# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Masahiko Maekawa' _publ_contact_author_email maekawa@rist.kindai.ac.jp _publ_section_title ; Framework dimensionality of copper(I) coordination polymers of 4,4'-bipyrimidine controlled by anions and solvents ; loop_ _publ_author_name M.Maekawa T.Tominaga K.Sugimoto T.Okubo Kuroda-Sowa Munakata ; S.Kitagawa ; ###END #------------------------------------------------------------------------------ data_{[Cu4(bpm)3(C2H4)3(MeOH)](BF4)4_2H2O_3MeOH}n_Complex-4-CCDC-803344 _database_code_depnum_ccdc_archive 'CCDC 803344' #TrackingRef '- cifs-complexes_1-5.cif' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_moiety 'C31 H33 Cu4 N12 O, 4(B F4), 3(C H3 O), O0.50, 3(O0.50)' _chemical_formula_sum 'C34 H42 B4 Cu4 F16 N12 O6' _chemical_formula_weight 1316.24 #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 63' _symmetry_space_group_name_Hall 'P 6c' _symmetry_Int_Tables_number 173 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 'x, y, z' 2 '-x, -y, z+1/2' 3 '-y, x-y, z' 4 '-x+y, -x, z' 5 'x-y, x, z+1/2' 6 'y, -x+y, z+1/2' #------------------------------------------------------------------------------ _cell_length_a 14.384(5) _cell_length_b 14.384(5) _cell_length_c 15.215(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 120.000(5) _cell_volume 2726.2(16) _cell_formula_units_Z 2 _cell_measurement_temperature 98(2) _cell_measurement_reflns_used 32111 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 27.49 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1316.0 _exptl_absorpt_coefficient_mu 1.645 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9242 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_ambient_temperature 98(2) _diffrn_radiation_wavelength 0.71069 _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 32111 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4171 _reflns_number_gt 4033 _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^)+(0.1304P)^2^+4.0956P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens noref _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0070(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(3) _refine_ls_number_reflns 4171 _refine_ls_number_parameters 216 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0703 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.1941 _refine_ls_wR_factor_gt 0.1917 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.000 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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' #------------------------------------------------------------------------------ # 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 C1 C 0.0828(4) -0.0868(4) 0.1145(4) 0.0287(11) Uani 1 1 d . . . H1 H 0.0535 -0.0668 0.1619 0.034 Uiso 1 1 calc R . . C2 C 0.0636(5) -0.2153(5) 0.0145(5) 0.0358(12) Uani 1 1 d . . . H2 H 0.0230 -0.2842 -0.0116 0.043 Uiso 1 1 calc R . . C3 C 0.1683(5) -0.1440(5) -0.0150(4) 0.0338(12) Uani 1 1 d . . . H3 H 0.2008 -0.1648 -0.0594 0.041 Uiso 1 1 calc R . . C4 C 0.2219(4) -0.0446(5) 0.0217(4) 0.0293(11) Uani 1 1 d . . . C5 C 0.3306(5) 0.0400(4) -0.0084(4) 0.0298(11) Uani 1 1 d . . . C6 C 0.3905(5) 0.0227(5) -0.0701(4) 0.0366(13) Uani 1 1 d . . . H6 H 0.3654 -0.0460 -0.0957 0.044 Uiso 1 1 calc R . . C7 C 0.4892(5) 0.1101(5) -0.0933(4) 0.0372(12) Uani 1 1 d . . . H7 H 0.5314 0.1006 -0.1365 0.045 Uiso 1 1 calc R . . C8 C 0.4649(4) 0.2173(4) 0.0019(4) 0.0276(10) Uani 1 1 d . . . H8 H 0.4904 0.2862 0.0271 0.033 Uiso 1 1 calc R . . C9 C 0.3693(7) 0.1792(8) 0.2389(5) 0.055(2) Uani 1 1 d . . . H9A H 0.3689 0.1161 0.2654 0.066 Uiso 1 1 calc R . . H9B H 0.4409 0.2449 0.2396 0.066 Uiso 1 1 calc R . . C10 C 0.2873(7) 0.1918(8) 0.2577(5) 0.0509(17) Uani 1 1 d . . . H10A H 0.3037 0.2659 0.2707 0.061 Uiso 1 1 calc R . . H10B H 0.2316 0.1370 0.2965 0.061 Uiso 1 1 calc R . . C11 C 0.6667 0.3333 -0.3027(10) 0.063(2) Uani 1 3 d S . . H11 H 0.7364 0.3901 -0.3256 0.108 Uiso 1 1 d . . . B1 B 0.0000 0.0000 0.3728(9) 0.037(2) Uani 1 3 d S . . B2 B 0.5202(11) 0.5094(11) -0.3490(8) 0.088(5) Uani 1 1 d . . . N1 N 0.1800(4) -0.0166(4) 0.0880(3) 0.0275(9) Uani 1 1 d . . . N2 N 0.0213(4) -0.1856(4) 0.0793(3) 0.0307(10) Uani 1 1 d . . . N3 N 0.5270(4) 0.2074(4) -0.0567(3) 0.0295(10) Uani 1 1 d . . . N4 N 0.3693(4) 0.1386(4) 0.0289(3) 0.0262(9) Uani 1 1 d . . . O1 O 0.6667 0.3333 -0.2280(7) 0.063(2) Uani 1 3 d S . . F1 F 0.0000 0.0000 0.2840(5) 0.0472(16) Uani 1 3 d S . . F2 F 0.0458(6) -0.0591(5) 0.4046(5) 0.0852(18) Uani 1 1 d . . . F3A F 0.4439(12) 0.4042(13) -0.3507(10) 0.078(3) Uiso 0.50(2) 1 d P A 1 F4A F 0.5156(13) 0.5453(12) -0.2605(10) 0.078(3) Uiso 0.50(2) 1 d P A 1 F5A F 0.6268(11) 0.5449(11) -0.3630(12) 0.078(3) Uiso 0.50(2) 1 d P A 1 F6A F 0.5214(14) 0.5753(12) -0.4135(10) 0.078(3) Uiso 0.50(2) 1 d P A 1 F3B F 0.4697(12) 0.4004(12) -0.3743(11) 0.081(3) Uiso 0.50(2) 1 d P A 2 F4B F 0.4780(13) 0.5141(13) -0.2586(11) 0.081(3) Uiso 0.50(2) 1 d P A 2 F5B F 0.6254(12) 0.5457(12) -0.3204(12) 0.081(3) Uiso 0.50(2) 1 d P A 2 F6B F 0.4627(14) 0.5583(11) -0.3934(10) 0.081(3) Uiso 0.50(2) 1 d P A 2 Cu1 Cu 0.28031(5) 0.15187(5) 0.12741(5) 0.0303(2) Uani 1 1 d . . . Cu2 Cu 0.6667 0.3333 -0.09956(8) 0.0276(3) Uani 1 3 d S . . O3 O 0.6667 0.3333 0.181(2) 0.094(4) Uani 0.50 3 d SP . . O4 O 0.3125(15) -0.2476(15) -0.0934(13) 0.094(4) Uani 0.50 1 d P . . O2 O 0.6814(7) 0.0682(7) -0.1657(7) 0.092(2) Uani 1 1 d . . . C12 C 0.7796(10) 0.1226(11) -0.2030(10) 0.092(2) Uani 1 1 d . . . H12A H 0.7885 0.1881 -0.2307 0.138 Uiso 1 1 calc R . . H12B H 0.7869 0.0775 -0.2476 0.138 Uiso 1 1 calc R . . H12C H 0.8348 0.1419 -0.1578 0.138 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.025(2) 0.027(2) 0.034(3) -0.001(2) -0.002(2) 0.0123(19) C2 0.030(3) 0.029(3) 0.046(3) -0.004(2) 0.004(2) 0.013(2) C3 0.025(3) 0.031(3) 0.036(3) -0.001(2) 0.003(2) 0.008(2) C4 0.028(2) 0.037(3) 0.025(2) 0.004(2) 0.000(2) 0.017(2) C5 0.030(3) 0.023(2) 0.033(3) -0.002(2) 0.000(2) 0.011(2) C6 0.033(3) 0.029(3) 0.039(3) -0.007(2) 0.003(2) 0.008(2) C7 0.038(3) 0.037(3) 0.035(3) -0.002(3) 0.009(3) 0.017(2) C8 0.026(2) 0.023(2) 0.028(2) 0.000(2) 0.001(2) 0.009(2) C9 0.048(4) 0.088(7) 0.035(4) -0.005(3) -0.010(3) 0.038(4) C10 0.056(4) 0.063(5) 0.030(3) -0.012(3) 0.000(3) 0.027(4) C11 0.072(3) 0.072(3) 0.044(4) 0.000 0.000 0.0359(17) B1 0.039(3) 0.039(3) 0.032(5) 0.000 0.000 0.0195(16) B2 0.080(8) 0.074(7) 0.056(6) 0.027(5) -0.033(5) -0.003(6) N1 0.030(2) 0.028(2) 0.028(2) -0.0010(18) -0.0007(17) 0.0168(19) N2 0.029(2) 0.026(2) 0.037(3) 0.0029(19) -0.0055(19) 0.0134(18) N3 0.028(2) 0.028(2) 0.029(2) 0.0027(18) 0.0018(18) 0.0115(18) N4 0.023(2) 0.026(2) 0.027(2) -0.0010(17) -0.0025(17) 0.0108(17) O1 0.072(3) 0.072(3) 0.044(4) 0.000 0.000 0.0359(17) F1 0.053(2) 0.053(2) 0.036(4) 0.000 0.000 0.0263(12) F2 0.102(4) 0.094(4) 0.082(4) 0.022(4) -0.016(4) 0.066(4) Cu1 0.0299(3) 0.0339(4) 0.0296(3) -0.0038(3) -0.0015(3) 0.0178(3) Cu2 0.0279(4) 0.0279(4) 0.0271(5) 0.000 0.000 0.01394(18) O3 0.099(7) 0.099(7) 0.084(10) 0.000 0.000 0.050(3) O4 0.099(7) 0.099(7) 0.084(10) 0.000 0.000 0.050(3) O2 0.083(4) 0.088(4) 0.104(5) -0.023(4) 0.014(4) 0.042(4) C12 0.083(4) 0.088(4) 0.104(5) -0.023(4) 0.014(4) 0.042(4) _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 C1 N1 1.314(7) . ? C1 N2 1.353(7) . ? C1 H1 0.9500 . ? C2 N2 1.335(8) . ? C2 C3 1.407(8) . ? C2 H2 0.9500 . ? C3 C4 1.360(9) . ? C3 H3 0.9500 . ? C4 N1 1.335(7) . ? C4 C5 1.494(8) . ? C5 N4 1.361(7) . ? C5 C6 1.378(8) . ? C6 C7 1.391(9) . ? C6 H6 0.9500 . ? C7 N3 1.343(8) . ? C7 H7 0.9500 . ? C8 N3 1.319(7) . ? C8 N4 1.336(7) . ? C8 H8 0.9500 . ? C9 C10 1.310(12) . ? C9 Cu1 2.042(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 Cu1 2.052(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 O1 1.14(2) . ? C11 H11 0.987(6) . ? B1 F1 1.351(16) . ? B1 F2 1.397(7) 3 ? B1 F2 1.397(7) . ? B1 F2 1.397(7) 4 ? B2 F3A 1.35(2) . ? B2 F6A 1.359(18) . ? B2 F5A 1.37(2) . ? B2 F5B 1.40(2) . ? B2 F3B 1.41(2) . ? B2 F4A 1.46(2) . ? B2 F6B 1.49(2) . ? B2 F4B 1.52(2) . ? N1 Cu1 2.194(5) . ? N2 Cu1 2.024(5) 4 ? N3 Cu2 2.026(5) . ? N4 Cu1 2.041(5) . ? O1 Cu2 1.954(11) . ? Cu1 N2 2.024(5) 3 ? Cu2 N3 2.026(5) 3_655 ? Cu2 N3 2.026(5) 4_665 ? O2 C12 1.351(15) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? 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 N1 C1 N2 124.9(5) . . ? N1 C1 H1 117.6 . . ? N2 C1 H1 117.6 . . ? N2 C2 C3 119.7(6) . . ? N2 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C4 C3 C2 118.2(6) . . ? C4 C3 H3 120.9 . . ? C2 C3 H3 120.9 . . ? N1 C4 C3 121.5(5) . . ? N1 C4 C5 115.6(5) . . ? C3 C4 C5 122.8(5) . . ? N4 C5 C6 120.3(5) . . ? N4 C5 C4 115.9(5) . . ? C6 C5 C4 123.8(5) . . ? C5 C6 C7 117.2(6) . . ? C5 C6 H6 121.4 . . ? C7 C6 H6 121.4 . . ? N3 C7 C6 122.3(6) . . ? N3 C7 H7 118.8 . . ? C6 C7 H7 118.8 . . ? N3 C8 N4 125.6(5) . . ? N3 C8 H8 117.2 . . ? N4 C8 H8 117.2 . . ? C10 C9 Cu1 71.7(5) . . ? C10 C9 H9A 116.4 . . ? Cu1 C9 H9A 116.4 . . ? C10 C9 H9B 116.4 . . ? Cu1 C9 H9B 116.4 . . ? H9A C9 H9B 113.4 . . ? C9 C10 Cu1 70.9(5) . . ? C9 C10 H10A 116.5 . . ? Cu1 C10 H10A 116.5 . . ? C9 C10 H10B 116.5 . . ? Cu1 C10 H10B 116.5 . . ? H10A C10 H10B 113.5 . . ? O1 C11 H11 110.7(9) . . ? F1 B1 F2 110.3(6) . 3 ? F1 B1 F2 110.3(6) . . ? F2 B1 F2 108.7(7) 3 . ? F1 B1 F2 110.3(6) . 4 ? F2 B1 F2 108.7(7) 3 4 ? F2 B1 F2 108.7(7) . 