Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Shinobu Itoh' _publ_contact_author_address ; Department of Chemistry Osaka City University Graduate School of Science 3-3-138 Sugimoto Sumiyoshi-ku Osaka 558-8585 JAPAN ; _publ_contact_author_email SHINOBU@SCI.OSAKA-CU.AC.JP _publ_section_title ; Structure and photoluminescence property of two-dimensional coordination polymer complexes involving CuI6X6 (X = Cl, Br, I) hexagon prism cluster supported by a tripodal tripyridine ligand with 1,3,5-triethylbenzene spacer ; loop_ _publ_author_name 'Shinobu Itoh' 'Takashi Kunimoto' 'Hiromi Ohi' 'Yoshimitsu Tachi' data__[Cu6Cl6L2]n _database_code_depnum_ccdc_archive 'CCDC 275920' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C33 H39 Cl3 Cu3 N3 ' _chemical_formula_moiety 'C33 H39 Cl3 Cu3 N3 ' _chemical_formula_weight 774.69 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' _symmetry_Int_Tables_number 148 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -Y,+X-Y,+Z 3 -X+Y,-X,+Z 4 -X,-Y,-Z 5 +Y,-X+Y,-Z 6 +X-Y,+X,-Z 7 2/3+X,1/3+Y,1/3+Z 8 2/3-Y,1/3+X-Y,1/3+Z 9 2/3-X+Y,1/3-X,1/3+Z 10 2/3-X,1/3-Y,1/3-Z 11 2/3+Y,1/3-X+Y,1/3-Z 12 2/3+X-Y,1/3+X,1/3-Z 13 1/3+X,2/3+Y,2/3+Z 14 1/3-Y,2/3+X-Y,2/3+Z 15 1/3-X+Y,2/3-X,2/3+Z 16 1/3-X,2/3-Y,2/3-Z 17 1/3+Y,2/3-X+Y,2/3-Z 18 1/3+X-Y,2/3+X,2/3-Z #------------------------------------------------------------------------------ _cell_length_a 15.029(4) _cell_length_b 15.029(4) _cell_length_c 23.744(8) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 120.0000 _cell_volume 4645(2) _cell_formula_units_Z 6 _cell_measurement_reflns_used 16304 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 163.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376.00 _exptl_absorpt_coefficient_mu 2.330 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.493 _exptl_absorpt_correction_T_max 0.830 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 14463 _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 1.056 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.056 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using all reflections. 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 2378 _reflns_number_gt 1948 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0272 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 2378 _refine_ls_number_parameters 140 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0001Fo^2^ + 1.0000\s(Fo^2^)]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.65 _refine_diff_density_min -0.50 _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) ; 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) ; #============================================================================== # 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 Cu(1) Cu 1.15215(2) 0.58826(2) 0.130320(10) 0.02626(8) Uani 1.00 1 d . . . Cl(1) Cl 1.26175(4) 0.76596(4) 0.10234(2) 0.02100(13) Uani 1.00 1 d . . . N(1) N 1.01263(12) 0.54044(12) 0.09621(6) 0.0173(4) Uani 1.00 1 d . . . C(1) C 0.77163(14) 0.36330(14) 0.21108(8) 0.0155(5) Uani 1.00 1 d . . . C(2) C 0.69641(14) 0.25862(14) 0.21098(9) 0.0162(5) Uani 1.00 1 d . . . C(3) C 0.72860(16) 0.17739(16) 0.21580(9) 0.0195(5) Uani 1.00 1 d . . . C(4) C 0.73251(18) 0.14852(18) 0.27661(9) 0.0286(6) Uani 1.00 1 d . . . C(5) C 0.88474(14) 0.39454(16) 0.21260(9) 0.0192(5) Uani 1.00 1 d . . . C(6) C 0.93182(16) 0.38742(16) 0.15626(9) 0.0200(5) Uani 1.00 1 d . . . C(7) C 0.92759(16) 0.45133(14) 0.10897(9) 0.0183(5) Uani 1.00 1 d . . . C(8) C 0.83788(17) 0.41690(17) 0.07796(9) 0.0247(6) Uani 1.00 1 d . . . C(9) C 0.83525(17) 0.47269(18) 0.03293(9) 0.0269(6) Uani 1.00 1 d . . . C(10) C 0.92242(17) 0.56454(17) 0.02018(10) 0.0247(6) Uani 1.00 1 d . . . C(11) C 1.00823(16) 0.59605(17) 0.05287(9) 0.0214(5) Uani 1.00 1 d . . . H(31) H 0.6808 0.1176 0.1959 0.023 Uiso 1.00 1 c R . . H(32) H 0.7949 0.2039 0.1996 0.023 Uiso 1.00 1 c R . . H(43) H 0.7991 0.1925 0.2915 0.037 Uiso 1.00 1 c R . . H(42) H 0.7174 0.0792 0.2788 0.037 Uiso 1.00 1 c R . . H(41) H 0.6832 0.1564 0.2977 0.037 Uiso 1.00 1 c R . . H(51) H 0.9222 0.4640 0.2247 0.023 Uiso 1.00 1 c R . . H(52) H 0.8928 0.3520 0.2393 0.023 Uiso 1.00 1 c R . . H(61) H 1.0019 0.4076 0.1624 0.024 Uiso 1.00 1 c R . . H(62) H 0.8953 0.3176 0.1446 0.024 Uiso 1.00 1 c R . . H(8) H 0.7784 0.3541 0.0879 0.027 Uiso 1.00 1 c R . . H(9) H 0.7746 0.4485 0.0110 0.031 Uiso 1.00 1 c R . . H(10) H 0.9228 0.6051 -0.0106 0.030 Uiso 1.00 1 c R . . H(11) H 1.0677 0.6601 0.0446 0.025 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) 0.02009(16) 0.02733(17) 0.02980(17) 0.01069(12) -0.00265(12) 0.00201(13) Cl(1) 0.0183(2) 0.0205(2) 0.0194(2) 0.0062(2) 0.0005(2) 0.0023(2) N(1) 0.0170(9) 0.0187(9) 0.0168(9) 0.0093(7) 0.0001(7) -0.0010(7) C(1) 0.0159(10) 0.0190(10) 0.0115(10) 0.0087(8) 0.0009(8) 0.0013(8) C(2) 0.0194(11) 0.0184(10) 0.0126(10) 0.0108(9) 0.0030(8) 0.0015(8) C(3) 0.0160(11) 0.0166(10) 0.0254(12) 0.0079(9) 0.0038(9) 0.0040(9) C(4) 0.0317(13) 0.0272(12) 0.0307(13) 0.0176(11) 0.0011(10) 0.0067(10) C(5) 0.0174(10) 0.0191(11) 0.0214(12) 0.0093(9) -0.0014(9) 0.0029(9) C(6) 0.0156(10) 0.0191(11) 0.0261(12) 0.0092(9) 0.0047(9) 0.0039(9) C(7) 0.0178(10) 0.0198(11) 0.0189(11) 0.0107(9) 0.0046(9) 0.0005(9) C(8) 0.0166(11) 0.0255(12) 0.0258(12) 0.0058(9) 0.0024(9) 0.0018(10) C(9) 0.0196(11) 0.0364(14) 0.0214(13) 0.0116(10) -0.0043(9) 0.0002(10) C(10) 0.0260(12) 0.0295(12) 0.0203(12) 0.0152(10) -0.0001(10) 0.0038(10) C(11) 0.0225(11) 0.0189(11) 0.0223(12) 0.0099(9) 0.0028(9) 0.0009(9) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.7.0' _computing_molecular_graphics ORTEP3 #============================================================================== # 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 Cu(1) Cl(1) 2.4265(5) ? . . Cu(1) Cl(1) 2.3660(8) ? . 75502 Cu(1) Cl(1) 2.3943(5) ? . 54512 Cu(1) N(1) 2.0155(18) ? . . N(1) C(7) 1.344(2) ? . . N(1) C(11) 1.348(3) ? . . C(1) C(2) 1.405(2) ? . . C(1) C(2) 1.403(3) ? . 65502 C(1) C(5) 1.521(3) ? . . C(2) C(3) 1.526(3) ? . . C(3) C(4) 1.517(3) ? . . C(5) C(6) 1.542(3) ? . . C(6) C(7) 1.500(3) ? . . C(7) C(8) 1.389(3) ? . . C(8) C(9) 1.371(3) ? . . C(9) C(10) 1.380(2) ? . . C(10) C(11) 1.371(3) ? . . C(3) H(31) 0.950 ? . . C(3) H(32) 0.950 ? . . C(4) H(43) 0.950 ? . . C(4) H(42) 0.950 ? . . C(4) H(41) 0.950 ? . . C(5) H(51) 0.950 ? . . C(5) H(52) 0.950 ? . . C(6) H(61) 0.950 ? . . C(6) H(62) 0.950 ? . . C(8) H(8) 0.950 ? . . C(9) H(9) 0.950 ? . . C(10) H(10) 0.950 ? . . C(11) H(11) 0.950 ? . . 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 Cl(1) Cu(1) Cl(1) 107.66(2) ? . . 75502 Cl(1) Cu(1) Cl(1) 103.440(18) ? . . 54512 Cl(1) Cu(1) N(1) 107.16(5) ? . . . Cl(1) Cu(1) Cl(1) 105.31(2) ? 75502 . 54512 Cl(1) Cu(1) N(1) 115.58(6) ? 75502 . . Cl(1) Cu(1) N(1) 116.74(5) ? 54512 . . Cu(1) Cl(1) Cu(1) 117.48(2) ? . . 77503 Cu(1) Cl(1) Cu(1) 74.799(15) ? . . 56511 Cu(1) Cl(1) Cu(1) 75.918(16) ? 77503 . 56511 Cu(1) N(1) C(7) 124.47(16) ? . . . Cu(1) N(1) C(11) 116.77(11) ? . . . C(7) N(1) C(11) 118.22(18) ? . . . C(2) C(1) C(2) 119.5(2) ? . . 65502 C(2) C(1) C(5) 119.7(2) ? . . . C(2) C(1) C(5) 120.78(16) ? 65502 . . C(1) C(2) C(1) 120.5(2) ? . . 66503 C(1) C(2) C(3) 119.8(2) ? . . . C(1) C(2) C(3) 119.59(16) ? 66503 . . C(2) C(3) C(4) 111.9(2) ? . . . C(1) C(5) C(6) 116.03(17) ? . . . C(5) C(6) C(7) 115.9(2) ? . . . N(1) C(7) C(6) 118.90(19) ? . . . N(1) C(7) C(8) 120.9(2) ? . . . C(6) C(7) C(8) 120.16(16) ? . . . C(7) C(8) C(9) 120.31(17) ? . . . C(8) C(9) C(10) 118.6(2) ? . . . C(9) C(10) C(11) 118.7(2) ? . . . N(1) C(11) C(10) 123.19(17) ? . . . C(2) C(3) H(31) 109.1 ? . . . C(2) C(3) H(32) 108.6 ? . . . C(4) C(3) H(31) 108.9 ? . . . C(4) C(3) H(32) 108.9 ? . . . H(31) C(3) H(32) 109.5 ? . . . C(3) C(4) H(43) 109.5 ? . . . C(3) C(4) H(42) 110.2 ? . . . C(3) C(4) H(41) 108.8 ? . . . H(43) C(4) H(42) 109.5 ? . . . H(43) C(4) H(41) 109.5 ? . . . H(42) C(4) H(41) 109.5 ? . . . C(1) C(5) H(51) 107.7 ? . . . C(1) C(5) H(52) 107.9 ? . . . C(6) C(5) H(51) 107.4 ? . . . C(6) C(5) H(52) 108.3 ? . . . H(51) C(5) H(52) 109.5 ? . . . C(5) C(6) H(61) 108.5 ? . . . C(5) C(6) H(62) 107.3 ? . . . C(7) C(6) H(61) 107.8 ? . . . C(7) C(6) H(62) 107.6 ? . . . H(61) C(6) H(62) 109.5 ? . . . C(7) C(8) H(8) 119.6 ? . . . C(9) C(8) H(8) 120.1 ? . . . C(8) C(9) H(9) 120.6 ? . . . C(10) C(9) H(9) 120.7 ? . . . C(9) C(10) H(10) 120.6 ? . . . C(11) C(10) H(10) 120.7 ? . . . N(1) C(11) H(11) 118.2 ? . . . C(10) C(11) H(11) 118.6 ? . . . 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 Cl(1) Cu(1) Cl(1) Cu(1) 51.39(2) ? . . 75502 75502 Cl(1) Cu(1) Cl(1) Cu(1) -51.89(2) ? 75502 . . 77503 Cl(1) Cu(1) Cl(1) Cu(1) -116.71(2) ? 75502 . . 56511 Cl(1) Cu(1) Cl(1) Cu(1) 5.59(2) ? . . 54512 56511 Cl(1) Cu(1) Cl(1) Cu(1) -118.55(2) ? . . 54512 54512 Cl(1) Cu(1) Cl(1) Cu(1) 59.27(3) ? 