Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_final _database_code_CSD 161556 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Ferey, Gerard' 'Livage, Carine' 'Loiseau, Thierry' 'Millange, Franck' 'O'Hare, Dermot' 'Simon, Nathalie' 'Walton, Richard' _publ_contact_author_name 'Prof Gerard Ferey' _publ_contact_author_address ; Prof Gerard Ferey UMR CNRS 8637 Universite de Versailles St Quentin-en-Yvelines Institut Lavoisier 45, Avenue des Etats-Unis Versailles 78035 FRANCE ; _publ_contact_author_email 'FEREY@CHIMIE.UVSQ.FR' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'Ga3F2(OH)4(H2PO4)(HPO4)3 [H3N(CH2)6NH3]2 3.5H2O' _chemical_formula_moiety 'C12 H52 F2 Ga3 N4 O23.50 P4' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C12 H52 F2 Ga3 N4 O23.50 P4' _chemical_formula_weight 999.62 _chemical_melting_point ? _chemical_compound_source 'synthesised by authors' 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' '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.2007(15) _cell_length_b 14.417(4) _cell_length_c 23.195(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.91(3) _cell_angle_gamma 90.00 _cell_volume 3393.0(14) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4263 _cell_measurement_theta_min 1.67 _cell_measurement_theta_max 26.37 _exptl_crystal_description parallelepiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.957 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 2044 _exptl_absorpt_coefficient_mu 2.659 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6616 _exptl_absorpt_correction_T_max 0.8578 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 20065 _diffrn_reflns_av_R_equivalents 0.0623 _diffrn_reflns_av_sigmaI/netI 0.0757 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 26.37 _reflns_number_total 6931 _reflns_number_observed 4263 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+16.0021P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00019(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6931 _refine_ls_number_parameters 395 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1067 _refine_ls_R_factor_obs 0.0562 _refine_ls_wR_factor_all 0.1564 _refine_ls_wR_factor_obs 0.1319 _refine_ls_goodness_of_fit_all 1.026 _refine_ls_goodness_of_fit_obs 1.119 _refine_ls_restrained_S_all 1.026 _refine_ls_restrained_S_obs 1.119 