data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Hatsumi Mori' _publ_contact_author_email hmori@issp.u-tokyo.ac.jp _publ_section_title ; Metallic Coordination Supramolecule, [Cu(I)Cl0.2Br1.3(pyra-TTF)0.5+] ; loop_ _publ_author_name 'Hatsumi Mori' 'Shun Ichikawa' 'Kazuyuki Takahashi' 'Masaki Matsuda' 'Hiroyuki Tajima' # Attachment '- CIF_CCDC 751037_ichikawa139_2_293K.cif' #============================================================================== data__Cytidine_(Rigaku_Master_f _database_code_depnum_ccdc_archive 'CCDC 751037' #TrackingRef '- CIF_CCDC 751037_ichikawa139_2_293K.cif' _audit_creation_date 2009-06-04 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C8 H4 Br1.31 Cl0.19 Cu N2 S4 ' _chemical_formula_moiety 'C8 H4 Br1.31 Cl0.19 Cu N2 S4 ' _chemical_formula_weight 431.33 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _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_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 7.4390(7) _cell_length_b 11.964(2) _cell_length_c 7.0620(12) _cell_angle_alpha 90.170(14) _cell_angle_beta 105.226(9) _cell_angle_gamma 84.984(10) _cell_volume 603.98(15) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15.2 _cell_measurement_theta_max 17.3 _cell_measurement_temperature 298.1 #------------------------------------------------------------------------------ _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 2.372 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 416.16 _exptl_absorpt_coefficient_mu 6.858 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.178 _exptl_absorpt_correction_T_max 0.254 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 3784 _diffrn_reflns_av_R_equivalents 0.020 _diffrn_reflns_theta_max 30.00 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_standards_number 3 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 298.1 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3520 _reflns_number_gt 2500 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0436 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 2500 _refine_ls_number_parameters 162 _refine_ls_goodness_of_fit_ref 0.776 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0010Fo^2^ + 3.0000\s(Fo^2^) + 0.5000]' _refine_ls_shift/su_max 0.0041 _refine_diff_density_max 1.17 _refine_diff_density_min -0.73 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Br Br -0.290 2.459 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Br(1) Br -0.23277(9) 0.10370(6) 0.44335(10) 0.04354(17) Uani 0.89 1 d P . . Br(2) Br 0.0000 0.0000 1.0000 0.0603(3) Uani 0.84 2 d SP . . Cu(1) Cu 0.05653(8) 0.05337(5) 0.68810(10) 0.04613(17) Uani 1.00 1 d . . . Cl(1) Cl -0.209(4) 0.096(2) 0.514(4) 0.0887 Uiso 0.11 1 d P . . Cl(2) Cl 0.0000 0.0000 1.0000 0.0887 Uiso 0.16 2 d SP . . S(1) S -0.01371(13) 0.33855(8) 0.72147(17) 0.0320(2) Uani 1.00 1 d . . . S(2) S 0.28978(13) 0.49250(8) 0.81866(18) 0.0352(2) Uani 1.00 1 d . . . S(3) S -0.31602(14) 0.55389(10) 0.68119(18) 0.0396(2) Uani 1.00 1 d . . . S(4) S -0.01446(17) 0.70281(9) 0.77491(19) 0.0419(3) Uani 1.00 1 d . . . N(1) N 0.2532(4) 0.1665(2) 0.7604(5) 0.0332(8) Uani 1.00 1 d . . . N(2) N 0.5384(4) 0.3129(2) 0.8584(6) 0.0389(9) Uani 1.00 1 d . . . C(1) C 0.4368(5) 0.1300(3) 0.8042(7) 0.0412(12) Uani 1.00 1 d . . . C(2) C 0.5755(5) 0.2018(3) 0.8541(7) 0.0444(12) Uani 1.00 1 d . . . C(3) C 0.2163(5) 0.2774(3) 0.7690(5) 0.0277(9) Uani 1.00 1 d . . . C(4) C 0.3586(5) 0.3491(3) 0.8149(6) 0.0311(10) Uani 1.00 1 d . . . C(5) C 0.0508(5) 0.4752(3) 0.7597(5) 0.0281(9) Uani 1.00 1 d . . . C(6) C -0.0770(5) 0.5658(3) 0.7439(6) 0.0297(9) Uani 1.00 1 d . . . C(7) C -0.3784(6) 0.6967(4) 0.6740(7) 0.0496(13) Uani 1.00 1 d . . . C(8) C -0.2420(7) 0.7636(4) 0.7159(7) 0.0509(14) Uani 1.00 1 d . . . H(1) H 0.4705 0.0533 0.8025 0.049 Uiso 1.00 1 c R . . H(2) H 0.7007 0.1726 0.8833 0.052 Uiso 1.00 1 c R . . H(3) H -0.5043 0.7248 0.6409 0.058 Uiso 1.00 1 c R . . H(4) H -0.2676 0.8412 0.7139 0.060 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br(1) 0.0371(3) 0.0354(3) 0.0537(4) 0.0089(2) 0.0081(2) -0.0086(2) Br(2) 0.0714(6) 0.0642(6) 0.0519(6) 0.0212(4) 0.0364(4) 0.0200(4) Cu(1) 0.0386(3) 0.0394(3) 0.0633(4) -0.0061(2) 0.0177(2) -0.0032(2) S(1) 0.0243(4) 0.0274(4) 0.0466(6) -0.0051(3) 0.0123(4) -0.0028(4) S(2) 0.0257(4) 0.0274(4) 0.0541(6) -0.0063(3) 0.0120(4) -0.0068(4) S(3) 0.0263(4) 0.0430(6) 0.0495(6) 0.0004(4) 0.0112(4) 0.0018(5) S(4) 0.0488(6) 0.0278(5) 0.0503(7) -0.0055(4) 0.0147(5) -0.0014(5) N(1) 0.0337(16) 0.0243(16) 0.043(2) -0.0025(13) 0.0122(15) -0.0021(15) N(2) 0.0256(15) 0.0326(18) 0.058(2) -0.0027(13) 0.0096(16) -0.0082(17) C(1) 0.038(2) 0.031(2) 0.053(2) 0.0009(17) 0.011(2) -0.002(2) C(2) 0.0264(19) 0.039(2) 0.063(3) 0.0030(16) 0.006(2) -0.007(2) C(3) 0.0280(17) 0.0248(17) 0.033(2) -0.0012(13) 0.0130(16) 0.0003(15) C(4) 0.0268(17) 0.0278(19) 0.041(2) -0.0043(14) 0.0117(16) -0.0054(17) C(5) 0.0276(17) 0.0267(18) 0.032(2) -0.0044(14) 0.0106(15) 0.0000(15) C(6) 0.0287(18) 0.0291(19) 0.033(2) -0.0033(14) 0.0111(16) -0.0010(16) C(7) 0.042(2) 0.049(2) 0.053(3) 0.018(2) 0.012(2) 0.004(2) C(8) 0.062(3) 0.035(2) 0.052(3) 0.016(2) 0.016(2) 0.002(2) #============================================================================== _computing_data_collection WinAFC _computing_cell_refinement WinAFC _computing_data_reduction CrystalStructure _computing_structure_solution ? _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Br(1) Cu(1) 2.4099(7) yes . . Br(1) Cu(1) 2.5119(9) yes . 2_556 Br(1) Cl(1) 0.49(3) yes . . Br(2) Cu(1) 2.4450(7) yes . . Br(2) Cu(1) 2.4450(7) yes . 2_557 Cu(1) Cl(1) 2.06(2) yes . . Cu(1) Cl(1) 2.65(3) yes . 2_556 Cu(1) Cl(2) 2.4450(7) yes . . Cu(1) N(1) 2.045(3) yes . . S(1) C(3) 1.748(3) yes . . S(1) C(5) 1.745(3) yes . . S(2) C(4) 1.749(3) yes . . S(2) C(5) 1.747(3) yes . . S(3) C(6) 1.735(3) yes . . S(3) C(7) 1.728(5) yes . . S(4) C(6) 1.740(4) yes . . S(4) C(8) 1.728(5) yes . . N(1) C(1) 1.351(5) yes . . N(1) C(3) 1.336(4) yes . . N(2) C(2) 1.336(5) yes . . N(2) C(4) 1.325(4) yes . . C(1) C(2) 1.374(6) yes . . C(3) C(4) 1.393(5) yes . . C(5) C(6) 1.362(5) yes . . C(7) C(8) 1.319(7) yes . . C(1) H(1) 0.931 no . . C(2) H(2) 0.935 no . . C(7) H(3) 0.936 no . . C(8) H(4) 0.931 no . . 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cu(1) Br(1) Cu(1) 72.07(2) yes . . 2_556 Cu(1) Br(1) Cl(1) 39(3) yes . . . Cu(1) Br(1) Cl(1) 101(3) yes 2_556 . . Cu(1) Br(2) Cu(1) 180.00(2) yes . . 2_557 Br(1) Cu(1) Br(1) 107.93(3) yes . . 2_556 Br(1) Cu(1) Br(2) 111.32(3) yes . . . Br(1) Cu(1) Cl(1) 8.6(10) yes . . . Br(1) Cu(1) Cl(1) 98.6(6) yes . . 2_556 Br(1) Cu(1) Cl(2) 111.32(3) yes . . . Br(1) Cu(1) N(1) 119.62(9) yes . . . Br(1) Cu(1) Br(2) 111.50(2) yes 2_556 . . Br(1) Cu(1) Cl(1) 113.9(9) yes 2_556 . . Br(1) Cu(1) Cl(1) 10.4(6) yes 2_556 . 2_556 Br(1) Cu(1) Cl(2) 111.50(2) yes 2_556 . . Br(1) Cu(1) N(1) 101.18(10) yes 2_556 . . Br(2) Cu(1) Cl(1) 102.9(10) yes . . . Br(2) Cu(1) Cl(1) 120.4(7) yes . . 2_556 Br(2) Cu(1) Cl(2) 0.0000 yes . . . Br(2) Cu(1) N(1) 104.88(11) yes . . . Cl(1) Cu(1) Cl(1) 105.1(11) yes . . 2_556 Cl(1) Cu(1) Cl(2) 102.9(10) yes . . . Cl(1) Cu(1) N(1) 122.3(8) yes . . . Cl(1) Cu(1) Cl(2) 120.4(7) yes 2_556 . . Cl(1) Cu(1) N(1) 102.7(6) yes 2_556 . . Cl(2) Cu(1) N(1) 104.88(11) yes . . . Br(1) Cl(1) Cu(1) 132(4) yes . . . Br(1) Cl(1) Cu(1) 69(3) yes . . 2_556 Cu(1) Cl(1) Cu(1) 74.9(9) yes . . 2_556 Cu(1) Cl(2) Cu(1) 180.00(2) yes . . 2_557 C(3) S(1) C(5) 94.45(17) yes . . . C(4) S(2) C(5) 94.62(17) yes . . . C(6) S(3) C(7) 95.1(2) yes . . . C(6) S(4) C(8) 94.8(2) yes . . . Cu(1) N(1) C(1) 119.7(2) yes . . . Cu(1) N(1) C(3) 125.1(2) yes . . . C(1) N(1) C(3) 115.1(3) yes . . . C(2) N(2) C(4) 115.4(3) yes . . . N(1) C(1) C(2) 122.5(3) yes . . . N(2) C(2) C(1) 122.4(3) yes . . . S(1) C(3) N(1) 121.2(2) yes . . . S(1) C(3) C(4) 117.2(2) yes . . . N(1) C(3) C(4) 121.6(3) yes . . . S(2) C(4) N(2) 120.3(3) yes . . . S(2) C(4) C(3) 116.7(2) yes . . . N(2) C(4) C(3) 123.0(3) yes . . . S(1) C(5) S(2) 117.0(2) yes . . . S(1) C(5) C(6) 122.5(2) yes . . . S(2) C(5) C(6) 120.5(2) yes . . . S(3) C(6) S(4) 114.7(2) yes . . . S(3) C(6) C(5) 122.5(3) yes . . . S(4) C(6) C(5) 122.8(3) yes . . . S(3) C(7) C(8) 117.4(3) yes . . . S(4) C(8) C(7) 118.0(3) yes . . . N(1) C(1) H(1) 118.7 no . . . C(2) C(1) H(1) 118.8 no . . . N(2) C(2) H(2) 118.2 no . . . C(1) C(2) H(2) 119.4 no . . . S(3) C(7) H(3) 120.8 no . . . C(8) C(7) H(3) 121.8 no . . . S(4) C(8) H(4) 121.0 no . . . C(7) C(8) H(4) 121.0 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Cu(1) Br(1) Cu(1) Cl(1) -6.6(10) ? . . 