# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2008 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Claire Carmalt' _publ_contact_author_address ; Department of Chemistry University College London 20 Gordon Street LONDON WC1H 0AJ UNITED KINGDOM ; _publ_contact_author_email C.J.CARMALT@UCL.AC.UK _publ_section_title ; Synthesis and Structures of Gallium Alkoxides ; loop_ _publ_author_name 'Claire Carmalt' 'Sarah A. Barnett' 'Siama Basharat' 'Caroline E. Knapp' 'D. Tocher' # Attachment 'STR0410.cif' data_STR0410 _database_code_depnum_ccdc_archive 'CCDC 663201' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'C10 H24 Cl Ga N2 O2' _chemical_melting_point ? _chemical_formula_moiety 'C10 H24 Cl Ga N2 O2' _chemical_formula_sum 'C10 H24 Cl Ga N2 O2' _chemical_formula_weight 309.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7913(13) _cell_length_b 7.9556(13) _cell_length_c 12.052(2) _cell_angle_alpha 99.069(2) _cell_angle_beta 93.211(3) _cell_angle_gamma 102.462(2) _cell_volume 717.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3706 _cell_measurement_theta_min 2.663 _cell_measurement_theta_max 28.195 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 324 _exptl_absorpt_coefficient_mu 2.095 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6874 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS v2.10' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6168 _diffrn_reflns_av_R_equivalents 0.0156 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 28.29 _reflns_number_total 3265 _reflns_number_gt 2983 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0398P)^2^+0.1281P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier synthesis' _atom_sites_solution_hydrogens 'those on methyl found from delta-F; others geometrically placed' _refine_ls_hydrogen_treatment 'methyl groups treated as rigid rotor model; others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3265 _refine_ls_number_parameters 151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0298 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0662 _refine_ls_wR_factor_gt 0.0649 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.48404(2) 0.52413(2) 0.250541(14) 0.01879(7) Uani 1 1 d . . . Cl1 Cl 0.62781(6) 0.31186(6) 0.23313(4) 0.03017(11) Uani 1 1 d . . . C1 C 0.3107(3) 0.8410(3) 0.07643(18) 0.0330(4) Uani 1 1 d . . . H1A H 0.2193 0.7747 0.0170 0.049 Uiso 1 1 calc R . . H1B H 0.3667 0.9522 0.0548 0.049 Uiso 1 1 calc R . . H1C H 0.2569 0.8638 0.1472 0.049 Uiso 1 1 calc R . . O1 O 0.36986(16) 0.57728(16) 0.12765(10) 0.0239(3) Uani 1 1 d . . . C2 C 0.4488(2) 0.7359(2) 0.09241(15) 0.0247(4) Uani 1 1 d . . . H2A H 0.4983 0.7079 0.0187 0.030 Uiso 1 1 calc R . . C3 C 0.5989(2) 0.8415(2) 0.17971(16) 0.0254(4) Uani 1 1 d . . . H3A H 0.6765 0.9316 0.1457 0.030 Uiso 1 1 calc R . . H3B H 0.5498 0.9014 0.2447 0.030 Uiso 1 1 calc R . . N1 N 0.70187(19) 0.72242(19) 0.21842(12) 0.0223(3) Uani 1 1 d . . . C4 C 0.8227(3) 0.8099(3) 0.31976(16) 0.0306(4) Uani 1 1 d . . . H4A H 0.9110 0.9062 0.3006 0.046 Uiso 1 1 calc R . . H4B H 0.8820 0.7255 0.3472 0.046 Uiso 1 1 calc R . . H4C H 0.7551 0.8559 0.3788 0.046 Uiso 1 1 calc R . . C5 C 0.8070(2) 0.6612(3) 0.12790(16) 0.0291(4) Uani 1 1 d . . . H5A H 0.8848 0.7623 0.1057 0.044 Uiso 1 1 calc R . . H5B H 0.7273 0.5945 0.0625 0.044 Uiso 1 1 calc R . . H5C H 0.8784 0.5864 0.1557 0.044 Uiso 1 1 calc R . . C11 C 0.2684(3) 0.7942(3) 0.48261(17) 0.0317(4) Uani 1 1 d . . . H11A H 0.3618 0.8643 0.5396 0.048 Uiso 1 1 calc R . . H11B H 0.1561 0.7724 0.5166 0.048 Uiso 1 1 calc R . . H11C H 0.2579 0.8575 0.4200 0.048 Uiso 1 1 calc R . . O11 O 0.47745(16) 0.65105(16) 0.39101(10) 0.0237(3) Uani 1 1 d . . . C12 C 0.3143(2) 0.6206(2) 0.43855(15) 0.0242(4) Uani 1 1 d . . . H12A H 0.3247 0.5570 0.5029 0.029 Uiso 1 1 calc R . . C13 C 0.1693(2) 0.5082(2) 0.35017(16) 0.0252(4) Uani 1 1 d . . . H13A H 0.0651 0.4584 0.3878 0.030 Uiso 1 1 calc R . . H13B H 0.1326 0.5810 0.2980 0.030 Uiso 1 1 calc R . . N11 N 0.23705(19) 0.36502(19) 0.28608(12) 0.0225(3) Uani 1 1 d . . . C14 C 0.1146(2) 0.2770(3) 0.18530(16) 0.0294(4) Uani 1 1 d . . . H14A H 0.0002 0.2235 0.2090 0.044 Uiso 1 1 calc R . . H14B H 0.1637 0.1863 0.1422 0.044 Uiso 1 1 calc R . . H14C H 0.0988 0.3630 0.1379 0.044 Uiso 1 1 calc R . . C15 C 0.2589(3) 0.2352(2) 0.35861(16) 0.0278(4) Uani 1 1 d . . . H15A H 0.3454 0.2919 0.4230 0.042 Uiso 1 1 calc R . . H15B H 0.3003 0.1397 0.3147 0.042 Uiso 1 1 calc R . . H15C H 0.1453 0.1884 