# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1856 data_global # 1. SUBMISSION DETAILS _publ_contact_author ; Prof. Dr. H. Schmidbaur, Dr. A. Schier Anorganisch-chemisches Institut der Technischen Universit\"at M\"unchen Lichtenbergstra\"se 4 D-85747 Garching Germany ; _publ_contact_author_phone '++49 89 2891-3130' _publ_contact_author_fax '++49 89 2891-3125' _publ_contact_author_email 'Annette.Schier@lrz.tum.de' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; please consider this CIF submission for publication in "J. Chem. Soc., Dalton Trans." Date of submission: November 1999. ; #============================================================================ # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================ # 3. TITLE AND AUTHOR LIST _publ_section_title ; Isomerism of Dimeric cis-Ethene-1,2-di(alkylamido)gallium Hydrides and Chlorides ; loop_ _publ_author_name _publ_author_address 'E.S. Schmidt' ; Anorganisch-chemisches Institut der Technischen Universit\"at M\"unchen Lichtenbergstra\"se 4 D-85747 Garching Germany ; 'A. Jockisch' ; Anorganisch-chemisches Institut der Technischen Universit\"at M\"unchen Lichtenbergstra\"se 4 D-85747 Garching Germany ; 'Hubert Schmidbaur' ; Anorganisch-chemisches Institut der Technischen Universit\"at M\"unchen Lichtenbergstra\"se 4 D-85747 Garching Germany ; #============================================================================== data_EVA1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H40 Cl2 Ga2 N4' _chemical_formula_weight 546.90 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' '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 61.445(13) _cell_length_b 10.4410(10) _cell_length_c 29.371(10) _cell_angle_alpha 90.00 _cell_angle_beta 101.450(10) _cell_angle_gamma 90.00 _cell_volume 18468(8) _cell_formula_units_Z 28 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 17 _cell_measurement_theta_max 25 _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7952 _exptl_absorpt_coefficient_mu 2.257 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Enraf Nonius CAD4' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600s _diffrn_standards_decay_% ? _diffrn_reflns_number 16523 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0695 _diffrn_reflns_limit_h_min -72 _diffrn_reflns_limit_h_max 71 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 24.98 _reflns_number_total 16188 _reflns_number_gt 10614 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf Nonius CAD4' _computing_cell_refinement 'Enraf Nonius CAD4' _computing_data_reduction CADSHEL _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-PLUS _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0464P)^2^+152.3001P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16188 _refine_ls_number_parameters 911 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1172 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.1436 _refine_ls_wR_factor_gt 0.1286 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 Ga11 Ga 0.219071(12) 0.59869(7) 0.13283(3) 0.03656(18) Uani 1 1 d . . . Ga12 Ga 0.209844(10) 0.86272(6) 0.10500(2) 0.02819(16) Uani 1 1 d . . . Cl11 Cl 0.25153(3) 0.50850(19) 0.15052(8) 0.0620(5) Uani 1 1 d . . . Cl12 Cl 0.19570(4) 0.44771(18) 0.14004(8) 0.0611(5) Uani 1 1 d . . . N11 N 0.21233(8) 0.7569(5) 0.16447(17) 0.0304(12) Uani 1 1 d . . . N12 N 0.18047(8) 0.9040(5) 0.10532(18) 0.0341(12) Uani 1 1 d . . . N13 N 0.21618(8) 0.6964(5) 0.07422(17) 0.0335(12) Uani 1 1 d . . . N14 N 0.23495(8) 0.9399(5) 0.09199(19) 0.0386(13) Uani 1 1 d . . . C11 C 0.18881(11) 0.7525(6) 0.1670(2) 0.0354(15) Uani 1 1 d . . . C12 C 0.17457(11) 0.8262(7) 0.1388(2) 0.0387(16) Uani 1 1 d . . . C13 C 0.23910(11) 0.7262(7) 0.0673(3) 0.0425(17) Uani 1 1 d . . . C14 C 0.24668(11) 0.8433(7) 0.0756(3) 0.0449(18) Uani 1 1 d . . . C111 C 0.22678(10) 0.7971(6) 0.2103(2) 0.0372(15) Uani 1 1 d . . . C112 C 0.25030(11) 0.8199(7) 0.2028(3) 0.0509(19) Uani 1 1 d . . . H11A H 0.2501 0.8859 0.1790 0.076 Uiso 1 1 calc R . . H11B H 0.2562 0.7401 0.1927 0.076 Uiso 1 1 calc R . . H11C H 0.2597 0.8484 0.2320 0.076 Uiso 1 1 calc R . . C113 C 0.21763(12) 0.9221(7) 0.2269(2) 0.0486(18) Uani 1 1 d . . . H11D H 0.2025 0.9076 0.2319 0.073 Uiso 1 1 calc R . . H11E H 0.2174 0.9886 0.2033 0.073 Uiso 1 1 calc R . . H11F H 0.2272 0.9497 0.2560 0.073 Uiso 1 1 calc R . . C114 C 0.22688(13) 0.6943(7) 0.2472(2) 0.054(2) Uani 1 1 d . . . H11G H 0.2117 0.6804 0.2519 0.081 Uiso 1 1 calc R . . H11H H 0.2363 0.7221 0.2765 0.081 Uiso 1 1 calc R . . H11I H 0.2327 0.6142 0.2370 0.081 Uiso 1 1 calc R . . C121 C 0.16506(11) 1.0028(7) 0.0828(3) 0.0451(17) Uani 1 1 d . . . C122 C 0.16394(14) 1.1121(8) 0.1160(3) 0.067(2) Uani 1 1 d . . . H12A H 0.1587 1.0800 0.1433 0.100 Uiso 1 1 calc R . . H12B H 0.1536 1.1776 0.1005 0.100 Uiso 1 1 calc R . . H12C H 0.1787 1.1497 0.1259 0.100 Uiso 1 1 calc R . . C123 C 0.17278(13) 1.0498(8) 0.0403(3) 0.065(2) Uani 1 1 d . . . H12D H 0.1735 0.9776 0.0193 0.097 Uiso 1 1 calc R . . H12E H 0.1875 1.0884 0.0495 0.097 Uiso 1 1 calc R . . H12F H 0.1623 1.1139 0.0244 0.097 Uiso 1 1 calc R . . C124 C 0.14156(12) 0.9454(9) 0.0669(3) 0.070(3) Uani 1 1 d . . . H12G H 0.1361 0.9147 0.0941 0.106 Uiso 1 1 calc R . . H12H H 0.1422 0.8738 0.0457 0.106 Uiso 1 1 calc R . . H12I H 0.1315 1.0114 0.0510 0.106 Uiso 1 1 calc R . . C131 C 0.20166(12) 0.6445(7) 0.0297(2) 0.0449(17) Uani 1 1 d . . . C132 C 0.17783(11) 0.6357(7) 0.0369(2) 0.0508(19) Uani 1 1 d . . . H13A H 0.1771 0.5760 0.0623 0.076 Uiso 1 1 calc R . . H13B H 0.1682 0.6049 0.0083 0.076 Uiso 1 1 calc R . . H13C H 0.1728 0.7206 0.0447 0.076 Uiso 1 1 calc R . . C133 C 0.20285(14) 0.7370(8) -0.0096(3) 0.061(2) Uani 1 1 d . . . H13D H 0.2182 0.7423 -0.0142 0.091 Uiso 1 1 calc R . . H13E H 0.1979 0.8220 -0.0018 0.091 Uiso 1 1 calc R . . H13F H 0.1932 0.7064 -0.0383 0.091 Uiso 1 1 calc R . . C134 C 0.21012(15) 0.5119(8) 0.0190(3) 0.069(2) Uani 1 1 d . . . H13G H 0.2254 0.5192 0.0142 0.103 Uiso 1 1 calc R . . H13H H 0.2006 0.4778 -0.0092 0.103 Uiso 1 1 calc R . . H13I H 0.2097 0.4541 0.0451 0.103 Uiso 1 1 calc R . . C141 C 0.24246(12) 1.0736(7) 0.0909(3) 0.0467(18) Uani 1 1 d . . . C142 C 0.23801(15) 1.1238(9) 0.0409(3) 0.073(3) Uani 1 1 d . . . H14A H 0.2462 1.0717 0.0222 0.110 Uiso 1 1 calc R . . H14B H 0.2429 1.2131 0.0408 0.110 Uiso 1 1 calc R . . H14C H 0.2221 1.1188 0.0278 0.110 Uiso 1 1 calc R . . C143 C 0.26759(12) 1.0856(8) 0.1115(3) 0.075(3) Uani 1 1 d . . . H14D H 0.2760 1.0360 0.0925 0.112 Uiso 1 1 calc R . . H14E H 0.2707 1.0525 0.1433 0.112 Uiso 1 1 calc R . . H14F H 0.2720 1.1758 0.1117 0.112 Uiso 1 1 calc R . . C144 C 0.23011(12) 1.1517(7) 0.1208(3) 0.055(2) Uani 1 1 d . . . H14G H 0.2330 1.1169 0.1524 0.082 Uiso 1 1 calc R . . H14H H 0.2141 1.1479 0.1078 0.082 Uiso 1 1 calc R . . H14I H 0.2351 1.2408 0.1215 0.082 Uiso 1 1 calc R . . H11 H 0.1853(8) 0.699(5) 0.1893(18) 0.016(14) Uiso 1 1 d . . . H12 H 0.1593(10) 0.825(5) 0.1393(19) 0.030(16) Uiso 1 1 d . . . H13 H 0.2463(9) 0.653(6) 0.0578(19) 0.024(15) Uiso 1 1 d . . . H14 H 0.2601(13) 0.861(8) 0.075(3) 0.07(3) Uiso 1 1 d . . . Ga21 Ga 0.145773(15) 0.37963(7) 0.33423(3) 0.0499(2) Uani 1 1 d . . . Ga22 Ga 0.146815(11) 0.10866(7) 0.31406(2) 0.03311(17) Uani 1 1 d . . . Cl21 Cl 0.16338(4) 0.47540(19) 0.39680(8) 0.0759(7) Uani 1 1 d . . . Cl22 Cl 0.12771(5) 0.5329(2) 0.29346(9) 0.0899(8) Uani 1 1 d . . . N21 N 0.16553(12) 0.2665(6) 0.3059(2) 0.0616(19) Uani 1 1 d . . . N22 N 0.16870(12) 0.0296(6) 0.3567(3) 0.076(2) Uani 1 1 d . . . N23 N 0.12756(9) 0.2320(5) 0.3418(2) 0.0502(16) Uani 1 1 d . . . N24 N 0.12597(9) 0.0679(5) 0.2621(2) 0.0473(15) Uani 1 1 d . . . C21 C 0.18742(15) 0.2412(8) 0.3453(3) 0.069(3) Uani 1 1 d . . . H21 H 0.1991 0.3013 0.3540 0.082 Uiso 1 1 calc R . . C22 C 0.18696(15) 0.1189(9) 0.3651(3) 0.077(3) Uani 1 1 d . . . H22 H 0.2000 0.0924 0.3861 0.093 Uiso 1 1 calc R . . C23 C 0.10811(17) 0.2428(9) 0.2983(3) 0.082(3) Uani 1 1 d . . . H23 H 0.0966 0.3040 0.2971 0.098 Uiso 1 1 calc R . . C24 C 0.10845(15) 