# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef 'purple_final_mmo_ccdc_deposit.cif' #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2010-07-17 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ; ? 2010-07-20 # Formatted by publCIF ; #============================================================================== # # SUBMISSION DETAILS _publ_contact_author_name 'Patra, Apurba K.' # Name of author for correspondence Patra, Apurba K. _publ_contact_author_address ;Department of Chemistry National Institute of Technology, Durgapur Durgapur 713 209 West Bengal, India ; # Address of author for correspondence _publ_contact_author_email apurba.patra@ch.nitdgp.ac.in _publ_contact_author_fax +91(0343)2547375 _publ_contact_author_phone +91(0343)2755475 _publ_contact_letter ; Submission dated :2010-07-17 Please consider this CIF for submission to the Cambridge Crystallographic Data Centre. I certify that all authors have seen and approved of this submission, that all have made significant scientific contributions to the work reported, and that all share responsibility and accountability for the results. This CIF is submitted as a personal communication This CIF is submitted as part of a journal submission Patra, Apurba K. ; #============================================================================== # # TITLE AND AUTHOR LIST _publ_section_title ; First Example of a Metal Thiocyanate that Promotes Regio-selective Cyclo-addition of a Coordinated Thiocyanate Ion to the Organic Ligand and Consequently Form a unique Heterocycle ; _publ_section_title_footnote . # 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 'Suprakash Roy' ;Department of Chemistry National Institute of Technology, Durgapur Durgapur 713 209 West Bengal, India ; S.Javed ;Department of Chemistry One Shields Ave. University of California Davis, CA 95616 USA ; M.Olmstead ;Department of Inorganic Chemistry Indian Association for the Cultivation of Science 2A & 2B Raja S. C. Mullick Road Jadavpur, Kolkata-700032, India. ; A.Patra ;Department of Chemistry National Institute of Technology, Durgapur Durgapur 713 209 West Bengal, India ; #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_purple _database_code_depnum_ccdc_archive 'CCDC 785238' #TrackingRef 'purple_final_mmo_ccdc_deposit.cif' _audit_creation_date 2010-07-17T12:50:57-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_common (pmtpm-SCN) _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C14 H11 N3 S2' _chemical_formula_sum 'C14 H11 N3 S2' _chemical_formula_weight 285.38 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.416(7) _cell_length_b 8.040(7) _cell_length_c 12.085(10) _cell_angle_alpha 74.754(12) _cell_angle_beta 79.687(12) _cell_angle_gamma 63.974(11) _cell_volume 623.1(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 1.75 _cell_measurement_theta_max 24.05 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description parallelepiped _exptl_crystal_colour 'bluish purple' _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 296 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.414 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker SMART Apex II' _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_unetI/netI 0.0908 _diffrn_reflns_number 4047 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 24.05 _diffrn_reflns_theta_full 24.05 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 1952 _reflns_number_gt 1313 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Apex2 (Bruker, 2006)' _computing_cell_refinement 'SAINT (Bruker, 2006)' _computing_data_reduction 'SAINT (Bruker, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0992P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 1952 _refine_ls_number_parameters 173 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0937 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1703 _refine_ls_wR_factor_gt 0.1517 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.671 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.102 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.17198(19) 0.28812(16) 0.25490(10) 0.0297(4) Uani 1 1 d . . . S2 S 0.36175(19) 0.76950(16) -0.38535(10) 0.0304(4) Uani 1 1 d . . . N1 N 0.3556(5) 0.4403(5) -0.2515(3) 0.0227(9) Uani 1 1 d . . . N2 N 0.2399(5) 0.4746(5) 0.0336(3) 0.0247(9) Uani 1 1 d . . . N3 N 0.2953(5) 0.6675(5) -0.1525(3) 0.0237(9) Uani 1 1 d . . . C1 C 0.3981(7) 0.3485(6) -0.3377(4) 0.0278(11) Uani 1 1 d . . . H1 H 0.4215 0.4048 -0.4134 0.033 Uiso 1 1 calc R . . C2 C 0.4057(7) 0.1681(6) -0.3097(4) 0.0283(11) Uani 1 1 d . . . H2 H 0.4371 0.0999 -0.367 0.034 Uiso 1 1 calc R . . C3 C 0.3666(7) 0.0865(6) -0.1960(4) 0.0291(11) Uani 1 1 d . . . H3 H 0.3693 -0.0343 -0.1782 0.035 Uiso 1 1 calc R . . C4 C 0.3238(7) 0.1858(6) -0.1099(4) 0.0273(11) Uani 1 1 d . . . H4 H 0.2989 0.1332 -0.0336 0.033 Uiso 1 1 calc R . . C5 C 0.3195(7) 0.3661(6) -0.1413(4) 0.0258(11) Uani 1 1 d . . . C6 C 0.2800(6) 0.5120(6) -0.0758(4) 0.0256(11) Uani 1 1 d . . . C7 C 0.1976(6) 0.5972(6) 0.1077(4) 0.0245(11) Uani 1 1 d . . . C8 C 0.1842(7) 0.7833(6) 0.0772(4) 0.0285(11) Uani 1 1 d . . . H8 H 0.2076 0.8362 0.0008 0.034 Uiso 1 1 calc R . . C9 C 0.1365(7) 0.8871(7) 0.1606(4) 0.0322(12) Uani 1 1 d . . . H9 H 0.1258 1.0108 0.14 0.039 Uiso 1 1 calc R . . C10 C 0.1044(7) 0.8098(7) 0.2739(4) 0.0325(12) Uani 1 1 d . . . H10 H 0.0733 0.8818 0.3292 0.039 Uiso 1 1 calc R . . C11 C 0.1175(7) 0.6269(6) 0.3075(4) 0.0311(11) Uani 1 1 d . . . H11 H 0.0976 0.5757 0.3848 0.037 Uiso 1 1 calc R . . C12 C 0.1610(6) 0.5192(6) 0.2237(4) 0.0241(10) Uani 1 1 d . . . C13 C 0.1236(7) 0.2407(7) 0.4084(4) 0.0339(12) Uani 1 1 d . . . H13A H 0.1332 0.1138 0.4346 0.051 Uiso 1 1 calc R . . H13B H -0.0091 0.3282 0.4289 0.051 Uiso 1 1 calc R . . H13C H 0.2209 0.2548 0.4436 0.051 Uiso 1 1 calc R . . C14 C 0.3349(7) 0.6388(6) -0.2583(4) 0.0243(10) Uani 1 1 d . . . 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 S1 0.0409(8) 0.0271(7) 0.0235(7) -0.0050(5) -0.0012(5) -0.0168(6) S2 0.0446(9) 0.0264(7) 0.0236(7) -0.0041(5) -0.0009(5) -0.0190(6) N1 0.028(2) 0.023(2) 0.021(2) -0.0045(16) -0.0001(16) -0.0147(18) N2 0.036(2) 0.023(2) 0.018(2) -0.0029(16) -0.0013(17) -0.0153(18) N3 0.028(2) 0.021(2) 0.023(2) -0.0033(17) -0.0030(16) -0.0112(17) C1 0.041(3) 0.029(3) 0.018(2) -0.005(2) -0.001(2) -0.018(2) C2 0.039(3) 0.026(3) 0.025(3) -0.009(2) -0.003(2) -0.016(2) C3 0.038(3) 0.022(2) 0.033(3) -0.006(2) -0.003(2) -0.018(2) C4 0.036(3) 0.023(3) 0.025(3) 0.000(2) -0.005(2) -0.016(2) C5 0.030(3) 0.028(3) 0.024(3) -0.006(2) -0.001(2) -0.016(2) C6 0.027(3) 0.021(3) 0.031(3) -0.006(2) -0.003(2) -0.012(2) C7 0.025(3) 0.026(3) 0.025(3) -0.008(2) -0.003(2) -0.010(2) C8 0.035(3) 0.026(3) 0.026(3) -0.005(2) 0.001(2) -0.015(2) C9 0.044(3) 0.026(3) 0.034(3) -0.008(2) -0.002(2) -0.021(2) C10 0.035(3) 0.038(3) 0.032(3) -0.017(2) 0.003(2) -0.018(2) C11 0.034(3) 0.030(3) 0.029(3) -0.006(2) -0.001(2) -0.013(2) C12 0.027(3) 0.021(2) 0.024(3) -0.002(2) -0.002(2) -0.011(2) C13 0.050(3) 0.039(3) 0.018(3) -0.002(2) -0.004(2) -0.024(3) C14 0.027(3) 0.023(2) 0.024(3) -0.005(2) -0.003(2) -0.011(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C12 1.764(5) . ? S1 C13 1.796(4) . ? S2 C14 1.652(5) . ? N1 C5 1.340(6) . ? N1 C1 1.347(5) . ? N1 C14 1.516(5) . ? N2 C6 1.287(6) . ? N2 C7 1.402(5) . ? N3 C14 1.318(5) . ? N3 C6 1.383(6) . ? C1 C2 1.378(6) . ? C1 H1 0.93 . ? C2 C3 1.397(6) . ? C2 H2 0.93 . ? C3 C4 1.385(6) . ? C3 H3 0.93 . ? C4 C5 1.386(6) . ? C4 H4 0.93 . ? C5 C6 1.480(6) . ? C7 C8 1.407(6) . ? C7 C12 1.408(6) . ? C8 C9 1.376(6) . ? C8 H8 0.93 . ? C9 C10 1.373(7) . ? C9 H9 0.93 . ? C10 C11 1.382(6) . ? C10 H10 0.93 . ? C11 C12 1.407(6) . ? C11 H11 0.93 . ? C13 H13A 0.96 . ? C13 H13B 0.96 . ? C13 H13C 0.96 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 S1 C13 103.1(2) . . ? C5 N1 C1 123.6(4) . . ? C5 N1 C14 108.0(3) . . ? C1 N1 C14 128.4(4) . . ? C6 N2 C7 125.4(4) . . ? C14 N3 C6 110.5(4) . . ? N1 C1 C2 117.5(4) . . ? N1 C1 H1 121.3 . . ? C2 C1 H1 121.3 . . ? C1 C2 C3 120.7(4) . . ? C1 C2 H2 119.6 . . ? C3 C2 H2 119.6 . . ? C4 C3 C2 119.9(4) . . ? C4 C3 H3 120 . . ? C2 C3 H3 120 . . ? C3 C4 C5 117.7(4) . . ? C3 C4 H4 121.2 . . ? C5 C4 H4 121.2 . . ? N1 C5 C4 120.6(4) . . ? N1 C5 C6 106.1(4) . . ? C4 C5 C6 133.3(4) . . ? N2 C6 N3 133.6(4) . . ? N2 C6 C5 118.2(4) . . ? N3 C6 C5 108.2(4) . . ? N2 C7 C8 127.1(4) . . ? N2 C7 C12 113.5(4) . . ? C8 C7 C12 119.5(4) . . ? C9 C8 C7 119.9(4) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C10 C9 C8 120.6(4) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 121.3(4) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C10 C11 C12 119.4(4) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C11 C12 C7 119.4(4) . . ? C11 C12 S1 123.7(4) . . ? C7 C12 S1 116.9(3) . . ? S1 C13 H13A 109.5 . . ? S1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? S1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C14 N1 107.1(4) . . ? N3 C14 S2 133.9(4) . . ? N1 C14 S2 119.0(3) . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF # Attachment 'sr8_final_mmo_ccdc_deposit.