2_556 2_556 Cu(1) Br(1) Cu(1) N(1) 126.40(10) ? . . 2_556 2_556 Cu(1) Br(1) Cu(1) Cl(1) 27(3) ? . . 2_556 . Cu(1) Br(1) Cu(1) Br(2) -122.66(3) ? 2_556 . . . Cu(1) Br(1) Cu(1) Cl(1) -135(5) ? 2_556 . . . Cu(1) Br(1) Cu(1) Cl(2) -122.66(3) ? 2_556 . . . Cu(1) Br(1) Cu(1) N(1) 114.73(13) ? 2_556 . . . Cu(1) Br(1) Cu(1) Cl(1) 4.8(7) ? 2_556 . . 2_556 Cu(1) Br(1) Cl(1) Cu(1) -43(4) ? . . . 2_556 Cl(1) Br(1) Cu(1) Br(1) 135(5) ? . . . 2_556 Cl(1) Br(1) Cu(1) Br(2) 12(5) ? . . . . Cl(1) Br(1) Cu(1) Cl(2) 12(5) ? . . . . Cl(1) Br(1) Cu(1) N(1) -110(5) ? . . . . Cl(1) Br(1) Cu(1) Cl(1) 140(5) ? . . . 2_556 Cu(1) Br(1) Cl(1) Cu(1) 43(4) ? 2_556 . . . Cl(1) Br(1) Cu(1) Br(1) -27(3) ? . . 2_556 2_556 Cl(1) Br(1) Cu(1) Cl(1) -34(3) ? . . 2_556 2_556 Cl(1) Br(1) Cu(1) N(1) 99(3) ? . . 2_556 2_556 Br(1) Cu(1) Cl(1) Cu(1) 41(5) ? . . . 2_556 Br(1) Cu(1) Cl(1) Br(1) -154(3) ? . . 2_556 2_556 Br(1) Cu(1) Cl(1) Cu(1) -5.7(8) ? . . 2_556 2_556 Br(1) Cu(1) N(1) C(1) -144.1(3) ? . . . . Br(1) Cu(1) N(1) C(3) 35.9(4) ? . . . . Br(1) Cu(1) Cl(1) Br(1) -47(5) ? 2_556 . . . Br(1) Cu(1) Cl(1) Cu(1) -6.0(9) ? 2_556 . . 2_556 Br(1) Cu(1) Cl(1) Cu(1) 148(4) ? 2_556 . 2_556 2_556 Br(1) Cu(1) N(1) C(1) -25.9(3) ? 2_556 . . . Br(1) Cu(1) N(1) C(3) 154.1(3) ? 2_556 . . . Br(2) Cu(1) Cl(1) Br(1) -168(5) ? . . . . Br(2) Cu(1) Cl(1) Cu(1) -126.8(4) ? . . . 2_556 Br(2) Cu(1) Cl(1) Br(1) -33(4) ? . . 2_556 2_556 Br(2) Cu(1) Cl(1) Cu(1) 115.2(6) ? . . 2_556 2_556 Br(2) Cu(1) N(1) C(1) 90.1(3) ? . . . . Br(2) Cu(1) N(1) C(3) -89.8(3) ? . . . . Cl(1) Cu(1) Cl(1) Br(1) -148(3) ? . . 2_556 2_556 Cl(1) Cu(1) Cl(1) Br(1) -41(5) ? 2_556 . . . Cl(2) Cu(1) Cl(1) Br(1) -168(5) ? . . . . Cl(2) Cu(1) Cl(1) Cu(1) -126.8(4) ? . . . 2_556 Cl(1) Cu(1) N(1) C(1) -153.7(12) ? . . . . Cl(1) Cu(1) N(1) C(3) 26.3(12) ? . . . . N(1) Cu(1) Cl(1) Br(1) 75(5) ? . . . . N(1) Cu(1) Cl(1) Cu(1) 116.1(5) ? . . . 2_556 Cl(2) Cu(1) Cl(1) Br(1) -33(4) ? . . 2_556 2_556 Cl(2) Cu(1) Cl(1) Cu(1) 115.2(6) ? . . 2_556 2_556 Cl(1) Cu(1) N(1) C(1) -36.4(7) ? 2_556 . . . Cl(1) Cu(1) N(1) C(3) 143.6(7) ? 2_556 . . . N(1) Cu(1) Cl(1) Br(1) 83(3) ? . . 2_556 2_556 N(1) Cu(1) Cl(1) Cu(1) -128.9(6) ? . . 2_556 2_556 Cl(2) Cu(1) N(1) C(1) 90.1(3) ? . . . . Cl(2) Cu(1) N(1) C(3) -89.8(3) ? . . . . C(3) S(1) C(5) S(2) 0.9(2) ? . . . . C(3) S(1) C(5) C(6) -179.5(3) ? . . . . C(5) S(1) C(3) N(1) 179.9(2) ? . . . . C(5) S(1) C(3) C(4) -0.4(3) ? . . . . C(4) S(2) C(5) S(1) -1.0(2) ? . . . . C(4) S(2) C(5) C(6) 179.4(3) ? . . . . C(5) S(2) C(4) N(2) -177.9(4) ? . . . . C(5) S(2) C(4) C(3) 0.7(3) ? . . . . C(6) S(3) C(7) C(8) -0.8(5) ? . . . . C(7) S(3) C(6) S(4) 1.6(3) ? . . . . C(7) S(3) C(6) C(5) -175.9(4) ? . . . . C(6) S(4) C(8) C(7) 1.2(5) ? . . . . C(8) S(4) C(6) S(3) -1.7(3) ? . . . . C(8) S(4) C(6) C(5) 175.8(4) ? . . . . Cu(1) N(1) C(1) C(2) -179.9(3) ? . . . . Cu(1) N(1) C(3) S(1) 1.3(5) ? . . . . Cu(1) N(1) C(3) C(4) -178.4(3) ? . . . . C(1) N(1) C(3) S(1) -178.7(3) ? . . . . C(1) N(1) C(3) C(4) 1.6(6) ? . . . . C(3) N(1) C(1) C(2) 0.1(6) ? . . . . C(2) N(2) C(4) S(2) 179.0(3) ? . . . . C(2) N(2) C(4) C(3) 0.5(7) ? . . . . C(4) N(2) C(2) C(1) 1.2(7) ? . . . . N(1) C(1) C(2) N(2) -1.6(8) ? . . . . S(1) C(3) C(4) S(2) -0.2(3) ? . . . . S(1) C(3) C(4) N(2) 178.3(3) ? . . . . N(1) C(3) C(4) S(2) 179.4(3) ? . . . . N(1) C(3) C(4) N(2) -2.0(7) ? . . . . S(1) C(5) C(6) S(3) -0.8(5) ? . . . . S(1) C(5) C(6) S(4) -178.1(2) ? . . . . S(2) C(5) C(6) S(3) 178.7(2) ? . . . . S(2) C(5) C(6) S(4) 1.5(5) ? . . . . S(3) C(7) C(8) S(4) -0.3(4) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Br(1) C(7) 3.507(4) ? . 2_466 Cl(1) C(2) 3.41(3) ? . 1_455 S(1) S(4) 3.5964(18) ? . 2_566 S(1) S(4) 3.5410(18) ? . 2_567 S(2) S(2) 3.5017(13) ? . 2_667 S(2) S(3) 3.4579(16) ? . 1_655 S(2) S(3) 3.5288(18) ? . 2_567 S(2) N(2) 3.349(3) ? . 2_667 S(3) S(2) 3.4579(16) ? . 1_455 S(3) S(2) 3.5288(18) ? . 2_567 S(3) S(3) 3.5528(14) ? . 2_466 S(3) N(2) 3.511(4) ? . 1_455 S(4) S(1) 3.5964(18) ? . 2_566 S(4) S(1) 3.5410(18) ? . 2_567 N(1) C(8) 3.446(6) ? . 2_566 N(2) S(2) 3.349(3) ? . 2_667 N(2) S(3) 3.511(4) ? . 1_655 C(2) Cl(1) 3.41(3) ? . 1_655 C(3) C(8) 3.510(7) ? . 2_566 C(4) C(7) 3.533(7) ? . 2_566 C(5) C(5) 3.585(5) ? . 2_566 C(5) C(6) 3.493(6) ? . 2_567 C(6) C(5) 3.493(6) ? . 2_567 C(7) Br(1) 3.507(4) ? . 2_466 C(7) C(4) 3.533(7) ? . 2_566 C(8) N(1) 3.446(6) ? . 2_566 C(8) C(3) 3.510(7) ? . 2_566 Br(1) H(2) 3.362 ? . 1_455 Br(1) H(3) 2.662 ? . 2_466 Br(1) H(4) 3.590 ? . 2_466 Br(2) H(2) 2.854 ? . 1_455 Br(2) H(2) 2.854 ? . 2_657 Br(2) H(4) 3.190 ? . 1_545 Br(2) H(4) 3.190 ? . 2_567 Cu(1) H(2) 3.491 ? . 1_455 Cl(1) H(1) 3.592 ? . 1_455 Cl(1) H(2) 2.984 ? . 1_455 Cl(1) H(3) 2.884 ? . 2_466 Cl(1) H(4) 3.478 ? . 1_545 Cl(2) H(2) 2.854 ? . 1_455 Cl(2) H(2) 2.854 ? . 2_657 Cl(2) H(4) 3.190 ? . 1_545 Cl(2) H(4) 3.190 ? . 2_567 S(1) H(2) 3.433 ? . 1_455 S(4) H(2) 3.335 ? . 2_667 N(1) H(4) 3.380 ? . 2_566 N(2) H(3) 3.499 ? . 2_566 C(1) H(1) 3.431 ? . 2_657 C(1) H(4) 3.550 ? . 2_566 C(2) H(3) 3.498 ? . 2_566 H(1) Cl(1) 3.592 ? . 1_655 H(1) C(1) 3.431 ? . 2_657 H(1) H(1) 2.981 ? . 2_657 H(1) H(4) 3.224 ? . 1_645 H(2) Br(1) 3.362 ? . 1_655 H(2) Br(2) 2.854 ? . 1_655 H(2) Cu(1) 3.491 ? . 1_655 H(2) Cl(1) 2.984 ? . 1_655 H(2) Cl(2) 2.854 ? . 1_655 H(2) S(1) 3.433 ? . 1_655 H(2) S(4) 3.335 ? . 2_667 H(3) Br(1) 2.662 ? . 2_466 H(3) Cl(1) 2.884 ? . 2_466 H(3) N(2) 3.499 ? . 2_566 H(3) C(2) 3.498 ? . 2_566 H(4) Br(1) 3.590 ? . 2_466 H(4) Br(2) 3.190 ? . 1_565 H(4) Cl(1) 3.478 ? . 1_565 H(4) Cl(2) 3.190 ? . 1_565 H(4) N(1) 3.380 ? . 2_566 H(4) C(1) 3.550 ? . 2_566 H(4) H(1) 3.224 ? . 1_465 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment '- CIF_CCDC 751038_090630_Pyra-TTFCuCl0.2Br1.3_120K.cif' data___090630 _database_code_depnum_ccdc_archive 'CCDC 751038' #TrackingRef '- CIF_CCDC 751038_090630_Pyra-TTFCuCl0.2Br1.3_120K.cif' _audit_creation_date 2009-10-11 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C16 H8 Br2.54 Cl0.46 Cu2 N4 S8 ' _chemical_formula_moiety 'C16 H8 Br2.54 Cl0.46 Cu2 N4 S8 ' _chemical_formula_weight 859.10 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _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_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 11.508(7) _cell_length_b 13.522(7) _cell_length_c 8.643(5) _cell_angle_alpha 106.62(2) _cell_angle_beta 93.65(2) _cell_angle_gamma 66.583(13) _cell_volume 1180.7(12) _cell_formula_units_Z 2 _cell_measurement_reflns_used 2271 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 120.0 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 2.416 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 829.44 _exptl_absorpt_coefficient_mu 6.889 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.186 _exptl_absorpt_correction_T_max 0.252 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 9120 _diffrn_reflns_av_R_equivalents 0.019 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.952 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 9 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5140 _reflns_number_gt 4161 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0767 _refine_ls_wR_factor_ref 0.0907 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 4161 _refine_ls_number_parameters 197 _refine_ls_goodness_of_fit_ref 1.716 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0010Fo^2^ + 3.0000\s(Fo^2^) + 0.5000]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 10.70 _refine_diff_density_min -8.35 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Br Br -0.290 2.459 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Br(1) Br 0.27694(19) 0.10864(19) -0.3447(2) 0.0162(7) Uiso 0.93 1 d P . . Br(2) Br 0.5000 0.0000 0.0000 0.0263(16) Uiso 0.85 2 d SP . . Br(3) Br 0.2067(2) 0.89994(19) 0.8465(2) 0.0142(8) Uiso 0.81 1 d P . . Br(4) Br 0.0000 1.0000 0.5000 