#------------------------------------------------------------------------------ #$Date: 2015-01-23 12:30:19 +0000 (Fri, 23 Jan 2015) $ #$Revision: 130086 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/23/2202389.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_2202389 loop_ _publ_author_name 'Meyer, Gerd' 'Cesur, Nazife' 'Pantenburg, Ingo' _publ_section_title ; Diamminehexabromodiscandium(III) ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first i145 _journal_page_last i146 _journal_paper_doi 10.1107/S1600536803021536 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '[Sc2 Br6 (N H3)2]' _chemical_formula_moiety 'Br6 H6 N2 Sc2' _chemical_formula_structural '[Sc2 Br6 (N H3)2]' _chemical_formula_sum 'Br6 H6 N2 Sc2' _chemical_formula_weight 603.45 _chemical_name_systematic ; Diamminehexabromodiscandium(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 73.07(2) _cell_angle_beta 80.04(2) _cell_angle_gamma 77.82(2) _cell_formula_units_Z 2 _cell_length_a 7.392(2) _cell_length_b 9.578(2) _cell_length_c 9.551(2) _cell_measurement_reflns_used 3629 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 29.75 _cell_measurement_theta_min 1.25 _cell_volume 627.8(3) _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 Details? _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 0.988 _diffrn_measured_fraction_theta_max 0.988 _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 0.072 _diffrn_reflns_av_sigmaI/netI 0.082 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 9270 _diffrn_reflns_theta_full 29.56 _diffrn_reflns_theta_max 29.56 _diffrn_reflns_theta_min 2.25 _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 20.121 _exptl_absorpt_correction_T_max 0.155 _exptl_absorpt_correction_T_min 0.052 _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 3.192 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description column _exptl_crystal_F_000 544 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 1.06 _refine_diff_density_min -1.19 _refine_ls_extinction_coef 0.0021(3) _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 0.789 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 93 _refine_ls_number_reflns 3470 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.789 _refine_ls_R_factor_all 0.095 _refine_ls_R_factor_gt 0.040 _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^)+(0.0430P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.083 _refine_ls_wR_factor_ref 0.096 _reflns_number_gt 1750 _reflns_number_total 3470 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bt6360.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 The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_database_code 2202389 _cod_database_fobs_code 2202389 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 Sc1 0.0800(2) 0.94111(15) 0.69559(16) 0.0309(3) Uani d . 1 . . Sc Br11 -0.21509(14) 1.06539(10) 0.81959(11) 0.0490(2) Uani d . 1 . . Br Br12 0.09954(11) 1.16842(9) 0.45800(9) 0.0363(2) Uani d . 1 . . Br Br1 0.08889(10) 0.69948(9) 0.91996(9) 0.0350(2) Uani d . 1 . . Br Br2 0.40163(10) 0.79309(8) 0.58317(9) 0.0370(2) Uani d . 1 . . Br Sc2 0.4011(2) 0.55114(15) 0.80663(16) 0.0315(3) Uani d . 1 . . Sc Br21 0.41246(11) 0.32866(9) 1.04857(10) 0.0366(2) Uani d . 1 . . Br Br22 0.23220(14) 0.42413(10) 0.68373(11) 0.0479(2) Uani d . 1 . . Br N1 0.2690(11) 1.0360(8) 0.7911(9) 0.0495(19) Uani d . 