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-07-17 at 12:10:34 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : d:\wingx\files\archive.reqdat # CIF files read : sr8 struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# #data_global #TrackingRef 'sr8_final_mmo_ccdc_deposit.cif' #------------------ AUDIT DETAILS -------------------------------------------# #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_sr8 _database_code_depnum_ccdc_archive 'CCDC 785239' #TrackingRef 'sr8_final_mmo_ccdc_deposit.cif' _audit_creation_date 2010-07-17T12:10:34-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_common '[(pmtpm)CuII(SCN)CuI(SCN)2]n' _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C16 H12 Cu2 N5 S4' _chemical_formula_sum 'C16 H12 Cu2 N5 S4' _chemical_formula_weight 529.63 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration Unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 6.7778(3) _cell_length_b 15.2422(8) _cell_length_c 18.9036(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1952.90(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 1.08 _cell_measurement_theta_max 23.29 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour 'greenish yellow' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.801 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1060 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_correction_type cylinder _exptl_absorpt_correction_T_min 0.4350 _exptl_absorpt_correction_T_max 0.4420 _exptl_absorpt_correction_T_ave 0.4388 _exptl_absorpt_coefficient_mu 2.617 _exptl_crystal_size_rad 0.2000 _exptl_absorpt_process_details ? #Give the reference to the method you used here #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker SMART Apex II' _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_av_R_equivalents 0.0692 _diffrn_reflns_av_unetI/netI 0.0392 _diffrn_reflns_number 19783 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 23.29 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 2816 _reflns_number_gt 2488 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Apex2 (Bruker, 2006)' _computing_cell_refinement 'SAINT (Bruker, 2006)' _computing_data_reduction 'SAINT (Bruker, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure was refined as a racemic twin. The largest difference map peak is 1.02\%A from Cu2 at a peak height of 1.57 e-\%A^-3^ and is of unknown origin. All other peaks are less than 1.00 e-\%A^-3^. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+5.5222P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2816 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0604 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1249 _refine_ls_wR_factor_gt 0.1184 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack (1983)' _refine_ls_abs_structure_Flack 0.53(3) _refine_diff_density_max 1.574 _refine_diff_density_min -0.791 _refine_diff_density_rms 0.101 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.21588(17) 0.77914(6) 0.66016(5) 0.0443(3) Uani 1 1 d . . . Cu2 Cu 0.2031(2) 1.15406(9) 0.59371(6) 0.0690(4) Uani 1 1 d . . . S1 S 0.3094(4) 0.66737(14) 0.58000(11) 0.0473(5) Uani 1 1 d . . . S2 S -0.1745(4) 0.73763(13) 0.66453(11) 0.0482(5) Uani 1 1 d . . . S3 S -0.0075(4) 1.02583(18) 0.55928(14) 0.0664(7) Uani 1 1 d . . . S4 S 0.5020(4) 1.10540(16) 0.54919(12) 0.0515(6) Uani 1 1 d . . . N1 N 0.2456(10) 0.8590(4) 0.7458(3) 0.0409(16) Uani 1 1 d . . . N2 N 0.2737(10) 0.6894(4) 0.7311(3) 0.0385(16) Uani 1 1 d . . . N3 N -0.1945(13) 0.6787(5) 0.8035(4) 0.063(2) Uani 1 1 d . . . N4 N 0.1842(14) 0.8711(5) 0.5881(4) 0.057(2) Uani 1 1 d . . . N5 N 0.6059(13) 1.2464(6) 0.4617(4) 0.062(2) Uani 1 1 d . . . C1 C 0.2287(13) 0.9457(5) 0.7509(4) 0.044(2) Uani 1 1 d . . . H1 H 0.2108 0.9785 0.7099 0.053 Uiso 1 1 calc R . . C2 C 0.2371(12) 0.9890(5) 0.8159(4) 0.046(2) Uani 1 1 d . . . H2 H 0.2236 1.0496 0.8183 0.055 Uiso 1 1 calc R . . C3 C 0.2654(13) 0.9409(5) 0.8756(4) 0.048(2) Uani 1 1 d . . . H3 H 0.2732 0.9687 0.9193 0.057 Uiso 1 1 calc R . . C4 C 0.2823(13) 0.8515(6) 0.8714(4) 0.046(2) Uani 1 1 d . . . H4 H 0.2993 0.8181 0.9121 0.055 Uiso 1 1 calc R . . C5 C 0.2740(13) 0.8115(5) 0.8061(4) 0.0386(19) Uani 1 1 d . . . C6 C 0.2880(13) 0.7185(5) 0.7951(4) 0.0404(18) Uani 1 1 d . . . H6 H 0.3068 0.6803 0.8329 0.049 Uiso 1 1 calc R . . C7 C 0.2779(12) 0.5991(5) 0.7132(4) 0.0351(17) Uani 1 1 d . . . C8 C 0.2694(13) 0.5305(5) 0.7615(4) 0.043(2) Uani 1 1 d . . . H8 H 0.2725 0.542 0.8098 0.052 Uiso 1 1 calc R . . C9 C 0.2563(12) 0.4457(6) 0.7374(5) 0.052(2) Uani 1 1 d . . . H9 H 0.2506 0.4001 0.77 0.063 Uiso 1 1 calc R . . C10 C 0.2515(13) 0.4268(5) 0.6673(5) 0.053(2) Uani 1 1 d . . . H10 H 0.2415 0.3688 0.6524 0.063 Uiso 1 1 calc R . . C11 C 0.2612(12) 0.4928(5) 0.6187(4) 0.045(2) Uani 1 1 d . . . H11 H 0.2573 0.4797 0.5706 0.054 Uiso 1 1 calc R . . C12 C 0.2770(13) 0.5794(4) 0.6408(4) 0.0383(19) Uani 1 1 d . . . C13 C 0.1115(17) 0.6532(7) 0.5168(5) 0.068(3) Uani 1 1 d . . . H13A H 0.1186 0.6986 0.4817 0.101 Uiso 1 1 calc R . . H13B H -0.013 0.6565 0.5409 0.101 Uiso 1 1 calc R . . H13C H 0.124 0.597 0.4944 0.101 Uiso 1 1 calc R . . C14 C -0.1880(13) 0.7043(5) 0.7458(4) 0.0419(19) Uani 1 1 d . . . C15 C 0.1147(15) 0.9313(7) 0.5795(5) 0.055(3) Uani 1 1 d . . . C16 C 0.5649(15) 1.1871(6) 0.4982(4) 0.050(2) Uani 1 1 d . . . 