11664 _refine_ls_number_parameters 578 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1554 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1416 _refine_ls_wR_factor_gt 0.1193 _refine_ls_goodness_of_fit_ref 0.756 _refine_ls_restrained_S_all 0.756 _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 1.10019(5) -0.23674(5) -0.33489(3) 0.08067(19) Uani 1 1 d . . . I2 I 1.20130(4) 0.07653(4) -0.11488(2) 0.04875(13) Uani 1 1 d . . . Ga1 Ga 1.22528(7) -0.13157(6) -0.33760(3) 0.0433(2) Uani 1 1 d . A . Ga2 Ga 1.34484(6) -0.17661(5) -0.24320(3) 0.02927(17) Uani 1 1 d . . . Ga3 Ga 1.27182(5) -0.12461(5) -0.12924(3) 0.02740(17) Uani 1 1 d . . . N1 N 1.2774(5) -0.1098(4) -0.4326(2) 0.057(2) Uani 1 1 d . . . N2 N 1.1369(6) 0.0141(5) -0.3782(2) 0.066(2) Uani 1 1 d . . . N3 N 1.4759(4) -0.3178(4) -0.2474(2) 0.0371(14) Uani 1 1 d . . . N4 N 1.4963(4) -0.1766(4) -0.2703(2) 0.0352(14) Uani 1 1 d . . . N5 N 1.3427(4) -0.2059(4) -0.0463(2) 0.0285(13) Uani 1 1 d . . . N6 N 1.1694(4) -0.1745(4) -0.0689(2) 0.0288(12) Uani 1 1 d . . . C1 C 1.2086(8) -0.0103(6) -0.4370(3) 0.068(3) Uani 1 1 d . A . C2 C 1.2075(10) 0.0672(7) -0.4986(4) 0.110(5) Uani 1 1 d . . . C3 C 1.1121(12) 0.1807(7) -0.4938(4) 0.183(7) Uani 1 1 d . A . H3A H 1.1256 0.2144 -0.4574 0.274 Uiso 1 1 calc R . . H3B H 1.0366 0.1781 -0.4844 0.274 Uiso 1 1 calc R . . H3C H 1.1128 0.2223 -0.5367 0.274 Uiso 1 1 calc R . . C4 C 1.3252(10) 0.0713(7) -0.5093(4) 0.123(4) Uani 1 1 d . A . H4A H 1.3384 0.0989 -0.4698 0.185 Uiso 1 1 calc R . . H4B H 1.3266 0.1184 -0.5494 0.185 Uiso 1 1 calc R . . H4C H 1.3863 -0.0008 -0.5157 0.185 Uiso 1 1 calc R . . C5 C 1.1818(9) 0.0253(8) -0.5604(4) 0.117(5) Uani 1 1 d . A . H5A H 1.1836 0.0717 -0.6008 0.176 Uiso 1 1 calc R . . H5B H 1.1049 0.0253 -0.5524 0.176 Uiso 1 1 calc R . . H5C H 1.2406 -0.0477 -0.5671 0.176 Uiso 1 1 calc R . . C6 C 1.3692(7) -0.1776(6) -0.4799(3) 0.069(3) Uani 1 1 d . . . H6A H 1.3760 -0.1318 -0.5210 0.083 Uiso 1 1 calc R . . C7 C 1.4853(8) -0.2312(7) -0.4503(3) 0.083(3) Uani 1 1 d . . . H7A H 1.5096 -0.1765 -0.4398 0.099 Uiso 1 1 calc R . . H7B H 1.4794 -0.2735 -0.4080 0.099 Uiso 1 1 calc R . . C8 C 1.5732(8) -0.3033(7) -0.5007(4) 0.090(4) Uani 1 1 d . . . H8A H 1.5837 -0.2587 -0.5408 0.107 Uiso 1 1 calc R . . H8B H 1.6486 -0.3402 -0.4804 0.107 Uiso 1 1 calc R . . C9 C 1.5421(10) -0.3845(7) -0.5229(5) 0.123(5) Uani 1 1 d . . . H9A H 1.5406 -0.4353 -0.4843 0.147 Uiso 1 1 calc R . . H9B H 1.6008 -0.4252 -0.5581 0.147 Uiso 1 1 calc R . . C10 C 1.4221(8) -0.3292(6) -0.5511(4) 0.085(3) Uani 1 1 d . . . H10A H 1.4263 -0.2842 -0.5925 0.102 Uiso 1 1 calc R . . H10B H 1.3995 -0.3840 -0.5635 0.102 Uiso 1 1 calc R . . C11 C 1.3326(8) -0.2616(6) -0.5012(4) 0.081(3) Uani 1 1 d . . . H11A H 1.3237 -0.3069 -0.4611 0.097 Uiso 1 1 calc R . . H11B H 1.2571 -0.2249 -0.5213 0.097 Uiso 1 1 calc R . . C12A C 1.0320(9) 0.1014(9) -0.3553(6) 0.022(3) Uiso 0.490(5) 1 d P A 1 H12A H 0.9870 0.1426 -0.3946 0.027 Uiso 0.490(5) 1 calc PR A 1 C13A C 1.0863(11) 0.1670(10) -0.3267(7) 0.047(4) Uiso 0.490(5) 1 d P A 1 H13A H 1.1330 0.1249 -0.2889 0.056 Uiso 0.490(5) 1 calc PR A 1 H13B H 1.1380 0.1833 -0.3623 0.056 Uiso 0.490(5) 1 calc PR A 1 C14A C 0.9887(16) 0.2719(15) -0.3018(10) 0.091(6) Uiso 0.490(5) 1 d P A 1 H14A H 1.0229 0.3130 -0.2825 0.110 Uiso 0.490(5) 1 calc PR A 1 H14B H 0.9453 0.3158 -0.3403 0.110 Uiso 0.490(5) 1 calc PR A 1 C15A C 0.9121(11) 0.2503(10) -0.2524(6) 0.041(4) Uiso 0.490(5) 1 d P A 1 H15A H 0.8511 0.3195 -0.2379 0.049 Uiso 0.490(5) 1 calc PR A 1 H15C H 0.9559 0.2124 -0.2127 0.049 Uiso 0.490(5) 1 calc PR A 1 C16A C 0.8418(11) 0.1735(11) -0.2752(7) 0.042(4) Uiso 0.490(5) 1 d P A 1 H16A H 0.7998 0.1523 -0.2358 0.050 Uiso 0.490(5) 1 calc PR A 1 H16B H 0.7884 0.2112 -0.3110 0.050 Uiso 0.490(5) 1 calc PR A 1 C17A C 0.9551(12) 0.0749(11) -0.3019(7) 0.055(4) Uiso 0.490(5) 1 d P A 1 H17A H 1.0011 0.0368 -0.2630 0.066 Uiso 0.490(5) 1 calc PR A 1 H17B H 0.9308 0.0249 -0.3197 0.066 Uiso 0.490(5) 1 calc PR A 1 C12B C 1.0541(11) 0.1182(11) -0.3556(6) 0.034(4) Uiso 0.510(5) 1 d P A 2 H12B H 1.0714 0.1788 -0.3769 0.041 Uiso 0.510(5) 1 calc PR A 2 C13B C 1.0492(11) 0.1100(10) -0.2807(6) 0.043(4) Uiso 0.510(5) 1 d P A 2 H13C H 1.0584 0.0373 -0.2637 0.052 Uiso 0.510(5) 1 calc PR A 2 H13D H 1.1146 0.1206 -0.2664 0.052 Uiso 0.510(5) 1 calc PR A 2 C14B C 0.9388(13) 0.1896(13) -0.2501(8) 0.068(5) Uiso 0.510(5) 1 d P A 2 H14C H 0.9314 0.1647 -0.2021 0.081 Uiso 0.510(5) 1 calc PR A 2 H14D H 0.9472 0.2571 -0.2505 0.081 Uiso 0.510(5) 1 calc PR A 2 C15B C 0.8411(13) 0.2130(13) -0.2748(8) 0.058(5) Uiso 0.510(5) 1 d P A 2 H15B H 0.7879 0.2865 -0.2629 0.070 Uiso 0.510(5) 1 calc PR A 2 H15D H 0.8085 0.1650 -0.2503 0.070 Uiso 0.510(5) 1 calc PR A 2 C16B C 0.8341(13) 0.2083(12) -0.3522(7) 0.068(5) Uiso 0.510(5) 1 d P A 2 H16C H 0.7658 0.1961 -0.3592 0.082 Uiso 0.510(5) 1 calc PR A 2 H16D H 0.8259 0.2769 -0.3767 0.082 Uiso 0.510(5) 1 calc PR A 2 C17B C 0.9428(11) 0.1188(11) -0.3787(7) 0.050(4) Uiso 0.510(5) 1 d P A 2 H17C H 0.9468 0.1250 -0.4286 0.060 Uiso 0.510(5) 1 calc PR A 2 H17D H 0.9396 0.0500 -0.3631 0.060 Uiso 0.510(5) 1 calc PR A 2 C18 C 1.5562(5) -0.2807(5) -0.2660(3) 0.0349(18) Uani 1 1 d . . . C19 C 1.6848(6) -0.3484(5) -0.2770(3) 0.047(2) Uani 1 1 d . . . C20 C 1.7358(6) -0.4072(7) -0.2118(4) 0.076(3) Uani 1 1 d . . . H20A H 1.7228 -0.3553 -0.1788 0.114 Uiso 1 1 calc R . . H20B H 1.8193 -0.4503 -0.2205 0.114 Uiso 1 1 calc R . . H20C H 1.6983 -0.4539 -0.1938 0.114 Uiso 1 1 calc R . . C21 C 1.7553(7) -0.2911(7) -0.3094(5) 0.111(4) Uani 1 1 d . . . H21A H 1.7446 -0.2333 -0.2817 0.166 Uiso 1 1 calc R . . H21B H 1.7300 -0.2612 -0.3544 0.166 Uiso 1 1 calc R . . H21C H 1.8374 -0.3414 -0.3131 0.166 Uiso 1 1 calc R . . C22 C 1.7102(7) -0.4378(7) -0.3258(4) 0.075(3) Uani 1 1 d . . . H22A H 1.6787 -0.4048 -0.3692 0.112 Uiso 1 1 calc R . . H22B H 1.6736 -0.4844 -0.3059 0.112 Uiso 1 1 calc R . . H22C H 1.7941 -0.4801 -0.3329 0.112 Uiso 1 1 calc R . . C23 C 1.4863(5) -0.4267(5) -0.2343(3) 0.0367(18) Uani 1 1 d . . . H23A H 1.5683 -0.4769 -0.2261 0.044 Uiso 1 1 calc R . . C24 C 1.4061(6) -0.4292(5) -0.1718(3) 0.0481(19) Uani 1 1 d . . . H24A H 1.4317 -0.4099 -0.1327 0.058 Uiso 1 1 calc R . . H24B H 1.3264 -0.3749 -0.1792 0.058 Uiso 1 1 calc R . . C25 C 1.4042(6) -0.5361(5) -0.1558(3) 0.062(2) Uani 1 1 d . . . H25A H 1.4821 -0.5893 -0.1438 0.074 Uiso 1 1 calc R . . H25B H 1.3486 -0.5322 -0.1161 0.074 Uiso 1 1 calc R . . C26 C 1.3705(6) -0.5718(5) -0.2135(3) 0.056(2) Uani 1 1 d . . . H26A H 1.2892 -0.5234 -0.2221 0.067 Uiso 1 1 calc R . . H26B H 1.3752 -0.6446 -0.2019 0.067 Uiso 1 1 calc R . . C27 C 1.4479(7) -0.5725(6) -0.2759(3) 0.066(2) Uani 1 1 d . . . H27A H 1.4207 -0.5922 -0.3142 0.079 Uiso 1 1 calc R . . H27B H 1.5280 -0.6265 -0.2691 0.079 Uiso 1 1 calc R . . C28 C 1.4475(7) -0.4617(5) -0.2924(3) 0.057(2) Uani 1 1 d . . . H28A H 1.4999 -0.4638 -0.3333 0.069 Uiso 1 1 calc R . . H28B H 1.3682 -0.4088 -0.3022 0.069 Uiso 1 1 calc R . . C29 C 1.5294(5) -0.0857(4) -0.2841(3) 0.0327(17) Uani 1 1 d . . . H29A H 1.5988 -0.1072 -0.3175 0.039 Uiso 1 1 calc R . . C30 C 1.5606(5) -0.0566(5) -0.2211(3) 0.0431(19) Uani 1 1 d . . . H30A H 1.4947 -0.0398 -0.1862 0.052 Uiso 1 1 calc R . . H30B H 1.6281 -0.1185 -0.2031 0.052 Uiso 1 1 calc R . . C31 C 1.5895(6) 0.0385(5) -0.2354(4) 0.063(2) Uani 1 1 d . . . H31A H 1.6062 0.0573 -0.1929 0.076 Uiso 1 1 calc R . . H31B H 1.6599 0.0195 -0.2670 0.076 Uiso 1 1 calc R . . C32 C 1.4924(7) 0.1318(6) -0.2651(4) 0.067(2) Uani 1 1 d . . . H32A H 1.5158 0.1910 -0.2770 0.080 Uiso 1 1 calc R . . H32B H 1.4249 0.1563 -0.2313 0.080 Uiso 1 1 calc R . . C33 C 1.4570(6) 0.1040(5) -0.3287(4) 0.058(2) Uani 1 1 d . . . H33A H 1.3865 0.1651 -0.3443 0.070 Uiso 1 1 calc R . . H33B H 1.5200 0.0909 -0.3652 0.070 Uiso 1 1 calc R . . C34 C 1.4339(5) 0.0076(4) -0.3144(3) 0.0378(18) Uani 1 1 d . . . H34A H 1.3629 0.0254 -0.2834 0.045 Uiso 1 1 calc R . . H34B H 1.4188 -0.0121 -0.3571 0.045 Uiso 1 1 calc R . . C35 C 1.2508(5) -0.2263(4) -0.0248(3) 0.0264(15) Uani 1 1 d . . . C36 C 1.2462(5) -0.2998(5) 0.0359(3) 0.0362(17) Uani 1 1 d . . . C37 C 1.2646(6) -0.2571(6) 0.0993(3) 0.052(2) Uani 1 1 d . . . H37A H 1.3366 -0.2476 0.0918 0.078 Uiso 1 1 calc R . . H37B H 1.2699 -0.3084 0.1381 0.078 Uiso 1 1 calc R . . H37C H 1.1991 -0.1884 0.1082 0.078 Uiso 1 1 calc R . . C38 C 1.3449(6) -0.4102(5) 0.0245(3) 0.047(2) Uani 1 1 d . . . H38A H 1.3334 -0.4374 -0.0157 0.071 Uiso 1 1 calc R . . H38B H 1.3455 -0.4593 0.0639 0.071 Uiso 1 1 calc R . . H38C H 1.4191 -0.4047 0.0182 0.071 Uiso 1 1 calc R . . C39 C 1.1355(6) -0.3137(6) 0.0524(4) 0.065(2) Uani 1 1 d . . . H39A H 1.1198 -0.3420 0.0140 0.098 Uiso 1 1 calc R . . H39B H 1.0711 -0.2444 0.0617 0.098 Uiso 1 1 calc R . . H39C H 1.1437 -0.3637 0.0922 0.098 Uiso 1 1 calc R . . C40 C 1.4481(4) -0.2297(4) -0.0151(3) 0.0236(14) Uani 1 1 d . . . H40A H 1.4604 -0.2890 0.0208 0.028 Uiso 1 1 calc R . . C41 C 1.4406(5) -0.1322(5) 0.0168(3) 0.0443(19) Uani 1 1 d . . . H41A H 1.3779 -0.1125 0.0538 0.053 Uiso 1 1 calc R . . H41B H 1.4208 -0.0711 -0.0174 0.053 Uiso 1 1 calc R . . C42 C 1.5548(5) -0.1539(6) 0.0448(3) 0.051(2) Uani 1 1 d . . . H42A H 1.5485 -0.0876 0.0623 0.061 Uiso 1 1 calc R . . H42B H 1.5695 -0.2088 0.0830 0.061 Uiso 1 1 calc R . . C43 C 1.6535(5) -0.1910(6) -0.0069(3) 0.055(2) Uani 1 1 d . . . H43A H 1.7262 -0.2082 0.0140 0.066 Uiso 1 1 calc R . . H43B H 1.6433 -0.1329 -0.0426 0.066 Uiso 1 1 calc R . . C44 C 1.6634(5) -0.2884(6) -0.0383(3) 0.049(2) Uani 1 1 d . . . H44A H 1.6817 -0.3490 -0.0036 0.059 Uiso 1 1 calc R . . H44B H 1.7274 -0.3086 -0.0744 0.059 Uiso 1 1 calc R . . C45 C 1.5482(5) -0.2657(5) -0.0682(3) 0.0374(16) Uani 1 1 d . . . H45A H 1.5336 -0.2095 -0.1056 0.045 Uiso 1 1 calc R . . H45B H 1.5548 -0.3313 -0.0867 0.045 Uiso 1 1 calc R . . C46 C 1.0570(5) -0.1731(5) -0.0767(3) 0.0355(17) Uani 1 1 d . . . H46A H 1.0234 -0.1895 -0.0316 0.043 Uiso 1 1 calc R . . C47 C 0.9772(5) -0.0611(6) -0.1031(3) 0.049(2) Uani 1 1 d . . . H47A H 1.0131 -0.0415 -0.1458 0.058 Uiso 1 1 calc R . . H47B H 0.9666 -0.0093 -0.0699 0.058 Uiso 1 1 calc R . . C48 C 0.8589(5) -0.0555(6) -0.1152(4) 0.055(2) Uani 1 1 d . . . H48A H 0.8194 -0.0670 -0.0715 0.066 Uiso 1 1 calc R . . H48B H 0.8102 0.0167 -0.1349 0.066 Uiso 1 1 calc R . . C49 C 0.8697(7) -0.1353(6) -0.1606(4) 0.072(3) Uani 1 1 d . . . H49A H 0.8992 -0.1176 -0.2061 0.086 Uiso 1 1 calc R . . H49B H 0.7920 -0.1321 -0.1642 0.086 Uiso 1 1 calc R . . C50 C 0.9476(6) -0.2441(7) -0.1377(5) 0.083(3) Uani 1 1 d . . . H50A H 0.9585 -0.2932 -0.1728 0.100 Uiso 1 1 calc R . . H50B H 0.9112 -0.2667 -0.0962 0.100 Uiso 1 1 calc R . . C51 C 1.0694(5) -0.2536(5) -0.1227(4) 0.053(2) Uani 1 1 d . . . H51A H 1.1152 -0.3260 -0.1022 0.064 Uiso 1 1 calc R . . H51B H 1.1120 -0.2437 -0.1656 0.064 Uiso 1 1 calc R . . C52 C 1.1278(16) 0.4507(15) -0.3565(10) 0.269(10) Uiso 1 1 d . . . H52A H 1.1668 0.4814 -0.3322 0.403 Uiso 1 1 calc R . . H52B H 1.1800 0.3760 -0.3642 0.403 Uiso 1 1 calc R . . H52C H 1.0574 0.4539 -0.3296 0.403 Uiso 1 1 calc R . . C53 C 1.0916(13) 0.5215(12) -0.4321(8) 0.197(7) Uiso 1 1 d . . . H53A H 1.0425 0.5965 -0.4215 0.236 Uiso 1 1 calc R . . H53B H 1.1646 0.5203 -0.4555 0.236 Uiso 1 1 calc R . . C54 C 1.041(3) 0.502(3) -0.4757(19) 0.47(2) Uiso 1 1 d . . . H54A H 1.0628 0.4269 -0.4573 0.570 Uiso 1 1 calc R . . H54B H 1.1036 0.4944 -0.5119 0.570 Uiso 1 1 calc R . . C55 C 1.0783(13) 0.4188(12) -0.1691(8) 0.196(7) Uiso 1 1 d . . . H55B H 1.1449 0.3567 -0.1869 0.294 Uiso 1 1 calc R . . H55C H 1.0794 0.4845 -0.1921 0.294 Uiso 1 1 calc R . . H55D H 1.0063 0.4148 -0.1768 0.294 Uiso 1 1 calc R . . C56 C 1.0853(15) 0.4194(14) -0.0914(9) 0.238(8) Uiso 1 1 d . . . H56A H 1.0940 0.3469 -0.0746 0.285 Uiso 1 1 calc R . . H56B H 1.1629 0.4176 -0.0895 0.285 Uiso 1 1 calc R . . C57 C 1.0170(15) 0.4847(14) -0.0340(7) 0.202(7) Uiso 1 1 d . . . H57A H 1.0194 0.5525 -0.0534 0.243 Uiso 1 1 calc R . . H57B H 0.9403 0.4925 -0.0447 0.243 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 0.0709(3) 0.1120(4) 0.0714(3) -0.0194(3) -0.0204(3) -0.0436(3) I2 0.0519(3) 0.0421(2) 0.0529(3) -0.0090(2) -0.0104(2) -0.0177(2) Ga1 0.0540(5) 0.0486(4) 0.0175(3) 0.0003(3) -0.0042(3) -0.0130(4) Ga2 0.0342(3) 0.0320(3) 0.0200(3) 0.0013(3) 0.0008(3) -0.0141(3) Ga3 0.0273(3) 0.0380(3) 0.0189(3) 0.0013(3) -0.0026(3) -0.0163(3) N1 0.079(4) 0.045(3) 0.015(3) -0.003(2) 0.011(3) 0.000(3) N2 0.084(5) 0.047(4) 0.014(3) 0.008(3) 0.001(3) 0.018(4) N3 0.040(3) 0.044(3) 0.029(3) 0.006(2) -0.001(2) -0.023(2) N4 0.028(3) 0.037(3) 0.034(3) 0.001(2) 0.009(2) -0.011(2) N5 0.023(2) 0.046(3) 0.015(2) 0.002(2) -0.005(2) -0.013(2) N6 0.021(2) 0.043(3) 0.025(2) 0.005(2) -0.005(2) -0.017(2) C1 0.088(6) 0.041(4) 0.028(4) -0.001(3) 0.006(4) 0.014(5) C2 0.171(10) 0.061(6) 0.023(4) 0.011(4) 0.020(5) 0.012(7) C3 0.284(16) 0.061(6) 0.047(5) 0.038(5) 0.064(7) 0.044(9) C4 0.268(12) 0.068(5) 0.030(4) 0.015(4) 0.000(6) -0.076(7) C5 0.118(9) 0.117(8) 0.026(4) 0.020(5) 0.003(5) 0.027(7) C6 0.113(7) 0.044(4) 0.016(3) -0.002(3) 0.026(4) -0.010(5) C7 0.095(7) 0.073(6) 0.030(4) 0.004(4) 0.011(4) 0.006(6) C8 0.099(7) 0.073(6) 0.029(4) -0.003(4) 0.020(4) 0.020(6) C9 0.179(11) 0.050(6) 0.066(6) -0.014(5) 0.049(7) 0.007(7) C10 0.124(8) 0.037(4) 0.056(5) -0.024(4) 0.027(5) -0.003(5) C11 0.118(7) 0.057(5) 0.050(5) -0.010(4) 0.015(5) -0.024(5) C18 0.035(4) 0.034(3) 0.019(3) 0.004(3) 0.005(3) -0.002(3) C19 0.054(4) 0.050(4) 0.026(3) 0.004(3) 0.012(3) -0.018(3) C20 0.044(5) 0.098(6) 0.057(5) 0.012(5) -0.003(4) -0.008(5) C21 0.056(5) 0.076(6) 0.174(9) 0.012(6) 0.053(6) -0.025(5) C22 0.051(5) 0.087(6) 0.055(5) -0.009(4) 0.014(4) -0.004(5) C23 0.039(4) 0.035(3) 0.031(3) -0.005(3) 0.000(3) -0.011(3) C24 0.087(4) 0.041(3) 0.029(3) -0.001(3) -0.005(3) -0.040(3) C25 0.124(5) 0.051(3) 0.035(4) 0.004(3) 0.007(4) -0.065(3) C26 0.074(4) 0.050(4) 0.054(4) -0.007(3) 0.006(4) -0.038(3) C27 0.097(6) 0.055(4) 0.043(4) -0.016(3) 0.004(4) -0.029(4) C28 0.095(5) 0.043(4) 0.037(4) -0.007(3) 0.006(4) -0.035(4) C29 0.023(3) 0.031(3) 0.041(3) 0.001(3) 0.011(3) -0.013(3) C30 0.043(4) 0.039(4) 0.043(4) 0.000(3) -0.004(3) -0.014(3) C31 0.077(4) 0.061(4) 0.071(5) -0.012(4) -0.004(4) -0.047(4) C32 0.081(5) 0.054(4) 0.063(5) -0.020(4) 0.021(4) -0.031(4) C33 0.072(5) 0.032(3) 0.065(5) 0.014(3) 0.005(4) -0.025(3) C34 0.049(4) 0.036(3) 0.024(3) 0.009(3) -0.009(3) -0.016(3) C35 0.020(3) 0.027(3) 0.023(3) -0.006(2) 0.000(3) -0.002(3) C36 0.030(3) 0.049(4) 0.021(3) 0.002(3) 0.002(3) -0.012(3) C37 0.061(4) 0.077(4) 0.022(3) 0.008(3) 0.006(3) -0.038(4) C38 0.061(4) 0.039(4) 0.034(4) 0.013(3) 0.002(3) -0.020(3) C39 0.054(4) 0.088(5) 0.053(4) 0.026(4) -0.010(4) -0.035(4) C40 0.024(3) 0.024(3) 0.022(3) -0.001(2) -0.004(2) -0.009(2) C41 0.036(3) 0.053(4) 0.044(4) -0.014(3) -0.013(3) -0.015(3) C42 0.054(4) 0.053(4) 0.046(4) -0.001(3) -0.025(3) -0.018(4) C43 0.043(3) 0.085(5) 0.055(4) -0.001(4) -0.015(3) -0.043(3) C44 0.031(3) 0.087(5) 0.035(4) -0.006(3) -0.002(3) -0.030(3) C45 0.037(3) 0.051(3) 