# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email maekawa@rist.kindai.ac.jp loop_ _publ_author_name 'M. Maekawa' 'T. Tominaga' 'K. Sugimoto' 'T. Okubo' T.Kuroda-Sowa 'M. Munakata' 'S. Kitagawa' data_{[Cu4(Me2bpm)3(C2H4)3(MeCN)](BF4)4_0.33MeOH}n _database_code_depnum_ccdc_archive 'CCDC 866528' #TrackingRef 'Complex-2.cif' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_moiety 'C38 H42 Cu4 N13, 4(B F4), 0.33(C O), 1.32(H)' _chemical_formula_sum 'C38.32 H43.32 B4 Cu4 F16 N13 O0.33' _chemical_formula_weight 1292.74 _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 146 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+2/3, y+1/3, z+1/3' 5 '-y+2/3, x-y+1/3, z+1/3' 6 '-x+y+2/3, -x+1/3, z+1/3' 7 'x+1/3, y+2/3, z+2/3' 8 '-y+1/3, x-y+2/3, z+2/3' 9 '-x+y+1/3, -x+2/3, z+2/3' #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #------------------------------------------------------------------------------ _cell_length_a 14.0511(8) _cell_length_b 14.0511(8) _cell_length_c 22.6054(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3865.1(4) _cell_formula_units_Z 3 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 14763 _cell_measurement_theta_min 3.78 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1966 _exptl_absorpt_coefficient_mu 1.733 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6244 _exptl_absorpt_correction_T_max 0.8458 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 14763 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.98 _diffrn_reflns_theta_max 27.45 _reflns_number_total 3920 _reflns_number_gt 3908 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+5.6213P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.054(15) _refine_ls_number_reflns 3920 _refine_ls_number_parameters 232 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0273 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0723 _refine_ls_wR_factor_gt 0.0722 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.86158(3) 0.70958(3) 0.795808(13) 0.01168(9) Uani 1 1 d . . . Cu2 Cu 0.6667 0.3333 0.63456(2) 0.01071(13) Uani 1 3 d S . . F1 F 0.5014(3) 0.4976(3) 0.89704(11) 0.0449(6) Uani 1 1 d . . . F2 F 0.5316(2) 0.4350(2) 0.80962(12) 0.0335(6) Uani 1 1 d . . . F3 F 0.3796(2) 0.4519(2) 0.82090(13) 0.0352(6) Uani 1 1 d . . . F4 F 0.5491(2) 0.6045(2) 0.81529(14) 0.0367(7) Uani 1 1 d . . . F5 F 0.3333 0.6667 0.55605(14) 0.0229(7) Uani 1 3 d S . . F6 F 0.3996(3) 0.6272(3) 0.63790(10) 0.0349(6) Uani 1 1 d . . . O1 O 0.3333 0.6667 0.2956(10) 0.061(5) Uiso 0.33 3 d SP . . H1O H 0.3422 0.7269 0.3080 0.091 Uiso 0.11 1 calc PR . . C15 C 0.3333 0.6667 0.2345(15) 0.063(8) Uiso 0.33 3 d SP . . H15A H 0.4040 0.7261 0.2200 0.094 Uiso 0.11 1 calc PR . . H15B H 0.2739 0.6778 0.2200 0.094 Uiso 0.11 1 calc PR . . H15C H 0.3222 0.5960 0.2200 0.094 Uiso 0.11 1 calc PR . . N1 N 0.7817(2) 0.9823(2) 0.76472(13) 0.0129(6) Uani 1 1 d . . . N2 N 0.7966(2) 0.8200(2) 0.76928(13) 0.0133(6) Uani 1 1 d . . . N3 N 0.6604(2) 0.4658(2) 0.66730(12) 0.0111(5) Uani 1 1 d . . . N4 N 0.7494(2) 0.6204(2) 0.73254(12) 0.0119(5) Uani 1 1 d . . . N5 N 0.6667 0.3333 0.5487(2) 0.0172(10) Uani 1 3 d S . . C1 C 0.7831(3) 0.6282(4) 0.87218(16) 0.0295(10) Uani 1 1 d . . . H1 H 0.7296 0.6469 0.8892 0.035 Uiso 1 1 calc R . . H2 H 0.7582 0.5488 0.8738 0.035 Uiso 1 1 calc R . . C2 C 0.8893(3) 0.6972(3) 0.88451(15) 0.0211(7) Uani 1 1 d . . . H3 H 0.9344 0.6632 0.8941 0.025 Uiso 1 1 calc R . . H4 H 0.9058 0.7614 0.9096 0.025 Uiso 1 1 calc R . . C3 C 0.8238(3) 0.9213(3) 0.78617(13) 0.0134(6) Uani 1 1 d . . . H5 H 0.8780 0.9538 0.8162 0.016 Uiso 1 1 calc R . . C4 C 0.7168(3) 0.7728(3) 0.72861(16) 0.0121(6) Uani 1 1 d . . . C5 C 0.6647(3) 0.8268(3) 0.70667(13) 0.0137(6) Uani 1 1 d . . . H6 H 0.6051 0.7908 0.6798 0.016 Uiso 1 1 calc R . . C6 C 0.7006(3) 0.9344(3) 0.72441(16) 0.0130(7) Uani 1 1 d . . . C7 C 0.7272(3) 0.5224(3) 0.71303(15) 0.0117(6) Uani 1 1 d . . . H7 H 0.7617 0.4884 0.7332 0.014 Uiso 1 1 calc R . . C8 C 0.6919(3) 0.6638(3) 0.70680(14) 0.0115(6) Uani 1 1 d . . . C9 C 0.6177(3) 0.6100(3) 0.66167(14) 0.0120(6) Uani 1 1 d . . . H8 H 0.5756 0.6395 0.6454 0.014 Uiso 1 1 calc R . . C10 C 0.6061(3) 0.5116(3) 0.64055(14) 0.0119(6) Uani 1 1 d . . . C11 C 0.6540(3) 0.9990(3) 0.69804(17) 0.0187(7) Uani 1 1 d . . . H9 H 0.6905 1.0729 0.7152 0.022 Uiso 1 1 calc R . . H10 H 0.5751 0.9625 0.7064 0.022 Uiso 1 1 calc R . . H11 H 0.6658 1.0041 0.6551 0.022 Uiso 1 1 calc R . . C12 C 0.5367(3) 0.4562(3) 0.58769(13) 0.0149(6) Uani 1 1 d . . . H12 H 0.5380 0.3884 0.5795 0.018 Uiso 1 1 calc R . . H13 H 0.5655 0.5054 0.5534 0.018 Uiso 1 1 calc R . . H14 H 0.4609 0.4386 0.5954 0.018 Uiso 1 1 calc R . . C13 C 0.6667 0.3333 0.4983(3) 0.0230(12) Uani 1 3 d S . . B1 B 0.4912(4) 0.4981(4) 0.83562(18) 0.0253(8) Uani 1 1 d . . . B2 B 0.3333 0.6667 0.6186(2) 0.0138(10) Uani 1 3 d S . . C14 C 0.6455(10) 0.3149(13) 0.4337(3) 0.018(2) Uiso 0.33 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.00995(19) 0.01304(18) 0.01014(14) -0.00066(13) -0.00079(17) 0.00431(17) Cu2 0.01067(18) 0.01067(18) 0.0108(3) 0.000 0.000 0.00534(9) F1 0.0419(17) 0.053(2) 0.0258(12) -0.0034(14) -0.0009(13) 0.0136(13) F2 0.0262(13) 0.0344(15) 0.0433(14) -0.0078(12) -0.0004(11) 0.0176(12) F3 0.0205(12) 0.0400(16) 0.0397(15) -0.0128(12) 0.0044(10) 0.0110(11) F4 0.0310(14) 0.0262(13) 0.0447(16) 0.0002(12) 0.0119(12) 0.0082(11) F5 0.0299(12) 0.0299(12) 0.0089(14) 0.000 0.000 0.0150(6) F6 0.0441(16) 0.0563(18) 0.0250(10) 0.0008(12) -0.0051(12) 0.0406(15) N1 0.0153(15) 0.0117(13) 0.0125(13) -0.0001(10) 0.0001(11) 0.0074(12) N2 0.0135(14) 0.0144(14) 0.0128(13) -0.0006(11) -0.0009(10) 0.0076(12) N3 0.0094(12) 0.0095(12) 0.0142(12) -0.0025(10) -0.0013(10) 0.0045(10) N4 0.0112(13) 0.0124(13) 0.0117(12) 0.0007(10) 0.0000(10) 0.0057(11) N5 0.0171(15) 0.0171(15) 0.018(2) 0.000 0.000 0.0085(7) C1 0.028(2) 0.036(2) 0.0104(17) 0.0066(14) 0.0050(13) 0.0054(18) C2 