# ic990553e.cif _manuscript_identification_# IC990553E _publ_requested_journal 'Inorganic Chemistry' _publ_requested_coeditor_name ' ' _publ_section_title ; Ring Opening of Dilithio Bis(amido)cyclodiphosphazanes as a Route to 1,3,-Diaza-2eta-phosphaallyl Gallkium Complexes ; _publ_author_names I.Schranz, D.F. Moser, L. Stahl, R.J. Staples data_ls27_COMPOUND_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H34 Cl Ga N4 P2' _chemical_formula_weight 449.58 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.5478(6) _cell_length_b 11.9540(7) _cell_length_c 10.1501(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.808(1) _cell_angle_gamma 90.00 _cell_volume 1147.7(1) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 31 _cell_measurement_theta_min 3.15 _cell_measurement_theta_max 19.67 _exptl_crystal_description chunk _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 1.461 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.815741 _exptl_absorpt_correction_T_max 0.962326 _exptl_special_details ; Data was collected using a Siemens SMART CCD (charge coupled device) based diffractometer equipped with an LT-2 low-temperature apparatus operating at 213 K. A suitable crystal was chosen and mounted on a glass fiber using grease. Data were measured using omega scans of 0.3\% per frame for 30 seconds, such that a hemisphere was collected. A total of 1271 frames were collected with a final resolution of 0.75 \%A. The first 50 frames were recollected at the end of data collection to monitor for decay. Cell parameters were retrieved using SMART software and refined using SAINT on all observed reflections. Data reduction was performed using the SAINT software which corrects for Lp and decay. Absorption corrections were applied using SADABS supplied by George Sheldrick. The structures are solved by the direct method using the SHELX-90 program and refined by least squares method on F2 SHELXL-97, incorporated in SHELXTL-PC V 5.03. ; _diffrn_ambient_temperature 213(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 ? _diffrn_measurement_method '\w, 0.3 deg' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 7546 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 28.29 _reflns_number_total 2895 _reflns_number_gt 2246 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'ASTRO (SIEMENS, V4.033, 1994)' _computing_cell_refinement 'SMART (SIEMENS, V4.033, 1994)' _computing_data_reduction 'SAINT (SIEMENS, V4.035, 1994)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (SIEMENS, 1994, ver 5.04)' _computing_publication_material 'CIFTAB (Sheldrick, 1993)' _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 w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+0.4440P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2895 _refine_ls_number_parameters 121 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0591 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0871 _refine_ls_wR_factor_gt 0.0781 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.21916(4) 0.2500 0.68600(3) 0.02604(12) Uani 1 d S . . P1 P 0.39471(6) 0.13722(5) 0.87612(5) 0.02406(14) Uani 1 d . . . Cl1 Cl 0.13676(11) 0.2500 0.47701(8) 0.0464(3) Uani 1 d S . . N1 N 0.4322(3) 0.2500 0.7675(2) 0.0239(6) Uani 1 d S . . N2 N 0.3779(3) 0.2500 0.9792(2) 0.0232(6) Uani 1 d S . . N3 N 0.2347(2) 0.11622(16) 0.78535(18) 0.0269(4) Uani 1 d . . . C1 C 0.5591(4) 0.2500 0.6950(3) 0.0328(8) Uani 1 d S . . C2 C 0.5523(3) 0.1452(3) 0.6089(3) 0.0512(8) Uani 1 d . . . H2A H 0.4663 0.1464 0.5458 0.077 Uiso 1 calc R . . H2B H 0.5525 0.0794 0.6649 0.077 Uiso 1 calc R . . H2C H 0.6336 0.1431 0.5611 0.077 Uiso 1 calc R . . C3 C 0.6937(4) 0.2500 0.7964(4) 0.0508(11) Uani 1 d S . . H3A H 0.6965 0.3164 0.8499 0.076 Uiso 0.50 d PR . . H3B H 0.7747 0.2500 0.7499 0.076 Uiso 1 d SR . . C4 C 0.3198(3) 0.2500 1.1068(3) 0.0266(7) Uani 1 d S . . C5 C 0.3718(3) 0.1453(3) 1.1851(3) 0.0481(7) Uani 1 d . . . H5A H 0.4744 0.1453 1.2006 0.072 Uiso 1 calc R . . H5B H 0.3389 0.0792 1.1347 0.072 Uiso 1 calc R . . H5C H 0.3353 0.1450 1.2697 0.072 Uiso 1 calc R . . C6 C 0.1576(4) 0.2500 1.0821(4) 0.0395(9) Uani 1 d S . . H6A H 0.1249 0.3158 1.0332 0.059 Uiso 0.50 d PR . . H6B H 0.1214 0.2500 1.1659 0.059 Uiso 1 d SR . . C7 C 0.1583(2) 0.0086(2) 0.7657(2) 0.0301(5) Uani 1 d . . . C8 C 0.2031(3) -0.0524(3) 0.6457(3) 0.0464(7) Uani 1 d . . . H8A H 0.3035 -0.0688 0.6624 0.070 Uiso 1 calc R . . H8B H 0.1838 -0.0054 0.5675 0.070 Uiso 1 calc R . . H8C H 0.1505 -0.1218 0.6312 0.070 Uiso 1 calc R . . C9 C 0.0007(3) 0.0347(3) 0.7402(3) 0.0484(7) Uani 1 d . . . H9A H -0.0272 0.0733 0.8166 0.073 Uiso 1 calc R . . H9B H -0.0522 -0.0344 0.7255 0.073 Uiso 1 calc R . . H9C H -0.0187 0.0820 0.6621 0.073 Uiso 1 calc R . . C10 C 0.1892(3) -0.0647(2) 0.8888(3) 0.0440(7) Uani 1 d . . . H10A H 0.1613 -0.0258 0.9649 0.066 Uiso 1 calc R . . H10B H 0.2896 -0.0811 0.9051 0.066 Uiso 1 calc R . . H10C H 0.1365 -0.1341 0.8749 0.066 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.0290(2) 0.0275(2) 0.02069(18) 0.000 0.00002(13) 0.000 P1 0.0249(3) 0.0263(3) 0.0214(3) 0.0009(2) 0.0047(2) 0.0019(2) Cl1 0.0602(6) 0.0514(6) 0.0236(4) 0.000 -0.0080(4) 0.000 N1 0.0243(13) 0.0269(14) 0.0219(13) 0.000 0.0083(10) 0.000 N2 0.0258(14) 0.0279(14) 0.0169(12) 0.000 0.0064(10) 0.000 N3 0.0312(10) 0.0249(10) 0.0241(9) 0.0012(8) 0.0018(8) -0.0039(8) C1 0.0301(18) 0.040(2) 0.0325(18) 0.000 0.0189(14) 0.000 C2 0.0565(18) 0.0542(19) 0.0494(17) -0.0112(15) 0.0300(14) 0.0037(15) C3 0.0228(19) 0.075(3) 0.056(3) 0.000 0.0111(17) 0.000 C4 0.0275(16) 0.0341(18) 0.0188(15) 0.000 0.0055(12) 0.000 C5 0.0596(19) 0.0550(19) 0.0312(14) 0.0154(13) 0.0121(13) 0.0174(15) C6 0.0326(19) 0.055(3) 0.0335(19) 0.000 0.0136(15) 0.000 C7 0.0307(13) 0.0268(12) 0.0331(12) -0.0050(10) 0.0056(10) -0.0064(10) C8 0.0558(17) 0.0405(16) 0.0429(15) -0.0163(13) 