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 Cu1 0.0599(7) 0.0365(5) 0.0365(5) 0.0057(4) -0.0009(5) 0.0008(5) Cu2 0.0769(9) 0.0857(9) 0.0443(6) 0.0107(6) 0.0089(7) 0.0261(8) S1 0.0548(14) 0.0482(12) 0.0388(11) 0.0047(9) 0.0046(11) 0.0049(12) S2 0.0575(14) 0.0460(12) 0.0413(11) 0.0017(10) -0.0031(11) 0.0010(10) S3 0.0644(17) 0.0696(18) 0.0652(15) 0.0021(14) -0.0133(14) 0.0070(14) S4 0.0561(15) 0.0500(14) 0.0485(13) -0.0004(11) 0.0021(12) 0.0047(12) N1 0.037(4) 0.045(4) 0.041(4) 0.001(3) 0.000(3) -0.007(3) N2 0.040(4) 0.043(4) 0.033(3) 0.002(3) 0.003(3) -0.003(3) N3 0.065(6) 0.073(5) 0.050(5) -0.004(4) 0.001(5) -0.013(5) N4 0.079(6) 0.020(3) 0.070(5) -0.008(3) 0.027(5) 0.003(4) N5 0.065(6) 0.074(6) 0.047(5) -0.009(4) 0.005(4) -0.022(4) C1 0.049(6) 0.036(4) 0.047(5) 0.010(4) -0.002(4) -0.005(4) C2 0.037(5) 0.041(4) 0.060(5) -0.006(4) -0.005(4) 0.004(4) C3 0.048(6) 0.051(5) 0.044(5) -0.005(4) -0.006(4) -0.002(4) C4 0.040(5) 0.057(5) 0.041(4) 0.007(4) -0.003(4) -0.003(5) C5 0.040(5) 0.038(4) 0.038(4) 0.003(3) -0.002(4) -0.002(4) C6 0.042(5) 0.042(4) 0.037(4) 0.011(4) -0.003(4) 0.014(5) C7 0.032(4) 0.032(4) 0.042(4) -0.004(3) 0.001(4) 0.002(4) C8 0.049(5) 0.042(5) 0.039(4) 0.008(4) -0.005(4) 0.005(4) C9 0.034(6) 0.048(5) 0.075(6) 0.021(5) -0.003(5) -0.003(4) C10 0.044(6) 0.041(4) 0.072(6) -0.006(4) 0.001(5) 0.002(4) C11 0.043(5) 0.046(5) 0.047(5) -0.006(4) 0.000(4) 0.007(4) C12 0.038(5) 0.029(4) 0.048(5) 0.006(3) 0.007(4) 0.005(4) C13 0.084(8) 0.087(7) 0.032(5) -0.007(5) -0.010(5) 0.020(7) C14 0.043(5) 0.045(5) 0.037(5) -0.005(4) 0.004(4) -0.004(4) C15 0.064(7) 0.068(7) 0.035(5) -0.001(5) 0.005(5) -0.032(6) C16 0.056(7) 0.059(6) 0.034(5) -0.006(5) -0.005(4) -0.010(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 1.956(6) . ? Cu1 N4 1.966(8) . ? Cu1 N1 2.035(6) . ? Cu1 S1 2.367(2) . ? Cu1 S2 2.722(3) . ? Cu2 N5 1.958(9) 3_476 ? Cu2 N3 1.981(8) 4_556 ? Cu2 S4 2.315(3) . ? Cu2 S3 2.506(3) . ? S1 C12 1.780(7) . ? S1 C13 1.809(10) . ? S2 C14 1.622(9) . ? S3 C15 1.705(12) . ? S4 C16 1.632(10) . ? N1 C1 1.331(10) . ? N1 C5 1.365(9) . ? N2 C6 1.291(9) . ? N2 C7 1.417(9) . ? N3 C14 1.158(10) . ? N3 Cu2 1.981(8) 4_546 ? N4 C15 1.044(11) . ? N5 C16 1.170(11) . ? N5 Cu2 1.958(9) 3_576 ? C1 C2 1.396(11) . ? C1 H1 0.93 . ? C2 C3 1.359(11) . ? C2 H2 0.93 . ? C3 C4 1.370(11) . ? C3 H3 0.93 . ? C4 C5 1.377(11) . ? C4 H4 0.93 . ? C5 C6 1.437(10) . ? C6 H6 0.93 . ? C7 C8 1.389(10) . ? C7 C12 1.401(11) . ? C8 C9 1.373(12) . ? C8 H8 0.93 . ? C9 C10 1.356(13) . ? C9 H9 0.93 . ? C10 C11 1.365(12) . ? C10 H10 0.93 . ? C11 C12 1.389(11) . ? C11 H11 0.93 . ? C13 H13A 0.96 . ? C13 H13B 0.96 . ? C13 H13C 0.96 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N4 174.7(3) . . ? N2 Cu1 N1 81.6(2) . . ? N4 Cu1 N1 97.8(3) . . ? N2 Cu1 S1 83.22(18) . . ? N4 Cu1 S1 95.7(2) . . ? N1 Cu1 S1 156.0(2) . . ? N2 Cu1 S2 90.7(2) . . ? N4 Cu1 S2 94.6(3) . . ? N1 Cu1 S2 102.18(19) . . ? S1 Cu1 S2 96.46(8) . . ? N5 Cu2 N3 111.6(3) 3_476 4_556 ? N5 Cu2 S4 110.4(3) 3_476 . ? N3 Cu2 S4 116.3(3) 4_556 . ? N5 Cu2 S3 105.9(3) 3_476 . ? N3 Cu2 S3 112.7(3) 4_556 . ? S4 Cu2 S3 98.86(10) . . ? C12 S1 C13 104.2(5) . . ? C12 S1 Cu1 95.5(3) . . ? C13 S1 Cu1 108.1(3) . . ? C14 S2 Cu1 99.0(3) . . ? C15 S3 Cu2 108.9(3) . . ? C16 S4 Cu2 101.5(4) . . ? C1 N1 C5 118.6(7) . . ? C1 N1 Cu1 130.1(5) . . ? C5 N1 Cu1 111.2(5) . . ? C6 N2 C7 123.8(6) . . ? C6 N2 Cu1 114.6(5) . . ? C7 N2 Cu1 121.3(5) . . ? C14 N3 Cu2 171.3(7) . 4_546 ? C15 N4 Cu1 141.7(8) . . ? C16 N5 Cu2 173.5(8) . 3_576 ? N1 C1 C2 122.0(7) . . ? N1 C1 H1 119 . . ? C2 C1 H1 119 . . ? C3 C2 C1 118.9(7) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C2 C3 C4 120.0(8) . . ? C2 C3 H3 120 . . ? C4 C3 H3 120 . . ? C3 C4 C5 119.3(8) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N1 C5 C4 121.4(7) . . ? N1 C5 C6 114.3(7) . . ? C4 C5 C6 124.3(7) . . ? N2 C6 C5 118.0(7) . . ? N2 C6 H6 121 . . ? C5 C6 H6 121 . . ? C8 C7 C12 118.7(7) . . ? C8 C7 N2 124.9(7) . . ? C12 C7 N2 116.2(6) . . ? C9 C8 C7 119.6(8) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C10 C9 C8 121.7(8) . . ? C10 C9 H9 119.1 . . ? C8 C9 H9 119.1 . . ? C9 C10 C11 120.0(8) . . ? C9 C10 H10 120 . . ? C11 C10 H10 120 . . ? C10 C11 C12 120.1(8) . . ? C10 C11 H11 120 . . ? C12 C11 H11 120 . . ? C11 C12 C7 119.9(7) . . ? C11 C12 S1 122.1(6) . . ? C7 C12 S1 117.9(5) . . ? S1 C13 H13A 109.5 . . ? S1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? S1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C14 S2 