4 ? F3A B2 F6A 119.1(12) . . ? F3A B2 F5A 123.1(18) . . ? F6A B2 F5A 90.4(13) . . ? F3A B2 F5B 122.9(16) . . ? F6A B2 F5B 109.3(13) . . ? F5A B2 F5B 27.0(7) . . ? F3A B2 F3B 22.3(8) . . ? F6A B2 F3B 113.5(12) . . ? F5A B2 F3B 103.4(16) . . ? F5B B2 F3B 111.1(16) . . ? F3A B2 F4A 105.0(12) . . ? F6A B2 F4A 114.0(16) . . ? F5A B2 F4A 104.6(11) . . ? F5B B2 F4A 79.2(10) . . ? F3B B2 F4A 123.8(12) . . ? F3A B2 F6B 100.8(11) . . ? F6A B2 F6B 32.7(7) . . ? F5A B2 F6B 122.4(13) . . ? F5B B2 F6B 135.8(13) . . ? F3B B2 F6B 107.6(11) . . ? F4A B2 F6B 96.7(15) . . ? F3A B2 F4B 87.0(11) . . ? F6A B2 F4B 119.2(17) . . ? F5A B2 F4B 121.4(11) . . ? F5B B2 F4B 94.8(10) . . ? F3B B2 F4B 107.5(11) . . ? F4A B2 F4B 19.3(8) . . ? F6B B2 F4B 93.5(14) . . ? C1 N1 C4 117.8(5) . . ? C1 N1 Cu1 128.7(4) . . ? C4 N1 Cu1 113.1(4) . . ? C2 N2 C1 117.7(5) . . ? C2 N2 Cu1 123.6(4) . 4 ? C1 N2 Cu1 118.7(4) . 4 ? C8 N3 C7 116.7(5) . . ? C8 N3 Cu2 123.0(4) . . ? C7 N3 Cu2 120.1(4) . . ? C8 N4 C5 117.8(5) . . ? C8 N4 Cu1 125.1(4) . . ? C5 N4 Cu1 117.0(4) . . ? C11 O1 Cu2 180.000(1) . . ? N2 Cu1 N4 110.3(2) 3 . ? N2 Cu1 C9 134.8(3) 3 . ? N4 Cu1 C9 105.4(3) . . ? N2 Cu1 C10 100.9(3) 3 . ? N4 Cu1 C10 142.2(3) . . ? C9 Cu1 C10 37.3(3) . . ? N2 Cu1 N1 97.71(18) 3 . ? N4 Cu1 N1 78.04(18) . . ? C9 Cu1 N1 116.3(3) . . ? C10 Cu1 N1 119.1(3) . . ? O1 Cu2 N3 108.77(14) . 3_655 ? O1 Cu2 N3 108.77(14) . . ? N3 Cu2 N3 110.16(13) 3_655 . ? O1 Cu2 N3 108.77(14) . 4_665 ? N3 Cu2 N3 110.16(13) 3_655 4_665 ? N3 Cu2 N3 110.16(13) . 4_665 ? O2 C12 H12A 109.5 . . ? O2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C2 C3 C4 -2.6(10) . . . . ? C2 C3 C4 N1 4.3(9) . . . . ? C2 C3 C4 C5 -175.9(6) . . . . ? N1 C4 C5 N4 -6.4(7) . . . . ? C3 C4 C5 N4 173.9(6) . . . . ? N1 C4 C5 C6 173.7(6) . . . . ? C3 C4 C5 C6 -6.1(9) . . . . ? N4 C5 C6 C7 -1.6(9) . . . . ? C4 C5 C6 C7 178.3(6) . . . . ? C5 C6 C7 N3 1.2(10) . . . . ? N2 C1 N1 C4 -0.4(8) . . . . ? N2 C1 N1 Cu1 171.7(4) . . . . ? C3 C4 N1 C1 -2.9(8) . . . . ? C5 C4 N1 C1 177.4(5) . . . . ? C3 C4 N1 Cu1 -176.2(5) . . . . ? C5 C4 N1 Cu1 4.1(6) . . . . ? C3 C2 N2 C1 -0.4(9) . . . . ? C3 C2 N2 Cu1 179.8(5) . . . 4 ? N1 C1 N2 C2 2.0(9) . . . . ? N1 C1 N2 Cu1 -178.2(4) . . . 4 ? N4 C8 N3 C7 1.3(8) . . . . ? N4 C8 N3 Cu2 176.0(4) . . . . ? C6 C7 N3 C8 -1.1(9) . . . . ? C6 C7 N3 Cu2 -175.9(5) . . . . ? N3 C8 N4 C5 -1.7(8) . . . . ? N3 C8 N4 Cu1 174.3(4) . . . . ? C6 C5 N4 C8 1.8(8) . . . . ? C4 C5 N4 C8 -178.1(5) . . . . ? C6 C5 N4 Cu1 -174.5(5) . . . . ? C4 C5 N4 Cu1 5.5(6) . . . . ? C8 N4 Cu1 N2 87.5(5) . . . 3 ? C5 N4 Cu1 N2 -96.5(4) . . . 3 ? C8 N4 Cu1 C9 -64.4(6) . . . . ? C5 N4 Cu1 C9 111.7(5) . . . . ? C8 N4 Cu1 C10 -56.1(7) . . . . ? C5 N4 Cu1 C10 119.9(6) . . . . ? C8 N4 Cu1 N1 -178.6(5) . . . . ? C5 N4 Cu1 N1 -2.6(4) . . . . ? C10 C9 Cu1 N2 30.2(8) . . . 3 ? C10 C9 Cu1 N4 171.7(6) . . . . ? C10 C9 Cu1 N1 -104.3(6) . . . . ? C9 C10 Cu1 N2 -158.7(6) . . . 3 ? C9 C10 Cu1 N4 -13.2(9) . . . . ? C9 C10 Cu1 N1 96.1(6) . . . . ? C1 N1 Cu1 N2 -64.1(5) . . . 3 ? C4 N1 Cu1 N2 108.3(4) . . . 3 ? C1 N1 Cu1 N4 -173.4(5) . . . . ? C4 N1 Cu1 N4 -1.0(4) . . . . ? C1 N1 Cu1 C9 85.1(6) . . . . ? C4 N1 Cu1 C9 -102.5(4) . . . . ? C1 N1 Cu1 C10 42.9(6) . . . . ? C4 N1 Cu1 C10 -144.7(4) . . . . ? C11 O1 Cu2 N3 31(100) . . . 3_655 ? C11 O1 Cu2 N3 -89(100) . . . . ? C11 O1 Cu2 N3 151(100) . . . 4_665 ? C8 N3 Cu2 O1 -129.1(4) . . . . ? C7 N3 Cu2 O1 45.3(5) . . . . ? C8 N3 Cu2 N3 111.7(3) . . . 3_655 ? C7 N3 Cu2 N3 -73.8(6) . . . 3_655 ? C8 N3 Cu2 N3 -10.0(5) . . . 4_665 ? C7 N3 Cu2 N3 164.5(4) . . . 4_665 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.237 _refine_diff_density_min -0.722 _refine_diff_density_rms 0.140 ###END #------------------------------------------------------------------------------ data_{[Cu3(bpm)3](SiF6)1.5}n_Complex-5-CCDC803345 _database_code_depnum_ccdc_archive 'CCDC 803345' #TrackingRef '- cifs-complexes_1-5.cif' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C24 H18 Cu3 F9 N12 Si2' _chemical_formula_moiety 'C24 H18 Cu3 F9 N12 Si2' _chemical_formula_weight 892.30 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'I a -3' _symmetry_space_group_name_Hall '-I 2b 2c 3' _symmetry_Int_Tables_number 206 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 'x, y, z' 2 '-x, -y+1/2, z' 3 'x, -y, -z+1/2' 4 '-x, y+1/2, -z+1/2' 5 'y, z, x' 6 '-y, -z+1/2, x' 7 'y, -z, -x+1/2' 8 '-y, z+1/2, -x+1/2' 9 'z, x, y' 10 '-z+1/2, x, -y' 11 '-z, -x+1/2, y' 12 'z+1/2, -x+1/2, -y' 13 'x+1/2, y+1/2, z+1/2' 14 '-x+1/2, -y+1, z+1/2' 15 'x+1/2, -y+1/2, -z+1' 16 '-x+1/2, y+1, -z+1' 17 'y+1/2, z+1/2, x+1/2' 18 '-y+1/2, -z+1, x+1/2' 19 'y+1/2, -z+1/2, -x+1' 20 '-y+1/2, z+1, -x+1' 21 'z+1/2, x+1/2, y+1/2' 22 '-z+1, x+1/2, -y+1/2' 23 '-z+1/2, -x+1, y+1/2' 24 'z+1, -x+1, -y+1/2' 25 '-x, -y, -z' 26 'x, y-1/2, -z' 27 '-x, y, z-1/2' 28 'x, -y-1/2, z-1/2' 29 '-y, -z, -x' 30 'y, z-1/2, -x' 31 '-y, z, x-1/2' 32 'y, -z-1/2, x-1/2' 33 '-z, -x, -y' 34 'z-1/2, -x, y' 35 'z, x-1/2, -y' 36 '-z-1/2, x-1/2, y' 37 '-x+1/2, -y+1/2, -z+1/2' 38 'x+1/2, y, -z+1/2' 39 '-x+1/2, y+1/2, z' 40 'x+1/2, -y, z' 41 '-y+1/2, -z+1/2, -x+1/2' 42 'y+1/2, z, -x+1/2' 43 '-y+1/2, z+1/2, x' 44 'y+1/2, -z, x' 45 '-z+1/2, -x+1/2, -y+1/2' 46 'z, -x+1/2, y+1/2' 47 'z+1/2, x, -y+1/2' 48 '-z, x, y+1/2' #------------------------------------------------------------------------------ _cell_length_a 18.673(3) _cell_length_b 18.673(3) _cell_length_c 18.673(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6510.9(18) _cell_formula_units_Z 8 _cell_measurement_temperature 118(2) _cell_measurement_reflns_used 35743 _cell_measurement_theta_min 3.09 _cell_measurement_theta_max 27.48 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.820 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3536 _exptl_absorpt_coefficient_mu 2.107 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.4862 _exptl_absorpt_correction_T_max 0.7429 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_ambient_temperature 118(2) _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku MercuryCCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 35743 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.0119 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1248 _reflns_number_gt 1247 _reflns_threshold_expression >2\s(I) _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 #------------------------------------------------------------------------------ # REFINEMENT DATA _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^)+(0.0422P)^2^+79.4008P] 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_number_reflns 1248 _refine_ls_number_parameters 94 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0727 _refine_ls_R_factor_gt 0.0726 _refine_ls_wR_factor_ref 0.1729 _refine_ls_wR_factor_gt 0.1728 _refine_ls_goodness_of_fit_ref 1.422 _refine_ls_restrained_S_all 1.419 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.236 _refine_diff_density_min -0.695 _refine_diff_density_rms 0.112 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' Si Si 0.0817 0.0704 'International Tables 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 Cu1 Cu 0.64111(5) 0.5000 0.7500 0.0288(3) Uani 1 2 d S . . Si1 Si 0.5000 0.5000 0.5000 0.0223(7) Uani 1 6 d S . . F1 F 0.58904(17) 0.48748(17) 0.51506(18) 0.0289(8) Uani 1 1 d . . . N1 N 0.5808(3) 0.4169(3) 0.7229(3) 0.0303(11) Uani 1 1 d . . . N2 N 0.7257(2) 0.4760(3) 0.8159(3) 0.0270(10) Uani 1 1 d . . . C1 C 0.5543(3) 0.3797(3) 0.7784(3) 0.0313(13) Uani 1 1 d . . . H1 H 0.5577 0.4010 0.8245 0.038 Uiso 1 1 calc R . . C2 C 0.7913(3) 0.4840(3) 0.7864(3) 0.0293(12) Uani 1 1 d . . . C3 C 0.8524(3) 0.4623(3) 0.8231(4) 0.0346(14) Uani 1 1 d . . . H2 H 0.8989 0.4704 0.8040 0.041 Uiso 1 1 calc R . . C4 C 0.5714(3) 0.3886(3) 0.6571(3) 0.0329(13) Uani 1 1 d . . . H3 H 0.5883 0.4140 0.6164 0.040 Uiso 1 1 calc R . . Si2 Si 0.7500 0.2500 0.7500 0.0190(13) Uani 0.50 6 d SP . . F2 F 0.6992(3) 0.3008(3) 0.8008(3) 0.037(3) Uani 0.50 3 d SP . . F3 F 0.784(3) 0.218(4) 0.8221(17) 0.049(8) Uani 0.17 1 d PU . . F4 F 0.753(4) 0.185(3) 0.807(2) 0.046(9) Uani 0.17 1 d PU . . 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 0.0222(5) 0.0284(5) 0.0357(6) 0.0122(4) 0.000 0.000 Si1 0.0223(7) 0.0223(7) 0.0223(7) 0.0022(8) 0.0022(8) 0.0022(8) F1 0.0244(15) 0.0301(17) 0.0323(18) 0.0040(13) 0.0022(13) 0.0031(13) N1 0.027(2) 0.034(3) 0.030(2) 0.008(2) 0.000(2) -0.002(2) N2 0.021(2) 0.030(2) 0.029(2) 0.0076(19) -0.0005(18) 0.0002(18) C1 0.034(3) 0.032(3) 0.028(3) 0.003(2) 0.000(2) -0.008(2) C2 0.024(3) 0.027(3) 0.036(3) 0.000(2) -0.003(2) 0.001(2) C3 0.024(3) 0.039(3) 0.041(3) 0.000(3) -0.006(2) 0.001(2) C4 0.033(3) 0.039(3) 0.026(3) 0.011(2) 0.005(2) 0.000(3) Si2 0.0190(13) 0.0190(13) 0.0190(13) -0.0009(14) 0.0009(14) 0.0009(14) F2 0.037(3) 0.037(3) 0.037(3) -0.011(3) 0.011(3) 0.011(3) F3 0.034(17) 0.08(3) 0.034(14) 0.009(15) -0.006(12) 0.013(15) F4 0.07(2) 0.05(2) 0.024(13) 0.016(11) 0.009(16) 0.007(12) _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 N1 1.983(5) . ? Cu1 N1 1.983(5) 3_566 ? Cu1 N2 2.052(5) . ? Cu1 N2 2.052(5) 3_566 ? Si1 F1 1.702(3) 29_666 ? Si1 F1 1.702(3) 5 ? Si1 F1 1.702(3) 33_666 ? Si1 F1 1.702(3) 25_666 ? Si1 F1 1.702(3) . ? Si1 F1 1.702(3) 9 ? N1 C1 1.344(7) . ? N1 C4 1.348(8) . ? N2 C1 1.321(7) 23_655 ? N2 C2 1.351(7) . ? C1 N2 1.321(7) 8_646 ? C1 H1 0.9500 . ? C2 C3 1.390(8) . ? C2 C2 1.485(12) 3_566 ? C3 C4 1.387(9) 23_655 ? C3 H2 0.9500 . ? C4 C3 1.387(9) 8_646 ? C4 H3 0.9500 . ? Si2 F3 1.61(3) 35_556 ? Si2 F3 1.61(3) 23_655 ? Si2 F3 1.61(3) 37_656 ? Si2 F3 1.61(3) 44_565 ? Si2 F3 1.61(3) 8_646 ? Si2 F3 1.61(3) . ? Si2 F4 1.63(2) 35_556 ? Si2 F4 1.63(2) 23_655 ? Si2 F4 1.63(2) 44_565 ? Si2 F4 1.63(2) 8_646 ? Si2 F4 1.63(2) 37_656 ? Si2 F4 1.63(2) . ? F3 F4 0.80(3) 35_556 ? F3 F4 0.89(3) . ? F3 F3 1.61(3) 44_565 ? F3 F3 1.61(3) 35_556 ? F4 F3 0.80(3) 44_565 ? F4 F4 1.64(3) 35_556 ? F4 F4 1.64(3) 44_565 ? 