54512 . . 77503 Cl(1) Cu(1) Cl(1) Cu(1) -5.55(2) ? 54512 . . 56511 Cl(1) Cu(1) N(1) C(7) -169.79(18) ? . . . . Cl(1) Cu(1) N(1) C(11) 18.78(19) ? . . . . N(1) Cu(1) Cl(1) Cu(1) -176.82(6) ? . . . 77503 N(1) Cu(1) Cl(1) Cu(1) 118.37(6) ? . . . 56511 Cl(1) Cu(1) Cl(1) Cu(1) 118.469(19) ? 75502 . 54512 56511 Cl(1) Cu(1) Cl(1) Cu(1) -5.665(16) ? 75502 . 54512 54512 Cl(1) Cu(1) Cl(1) Cu(1) -58.49(2) ? 54512 . 75502 75502 Cl(1) Cu(1) N(1) C(7) 70.22(19) ? 75502 . . . Cl(1) Cu(1) N(1) C(11) -101.21(18) ? 75502 . . . N(1) Cu(1) Cl(1) Cu(1) 171.11(5) ? . . 75502 75502 Cl(1) Cu(1) N(1) C(7) -54.4(2) ? 54512 . . . Cl(1) Cu(1) N(1) C(11) 134.12(16) ? 54512 . . . N(1) Cu(1) Cl(1) Cu(1) -111.81(6) ? . . 54512 56511 N(1) Cu(1) Cl(1) Cu(1) 124.06(6) ? . . 54512 54512 Cu(1) N(1) C(7) C(6) 7.4(3) ? . . . . Cu(1) N(1) C(7) C(8) -170.64(19) ? . . . . Cu(1) N(1) C(11) C(10) 169.8(2) ? . . . . C(7) N(1) C(11) C(10) -2.2(3) ? . . . . C(11) N(1) C(7) C(6) 178.7(2) ? . . . . C(11) N(1) C(7) C(8) 0.7(3) ? . . . . C(2) C(1) C(2) C(1) 0.3(3) ? . . 65502 65502 C(2) C(1) C(2) C(3) 175.16(18) ? . . 65502 65502 C(2) C(1) C(2) C(1) -0.3(3) ? 65502 . . 66503 C(2) C(1) C(2) C(3) -175.15(18) ? 65502 . . . C(2) C(1) C(5) C(6) 78.5(2) ? . . . . C(5) C(1) C(2) C(1) 178.32(18) ? . . . 66503 C(5) C(1) C(2) C(3) 3.5(2) ? . . . . C(2) C(1) C(5) C(6) -102.9(2) ? 65502 . . . C(5) C(1) C(2) C(1) -178.31(18) ? . . 65502 65502 C(5) C(1) C(2) C(3) -3.5(2) ? . . 65502 65502 C(1) C(2) C(3) C(4) 90.6(2) ? . . . . C(1) C(2) C(3) C(4) -84.2(2) ? 66503 . . . C(1) C(5) C(6) C(7) 59.4(2) ? . . . . C(5) C(6) C(7) N(1) 101.4(2) ? . . . . C(5) C(6) C(7) C(8) -80.6(2) ? . . . . N(1) C(7) C(8) C(9) 1.2(4) ? . . . . C(6) C(7) C(8) C(9) -176.8(2) ? . . . . C(7) C(8) C(9) C(10) -1.7(4) ? . . . . C(8) C(9) C(10) C(11) 0.3(4) ? . . . . C(9) C(10) C(11) N(1) 1.7(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 Cl(1) C(9) 3.481(2) ? . 65506 Cl(1) C(10) 3.561(2) ? . 65506 N(1) C(10) 3.552(3) ? . 76504 C(9) Cl(1) 3.481(2) ? . 56505 C(10) Cl(1) 3.561(2) ? . 56505 C(10) N(1) 3.552(3) ? . 76504 C(10) C(11) 3.526(4) ? . 76504 C(11) C(10) 3.526(4) ? . 76504 Cl(1) H(9) 2.840 ? . 65506 Cl(1) H(10) 3.005 ? . 65506 N(1) H(10) 3.462 ? . 76504 C(3) H(32) 3.240 ? . 65510 C(3) H(61) 3.568 ? . 65510 C(3) H(62) 2.880 ? . 65510 C(4) H(43) 3.572 ? . 55517 C(4) H(41) 3.441 ? . 54518 C(4) H(62) 3.138 ? . 65510 C(4) H(10) 3.000 ? . 44507 C(4) H(11) 3.360 ? . 44507 C(6) H(31) 3.101 ? . 65510 C(6) H(32) 3.555 ? . 65510 C(6) H(42) 3.232 ? . 65510 C(7) H(42) 3.396 ? . 65510 C(9) H(11) 3.523 ? . 76504 C(10) H(42) 3.006 ? . 55413 C(11) H(42) 3.246 ? . 55413 H(31) C(6) 3.101 ? . 65510 H(31) H(32) 3.152 ? . 65510 H(31) H(61) 2.833 ? . 65510 H(31) H(62) 2.512 ? . 65510 H(32) C(3) 3.240 ? . 65510 H(32) C(6) 3.555 ? . 65510 H(32) H(31) 3.152 ? . 65510 H(32) H(32) 2.515 ? . 65510 H(32) H(62) 2.682 ? . 65510 H(43) C(4) 3.572 ? . 54518 H(43) H(42) 3.574 ? . 54518 H(43) H(41) 2.765 ? . 54518 H(43) H(51) 3.581 ? . 55517 H(43) H(52) 3.553 ? . 55517 H(43) H(62) 3.476 ? . 65510 H(43) H(11) 3.348 ? . 44507 H(42) C(6) 3.232 ? . 65510 H(42) C(7) 3.396 ? . 65510 H(42) C(10) 3.006 ? . 44507 H(42) C(11) 3.246 ? . 44507 H(42) H(43) 3.574 ? . 55517 H(42) H(61) 3.270 ? . 65510 H(42) H(62) 2.631 ? . 65510 H(42) H(10) 2.278 ? . 44507 H(42) H(11) 2.756 ? . 44507 H(41) C(4) 3.441 ? . 55517 H(41) H(43) 2.765 ? . 55517 H(41) H(41) 3.264 ? . 55517 H(41) H(41) 3.264 ? . 54518 H(41) H(52) 3.115 ? . 55517 H(41) H(10) 2.906 ? . 44507 H(41) H(11) 3.479 ? . 44507 H(51) H(43) 3.581 ? . 54518 H(51) H(10) 3.437 ? . 65508 H(52) H(43) 3.553 ? . 54518 H(52) H(41) 3.115 ? . 54518 H(61) C(3) 3.568 ? . 65510 H(61) H(31) 2.833 ? . 65510 H(61) H(42) 3.270 ? . 65510 H(62) C(3) 2.880 ? . 65510 H(62) C(4) 3.138 ? . 65510 H(62) H(31) 2.512 ? . 65510 H(62) H(32) 2.682 ? . 65510 H(62) H(43) 3.476 ? . 65510 H(62) H(42) 2.631 ? . 65510 H(9) Cl(1) 2.840 ? . 56505 H(10) Cl(1) 3.005 ? . 56505 H(10) N(1) 3.462 ? . 76504 H(10) C(4) 3.000 ? . 55413 H(10) H(42) 2.278 ? . 55413 H(10) H(41) 2.906 ? . 55413 H(10) H(51) 3.437 ? . 66415 H(11) C(4) 3.360 ? . 55413 H(11) C(9) 3.523 ? . 76504 H(11) H(43) 3.348 ? . 55413 H(11) H(42) 2.756 ? . 55413 H(11) H(41) 3.479 ? . 55413 Cu(1) Cu(1) 2.9281(4) ? . 54512 Cu(1) Cu(1) 4.0969(4) ? . 75502 Cu(1) Cu(1) 5.0357(3) ? . 76510 Cu(1) Cu(1) 4.0969(3) ? . 77503 Cu(1) Cu(1) 2.9281(3) ? . 56511 Cu(1) Cl(1) 2.3943(5) ? . 54512 Cu(1) Cl(1) 2.3660(8) ? . 75502 #============================================================================== # 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 #============================================================================== #===END #============================================================================== data__[Cu6Br6L2]n _database_code_depnum_ccdc_archive 'CCDC 275921' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C33 H39 Br3 Cu3 N3 ' _chemical_formula_moiety 'C33 H39 Br3 Cu3 N3 ' _chemical_formula_weight 908.04 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' _symmetry_Int_Tables_number 148 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -Y,+X-Y,+Z 3 -X+Y,-X,+Z 4 -X,-Y,-Z 5 +Y,-X+Y,-Z 6 +X-Y,+X,-Z 7 2/3+X,1/3+Y,1/3+Z 8 2/3-Y,1/3+X-Y,1/3+Z 9 2/3-X+Y,1/3-X,1/3+Z 10 2/3-X,1/3-Y,1/3-Z 11 2/3+Y,1/3-X+Y,1/3-Z 12 2/3+X-Y,1/3+X,1/3-Z 13 1/3+X,2/3+Y,2/3+Z 14 1/3-Y,2/3+X-Y,2/3+Z 15 1/3-X+Y,2/3-X,2/3+Z 16 1/3-X,2/3-Y,2/3-Z 17 1/3+Y,2/3-X+Y,2/3-Z 18 1/3+X-Y,2/3+X,2/3-Z #------------------------------------------------------------------------------ _cell_length_a 15.1677(9) _cell_length_b 15.1677(9) _cell_length_c 24.4621(18) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 120.0000 _cell_volume 4873.8(5) _cell_formula_units_Z 6 _cell_measurement_reflns_used 13675 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 163.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.856 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2700.00 _exptl_absorpt_coefficient_mu 5.675 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.257 _exptl_absorpt_correction_T_max 0.567 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 15918 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 1.064 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.064 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using all reflections. 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 2485 _reflns_number_gt 2121 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0264 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 2485 _refine_ls_number_parameters 140 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0001Fo^2^ + 1.0000\s(Fo^2^) + 0.2000]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.80 _refine_diff_density_min -0.64 _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) ; Cu Cu 0.320 1.265 ; 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 1.26100(2) 0.76966(2) 0.098620(10) 0.02013(7) Uani 1.00 1 d . . . Cu(1) Cu 1.14783(3) 0.58812(3) 0.133840(10) 0.02454(9) Uani 1.00 1 d . . . N(1) N 1.00853(16) 0.53646(16) 0.09930(9) 0.0175(5) Uani 1.00 1 d . . . C(1) C 0.77010(18) 0.36094(19) 0.21030(10) 0.0148(6) Uani 1.00 1 d . . . C(2) C 0.69400(19) 0.25735(19) 0.21027(10) 0.0159(6) Uani 1.00 1 d . . . C(3) C 0.7236(2) 0.1754(2) 0.21507(11) 0.0197(7) Uani 1.00 1 d . . . C(4) C 0.7258(2) 0.1453(2) 0.27459(12) 0.0302(8) Uani 1.00 1 d . . . C(5) C 0.88222(19) 0.3899(2) 0.21193(11) 0.0184(6) Uani 1.00 1 d . . . C(6) C 0.9287(2) 0.3828(2) 0.15683(11) 0.0210(7) Uani 1.00 1 d . . . C(7) C 0.92461(19) 0.44625(19) 0.11076(11) 0.0184(6) Uani 1.00 1 d . . . C(8) C 0.8370(2) 0.4111(2) 0.07988(12) 0.0283(7) Uani 1.00 1 d . . . C(9) C 0.8339(2) 0.4669(2) 0.03613(12) 0.0317(8) Uani 1.00 1 d . . . C(10) C 0.9190(2) 0.5594(2) 0.02462(12) 0.0265(7) Uani 1.00 1 d . . . C(11) C 1.0037(2) 0.5908(2) 0.05700(11) 0.0223(7) Uani 1.00 1 d . . . H(31) H 0.6753 0.1167 0.1957 0.024 Uiso 1.00 1 c R . . H(32) H 0.7892 0.2000 0.1995 0.024 Uiso 1.00 1 c R . . H(41) H 0.7921 0.1875 0.2891 0.040 Uiso 1.00 1 c R . . H(42) H 0.7090 0.0761 0.2766 0.040 Uiso 1.00 1 c R . . H(43) H 0.6779 0.1546 0.2951 0.040 Uiso 1.00 1 c R . . H(51) H 0.9201 0.4585 0.2241 0.022 Uiso 1.00 1 c R . . H(52) H 0.8889 0.3467 0.2377 0.021 Uiso 1.00 1 c R . . H(61) H 0.9982 0.4030 0.1629 0.025 Uiso 1.00 1 c R . . H(62) H 0.8928 0.3136 0.1455 0.025 Uiso 1.00 1 c R . . H(8) H 0.7790 0.3476 0.0889 0.029 Uiso 1.00 1 c R . . H(9) H 0.7743 0.4424 0.0144 0.035 Uiso 1.00 1 c R . . H(10) H 0.9195 0.6002 -0.0050 0.031 Uiso 1.00 1 c R . . H(11) H 1.0621 0.6549 0.0494 0.025 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) 0.01765(13) 0.02004(14) 0.01920(13) 0.00680(12) 0.00052(11) 0.00225(12) Cu(1) 0.01929(19) 0.0269(2) 0.0261(2) 0.01056(16) -0.00211(14) 0.00190(16) N(1) 0.0191(11) 0.0175(11) 0.0181(11) 0.0109(9) 0.0004(9) 0.0008(9) C(1) 0.0137(12) 0.0167(12) 0.0134(12) 0.0073(10) 0.0002(10) 0.0012(10) C(2) 0.0186(13) 0.0170(12) 0.0139(12) 0.0102(11) 0.0017(10) 0.0009(10) C(3) 0.0179(13) 0.0166(13) 0.0262(15) 0.0098(11) 0.0043(11) 0.0045(11) C(4) 0.0352(17) 0.0294(16) 0.0334(17) 0.0217(14) 0.0032(14) 0.0085(13) C(5) 0.0154(12) 0.0172(13) 0.0219(14) 0.0075(11) -0.0013(11) 0.0014(11) C(6) 0.0153(13) 0.0193(13) 0.0286(15) 0.0089(11) 0.0041(11) 0.0040(11) C(7) 0.0164(13) 0.0206(13) 0.0207(14) 0.0111(11) 0.0034(10) 0.0003(11) C(8) 0.0170(14) 0.0296(16) 0.0264(15) 0.0027(12) 0.0007(12) 0.0041(13) C(9) 0.0200(14) 0.0396(18) 0.0266(16) 0.0083(13) -0.0050(12) 0.0035(13) C(10) 0.0250(15) 0.0303(16) 0.0227(15) 0.0126(13) -0.0009(12) 0.0065(13) C(11) 0.0205(14) 0.0200(14) 0.0233(14) 0.0078(12) 0.0016(11) 0.0007(11) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.7.0' _computing_molecular_graphics ORTEP3 #============================================================================== # 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) 2.5582(4) ? . . Br(1) Cu(1) 2.5101(4) ? . 