0.3860 0.042 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.01929(11) 0.01769(11) 0.01892(11) 0.00202(7) 0.00052(7) 0.00435(7) Cl1 0.0339(2) 0.0256(2) 0.0354(2) 0.00657(18) 0.00703(19) 0.01435(18) C1 0.0306(10) 0.0322(10) 0.0404(11) 0.0126(9) 0.0014(8) 0.0123(8) O1 0.0251(6) 0.0217(6) 0.0233(6) 0.0072(5) -0.0032(5) 0.0008(5) C2 0.0258(9) 0.0243(9) 0.0261(9) 0.0089(7) 0.0033(7) 0.0073(7) C3 0.0255(9) 0.0198(8) 0.0306(9) 0.0059(7) 0.0025(7) 0.0035(7) N1 0.0199(7) 0.0220(7) 0.0238(7) 0.0017(6) 0.0017(6) 0.0039(6) C4 0.0255(9) 0.0304(10) 0.0308(10) 0.0000(8) -0.0024(8) 0.0005(8) C5 0.0227(9) 0.0326(10) 0.0314(10) 0.0023(8) 0.0066(7) 0.0061(8) C11 0.0317(10) 0.0282(10) 0.0349(10) 0.0000(8) 0.0070(8) 0.0089(8) O11 0.0211(6) 0.0259(6) 0.0214(6) -0.0016(5) 0.0020(5) 0.0034(5) C12 0.0245(9) 0.0262(9) 0.0227(8) 0.0047(7) 0.0052(7) 0.0064(7) C13 0.0194(8) 0.0253(9) 0.0313(9) 0.0054(7) 0.0038(7) 0.0049(7) N11 0.0218(7) 0.0198(7) 0.0249(7) 0.0032(6) 0.0009(6) 0.0032(6) C14 0.0248(9) 0.0285(10) 0.0305(10) 0.0022(7) -0.0027(7) 0.0003(7) C15 0.0284(9) 0.0226(9) 0.0322(10) 0.0087(7) 0.0015(8) 0.0024(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 O1 1.8373(12) . y Ga1 O11 1.8389(12) . y Ga1 N1 2.1516(15) . y Ga1 N11 2.1681(15) . y Ga1 Cl1 2.2094(5) . y C1 C2 1.520(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? O1 C2 1.419(2) . ? C2 C3 1.530(3) . ? C2 H2A 1.0000 . ? C3 N1 1.478(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N1 C4 1.477(2) . ? N1 C5 1.484(2) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C11 C12 1.523(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? O11 C12 1.413(2) . ? C12 C13 1.529(3) . ? C12 H12A 1.0000 . ? C13 N11 1.483(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? N11 C14 1.480(2) . ? N11 C15 1.484(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? 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 Ga1 O11 118.91(6) . . y O1 Ga1 N1 84.28(6) . . y O11 Ga1 N1 90.34(6) . . y O1 Ga1 N11 89.82(6) . . y O11 Ga1 N11 84.18(5) . . y N1 Ga1 N11 168.80(6) . . y O1 Ga1 Cl1 121.55(4) . . y O11 Ga1 Cl1 119.54(4) . . y N1 Ga1 Cl1 95.45(4) . . y N11 Ga1 Cl1 95.76(4) . . y C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 O1 Ga1 116.28(11) . . ? O1 C2 C1 109.85(15) . . ? O1 C2 C3 109.96(14) . . ? C1 C2 C3 110.44(16) . . ? O1 C2 H2A 108.8 . . ? C1 C2 H2A 108.8 . . ? C3 C2 H2A 108.8 . . ? N1 C3 C2 109.21(14) . . ? N1 C3 H3A 109.8 . . ? C2 C3 H3A 109.8 . . ? N1 C3 H3B 109.8 . . ? C2 C3 H3B 109.8 . . ? H3A C3 H3B 108.3 . . ? C4 N1 C3 111.20(15) . . ? C4 N1 C5 108.88(14) . . ? C3 N1 C5 110.32(14) . . ? C4 N1 Ga1 113.94(12) . . ? C3 N1 Ga1 97.97(10) . . ? C5 N1 Ga1 114.16(11) . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C12 O11 Ga1 116.54(11) . . ? O11 C12 C11 109.80(15) . . ? O11 C12 C13 109.98(14) . . ? C11 C12 C13 110.38(16) . . ? O11 C12 H12A 108.9 . . ? C11 C12 H12A 108.9 . . ? C13 C12 H12A 108.9 . . ? N11 C13 C12 109.38(14) . . ? N11 C13 H13A 109.8 . . ? C12 C13 H13A 109.8 . . ? N11 C13 H13B 109.8 . . ? C12 C13 H13B 109.8 . . ? H13A C13 H13B 108.2 . . ? C14 N11 C13 110.50(15) . . ? C14 N11 C15 109.44(14) . . ? C13 N11 C15 110.27(14) . . ? C14 N11 Ga1 114.83(11) . . ? C13 N11 Ga1 97.26(10) . . ? C15 N11 Ga1 113.95(11) . . ? N11 C14 H14A 109.5 . . ? N11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N11 C15 H15A 109.5 . . ? N11 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N11 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? 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 O11 Ga1 O1 C2 71.99(13) . . . . ? N1 Ga1 O1 C2 -15.23(12) . . . . ? N11 Ga1 O1 C2 155.23(12) . . . . ? Cl1 Ga1 O1 C2 -108.12(11) . . . . ? Ga1 O1 C2 C1 -130.97(13) . . . . ? Ga1 O1 C2 C3 -9.22(18) . . . . ? O1 C2 C3 N1 42.05(19) . . . . ? C1 C2 C3 N1 163.45(15) . . . . ? C2 C3 N1 C4 -167.51(15) . . . . ? C2 C3 N1 C5 71.58(18) . . . . ? C2 C3 N1 Ga1 -47.93(15) . . . . ? O1 Ga1 N1 C4 152.74(13) . . . . ? O11 Ga1 N1 C4 33.72(13) . . . . ? N11 Ga1 N1 C4 94.2(3) . . . . ? Cl1 Ga1 N1 C4 -86.01(12) . . . . ? O1 Ga1 N1 C3 35.25(11) . . . . ? O11 Ga1 N1 C3 -83.77(11) . . . . ? N11 Ga1 N1 C3 -23.3(3) . . . . ? Cl1 Ga1 N1 C3 156.50(10) . . . . ? O1 Ga1 N1 C5 -81.30(13) . . . . ? O11 Ga1 N1 C5 159.67(12) . . . . ? N11 Ga1 N1 C5 -139.8(3) . . . . ? Cl1 Ga1 N1 C5 39.94(12) . . . . ? O1 Ga1 O11 C12 71.69(13) . . . . ? N1 Ga1 O11 C12 155.34(12) . . . . ? N11 Ga1 O11 C12 -14.87(12) . . . . ? Cl1 Ga1 O11 C12 -108.20(12) . . . . ? Ga1 O11 C12 C11 -131.55(13) . . . . ? Ga1 O11 C12 C13 -9.90(18) . . . . ? O11 C12 C13 N11 43.0(2) . . . . ? C11 C12 C13 N11 164.32(15) . . . . ? C12 C13 N11 C14 -168.17(15) . . . . ? C12 C13 N11 C15 70.71(18) . . . . ? C12 C13 N11 Ga1 -48.20(15) . . . . ? O1 Ga1 N11 C14 32.59(13) . . . . ? O11 Ga1 N11 C14 151.69(13) . . . . ? N1 Ga1 N11 C14 90.6(3) . . . . ? Cl1 Ga1 N11 C14 -89.11(12) . . . . ? O1 Ga1 N11 C13 -84.02(11) . . . . ? O11 Ga1 N11 C13 35.07(11) . . . . ? N1 Ga1 N11 C13 -26.0(3) . . . . ? Cl1 Ga1 N11 C13 154.28(10) . . . . ? O1 Ga1 N11 C15 159.96(12) . . . . ? O11 Ga1 N11 C15 -80.95(12) . . . . ? N1 Ga1 N11 C15 -142.0(3) . . . . ? Cl1 Ga1 N11 C15 38.25(12) . . . . ? _diffrn_measured_fraction_theta_max 0.914 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.728 _refine_diff_density_min -0.322 _refine_diff_density_rms 0.068 data_STR0492 _database_code_depnum_ccdc_archive 'CCDC 663202' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'C10 H22 Cl4 Ga2 O4' _chemical_melting_point ? _chemical_formula_moiety 'C10 H22 Cl4 Ga2 O4' _chemical_formula_sum 'C10 H22 Cl4 Ga2 O4' _chemical_formula_weight 487.52 _exptl_special_details ; The initial solution failed to give a refinement with an acceptable R-factor. On checking the data again it was evident, through the use of RLATT (Bruker 2000), that the crystal was twinned (non-merohedral). GEMINI (Bruker 2000) was used to index the data and showed that there were two, approximately equal components. The output p4p files for each component were read back into SMART and run through the BRAVAIS and L.S. routines. The data were combined to give a single p4p file (p4p2twin routine) and integrated simultaneously using SAINTPLUS (Bruker 2003). The twin law was found to be: -0.04032 -0.00085 0.96173 -0.04 0.00 0.96 0.00041 -0.99973 -0.00203 0.00 -1.00 0.00 1.03817 0.00045 0.03941 1.04 0.00 0.04 The dataset had 5280 data from component 1 only, 5271 data from component 2 only and 2690 data belonging to both. I/sigma for overlapping reflections was 28.4. The dataset was corrected for absorption using TWINABS (Bruker 2003) It was also used to produce an HKLF 4 file (non-overlapping reflections for component 1 only) for structure solution and initial refinement and an HKLF 5 file for final refinement of the structure. The twin ratio refined to 0.4392(15) (using the BASF instruction). ; 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' 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.4505(10) _cell_length_b 13.7024(17) _cell_length_c 8.6396(11) _cell_angle_alpha 90.00 _cell_angle_beta 113.648(2) _cell_angle_gamma 90.00 _cell_volume 916.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5467 _cell_measurement_theta_min 2.899 _cell_measurement_theta_max 28.146 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 3.529 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5638 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'TWINABS v1.02' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13241 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0218 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 28.24 _reflns_number_total 4429 _reflns_number_gt 2353 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0524P)^2^+0.3226P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier synthesis' _atom_sites_solution_hydrogens 'those on methyl found from delta-F; others geometrically placed' _refine_ls_hydrogen_treatment 'methyl groups treated as rigid rotor model; others riding ' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2584 _refine_ls_number_parameters 95 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0829 _refine_ls_wR_factor_gt 0.0818 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.14859(4) 0.070690(19) 0.53382(4) 0.01628(10) Uani 1 1 d . . . Cl1 Cl 0.18584(10) 0.12651(5) 0.31558(9) 0.02606(17) Uani 1 1 d . . . Cl2 Cl 0.38003(9) 0.04621(5) 0.75867(9) 0.02673(17) Uani 1 1 d . . . O1 O 0.1203(2) 0.21565(14) 0.6180(2) 0.0211(4) Uani 1 1 d . . . O2 O -0.0709(3) 0.06363(12) 0.5419(3) 0.0180(4) Uani 1 1 d . . . C1 C 0.2101(4) 0.2992(2) 0.5915(4) 0.0271(6) Uani 1 1 d . . . H1A H 0.1519 0.3215 0.4744 0.041 Uiso 1 1 calc R . . H1B H 0.3295 0.2812 0.6141 0.041 Uiso 1 1 calc R . . H1C H 0.2098 0.3519 0.6682 0.041 Uiso 1 1 calc R . . C2 C -0.0592(4) 0.2336(2) 0.5817(4) 0.0223(6) Uani 1 1 d . . . H2A H -0.1237 0.2494 0.4606 0.027 Uiso 1 1 calc R . . H2B H -0.0713 0.2886 0.6504 0.027 Uiso 1 1 calc R . . C3 C -0.1259(4) 0.1396(2) 0.6269(4) 