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 N1 Cu1 N1 110.8(3) . 3_566 ? N1 Cu1 N2 114.8(2) . . ? N1 Cu1 N2 117.0(2) 3_566 . ? N1 Cu1 N2 117.0(2) . 3_566 ? N1 Cu1 N2 114.8(2) 3_566 3_566 ? N2 Cu1 N2 79.3(3) . 3_566 ? F1 Si1 F1 180.000(1) 29_666 5 ? F1 Si1 F1 89.75(16) 29_666 33_666 ? F1 Si1 F1 90.25(16) 5 33_666 ? F1 Si1 F1 89.75(16) 29_666 25_666 ? F1 Si1 F1 90.25(16) 5 25_666 ? F1 Si1 F1 89.75(16) 33_666 25_666 ? F1 Si1 F1 90.25(16) 29_666 . ? F1 Si1 F1 89.75(16) 5 . ? F1 Si1 F1 90.25(16) 33_666 . ? F1 Si1 F1 180.0(2) 25_666 . ? F1 Si1 F1 90.25(16) 29_666 9 ? F1 Si1 F1 89.75(16) 5 9 ? F1 Si1 F1 180.0(2) 33_666 9 ? F1 Si1 F1 90.25(16) 25_666 9 ? F1 Si1 F1 89.75(16) . 9 ? C1 N1 C4 116.9(5) . . ? C1 N1 Cu1 114.6(4) . . ? C4 N1 Cu1 127.9(4) . . ? C1 N2 C2 117.9(5) 23_655 . ? C1 N2 Cu1 126.1(4) 23_655 . ? C2 N2 Cu1 115.4(4) . . ? N2 C1 N1 125.4(6) 8_646 . ? N2 C1 H1 117.3 8_646 . ? N1 C1 H1 117.3 . . ? N2 C2 C3 120.7(5) . . ? N2 C2 C2 114.7(3) . 3_566 ? C3 C2 C2 124.6(4) . 3_566 ? C4 C3 C2 117.5(6) 23_655 . ? C4 C3 H2 121.2 23_655 . ? C2 C3 H2 121.2 . . ? N1 C4 C3 121.4(5) . 8_646 ? N1 C4 H3 119.3 . . ? C3 C4 H3 119.3 8_646 . ? F3 Si2 F3 180.0(13) 35_556 23_655 ? F3 Si2 F3 119.86(19) 35_556 37_656 ? F3 Si2 F3 60.14(19) 23_655 37_656 ? F3 Si2 F3 119.86(19) 35_556 44_565 ? F3 Si2 F3 60.1(2) 23_655 44_565 ? F3 Si2 F3 119.86(19) 37_656 44_565 ? F3 Si2 F3 60.1(2) 35_556 8_646 ? F3 Si2 F3 119.86(19) 23_655 8_646 ? F3 Si2 F3 60.1(2) 37_656 8_646 ? F3 Si2 F3 180.0(13) 44_565 8_646 ? F3 Si2 F3 60.14(19) 35_556 . ? F3 Si2 F3 119.86(18) 23_655 . ? F3 Si2 F3 180.0(12) 37_656 . ? F3 Si2 F3 60.14(19) 44_565 . ? F3 Si2 F3 119.9(2) 8_646 . ? F3 Si2 F4 148.0(12) 23_655 35_556 ? F3 Si2 F4 151.3(12) 37_656 35_556 ? F3 Si2 F4 88.8(11) 44_565 35_556 ? F3 Si2 F4 91.2(11) 8_646 35_556 ? F3 Si2 F4 148.0(12) 35_556 23_655 ? F3 Si2 F4 91.2(11) 44_565 23_655 ? F3 Si2 F4 88.8(11) 8_646 23_655 ? F3 Si2 F4 151.3(12) . 23_655 ? F4 Si2 F4 180.000(13) 35_556 23_655 ? F3 Si2 F4 151.3(12) 35_556 44_565 ? F3 Si2 F4 88.8(11) 37_656 44_565 ? F3 Si2 F4 148.0(12) 8_646 44_565 ? F3 Si2 F4 91.2(11) . 44_565 ? F4 Si2 F4 119.4(3) 35_556 44_565 ? F4 Si2 F4 60.6(3) 23_655 44_565 ? F3 Si2 F4 151.3(12) 23_655 8_646 ? F3 Si2 F4 91.2(11) 37_656 8_646 ? F3 Si2 F4 148.0(12) 44_565 8_646 ? F3 Si2 F4 88.8(11) . 8_646 ? F4 Si2 F4 60.6(3) 35_556 8_646 ? F4 Si2 F4 119.4(3) 23_655 8_646 ? F4 Si2 F4 180.0(17) 44_565 8_646 ? F3 Si2 F4 88.8(11) 35_556 37_656 ? F3 Si2 F4 91.2(11) 23_655 37_656 ? F3 Si2 F4 151.3(12) 44_565 37_656 ? F3 Si2 F4 148.0(12) . 37_656 ? F4 Si2 F4 119.4(3) 35_556 37_656 ? F4 Si2 F4 60.6(3) 23_655 37_656 ? F4 Si2 F4 119.4(3) 44_565 37_656 ? F4 Si2 F4 60.6(3) 8_646 37_656 ? F3 Si2 F4 91.2(11) 35_556 . ? F3 Si2 F4 88.8(11) 23_655 . ? F3 Si2 F4 148.0(12) 37_656 . ? F3 Si2 F4 151.3(12) 8_646 . ? F4 Si2 F4 60.6(3) 35_556 . ? F4 Si2 F4 119.4(3) 23_655 . ? F4 Si2 F4 60.6(3) 44_565 . ? F4 Si2 F4 119.4(3) 8_646 . ? F4 Si2 F4 180.000(14) 37_656 . ? F4 F3 F4 151(6) 35_556 . ? F4 F3 Si2 77(3) 35_556 . ? F4 F3 Si2 75(3) . . ? F4 F3 F3 137(3) 35_556 44_565 ? Si2 F3 F3 59.93(9) . 44_565 ? F4 F3 F3 133(3) . 35_556 ? Si2 F3 F3 59.93(9) . 35_556 ? F3 F3 F3 119.4(8) 44_565 35_556 ? F3 F4 F3 144(6) 44_565 . ? F3 F4 Si2 74(3) 44_565 . ? F3 F4 Si2 73(3) . . ? F3 F4 F4 133(3) 44_565 35_556 ? Si2 F4 F4 59.71(15) . 35_556 ? F3 F4 F4 129(3) . 44_565 ? Si2 F4 F4 59.71(15) . 44_565 ? F4 F4 F4 117.8(12) 35_556 44_565 ? 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 N1 Cu1 N1 C1 -79.9(4) 3_566 . . . ? N2 Cu1 N1 C1 55.4(5) . . . . ? N2 Cu1 N1 C1 145.8(4) 3_566 . . . ? N1 Cu1 N1 C4 109.7(5) 3_566 . . . ? N2 Cu1 N1 C4 -114.9(5) . . . . ? N2 Cu1 N1 C4 -24.6(6) 3_566 . . . ? N1 Cu1 N2 C1 -58.2(6) . . . 23_655 ? N1 Cu1 N2 C1 74.2(6) 3_566 . . 23_655 ? N2 Cu1 N2 C1 -173.2(6) 3_566 . . 23_655 ? N1 Cu1 N2 C2 112.7(4) . . . . ? N1 Cu1 N2 C2 -114.9(4) 3_566 . . . ? N2 Cu1 N2 C2 -2.3(3) 3_566 . . . ? C4 N1 C1 N2 4.3(9) . . . 8_646 ? Cu1 N1 C1 N2 -167.2(5) . . . 8_646 ? C1 N2 C2 C3 -1.5(9) 23_655 . . . ? Cu1 N2 C2 C3 -173.2(5) . . . . ? C1 N2 C2 C2 177.8(6) 23_655 . . 3_566 ? Cu1 N2 C2 C2 6.1(8) . . . 3_566 ? N2 C2 C3 C4 3.9(9) . . . 23_655 ? C2 C2 C3 C4 -175.4(7) 3_566 . . 23_655 ? C1 N1 C4 C3 -1.6(9) . . . 8_646 ? Cu1 N1 C4 C3 168.6(5) . . . 8_646 ? F3 Si2 F3 F4 9(2) 35_556 . . 35_556 ? F3 Si2 F3 F4 -171(2) 23_655 . . 35_556 ? F3 Si2 F3 F4 -179(6) 44_565 . . 35_556 ? F3 Si2 F3 F4 1(6) 8_646 . . 35_556 ? F4 Si2 F3 F4 180.000(6) 23_655 . . 35_556 ? F4 Si2 F3 F4 -170(5) 44_565 . . 35_556 ? F4 Si2 F3 F4 10(5) 8_646 . . 35_556 ? F4 Si2 F3 F4 -7(5) 37_656 . . 35_556 ? F4 Si2 F3 F4 173(5) . . . 35_556 ? F3 Si2 F3 F4 -165(5) 35_556 . . . ? F3 Si2 F3 F4 15(5) 23_655 . . . ? F3 Si2 F3 F4 8(2) 44_565 . . . ? F3 Si2 F3 F4 -172(2) 8_646 . . . ? F4 Si2 F3 F4 -173(5) 35_556 . . . ? F4 Si2 F3 F4 7(5) 23_655 . . . ? F4 Si2 F3 F4 16(4) 44_565 . . . ? F4 Si2 F3 F4 -164(4) 8_646 . . . ? F4 Si2 F3 F4 180.000(11) 37_656 . . . ? F3 Si2 F3 F3 -173(5) 35_556 . . 44_565 ? F3 Si2 F3 F3 7(5) 23_655 . . 44_565 ? F3 Si2 F3 F3 180.000(4) 8_646 . . 44_565 ? F4 Si2 F3 F3 179(6) 35_556 . . 44_565 ? F4 Si2 F3 F3 -1(6) 23_655 . . 44_565 ? F4 Si2 F3 F3 8(3) 44_565 . . 44_565 ? F4 Si2 F3 F3 -172(3) 8_646 . . 44_565 ? F4 Si2 F3 F3 172(2) 37_656 . . 44_565 ? F4 Si2 F3 F3 -8(2) . . . 44_565 ? F3 Si2 F3 F3 180.0 23_655 . . 35_556 ? F3 Si2 F3 F3 173(5) 44_565 . . 35_556 ? F3 Si2 F3 F3 -7(5) 8_646 . . 35_556 ? F4 Si2 F3 F3 -9(2) 35_556 . . 35_556 ? F4 Si2 F3 F3 171(2) 23_655 . . 35_556 ? F4 Si2 F3 F3 -179(3) 44_565 . . 35_556 ? F4 Si2 F3 F3 1(3) 8_646 . . 35_556 ? F4 Si2 F3 F3 -15(5) 37_656 . . 35_556 ? F4 Si2 F3 F3 165(5) . . . 35_556 ? F4 F3 F4 F3 -38(10) 35_556 . . 44_565 ? Si2 F3 F4 F3 -25(7) . . . 44_565 ? F3 F3 F4 F3 -43(9) 35_556 . . 44_565 ? F4 F3 F4 Si2 -13(10) 35_556 . . . ? F3 F3 F4 Si2 25(7) 44_565 . . . ? F3 F3 F4 Si2 -18(5) 35_556 . . . ? Si2 F3 F4 F4 13(10) . . . 35_556 ? F3 F3 F4 F4 38(10) 44_565 . . 35_556 ? F3 F3 F4 F4 -5(6) 35_556 . . 35_556 ? F4 F3 F4 F4 -34(12) 35_556 . . 44_565 ? Si2 F3 F4 F4 -21(4) . . . 44_565 ? F3 F3 F4 F4 4(5) 44_565 . . 44_565 ? F3 F3 F4 F4 -39(9) 35_556 . . 44_565 ? F3 Si2 F4 F3 179(5) 35_556 . . 44_565 ? F3 Si2 F4 F3 -1(5) 23_655 . . 44_565 ? F3 Si2 F4 F3 -15(4) 37_656 . . 44_565 ? F3 Si2 F4 F3 180.000(4) 8_646 . . 44_565 ? F3 Si2 F4 F3 165(4) . . . 44_565 ? F4 Si2 F4 F3 169(5) 35_556 . . 44_565 ? F4 Si2 F4 F3 -11(5) 23_655 . . 44_565 ? F4 Si2 F4 F3 4(3) 44_565 . . 44_565 ? F4 Si2 F4 F3 -176(3) 8_646 . . 44_565 ? F3 Si2 F4 F3 13(4) 35_556 . . . ? F3 Si2 F4 F3 -167(4) 23_655 . . . ? F3 Si2 F4 F3 180.000(5) 37_656 . . . ? F3 Si2 F4 F3 -165(4) 44_565 . . . ? F3 Si2 F4 F3 15(4) 8_646 . . . ? F4 Si2 F4 F3 4(3) 35_556 . . . ? F4 Si2 F4 F3 -176(3) 23_655 . . . ? F4 Si2 F4 F3 -161(4) 44_565 . . . ? F4 Si2 F4 F3 19(4) 8_646 . . . ? F3 Si2 F4 F4 10(2) 35_556 . . 35_556 ? F3 Si2 F4 F4 -170(2) 23_655 . . 35_556 ? F3 Si2 F4 F4 176(3) 37_656 . . 35_556 ? F3 Si2 F4 F4 -169(5) 44_565 . . 35_556 ? F3 Si2 F4 F4 11(5) 8_646 . . 35_556 ? F3 Si2 F4 F4 -4(3) . . . 35_556 ? F4 Si2 F4 F4 180.000(4) 23_655 . . 35_556 ? F4 Si2 F4 F4 -165(4) 44_565 . . 35_556 ? F4 Si2 F4 F4 15(4) 8_646 . . 35_556 ? F3 Si2 F4 F4 175(3) 35_556 . . 44_565 ? F3 Si2 F4 F4 -5(3) 23_655 . . 44_565 ? F3 Si2 F4 F4 -19(4) 37_656 . . 44_565 ? F3 Si2 F4 F4 -4(3) 44_565 . . 44_565 ? F3 Si2 F4 F4 176(3) 8_646 . . 44_565 ? F3 Si2 F4 F4 161(4) . . . 44_565 ? F4 Si2 F4 F4 165(4) 35_556 . . 44_565 ? F4 Si2 F4 F4 -15(4) 23_655 . . 44_565 ? F4 Si2 F4 F4 180.000(1) 8_646 . . 44_565 ? #------------------------------------------------------------------------------ _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' #------------------------------------------------------------------------------ ### END # Attachment '- cifs-complexes_1-5.cif' #------------------------------------------------------------------------------ data_[Cu2(bpm)(C2H4)(NO3)2]n_Complex-1-CCDC829823 _database_code_depnum_ccdc_archive 'CCDC 829823' #TrackingRef '- cifs-complexes_1-5.cif' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_melting_point ? _chemical_formula_moiety 'C10 H10 Cu2 N6 O6' _chemical_formula_sum 'C10 H10 Cu2 N6 O6' _chemical_formula_weight 437.32 #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' _symmetry_space_group_name_Hall '-P 2yab' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 'x, y, z' 2 '-x+1/2, y+1/2, -z' 3 '-x, -y, -z' 4 'x-1/2, -y-1/2, z' #------------------------------------------------------------------------------ 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #------------------------------------------------------------------------------ _cell_length_a 14.897(9) _cell_length_b 5.819(3) _cell_length_c 17.441(10) _cell_angle_alpha 90.00 _cell_angle_beta 107.581(6) _cell_angle_gamma 90.00 _cell_volume 1441.4(14) _cell_formula_units_Z 4 _cell_measurement_temperature 117(2) _cell_measurement_reflns_used 3973 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description chip _exptl_crystal_colour brown _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.015 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 2.995 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2666 _exptl_absorpt_correction_T_max 0.9425 _exptl_absorpt_process_details ? _exptl_special_details ; Jacobson, R. (1998) Private communication ; _diffrn_ambient_temperature 117(1) _diffrn_radiation_wavelength 0.71073 _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 10327 _diffrn_reflns_av_R_equivalents 0.0237 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3258 _reflns_number_gt 2814 _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^)+(0.0325P)^2^+1.6529P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3258 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0718 _refine_ls_wR_factor_gt 0.0686 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _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 0.19674(2) -0.32116(6) 0.146217(17) 0.01576(9) Uani 1 1 d . . . Cu2 Cu 0.01630(2) 0.42737(5) 0.281602(18) 0.01595(9) Uani 1 1 d . . . O1 O -0.00967(13) 0.6313(4) 0.17949(12) 0.0309(5) Uani 1 1 d . . . O2 O -0.09706(14) 0.8829(3) 0.10017(12) 0.0249(4) Uani 1 1 d . . . O3 O -0.16257(12) 0.5944(3) 0.14237(11) 0.0197(4) Uani 1 1 d . . . O4 O 0.07779(13) 0.7087(3) 0.35360(10) 0.0205(4) Uani 1 1 d . . . O5 O 0.13045(15) 0.8413(4) 0.47525(11) 0.0278(5) Uani 1 1 d . . . O6 O 0.08466(14) 0.4855(3) 0.45539(11) 0.0235(4) Uani 1 1 d . . . N1 N 0.42173(14) -0.7140(4) 0.30020(12) 0.0143(4) Uani 1 1 d . . . N2 N 0.29547(14) -0.4633(4) 0.23885(12) 0.0138(4) Uani 1 1 d . . . N3 N 0.12815(14) 0.2194(4) 0.28555(12) 0.0153(4) Uani 1 1 d . . . N4 N 0.18678(14) -0.1005(4) 0.23163(12) 0.0125(4) Uani 1 1 d . . . N5 N -0.09068(15) 0.7038(4) 0.13994(12) 0.0168(4) Uani 1 1 d . . . N6 N 0.09814(15) 0.6782(4) 0.42923(13) 0.0178(4) Uani 1 1 d . . . C1 C 0.1561(2) -0.4990(6) 0.04343(16) 0.0290(7) Uani 1 1 d . . . H1A H 0.2021 -0.5106 0.0128 0.035 Uiso 1 1 calc R . . H1B H 0.1211 -0.6433 0.0440 0.035 Uiso 1 1 calc R . . C2 C 0.10534(19) -0.2987(5) 0.03487(15) 0.0247(6) Uani 1 1 d . . . H2A H 0.0377 -0.3134 0.0302 0.030 Uiso 1 1 calc R . . H2B H 0.1187 -0.1805 -0.0010 0.030 Uiso 1 1 calc R . . C3 C 0.34912(17) -0.6436(4) 0.23786(14) 0.0143(5) Uani 1 1 d . . . H3 H 0.3354 -0.7299 0.1895 0.017 Uiso 1 1 calc R . . C4 C 0.31519(16) -0.3363(4) 0.30739(14) 0.0122(5) Uani 1 1 d . . . C5 C 0.38720(17) -0.3993(5) 0.37430(15) 0.0164(5) Uani 1 1 d . . . H5 H 0.4008 -0.3134 0.4228 0.020 Uiso 1 1 calc R . . C6 C 0.43914(18) -0.5916(5) 0.36859(15) 0.0172(5) Uani 1 1 d . . . H6 H 0.4887 -0.6390 0.4144 0.021 Uiso 1 1 calc R . . C7 C 0.12632(17) 0.0707(4) 0.22625(15) 0.0153(5) Uani 1 1 d . . . H7 H 0.0780 0.0894 0.1766 0.018 Uiso 1 1 calc R . . C8 C 0.25443(16) -0.1338(4) 0.30310(14) 0.0139(5) Uani 1 1 d . . . C9 C 0.26190(17) 0.0136(5) 0.36676(15) 0.0154(5) Uani 1 1 d . . . H9 H 0.3097 -0.0062 0.4166 0.019 Uiso 1 1 calc R . . C10 C 0.19749(17) 0.1911(5) 0.35538(14) 0.0157(5) Uani 1 1 d . . . H10 H 0.2022 0.2962 0.3981 0.019 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01694(16) 0.01702(17) 0.01073(15) -0.00227(12) 0.00028(11) 0.00223(13) Cu2 0.01433(15) 0.01474(17) 0.01832(16) -0.00017(12) 0.00425(12) -0.00077(12) O1 0.0159(9) 0.0514(15) 0.0236(10) 0.0173(10) 0.0032(8) 0.0022(9) O2 0.0295(11) 0.0209(10) 0.0252(10) 0.0070(8) 0.0095(8) -0.0007(8) O3 0.0174(9) 0.0194(10) 0.0227(9) 0.0027(8) 0.0065(7) 0.0001(7) O4 0.0267(10) 0.0208(10) 0.0127(8) -0.0009(7) 0.0039(7) -0.0031(8) O5 0.0385(12) 0.0215(10) 0.0192(9) -0.0098(8) 0.0026(8) -0.0037(9) O6 0.0286(10) 0.0215(10) 0.0180(9) 0.0029(8) 0.0036(8) -0.0053(8) N1 0.0116(9) 0.0156(11) 0.0158(10) -0.0005(8) 0.0040(8) -0.0001(8) N2 0.0132(10) 0.0151(11) 0.0128(9) -0.0009(8) 0.0036(8) -0.0017(8) N3 0.0134(10) 0.0159(11) 0.0168(10) -0.0002(8) 0.0049(8) 0.0005(8) N4 0.0114(9) 0.0140(10) 0.0120(9) -0.0001(8) 0.0034(7) -0.0004(8) N5 0.0186(10) 0.0206(12) 0.0113(9) 0.0001(9) 0.0048(8) 0.0004(9) N6 0.0154(10) 0.0204(11) 0.0176(10) -0.0031(9) 0.0047(8) 0.0021(9) C1 0.0289(15) 0.0387(18) 0.0154(13) -0.0130(12) 0.0004(11) -0.0057(13) C2 0.0204(13) 0.0379(17) 0.0119(11) 0.0011(12) -0.0008(10) -0.0015(12) C3 0.0151(11) 0.0133(12) 0.0145(11) -0.0018(9) 0.0047(9) -0.0012(9) C4 0.0122(11) 0.0133(12) 0.0117(10) -0.0009(9) 0.0043(9) -0.0020(9) C5 0.0166(12) 0.0183(13) 0.0135(11) -0.0031(10) 0.0033(9) -0.0010(10) C6 0.0148(11) 0.0200(13) 0.0147(11) 0.0012(10) 0.0014(9) 0.0007(10) C7 0.0124(11) 0.0171(13) 0.0166(11) 0.0009(10) 0.0045(9) 0.0018(10) C8 0.0118(11) 0.0158(12) 0.0135(11) 0.0023(9) 0.0026(9) -0.0033(9) C9 0.0162(12) 0.0167(12) 0.0127(11) -0.0017(10) 0.0034(9) -0.0019(10) C10 0.0153(11) 0.0181(13) 0.0143(11) -0.0021(10) 0.0054(9) 0.0005(10) _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 C1 1.999(3) . ? Cu1 N4 2.006(2) . ? Cu1 N2 2.006(2) . ? Cu1 C2 2.011(3) . ? Cu2 N1 1.977(2) 4 ? Cu2 N3 2.044(2) . ? Cu2 O1 2.077(2) . ? Cu2 O4 2.098(2) . ? O1 N5 1.268(3) . ? O2 N5 1.239(3) . ? O3 N5 1.258(3) . ? O4 N6 1.273(3) . ? O5 N6 1.242(3) . ? O6 N6 1.249(3) . ? N1 C6 1.345(3) . ? N1 C3 1.345(3) . ? N1 Cu2 1.977(2) 4_655 ? N2 C3 1.322(3) . ? N2 C4 1.360(3) . ? N3 C7 1.343(3) . ? N3 C10 1.348(3) . ? N4 C7 1.327(3) . ? N4 C8 1.359(3) . ? C1 C2 1.373(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3 0.9500 . ? C4 C5 1.375(3) . ? C4 C8 1.474(3) . ? C5 C6 1.381(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.381(4) . ? C9 C10 1.383(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? 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 C1 Cu1 N4 157.99(11) . . ? C1 Cu1 N2 117.31(12) . . ? N4 Cu1 N2 82.33(9) . . ? C1 Cu1 C2 40.03(13) . . ? N4 Cu1 C2 119.68(11) . . ? N2 Cu1 C2 157.30(11) . . ? N1 Cu2 N3 103.69(10) 4 . ? N1 Cu2 O1 122.84(9) 4 . ? N3 Cu2 O1 107.82(9) . . ? N1 Cu2 O4 126.58(8) 4 . ? N3 Cu2 O4 103.76(9) . . ? O1 Cu2 O4 90.10(9) . . ? N5 O1 Cu2 123.84(16) . . ? N6 O4 Cu2 115.82(16) . . ? C6 N1 C3 116.6(2) . . ? C6 N1 Cu2 121.46(17) . 4_655 ? C3 N1 Cu2 119.84(17) . 4_655 ? C3 N2 C4 118.2(2) . . ? C3 N2 Cu1 128.01(17) . . ? C4 N2 Cu1 113.27(16) . . ? C7 N3 C10 116.7(2) . . ? C7 N3 Cu2 121.95(17) . . ? C10 N3 Cu2 119.82(17) . . ? C7 N4 C8 118.1(2) . . ? C7 N4 Cu1 128.97(17) . . ? C8 N4 Cu1 112.90(17) . . ? O2 N5 O3 121.5(2) . . ? O2 N5 O1 118.9(2) . . ? O3 N5 O1 119.6(2) . . ? O5 N6 O6 121.5(2) . . ? O5 N6 O4 119.2(2) . . ? O6 N6 O4 119.3(2) . . ? C2 C1 Cu1 70.47(16) . . ? C2 C1 H1A 116.6 . . ? Cu1 C1 H1A 116.6 . . ? C2 C1 H1B 116.6 . . ? Cu1 C1 H1B 116.6 . . ? H1A C1 H1B 113.6 . . ? C1 C2 Cu1 69.50(15) . . ? C1 C2 H2A 116.7 . . ? Cu1 C2 H2A 116.7 . . ? C1 C2 H2B 116.7 . . ? Cu1 C2 H2B 116.7 . . ? H2A C2 H2B 113.7 . . ? N2 C3 N1 124.9(2) . . ? N2 C3 H3 117.5 . . ? N1 C3 H3 117.5 . . ? N2 C4 C5 120.5(2) . . ? N2 C4 C8 115.1(2) . . ? C5 C4 C8 124.5(2) . . ? C4 C5 C6 117.7(2) . . ? C4 C5 H5 121.1 . . ? C6 C5 H5 121.1 . . ? N1 C6 C5 122.0(2) . . ? N1 C6 H6 119.0 . . ? C5 C6 H6 119.0 . . ? N4 C7 N3 125.0(2) . . ? N4 C7 H7 117.5 . . ? N3 C7 H7 117.5 . . ? N4 C8 C9 120.4(2) . . ? N4 C8 C4 115.7(2) . . ? C9 C8 C4 123.8(2) . . ? C8 C9 C10 117.7(2) . . ? C8 C9 H9 121.2 . . ? C10 C9 H9 121.2 . . ? N3 C10 C9 122.0(2) . . ? N3 C10 H10 119.0 . . ? C9 C10 H10 119.0 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.679 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.082 ###END #------------------------------------------------------------------------------ data_{[Cu3(bpm)2(C2H4)2](ClO4)3}n_Complex-2-CCDC829824 _database_code_depnum_ccdc_archive 'CCDC 829824' #TrackingRef '- cifs-complexes_1-5.cif' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_moiety 'C20 H20 Cl2 Cu3 N8 O8, Cl O4' _chemical_formula_sum 'C20 H20 Cl3 Cu3 N8 O12' _chemical_formula_weight 861.44 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc ' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 'x, y, z' 2 '-x, y, -z+1/2' 3 'x+1/2, y+1/2, z' 4 '-x+1/2, y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x, -y, z-1/2' 7 '-x+1/2, -y+1/2, -z' 8 'x+1/2, -y+1/2, z-1/2' #------------------------------------------------------------------------------ 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 20.8073(9) _cell_length_b 13.2133(18) _cell_length_c 15.3486(11) _cell_angle_alpha 90.00 _cell_angle_beta 132.126(2) _cell_angle_gamma 90.00 _cell_volume 3129.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 108(2) _cell_measurement_reflns_used 11447 _cell_measurement_theta_min 3.78 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.828 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 2.347 _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 108(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 11447 _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_av_sigmaI/netI 0.0513 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.46 _reflns_number_total 3561 _reflns_number_gt 2606 _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^)+(0.0690P)^2^+14.6926P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3561 _refine_ls_number_parameters 198 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0870 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1475 _refine_ls_wR_factor_gt 0.1320 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 N4 N 0.1646(3) 0.3260(3) 0.2606(3) 0.0248(8) Uani 1 1 d . . . C7 C 0.2427(3) 0.3553(4) 0.3599(4) 0.0266(10) Uani 1 1 d . . . H7 H 0.2916 0.3200 0.3863 0.032 Uiso 1 1 calc R . . C8 C 0.0965(3) 0.3789(3) 0.2263(4) 0.0241(10) Uani 1 1 d . . . H8 H 0.0424 0.3596 0.1563 0.029 Uiso 1 1 calc R . . C9 C 0.0943(5) 0.0952(5) 0.1791(6) 0.0518(18) Uani 1 1 d . . . H9A H 0.1333 0.0551 0.2501 0.062 Uiso 1 1 calc R . . H9B H 0.0387 0.1080 0.1559 0.062 Uiso 1 1 calc R . . C10 C 0.0933(5) 0.0743(5) 0.0897(6) 0.0540(18) Uani 1 1 d . . . H10A H 0.0370 0.0738 0.0104 0.065 Uiso 1 1 calc R . . H10B H 0.1316 0.0209 0.1046 0.065 Uiso 1 1 calc R . . Cu1 Cu 0.14767(4) 0.21149(4) 0.15983(5) 0.02428(18) Uani 1 1 d . . . Cu2 Cu 0.0000 0.53414(6) 0.2500 0.0244(2) Uani 1 2 d S . . N1 N 0.1648(2) 0.2854(3) 0.0621(3) 0.0213(8) Uani 1 1 d . . . N3 N 0.0989(2) 0.4568(3) 0.2830(3) 0.0222(8) Uani 1 1 d . . . C6 C 0.2521(3) 0.4366(4) 0.4240(4) 0.0266(10) Uani 1 1 d . . . H6 H 0.3066 0.4575 