0.035(3) 0.000(3) -0.006(3) -0.029(3) C46 0.027(3) 0.056(4) 0.026(3) 0.013(3) -0.005(3) -0.023(3) C47 0.025(3) 0.067(5) 0.046(4) -0.005(3) -0.005(3) -0.011(3) C48 0.025(3) 0.075(5) 0.059(4) -0.002(4) -0.013(3) -0.015(4) C49 0.064(4) 0.080(5) 0.082(6) 0.015(4) -0.035(4) -0.038(4) C50 0.061(4) 0.099(5) 0.120(7) -0.037(5) -0.006(5) -0.054(4) C51 0.036(3) 0.061(4) 0.071(5) -0.005(4) -0.010(4) -0.027(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 I1 Ga1 2.5915(12) . ? I2 Ga3 2.5808(11) . ? Ga1 N1 1.972(5) . ? Ga1 N2 1.977(5) . ? Ga1 C1 2.423(7) . ? Ga1 Ga2 2.4303(12) . ? Ga2 N4 1.954(5) . ? Ga2 N3 1.959(5) . ? Ga2 Ga3 2.4236(11) . ? Ga2 C18 2.473(6) . ? Ga3 N6 1.971(4) . ? Ga3 N5 1.977(4) . ? Ga3 C35 2.442(5) . ? N1 C1 1.279(8) . ? N1 C6 1.465(8) . ? N2 C1 1.380(8) . ? N2 C12A 1.435(11) . ? N2 C12B 1.460(14) . ? N3 C18 1.339(8) . ? N3 C23 1.458(8) . ? N4 C18 1.311(7) . ? N4 C29 1.489(8) . ? N5 C35 1.340(7) . ? N5 C40 1.447(7) . ? N6 C35 1.346(7) . ? N6 C46 1.462(7) . ? C1 C2 1.541(10) . ? C2 C4 1.525(16) . ? C2 C3 1.527(12) . ? C2 C5 1.551(14) . ? C6 C7 1.508(12) . ? C6 C11 1.550(12) . ? C7 C8 1.507(10) . ? C8 C9 1.478(14) . ? C9 C10 1.539(14) . ? C10 C11 1.484(10) . ? C12A C17A 1.492(18) . ? C12A C13A 1.55(2) . ? C13A C14A 1.54(2) . ? C14A C15A 1.41(2) . ? C15A C16A 1.79(2) . ? C16A C17A 1.592(18) . ? C12B C13B 1.486(17) . ? C12B C17B 1.549(19) . ? C13B C14B 1.481(18) . ? C14B C15B 1.30(2) . ? C15B C16B 1.57(2) . ? C16B C17B 1.498(18) . ? C18 C19 1.507(8) . ? C19 C21 1.496(10) . ? C19 C20 1.516(9) . ? C19 C22 1.568(10) . ? C23 C28 1.521(9) . ? C23 C24 1.529(8) . ? C24 C25 1.495(8) . ? C25 C26 1.484(10) . ? C26 C27 1.498(9) . ? C27 C28 1.538(10) . ? C29 C34 1.474(7) . ? C29 C30 1.515(9) . ? C30 C31 1.510(9) . ? C31 C32 1.481(9) . ? C32 C33 1.541(11) . ? C33 C34 1.485(9) . ? C35 C36 1.508(8) . ? C36 C39 1.508(9) . ? C36 C38 1.531(8) . ? C36 C37 1.543(9) . ? C40 C45 1.505(7) . ? C40 C41 1.525(8) . ? C41 C42 1.526(9) . ? C42 C43 1.477(9) . ? C43 C44 1.507(10) . ? C44 C45 1.552(8) . ? C46 C51 1.474(9) . ? C46 C47 1.521(8) . ? C47 C48 1.533(9) . ? C48 C49 1.463(11) . ? C49 C50 1.464(10) . ? C50 C51 1.573(10) . ? C52 C53 1.71(2) . ? C53 C54 1.26(4) . ? C54 C54 1.54(7) 2_764 ? C55 C56 1.57(2) . ? C56 C57 1.49(2) . ? C57 C57 1.43(3) 2_765 ? 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 66.3(2) . . ? N1 Ga1 C1 31.8(2) . . ? N2 Ga1 C1 34.7(2) . . ? N1 Ga1 Ga2 124.7(2) . . ? N2 Ga1 Ga2 125.7(2) . . ? C1 Ga1 Ga2 131.1(2) . . ? N1 Ga1 I1 107.8(2) . . ? N2 Ga1 I1 108.0(2) . . ? C1 Ga1 I1 113.9(2) . . ? Ga2 Ga1 I1 114.89(4) . . ? N4 Ga2 N3 64.4(2) . . ? N4 Ga2 Ga3 113.67(15) . . ? N3 Ga2 Ga3 113.72(14) . . ? N4 Ga2 Ga1 112.37(14) . . ? N3 Ga2 Ga1 112.77(15) . . ? Ga3 Ga2 Ga1 124.66(4) . . ? N4 Ga2 C18 31.8(2) . . ? N3 Ga2 C18 32.6(2) . . ? Ga3 Ga2 C18 117.98(14) . . ? Ga1 Ga2 C18 117.35(14) . . ? N6 Ga3 N5 66.58(18) . . ? N6 Ga3 Ga2 125.52(15) . . ? N5 Ga3 Ga2 125.22(13) . . ? N6 Ga3 C35 33.41(18) . . ? N5 Ga3 C35 33.24(19) . . ? Ga2 Ga3 C35 132.22(14) . . ? N6 Ga3 I2 107.66(14) . . ? N5 Ga3 I2 108.58(15) . . ? Ga2 Ga3 I2 114.33(4) . . ? C35 Ga3 I2 113.45(14) . . ? C1 N1 C6 131.7(6) . . ? C1 N1 Ga1 93.9(4) . . ? C6 N1 Ga1 134.0(4) . . ? C1 N2 C12A 136.9(6) . . ? C1 N2 C12B 129.4(7) . . ? C12A N2 C12B 17.4(8) . . ? C1 N2 Ga1 90.6(4) . . ? C12A N2 Ga1 132.0(6) . . ? C12B N2 Ga1 137.9(6) . . ? C18 N3 C23 131.1(5) . . ? C18 N3 Ga2 95.3(4) . . ? C23 N3 Ga2 133.6(4) . . ? C18 N4 C29 133.3(5) . . ? C18 N4 Ga2 96.5(4) . . ? C29 N4 Ga2 130.0(3) . . ? C35 N5 C40 131.4(4) . . ? C35 N5 Ga3 92.8(3) . . ? C40 N5 Ga3 135.6(4) . . ? C35 N6 C46 133.6(5) . . ? C35 N6 Ga3 92.9(3) . . ? C46 N6 Ga3 132.5(3) . . ? N1 C1 N2 108.7(6) . . ? N1 C1 C2 124.6(6) . . ? N2 C1 C2 126.7(6) . . ? N1 C1 Ga1 54.3(3) . . ? N2 C1 Ga1 54.7(3) . . ? C2 C1 Ga1 175.1(8) . . ? C4 C2 C3 109.2(10) . . ? C4 C2 C1 108.6(8) . . ? C3 C2 C1 114.9(7) . . ? C4 C2 C5 111.5(7) . . ? C3 C2 C5 104.7(9) . . ? C1 C2 C5 107.8(9) . . ? N1 C6 C7 112.3(6) . . ? N1 C6 C11 108.3(7) . . ? C7 C6 C11 110.9(7) . . ? C8 C7 C6 109.0(7) . . ? C9 C8 C7 114.4(9) . . ? C8 C9 C10 109.5(7) . . ? C11 C10 C9 111.5(7) . . ? C10 C11 C6 109.6(8) . . ? N2 C12A C17A 116.9(10) . . ? N2 C12A C13A 98.8(9) . . ? C17A C12A C13A 110.3(11) . . ? C14A C13A C12A 109.4(12) . . ? C15A C14A C13A 110.6(14) . . ? C14A C15A C16A 117.7(13) . . ? C17A C16A C15A 97.6(10) . . ? C12A C17A C16A 116.0(11) . . ? N2 C12B C13B 107.1(9) . . ? N2 C12B C17B 98.3(10) . . ? C13B C12B C17B 109.8(11) . . ? C14B C13B C12B 112.5(11) . . ? C15B C14B C13B 120.8(15) . . ? C14B C15B C16B 121.5(14) . . ? C17B C16B C15B 108.7(12) . . ? C16B C17B C12B 113.0(12) . . ? N4 C18 N3 103.8(5) . . ? N4 C18 C19 130.7(6) . . ? N3 C18 C19 125.4(5) . . ? N4 C18 Ga2 51.7(3) . . ? N3 C18 Ga2 52.1(3) . . ? C19 C18 Ga2 177.0(4) . . ? C21 C19 C18 115.8(6) . . ? C21 C19 C20 108.8(7) . . ? C18 C19 C20 111.5(5) . . ? C21 C19 C22 104.0(6) . . ? C18 C19 C22 110.7(6) . . ? C20 C19 C22 105.4(6) . . ? N3 C23 C28 111.6(5) . . ? N3 C23 C24 108.0(5) . . ? C28 C23 C24 107.3(5) . . ? C25 C24 C23 112.8(5) . . ? C26 C25 C24 111.8(5) . . ? C25 C26 C27 111.2(6) . . ? C26 C27 C28 110.3(6) . . ? C23 C28 C27 111.6(5) . . ? C34 C29 N4 109.6(5) . . ? C34 C29 C30 110.3(5) . . ? N4 C29 C30 112.1(5) . . ? C31 C30 C29 111.4(5) . . ? C32 C31 C30 111.1(6) . . ? C31 C32 C33 111.4(6) . . ? C34 C33 C32 110.8(6) . . ? C29 C34 C33 114.0(6) . . ? N5 C35 N6 107.5(4) . . ? N5 C35 C36 124.6(5) . . ? N6 C35 C36 127.8(5) . . ? N5 C35 Ga3 53.9(3) . . ? N6 C35 Ga3 53.7(3) . . ? C36 C35 Ga3 173.9(4) . . ? C35 C36 C39 117.3(5) . . ? C35 C36 C38 107.6(4) . . ? C39 C36 C38 107.7(6) . . ? C35 C36 C37 109.1(5) . . ? C39 C36 C37 105.7(5) . . ? C38 C36 C37 109.3(5) . . ? N5 C40 C45 108.4(4) . . ? N5 C40 C41 111.2(4) . . ? C45 C40 C41 110.2(5) . . ? C40 C41 C42 111.5(5) . . ? C43 C42 C41 112.0(5) . . ? C42 C43 C44 111.7(6) . . ? C43 C44 C45 110.4(5) . . ? C40 C45 C44 110.9(5) . . ? N6 C46 C51 110.9(5) . . ? N6 C46 C47 108.1(5) . . ? C51 C46 C47 111.2(5) . . ? C46 C47 C48 110.7(6) . . ? C49 C48 C47 112.0(6) . . ? C48 C49 C50 112.8(7) . . ? C49 C50 C51 112.5(7) . . ? C46 C51 C50 111.2(6) . . ? C54 C53 C52 125(3) . . ? C53 C54 C54 168(4) . 2_764 ? C57 C56 C55 138.8(15) . . ? C57 C57 C56 159(2) 2_765 . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 0.959 _refine_diff_density_min -1.131 _refine_diff_density_rms 0.129 _exptl_crystal_recrystallization_method 'from n-hexane' # Attachment '- 3b - TZE94A.CIF' data_3b _database_code_depnum_ccdc_archive 'CCDC 811978' #TrackingRef '- 3b - TZE94A.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis-(N,N'-dicyclohexylneopentylamidinato-iodo-gallium(II)) -N,N'-dicyclohexylneopentylamidinato-gallium(I) toluene solvate ; _chemical_name_common ; bis-(N,N'-dicyclohexylneopentylamidinato-iodo-gallium(ii)) - N,N'-dicyclohexylneopentylamidinato-gallium(i) toluene solvate ; _chemical_melting_point '603 (dec)' _chemical_formula_moiety 'C51 H93 Ga3 I2 N6, C7 H8' _chemical_formula_sum 'C58 H101 Ga3 I2 N6' _chemical_formula_weight 1345.41 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.912(3) _cell_length_b 16.090(3) _cell_length_c 16.506(3) _cell_angle_alpha 78.66(3) _cell_angle_beta 85.66(3) _cell_angle_gamma 71.01(3) _cell_volume 3179.0(11) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description columns _exptl_crystal_colour colourless _exptl_crystal_size_max 0.416 _exptl_crystal_size_mid 0.157 _exptl_crystal_size_min 0.137 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1380 _exptl_absorpt_coefficient_mu 2.272 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.6213 _exptl_absorpt_correction_T_max 0.7632 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38406 _diffrn_reflns_av_R_equivalents 0.0986 _diffrn_reflns_av_sigmaI/netI 0.2300 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 30.59 _reflns_number_total 17618 _reflns_number_gt 5883 _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^)+(0.0462P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17618 _refine_ls_number_parameters 622 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1697 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1406 _refine_ls_wR_factor_gt 0.1113 _refine_ls_goodness_of_fit_ref 0.718 _refine_ls_restrained_S_all 0.724 _refine_ls_shift/su_max 0.005 _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 0.39442(4) 0.53401(2) 0.26526(2) 0.04447(10) Uani 1 1 d . . . I2 I 0.54132(3) 0.92731(3) 0.28734(3) 0.04923(11) Uani 1 1 d . . . Ga1 Ga 0.35734(4) 0.69510(4) 0.17653(3) 0.02933(13) Uani 1 1 d . . . Ga2 Ga 0.28745(5) 0.81797(4) 0.25366(3) 0.02978(13) Uani 1 1 d . . . Ga3 Ga 0.39710(5) 0.84927(4) 0.35209(3) 0.03321(14) Uani 1 1 d . . . N1 N 0.4724(3) 0.6931(3) 0.0906(3) 0.0350(10) Uani 1 1 d . . . N2 N 0.3134(3) 0.6891(3) 0.0654(2) 0.0340(10) Uani 1 1 d . . . N3 N 0.1301(4) 0.8427(3) 0.2873(3) 0.0400(12) Uani 1 1 d . . . N4 N 0.1864(3) 0.9281(3) 0.1866(3) 0.0331(10) Uani 1 1 d . . . N5 N 0.3346(4) 0.8975(3) 0.4531(3) 0.0369(11) Uani 1 1 d . . . N6 N 0.4605(4) 0.7685(3) 0.4565(2) 0.0337(10) Uani 1 1 d . . . C1 C 0.4093(4) 0.6926(3) 0.0305(3) 0.0319(12) Uani 1 1 d . . . C2 C 0.4311(5) 0.7013(4) -0.0632(3) 0.0406(13) Uani 1 1 d . . . C3 C 0.5408(5) 0.7118(5) -0.0916(4) 0.0616(17) Uani 1 1 d . . . H3A H 0.5994 0.6600 -0.0647 0.092 Uiso 1 1 calc R . . H3B H 0.5463 0.7663 -0.0768 0.092 Uiso 1 1 calc R . . H3C H 0.5479 0.7160 -0.1516 0.092 Uiso 1 1 calc R . . C4 C 0.4249(5) 0.6168(4) -0.0907(3) 0.0494(15) Uani 1 1 d . . . H4A H 0.4797 0.5640 -0.0611 0.074 Uiso 1 1 calc R . . H4B H 0.4394 0.6213 -0.1503 0.074 Uiso 1 1 calc R . . H4C H 0.3516 0.6115 -0.0783 0.074 Uiso 1 1 calc R . . C5 C 0.3463(6) 0.7873(4) -0.1089(4) 0.0563(18) Uani 1 1 d . . . H5A H 0.3608 0.7932 -0.1686 0.084 Uiso 1 1 calc R . . H5B H 0.3523 0.8396 -0.0899 0.084 Uiso 1 1 calc R . . H5C H 0.2722 0.7836 -0.0971 0.084 Uiso 1 1 calc R . . C6 C 0.5883(4) 0.6805(3) 0.0928(3) 0.0328(12) Uani 1 1 d . . . H6A H 0.6115 0.7138 0.0408 0.039 Uiso 1 1 calc R . . C7 C 0.6556(5) 0.5810(4) 0.1038(4) 0.0543(17) Uani 1 1 d . . . H7A H 0.6458 0.5569 0.0553 0.065 Uiso 1 1 calc R . . H7B H 0.6290 0.5477 0.1534 0.065 Uiso 1 1 calc R . . C8 C 0.7778(5) 0.5676(5) 0.1132(4) 0.0573(19) Uani 1 1 d . . . H8A H 0.8197 0.5031 0.1203 0.069 Uiso 1 1 calc R . . H8B H 0.8053 0.5985 0.0625 0.069 Uiso 1 1 calc R . . C9 C 0.7955(5) 0.6042(5) 0.1872(4) 0.0567(19) Uani 1 1 d . . . H9A H 0.8743 0.5969 0.1911 0.068 Uiso 1 1 calc R . . H9B H 0.7735 0.5700 0.2384 0.068 Uiso 1 1 calc R . . C10 C 0.7286(5) 0.7030(4) 0.1794(4) 0.0493(16) Uani 1 1 d . . . H10A H 0.7374 0.7245 0.2299 0.059 Uiso 1 1 calc R . . H10B H 0.7564 0.7381 0.1318 0.059 Uiso 1 1 calc R . . C11 C 0.6074(4) 0.7178(4) 0.1674(3) 0.0407(14) Uani 1 1 d . . . H11A H 0.5669 0.7826 0.1594 0.049 Uiso 1 1 calc R . . H11B H 0.5778 0.6883 0.2180 0.049 Uiso 1 1 calc R . . C12 C 0.2121(4) 0.6889(3) 0.0298(3) 0.0355(12) Uani 1 1 d . . . H12A H 0.2241 0.6882 -0.0307 0.043 Uiso 1 1 calc R . . C13 C 0.1851(5) 0.6047(4) 0.0719(4) 0.0458(15) Uani 1 1 d . . . H13A H 0.1783 0.6026 0.1324 0.055 Uiso 1 1 calc R . . H13B H 0.2451 0.5509 0.0614 0.055 Uiso 1 1 calc R . . C14 C 0.0757(5) 0.6050(4) 0.0379(4) 0.0566(17) Uani 1 1 d . . . H14A H 0.0849 0.6011 -0.0215 0.068 Uiso 1 1 calc R . . H14B H 0.0560 0.5524 0.0677 0.068 Uiso 1 1 calc R . . C15 C -0.0152(5) 0.6903(4) 0.0490(4) 0.0520(17) Uani 1 1 d . . . H15A H -0.0832 0.6916 0.0241 0.062 Uiso 1 1 calc R . . H15B H -0.0295 0.6906 0.1088 0.062 Uiso 1 1 calc R . . C16 C 0.0146(5) 0.7730(4) 0.0093(4) 0.0502(17) Uani 1 1 d . . . H16A H 0.0213 0.7760 -0.0513 0.060 Uiso 1 1 calc R . . H16B H -0.0449 0.8269 0.0201 0.060 Uiso 1 1 calc R . . C17 C 0.1207(5) 0.7731(4) 0.0417(4) 0.0428(15) Uani 1 1 d . . . H17A H 0.1121 0.7765 0.1012 0.051 Uiso 1 1 calc R . . H17B H 0.1395 0.8262 0.0120 0.051 Uiso 1 1 calc R . . C18 C 0.0966(4) 0.9182(3) 0.2280(3) 0.0334(12) Uani 1 1 d . . . C19 C -0.0194(5) 0.9802(4) 0.2084(3) 0.0403(14) Uani 1 1 d . . . C20 C -0.0483(5) 0.9776(4) 0.1214(4) 0.0491(16) Uani 1 1 d . . . H20A H 0.0080 0.9904 0.0823 0.074 Uiso 1 1 calc R . . H20B H -0.1194 1.0226 0.1064 0.074 Uiso 1 1 calc R . . H20C H -0.0520 0.9182 0.1194 0.074 Uiso 1 1 calc R . . C21 C -0.0255(5) 1.0777(4) 0.2145(4) 0.0486(17) Uani 1 1 d . . . H21A H 0.0300 1.0952 0.1777 0.073 Uiso 1 1 calc R . . H21B H -0.0120 1.0799 0.2715 0.073 Uiso 1 1 calc R . . H21C H -0.0984 1.1188 0.1979 0.073 Uiso 1 1 calc R . . C22 C -0.1099(5) 0.9609(4) 0.2700(4) 0.058(2) Uani 1 1 d . . . H22A H -0.1114 0.9003 0.2704 0.086 Uiso 1 1 calc R . . H22B H -0.1813 1.0042 0.2527 0.086 Uiso 1 1 calc R . . H22C H -0.0939 0.9660 0.3256 0.086 Uiso 1 1 calc R . . C23 C 0.0719(4) 0.7886(3) 0.3401(3) 0.0326(12) Uani 1 1 d D . . H23A H 0.0043 0.8288 0.3629 0.039 Uiso 1 1 calc R . . C24 C 0.0403(5) 0.7283(3) 0.2941(3) 0.0483(16) Uani 1 1 d D . . H24A H 0.1073 0.6890 0.2712 0.058 Uiso 1 1 calc R . . H24B H -0.0068 0.7655 0.2471 0.058 Uiso 1 1 calc R . . C25 C -0.0205(5) 0.6706(4) 0.3483(4) 0.0640(19) Uani 1 1 d D . . H25A H -0.0370 0.6306 0.3162 0.077 Uiso 1 1 calc R . . H25B H -0.0904 0.7089 0.3686 0.077 Uiso 1 1 calc R . . C26 C 0.0527(6) 0.6153(4) 0.4212(4) 0.081(2) Uani 1 1 d D . . H26A H 0.0134 0.5786 0.4578 0.097 Uiso 1 1 calc R . . H26B H 0.1196 0.5740 0.4001 0.097 Uiso 1 1 calc R . . C27 C 0.0860(6) 0.6712(4) 0.4714(3) 0.0596(19) Uani 1 1 d D . . H27A H 0.1367 0.6320 0.5156 0.072 Uiso 1 1 calc R . . H27B H 0.0207 0.7089 0.4975 0.072 Uiso 1 1 calc R . . C28 C 0.1461(5) 0.7338(4) 0.4098(3) 0.0434(15) Uani 1 1 d D . . H28A H 0.1650 0.7737 0.4407 0.052 Uiso 1 1 calc R . . H28B H 0.2148 0.6959 0.3876 0.052 Uiso 1 1 calc R . . C29 C 0.2055(4) 0.9982(3) 0.1221(3) 0.0337(13) Uani 1 1 d . . . H29A H 0.1339 1.0354 0.0958 0.040 Uiso 1 1 calc R . . C30 C 0.2530(5) 1.0593(3) 0.1578(3) 0.0393(14) Uani 1 1 d . . . H30A H 0.1981 1.0918 0.1954 0.047 Uiso 1 1 calc R . . H30B H 0.3185 1.0221 0.1907 0.047 Uiso 1 1 calc R . . C31 C 0.2849(5) 1.1272(4) 0.0902(4) 0.0497(16) Uani 1 1 d . . . H31A H 0.2180 1.1701 0.0625 0.060 Uiso 1 1 calc R . . H31B H 0.3210 1.1612 0.1157 0.060 Uiso 1 1 calc R . . C32 C 0.3620(5) 1.0814(4) 0.0263(4) 0.0538(17) Uani 1 1 d . . . H32A H 0.3766 1.1273 -0.0184 0.065 Uiso 1 1 calc R . . H32B H 0.4326 1.0443 0.0526 0.065 Uiso 1 1 calc R . . C33 C 0.3139(5) 1.0231(4) -0.0103(4) 0.0479(16) Uani 1 1 d . . . H33A H 0.3683 0.9907 -0.0482 0.058 Uiso 1 1 calc R . . H33B H 0.2486 1.0613 -0.0429 0.058 Uiso 1 1 calc R . . C34 C 0.2809(5) 0.9547(3) 0.0573(3) 0.0373(13) Uani 1 1 d . . . H34A H 0.2440 0.9218 0.0311 0.045 Uiso 1 1 calc R . . H34B H 0.3478 0.9109 0.0842 0.045 Uiso 1 1 calc R . . C35 C 0.3934(4) 0.8225(3) 0.5021(3) 0.0362(12) Uani 1 1 d . . . C36 C 0.3855(5) 0.8020(4) 0.5986(3) 0.0524(16) Uani 1 1 d . . . C37 C 0.4690(11) 0.8255(13) 0.6304(6) 0.356(6) Uani 1 1 d . . . H37A H 0.4646 0.8146 0.6909 0.533 Uiso 1 1 calc R . . H37B H 0.4594 0.8890 0.6097 0.533 Uiso 1 1 calc R . . H37C H 0.5408 