0.1620(10) 0.2628(4) 0.080(3) Uani 1 1 d . . . H24 H 0.0966 0.1664 0.2367 0.096 Uiso 1 1 calc R . . C211 C 0.17522(15) 0.3043(8) 0.2672(4) 0.072(3) Uani 1 1 d . . . C212 C 0.15295(17) 0.3191(11) 0.2270(3) 0.100(4) Uani 1 1 d . . . H21A H 0.1452 0.2368 0.2225 0.150 Uiso 1 1 calc R . . H21B H 0.1571 0.3456 0.1979 0.150 Uiso 1 1 calc R . . H21C H 0.1432 0.3838 0.2365 0.150 Uiso 1 1 calc R . . C213 C 0.18681(14) 0.4301(8) 0.2728(3) 0.064(2) Uani 1 1 d . . . H21D H 0.1770 0.4948 0.2822 0.096 Uiso 1 1 calc R . . H21E H 0.1907 0.4553 0.2433 0.096 Uiso 1 1 calc R . . H21F H 0.2004 0.4229 0.2968 0.096 Uiso 1 1 calc R . . C214 C 0.18913(12) 0.1988(8) 0.2525(3) 0.062(2) Uani 1 1 d . . . H21G H 0.1807 0.1187 0.2490 0.093 Uiso 1 1 calc R . . H21H H 0.2027 0.1879 0.2761 0.093 Uiso 1 1 calc R . . H21I H 0.1931 0.2214 0.2227 0.093 Uiso 1 1 calc R . . C221 C 0.17440(13) -0.0995(7) 0.3718(3) 0.061(2) Uani 1 1 d . . . C222 C 0.18661(16) -0.1699(9) 0.3384(3) 0.081(3) Uani 1 1 d . . . H22A H 0.1773 -0.1701 0.3071 0.121 Uiso 1 1 calc R . . H22B H 0.1896 -0.2583 0.3490 0.121 Uiso 1 1 calc R . . H22C H 0.2007 -0.1261 0.3377 0.121 Uiso 1 1 calc R . . C223 C 0.15208(18) -0.1679(9) 0.3679(4) 0.104(4) Uani 1 1 d . . . H22D H 0.1438 -0.1633 0.3358 0.156 Uiso 1 1 calc R . . H22E H 0.1435 -0.1264 0.3885 0.156 Uiso 1 1 calc R . . H22F H 0.1547 -0.2578 0.3770 0.156 Uiso 1 1 calc R . . C224 C 0.1876(2) -0.1031(12) 0.4196(3) 0.154(7) Uani 1 1 d . . . H22G H 0.1796 -0.0577 0.4404 0.231 Uiso 1 1 calc R . . H22H H 0.2020 -0.0616 0.4204 0.231 Uiso 1 1 calc R . . H22I H 0.1900 -0.1923 0.4297 0.231 Uiso 1 1 calc R . . C231 C 0.1178(2) 0.2104(9) 0.3817(4) 0.100(4) Uani 1 1 d . . . C232 C 0.10123(15) 0.0959(8) 0.3751(3) 0.075(3) Uani 1 1 d . . . H23A H 0.0882 0.1177 0.3513 0.112 Uiso 1 1 calc R . . H23B H 0.0966 0.0778 0.4045 0.112 Uiso 1 1 calc R . . H23C H 0.1085 0.0201 0.3652 0.112 Uiso 1 1 calc R . . C233 C 0.13897(17) 0.1818(9) 0.4188(4) 0.092(3) Uani 1 1 d . . . H23D H 0.1463 0.1052 0.4097 0.138 Uiso 1 1 calc R . . H23E H 0.1349 0.1672 0.4490 0.138 Uiso 1 1 calc R . . H23F H 0.1491 0.2549 0.4211 0.138 Uiso 1 1 calc R . . C234 C 0.10484(18) 0.3290(11) 0.3920(4) 0.098(3) Uiso 1 1 d . . . H23G H 0.0919 0.3412 0.3670 0.147 Uiso 1 1 calc R . . H23H H 0.1145 0.4045 0.3942 0.147 Uiso 1 1 calc R . . H23I H 0.0999 0.3169 0.4215 0.147 Uiso 1 1 calc R . . C241 C 0.12038(13) -0.0434(8) 0.2314(3) 0.061(2) Uani 1 1 d . . . C242 C 0.14115(14) -0.1171(9) 0.2298(3) 0.078(3) Uani 1 1 d . . . H24A H 0.1521 -0.0599 0.2203 0.117 Uiso 1 1 calc R . . H24B H 0.1377 -0.1873 0.2073 0.117 Uiso 1 1 calc R . . H24C H 0.1472 -0.1522 0.2606 0.117 Uiso 1 1 calc R . . C243 C 0.1044(2) -0.1263(11) 0.2464(6) 0.173(8) Uani 1 1 d . . . H24D H 0.0908 -0.0777 0.2473 0.260 Uiso 1 1 calc R . . H24E H 0.1106 -0.1594 0.2775 0.260 Uiso 1 1 calc R . . H24F H 0.1008 -0.1979 0.2247 0.260 Uiso 1 1 calc R . . C244 C 0.11147(19) 0.0098(12) 0.1805(3) 0.112(4) Uani 1 1 d . . . H24G H 0.1227 0.0654 0.1714 0.168 Uiso 1 1 calc R . . H24H H 0.0978 0.0589 0.1799 0.168 Uiso 1 1 calc R . . H24I H 0.1083 -0.0620 0.1587 0.168 Uiso 1 1 calc R . . Ga31 Ga 0.075036(12) 0.67935(7) 0.04599(3) 0.03881(19) Uani 1 1 d . . . Ga32 Ga 0.073897(11) 0.40821(7) 0.02430(3) 0.03527(18) Uani 1 1 d . . . Cl31 Cl 0.06402(3) 0.77436(17) 0.10321(7) 0.0566(5) Uani 1 1 d . . . Cl32 Cl 0.08742(3) 0.83259(17) 0.00787(7) 0.0560(5) Uani 1 1 d . . . N31 N 0.09647(8) 0.5362(5) 0.05896(19) 0.0384(13) Uani 1 1 d . . . N32 N 0.09194(8) 0.3749(5) -0.01845(19) 0.0406(13) Uani 1 1 d . . . N33 N 0.05239(8) 0.5590(5) 0.01288(19) 0.0361(13) Uani 1 1 d . . . N34 N 0.05583(9) 0.3218(5) 0.0578(2) 0.0473(15) Uani 1 1 d . . . C31 C 0.11127(11) 0.5448(7) 0.0255(3) 0.0444(18) Uani 1 1 d . . . C32 C 0.10882(11) 0.4635(7) -0.0097(3) 0.0459(18) Uani 1 1 d . . . C33 C 0.03793(12) 0.5246(7) 0.0450(3) 0.0451(18) Uani 1 1 d . . . C34 C 0.03987(12) 0.4088(7) 0.0649(3) 0.0471(18) Uani 1 1 d . . . C311 C 0.10956(11) 0.5114(7) 0.1078(3) 0.0487(19) Uani 1 1 d . . . C312 C 0.09332(13) 0.4853(8) 0.1396(3) 0.058(2) Uani 1 1 d . . . H31A H 0.0839 0.4119 0.1278 0.087 Uiso 1 1 calc R . . H31B H 0.0840 0.5609 0.1406 0.087 Uiso 1 1 calc R . . H31C H 0.1016 0.4663 0.1710 0.087 Uiso 1 1 calc R . . C313 C 0.12436(12) 0.3931(7) 0.1059(3) 0.061(2) Uani 1 1 d . . . H31D H 0.1348 0.4109 0.0854 0.092 Uiso 1 1 calc R . . H31E H 0.1150 0.3197 0.0939 0.092 Uiso 1 1 calc R . . H31F H 0.1326 0.3736 0.1372 0.092 Uiso 1 1 calc R . . C314 C 0.12395(14) 0.6256(8) 0.1254(3) 0.069(2) Uani 1 1 d . . . H31G H 0.1343 0.6418 0.1047 0.103 Uiso 1 1 calc R . . H31H H 0.1323 0.6079 0.1568 0.103 Uiso 1 1 calc R . . H31I H 0.1145 0.7011 0.1261 0.103 Uiso 1 1 calc R . . C321 C 0.09350(12) 0.2691(7) -0.0507(2) 0.0453(18) Uani 1 1 d . . . C322 C 0.07238(12) 0.1922(8) -0.0578(3) 0.061(2) Uani 1 1 d . . . H32A H 0.0701 0.1602 -0.0277 0.091 Uiso 1 1 calc R . . H32B H 0.0735 0.1196 -0.0784 0.091 Uiso 1 1 calc R . . H32C H 0.0598 0.2465 -0.0718 0.091 Uiso 1 1 calc R . . C323 C 0.09668(16) 0.3183(8) -0.0974(3) 0.072(3) Uani 1 1 d . . . H32D H 0.1103 0.3694 -0.0933 0.108 Uiso 1 1 calc R . . H32E H 0.0840 0.3717 -0.1112 0.108 Uiso 1 1 calc R . . H32F H 0.0978 0.2457 -0.1180 0.108 Uiso 1 1 calc R . . C324 C 0.11321(13) 0.1828(8) -0.0298(3) 0.065(2) Uani 1 1 d . . . H32G H 0.1270 0.2327 -0.0254 0.097 Uiso 1 1 calc R . . H32H H 0.1141 0.1113 -0.0509 0.097 Uiso 1 1 calc R . . H32I H 0.1111 0.1495 0.0002 0.097 Uiso 1 1 calc R . . C331 C 0.03870(11) 0.5931(7) -0.0347(2) 0.0441(17) Uani 1 1 d . . . C332 C 0.05441(12) 0.6133(8) -0.0680(3) 0.0542(19) Uani 1 1 d . . . H33A H 0.0644 0.6852 -0.0571 0.081 Uiso 1 1 calc R . . H33B H 0.0458 0.6323 -0.0990 0.081 Uiso 1 1 calc R . . H33C H 0.0632 0.5355 -0.0691 0.081 Uiso 1 1 calc R . . C333 C 0.02330(12) 0.4815(8) -0.0514(3) 0.059(2) Uani 1 1 d . . . H33D H 0.0131 0.4687 -0.0300 0.089 Uiso 1 1 calc R . . H33E H 0.0321 0.4036 -0.0525 0.089 Uiso 1 1 calc R . . H33F H 0.0147 0.5001 -0.0826 0.089 Uiso 1 1 calc R . . C334 C 0.02534(13) 0.7147(8) -0.0323(3) 0.065(2) Uani 1 1 d . . . H33G H 0.0355 0.7859 -0.0217 0.097 Uiso 1 1 calc R . . H33H H 0.0154 0.7023 -0.0104 0.097 Uiso 1 1 calc R . . H33I H 0.0166 0.7343 -0.0632 0.097 Uiso 1 1 calc R . . C341 C 0.05470(13) 0.1889(7) 0.0735(3) 0.056(2) Uani 1 1 d . . . C342 C 0.07730(12) 0.1264(7) 0.0741(3) 0.058(2) Uani 1 1 d . . . H34A H 0.0888 0.1718 0.0962 0.087 Uiso 1 1 calc R . . H34B H 0.0808 0.1307 0.0430 0.087 Uiso 1 1 calc R . . H34C H 0.0768 0.0366 0.0836 0.087 Uiso 1 1 calc R . . C343 C 0.03680(14) 0.1151(8) 0.0394(4) 0.079(3) Uani 1 1 d . . . H34D H 0.0223 0.1546 0.0386 0.119 Uiso 1 1 calc R . . H34E H 0.0365 0.0258 0.0495 0.119 Uiso 1 1 calc R . . H34F H 0.0403 0.1178 0.0083 0.119 Uiso 1 1 calc R . . C344 C 0.04973(16) 0.1804(8) 0.1223(3) 0.079(3) Uani 1 1 d . . . H34G H 0.0353 0.2196 0.1225 0.119 Uiso 1 1 calc R . . H34H H 0.0613 0.2260 0.1441 0.119 Uiso 1 1 calc R . . H34I H 0.0495 0.0904 0.1315 0.119 Uiso 1 1 calc R . . H31 H 0.1216(13) 0.607(8) 0.029(3) 0.07(3) Uiso 1 1 d . . . H32 H 0.1184(10) 0.470(6) -0.032(2) 0.034(17) Uiso 1 1 d . . . H33 H 0.0288(13) 0.576(8) 0.057(3) 0.07(3) Uiso 1 1 d . . . H34 H 0.0322(11) 0.390(6) 0.088(2) 0.04(2) Uiso 1 1 d . . . Ga41 Ga 0.0000 0.43829(11) 0.2500 0.0557(3) Uani 1 2 d S . . Ga42 Ga 0.0000 0.71440(10) 0.2500 0.0439(3) Uani 1 2 d S . . Cl4 Cl 0.00504(5) 0.3131(3) 0.31008(13) 0.1216(13) Uani 1 1 d . . . N41 N 0.02293(9) 0.5711(5) 0.2576(2) 0.0477(15) Uani 1 1 d . . . N42 N 0.01002(12) 0.7758(6) 0.3092(2) 0.069(2) Uani 1 1 d . . . C41 C 0.03218(13) 0.5840(8) 0.3088(3) 0.062(2) Uani 1 1 d . . . H41 H 0.0422 0.5227 0.3252 0.074 Uiso 1 1 calc R . . C42 C 0.02570(16) 0.6851(9) 0.3303(3) 0.078(3) Uani 1 1 d . . . H42 H 0.0321 0.6967 0.3622 0.093 Uiso 1 1 calc R . . C411 C 0.04170(15) 0.5618(10) 0.2323(4) 0.086(3) Uani 1 1 d . . . C412 C 0.03100(18) 0.5700(12) 0.1795(3) 0.103(4) Uani 1 1 d . . . H41A H 0.0204 0.4998 0.1712 0.154 Uiso 1 1 calc R . . H41B H 0.0426 0.5633 0.1611 0.154 Uiso 1 1 calc R . . H41C