#------------------------------------------------------------------------------ #$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/23/2202388.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_2202388 loop_ _publ_author_name 'Meyer, Gerd' 'Cesur, Nazife' 'Bremm, Stephan' _publ_section_title ; Tetraamminehexabromodiscandium(III) ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first i142 _journal_page_last i144 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '[Sc2 Br6 (N H3)4]' _chemical_formula_moiety 'Br6 H12 N4 Sc2' _chemical_formula_structural '[Sc2 Br6 (N H3)4]' _chemical_formula_sum 'Br6 H12 N4 Sc2' _chemical_formula_weight 637.52 _chemical_name_systematic ; Tetraamminehexabromodiscandium(III) ; _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 SHELXL97 _cell_angle_alpha 105.39(2) _cell_angle_beta 90.76(2) _cell_angle_gamma 109.85(2) _cell_formula_units_Z 2 _cell_length_a 7.211(2) _cell_length_b 10.157(3) _cell_length_c 11.350(3) _cell_measurement_reflns_used 2678 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 29.65 _cell_measurement_theta_min 1.87 _cell_volume 749.0(4) _computing_cell_refinement X-AREA _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction X-AREA _computing_molecular_graphics 'DIAMOND (Brandenburg, 1996)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 'not measured' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method '\w and \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 0.077 _diffrn_reflns_av_sigmaI/netI 0.141 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 6953 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 1.87 _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 16.878 _exptl_absorpt_correction_T_max 0.148 _exptl_absorpt_correction_T_min 0.100 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; the absorption correction (X-RED; Stoe & Cie, 2001) was performed after optimizing the crystal shape using X-SHAPE (Stoe & Cie, 1999) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.827 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description column _exptl_crystal_F_000 584 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.66 _refine_diff_density_min -0.70 _refine_ls_extinction_coef 0.00190(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)' _refine_ls_goodness_of_fit_ref 0.700 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 111 _refine_ls_number_reflns 2938 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.700 _refine_ls_R_factor_all 0.118 _refine_ls_R_factor_gt 0.039 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0201P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.066 _refine_ls_wR_factor_ref 0.081 _reflns_number_gt 1237 _reflns_number_total 2938 _reflns_threshold_expression I>2s(I) _[local]_cod_data_source_file bt6359.cif _[local]_cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_chemical_melting_point' value 'unknown' was changed to '?' - the value is undefined or not given. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana The following automatic conversions were performed: '_chemical_melting_point' value 'unknown' was changed to '?' - the value is undefined or not given. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2202388 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 Br21 0.1258(2) 0.40251(16) 0.34540(12) 0.0546(4) Uani d . 1 . . Br Br11 -0.14637(19) -0.42322(15) 0.13769(11) 0.0521(4) Uani d . 1 . . Br Br1 -0.0130(2) -0.01176(15) 0.24330(12) 0.0481(3) Uani d . 1 . . Br Br2 0.5115(2) 0.02968(14) 0.25850(12) 0.0486(4) Uani d . 1 . . Br Br23 0.33607(19) 0.22062(15) 0.53367(11) 0.0511(4) Uani d . 1 . . Br Br22 0.3424(2) 0.22896(17) 0.07698(11) 0.0558(4) Uani d . 1 . . Br Sc1 0.1727(3) -0.2021(3) 0.1969(2) 0.0415(5) Uani d . 1 . . Sc Sc2 0.3187(3) 0.2260(3) 0.3042(2) 0.0394(5) Uani d . 1 . . Sc N13 0.1770(14) -0.1951(11) 0.3998(8) 0.052(3) Uani d . 1 . . N H13A 0.2940 -0.1334 0.4400 0.117(16) Uiso calc R 1 . . H H13B 0.1576 -0.2840 0.4066 0.117(16) Uiso calc R 1 . . H H13C 0.0812 -0.1653 0.4317 0.117(16) Uiso calc R 1 . . H N11 0.1814(14) -0.1890(11) 0.0005(8) 0.051(3) Uani d . 