77503 Br(1) Cu(1) 2.4713(3) ? . 56511 Cu(1) N(1) 2.034(2) ? . . N(1) C(7) 1.353(2) ? . . N(1) C(11) 1.348(3) ? . . C(1) C(2) 1.410(3) ? . . C(1) C(2) 1.404(4) ? . 65502 C(1) C(5) 1.530(4) ? . . C(2) C(3) 1.523(5) ? . . C(3) C(4) 1.531(4) ? . . C(5) C(6) 1.550(4) ? . . C(6) C(7) 1.504(4) ? . . C(7) C(8) 1.383(3) ? . . C(8) C(9) 1.379(4) ? . . C(9) C(10) 1.380(3) ? . . C(10) C(11) 1.376(4) ? . . C(3) H(31) 0.950 ? . . C(3) H(32) 0.950 ? . . C(4) H(41) 0.950 ? . . C(4) H(42) 0.950 ? . . C(4) H(43) 0.950 ? . . C(5) H(51) 0.950 ? . . C(5) H(52) 0.950 ? . . C(6) H(61) 0.950 ? . . C(6) H(62) 0.950 ? . . C(8) H(8) 0.950 ? . . C(9) H(9) 0.950 ? . . C(10) H(10) 0.950 ? . . C(11) H(11) 0.950 ? . . 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) 113.433(18) ? . . 77503 Cu(1) Br(1) Cu(1) 71.136(12) ? . . 56511 Cu(1) Br(1) Cu(1) 71.948(13) ? 77503 . 56511 Br(1) Cu(1) Br(1) 104.564(16) ? . . 75502 Br(1) Cu(1) Br(1) 107.442(14) ? . . 54512 Br(1) Cu(1) N(1) 106.47(6) ? . . . Br(1) Cu(1) Br(1) 108.97(2) ? 75502 . 54512 Br(1) Cu(1) N(1) 110.96(7) ? 75502 . . Br(1) Cu(1) N(1) 117.55(6) ? 54512 . . Cu(1) N(1) C(7) 125.1(2) ? . . . Cu(1) N(1) C(11) 116.53(15) ? . . . C(7) N(1) C(11) 117.8(2) ? . . . C(2) C(1) C(2) 120.0(2) ? . . 65502 C(2) C(1) C(5) 119.5(2) ? . . . C(2) C(1) C(5) 120.5(2) ? 65502 . . C(1) C(2) C(1) 120.0(3) ? . . 66503 C(1) C(2) C(3) 119.9(2) ? . . . C(1) C(2) C(3) 119.9(2) ? 66503 . . C(2) C(3) C(4) 112.1(2) ? . . . C(1) C(5) C(6) 115.9(2) ? . . . C(5) C(6) C(7) 116.2(2) ? . . . N(1) C(7) C(6) 118.9(2) ? . . . N(1) C(7) C(8) 120.9(2) ? . . . C(6) C(7) C(8) 120.2(2) ? . . . C(7) C(8) C(9) 120.5(2) ? . . . C(8) C(9) C(10) 118.8(2) ? . . . C(9) C(10) C(11) 118.1(2) ? . . . N(1) C(11) C(10) 123.8(2) ? . . . C(2) C(3) H(31) 108.7 ? . . . C(2) C(3) H(32) 109.1 ? . . . C(4) C(3) H(31) 108.5 ? . . . C(4) C(3) H(32) 109.0 ? . . . H(31) C(3) H(32) 109.5 ? . . . C(3) C(4) H(41) 109.2 ? . . . C(3) C(4) H(42) 110.2 ? . . . C(3) C(4) H(43) 109.0 ? . . . H(41) C(4) H(42) 109.5 ? . . . H(41) C(4) H(43) 109.5 ? . . . H(42) C(4) H(43) 109.5 ? . . . C(1) C(5) H(51) 107.4 ? . . . C(1) C(5) H(52) 107.8 ? . . . C(6) C(5) H(51) 107.5 ? . . . C(6) C(5) H(52) 108.6 ? . . . H(51) C(5) H(52) 109.5 ? . . . C(5) C(6) H(61) 108.1 ? . . . C(5) C(6) H(62) 107.5 ? . . . C(7) C(6) H(61) 107.8 ? . . . C(7) C(6) H(62) 107.7 ? . . . H(61) C(6) H(62) 109.5 ? . . . C(7) C(8) H(8) 119.2 ? . . . C(9) C(8) H(8) 120.2 ? . . . C(8) C(9) H(9) 120.7 ? . . . C(10) C(9) H(9) 120.5 ? . . . C(9) C(10) H(10) 121.1 ? . . . C(11) C(10) H(10) 120.8 ? . . . N(1) C(11) H(11) 117.9 ? . . . C(10) C(11) H(11) 118.2 ? . . . 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) Br(1) 61.049(17) ? . . 77503 77503 Cu(1) Br(1) Cu(1) N(1) 175.46(7) ? . . 77503 77503 Cu(1) Br(1) Cu(1) Br(1) -61.534(18) ? 77503 . . 75502 Cu(1) Br(1) Cu(1) Br(1) 54.17(2) ? 77503 . . 54512 Cu(1) Br(1) Cu(1) N(1) -179.07(7) ? 77503 . . . Cu(1) Br(1) Cu(1) Br(1) 5.46(2) ? . . 56511 54512 Cu(1) Br(1) Cu(1) Br(1) 118.21(2) ? . . 56511 56511 Cu(1) Br(1) Cu(1) N(1) -121.85(5) ? . . 56511 56511 Cu(1) Br(1) Cu(1) Br(1) -121.203(19) ? 56511 . . 75502 Cu(1) Br(1) Cu(1) Br(1) -5.50(2) ? 56511 . . 54512 Cu(1) Br(1) Cu(1) N(1) 121.26(7) ? 56511 . . . Cu(1) Br(1) Cu(1) Br(1) -118.14(2) ? 77503 . 56511 54512 Cu(1) Br(1) Cu(1) Br(1) -5.387(19) ? 77503 . 56511 56511 Cu(1) Br(1) Cu(1) N(1) 114.55(5) ? 77503 . 56511 56511 Cu(1) Br(1) Cu(1) Br(1) 120.259(18) ? 56511 . 77503 77503 Cu(1) Br(1) Cu(1) N(1) -125.33(8) ? 56511 . 77503 77503 Br(1) Cu(1) N(1) C(7) -174.6(2) ? . . . . Br(1) Cu(1) N(1) C(11) 14.3(2) ? . . . . Br(1) Cu(1) N(1) C(7) 72.2(2) ? 75502 . . . Br(1) Cu(1) N(1) C(11) -98.9(2) ? 75502 . . . Br(1) Cu(1) N(1) C(7) -54.2(2) ? 54512 . . . Br(1) Cu(1) N(1) C(11) 134.7(2) ? 54512 . . . Cu(1) N(1) C(7) C(6) 7.4(4) ? . . . . Cu(1) N(1) C(7) C(8) -170.9(2) ? . . . . Cu(1) N(1) C(11) C(10) 171.1(2) ? . . . . C(7) N(1) C(11) C(10) -0.7(5) ? . . . . C(11) N(1) C(7) C(6) 178.4(2) ? . . . . C(11) N(1) C(7) C(8) 0.2(4) ? . . . . C(2) C(1) C(2) C(1) 0.1(2) ? . . 65502 65502 C(2) C(1) C(2) C(3) 174.9(2) ? . . 65502 65502 C(2) C(1) C(2) C(1) -0.1(2) ? 65502 . . 66503 C(2) C(1) C(2) C(3) -174.9(2) ? 65502 . . . C(2) C(1) C(5) C(6) 79.3(3) ? . . . . C(5) C(1) C(2) C(1) 178.2(2) ? . . . 66503 C(5) C(1) C(2) C(3) 3.4(3) ? . . . . C(2) C(1) C(5) C(6) -102.4(2) ? 65502 . . . C(5) C(1) C(2) C(1) -178.2(2) ? . . 65502 65502 C(5) C(1) C(2) C(3) -3.4(3) ? . . 65502 65502 C(1) C(2) C(3) C(4) 91.2(2) ? . . . . C(1) C(2) C(3) C(4) -83.7(2) ? 66503 . . . C(1) C(5) C(6) C(7) 58.3(2) ? . . . . C(5) C(6) C(7) N(1) 99.3(3) ? . . . . C(5) C(6) C(7) C(8) -82.4(3) ? . . . . N(1) C(7) C(8) C(9) 1.0(5) ? . . . . C(6) C(7) C(8) C(9) -177.3(3) ? . . . . C(7) C(8) C(9) C(10) -1.6(5) ? . . . . C(8) C(9) C(10) C(11) 1.1(5) ? . . . . C(9) C(10) C(11) N(1) 0.1(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(9) 3.583(2) ? . 65506 C(9) Br(1) 3.583(3) ? . 56505 Br(1) H(9) 2.956 ? . 65506 Br(1) H(10) 3.030 ? . 65506 C(3) H(32) 3.360 ? . 65510 C(3) H(61) 3.550 ? . 65510 C(3) H(62) 2.899 ? . 65510 C(4) H(43) 3.563 ? . 54518 C(4) H(62) 3.171 ? . 65510 C(4) H(10) 3.120 ? . 44507 C(4) H(11) 3.576 ? . 44507 C(6) H(31) 3.142 ? . 65510 C(6) H(32) 3.506 ? . 65510 C(6) H(42) 3.264 ? . 65510 C(7) H(42) 3.414 ? . 65510 C(10) H(42) 3.160 ? . 55413 C(11) H(42) 3.470 ? . 55413 H(31) C(6) 3.142 ? . 65510 H(31) H(32) 3.315 ? . 65510 H(31) H(61) 2.845 ? . 65510 H(31) H(62) 2.577 ? . 65510 H(32) C(3) 3.360 ? . 65510 H(32) C(6) 3.506 ? . 65510 H(32) H(31) 3.315 ? . 65510 H(32) H(32) 2.598 ? . 65510 H(32) H(62) 2.642 ? . 65510 H(41) H(43) 2.893 ? . 54518 H(41) H(62) 3.462 ? . 65510 H(41) H(11) 3.521 ? . 44507 H(42) C(6) 3.264 ? . 65510 H(42) C(7) 3.414 ? . 65510 H(42) C(10) 3.160 ? . 44507 H(42) C(11) 3.470 ? . 44507 H(42) H(61) 3.264 ? . 65510 H(42) H(62) 2.694 ? . 65510 H(42) H(10) 2.392 ? . 44507 H(42) H(11) 3.001 ? . 44507 H(43) C(4) 3.563 ? . 55517 H(43) H(41) 2.893 ? . 55517 H(43) H(43) 3.367 ? . 55517 H(43) H(43) 3.367 ? . 54518 H(43) H(52) 3.310 ? . 55517 H(43) H(10) 3.029 ? . 44507 H(52) H(43) 3.310 ? . 54518 H(61) C(3) 3.550 ? . 65510 H(61) H(31) 2.845 ? . 65510 H(61) H(42) 3.264 ? . 65510 H(62) C(3) 2.899 ? . 65510 H(62) C(4) 3.171 ? . 65510 H(62) H(31) 2.577 ? . 65510 H(62) H(32) 2.642 ? . 65510 H(62) H(41) 3.462 ? . 65510 H(62) H(42) 2.694 ? . 65510 H(9) Br(1) 2.956 ? . 56505 H(10) Br(1) 3.030 ? . 56505 H(10) C(4) 3.120 ? . 55413 H(10) H(42) 2.392 ? . 55413 H(10) H(43) 3.029 ? . 55413 H(11) C(4) 3.576 ? . 55413 H(11) H(41) 3.521 ? . 55413 H(11) H(42) 3.001 ? . 55413 Cu(1) Cu(1) 2.9263(6) ? . 54512 Cu(1) Cu(1) 4.2370(7) ? . 75502 Cu(1) Cu(1) 5.1493(5) ? . 76510 Cu(1) Cu(1) 4.2370(4) ? . 77503 Cu(1) Cu(1) 2.9263(4) ? . 56511 Cu(1) Br(1) 2.4713(3) ? . 54512 Cu(1) Br(1) 2.5101(6) ? . 75502 #============================================================================== # 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 #============================================================================== #===END #============================================================================== data__[Cu6I6L2]n _database_code_depnum_ccdc_archive 'CCDC 275922' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C33 H39 Cu3 I3 N3 ' _chemical_formula_moiety 'C33 H39 Cu3 I3 N3 ' _chemical_formula_weight 1049.04 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' _symmetry_Int_Tables_number 148 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -Y,+X-Y,+Z 3 -X+Y,-X,+Z 4 -X,-Y,-Z 5 +Y,-X+Y,-Z 6 +X-Y,+X,-Z 7 2/3+X,1/3+Y,1/3+Z 8 2/3-Y,1/3+X-Y,1/3+Z 9 2/3-X+Y,1/3-X,1/3+Z 10 2/3-X,1/3-Y,1/3-Z 11 2/3+Y,1/3-X+Y,1/3-Z 12 2/3+X-Y,1/3+X,1/3-Z 13 1/3+X,2/3+Y,2/3+Z 14 1/3-Y,2/3+X-Y,2/3+Z 15 1/3-X+Y,2/3-X,2/3+Z 16 1/3-X,2/3-Y,2/3-Z 17 1/3+Y,2/3-X+Y,2/3-Z 18 1/3+X-Y,2/3+X,2/3-Z #------------------------------------------------------------------------------ _cell_length_a 15.3547(17) _cell_length_b 15.3547(17) _cell_length_c 25.539(5) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 120.0000 _cell_volume 5214.5(13) _cell_formula_units_Z 6 _cell_measurement_reflns_used 10896 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 163.