0.0256(18) Uiso 0.76 2 d SP . . Cu(1) Cu 0.2874(2) 0.0512(2) -0.0962(2) 0.0192(7) Uani 1.00 1 d . . . Cu(2) Cu 0.2142(2) 0.9440(2) 0.6039(2) 0.0164(7) Uani 1.00 1 d . . . Cl(1) Cl 0.27698(19) 0.10866(19) -0.3447(2) 0.0127 Uiso 0.07 1 d P . . Cl(2) Cl 0.5000 0.0000 0.0000 0.0127 Uiso 0.16 2 d SP . . Cl(3) Cl 0.2068(2) 0.89993(19) 0.8465(2) 0.0127 Uiso 0.19 1 d P . . Cl(4) Cl 0.0000 1.0000 0.5000 0.0127 Uiso 0.24 2 d SP . . S(1) S 0.0408(6) 0.7011(5) 0.2305(5) 0.0180(16) Uani 1.00 1 d . . . S(2) S 0.2223(5) 0.5515(5) -0.0420(5) 0.0129(14) Uani 1.00 1 d . . . S(3) S 0.0138(5) 0.4915(5) 0.2998(5) 0.0139(15) Uani 1.00 1 d . . . S(4) S 0.1969(6) 0.3361(4) 0.0227(5) 0.0149(15) Uani 1.00 1 d . . . S(5) S 0.2754(5) 0.4461(5) 0.5358(6) 0.0186(17) Uani 1.00 1 d . . . S(6) S 0.4580(5) 0.2950(4) 0.2620(5) 0.0152(15) Uani 1.00 1 d . . . S(7) S 0.3026(5) 0.6600(5) 0.4754(5) 0.0107(14) Uani 1.00 1 d . . . S(8) S 0.4878(5) 0.5042(4) 0.1960(5) 0.0131(15) Uani 1.00 1 d . . . N(1) N -0.0001(14) 0.3090(12) 0.3574(15) 0.008(3) Uiso 1.00 1 d . . . N(2) N 0.1683(13) 0.1627(11) 0.0994(14) 0.005(2) Uiso 1.00 1 d . . . N(3) N 0.3325(15) 0.8284(13) 0.4162(16) 0.015(3) Uiso 1.00 1 d . . . N(4) N 0.5082(16) 0.6775(14) 0.1457(17) 0.023(4) Uiso 1.00 1 d . . . C(1) C 0.0959(19) 0.7649(18) 0.116(2) 0.010(4) Uiso 1.00 1 d . . . C(2) C 0.1743(16) 0.7026(14) 0.0026(18) 0.007(3) Uiso 1.00 1 d . . . C(3) C 0.1244(17) 0.5646(16) 0.1140(18) 0.005(4) Uiso 1.00 1 d . . . C(4) C 0.118(2) 0.4717(18) 0.136(2) 0.020(4) Uiso 1.00 1 d . . . C(5) C 0.0451(19) 0.3508(17) 0.261(2) 0.007(4) Uiso 1.00 1 d . . . C(6) C 0.1330(16) 0.2708(14) 0.1321(18) 0.011(3) Uiso 1.00 1 d . . . C(7) C 0.0374(19) 0.1954(18) 0.316(2) 0.023(5) Uiso 1.00 1 d . . . C(8) C 0.108(2) 0.1352(18) 0.189(2) 0.023(5) Uiso 1.00 1 d . . . C(9) C 0.3785(17) 0.8749(15) 0.3143(18) 0.008(3) Uiso 1.00 1 d . . . C(10) C 0.4742(16) 0.7904(15) 0.1815(19) 0.010(3) Uiso 1.00 1 d . . . C(11) C 0.3630(16) 0.7171(14) 0.3679(17) 0.008(3) Uiso 1.00 1 d . . . C(12) C 0.448(2) 0.6508(19) 0.237(2) 0.012(4) Uiso 1.00 1 d . . . C(13) C 0.3880(16) 0.5216(15) 0.3483(18) 0.003(3) Uiso 1.00 1 d . . . C(14) C 0.372(2) 0.4316(19) 0.376(2) 0.016(5) Uiso 1.00 1 d . . . C(15) C 0.314(2) 0.3129(18) 0.510(2) 0.028(5) Uiso 1.00 1 d . . . C(16) C 0.404(2) 0.236(2) 0.370(2) 0.026(5) Uiso 1.00 1 d . . . H(1) H 0.0660 0.8443 0.1392 0.012 Uiso 1.00 1 c R . . H(2) H 0.2070 0.7309 -0.0652 0.008 Uiso 1.00 1 c R . . H(3) H 0.0025 0.1644 0.3775 0.028 Uiso 1.00 1 c R . . H(4) H 0.1291 0.0567 0.1634 0.028 Uiso 1.00 1 c R . . H(5) H 0.3566 0.9534 0.3366 0.010 Uiso 1.00 1 c R . . H(6) H 0.5068 0.8189 0.1138 0.012 Uiso 1.00 1 c R . . H(7) H 0.2796 0.2852 0.5766 0.033 Uiso 1.00 1 c R . . H(8) H 0.4285 0.1570 0.3432 0.031 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu(1) 0.0163(16) 0.0199(17) 0.0216(12) -0.0067(13) 0.0065(12) 0.0056(11) Cu(2) 0.0163(16) 0.0166(16) 0.0175(11) -0.0083(12) 0.0057(11) 0.0024(11) S(1) 0.016(3) 0.020(3) 0.015(2) -0.007(2) 0.005(2) -0.000(2) S(2) 0.008(2) 0.020(3) 0.013(2) -0.003(2) -0.001(2) 0.011(2) S(3) 0.008(3) 0.017(3) 0.017(2) -0.004(2) 0.005(2) 0.005(2) S(4) 0.015(3) 0.008(3) 0.023(2) -0.003(2) 0.011(2) 0.006(2) S(5) 0.018(3) 0.021(3) 0.023(2) -0.015(3) 0.006(2) 0.004(2) S(6) 0.014(3) 0.009(3) 0.023(2) -0.004(2) 0.000(2) 0.005(2) S(7) 0.006(2) 0.021(3) 0.005(2) -0.009(2) 0.000(2) -0.001(2) S(8) 0.018(3) 0.009(3) 0.013(2) -0.009(2) 0.008(2) -0.003(2) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR2002 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Br(1) Cu(1) 2.465(3) yes . . Br(1) Cl(1) 0.001(4) yes . . Br(2) Cu(1) 2.426(2) yes . . Br(2) Cu(1) 2.426(2) yes . 2_655 Br(3) Cu(2) 2.353(3) yes . . Br(3) Cl(3) 0.001(4) yes . . Br(4) Cu(2) 2.466(2) yes . . Br(4) Cu(2) 2.466(2) yes . 2_576 Cu(1) Cl(1) 2.465(3) yes . . Cu(1) Cl(2) 2.426(2) yes . . Cu(1) N(2) 2.050(11) yes . . Cu(2) Cl(3) 2.352(3) yes . . Cu(2) Cl(4) 2.466(2) yes . . Cu(2) N(3) 2.017(12) yes . . S(1) C(1) 1.77(2) yes . . S(1) C(3) 1.730(17) yes . . S(2) C(2) 1.819(19) yes . . S(2) C(3) 1.74(2) yes . . S(3) C(4) 1.80(2) yes . . S(3) C(5) 1.72(2) yes . . S(4) C(4) 1.707(19) yes . . S(4) C(6) 1.82(2) yes . . S(5) C(14) 1.74(2) yes . . S(5) C(15) 1.62(2) yes . . S(6) C(14) 1.73(2) yes . . S(6) C(16) 1.67(3) yes . . S(7) C(11) 1.69(2) yes . . S(7) C(13) 1.782(15) yes . . S(8) C(12) 1.78(2) yes . . S(8) C(13) 1.71(2) yes . . N(1) C(5) 1.35(3) yes . . N(1) C(7) 1.36(2) yes . . N(2) C(6) 1.30(2) yes . . N(2) C(8) 1.28(3) yes . . N(3) C(9) 1.45(3) yes . . N(3) C(11) 1.34(2) yes . . N(4) C(10) 1.36(2) yes . . N(4) C(12) 1.29(3) yes . . C(1) C(2) 1.23(2) yes . . C(3) C(4) 1.36(3) yes . . C(5) C(6) 1.42(2) yes . . C(7) C(8) 1.27(2) yes . . C(9) C(10) 1.50(2) yes . . C(11) C(12) 1.38(2) yes . . C(13) C(14) 1.39(3) yes . . C(15) C(16) 1.48(2) yes . . C(1) H(1) 0.950 no . . C(2) H(2) 0.950 no . . C(7) H(3) 0.950 no . . C(8) H(4) 0.950 no . . C(9) H(5) 0.950 no . . C(10) H(6) 0.950 no . . C(15) H(7) 0.950 no . . C(16) H(8) 0.950 no . . 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cu(1) Br(1) Cu(2) 69.49(12) yes . . 1_544 Cu(1) Br(1) Cl(1) 124(123) yes . . . Cu(2) Br(1) Cl(1) 147(159) yes 1_544 . . Cu(1) Br(2) Cu(1) 180.00(14) yes . . 2_655 Cu(1) Br(3) Cu(2) 71.91(13) yes 1_566 . . Cu(1) Br(3) Cl(3) 63(123) yes 1_566 . . Cu(2) Br(3) Cl(3) 54(128) yes . . . Cu(2) Br(4) Cu(2) 0(440) yes . . 2_576 Br(1) Cu(1) Br(2) 110.56(14) yes . . . Br(1) Cu(1) Br(3) 107.90(12) yes . . 1_544 Br(1) Cu(1) Cl(1) 0.01(7) yes . . . Br(1) Cu(1) Cl(2) 110.56(14) yes . . . Br(1) Cu(1) Cl(3) 107.89(12) yes . . 1_544 Br(1) Cu(1) N(2) 118.5(4) yes . . . Br(2) Cu(1) Br(3) 114.36(12) yes . . 1_544 Br(2) Cu(1) Cl(1) 110.54(14) yes . . . Br(2) Cu(1) Cl(2) 0.0000 yes . . . Br(2) Cu(1) Cl(3) 114.36(12) yes . . 1_544 Br(2) Cu(1) N(2) 105.9(4) yes . . . Br(3) Cu(1) Cl(1) 107.91(12) yes 1_544 . . Br(3) Cu(1) Cl(2) 114.36(12) yes 1_544 . . Br(3) Cu(1) Cl(3) 0.01(6) yes 1_544 . 1_544 Br(3) Cu(1) N(2) 99.4(5) yes 1_544 . . Cl(1) Cu(1) Cl(2) 110.54(14) yes . . . Cl(1) Cu(1) Cl(3) 107.90(12) yes . . 1_544 Cl(1) Cu(1) N(2) 118.5(4) yes . . . Cl(2) Cu(1) Cl(3) 114.36(12) yes . . 1_544 Cl(2) Cu(1) N(2) 105.9(4) yes . . . Cl(3) Cu(1) N(2) 99.4(5) yes 1_544 . . Br(1) Cu(2) Br(3) 110.31(12) yes 1_566 . . Br(1) Cu(2) Br(4) 107.51(11) yes 1_566 . . Br(1) Cu(2) Cl(1) 0.00(8) yes 1_566 . 1_566 Br(1) Cu(2) Cl(3) 110.31(12) yes 1_566 . . Br(1) Cu(2) Cl(4) 107.51(11) yes 1_566 . . Br(1) Cu(2) N(3) 103.6(6) yes 1_566 . . Br(3) Cu(2) Br(4) 108.59(14) yes . . . Br(3) Cu(2) Cl(1) 110.31(12) yes . . 1_566 Br(3) Cu(2) Cl(3) 0.01(8) yes . . . Br(3) Cu(2) Cl(4) 108.59(14) yes . . . Br(3) Cu(2) N(3) 120.2(5) yes . . . Br(4) Cu(2) Cl(1) 107.51(11) yes . . 1_566 Br(4) Cu(2) Cl(3) 108.60(14) yes . . . Br(4) Cu(2) Cl(4) 0.0000 yes . . . Br(4) Cu(2) N(3) 106.0(4) yes . . . Cl(1) Cu(2) Cl(3) 110.31(12) yes 1_566 . . Cl(1) Cu(2) Cl(4) 107.51(11) yes 1_566 . . Cl(1) Cu(2) N(3) 103.6(6) yes 1_566 . . Cl(3) Cu(2) Cl(4) 108.60(14) yes . . . Cl(3) Cu(2) N(3) 120.2(5) yes . . . Cl(4) Cu(2) N(3) 106.0(4) yes . . . Br(1) Cl(1) Cu(1) 56(123) yes . . . Br(1) Cl(1) Cu(2) 33(159) yes . . 1_544 Cu(1) Cl(1) Cu(2) 69.47(12) yes . . 1_544 Cu(1) Cl(2) Cu(1) 180.00(14) yes . . 2_655 Br(3) Cl(3) Cu(1) 117(123) yes . . 1_566 Br(3) Cl(3) Cu(2) 126(128) yes . . . Cu(1) Cl(3) Cu(2) 71.92(13) yes 1_566 . . Cu(2) Cl(4) Cu(2) 0(440) yes . . 