0.0235(19) 0.027(2) 0.0086(14) 0.0042(14) -0.0040(13) 0.0095(15) C3 0.0140(14) 0.0125(16) 0.0150(13) -0.0018(12) -0.0014(10) 0.0077(13) C4 0.0104(15) 0.0136(16) 0.0124(15) 0.0022(12) 0.0030(12) 0.0061(13) C5 0.0143(15) 0.0145(17) 0.0141(13) -0.0033(13) -0.0038(11) 0.0084(15) C6 0.0136(15) 0.0147(16) 0.0124(16) 0.0006(12) 0.0023(12) 0.0082(13) C7 0.0122(15) 0.0116(14) 0.0117(13) -0.0014(10) -0.0029(11) 0.0063(13) C8 0.0109(15) 0.0110(15) 0.0121(15) -0.0001(12) -0.0026(12) 0.0050(12) C9 0.0125(14) 0.0124(15) 0.0126(14) -0.0019(11) -0.0038(11) 0.0074(12) C10 0.0103(14) 0.0110(15) 0.0116(14) 0.0021(11) 0.0003(11) 0.0032(12) C11 0.0261(19) 0.0159(17) 0.0199(17) -0.0025(13) -0.0058(14) 0.0149(16) C12 0.0133(16) 0.0142(16) 0.0176(13) -0.0030(14) -0.0035(14) 0.0072(12) C13 0.0266(18) 0.0266(18) 0.016(3) 0.000 0.000 0.0133(9) B1 0.020(2) 0.027(2) 0.0242(18) -0.0022(18) 0.0050(18) 0.0078(17) B2 0.0165(16) 0.0165(16) 0.008(2) 0.000 0.000 0.0082(8) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N4 2.031(3) . ? Cu1 N1 2.032(3) 2_765 ? Cu1 C1 2.060(4) . ? Cu1 C2 2.066(3) . ? Cu1 N2 2.240(3) . ? Cu2 N5 1.940(5) . ? Cu2 N3 2.046(3) 3_665 ? Cu2 N3 2.046(3) 2_655 ? Cu2 N3 2.046(3) . ? F1 B1 1.396(5) . ? F2 B1 1.400(5) . ? F3 B1 1.404(5) . ? F4 B1 1.376(6) . ? F5 B2 1.413(6) . ? F6 B2 1.372(3) . ? O1 C15 1.38(4) . ? O1 H1O 0.8400 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? N1 C6 1.348(5) . ? N1 C3 1.351(5) . ? N1 Cu1 2.032(3) 3_675 ? N2 C3 1.331(5) . ? N2 C4 1.341(5) . ? N3 C7 1.354(4) . ? N3 C10 1.361(4) . ? N4 C7 1.326(5) . ? N4 C8 1.362(4) . ? N5 C13 1.140(7) . ? C1 C2 1.340(6) . ? C1 H1 0.9900 . ? C1 H2 0.9900 . ? C2 H3 0.9900 . ? C2 H4 0.9900 . ? C3 H5 0.9500 . ? C4 C5 1.382(5) . ? C4 C8 1.476(5) . ? C5 C6 1.392(5) . ? C5 H6 0.9500 . ? C6 C11 1.484(5) . ? C7 H7 0.9500 . ? C8 C9 1.382(4) . ? C9 C10 1.393(5) . ? C9 H8 0.9500 . ? C10 C12 1.491(4) . ? C11 H9 0.9800 . ? C11 H10 0.9800 . ? C11 H11 0.9800 . ? C12 H12 0.9800 . ? C12 H13 0.9800 . ? C12 H14 0.9800 . ? C13 C14 1.486(9) 2_655 ? C13 C14 1.486(9) 3_665 ? C13 C14 1.486(9) . ? B2 F6 1.372(3) 2_665 ? B2 F6 1.372(3) 3_565 ? C14 C14 0.485(17) 3_665 ? C14 C14 0.485(17) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cu1 N1 113.80(12) . 2_765 ? N4 Cu1 C1 102.28(14) . . ? N1 Cu1 C1 138.30(14) 2_765 . ? N4 Cu1 C2 138.76(14) . . ? N1 Cu1 C2 101.40(14) 2_765 . ? C1 Cu1 C2 37.91(16) . . ? N4 Cu1 N2 77.26(11) . . ? N1 Cu1 N2 99.47(10) 2_765 . ? C1 Cu1 N2 108.54(16) . . ? C2 Cu1 N2 118.50(14) . . ? N5 Cu2 N3 111.21(8) . 3_665 ? N5 Cu2 N3 111.21(8) . 2_655 ? N3 Cu2 N3 107.68(8) 3_665 2_655 ? N5 Cu2 N3 111.21(8) . . ? N3 Cu2 N3 107.68(8) 3_665 . ? N3 Cu2 N3 107.68(8) 2_655 . ? C15 O1 H1O 109.5 . . ? O1 C15 H15A 109.5 . . ? O1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C6 N1 C3 117.0(3) . . ? C6 N1 Cu1 126.1(2) . 3_675 ? C3 N1 Cu1 116.8(2) . 3_675 ? C3 N2 C4 116.6(3) . . ? C3 N2 Cu1 131.7(2) . . ? C4 N2 Cu1 111.8(2) . . ? C7 N3 C10 116.7(3) . . ? C7 N3 Cu2 118.5(2) . . ? C10 N3 Cu2 123.9(2) . . ? C7 N4 C8 116.0(3) . . ? C7 N4 Cu1 125.6(2) . . ? C8 N4 Cu1 118.4(2) . . ? C13 N5 Cu2 180.000(1) . . ? C2 C1 Cu1 71.3(2) . . ? C2 C1 H1 116.5 . . ? Cu1 C1 H1 116.5 . . ? C2 C1 H2 116.5 . . ? Cu1 C1 H2 116.5 . . ? H1 C1 H2 113.5 . . ? C1 C2 Cu1 70.8(2) . . ? C1 C2 H3 116.5 . . ? Cu1 C2 H3 116.5 . . ? C1 C2 H4 116.5 . . ? Cu1 C2 H4 116.5 . . ? H3 C2 H4 113.5 . . ? N2 C3 N1 126.3(3) . . ? N2 C3 H5 116.8 . . ? N1 C3 H5 116.8 . . ? N2 C4 C5 121.1(3) . . ? N2 C4 C8 116.6(3) . . ? C5 C4 C8 122.3(3) . . ? C4 C5 C6 119.2(3) . . ? C4 C5 H6 120.4 . . ? C6 C5 H6 120.4 . . ? N1 C6 C5 119.6(3) . . ? N1 C6 C11 119.2(3) . . ? C5 C6 C11 121.2(3) . . ? N4 C7 N3 126.6(3) . . ? N4 C7 H7 116.7 . . ? N3 C7 H7 116.7 . . ? N4 C8 C9 121.6(3) . . ? N4 C8 C4 115.9(3) . . ? C9 C8 C4 122.5(3) . . ? C8 C9 C10 118.6(3) . . ? C8 C9 H8 120.7 . . ? C10 C9 H8 120.7 . . ? N3 C10 C9 120.1(3) . . ? N3 C10 C12 119.0(3) . . ? C9 C10 C12 120.9(3) . . ? C6 C11 H9 109.5 . . ? C6 C11 H10 109.5 . . ? H9 C11 H10 109.5 . . ? C6 C11 H11 109.5 . . ? H9 C11 H11 109.5 . . ? H10 C11 H11 109.5 . . ? C10 C12 H12 109.5 . . ? C10 C12 H13 109.5 . . ? H12 C12 H13 109.5 . . ? C10 C12 H14 109.5 . . ? H12 C12 H14 109.5 . . ? H13 C12 H14 109.5 . . ? N5 C13 C14 169.1(4) . 2_655 ? N5 C13 C14 169.1(4) . 3_665 ? C14 C13 C14 18.8(6) 2_655 3_665 ? N5 C13 C14 169.1(4) . . ? C14 C13 C14 18.8(6) 2_655 . ? C14 C13 C14 18.8(6) 3_665 . ? F4 B1 F1 109.3(4) . . ? F4 B1 F2 110.0(3) . . ? F1 B1 F2 109.8(4) . . ? F4 B1 F3 109.9(3) . . ? F1 B1 F3 109.1(4) . . ? F2 B1 F3 108.7(4) . . ? F6 B2 F6 110.3(2) 2_665 3_565 ? F6 B2 F6 110.3(2) 2_665 . ? F6 B2 F6 110.3(2) 3_565 . ? F6 B2 F5 108.6(2) 2_665 . ? F6 B2 F5 108.6(2) 3_565 . ? F6 B2 F5 108.6(2) . . ? C14 C14 C14 60.000(17) 3_665 2_655 ? C14 C14 C13 80.6(3) 3_665 . ? C14 C14 C13 80.6(3) 2_655 . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.067 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.075 # Attachment 'Complex-3.cif' #------------------------------------------------------------------------------ data_{[Cu4(Me2bpm)3(C2H4)3(MeOH)0.33](ClO4)4}n _database_code_depnum_ccdc_archive 'CCDC 866529' #TrackingRef 'Complex-3.cif' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_moiety 'C36 H42 Cu4 N12 O0.33, 4(Cl O4), 0.33(C)' _chemical_formula_sum 'C36.33 H42 Cl4 Cu4 N12 O16.33' _chemical_formula_weight 1304.06 _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 146 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+2/3, y+1/3, z+1/3' 5 '-y+2/3, x-y+1/3, z+1/3' 6 '-x+y+2/3, -x+1/3, z+1/3' 7 'x+1/3, y+2/3, z+2/3' 8 '-y+1/3, x-y+2/3, z+2/3' 9 '-x+y+1/3, -x+2/3, z+2/3' #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #------------------------------------------------------------------------------ _cell_length_a 14.448(14) _cell_length_b 14.448(14) _cell_length_c 21.25(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3841(6) _cell_formula_units_Z 