H 0.0233 0.6521 0.1730 0.154 Uiso 1 1 calc R . . C413 C 0.05427(15) 0.4335(10) 0.2440(4) 0.106(4) Uani 1 1 d . . . H41D H 0.0440 0.3620 0.2354 0.159 Uiso 1 1 calc R . . H41E H 0.0605 0.4299 0.2774 0.159 Uiso 1 1 calc R . . H41F H 0.0663 0.4276 0.2267 0.159 Uiso 1 1 calc R . . C414 C 0.05794(16) 0.6702(11) 0.2459(4) 0.109(4) Uani 1 1 d . . . H41G H 0.0503 0.7522 0.2389 0.163 Uiso 1 1 calc R . . H41H H 0.0699 0.6634 0.2285 0.163 Uiso 1 1 calc R . . H41I H 0.0642 0.6652 0.2793 0.163 Uiso 1 1 calc R . . C421 C 0.00701(17) 0.8954(9) 0.3343(4) 0.088(3) Uani 1 1 d . . . C422 C -0.01327(18) 0.9623(10) 0.3081(5) 0.127(5) Uani 1 1 d . . . H42A H -0.0263 0.9070 0.3067 0.190 Uiso 1 1 calc R . . H42B H -0.0113 0.9815 0.2765 0.190 Uiso 1 1 calc R . . H42C H -0.0155 1.0424 0.3240 0.190 Uiso 1 1 calc R . . C424 C 0.02770(18) 0.9809(10) 0.3363(5) 0.125(5) Uani 1 1 d . . . H42D H 0.0408 0.9367 0.3538 0.187 Uiso 1 1 calc R . . H42E H 0.0256 1.0618 0.3518 0.187 Uiso 1 1 calc R . . H42F H 0.0298 0.9983 0.3047 0.187 Uiso 1 1 calc R . . C423 C 0.0046(2) 0.8706(13) 0.3841(4) 0.131(5) Uani 1 1 d . . . H42G H 0.0180 0.8277 0.4011 0.197 Uiso 1 1 calc R . . H42H H -0.0084 0.8159 0.3841 0.197 Uiso 1 1 calc R . . H42I H 0.0026 0.9522 0.3993 0.197 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 Ga11 0.0375(4) 0.0297(4) 0.0410(4) -0.0005(3) 0.0042(3) 0.0032(3) Ga12 0.0248(3) 0.0301(4) 0.0296(4) 0.0003(3) 0.0054(3) 0.0010(3) Cl11 0.0511(11) 0.0525(11) 0.0765(14) 0.0031(11) -0.0017(10) 0.0237(9) Cl12 0.0728(14) 0.0390(10) 0.0738(14) -0.0002(10) 0.0201(11) -0.0152(9) N11 0.031(3) 0.032(3) 0.027(3) 0.001(2) 0.004(2) 0.002(2) N12 0.025(3) 0.040(3) 0.036(3) 0.003(3) 0.004(2) 0.005(2) N13 0.037(3) 0.031(3) 0.032(3) -0.001(2) 0.006(2) 0.001(2) N14 0.033(3) 0.039(3) 0.046(3) 0.000(3) 0.014(3) -0.003(2) C11 0.037(4) 0.037(4) 0.034(4) 0.005(3) 0.010(3) -0.005(3) C12 0.027(3) 0.046(4) 0.042(4) -0.005(3) 0.005(3) -0.001(3) C13 0.037(4) 0.046(4) 0.048(5) -0.003(4) 0.015(3) 0.009(3) C14 0.024(4) 0.055(5) 0.057(5) 0.002(4) 0.011(3) -0.003(3) C111 0.036(4) 0.044(4) 0.029(4) -0.001(3) -0.001(3) 0.000(3) C112 0.034(4) 0.061(5) 0.051(5) -0.006(4) -0.005(3) -0.002(3) C113 0.052(4) 0.051(4) 0.039(4) -0.010(4) 0.000(3) -0.002(4) C114 0.057(5) 0.056(5) 0.043(4) 0.010(4) -0.005(4) 0.004(4) C121 0.036(4) 0.045(4) 0.055(5) 0.007(4) 0.010(3) 0.014(3) C122 0.070(6) 0.049(5) 0.084(6) -0.005(5) 0.025(5) 0.016(4) C123 0.058(5) 0.070(6) 0.063(6) 0.024(5) 0.005(4) 0.022(4) C124 0.035(4) 0.086(7) 0.085(6) 0.008(5) -0.001(4) 0.011(4) C131 0.049(4) 0.041(4) 0.041(4) -0.014(3) 0.002(3) 0.007(3) C132 0.044(4) 0.056(5) 0.047(4) -0.013(4) -0.006(3) -0.006(4) C133 0.068(5) 0.074(6) 0.038(5) 0.001(4) 0.006(4) 0.005(4) C134 0.087(6) 0.052(5) 0.064(6) -0.026(4) 0.004(5) 0.006(5) C141 0.045(4) 0.040(4) 0.057(5) 0.004(4) 0.016(4) -0.010(3) C142 0.073(6) 0.083(6) 0.068(6) 0.031(5) 0.023(5) 0.001(5) C143 0.045(5) 0.061(5) 0.115(8) 0.005(5) 0.007(5) -0.023(4) C144 0.055(5) 0.035(4) 0.072(5) -0.009(4) 0.008(4) -0.019(3) Ga21 0.0740(6) 0.0294(4) 0.0462(5) 0.0024(4) 0.0113(4) 0.0116(4) Ga22 0.0328(4) 0.0283(4) 0.0362(4) -0.0026(3) 0.0019(3) 0.0031(3) Cl21 0.116(2) 0.0414(11) 0.0652(14) -0.0149(10) 0.0060(13) -0.0048(12) Cl22 0.127(2) 0.0520(13) 0.0877(18) 0.0222(12) 0.0154(16) 0.0412(14) N21 0.102(6) 0.031(3) 0.062(4) 0.007(3) 0.042(4) 0.004(3) N22 0.078(5) 0.027(3) 0.094(6) 0.008(3) -0.051(4) -0.003(3) N23 0.038(3) 0.041(3) 0.072(5) -0.019(3) 0.012(3) 0.003(3) N24 0.048(3) 0.039(3) 0.048(4) -0.005(3) -0.006(3) -0.009(3) C21 0.070(6) 0.061(5) 0.059(6) -0.001(4) -0.023(4) 0.025(5) C22 0.068(6) 0.068(6) 0.087(7) 0.003(5) -0.004(5) 0.015(5) C23 0.102(8) 0.065(6) 0.073(7) -0.009(5) 0.002(6) 0.024(6) C24 0.063(6) 0.083(7) 0.087(7) 0.001(6) 0.002(5) 0.000(5) C211 0.067(6) 0.046(5) 0.114(8) -0.009(5) 0.047(6) -0.015(4) C212 0.097(8) 0.117(9) 0.066(6) -0.029(6) -0.033(6) 0.042(7) C213 0.075(6) 0.055(5) 0.062(5) 0.000(4) 0.015(4) -0.026(4) C214 0.045(4) 0.068(5) 0.077(6) -0.006(5) 0.022(4) -0.008(4) C221 0.048(4) 0.039(4) 0.096(7) 0.023(4) 0.013(4) 0.011(4) C222 0.078(6) 0.072(6) 0.093(7) -0.003(6) 0.020(6) 0.001(5) C223 0.115(9) 0.054(6) 0.168(12) -0.002(7) 0.089(9) 0.003(6) C224 0.258(17) 0.139(11) 0.044(6) 0.005(7) -0.022(8) 0.120(12) C231 0.133(10) 0.051(6) 0.144(11) -0.005(6) 0.095(9) 0.009(6) C232 0.088(7) 0.058(6) 0.087(7) 0.012(5) 0.040(5) -0.009(5) C233 0.098(8) 0.056(6) 0.107(8) 0.003(6) -0.015(7) 0.001(5) C241 0.051(5) 0.066(5) 0.066(6) -0.029(5) 0.011(4) -0.013(4) C242 0.072(6) 0.073(6) 0.094(7) -0.016(6) 0.029(5) 0.010(5) C243 0.138(11) 0.074(8) 0.35(2) -0.093(11) 0.159(14) -0.057(8) C244 0.125(10) 0.123(10) 0.072(7) -0.033(7) -0.020(7) 0.016(8) Ga31 0.0349(4) 0.0310(4) 0.0515(5) -0.0010(3) 0.0107(3) -0.0021(3) Ga32 0.0282(4) 0.0315(4) 0.0463(4) -0.0023(3) 0.0077(3) -0.0006(3) Cl31 0.0675(13) 0.0405(10) 0.0666(13) -0.0091(9) 0.0250(10) -0.0006(9) Cl32 0.0578(11) 0.0397(10) 0.0737(13) 0.0027(9) 0.0206(10) -0.0124(9) N31 0.031(3) 0.035(3) 0.048(3) -0.003(3) 0.004(3) -0.003(2) N32 0.034(3) 0.039(3) 0.049(3) -0.008(3) 0.009(3) 0.004(3) N33 0.028(3) 0.035(3) 0.046(3) 0.001(3) 0.008(2) -0.002(2) N34 0.046(3) 0.035(3) 0.064(4) 0.004(3) 0.019(3) -0.008(3) C31 0.031(4) 0.046(4) 0.057(5) -0.005(4) 0.012(3) -0.004(3) C32 0.032(4) 0.049(5) 0.059(5) 0.005(4) 0.017(4) 0.005(3) C33 0.038(4) 0.041(4) 0.061(5) -0.005(4) 0.020(4) 0.002(3) C34 0.040(4) 0.043(4) 0.064(5) 0.000(4) 0.023(4) -0.005(3) C311 0.034(4) 0.049(4) 0.057(5) -0.005(4) -0.006(3) -0.004(3) C312 0.070(5) 0.061(5) 0.040(4) 0.000(4) 0.002(4) -0.004(4) C313 0.052(5) 0.055(5) 0.065(5) -0.002(4) -0.016(4) 0.016(4) C314 0.064(5) 0.055(5) 0.077(6) -0.021(5) -0.009(5) -0.007(4) C321 0.047(4) 0.041(4) 0.046(4) -0.006(3) 0.005(3) 0.011(3) C322 0.055(5) 0.059(5) 0.065(5) -0.023(4) 0.002(4) 0.003(4) C323 0.098(7) 0.064(6) 0.059(5) -0.013(5) 0.026(5) 0.011(5) C324 0.054(5) 0.060(5) 0.075(6) -0.003(5) 0.000(4) 0.026(4) C331 0.034(4) 0.044(4) 0.053(4) 0.005(4) 0.005(3) 0.008(3) C332 0.049(4) 0.062(5) 0.052(5) 0.009(4) 0.010(4) 0.006(4) C333 0.034(4) 0.071(6) 0.069(6) -0.001(5) 0.003(4) -0.004(4) C334 0.051(5) 0.063(5) 0.080(6) 0.009(5) 0.014(4) 0.023(4) C341 0.061(5) 0.035(4) 0.076(6) 0.003(4) 0.019(4) -0.008(4) C342 0.058(5) 0.036(4) 0.077(6) 0.015(4) 0.008(4) 0.006(4) C343 0.055(5) 0.043(5) 0.136(9) -0.002(5) 0.009(5) -0.013(4) C344 0.101(7) 0.052(5) 0.095(7) 0.018(5) 0.045(6) 0.003(5) Ga41 0.0445(7) 0.0329(6) 0.0875(10) 0.000 0.0081(6) 0.000 Ga42 0.0385(6) 0.0360(6) 0.0522(7) 0.000 -0.0030(5) 0.000 Cl4 0.0884(19) 0.0763(18) 0.188(3) 0.077(2) -0.002(2) -0.0023(15) N41 0.036(3) 0.039(3) 0.068(4) 0.000(3) 0.009(3) 0.000(3) N42 0.080(5) 0.054(4) 0.060(5) -0.013(4) -0.020(4) 0.017(4) C41 0.058(5) 0.054(5) 0.068(6) -0.005(4) -0.001(4) 0.008(4) C42 0.083(7) 0.066(6) 0.072(6) -0.003(5) -0.014(5) -0.001(5) C411 0.052(5) 0.080(7) 0.134(10) -0.003(7) 0.041(6) -0.004(5) C412 0.101(8) 0.141(11) 0.070(7) -0.001(7) 0.029(6) -0.012(8) C413 0.055(6) 0.105(9) 0.161(11) -0.016(8) 0.028(7) 0.034(6) C414 0.056(6) 0.120(10) 0.152(11) 0.007(8) 0.024(7) -0.033(6) C421 0.086(7) 0.064(6) 0.095(8) -0.033(6) -0.026(6) 0.024(5) C422 0.086(8) 0.081(8) 0.187(13) -0.040(8) -0.038(8) 0.023(6) C424 0.099(9) 0.061(7) 0.183(13) -0.022(8) -0.047(9) 0.011(6) C423 0.158(12) 0.134(11) 0.093(9) -0.062(8) 0.002(8) 0.034(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga11 N13 1.979(5) . ? Ga11 N11 1.979(5) . ? Ga11 Cl12 2.171(2) . ? Ga11 Cl11 2.1731(19) . ? Ga11 Ga12 2.8992(10) . ? Ga12 N14 1.846(5) . ? Ga12 N12 1.857(5) . ? Ga12 N13 2.031(5) . ? Ga12 N11 2.047(5) . ? N11 C11 1.462(8) . ? N11 C111 1.518(8) . ? N12 C12 1.380(8) . ? N12 C121 1.466(8) . ? N13 C13 1.495(8) . ? N13 C131 1.527(8) . ? N14 C14 1.381(9) . ? N14 C141 1.473(8) . ? C11 C12 1.325(9) . ? C11 H11 0.92(5) . ? C12 H12 0.94(6) . ? C13 C14 1.314(10) . ? C13 H13 0.95(6) . ? C14 H14 0.85(8) . ? C111 C112 1.523(9) . ? C111 C114 1.524(9) . ? C111 C113 1.538(9) . ? C112 H11A 0.9800 . ? C112 H11B 0.9800 . ? C112 H11C 0.9800 . ? C113 H11D 0.9800 . ? C113 H11E 0.9800 . ? C113 H11F 0.9800 . ? C114 H11G 0.9800 . ? C114 H11H 0.9800 . ? C114 H11I 0.9800 . ? C121 C123 1.502(10) . ? C121 C122 1.513(10) . ? C121 C124 1.547(10) . ? C122 H12A 0.9800 . ? C122 H12B 0.9800 . ? C122 H12C 0.9800 . ? C123 H12D 0.9800 . ? C123 H12E 0.9800 . ? C123 H12F 0.9800 . ? C124 H12G 0.9800 . ? C124 H12H 0.9800 . ? C124 H12I 0.9800 . ? C131 C133 1.520(10) . ? C131 C132 1.523(9) . ? C131 C134 1.533(10) . ? C132 H13A 0.9800 . ? C132 H13B 0.9800 . ? C132 H13C 0.9800 . ? C133 H13D 0.9800 . ? C133 H13E 0.9800 . ? C133 H13F 0.9800 . ? C134 H13G 0.9800 . ? C134 H13H 0.9800 . ? C134 H13I 0.9800 . ? C141 C144 1.509(10) . ? C141 C142 1.530(10) . ? C141 C143 1.548(10) . ? C142 H14A 0.9800 . ? C142 H14B 0.9800 . ? C142 H14C 0.9800 . ? C143 H14D 0.9800 . ? C143 H14E 0.9800 . ? C143 H14F 0.9800 . ? C144 H14G 0.9800 . ? C144 H14H 0.9800 . ? C144 H14I 0.9800 . ? Ga21 N23 1.943(6) . ? Ga21 N21 1.991(6) . ? Ga21 Cl22 2.168(2) . ? Ga21 Cl21 2.182(2) . ? Ga21 Ga22 2.8938(10) . ? Ga22 N24 1.837(5) . ? Ga22 N22 1.842(6) . ? Ga22 N23 2.026(6) . ? Ga22 N21 2.051(6) . ? N21 C211 1.439(10) . ? N21 C21 1.612(10) . ? N22 C221 1.441(9) . ? N22 C22 1.442(11) . ? N23 C231 1.438(11) . ? N23 C23 1.571(11) . ? N24 C24 1.461(11) . ? N24 C241 1.469(9) . ? C21 C22 1.405(12) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.343(12) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C211 C213 1.488(10) . ? C211 C214 1.508(11) . ? C211 C212 1.627(12) . ? C212 H21A 0.9800 . ? C212 H21B 0.9800 . ? C212 H21C 0.9800 . ? C213 H21D 0.9800 . ? C213 H21E 0.9800 . ? C213 H21F 0.9800 . ? C214 H21G 0.9800 . ? C214 H21H 0.9800 . ? C214 H21I 0.9800 . ? C221 C224 1.474(12) . ? C221 C223 1.530(12) . ? C221 C222 1.536(12) . ? C222 H22A 0.9800 . ? C222 H22B 0.9800 . ? C222 H22C 0.9800 . ? C223 H22D 0.9800 . ? C223 H22E 0.9800 . ? C223 H22F 0.9800 . ? C224 H22G 0.9800 . ? C224 H22H 0.9800 . ? C224 H22I 0.9800 . ? C231 C234 1.534(13) . ? C231 C233 1.553(15) . ? C231 C232 1.555(13) . ? C232 H23A 0.9800 . ? C232 H23B 0.9800 . ? C232 H23C 0.9800 . ? C233 H23D 0.9800 . ? C233 H23E 0.9800 . ? C233 H23F 0.9800 . ? C234 H23G 0.9800 . ? C234 H23H 0.9800 . ? C234 H23I 0.9800 . ? C241 C243 1.444(13) . ? C241 C242 1.499(11) . ? C241 C244 1.588(13) . ? C242 H24A 0.9800 . ? C242 H24B 0.9800 . ? C242 H24C 0.9800 . ? C243 H24D 0.9800 . ? C243 H24E 0.9800 . ? C243 H24F 0.9800 . ? C244 H24G 0.9800 . ? C244 H24H 0.9800 . ? C244 H24I 0.9800 . ? Ga31 N31 1.978(5) . ? Ga31 N33 1.981(5) . ? Ga31 Cl31 2.172(2) . ? Ga31 Cl32 2.175(2) . ? Ga31 Ga32 2.8995(10) . ? Ga32 N34 1.858(5) . ? Ga32 N32 1.865(5) . ? Ga32 N33 2.040(5) . ? Ga32 N31 2.046(5) . ? N31 C31 1.468(9) . ? N31 C311 1.521(9) . ? N32 C32 1.375(9) . ? N32 C321 1.471(8) . ? N33 C33 1.463(9) . ? N33 C331 1.524(8) . ? N34 C34 1.383(9) . ? N34 C341 1.468(9) . ? C31 C32 1.324(10) . ? C31 H31 0.90(8) . ? C32 H32 0.97(6) . ? C33 C34 1.339(10) . ? C33 H33 0.90(8) . ? C34 H34 0.91(7) . ? C311 C314 1.513(10) . ? C311 C312 1.521(10) . ? C311 C313 1.541(10) . ? C312 H31A 0.9800 . ? C312 H31B 0.9800 . ? C312 H31C 0.9800 . ? C313 H31D 0.9800 . ? C313 H31E 0.9800 . ? C313 H31F 0.9800 . ? C314 H31G 0.9800 . ? C314 H31H 0.9800 . ? C314 H31I 0.9800 . ? C321 C322 1.506(10) . ? C321 C323 1.512(11) . ? C321 C324 1.536(9) . ? C322 H32A 0.9800 . ? C322 H32B 0.9800 . ? C322 H32C 0.9800 . ? C323 H32D 0.9800 . ? C323 H32E 0.9800 . ? C323 H32F 0.9800 . ? C324 H32G 0.9800 . ? C324 H32H 0.9800 . ? C324 H32I 0.9800 . ? C331 C332 1.517(9) . ? C331 C333 1.520(10) . ? C331 C334 1.522(9) . ? C332 H33A 0.9800 . ? C332 H33B 0.9800 . ? C332 H33C 0.9800 . ? C333 H33D 0.9800 . ? C333 H33E 0.9800 . ? C333 H33F 0.9800 . ? C334 H33G 0.9800 . ? C334 H33H 0.9800 . ? C334 H33I 0.9800 . ? C341 C344 1.524(11) . ? C341 C342 1.531(10) . ? C341 C343 1.540(11) . ? C342 H34A 0.9800 . ? C342 H34B 0.9800 . ? C342 H34C 0.9800 . ? C343 H34D 0.9800 . ? C343 H34E 0.9800 . ? C343 H34F 0.9800 . ? C344 H34G 0.9800 . ? C344 H34H 0.9800 . ? C344 H34I 0.9800 . ? Ga41 N41 1.958(6) . ? Ga41 N41 1.958(6) 2 ? Ga41 Cl4 2.168(3) 2 ? Ga41 Cl4 2.168(3) . ? Ga41 Ga42 2.8829(16) . ? Ga42 N42 1.842(6) . ? Ga42 N42 1.842(6) 2 ? Ga42 N41 2.037(6) . ? Ga42 N41 2.037(6) 2 ? N41 C411 1.493(10) . ? N41 C41 1.506(10) . ? N42 C42 1.404(10) . ? N42 C421 1.479(11) . ? C41 C42 1.330(11) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C411 C414 1.509(13) . ? C411 C413 1.551(13) . ? C411 C412 1.563(14) . ? C412 H41A 0.9800 . ? C412 H41B 0.9800 . ? C412 H41C 0.9800 . ? C413 H41D 0.9800 . ? C413 H41E 0.9800 . ? C413 H41F 0.9800 . ? C414 H41G 0.9800 . ? C414 H41H 0.9800 . ? C414 H41I 0.9800 . ? C421 C422 1.501(13) . ? C421 C423 1.523(15) . ? C421 C424 1.545(15) . ? C422 H42A 0.9800 . ? C422 H42B 0.9800 . ? C422 H42C 0.9800 . ? C424 H42D 0.9800 . ? C424 H42E 0.9800 . ? C424 H42F 0.9800 . ? C423 H42G 0.9800 . ? C423 H42H 0.9800 . ? C423 H42I 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 N13 Ga11 N11 89.3(2) . . ? N13 Ga11 Cl12 120.83(16) . . ? N11 Ga11 Cl12 110.86(16) . . ? N13 Ga11 Cl11 110.55(16) . . ? N11 Ga11 Cl11 121.15(15) . . ? Cl12 Ga11 Cl11 104.80(9) . . ? N13 Ga11 Ga12 44.41(15) . . ? N11 Ga11 Ga12 44.87(14) . . ? Cl12 Ga11 Ga12 128.46(7) . . ? Cl11 Ga11 Ga12 126.75(7) . . ? N14 Ga12 N12 138.8(2) . . ? N14 Ga12 N13 92.2(2) . . ? N12 Ga12 N13 118.2(2) . . ? N14 Ga12 N11 119.2(2) . . ? N12 Ga12 N11 91.7(2) . . ? N13 Ga12 N11 86.0(2) . . ? N14 Ga12 Ga11 110.39(17) . . ? N12 Ga12 Ga11 110.80(16) . . ? N13 Ga12 Ga11 42.98(14) . . ? N11 Ga12 Ga11 43.02(14) . . ? C11 N11 C111 111.9(5) . . ? C11 N11 Ga11 107.4(4) . . ? C111 N11 Ga11 120.5(4) . . ? C11 N11 Ga12 98.9(4) . . ? C111 N11 Ga12 122.7(4) . . ? Ga11 N11 Ga12 92.1(2) . . ? C12 N12 C121 119.9(5) . . ? C12 N12 Ga12 105.1(4) . . ? C121 N12 Ga12 134.6(4) . . ? C13 N13 C131 111.3(5) . . ? C13 N13 Ga11 107.6(4) . . ? C131 N13 Ga11 119.8(4) . . ? C13 N13 Ga12 98.7(4) . . ? C131 N13 Ga12 123.6(4) . . ? Ga11 N13 Ga12 92.6(2) . . ? C14 N14 C141 119.8(6) . . ? C14 N14 Ga12 105.6(4) . . ? C141 N14 Ga12 134.1(4) . . ? C12 C11 N11 119.1(6) . . ? C12 C11 H11 126(3) . . ? N11 C11 H11 115(3) . . ? C11 C12 N12 123.6(6) . . ? C11 C12 H12 121(4) . . ? N12 C12 H12 115(4) . . ? C14 C13 N13 118.5(6) . . ? C14 C13 H13 129(3) . . ? N13 C13 H13 112(3) . . ? C13 C14 N14 123.7(7) . . ? C13 C14 H14 121(6) . . ? N14 C14 H14 115(6) . . ? N11 C111 C112 108.6(5) . . ? N11 C111 C114 110.8(5) . . ? C112 C111 C114 110.1(6) . . ? N11 C111 C113 109.2(5) . . ? C112 C111 C113 109.3(6) . . ? C114 C111 C113 108.9(6) . . ? C111 C112 H11A 109.5 . . ? C111 C112 H11B 109.5 . . ? H11A C112 H11B 109.5 . . ? C111 C112 H11C 109.5 . . ? H11A C112 H11C 109.5 . . ? H11B C112 H11C 109.5 . . ? C111 C113 H11D 109.5 . . ? C111 C113 H11E 109.5 . . ? H11D C113 H11E 109.5 . . ? C111 C113 H11F 109.5 . . ? H11D C113 H11F 109.5 . . ? H11E C113 H11F 109.5 . . ? C111 C114 H11G 109.5 . . ? C111 C114 H11H 109.5 . . ? H11G C114 H11H 109.5 . . ? C111 C114 H11I 109.5 . . ? H11G C114 H11I 109.5 . . ? H11H C114 H11I 109.5 . . ? N12 C121 C123 108.8(5) . . ? N12 C121 C122 110.3(6) . . ? C123 C121 C122 110.6(7) . . ? N12 C121 C124 110.1(6) . . ? C123 C121 C124 107.8(7) . . ? C122 C121 C124 109.1(6) . . ? C121 C122 H12A 109.5 . . ? C121 C122 H12B 109.5 . . ? H12A C122 H12B 109.5 . . ? C121 C122 H12C 109.5 . . ? H12A C122 H12C 109.5 . . ? H12B C122 H12C 109.5 . . ? C121 C123 H12D 109.5 . . ? C121 C123 H12E 109.5 . . ? H12D C123 H12E 109.5 . . ? C121 C123 H12F 109.5 . . ? H12D C123 H12F 109.5 . . ? H12E C123 H12F 109.5 . . ? C121 C124 H12G 109.5 . . ? C121 C124 H12H 109.5 . . ? H12G C124 H12H 109.5 . . ? C121 C124 H12I 109.5 . . ? H12G C124 H12I 109.5 . . ? H12H C124 H12I 109.5 . . ? C133 C131 C132 109.7(6) . . ? C133 C131 N13 108.5(6) . . ? C132 C131 N13 108.5(5) . . ? C133 C131 C134 110.3(6) . . ? C132 C131 C134 110.4(6) . . ? N13 C131 C134 109.4(6) . . ? C131 C132 H13A 109.5 . . ? C131 C132 H13B 109.5 . . ? H13A C132 H13B 109.5 . . ? C131 C132 H13C 109.5 . . ? H13A C132 H13C 109.5 . . ? H13B C132 