# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2187 data_CRYSTALS_cif _audit_creation_date 00-05-11 _audit_creation_method CRYSTALS # [H2NCH2CH2NH2]0.5[Cu2SbS3] at 150K #**************************************************************************** # The contents of this file between this point and the next #***** line # are held in the file CRYSTALS\SCRIPT\REF.CIF # This is a character file which you may edit to reflect local # conditions # # 1. SUBMISSION DETAILS _publ_contact_author_name 'A.V. Powell' _publ_contact_author_address ; Department of Chemistry Heriot-Watt University Edinburgh EH14 4AS ; _publ_contact_author_phone ' 0131 451 8034 ' _publ_contact_author_fax ' 0131 451 3180 ' _publ_contact_author_email 'a.v.powell@hw.ac.uk ' #============================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; A new mixed-valence copper antimony sulfide ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Powell, A. V.' ; to whom correspondence should be addressed ; ; Department of Chemistry Heriot-Watt University Edinburgh EH14 4AS ; 'Boissiere, S.' ? ; Department of Chemistry Heriot-Watt University Edinburgh EH14 4AS ; 'Chippindale, A.M.' ? ; Department of Chemistry University of Reading Reading RG6 6AD ; #============================================================================== # 4. TEXT _publ_section_exptl_refinement ; H atoms placed geometrically after each cycle ; ## -----------------REFERENCES ----------------------## _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. 27, 435. ATOMS for Windows v4.0, Shape Software, 521 Hidden Valley Road, Kingsport TN, USA Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods in Enzymology 276, Ed Carter, C.W. & Sweet, R.M., Academic Press. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; #========================================================================== # Diffractometer details #========================================================================== _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' Enraf-Nonius DIP2020 ' _computing_data_collection 'DIP2000 software Xpress (MAC Science, 1989)' _computing_data_reduction ; DIP2000 software DENZO (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DIP2000 software DENZO (Otwinowski & Minor, 1996) ; #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; ATOMS for Windows v4.0 Cameron ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' #========================================================================== _chemical_name_systematic ; ethylenediamine copper-antimony sulphide ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary Direct_Methods _atom_sites_solution_hydrogens Geometric _refine_ls_hydrogen_treatment ; noref ; #**************************************************************************** _cell_length_a 6.101(1) _cell_angle_alpha 90 _cell_length_b 18.445(3) _cell_angle_beta 112.92(1) _cell_length_c 6.518(1) _cell_angle_gamma 90 _cell_volume 675.56 _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'Cu ' 0.2630 1.2660 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126 1.1910 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'S ' 0.1100 0.1240 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International_Tables_Vol_IV_Table_2.2B' 'Sb ' -0.8160 1.5460 19.6418 5.3034 19.0455 0.4607 5.0371 27.9074 2.6827 75.2825 4.5909 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C1 H4 Sb1 Cu2 S3 N1 ' _chemical_formula_moiety ' C1 H4 Sb1 Cu2 S3 N1 ' _chemical_compound_source ; solvothermal synthesis ; _chemical_formula_weight 375.06 _cell_measurement_reflns_used 2759 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _cell_formula_units_Z 4.00 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' orange ' _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 3.69 _exptl_crystal_density_meas ? _exptl_crystal_F_000 696.04 _exptl_absorpt_coefficient_mu 11.05 _exptl_absorpt_correction_type NONE _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 2759 _reflns_number_total 1327 _diffrn_reflns_av_R_equivalents 