3 _cell_measurement_temperature 119(2) _cell_measurement_reflns_used 9878 _cell_measurement_theta_min 3.78 _cell_measurement_theta_max 27.48 _exptl_crystal_description chip _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.700 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976.0 _exptl_absorpt_coefficient_mu 1.926 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7610 _exptl_absorpt_correction_T_max 0.9445 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 119(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 9878 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0530 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.78 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3420 _reflns_number_gt 3070 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+4.0543P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(2) _refine_ls_number_reflns 3420 _refine_ls_number_parameters 214 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1293 _refine_ls_wR_factor_gt 0.1252 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.61500(5) 0.79264(5) 0.59552(3) 0.01676(16) Uani 1 1 d . . . Cu2 Cu 1.0000 1.0000 0.43711(5) 0.0159(2) Uani 1 3 d S . . Cl2 Cl 0.8444(9) 1.1415(8) 0.6548(5) 0.0406(8) Uani 0.289(8) 1 d PU A 1 O6 O 0.9071(17) 1.2618(14) 0.6468(9) 0.0406(8) Uani 0.289(8) 1 d PU A 1 O7 O 0.897(2) 1.1038(16) 0.6143(11) 0.0406(8) Uani 0.289(8) 1 d PU A 1 O8 O 0.8583(15) 1.1137(15) 0.7106(9) 0.0406(8) Uani 0.289(8) 1 d PU A 1 O9 O 0.7160(19) 1.0749(16) 0.6429(11) 0.0406(8) Uani 0.289(8) 1 d PU A 1 Cl1 Cl 0.8283(3) 1.1619(3) 0.64375(19) 0.0406(8) Uani 0.711(8) 1 d PU A 2 O2 O 0.8583(6) 1.2714(5) 0.6268(4) 0.0406(8) Uani 0.711(8) 1 d PU A 2 O3 O 0.8915(8) 1.1288(6) 0.6086(5) 0.0406(8) Uani 0.711(8) 1 d PU A 2 O4 O 0.8470(6) 1.1590(6) 0.7108(4) 0.0406(8) Uani 0.711(8) 1 d PU A 2 O5 O 0.7253(8) 1.0985(6) 0.6295(4) 0.0406(8) Uani 0.711(8) 1 d PU A 2 Cl3 Cl 0.6667 1.3333 0.43387(11) 0.0188(4) Uani 1 3 d S . . O10 O 0.6667 1.3333 0.3677(4) 0.049(2) Uani 1 3 d S . . O11 O 0.7047(4) 1.2638(4) 0.4550(3) 0.0447(13) Uani 1 1 d . . . N1 N 0.5213(4) 0.6385(3) 0.5653(2) 0.0161(9) Uani 1 1 d . . . N2 N 0.5157(4) 0.8628(3) 0.5697(2) 0.0186(10) Uani 1 1 d . . . N3 N 0.8631(3) 0.9952(3) 0.4653(2) 0.0159(9) Uani 1 1 d . . . N4 N 0.7078(4) 0.9043(4) 0.5302(2) 0.0149(9) Uani 1 1 d . . . C1 C 0.6988(6) 0.8626(5) 0.6771(3) 0.0343(14) Uani 1 1 d . . . H1A H 0.7742 0.8796 0.6783 0.041 Uiso 1 1 calc R . . H1B H 0.6873 0.9186 0.6962 0.041 Uiso 1 1 calc R . . C2 C 0.6253(6) 0.7623(6) 0.6889(3) 0.0357(16) Uani 1 1 d . . . H2A H 0.5650 0.7514 0.7161 0.043 Uiso 1 1 calc R . . H2B H 0.6518 0.7125 0.6982 0.043 Uiso 1 1 calc R . . C3 C 0.4206(4) 0.5837(4) 0.5863(3) 0.0193(11) Uani 1 1 d . . . H3 H 0.3993 0.6188 0.6158 0.023 Uiso 1 1 calc R . . C4 C 0.5661(4) 0.9460(4) 0.5303(3) 0.0166(11) Uani 1 1 d . . . C5 C 0.5188(4) 1.0036(4) 0.5100(3) 0.0164(11) Uani 1 1 d . . . H5 H 0.5574 1.0656 0.4847 0.020 Uiso 1 1 calc R . . C6 C 0.5559(4) 0.5874(4) 0.5275(3) 0.0192(11) Uani 1 1 d . . . C7 C 0.8023(4) 0.9244(4) 0.5094(3) 0.0190(11) Uani 1 1 d . . . H7 H 0.8304 0.8838 0.5279 0.023 Uiso 1 1 calc R . . C8 C 0.6720(4) 0.9684(4) 0.5076(3) 0.0146(10) Uani 1 1 d . . . C9 C 0.7302(4) 1.0466(4) 0.4638(3) 0.0175(10) Uani 1 1 d . . . H9 H 0.7055 1.0925 0.4490 0.021 Uiso 1 1 calc R . . C10 C 0.8257(4) 1.0571(4) 0.4415(2) 0.0158(10) Uani 1 1 d . . . C11 C 0.6658(4) 0.6475(5) 0.5024(3) 0.0238(12) Uani 1 1 d . . . H11A H 0.7151 0.6891 0.5363 0.029 Uiso 1 1 calc R . . H11B H 0.6690 0.6960 0.4691 0.029 Uiso 1 1 calc R . . H11C H 0.6862 0.5974 0.4851 0.029 Uiso 1 1 calc R . . C12 C 0.8866(5) 1.1322(5) 0.3904(3) 0.0234(13) Uani 1 1 d . . . H12A H 0.9633 1.1646 0.3988 0.028 Uiso 1 1 calc R . . H12B H 0.8674 1.1883 0.3881 0.028 Uiso 1 1 calc R . . H12C H 0.8695 1.0935 0.3503 0.028 Uiso 1 1 calc R . . C13 C 1.0000 1.0000 0.2797(12) 0.010(4) Uiso 0.33 3 d SP . . O1 O 1.016(3) 0.988(4) 0.3352(13) 0.010(4) Uiso 0.11 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0164(3) 0.0136(3) 0.0184(3) 0.0022(3) 0.0011(3) 0.0061(3) Cu2 0.0134(3) 0.0134(3) 0.0209(6) 0.000 0.000 0.00670(17) Cl2 0.0439(12) 0.0261(14) 0.0408(14) -0.0082(11) 0.0116(10) 0.0092(9) O6 0.0439(12) 0.0261(14) 0.0408(14) -0.0082(11) 0.0116(10) 0.0092(9) O7 0.0439(12) 0.0261(14) 0.0408(14) -0.0082(11) 0.0116(10) 0.0092(9) O8 0.0439(12) 0.0261(14) 0.0408(14) -0.0082(11) 0.0116(10) 0.0092(9) O9 0.0439(12) 0.0261(14) 0.0408(14) -0.0082(11) 0.0116(10) 0.0092(9) Cl1 0.0439(12) 0.0261(14) 0.0408(14) -0.0082(11) 0.0116(10) 0.0092(9) O2 0.0439(12) 0.0261(14) 0.0408(14) -0.0082(11) 0.0116(10) 0.0092(9) O3 0.0439(12) 0.0261(14) 0.0408(14) -0.0082(11) 0.0116(10) 0.0092(9) O4 0.0439(12) 0.0261(14) 0.0408(14) -0.0082(11) 0.0116(10) 0.0092(9) O5 0.0439(12) 0.0261(14) 0.0408(14) -0.0082(11) 0.0116(10) 0.0092(9) Cl3 0.0182(6) 0.0182(6) 0.0201(11) 0.000 0.000 0.0091(3) O10 0.065(4) 0.065(4) 0.017(4) 0.000 0.000 0.032(2) O11 0.047(3) 0.030(3) 0.063(4) 0.011(2) -0.007(3) 0.023(2) N1 0.012(2) 0.012(2) 0.021(2) -0.0003(17) 0.0020(17) 0.0038(18) N2 0.016(2) 0.015(2) 0.027(3) 0.0051(18) 0.0026(19) 0.0095(19) N3 0.013(2) 0.010(2) 0.022(2) -0.0012(17) -0.0001(17) 0.0037(17) N4 0.013(2) 0.012(2) 0.019(2) 0.0036(17) 0.0029(18) 0.0055(18) C1 0.043(4) 0.039(4) 0.021(3) -0.005(3) -0.009(3) 0.021(3) C2 0.033(4) 0.047(4) 0.015(3) 0.011(3) -0.002(3) 0.012(3) C3 0.016(3) 0.012(2) 0.027(3) -0.002(2) -0.001(2) 0.005(2) C4 0.010(2) 0.015(2) 0.025(3) 0.002(2) -0.001(2) 0.007(2) C5 0.016(3) 0.012(2) 0.021(3) 0.005(2) 0.005(2) 0.007(2) C6 0.018(3) 0.013(2) 0.025(3) 0.000(2) 0.001(2) 0.007(2) C7 0.018(3) 0.014(3) 0.026(3) -0.001(2) -0.005(2) 0.009(2) C8 0.011(2) 0.013(2) 0.020(3) -0.0023(19) 0.0002(19) 0.006(2) C9 0.017(3) 0.014(2) 0.023(3) 0.003(2) -0.002(2) 0.009(2) C10 0.011(2) 0.011(2) 0.021(3) 0.002(2) -0.001(2) 0.003(2) C11 0.020(3) 0.018(3) 