0.7893 0.6125 0.533 Uiso 1 1 calc R . . C38 C 0.2765(10) 0.8397(9) 0.6305(6) 0.245(7) Uani 1 1 d . . . H38A H 0.2311 0.8035 0.6228 0.367 Uiso 1 1 calc R . . H38B H 0.2443 0.9010 0.6008 0.367 Uiso 1 1 calc R . . H38C H 0.2802 0.8401 0.6895 0.367 Uiso 1 1 calc R . . C39 C 0.4029(16) 0.7109(7) 0.6329(6) 0.289(10) Uani 1 1 d . . . H39A H 0.3685 0.6848 0.5981 0.434 Uiso 1 1 calc R . . H39B H 0.3705 0.7060 0.6886 0.434 Uiso 1 1 calc R . . H39C H 0.4817 0.6789 0.6359 0.434 Uiso 1 1 calc R . . C40 C 0.2584(5) 0.9815(4) 0.4690(4) 0.0538(18) Uani 1 1 d D . . H40A H 0.2280 0.9721 0.5264 0.065 Uiso 1 1 calc R . . C41 C 0.3228(8) 1.0421(5) 0.4639(8) 0.295(5) Uani 1 1 d D . . H41A H 0.3432 1.0578 0.4052 0.354 Uiso 1 1 calc R . . H41B H 0.3915 1.0091 0.4945 0.354 Uiso 1 1 calc R . . C42 C 0.2694(10) 1.1280(7) 0.4964(7) 0.356(5) Uani 1 1 d D . . H42A H 0.3194 1.1633 0.4967 0.428 Uiso 1 1 calc R . . H42B H 0.2337 1.1191 0.5512 0.428 Uiso 1 1 calc R . . C43 C 0.1892(7) 1.1647(6) 0.4258(5) 0.136(4) Uani 1 1 d D . . H43A H 0.1508 1.2277 0.4307 0.164 Uiso 1 1 calc R . . H43B H 0.2350 1.1667 0.3750 0.164 Uiso 1 1 calc R . . C44 C 0.1034(9) 1.1301(5) 0.4068(6) 0.153(5) Uani 1 1 d D . . H44A H 0.0736 1.1591 0.3511 0.184 Uiso 1 1 calc R . . H44B H 0.0428 1.1407 0.4479 0.184 Uiso 1 1 calc R . . C45 C 0.1696(10) 1.0137(6) 0.4112(7) 0.350(7) Uani 1 1 d D . . H45A H 0.1161 0.9811 0.4286 0.420 Uiso 1 1 calc R . . H45B H 0.1982 1.0024 0.3557 0.420 Uiso 1 1 calc R . . C46 C 0.5441(4) 0.6831(4) 0.4755(3) 0.0408(14) Uani 1 1 d D . . H46A H 0.5358 0.6534 0.5337 0.049 Uiso 1 1 calc R . . C47 C 0.6459(7) 0.7043(7) 0.4645(9) 0.281(8) Uani 1 1 d DU . . H47A H 0.6360 0.7574 0.4898 0.338 Uiso 1 1 calc R . . H47B H 0.6580 0.7218 0.4045 0.338 Uiso 1 1 calc R . . C48 C 0.7476(9) 0.6334(7) 0.4990(7) 0.194(5) Uani 1 1 d D . . H48A H 0.7376 0.6040 0.5563 0.233 Uiso 1 1 calc R . . H48B H 0.8116 0.6550 0.4952 0.233 Uiso 1 1 calc R . . C49 C 0.7514(8) 0.5746(5) 0.4342(5) 0.118(4) Uani 1 1 d D . . H49A H 0.7694 0.6080 0.3809 0.142 Uiso 1 1 calc R . . H49B H 0.8162 0.5209 0.4483 0.142 Uiso 1 1 calc R . . C50 C 0.6660(6) 0.5415(8) 0.4158(5) 0.158(7) Uani 1 1 d D . . H50A H 0.6657 0.4880 0.4572 0.190 Uiso 1 1 calc R . . H50B H 0.6790 0.5246 0.3605 0.190 Uiso 1 1 calc R . . C51 C 0.5369(10) 0.6284(6) 0.4182(7) 0.343(8) Uani 1 1 d D . . H51A H 0.5196 0.6652 0.3624 0.412 Uiso 1 1 calc R . . H51B H 0.4778 0.6017 0.4358 0.412 Uiso 1 1 calc R . . C52 C 1.0100(7) 0.6434(5) 0.7504(5) 0.083(3) Uani 1 1 d . . . C53 C 0.9357(6) 0.6749(5) 0.8097(5) 0.070(2) Uani 1 1 d . . . H53A H 0.9509 0.7096 0.8449 0.084 Uiso 1 1 calc R . . C54 C 0.8404(7) 0.6562(6) 0.8175(7) 0.102(3) Uani 1 1 d . . . H54A H 0.7879 0.6816 0.8568 0.123 Uiso 1 1 calc R . . C55 C 0.8157(8) 0.6051(6) 0.7745(7) 0.104(3) Uani 1 1 d . . . H55A H 0.7491 0.5914 0.7851 0.124 Uiso 1 1 calc R . . C56 C 0.8821(9) 0.5737(6) 0.7177(6) 0.106(3) Uani 1 1 d . . . H56A H 0.8622 0.5380 0.6861 0.127 Uiso 1 1 calc R . . C57 C 0.9806(10) 0.5894(5) 0.7008(5) 0.102(4) Uani 1 1 d . . . H57A H 1.0278 0.5657 0.6581 0.122 Uiso 1 1 calc R . . C58 C 1.1142(8) 0.6670(8) 0.7421(9) 0.156(6) Uani 1 1 d . . . H58A H 1.1149 0.7025 0.7838 0.233 Uiso 1 1 calc R . . H58B H 1.1187 0.7017 0.6868 0.233 Uiso 1 1 calc R . . H58C H 1.1771 0.6121 0.7501 0.233 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 0.0596(2) 0.03202(16) 0.03830(18) -0.00365(14) -0.00399(17) -0.01064(17) I2 0.0489(2) 0.0500(2) 0.0504(2) -0.00712(17) 0.00338(18) -0.01998(18) Ga1 0.0281(3) 0.0308(2) 0.0297(3) -0.0083(2) 0.0007(2) -0.0089(2) Ga2 0.0307(3) 0.0273(2) 0.0284(3) -0.0046(2) 0.0005(2) -0.0057(2) Ga3 0.0400(3) 0.0296(3) 0.0284(3) -0.0087(2) -0.0012(2) -0.0068(2) N1 0.028(2) 0.039(2) 0.045(2) -0.0138(18) -0.0024(18) -0.0162(17) N2 0.032(2) 0.048(2) 0.0260(19) -0.0040(17) 0.0024(17) -0.0198(18) N3 0.043(3) 0.027(2) 0.041(2) 0.0004(18) 0.010(2) -0.005(2) N4 0.026(2) 0.033(2) 0.036(2) -0.0061(17) 0.0004(18) -0.0034(18) N5 0.042(3) 0.033(2) 0.032(2) -0.0123(17) -0.0005(19) -0.002(2) N6 0.039(2) 0.032(2) 0.029(2) -0.0106(16) 0.0010(18) -0.0070(19) C1 0.025(2) 0.035(2) 0.039(3) -0.010(2) 0.005(2) -0.014(2) C2 0.049(3) 0.045(3) 0.032(3) -0.011(2) 0.008(2) -0.020(2) C3 0.070(4) 0.098(4) 0.036(3) -0.021(3) 0.014(3) -0.051(3) C4 0.053(3) 0.059(3) 0.043(3) -0.028(2) 0.005(3) -0.018(3) C5 0.078(4) 0.057(3) 0.033(3) -0.008(3) 0.009(3) -0.021(3) C6 0.029(2) 0.034(2) 0.038(3) -0.010(2) -0.001(2) -0.011(2) C7 0.051(3) 0.044(3) 0.071(4) -0.024(3) 0.015(3) -0.014(3) C8 0.033(3) 0.053(4) 0.072(4) -0.004(3) 0.002(3) -0.001(3) C9 0.028(3) 0.067(4) 0.061(4) 0.005(3) 0.002(3) -0.007(3) C10 0.038(3) 0.060(3) 0.050(3) -0.014(3) 0.000(3) -0.013(3) C11 0.028(3) 0.054(3) 0.043(3) -0.016(2) 0.002(2) -0.013(2) C12 0.032(2) 0.047(3) 0.035(3) -0.012(2) 0.006(2) -0.021(2) C13 0.037(3) 0.041(3) 0.057(3) 0.007(3) -0.020(3) -0.014(3) C14 0.057(3) 0.044(3) 0.077(4) 0.000(3) -0.018(3) -0.030(3) C15 0.028(3) 0.072(4) 0.056(4) -0.003(3) 0.000(3) -0.021(3) C16 0.042(3) 0.058(4) 0.043(3) -0.009(3) -0.011(3) -0.005(3) C17 0.043(3) 0.036(3) 0.045(3) -0.005(2) -0.002(3) -0.007(3) C18 0.033(3) 0.035(2) 0.027(2) -0.007(2) 0.007(2) -0.004(2) C19 0.036(3) 0.036(3) 0.041(3) -0.007(2) 0.003(2) -0.002(2) C20 0.044(3) 0.049(3) 0.055(3) -0.012(3) -0.006(3) -0.012(3) C21 0.040(3) 0.034(3) 0.058(4) -0.002(3) -0.003(3) 0.003(3) C22 0.037(3) 0.044(3) 0.070(4) 0.006(3) 0.007(3) 0.005(3) C23 0.030(3) 0.029(2) 0.032(2) -0.005(2) 0.005(2) -0.002(2) C24 0.069(4) 0.041(3) 0.034(3) -0.007(2) -0.001(3) -0.015(3) C25 0.084(4) 0.043(3) 0.071(4) 0.001(3) -0.020(4) -0.030(3) C26 0.116(5) 0.067(4) 0.079(5) 0.013(3) -0.029(4) -0.063(4) C27 0.094(5) 0.055(3) 0.029(3) 0.010(3) -0.006(3) -0.032(3) C28 0.050(3) 0.040(3) 0.037(3) -0.006(2) 0.002(3) -0.011(3) C29 0.038(3) 0.028(2) 0.032(2) -0.001(2) 0.007(2) -0.009(2) C30 0.050(3) 0.026(2) 0.039(3) -0.007(2) -0.005(3) -0.006(2) C31 0.053(3) 0.038(3) 0.060(4) -0.007(3) -0.005(3) -0.018(3) C32 0.046(3) 0.062(3) 0.056(4) -0.007(3) 0.009(3) -0.026(3) C33 0.034(3) 0.065(3) 0.044(3) -0.002(3) 0.010(2) -0.022(3) C34 0.039(3) 0.039(3) 0.034(3) -0.012(2) 0.005(2) -0.011(2) C35 0.037(3) 0.049(3) 0.029(2) -0.018(2) 0.004(2) -0.018(2) C36 0.060(3) 0.075(4) 0.035(3) -0.016(3) 0.008(3) -0.037(3) C37 0.436(9) 0.835(17) 0.025(4) -0.061(8) 0.018(6) -0.526 C38 0.224(10) 0.211(12) 0.080(6) 0.065(7) 0.103(6) 0.153(10) C39 0.49(2) 0.092(7) 0.066(5) 0.052(5) 0.123(9) 0.136(11) C40 0.068(4) 0.041(3) 0.047(3) -0.018(3) 0.008(3) -0.006(3) C41 0.319(10) 0.135(5) 0.514(12) -0.245(6) 0.335(9) -0.154(6) C42 0.611(12) 0.511(10) 0.230(12) -0.246(9) 0.250(11) -0.512 C43 0.155(10) 0.122(6) 0.081(5) -0.071(4) -0.042(6) 0.064(7) C44 0.277(14) 0.114(6) 0.075(5) -0.060(4) -0.033(7) -0.038(9) C45 0.362(14) 0.273(8) 0.257(7) -0.239(6) -0.262(8) 0.279(9) C46 0.033(3) 0.051(3) 0.031(3) -0.006(2) -0.004(2) -0.004(3) C47 0.033(6) 0.253(12) 0.378(17) 0.264(11) -0.038(9) 0.017(9) C48 0.243(11) 0.284(13) 0.130(10) -0.025(9) -0.004(10) -0.192(10) C49 0.168(10) 0.050(4) 0.075(5) -0.020(4) -0.052(6) 0.065(6) C50 0.048(5) 0.315(18) 0.048(5) 0.010(8) 0.007(4) 0.002(8) C51 0.480(19) 0.133(6) 0.277(9) -0.164(6) -0.309(10) 0.232(9) C52 0.082(5) 0.050(4) 0.085(5) 0.022(4) 0.022(5) -0.004(4) C53 0.065(5) 0.069(4) 0.076(5) -0.025(4) 0.007(4) -0.016(4) C54 0.084(5) 0.096(5) 0.147(8) -0.050(5) 0.026(6) -0.046(5) C55 0.108(6) 0.080(5) 0.134(8) -0.003(5) -0.029(6) -0.047(5) C56 0.141(8) 0.089(5) 0.098(6) -0.046(5) -0.003(6) -0.033(6) C57 0.157(9) 0.046(4) 0.063(5) -0.010(4) 0.013(6) 0.017(6) C58 0.057(6) 0.104(8) 0.232(13) 0.073(8) 0.022(8) 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 Ga1 2.6264(11) . ? I2 Ga3 2.6231(10) . ? Ga1 N1 1.972(4) . ? Ga1 N2 1.989(4) . ? Ga1 Ga2 2.4491(11) . ? Ga1 C1 2.456(5) . ? Ga2 N3 1.996(5) . ? Ga2 N4 2.003(4) . ? Ga2 Ga3 2.4559(10) . ? Ga2 C18 2.481(5) . ? Ga3 N5 1.982(4) . ? Ga3 N6 1.993(4) . ? Ga3 C35 2.428(5) . ? N1 C1 1.332(7) . ? N1 C6 1.445(6) . ? N2 C1 1.339(6) . ? N2 C12 1.476(6) . ? N3 C18 1.371(6) . ? N3 C23 1.453(6) . ? N4 C18 1.339(6) . ? N4 C29 1.462(6) . ? N5 C35 1.342(6) . ? N5 C40 1.449(7) . ? N6 C35 1.319(6) . ? N6 C46 1.438(6) . ? C1 C2 1.539(7) . ? C2 C3 1.509(8) . ? C2 C4 1.544(8) . ? C2 C5 1.553(8) . ? C6 C7 1.534(7) . ? C6 C11 1.539(7) . ? C7 C8 1.537(9) . ? C8 C9 1.518(10) . ? C9 C10 1.528(9) . ? C10 C11 1.528(8) . ? C12 C17 1.515(7) . ? C12 C13 1.531(8) . ? C13 C14 1.557(8) . ? C14 C15 1.521(8) . ? C15 C16 1.518(9) . ? C16 C17 1.508(8) . ? C18 C19 1.523(7) . ? C19 C20 1.522(8) . ? C19 C22 1.558(8) . ? C19 C21 1.567(8) . ? C23 C28 1.495(7) . ? C23 C24 1.510(7) . ? C24 C25 1.524(8) . ? C25 C26 1.529(8) . ? C26 C27 1.509(9) . ? C27 C28 1.625(8) . ? C29 C34 1.509(7) . ? C29 C30 1.537(8) . ? C30 C31 1.534(8) . ? C31 C32 1.521(8) . ? C32 C33 1.514(9) . ? C33 C34 1.544(8) . ? C35 C36 1.563(7) . ? C36 C39 1.413(13) . ? C36 C37 1.419(14) . ? C36 C38 1.443(12) . ? C40 C45 1.442(10) . ? C40 C41 1.460(10) . ? C41 C42 1.514(11) . ? C42 C43 1.515(12) . ? C43 C44 1.470(12) . ? C44 C45 1.776(10) . ? C46 C51 1.439(10) . ? C46 C47 1.452(10) . ? C47 C48 1.494(12) . ? C48 C49 1.550(12) . ? C49 C50 1.443(12) . ? C50 C51 1.797(11) . ? C52 C53 1.368(11) . ? C52 C57 1.454(13) . ? C52 C58 1.503(14) . ? C53 C54 1.351(12) . ? C54 C55 1.310(13) . ? C55 C56 1.284(13) . ? C56 C57 1.374(15) . ? 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 65.69(17) . . ? N1 Ga1 Ga2 122.08(13) . . ? N2 Ga1 Ga2 128.25(12) . . ? N1 Ga1 C1 32.76(17) . . ? N2 Ga1 C1 32.97(16) . . ? Ga2 Ga1 C1 132.00(12) . . ? N1 Ga1 I1 109.31(12) . . ? N2 Ga1 I1 106.33(13) . . ? Ga2 Ga1 I1 115.36(3) . . ? C1 Ga1 I1 112.55(12) . . ? N3 Ga2 N4 66.07(17) . . ? N3 Ga2 Ga1 113.95(14) . . ? N4 Ga2 Ga1 112.45(12) . . ? N3 Ga2 Ga3 113.20(14) . . ? N4 Ga2 Ga3 113.67(13) . . ? Ga1 Ga2 Ga3 123.65(4) . . ? N3 Ga2 C18 33.48(16) . . ? N4 Ga2 C18 32.59(16) . . ? Ga1 Ga2 C18 117.92(13) . . ? Ga3 Ga2 C18 118.42(13) . . ? N5 Ga3 N6 66.30(17) . . ? N5 Ga3 C35 33.52(16) . . ? N6 Ga3 C35 32.88(16) . . ? N5 Ga3 Ga2 123.32(14) . . ? N6 Ga3 Ga2 126.07(13) . . ? C35 Ga3 Ga2 130.84(13) . . ? N5 Ga3 I2 108.16(14) . . ? N6 Ga3 I2 106.99(14) . . ? C35 Ga3 I2 113.13(13) . . ? Ga2 Ga3 I2 116.02(3) . . ? C1 N1 C6 131.6(4) . . ? C1 N1 Ga1 94.0(3) . . ? C6 N1 Ga1 133.5(3) . . ? C1 N2 C12 131.6(4) . . ? C1 N2 Ga1 93.1(3) . . ? C12 N2 Ga1 135.2(3) . . ? C18 N3 C23 133.0(5) . . ? C18 N3 Ga2 93.1(3) . . ? C23 N3 Ga2 132.3(3) . . ? C18 N4 C29 133.2(4) . . ? C18 N4 Ga2 93.8(3) . . ? C29 N4 Ga2 132.8(3) . . ? C35 N5 C40 133.5(4) . . ? C35 N5 Ga3 91.8(3) . . ? C40 N5 Ga3 134.7(4) . . ? C35 N6 C46 133.7(4) . . ? C35 N6 Ga3 92.0(3) . . ? C46 N6 Ga3 134.3(3) . . ? N1 C1 N2 107.1(4) . . ? N1 C1 C2 129.9(4) . . ? N2 C1 C2 122.9(5) . . ? N1 C1 Ga1 53.2(2) . . ? N2 C1 Ga1 53.9(2) . . ? C2 C1 Ga1 173.4(4) . . ? C3 C2 C1 115.1(5) . . ? C3 C2 C4 107.4(5) . . ? C1 C2 C4 108.7(4) . . ? C3 C2 C5 104.4(5) . . ? C1 C2 C5 109.6(4) . . ? C4 C2 C5 111.6(5) . . ? N1 C6 C7 111.1(4) . . ? N1 C6 C11 107.3(4) . . ? C7 C6 C11 108.9(4) . . ? C6 C7 C8 110.8(5) . . ? C9 C8 C7 110.7(5) . . ? C8 C9 C10 110.7(5) . . ? C11 C10 C9 111.0(5) . . ? C10 C11 C6 112.2(4) . . ? N2 C12 C17 108.9(4) . . ? N2 C12 C13 108.9(4) . . ? C17 C12 C13 111.6(4) . . ? C12 C13 C14 109.8(5) . . ? C15 C14 C13 110.0(5) . . ? C16 C15 C14 111.7(5) . . ? C17 C16 C15 112.0(5) . . ? C16 C17 C12 110.3(5) . . ? N4 C18 N3 107.1(4) . . ? N4 C18 C19 124.5(4) . . ? N3 C18 C19 128.4(5) . . ? N4 C18 Ga2 53.6(2) . . ? N3 C18 Ga2 53.5(3) . . ? C19 C18 Ga2 177.6(4) . . ? C20 C19 C18 109.5(4) . . ? C20 C19 C22 109.2(5) . . ? C18 C19 C22 115.4(4) . . ? C20 C19 C21 109.8(5) . . ? C18 C19 C21 108.8(5) . . ? C22 C19 C21 104.0(5) . . ? N3 C23 C28 107.2(4) . . ? N3 C23 C24 112.0(4) . . ? C28 C23 C24 110.1(4) . . ? C23 C24 C25 112.9(5) . . ? C24 C25 C26 108.0(5) . . ? C27 C26 C25 113.5(5) . . ? C26 C27 C28 108.2(5) . . ? C23 C28 C27 109.8(5) . . ? N4 C29 C34 108.5(4) . . ? N4 C29 C30 111.5(4) . . ? C34 C29 C30 111.3(4) . . ? C31 C30 C29 112.3(4) . . ? C32 C31 C30 111.5(5) . . ? C33 C32 C31 111.4(5) . . ? C32 C33 C34 111.8(5) . . ? C29 C34 C33 112.6(4) . . ? N6 C35 N5 109.6(4) . . ? N6 C35 C36 124.8(5) . . ? N5 C35 C36 125.7(5) . . ? N6 C35 Ga3 55.1(2) . . ? N5 C35 Ga3 54.7(2) . . ? C36 C35 Ga3 176.2(4) . . ? C39 C36 C37 106.1(12) . . ? C39 C36 C38 99.2(10) . . ? C37 C36 C38 115.6(10) . . ? C39 C36 C35 114.5(6) . . ? C37 C36 C35 107.9(6) . . ? C38 C36 C35 113.4(6) . . ? C45 C40 N5 110.4(5) . . ? C45 C40 C41 113.4(8) . . ? N5 C40 C41 106.0(5) . . ? C40 C41 C42 117.0(8) . . ? C41 C42 C43 91.8(8) . . ? C44 C43 C42 128.1(9) . . ? C43 C44 C45 105.0(8) . . ? C40 C45 C44 110.2(7) . . ? N6 C46 C51 108.8(5) . . ? N6 C46 C47 104.1(6) . . ? C51 C46 C47 111.4(9) . . ? C46 C47 C48 117.7(9) . . ? C47 C48 C49 93.6(9) . . ? C50 C49 C48 127.5(8) . . ? C49 C50 C51 108.4(8) . . ? C46 C51 C50 108.6(8) . . ? C53 C52 C57 116.5(8) . . ? C53 C52 C58 117.9(10) . . ? C57 C52 C58 125.6(9) . . ? C54 C53 C52 119.1(8) . . ? C55 C54 C53 124.1(9) . . ? C56 C55 C54 119.5(10) . . ? C55 C56 C57 122.9(10) . . ? C56 C57 C52 117.7(8) . . ? _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 30.59 _diffrn_measured_fraction_theta_full 0.900 _refine_diff_density_max 2.010 _refine_diff_density_min -1.091 _refine_diff_density_rms 0.129 _exptl_crystal_recrystallization_method 'from toluene' # Attachment '- 3c - TZE30.CIF' data_3c _database_code_depnum_ccdc_archive 'CCDC 811979' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis-(N,N'-dicyclohexylneopentylamidinato-iodo-gallium(II))-N,N' -dicyclohexylneopentylamidinato-gallium(I) tetrahydrofurane solvate ; _chemical_name_common ; bis-(N,N'-dicyclohexylneopentylamidinato-iodo-gallium(ii))- N,N' -dicyclohexylneopentylamidinato-gallium(i) tetrahydrofurane solvate ; _chemical_melting_point '603 (dec)' _chemical_formula_moiety ;C51 H93 Ga3 I2 N6, 2(C4 H8 O) ; _chemical_formula_sum 'C59 H109 Ga3 I2 N6 O2' _chemical_formula_weight 1397.48 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 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 13.486(3) _cell_length_b 22.613(5) _cell_length_c 21.158(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.95(3) _cell_angle_gamma 90.00 _cell_volume 6451(2) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cube _exptl_crystal_colour colourless _exptl_crystal_size_max 0.519 _exptl_crystal_size_mid 0.513 _exptl_crystal_size_min 0.506 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 2.244 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.3763 _exptl_absorpt_correction_T_max 0.4323 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37090 _diffrn_reflns_av_R_equivalents 0.1520 _diffrn_reflns_av_sigmaI/netI 0.1539 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.99 _reflns_number_total 11096 _reflns_number_gt 5738 _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^)+(0.1013P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11096 _refine_ls_number_parameters 649 