2_576 C(1) S(1) C(3) 95.5(10) yes . . . C(2) S(2) C(3) 93.3(9) yes . . . C(4) S(3) C(5) 95.0(10) yes . . . C(4) S(4) C(6) 97.1(10) yes . . . C(14) S(5) C(15) 96.9(11) yes . . . C(14) S(6) C(16) 94.8(12) yes . . . C(11) S(7) C(13) 92.0(8) yes . . . C(12) S(8) C(13) 93.7(9) yes . . . C(5) N(1) C(7) 117.2(14) yes . . . Cu(1) N(2) C(6) 122.7(13) yes . . . Cu(1) N(2) C(8) 123.9(13) yes . . . C(6) N(2) C(8) 112.8(14) yes . . . Cu(2) N(3) C(9) 114.4(11) yes . . . Cu(2) N(3) C(11) 127.9(14) yes . . . C(9) N(3) C(11) 117.4(13) yes . . . C(10) N(4) C(12) 112.8(15) yes . . . S(1) C(1) C(2) 117.6(19) yes . . . S(2) C(2) C(1) 119(2) yes . . . S(1) C(3) S(2) 114.9(14) yes . . . S(1) C(3) C(4) 125.1(15) yes . . . S(2) C(3) C(4) 120.0(12) yes . . . S(3) C(4) S(4) 115.9(16) yes . . . S(3) C(4) C(3) 117.7(13) yes . . . S(4) C(4) C(3) 126.4(16) yes . . . S(3) C(5) N(1) 123.7(11) yes . . . S(3) C(5) C(6) 119.5(19) yes . . . N(1) C(5) C(6) 116.5(19) yes . . . S(4) C(6) N(2) 123.3(12) yes . . . S(4) C(6) C(5) 112.5(16) yes . . . N(2) C(6) C(5) 124(2) yes . . . N(1) C(7) C(8) 119(2) yes . . . N(2) C(8) C(7) 129(2) yes . . . N(3) C(9) C(10) 115.3(16) yes . . . N(4) C(10) C(9) 124(2) yes . . . S(7) C(11) N(3) 119.2(12) yes . . . S(7) C(11) C(12) 121.3(17) yes . . . N(3) C(11) C(12) 119(2) yes . . . S(8) C(12) N(4) 115.1(13) yes . . . S(8) C(12) C(11) 114.4(19) yes . . . N(4) C(12) C(11) 130(2) yes . . . S(7) C(13) S(8) 118.5(13) yes . . . S(7) C(13) C(14) 119.3(13) yes . . . S(8) C(13) C(14) 122.1(12) yes . . . S(5) C(14) S(6) 115.6(16) yes . . . S(5) C(14) C(13) 123.2(13) yes . . . S(6) C(14) C(13) 121.0(15) yes . . . S(5) C(15) C(16) 116(2) yes . . . S(6) C(16) C(15) 117(2) yes . . . S(1) C(1) H(1) 121.7 no . . . C(2) C(1) H(1) 120.7 no . . . S(2) C(2) H(2) 119.1 no . . . C(1) C(2) H(2) 122.2 no . . . N(1) C(7) H(3) 118.8 no . . . C(8) C(7) H(3) 121.9 no . . . N(2) C(8) H(4) 114.5 no . . . C(7) C(8) H(4) 115.6 no . . . N(3) C(9) H(5) 122.4 no . . . C(10) C(9) H(5) 122.0 no . . . N(4) C(10) H(6) 119.0 no . . . C(9) C(10) H(6) 117.0 no . . . S(5) C(15) H(7) 123.0 no . . . C(16) C(15) H(7) 121.3 no . . . S(6) C(16) H(8) 121.7 no . . . C(15) C(16) H(8) 121.4 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Cu(1) Br(1) Cu(2) Br(3) 5.03(11) ? . . 1_544 1_544 Cu(1) Br(1) Cu(2) Br(4) 123.27(11) ? . . 1_544 1_544 Cu(1) Br(1) Cu(2) Cl(3) 5.02(11) ? . . 1_544 1_544 Cu(1) Br(1) Cu(2) Cl(4) 123.27(11) ? . . 1_544 1_544 Cu(1) Br(1) Cu(2) N(3) -124.8(4) ? . . 1_544 1_544 Cu(2) Br(1) Cu(1) Br(2) 121.04(12) ? 1_544 . . . Cu(2) Br(1) Cu(1) Cl(1) 145(163) ? 1_544 . . . Cu(2) Br(1) Cu(1) Cl(2) 121.04(12) ? 1_544 . . . Cu(2) Br(1) Cu(1) N(2) -116.5(5) ? 1_544 . . . Cu(2) Br(1) Cu(1) Br(3) -4.70(10) ? 1_544 . . 1_544 Cu(2) Br(1) Cu(1) Cl(3) -4.69(10) ? 1_544 . . 1_544 Cu(1) Br(1) Cl(1) Cu(2) 105(126) ? . . . 1_544 Cl(1) Br(1) Cu(1) Br(2) -24(175) ? . . . . Cl(1) Br(1) Cu(1) Cl(2) -24(175) ? . . . . Cl(1) Br(1) Cu(1) N(2) 98(99) ? . . . . Cl(1) Br(1) Cu(1) Br(3) -150(167) ? . . . 1_544 Cl(1) Br(1) Cu(1) Cl(3) -150(167) ? . . . 1_544 Cu(2) Br(1) Cl(1) Cu(1) -105(126) ? 1_544 . . . Cl(1) Br(1) Cu(2) Br(3) 126(146) ? . . 1_544 1_544 Cl(1) Br(1) Cu(2) Br(4) -116(147) ? . . 1_544 1_544 Cl(1) Br(1) Cu(2) Cl(3) 126(146) ? . . 1_544 1_544 Cl(1) Br(1) Cu(2) Cl(4) -116(147) ? . . 1_544 1_544 Cl(1) Br(1) Cu(2) N(3) -4(199) ? . . 1_544 1_544 Cu(1) Br(3) Cu(2) Br(1) -4.92(11) ? 1_566 . . 1_566 Cu(1) Br(3) Cu(2) Br(4) -122.50(12) ? 1_566 . . . Cu(1) Br(3) Cu(2) Cl(3) 69(136) ? 1_566 . . . Cu(1) Br(3) Cu(2) Cl(4) -122.50(12) ? 1_566 . . . Cu(1) Br(3) Cu(2) N(3) 115.4(6) ? 1_566 . . . Cu(1) Br(3) Cu(2) Cl(1) -4.92(11) ? 1_566 . . 1_566 Cu(2) Br(3) Cu(1) Br(1) 4.96(11) ? . . 1_566 1_566 Cu(2) Br(3) Cu(1) Br(2) -118.49(12) ? . . 1_566 1_566 Cu(2) Br(3) Cu(1) Cl(1) 4.95(11) ? . . 1_566 1_566 Cu(2) Br(3) Cu(1) Cl(2) -118.49(12) ? . . 1_566 1_566 Cu(2) Br(3) Cu(1) N(2) 129.2(3) ? . . 1_566 1_566 Cu(2) Br(3) Cu(1) Cl(3) -58(136) ? . . 1_566 . Cu(1) Br(3) Cl(3) Cu(2) -87(99) ? 1_566 . . . Cl(3) Br(3) Cu(1) Br(1) 63(138) ? . . 1_566 1_566 Cl(3) Br(3) Cu(1) Br(2) -60(149) ? . . 1_566 1_566 Cl(3) Br(3) Cu(1) Cl(1) 63(138) ? . . 1_566 1_566 Cl(3) Br(3) Cu(1) Cl(2) -60(149) ? . . 1_566 1_566 Cl(3) Br(3) Cu(1) N(2) -173(182) ? . . 1_566 1_566 Cu(2) Br(3) Cl(3) Cu(1) 87(99) ? . . . 1_566 Cl(3) Br(3) Cu(2) Br(1) -74(136) ? . . . 1_566 Cl(3) Br(3) Cu(2) Br(4) 169(186) ? . . . . Cl(3) Br(3) Cu(2) Cl(4) 169(186) ? . . . . Cl(3) Br(3) Cu(2) N(3) 47(117) ? . . . . Cl(3) Br(3) Cu(2) Cl(1) -74(136) ? . . . 1_566 Br(1) Cu(1) Cl(1) Cu(2) -35(163) ? . . . 1_544 Br(1) Cu(1) Cl(3) Br(3) -117(138) ? . . 1_544 1_544 Br(1) Cu(1) Cl(3) Cu(2) 4.95(11) ? . . 1_544 1_544 Br(1) Cu(1) N(2) C(6) -32.8(15) ? . . . . Br(1) Cu(1) N(2) C(8) 137.5(14) ? . . . . Br(2) Cu(1) Cl(1) Br(1) 156(175) ? . . . . Br(2) Cu(1) Cl(1) Cu(2) 121.04(12) ? . . . 1_544 Br(2) Cu(1) Cl(3) Br(3) 120(149) ? . . 1_544 1_544 Br(2) Cu(1) Cl(3) Cu(2) -118.50(12) ? . . 1_544 1_544 Br(2) Cu(1) N(2) C(6) 92.0(13) ? . . . . Br(2) Cu(1) N(2) C(8) -97.7(15) ? . . . . Br(3) Cu(1) Cl(1) Br(1) 30(167) ? 1_544 . . . Br(3) Cu(1) Cl(1) Cu(2) -4.69(10) ? 1_544 . . 1_544 Br(3) Cu(1) Cl(3) Cu(2) 122(136) ? 1_544 . 1_544 1_544 Br(3) Cu(1) N(2) C(6) -149.2(13) ? 1_544 . . . Br(3) Cu(1) N(2) C(8) 21.1(15) ? 1_544 . . . Cl(2) Cu(1) Cl(1) Br(1) 156(175) ? . . . . Cl(2) Cu(1) Cl(1) Cu(2) 121.04(12) ? . . . 1_544 Cl(1) Cu(1) Cl(3) Br(3) -117(138) ? . . 1_544 1_544 Cl(1) Cu(1) Cl(3) Cu(2) 4.94(11) ? . . 1_544 1_544 Cl(3) Cu(1) Cl(1) Br(1) 30(167) ? 1_544 . . . Cl(3) Cu(1) Cl(1) Cu(2) -4.68(10) ? 1_544 . . 1_544 Cl(1) Cu(1) N(2) C(6) -32.8(15) ? . . . . Cl(1) Cu(1) N(2) C(8) 137.5(14) ? . . . . N(2) Cu(1) Cl(1) Br(1) -82(99) ? . . . . N(2) Cu(1) Cl(1) Cu(2) -116.5(5) ? . . . 1_544 Cl(2) Cu(1) Cl(3) Br(3) 120(149) ? . . 1_544 1_544 Cl(2) Cu(1) Cl(3) Cu(2) -118.50(12) ? . . 1_544 1_544 Cl(2) Cu(1) N(2) C(6) 92.0(13) ? . . . . Cl(2) Cu(1) N(2) C(8) -97.7(15) ? . . . . Cl(3) Cu(1) N(2) C(6) -149.2(13) ? 1_544 . . . Cl(3) Cu(1) N(2) C(8) 21.1(15) ? 1_544 . . . N(2) Cu(1) Cl(3) Br(3) 7(182) ? . . 1_544 1_544 N(2) Cu(1) Cl(3) Cu(2) 129.2(3) ? . . 1_544 1_544 Br(1) Cu(2) Cl(3) Br(3) 106(136) ? 1_566 . . . Br(1) Cu(2) Cl(3) Cu(1) -4.91(11) ? 1_566 . . 1_566 Br(1) Cu(2) N(3) C(9) -25.9(12) ? 1_566 . . . Br(1) Cu(2) N(3) C(11) 160.8(14) ? 1_566 . . . Br(3) Cu(2) Cl(1) Br(1) -54(146) ? . . 1_566 1_566 Br(3) Cu(2) Cl(1) Cu(1) 5.03(11) ? . . 1_566 1_566 Br(3) Cu(2) Cl(3) Cu(1) -111(136) ? . . . 1_566 Br(3) Cu(2) N(3) C(9) -149.5(10) ? . . . . Br(3) Cu(2) N(3) C(11) 37.2(17) ? . . . . Br(4) Cu(2) Cl(1) Br(1) 64(147) ? . . 1_566 1_566 Br(4) Cu(2) Cl(1) Cu(1) 123.27(11) ? . . 1_566 1_566 Br(4) Cu(2) Cl(3) Br(3) -11(186) ? . . . . Br(4) Cu(2) Cl(3) Cu(1) -122.49(12) ? . . . 1_566 Br(4) Cu(2) N(3) C(9) 87.1(12) ? . . . . Br(4) Cu(2) N(3) C(11) -86.2(14) ? . . . . Cl(1) Cu(2) Cl(3) Br(3) 106(136) ? 1_566 . . . Cl(1) Cu(2) Cl(3) Cu(1) -4.90(11) ? 1_566 . . 1_566 Cl(3) Cu(2) Cl(1) Br(1) -54(146) ? . . 1_566 1_566 Cl(3) Cu(2) Cl(1) Cu(1) 5.01(11) ? . . 1_566 1_566 Cl(4) Cu(2) Cl(1) Br(1) 64(147) ? . . 1_566 1_566 Cl(4) Cu(2) Cl(1) Cu(1) 123.27(11) ? . . 1_566 1_566 Cl(1) Cu(2) N(3) C(9) -25.9(12) ? 1_566 . . . Cl(1) Cu(2) N(3) C(11) 160.8(14) ? 1_566 . . . N(3) Cu(2) Cl(1) Br(1) 176(199) ? . . 1_566 1_566 N(3) Cu(2) Cl(1) Cu(1) -124.8(4) ? . . 1_566 1_566 Cl(4) Cu(2) Cl(3) Br(3) -11(186) ? . . . . Cl(4) Cu(2) Cl(3) Cu(1) -122.49(12) ? . . . 1_566 Cl(3) Cu(2) N(3) C(9) -149.5(10) ? . . . . Cl(3) Cu(2) N(3) C(11) 37.2(17) ? . . . . N(3) Cu(2) Cl(3) Br(3) -133(117) ? . . . . N(3) Cu(2) Cl(3) Cu(1) 115.4(6) ? . . . 1_566 Cl(4) Cu(2) N(3) C(9) 87.1(12) ? . . . . Cl(4) Cu(2) N(3) C(11) -86.2(14) ? . . . . C(1) S(1) C(3) S(2) 3.0(12) ? . . . . C(1) S(1) C(3) C(4) -176.7(18) ? . . . . C(3) S(1) C(1) C(2) -3.3(18) ? . . . . C(2) S(2) C(3) S(1) -2.1(11) ? . . . . C(2) S(2) C(3) C(4) 177.6(16) ? . . . . C(3) S(2) C(2) C(1) -0.2(15) ? . . . . C(4) S(3) C(5) N(1) 174.4(17) ? . . . . C(4) S(3) C(5) C(6) 1.0(15) ? . . . . C(5) S(3) C(4) S(4) -0.3(6) ? . . . . C(5) S(3) C(4) C(3) 179.0(17) ? . . . . C(4) S(4) C(6) N(2) -176.4(15) ? . . . . C(4) S(4) C(6) C(5) 0.9(15) ? . . . . C(6) S(4) C(4) S(3) -0.2(13) ? . . . . C(6) S(4) C(4) C(3) -179.5(17) ? . . . . C(14) S(5) C(15) C(16) -2.6(19) ? . . . . C(15) S(5) C(14) S(6) 1.9(15) ? . . . . C(15) S(5) C(14) C(13) -173.4(18) ? . . . . C(14) S(6) C(16) C(15) -1.0(16) ? . . . . C(16) S(6) C(14) S(5) -0.7(15) ? . . . . C(16) S(6) C(14) C(13) 174.7(18) ? . . . . C(11) S(7) C(13) S(8) 2.5(11) ? . . . . C(11) S(7) C(13) C(14) -177.9(15) ? . . . . C(13) S(7) C(11) N(3) -177.5(14) ? . . . . C(13) S(7) C(11) C(12) -0.8(14) ? . . . . C(12) S(8) C(13) S(7) -2.9(12) ? . . . . C(12) S(8) C(13) C(14) 177.5(16) ? . . . . C(13) S(8) C(12) N(4) 178.3(16) ? . . . . C(13) S(8) C(12) C(11) 2.3(16) ? . . . . C(5) N(1) C(7) C(8) -3(2) ? . . . . C(7) N(1) C(5) S(3) -176.9(15) ? . . . . C(7) N(1) C(5) C(6) -3(2) ? . . . . Cu(1) N(2) C(6) S(4) -7(2) ? . . . . Cu(1) N(2) C(6) C(5) 