0.028(3) -0.006(2) 0.003(2) 0.006(2) C12 0.022(3) 0.017(3) 0.028(3) 0.002(2) 0.002(2) 0.007(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N4 2.041(5) . ? Cu1 N1 2.047(5) . ? Cu1 C2 2.053(7) . ? Cu1 C1 2.065(7) . ? Cu1 N2 2.201(5) . ? Cu2 N3 2.035(5) 3_675 ? Cu2 N3 2.035(5) . ? Cu2 N3 2.035(5) 2_765 ? Cu2 O1 2.20(3) 3_675 ? Cu2 O1 2.20(3) . ? Cu2 O1 2.20(3) 2_765 ? Cl2 O8 1.30(2) . ? Cl2 O7 1.43(2) . ? Cl2 O6 1.515(19) . ? Cl2 O9 1.63(3) . ? Cl1 O5 1.335(11) . ? Cl1 O3 1.434(9) . ? Cl1 O4 1.454(9) . ? Cl1 O2 1.461(8) . ? Cl3 O10 1.407(9) . ? Cl3 O11 1.438(5) . ? Cl3 O11 1.438(5) 2_775 ? Cl3 O11 1.438(5) 3_575 ? N1 C3 1.338(7) . ? N1 C6 1.345(7) . ? N2 C3 1.338(7) 2_665 ? N2 C4 1.341(7) . ? N3 C7 1.341(7) . ? N3 C10 1.353(7) . ? N4 C7 1.322(7) . ? N4 C8 1.354(7) . ? C1 C2 1.323(10) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N2 1.338(7) 3_565 ? C3 H3 0.9500 . ? C4 C5 1.385(7) . ? C4 C8 1.477(7) . ? C5 C6 1.404(7) 2_665 ? C5 H5 0.9500 . ? C6 C5 1.404(7) 3_565 ? C6 C11 1.477(8) . ? C7 H7 0.9500 . ? C8 C9 1.379(8) . ? C9 C10 1.394(8) . ? C9 H9 0.9500 . ? C10 C12 1.475(8) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 O1 1.23(4) 2_765 ? C13 O1 1.23(4) . ? C13 O1 1.23(4) 3_675 ? O1 O1 0.63(4) 3_675 ? O1 O1 0.63(4) 2_765 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cu1 N1 117.54(19) . . ? N4 Cu1 C2 137.5(3) . . ? N1 Cu1 C2 98.6(3) . . ? N4 Cu1 C1 101.0(3) . . ? N1 Cu1 C1 134.6(2) . . ? C2 Cu1 C1 37.5(3) . . ? N4 Cu1 N2 77.75(18) . . ? N1 Cu1 N2 101.20(18) . . ? C2 Cu1 N2 118.2(3) . . ? C1 Cu1 N2 109.9(2) . . ? N3 Cu2 N3 111.70(12) 3_675 . ? N3 Cu2 N3 111.70(12) 3_675 2_765 ? N3 Cu2 N3 111.70(12) . 2_765 ? N3 Cu2 O1 115.5(9) 3_675 3_675 ? N3 Cu2 O1 99.1(9) . 3_675 ? N3 Cu2 O1 106.4(13) 2_765 3_675 ? N3 Cu2 O1 106.4(13) 3_675 . ? N3 Cu2 O1 115.5(8) . . ? N3 Cu2 O1 99.1(9) 2_765 . ? O1 Cu2 O1 16.4(11) 3_675 . ? N3 Cu2 O1 99.1(9) 3_675 2_765 ? N3 Cu2 O1 106.4(13) . 2_765 ? N3 Cu2 O1 115.5(8) 2_765 2_765 ? O1 Cu2 O1 16.4(11) 3_675 2_765 ? O1 Cu2 O1 16.4(11) . 2_765 ? O8 Cl2 O7 103.6(14) . . ? O8 Cl2 O6 111.2(13) . . ? O7 Cl2 O6 104.0(12) . . ? O8 Cl2 O9 105.5(12) . . ? O7 Cl2 O9 110.5(13) . . ? O6 Cl2 O9 120.8(13) . . ? O5 Cl1 O3 109.3(6) . . ? O5 Cl1 O4 111.2(5) . . ? O3 Cl1 O4 110.0(5) . . ? O5 Cl1 O2 108.2(6) . . ? O3 Cl1 O2 109.8(5) . . ? O4 Cl1 O2 108.3(5) . . ? O10 Cl3 O11 108.2(3) . . ? O10 Cl3 O11 108.2(3) . 2_775 ? O11 Cl3 O11 110.8(3) . 2_775 ? O10 Cl3 O11 108.2(3) . 3_575 ? O11 Cl3 O11 110.8(3) . 3_575 ? O11 Cl3 O11 110.8(3) 2_775 3_575 ? C3 N1 C6 117.8(5) . . ? C3 N1 Cu1 118.1(4) . . ? C6 N1 Cu1 124.0(4) . . ? C3 N2 C4 116.1(5) 2_665 . ? C3 N2 Cu1 131.4(4) 2_665 . ? C4 N2 Cu1 112.4(3) . . ? C7 N3 C10 116.2(5) . . ? C7 N3 Cu2 119.1(4) . . ? C10 N3 Cu2 124.7(4) . . ? C7 N4 C8 116.0(5) . . ? C7 N4 Cu1 126.7(4) . . ? C8 N4 Cu1 117.2(3) . . ? C2 C1 Cu1 70.8(4) . . ? C2 C1 H1A 116.5 . . ? Cu1 C1 H1A 116.5 . . ? C2 C1 H1B 116.5 . . ? Cu1 C1 H1B 116.5 . . ? H1A C1 H1B 113.5 . . ? C1 C2 Cu1 71.8(4) . . ? C1 C2 H2A 116.4 . . ? Cu1 C2 H2A 116.4 . . ? C1 C2 H2B 116.4 . . ? Cu1 C2 H2B 116.4 . . ? H2A C2 H2B 113.4 . . ? N2 C3 N1 126.3(5) 3_565 . ? N2 C3 H3 116.8 3_565 . ? N1 C3 H3 116.8 . . ? N2 C4 C5 121.6(5) . . ? N2 C4 C8 116.0(5) . . ? C5 C4 C8 122.3(5) . . ? C4 C5 C6 118.6(5) . 2_665 ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 2_665 . ? N1 C6 C5 119.2(5) . 3_565 ? N1 C6 C11 118.6(5) . . ? C5 C6 C11 122.1(5) 3_565 . ? N4 C7 N3 127.6(5) . . ? N4 C7 H7 116.2 . . ? N3 C7 H7 116.2 . . ? N4 C8 C9 120.9(5) . . ? N4 C8 C4 116.3(5) . . ? C9 C8 C4 122.8(5) . . ? C8 C9 C10 119.0(5) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? N3 C10 C9 120.1(5) . . ? N3 C10 C12 118.3(5) . . ? C9 C10 C12 121.6(5) . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O1 C13 O1 29(2) 2_765 . ? O1 C13 O1 29(2) 2_765 3_675 ? O1 C13 O1 29(2) . 3_675 ? O1 O1 O1 60.000(18) 3_675 2_765 ? O1 O1 C13 75.3(10) 3_675 . ? O1 O1 C13 75.3(10) 2_765 . ? O1 O1 Cu2 81.8(5) 3_675 . ? O1 O1 Cu2 81.8(5) 2_765 . ? C13 O1 Cu2 153.4(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Cu1 N1 C3 -136.4(4) . . . . ? C2 Cu1 N1 C3 66.7(5) . . . . ? C1 Cu1 N1 C3 78.6(5) . . . . ? N2 Cu1 N1 C3 -54.5(4) . . . . ? N4 Cu1 N1 C6 46.3(5) . . . . ? C2 Cu1 N1 C6 -110.7(5) . . . . ? C1 Cu1 N1 C6 -98.7(5) . . . . ? N2 Cu1 N1 C6 128.2(4) . . . . ? N4 Cu1 N2 C3 174.6(5) . . . 2_665 ? N1 Cu1 N2 C3 58.5(5) . . . 2_665 ? C2 Cu1 N2 C3 -47.7(6) . . . 2_665 ? C1 Cu1 N2 C3 -88.0(6) . . . 2_665 ? N4 Cu1 N2 C4 -5.3(4) . . . . ? N1 Cu1 N2 C4 -121.4(4) . . . . ? C2 Cu1 N2 C4 132.4(4) . . . . ? C1 Cu1 N2 C4 92.1(4) . . . . ? N3 Cu2 N3 C7 -111.3(3) 3_675 . . . ? N3 Cu2 N3 C7 14.6(5) 2_765 . . . ? O1 Cu2 N3 C7 126.5(12) 3_675 . . . ? O1 Cu2 N3 C7 126.9(13) . . . . ? O1 Cu2 N3 C7 141.6(8) 2_765 . . . ? N3 Cu2 N3 C10 70.7(6) 3_675 . . . ? N3 Cu2 N3 C10 -163.4(4) 2_765 . . . ? O1 Cu2 N3 C10 -51.5(12) 3_675 . . . ? O1 Cu2 N3 C10 -51.1(13) . . . . ? O1 Cu2 N3 C10 -36.4(8) 2_765 . . . ? N1 Cu1 N4 C7 -82.4(5) . . . . ? C2 Cu1 N4 C7 62.6(6) . . . . ? C1 Cu1 N4 C7 73.0(5) . . . . ? N2 Cu1 N4 C7 -178.8(5) . . . . ? N1 Cu1 N4 C8 101.0(4) . . . . ? C2 Cu1 N4 C8 -114.0(5) . . . . ? C1 Cu1 N4 C8 -103.6(4) . . . . ? N2 Cu1 N4 C8 4.6(4) . . . . ? N4 Cu1 C1 C2 -168.4(5) . . . . ? N1 Cu1 C1 C2 -19.7(6) . . . . ? N2 Cu1 C1 C2 110.7(5) . . . . ? N4 Cu1 C2 C1 16.9(7) . . . . ? N1 Cu1 C2 C1 166.0(5) . . . . ? N2 Cu1 C2 C1 -86.3(5) . . . . ? C6 N1 C3 N2 -5.3(9) . . . 3_565 ? Cu1 N1 C3 N2 177.2(4) . . . 3_565 ? C3 N2 C4 C5 2.3(8) 2_665 . . . ? Cu1 N2 C4 C5 -177.9(4) . . . . ? C3 N2 C4 C8 -174.7(5) 2_665 . . . ? Cu1 N2 C4 C8 5.2(6) . . . . ? N2 C4 C5 C6 -4.9(9) . . . 2_665 ? C8 C4 C5 C6 171.9(5) . . . 2_665 ? C3 N1 C6 C5 2.2(8) . . . 3_565 ? Cu1 N1 C6 C5 179.5(4) . . . 