# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 #TrackingRef '18184_web_deposit_cif_file_0_AlexeyY.Timoshkin_1362253790.Al2Br6pyz.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H4 Al2 Br6 N2' _chemical_formula_structural (Br3Al)2(N2C4H4) _chemical_formula_sum 'C4 H4 Al2 Br6 N2' _chemical_formula_iupac ? _chemical_formula_weight 613.45 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.2130 0.2455 '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' C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 6.9688(3) _cell_length_b 15.8935(4) _cell_length_c 7.5060(3) _cell_angle_alpha 90 _cell_angle_beta 117.596(5) _cell_angle_gamma 90 _cell_volume 736.78(6) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 2666 _cell_measurement_theta_min 2.7711 _cell_measurement_theta_max 66.2138 _cell_special_details ; ; _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.320 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.060 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.765 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 556 _exptl_absorpt_coefficient_mu 20.616 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.01039 _exptl_absorpt_correction_T_max 1.00000 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 123 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Oxford Diffraction Gemini Ultra' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean 10.5431 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 5528 _diffrn_reflns_av_R_equivalents 0.0713 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 5.57 _diffrn_reflns_theta_max 65.06 _diffrn_reflns_theta_full 65.06 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 1250 # number of observed reflections (> n sig(I)) _reflns_number_gt 1056 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_solution 'SIR-97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^] 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 noref _refine_ls_extinction_method none _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 1250 _refine_ls_number_parameters 64 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0444 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0877 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.910 _refine_diff_density_min -1.014 _refine_diff_density_rms 0.213 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Br1 Br Uani 0.56235(10) 0.18304(4) 1.45771(8) 1.000 0.0205(2) . . Br2 Br Uani 0.09573(11) 0.03274(4) 1.32555(9) 1.000 0.0242(2) . . Br3 Br Uani 0.04270(10) 0.20716(4) 0.95933(8) 1.000 0.0236(2) . . Al1 Al Uani 0.2653(3) 0.12293(10) 1.2107(2) 1.000 0.0136(5) . . N1 N Uani 0.3994(8) 0.0487(3) 1.0838(7) 1.000 0.0142(14) . . C1 C Uani 0.4548(10) 0.0814(4) 0.9487(9) 1.000 0.0207(19) . . C2 C Uani 0.5592(10) 0.0325(4) 0.8667(9) 1.000 0.0211(19) . . H1 H Uiso 0.42200 0.13850 0.90890 1.000 0.0250 calc R H2 H Uiso 0.60160 0.05700 0.77490 1.000 0.0250 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 Br1 0.0197(3) 0.0169(3) 0.0192(3) -0.0028(2) 0.0042(3) -0.0023(2) Br2 0.0310(4) 0.0226(4) 0.0282(4) -0.0016(2) 0.0214(3) -0.0075(3) Br3 0.0234(4) 0.0273(4) 0.0178(3) 0.0053(2) 0.0076(3) 0.0096(3) Al1 0.0168(9) 0.0122(7) 0.0138(8) -0.0009(6) 0.0087(7) -0.0001(7) N1 0.021(3) 0.011(2) 0.014(2) -0.0022(17) 0.011(2) -0.0026(19) C1 0.029(4) 0.013(3) 0.029(3) 0.004(2) 0.021(3) 0.003(3) C2 0.029(4) 0.015(3) 0.021(3) 0.002(2) 0.013(3) 0.002(3) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Al1 2.2538(18) . . yes Br2 Al1 2.267(2) . . yes Br3 Al1 2.2465(16) . . yes Al1 N1 1.999(6) . . yes N1 C1 1.345(9) . . yes N1 C2 1.337(8) . 