H13C 109.5 . . ? C131 C133 H13D 109.5 . . ? C131 C133 H13E 109.5 . . ? H13D C133 H13E 109.5 . . ? C131 C133 H13F 109.5 . . ? H13D C133 H13F 109.5 . . ? H13E C133 H13F 109.5 . . ? C131 C134 H13G 109.5 . . ? C131 C134 H13H 109.5 . . ? H13G C134 H13H 109.5 . . ? C131 C134 H13I 109.5 . . ? H13G C134 H13I 109.5 . . ? H13H C134 H13I 109.5 . . ? N14 C141 C144 107.7(5) . . ? N14 C141 C142 110.4(6) . . ? C144 C141 C142 111.0(7) . . ? N14 C141 C143 111.1(6) . . ? C144 C141 C143 107.8(7) . . ? C142 C141 C143 108.8(6) . . ? C141 C142 H14A 109.5 . . ? C141 C142 H14B 109.5 . . ? H14A C142 H14B 109.5 . . ? C141 C142 H14C 109.5 . . ? H14A C142 H14C 109.5 . . ? H14B C142 H14C 109.5 . . ? C141 C143 H14D 109.5 . . ? C141 C143 H14E 109.5 . . ? H14D C143 H14E 109.5 . . ? C141 C143 H14F 109.5 . . ? H14D C143 H14F 109.5 . . ? H14E C143 H14F 109.5 . . ? C141 C144 H14G 109.5 . . ? C141 C144 H14H 109.5 . . ? H14G C144 H14H 109.5 . . ? C141 C144 H14I 109.5 . . ? H14G C144 H14I 109.5 . . ? H14H C144 H14I 109.5 . . ? N23 Ga21 N21 89.4(2) . . ? N23 Ga21 Cl22 113.9(2) . . ? N21 Ga21 Cl22 119.7(2) . . ? N23 Ga21 Cl21 117.9(2) . . ? N21 Ga21 Cl21 112.5(2) . . ? Cl22 Ga21 Cl21 103.94(10) . . ? N23 Ga21 Ga22 44.33(16) . . ? N21 Ga21 Ga22 45.10(18) . . ? Cl22 Ga21 Ga22 129.67(8) . . ? Cl21 Ga21 Ga22 126.38(7) . . ? N24 Ga22 N22 139.1(3) . . ? N24 Ga22 N23 96.6(3) . . ? N22 Ga22 N23 114.6(3) . . ? N24 Ga22 N21 113.8(3) . . ? N22 Ga22 N21 95.1(3) . . ? N23 Ga22 N21 85.5(2) . . ? N24 Ga22 Ga21 110.89(19) . . ? N22 Ga22 Ga21 110.0(2) . . ? N23 Ga22 Ga21 42.08(17) . . ? N21 Ga22 Ga21 43.46(18) . . ? C211 N21 C21 101.2(7) . . ? C211 N21 Ga21 123.4(5) . . ? C21 N21 Ga21 106.7(5) . . ? C211 N21 Ga22 130.0(5) . . ? C21 N21 Ga22 101.0(5) . . ? Ga21 N21 Ga22 91.4(3) . . ? C221 N22 C22 114.8(6) . . ? C221 N22 Ga22 136.8(5) . . ? C22 N22 Ga22 105.3(5) . . ? C231 N23 C23 107.5(8) . . ? C231 N23 Ga21 124.2(6) . . ? C23 N23 Ga21 102.3(5) . . ? C231 N23 Ga22 126.9(6) . . ? C23 N23 Ga22 97.4(5) . . ? Ga21 N23 Ga22 93.6(3) . . ? C24 N24 C241 117.3(6) . . ? C24 N24 Ga22 103.0(5) . . ? C241 N24 Ga22 137.1(5) . . ? C22 C21 N21 111.3(8) . . ? C22 C21 H21 124.3 . . ? N21 C21 H21 124.3 . . ? C21 C22 N22 126.6(8) . . ? C21 C22 H22 116.7 . . ? N22 C22 H22 116.7 . . ? C24 C23 N23 117.3(8) . . ? C24 C23 H23 121.3 . . ? N23 C23 H23 121.3 . . ? C23 C24 N24 124.0(9) . . ? C23 C24 H24 118.0 . . ? N24 C24 H24 118.0 . . ? N21 C211 C213 114.7(8) . . ? N21 C211 C214 111.9(7) . . ? C213 C211 C214 113.0(7) . . ? N21 C211 C212 100.3(7) . . ? C213 C211 C212 108.2(8) . . ? C214 C211 C212 107.7(8) . . ? C211 C212 H21A 109.5 . . ? C211 C212 H21B 109.5 . . ? H21A C212 H21B 109.5 . . ? C211 C212 H21C 109.5 . . ? H21A C212 H21C 109.5 . . ? H21B C212 H21C 109.5 . . ? C211 C213 H21D 109.5 . . ? C211 C213 H21E 109.5 . . ? H21D C213 H21E 109.5 . . ? C211 C213 H21F 109.5 . . ? H21D C213 H21F 109.5 . . ? H21E C213 H21F 109.5 . . ? C211 C214 H21G 109.5 . . ? C211 C214 H21H 109.5 . . ? H21G C214 H21H 109.5 . . ? C211 C214 H21I 109.5 . . ? H21G C214 H21I 109.5 . . ? H21H C214 H21I 109.5 . . ? N22 C221 C224 111.8(8) . . ? N22 C221 C223 104.7(7) . . ? C224 C221 C223 112.0(10) . . ? N22 C221 C222 111.8(8) . . ? C224 C221 C222 110.5(8) . . ? C223 C221 C222 105.8(7) . . ? C221 C222 H22A 109.5 . . ? C221 C222 H22B 109.5 . . ? H22A C222 H22B 109.5 . . ? C221 C222 H22C 109.5 . . ? H22A C222 H22C 109.5 . . ? H22B C222 H22C 109.5 . . ? C221 C223 H22D 109.5 . . ? C221 C223 H22E 109.5 . . ? H22D C223 H22E 109.5 . . ? C221 C223 H22F 109.5 . . ? H22D C223 H22F 109.5 . . ? H22E C223 H22F 109.5 . . ? C221 C224 H22G 109.5 . . ? C221 C224 H22H 109.5 . . ? H22G C224 H22H 109.5 . . ? C221 C224 H22I 109.5 . . ? H22G C224 H22I 109.5 . . ? H22H C224 H22I 109.5 . . ? N23 C231 C234 110.6(8) . . ? N23 C231 C233 100.0(8) . . ? C234 C231 C233 114.3(10) . . ? N23 C231 C232 112.8(9) . . ? C234 C231 C232 107.1(8) . . ? C233 C231 C232 112.1(9) . . ? C231 C232 H23A 109.5 . . ? C231 C232 H23B 109.5 . . ? H23A C232 H23B 109.5 . . ? C231 C232 H23C 109.5 . . ? H23A C232 H23C 109.5 . . ? H23B C232 H23C 109.5 . . ? C231 C233 H23D 109.5 . . ? C231 C233 H23E 109.5 . . ? H23D C233 H23E 109.5 . . ? C231 C233 H23F 109.5 . . ? H23D C233 H23F 109.5 . . ? H23E C233 H23F 109.5 . . ? C231 C234 H23G 109.5 . . ? C231 C234 H23H 109.5 . . ? H23G C234 H23H 109.5 . . ? C231 C234 H23I 109.5 . . ? H23G C234 H23I 109.5 . . ? H23H C234 H23I 109.5 . . ? C243 C241 N24 112.1(8) . . ? C243 C241 C242 109.8(9) . . ? N24 C241 C242 109.2(7) . . ? C243 C241 C244 111.7(10) . . ? N24 C241 C244 107.2(7) . . ? C242 C241 C244 106.6(8) . . ? C241 C242 H24A 109.5 . . ? C241 C242 H24B 109.5 . . ? H24A C242 H24B 109.5 . . ? C241 C242 H24C 109.5 . . ? H24A C242 H24C 109.5 . . ? H24B C242 H24C 109.5 . . ? C241 C243 H24D 109.5 . . ? C241 C243 H24E 109.5 . . ? H24D C243 H24E 109.5 . . ? C241 C243 H24F 109.5 . . ? H24D C243 H24F 109.5 . . ? H24E C243 H24F 109.5 . . ? C241 C244 H24G 109.5 . . ? C241 C244 H24H 109.5 . . ? H24G C244 H24H 109.5 . . ? C241 C244 H24I 109.5 . . ? H24G C244 H24I 109.5 . . ? H24H C244 H24I 109.5 . . ? N31 Ga31 N33 89.5(2) . . ? N31 Ga31 Cl31 119.58(17) . . ? N33 Ga31 Cl31 111.91(16) . . ? N31 Ga31 Cl32 111.55(17) . . ? N33 Ga31 Cl32 119.83(17) . . ? Cl31 Ga31 Cl32 104.89(8) . . ? N31 Ga31 Ga32 44.84(15) . . ? N33 Ga31 Ga32 44.68(15) . . ? Cl31 Ga31 Ga32 128.19(6) . . ? Cl32 Ga31 Ga32 126.93(6) . . ? N34 Ga32 N32 139.8(2) . . ? N34 Ga32 N33 91.5(2) . . ? N32 Ga32 N33 119.0(2) . . ? N34 Ga32 N31 118.1(2) . . ? N32 Ga32 N31 91.3(2) . . ? N33 Ga32 N31 86.0(2) . . ? N34 Ga32 Ga31 110.41(18) . . ? N32 Ga32 Ga31 109.77(17) . . ? N33 Ga32 Ga31 43.04(14) . . ? N31 Ga32 Ga31 42.98(15) . . ? C31 N31 C311 111.1(5) . . ? C31 N31 Ga31 107.6(4) . . ? C311 N31 Ga31 121.2(4) . . ? C31 N31 Ga32 99.0(4) . . ? C311 N31 Ga32 122.5(4) . . ? Ga31 N31 Ga32 92.2(2) . . ? C32 N32 C321 118.8(6) . . ? C32 N32 Ga32 106.0(5) . . ? C321 N32 Ga32 134.2(5) . . ? C33 N33 C331 110.7(5) . . ? C33 N33 Ga31 107.3(4) . . ? C331 N33 Ga31 120.6(4) . . ? C33 N33 Ga32 99.3(4) . . ? C331 N33 Ga32 123.5(4) . . ? Ga31 N33 Ga32 92.3(2) . . ? C34 N34 C341 119.6(6) . . ? C34 N34 Ga32 106.1(5) . . ? C341 N34 Ga32 134.1(5) . . ? C32 C31 N31 119.7(7) . . ? C32 C31 H31 121(5) . . ? N31 C31 H31 120(5) . . ? C31 C32 N32 122.8(7) . . ? C31 C32 H32 120(4) . . ? N32 C32 H32 117(4) . . ? C34 C33 N33 119.4(7) . . ? C34 C33 H33 112(5) . . ? N33 C33 H33 128(5) . . ? C33 C34 N34 122.1(7) . . ? C33 C34 H34 120(4) . . ? N34 C34 H34 117(4) . . ? C314 C311 C312 110.0(7) . . ? C314 C311 N31 110.6(6) . . ? C312 C311 N31 108.7(5) . . ? C314 C311 C313 109.6(6) . . ? C312 C311 C313 110.0(7) . . ? N31 C311 C313 107.9(6) . . ? C311 C312 H31A 109.5 . . ? C311 C312 H31B 109.5 . . ? H31A C312 H31B 109.5 . . ? C311 C312 H31C 109.5 . . ? H31A C312 H31C 109.5 . . ? H31B C312 H31C 109.5 . . ? C311 C313 H31D 109.5 . . ? C311 C313 H31E 109.5 . . ? H31D C313 H31E 109.5 . . ? C311 C313 H31F 109.5 . . ? H31D C313 H31F 109.5 . . ? H31E C313 H31F 109.5 . . ? C311 C314 H31G 109.5 . . ? C311 C314 H31H 109.5 . . ? H31G C314 H31H 109.5 . . ? C311 C314 H31I 109.5 . . ? H31G C314 H31I 109.5 . . ? H31H C314 H31I 109.5 . . ? N32 C321 C322 108.9(6) . . ? N32 C321 C323 111.5(6) . . ? C322 C321 C323 108.7(7) . . ? N32 C321 C324 109.2(6) . . ? C322 C321 C324 109.3(6) . . ? C323 C321 C324 109.2(7) . . ? C321 C322 H32A 109.5 . . ? C321 C322 H32B 109.5 . . ? H32A C322 H32B 109.5 . . ? C321 C322 H32C 109.5 . . ? H32A C322 H32C 109.5 . . ? H32B C322 H32C 109.5 . . ? C321 C323 H32D 109.5 . . ? C321 C323 H32E 109.5 . . ? H32D C323 H32E 109.5 . . ? C321 C323 H32F 109.5 . . ? H32D C323 H32F 109.5 . . ? H32E C323 H32F 109.5 . . ? C321 C324 H32G 109.5 . . ? C321 C324 H32H 109.5 . . ? H32G C324 H32H 109.5 . . ? C321 C324 H32I 109.5 . . ? H32G C324 H32I 109.5 . . ? H32H C324 H32I 109.5 . . ? C332 C331 C333 109.5(6) . . ? C332 C331 C334 109.4(6) . . ? C333 C331 C334 110.4(6) . . ? C332 C331 N33 108.5(5) . . ? C333 C331 N33 108.2(6) . . ? C334 C331 N33 110.9(6) . . ? C331 C332 H33A 109.5 . . ? C331 C332 H33B 109.5 . . ? H33A C332 H33B 109.5 . . ? C331 C332 H33C 109.5 . . ? H33A C332 H33C 109.5 . . ? H33B C332 H33C 109.5 . . ? C331 C333 H33D 109.5 . . ? C331 C333 H33E 109.5 . . ? H33D C333 H33E 109.5 . . ? C331 C333 H33F 109.5 . . ? H33D C333 H33F 109.5 . . ? H33E C333 H33F 109.5 . . ? C331 C334 H33G 109.5 . . ? C331 C334 H33H 109.5 . . ? H33G C334 H33H 109.5 . . ? C331 C334 H33I 109.5 . . ? H33G C334 H33I 109.5 . . ? H33H C334 H33I 109.5 . . ? N34 C341 C344 112.4(7) . . ? N34 C341 C342 107.9(6) . . ? C344 C341 C342 108.4(7) . . ? N34 C341 C343 109.9(7) . . ? C344 C341 C343 109.4(7) . . ? C342 C341 C343 108.8(7) . . ? C341 C342 H34A 109.5 . . ? C341 C342 H34B 109.5 . . ? H34A C342 H34B 109.5 . . ? C341 C342 H34C 109.5 . . ? H34A C342 H34C 109.5 . . ? H34B C342 H34C 109.5 . . ? C341 C343 H34D 109.5 . . ? C341 C343 H34E 109.5 . . ? H34D C343 H34E 109.5 . . ? C341 C343 H34F 109.5 . . ? H34D C343 H34F 109.5 . . ? H34E C343 H34F 109.5 . . ? C341 C344 H34G 109.5 . . ? C341 C344 H34H 109.5 . . ? H34G C344 H34H 109.5 . . ? C341 C344 H34I 109.5 . . ? H34G C344 H34I 109.5 . . ? H34H C344 H34I 109.5 . . ? N41 Ga41 N41 89.8(3) . 