0.059 _reflns_number_observed 1128 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 26.57 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 7 _reflns_limit_h_min -7 _reflns_limit_h_max 7 _reflns_limit_k_min 0 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 8 _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -2.43 _refine_diff_density_max 2.71 _refine_ls_number_reflns 1128 _refine_ls_number_parameters 73 _refine_ls_R_factor_obs 0.0553 _refine_ls_wR_factor_obs 0.0645 _refine_ls_goodness_of_fit_obs 1.0875 _refine_ls_shift/esd_max 0.000257 _refine_ls_structure_factor_coef F _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method \wA loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type SB1 0.83273(7) 0.19588(2) -0.07618(7) 0.0095 1.0000 Uani CU1 0.9317(1) 0.32821(5) -0.1782(1) 0.0141 1.0000 Uani CU2 0.8988(2) 0.18099(5) 0.4182(2) 0.0167 1.0000 Uani S1 1.0640(3) 0.11314(9) 0.2170(3) 0.0119 1.0000 Uani S2 0.7298(3) 0.11300(9) -0.3902(3) 0.0118 1.0000 Uani S3 0.4572(3) 0.19842(8) -0.0237(3) 0.0120 1.0000 Uani N1 1.227(1) 0.5442(3) -0.248(1) 0.0176 1.0000 Uani C1 1.030(1) 0.4958(4) -0.377(1) 0.0182 1.0000 Uani H11 1.2643 0.5382 -0.0856 0.0170 1.0000 Uiso H12 1.1799 0.5957 -0.2924 0.0170 1.0000 Uiso H101 0.8864 0.5082 -0.3448 0.0180 1.0000 Uiso H102 1.0771 0.4444 -0.3318 0.0180 1.0000 Uiso 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 SB1 0.0085(3) 0.0139(4) 0.0062(4) 0.0009(1) -0.0003(3) -0.0004(1) CU1 0.0111(5) 0.0200(5) 0.0110(5) -0.0007(3) -0.0010(4) -0.0015(3) CU2 0.0176(5) 0.0193(5) 0.0143(5) -0.0011(3) 0.0067(4) -0.0017(3) S1 0.0107(7) 0.0179(8) 0.0077(7) 0.0013(5) 0.0005(6) 0.0015(5) S2 0.0107(7) 0.0158(8) 0.0082(7) 0.0004(5) 0.0001(6) 0.0004(6) S3 0.0099(8) 0.0181(9) 0.0089(8) 0.0008(5) 0.0024(7) 0.0012(5) N1 0.013(3) 0.024(3) 0.015(3) -0.003(2) 0.001(3) -0.003(2) C1 0.016(3) 0.015(3) 0.024(4) -0.001(3) 0.003(3) -0.005(3) _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag SB1 . CU1 . 2.6605(9) yes SB1 . CU2 . 3.100(1) yes SB1 . S1 . 2.423(2) yes SB1 . S2 . 2.433(2) yes SB1 . S3 . 2.445(2) yes CU1 . CU2 4_554 2.674(1) yes CU1 . S1 4_454 2.340(2) yes CU1 . S2 4_555 2.313(2) yes CU1 . S3 4_554 2.368(2) yes CU2 . S1 . 2.309(2) yes CU2 . S2 1_556 2.280(2) yes CU2 . S3 4_555 2.261(2) yes N1 . C1 . 1.470(9) yes N1 . H11 . 1.000(6) no N1 . H12 . 1.000(6) no C1 . C1 2_764 1.51(2) yes C1 . H101 . 1.000(7) no C1 . H102 . 1.000(7) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag CU1 . SB1 . CU2 . 113.01(3) no CU1 . SB1 . S1 . 130.98(5) no CU2 . SB1 . S1 . 47.51(4) no CU1 . SB1 . S2 . 112.05(4) no CU2 . SB1 . S2 . 134.85(4) no S1 . SB1 . S2 . 98.50(5) no CU1 . SB1 . S3 . 109.50(4) no CU2 . SB1 . S3 . 66.78(4) no S1 . SB1 . S3 . 101.03(5) no S2 . SB1 . S3 . 100.43(5) no SB1 . CU1 . CU2 4_554 102.00(3) no SB1 . CU1 . S1 4_454 102.24(5) no CU2 4_554 CU1 . S1 4_454 155.61(6) no SB1 . CU1 . S2 4_555 114.24(5) no CU2 4_554 CU1 . S2 4_555 53.83(5) no S1 4_454 CU1 . S2 4_555 112.43(6) no SB1 . CU1 . S3 4_554 98.79(5) no CU2 4_554 CU1 . S3 4_554 75.62(5) no S1 4_454 CU1 . S3 4_554 103.23(7) no S2 4_555 CU1 . S3 4_554 123.16(7) no SB1 . CU2 . CU1 4_455 93.79(3) no SB1 . CU2 . S1 . 50.69(4) no CU1 4_455 CU2 . S1 . 119.55(6) no SB1 . CU2 . S2 1_556 135.62(6) no CU1 4_455 CU2 . S2 1_556 54.97(5) no S1 . CU2 . S2 1_556 113.80(7) no SB1 . CU2 . S3 4_555 92.02(5) no CU1 4_455 CU2 . S3 4_555 100.71(6) no S1 . CU2 . S3 4_555 123.58(7) no S2 1_556 CU2 . S3 4_555 121.65(7) no SB1 . S1 . CU1 4_555 97.85(6) no SB1 . S1 . CU2 . 81.80(6) no CU1 4_555 S1 . CU2 . 99.48(7) no SB1 . S2 . CU1 4_454 104.60(6) no SB1 . S2 . CU2 1_554 95.26(6) no CU1 4_454 S2 . CU2 1_554 71.20(6) no SB1 . S3 . CU1 4_455 122.77(8) no SB1 . S3 . CU2 4_454 95.20(6) no CU1 4_455 S3 . CU2 4_454 107.39(7) no C1 . N1 . H11 . 109.5(6) no C1 . N1 . H12 . 109.5(5) no H11 . N1 . H12 . 109.5(5) no N1 . C1 . C1 2_764 110.2(7) no N1 . C1 . H101 . 109.3(6) no C1 2_764 C1 . H101 . 109.3(8) no N1 . C1 . H102 . 109.3(6) no C1 2_764 C1 . H102 . 109.3(8) no H101 . C1 . H102 . 109.5(7) no