178.3(9) . . ? N4 C15 S3 175.3(10) . . ? N5 C16 S4 178.6(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Cu1 S1 C12 19.1(4) . . . . ? N4 Cu1 S1 C12 -166.1(4) . . . . ? N1 Cu1 S1 C12 70.1(6) . . . . ? S2 Cu1 S1 C12 -70.8(3) . . . . ? N2 Cu1 S1 C13 126.0(4) . . . . ? N4 Cu1 S1 C13 -59.3(5) . . . . ? N1 Cu1 S1 C13 176.9(6) . . . . ? S2 Cu1 S1 C13 36.1(4) . . . . ? N2 Cu1 S2 C14 29.5(3) . . . . ? N4 Cu1 S2 C14 -151.0(3) . . . . ? N1 Cu1 S2 C14 -52.1(3) . . . . ? S1 Cu1 S2 C14 112.7(3) . . . . ? N5 Cu2 S3 C15 159.0(4) 3_476 . . . ? N3 Cu2 S3 C15 -78.8(4) 4_556 . . . ? S4 Cu2 S3 C15 44.7(4) . . . . ? N5 Cu2 S4 C16 14.7(4) 3_476 . . . ? N3 Cu2 S4 C16 -113.8(4) 4_556 . . . ? S3 Cu2 S4 C16 125.4(3) . . . . ? N2 Cu1 N1 C1 -179.6(8) . . . . ? N4 Cu1 N1 C1 5.7(8) . . . . ? S1 Cu1 N1 C1 129.2(7) . . . . ? S2 Cu1 N1 C1 -90.7(7) . . . . ? N2 Cu1 N1 C5 -4.4(6) . . . . ? N4 Cu1 N1 C5 -179.1(6) . . . . ? S1 Cu1 N1 C5 -55.6(8) . . . . ? S2 Cu1 N1 C5 84.5(6) . . . . ? N4 Cu1 N2 C6 88(3) . . . . ? N1 Cu1 N2 C6 4.7(6) . . . . ? S1 Cu1 N2 C6 166.0(6) . . . . ? S2 Cu1 N2 C6 -97.6(6) . . . . ? N4 Cu1 N2 C7 -99(3) . . . . ? N1 Cu1 N2 C7 178.3(6) . . . . ? S1 Cu1 N2 C7 -20.3(6) . . . . ? S2 Cu1 N2 C7 76.1(6) . . . . ? N2 Cu1 N4 C15 -123(3) . . . . ? N1 Cu1 N4 C15 -41.2(15) . . . . ? S1 Cu1 N4 C15 158.7(14) . . . . ? S2 Cu1 N4 C15 61.7(15) . . . . ? C5 N1 C1 C2 -0.7(12) . . . . ? Cu1 N1 C1 C2 174.2(6) . . . . ? N1 C1 C2 C3 0.7(13) . . . . ? C1 C2 C3 C4 -0.9(13) . . . . ? C2 C3 C4 C5 1.2(14) . . . . ? C1 N1 C5 C4 1.0(13) . . . . ? Cu1 N1 C5 C4 -174.8(7) . . . . ? C1 N1 C5 C6 179.3(8) . . . . ? Cu1 N1 C5 C6 3.5(10) . . . . ? C3 C4 C5 N1 -1.2(14) . . . . ? C3 C4 C5 C6 -179.4(9) . . . . ? C7 N2 C6 C5 -177.6(8) . . . . ? Cu1 N2 C6 C5 -4.1(11) . . . . ? N1 C5 C6 N2 0.3(13) . . . . ? C4 C5 C6 N2 178.5(8) . . . . ? C6 N2 C7 C8 9.6(14) . . . . ? Cu1 N2 C7 C8 -163.5(7) . . . . ? C6 N2 C7 C12 -174.9(8) . . . . ? Cu1 N2 C7 C12 12.0(10) . . . . ? C12 C7 C8 C9 -1.3(13) . . . . ? N2 C7 C8 C9 174.0(8) . . . . ? C7 C8 C9 C10 0.0(14) . . . . ? C8 C9 C10 C11 0.5(14) . . . . ? C9 C10 C11 C12 0.3(13) . . . . ? C10 C11 C12 C7 -1.6(13) . . . . ? C10 C11 C12 S1 175.0(7) . . . . ? C8 C7 C12 C11 2.1(13) . . . . ? N2 C7 C12 C11 -173.7(7) . . . . ? C8 C7 C12 S1 -174.7(6) . . . . ? N2 C7 C12 S1 9.5(11) . . . . ? C13 S1 C12 C11 52.6(8) . . . . ? Cu1 S1 C12 C11 162.8(7) . . . . ? C13 S1 C12 C7 -130.7(7) . . . . ? Cu1 S1 C12 C7 -20.5(7) . . . . ? Cu2 N3 C14 S2 14E1(3) 4_546 . . . ? Cu1 S2 C14 N3 -7E1(3) . . . . ? Cu1 N4 C15 S3 -124(11) . . . . ? Cu2 S3 C15 N4 -146(12) . . . . ? Cu2 N5 C16 S4 14E1(3) 3_576 . . . ? Cu2 S4 C16 N5 -2E1(3) . . . . ? # END of CIF #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_sr21 _database_code_depnum_ccdc_archive 'CCDC 788792' #TrackingRef 'sr21_CCDC_Deposit.cif' _audit_creation_date 2010-08-11T11:55:58-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic '[(pmtpm)Cu(N3)Cl]' _chemical_formula_sum 'C13 H12 Cl Cu N5 S' _chemical_formula_weight 369.33 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.950(2) _cell_length_b 7.115(2) _cell_length_c 14.846(5) _cell_angle_alpha 89.315(10) _cell_angle_beta 83.557(9) _cell_angle_gamma 79.712(9) _cell_volume 717.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Rectangular _exptl_crystal_colour Green _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 362 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_correction_type cylinder _exptl_absorpt_correction_T_min 0.5123 _exptl_absorpt_correction_T_max 0.5181 _exptl_absorpt_correction_T_ave 0.5155 _exptl_crystal_size_rad 0.2000 _exptl_absorpt_coefficient_mu 1.849 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_unetI/netI 0.057 _diffrn_reflns_number 8141 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 24.68 _diffrn_reflns_theta_full 24.68 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 2439 _reflns_number_gt 1900 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Apex2 (Bruker, 2006)' _computing_cell_refinement 'SAINT (Bruker, 2006)' _computing_data_reduction 'SAINT (Bruker, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2439 _refine_ls_number_parameters 238 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0576 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1054 _refine_ls_wR_factor_gt 0.0979 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.663 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.095 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 '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' S S 0.1246 0.1234 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.20564(7) 0.70129(7) 0.75998(3) 0.02246(19) Uani 1 1 d . . . S1 S 0.30509(15) 0.47730(15) 0.64004(7) 0.0233(3) Uani 1 1 d . . . Cl1 Cl 0.32902(16) 0.48441(16) 0.87802(8) 0.0341(3) Uani 1 1 d . . . N3 N 0.4174(5) 0.8498(5) 0.7273(3) 0.0269(9) Uani 1 1 d . . . N4 N 0.5281(6) 0.8161(5) 0.6635(3) 0.0305(9) Uani 1 1 d . . . N5 N 0.6453(7) 0.7884(6) 0.5995(3) 0.0492(12) Uani 1 1 d . . . C7 C -0.0635(6) 0.4368(5) 0.7198(3) 0.0205(9) Uani 1 1 d . . . C12 C 0.1005(6) 0.3564(6) 0.6609(3) 0.0204(9) Uani 1 1 d . . . C10 C -0.0601(7) 0.0997(6) 0.6273(3) 0.0279(11) Uani 1 1 d . . . C9 C -0.2243(7) 0.1827(6) 0.6844(3) 0.0282(11) Uani 1 1 d . . . C11 C 0.1021(7) 0.1869(6) 0.6154(3) 0.0231(10) Uani 1 1 d . . . C8 C -0.2242(6) 0.3487(6) 0.7305(3) 0.0226(10) Uani 1 1 d . . . N2 N -0.0501(5) 0.6078(5) 0.7652(2) 0.0205(8) Uani 1 1 d . . . C6 C -0.1897(7) 0.7014(6) 0.8183(3) 0.0250(10) Uani 1 1 d . . . C5 C -0.1538(6) 0.8778(6) 0.8588(3) 0.0240(10) Uani 1 1 d . . . C1 C 0.0786(7) 1.0713(6) 0.8693(3) 0.0264(10) Uani 1 1 d . . . C3 C -0.2457(7) 1.1651(6) 0.9454(3) 0.0304(11) Uani 1 1 d . . . C4 C -0.2952(7) 1.0005(7) 0.9115(3) 0.0291(11) Uani 1 1 d . . . C2 C -0.0564(7) 1.1984(6) 0.9241(3) 0.0289(11) Uani 1 1 d . . . N1 N 0.0320(5) 0.9123(5) 0.8366(2) 0.0220(8) Uani 1 1 d . . . C13 C 0.2372(9) 0.6092(7) 0.5398(3) 0.0297(11) Uani 1 1 d . . . H7 H -0.307(6) 0.674(5) 0.837(3) 0.011(10) Uiso 1 1 d . . . H5 H -0.327(6) 0.396(5) 0.766(2) 0.007(10) Uiso 1 1 d . . . H4 H -0.336(6) 0.138(5) 0.690(2) 0.009(10) Uiso 1 1 d . . . H8 H -0.034(6) 1.319(6) 0.942(3) 0.028(12) Uiso 1 1 d . . . H2 H 0.194(6) 0.136(5) 0.583(3) 0.008(11) Uiso 1 1 d . . . H6 H -0.408(7) 0.967(6) 0.927(3) 0.022(12) Uiso 1 1 d . . . H3 H -0.060(7) -0.009(7) 0.593(3) 0.039(13) Uiso 1 1 d . . . H9 H 0.208(7) 1.097(6) 0.847(3) 0.028(12) Uiso 1 1 d . . . H10 H -0.335(7) 1.257(6) 0.982(3) 0.033(12) Uiso 1 1 d . . . H13 H 0.239(6) 0.532(6) 0.491(3) 0.025(12) Uiso 1 1 d . . . H14 H 0.120(8) 0.660(7) 0.548(3) 0.045(17) Uiso 1 1 d . . . H15 H 0.320(7) 0.684(6) 0.531(3) 0.034(14) Uiso 1 1 d . . . 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 Cu1 0.0164(3) 0.0271(3) 0.0245(3) -0.0057(2) -0.0012(2) -0.0058(2) S1 0.0179(5) 0.0281(6) 0.0243(6) -0.0036(5) -0.0006(5) -0.0056(4) Cl1 0.0258(6) 0.0386(7) 0.0369(7) -0.0059(5) -0.0055(5) -0.0015(5) N3 0.024(2) 0.032(2) 0.028(2) -0.0085(18) -0.0003(18) -0.0131(16) N4 0.033(2) 0.026(2) 0.039(3) -0.0007(19) -0.010(2) -0.0182(18) N5 0.050(3) 0.058(3) 0.046(3) -0.016(2) 0.009(2) -0.032(2) C7 0.021(2) 0.019(2) 0.023(2) -0.0012(18) -0.0073(19) -0.0025(17) C12 0.020(2) 0.023(2) 0.020(2) 0.0054(18) -0.0042(18) -0.0070(17) C10 0.033(3) 0.023(2) 0.030(3) -0.001(2) -0.009(2) -0.006(2) C9 0.026(3) 0.030(2) 0.033(3) 0.003(2) -0.007(2) -0.013(2) C11 0.020(2) 0.023(2) 0.025(3) -0.003(2) -0.001(2) 0.0004(19) C8 0.016(2) 0.024(2) 0.026(3) 0.000(2) -0.002(2) 0.0014(18) N2 0.0153(18) 0.0243(18) 0.021(2) -0.0037(15) -0.0017(15) -0.0022(14) C6 0.018(2) 0.031(2) 0.025(3) 0.002(2) 0.001(2) -0.0032(19) C5 0.022(2) 0.028(2) 0.023(3) -0.0016(19) -0.0047(19) -0.0028(18) C1 0.029(3) 0.023(2) 0.028(3) -0.002(2) -0.006(2) -0.005(2) C3 0.036(3) 0.030(2) 0.021(3) -0.006(2) -0.002(2) 0.004(2) C4 0.023(3) 0.036(3) 0.026(3) -0.004(2) -0.001(2) -0.001(2) C2 0.039(3) 0.022(2) 0.026(3) 0.000(2) -0.010(2) -0.004(2) N1 0.0198(19) 0.0257(19) 0.020(2) -0.0026(15) -0.0034(15) -0.0033(15) C13 0.034(3) 0.032(3) 0.024(3) -0.005(2) -0.004(2) -0.011(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 1.975(4) . ? Cu1 N2 1.999(3) . ? Cu1 N1 2.022(3) . ? Cu1 S1 2.3634(13) . ? Cu1 Cl1 2.4468(14) . ? S1 C12 1.786(4) . ? S1 C13 1.812(5) . ? N3 N4 1.150(5) . ? N4 N5 1.174(6) . ? C7 C8 1.369(6) . ? C7 C12 1.395(6) . ? C7 N2 1.420(5) . ? C12 C11 1.387(6) . ? C10 C11 1.375(6) . ? C10 C9 1.387(6) . ? C9 C8 1.371(6) . ? N2 C6 1.271(5) . ? C6 C5 1.471(6) . ? C5 N1 1.361(5) . ? C5 C4 1.371(6) . ? C1 N1 1.342(5) . ? C1 C2 1.380(6) . ? C3 C2 1.379(7) . ? C3 C4 1.393(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cu1 N2 161.85(15) . . ? N3 Cu1 N1 94.54(15) . . ? N2 Cu1 N1 80.65(13) . . ? N3 Cu1 S1 95.36(11) . . ? N2 Cu1 S1 84.04(10) . . ? N1 Cu1 S1 158.50(10) . . ? N3 Cu1 Cl1 104.23(12) . . ? N2 Cu1 Cl1 93.87(10) . . ? N1 Cu1 Cl1 100.64(10) . . ? S1 Cu1 Cl1 95.35(5) . . ? C12 S1 C13 99.3(2) . . ? C12 S1 Cu1 96.19(14) . . ? C13 S1 Cu1 104.41(18) . . ? N4 N3 Cu1 122.2(3) . . ? N3 N4 N5 176.9(4) . . ? C8 C7 C12 119.2(4) . . ? C8 C7 N2 124.4(4) . . ? C12 C7 N2 116.4(4) . . ? C11 C12 C7 120.3(4) . . ? C11 C12 S1 119.7(3) . . ? C7 C12 S1 119.9(3) . . ? C11 C10 C9 119.6(4) . . ? C8 C9 C10 120.5(4) . . ? C10 C11 C12 119.8(4) . . ? C7 C8 C9 120.7(4) . . ? C6 N2 C7 123.7(4) . . ? C6 N2 Cu1 115.0(3) . . ? C7 N2 Cu1 120.9(3) . . ? N2 C6 C5 117.1(4) . . ? N1 C5 C4 122.7(4) . . ? N1 C5 C6 113.8(4) . . ? C4 C5 C6 123.5(4) . . ? N1 C1 C2 121.7(4) . . ? C2 C3 C4 118.6(4) . . ? C5 C4 C3 118.7(5) . . ? C3 C2 C1 120.0(4) . . ? C1 N1 C5 118.3(4) . . ? C1 N1 Cu1 128.9(3) . . ? C5 N1 Cu1 112.