3_565 ? C3 N1 C6 C11 178.2(5) . . . . ? Cu1 N1 C6 C11 -4.4(7) . . . . ? C8 N4 C7 N3 -5.4(8) . . . . ? Cu1 N4 C7 N3 178.0(4) . . . . ? C10 N3 C7 N4 3.5(8) . . . . ? Cu2 N3 C7 N4 -174.6(4) . . . . ? C7 N4 C8 C9 2.5(8) . . . . ? Cu1 N4 C8 C9 179.4(4) . . . . ? C7 N4 C8 C4 179.6(5) . . . . ? Cu1 N4 C8 C4 -3.4(6) . . . . ? N2 C4 C8 N4 -1.5(7) . . . . ? C5 C4 C8 N4 -178.5(5) . . . . ? N2 C4 C8 C9 175.6(5) . . . . ? C5 C4 C8 C9 -1.4(9) . . . . ? N4 C8 C9 C10 1.7(8) . . . . ? C4 C8 C9 C10 -175.3(5) . . . . ? C7 N3 C10 C9 1.2(7) . . . . ? Cu2 N3 C10 C9 179.3(4) . . . . ? C7 N3 C10 C12 -176.6(5) . . . . ? Cu2 N3 C10 C12 1.4(7) . . . . ? C8 C9 C10 N3 -3.6(8) . . . . ? C8 C9 C10 C12 174.2(5) . . . . ? O1 C13 O1 O1 62.3(3) 2_765 . . 3_675 ? O1 C13 O1 O1 -62.3(3) 3_675 . . 2_765 ? O1 C13 O1 Cu2 31.13(15) 2_765 . . . ? O1 C13 O1 Cu2 -31.13(17) 3_675 . . . ? N3 Cu2 O1 O1 -126(8) 3_675 . . 3_675 ? N3 Cu2 O1 O1 -1(8) . . . 3_675 ? N3 Cu2 O1 O1 118(7) 2_765 . . 3_675 ? O1 Cu2 O1 O1 -60.69(8) 2_765 . . 3_675 ? N3 Cu2 O1 O1 -65(8) 3_675 . . 2_765 ? N3 Cu2 O1 O1 59(8) . . . 2_765 ? N3 Cu2 O1 O1 179(7) 2_765 . . 2_765 ? O1 Cu2 O1 O1 60.69(11) 3_675 . . 2_765 ? N3 Cu2 O1 C13 -96(8) 3_675 . . . ? N3 Cu2 O1 C13 29(8) . . . . ? N3 Cu2 O1 C13 148(7) 2_765 . . . ? O1 Cu2 O1 C13 30.34(7) 3_675 . . . ? O1 Cu2 O1 C13 -30.34(4) 2_765 . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.355 _refine_diff_density_min -0.712 _refine_diff_density_rms 0.124 # Attachment 'Complex-4.cif' #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_{[Cu4(Me2bpm)3(CO)3(MeCN)](PF6)4_0.33MeCN}n _database_code_depnum_ccdc_archive 'CCDC 866530' #TrackingRef 'Complex-4.cif' _audit_creation_date 2010-12-13T20:40:02-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C37 H30 Cu4 F24 N14 O3 P4' _chemical_formula_weight 1552.79 _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 14.3797(15) _cell_length_b 14.3797(15) _cell_length_c 23.083(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 4133.6(8) _cell_formula_units_Z 3 _cell_measurement_temperature 120(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.871 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2298 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.772 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7183 _exptl_absorpt_correction_T_max 0.9166 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_unetI/netI 0.0604 _diffrn_reflns_number 10806 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 4212 _reflns_number_gt 3882 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+30.4239P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4212 _refine_ls_number_parameters 248 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0639 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1231 _refine_ls_wR_factor_gt 0.1198 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(2) _refine_diff_density_max 1.02 _refine_diff_density_min -0.864 _refine_diff_density_rms 0.112 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0 0 0.29539(5) 0.0135(2) Uani 1 3 d S . . Cu2 Cu 0.38958(5) 0.20108(5) 0.14569(3) 0.01305(15) Uani 1 1 d . . . P1 P 0.15836(14) 0.32551(15) 0.09180(9) 0.0321(4) Uani 1 1 d . . . P2 P 0.3333 0.6667 0.32383(11) 0.0209(5) Uani 1 3 d S . . F1A F 0.1966(8) 0.4328(9) 0.0555(5) 0.0549(16) Uani 0.592(13) 1 d P . . F2A F 0.1193(9) 0.2413(10) 0.1427(5) 0.0549(16) Uani 0.592(13) 1 d P . . F3A F 0.0389(7) 0.3109(9) 0.0895(4) 0.0549(16) Uani 0.592(13) 1 d P . . F4A F 0.1434(8) 0.2614(8) 0.0353(4) 0.0549(16) Uani 0.592(13) 1 d P . . F5A F 0.2795(10) 0.3514(9) 0.0976(6) 0.0549(16) Uani 0.592(13) 1 d P . . F6A F 0.1745(7) 0.3925(8) 0.1525(5) 0.0549(16) Uani 0.592(13) 1 d P . . F1B F 0.1856(12) 0.4015(12) 0.0349(7) 0.057(2) Uani 0.408(13) 1 d P . . F2B F 0.1331(13) 0.2181(13) 0.1296(7) 0.057(2) Uani 0.408(13) 1 d P . . F3B F 0.0339(11) 0.2521(12) 0.0747(6) 0.057(2) Uani 0.408(13) 1 d P . . F4B F 0.1760(12) 0.2445(11) 0.0490(6) 0.057(2) Uani 0.408(13) 1 d P . . F5B F 0.2806(15) 0.3795(13) 0.1055(9) 0.057(2) Uani 0.408(13) 1 d P . . F6B F 0.1467(11) 0.4063(11) 0.1289(7) 0.057(2) Uani 0.408(13) 1 d P . . F7 F 0.2688(5) 0.7023(5) 0.2846(2) 0.0647(16) Uani 1 1 d . . . F8 F 0.3690(6) 0.7688(4) 0.3644(2) 0.0777(19) Uani 1 1 d . . . N1 N 0.2913(4) 0.0901(4) 0.2066(2) 0.0140(9) Uani 1 1 d . . . N2 N 0.1330(3) -0.0037(3) 0.26529(19) 0.0125(9) Uani 1 1 d . . . N3 N 0.4852(3) 0.1353(4) 0.17034(19) 0.0134(9) Uani 1 1 d . . . N4 N 0.6418(4) 0.1200(4) 0.1743(2) 0.0149(9) Uani 1 1 d . . . N6 N 0.6667 0.3333 0.2558(7) 0.078(5) Uani 1 3 d S . . C1 C 0.1915(4) 0.0672(4) 0.2242(2) 0.0130(10) Uani 1 1 d . . . H1 H 0.161 0.1047 0.2057 0.016 Uiso 1 1 calc R . . C2 C 0.1740(4) -0.0604(4) 0.2903(2) 0.0133(10) Uani 1 1 d . . . C3 C 0.2728(5) -0.0465(4) 0.2725(2) 0.0178(11) Uani 1 1 d . . . H3 H 0.3002 -0.0888 0.2886 0.021 Uiso 1 1 calc R . . C4 C 0.3303(4) 0.0304(4) 0.2306(2) 0.0119(10) Uani 1 1 d . . . C5 C 0.1128(4) -0.1366(4) 0.3388(3) 0.0166(11) Uani 1 1 d . . . H5A H 0.0357 -0.1725 0.3304 0.025 Uiso 1 1 calc R . . H5B H 0.1276 -0.0966 0.3752 0.025 Uiso 1 1 calc R . . H5C H 0.1353 -0.1905 0.3423 0.025 Uiso 1 1 calc R . . C6 C 0.5831(4) 0.1616(4) 0.1546(2) 0.0168(11) Uani 1 1 d . . . H6 H 0.6157 0.2163 0.126 0.02 Uiso 1 1 calc R . . C7 C 0.5941(4) 0.0374(4) 0.2119(2) 0.0160(11) Uani 1 1 d . . . C8 C 0.4874(4) 0.0012(4) 0.2293(3) 0.0168(11) Uani 1 1 d . . . H8 H 0.451 -0.0593 0.2541 0.02 Uiso 1 1 calc R . . C9 C 0.4376(5) 0.0545(4) 0.2102(2) 0.0153(11) Uani 1 1 d . . . C10 C 0.6555(5) -0.0105(5) 0.2364(3) 0.0237(13) Uani 1 1 d . . . H10A H 0.6959 -0.0212 0.2055 0.036 Uiso 1 1 calc R . . H10B H 0.6058 -0.0799 0.2542 0.036 Uiso 1 1 calc R . . H10C H 0.7054 0.0377 0.2658 0.036 Uiso 1 1 calc R . . O1 O 0.3099(5) 0.1777(5) 0.0258(2) 0.0476(12) Uani 1 1 d . . . C11 C 0.3403(8) 0.1867(7) 0.0717(3) 0.0476(12) Uani 1 1 d . . . N5 N 0 0 0.3797(4) 0.0378(16) Uani 1 3 d S . . C12 C 0 0 0.4292(5) 0.0378(16) Uani 1 3 d S . . C13 C 0 0 0.4913(5) 0.0378(16) Uani 1 3 d S . . H13A H 0.0302 -0.0436 0.5054 0.057 Uiso 0.33 1 calc PR . . H13B H -0.0738 -0.0302 0.5054 0.057 Uiso 0.33 1 calc PR . . H13C H 0.0436 0.0738 0.5054 0.057 Uiso 0.33 1 calc PR . . C14 C 0.6667 0.3333 0.3035(8) 0.067(5) Uani 1 3 d S . . C15 C 0.6667 0.3333 0.3665(8) 0.071(5) Uani 1 3 d S . . H15A H 0.7081 0.3008 0.3806 0.107 Uiso 0.33 1 calc PR . . H15B H 0.5927 0.2919 0.3806 0.107 Uiso 0.33 1 calc PR . . H15C H 0.6992 0.4073 0.3806 0.107 Uiso 0.33 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0136(4) 0.0136(4) 0.0132(5) 0 0 0.00680(18) Cu2 0.0112(3) 0.0121(3) 0.0145(3) 0.0020(3) -0.0002(3) 0.0049(3) P1 0.0237(9) 0.0355(10) 0.0367(10) 0.0177(8) 0.0107(7) 0.0144(8) P2 0.0248(8) 0.0248(8) 0.0130(12) 0 0 0.0124(4) F1A 0.051(2) 0.071(3) 0.060(3) 0.020(2) 0.0052(19) 0.043(2) F2A 0.051(2) 0.071(3) 0.060(3) 0.020(2) 0.0052(19) 0.043(2) F3A 0.051(2) 0.071(3) 0.060(3) 0.020(2) 0.0052(19) 0.043(2) F4A 0.051(2) 0.071(3) 0.060(3) 0.020(2) 0.0052(19) 0.043(2) F5A 0.051(2) 0.071(3) 0.060(3) 0.020(2) 0.0052(19) 0.043(2) F6A 0.051(2) 0.071(3) 0.060(3) 0.020(2) 0.0052(19) 0.043(2) F1B 0.053(4) 0.056(4) 0.063(4) 0.018(3) 0.006(3) 0.027(3) F2B 0.053(4) 0.056(4) 0.063(4) 0.018(3) 0.006(3) 0.027(3) F3B 0.053(4) 0.056(4) 0.063(4) 0.018(3) 0.006(3) 0.027(3) F4B 0.053(4) 0.056(4) 0.063(4) 0.018(3) 0.006(3) 0.027(3) F5B 0.053(4) 0.056(4) 0.063(4) 0.018(3) 0.006(3) 0.027(3) F6B 0.053(4) 0.056(4) 0.063(4) 0.018(3) 0.006(3) 0.027(3) F7 0.092(4) 0.115(5) 0.036(3) 0.001(3) -0.008(3) 0.089(4) F8 0.129(6) 0.057(3) 0.037(3) -0.027(3) -0.007(3) 0.039(4) N1 0.013(2) 0.014(2) 0.016(2) 0.0015(18) -0.0008(18) 0.0080(19) N2 0.010(2) 0.009(2) 0.015(2) -0.0003(16) 0.0007(17) 0.0013(18) N3 0.009(2) 0.013(2) 0.016(2) 0.0069(17) 0.0002(17) 0.0038(18) N4 0.015(2) 0.011(2) 0.018(2) 0.0009(17) 0.0000(18) 0.0056(19) N6 0.089(8) 0.089(8) 0.058(10) 0 0 0.044(4) C1 0.014(2) 0.012(2) 0.015(3) 0.002(2) -0.002(2) 0.008(2) C2 0.013(2) 0.010(2) 0.015(3) -0.0044(19) -0.0049(19) 0.005(2) C3 0.017(3) 0.015(3) 0.021(3) 0.001(2) -0.001(2) 0.007(2) C4 0.009(2) 0.013(2) 0.013(2) -0.0033(19) -0.0036(19) 0.004(2) C5 0.014(3) 0.013(3) 0.023(3) 0.005(2) -0.001(2) 0.007(2) C6 0.012(3) 0.016(3) 0.019(3) 0.000(2) 0.002(2) 0.004(2) C7 0.016(3) 0.016(3) 0.017(3) -0.001(2) 0.001(2) 0.009(2) C8 0.015(3) 0.012(3) 0.020(3) 0.004(2) 0.000(2) 0.005(2) C9 0.018(3) 0.012(2) 0.015(3) -0.001(2) 0.001(2) 0.007(2) C10 0.021(3) 0.025(3) 0.034(3) 0.015(3) 0.009(3) 0.018(3) O1 0.071(3) 0.059(3) 0.026(2) -0.005(2) -0.011(2) 0.042(3) C11 0.071(3) 0.059(3) 0.026(2) -0.005(2) -0.011(2) 0.042(3) N5 0.047(2) 0.047(2) 0.020(3) 0 0 0.0233(12) C12 0.047(2) 0.047(2) 0.020(3) 0 0 0.0233(12) C13 0.047(2) 0.047(2) 0.020(3) 0 0 0.0233(12) C14 0.082(8) 0.082(8) 0.037(9) 0 0 0.041(4) C15 0.077(8) 0.077(8) 0.060(12) 0 0 0.038(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N5 1.946(10) . ? Cu1 N2 2.060(4) 3 ? Cu1 N2 2.060(4) 2 ? Cu1 N2 2.060(4) . ? Cu2 C11 1.822(8) . ? Cu2 N1 2.066(5) . ? Cu2 N4 2.070(5) 3_665 ? Cu2 N3 2.100(4) . ? P1 F6B 1.518(15) . ? P1 F4A 1.550(10) . ? P1 F5B 1.56(2) . ? P1 F2A 1.576(11) . ? P1 F1A 1.593(10) . ? P1 F5A 1.595(12) . ? P1 F3B 1.607(14) . ? P1 F3A 1.624(9) . ? P1 F1B 1.627(15) . ? P1 F4B 1.641(15) . ? P1 F2B 1.648(15) . ? P1 F6A 1.650(10) . ? P2 F7 1.555(5) . ? P2 F7 1.555(5) 3_565 ? P2 F7 1.555(5) 2_665 ? P2 F8 1.595(5) . ? P2 F8 1.595(5) 2_665 ? P2 F8 1.595(5) 3_565 ? F1A F1B 0.619(17) . ? F2A F2B 0.557(16) . ? F3A F3B 0.881(15) . ? F3A F6B 1.728(18) . ? F4A F4B 0.702(14) . ? F4A F3B 1.765(17) . ? F6A F6B 0.757(13) . ? N1 C4 1.356(7) . ? N1 C1 1.363(7) . ? N2 C1 1.338(7) . ? N2 C2 1.352(7) . ? N3 C6 1.314(7) . ? N3 C9 1.367(7) . ? N4 C6 1.334(7) . ? N4 C7 1.350(7) . ? N4 Cu2 2.070(5) 2_655 ? N6 C14 1.10(2) . ? C2 C3 1.394(8) . ? C2 C5 1.503(7) . ? C3 C4 1.388(7) . ? C4 C9 1.480(7) . ? C7 C8 1.410(8) . ? C7 C10 1.477(8) . ? C8 C9 1.357(8) . ? O1 C11 1.129(9) . ? N5 C12 1.142(15) . ? C12 C13 1.433(16) . ? C14 C15 1.45(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Cu1 N2 109.71(12) . 3 ? N5 Cu1 N2 109.71(12) . 2 ? N2 Cu1 N2 109.23(13) 3 2 ? N5 Cu1 N2 109.71(12) . . ? N2 Cu1 N2 109.23(13) 3 . ? N2 Cu1 N2 109.23(13) 2 . ? C11 Cu2 N1 118.3(3) . . ? C11 Cu2 N4 114.5(3) . 3_665 ? N1 Cu2 N4 115.88(18) . 3_665 ? C11 Cu2 N3 120.6(3) . . ? N1 Cu2 N3 79.44(17) . . ? N4 Cu2 N3 102.75(17) 3_665 . ? F6B P1 F4A 153.5(6) . . ? F6B P1 F5B 91.8(8) . . ? F4A P1 F5B 104.7(7) . . ? F6B P1 F2A 91.9(7) . . ? F4A P1 F2A 106.3(6) . . ? F5B P1 F2A 96.4(8) . . ? F6B P1 F1A 70.9(6) . . ? F4A P1 F1A 90.7(5) . . ? F5B P1 F1A 82.4(7) . . ? F2A P1 F1A 162.6(6) . . ? F6B P1 F5A 107.4(7) . . ? F4A P1 F5A 91.2(6) . . ? F5B P1 F5A 15.9(7) . . ? F2A P1 F5A 92.6(6) . . ? F1A P1 F5A 90.6(6) . . ? F6B P1 F3B 97.4(8) . . ? F4A P1 F3B 68.0(6) . . ? F5B P1 F3B 170.2(8) . . ? F2A P1 F3B 80.0(6) . . ? F1A P1 F3B 103.8(6) . . ? F5A P1 F3B 154.4(7) . . ? F6B P1 F3A 66.6(7) . . ? F4A P1 F3A 94.2(5) . . ? F5B P1 F3A 158.1(7) . . ? F2A P1 F3A 88.7(5) . . ? F1A P1 F3A 86.5(5) . . ? F5A P1 F3A 174.0(6) . . ? F3B P1 F3A 31.6(5) . . ? F6B P1 F1B 91.3(7) . . ? F4A P1 F1B 68.6(6) . . ? F5B P1 F1B 89.8(9) . . ? F2A P1 F1B 172.9(7) . . ? F1A P1 F1B 22.1(6) . . ? F5A P1 F1B 92.5(7) . . ? F3B P1 F1B 93.3(7) . . ? F3A P1 F1B 86.8(6) . . ? F6B P1 F4B 176.4(7) . . ? F4A P1 F4B 25.2(5) . . ? F5B P1 F4B 86.6(8) . . ? F2A P1 F4B 91.5(7) . . ? F1A P1 F4B 105.7(6) . . ? F5A P1 F4B 71.2(7) . . ? F3B P1 F4B 84.4(7) . . ? F3A P1 F4B 114.7(7) . . ? F1B P1 F4B 85.4(7) . . ? F6B P1 F2B 111.2(9) . . ? F4A P1 F2B 89.3(7) . . ? F5B P1 F2B 91.4(8) . . ? F2A P1 F2B 19.7(6) . . ? F1A P1 F2B 173.6(6) . . ? F5A P1 F2B 83.0(7) . . ? F3B P1 F2B 82.1(7) . . ? F3A P1 F2B 99.9(6) . . ? F1B P1 F2B 157.4(9) . . ? F4B P1 F2B 72.1(8) . . ? F6B P1 F6A 27.2(5) . . ? F4A P1 F6A 179.2(5) . . ? F5B P1 F6A 75.1(7) . . ? F2A P1 F6A 73.0(6) . . ? F1A P1 F6A 90.1(5) . . ? F5A P1 F6A 88.5(5) . . ? F3B P1 F6A 112.2(6) . . ? F3A P1 F6A 86.2(5) . . ? F1B P1 F6A 112.1(6) . . ? F4B P1 F6A 154.1(6) . . ? F2B P1 F6A 90.0(7) . . ? F7 P2 F7 89.5(3) . 