#------------------------------------------------------------------------------ #$Date: 2015-02-25 13:01:53 +0000 (Wed, 25 Feb 2015) $ #$Revision: 132410 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/23/2202313.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_2202313 loop_ _publ_author_name 'Bremm, Stephan' 'Meyer, Gerd' _publ_section_title ; Triamminetrichloroindium(III), [InCl~3~(NH~3~)~3~] ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first i110 _journal_page_last i111 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '2[In Cl3 (N H3)3]' _chemical_formula_moiety '[In(NH~3~)~4~Cl~2~]^+^ , [In(NH~3~)~2~Cl~4~]^-^' _chemical_formula_sum 'Cl6 H18 In2 N6' _chemical_formula_weight 544.54 _chemical_name_systematic ? _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 86.14(3) _cell_angle_beta 86.68(3) _cell_angle_gamma 85.26(3) _cell_formula_units_Z 1 _cell_length_a 5.8652(15) _cell_length_b 6.8130(18) _cell_length_c 9.794(2) _cell_measurement_reflns_used 1719 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26 _cell_measurement_theta_min 1.9 _cell_volume 388.60(17) _computing_cell_refinement IPDS _computing_data_collection 'IPDS (Stoe & Cie, 1996-1997)' _computing_data_reduction IPDS _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.806 _diffrn_measured_fraction_theta_max 0.806 _diffrn_measurement_device_type 'Stoe Imaging Plate Diffraction System' _diffrn_measurement_method \f _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 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0214 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 1719 _diffrn_reflns_theta_full 25.99 _diffrn_reflns_theta_max 25.99 _diffrn_reflns_theta_min 3.49 _diffrn_standards_decay_% 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_interval_time 'not measured' _diffrn_standards_number 'not measured' _exptl_absorpt_coefficient_mu 3.978 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.327 _exptl_crystal_density_method 'not measured' _exptl_crystal_description irregular _exptl_crystal_F_000 260 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.812 _refine_diff_density_min -0.749 _refine_ls_extinction_coef 0.023(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 68 _refine_ls_number_reflns 1234 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.958 _refine_ls_R_factor_all 0.0332 _refine_ls_R_factor_gt 0.0282 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0559P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0707 _refine_ls_wR_factor_ref 0.0727 _reflns_number_gt 1049 _reflns_number_total 1234 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bt6243.cif _[local]_cod_data_source_block I _[local]_cod_chemical_formula_sum_orig 'H18 Cl6 In2 N6' _cod_original_cell_volume 388.59(17) _cod_database_code 2202313 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _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 _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol In1 0.0000 0.5000 0.0000 0.02408(19) Uani d S 1 . . In In2 0.5000 0.0000 0.5000 0.02292(18) Uani d S 1 . . In Cl1 -0.2706(2) 0.00305(19) 0.27341(11) 0.0342(3) Uani d . 1 . . Cl Cl2 -0.2624(2) 0.69134(17) 0.58217(13) 0.0361(3) Uani d . 1 . . Cl Cl3 0.28373(19) 0.70997(17) 0.08736(12) 0.0326(3) Uani d . 1 . . Cl N1 0.7470(7) 0.1896(6) 0.5817(4) 0.0301(8) Uani d . 1 . . N H1A 0.7116 0.3152 0.5545 0.045 Uiso calc R 1 . . H H1B 0.8884 0.1528 0.5502 0.045 Uiso calc R 1 . . H H1C 0.7395 0.1763 0.6728 0.045 Uiso calc R 1 . . H N2 0.7969(7) 0.7762(6) 0.9238(5) 0.0342(8) Uani d . 