176.4(13) ? . . . . Cu(1) N(2) C(8) C(7) 176.1(18) ? . . . . C(6) N(2) C(8) C(7) -13(3) ? . . . . C(8) N(2) C(6) S(4) -178.0(14) ? . . . . C(8) N(2) C(6) C(5) 5(2) ? . . . . Cu(2) N(3) C(9) C(10) 175.6(11) ? . . . . Cu(2) N(3) C(11) S(7) -2(2) ? . . . . Cu(2) N(3) C(11) C(12) -179.1(13) ? . . . . C(9) N(3) C(11) S(7) -175.5(12) ? . . . . C(9) N(3) C(11) C(12) 8(2) ? . . . . C(11) N(3) C(9) C(10) -10(2) ? . . . . C(10) N(4) C(12) S(8) 180.0(12) ? . . . . C(10) N(4) C(12) C(11) -5(3) ? . . . . C(12) N(4) C(10) C(9) 1(2) ? . . . . S(1) C(1) C(2) S(2) 2(2) ? . . . . S(1) C(3) C(4) S(3) -0(2) ? . . . . S(1) C(3) C(4) S(4) 179.2(12) ? . . . . S(2) C(3) C(4) S(3) -179.7(10) ? . . . . S(2) C(3) C(4) S(4) -1(2) ? . . . . S(3) C(5) C(6) S(4) -1.3(19) ? . . . . S(3) C(5) C(6) N(2) 175.9(14) ? . . . . N(1) C(5) C(6) S(4) -175.1(13) ? . . . . N(1) C(5) C(6) N(2) 2(2) ? . . . . N(1) C(7) C(8) N(2) 12(3) ? . . . . N(3) C(9) C(10) N(4) 6(2) ? . . . . S(7) C(11) C(12) S(8) -1.0(18) ? . . . . S(7) C(11) C(12) N(4) -176.3(18) ? . . . . N(3) C(11) C(12) S(8) 175.7(13) ? . . . . N(3) C(11) C(12) N(4) 0(2) ? . . . . S(7) C(13) C(14) S(5) -2(2) ? . . . . S(7) C(13) C(14) S(6) -177.2(10) ? . . . . S(8) C(13) C(14) S(5) 177.5(11) ? . . . . S(8) C(13) C(14) S(6) 2(2) ? . . . . S(5) C(15) C(16) S(6) 3(2) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Br(1) Cu(2) 2.520(4) ? . 1_544 Br(1) S(1) 3.535(5) ? . 2_565 Br(1) N(3) 3.578(15) ? . 1_544 Br(1) C(9) 3.495(14) ? . 1_544 Br(1) C(15) 3.52(2) ? . 1_554 Br(3) Cu(1) 2.482(4) ? . 1_566 Br(3) N(2) 3.468(13) ? . 1_566 Br(3) C(2) 3.46(2) ? . 1_556 Br(3) C(7) 3.59(2) ? . 2_566 Br(3) C(8) 3.511(18) ? . 1_566 Cu(1) Br(3) 2.482(4) ? . 1_544 Cu(1) Cu(2) 2.841(3) ? . 1_544 Cu(1) Cl(3) 2.482(4) ? . 1_544 Cu(2) Br(1) 2.520(4) ? . 1_566 Cu(2) Cu(1) 2.841(3) ? . 1_566 Cu(2) Cl(1) 2.520(4) ? . 1_566 Cl(1) Cu(2) 2.520(4) ? . 1_544 Cl(1) S(1) 3.535(5) ? . 2_565 Cl(1) N(3) 3.578(15) ? . 1_544 Cl(1) C(9) 3.495(14) ? . 1_544 Cl(1) C(15) 3.52(2) ? . 1_554 Cl(3) Cu(1) 2.482(4) ? . 1_566 Cl(3) N(2) 3.469(13) ? . 1_566 Cl(3) C(2) 3.46(2) ? . 1_556 Cl(3) C(7) 3.59(2) ? . 2_566 Cl(3) C(8) 3.511(18) ? . 1_566 S(1) Br(1) 3.535(5) ? . 2_565 S(1) Cl(1) 3.535(5) ? . 2_565 S(1) S(4) 3.497(9) ? . 2_565 S(1) S(7) 3.521(8) ? . . S(2) S(3) 3.525(8) ? . 2_565 S(2) S(5) 3.512(6) ? . 1_554 S(2) S(8) 3.518(7) ? . . S(2) S(8) 3.386(9) ? . 2_665 S(2) N(4) 3.338(15) ? . 2_665 S(2) C(5) 3.503(19) ? . 2_565 S(3) S(2) 3.525(8) ? . 2_565 S(3) S(3) 3.429(7) ? . 2_566 S(3) S(5) 3.474(8) ? . . S(3) S(5) 3.390(9) ? . 2_566 S(3) N(1) 3.351(13) ? . 2_566 S(4) S(1) 3.497(9) ? . 2_565 S(4) S(6) 3.486(8) ? . . S(5) S(2) 3.512(6) ? . 1_556 S(5) S(3) 3.474(8) ? . . S(5) S(3) 3.390(9) ? . 2_566 S(5) N(1) 3.484(13) ? . 2_566 S(6) S(4) 3.486(8) ? . . S(6) S(7) 3.586(8) ? . 2_666 S(7) S(1) 3.521(8) ? . . S(7) S(6) 3.586(8) ? . 2_666 S(8) S(2) 3.518(7) ? . . S(8) S(2) 3.386(9) ? . 2_665 S(8) S(8) 3.382(7) ? . 2_665 S(8) N(4) 3.246(15) ? . 2_665 N(1) S(3) 3.351(13) ? . 2_566 N(1) S(5) 3.484(13) ? . 2_566 N(1) C(2) 3.59(2) ? . 2_565 N(2) Br(3) 3.468(13) ? . 1_544 N(2) Cl(3) 3.469(13) ? . 1_544 N(2) C(1) 3.41(2) ? . 2_565 N(3) Br(1) 3.578(15) ? . 1_566 N(3) Cl(1) 3.578(15) ? . 1_566 N(3) C(16) 3.39(2) ? . 2_666 N(4) S(2) 3.338(15) ? . 2_665 N(4) S(8) 3.246(16) ? . 2_665 N(4) C(15) 3.50(2) ? . 2_666 C(1) N(2) 3.41(2) ? . 2_565 C(1) C(6) 3.39(2) ? . 2_565 C(2) Br(3) 3.46(2) ? . 1_554 C(2) Cl(3) 3.46(2) ? . 1_554 C(2) N(1) 3.59(2) ? . 2_565 C(2) C(5) 3.45(2) ? . 2_565 C(2) C(6) 3.56(2) ? . 2_565 C(2) C(12) 3.57(2) ? . . C(3) C(4) 3.52(3) ? . 2_565 C(3) C(13) 3.48(2) ? . . C(4) C(3) 3.52(3) ? . 2_565 C(4) C(4) 3.47(2) ? . 2_565 C(4) C(14) 3.43(3) ? . . C(5) S(2) 3.503(19) ? . 2_565 C(5) C(2) 3.45(2) ? . 2_565 C(6) C(1) 3.39(2) ? . 2_565 C(6) C(2) 3.56(2) ? . 2_565 C(6) C(16) 3.57(3) ? . . C(7) Br(3) 3.59(2) ? . 2_566 C(7) Cl(3) 3.59(2) ? . 2_566 C(8) Br(3) 3.511(18) ? . 1_544 C(8) Cl(3) 3.511(18) ? . 1_544 C(9) Br(1) 3.495(14) ? . 1_566 C(9) Cl(1) 3.495(14) ? . 1_566 C(11) C(16) 3.53(3) ? . 2_666 C(12) C(2) 3.57(2) ? . . C(12) C(15) 3.50(3) ? . 2_666 C(13) C(3) 3.48(2) ? . . C(13) C(13) 3.56(2) ? . 2_666 C(14) C(4) 3.43(3) ? . . C(15) Br(1) 3.52(2) ? . 1_556 C(15) Cl(1) 3.52(2) ? . 1_556 C(15) N(4) 3.50(2) ? . 2_666 C(15) C(12) 3.50(3) ? . 2_666 C(16) N(3) 3.39(2) ? . 2_666 C(16) C(6) 3.57(3) ? . . C(16) C(11) 3.53(3) ? . 2_666 Br(1) H(5) 2.884 ? . 1_544 Br(1) H(6) 3.366 ? . 2_665 Br(1) H(7) 2.674 ? . 1_554 Br(2) H(6) 2.862 ? . 1_545 Br(2) H(6) 2.862 ? . 2_665 Br(2) H(8) 3.050 ? . . Br(2) H(8) 3.050 ? . 2_655 Br(3) H(1) 3.488 ? . 1_556 Br(3) H(2) 2.607 ? . 1_556 Br(3) H(3) 3.227 ? . 2_566 Br(3) H(4) 2.877 ? . 1_566 Br(4) H(1) 3.163 ? . . Br(4) H(1) 3.163 ? . 2_576 Br(4) H(3) 2.732 ? . 1_565 Br(4) H(3) 2.732 ? . 2_566 Cu(1) H(6) 3.497 ? . 2_665 Cu(2) H(3) 3.389 ? . 2_566 Cl(1) H(5) 2.884 ? . 1_544 Cl(1) H(6) 3.365 ? . 2_665 Cl(1) H(7) 2.674 ? . 1_554 Cl(2) H(6) 2.862 ? . 1_545 Cl(2) H(6) 2.862 ? . 2_665 Cl(2) H(8) 3.050 ? . . Cl(2) H(8) 3.050 ? . 2_655 Cl(3) H(1) 3.488 ? . 1_556 Cl(3) H(2) 2.607 ? . 1_556 Cl(3) H(3) 3.227 ? . 2_566 Cl(3) H(4) 2.877 ? . 1_566 Cl(4) H(1) 3.163 ? . . Cl(4) H(1) 3.163 ? . 2_576 Cl(4) H(3) 2.732 ? . 1_565 Cl(4) H(3) 2.732 ? . 2_566 S(1) H(3) 3.318 ? . 2_566 S(3) H(7) 3.488 ? . 2_566 S(4) H(6) 3.291 ? . 2_665 S(6) H(6) 3.145 ? . 2_665 S(7) H(3) 3.435 ? . 2_566 N(1) H(2) 3.438 ? . 2_565 N(1) H(7) 3.578 ? . . N(2) H(1) 3.304 ? . 2_565 N(2) H(8) 3.538 ? . . N(3) H(8) 3.376 ? . 2_666 N(4) H(7) 3.394 ? . 2_666 C(7) H(2) 3.443 ? . 2_565 C(8) H(1) 3.376 ? . 2_565 C(8) H(2) 3.600 ? . 2_565 C(8) H(5) 3.407 ? . 1_545 C(9) H(4) 3.426 ? . 1_565 C(10) H(7) 3.407 ? . 2_666 H(1) Br(3) 3.488 ? . 1_554 H(1) Br(4) 3.163 ? . . H(1) Cl(3) 3.488 ? . 1_554 H(1) Cl(4) 3.163 ? . . H(1) N(2) 3.304 ? . 2_565 H(1) C(8) 3.376 ? . 2_565 H(1) H(4) 3.180 ? . 1_565 H(1) H(4) 3.541 ? . 2_565 H(2) Br(3) 2.607 ? . 1_554 H(2) Cl(3) 2.607 ? . 1_554 H(2) N(1) 3.438 ? . 2_565 H(2) C(7) 3.443 ? . 2_565 H(2) C(8) 3.600 ? . 2_565 H(3) Br(3) 3.227 ? . 2_566 H(3) Br(4) 2.732 ? . 1_545 H(3) Cu(2) 3.389 ? . 2_566 H(3) Cl(3) 3.227 ? . 2_566 H(3) Cl(4) 2.732 ? . 1_545 H(3) S(1) 3.318 ? . 2_566 H(3) S(7) 3.435 ? . 2_566 H(4) Br(3) 2.877 ? . 1_544 H(4) Cl(3) 2.877 ? . 1_544 H(4) C(9) 3.426 ? . 1_545 H(4) H(1) 3.180 ? . 1_545 H(4) H(1) 3.541 ? . 2_565 H(4) H(5) 2.973 ? . 1_545 H(5) Br(1) 2.884 ? . 1_566 H(5) Cl(1) 2.884 ? . 1_566 H(5) C(8) 3.407 ? . 1_565 H(5) H(4) 2.973 ? . 1_565 H(5) H(8) 3.159 ? . 1_565 H(6) Br(1) 3.366 ? . 2_665 H(6) Br(2) 2.862 ? . 1_565 H(6) Cu(1) 3.497 ? . 2_665 H(6) Cl(1) 3.365 ? . 2_665 H(6) Cl(2) 2.862 ? . 1_565 H(6) S(4) 3.291 ? . 2_665 H(6) S(6) 3.145 ? . 2_665 H(7) Br(1) 2.674 ? . 1_556 H(7) Cl(1) 2.674 ? . 1_556 H(7) S(3) 3.488 ? . 2_566 H(7) N(1) 3.578 ? . . H(7) N(4) 3.394 ? . 2_666 H(7) C(10) 3.407 ? . 2_666 H(8) Br(2) 3.050 ? . . H(8) Cl(2) 3.050 ? . . H(8) N(2) 3.538 ? . . H(8) N(3) 3.376 ? . 2_666 H(8) H(5) 3.159 ? . 1_545 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment '- CIF_CCDC 751039_090630_Pyra-TTFCuCl0.2Br1.3_160K.cif' #============================================================================== data___090630_160K _database_code_depnum_ccdc_archive 'CCDC 751039' #TrackingRef '- CIF_CCDC 751039_090630_Pyra-TTFCuCl0.2Br1.3_160K.cif' _audit_creation_date 2009-09-04 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C8 H4 Br1.30 Cl0.20 Cu N2 S4 ' _chemical_formula_moiety 'C8 H4 Br1.30 Cl0.20 Cu N2 S4 ' _chemical_formula_weight 430.88 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _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_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 7.4234(17) _cell_length_b 11.953(3) _cell_length_c 7.0000(16) _cell_angle_alpha 90.147(7) _cell_angle_beta 105.932(5) _cell_angle_gamma 85.179(6) _cell_volume 595.0(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 1993 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 160.0 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 2.405 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 415.80 _exptl_absorpt_coefficient_mu 6.930 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.190 _exptl_absorpt_correction_T_max 