Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Cameron Jones' _publ_contact_author_address ; School of Chemistry Cardiff University Main Building Cardiff CF10 3AT UNITED KINGDOM ; _publ_contact_author_email JONESCA6@CARDIFF.AC.UK _publ_section_title ; The Reactivity of Gallium (I), (II) and (III) Heterocycles Towards Group 15 Substrates: Attempts to Prepare Gallium-Terminal PnictinideneComplexes ; loop_ _publ_author_name 'Cameron Jones' 'Robert J. Baker' 'Evamarie Hey-Hawkins' 'David P. Mills' 'Damien M. Murphy' 'Robert Wolf' data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 280910' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H72 Ga K N4 P4' _chemical_formula_weight 1033.88 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' P P 0.1023 0.0942 '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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.808(4) _cell_length_b 13.871(3) _cell_length_c 20.504(4) _cell_angle_alpha 90.00 _cell_angle_beta 114.97(3) _cell_angle_gamma 90.00 _cell_volume 5623(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2184 _exptl_absorpt_coefficient_mu 0.715 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.702 _exptl_absorpt_correction_T_max 0.905 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18873 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0734 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 25.04 _reflns_number_total 9844 _reflns_number_gt 7833 _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. The relatively high R-factors for the crystal structure arose from the poor quality and high mosaicity of the crystal used for the experiment. A number of attempts were made to select better crystal samples but to no avail. In addition, the X-ray data were found to be weak at the higher angles of the collection. Despite this the molecular connectivity exhibited by the crystal structure is unambiguous. ; _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^)+(0.1067P)^2^+31.0454P] 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 'calculated (riding model)' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0049(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9844 _refine_ls_number_parameters 608 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1131 _refine_ls_R_factor_gt 0.0947 _refine_ls_wR_factor_ref 0.2459 _refine_ls_wR_factor_gt 0.2364 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _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 0.22940(3) 0.96044(5) 0.29006(4) 0.0219(2) Uani 1 1 d . . . K1 K 0.18060(8) 1.24220(11) 0.34115(9) 0.0366(4) Uani 1 1 d . . . P1 P 0.24923(8) 1.02524(12) 0.19310(9) 0.0254(4) Uani 1 1 d . . . P2 P 0.27934(8) 1.16511(12) 0.24814(9) 0.0281(4) Uani 1 1 d . . . P3 P 0.36274(8) 1.12725(12) 0.35440(9) 0.0263(4) Uani 1 1 d . . . P4 P 0.29165(8) 1.06325(12) 0.39234(9) 0.0241(4) Uani 1 1 d . . . N1 N 0.1375(3) 0.9642(4) 0.2799(3) 0.0260(11) Uani 1 1 d . . . N2 N 0.2259(3) 0.8237(4) 0.2936(3) 0.0248(11) Uani 1 1 d . . . N3 N 0.1726(3) 1.3630(5) 0.4452(3) 0.0438(15) Uani 1 1 d . . . N4 N 0.1648(3) 1.4391(5) 0.3046(4) 0.0457(16) Uani 1 1 d . . . C1 C 0.1190(3) 0.8693(5) 0.2868(3) 0.0281(14) Uani 1 1 d . . . H1 H 0.0772 0.8554 0.2889 0.034 Uiso 1 1 calc R . . C2 C 0.1626(3) 0.7981(5) 0.2905(4) 0.0293(14) Uani 1 1 d . . . H2 H 0.1506 0.7323 0.2910 0.035 Uiso 1 1 calc R . . C3 C 0.0983(3) 1.0405(4) 0.2870(4) 0.0273(14) Uani 1 1 d . . . C4 C 0.0698(3) 1.1088(5) 0.2307(4) 0.0297(14) Uani 1 1 d . . . C5 C 0.0294(3) 1.1833(5) 0.2368(4) 0.0387(17) Uani 1 1 d . . . H5 H 0.0109 1.2294 0.1992 0.046 Uiso 1 1 calc R . . C6 C 0.0158(4) 1.1909(6) 0.2973(4) 0.0415(18) Uani 1 1 d . . . H6 H -0.0129 1.2406 0.3004 0.050 Uiso 1 1 calc R . . C7 C 0.0445(3) 1.1257(5) 0.3523(4) 0.0370(16) Uani 1 1 d . . . H7 H 0.0360 1.1320 0.3939 0.044 Uiso 1 1 calc R . . C8 C 0.0856(3) 1.0505(5) 0.3492(4) 0.0302(15) Uani 1 1 d . . . C9 C 0.0821(3) 1.0989(5) 0.1629(4) 0.0327(15) Uani 1 1 d . . . H9 H 0.1301 1.0775 0.1790 0.039 Uiso 1 1 calc R . . C10 C 0.0746(5) 1.1929(6) 0.1212(5) 0.055(2) Uani 1 1 d . . . H10A H 0.0920 1.1838 0.0847 0.082 Uiso 1 1 calc R . . H10B H 0.1002 1.2441 0.1544 0.082 Uiso 1 1 calc R . . H10C H 0.0267 1.2109 0.0976 0.082 Uiso 1 1 calc R . . C11 C 0.0384(5) 1.0211(7) 0.1141(5) 0.060(2) Uani 1 1 d . . . H11A H 0.0431 0.9618 0.1419 0.090 Uiso 1 1 calc R . . H11B H 0.0526 1.0089 0.0755 0.090 Uiso 1 1 calc R . . H11C H -0.0090 1.0419 0.0933 0.090 Uiso 1 1 calc R . . C12 C 0.1171(3) 0.9841(5) 0.4145(4) 0.0311(15) Uani 1 1 d . . . H12 H 0.1485 0.9392 0.4054 0.037 Uiso 1 1 calc R . . C13 C 0.1585(4) 1.0396(6) 0.4832(4) 0.0420(18) Uani 1 1 d . . . H13A H 0.1928 1.0784 0.4762 0.063 Uiso 1 1 calc R . . H13B H 0.1808 0.9941 0.5228 0.063 Uiso 1 1 calc R . . H13C H 0.1287 1.0821 0.4949 0.063 Uiso 1 1 calc R . . C14 C 0.0629(4) 0.9226(6) 0.4237(4) 0.0446(18) Uani 1 1 d . . . H14A H 0.0292 0.9648 0.4289 0.067 Uiso 1 1 calc R . . H14B H 0.0841 0.8821 0.4666 0.067 Uiso 1 1 calc R . . H14C H 0.0407 0.8815 0.3812 0.067 Uiso 1 1 calc R . . C15 C 0.2601(3) 0.7549(4) 0.2694(4) 0.0288(14) Uani 1 1 d . . . C16 C 0.3213(4) 0.7151(5) 0.3183(4) 0.0327(15) Uani 1 1 d . . . C17 C 0.3541(4) 0.6456(5) 0.2954(5) 0.0434(18) Uani 1 1 d . . . H17 H 0.3961 0.6201 0.3286 0.052 Uiso 1 1 calc R . . C18 C 0.3262(4) 0.6134(6) 0.2254(5) 0.0465(19) Uani 1 1 d . . . H18 H 0.3479 0.5642 0.2106 0.056 Uiso 1 1 calc R . . C19 C 0.2668(4) 0.6535(6) 0.1774(4) 0.0442(19) Uani 1 1 d . . . H19 H 0.2484 0.6322 0.1288 0.053 Uiso 1 1 calc R . . C20 C 0.2323(4) 0.7243(5) 0.1970(4) 0.0337(15) Uani 1 1 d . . . C21 C 0.3504(4) 0.7435(5) 0.3986(4) 0.0400(17) Uani 1 1 d . . . H21 H 0.3363 0.8115 0.4008 0.048 Uiso 1 1 calc R . . C22 C 0.3187(5) 0.6819(6) 0.4371(4) 0.051(2) Uani 1 1 d . . . H22A H 0.2695 0.6902 0.4142 0.077 Uiso 1 1 calc R . . H22B H 0.3363 0.7016 0.4876 0.077 Uiso 1 1 calc R . . H22C H 0.3298 0.6140 0.4343 0.077 Uiso 1 1 calc R . . C23 C 0.4281(4) 0.7410(7) 0.4362(5) 0.061(2) Uani 1 1 d . . . H23A H 0.4435 0.7701 0.4841 0.091 Uiso 1 1 calc R . . H23B H 0.4466 0.7772 0.4076 0.091 Uiso 1 1 calc R . . H23C H 0.4437 0.6740 0.4410 0.091 Uiso 1 1 calc R . . C24 C 0.1691(4) 0.7703(5) 0.1401(4) 0.0384(17) Uani 1 1 d . . . H24 H 0.1581 0.8284 0.1621 0.046 Uiso 1 1 calc R . . C25 C 0.1785(5) 0.8036(7) 0.0738(4) 0.052(2) Uani 1 1 d . . . H25A H 0.2184 0.8454 0.0888 0.078 Uiso 1 1 calc R . . H25B H 0.1384 0.8394 0.0416 0.078 Uiso 1 1 calc R . . H25C H 0.1849 0.7473 0.0484 0.078 Uiso 1 1 calc R . . C26 C 0.1086(4) 0.7009(6) 0.1172(4) 0.0460(19) Uani 1 1 d . . . H26A H 0.1191 0.6415 0.0981 0.069 Uiso 1 1 calc R . . H26B H 0.0686 0.7314 0.0799 0.069 Uiso 1 1 calc R . . H26C H 0.0994 0.6855 0.1589 0.069 Uiso 1 1 calc R . . C27 C 0.3271(3) 0.9661(5) 0.2000(4) 0.0307(15) Uani 1 1 d . . . C28 C 0.3399(4) 0.9654(6) 0.1386(4) 0.0384(17) Uani 1 1 d . . . H28 H 0.3085 0.9958 0.0961 0.046 Uiso 1 1 calc R . . C29 C 0.3963(4) 0.9220(6) 0.1377(5) 0.048(2) Uani 1 1 d . . . H29 H 0.4032 0.9206 0.0950 0.057 Uiso 1 1 calc R . . C30 C 0.4428(4) 0.8804(7) 0.2005(5) 0.059(2) Uani 1 1 d . . . H30 H 0.4830 0.8527 0.2015 0.071 Uiso 1 1 calc R . . C31 C 0.4311(4) 0.8788(7) 0.2614(5) 0.054(2) Uani 1 1 d . . . H31 H 0.4625 0.8473 0.3034 0.064 Uiso 1 1 calc R . . C32 C 0.3745(3) 0.9221(5) 0.2624(4) 0.0345(16) Uani 1 1 d . . . H32 H 0.3678 0.9221 0.3052 0.041 Uiso 1 1 calc R . . C33 C 0.3268(4) 1.2242(5) 0.2034(4) 0.0333(15) Uani 1 1 d . . . C34 C 0.3869(3) 1.1873(6) 0.2057(4) 0.0371(17) Uani 1 1 d . . . H34 H 0.4058 1.1302 0.2323 0.044 Uiso 1 1 calc R . . C35 C 0.4193(4) 1.2336(7) 0.1692(4) 0.051(2) Uani 1 1 d . . . H35 H 0.4597 1.2071 0.1697 0.062 Uiso 1 1 calc R . . C36 C 0.3933(5) 1.3176(8) 0.1323(5) 0.068(3) Uani 1 1 d . . . H36 H 0.4162 1.3491 0.1077 0.081 Uiso 1 1 calc R . . C37 C 0.3348(6) 1.3565(7) 0.1305(4) 0.069(3) Uani 1 1 d . . . H37 H 0.3175 1.4148 0.1051 0.083 Uiso 1 1 calc R . . C38 C 0.3001(4) 1.3106(6) 0.1661(4) 0.049(2) Uani 1 1 d . . . H38 H 0.2596 1.3373 0.1650 0.058 Uiso 1 1 calc R . . C39 C 0.3802(3) 1.2469(5) 0.3966(4) 0.0301(15) Uani 1 1 d . . . C40 C 0.4126(3) 1.3173(5) 0.3708(4) 0.0365(16) Uani 1 1 d . . . H40 H 0.4211 1.3028 0.3302 0.044 Uiso 1 1 calc R . . C41 C 0.4315(4) 1.4053(5) 0.4035(4) 0.0423(18) Uani 1 1 d . . . H41 H 0.4531 1.4507 0.3854 0.051 Uiso 1 1 calc R . . C42 C 0.4196(4) 1.4284(5) 0.4622(4) 0.0427(19) Uani 1 1 d . . . H42 H 0.4328 1.4897 0.4845 0.051 Uiso 1 1 calc R . . C43 C 0.3884(4) 1.3628(5) 0.4888(5) 0.0430(18) Uani 1 1 d . . . H43 H 0.3808 1.3785 0.5299 0.052 Uiso 1 1 calc R . . C44 C 0.3680(3) 1.2733(5) 0.4555(4) 0.0359(16) Uani 1 1 d . . . H44 H 0.3454 1.2295 0.4734 0.043 Uiso 1 1 calc R . . C45 C 0.3464(3) 0.9926(5) 0.4708(3) 0.0280(14) Uani 1 1 d . . . C46 C 0.4159(3) 1.0113(5) 0.5088(4) 0.0345(16) Uani 1 1 d . . . H46 H 0.4370 1.0574 0.4907 0.041 Uiso 1 1 calc R . . C47 C 0.4541(4) 0.9631(6) 0.5724(4) 0.0450(19) Uani 1 1 d . . . H47 H 0.5009 0.9774 0.5981 0.054 Uiso 1 1 calc R . . C48 C 0.4246(4) 0.8946(6) 0.5986(4) 0.048(2) Uani 1 1 d . . . H48 H 0.4509 0.8606 0.6416 0.058 Uiso 1 1 calc R . . C49 C 0.3564(4) 0.8759(6) 0.5616(4) 0.0451(19) Uani 1 1 d . . . H49 H 0.3358 0.8293 0.5799 0.054 Uiso 1 1 calc R . . C50 C 0.3177(4) 0.9236(5) 0.4988(4) 0.0361(16) Uani 1 1 d . . . H50 H 0.2709 0.9094 0.4742 0.043 Uiso 1 1 calc R . . C51 C 0.1035(4) 1.3627(8) 0.4410(5) 0.061(2) Uani 1 1 d . . . H51A H 0.0970 1.4197 0.4656 0.092 Uiso 1 1 calc R . . H51B H 0.0967 1.3043 0.4641 0.092 Uiso 1 1 calc R . . H51C H 0.0707 1.3638 0.3904 0.092 Uiso 1 1 calc R . . C52 C 0.2188(4) 1.3268(7) 0.5164(5) 0.055(2) Uani 1 1 d . . . H52A H 0.2656 1.3403 0.5246 0.082 Uiso 1 1 calc R . . H52B H 0.2126 1.2571 0.5186 0.082 Uiso 1 1 calc R . . H52C H 0.2090 1.3589 0.5535 0.082 Uiso 1 1 calc R . . C53 C 0.1932(5) 1.4603(6) 0.4344(5) 0.049(2) Uani 1 1 d . . . H53A H 0.2422 1.4598 0.4465 0.058 Uiso 1 1 calc R . . H53B H 0.1859 1.5051 0.4681 0.058 Uiso 1 1 calc R . . C54 C 0.1559(5) 1.4976(6) 0.3596(5) 0.054(2) Uani 1 1 d . . . H54A H 0.1071 1.5007 0.3482 0.065 Uiso 1 1 calc R . . H54B H 0.1714 1.5641 0.3574 0.065 Uiso 1 1 calc R . . C55 C 0.1100(6) 1.4609(8) 0.2338(6) 0.088(4) Uani 1 1 d . . . H55A H 0.0663 1.4488 0.2351 0.132 Uiso 1 1 calc R . . H55B H 0.1145 1.4196 0.1973 0.132 Uiso 1 1 calc R . . H55C H 0.1128 1.5287 0.2219 0.132 Uiso 1 1 calc R . . C56 C 0.2304(5) 1.4588(7) 0.3031(5) 0.063(3) Uani 1 1 d . . . H56A H 0.2335 1.5275 0.2937 0.095 Uiso 1 1 calc R . . H56B H 0.2345 1.4205 0.2650 0.095 Uiso 1 1 calc R . . H56C H 0.2670 1.4416 0.3496 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 0.0200(4) 0.0202(4) 0.0256(4) -0.0004(3) 0.0097(3) -0.0004(2) K1 0.0392(9) 0.0284(8) 0.0436(9) -0.0013(7) 0.0186(7) 0.0044(6) P1 0.0255(8) 0.0269(9) 0.0253(8) -0.0004(7) 0.0120(7) -0.0014(6) P2 0.0280(9) 0.0268(9) 0.0292(9) 0.0017(7) 0.0117(7) -0.0005(7) P3 0.0237(8) 0.0251(9) 0.0311(9) -0.0024(7) 0.0127(7) -0.0025(6) P4 0.0221(8) 0.0242(8) 0.0259(8) -0.0020(6) 0.0100(7) -0.0008(6) N1 0.024(3) 0.024(3) 0.032(3) 0.001(2) 0.013(2) -0.001(2) N2 0.031(3) 0.019(3) 0.026(3) 0.001(2) 0.014(2) 0.003(2) N3 0.051(4) 0.042(4) 0.042(4) -0.004(3) 0.023(3) 0.000(3) N4 0.052(4) 0.037(4) 0.040(4) 0.004(3) 0.012(3) -0.002(3) C1 0.028(3) 0.026(3) 0.032(3) -0.005(3) 0.015(3) -0.004(3) C2 0.030(3) 0.021(3) 0.037(4) -0.001(3) 0.015(3) -0.003(3) C3 0.020(3) 0.024(3) 0.037(4) 0.000(3) 0.012(3) -0.002(2) C4 0.026(3) 0.030(4) 0.033(4) 0.000(3) 0.011(3) -0.004(3) C5 0.031(4) 0.038(4) 0.048(4) 0.010(3) 0.017(3) 0.011(3) C6 0.035(4) 0.041(4) 0.054(5) 0.005(4) 0.024(4) 0.017(3) C7 0.034(4) 0.041(4) 0.043(4) 0.007(3) 0.024(3) 0.007(3) C8 0.021(3) 0.032(4) 0.036(4) 0.008(3) 0.011(3) 0.004(3) C9 0.025(3) 0.043(4) 0.028(3) 0.005(3) 0.010(3) 0.003(3) C10 0.068(6) 0.053(5) 0.054(5) 0.021(4) 0.036(4) 0.017(4) C11 0.065(6) 0.067(6) 0.042(5) -0.012(4) 0.017(4) -0.015(5) C12 0.032(4) 0.028(4) 0.033(4) 0.004(3) 0.014(3) 0.003(3) C13 0.041(4) 0.043(4) 0.039(4) 0.003(3) 0.014(3) 0.009(3) C14 0.050(5) 0.045(4) 0.043(4) 0.007(4) 0.024(4) -0.003(4) C15 0.037(4) 0.022(3) 0.030(3) -0.003(3) 0.017(3) -0.002(3) C16 0.040(4) 0.024(3) 0.035(4) 0.001(3) 0.017(3) 0.004(3) C17 0.042(4) 0.033(4) 0.060(5) 0.002(4) 0.026(4) 0.008(3) C18 0.047(5) 0.039(4) 0.062(5) -0.010(4) 0.031(4) 0.007(3) C19 0.050(5) 0.046(5) 0.044(4) -0.017(4) 0.027(4) -0.010(4) C20 0.040(4) 0.031(4) 0.037(4) -0.005(3) 0.024(3) -0.008(3) C21 0.038(4) 0.035(4) 0.037(4) 0.000(3) 0.007(3) 0.008(3) C22 0.073(6) 0.039(4) 0.035(4) -0.001(4) 0.017(4) 0.000(4) C23 0.045(5) 0.073(6) 0.044(5) 0.004(4) 0.000(4) 0.017(4) C24 0.042(4) 0.039(4) 0.030(4) -0.004(3) 0.011(3) -0.008(3) C25 0.064(5) 0.055(5) 0.035(4) -0.002(4) 0.019(4) -0.019(4) C26 0.041(4) 0.059(5) 0.036(4) -0.014(4) 0.015(3) -0.017(4) C27 0.029(3) 0.028(3) 0.042(4) -0.006(3) 0.021(3) -0.003(3) C28 0.034(4) 0.045(4) 0.039(4) -0.001(3) 0.018(3) -0.002(3) C29 0.045(5) 0.060(5) 0.048(5) -0.012(4) 0.029(4) -0.001(4) C30 0.049(5) 0.082(7) 0.060(6) -0.008(5) 0.036(4) 0.018(5) C31 0.045(5) 0.066(6) 0.048(5) 0.003(4) 0.018(4) 0.021(4) C32 0.035(4) 0.035(4) 0.040(4) -0.003(3) 0.022(3) 0.003(3) C33 0.039(4) 0.031(4) 0.030(4) -0.005(3) 0.014(3) -0.011(3) C34 0.035(4) 0.047(4) 0.032(4) -0.007(3) 0.016(3) -0.017(3) C35 0.054(5) 0.063(6) 0.040(4) -0.003(4) 0.022(4) -0.030(4) C36 0.065(6) 0.093(8) 0.038(5) 0.008(5) 0.015(4) -0.042(6) C37 0.090(8) 0.052(5) 0.033(5) 0.016(4) -0.005(5) -0.035(5) C38 0.050(5) 0.036(4) 0.045(5) 0.004(4) 0.006(4) -0.015(4) C39 0.019(3) 0.030(4) 0.037(4) -0.006(3) 0.008(3) -0.001(2) C40 0.035(4) 0.039(4) 0.039(4) -0.003(3) 0.019(3) -0.010(3) C41 0.039(4) 0.033(4) 0.055(5) -0.002(4) 0.020(4) -0.011(3) C42 0.035(4) 0.027(4) 0.057(5) -0.011(3) 0.010(3) -0.004(3) C43 0.039(4) 0.034(4) 0.054(5) -0.009(4) 0.018(4) -0.002(3) C44 0.035(4) 0.031(4) 0.038(4) -0.005(3) 0.012(3) -0.005(3) C45 0.030(3) 0.029(3) 0.028(3) -0.005(3) 0.015(3) 0.003(3) C46 0.032(4) 0.040(4) 0.033(4) -0.006(3) 0.015(3) 0.003(3) C47 0.041(4) 0.052(5) 0.032(4) -0.004(4) 0.006(3) 0.017(4) C48 0.054(5) 0.057(5) 0.029(4) 0.008(4) 0.014(4) 0.023(4) C49 0.069(6) 0.035(4) 0.040(4) 0.008(3) 0.031(4) 0.006(4) C50 0.040(4) 0.031(4) 0.043(4) -0.003(3) 0.023(3) 0.005(3) C51 0.054(5) 0.071(6) 0.061(6) -0.003(5) 0.027(5) 0.006(5) C52 0.053(5) 0.055(5) 0.045(5) -0.004(4) 0.009(4) -0.003(4) C53 0.061(5) 0.034(4) 0.050(5) -0.010(4) 0.023(4) 0.000(4) C54 0.068(6) 0.033(4) 0.059(5) 0.001(4) 0.026(5) 0.004(4) C55 0.100(9) 0.064(7) 0.056(6) 0.006(5) -0.010(6) 0.003(6) C56 0.075(7) 0.058(6) 0.061(6) -0.005(5) 0.034(5) -0.015(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 N2 1.901(5) . ? Ga1 N1 1.927(5) . ? Ga1 P1 2.3818(18) . ? Ga1 P4 2.4230(18) . ? K1 N3 2.776(7) . ? K1 N4 2.814(7) . ? K1 C4 3.126(7) . ? K1 C5 3.188(7) . ? K1 C3 3.256(6) . ? K1 P4 3.314(2) . ? K1 C6 3.391(8) . ? K1 C8 3.416(7) . ? K1 C7 3.470(7) . ? K1 P2 3.590(2) . ? P1 C27 1.837(7) . ? P1 P2 2.201(2) . ? P2 C33 1.840(7) . ? P2 P3 2.233(3) . ? P3 C39 1.836(7) . ? P3 P4 2.194(2) . ? P4 C45 1.832(7) . ? N1 C1 1.402(8) . ? N1 C3 1.406(8) . ? N2 C2 1.401(8) . ? N2 C15 1.423(8) . ? N3 C53 1.468(10) . ? N3 C52 1.469(11) . ? N3 C51 1.472(11) . ? N4 C54 1.467(11) . ? N4 C56 1.470(11) . ? N4 C55 1.470(11) . ? C1 C2 1.351(9) . ? C3 C4 1.419(9) . ? C3 C8 1.421(10) . ? C4 C5 1.397(10) . ? C4 C9 1.528(9) . ? C5 C6 1.396(11) . ? C6 C7 1.374(10) . ? C7 C8 1.393(10) . ? C8 C12 1.529(9) . ? C9 C11 1.506(11) . ? C9 C10 1.530(11) . ? C12 C13 1.523(10) . ? C12 C14 1.531(10) . ? C15 C16 1.400(9) . ? C15 C20 1.412(9) . ? C16 C17 1.394(10) . ? C16 C21 1.545(10) . ? C17 C18 1.376(12) . ? C18 C19 1.371(12) . ? C19 C20 1.397(10) . ? C20 C24 1.520(10) . ? C21 C22 1.513(12) . ? C21 C23 1.537(11) . ? C24 C25 1.531(11) . ? C24 C26 1.538(10) . ? C27 C28 1.399(10) . ? C27 C32 1.401(10) . ? C28 C29 1.377(11) . ? C29 C30 1.384(13) . ? C30 C31 1.376(12) . ? C31 C32 1.380(10) . ? C33 C34 1.391(10) . ? C33 C38 1.409(11) . ? C34 C35 1.384(10) . ? C35 C36 1.375(14) . ? C36 C37 1.374(16) . ? C37 C38 1.404(13) . ? C39 C44 1.391(10) . ? C39 C40 1.430(10) . ? C40 C41 1.369(10) . ? C41 C42 1.371(11) . ? C42 C43 1.380(11) . ? C43 C44 1.396(10) . ? C45 C50 1.391(10) . ? C45 C46 1.406(10) . ? C46 C47 1.387(10) . ? C47 C48 1.378(12) . ? C48 C49 1.378(12) . ? C49 C50 1.375(11) . ? C53 C54 1.493(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ga1 N1 88.5(2) . . ? N2 Ga1 P1 115.67(16) . . ? N1 Ga1 P1 116.53(17) . . ? N2 Ga1 P4 124.80(16) . . ? N1 Ga1 P4 104.77(17) . . ? P1 Ga1 P4 105.52(6) . . ? N3 K1 N4 65.1(2) . . ? N3 K1 C4 129.36(19) . . ? N4 K1 C4 114.28(19) . . ? N3 K1 C5 106.7(2) . . ? N4 K1 C5 95.4(2) . . ? C4 K1 C5 25.55(18) . . ? N3 K1 C3 125.18(19) . . ? N4 K1 C3 139.06(18) . . ? C4 K1 C3 25.59(17) . . ? C5 K1 C3 44.42(17) . . ? N3 K1 P4 118.91(15) . . ? N4 K1 P4 143.33(16) . . ? C4 K1 P4 91.38(13) . . ? C5 K1 P4 115.54(14) . . ? C3 K1 P4 71.84(12) . . ? N3 K1 C6 85.8(2) . . ? N4 K1 C6 97.8(2) . . ? C4 K1 C6 43.57(18) . . ? C5 K1 C6 24.25(19) . . ? C3 K1 C6 50.16(17) . . ? P4 K1 C6 118.55(14) . . ? N3 K1 C8 101.32(19) . . ? N4 K1 C8 139.41(19) . . ? C4 K1 C8 43.60(17) . . ? C5 K1 C8 49.98(17) . . ? C3 K1 C8 24.44(17) . . ? P4 K1 C8 77.21(11) . . ? C6 K1 C8 41.72(16) . . ? N3 K1 C7 84.11(19) . . ? N4 K1 C7 117.23(19) . . ? C4 K1 C7 49.57(18) . . ? C5 K1 C7 41.76(19) . . ? C3 K1 C7 42.14(17) . . ? P4 K1 C7 99.27(13) . . ? C6 K1 C7 23.07(17) . . ? C8 K1 C7 23.32(16) . . ? N3 K1 P2 146.59(15) . . ? N4 K1 P2 100.44(16) . . ? C4 K1 P2 83.80(13) . . ? C5 K1 P2 104.44(15) . . ? C3 K1 P2 86.04(12) . . ? P4 K1 P2 54.76(5) . . ? C6 K1 P2 127.07(14) . . ? C8 K1 P2 107.81(13) . . ? C7 K1 P2 128.15(14) . . ? C27 P1 P2 106.7(2) . . ? C27 P1 Ga1 104.8(2) . . ? P2 P1 Ga1 91.42(8) . . ? C33 P2 P1 104.3(2) . . ? C33 P2 P3 101.2(2) . . ? P1 P2 P3 103.70(9) . . ? C33 P2 K1 136.2(2) . . ? P1 P2 K1 114.77(8) . . ? P3 P2 K1 88.62(7) . . ? C39 P3 P4 103.7(2) . . ? C39 P3 P2 99.7(2) . . ? P4 P3 P2 91.99(9) . . ? C45 P4 P3 103.4(2) . . ? C45 P4 Ga1 111.4(2) . . ? P3 P4 Ga1 98.78(8) . . ? C45 P4 K1 142.9(2) . . ? P3 P4 K1 96.66(8) . . ? Ga1 P4 K1 95.69(6) . . ? C1 N1 C3 118.9(5) . . ? C1 N1 Ga1 107.1(4) . . ? C3 N1 Ga1 131.3(4) . . ? C2 N2 C15 117.7(5) . . ? C2 N2 Ga1 107.8(4) . . ? C15 N2 Ga1 128.3(4) . . ? C53 N3 C52 109.8(7) . . ? C53 N3 C51 111.4(7) . . ? C52 N3 C51 108.3(7) . . ? C53 N3 K1 108.5(5) . . ? C52 N3 K1 108.6(5) . . ? C51 N3 K1 110.3(5) . . ? C54 N4 C56 111.1(7) . . ? C54 N4 C55 109.2(8) . . ? C56 N4 C55 109.5(8) . . ? C54 N4 K1 111.9(5) . . ? C56 N4 K1 100.1(5) . . ? C55 N4 K1 114.8(6) . . ? C2 C1 N1 117.8(6) . . ? C1 C2 N2 118.3(6) . . ? N1 C3 C4 119.6(6) . . ? N1 C3 C8 121.6(6) . . ? C4 C3 C8 118.8(6) . . ? N1 C3 K1 114.2(4) . . ? C4 C3 K1 72.1(4) . . ? C8 C3 K1 84.1(4) . . ? C5 C4 C3 119.8(6) . . ? C5 C4 C9 120.5(6) . . ? C3 C4 C9 119.7(6) . . ? C5 C4 K1 79.7(4) . . ? C3 C4 K1 82.3(4) . . ? C9 C4 K1 109.5(4) . . ? C6 C5 C4 121.0(7) . . ? C6 C5 K1 86.1(5) . . ? C4 C5 K1 74.8(4) . . ? C7 C6 C5 119.1(6) . . ? C7 C6 K1 81.7(4) . . ? C5 C6 K1 69.7(4) . . ? C6 C7 C8 122.3(7) . . ? C6 C7 K1 75.2(4) . . ? C8 C7 K1 76.2(4) . . ? C7 C8 C3 119.1(6) . . ? C7 C8 C12 118.1(6) . . ? C3 C8 C12 122.8(6) . . ? C7 C8 K1 80.5(4) . . ? C3 C8 K1 71.5(4) . . ? C12 C8 K1 117.1(4) . . ? C11 C9 C4 111.3(6) . . ? C11 C9 C10 110.5(7) . . ? C4 C9 C10 114.4(6) . . ? C13 C12 C8 112.1(6) . . ? C13 C12 C14 110.9(6) . . ? C8 C12 C14 111.1(6) . . ? C16 C15 C20 119.4(6) . . ? C16 C15 N2 119.7(6) . . ? C20 C15 N2 120.9(6) . . ? C17 C16 C15 120.1(7) . . ? C17 C16 C21 119.7(6) . . ? C15 C16 C21 120.0(6) . . ? C18 C17 C16 120.8(7) . . ? C19 C18 C17 119.0(7) . . ? C18 C19 C20 122.6(7) . . ? C19 C20 C15 118.0(7) . . ? C19 C20 C24 119.9(7) . . ? C15 C20 C24 121.9(6) . . ? C22 C21 C23 112.0(7) . . ? C22 C21 C16 109.9(6) . . ? C23 C21 C16 113.5(7) . . ? C20 C24 C25 112.9(7) . . ? C20 C24 C26 110.8(6) . . ? C25 C24 C26 109.7(6) . . ? C28 C27 C32 117.9(6) . . ? C28 C27 P1 117.6(5) . . ? C32 C27 P1 124.5(5) . . ? C29 C28 C27 122.2(7) . . ? C28 C29 C30 118.6(7) . . ? C31 C30 C29 120.5(7) . . ? C30 C31 C32 121.0(8) . . ? C31 C32 C27 119.8(7) . . ? C34 C33 C38 119.9(7) . . ? C34 C33 P2 122.7(6) . . ? C38 C33 P2 117.4(6) . . ? C35 C34 C33 120.0(8) . . ? C36 C35 C34 120.4(9) . . ? C37 C36 C35 120.6(8) . . ? C36 C37 C38 120.5(9) . . ? C37 C38 C33 118.6(9) . . ? C44 C39 C40 116.5(6) . . ? C44 C39 P3 124.7(5) . . ? C40 C39 P3 118.7(5) . . ? C41 C40 C39 121.4(7) . . ? C40 C41 C42 120.6(7) . . ? C41 C42 C43 120.0(7) . . ? C42 C43 C44 120.1(8) . . ? C39 C44 C43 121.4(7) . . ? C50 C45 C46 117.8(6) . . ? C50 C45 P4 119.4(5) . . ? C46 C45 P4 122.6(5) . . ? C47 C46 C45 120.7(7) . . ? C48 C47 C46 120.3(7) . . ? C47 C48 C49 119.3(7) . . ? C50 C49 C48 121.1(8) . . ? C49 C50 C45 120.8(7) . . ? N3 C53 C54 113.9(7) . . ? N4 C54 C53 114.0(7) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.273 #(near Ga1) _refine_diff_density_min -0.477 _refine_diff_density_rms 0.130 data_compound3 _database_code_depnum_ccdc_archive 'CCDC 280911' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H79 Ga K N6 O' _chemical_formula_weight 901.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2/c 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 20.663(4) _cell_length_b 14.230(3) _cell_length_c 35.603(7) _cell_angle_alpha 90.00 _cell_angle_beta 101.76(3) _cell_angle_gamma 90.00 _cell_volume 10249(4) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.168 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3880 _exptl_absorpt_coefficient_mu 0.658 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.801 _exptl_absorpt_correction_T_max 0.949 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15119 _diffrn_reflns_av_R_equivalents 0.0700 _diffrn_reflns_av_sigmaI/netI 0.1139 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 25.03 _reflns_number_total 8869 _reflns_number_gt 5902 _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. During the course of refinement, a molecule of hexane, sitting on a crystallographic 2-fold axis, was located in the crystal lattice and found to be disordered over 2 sites. The disorder was successfully modelled and the atoms of the hexane molecule refined isotropically without including H-atoms in calculated positions. The amine H-atom, H(4), was located from difference maps and refined isotropically without restraints. ; _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^)+(0.0556P)^2^+46.7960P] 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 8869 _refine_ls_number_parameters 547 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.1293 _refine_ls_R_factor_gt 0.0797 _refine_ls_wR_factor_ref 0.1722 _refine_ls_wR_factor_gt 0.1526 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.045 _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 0.24761(3) 0.63055(4) 0.118680(14) 0.02162(18) Uani 1 1 d . . . K1 K 0.17975(7) 0.92701(10) 0.09873(4) 0.0557(4) Uani 1 1 d . . . O1 O 0.1133(2) 1.0227(3) 0.03548(12) 0.0576(12) Uani 1 1 d . . . N1 N 0.24359(19) 0.6384(3) 0.17171(10) 0.0260(9) Uani 1 1 d . . . N2 N 0.22800(19) 0.4998(3) 0.12103(10) 0.0260(10) Uani 1 1 d . . . N3 N 0.18065(19) 0.7078(3) 0.08546(11) 0.0274(10) Uani 1 1 d . . . N4 N 0.2078(2) 0.7662(3) 0.05937(12) 0.0297(10) Uani 1 1 d D . . N5 N 0.3044(3) 0.9988(4) 0.13036(16) 0.0610(15) Uani 1 1 d . . . N6 N 0.1857(4) 1.0938(4) 0.15260(18) 0.0718(19) Uani 1 1 d . . . C1 C 0.2280(2) 0.5497(4) 0.18378(14) 0.0285(12) Uani 1 1 d . . . H1 H 0.2230 0.5397 0.2094 0.034 Uiso 1 1 calc R . . C2 C 0.2201(2) 0.4787(4) 0.15854(13) 0.0280(12) Uani 1 1 d . . . H2 H 0.2097 0.4170 0.1656 0.034 Uiso 1 1 calc R . . C3 C 0.2673(2) 0.7074(3) 0.20014(13) 0.0250(11) Uani 1 1 d . . . C4 C 0.3355(3) 0.7195(4) 0.21335(14) 0.0323(13) Uani 1 1 d . . . C5 C 0.3571(3) 0.7883(4) 0.24106(15) 0.0423(15) Uani 1 1 d . . . H5 H 0.4031 0.7978 0.2501 0.051 Uiso 1 1 calc R . . C6 C 0.3125(3) 0.8428(4) 0.25553(16) 0.0469(16) Uani 1 1 d . . . H6 H 0.3280 0.8890 0.2745 0.056 Uiso 1 1 calc R . . C7 C 0.2457(3) 0.8301(4) 0.24245(15) 0.0437(15) Uani 1 1 d . . . H7 H 0.2154 0.8679 0.2525 0.052 Uiso 1 1 calc R . . C8 C 0.2218(3) 0.7628(4) 0.21465(14) 0.0307(12) Uani 1 1 d . . . C9 C 0.3860(3) 0.6569(4) 0.19994(15) 0.0373(14) Uani 1 1 d . . . H9 H 0.3639 0.6304 0.1745 0.045 Uiso 1 1 calc R . . C10 C 0.4472(3) 0.7088(5) 0.19361(16) 0.0475(16) Uani 1 1 d . . . H10A H 0.4339 0.7630 0.1768 0.071 Uiso 1 1 calc R . . H10B H 0.4744 0.6664 0.1816 0.071 Uiso 1 1 calc R . . H10C H 0.4729 0.7304 0.2183 0.071 Uiso 1 1 calc R . . C11 C 0.4049(3) 0.5729(4) 0.22724(17) 0.0481(16) Uani 1 1 d . . . H11A H 0.4345 0.5309 0.2168 0.072 Uiso 1 1 calc R . . H11B H 0.3649 0.5386 0.2298 0.072 Uiso 1 1 calc R . . H11C H 0.4275 0.5958 0.2525 0.072 Uiso 1 1 calc R . . C12 C 0.1483(3) 0.7505(4) 0.20005(15) 0.0410(15) Uani 1 1 d . . . H12 H 0.1427 0.6903 0.1852 0.049 Uiso 1 1 calc R . . C13 C 0.1096(5) 0.7402(8) 0.2306(3) 0.121(3) Uani 1 1 d U . . H13A H 0.0638 0.7243 0.2191 0.182 Uiso 1 1 calc R . . H13B H 0.1107 0.7995 0.2448 0.182 Uiso 1 1 calc R . . H13C H 0.1289 0.6901 0.2483 0.182 Uiso 1 1 calc R . . C14 C 0.1200(5) 0.8234(7) 0.1735(3) 0.117(3) Uani 1 1 d U . . H14A H 0.0745 0.8066 0.1615 0.176 Uiso 1 1 calc R . . H14B H 0.1463 0.8301 0.1536 0.176 Uiso 1 1 calc R . . H14C H 0.1201 0.8830 0.1873 0.176 Uiso 1 1 calc R . . C15 C 0.2401(2) 0.4238(3) 0.09745(13) 0.0251(11) Uani 1 1 d . . . C16 C 0.1895(3) 0.3957(4) 0.06626(14) 0.0312(13) Uani 1 1 d . . . C17 C 0.2019(3) 0.3205(4) 0.04360(15) 0.0387(14) Uani 1 1 d . . . H17 H 0.1688 0.3014 0.0224 0.046 Uiso 1 1 calc R . . C18 C 0.2612(3) 0.2736(4) 0.05139(15) 0.0427(15) Uani 1 1 d . . . H18 H 0.2685 0.2221 0.0358 0.051 Uiso 1 1 calc R . . C19 C 0.3103(3) 0.3008(4) 0.08186(16) 0.0395(14) Uani 1 1 d . . . H19 H 0.3512 0.2679 0.0870 0.047 Uiso 1 1 calc R . . C20 C 0.3003(2) 0.3766(4) 0.10528(14) 0.0306(12) Uani 1 1 d . . . C21 C 0.1236(3) 0.4451(4) 0.05748(15) 0.0367(13) Uani 1 1 d . . . H21 H 0.1232 0.4905 0.0789 0.044 Uiso 1 1 calc R . . C22 C 0.0655(3) 0.3788(5) 0.0565(2) 0.0625(19) Uani 1 1 d . . . H22A H 0.0630 0.3346 0.0351 0.094 Uiso 1 1 calc R . . H22B H 0.0245 0.4152 0.0530 0.094 Uiso 1 1 calc R . . H22C H 0.0717 0.3439 0.0807 0.094 Uiso 1 1 calc R . . C23 C 0.1148(3) 0.5018(5) 0.02107(19) 0.066(2) Uani 1 1 d . . . H23A H 0.1524 0.5444 0.0224 0.099 Uiso 1 1 calc R . . H23B H 0.0739 0.5384 0.0179 0.099 Uiso 1 1 calc R . . H23C H 0.1123 0.4593 -0.0009 0.099 Uiso 1 1 calc R . . C24 C 0.3571(2) 0.4058(4) 0.13774(15) 0.0365(13) Uani 1 1 d . . . H24 H 0.3430 0.4644 0.1494 0.044 Uiso 1 1 calc R . . C25 C 0.4192(3) 0.4292(5) 0.12314(19) 0.0555(18) Uani 1 1 d . . . H25A H 0.4368 0.3719 0.1137 0.083 Uiso 1 1 calc R . . H25B H 0.4523 0.4559 0.1441 0.083 Uiso 1 1 calc R . . H25C H 0.4086 0.4750 0.1022 0.083 Uiso 1 1 calc R . . C26 C 0.3717(3) 0.3326(5) 0.16937(17) 0.0551(18) Uani 1 1 d . . . H26A H 0.3871 0.2746 0.1592 0.083 Uiso 1 1 calc R . . H26B H 0.3314 0.3196 0.1790 0.083 Uiso 1 1 calc R . . H26C H 0.4060 0.3563 0.1904 0.083 Uiso 1 1 calc R . . C27 C 0.1128(2) 0.7071(4) 0.07931(13) 0.0274(12) Uani 1 1 d . . . C28 C 0.0706(2) 0.7589(4) 0.05061(15) 0.0323(13) Uani 1 1 d . . . H28 H 0.0890 0.8012 0.0350 0.039 Uiso 1 1 calc R . . C29 C 0.0025(3) 0.7487(4) 0.04496(17) 0.0442(15) Uani 1 1 d . . . H29 H -0.0251 0.7839 0.0253 0.053 Uiso 1 1 calc R . . C30 C -0.0258(3) 0.6886(4) 0.06725(18) 0.0459(16) Uani 1 1 d . . . H30 H -0.0723 0.6804 0.0627 0.055 Uiso 1 1 calc R . . C31 C 0.0153(3) 0.6404(4) 0.09647(16) 0.0421(14) Uani 1 1 d . . . H31 H -0.0038 0.6006 0.1127 0.051 Uiso 1 1 calc R . . C32 C 0.0827(2) 0.6486(4) 0.10270(14) 0.0316(13) Uani 1 1 d . . . H32 H 0.1095 0.6144 0.1230 0.038 Uiso 1 1 calc R . . C33 C 0.2770(2) 0.7506(3) 0.06301(13) 0.0249(11) Uani 1 1 d . . . C34 C 0.3093(3) 0.7996(4) 0.03831(14) 0.0347(13) Uani 1 1 d . . . H34 H 0.2851 0.8390 0.0189 0.042 Uiso 1 1 calc R . . C35 C 0.3769(3) 0.7901(4) 0.04253(16) 0.0406(14) Uani 1 1 d . . . H35 H 0.3993 0.8225 0.0256 0.049 Uiso 1 1 calc R . . C36 C 0.4123(3) 0.7335(4) 0.07125(15) 0.0360(13) Uani 1 1 d . . . H36 H 0.4590 0.7282 0.0746 0.043 Uiso 1 1 calc R . . C37 C 0.3788(2) 0.6851(4) 0.09481(14) 0.0290(12) Uani 1 1 d . . . H37 H 0.4032 0.6457 0.1141 0.035 Uiso 1 1 calc R . . C38 C 0.3105(2) 0.6913(3) 0.09162(13) 0.0244(11) Uani 1 1 d . . . C39 C 0.3281(4) 0.9164(5) 0.1538(2) 0.090(3) Uani 1 1 d . . . H39A H 0.3697 0.9319 0.1715 0.135 Uiso 1 1 calc R . . H39B H 0.3355 0.8645 0.1371 0.135 Uiso 1 1 calc R . . H39C H 0.2950 0.8978 0.1686 0.135 Uiso 1 1 calc R . . C40 C 0.3457(4) 1.0143(6) 0.1021(3) 0.099(3) Uani 1 1 d . . . H40A H 0.3278 1.0670 0.0854 0.149 Uiso 1 1 calc R . . H40B H 0.3459 0.9575 0.0866 0.149 Uiso 1 1 calc R . . H40C H 0.3909 1.0290 0.1153 0.149 Uiso 1 1 calc R . . C41 C 0.3054(5) 1.0826(6) 0.1537(3) 0.098(3) Uani 1 1 d . . . H41A H 0.3484 1.0848 0.1721 0.118 Uiso 1 1 calc R . . H41B H 0.3036 1.1380 0.1367 0.118 Uiso 1 1 calc R . . C42 C 0.2533(7) 1.0920(7) 0.1752(3) 0.117(4) Uani 1 1 d . . . H42A H 0.2610 1.1508 0.1904 0.141 Uiso 1 1 calc R . . H42B H 0.2571 1.0392 0.1936 0.141 Uiso 1 1 calc R . . C43 C 0.1734(5) 1.1760(6) 0.1291(3) 0.098(3) Uani 1 1 d . . . H43A H 0.1884 1.2317 0.1446 0.146 Uiso 1 1 calc R . . H43B H 0.1259 1.1812 0.1184 0.146 Uiso 1 1 calc R . . H43C H 0.1975 1.1713 0.1081 0.146 Uiso 1 1 calc R . . C44 C 0.1432(5) 1.0945(7) 0.1806(3) 0.114(3) Uani 1 1 d U . . H44A H 0.1491 1.1537 0.1950 0.171 Uiso 1 1 calc R . . H44B H 0.1549 1.0418 0.1984 0.171 Uiso 1 1 calc R . . H44C H 0.0969 1.0885 0.1673 0.171 Uiso 1 1 calc R . . C45 C 0.0309(4) 1.0280(5) 0.0723(3) 0.088(3) Uani 1 1 d . . . H45A H 0.0270 0.9599 0.0682 0.131 Uiso 1 1 calc R . . H45B H -0.0126 1.0543 0.0730 0.131 Uiso 1 1 calc R . . H45C H 0.0614 1.0409 0.0966 0.131 Uiso 1 1 calc R . . C46 C 0.0569(4) 1.0723(5) 0.0400(2) 0.071(2) Uani 1 1 d . . . H46A H 0.0228 1.0696 0.0160 0.086 Uiso 1 1 calc R . . H46B H 0.0681 1.1390 0.0460 0.086 Uiso 1 1 calc R . . C47 C 0.1365(3) 1.0583(5) 0.0025(2) 0.0633(19) Uani 1 1 d . . . H47A H 