1 . . N H11A 0.3022 -0.1796 -0.0215 0.117(16) Uiso calc R 1 . . H H11B 0.1524 -0.1121 -0.0047 0.117(16) Uiso calc R 1 . . H H11C 0.0930 -0.2701 -0.0494 0.117(16) Uiso calc R 1 . . H N21 0.6158(15) 0.3995(11) 0.3506(9) 0.052(3) Uani d . 1 . . N H21A 0.6266 0.4603 0.3051 0.117(16) Uiso calc R 1 . . H H21B 0.7083 0.3593 0.3356 0.117(16) Uiso calc R 1 . . H H21C 0.6320 0.4487 0.4299 0.117(16) Uiso calc R 1 . . H N12 0.3669(15) -0.3404(11) 0.1667(8) 0.053(3) Uani d . 1 . . N H12A 0.2912 -0.4341 0.1522 0.117(16) Uiso calc R 1 . . H H12B 0.4524 -0.3132 0.2335 0.117(16) Uiso calc R 1 . . H H12C 0.4334 -0.3283 0.1025 0.117(16) 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 Br21 0.0542(9) 0.0524(9) 0.0616(8) 0.0289(7) 0.0031(6) 0.0107(7) Br11 0.0482(8) 0.0467(8) 0.0525(7) 0.0078(7) 0.0048(6) 0.0116(6) Br1 0.0359(6) 0.0443(8) 0.0604(8) 0.0142(6) 0.0044(5) 0.0090(6) Br2 0.0362(6) 0.0433(8) 0.0626(8) 0.0160(6) 0.0046(5) 0.0068(6) Br23 0.0578(8) 0.0577(9) 0.0392(6) 0.0215(7) 0.0062(6) 0.0148(6) Br22 0.0556(8) 0.0706(10) 0.0404(7) 0.0194(7) 0.0068(6) 0.0185(6) Sc1 0.0406(12) 0.0385(13) 0.0446(10) 0.0144(10) 0.0057(9) 0.0101(10) Sc2 0.0378(11) 0.0396(13) 0.0396(10) 0.0141(10) 0.0045(8) 0.0090(9) N13 0.044(6) 0.059(7) 0.054(6) 0.017(5) 0.006(5) 0.019(5) N11 0.050(6) 0.049(7) 0.047(6) 0.012(5) 0.004(4) 0.010(5) N21 0.052(7) 0.047(6) 0.054(6) 0.014(5) 0.012(5) 0.011(5) N12 0.067(7) 0.045(6) 0.058(6) 0.035(5) 0.013(5) 0.013(5) 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 Br21 Sc2 . 2.575(3) yes Br11 Sc1 . 2.538(3) yes Br1 Sc1 . 2.654(3) yes Br1 Sc2 . 2.679(3) yes Br2 Sc1 . 2.679(3) yes Br2 Sc2 . 2.745(3) yes Br23 Sc2 . 2.622(3) yes Br22 Sc2 . 2.594(3) yes Sc1 N11 . 2.269(9) yes Sc1 N12 . 2.269(9) yes Sc1 N13 . 2.284(10) yes Sc2 N21 . 2.211(10) yes N13 H13A . 0.8900 no N13 H13B . 0.8900 no N13 H13C . 0.8900 no N11 H11A . 0.8900 no N11 H11B . 0.8900 no N11 H11C . 0.8900 no N21 H21A . 0.8900 no N21 H21B . 0.8900 no N21 H21C . 0.8900 no N12 H12A . 0.8900 no N12 H12B . 0.8900 no N12 H12C . 0.8900 no 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' H H 0.0000 0.0000 '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' Sc Sc 0.2519 0.3716 '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 _geom_angle_publ_flag Sc1 Br1 Sc2 95.35(9) yes Sc1 Br2 Sc2 93.25(8) yes N11 Sc1 N12 91.6(4) yes N11 Sc1 N13 175.3(4) yes N12 Sc1 N13 90.5(3) yes N11 Sc1 Br11 91.6(3) yes N12 Sc1 Br11 93.2(3) yes N13 Sc1 Br11 92.4(3) yes N11 Sc1 Br1 89.0(3) yes N12 Sc1 Br1 172.8(3) yes N13 Sc1 Br1 88.4(3) yes Br11 Sc1 Br1 93.95(9) yes N11 Sc1 Br2 88.2(3) yes N12 Sc1 Br2 86.3(3) yes N13 Sc1 Br2 87.7(3) yes Br11 Sc1 Br2 179.43(12) yes Br1 Sc1 Br2 86.61(9) yes N21 Sc2 Br21 95.2(3) yes N21 Sc2 Br22 87.9(3) yes Br21 Sc2 Br22 92.64(9) yes N21 Sc2 Br23 87.8(3) yes Br21 Sc2 Br23 92.89(8) yes Br22 Sc2 Br23 173.27(10) yes N21 Sc2 Br1 171.6(3) yes Br21 Sc2 Br1 93.17(9) yes Br22 Sc2 Br1 92.17(9) yes Br23 Sc2 Br1 91.35(9) yes N21 Sc2 Br2 86.8(3) yes Br21 Sc2 Br2 177.95(11) yes Br22 Sc2 Br2 87.55(8) yes Br23 Sc2 Br2 87.06(8) yes Br1 Sc2 Br2 84.79(9) yes Sc1 N13 H13A 109.5 no Sc1 N13 H13B 109.5 no H13A N13 H13B 109.5 no Sc1 N13 H13C 109.5 no H13A N13 H13C 109.5 no H13B N13 H13C 109.5 no Sc1 N11 H11A 109.5 no Sc1 N11 H11B 109.5 no H11A N11 H11B 109.5 no Sc1 N11 H11C 109.5 no H11A N11 H11C 109.5 no H11B N11 H11C 109.5 no Sc2 N21 H21A 109.5 no Sc2 N21 H21B 109.5 no H21A N21 H21B 109.5 no Sc2 N21 H21C 109.5 no H21A N21 H21C 109.5 no H21B N21 H21C 109.5 no Sc1 N12 H12A 109.5 no Sc1 N12 H12B 109.5 no H12A N12 H12B 109.5 no Sc1 N12 H12C 109.5 no H12A N12 H12C 109.5 no H12B N12 H12C 109.5 no 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 _geom_hbond_publ_flag N13 H13A Br23 2_656 0.89 3.12 3.690(10) 124.1 yes N13 H13B Br21 1_545 0.89 3.00 3.854(11) 161.3 yes N13 H13C Br23 2_556 0.89 2.92 3.722(9) 150.9 yes N11 H11A Br22 2_655 0.89 2.82 3.684(9) 163.3 yes N11 H11B Br22 . 0.89 3.13 3.846(11) 139.4 yes N21 H21A Br11 1_665 0.89 2.77 3.514(10) 142.5 yes N21 H21B Br21 1_655 0.89 2.89 3.669(10) 147.5 yes N21 H21C Br21 2_666 0.89 2.81 3.609(10) 150.5 yes N12 H12A Br21 1_545 0.89 3.11 3.712(10) 127.2 yes N12 H12B Br23 2_656 0.89 2.79 3.671(10) 169.7 yes N12 H12C Br22 2_655 0.89 2.80 3.678(9) 168.2 yes _cod_database_fobs_code 2202388 _journal_paper_doi 10.1107/S1600536803021524