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ga1 Ga 0.24128(7) 0.38146(5) 0.21751(3) 0.0184(2) Uani 1 d . . Ga2 Ga 0.50279(7) 0.21421(5) 0.25168(3) 0.0183(2) Uani 1 d . . Ga3 Ga 0.73896(7) 0.54780(5) 0.21461(3) 0.0185(2) Uani 1 d . . P1 P 0.5222(2) 0.39373(12) 0.17025(7) 0.0184(4) Uani 1 d . . P2 P 0.2655(2) 0.18661(12) 0.15595(8) 0.0215(4) Uani 1 d . . P3 P 0.7608(2) 0.74292(13) 0.15200(8) 0.0224(4) Uani 1 d . . P4 P 0.0246(2) 0.53344(12) 0.16890(7) 0.0188(4) Uani 1 d . . O1 O 0.1000(4) 0.3309(3) 0.2536(2) 0.0125(9) Uani 1 d . . O2 O 0.1328(5) 0.4613(3) 0.1674(2) 0.0257(11) Uani 1 d . . O3 O 0.2576(4) 0.4669(3) 0.2817(2) 0.0140(9) Uani 1 d . . O4 O 0.2272(5) 0.2877(3) 0.1572(2) 0.0240(11) Uani 1 d . . O5 O 0.4015(4) 0.4363(3) 0.1942(2) 0.0220(11) Uani 1 d . . O6 O 0.5987(5) 0.2623(3) 0.3203(2) 0.0256(11) Uani 1 d . . O7 O 0.4032(4) 0.1646(3) 0.1824(2) 0.0240(11) Uani 1 d . . O8 O 0.4245(5) 0.1180(3) 0.2966(2) 0.0267(12) Uani 1 d . . O9 O 0.5781(4) 0.3104(3) 0.2050(2) 0.0256(11) Uani 1 d . . O10 O 0.5971(4) 0.5966(3) 0.2511(2) 0.0113(9) Uani 1 d . . O11 O 0.7574(4) 0.4619(3) 0.2777(2) 0.0130(9) Uani 1 d . . O12 O 0.6296(4) 0.4658(3) 0.1657(2) 0.0213(10) Uani 1 d . . O13 O 0.7264(5) 0.6400(3) 0.1543(2) 0.0236(11) Uani 1 d . . O14 O 0.9004(5) 0.4927(3) 0.1905(2) 0.0279(12) Uani 1 d . . O15 O 0.4814(5) 0.3616(4) 0.1060(2) 0.0358(13) Uani 1 d . . O16 O 0.7378(5) 0.7833(4) 0.0928(2) 0.0364(13) Uani 1 d . . O17 O 0.2484(5) 0.1492(4) 0.0933(2) 0.0400(14) Uani 1 d . . O18 O 0.1652(5) 0.1308(3) 0.1907(2) 0.0327(13) Uani 1 d . . O19 O 0.6657(5) 0.7933(4) 0.1934(2) 0.0346(13) Uani 1 d . . O20 O -0.0035(6) 0.5615(4) 0.1031(2) 0.0404(14) Uani 1 d . . F1 F 0.3551(4) 0.2939(3) 0.2669(2) 0.0222(9) Uani 1 d . . F2 F 0.8528(4) 0.6338(3) 0.2649(2) 0.0229(9) Uani 1 d . . N1 N 0.1364(6) 0.1593(5) 0.3138(3) 0.037(2) Uiso 1 d . . H1A H 0.0753(35) 0.1246(31) 0.2940(4) 0.056 Uiso 1 calc R . H1B H 0.2161(22) 0.1385(36) 0.3079(4) 0.056 Uiso 1 calc R . H1C H 0.1278(54) 0.2179(7) 0.3020(6) 0.056 Uiso 1 calc R . N2 N -0.1384(7) 0.2696(5) 0.1854(3) 0.040(2) Uiso 1 d . . H2A H -0.0756(34) 0.3076(32) 0.2008(7) 0.061 Uiso 1 calc R . H2B H -0.1334(56) 0.2159(7) 0.2044(6) 0.061 Uiso 1 calc R . H2C H -0.2170(24) 0.2952(37) 0.1880(3) 0.061 Uiso 1 calc R . N3 N 0.4893(6) -0.0250(4) 0.1747(2) 0.0255(14) Uani 1 d . . H3A H 0.4451(39) -0.0676(19) 0.1926(4) 0.038 Uiso 1 calc R . H3B H 0.4556(42) 0.0308(14) 0.1803(3) 0.038 Uiso 1 calc R . H3C H 0.5737(7) -0.0259(32) 0.1889(5) 0.038 Uiso 1 calc R . N4 N 0.5172(6) 0.4487(4) 0.3274(2) 0.0275(14) Uani 1 d . . H4A H 0.5424(44) 0.3900(11) 0.3246(5) 0.041 Uiso 1 calc R . H4B H 0.5610(38) 0.4841(22) 0.3045(4) 0.041 Uiso 1 calc R . H4C H 0.4311(9) 0.4533(32) 0.3167(7) 0.041 Uiso 1 calc R . C1 C 0.1195(9) 0.1541(7) 0.3766(4) 0.050(2) Uiso 1 d . . H1A H 0.0331(9) 0.1779(7) 0.3827(4) 0.060 Uiso 1 calc R . H1B H 0.1227(9) 0.0896(7) 0.3885(4) 0.060 Uiso 1 calc R . C2 C 0.2189(9) 0.2057(7) 0.4136(4) 0.046(2) Uiso 1 d . . H2A H 0.2118(9) 0.2710(7) 0.4038(4) 0.055 Uiso 1 calc R . H2B H 0.3058(9) 0.1848(7) 0.4059(4) 0.055 Uiso 1 calc R . C3 C 0.2060(14) 0.1947(10) 0.4761(6) 0.098(4) Uiso 1 d . . H3A H 0.1213(14) 0.2207(10) 0.4830(6) 0.117 Uiso 1 calc R . H3B H 0.2011(14) 0.1286(10) 0.4835(6) 0.117 Uiso 1 calc R . C4 C -0.1988(10) 0.2679(8) 0.0193(4) 0.061(3) Uiso 1 d . . H4A H -0.1136(10) 0.2920(8) 0.0115(4) 0.073 Uiso 1 calc R . H4B H -0.1963(10) 0.2014(8) 0.0129(4) 0.073 Uiso 1 calc R . C5 C -0.2093(13) 0.2817(10) 0.0813(5) 0.088(4) Uiso 1 d . . H5A H -0.2188(13) 0.3480(10) 0.0865(5) 0.105 Uiso 1 calc R . H5B H -0.2926(13) 0.2542(10) 0.0888(5) 0.105 Uiso 1 calc R . C6 C -0.1211(13) 0.2535(10) 0.1248(5) 0.092(4) Uiso 1 d . . H6A H -0.0373(13) 0.2811(10) 0.1181(5) 0.110 Uiso 1 calc R . H6B H -0.1112(13) 0.1870(10) 0.1203(5) 0.110 Uiso 1 calc R . C7 C 0.4786(8) -0.0454(6) 0.1119(3) 0.032(2) Uani 1 d . . H7A H 0.3868(8) -0.0432(6) 0.0961(3) 0.038 Uiso 1 calc R . H7B H 0.5117(8) -0.1073(6) 0.1057(3) 0.038 Uiso 1 calc R . C8 C 0.5571(9) 0.0250(7) 0.0810(3) 0.047(2) Uani 1 d . . H8A H 0.6455(9) 0.0291(7) 0.1006(3) 0.057 Uiso 1 calc R . H8B H 0.5162(9) 0.0855(7) 0.0829(3) 0.057 Uiso 1 calc R . C9 C 0.5649(9) -0.0008(9) 0.0178(4) 0.061(3) Uani 1 d . . H9A H 0.6240(9) 0.0421(9) 0.0012(4) 0.073 Uiso 1 calc R . H9B H 0.6024(9) -0.0624(9) 0.0161(4) 0.073 Uiso 1 calc R . C10 C 0.5453(8) 0.4800(6) 0.3878(3) 0.038(2) Uani 1 d . . H10A H 0.5239(8) 0.5454(6) 0.3899(3) 0.046 Uiso 1 calc R . H10B H 0.6388(8) 0.4731(6) 0.3995(3) 0.046 Uiso 1 calc R . C11 C 0.4701(10) 0.4278(6) 0.4290(3) 0.048(2) Uani 1 d . . H11A H 0.4815(10) 0.3617(6) 0.4232(3) 0.058 Uiso 1 calc R . H11B H 0.3770(10) 0.4418(6) 0.4210(3) 0.058 Uiso 1 calc R . C12 C 0.0153(12) 0.0480(6) -0.0079(4) 0.060(3) Uani 1 d . . H12A H 0.1097(12) 0.0574(6) -0.0010(4) 0.071 Uiso 1 calc R . H12B H -0.0265(12) 0.0902(6) 0.0172(4) 0.071 Uiso 1 calc R . OW1 O 0.2445(7) 0.4238(5) 0.0568(3) 0.068(2) Uiso 1 d . . OW2 O 0.3723(21) 0.2284(16) 0.0145(9) 0.127(7) Uiso 0.50 d P . OW3A O 0.1829(11) 0.2487(8) 0.0115(5) 0.082(3) Uiso 0.70 d P . OW3B O 0.0818(24) 0.3091(18) -0.0349(11) 0.072(7) Uiso 0.30 d P . OW4A O 0.6324(19) 0.5370(13) 0.0437(8) 0.066(5) Uiso 0.40 d P . OW4B O 0.7256(13) 0.5315(9) 0.0572(5) 0.069(3) Uiso 0.60 d P . 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 0.0169(4) 0.0137(4) 0.0248(4) -0.0005(3) 0.0032(3) 0.0009(3) Ga2 0.0165(4) 0.0136(4) 0.0247(4) 0.0005(3) 0.0017(3) 0.0004(3) Ga3 0.0160(4) 0.0144(4) 0.0252(4) 0.0008(3) 0.0032(3) -0.0010(3) P1 0.0171(9) 0.0156(9) 0.0224(9) -0.0009(7) 0.0008(7) -0.0022(7) P2 0.0219(10) 0.0148(9) 0.0269(10) -0.0043(8) -0.0014(8) -0.0002(7) P3 0.0240(10) 0.0170(10) 0.0254(10) 0.0025(8) -0.0012(8) -0.0005(8) P4 0.0165(9) 0.0162(9) 0.0235(9) -0.0016(8) 0.0014(7) 0.0012(7) O1 0.009(2) 0.010(2) 0.019(2) 0.001(2) 0.005(2) -0.001(2) O2 0.022(3) 0.020(3) 0.035(3) 0.001(2) 0.002(2) 0.005(2) O3 0.013(2) 0.009(2) 0.019(2) -0.007(2) 0.000(2) 0.002(2) O4 0.028(3) 0.016(3) 0.027(3) -0.002(2) -0.003(2) 0.004(2) O5 0.016(2) 0.019(3) 0.031(3) 0.003(2) 0.006(2) -0.004(2) O6 0.021(3) 0.023(3) 0.031(3) -0.004(2) -0.004(2) 0.004(2) O7 0.022(3) 0.019(3) 0.031(3) -0.008(2) 0.000(2) 0.005(2) O8 0.022(3) 0.018(3) 0.041(3) 0.010(2) 0.008(2) 0.002(2) O9 0.022(3) 0.018(3) 0.037(3) 0.008(2) 0.005(2) 0.001(2) O10 0.004(2) 0.014(2) 0.017(2) -0.004(2) 0.006(2) 0.001(2) O11 0.011(2) 0.011(2) 0.016(2) 0.008(2) -0.001(2) -0.004(2) O12 0.021(3) 0.015(2) 0.028(3) 0.000(2) 0.005(2) -0.005(2) O13 0.029(3) 0.017(3) 0.024(3) 0.003(2) 0.001(2) -0.003(2) O14 0.023(3) 0.020(3) 0.041(3) -0.007(2) 0.004(2) -0.002(2) O15 0.034(3) 0.047(4) 0.026(3) -0.011(3) -0.003(2) -0.005(3) O16 0.043(3) 0.032(3) 0.032(3) 0.008(3) -0.007(2) -0.007(3) O17 0.046(4) 0.038(3) 0.034(3) -0.016(3) -0.007(3) 0.008(3) O18 0.027(3) 0.022(3) 0.050(3) 0.004(3) 0.008(2) -0.004(2) O19 0.030(3) 0.032(3) 0.043(3) -0.003(3) 0.007(2) 0.006(2) O20 0.047(4) 0.048(4) 0.026(3) 0.010(3) 0.003(2) 0.001(3) F1 0.025(2) 0.014(2) 0.027(2) -0.001(2) 0.003(2) 0.004(2) F2 0.021(2) 0.023(2) 0.025(2) 0.000(2) 0.003(2) -0.003(2) N3 0.025(3) 0.020(3) 0.030(3) -0.002(3) 0.001(3) -0.002(3) N4 0.028(3) 0.025(3) 0.031(3) -0.003(3) 0.007(3) -0.002(3) C7 0.033(4) 0.034(5) 0.028(4) -0.008(4) 0.000(3) 0.001(4) C8 0.041(5) 0.066(7) 0.036(5) 0.009(5) 0.006(4) -0.006(5) C9 0.048(6) 0.099(9) 0.037(5) 0.018(6) 0.010(4) 0.009(6) C10 0.043(5) 0.037(5) 0.033(4) -0.005(4) -0.003(4) -0.014(4) C11 0.076(7) 0.038(5) 0.032(5) -0.004(4) 0.013(4) -0.012(5) C12 0.101(8) 0.046(6) 0.033(5) -0.003(5) 0.016(5) -0.002(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 O1 1.886(4) . ? Ga1 O2 1.907(5) . ? Ga1 O3 1.926(4) . ? Ga1 O4 1.940(5) . ? Ga1 O5 1.942(4) . ? Ga1 F1 1.994(4) . ? Ga2 O6 1.912(5) . ? Ga2 F2 1.944(4) 2_645 ? Ga2 O7 1.946(5) . ? Ga2 O8 1.954(5) . ? Ga2 F1 1.956(4) . ? Ga2 O9 1.964(5) . ? Ga3 O10 1.886(4) . ? Ga3 O11 1.912(4) . ? Ga3 O12 1.915(4) . ? Ga3 O13 1.925(5) . ? Ga3 O14 1.962(5) . ? Ga3 F2 1.992(4) . ? P1 O12 1.521(5) . ? P1 O9 1.525(5) . ? P1 O5 1.530(5) . ? P1 O15 1.575(5) . ? P2 O7 1.508(5) . ? P2 O4 1.509(5) . ? P2 O17 1.543(5) . ? P2 O18 1.585(5) . ? P3 O16 1.487(5) . ? P3 O13 1.526(5) . ? P3 O6 1.534(5) 2_655 ? P3 O19 1.607(5) . ? P4 O8 1.520(5) 2 ? P4 O2 1.520(5) . ? P4 O14 1.526(5) 1_455 ? P4 O20 1.575(5) . ? O6 P3 1.534(5) 2_645 ? O8 P4 1.520(5) 2_545 ? O14 P4 1.526(5) 1_655 ? F2 Ga2 1.944(4) 2_655 ? N1 C1 1.486(10) . ? N1 H1A 0.89 . ? N1 H1B 0.89 . ? N1 H1C 0.89 . ? N2 C6 1.453(13) . ? N2 H2A 0.89 . ? N2 H2B 0.89 . ? N2 H2C 0.89 . ? N3 C7 1.479(8) . ? N3 H3A 0.89 . ? N3 H3B 0.89 . ? N3 H3C 0.89 . ? N4 C10 1.470(9) . ? N4 H4A 0.89 . ? N4 H4B 0.89 . ? N4 H4C 0.89 . ? C1 C2 1.462(12) . ? C1 H1A 0.97 . ? C1 H1B 0.97 . ? C2 C3 1.476(14) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C3 C4 1.429(15) 4_666 ? C3 H3A 0.97 . ? C3 H3B 0.97 . ? C4 C3 1.429(15) 4_565 ? C4 C5 1.467(14) . ? C4 H4A 0.97 . ? C4 H4B 0.97 . ? C5 C6 1.344(15) . ? C5 H5A 0.97 . ? C5 H5B 0.97 . ? C6 H6A 0.97 . ? C6 H6B 0.97 . ? C7 C8 1.518(11) . ? C7 H7A 0.97 . ? C7 H7B 0.97 . ? C8 C9 1.521(12) . ? C8 H8A 0.97 . ? C8 H8B 0.97 . ? C9 C9 1.49(2) 3_655 ? C9 H9A 0.97 . ? C9 H9B 0.97 . ? C10 C11 1.491(11) . ? C10 H10A 0.97 . ? C10 H10B 0.97 . ? C11 C12 1.528(12) 4_666 ? C11 H11A 0.97 . ? C11 H11B 0.97 . ? C12 C12 1.47(2) 3 ? C12 C11 1.529(12) 4_565 ? C12 H12A 0.97 . ? C12 H12B 0.97 . ? OW3A OW3B 1.66(3) . ? OW4A OW4B 