Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Claire J. Carmalt' 'John D. Mileham' 'A. White' 'D. Williams' _publ_contact_author_name 'Dr Claire J Carmalt' _publ_contact_author_address ; Department of Chemistry Christopher Ingold Laboratory University College London 20 Gordon Street London WC1H 0AJ UK ; _publ_contact_author_email C.J.CARMALT@UCL.AC.UK _publ_section_title ; Reactivity of GaX3 with silylamines and thermal decomposition of the compounds [Cl2Ga{NH(SiMe3)}]2 and [Cl3Ga{NH(SiMe3)2}] ; data_Compound_1 _database_code_CSD 207598 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H19 Cl3 Ga N Si2' _chemical_formula_weight 337.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga -1.2846 0.7763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.1596(7) _cell_length_b 11.8563(5) _cell_length_c 19.657(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3066.9(4) _cell_formula_units_Z 8 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 11.98 _cell_measurement_theta_max 27.83 _exptl_crystal_description 'platy needles' _exptl_crystal_colour Clear _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 8.497 _exptl_absorpt_correction_type 'Lamina [0 0 1]' _exptl_absorpt_correction_T_min 0.1420 _exptl_absorpt_correction_T_max 0.8078 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4/RA' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2090 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 7.47 _diffrn_reflns_theta_max 59.96 _reflns_number_total 2090 _reflns_number_gt 1655 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0986P)^2^+0.0000P] 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 SHELXL _refine_ls_extinction_coef 0.00052(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2090 _refine_ls_number_parameters 176 _refine_ls_number_restraints 77 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1413 _refine_ls_wR_factor_gt 0.1322 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 0.999 _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 N N 0.4997(3) 0.1534(3) 0.6034(2) 0.0442(9) Uani 0.95 1 d PDU A 1 H H 0.4734 0.1391 0.5620 0.053 Uiso 0.95 1 calc PR A 1 Ga Ga 0.62295(5) 0.05334(6) 0.60672(4) 0.0549(3) Uani 0.95 1 d PD A 1 Cl1 Cl 0.65417(17) 0.0223(2) 0.71346(10) 0.0655(6) Uani 0.95 1 d PD A 1 Cl2 Cl 0.5832(2) -0.10577(15) 0.55712(11) 0.0731(6) Uani 0.95 1 d PD A 1 Cl3 Cl 0.7507(2) 0.1153(2) 0.55487(18) 0.1193(10) Uani 0.95 1 d PD A 1 Si1 Si 0.39638(11) 0.11238(12) 0.66143(7) 0.0494(4) Uani 0.95 1 d PD A 1 Si2 Si 0.53409(13) 0.30357(12) 0.59827(8) 0.0536(4) Uani 0.95 1 d PD A 1 C1 C 0.4207(7) 0.1724(7) 0.7465(3) 