0.0204(6) Uani 1 1 d . . . C4 C -0.0464(4) 0.1215(2) 0.8171(4) 0.0267(6) Uani 1 1 d . . . H4A H -0.0950 0.0617 0.8424 0.040 Uiso 1 1 calc R . . H4B H -0.0721 0.1768 0.8752 0.040 Uiso 1 1 calc R . . H4C H 0.0791 0.1144 0.8559 0.040 Uiso 1 1 calc R . . C5 C -0.3218(4) 0.1410(2) 0.5575(4) 0.0276(6) Uani 1 1 d . . . H5A H -0.3689 0.1462 0.4340 0.041 Uiso 1 1 calc R . . H5B H -0.3599 0.1971 0.6041 0.041 Uiso 1 1 calc R . . H5C H -0.3630 0.0806 0.5895 0.041 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.01840(17) 0.01325(15) 0.01973(18) -0.00010(10) 0.01029(13) -0.00153(11) Cl1 0.0370(4) 0.0205(3) 0.0284(4) 0.0024(3) 0.0213(3) -0.0026(3) Cl2 0.0240(3) 0.0221(3) 0.0279(4) 0.0003(3) 0.0038(3) -0.0008(3) O1 0.0238(10) 0.0138(9) 0.0291(11) -0.0007(7) 0.0142(9) -0.0028(7) O2 0.0202(9) 0.0131(9) 0.0242(10) -0.0034(7) 0.0124(8) -0.0014(7) C1 0.0349(16) 0.0149(13) 0.0375(17) -0.0009(12) 0.0208(14) -0.0061(12) C2 0.0252(14) 0.0142(12) 0.0305(15) -0.0033(11) 0.0141(12) 0.0020(11) C3 0.0243(14) 0.0174(13) 0.0256(14) -0.0037(11) 0.0162(12) 0.0008(11) C4 0.0356(17) 0.0246(15) 0.0248(15) -0.0028(12) 0.0171(13) -0.0024(12) C5 0.0240(14) 0.0247(15) 0.0395(18) -0.0051(13) 0.0183(14) 0.0001(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 O2 1.886(2) . y Ga1 O2 1.9753(17) 3_556 y Ga1 Cl2 2.1595(8) . y Ga1 O1 2.1613(19) . y Ga1 Cl1 2.1715(8) . y O1 C1 1.442(3) . ? O1 C2 1.442(3) . ? O2 C3 1.454(3) . ? O2 Ga1 1.9753(17) 3_556 ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.519(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C5 1.517(4) . ? C3 C4 1.526(4) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? 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 Ga1 O2 76.30(9) . 3_556 y O2 Ga1 Cl2 120.54(7) . . y O2 Ga1 Cl2 102.35(6) 3_556 . y O2 Ga1 O1 77.98(7) . . y O2 Ga1 O1 154.27(8) 3_556 . y Cl2 Ga1 O1 91.29(6) . . y O2 Ga1 Cl1 122.49(7) . . y O2 Ga1 Cl1 100.69(6) 3_556 . y Cl2 Ga1 Cl1 116.19(3) . . y O1 Ga1 Cl1 92.44(5) . . y C1 O1 C2 113.8(2) . . ? C1 O1 Ga1 122.72(16) . . ? C2 O1 Ga1 109.42(15) . . ? C3 O2 Ga1 120.02(15) . . ? C3 O2 Ga1 134.70(17) . 3_556 ? Ga1 O2 Ga1 103.70(9) . 3_556 ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 105.4(2) . . ? O1 C2 H2A 110.7 . . ? C3 C2 H2A 110.7 . . ? O1 C2 H2B 110.7 . . ? C3 C2 H2B 110.7 . . ? H2A C2 H2B 108.8 . . ? O2 C3 C5 109.2(2) . . ? O2 C3 C2 104.5(2) . . ? C5 C3 C2 110.3(2) . . ? O2 C3 C4 109.6(2) . . ? C5 C3 C4 111.5(2) . . ? C2 C3 C4 111.5(2) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? 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 Ga1 O1 C1 -155.2(2) . . . . ? O2 Ga1 O1 C1 -153.5(2) 3_556 . . . ? Cl2 Ga1 O1 C1 83.8(2) . . . . ? Cl1 Ga1 O1 C1 -32.4(2) . . . . ? O2 Ga1 O1 C2 -17.79(16) . . . . ? O2 Ga1 O1 C2 -16.1(3) 3_556 . . . ? Cl2 Ga1 O1 C2 -138.78(16) . . . . ? Cl1 Ga1 O1 C2 104.94(16) . . . . ? O2 Ga1 O2 C3 167.7(2) 3_556 . . . ? Cl2 Ga1 O2 C3 71.26(19) . . . . ? O1 Ga1 O2 C3 -13.07(18) . . . . ? Cl1 Ga1 O2 C3 -98.25(18) . . . . ? O2 Ga1 O2 Ga1 0.0 3_556 . . 3_556 ? Cl2 Ga1 O2 Ga1 -96.42(8) . . . 3_556 ? O1 Ga1 O2 Ga1 179.26(10) . . . 3_556 ? Cl1 Ga1 O2 Ga1 94.08(8) . . . 3_556 ? C1 O1 C2 C3 -176.8(2) . . . . ? Ga1 O1 C2 C3 41.7(2) . . . . ? Ga1 O2 C3 C5 157.08(18) . . . . ? Ga1 O2 C3 C5 -39.9(3) 3_556 . . . ? Ga1 O2 C3 C2 39.1(3) . . . . ? Ga1 O2 C3 C2 -157.85(19) 3_556 . . . ? Ga1 O2 C3 C4 -80.5(2) . . . . ? Ga1 O2 C3 C4 82.5(3) 3_556 . . . ? O1 C2 C3 O2 -49.9(3) . . . . ? O1 C2 C3 C5 -167.1(2) . . . . ? O1 C2 C3 C4 68.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.119 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.095 # Attachment 'STR0498_2.cif' data_STR0498 _database_code_depnum_ccdc_archive 'CCDC 663203' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'C8 H20 Cl Ga N2 O2' _chemical_melting_point ? _chemical_formula_moiety 'C8 H20 Cl Ga N2 O2' _chemical_formula_sum 'C8 H20 Cl Ga N2 O2' _chemical_formula_weight 281.43 _exptl_special_details ; The structure was found to be disordered over two sites in the ratio 82:18 but with Ga1 and Cl1 common to both parts. The ligands were modelled anisotropically with SADI and EADP restraints and constraints used. The hydrogen atoms were geometrically placed on all atoms as necessary within the part instructions including those of the methyl groups. In addition, the structure was found to be a racemic twin with the ratio 66:33. ; 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 Pna21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 