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Cu1 S1 C12 -174.19(17) . . . . ? N2 Cu1 S1 C12 -12.42(16) . . . . ? N1 Cu1 S1 C12 -57.1(3) . . . . ? Cl1 Cu1 S1 C12 80.93(13) . . . . ? N3 Cu1 S1 C13 -72.9(2) . . . . ? N2 Cu1 S1 C13 88.9(2) . . . . ? N1 Cu1 S1 C13 44.2(3) . . . . ? Cl1 Cu1 S1 C13 -177.8(2) . . . . ? N2 Cu1 N3 N4 -83.2(6) . . . . ? N1 Cu1 N3 N4 -156.9(4) . . . . ? S1 Cu1 N3 N4 4.0(4) . . . . ? Cl1 Cu1 N3 N4 100.9(4) . . . . ? Cu1 N3 N4 N5 -18E1(10) . . . . ? C8 C7 C12 C11 -1.5(6) . . . . ? N2 C7 C12 C11 178.4(4) . . . . ? C8 C7 C12 S1 175.7(3) . . . . ? N2 C7 C12 S1 -4.3(5) . . . . ? C13 S1 C12 C11 84.1(4) . . . . ? Cu1 S1 C12 C11 -170.1(3) . . . . ? C13 S1 C12 C7 -93.2(4) . . . . ? Cu1 S1 C12 C7 12.6(3) . . . . ? C11 C10 C9 C8 -1.3(7) . . . . ? C9 C10 C11 C12 0.3(7) . . . . ? C7 C12 C11 C10 1.2(6) . . . . ? S1 C12 C11 C10 -176.1(3) . . . . ? C12 C7 C8 C9 0.5(6) . . . . ? N2 C7 C8 C9 -179.5(4) . . . . ? C10 C9 C8 C7 1.0(7) . . . . ? C8 C7 N2 C6 -2.7(6) . . . . ? C12 C7 N2 C6 177.3(4) . . . . ? C8 C7 N2 Cu1 170.2(3) . . . . ? C12 C7 N2 Cu1 -9.8(5) . . . . ? N3 Cu1 N2 C6 -83.2(6) . . . . ? N1 Cu1 N2 C6 -7.4(3) . . . . ? S1 Cu1 N2 C6 -172.2(3) . . . . ? Cl1 Cu1 N2 C6 92.8(3) . . . . ? N3 Cu1 N2 C7 103.3(5) . . . . ? N1 Cu1 N2 C7 179.1(3) . . . . ? S1 Cu1 N2 C7 14.3(3) . . . . ? Cl1 Cu1 N2 C7 -80.7(3) . . . . ? C7 N2 C6 C5 -178.9(3) . . . . ? Cu1 N2 C6 C5 7.8(5) . . . . ? N2 C6 C5 N1 -3.0(6) . . . . ? N2 C6 C5 C4 174.8(4) . . . . ? N1 C5 C4 C3 -1.4(7) . . . . ? C6 C5 C4 C3 -179.1(4) . . . . ? C2 C3 C4 C5 0.3(7) . . . . ? C4 C3 C2 C1 0.9(7) . . . . ? N1 C1 C2 C3 -1.1(7) . . . . ? C2 C1 N1 C5 0.0(6) . . . . ? C2 C1 N1 Cu1 -177.2(3) . . . . ? C4 C5 N1 C1 1.3(6) . . . . ? C6 C5 N1 C1 179.2(4) . . . . ? C4 C5 N1 Cu1 178.9(3) . . . . ? C6 C5 N1 Cu1 -3.2(4) . . . . ? N3 Cu1 N1 C1 -14.8(4) . . . . ? N2 Cu1 N1 C1 -177.2(4) . . . . ? S1 Cu1 N1 C1 -132.0(3) . . . . ? Cl1 Cu1 N1 C1 90.6(4) . . . . ? N3 Cu1 N1 C5 167.8(3) . . . . ? N2 Cu1 N1 C5 5.5(3) . . . . ? S1 Cu1 N1 C5 50.6(5) . . . . ? Cl1 Cu1 N1 C5 -86.7(3) . . . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_sr24 _database_code_depnum_ccdc_archive 'CCDC 790423' #TrackingRef 'ccdc_deposit_240810.cif' _audit_creation_date 2010-08-24T18:10:22-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_common '[(pmtpm)CuII(N3)(SCN)]' _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C14 H12 Cu1 N6 S2' _chemical_formula_sum 'C14 H12 Cu1 N6 S2' _chemical_formula_weight 391.96 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.9433(8) _cell_length_b 10.6557(8) _cell_length_c 14.4837(11) _cell_angle_alpha 90 _cell_angle_beta 90.237(2) _cell_angle_gamma 90 _cell_volume 1534.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 1.41 _cell_measurement_theta_max 24.34 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.021 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 318 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_correction_T_min 0.8614 _exptl_absorpt_correction_T_max 0.8616 #_exptl_absorpt_correction_T_ave 0.8615 _exptl_absorpt_coefficient_mu 1.702 _exptl_crystal_size_rad 0.0600 #_exptl_absorpt_coefficient_mu 1.508 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker SMART Apex II' _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0893 _diffrn_reflns_av_unetI/netI 0.0459 _diffrn_reflns_number 10735 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 24.34 _diffrn_reflns_theta_full 24.34 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 1450 _reflns_number_gt 1118 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Apex2 (Bruker, 2006)' _computing_cell_refinement 'SAINT (Bruker, 2006)' _computing_data_reduction 'SAINT (Bruker, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+6.0321P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 1450 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.0939 _refine_ls_wR_factor_gt 0.0859 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.319 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.08 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N6 N 0.7812(6) 0.2749(6) 0.5171(4) 0.0187(17) Uani 1 1 d . . . C14 C 0.7079(9) 0.3109(7) 0.4740(6) 0.021(2) Uani 1 1 d . . . S3 S 0.5885(2) 0.3698(2) 0.40132(15) 0.0421(7) Uani 1 1 d . . . Cu1 Cu 0.89956(8) 0.24739(8) 0.63872(6) 0.0185(3) Uani 1 1 d . . . S1 S 0.75579(18) 0.35484(16) 0.74428(12) 0.0205(5) Uani 1 1 d . . . C12 C 0.7971(7) 0.5082(6) 0.7044(4) 0.0138(17) Uani 1 1 d . . . C7 C 0.9194(6) 0.5262(6) 0.6596(4) 0.0130(17) Uani 1 1 d . . . C8 C 0.9614(7) 0.6463(7) 0.6369(5) 0.0210(19) Uani 