0.0640(18) Uani 0.95 1 d PD A 1 H1A H 0.4250 0.2548 0.7431 0.096 Uiso 0.95 1 calc PR A 1 H1B H 0.4850 0.1426 0.7642 0.096 Uiso 0.95 1 calc PR A 1 H1C H 0.3652 0.1518 0.7773 0.096 Uiso 0.95 1 calc PR A 1 C2 C 0.3875(5) -0.0438(6) 0.6636(4) 0.0666(16) Uani 0.95 1 d PD A 1 H2A H 0.3743 -0.0722 0.6177 0.100 Uiso 0.95 1 calc PR A 1 H2B H 0.3319 -0.0663 0.6939 0.100 Uiso 0.95 1 calc PR A 1 H2C H 0.4516 -0.0752 0.6805 0.100 Uiso 0.95 1 calc PR A 1 C3 C 0.2763(5) 0.1645(7) 0.6231(5) 0.075(2) Uani 0.95 1 d PD A 1 H3A H 0.2668 0.1297 0.5783 0.112 Uiso 0.95 1 calc PR A 1 H3B H 0.2797 0.2466 0.6181 0.112 Uiso 0.95 1 calc PR A 1 H3C H 0.2191 0.1446 0.6527 0.112 Uiso 0.95 1 calc PR A 1 C4 C 0.4244(6) 0.3964(5) 0.6163(4) 0.0745(18) Uani 0.95 1 d PD A 1 H4A H 0.4010 0.3837 0.6629 0.112 Uiso 0.95 1 calc PR A 1 H4B H 0.3693 0.3794 0.5844 0.112 Uiso 0.95 1 calc PR A 1 H4C H 0.4450 0.4754 0.6110 0.112 Uiso 0.95 1 calc PR A 1 C5 C 0.5739(7) 0.3315(6) 0.5090(4) 0.0754(19) Uani 0.95 1 d PD A 1 H5A H 0.6320 0.2834 0.4975 0.113 Uiso 0.95 1 calc PR A 1 H5B H 0.5935 0.4109 0.5044 0.113 Uiso 0.95 1 calc PR A 1 H5C H 0.5173 0.3151 0.4782 0.113 Uiso 0.95 1 calc PR A 1 C6 C 0.6369(6) 0.3268(6) 0.6627(4) 0.0758(18) Uani 0.95 1 d PD A 1 H6A H 0.6945 0.2771 0.6527 0.114 Uiso 0.95 1 calc PR A 1 H6B H 0.6107 0.3100 0.7083 0.114 Uiso 0.95 1 calc PR A 1 H6C H 0.6594 0.4056 0.6609 0.114 Uiso 0.95 1 calc PR A 1 N' N 0.509(2) 0.1503(17) 0.604(2) 0.044(6) Uiso 0.05 1 d PDU B 2 H' H 0.4828 0.1414 0.5616 0.053 Uiso 0.05 1 calc PR B 2 Ga' Ga 0.5386(9) -0.0103(9) 0.6293(5) 0.046(3) Uani 0.05 1 d PD B 2 Cl1' Cl 0.648(3) -0.008(4) 0.7108(19) 0.066(12) Uiso 0.05 1 d PDU B 2 Cl2' Cl 0.6140(19) -0.086(2) 0.5400(12) 0.046(8) Uiso 0.05 1 d PDU B 2 Cl3' Cl 0.410(2) -0.106(3) 0.6485(18) 0.083(8) Uiso 0.05 1 d PDU B 2 Si1' Si 0.6195(19) 0.239(2) 0.5855(15) 0.061(6) Uiso 0.05 1 d PDU B 2 Si2' Si 0.3998(18) 0.209(2) 0.6493(15) 0.054(6) Uiso 0.05 1 d PDU B 2 C1' C 0.686(6) 0.273(9) 0.665(3) 0.076(15) Uiso 0.05 1 d PDU B 2 H1'1 H 0.6884 0.2062 0.6945 0.113 Uiso 0.05 1 calc PR B 2 H1'2 H 0.6495 0.3338 0.6890 0.113 Uiso 0.05 1 calc PR B 2 H1'3 H 0.7553 0.2980 0.6551 0.113 Uiso 0.05 1 calc PR B 2 C2' C 0.704(5) 0.172(7) 0.522(4) 0.068(15) Uiso 0.05 1 d PDU B 2 H2'1 H 0.7537 0.1239 0.5450 0.102 Uiso 0.05 1 calc PR B 2 H2'2 H 0.7392 0.2301 0.4957 0.102 Uiso 0.05 1 calc PR B 2 H2'3 H 0.6630 0.1252 0.4908 0.102 Uiso 0.05 1 calc PR B 2 C3' C 0.568(5) 0.366(5) 0.542(5) 0.075(15) Uiso 0.05 1 d PDU B 2 H3'1 H 0.5036 0.3878 0.5626 0.113 Uiso 0.05 1 calc PR B 2 H3'2 H 0.5577 0.3494 0.4935 0.113 Uiso 0.05 1 calc PR B 2 H3'3 H 0.6169 0.4284 0.5462 0.113 Uiso 0.05 1 calc PR B 2 C4' C 0.384(7) 0.362(3) 0.633(6) 0.065(16) Uiso 0.05 1 d PDU B 2 H4'1 H 0.4450 0.4028 0.6480 0.098 Uiso 0.05 1 calc PR B 2 H4'2 H 0.3246 0.3905 0.6572 0.098 Uiso 0.05 1 calc PR B 2 H4'3 H 0.3749 0.3747 0.5836 0.098 Uiso 0.05 1 calc PR B 2 C5' C 0.283(3) 0.139(9) 0.617(7) 0.064(17) Uiso 0.05 1 d PDU B 2 H5'1 H 0.2901 0.0573 0.6218 0.096 Uiso 0.05 1 calc PR B 2 H5'2 H 0.2738 0.1581 0.5687 0.096 Uiso 0.05 1 calc PR B 2 H5'3 H 0.2243 0.1652 0.6430 0.096 Uiso 0.05 1 calc PR B 2 C6' C 0.424(9) 0.186(12) 0.7422(18) 0.067(16) Uiso 0.05 1 d PDU B 2 H6'1 H 0.4256 0.1046 0.7516 0.100 Uiso 0.05 1 calc PR B 2 H6'2 H 0.3697 0.2210 0.7689 0.100 Uiso 0.05 1 calc PR B 2 H6'3 H 0.4895 0.2193 0.7547 0.100 Uiso 0.05 1 calc PR B 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 N 0.048(2) 0.045(2) 0.0402(19) -0.0031(16) -0.0012(16) -0.0031(16) Ga 0.0548(4) 0.0557(4) 0.0541(4) -0.0062(3) 0.0018(3) 0.0089(3) Cl1 0.0620(10) 0.0788(15) 0.0555(9) -0.0049(9) -0.0123(6) 0.0140(9) Cl2 0.1018(15) 0.0555(9) 0.0620(9) -0.0152(8) -0.0174(11) 0.0155(9) Cl3 0.0915(14) 0.1169(16) 0.149(2) 0.0114(18) 0.0527(17) 0.0062(13) Si1 0.0461(7) 0.0521(8) 0.0501(7) 0.0050(6) 0.0005(6) -0.0026(5) Si2 0.0662(9) 0.0407(7) 0.0538(8) -0.0027(6) 0.0064(7) -0.0068(6) C1 0.069(4) 0.074(4) 0.049(3) -0.002(3) 0.010(3) 0.002(3) C2 0.065(3) 0.056(3) 0.078(4) 0.007(3) 0.006(3) -0.012(3) C3 0.050(3) 0.088(5) 0.086(5) 0.018(4) -0.009(3) 0.003(3) C4 0.093(5) 0.047(3) 0.083(4) 0.007(3) 0.012(4) 0.014(3) C5 0.109(6) 0.058(3) 0.059(3) 0.010(3) 0.024(4) -0.013(3) C6 0.080(4) 0.068(4) 0.080(4) -0.012(4) -0.005(4) -0.022(3) Ga' 0.067(7) 0.036(5) 0.034(5) -0.003(4) -0.014(5) 0.006(5) _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 N Si2 1.839(4) . ? N Si1 1.840(5) . ? N Ga 2.011(4) . ? Ga Cl3 2.099(2) . ? Ga Cl1 2.169(2) . ? Ga Cl2 2.1869(18) . ? Si1 C1 1.845(7) . ? Si1 C2 1.856(7) . ? Si1 C3 1.856(7) . ? Si2 C4 1.849(7) . ? Si2 C5 1.861(7) . ? Si2 C6 1.874(8) . ? N' Si1' 1.828(19) . ? N' Si2' 1.834(18) . ? N' Ga' 2.008(17) . ? Ga' Cl3' 2.073(17) . ? Ga' Cl1' 2.158(17) . ? Ga' Cl2' 2.208(16) . ? Si1' C1' 1.84(2) . ? Si1' C2' 1.85(2) . ? Si1' C3' 1.86(2) . ? Si2' C4' 1.86(2) . ? Si2' C5' 1.86(2) . ? Si2' C6' 1.88(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Si2 N Si1 118.2(2) . . ? Si2 N Ga 112.0(2) . . ? Si1 N Ga 114.8(2) . . ? N Ga Cl3 115.07(15) . . ? N Ga Cl1 106.54(14) . . ? Cl3 Ga Cl1 112.18(13) . . ? N Ga Cl2 107.56(14) . . ? Cl3 Ga Cl2 106.07(12) . . ? Cl1 Ga Cl2 109.27(10) . . ? N Si1 C1 109.4(3) . . ? N Si1 C2 109.0(3) . . ? C1 Si1 C2 112.0(4) . . ? N Si1 C3 106.8(3) . . ? C1 