9.3818(8) _cell_length_b 12.2919(10) _cell_length_c 10.7257(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1236.89(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5075 _cell_measurement_theta_min 2.520 _cell_measurement_theta_max 28.260 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 2.421 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8189 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS v2.03' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10360 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 28.26 _reflns_number_total 2945 _reflns_number_gt 2812 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0279P)^2^+0.5385P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier synthesis' _atom_sites_solution_hydrogens 'geometrically placed' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.332(13) _refine_ls_number_reflns 2945 _refine_ls_number_parameters 165 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0292 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0637 _refine_ls_wR_factor_gt 0.0628 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.67682(2) 0.484909(17) 0.42818(4) 0.02351(8) Uani 1 1 d . . . Cl1 Cl 0.76723(8) 0.41660(7) 0.25108(7) 0.03539(16) Uani 1 1 d . A . O1 O 0.5282(2) 0.58057(17) 0.4047(3) 0.0338(6) Uani 0.821(2) 1 d PD A 1 C1 C 0.3901(4) 0.5350(3) 0.3902(4) 0.0371(8) Uani 0.821(2) 1 d PD A 1 H1A H 0.3406 0.5707 0.3197 0.044 Uiso 0.821(2) 1 calc PR A 1 H1B H 0.3334 0.5477 0.4667 0.044 Uiso 0.821(2) 1 calc PR A 1 C2 C 0.4020(4) 0.4135(3) 0.3656(4) 0.0334(7) Uani 0.821(2) 1 d PD A 1 H2A H 0.3084 0.3782 0.3789 0.040 Uiso 0.821(2) 1 calc PR A 1 H2B H 0.4315 0.4007 0.2782 0.040 Uiso 0.821(2) 1 calc PR A 1 N1 N 0.5075(3) 0.3673(2) 0.4508(3) 0.0259(6) Uani 0.821(2) 1 d PD A 1 C3 C 0.5444(4) 0.2548(3) 0.4134(6) 0.0460(10) Uani 0.821(2) 1 d PD A 1 H3A H 0.4619 0.2072 0.4268 0.069 Uiso 0.821(2) 1 calc PR A 1 H3B H 0.6247 0.2289 0.4638 0.069 Uiso 0.821(2) 1 calc PR A 1 H3C H 0.5709 0.2537 0.3251 0.069 Uiso 0.821(2) 1 calc PR A 1 C4 C 0.4561(4) 0.3656(3) 0.5786(4) 0.0407(9) Uani 0.821(2) 1 d PD A 1 H4A H 0.3794 0.3118 0.5863 0.061 Uiso 0.821(2) 1 calc PR A 1 H4B H 0.4197 0.4377 0.6010 0.061 Uiso 0.821(2) 1 calc PR A 1 H4C H 0.5345 0.3460 0.6347 0.061 Uiso 0.821(2) 1 calc PR A 1 O11 O 0.7675(3) 0.4264(2) 0.5649(3) 0.0348(6) Uani 0.821(2) 1 d PD A 1 C11 C 0.8960(4) 0.4774(3) 0.5990(4) 0.0414(9) Uani 0.821(2) 1 d PD A 1 H11A H 0.9701 0.4214 0.6131 0.050 Uiso 0.821(2) 1 calc PR A 1 H11B H 0.8820 0.5176 0.6781 0.050 Uiso 0.821(2) 1 calc PR A 1 C12 C 0.9461(4) 0.5557(3) 0.4987(4) 0.0388(9) Uani 0.821(2) 1 d PD A 1 H12A H 1.0158 0.6075 0.5343 0.047 Uiso 0.821(2) 1 calc PR A 1 H12B H 0.9935 0.5149 0.4308 0.047 Uiso 0.821(2) 1 calc PR A 1 N11 N 0.8228(3) 0.6150(2) 0.4493(3) 0.0297(7) Uani 0.821(2) 1 d PD A 1 C13 C 0.8562(6) 0.6751(4) 0.3341(4) 0.0398(10) Uani 0.821(2) 1 d PD A 1 H13A H 0.9242 0.7333 0.3527 0.060 Uiso 0.821(2) 1 calc PR A 1 H13B H 0.7685 0.7067 0.3000 0.060 Uiso 0.821(2) 1 calc PR A 1 H13C H 0.8979 0.6252 0.2728 0.060 Uiso 0.821(2) 1 calc PR A 1 C14 C 0.7681(5) 0.6946(3) 0.5420(4) 0.0459(9) Uani 0.821(2) 1 d PD A 1 H14A H 0.8363 0.7544 0.5509 0.069 Uiso 0.821(2) 1 calc PR A 1 H14B H 0.7556 0.6584 0.6227 0.069 Uiso 0.821(2) 1 calc PR A 1 H14C H 0.6762 0.7234 0.5136 0.069 Uiso 0.821(2) 1 calc PR A 1 O1' O 0.7125(13) 0.4065(10) 0.5637(14) 0.0338(6) Uani 0.179(2) 1 d PD A 2 C1' C 0.6075(15) 0.3270(12) 0.5866(14) 0.0371(8) Uani 0.179(2) 1 d PD A 2 H1'A H 0.5470 0.3501 0.6574 0.044 Uiso 0.179(2) 1 calc PR A 2 H1'B H 0.6539 0.2574 0.6092 0.044 Uiso 0.179(2) 1 calc PR A 2 C2' C 0.5153(17) 0.3108(13) 0.4709(15) 0.0334(7) Uani 0.179(2) 1 d PD A 2 H2'A H 0.5668 0.2654 0.4093 0.040 Uiso 0.179(2) 1 calc PR A 2 H2'B H 0.4260 0.2729 0.4939 0.040 Uiso 0.179(2) 1 calc PR A 2 N1' N 0.4826(12) 0.4157(9) 0.4171(12) 0.0259(6) Uani 0.179(2) 1 d PD A 2 C3' C 0.424(2) 0.3976(14) 0.2937(17) 0.0460(10) Uani 0.179(2) 1 d PD A 2 H3'A H 0.3289 0.3645 0.3013 0.069 Uiso 0.179(2) 1 calc PR A 2 H3'B H 0.4863 0.3488 0.2467 0.069 Uiso 0.179(2) 1 calc PR A 2 H3'C H 0.4155 0.4672 0.2497 0.069 Uiso 0.179(2) 1 calc PR A 2 C4' C 0.3804(19) 0.4763(14) 0.4922(17) 0.0407(9) Uani 0.179(2) 1 d PD A 2 H4'A H 0.2862 0.4423 0.4851 0.061 Uiso 0.179(2) 1 calc PR A 2 H4'B H 0.3755 0.5515 0.4624 0.061 Uiso 0.179(2) 1 calc PR A 2 H4'C H 0.4108 0.4756 0.5796 0.061 Uiso 0.179(2) 1 calc PR A 2 O11' O 0.6069(12) 0.6224(9) 0.3811(10) 0.0348(6) Uani 0.179(2) 1 d PD A 2 C11' C 0.7034(15) 0.7130(13) 0.3715(18) 0.0414(9) Uani 0.179(2) 1 d PD A 2 H11C H 0.6886 0.7631 0.4426 0.050 Uiso 0.179(2) 1 calc PR A 2 H11D H 0.6845 0.7536 0.2935 0.050 Uiso 0.179(2) 1 calc PR A 2 C12' C 0.856(2) 0.672(2) 0.372(2) 0.0388(9) Uani 0.179(2) 1 d PD A 2 H12C H 0.8805 0.6433 0.2882 0.047 Uiso 0.179(2) 1 calc PR A 2 H12D H 0.9217 0.7321 0.3916 0.047 Uiso 0.179(2) 1 calc PR A 2 N11' N 0.8701(16) 0.5860(11) 0.4642(14) 0.0297(7) Uani 0.179(2) 1 d PD A 2 C13' C 1.0057(18) 0.5290(13) 0.4558(17) 0.0398(10) Uani 0.179(2) 1 d PD A 2 H13D H 1.0837 0.5802 0.4720 0.060 Uiso 0.179(2) 1 calc PR A 2 H13E H 1.0166 0.4982 0.3721 0.060 Uiso 0.179(2) 1 calc PR A 2 H13F H 1.0083 0.4704 0.5177 0.060 Uiso 0.179(2) 1 calc PR A 2 C14' C 0.856(2) 0.6336(15) 0.5920(15) 0.0459(9) Uani 0.179(2) 1 d PD A 2 H14D H 0.9398 0.6790 0.6099 0.069 Uiso 0.179(2) 1 calc PR A 2 H14E H 0.8504 0.5748 0.6536 0.069 Uiso 0.179(2) 1 calc PR A 2 H14F H 0.7699 0.6782 0.5964 0.069 Uiso 0.179(2) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.02244(12) 0.02193(12) 0.02617(13) -0.00453(19) -0.00423(14) 0.00014(9) Cl1 0.0365(4) 0.0410(4) 0.0286(3) -0.0106(3) 0.0041(3) -0.0042(3) O1 0.0249(11) 0.0242(10) 0.0523(18) 0.0015(10) -0.0030(11) 0.0005(8) C1 0.0267(16) 0.0363(18) 0.048(2) 0.0064(14) -0.0059(13) 0.0037(14) C2 0.0285(18) 0.0347(19) 0.0369(18) -0.0057(15) -0.0042(14) -0.0078(15) N1 0.0264(12) 0.0199(14) 0.0313(18) 0.0003(11) -0.0049(10) -0.0048(11) C3 0.0396(18) 0.0236(14) 0.075(3) -0.010(2) -0.009(2) -0.0043(13) C4 0.033(2) 0.044(2) 0.046(2) 0.0091(16) 0.0004(16) -0.0046(15) O11 0.0367(15) 0.0355(14) 0.0321(12) 0.0074(11) -0.0097(12) -0.0100(12) C11 0.035(2) 0.045(2) 0.044(2) -0.0008(16) -0.0163(17) -0.0090(16) C12 0.034(2) 0.042(2) 0.040(2) -0.0045(16) -0.0073(16) -0.0116(17) N11 0.0343(17) 0.0256(14) 0.0291(18) -0.0072(13) 0.0002(13) -0.0054(11) C13 0.047(2) 0.0323(19) 0.040(3) 0.001(2) -0.0002(19) -0.0134(17) C14 0.054(3) 0.033(2) 0.050(2) -0.0204(17) 0.0036(19) -0.0084(18) O1' 0.0249(11) 0.0242(10) 0.0523(18) 0.0015(10) -0.0030(11) 0.0005(8) C1' 0.0267(16) 0.0363(18) 0.048(2) 0.0064(14) -0.0059(13) 0.0037(14) C2' 0.0285(18) 0.0347(19) 0.0369(18) -0.0057(15) -0.0042(14) -0.0078(15) N1' 0.0264(12) 0.0199(14) 0.0313(18) 0.0003(11) -0.0049(10) -0.0048(11) C3' 0.0396(18) 0.0236(14) 0.075(3) -0.010(2) -0.009(2) -0.0043(13) C4' 0.033(2) 0.044(2) 0.046(2) 0.0091(16) 0.0004(16) -0.0046(15) O11' 0.0367(15) 0.0355(14) 0.0321(12) 0.0074(11) -0.0097(12) -0.0100(12) C11' 0.035(2) 0.045(2) 0.044(2) -0.0008(16) -0.0163(17) -0.0090(16) C12' 0.034(2) 0.042(2) 0.040(2) -0.0045(16) -0.0073(16) -0.0116(17) N11' 0.0343(17) 0.0256(14) 0.0291(18) -0.0072(13) 0.0002(13) -0.0054(11) C13' 0.047(2) 0.0323(19) 0.040(3) 0.001(2) -0.0002(19) -0.0134(17) C14' 0.054(3) 0.033(2) 0.050(2) -0.0204(17) 0.0036(19) -0.0084(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 O1' 1.776(14) . y Ga1 O1 1.841(2) . y Ga1 O11 1.842(3) . y Ga1 O11' 1.882(11) . y Ga1 N1' 2.014(11) . y Ga1 N11 2.118(3) . y Ga1 N1 2.161(3) . y Ga1 N11' 2.231(14) . y Ga1 Cl1 2.2433(8) . y O1 C1 1.421(4) . ? C1 C2 1.521(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N1 1.462(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N1 C4 1.453(5) . ? N1 C3 1.481(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? O11 C11 1.407(4) . ? C11 C12 1.518(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N11 1.466(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? N11 C13 1.473(5) . ? N11 C14 1.487(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? O1' C1' 1.409(14) . ? C1' C2' 1.525(15) . ? C1' H1'A 0.9900 . ? C1' H1'B 0.9900 . ? C2' N1' 1.446(15) . ? C2' H2'A 0.9900 . ? C2' H2'B 0.9900 . ? N1' C3' 1.453(16) . ? N1' C4' 1.457(15) . ? C3' H3'A 0.9800 . ? C3' H3'B 0.9800 . ? C3' H3'C 0.9800 . ? C4' H4'A 0.9800 . ? C4' H4'B 0.9800 . ? C4' H4'C 0.9800 . ? O11' C11' 1.440(15) . ? C11' C12' 1.517(18) . ? C11' H11C 0.9900 . ? C11' H11D 0.9900 . ? C12' N11' 1.454(17) . ? C12' H12C 0.9900 . ? C12' H12D 0.9900 . ? N11' C13' 1.455(15) . ? N11' C14' 1.497(15) . ? C13' H13D 0.9800 . ? C13' H13E 0.9800 . ? C13' H13F 0.9800 . ? C14' H14D 0.9800 . ? C14' H14E 0.9800 . ? C14' H14F 0.9800 . ? 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' Ga1 O1 127.0(5) . . ? O1' Ga1 O11 18.0(3) . . ? O1 Ga1 O11 135.08(13) . . y O1' Ga1 O11' 140.6(6) . . y O1 Ga1 O11' 29.0(3) . . ? O11 Ga1 O11' 136.5(3) . . ? O1' Ga1 N1' 89.4(5) . . y O1 Ga1 N1' 65.0(3) . . ? O11 Ga1 N1' 107.4(4) . . ? O11' Ga1 N1' 92.7(5) . . y O1' Ga1 N11 101.5(4) . . ? O1 Ga1 N11 91.27(11) . . y O11 Ga1 N11 84.89(12) . . y O11' Ga1 N11 64.9(3) . . ? N1' Ga1 N11 155.5(3) . . ? O1' Ga1 N1 71.6(4) . . ? O1 Ga1 N1 83.45(11) . . y O11 Ga1 N1 89.37(12) . . y O11' Ga1 N1 112.0(3) . . ? N1' Ga1 N1 19.8(3) . . ? N11 Ga1 N1 165.55(11) . . y O1' Ga1 N11' 90.4(5) . . y O1 Ga1 N11' 106.5(4) . . ? O11 Ga1 N11' 72.8(4) . . ? O11' Ga1 N11' 80.2(5) . . y N1' Ga1 N11' 168.6(5) . . y N11 Ga1 N11' 15.3(3) . . ? N1 Ga1 N11' 161.8(4) . . ? O1' Ga1 Cl1 114.8(5) . . y O1 Ga1 Cl1 114.18(9) . . y O11 Ga1 Cl1 110.70(10) . . y O11' Ga1 Cl1 103.9(4) . . y N1' Ga1 Cl1 97.7(3) . . y N11 Ga1 Cl1 97.38(8) . . y N1 Ga1 Cl1 97.05(7) . . y N11' Ga1 Cl1 92.7(4) . . y C1 O1 Ga1 117.02(19) . . ? O1 C1 C2 109.8(3) . . ? O1 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? O1 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? N1 C2 C1 108.9(3) . . ? N1 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? N1 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C4 N1 C2 111.7(3) . . ? C4 N1 C3 108.6(3) . . ? C2 N1 C3 110.6(3) . . ? C4 N1 Ga1 111.1(2) . . ? C2 N1 Ga1 99.7(2) . . ? C3 N1 Ga1 115.0(2) . . ? N1 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C11 O11 Ga1 115.4(2) . . ? O11 C11 C12 111.3(3) . . ? O11 C11 H11A 109.4 . . ? C12 C11 H11A 109.4 . . ? O11 C11 H11B 109.4 . . ? C12 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? N11 C12 C11 109.1(3) . . ? N11 C12 H12A 109.9 . . ? C11 C12 H12A 109.9 . . ? N11 C12 H12B 109.9 . . ? C11 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? C12 N11 C13 112.7(3) . . ? C12 N11 C14 111.0(3) . . ? C13 N11 C14 107.7(3) . . ? C12 N11 Ga1 100.0(2) . . ? C13 N11 Ga1 115.2(3) . . ? C14 N11 Ga1 110.2(2) . . ? N11 C13 H13A 109.5 . . ? N11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N11 C14 H14A 109.5 . . ? N11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C1' O1' Ga1 112.8(10) . . ? O1' C1' C2' 110.2(12) . . ? O1' C1' H1'A 109.6 . . ? C2' C1' H1'A 109.6 . . ? O1' C1' H1'B 109.6 . . ? C2' C1' H1'B 109.6 . . ? H1'A C1' H1'B 108.1 . . ? N1' C2' C1' 109.2(12) . . ? N1' C2' H2'A 109.8 . . ? C1' C2' H2'A 109.8 . . ? N1' C2' H2'B 109.8 . . ? C1' C2' H2'B 109.8 . . ? H2'A C2' H2'B 108.3 . . ? C2' N1' C3' 107.9(11) . . ? C2' N1' C4' 112.0(13) . . ? C3' N1' C4' 109.3(13) . . ? C2' N1' Ga1 99.3(9) . . ? C3' N1' Ga1 117.6(11) . . ? C4' N1' Ga1 110.3(10) . . ? N1' C3' H3'A 109.5 . . ? N1' C3' H3'B 109.5 . . ? H3'A C3' H3'B 109.5 . . ? N1' C3' H3'C 109.5 . . ? H3'A C3' H3'C 109.5 . . ? H3'B C3' H3'C 109.5 . . ? N1' C4' H4'A 109.5 . . ? N1' C4' H4'B 109.5 . . ? H4'A C4' H4'B 109.5 . . ? N1' C4' H4'C 109.5 . . ? H4'A C4' H4'C 109.5 . . ? H4'B C4' H4'C 109.5 . . ? C11' O11' Ga1 119.7(9) . . ? O11' C11' C12' 109.5(15) . . ? O11' C11' H11C 109.8 . . ? C12' C11' H11C 109.8 . . ? O11' C11' H11D 109.8 . . ? C12' C11' H11D 109.8 . . ? H11C C11' H11D 108.2 . . ? N11' C12' C11' 109.3(15) . . ? N11' C12' H12C 109.8 . . ? C11' C12' H12C 109.8 . . ? N11' C12' H12D 109.8 . . ? C11' C12' H12D 109.8 . . ? H12C C12' H12D 108.3 . . ? C12' N11' C13' 112.8(13) . . ? C12' N11' C14' 109.5(15) . . ? C13' N11' C14' 108.6(13) . . ? C12' N11' Ga1 102.2(12) . . ? C13' N11' Ga1 115.6(10) . . ? C14' N11' Ga1 107.9(10) . . ? N11' C13' H13D 109.5 . . ? N11' C13' H13E 109.5 . . ? H13D C13' H13E 109.5 . . ? N111' C13' H13F 109.5 . . ? H13D C13' H13F 109.5 . . ? H13E C13' H13F 109.5 . . ? N11' C14' H14D 109.5 . . ? N11' C14' H14E 109.5 . . ? H14D C14' H14E 109.5 . . ? N11' C14' H14F 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? 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 O1' Ga1 O1 C1 -71.6(6) . . . . ? O11 Ga1 O1 C1 -93.0(3) . . . . ? O11' Ga1 O1 C1 158.9(8) . . . . ? N1' Ga1 O1 C1 -3.0(5) . . . . ? N11 Ga1 O1 C1 -177.1(3) . . . . ? N1 Ga1 O1 C1 -10.5(3) . . . . ? N11' Ga1 O1 C1 -175.0(5) . . . . ? Cl1 Ga1 O1 C1 84.3(3) . . . . ? Ga1 O1 C1 C2 -14.0(4) . . . . ? O1 C1 C2 N1 43.8(4) . . . . ? C1 C2 N1 C4 70.5(4) . . . . ? C1 C2 N1 C3 -168.3(3) . . . . ? C1 C2 N1 Ga1 -46.9(3) . . . . ? O1' Ga1 N1 C4 47.0(5) . . . . ? O1 Ga1 N1 C4 -85.6(2) . . . . ? O11 Ga1 N1 C4 50.0(3) . . . . ? O11' Ga1 N1 C4 -91.1(4) . . . . ? N1' Ga1 N1 C4 -106.0(11) . . . . ? N11 Ga1 N1 C4 -16.4(6) . . . . ? N11' Ga1 N1 C4 38.8(12) . . . . ? Cl1 Ga1 N1 C4 160.8(2) . . . . ? O1' Ga1 N1 C2 164.9(5) . . . . ? O1 Ga1 N1 C2 32.4(2) . . . . ? O11 Ga1 N1 C2 167.9(2) . . . . ? O11' Ga1 N1 C2 26.9(4) . . . . ? N1' Ga1 N1 C2 11.9(10) . . . . ? N11 Ga1 N1 C2 101.5(5) . . . . ? N11' Ga1 N1 C2 156.7(11) . . . . ? Cl1 Ga1 N1 C2 -81.3(2) . . . . ? O1' Ga1 N1 C3 -76.8(6) . . . . ? O1 Ga1 N1 C3 150.6(3) . . . . ? O11 Ga1 N1 C3 -73.8(3) . . . . ? O11' Ga1 N1 C3 145.1(5) . . . . ? N1' Ga1 N1 C3 130.2(11) . . . . ? N11 Ga1 N1 C3 -140.2(5) . . . . ? N11' Ga1 N1 C3 -85.0(12) . . . . ? Cl1 Ga1 N1 C3 37.0(3) . . . . ? O1' Ga1 O11 C11 -169.4(17) . . . . ? O1 Ga1 O11 C11 -98.7(3) . . . . ? O11' Ga1 O11 C11 -56.6(6) . . . . ? N1' Ga1 O11 C11 -170.4(4) . . . . ? N11 Ga1 O11 C11 -12.0(3) . . . . ? N1 Ga1 O11 C11 -178.7(3) . . . . ? N11' Ga1 O11 C11 -2.4(4) . . . . ? Cl1 Ga1 O11 C11 84.0(3) . . . . ? Ga1 O11 C11 C12 -11.5(4) . . . . ? O11 C11 C12 N11 40.7(4) . . . . ? C11 C12 N11 C13 -167.7(3) . . . . ? C11 C12 N11 C14 71.4(4) . . . . ? C11 C12 N11 Ga1 -44.8(3) . . . . ? O1' Ga1 N11 C12 39.1(5) . . . . ? O1 Ga1 N11 C12 167.3(2) . . . . ? O11 Ga1 N11 C12 32.1(2) . . . . ? O11' Ga1 N11 C12 179.9(5) . . . . ? N1' Ga1 N11 C12 154.1(9) . . . . ? N1 Ga1 N11 C12 99.0(5) . . . . ? N11' Ga1 N11 C12 -5.1(15) . . . . ? Cl1 Ga1 N11 C12 -78.2(2) . . . . ? O1' Ga1 N11 C13 160.1(5) . . . . ? O1 Ga1 N11 C13 -71.7(3) . . . . ? O11 Ga1 N11 C13 153.1(3) . . . . ? O11' Ga1 N11 C13 -59.1(5) . . . . ? N1' Ga1 N11 C13 -84.9(10) . . . . ? N1 Ga1 N11 C13 -139.9(5) . . . . ? N11' Ga1 N11 C13 115.9(16) . . . . ? Cl1 Ga1 N11 C13 42.9(3) . . . . ? O1' Ga1 N11 C14 -77.8(5) . . . . ? O1 Ga1 N11 C14 50.4(3) . . . . ? O11 Ga1 N11 C14 -84.8(3) . . . . ? O11' Ga1 N11 C14 63.0(5) . . . . ? N1' Ga1 N11 C14 37.3(10) . . . . ? N1 Ga1 N11 C14 -17.8(6) . . . . ? N11' Ga1 N11 C14 -121.9(16) . . . . ? Cl1 Ga1 N11 C14 165.0(3) . . . . ? O1 Ga1 O1' C1' 66.4(13) . . . . ? O11 Ga1 O1' C1' -170(2) . . . . ? O11' Ga1 O1' C1' 102.5(12) . . . . ? N1' Ga1 O1' C1' 8.9(11) . . . . ? N11 Ga1 O1' C1' 166.9(10) . . . . ? N1 Ga1 O1' C1' 0.1(10) . . . . ? N11' Ga1 O1' C1' 177.5(12) . . . . ? Cl1 Ga1 O1' C1' -89.3(11) . . . . ? Ga1 O1' C1' C2' 15.1(17) . . . . ? O1' C1' C2' N1' -42.5(18) . . . . ? C1' C2' N1' C3' 167.3(14) . . . . ? C1' C2' N1' C4' -72.3(16) . . . . ? C1' C2' N1' Ga1 44.1(14) . . . . ? O1' Ga1 N1' C2' -30.7(10) . . . . ? O1 Ga1 N1' C2' -162.6(10) . . . . ? O11 Ga1 N1' C2' -30.3(9) . . . . ? O11' Ga1 N1' C2' -171.3(9) . . . . ? N11 Ga1 N1' C2' -148.1(8) . . . . ? N1 Ga1 N1' C2' -5.1(8) . . . . ? N11' Ga1 N1' C2' -120(3) . . . . ? Cl1 Ga1 N1' C2' 84.3(9) . . . . ? O1' Ga1 N1' C3' -146.6(11) . . . . ? O1 Ga1 N1' C3' 81.4(10) . . . . ? O11 Ga1 N1' C3' -146.3(10) . . . . ? O11' Ga1 N1' C3' 72.8(11) . . . . ? N11 Ga1 N1' C3' 96.0(12) . . . . ? N1 Ga1 N1' C3' -121.1(16) . . . . ? N11' Ga1 N1' C3' 124(3) . . . . ? Cl1 Ga1 N1' C3' -31.7(11) . . . . ? O1' Ga1 N1' C4' 87.1(11) . . . . ? O1 Ga1 N1' C4' -44.9(10) . . . . ? O11 Ga1 N1' C4' 87.4(10) . . . . ? O11' Ga1 N1' C4' -53.5(11) . . . . ? N11 Ga1 N1' C4' -30.3(16) . . . . ? N1 Ga1 N1' C4' 112.6(16) . . . . ? N11' Ga1 N1' C4' -2(3) . . . . ? Cl1 Ga1 N1' C4' -158.0(10) . . . . ? O1' Ga1 O11' C11' 87.7(14) . . . . ? O1 Ga1 O11' C11' 163.7(16) . . . . ? O11 Ga1 O11' C11' 61.0(13) . . . . ? N1' Ga1 O11' C11' -179.9(12) . . . . ? N11 Ga1 O11' C11' 10.4(11) . . . . ? N1 Ga1 O11' C11' 175.0(11) . . . . ? N11' Ga1 O11' C11' 9.1(12) . . . . ? Cl1 Ga1 O11' C11' -81.3(12) . . . . ? Ga1 O11' C11' C12' 14.0(19) . . . . ? O11' C11' C12' N11' -42(2) . . . . ? C11' C12' N11' C13' 170.0(16) . . . . ? C11' C12' N11' C14' -69(2) . . . . ? C11' C12' N11' Ga1 45.3(19) . . . . ? O1' Ga1 N11' C12' -171.9(12) . . . . ? O1 Ga1 N11' C12' -42.9(12) . . . . ? O11 Ga1 N11' C12' -175.9(12) . . . . ? O11' Ga1 N11' C12' -30.4(11) . . . . ? N1' Ga1 N11' C12' -83(3) . . . . ? N11 Ga1 N11' C12' -34.9(14) . . . . ? N1 Ga1 N11' C12' -164.1(12) . . . . ? Cl1 Ga1 N11' C12' 73.3(11) . . . . ? O1' Ga1 N11' C13' 65.2(12) . . . . ? O1 Ga1 N11' C13' -165.8(10) . . . . ? O11 Ga1 N11' C13' 61.2(11) . . . . ? O11' Ga1 N11' C13' -153.3(12) . . . . ? N1' Ga1 N11' C13' 154(2) . . . . ? N11 Ga1 N11' C13' -158(2) . . . . ? N1 Ga1 N11' C13' 73.0(17) . . . . ? Cl1 Ga1 N11' C13' -49.6(11) . . . . ? O1' Ga1 N11' C14' -56.6(11) . . . . ? O1 Ga1 N11' C14' 72.4(11) . . . . ? O11 Ga1 N11' C14' -60.6(10) . . . . ? O11' Ga1 N11' C14' 84.9(11) . . . . ? N1' Ga1 N11' C14' 32(3) . . . . ? N11 Ga1 N11' C14' 80.4(17) . . . . ? N1 Ga1 N11' C14' -48.8(18) . . . . ? Cl1 Ga1 N11' C14' -171.4(10) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.718 _refine_diff_density_min -0.296 _refine_diff_density_rms 0.069