0.0071(13) -0.0037(14) C9 0.0333(14) 0.0461(17) 0.0651(19) -0.0005(15) 0.0047(13) -0.0051(13) C10 0.0506(16) 0.0318(15) 0.0498(16) 0.0053(13) 0.0076(13) -0.0091(13) _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 N3 1.8856(19) 4_565 ? Ga1 N3 1.8856(19) . ? Ga1 N1 2.089(3) . ? Ga1 Cl1 2.1600(9) . ? Ga1 P1 2.7334(6) 4_565 ? Ga1 P1 2.7334(6) . ? P1 N3 1.692(2) . ? P1 N2 1.7270(16) . ? P1 N1 1.8076(17) . ? P1 P1 2.6963(12) 4_565 ? N1 C1 1.501(4) . ? N1 P1 1.8076(17) 4_565 ? N2 C4 1.477(4) . ? N2 P1 1.7270(16) 4_565 ? N3 C7 1.479(3) . ? C1 C2 1.524(3) . ? C1 C2 1.524(3) 4_565 ? C1 C3 1.533(5) . ? C4 C5 1.529(3) 4_565 ? C4 C5 1.529(3) . ? C4 C6 1.535(5) . ? C7 C10 1.522(3) . ? C7 C9 1.524(3) . ? C7 C8 1.530(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 N3 Ga1 N3 116.01(11) 4_565 . ? N3 Ga1 N1 77.67(7) 4_565 . ? N3 Ga1 N1 77.67(7) . . ? N3 Ga1 Cl1 121.12(6) 4_565 . ? N3 Ga1 Cl1 121.12(6) . . ? N1 Ga1 Cl1 126.45(8) . . ? N3 Ga1 P1 37.63(6) 4_565 4_565 ? N3 Ga1 P1 92.56(6) . 4_565 ? N1 Ga1 P1 41.39(5) . 4_565 ? Cl1 Ga1 P1 143.12(2) . 4_565 ? N3 Ga1 P1 92.56(6) 4_565 . ? N3 Ga1 P1 37.63(6) . . ? N1 Ga1 P1 41.39(5) . . ? Cl1 Ga1 P1 143.12(2) . . ? P1 Ga1 P1 59.10(3) 4_565 . ? N3 P1 N2 107.12(11) . . ? N3 P1 N1 91.01(10) . . ? N2 P1 N1 80.17(9) . . ? N3 P1 P1 98.53(7) . 4_565 ? N2 P1 P1 38.68(6) . 4_565 ? N1 P1 P1 41.77(6) . 4_565 ? N3 P1 Ga1 42.87(7) . . ? N2 P1 Ga1 86.79(8) . . ? N1 P1 Ga1 49.84(8) . . ? P1 P1 Ga1 60.448(13) 4_565 . ? C1 N1 P1 122.62(12) . 4_565 ? C1 N1 P1 122.62(12) . . ? P1 N1 P1 96.46(12) 4_565 . ? C1 N1 Ga1 127.8(2) . . ? P1 N1 Ga1 88.78(9) 4_565 . ? P1 N1 Ga1 88.78(9) . . ? C4 N2 P1 127.45(7) . . ? C4 N2 P1 127.45(7) . 4_565 ? P1 N2 P1 102.64(13) . 4_565 ? C7 N3 P1 126.49(16) . . ? C7 N3 Ga1 131.61(15) . . ? P1 N3 Ga1 99.50(10) . . ? N1 C1 C2 107.87(19) . . ? N1 C1 C2 107.87(19) . 4_565 ? C2 C1 C2 110.6(3) . 4_565 ? N1 C1 C3 109.2(3) . . ? C2 C1 C3 110.6(2) . . ? C2 C1 C3 110.6(2) 4_565 . ? N2 C4 C5 108.79(18) . 4_565 ? N2 C4 C5 108.79(18) . . ? C5 C4 C5 109.9(3) 4_565 . ? N2 C4 C6 110.3(3) . . ? C5 C4 C6 109.51(19) 4_565 . ? C5 C4 C6 109.51(19) . . ? N3 C7 C10 110.69(19) . . ? N3 C7 C9 107.6(2) . . ? C10 C7 C9 109.6(2) . . ? N3 C7 C8 109.6(2) . . ? C10 C7 C8 109.6(2) . . ? C9 C7 C8 109.8(2) . . ? 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 N3 Ga1 P1 N3 131.39(15) 4_565 . . . ? N1 Ga1 P1 N3 -160.57(12) . . . . ? Cl1 Ga1 P1 N3 -71.44(11) . . . . ? P1 Ga1 P1 N3 149.47(10) 4_565 . . . ? N3 Ga1 P1 N2 11.81(9) 4_565 . . . ? N3 Ga1 P1 N2 -119.58(13) . . . . ? N1 Ga1 P1 N2 79.84(11) . . . . ? Cl1 Ga1 P1 N2 168.98(9) . . . . ? P1 Ga1 P1 N2 29.89(8) 4_565 . . . ? N3 Ga1 P1 N1 -68.04(10) 4_565 . . . ? N3 Ga1 P1 N1 160.57(12) . . . . ? Cl1 Ga1 P1 N1 89.13(9) . . . . ? P1 Ga1 P1 N1 -49.95(8) 4_565 . . . ? N3 Ga1 P1 P1 -18.08(6) 4_565 . . 4_565 ? N3 Ga1 P1 P1 -149.47(10) . . . 4_565 ? N1 Ga1 P1 P1 49.95(8) . . . 