0.4922 0.032 Uiso 1 1 calc R . . C2 C 0.0960(3) 0.3261(4) -0.0402(4) 0.0231(9) Uani 1 1 d . . . H2 H 0.0415 0.3034 -0.0727 0.028 Uiso 1 1 calc R . . C5 C 0.1778(3) 0.4861(3) 0.3834(4) 0.0205(9) Uani 1 1 d . . . N2 N 0.0991(2) 0.3963(3) -0.0994(3) 0.0218(8) Uani 1 1 d . . . C4 C 0.1777(3) 0.5712(3) 0.4465(4) 0.0200(9) Uani 1 1 d . . . C3 C 0.2521(3) 0.6130(4) 0.5484(4) 0.0258(10) Uani 1 1 d . . . H3 H 0.3065 0.5935 0.5779 0.031 Uiso 1 1 calc R . . C1 C 0.2432(3) 0.3148(4) 0.1055(4) 0.0240(10) Uani 1 1 d . . . H1 H 0.2925 0.2864 0.1751 0.029 Uiso 1 1 calc R . . Cl1 Cl 0.0000 0.10211(13) 0.7500 0.0259(4) Uani 1 2 d S . . O2 O 0.0589(2) 0.0388(3) 0.8513(3) 0.0389(9) Uani 1 1 d . . . O1 O 0.0485(2) 0.1639(3) 0.7352(4) 0.0521(12) Uani 1 1 d . . . Cl2 Cl 0.35630(8) 0.10995(10) 0.39363(11) 0.0327(3) Uani 1 1 d . . . O3 O 0.3026(4) 0.1759(5) 0.2960(6) 0.0327(3) Uani 0.621(4) 1 d P . . O4 O 0.3587(4) 0.1336(5) 0.4853(5) 0.0327(3) Uani 0.621(4) 1 d P . . O5 O 0.3250(4) 0.0039(4) 0.3536(5) 0.0327(3) Uani 0.621(4) 1 d P . . O6 O 0.4434(4) 0.1114(4) 0.4381(5) 0.0327(3) Uani 0.621(4) 1 d P . . O7 O 0.2887(7) 0.1445(8) 0.2711(9) 0.0327(3) Uani 0.379(4) 1 d P . . O8 O 0.3175(7) 0.1281(8) 0.4467(9) 0.0327(3) Uani 0.379(4) 1 d P . . O9 O 0.3815(7) 0.0168(7) 0.4032(8) 0.0327(3) Uani 0.379(4) 1 d P . . O10 O 0.4255(6) 0.1892(7) 0.4475(8) 0.0327(3) Uani 0.379(4) 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 N4 0.025(2) 0.025(2) 0.0218(19) 0.0012(17) 0.0147(18) 0.0000(17) C7 0.024(2) 0.027(2) 0.028(2) -0.001(2) 0.017(2) 0.0046(19) C8 0.024(2) 0.024(2) 0.025(2) -0.0004(19) 0.017(2) 0.0011(19) C9 0.081(5) 0.039(3) 0.059(4) -0.016(3) 0.057(4) -0.031(3) C10 0.084(5) 0.039(3) 0.062(4) -0.026(3) 0.059(4) -0.037(3) Cu1 0.0288(3) 0.0218(3) 0.0240(3) -0.0018(2) 0.0184(3) -0.0036(2) Cu2 0.0176(4) 0.0272(4) 0.0200(4) 0.000 0.0092(3) 0.000 N1 0.0215(18) 0.0196(19) 0.0215(19) -0.0015(15) 0.0139(17) -0.0015(15) N3 0.0194(19) 0.0218(19) 0.0186(18) -0.0010(16) 0.0100(16) -0.0024(16) C6 0.020(2) 0.027(3) 0.023(2) -0.005(2) 0.011(2) -0.0004(19) C2 0.023(2) 0.022(2) 0.023(2) 0.0003(19) 0.015(2) -0.0003(18) C5 0.023(2) 0.017(2) 0.021(2) -0.0026(18) 0.0145(19) -0.0022(18) N2 0.0207(19) 0.0218(19) 0.0183(18) -0.0021(15) 0.0112(17) -0.0036(15) C4 0.021(2) 0.020(2) 0.019(2) 0.0020(18) 0.0139(19) 0.0007(18) C3 0.022(2) 0.028(3) 0.024(2) -0.003(2) 0.014(2) -0.0005(19) C1 0.022(2) 0.026(2) 0.020(2) 0.0047(19) 0.012(2) 0.0019(19) Cl1 0.0182(7) 0.0298(8) 0.0251(8) 0.000 0.0125(7) 0.000 O2 0.0230(18) 0.057(3) 0.0270(19) 0.0143(18) 0.0127(16) -0.0006(17) O1 0.0244(19) 0.055(3) 0.060(3) 0.029(2) 0.022(2) 0.0014(19) Cl2 0.0352(6) 0.0354(6) 0.0276(6) 0.0062(5) 0.0211(5) 0.0052(5) O3 0.0352(6) 0.0354(6) 0.0276(6) 0.0062(5) 0.0211(5) 0.0052(5) O4 0.0352(6) 0.0354(6) 0.0276(6) 0.0062(5) 0.0211(5) 0.0052(5) O5 0.0352(6) 0.0354(6) 0.0276(6) 0.0062(5) 0.0211(5) 0.0052(5) O6 0.0352(6) 0.0354(6) 0.0276(6) 0.0062(5) 0.0211(5) 0.0052(5) O7 0.0352(6) 0.0354(6) 0.0276(6) 0.0062(5) 0.0211(5) 0.0052(5) O8 0.0352(6) 0.0354(6) 0.0276(6) 0.0062(5) 0.0211(5) 0.0052(5) O9 0.0352(6) 0.0354(6) 0.0276(6) 0.0062(5) 0.0211(5) 0.0052(5) O10 0.0352(6) 0.0354(6) 0.0276(6) 0.0062(5) 0.0211(5) 0.0052(5) _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 N4 C8 1.332(6) . ? N4 C7 1.338(6) . ? N4 Cu1 2.019(4) . ? C7 C6 1.380(7) . ? C7 H7 0.9300 . ? C8 N3 1.326(6) . ? C8 H8 0.9300 . ? C9 C10 1.385(8) . ? C9 Cu1 2.030(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 Cu1 2.023(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? Cu1 N1 2.012(4) . ? Cu1 O7 2.363(11) . ? Cu1 O3 2.438(7) . ? Cu2 N2 2.011(4) 6_566 ? Cu2 N2 2.011(4) 5_565 ? Cu2 N3 2.034(4) 2 ? Cu2 N3 2.034(4) . ? N1 C2 1.337(6) . ? N1 C1 1.341(6) . ? N3 C5 1.351(6) . ? C6 C5 1.383(6) . ? C6 H6 0.9300 . ? C2 N2 1.330(6) . ? C2 H2 0.9300 . ? C5 C4 1.485(6) . ? N2 C4 1.346(6) 6_565 ? N2 Cu2 2.011(4) 5_565 ? C4 N2 1.346(6) 6_566 ? C4 C3 1.377(6) . ? C3 C1 1.391(7) 6_566 ? C3 H3 0.9300 . ? C1 C3 1.391(7) 6_565 ? C1 H1 0.9300 . ? Cl1 O1 1.431(4) . ? Cl1 O1 1.431(4) 2_556 ? Cl1 O2 1.436(4) 2_556 ? Cl1 O2 1.436(4) . ? Cl2 O9 1.307(10) . ? Cl2 O4 1.409(6) . ? Cl2 O3 1.417(7) . ? Cl2 O6 1.446(6) . ? Cl2 O7 1.474(11) . ? Cl2 O5 1.493(6) . ? Cl2 O10 1.502(10) . ? Cl2 O8 1.503(10) . ? O3 O7 0.503(11) . ? O4 O8 0.641(10) . ? O5 O9 0.890(10) . ? O6 O10 1.134(11) . ? O6 O9 1.606(12) . ? 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 C8 N4 C7 117.1(4) . . ? C8 N4 Cu1 119.9(3) . . ? C7 N4 Cu1 122.9(3) . . ? N4 C7 C6 121.3(4) . . ? N4 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? N3 C8 N4 125.9(4) . . ? N3 C8 H8 117.1 . . ? N4 C8 H8 117.1 . . ? C10 C9 Cu1 69.7(3) . . ? C10 C9 H9A 116.7 . . ? Cu1 C9 H9A 116.7 . . ? C10 C9 H9B 116.7 . . ? Cu1 C9 H9B 116.7 . . ? H9A C9 H9B 113.7 . . ? C9 C10 Cu1 70.3(3) . . ? C9 C10 H10A 116.6 . . ? Cu1 C10 H10A 116.6 . . ? C9 C10 H10B 116.6 . . ? Cu1 C10 H10B 116.6 . . ? H10A C10 H10B 113.6 . . ? N1 Cu1 N4 100.39(15) . . ? N1 Cu1 C10 110.8(2) . . ? N4 Cu1 C10 145.8(2) . . ? N1 Cu1 C9 149.7(2) . . ? N4 Cu1 C9 106.7(2) . . ? C10 Cu1 C9 40.0(2) . . ? N1 Cu1 O7 88.1(3) . . ? N4 Cu1 O7 103.5(3) . . ? C10 Cu1 O7 91.7(3) . . ? C9 Cu1 O7 98.4(4) . . ? N1 Cu1 O3 86.51(19) . . ? N4 Cu1 O3 92.13(19) . . ? C10 Cu1 O3 103.3(3) . . ? C9 Cu1 O3 105.5(3) . . ? O7 Cu1 O3 11.9(3) . . ? N2 Cu2 N2 125.6(2) 6_566 5_565 ? N2 Cu2 N3 127.01(15) 6_566 2 ? N2 Cu2 N3 81.80(15) 5_565 2 ? N2 Cu2 N3 81.80(15) 6_566 . ? N2 Cu2 N3 127.01(15) 5_565 . ? N3 Cu2 N3 119.7(2) 2 . ? C2 N1 C1 117.0(4) . . ? C2 N1 Cu1 119.1(3) . . ? C1 N1 Cu1 122.3(3) . . ? C8 N3 C5 116.9(4) . . ? C8 N3 Cu2 129.8(3) . . ? C5 N3 Cu2 113.1(3) . . ? C7 C6 C5 117.8(4) . . ? C7 C6 H6 121.1 . . ? C5 C6 H6 121.1 . . ? N2 C2 N1 125.4(4) . . ? N2 C2 H2 117.3 . . ? N1 C2 H2 117.3 . . ? N3 C5 C6 121.0(4) . . ? N3 C5 C4 115.4(4) . . ? C6 C5 C4 123.6(4) . . ? C2 N2 C4 117.6(4) . 6_565 ? C2 N2 Cu2 128.5(3) . 5_565 ? C4 N2 Cu2 114.0(3) 6_565 5_565 ? N2 C4 C3 120.9(4) 6_566 . ? N2 C4 C5 115.6(4) 6_566 . ? C3 C4 C5 123.5(4) . . ? C4 C3 C1 117.8(4) . 6_566 ? C4 C3 H3 121.1 . . ? C1 C3 H3 121.1 6_566 . ? N1 C1 C3 121.2(4) . 6_565 ? N1 C1 H1 119.4 . . ? C3 C1 H1 119.4 6_565 . ? O1 Cl1 O1 110.4(4) . 2_556 ? O1 Cl1 O2 109.9(3) . 2_556 ? O1 Cl1 O2 108.9(2) 2_556 2_556 ? O1 Cl1 O2 108.9(2) . . ? O1 Cl1 O2 109.9(3) 2_556 . ? O2 Cl1 O2 108.8(4) 2_556 . ? O9 Cl2 O4 110.7(5) . . ? O9 Cl2 O3 132.1(5) . . ? O4 Cl2 O3 113.2(4) . . ? O9 Cl2 O6 71.2(5) . . ? O4 Cl2 O6 109.4(4) . . ? O3 Cl2 O6 109.9(4) . . ? O9 Cl2 O7 113.8(6) . . ? O4 Cl2 O7 124.7(5) . . ? O3 Cl2 O7 19.9(4) . . ? O6 Cl2 O7 114.9(5) . . ? O9 Cl2 O5 36.3(4) . . ? O4 Cl2 O5 109.4(3) . . ? O3 Cl2 O5 109.0(3) . . ? O6 Cl2 O5 105.6(3) . . ? O7 Cl2 O5 89.2(5) . . ? O9 Cl2 O10 115.5(6) . . ? O4 Cl2 O10 85.3(4) . . ? O3 Cl2 O10 86.4(5) . . ? O6 Cl2 O10 45.2(4) . . ? O7 Cl2 O10 103.2(6) . . ? O5 Cl2 O10 150.9(4) . . ? O9 Cl2 O8 114.3(6) . . ? O4 Cl2 O8 25.2(4) . . ? O3 Cl2 O8 98.4(5) . . ? O6 Cl2 O8 134.5(5) . . ? O7 Cl2 O8 104.0(6) . . ? O5 Cl2 O8 97.4(5) . . ? O10 Cl2 O8 104.8(6) . . ? O7 O3 Cl2 86.5(18) . . ? O7 O3 Cu1 75.6(18) . . ? Cl2 O3 Cu1 132.5(4) . . ? O8 O4 Cl2 85.6(12) . . ? O9 O5 Cl2 60.4(7) . . ? O10 O6 Cl2 70.0(6) . . ? O10 O6 O9 119.3(7) . . ? Cl2 O6 O9 50.4(4) . . ? O3 O7 Cl2 73.6(17) . . ? O3 O7 Cu1 92.5(19) . . ? Cl2 O7 Cu1 134.3(6) . . ? O4 O8 Cl2 69.2(11) . . ? O5 O9 Cl2 83.3(8) . . ? O5 O9 O6 137.6(10) . . ? Cl2 O9 O6 58.4(4) . . ? O6 O10 Cl2 64.8(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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C8 N4 C7 C6 0.1(7) . . . . ? Cu1 N4 C7 C6 177.2(4) . . . . ? C7 N4 C8 N3 -1.5(7) . . . . ? Cu1 N4 C8 N3 -178.7(4) . . . . ? C8 N4 Cu1 N1 92.3(4) . . . . ? C7 N4 Cu1 N1 -84.7(4) . . . . ? C8 N4 Cu1 C10 -63.3(6) . . . . ? C7 N4 Cu1 C10 119.7(5) . . . . ? C8 N4 Cu1 C9 -74.0(4) . . . . ? C7 N4 Cu1 C9 109.0(4) . . . . ? C8 N4 Cu1 O7 -177.2(4) . . . . ? C7 N4 Cu1 O7 5.8(5) . . . . ? C8 N4 Cu1 O3 179.1(4) . . . . ? C7 N4 Cu1 O3 2.1(4) . . . . ? C9 C10 Cu1 N1 -170.3(4) . . . . ? C9 C10 Cu1 N4 -16.1(7) . . . . ? C9 C10 Cu1 O7 101.1(5) . . . . ? C9 C10 Cu1 O3 98.4(5) . . . . ? C10 C9 Cu1 N1 18.2(8) . . . . ? C10 C9 Cu1 N4 170.6(4) . . . . ? C10 C9 Cu1 O7 -82.5(5) . . . . ? C10 C9 Cu1 O3 -92.3(5) . . . . ? N4 Cu1 N1 C2 -90.7(3) . . . . ? C10 Cu1 N1 C2 74.9(4) . . . . ? C9 Cu1 N1 C2 62.5(6) . . . . ? O7 Cu1 N1 C2 166.0(4) . . . . ? O3 Cu1 N1 C2 177.8(4) . . . . ? N4 Cu1 N1 C1 74.4(4) . . . . ? C10 Cu1 N1 C1 -120.0(4) . . . . ? C9 Cu1 N1 C1 -132.4(5) . . . . ? O7 Cu1 N1 C1 -28.9(4) . . . . ? O3 Cu1 N1 C1 -17.1(4) . . . . ? N4 C8 N3 C5 1.5(7) . . . . ? N4 C8 N3 Cu2 -172.8(3) . . . . ? N2 Cu2 N3 C8 175.1(4) 6_566 . . . ? N2 Cu2 N3 C8 -56.0(5) 5_565 . . . ? N3 Cu2 N3 C8 46.9(4) 2 . . . ? N2 Cu2 N3 C5 0.6(3) 6_566 . . . ? N2 Cu2 N3 C5 129.6(3) 5_565 . . . ? N3 Cu2 N3 C5 -127.5(3) 2 . . . ? N4 C7 C6 C5 1.2(7) . . . . ? C1 N1 C2 N2 -3.2(7) . . . . ? Cu1 N1 C2 N2 162.7(4) . . . . ? C8 N3 C5 C6 0.0(7) . . . . ? Cu2 N3 C5 C6 175.2(4) . . . . ? C8 N3 C5 C4 -178.0(4) . . . . ? Cu2 N3 C5 C4 -2.8(5) . . . . ? C7 C6 C5 N3 -1.3(7) . . . . ? C7 C6 C5 C4 176.6(4) . . . . ? N1 C2 N2 C4 0.6(7) . . . 6_565 ? N1 C2 N2 Cu2 -177.4(3) . . . 5_565 ? N3 C5 C4 N2 4.5(6) . . . 6_566 ? C6 C5 C4 N2 -173.5(4) . . . 6_566 ? N3 C5 C4 C3 -178.1(4) . . . . ? C6 C5 C4 C3 3.9(7) . . . . ? N2 C4 C3 C1 3.7(7) 6_566 . . 6_566 ? C5 C4 C3 C1 -173.5(4) . . . 6_566 ? C2 N1 C1 C3 2.2(7) . . . 6_565 ? Cu1 N1 C1 C3 -163.2(4) . . . 