#------------------------------------------------------------------------------ #$Date: 2011-09-17 23:27:16 +0300 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2212403.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2212403 loop_ _publ_author_name 'Hisanori Yamane' 'Yutaka Mikawa' 'Chiaki Yokoyama' _publ_section_title ; [Ga(NH~3~)~5~Cl]Cl~2~ ; _journal_coeditor_code WM2091 _journal_issue 2 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first i59 _journal_page_last i61 _journal_volume 63 _journal_year 2007 _chemical_formula_moiety 'Cl Ga H15 N5 2+ , 2Cl -' _chemical_formula_structural '[Ga (N H3)5 Cl] Cl2' _chemical_formula_sum 'Cl3 Ga H15 N5' _chemical_formula_weight 261.24 _chemical_name_systematic ; pentaamminechlorogallium(III) dichloride ; _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _audit_creation_method SHELXL97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 13.448(6) _cell_length_b 10.518(5) _cell_length_c 6.750(4) _cell_measurement_reflns_used 7848 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 3.0 _cell_volume 954.8(8) _computing_cell_refinement PROCESS-AUTO _computing_data_collection 'PROCESS-AUTO (Rigaku/MSC, 2005)' _computing_data_reduction 'CrystalStructure (Rigaku/MSC, 2005)' _computing_molecular_graphics 'ATOMS (Dowty, 2005)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution ; coordinates taken from an isotypic structure (Jacobs & Schr\"oder, 2002) ; _diffrn_ambient_temperature 295(3) _diffrn_detector_area_resol_mean 10.00 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID CCD area-detector' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0199 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 8938 _diffrn_reflns_theta_full 27.47 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_theta_min 3.03 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.662 _exptl_absorpt_correction_T_max 0.577 _exptl_absorpt_correction_T_min 0.476 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(NUMABS; Higashi, 1999)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.817 _exptl_crystal_description block _exptl_crystal_F_000 528 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.308 _refine_diff_density_min -0.279 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 82 _refine_ls_number_reflns 1157 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.065 _refine_ls_R_factor_all 0.0248 _refine_ls_R_factor_gt 0.0215 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0282P)^2^+0.3606P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.0533 _reflns_number_gt 1041 _reflns_number_total 1157 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file wm2091.cif loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z+1/2' 'x, -y+1/2, z' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z-1/2' '-x, y-1/2, -z' 'x-1/2, y, -z-1/2' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 2.09 4.11 -11.65 0.0842 -1.54 -7.25 9.24 0.0970 -2.35 -1.12 12.52 0.0766 1.13 8.65 -7.29 0.1088 -0.18 1.36 -13.33 0.0680 0.28 -2.96 -12.89 0.0868 1.04 -9.93 -3.87 0.1352 1.03 -9.64 4.94 0.1231 0.04 -0.04 13.45 0.0453 -0.63 6.28 10.70 0.0707 -0.47 4.12 -12.33 0.0855 -5.94 0.01 -6.38 0.0970 -4.41 -5.41 -7.46 0.1133 4.92 -7.06 1.75 0.1040 4.94 4.21 7.42 0.0866 3.27 7.29 7.17 0.0906 -1.44 9.91 3.42 0.1200 -5.19 6.45 -2.35 0.1062 5.72 -5.01 -3.07 0.0946 6.71 0.35 -1.31 0.0760 5.48 6.08 1.05 0.0877 0.30 10.11 3.64 0.1179 -3.66 -8.80 -0.94 0.1116 -5.73 -5.47 1.30 0.1064 -4.78 6.42 4.74 0.1020 -1.28 9.84 3.97 0.1181 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' N N 0.0061 0.0033 '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' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy Cl Cl1 -0.02810(5) 0.2500 -0.05178(10) 0.02976(15) Uani d S 1 Cl Cl2 0.35244(3) 0.00215(5) 0.16337(7) 0.03187(13) Uani d . 1 Ga Ga1 0.104663(19) 0.2500 0.18229(4) 0.02031(10) Uani d S 1 N N1 0.2066(2) 0.2500 -0.0481(4) 0.0354(6) Uani d S 1 N N2 0.0042(2) 0.2500 0.4150(4) 0.0326(5) Uani d S 1 N N3 0.2209(2) 0.2500 0.3846(4) 0.0314(5) Uani d S 1 N N4 0.10274(15) 0.05470(17) 0.1783(3) 0.0319(4) Uani d . 1 H H1 0.262(5) 0.2500 -0.006(11) 0.12(2) Uiso d S 1 H H2 0.198(3) 0.194(3) -0.121(5) 0.098(14) Uiso d . 1 H H3 0.033(4) 0.2500 0.528(9) 0.11(2) Uiso d S 1 H H4 -0.027(2) 0.192(3) 0.407(4) 0.067(10) Uiso d . 1 H H5 0.277(4) 0.2500 0.342(7) 0.089(19) Uiso d S 1 H H6 0.215(3) 0.189(3) 0.466(6) 0.107(14) Uiso d . 1 H H7 0.047(3) 0.024(3) 0.207(5) 0.071(10) Uiso d . 1 H H8 0.113(2) 0.027(3) 0.074(6) 0.069(11) Uiso d . 1 H H9 0.145(3) 0.022(4) 0.249(7) 0.113(15) Uiso d . 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cl1 0.0294(3) 0.0296(3) 0.0303(3) 0.000 -0.0078(3) 0.000 Cl2 0.0335(2) 0.0295(2) 0.0326(3) -0.00100(19) -0.00102(18) -0.00154(18) Ga1 0.02220(15) 0.01730(14) 0.02142(15) 0.000 -0.00078(9) 0.000 N1 0.0349(14) 0.0393(14) 0.0319(14) 0.000 0.0061(11) 0.000 N2 0.0347(13) 0.0330(13) 0.0299(15) 0.000 0.0050(11) 0.000 N3 0.0289(12) 0.0299(12) 0.0354(13) 0.000 -0.0109(10) 0.000 N4 0.0363(9) 0.0216(8) 0.0378(10) -0.0013(7) -0.0046(8) -0.0014(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Cl1 Ga1 2.3840(11) yes Ga1 N4 2.055(2) yes Ga1 N2 2.072(3) yes Ga1 N1 2.073(3) yes Ga1 N3 2.076(3) yes N1 H1 0.79(6) ? N1 H2 0.77(4) ? N2 H3 0.85(6) ? N2 H4 0.74(3) ? N3 H5 0.81(6) ? N3 H6 0.85(4) ? N4 H7 0.83(4) ? N4 H8 0.77(4) ? N4 H9 0.81(5) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 Ga1 N3 . . 89.73(13) yes N1 Ga1 Cl1 . . 89.89(10) yes N2 Ga1 N3 . . 89.57(13) yes N2 Ga1 N1 . . 179.30(13) yes N2 Ga1 Cl1 . . 90.80(10) yes N3 Ga1 Cl1 . . 179.63(9) yes N4 Ga1 N4 . 3 177.91(12) yes N4 Ga1 N2 . . 90.10(6) yes N4 Ga1 N2 3 . 90.10(6) ? N4 Ga1 N1 . . 89.91(6) yes N4 Ga1 N1 3 . 89.91(6) ? N4 Ga1 N3 . . 91.04(6) yes N4 Ga1 N3 3 . 91.04(6) ? N4 Ga1 Cl1 . . 88.96(6) yes N4 Ga1 Cl1 3 . 88.96(6) ? H1 N1 H2 . . 111(4) ? H2 N1 H2 3 . 99(5) ? H3 N2 H4 . . 109(3) ? H4 N2 H4 3 . 110(5) ? H5 N3 H6 . . 109(3) ? H6 N3 H6 3 . 98(5) ? H7 N4 H8 . . 103(3) ? H7 N4 H9 . . 109(4) ? H8 N4 H9 . . 105(4) ? Ga1 N1 H2 . . 112(3) ? Ga1 N1 H1 . . 111(5) ? Ga1 N2 H3 . . 113(4) ? Ga1 N2 H4 . . 109(2) ? Ga1 N3 H5 . . 118(4) ? Ga1 N3 H6 . . 111(3) ? Ga1 N4 H7 . . 113(2) ? Ga1 N4 H8 . . 112(3) ? Ga1 N4 H9 . . 114(3) ? H2 N1 Ga1 3 . 112(3) ? H4 N2 Ga1 3 . 109(2) ? H6 N3 Ga1 3 . 111(3) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N1 H1 Cl2 . 0.79(6) 3.10(4) 3.561(3) 120.0(16) N1 H2 Cl2 4_554 0.77(4) 2.62(4) 3.385(2) 172(4) N2 H3 Cl2 4 0.85(6) 3.20(3) 3.683(3) 118.2(17) N2 H4 Cl2 8_556 0.74(3) 2.61(3) 3.353(2) 172(3) N3 H5 Cl2 . 0.81(6) 3.04(3) 3.486(2) 116.9(16) N3 H6 Cl2 4 0.85(4) 2.58(4) 3.398(2) 164(3) N4 H7 Cl2 8_556 0.83(4) 2.77(4) 3.575(3) 162(3) N4 H8 Cl2 4_554 0.77(4) 2.83(4) 3.578(3) 164(3) N4 H9 Cl2 4 0.81(5) 2.81(5) 3.383(3) 129(4) N4 H9 Cl2 . 0.81(5) 2.86(4) 3.405(3) 126(4) _cod_database_code 2212403