0.250 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 4547 _diffrn_reflns_av_R_equivalents 0.018 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.953 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_ambient_temperature 160.0 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2594 _reflns_number_gt 3913 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.0548 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 3921 _refine_ls_number_parameters 162 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0010Fo^2^ + 3.0000\s(Fo^2^) + 0.5000]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.69 _refine_diff_density_min -2.70 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Br Br -0.290 2.459 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Br(1) Br 0.26579(18) 0.10463(8) 0.43967(17) 0.0248(2) Uani 0.89 1 d P . . Br(2) Br 0.5000 0.0000 1.0000 0.0366(2) Uani 0.82 2 d SP . . Cu(1) Cu 0.55881(7) 0.05368(4) 0.68701(8) 0.02585(15) Uani 1.00 1 d . . . Cl(1) Cl 0.264(5) 0.088(2) 0.471(4) 0.0380 Uiso 0.11 1 d P . . Cl(2) Cl 0.5000 0.0000 1.0000 0.0380 Uiso 0.18 2 d SP . . S(1) S 0.48833(15) 0.70294(8) 0.77531(15) 0.0232(2) Uani 1.00 1 d . . . S(2) S 0.18453(13) 0.55304(9) 0.68358(15) 0.0219(2) Uani 1.00 1 d . . . S(3) S 0.79368(13) 0.49314(8) 0.81592(15) 0.0192(2) Uani 1.00 1 d . . . S(4) S 0.48793(13) 0.33803(8) 0.72085(15) 0.0176(2) Uani 1.00 1 d . . . N(1) N 1.0430(4) 0.3146(2) 0.8542(4) 0.0223(9) Uani 1.00 1 d . . . N(2) N 0.7560(4) 0.1665(2) 0.7597(4) 0.0186(8) Uani 1.00 1 d . . . C(1) C 0.2595(6) 0.7649(3) 0.7162(5) 0.0268(11) Uani 1.00 1 d . . . C(2) C 0.1233(6) 0.6960(3) 0.6749(6) 0.0275(11) Uani 1.00 1 d . . . C(3) C 0.4249(5) 0.5655(3) 0.7443(5) 0.0152(9) Uani 1.00 1 d . . . C(4) C 0.5538(5) 0.4755(3) 0.7593(5) 0.0157(9) Uani 1.00 1 d . . . C(5) C 0.8629(5) 0.3498(3) 0.8122(5) 0.0155(9) Uani 1.00 1 d . . . C(6) C 0.7193(5) 0.2774(3) 0.7670(5) 0.0157(9) Uani 1.00 1 d . . . C(7) C 1.0819(5) 0.2029(3) 0.8512(6) 0.0240(11) Uani 1.00 1 d . . . C(8) C 0.9414(5) 0.1304(3) 0.8037(5) 0.0226(11) Uani 1.00 1 d . . . H(1) H 0.2334 0.8441 0.7143 0.031 Uiso 1.00 1 c R . . H(2) H -0.0051 0.7247 0.6399 0.033 Uiso 1.00 1 c R . . H(3) H 1.2094 0.1728 0.8833 0.028 Uiso 1.00 1 c R . . H(4) H 0.9758 0.0522 0.8014 0.027 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br(1) 0.0202(2) 0.0207(4) 0.0326(5) 0.0048(2) 0.0076(3) -0.0051(2) Br(2) 0.0422(5) 0.0419(5) 0.0311(5) 0.0164(3) 0.0251(4) 0.0125(3) Cu(1) 0.0194(2) 0.0245(3) 0.0367(3) -0.0040(2) 0.0123(2) -0.0034(2) S(1) 0.0241(5) 0.0189(5) 0.0284(6) -0.0029(4) 0.0097(4) -0.0012(4) S(2) 0.0126(4) 0.0267(5) 0.0280(6) 0.0004(3) 0.0087(4) 0.0005(4) S(3) 0.0126(4) 0.0172(4) 0.0300(5) -0.0031(3) 0.0089(4) -0.0049(4) S(4) 0.0117(4) 0.0178(4) 0.0254(5) -0.0028(3) 0.0085(4) -0.0022(4) N(1) 0.0144(16) 0.0228(18) 0.0303(19) -0.0020(13) 0.0070(15) -0.0052(15) N(2) 0.0190(17) 0.0163(16) 0.0221(18) -0.0010(13) 0.0083(14) -0.0007(14) C(1) 0.033(2) 0.024(2) 0.022(2) 0.0113(18) 0.0085(19) 0.0028(18) C(2) 0.024(2) 0.030(2) 0.027(2) 0.0124(18) 0.0086(19) 0.0038(19) C(3) 0.0150(18) 0.0173(18) 0.015(2) -0.0021(14) 0.0060(15) -0.0009(15) C(4) 0.0141(18) 0.0195(19) 0.015(2) -0.0038(14) 0.0056(15) -0.0013(15) C(5) 0.0150(18) 0.0161(18) 0.016(2) -0.0005(14) 0.0066(15) -0.0034(15) C(6) 0.0130(18) 0.023(2) 0.014(2) 0.0016(14) 0.0083(15) 0.0005(15) C(7) 0.0131(19) 0.026(2) 0.032(2) 0.0029(16) 0.0051(18) -0.0072(19) C(8) 0.019(2) 0.019(2) 0.030(2) 0.0032(16) 0.0078(18) -0.0037(18) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR2002 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Br(1) Cu(1) 2.4115(11) yes . . Br(1) Cu(1) 2.5047(12) yes . 2_656 Br(1) Cl(1) 0.29(3) yes . . Br(2) Cu(1) 2.4458(5) yes . . Br(2) Cu(1) 2.4458(5) yes . 2_657 Cu(1) Cl(1) 2.30(3) yes . . Cu(1) Cl(1) 2.50(3) yes . 2_656 Cu(1) Cl(2) 2.4458(5) yes . . Cu(1) N(2) 2.034(3) yes . . S(1) C(1) 1.735(4) yes . . S(1) C(3) 1.743(3) yes . . S(2) C(2) 1.728(4) yes . . S(2) C(3) 1.737(3) yes . . S(3) C(4) 1.746(3) yes . . S(3) C(5) 1.750(3) yes . . S(4) C(4) 1.753(3) yes . . S(4) C(6) 1.751(3) yes . . N(1) C(5) 1.319(4) yes . . N(1) C(7) 1.344(5) yes . . N(2) C(6) 1.335(4) yes . . N(2) C(8) 1.357(4) yes . . C(1) C(2) 1.327(6) yes . . C(3) C(4) 1.362(5) yes . . C(5) C(6) 1.397(5) yes . . C(7) C(8) 1.381(5) yes . . C(1) H(1) 0.950 no . . C(2) H(2) 0.950 no . . C(7) H(3) 0.950 no . . C(8) H(4) 0.950 no . . 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cu(1) Br(1) Cu(1) 71.12(3) yes . . 2_656 Cu(1) Br(1) Cl(1) 64(6) yes . . . Cu(1) Br(1) Cl(1) 85(6) yes 2_656 . . Cu(1) Br(2) Cu(1) 0(440) yes . . 2_657 Br(1) Cu(1) Br(1) 108.88(4) yes . . 2_656 Br(1) Cu(1) Br(2) 110.29(4) yes . . . Br(1) Cu(1) Cl(1) 6.6(9) yes . . . Br(1) Cu(1) Cl(1) 105.8(6) yes . . 2_656 Br(1) Cu(1) Cl(2) 110.29(4) yes . . . Br(1) Cu(1) N(2) 119.43(8) yes . . . Br(1) Cu(1) Br(2) 110.83(3) yes 2_656 . . Br(1) Cu(1) Cl(1) 109.2(8) yes 2_656 . . Br(1) Cu(1) Cl(1) 6.7(7) yes 2_656 . 2_656 Br(1) Cu(1) Cl(2) 110.83(3) yes 2_656 . . Br(1) Cu(1) N(2) 101.34(10) yes 2_656 . . Br(2) Cu(1) Cl(1) 104.4(9) yes . . . Br(2) Cu(1) Cl(1) 117.5(7) yes . . 2_656 Br(2) Cu(1) Cl(2) 0.0000 yes . . . Br(2) Cu(1) N(2) 105.67(9) yes . . . Cl(1) Cu(1) Cl(1) 106.9(11) yes . . 2_656 Cl(1) Cu(1) Cl(2) 104.4(9) yes . . . Cl(1) Cu(1) N(2) 125.1(8) yes . . . Cl(1) Cu(1) Cl(2) 117.5(7) yes 2_656 . . Cl(1) Cu(1) N(2) 98.2(8) yes 2_656 . . Cl(2) Cu(1) N(2) 105.67(9) yes . . . Br(1) Cl(1) Cu(1) 110(7) yes . . . Br(1) Cl(1) Cu(1) 88(7) yes . . 2_656 Cu(1) Cl(1) Cu(1) 73.1(9) yes . . 2_656 Cu(1) Cl(2) Cu(1) 0(440) yes . . 2_657 C(1) S(1) C(3) 95.28(19) yes . . . C(2) S(2) C(3) 94.80(19) yes . . . C(4) S(3) C(5) 94.80(17) yes . . . C(4) S(4) C(6) 94.24(17) yes . . . C(5) N(1) C(7) 115.6(3) yes . . . Cu(1) N(2) C(6) 125.2(2) yes . . . Cu(1) N(2) C(8) 119.9(2) yes . . . C(6) N(2) C(8) 114.9(3) yes . . . S(1) C(1) C(2) 116.6(3) yes . . . S(2) C(2) C(1) 118.5(3) yes . . . S(1) C(3) S(2) 114.7(2) yes . . . S(1) C(3) C(4) 122.5(2) yes . . . S(2) C(3) C(4) 122.8(2) yes . . . S(3) C(4) S(4) 117.0(2) yes . . . S(3) C(4) C(3) 120.9(2) yes . . . S(4) C(4) C(3) 122.1(2) yes . . . S(3) C(5) N(1) 120.1(2) yes . . . S(3) C(5) C(6) 116.6(2) yes . . . N(1) C(5) C(6) 123.3(3) yes . . . S(4) C(6) N(2) 121.0(2) yes . . . S(4) C(6) C(5) 117.3(2) yes . . . N(2) C(6) C(5) 121.7(3) yes . . . N(1) C(7) C(8) 121.8(3) yes . . . N(2) C(8) C(7) 122.7(3) yes . . . S(1) C(1) H(1) 121.6 no . . . C(2) C(1) H(1) 121.8 no . . . S(2) C(2) H(2) 120.7 no . . . C(1) C(2) H(2) 120.8 no . . . N(1) C(7) H(3) 119.2 no . . . C(8) C(7) H(3) 119.0 no . . . N(2) C(8) H(4) 118.6 no . . . C(7) C(8) H(4) 118.7 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Cu(1) Br(1) Cu(1) Cl(1) -7.0(9) ? . . 2_656 2_656 Cu(1) Br(1) Cu(1) N(2) 126.74(9) ? . . 2_656 2_656 Cu(1) Br(1) Cu(1) Cl(1) 64(6) ? . . 2_656 . Cu(1) Br(1) Cu(1) Br(2) -121.81(3) ? 2_656 . . . Cu(1) Br(1) Cu(1) Cl(1) -94(7) ? 2_656 . . . Cu(1) Br(1) Cu(1) Cl(2) -121.81(3) ? 2_656 . . . Cu(1) Br(1) Cu(1) N(2) 115.56(11) ? 2_656 . . . Cu(1) Br(1) Cu(1) Cl(1) 6.3(8) ? 2_656 . . 2_656 Cu(1) Br(1) Cl(1) Cu(1) -71(3) ? . . . 2_656 Cl(1) Br(1) Cu(1) Br(1) 94(7) ? . . . 2_656 Cl(1) Br(1) Cu(1) Br(2) -28(7) ? . . . . Cl(1) Br(1) Cu(1) Cl(2) -28(7) ? . . . . Cl(1) Br(1) Cu(1) N(2) -150(7) ? . . . . Cl(1) Br(1) Cu(1) Cl(1) 100(7) ? . . . 2_656 Cu(1) Br(1) Cl(1) Cu(1) 71(3) ? 2_656 . . . Cl(1) Br(1) Cu(1) Br(1) -64(6) ? . . 2_656 2_656 Cl(1) Br(1) Cu(1) Cl(1) -71(6) ? . . 2_656 2_656 Cl(1) Br(1) Cu(1) N(2) 63(6) ? . . 2_656 2_656 Br(1) Cu(1) Cl(1) Cu(1) 81(7) ? . . . 2_656 Br(1) Cu(1) Cl(1) Br(1) -118(6) ? . . 2_656 2_656 Br(1) Cu(1) Cl(1) Cu(1) -6.8(9) ? . . 2_656 2_656 Br(1) Cu(1) N(2) C(6) 35.2(3) ? . . . . Br(1) Cu(1) N(2) C(8) -144.1(2) ? . . . . Br(1) Cu(1) Cl(1) Br(1) -88(7) ? 2_656 . . . Br(1) Cu(1) Cl(1) Cu(1) -6.7(9) ? 2_656 . . 2_656 Br(1) Cu(1) Cl(1) Cu(1) 111(6) ? 2_656 . 2_656 2_656 Br(1) Cu(1) N(2) C(6) 154.7(3) ? 2_656 . . . Br(1) Cu(1) N(2) C(8) -24.7(3) ? 2_656 . . . Br(2) Cu(1) Cl(1) Br(1) 153(7) ? . . . . Br(2) Cu(1) Cl(1) Cu(1) -125.2(5) ? . . . 2_656 Br(2) Cu(1) Cl(1) Br(1) 6(6) ? . . 2_656 2_656 Br(2) Cu(1) Cl(1) Cu(1) 116.9(5) ? . . 