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1445 _refine_ls_R_factor_gt 0.0763 _refine_ls_wR_factor_ref 0.1997 _refine_ls_wR_factor_gt 0.1728 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _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 1.00200(7) 0.27490(4) 1.30495(4) 0.0671(3) Uani 1 1 d . . . I2 I 0.61335(6) 0.24019(3) 1.21120(3) 0.0523(3) Uani 1 1 d . . . Ga1 Ga 0.89468(8) 0.18980(4) 1.34911(4) 0.0322(3) Uani 1 1 d . . . Ga2 Ga 0.82667(8) 0.12225(4) 1.27034(4) 0.0282(3) Uani 1 1 d . . . Ga3 Ga 0.74095(8) 0.16043(4) 1.17733(4) 0.0308(3) Uani 1 1 d . . . C1 C 0.8924(7) 0.1954(4) 1.4636(4) 0.030(2) Uani 1 1 d . . . C2 C 0.8854(8) 0.1991(5) 1.5362(5) 0.042(3) Uani 1 1 d . . . C3 C 0.9632(10) 0.1656(6) 1.5713(4) 0.066(4) Uani 1 1 d . . . H3A H 0.9584 0.1244 1.5606 0.099 Uiso 1 1 calc R . . H3B H 0.9540 0.1704 1.6159 0.099 Uiso 1 1 calc R . . H3C H 1.0273 0.1802 1.5602 0.099 Uiso 1 1 calc R . . C4 C 0.7838(10) 0.1774(7) 1.5544(5) 0.076(4) Uani 1 1 d . . . H4A H 0.7767 0.1366 1.5428 0.113 Uiso 1 1 calc R . . H4B H 0.7339 0.2004 1.5328 0.113 Uiso 1 1 calc R . . H4C H 0.7761 0.1815 1.5992 0.113 Uiso 1 1 calc R . . C5 C 0.8984(11) 0.2643(5) 1.5550(5) 0.068(4) Uani 1 1 d . . . H5A H 0.8501 0.2879 1.5327 0.102 Uiso 1 1 calc R . . H5B H 0.9638 0.2772 1.5443 0.102 Uiso 1 1 calc R . . H5C H 0.8893 0.2684 1.5997 0.102 Uiso 1 1 calc R . . C6 C 1.0387(8) 0.1253(5) 1.4463(5) 0.045(3) Uani 1 1 d . . . H6A H 1.0424 0.1206 1.4923 0.054 Uiso 1 1 calc R . . C7 C 1.0211(14) 0.0684(7) 1.4170(14) 0.190(14) Uani 1 1 d . . . H7A H 1.0107 0.0739 1.3719 0.228 Uiso 1 1 calc R . . H7B H 0.9612 0.0513 1.4339 0.228 Uiso 1 1 calc R . . C8 C 1.1110(17) 0.0237(7) 1.4284(17) 0.218(19) Uani 1 1 d . . . H8A H 1.1164 0.0128 1.4726 0.261 Uiso 1 1 calc R . . H8B H 1.1018 -0.0118 1.4033 0.261 Uiso 1 1 calc R . . C9 C 1.194(3) 0.0538(17) 1.4099(10) 0.23(2) Uani 1 1 d . . . H9A H 1.2492 0.0264 1.4107 0.282 Uiso 1 1 calc R . . H9B H 1.1837 0.0661 1.3664 0.282 Uiso 1 1 calc R . . C10 C 1.2186(12) 0.0991(15) 1.4420(18) 0.26(2) Uani 1 1 d . . . H10A H 1.2830 0.1138 1.4296 0.308 Uiso 1 1 calc R . . H10B H 1.2204 0.0903 1.4869 0.308 Uiso 1 1 calc R . . C11 C 1.1294(10) 0.1475(9) 1.4244(16) 0.26(2) Uani 1 1 d . . . H11A H 1.1439 0.1852 1.4443 0.307 Uiso 1 1 calc R . . H11B H 1.1254 0.1534 1.3790 0.307 Uiso 1 1 calc R . . C12 C 0.7496(7) 0.2630(4) 1.4362(4) 0.031(2) Uani 1 1 d . . . H12A H 0.7421 0.2668 1.4820 0.038 Uiso 1 1 calc R . . C13 C 0.6535(10) 0.2394(5) 1.4084(7) 0.067(4) Uani 1 1 d . . . H13A H 0.6379 0.2018 1.4280 0.081 Uiso 1 1 calc R . . H13B H 0.6611 0.2328 1.3634 0.081 Uiso 1 1 calc R . . C14 C 0.5681(9) 0.2833(6) 1.4190(8) 0.078(4) Uani 1 1 d . . . H14A H 0.5087 0.2689 1.3976 0.093 Uiso 1 1 calc R . . H14B H 0.5546 0.2857 1.4638 0.093 Uiso 1 1 calc R . . C15 C 0.5920(12) 0.3421(6) 1.3953(7) 0.080(5) Uani 1 1 d . . . H15A H 0.5389 0.3691 1.4060 0.097 Uiso 1 1 calc R . . H15B H 0.5959 0.3406 1.3496 0.097 Uiso 1 1 calc R . . C16 C 0.6857(11) 0.3650(5) 1.4213(8) 0.081(5) Uani 1 1 d . . . H16A H 0.6794 0.3712 1.4664 0.097 Uiso 1 1 calc R . . H16B H 0.7003 0.4028 1.4019 0.097 Uiso 1 1 calc R . . C17 C 0.7699(10) 0.3227(5) 1.4096(7) 0.079(5) Uani 1 1 d . . . H17A H 0.7801 0.3193 1.3645 0.094 Uiso 1 1 calc R . . H17B H 0.8303 0.3383 1.4288 0.094 Uiso 1 1 calc R . . C18 C 0.8439(7) 0.0149(4) 1.2852(4) 0.030(2) Uani 1 1 d . . . C19 C 0.8498(8) -0.0510(4) 1.2944(4) 0.038(3) Uani 1 1 d . . . C20 C 0.7617(9) -0.0812(4) 1.2606(5) 0.048(3) Uani 1 1 d . . . H20A H 0.7008 -0.0645 1.2754 0.072 Uiso 1 1 calc R . . H20B H 0.7629 -0.1228 1.2694 0.072 Uiso 1 1 calc R . . H20C H 0.7662 -0.0750 1.2158 0.072 Uiso 1 1 calc R . . C21 C 0.9434(9) -0.0799(4) 1.2691(5) 0.057(3) Uani 1 1 d . . . H21A H 1.0008 -0.0623 1.2889 0.086 Uiso 1 1 calc R . . H21B H 0.9461 -0.0741 1.2242 0.086 Uiso 1 1 calc R . . H21C H 0.9424 -0.1215 1.2782 0.086 Uiso 1 1 calc R . . C22 C 0.8493(9) -0.0666(4) 1.3646(5) 0.045(3) Uani 1 1 d . . . H22A H 0.7911 -0.0503 1.3835 0.068 Uiso 1 1 calc R . . H22B H 0.9074 -0.0505 1.3850 0.068 Uiso 1 1 calc R . . H22C H 0.8490 -0.1088 1.3694 0.068 Uiso 1 1 calc R . . C23 C 0.9791(7) 0.0377(4) 1.2061(4) 0.033(2) Uani 1 1 d . . . H23A H 1.0224 0.0055 1.2207 0.039 Uiso 1 1 calc R . . C24 C 0.9286(8) 0.0203(5) 1.1454(4) 0.042(3) Uani 1 1 d . . . H24A H 0.8826 0.0512 1.1325 0.051 Uiso 1 1 calc R . . H24B H 0.8910 -0.0157 1.1518 0.051 Uiso 1 1 calc R . . C25 C 1.0029(10) 0.0104(5) 1.0937(5) 0.062(4) Uani 1 1 d . . . H25A H 1.0476 -0.0214 1.1058 0.075 Uiso 1 1 calc R . . H25B H 0.9684 -0.0009 1.0550 0.075 Uiso 1 1 calc R . . C26 C 1.0602(11) 0.0650(6) 1.0830(6) 0.074(4) Uani 1 1 d . . . H26A H 1.0157 0.0959 1.0681 0.088 Uiso 1 1 calc R . . H26B H 1.1085 0.0579 1.0504 0.088 Uiso 1 1 calc R . . C27 C 1.1126(9) 0.0856(5) 1.1419(6) 0.061(4) Uani 1 1 d . . . H27A H 1.1449 0.1231 1.1338 0.073 Uiso 1 1 calc R . . H27B H 1.1635 0.0572 1.1538 0.073 Uiso 1 1 calc R . . C28 C 1.0397(8) 0.0929(5) 1.1969(5) 0.048(3) Uani 1 1 d . . . H28A H 1.0766 0.1017 1.2355 0.058 Uiso 1 1 calc R . . H28B H 0.9957 0.1259 1.1881 0.058 Uiso 1 1 calc R . . C29 C 0.6881(7) 0.0354(4) 1.3491(4) 0.030(2) Uani 1 1 d . . . H29A H 0.6814 -0.0077 1.3522 0.036 Uiso 1 1 calc R . . C30 C 0.7114(8) 0.0595(5) 1.4140(4) 0.043(3) Uani 1 1 d . . . H30A H 0.7229 0.1018 1.4114 0.051 Uiso 1 1 calc R . . H30B H 0.7712 0.0410 1.4307 0.051 Uiso 1 1 calc R . . C31 C 0.6251(10) 0.0473(6) 1.4580(5) 0.062(4) Uani 1 1 d . . . H31A H 0.6199 0.0050 1.4649 0.074 Uiso 1 1 calc R . . H31B H 0.6387 0.0658 1.4986 0.074 Uiso 1 1 calc R . . C32 C 0.5276(9) 0.0701(6) 1.4320(6) 0.062(4) Uani 1 1 d . . . H32A H 0.4746 0.0584 1.4597 0.074 Uiso 1 1 calc R . . H32B H 0.5292 0.1130 1.4306 0.074 Uiso 1 1 calc R . . C33 C 0.5071(9) 0.0468(6) 1.3675(6) 0.060(3) Uani 1 1 d . . . H33A H 0.4466 0.0644 1.3507 0.072 Uiso 1 1 calc R . . H33B H 0.4973 0.0043 1.3696 0.072 Uiso 1 1 calc R . . C34 C 0.5924(8) 0.0603(5) 1.3230(5) 0.045(3) Uani 1 1 d . . . H34A H 0.5783 0.0432 1.2818 0.054 Uiso 1 1 calc R . . H34B H 0.5987 0.1027 1.3179 0.054 Uiso 1 1 calc R . . C35 C 0.7399(8) 0.1499(4) 1.0634(4) 0.034(2) Uani 1 1 d . . . C36 C 0.7338(9) 0.1397(5) 0.9907(4) 0.047(3) Uani 1 1 d . . . C37 C 0.8097(11) 0.1762(7) 0.9534(5) 0.087(5) Uani 1 1 d . . . H37A H 0.7958 0.2175 0.9583 0.131 Uiso 1 1 calc R . . H37B H 0.8051 0.1658 0.9094 0.131 Uiso 1 1 calc R . . H37C H 0.8753 0.1678 0.9691 0.131 Uiso 1 1 calc R . . C38 C 0.7621(11) 0.0744(5) 0.9786(5) 0.070(4) Uani 1 1 d . . . H38A H 0.7181 0.0490 1.0013 0.105 Uiso 1 1 calc R . . H38B H 0.8291 0.0677 0.9929 0.105 Uiso 1 1 calc R . . H38C H 0.7565 0.0661 0.9342 0.105 Uiso 1 1 calc R . . C39 C 0.6323(9) 0.1530(6) 0.9672(5) 0.060(3) Uani 1 1 d . . . H39A H 0.6172 0.1938 0.9755 0.091 Uiso 1 1 calc R . . H39B H 0.5856 0.1282 0.9884 0.091 Uiso 1 1 calc R . . H39C H 0.6282 0.1458 0.9225 0.091 Uiso 1 1 calc R . . C40 C 0.6128(7) 0.0720(4) 1.0942(4) 0.034(2) Uani 1 1 d . . . H40A H 0.6033 0.0659 1.0486 0.041 Uiso 1 1 calc R . . C41 C 0.5137(8) 0.0885(5) 1.1220(6) 0.049(3) Uani 1 1 d . . . H41A H 0.4898 0.1244 1.1019 0.059 Uiso 1 1 calc R . . H41B H 0.5229 0.0965 1.1667 0.059 Uiso 1 1 calc R . . C42 C 0.4361(9) 0.0402(5) 1.1136(7) 0.063(4) Uani 1 1 d . . . H42A H 0.3753 0.0517 1.1341 0.075 Uiso 1 1 calc R . . H42B H 0.4216 0.0343 1.0690 0.075 Uiso 1 1 calc R . . C43 C 0.4753(10) -0.0159(5) 1.1423(6) 0.067(4) Uani 1 1 d . . . H43A H 0.4272 -0.0472 1.1354 0.081 Uiso 1 1 calc R . . H43B H 0.4835 -0.0104 1.1875 0.081 Uiso 1 1 calc R . . C44 C 0.5733(9) -0.0345(5) 1.1150(6) 0.059(3) Uani 1 1 d . . . H44A H 0.5644 -0.0439 1.0705 0.071 Uiso 1 1 calc R . . H44B H 0.5974 -0.0697 1.1366 0.071 Uiso 1 1 calc R . . C45 C 0.6489(8) 0.0154(4) 1.1227(6) 0.050(3) Uani 1 1 d . . . H45A H 0.6629 0.0215 1.1674 0.060 Uiso 1 1 calc R . . H45B H 0.7103 0.0039 1.1028 0.060 Uiso 1 1 calc R . . C46 C 0.8598(9) 0.2362(4) 1.0779(4) 0.044(3) Uani 1 1 d . . . H46A H 0.8846 0.2291 1.0353 0.053 Uiso 1 1 calc R . . C47 C 0.8083(13) 0.2923(6) 1.0788(13) 0.156(11) Uani 1 1 d . . . H47A H 0.7791 0.2982 1.1199 0.187 Uiso 1 1 calc R . . H47B H 0.7553 0.2920 1.0473 0.187 Uiso 1 1 calc R . . C48 C 0.8809(18) 0.3439(8) 1.0648(16) 0.171(13) Uani 1 1 d . . . H48A H 0.9030 0.3406 1.0216 0.205 Uiso 1 1 calc R . . H48B H 0.8458 0.3811 1.0687 0.205 Uiso 1 1 calc R . . C49 C 0.966(3) 0.3445(12) 1.1064(10) 0.181(18) Uani 1 1 d . . . H49A H 1.0111 0.3752 1.0932 0.217 Uiso 1 1 calc R . . H49B H 0.9448 0.3537 1.1489 0.217 Uiso 1 1 calc R . . C50 C 1.0136(16) 0.2907(10) 1.1065(11) 0.141(9) Uani 1 1 d . . . H50A H 1.0685 0.2922 1.1366 0.169 Uiso 1 1 calc R . . H50B H 1.0409 0.2839 1.0650 0.169 Uiso 1 1 calc R . . C51 C 0.9458(13) 0.2382(7) 1.1234(8) 0.106(6) Uani 1 1 d . . . H51A H 0.9828 0.2015 1.1213 0.127 Uiso 1 1 calc R . . H51B H 0.9220 0.2429 1.1661 0.127 Uiso 1 1 calc R . . C52 C 1.235(2) 0.4819(8) 1.2384(8) 0.150(10) Uani 1 1 d . . . H52A H 1.2900 0.4966 1.2137 0.181 Uiso 1 1 calc R . . H52B H 1.1924 0.5149 1.2486 0.181 Uiso 1 1 calc R . . C53 C 1.1795(17) 0.4370(10) 1.2025(10) 0.132(7) Uani 1 1 d . . . H53A H 1.1101 0.4360 1.2138 0.159 Uiso 1 1 calc R . . H53B H 1.1851 0.4424 1.1572 0.159 Uiso 1 1 calc R . . C54 C 1.233(3) 0.3848(8) 1.2247(10) 0.206(16) Uani 1 1 d . . . H54A H 1.1892 0.3508 1.2249 0.247 Uiso 1 1 calc R . . H54B H 1.2881 0.3764 1.1972 0.247 Uiso 1 1 calc R . . C55 C 1.266(2) 0.3966(7) 1.2838(11) 0.171(12) Uani 1 1 d . . . H55A H 1.2225 0.3789 1.3143 0.205 Uiso 1 1 calc R . . H55B H 1.3319 0.3798 1.2900 0.205 Uiso 1 1 calc R . . C56 C 0.657(2) 0.8569(9) 0.728(2) 0.197(18) Uani 1 1 d . . . H56A H 0.7013 0.8864 0.7108 0.236 Uiso 1 1 calc R . . H56B H 0.6012 0.8766 0.7471 0.236 Uiso 1 1 calc R . . C57 C 0.698(2) 0.827(2) 0.764(2) 0.26(3) Uani 1 1 d . . . H57A H 0.6769 0.8422 0.8047 0.309 Uiso 1 1 calc R . . H57B H 0.7670 0.8393 0.7609 0.309 Uiso 1 1 calc R . . C58 C 0.705(3) 0.7688(16) 0.7738(13) 0.24(2) Uani 1 1 d . . . H58A H 0.6596 0.7544 0.8056 0.291 Uiso 1 1 calc R . . H58B H 0.7717 0.7552 0.7825 0.291 Uiso 1 1 calc R . . C59 C 0.6691(19) 0.7564(10) 0.7061(11) 0.146(9) Uani 1 1 d . . . H59A H 0.6192 0.7255 0.7058 0.175 Uiso 1 1 calc R . . H59B H 0.7242 0.7436 0.6806 0.175 Uiso 1 1 calc R . . N1 N 0.9593(6) 0.1665(4) 1.4297(3) 0.039(2) Uani 1 1 d . . . N2 N 0.8293(6) 0.2214(3) 1.4244(3) 0.0311(19) Uani 1 1 d . . . N3 N 0.9068(5) 0.0511(3) 1.2548(3) 0.0281(18) Uani 1 1 d . . . N4 N 0.7697(6) 0.0488(3) 1.3059(4) 0.032(2) Uani 1 1 d . . . N5 N 0.6846(6) 0.1198(3) 1.1037(3) 0.037(2) Uani 1 1 d . . . N6 N 0.7938(7) 0.1868(4) 1.0956(4) 0.043(2) Uani 1 1 d . . . O1 O 1.2702(13) 0.4553(8) 1.2929(7) 0.160(6) Uani 1 1 d . . . O2 O 0.6242(16) 0.8152(12) 0.6791(11) 0.212(8) Uani 1 1 d . . . 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 0.0757(7) 0.0834(6) 0.0426(4) -0.0061(4) 0.0135(4) -0.0387(5) I2 0.0662(6) 0.0451(4) 0.0457(4) -0.0017(3) 0.0054(4) 0.0145(4) Ga1 0.0372(7) 0.0380(6) 0.0214(5) -0.0050(4) 0.0036(5) 0.0038(5) Ga2 0.0353(7) 0.0287(5) 0.0208(5) 0.0000(4) 0.0074(5) 0.0000(5) Ga3 0.0388(7) 0.0327(6) 0.0209(5) 0.0021(4) 0.0034(5) -0.0057(5) C1 0.025(6) 0.036(5) 0.029(5) -0.007(4) -0.002(5) -0.001(5) C2 0.040(7) 0.053(6) 0.032(5) -0.003(5) 0.003(5) -0.004(5) C3 0.096(11) 0.084(9) 0.018(5) -0.016(5) -0.008(6) 0.031(8) C4 0.063(9) 0.132(12) 0.032(6) 0.028(7) -0.001(6) -0.019(8) C5 0.090(11) 0.070(8) 0.044(7) -0.018(6) 0.005(7) 0.008(7) C6 0.042(7) 0.059(7) 0.034(5) -0.004(5) 0.008(5) 0.013(6) C7 0.102(15) 0.062(10) 0.40(4) -0.052(15) -0.19(2) 0.031(10) C8 0.15(2) 0.033(9) 0.46(5) -0.015(16) -0.20(3) 0.001(11) C9 0.28(4) 0.36(5) 0.057(12) -0.10(2) -0.001(18) 0.18(4) C10 0.015(9) 0.36(4) 0.39(5) 0.28(4) 0.024(18) -0.009(17) C11 0.010(8) 0.166(19) 0.59(6) 0.22(3) 0.072(17) 0.036(10) C12 0.039(7) 0.026(5) 0.029(5) -0.001(4) 0.011(5) 0.002(5) C13 0.061(9) 0.052(7) 0.089(10) -0.008(7) -0.001(8) 0.023(7) C14 0.033(8) 0.079(10) 0.120(13) -0.003(9) -0.006(8) 0.017(7) C15 0.079(12) 0.083(10) 0.080(10) 0.027(8) 0.038(9) 0.049(9) C16 0.071(11) 0.039(7) 0.133(13) 0.017(7) 0.048(10) 0.014(7) C17 0.074(10) 0.046(7) 0.118(12) 0.016(7) 0.041(9) 0.012(7) C18 0.032(6) 0.036(5) 0.023(5) 0.005(4) 0.005(4) 0.004(5) C19 0.052(7) 0.026(5) 0.036(5) -0.002(4) 0.006(5) -0.003(5) C20 0.056(8) 0.034(6) 0.055(7) 0.005(5) 0.005(6) -0.001(5) C21 0.083(10) 0.031(6) 0.058(7) -0.004(5) 0.018(7) 0.012(6) C22 0.056(8) 0.032(5) 0.047(6) 0.010(4) 0.012(6) 0.008(5) C23 0.030(6) 0.038(5) 0.029(5) -0.002(4) 0.006(5) 0.007(5) C24 0.043(7) 0.047(6) 0.036(6) -0.006(5) 0.008(5) -0.010(5) C25 0.088(10) 0.056(7) 0.044(6) -0.016(5) 0.031(7) -0.005(7) C26 0.089(11) 0.080(9) 0.054(7) -0.009(6) 0.049(8) -0.015(8) C27 0.053(8) 0.068(8) 0.063(8) -0.018(6) 0.026(7) -0.014(6) C28 0.055(8) 0.054(6) 0.036(5) -0.016(5) 0.022(6) -0.010(6) C29 0.028(6) 0.036(5) 0.026(5) 0.004(4) 0.011(4) -0.006(4) C30 0.040(7) 0.053(6) 0.036(6) 0.006(5) 0.014(5) -0.008(5) C31 0.072(10) 0.078(8) 0.036(6) -0.002(6) 0.029(7) -0.030(7) C32 0.036(8) 0.076(8) 0.074(9) -0.004(7) 0.033(7) -0.006(6) C33 0.040(8) 0.075(8) 0.067(8) 0.003(6) 0.020(7) -0.004(6) C34 0.030(7) 0.058(7) 0.047(6) 0.008(5) 0.005(6) 0.005(5) C35 0.032(6) 0.043(6) 0.028(5) 0.003(4) 0.005(5) -0.005(5) C36 0.056(8) 0.062(7) 0.024(5) -0.002(5) 0.008(5) -0.013(6) C37 0.101(12) 0.132(12) 0.029(6) -0.017(7) 0.024(7) -0.055(10) C38 0.100(12) 0.077(9) 0.033(6) -0.016(6) 0.021(7) -0.005(8) C39 0.056(9) 0.087(9) 0.037(6) 0.016(6) -0.005(6) -0.013(7) C40 0.034(6) 0.034(5) 0.034(5) -0.002(4) -0.001(5) -0.004(5) C41 0.028(7) 0.051(7) 0.068(8) 0.001(6) 0.000(6) 0.006(5) C42 0.031(7) 0.067(8) 0.089(10) -0.008(7) 0.002(7) -0.017(6) C43 0.080(10) 0.056(8) 0.065(8) -0.006(6) 0.015(8) -0.032(7) C44 0.046(8) 0.046(7) 0.084(9) -0.004(6) -0.004(7) -0.007(6) C45 0.038(7) 0.049(7) 0.062(7) -0.002(5) -0.002(6) -0.012(6) C46 0.055(8) 0.056(7) 0.022(5) 0.005(4) 0.006(5) -0.031(6) C47 0.088(13) 0.049(9) 0.33(3) 0.064(13) 0.094(17) 0.011(9) C48 0.15(2) 0.051(11) 0.31(4) 0.067(17) 0.12(2) 0.008(12) C49 0.32(4) 0.14(2) 0.086(14) -0.064(15) 0.10(2) -0.16(3) C50 0.128(18) 0.142(18) 0.152(19) 0.050(16) -0.028(15) -0.098(17) C51 0.109(14) 0.098(12) 0.111(13) 0.033(10) -0.039(12) -0.078(11) C52 0.29(3) 0.108(14) 0.057(10) 0.010(10) 0.037(15) -0.065(17) C53 0.139(19) 0.145(18) 0.111(15) -0.028(14) -0.054(14) 0.027(15) C54 0.42(5) 0.077(13) 0.117(17) -0.047(12) -0.11(2) 0.06(2) C55 0.32(4) 0.048(10) 0.14(2) -0.020(11) -0.07(2) 0.019(15) C56 0.15(3) 0.069(14) 0.37(5) -0.10(2) 0.03(3) -0.037(15) C57 0.10(2) 0.43(8) 0.24(4) 0.01(5) -0.12(3) -0.02(3) C58 0.28(4) 0.35(5) 0.102(18) -0.01(2) 0.03(2) 0.25(4) C59 0.17(2) 0.141(19) 0.130(19) -0.034(15) 0.032(17) 0.031(17) N1 0.037(5) 0.054(5) 0.026(4) -0.010(4) -0.010(4) 0.018(4) N2 0.036(5) 0.037(4) 0.021(4) -0.003(3) -0.002(4) 0.007(4) N3 0.023(5) 0.032(4) 0.030(4) -0.002(3) 0.010(4) 0.001(3) N4 0.026(5) 0.032(4) 0.040(4) 0.008(3) 0.011(4) -0.002(4) N5 0.046(6) 0.039(5) 0.024(4) -0.001(3) 0.003(4) -0.010(4) N6 0.054(6) 0.048(5) 0.025(4) 0.004(4) 0.009(4) -0.011(5) O1 0.192(16) 0.184(16) 0.103(11) -0.016(11) -0.017(11) -0.050(12) O2 0.20(2) 0.22(2) 0.21(2) 0.057(18) -0.014(17) 0.022(18) _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 2.5915(13) . ? I2 Ga3 2.6017(13) . ? Ga1 N2 1.968(7) . ? Ga1 N1 1.973(8) . ? Ga1 C1 2.426(9) . ? Ga1 Ga2 2.4292(15) . ? Ga2 N3 1.969(7) . ? Ga2 N4 1.985(7) . ? Ga2 Ga3 2.4246(16) . ? Ga2 C18 2.459(9) . ? Ga3 N5 1.951(8) . ? Ga3 N6 1.974(7) . ? Ga3 C35 2.422(9) . ? C1 N2 1.317(12) . ? C1 N1 1.334(11) . ? C1 C2 1.543(13) . ? C2 C3 1.484(16) . ? C2 C4 1.512(15) . ? C2 C5 1.536(15) . ? C6 C11 1.407(17) . ? C6 C7 1.446(18) . ? C6 N1 1.457(13) . ? C7 C8 1.59(2) . ? C8 C9 1.37(4) . ? C9 C10 1.27(4) . ? C10 C11 1.66(3) . ? C12 N2 1.452(12) . ? C12 C17 1.490(14) . ? C12 C13 1.511(16) . ? C13 C14 1.540(16) . ? C14 C15 1.459(18) . ? C15 C16 1.46(2) . ? C16 C17 1.508(16) . ? C18 N4 1.340(11) . ? C18 N3 1.351(11) . ? C18 C19 1.503(12) . ? C19 C21 1.527(14) . ? C19 C22 1.526(13) . ? C19 C20 1.537(15) . ? C23 N3 1.461(10) . ? C23 C24 1.497(14) . ? C23 C28 1.506(14) . ? C24 C25 1.511(13) . ? C25 C26 1.476(16) . ? C26 C27 1.497(18) . ? C27 C28 1.545(12) . ? C29 N4 1.473(10) . ? C29 C34 1.505(14) . ? C29 C30 1.505(13) . ? C30 C31 1.528(13) . ? C31 C32 1.509(18) . ? C32 C33 1.485(17) . ? C33 C34 1.528(13) . ? C35 N6 1.293(13) . ? C35 N5 1.329(11) . ? C35 C36 1.557(13) . ? C36 C39 1.479(16) . ? C36 C37 1.542(15) . ? C36 C38 1.547(16) . ? C40 N5 1.464(12) . ? C40 C45 1.493(14) . ? C40 C41 1.516(13) . ? C41 C42 1.521(15) . ? C42 C43 1.500(17) . ? C43 C44 1.511(16) . ? C44 C45 1.529(15) . ? C46 C47 1.448(18) . ? C46 N6 1.479(12) . ? C46 C51 1.494(19) . ? C47 C48 1.55(2) . ? C48 C49 1.43(3) . ? C49 C50 1.38(3) . ? C50 C51 1.54(2) . ? C52 O1 1.38(2) . ? C52 C53 1.47(3) . ? C53 C54 1.46(3) . ? C54 C55 1.35(3) . ? C55 O1 1.34(2) . ? C56 C57 1.16(5) . ? C56 O2 1.46(3) . ? C57 C58 1.34(5) . ? C58 C59 1.53(4) . ? C59 O2 1.56(3) . ? 