3_565 ? F7 P2 F7 89.5(3) . 2_665 ? F7 P2 F7 89.5(3) 3_565 2_665 ? F7 P2 F8 90.5(3) . . ? F7 P2 F8 91.0(3) 3_565 . ? F7 P2 F8 179.5(4) 2_665 . ? F7 P2 F8 91.0(3) . 2_665 ? F7 P2 F8 179.5(4) 3_565 2_665 ? F7 P2 F8 90.5(3) 2_665 2_665 ? F8 P2 F8 89.0(3) . 2_665 ? F7 P2 F8 179.5(4) . 3_565 ? F7 P2 F8 90.5(3) 3_565 3_565 ? F7 P2 F8 91.0(3) 2_665 3_565 ? F8 P2 F8 89.0(3) . 3_565 ? F8 P2 F8 89.0(3) 2_665 3_565 ? F1B F1A P1 82(2) . . ? F2B F2A P1 87(2) . . ? F3B F3A P1 73.2(11) . . ? F3B F3A F6B 125.2(14) . . ? P1 F3A F6B 53.8(6) . . ? F4B F4A P1 84.7(17) . . ? F4B F4A F3B 117.8(17) . . ? P1 F4A F3B 57.6(6) . . ? F6B F6A P1 66.6(15) . . ? F1A F1B P1 76(2) . . ? F2A F2B P1 73(2) . . ? F3A F3B P1 75.2(12) . . ? F3A F3B F4A 119.1(14) . . ? P1 F3B F4A 54.5(5) . . ? F4A F4B P1 70.1(16) . . ? F6A F6B P1 86.1(15) . . ? F6A F6B F3A 123.5(17) . . ? P1 F6B F3A 59.6(6) . . ? C4 N1 C1 116.4(5) . . ? C4 N1 Cu2 115.3(3) . . ? C1 N1 Cu2 128.3(3) . . ? C1 N2 C2 117.7(5) . . ? C1 N2 Cu1 117.2(4) . . ? C2 N2 Cu1 124.2(4) . . ? C6 N3 C9 116.1(5) . . ? C6 N3 Cu2 130.1(4) . . ? C9 N3 Cu2 113.8(4) . . ? C6 N4 C7 117.2(5) . . ? C6 N4 Cu2 117.6(4) . 2_655 ? C7 N4 Cu2 125.2(4) . 2_655 ? N2 C1 N1 125.4(5) . . ? N2 C2 C3 120.5(5) . . ? N2 C2 C5 119.0(5) . . ? C3 C2 C5 120.5(5) . . ? C4 C3 C2 118.6(5) . . ? N1 C4 C3 121.2(5) . . ? N1 C4 C9 115.8(5) . . ? C3 C4 C9 122.9(5) . . ? N3 C6 N4 127.1(5) . . ? N4 C7 C8 119.2(5) . . ? N4 C7 C10 119.9(5) . . ? C8 C7 C10 120.8(5) . . ? C9 C8 C7 118.9(5) . . ? C8 C9 N3 121.2(5) . . ? C8 C9 C4 123.2(5) . . ? N3 C9 C4 115.6(5) . . ? O1 C11 Cu2 179.8(9) . . ? C12 N5 Cu1 180.000(2) . . ? N5 C12 C13 180.000(3) . . ? N6 C14 C15 180.000(5) . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF # Attachment 'Complex-5.cif' #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_[Cu4(Me2bpm)4(CO)4](BF4)4_4MeOH _database_code_depnum_ccdc_archive 'CCDC 866531' #TrackingRef 'Complex-5.cif' _audit_creation_date 2010-12-14T21:22:02-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C48 H56 B4 Cu4 F16 N16 O8' _chemical_formula_weight 1586.49 _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I -4 2 d' _symmetry_space_group_name_Hall 'I -4 2bw' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, -z+1/4' '-x, -y, z' '-x, y+1/2, -z+1/4' '-y+1/2, -x, z+3/4' '-y, x, -z' 'y, -x, -z' 'y+1/2, x, z+3/4' 'x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1, -z+3/4' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1, -z+3/4' '-y+1, -x+1/2, z+5/4' '-y+1/2, x+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' 'y+1, x+1/2, z+5/4' _cell_length_a 12.9479(9) _cell_length_b 12.9479(9) _cell_length_c 40.274(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6751.9(8) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9091 _cell_measurement_theta_min 2.2243 _cell_measurement_theta_max 28.2771 _cell_measurement_temperature 120(1) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3200 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.347 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_max 0.817 _exptl_absorpt_correction_T_min 0.772 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 120(1) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_unetI/netI 0.0367 _diffrn_reflns_number 20146 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 53 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 28.28 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _reflns_number_total 4141 _reflns_number_gt 3900 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0764P)^2^+5.4638P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4141 _refine_ls_number_parameters 231 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_gt 0.042 _refine_ls_wR_factor_ref 0.1179 _refine_ls_wR_factor_gt 0.1157 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.005(17) _refine_diff_density_max 1.021 _refine_diff_density_min -0.681 _refine_diff_density_rms 0.08 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.21020(3) 0.30978(3) 0.213649(8) 0.02415(12) Uani 1 1 d . . . F1 F 0.0295(3) 0.5832(3) 0.19285(8) 0.0774(11) Uani 1 1 d . . . F2 F 0.0823(2) 0.4705(2) 0.15369(6) 0.0500(6) Uani 1 1 d . . . B1 B 0 0.5 0.17326(14) 0.0376(13) Uani 1 2 d S . . F3A F 0.4800(5) 0.2554(4) 0.15984(14) 0.0582(8) Uani 0.514(4) 1 d P . . F4A F 0.5907(5) 0.3129(5) 0.12211(13) 0.0582(8) Uani 0.514(4) 1 d P . . F3B F 0.5387(5) 0.3538(5) 0.12677(15) 0.0582(8) Uani 0.486(4) 1 d P . . F4B F 0.4255(5) 0.2305(5) 0.14222(14) 0.0582(8) Uani 0.486(4) 1 d P . . B2 B 0.5082(6) 0.25 0.125 0.0389(13) Uani 1 2 d S . . O1 O 0.1317(3) 0.1972(3) 0.15612(8) 0.0646(8) Uani 1 1 d . . . O2 O 0.4004(8) 0.4617(8) 0.2824(2) 0.081(3) Uani 0.5 1 d P . . H2 H 0.3916 0.4794 0.3018 0.122 Uiso 0.5 1 calc PR . . O3 O 0.4071(10) 0.3853(7) 0.3466(2) 0.093(4) Uani 0.5 1 d P . . H3 H 0.4354 0.4386 0.3528 0.14 Uiso 0.5 1 calc PR . . N1 N 0.1217(2) 0.2817(2) 0.25572(6) 0.0229(5) Uani 1 1 d . . . N2 N 0.3223(2) 0.2522(2) 0.24510(6) 0.0227(5) Uani 1 1 d . . . N3 N 0.4922(2) 0.2065(3) 0.26138(7) 0.0375(7) Uani 1 1 d . . . N4 N -0.0351(2) 0.2596(2) 0.28550(6) 0.0258(5) Uani 1 1 d . . . C1 C 0.4236(3) 0.2419(3) 0.24013(8) 0.0286(7) Uani 1 1 d . . . H1 H 0.4485 0.2618 0.2194 0.034 Uiso 1 1 calc R . . C2 C 0.4567(3) 0.1772(3) 0.29118(8) 0.0357(8) Uani 1 1 d . . . C3 C 0.5341(3) 0.1359(6) 0.31598(12) 0.0723(19) Uani 1 1 d . . . H3A H 0.5729 0.0808 0.306 0.108 Uiso 1 1 calc R . . H3B H 0.4984 0.1105 0.3352 0.108 Uiso 1 1 calc R . . H3C H 0.5803 0.1903 0.3224 0.108 Uiso 1 1 calc R . . C4 C 0.3532(2) 0.1836(3) 0.29909(8) 0.0289(7) Uani 1 1 d . . . H4 H 0.3289 0.163 0.3198 0.035 Uiso 1 1 calc R . . C5 C 0.2868(2) 0.2219(2) 0.27496(7) 0.0214(5) Uani 1 1 d . . . C6 C 0.1727(2) 0.2327(2) 0.28030(7) 0.0220(6) Uani 1 1 d . . . C7 C 0.1226(2) 0.1955(3) 0.30782(7) 0.0283(6) Uani 