0.97(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 O1 Ga1 O2 94.7(2) . . ? O1 Ga1 O3 85.1(2) . . ? O2 Ga1 O3 94.8(2) . . ? O1 Ga1 O4 92.7(2) . . ? O2 Ga1 O4 89.2(2) . . ? O3 Ga1 O4 175.5(2) . . ? O1 Ga1 O5 169.9(2) . . ? O2 Ga1 O5 92.1(2) . . ? O3 Ga1 O5 87.0(2) . . ? O4 Ga1 O5 94.9(2) . . ? O1 Ga1 F1 85.8(2) . . ? O2 Ga1 F1 177.4(2) . . ? O3 Ga1 F1 87.8(2) . . ? O4 Ga1 F1 88.2(2) . . ? O5 Ga1 F1 87.7(2) . . ? O6 Ga2 F2 92.7(2) . 2_645 ? O6 Ga2 O7 179.2(2) . . ? F2 Ga2 O7 87.7(2) 2_645 . ? O6 Ga2 O8 90.9(2) . . ? F2 Ga2 O8 92.4(2) 2_645 . ? O7 Ga2 O8 88.4(2) . . ? O6 Ga2 F1 88.5(2) . . ? F2 Ga2 F1 178.8(2) 2_645 . ? O7 Ga2 F1 91.1(2) . . ? O8 Ga2 F1 87.5(2) . . ? O6 Ga2 O9 90.4(2) . . ? F2 Ga2 O9 87.9(2) 2_645 . ? O7 Ga2 O9 90.3(2) . . ? O8 Ga2 O9 178.6(2) . . ? F1 Ga2 O9 92.1(2) . . ? O10 Ga3 O11 85.2(2) . . ? O10 Ga3 O12 93.9(2) . . ? O11 Ga3 O12 93.4(2) . . ? O10 Ga3 O13 94.1(2) . . ? O11 Ga3 O13 176.3(2) . . ? O12 Ga3 O13 90.3(2) . . ? O10 Ga3 O14 170.0(2) . . ? O11 Ga3 O14 86.4(2) . . ? O12 Ga3 O14 92.1(2) . . ? O13 Ga3 O14 93.9(2) . . ? O10 Ga3 F2 86.2(2) . . ? O11 Ga3 F2 87.1(2) . . ? O12 Ga3 F2 179.5(2) . . ? O13 Ga3 F2 89.2(2) . . ? O14 Ga3 F2 87.9(2) . . ? O12 P1 O9 110.0(3) . . ? O12 P1 O5 111.3(3) . . ? O9 P1 O5 113.3(3) . . ? O12 P1 O15 104.9(3) . . ? O9 P1 O15 108.4(3) . . ? O5 P1 O15 108.5(3) . . ? O7 P2 O4 115.3(3) . . ? O7 P2 O17 108.7(3) . . ? O4 P2 O17 110.6(3) . . ? O7 P2 O18 108.0(3) . . ? O4 P2 O18 107.3(3) . . ? O17 P2 O18 106.5(3) . . ? O16 P3 O13 113.5(3) . . ? O16 P3 O6 111.5(3) . 2_655 ? O13 P3 O6 111.7(3) . 2_655 ? O16 P3 O19 109.0(3) . . ? O13 P3 O19 105.3(3) . . ? O6 P3 O19 105.3(3) 2_655 . ? O8 P4 O2 110.6(3) 2 . ? O8 P4 O14 112.7(3) 2 1_455 ? O2 P4 O14 111.9(3) . 1_455 ? O8 P4 O20 108.8(3) 2 . ? O2 P4 O20 102.3(3) . . ? O14 P4 O20 110.0(3) 1_455 . ? P4 O2 Ga1 140.9(3) . . ? P2 O4 Ga1 133.4(3) . . ? P1 O5 Ga1 132.1(3) . . ? P3 O6 Ga2 131.2(3) 2_645 . ? P2 O7 Ga2 130.1(3) . . ? P4 O8 Ga2 135.6(3) 2_545 . ? P1 O9 Ga2 134.6(3) . . ? P1 O12 Ga3 139.5(3) . . ? P3 O13 Ga3 134.3(3) . . ? P4 O14 Ga3 133.4(3) 1_655 . ? Ga2 F1 Ga1 133.0(2) . . ? Ga2 F2 Ga3 131.6(2) 2_655 . ? C1 N1 H1A 109.5(4) . . ? C1 N1 H1B 109.5(5) . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5(5) . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C6 N2 H2A 109.5(6) . . ? C6 N2 H2B 109.5(6) . . ? H2A N2 H2B 109.5 . . ? C6 N2 H2C 109.5(6) . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C7 N3 H3A 109.5(4) . . ? C7 N3 H3B 109.5(4) . . ? H3A N3 H3B 109.5 . . ? C7 N3 H3C 109.5(4) . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? C10 N4 H4A 109.5(4) . . ? C10 N4 H4B 109.5(4) . . ? H4A N4 H4B 109.5 . . ? C10 N4 H4C 109.5(4) . . ? H4A N4 H4C 109.5 . . ? H4B N4 H4C 109.5 . . ? C2 C1 N1 114.0(8) . . ? C2 C1 H1A 108.8(5) . . ? N1 C1 H1A 108.8(5) . . ? C2 C1 H1B 108.8(5) . . ? N1 C1 H1B 108.8(5) . . ? H1A C1 H1B 107.7 . . ? C1 C2 C3 113.2(9) . . ? C1 C2 H2A 108.9(5) . . ? C3 C2 H2A 108.9(7) . . ? C1 C2 H2B 108.9(5) . . ? C3 C2 H2B 108.9(7) . . ? H2A C2 H2B 107.7 . . ? C4 C3 C2 121.7(11) 4_666 . ? C4 C3 H3A 106.9(8) 4_666 . ? C2 C3 H3A 106.9(7) . . ? C4 C3 H3B 106.9(7) 4_666 . ? C2 C3 H3B 106.9(7) . . ? H3A C3 H3B 106.7 . . ? C3 C4 C5 121.6(11) 4_565 . ? C3 C4 H4A 106.9(8) 4_565 . ? C5 C4 H4A 106.9(7) . . ? C3 C4 H4B 106.9(7) 4_565 . ? C5 C4 H4B 106.9(7) . . ? H4A C4 H4B 106.7 . . ? C6 C5 C4 125.7(12) . . ? C6 C5 H5A 105.9(9) . . ? C4 C5 H5A 105.9(7) . . ? C6 C5 H5B 105.9(9) . . ? C4 C5 H5B 105.9(7) . . ? H5A C5 H5B 106.2 . . ? C5 C6 N2 122.6(12) . . ? C5 C6 H6A 106.7(9) . . ? N2 C6 H6A 106.7(6) . . ? C5 C6 H6B 106.7(9) . . ? N2 C6 H6B 106.7(6) . . ? H6A C6 H6B 106.6 . . ? N3 C7 C8 110.1(6) . . ? N3 C7 H7A 109.6(4) . . ? C8 C7 H7A 109.6(4) . . ? N3 C7 H7B 109.6(4) . . ? C8 C7 H7B 109.6(5) . . ? H7A C7 H7B 108.2 . . ? C7 C8 C9 112.0(8) . . ? C7 C8 H8A 109.2(4) . . ? C9 C8 H8A 109.2(5) . . ? C7 C8 H8B 109.2(5) . . ? C9 C8 H8B 109.2(6) . . ? H8A C8 H8B 107.9 . . ? C9 C9 C8 113.6(10) 3_655 . ? C9 C9 H9A 108.9(8) 3_655 . ? C8 C9 H9A 108.9(6) . . ? C9 C9 H9B 108.9(10) 3_655 . ? C8 C9 H9B 108.9(6) . . ? H9A C9 H9B 107.7 . . ? N4 C10 C11 113.2(6) . . ? N4 C10 H10A 108.9(4) . . ? C11 C10 H10A 108.9(5) . . ? N4 C10 H10B 108.9(4) . . ? C11 C10 H10B 108.9(5) . . ? H10A C10 H10B 107.8 . . ? C10 C11 C12 112.0(8) . 4_666 ? C10 C11 H11A 109.2(5) . . ? C12 C11 H11A 109.2(5) 4_666 . ? C10 C11 H11B 109.2(5) . . ? C12 C11 H11B 109.2(6) 4_666 . ? H11A C11 H11B 107.9 . . ? C12 C12 C11 113.7(10) 3 4_565 ? C12 C12 H12A 108.8(9) 3 . ? C11 C12 H12A 108.8(6) 4_565 . ? C12 C12 H12B 108.8(8) 3 . ? C11 C12 H12B 108.8(5) 4_565 . ? H12A C12 H12B 107.7 . . ? _refine_diff_density_max 0.962 _refine_diff_density_min -0.987 _refine_diff_density_rms 0.143