1 . . N H1A 0.3872 1.0048 0.7601 0.115(19) Uiso calc R 1 . . H H1B 0.2504 1.0063 0.8890 0.115(19) Uiso calc R 1 . . H H1C 0.2442 1.1345 0.7618 0.115(19) Uiso calc R 1 . . H N2 0.6822(10) 0.4583(8) 0.7072(9) 0.0471(18) Uani d . 1 . . N H2A 0.7703 0.4899 0.7367 0.115(19) Uiso calc R 1 . . H H2B 0.6886 0.4883 0.6094 0.115(19) Uiso calc R 1 . . H H2C 0.6990 0.3598 0.7362 0.115(19) 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 Sc1 0.0288(6) 0.0323(7) 0.0310(7) 0.0000(5) -0.0082(5) -0.0085(6) Br11 0.0474(5) 0.0466(5) 0.0440(5) 0.0099(4) -0.0007(4) -0.0140(4) Br12 0.0387(4) 0.0343(4) 0.0369(5) -0.0102(3) -0.0139(3) -0.0027(3) Br1 0.0280(4) 0.0367(4) 0.0328(4) 0.0000(3) -0.0024(3) -0.0022(3) Br2 0.0287(4) 0.0386(5) 0.0337(5) 0.0007(3) -0.0019(3) 0.0001(4) Sc2 0.0300(6) 0.0308(7) 0.0313(7) -0.0003(5) -0.0078(5) -0.0055(6) Br21 0.0360(4) 0.0341(4) 0.0383(5) -0.0083(3) -0.0144(3) -0.0003(3) Br22 0.0609(6) 0.0459(5) 0.0434(5) -0.0131(4) -0.0148(4) -0.0141(4) N1 0.060(5) 0.044(4) 0.050(5) -0.012(3) -0.021(4) -0.011(3) N2 0.043(4) 0.045(4) 0.044(4) 0.009(3) -0.004(3) -0.010(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' N N 0.0061 0.0033 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 Sc1 Br11 . . 93.8(2) yes N1 Sc1 Br1 . . 92.4(2) yes Br11 Sc1 Br1 . . 91.10(6) yes N1 Sc1 Br12 . . 87.8(2) yes Br11 Sc1 Br12 . . 94.50(6) yes Br1 Sc1 Br12 . . 174.38(6) yes N1 Sc1 Br12 . 2_576 170.1(2) yes Br11 Sc1 Br12 . 2_576 94.49(6) yes Br1 Sc1 Br12 . 2_576 92.78(6) yes Br12 Sc1 Br12 . 2_576 86.30(5) yes N1 Sc1 Br2 . . 84.9(2) yes Br11 Sc1 Br2 . . 175.57(7) yes Br1 Sc1 Br2 . . 84.73(5) yes Br12 Sc1 Br2 . . 89.69(6) yes Br12 Sc1 Br2 2_576 . 87.21(5) yes Sc1 Br12 Sc1 . 2_576 93.70(5) yes Sc1 Br1 Sc2 . . 95.32(6) yes Sc2 Br2 Sc1 . . 94.33(6) yes N2 Sc2 Br22 . . 92.8(2) yes N2 Sc2 Br21 . . 92.6(2) yes Br22 Sc2 Br21 . . 92.49(6) yes N2 Sc2 Br2 . . 88.7(2) yes Br22 Sc2 Br2 . . 94.32(6) yes Br21 Sc2 Br2 . . 172.99(6) yes N2 Sc2 Br1 . . 171.1(2) yes Br22 Sc2 Br1 . . 94.51(6) yes Br21 Sc2 Br1 . . 92.25(6) yes Br2 Sc2 Br1 . . 85.59(5) yes N2 Sc2 Br21 . 2_667 86.6(2) yes Br22 Sc2 Br21 . 2_667 176.44(7) yes Br21 Sc2 Br21 . 2_667 84.05(5) yes Br2 Sc2 Br21 . 2_667 89.16(6) yes Br1 Sc2 Br21 . 2_667 86.49(5) yes Sc2 Br21 Sc2 . 2_667 95.95(5) yes Sc1 N1 H1A . . 109.5 no Sc1 N1 H1B . . 109.5 no H1A N1 H1B . . 109.5 no Sc1 N1 H1C . . 109.5 no H1A N1 H1C . . 109.5 no H1B N1 H1C . . 109.5 no Sc2 N2 H2A . . 109.5 no Sc2 N2 H2B . . 109.5 no H2A N2 H2B . . 109.5 no Sc2 N2 H2C . . 109.5 no H2A N2 H2C . . 109.5 no H2B N2 H2C . . 109.5 no 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 Sc1 N1 . 2.252(7) yes Sc1 Br11 . 2.5316(18) yes Sc1 Br1 . 2.6548(18) yes Sc1 Br12 . 2.6555(19) yes Sc1 Br12 2_576 2.6779(17) no Sc1 Br2 . 2.7197(17) yes Br12 Sc1 2_576 2.6779(17) yes Br1 Sc2 . 2.6769(18) yes Br2 Sc2 . 2.6542(18) yes Sc2 N2 . 2.244(7) yes Sc2 Br22 . 2.5293(18) yes Sc2 Br21 . 2.6477(18) yes Sc2 Br21 2_667 2.7190(18) yes Br21 Sc2 2_667 2.7190(18) no N1 H1A . 0.8900 no N1 H1B . 0.8900 no N1 H1C . 0.8900 no N2 H2A . 0.8900 no N2 H2B . 0.8900 no N2 H2C . 0.8900 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 N1 H1B Br11 2_577 0.89 2.64 3.532(8) 175 yes N1 H1C Br22 1_565 0.89 2.64 3.520(8) 170 yes N2 H2B Br22 2_666 0.89 2.68 3.556(8) 171 yes N2 H2C Br11 1_645 0.89 2.66 3.551(7) 174 yes