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 66.2(3) . . ? N2 Ga1 C1 32.8(3) . . ? N1 Ga1 C1 33.3(3) . . ? N2 Ga1 Ga2 127.9(2) . . ? N1 Ga1 Ga2 125.5(2) . . ? C1 Ga1 Ga2 135.0(2) . . ? N2 Ga1 I1 106.4(2) . . ? N1 Ga1 I1 105.6(3) . . ? C1 Ga1 I1 109.7(2) . . ? Ga2 Ga1 I1 115.23(5) . . ? N3 Ga2 N4 66.2(3) . . ? N3 Ga2 Ga3 114.3(2) . . ? N4 Ga2 Ga3 115.0(3) . . ? N3 Ga2 Ga1 115.3(2) . . ? N4 Ga2 Ga1 114.2(2) . . ? Ga3 Ga2 Ga1 120.17(5) . . ? N3 Ga2 C18 33.2(3) . . ? N4 Ga2 C18 32.9(3) . . ? Ga3 Ga2 C18 119.9(2) . . ? Ga1 Ga2 C18 119.9(2) . . ? N5 Ga3 N6 65.4(3) . . ? N5 Ga3 C35 33.2(3) . . ? N6 Ga3 C35 32.2(3) . . ? N5 Ga3 Ga2 130.9(2) . . ? N6 Ga3 Ga2 130.1(3) . . ? C35 Ga3 Ga2 140.1(2) . . ? N5 Ga3 I2 107.2(3) . . ? N6 Ga3 I2 106.4(3) . . ? C35 Ga3 I2 110.5(2) . . ? Ga2 Ga3 I2 109.39(4) . . ? N2 C1 N1 108.4(8) . . ? N2 C1 C2 123.6(8) . . ? N1 C1 C2 128.0(9) . . ? N2 C1 Ga1 54.1(4) . . ? N1 C1 Ga1 54.4(5) . . ? C2 C1 Ga1 177.2(7) . . ? C3 C2 C4 110.1(10) . . ? C3 C2 C5 106.5(10) . . ? C4 C2 C5 110.2(10) . . ? C3 C2 C1 114.6(8) . . ? C4 C2 C1 107.9(9) . . ? C5 C2 C1 107.5(8) . . ? C11 C6 C7 108.2(18) . . ? C11 C6 N1 109.4(10) . . ? C7 C6 N1 110.5(10) . . ? C6 C7 C8 112.4(13) . . ? C9 C8 C7 105(2) . . ? C10 C9 C8 117(2) . . ? C9 C10 C11 103(3) . . ? C6 C11 C10 108.8(13) . . ? N2 C12 C17 112.3(8) . . ? N2 C12 C13 109.7(8) . . ? C17 C12 C13 109.5(10) . . ? C12 C13 C14 110.8(10) . . ? C15 C14 C13 111.6(11) . . ? C14 C15 C16 112.8(12) . . ? C15 C16 C17 111.2(12) . . ? C12 C17 C16 111.7(9) . . ? N4 C18 N3 106.7(7) . . ? N4 C18 C19 124.3(8) . . ? N3 C18 C19 129.0(8) . . ? N4 C18 Ga2 53.7(4) . . ? N3 C18 Ga2 53.0(4) . . ? C19 C18 Ga2 177.6(7) . . ? C18 C19 C21 114.9(8) . . ? C18 C19 C22 110.7(7) . . ? C21 C19 C22 105.0(9) . . ? C18 C19 C20 109.9(9) . . ? C21 C19 C20 106.5(8) . . ? C22 C19 C20 109.5(8) . . ? N3 C23 C24 111.1(8) . . ? N3 C23 C28 106.8(7) . . ? C24 C23 C28 110.3(8) . . ? C23 C24 C25 111.2(9) . . ? C26 C25 C24 110.0(9) . . ? C25 C26 C27 111.9(10) . . ? C26 C27 C28 111.3(10) . . ? C23 C28 C27 111.2(8) . . ? N4 C29 C34 109.9(7) . . ? N4 C29 C30 110.2(8) . . ? C34 C29 C30 111.3(8) . . ? C29 C30 C31 109.9(9) . . ? C32 C31 C30 112.6(9) . . ? C33 C32 C31 111.2(10) . . ? C32 C33 C34 111.4(10) . . ? C29 C34 C33 110.5(9) . . ? N6 C35 N5 108.0(8) . . ? N6 C35 C36 129.5(8) . . ? N5 C35 C36 122.5(9) . . ? N6 C35 Ga3 54.5(5) . . ? N5 C35 Ga3 53.5(5) . . ? C36 C35 Ga3 176.0(7) . . ? C39 C36 C37 109.7(10) . . ? C39 C36 C38 111.6(10) . . ? C37 C36 C38 105.0(9) . . ? C39 C36 C35 109.6(9) . . ? C37 C36 C35 113.7(9) . . ? C38 C36 C35 107.2(9) . . ? N5 C40 C45 111.5(9) . . ? N5 C40 C41 110.5(8) . . ? C45 C40 C41 109.7(8) . . ? C40 C41 C42 112.8(9) . . ? C43 C42 C41 108.8(10) . . ? C42 C43 C44 112.7(10) . . ? C43 C44 C45 109.8(9) . . ? C40 C45 C44 112.1(10) . . ? C47 C46 N6 111.6(10) . . ? C47 C46 C51 109.3(14) . . ? N6 C46 C51 108.9(9) . . ? C46 C47 C48 110.6(13) . . ? C49 C48 C47 113(2) . . ? C50 C49 C48 111.3(17) . . ? C49 C50 C51 113(2) . . ? C46 C51 C50 109.3(13) . . ? O1 C52 C53 107.2(15) . . ? C54 C53 C52 98.4(19) . . ? C55 C54 C53 107.2(16) . . ? O1 C55 C54 109.9(18) . . ? C57 C56 O2 103(3) . . ? C56 C57 C58 135(5) . . ? C57 C58 C59 91(3) . . ? C58 C59 O2 107.4(19) . . ? C1 N1 C6 133.2(8) . . ? C1 N1 Ga1 92.3(6) . . ? C6 N1 Ga1 133.8(6) . . ? C1 N2 C12 130.7(7) . . ? C1 N2 Ga1 93.1(5) . . ? C12 N2 Ga1 135.9(6) . . ? C18 N3 C23 130.0(7) . . ? C18 N3 Ga2 93.7(5) . . ? C23 N3 Ga2 131.4(6) . . ? C18 N4 C29 130.9(7) . . ? C18 N4 Ga2 93.4(5) . . ? C29 N4 Ga2 134.8(6) . . ? C35 N5 C40 131.8(8) . . ? C35 N5 Ga3 93.2(6) . . ? C40 N5 Ga3 134.9(6) . . ? C35 N6 C46 133.6(8) . . ? C35 N6 Ga3 93.3(6) . . ? C46 N6 Ga3 132.6(6) . . ? C55 O1 C52 107.5(16) . . ? C56 O2 C59 100(2) . . ? _diffrn_measured_fraction_theta_max 0.876 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.876 _refine_diff_density_max 1.136 _refine_diff_density_min -0.807 _refine_diff_density_rms 0.151 _exptl_crystal_recrystallization_method 'from tetrahydrofurane' # Attachment '- 4 - TZE55A.CIF' data_4 _database_code_depnum_ccdc_archive 'CCDC 811980' _audit_creation_method SHELXL-97 _chemical_name_systematic ; N,N'-dicyclohexylneopentylamidinato-isopropylimino-gallium(II)-N,N' -dicyclohexylneopentylamidinato-iodo-gallium(II)-N,N' -dicyclohexylneopentylamidinato-gallium(I) ; _chemical_name_common ; N,N'-dicyclohexylneopentylamidinato-isopropylimino- gallium(ii)-N,N' -dicyclohexylneopentylamidinato-iodo-gallium(ii)-N,N' - dicyclohexylneopentylamidinato-gallium(i) ; _chemical_melting_point '533 (dec)' _chemical_formula_moiety ;C54 H99 Ga3 I N7, 3(C4 H8 O) ; _chemical_formula_sum 'C66 H123 Ga3 I N7 O3' _chemical_formula_weight 1398.77 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' 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 'C c' _symmetry_int_tables_number 9 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 13.184(3) _cell_length_b 30.314(6) _cell_length_c 17.950(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.17(3) _cell_angle_gamma 90.00 _cell_volume 7145(2) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plates _exptl_crystal_colour colourless _exptl_crystal_size_max 0.258 _exptl_crystal_size_mid 0.202 _exptl_crystal_size_min 0.089 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.300 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2952 _exptl_absorpt_coefficient_mu 1.601 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.5012 _exptl_absorpt_correction_T_max 0.8727 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23360 _diffrn_reflns_av_R_equivalents 0.1485 _diffrn_reflns_av_sigmaI/netI 0.2570 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 24.26 _reflns_number_total 10854 _reflns_number_gt 4701 _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^)+(0.0324P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _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 -0.01(3) _refine_ls_number_reflns 10854 _refine_ls_number_parameters 721 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.1440 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.1640 _refine_ls_wR_factor_gt 0.1358 _refine_ls_goodness_of_fit_ref 0.769 _refine_ls_restrained_S_all 0.770 _refine_ls_shift/su_max 0.007 _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 -0.14844(8) 0.40267(4) 0.25880(6) 0.0418(3) Uani 1 1 d . . . Ga2 Ga -0.13406(7) 0.36135(3) 0.14506(6) 0.0339(3) Uani 1 1 d . . . Ga3 Ga 0.00437(8) 0.31064(4) 0.12549(7) 0.0376(3) Uani 1 1 d . . . I1 I 0.00656(8) 0.45271(4) 0.29019(7) 0.1018(4) Uani 1 1 d . . . N1 N -0.1850(6) 0.3779(3) 0.3523(4) 0.039(2) Uani 1 1 d . . . N2 N -0.2700(7) 0.4306(3) 0.2960(5) 0.043(2) Uani 1 1 d . . . N3 N -0.2659(6) 0.3403(3) 0.0997(5) 0.048(3) Uani 1 1 d . . . N4 N -0.1868(5) 0.3946(2) 0.0545(4) 0.032(2) Uani 1 1 d . . . N5 N 0.1412(6) 0.3279(3) 0.1046(5) 0.040(2) Uani 1 1 d . . . N6 N 0.0361(6) 0.2911(3) 0.0253(4) 0.044(2) Uani 1 1 d . . . C1 C -0.2681(7) 0.4041(4) 0.3557(6) 0.042(3) Uani 1 1 d . . . C2 C -0.3468(8) 0.4045(4) 0.4101(6) 0.053(3) Uani 1 1 d . . . C3 C -0.3523(9) 0.4482(4) 0.4512(7) 0.067(4) Uani 1 1 d . . . H3A H -0.3587 0.4724 0.4148 0.101 Uiso 1 1 calc R . . H3B H -0.2901 0.4523 0.4848 0.101 Uiso 1 1 calc R . . H3C H -0.4115 0.4482 0.4805 0.101 Uiso 1 1 calc R . . C4 C -0.4512(8) 0.3947(4) 0.3656(8) 0.068(4) Uani 1 1 d . . . H4A H -0.4664 0.4178 0.3281 0.102 Uiso 1 1 calc R . . H4B H -0.5047 0.3941 0.4000 0.102 Uiso 1 1 calc R . . H4C H -0.4481 0.3661 0.3406 0.102 Uiso 1 1 calc R . . C5 C -0.3340(10) 0.3662(4) 0.4678(7) 0.083(4) Uani 1 1 d . . . H5A H -0.2678 0.3688 0.4971 0.124 Uiso 1 1 calc R . . H5B H -0.3375 0.3379 0.4412 0.124 Uiso 1 1 calc R . . H5C H -0.3885 0.3676 0.5013 0.124 Uiso 1 1 calc R . . C6 C -0.1361(8) 0.3456(4) 0.4033(7) 0.054(3) Uani 1 1 d . . . H6A H -0.1883 0.3275 0.4265 0.064 Uiso 1 1 calc R . . C7 C -0.0659(10) 0.3698(4) 0.4649(7) 0.073(4) Uani 1 1 d . . . H7A H -0.0191 0.3897 0.4407 0.087 Uiso 1 1 calc R . . H7B H -0.1084 0.3882 0.4955 0.087 Uiso 1 1 calc R . . C8 C -0.0047(11) 0.3382(5) 0.5148(8) 0.097(5) Uani 1 1 d . . . H8A H -0.0510 0.3196 0.5420 0.116 Uiso 1 1 calc R . . H8B H 0.0401 0.3548 0.5521 0.116 Uiso 1 1 calc R . . C9 C 0.0605(9) 0.3086(4) 0.4684(7) 0.071(4) Uani 1 1 d . . . H9A H 0.1104 0.3272 0.4449 0.085 Uiso 1 1 calc R . . H9B H 0.0991 0.2876 0.5023 0.085 Uiso 1 1 calc R . . C10 C -0.0003(9) 0.2834(4) 0.4092(7) 0.062(4) Uani 1 1 d . . . H10A H -0.0435 0.2616 0.4324 0.074 Uiso 1 1 calc R . . H10B H 0.0460 0.2672 0.3784 0.074 Uiso 1 1 calc R . . C11 C -0.0714(8) 0.3165(4) 0.3564(6) 0.056(3) Uani 1 1 d . . . H11A H -0.0279 0.3353 0.3274 0.067 Uiso 1 1 calc R . . H11B H -0.1166 0.2990 0.3206 0.067 Uiso 1 1 calc R . . C12 C -0.3367(9) 0.4657(3) 0.2720(5) 0.049(3) Uani 1 1 d . . . H12A H -0.3911 0.4685 0.3071 0.059 Uiso 1 1 calc R . . C13 C -0.3851(9) 0.4553(4) 0.1938(6) 0.056(3) Uani 1 1 d . . . H13A H -0.4279 0.4285 0.1956 0.067 Uiso 1 1 calc R . . H13B H -0.3310 0.4491 0.1604 0.067 Uiso 1 1 calc R . . C14 C -0.4518(9) 0.4945(3) 0.1615(7) 0.056(3) Uani 1 1 d . . . H14A H -0.4811 0.4868 0.1104 0.067 Uiso 1 1 calc R . . H14B H -0.5090 0.4989 0.1929 0.067 Uiso 1 1 calc R . . C15 C -0.3919(11) 0.5378(4) 0.1583(7) 0.075(4) Uani 1 1 d . . . H15A H -0.3378 0.5348 0.1238 0.090 Uiso 1 1 calc R . . H15B H -0.4378 0.5622 0.1405 0.090 Uiso 1 1 calc R . . C16 C -0.3456(10) 0.5467(4) 0.2375(7) 0.066(4) Uani 1 1 d . . . H16A H -0.3045 0.5740 0.2376 0.079 Uiso 1 1 calc R . . H16B H -0.4011 0.5517 0.2701 0.079 Uiso 1 1 calc R . . C17 C -0.2794(9) 0.5096(3) 0.2691(6) 0.053(3) Uani 1 1 d . . . H17A H -0.2512 0.5176 0.3203 0.064 Uiso 1 1 calc R . . H17B H -0.2216 0.5058 0.2381 0.064 Uiso 1 1 calc R . . C18 C -0.2702(7) 0.3699(3) 0.0418(5) 0.035(3) Uani 1 1 d . . . C19 C -0.3585(9) 0.3762(3) -0.0161(6) 0.051(3) Uani 1 1 d . . . C20 C -0.4095(13) 0.4163(6) -0.0002(10) 0.146(7) Uani 1 1 d . . . H20A H -0.4415 0.4131 0.0467 0.219 Uiso 1 1 calc R . . H20B H -0.4619 0.4228 -0.0410 0.219 Uiso 1 1 calc R . . H20C H -0.3601 0.4405 0.0045 0.219 Uiso 1 1 calc R . . C21 C -0.4202(11) 0.3363(5) -0.0360(8) 0.106(5) Uani 1 1 d . . . H21A H -0.4545 0.3267 0.0075 0.159 Uiso 1 1 calc R . . H21B H -0.3757 0.3127 -0.0510 0.159 Uiso 1 1 calc R . . H21C H -0.4712 0.3432 -0.0775 0.159 Uiso 1 1 calc R . . C22 C -0.3135(14) 0.3853(6) -0.0932(8) 0.136(7) Uani 1 1 d . . . H22A H -0.3695 0.3891 -0.1325 0.204 Uiso 1 1 calc R . . H22B H -0.2711 0.3604 -0.1058 0.204 Uiso 1 1 calc R . . H22C H -0.2721 0.4122 -0.0893 0.204 Uiso 1 1 calc R . . C23 C -0.3418(9) 0.3070(3) 0.1224(7) 0.057(4) Uani 1 1 d . . . H23A H -0.3863 0.2972 0.0774 0.068 Uiso 1 1 calc R . . C24 C -0.4038(11) 0.3257(4) 0.1770(11) 0.116(6) Uani 1 1 d . . . H24A H -0.4417 0.3514 0.1548 0.139 Uiso 1 1 calc R . . H24B H -0.3591 0.3362 0.2207 0.139 Uiso 1 1 calc R . . C25 C -0.4782(11) 0.2923(4) 0.2025(10) 0.091(5) Uani 1 1 d . . . H25A H -0.5207 0.3059 0.2389 0.109 Uiso 1 1 calc R . . H25B H -0.5235 0.2817 0.1592 0.109 Uiso 1 1 calc R . . C26 C -0.4188(11) 0.2548(5) 0.2379(7) 0.091(5) Uani 1 1 d . . . H26A H -0.4662 0.2321 0.2541 0.110 Uiso 1 1 calc R . . H26B H -0.3765 0.2654 0.2827 0.110 Uiso 1 1 calc R . . C27 C -0.3510(12) 0.2345(4) 0.1833(11) 0.108(6) Uani 1 1 d . . . H27A H -0.3938 0.2217 0.1406 0.129 Uiso 1 1 calc R . . H27B H -0.3104 0.2104 0.2084 0.129 Uiso 1 1 calc R . . C28 C -0.2796(9) 0.2687(3) 0.1545(8) 0.070(4) Uani 1 1 d . . . H28A H -0.2307 0.2790 0.1960 0.084 Uiso 1 1 calc R . . H28B H -0.2407 0.2555 0.1155 0.084 Uiso 1 1 calc R . . C29 C -0.1462(8) 0.4290(3) 0.0155(6) 0.045(3) Uani 1 1 d . . . H29A H -0.1956 0.4376 -0.0276 0.054 Uiso 1 1 calc R . . C30 C -0.1216(18) 0.4697(4) 0.0657(12) 0.203(9) Uani 1 1 d . . . H30A H -0.0731 0.4607 0.1083 0.243 Uiso 1 1 calc R . . H30B H -0.1850 0.4795 0.0865 0.243 Uiso 1 1 calc R . . C31 C -0.0755(15) 0.5098(5) 0.0259(11) 0.145(7) Uani 1 1 d . . . H31A H -0.1248 0.5209 -0.0146 0.174 Uiso 1 1 calc R . . H31B H -0.0592 0.5339 0.0620 0.174 Uiso 1 1 calc R . . C32 C 0.0146(11) 0.4948(4) -0.0043(8) 0.082(5) Uani 1 1 d . . . H32A H 0.0348 0.5172 -0.0405 0.098 Uiso 1 1 calc R . . H32B H 0.0698 0.4932 0.0368 0.098 Uiso 1 1 calc R . . C33 C 0.0079(12) 0.4561(5) -0.0383(14) 0.144(9) Uani 1 1 d . . . H33A H 0.0786 0.4458 -0.0414 0.173 Uiso 1 1 calc R . . H33B H -0.0207 0.4619 -0.0903 0.173 Uiso 1 1 calc R . . C34 C -0.0492(9) 0.4184(4) -0.0116(11) 0.113(6) Uani 1 1 d . . . H34A H -0.0609 0.3969 -0.0530 0.136 Uiso 1 1 calc R . . H34B H -0.0063 0.4037 0.0292 0.136 Uiso 1 1 calc R . . C35 C 0.1297(7) 0.3104(3) 0.0323(6) 0.045(3) Uani 1 1 d . . . C36 C 0.2038(8) 0.3077(3) -0.0288(6) 0.047(3) Uani 1 1 d . . . C37 C 0.1570(10) 0.3350(5) -0.0926(7) 0.076(4) Uani 1 1 d . . . H37A H 0.2013 0.3344 -0.1336 0.114 Uiso 1 1 calc R . . H37B H 0.1491 0.3654 -0.0759 0.114 Uiso 1 1 calc R . . H37C H 0.0902 0.3228 -0.1101 0.114 Uiso 1 1 calc R . . C38 C 0.3067(9) 0.3272(5) -0.0112(8) 0.096(5) Uani 1 1 d . . . H38A H 0.3464 0.3239 -0.0545 0.143 Uiso 1 1 calc R . . H38B H 0.3415 0.3121 0.0320 0.143 Uiso 1 1 calc R . . H38C H 0.2999 0.3587 0.0003 0.143 Uiso 1 1 calc R . . C39 C 0.2224(11) 0.2621(4) -0.0538(8) 0.084(5) Uani 1 1 d . . . H39A H 0.2693 0.2627 -0.0932 0.125 Uiso 1 1 calc R . . H39B H 0.1578 0.2487 -0.0734 0.125 Uiso 1 1 calc R . . H39C H 0.2525 0.2447 -0.0114 0.125 Uiso 1 1 calc R . . C40 C 0.2210(9) 0.3549(4) 0.1362(6) 0.045(3) Uani 1 1 d . . . H40A H 0.2878 0.3443 0.1206 0.054 Uiso 1 1 calc R . . C41 C 0.2073(10) 0.4018(4) 0.1182(8) 0.078(4) Uani 1 1 d . . . H41A H 0.1426 0.4118 0.1366 0.093 Uiso 1 1 calc R . . H41B H 0.2007 0.4052 0.0631 0.093 Uiso 1 1 calc R . . C42 C 0.2935(11) 0.4323(5) 0.1510(8) 0.089(5) Uani 1 1 d . . . H42A H 0.3589 0.4241 0.1318 0.107 Uiso 1 1 calc R . . H42B H 0.2781 0.4634 0.1378 0.107 Uiso 1 1 calc R . . C43 C 0.2986(11) 0.4257(5) 0.2360(9) 0.098(5) Uani 1 1 d . . . H43A H 0.3585 0.4417 0.2596 0.117 Uiso 1 1 calc R . . H43B H 0.2371 0.4387 0.2548 0.117 Uiso 1 1 calc R . . C44 C 0.3059(12) 0.3797(4) 0.2586(8) 0.085(5) Uani 1 1 d . . . H44A H 0.3029 0.3777 0.3134 0.102 Uiso 1 1 calc R . . H44B H 0.3723 0.3677 0.2466 0.102 Uiso 1 1 calc R . . C45 C 0.2205(11) 0.3521(4) 0.2194(7) 0.077(5) Uani 1 1 d . . . H45A H 0.2288 0.3209 0.2354 0.093 Uiso 1 1 calc R . . H45B H 0.1541 0.3626 0.2342 0.093 Uiso 1 1 calc R . . C46 C -0.0186(8) 0.2667(4) -0.0352(7) 0.057(4) Uani 1 1 d . . . H46A H 0.0274 0.2621 -0.0759 0.068 Uiso 1 1 calc R . . C47 C -0.1098(10) 0.2959(5) -0.0658(8) 0.078(4) Uani 1 1 d . . . H47A H -0.1539 0.3030 -0.0256 0.094 Uiso 1 1 calc R . . H47B H -0.0855 0.3238 -0.0867 0.094 Uiso 1 1 calc R . . C48 C -0.1678(12) 0.2683(6) -0.1268(8) 0.099(6) Uani 1 1 d . . . H48A H -0.2249 0.2862 -0.1504 0.118 Uiso 1 1 calc R . . H48B H -0.1216 0.2616 -0.1658 0.118 Uiso 1 1 calc R . . C49 C -0.2081(11) 0.2275(6) -0.1008(8) 0.117(6) Uani 1 1 d . . . H49A H -0.2507 0.2329 -0.0590 0.141 Uiso 1 1 calc R . . H49B H -0.2500 0.2124 -0.1417 0.141 Uiso 1 1 calc R . . C50 C -0.1205(12) 0.2013(5) -0.0761(10) 0.111(6) Uani 1 1 d . . . H50A H -0.0797 0.1955 -0.1187 0.133 Uiso 1 1 calc R . . H50B H -0.1428 0.1726 -0.0568 0.133 Uiso 1 1 calc R . . C51 C -0.0543(10) 0.2261(4) -0.0135(7) 0.062(4) Uani 1 1 d . . . H51A H -0.0952 0.2306 0.0296 0.075 Uiso 1 1 calc R . . H51B H 0.0046 0.2074 0.0037 0.075 Uiso 1 1 calc R . . C52 C 0.0630(10) 0.2279(4) 0.2020(7) 0.074(3) Uani 1 1 d DU . . C53 C 0.1649(12) 0.2232(6) 0.1590(9) 0.128(5) Uani 1 1 d U . . H53A H 0.1780 0.2511 0.1339 0.193 Uiso 1 1 calc R . . H53B H 0.1557 0.1996 0.1218 0.193 Uiso 1 1 calc R . . H53C H 0.2227 0.2162 0.1952 0.193 Uiso 1 1 calc R . . O1 O -0.1224(10) 0.0486(5) 0.3177(7) 0.202(8) Uani 1 1 d D . . C55 C -0.2104(11) 0.0575(6) 0.3548(11) 0.342(19) Uani 1 1 d D . . H55A H -0.2737 0.0521 0.3221 0.410 Uiso 1 1 calc R . . H55B H -0.2105 0.0880 0.3744 0.410 Uiso 1 1 calc R . . C56 C -0.1966(11) 0.0254(5) 0.4142(11) 0.235(11) Uani 1 1 d D . . H56A H -0.1921 0.0409 0.4630 0.283 Uiso 1 1 calc R . . H56B H -0.2567 0.0057 0.4119 0.283 Uiso 1 1 calc R . . C57 C -0.1132(9) 0.0013(5) 0.4098(9) 0.122(7) Uani 1 1 d D . . H57A H -0.0707 0.0017 0.4582 0.146 Uiso 1 1 calc R . . H57B H -0.1316 -0.0296 0.3974 0.146 Uiso 1 1 calc R . . C58 C -0.0630(8) 0.0189(4) 0.3567(7) 0.077(5) Uani 1 1 d D . . H58A H -0.0426 -0.0046 0.3228 0.092 Uiso 1 1 calc R . . H58B H -0.0005 0.0335 0.3794 0.092 Uiso 1 1 calc R . . O2 O 0.4039(15) -0.0918(5) 0.6614(9) 0.427(18) Uani 1 1 d D . . C59 C 0.4816(17) -0.0769(5) 0.7151(16) 0.33(2) Uani 1 1 d D . . H59A H 0.4556 -0.0581 0.7542 0.399 Uiso 1 1 calc R . . H59B H 0.5381 -0.0619 0.6924 0.399 Uiso 1 1 calc R . . C60 C 0.5074(13) -0.1211(7) 0.7409(16) 0.31(2) Uani 1 1 d D . . H60A H 0.5444 -0.1370 0.7035 0.372 Uiso 1 1 calc R . . H60B H 0.5509 -0.1201 0.7888 0.372 Uiso 1 1 calc R . . C61 C 0.4188(16) -0.1410(8) 0.7500(11) 0.38(3) Uani 1 1 d D . . H61A H 0.4265 -0.1735 0.7511 0.460 Uiso 1 1 calc R . . H61B H 0.3908 -0.1311 0.7966 0.460 Uiso 1 1 calc R . . C62 C 0.3602(14) -0.1280(5) 0.6899(12) 0.252(17) Uani 1 1 d D . . H62A H 0.2912 -0.1207 0.7037 0.303 Uiso 1 1 calc R . . H62B H 0.3542 -0.1519 0.6522 0.303 Uiso 1 1 calc R . . O3 O -0.1707(15) -0.1304(6) 0.6197(9) 0.355(17) Uani 1 1 d D . . C63 C -0.2699(15) -0.1141(7) 0.6243(18) 0.558(19) Uani 1 1 d D . . H63A H -0.2888 -0.1124 0.6764 0.670 Uiso 1 1 calc R . . H63B H -0.3221 -0.1307 0.5927 0.670 Uiso 1 1 calc R . . C64 C -0.2482(18) -0.0712(6) 0.5936(13) 0.30(2) Uani 1 1 d D . . H64A H -0.3121 -0.0569 0.5728 0.362 Uiso 1 1 calc R . . H64B H -0.2152 -0.0519 0.6332 0.362 Uiso 1 1 calc R . . C65 C -0.1859(18) -0.0774(6) 0.5396(12) 0.30(2) Uani 1 1 d D . . H65A H -0.2218 -0.0911 0.4946 0.362 Uiso 1 1 calc R . . H65B H -0.1537 -0.0495 0.5255 0.362 Uiso 1 1 calc R . . C66 C -0.1186(15) -0.1048(7) 0.5739(16) 0.49(3) Uani 1 1 d D . . H66A H -0.0644 -0.0880 0.6035 0.591 Uiso 1 1 calc R . . H66B H -0.0867 -0.1232 0.5370 0.591 Uiso 1 1 calc R . . C54 C 0.0254(15) 0.1868(3) 0.2453(8) 0.125(5) Uani 1 1 d DU . . H54A H -0.0372 0.1944 0.2680 0.188 Uiso 1 1 calc R . . H54D H 0.0781 0.1781 0.2845 0.188 Uiso 1 1 calc R . . H54B H 0.0118 0.1622 0.2103 0.188 Uiso 1 1 calc R . . N7 N 0.0135(7) 0.2589(3) 0.1966(6) 0.058(3) Uani 1 1 d U . . 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 0.0352(6) 0.0539(7) 0.0363(6) -0.0064(6) 0.0030(5) 0.0040(6) Ga2 0.0295(5) 0.0416(6) 0.0305(6) -0.0006(6) 0.0024(5) -0.0029(6) Ga3 0.0350(6) 0.0452(6) 0.0333(6) -0.0007(6) 0.0061(5) 0.0029(6) I1 0.0776(6) 0.1127(7) 0.1147(8) -0.0426(7) 0.0065(6) -0.0130(7) N1 0.028(4) 0.055(5) 0.033(5) 0.003(4) 0.005(4) 0.018(4) N2 0.053(5) 0.042(5) 0.033(5) 0.000(4) -0.002(4) 0.014(4) N3 0.036(5) 0.044(5) 0.065(6) 0.000(5) 0.007(5) -0.010(4) N4 0.025(4) 0.023(4) 0.048(5) 0.011(4) -0.001(4) -0.002(3) N5 0.035(5) 0.044(5) 0.037(5) -0.008(4) -0.012(4) -0.001(4) N6 0.035(5) 0.070(6) 0.029(5) 0.000(4) 0.003(4) -0.006(4) C1 0.028(5) 0.059(6) 0.038(6) -0.016(6) 0.001(5) 0.008(5) C2 0.035(6) 0.076(8) 0.046(7) -0.001(6) -0.008(6) 0.012(6) C3 0.052(7) 0.098(9) 0.051(8) -0.013(7) 0.007(6) 0.011(7) C4 0.033(6) 0.091(9) 0.079(9) -0.011(8) -0.002(6) -0.008(7) C5 0.066(8) 0.119(10) 0.066(8) 0.034(8) 0.026(7) 0.047(8) C6 0.036(6) 0.067(7) 0.057(8) 0.008(6) 0.003(6) 0.011(6) C7 0.095(9) 0.053(7) 0.059(8) -0.024(6) -0.046(7) 0.031(7) C8 0.087(9) 0.115(11) 0.079(10) -0.014(9) -0.049(8) 0.048(9) C9 0.063(7) 0.093(9) 0.051(7) -0.003(7) -0.021(6) 0.034(8) C10 0.057(7) 0.053(7) 0.076(9) 0.000(6) 0.003(7) 0.020(6) C11 0.044(6) 0.061(7) 0.062(8) -0.025(6) 0.002(6) 0.012(6) C12 0.066(7) 0.069(7) 0.010(5) -0.013(5) -0.001(5) 0.024(6) C13 0.069(8) 0.058(7) 0.037(6) -0.021(6) -0.013(6) 0.020(6) C14 0.068(7) 0.038(6) 0.058(8) -0.007(5) -0.011(7) 0.011(6) C15 0.094(9) 0.066(8) 0.065(9) -0.027(7) 0.007(8) 0.021(8) C16 0.073(8) 0.043(6) 0.083(10) 0.013(7) 0.014(8) 0.016(6) C17 0.069(8) 0.052(6) 0.038(6) -0.002(5) -0.004(6) 0.000(6) C18 0.037(5) 0.037(6) 0.027(5) 0.012(4) -0.017(5) 0.012(5) C19 0.055(7) 0.055(7) 0.038(6) 0.003(5) -0.022(6) 0.011(6) C20 0.134(12) 0.168(16) 0.118(13) -0.033(12) -0.092(11) 0.073(13) C21 0.098(10) 0.131(12) 0.075(9) 0.038(9) -0.064(8) -0.046(10) C22 0.170(15) 0.181(14) 0.051(9) 0.057(9) -0.020(10) -0.108(13) C23 0.051(7) 0.038(6) 0.079(9) 0.016(6) -0.008(7) -0.005(6) C24 0.104(10) 0.040(7) 0.221(19) 0.004(9) 0.107(12) -0.003(7) C25 0.082(9) 0.081(9) 0.116(13) 0.008(9) 0.044(10) -0.017(8) C26 0.074(9) 0.149(13) 0.050(8) 0.040(9) -0.001(8) -0.029(10) C27 0.106(11) 0.055(8) 0.173(16) 0.038(9) 0.067(12) -0.017(8) C28 0.052(7) 0.049(6) 0.116(11) 0.048(7) 0.036(7) 0.020(6) C29 0.040(6) 0.053(6) 0.040(7) 0.005(6) 0.001(5) 0.001(5) C30 0.36(2) 0.053(9) 0.236(18) -0.015(10) 0.239(17) -0.070(12) C31 0.201(15) 0.085(10) 0.166(16) 0.035(11) 0.107(14) -0.069(11) C32 0.093(10) 0.066(8) 0.088(11) 0.013(8) 0.010(9) -0.050(8) C33 0.076(10) 0.080(11) 0.28(3) 0.023(15) 0.045(14) -0.031(10) C34 0.054(7) 0.051(8) 0.247(19) 0.035(10) 0.088(10) -0.015(6) C35 0.019(5) 0.055(6) 0.063(8) 0.019(6) 0.007(5) -0.010(5) C36 0.042(6) 0.055(7) 0.047(7) -0.003(6) 0.015(6) -0.008(6) C37 0.075(9) 0.109(10) 0.046(8) 0.006(8) 0.021(7) -0.019(8) C38 0.043(7) 0.178(14) 0.072(10) -0.028(10) 0.036(7) -0.048(9) C39 0.068(8) 0.087(9) 0.101(11) -0.045(8) 0.038(8) -0.003(8) C40 0.044(6) 0.055(7) 0.034(6) -0.018(5) 0.001(5) -0.003(6) C41 0.077(9) 0.063(8) 0.088(10) -0.006(8) -0.023(8) -0.021(8) C42 0.085(9) 0.111(11) 0.068(10) 0.015(8) -0.016(8) -0.054(9) C43 0.062(8) 0.129(12) 0.104(12) -0.055(10) 0.018(9) -0.036(9) C44 0.107(11) 0.068(8) 0.068(9) -0.014(7) -0.049(9) -0.008(8) C45 0.090(10) 0.072(9) 0.066(9) -0.005(7) -0.012(8) -0.008(8) C46 0.037(6) 0.071(8) 0.062(8) -0.016(7) 0.006(6) -0.021(6) C47 0.061(8) 0.097(10) 0.069(9) -0.028(8) -0.035(7) 0.001(8) C48 0.075(10) 0.163(14) 0.055(9) -0.047(10) -0.008(8) 0.003(11) C49 0.067(9) 0.217(16) 0.075(9) -0.096(10) 0.043(8) -0.074(10) C50 0.069(9) 0.117(11) 0.147(14) -0.086(10) 0.021(10) -0.029(9) C51 0.069(8) 0.064(7) 0.052(7) -0.010(6) -0.011(7) -0.028(7) C52 0.078(7) 0.075(7) 0.060(8) 0.018(6) -0.040(5) 0.001(6) C53 0.144(8) 0.169(12) 0.069(10) -0.005(9) -0.003(7) 0.124(8) O1 0.166(12) 0.293(19) 0.147(14) 0.012(14) 0.011(11) 0.099(14) C55 0.163(14) 0.53(4) 0.34(4) -0.08(4) 0.03(2) 0.26(2) C56 0.216(18) 0.158(16) 0.37(3) 0.132(17) 0.225(19) 0.126(14) C57 0.047(9) 0.153(15) 0.166(19) 0.018(14) 0.015(11) 0.010(11) C58 0.044(7) 0.110(11) 0.078(10) 0.001(9) 0.015(8) 0.018(8) O2 0.91(5) 0.174(14) 0.24(2) -0.071(16) 0.27(3) -0.20(3) C59 0.27(4) 0.103(15) 0.60(6) -0.16(3) -0.11(4) 0.00(2) C60 0.26(3) 0.39(5) 0.25(3) 0.09(4) -0.11(3) 0.09(4) C61 0.32(4) 0.72(8) 0.09(2) 0.08(3) -0.01(3) -0.28(5) C62 0.24(3) 0.105(15) 0.39(4) -0.08(2) -0.13(3) -0.057(17) O3 0.60(4) 0.30(2) 0.135(14) 0.062(16) -0.16(2) 0.03(3) C63 0.59(3) 0.67(4) 0.36(5) 0.27(4) -0.29(4) -0.560 C64 0.61(8) 0.16(2) 0.14(2) 0.074(18) 0.07(3) 0.05(3) C65 0.50(6) 0.178(19) 0.25(3) 0.16(2) 0.15(3) 0.00(3) C66 0.76(6) 0.091(18) 0.72(7) -0.02(3) 0.58(5) 0.04(3) C54 0.238(15) 0.022(5) 0.100(11) -0.005(6) -0.072(9) -0.004(8) N7 0.048(5) 0.054(5) 0.071(7) -0.026(5) 0.001(5) 0.017(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 N1 1.939(8) . ? Ga1 N2 1.981(9) . ? Ga1 Ga2 2.4172(16) . ? Ga1 C1 2.452(10) . ? Ga1 I1 2.5666(16) . ? Ga2 N3 1.958(8) . ? Ga2 N4 1.984(7) . ? Ga2 Ga3 2.4358(15) . ? Ga2 C18 2.475(9) . ? Ga3 N5 1.947(8) . ? Ga3 N6 1.974(8) . ? Ga3 N7 2.018(10) . ? Ga3 C35 2.454(11) . ? N1 C1 1.360(12) . ? N1 C6 1.449(13) . ? N2 C1 1.338(13) . ? N2 C12 1.422(12) . ? N3 C18 1.370(12) . ? N3 C23 1.504(13) . ? N4 C18 1.333(11) . ? N4 C29 1.391(12) . ? N5 C35 1.397(14) . ? N5 C40 1.411(13) . ? N6 C35 1.362(12) . ? N6 C46 1.451(14) . ? C1 C2 1.488(15) . ? C2 C3 1.521(16) . ? C2 C5 1.556(16) . ? C2 C4 1.558(15) . ? C6 C11 1.532(15) . ? C6 C7 1.560(15) . ? C7 C8 1.499(17) . ? C8 C9 1.537(18) . ? C9 C10 1.484(17) . ? C10 C11 1.618(16) . ? C12 C13 1.523(14) . ? C12 C17 1.533(15) . ? C13 C14 1.559(14) . ? C14 C15 1.535(16) . ? C15 C16 1.520(17) . ? C16 C17 1.503(15) . ? C18 C19 1.501(13) . ? C19 C20 1.431(19) . ? C19 C21 1.483(17) . ? C19 C22 1.579(18) . ? C23 C24 1.447(18) . ? C23 C28 1.507(15) . ? C24 C25 1.509(17) . ? C25 C26 1.491(19) . ? C26 C27 1.51(2) . ? C27 C28 1.521(17) . ? C29 C34 1.446(16) . ? C29 C30 1.546(19) . ? C30 C31 1.559(18) . ? C31 C32 1.42(2) . ? C32 C33 1.32(2) . ? C33 C34 1.473(18) . ? C35 C36 1.536(15) . ? C36 C39 1.482(16) . ? C36 C38 1.488(15) . ? C36 C37 1.500(16) . ? C40 C41 1.467(16) . ? C40 C45 1.497(17) . ? C41 C42 1.539(17) . ? C42 C43 1.53(2) . ? C43 C44 1.452(19) . ? C44 C45 1.524(18) . ? C46 C51 1.387(16) . ? C46 C47 1.552(17) . ? C47 C48 1.527(18) . ? C48 C49 1.44(2) . ? C49 C50 1.44(2) . ? C50 C51 1.554(18) . ? C52 N7 1.144(14) . ? C52 C54 1.573(14) . ? C52 C53 1.61(2) . ? O1 C58 1.348(15) . ? O1 C55 1.415(17) . ? C55 C56 1.442(19) . ? C56 C57 1.328(16) . ? C57 C58 1.320(16) . ? O2 C62 1.361(17) . ? O2 C59 1.42(2) . ? C59 C60 1.45(2) . ? C60 C61 1.338(19) . ? C61 C62 1.328(19) . ? O3 C66 1.361(19) . ? O3 C63 1.41(2) . ? C63 C64 1.45(2) . ? C64 C65 1.339(19) . ? C65 C66 1.32(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ga1 N2 66.6(3) . . ? N1 Ga1 Ga2 125.0(2) . . ? N2 Ga1 Ga2 129.3(2) . . ? N1 Ga1 C1 33.6(3) . . ? N2 Ga1 C1 33.0(3) . . ? Ga2 Ga1 C1 135.5(2) . . ? N1 Ga1 I1 107.1(2) . . ? N2 Ga1 I1 109.0(2) . . ? Ga2 Ga1 I1 111.73(6) . . ? C1 Ga1 I1 112.6(2) . . ? N3 Ga2 N4 65.9(3) . . ? N3 Ga2 Ga1 112.7(3) . . ? N4 Ga2 Ga1 112.4(2) . . ? N3 Ga2 Ga3 112.5(3) . . ? N4 Ga2 Ga3 114.5(2) . . ? Ga1 Ga2 Ga3 124.45(6) . . ? N3 Ga2 C18 33.5(3) . . ? N4 Ga2 C18 32.5(3) . . ? Ga1 Ga2 C18 118.1(2) . . ? Ga3 Ga2 C18 117.4(2) . . ? N5 Ga3 N6 68.2(3) . . ? N5 Ga3 N7 109.1(4) . . ? N6 Ga3 N7 109.7(4) . . ? N5 Ga3 Ga2 125.2(2) . . ? N6 Ga3 Ga2 122.9(2) . . ? N7 Ga3 Ga2 113.7(3) . . ? N5 Ga3 C35 34.6(3) . . ? N6 Ga3 C35 33.7(3) . . ? N7 Ga3 C35 115.0(4) . . ? Ga2 Ga3 C35 131.2(2) . . ? C1 N1 C6 132.9(9) . . ? C1 N1 Ga1 94.4(6) . . ? C6 N1 Ga1 132.6(7) . . ? C1 N2 C12 131.2(9) . . ? C1 N2 Ga1 93.2(6) . . ? C12 N2 Ga1 135.6(7) . . ? C18 N3 C23 131.4(8) . . ? C18 N3 Ga2 94.5(6) . . ? C23 N3 Ga2 134.0(7) . . ? C18 N4 C29 133.2(8) . . ? C18 N4 Ga2 94.5(5) . . ? C29 N4 Ga2 132.2(6) . . ? C35 N5 C40 127.4(9) . . ? C35 N5 Ga3 93.0(6) . . ? C40 N5 Ga3 138.5(7) . . ? C35 N6 C46 132.4(9) . . ? C35 N6 Ga3 92.9(7) . . ? C46 N6 Ga3 134.7(7) . . ? N2 C1 N1 105.8(9) . . ? N2 C1 C2 123.8(9) . . ? N1 C1 C2 130.3(10) . . ? N2 C1 Ga1 53.8(5) . . ? N1 C1 Ga1 52.1(5) . . ? C2 C1 Ga1 175.9(7) . . ? C1 C2 C3 113.1(10) . . ? C1 C2 C5 112.9(9) . . ? C3 C2 C5 109.6(10) . . ? C1 C2 C4 107.3(9) . . ? C3 C2 C4 109.7(9) . . ? C5 C2 C4 103.7(10) . . ? N1 C6 C11 106.3(9) . . ? N1 C6 C7 109.4(9) . . ? C11 C6 C7 109.6(9) . . ? C8 C7 C6 112.1(10) . . ? C7 C8 C9 110.3(11) . . ? C10 C9 C8 113.3(10) . . ? C9 C10 C11 110.3(9) . . ? C6 C11 C10 111.0(9) . . ? N2 C12 C13 108.7(8) . . ? N2 C12 C17 111.5(9) . . ? C13 C12 C17 108.4(9) . . ? C12 C13 C14 111.1(8) . . ? C15 C14 C13 113.0(10) . . ? C16 C15 C14 106.4(10) . . ? C17 C16 C15 113.0(10) . . ? C16 C17 C12 113.0(9) . . ? N4 C18 N3 105.0(7) . . ? N4 C18 C19 128.6(8) . . ? N3 C18 C19 125.9(9) . . ? N4 C18 Ga2 53.0(4) . . ? N3 C18 Ga2 52.0(4) . . ? C19 C18 Ga2 175.3(8) . . ? C20 C19 C21 118.9(12) . . ? C20 C19 C18 108.6(10) . . ? C21 C19 C18 115.9(9) . . ? C20 C19 C22 104.2(12) . . ? C21 C19 C22 100.0(10) . . ? C18 C19 C22 107.5(10) . . ? C24 C23 N3 110.5(9) . . ? C24 C23 C28 111.3(12) . . ? N3 C23 C28 105.6(9) . . ? C23 C24 C25 111.3(11) . . ? C26 C25 C24 108.1(12) . . ? C25 C26 C27 110.6(12) . . ? C26 C27 C28 111.3(12) . . ? C23 C28 C27 108.9(10) . . ? N4 C29 C34 113.2(9) . . ? N4 C29 C30 112.1(10) . . ? C34 C29 C30 103.2(12) . . ? C29 C30 C31 115.0(15) . . ? C32 C31 C30 107.5(14) . . ? C33 C32 C31 115.7(14) . . ? C32 C33 C34 123.7(19) . . ? C29 C34 C33 115.4(12) . . ? N6 C35 N5 105.8(9) . . ? N6 C35 C36 122.6(10) . . ? N5 C35 C36 131.4(8) . . ? N6 C35 Ga3 53.5(5) . . ? N5 C35 Ga3 52.4(5) . . ? C36 C35 Ga3 176.0(8) . . ? C39 C36 C38 105.3(11) . . ? C39 C36 C37 110.5(11) . . ? C38 C36 C37 104.3(10) . . ? C39 C36 C35 113.6(9) . . ? C38 C36 C35 117.0(10) . . ? C37 C36 C35 105.8(9) . . ? N5 C40 C41 113.6(10) . . ? N5 C40 C45 107.3(9) . . ? C41 C40 C45 105.3(10) . . ? C40 C41 C42 115.2(11) . . ? C43 C42 C41 105.5(11) . . ? C44 C43 C42 113.5(12) . . ? C43 C44 C45 111.8(12) . . ? C40 C45 C44 111.0(11) . . ? C51 C46 N6 113.5(10) . . ? C51 C46 C47 109.5(10) . . ? N6 C46 C47 107.0(9) . . ? C48 C47 C46 105.3(11) . . ? C49 C48 C47 114.4(13) . . ? C50 C49 C48 105.4(12) . . ? C49 C50 C51 109.8(12) . . ? C46 C51 C50 114.1(12) . . ? N7 C52 C54 119.4(13) . . ? N7 C52 C53 121.6(12) . . ? C54 C52 C53 118.6(12) . . ? C58 O1 C55 110.1(12) . . ? O1 C55 C56 99.5(11) . . ? C57 C56 C55 112.1(13) . . ? C58 C57 C56 107.0(12) . . ? C57 C58 O1 109.8(10) . . ? C62 O2 C59 107.8(14) . . ? O2 C59 C60 93.3(12) . . ? C61 C60 C59 105.9(16) . . ? C62 C61 C60 102.5(16) . . ? C61 C62 O2 108.1(14) . . ? C66 O3 C63 110.9(15) . . ? O3 C63 C64 94.4(14) . . ? C65 C64 C63 107.7(17) . . ? C66 C65 C64 100.4(17) . . ? C65 C66 O3 106.5(15) . . ? C52 N7 Ga3 133.9(10) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 24.26 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.612 _refine_diff_density_min -0.845 _refine_diff_density_rms 0.115 _exptl_crystal_recrystallization_method 'from tetrahydrofurane' # Attachment '- 5 - tze83a.CIF' data_5 _database_code_depnum_ccdc_archive 'CCDC 811981' _audit_creation_method SHELXL-97 _chemical_name_systematic ; N,N'-dicyclohexylneopentylamidinato-ethyl-gallium(II)-N,N' -dicyclohexylneopentylamidinato-hydrido-gallium(II)-N,N' -dicyclohexylneopentylamidinato-gallium(I) ; _chemical_name_common ; N,N'-dicyclohexylneopentylamidinato-ethyl-gallium(ii)-N,N' - dicyclohexylneopentylamidinato-hydrido-gallium(ii)-N,N' - dicyclohexylneopentylamidinato-gallium(i) ; _chemical_melting_point ? _chemical_formula_moiety 'C53 H99 Ga3 N6' _chemical_formula_sum 'C53 H99 Ga3 N6' _chemical_formula_weight 1029.