3_657 yes C1 C2 1.388(10) . . no C1 H1 0.9500 . . no C2 H2 0.9500 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Br1 Al1 Br2 113.40(6) . . . yes Br1 Al1 Br3 116.88(7) . . . yes Br1 Al1 N1 100.85(18) . . . yes Br2 Al1 Br3 114.67(9) . . . yes Br2 Al1 N1 104.43(16) . . . yes Br3 Al1 N1 104.17(15) . . . yes Al1 N1 C1 119.5(4) . . . yes Al1 N1 C2 121.7(5) . . 3_657 yes C1 N1 C2 118.8(6) . . 3_657 yes N1 C1 C2 120.7(6) . . . yes N1 C2 C1 120.5(6) 3_657 . . yes N1 C1 H1 120.00 . . . no C2 C1 H1 120.00 . . . no C1 C2 H2 120.00 . . . no N1 C2 H2 120.00 3_657 . . no 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 Br1 Al1 N1 C1 -82.5(5) . . . . no Br2 Al1 N1 C1 159.6(5) . . . . no Br3 Al1 N1 C1 39.0(5) . . . . no Br1 Al1 N1 C2 95.8(5) . . . 3_657 no Br2 Al1 N1 C2 -22.1(5) . . . 3_657 no Br3 Al1 N1 C2 -142.7(5) . . . 3_657 no Al1 N1 C1 C2 176.4(5) . . . . no C2 N1 C1 C2 -2.0(9) 3_657 . . . no Al1 N1 C2 C1 176.3(5) 3_657 3_657 . . no C1 N1 C2 C1 -2.0(9) 3_657 3_657 . . no N1 C1 C2 N1 2.0(10) . . . 3_657 no 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 Br1 Br2 3.7784(10) . . no Br1 Br3 3.8346(9) . . no Br1 Br3 3.7218(8) . 1_656 no Br1 N1 3.282(5) . . no Br1 Br3 3.7701(10) . 4_655 no Br2 Br2 3.5998(10) . 3_558 no Br2 N1 3.375(6) . . no Br2 Br1 3.7784(10) . . no Br2 Br3 3.7995(9) . . no Br2 C2 3.486(7) . 3_657 no Br2 C2 3.730(7) . 1_455 no Br3 C1 3.530(7) . . no Br3 Al1 3.9829(19) . 4_554 no Br3 Br1 3.7701(10) . 4_454 no Br3 Br1 3.7218(8) . 1_454 no Br3 Br1 3.8346(9) . . no Br3 Br2 3.7995(9) . . no Br3 N1 3.353(5) . . no Br1 H2 3.0300 . 1_556 no Br1 H1 2.9700 . 4_555 no Br2 H2 2.9200 . 3_657 no Br3 H1 3.0400 . . no Al1 Br3 3.9829(19) . 4_555 no N1 Br1 3.282(5) . . no N1 Br2 3.375(6) . . no N1 Br3 3.353(5) . . no N1 N1 2.753(8) . 3_657 no C2 Br2 3.730(7) . 1_655 no H1 Br3 3.0400 . . no H1 Br1 2.9700 . 4_554 no H2 Br1 3.0300 . 1_554 no H2 Br2 2.9200 . 3_657 no 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 # #D H A D - H H...A D...A D - H...A symm(A) # C2 H2 Br2 0.9500 2.9200 3.486(7) 119.00 3_657 yes _vrf_PLAT027_1 ; PROBLEM: _diffrn_reflns_theta_full (too) Low ............ 65.06 Deg. RESPONSE: Theta was technically limited at the Gemini Ultra system in older software versions. ; _database_code_depnum_ccdc_archive 'CCDC 927394' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ta01 #TrackingRef '18185_web_deposit_cif_file_1_AlexeyY.Timoshkin_1362253790.AlBr3pyz.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H4 Al Br3 N2' _chemical_formula_structural ? _chemical_formula_sum 'C4 H4 Al Br3 N2' _chemical_formula_iupac ? _chemical_formula_weight 346.77 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,y,1/2-z 3 -x,-y,-z 4 x,-y,1/2+z 5 1/2+x,1/2+y,z 6 1/2-x,1/2+y,1/2-z 7 1/2-x,1/2-y,-z 8 1/2+x,1/2-y,1/2+z _cell_length_a 11.2325(11) _cell_length_b 6.7023(4) _cell_length_c 11.8372(19) _cell_angle_alpha 90 _cell_angle_beta 104.753(14) _cell_angle_gamma 90 _cell_volume 861.77(18) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 2419 _cell_measurement_theta_min 3.0316 _cell_measurement_theta_max 32.5680 _cell_special_details ; ; _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.180 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.673 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 14.072 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_T_min 0.11272 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Analytical absorption correction using crystal faces, implemented in SCALE3 ABSPACK scaling algorithm. ; #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini Ultra' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean 10.5431 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 4473 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 30.51 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 