1 1 d . . . H7 H 0.1586 0.1617 0.3246 0.034 Uiso 1 1 calc R . . C8 C 0.0156(2) 0.2098(3) 0.30997(7) 0.0269(6) Uani 1 1 d . . . C9 C 0.0202(2) 0.2926(3) 0.25949(7) 0.0263(6) Uani 1 1 d . . . H9 H -0.0155 0.3261 0.2426 0.032 Uiso 1 1 calc R . . C10 C -0.0445(3) 0.1718(3) 0.33912(9) 0.0386(9) Uani 1 1 d . . . H10A H -0.0788 0.2289 0.3496 0.058 Uiso 1 1 calc R . . H10B H 0.0015 0.1397 0.3547 0.058 Uiso 1 1 calc R . . H10C H -0.0949 0.1224 0.3318 0.058 Uiso 1 1 calc R . . C11 C 0.1632(5) 0.2414(4) 0.17688(12) 0.0646(8) Uani 1 1 d . . . C12 C 0.5 0.5 0.2708(4) 0.113(4) Uani 1 2 d S . . C13 C 0.3007(15) 0.3795(11) 0.3613(3) 0.090(4) Uani 0.5 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0318(2) 0.02108(18) 0.01955(16) 0.00280(13) 0.00311(14) 0.00230(14) F1 0.078(2) 0.088(2) 0.0663(19) -0.0480(18) -0.0179(17) 0.0244(19) F2 0.0580(16) 0.0566(15) 0.0355(11) -0.0022(11) 0.0106(11) 0.0165(13) B1 0.043(3) 0.047(3) 0.023(2) 0 0 0.011(3) F3A 0.069(2) 0.0542(18) 0.0517(15) -0.0119(13) 0.0215(14) -0.0183(14) F4A 0.069(2) 0.0542(18) 0.0517(15) -0.0119(13) 0.0215(14) -0.0183(14) F3B 0.069(2) 0.0542(18) 0.0517(15) -0.0119(13) 0.0215(14) -0.0183(14) F4B 0.069(2) 0.0542(18) 0.0517(15) -0.0119(13) 0.0215(14) -0.0183(14) B2 0.046(4) 0.034(3) 0.037(3) -0.008(2) 0 0 O1 0.098(2) 0.0582(17) 0.0379(12) -0.0066(11) -0.0193(14) -0.0016(17) O2 0.099(7) 0.080(6) 0.065(5) -0.008(4) -0.026(5) 0.017(5) O3 0.147(10) 0.061(5) 0.072(5) -0.032(4) -0.054(6) 0.024(6) N1 0.0244(12) 0.0234(12) 0.0208(11) 0.0051(9) -0.0008(9) -0.0028(11) N2 0.0234(12) 0.0212(11) 0.0236(12) 0.0024(9) 0.0025(9) -0.0001(10) N3 0.0253(13) 0.056(2) 0.0311(13) 0.0040(14) 0.0047(11) 0.0002(14) N4 0.0218(12) 0.0308(13) 0.0249(11) 0.0094(10) -0.0024(10) -0.0024(10) C1 0.0287(16) 0.0310(16) 0.0262(14) 0.0021(12) 0.0097(12) 0.0005(13) C2 0.0227(15) 0.056(2) 0.0282(15) 0.0052(15) -0.0022(12) -0.0026(15) C3 0.0250(19) 0.143(6) 0.049(2) 0.035(3) -0.0042(18) 0.009(3) C4 0.0243(14) 0.0415(18) 0.0209(12) 0.0044(13) 0.0007(11) -0.0016(14) C5 0.0224(13) 0.0198(12) 0.0219(12) -0.0006(10) -0.0012(11) 0.0009(11) C6 0.0216(14) 0.0203(13) 0.0240(13) 0.0031(10) -0.0011(10) -0.0020(10) C7 0.0228(14) 0.0365(17) 0.0255(13) 0.0132(13) -0.0034(11) -0.0024(14) C8 0.0219(13) 0.0338(17) 0.0251(13) 0.0106(12) -0.0021(10) -0.0029(13) C9 0.0256(14) 0.0319(16) 0.0213(12) 0.0040(12) -0.0034(10) -0.0011(13) C10 0.0248(16) 0.056(2) 0.0349(17) 0.0234(16) 0.0012(14) -0.0031(15) C11 0.098(2) 0.0582(17) 0.0379(12) -0.0066(11) -0.0193(14) -0.0016(17) C12 0.116(10) 0.075(7) 0.150(12) 0 0 -0.041(7) C13 0.121(13) 0.080(8) 0.069(7) -0.004(6) -0.017(8) -0.002(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 C11 1.830(5) . ? Cu1 N4 2.046(3) 14 ? Cu1 N2 2.065(3) . ? Cu1 N1 2.078(2) . ? F1 B1 1.389(4) . ? F2 B1 1.379(4) . ? B1 F2 1.379(4) 3_565 ? B1 F1 1.389(4) 3_565 ? F3A B2 1.451(5) . ? F4A B2 1.349(8) . ? F4A F4A 1.646(12) 2 ? F3B B2 1.403(6) . ? F4B B2 1.300(8) . ? F4B F4B 1.476(12) 2 ? B2 F4B 1.300(8) 2 ? B2 F4A 1.349(8) 2 ? B2 F3B 1.403(6) 2 ? B2 F3A 1.451(5) 2 ? O1 C11 1.092(6) . ? O2 C12 1.460(12) . ? O2 H2 0.82 . ? O3 C13 1.50(2) . ? O3 H3 0.82 . ? N1 C9 1.330(4) . ? N1 C6 1.349(4) . ? N2 C1 1.334(4) . ? N2 C5 1.346(4) . ? N3 C1 1.316(5) . ? N3 C2 1.340(4) . ? N4 C9 1.339(4) . ? N4 C8 1.349(4) . ? N4 Cu1 2.046(3) 15_455 ? C1 H1 0.93 . ? C2 C4 1.379(5) . ? C2 C3 1.513(5) . ? C3 H3A 0.96 . ? C3 H3B 0.96 . ? C3 H3C 0.96 . ? C4 C5 1.389(4) . ? C4 H4 0.93 . ? C5 C6 1.499(4) . ? C6 C7 1.372(4) . ? C7 C8 1.400(4) . ? C7 H7 0.93 . ? C8 C10 1.492(4) . ? C9 H9 0.93 . ? C10 H10A 0.96 . ? C10 H10B 0.96 . ? C10 H10C 0.96 . ? C12 O2 1.460(12) 3_665 ? C13 C13 1.72(4) 12_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Cu1 N4 123.50(19) . 14 ? C11 Cu1 N2 123.8(2) . . ? N4 Cu1 N2 102.09(11) 14 . ? C11 Cu1 N1 113.1(2) . . ? N4 Cu1 N1 105.29(10) 14 . ? N2 Cu1 N1 79.90(10) . . ? F2 B1 F2 110.3(4) 3_565 . ? F2 B1 F1 108.84(19) 3_565 . ? F2 B1 F1 109.0(2) . . ? F2 B1 F1 109.0(2) 3_565 3_565 ? F2 B1 F1 108.84(19) . 3_565 ? F1 B1 F1 110.8(5) . 3_565 ? B2 F4A F4A 52.4(4) . 2 ? B2 F4B F4B 55.4(4) . 2 ? F4B B2 F4B 69.2(7) 2 . ? F4B B2 F4A 119.3(4) 2 . ? F4B B2 F4A 144.6(3) . . ? F4B B2 F4A 144.6(3) 2 2 ? F4B B2 F4A 119.3(4) . 2 ? F4A B2 F4A 75.2(7) . 2 ? F4B B2 F3B 113.0(4) 2 2 ? F4B B2 F3B 94.2(4) . 2 ? F4A B2 F3B 110.6(7) . 2 ? F4A B2 F3B 37.1(3) 2 2 ? F4B B2 F3B 94.2(4) 2 . ? F4B B2 F3B 113.0(4) . . ? F4A B2 F3B 37.1(3) . . ? F4A B2 F3B 110.6(7) 2 . ? F3B B2 F3B 147.3(8) 2 . ? F4B B2 F3A 44.5(4) 2 2 ? F4B B2 F3A 107.5(6) . 2 ? F4A B2 F3A 98.3(4) . 2 ? F4A B2 F3A 104.7(4) 2 2 ? F3B B2 F3A 88.6(3) 2 2 ? F3B B2 F3A 99.5(4) . 2 ? F4B B2 F3A 107.5(6) 2 . ? F4B B2 F3A 44.5(4) . . ? F4A B2 F3A 104.7(4) . . ? F4A B2 F3A 98.3(4) 2 . ? F3B B2 F3A 99.5(4) 2 . ? F3B B2 F3A 88.6(3) . . ? F3A B2 F3A 150.9(8) 2 . ? C12 O2 H2 109.5 . . ? C13 O3 H3 109.5 . . ? C9 N1 C6 116.8(2) . . ? C9 N1 Cu1 128.28(19) . . ? C6 N1 Cu1 114.2(2) . . ? C1 N2 C5 116.1(3) . . ? C1 N2 Cu1 129.5(2) . . ? C5 N2 Cu1 114.4(2) . . ? C1 N3 C2 116.7(3) . . ? C9 N4 C8 117.6(3) . . ? C9 N4 Cu1 118.5(2) . 15_455 ? C8 N4 Cu1 123.9(2) . 15_455 ? N3 C1 N2 127.0(3) . . ? N3 C1 H1 116.5 . . ? N2 C1 H1 116.5 . . ? N3 C2 C4 121.6(3) . . ? N3 C2 C3 117.6(3) . . ? C4 C2 C3 120.8(3) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 C5 117.5(3) . . ? C2 C4 H4 121.3 . . ? C5 C4 H4 121.3 . . ? N2 C5 C4 121.2(3) . . ? N2 C5 C6 115.9(3) . . ? C4 C5 C6 122.9(3) . . ? N1 C6 C7 121.7(3) . . ? N1 C6 C5 114.9(3) . . ? C7 C6 C5 123.3(3) . . ? C6 C7 C8 118.1(3) . . ? C6 C7 H7 120.9 . . ? C8 C7 H7 120.9 . . ? N4 C8 C7 120.0(3) . . ? N4 C8 C10 118.6(3) . . ? C7 C8 C10 121.4(3) . . ? N1 C9 N4 125.7(3) . . ? N1 C9 H9 117.1 . . ? N4 C9 H9 117.1 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O1 C11 Cu1 175.8(6) . . ? O2 C12 O2 142.5(15) . 3_665 ? O3 C13 C13 162.8(15) . 12_545 ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF