# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Bradley Holliday' _publ_contact_author_email bholliday@cm.utexas.edu _publ_section_title ; Gallium-containing conducting metallopolymers which display chemically tunable reactivity for the growth of Ga2S3 semiconducting nanoparticles ; loop_ _publ_author_name 'Michelle Mejia' 'Gregor Reeske' 'Bradley Holliday' # Attachment 'complex-2.CIF.txt' data_grgr065 _database_code_depnum_ccdc_archive 'CCDC 770626' #TrackingRef 'complex-2.CIF.txt' _audit_creation_method ; manual editing of the .cif file created by SHELXTL Ver. 6.10 ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H28 Cl Ga N2 O2 S4, 2(C H2 Cl2)' _chemical_formula_sum 'C37 H32 Cl5 Ga N2 O2 S4' _chemical_formula_weight 911.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 _symmetry_space_group_name_Hall -p1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.418(5) _cell_length_b 13.039(5) _cell_length_c 17.289(5) _cell_angle_alpha 92.035(5) _cell_angle_beta 97.726(5) _cell_angle_gamma 97.726(5) _cell_volume 2081.6(15) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 12554 _cell_measurement_theta_min 1.92 _cell_measurement_theta_max 27.5 _exptl_crystal_description plate _exptl_crystal_colour orange _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 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 1.217 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.803 _exptl_absorpt_correction_T_max 0.907 _exptl_absorpt_process_details 'DENZO and Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71069 _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 \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12554 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0565 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8199 _reflns_number_gt 5927 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _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. Data is 94.6% up to 50 degrees. ; _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^+2.0930P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8199 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0762 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1326 _refine_ls_wR_factor_gt 0.1145 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6510(4) 0.3834(3) 0.9121(2) 0.0492(10) Uani 1 1 d . . . C2 C 0.8154(4) 0.4113(3) 0.8940(2) 0.0468(9) Uani 1 1 d . . . H2A H 0.8283 0.4766 0.8666 0.056 Uiso 1 1 calc R . . H2B H 0.8855 0.4174 0.9426 0.056 Uiso 1 1 calc R . . C3 C 0.5668(4) 0.2600(3) 0.9031(2) 0.0450(9) Uani 1 1 d . . . H3A H 0.4746 0.2556 0.9251 0.054 Uiso 1 1 calc R . . H3B H 0.5449 0.2362 0.8472 0.054 Uiso 1 1 calc R . . C4 C 0.6570(5) 0.4277(3) 0.9959(2) 0.0633(12) Uani 1 1 d . . . H4A H 0.7006 0.5007 0.9998 0.095 Uiso 1 1 calc R . . H4B H 0.7156 0.3885 1.0319 0.095 Uiso 1 1 calc R . . H4C H 0.5588 0.4225 1.0096 0.095 Uiso 1 1 calc R . . C5 C 0.5591(6) 0.4321(4) 0.8541(3) 0.0752(15) Uani 1 1 d . . . H5A H 0.4584 0.4179 0.8638 0.113 Uiso 1 1 calc R . . H5B H 0.5670 0.4041 0.8017 0.113 Uiso 1 1 calc R . . H5C H 0.5901 0.5072 0.8577 0.113 Uiso 1 1 calc R . . C6 C 0.8376(4) 0.3346(3) 0.7715(2) 0.0434(9) Uani 1 1 d . . . H6 H 0.8351 0.4022 0.7531 0.052 Uiso 1 1 calc R . . C7 C 0.8484(4) 0.2534(3) 0.7159(2) 0.0403(8) Uani 1 1 d . . . C8 C 0.8605(4) 0.1522(3) 0.7370(2) 0.0390(8) Uani 1 1 d . . . C9 C 0.8737(4) 0.0821(3) 0.6779(2) 0.0421(8) Uani 1 1 d . . . H9 H 0.8844 0.0129 0.6903 0.051 Uiso 1 1 calc R . . C10 C 0.8719(4) 0.1087(3) 0.6011(2) 0.0428(8) Uani 1 1 d . . . H10 H 0.8801 0.0570 0.5624 0.051 Uiso 1 1 calc R . . C11 C 0.8586(4) 0.2080(3) 0.5788(2) 0.0395(8) Uani 1 1 d . . . C12 C 0.8479(4) 0.2784(3) 0.6378(2) 0.0418(8) Uani 1 1 d . . . H12 H 0.8398 0.3478 0.6251 0.050 Uiso 1 1 calc R . . C13 C 0.6149(4) 0.1544(3) 1.0056(2) 0.0410(8) Uani 1 1 d . . . H13 H 0.5291 0.1735 1.0217 0.049 Uiso 1 1 calc R . . C14 C 0.6815(4) 0.0853(3) 1.0493(2) 0.0379(8) Uani 1 1 d . . . C15 C 0.7810(4) 0.0393(2) 1.0175(2) 0.0387(8) Uani 1 1 d . . . C16 C 0.8336(4) -0.0319(3) 1.0635(2) 0.0447(9) Uani 1 1 d . . . H16 H 0.9044 -0.0686 1.0454 0.054 Uiso 1 1 calc R . . C17 C 0.7921(4) -0.0554(3) 1.1350(2) 0.0431(9) Uani 1 1 d . . . H17 H 0.8377 -0.1060 1.1634 0.052 Uiso 1 1 calc R . . C18 C 0.6916(4) -0.0115(3) 1.1670(2) 0.0385(8) Uani 1 1 d . . . C19 C 0.6384(4) 0.0581(3) 1.1220(2) 0.0399(8) Uani 1 1 d . . . H19 H 0.5653 0.0926 1.1399 0.048 Uiso 1 1 calc R . . C20 C 0.8525(4) 0.2355(3) 0.4974(2) 0.0419(8) Uani 1 1 d . . . C21 C 0.8445(4) 0.1738(3) 0.4304(2) 0.0481(9) Uani 1 1 d . . . H21 H 0.8481 0.1014 0.4309 0.058 Uiso 1 1 calc R . . C22 C 0.8306(4) 0.2263(3) 0.3614(2) 0.0499(9) Uani 1 1 d . . . H22 H 0.8233 0.1937 0.3107 0.060 Uiso 1 1 calc R . . C23 C 0.8287(4) 0.3296(3) 0.3751(2) 0.0450(9) Uani 1 1 d . . . C24 C 0.8150(4) 0.4093(3) 0.3213(2) 0.0484(9) Uani 1 1 d . . . C25 C 0.7999(4) 0.5083(3) 0.3373(2) 0.0546(10) Uani 1 1 d . . . H25 H 0.7962 0.5363 0.3884 0.066 Uiso 1 1 calc R . . C26 C 0.7901(5) 0.5662(4) 0.2703(2) 0.0633(12) Uani 1 1 d . . . H26 H 0.7790 0.6375 