1316 # number of observed reflections (> n sig(I)) _reflns_number_gt 1027 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_solution 'SIR-97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0495P)^2^] 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 constr _refine_ls_extinction_method shelxl _refine_ls_extinction_coef 0.0029(3) _refine_ls_extinction_expression FC^*^=KFC[1+0.001XFC^2^\L^3^/SIN(2\Q)]^-1/4^ _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 1316 _refine_ls_number_parameters 48 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0795 _refine_ls_wR_factor_gt 0.0762 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.265 _refine_diff_density_min -0.769 _refine_diff_density_rms 0.190 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Br1 Br Uani 0.50000 0.86826(7) 0.25000 1.000 0.0173(1) . . Br2 Br Uani 0.38852(3) 1.36476(5) 0.36709(3) 1.000 0.0144(1) . . Al3 Al Uani 0.50000 1.2129(2) 0.25000 1.000 0.0099(3) . . N1 N Uani 0.6550(2) 1.2319(4) 0.3976(2) 1.000 0.0102(7) . . C1 C Uani 0.6724(3) 1.0972(5) 0.4841(3) 1.000 0.0145(9) . . C2 C Uani 0.7330(3) 1.3864(5) 0.4148(3) 1.000 0.0139(9) . . H1 H Uiso 0.61800 0.98650 0.47580 1.000 0.0170 calc R H2 H Uiso 0.72350 1.48690 0.35660 1.000 0.0170 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 Br1 0.0198(3) 0.0119(2) 0.0157(2) 0.0000 -0.0039(2) 0.0000 Br2 0.0122(2) 0.0209(2) 0.0102(2) -0.0012(1) 0.0030(1) 0.0026(1) Al3 0.0083(6) 0.0126(6) 0.0079(6) 0.0000 0.0003(5) 0.0000 N1 0.0078(13) 0.0136(13) 0.0092(12) -0.0003(10) 0.0020(10) 0.0007(10) C1 0.0132(16) 0.0182(16) 0.0113(15) 0.0015(13) 0.0017(13) -0.0025(14) C2 0.0157(16) 0.0147(16) 0.0097(15) 0.0027(12) 0.0004(13) -0.0002(13) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Al3 2.3099(15) . . yes Br2 Al3 2.3257(8) . . yes Al3 N1 2.133(2) . . yes Al3 N1 2.133(2) . 2_655 yes N1 C1 1.342(4) . . yes N1 C2 1.338(4) . . yes C1 C2 1.388(5) . 7_676 no C1 H1 0.9500 . . no C2 H2 0.9500 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Br1 Al3 Br2 115.95(3) . . . yes Br1 Al3 N1 93.42(8) . . . yes Br1 Al3 Br2 115.95(3) . . 2_655 yes Br1 Al3 N1 93.42(8) . . 2_655 yes Br2 Al3 N1 86.38(7) . . . yes Br2 Al3 Br2 128.09(6) . . 2_655 yes Br2 Al3 N1 90.63(7) . . 2_655 yes Br2 Al3 N1 90.63(7) 2_655 . . yes N1 Al3 N1 173.16(13) . . 2_655 yes Br2 Al3 N1 86.38(7) 2_655 . 2_655 yes Al3 N1 C1 121.0(2) . . . yes Al3 N1 C2 122.5(2) . . . yes C1 N1 C2 116.2(3) . . . yes N1 C1 C2 122.4(3) . . 7_676 yes N1 C2 C1 121.4(3) . . 7_676 yes N1 C1 H1 119.00 . . . no C2 C1 H1 119.00 7_676 . . no N1 C2 H2 119.00 . . . no C1 C2 H2 119.00 7_676 . . no 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 Br1 Al3 N1 C1 -34.7(2) . . . . no Br1 Al3 N1 C2 151.8(2) . . . . no Br2 Al3 N1 C1 81.1(2) . . . . no Br2 Al3 N1 C2 -92.4(2) . . . . no Br2 Al3 N1 C1 -150.7(2) 2_655 . . . no Br2 Al3 N1 C2 35.7(2) 2_655 . . . no Al3 N1 C1 C2 -175.1(3) . . . 7_676 no C2 N1 C1 C2 -1.1(5) . . . 7_676 no Al3 N1 C2 C1 175.0(2) . . . 7_676 no C1 N1 C2 C1 1.1(5) . . . 7_676 no N1 C1 C2 N1 1.2(5) . . 7_676 7_676 no 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 Br1 N1 3.237(3) . . no Br1 C1 3.324(3) . . no Br1 N1 3.237(3) . 2_655 no Br1 C1 3.324(3) . 2_655 no Br2 C2 3.271(3) . 2_655 no Br2 C2 3.620(4) . 3_686 no Br2 N1 3.055(2) . . no Br2 C1 3.613(4) . . no Br2 N1 3.173(2) . 2_655 no Br2 C1 3.711(3) . 3_676 no Br2 C1 3.457(4) . 5_455 no Br1 H1 2.7800 . . no Br1 H1 2.7800 . 2_655 no Br2 H2 2.7500 . 2_655 no Br2 H1 3.0100 . 3_676 no Br2 H2 3.1200 . 5_445 no N1 Br1 3.237(3) . . no N1 Br2 3.055(2) . . no N1 Br2 3.173(2) . 2_655 no N1 N1 2.803(3) . 7_676 no C1 Br2 3.711(3) . 3_676 no C1 Br2 3.457(4) . 5_545 no C2 Br2 3.620(3) . 3_686 no H1 Br1 2.7800 . . no H1 Br2 3.0100 . 