1 . . N H2A 0.7155 0.7495 0.8544 0.051 Uiso calc R 1 . . H H2B 0.8920 0.8676 0.8956 0.051 Uiso calc R 1 . . H H2C 0.7027 0.8209 0.9914 0.051 Uiso calc R 1 . . H N3 0.1954(7) 0.4972(6) 0.7946(4) 0.0333(8) Uani d . 1 . . N H3A 0.2994 0.5857 0.7905 0.050 Uiso calc R 1 . . H H3B 0.0986 0.5271 0.7282 0.050 Uiso calc R 1 . . H H3C 0.2652 0.3777 0.7841 0.050 Uiso calc R 1 . . H 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 In1 0.0245(2) 0.0224(3) 0.0253(3) -0.00095(17) -0.00252(15) -0.00183(16) In2 0.0231(2) 0.0210(2) 0.0250(3) -0.00240(16) -0.00260(15) -0.00150(16) Cl1 0.0376(6) 0.0348(6) 0.0299(5) -0.0048(5) 0.0052(4) -0.0026(5) Cl2 0.0360(6) 0.0267(5) 0.0448(6) 0.0026(5) -0.0098(5) 0.0024(5) Cl3 0.0313(5) 0.0334(6) 0.0351(5) -0.0077(5) -0.0045(4) -0.0071(4) N1 0.0292(18) 0.0283(19) 0.0341(18) -0.0049(16) -0.0037(15) -0.0067(16) N2 0.0328(19) 0.0251(18) 0.043(2) 0.0031(17) -0.0014(17) -0.0001(17) N3 0.0342(19) 0.032(2) 0.0326(19) 0.0001(17) 0.0031(16) -0.0048(17) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag In1 N2 1_454 2.250(4) ? In1 N2 2_666 2.250(4) ? In1 N3 1_554 2.258(4) ? In1 N3 2_566 2.258(4) ? In1 Cl3 2_565 2.5043(12) ? In1 Cl3 . 2.5043(12) ? In2 N1 2_656 2.234(3) ? In2 N1 . 2.234(3) ? In2 Cl1 1_655 2.5276(14) ? In2 Cl1 2_556 2.5276(14) ? In2 Cl2 1_645 2.5355(15) ? In2 Cl2 2_566 2.5355(15) ? Cl1 In2 1_455 2.5276(14) ? Cl2 In2 1_465 2.5355(15) ? N1 H1A . 0.8900 ? N1 H1B . 0.8900 ? N1 H1C . 0.8900 ? N2 In1 1_656 2.250(4) ? N2 H2A . 0.8900 ? N2 H2B . 0.8900 ? N2 H2C . 0.8900 ? N3 In1 1_556 2.258(4) ? N3 H3A . 0.8900 ? N3 H3B . 0.8900 ? N3 H3C . 0.8900 ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_ _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 N2 In1 N2 1_454 2_666 180.0 N2 In1 N3 1_454 1_554 88.70(17) N2 In1 N3 2_666 1_554 91.30(17) N2 In1 N3 1_454 2_566 91.30(17) N2 In1 N3 2_666 2_566 88.70(17) N3 In1 N3 1_554 2_566 180.0(2) N2 In1 Cl3 1_454 2_565 90.97(11) N2 In1 Cl3 2_666 2_565 89.03(11) N3 In1 Cl3 1_554 2_565 89.59(11) N3 In1 Cl3 2_566 2_565 90.41(11) N2 In1 Cl3 1_454 . 89.03(11) N2 In1 Cl3 2_666 . 90.97(11) N3 In1 Cl3 1_554 . 90.41(11) N3 In1 Cl3 2_566 . 89.59(11) Cl3 In1 Cl3 2_565 . 180.00(5) N1 In2 N1 2_656 . 180.0000(10) N1 In2 Cl1 2_656 1_655 90.33(11) N1 In2 Cl1 . 1_655 89.67(11) N1 In2 Cl1 2_656 2_556 89.67(11) N1 In2 Cl1 . 2_556 90.33(11) Cl1 In2 Cl1 1_655 2_556 180.0 N1 In2 Cl2 2_656 1_645 89.31(12) N1 In2 Cl2 . 1_645 90.69(12) Cl1 In2 Cl2 1_655 1_645 89.88(5) Cl1 In2 Cl2 2_556 1_645 90.12(5) N1 In2 Cl2 2_656 2_566 90.69(12) N1 In2 Cl2 . 2_566 89.31(12) Cl1 In2 Cl2 1_655 2_566 90.12(5) Cl1 In2 Cl2 2_556 2_566 89.88(5) Cl2 In2 Cl2 1_645 2_566 180.00(6) In2 N1 H1A . . 109.5 In2 N1 H1B . . 109.5 H1A N1 H1B . . 109.5 In2 N1 H1C . . 109.5 H1A N1 H1C . . 109.5 H1B N1 H1C . . 109.5 In1 N2 H2A 1_656 . 109.5 In1 N2 H2B 1_656 . 109.5 H2A N2 H2B . . 109.5 In1 N2 H2C 1_656 . 109.5 H2A N2 H2C . . 109.5 H2B N2 H2C . . 109.5 In1 N3 H3A 1_556 . 109.5 In1 N3 H3B 1_556 . 109.5 H3A N3 H3B . . 109.5 In1 N3 H3C 1_556 . 109.5 H3A N3 H3C . . 109.5 H3B N3 H3C . . 109.5 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 H1A Cl2 1_655 0.89 2.61 3.415(4) 150 N1 H1B Cl2 2_666 0.89 2.74 3.470(4) 141 N1 H1C Cl3 2_666 0.89 2.52 3.349(4) 156 N2 H2A Cl2 1_655 0.89 2.72 3.476(5) 144 N2 H2B Cl1 2_666 0.89 2.85 3.659(5) 151 N2 H2C Cl3 1_556 0.89 2.73 3.376(5) 131 N3 H3A Cl1 2_566 0.89 2.82 3.484(5) 132 N3 H3B Cl2 . 0.89 2.74 3.602(4) 163 N3 H3C Cl1 2_556 0.89 2.69 3.504(5) 153 _cod_database_fobs_code 2202313 _journal_paper_doi 10.1107/S1600536803013539