# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Axel Schulz' _publ_contact_author_address ; Department Chemie und Biochemie Ludwig-Maximilians Universitat Butenandtstrase 5-13 (Haus F) D-81377 Munchen Bundesrepublik Deutschland ; loop_ _publ_author_name _publ_author_address 'Alexander Villinger' ; Department Chemie Ludwig-Maximilians Universitat Butenandtstrase 5-13 (Haus F) D-81377 Munchen Bundesrepublik Deutschland ; 'Peter Mayer' ; Department Chemie Ludwig-Maximilians Universitat Butenandtstrase 5-13 (Haus D) D-81377 Munchen Bundesrepublik Deutschland ; 'Axel Schulz' ; Department Chemie Ludwig-Maximilians Universitat Butenandtstrase 5-13 (Haus F) D-81377 Munchen Bundesrepublik Deutschland ; _publ_contact_author_email lex@cup.uni-muenchen.de _publ_contact_author_fax +49-89-2180-77492 _publ_contact_author_phone ? _publ_section_title ; GaCl3 Assisted [2+3] Cycloaddition: A Route to Tetrazaphospholes ; _publ_section_abstract ? _publ_section_comment ? data_jn337 _database_code_depnum_ccdc_archive 'CCDC 292916' _audit_update_record 11-Jan-06 _chemical_name_common ? _chemical_compound_source ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_method 'not measured' _exptl_crystal_density_meas ? _exptl_special_details ? _audit_author_name 'Mayer, P.' _audit_creation_date 01-Sept-05 _diffrn_ambient_temperature 200(2) _diffrn_source_type 'FR 591 generator' _diffrn_source_power 2.200 _diffrn_source_voltage 55.00 _diffrn_source_current 40.00 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation 0.25 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method phi/omega-scan _diffrn_detector_area_resol_mean 9 _diffrn_special_details ? _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_UB_11 -0.0931670 _diffrn_orient_matrix_UB_12 0.0556833 _diffrn_orient_matrix_UB_13 -0.0036717 _diffrn_orient_matrix_UB_21 -0.1220233 _diffrn_orient_matrix_UB_22 -0.0321951 _diffrn_orient_matrix_UB_23 0.0338472 _diffrn_orient_matrix_UB_31 0.0644571 _diffrn_orient_matrix_UB_32 0.0195370 _diffrn_orient_matrix_UB_33 0.0662417 loop_ _reflns_scale_group_code _reflns_scale_meas_F 1 1.0 _cell_length_a 6.0103(2) _cell_length_b 14.8760(4) _cell_length_c 13.4368(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.2260(13) _cell_angle_gamma 90.00 _cell_volume 1200.47(6) _cell_measurement_temperature 200(2) #?# in K _cell_measurement_reflns_used 15571 _cell_measurement_theta_min 3.134 _cell_measurement_theta_max 27.485 _cell_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.070000 -1 0 0 0.070000 0 1 0 0.020000 0 -1 0 0.020000 0 0 -1 0.010000 0 0 1 0.010000 _exptl_absorpt_coefficient_mu 1.557 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _diffrn_reflns_number 22291 #xl _diffrn_reflns_av_R_equivalents 0.1193 #xl _diffrn_reflns_av_sigmaI/netI 0.0532 #xl _diffrn_reflns_limit_h_min -7 #xl _diffrn_reflns_limit_h_max 7 #xl _diffrn_reflns_limit_k_min -19 #xl _diffrn_reflns_limit_k_max 17 #xl _diffrn_reflns_limit_l_min -17 #xl _diffrn_reflns_limit_l_max 