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 2.004 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3024.00 _exptl_absorpt_coefficient_mu 4.511 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.331 _exptl_absorpt_correction_T_max 0.729 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 16836 _diffrn_reflns_av_R_equivalents 0.044 _diffrn_reflns_theta_max 27.43 _diffrn_measured_fraction_theta_max 1.062 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 1.062 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using all reflections. 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 2646 _reflns_number_gt 2142 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0203 _refine_ls_wR_factor_ref 0.0230 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 2646 _refine_ls_number_parameters 140 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0001Fo^2^ + 0.3000\s(Fo^2^)]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.19 _refine_diff_density_min -0.75 _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) ; Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; I I -0.474 1.812 ; 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 I(1) I 1.262140(10) 0.776480(10) 0.095220(10) 0.02231(5) Uani 1.00 1 d . . . Cu(1) Cu 1.14410(3) 0.58963(3) 0.13644(2) 0.02756(10) Uani 1.00 1 d . . . N(1) N 1.00353(18) 0.53367(18) 0.10337(10) 0.0238(7) Uani 1.00 1 d . . . C(1) C 0.76831(19) 0.3588(2) 0.20809(12) 0.0190(7) Uani 1.00 1 d . . . C(2) C 0.6917(2) 0.2571(2) 0.20800(12) 0.0199(7) Uani 1.00 1 d . . . C(3) C 0.7187(2) 0.1742(2) 0.21324(12) 0.0245(8) Uani 1.00 1 d . . . C(4) C 0.7209(2) 0.1452(2) 0.27042(14) 0.0369(10) Uani 1.00 1 d . . . C(5) C 0.8789(2) 0.3853(2) 0.20977(12) 0.0229(8) Uani 1.00 1 d . . . C(6) C 0.9254(2) 0.3798(2) 0.15739(12) 0.0259(8) Uani 1.00 1 d . . . C(7) C 0.9219(2) 0.4427(2) 0.11368(12) 0.0241(8) Uani 1.00 1 d . . . C(8) C 0.8355(2) 0.4063(2) 0.08304(14) 0.0388(9) Uani 1.00 1 d . . . C(9) C 0.8324(2) 0.4621(2) 0.04167(14) 0.0439(11) Uani 1.00 1 d . . . C(10) C 0.9144(2) 0.5551(2) 0.03170(14) 0.0378(10) Uani 1.00 1 d . . . C(11) C 0.9974(2) 0.5878(2) 0.06332(12) 0.0286(8) Uani 1.00 1 d . . . H(32) H 0.6701 0.1163 0.1949 0.029 Uiso 1.00 1 c R . . H(31) H 0.7832 0.1970 0.1982 0.029 Uiso 1.00 1 c R . . H(41) H 0.7866 0.1862 0.2842 0.047 Uiso 1.00 1 c R . . H(42) H 0.7029 0.0765 0.2728 0.047 Uiso 1.00 1 c R . . H(43) H 0.6744 0.1560 0.2899 0.047 Uiso 1.00 1 c R . . H(51) H 0.9170 0.4525 0.2221 0.027 Uiso 1.00 1 c R . . H(52) H 0.8838 0.3410 0.2340 0.027 Uiso 1.00 1 c R . . H(61) H 0.9941 0.4005 0.1635 0.031 Uiso 1.00 1 c R . . H(62) H 0.8908 0.3115 0.1464 0.031 Uiso 1.00 1 c R . . H(8) H 0.7790 0.3424 0.0907 0.039 Uiso 1.00 1 c R . . H(9) H 0.7744 0.4363 0.0201 0.047 Uiso 1.00 1 c R . . H(10) H 0.9136 0.5958 0.0039 0.044 Uiso 1.00 1 c R . . H(11) H 1.0539 0.6523 0.0567 0.032 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 I(1) 0.01934(11) 0.02128(11) 0.02504(11) 0.00921(9) 0.00130(9) 0.00238(9) Cu(1) 0.0219(2) 0.0309(2) 0.0293(2) 0.01277(18) -0.00084(18) 0.00227(19) N(1) 0.0238(13) 0.0251(13) 0.0238(16) 0.0132(11) 0.0010(11) 0.0014(11) C(1) 0.0132(13) 0.0180(14) 0.0233(18) 0.0060(11) 0.0007(12) 0.0036(12) C(2) 0.0216(15) 0.0205(14) 0.0209(17) 0.0131(12) 0.0004(12) 0.0010(12) C(3) 0.0187(15) 0.0176(14) 0.036(2) 0.0084(12) 0.0010(14) 0.0031(14) C(4) 0.039(2) 0.0347(19) 0.043(2) 0.0228(16) 0.0047(17) 0.0104(17) C(5) 0.0183(14) 0.0205(15) 0.030(2) 0.0098(12) -0.0011(13) 0.0023(13) C(6) 0.0178(15) 0.0214(15) 0.037(2) 0.0088(13) 0.0025(14) 0.0006(14) C(7) 0.0188(14) 0.0259(16) 0.0274(19) 0.0111(13) 0.0012(13) -0.0005(14) C(8) 0.0215(17) 0.040(2) 0.036(2) 0.0009(15) -0.0010(16) 0.0084(18) C(9) 0.0213(17) 0.060(2) 0.035(2) 0.0092(17) -0.0065(16) 0.0070(19) C(10) 0.0320(18) 0.045(2) 0.032(2) 0.0162(17) -0.0019(16) 0.0119(17) C(11) 0.0240(16) 0.0282(17) 0.027(2) 0.0083(14) -0.0012(14) 0.0045(15) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.7.0' _computing_molecular_graphics ORTEP3 #============================================================================== # 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 I(1) Cu(1) 2.7248(4) ? . . I(1) Cu(1) 2.6628(4) ? . 77503 I(1) Cu(1) 2.5991(5) ? . 56511 Cu(1) N(1) 2.063(2) ? . . N(1) C(7) 1.356(3) ? . . N(1) C(11) 1.351(4) ? . . C(1) C(2) 1.409(3) ? . . C(1) C(2) 1.401(5) ? . 65502 C(1) C(5) 1.536(4) ? . . C(2) C(3) 1.529(5) ? . . C(3) C(4) 1.532(5) ? . . C(5) C(6) 1.539(4) ? . . C(6) C(7) 1.495(5) ? . . C(7) C(8) 1.394(4) ? . . C(8) C(9) 1.375(6) ? . . C(9) C(10) 1.375(4) ? . . C(10) C(11) 1.374(4) ? . . C(3) H(32) 0.950 ? . . C(3) H(31) 0.950 ? . . C(4) H(41) 0.950 ? . . C(4) H(42) 0.950 ? . . C(4) H(43) 0.950 ? . . C(5) H(51) 0.950 ? . . C(5) H(52) 0.950 ? . . C(6) H(61) 0.950 ? . . C(6) H(62) 0.950 ? . . C(8) H(8) 0.950 ? . . C(9) H(9) 0.950 ? . . C(10) H(10) 0.950 ? . . C(11) H(11) 0.950 ? . . 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) I(1) Cu(1) 108.895(16) ? . . 77503 Cu(1) I(1) Cu(1) 67.627(14) ? . . 56511 Cu(1) I(1) Cu(1) 68.570(15) ? 77503 . 56511 I(1) Cu(1) I(1) 102.451(16) ? . . 75502 I(1) Cu(1) I(1) 110.755(15) ? . . 54512 I(1) Cu(1) N(1) 106.68(7) ? . . . I(1) Cu(1) I(1) 112.75(2) ? 75502 . 54512 I(1) Cu(1) N(1) 106.61(8) ? 75502 . . I(1) Cu(1) N(1) 116.49(7) ? 54512 . . Cu(1) N(1) C(7) 125.8(2) ? . . . Cu(1) N(1) C(11) 115.73(16) ? . . . C(7) N(1) C(11) 117.9(2) ? . . . C(2) C(1) C(2) 119.8(2) ? . . 65502 C(2) C(1) C(5) 119.5(3) ? . . . C(2) C(1) C(5) 120.7(2) ? 65502 . . C(1) C(2) C(1) 120.2(3) ? . . 66503 C(1) C(2) C(3) 120.0(2) ? . . . C(1) C(2) C(3) 119.5(2) ? 66503 . . C(2) C(3) C(4) 112.3(3) ? . . . C(1) C(5) C(6) 116.3(2) ? . . . C(5) C(6) C(7) 116.5(3) ? . . . N(1) C(7) C(6) 119.8(2) ? . . . N(1) C(7) C(8) 120.5(3) ? . . . C(6) C(7) C(8) 119.6(2) ? . . . C(7) C(8) C(9) 120.2(2) ? . . . C(8) C(9) C(10) 119.4(3) ? . . . C(9) C(10) C(11) 118.1(3) ? . . . N(1) C(11) C(10) 123.9(2) ? . . . C(2) C(3) H(32) 108.8 ? . . . C(2) C(3) H(31) 108.9 ? . . . C(4) C(3) H(32) 108.6 ? . . . C(4) C(3) H(31) 108.8 ? . . . H(32) C(3) H(31) 109.5 ? . . . C(3) C(4) H(41) 109.3 ? . . . C(3) C(4) H(42) 110.4 ? . . . C(3) C(4) H(43) 108.7 ? . . . H(41) C(4) H(42) 109.5 ? . . . H(41) C(4) H(43) 109.5 ? . . . H(42) C(4) H(43) 109.5 ? . . . C(1) C(5) H(51) 107.2 ? . . . C(1) C(5) H(52) 107.6 ? . . . C(6) C(5) H(51) 107.3 ? . . . C(6) C(5) H(52) 108.8 ? . . . H(51) C(5) H(52) 109.5 ? . . . C(5) C(6) H(61) 107.9 ? . . . C(5) C(6) H(62) 107.3 ? . . . C(7) C(6) H(61) 107.4 ? . . . C(7) C(6) H(62) 108.2 ? . . . H(61) C(6) H(62) 109.5 ? . . . C(7) C(8) H(8) 119.5 ? . . . C(9) C(8) H(8) 120.3 ? . . . C(8) C(9) H(9) 120.3 ? . . . C(10) C(9) H(9) 120.4 ? . . . C(9) C(10) H(10) 121.0 ? . . . C(11) C(10) H(10) 120.9 ? . . . N(1) C(11) H(11) 117.9 ? . . . C(10) C(11) H(11) 118.3 ? . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Cu(1) I(1) Cu(1) I(1) 68.01(2) ? . . 77503 77503 Cu(1) I(1) Cu(1) N(1) 179.88(8) ? . . 77503 77503 Cu(1) I(1) Cu(1) I(1) -68.71(2) ? 77503 . . 75502 Cu(1) I(1) Cu(1) I(1) 51.76(2) ? 77503 . . 54512 Cu(1) I(1) Cu(1) N(1) 179.46(8) ? 77503 . . . Cu(1) I(1) Cu(1) I(1) 4.240(18) ? . . 56511 54512 Cu(1) I(1) Cu(1) I(1) 118.38(2) ? . . 56511 56511 Cu(1) I(1) Cu(1) N(1) -119.50(6) ? . . 56511 56511 Cu(1) I(1) Cu(1) I(1) -124.76(2) ? 56511 . . 75502 Cu(1) I(1) Cu(1) I(1) -4.284(18) ? 56511 . . 54512 Cu(1) I(1) Cu(1) N(1) 123.41(8) ? 56511 . . . Cu(1) I(1) Cu(1) I(1) -118.29(2) ? 77503 . 56511 54512 Cu(1) I(1) Cu(1) I(1) -4.153(16) ? 77503 . 56511 56511 Cu(1) I(1) Cu(1) N(1) 117.97(6) ? 77503 . 56511 56511 Cu(1) I(1) Cu(1) I(1) 123.502(19) ? 56511 . 77503 77503 Cu(1) I(1) Cu(1) N(1) -124.62(8) ? 56511 . 77503 77503 I(1) Cu(1) N(1) C(7) -179.3(2) ? . . . . I(1) Cu(1) N(1) C(11) 9.6(2) ? . . . . I(1) Cu(1) N(1) C(7) 71.8(2) ? 75502 . . . I(1) Cu(1) N(1) C(11) -99.3(2) ? 75502 . . . I(1) Cu(1) N(1) C(7) -55.1(3) ? 54512 . . . I(1) Cu(1) N(1) C(11) 133.9(2) ? 54512 . . . Cu(1) N(1) C(7) C(6) 8.7(4) ? . . . . Cu(1) N(1) C(7) C(8) -169.8(2) ? . . . . Cu(1) N(1) C(11) C(10) 170.1(3) ? . . . . C(7) N(1) C(11) C(10) -1.7(5) ? . . . . C(11) N(1) C(7) C(6) 179.6(3) ? . . . . C(11) N(1) C(7) C(8) 1.1(5) ? . . . . C(2) C(1) C(2) C(1) 0.3(4) ? . . 65502 65502 C(2) C(1) C(2) C(3) 174.3(2) ? . . 65502 65502 C(2) C(1) C(2) C(1) -0.3(4) ? 