0.1535 1.1232 0.0076 0.076 Uiso 1 1 calc R . . H47B H 0.0998 1.0597 -0.0202 0.076 Uiso 1 1 calc R . . C48 C 0.1895(3) 0.9964(5) -0.0048(2) 0.067(2) Uani 1 1 d . . . H48A H 0.2253 0.9946 0.0180 0.101 Uiso 1 1 calc R . . H48B H 0.2066 1.0205 -0.0267 0.101 Uiso 1 1 calc R . . H48C H 0.1720 0.9329 -0.0106 0.101 Uiso 1 1 calc R . . C49 C 0.5000 1.0257(10) 0.2500 0.110(4) Uiso 1 2 d SD . . C50 C 0.4891(3) 0.9614(5) 0.2799(2) 0.0649(19) Uiso 1 1 d D . . C51 C 0.4606(7) 0.9898(11) 0.3098(4) 0.187(6) Uiso 1 1 d D . . C52 C 0.4612(7) 0.9111(11) 0.3402(4) 0.069(4) Uiso 0.50 1 d PD . . H4 H 0.188(2) 0.752(3) 0.0353(7) 0.027(14) Uiso 1 1 d 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 Ga1 0.0269(3) 0.0186(3) 0.0196(3) 0.0015(3) 0.0051(2) -0.0009(3) K1 0.0606(9) 0.0426(9) 0.0673(10) -0.0174(7) 0.0208(7) -0.0065(7) O1 0.067(3) 0.041(3) 0.076(3) -0.002(2) 0.044(2) -0.001(2) N1 0.037(2) 0.021(2) 0.020(2) -0.0029(19) 0.0074(17) -0.004(2) N2 0.036(2) 0.020(2) 0.023(2) 0.0003(19) 0.0085(17) -0.0044(19) N3 0.029(2) 0.026(2) 0.028(2) 0.0074(19) 0.0089(18) 0.0017(19) N4 0.036(3) 0.029(3) 0.023(2) 0.008(2) 0.0057(19) 0.001(2) N5 0.070(4) 0.031(3) 0.076(4) -0.001(3) 0.001(3) -0.010(3) N6 0.125(6) 0.040(4) 0.065(4) -0.010(3) 0.053(4) -0.011(4) C1 0.041(3) 0.025(3) 0.022(3) 0.006(2) 0.011(2) -0.002(2) C2 0.039(3) 0.021(3) 0.026(3) 0.003(2) 0.011(2) -0.005(2) C3 0.040(3) 0.019(3) 0.017(2) -0.001(2) 0.008(2) -0.004(2) C4 0.041(3) 0.028(3) 0.027(3) -0.001(2) 0.005(2) 0.001(3) C5 0.040(3) 0.049(4) 0.035(3) -0.017(3) 0.000(3) -0.006(3) C6 0.064(4) 0.039(4) 0.037(3) -0.021(3) 0.008(3) -0.014(3) C7 0.055(4) 0.042(4) 0.038(3) -0.014(3) 0.017(3) 0.003(3) C8 0.039(3) 0.025(3) 0.029(3) -0.001(2) 0.008(2) 0.002(2) C9 0.037(3) 0.039(4) 0.032(3) -0.009(3) -0.003(2) 0.003(3) C10 0.041(4) 0.059(4) 0.039(3) -0.006(3) 0.001(3) 0.004(3) C11 0.043(4) 0.045(4) 0.053(4) -0.003(3) 0.003(3) 0.003(3) C12 0.051(4) 0.043(4) 0.028(3) -0.010(3) 0.008(3) 0.008(3) C13 0.108(5) 0.149(6) 0.110(5) 0.003(4) 0.029(4) -0.027(4) C14 0.102(5) 0.106(5) 0.133(5) 0.024(4) -0.002(4) -0.011(4) C15 0.038(3) 0.021(3) 0.020(2) -0.002(2) 0.014(2) -0.005(2) C16 0.048(3) 0.023(3) 0.024(3) 0.004(2) 0.009(2) -0.006(2) C17 0.054(4) 0.031(3) 0.031(3) -0.005(3) 0.008(3) -0.005(3) C18 0.071(4) 0.029(3) 0.032(3) -0.009(3) 0.020(3) 0.001(3) C19 0.051(4) 0.030(3) 0.043(3) 0.005(3) 0.022(3) 0.006(3) C20 0.038(3) 0.025(3) 0.031(3) -0.004(3) 0.011(2) -0.006(3) C21 0.047(4) 0.029(3) 0.031(3) -0.002(3) 0.002(2) -0.005(3) C22 0.051(4) 0.053(5) 0.082(5) 0.008(4) 0.010(3) -0.005(4) C23 0.066(5) 0.059(5) 0.070(5) 0.029(4) 0.007(4) 0.007(4) C24 0.034(3) 0.030(3) 0.045(3) 0.000(3) 0.007(3) 0.005(2) C25 0.043(4) 0.052(4) 0.074(5) -0.006(4) 0.019(3) 0.003(3) C26 0.059(4) 0.051(4) 0.047(4) 0.008(3) -0.008(3) -0.008(3) C27 0.028(3) 0.028(3) 0.027(3) -0.006(2) 0.008(2) 0.000(2) C28 0.033(3) 0.022(3) 0.041(3) -0.003(3) 0.003(2) 0.007(2) C29 0.036(4) 0.036(4) 0.055(4) -0.004(3) -0.005(3) 0.015(3) C30 0.027(3) 0.040(4) 0.070(4) -0.011(3) 0.008(3) 0.002(3) C31 0.042(3) 0.035(4) 0.053(4) -0.007(3) 0.019(3) 0.002(3) C32 0.030(3) 0.031(3) 0.036(3) 0.000(2) 0.011(2) 0.003(2) C33 0.028(3) 0.021(3) 0.027(3) 0.002(2) 0.008(2) -0.002(2) C34 0.047(4) 0.029(3) 0.032(3) 0.015(3) 0.016(2) 0.004(3) C35 0.049(4) 0.036(4) 0.043(3) 0.003(3) 0.026(3) -0.008(3) C36 0.030(3) 0.037(3) 0.044(3) 0.006(3) 0.013(2) -0.003(3) C37 0.027(3) 0.027(3) 0.032(3) 0.005(2) 0.004(2) 0.002(2) C38 0.028(3) 0.022(3) 0.026(3) -0.001(2) 0.012(2) -0.003(2) C39 0.115(7) 0.040(5) 0.094(6) 0.008(4) -0.028(5) -0.002(4) C40 0.078(6) 0.082(7) 0.137(8) -0.003(6) 0.021(6) -0.034(5) C41 0.109(7) 0.042(5) 0.117(8) -0.022(5) -0.040(6) -0.013(5) C42 0.199(13) 0.075(7) 0.075(7) -0.029(5) 0.020(8) -0.017(8) C43 0.139(8) 0.057(6) 0.098(7) 0.011(5) 0.026(6) -0.018(5) C44 0.138(5) 0.105(5) 0.112(5) -0.012(4) 0.055(4) -0.008(4) C45 0.086(6) 0.049(5) 0.149(8) 0.005(5) 0.074(6) 0.007(4) C46 0.073(5) 0.039(4) 0.109(6) 0.006(4) 0.037(5) 0.005(4) C47 0.073(5) 0.045(4) 0.076(5) 0.009(4) 0.027(4) -0.006(4) C48 0.081(5) 0.051(5) 0.080(5) 0.026(4) 0.040(4) 0.013(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 1.910(4) . ? Ga1 N2 1.910(4) . ? Ga1 N3 1.964(4) . ? Ga1 C38 1.969(5) . ? K1 O1 2.748(5) . ? K1 N5 2.786(6) . ? K1 N4 2.804(5) . ? K1 N6 3.038(6) . ? K1 N3 3.155(4) . ? K1 C27 3.435(5) . ? K1 C28 3.488(5) . ? O1 C46 1.401(7) . ? O1 C47 1.447(7) . ? N1 C1 1.392(6) . ? N1 C3 1.424(6) . ? N2 C2 1.410(6) . ? N2 C15 1.421(6) . ? N3 C27 1.374(6) . ? N3 N4 1.442(5) . ? N4 C33 1.427(6) . ? N5 C41 1.451(9) . ? N5 C40 1.463(9) . ? N5 C39 1.465(8) . ? N6 C43 1.430(9) . ? N6 C44 1.458(9) . ? N6 C42 1.464(12) . ? C1 C2 1.339(7) . ? C3 C4 1.402(7) . ? C3 C8 1.404(7) . ? C4 C5 1.397(7) . ? C4 C9 1.520(7) . ? C5 C6 1.380(8) . ? C6 C7 1.376(8) . ? C7 C8 1.394(7) . ? C8 C12 1.512(7) . ? C9 C10 1.522(8) . ? C9 C11 1.539(8) . ? C12 C14 1.446(10) . ? C12 C13 1.483(10) . ? C15 C20 1.392(7) . ? C15 C16 1.418(7) . ? C16 C17 1.395(7) . ? C16 C21 1.508(7) . ? C17 C18 1.372(8) . ? C18 C19 1.381(8) . ? C19 C20 1.404(7) . ? C20 C24 1.527(7) . ? C21 C23 1.506(8) . ? C21 C22 1.521(8) . ? C24 C25 1.517(8) . ? C24 C26 1.519(8) . ? C27 C32 1.408(7) . ? C27 C28 1.409(7) . ? C28 C29 1.388(7) . ? C29 C30 1.375(8) . ? C30 C31 1.383(8) . ? C31 C32 1.370(7) . ? C33 C38 1.394(7) . ? C33 C34 1.394(6) . ? C34 C35 1.382(7) . ? C35 C36 1.387(7) . ? C36 C37 1.377(7) . ? C37 C38 1.395(6) . ? C41 C42 1.448(12) . ? C45 C46 1.502(9) . ? C47 C48 1.469(9) . ? C49 C50 1.454(10) . ? C49 C50 1.454(10) 2_655 ? C50 C51 1.379(12) . ? C51 C52 1.556(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ga1 N2 87.78(17) . . ? N1 Ga1 N3 113.29(17) . . ? N2 Ga1 N3 116.25(17) . . ? N1 Ga1 C38 128.62(18) . . ? N2 Ga1 C38 128.06(18) . . ? N3 Ga1 C38 85.05(18) . . ? O1 K1 N5 114.56(16) . . ? O1 K1 N4 96.56(13) . . ? N5 K1 N4 103.50(15) . . ? O1 K1 N6 94.55(17) . . ? N5 K1 N6 62.82(19) . . ? N4 K1 N6 165.23(19) . . ? O1 K1 N3 112.60(12) . . ? N5 K1 N3 112.96(14) . . ? N4 K1 N3 27.19(11) . . ? N6 K1 N3 150.00(15) . . ? O1 K1 C27 99.97(13) . . ? N5 K1 C27 135.80(15) . . ? N4 K1 C27 43.25(12) . . ? N6 K1 C27 143.29(14) . . ? N3 K1 C27 23.59(10) . . ? O1 K1 C28 76.84(13) . . ? N5 K1 C28 154.40(15) . . ? N4 K1 C28 51.21(12) . . ? N6 K1 C28 141.69(17) . . ? N3 K1 C28 43.23(11) . . ? C27 K1 C28 23.46(11) . . ? C46 O1 C47 109.8(5) . . ? C46 O1 K1 116.4(4) . . ? C47 O1 K1 130.2(4) . . ? C1 N1 C3 118.3(4) . . ? C1 N1 Ga1 108.2(3) . . ? C3 N1 Ga1 131.7(3) . . ? C2 N2 C15 117.8(4) . . ? C2 N2 Ga1 108.3(3) . . ? C15 N2 Ga1 130.6(3) . . ? C27 N3 N4 114.8(4) . . ? C27 N3 Ga1 131.5(3) . . ? N4 N3 Ga1 113.1(3) . . ? C27 N3 K1 89.7(3) . . ? N4 N3 K1 62.7(2) . . ? Ga1 N3 K1 119.23(17) . . ? C33 N4 N3 111.5(4) . . ? C33 N4 K1 112.7(3) . . ? N3 N4 K1 90.1(3) . . ? C41 N5 C40 109.1(7) . . ? C41 N5 C39 111.6(6) . . ? C40 N5 C39 109.8(7) . . ? C41 N5 K1 115.9(5) . . ? C40 N5 K1 113.4(4) . . ? C39 N5 K1 96.4(4) . . ? C43 N6 C44 109.6(7) . . ? C43 N6 C42 111.8(7) . . ? C44 N6 C42 105.4(8) . . ? C43 N6 K1 106.8(5) . . ? C44 N6 K1 119.0(5) . . ? C42 N6 K1 104.1(5) . . ? C2 C1 N1 118.7(4) . . ? C1 C2 N2 117.0(4) . . ? C4 C3 C8 120.7(4) . . ? C4 C3 N1 120.0(4) . . ? C8 C3 N1 119.3(4) . . ? C5 C4 C3 118.4(5) . . ? C5 C4 C9 119.5(5) . . ? C3 C4 C9 122.0(4) . . ? C6 C5 C4 121.1(5) . . ? C7 C6 C5 119.9(5) . . ? C6 C7 C8 121.2(5) . . ? C7 C8 C3 118.7(5) . . ? C7 C8 C12 120.7(5) . . ? C3 C8 C12 120.6(5) . . ? C4 C9 C10 114.0(5) . . ? C4 C9 C11 111.1(4) . . ? C10 C9 C11 111.0(5) . . ? C14 C12 C13 110.2(7) . . ? C14 C12 C8 112.7(6) . . ? C13 C12 C8 114.4(5) . . ? C20 C15 C16 120.4(4) . . ? C20 C15 N2 120.4(4) . . ? C16 C15 N2 119.2(4) . . ? C17 C16 C15 118.5(5) . . ? C17 C16 C21 120.2(5) . . ? C15 C16 C21 121.3(5) . . ? C18 C17 C16 121.2(5) . . ? C17 C18 C19 120.3(5) . . ? C18 C19 C20 120.6(5) . . ? C15 C20 C19 119.0(5) . . ? C15 C20 C24 122.6(5) . . ? C19 C20 C24 118.4(5) . . ? C23 C21 C16 112.0(5) . . ? C23 C21 C22 110.8(5) . . ? C16 C21 C22 113.0(5) . . ? C25 C24 C26 110.5(5) . . ? C25 C24 C20 111.9(5) . . ? C26 C24 C20 112.4(5) . . ? N3 C27 C32 118.0(4) . . ? N3 C27 C28 124.8(5) . . ? C32 C27 C28 117.1(5) . . ? N3 C27 K1 66.7(3) . . ? C32 C27 K1 128.9(3) . . ? C28 C27 K1 80.4(3) . . ? C29 C28 C27 120.6(5) . . ? C29 C28 K1 132.7(4) . . ? C27 C28 K1 76.1(3) . . ? C30 C29 C28 121.2(5) . . ? C29 C30 C31 118.4(5) . . ? C32 C31 C30 121.8(6) . . ? C31 C32 C27 120.7(5) . . ? C38 C33 C34 122.2(5) . . ? C38 C33 N4 120.0(4) . . ? C34 C33 N4 117.7(4) . . ? C35 C34 C33 119.1(5) . . ? C34 C35 C36 120.5(5) . . ? C37 C36 C35 118.9(5) . . ? C36 C37 C38 123.1(5) . . ? C33 C38 C37 116.2(4) . . ? C33 C38 Ga1 110.1(3) . . ? C37 C38 Ga1 133.6(4) . . ? C42 C41 N5 116.9(8) . . ? C41 C42 N6 116.1(8) . . ? O1 C46 C45 108.2(6) . . ? O1 C47 C48 108.4(5) . . ? C50 C49 C50 102.1(11) . 2_655 ? C51 C50 C49 122.3(9) . . ? C50 C51 C52 112.5(12) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.798 _refine_diff_density_min -0.439 _refine_diff_density_rms 0.078 data_compound5 _database_code_depnum_ccdc_archive 'CCDC 280912' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H90 Ga2 N6 Si2' _chemical_formula_weight 1066.98 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.592(3) _cell_length_b 21.742(4) _cell_length_c 17.818(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.34(3) _cell_angle_gamma 90.00 _cell_volume 5901(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue-green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.201 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2280 _exptl_absorpt_coefficient_mu 0.994 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.838 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47327 _diffrn_reflns_av_R_equivalents 0.0837 _diffrn_reflns_av_sigmaI/netI 0.0762 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 25.04 _reflns_number_total 10395 _reflns_number_gt 7409 _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^)+(0.0395P)^2^+3.6071P] 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 'calculated (riding model)' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00171(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10395 _refine_ls_number_parameters 636 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0856 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1128 _refine_ls_wR_factor_gt 0.1022 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.002 _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 0.31081(2) 0.472087(15) 0.80555(2) 0.01975(11) Uani 1 1 d . . . Ga2 Ga 0.18654(2) 0.525065(15) 0.70034(2) 0.02051(12) Uani 1 1 d . . . Si1 Si 0.19551(6) 0.37411(4) 0.68192(6) 0.0276(2) Uani 1 1 d . . . Si2 Si 0.26976(6) 0.61527(4) 0.84917(6) 0.0281(2) Uani 1 1 d . . . N1 N 0.23242(16) 0.44435(11) 0.71748(15) 0.0218(6) Uani 1 1 d . . . N2 N 0.26152(16) 0.55226(11) 0.79102(15) 0.0223(6) Uani 1 1 d . . . N3 N 0.44293(16) 0.47119(11) 0.82307(16) 0.0216(6) Uani 1 1 d . . . N4 N 0.33215(16) 0.42768(11) 0.90689(15) 0.0222(6) Uani 1 1 d . . . N5 N 0.05704(16) 0.54139(11) 0.67375(16) 0.0229(6) Uani 1 1 d . . . N6 N 0.18167(16) 0.55527(12) 0.59168(16) 0.0242(6) Uani 1 1 d . . . C1 C 0.4744(2) 0.45563(13) 0.8959(2) 0.0234(8) Uani 1 1 d . . . H1 H 0.5351 0.4604 0.9181 0.028 Uiso 1 1 calc R . . C2 C 0.4175(2) 0.43231(14) 0.93942(19) 0.0233(8) Uani 1 1 d . . . H2 H 0.4389 0.4199 0.9912 0.028 Uiso 1 1 calc R . . C3 C 0.5084(2) 0.47752(14) 0.77654(19) 0.0243(8) Uani 1 1 d . . . C4 C 0.5320(2) 0.53513(15) 0.7526(2) 0.0284(8) Uani 1 1 d . . . C5 C 0.6020(2) 0.53812(17) 0.7152(2) 0.0376(9) Uani 1 1 d . . . H5 H 0.6188 0.5770 0.6988 0.045 Uiso 1 1 calc R . . C6 C 0.6472(2) 0.48655(18) 0.7015(2) 0.0419(10) Uani 1 1 d . . . H6 H 0.6960 0.4900 0.6776 0.050 Uiso 1 1 calc R . . C7 C 0.6210(2) 0.42990(17) 0.7227(2) 0.0362(9) Uani 1 1 d . . . H7 H 0.6513 0.3941 0.7121 0.043 Uiso 1 1 calc R . . C8 C 0.5511(2) 0.42362(15) 0.7596(2) 0.0279(8) Uani 1 1 d . . . C9 C 0.4872(2) 0.59453(14) 0.7673(2) 0.0314(9) Uani 1 1 d . . . H9 H 0.4358 0.5840 0.7903 0.038 Uiso 1 1 calc R . . C10 C 0.5504(3) 0.63482(16) 0.8248(2) 0.0432(10) Uani 1 1 d . . . H10A H 0.5756 0.6105 0.8706 0.065 Uiso 1 1 calc R . . H10B H 0.5183 0.6700 0.8396 0.065 Uiso 1 1 calc R . . H10C H 0.5976 0.6497 0.8010 0.065 Uiso 1 1 calc R . . C11 C 0.4534(2) 0.62974(16) 0.6926(2) 0.0419(10) Uani 1 1 d . . . H11A H 0.5026 0.6389 0.6681 0.063 Uiso 1 1 calc R . . H11B H 0.4261 0.6683 0.7039 0.063 Uiso 1 1 calc R . . H11C H 0.4100 0.6046 0.6579 0.063 Uiso 1 1 calc R . . C12 C 0.5247(2) 0.35902(15) 0.7787(2) 0.0325(9) Uani 1 1 d . . . H12 H 0.4650 0.3614 0.7908 0.039 Uiso 1 1 calc R . . C13 C 0.5882(3) 0.33356(17) 0.8495(2) 0.0476(11) Uani 1 1 d . . . H13A H 0.6480 0.3334 0.8402 0.071 Uiso 1 1 calc R . . H13B H 0.5711 0.2915 0.8594 0.071 Uiso 1 1 calc R . . H13C H 0.5863 0.3595 0.8941 0.071 Uiso 1 1 calc R . . C14 C 0.5199(2) 0.31433(16) 0.7118(2) 0.0405(10) Uani 1 1 d . . . H14A H 0.4851 0.3327 0.6648 0.061 Uiso 1 1 calc R . . H14B H 0.4922 0.2759 0.7230 0.061 Uiso 1 1 calc R . . H14C H 0.5794 0.3057 0.7047 0.061 Uiso 1 1 calc R . . C15 C 0.2793(2) 0.38637(14) 0.94208(19) 0.0256(8) Uani 1 1 d . . . C16 C 0.2971(2) 0.32226(15) 0.9432(2) 0.0307(8) Uani 1 1 d . . . C17 C 0.2439(2) 0.28399(16) 0.9765(2) 0.0387(9) Uani 1 1 d . . . H17 H 0.2554 0.2410 0.9787 0.046 Uiso 1 1 calc R . . C18 C 0.1762(3) 0.30581(17) 1.0061(2) 0.0429(10) Uani 1 1 d . . . H18 H 0.1400 0.2782 1.0267 0.051 Uiso 1 1 calc R . . C19 C 0.1604(2) 0.36849(17) 1.0059(2) 0.0397(10) Uani 1 1 d . . . H19 H 0.1134 0.3836 1.0270 0.048 Uiso 1 1 calc R . . C20 C 0.2120(2) 0.40981(15) 0.9754(2) 0.0283(8) Uani 1 1 d . . . C21 C 0.3711(2) 0.29322(15) 0.9122(2) 0.0358(9) Uani 1 1 d . . . H21 H 0.3969 0.3256 0.8838 0.043 Uiso 1 1 calc R . . C22 C 0.3401(3) 0.23990(17) 0.8563(3) 0.0535(12) Uani 1 1 d . . . H22A H 0.3195 0.2059 0.8841 0.080 Uiso 1 1 calc R . . H22B H 0.3890 0.2257 0.8342 0.080 Uiso 1 1 calc R . . H22C H 0.2920 0.2540 0.8151 0.080 Uiso 1 1 calc R . . C23 C 0.4434(3) 0.27023(18) 0.9782(3) 0.0506(11) Uani 1 1 d . . . H23A H 0.4185 0.2408 1.0094 0.076 Uiso 1 1 calc R . . H23B H 0.4686 0.3051 1.0103 0.076 Uiso 1 1 calc R . . H23C H 0.4894 0.2500 0.9573 0.076 Uiso 1 1 calc R . . C24 C 0.2029(2) 0.47874(15) 0.9862(2) 0.0317(9) Uani 1 1 d . . . H24 H 0.2163 0.5002 0.9403 0.038 Uiso 1 1 calc R . . C25 C 0.2711(2) 0.49868(17) 1.0572(2) 0.0399(10) Uani 1 1 d . . . H25A H 0.2590 0.4781 1.1028 0.060 Uiso 1 1 calc R . . H25B H 0.2679 0.5433 1.0636 0.060 Uiso 1 1 calc R . . H25C H 0.3299 0.4874 1.0507 0.060 Uiso 1 1 calc R . . C26 C 0.1111(2) 0.49845(19) 0.9948(3) 0.0496(11) Uani 1 1 d . . . H26A H 0.0678 0.4864 0.9488 0.074 Uiso 1 1 calc R . . H26B H 0.1098 0.5432 1.0012 0.074 Uiso 1 1 calc R . . H26C H 0.0972 0.4783 1.0400 0.074 Uiso 1 1 calc R . . C27 C 0.0324(2) 0.54962(14) 0.5982(2) 0.0252(8) Uani 1 1 d . . . H27 H -0.0280 0.5509 0.5738 0.030 Uiso 1 1 calc R . . C28 C 0.0978(2) 0.55644(14) 0.5553(2) 0.0255(8) Uani 1 1 d . . . H28 H 0.0823 0.5618 0.5012 0.031 Uiso 1 1 calc R . . C29 C -0.0073(2) 0.55707(15) 0.7184(2) 0.0257(8) Uani 1 1 d . . . C30 C -0.0525(2) 0.51119(15) 0.7502(2) 0.0308(8) Uani 1 1 d . . . C31 C -0.1183(2) 0.52958(17) 0.7866(2) 0.0428(10) Uani 1 1 d . . . H31 H -0.1499 0.4992 0.8078 0.051 Uiso 1 1 calc R . . C32 C -0.1393(3) 0.59075(18) 0.7930(3) 0.0497(11) Uani 1 1 d . . . H32 H -0.1850 0.6022 0.8179 0.060 Uiso 1 1 calc R . . C33 C -0.0938(2) 0.63438(17) 0.7634(2) 0.0461(11) Uani 1 1 d . . . H33 H -0.1079 0.6764 0.7688 0.055 Uiso 1 1 calc R . . C34 C -0.0274(2) 0.61981(16) 0.7253(2) 0.0349(9) Uani 1 1 d . . . C35 C -0.0350(2) 0.44288(15) 0.7415(2) 0.0340(9) Uani 1 1 d . . . H35 H 0.0230 0.4384 0.7266 0.041 Uiso 1 1 calc R . . C36 C -0.1048(3) 0.4162(2) 0.6782(3) 0.0696(15) Uani 1 1 d . . . H36A H -0.0904 0.3733 0.6693 0.104 Uiso 1 1 calc R . . H36B H -0.1078 0.4400 0.6310 0.104 Uiso 1 1 calc R . . H36C H -0.1617 0.4179 0.6931 0.104 Uiso 1 1 calc R . . C37 C -0.0309(4) 0.40791(19) 0.8157(3) 0.0753(16) Uani 1 1 d . . . H37A H 0.0161 0.4249 0.8558 0.113 Uiso 1 1 calc R . . H37B H -0.0190 0.3644 0.8078 0.113 Uiso 1 1 calc R . . H37C H -0.0871 0.4118 0.8314 0.113 Uiso 1 1 calc R . . C38 C 0.0187(2) 0.67149(15) 0.6921(2) 0.0402(10) Uani 1 1 d . . . H38 H 0.0717 0.6538 0.6768 0.048 Uiso 1 1 calc R . . C39 C 0.0490(2) 0.72360(16) 0.7486(3) 0.0504(12) Uani 1 1 d . . . H39A H -0.0023 0.7445 0.7602 0.076 Uiso 1 1 calc R . . H39B H 0.0838 0.7530 0.7259 0.076 Uiso 1 1 calc R . . H39C H 0.0850 0.7068 0.7961 0.076 Uiso 1 1 calc R . . C40 C -0.0412(3) 0.69743(18) 0.6204(3) 0.0600(13) Uani 1 1 d . . . H40A H -0.0549 0.6651 0.5813 0.090 Uiso 1 1 calc R . . H40B H -0.0116 0.7316 0.6005 0.090 Uiso 1 1 calc R . . H40C H -0.0957 0.7123 0.6332 0.090 Uiso 1 1 calc R . . C41 C 0.2449(2) 0.57925(15) 0.54980(19) 0.0272(8) Uani 1 1 d . . . C42 C 0.2424(2) 0.64277(16) 0.5323(2) 0.0329(9) Uani 1 1 d . . . C43 C 0.3042(3) 0.66514(18) 0.4929(2) 0.0447(10) Uani 1 1 d . . . H43 H 0.3035 0.7076 0.4804 0.054 Uiso 1 1 calc R . . C44 C 0.3655(3) 0.6283(2) 0.4718(3) 0.0548(12) Uani 1 1 d . . . H44 H 0.4073 0.6450 0.4458 0.066 Uiso 1 1 calc R . . C45 C 0.3664(2) 0.56606(19) 0.4887(2) 0.0431(10) Uani 1 1 d . . . H45 H 0.4083 0.5402 0.4729 0.052 Uiso 1 1 calc R . . C46 C 0.3068(2) 0.54055(16) 0.5284(2) 0.0325(9) Uani 1 1 d . . . C47 C 0.1755(2) 0.68775(15) 0.5517(2) 0.0367(9) Uani 1 1 d . . . H47 H 0.1436 0.6668 0.5875 0.044 Uiso 1 1 calc R . . C48 C 0.2191(3) 0.74614(17) 0.5917(2) 0.0486(11) Uani 1 1 d . . . H48A H 0.2661 0.7344 0.6353 0.073 Uiso 1 1 calc R . . H48B H 0.1751 0.7706 0.6103 0.073 Uiso 1 1 calc R . . H48C H 0.2438 0.7705 0.5552 0.073 Uiso 1 1 calc R . . C49 C 0.1082(3) 0.70641(17) 0.4798(3) 0.0498(11) Uani 1 1 d . . . H49A H 0.1383 0.7258 0.4430 0.075 Uiso 1 1 calc R . . H49B H 0.0663 0.7355 0.4938 0.075 Uiso 1 1 calc R . . H49C H 0.0767 0.6698 0.4564 0.075 Uiso 1 1 calc R . . C50 C 0.3072(2) 0.47101(16) 0.5407(2) 0.0347(9) Uani 1 1 d . . . H50 H 0.2773 0.4621 0.5839 0.042 Uiso 1 1 calc R . . C51 C 0.4003(3) 0.4450(2) 0.5619(3) 0.0640(14) Uani 1 1 d . . . H51A H 0.4289 0.4499 0.5183 0.096 Uiso 1 1 calc R . . H51B H 0.3977 0.4012 0.5743 0.096 Uiso 1 1 calc R . . H51C H 0.4339 0.4671 0.6065 0.096 Uiso 1 1 calc R . . C52 C 0.2553(3) 0.43966(19) 0.4683(2) 0.0542(12) Uani 1 1 d . . . H52A H 0.1968 0.4583 0.4539 0.081 Uiso 1 1 calc R . . H52B H 0.2494 0.3957 0.4784 0.081 Uiso 1 1 calc R . . H52C H 0.2862 0.4449 0.4263 0.081 Uiso 1 1 calc R . . C53 C 0.2846(2) 0.32442(16) 0.6592(2) 0.0397(10) Uani 1 1 d . . . H53A H 0.3059 0.3422 0.6160 0.060 Uiso 1 1 calc R . . H53B H 0.2615 0.2831 0.6455 0.060 Uiso 1 1 calc R . . H53C H 0.3332 0.3220 0.7042 0.060 Uiso 1 1 calc R . . C54 C 0.1437(2) 0.32790(15) 0.7493(3) 0.0445(11) Uani 1 1 d . . . H54A H 0.1795 0.3312 0.8015 0.067 Uiso 1 1 calc R . . H54B H 0.1400 0.2847 0.7333 0.067 Uiso 1 1 calc R . . H54C H 0.0846 0.3437 0.7484 0.067 Uiso 1 1 calc R . . C55 C 0.1095(2) 0.38439(17) 0.5916(2) 0.0413(10) Uani 1 1 d . . . H55A H 0.0591 0.4063 0.6034 0.062 Uiso 1 1 calc R . . H55B H 0.0905 0.3440 0.5698 0.062 Uiso 1 1 calc R . . H55C H 0.1339 0.4082 0.5544 0.062 Uiso 1 1 calc R . . C56 C 0.3680(2) 0.60716(16) 0.9299(2) 0.0408(10) Uani 1 1 d . . . H56A H 0.3609 0.5708 0.9606 0.061 Uiso 1 1 calc R . . H56B H 0.3736 0.6439 0.9624 0.061 Uiso 1 1 calc R . . H56C H 0.4208 0.6025 0.9089 0.061 Uiso 1 1 calc R . . C57 C 0.2828(3) 0.68826(15) 0.7971(2) 0.0428(10) Uani 1 1 d . . . H57A H 0.3396 0.6880 0.7818 0.064 Uiso 1 1 calc R . . H57B H 0.2804 0.7234 0.8310 0.064 Uiso 1 1 calc R . . H57C H 0.2354 0.6916 0.7513 0.064 Uiso 1 1 calc R . . C58 C 0.1746(3) 0.62661(16) 0.8960(2) 0.0453(11) Uani 1 1 d . . . H58A H 0.1202 0.6153 0.8600 0.068 Uiso 1 1 calc R . . H58B H 0.1717 0.6698 0.9108 0.068 Uiso 1 1 calc R . . H58C H 0.1820 0.6006 0.9419 0.068 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 0.01847(19) 0.01634(19) 0.0232(2) 0.00061(16) 0.00162(16) 0.00095(14) Ga2 0.01784(19) 0.01819(19) 0.0239(2) 0.00101(16) 0.00088(16) 0.00046(15) Si1 0.0235(5) 0.0192(5) 0.0367(6) -0.0029(4) -0.0012(4) -0.0006(4) Si2 0.0334(5) 0.0185(5) 0.0299(6) -0.0029(4) 0.0010(4) 0.0032(4) N1 0.0223(14) 0.0165(13) 0.0243(17) 0.0015(12) 0.0000(12) 0.0020(11) N2 0.0220(14) 0.0181(13) 0.0241(17) 0.0004(12) -0.0011(12) 0.0063(11) N3 0.0187(13) 0.0170(13) 0.0271(18) 0.0003(12) 0.0005(12) 0.0015(11) N4 0.0238(14) 0.0220(14) 0.0210(16) 0.0027(12) 0.0053(12) 0.0033(12) N5 0.0193(14) 0.0206(14) 0.0279(18) 0.0013(12) 0.0028(13) 0.0002(11) N6 0.0217(14) 0.0250(14) 0.0246(17) 0.0023(12) 0.0018(13) -0.0007(12) C1 0.0183(16) 0.0198(17) 0.030(2) -0.0006(15) 0.0004(16) 0.0004(13) C2 0.0228(17) 0.0209(17) 0.023(2) 0.0037(15) -0.0017(15) 0.0033(14) C3 0.0180(16) 0.0303(19) 0.024(2) -0.0001(16) 0.0034(14) -0.0012(15) C4 0.0260(18) 0.0311(19) 0.027(2) 0.0025(16) 0.0031(16) -0.0051(15) C5 0.034(2) 0.040(2) 0.040(3) 0.0070(18) 0.0108(19) -0.0076(17) C6 0.031(2) 0.053(3) 0.045(3) 0.001(2) 0.0149(19) -0.0019(19) C7 0.0298(19) 0.041(2) 0.039(2) -0.0011(19) 0.0100(18) 0.0079(17) C8 0.0229(17) 0.0299(19) 0.029(2) 0.0018(16) 0.0010(15) 0.0017(15) C9 0.0311(19) 0.0239(18) 0.037(2) 0.0058(16) 0.0039(17) -0.0041(15) C10 0.054(2) 0.031(2) 0.039(3) -0.0009(18) -0.001(2) -0.0074(19) C11 0.042(2) 0.035(2) 0.045(3) 0.0072(19) 0.0011(19) -0.0031(18) C12 0.0331(19) 0.0277(19) 0.038(2) -0.0033(17) 0.0099(17) 0.0074(16) C13 0.060(3) 0.036(2) 0.045(3) 0.004(2) 0.006(2) 0.014(2) C14 0.040(2) 0.032(2) 0.051(3) -0.0056(19) 0.012(2) 0.0066(17) C15 0.0252(17) 0.0271(18) 0.022(2) 0.0055(15) 0.0004(15) -0.0036(15) C16 0.034(2) 0.0254(19) 0.030(2) 0.0030(16) 0.0011(17) -0.0030(16) C17 0.050(2) 0.0277(19) 0.038(3) 0.0057(17) 0.010(2) -0.0058(18) C18 0.047(2) 0.037(2) 0.046(3) 0.0081(19) 0.013(2) -0.0151(19) C19 0.034(2) 0.045(2) 0.042(3) 0.0002(19) 0.0113(19) -0.0074(18) C20 0.0252(18) 0.0307(19) 0.029(2) 0.0015(16) 0.0060(16) -0.0023(15) C21 0.042(2) 0.0232(18) 0.043(3) 0.0060(17) 0.0096(19) 0.0022(16) C22 0.065(3) 0.033(2) 0.060(3) -0.003(2) 0.007(2) 0.012(2) C23 0.045(2) 0.040(2) 0.064(3) -0.001(2) 0.005(2) 0.0029(19) C24 0.0251(18) 0.032(2) 0.039(2) 0.0002(17) 0.0090(17) -0.0004(16) C25 0.035(2) 0.035(2) 0.051(3) -0.0077(19) 0.0137(19) -0.0038(18) C26 0.033(2) 0.051(2) 0.068(3) -0.007(2) 0.019(2) 0.0028(19) C27 0.0218(17) 0.0203(17) 0.030(2) -0.0004(15) -0.0016(16) -0.0004(14) C28 0.0301(19) 0.0200(17) 0.024(2) 0.0003(15) 0.0006(16) -0.0016(15) C29 0.0191(16) 0.0270(18) 0.030(2) -0.0002(16) 0.0034(15) 0.0031(15) C30 0.0239(18) 0.034(2) 0.034(2) 0.0009(17) 0.0043(16) 0.0018(16) C31 0.037(2) 0.045(2) 0.052(3) 0.002(2) 0.022(2) -0.0033(19) C32 0.040(2) 0.048(3) 0.068(3) -0.008(2) 0.027(2) 0.006(2) C33 0.045(2) 0.035(2) 0.062(3) 0.001(2) 0.019(2) 0.0106(19) C34 0.0293(19) 0.032(2) 0.043(3) 0.0037(18) 0.0082(18) 0.0085(17) C35 0.040(2) 0.0265(18) 0.039(2) -0.0004(17) 0.0161(18) -0.0031(17) C36 0.068(3) 0.056(3) 0.079(4) -0.032(3) 0.005(3) 0.002(3) C37 0.135(5) 0.042(3) 0.055(3) 0.006(2) 0.034(3) 0.016(3) C38 0.040(2) 0.0226(18) 0.060(3) 0.0040(19) 0.017(2) 0.0088(17) C39 0.040(2) 0.030(2) 0.079(4) 0.000(2) 0.008(2) 0.0073(18) C40 0.080(3) 0.033(2) 0.066(4) 0.007(2) 0.014(3) 0.001(2) C41 0.0226(17) 0.037(2) 0.019(2) 0.0048(16) -0.0014(15) -0.0081(16) C42 0.034(2) 0.032(2) 0.028(2) 0.0038(17) -0.0022(17) -0.0092(17) C43 0.052(2) 0.043(2) 0.040(3) 0.007(2) 0.011(2) -0.017(2) C44 0.054(3) 0.068(3) 0.048(3) 0.006(2) 0.024(2) -0.022(2) C45 0.037(2) 0.057(3) 0.039(3) 0.000(2) 0.0160(19) -0.005(2) C46 0.0257(19) 0.047(2) 0.023(2) 0.0032(17) 0.0016(16) -0.0025(17) C47 0.039(2) 0.0267(19) 0.042(3) 0.0071(17) 0.0039(19) -0.0109(17) C48 0.062(3) 0.035(2) 0.045(3) 0.001(2) 0.003(2) -0.015(2) C49 0.046(2) 0.033(2) 0.064(3) 0.007(2) -0.002(2) -0.0057(19) C50 0.031(2) 0.043(2) 0.031(2) 0.0036(18) 0.0087(17) 0.0035(17) C51 0.042(2) 0.070(3) 0.082(4) 0.019(3) 0.018(2) 0.014(2) C52 0.069(3) 0.045(2) 0.047(3) 0.001(2) 0.009(2) -0.008(2) C53 0.040(2) 0.031(2) 0.046(3) -0.0100(18) 0.0047(19) 0.0022(17) C54 0.036(2) 0.0249(19) 0.073(3) 0.012(2) 0.012(2) -0.0047(17) C55 0.035(2) 0.037(2) 0.045(3) -0.0118(19) -0.0064(19) -0.0076(18) C56 0.051(2) 0.035(2) 0.031(2) -0.0082(18) -0.0033(19) -0.0027(18) C57 0.047(2) 0.0235(19) 0.056(3) -0.0005(19) 0.006(2) 0.0019(18) C58 0.062(3) 0.032(2) 0.046(3) 0.0034(19) 0.022(2) 0.022(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 1.871(3) . ? Ga1 N2 1.900(2) . ? Ga1 N4 2.012(3) . ? Ga1 N3 2.017(2) . ? Ga2 N2 1.876(3) . ? Ga2 N1 1.895(2) . ? Ga2 N5 2.005(3) . ? Ga2 N6 2.030(3) . ? Si1 N1 1.706(3) . ? Si1 C53 1.871(3) . ? Si1 C55 1.875(4) . ? Si1 C54 1.876(4) . ? Si2 N2 1.706(3) . ? Si2 C58 1.868(4) . ? Si2 C57 1.871(4) . ? Si2 C56 1.872(4) . ? N3 C1 1.330(4) . ? N3 C3 1.453(4) . ? N4 C2 1.337(4) . ? N4 C15 1.449(4) . ? N5 C27 1.330(4) . ? N5 C29 1.448(4) . ? N6 C28 1.329(4) . ? N6 C41 1.454(4) . ? C1 C2 1.392(4) . ? C3 C4 1.398(4) . ? C3 C8 1.412(4) . ? C4 C5 1.396(5) . ? C4 C9 1.518(5) . ? C5 C6 1.374(5) . ? C6 C7 1.377(5) . ? C7 C8 1.394(5) . ? C8 C12 1.523(5) . ? C9 C11 1.529(5) . ? C9 C10 1.535(5) . ? C12 C14 1.528(5) . ? C12 C13 1.531(5) . ? C15 C20 1.406(5) . ? C15 C16 1.421(4) . ? C16 C17 1.394(5) . ? C16 C21 1.518(5) . ? C17 C18 1.363(5) . ? C18 C19 1.385(5) . ? C19 C20 1.392(5) . ? C20 C24 1.522(5) . ? C21 C23 1.529(5) . ? C21 C22 1.537(5) . ? C24 C25 1.532(5) . ? C24 C26 1.533(4) . ? C27 C28 1.407(5) . ? C29 C30 1.408(5) . ? C29 C34 1.411(5) . ? C30 C31 1.385(5) . ? C30 C35 1.524(5) . ? C31 C32 1.380(5) . ? C32 C33 1.357(5) . ? C33 C34 1.389(5) . ? C34 C38 1.520(5) . ? C35 C36 1.507(5) . ? C35 C37 1.514(6) . ? C38 C40 1.521(6) . ? C38 C39 1.522(5) . ? C41 C46 1.393(5) . ? C41 C42 1.415(5) . ? C42 C43 1.396(5) . ? C42 C47 1.522(5) . ? C43 C44 1.360(6) . ? C44 C45 1.385(6) . ? C45 C46 1.398(5) . ? C46 C50 1.527(5) . ? C47 C49 1.528(5) . ? C47 C48 1.541(5) . ? C50 C51 1.528(5) . ? C50 C52 1.529(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 90.50(11) . . ? N1 Ga1 N4 123.45(11) . . ? N2 Ga1 N4 123.17(11) . . ? N1 Ga1 N3 126.11(11) . . ? N2 Ga1 N3 113.58(10) . . ? N4 Ga1 N3 83.62(11) . . ? N2 Ga2 N1 90.50(11) . . ? N2 Ga2 N5 123.95(11) . . ? N1 Ga2 N5 121.91(10) . . ? N2 Ga2 N6 127.50(11) . . ? N1 Ga2 N6 112.90(11) . . ? N5 Ga2 N6 83.50(11) . . ? N1 Si1 C53 112.95(15) . . ? N1 Si1 C55 109.55(15) . . ? C53 Si1 C55 108.13(18) . . ? N1 Si1 C54 113.51(16) . . ? C53 Si1 C54 105.69(17) . . ? C55 Si1 C54 106.66(18) . . ? N2 Si2 C58 114.43(16) . . ? N2 Si2 C57 112.45(16) . . ? C58 Si2 C57 106.92(17) . . ? N2 Si2 C56 109.52(15) . . ? C58 Si2 C56 105.45(19) . . ? C57 Si2 C56 107.64(18) . . ? Si1 N1 Ga1 135.09(15) . . ? Si1 N1 Ga2 133.12(15) . . ? Ga1 N1 Ga2 89.61(11) . . ? Si2 N2 Ga2 136.75(15) . . ? Si2 N2 Ga1 132.70(15) . . ? Ga2 N2 Ga1 89.30(11) . . ? C1 N3 C3 115.1(3) . . ? C1 N3 Ga1 107.7(2) . . ? C3 N3 Ga1 136.9(2) . . ? C2 N4 C15 117.7(3) . . ? C2 N4 Ga1 108.1(2) . . ? C15 N4 Ga1 133.3(2) . . ? C27 N5 C29 116.1(3) . . ? C27 N5 Ga2 108.7(2) . . ? C29 N5 Ga2 133.9(2) . . ? C28 N6 C41 116.5(3) . . ? C28 N6 Ga2 107.7(2) . . ? C41 N6 Ga2 135.6(2) . . ? N3 C1 C2 119.4(3) . . ? N4 C2 C1 118.7(3) . . ? C4 C3 C8 120.8(3) . . ? C4 C3 N3 121.5(3) . . ? C8 C3 N3 117.7(3) . . ? C5 C4 C3 118.1(3) . . ? C5 C4 C9 118.6(3) . . ? C3 C4 C9 123.3(3) . . ? C6 C5 C4 122.0(3) . . ? C5 C6 C7 119.1(3) . . ? C6 C7 C8 121.7(3) . . ? C7 C8 C3 118.1(3) . . ? C7 C8 C12 118.2(3) . . ? C3 C8 C12 123.7(3) . . ? C4 C9 C11 111.2(3) . . ? C4 C9 C10 110.3(3) . . ? C11 C9 C10 110.4(3) . . ? C8 C12 C14 112.4(3) . . ? C8 C12 C13 111.1(3) . . ? C14 C12 C13 109.1(3) . . ? C20 C15 C16 120.8(3) . . ? C20 C15 N4 120.2(3) . . ? C16 C15 N4 119.1(3) . . ? C17 C16 C15 117.3(3) . . ? C17 C16 C21 118.3(3) . . ? C15 C16 C21 124.4(3) . . ? C18 C17 C16 122.5(3) . . ? C17 C18 C19 119.6(3) . . ? C18 C19 C20 121.2(4) . . ? C19 C20 C15 118.5(3) . . ? C19 C20 C24 120.6(3) . . ? C15 C20 C24 120.6(3) . . ? C16 C21 C23 110.4(3) . . ? C16 C21 C22 113.0(3) . . ? C23 C21 C22 109.3(3) . . ? C20 C24 C25 108.5(3) . . ? C20 C24 C26 113.7(3) . . ? C25 C24 C26 109.6(3) . . ? N5 C27 C28 118.6(3) . . ? N6 C28 C27 119.0(3) . . ? C30 C29 C34 120.7(3) . . ? C30 C29 N5 121.3(3) . . ? C34 C29 N5 117.9(3) . . ? C31 C30 C29 117.9(3) . . ? C31 C30 C35 119.7(3) . . ? C29 C30 C35 122.3(3) . . ? C32 C31 C30 122.0(4) . . ? C33 C32 C31 119.2(4) . . ? C32 C33 C34 122.4(4) . . ? C33 C34 C29 117.7(3) . . ? C33 C34 C38 119.0(3) . . ? C29 C34 C38 123.2(3) . . ? C36 C35 C37 110.4(4) . . ? C36 C35 C30 109.6(3) . . ? C37 C35 C30 112.1(3) . . ? C34 C38 C40 110.2(3) . . ? C34 C38 C39 113.5(3) . . ? C40 C38 C39 109.1(3) . . ? C46 C41 C42 121.2(3) . . ? C46 C41 N6 120.6(3) . . ? C42 C41 N6 118.3(3) . . ? C43 C42 C41 117.5(3) . . ? C43 C42 C47 118.1(3) . . ? C41 C42 C47 124.4(3) . . ? C44 C43 C42 122.3(4) . . ? C43 C44 C45 119.4(4) . . ? C44 C45 C46 121.4(4) . . ? C41 C46 C45 118.2(3) . . ? C41 C46 C50 122.8(3) . . ? C45 C46 C50 118.8(3) . . ? C42 C47 C49 111.2(3) . . ? C42 C47 C48 112.3(3) . . ? C49 C47 C48 109.0(3) . . ? C46 C50 C51 112.2(3) . . ? C46 C50 C52 109.6(3) . . ? C51 C50 C52 110.3(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.774 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.068 data_compound_6 _database_code_depnum_ccdc_archive 'CCDC 280913' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H82.5 Ga I2 Li N2 O2 P' _chemical_formula_weight 1129.13 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' P P 0.1023 0.0942 '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' Li Li -0.0003 0.0001 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.088(2) _cell_length_b 49.646(10) _cell_length_c 22.378(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.94(3) _cell_angle_gamma 90.00 _cell_volume 11100(4) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4636 _exptl_absorpt_coefficient_mu 1.674 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.685 _exptl_absorpt_correction_T_max 0.920 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57446 _diffrn_reflns_av_R_equivalents 0.1030 _diffrn_reflns_av_sigmaI/netI 0.1274 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 59 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.00 _reflns_number_total 19185 _reflns_number_gt 10892 _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. Two crystallographically independent molecules were located in the asymmetric unit and no significant geometrical differences were found between them. In both, the P-H hydrogens, H1A and H2A, were located from difference maps and refined isotropically. Upon convergence of the structural refinement, close contacts between H2A and 2 methyl hydrogens of a supermesityl substituent were observed (H2A-H87A 1.77 ang., H2A-H88B 1.97 ang.). In addition,a close contact between H1A and 1 methyl hydrogen of a supermesityl substituent was observed (H1A-H43A 1.91 ang). These close contacts occur because, although the position of P-H hydrogens can be considered as relatively accurate (through isotropic refinement),the methyl hydrogen atoms are in calculated positions (riding model) and thus their positions should not be regarded as accurate and the aforementioned H..H contacts should be disregarded. Each molecule in the asymmetric unit was found to contain a tert-butyl group each of which is disordered over 2 sites. This disorder was successfully modelled. The asymmetric unit of the crystal structure was additionally found to contain a dimeric molecule of [Li2I2(THF)3.5(OEt2)0.5]. In this molecule 3 THF ligands are present at full occupancy and one refined with 50% occupancy, its coordination site being disordered with diethyl ether which was refined at 50% occupancy. The 50% occupancy THF and diethyl ether molecules were refined isotropically. ; _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^)+(0.0525P)^2^+15.9135P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00028(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 19185 _refine_ls_number_parameters 1187 _refine_ls_number_restraints 104 _refine_ls_R_factor_all 0.1411 _refine_ls_R_factor_gt 0.0663 _refine_ls_wR_factor_ref 0.1528 _refine_ls_wR_factor_gt 0.1283 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.58842(5) 0.970740(11) 0.75495(2) 0.04522(17) Uani 1 1 d . . . I2 I 0.57952(5) 0.752970(10) 0.49642(2) 0.03809(15) Uani 1 1 d . . . I3 I 1.36478(7) 0.583620(12) 0.64689(3) 0.0722(2) Uani 1 1 d . A . I4 I 1.05756(7) 0.646380(14) 0.65497(3) 0.0783(2) Uani 1 1 d . A . Ga1 Ga 0.83976(8) 0.971400(16) 0.75054(3) 0.0317(2) Uani 1 1 d . . . Ga2 Ga 0.83435(7) 0.751600(15) 0.50025(3) 0.0273(2) Uani 1 1 d . . . P1 P 0.9097(2) 0.93831(4) 0.68750(9) 0.0398(5) Uani 1 1 d D . . P2 P 0.9248(2) 0.78740(4) 0.45227(8) 0.0325(5) Uani 1 1 d D . . O1 O 1.3339(7) 0.62820(13) 0.7838(3) 0.0694(18) Uani 1 1 d . . . O2 O 1.4453(7) 0.65660(12) 0.6745(3) 0.0696(18) Uani 1 1 d . . . O3 O 1.1147(9) 0.60751(15) 0.5165(3) 0.097(3) Uani 1 1 d . A . O4 O 0.9920(12) 0.5697(2) 0.5849(6) 0.064(4) Uiso 0.50 1 d PD A 1 O4A O 0.9658(15) 0.5732(3) 0.6137(8) 0.094(5) Uiso 0.50 1 d PD A 2 N1 N 0.9280(6) 0.97855(11) 0.8334(2) 0.0302(14) Uani 1 1 d . . . N2 N 0.8999(6) 1.00816(12) 0.7343(3) 0.0367(15) Uani 1 1 d . . . N3 N 0.8828(6) 0.71394(11) 0.4846(2) 0.0312(14) Uani 1 1 d . . . N4 N 0.9142(5) 0.74360(11) 0.5839(2) 0.0272(14) Uani 1 1 d . . . C1 C 0.9644(7) 1.00466(16) 0.8380(3) 0.043(2) Uani 1 1 d . . . H1 H 0.9991 1.0123 0.8759 0.051 Uiso 1 1 calc R . . C2 C 0.9497(7) 1.02025(15) 0.7853(3) 0.0374(19) Uani 1 1 d . . . H2 H 0.9745 1.0387 0.7860 0.045 Uiso 1 1 calc R . . C3 C 0.9580(8) 0.96140(14) 0.8852(3) 0.0356(19) Uani 1 1 d . . . C4 C 1.0677(8) 0.94437(15) 0.8872(4) 0.046(2) Uani 1 1 d . . . C5 C 1.0966(10) 0.92681(16) 0.9358(4) 0.058(3) Uani 1 1 d . . . H5 H 1.1707 0.9149 0.9373 0.070 Uiso 1 1 calc R . . C6 C 1.0185(11) 0.92662(19) 0.9816(4) 0.063(3) Uani 1 1 d . . . H6 H 1.0392 0.9147 1.0148 0.075 Uiso 1 1 calc R . . C7 C 0.9111(9) 0.94356(18) 0.9792(4) 0.055(2) Uani 1 1 d . . . H7 H 0.8574 0.9431 1.0108 0.066 Uiso 1 1 calc R . . C8 C 0.8783(8) 0.96157(16) 0.9311(3) 0.043(2) Uani 1 1 d . . . C9 C 1.1638(8) 0.94558(18) 0.8401(4) 0.058(3) Uani 1 1 d . . . H9 H 1.1103 0.9512 0.8011 0.069 Uiso 1 1 calc R . . C10 C 1.2311(10) 0.9189(2) 0.8288(4) 0.089(4) Uani 1 1 d . . . H10A H 1.2939 0.9139 0.8645 0.133 Uiso 1 1 calc R . . H10B H 1.2797 0.9207 0.7940 0.133 Uiso 1 1 calc R . . H10C H 1.1628 0.9048 0.8206 0.133 Uiso 1 1 calc R . . C11 C 1.2677(9) 0.9675(2) 0.8577(4) 0.076(3) Uani 1 1 d . . . H11A H 1.3177 0.9634 0.8973 0.114 Uiso 1 1 calc R . . H11B H 1.2227 0.9849 0.8594 0.114 Uiso 1 1 calc R . . H11C H 1.3296 0.9683 0.8276 0.114 Uiso 1 1 calc R . . C12 C 0.7618(8) 0.98059(17) 0.9325(4) 0.051(2) Uani 1 1 d . . . H12 H 0.7494 0.9912 0.8942 0.061 Uiso 1 1 calc R . . C13 C 0.7907(10) 1.0002(2) 0.9857(4) 0.077(3) Uani 1 1 d . . . H13A H 0.8101 0.9900 1.0234 0.116 Uiso 1 1 calc R . . H13B H 0.7124 1.0117 0.9874 0.116 Uiso 1 1 calc R . . H13C H 0.8680 1.0114 0.9802 0.116 Uiso 1 1 calc R . . C14 C 0.6314(8) 0.9652(2) 0.9374(4) 0.071(3) Uani 1 1 d . . . H14A H 0.6069 0.9543 0.9009 0.106 Uiso 1 1 calc R . . H14B H 0.5596 0.9780 0.9417 0.106 Uiso 1 1 calc R . . H14C H 0.6448 0.9533 0.9727 0.106 Uiso 1 1 calc R . . C15 C 0.8988(8) 1.02161(15) 0.6773(3) 0.042(2) Uani 1 1 d . . . C16 C 1.0011(9) 1.01538(17) 0.6434(4) 0.054(2) Uani 1 1 d . . . C17 C 0.9948(11) 1.0266(2) 0.5863(5) 0.074(3) Uani 1 1 d . . . H17 H 1.0626 1.0225 0.5622 0.089 Uiso 1 1 calc R . . C18 C 0.8928(11) 1.0435(2) 0.5642(4) 0.072(3) Uani 1 1 d . . . H18 H 0.8889 1.0506 0.5247 0.086 Uiso 1 1 calc R . . C19 C 0.7955(10) 1.05014(17) 0.5992(4) 0.064(3) Uani 1 1 d . . . H19 H 0.7268 1.0624 0.5836 0.077 Uiso 1 1 calc R . . C20 C 0.7951(8) 1.03933(16) 0.6573(4) 0.046(2) Uani 1 1 d . . . C21 C 1.1239(8) 0.99880(17) 0.6703(4) 0.058(2) Uani 1 1 d . . . H21 H 1.0937 0.9855 0.6991 0.069 Uiso 1 1 calc R . . C22 C 1.2269(9) 1.01761(19) 0.7065(5) 0.082(3) Uani 1 1 d . . . H22A H 1.2556 1.0314 0.6796 0.123 Uiso 1 1 calc R . . H22B H 1.3047 1.0071 0.7243 0.123 Uiso 1 1 calc R . . H22C H 1.1860 1.0264 0.7387 0.123 Uiso 1 1 calc R . . C23 C 1.1888(11) 0.9831(2) 0.6230(5) 0.093(4) Uani 1 1 d . . . H23A H 1.1192 0.9737 0.5958 0.140 Uiso 1 1 calc R . . H23B H 1.2520 0.9699 0.6432 0.140 Uiso 1 1 calc R . . H23C H 1.2365 0.9956 0.5996 0.140 Uiso 1 1 calc R . . C24 C 0.6899(8) 1.04742(15) 0.6954(4) 0.047(2) Uani 1 1 d . . . H24 H 0.6949 1.0345 0.7300 0.056 Uiso 1 1 calc R . . C25 C 0.7191(10) 1.07580(16) 0.7216(5) 0.079(3) Uani 1 1 d . . . H25A H 0.8056 1.0758 0.7476 0.118 Uiso 1 1 calc R . . H25B H 0.6485 1.0810 0.7454 0.118 Uiso 1 1 calc R . . H25C H 0.7217 1.0887 0.6886 0.118 Uiso 1 1 calc R . . C26 C 0.5479(9) 1.0463(2) 0.6617(4) 0.081(3) Uani 1 1 d . . . H26A H 0.5376 1.0599 0.6297 0.122 Uiso 1 1 calc R . . H26B H 0.4838 1.0498 0.6899 0.122 Uiso 1 1 calc R . . H26C H 0.5311 1.0284 0.6438 0.122 Uiso 1 1 calc R . . C27 C 0.7512(7) 0.92044(14) 0.6613(3) 0.0331(18) Uani 1 1 d . . . C28 C 0.7106(7) 0.89833(14) 0.6966(3) 0.0341(18) Uani 1 1 d . . . C29 C 0.5816(8) 0.88889(14) 0.6835(3) 0.0336(18) Uani 1 1 d . . . H29 H 0.5553 0.8748 0.7080 0.040 Uiso 1 1 calc R . . C30 C 0.4873(8) 0.89824(14) 0.6375(3) 0.0347(19) Uani 1 1 d . B . C31 C 0.5342(8) 0.91737(15) 0.5997(3) 0.044(2) Uani 1 1 d . . . H31 H 0.4746 0.9234 0.5658 0.053 Uiso 1 1 calc R . . C32 C 0.6630(8) 0.92820(14) 0.6087(3) 0.0354(19) Uani 1 1 d . . . C33 C 0.8064(8) 0.88364(15) 0.7465(3) 0.042(2) Uani 1 1 d . . . C34 C 0.8427(8) 0.90196(15) 0.8024(3) 0.049(2) Uani 1 1 d . . . H34A H 0.8946 0.9174 0.7915 0.073 Uiso 1 1 calc R . . H34B H 0.8960 0.8917 0.8346 0.073 Uiso 1 1 calc R . . H34C H 0.7605 0.9083 0.8165 0.073 Uiso 1 1 calc R . . C35 C 0.9313(8) 0.87363(16) 0.7221(4) 0.057(2) Uani 1 1 d . . . H35A H 0.9055 0.8609 0.6890 0.086 Uiso 1 1 calc R . . H35B H 0.9904 0.8646 0.7544 0.086 Uiso 1 1 calc R . . H35C H 0.9784 0.8890 0.7071 0.086 Uiso 1 1 calc R . . C36 C 0.7392(10) 0.85838(15) 0.7701(4) 0.065(3) Uani 1 1 d . . . H36A H 0.6582 0.8638 0.7866 0.098 Uiso 1 1 calc R . . H36B H 0.8016 0.8497 0.8018 0.098 Uiso 1 1 calc R . . H36C H 0.7153 0.8457 0.7368 0.098 Uiso 1 1 calc R . . C37 C 0.3447(8) 0.88788(16) 0.6264(3) 0.043(2) Uani 1 1 d . . . C38 C 0.2386(19) 0.9107(3) 0.6252(9) 0.051(6) Uani 0.453(13) 1 d P B 1 H38A H 0.2588 0.9249 0.5975 0.076 Uiso 0.453(13) 1 calc PR B 1 H38B H 0.2408 0.9182 0.6658 0.076 Uiso 0.453(13) 1 calc PR B 1 H38C H 0.1495 0.9033 0.6115 0.076 Uiso 0.453(13) 1 calc PR B 1 C38A C 0.2884(17) 0.8954(4) 0.6828(8) 0.075(7) Uani 0.547(13) 1 d P B 2 H38D H 0.2010 0.8868 0.6826 0.112 Uiso 0.547(13) 1 calc PR B 2 H38E H 0.2781 0.9150 0.6845 0.112 Uiso 0.547(13) 1 calc PR B 2 H38F H 0.3494 0.8893 0.7181 0.112 Uiso 0.547(13) 1 calc PR B 2 C39 C 0.3051(18) 0.8675(4) 0.6744(8) 0.052(6) Uani 0.453(13) 1 d P B 1 H39A H 0.3569 0.8508 0.6729 0.079 Uiso 0.453(13) 1 calc PR B 1 H39B H 0.2094 0.8634 0.6656 0.079 Uiso 0.453(13) 1 calc PR B 1 H39C H 0.3243 0.8754 0.7147 0.079 Uiso 0.453(13) 1 calc PR B 1 C39A C 0.3486(17) 0.8585(3) 0.6155(9) 0.072(7) Uani 0.547(13) 1 d P B 2 H39D H 0.3968 0.8496 0.6511 0.107 Uiso 0.547(13) 1 calc PR B 2 H39E H 0.3946 0.8550 0.5805 0.107 Uiso 0.547(13) 1 calc PR B 2 H39F H 0.2570 0.8515 0.6078 0.107 Uiso 0.547(13) 1 calc PR B 2 C40 C 0.3178(19) 0.8732(4) 0.5649(7) 0.050(6) Uani 0.453(13) 1 d P B 1 H40A H 0.3674 0.8562 0.5672 0.076 Uiso 0.453(13) 1 calc PR B 1 H40B H 0.3472 0.8846 0.5334 0.076 Uiso 0.453(13) 1 calc PR B 1 H40C H 0.2218 0.8696 0.5550 0.076 Uiso 0.453(13) 1 calc PR B 1 C40A C 0.2628(17) 0.9016(4) 0.5701(8) 0.068(6) Uani 0.547(13) 1 d P B 2 H40D H 0.3003 0.8964 0.5337 0.101 Uiso 0.547(13) 1 calc PR B 2 H40E H 0.2677 0.9212 0.5748 0.101 Uiso 0.547(13) 1 calc PR B 2 H40F H 0.1692 0.8958 0.5666 0.101 Uiso 0.547(13) 1 calc PR B 2 C41 C 0.7010(10) 0.94729(17) 0.5592(3) 0.059(3) Uani 1 1 d . . . C42 C 0.6968(11) 0.97745(16) 0.5799(4) 0.076(3) Uani 1 1 d . . . H42A H 0.6079 0.9816 0.5904 0.115 Uiso 1 1 calc R . . H42B H 0.7154 0.9893 0.5469 0.115 Uiso 1 1 calc R . . H42C H 0.7644 0.9804 0.6151 0.115 Uiso 1 1 calc R . . C43 C 0.8342(11) 0.9396(2) 0.5385(4) 0.081(3) Uani 1 1 d . . . H43A H 0.8959 0.9330 0.5731 0.121 Uiso 1 1 calc R . . H43B H 0.8730 0.9554 0.5213 0.121 Uiso 1 1 calc R . . H43C H 0.8190 0.9254 0.5078 0.121 Uiso 1 1 calc R . . C44 C 0.5959(11) 0.94623(19) 0.5004(4) 0.083(3) Uani 1 1 d U . . H44A H 0.5764 0.9274 0.4893 0.125 Uiso 1 1 calc R . . H44B H 0.6326 0.9554 0.4675 0.125 Uiso 1 1 calc R . . H44C H 0.5134 0.9553 0.5078 0.125 Uiso 1 1 calc R . . C45 C 0.9228(7) 0.70178(14) 0.5373(3) 0.0336(18) Uani 1 1 d . . . H45 H 0.9389 0.6829 0.5392 0.040 Uiso 1 1 calc R . . C46 C 0.9401(7) 0.71738(15) 0.5892(3) 0.0310(18) Uani 1 1 d . . . H46 H 0.9695 0.7096 0.6275 0.037 Uiso 1 1 calc R . . C47 C 0.8880(7) 0.69940(13) 0.4294(3) 0.0284(17) Uani 1 1 d . . . C48 C 0.9994(7) 0.70351(14) 0.3991(3) 0.0322(18) Uani 1 1 d . . . C49 C 1.0038(9) 0.68991(17) 0.3447(4) 0.050(2) Uani 1 1 d . . . H49 H 1.0784 0.6923 0.3235 0.060 Uiso 1 1 calc R . . C50 C 0.9019(9) 0.67316(16) 0.3216(4) 0.051(2) Uani 1 1 d . . . H50 H 0.9058 0.6644 0.2842 0.061 Uiso 1 1 calc R . . C51 C 0.7945(9) 0.66879(15) 0.3516(3) 0.045(2) Uani 1 1 d . . . H51 H 0.7263 0.6566 0.3354 0.054 Uiso 1 1 calc R . . C52 C 0.7839(7) 0.68210(13) 0.4059(3) 0.0322(18) Uani 1 1 d . . . C53 C 1.1162(8) 0.72118(15) 0.4267(3) 0.041(2) Uani 1 1 d . . . H53 H 1.0789 0.7354 0.4514 0.049 Uiso 1 1 calc R . . C54 C 1.2162(8) 0.70451(17) 0.4696(4) 0.056(2) Uani 1 1 d . . . H54A H 1.1730 0.6982 0.5036 0.084 Uiso 1 1 calc R . . H54B H 1.2937 0.7157 0.4846 0.084 Uiso 1 1 calc R . . H54C H 1.2458 0.6890 0.4478 0.084 Uiso 1 1 calc R . . C55 C 1.1872(9) 0.73557(17) 0.3793(4) 0.057(2) Uani 1 1 d . . . H55A H 1.2312 0.7222 0.3564 0.085 Uiso 1 1 calc R . . H55B H 1.2542 0.7480 0.3994 0.085 Uiso 1 1 calc R . . H55C H 1.1213 0.7456 0.3516 0.085 Uiso 1 1 calc R . . C56 C 0.6629(8) 0.67728(14) 0.4381(3) 0.041(2) Uani 1 1 d . . . H56 H 0.6695 0.6898 0.4735 0.049 Uiso 1 1 calc R . . C57 C 0.6604(11) 0.64845(17) 0.4619(5) 0.081(3) Uani 1 1 d . . . H57A H 0.6562 0.6358 0.4281 0.121 Uiso 1 1 calc R . . H57B H 0.5817 0.6460 0.4826 0.121 Uiso 1 1 calc R . . H57C H 0.7418 0.6451 0.4903 0.121 Uiso 1 1 calc R . . C58 C 0.5339(8) 0.68359(19) 0.3973(4) 0.068(3) Uani 1 1 d . . . H58A H 0.5229 0.6710 0.3632 0.103 Uiso 1 1 calc R . . H58B H 0.5373 0.7021 0.3822 0.103 Uiso 1 1 calc R . . H58C H 0.4581 0.6817 0.4201 0.103 Uiso 1 1 calc R . . C59 C 0.9574(7) 0.76140(13) 0.6337(3) 0.0305(18) Uani 1 1 d . . . C60 C 0.8749(7) 0.76691(14) 0.6769(3) 0.0318(18) Uani 1 1 d . . . C61 C 0.9227(8) 0.78478(16) 0.7235(3) 0.047(2) Uani 1 1 d . . . H61 H 0.8684 0.7890 0.7537 0.057 Uiso 1 1 calc R . . C62 C 1.0478(9) 0.79635(16) 0.7259(4) 0.049(2) Uani 1 1 d . . . H62 H 1.0802 0.8080 0.7583 0.059 Uiso 1 1 calc R . . C63 C 1.1252(8) 0.79096(15) 0.6817(3) 0.041(2) Uani 1 1 d . . . H63 H 1.2094 0.7997 0.6832 0.049 Uiso 1 1 calc R . . C64 C 1.0852(7) 0.77322(14) 0.6349(3) 0.0333(18) Uani 1 1 d . . . C65 C 0.7395(8) 0.75373(17) 0.6761(3) 0.047(2) Uani 1 1 d . . . H65 H 0.7149 0.7454 0.6355 0.057 Uiso 1 1 calc R . . C66 C 0.7486(9) 0.73106(18) 0.7229(4) 0.066(3) Uani 1 1 d . . . H66A H 0.8129 0.7175 0.7132 0.099 Uiso 1 1 calc R . . H66B H 0.6604 0.7227 0.7223 0.099 Uiso 1 1 calc R . . H66C H 0.7784 0.7385 0.7631 0.099 Uiso 1 1 calc R . . C67 C 0.6312(9) 0.7739(2) 0.6849(4) 0.070(3) Uani 1 1 d . . . H67A H 0.6511 0.7821 0.7249 0.105 Uiso 1 1 calc R . . H67B H 0.5446 0.7647 0.6814 0.105 Uiso 1 1 calc R . . H67C H 0.6280 0.7879 0.6539 0.105 Uiso 1 1 calc R . . C68 C 1.1774(7) 0.76695(14) 0.5888(3) 0.0357(19) Uani 1 1 d . . . H68 H 1.1203 0.7603 0.5517 0.043 Uiso 1 1 calc R . . C69 C 1.2569(8) 0.79107(16) 0.5703(4) 0.057(2) Uani 1 1 d . . . H69A H 1.1954 0.8059 0.5574 0.085 Uiso 1 1 calc R . . H69B H 1.3050 0.7859 0.5370 0.085 Uiso 1 1 calc R . . H69C H 1.3212 0.7969 0.6048 0.085 Uiso 1 1 calc R . . C70 C 1.2729(8) 0.74393(15) 0.6120(3) 0.045(2) Uani 1 1 d . . . H70A H 1.3243 0.7491 0.6507 0.068 Uiso 1 1 calc R . . H70B H 1.3344 0.7404 0.5826 0.068 Uiso 1 1 calc R . . H70C H 1.2209 0.7277 0.6174 0.068 Uiso 1 1 calc R . . C71 C 0.7689(7) 0.80644(13) 0.4249(3) 0.0291(17) Uani 1 1 d . . . C72 C 0.6949(7) 0.79975(13) 0.3680(3) 0.0320(18) Uani 1 1 d . . . C73 C 0.5664(8) 0.81010(14) 0.3559(3) 0.0361(19) Uani 1 1 d . . . H73 H 0.5136 0.8047 0.3194 0.043 Uiso 1 1 calc R . . C74 C 0.5089(7) 0.82781(14) 0.3930(3) 0.0330(18) Uani 1 1 d . C . C75 C 0.5903(8) 0.83618(14) 0.4439(3) 0.0362(19) Uani 1 1 d . . . H75 H 0.5558 0.8492 0.4689 0.043 Uiso 1 1 calc R . . C76 C 0.7200(7) 0.82689(13) 0.4613(3) 0.0315(18) Uani 1 1 d . . . C77 C 0.7464(8) 0.78214(14) 0.3189(3) 0.0375(19) Uani 1 1 d . . . C78 C 0.7648(9) 0.75248(14) 0.3387(4) 0.049(2) Uani 1 1 d . . . H78A H 0.7798 0.7414 0.3040 0.073 Uiso 1 1 calc R . . H78B H 0.6842 0.7462 0.3544 0.073 Uiso 1 1 calc R . . H78C H 0.8421 0.7510 0.3703 0.073 Uiso 1 1 calc R . . C79 C 0.8756(9) 0.79412(16) 0.3015(3) 0.053(2) Uani 1 1 d . . . H79A H 0.8574 0.8121 0.2845 0.079 Uiso 1 1 calc R . . H79B H 0.9091 0.7825 0.2714 0.079 Uiso 1 1 calc R . . H79C H 0.9429 0.7953 0.3374 0.079 Uiso 1 1 calc R . . C80 C 0.6455(9) 0.78131(17) 0.2602(3) 0.058(3) Uani 1 1 d . . . H80A H 0.6303 0.7996 0.2444 0.087 Uiso 1 1 calc R . . H80B H 0.5606 0.7737 0.2688 0.087 Uiso 1 1 calc R . . H80C H 0.6817 0.7701 0.2302 0.087 Uiso 1 1 calc R . . C81 C 0.3637(8) 0.83716(16) 0.3776(4) 0.046(2) Uani 1 1 d . . . C82 C 0.2732(12) 0.8136(3) 0.3802(9) 0.088(7) Uani 0.725(16) 1 d P C 1 H82A H 0.2772 0.8076 0.4221 0.131 Uiso 0.725(16) 1 calc PR C 1 H82B H 0.3017 0.7989 0.3556 0.131 Uiso 0.725(16) 1 calc PR C 1 H82C H 0.1813 0.8189 0.3646 0.131 Uiso 0.725(16) 1 calc PR C 1 C82A C 0.284(3) 0.8272(7) 0.4282(15) 0.049(10) Uiso 0.275(16) 1 d P C 2 H82D H 0.3123 0.8372 0.4654 0.074 Uiso 0.275(16) 1 calc PR C 2 H82E H 0.3010 0.8079 0.4354 0.074 Uiso 0.275(16) 1 calc PR C 2 H82F H 0.1879 0.8300 0.4155 0.074 Uiso 0.275(16) 1 calc PR C 2 C83 C 0.3423(14) 0.8486(3) 0.3133(5) 0.072(5) Uani 0.725(16) 1 d P C 1 H83A H 0.2471 0.8525 0.3015 0.108 Uiso 0.725(16) 1 calc PR C 1 H83B H 0.3718 0.8353 0.2855 0.108 Uiso 0.725(16) 1 calc PR C 1 H83C H 0.3943 0.8652 0.3120 0.108 Uiso 0.725(16) 1 calc PR C 1 C83A C 0.293(4) 0.8269(8) 0.3171(15) 0.065(12) Uiso 0.275(16) 1 d P C 2 H83D H 0.1987 0.8326 0.3121 0.098 Uiso 0.275(16) 1 calc PR C 2 H83E H 0.2975 0.8072 0.3161 0.098 Uiso 0.275(16) 1 calc PR C 2 H83F H 0.3362 0.8344 0.2843 0.098 Uiso 0.275(16) 1 calc PR C 2 C84 C 0.3249(15) 0.8594(3) 0.4186(8) 0.084(5) Uani 0.725(16) 1 d PU C 1 H84A H 0.3873 0.8745 0.4183 0.125 Uiso 0.725(16) 1 calc PR C 1 H84B H 0.3285 0.8525 0.4598 0.125 Uiso 0.725(16) 1 calc PR C 1 H84C H 0.2338 0.8656 0.4040 0.125 Uiso 0.725(16) 1 calc PR C 1 C84A C 0.359(3) 0.8673(6) 0.3819(16) 0.048(10) Uiso 0.275(16) 1 d P C 2 H84D H 0.2660 0.8732 0.3803 0.072 Uiso 0.275(16) 1 calc PR C 2 H84E H 0.3978 0.8753 0.3482 0.072 Uiso 0.275(16) 1 calc PR C 2 H84F H 0.4106 0.8732 0.4201 0.072 Uiso 0.275(16) 1 calc PR C 2 C85 C 0.7993(8) 0.83986(15) 0.5192(3) 0.042(2) Uani 1 1 d . . . C86 C 0.7250(9) 0.86447(17) 0.5407(4) 0.067(3) Uani 1 1 d . . . H86A H 0.7797 0.8727 0.5756 0.100 Uiso 1 1 calc R . . H86B H 0.6392 0.8587 0.5523 0.100 Uiso 1 1 calc R . . H86C H 0.7089 0.8777 0.5079 0.100 Uiso 1 1 calc R . . C87 C 0.8125(10) 0.81978(17) 0.5723(3) 0.072(3) Uani 1 1 d . . . H87A H 0.8561 0.8033 0.5609 0.107 Uiso 1 1 calc R . . H87B H 0.7233 0.8154 0.5822 0.107 Uiso 1 1 calc R . . H87C H 0.8664 0.8279 0.6075 0.107 Uiso 1 1 calc R . . C88 C 0.9351(8) 0.85045(16) 0.5058(4) 0.057(2) Uani 1 1 d . . . H88A H 0.9210 0.8662 0.4792 0.086 Uiso 1 1 calc R . . H88B H 0.9809 0.8363 0.4859 0.086 Uiso 1 1 calc R . . H88C H 0.9900 0.8556 0.5436 0.086 Uiso 1 1 calc R . . C89 C 1.2302(13) 0.6250(3) 0.8182(5) 0.114(4) Uani 1 1 d U . . H89A H 1.1437 0.6232 0.7916 0.137 Uiso 1 1 calc R . . H89B H 1.2251 0.6409 0.8446 0.137 Uiso 1 1 calc R . . C90 C 1.2569(15) 0.6011(3) 0.8542(7) 0.136(5) Uani 1 1 d U . . H90A H 1.2029 0.5856 0.8365 0.164 Uiso 1 1 calc R . . H90B H 1.2393 0.6040 0.8961 0.164 Uiso 1 1 calc R . . C91 C 1.4091(17) 0.5967(3) 0.8513(7) 0.149(6) Uani 1 1 d U . . H91A H 1.4599 0.5959 0.8924 0.178 Uiso 1 1 calc R . . H91B H 1.4239 0.5797 0.8299 0.178 Uiso 1 1 calc R . . C92 C 1.4494(14) 0.6195(3) 0.8188(6) 0.123(5) Uani 1 1 d U . . H92A H 1.4868 0.6338 0.8470 0.148 Uiso 1 1 calc R . . H92B H 1.5177 0.6143 0.7932 0.148 Uiso 1 1 calc R . . C93 C 1.5838(14) 0.6514(3) 0.6746(6) 0.126(5) Uani 1 1 d U . . H93A H 1.6348 0.6585 0.7122 0.151 Uiso 1 1 calc R . . H93B H 1.5986 0.6316 0.6739 0.151 Uiso 1 1 calc R . . C94 C 1.6312(15) 0.6632(3) 0.6248(6) 0.139(5) Uani 1 1 d U . . H94A H 1.6483 0.6493 0.5950 0.167 Uiso 1 1 calc R . . H94B H 1.7152 0.6732 0.6375 0.167 Uiso 1 1 calc R . . C95 C 1.5215(12) 0.6820(3) 0.5984(5) 0.106(4) Uani 1 1 d U . . H95A H 1.5542 0.7008 0.5993 0.127 Uiso 1 1 calc R . . H95B H 1.4886 0.6770 0.5561 0.127 Uiso 1 1 calc R . . C96 C 1.4166(13) 0.6790(2) 0.6358(5) 0.098(4) Uani 1 1 d U . . H96A H 1.4105 0.6955 0.6601 0.118 Uiso 1 1 calc R . . H96B H 1.3296 0.6763 0.6101 0.118 Uiso 1 1 calc R . . C97 C 1.2140(15) 0.6257(3) 0.5002(6) 0.123(5) Uani 1 1 d U . . H97A H 1.1986 0.6441 0.5151 0.148 Uiso 1 1 calc R . . H97B H 1.3044 0.6197 0.5181 0.148 Uiso 1 1 calc R . . C98 C 1.2032(15) 0.6257(3) 0.4363(6) 0.128(5) Uani 1 1 d U . . H98A H 1.2741 0.6144 0.4224 0.154 Uiso 1 1 calc R . . H98B H 1.2102 0.6442 0.4206 0.154 Uiso 1 1 calc R . . C99 C 1.0694(15) 0.6143(3) 0.4161(6) 0.141(5) Uani 1 1 d U . . H99A H 1.0106 0.6281 0.3945 0.170 Uiso 1 1 calc R . . H99B H 1.0767 0.5990 0.3882 0.170 Uiso 1 1 calc R . . C100 C 1.0130(12) 0.6049(3) 0.4692(5) 0.100(4) Uani 1 1 d U . . H10D H 0.9352 0.6161 0.4759 0.120 Uiso 1 1 calc R . . H10E H 0.9840 0.5859 0.4642 0.120 Uiso 1 1 calc R . . C101 C 0.8526(17) 0.5744(4) 0.5816(9) 0.080(7) Uiso 0.50 1 d PD A 1 H10F H 0.8058 0.5704 0.5407 0.096 Uiso 0.50 1 calc PR A 1 H10G H 0.8345 0.5933 0.5920 0.096 Uiso 0.50 1 calc PR A 1 C102 C 0.809(2) 0.5555(6) 0.6270(12) 0.140(12) Uiso 0.50 1 d PD A 1 H10H H 0.7434 0.5423 0.6076 0.168 Uiso 0.50 1 calc PR A 1 H10I H 0.7693 0.5654 0.6585 0.168 Uiso 0.50 1 calc PR A 1 C103 C 0.941(3) 0.5412(6) 0.6544(11) 0.145(11) Uiso 0.50 1 d PD A 1 H10J H 0.9843 0.5505 0.6910 0.174 Uiso 0.50 1 calc PR A 1 H10K H 0.9252 0.5221 0.6640 0.174 Uiso 0.50 1 calc PR A 1 C104 C 1.0215(16) 0.5438(3) 0.6035(7) 0.053(5) Uiso 0.50 1 d PD A 1 H10L H 1.1183 0.5414 0.6174 0.064 Uiso 0.50 1 calc PR A 1 H10M H 0.9926 0.5306 0.5711 0.064 Uiso 0.50 1 calc PR A 1 C105 C 0.8217(18) 0.5708(4) 0.6144(12) 0.089(7) Uiso 0.50 1 d PD A 2 H10N H 0.8037 0.5626 0.6528 0.107 Uiso 0.50 1 calc PR A 2 H10O H 0.7812 0.5593 0.5806 0.107 Uiso 0.50 1 calc PR A 2 C106 C 0.764(2) 0.5984(4) 0.6082(10) 0.096(7) Uiso 0.50 1 d PD A 2 H10P H 0.8101 0.6101 0.6397 0.144 Uiso 0.50 1 calc PR A 2 H10Q H 0.6683 0.5976 0.6124 0.144 Uiso 0.50 1 calc PR A 2 H10R H 0.7741 0.6057 0.5684 0.144 Uiso 0.50 1 calc PR A 2 C107 C 1.020(5) 0.5548(7) 0.6616(14) 0.33(3) Uiso 0.50 1 d PD A 2 H10S H 0.9528 0.5512 0.6890 0.391 Uiso 0.50 1 calc PR A 2 H10T H 1.1011 0.5625 0.6853 0.391 Uiso 0.50 1 calc PR A 2 C108 C 1.052(4) 0.5299(6) 0.6300(16) 0.194(16) Uiso 0.50 1 d PD A 2 H10U H 1.0927 0.5347 0.5942 0.292 Uiso 0.50 1 calc PR A 2 H10V H 0.9696 0.5196 0.6179 0.292 Uiso 0.50 1 calc PR A 2 H10W H 1.1146 0.5189 0.6572 0.292 Uiso 0.50 1 calc PR A 2 Li1 Li 1.3174(15) 0.6326(3) 0.6980(6) 0.057(4) Uani 1 1 d . . . Li2 Li 1.1092(17) 0.5988(3) 0.5998(8) 0.086(6) Uani 1 1 d D . . H1A H 0.919(9) 0.9554(13) 0.643(3) 0.10(3) Uiso 1 1 d D . . H2A H 0.963(8) 0.7980(13) 0.5058(16) 0.08(3) Uiso 1 1 d 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 0.0270(3) 0.0573(4) 0.0501(3) -0.0041(3) 0.0009(2) -0.0027(3) I2 0.0267(3) 0.0452(3) 0.0422(3) -0.0003(3) 0.0042(2) 0.0014(2) I3 0.0766(5) 0.0576(4) 0.0780(5) -0.0097(3) -0.0049(4) 0.0190(4) I4 0.0779(5) 0.0717(5) 0.0825(5) 0.0180(4) 0.0018(4) 0.0300(4) Ga1 0.0274(5) 0.0343(5) 0.0322(5) -0.0012(4) -0.0004(4) -0.0042(4) Ga2 0.0269(5) 0.0291(4) 0.0257(4) 0.0008(4) 0.0022(3) 0.0023(4) P1 0.0384(13) 0.0416(13) 0.0407(12) -0.0074(10) 0.0101(10) -0.0067(10) P2 0.0299(11) 0.0322(11) 0.0341(11) 0.0040(9) -0.0005(9) 0.0017(9) O1 0.064(5) 0.095(5) 0.049(4) 0.016(3) 0.005(3) -0.002(4) O2 0.083(5) 0.066(4) 0.061(4) 0.018(3) 0.013(4) -0.004(4) O3 0.123(7) 0.097(6) 0.062(5) -0.002(4) -0.020(5) -0.026(5) N1 0.027(3) 0.028(4) 0.034(3) -0.003(3) 0.001(3) 0.002(3) N2 0.031(4) 0.038(4) 0.039(4) -0.006(3) -0.004(3) -0.002(3) N3 0.029(4) 0.030(3) 0.034(4) 0.001(3) 0.002(3) 0.004(3) N4 0.030(4) 0.024(3) 0.027(3) 0.004(3) 0.001(3) -0.002(3) C1 0.031(5) 0.049(5) 0.044(5) -0.015(4) -0.010(4) -0.003(4) C2 0.035(5) 0.030(4) 0.047(5) -0.004(4) 0.006(4) -0.006(4) C3 0.039(5) 0.033(4) 0.032(4) -0.005(4) -0.007(4) -0.002(4) C4 0.044(5) 0.038(5) 0.051(5) -0.009(4) -0.011(4) -0.002(4) C5 0.069(7) 0.036(5) 0.064(6) -0.002(5) -0.013(6) 0.013(5) C6 0.068(7) 0.066(7) 0.048(6) 0.013(5) -0.014(5) -0.005(6) C7 0.051(6) 0.075(7) 0.040(5) -0.001(5) 0.003(5) -0.027(5) C8 0.043(5) 0.049(5) 0.037(5) -0.001(4) 0.002(4) -0.007(4) C9 0.036(5) 0.087(7) 0.044(5) -0.015(5) -0.014(4) 0.012(5) C10 0.068(7) 0.108(9) 0.085(7) -0.038(6) -0.006(6) 0.055(7) C11 0.041(6) 0.117(9) 0.072(7) 0.002(6) 0.017(5) 0.002(6) C12 0.041(5) 0.065(6) 0.047(5) -0.014(4) 0.007(4) -0.010(5) C13 0.066(7) 0.099(8) 0.065(6) -0.030(6) 0.000(5) 0.021(6) C14 0.040(6) 0.113(8) 0.055(6) -0.001(6) -0.006(5) -0.025(6) C15 0.042(5) 0.038(5) 0.044(5) 0.005(4) -0.001(4) -0.009(4) C16 0.040(6) 0.061(6) 0.062(6) 0.008(5) 0.013(5) -0.010(5) C17 0.076(8) 0.075(7) 0.077(7) 0.014(6) 0.028(6) -0.009(6) C18 0.075(8) 0.086(8) 0.056(6) 0.028(6) 0.014(6) -0.017(6) C19 0.063(7) 0.052(6) 0.074(7) 0.021(5) -0.004(6) -0.010(5) C20 0.046(5) 0.047(5) 0.042(5) 0.009(4) 0.002(4) -0.004(4) C21 0.039(5) 0.051(6) 0.086(7) 0.011(5) 0.018(5) -0.003(5) C22 0.042(6) 0.082(7) 0.119(9) 0.002(7) 0.003(6) -0.007(5) C23 0.067(8) 0.097(8) 0.127(10) 0.004(7) 0.050(7) 0.006(7) C24 0.044(5) 0.038(5) 0.057(5) 0.007(4) 0.002(4) 0.002(4) C25 0.077(8) 0.044(6) 0.113(8) -0.008(6) 0.006(7) 0.006(5) C26 0.055(7) 0.087(8) 0.095(8) 0.028(6) -0.009(6) 0.000(6) C27 0.042(5) 0.033(4) 0.023(4) -0.005(3) 0.002(3) -0.006(4) C28 0.031(5) 0.036(5) 0.035(4) -0.008(4) 0.004(4) 0.005(4) C29 0.046(5) 0.030(4) 0.025(4) 0.003(3) 0.004(4) -0.001(4) C30 0.044(5) 0.028(4) 0.030(4) -0.004(4) -0.001(4) -0.001(4) C31 0.054(6) 0.039(5) 0.037(5) -0.003(4) -0.002(4) 0.005(4) C32 0.046(5) 0.032(4) 0.027(4) 0.000(3) 0.002(4) -0.008(4) C33 0.035(5) 0.036(5) 0.052(5) -0.006(4) -0.010(4) 0.000(4) C34 0.053(6) 0.053(5) 0.037(5) 0.001(4) -0.007(4) 0.004(4) C35 0.052(6) 0.051(6) 0.062(6) -0.005(5) -0.012(5) 0.015(5) C36 0.088(8) 0.037(5) 0.060(6) 0.020(4) -0.031(5) -0.007(5) C37 0.039(5) 0.047(5) 0.040(5) 0.000(4) 0.001(4) -0.006(4) C38 0.061(14) 0.042(12) 0.045(13) 0.014(10) -0.007(10) 0.009(10) C38A 0.051(12) 0.096(17) 0.083(14) -0.028(12) 0.028(10) -0.013(11) C39 0.038(12) 0.073(16) 0.051(13) 0.004(11) 0.021(10) -0.001(11) C39A 0.054(12) 0.052(12) 0.101(18) -0.010(11) -0.019(11) -0.005(9) C40 0.048(13) 0.070(16) 0.032(11) 0.009(10) 0.001(9) -0.027(11) C40A 0.048(12) 0.071(14) 0.079(15) 0.003(11) -0.006(10) -0.014(10) C41 0.095(8) 0.047(6) 0.032(5) 0.004(4) -0.004(5) -0.018(5) C42 0.109(9) 0.051(6) 0.063(6) 0.020(5) -0.008(6) -0.010(6) C43 0.109(9) 0.091(8) 0.050(6) -0.004(5) 0.036(6) -0.046(7) C44 0.109(7) 0.084(6) 0.051(5) 0.026(5) -0.010(5) -0.030(6) C45 0.036(5) 0.029(4) 0.038(5) 0.001(4) 0.010(4) -0.005(4) C46 0.021(4) 0.047(5) 0.024(4) 0.006(4) 0.001(3) 0.003(4) C47 0.042(5) 0.018(4) 0.024(4) -0.005(3) -0.001(4) 0.008(3) C48 0.038(5) 0.029(4) 0.030(4) 0.007(3) 0.008(4) 0.011(4) C49 0.047(6) 0.062(6) 0.046(5) -0.002(5) 0.021(4) 0.012(5) C50 0.054(6) 0.051(6) 0.046(5) -0.014(4) 0.001(5) 0.006(5) C51 0.046(6) 0.037(5) 0.051(5) -0.018(4) -0.001(4) -0.002(4) C52 0.042(5) 0.025(4) 0.030(4) 0.001(3) 0.006(4) 0.004(4) C53 0.034(5) 0.036(5) 0.056(5) 0.004(4) 0.014(4) -0.002(4) C54 0.041(5) 0.071(6) 0.057(6) 0.006(5) 0.007(4) 0.004(5) C55 0.049(6) 0.061(6) 0.065(6) 0.006(5) 0.026(5) -0.006(5) C56 0.039(5) 0.033(5) 0.051(5) -0.006(4) 0.006(4) -0.011(4) C57 0.098(9) 0.055(6) 0.101(8) 0.006(6) 0.054(7) -0.010(6) C58 0.041(6) 0.088(7) 0.077(7) -0.028(6) 0.009(5) -0.009(5) C59 0.032(5) 0.028(4) 0.029(4) 0.002(3) -0.006(3) 0.003(3) C60 0.030(4) 0.041(5) 0.025(4) -0.002(4) 0.004(3) 0.007(4) C61 0.045(6) 0.059(6) 0.038(5) -0.014(4) 0.005(4) 0.009(5) C62 0.052(6) 0.045(5) 0.045(5) -0.019(4) -0.014(5) 0.003(4) C63 0.045(5) 0.040(5) 0.036(5) -0.002(4) -0.002(4) -0.003(4) C64 0.033(5) 0.035(4) 0.032(4) 0.007(4) 0.005(4) 0.003(4) C65 0.028(5) 0.085(7) 0.028(4) -0.008(4) -0.002(4) -0.009(5) C66 0.054(6) 0.087(7) 0.060(6) 0.011(6) 0.016(5) -0.018(5) C67 0.038(6) 0.118(9) 0.054(6) -0.002(6) 0.011(5) 0.009(6) C68 0.025(4) 0.045(5) 0.038(4) 0.004(4) 0.003(4) -0.008(4) C69 0.043(6) 0.066(6) 0.061(6) 0.012(5) 0.010(5) -0.005(5) C70 0.037(5) 0.048(5) 0.052(5) 0.003(4) 0.013(4) 0.001(4) C71 0.029(4) 0.023(4) 0.034(4) 0.005(3) -0.001(3) -0.002(3) C72 0.038(5) 0.023(4) 0.035(4) 0.004(3) 0.003(4) 0.002(3) C73 0.044(5) 0.037(5) 0.024(4) -0.004(4) -0.005(4) 0.003(4) C74 0.036(5) 0.028(4) 0.035(4) 0.002(3) 0.006(4) 0.006(4) C75 0.043(5) 0.030(4) 0.035(4) 0.004(4) 0.005(4) 0.007(4) C76 0.040(5) 0.025(4) 0.028(4) 0.003(3) -0.003(4) -0.003(3) C77 0.045(5) 0.038(5) 0.028(4) 0.000(4) -0.001(4) 0.008(4) C78 0.057(6) 0.040(5) 0.049(5) -0.005(4) 0.006(4) 0.010(4) C79 0.066(6) 0.058(6) 0.039(5) 0.002(4) 0.020(5) 0.005(5) C80 0.075(7) 0.062(6) 0.033(5) -0.015(4) -0.009(5) 0.028(5) C81 0.024(4) 0.051(5) 0.062(6) -0.008(5) 0.005(4) 0.002(4) C82 0.029(8) 0.087(11) 0.150(18) 0.032(12) 0.022(9) 0.007(7) C83 0.054(9) 0.096(13) 0.059(9) 0.009(8) -0.019(7) 0.037(9) C84 0.070(8) 0.094(9) 0.086(9) -0.020(7) 0.012(7) 0.035(7) C85 0.050(5) 0.036(5) 0.036(5) -0.012(4) -0.010(4) 0.003(4) C86 0.075(7) 0.062(6) 0.056(6) -0.034(5) -0.014(5) 0.015(5) C87 0.106(9) 0.064(6) 0.035(5) 0.003(5) -0.022(5) -0.009(6) C88 0.057(6) 0.042(5) 0.067(6) -0.012(4) -0.008(5) -0.005(5) C89 0.099(8) 0.154(9) 0.091(7) 0.024(7) 0.023(6) 0.043(7) C90 0.139(9) 0.122(8) 0.154(9) 0.026(7) 0.043(8) -0.039(7) C91 0.156(10) 0.115(8) 0.169(9) 0.027(7) 0.002(8) 0.030(8) C92 0.106(8) 0.157(9) 0.104(7) 0.015(7) 0.008(7) 0.000(7) C93 0.102(8) 0.138(8) 0.132(8) 0.055(7) -0.003(7) -0.009(7) C94 0.123(9) 0.174(9) 0.126(8) 0.034(7) 0.039(7) 0.013(8) C95 0.099(7) 0.117(8) 0.106(7) 0.037(6) 0.028(6) 0.013(7) C96 0.111(8) 0.087(7) 0.101(7) 0.019(6) 0.032(6) 0.011(6) C97 0.143(9) 0.118(8) 0.106(8) 0.001(7) 0.005(7) -0.025(7) C98 0.149(9) 0.130(8) 0.105(8) -0.016(7) 0.015(7) -0.026(7) C99 0.140(9) 0.158(9) 0.119(8) 0.016(7) -0.005(7) -0.008(8) C100 0.081(7) 0.123(8) 0.092(7) 0.007(6) -0.002(6) 0.011(6) Li1 0.059(10) 0.056(9) 0.057(9) -0.002(8) 0.009(8) 0.011(8) Li2 0.081(13) 0.072(11) 0.092(13) 0.012(10) -0.038(11) -0.008(10) _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 2.5512(11) . ? I2 Ga2 2.5612(10) . ? I3 Li2 2.752(16) . ? I3 Li1 2.759(14) . ? I4 Li2 2.749(19) . ? I4 Li1 2.751(15) . ? Ga1 N2 1.972(6) . ? Ga1 N1 1.976(5) . ? Ga1 P1 2.337(2) . ? Ga2 N4 1.973(5) . ? Ga2 N3 1.976(5) . ? Ga2 P2 2.327(2) . ? P1 C27 1.852(7) . ? P2 C71 1.864(7) . ? O1 C92 1.381(13) . ? O1 C89 1.391(12) . ? O1 Li1 1.918(15) . ? O2 C96 1.413(11) . ? O2 C93 1.421(14) . ? O2 Li1 1.882(17) . ? O3 C100 1.375(11) . ? O3 C97 1.433(13) . ? O3 Li2 1.920(19) . ? O4 C104 1.374(14) . ? O4 C101 1.418(16) . ? O4 Li2 1.87(2) . ? O4A C107 1.453(19) . ? O4A C105 1.460(17) . ? O4A Li2 1.984(16) . ? N1 C1 1.347(9) . ? N1 C3 1.436(8) . ? N2 C2 1.324(8) . ? N2 C15 1.440(9) . ? N3 C45 1.336(8) . ? N3 C47 1.439(8) . ? N4 C46 1.330(8) . ? N4 C59 1.443(8) . ? C1 C2 1.402(10) . ? C3 C4 1.388(10) . ? C3 C8 1.390(10) . ? C4 C5 1.393(11) . ? C4 C9 1.528(12) . ? C5 C6 1.376(12) . ? C6 C7 1.366(12) . ? C7 C8 1.402(11) . ? C8 C12 1.511(11) . ? C9 C11 1.524(12) . ? C9 C10 1.527(11) . ? C12 C13 1.534(10) . ? C12 C14 1.539(11) . ? C15 C20 1.393(11) . ? C15 C16 1.397(11) . ? C16 C17 1.388(12) . ? C16 C21 1.539(11) . ? C17 C18 1.365(13) . ? C18 C19 1.376(13) . ? C19 C20 1.408(11) . ? C20 C24 1.506(11) . ? C21 C23 1.533(12) . ? C21 C22 1.542(12) . ? C24 C26 1.525(11) . ? C24 C25 1.539(11) . ? C27 C32 1.427(9) . ? C27 C28 1.443(9) . ? C28 C29 1.376(10) . ? C28 C33 1.555(10) . ? C29 C30 1.382(9) . ? C30 C31 1.396(10) . ? C30 C37 1.515(10) . ? C31 C32 1.395(10) . ? C32 C41 1.546(10) . ? C33 C35 1.525(11) . ? C33 C34 1.549(10) . ? C33 C36 1.552(10) . ? C37 C39A 1.480(17) . ? C37 C38A 1.500(17) . ? C37 C40 1.548(18) . ? C37 C38 1.556(19) . ? C37 C40A 1.565(17) . ? C37 C39 1.568(19) . ? C41 C43 1.529(13) . ? C41 C42 1.569(11) . ? C41 C44 1.572(11) . ? C45 C46 1.387(9) . ? C47 C52 1.402(9) . ? C47 C48 1.405(10) . ? C48 C49 1.399(10) . ? C48 C53 1.529(10) . ? C49 C50 1.366(11) . ? C50 C51 1.368(11) . ? C51 C52 1.400(9) . ? C52 C56 1.520(10) . ? C53 C54 1.535(10) . ? C53 C55 1.536(10) . ? C56 C58 1.516(11) . ? C56 C57 1.528(10) . ? C59 C60 1.386(9) . ? C59 C64 1.414(10) . ? C60 C61 1.403(10) . ? C60 C65 1.512(10) . ? C61 C62 1.381(11) . ? C62 C63 1.368(10) . ? C63 C64 1.386(9) . ? C64 C68 1.512(10) . ? C65 C67 1.514(11) . ? C65 C66 1.531(11) . ? C68 C69 1.530(10) . ? C68 C70 1.538(10) . ? C71 C72 1.424(9) . ? C71 C76 1.431(9) . ? C72 C73 1.385(10) . ? C72 C77 1.549(10) . ? C73 C74 1.390(9) . ? C74 C75 1.374(9) . ? C74 C81 1.529(10) . ? C75 C76 1.391(10) . ? C76 C85 1.565(9) . ? C77 C79 1.532(11) . ? C77 C78 1.542(9) . ? C77 C80 1.547(9) . ? C81 C82 1.489(15) . ? C81 C84A 1.50(3) . ? C81 C84 1.521(14) . ? C81 C83A 1.53(3) . ? C81 C83 1.533(14) . ? C81 C82A 1.56(3) . ? C85 C88 1.535(11) . ? C85 C87 1.542(10) . ? C85 C86 1.544(10) . ? C89 C90 1.439(15) . ? C90 C91 1.560(18) . ? C91 C92 1.434(16) . ? C93 C94 1.403(15) . ? C94 C95 1.504(15) . ? C95 C96 1.446(14) . ? C97 C98 1.420(14) . ? C98 C99 1.476(17) . ? C99 C100 1.462(15) . ? C101 C102 1.491(17) . ? C102 C103 1.554(17) . ? C103 C104 1.493(17) . ? C105 C106 1.488(17) . ? C107 C108 1.48(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 Li2 I3 Li1 73.2(5) . . ? Li2 I4 Li1 73.4(4) . . ? N2 Ga1 N1 84.0(2) . . ? N2 Ga1 P1 114.43(19) . . ? N1 Ga1 P1 123.97(17) . . ? N2 Ga1 I1 110.57(18) . . ? N1 Ga1 I1 106.69(17) . . ? P1 Ga1 I1 113.49(6) . . ? N4 Ga2 N3 84.2(2) . . ? N4 Ga2 P2 117.18(17) . . ? N3 Ga2 P2 121.25(18) . . ? N4 Ga2 I2 108.27(17) . . ? N3 Ga2 I2 106.92(17) . . ? P2 Ga2 I2 114.83(6) . . ? C27 P1 Ga1 102.0(2) . . ? C71 P2 Ga2 99.9(2) . . ? C92 O1 C89 106.9(8) . . ? C92 O1 Li1 123.6(9) . . ? C89 O1 Li1 126.8(8) . . ? C96 O2 C93 105.3(9) . . ? C96 O2 Li1 125.3(8) . . ? C93 O2 Li1 126.5(8) . . ? C100 O3 C97 109.6(9) . . ? C100 O3 Li2 127.5(9) . . ? C97 O3 Li2 120.3(8) . . ? C104 O4 C101 109.9(12) . . ? C104 O4 Li2 124.5(12) . . ? C101 O4 Li2 118.8(13) . . ? C107 O4A C105 102(2) . . ? C107 O4A Li2 108(2) . . ? C105 O4A Li2 143.3(14) . . ? C1 N1 C3 119.0(6) . . ? C1 N1 Ga1 109.1(5) . . ? C3 N1 Ga1 131.9(4) . . ? C2 N2 C15 120.6(6) . . ? C2 N2 Ga1 110.6(5) . . ? C15 N2 Ga1 128.9(5) . . ? C45 N3 C47 119.3(6) . . ? C45 N3 Ga2 108.9(5) . . ? C47 N3 Ga2 131.7(4) . . ? C46 N4 C59 119.7(5) . . ? C46 N4 Ga2 109.4(4) . . ? C59 N4 Ga2 130.6(4) . . ? N1 C1 C2 118.1(7) . . ? N2 C2 C1 117.2(7) . . ? C4 C3 C8 121.3(7) . . ? C4 C3 N1 117.8(7) . . ? C8 C3 N1 120.9(7) . . ? C3 C4 C5 119.1(9) . . ? C3 C4 C9 122.2(7) . . ? C5 C4 C9 118.6(8) . . ? C6 C5 C4 120.4(9) . . ? C7 C6 C5 119.9(8) . . ? C6 C7 C8 121.7(9) . . ? C3 C8 C7 117.6(8) . . ? C3 C8 C12 123.4(7) . . ? C7 C8 C12 119.0(8) . . ? C11 C9 C10 110.9(8) . . ? C11 C9 C4 109.3(7) . . ? C10 C9 C4 114.8(8) . . ? C8 C12 C13 110.4(7) . . ? C8 C12 C14 111.4(7) . . ? C13 C12 C14 109.5(7) . . ? C20 C15 C16 122.9(8) . . ? C20 C15 N2 119.4(7) . . ? C16 C15 N2 117.6(7) . . ? C17 C16 C15 117.9(9) . . ? C17 C16 C21 120.5(9) . . ? C15 C16 C21 121.4(8) . . ? C18 C17 C16 121.0(10) . . ? C17 C18 C19 120.2(9) . . ? C18 C19 C20 121.7(9) . . ? C15 C20 C19 116.1(8) . . ? C15 C20 C24 122.9(7) . . ? C19 C20 C24 120.9(8) . . ? C23 C21 C16 113.5(8) . . ? C23 C21 C22 110.5(8) . . ? C16 C21 C22 109.2(7) . . ? C20 C24 C26 113.4(7) . . ? C20 C24 C25 110.3(7) . . ? C26 C24 C25 109.9(7) . . ? C32 C27 C28 117.7(6) . . ? C32 C27 P1 123.0(5) . . ? C28 C27 P1 119.3(5) . . ? C29 C28 C27 118.3(6) . . ? C29 C28 C33 118.0(7) . . ? C27 C28 C33 123.7(6) . . ? C28 C29 C30 125.3(7) . . ? C29 C30 C31 115.0(7) . . ? C29 C30 C37 123.2(7) . . ? C31 C30 C37 121.7(7) . . ? C32 C31 C30 124.2(7) . . ? C31 C32 C27 118.5(7) . . ? C31 C32 C41 116.8(7) . . ? C27 C32 C41 124.7(7) . . ? C35 C33 C34 111.5(6) . . ? C35 C33 C36 106.3(7) . . ? C34 C33 C36 105.4(6) . . ? C35 C33 C28 110.9(6) . . ? C34 C33 C28 111.1(6) . . ? C36 C33 C28 111.5(6) . . ? C39A C37 C38A 113.8(13) . . ? C39A C37 C30 108.4(9) . . ? C38A C37 C30 103.9(9) . . ? C39A C37 C40 52.8(10) . . ? C38A C37 C40 145.5(11) . . ? C30 C37 C40 110.5(9) . . ? C39A C37 C38 138.4(11) . . ? C38A C37 C38 59.7(10) . . ? C30 C37 C38 113.0(9) . . ? C40 C37 C38 106.9(11) . . ? C39A C37 C40A 108.7(11) . . ? C38A C37 C40A 110.5(12) . . ? C30 C37 C40A 111.5(8) . . ? C40 C37 C40A 58.7(10) . . ? C38 C37 C40A 51.9(9) . . ? C39A C37 C39 59.4(11) . . ? C38A C37 C39 54.7(10) . . ? C30 C37 C39 115.7(9) . . ? C40 C37 C39 106.0(11) . . ? C38 C37 C39 104.0(11) . . ? C40A C37 C39 132.6(11) . . ? C43 C41 C32 112.3(7) . . ? C43 C41 C42 112.9(8) . . ? C32 C41 C42 110.8(7) . . ? C43 C41 C44 104.9(7) . . ? C32 C41 C44 112.0(7) . . ? C42 C41 C44 103.6(7) . . ? N3 C45 C46 118.3(6) . . ? N4 C46 C45 118.1(6) . . ? C52 C47 C48 121.1(6) . . ? C52 C47 N3 121.0(7) . . ? C48 C47 N3 117.9(6) . . ? C49 C48 C47 118.3(7) . . ? C49 C48 C53 120.9(7) . . ? C47 C48 C53 120.7(6) . . ? C50 C49 C48 120.6(8) . . ? C49 C50 C51 121.2(8) . . ? C50 C51 C52 120.7(7) . . ? C51 C52 C47 118.1(7) . . ? C51 C52 C56 120.0(7) . . ? C47 C52 C56 121.8(6) . . ? C48 C53 C54 110.3(6) . . ? C48 C53 C55 113.2(6) . . ? C54 C53 C55 110.7(7) . . ? C58 C56 C52 111.1(7) . . ? C58 C56 C57 110.5(7) . . ? C52 C56 C57 111.4(7) . . ? C60 C59 C64 122.7(6) . . ? C60 C59 N4 120.8(6) . . ? C64 C59 N4 116.5(7) . . ? C59 C60 C61 117.7(7) . . ? C59 C60 C65 122.4(6) . . ? C61 C60 C65 119.9(7) . . ? C62 C61 C60 120.7(8) . . ? C63 C62 C61 120.0(7) . . ? C62 C63 C64 122.4(8) . . ? C63 C64 C59 116.5(7) . . ? C63 C64 C68 120.3(7) . . ? C59 C64 C68 123.2(6) . . ? C60 C65 C67 112.3(7) . . ? C60 C65 C66 110.0(6) . . ? C67 C65 C66 112.0(7) . . ? C64 C68 C69 114.7(6) . . ? C64 C68 C70 109.8(6) . . ? C69 C68 C70 110.2(6) . . ? C72 C71 C76 119.7(6) . . ? C72 C71 P2 119.3(5) . . ? C76 C71 P2 121.0(5) . . ? C73 C72 C71 116.7(6) . . ? C73 C72 C77 117.8(6) . . ? C71 C72 C77 125.5(6) . . ? C72 C73 C74 125.1(7) . . ? C75 C74 C73 115.8(7) . . ? C75 C74 C81 122.6(7) . . ? C73 C74 C81 121.6(7) . . ? C74 C75 C76 124.3(7) . . ? C75 C76 C71 117.5(6) . . ? C75 C76 C85 116.7(6) . . ? C71 C76 C85 125.9(6) . . ? C79 C77 C78 111.8(7) . . ? C79 C77 C80 106.1(6) . . ? C78 C77 C80 104.9(6) . . ? C79 C77 C72 110.0(6) . . ? C78 C77 C72 112.0(6) . . ? C80 C77 C72 111.8(6) . . ? C82 C81 C84A 139.1(16) . . ? C82 C81 C84 109.6(10) . . ? C84A C81 C84 39.1(12) . . ? C82 C81 C74 109.0(8) . . ? C84A C81 C74 109.0(14) . . ? C84 C81 C74 113.8(8) . . ? C82 C81 C83A 63.8(15) . . ? C84A C81 C83A 111.9(19) . . ? C84 C81 C83A 130.3(16) . . ? C74 C81 C83A 114.6(15) . . ? C82 C81 C83 108.6(10) . . ? C84A C81 C83 72.0(14) . . ? C84 C81 C83 106.4(9) . . ? C74 C81 C83 109.3(8) . . ? C83A C81 C83 45.9(14) . . ? C82 C81 C82A 48.7(12) . . ? C84A C81 C82A 104.3(18) . . ? C84 C81 C82A 65.9(13) . . ? C74 C81 C82A 108.3(13) . . ? C83A C81 C82A 108.1(19) . . ? C83 C81 C82A 141.2(14) . . ? C88 C85 C87 112.9(7) . . ? C88 C85 C86 105.9(7) . . ? C87 C85 C86 105.4(7) . . ? C88 C85 C76 110.3(6) . . ? C87 C85 C76 110.6(6) . . ? C86 C85 C76 111.6(6) . . ? O1 C89 C90 107.8(11) . . ? C89 C90 C91 101.6(11) . . ? C92 C91 C90 105.1(11) . . ? O1 C92 C91 104.9(12) . . ? C94 C93 O2 111.3(11) . . ? C93 C94 C95 105.0(12) . . ? C96 C95 C94 105.5(10) . . ? O2 C96 C95 109.3(10) . . ? C98 C97 O3 107.3(11) . . ? C97 C98 C99 104.3(13) . . ? C100 C99 C98 108.4(12) . . ? O3 C100 C99 105.3(11) . . ? O4 C101 C102 104.1(13) . . ? C101 C102 C103 103.9(14) . . ? C104 C103 C102 100.8(14) . . ? O4 C104 C103 101.1(14) . . ? O4A C105 C106 107.8(17) . . ? O4A C107 C108 105(2) . . ? O2 Li1 O1 112.7(8) . . ? O2 Li1 I4 113.7(6) . . ? O1 Li1 I4 109.0(7) . . ? O2 Li1 I3 106.1(6) . . ? O1 Li1 I3 108.5(6) . . ? I4 Li1 I3 106.5(5) . . ? O4 Li2 O3 95.9(9) . . ? O4 Li2 O4A 22.2(6) . . ? O3 Li2 O4A 114.6(9) . . ? O4 Li2 I4 126.2(10) . . ? O3 Li2 I4 106.0(7) . . ? O4A Li2 I4 107.0(9) . . ? O4 Li2 I3 113.2(8) . . ? O3 Li2 I3 106.4(8) . . ? O4A Li2 I3 115.4(8) . . ? I4 Li2 I3 106.8(5) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.120 _refine_diff_density_min -1.225 _refine_diff_density_rms 0.122 data_compound_8 _database_code_depnum_ccdc_archive 'CCDC 280914' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H82 Ga N4 P' _chemical_formula_weight 875.92 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.127(2) _cell_length_b 18.270(4) _cell_length_c 24.459(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.49(3) _cell_angle_gamma 90.00 _cell_volume 4957.0(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.174 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 0.625 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.715 _exptl_absorpt_correction_T_max 0.874 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30202 _diffrn_reflns_av_R_equivalents 0.0819 _diffrn_reflns_av_sigmaI/netI 0.0789 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 25.34 _reflns_number_total 8967 _reflns_number_gt 6813 _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. The phosphine hydrogen atom, H(1), was located from difference maps and refined isotropically. Upon convergence of the structural refinement, close contacts between H1A and 2 methyl hydrogens of a supermesityl substituent were observed (H1A-H34C 1.90 ang., H1A-H35C 1.95 ang.). These close contacts occur because, although the position of P-H hydrogen can be considered as relatively accurate (through isotropic refinement), the methyl hydrogen atoms are in calculated positions (riding model) and thus their positions should not be regarded as accurate and the aforementioned H..H contacts should be disregarded. ; _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^)+(0.0526P)^2^+10.8205P] 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 8967 _refine_ls_number_parameters 555 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0991 _refine_ls_R_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.1581 _refine_ls_wR_factor_gt 0.1461 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.070 _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 0.27958(4) 0.80776(2) 0.179899(17) 0.02271(15) Uani 1 1 d . . . P1 P 0.25893(10) 0.75967(6) 0.08977(4) 0.0283(3) Uani 1 1 d . . . N1 N 0.3171(3) 0.91004(18) 0.18572(12) 0.0229(7) Uani 1 1 d . . . N2 N 0.1266(3) 0.82831(18) 0.20675(12) 0.0224(7) Uani 1 1 d . . . N3 N 0.3909(3) 0.7502(2) 0.23373(13) 0.0311(8) Uani 1 1 d . . . N4 N 0.5176(4) 0.7378(2) 0.31462(16) 0.0565(13) Uani 1 1 d . . . C1 C 0.2178(4) 0.9447(2) 0.20744(16) 0.0274(9) Uani 1 1 d . . . H1 H 0.2186 0.9959 0.2144 0.033 Uiso 1 1 calc R . . C2 C 0.1226(4) 0.9037(2) 0.21796(15) 0.0256(9) Uani 1 1 d . . . H2 H 0.0541 0.9249 0.2326 0.031 Uiso 1 1 calc R . . C3 C 0.3968(4) 0.9523(2) 0.15532(15) 0.0234(9) Uani 1 1 d . . . C4 C 0.5204(4) 0.9543(2) 0.17369(16) 0.0272(9) Uani 1 1 d . . . C5 C 0.5999(4) 0.9935(3) 0.14370(19) 0.0373(11) Uani 1 1 d . . . H5 H 0.6830 0.9949 0.1559 0.045 Uiso 1 1 calc R . . C6 C 0.5594(4) 1.0308(3) 0.0959(2) 0.0436(12) Uani 1 1 d . . . H6 H 0.6145 1.0572 0.0755 0.052 Uiso 1 1 calc R . . C7 C 0.4395(4) 1.0289(3) 0.07876(18) 0.0380(11) Uani 1 1 d . . . H7 H 0.4124 1.0547 0.0464 0.046 Uiso 1 1 calc R . . C8 C 0.3551(4) 0.9904(2) 0.10714(16) 0.0277(9) Uani 1 1 d . . . C9 C 0.5654(4) 0.9184(2) 0.22705(17) 0.0295(10) Uani 1 1 d . . . H9 H 0.5092 0.8772 0.2335 0.035 Uiso 1 1 calc R . . C10 C 0.6920(4) 0.8859(3) 0.22768(19) 0.0411(11) Uani 1 1 d . . . H10A H 0.6970 0.8538 0.1958 0.062 Uiso 1 1 calc R . . H10B H 0.7092 0.8575 0.2614 0.062 Uiso 1 1 calc R . . H10C H 0.7511 0.9255 0.2263 0.062 Uiso 1 1 calc R . . C11 C 0.5565(5) 0.9728(3) 0.27381(19) 0.0446(12) Uani 1 1 d . . . H11A H 0.6115 1.0138 0.2692 0.067 Uiso 1 1 calc R . . H11B H 0.5784 0.9484 0.3089 0.067 Uiso 1 1 calc R . . H11C H 0.4736 0.9911 0.2735 0.067 Uiso 1 1 calc R . . C12 C 0.2248(4) 0.9902(2) 0.08494(17) 0.0324(10) Uani 1 1 d . . . H12 H 0.1809 0.9542 0.1069 0.039 Uiso 1 1 calc R . . C13 C 0.2096(5) 0.9658(3) 0.02439(18) 0.0474(13) Uani 1 1 d . . . H13A H 0.2528 0.9998 0.0019 0.071 Uiso 1 1 calc R . . H13B H 0.1238 0.9658 0.0118 0.071 Uiso 1 1 calc R . . H13C H 0.2425 0.9164 0.0210 0.071 Uiso 1 1 calc R . . C14 C 0.1662(4) 1.0653(3) 0.0913(2) 0.0417(12) Uani 1 1 d . . . H14A H 0.1732 1.0796 0.1300 0.063 Uiso 1 1 calc R . . H14B H 0.0809 1.0628 0.0780 0.063 Uiso 1 1 calc R . . H14C H 0.2072 1.1017 0.0698 0.063 Uiso 1 1 calc R . . C15 C 0.0170(3) 0.7878(2) 0.19688(16) 0.0245(9) Uani 1 1 d . . . C16 C -0.0554(4) 0.7947(2) 0.14662(16) 0.0287(10) Uani 1 1 d . . . C17 C -0.1555(4) 0.7500(3) 0.13763(18) 0.0364(11) Uani 1 1 d . . . H17 H -0.2038 0.7542 0.1040 0.044 Uiso 1 1 calc R . . C18 C -0.1874(4) 0.6995(3) 0.17605(18) 0.0356(11) Uani 1 1 d . . . H18 H -0.2559 0.6690 0.1687 0.043 Uiso 1 1 calc R . . C19 C -0.1181(4) 0.6941(2) 0.22505(18) 0.0316(10) Uani 1 1 d . . . H19 H -0.1402 0.6599 0.2517 0.038 Uiso 1 1 calc R . . C20 C -0.0171(4) 0.7374(2) 0.23653(16) 0.0273(9) Uani 1 1 d . . . C21 C -0.0263(4) 0.8504(3) 0.10351(17) 0.0332(10) Uani 1 1 d . . . H21 H 0.0615 0.8620 0.1094 0.040 Uiso 1 1 calc R . . C22 C -0.0959(4) 0.9215(3) 0.1102(2) 0.0432(12) Uani 1 1 d . . . H22A H -0.1826 0.9118 0.1048 0.065 Uiso 1 1 calc R . . H22B H -0.0732 0.9572 0.0829 0.065 Uiso 1 1 calc R . . H22C H -0.0764 0.9412 0.1471 0.065 Uiso 1 1 calc R . . C23 C -0.0502(4) 0.8222(3) 0.04447(17) 0.0435(12) Uani 1 1 d . . . H23A H -0.0147 0.7734 0.0415 0.065 Uiso 1 1 calc R . . H23B H -0.0138 0.8557 0.0192 0.065 Uiso 1 1 calc R . . H23C H -0.1374 0.8195 0.0350 0.065 Uiso 1 1 calc R . . C24 C 0.0541(4) 0.7317(2) 0.29172(17) 0.0320(10) Uani 1 1 d . . . H24 H 0.1259 0.7645 0.2908 0.038 Uiso 1 1 calc R . . C25 C 0.0990(7) 0.6565(4) 0.3046(3) 0.083(2) Uani 1 1 d U . . H25A H 0.1443 0.6564 0.3406 0.125 Uiso 1 1 calc R . . H25B H 0.1517 0.6408 0.2765 0.125 Uiso 1 1 calc R . . H25C H 0.0305 0.6229 0.3050 0.125 Uiso 1 1 calc R . . C26 C -0.0193(7) 0.7585(5) 0.3362(3) 0.101(2) Uani 1 1 d U . . H26A H 0.0272 0.7533 0.3717 0.152 Uiso 1 1 calc R . . H26B H -0.0935 0.7296 0.3362 0.152 Uiso 1 1 calc R . . H26C H -0.0398 0.8101 0.3298 0.152 Uiso 1 1 calc R . . C27 C 0.3556(4) 0.6788(2) 0.07901(16) 0.0284(10) Uani 1 1 d . . . C28 C 0.3218(4) 0.6064(2) 0.09335(17) 0.0323(10) Uani 1 1 d . . . C29 C 0.4117(4) 0.5523(2) 0.09823(17) 0.0330(10) Uani 1 1 d . . . H29 H 0.3903 0.5048 0.1100 0.040 Uiso 1 1 calc R . . C30 C 0.5302(4) 0.5648(2) 0.08674(16) 0.0293(10) Uani 1 1 d . . . C31 C 0.5554(4) 0.6324(2) 0.06481(16) 0.0287(9) Uani 1 1 d . . . H31 H 0.6342 0.6409 0.0537 0.034 Uiso 1 1 calc R . . C32 C 0.4705(4) 0.6888(2) 0.05819(15) 0.0269(9) Uani 1 1 d . . . C33 C 0.1906(4) 0.5830(3) 0.1024(2) 0.0429(12) Uani 1 1 d . . . C34 C 0.1055(5) 0.6048(3) 0.0521(2) 0.0565(15) Uani 1 1 d . . . H34A H 0.0224 0.5918 0.0588 0.085 Uiso 1 1 calc R . . H34B H 0.1291 0.5787 0.0196 0.085 Uiso 1 1 calc R . . H34C H 0.1109 0.6577 0.0461 0.085 Uiso 1 1 calc R . . C35 C 0.1491(5) 0.6127(3) 0.1569(2) 0.0611(16) Uani 1 1 d . . . H35A H 0.2027 0.5943 0.1875 0.092 Uiso 1 1 calc R . . H35B H 0.0664 0.5965 0.1612 0.092 Uiso 1 1 calc R . . H35C H 0.1517 0.6664 0.1565 0.092 Uiso 1 1 calc R . . C36 C 0.1786(5) 0.4987(3) 0.1068(3) 0.0651(17) Uani 1 1 d . . . H36A H 0.2305 0.4811 0.1383 0.098 Uiso 1 1 calc R . . H36B H 0.2031 0.4759 0.0732 0.098 Uiso 1 1 calc R . . H36C H 0.0946 0.4860 0.1117 0.098 Uiso 1 1 calc R . . C37 C 0.6243(4) 0.5033(3) 0.09511(17) 0.0359(11) Uani 1 1 d . . . C38 C 0.6361(5) 0.4826(3) 0.15660(19) 0.0496(13) Uani 1 1 d . . . H38A H 0.6675 0.5245 0.1783 0.074 Uiso 1 1 calc R . . H38B H 0.6916 0.4411 0.1623 0.074 Uiso 1 1 calc R . . H38C H 0.5568 0.4689 0.1682 0.074 Uiso 1 1 calc R . . C39 C 0.5823(5) 0.4360(3) 0.0620(2) 0.0523(14) Uani 1 1 d . . . H39A H 0.5052 0.4190 0.0742 0.078 Uiso 1 1 calc R . . H39B H 0.6425 0.3970 0.0676 0.078 Uiso 1 1 calc R . . H39C H 0.5721 0.4486 0.0230 0.078 Uiso 1 1 calc R . . C40 C 0.7485(4) 0.5259(3) 0.0782(2) 0.0493(13) Uani 1 1 d . . . H40A H 0.7421 0.5397 0.0393 0.074 Uiso 1 1 calc R . . H40B H 0.8047 0.4848 0.0839 0.074 Uiso 1 1 calc R . . H40C H 0.7783 0.5678 0.1004 0.074 Uiso 1 1 calc R . . C41 C 0.5065(4) 0.7577(2) 0.02589(17) 0.0293(9) Uani 1 1 d . . . C42 C 0.5355(5) 0.8237(3) 0.0639(2) 0.0450(12) Uani 1 1 d . . . H42A H 0.5660 0.8641 0.0425 0.068 Uiso 1 1 calc R . . H42B H 0.5968 0.8096 0.0929 0.068 Uiso 1 1 calc R . . H42C H 0.4622 0.8393 0.0803 0.068 Uiso 1 1 calc R . . C43 C 0.4079(4) 0.7763(2) -0.01987(17) 0.0329(10) Uani 1 1 d . . . H43A H 0.3328 0.7885 -0.0035 0.049 Uiso 1 1 calc R . . H43B H 0.3944 0.7341 -0.0442 0.049 Uiso 1 1 calc R . . H43C H 0.4338 0.8183 -0.0410 0.049 Uiso 1 1 calc R . . C44 C 0.6200(4) 0.7432(3) -0.00518(18) 0.0382(11) Uani 1 1 d . . . H44A H 0.6356 0.7856 -0.0281 0.057 Uiso 1 1 calc R . . H44B H 0.6070 0.6998 -0.0284 0.057 Uiso 1 1 calc R . . H44C H 0.6895 0.7351 0.0213 0.057 Uiso 1 1 calc R . . C45 C 0.4224(5) 0.7679(3) 0.28407(18) 0.0408(12) Uani 1 1 d . . . C46 C 0.3554(4) 0.8277(3) 0.31313(17) 0.0374(11) Uani 1 1 d . . . H46A H 0.4062 0.8721 0.3172 0.045 Uiso 1 1 calc R . . H46B H 0.2802 0.8405 0.2909 0.045 Uiso 1 1 calc R . . C47 C 0.3256(5) 0.8012(3) 0.36897(18) 0.0473(13) Uani 1 1 d . . . H47A H 0.2519 0.8277 0.3777 0.057 Uiso 1 1 calc R . . H47B H 0.3028 0.7491 0.3646 0.057 Uiso 1 1 calc R . . C48 C 0.4089(6) 0.8056(4) 0.4176(3) 0.0757(19) Uani 1 1 d . . . H48A H 0.3671 0.7910 0.4501 0.091 Uiso 1 1 calc R . . H48B H 0.4366 0.8568 0.4229 0.091 Uiso 1 1 calc R . . C49 C 0.5161(6) 0.7567(4) 0.4124(3) 0.083(2) Uani 1 1 d . . . H49A H 0.5724 0.7626 0.4455 0.099 Uiso 1 1 calc R . . H49B H 0.4885 0.7052 0.4111 0.099 Uiso 1 1 calc R . . C50 C 0.5815(7) 0.7716(4) 0.3635(3) 0.080(2) Uani 1 1 d . . . H50A H 0.6642 0.7515 0.3689 0.096 Uiso 1 1 calc R . . H50B H 0.5877 0.8251 0.3580 0.096 Uiso 1 1 calc R . . C51 C 0.5733(6) 0.6695(3) 0.2989(2) 0.0692(18) Uani 1 1 d . . . H51A H 0.5801 0.6357 0.3307 0.083 Uiso 1 1 calc R . . H51B H 0.6556 0.6794 0.2880 0.083 Uiso 1 1 calc R . . C52 C 0.4992(5) 0.6340(3) 0.25183(19) 0.0546(15) Uani 1 1 d . . . H52A H 0.5468 0.5956 0.2348 0.066 Uiso 1 1 calc R . . H52B H 0.4261 0.6111 0.2650 0.066 Uiso 1 1 calc R . . C53 C 0.4649(5) 0.6933(3) 0.21107(19) 0.0458(12) Uani 1 1 d . . . H53A H 0.5391 0.7158 0.1988 0.055 Uiso 1 1 calc R . . H53B H 0.4199 0.6714 0.1786 0.055 Uiso 1 1 calc R . . H1A H 0.148(7) 0.736(4) 0.096(3) 0.12(3) Uiso 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 Ga1 0.0248(2) 0.0216(3) 0.0219(2) 0.00419(19) 0.00333(16) 0.00094(19) P1 0.0340(6) 0.0253(6) 0.0260(6) 0.0002(5) 0.0054(4) 0.0033(5) N1 0.0268(18) 0.0225(19) 0.0194(16) 0.0002(14) 0.0025(13) -0.0019(14) N2 0.0235(17) 0.0242(19) 0.0199(16) 0.0019(14) 0.0039(13) 0.0017(14) N3 0.036(2) 0.033(2) 0.0237(19) 0.0041(16) 0.0030(15) 0.0023(16) N4 0.082(3) 0.052(3) 0.033(2) -0.003(2) -0.018(2) 0.026(2) C1 0.036(2) 0.024(2) 0.023(2) -0.0024(18) 0.0056(17) 0.0021(18) C2 0.028(2) 0.029(2) 0.021(2) -0.0017(17) 0.0069(16) 0.0037(18) C3 0.034(2) 0.017(2) 0.021(2) -0.0015(16) 0.0100(16) -0.0010(17) C4 0.031(2) 0.021(2) 0.030(2) -0.0018(18) 0.0045(17) -0.0012(17) C5 0.032(2) 0.034(3) 0.047(3) 0.002(2) 0.012(2) -0.001(2) C6 0.051(3) 0.037(3) 0.046(3) 0.015(2) 0.024(2) -0.001(2) C7 0.051(3) 0.033(3) 0.031(2) 0.012(2) 0.010(2) 0.003(2) C8 0.041(2) 0.019(2) 0.024(2) -0.0003(17) 0.0072(18) -0.0008(18) C9 0.029(2) 0.029(2) 0.030(2) 0.0008(19) 0.0014(17) -0.0017(18) C10 0.042(3) 0.043(3) 0.037(3) -0.003(2) 0.001(2) 0.010(2) C11 0.052(3) 0.043(3) 0.039(3) -0.004(2) 0.003(2) 0.007(2) C12 0.044(3) 0.028(3) 0.024(2) 0.0053(19) -0.0015(18) 0.000(2) C13 0.068(4) 0.045(3) 0.028(2) 0.003(2) -0.004(2) 0.006(3) C14 0.045(3) 0.038(3) 0.041(3) 0.003(2) -0.001(2) 0.009(2) C15 0.022(2) 0.024(2) 0.028(2) -0.0004(17) 0.0070(16) 0.0025(16) C16 0.025(2) 0.035(3) 0.026(2) 0.0040(19) 0.0007(16) 0.0018(18) C17 0.033(2) 0.042(3) 0.032(2) -0.001(2) -0.0046(19) -0.001(2) C18 0.028(2) 0.037(3) 0.042(3) -0.005(2) 0.0049(19) -0.0058(19) C19 0.035(2) 0.026(2) 0.036(2) 0.000(2) 0.0137(18) 0.003(2) C20 0.027(2) 0.027(2) 0.029(2) -0.0014(18) 0.0067(17) 0.0019(18) C21 0.028(2) 0.046(3) 0.026(2) 0.009(2) 0.0001(17) -0.001(2) C22 0.040(3) 0.044(3) 0.045(3) 0.016(2) 0.000(2) 0.005(2) C23 0.044(3) 0.062(4) 0.024(2) 0.008(2) 0.0000(19) -0.004(2) C24 0.038(3) 0.032(3) 0.026(2) 0.0071(19) 0.0053(18) -0.003(2) C25 0.100(4) 0.068(4) 0.075(3) 0.010(3) -0.032(3) 0.004(3) C26 0.102(4) 0.132(5) 0.068(4) -0.020(3) 0.000(3) 0.034(4) C27 0.033(2) 0.030(3) 0.022(2) -0.0010(18) 0.0023(17) 0.0043(18) C28 0.039(3) 0.028(3) 0.032(2) 0.0006(19) 0.0117(19) 0.0011(19) C29 0.052(3) 0.020(2) 0.028(2) 0.0035(18) 0.0075(19) 0.003(2) C30 0.039(3) 0.028(2) 0.020(2) -0.0035(18) -0.0004(17) 0.0047(19) C31 0.034(2) 0.030(3) 0.022(2) -0.0042(18) 0.0005(17) 0.0014(19) C32 0.034(2) 0.026(2) 0.021(2) -0.0060(18) 0.0041(16) -0.0024(19) C33 0.045(3) 0.032(3) 0.055(3) 0.000(2) 0.021(2) -0.005(2) C34 0.042(3) 0.051(4) 0.076(4) -0.011(3) 0.004(3) -0.008(3) C35 0.064(4) 0.054(4) 0.071(4) -0.001(3) 0.040(3) -0.005(3) C36 0.063(4) 0.039(3) 0.098(5) 0.004(3) 0.039(3) -0.009(3) C37 0.046(3) 0.033(3) 0.028(2) -0.002(2) -0.0038(19) 0.010(2) C38 0.062(3) 0.053(3) 0.032(3) 0.005(2) -0.007(2) 0.018(3) C39 0.070(4) 0.031(3) 0.052(3) -0.009(2) -0.017(3) 0.018(3) C40 0.044(3) 0.047(3) 0.057(3) -0.003(3) 0.006(2) 0.016(2) C41 0.032(2) 0.028(2) 0.027(2) -0.0008(18) 0.0015(17) -0.0039(18) C42 0.065(3) 0.029(3) 0.041(3) -0.003(2) 0.001(2) -0.003(2) C43 0.044(3) 0.027(2) 0.029(2) 0.0073(19) 0.0095(19) 0.001(2) C44 0.039(3) 0.040(3) 0.037(3) 0.005(2) 0.007(2) -0.007(2) C45 0.058(3) 0.035(3) 0.029(3) 0.006(2) 0.005(2) 0.000(2) C46 0.053(3) 0.033(3) 0.026(2) -0.0031(19) 0.006(2) 0.001(2) C47 0.077(4) 0.039(3) 0.027(2) 0.000(2) 0.011(2) 0.006(3) C48 0.085(5) 0.082(5) 0.061(4) 0.003(4) 0.012(3) 0.003(4) C49 0.071(4) 0.078(5) 0.103(6) 0.002(4) 0.030(4) 0.002(4) C50 0.091(5) 0.091(5) 0.055(4) 0.004(4) -0.005(3) 0.004(4) C51 0.085(4) 0.066(4) 0.053(4) 0.005(3) -0.015(3) 0.035(3) C52 0.077(4) 0.056(4) 0.030(3) 0.000(2) 0.000(2) 0.030(3) C53 0.063(3) 0.041(3) 0.034(3) -0.001(2) 0.008(2) 0.020(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 N2 1.909(3) . ? Ga1 N1 1.918(3) . ? Ga1 N3 2.029(3) . ? Ga1 P1 2.3675(12) . ? P1 C27 1.859(4) . ? P1 H1A 1.33(7) . ? N1 C1 1.413(5) . ? N1 C3 1.427(5) . ? N2 C2 1.405(5) . ? N2 C15 1.431(5) . ? N3 C45 1.294(6) . ? N3 C53 1.463(6) . ? N4 C45 1.363(6) . ? N4 C51 1.458(7) . ? N4 C50 1.477(7) . ? C1 C2 1.339(6) . ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? C3 C4 1.414(6) . ? C3 C8 1.415(6) . ? C4 C5 1.391(6) . ? C4 C9 1.511(6) . ? C5 C6 1.398(7) . ? C5 H5 0.9500 . ? C6 C7 1.367(7) . ? C6 H6 0.9500 . ? C7 C8 1.400(6) . ? C7 H7 0.9500 . ? C8 C12 1.507(6) . ? C9 C11 1.524(6) . ? C9 C10 1.528(6) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C14 1.533(6) . ? C12 C13 1.543(6) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C20 1.410(6) . ? C15 C16 1.422(6) . ? C16 C17 1.384(6) . ? C16 C21 1.519(6) . ? C17 C18 1.383(6) . ? C17 H17 0.9500 . ? C18 C19 1.377(6) . ? C18 H18 0.9500 . ? C19 C20 1.385(6) . ? C19 H19 0.9500 . ? C20 C24 1.514(6) . ? C21 C22 1.528(6) . ? C21 C23 1.537(6) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.487(8) . ? C24 C26 1.492(8) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C32 1.424(6) . ? C27 C28 1.427(6) . ? C28 C29 1.404(6) . ? C28 C33 1.554(6) . ? C29 C30 1.389(6) . ? C29 H29 0.9500 . ? C30 C31 1.384(6) . ? C30 C37 1.538(6) . ? C31 C32 1.398(6) . ? C31 H31 0.9500 . ? C32 C41 1.555(6) . ? C33 C35 1.544(7) . ? C33 C34 1.544(7) . ? C33 C36 1.549(7) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C39 1.526(6) . ? C37 C40 1.530(7) . ? C37 C38 1.547(6) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.541(6) . ? C41 C43 1.543(6) . ? C41 C44 1.547(6) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.529(6) . ? C46 C47 1.509(6) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.451(8) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.503(9) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.473(9) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.510(8) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.502(7) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? 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 88.72(13) . . ? N2 Ga1 N3 113.20(14) . . ? N1 Ga1 N3 109.76(14) . . ? N2 Ga1 P1 111.67(10) . . ? N1 Ga1 P1 115.81(10) . . ? N3 Ga1 P1 114.96(11) . . ? C27 P1 Ga1 114.32(13) . . ? C27 P1 H1A 108(3) . . ? Ga1 P1 H1A 92(3) . . ? C1 N1 C3 119.3(3) . . ? C1 N1 Ga1 107.0(2) . . ? C3 N1 Ga1 129.0(2) . . ? C2 N2 C15 120.0(3) . . ? C2 N2 Ga1 107.6(2) . . ? C15 N2 Ga1 127.7(3) . . ? C45 N3 C53 114.8(4) . . ? C45 N3 Ga1 126.5(3) . . ? C53 N3 Ga1 117.1(3) . . ? C45 N4 C51 121.9(4) . . ? C45 N4 C50 125.4(5) . . ? C51 N4 C50 112.5(5) . . ? C2 C1 N1 118.3(4) . . ? C2 C1 H1 120.8 . . ? N1 C1 H1 120.8 . . ? C1 C2 N2 118.3(4) . . ? C1 C2 H2 120.9 . . ? N2 C2 H2 120.9 . . ? C4 C3 C8 120.0(4) . . ? C4 C3 N1 118.5(3) . . ? C8 C3 N1 121.6(4) . . ? C5 C4 C3 119.3(4) . . ? C5 C4 C9 119.8(4) . . ? C3 C4 C9 120.8(4) . . ? C4 C5 C6 121.1(4) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C7 C6 C5 119.1(4) . . ? C7 C6 H6 120.5 . . ? C5 C6 H6 120.5 . . ? C6 C7 C8 122.5(4) . . ? C6 C7 H7 118.7 . . ? C8 C7 H7 118.7 . . ? C7 C8 C3 118.1(4) . . ? C7 C8 C12 119.1(4) . . ? C3 C8 C12 122.8(4) . . ? C4 C9 C11 109.2(4) . . ? C4 C9 C10 114.9(4) . . ? C11 C9 C10 111.1(4) . . ? C4 C9 H9 107.1 . . ? C11 C9 H9 107.1 . . ? C10 C9 H9 107.1 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C8 C12 C14 111.5(4) . . ? C8 C12 C13 112.1(4) . . ? C14 C12 C13 109.8(4) . . ? C8 C12 H12 107.7 . . ? C14 C12 H12 107.7 . . ? C13 C12 H12 107.7 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C15 C16 119.2(4) . . ? C20 C15 N2 119.5(3) . . ? C16 C15 N2 121.2(3) . . ? C17 C16 C15 118.7(4) . . ? C17 C16 C21 119.8(4) . . ? C15 C16 C21 121.5(4) . . ? C18 C17 C16 122.1(4) . . ? C18 C17 H17 118.9 . . ? C16 C17 H17 118.9 . . ? C19 C18 C17 118.9(4) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C18 C19 C20 121.7(4) . . ? C18 C19 H19 119.1 . . ? C20 C19 H19 119.1 . . ? C19 C20 C15 119.4(4) . . ? C19 C20 C24 120.1(4) . . ? C15 C20 C24 120.5(4) . . ? C16 C21 C22 111.1(4) . . ? C16 C21 C23 113.4(4) . . ? C22 C21 C23 109.5(4) . . ? C16 C21 H21 107.5 . . ? C22 C21 H21 107.5 . . ? C23 C21 H21 107.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C26 110.0(5) . . ? C25 C24 C20 113.3(4) . . ? C26 C24 C20 110.4(4) . . ? C25 C24 H24 107.6 . . ? C26 C24 H24 107.6 . . ? C20 C24 H24 107.6 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C32 C27 C28 117.9(4) . . ? C32 C27 P1 119.6(3) . . ? C28 C27 P1 122.4(3) . . ? C29 C28 C27 118.3(4) . . ? C29 C28 C33 117.7(4) . . ? C27 C28 C33 124.0(4) . . ? C30 C29 C28 123.2(4) . . ? C30 C29 H29 118.4 . . ? C28 C29 H29 118.4 . . ? C31 C30 C29 116.7(4) . . ? C31 C30 C37 123.1(4) . . ? C29 C30 C37 120.0(4) . . ? C30 C31 C32 123.1(4) . . ? C30 C31 H31 118.4 . . ? C32 C31 H31 118.4 . . ? C31 C32 C27 118.8(4) . . ? C31 C32 C41 117.1(4) . . ? C27 C32 C41 124.0(4) . . ? C35 C33 C34 112.9(4) . . ? C35 C33 C36 104.9(4) . . ? C34 C33 C36 105.1(4) . . ? C35 C33 C28 112.0(4) . . ? C34 C33 C28 109.9(4) . . ? C36 C33 C28 111.8(4) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C39 C37 C40 108.7(4) . . ? C39 C37 C30 109.9(4) . . ? C40 C37 C30 112.8(4) . . ? C39 C37 C38 108.5(4) . . ? C40 C37 C38 108.7(4) . . ? C30 C37 C38 108.3(4) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C43 111.6(4) . . ? C42 C41 C44 106.8(4) . . ? C43 C41 C44 104.1(3) . . ? C42 C41 C32 112.2(3) . . ? C43 C41 C32 110.5(3) . . ? C44 C41 C32 111.4(3) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N3 C45 N4 124.2(4) . . ? N3 C45 C46 121.0(4) . . ? N4 C45 C46 114.8(4) . . ? C47 C46 C45 110.0(4) . . ? C47 C46 H46A 109.7 . . ? C45 C46 H46A 109.7 . . ? C47 C46 H46B 109.7 . . ? C45 C46 H46B 109.7 . . ? H46A C46 H46B 108.2 . . ? C48 C47 C46 123.5(5) . . ? C48 C47 H47A 106.5 . . ? C46 C47 H47A 106.5 . . ? C48 C47 H47B 106.5 . . ? C46 C47 H47B 106.5 . . ? H47A C47 H47B 106.5 . . ? C47 C48 C49 111.0(6) . . ? C47 C48 H48A 109.4 . . ? C49 C48 H48A 109.4 . . ? C47 C48 H48B 109.4 . . ? C49 C48 H48B 109.4 . . ? H48A C48 H48B 108.0 . . ? C50 C49 C48 113.8(6) . . ? C50 C49 H49A 108.8 . . ? C48 C49 H49A 108.8 . . ? C50 C49 H49B 108.8 . . ? C48 C49 H49B 108.8 . . ? H49A C49 H49B 107.7 . . ? C49 C50 N4 110.0(6) . . ? C49 C50 H50A 109.7 . . ? N4 C50 H50A 109.7 . . ? C49 C50 H50B 109.7 . . ? N4 C50 H50B 109.7 . . ? H50A C50 H50B 108.2 . . ? N4 C51 C52 110.5(4) . . ? N4 C51 H51A 109.5 . . ? C52 C51 H51A 109.5 . . ? N4 C51 H51B 109.5 . . ? C52 C51 H51B 109.5 . . ? H51A C51 H51B 108.1 . . ? C53 C52 C51 106.9(5) . . ? C53 C52 H52A 110.3 . . ? C51 C52 H52A 110.3 . . ? C53 C52 H52B 110.3 . . ? C51 C52 H52B 110.3 . . ? H52A C52 H52B 108.6 . . ? N3 C53 C52 112.5(4) . . ? N3 C53 H53A 109.1 . . ? C52 C53 H53A 109.1 . . ? N3 C53 H53B 109.1 . . ? C52 C53 H53B 109.1 . . ? H53A C53 H53B 107.8 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.383 #(near Ga1) _refine_diff_density_min -0.597 _refine_diff_density_rms 0.076