0.2716 0.076 Uiso 1 1 calc R . . C27 C 0.7978(5) 0.5113(4) 0.2043(3) 0.0663(12) Uani 1 1 d . . . H27 H 0.7924 0.5387 0.1540 0.080 Uiso 1 1 calc R . . C28 C 0.6424(4) -0.0392(3) 1.2422(2) 0.0386(8) Uani 1 1 d . C . C29 C 0.5213(4) -0.0263(3) 1.2722(2) 0.0480(9) Uani 1 1 d . . . H29 H 0.4462 0.0042 1.2433 0.058 Uiso 1 1 calc R . . C30 C 0.5097(4) -0.0598(3) 1.3480(2) 0.0473(9) Uani 1 1 d . . . H30 H 0.4292 -0.0530 1.3745 0.057 Uiso 1 1 calc R . . C31 C 0.6209(4) -0.1006(3) 1.3772(2) 0.0412(8) Uani 1 1 d . C . C32 C 0.6480(4) -0.1363(3) 1.4546(2) 0.0425(8) Uani 1 1 d . . . C34 C 0.6273(5) -0.1800(3) 1.5864(2) 0.0624(12) Uani 1 1 d . . . H34 H 0.5891 -0.1903 1.6341 0.075 Uiso 1 1 calc R A 1 C35 C 0.7577(5) -0.1927(3) 1.5717(3) 0.0636(12) Uani 1 1 d . C . H35 H 0.8242 -0.2169 1.6108 0.076 Uiso 1 1 calc R B 1 C36 C 0.8124(5) -0.1585(3) 0.8501(2) 0.0613(12) Uani 1 1 d . . . H36A H 0.8124 -0.0832 0.8441 0.074 Uiso 1 1 calc R . . H36B H 0.8547 -0.1687 0.9044 0.074 Uiso 1 1 calc R . . C37 C 0.5982(5) -0.4624(4) 0.6281(3) 0.0762(14) Uani 1 1 d . . . H37A H 0.5610 -0.4164 0.5882 0.091 Uiso 1 1 calc R . . H37B H 0.5688 -0.4398 0.6781 0.091 Uiso 1 1 calc R . . N1 N 0.8309(3) 0.3234(2) 0.84431(16) 0.0417(7) Uani 1 1 d . . . N2 N 0.6572(3) 0.1978(2) 0.94298(16) 0.0392(7) Uani 1 1 d . . . O1 O 0.8577(3) 0.11970(18) 0.80896(14) 0.0455(6) Uani 1 1 d . . . O2 O 0.8203(3) 0.05756(18) 0.94801(14) 0.0444(6) Uani 1 1 d . . . S1 S 0.81810(13) 0.38815(10) 0.22191(6) 0.0664(3) Uani 1 1 d . . . S2 S 0.84444(11) 0.36163(7) 0.47444(5) 0.0489(3) Uani 1 1 d . . . S3 S 0.74048(10) -0.09779(7) 1.30917(5) 0.0456(2) Uani 1 1 d . . . S4A S 0.8032(4) -0.1674(4) 1.4891(3) 0.0494(8) Uani 0.514(5) 1 d P C 1 C33A C 0.549(3) -0.145(2) 1.5092(16) 0.0525(10) Uani 0.514(5) 1 d P C 1 H33A H 0.4521 -0.1313 1.5002 0.063 Uiso 0.514(5) 1 calc PR C 1 S4B S 0.5344(8) -0.1406(6) 1.5210(4) 0.0525(10) Uani 0.486(5) 1 d P C 2 C33B C 0.774(2) -0.165(2) 1.4841(17) 0.0494(8) Uani 0.486(5) 1 d P C 2 H33B H 0.8559 -0.1677 1.4582 0.059 Uiso 0.486(5) 1 calc PR C 2 Cl1 Cl 1.06178(11) 0.28614(8) 0.97611(6) 0.0573(3) Uani 1 1 d . . . Cl2 Cl 0.61376(14) -0.23130(10) 0.82865(9) 0.0843(4) Uani 1 1 d . . . Cl3 Cl 0.90998(16) -0.20561(14) 0.78733(9) 0.1008(5) Uani 1 1 d . . . Cl4 Cl 0.79378(15) -0.43679(10) 0.63912(10) 0.0932(5) Uani 1 1 d . . . Cl5 Cl 0.49695(16) -0.59996(10) 0.60005(11) 0.0966(5) Uani 1 1 d . . . Ga1 Ga 0.84283(4) 0.19037(3) 0.90097(2) 0.03870(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.072(3) 0.044(2) 0.0402(19) 0.0038(16) 0.0065(18) 0.0386(19) C2 0.068(3) 0.0340(19) 0.0420(19) -0.0018(15) 0.0025(18) 0.0261(18) C3 0.049(2) 0.045(2) 0.046(2) -0.0002(16) -0.0016(16) 0.0326(17) C4 0.096(3) 0.047(2) 0.057(2) -0.0016(19) 0.025(2) 0.033(2) C5 0.095(4) 0.070(3) 0.074(3) 0.021(2) 0.006(3) 0.060(3) C6 0.053(2) 0.040(2) 0.043(2) 0.0074(16) 0.0106(17) 0.0263(17) C7 0.045(2) 0.0397(19) 0.0406(19) 0.0054(15) 0.0058(15) 0.0204(16) C8 0.0398(19) 0.0403(19) 0.0411(19) 0.0017(15) 0.0069(15) 0.0199(15) C9 0.0418(19) 0.040(2) 0.051(2) 0.0036(16) 0.0119(16) 0.0222(16) C10 0.0398(19) 0.043(2) 0.051(2) -0.0017(16) 0.0137(16) 0.0180(16) C11 0.0350(18) 0.043(2) 0.0447(19) 0.0041(16) 0.0086(15) 0.0164(15) C12 0.045(2) 0.040(2) 0.045(2) 0.0060(16) 0.0094(16) 0.0190(16) C13 0.0397(19) 0.0354(19) 0.053(2) 0.0004(16) 0.0079(16) 0.0212(15) C14 0.0377(18) 0.0355(18) 0.0461(19) 0.0041(15) 0.0100(15) 0.0205(15) C15 0.0410(19) 0.0308(18) 0.050(2) 0.0047(15) 0.0130(16) 0.0170(15) C16 0.044(2) 0.044(2) 0.055(2) 0.0095(17) 0.0191(17) 0.0285(17) C17 0.042(2) 0.041(2) 0.054(2) 0.0106(16) 0.0120(17) 0.0249(16) C18 0.0343(18) 0.0390(19) 0.047(2) 0.0049(15) 0.0103(15) 0.0171(15) C19 0.0371(18) 0.0380(19) 0.050(2) 0.0024(16) 0.0109(16) 0.0211(15) C20 0.0363(19) 0.047(2) 0.046(2) 0.0008(16) 0.0084(15) 0.0157(16) C21 0.049(2) 0.049(2) 0.051(2) -0.0028(18) 0.0140(17) 0.0178(18) C22 0.051(2) 0.058(2) 0.043(2) -0.0074(18) 0.0094(17) 0.0160(19) C23 0.041(2) 0.059(2) 0.0368(19) 0.0011(17) 0.0051(15) 0.0144(17) C24 0.043(2) 0.069(3) 0.0370(19) 0.0033(18) 0.0073(16) 0.0177(19) C25 0.056(2) 0.066(3) 0.046(2) 0.0075(19) 0.0059(18) 0.025(2) C26 0.062(3) 0.077(3) 0.056(3) 0.012(2) 0.004(2) 0.033(2) C27 0.063(3) 0.091(3) 0.049(2) 0.015(2) 0.001(2) 0.034(2) C28 0.0395(19) 0.0362(19) 0.0447(19) 0.0045(15) 0.0080(15) 0.0190(15) C29 0.039(2) 0.055(2) 0.057(2) 0.0102(18) 0.0118(17) 0.0260(17) C30 0.038(2) 0.057(2) 0.054(2) 0.0076(18) 0.0165(17) 0.0235(17) C31 0.0386(19) 0.043(2) 0.047(2) 0.0030(16) 0.0109(16) 0.0172(15) C32 0.048(2) 0.0365(19) 0.047(2) 0.0045(16) 0.0097(17) 0.0165(16) C34 0.090(3) 0.052(3) 0.050(2) 0.0037(19) 0.026(2) 0.014(2) C35 0.067(3) 0.052(3) 0.073(3) 0.013(2) -0.006(2) 0.021(2) C36 0.070(3) 0.068(3) 0.055(2) -0.001(2) 0.011(2) 0.043(2) C37 0.082(3) 0.055(3) 0.098(4) -0.004(3) 0.019(3) 0.028(2) N1 0.0527(18) 0.0370(16) 0.0408(16) 0.0005(12) 0.0051(13) 0.0275(14) N2 0.0424(16) 0.0339(15) 0.0456(17) 0.0004(13) 0.0030(13) 0.0241(13) O1 0.0577(15) 0.0439(14) 0.0436(14) 0.0081(11) 0.0102(11) 0.0348(12) O2 0.0562(15) 0.0417(14) 0.0472(14) 0.0107(11) 0.0207(12) 0.0345(12) S1 0.0761(8) 0.0894(9) 0.0398(5) 0.0027(5) 0.0055(5) 0.0361(7) S2 0.0641(6) 0.0479(6) 0.0400(5) 0.0026(4) 0.0118(4) 0.0219(5) S3 0.0456(5) 0.0514(6) 0.0488(5) 0.0092(4) 0.0137(4) 0.0304(4) S4A 0.050(2) 0.0538(11) 0.0527(13) 0.0118(9) 0.0095(16) 0.0321(14) C33A 0.054(2) 0.0629(14) 0.047(2) 0.0040(15) 0.0188(13) 0.0223(11) S4B 0.054(2) 0.0629(14) 0.047(2) 0.0040(15) 0.0188(13) 0.0223(11) C33B 0.050(2) 0.0538(11) 0.0527(13) 0.0118(9) 0.0095(16) 0.0321(14) Cl1 0.0563(6) 0.0492(6) 0.0640(6) 0.0074(5) -0.0105(5) 0.0163(5) Cl2 0.0685(8) 0.0798(8) 0.1141(11) -0.0008(7) 0.0224(7) 0.0362(6) Cl3 0.0878(9) 0.1380(13) 0.0872(9) -0.0343(9) 0.0228(7) 0.0541(9) Cl4 0.0756(8) 0.0541(7) 0.1485(13) 0.0065(7) -0.0080(8) 0.0279(6) Cl5 0.0896(10) 0.0562(8) 0.1473(14) -0.0171(8) 0.0331(9) 0.0118(7) Ga1 0.0434(2) 0.0358(2) 0.0421(2) 0.00499(16) 0.00660(17) 0.02275(17) _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 C1 C5 1.455(5) . ? C1 C4 1.532(5) . ? C1 C2 1.617(6) . ? C1 C3 1.688(6) . ? C2 N1 1.443(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N2 1.387(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 N1 1.281(4) . ? C6 C7 1.428(5) . ? C6 H6 0.9500 . ? C7 C8 1.396(5) . ? C7 C12 1.398(5) . ? C8 O1 1.331(4) . ? C8 C9 1.376(5) . ? C9 C10 1.382(5) . ? C9 H9 0.9500 . ? C10 C11 1.381(5) . ? C10 H10 0.9500 . ? C11 C12 1.371(5) . ? C11 C20 1.460(5) . ? C12 H12 0.9500 . ? C13 N2 1.323(5) . ? C13 C14 1.360(4) . ? C13 H13 0.9500 . ? C14 C15 1.345(4) . ? C14 C19 1.414(5) . ? C15 O2 1.323(4) . ? C15 C16 1.345(4) . ? C16 C17 1.378(5) . ? C16 H16 0.9500 . ? C17 C18 1.339(4) . ? C17 H17 0.9500 . ? C18 C19 1.322(4) . ? C18 C28 1.479(5) . ? C19 H19 0.9500 . ? C20 C21 1.375(5) . ? C20 S2 1.715(4) . ? C21 C22 1.396(5) . ? C21 H21 0.9500 . ? C22 C23 1.362(5) . ? C22 H22 0.9500 . ? C23 C24 1.427(5) . ? C23 S2 1.735(4) . ? C24 C25 1.340(5) . ? C24 S1 1.736(4) . ? C25 C26 1.405(6) . ? C25 H25 0.9500 . ? C26 C27 1.340(6) . ? C26 H26 0.9500 . ? C27 S1 1.676(5) . ? C27 H27 0.9500 . ? C28 C29 1.341(5) . ? C28 S3 1.656(3) . ? C29 C30 1.410(5) . ? C29 H29 0.9500 . ? C30 C31 1.289(4) . ? C30 H30 0.9500 . ? C31 C32 1.433(5) . ? C31 S3 1.733(4) . ? C32 C33B 1.328(18) . ? C32 C33A 1.41(2) . ? C32 S4A 1.613(4) . ? C32 S4B 1.669(6) . ? C34 C35 1.318(6) . ? C34 S4B 1.484(10) . ? C34 C33A 1.55(3) . ? C34 H34 0.9500 . ? C35 S4A 1.578(8) . ? C35 C33B 1.59(3) . ? C35 H35 0.9500 . ? C36 Cl3 1.665(4) . ? C36 Cl2 1.962(5) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 Cl4 1.810(5) . ? C37 Cl5 1.928(5) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? N1 Ga1 2.031(3) . ? N2 Ga1 1.994(3) . ? O1 Ga1 1.841(2) . ? O2 Ga1 1.937(2) . ? C33A H33A 0.9500 . ? C33B H33B 0.9500 . ? Cl1 Ga1 2.4436(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 C1 C4 114.1(3) . . ? C5 C1 C2 107.1(3) . . ? C4 C1 C2 103.8(3) . . ? C5 C1 C3 101.2(3) . . ? C4 C1 C3 110.1(3) . . ? C2 C1 C3 121.1(2) . . ? N1 C2 C1 102.2(3) . . ? N1 C2 H2A 111.3 . . ? C1 C2 H2A 111.3 . . ? N1 C2 H2B 111.3 . . ? C1 C2 H2B 111.3 . . ? H2A C2 H2B 109.2 . . ? N2 C3 C1 108.6(3) . . ? N2 C3 H3A 110.0 . . ? C1 C3 H3A 110.0 . . ? N2 C3 H3B 110.0 . . ? C1 C3 H3B 110.0 . . ? H3A C3 H3B 108.4 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C1 C5 H5A 109.5 . . ? C1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C7 125.1(3) . . ? N1 C6 H6 117.4 . . ? C7 C6 H6 117.4 . . ? C8 C7 C12 120.0(3) . . ? C8 C7 C6 122.4(3) . . ? C12 C7 C6 117.6(3) . . ? O1 C8 C9 118.8(3) . . ? O1 C8 C7 124.7(3) . . ? C9 C8 C7 116.5(3) . . ? C8 C9 C10 122.4(3) . . ? C8 C9 H9 118.8 . . ? C10 C9 H9 118.8 . . ? C11 C10 C9 122.0(3) . . ? C11 C10 H10 119.0 . . ? C9 C10 H10 119.0 . . ? C12 C11 C10 115.6(3) . . ? C12 C11 C20 122.2(3) . . ? C10 C11 C20 122.1(3) . . ? C11 C12 C7 123.4(3) . . ? C11 C12 H12 118.3 . . ? C7 C12 H12 118.3 . . ? N2 C13 C14 126.8(3) . . ? N2 C13 H13 116.6 . . ? C14 C13 H13 116.6 . . ? C15 C14 C13 116.9(3) . . ? C15 C14 C19 122.3(3) . . ? C13 C14 C19 120.7(3) . . ? O2 C15 C14 125.0(3) . . ? O2 C15 C16 123.0(3) . . ? C14 C15 C16 111.9(3) . . ? C15 C16 C17 124.8(3) . . ? C15 C16 H16 117.6 . . ? C17 C16 H16 117.6 . . ? C18 C17 C16 124.1(3) . . ? C18 C17 H17 118.0 . . ? C16 C17 H17 118.0 . . ? C19 C18 C17 111.7(3) . . ? C19 C18 C28 123.8(3) . . ? C17 C18 C28 124.4(3) . . ? C18 C19 C14 125.3(3) . . ? C18 C19 H19 117.4 . . ? C14 C19 H19 117.4 . . ? C21 C20 C11 130.3(3) . . ? C21 C20 S2 110.0(3) . . ? C11 C20 S2 119.6(3) . . ? C20 C21 C22 114.6(3) . . ? C20 C21 H21 122.7 . . ? C22 C21 H21 122.7 . . ? C23 C22 C21 112.2(3) . . ? C23 C22 H22 123.9 . . ? C21 C22 H22 123.9 . . ? C22 C23 C24 129.9(3) . . ? C22 C23 S2 111.2(3) . . ? C24 C23 S2 118.9(3) . . ? C25 C24 C23 127.5(4) . . ? C25 C24 S1 110.1(3) . . ? C23 C24 S1 122.4(3) . . ? C24 C25 C26 112.6(4) . . ? C24 C25 H25 123.7 . . ? C26 C25 H25 123.7 . . ? C27 C26 C25 113.8(4) . . ? C27 C26 H26 123.1 . . ? C25 C26 H26 123.1 . . ? C26 C27 S1 111.4(3) . . ? C26 C27 H27 124.3 . . ? S1 C27 H27 124.3 . . ? C29 C28 C18 132.0(3) . . ? C29 C28 S3 105.7(3) . . ? C18 C28 S3 122.4(2) . . ? C28 C29 C30 117.6(3) . . ? C28 C29 H29 121.2 . . ? C30 C29 H29 121.2 . . ? C31 C30 C29 112.3(3) . . ? C31 C30 H30 123.9 . . ? C29 C30 H30 123.9 . . ? C30 C31 C32 126.6(3) . . ? C30 C31 S3 108.4(3) . . ? C32 C31 S3 124.8(3) . . ? C33B C32 C33A 111.2(19) . . ? C33B C32 C31 123.0(13) . . ? C33A C32 C31 125.7(14) . . ? C33A C32 S4A 112.6(14) . . ? C31 C32 S4A 121.6(4) . . ? C33B C32 S4B 111.1(13) . . ? S4A C32 S4B 112.4(4) . . ? C35 C34 S4B 114.9(4) . . ? C35 C34 C33A 105.3(10) . . ? C35 C34 H34 127.3 . . ? S4B C34 H34 117.7 . . ? C33A C34 H34 127.3 . . ? C34 C35 S4A 119.8(3) . . ? C34 C35 C33B 109.5(7) . . ? C34 C35 H35 120.1 . . ? S4A C35 H35 120.1 . . ? C33B C35 H35 130.4 . . ? Cl3 C36 Cl2 108.6(2) . . ? Cl3 C36 H36A 110.0 . . ? Cl2 C36 H36A 110.0 . . ? Cl3 C36 H36B 110.0 . . ? Cl2 C36 H36B 110.0 . . ? H36A C36 H36B 108.4 . . ? Cl4 C37 Cl5 121.0(2) . . ? Cl4 C37 H37A 107.1 . . ? Cl5 C37 H37A 107.1 . . ? Cl4 C37 H37B 107.1 . . ? Cl5 C37 H37B 107.1 . . ? H37A C37 H37B 106.8 . . ? C6 N1 C2 119.7(3) . . ? C6 N1 Ga1 126.3(2) . . ? C2 N1 Ga1 114.1(2) . . ? C13 N2 C3 117.5(3) . . ? C13 N2 Ga1 127.4(2) . . ? C3 N2 Ga1 115.0(3) . . ? C8 O1 Ga1 130.7(2) . . ? C15 O2 Ga1 126.7(2) . . ? C27 S1 C24 92.2(2) . . ? C20 S2 C23 91.99(18) . . ? C28 S3 C31 96.02(17) . . ? C35 S4A C32 94.1(3) . . ? C32 C33A C34 108(2) . . ? C32 C33A H33A 126.0 . . ? C34 C33A H33A 126.0 . . ? C34 S4B C32 98.7(4) . . ? C32 C33B C35 105.8(17) . . ? C32 C33B H33B 127.1 . . ? C35 C33B H33B 127.1 . . ? O1 Ga1 O2 87.65(10) . . ? O1 Ga1 N2 124.27(12) . . ? O2 Ga1 N2 80.41(10) . . ? O1 Ga1 N1 90.64(11) . . ? O2 Ga1 N1 170.40(11) . . ? N2 Ga1 N1 92.80(11) . . ? O1 Ga1 Cl1 118.78(9) . . ? O2 Ga1 Cl1 104.35(8) . . ? N2 Ga1 Cl1 116.92(9) . . ? N1 Ga1 Cl1 84.74(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C1 C2 N1 -93.2(3) . . . . ? C4 C1 C2 N1 145.8(3) . . . . ? C3 C1 C2 N1 21.8(4) . . . . ? C5 C1 C3 N2 167.8(3) . . . . ? C4 C1 C3 N2 -71.2(4) . . . . ? C2 C1 C3 N2 49.8(4) . . . . ? N1 C6 C7 C8 -3.4(6) . . . . ? N1 C6 C7 C12 177.2(4) . . . . ? C12 C7 C8 O1 -178.0(3) . . . . ? C6 C7 C8 O1 2.7(6) . . . . ? C12 C7 C8 C9 1.0(5) . . . . ? C6 C7 C8 C9 -178.4(3) . . . . ? O1 C8 C9 C10 177.5(3) . . . . ? C7 C8 C9 C10 -1.5(5) . . . . ? C8 C9 C10 C11 0.9(6) . . . . ? C9 C10 C11 C12 0.3(5) . . . . ? C9 C10 C11 C20 -178.2(3) . . . . ? C10 C11 C12 C7 -0.7(5) . . . . ? C20 C11 C12 C7 177.7(3) . . . . ? C8 C7 C12 C11 0.1(6) . . . . ? C6 C7 C12 C11 179.6(3) . . . . ? N2 C13 C14 C15 -15.4(6) . . . . ? N2 C13 C14 C19 169.5(3) . . . . ? C13 C14 C15 O2 1.3(6) . . . . ? C19 C14 C15 O2 176.3(3) . . . . ? C13 C14 C15 C16 -176.3(3) . . . . ? C19 C14 C15 C16 -1.2(5) . . . . ? O2 C15 C16 C17 -177.9(4) . . . . ? C14 C15 C16 C17 -0.3(6) . . . . ? C15 C16 C17 C18 1.4(7) . . . . ? C16 C17 C18 C19 -0.7(6) . . . . ? C16 C17 C18 C28 177.5(4) . . . . ? C17 C18 C19 C14 -0.8(6) . . . . ? C28 C18 C19 C14 -179.0(3) . . . . ? C15 C14 C19 C18 1.9(6) . . . . ? C13 C14 C19 C18 176.8(4) . . . . ? C12 C11 C20 C21 -171.5(4) . . . . ? C10 C11 C20 C21 6.8(6) . . . . ? C12 C11 C20 S2 4.7(5) . . . . ? C10 C11 C20 S2 -177.0(3) . . . . ? C11 C20 C21 C22 175.9(4) . . . . ? S2 C20 C21 C22 -0.6(4) . . . . ? C20 C21 C22 C23 0.3(5) . . . . ? C21 C22 C23 C24 -179.4(4) . . . . ? C21 C22 C23 S2 0.1(4) . . . . ? C22 C23 C24 C25 173.1(4) . . . . ? S2 C23 C24 C25 -6.3(6) . . . . ? C22 C23 C24 S1 -7.6(6) . . . . ? S2 C23 C24 S1 172.9(2) . . . . ? C23 C24 C25 C26 179.7(4) . . . . ? S1 C24 C25 C26 0.4(5) . . . . ? C24 C25 C26 C27 0.0(6) . . . . ? C25 C26 C27 S1 -0.3(5) . . . . ? C19 C18 C28 C29 19.1(6) . . . . ? C17 C18 C28 C29 -158.9(4) . . . . ? C19 C18 C28 S3 -161.0(3) . . . . ? C17 C18 C28 S3 21.0(5) . . . . ? C18 C28 C29 C30 -178.2(4) . . . . ? S3 C28 C29 C30 1.9(4) . . . . ? C28 C29 C30 C31 -1.1(5) . . . . ? C29 C30 C31 C32 175.8(4) . . . . ? C29 C30 C31 S3 -0.3(4) . . . . ? C30 C31 C32 C33B -170.7(15) . . . . ? S3 C31 C32 C33B 4.8(16) . . . . ? C30 C31 C32 C33A 8.4(17) . . . . ? S3 C31 C32 C33A -176.1(16) . . . . ? C30 C31 C32 S4A -169.2(4) . . . . ? S3 C31 C32 S4A 6.3(5) . . . . ? C30 C31 C32 S4B 5.0(7) . . . . ? S3 C31 C32 S4B -179.5(4) . . . . ? S4B C34 C35 S4A -0.7(7) . . . . ? C33A C34 C35 S4A 2.3(13) . . . . ? S4B C34 C35 C33B -2.2(12) . . . . ? C33A C34 C35 C33B 0.8(17) . . . . ? C7 C6 N1 C2 -178.0(3) . . . . ? C7 C6 N1 Ga1 2.9(5) . . . . ? C1 C2 N1 C6 109.1(4) . . . . ? C1 C2 N1 Ga1 -71.7(3) . . . . ? C14 C13 N2 C3 174.8(3) . . . . ? C14 C13 N2 Ga1 -8.5(5) . . . . ? C1 C3 N2 C13 113.5(3) . . . . ? C1 C3 N2 Ga1 -63.6(3) . . . . ? C9 C8 O1 Ga1 179.5(2) . . . . ? C7 C8 O1 Ga1 -1.6(5) . . . . ? C14 C15 O2 Ga1 37.8(5) . . . . ? C16 C15 O2 Ga1 -144.9(3) . . . . ? C26 C27 S1 C24 0.4(4) . . . . ? C25 C24 S1 C27 -0.5(3) . . . . ? C23 C24 S1 C27 -179.8(3) . . . . ? C21 C20 S2 C23 0.5(3) . . . . ? C11 C20 S2 C23 -176.4(3) . . . . ? C22 C23 S2 C20 -0.4(3) . . . . ? C24 C23 S2 C20 179.2(3) . . . . ? C29 C28 S3 C31 -1.7(3) . . . . ? C18 C28 S3 C31 178.4(3) . . . . ? C30 C31 S3 C28 1.2(3) . . . . ? C32 C31 S3 C28 -175.0(3) . . . . ? C34 C35 S4A C32 -1.6(5) . . . . ? C33B C35 S4A C32 6(6) . . . . ? C33A C32 S4A C35 0.0(14) . . . . ? C31 C32 S4A C35 177.9(3) . . . . ? S4B C32 S4A C35 3.0(5) . . . . ? C33B C32 C33A C34 3(3) . . . . ? C31 C32 C33A C34 -176.6(8) . . . . ? C35 C34 C33A C32 -2(2) . . . . ? C35 C34 S4B C32 2.5(6) . . . . ? C33A C34 S4B C32 -15(8) . . . . ? C33B C32 S4B C34 -2.0(14) . . . . ? C31 C32 S4B C34 -178.1(4) . . . . ? S4A C32 S4B C34 -3.5(6) . . . . ? C33A C32 C33B C35 -2(2) . . . . ? C31 C32 C33B C35 177.2(7) . . . . ? S4B C32 C33B C35 0.9(19) . . . . ? C34 C35 C33B C32 1(2) . . . . ? C8 O1 Ga1 O2 171.3(3) . . . . ? C8 O1 Ga1 N2 94.6(3) . . . . ? C8 O1 Ga1 N1 0.8(3) . . . . ? C8 O1 Ga1 Cl1 -83.6(3) . . . . ? C15 O2 Ga1 O1 -169.3(3) . . . . ? C15 O2 Ga1 N2 -44.0(3) . . . . ? C15 O2 Ga1 Cl1 71.5(3) . . . . ? C13 N2 Ga1 O1 110.6(3) . . . . ? C3 N2 Ga1 O1 -72.5(3) . . . . ? C13 N2 Ga1 O2 30.2(3) . . . . ? C3 N2 Ga1 O2 -153.0(3) . . . . ? C13 N2 Ga1 N1 -156.7(3) . . . . ? C3 N2 Ga1 N1 20.1(2) . . . . ? C13 N2 Ga1 Cl1 -71.2(3) . . . . ? C3 N2 Ga1 Cl1 105.7(2) . . . . ? C6 N1 Ga1 O1 -1.4(3) . . . . ? C2 N1 Ga1 O1 179.4(3) . . . . ? C6 N1 Ga1 N2 -125.8(3) . . . . ? C2 N1 Ga1 N2 55.1(3) . . . . ? C6 N1 Ga1 Cl1 117.4(3) . . . . ? C2 N1 Ga1 Cl1 -61.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.857 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.857 _refine_diff_density_max 0.649 _refine_diff_density_min -0.818 _refine_diff_density_rms 0.072 # Attachment 'complex-4.cif.txt' data_grgr116 _database_code_depnum_ccdc_archive 'CCDC 770627' #TrackingRef 'complex-4.cif.txt' _audit_creation_method ; manual editing of the .cif file created by SHELXTL Ver. 6.10 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H52 Cl Ga N2 O2' _chemical_formula_sum 'C35 H52 Cl Ga N2 O2' _chemical_formula_weight 637.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 orthorhombic _symmetry_space_group_name_H-M pbca _symmetry_space_group_name_Hall -P2ac2ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 12.128(2) _cell_length_b 22.649(3) _cell_length_c 25.834(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7096(2) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 15270 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 24.7 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.194 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2720 _exptl_absorpt_coefficient_mu 0.881 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8366 _exptl_absorpt_correction_T_max 0.8575 _exptl_absorpt_process_details 'DENZO and Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71069 _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 \f-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15270 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0672 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 27.46 _reflns_number_total 8090 _reflns_number_gt 5283 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _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. One molecule of what appeared to be chloroform was found to be badly disordered. Attempts to model the disorder were unsatisfactory. The contributions to the scattering factors due to these solvent molecules were removed by use of the utility SQUEEZE (Sluis and Spek, 1990) in PLATON98 (Spek, 1998). PLATON98 was used as incorporated in WinGX (Farrugia, 1999). ; _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^)+(0.0521P)^2^+0.9738P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8090 _refine_ls_number_parameters 384 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0864 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1099 _refine_ls_wR_factor_gt 0.0936 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.73389(17) 0.14090(10) 0.48825(10) 0.0229(5) Uani 1 1 d . . . C2 C 0.79803(19) 0.14918(11) 0.43813(11) 0.0324(6) Uani 1 1 d . . . H2A H 0.8348 0.1121 0.4289 0.049 Uiso 1 1 calc R . . H2B H 0.8534 0.1802 0.4428 0.049 Uiso 1 1 calc R . . H2C H 0.7472 0.1605 0.4104 0.049 Uiso 1 1 calc R . . C3 C 0.8125(2) 0.13139(11) 0.53429(12) 0.0363(7) Uani 1 1 d . . . H3A H 0.7694 0.1230 0.5655 0.054 Uiso 1 1 calc R . . H3B H 0.8566 0.1671 0.5397 0.054 Uiso 1 1 calc R . . H3C H 0.8614 0.0980 0.5270 0.054 Uiso 1 1 calc R . . C4 C 0.66432(17) 0.19631(10) 0.49967(10) 0.0248(6) Uani 1 1 d . . . H4A H 0.6530 0.1999 0.5375 0.030 Uiso 1 1 calc R . . H4B H 0.7045 0.2318 0.4877 0.030 Uiso 1 1 calc R . . C5 C 0.66046(17) 0.08596(10) 0.48089(9) 0.0219(5) Uani 1 1 d . . . H5A H 0.6327 0.0858 0.4448 0.026 Uiso 1 1 calc R . . H5B H 0.7067 0.0503 0.4854 0.026 Uiso 1 1 calc R . . C6 C 0.53879(17) 0.22360(10) 0.43280(10) 0.0247(5) Uani 1 1 d . . . H6 H 0.5967 0.2484 0.4210 0.030 Uiso 1 1 calc R . . C7 C 0.43802(17) 0.22346(10) 0.40285(10) 0.0246(5) Uani 1 1 d . . . C8 C 0.43383(18) 0.26116(11) 0.35924(10) 0.0294(6) Uani 1 1 d . . . H8 H 0.4966 0.2844 0.3509 0.035 Uiso 1 1 calc R . . C9 C 0.34151(19) 0.26515(11) 0.32853(10) 0.0312(6) Uani 1 1 d . . . C10 C 0.25089(19) 0.22923(11) 0.34314(10) 0.0298(6) Uani 1 1 d . . . H10 H 0.1855 0.2322 0.3230 0.036 Uiso 1 1 calc R . . C11 C 0.25035(17) 0.19044(10) 0.38420(9) 0.0232(5) Uani 1 1 d . . . C12 C 0.34759(18) 0.18719(10) 0.41528(9) 0.0237(5) Uani 1 1 d . . . C13 C 0.3334(2) 0.30522(13) 0.28106(12) 0.0452(8) Uani 1 1 d . . . C14 C 0.4416(3) 0.33629(18) 0.26932(16) 0.0850(15) Uani 1 1 d . . . H14A H 0.4667 0.3575 0.3002 0.128 Uiso 1 1 calc R . . H14B H 0.4307 0.3644 0.2409 0.128 Uiso 1 1 calc R . . H14C H 0.4972 0.3070 0.2593 0.128 Uiso 1 1 calc R . . C15 C 0.2964(3) 0.27009(17) 0.23407(13) 0.0784(12) Uani 1 1 d . . . H15A H 0.3513 0.2396 0.2262 0.118 Uiso 1 1 calc R . . H15B H 0.2888 0.2966 0.2043 0.118 Uiso 1 1 calc R . . H15C H 0.2252 0.2514 0.2414 0.118 Uiso 1 1 calc R . . C16 C 0.2468(3) 0.35382(16) 0.29137(17) 0.0823(13) Uani 1 1 d . . . H16A H 0.1764 0.3355 0.3008 0.123 Uiso 1 1 calc R . . H16B H 0.2371 0.3777 0.2601 0.123 Uiso 1 1 calc R . . H16C H 0.2720 0.3791 0.3198 0.123 Uiso 1 1 calc R . . C17 C 0.15165(17) 0.14950(10) 0.39619(10) 0.0233(5) Uani 1 1 d . . . C18 C 0.10651(19) 0.15987(11) 0.45112(10) 0.0267(6) Uani 1 1 d . . . H18A H 0.0503 0.1301 0.4590 0.040 Uiso 1 1 calc R . . H18B H 0.0736 0.1993 0.4531 0.040 Uiso 1 1 calc R . . H18C H 0.1668 0.1568 0.4762 0.040 Uiso 1 1 calc R . . C19 C 0.18803(19) 0.08471(10) 0.39067(11) 0.0311(6) Uani 1 1 d . . . H19A H 0.2183 0.0783 0.3559 0.047 Uiso 1 1 calc R . . H19B H 0.1244 0.0588 0.3960 0.047 Uiso 1 1 calc R . . H19C H 0.2446 0.0758 0.4166 0.047 Uiso 1 1 calc R . . C20 C 0.05594(17) 0.16067(11) 0.35826(10) 0.0273(6) Uani 1 1 d . . . H20A H 0.0809 0.1531 0.3228 0.041 Uiso 1 1 calc R . . H20B H 0.0316 0.2018 0.3612 0.041 Uiso 1 1 calc R . . H20C H -0.0055 0.1342 0.3666 0.041 Uiso 1 1 calc R . . C21 C 0.56401(17) 0.03986(10) 0.55013(9) 0.0220(5) Uani 1 1 d . . . H21 H 0.6282 0.0160 0.5529 0.026 Uiso 1 1 calc R . . C22 C 0.47399(17) 0.02601(10) 0.58442(9) 0.0213(5) Uani 1 1 d . . . C23 C 0.49558(17) -0.01277(10) 0.62578(10) 0.0258(5) Uani 1 1 d . . . H23 H 0.5683 -0.0274 0.6305 0.031 Uiso 1 1 calc R . . C24 C 0.41409(18) -0.02989(11) 0.65935(10) 0.0263(5) Uani 1 1 d . . . C25 C 0.30692(18) -0.00806(10) 0.64923(9) 0.0255(5) Uani 1 1 d . . . H25 H 0.2496 -0.0197 0.6721 0.031 Uiso 1 1 calc R . . C26 C 0.27913(17) 0.02880(10) 0.60875(9) 0.0228(5) Uani 1 1 d . . . C27 C 0.36547(17) 0.04752(10) 0.57492(9) 0.0215(5) Uani 1 1 d . . . C28 C 0.43349(19) -0.06868(11) 0.70662(10) 0.0306(6) Uani 1 1 d . . . C29 C 0.5541(2) -0.08859(14) 0.71126(12) 0.0493(8) Uani 1 1 d . . . H29A H 0.5747 -0.1114 0.6805 0.074 Uiso 1 1 calc R . . H29B H 0.5628 -0.1133 0.7421 0.074 Uiso 1 1 calc R . . H29C H 0.6019 -0.0538 0.7141 0.074 Uiso 1 1 calc R . . C30 C 0.4038(2) -0.03280(13) 0.75494(11) 0.0416(7) Uani 1 1 d . . . H30A H 0.4472 0.0037 0.7555 0.062 Uiso 1 1 calc R . . H30B H 0.4199 -0.0561 0.7860 0.062 Uiso 1 1 calc R . . H30C H 0.3251 -0.0230 0.7542 0.062 Uiso 1 1 calc R . . C31 C 0.3615(2) -0.12435(12) 0.70376(12) 0.0445(7) Uani 1 1 d . . . H31A H 0.2838 -0.1129 0.7013 0.067 Uiso 1 1 calc R . . H31B H 0.3729 -0.1482 0.7350 0.067 Uiso 1 1 calc R . . H31C H 0.3821 -0.1475 0.6732 0.067 Uiso 1 1 calc R . . C32 C 0.15973(17) 0.05029(10) 0.60041(10) 0.0260(5) Uani 1 1 d . . . C33 C 0.1549(2) 0.11840(11) 0.60325(11) 0.0331(6) Uani 1 1 d . . . H33A H 0.0791 0.1317 0.5971 0.050 Uiso 1 1 calc R . . H33B H 0.2037 0.1353 0.5769 0.050 Uiso 1 1 calc R . . H33C H 0.1789 0.1315 0.6376 0.050 Uiso 1 1 calc R . . C34 C 0.11595(18) 0.02988(11) 0.54764(11) 0.0307(6) Uani 1 1 d . . . H34A H 0.1127 -0.0133 0.5469 0.046 Uiso 1 1 calc R . . H34B H 0.1653 0.0439 0.5202 0.046 Uiso 1 1 calc R . . H34C H 0.0419 0.0461 0.5421 0.046 Uiso 1 1 calc R . . C35 C 0.08169(19) 0.02660(12) 0.64217(11) 0.0371(7) Uani 1 1 d . . . H35A H 0.0825 -0.0167 0.6416 0.056 Uiso 1 1 calc R . . H35B H 0.0067 0.0407 0.6354 0.056 Uiso 1 1 calc R . . H35C H 0.1059 0.0406 0.6762 0.056 Uiso 1 1 calc R . . N1 N 0.55698(14) 0.19332(8) 0.47369(8) 0.0228(4) Uani 1 1 d . . . N2 N 0.56598(13) 0.08162(8) 0.51594(8) 0.0205(4) Uani 1 1 d . . . O1 O 0.34930(12) 0.14952(7) 0.45458(7) 0.0300(4) Uani 1 1 d . . . O2 O 0.34348(11) 0.08096(7) 0.53440(6) 0.0227(4) Uani 1 1 d . . . Cl1 Cl 0.42959(5) 0.19807(3) 0.57891(3) 0.03599(17) Uani 1 1 d . . . Ga1 Ga 0.443081(18) 0.140136(11) 0.510198(11) 0.02043(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0160(11) 0.0219(13) 0.0308(14) -0.0012(11) 0.0006(10) -0.0018(9) C2 0.0243(12) 0.0283(14) 0.0447(17) -0.0011(13) 0.0075(11) -0.0053(10) C3 0.0257(13) 0.0351(16) 0.0482(18) -0.0007(13) -0.0110(12) -0.0003(11) C4 0.0176(11) 0.0215(13) 0.0353(16) -0.0016(11) -0.0024(9) -0.0026(9) C5 0.0175(11) 0.0224(13) 0.0258(14) -0.0015(11) 0.0050(9) -0.0003(9) C6 0.0208(12) 0.0207(13) 0.0327(15) 0.0009(11) 0.0021(10) 0.0003(9) C7 0.0216(11) 0.0251(13) 0.0272(14) 0.0014(11) 0.0001(10) 0.0008(9) C8 0.0270(12) 0.0258(14) 0.0354(16) 0.0040(12) -0.0005(11) -0.0046(10) C9 0.0328(13) 0.0297(14) 0.0311(15) 0.0076(12) -0.0046(11) -0.0032(10) C10 0.0261(12) 0.0308(14) 0.0324(16) 0.0027(12) -0.0069(11) -0.0011(10) C11 0.0218(11) 0.0224(13) 0.0255(13) -0.0002(11) -0.0016(10) 0.0017(9) C12 0.0235(11) 0.0220(13) 0.0257(14) 0.0024(11) 0.0005(10) 0.0012(9) C13 0.0476(16) 0.0464(18) 0.0415(18) 0.0206(15) -0.0152(14) -0.0161(14) C14 0.078(3) 0.103(3) 0.074(3) 0.065(3) -0.027(2) -0.044(2) C15 0.117(3) 0.078(3) 0.040(2) 0.020(2) -0.020(2) -0.036(2) C16 0.096(3) 0.061(2) 0.090(3) 0.039(2) -0.019(3) 0.009(2) C17 0.0183(11) 0.0253(13) 0.0262(14) -0.0013(11) -0.0016(10) -0.0009(9) C18 0.0219(11) 0.0300(14) 0.0283(15) -0.0003(12) 0.0003(10) -0.0019(10) C19 0.0256(12) 0.0261(14) 0.0416(17) -0.0032(12) -0.0036(11) 0.0007(10) C20 0.0207(11) 0.0335(14) 0.0278(14) -0.0017(12) -0.0032(10) 0.0002(10) C21 0.0172(11) 0.0215(13) 0.0274(14) -0.0041(11) -0.0026(9) 0.0017(9) C22 0.0195(10) 0.0224(13) 0.0220(13) -0.0008(10) 0.0000(9) 0.0011(9) C23 0.0195(12) 0.0274(13) 0.0305(15) 0.0026(12) -0.0035(10) 0.0010(10) C24 0.0272(12) 0.0270(13) 0.0246(14) 0.0022(11) -0.0027(10) -0.0022(10) C25 0.0257(12) 0.0274(14) 0.0234(14) -0.0003(11) 0.0031(10) -0.0036(10) C26 0.0220(11) 0.0217(13) 0.0247(14) -0.0008(11) 0.0015(9) -0.0009(9) C27 0.0237(11) 0.0176(12) 0.0233(14) -0.0025(11) 0.0001(9) -0.0019(9) C28 0.0306(13) 0.0357(15) 0.0254(14) 0.0059(12) -0.0034(10) -0.0014(11) C29 0.0399(16) 0.061(2) 0.0468(19) 0.0268(17) -0.0046(13) 0.0067(14) C30 0.0532(17) 0.0460(17) 0.0256(16) 0.0065(14) -0.0067(13) -0.0055(13) C31 0.0568(18) 0.0387(16) 0.0380(18) 0.0139(14) -0.0097(14) -0.0115(13) C32 0.0194(11) 0.0244(13) 0.0342(15) 0.0008(11) 0.0040(10) 0.0011(9) C33 0.0277(13) 0.0283(14) 0.0433(17) -0.0023(13) 0.0068(12) 0.0025(10) C34 0.0201(12) 0.0298(14) 0.0421(17) -0.0018(13) -0.0019(11) 0.0011(10) C35 0.0248(13) 0.0423(17) 0.0443(18) 0.0048(14) 0.0096(12) -0.0001(11) N1 0.0180(9) 0.0201(11) 0.0303(12) 0.0013(9) -0.0022(8) 0.0003(7) N2 0.0178(9) 0.0193(10) 0.0244(11) -0.0003(9) 0.0010(8) -0.0023(7) O1 0.0218(8) 0.0328(10) 0.0353(11) 0.0124(9) -0.0061(7) -0.0068(7) O2 0.0186(7) 0.0234(9) 0.0262(9) 0.0035(8) 0.0000(7) -0.0010(6) Cl1 0.0379(4) 0.0285(3) 0.0415(4) -0.0114(3) 0.0111(3) -0.0057(3) Ga1 0.01622(14) 0.01951(15) 0.02557(16) 0.00182(11) -0.00004(10) 0.00024(9) _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 C1 C2 1.522(3) . ? C1 C3 1.539(3) . ? C1 C4 1.541(3) . ? C1 C5 1.542(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 N1 1.466(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 N2 1.464(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N1 1.279(3) . ? C6 C7 1.446(3) . ? C6 H6 0.9500 . ? C7 C12 1.407(3) . ? C7 C8 1.415(3) . ? C8 C9 1.375(3) . ? C8 H8 0.9500 . ? C9 C10 1.419(3) . ? C9 C13 1.529(4) . ? C10 C11 1.377(3) . ? C10 H10 0.9500 . ? C11 C12 1.429(3) . ? C11 C17 1.545(3) . ? C12 O1 1.326(3) . ? C13 C15 1.519(4) . ? C13 C14 1.520(4) . ? C13 C16 1.544(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.539(3) . ? C17 C19 1.539(3) . ? C17 C20 1.540(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 N2 1.294(3) . ? C21 C22 1.441(3) . ? C21 H21 0.9500 . ? C22 C23 1.408(3) . ? C22 C27 1.425(3) . ? C23 C24 1.371(3) . ? C23 H23 0.9500 . ? C24 C25 1.415(3) . ? C24 C28 1.523(3) . ? C25 C26 1.380(3) . ? C25 H25 0.9500 . ? C26 C27 1.428(3) . ? C26 C32 1.543(3) . ? C27 O2 1.319(3) . ? C28 C30 1.533(4) . ? C28 C31 1.535(4) . ? C28 C29 1.536(3) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C35 1.532(3) . ? C32 C34 1.534(3) . ? C32 C33 1.546(3) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? N1 Ga1 2.0613(19) . ? N2 Ga1 2.0001(18) . ? O1 Ga1 1.8448(16) . ? O2 Ga1 1.9096(15) . ? Cl1 Ga1 2.2135(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C3 111.0(2) . . ? C2 C1 C4 110.0(2) . . ? C3 C1 C4 107.8(2) . . ? C2 C1 C5 106.84(19) . . ? C3 C1 C5 109.9(2) . . ? C4 C1 C5 111.38(17) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 C1 111.16(18) . . ? N1 C4 H4A 109.4 . . ? C1 C4 H4A 109.4 . . ? N1 C4 H4B 109.4 . . ? C1 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? N2 C5 C1 115.48(18) . . ? N2 C5 H5A 108.4 . . ? C1 C5 H5A 108.4 . . ? N2 C5 H5B 108.4 . . ? C1 C5 H5B 108.4 . . ? H5A C5 H5B 107.5 . . ? N1 C6 C7 125.9(2) . . ? N1 C6 H6 117.0 . . ? C7 C6 H6 117.0 . . ? C12 C7 C8 120.4(2) . . ? C12 C7 C6 122.5(2) . . ? C8 C7 C6 117.1(2) . . ? C9 C8 C7 121.9(2) . . ? C9 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? C8 C9 C10 116.1(2) . . ? C8 C9 C13 123.7(2) . . ? C10 C9 C13 120.3(2) . . ? C11 C10 C9 125.1(2) . . ? C11 C10 H10 117.5 . . ? C9 C10 H10 117.5 . . ? C10 C11 C12 117.5(2) . . ? C10 C11 C17 122.7(2) . . ? C12 C11 C17 119.7(2) . . ? O1 C12 C7 122.5(2) . . ? O1 C12 C11 118.44(19) . . ? C7 C12 C11 119.0(2) . . ? C15 C13 C14 109.8(3) . . ? C15 C13 C9 110.4(2) . . ? C14 C13 C9 112.3(2) . . ? C15 C13 C16 108.1(3) . . ? C14 C13 C16 106.9(3) . . ? C9 C13 C16 109.2(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C19 109.4(2) . . ? C18 C17 C20 107.07(18) . . ? C19 C17 C20 108.28(19) . . ? C18 C17 C11 111.64(19) . . ? C19 C17 C11 109.36(18) . . ? C20 C17 C11 110.96(19) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N2 C21 C22 126.4(2) . . ? N2 C21 H21 116.8 . . ? C22 C21 H21 116.8 . . ? C23 C22 C27 121.1(2) . . ? C23 C22 C21 117.5(2) . . ? C27 C22 C21 121.3(2) . . ? C24 C23 C22 121.5(2) . . ? C24 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? C23 C24 C25 116.5(2) . . ? C23 C24 C28 124.0(2) . . ? C25 C24 C28 119.5(2) . . ? C26 C25 C24 125.2(2) . . ? C26 C25 H25 117.4 . . ? C24 C25 H25 117.4 . . ? C25 C26 C27 117.7(2) . . ? C25 C26 C32 121.7(2) . . ? C27 C26 C32 120.6(2) . . ? O2 C27 C22 121.3(2) . . ? O2 C27 C26 120.52(19) . . ? C22 C27 C26 118.1(2) . . ? C24 C28 C30 108.1(2) . . ? C24 C28 C31 110.3(2) . . ? C30 C28 C31 109.9(2) . . ? C24 C28 C29 112.3(2) . . ? C30 C28 C29 108.4(2) . . ? C31 C28 C29 107.7(2) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C35 C32 C34 107.8(2) . . ? C35 C32 C26 111.8(2) . . ? C34 C32 C26 110.72(19) . . ? C35 C32 C33 107.0(2) . . ? C34 C32 C33 109.3(2) . . ? C26 C32 C33 110.10(18) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C6 N1 C4 120.44(19) . . ? C6 N1 Ga1 125.16(15) . . ? C4 N1 Ga1 114.36(15) . . ? C21 N2 C5 119.06(18) . . ? C21 N2 Ga1 121.41(15) . . ? C5 N2 Ga1 119.53(14) . . ? C12 O1 Ga1 132.83(14) . . ? C27 O2 Ga1 122.34(13) . . ? O1 Ga1 O2 86.90(7) . . ? O1 Ga1 N2 126.41(8) . . ? O2 Ga1 N2 88.97(7) . . ? O1 Ga1 N1 89.40(7) . . ? O2 Ga1 N1 169.71(7) . . ? N2 Ga1 N1 85.51(7) . . ? O1 Ga1 Cl1 120.71(6) . . ? O2 Ga1 Cl1 96.12(5) . . ? N2 Ga1 Cl1 112.86(6) . . ? N1 Ga1 Cl1 94.02(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 C1 C4 N1 86.5(2) . . . . ? C3 C1 C4 N1 -152.4(2) . . . . ? C5 C1 C4 N1 -31.8(3) . . . . ? C2 C1 C5 N2 -159.61(19) . . . . ? C3 C1 C5 N2 79.9(2) . . . . ? C4 C1 C5 N2 -39.4(3) . . . . ? N1 C6 C7 C12 -2.1(4) . . . . ? N1 C6 C7 C8 178.8(2) . . . . ? C12 C7 C8 C9 1.9(4) . . . . ? C6 C7 C8 C9 -179.0(2) . . . . ? C7 C8 C9 C10 0.0(4) . . . . ? C7 C8 C9 C13 -179.9(3) . . . . ? C8 C9 C10 C11 -1.8(4) . . . . ? C13 C9 C10 C11 178.1(3) . . . . ? C9 C10 C11 C12 1.7(4) . . . . ? C9 C10 C11 C17 -176.0(2) . . . . ? C8 C7 C12 O1 177.4(2) . . . . ? C6 C7 C12 O1 -1.7(4) . . . . ? C8 C7 C12 C11 -2.0(3) . . . . ? C6 C7 C12 C11 179.0(2) . . . . ? C10 C11 C12 O1 -179.1(2) . . . . ? C17 C11 C12 O1 -1.3(3) . . . . ? C10 C11 C12 C7 0.3(3) . . . . ? C17 C11 C12 C7 178.0(2) . . . . ? C8 C9 C13 C15 127.4(3) . . . . ? C10 C9 C13 C15 -52.5(4) . . . . ? C8 C9 C13 C14 4.5(4) . . . . ? C10 C9 C13 C14 -175.4(3) . . . . ? C8 C9 C13 C16 -113.9(3) . . . . ? C10 C9 C13 C16 66.2(3) . . . . ? C10 C11 C17 C18 -122.1(2) . . . . ? C12 C11 C17 C18 60.3(3) . . . . ? C10 C11 C17 C19 116.7(3) . . . . ? C12 C11 C17 C19 -60.9(3) . . . . ? C10 C11 C17 C20 -2.7(3) . . . . ? C12 C11 C17 C20 179.7(2) . . . . ? N2 C21 C22 C23 -167.3(2) . . . . ? N2 C21 C22 C27 16.9(4) . . . . ? C27 C22 C23 C24 -2.0(4) . . . . ? C21 C22 C23 C24 -177.9(2) . . . . ? C22 C23 C24 C25 1.9(4) . . . . ? C22 C23 C24 C28 -176.2(2) . . . . ? C23 C24 C25 C26 -0.2(4) . . . . ? C28 C24 C25 C26 178.0(2) . . . . ? C24 C25 C26 C27 -1.4(4) . . . . ? C24 C25 C26 C32 179.7(2) . . . . ? C23 C22 C27 O2 -175.8(2) . . . . ? C21 C22 C27 O2 -0.1(3) . . . . ? C23 C22 C27 C26 0.3(3) . . . . ? C21 C22 C27 C26 176.0(2) . . . . ? C25 C26 C27 O2 177.4(2) . . . . ? C32 C26 C27 O2 -3.6(3) . . . . ? C25 C26 C27 C22 1.3(3) . . . . ? C32 C26 C27 C22 -179.7(2) . . . . ? C23 C24 C28 C30 117.3(3) . . . . ? C25 C24 C28 C30 -60.8(3) . . . . ? C23 C24 C28 C31 -122.5(3) . . . . ? C25 C24 C28 C31 59.5(3) . . . . ? C23 C24 C28 C29 -2.3(4) . . . . ? C25 C24 C28 C29 179.6(2) . . . . ? C25 C26 C32 C35 0.9(3) . . . . ? C27 C26 C32 C35 -178.0(2) . . . . ? C25 C26 C32 C34 -119.3(2) . . . . ? C27 C26 C32 C34 61.8(3) . . . . ? C25 C26 C32 C33 119.8(2) . . . . ? C27 C26 C32 C33 -59.1(3) . . . . ? C7 C6 N1 C4 178.3(2) . . . . ? C7 C6 N1 Ga1 -4.1(3) . . . . ? C1 C4 N1 C6 -103.7(2) . . . . ? C1 C4 N1 Ga1 78.4(2) . . . . ? C22 C21 N2 C5 -174.2(2) . . . . ? C22 C21 N2 Ga1 5.9(3) . . . . ? C1 C5 N2 C21 -112.9(2) . . . . ? C1 C5 N2 Ga1 67.0(2) . . . . ? C7 C12 O1 Ga1 13.4(4) . . . . ? C11 C12 O1 Ga1 -167.22(17) . . . . ? C22 C27 O2 Ga1 -38.4(3) . . . . ? C26 C27 O2 Ga1 145.64(17) . . . . ? C12 O1 Ga1 O2 174.7(2) . . . . ? C12 O1 Ga1 N2 -98.9(2) . . . . ? C12 O1 Ga1 N1 -14.9(2) . . . . ? C12 O1 Ga1 Cl1 79.4(2) . . . . ? C27 O2 Ga1 O1 173.16(17) . . . . ? C27 O2 Ga1 N2 46.61(17) . . . . ? C27 O2 Ga1 N1 104.1(4) . . . . ? C27 O2 Ga1 Cl1 -66.27(16) . . . . ? C21 N2 Ga1 O1 -115.43(18) . . . . ? C5 N2 Ga1 O1 64.68(18) . . . . ? C21 N2 Ga1 O2 -30.05(18) . . . . ? C5 N2 Ga1 O2 150.06(16) . . . . ? C21 N2 Ga1 N1 158.64(19) . . . . ? C5 N2 Ga1 N1 -21.25(16) . . . . ? C21 N2 Ga1 Cl1 66.16(18) . . . . ? C5 N2 Ga1 Cl1 -113.73(15) . . . . ? C6 N1 Ga1 O1 9.8(2) . . . . ? C4 N1 Ga1 O1 -172.44(16) . . . . ? C6 N1 Ga1 O2 78.7(4) . . . . ? C4 N1 Ga1 O2 -103.6(4) . . . . ? C6 N1 Ga1 N2 136.4(2) . . . . ? C4 N1 Ga1 N2 -45.84(15) . . . . ? C6 N1 Ga1 Cl1 -110.93(19) . . . . ? C4 N1 Ga1 Cl1 66.81(15) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.595 _refine_diff_density_min -0.687 _refine_diff_density_rms 0.071