2_656 2_656 Br(2) Cu(1) N(2) C(6) -89.6(3) ? . . . . Br(2) Cu(1) N(2) C(8) 91.0(3) ? . . . . Cl(1) Cu(1) Cl(1) Br(1) -111(6) ? . . 2_656 2_656 Cl(1) Cu(1) Cl(1) Br(1) -81(7) ? 2_656 . . . Cl(2) Cu(1) Cl(1) Br(1) 153(7) ? . . . . Cl(2) Cu(1) Cl(1) Cu(1) -125.2(5) ? . . . 2_656 Cl(1) Cu(1) N(2) C(6) 31.2(12) ? . . . . Cl(1) Cu(1) N(2) C(8) -148.1(12) ? . . . . N(2) Cu(1) Cl(1) Br(1) 32(7) ? . . . . N(2) Cu(1) Cl(1) Cu(1) 113.3(5) ? . . . 2_656 Cl(2) Cu(1) Cl(1) Br(1) 6(6) ? . . 2_656 2_656 Cl(2) Cu(1) Cl(1) Cu(1) 116.9(5) ? . . 2_656 2_656 Cl(1) Cu(1) N(2) C(6) 148.6(7) ? 2_656 . . . Cl(1) Cu(1) N(2) C(8) -30.7(7) ? 2_656 . . . N(2) Cu(1) Cl(1) Br(1) 118(6) ? . . 2_656 2_656 N(2) Cu(1) Cl(1) Cu(1) -130.6(6) ? . . 2_656 2_656 Cl(2) Cu(1) N(2) C(6) -89.6(3) ? . . . . Cl(2) Cu(1) N(2) C(8) 91.0(3) ? . . . . C(1) S(1) C(3) S(2) -2.2(2) ? . . . . C(1) S(1) C(3) C(4) 175.5(3) ? . . . . C(3) S(1) C(1) C(2) 1.4(3) ? . . . . C(2) S(2) C(3) S(1) 2.2(2) ? . . . . C(2) S(2) C(3) C(4) -175.5(3) ? . . . . C(3) S(2) C(2) C(1) -1.4(3) ? . . . . C(4) S(3) C(5) N(1) -177.9(3) ? . . . . C(4) S(3) C(5) C(6) 1.0(3) ? . . . . C(5) S(3) C(4) S(4) -1.3(2) ? . . . . C(5) S(3) C(4) C(3) 179.3(3) ? . . . . C(4) S(4) C(6) N(2) 179.3(3) ? . . . . C(4) S(4) C(6) C(5) -0.4(3) ? . . . . C(6) S(4) C(4) S(3) 1.1(2) ? . . . . C(6) S(4) C(4) C(3) -179.5(3) ? . . . . C(5) N(1) C(7) C(8) 1.1(5) ? . . . . C(7) N(1) C(5) S(3) 178.7(3) ? . . . . C(7) N(1) C(5) C(6) -0.1(4) ? . . . . Cu(1) N(2) C(6) S(4) 2.3(4) ? . . . . Cu(1) N(2) C(6) C(5) -177.9(2) ? . . . . Cu(1) N(2) C(8) C(7) 179.0(3) ? . . . . C(6) N(2) C(8) C(7) -0.4(5) ? . . . . C(8) N(2) C(6) S(4) -178.3(2) ? . . . . C(8) N(2) C(6) C(5) 1.4(5) ? . . . . S(1) C(1) C(2) S(2) -0.0(5) ? . . . . S(1) C(3) C(4) S(3) 1.2(4) ? . . . . S(1) C(3) C(4) S(4) -178.1(2) ? . . . . S(2) C(3) C(4) S(3) 178.7(2) ? . . . . S(2) C(3) C(4) S(4) -0.6(4) ? . . . . S(3) C(5) C(6) S(4) -0.4(4) ? . . . . S(3) C(5) C(6) N(2) 179.9(2) ? . . . . N(1) C(5) C(6) S(4) 178.5(3) ? . . . . N(1) C(5) C(6) N(2) -1.3(6) ? . . . . N(1) C(7) C(8) N(2) -0.8(6) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Br(1) C(2) 3.499(4) ? . 2_566 Cl(1) C(7) 3.53(3) ? . 1_455 S(1) S(4) 3.5562(15) ? . 2_666 S(1) S(4) 3.5161(15) ? . 2_667 S(2) S(2) 3.5243(12) ? . 2_566 S(2) S(3) 3.4084(15) ? . 1_455 S(2) S(3) 3.5836(15) ? . 2_666 S(2) S(3) 3.5056(15) ? . 2_667 S(2) N(1) 3.444(3) ? . 1_455 S(2) C(5) 3.578(3) ? . 2_666 S(3) S(2) 3.4084(15) ? . 1_655 S(3) S(2) 3.5836(15) ? . 2_666 S(3) S(2) 3.5056(15) ? . 2_667 S(3) S(3) 3.4351(12) ? . 2_767 S(3) N(1) 3.314(3) ? . 2_767 S(4) S(1) 3.5562(15) ? . 2_666 S(4) S(1) 3.5161(15) ? . 2_667 N(1) S(2) 3.444(3) ? . 1_655 N(1) S(3) 3.314(3) ? . 2_767 N(1) C(2) 3.574(5) ? . 2_666 N(2) C(1) 3.401(5) ? . 2_666 C(1) N(2) 3.401(5) ? . 2_666 C(1) C(6) 3.462(5) ? . 2_666 C(2) Br(1) 3.499(4) ? . 2_566 C(2) N(1) 3.574(5) ? . 2_666 C(2) C(5) 3.480(5) ? . 2_666 C(3) C(4) 3.469(5) ? . 2_667 C(4) C(3) 3.469(5) ? . 2_667 C(4) C(4) 3.536(5) ? . 2_666 C(5) S(2) 3.578(3) ? . 2_666 C(5) C(2) 3.480(5) ? . 2_666 C(6) C(1) 3.462(5) ? . 2_666 C(7) Cl(1) 3.53(3) ? . 1_655 Br(1) H(1) 3.563 ? . 2_566 Br(1) H(2) 2.640 ? . 2_566 Br(1) H(3) 3.336 ? . 1_455 Br(2) H(1) 3.133 ? . 1_545 Br(2) H(1) 3.133 ? . 2_667 Br(2) H(3) 2.807 ? . 1_455 Br(2) H(3) 2.807 ? . 2_757 Cu(1) H(3) 3.460 ? . 1_455 Cl(1) H(1) 3.441 ? . 1_545 Cl(1) H(1) 3.586 ? . 2_566 Cl(1) H(2) 2.786 ? . 2_566 Cl(1) H(3) 3.176 ? . 1_455 Cl(2) H(1) 3.133 ? . 1_545 Cl(2) H(1) 3.133 ? . 2_667 Cl(2) H(3) 2.807 ? . 1_455 Cl(2) H(3) 2.807 ? . 2_757 S(1) H(3) 3.248 ? . 2_767 S(4) H(3) 3.385 ? . 1_455 N(1) H(2) 3.427 ? . 2_666 N(2) H(1) 3.342 ? . 2_666 C(7) H(2) 3.427 ? . 2_666 C(8) H(1) 3.504 ? . 2_666 C(8) H(4) 3.414 ? . 2_757 H(1) Br(1) 3.563 ? . 2_566 H(1) Br(2) 3.133 ? . 1_565 H(1) Cl(1) 3.441 ? . 1_565 H(1) Cl(1) 3.586 ? . 2_566 H(1) Cl(2) 3.133 ? . 1_565 H(1) N(2) 3.342 ? . 2_666 H(1) C(8) 3.504 ? . 2_666 H(1) H(4) 3.169 ? . 1_465 H(2) Br(1) 2.640 ? . 2_566 H(2) Cl(1) 2.786 ? . 2_566 H(2) N(1) 3.427 ? . 2_666 H(2) C(7) 3.427 ? . 2_666 H(3) Br(1) 3.336 ? . 1_655 H(3) Br(2) 2.807 ? . 1_655 H(3) Cu(1) 3.460 ? . 1_655 H(3) Cl(1) 3.176 ? . 1_655 H(3) Cl(2) 2.807 ? . 1_655 H(3) S(1) 3.248 ? . 2_767 H(3) S(4) 3.385 ? . 1_655 H(4) C(8) 3.414 ? . 2_757 H(4) H(1) 3.169 ? . 1_645 H(4) H(4) 2.968 ? . 2_757 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment '- CIF_CCDC 770776_(Pyra-TTF)CuBr2.cif' #============================================================================== data___pyraTTF-TBA2CuBr4_01 _database_code_depnum_ccdc_archive 'CCDC 770776' #TrackingRef '- CIF_CCDC 770776_(Pyra-TTF)CuBr2.cif' _audit_creation_date 2008-11-18 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C8 H4 Br2 Cu N2 S4 ' _chemical_formula_moiety 'C8 H4 Br2 Cu N2 S4 ' _chemical_formula_weight 479.73 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 8.776(17) _cell_length_b 13.20(2) _cell_length_c 10.786(19) _cell_angle_alpha 90.0000 _cell_angle_beta 93.665(18) _cell_angle_gamma 90.0000 _cell_volume 1247(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 2310 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 293.3 #------------------------------------------------------------------------------ _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 2.556 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 916.00 _exptl_absorpt_coefficient_mu 8.824 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.089 _exptl_absorpt_correction_T_max 0.171 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 9191 _diffrn_reflns_av_R_equivalents 0.062 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.977 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 10 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2788 _reflns_number_gt 1251 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1692 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 1266 _refine_ls_number_parameters 158 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0036Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.83 _refine_diff_density_min -1.08 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Br Br -0.290 2.459 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 B(R1) Br 0.2073(2) 0.11261(15) 0.29860(13) 0.0492(5) Uani 1.00 1 d . . . B(R2) Br 0.62627(19) 0.12359(14) 0.49109(13) 0.0416(5) Uani 1.00 1 d . . . C(U1) Cu 0.3632(2) 0.0667(2) 0.47819(17) 0.0516(7) Uani 1.00 1 d . . . S(1) S 0.4878(4) 0.1024(3) 0.7841(3) 0.0382(11) Uani 1.00 1 d . . . S(2) S 0.2923(4) 0.1396(3) 0.9895(3) 0.0395(12) Uani 1.00 1 d . . . S(3) S 0.7752(4) 0.1087(3) 0.9643(3) 0.0409(12) Uani 1.00 1 d . . . S(4) S 0.5946(4) 0.1401(3) 1.1771(3) 0.0388(12) Uani 1.00 1 d . . . N(1) N 0.2362(13) 0.1075(9) 0.6294(9) 0.033(3) Uani 1.00 1 d . . . N(2) N 0.0504(13) 0.1303(10) 0.8283(10) 0.037(3) Uani 1.00 1 d . . . C(1) C 0.0865(18) 0.1124(12) 0.6123(12) 0.040(4) Uani 1.00 1 d . . . C(2) C 0.0000(16) 0.1255(11) 0.7110(13) 0.034(4) Uani 1.00 1 d . . . C(3) C 0.2947(18) 0.1152(12) 0.7450(11) 0.037(4) Uani 1.00 1 d . . . C(4) C 0.2015(14) 0.1293(10) 0.8422(11) 0.022(3) Uani 1.00 1 d . . . C(5) C 0.4676(14) 0.1209(11) 0.9396(11) 0.027(3) Uani 1.00 1 d . . . C(6) C 0.6010(17) 0.1215(12) 1.0197(11) 0.035(4) Uani 1.00 1 d . . . C(7) C 0.8719(16) 0.1238(12) 1.1054(12) 0.033(4) Uani 1.00 1 d . . . C(8) C 0.7878(18) 0.1417(13) 1.2014(11) 0.042(4) Uani 1.00 1 d . . . H(1) H 0.0390 0.1067 0.5310 0.047 Uiso 1.00 1 c R . . H(2) H -0.1071 0.1318 0.6937 0.040 Uiso 1.00 1 c R . . H(3) H 0.9801 0.1197 1.1150 0.039 Uiso 1.00 1 c R . . H(4) H 0.8346 0.1550 1.2816 0.049 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 B(R1) 0.0565(12) 0.0664(14) 0.0237(7) 0.0023(10) -0.0057(7) 0.0038(8) B(R2) 0.0478(11) 0.0454(12) 0.0314(7) 0.0000(8) 0.0024(6) 0.0006(7) C(U1) 0.0546(14) 0.0701(18) 0.0297(9) 0.0014(12) -0.0013(9) 0.0011(10) S(1) 0.035(2) 0.063(3) 0.0171(14) 0.001(2) 0.0036(14) -0.0015(17) S(2) 0.042(2) 0.058(3) 0.0195(15) 0.007(2) 0.0051(15) -0.0032(16) S(3) 0.034(2) 0.063(3) 0.0259(16) 0.005(2) 0.0003(15) -0.0023(18) S(4) 0.044(2) 0.052(3) 0.0208(16) 0.000(2) -0.0008(15) -0.0013(17) N(1) 0.039(8) 0.036(8) 0.023(5) -0.015(6) 0.001(5) 0.007(5) N(2) 0.028(7) 0.050(9) 0.033(6) 0.002(6) -0.001(5) -0.002(6) C(1) 0.045(10) 0.042(11) 0.030(7) 0.007(8) -0.013(6) -0.013(7) C(2) 0.027(8) 0.028(9) 0.047(8) 0.002(7) -0.000(6) 0.003(7) C(3) 0.062(11) 0.031(10) 0.016(5) -0.011(8) -0.011(6) 0.003(6) C(4) 0.020(7) 0.020(8) 0.026(6) -0.009(6) 0.004(5) 0.001(5) C(5) 0.018(7) 0.045(10) 0.017(5) -0.008(7) 0.006(5) -0.006(6) C(6) 0.039(9) 0.048(11) 0.020(6) 0.022(8) 0.009(6) 0.004(6) C(7) 0.017(7) 0.041(10) 0.040(7) -0.007(7) 0.000(5) -0.001(7) C(8) 0.051(10) 0.055(12) 0.018(6) -0.006(8) -0.009(6) -0.001(6) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 B(R1) C(U1) 2.377(2) yes . . B(R2) C(U1) 2.423(2) yes . . B(R2) C(U1) 2.534(3) yes . 3_656 C(U1) N(1) 2.103(11) yes . . S(1) C(3) 1.728(16) yes . . S(1) C(5) 1.715(12) yes . . S(2) C(4) 1.737(12) yes . . S(2) C(5) 1.681(13) yes . . S(3) C(6) 1.685(15) yes . . S(3) C(7) 1.706(14) yes . . S(4) C(6) 1.721(13) yes . . S(4) C(8) 1.699(16) yes . . N(1) C(1) 1.32(2) yes . . N(1) C(3) 1.322(15) yes . . N(2) C(2) 1.314(18) yes . . N(2) C(4) 1.325(17) yes . . C(1) C(2) 1.36(2) yes . . C(3) C(4) 1.383(19) yes . . C(5) C(6) 1.410(18) yes . . C(7) C(8) 1.33(2) yes . . C(1) H(1) 0.950 no . . C(2) H(2) 0.950 no . . C(7) H(3) 0.950 no . . C(8) H(4) 0.950 no . . 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C(U1) B(R2) C(U1) 74.18(9) yes . . 3_656 B(R1) C(U1) B(R2) 117.67(10) yes . . . B(R1) C(U1) B(R2) 111.91(10) yes . . 3_656 B(R1) C(U1) N(1) 105.1(3) yes . . . B(R2) C(U1) B(R2) 105.82(10) yes . . 3_656 B(R2) C(U1) N(1) 115.2(3) yes . . . B(R2) C(U1) N(1) 99.7(3) yes 3_656 . . C(3) S(1) C(5) 93.6(6) yes . . . C(4) S(2) C(5) 94.1(6) yes . . . C(6) S(3) C(7) 94.8(6) yes . . . C(6) S(4) C(8) 93.3(6) yes . . . C(U1) N(1) C(1) 118.5(8) yes . . . C(U1) N(1) C(3) 123.9(10) yes . . . C(1) N(1) C(3) 116.9(12) yes . . . C(2) N(2) C(4) 112.4(11) yes . . . N(1) C(1) C(2) 120.0(12) yes . . . N(2) C(2) C(1) 126.1(13) yes . . . S(1) C(3) N(1) 122.5(11) yes . . . S(1) C(3) C(4) 116.6(9) yes . . . N(1) C(3) C(4) 120.8(13) yes . . . S(2) C(4) N(2) 120.0(9) yes . . . S(2) C(4) C(3) 116.4(10) yes . . . N(2) C(4) C(3) 123.5(11) yes . . . S(1) C(5) S(2) 119.2(7) yes . . . S(1) C(5) C(6) 117.8(10) yes . . . S(2) C(5) C(6) 122.9(9) yes . . . S(3) C(6) S(4) 116.9(8) yes . . . S(3) C(6) C(5) 121.3(9) yes . . . S(4) C(6) C(5) 121.8(11) yes . . . S(3) C(7) C(8) 116.5(11) yes . . . S(4) C(8) C(7) 118.4(10) yes . . . N(1) C(1) H(1) 120.0 no . . . C(2) C(1) H(1) 120.0 no . . . N(2) C(2) H(2) 116.9 no . . . C(1) C(2) H(2) 116.9 no . . . S(3) C(7) H(3) 121.8 no . . . C(8) C(7) H(3) 121.8 no . . . S(4) C(8) H(4) 120.8 no . . . C(7) C(8) H(4) 120.8 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C(U1) B(R2) C(U1) B(R1) -129.37(10) ? . . 3_656 3_656 C(U1) B(R2) C(U1) N(1) 119.9(3) ? . . 3_656 3_656 C(U1) B(R2) C(U1) B(R1) -125.92(12) ? 3_656 . . . C(U1) B(R2) C(U1) N(1) 109.1(3) ? 3_656 . . . B(R1) C(U1) N(1) C(1) 25.1(12) ? . . . . B(R1) C(U1) N(1) C(3) -164.6(11) ? . . . . B(R2) C(U1) N(1) C(1) 156.4(10) ? . . . . B(R2) C(U1) N(1) C(3) -33.3(13) ? . . . . B(R2) C(U1) N(1) C(1) -90.9(11) ? 3_656 . . . B(R2) C(U1) N(1) C(3) 79.4(12) ? 3_656 . . . C(3) S(1) C(5) S(2) 1.1(11) ? . . . . C(3) S(1) C(5) C(6) -177.7(13) ? . . . . C(5) S(1) C(3) N(1) -179.7(11) ? . . . . C(5) S(1) C(3) C(4) -2.7(13) ? . . . . C(4) S(2) C(5) S(1) 0.4(4) ? . . . . C(4) S(2) C(5) C(6) 179.2(10) ? . . . . C(5) S(2) C(4) N(2) 174.4(12) ? . . . . C(5) S(2) C(4) C(3) -2.3(13) ? . . . . C(6) S(3) C(7) C(8) -1.7(15) ? . . . . C(7) S(3) C(6) S(4) -1.0(11) ? . . . . C(7) S(3) C(6) C(5) 176.7(14) ? . . . . C(6) S(4) C(8) C(7) -3.9(15) ? . . . . C(8) S(4) C(6) S(3) 2.6(11) ? . . . . C(8) S(4) C(6) C(5) -175.1(14) ? . . . . C(U1) N(1) C(1) C(2) 171.5(11) ? . . . . C(U1) N(1) C(3) S(1) 5.4(19) ? . . . . C(U1) N(1) C(3) C(4) -171.5(10) ? . . . . C(1) N(1) C(3) S(1) 175.8(12) ? . . . . C(1) N(1) C(3) C(4) -1.0(17) ? . . . . C(3) N(1) C(1) C(2) 0.5(15) ? . . . . C(2) N(2) C(4) S(2) 177.8(11) ? . . . . C(2) N(2) C(4) C(3) -6(2) ? . . . . C(4) N(2) C(2) C(1) 5(2) ? . . . . N(1) C(1) C(2) N(2) -3(2) ? . . . . S(1) C(3) C(4) S(2) 3.6(16) ? . . . . S(1) C(3) C(4) N(2) -173.0(12) ? . . . . N(1) C(3) C(4) S(2) -179.4(8) ? . . . . N(1) C(3) C(4) N(2) 4(2) ? . . . . S(1) C(5) C(6) S(3) 2.1(19) ? . . . . S(1) C(5) C(6) S(4) 179.7(3) ? . . . . S(2) C(5) C(6) S(3) -176.7(9) ? . . . . S(2) C(5) C(6) S(4) 0.9(15) ? . . . . S(3) C(7) C(8) S(4) 3.9(19) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 B(R1) S(2) 3.481(3) ? . 1_554 B(R1) S(4) 3.737(4) ? . 1_554 B(R1) N(2) 3.684(13) ? . 4_554 B(R1) C(2) 3.629(15) ? . 3_556 B(R1) C(3) 3.726(16) ? . 4_554 B(R1) C(4) 3.438(14) ? . 4_554 B(R1) C(7) 3.499(13) ? . 1_454 B(R1) C(8) 3.783(15) ? . 1_454 B(R2) S(3) 3.784(5) ? . 4_554 B(R2) S(4) 3.387(3) ? . 1_554 B(R2) S(4) 3.729(4) ? . 4_554 B(R2) C(5) 3.677(15) ? . 4_554 B(R2) C(6) 3.386(16) ? . 4_554 B(R2) C(8) 3.521(13) ? . 1_554 S(1) S(4) 3.312(6) ? . 3_657 S(1) S(4) 3.728(6) ? . 4_554 S(1) C(6) 3.746(15) ? . 3_657 S(2) B(R1) 3.481(3) ? . 1_556 S(2) S(3) 3.372(6) ? . 3_657 S(2) N(1) 3.709(13) ? . 4_555 S(2) C(6) 3.573(17) ? . 3_657 S(3) B(R2) 3.784(5) ? . 4_555 S(3) S(2) 3.372(6) ? . 3_657 S(3) N(2) 2.919(12) ? . 1_655 S(3) C(2) 3.478(15) ? . 1_655 S(3) C(4) 3.770(14) ? . 3_657 S(4) B(R1) 3.737(4) ? . 1_556 S(4) B(R2) 3.387(3) ? . 1_556 S(4) B(R2) 3.729(4) ? . 4_555 S(4) S(1) 3.312(6) ? . 3_657 S(4) S(1) 3.728(6) ? . 4_555 S(4) C(3) 3.591(16) ? . 3_657 S(4) C(5) 3.695(15) ? . 3_657 N(1) S(2) 3.709(13) ? . 4_554 N(1) C(8) 3.77(2) ? . 3_657 N(2) B(R1) 3.684(13) ? . 4_555 N(2) S(3) 2.919(12) ? . 1_455 N(2) C(7) 3.464(18) ? . 1_455 N(2) C(7) 3.49(2) ? . 3_657 C(2) B(R1) 3.629(15) ? . 3_556 C(2) S(3) 3.478(15) ? . 1_455 C(2) C(7) 3.65(2) ? . 4_454 C(2) C(8) 3.59(2) ? . 4_454 C(3) B(R1) 3.726(16) ? . 4_555 C(3) S(4) 3.591(16) ? . 3_657 C(3) C(8) 3.52(2) ? . 3_657 C(4) B(R1) 3.438(14) ? . 4_555 C(4) S(3) 3.770(14) ? . 3_657 C(4) C(7) 3.46(2) ? . 3_657 C(4) C(8) 3.61(2) ? . 3_657 C(5) B(R2) 3.677(15) ? . 4_555 C(5) S(4) 3.695(15) ? . 3_657 C(5) C(5) 3.48(2) ? . 3_657 C(5) C(6) 3.29(2) ? . 3_657 C(6) B(R2) 3.386(16) ? . 4_555 C(6) S(1) 3.746(15) ? . 3_657 C(6) S(2) 3.573(17) ? . 3_657 C(6) C(5) 3.29(2) ? . 3_657 C(6) C(6) 3.68(2) ? . 3_657 C(7) B(R1) 3.499(13) ? . 1_656 C(7) N(2) 3.464(18) ? . 1_655 C(7) N(2) 3.49(2) ? . 3_657 C(7) C(2) 3.65(2) ? . 4_655 C(7) C(4) 3.46(2) ? . 3_657 C(8) B(R1) 3.783(15) ? . 1_656 C(8) B(R2) 3.521(13) ? . 1_556 C(8) N(1) 3.77(2) ? . 3_657 C(8) C(2) 3.59(2) ? . 4_655 C(8) C(3) 3.52(2) ? . 3_657 C(8) C(4) 3.61(2) ? . 3_657 B(R1) H(2) 3.345 ? . 3_556 B(R1) H(3) 2.721 ? . 1_454 B(R1) H(4) 3.312 ? . 1_454 B(R2) H(1) 3.627 ? . 1_655 B(R2) H(2) 3.100 ? . 1_655 B(R2) H(4) 3.025 ? . 1_554 S(1) H(2) 3.766 ? . 1_655 S(2) H(3) 3.143 ? . 1_455 S(3) H(2) 3.172 ? . 1_655 S(3) H(4) 3.743 ? . 4_554 N(1) H(4) 3.658 ? . 3_657 N(2) H(3) 3.195 ? . 1_455 N(2) H(3) 3.369 ? . 3_657 N(2) H(4) 3.428 ? . 4_454 C(1) H(1) 3.427 ? . 3_556 C(1) H(3) 3.657 ? . 4_454 C(1) H(4) 3.760 ? . 3_657 C(2) H(3) 3.739 ? . 3_657 C(2) H(3) 3.520 ? . 4_454 C(2) H(4) 3.350 ? . 4_454 C(3) H(4) 3.747 ? . 3_657 C(4) H(3) 3.630 ? . 1_455 C(4) H(3) 3.695 ? . 3_657 C(7) H(2) 3.365 ? . 4_655 C(8) H(2) 3.132 ? . 4_655 H(1) B(R2) 3.627 ? . 1_455 H(1) C(1) 3.427 ? . 3_556 H(1) H(1) 2.965 ? . 3_556 H(1) H(3) 3.765 ? . 4_454 H(1) H(4) 3.201 ? . 1_454 H(2) B(R1) 3.345 ? . 3_556 H(2) B(R2) 3.100 ? . 1_455 H(2) S(1) 3.766 ? . 1_455 H(2) S(3) 3.172 ? . 1_455 H(2) C(7) 3.365 ? . 4_454 H(2) C(8) 3.132 ? . 4_454 H(2) H(3) 3.485 ? . 4_454 H(2) H(4) 3.023 ? . 4_454 H(3) B(R1) 2.721 ? . 1_656 H(3) S(2) 3.143 ? . 1_655 H(3) N(2) 3.195 ? . 1_655 H(3) N(2) 3.369 ? . 3_657 H(3) C(1) 3.657 ? . 4_655 H(3) C(2) 3.739 ? . 3_657 H(3) C(2) 3.520 ? . 4_655 H(3) C(4) 3.630 ? . 1_655 H(3) C(4) 3.695 ? . 3_657 H(3) H(1) 3.765 ? . 4_655 H(3) H(2) 3.485 ? . 4_655 H(4) B(R1) 3.312 ? . 1_656 H(4) B(R2) 3.025 ? . 1_556 H(4) S(3) 3.743 ? . 4_555 H(4) N(1) 3.658 ? . 3_657 H(4) N(2) 3.428 ? . 4_655 H(4) C(1) 3.760 ? . 3_657 H(4) C(2) 3.350 ? . 4_655 H(4) C(3) 3.747 ? . 3_657 H(4) H(1) 3.201 ? . 1_656 H(4) H(2) 3.023 ? . 4_655 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================