17 #xl _diffrn_reflns_theta_min 3.33 #xl _diffrn_reflns_theta_max 27.49 #xl _diffrn_measured_fraction_theta_max 0.998 #xl _diffrn_reflns_theta_full 27.49 #xl _diffrn_measured_fraction_theta_full 0.998 #xl _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/m' _symmetry_Int_Tables_number 11 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' 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' P P 0.1023 0.0942 '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' _reflns_number_total 2857 #xl _reflns_number_gt 2213 #xl _reflns_threshold_expression >2sigma(I) #xl _reflns_special_details ? _refine_ls_structure_factor_coef Fsqd #xl _refine_ls_matrix_type full #xl _refine_ls_weighting_scheme calc #xl _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+1.0199P] where P=(Fo^2^+2Fc^2^)/3' #xl _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr #?# mixed --> _refine_special_details _refine_ls_extinction_method none #xl _refine_ls_extinction_coef ? #xl _refine_ls_abs_structure_details ? #xl _refine_ls_abs_structure_Flack ? #xl _refine_ls_number_reflns 2857 #xl _refine_ls_number_parameters 158 #xl _refine_ls_number_restraints 2 #xl _refine_ls_R_factor_all 0.0694 #xl _refine_ls_R_factor_gt 0.0483 #xl _refine_ls_wR_factor_ref 0.1242 #xl _refine_ls_wR_factor_gt 0.1137 #xl _refine_ls_goodness_of_fit_ref 1.092 #xl _refine_ls_restrained_S_all 1.097 #xl _refine_ls_shift/su_max 0.000 #xl _refine_ls_shift/su_mean 0.000 #xl _refine_diff_density_max 0.456 #xl _refine_diff_density_min -0.579 #xl _refine_diff_density_rms 0.079 #xl _refine_special_details ; H with HFIX riding on their parent atoms with U(H)=1.2*U(C) for CH, 1.5*U(C) for CH3 disorder in methyl group described by a split model ; _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution ; A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A. Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for crystal structure determination and refinement; J. Appl. Crystallogr. 1999, 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of Gottingen, 97-2 version)' _computing_molecular_graphics ? _computing_publication_material ? 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 0.92126(8) 0.2500 -0.09545(3) 0.03778(17) Uani 1 2 d S . . Cl1 Cl 0.6365(2) 0.2500 -0.19688(10) 0.0627(4) Uani 1 2 d S . . Cl2 Cl 1.11322(17) 0.37082(7) -0.09707(8) 0.0605(3) Uani 1 1 d . . . P P 0.5165(2) 0.2500 0.06153(8) 0.0403(3) Uani 1 2 d S . . N1 N 0.7797(6) 0.2500 0.0360(3) 0.0383(8) Uani 1 2 d S . . N2 N 0.9225(6) 0.2500 0.1183(3) 0.0442(9) Uani 1 2 d S . . N3 N 0.8170(6) 0.2500 0.1998(3) 0.0429(9) Uani 1 2 d S . . N4 N 0.5937(6) 0.2500 0.1818(2) 0.0317(7) Uani 1 2 d S . . C1 C 0.4513(7) 0.2500 0.2674(3) 0.0297(8) Uani 1 2 d S . . C2 C 0.3889(5) 0.33332(19) 0.3067(2) 0.0305(6) Uani 1 1 d . A . C3 C 0.2605(5) 0.3298(2) 0.3912(2) 0.0327(6) Uani 1 1 d . . . H3 H 0.2151 0.3848 0.4201 0.039 Uiso 1 1 calc R . . C4 C 0.1964(7) 0.2500 0.4347(3) 0.0325(9) Uani 1 2 d S . . C5 C 0.4550(5) 0.4276(2) 0.2668(2) 0.0399(7) Uani 1 1 d D . . C61 C 0.3191(15) 0.5052(5) 0.3097(7) 0.039(2) Uiso 0.431(10) 1 d P A 1 H61A H 0.3335 0.5040 0.3826 0.059 Uiso 0.431(10) 1 calc PR A 1 H61B H 0.1620 0.4983 0.2887 0.059 Uiso 0.431(10) 1 calc PR A 1 H61C H 0.3751 0.5626 0.2853 0.059 Uiso 0.431(10) 1 calc PR A 1 C71 C 0.4557(18) 0.4416(7) 0.1546(7) 0.059(3) Uiso 0.431(10) 1 d P A 1 H71A H 0.4829 0.5051 0.1402 0.088 Uiso 0.431(10) 1 calc PR A 1 H71B H 0.3111 0.4237 0.1246 0.088 Uiso 0.431(10) 1 calc PR A 1 H71C H 0.5734 0.4049 0.1266 0.088 Uiso 0.431(10) 1 calc PR A 1 C81 C 0.6968(9) 0.4483(6) 0.3044(7) 0.048(2) Uiso 0.431(10) 1 d PD A 1 H81A H 0.7962 0.4006 0.2824 0.072 Uiso 0.431(10) 1 calc PR A 1 H81B H 0.7031 0.4512 0.3773 0.072 Uiso 0.431(10) 1 calc PR A 1 H81C H 0.7439 0.5061 0.2772 0.072 Uiso 0.431(10) 1 calc PR A 1 C62 C 0.3912(13) 0.5006(5) 0.3409(6) 0.0507(18) Uiso 0.569(10) 1 d P A 2 H62A H 0.4699 0.4900 0.4051 0.076 Uiso 0.569(10) 1 calc PR A 2 H62B H 0.2302 0.4988 0.3499 0.076 Uiso 0.569(10) 1 calc PR A 2 H62C H 0.4327 0.5597 0.3153 0.076 Uiso 0.569(10) 1 calc PR A 2 C72 C 0.3126(11) 0.4456(4) 0.1704(4) 0.0471(18) Uiso 0.569(10) 1 d PD A 2 H72A H 0.3469 0.5055 0.1448 0.071 Uiso 0.569(10) 1 calc PR A 2 H72B H 0.1543 0.4424 0.1850 0.071 Uiso 0.569(10) 1 calc PR A 2 H72C H 0.3465 0.4002 0.1203 0.071 Uiso 0.569(10) 1 calc PR A 2 C82 C 0.6962(11) 0.4367(5) 0.2460(6) 0.0512(19) Uiso 0.569(10) 1 d P A 2 H82A H 0.7318 0.3978 0.1899 0.077 Uiso 0.569(10) 1 calc PR A 2 H82B H 0.7862 0.4188 0.3051 0.077 Uiso 0.569(10) 1 calc PR A 2 H82C H 0.7289 0.4993 0.2293 0.077 Uiso 0.569(10) 1 calc PR A 2 C9 C 0.0600(8) 0.2500 0.5289(3) 0.0392(10) Uani 1 2 d S . . C10 C 0.1795(18) 0.3118(10) 0.6060(7) 0.090(4) Uani 0.50 1 d P . . H10A H 0.3284 0.2879 0.6225 0.135 Uiso 0.50 1 calc PR . . H10B H 0.0935 0.3143 0.6664 0.135 Uiso 0.50 1 calc PR . . H10C H 0.1925 0.3723 0.5781 0.135 Uiso 0.50 1 calc PR . . C11 C -0.1660(12) 0.2929(7) 0.5046(6) 0.072(3) Uani 0.50 1 d P . . H11A H -0.2493 0.2556 0.4560 0.109 Uiso 0.50 1 calc PR . . H11B H -0.1444 0.3530 0.4768 0.109 Uiso 0.50 1 calc PR . . H11C H -0.2497 0.2977 0.5656 0.109 Uiso 0.50 1 calc PR . . C12 C 0.024(3) 0.1601(7) 0.5718(10) 0.100(5) Uani 0.50 1 d P . . H12A H -0.0644 0.1234 0.5242 0.151 Uiso 0.50 1 calc PR . . H12B H -0.0564 0.1660 0.6336 0.151 Uiso 0.50 1 calc PR . . H12C H 0.1677 0.1310 0.5861 0.151 Uiso 0.50 1 calc PR . . 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 0.0389(3) 0.0464(3) 0.0285(3) 0.000 0.00760(19) 0.000 Cl1 0.0482(7) 0.0986(11) 0.0409(7) 0.000 -0.0023(5) 0.000 Cl2 0.0676(6) 0.0532(6) 0.0611(6) 0.0127(4) 0.0063(5) -0.0127(5) P 0.0348(6) 0.0584(8) 0.0277(6) 0.000 0.0026(4) 0.000 N1 0.037(2) 0.049(2) 0.0296(18) 0.000 0.0033(15) 0.000 N2 0.039(2) 0.063(3) 0.0312(19) 0.000 0.0088(16) 0.000 N3 0.0319(19) 0.065(3) 0.032(2) 0.000 0.0032(15) 0.000 N4 0.0305(18) 0.0392(19) 0.0257(17) 0.000 0.0038(13) 0.000 C1 0.028(2) 0.036(2) 0.0248(19) 0.000 0.0042(15) 0.000 C2 0.0296(14) 0.0304(15) 0.0315(14) 0.0005(11) 0.0022(11) -0.0019(11) C3 0.0323(15) 0.0325(15) 0.0337(15) -0.0039(12) 0.0041(12) 0.0012(12) C4 0.030(2) 0.041(2) 0.027(2) 0.000 0.0038(16) 0.000 C5 0.0478(18) 0.0291(15) 0.0436(18) 0.0029(13) 0.0092(14) -0.0028(13) C9 0.039(2) 0.052(3) 0.028(2) 0.000 0.0081(17) 0.000 C10 0.068(6) 0.171(12) 0.033(4) -0.031(6) 0.020(4) -0.047(7) C11 0.041(4) 0.130(9) 0.048(4) -0.005(4) 0.017(3) 0.013(4) C12 0.147(11) 0.062(6) 0.100(9) 0.028(6) 0.096(9) 0.014(7) 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 N1 1.990(4) . ? Ga Cl2 2.1363(10) . ? Ga Cl2 2.1363(10) 4_565 ? Ga Cl1 2.1459(14) . ? P N1 1.631(4) . ? P N4 1.664(3) . ? N1 N2 1.374(5) . ? N2 N3 1.286(5) . ? N3 N4 1.355(5) . ? N4 C1 1.460(5) . ? C1 C2 1.404(3) . ? C1 C2 1.404(3) 4_565 ? C2 C3 1.398(4) . ? C2 C5 1.559(4) . ? C3 C4 1.385(4) . ? C3 H3 0.9500 . ? C4 C3 1.385(4) 4_565 ? C4 C9 1.535(6) . ? C5 C82 1.493(7) . ? C5 C71 1.522(10) . ? C5 C62 1.532(8) . ? C5 C61 1.539(9) . ? C5 C72 1.548(4) . ? C5 C81 1.551(5) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C9 C12 1.476(10) 4_565 ? C9 C12 1.476(10) . ? C9 C11 1.525(9) 4_565 ? C9 C11 1.525(9) . ? C9 C10 1.541(10) . ? C9 C10 1.541(10) 4_565 ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 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 N1 Ga Cl2 105.00(6) . . ? N1 Ga Cl2 105.00(6) . 4_565 ? Cl2 Ga Cl2 114.56(6) . 4_565 ? N1 Ga Cl1 101.87(11) . . ? Cl2 Ga Cl1 114.28(3) . . ? Cl2 Ga Cl1 114.28(3) 4_565 . ? N1 P N4 88.19(18) . . ? N2 N1 P 114.3(3) . . ? N2 N1 Ga 116.1(3) . . ? P N1 Ga 129.7(2) . . ? N3 N2 N1 111.8(4) . . ? N2 N3 N4 111.5(3) . . ? N3 N4 C1 117.8(3) . . ? N3 N4 P 114.2(3) . . ? C1 N4 P 128.0(3) . . ? C2 C1 C2 123.9(3) . 4_565 ? C2 C1 N4 118.03(17) . . ? C2 C1 N4 118.03(17) 4_565 . ? C3 C2 C1 115.9(3) . . ? C3 C2 C5 118.0(3) . . ? C1 C2 C5 126.1(3) . . ? C4 C3 C2 123.1(3) . . ? C4 C3 H3 118.4 . . ? C2 C3 H3 118.4 . . ? C3 C4 C3 118.0(4) 4_565 . ? C3 C4 C9 120.97(18) 4_565 . ? C3 C4 C9 120.97(18) . . ? C82 C5 C71 76.3(5) . . ? C82 C5 C62 109.1(4) . . ? C71 C5 C62 123.9(5) . . ? C82 C5 C61 122.4(5) . . ? C71 C5 C61 106.9(5) . . ? C62 C5 C61 22.4(3) . . ? C82 C5 C72 109.7(4) . . ? C71 C5 C72 33.9(4) . . ? C62 C5 C72 106.1(4) . . ? C61 C5 C72 84.3(5) . . ? C82 C5 C81 30.5(3) . . ? C71 C5 C81 104.9(5) . . ? C62 C5 C81 84.4(5) . . ? C61 C5 C81 103.5(5) . . ? C72 C5 C81 136.0(5) . . ? C82 C5 C2 114.1(3) . . ? C71 C5 C2 118.3(4) . . ? C62 C5 C2 109.9(3) . . ? C61 C5 C2 113.5(4) . . ? C72 C5 C2 107.6(3) . . ? C81 C5 C2 108.3(4) . . ? C5 C61 H61A 109.5 . . ? C5 C61 H61B 109.5 . . ? C5 C61 H61C 109.5 . . ? C5 C71 H71A 109.5 . . ? C5 C71 H71B 109.5 . . ? C5 C71 H71C 109.5 . . ? C5 C81 H81A 109.5 . . ? C5 C81 H81B 109.5 . . ? C5 C81 H81C 109.5 . . ? C5 C62 H62A 109.5 . . ? C5 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C5 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C5 C72 H72A 109.5 . . ? C5 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C5 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C5 C82 H82A 109.5 . . ? C5 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C5 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C12 C9 C12 130.0(9) 4_565 . ? C12 C9 C11 108.6(8) 4_565 4_565 ? C12 C9 C11 63.9(8) . 4_565 ? C12 C9 C11 63.9(7) 4_565 . ? C12 C9 C11 108.6(8) . . ? C11 C9 C11 49.5(8) 4_565 . ? C12 C9 C4 114.4(4) 4_565 . ? C12 C9 C4 114.4(4) . . ? C11 C9 C4 108.9(4) 4_565 . ? C11 C9 C4 108.9(4) . . ? C12 C9 C10 43.1(7) 4_565 . ? C12 C9 C10 110.5(10) . . ? C11 C9 C10 141.4(6) 4_565 . ? C11 C9 C10 106.4(7) . . ? C4 C9 C10 107.7(4) . . ? C12 C9 C10 110.5(10) 4_565 4_565 ? C12 C9 C10 43.1(7) . 4_565 ? C11 C9 C10 106.4(7) 4_565 4_565 ? C11 C9 C10 141.4(6) . 4_565 ? C4 C9 C10 107.7(4) . 4_565 ? C10 C9 C10 73.2(12) . 4_565 ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 P N1 N2 0.0 . . . . ? N4 P N1 Ga 180.0 . . . . ? Cl2 Ga N1 N2 -60.57(4) . . . . ? Cl2 Ga N1 N2 60.57(4) 4_565 . . . ? Cl1 Ga N1 N2 180.0 . . . . ? Cl2 Ga N1 P 119.43(4) . . . . ? Cl2 Ga N1 P -119.43(4) 4_565 . . . ? Cl1 Ga N1 P 0.0 . . . . ? P N1 N2 N3 0.0 . . . . ? Ga N1 N2 N3 180.0 . . . . ? N1 N2 N3 N4 0.0 . . . . ? N2 N3 N4 C1 180.0 . . . . ? N2 N3 N4 P 0.0 . . . . ? N1 P N4 N3 0.0 . . . . ? N1 P N4 C1 180.0 . . . . ? N3 N4 C1 C2 89.3(3) . . . . ? P N4 C1 C2 -90.7(3) . . . . ? N3 N4 C1 C2 -89.3(3) . . . 4_565 ? P N4 C1 C2 90.7(3) . . . 4_565 ? C2 C1 C2 C3 1.2(6) 4_565 . . . ? N4 C1 C2 C3 -177.4(3) . . . . ? C2 C1 C2 C5 179.4(2) 4_565 . . . ? N4 C1 C2 C5 0.8(5) . . . . ? C1 C2 C3 C4 -0.1(5) . . . . ? C5 C2 C3 C4 -178.4(3) . . . . ? C2 C3 C4 C3 -1.0(6) . . . 4_565 ? C2 C3 C4 C9 178.5(3) . . . . ? C3 C2 C5 C82 131.5(4) . . . . ? C1 C2 C5 C82 -46.6(5) . . . . ? C3 C2 C5 C71 -141.6(5) . . . . ? C1 C2 C5 C71 40.2(6) . . . . ? C3 C2 C5 C62 8.7(5) . . . . ? C1 C2 C5 C62 -169.5(5) . . . . ? C3 C2 C5 C61 -15.1(6) . . . . ? C1 C2 C5 C61 166.8(5) . . . . ? C3 C2 C5 C72 -106.5(4) . . . . ? C1 C2 C5 C72 75.4(5) . . . . ? C3 C2 C5 C81 99.3(5) . . . . ? C1 C2 C5 C81 -78.8(5) . . . . ? C3 C4 C9 C12 174.3(8) 4_565 . . 4_565 ? C3 C4 C9 C12 -5.2(10) . . . 4_565 ? C3 C4 C9 C12 5.2(10) 4_565 . . . ? C3 C4 C9 C12 -174.3(8) . . . . ? C3 C4 C9 C11 -64.0(6) 4_565 . . 4_565 ? C3 C4 C9 C11 116.5(5) . . . 4_565 ? C3 C4 C9 C11 -116.5(5) 4_565 . . . ? C3 C4 C9 C11 64.0(6) . . . . ? C3 C4 C9 C10 128.5(7) 4_565 . . . ? C3 C4 C9 C10 -51.0(8) . . . . ? C3 C4 C9 C10 51.0(8) 4_565 . . 4_565 ? C3 C4 C9 C10 -128.5(7) . . . 4_565 ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag ? ? ? ? ? ? ? ? ? _geom_special_details ? _audit_block_code PN4C18H29_GaCl3_jn337_schulz _audit_creation_method 'form98_non/compatible with shelxl97-2' _chemical_name_systematic ? _chemical_formula_moiety 'N4 P Ga Cl3 C18 H29' _chemical_formula_sum 'C18 H29 Cl3 Ga N4 P' _chemical_formula_weight 508.505 _chemical_melting_point ? #?# in K! _cell_formula_units_Z 2 #?# adjust to _chemical_formula_[] _exptl_crystal_density_diffrn 1.40679(7) _exptl_crystal_F_000 524