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.634(3) _cell_length_b 20.821(4) _cell_length_c 21.296(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.57(3) _cell_angle_gamma 90.00 _cell_volume 5601.7(19) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 54866 _cell_measurement_theta_min 5.0 _cell_measurement_theta_max 56.3 _exptl_crystal_description column _exptl_crystal_colour colourless _exptl_crystal_size_max 0.274 _exptl_crystal_size_mid 0.257 _exptl_crystal_size_min 0.163 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 1.470 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.7026 _exptl_absorpt_correction_T_max 0.8234 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54075 _diffrn_reflns_av_R_equivalents 0.1777 _diffrn_reflns_av_sigmaI/netI 0.2135 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 28.17 _reflns_number_total 13382 _reflns_number_gt 4061 _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^)+(0.0491P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13382 _refine_ls_number_parameters 563 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1995 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.1617 _refine_ls_wR_factor_gt 0.1179 _refine_ls_goodness_of_fit_ref 0.780 _refine_ls_restrained_S_all 0.780 _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 0.28002(6) 0.63217(4) 0.20111(4) 0.0496(2) Uani 1 1 d . . . H1 H 0.328(4) 0.693(3) 0.172(3) 0.037(17) Uiso 1 1 d . . . Ga2 Ga 0.24726(5) 0.62526(5) 0.31442(3) 0.0470(2) Uani 1 1 d . . . Ga3 Ga 0.39422(5) 0.62590(5) 0.39132(3) 0.0473(2) Uani 1 1 d . . . N1 N 0.1824(5) 0.5947(3) 0.1357(3) 0.0631(18) Uani 1 1 d . . . N2 N 0.3344(4) 0.5519(3) 0.1589(3) 0.0510(15) Uani 1 1 d . . . N3 N 0.1160(5) 0.6741(3) 0.3408(3) 0.0567(17) Uani 1 1 d . . . N4 N 0.1243(5) 0.5700(3) 0.3401(3) 0.0525(16) Uani 1 1 d . . . N5 N 0.4792(5) 0.7084(3) 0.3904(3) 0.0563(17) Uani 1 1 d . . . N6 N 0.3798(4) 0.6807(3) 0.4682(3) 0.0524(15) Uani 1 1 d . . . C1 C 0.2472(6) 0.5450(3) 0.1232(4) 0.0512(18) Uani 1 1 d . . . C2 C 0.2270(6) 0.4887(4) 0.0780(4) 0.060(2) Uani 1 1 d . . . C3 C 0.1199(9) 0.4871(5) 0.0442(5) 0.112(4) Uani 1 1 d . . . H3A H 0.1119 0.5258 0.0184 0.168 Uiso 1 1 calc R . . H3B H 0.0632 0.4856 0.0753 0.168 Uiso 1 1 calc R . . H3C H 0.1159 0.4490 0.0173 0.168 Uiso 1 1 calc R . . C4 C 0.2304(7) 0.4255(4) 0.1173(5) 0.075(2) Uani 1 1 d . . . H4A H 0.1743 0.4264 0.1487 0.113 Uiso 1 1 calc R . . H4B H 0.2994 0.4217 0.1385 0.113 Uiso 1 1 calc R . . H4C H 0.2198 0.3886 0.0893 0.113 Uiso 1 1 calc R . . C5 C 0.3136(8) 0.4879(5) 0.0280(5) 0.089(3) Uani 1 1 d . . . H5A H 0.3101 0.5276 0.0034 0.133 Uiso 1 1 calc R . . H5B H 0.3028 0.4510 0.0001 0.133 Uiso 1 1 calc R . . H5C H 0.3832 0.4845 0.0485 0.133 Uiso 1 1 calc R . . C6 C 0.0780(5) 0.6140(4) 0.1141(4) 0.0491(18) Uani 1 1 d . . . H6A H 0.0614 0.5922 0.0733 0.059 Uiso 1 1 calc R . . C7 C 0.0769(7) 0.6843(5) 0.1048(6) 0.091(3) Uani 1 1 d . . . H7A H 0.1297 0.6960 0.0728 0.109 Uiso 1 1 calc R . . H7B H 0.0973 0.7057 0.1446 0.109 Uiso 1 1 calc R . . C8 C -0.0345(9) 0.7086(6) 0.0833(8) 0.128(5) Uani 1 1 d . . . H8A H -0.0343 0.7559 0.0789 0.154 Uiso 1 1 calc R . . H8B H -0.0544 0.6894 0.0424 0.154 Uiso 1 1 calc R . . C9 C -0.1108(8) 0.6887(6) 0.1325(7) 0.109(5) Uani 1 1 d . . . H9A H -0.0908 0.7089 0.1729 0.131 Uiso 1 1 calc R . . H9B H -0.1826 0.7038 0.1207 0.131 Uiso 1 1 calc R . . C10 C -0.1121(7) 0.6198(9) 0.1398(5) 0.124(5) Uani 1 1 d . . . H10A H -0.1331 0.5993 0.0997 0.149 Uiso 1 1 calc R . . H10B H -0.1644 0.6076 0.1721 0.149 Uiso 1 1 calc R . . C11 C -0.0001(6) 0.5962(6) 0.1601(5) 0.094(3) Uani 1 1 d . . . H11A H 0.0192 0.6152 0.2012 0.113 Uiso 1 1 calc R . . H11B H -0.0009 0.5489 0.1649 0.113 Uiso 1 1 calc R . . C12 C 0.4317(5) 0.5162(4) 0.1633(4) 0.0529(19) Uani 1 1 d . . . H12A H 0.4233 0.4759 0.1382 0.063 Uiso 1 1 calc R . . C13 C 0.5235(6) 0.5537(5) 0.1371(4) 0.070(2) Uani 1 1 d . . . H13A H 0.5249 0.5968 0.1567 0.085 Uiso 1 1 calc R . . H13B H 0.5120 0.5596 0.0914 0.085 Uiso 1 1 calc R . . C14 C 0.6308(6) 0.5215(5) 0.1478(5) 0.087(3) Uani 1 1 d . . . H14A H 0.6339 0.4813 0.1230 0.104 Uiso 1 1 calc R . . H14B H 0.6875 0.5503 0.1328 0.104 Uiso 1 1 calc R . . C15 C 0.6498(7) 0.5062(5) 0.2170(5) 0.084(3) Uani 1 1 d . . . H15A H 0.7176 0.4828 0.2223 0.101 Uiso 1 1 calc R . . H15B H 0.6542 0.5465 0.2416 0.101 Uiso 1 1 calc R . . C16 C 0.5595(8) 0.4653(5) 0.2405(5) 0.086(3) Uani 1 1 d . . . H16A H 0.5702 0.4568 0.2859 0.103 Uiso 1 1 calc R . . H16B H 0.5599 0.4236 0.2183 0.103 Uiso 1 1 calc R . . C17 C 0.4524(6) 0.4977(4) 0.2304(4) 0.065(2) Uani 1 1 d . . . H17A H 0.3959 0.4682 0.2443 0.077 Uiso 1 1 calc R . . H17B H 0.4491 0.5367 0.2569 0.077 Uiso 1 1 calc R . . C18 C 0.0614(5) 0.6203(4) 0.3535(3) 0.0534(18) Uani 1 1 d . . . C19 C -0.0524(5) 0.6132(4) 0.3777(4) 0.066(2) Uani 1 1 d . . . C20 C -0.1093(8) 0.6763(5) 0.3890(8) 0.137(6) Uani 1 1 d . . . H20A H -0.1809 0.6677 0.4042 0.205 Uiso 1 1 calc R . . H20B H -0.1135 0.7006 0.3497 0.205 Uiso 1 1 calc R . . H20C H -0.0701 0.7014 0.4205 0.205 Uiso 1 1 calc R . . C21 C -0.1186(6) 0.5760(4) 0.3305(5) 0.077(3) Uani 1 1 d . . . H21A H -0.0862 0.5339 0.3231 0.116 Uiso 1 1 calc R . . H21B H -0.1223 0.5999 0.2909 0.116 Uiso 1 1 calc R . . H21C H -0.1902 0.5701 0.3468 0.116 Uiso 1 1 calc R . . C22 C -0.0504(7) 0.5776(6) 0.4405(4) 0.093(3) Uani 1 1 d . . . H22A H -0.0128 0.5368 0.4357 0.139 Uiso 1 1 calc R . . H22B H -0.1231 0.5693 0.4539 0.139 Uiso 1 1 calc R . . H22C H -0.0141 0.6040 0.4721 0.139 Uiso 1 1 calc R . . C23 C 0.0923(6) 0.7432(4) 0.3471(4) 0.059(2) Uani 1 1 d . . . H23A H 0.0149 0.7511 0.3407 0.071 Uiso 1 1 calc R . . C24 C 0.1550(12) 0.7813(5) 0.3011(7) 0.147(7) Uani 1 1 d . . . H24A H 0.1379 0.7665 0.2580 0.176 Uiso 1 1 calc R . . H24B H 0.2314 0.7737 0.3088 0.176 Uiso 1 1 calc R . . C25 C 0.1316(10) 0.8568(5) 0.3060(6) 0.099(4) Uani 1 1 d . . . H25A H 0.1719 0.8813 0.2743 0.119 Uiso 1 1 calc R . . H25B H 0.0552 0.8661 0.3007 0.119 Uiso 1 1 calc R . . C26 C 0.1675(11) 0.8715(8) 0.3685(6) 0.137(5) Uani 1 1 d . . . H26A H 0.1638 0.9186 0.3746 0.164 Uiso 1 1 calc R . . H26B H 0.2428 0.8587 0.3725 0.164 Uiso 1 1 calc R . . C27 C 0.1091(13) 0.8408(6) 0.4176(7) 0.136(5) Uani 1 1 d . . . H27A H 0.0327 0.8511 0.4138 0.164 Uiso 1 1 calc R . . H27B H 0.1350 0.8551 0.4594 0.164 Uiso 1 1 calc R . . C28 C 0.1277(12) 0.7687(6) 0.4090(6) 0.122(5) Uani 1 1 d . . . H28A H 0.2043 0.7598 0.4144 0.147 Uiso 1 1 calc R . . H28B H 0.0900 0.7453 0.4425 0.147 Uiso 1 1 calc R . . C29 C 0.1130(6) 0.5007(4) 0.3492(4) 0.055(2) Uani 1 1 d . . . H29A H 0.0392 0.4910 0.3629 0.066 Uiso 1 1 calc R . . C30 C 0.1339(9) 0.4673(4) 0.2875(5) 0.088(3) Uani 1 1 d . . . H30A H 0.2044 0.4801 0.2719 0.106 Uiso 1 1 calc R . . H30B H 0.0802 0.4808 0.2560 0.106 Uiso 1 1 calc R . . C31 C 0.1300(12) 0.3938(6) 0.2954(6) 0.124(5) Uani 1 1 d . . . H31A H 0.0581 0.3805 0.3081 0.149 Uiso 1 1 calc R . . H31B H 0.1460 0.3727 0.2549 0.149 Uiso 1 1 calc R . . C32 C 0.2094(9) 0.3730(6) 0.3444(7) 0.122(5) Uani 1 1 d . . . H32A H 0.2062 0.3258 0.3496 0.147 Uiso 1 1 calc R . . H32B H 0.2815 0.3845 0.3307 0.147 Uiso 1 1 calc R . . C33 C 0.1868(7) 0.4048(5) 0.4058(5) 0.083(3) Uani 1 1 d . . . H33A H 0.2403 0.3915 0.4375 0.100 Uiso 1 1 calc R . . H33B H 0.1162 0.3914 0.4208 0.100 Uiso 1 1 calc R . . C34 C 0.1893(7) 0.4779(5) 0.3981(5) 0.081(3) Uani 1 1 d . . . H34A H 0.1723 0.4984 0.4387 0.098 Uiso 1 1 calc R . . H34B H 0.2617 0.4914 0.3864 0.098 Uiso 1 1 calc R . . C35 C 0.4452(6) 0.7266(4) 0.4470(4) 0.057(2) Uani 1 1 d . . . C36 C 0.4766(8) 0.7893(5) 0.4812(4) 0.083(3) Uani 1 1 d . . . C37 C 0.5815(11) 0.7791(8) 0.5081(11) 0.250(14) Uani 1 1 d . . . H37A H 0.5802 0.7415 0.5359 0.375 Uiso 1 1 calc R . . H37B H 0.6029 0.8171 0.5322 0.375 Uiso 1 1 calc R . . H37C H 0.6321 0.7716 0.4742 0.375 Uiso 1 1 calc R . . C38 C 0.4789(11) 0.8494(5) 0.4359(6) 0.130(5) Uani 1 1 d . . . H38A H 0.4978 0.8879 0.4599 0.196 Uiso 1 1 calc R . . H38B H 0.4089 0.8552 0.4164 0.196 Uiso 1 1 calc R . . H38C H 0.5316 0.8423 0.4031 0.196 Uiso 1 1 calc R . . C39 C 0.3972(11) 0.8134(5) 0.5257(7) 0.124(5) Uani 1 1 d . . . H39A H 0.3854 0.7812 0.5584 0.186 Uiso 1 1 calc R . . H39B H 0.3305 0.8217 0.5032 0.186 Uiso 1 1 calc R . . H39C H 0.4228 0.8532 0.5450 0.186 Uiso 1 1 calc R . . C40 C 0.5456(5) 0.7366(4) 0.3430(4) 0.053(2) Uani 1 1 d . . . H40A H 0.5991 0.7654 0.3635 0.064 Uiso 1 1 calc R . . C41 C 0.4834(6) 0.7738(4) 0.2951(4) 0.062(2) Uani 1 1 d . . . H41A H 0.4494 0.8109 0.3159 0.074 Uiso 1 1 calc R . . H41B H 0.4266 0.7461 0.2778 0.074 Uiso 1 1 calc R . . C42 C 0.5514(7) 0.7986(4) 0.2408(4) 0.066(2) Uani 1 1 d . . . H42A H 0.5057 0.8214 0.2100 0.079 Uiso 1 1 calc R . . H42B H 0.6044 0.8294 0.2572 0.079 Uiso 1 1 calc R . . C43 C 0.6067(8) 0.7447(4) 0.2087(5) 0.081(3) Uani 1 1 d . . . H43A H 0.5539 0.7165 0.1879 0.097 Uiso 1 1 calc R . . H43B H 0.6539 0.7621 0.1761 0.097 Uiso 1 1 calc R . . C44 C 0.6690(9) 0.7071(6) 0.2539(6) 0.118(5) Uani 1 1 d . . . H44A H 0.7275 0.7340 0.2707 0.142 Uiso 1 1 calc R . . H44B H 0.7007 0.6698 0.2322 0.142 Uiso 1 1 calc R . . C45 C 0.6019(7) 0.6832(5) 0.3083(6) 0.097(4) Uani 1 1 d . . . H45A H 0.5485 0.6526 0.2919 0.116 Uiso 1 1 calc R . . H45B H 0.6480 0.6597 0.3384 0.116 Uiso 1 1 calc R . . C46 C 0.3193(6) 0.6742(4) 0.5265(4) 0.056(2) Uani 1 1 d . . . H46A H 0.2927 0.7177 0.5384 0.067 Uiso 1 1 calc R . . C47 C 0.2282(6) 0.6338(7) 0.5128(4) 0.103(4) Uani 1 1 d . . . H47A H 0.2535 0.5921 0.4963 0.123 Uiso 1 1 calc R . . H47B H 0.1853 0.6545 0.4793 0.123 Uiso 1 1 calc R . . C48 C 0.1560(6) 0.6209(9) 0.5705(5) 0.129(5) Uani 1 1 d . . . H48A H 0.1196 0.6610 0.5827 0.154 Uiso 1 1 calc R . . H48B H 0.1014 0.5886 0.5593 0.154 Uiso 1 1 calc R . . C49 C 0.2205(11) 0.5971(5) 0.6238(5) 0.107(4) Uani 1 1 d . . . H49A H 0.2517 0.5549 0.6129 0.128 Uiso 1 1 calc R . . H49B H 0.1752 0.5911 0.6609 0.128 Uiso 1 1 calc R . . C50 C 0.3074(9) 0.6440(8) 0.6389(5) 0.134(6) Uani 1 1 d . . . H50A H 0.3505 0.6286 0.6750 0.161 Uiso 1 1 calc R . . H50B H 0.2774 0.6865 0.6496 0.161 Uiso 1 1 calc R . . C51 C 0.3762(8) 0.6488(9) 0.5789(6) 0.159(8) Uani 1 1 d . . . H51A H 0.4382 0.6765 0.5878 0.191 Uiso 1 1 calc R . . H51B H 0.4027 0.6054 0.5681 0.191 Uiso 1 1 calc R . . C52 C 0.4942(6) 0.5546(4) 0.4103(4) 0.070(2) Uani 1 1 d . . . H52A H 0.4538 0.5187 0.4290 0.084 Uiso 1 1 calc R . . H52B H 0.5239 0.5389 0.3702 0.084 Uiso 1 1 calc R . . C53 C 0.5858(7) 0.5716(5) 0.4545(5) 0.084(3) Uani 1 1 d . . . H53A H 0.6309 0.5338 0.4608 0.125 Uiso 1 1 calc R . . H53B H 0.5578 0.5856 0.4950 0.125 Uiso 1 1 calc R . . H53C H 0.6276 0.6064 0.4362 0.125 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 0.0601(4) 0.0508(5) 0.0379(5) -0.0045(4) 0.0036(3) -0.0023(4) Ga2 0.0423(3) 0.0602(5) 0.0386(5) -0.0053(5) 0.0050(3) -0.0050(4) Ga3 0.0449(4) 0.0593(5) 0.0378(5) 0.0005(5) 0.0039(3) -0.0082(4) N1 0.079(4) 0.058(4) 0.052(5) -0.013(3) -0.011(3) 0.013(3) N2 0.054(3) 0.067(4) 0.032(4) -0.006(3) -0.002(3) 0.003(3) N3 0.051(3) 0.065(4) 0.055(5) -0.016(3) 0.008(3) -0.007(3) N4 0.049(3) 0.056(4) 0.053(4) -0.011(3) 0.010(3) -0.004(3) N5 0.056(3) 0.074(5) 0.039(4) 0.002(3) 0.011(3) -0.016(3) N6 0.055(3) 0.063(4) 0.040(4) 0.013(3) 0.002(3) -0.022(3) C1 0.072(5) 0.043(4) 0.038(5) -0.003(3) -0.002(3) 0.014(3) C2 0.081(5) 0.051(5) 0.046(5) -0.015(4) -0.008(4) 0.006(4) C3 0.144(10) 0.091(8) 0.100(10) -0.050(7) -0.063(7) 0.047(7) C4 0.101(6) 0.054(5) 0.070(7) -0.009(5) 0.002(5) -0.007(5) C5 0.142(9) 0.071(6) 0.054(7) -0.018(5) 0.011(6) 0.005(6) C6 0.057(4) 0.049(5) 0.042(4) -0.002(3) -0.005(3) 0.004(3) C7 0.066(5) 0.090(7) 0.116(10) 0.030(7) 0.001(5) 0.014(5) C8 0.103(8) 0.091(8) 0.191(16) 0.064(9) 0.017(9) 0.008(7) C9 0.066(6) 0.101(9) 0.162(14) -0.039(8) 0.022(7) 0.011(6) C10 0.061(5) 0.225(17) 0.085(8) -0.008(11) 0.014(5) -0.008(9) C11 0.062(5) 0.133(9) 0.088(8) 0.021(7) 0.000(5) -0.012(5) C12 0.051(4) 0.063(5) 0.045(5) -0.005(4) 0.009(3) 0.001(3) C13 0.065(5) 0.091(7) 0.056(6) 0.017(5) 0.007(4) -0.004(4) C14 0.059(5) 0.107(8) 0.096(9) 0.002(6) 0.015(5) -0.003(5) C15 0.066(5) 0.087(7) 0.100(9) -0.026(6) -0.018(5) 0.007(5) C16 0.096(7) 0.090(7) 0.071(8) -0.001(6) -0.009(5) 0.023(6) C17 0.077(5) 0.066(5) 0.051(6) 0.009(4) 0.002(4) 0.016(4) C18 0.046(3) 0.062(5) 0.053(5) -0.010(4) 0.005(3) -0.003(4) C19 0.049(4) 0.078(7) 0.071(6) -0.012(5) 0.011(4) -0.006(4) C20 0.087(7) 0.081(7) 0.244(18) -0.029(10) 0.080(9) -0.008(6) C21 0.041(4) 0.086(7) 0.104(8) 0.005(6) -0.004(4) -0.005(4) C22 0.067(5) 0.155(10) 0.057(6) -0.020(6) 0.027(4) -0.034(6) C23 0.052(4) 0.066(5) 0.061(6) -0.018(4) 0.007(4) -0.008(4) C24 0.206(14) 0.075(8) 0.161(15) -0.036(8) 0.104(12) -0.037(9) C25 0.149(10) 0.072(8) 0.078(9) 0.013(6) 0.012(7) -0.013(6) C26 0.154(11) 0.166(13) 0.089(10) -0.001(11) 0.010(8) -0.065(11) C27 0.225(16) 0.086(9) 0.098(11) -0.022(8) -0.018(11) 0.050(9) C28 0.195(13) 0.086(8) 0.086(10) -0.017(7) -0.042(9) 0.019(8) C29 0.049(4) 0.060(5) 0.055(6) -0.001(4) 0.009(3) -0.002(3) C30 