3_676 no H2 Br2 2.7500 . 2_655 no H2 Br2 3.1200 . 5_555 no 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 # #D H A D - H H...A D...A D - H...A symm(A) # C1 H1 Br1 0.9500 2.7800 3.324(3) 117.00 . yes C2 H2 Br2 0.9500 2.7500 3.271(3) 115.00 2_655 yes _database_code_depnum_ccdc_archive 'CCDC 927395' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ayt12 #TrackingRef '18186_web_deposit_cif_file_2_AlexeyY.Timoshkin_1362253790.Ga2Cl6pyz.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H4 Cl6 Ga2 N2' _chemical_formula_structural ? _chemical_formula_sum 'C4 H4 Cl6 Ga2 N2' _chemical_formula_iupac ? _chemical_formula_weight 432.23 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0311 0.0180 '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' Cl Cl 0.3639 0.7018 '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' C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 1/2+x,1/2-y,1/2+z _cell_length_a 6.6265(7) _cell_length_b 15.4544(10) _cell_length_c 7.1401(8) _cell_angle_alpha 90 _cell_angle_beta 115.721(13) _cell_angle_gamma 90 _cell_volume 658.76(13) _cell_formula_units_Z 2 _cell_measurement_temperature 123.0(1) _cell_measurement_reflns_used 3415 _cell_measurement_theta_min 2.8586 _cell_measurement_theta_max 66.3682 _cell_special_details ; ; _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.490 _exptl_crystal_size_mid 0.320 _exptl_crystal_size_min 0.230 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.179 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 412 _exptl_absorpt_coefficient_mu 15.948 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_T_min 0.09657 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.30 (release 18-06-2008 CrysAlis171 .NET) (compiled Jun 18 2008,17:52:12) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 123.0(1) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Oxford Diffraction Gemini Ultra' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean 10.5431 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 4464 _diffrn_reflns_av_R_equivalents 0.1356 _diffrn_reflns_av_sigmaI/netI 0.0686 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 5.73 _diffrn_reflns_theta_max 66.68 _diffrn_reflns_theta_full 66.68 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measured_fraction_theta_full 0.985 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 1151 # number of observed reflections (> n sig(I)) _reflns_number_gt 1088 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.30 (release 18-06-2008 CrysAlis171 .NET) (compiled Jun 18 2008,17:52:12) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.30 (release 18-06-2008 CrysAlis171 .NET) (compiled Jun 18 2008,17:52:12) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.30 (release 18-06-2008 CrysAlis171 .NET) (compiled Jun 18 2008,17:52:12) ; _computing_structure_solution 'SIR-97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1921P)^2^+2.8870P] 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 constr _refine_ls_extinction_method none _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 1151 _refine_ls_number_parameters 64 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0957 _refine_ls_R_factor_gt 0.0936 _refine_ls_wR_factor_ref 0.2505 _refine_ls_wR_factor_gt 0.2485 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.566 _refine_diff_density_min -2.532 _refine_diff_density_rms 0.399 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Ga1 Ga Uani 0.46676(15) 0.87369(5) 0.22306(14) 1.000 0.0104(5) . . Cl1 Cl Uani 0.4198(3) 0.81620(11) 0.4732(3) 1.000 0.0167(6) . . Cl2 Cl Uani 0.7358(3) 0.96588(12) 0.3260(3) 1.000 0.0209(7) . . Cl3 Cl Uani 0.4423(3) 0.79020(14) -0.0231(3) 1.000 0.0231(7) . . N1 