1 1 d . . . H5 H 1.0442 0.6593 0.6088 0.025 Uiso 1 1 calc R . . C11 C 0.7147(7) 0.6092(7) 0.7226(5) 0.0212(19) Uani 1 1 d . . . H2 H 0.6323 0.5973 0.7515 0.025 Uiso 1 1 calc R . . C10 C 0.7558(7) 0.7285(7) 0.6975(5) 0.0208(18) Uani 1 1 d . . . H3 H 0.7003 0.7971 0.7084 0.025 Uiso 1 1 calc R . . C9 C 0.8789(7) 0.7454(7) 0.6565(4) 0.0198(18) Uani 1 1 d . . . H4 H 0.9068 0.8263 0.6417 0.024 Uiso 1 1 calc R . . N2 N 0.9912(6) 0.4152(5) 0.6368(4) 0.0168(14) Uani 1 1 d . . . C6 C 1.1144(7) 0.4129(7) 0.6107(5) 0.0199(19) Uani 1 1 d . . . H7 H 1.1659 0.4857 0.6086 0.024 Uiso 1 1 calc R . . C4 C 1.2995(7) 0.2774(7) 0.5520(5) 0.0208(19) Uani 1 1 d . . . H9 H 1.3554 0.3467 0.5446 0.025 Uiso 1 1 calc R . . C2 C 1.2582(7) 0.0576(7) 0.5430(5) 0.0237(19) Uani 1 1 d . . . H11 H 1.286 -0.0238 0.53 0.028 Uiso 1 1 calc R . . C3 C 1.3445(7) 0.1570(7) 0.5306(5) 0.0223(19) Uani 1 1 d . . . H10 H 1.431 0.1442 0.5083 0.027 Uiso 1 1 calc R . . C1 C 1.1292(7) 0.0805(7) 0.5752(4) 0.0168(18) Uani 1 1 d . . . H12 H 1.0711 0.0128 0.5824 0.02 Uiso 1 1 calc R . . C5 C 1.1703(7) 0.2913(6) 0.5845(5) 0.0177(18) Uani 1 1 d . . . N1 N 1.0848(6) 0.1946(5) 0.5961(4) 0.0168(15) Uani 1 1 d . . . N5 N 0.6074(7) 0.0260(6) 0.6563(4) 0.0287(17) Uani 1 1 d . . . N3 N 0.8401(6) 0.0764(5) 0.6707(4) 0.0221(16) Uani 1 1 d . . . N4 N 0.7214(8) 0.0534(5) 0.6632(4) 0.0252(16) Uani 1 1 d . . . C13 C 0.5850(7) 0.3402(7) 0.7019(5) 0.032(2) Uani 1 1 d . . . H14A H 0.5262 0.3901 0.7393 0.048 Uiso 1 1 calc R . . H14B H 0.5576 0.2539 0.7048 0.048 Uiso 1 1 calc R . . H14C H 0.5805 0.3687 0.6391 0.048 Uiso 1 1 calc R . . 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 N6 0.024(4) 0.010(4) 0.022(4) -0.004(3) 0.006(3) -0.008(3) C14 0.031(6) 0.008(5) 0.025(6) -0.007(4) 0.018(5) -0.015(4) S3 0.0390(14) 0.0389(15) 0.0484(15) 0.0049(12) -0.0063(12) 0.0029(11) Cu1 0.0185(5) 0.0102(5) 0.0269(6) 0.0001(4) 0.0013(4) -0.0008(4) S1 0.0238(11) 0.0110(11) 0.0269(12) 0.0020(9) 0.0045(9) -0.0022(9) C12 0.017(4) 0.009(4) 0.015(4) -0.003(3) -0.007(4) 0.001(4) C7 0.012(4) 0.011(5) 0.016(4) -0.002(3) -0.002(4) 0.005(4) C8 0.023(4) 0.015(5) 0.024(5) -0.005(4) -0.001(4) -0.002(4) C11 0.024(5) 0.020(5) 0.020(4) 0.000(4) -0.003(4) -0.005(4) C10 0.020(4) 0.021(5) 0.021(4) -0.001(4) -0.003(4) 0.006(4) C9 0.030(5) 0.006(4) 0.022(4) 0.004(4) -0.007(4) 0.000(4) N2 0.017(4) 0.015(4) 0.018(4) 0.000(3) -0.001(3) -0.001(3) C6 0.022(5) 0.014(5) 0.024(5) -0.001(4) -0.001(4) -0.009(4) C4 0.015(5) 0.023(5) 0.025(5) 0.005(4) -0.003(4) -0.003(4) C2 0.034(5) 0.011(5) 0.026(5) 0.005(4) 0.000(4) 0.002(4) C3 0.023(5) 0.022(5) 0.021(4) 0.001(4) -0.001(4) 0.009(4) C1 0.022(5) 0.018(5) 0.010(4) 0.003(3) -0.005(4) -0.004(4) C5 0.022(5) 0.010(5) 0.021(5) 0.002(3) -0.003(4) -0.001(4) N1 0.022(4) 0.005(4) 0.024(4) -0.002(3) -0.004(3) 0.001(3) N5 0.027(4) 0.018(4) 0.041(4) -0.002(3) 0.012(4) -0.004(3) N3 0.015(4) 0.007(4) 0.044(4) -0.003(3) -0.003(3) 0.000(3) N4 0.046(5) 0.008(4) 0.022(4) 0.001(3) 0.009(4) 0.002(4) C13 0.021(5) 0.016(5) 0.058(6) -0.006(4) 0.013(4) -0.003(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N6 C14 1.031(8) . ? N6 Cu1 2.135(7) . ? C14 S3 1.703(10) . ? Cu1 N3 1.971(6) . ? Cu1 N2 2.007(5) . ? Cu1 N1 2.025(6) . ? Cu1 S1 2.3895(19) . ? S1 C12 1.782(7) . ? S1 C13 1.810(7) . ? C12 C11 1.379(9) . ? C12 C7 1.394(9) . ? C7 C8 1.387(9) . ? C7 N2 1.421(8) . ? C8 C9 1.368(9) . ? C11 C10 1.384(9) . ? C10 C9 1.375(9) . ? N2 C6 1.283(8) . ? C6 C5 1.461(9) . ? C4 C5 1.378(9) . ? C4 C3 1.394(10) . ? C2 C3 1.375(9) . ? C2 C1 1.389(9) . ? C1 N1 1.329(8) . ? C5 N1 1.347(8) . ? N5 N4 1.175(9) . ? N3 N4 1.209(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C14 N6 Cu1 159.4(7) . . ? N6 C14 S3 179.1(9) . . ? N3 Cu1 N2 164.4(2) . . ? N3 Cu1 N1 95.1(2) . . ? N2 Cu1 N1 80.2(2) . . ? N3 Cu1 N6 99.0(2) . . ? N2 Cu1 N6 96.6(2) . . ? N1 Cu1 N6 106.6(2) . . ? N3 Cu1 S1 96.41(18) . . ? N2 Cu1 S1 81.67(17) . . ? N1 Cu1 S1 151.11(17) . . ? N6 Cu1 S1 97.64(17) . . ? C12 S1 C13 100.8(3) . . ? C12 S1 Cu1 95.3(2) . . ? C13 S1 Cu1 107.7(2) . . ? C11 C12 C7 120.2(6) . . ? C11 C12 S1 121.0(5) . . ? C7 C12 S1 118.7(5) . . ? C8 C7 C12 120.1(6) . . ? C8 C7 N2 124.1(6) . . ? C12 C7 N2 115.7(6) . . ? C9 C8 C7 118.8(7) . . ? C12 C11 C10 119.3(6) . . ? C9 C10 C11 119.9(7) . . ? C8 C9 C10 121.6(7) . . ? C6 N2 C7 124.4(6) . . ? C6 N2 Cu1 114.9(5) . . ? C7 N2 Cu1 120.6(4) . . ? N2 C6 C5 117.2(6) . . ? C5 C4 C3 118.3(6) . . ? C3 C2 C1 119.1(7) . . ? C2 C3 C4 118.6(6) . . ? N1 C1 C2 123.1(7) . . ? N1 C5 C4 123.4(6) . . ? N1 C5 C6 113.9(6) . . ? C4 C5 C6 122.7(7) . . ? C1 N1 C5 117.5(6) . . ? C1 N1 Cu1 128.9(5) . . ? C5 N1 Cu1 113.6(4) . . ? N4 N3 Cu1 117.4(5) . . ? N5 N4 N3 177.3(7) . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF