Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Prof. Alessandra Crispini' _publ_contact_author_address ; Dipartimento di Chimica Universit\'a della Calabria 87030 Arcavacata di Rende (CS) Italy ; _publ_contact_author_email A.CRISPINI@UNICAL.IT _publ_contact_author_fax 0984492066 _publ_contact_author_phone 0984492062 _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for publication as a Full Paper in Crystal Growth & Design ; _publ_requested_category FP _publ_section_title ; Synthesis and Solid State Characterization of Hexacoordinated 1:1 Ionic Gallium(III) Complexes ; _publ_section_title_footnote ; ? ; loop_ _publ_author_name _publ_author_address M.Ghedini ; Dipartimento di Chimica Universit\'a della Calabria 87030 Arcavacata di Rende (CS) Italy ; A.Crispini ; Dipartimento di Chimica Universit\'a della Calabria 87030 Arcavacata di Rende (CS) Italy ; 'I.De Franco' ; Dipartimento di Chimica Universit\'a della Calabria 87030 Arcavacata di Rende (CS) Italy ; I.Aiello ; Dipartimento di Chimica Universit\'a della Calabria 87030 Arcavacata di Rende (CS) Italy ; 'M.La Deda' ; Dipartimento di Chimica Universit\'a della Calabria 87030 Arcavacata di Rende (CS) Italy ; N.Godbert ; Dipartimento di Chimica Universit\'a della Calabria 87030 Arcavacata di Rende (CS) Italy ; ; A.Bellusci ; ; Dipartimento di Chimica Universit\'a della Calabria 87030 Arcavacata di Rende (CS) Italy ; data_(1a) _database_code_depnum_ccdc_archive 'CCDC 665245' _audit_creation_method SHELXL-97 _chemical_formula_moiety '(C30 H24 Ga N4 O2), (N O3), 0.5(C H2 Cl2)' _chemical_formula_sum 'C30.50 H25 Cl Ga N5 O5' _chemical_formula_weight 646.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M ' P 21/n ' _symmetry_space_group_name_Hall '-P 2yn' 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 11.5436(18) _cell_length_b 19.380(3) _cell_length_c 13.724(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.353(3) _cell_angle_gamma 90.00 _cell_volume 3037.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4418 _cell_measurement_theta_min 1.83 _cell_measurement_theta_max 24.49 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1324 _exptl_absorpt_coefficient_mu 1.041 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22887 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0425 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 24.49 _reflns_number_total 5034 _reflns_number_gt 3604 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1463P)^2^+1.7367P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _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 5034 _refine_ls_number_parameters 380 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0931 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.2327 _refine_ls_wR_factor_gt 0.2117 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.097 _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 Ga Ga 0.32254(5) 0.65603(3) 0.39562(4) 0.0440(3) Uani 1 1 d . . . O1 O 0.2369(3) 0.57732(19) 0.4291(3) 0.0533(10) Uani 1 1 d . . . O2 O 0.4140(3) 0.73263(19) 0.3676(3) 0.0548(10) Uani 1 1 d . . . N1 N 0.1999(4) 0.6523(2) 0.2641(3) 0.0467(11) Uani 1 1 d . . . N2 N 0.2242(4) 0.7361(2) 0.4567(3) 0.0535(12) Uani 1 1 d . . . N3 N 0.4391(4) 0.6360(2) 0.5246(3) 0.0514(11) Uani 1 1 d . . . N4 N 0.4478(4) 0.5936(2) 0.3418(3) 0.0505(11) Uani 1 1 d . . . N5 N -0.1908(7) 0.9084(4) 0.4428(7) 0.105(2) Uani 1 1 d . . . C1 C 0.1409(5) 0.5631(3) 0.3662(4) 0.0519(14) Uani 1 1 d . . . C2 C 0.0633(5) 0.5106(3) 0.3793(5) 0.0650(16) Uani 1 1 d . . . H2 H 0.0788 0.4824 0.4344 0.078 Uiso 1 1 calc R . . C3 C -0.0369(6) 0.4991(4) 0.3124(6) 0.080(2) Uani 1 1 d . . . H3 H -0.0889 0.4647 0.3250 0.095 Uiso 1 1 calc R . . C4 C -0.0603(6) 0.5370(4) 0.2294(6) 0.080(2) Uani 1 1 d . . . H4A H -0.1273 0.5280 0.1849 0.096 Uiso 1 1 calc R . . C5 C 0.0157(5) 0.5900(4) 0.2098(5) 0.0648(17) Uani 1 1 d . . . C6 C 0.1174(4) 0.6032(3) 0.2781(4) 0.0491(13) Uani 1 1 d . . . C7 C 0.1864(5) 0.6887(3) 0.1811(4) 0.0526(14) Uani 1 1 d . . . C8 C 0.0852(6) 0.6791(4) 0.1099(5) 0.0733(19) Uani 1 1 d . . . H8A H 0.0757 0.7055 0.0528 0.088 Uiso 1 1 calc R . . C9 C 0.0030(6) 0.6325(4) 0.1238(5) 0.078(2) Uani 1 1 d . . . H9 H -0.0631 0.6278 0.0767 0.093 Uiso 1 1 calc R . . C10 C 0.2778(6) 0.7383(3) 0.1606(4) 0.0693(18) Uani 1 1 d . . . H10A H 0.3395 0.7396 0.2156 0.104 Uiso 1 1 calc R . . H10B H 0.2440 0.7834 0.1502 0.104 Uiso 1 1 calc R . . H10C H 0.3091 0.7240 0.1027 0.104 Uiso 1 1 calc R . . C11 C 0.3717(5) 0.7939(3) 0.3843(4) 0.0523(14) Uani 1 1 d . . . C12 C 0.4221(7) 0.8560(3) 0.3582(5) 0.0677(18) Uani 1 1 d . . . H12 H 0.4884 0.8555 0.3270 0.081 Uiso 1 1 calc R . . C13 C 0.3706(8) 0.9188(3) 0.3803(5) 0.081(2) Uani 1 1 d . . . H13 H 0.4064 0.9594 0.3643 0.098 Uiso 1 1 calc R . . C14 C 0.2741(7) 0.9241(3) 0.4223(5) 0.073(2) Uani 1 1 d . . . H14 H 0.2433 0.9672 0.4339 0.088 Uiso 1 1 calc R . . C15 C 0.2190(6) 0.8628(4) 0.4490(5) 0.0641(17) Uani 1 1 d . . . C16 C 0.2685(5) 0.7979(3) 0.4310(4) 0.0514(14) Uani 1 1 d . . . C17 C 0.1308(5) 0.7360(4) 0.5025(5) 0.0676(17) Uani 1 1 d . . . C18 C 0.0761(7) 0.7997(5) 0.5208(6) 0.093(2) Uani 1 1 d . . . H18 H 0.0097 0.7994 0.5518 0.112 Uiso 1 1 calc R . . C19 C 0.1197(7) 0.8612(4) 0.4935(6) 0.085(2) Uani 1 1 d . . . H19 H 0.0820 0.9022 0.5051 0.103 Uiso 1 1 calc R . . C20 C 0.0847(8) 0.6703(4) 0.5377(7) 0.103(3) Uani 1 1 d . . . H20A H 0.1306 0.6324 0.5193 0.155 Uiso 1 1 calc R . . H20B H 0.0047 0.6644 0.5084 0.155 Uiso 1 1 calc R . . H20C H 0.0893 0.6716 0.6081 0.155 Uiso 1 1 calc R . . C21 C 0.4292(6) 0.6594(3) 0.6141(5) 0.0644(17) Uani 1 1 d . . . H21 H 0.3649 0.6864 0.6226 0.077 Uiso 1 1 calc R . . C22 C 0.5118(8) 0.6447(4) 0.6947(5) 0.079(2) Uani 1 1 d . . . H22 H 0.5030 0.6613 0.7568 0.095 Uiso 1 1 calc R . . C23 C 0.6058(7) 0.6057(4) 0.6818(6) 0.079(2) Uani 1 1 d . . . H23 H 0.6625 0.5957 0.7353 0.095 Uiso 1 1 calc R . . C24 C 0.6174(6) 0.5811(3) 0.5911(5) 0.0665(17) Uani 1 1 d . . . H24 H 0.6816 0.5542 0.5821 0.080 Uiso 1 1 calc R . . C25 C 0.5320(5) 0.5968(3) 0.5118(4) 0.0523(14) Uani 1 1 d . . . C26 C 0.5363(4) 0.5729(3) 0.4107(4) 0.0516(14) Uani 1 1 d . . . C27 C 0.6234(5) 0.5304(3) 0.3845(5) 0.0674(17) Uani 1 1 d . . . H27 H 0.6842 0.5158 0.4321 0.081 Uiso 1 1 calc R . . C28 C 0.6200(6) 0.5100(4) 0.2878(6) 0.0743(19) Uani 1 1 d . . . H28 H 0.6776 0.4811 0.2696 0.089 Uiso 1 1 calc R . . C29 C 0.5304(6) 0.5328(3) 0.2191(5) 0.0705(18) Uani 1 1 d . . . H29 H 0.5273 0.5204 0.1533 0.085 Uiso 1 1 calc R . . C30 C 0.4454(5) 0.5741(3) 0.2480(4) 0.0587(15) Uani 1 1 d . . . H30 H 0.3842 0.5890 0.2011 0.070 Uiso 1 1 calc R . . O3 O -0.1262(11) 0.9586(7) 0.4674(9) 0.137(5) Uiso 0.690(16) 1 d P A 1 O4 O -0.2315(11) 0.9039(7) 0.3543(11) 0.159(6) Uiso 0.690(16) 1 d P A 1 O5 O -0.2041(12) 0.8708(9) 0.5044(12) 0.154(5) Uiso 0.690(16) 1 d P A 1 O3A O -0.1527(16) 0.9152(11) 0.5347(15) 0.095(8) Uiso 0.310(16) 1 d P A 2 O4A O -0.205(3) 0.9555(18) 0.402(2) 0.146(11) Uiso 0.310(16) 1 d P A 2 O5A O -0.222(2) 0.8413(13) 0.450(2) 0.125(10) Uiso 0.310(16) 1 d P A 2 C31 C -0.290(2) 0.7128(11) 0.2660(17) 0.138(8) Uiso 0.50 1 d P . . H31A H -0.2704 0.6848 0.2122 0.166 Uiso 0.50 1 calc PR . . H31B H -0.3719 0.7048 0.2718 0.166 Uiso 0.50 1 calc PR . . Cl1 Cl -0.2726(12) 0.7839(7) 0.2459(10) 0.294(6) Uiso 0.50 1 d PD . . Cl2 Cl -0.1923(14) 0.6869(10) 0.3878(11) 0.346(8) Uiso 0.50 1 d PD . . 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 Ga 0.0426(4) 0.0442(4) 0.0436(4) 0.0035(2) 0.0007(3) 0.0035(2) O1 0.047(2) 0.052(2) 0.057(2) 0.0120(18) -0.0057(18) -0.0026(18) O2 0.046(2) 0.049(2) 0.070(3) 0.0007(19) 0.0090(19) 0.0032(18) N1 0.046(3) 0.051(3) 0.042(3) 0.001(2) 0.001(2) 0.010(2) N2 0.053(3) 0.057(3) 0.050(3) -0.004(2) 0.005(2) 0.002(2) N3 0.055(3) 0.053(3) 0.044(3) 0.004(2) 0.000(2) -0.001(2) N4 0.051(3) 0.045(3) 0.055(3) 0.003(2) 0.005(2) 0.002(2) N5 0.125(6) 0.070(5) 0.114(7) 0.017(5) -0.004(5) -0.002(4) C1 0.045(3) 0.051(3) 0.059(3) 0.000(3) 0.001(3) 0.001(3) C2 0.056(4) 0.068(4) 0.072(4) 0.009(3) 0.014(3) -0.006(3) C3 0.054(4) 0.085(5) 0.098(6) 0.002(4) 0.010(4) -0.021(4) C4 0.053(4) 0.097(5) 0.086(5) -0.007(4) -0.006(3) -0.015(4) C5 0.046(3) 0.084(5) 0.063(4) -0.005(3) 0.000(3) 0.002(3) C6 0.040(3) 0.053(3) 0.052(3) -0.002(3) 0.000(2) 0.008(3) C7 0.060(3) 0.055(3) 0.042(3) 0.007(3) 0.005(3) 0.014(3) C8 0.072(5) 0.083(5) 0.060(4) 0.009(4) -0.008(3) 0.012(4) C9 0.065(4) 0.104(6) 0.055(4) 0.000(4) -0.021(3) 0.005(4) C10 0.091(5) 0.067(4) 0.049(4) 0.014(3) 0.007(3) 0.002(4) C11 0.053(3) 0.051(3) 0.049(3) 0.003(3) -0.007(3) -0.003(3) C12 0.079(5) 0.058(4) 0.063(4) 0.006(3) -0.002(3) -0.011(3) C13 0.125(7) 0.045(4) 0.069(5) 0.004(3) -0.007(5) -0.015(4) C14 0.106(6) 0.046(4) 0.060(4) -0.002(3) -0.011(4) 0.011(4) C15 0.070(4) 0.067(4) 0.048(3) -0.007(3) -0.012(3) 0.020(3) C16 0.058(3) 0.049(3) 0.044(3) -0.004(2) -0.006(3) 0.006(3) C17 0.057(4) 0.077(5) 0.072(4) -0.015(4) 0.021(3) 0.003(3) C18 0.070(5) 0.115(7) 0.100(6) -0.026(5) 0.031(4) 0.014(5) C19 0.089(6) 0.076(5) 0.088(5) -0.022(4) 0.002(4) 0.029(4) C20 0.099(6) 0.109(6) 0.114(7) -0.014(5) 0.059(6) -0.017(5) C21 0.068(4) 0.071(4) 0.052(4) 0.004(3) 0.000(3) 0.002(3) C22 0.105(6) 0.080(5) 0.047(4) 0.000(3) -0.011(4) -0.017(4) C23 0.080(5) 0.068(4) 0.078(5) 0.011(4) -0.031(4) -0.005(4) C24 0.060(4) 0.067(4) 0.066(4) 0.015(3) -0.013(3) 0.000(3) C25 0.043(3) 0.048(3) 0.062(4) 0.010(3) -0.006(3) -0.006(3) C26 0.039(3) 0.045(3) 0.068(4) 0.011(3) -0.001(3) 0.004(2) C27 0.042(3) 0.068(4) 0.090(5) 0.001(4) 0.004(3) 0.009(3) C28 0.054(4) 0.071(4) 0.101(6) 0.003(4) 0.023(4) 0.010(3) C29 0.079(4) 0.059(4) 0.079(5) -0.002(3) 0.030(4) 0.001(3) C30 0.063(4) 0.056(3) 0.059(4) -0.002(3) 0.014(3) 0.007(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 Ga O2 1.893(4) . ? Ga O1 1.910(4) . ? Ga N3 2.099(4) . ? Ga N4 2.101(5) . ? Ga N1 2.128(4) . ? Ga N2 2.162(5) . ? O1 C1 1.332(6) . ? O2 C11 1.317(6) . ? N1 C7 1.330(7) . ? N1 C6 1.379(7) . ? N2 C17 1.324(7) . ? N2 C16 1.369(7) . ? N3 C21 1.329(8) . ? N3 C25 1.346(7) . ? N4 C30 1.338(7) . ? N4 C26 1.348(7) . ? N5 O4A 1.07(3) . ? N5 O5 1.144(15) . ? N5 O4 1.240(15) . ? N5 O3 1.242(14) . ? N5 O3A 1.28(2) . ? N5 O5A 1.36(3) . ? C1 C2 1.384(8) . ? C1 C6 1.430(8) . ? C2 C3 1.387(9) . ? C3 C4 1.349(10) . ? C4 C5 1.402(9) . ? C5 C6 1.415(8) . ? C5 C9 1.429(10) . ? C7 C8 1.422(8) . ? C7 C10 1.484(8) . ? C8 C9 1.343(10) . ? C11 C12 1.405(8) . ? C11 C16 1.433(8) . ? C12 C13 1.407(10) . ? C13 C14 1.330(11) . ? C14 C15 1.421(10) . ? C15 C19 1.374(10) . ? C15 C16 1.420(8) . ? C17 C18 1.424(9) . ? C17 C20 1.488(10) . ? C18 C19 1.367(11) . ? C21 C22 1.381(9) . ? C22 C23 1.356(10) . ? C23 C24 1.356(10) . ? C24 C25 1.392(8) . ? C25 C26 1.471(8) . ? C26 C27 1.386(8) . ? C27 C28 1.381(9) . ? C28 C29 1.367(9) . ? C29 C30 1.369(8) . ? C31 Cl1 1.426(19) . ? C31 Cl2 1.94(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 O2 Ga O1 176.96(15) . . ? O2 Ga N3 90.49(17) . . ? O1 Ga N3 86.54(16) . . ? O2 Ga N4 87.01(17) . . ? O1 Ga N4 91.78(17) . . ? N3 Ga N4 78.46(18) . . ? O2 Ga N1 100.17(17) . . ? O1 Ga N1 82.71(16) . . ? N3 Ga N1 167.32(18) . . ? N4 Ga N1 95.13(17) . . ? O2 Ga N2 81.72(18) . . ? O1 Ga N2 99.23(18) . . ? N3 Ga N2 96.56(18) . . ? N4 Ga N2 167.67(18) . . ? N1 Ga N2 91.79(17) . . ? C1 O1 Ga 114.9(3) . . ? C11 O2 Ga 116.1(3) . . ? C7 N1 C6 119.2(5) . . ? C7 N1 Ga 133.6(4) . . ? C6 N1 Ga 107.1(3) . . ? C17 N2 C16 118.9(5) . . ? C17 N2 Ga 133.9(4) . . ? C16 N2 Ga 106.9(3) . . ? C21 N3 C25 119.4(5) . . ? C21 N3 Ga 125.8(4) . . ? C25 N3 Ga 114.8(4) . . ? C30 N4 C26 119.9(5) . . ? C30 N4 Ga 125.6(4) . . ? C26 N4 Ga 114.5(4) . . ? O4A N5 O5 155(2) . . ? O4A N5 O4 62.4(17) . . ? O5 N5 O4 127.4(13) . . ? O4A N5 O3 61.3(16) . . ? O5 N5 O3 116.0(13) . . ? O4 N5 O3 116.6(11) . . ? O4A N5 O3A 116(2) . . ? O5 N5 O3A 53.2(11) . . ? O4 N5 O3A 177.2(13) . . ? O3 N5 O3A 63.0(11) . . ? O4A N5 O5A 146(2) . . ? O5 N5 O5A 42.9(12) . . ? O4 N5 O5A 86.6(14) . . ? O3 N5 O5A 152.1(15) . . ? O3A N5 O5A 94.6(16) . . ? O1 C1 C2 124.2(5) . . ? O1 C1 C6 118.3(5) . . ? C2 C1 C6 117.5(5) . . ? C1 C2 C3 121.8(6) . . ? C4 C3 C2 121.1(6) . . ? C3 C4 C5 120.5(6) . . ? C4 C5 C6 119.2(6) . . ? C4 C5 C9 126.1(6) . . ? C6 C5 C9 114.7(6) . . ? N1 C6 C5 123.8(5) . . ? N1 C6 C1 116.3(4) . . ? C5 C6 C1 119.9(5) . . ? N1 C7 C8 120.1(6) . . ? N1 C7 C10 120.6(5) . . ? C8 C7 C10 119.4(5) . . ? C9 C8 C7 121.2(6) . . ? C8 C9 C5 121.0(6) . . ? O2 C11 C12 123.3(6) . . ? O2 C11 C16 118.6(5) . . ? C12 C11 C16 118.1(6) . . ? C11 C12 C13 118.8(7) . . ? C14 C13 C12 124.6(7) . . ? C13 C14 C15 118.8(6) . . ? C19 C15 C16 116.1(7) . . ? C19 C15 C14 124.6(7) . . ? C16 C15 C14 119.3(6) . . ? N2 C16 C15 123.7(6) . . ? N2 C16 C11 115.8(5) . . ? C15 C16 C11 120.5(6) . . ? N2 C17 C18 119.7(6) . . ? N2 C17 C20 120.5(6) . . ? C18 C17 C20 119.8(6) . . ? C19 C18 C17 121.1(7) . . ? C18 C19 C15 120.3(7) . . ? N3 C21 C22 121.9(6) . . ? C23 C22 C21 118.9(7) . . ? C22 C23 C24 120.2(6) . . ? C23 C24 C25 119.2(6) . . ? N3 C25 C24 120.5(6) . . ? N3 C25 C26 116.0(4) . . ? C24 C25 C26 123.5(5) . . ? N4 C26 C27 120.0(6) . . ? N4 C26 C25 116.2(5) . . ? C27 C26 C25 123.8(5) . . ? C28 C27 C26 119.9(6) . . ? C29 C28 C27 118.9(6) . . ? C28 C29 C30 119.4(7) . . ? N4 C30 C29 121.9(6) . . ? Cl1 C31 Cl2 109.6(15) . . ? 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 O2 Ga O1 C1 -169(3) . . . . ? N3 Ga O1 C1 179.6(4) . . . . ? N4 Ga O1 C1 -102.1(4) . . . . ? N1 Ga O1 C1 -7.2(4) . . . . ? N2 Ga O1 C1 83.5(4) . . . . ? O1 Ga O2 C11 -116(3) . . . . ? N3 Ga O2 C11 -104.5(4) . . . . ? N4 Ga O2 C11 177.1(4) . . . . ? N1 Ga O2 C11 82.4(4) . . . . ? N2 Ga O2 C11 -7.9(4) . . . . ? O2 Ga N1 C7 2.3(5) . . . . ? O1 Ga N1 C7 -176.7(5) . . . . ? N3 Ga N1 C7 -144.5(7) . . . . ? N4 Ga N1 C7 -85.5(5) . . . . ? N2 Ga N1 C7 84.2(5) . . . . ? O2 Ga N1 C6 -173.1(3) . . . . ? O1 Ga N1 C6 7.9(3) . . . . ? N3 Ga N1 C6 40.1(9) . . . . ? N4 Ga N1 C6 99.0(3) . . . . ? N2 Ga N1 C6 -91.2(3) . . . . ? O2 Ga N2 C17 -178.5(6) . . . . ? O1 Ga N2 C17 -1.4(6) . . . . ? N3 Ga N2 C17 -88.9(6) . . . . ? N4 Ga N2 C17 -154.3(8) . . . . ? N1 Ga N2 C17 81.5(6) . . . . ? O2 Ga N2 C16 8.2(3) . . . . ? O1 Ga N2 C16 -174.7(3) . . . . ? N3 Ga N2 C16 97.8(3) . . . . ? N4 Ga N2 C16 32.4(10) . . . . ? N1 Ga N2 C16 -91.8(3) . . . . ? O2 Ga N3 C21 92.8(5) . . . . ? O1 Ga N3 C21 -87.8(5) . . . . ? N4 Ga N3 C21 179.7(5) . . . . ? N1 Ga N3 C21 -119.8(8) . . . . ? N2 Ga N3 C21 11.1(5) . . . . ? O2 Ga N3 C25 -85.8(4) . . . . ? O1 Ga N3 C25 93.6(4) . . . . ? N4 Ga N3 C25 1.0(4) . . . . ? N1 Ga N3 C25 61.6(9) . . . . ? N2 Ga N3 C25 -167.5(4) . . . . ? O2 Ga N4 C30 -89.3(5) . . . . ? O1 Ga N4 C30 93.5(5) . . . . ? N3 Ga N4 C30 179.6(5) . . . . ? N1 Ga N4 C30 10.6(5) . . . . ? N2 Ga N4 C30 -113.2(8) . . . . ? O2 Ga N4 C26 90.6(4) . . . . ? O1 Ga N4 C26 -86.6(4) . . . . ? N3 Ga N4 C26 -0.5(4) . . . . ? N1 Ga N4 C26 -169.5(4) . . . . ? N2 Ga N4 C26 66.7(9) . . . . ? Ga O1 C1 C2 -176.5(5) . . . . ? Ga O1 C1 C6 5.2(6) . . . . ? O1 C1 C2 C3 178.5(6) . . . . ? C6 C1 C2 C3 -3.2(9) . . . . ? C1 C2 C3 C4 2.8(11) . . . . ? C2 C3 C4 C5 -1.1(12) . . . . ? C3 C4 C5 C6 0.1(10) . . . . ? C3 C4 C5 C9 178.1(7) . . . . ? C7 N1 C6 C5 -1.9(8) . . . . ? Ga N1 C6 C5 174.4(5) . . . . ? C7 N1 C6 C1 176.4(5) . . . . ? Ga N1 C6 C1 -7.4(5) . . . . ? C4 C5 C6 N1 177.5(6) . . . . ? C9 C5 C6 N1 -0.7(9) . . . . ? C4 C5 C6 C1 -0.6(9) . . . . ? C9 C5 C6 C1 -178.8(6) . . . . ? O1 C1 C6 N1 2.3(7) . . . . ? C2 C1 C6 N1 -176.2(5) . . . . ? O1 C1 C6 C5 -179.4(5) . . . . ? C2 C1 C6 C5 2.1(8) . . . . ? C6 N1 C7 C8 2.9(8) . . . . ? Ga N1 C7 C8 -172.1(4) . . . . ? C6 N1 C7 C10 -175.6(5) . . . . ? Ga N1 C7 C10 9.4(8) . . . . ? N1 C7 C8 C9 -1.4(10) . . . . ? C10 C7 C8 C9 177.1(7) . . . . ? C7 C8 C9 C5 -1.2(11) . . . . ? C4 C5 C9 C8 -175.9(7) . . . . ? C6 C5 C9 C8 2.2(10) . . . . ? Ga O2 C11 C12 -173.3(4) . . . . ? Ga O2 C11 C16 6.3(6) . . . . ? O2 C11 C12 C13 -179.4(5) . . . . ? C16 C11 C12 C13 1.0(9) . . . . ? C11 C12 C13 C14 -2.0(11) . . . . ? C12 C13 C14 C15 1.2(11) . . . . ? C13 C14 C15 C19 179.5(7) . . . . ? C13 C14 C15 C16 0.4(10) . . . . ? C17 N2 C16 C15 -1.1(8) . . . . ? Ga N2 C16 C15 173.4(4) . . . . ? C17 N2 C16 C11 178.2(5) . . . . ? Ga N2 C16 C11 -7.3(6) . . . . ? C19 C15 C16 N2 -1.2(8) . . . . ? C14 C15 C16 N2 177.9(5) . . . . ? C19 C15 C16 C11 179.6(6) . . . . ? C14 C15 C16 C11 -1.3(8) . . . . ? O2 C11 C16 N2 1.6(7) . . . . ? C12 C11 C16 N2 -178.7(5) . . . . ? O2 C11 C16 C15 -179.1(5) . . . . ? C12 C11 C16 C15 0.6(8) . . . . ? C16 N2 C17 C18 2.2(9) . . . . ? Ga N2 C17 C18 -170.4(5) . . . . ? C16 N2 C17 C20 -175.9(6) . . . . ? Ga N2 C17 C20 11.5(10) . . . . ? N2 C17 C18 C19 -1.2(11) . . . . ? C20 C17 C18 C19 176.9(8) . . . . ? C17 C18 C19 C15 -1.1(12) . . . . ? C16 C15 C19 C18 2.2(10) . . . . ? C14 C15 C19 C18 -176.9(7) . . . . ? C25 N3 C21 C22 0.0(9) . . . . ? Ga N3 C21 C22 -178.6(5) . . . . ? N3 C21 C22 C23 0.4(10) . . . . ? C21 C22 C23 C24 -0.6(11) . . . . ? C22 C23 C24 C25 0.3(11) . . . . ? C21 N3 C25 C24 -0.3(8) . . . . ? Ga N3 C25 C24 178.4(4) . . . . ? C21 N3 C25 C26 179.9(5) . . . . ? Ga N3 C25 C26 -1.4(6) . . . . ? C23 C24 C25 N3 0.2(9) . . . . ? C23 C24 C25 C26 179.9(6) . . . . ? C30 N4 C26 C27 -1.2(8) . . . . ? Ga N4 C26 C27 178.9(4) . . . . ? C30 N4 C26 C25 179.9(5) . . . . ? Ga N4 C26 C25 0.0(6) . . . . ? N3 C25 C26 N4 0.9(7) . . . . ? C24 C25 C26 N4 -178.9(5) . . . . ? N3 C25 C26 C27 -178.0(5) . . . . ? C24 C25 C26 C27 2.3(9) . . . . ? N4 C26 C27 C28 0.6(9) . . . . ? C25 C26 C27 C28 179.4(6) . . . . ? C26 C27 C28 C29 0.7(10) . . . . ? C27 C28 C29 C30 -1.3(10) . . . . ? C26 N4 C30 C29 0.5(9) . . . . ? Ga N4 C30 C29 -179.6(4) . . . . ? C28 C29 C30 N4 0.7(10) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.264 _refine_diff_density_min -0.498 #===END data_(2a) _database_code_depnum_ccdc_archive 'CCDC 665246' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C32 H24 Ga N4 O2, C2 H5 O, N O3' _chemical_formula_sum 'C34 H29 Ga N5 O6' _chemical_formula_weight 673.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M ' P 21/n ' _symmetry_space_group_name_Hall ' -P 2yn ' 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 11.8012(7) _cell_length_b 19.8165(12) _cell_length_c 13.4428(8) _cell_angle_alpha 90.00 _cell_angle_beta 97.022(3) _cell_angle_gamma 90.00 _cell_volume 3120.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 7529 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 28.28 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1388 _exptl_absorpt_coefficient_mu 0.936 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54939 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.0696 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7680 _reflns_number_gt 3910 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0730P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _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 7680 _refine_ls_number_parameters 417 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0960 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1242 _refine_ls_wR_factor_gt 0.1141 _refine_ls_goodness_of_fit_ref 0.890 _refine_ls_restrained_S_all 0.890 _refine_ls_shift/su_max 0.006 _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 Ga Ga 0.27398(2) 0.661501(13) 0.373987(19) 0.04305(12) Uani 1 1 d . . . N1 N 0.18192(16) 0.74224(10) 0.43378(14) 0.0441(5) Uani 1 1 d . . . N2 N 0.15824(17) 0.65356(10) 0.23975(15) 0.0453(5) Uani 1 1 d . . . N4 N 0.38534(17) 0.64682(9) 0.50871(15) 0.0455(5) Uani 1 1 d . . . N3 N 0.40048(16) 0.59949(9) 0.32337(14) 0.0442(5) Uani 1 1 d . . . N5 N 0.8024(2) 0.91034(15) 0.4284(2) 0.0715(7) Uani 1 1 d . . . O1 O 0.36605(13) 0.73399(8) 0.33735(12) 0.0493(4) Uani 1 1 d . . . O2 O 0.19012(14) 0.58596(8) 0.41251(12) 0.0490(4) Uani 1 1 d . . . O3 O 0.7853(3) 0.90437(14) 0.3379(2) 0.1189(10) Uani 1 1 d . . . O4 O 0.8569(3) 0.96172(15) 0.4574(2) 0.1284(10) Uani 1 1 d . . . O5 O 0.7748(3) 0.8737(2) 0.4849(3) 0.1902(19) Uani 1 1 d . . . C1 C 0.3297(2) 0.79508(13) 0.35573(17) 0.0456(6) Uani 1 1 d . . . C2 C 0.3810(2) 0.85337(13) 0.3267(2) 0.0577(7) Uani 1 1 d . . . H2 H 0.4445 0.8503 0.2923 0.069 Uiso 1 1 calc R . . C3 C 0.3382(3) 0.91711(14) 0.3485(2) 0.0636(8) Uani 1 1 d . . . H3 H 0.3736 0.9556 0.3276 0.076 Uiso 1 1 calc R . . C4 C 0.2457(3) 0.92376(13) 0.3995(2) 0.0621(8) Uani 1 1 d . . . H4 H 0.2197 0.9665 0.4142 0.075 Uiso 1 1 calc R . . C5 C 0.1898(2) 0.86608(14) 0.42993(19) 0.0530(7) Uani 1 1 d . . . C6 C 0.2310(2) 0.80132(12) 0.40746(17) 0.0452(6) Uani 1 1 d . . . C7 C 0.0910(2) 0.74534(14) 0.4838(2) 0.0543(7) Uani 1 1 d . . . C8 C 0.0460(2) 0.80820(16) 0.5085(2) 0.0695(8) Uani 1 1 d . . . H8 H -0.0170 0.8095 0.5438 0.083 Uiso 1 1 calc R . . C9 C 0.0929(3) 0.86673(16) 0.4817(2) 0.0724(9) Uani 1 1 d . . . H9 H 0.0610 0.9077 0.4975 0.087 Uiso 1 1 calc R . . C10 C 0.0363(3) 0.68153(16) 0.5152(2) 0.0768(9) Uani 1 1 d . . . H10A H 0.0938 0.6476 0.5308 0.115 Uiso 1 1 calc R . . H10B H -0.0187 0.6659 0.4616 0.115 Uiso 1 1 calc R . . H10C H -0.0012 0.6903 0.5734 0.115 Uiso 1 1 calc R . . C11 C 0.1034(2) 0.56691(13) 0.34646(19) 0.0483(6) Uani 1 1 d . . . C12 C 0.0316(2) 0.51390(13) 0.3624(2) 0.0587(7) Uani 1 1 d . . . H12 H 0.0450 0.4889 0.4213 0.070 Uiso 1 1 calc R . . C13 C -0.0614(3) 0.49716(17) 0.2909(3) 0.0775(9) Uani 1 1 d . . . H13 H -0.1090 0.4615 0.3035 0.093 Uiso 1 1 calc R . . C14 C -0.0830(3) 0.53255(18) 0.2033(3) 0.0810(10) Uani 1 1 d . . . H14 H -0.1449 0.5210 0.1568 0.097 Uiso 1 1 calc R . . C15 C -0.0115(2) 0.58617(16) 0.1836(2) 0.0628(8) Uani 1 1 d . . . C16 C 0.0819(2) 0.60328(12) 0.25461(18) 0.0466(6) Uani 1 1 d . . . C17 C 0.1464(2) 0.68778(14) 0.15248(18) 0.0519(7) Uani 1 1 d . . . C18 C 0.0530(3) 0.67382(17) 0.0807(2) 0.0722(9) Uani 1 1 d . . . H18 H 0.0435 0.6988 0.0217 0.087 Uiso 1 1 calc R . . C19 C -0.0237(3) 0.62525(17) 0.0945(2) 0.0765(9) Uani 1 1 d . . . H19 H -0.0849 0.6174 0.0454 0.092 Uiso 1 1 calc R . . C20 C 0.2320(3) 0.73933(15) 0.13201(19) 0.0665(8) Uani 1 1 d . . . H20A H 0.3074 0.7220 0.1512 0.100 Uiso 1 1 calc R . . H20B H 0.2211 0.7794 0.1698 0.100 Uiso 1 1 calc R . . H20C H 0.2226 0.7499 0.0618 0.100 Uiso 1 1 calc R . . C21 C 0.4062(2) 0.57645(12) 0.23143(19) 0.0511(6) Uani 1 1 d . . . H21 H 0.3461 0.5856 0.1818 0.061 Uiso 1 1 calc R . . C22 C 0.4987(2) 0.53903(12) 0.2062(2) 0.0573(7) Uani 1 1 d . . . H22 H 0.4996 0.5235 0.1410 0.069 Uiso 1 1 calc R . . C23 C 0.5874(2) 0.52540(13) 0.2777(2) 0.0602(7) Uani 1 1 d . . . H23 H 0.6496 0.5006 0.2616 0.072 Uiso 1 1 calc R . . C24 C 0.5850(2) 0.54901(12) 0.3764(2) 0.0495(7) Uani 1 1 d . . . C25 C 0.48909(19) 0.58638(11) 0.39524(18) 0.0419(6) Uani 1 1 d . . . C26 C 0.4800(2) 0.61119(11) 0.49403(18) 0.0431(6) Uani 1 1 d . . . C27 C 0.3729(2) 0.66823(13) 0.60059(19) 0.0574(7) Uani 1 1 d . . . H27 H 0.3075 0.6922 0.6107 0.069 Uiso 1 1 calc R . . C28 C 0.4553(3) 0.65575(14) 0.6821(2) 0.0657(8) Uani 1 1 d . . . H28 H 0.4445 0.6711 0.7456 0.079 Uiso 1 1 calc R . . C29 C 0.5519(2) 0.62092(14) 0.6682(2) 0.0607(7) Uani 1 1 d . . . H29 H 0.6076 0.6130 0.7221 0.073 Uiso 1 1 calc R . . C30 C 0.5669(2) 0.59728(12) 0.5732(2) 0.0505(6) Uani 1 1 d . . . C31 C 0.6638(2) 0.55927(14) 0.5511(2) 0.0631(8) Uani 1 1 d . . . H31 H 0.7220 0.5500 0.6023 0.076 Uiso 1 1 calc R . . C32 C 0.6728(2) 0.53647(14) 0.4577(2) 0.0659(8) Uani 1 1 d . . . H32 H 0.7373 0.5122 0.4459 0.079 Uiso 1 1 calc R . . C33 C 0.6663(4) 0.7301(2) 0.2940(4) 0.1324(16) Uani 1 1 d . . . H33A H 0.6444 0.7376 0.3604 0.159 Uiso 1 1 calc R . . H33B H 0.6088 0.7015 0.2575 0.159 Uiso 1 1 calc R . . C34 C 0.7687(5) 0.6977(3) 0.3027(6) 0.225(4) Uani 1 1 d . . . H34A H 0.7626 0.6555 0.3366 0.338 Uiso 1 1 calc R . . H34B H 0.8257 0.7252 0.3403 0.338 Uiso 1 1 calc R . . H34C H 0.7903 0.6895 0.2371 0.338 Uiso 1 1 calc R . . O6 O 0.6689(2) 0.79330(14) 0.2437(2) 0.1213(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 Ga 0.04084(18) 0.04590(19) 0.04163(18) -0.00268(12) 0.00197(12) 0.00527(12) N1 0.0378(11) 0.0511(13) 0.0421(12) -0.0029(10) 0.0003(10) 0.0060(10) N2 0.0408(12) 0.0515(13) 0.0427(13) -0.0026(10) 0.0019(10) 0.0074(10) N4 0.0424(12) 0.0524(12) 0.0406(12) -0.0038(9) 0.0008(10) 0.0002(10) N3 0.0444(12) 0.0453(12) 0.0418(12) -0.0039(9) 0.0011(10) 0.0052(10) N5 0.0651(17) 0.0758(19) 0.076(2) 0.0093(17) 0.0174(16) 0.0112(15) O1 0.0461(10) 0.0453(10) 0.0578(11) -0.0053(8) 0.0114(8) 0.0028(8) O2 0.0494(10) 0.0516(10) 0.0442(10) 0.0026(8) -0.0023(8) -0.0001(8) O3 0.157(3) 0.122(2) 0.0823(19) 0.0042(17) 0.0324(18) 0.0025(19) O4 0.117(2) 0.113(2) 0.159(3) -0.037(2) 0.030(2) 0.0009(19) O5 0.163(3) 0.228(4) 0.193(4) 0.140(3) 0.080(3) 0.015(3) C1 0.0458(15) 0.0509(17) 0.0383(14) -0.0045(12) -0.0022(12) 0.0003(13) C2 0.0603(18) 0.0579(18) 0.0542(17) -0.0004(13) 0.0041(14) -0.0081(14) C3 0.086(2) 0.0474(17) 0.0532(17) 0.0033(13) -0.0072(16) -0.0020(16) C4 0.083(2) 0.0410(16) 0.0575(17) -0.0057(13) -0.0104(16) 0.0182(16) C5 0.0595(17) 0.0542(16) 0.0420(15) -0.0050(13) -0.0073(13) 0.0171(15) C6 0.0459(15) 0.0501(17) 0.0367(13) -0.0051(12) -0.0067(12) 0.0110(13) C7 0.0460(16) 0.0666(18) 0.0509(16) -0.0048(13) 0.0081(13) 0.0068(14) C8 0.0609(19) 0.079(2) 0.072(2) -0.0089(18) 0.0220(16) 0.0218(18) C9 0.077(2) 0.069(2) 0.071(2) -0.0122(17) 0.0057(18) 0.0299(19) C10 0.065(2) 0.093(2) 0.078(2) -0.0053(18) 0.0295(18) -0.0029(18) C11 0.0420(15) 0.0512(15) 0.0518(17) -0.0080(13) 0.0059(13) 0.0063(12) C12 0.0522(17) 0.0627(18) 0.0626(18) -0.0026(14) 0.0130(14) -0.0049(15) C13 0.0584(19) 0.084(2) 0.092(3) -0.016(2) 0.0170(19) -0.0263(17) C14 0.0506(19) 0.111(3) 0.079(2) -0.017(2) -0.0031(17) -0.0138(19) C15 0.0430(16) 0.086(2) 0.0568(19) -0.0115(16) -0.0029(14) 0.0012(16) C16 0.0401(14) 0.0547(16) 0.0446(15) -0.0069(12) 0.0043(12) 0.0088(13) C17 0.0576(17) 0.0581(16) 0.0388(15) -0.0023(13) 0.0014(13) 0.0166(14) C18 0.070(2) 0.098(2) 0.0449(17) 0.0063(16) -0.0076(16) 0.0161(19) C19 0.058(2) 0.114(3) 0.0520(19) -0.0035(19) -0.0154(16) -0.002(2) C20 0.093(2) 0.0564(17) 0.0502(17) 0.0037(13) 0.0104(16) 0.0070(16) C21 0.0523(16) 0.0532(15) 0.0479(16) -0.0087(13) 0.0066(13) 0.0015(13) C22 0.0653(19) 0.0503(16) 0.0591(18) -0.0101(13) 0.0193(16) 0.0013(14) C23 0.0583(18) 0.0467(16) 0.080(2) -0.0005(15) 0.0273(17) 0.0058(13) C24 0.0429(15) 0.0415(15) 0.0644(18) 0.0062(13) 0.0072(14) 0.0028(12) C25 0.0396(14) 0.0355(13) 0.0510(15) 0.0036(11) 0.0065(12) 0.0002(11) C26 0.0400(14) 0.0377(13) 0.0513(15) 0.0053(11) 0.0042(12) -0.0022(11) C27 0.0570(17) 0.0702(19) 0.0446(16) -0.0072(13) 0.0040(14) 0.0018(14) C28 0.074(2) 0.083(2) 0.0370(16) 0.0006(14) -0.0030(15) -0.0117(18) C29 0.0572(19) 0.0705(19) 0.0510(18) 0.0152(15) -0.0070(14) -0.0066(15) C30 0.0434(15) 0.0504(15) 0.0556(17) 0.0100(13) -0.0022(13) -0.0054(12) C31 0.0481(17) 0.0647(19) 0.073(2) 0.0154(16) -0.0079(15) 0.0069(14) C32 0.0473(17) 0.0588(18) 0.092(2) 0.0126(17) 0.0104(17) 0.0122(14) C33 0.139(4) 0.123(4) 0.137(4) 0.029(3) 0.024(3) -0.036(3) C34 0.106(4) 0.160(5) 0.415(11) 0.123(6) 0.052(5) 0.013(4) O6 0.134(2) 0.125(2) 0.102(2) 0.0195(17) 0.0063(17) -0.0115(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga O2 1.9010(16) . ? Ga O1 1.9019(16) . ? Ga N3 2.1095(19) . ? Ga N4 2.124(2) . ? Ga N2 2.132(2) . ? Ga N1 2.1448(19) . ? N1 C7 1.336(3) . ? N1 C6 1.372(3) . ? N2 C17 1.347(3) . ? N2 C16 1.374(3) . ? N4 C27 1.331(3) . ? N4 C26 1.356(3) . ? N3 C21 1.327(3) . ? N3 C25 1.359(3) . ? N5 O5 1.126(3) . ? N5 O3 1.215(3) . ? N5 O4 1.241(3) . ? O1 C1 1.318(3) . ? O2 C11 1.325(3) . ? C1 C2 1.382(3) . ? C1 C6 1.433(3) . ? C2 C3 1.404(4) . ? C3 C4 1.364(4) . ? C4 C5 1.406(4) . ? C5 C9 1.410(4) . ? C5 C6 1.418(3) . ? C7 C8 1.409(4) . ? C7 C10 1.503(4) . ? C8 C9 1.353(4) . ? C11 C12 1.383(3) . ? C11 C16 1.425(3) . ? C12 C13 1.407(4) . ? C13 C14 1.368(4) . ? C14 C15 1.402(4) . ? C15 C16 1.409(3) . ? C15 C19 1.419(4) . ? C17 C18 1.402(4) . ? C17 C20 1.485(4) . ? C18 C19 1.349(4) . ? C21 C22 1.395(3) . ? C22 C23 1.359(4) . ? C23 C24 1.411(4) . ? C24 C25 1.401(3) . ? C24 C32 1.432(4) . ? C25 C26 1.432(3) . ? C26 C30 1.411(3) . ? C27 C28 1.395(4) . ? C28 C29 1.364(4) . ? C29 C30 1.393(4) . ? C30 C31 1.431(4) . ? C31 C32 1.351(4) . ? C33 C34 1.362(6) . ? C33 O6 1.426(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ga O1 176.55(7) . . ? O2 Ga N3 92.39(7) . . ? O1 Ga N3 84.67(7) . . ? O2 Ga N4 87.04(7) . . ? O1 Ga N4 90.62(7) . . ? N3 Ga N4 78.86(8) . . ? O2 Ga N2 82.61(7) . . ? O1 Ga N2 99.43(8) . . ? N3 Ga N2 95.13(7) . . ? N4 Ga N2 167.82(8) . . ? O2 Ga N1 100.42(8) . . ? O1 Ga N1 82.25(7) . . ? N3 Ga N1 165.09(8) . . ? N4 Ga N1 94.11(7) . . ? N2 Ga N1 94.06(7) . . ? C7 N1 C6 118.8(2) . . ? C7 N1 Ga 134.26(18) . . ? C6 N1 Ga 106.90(14) . . ? C17 N2 C16 119.4(2) . . ? C17 N2 Ga 133.41(18) . . ? C16 N2 Ga 107.11(15) . . ? C27 N4 C26 119.2(2) . . ? C27 N4 Ga 128.38(18) . . ? C26 N4 Ga 112.46(15) . . ? C21 N3 C25 118.3(2) . . ? C21 N3 Ga 128.28(17) . . ? C25 N3 Ga 113.29(15) . . ? O5 N5 O3 125.9(4) . . ? O5 N5 O4 119.9(4) . . ? O3 N5 O4 114.2(3) . . ? C1 O1 Ga 115.84(15) . . ? C11 O2 Ga 115.27(15) . . ? O1 C1 C2 123.4(2) . . ? O1 C1 C6 118.2(2) . . ? C2 C1 C6 118.3(2) . . ? C1 C2 C3 120.8(3) . . ? C4 C3 C2 121.5(3) . . ? C3 C4 C5 120.0(3) . . ? C4 C5 C9 125.1(3) . . ? C4 C5 C6 119.3(3) . . ? C9 C5 C6 115.7(3) . . ? N1 C6 C5 123.4(2) . . ? N1 C6 C1 116.5(2) . . ? C5 C6 C1 120.1(2) . . ? N1 C7 C8 120.5(3) . . ? N1 C7 C10 120.1(2) . . ? C8 C7 C10 119.4(3) . . ? C9 C8 C7 121.1(3) . . ? C8 C9 C5 120.5(3) . . ? O2 C11 C12 123.4(2) . . ? O2 C11 C16 118.5(2) . . ? C12 C11 C16 118.1(2) . . ? C11 C12 C13 121.0(3) . . ? C14 C13 C12 121.0(3) . . ? C13 C14 C15 119.9(3) . . ? C14 C15 C16 119.6(3) . . ? C14 C15 C19 124.9(3) . . ? C16 C15 C19 115.5(3) . . ? N2 C16 C15 123.3(2) . . ? N2 C16 C11 116.2(2) . . ? C15 C16 C11 120.5(2) . . ? N2 C17 C18 119.3(3) . . ? N2 C17 C20 120.5(2) . . ? C18 C17 C20 120.2(2) . . ? C19 C18 C17 122.0(3) . . ? C18 C19 C15 120.3(3) . . ? N3 C21 C22 122.7(2) . . ? C23 C22 C21 119.4(2) . . ? C22 C23 C24 119.8(2) . . ? C25 C24 C23 117.1(2) . . ? C25 C24 C32 118.7(2) . . ? C23 C24 C32 124.3(2) . . ? N3 C25 C24 122.8(2) . . ? N3 C25 C26 117.1(2) . . ? C24 C25 C26 120.1(2) . . ? N4 C26 C30 121.8(2) . . ? N4 C26 C25 118.0(2) . . ? C30 C26 C25 120.2(2) . . ? N4 C27 C28 121.8(3) . . ? C29 C28 C27 119.8(3) . . ? C28 C29 C30 119.8(3) . . ? C29 C30 C26 117.7(2) . . ? C29 C30 C31 124.2(3) . . ? C26 C30 C31 118.2(2) . . ? C32 C31 C30 121.6(3) . . ? C31 C32 C24 121.2(3) . . ? C34 C33 O6 112.6(4) . . ? 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 O2 Ga N1 C7 -0.5(2) . . . . ? O1 Ga N1 C7 -178.3(2) . . . . ? N3 Ga N1 C7 -149.4(3) . . . . ? N4 Ga N1 C7 -88.3(2) . . . . ? N2 Ga N1 C7 82.7(2) . . . . ? O2 Ga N1 C6 -177.50(14) . . . . ? O1 Ga N1 C6 4.70(14) . . . . ? N3 Ga N1 C6 33.7(4) . . . . ? N4 Ga N1 C6 94.76(15) . . . . ? N2 Ga N1 C6 -94.28(15) . . . . ? O2 Ga N2 C17 -178.0(2) . . . . ? O1 Ga N2 C17 -0.8(2) . . . . ? N3 Ga N2 C17 -86.3(2) . . . . ? N4 Ga N2 C17 -146.0(3) . . . . ? N1 Ga N2 C17 82.0(2) . . . . ? O2 Ga N2 C16 4.32(14) . . . . ? O1 Ga N2 C16 -178.49(14) . . . . ? N3 Ga N2 C16 96.08(14) . . . . ? N4 Ga N2 C16 36.3(4) . . . . ? N1 Ga N2 C16 -95.68(15) . . . . ? O2 Ga N4 C27 -83.4(2) . . . . ? O1 Ga N4 C27 99.1(2) . . . . ? N3 Ga N4 C27 -176.4(2) . . . . ? N2 Ga N4 C27 -115.2(4) . . . . ? N1 Ga N4 C27 16.8(2) . . . . ? O2 Ga N4 C26 97.16(16) . . . . ? O1 Ga N4 C26 -80.31(16) . . . . ? N3 Ga N4 C26 4.14(15) . . . . ? N2 Ga N4 C26 65.4(4) . . . . ? N1 Ga N4 C26 -162.59(16) . . . . ? O2 Ga N3 C21 93.2(2) . . . . ? O1 Ga N3 C21 -88.6(2) . . . . ? N4 Ga N3 C21 179.7(2) . . . . ? N2 Ga N3 C21 10.4(2) . . . . ? N1 Ga N3 C21 -117.4(3) . . . . ? O2 Ga N3 C25 -91.26(16) . . . . ? O1 Ga N3 C25 86.93(16) . . . . ? N4 Ga N3 C25 -4.76(15) . . . . ? N2 Ga N3 C25 -174.05(16) . . . . ? N1 Ga N3 C25 58.1(4) . . . . ? O2 Ga O1 C1 -146.2(11) . . . . ? N3 Ga O1 C1 -177.89(16) . . . . ? N4 Ga O1 C1 -99.14(16) . . . . ? N2 Ga O1 C1 87.78(16) . . . . ? N1 Ga O1 C1 -5.08(15) . . . . ? O1 Ga O2 C11 -129.1(11) . . . . ? N3 Ga O2 C11 -97.56(16) . . . . ? N4 Ga O2 C11 -176.26(16) . . . . ? N2 Ga O2 C11 -2.69(16) . . . . ? N1 Ga O2 C11 90.10(16) . . . . ? Ga O1 C1 C2 -174.63(19) . . . . ? Ga O1 C1 C6 4.6(3) . . . . ? O1 C1 C2 C3 180.0(2) . . . . ? C6 C1 C2 C3 0.8(4) . . . . ? C1 C2 C3 C4 0.6(4) . . . . ? C2 C3 C4 C5 -1.2(4) . . . . ? C3 C4 C5 C9 -179.1(3) . . . . ? C3 C4 C5 C6 0.4(4) . . . . ? C7 N1 C6 C5 -0.5(3) . . . . ? Ga N1 C6 C5 177.05(18) . . . . ? C7 N1 C6 C1 178.8(2) . . . . ? Ga N1 C6 C1 -3.7(2) . . . . ? C4 C5 C6 N1 -179.8(2) . . . . ? C9 C5 C6 N1 -0.3(3) . . . . ? C4 C5 C6 C1 1.0(3) . . . . ? C9 C5 C6 C1 -179.5(2) . . . . ? O1 C1 C6 N1 -0.1(3) . . . . ? C2 C1 C6 N1 179.2(2) . . . . ? O1 C1 C6 C5 179.2(2) . . . . ? C2 C1 C6 C5 -1.6(3) . . . . ? C6 N1 C7 C8 0.4(4) . . . . ? Ga N1 C7 C8 -176.31(18) . . . . ? C6 N1 C7 C10 -179.0(2) . . . . ? Ga N1 C7 C10 4.3(4) . . . . ? N1 C7 C8 C9 0.5(4) . . . . ? C10 C7 C8 C9 179.9(3) . . . . ? C7 C8 C9 C5 -1.3(4) . . . . ? C4 C5 C9 C8 -179.4(3) . . . . ? C6 C5 C9 C8 1.2(4) . . . . ? Ga O2 C11 C12 -178.66(18) . . . . ? Ga O2 C11 C16 0.5(3) . . . . ? O2 C11 C12 C13 178.0(2) . . . . ? C16 C11 C12 C13 -1.2(4) . . . . ? C11 C12 C13 C14 0.5(4) . . . . ? C12 C13 C14 C15 0.3(5) . . . . ? C13 C14 C15 C16 -0.2(4) . . . . ? C13 C14 C15 C19 178.3(3) . . . . ? C17 N2 C16 C15 -1.7(3) . . . . ? Ga N2 C16 C15 176.4(2) . . . . ? C17 N2 C16 C11 176.7(2) . . . . ? Ga N2 C16 C11 -5.2(2) . . . . ? C14 C15 C16 N2 177.7(2) . . . . ? C19 C15 C16 N2 -0.9(4) . . . . ? C14 C15 C16 C11 -0.6(4) . . . . ? C19 C15 C16 C11 -179.2(2) . . . . ? O2 C11 C16 N2 3.6(3) . . . . ? C12 C11 C16 N2 -177.2(2) . . . . ? O2 C11 C16 C15 -178.0(2) . . . . ? C12 C11 C16 C15 1.3(3) . . . . ? C16 N2 C17 C18 3.3(3) . . . . ? Ga N2 C17 C18 -174.09(18) . . . . ? C16 N2 C17 C20 -176.1(2) . . . . ? Ga N2 C17 C20 6.4(4) . . . . ? N2 C17 C18 C19 -2.5(4) . . . . ? C20 C17 C18 C19 176.9(3) . . . . ? C17 C18 C19 C15 -0.1(5) . . . . ? C14 C15 C19 C18 -176.8(3) . . . . ? C16 C15 C19 C18 1.8(4) . . . . ? C25 N3 C21 C22 0.6(4) . . . . ? Ga N3 C21 C22 175.87(17) . . . . ? N3 C21 C22 C23 -0.3(4) . . . . ? C21 C22 C23 C24 0.2(4) . . . . ? C22 C23 C24 C25 -0.4(4) . . . . ? C22 C23 C24 C32 178.8(2) . . . . ? C21 N3 C25 C24 -0.8(3) . . . . ? Ga N3 C25 C24 -176.79(17) . . . . ? C21 N3 C25 C26 -179.3(2) . . . . ? Ga N3 C25 C26 4.7(2) . . . . ? C23 C24 C25 N3 0.7(3) . . . . ? C32 C24 C25 N3 -178.5(2) . . . . ? C23 C24 C25 C26 179.2(2) . . . . ? C32 C24 C25 C26 -0.1(3) . . . . ? C27 N4 C26 C30 -1.2(3) . . . . ? Ga N4 C26 C30 178.24(17) . . . . ? C27 N4 C26 C25 177.5(2) . . . . ? Ga N4 C26 C25 -3.0(3) . . . . ? N3 C25 C26 N4 -1.1(3) . . . . ? C24 C25 C26 N4 -179.7(2) . . . . ? N3 C25 C26 C30 177.6(2) . . . . ? C24 C25 C26 C30 -0.9(3) . . . . ? C26 N4 C27 C28 0.8(4) . . . . ? Ga N4 C27 C28 -178.57(19) . . . . ? N4 C27 C28 C29 0.2(4) . . . . ? C27 C28 C29 C30 -0.8(4) . . . . ? C28 C29 C30 C26 0.4(4) . . . . ? C28 C29 C30 C31 -178.8(2) . . . . ? N4 C26 C30 C29 0.6(3) . . . . ? C25 C26 C30 C29 -178.1(2) . . . . ? N4 C26 C30 C31 179.9(2) . . . . ? C25 C26 C30 C31 1.2(3) . . . . ? C29 C30 C31 C32 178.7(3) . . . . ? C26 C30 C31 C32 -0.5(4) . . . . ? C30 C31 C32 C24 -0.4(4) . . . . ? C25 C24 C32 C31 0.8(4) . . . . ? C23 C24 C32 C31 -178.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.747 _refine_diff_density_min -0.263 _refine_diff_density_rms 0.072 #===END data_(1b) _database_code_depnum_ccdc_archive 'CCDC 665247' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C30 H24 Ga N4 O2, F6 P' _chemical_formula_sum 'C30 H24 F6 Ga N4 O2 P' _chemical_formula_weight 687.22 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' F F 0.0171 0.0103 '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 Orthorhombic _symmetry_space_group_name_H-M ' Pnna ' _symmetry_space_group_name_Hall '-P 2a 2bc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 16.2510(14) _cell_length_b 28.641(2) _cell_length_c 12.4848(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5811.0(9) _cell_formula_units_Z 8 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 6720 _cell_measurement_theta_min 1.42 _cell_measurement_theta_max 24.36 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2784 _exptl_absorpt_coefficient_mu 1.077 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 90026 _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 24.36 _reflns_number_total 4751 _reflns_number_gt 3627 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1208P)^2^+6.7153P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _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 4751 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0751 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1930 _refine_ls_wR_factor_gt 0.1657 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 Ga Ga 0.56826(3) 0.107418(16) 0.15567(4) 0.0412(2) Uani 1 1 d . . . P1 P 0.03355(16) 0.2500 0.2500 0.0748(6) Uani 1 2 d S . . P2 P 0.2500 0.0000 0.43931(19) 0.0759(6) Uani 1 2 d S . . F1 F 0.0278(6) 0.2901(2) 0.1665(5) 0.173(3) Uani 1 1 d . . . F2 F -0.0347(4) 0.22309(19) 0.1841(5) 0.1366(18) Uani 1 1 d . . . F3 F 0.0968(4) 0.2216(3) 0.1897(8) 0.216(4) Uani 1 1 d . . . F4 F 0.2602(7) 0.0407(4) 0.3677(8) 0.293(6) Uani 1 1 d . . . F5 F 0.3416(4) -0.0094(3) 0.4345(10) 0.261(5) Uani 1 1 d . . . F6 F 0.2640(5) 0.0378(3) 0.5213(7) 0.224(4) Uani 1 1 d . . . O1 O 0.6795(2) 0.12732(13) 0.1516(3) 0.0588(9) Uani 1 1 d . . . O2 O 0.4568(2) 0.08856(12) 0.1627(3) 0.0518(8) Uani 1 1 d . . . N1 N 0.5857(3) 0.11533(14) 0.3246(3) 0.0520(10) Uani 1 1 d . . . N2 N 0.5150(3) 0.17497(13) 0.1302(3) 0.0490(9) Uani 1 1 d . . . N3 N 0.5692(2) 0.09162(13) -0.0088(3) 0.0457(9) Uani 1 1 d . . . N4 N 0.6051(3) 0.03662(13) 0.1554(3) 0.0496(10) Uani 1 1 d . . . C1 C 0.7091(3) 0.14134(17) 0.2466(5) 0.0630(14) Uani 1 1 d . . . C2 C 0.7854(4) 0.1620(2) 0.2570(7) 0.088(2) Uani 1 1 d . . . H2 H 0.8178 0.1681 0.1972 0.105 Uiso 1 1 calc R . . C3 C 0.8136(5) 0.1740(3) 0.3634(9) 0.110(3) Uani 1 1 d . . . H3 H 0.8654 0.1874 0.3711 0.132 Uiso 1 1 calc R . . C4 C 0.7685(6) 0.1666(3) 0.4509(8) 0.110(3) Uani 1 1 d . . . H4 H 0.7898 0.1746 0.5175 0.132 Uiso 1 1 calc R . . C5 C 0.6902(4) 0.1470(2) 0.4450(5) 0.0765(18) Uani 1 1 d . . . C6 C 0.6607(3) 0.13447(16) 0.3389(4) 0.0550(13) Uani 1 1 d . . . C7 C 0.5367(4) 0.1071(2) 0.4109(4) 0.0668(15) Uani 1 1 d . . . C8 C 0.5628(5) 0.1197(3) 0.5121(5) 0.084(2) Uani 1 1 d . . . H8 H 0.5284 0.1145 0.5705 0.101 Uiso 1 1 calc R . . C9 C 0.6356(6) 0.1390(2) 0.5276(5) 0.087(2) Uani 1 1 d . . . H9 H 0.6506 0.1475 0.5968 0.105 Uiso 1 1 calc R . . C10 C 0.4558(5) 0.0840(4) 0.3988(6) 0.116(3) Uani 1 1 d . . . H10A H 0.4554 0.0554 0.4390 0.174 Uiso 1 1 calc R . . H10B H 0.4462 0.0772 0.3245 0.174 Uiso 1 1 calc R . . H10C H 0.4133 0.1043 0.4249 0.174 Uiso 1 1 calc R . . C11 C 0.4025(3) 0.1243(2) 0.1603(4) 0.0569(13) Uani 1 1 d . . . C12 C 0.3197(4) 0.1174(3) 0.1761(5) 0.0834(19) Uani 1 1 d . . . H12 H 0.2991 0.0878 0.1903 0.100 Uiso 1 1 calc R . . C13 C 0.2658(4) 0.1569(4) 0.1700(6) 0.101(3) Uani 1 1 d . . . H13 H 0.2095 0.1524 0.1791 0.121 Uiso 1 1 calc R . . C14 C 0.2941(5) 0.2002(3) 0.1517(6) 0.102(3) Uani 1 1 d . . . H14 H 0.2574 0.2251 0.1497 0.122 Uiso 1 1 calc R . . C15 C 0.3772(4) 0.2083(2) 0.1356(5) 0.0769(18) Uani 1 1 d . . . C16 C 0.4322(3) 0.1699(2) 0.1423(4) 0.0543(13) Uani 1 1 d . . . C17 C 0.5473(4) 0.21763(17) 0.1091(4) 0.0615(14) Uani 1 1 d . . . C18 C 0.4948(5) 0.2566(2) 0.1022(5) 0.086(2) Uani 1 1 d . . . H18 H 0.5172 0.2859 0.0888 0.103 Uiso 1 1 calc R . . C19 C 0.4140(5) 0.2523(3) 0.1144(6) 0.091(2) Uani 1 1 d . . . H19 H 0.3808 0.2787 0.1090 0.110 Uiso 1 1 calc R . . C20 C 0.6365(5) 0.2243(2) 0.0914(6) 0.095(2) Uani 1 1 d . . . H20A H 0.6455 0.2361 0.0204 0.142 Uiso 1 1 calc R . . H20B H 0.6643 0.1949 0.0994 0.142 Uiso 1 1 calc R . . H20C H 0.6576 0.2461 0.1429 0.142 Uiso 1 1 calc R . . C21 C 0.5459(4) 0.12109(19) -0.0873(4) 0.0606(13) Uani 1 1 d . . . H21 H 0.5318 0.1516 -0.0698 0.073 Uiso 1 1 calc R . . C22 C 0.5425(5) 0.1073(2) -0.1915(5) 0.0747(17) Uani 1 1 d . . . H22 H 0.5260 0.1280 -0.2446 0.090 Uiso 1 1 calc R . . C23 C 0.5638(4) 0.0624(2) -0.2168(5) 0.083(2) Uani 1 1 d . . . H23 H 0.5629 0.0529 -0.2880 0.100 Uiso 1 1 calc R . . C24 C 0.5861(4) 0.0318(2) -0.1405(4) 0.0675(15) Uani 1 1 d . . . H24 H 0.5996 0.0012 -0.1581 0.081 Uiso 1 1 calc R . . C25 C 0.5886(3) 0.04703(16) -0.0331(4) 0.0508(11) Uani 1 1 d . . . C26 C 0.6115(3) 0.01727(15) 0.0569(4) 0.0478(11) Uani 1 1 d . . . C27 C 0.6387(4) -0.02819(18) 0.0444(5) 0.0695(15) Uani 1 1 d . . . H27 H 0.6417 -0.0416 -0.0234 0.083 Uiso 1 1 calc R . . C28 C 0.6615(4) -0.0532(2) 0.1336(6) 0.084(2) Uani 1 1 d . . . H28 H 0.6814 -0.0835 0.1265 0.101 Uiso 1 1 calc R . . C29 C 0.6547(4) -0.03331(19) 0.2337(6) 0.0805(19) Uani 1 1 d . . . H29 H 0.6689 -0.0500 0.2948 0.097 Uiso 1 1 calc R . . C30 C 0.6263(3) 0.01213(17) 0.2414(5) 0.0626(14) Uani 1 1 d . . . H30 H 0.6219 0.0259 0.3086 0.075 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 Ga 0.0457(3) 0.0352(3) 0.0426(3) -0.00436(19) 0.0015(2) -0.00204(19) P1 0.0862(15) 0.0583(13) 0.0799(15) -0.0098(11) 0.000 0.000 P2 0.0896(17) 0.0714(14) 0.0667(14) 0.000 0.000 -0.0154(12) F1 0.293(9) 0.098(4) 0.129(5) 0.024(3) 0.036(5) -0.027(5) F2 0.149(4) 0.124(4) 0.136(4) -0.033(3) -0.037(3) -0.018(3) F3 0.109(4) 0.166(6) 0.374(11) -0.102(6) 0.085(5) 0.012(4) F4 0.290(11) 0.332(12) 0.256(10) 0.216(9) -0.042(8) -0.117(10) F5 0.115(5) 0.150(6) 0.518(17) -0.082(8) 0.086(7) -0.022(4) F6 0.240(8) 0.181(6) 0.251(9) -0.114(6) -0.073(7) 0.042(6) O1 0.0487(19) 0.051(2) 0.077(2) -0.0147(17) 0.0120(17) -0.0040(16) O2 0.0511(18) 0.0465(19) 0.058(2) -0.0066(15) 0.0047(14) -0.0049(16) N1 0.062(3) 0.041(2) 0.053(2) -0.0064(18) -0.0057(19) -0.0001(19) N2 0.065(3) 0.042(2) 0.040(2) -0.0047(16) 0.0022(18) 0.0056(19) N3 0.056(2) 0.0377(19) 0.044(2) -0.0092(17) 0.0066(17) -0.0031(16) N4 0.052(2) 0.040(2) 0.057(2) -0.0055(18) -0.0110(18) 0.0026(18) C1 0.049(3) 0.043(3) 0.097(4) -0.022(3) -0.020(3) 0.000(2) C2 0.059(3) 0.070(4) 0.134(6) -0.026(4) 0.005(4) -0.009(3) C3 0.060(4) 0.105(6) 0.166(9) -0.053(6) -0.035(5) -0.016(4) C4 0.098(6) 0.114(6) 0.118(7) -0.038(5) -0.049(5) -0.002(5) C5 0.087(4) 0.056(3) 0.087(4) -0.019(3) -0.034(4) 0.004(3) C6 0.064(3) 0.036(3) 0.065(3) -0.012(2) -0.007(3) 0.009(2) C7 0.093(4) 0.067(4) 0.041(3) 0.002(2) 0.002(3) 0.002(3) C8 0.118(6) 0.085(4) 0.048(3) 0.000(3) -0.006(3) 0.000(4) C9 0.134(6) 0.076(4) 0.051(3) -0.007(3) -0.019(4) 0.016(4) C10 0.117(6) 0.167(8) 0.063(4) 0.003(5) 0.026(4) -0.055(6) C11 0.048(3) 0.074(4) 0.049(3) -0.018(2) -0.003(2) 0.004(3) C12 0.053(3) 0.111(5) 0.086(4) -0.027(4) 0.003(3) -0.004(3) C13 0.051(4) 0.147(8) 0.105(6) -0.040(5) -0.006(3) 0.022(5) C14 0.069(5) 0.113(7) 0.123(7) -0.018(5) -0.017(4) 0.041(5) C15 0.082(4) 0.083(5) 0.066(4) -0.008(3) -0.008(3) 0.031(3) C16 0.062(3) 0.058(3) 0.043(3) -0.008(2) -0.005(2) 0.011(2) C17 0.097(4) 0.040(3) 0.048(3) 0.000(2) 0.004(3) 0.007(3) C18 0.139(7) 0.048(3) 0.070(4) 0.007(3) 0.010(4) 0.017(4) C19 0.120(6) 0.068(5) 0.087(5) 0.011(4) -0.011(5) 0.035(4) C20 0.116(6) 0.053(4) 0.116(6) 0.008(4) 0.019(5) -0.022(3) C21 0.090(4) 0.047(3) 0.044(3) 0.000(2) 0.004(3) -0.001(3) C22 0.118(5) 0.061(4) 0.045(3) 0.002(3) 0.006(3) -0.003(3) C23 0.136(6) 0.066(4) 0.047(3) -0.013(3) 0.013(3) 0.001(4) C24 0.092(4) 0.052(3) 0.058(3) -0.019(3) 0.001(3) 0.005(3) C25 0.053(3) 0.044(3) 0.056(3) -0.014(2) 0.003(2) -0.003(2) C26 0.045(2) 0.042(2) 0.057(3) -0.012(2) -0.006(2) 0.002(2) C27 0.074(3) 0.052(3) 0.083(4) -0.018(3) -0.016(3) 0.016(3) C28 0.095(5) 0.049(3) 0.109(5) -0.012(3) -0.032(4) 0.022(3) C29 0.098(4) 0.050(3) 0.094(5) 0.003(3) -0.047(4) 0.010(3) C30 0.071(3) 0.050(3) 0.067(3) 0.000(3) -0.021(3) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga O2 1.893(3) . ? Ga O1 1.896(3) . ? Ga N3 2.102(4) . ? Ga N4 2.114(4) . ? Ga N1 2.140(4) . ? Ga N2 2.143(4) . ? P1 F3 1.511(6) 4 ? P1 F3 1.511(5) . ? P1 F1 1.553(5) . ? P1 F1 1.553(5) 4 ? P1 F2 1.582(5) . ? P1 F2 1.582(5) 4 ? P2 F4 1.478(7) . ? P2 F4 1.478(7) 2 ? P2 F6 1.507(6) . ? P2 F6 1.507(6) 2 ? P2 F5 1.514(7) . ? P2 F5 1.514(7) 2 ? O1 C1 1.341(6) . ? O2 C11 1.351(7) . ? N1 C6 1.348(7) . ? N1 C7 1.361(7) . ? N2 C17 1.356(6) . ? N2 C16 1.361(6) . ? N3 C21 1.347(7) . ? N3 C25 1.350(6) . ? N4 C30 1.327(6) . ? N4 C26 1.353(6) . ? C1 C2 1.382(7) . ? C1 C6 1.408(8) . ? C2 C3 1.447(11) . ? C3 C4 1.333(11) . ? C4 C5 1.391(10) . ? C5 C9 1.381(10) . ? C5 C6 1.454(7) . ? C7 C8 1.382(9) . ? C7 C10 1.479(10) . ? C8 C9 1.320(10) . ? C11 C12 1.374(8) . ? C11 C16 1.412(8) . ? C12 C13 1.432(10) . ? C13 C14 1.343(12) . ? C14 C15 1.385(11) . ? C15 C16 1.419(8) . ? C15 C19 1.420(10) . ? C17 C18 1.407(8) . ? C17 C20 1.478(9) . ? C18 C19 1.328(10) . ? C21 C22 1.361(8) . ? C22 C23 1.369(8) . ? C23 C24 1.344(8) . ? C24 C25 1.410(7) . ? C25 C26 1.459(7) . ? C26 C27 1.384(7) . ? C27 C28 1.376(8) . ? C28 C29 1.378(9) . ? C29 C30 1.384(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ga O1 178.55(14) . . ? O2 Ga N3 89.48(14) . . ? O1 Ga N3 91.82(14) . . ? O2 Ga N4 89.86(15) . . ? O1 Ga N4 91.05(16) . . ? N3 Ga N4 77.89(15) . . ? O2 Ga N1 96.39(16) . . ? O1 Ga N1 82.43(16) . . ? N3 Ga N1 169.81(16) . . ? N4 Ga N1 93.74(15) . . ? O2 Ga N2 82.98(15) . . ? O1 Ga N2 96.30(16) . . ? N3 Ga N2 92.98(14) . . ? N4 Ga N2 168.49(15) . . ? N1 Ga N2 95.99(14) . . ? F3 P1 F3 94.3(6) 4 . ? F3 P1 F1 88.7(5) 4 . ? F3 P1 F1 96.0(5) . . ? F3 P1 F1 96.0(5) 4 4 ? F3 P1 F1 88.7(5) . 4 ? F1 P1 F1 173.1(7) . 4 ? F3 P1 F2 176.6(4) 4 . ? F3 P1 F2 87.5(4) . . ? F1 P1 F2 88.2(4) . . ? F1 P1 F2 86.9(4) 4 . ? F3 P1 F2 87.5(4) 4 4 ? F3 P1 F2 176.6(4) . 4 ? F1 P1 F2 86.9(4) . 4 ? F1 P1 F2 88.2(4) 4 4 ? F2 P1 F2 90.9(5) . 4 ? F4 P2 F4 105.5(10) . 2 ? F4 P2 F6 80.1(6) . . ? F4 P2 F6 173.7(7) 2 . ? F4 P2 F6 173.7(7) . 2 ? F4 P2 F6 80.1(6) 2 2 ? F6 P2 F6 94.3(8) . 2 ? F4 P2 F5 90.3(6) . . ? F4 P2 F5 86.9(6) 2 . ? F6 P2 F5 90.4(5) . . ? F6 P2 F5 92.7(5) 2 . ? F4 P2 F5 86.9(6) . 2 ? F4 P2 F5 90.3(6) 2 2 ? F6 P2 F5 92.7(5) . 2 ? F6 P2 F5 90.4(5) 2 2 ? F5 P2 F5 175.5(10) . 2 ? C1 O1 Ga 114.1(3) . . ? C11 O2 Ga 114.1(4) . . ? C6 N1 C7 119.7(5) . . ? C6 N1 Ga 107.1(3) . . ? C7 N1 Ga 133.2(4) . . ? C17 N2 C16 120.0(4) . . ? C17 N2 Ga 133.3(4) . . ? C16 N2 Ga 106.7(3) . . ? C21 N3 C25 119.6(4) . . ? C21 N3 Ga 125.0(3) . . ? C25 N3 Ga 115.2(3) . . ? C30 N4 C26 119.9(4) . . ? C30 N4 Ga 125.4(3) . . ? C26 N4 Ga 114.6(3) . . ? O1 C1 C2 122.3(6) . . ? O1 C1 C6 118.8(4) . . ? C2 C1 C6 118.9(6) . . ? C1 C2 C3 118.2(7) . . ? C4 C3 C2 122.7(7) . . ? C3 C4 C5 121.6(7) . . ? C9 C5 C4 127.9(7) . . ? C9 C5 C6 115.3(6) . . ? C4 C5 C6 116.7(7) . . ? N1 C6 C1 116.9(4) . . ? N1 C6 C5 121.3(5) . . ? C1 C6 C5 121.8(5) . . ? N1 C7 C8 119.9(6) . . ? N1 C7 C10 121.2(5) . . ? C8 C7 C10 118.9(6) . . ? C9 C8 C7 121.3(7) . . ? C8 C9 C5 122.4(6) . . ? O2 C11 C12 121.9(6) . . ? O2 C11 C16 118.8(5) . . ? C12 C11 C16 119.3(6) . . ? C11 C12 C13 118.7(7) . . ? C14 C13 C12 121.9(7) . . ? C13 C14 C15 120.9(7) . . ? C14 C15 C16 118.4(7) . . ? C14 C15 C19 125.9(7) . . ? C16 C15 C19 115.7(6) . . ? N2 C16 C11 117.0(5) . . ? N2 C16 C15 122.3(6) . . ? C11 C16 C15 120.8(5) . . ? N2 C17 C18 119.4(6) . . ? N2 C17 C20 121.7(5) . . ? C18 C17 C20 118.9(6) . . ? C19 C18 C17 121.3(6) . . ? C18 C19 C15 121.3(6) . . ? N3 C21 C22 121.6(5) . . ? C21 C22 C23 118.9(6) . . ? C24 C23 C22 121.1(6) . . ? C23 C24 C25 118.7(5) . . ? N3 C25 C24 120.0(5) . . ? N3 C25 C26 116.0(4) . . ? C24 C25 C26 124.0(4) . . ? N4 C26 C27 120.8(5) . . ? N4 C26 C25 116.2(4) . . ? C27 C26 C25 123.0(5) . . ? C28 C27 C26 119.0(5) . . ? C27 C28 C29 119.8(5) . . ? C28 C29 C30 118.6(5) . . ? N4 C30 C29 121.8(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Ga O1 C1 27(7) . . . . ? N3 Ga O1 C1 -179.2(3) . . . . ? N4 Ga O1 C1 -101.3(3) . . . . ? N1 Ga O1 C1 -7.7(3) . . . . ? N2 Ga O1 C1 87.6(3) . . . . ? O1 Ga O2 C11 54(7) . . . . ? N3 Ga O2 C11 -99.4(3) . . . . ? N4 Ga O2 C11 -177.3(3) . . . . ? N1 Ga O2 C11 88.9(3) . . . . ? N2 Ga O2 C11 -6.4(3) . . . . ? O2 Ga N1 C6 -172.8(3) . . . . ? O1 Ga N1 C6 6.4(3) . . . . ? N3 Ga N1 C6 62.4(9) . . . . ? N4 Ga N1 C6 96.9(3) . . . . ? N2 Ga N1 C6 -89.2(3) . . . . ? O2 Ga N1 C7 3.8(5) . . . . ? O1 Ga N1 C7 -177.1(5) . . . . ? N3 Ga N1 C7 -121.1(9) . . . . ? N4 Ga N1 C7 -86.5(5) . . . . ? N2 Ga N1 C7 87.3(5) . . . . ? O2 Ga N2 C17 -176.4(5) . . . . ? O1 Ga N2 C17 4.8(5) . . . . ? N3 Ga N2 C17 -87.3(4) . . . . ? N4 Ga N2 C17 -124.5(8) . . . . ? N1 Ga N2 C17 87.8(5) . . . . ? O2 Ga N2 C16 5.6(3) . . . . ? O1 Ga N2 C16 -173.2(3) . . . . ? N3 Ga N2 C16 94.7(3) . . . . ? N4 Ga N2 C16 57.5(9) . . . . ? N1 Ga N2 C16 -90.2(3) . . . . ? O2 Ga N3 C21 86.5(4) . . . . ? O1 Ga N3 C21 -92.9(4) . . . . ? N4 Ga N3 C21 176.4(4) . . . . ? N1 Ga N3 C21 -148.2(8) . . . . ? N2 Ga N3 C21 3.5(4) . . . . ? O2 Ga N3 C25 -88.0(3) . . . . ? O1 Ga N3 C25 92.7(3) . . . . ? N4 Ga N3 C25 2.0(3) . . . . ? N1 Ga N3 C25 37.3(10) . . . . ? N2 Ga N3 C25 -170.9(3) . . . . ? O2 Ga N4 C30 -94.3(4) . . . . ? O1 Ga N4 C30 84.6(4) . . . . ? N3 Ga N4 C30 176.2(4) . . . . ? N1 Ga N4 C30 2.1(4) . . . . ? N2 Ga N4 C30 -145.7(7) . . . . ? O2 Ga N4 C26 90.0(3) . . . . ? O1 Ga N4 C26 -91.1(3) . . . . ? N3 Ga N4 C26 0.5(3) . . . . ? N1 Ga N4 C26 -173.6(3) . . . . ? N2 Ga N4 C26 38.6(10) . . . . ? Ga O1 C1 C2 -172.3(4) . . . . ? Ga O1 C1 C6 8.0(6) . . . . ? O1 C1 C2 C3 -177.2(6) . . . . ? C6 C1 C2 C3 2.5(9) . . . . ? C1 C2 C3 C4 -1.2(12) . . . . ? C2 C3 C4 C5 -0.6(14) . . . . ? C3 C4 C5 C9 -177.3(8) . . . . ? C3 C4 C5 C6 0.9(11) . . . . ? C7 N1 C6 C1 178.9(5) . . . . ? Ga N1 C6 C1 -4.0(5) . . . . ? C7 N1 C6 C5 -0.6(7) . . . . ? Ga N1 C6 C5 176.5(4) . . . . ? O1 C1 C6 N1 -2.1(7) . . . . ? C2 C1 C6 N1 178.2(5) . . . . ? O1 C1 C6 C5 177.4(4) . . . . ? C2 C1 C6 C5 -2.3(8) . . . . ? C9 C5 C6 N1 -1.5(8) . . . . ? C4 C5 C6 N1 -180.0(6) . . . . ? C9 C5 C6 C1 179.0(5) . . . . ? C4 C5 C6 C1 0.5(8) . . . . ? C6 N1 C7 C8 2.1(8) . . . . ? Ga N1 C7 C8 -174.1(5) . . . . ? C6 N1 C7 C10 -176.9(6) . . . . ? Ga N1 C7 C10 6.9(9) . . . . ? N1 C7 C8 C9 -1.3(10) . . . . ? C10 C7 C8 C9 177.7(7) . . . . ? C7 C8 C9 C5 -1.0(11) . . . . ? C4 C5 C9 C8 -179.4(7) . . . . ? C6 C5 C9 C8 2.4(9) . . . . ? Ga O2 C11 C12 -173.0(4) . . . . ? Ga O2 C11 C16 6.3(5) . . . . ? O2 C11 C12 C13 -178.7(5) . . . . ? C16 C11 C12 C13 2.1(8) . . . . ? C11 C12 C13 C14 -1.4(11) . . . . ? C12 C13 C14 C15 1.3(12) . . . . ? C13 C14 C15 C16 -1.9(11) . . . . ? C13 C14 C15 C19 179.3(7) . . . . ? C17 N2 C16 C11 177.8(4) . . . . ? Ga N2 C16 C11 -3.8(5) . . . . ? C17 N2 C16 C15 -1.2(7) . . . . ? Ga N2 C16 C15 177.2(4) . . . . ? O2 C11 C16 N2 -1.1(6) . . . . ? C12 C11 C16 N2 178.2(5) . . . . ? O2 C11 C16 C15 177.9(4) . . . . ? C12 C11 C16 C15 -2.8(7) . . . . ? C14 C15 C16 N2 -178.4(5) . . . . ? C19 C15 C16 N2 0.5(8) . . . . ? C14 C15 C16 C11 2.7(8) . . . . ? C19 C15 C16 C11 -178.4(5) . . . . ? C16 N2 C17 C18 1.3(7) . . . . ? Ga N2 C17 C18 -176.5(4) . . . . ? C16 N2 C17 C20 -177.7(5) . . . . ? Ga N2 C17 C20 4.5(8) . . . . ? N2 C17 C18 C19 -1.0(10) . . . . ? C20 C17 C18 C19 178.1(7) . . . . ? C17 C18 C19 C15 0.4(11) . . . . ? C14 C15 C19 C18 178.7(7) . . . . ? C16 C15 C19 C18 -0.2(10) . . . . ? C25 N3 C21 C22 -0.9(8) . . . . ? Ga N3 C21 C22 -175.2(4) . . . . ? N3 C21 C22 C23 -0.4(10) . . . . ? C21 C22 C23 C24 1.5(11) . . . . ? C22 C23 C24 C25 -1.1(10) . . . . ? C21 N3 C25 C24 1.3(7) . . . . ? Ga N3 C25 C24 176.1(4) . . . . ? C21 N3 C25 C26 -178.8(4) . . . . ? Ga N3 C25 C26 -4.0(5) . . . . ? C23 C24 C25 N3 -0.3(9) . . . . ? C23 C24 C25 C26 179.8(5) . . . . ? C30 N4 C26 C27 1.0(7) . . . . ? Ga N4 C26 C27 176.9(4) . . . . ? C30 N4 C26 C25 -178.7(4) . . . . ? Ga N4 C26 C25 -2.7(5) . . . . ? N3 C25 C26 N4 4.5(6) . . . . ? C24 C25 C26 N4 -175.6(5) . . . . ? N3 C25 C26 C27 -175.1(5) . . . . ? C24 C25 C26 C27 4.8(8) . . . . ? N4 C26 C27 C28 -1.7(8) . . . . ? C25 C26 C27 C28 178.0(5) . . . . ? C26 C27 C28 C29 1.8(10) . . . . ? C27 C28 C29 C30 -1.2(10) . . . . ? C26 N4 C30 C29 -0.4(8) . . . . ? Ga N4 C30 C29 -175.9(4) . . . . ? C28 C29 C30 N4 0.5(9) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.36 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.835 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.100 #===END data_(2b) _database_code_depnum_ccdc_archive 'CCDC 665248' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C32 H24 Ga N4 O2, F6 P' _chemical_formula_sum 'C32 H24 F6 Ga N4 O2 P' _chemical_formula_weight 711.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 20.2459(8) _cell_length_b 14.9905(7) _cell_length_c 10.4419(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.551(2) _cell_angle_gamma 90.00 _cell_volume 2986.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 8454 _cell_measurement_theta_min 1.73 _cell_measurement_theta_max 26.37 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 1.051 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24446 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0216 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3028 _reflns_number_gt 2393 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1361P)^2^+1.2474P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _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 3028 _refine_ls_number_parameters 211 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0708 _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.1848 _refine_ls_wR_factor_gt 0.1709 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.050 _refine_ls_shift/su_mean 0.006 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 Ga Ga 0.5000 0.76962(3) 0.7500 0.0464(2) Uani 1 2 d S . . N1 N 0.57044(15) 0.67246(18) 0.7175(3) 0.0539(7) Uani 1 1 d . . . N3 N 0.45182(13) 0.87955(18) 0.8129(3) 0.0473(6) Uani 1 1 d . . . O1 O 0.56696(13) 0.77373(14) 0.9274(3) 0.0537(6) Uani 1 1 d . . . C1 C 0.62030(19) 0.7182(2) 0.9520(4) 0.0529(8) Uani 1 1 d . . . C2 C 0.6721(2) 0.7101(3) 1.0750(4) 0.0657(10) Uani 1 1 d . . . H2 H 0.6711 0.7465 1.1464 0.079 Uiso 1 1 calc R . . C3 C 0.7264(2) 0.6490(3) 1.0966(4) 0.0712(11) Uani 1 1 d . . . H3 H 0.7608 0.6457 1.1819 0.085 Uiso 1 1 calc R . . C4 C 0.7304(2) 0.5941(3) 0.9961(4) 0.0760(12) Uani 1 1 d . . . H4 H 0.7671 0.5536 1.0123 0.091 Uiso 1 1 calc R . . C5 C 0.6776(2) 0.5992(3) 0.8655(4) 0.0664(10) Uani 1 1 d . . . C6 C 0.62381(17) 0.6607(2) 0.8433(4) 0.0524(8) Uani 1 1 d . . . C7 C 0.5735(2) 0.6229(3) 0.6153(4) 0.0672(10) Uani 1 1 d . . . C8 C 0.6255(2) 0.5574(3) 0.6327(5) 0.0790(14) Uani 1 1 d . . . H8 H 0.6252 0.5224 0.5589 0.095 Uiso 1 1 calc R . . C9 C 0.6760(3) 0.5441(3) 0.7546(5) 0.0873(14) Uani 1 1 d . . . H9 H 0.7091 0.4993 0.7652 0.105 Uiso 1 1 calc R . . C10 C 0.5213(3) 0.6370(4) 0.4758(5) 0.0944(15) Uani 1 1 d . . . H10A H 0.4824 0.6711 0.4823 0.142 Uiso 1 1 calc R . . H10B H 0.5048 0.5802 0.4350 0.142 Uiso 1 1 calc R . . H10C H 0.5432 0.6686 0.4208 0.142 Uiso 1 1 calc R . . C11 C 0.47380(15) 0.9592(2) 0.7835(3) 0.0461(7) Uani 1 1 d . . . C12 C 0.44940(18) 1.0408(2) 0.8167(4) 0.0577(9) Uani 1 1 d . . . C13 C 0.3993(2) 1.0356(3) 0.8850(4) 0.0648(10) Uani 1 1 d . . . H13 H 0.3813 1.0875 0.9092 0.078 Uiso 1 1 calc R . . C14 C 0.3780(2) 0.9548(3) 0.9145(5) 0.0648(10) Uani 1 1 d . . . H14 H 0.3454 0.9513 0.9594 0.078 Uiso 1 1 calc R . . C15 C 0.40509(18) 0.8763(3) 0.8775(4) 0.0558(8) Uani 1 1 d . . . H15 H 0.3902 0.8212 0.8983 0.067 Uiso 1 1 calc R . . C16 C 0.4755(2) 1.1219(2) 0.7810(4) 0.0689(10) Uani 1 1 d . . . H16 H 0.4585 1.1760 0.8006 0.083 Uiso 1 1 calc R . . P1 P 0.7500 0.7500 0.5000 0.0717(5) Uani 1 2 d S . . F2 F 0.7168(2) 0.7368(3) 0.6154(4) 0.1306(14) Uani 1 1 d . . . F1 F 0.7290(3) 0.6557(3) 0.4410(6) 0.1756(19) Uani 1 1 d . . . F3 F 0.6795(3) 0.7882(5) 0.4083(5) 0.201(3) 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 Ga 0.0424(3) 0.0362(3) 0.0570(4) 0.000 0.0118(2) 0.000 N1 0.0567(16) 0.0380(14) 0.0702(18) -0.0024(13) 0.0255(14) 0.0017(12) N3 0.0387(13) 0.0403(14) 0.0597(16) 0.0007(12) 0.0121(12) 0.0015(11) O1 0.0511(14) 0.0439(14) 0.0582(14) -0.0063(10) 0.0081(11) 0.0086(10) C1 0.0461(18) 0.0466(19) 0.063(2) 0.0031(15) 0.0147(15) 0.0000(14) C2 0.060(2) 0.065(2) 0.068(2) 0.0039(19) 0.0160(18) 0.0026(19) C3 0.055(2) 0.083(3) 0.070(2) 0.012(2) 0.0120(18) 0.008(2) C4 0.058(2) 0.079(3) 0.089(3) 0.016(2) 0.022(2) 0.021(2) C5 0.058(2) 0.066(2) 0.081(2) 0.005(2) 0.0318(19) 0.0089(18) C6 0.0493(18) 0.0411(17) 0.068(2) 0.0048(15) 0.0211(15) 0.0022(14) C7 0.071(2) 0.058(2) 0.076(2) -0.0064(19) 0.030(2) -0.0031(19) C8 0.083(3) 0.071(3) 0.092(3) -0.022(2) 0.041(3) 0.009(2) C9 0.081(3) 0.081(3) 0.102(3) -0.005(3) 0.034(3) 0.027(2) C10 0.091(3) 0.103(4) 0.076(3) -0.017(3) 0.010(2) 0.012(3) C11 0.0372(15) 0.0384(16) 0.0548(17) -0.0018(13) 0.0049(12) 0.0026(12) C12 0.0476(18) 0.0450(18) 0.071(2) -0.0060(16) 0.0069(16) 0.0072(15) C13 0.057(2) 0.056(2) 0.078(2) -0.0126(19) 0.0173(17) 0.0139(18) C14 0.051(2) 0.062(2) 0.084(2) -0.009(2) 0.0257(18) 0.0079(17) C15 0.0448(18) 0.053(2) 0.069(2) 0.0003(16) 0.0186(15) 0.0041(15) C16 0.070(2) 0.0383(18) 0.089(3) -0.0034(18) 0.015(2) 0.0045(16) P1 0.0611(10) 0.0870(11) 0.0704(10) -0.0140(8) 0.0267(8) 0.0087(8) F2 0.128(3) 0.172(4) 0.113(3) -0.005(2) 0.068(3) 0.004(2) F1 0.235(5) 0.121(3) 0.196(4) -0.075(3) 0.106(4) -0.051(3) F3 0.150(4) 0.300(8) 0.120(3) -0.041(4) 0.002(3) 0.123(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 Ga O1 1.895(2) 2_656 ? Ga O1 1.895(2) . ? Ga N3 2.128(3) 2_656 ? Ga N3 2.128(3) . ? Ga N1 2.143(3) 2_656 ? Ga N1 2.143(3) . ? N1 C7 1.318(5) . ? N1 C6 1.405(4) . ? N3 C15 1.334(4) . ? N3 C11 1.346(4) . ? O1 C1 1.318(4) . ? C1 C2 1.365(5) . ? C1 C6 1.446(5) . ? C2 C3 1.390(6) . ? C3 C4 1.358(6) . ? C4 C5 1.426(6) . ? C5 C6 1.386(5) . ? C5 C9 1.414(6) . ? C7 C8 1.407(6) . ? C7 C10 1.502(6) . ? C8 C9 1.354(6) . ? C11 C12 1.405(5) . ? C11 C11 1.453(6) 2_656 ? C12 C16 1.423(5) . ? C12 C13 1.423(6) . ? C13 C14 1.356(6) . ? C14 C15 1.405(5) . ? C16 C16 1.354(8) 2_656 ? P1 F3 1.538(4) 7_666 ? P1 F3 1.538(4) . ? P1 F1 1.544(4) . ? P1 F1 1.544(4) 7_666 ? P1 F2 1.576(4) 7_666 ? P1 F2 1.576(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ga O1 176.28(13) 2_656 . ? O1 Ga N3 85.69(10) 2_656 2_656 ? O1 Ga N3 91.42(10) . 2_656 ? O1 Ga N3 91.42(10) 2_656 . ? O1 Ga N3 85.69(10) . . ? N3 Ga N3 78.49(14) 2_656 . ? O1 Ga N1 83.14(11) 2_656 2_656 ? O1 Ga N1 99.42(11) . 2_656 ? N3 Ga N1 166.70(11) 2_656 2_656 ? N3 Ga N1 94.55(11) . 2_656 ? O1 Ga N1 99.42(11) 2_656 . ? O1 Ga N1 83.14(11) . . ? N3 Ga N1 94.55(10) 2_656 . ? N3 Ga N1 166.70(11) . . ? N1 Ga N1 94.39(15) 2_656 . ? C7 N1 C6 117.1(3) . . ? C7 N1 Ga 136.5(3) . . ? C6 N1 Ga 106.3(2) . . ? C15 N3 C11 119.5(3) . . ? C15 N3 Ga 127.2(2) . . ? C11 N3 Ga 113.3(2) . . ? C1 O1 Ga 116.2(2) . . ? O1 C1 C2 124.1(4) . . ? O1 C1 C6 118.4(3) . . ? C2 C1 C6 117.4(3) . . ? C1 C2 C3 121.9(4) . . ? C4 C3 C2 121.5(4) . . ? C3 C4 C5 119.2(4) . . ? C6 C5 C9 116.8(4) . . ? C6 C5 C4 119.4(4) . . ? C9 C5 C4 123.8(4) . . ? C5 C6 N1 123.7(3) . . ? C5 C6 C1 120.5(3) . . ? N1 C6 C1 115.8(3) . . ? N1 C7 C8 121.7(4) . . ? N1 C7 C10 119.9(4) . . ? C8 C7 C10 118.5(4) . . ? C9 C8 C7 121.3(4) . . ? C8 C9 C5 119.2(4) . . ? N3 C11 C12 123.1(3) . . ? N3 C11 C11 117.41(17) . 2_656 ? C12 C11 C11 119.5(2) . 2_656 ? C11 C12 C16 119.1(3) . . ? C11 C12 C13 116.4(3) . . ? C16 C12 C13 124.5(3) . . ? C14 C13 C12 119.8(4) . . ? C13 C14 C15 120.2(4) . . ? N3 C15 C14 121.1(4) . . ? C16 C16 C12 121.4(2) 2_656 . ? F3 P1 F3 180.000(1) 7_666 . ? F3 P1 F1 89.0(3) 7_666 . ? F3 P1 F1 91.0(3) . . ? F3 P1 F1 91.0(3) 7_666 7_666 ? F3 P1 F1 89.0(3) . 7_666 ? F1 P1 F1 180.000(1) . 7_666 ? F3 P1 F2 88.7(3) 7_666 7_666 ? F3 P1 F2 91.3(3) . 7_666 ? F1 P1 F2 86.6(2) . 7_666 ? F1 P1 F2 93.4(2) 7_666 7_666 ? F3 P1 F2 91.3(3) 7_666 . ? F3 P1 F2 88.7(3) . . ? F1 P1 F2 93.4(2) . . ? F1 P1 F2 86.6(2) 7_666 . ? F2 P1 F2 180.000(2) 7_666 . ? 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 O1 Ga N1 C7 -1.8(4) 2_656 . . . ? O1 Ga N1 C7 -179.1(4) . . . . ? N3 Ga N1 C7 -88.2(4) 2_656 . . . ? N3 Ga N1 C7 -146.0(4) . . . . ? N1 Ga N1 C7 81.9(4) 2_656 . . . ? O1 Ga N1 C6 -179.1(2) 2_656 . . . ? O1 Ga N1 C6 3.6(2) . . . . ? N3 Ga N1 C6 94.5(2) 2_656 . . . ? N3 Ga N1 C6 36.7(5) . . . . ? N1 Ga N1 C6 -95.4(2) 2_656 . . . ? O1 Ga N3 C15 96.0(3) 2_656 . . . ? O1 Ga N3 C15 -86.3(3) . . . . ? N3 Ga N3 C15 -178.7(3) 2_656 . . . ? N1 Ga N3 C15 12.8(3) 2_656 . . . ? N1 Ga N3 C15 -119.3(5) . . . . ? O1 Ga N3 C11 -85.1(2) 2_656 . . . ? O1 Ga N3 C11 92.6(2) . . . . ? N3 Ga N3 C11 0.24(16) 2_656 . . . ? N1 Ga N3 C11 -168.3(2) 2_656 . . . ? N1 Ga N3 C11 59.6(5) . . . . ? O1 Ga O1 C1 -136.0(2) 2_656 . . . ? N3 Ga O1 C1 -96.9(2) 2_656 . . . ? N3 Ga O1 C1 -175.2(3) . . . . ? N1 Ga O1 C1 90.9(3) 2_656 . . . ? N1 Ga O1 C1 -2.5(2) . . . . ? Ga O1 C1 C2 -177.8(3) . . . . ? Ga O1 C1 C6 0.8(4) . . . . ? O1 C1 C2 C3 178.4(4) . . . . ? C6 C1 C2 C3 -0.2(6) . . . . ? C1 C2 C3 C4 -0.2(7) . . . . ? C2 C3 C4 C5 0.0(7) . . . . ? C3 C4 C5 C6 0.7(6) . . . . ? C3 C4 C5 C9 -178.8(5) . . . . ? C9 C5 C6 N1 -2.2(6) . . . . ? C4 C5 C6 N1 178.3(4) . . . . ? C9 C5 C6 C1 178.4(4) . . . . ? C4 C5 C6 C1 -1.1(6) . . . . ? C7 N1 C6 C5 -1.5(5) . . . . ? Ga N1 C6 C5 176.4(3) . . . . ? C7 N1 C6 C1 177.9(3) . . . . ? Ga N1 C6 C1 -4.2(3) . . . . ? O1 C1 C6 C5 -177.9(3) . . . . ? C2 C1 C6 C5 0.8(5) . . . . ? O1 C1 C6 N1 2.7(5) . . . . ? C2 C1 C6 N1 -178.6(3) . . . . ? C6 N1 C7 C8 3.6(6) . . . . ? Ga N1 C7 C8 -173.5(3) . . . . ? C6 N1 C7 C10 -175.4(4) . . . . ? Ga N1 C7 C10 7.6(6) . . . . ? N1 C7 C8 C9 -1.9(7) . . . . ? C10 C7 C8 C9 177.0(5) . . . . ? C7 C8 C9 C5 -2.0(7) . . . . ? C6 C5 C9 C8 3.8(7) . . . . ? C4 C5 C9 C8 -176.7(5) . . . . ? C15 N3 C11 C12 -0.5(5) . . . . ? Ga N3 C11 C12 -179.5(2) . . . . ? C15 N3 C11 C11 178.3(3) . . . 2_656 ? Ga N3 C11 C11 -0.7(4) . . . 2_656 ? N3 C11 C12 C16 -179.8(3) . . . . ? C11 C11 C12 C16 1.4(6) 2_656 . . . ? N3 C11 C12 C13 0.2(5) . . . . ? C11 C11 C12 C13 -178.6(4) 2_656 . . . ? C11 C12 C13 C14 0.1(5) . . . . ? C16 C12 C13 C14 -179.9(4) . . . . ? C12 C13 C14 C15 -0.2(6) . . . . ? C11 N3 C15 C14 0.4(5) . . . . ? Ga N3 C15 C14 179.3(3) . . . . ? C13 C14 C15 N3 -0.1(6) . . . . ? C11 C12 C16 C16 -1.7(7) . . . 2_656 ? C13 C12 C16 C16 178.3(5) . . . 2_656 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.139 _refine_diff_density_min -0.359 _refine_diff_density_rms 0.103