N Uani 0.1879(10) 0.9497(4) 0.0888(10) 1.000 0.0097(17) . . C1 C Uani 0.1945(13) 1.0335(5) 0.1389(12) 1.000 0.014(2) . . C2 C Uani -0.0042(14) 0.9165(5) -0.0505(13) 1.000 0.017(2) . . H1 H Uiso 0.32800 1.05800 0.23380 1.000 0.0170 calc R H2 H Uiso -0.00990 0.85860 -0.08840 1.000 0.0200 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 0.0078(8) 0.0075(8) 0.0154(8) 0.0004(3) 0.0047(6) -0.0004(3) Cl1 0.0221(11) 0.0097(10) 0.0215(12) 0.0019(7) 0.0125(9) -0.0018(7) Cl2 0.0104(11) 0.0191(11) 0.0286(13) 0.0031(7) 0.0043(9) -0.0083(8) Cl3 0.0194(11) 0.0265(12) 0.0230(12) -0.0069(8) 0.0089(9) 0.0061(8) N1 0.008(3) 0.005(3) 0.015(3) -0.001(2) 0.004(3) -0.001(2) C1 0.012(4) 0.008(4) 0.018(4) -0.006(3) 0.002(3) -0.003(3) C2 0.014(4) 0.006(3) 0.029(5) -0.006(3) 0.008(3) -0.004(3) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 Cl1 2.135(2) . . yes Ga1 Cl2 2.147(2) . . yes Ga1 Cl3 2.129(2) . . yes Ga1 N1 2.044(7) . . yes N1 C1 1.339(10) . . yes N1 C2 1.332(11) . . yes C1 C2 1.377(13) . 3_575 no C1 H1 0.9300 . . no C2 H2 0.9300 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Ga1 Cl2 112.99(8) . . . yes Cl1 Ga1 Cl3 116.86(8) . . . yes Cl1 Ga1 N1 101.6(2) . . . yes Cl2 Ga1 Cl3 116.05(9) . . . yes Cl2 Ga1 N1 103.10(19) . . . yes Cl3 Ga1 N1 103.40(19) . . . yes Ga1 N1 C1 120.8(6) . . . yes Ga1 N1 C2 120.4(5) . . . yes C1 N1 C2 118.8(7) . . . yes N1 C1 C2 120.2(8) . . 3_575 yes N1 C2 C1 121.0(7) . . 3_575 yes N1 C1 H1 120.00 . . . no C2 C1 H1 120.00 3_575 . . no N1 C2 H2 120.00 . . . no C1 C2 H2 120.00 3_575 . . no 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 Cl1 Ga1 N1 C1 95.2(6) . . . . no Cl2 Ga1 N1 C1 -22.1(7) . . . . no Cl3 Ga1 N1 C1 -143.3(6) . . . . no Cl1 Ga1 N1 C2 -84.8(6) . . . . no Cl2 Ga1 N1 C2 158.0(6) . . . . no Cl3 Ga1 N1 C2 36.7(7) . . . . no Ga1 N1 C1 C2 -178.6(6) . . . 3_575 no C2 N1 C1 C2 1.3(12) . . . 3_575 no Ga1 N1 C2 C1 178.6(6) . . . 3_575 no C1 N1 C2 C1 -1.4(13) . . . 3_575 no N1 C1 C2 N1 -1.4(13) . . 3_575 3_575 no 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 Ga1 Cl3 3.831(2) . 4_565 no Cl1 Cl2 3.571(3) . . no Cl1 Cl3 3.633(3) . . no Cl1 Cl3 3.557(3) . 1_556 no Cl1 N1 3.239(7) . . no Cl1 Cl3 3.576(3) . 4_465 no Cl1 C2 3.645(8) . 4_565 no Cl2 C1 3.404(9) . . no Cl2 N1 3.468(7) . 3_675 no Cl2 Cl1 3.571(3) . . no Cl2 Cl3 3.628(3) . . no Cl2 N1 3.283(7) . . no Cl2 C1 3.544(8) . 3_675 no Cl2 Cl2 3.463(3) . 3_776 no Cl2 C1 3.644(8) . 3_676 no Cl3 Cl2 3.628(3) . . no Cl3 C2 3.479(10) . . no Cl3 Cl1 3.633(3) . . no Cl3 Cl1 3.557(3) . 1_554 no Cl3 Cl1 3.576(3) . 4_564 no Cl3 N1 3.275(7) . . no Cl3 Ga1 3.831(2) . 4_464 no Cl1 H1 2.8100 . 3_676 no Cl1 H2 2.8100 . 4_565 no Cl2 H1 2.8700 . . no Cl3 H2 3.0200 . . no N1 Cl1 3.239(7) . . no N1 Cl2 3.283(7) . . no N1 Cl3 3.275(7) . . no N1 Cl2 3.468(7) . 3_675 no N1 N1 2.736(10) . 3_575 no C1 Cl2 3.544(8) . 3_675 no C1 Cl2 3.644(8) . 3_676 no C2 Cl1 3.645(8) . 4_464 no H1 Cl2 2.8700 . . no H1 Cl1 2.8100 . 3_676 no H2 Cl3 3.0200 . . no H2 Cl1 2.8100 . 4_464 no 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 # #D H A D - H H...A D...A D - H...A symm(A) # C1 H1 Cl1 0.9300 2.8100 3.668(8) 153.00 3_676 yes C2 H2 Cl1 0.9300 2.8100 3.645(8) 150.00 4_464 yes _database_code_depnum_ccdc_archive 'CCDC 927396' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ayt6 #TrackingRef '18187_web_deposit_cif_file_3_AlexeyY.Timoshkin_1362253790.GaCl3pyz.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H4 Cl3 Ga N2' _chemical_formula_structural ? _chemical_formula_sum 'C4 H4 Cl3 Ga N2' _chemical_formula_iupac ? _chemical_formula_weight 256.16 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0311 0.0180 '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' Cl Cl 0.3639 0.7018 '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' C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,y,1/2-z 3 -x,-y,-z 4 x,-y,1/2+z 5 1/2+x,1/2+y,z 6 1/2-x,1/2+y,1/2-z 7 1/2-x,1/2-y,-z 8 1/2+x,1/2-y,1/2+z _cell_length_a 11.1474(7) _cell_length_b 6.3189(5) _cell_length_c 11.5922(8) _cell_angle_alpha 90 _cell_angle_beta 101.953(7) _cell_angle_gamma 90 _cell_volume 798.84(10) _cell_formula_units_Z 4 _cell_measurement_temperature 123.0(1) _cell_measurement_reflns_used 969 _cell_measurement_theta_min 3.8898 _cell_measurement_theta_max 61.9455 _cell_special_details ; ; _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.128 _exptl_crystal_size_mid 0.018 _exptl_crystal_size_min 0.017 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.130 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 13.328 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_T_min 0.353 _exptl_absorpt_correction_T_max 0.797 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 123.0(1) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Oxford Diffraction Gemini Ultra' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean 10.5431 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 1179 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 7.81 _diffrn_reflns_theta_max 58.92 _diffrn_reflns_theta_full 58.92 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measured_fraction_theta_full 0.989 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 565 # number of observed reflections (> n sig(I)) _reflns_number_gt 510 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) ; _computing_structure_solution 'SIR-97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0886P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # constr - H parameters constrained # mixed - some constrained, some independent # undef - H-atom parameters not defined _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 565 _refine_ls_number_parameters 47 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1149 _refine_ls_wR_factor_gt 0.1127 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.212 _refine_diff_density_min -0.772 _refine_diff_density_rms 0.192 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Ga1 Ga Uani 0.50000 0.22026(14) 0.25000 1.000 0.0163(3) . . Cl1 Cl Uani 0.39262(12) 0.3790(2) 0.36223(12) 1.000 0.0215(5) . . Cl2 Cl Uani 0.50000 -0.1238(3) 0.25000 1.000 0.0260(7) . . N1 N Uani 0.3426(4) 0.2334(7) 0.0997(4) 1.000 0.0171(14) . . C1 C Uani 0.3273(5) 0.0877(9) 0.0148(5) 1.000 0.0202(17) . . C2 C Uani 0.2646(5) 0.3961(9) 0.0842(5) 1.000 0.0214(17) . . H1 H Uiso 0.38130 -0.03030 0.02280 1.000 0.0240 calc R H2 H Uiso 0.27280 0.50310 0.14280 1.000 0.0250 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 0.0099(6) 0.0174(6) 0.0216(6) 0.0000 0.0034(4) 0.0000 Cl1 0.0146(8) 0.0267(9) 0.0241(9) -0.0015(5) 0.0059(6) 0.0029(5) Cl2 0.0243(11) 0.0177(11) 0.0320(12) 0.0000 -0.0032(9) 0.0000 N1 0.008(2) 0.023(2) 0.019(3) 0.0012(19) 0.000(2) -0.0031(18) C1 0.014(3) 0.021(3) 0.026(3) 0.001(2) 0.005(3) 0.003(2) C2 0.020(3) 0.016(3) 0.029(3) -0.002(2) 0.007(3) 0.001(2) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 Cl1 2.1855(14) . . yes Ga1 Cl2 2.174(2) . . yes Ga1 N1 2.203(5) . . yes Ga1 Cl1 2.1855(14) . 2_655 yes Ga1 N1 2.203(5) . 2_655 yes N1 C1 1.333(7) . . yes N1 C2 1.334(7) . . yes C1 C2 1.375(8) . 7_555 no C1 H1 0.9500 . . no C2 H2 0.9500 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Ga1 Cl2 117.32(4) . . . yes Cl1 Ga1 N1 90.50(12) . . . yes Cl1 Ga1 Cl1 125.36(6) . . 2_655 yes Cl1 Ga1 N1 87.51(12) . . 2_655 yes Cl2 Ga1 N1 92.16(12) . . . yes Cl1 Ga1 Cl2 117.32(4) 2_655 . . yes Cl2 Ga1 N1 92.16(12) . . 2_655 yes Cl1 Ga1 N1 87.51(12) 2_655 . . yes N1 Ga1 N1 175.68(17) . . 2_655 yes Cl1 Ga1 N1 90.50(12) 2_655 . 2_655 yes Ga1 N1 C1 121.1(4) . . . yes Ga1 N1 C2 121.7(4) . . . yes C1 N1 C2 116.9(5) . . . yes N1 C1 C2 121.6(5) . . 7_555 yes N1 C2 C1 121.5(5) . . 7_555 yes N1 C1 H1 119.00 . . . no C2 C1 H1 119.00 7_555 . . no N1 C2 H2 119.00 . . . no C1 C2 H2 119.00 7_555 . . no 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 Cl1 Ga1 N1 C1 -151.2(4) . . . . no Cl2 Ga1 N1 C1 -33.9(4) . . . . no Cl1 Ga1 N1 C1 83.4(4) 2_655 . . . no Cl1 Ga1 N1 C2 34.6(4) . . . . no Cl2 Ga1 N1 C2 152.0(4) . . . . no Cl1 Ga1 N1 C2 -90.7(4) 2_655 . . . no Ga1 N1 C1 C2 -174.5(4) . . . 7_555 no C2 N1 C1 C2 -0.1(8) . . . 7_555 no Ga1 N1 C2 C1 174.4(4) . . . 7_555 no C1 N1 C2 C1 0.1(8) . . . 7_555 no N1 C1 C2 N1 0.1(9) . . 7_555 7_555 no 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 Cl1 Cl2 3.693(2) . 1_565 no Cl1 N1 3.117(5) . . no Cl1 C2 3.245(6) . . no Cl1 C2 3.636(6) . 6_545 no Cl1 Cl2 3.693(2) . 2_665 no Cl1 N1 3.035(5) . 2_655 no Cl1 C1 3.590(6) . 4_555 no Cl1 C2 3.493(6) . 4_565 no Cl1 C1 3.351(6) . 6_555 no Cl2 C1 3.279(6) . . no Cl2 C1 3.279(6) . 2_655 no Cl2 N1 3.153(5) . 2_655 no Cl2 Cl1 3.693(2) . 1_545 no Cl2 N1 3.153(5) . . no Cl2 Cl1 3.693(2) . 2_645 no Cl1 H1 2.9000 . 4_555 no Cl1 H2 2.7300 . . no Cl1 H2 3.0000 . 6_545 no Cl2 H1 2.7600 . . no Cl2 H1 2.7600 . 2_655 no N1 Cl1 3.117(5) . . no N1 Cl2 3.153(5) . . no N1 Cl1 3.035(5) . 2_655 no N1 N1 2.770(6) . 7_555 no C1 Cl1 3.590(6) . 4_554 no C1 Cl1 3.351(6) . 6_545 no C2 Cl1 3.493(6) . 4_564 no C2 Cl1 3.636(6) . 6_555 no H1 Cl2 2.7600 . . no H1 Cl1 2.9000 . 4_554 no H2 Cl1 2.7300 . . no H2 Cl1 3.0000 . 6_555 no 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 # #D H A D - H H...A D...A D - H...A symm(A) # C1 H1 Cl2 0.9500 2.7600 3.279(6) 115.00 . yes C2 H2 Cl1 0.9500 2.7300 3.245(6) 115.00 . yes _database_code_depnum_ccdc_archive 'CCDC 927397' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ayt26 #TrackingRef '18188_web_deposit_cif_file_4_AlexeyY.Timoshkin_1362253790.GaI3pyz.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H4 Ga I3 N2' _chemical_formula_structural ? _chemical_formula_sum 'C4 H4 Ga I3 N2' _chemical_formula_iupac ? _chemical_formula_weight 530.51 _chemical_compound_source 'see text' 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' Ga Ga 0.2307 1.6083 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 ' 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' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 7.1493(10) _cell_length_b 9.3992(17) _cell_length_c 9.5165(12) _cell_angle_alpha 60.776(16) _cell_angle_beta 79.488(12) _cell_angle_gamma 87.758(13) _cell_volume 547.79(17) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 2272 _cell_measurement_theta_min 3.4575 _cell_measurement_theta_max 29.2892 _cell_special_details ; ; _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.216 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 464 _exptl_absorpt_coefficient_mu 10.908 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_T_min 0.43892 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini Ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5431 # number of measured reflections (redundant set) _diffrn_reflns_number 5809 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0598 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 29.23 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_max 0.866 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 2573 # number of observed reflections (> n sig(I)) _reflns_number_gt 2125 _reflns_threshold_expression >2\s(i) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_structure_solution 