4_565 ? Cl1 Ga1 P1 P1 139.09(5) . . . 4_565 ? N3 P1 N1 C1 -122.5(2) . . . . ? N2 P1 N1 C1 130.3(2) . . . . ? P1 P1 N1 C1 135.8(3) 4_565 . . . ? Ga1 P1 N1 C1 -135.6(2) . . . . ? N3 P1 N1 P1 101.71(11) . . . 4_565 ? N2 P1 N1 P1 -5.49(12) . . . 4_565 ? Ga1 P1 N1 P1 88.63(10) . . . 4_565 ? N3 P1 N1 Ga1 13.08(8) . . . . ? N2 P1 N1 Ga1 -94.12(10) . . . . ? P1 P1 N1 Ga1 -88.63(10) 4_565 . . . ? N3 Ga1 N1 C1 -119.76(6) 4_565 . . . ? N3 Ga1 N1 C1 119.76(6) . . . . ? Cl1 Ga1 N1 C1 0.0 . . . . ? P1 Ga1 N1 C1 -131.75(6) 4_565 . . . ? P1 Ga1 N1 C1 131.75(6) . . . . ? N3 Ga1 N1 P1 12.00(7) 4_565 . . 4_565 ? N3 Ga1 N1 P1 -108.49(9) . . . 4_565 ? Cl1 Ga1 N1 P1 131.75(6) . . . 4_565 ? P1 Ga1 N1 P1 -96.49(12) . . . 4_565 ? N3 Ga1 N1 P1 108.49(9) 4_565 . . . ? N3 Ga1 N1 P1 -12.00(7) . . . . ? Cl1 Ga1 N1 P1 -131.75(6) . . . . ? P1 Ga1 N1 P1 96.49(12) 4_565 . . . ? N3 P1 N2 C4 80.9(3) . . . . ? N1 P1 N2 C4 168.9(3) . . . . ? P1 P1 N2 C4 163.1(3) 4_565 . . . ? Ga1 P1 N2 C4 119.1(2) . . . . ? N3 P1 N2 P1 -82.17(13) . . . 4_565 ? N1 P1 N2 P1 5.85(12) . . . 4_565 ? Ga1 P1 N2 P1 -43.92(11) . . . 4_565 ? N2 P1 N3 C7 -130.69(18) . . . . ? N1 P1 N3 C7 149.28(19) . . . . ? P1 P1 N3 C7 -169.45(17) 4_565 . . . ? Ga1 P1 N3 C7 164.0(2) . . . . ? N2 P1 N3 Ga1 65.30(11) . . . . ? N1 P1 N3 Ga1 -14.73(9) . . . . ? P1 P1 N3 Ga1 26.54(8) 4_565 . . . ? N3 Ga1 N3 C7 140.72(16) 4_565 . . . ? N1 Ga1 N3 C7 -149.8(2) . . . . ? Cl1 Ga1 N3 C7 -24.4(2) . . . . ? P1 Ga1 N3 C7 171.36(19) 4_565 . . . ? P1 Ga1 N3 C7 -162.8(3) . . . . ? N3 Ga1 N3 P1 -56.51(15) 4_565 . . . ? N1 Ga1 N3 P1 13.01(9) . . . . ? Cl1 Ga1 N3 P1 138.35(7) . . . . ? P1 Ga1 N3 P1 -25.87(8) 4_565 . . . ? P1 N1 C1 C2 -177.41(19) 4_565 . . . ? P1 N1 C1 C2 58.0(3) . . . . ? Ga1 N1 C1 C2 -59.7(2) . . . . ? P1 N1 C1 C2 -58.0(3) 4_565 . . 4_565 ? P1 N1 C1 C2 177.41(19) . . . 4_565 ? Ga1 N1 C1 C2 59.7(2) . . . 4_565 ? P1 N1 C1 C3 62.31(16) 4_565 . . . ? P1 N1 C1 C3 -62.31(16) . . . . ? Ga1 N1 C1 C3 180.0 . . . . ? P1 N2 C4 C5 160.3(2) . . . 4_565 ? P1 N2 C4 C5 -40.6(3) 4_565 . . 4_565 ? P1 N2 C4 C5 40.6(3) . . . . ? P1 N2 C4 C5 -160.3(2) 4_565 . . . ? P1 N2 C4 C6 -79.5(2) . . . . ? P1 N2 C4 C6 79.5(2) 4_565 . . . ? P1 N3 C7 C10 32.9(3) . . . . ? Ga1 N3 C7 C10 -168.44(18) . . . . ? P1 N3 C7 C9 152.54(19) . . . . ? Ga1 N3 C7 C9 -48.8(3) . . . . ? P1 N3 C7 C8 -88.1(2) . . . . ? Ga1 N3 C7 C8 70.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.401 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.070 data_ls25_Compound_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H52 Ga N6 P3' _chemical_formula_weight 587.35 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' 'Ga' 'Ga' 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 19.0514(2) _cell_length_b 17.5082(1) _cell_length_c 9.6695(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3225.32(5) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 159 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 20.53 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.210 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 1.024 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8301 _exptl_absorpt_correction_T_max 0.8780 _exptl_special_details ; Data was collected using a Siemens SMART CCD (charge coupled device) based diffractometer equipped with an LT-2 low-temperature apparatus operating at 213 K. A suitable crystal was chosen and mounted on a glass fiber using grease. Data were measured using omega scans of 0.3\% per frame for 30 seconds, such that a hemisphere was collected. A total of 1271 frames were collected with a final resolution of 0.75 \%A. The first 50 frames were recollected at the end of data collection to monitor for decay. Cell parameters were retrieved using SMART software and refined using SAINT on all observed reflections. Data reduction was performed using the SAINT software which corrects for Lp and decay. Absorption corrections were applied using SADABS supplied by George Sheldrick. The structures are solved by the direct method using the SHELX-90 program and refined by least squares method on F2 SHELXL-97, incorporated in SHELXTL-PC V 5.03. ; _diffrn_ambient_temperature 213(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 ? _diffrn_measurement_method '\w, 0.3 deg' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 14466 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.66 _reflns_number_total 3589 _reflns_number_gt 3058 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'ASTRO (SIEMENS, V4.033, 1994)' _computing_cell_refinement 'SMART (SIEMENS, V4.033, 1994)' _computing_data_reduction 'SAINT (SIEMENS, V4.035, 1994)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (SIEMENS, 1994, ver 5.04)' _computing_publication_material 'CIFTAB (Sheldrick, 1993)' _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 w=1/[\s^2^(Fo^2^)+(0.0672P)^2^+5.0200P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3589 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1395 _refine_ls_wR_factor_gt 0.1309 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.002 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.40293(2) 0.2500 0.63493(4) 0.02508(16) Uani 1 d S . . P1 P 0.34424(5) 0.2500 0.34857(10) 0.0264(2) Uani 1 d S . . P2 P 0.25296(5) 0.2500 0.54864(11) 0.0311(3) Uani 1 d S . . P3 P 0.50890(7) 0.2500 0.82282(14) 0.0399(3) Uani 1 d S . . N1 N 0.29561(13) 0.18427(16) 0.4427(3) 0.0330(6) Uani 1 d . . . N2 N 0.42040(17) 0.2500 0.4389(4) 0.0271(7) Uani 1 d S . . N3 N 0.30705(18) 0.2500 0.6876(3) 0.0294(8) Uani 1 d S . . N4 N 0.46640(14) 0.18186(15) 0.7483(3) 0.0338(6) Uani 1 d . . . C1 C 0.26437(19) 0.1134(2) 0.3870(4) 0.0411(8) Uani 1 d . . . C2 C 0.2030(2) 0.1329(3) 0.2895(5) 0.0725(14) Uani 1 d . . . H2A H 0.2201 0.1636 0.2131 0.109 Uiso 1 calc R . . H2B H 0.1675 0.1612 0.3400 0.109 Uiso 1 calc R . . H2C H 0.1826 0.0860 0.2539 0.109 Uiso 1 calc R . . C3 C 0.2377(3) 0.0650(3) 0.5072(5) 0.0703(13) Uani 1 d . . . H3A H 0.2764 0.0529 0.5684 0.105 Uiso 1 calc R . . H3B H 0.2173 0.0182 0.4718 0.105 Uiso 1 calc R . . H3C H 0.2023 0.0934 0.5579 0.105 Uiso 1 calc R . . C4 C 0.3197(3) 0.0704(3) 0.3052(5) 0.0691(13) Uani 1 d . . . H4A H 0.3587 0.0577 0.3653 0.104 Uiso 1 calc R . . H4B H 0.3362 0.1022 0.2298 0.104 Uiso 1 calc R . . H4C H 0.2995 0.0239 0.2681 0.104 Uiso 1 calc R . . C5 C 0.4869(2) 0.2500 0.3577(5) 0.0346(10) Uani 1 d S . . C6 C 0.4906(2) 0.1779(3) 0.2674(5) 0.0624(12) Uani 1 d . . . H6A H 0.4509 0.1770 0.2046 0.094 Uiso 1 calc R . . H6B H 0.4893 0.1329 0.3260 0.094 Uiso 1 calc R . . H6C H 0.5338 0.1781 0.2146 0.094 Uiso 1 calc R . . C7 C 0.5499(3) 0.2500 0.4555(6) 0.0595(17) Uani 1 d S . . H7A H 0.5484 0.2948 0.5127 0.089 Uiso 0.50 d PR . . H7B H 0.5925 0.2500 0.4025 0.089 Uiso 1 d SR . . C8 C 0.2728(3) 0.2500 0.8271(5) 0.0385(11) Uani 1 d S . . C9 C 0.2276(3) 0.1782(3) 0.8458(4) 0.0708(15) Uani 1 d . . . H9A H 0.1914 0.1771 0.7753 0.106 Uiso 1 calc R . . H9B H 0.2058 0.1791 0.9366 0.106 Uiso 1 calc R . . H9C H 0.2568 0.1331 0.8375 0.106 Uiso 1 calc R . . C10 C 0.3290(3) 0.2500 0.9393(5) 0.0528(14) Uani 1 d S . . H10A H 0.3580 0.2945 0.9295 0.079 Uiso 0.50 d PR . . H10B H 0.3070 0.2500 1.0286 0.079 Uiso 1 d SR . . C11 C 0.4768(2) 0.0991(2) 0.7674(4) 0.0476(9) Uani 1 d . . . C12 C 0.4768(9) 0.0638(4) 0.6331(7) 0.251(9) Uani 1 d . . . H12A H 0.4331 0.0756 0.5860 0.377 Uiso 1 calc R . . H12B H 0.4813 0.0089 0.6433 0.377 Uiso 1 calc R . . H12C H 0.5159 0.0832 0.5794 0.377 Uiso 1 calc R . . C13 C 0.4197(3) 0.0658(3) 0.8517(10) 0.137(4) Uani 1 d . . . H13A H 0.3749 0.0754 0.8071 0.206 Uiso 1 calc R . . H13B H 0.4198 0.0890 0.9428 0.206 Uiso 1 calc R . . H13C H 0.4268 0.0112 0.8605 0.206 Uiso 1 calc R . . C14 C 0.5433(3) 0.0820(4) 0.8424(10) 0.147(4) Uani 1 d . . . H14A H 0.5827 0.1027 0.7910 0.221 Uiso 1 calc R . . H14B H 0.5488 0.0271 0.8513 0.221 Uiso 1 calc R . . H14C H 0.5418 0.1050 0.9336 0.221 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.0252(2) 0.0274(3) 0.0226(2) 0.000 -0.00101(16) 0.000 P1 0.0245(5) 0.0357(6) 0.0190(5) 0.000 -0.0007(4) 0.000 P2 0.0222(5) 0.0472(7) 0.0240(5) 0.000 0.0005(4) 0.000 P3 0.0368(6) 0.0464(7) 0.0366(7) 0.000 -0.0133(5) 0.000 N1 0.0326(13) 0.0370(15) 0.0295(13) -0.0069(11) 0.0048(10) -0.0128(11) N2 0.0231(16) 0.0353(19) 0.0229(17) 0.000 0.0042(13) 0.000 N3 0.0257(17) 0.045(2) 0.0175(16) 0.000 0.0018(13) 0.000 N4 0.0383(14) 0.0304(14) 0.0328(14) 0.0030(11) -0.0052(11) 0.0044(11) C1 0.0445(19) 0.0412(19) 0.0376(18) -0.0051(15) -0.0050(14) -0.0182(15) C2 0.062(3) 0.088(4) 0.067(3) -0.007(3) -0.028(2) -0.027(2) C3 0.092(3) 0.057(3) 0.062(3) 0.003(2) 0.005(3) -0.036(3) C4 0.080(3) 0.054(3) 0.073(3) -0.031(2) 0.007(3) -0.016(2) C5 0.024(2) 0.049(3) 0.030(2) 0.000 0.0072(17) 0.000 C6 0.044(2) 0.084(3) 0.059(3) -0.026(2) 0.0162(19) 0.011(2) C7 0.022(2) 0.108(5) 0.049(3) 0.000 0.007(2) 0.000 C8 0.040(2) 0.058(3) 0.018(2) 0.000 0.0087(18) 0.000 C9 0.068(3) 0.104(4) 0.040(2) 0.013(2) 0.012(2) -0.035(3) C10 0.053(3) 0.086(4) 0.020(2) 0.000 0.002(2) 0.000 C11 0.062(2) 0.0352(18) 0.046(2) 0.0085(16) -0.0057(17) 0.0119(17) C12 0.64(3) 0.049(4) 0.060(4) -0.007(3) -0.024(8) 0.098(8) C13 0.093(4) 0.049(3) 0.270(12) 0.046(5) 0.045(6) -0.004(3) C14 0.072(4) 0.076(4) 0.294(12) 0.083(6) -0.048(5) 0.010(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 N3 1.896(3) . ? Ga1 N2 1.924(3) . ? Ga1 N4 2.021(3) 7_565 ? Ga1 N4 2.021(3) . ? Ga1 P3 2.7160(13) . ? P1 N2 1.694(4) . ? P1 N1 1.735(3) 7_565 ? P1 N1 1.735(3) . ? P1 P2 2.6012(15) . ? P2 N3 1.693(4) . ? P2 N1 1.742(3) 7_565 ? P2 N1 1.742(3) . ? P3 N4 1.612(3) . ? P3 N4 1.612(3) 7_565 ? N1 C1 1.478(4) . ? N2 C5 1.491(5) . ? N3 C8 1.498(5) . ? N4 C11 1.475(4) . ? C1 C4 1.517(6) . ? C1 C3 1.525(5) . ? C1 C2 1.541(5) . ? C5 C7 1.529(7) . ? C5 C6 1.537(5) 7_565 ? C5 C6 1.537(5) . ? C8 C10 1.525(7) . ? C8 C9 1.535(5) 7_565 ? C8 C9 1.535(5) . ? C11 C12 1.438(7) . ? C11 C13 1.479(7) . ? C11 C14 1.490(7) . ? 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 N3 Ga1 N2 115.55(15) . . ? N3 Ga1 N4 115.50(11) . 7_565 ? N2 Ga1 N4 115.50(11) . 7_565 ? N3 Ga1 N4 115.50(11) . . ? N2 Ga1 N4 115.50(11) . . ? N4 Ga1 N4 72.34(15) 7_565 . ? N3 Ga1 P3 122.43(11) . . ? N2 Ga1 P3 122.02(11) . . ? N4 Ga1 P3 36.17(8) 7_565 . ? N4 Ga1 P3 36.17(8) . . ? N2 P1 N1 100.76(13) . 7_565 ? N2 P1 N1 100.76(13) . . ? N1 P1 N1 83.09(18) 7_565 . ? N2 P1 P2 100.89(12) . . ? N1 P1 P2 41.67(9) 7_565 . ? N1 P1 P2 41.67(9) . . ? N3 P2 N1 100.54(13) . 7_565 ? N3 P2 N1 100.54(13) . . ? N1 P2 N1 82.71(18) 7_565 . ? N3 P2 P1 100.57(12) . . ? N1 P2 P1 41.48(9) 7_565 . ? N1 P2 P1 41.48(9) . . ? N4 P3 N4 95.47(19) . 7_565 ? N4 P3 Ga1 47.74(10) . . ? N4 P3 Ga1 47.74(10) 7_565 . ? C1 N1 P1 125.5(2) . . ? C1 N1 P2 125.5(2) . . ? P1 N1 P2 96.85(14) . . ? C5 N2 P1 117.1(3) . . ? C5 N2 Ga1 131.8(3) . . ? P1 N2 Ga1 111.10(17) . . ? C8 N3 P2 116.7(3) . . ? C8 N3 Ga1 131.4(3) . . ? P2 N3 Ga1 111.89(18) . . ? C11 N4 P3 127.1(2) . . ? C11 N4 Ga1 136.8(2) . . ? P3 N4 Ga1 96.10(13) . . ? N1 C1 C4 109.0(3) . . ? N1 C1 C3 108.8(3) . . ? C4 C1 C3 110.8(4) . . ? N1 C1 C2 110.0(3) . . ? C4 C1 C2 108.5(4) . . ? C3 C1 C2 109.7(3) . . ? N2 C5 C7 110.0(4) . . ? N2 C5 C6 109.7(3) . 7_565 ? C7 C5 C6 108.4(3) . 7_565 ? N2 C5 C6 109.7(3) . . ? C7 C5 C6 108.4(3) . . ? C6 C5 C6 110.5(5) 7_565 . ? N3 C8 C10 109.6(4) . . ? N3 C8 C9 110.6(3) . 7_565 ? C10 C8 C9 108.1(3) . 7_565 ? N3 C8 C9 110.6(3) . . ? C10 C8 C9 108.1(3) . . ? C9 C8 C9 109.9(5) 7_565 . ? C12 C11 N4 108.0(4) . . ? C12 C11 C13 109.2(7) . . ? N4 C11 C13 111.0(4) . . ? C12 C11 C14 110.7(7) . . ? N4 C11 C14 111.9(4) . . ? C13 C11 C14 106.2(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 N2 P1 P2 N3 0.0 . . . . ? N1 P1 P2 N3 -94.00(13) 7_565 . . . ? N1 P1 P2 N3 94.00(13) . . . . ? N2 P1 P2 N1 94.00(13) . . . 7_565 ? N1 P1 P2 N1 -172.0(3) . . . 7_565 ? N2 P1 P2 N1 -94.00(13) . . . . ? N1 P1 P2 N1 172.0(3) 7_565 . . . ? N3 Ga1 P3 N4 89.73(14) . . . . ? N2 Ga1 P3 N4 -90.27(14) . . . . ? N4 Ga1 P3 N4 179.5(3) 7_565 . . . ? N3 Ga1 P3 N4 -89.73(14) . . . 7_565 ? N2 Ga1 P3 N4 90.27(14) . . . 7_565 ? N4 Ga1 P3 N4 -179.5(3) . . . 7_565 ? N2 P1 N1 C1 -122.1(3) . . . . ? N1 P1 N1 C1 138.3(2) 7_565 . . . ? P2 P1 N1 C1 143.6(3) . . . . ? N2 P1 N1 P2 94.34(13) . . . . ? N1 P1 N1 P2 -5.35(18) 7_565 . . . ? N3 P2 N1 C1 122.3(3) . . . . ? N1 P2 N1 C1 -138.3(2) 7_565 . . . ? P1 P2 N1 C1 -143.6(3) . . . . ? N3 P2 N1 P1 -94.09(13) . . . . ? N1 P2 N1 P1 5.34(18) 7_565 . . . ? N1 P1 N2 C5 -137.54(9) 7_565 . . . ? N1 P1 N2 C5 137.54(9) . . . . ? P2 P1 N2 C5 180.0 . . . . ? N1 P1 N2 Ga1 42.46(9) 7_565 . . . ? N1 P1 N2 Ga1 -42.46(9) . . . . ? P2 P1 N2 Ga1 0.0 . . . . ? N3 Ga1 N2 C5 180.0 . . . . ? N4 Ga1 N2 C5 40.83(9) 7_565 . . . ? N4 Ga1 N2 C5 -40.83(9) . . . . ? P3 Ga1 N2 C5 0.0 . . . . ? N3 Ga1 N2 P1 0.0 . . . . ? N4 Ga1 N2 P1 -139.17(9) 7_565 . . . ? N4 Ga1 N2 P1 139.17(9) . . . . ? P3 Ga1 N2 P1 180.0 . . . . ? N1 P2 N3 C8 137.77(9) 7_565 . . . ? N1 P2 N3 C8 -137.77(9) . . . . ? P1 P2 N3 C8 180.0 . . . . ? N1 P2 N3 Ga1 -42.23(9) 7_565 . . . ? N1 P2 N3 Ga1 42.23(9) . . . . ? P1 P2 N3 Ga1 0.0 . . . . ? N2 Ga1 N3 C8 180.0 . . . . ? N4 Ga1 N3 C8 -40.83(9) 7_565 . . . ? N4 Ga1 N3 C8 40.83(9) . . . . ? P3 Ga1 N3 C8 0.0 . . . . ? N2 Ga1 N3 P2 0.0 . . . . ? N4 Ga1 N3 P2 139.17(9) 7_565 . . . ? N4 Ga1 N3 P2 -139.17(9) . . . . ? P3 Ga1 N3 P2 180.0 . . . . ? N4 P3 N4 C11 -179.7(2) 7_565 . . . ? Ga1 P3 N4 C11 179.9(4) . . . . ? N4 P3 N4 Ga1 0.4(2) 7_565 . . . ? N3 Ga1 N4 C11 69.3(4) . . . . ? N2 Ga1 N4 C11 -69.9(4) . . . . ? N4 Ga1 N4 C11 179.7(3) 7_565 . . . ? P3 Ga1 N4 C11 -179.9(4) . . . . ? N3 Ga1 N4 P3 -110.74(13) . . . . ? N2 Ga1 N4 P3 110.07(13) . . . . ? N4 Ga1 N4 P3 -0.34(17) 7_565 . . . ? P1 N1 C1 C4 48.9(4) . . . . ? P2 N1 C1 C4 -177.4(3) . . . . ? P1 N1 C1 C3 169.8(3) . . . . ? P2 N1 C1 C3 -56.5(4) . . . . ? P1 N1 C1 C2 -70.0(4) . . . . ? P2 N1 C1 C2 63.6(4) . . . . ? P1 N2 C5 C7 180.0 . . . . ? Ga1 N2 C5 C7 0.0 . . . . ? P1 N2 C5 C6 60.8(3) . . . 7_565 ? Ga1 N2 C5 C6 -119.2(3) . . . 7_565 ? P1 N2 C5 C6 -60.8(3) . . . . ? Ga1 N2 C5 C6 119.2(3) . . . . ? P2 N3 C8 C10 180.0 . . . . ? Ga1 N3 C8 C10 0.0 . . . . ? P2 N3 C8 C9 -61.0(3) . . . 7_565 ? Ga1 N3 C8 C9 119.0(3) . . . 7_565 ? P2 N3 C8 C9 61.0(3) . . . . ? Ga1 N3 C8 C9 -119.0(3) . . . . ? P3 N4 C11 C12 -134.9(7) . . . . ? Ga1 N4 C11 C12 45.0(9) . . . . ? P3 N4 C11 C13 105.5(5) . . . . ? Ga1 N4 C11 C13 -74.6(6) . . . . ? P3 N4 C11 C14 -12.9(6) . . . . ? Ga1 N4 C11 C14 167.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.853 _diffrn_reflns_theta_full 27.66 _diffrn_measured_fraction_theta_full 0.853 _refine_diff_density_max 1.953 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.090