2 ? N41 Ga41 Cl4 120.2(2) . 2 ? N41 Ga41 Cl4 110.6(2) 2 2 ? N41 Ga41 Cl4 110.6(2) . . ? N41 Ga41 Cl4 120.2(2) 2 . ? Cl4 Ga41 Cl4 105.8(2) 2 . ? N41 Ga41 Ga42 44.92(16) . . ? N41 Ga41 Ga42 44.92(16) 2 . ? Cl4 Ga41 Ga42 127.08(10) 2 . ? Cl4 Ga41 Ga42 127.08(10) . . ? N42 Ga42 N42 139.3(4) . 2 ? N42 Ga42 N41 93.3(3) . . ? N42 Ga42 N41 116.9(3) 2 . ? N42 Ga42 N41 116.9(3) . 2 ? N42 Ga42 N41 93.3(3) 2 2 ? N41 Ga42 N41 85.4(3) . 2 ? N42 Ga42 Ga41 110.4(2) . . ? N42 Ga42 Ga41 110.4(2) 2 . ? N41 Ga42 Ga41 42.72(16) . . ? N41 Ga42 Ga41 42.72(16) 2 . ? C411 N41 C41 109.1(7) . . ? C411 N41 Ga41 120.5(5) . . ? C41 N41 Ga41 107.3(5) . . ? C411 N41 Ga42 125.4(5) . . ? C41 N41 Ga42 99.1(4) . . ? Ga41 N41 Ga42 92.4(2) . . ? C42 N42 C421 119.6(7) . . ? C42 N42 Ga42 104.6(6) . . ? C421 N42 Ga42 135.4(6) . . ? C42 C41 N41 117.1(7) . . ? C42 C41 H41 121.5 . . ? N41 C41 H41 121.5 . . ? C41 C42 N42 124.8(8) . . ? C41 C42 H42 117.6 . . ? N42 C42 H42 117.6 . . ? N41 C411 C414 110.8(9) . . ? N41 C411 C413 110.2(8) . . ? C414 C411 C413 108.3(8) . . ? N41 C411 C412 106.0(8) . . ? C414 C411 C412 110.4(9) . . ? C413 C411 C412 111.1(10) . . ? C411 C412 H41A 109.5 . . ? C411 C412 H41B 109.5 . . ? H41A C412 H41B 109.5 . . ? C411 C412 H41C 109.5 . . ? H41A C412 H41C 109.5 . . ? H41B C412 H41C 109.5 . . ? C411 C413 H41D 109.5 . . ? C411 C413 H41E 109.5 . . ? H41D C413 H41E 109.5 . . ? C411 C413 H41F 109.5 . . ? H41D C413 H41F 109.5 . . ? H41E C413 H41F 109.5 . . ? C411 C414 H41G 109.5 . . ? C411 C414 H41H 109.5 . . ? H41G C414 H41H 109.5 . . ? C411 C414 H41I 109.5 . . ? H41G C414 H41I 109.5 . . ? H41H C414 H41I 109.5 . . ? N42 C421 C422 108.2(8) . . ? N42 C421 C423 112.3(9) . . ? C422 C421 C423 110.0(10) . . ? N42 C421 C424 108.9(9) . . ? C422 C421 C424 110.1(9) . . ? C423 C421 C424 107.3(9) . . ? C421 C422 H42A 109.5 . . ? C421 C422 H42B 109.5 . . ? H42A C422 H42B 109.5 . . ? C421 C422 H42C 109.5 . . ? H42A C422 H42C 109.5 . . ? H42B C422 H42C 109.5 . . ? C421 C424 H42D 109.5 . . ? C421 C424 H42E 109.5 . . ? H42D C424 H42E 109.5 . . ? C421 C424 H42F 109.5 . . ? H42D C424 H42F 109.5 . . ? H42E C424 H42F 109.5 . . ? C421 C423 H42G 109.5 . . ? C421 C423 H42H 109.5 . . ? H42G C423 H42H 109.5 . . ? C421 C423 H42I 109.5 . . ? H42G C423 H42I 109.5 . . ? H42H C423 H42I 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.300 _refine_diff_density_min -0.887 _refine_diff_density_rms 0.100 data_EVA2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H48 Cl2 Ga2 N4' _chemical_formula_weight 651.04 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' '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 8.140(2) _cell_length_b 8.639(2) _cell_length_c 10.674(2) _cell_angle_alpha 82.15(2) _cell_angle_beta 89.32(2) _cell_angle_gamma 81.16(2) _cell_volume 734.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 17 _cell_measurement_theta_max 25 _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 340 _exptl_absorpt_coefficient_mu 2.040 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Enraf Nonius CAD4' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600s _diffrn_standards_decay_% ? _diffrn_reflns_number 3177 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 27.03 _reflns_number_total 3177 _reflns_number_gt 2826 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf Nonius CAD4' _computing_cell_refinement 'Enraf Nonius CAD4' _computing_data_reduction CADSHEL _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-PLUS _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0545P)^2^+0.2070P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3177 _refine_ls_number_parameters 259 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.0781 _refine_ls_wR_factor_gt 0.0741 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 0.38921(3) 0.43024(2) 0.58966(2) 0.01723(9) Uani 1 1 d . . . Cl Cl 0.21579(7) 0.53650(6) 0.71908(5) 0.02791(13) Uani 1 1 d . . . N1 N 0.6338(2) 0.4464(2) 0.58208(17) 0.0189(3) Uani 1 1 d . . . N2 N 0.4337(2) 0.2104(2) 0.60440(17) 0.0210(4) Uani 1 1 d . . . C1 C 0.7026(3) 0.2822(2) 0.5696(2) 0.0205(4) Uani 1 1 d . . . C2 C 0.6024(3) 0.1717(2) 0.5863(2) 0.0208(4) Uani 1 1 d . . . C11 C 0.7217(3) 0.5017(2) 0.6873(2) 0.0209(4) Uani 1 1 d . . . C12 C 0.6557(3) 0.6733(3) 0.7001(2) 0.0255(5) Uani 1 1 d . . . C13 C 0.7475(3) 0.7288(3) 0.8055(2) 0.0300(5) Uani 1 1 d . . . C14 C 0.7359(4) 0.6252(3) 0.9308(2) 0.0326(5) Uani 1 1 d . . . C15 C 0.7984(4) 0.4527(3) 0.9180(2) 0.0339(6) Uani 1 1 d . . . C16 C 0.7059(3) 0.3977(3) 0.8124(2) 0.0287(5) Uani 1 1 d . . . C21 C 0.3452(3) 0.0897(2) 0.6731(2) 0.0201(4) Uani 1 1 d . . . C22 C 0.3634(3) 0.0802(3) 0.8163(2) 0.0260(5) Uani 1 1 d . . . C23 C 0.2715(3) -0.0465(3) 0.8860(2) 0.0318(5) Uani 1 1 d . . . C24 C 0.0898(3) -0.0195(3) 0.8461(3) 0.0324(5) Uani 1 1 d . . . C25 C 0.0712(3) -0.0092(3) 0.7038(2) 0.0281(5) Uani 1 1 d . . . C26 C 0.1625(3) 0.1188(3) 0.6345(2) 0.0237(4) Uani 1 1 d . . . H1 H 0.814(3) 0.254(3) 0.548(2) 0.021(6) Uiso 1 1 d . . . H2 H 0.643(3) 0.064(4) 0.581(3) 0.026(7) Uiso 1 1 d . . . H11 H 0.841(3) 0.493(3) 0.664(2) 0.018(6) Uiso 1 1 d . . . H121 H 0.669(4) 0.737(4) 0.622(3) 0.036(8) Uiso 1 1 d . . . H122 H 0.548(4) 0.680(4) 0.719(3) 0.041(9) Uiso 1 1 d . . . H131 H 0.858(4) 0.723(4) 0.784(3) 0.035(8) Uiso 1 1 d . . . H132 H 0.704(4) 0.836(4) 0.815(3) 0.042(8) Uiso 1 1 d . . . H141 H 0.793(4) 0.660(4) 0.996(3) 0.037(8) Uiso 1 1 d . . . H142 H 0.617(4) 0.638(4) 0.957(3) 0.044(9) Uiso 1 1 d . . . H151 H 0.784(4) 0.394(4) 0.992(3) 0.048(9) Uiso 1 1 d . . . H152 H 0.913(4) 0.434(4) 0.905(3) 0.037(8) Uiso 1 1 d . . . H161 H 0.751(4) 0.294(4) 0.800(3) 0.029(7) Uiso 1 1 d . . . H162 H 0.590(4) 0.404(4) 0.832(3) 0.036(8) Uiso 1 1 d . . . H21 H 0.396(3) -0.010(3) 0.652(2) 0.015(6) Uiso 1 1 d . . . H221 H 0.321(4) 0.181(3) 0.842(3) 0.025(7) Uiso 1 1 d . . . H222 H 0.477(4) 0.066(3) 0.835(3) 0.031(7) Uiso 1 1 d . . . H231 H 0.278(4) -0.052(4) 0.979(3) 0.045(9) Uiso 1 1 d . . . H232 H 0.322(4) -0.155(4) 0.865(3) 0.038(8) Uiso 1 1 d . . . H241 H 0.039(4) 0.070(4) 0.867(3) 0.037(8) Uiso 1 1 d . . . H242 H 0.032(4) -0.102(4) 0.885(3) 0.033(8) Uiso 1 1 d . . . H251 H -0.036(4) 0.007(4) 0.679(3) 0.038(8) Uiso 1 1 d . . . H252 H 0.120(4) -0.106(4) 0.679(3) 0.032(7) Uiso 1 1 d . . . H261 H 0.156(3) 0.123(3) 0.541(3) 0.028(7) Uiso 1 1 d . . . H262 H 0.112(4) 0.222(3) 0.656(3) 0.028(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga 0.01763(13) 0.01212(12) 0.02119(13) -0.00174(8) 0.00099(8) -0.00043(8) Cl 0.0297(3) 0.0221(3) 0.0305(3) -0.0050(2) 0.0099(2) 0.0010(2) N1 0.0220(8) 0.0128(8) 0.0217(8) -0.0030(6) -0.0024(7) -0.0014(7) N2 0.0208(9) 0.0144(8) 0.0270(9) -0.0007(7) 0.0010(7) -0.0017(7) C1 0.0204(10) 0.0152(9) 0.0243(10) -0.0018(8) -0.0005(8) 0.0015(8) C2 0.0243(10) 0.0148(10) 0.0217(10) -0.0018(7) 0.0007(8) 0.0009(8) C11 0.0218(10) 0.0188(10) 0.0226(10) -0.0029(8) -0.0026(8) -0.0044(8) C12 0.0324(13) 0.0176(10) 0.0259(11) -0.0038(8) -0.0036(9) -0.0012(9) C13 0.0367(14) 0.0232(11) 0.0324(13) -0.0081(9) -0.0033(10) -0.0077(10) C14 0.0398(14) 0.0333(13) 0.0259(12) -0.0089(10) -0.0054(10) -0.0048(11) C15 0.0463(16) 0.0276(12) 0.0269(12) -0.0009(10) -0.0104(11) -0.0046(11) C16 0.0383(14) 0.0230(11) 0.0242(11) 0.0000(9) -0.0043(10) -0.0056(10) C21 0.0231(10) 0.0124(9) 0.0248(10) -0.0021(8) 0.0000(8) -0.0024(8) C22 0.0277(12) 0.0252(11) 0.0257(11) -0.0015(9) -0.0028(9) -0.0072(9) C23 0.0384(14) 0.0306(13) 0.0250(12) 0.0047(9) -0.0010(10) -0.0086(11) C24 0.0340(13) 0.0278(12) 0.0356(13) 0.0004(10) 0.0072(10) -0.0103(11) C25 0.0246(11) 0.0213(11) 0.0387(13) -0.0007(9) -0.0032(10) -0.0068(9) C26 0.0251(11) 0.0186(10) 0.0272(11) 0.0002(8) -0.0017(9) -0.0054(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga N2 1.8633(18) . ? Ga N1 1.9860(18) 2_666 ? Ga N1 2.0169(19) . ? Ga Cl 2.1554(8) . ? Ga Ga 2.8854(8) 2_666 ? N1 C1 1.466(3) . ? N1 C11 1.507(3) . ? N1 Ga 1.9860(18) 2_666 ? N2 C2 1.380(3) . ? N2 C21 1.468(3) . ? C1 C2 1.341(3) . ? C1 H1 0.94(3) . ? C2 H2 0.95(3) . ? C11 C16 1.521(3) . ? C11 C12 1.521(3) . ? C11 H11 1.00(3) . ? C12 C13 1.527(3) . ? C12 H121 0.95(3) . ? C12 H122 0.89(3) . ? C13 C14 1.515(4) . ? C13 H131 0.92(3) . ? C13 H132 0.96(3) . ? C14 C15 1.523(4) . ? C14 H141 0.95(3) . ? C14 H142 1.00(3) . ? C15 C16 1.529(3) . ? C15 H151 0.89(4) . ? C15 H152 0.94(3) . ? C16 H161 0.94(3) . ? C16 H162 0.96(3) . ? C21 C26 1.522(3) . ? C21 C22 1.528(3) . ? C21 H21 0.95(3) . ? C22 C23 1.525(3) . ? C22 H221 0.96(3) . ? C22 H222 0.93(3) . ? C23 C24 1.519(4) . ? C23 H231 0.99(3) . ? C23 H232 1.02(3) . ? C24 C25 1.518(4) . ? C24 H241 0.87(3) . ? C24 H242 0.96(3) . ? C25 C26 1.529(3) . ? C25 H251 0.90(3) . ? C25 H252 0.94(3) . ? C26 H261 0.99(3) . ? C26 H262 0.98(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ga N1 118.68(8) . 2_666 ? N2 Ga N1 91.57(8) . . ? N1 Ga N1 87.76(8) 2_666 . ? N2 Ga Cl 118.39(6) . . ? N1 Ga Cl 111.21(6) 2_666 . ? N1 Ga Cl 124.99(5) . . ? N2 Ga Ga 110.46(6) . 2_666 ? N1 Ga Ga 44.30(5) 2_666 2_666 ? N1 Ga Ga 43.45(5) . 2_666 ? Cl Ga Ga 130.53(2) . 2_666 ? C1 N1 C11 110.14(16) . . ? C1 N1 Ga 108.35(13) . 2_666 ? C11 N1 Ga 121.26(13) . 2_666 ? C1 N1 Ga 100.02(13) . . ? C11 N1 Ga 121.87(14) . . ? Ga N1 Ga 92.24(8) 2_666 . ? C2 N2 C21 118.21(17) . . ? C2 N2 Ga 106.43(14) . . ? C21 N2 Ga 130.52(14) . . ? C2 C1 N1 119.07(19) . . ? C2 C1 H1 119.6(16) . . ? N1 C1 H1 121.4(16) . . ? C1 C2 N2 121.72(19) . . ? C1 C2 H2 121.4(17) . . ? N2 C2 H2 116.7(17) . . ? N1 C11 C16 111.22(17) . . ? N1 C11 C12 111.25(17) . . ? C16 C11 C12 109.95(19) . . ? N1 C11 H11 106.3(14) . . ? C16 C11 H11 109.1(14) . . ? C12 C11 H11 108.9(15) . . ? C11 C12 C13 110.80(19) . . ? C11 C12 H121 109.2(19) . . ? C13 C12 H121 110.1(19) . . ? C11 C12 H122 108(2) . . ? C13 C12 H122 109(2) . . ? H121 C12 H122 109(3) . . ? C14 C13 C12 111.7(2) . . ? C14 C13 H131 108(2) . . ? C12 C13 H131 108(2) . . ? C14 C13 H132 109(2) . . ? C12 C13 H132 111(2) . . ? H131 C13 H132 109(3) . . ? C13 C14 C15 110.5(2) . . ? C13 C14 H141 111.5(19) . . ? C15 C14 H141 111.9(19) . . ? C13 C14 H142 107.8(19) . . ? C15 C14 H142 110(2) . . ? H141 C14 H142 105(3) . . ? C14 C15 C16 111.3(2) . . ? C14 C15 H151 108(2) . . ? C16 C15 H151 110(2) . . ? C14 C15 H152 112(2) . . ? C16 C15 H152 111(2) . . ? H151 C15 H152 104(3) . . ? C11 C16 C15 110.8(2) . . ? C11 C16 H161 106.6(17) . . ? C15 C16 H161 110.8(17) . . ? C11 C16 H162 107.8(19) . . ? C15 C16 H162 109.9(19) . . ? H161 C16 H162 111(3) . . ? N2 C21 C26 110.75(17) . . ? N2 C21 C22 112.21(17) . . ? C26 C21 C22 110.55(19) . . ? N2 C21 H21 107.2(15) . . ? C26 C21 H21 109.4(15) . . ? C22 C21 H21 106.5(15) . . ? C23 C22 C21 111.43(19) . . ? C23 C22 H221 109.7(17) . . ? C21 C22 H221 109.5(17) . . ? C23 C22 H222 114.1(18) . . ? C21 C22 H222 107.6(18) . . ? H221 C22 H222 104(2) . . ? C24 C23 C22 111.1(2) . . ? C24 C23 H231 109(2) . . ? C22 C23 H231 113(2) . . ? C24 C23 H232 107.2(18) . . ? C22 C23 H232 110.0(18) . . ? H231 C23 H232 107(3) . . ? C25 C24 C23 111.4(2) . . ? C25 C24 H241 107(2) . . ? C23 C24 H241 110(2) . . ? C25 C24 H242 108.1(18) . . ? C23 C24 H242 111.9(19) . . ? H241 C24 H242 108(3) . . ? C24 C25 C26 111.3(2) . . ? C24 C25 H251 112(2) . . ? C26 C25 H251 110(2) . . ? C24 C25 H252 108.8(18) . . ? C26 C25 H252 107.2(18) . . ? H251 C25 H252 107(3) . . ? C21 C26 C25 110.74(19) . . ? C21 C26 H261 108.1(17) . . ? C25 C26 H261 111.9(16) . . ? C21 C26 H262 108.8(17) . . ? C25 C26 H262 109.2(17) . . ? H261 C26 H262 108(2) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.03 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.769 _refine_diff_density_min -1.078 _refine_diff_density_rms 0.082 data_EVA6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H42 Ga2 N4' _chemical_formula_weight 478.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 10.077(2) _cell_length_b 9.8180(10) _cell_length_c 12.304(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.160(10) _cell_angle_gamma 90.00 _cell_volume 1198.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13 _cell_measurement_theta_max 16 _exptl_crystal_description 'transparent block ' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504 _exptl_absorpt_coefficient_mu 2.259 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(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 'Enraf-Nonius CAD4 ' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600s _diffrn_standards_decay_% ? _diffrn_reflns_number 4436 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 26.94 _reflns_number_total 2580 _reflns_number_gt 1994 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Software (Enraf-Nonius 1989)' _computing_cell_refinement 'CAD4 Software (Enraf-Nonius 1989)' _computing_data_reduction 'Cadshel 3.1' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-PLUS _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. - Disorder of the molecule, refinement in split positions ; _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^)+(0.0390P)^2^+0.2247P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom (CH), Difmap (GaH)' _refine_ls_hydrogen_treatment 'riding (CH), isotropic (GaH)' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2580 _refine_ls_number_parameters 243 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0770 _refine_ls_wR_factor_gt 0.0710 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.079 _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 0.95004(4) 0.13670(4) 0.46626(3) 0.02965(12) Uani 0.50 1 d P . 1 H11 H 0.995(6) 0.221(7) 0.382(5) 0.07(2) Uiso 0.50 1 d P A 1 N1 N 1.0994(3) 0.0576(3) 0.5775(3) 0.0301(6) Uani 0.50 1 d PD . 1 N2 N 0.8659(7) 0.2018(6) 0.5796(4) 0.0352(12) Uani 0.50 1 d PD B 1 C1 C 1.0465(4) 0.0776(4) 0.6806(3) 0.0337(8) Uani 0.50 1 d P B 1 H1 H 1.0907 0.0384 0.7479 0.051 Uiso 0.50 1 calc PR B 1 C2 C 0.9353(4) 0.1519(4) 0.6774(3) 0.0401(9) Uani 0.50 1 d P B 1 H2 H 0.9036 0.1707 0.7441 0.060 Uiso 0.50 1 calc PR B 1 C11 C 1.2433(7) 0.1109(8) 0.5879(5) 0.0311(16) Uani 0.50 1 d PD C 1 C12 C 1.248(2) 0.2586(12) 0.6275(17) 0.055(5) Uani 0.50 1 d PD C 1 H12A H 1.1861 0.3123 0.5765 0.083 Uiso 0.50 1 calc PR C 1 H12B H 1.3376 0.2937 0.6316 0.083 Uiso 0.50 1 calc PR C 1 H12C H 1.2230 0.2625 0.6992 0.083 Uiso 0.50 1 calc PR C 1 C13 C 1.3408(5) 0.0273(7) 0.6683(5) 0.0432(13) Uani 0.50 1 d PD C 1 H13A H 1.3366 -0.0661 0.6448 0.065 Uiso 0.50 1 calc PR C 1 H13B H 1.3173 0.0335 0.7404 0.065 Uiso 0.50 1 calc PR C 1 H13C H 1.4306 0.0613 0.6708 0.065 Uiso 0.50 1 calc PR C 1 C14 C 1.2822(6) 0.1034(6) 0.4736(4) 0.0506(13) Uani 0.50 1 d PD C 1 H14A H 1.2189 0.1550 0.4221 0.076 Uiso 0.50 1 calc PR C 1 H14B H 1.2812 0.0101 0.4500 0.076 Uiso 0.50 1 calc PR C 1 H14C H 1.3710 0.1404 0.4767 0.076 Uiso 0.50 1 calc PR C 1 C21 C 0.7729(9) 0.3149(10) 0.5815(7) 0.048(4) Uani 0.50 1 d PD B 1 C22 C 0.8456(14) 0.4305(14) 0.6517(12) 0.073(4) Uani 0.50 1 d PD B 1 H22A H 0.9203 0.4614 0.6195 0.110 Uiso 0.50 1 calc PR B 1 H22B H 0.8779 0.3979 0.7252 0.110 Uiso 0.50 1 calc PR B 1 H22C H 0.7841 0.5045 0.6545 0.110 Uiso 0.50 1 calc PR B 1 C23 C 0.6647(7) 0.2863(8) 0.6509(7) 0.0673(19) Uani 0.50 1 d PD B 1 H23A H 0.7067 0.2588 0.7237 0.101 Uiso 0.50 1 calc PR B 1 H23B H 0.6067 0.2148 0.6171 0.101 Uiso 0.50 1 calc PR B 1 H23C H 0.6126 0.3672 0.6556 0.101 Uiso 0.50 1 calc PR B 1 C24 C 0.7103(7) 0.3584(6) 0.4653(5) 0.0592(14) Uani 0.50 1 d PD B 1 H24A H 0.7803 0.3745 0.4231 0.089 Uiso 0.50 1 calc PR B 1 H24B H 0.6594 0.4404 0.4686 0.089 Uiso 0.50 1 calc PR B 1 H24C H 0.6518 0.2877 0.4309 0.089 Uiso 0.50 1 calc PR B 1 Ga2 Ga 0.94990(4) 0.06399(4) 0.59276(3) 0.03265(13) Uani 0.50 1 d P . 2 H21 H 0.975(5) 0.021(5) 0.718(4) 0.054(13) Uiso 0.50 1 d P D 2 N3 N 1.0934(3) 0.1044(3) 0.5020(3) 0.0329(7) Uani 0.50 1 d PD . 2 N4 N 0.8527(7) 0.2228(6) 0.5379(4) 0.0382(13) Uani 0.50 1 d PD E 2 C3 C 1.0306(5) 0.2159(4) 0.4330(4) 0.0373(9) Uani 0.50 1 d P E 2 H3 H 1.0701 0.2494 0.3736 0.056 Uiso 0.50 1 calc PR E 2 C4 C 0.9169(4) 0.2698(4) 0.4548(3) 0.0387(9) Uani 0.50 1 d P E 2 H4 H 0.8780 0.3443 0.4111 0.058 Uiso 0.50 1 calc PR E 2 C31 C 1.2351(8) 0.1399(9) 0.5589(6) 0.0364(16) Uani 0.50 1 d PD F 2 C32 C 1.231(2) 0.2678(12) 0.6268(15) 0.045(3) Uani 0.50 1 d P F 2 H32A H 1.1953 0.3415 0.5791 0.067 Uiso 0.50 1 calc PR F 2 H32B H 1.3201 0.2900 0.6636 0.067 Uiso 0.50 1 calc PR F 2 H32C H 1.1739 0.2529 0.6806 0.067 Uiso 0.50 1 calc PR F 2 C33 C 1.2903(6) 0.0240(7) 0.6349(5) 0.0471(14) Uani 0.50 1 d PD F 2 H33A H 1.2338 0.0106 0.6891 0.071 Uiso 0.50 1 calc PR F 2 H33B H 1.3801 0.0458 0.6712 0.071 Uiso 0.50 1 calc PR F 2 H33C H 1.2921 -0.0578 0.5925 0.071 Uiso 0.50 1 calc PR F 2 C34 C 1.3241(5) 0.1637(7) 0.4726(5) 0.0590(15) Uani 0.50 1 d PD F 2 H34A H 1.2877 0.2370 0.4248 0.089 Uiso 0.50 1 calc PR F 2 H34B H 1.3271 0.0823 0.4298 0.089 Uiso 0.50 1 calc PR F 2 H34C H 1.4136 0.1868 0.5088 0.089 Uiso 0.50 1 calc PR F 2 C41 C 0.7664(8) 0.3184(9) 0.5912(7) 0.048(4) Uani 0.50 1 d PD E 2 C42 C 0.8555(11) 0.4409(13) 0.6346(13) 0.090(5) Uani 0.50 1 d PD E 2 H42A H 0.8879 0.4840 0.5743 0.134 Uiso 0.50 1 calc PR E 2 H42B H 0.9306 0.4102 0.6881 0.134 Uiso 0.50 1 calc PR E 2 H42C H 0.8034 0.5050 0.6684 0.134 Uiso 0.50 1 calc PR E 2 C43 C 0.6980(7) 0.2255(7) 0.6654(7) 0.0611(17) Uani 0.50 1 d PD E 2 H43A H 0.7648 0.1896 0.7237 0.092 Uiso 0.50 1 calc PR E 2 H43B H 0.6536 0.1518 0.6224 0.092 Uiso 0.50 1 calc PR E 2 H43C H 0.6330 0.2771 0.6966 0.092 Uiso 0.50 1 calc PR E 2 C44 C 0.6548(7) 0.3717(7) 0.4995(6) 0.076(2) Uani 0.50 1 d PD E 2 H44A H 0.6938 0.4303 0.4512 0.114 Uiso 0.50 1 calc PR E 2 H44B H 0.5899 0.4218 0.5319 0.114 Uiso 0.50 1 calc PR E 2 H44C H 0.6112 0.2963 0.4582 0.114 Uiso 0.50 1 calc PR E 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 0.0302(2) 0.0286(2) 0.0287(2) 0.00512(16) 0.00127(15) -0.00308(16) N1 0.0302(15) 0.0292(15) 0.0295(16) 0.0031(14) 0.0016(13) -0.0030(12) N2 0.033(2) 0.028(3) 0.043(3) 0.007(2) 0.002(3) 0.0026(18) C1 0.036(2) 0.0369(18) 0.0265(18) 0.0005(15) -0.0003(15) -0.0026(16) C2 0.039(2) 0.045(2) 0.037(2) -0.0032(19) 0.0091(17) -0.0015(18) C11 0.031(3) 0.032(4) 0.028(3) 0.008(3) -0.002(2) -0.009(2) C12 0.048(6) 0.052(7) 0.065(8) 0.013(5) 0.006(5) 0.000(4) C13 0.032(3) 0.042(3) 0.051(3) 0.007(3) -0.007(2) 0.000(2) C14 0.038(3) 0.062(3) 0.053(3) 0.010(3) 0.012(2) -0.016(2) C21 0.050(7) 0.048(7) 0.049(5) -0.015(4) 0.017(5) -0.012(5) C22 0.074(7) 0.051(5) 0.106(7) -0.017(5) 0.049(6) -0.014(4) C23 0.046(3) 0.083(5) 0.075(4) -0.007(4) 0.017(3) 0.016(3) C24 0.064(4) 0.048(3) 0.065(4) 0.000(3) 0.009(3) 0.019(3) Ga2 0.0367(2) 0.0272(2) 0.0332(2) 0.00608(17) 0.00392(17) -0.00509(16) N3 0.0381(17) 0.0264(14) 0.0327(17) 0.0045(14) 0.0016(14) -0.0042(12) N4 0.040(2) 0.022(2) 0.050(4) 0.014(2) 0.001(3) 0.0038(17) C3 0.052(3) 0.0239(17) 0.035(2) 0.0121(17) 0.0048(19) -0.0079(17) C4 0.045(2) 0.0300(18) 0.038(2) 0.0063(17) -0.0009(17) -0.0048(16) C31 0.033(2) 0.036(4) 0.036(4) 0.010(3) -0.005(3) -0.006(2) C32 0.045(5) 0.025(4) 0.056(6) -0.005(4) -0.017(4) -0.018(4) C33 0.039(4) 0.047(3) 0.049(4) 0.003(3) -0.008(2) 0.001(3) C34 0.043(3) 0.079(4) 0.056(3) 0.003(3) 0.010(2) -0.022(3) C41 0.039(6) 0.035(6) 0.067(6) 0.009(4) 0.004(5) 0.017(4) C42 0.061(6) 0.051(6) 0.137(10) -0.044(6) -0.035(7) 0.016(4) C43 0.056(4) 0.056(4) 0.077(4) 0.000(3) 0.027(3) 0.006(3) C44 0.061(4) 0.069(4) 0.101(6) 0.028(4) 0.023(4) 0.022(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 N2 1.867(6) . ? Ga1 N1 2.004(3) . ? Ga1 N1 2.021(3) 3_756 ? Ga1 Ga1 2.9349(8) 3_756 ? Ga1 H11 1.46(6) . ? N1 C1 1.473(5) . ? N1 C11 1.526(8) . ? N1 Ga1 2.021(3) 3_756 ? N2 C2 1.372(6) . ? N2 C21 1.457(10) . ? C1 C2 1.331(6) . ? C1 H1 0.9500 . ? C1 H21 1.08(5) . ? C2 H2 0.9500 . ? C2 H21 1.41(5) . ? C11 C13 1.508(6) . ? C11 C14 1.527(6) . ? C11 C12 1.527(8) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C21 C24 1.518(6) . ? C21 C23 1.525(6) . ? C21 C22 1.532(7) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? Ga2 N4 1.901(6) . ? Ga2 N3 2.016(3) . ? Ga2 N3 2.026(3) 3_756 ? Ga2 Ga2 2.9364(9) 3_756 ? Ga2 H21 1.58(5) . ? N3 C3 1.460(5) . ? N3 C31 1.516(9) . ? N3 Ga2 2.026(3) 3_756 ? N4 C4 1.382(7) . ? N4 C41 1.506(10) . ? C3 C4 1.332(6) . ? C3 H11 0.66(6) . ? C3 H3 0.9500 . ? C4 H11 1.37(6) . ? C4 H4 0.9500 . ? C31 C32 1.512(12) . ? C31 C33 1.515(6) . ? C31 C34 1.525(6) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C41 C43 1.537(6) . ? C41 C44 1.537(6) . ? C41 C42 1.540(6) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ga1 N1 90.44(18) . . ? N2 Ga1 N1 113.5(2) . 3_756 ? N1 Ga1 N1 86.35(12) . 3_756 ? N2 Ga1 Ga1 106.26(16) . 3_756 ? N1 Ga1 Ga1 43.40(8) . 3_756 ? N1 Ga1 Ga1 42.95(9) 3_756 3_756 ? N2 Ga1 H11 125(3) . . ? N1 Ga1 H11 115(2) . . ? N1 Ga1 H11 116(2) 3_756 . ? Ga1 Ga1 H11 126(3) 3_756 . ? C1 N1 C11 111.4(4) . . ? C1 N1 Ga1 101.2(2) . . ? C11 N1 Ga1 120.8(3) . . ? C1 N1 Ga1 104.2(2) . 3_756 ? C11 N1 Ga1 122.2(3) . 3_756 ? Ga1 N1 Ga1 93.65(12) . 3_756 ? C2 N2 C21 119.2(5) . . ? C2 N2 Ga1 107.7(4) . . ? C21 N2 Ga1 130.7(4) . . ? C2 C1 N1 118.6(3) . . ? C2 C1 H1 120.7 . . ? N1 C1 H1 120.7 . . ? C2 C1 H21 71(3) . . ? N1 C1 H21 132(3) . . ? H1 C1 H21 70.3 . . ? C1 C2 N2 121.2(4) . . ? C1 C2 H2 119.4 . . ? N2 C2 H2 119.4 . . ? C1 C2 H21 46.1(19) . . ? N2 C2 H21 134.9(19) . . ? H2 C2 H21 89.3 . . ? C13 C11 N1 111.6(5) . . ? C13 C11 C14 109.6(6) . . ? N1 C11 C14 107.5(5) . . ? C13 C11 C12 109.1(10) . . ? N1 C11 C12 109.1(9) . . ? C14 C11 C12 110.0(9) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C21 C24 111.1(6) . . ? N2 C21 C23 113.2(7) . . ? C24 C21 C23 111.1(7) . . ? N2 C21 C22 109.2(9) . . ? C24 C21 C22 113.6(9) . . ? C23 C21 C22 98.0(8) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N4 Ga2 N3 91.0(2) . . ? N4 Ga2 N3 114.8(2) . 3_756 ? N3 Ga2 N3 86.80(12) . 3_756 ? N4 Ga2 Ga2 107.54(19) . 3_756 ? N3 Ga2 Ga2 43.53(9) . 3_756 ? N3 Ga2 Ga2 43.26(9) 3_756 3_756 ? N4 Ga2 H21 123.4(18) . . ? N3 Ga2 H21 126.0(17) . . ? N3 Ga2 H21 109.0(18) 3_756 . ? Ga2 Ga2 H21 128.9(17) 3_756 . ? C3 N3 C31 111.9(4) . . ? C3 N3 Ga2 101.0(2) . . ? C31 N3 Ga2 119.9(3) . . ? C3 N3 Ga2 104.5(2) . 3_756 ? C31 N3 Ga2 122.9(4) . 3_756 ? Ga2 N3 Ga2 93.20(12) . 3_756 ? C4 N4 C41 119.7(5) . . ? C4 N4 Ga2 104.9(4) . . ? C41 N4 Ga2 131.1(4) . . ? C4 C3 N3 118.7(4) . . ? C4 C3 H11 79(6) . . ? N3 C3 H11 136(6) . . ? C4 C3 H3 120.6 . . ? N3 C3 H3 120.6 . . ? H11 C3 H3 59.0 . . ? C3 C4 N4 123.2(4) . . ? C3 C4 H11 28(2) . . ? N4 C4 H11 139(3) . . ? C3 C4 H4 118.4 . . ? N4 C4 H4 118.4 . . ? H11 C4 H4 97.2 . . ? C32 C31 C33 109.1(9) . . ? C32 C31 N3 109.2(9) . . ? C33 C31 N3 109.0(6) . . ? C32 C31 C34 109.6(9) . . ? C33 C31 C34 110.3(6) . . ? N3 C31 C34 109.6(5) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N4 C41 C43 104.1(6) . . ? N4 C41 C44 107.3(7) . . ? C43 C41 C44 107.0(6) . . ? N4 C41 C42 107.0(8) . . ? C43 C41 C42 123.5(9) . . ? C44 C41 C42 107.1(7) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.94 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.266 _refine_diff_density_min -0.210 _refine_diff_density_rms 0.046