Si1 C3 112.8(4) . . ? C2 Si1 C3 106.7(4) . . ? N Si2 C4 111.9(3) . . ? N Si2 C5 107.1(3) . . ? C4 Si2 C5 107.1(4) . . ? N Si2 C6 106.5(3) . . ? C4 Si2 C6 110.3(4) . . ? C5 Si2 C6 114.1(4) . . ? Si1' N' Si2' 120.0(17) . . ? Si1' N' Ga' 116.0(15) . . ? Si2' N' Ga' 113.0(15) . . ? N' Ga' Cl3' 114.0(13) . . ? N' Ga' Cl1' 107.8(14) . . ? Cl3' Ga' Cl1' 114.7(15) . . ? N' Ga' Cl2' 105.9(12) . . ? Cl3' Ga' Cl2' 106.8(12) . . ? Cl1' Ga' Cl2' 107.1(14) . . ? N' Si1' C1' 110(2) . . ? N' Si1' C2' 111(2) . . ? C1' Si1' C2' 113(2) . . ? N' Si1' C3' 105(2) . . ? C1' Si1' C3' 113(2) . . ? C2' Si1' C3' 105(2) . . ? N' Si2' C4' 112(2) . . ? N' Si2' C5' 108(2) . . ? C4' Si2' C5' 107(2) . . ? N' Si2' C6' 107(2) . . ? C4' Si2' C6' 110(2) . . ? C5' Si2' C6' 114(2) . . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 59.96 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 0.444 _refine_diff_density_min -0.523 _refine_diff_density_rms 0.086 #===END data_Compound_8 _database_code_CSD 207599 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C8 H20 N2 Cl4 Ga2' _chemical_formula_weight 425.50 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga -1.2846 0.7763 '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 6.4619(10) _cell_length_b 11.8491(15) _cell_length_c 10.730(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.286(13) _cell_angle_gamma 90.00 _cell_volume 816.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 5.59 _cell_measurement_theta_max 27.38 _exptl_crystal_description prisms _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.730 _exptl_crystal_density_method ? _exptl_crystal_F_000 424 _exptl_absorpt_coefficient_mu 9.898 _exptl_absorpt_correction_type Ellipsoidal _exptl_absorpt_correction_T_min 0.0230 _exptl_absorpt_correction_T_max 0.1196 _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1490 _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_sigmaI/netI 0.0199 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 5.58 _diffrn_reflns_theta_max 63.95 _reflns_number_total 1361 _reflns_number_observed 1343 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 13 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+0.6039P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0324(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1348 _refine_ls_number_parameters 78 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0406 _refine_ls_R_factor_obs 0.0345 _refine_ls_wR_factor_all 0.1070 _refine_ls_wR_factor_obs 0.0928 _refine_ls_goodness_of_fit_all 1.206 _refine_ls_goodness_of_fit_obs 1.208 _refine_ls_restrained_S_all 1.402 _refine_ls_restrained_S_obs 1.207 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ga Ga 0.09215(5) 0.61030(3) 0.00743(3) 0.0324(2) Uani 1 d . . Cl1 Cl 0.41288(12) 0.64553(8) 0.07406(8) 0.0466(3) Uani 1 d . . Cl2 Cl -0.06798(14) 0.76331(7) -0.04857(8) 0.0488(3) Uani 1 d . . N N 0.0769(4) 0.4821(2) -0.1111(2) 0.0323(6) Uani 1 d D . H H 0.2033(23) 0.4507(27) -0.0923(31) 0.032(8) Uiso 1 d D . C1 C 0.0399(5) 0.4939(3) -0.2524(3) 0.0372(7) Uani 1 d . . C2 C 0.0665(7) 0.3770(3) -0.3080(4) 0.0493(9) Uani 1 d . . H2A H 0.2082(7) 0.3498(3) -0.2830(4) 0.074 Uiso 1 calc R . H2B H 0.0424(7) 0.3812(3) -0.3996(4) 0.074 Uiso 1 calc R . H2C H -0.0339(7) 0.3248(3) -0.2771(4) 0.074 Uiso 1 calc R . C3 C 0.2027(6) 0.5751(4) -0.2931(3) 0.0510(9) Uani 1 d . . H3A H 0.3421(6) 0.5447(4) -0.2682(3) 0.077 Uiso 1 calc R . H3B H 0.1885(6) 0.6485(4) -0.2528(3) 0.077 Uiso 1 calc R . H3C H 0.1820(6) 0.5842(4) -0.3844(3) 0.077 Uiso 1 calc R . C4 C -0.1785(5) 0.5384(3) -0.2895(3) 0.0473(8) Uani 1 d . . H4A H -0.2804(5) 0.4850(3) -0.2625(3) 0.071 Uiso 1 calc R . H4B H -0.2013(5) 0.5474(3) -0.3808(3) 0.071 Uiso 1 calc R . H4C H -0.1947(5) 0.6117(3) -0.2493(3) 0.071 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 Ga 0.0315(3) 0.0328(3) 0.0332(3) 0.00027(13) 0.0040(2) -0.00027(13) Cl1 0.0344(4) 0.0492(5) 0.0552(5) -0.0052(4) 0.0001(3) -0.0057(3) Cl2 0.0528(5) 0.0403(5) 0.0543(5) 0.0076(4) 0.0109(4) 0.0112(3) N 0.0290(13) 0.0368(13) 0.0306(12) 0.0008(10) 0.0018(10) 0.0015(10) C1 0.039(2) 0.044(2) 0.0283(14) 0.0007(13) 0.0008(12) -0.0004(14) C2 0.056(2) 0.054(2) 0.037(2) -0.0075(15) 0.001(2) 0.004(2) C3 0.051(2) 0.062(2) 0.041(2) 0.010(2) 0.010(2) -0.008(2) C4 0.043(2) 0.058(2) 0.039(2) 0.007(2) -0.0016(14) 0.005(2) _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 N 1.973(2) 3_565 ? Ga N 1.977(2) . ? Ga Cl2 2.1408(9) . ? Ga Cl1 2.1579(9) . ? Ga Ga 2.8695(8) 3_565 ? N C1 1.516(4) . ? N Ga 1.973(2) 3_565 ? C1 C4 1.518(4) . ? C1 C3 1.524(5) . ? C1 C2 1.526(5) . ? 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 N Ga N 86.82(10) 3_565 . ? N Ga Cl2 110.33(8) 3_565 . ? N Ga Cl2 118.81(8) . . ? N Ga Cl1 119.44(8) 3_565 . ? N Ga Cl1 109.89(8) . . ? Cl2 Ga Cl1 110.26(4) . . ? N Ga Ga 43.46(7) 3_565 3_565 ? N Ga Ga 43.36(7) . 3_565 ? Cl2 Ga Ga 124.82(3) . 3_565 ? Cl1 Ga Ga 124.91(3) . 3_565 ? C1 N Ga 125.4(2) . 3_565 ? C1 N Ga 124.3(2) . . ? Ga N Ga 93.18(10) 3_565 . ? N C1 C4 109.6(2) . . ? N C1 C3 107.9(3) . . ? C4 C1 C3 110.8(3) . . ? N C1 C2 107.2(3) . . ? C4 C1 C2 110.8(3) . . ? C3 C1 C2 110.5(3) . . ? _refine_diff_density_max 0.653 _refine_diff_density_min -0.749 _refine_diff_density_rms 0.104 #===END