0.147(9) 0.064(6) 0.055(7) -0.001(5) 0.022(6) -0.013(6) C31 0.199(14) 0.075(9) 0.101(11) -0.008(7) 0.061(10) 0.007(8) C32 0.130(9) 0.064(6) 0.174(13) 0.027(9) 0.098(9) 0.030(7) C33 0.070(5) 0.083(7) 0.098(8) 0.019(6) 0.007(5) 0.005(5) C34 0.065(5) 0.079(7) 0.100(9) 0.008(6) -0.022(5) -0.011(4) C35 0.065(4) 0.066(5) 0.041(5) -0.005(4) 0.000(3) -0.027(4) C36 0.117(7) 0.099(7) 0.034(5) -0.011(5) 0.003(5) -0.067(6) C37 0.156(13) 0.184(16) 0.41(3) -0.191(19) -0.180(17) 0.051(11) C38 0.216(14) 0.082(8) 0.094(10) -0.016(6) 0.039(9) -0.062(8) C39 0.164(12) 0.074(8) 0.135(13) -0.024(8) 0.022(10) -0.043(8) C40 0.045(4) 0.069(5) 0.045(5) 0.004(4) 0.004(3) -0.019(3) C41 0.071(5) 0.055(5) 0.058(6) 0.009(4) 0.014(4) 0.001(4) C42 0.074(5) 0.065(5) 0.059(6) 0.018(4) 0.016(4) 0.001(4) C43 0.107(7) 0.067(6) 0.069(7) 0.007(5) 0.042(6) -0.007(5) C44 0.102(7) 0.112(9) 0.143(12) 0.053(8) 0.081(8) 0.037(7) C45 0.079(6) 0.096(7) 0.117(9) 0.038(7) 0.058(6) 0.028(5) C46 0.074(5) 0.052(5) 0.043(5) -0.003(4) 0.018(4) -0.019(4) C47 0.056(4) 0.204(12) 0.049(6) 0.010(8) -0.001(4) -0.034(7) C48 0.051(4) 0.268(16) 0.067(7) -0.015(10) 0.026(4) -0.045(8) C49 0.207(13) 0.062(6) 0.052(7) 0.007(5) 0.033(8) -0.032(7) C50 0.123(9) 0.220(17) 0.060(8) 0.034(9) -0.001(6) -0.036(10) C51 0.080(7) 0.31(2) 0.083(9) 0.090(12) -0.002(6) -0.026(10) C52 0.071(5) 0.077(6) 0.061(6) -0.005(5) -0.003(4) -0.001(4) C53 0.075(6) 0.103(8) 0.073(7) 0.024(6) -0.012(5) -0.007(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 H1 1.54(6) . ? Ga1 N1 2.009(7) . ? Ga1 N2 2.021(6) . ? Ga1 Ga2 2.4567(12) . ? Ga1 C1 2.491(7) . ? Ga2 N4 2.013(6) . ? Ga2 N3 2.029(6) . ? Ga2 Ga3 2.4633(13) . ? Ga2 C18 2.501(6) . ? Ga3 C52 1.988(9) . ? Ga3 N6 2.006(7) . ? Ga3 N5 2.026(6) . ? Ga3 C35 2.490(8) . ? N1 C1 1.346(9) . ? N1 C6 1.449(9) . ? N2 C1 1.339(9) . ? N2 C12 1.439(9) . ? N3 C18 1.344(10) . ? N3 C23 1.476(10) . ? N4 C18 1.346(9) . ? N4 C29 1.463(10) . ? N5 C35 1.337(9) . ? N5 C40 1.444(9) . ? N6 C35 1.344(8) . ? N6 C46 1.471(8) . ? C1 C2 1.537(10) . ? C2 C3 1.527(12) . ? C2 C5 1.535(11) . ? C2 C4 1.559(12) . ? C6 C11 1.446(11) . ? C6 C7 1.476(12) . ? C7 C8 1.561(14) . ? C8 C9 1.488(16) . ? C9 C10 1.442(18) . ? C10 C11 1.556(14) . ? C12 C17 1.500(11) . ? C12 C13 1.511(10) . ? C13 C14 1.527(12) . ? C14 C15 1.525(14) . ? C15 C16 1.512(13) . ? C16 C17 1.526(11) . ? C18 C19 1.540(9) . ? C19 C21 1.515(12) . ? C19 C20 1.518(13) . ? C19 C22 1.527(13) . ? C23 C28 1.487(14) . ? C23 C24 1.494(13) . ? C24 C25 1.603(15) . ? C25 C26 1.435(16) . ? C26 C27 1.437(16) . ? C27 C28 1.532(15) . ? C29 C34 1.490(12) . ? C29 C30 1.513(12) . ? C30 C31 1.541(14) . ? C31 C32 1.504(18) . ? C32 C33 1.495(16) . ? C33 C34 1.531(13) . ? C35 C36 1.546(11) . ? C36 C37 1.454(16) . ? C36 C39 1.474(14) . ? C36 C38 1.582(15) . ? C40 C41 1.499(11) . ? C40 C45 1.515(12) . ? C41 C42 1.536(10) . ? C42 C43 1.490(11) . ? C43 C44 1.464(15) . ? C44 C45 1.526(12) . ? C46 C51 1.423(13) . ? C46 C47 1.452(12) . ? C47 C48 1.563(11) . ? C48 C49 1.476(16) . ? C49 C50 1.503(16) . ? C50 C51 1.556(14) . ? C52 C53 1.528(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 H1 Ga1 N1 107(2) . . ? H1 Ga1 N2 112(2) . . ? N1 Ga1 N2 65.1(2) . . ? H1 Ga1 Ga2 121(2) . . ? N1 Ga1 Ga2 123.4(2) . . ? N2 Ga1 Ga2 116.75(18) . . ? H1 Ga1 C1 114(2) . . ? N1 Ga1 C1 32.6(2) . . ? N2 Ga1 C1 32.5(2) . . ? Ga2 Ga1 C1 125.68(18) . . ? N4 Ga2 N3 64.9(2) . . ? N4 Ga2 Ga1 116.0(2) . . ? N3 Ga2 Ga1 112.9(2) . . ? N4 Ga2 Ga3 113.7(2) . . ? N3 Ga2 Ga3 115.2(2) . . ? Ga1 Ga2 Ga3 121.29(4) . . ? N4 Ga2 C18 32.5(3) . . ? N3 Ga2 C18 32.4(3) . . ? Ga1 Ga2 C18 119.80(17) . . ? Ga3 Ga2 C18 118.89(17) . . ? C52 Ga3 N6 108.8(3) . . ? C52 Ga3 N5 107.4(3) . . ? N6 Ga3 N5 65.0(2) . . ? C52 Ga3 Ga2 127.1(3) . . ? N6 Ga3 Ga2 118.15(18) . . ? N5 Ga3 Ga2 113.2(2) . . ? C52 Ga3 C35 111.8(3) . . ? N6 Ga3 C35 32.6(2) . . ? N5 Ga3 C35 32.4(2) . . ? Ga2 Ga3 C35 120.7(2) . . ? C1 N1 C6 134.7(7) . . ? C1 N1 Ga1 93.7(5) . . ? C6 N1 Ga1 131.5(5) . . ? C1 N2 C12 132.8(6) . . ? C1 N2 Ga1 93.4(4) . . ? C12 N2 Ga1 133.8(5) . . ? C18 N3 C23 133.6(6) . . ? C18 N3 Ga2 93.5(5) . . ? C23 N3 Ga2 132.8(5) . . ? C18 N4 C29 132.8(6) . . ? C18 N4 Ga2 94.1(5) . . ? C29 N4 Ga2 132.5(5) . . ? C35 N5 C40 135.1(7) . . ? C35 N5 Ga3 93.2(4) . . ? C40 N5 Ga3 131.5(5) . . ? C35 N6 C46 132.5(7) . . ? C35 N6 Ga3 93.9(5) . . ? C46 N6 Ga3 133.5(5) . . ? N2 C1 N1 107.7(6) . . ? N2 C1 C2 124.5(6) . . ? N1 C1 C2 127.8(7) . . ? N2 C1 Ga1 54.1(4) . . ? N1 C1 Ga1 53.6(4) . . ? C2 C1 Ga1 176.9(6) . . ? C3 C2 C5 107.8(8) . . ? C3 C2 C1 116.8(7) . . ? C5 C2 C1 109.1(7) . . ? C3 C2 C4 104.7(8) . . ? C5 C2 C4 110.3(7) . . ? C1 C2 C4 107.8(7) . . ? C11 C6 N1 109.8(7) . . ? C11 C6 C7 109.8(8) . . ? N1 C6 C7 109.0(7) . . ? C6 C7 C8 111.6(8) . . ? C9 C8 C7 107.0(10) . . ? C10 C9 C8 111.2(9) . . ? C9 C10 C11 109.5(10) . . ? C6 C11 C10 110.9(9) . . ? N2 C12 C17 109.7(6) . . ? N2 C12 C13 111.5(7) . . ? C17 C12 C13 111.0(7) . . ? C12 C13 C14 113.7(7) . . ? C15 C14 C13 111.6(7) . . ? C16 C15 C14 109.0(8) . . ? C15 C16 C17 112.1(8) . . ? C12 C17 C16 113.2(7) . . ? N3 C18 N4 107.5(5) . . ? N3 C18 C19 129.0(7) . . ? N4 C18 C19 123.5(7) . . ? N3 C18 Ga2 54.1(3) . . ? N4 C18 Ga2 53.4(3) . . ? C19 C18 Ga2 176.9(6) . . ? C21 C19 C20 106.8(8) . . ? C21 C19 C22 109.8(8) . . ? C20 C19 C22 106.5(9) . . ? C21 C19 C18 109.7(7) . . ? C20 C19 C18 114.5(7) . . ? C22 C19 C18 109.5(7) . . ? N3 C23 C28 111.7(8) . . ? N3 C23 C24 110.5(7) . . ? C28 C23 C24 103.6(10) . . ? C23 C24 C25 112.3(9) . . ? C26 C25 C24 102.3(12) . . ? C25 C26 C27 114.9(12) . . ? C26 C27 C28 105.5(13) . . ? C23 C28 C27 114.3(10) . . ? N4 C29 C34 110.1(7) . . ? N4 C29 C30 108.7(7) . . ? C34 C29 C30 110.0(8) . . ? C29 C30 C31 110.8(8) . . ? C32 C31 C30 109.9(12) . . ? C33 C32 C31 110.3(9) . . ? C32 C33 C34 110.0(9) . . ? C29 C34 C33 112.2(8) . . ? N5 C35 N6 107.8(6) . . ? N5 C35 C36 125.5(6) . . ? N6 C35 C36 126.6(7) . . ? N5 C35 Ga3 54.3(4) . . ? N6 C35 Ga3 53.5(4) . . ? C36 C35 Ga3 179.7(7) . . ? C37 C36 C39 114.9(12) . . ? C37 C36 C35 106.8(10) . . ? C39 C36 C35 114.7(7) . . ? C37 C36 C38 109.5(12) . . ? C39 C36 C38 98.1(10) . . ? C35 C36 C38 112.7(8) . . ? N5 C40 C41 112.5(6) . . ? N5 C40 C45 108.8(7) . . ? C41 C40 C45 107.0(8) . . ? C40 C41 C42 113.2(6) . . ? C43 C42 C41 111.1(7) . . ? C44 C43 C42 110.7(9) . . ? C43 C44 C45 112.0(8) . . ? C40 C45 C44 113.4(8) . . ? C51 C46 C47 109.6(9) . . ? C51 C46 N6 115.7(7) . . ? C47 C46 N6 107.5(7) . . ? C46 C47 C48 114.1(8) . . ? C49 C48 C47 109.8(8) . . ? C48 C49 C50 110.1(9) . . ? C49 C50 C51 106.1(11) . . ? C46 C51 C50 112.7(9) . . ? C53 C52 Ga3 115.3(7) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 28.17 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.688 _refine_diff_density_min -0.555 _refine_diff_density_rms 0.081 _exptl_crystal_recrystallization_method 'from n-hexane' # Attachment '- 6-TZE102A-GaDcnaI2.CIF' data_6 _database_code_depnum_ccdc_archive 'CCDC 811982' _audit_creation_method SHELXL-97 _chemical_name_systematic diiodo-(N,N'-dicyclohexylneopentylamidinato)-gallium(III) _chemical_name_common diiodo-(N,N'-dicyclohexylneopentylamidinato)-gallium(iii) _chemical_melting_point ? _chemical_formula_moiety 'C17 H31 Ga I2 N2' _chemical_formula_sum 'C17 H31 Ga I2 N2' _chemical_formula_weight 586.96 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 'C 2/c' _symmetry_int_tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.952(6) _cell_length_b 10.316(2) _cell_length_c 17.640(4) _cell_angle_alpha 90.00 _cell_angle_beta 123.05(3) _cell_angle_gamma 90.00 _cell_volume 4263.4(15) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blocks _exptl_crystal_colour colourless _exptl_crystal_size_max 0.453 _exptl_crystal_size_mid 0.183 _exptl_crystal_size_min 0.155 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.829 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 4.187 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.2492 _exptl_absorpt_correction_T_max 0.5350 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20006 _diffrn_reflns_av_R_equivalents 0.1085 _diffrn_reflns_av_sigmaI/netI 0.0790 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 28.00 _reflns_number_total 5052 _reflns_number_gt 3457 _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^)+(0.0572P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5052 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0668 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1122 _refine_ls_wR_factor_gt 0.1044 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.937 _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 0.13509(2) 0.61786(5) 0.01056(3) 0.02613(13) Uani 1 1 d . . . I1 I 0.217461(17) 0.46406(4) 0.09438(3) 0.04437(12) Uani 1 1 d . . . I2 I 0.042622(18) 0.50100(4) -0.08297(3) 0.05110(14) Uani 1 1 d . . . N1 N 0.13318(18) 0.7727(4) 0.0712(3) 0.0271(8) Uani 1 1 d . . . N2 N 0.14563(17) 0.7744(4) -0.0402(2) 0.0263(8) Uani 1 1 d . . . C1 C 0.14013(19) 0.8509(5) 0.0173(3) 0.0247(9) Uani 1 1 d . . . C2 C 0.1418(2) 0.9981(5) 0.0234(3) 0.0294(10) Uani 1 1 d . . . C3 C 0.0850(3) 1.0467(6) 0.0062(4) 0.0420(13) Uani 1 1 d . . . H3A H 0.0777 1.0053 0.0490 0.063 Uiso 1 1 calc R . . H3B H 0.0541 1.0250 -0.0558 0.063 Uiso 1 1 calc R . . H3C H 0.0867 1.1409 0.0144 0.063 Uiso 1 1 calc R . . C4 C 0.1512(3) 1.0658(6) -0.0447(4) 0.0467(15) Uani 1 1 d . . . H4A H 0.1201 1.0432 -0.1063 0.070 Uiso 1 1 calc R . . H4B H 0.1877 1.0378 -0.0348 0.070 Uiso 1 1 calc R . . H4C H 0.1518 1.1599 -0.0365 0.070 Uiso 1 1 calc R . . C5 C 0.1919(3) 1.0390(5) 0.1163(4) 0.0416(13) Uani 1 1 d . . . H5A H 0.1884 0.9980 0.1632 0.062 Uiso 1 1 calc R . . H5B H 0.1917 1.1335 0.1221 0.062 Uiso 1 1 calc R . . H5C H 0.2277 1.0118 0.1235 0.062 Uiso 1 1 calc R . . C6 C 0.1251(2) 0.7971(5) 0.1448(3) 0.0274(10) Uani 1 1 d . . . H6A H 0.1349 0.8895 0.1646 0.033 Uiso 1 1 calc R . . C7 C 0.0632(2) 0.7711(6) 0.1144(3) 0.0357(11) Uani 1 1 d . . . H7A H 0.0525 0.6817 0.0904 0.043 Uiso 1 1 calc R . . H7B H 0.0376 0.8318 0.0652 0.043 Uiso 1 1 calc R . . C8 C 0.0551(2) 0.7876(6) 0.1930(4) 0.0397(13) Uani 1 1 d . . . H8A H 0.0630 0.8785 0.2143 0.048 Uiso 1 1 calc R . . H8B H 0.0150 0.7676 0.1722 0.048 Uiso 1 1 calc R . . C9 C 0.0950(3) 0.6978(6) 0.2703(3) 0.0406(13) Uani 1 1 d . . . H9A H 0.0904 0.7120 0.3215 0.049 Uiso 1 1 calc R . . H9B H 0.0847 0.6067 0.2503 0.049 Uiso 1 1 calc R . . C10 C 0.1563(3) 0.7208(6) 0.3014(4) 0.0439(13) Uani 1 1 d . . . H10A H 0.1809 0.6569 0.3488 0.053 Uiso 1 1 calc R . . H10B H 0.1680 0.8085 0.3282 0.053 Uiso 1 1 calc R . . C11 C 0.1645(2) 0.7089(6) 0.2230(3) 0.0364(12) Uani 1 1 d . . . H11A H 0.2046 0.7303 0.2448 0.044 Uiso 1 1 calc R . . H11B H 0.1575 0.6180 0.2015 0.044 Uiso 1 1 calc R . . C12 C 0.1437(2) 0.7963(5) -0.1242(3) 0.0284(10) Uani 1 1 d . . . H12A H 0.1633 0.8800 -0.1193 0.034 Uiso 1 1 calc R . . C13 C 0.0825(2) 0.8027(6) -0.2049(3) 0.0402(13) Uani 1 1 d . . . H13A H 0.0634 0.8787 -0.1986 0.048 Uiso 1 1 calc R . . H13B H 0.0619 0.7239 -0.2063 0.048 Uiso 1 1 calc R . . C14 C 0.0798(3) 0.8133(6) -0.2938(4) 0.0497(15) Uani 1 1 d . . . H14A H 0.0395 0.8111 -0.3452 0.060 Uiso 1 1 calc R . . H14B H 0.0963 0.8974 -0.2956 0.060 Uiso 1 1 calc R . . C15 C 0.1120(3) 0.7047(6) -0.3041(4) 0.0468(15) Uani 1 1 d . . . H15A H 0.1117 0.7182 -0.3599 0.056 Uiso 1 1 calc R . . H15B H 0.0926 0.6213 -0.3101 0.056 Uiso 1 1 calc R . . C16 C 0.1732(3) 0.6981(6) -0.2234(4) 0.0442(14) Uani 1 1 d . . . H16A H 0.1939 0.7772 -0.2215 0.053 Uiso 1 1 calc R . . H16B H 0.1925 0.6224 -0.2299 0.053 Uiso 1 1 calc R . . C17 C 0.1755(2) 0.6863(6) -0.1351(3) 0.0353(12) Uani 1 1 d . . . H17A H 0.1584 0.6026 -0.1344 0.042 Uiso 1 1 calc R . . H17B H 0.2158 0.6868 -0.0835 0.042 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.0327(3) 0.0217(3) 0.0286(2) -0.00165(19) 0.0197(2) -0.0020(2) I1 0.0455(2) 0.0370(2) 0.0524(2) 0.01067(16) 0.02789(19) 0.01205(16) I2 0.0419(2) 0.0505(3) 0.0616(3) -0.02156(19) 0.0287(2) -0.02026(18) N1 0.039(2) 0.021(2) 0.0300(19) -0.0017(15) 0.0246(18) -0.0003(17) N2 0.036(2) 0.026(2) 0.0212(17) 0.0002(14) 0.0188(17) -0.0012(17) C1 0.025(2) 0.024(3) 0.027(2) 0.0002(17) 0.0150(19) -0.0003(18) C2 0.039(3) 0.022(3) 0.031(2) 0.0058(18) 0.021(2) 0.003(2) C3 0.049(3) 0.030(3) 0.045(3) 0.004(2) 0.024(3) 0.011(2) C4 0.085(5) 0.025(3) 0.048(3) 0.002(2) 0.048(3) -0.004(3) C5 0.055(4) 0.025(3) 0.045(3) -0.005(2) 0.027(3) -0.010(2) C6 0.034(3) 0.028(3) 0.027(2) -0.0065(17) 0.022(2) -0.0080(19) C7 0.038(3) 0.042(3) 0.032(2) -0.005(2) 0.022(2) -0.001(2) C8 0.045(3) 0.041(3) 0.046(3) -0.012(2) 0.034(3) -0.012(2) C9 0.062(4) 0.040(3) 0.036(3) -0.008(2) 0.037(3) -0.015(3) C10 0.049(3) 0.051(4) 0.033(3) 0.002(2) 0.022(3) -0.004(3) C11 0.039(3) 0.043(3) 0.030(2) 0.004(2) 0.021(2) 0.004(2) C12 0.037(3) 0.028(3) 0.026(2) -0.0044(17) 0.021(2) -0.006(2) C13 0.042(3) 0.046(4) 0.030(2) 0.007(2) 0.018(2) 0.009(2) C14 0.069(4) 0.047(4) 0.026(2) 0.006(2) 0.022(3) 0.008(3) C15 0.076(5) 0.039(3) 0.036(3) -0.001(2) 0.037(3) -0.004(3) C16 0.060(4) 0.044(4) 0.042(3) -0.010(2) 0.036(3) 0.001(3) C17 0.037(3) 0.044(3) 0.028(2) 0.001(2) 0.020(2) 0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 N1 1.939(4) . ? Ga1 N2 1.946(4) . ? Ga1 C1 2.407(5) . ? Ga1 I2 2.4909(11) . ? Ga1 I1 2.5084(9) . ? N1 C1 1.339(6) . ? N1 C6 1.456(5) . ? N2 C1 1.359(6) . ? N2 C12 1.471(5) . ? C1 C2 1.521(7) . ? C2 C5 1.524(7) . ? C2 C4 1.530(6) . ? C2 C3 1.531(7) . ? C6 C11 1.512(7) . ? C6 C7 1.532(7) . ? C7 C8 1.532(6) . ? C8 C9 1.517(8) . ? C9 C10 1.506(8) . ? C10 C11 1.526(7) . ? C12 C13 1.516(7) . ? C12 C17 1.517(7) . ? C13 C14 1.532(7) . ? C14 C15 1.508(9) . ? C15 C16 1.518(9) . ? C16 C17 1.527(6) . ? 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 68.08(15) . . ? N1 Ga1 C1 33.75(14) . . ? N2 Ga1 C1 34.34(14) . . ? N1 Ga1 I2 115.68(13) . . ? N2 Ga1 I2 117.37(12) . . ? C1 Ga1 I2 121.85(11) . . ? N1 Ga1 I1 119.25(13) . . ? N2 Ga1 I1 118.40(12) . . ? C1 Ga1 I1 126.33(11) . . ? I2 Ga1 I1 111.81(4) . . ? C1 N1 C6 133.0(4) . . ? C1 N1 Ga1 92.7(3) . . ? C6 N1 Ga1 134.3(3) . . ? C1 N2 C12 134.9(4) . . ? C1 N2 Ga1 91.8(3) . . ? C12 N2 Ga1 131.3(3) . . ? N1 C1 N2 107.4(4) . . ? N1 C1 C2 124.2(4) . . ? N2 C1 C2 128.3(4) . . ? N1 C1 Ga1 53.6(2) . . ? N2 C1 Ga1 53.9(2) . . ? C2 C1 Ga1 177.6(3) . . ? C1 C2 C5 109.1(4) . . ? C1 C2 C4 114.4(4) . . ? C5 C2 C4 105.5(4) . . ? C1 C2 C3 108.9(4) . . ? C5 C2 C3 111.5(4) . . ? C4 C2 C3 107.4(5) . . ? N1 C6 C11 108.6(4) . . ? N1 C6 C7 110.6(4) . . ? C11 C6 C7 109.6(4) . . ? C6 C7 C8 111.1(4) . . ? C9 C8 C7 110.2(5) . . ? C10 C9 C8 111.4(4) . . ? C9 C10 C11 111.1(4) . . ? C6 C11 C10 112.5(4) . . ? N2 C12 C13 110.8(4) . . ? N2 C12 C17 108.1(4) . . ? C13 C12 C17 110.6(4) . . ? C12 C13 C14 111.4(5) . . ? C15 C14 C13 111.7(5) . . ? C14 C15 C16 111.2(5) . . ? C15 C16 C17 111.0(5) . . ? C12 C17 C16 111.6(4) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.159 _refine_diff_density_min -1.101 _refine_diff_density_rms 0.153 _exptl_crystal_recrystallization_method 'from toluene'