'SIR-92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SXGRAPH (Farrugia, 1999)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0321P)^2^] 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 constr _refine_ls_extinction_method none _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 2573 _refine_ls_number_parameters 91 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.0863 _refine_ls_wR_factor_gt 0.0789 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.358 _refine_diff_density_min -1.436 _refine_diff_density_rms 0.268 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I Uani 0.34237(7) 0.24413(6) 0.15283(5) 1.000 0.0274(2) d . . . I2 I Uani 0.23540(7) 0.23945(5) 0.61178(5) 1.000 0.0251(2) d . . . I3 I Uani -0.21036(7) 0.27563(6) 0.36465(5) 1.000 0.0288(2) d . . . Ga4 Ga Uani 0.13816(11) 0.32785(8) 0.34180(8) 1.000 0.0190(2) d . . . N1 N Uani 0.1819(8) 0.5755(6) 0.2164(6) 1.000 0.0176(17) d . . . N2 N Uani 0.2441(9) 0.9141(7) 0.0309(6) 1.000 0.0251(19) d . . . C1 C Uani 0.2993(11) 0.6564(8) 0.2510(8) 1.000 0.024(2) d . . . C2 C Uani 0.3267(11) 0.8227(9) 0.1578(8) 1.000 0.028(2) d . . . C3 C Uani 0.1283(11) 0.8313(8) -0.0014(8) 1.000 0.025(2) d . . . C4 C Uani 0.0948(10) 0.6640(8) 0.0904(7) 1.000 0.022(2) d . . . H1 H Uiso 0.36380 0.59850 0.34030 1.000 0.0290 c R . . H2 H Uiso 0.41070 0.87630 0.18620 1.000 0.0330 c R . . H3 H Uiso 0.06560 0.88980 -0.09180 1.000 0.0300 c R . . H4 H Uiso 0.00830 0.61120 0.06340 1.000 0.0260 c 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 I1 0.0239(3) 0.0311(3) 0.0307(3) -0.0194(2) -0.0001(2) 0.0004(2) I2 0.0245(3) 0.0271(3) 0.0179(2) -0.0065(2) -0.0038(2) -0.0017(2) I3 0.0178(3) 0.0381(3) 0.0310(3) -0.0181(2) -0.0002(2) -0.0066(2) Ga4 0.0176(4) 0.0183(4) 0.0182(4) -0.0072(3) -0.0011(3) -0.0026(3) N1 0.014(3) 0.019(3) 0.016(3) -0.006(2) -0.002(2) 0.002(2) N2 0.025(4) 0.023(3) 0.022(3) -0.009(3) 0.003(3) -0.006(3) C1 0.028(4) 0.025(4) 0.020(3) -0.011(3) -0.005(3) -0.005(3) C2 0.020(4) 0.032(4) 0.025(4) -0.008(3) -0.006(3) -0.009(3) C3 0.031(5) 0.026(4) 0.018(3) -0.010(3) -0.006(3) 0.002(3) C4 0.017(4) 0.026(4) 0.016(3) -0.005(3) -0.005(3) -0.001(3) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Ga4 2.5137(10) . . yes I2 Ga4 2.5094(9) . . yes I3 Ga4 2.5081(11) . . yes Ga4 N1 2.037(6) . . yes N1 C1 1.337(10) . . yes N1 C4 1.333(8) . . yes N2 C2 1.324(9) . . yes N2 C3 1.328(11) . . yes C1 C2 1.369(12) . . no C3 C4 1.380(11) . . no C1 H1 0.9500 . . no C2 H2 0.9500 . . no C3 H3 0.9500 . . no C4 H4 0.9500 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I1 Ga4 I2 116.57(4) . . . yes I1 Ga4 I3 112.09(4) . . . yes I1 Ga4 N1 102.54(16) . . . yes I2 Ga4 I3 113.83(3) . . . yes I2 Ga4 N1 105.09(16) . . . yes I3 Ga4 N1 105.05(17) . . . yes Ga4 N1 C1 123.3(5) . . . yes Ga4 N1 C4 119.7(5) . . . yes C1 N1 C4 117.0(6) . . . yes C2 N2 C3 114.4(7) . . . yes N1 C1 C2 120.0(7) . . . yes N2 C2 C1 124.5(8) . . . yes N2 C3 C4 123.0(7) . . . yes N1 C4 C3 121.0(7) . . . yes N1 C1 H1 120.00 . . . no C2 C1 H1 120.00 . . . no N2 C2 H2 118.00 . . . no C1 C2 H2 118.00 . . . no N2 C3 H3 119.00 . . . no C4 C3 H3 118.00 . . . no N1 C4 H4 120.00 . . . no C3 C4 H4 119.00 . . . no 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 I1 Ga4 N1 C1 -101.1(5) . . . . no I2 Ga4 N1 C1 21.2(6) . . . . no I3 Ga4 N1 C1 141.6(5) . . . . no I1 Ga4 N1 C4 77.1(5) . . . . no I2 Ga4 N1 C4 -160.6(5) . . . . no I3 Ga4 N1 C4 -40.2(5) . . . . no Ga4 N1 C1 C2 177.8(5) . . . . no C4 N1 C1 C2 -0.5(10) . . . . no Ga4 N1 C4 C3 -177.1(5) . . . . no C1 N1 C4 C3 1.2(10) . . . . no C3 N2 C2 C1 0.1(11) . . . . no C2 N2 C3 C4 0.7(11) . . . . no N1 C1 C2 N2 -0.2(12) . . . . no N2 C3 C4 N1 -1.4(11) . . . . no #===END _database_code_depnum_ccdc_archive 'CCDC 927398'