65502 . . 66503 C(2) C(1) C(2) C(3) -174.3(2) ? 65502 . . . C(2) C(1) C(5) C(6) 80.6(3) ? . . . . C(5) C(1) C(2) C(1) 178.1(2) ? . . . 66503 C(5) C(1) C(2) C(3) 4.1(4) ? . . . . C(2) C(1) C(5) C(6) -101.1(3) ? 65502 . . . C(5) C(1) C(2) C(1) -178.0(2) ? . . 65502 65502 C(5) C(1) C(2) C(3) -4.0(4) ? . . 65502 65502 C(1) C(2) C(3) C(4) 90.2(3) ? . . . . C(1) C(2) C(3) C(4) -83.8(3) ? 66503 . . . C(1) C(5) C(6) C(7) 56.8(3) ? . . . . C(5) C(6) C(7) N(1) 97.9(3) ? . . . . C(5) C(6) C(7) C(8) -83.7(3) ? . . . . N(1) C(7) C(8) C(9) 0.5(6) ? . . . . C(6) C(7) C(8) C(9) -177.9(3) ? . . . . C(7) C(8) C(9) C(10) -1.7(6) ? . . . . C(8) C(9) C(10) C(11) 1.1(6) ? . . . . C(9) C(10) C(11) N(1) 0.6(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 I(1) H(9) 3.173 ? . 65506 I(1) H(10) 3.126 ? . 65506 C(3) H(31) 3.491 ? . 65510 C(3) H(61) 3.583 ? . 65510 C(3) H(62) 2.957 ? . 65510 C(4) H(62) 3.233 ? . 65510 C(4) H(10) 3.380 ? . 44507 C(6) H(32) 3.225 ? . 65510 C(6) H(31) 3.508 ? . 65510 C(6) H(42) 3.339 ? . 65510 C(7) H(42) 3.499 ? . 65510 C(10) H(42) 3.461 ? . 55413 H(32) C(6) 3.225 ? . 65510 H(32) H(31) 3.487 ? . 65510 H(32) H(61) 2.908 ? . 65510 H(32) H(62) 2.672 ? . 65510 H(31) C(3) 3.491 ? . 65510 H(31) C(6) 3.508 ? . 65510 H(31) H(32) 3.487 ? . 65510 H(31) H(31) 2.697 ? . 65510 H(31) H(62) 2.651 ? . 65510 H(41) H(43) 3.142 ? . 54518 H(41) H(62) 3.486 ? . 65510 H(42) C(6) 3.339 ? . 65510 H(42) C(7) 3.499 ? . 65510 H(42) C(10) 3.461 ? . 44507 H(42) H(61) 3.314 ? . 65510 H(42) H(62) 2.778 ? . 65510 H(42) H(10) 2.667 ? . 44507 H(42) H(11) 3.370 ? . 44507 H(43) H(41) 3.142 ? . 55517 H(43) H(43) 3.561 ? . 55517 H(43) H(43) 3.561 ? . 54518 H(43) H(10) 3.264 ? . 44507 H(61) C(3) 3.583 ? . 65510 H(61) H(32) 2.908 ? . 65510 H(61) H(42) 3.314 ? . 65510 H(62) C(3) 2.957 ? . 65510 H(62) C(4) 3.233 ? . 65510 H(62) H(32) 2.672 ? . 65510 H(62) H(31) 2.651 ? . 65510 H(62) H(41) 3.486 ? . 65510 H(62) H(42) 2.778 ? . 65510 H(9) I(1) 3.173 ? . 56505 H(10) I(1) 3.126 ? . 56505 H(10) C(4) 3.380 ? . 55413 H(10) H(42) 2.667 ? . 55413 H(10) H(43) 3.264 ? . 55413 H(11) H(42) 3.370 ? . 55413 Cu(1) Cu(1) 2.9645(7) ? . 54512 Cu(1) Cu(1) 4.3834(7) ? . 75502 Cu(1) Cu(1) 5.2918(6) ? . 76510 Cu(1) Cu(1) 4.3834(4) ? . 77503 Cu(1) Cu(1) 2.9645(5) ? . 56511 Cu(1) I(1) 2.5991(5) ? . 54512 Cu(1) I(1) 2.6628(5) ? . 75502 #============================================================================== # 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 #============================================================================== #===END #============================================================================== data__[CuL]PF6 _database_code_depnum_ccdc_archive 'CCDC 275923' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C33 H39 Cu F6 N3 P ' _chemical_formula_moiety 'C33 H39 Cu F6 N3 P ' _chemical_formula_weight 686.20 _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 10.027(4) _cell_length_b 10.254(3) _cell_length_c 16.081(6) _cell_angle_alpha 82.509(14) _cell_angle_beta 77.487(19) _cell_angle_gamma 82.478(17) _cell_volume 1591.3(10) _cell_formula_units_Z 2 _cell_measurement_reflns_used 6678 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 160.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712.00 _exptl_absorpt_coefficient_mu 0.800 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.725 _exptl_absorpt_correction_T_max 0.887 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 15670 _diffrn_reflns_av_R_equivalents 0.022 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using all reflections. 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 7254 _reflns_number_gt 5961 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.0593 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 7254 _refine_ls_number_parameters 436 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0017Fo^2^ + 1.0000\s(Fo^2^)]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.64 _refine_diff_density_min -0.48 _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) ; Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.017 0.010 ; 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 Cu(1) Cu 0.10942(3) 0.07467(2) 0.85239(2) 0.02977(7) Uani 1.00 1 d . . . P(1) P 0.26581(5) 0.26363(5) 1.01522(3) 0.02519(13) Uani 1.00 1 d . . . F(1) F 0.38425(16) 0.14487(13) 1.01834(12) 0.0530(4) Uani 1.00 1 d . . . F(2) F 0.35687(14) 0.35908(12) 1.04411(10) 0.0432(4) Uani 1.00 1 d . . . F(3) F 0.14576(16) 0.38107(14) 1.01252(12) 0.0539(4) Uani 1.00 1 d . . . F(4) F 0.17388(14) 0.16877(13) 0.98546(9) 0.0432(4) Uani 1.00 1 d . . . F(5) F 0.33068(18) 0.30617(18) 0.91735(9) 0.0561(4) Uani 1.00 1 d . . . F(6) F 0.19927(17) 0.22029(17) 1.11257(9) 0.0541(4) Uani 1.00 1 d . . . N(1) N -0.2126(2) -0.13614(19) 0.57971(12) 0.0335(4) Uani 1.00 1 d . . . N(2) N 0.22028(18) -0.09141(17) 0.86367(11) 0.0265(4) Uani 1.00 1 d . . . N(3) N -0.06063(18) 0.18728(16) 0.86603(11) 0.0259(4) Uani 1.00 1 d . . . C(1) C 0.0949(2) 0.06454(19) 0.64555(12) 0.0242(4) Uani 1.00 1 d . . . C(2) C 0.2246(2) 0.00767(19) 0.65956(12) 0.0250(4) Uani 1.00 1 d . . . C(3) C 0.3115(2) 0.0857(2) 0.68504(12) 0.0263(4) Uani 1.00 1 d . . . C(4) C 0.2664(2) 0.2190(2) 0.69805(12) 0.0272(4) Uani 1.00 1 d . . . C(5) C 0.1332(2) 0.27264(19) 0.68908(12) 0.0261(4) Uani 1.00 1 d . . . C(6) C 0.0480(2) 0.19564(19) 0.66165(12) 0.0246(4) Uani 1.00 1 d . . . C(7) C 0.2715(2) -0.1363(2) 0.64421(13) 0.0306(5) Uani 1.00 1 d . . . C(8) C 0.3450(2) -0.1507(2) 0.55150(16) 0.0398(6) Uani 1.00 1 d . . . C(9) C 0.3652(2) 0.3080(2) 0.71580(13) 0.0328(5) Uani 1.00 1 d . . . C(10) C 0.4402(3) 0.3787(3) 0.63230(18) 0.0590(8) Uani 1.00 1 d . . . C(11) C -0.0936(2) 0.2551(2) 0.64731(13) 0.0311(5) Uani 1.00 1 d . . . C(12) C -0.0876(2) 0.3313(2) 0.55838(16) 0.0425(6) Uani 1.00 1 d . . . C(13) C 0.0042(2) -0.01735(19) 0.61428(12) 0.0250(4) Uani 1.00 1 d . . . C(14) C -0.0945(2) -0.0891(2) 0.68753(12) 0.0292(5) Uani 1.00 1 d . . . C(15) C -0.1756(2) -0.17858(19) 0.65469(12) 0.0239(4) Uani 1.00 1 d . . . C(16) C -0.2090(2) -0.2980(2) 0.69972(14) 0.0354(6) Uani 1.00 1 d . . . C(17) C -0.2832(2) -0.3768(2) 0.66740(16) 0.0410(6) Uani 1.00 1 d . . . C(18) C -0.3196(2) -0.3344(2) 0.58969(14) 0.0354(6) Uani 1.00 1 d . . . C(19) C -0.2820(2) -0.2149(2) 0.54849(13) 0.0362(6) Uani 1.00 1 d . . . C(20) C 0.4494(2) 0.0270(2) 0.70455(13) 0.0319(5) Uani 1.00 1 d . . . C(21) C 0.4417(2) -0.0056(2) 0.80235(13) 0.0333(5) Uani 1.00 1 d . . . C(22) C 0.3580(2) -0.1173(2) 0.84029(12) 0.0285(5) Uani 1.00 1 d . . . C(23) C 0.4201(2) -0.2469(2) 0.84894(14) 0.0384(6) Uani 1.00 1 d . . . C(24) C 0.3428(2) -0.3504(2) 0.88153(17) 0.0444(6) Uani 1.00 1 d . . . C(25) C 0.2015(2) -0.3238(2) 0.90526(16) 0.0382(6) Uani 1.00 1 d . . . C(26) C 0.1454(2) -0.1944(2) 0.89523(13) 0.0333(5) Uani 1.00 1 d . . . C(27) C 0.0789(2) 0.40793(19) 0.71815(12) 0.0292(5) Uani 1.00 1 d . . . C(28) C 0.0369(2) 0.3987(2) 0.81734(12) 0.0295(5) Uani 1.00 1 d . . . C(29) C -0.0832(2) 0.32098(19) 0.85238(12) 0.0261(4) Uani 1.00 1 d . . . C(30) C -0.2161(2) 0.3842(2) 0.86832(13) 0.0337(5) Uani 1.00 1 d . . . C(31) C -0.3270(2) 0.3132(2) 0.89765(16) 0.0394(6) Uani 1.00 1 d . . . C(32) C -0.3034(2) 0.1758(2) 0.91036(16) 0.0384(6) Uani 1.00 1 d . . . C(33) C -0.1722(2) 0.1190(2) 0.89429(13) 0.0327(5) Uani 1.00 1 d . . . H(71) H 0.3327 -0.1719 0.6810 0.038 Uiso 1.00 1 c R . . H(72) H 0.1935 -0.1844 0.6571 0.037 Uiso 1.00 1 c R . . H(81) H 0.2799 -0.1608 0.5185 0.049 Uiso 1.00 1 c R . . H(82) H 0.4112 -0.2261 0.5499 0.049 Uiso 1.00 1 c R . . H(83) H 0.3897 -0.0738 0.5286 0.049 Uiso 1.00 1 c R . . H(92) H 0.3139 0.3733 0.7503 0.041 Uiso 1.00 1 c R . . H(91) H 0.4297 0.2566 0.7455 0.040 Uiso 1.00 1 c R . . H(101) H 0.5231 0.3255 0.6122 0.074 Uiso 1.00 1 c R . . H(102) H 0.4611 0.4623 0.6423 0.074 Uiso 1.00 1 c R . . H(103) H 0.3844 0.3907 0.5905 0.074 Uiso 1.00 1 c R . . H(111) H -0.1498 0.1854 0.6528 0.038 Uiso 1.00 1 c R . . H(112) H -0.1328 0.3134 0.6896 0.038 Uiso 1.00 1 c R . . H(121) H -0.0767 0.4211 0.5613 0.053 Uiso 1.00 1 c R . . H(122) H -0.1706 0.3267 0.5401 0.053 Uiso 1.00 1 c R . . H(123) H -0.0122 0.2939 0.5188 0.053 Uiso 1.00 1 c R . . H(131) H -0.0489 0.0394 0.5793 0.030 Uiso 1.00 1 c R . . H(132) H 0.0612 -0.0816 0.5814 0.031 Uiso 1.00 1 c R . . H(141) H -0.0422 -0.1413 0.7249 0.036 Uiso 1.00 1 c R . . H(142) H -0.1563 -0.0250 0.7180 0.036 Uiso 1.00 1 c R . . H(16) H -0.1816 -0.3256 0.7528 0.044 Uiso 1.00 1 c R . . H(17) H -0.3090 -0.4580 0.6985 0.051 Uiso 1.00 1 c R . . H(18) H -0.3683 -0.3873 0.5648 0.045 Uiso 1.00 1 c R . . H(19) H -0.3075 -0.1858 0.4950 0.045 Uiso 1.00 1 c R . . H(201) H 0.4770 -0.0525 0.6781 0.038 Uiso 1.00 1 c R . . H(202) H 0.5151 0.0881 0.6821 0.038 Uiso 1.00 1 c R . . H(211) H 0.5323 -0.0291 0.8122 0.041 Uiso 1.00 1 c R . . H(212) H 0.4019 0.0709 0.8298 0.041 Uiso 1.00 1 c R . . H(23) H 0.5169 -0.2638 0.8313 0.046 Uiso 1.00 1 c R . . H(24) H 0.3854 -0.4385 0.8881 0.052 Uiso 1.00 1 c R . . H(25) H 0.1451 -0.3929 0.9280 0.046 Uiso 1.00 1 c R . . H(26) H 0.0485 -0.1761 0.9109 0.040 Uiso 1.00 1 c R . . H(271) H 0.1485 0.4659 0.6990 0.036 Uiso 1.00 1 c R . . H(272) H 0.0010 0.4416 0.6942 0.036 Uiso 1.00 1 c R . . H(281) H 0.1127 0.3567 0.8408 0.036 Uiso 1.00 1 c R . . H(282) H 0.0140 0.4857 0.8341 0.036 Uiso 1.00 1 c R . . H(30) H -0.2300 0.4779 0.8581 0.039 Uiso 1.00 1 c R . . H(31) H -0.4177 0.3567 0.9088 0.045 Uiso 1.00 1 c R . . H(32) H -0.3774 0.1232 0.9305 0.045 Uiso 1.00 1 c R . . H(33) H -0.1562 0.0253 0.9034 0.039 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) 0.02833(14) 0.02849(14) 0.03177(14) 0.00097(10) -0.00635(11) -0.00407(11) P(1) 0.0258(2) 0.0269(2) 0.0234(2) -0.0043(2) -0.0051(2) -0.0028(2) F(1) 0.0418(8) 0.0384(7) 0.0783(11) 0.0082(6) -0.0162(8) -0.0097(7) F(2) 0.0395(7) 0.0394(7) 0.0580(8) -0.0092(5) -0.0176(6) -0.0143(6) F(3) 0.0408(8) 0.0406(7) 0.0824(11) 0.0069(6) -0.0227(8) -0.0076(7) F(4) 0.0467(8) 0.0468(7) 0.0427(7) -0.0200(6) -0.0116(6) -0.0100(6) F(5) 0.0612(10) 0.0761(11) 0.0306(7) -0.0303(8) -0.0009(7) 0.0049(7) F(6) 0.0614(10) 0.0747(10) 0.0257(6) -0.0206(8) -0.0017(6) -0.0017(7) N(1) 0.0346(10) 0.0398(9) 0.0298(9) -0.0176(8) -0.0116(7) 0.0044(7) N(2) 0.0258(8) 0.0299(8) 0.0241(8) -0.0013(6) -0.0060(6) -0.0034(6) N(3) 0.0272(9) 0.0260(8) 0.0237(8) -0.0028(6) -0.0040(6) -0.0021(6) C(1) 0.0283(10) 0.0287(9) 0.0171(8) -0.0114(7) -0.0036(7) -0.0012(7) C(2) 0.0300(10) 0.0271(9) 0.0184(8) -0.0088(7) -0.0029(7) -0.0018(7) C(3) 0.0249(10) 0.0350(10) 0.0194(8) -0.0103(8) -0.0013(7) -0.0027(8) C(4) 0.0314(10) 0.0316(10) 0.0205(9) -0.0145(8) -0.0031(8) -0.0024(7) C(5) 0.0327(11) 0.0257(9) 0.0199(8) -0.0103(7) -0.0020(8) -0.0008(7) C(6) 0.0276(10) 0.0274(9) 0.0190(8) -0.0089(7) -0.0031(7) 0.0006(7) C(7) 0.0331(11) 0.0290(10) 0.0320(10) -0.0041(8) -0.0106(9) -0.0037(8) C(8) 0.0403(13) 0.0420(12) 0.0384(12) 0.0027(10) -0.0092(10) -0.0145(10) C(9) 0.0350(11) 0.0368(11) 0.0301(10) -0.0178(9) -0.0039(9) -0.0070(9) C(10) 0.067(2) 0.0738(19) 0.0418(14) -0.0523(17) 0.0044(13) -0.0074(13) C(11) 0.0333(11) 0.0307(10) 0.0317(10) -0.0056(8) -0.0094(9) -0.0051(8) C(12) 0.0512(15) 0.0418(12) 0.0377(12) 0.0020(10) -0.0204(11) -0.0032(10) C(13) 0.0282(10) 0.0271(9) 0.0218(9) -0.0109(7) -0.0053(7) -0.0014(7) C(14) 0.0349(11) 0.0340(10) 0.0211(9) -0.0153(8) -0.0046(8) -0.0024(8) C(15) 0.0224(9) 0.0256(9) 0.0239(9) -0.0051(7) -0.0030(7) -0.0041(7) C(16) 0.0457(13) 0.0328(10) 0.0323(11) -0.0135(9) -0.0164(10) 0.0033(9) C(17) 0.0555(15) 0.0279(10) 0.0446(13) -0.0170(10) -0.0185(11) 0.0039(9) C(18) 0.0361(12) 0.0370(11) 0.0392(12) -0.0155(9) -0.0127(9) -0.0062(9) C(19) 0.0333(11) 0.0497(13) 0.0291(10) -0.0190(10) -0.0103(9) 0.0039(9) C(20) 0.0260(10) 0.0403(11) 0.0295(10) -0.0092(8) -0.0025(8) -0.0032(9) C(21) 0.0251(10) 0.0461(12) 0.0319(11) -0.0064(8) -0.0108(8) -0.0052(9) C(22) 0.0263(10) 0.0385(11) 0.0226(9) -0.0016(8) -0.0092(8) -0.0045(8) C(23) 0.0308(11) 0.0461(13) 0.0367(11) 0.0087(9) -0.0121(9) -0.0027(10) C(24) 0.0514(15) 0.0343(11) 0.0454(14) 0.0091(10) -0.0158(11) 0.0005(10) C(25) 0.0465(14) 0.0295(10) 0.0389(12) -0.0054(9) -0.0133(10) 0.0040(9) C(26) 0.0291(11) 0.0374(11) 0.0330(11) -0.0051(8) -0.0069(9) -0.0001(9) C(27) 0.0382(11) 0.0244(9) 0.0269(10) -0.0107(8) -0.0073(8) -0.0012(8) C(28) 0.0383(12) 0.0239(9) 0.0283(10) -0.0067(8) -0.0065(8) -0.0068(8) C(29) 0.0323(10) 0.0256(9) 0.0213(9) -0.0028(7) -0.0060(8) -0.0052(7) C(30) 0.0403(12) 0.0278(10) 0.0294(10) 0.0043(8) -0.0034(9) -0.0035(8) C(31) 0.0291(11) 0.0450(12) 0.0392(12) 0.0057(9) -0.0016(9) -0.0054(10) C(32) 0.0312(12) 0.0435(12) 0.0385(12) -0.0088(9) -0.0014(9) -0.0020(10) C(33) 0.0360(11) 0.0271(9) 0.0336(11) -0.0070(8) -0.0037(9) 0.0008(8) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.7.0' _computing_molecular_graphics ORTEP3 #============================================================================== # 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 Cu(1) N(2) 1.9182(16) ? . . Cu(1) N(3) 1.9176(16) ? . . P(1) F(1) 1.5896(15) ? . . P(1) F(2) 1.5949(17) ? . . P(1) F(3) 1.5907(15) ? . . P(1) F(4) 1.6038(17) ? . . P(1) F(5) 1.5944(14) ? . . P(1) F(6) 1.5928(14) ? . . N(1) C(15) 1.340(2) ? . . N(1) C(19) 1.339(3) ? . . N(2) C(22) 1.350(2) ? . . N(2) C(26) 1.356(2) ? . . N(3) C(29) 1.357(2) ? . . N(3) C(33) 1.360(2) ? . . C(1) C(2) 1.406(2) ? . . C(1) C(6) 1.403(2) ? . . C(1) C(13) 1.515(3) ? . . C(2) C(3) 1.411(3) ? . . C(2) C(7) 1.525(2) ? . . C(3) C(4) 1.410(2) ? . . C(3) C(20) 1.515(3) ? . . C(4) C(5) 1.406(3) ? . . C(4) C(9) 1.524(3) ? . . C(5) C(6) 1.407(3) ? . . C(5) C(27) 1.517(2) ? . . C(6) C(11) 1.523(3) ? . . C(7) C(8) 1.530(3) ? . . C(9) C(10) 1.532(3) ? . . C(11) C(12) 1.531(3) ? . . C(13) C(14) 1.539(2) ? . . C(14) C(15) 1.513(3) ? . . C(15) C(16) 1.381(2) ? . . C(16) C(17) 1.382(3) ? . . C(17) C(18) 1.378(3) ? . . C(18) C(19) 1.372(3) ? . . C(20) C(21) 1.552(3) ? . . C(21) C(22) 1.495(3) ? . . C(22) C(23) 1.395(3) ? . . C(23) C(24) 1.378(3) ? . . C(24) C(25) 1.385(3) ? . . C(25) C(26) 1.376(3) ? . . C(27) C(28) 1.553(2) ? . . C(28) C(29) 1.497(3) ? . . C(29) C(30) 1.390(3) ? . . C(30) C(31) 1.372(3) ? . . C(31) C(32) 1.393(3) ? . . C(32) C(33) 1.352(3) ? . . C(7) H(71) 0.950 ? . . C(7) H(72) 0.950 ? . . C(8) H(81) 0.950 ? . . C(8) H(82) 0.950 ? . . C(8) H(83) 0.950 ? . . C(9) H(92) 0.950 ? . . C(9) H(91) 0.950 ? . . C(10) H(101) 0.950 ? . . C(10) H(102) 0.950 ? . . C(10) H(103) 0.950 ? . . C(11) H(111) 0.950 ? . . C(11) H(112) 0.950 ? . . C(12) H(121) 0.950 ? . . C(12) H(122) 0.950 ? . . C(12) H(123) 0.950 ? . . C(13) H(131) 0.950 ? . . C(13) H(132) 0.950 ? . . C(14) H(141) 0.950 ? . . C(14) H(142) 0.950 ? . . C(16) H(16) 0.950 ? . . C(17) H(17) 0.950 ? . . C(18) H(18) 0.950 ? . . C(19) H(19) 0.950 ? . . C(20) H(201) 0.950 ? . . C(20) H(202) 0.950 ? . . C(21) H(211) 0.950 ? . . C(21) H(212) 0.950 ? . . C(23) H(23) 0.950 ? . . C(24) H(24) 0.950 ? . . C(25) H(25) 0.950 ? . . C(26) H(26) 0.950 ? . . C(27) H(271) 0.950 ? . . C(27) H(272) 0.950 ? . . C(28) H(281) 0.950 ? . . C(28) H(282) 0.950 ? . . C(30) H(30) 0.950 ? . . C(31) H(31) 0.950 ? . . C(32) H(32) 0.950 ? . . C(33) H(33) 0.950 ? . . 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 N(2) Cu(1) N(3) 154.11(7) ? . . . F(1) P(1) F(2) 90.35(8) ? . . . F(1) P(1) F(3) 179.22(8) ? . . . F(1) P(1) F(4) 90.05(8) ? . . . F(1) P(1) F(5) 90.42(9) ? . . . F(1) P(1) F(6) 89.80(8) ? . . . F(2) P(1) F(3) 90.30(8) ? . . . F(2) P(1) F(4) 179.44(7) ? . . . F(2) P(1) F(5) 89.89(9) ? . . . F(2) P(1) F(6) 90.90(9) ? . . . F(3) P(1) F(4) 89.31(8) ? . . . F(3) P(1) F(5) 90.02(9) ? . . . F(3) P(1) F(6) 89.75(8) ? . . . F(4) P(1) F(5) 89.70(9) ? . . . F(4) P(1) F(6) 89.50(8) ? . . . F(5) P(1) F(6) 179.17(10) ? . . . C(15) N(1) C(19) 117.63(18) ? . . . Cu(1) N(2) C(22) 128.50(14) ? . . . Cu(1) N(2) C(26) 113.20(14) ? . . . C(22) N(2) C(26) 118.19(17) ? . . . Cu(1) N(3) C(29) 129.55(14) ? . . . Cu(1) N(3) C(33) 112.84(13) ? . . . C(29) N(3) C(33) 117.61(17) ? . . . C(2) C(1) C(6) 120.6(2) ? . . . C(2) C(1) C(13) 119.64(17) ? . . . C(6) C(1) C(13) 119.79(18) ? . . . C(1) C(2) C(3) 119.58(17) ? . . . C(1) C(2) C(7) 119.6(2) ? . . . C(3) C(2) C(7) 120.79(18) ? . . . C(2) C(3) C(4) 119.79(19) ? . . . C(2) C(3) C(20) 121.31(18) ? . . . C(4) C(3) C(20) 118.8(2) ? . . . C(3) C(4) C(5) 120.2(2) ? . . . C(3) C(4) C(9) 120.03(19) ? . . . C(5) C(4) C(9) 119.66(18) ? . . . C(4) C(5) C(6) 119.86(18) ? . . . C(4) C(5) C(27) 118.9(2) ? . . . C(6) C(5) C(27) 120.95(19) ? . . . C(1) C(6) C(5) 119.85(18) ? . . . C(1) C(6) C(11) 119.9(2) ? . . . C(5) C(6) C(11) 120.25(17) ? . . . C(2) C(7) C(8) 112.19(16) ? . . . C(4) C(9) C(10) 110.9(2) ? . . . C(6) C(11) C(12) 112.14(17) ? . . . C(1) C(13) C(14) 113.17(16) ? . . . C(13) C(14) C(15) 111.95(17) ? . . . N(1) C(15) C(14) 116.57(17) ? . . . N(1) C(15) C(16) 121.9(2) ? . . . C(14) C(15) C(16) 121.5(2) ? . . . C(15) C(16) C(17) 119.7(2) ? . . . C(16) C(17) C(18) 118.6(2) ? . . . C(17) C(18) C(19) 118.4(2) ? . . . N(1) C(19) C(18) 123.8(2) ? . . . C(3) C(20) C(21) 111.55(16) ? . . . C(20) C(21) C(22) 112.8(2) ? . . . N(2) C(22) C(21) 118.95(18) ? . . . N(2) C(22) C(23) 120.25(19) ? . . . C(21) C(22) C(23) 120.76(19) ? . . . C(22) C(23) C(24) 120.9(2) ? . . . C(23) C(24) C(25) 118.8(2) ? . . . C(24) C(25) C(26) 118.0(2) ? . . . N(2) C(26) C(25) 123.9(2) ? . . . C(5) C(27) C(28) 110.54(15) ? . . . C(27) C(28) C(29) 112.78(19) ? . . . N(3) C(29) C(28) 118.97(17) ? . . . N(3) C(29) C(30) 120.38(19) ? . . . C(28) C(29) C(30) 120.62(17) ? . . . C(29) C(30) C(31) 120.9(2) ? . . . C(30) C(31) C(32) 118.4(2) ? . . . C(31) C(32) C(33) 118.4(2) ? . . . N(3) C(33) C(32) 124.2(2) ? . . . C(2) C(7) H(71) 108.7 ? . . . C(2) C(7) H(72) 108.9 ? . . . C(8) C(7) H(71) 108.8 ? . . . C(8) C(7) H(72) 108.8 ? . . . H(71) C(7) H(72) 109.5 ? . . . C(7) C(8) H(81) 109.5 ? . . . C(7) C(8) H(82) 109.6 ? . . . C(7) C(8) H(83) 109.4 ? . . . H(81) C(8) H(82) 109.5 ? . . . H(81) C(8) H(83) 109.5 ? . . . H(82) C(8) H(83) 109.5 ? . . . C(4) C(9) H(92) 108.6 ? . . . C(4) C(9) H(91) 109.6 ? . . . C(10) C(9) H(92) 108.2 ? . . . C(10) C(9) H(91) 110.1 ? . . . H(92) C(9) H(91) 109.5 ? . . . C(9) C(10) H(101) 108.4 ? . . . C(9) C(10) H(102) 110.0 ? . . . C(9) C(10) H(103) 110.0 ? . . . H(101) C(10) H(102) 109.5 ? . . . H(101) C(10) H(103) 109.5 ? . . . H(102) C(10) H(103) 109.5 ? . . . C(6) C(11) H(111) 108.6 ? . . . C(6) C(11) H(112) 108.9 ? . . . C(12) C(11) H(111) 108.6 ? . . . C(12) C(11) H(112) 109.1 ? . . . H(111) C(11) H(112) 109.5 ? . . . C(11) C(12) H(121) 109.2 ? . . . C(11) C(12) H(122) 109.3 ? . . . C(11) C(12) H(123) 109.9 ? . . . H(121) C(12) H(122) 109.5 ? . . . H(121) C(12) H(123) 109.5 ? . . . H(122) C(12) H(123) 109.5 ? . . . C(1) C(13) H(131) 108.6 ? . . . C(1) C(13) H(132) 108.6 ? . . . C(14) C(13) H(131) 108.4 ? . . . C(14) C(13) H(132) 108.5 ? . . . H(131) C(13) H(132) 109.5 ? . . . C(13) C(14) H(141) 108.6 ? . . . C(13) C(14) H(142) 108.8 ? . . . C(15) C(14) H(141) 108.7 ? . . . C(15) C(14) H(142) 109.2 ? . . . H(141) C(14) H(142) 109.5 ? . . . C(15) C(16) H(16) 120.1 ? . . . C(17) C(16) H(16) 120.2 ? . . . C(16) C(17) H(17) 120.5 ? . . . C(18) C(17) H(17) 120.9 ? . . . C(17) C(18) H(18) 120.8 ? . . . C(19) C(18) H(18) 120.9 ? . . . N(1) C(19) H(19) 118.0 ? . . . C(18) C(19) H(19) 118.1 ? . . . C(3) C(20) H(201) 108.7 ? . . . C(3) C(20) H(202) 109.2 ? . . . C(21) C(20) H(201) 108.6 ? . . . C(21) C(20) H(202) 109.4 ? . . . H(201) C(20) H(202) 109.5 ? . . . C(20) C(21) H(211) 108.7 ? . . . C(20) C(21) H(212) 108.6 ? . . . C(22) C(21) H(211) 108.6 ? . . . C(22) C(21) H(212) 108.7 ? . . . H(211) C(21) H(212) 109.5 ? . . . C(22) C(23) H(23) 119.3 ? . . . C(24) C(23) H(23) 119.7 ? . . . C(23) C(24) H(24) 120.7 ? . . . C(25) C(24) H(24) 120.5 ? . . . C(24) C(25) H(25) 120.9 ? . . . C(26) C(25) H(25) 121.1 ? . . . N(2) C(26) H(26) 118.0 ? . . . C(25) C(26) H(26) 118.1 ? . . . C(5) C(27) H(271) 109.1 ? . . . C(5) C(27) H(272) 109.3 ? . . . C(28) C(27) H(271) 109.2 ? . . . C(28) C(27) H(272) 109.2 ? . . . H(271) C(27) H(272) 109.5 ? . . . C(27) C(28) H(281) 108.6 ? . . . C(27) C(28) H(282) 108.8 ? . . . C(29) C(28) H(281) 108.3 ? . . . C(29) C(28) H(282) 108.9 ? . . . H(281) C(28) H(282) 109.5 ? . . . C(29) C(30) H(30) 119.2 ? . . . C(31) C(30) H(30) 119.8 ? . . . C(30) C(31) H(31) 120.7 ? . . . C(32) C(31) H(31) 120.8 ? . . . C(31) C(32) H(32) 121.0 ? . . . C(33) C(32) H(32) 120.6 ? . . . N(3) C(33) H(33) 117.4 ? . . . C(32) C(33) H(33) 118.3 ? . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 N(2) Cu(1) N(3) C(29) 171.07(18) ? . . . . N(2) Cu(1) N(3) C(33) -8.3(2) ? . . . . N(3) Cu(1) N(2) C(22) -178.40(18) ? . . . . N(3) Cu(1) N(2) C(26) 5.5(2) ? . . . . C(15) N(1) C(19) C(18) 1.5(3) ? . . . . C(19) N(1) C(15) C(14) 178.62(17) ? . . . . C(19) N(1) C(15) C(16) -1.1(2) ? . . . . Cu(1) N(2) C(22) C(21) 1.8(3) ? . . . . Cu(1) N(2) C(22) C(23) -176.08(17) ? . . . . Cu(1) N(2) C(26) C(25) 176.9(2) ? . . . . C(22) N(2) C(26) C(25) 0.3(3) ? . . . . C(26) N(2) C(22) C(21) 177.8(2) ? . . . . C(26) N(2) C(22) C(23) -0.1(2) ? . . . . Cu(1) N(3) C(29) C(28) 3.5(3) ? . . . . Cu(1) N(3) C(29) C(30) -178.43(16) ? . . . . Cu(1) N(3) C(33) C(32) 178.8(2) ? . . . . C(29) N(3) C(33) C(32) -0.7(3) ? . . . . C(33) N(3) C(29) C(28) -177.15(19) ? . . . . C(33) N(3) C(29) C(30) 0.9(3) ? . . . . C(2) C(1) C(6) C(5) 2.3(2) ? . . . . C(2) C(1) C(6) C(11) -179.15(16) ? . . . . C(6) C(1) C(2) C(3) -3.9(2) ? . . . . C(6) C(1) C(2) C(7) 178.13(16) ? . . . . C(2) C(1) C(13) C(14) 91.6(2) ? . . . . C(13) C(1) C(2) C(3) 177.21(16) ? . . . . C(13) C(1) C(2) C(7) -0.8(2) ? . . . . C(6) C(1) C(13) C(14) -87.3(2) ? . . . . C(13) C(1) C(6) C(5) -178.75(16) ? . . . . C(13) C(1) C(6) C(11) -0.2(2) ? . . . . C(1) C(2) C(3) C(4) 1.4(2) ? . . . . C(1) C(2) C(3) C(20) 177.31(16) ? . . . . C(1) C(2) C(7) C(8) 88.4(2) ? . . . . C(3) C(2) C(7) C(8) -89.6(2) ? . . . . C(7) C(2) C(3) C(4) 179.38(17) ? . . . . C(7) C(2) C(3) C(20) -4.7(2) ? . . . . C(2) C(3) C(4) C(5) 2.6(2) ? . . . . C(2) C(3) C(4) C(9) -173.18(17) ? . . . . C(2) C(3) C(20) C(21) -99.3(2) ? . . . . C(4) C(3) C(20) C(21) 76.6(2) ? . . . . C(20) C(3) C(4) C(5) -173.43(17) ? . . . . C(20) C(3) C(4) C(9) 10.8(2) ? . . . . C(3) C(4) C(5) C(6) -4.1(2) ? . . . . C(3) C(4) C(5) C(27) 169.55(16) ? . . . . C(3) C(4) C(9) C(10) 90.7(2) ? . . . . C(5) C(4) C(9) C(10) -85.1(2) ? . . . . C(9) C(4) C(5) C(6) 171.64(17) ? . . . . C(9) C(4) C(5) C(27) -14.7(2) ? . . . . C(4) C(5) C(6) C(1) 1.7(2) ? . . . . C(4) C(5) C(6) C(11) -176.84(17) ? . . . . C(4) C(5) C(27) C(28) -75.9(2) ? . . . . C(6) C(5) C(27) C(28) 97.7(2) ? . . . . C(27) C(5) C(6) C(1) -171.86(16) ? . . . . C(27) C(5) C(6) C(11) 9.6(2) ? . . . . C(1) C(6) C(11) C(12) -94.5(2) ? . . . . C(5) C(6) C(11) C(12) 84.0(2) ? . . . . C(1) C(13) C(14) C(15) -175.44(15) ? . . . . C(13) C(14) C(15) N(1) -35.5(2) ? . . . . C(13) C(14) C(15) C(16) 144.24(18) ? . . . . N(1) C(15) C(16) C(17) -0.2(3) ? . . . . C(14) C(15) C(16) C(17) -179.94(17) ? . . . . C(15) C(16) C(17) C(18) 1.2(3) ? . . . . C(16) C(17) C(18) C(19) -0.8(3) ? . . . . C(17) C(18) C(19) N(1) -0.6(3) ? . . . . C(3) C(20) C(21) C(22) 68.5(2) ? . . . . C(20) C(21) C(22) N(2) -84.4(2) ? . . . . C(20) C(21) C(22) C(23) 93.5(2) ? . . . . N(2) C(22) C(23) C(24) -0.2(3) ? . . . . C(21) C(22) C(23) C(24) -178.1(2) ? . . . . C(22) C(23) C(24) C(25) 0.4(4) ? . . . . C(23) C(24) C(25) C(26) -0.2(3) ? . . . . C(24) C(25) C(26) N(2) -0.1(3) ? . . . . C(5) C(27) C(28) C(29) -66.2(2) ? . . . . C(27) C(28) C(29) N(3) 84.3(2) ? . . . . C(27) C(28) C(29) C(30) -93.8(2) ? . . . . N(3) C(29) C(30) C(31) -0.3(3) ? . . . . C(28) C(29) C(30) C(31) 177.7(2) ? . . . . C(29) C(30) C(31) C(32) -0.6(3) ? . . . . C(30) C(31) C(32) C(33) 0.9(3) ? . . . . C(31) C(32) C(33) N(3) -0.2(3) ? . . . . 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 Cu(1) F(4) 2.6887(16) ? . . F(1) F(1) 3.5525(19) ? . 65702 F(1) C(23) 3.526(3) ? . 65702 F(1) C(32) 3.269(2) ? . 65501 F(1) C(32) 3.478(2) ? . 55702 F(2) C(23) 3.124(3) ? . 65702 F(2) C(24) 3.460(3) ? . 65702 F(2) C(30) 3.168(2) ? . 56702 F(2) C(31) 3.533(2) ? . 65501 F(2) C(31) 3.563(3) ? . 56702 F(3) C(25) 3.333(2) ? . 56501 F(3) C(25) 3.543(3) ? . 55702 F(3) C(28) 3.516(3) ? . . F(3) C(30) 3.492(3) ? . 56702 F(4) Cu(1) 2.6887(16) ? . . F(4) N(2) 3.437(2) ? . . F(4) N(3) 3.316(2) ? . . F(4) C(26) 3.354(2) ? . 55702 F(4) C(33) 3.310(2) ? . 55702 F(5) C(9) 3.182(2) ? . . F(5) C(24) 3.507(3) ? . 56501 F(5) C(31) 3.388(3) ? . 65501 F(6) C(14) 3.320(2) ? . 55702 F(6) C(16) 3.245(3) ? . 55702 F(6) C(26) 3.531(3) ? . 55702 F(6) C(33) 3.542(2) ? . 55702 N(1) C(1) 3.569(2) ? . 55602 N(2) F(4) 3.437(2) ? . . N(3) F(4) 3.316(2) ? . . C(1) N(1) 3.569(2) ? . 55602 C(1) C(19) 3.550(2) ? . 55602 C(9) F(5) 3.182(2) ? . . C(14) F(6) 3.320(2) ? . 55702 C(16) F(6) 3.245(3) ? . 55702 C(19) C(1) 3.550(2) ? . 55602 C(23) F(1) 3.526(3) ? . 65702 C(23) F(2) 3.124(3) ? . 65702 C(24) F(2) 3.460(3) ? . 65702 C(24) F(5) 3.507(3) ? . 54501 C(24) C(31) 3.588(3) ? . 55702 C(25) F(3) 3.333(2) ? . 54501 C(25) F(3) 3.543(3) ? . 55702 C(26) F(4) 3.354(2) ? . 55702 C(26) F(6) 3.531(3) ? . 55702 C(28) F(3) 3.516(3) ? . . C(30) F(2) 3.168(2) ? . 56702 C(30) F(3) 3.492(3) ? . 56702 C(31) F(2) 3.533(2) ? . 45501 C(31) F(2) 3.563(3) ? . 56702 C(31) F(5) 3.388(3) ? . 45501 C(31) C(24) 3.588(3) ? . 55702 C(32) F(1) 3.269(2) ? . 45501 C(32) F(1) 3.478(2) ? . 55702 C(33) F(4) 3.310(2) ? . 55702 C(33) F(6) 3.542(2) ? . 55702 P(1) H(26) 3.315 ? . 55702 P(1) H(281) 3.453 ? . . P(1) H(30) 3.485 ? . 56702 P(1) H(31) 3.454 ? . 65501 P(1) H(33) 3.304 ? . 55702 F(1) H(211) 3.070 ? . 65702 F(1) H(212) 3.183 ? . . F(1) H(23) 3.231 ? . 65702 F(1) H(31) 3.222 ? . 65501 F(1) H(32) 2.498 ? . 65501 F(1) H(32) 2.770 ? . 55702 F(1) H(33) 3.014 ? . 55702 F(2) H(16) 3.355 ? . 55702 F(2) H(23) 2.615 ? . 65702 F(2) H(24) 3.028 ? . 56501 F(2) H(24) 3.245 ? . 65702 F(2) H(30) 2.479 ? . 56702 F(2) H(31) 2.777 ? . 65501 F(2) H(31) 3.268 ? . 56702 F(3) H(24) 3.364 ? . 56501 F(3) H(25) 2.529 ? . 56501 F(3) H(25) 2.858 ? . 55702 F(3) H(26) 3.014 ? . 55702 F(3) H(281) 2.898 ? . . F(3) H(282) 3.405 ? . . F(3) H(282) 3.018 ? . 56702 F(3) H(30) 3.000 ? . 56702 F(4) H(212) 3.174 ? . . F(4) H(26) 2.476 ? . 55702 F(4) H(281) 2.940 ? . . F(4) H(33) 2.493 ? . 55702 F(5) H(92) 2.721 ? . . F(5) H(91) 2.816 ? . . F(5) H(212) 2.883 ? . . F(5) H(24) 2.706 ? . 56501 F(5) H(25) 3.392 ? . 56501 F(5) H(281) 2.695 ? . . F(5) H(31) 2.613 ? . 65501 F(5) H(32) 3.295 ? . 65501 F(6) H(141) 2.822 ? . 55702 F(6) H(142) 3.148 ? . 55702 F(6) H(16) 2.506 ? . 55702 F(6) H(211) 3.459 ? . 65702 F(6) H(23) 3.265 ? . 65702 F(6) H(26) 2.696 ? . 55702 F(6) H(282) 3.548 ? . 56702 F(6) H(30) 3.254 ? . 56702 F(6) H(33) 2.664 ? . 55702 N(1) H(81) 3.300 ? . 55602 N(1) H(83) 3.191 ? . 55602 N(1) H(123) 2.894 ? . 55602 N(1) H(131) 3.393 ? . 55602 N(1) H(132) 3.417 ? . 55602 N(1) H(201) 3.232 ? . 45501 N(1) H(202) 3.584 ? . 45501 C(1) H(19) 3.013 ? . 55602 C(2) H(19) 2.920 ? . 55602 C(3) H(19) 2.950 ? . 55602 C(4) H(19) 3.100 ? . 55602 C(5) H(19) 3.263 ? . 55602 C(6) H(19) 3.207 ? . 55602 C(8) H(101) 3.316 ? . 65602 C(8) H(122) 3.334 ? . 55602 C(8) H(18) 3.535 ? . 65501 C(8) H(19) 3.388 ? . 65501 C(8) H(19) 3.423 ? . 55602 C(10) H(82) 3.456 ? . 65602 C(10) H(18) 3.201 ? . 66501 C(10) H(18) 3.388 ? . 55602 C(10) H(19) 3.577 ? . 55602 C(11) H(17) 3.491 ? . 56501 C(12) H(81) 3.283 ? . 55602 C(12) H(121) 3.362 ? . 56602 C(12) H(132) 3.569 ? . 55602 C(12) H(17) 3.538 ? . 56501 C(13) H(131) 3.081 ? . 55602 C(13) H(132) 3.353 ? . 55602 C(15) H(123) 3.275 ? . 55602 C(15) H(201) 3.511 ? . 45501 C(16) H(23) 3.094 ? . 45501 C(16) H(272) 3.175 ? . 54501 C(16) H(30) 3.191 ? . 54501 C(17) H(102) 3.345 ? . 44501 C(17) H(112) 3.343 ? . 54501 C(17) H(121) 3.124 ? . 54501 C(17) H(23) 3.195 ? . 45501 C(17) H(272) 3.272 ? . 54501 C(17) H(30) 3.350 ? . 54501 C(18) H(82) 2.950 ? . 45501 C(18) H(102) 3.135 ? . 44501 C(18) H(103) 3.241 ? . 55602 C(18) H(121) 3.263 ? . 54501 C(18) H(123) 3.456 ? . 55602 C(18) H(201) 3.579 ? . 45501 C(19) H(82) 3.089 ? . 45501 C(19) H(83) 3.482 ? . 45501 C(19) H(83) 3.202 ? . 55602 C(19) H(103) 3.440 ? . 55602 C(19) H(123) 2.957 ? . 55602 C(19) H(201) 3.260 ? . 45501 C(21) H(32) 3.498 ? . 65501 C(25) H(282) 3.337 ? . 54501 C(27) H(16) 3.535 ? . 56501 C(28) H(16) 3.530 ? . 56501 C(28) H(25) 3.368 ? . 56501 C(30) H(16) 3.313 ? . 56501 C(30) H(17) 3.240 ? . 56501 C(30) H(25) 3.514 ? . 55702 C(32) H(211) 3.539 ? . 45501 H(81) N(1) 3.300 ? . 55602 H(81) C(12) 3.283 ? . 55602 H(81) H(101) 3.070 ? . 65602 H(81) H(111) 3.343 ? . 55602 H(81) H(122) 2.516 ? . 55602 H(81) H(123) 3.360 ? . 55602 H(81) H(131) 3.114 ? . 55602 H(81) H(19) 3.577 ? . 55602 H(81) H(202) 3.477 ? . 65602 H(82) C(10) 3.456 ? . 65602 H(82) C(18) 2.950 ? . 65501 H(82) C(19) 3.089 ? . 65501 H(82) H(101) 2.836 ? . 65602 H(82) H(102) 3.365 ? . 54501 H(82) H(103) 3.198 ? . 65602 H(82) H(122) 3.395 ? . 55602 H(82) H(18) 2.617 ? . 65501 H(82) H(19) 2.835 ? . 65501 H(83) N(1) 3.191 ? . 55602 H(83) C(19) 3.482 ? . 65501 H(83) C(19) 3.202 ? . 55602 H(83) H(83) 2.769 ? . 65602 H(83) H(101) 3.553 ? . 65602 H(83) H(19) 3.061 ? . 65501 H(83) H(19) 2.685 ? . 55602 H(83) H(201) 3.452 ? . 65602 H(83) H(202) 3.332 ? . 65602 H(92) F(5) 2.721 ? . . H(92) H(24) 3.365 ? . 56501 H(91) F(5) 2.816 ? . . H(101) C(8) 3.316 ? . 65602 H(101) H(81) 3.070 ? . 65602 H(101) H(82) 2.836 ? . 65602 H(101) H(83) 3.553 ? . 65602 H(101) H(111) 3.564 ? . 65501 H(101) H(122) 3.040 ? . 65501 H(101) H(17) 3.532 ? . 66501 H(101) H(18) 3.215 ? . 66501 H(101) H(18) 3.479 ? . 55602 H(101) H(19) 3.573 ? . 55602 H(102) C(17) 3.345 ? . 66501 H(102) C(18) 3.135 ? . 66501 H(102) H(82) 3.365 ? . 56501 H(102) H(17) 2.896 ? . 66501 H(102) H(18) 2.474 ? . 66501 H(103) C(18) 3.241 ? . 55602 H(103) C(19) 3.440 ? . 55602 H(103) H(82) 3.198 ? . 65602 H(103) H(18) 3.506 ? . 66501 H(103) H(18) 2.544 ? . 55602 H(103) H(19) 2.922 ? . 55602 H(111) H(81) 3.343 ? . 55602 H(111) H(101) 3.564 ? . 45501 H(111) H(202) 3.547 ? . 45501 H(112) C(17) 3.343 ? . 56501 H(112) H(17) 2.744 ? . 56501 H(121) C(12) 3.362 ? . 56602 H(121) C(17) 3.124 ? . 56501 H(121) C(18) 3.263 ? . 56501 H(121) H(121) 2.715 ? . 56602 H(121) H(123) 3.192 ? . 56602 H(121) H(17) 3.091 ? . 56501 H(121) H(18) 3.296 ? . 56501 H(122) C(8) 3.334 ? . 55602 H(122) H(81) 2.516 ? . 55602 H(122) H(82) 3.395 ? . 55602 H(122) H(101) 3.040 ? . 45501 H(122) H(132) 3.310 ? . 55602 H(122) H(17) 3.524 ? . 56501 H(122) H(18) 3.337 ? . 56501 H(123) N(1) 2.894 ? . 55602 H(123) C(15) 3.275 ? . 55602 H(123) C(18) 3.456 ? . 55602 H(123) C(19) 2.957 ? . 55602 H(123) H(81) 3.360 ? . 55602 H(123) H(121) 3.192 ? . 56602 H(123) H(132) 3.018 ? . 55602 H(123) H(19) 3.222 ? . 55602 H(131) N(1) 3.393 ? . 55602 H(131) C(13) 3.081 ? . 55602 H(131) H(81) 3.114 ? . 55602 H(131) H(131) 2.713 ? . 55602 H(131) H(132) 2.590 ? . 55602 H(132) N(1) 3.417 ? . 55602 H(132) C(12) 3.569 ? . 55602 H(132) C(13) 3.353 ? . 55602 H(132) H(122) 3.310 ? . 55602 H(132) H(123) 3.018 ? . 55602 H(132) H(131) 2.590 ? . 55602 H(132) H(132) 3.296 ? . 55602 H(141) F(6) 2.822 ? . 55702 H(142) F(6) 3.148 ? . 55702 H(142) H(202) 3.491 ? . 45501 H(142) H(211) 3.164 ? . 45501 H(16) F(2) 3.355 ? . 55702 H(16) F(6) 2.506 ? . 55702 H(16) C(27) 3.535 ? . 54501 H(16) C(28) 3.530 ? . 54501 H(16) C(30) 3.313 ? . 54501 H(16) H(23) 3.031 ? . 45501 H(16) H(272) 2.938 ? . 54501 H(16) H(282) 2.960 ? . 54501 H(16) H(30) 2.485 ? . 54501 H(17) C(11) 3.491 ? . 54501 H(17) C(12) 3.538 ? . 54501 H(17) C(30) 3.240 ? . 54501 H(17) H(101) 3.532 ? . 44501 H(17) H(102) 2.896 ? . 44501 H(17) H(112) 2.744 ? . 54501 H(17) H(121) 3.091 ? . 54501 H(17) H(122) 3.524 ? . 54501 H(17) H(23) 3.188 ? . 45501 H(17) H(272) 3.132 ? . 54501 H(17) H(30) 2.821 ? . 54501 H(18) C(8) 3.535 ? . 45501 H(18) C(10) 3.201 ? . 44501 H(18) C(10) 3.388 ? . 55602 H(18) H(82) 2.617 ? . 45501 H(18) H(101) 3.215 ? . 44501 H(18) H(101) 3.479 ? . 55602 H(18) H(102) 2.474 ? . 44501 H(18) H(103) 3.506 ? . 44501 H(18) H(103) 2.544 ? . 55602 H(18) H(121) 3.296 ? . 54501 H(18) H(122) 3.337 ? . 54501 H(19) C(1) 3.013 ? . 55602 H(19) C(2) 2.920 ? . 55602 H(19) C(3) 2.950 ? . 55602 H(19) C(4) 3.100 ? . 55602 H(19) C(5) 3.263 ? . 55602 H(19) C(6) 3.207 ? . 55602 H(19) C(8) 3.388 ? . 45501 H(19) C(8) 3.423 ? . 55602 H(19) C(10) 3.577 ? . 55602 H(19) H(81) 3.577 ? . 55602 H(19) H(82) 2.835 ? . 45501 H(19) H(83) 3.061 ? . 45501 H(19) H(83) 2.685 ? . 55602 H(19) H(101) 3.573 ? . 55602 H(19) H(103) 2.922 ? . 55602 H(19) H(123) 3.222 ? . 55602 H(19) H(201) 3.567 ? . 45501 H(201) N(1) 3.232 ? . 65501 H(201) C(15) 3.511 ? . 65501 H(201) C(18) 3.579 ? . 65501 H(201) C(19) 3.260 ? . 65501 H(201) H(83) 3.452 ? . 65602 H(201) H(19) 3.567 ? . 65501 H(202) N(1) 3.584 ? . 65501 H(202) H(81) 3.477 ? . 65602 H(202) H(83) 3.332 ? . 65602 H(202) H(111) 3.547 ? . 65501 H(202) H(142) 3.491 ? . 65501 H(211) F(1) 3.070 ? . 65702 H(211) F(6) 3.459 ? . 65702 H(211) C(32) 3.539 ? . 65501 H(211) H(142) 3.164 ? . 65501 H(211) H(32) 2.961 ? . 65501 H(212) F(1) 3.183 ? . . H(212) F(4) 3.174 ? . . H(212) F(5) 2.883 ? . . H(212) H(32) 3.145 ? . 65501 H(23) F(1) 3.231 ? . 65702 H(23) F(2) 2.615 ? . 65702 H(23) F(6) 3.265 ? . 65702 H(23) C(16) 3.094 ? . 65501 H(23) C(17) 3.195 ? . 65501 H(23) H(16) 3.031 ? . 65501 H(23) H(17) 3.188 ? . 65501 H(23) H(30) 3.472 ? . 64501 H(24) F(2) 3.028 ? . 54501 H(24) F(2) 3.245 ? . 65702 H(24) F(3) 3.364 ? . 54501 H(24) F(5) 2.706 ? . 54501 H(24) H(92) 3.365 ? . 54501 H(24) H(31) 2.727 ? . 64501 H(24) H(31) 3.566 ? . 55702 H(25) F(3) 2.529 ? . 54501 H(25) F(3) 2.858 ? . 55702 H(25) F(5) 3.392 ? . 54501 H(25) C(28) 3.368 ? . 54501 H(25) C(30) 3.514 ? . 55702 H(25) H(281) 3.165 ? . 54501 H(25) H(282) 2.708 ? . 54501 H(26) P(1) 3.315 ? . 55702 H(26) F(3) 3.014 ? . 55702 H(26) F(4) 2.476 ? . 55702 H(26) F(6) 2.696 ? . 55702 H(272) C(16) 3.175 ? . 56501 H(272) C(17) 3.272 ? . 56501 H(272) H(16) 2.938 ? . 56501 H(272) H(17) 3.132 ? . 56501 H(281) P(1) 3.453 ? . . H(281) F(3) 2.898 ? . . H(281) F(4) 2.940 ? . . H(281) F(5) 2.695 ? . . H(281) H(25) 3.165 ? . 56501 H(282) F(3) 3.405 ? . . H(282) F(3) 3.018 ? . 56702 H(282) F(6) 3.548 ? . 56702 H(282) C(25) 3.337 ? . 56501 H(282) H(16) 2.960 ? . 56501 H(282) H(25) 2.708 ? . 56501 H(30) P(1) 3.485 ? . 56702 H(30) F(2) 2.479 ? . 56702 H(30) F(3) 3.000 ? . 56702 H(30) F(6) 3.254 ? . 56702 H(30) C(16) 3.191 ? . 56501 H(30) C(17) 3.350 ? . 56501 H(30) H(16) 2.485 ? . 56501 H(30) H(17) 2.821 ? . 56501 H(30) H(23) 3.472 ? . 46501 H(31) P(1) 3.454 ? . 45501 H(31) F(1) 3.222 ? . 45501 H(31) F(2) 2.777 ? . 45501 H(31) F(2) 3.268 ? . 56702 H(31) F(5) 2.613 ? . 45501 H(31) H(24) 2.727 ? . 46501 H(31) H(24) 3.566 ? . 55702 H(32) F(1) 2.498 ? . 45501 H(32) F(1) 2.770 ? . 55702 H(32) F(5) 3.295 ? . 45501 H(32) C(21) 3.498 ? . 45501 H(32) H(211) 2.961 ? . 45501 H(32) H(212) 3.145 ? . 45501 H(33) P(1) 3.304 ? . 55702 H(33) F(1) 3.014 ? . 55702 H(33) F(4) 2.493 ? . 55702 H(33) F(6) 2.664 ? . 55702 #============================================================================== # 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 #============================================================================== #===END