6_565 ? O9 Cl2 O3 O7 26(2) . . . . ? O4 Cl2 O3 O7 -129.2(18) . . . . ? O6 Cl2 O3 O7 108.2(18) . . . . ? O5 Cl2 O3 O7 -7.1(19) . . . . ? O10 Cl2 O3 O7 147.5(19) . . . . ? O8 Cl2 O3 O7 -108.0(19) . . . . ? O9 Cl2 O3 Cu1 92.6(8) . . . . ? O4 Cl2 O3 Cu1 -62.5(6) . . . . ? O6 Cl2 O3 Cu1 174.9(4) . . . . ? O7 Cl2 O3 Cu1 66.7(18) . . . . ? O5 Cl2 O3 Cu1 59.6(6) . . . . ? O10 Cl2 O3 Cu1 -145.7(6) . . . . ? O8 Cl2 O3 Cu1 -41.3(7) . . . . ? N1 Cu1 O3 O7 -97.2(18) . . . . ? N4 Cu1 O3 O7 162.5(18) . . . . ? C10 Cu1 O3 O7 13.3(18) . . . . ? C9 Cu1 O3 O7 54.6(18) . . . . ? N1 Cu1 O3 Cl2 -168.4(5) . . . . ? N4 Cu1 O3 Cl2 91.3(5) . . . . ? C10 Cu1 O3 Cl2 -57.9(6) . . . . ? C9 Cu1 O3 Cl2 -16.6(6) . . . . ? O7 Cu1 O3 Cl2 -71.2(18) . . . . ? O9 Cl2 O4 O8 -103.2(13) . . . . ? O3 Cl2 O4 O8 57.3(13) . . . . ? O6 Cl2 O4 O8 -179.7(12) . . . . ? O7 Cl2 O4 O8 38.6(14) . . . . ? O5 Cl2 O4 O8 -64.5(13) . . . . ? O10 Cl2 O4 O8 141.4(13) . . . . ? O4 Cl2 O5 O9 -98.9(8) . . . . ? O3 Cl2 O5 O9 136.8(8) . . . . ? O6 Cl2 O5 O9 18.8(8) . . . . ? O7 Cl2 O5 O9 134.4(9) . . . . ? O10 Cl2 O5 O9 18.0(12) . . . . ? O8 Cl2 O5 O9 -121.6(9) . . . . ? O9 Cl2 O6 O10 -167.9(7) . . . . ? O4 Cl2 O6 O10 -61.8(6) . . . . ? O3 Cl2 O6 O10 63.1(6) . . . . ? O7 Cl2 O6 O10 84.0(7) . . . . ? O5 Cl2 O6 O10 -179.5(6) . . . . ? O8 Cl2 O6 O10 -62.0(8) . . . . ? O4 Cl2 O6 O9 106.1(5) . . . . ? O3 Cl2 O6 O9 -129.0(5) . . . . ? O7 Cl2 O6 O9 -108.1(6) . . . . ? O5 Cl2 O6 O9 -11.6(5) . . . . ? O10 Cl2 O6 O9 167.9(7) . . . . ? O8 Cl2 O6 O9 105.9(7) . . . . ? Cu1 O3 O7 Cl2 -135.7(4) . . . . ? Cl2 O3 O7 Cu1 135.7(4) . . . . ? O9 Cl2 O7 O3 -159.2(17) . . . . ? O4 Cl2 O7 O3 60(2) . . . . ? O6 Cl2 O7 O3 -79.9(19) . . . . ? O5 Cl2 O7 O3 173.2(18) . . . . ? O10 Cl2 O7 O3 -33.4(19) . . . . ? O8 Cl2 O7 O3 75.9(19) . . . . ? O9 Cl2 O7 Cu1 123.6(8) . . . . ? O4 Cl2 O7 Cu1 -17.1(11) . . . . ? O3 Cl2 O7 Cu1 -77.1(18) . . . . ? O6 Cl2 O7 Cu1 -157.0(7) . . . . ? O5 Cl2 O7 Cu1 96.1(8) . . . . ? O10 Cl2 O7 Cu1 -110.5(8) . . . . ? O8 Cl2 O7 Cu1 -1.3(10) . . . . ? N1 Cu1 O7 O3 82.2(18) . . . . ? N4 Cu1 O7 O3 -18.0(19) . . . . ? C10 Cu1 O7 O3 -167.1(18) . . . . ? C9 Cu1 O7 O3 -127.5(18) . . . . ? N1 Cu1 O7 Cl2 151.6(8) . . . . ? N4 Cu1 O7 Cl2 51.4(9) . . . . ? C10 Cu1 O7 Cl2 -97.6(9) . . . . ? C9 Cu1 O7 Cl2 -58.1(9) . . . . ? O3 Cu1 O7 Cl2 69.4(17) . . . . ? O9 Cl2 O8 O4 87.3(13) . . . . ? O3 Cl2 O8 O4 -128.6(12) . . . . ? O6 Cl2 O8 O4 0.4(16) . . . . ? O7 Cl2 O8 O4 -148.1(12) . . . . ? O5 Cl2 O8 O4 120.9(12) . . . . ? O10 Cl2 O8 O4 -40.1(13) . . . . ? Cl2 O5 O9 O6 -24.5(11) . . . . ? O4 Cl2 O9 O5 94.9(7) . . . . ? O3 Cl2 O9 O5 -60.7(10) . . . . ? O6 Cl2 O9 O5 -160.9(8) . . . . ? O7 Cl2 O9 O5 -51.3(9) . . . . ? O10 Cl2 O9 O5 -170.4(7) . . . . ? O8 Cl2 O9 O5 67.9(9) . . . . ? O4 Cl2 O9 O6 -104.2(4) . . . . ? O3 Cl2 O9 O6 100.2(6) . . . . ? O7 Cl2 O9 O6 109.6(6) . . . . ? O5 Cl2 O9 O6 160.9(8) . . . . ? O10 Cl2 O9 O6 -9.5(6) . . . . ? O8 Cl2 O9 O6 -131.2(5) . . . . ? O10 O6 O9 O5 41.9(17) . . . . ? Cl2 O6 O9 O5 28.9(13) . . . . ? O10 O6 O9 Cl2 13.1(8) . . . . ? O9 O6 O10 Cl2 -10.7(6) . . . . ? O9 Cl2 O10 O6 12.7(7) . . . . ? O4 Cl2 O10 O6 123.4(5) . . . . ? O3 Cl2 O10 O6 -122.9(6) . . . . ? O7 Cl2 O10 O6 -112.0(6) . . . . ? O5 Cl2 O10 O6 1.0(11) . . . . ? O8 Cl2 O10 O6 139.4(6) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.009 _refine_diff_density_min -1.245 _refine_diff_density_rms 0.127 ###END #------------------------------------------------------------------------------ data_{[Cu3(bpm)2(C2H4)2](BF4)3}n_Complex-3-CCDC829825 _database_code_depnum_ccdc_archive 'CCDC 829825' #TrackingRef '- cifs-complexes_1-5.cif' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_moiety 'C20 H20 B2 Cu3 F8 N8, B F4' _chemical_formula_sum 'C20 H20 B3 Cu3 F12 N8' _chemical_formula_weight 823.49 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc ' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,+Y,1/2-Z 3 -X,-Y,-Z 4 +X,-Y,1/2+Z 5 1/2+X,1/2+Y,+Z 6 1/2-X,1/2+Y,1/2-Z 7 1/2-X,1/2-Y,-Z 8 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ 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' 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' #------------------------------------------------------------------------------ _cell_length_a 20.8286(7) _cell_length_b 12.9965(5) _cell_length_c 15.3593(5) _cell_angle_alpha 90.00 _cell_angle_beta 132.5660(10) _cell_angle_gamma 90.00 _cell_volume 3062.17(19) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 16008 _cell_measurement_theta_min 3.135 _cell_measurement_theta_max 27.515 _exptl_crystal_description Chip _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.786 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 2.165 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.771 _exptl_absorpt_correction_T_max 0.897 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 17589 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3464 _reflns_number_gt 2955 _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^)+(0.0296P)^2^+7.7916P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3464 _refine_ls_number_parameters 246 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0761 _refine_ls_wR_factor_gt 0.0719 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.054 _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 Cu(1) Cu 0.646763(19) 0.79161(2) 0.65980(3) 0.02276(8) Uani 1.00 1 d . . . Cu(2) Cu 0.5000 0.46377(3) 0.7500 0.02355(11) Uani 1.00 2 d S . . F(1) F 0.54493(11) 0.15753(15) 0.73221(17) 0.0563(5) Uani 1.00 1 d . . . F(2) F 0.55954(9) 0.03477(14) 0.84819(14) 0.0408(4) Uani 1.00 1 d . . . F(3) F 0.8038(4) 0.8285(4) 0.8004(6) 0.0347(10) Uani 0.74 1 d P . . F(4) F 0.8650(3) 0.8697(6) 0.9886(5) 0.0444(11) Uani 0.74 1 d P . . F(5) F 0.94453(19) 0.8774(4) 0.9398(3) 0.0651(13) Uani 0.74 1 d P . . F(6) F 0.8374(3) 0.9947(2) 0.8625(4) 0.0504(10) Uani 0.74 1 d P . . F(7) F 0.8859(10) 0.9822(9) 0.9069(12) 0.059(2) Uani 0.26 1 d P . . F(8) F 0.8291(10) 0.8743(15) 0.9537(16) 0.048(3) Uani 0.26 1 d P . . F(9) F 0.7946(16) 0.8576(15) 0.788(2) 0.065(6) Uani 0.26 1 d P . . F(10) F 0.9299(7) 0.8163(11) 0.9498(9) 0.071(3) Uani 0.26 1 d P . . N(1) N 0.66355(13) 0.67806(15) 0.76203(18) 0.0237(4) Uani 1.00 1 d . . . N(2) N 0.59933(12) 0.54265(15) 0.78424(17) 0.0210(4) Uani 1.00 1 d . . . N(3) N 0.59977(12) 0.39514(15) 0.90220(17) 0.0204(4) Uani 1.00 1 d . . . N(4) N 0.66600(12) 0.28424(14) 1.06559(17) 0.0209(4) Uani 1.00 1 d . . . C(1) C 0.74205(16) 0.6515(2) 0.8654(2) 0.0282(5) Uani 1.00 1 d . . . C(2) C 0.59533(15) 0.62137(18) 0.7252(2) 0.0236(4) Uani 1.00 1 d . . . C(3) C 0.75255(16) 0.56955(19) 0.9306(2) 0.0271(5) Uani 1.00 1 d . . . C(4) C 0.67875(14) 0.51599(17) 0.8877(2) 0.0200(4) Uani 1.00 1 d . . . C(5) C 0.67938(14) 0.42977(17) 0.9511(2) 0.0197(4) Uani 1.00 1 d . . . C(6) C 0.75450(15) 0.38810(18) 1.0551(2) 0.0235(4) Uani 1.00 1 d . . . C(7) C 0.74504(15) 0.31520(18) 1.1109(2) 0.0236(4) Uani 1.00 1 d . . . C(8) C 0.59669(15) 0.32375(18) 0.9612(2) 0.0215(4) Uani 1.00 1 d . . . C(9) C 0.6003(2) 0.9155(2) 0.6811(3) 0.0544(9) Uani 1.00 1 d . . . C(10) C 0.6040(2) 0.9353(2) 0.5969(3) 0.0522(9) Uani 1.00 1 d . . . B(1) B 0.5000 0.0987(3) 0.7500 0.0277(8) Uani 1.00 2 d S . . B(2) B 0.8628(2) 0.8918(2) 0.8989(2) 0.0318(6) Uani 1.00 1 d . . . H(1) H 0.7907 0.6897 0.8937 0.034 Uiso 1.00 1 c R . . H(2) H 0.5409 0.6383 0.6529 0.028 Uiso 1.00 1 c R . . H(3) H 0.8074 0.5507 1.0012 0.033 Uiso 1.00 1 c R . . H(4) H 0.8093 0.4085 1.0862 0.028 Uiso 1.00 1 c R . . H(5) H 0.7946 0.2867 1.1816 0.028 Uiso 1.00 1 c R . . H(6) H 0.5420 0.2994 0.9272 0.026 Uiso 1.00 1 c R . . H(7) H 0.5426 0.9091 0.6536 0.065 Uiso 1.00 1 c R . . H(8) H 0.6413 0.9525 0.7552 0.065 Uiso 1.00 1 c R . . H(9) H 0.6473 0.9849 0.6177 0.063 Uiso 1.00 1 c R . . H(10) H 0.5487 0.9415 0.5161 0.063 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) 0.02643(16) 0.02068(15) 0.02181(16) 0.00262(11) 0.01657(14) 0.00151(11) Cu(2) 0.01602(19) 0.0270(2) 0.0187(2) 0.0000 0.00819(17) 0.0000 F(1) 0.0280(8) 0.0600(11) 0.0631(12) 0.0057(8) 0.0237(8) 0.0345(9) F(2) 0.0227(7) 0.0598(11) 0.0308(8) 0.0015(7) 0.0145(7) 0.0148(7) F(3) 0.0364(19) 0.030(2) 0.0336(18) -0.0093(18) 0.0220(16) -0.0142(18) F(4) 0.063(2) 0.0422(17) 0.037(2) -0.005(2) 0.038(2) -0.0052(18) F(5) 0.0310(14) 0.106(3) 0.0520(18) -0.0080(17) 0.0254(13) -0.021(2) F(6) 0.085(2) 0.0246(12) 0.057(2) -0.0054(16) 0.054(2) -0.0037(13) F(7) 0.086(6) 0.049(4) 0.062(7) -0.034(4) 0.057(6) -0.021(4) F(8) 0.081(8) 0.034(4) 0.061(10) -0.012(8) 0.060(7) -0.010(6) F(9) 0.052(7) 0.041(10) 0.056(8) -0.009(7) 0.018(6) -0.024(7) F(10) 0.048(5) 0.086(6) 0.063(5) 0.012(5) 0.031(4) 0.007(5) N(1) 0.0261(10) 0.0226(9) 0.0219(10) 0.0006(8) 0.0161(9) 0.0014(8) N(2) 0.0195(9) 0.0224(9) 0.0182(9) 0.0003(7) 0.0116(8) 0.0003(7) N(3) 0.0184(9) 0.0204(9) 0.0184(9) -0.0024(7) 0.0109(8) -0.0016(7) N(4) 0.0212(9) 0.0202(9) 0.0192(9) -0.0017(7) 0.0129(8) -0.0014(7) C(1) 0.0241(12) 0.0301(13) 0.0270(13) -0.0024(9) 0.0159(11) 0.0026(10) C(2) 0.0229(11) 0.0263(12) 0.0190(11) 0.0016(9) 0.0133(10) 0.0026(9) C(3) 0.0216(11) 0.0279(12) 0.0242(12) -0.0010(9) 0.0124(10) 0.0033(9) C(4) 0.0207(10) 0.0209(11) 0.0185(11) 0.0004(8) 0.0133(9) -0.0001(8) C(5) 0.0192(10) 0.0210(11) 0.0181(11) -0.0009(8) 0.0122(9) -0.0019(8) C(6) 0.0180(10) 0.0265(12) 0.0226(11) -0.0003(9) 0.0123(10) 0.0017(9) C(7) 0.0192(10) 0.0265(12) 0.0198(11) 0.0016(9) 0.0111(9) 0.0026(9) C(8) 0.0182(10) 0.0230(11) 0.0178(11) -0.0027(8) 0.0101(9) -0.0019(8) C(9) 0.090(2) 0.0357(16) 0.068(2) 0.0283(17) 0.065(2) 0.0125(15) C(10) 0.084(2) 0.0303(15) 0.068(2) 0.0274(16) 0.061(2) 0.0222(15) B(1) 0.0155(17) 0.034(2) 0.025(2) 0.0000 0.0103(16) 0.0000 B(2) 0.0353(16) 0.0320(15) 0.0298(16) -0.0080(12) 0.0227(14) -0.0100(12) #============================================================================== # 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(1) 2.006(2) yes . . Cu(1) N(4) 2.003(3) yes . 4_564 Cu(2) N(2) 2.034(2) yes . . Cu(2) N(2) 2.034(2) yes . 2_656 Cu(2) N(3) 2.0017(16) yes . . Cu(2) N(3) 2.0017(16) yes . 2_656 F(3) F(9) 0.41(2) yes . . F(3) B(2) 1.400(6) yes . . F(4) F(8) 0.555(15) yes . . F(4) B(2) 1.377(10) yes . . F(5) F(7) 1.663(16) yes . . F(5) F(10) 0.901(17) yes . . F(5) B(2) 1.372(5) yes . . F(6) F(7) 0.761(16) yes . . F(6) B(2) 1.407(4) yes . . F(7) B(2) 1.244(14) yes . . F(8) B(2) 1.43(3) yes . . F(9) B(2) 1.36(2) yes . . F(10) B(2) 1.433(14) yes . . N(1) C(1) 1.342(2) yes . . C(1) H(1) 0.930 yes . . C(2) H(2) 0.930 yes . . C(3) C(4) 1.382(4) yes . . C(3) H(3) 0.930 yes . . C(4) C(5) 1.479(4) yes . . C(5) C(6) 1.383(2) yes . . C(6) C(7) 1.378(4) yes . . C(6) H(4) 0.930 yes . . C(7) H(5) 0.930 yes . . C(8) H(6) 0.930 yes . . C(9) C(10) 1.370(9) yes . . C(9) H(7) 0.970 yes . . C(9) H(8) 0.970 yes . . C(10) H(9) 0.970 yes . . C(10) H(10) 0.970 yes . . 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(1) Cu(1) N(4) 100.91(10) yes . . 4_564 N(1) Cu(1) C(9) 108.02(18) yes . . . N(1) Cu(1) C(10) 147.6(2) yes . . . N(4) Cu(1) C(9) 149.65(15) yes 4_564 . . N(4) Cu(1) C(10) 110.49(18) yes 4_564 . . C(9) Cu(1) C(10) 39.8(2) yes . . . N(2) Cu(2) N(2) 119.46(8) yes . . 2_656 N(2) Cu(2) N(3) 81.47(9) yes . . . N(2) Cu(2) N(3) 126.69(11) yes . . 2_656 N(2) Cu(2) N(3) 126.69(11) yes 2_656 . . N(2) Cu(2) N(3) 81.47(9) yes 2_656 . 2_656 N(3) Cu(2) N(3) 127.08(7) yes . . 2_656 F(9) F(3) B(2) 76(3) yes . . . F(8) F(4) B(2) 84(3) yes . . . F(7) F(5) F(10) 120.7(13) yes . . . F(7) F(5) B(2) 47.2(6) yes . . . F(10) F(5) B(2) 74.9(10) yes . . . F(7) F(6) B(2) 61.8(10) yes . . . F(5) F(7) F(6) 134.7(12) yes . . . F(5) F(7) B(2) 54.0(5) yes . . . F(6) F(7) B(2) 85.6(13) yes . . . F(4) F(8) B(2) 73(3) yes . . . F(3) F(9) B(2) 87(3) yes . . . F(5) F(10) B(2) 67.7(9) yes . . . Cu(1) N(1) C(1) 122.9(2) yes . . . Cu(1) N(1) C(2) 120.07(14) yes . . . C(1) N(1) C(2) 117.0(2) yes . . . Cu(2) N(2) C(2) 128.83(14) yes . . . Cu(2) N(2) C(4) 113.4(2) yes . . . C(2) N(2) C(4) 117.4(2) yes . . . Cu(2) N(3) C(5) 114.47(18) yes . . . Cu(2) N(3) C(8) 128.09(17) yes . . . C(5) N(3) C(8) 117.40(17) yes . . . Cu(1) N(4) C(7) 123.18(16) yes 4_565 . . Cu(1) N(4) C(8) 118.3(2) yes 4_565 . . C(7) N(4) C(8) 117.2(2) yes . . . N(1) C(1) C(3) 121.8(2) yes . . . N(1) C(1) H(1) 119.1 yes . . . C(3) C(1) H(1) 119.1 yes . . . N(1) C(2) N(2) 125.12(17) yes . . . N(1) C(2) H(2) 117.4 yes . . . N(2) C(2) H(2) 117.4 yes . . . C(1) C(3) C(4) 117.72(19) yes . . . C(1) C(3) H(3) 121.1 yes . . . C(4) C(3) H(3) 121.1 yes . . . N(2) C(4) C(3) 120.9(2) yes . . . N(2) C(4) C(5) 115.3(2) yes . . . C(3) C(4) C(5) 123.76(17) yes . . . N(3) C(5) C(4) 115.15(17) yes . . . N(3) C(5) C(6) 121.0(2) yes . . . C(4) C(5) C(6) 123.8(2) yes . . . C(5) C(6) C(7) 117.5(2) yes . . . C(5) C(6) H(4) 121.3 yes . . . C(7) C(6) H(4) 121.2 yes . . . N(4) C(7) C(6) 121.62(18) yes . . . N(4) C(7) H(5) 119.2 yes . . . C(6) C(7) H(5) 119.2 yes . . . N(3) C(8) N(4) 125.1(2) yes . . . N(3) C(8) H(6) 117.4 yes . . . N(4) C(8) H(6) 117.4 yes . . . Cu(1) C(9) C(10) 70.0(2) yes . . . Cu(1) C(9) H(7) 116.6 yes . . . Cu(1) C(9) H(8) 116.6 yes . . . C(10) C(9) H(7) 116.6 yes . . . C(10) C(9) H(8) 116.7 yes . . . H(7) C(9) H(8) 113.6 yes . . . Cu(1) C(10) C(9) 70.3(2) yes . . . Cu(1) C(10) H(9) 116.6 yes . . . Cu(1) C(10) H(10) 116.6 yes . . . C(9) C(10) H(9) 116.6 yes . . . C(9) C(10) H(10) 116.6 yes . . . H(9) C(10) H(10) 113.6 yes . . . F(1) B(1) F(1) 112.2(3) yes . . 2_656 F(1) B(1) F(2) 108.53(10) yes . . . F(1) B(1) F(2) 109.98(13) yes . . 2_656 F(1) B(1) F(2) 109.98(13) yes 2_656 . . F(1) B(1) F(2) 108.53(10) yes 2_656 . 2_656 F(2) B(1) F(2) 107.5(2) yes . . 2_656 F(3) B(2) F(4) 111.7(6) yes . . . F(3) B(2) F(5) 108.9(5) yes . . . F(3) B(2) F(6) 108.0(3) yes . . . F(3) B(2) F(7) 131.3(8) yes . . . F(3) B(2) F(8) 97.0(8) yes . . . F(3) B(2) F(9) 17.0(8) yes . . . F(3) B(2) F(10) 90.4(5) yes . . . F(4) B(2) F(5) 108.8(3) yes . . . F(4) B(2) F(6) 110.3(5) yes . . . F(4) B(2) F(7) 110.5(10) yes . . . F(4) B(2) F(8) 22.7(5) yes . . . F(4) B(2) F(9) 119.4(18) yes . . . F(4) B(2) F(10) 87.2(8) yes . . . F(5) B(2) F(6) 109.0(4) yes . . . F(5) B(2) F(7) 78.8(9) yes . . . F(5) B(2) F(8) 131.2(6) yes . . . F(5) B(2) F(9) 116.6(18) yes . . . F(5) B(2) F(10) 37.4(7) yes . . . F(6) B(2) F(7) 32.6(7) yes . . . F(6) B(2) F(8) 100.6(9) yes . . . F(6) B(2) F(9) 91.0(8) yes . . . F(6) B(2) F(10) 146.4(7) yes . . . F(7) B(2) F(8) 113.8(14) yes . . . F(7) B(2) F(9) 115.9(12) yes . . . F(7) B(2) F(10) 115.0(10) yes . . . F(8) B(2) F(9) 100.3(19) yes . . . F(8) B(2) F(10) 104.8(10) yes . . . F(9) B(2) F(10) 105.4(12) yes . . . 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(1) Cu(1) N(4) C(7) -73.5(2) ? . . 4_564 4_564 N(1) Cu(1) N(4) C(8) 92.75(19) ? . . 4_564 4_564 N(4) Cu(1) N(1) C(1) 86.3(2) ? 4_564 . . . N(4) Cu(1) N(1) C(2) -90.2(2) ? 4_564 . . . N(1) Cu(1) C(9) C(10) -176.02(19) ? . . . . N(1) Cu(1) C(9) H(7) -65.5 ? . . . . N(1) Cu(1) C(9) H(8) 73.4 ? . . . . C(9) Cu(1) N(1) C(1) -103.0(2) ? . . . . C(9) Cu(1) N(1) C(2) 80.5(2) ? . . . . N(1) Cu(1) C(10) C(9) 7.1(3) ? . . . . N(1) Cu(1) C(10) H(9) 117.7 ? . . . . N(1) Cu(1) C(10) H(10) -103.6 ? . . . . C(10) Cu(1) N(1) C(1) -107.7(3) ? . . . . C(10) Cu(1) N(1) C(2) 75.8(3) ? . . . . N(4) Cu(1) C(9) C(10) -14.3(3) ? 4_564 . . . N(4) Cu(1) C(9) H(7) 96.3 ? 4_564 . . . N(4) Cu(1) C(9) H(8) -124.8 ? 4_564 . . . C(9) Cu(1) N(4) C(7) 124.1(3) ? . . 4_564 4_564 C(9) Cu(1) N(4) C(8) -69.6(3) ? . . 4_564 4_564 N(4) Cu(1) C(10) C(9) 172.35(19) ? 4_564 . . . N(4) Cu(1) C(10) H(9) -77.0 ? 4_564 . . . N(4) Cu(1) C(10) H(10) 61.7 ? 4_564 . . . C(10) Cu(1) N(4) C(7) 114.4(2) ? . . 4_564 4_564 C(10) Cu(1) N(4) C(8) -79.3(2) ? . . 4_564 4_564 C(9) Cu(1) C(10) H(9) 110.6 ? . . . . C(9) Cu(1) C(10) H(10) -110.6 ? . . . . C(10) Cu(1) C(9) H(7) 110.6 ? . . . . C(10) Cu(1) C(9) H(8) -110.5 ? . . . . N(2) Cu(2) N(2) C(2) -47.7(3) ? . . 2_656 2_656 N(2) Cu(2) N(2) C(4) 125.2(2) ? . . 2_656 2_656 N(2) Cu(2) N(2) C(2) -47.7(3) ? 2_656 . . . N(2) Cu(2) N(2) C(4) 125.2(2) ? 2_656 . . . N(2) Cu(2) N(3) C(5) -0.7(2) ? . . . . N(2) Cu(2) N(3) C(8) 176.9(2) ? . . . . N(3) Cu(2) N(2) C(2) -175.3(2) ? . . . . N(3) Cu(2) N(2) C(4) -2.4(2) ? . . . . N(2) Cu(2) N(3) C(5) -121.3(2) ? . . 2_656 2_656 N(2) Cu(2) N(3) C(8) 56.3(2) ? . . 2_656 2_656 N(3) Cu(2) N(2) C(2) 54.3(3) ? 2_656 . . . N(3) Cu(2) N(2) C(4) -132.8(2) ? 2_656 . . . N(2) Cu(2) N(3) C(5) -121.3(2) ? 2_656 . . . N(2) Cu(2) N(3) C(8) 56.3(2) ? 2_656 . . . N(3) Cu(2) N(2) C(2) 54.3(3) ? . . 2_656 2_656 N(3) Cu(2) N(2) C(4) -132.8(2) ? . . 2_656 2_656 N(2) Cu(2) N(3) C(5) -0.7(2) ? 2_656 . 2_656 2_656 N(2) Cu(2) N(3) C(8) 176.9(2) ? 2_656 . 2_656 2_656 N(3) Cu(2) N(2) C(2) -175.3(2) ? 2_656 . 2_656 2_656 N(3) Cu(2) N(2) C(4) -2.4(2) ? 2_656 . 2_656 2_656 N(3) Cu(2) N(3) C(5) 129.4(2) ? . . 2_656 2_656 N(3) Cu(2) N(3) C(8) -53.1(3) ? . . 2_656 2_656 N(3) Cu(2) N(3) C(5) 129.4(2) ? 2_656 . . . N(3) Cu(2) N(3) C(8) -53.1(3) ? 2_656 . . . F(9) F(3) B(2) F(4) 120(6) ? . . . . F(9) F(3) B(2) F(5) -120(6) ? . . . . F(9) F(3) B(2) F(6) -1(5) ? . . . . F(9) F(3) B(2) F(7) -28(7) ? . . . . F(9) F(3) B(2) F(8) 102(6) ? . . . . F(9) F(3) B(2) F(10) -153(6) ? . . . . F(8) F(4) B(2) F(3) -52(2) ? . . . . F(8) F(4) B(2) F(5) -172(2) ? . . . . F(8) F(4) B(2) F(6) 68(2) ? . . . . F(8) F(4) B(2) F(7) 103(2) ? . . . . F(8) F(4) B(2) F(9) -35(2) ? . . . . F(8) F(4) B(2) F(10) -141(2) ? . . . . F(7) F(5) F(10) B(2) 12.0(9) ? . . . . F(10) F(5) F(7) F(6) -47(3) ? . . . . F(10) F(5) F(7) B(2) -15.8(13) ? . . . . F(7) F(5) B(2) F(3) 130.0(10) ? . . . . F(7) F(5) B(2) F(4) -108.0(9) ? . . . . F(7) F(5) B(2) F(6) 12.3(9) ? . . . . F(7) F(5) B(2) F(8) -111.8(14) ? . . . . F(7) F(5) B(2) F(9) 113.5(15) ? . . . . F(7) F(5) B(2) F(10) -166.0(13) ? . . . . B(2) F(5) F(7) F(6) -32(2) ? . . . . F(10) F(5) B(2) F(3) -64.1(10) ? . . . . F(10) F(5) B(2) F(4) 58.0(10) ? . . . . F(10) F(5) B(2) F(6) 178.3(10) ? . . . . F(10) F(5) B(2) F(7) 166.0(13) ? . . . . F(10) F(5) B(2) F(8) 54.1(15) ? . . . . F(10) F(5) B(2) F(9) -80.5(15) ? . . . . F(7) F(6) B(2) F(3) -141(2) ? . . . . F(7) F(6) B(2) F(4) 97(2) ? . . . . F(7) F(6) B(2) F(5) -23(2) ? . . . . F(7) F(6) B(2) F(8) 118(2) ? . . . . F(7) F(6) B(2) F(9) -141(2) ? . . . . F(7) F(6) B(2) F(10) -21(2) ? . . . . B(2) F(6) F(7) F(5) 25(2) ? . . . . F(5) F(7) B(2) F(3) -105.4(11) ? . . . . F(5) F(7) B(2) F(4) 106.0(5) ? . . . . F(5) F(7) B(2) F(6) -158.0(19) ? . . . . F(5) F(7) B(2) F(8) 130.3(7) ? . . . . F(5) F(7) B(2) F(9) -114(2) ? . . . . F(5) F(7) B(2) F(10) 9.4(9) ? . . . . F(6) F(7) B(2) F(3) 53(2) ? . . . . F(6) F(7) B(2) F(4) -95.9(16) ? . . . . F(6) F(7) B(2) F(5) 158.0(19) ? . . . . F(6) F(7) B(2) F(8) -71.7(18) ? . . . . F(6) F(7) B(2) F(9) 44(2) ? . . . . F(6) F(7) B(2) F(10) 167.4(15) ? . . . . F(4) F(8) B(2) F(3) 132(2) ? . . . . F(4) F(8) B(2) F(5) 9(2) ? . . . . F(4) F(8) B(2) F(6) -118(2) ? . . . . F(4) F(8) B(2) F(7) -86(2) ? . . . . F(4) F(8) B(2) F(9) 149(2) ? . . . . F(4) F(8) B(2) F(10) 40(2) ? . . . . F(3) F(9) B(2) F(4) -67(6) ? . . . . F(3) F(9) B(2) F(5) 67(6) ? . . . . F(3) F(9) B(2) F(6) 179(4) ? . . . . F(3) F(9) B(2) F(7) 157(5) ? . . . . F(3) F(9) B(2) F(8) -80(6) ? . . . . F(3) F(9) B(2) F(10) 28(7) ? . . . . F(5) F(10) B(2) F(3) 121.7(9) ? . . . . F(5) F(10) B(2) F(4) -126.5(8) ? . . . . F(5) F(10) B(2) F(6) -3.0(17) ? . . . . F(5) F(10) B(2) F(7) -15.2(15) ? . . . . F(5) F(10) B(2) F(8) -140.9(10) ? . . . . F(5) F(10) B(2) F(9) 113.8(19) ? . . . . Cu(1) N(1) C(1) C(3) -176.1(2) ? . . . . Cu(1) N(1) C(1) H(1) 3.9 ? . . . . Cu(1) N(1) C(2) N(2) 178.1(2) ? . . . . Cu(1) N(1) C(2) H(2) -1.9 ? . . . . C(1) N(1) C(2) N(2) 1.4(5) ? . . . . C(1) N(1) C(2) H(2) -178.6 ? . . . . C(2) N(1) C(1) C(3) 0.5(5) ? . . . . C(2) N(1) C(1) H(1) -179.5 ? . . . . Cu(2) N(2) C(2) N(1) 170.7(2) ? . . . . Cu(2) N(2) C(2) H(2) -9.3 ? . . . . Cu(2) N(2) C(4) C(3) -173.1(2) ? . . . . Cu(2) N(2) C(4) C(5) 4.8(3) ? . . . . C(2) N(2) C(4) C(3) 0.7(4) ? . . . . C(2) N(2) C(4) C(5) 178.6(2) ? . . . . C(4) N(2) C(2) N(1) -2.0(5) ? . . . . C(4) N(2) C(2) H(2) 178.1 ? . . . . Cu(2) N(3) C(5) C(4) 3.4(3) ? . . . . Cu(2) N(3) C(5) C(6) -178.7(2) ? . . . . Cu(2) N(3) C(8) N(4) -176.8(2) ? . . . . Cu(2) N(3) C(8) H(6) 3.2 ? . . . . C(5) N(3) C(8) N(4) 0.7(4) ? . . . . C(5) N(3) C(8) H(6) -179.3 ? . . . . C(8) N(3) C(5) C(4) -174.4(2) ? . . . . C(8) N(3) C(5) C(6) 3.5(4) ? . . . . Cu(1) N(4) C(7) C(6) -163.5(2) ? 4_565 . . . Cu(1) N(4) C(7) H(5) 16.5 ? 4_565 . . . Cu(1) N(4) C(8) N(3) 163.2(2) ? 4_565 . . . Cu(1) N(4) C(8) H(6) -16.8 ? 4_565 . . . C(7) N(4) C(8) N(3) -3.9(4) ? . . . . C(7) N(4) C(8) H(6) 176.1 ? . . . . C(8) N(4) C(7) C(6) 2.9(4) ? . . . . C(8) N(4) C(7) H(5) -177.0 ? . . . . N(1) C(1) C(3) C(4) -1.6(5) ? . . . . N(1) C(1) C(3) H(3) 178.4 ? . . . . H(1) C(1) C(3) C(4) 178.4 ? . . . . H(1) C(1) C(3) H(3) -1.6 ? . . . . C(1) C(3) C(4) N(2) 1.0(5) ? . . . . C(1) C(3) C(4) C(5) -176.7(3) ? . . . . H(3) C(3) C(4) N(2) -179.0 ? . . . . H(3) C(3) C(4) C(5) 3.4 ? . . . . N(2) C(4) C(5) N(3) -5.5(4) ? . . . . N(2) C(4) C(5) C(6) 176.6(3) ? . . . . C(3) C(4) C(5) N(3) 172.3(3) ? . . . . C(3) C(4) C(5) C(6) -5.6(5) ? . . . . N(3) C(5) C(6) C(7) -4.3(4) ? . . . . N(3) C(5) C(6) H(4) 175.7 ? . . . . C(4) C(5) C(6) C(7) 173.5(2) ? . . . . C(4) C(5) C(6) H(4) -6.6 ? . . . . C(5) C(6) C(7) N(4) 1.0(4) ? . . . . C(5) C(6) C(7) H(5) -179.0 ? . . . . H(4) C(6) C(7) N(4) -179.0 ? . . . . H(4) C(6) C(7) H(5) 1.0 ? . . . . Cu(1) C(9) C(10) H(9) -110.6 ? . . . . Cu(1) C(9) C(10) H(10) 110.6 ? . . . . H(7) C(9) C(10) Cu(1) -110.5 ? . . . . H(7) C(9) C(10) H(9) 138.9 ? . . . . H(7) C(9) C(10) H(10) 0.1 ? . . . . H(8) C(9) C(10) Cu(1) 110.6 ? . . . . H(8) C(9) C(10) H(9) -0.0 ? . . . . H(8) C(9) C(10) H(10) -138.8 ? . . . . 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(3) 2.457(7) ? . . Cu(1) F(8) 3.573(15) ? . . Cu(1) F(9) 2.43(2) ? . . Cu(1) C(2) 2.917(3) ? . . Cu(1) C(7) 2.960(3) ? . 4_564 Cu(1) C(8) 2.887(3) ? . 4_564 Cu(1) C(9) 2.017(4) ? . . Cu(1) C(10) 2.013(2) ? . . Cu(1) H(2) 2.919 ? . . Cu(1) H(5) 3.038 ? . 4_564 Cu(1) H(6) 2.894 ? . 4_564 Cu(1) H(7) 2.601 ? . . Cu(1) H(8) 2.601 ? . . Cu(1) H(9) 2.596 ? . . Cu(1) H(10) 2.596 ? . . Cu(2) C(2) 3.050(3) ? . . Cu(2) C(2) 3.050(3) ? . 2_656 Cu(2) C(4) 2.854(2) ? . . Cu(2) C(4) 2.854(2) ? . 2_656 Cu(2) C(5) 2.8429(18) ? . . Cu(2) C(5) 2.8429(18) ? . 2_656 Cu(2) C(8) 3.009(2) ? . . Cu(2) C(8) 3.009(2) ? . 2_656 Cu(2) H(2) 3.134 ? . . Cu(2) H(2) 3.134 ? . 2_656 Cu(2) H(6) 3.085 ? . . Cu(2) H(6) 3.085 ? . 2_656 F(1) F(1) 2.277(4) ? . 2_656 F(1) F(2) 2.274(2) ? . 2_656 F(1) C(6) 3.164(2) ? . 7_657 F(1) C(7) 3.287(3) ? . 7_657 F(1) C(8) 3.215(2) ? . 2_656 F(1) B(1) 1.371(3) ? . . F(1) H(4) 2.505 ? . 7_657 F(1) H(5) 2.732 ? . 7_657 F(1) H(6) 3.552 ? . . F(1) H(6) 2.584 ? . 2_656 F(1) H(7) 3.437 ? . 1_545 F(1) H(8) 3.208 ? . 1_545 F(1) H(10) 3.153 ? . 3_666 F(2) F(1) 2.274(2) ? . 2_656 F(2) F(2) 2.2646(18) ? . 2_656 F(2) C(3) 3.273(2) ? . 7_657 F(2) C(6) 3.229(3) ? . 7_657 F(2) C(9) 3.557(6) ? . 1_545 F(2) C(9) 3.415(6) ? . 2_646 F(2) C(10) 3.289(6) ? . 4_565 F(2) B(1) 1.404(2) ? . . F(2) H(3) 2.365 ? . 7_657 F(2) H(4) 2.301 ? . 7_657 F(2) H(7) 3.210 ? . 1_545 F(2) H(7) 2.668 ? . 2_646 F(2) H(8) 3.060 ? . 1_545 F(2) H(8) 3.489 ? . 2_646 F(2) H(9) 3.210 ? . 4_565 F(2) H(10) 2.754 ? . 4_565 F(3) Cu(1) 2.457(7) ? . . F(3) F(4) 2.299(12) ? . . F(3) F(5) 2.256(7) ? . . F(3) F(6) 2.272(7) ? . . F(3) F(7) 2.410(13) ? . . F(3) F(8) 2.12(2) ? . . F(3) F(10) 2.010(11) ? . . F(3) N(1) 3.221(10) ? . . F(3) N(4) 3.064(6) ? . 4_564 F(3) C(1) 3.111(10) ? . . F(3) C(7) 2.939(8) ? . 4_564 F(3) C(9) 3.478(10) ? . . F(3) C(10) 3.379(7) ? . . F(3) H(1) 2.432 ? . . F(3) H(5) 2.266 ? . 4_564 F(3) H(8) 3.371 ? . . F(3) H(9) 3.203 ? . . F(4) F(3) 2.299(12) ? . . F(4) F(5) 2.235(10) ? . . F(4) F(6) 2.284(9) ? . . F(4) F(7) 2.15(2) ? . . F(4) F(9) 2.36(3) ? . . F(4) F(10) 1.94(2) ? . . F(4) N(2) 3.243(9) ? . 7_667 F(4) N(3) 3.321(8) ? . 7_667 F(4) C(1) 3.409(7) ? . . F(4) C(2) 3.556(5) ? . 8_565 F(4) C(3) 3.503(10) ? . 7_667 F(4) C(4) 2.999(9) ? . 7_667 F(4) C(5) 3.109(8) ? . 7_667 F(4) H(1) 2.634 ? . . F(4) H(2) 2.701 ? . 8_565 F(5) F(3) 2.256(7) ? . . F(5) F(4) 2.235(10) ? . . F(5) F(6) 2.264(6) ? . . F(5) F(7) 3.178(15) ? . 3_777 F(5) F(8) 2.55(2) ? . . F(5) F(9) 2.33(2) ? . . F(5) C(2) 3.234(4) ? . 8_565 F(5) C(8) 3.038(6) ? . 5_555 F(5) H(2) 2.428 ? . 8_565 F(5) H(6) 2.392 ? . 5_555 F(6) F(3) 2.272(7) ? . . F(6) F(4) 2.284(9) ? . . F(6) F(5) 2.264(6) ? . . F(6) F(8) 2.18(2) ? . . F(6) F(9) 1.98(2) ? . . F(6) F(10) 2.719(14) ? . . F(6) N(1) 3.047(6) ? . 6_656 F(6) N(2) 3.349(9) ? . 6_656 F(6) N(3) 3.230(6) ? . 7_667 F(6) N(4) 3.097(4) ? . 7_667 F(6) C(1) 3.363(5) ? . 6_656 F(6) C(2) 3.006(8) ? . 6_656 F(6) C(5) 3.263(8) ? . 7_667 F(6) C(6) 3.298(8) ? . 7_667 F(6) C(7) 3.190(6) ? . 7_667 F(6) C(8) 3.124(5) ? . 7_667 F(6) H(2) 3.281 ? . 6_656 F(6) H(6) 3.596 ? . 7_667 F(6) H(8) 3.257 ? . . F(6) H(9) 3.113 ? . . F(7) F(3) 2.410(13) ? . . F(7) F(4) 2.15(2) ? . . F(7) F(5) 3.178(15) ? . 3_777 F(7) F(7) 3.55(2) ? . 3_777 F(7) F(8) 2.24(3) ? . . F(7) F(9) 2.21(2) ? . . F(7) F(10) 2.260(19) ? . . F(7) N(1) 3.265(15) ? . 6_656 F(7) N(2) 3.25(2) ? . 6_656 F(7) N(3) 3.17(2) ? . 7_667 F(7) N(4) 3.344(15) ? . 7_667 F(7) C(2) 2.94(2) ? . 6_656 F(7) C(5) 3.45(2) ? . 7_667 F(7) C(8) 3.099(16) ? . 7_667 F(7) H(2) 3.030 ? . 6_656 F(7) H(2) 3.263 ? . 8_565 F(7) H(6) 3.410 ? . 7_667 F(8) Cu(1) 3.573(15) ? . . F(8) F(3) 2.12(2) ? . . F(8) F(5) 2.55(2) ? . . F(8) F(6) 2.18(2) ? . . F(8) F(7) 2.24(3) ? . . F(8) F(9) 2.14(4) ? . . F(8) F(10) 2.27(3) ? . . F(8) N(2) 3.39(2) ? . 7_667 F(8) N(3) 3.41(2) ? . 7_667 F(8) C(1) 3.191(19) ? . . F(8) C(3) 3.27(2) ? . 7_667 F(8) C(4) 2.92(2) ? . 7_667 F(8) C(5) 3.00(2) ? . 7_667 F(8) C(6) 3.50(2) ? . 7_667 F(8) H(1) 2.500 ? . . F(8) H(2) 3.254 ? . 8_565 F(8) H(3) 3.491 ? . 7_667 F(8) H(8) 3.082 ? . . F(9) Cu(1) 2.43(2) ? . . F(9) F(4) 2.36(3) ? . . F(9) F(5) 2.33(2) ? . . F(9) F(6) 1.98(2) ? . . F(9) F(7) 2.21(2) ? . . F(9) F(8) 2.14(4) ? . . F(9) F(10) 2.22(2) ? . . F(9) N(1) 3.41(3) ? . . F(9) N(4) 3.14(2) ? . 4_564 F(9) C(1) 3.40(3) ? . . F(9) C(7) 3.11(2) ? . 4_564 F(9) C(9) 3.27(3) ? . . F(9) C(10) 3.10(2) ? . . F(9) H(1) 2.759 ? . . F(9) H(5) 2.483 ? . 4_564 F(9) H(8) 3.134 ? . . F(9) H(9) 2.851 ? . . F(10) F(3) 2.010(11) ? . . F(10) F(4) 1.94(2) ? . . F(10) F(6) 2.719(14) ? . . F(10) F(7) 2.260(19) ? . . F(10) F(8) 2.27(3) ? . . F(10) F(9) 2.22(2) ? . . F(10) C(2) 3.272(9) ? . 8_565 F(10) C(8) 3.359(18) ? . 5_555 F(10) H(1) 2.912 ? . . F(10) H(2) 2.380 ? . 8_565 F(10) H(5) 3.317 ? . 4_564 F(10) H(6) 2.592 ? . 5_555 N(1) F(3) 3.221(10) ? . . N(1) F(6) 3.047(6) ? . 6_646 N(1) F(7) 3.265(15) ? . 6_646 N(1) F(9) 3.41(3) ? . . N(1) C(2) 1.340(3) ? . . N(1) C(3) 2.374(3) ? . . N(1) C(4) 2.727(3) ? . . N(1) C(9) 3.255(3) ? . . N(1) H(2) 1.951 ? . . N(1) H(3) 3.212 ? . . N(1) H(7) 3.529 ? . . N(1) H(8) 3.589 ? . . N(2) F(4) 3.243(9) ? . 7_667 N(2) F(6) 3.349(9) ? . 6_646 N(2) F(7) 3.25(2) ? . 6_646 N(2) F(8) 3.39(2) ? . 7_667 N(2) C(2) 1.331(3) ? . . N(2) C(3) 2.378(2) ? . . N(2) C(4) 1.351(2) ? . . N(2) C(5) 2.391(3) ? . . N(2) H(2) 1.944 ? . . N(2) H(3) 3.219 ? . . N(3) F(4) 3.321(8) ? . 7_667 N(3) F(6) 3.230(6) ? . 7_667 N(3) F(7) 3.17(2) ? . 7_667 N(3) F(8) 3.41(2) ? . 7_667 N(3) C(4) 2.391(4) ? . . N(3) C(5) 1.353(3) ? . . N(3) C(6) 2.381(2) ? . . N(3) C(7) 2.718(2) ? . . N(3) C(8) 1.329(4) ? . . N(3) H(4) 3.222 ? . . N(3) H(6) 1.941 ? . . N(4) F(3) 3.064(6) ? . 4_565 N(4) F(6) 3.097(4) ? . 7_667 N(4) F(7) 3.344(15) ? . 7_667 N(4) F(9) 3.14(2) ? . 4_565 N(4) C(5) 2.722(4) ? . . N(4) C(6) 2.377(4) ? . . N(4) C(7) 1.344(3) ? . . N(4) C(8) 1.337(2) ? . . N(4) C(10) 3.299(4) ? . 4_565 N(4) H(4) 3.216 ? . . N(4) H(5) 1.973 ? . . N(4) H(6) 1.949 ? . . N(4) H(10) 3.555 ? . 4_565 C(1) F(3) 3.111(10) ? . . C(1) F(4) 3.409(7) ? . . C(1) F(6) 3.363(5) ? . 6_646 C(1) F(8) 3.191(19) ? . . C(1) F(9) 3.40(3) ? . . C(1) C(2) 2.286(3) ? . . C(1) C(3) 1.375(4) ? . . C(1) C(4) 2.360(4) ? . . C(1) H(2) 3.120 ? . . C(1) H(3) 2.019 ? . . C(1) H(9) 3.043 ? . 6_646 C(2) Cu(1) 2.917(3) ? . . C(2) Cu(2) 3.050(3) ? . . C(2) F(4) 3.556(5) ? . 8_464 C(2) F(5) 3.234(4) ? . 8_464 C(2) F(6) 3.006(8) ? . 6_646 C(2) F(7) 2.94(2) ? . 6_646 C(2) F(10) 3.272(10) ? . 8_464 C(2) N(1) 1.340(3) ? . . C(2) N(2) 1.331(3) ? . . C(2) C(1) 2.286(3) ? . . C(2) C(3) 2.674(2) ? . . C(2) C(4) 2.292(3) ? . . C(2) H(1) 3.130 ? . . C(3) F(2) 3.273(2) ? . 7_657 C(3) F(4) 3.503(10) ? . 7_667 C(3) F(8) 3.27(2) ? . 7_667 C(3) N(1) 2.374(3) ? . . C(3) N(2) 2.378(2) ? . . C(3) C(1) 1.375(4) ? . . C(3) C(2) 2.674(2) ? . . C(3) C(5) 2.524(4) ? . . C(3) C(6) 3.018(4) ? . . C(3) H(1) 2.000 ? . . C(3) H(4) 2.769 ? . . C(3) H(9) 2.865 ? . 6_646 C(4) Cu(2) 2.854(2) ? . . C(4) F(4) 2.999(9) ? . 7_667 C(4) F(8) 2.92(2) ? . 7_667 C(4) N(1) 2.727(3) ? . . C(4) N(2) 1.351(2) ? . . C(4) N(3) 2.391(4) ? . . C(4) C(1) 2.360(4) ? . . C(4) C(2) 2.292(3) ? . . C(4) C(6) 2.525(3) ? . . C(4) H(1) 3.201 ? . . C(4) H(2) 3.126 ? . . C(4) H(3) 2.026 ? . . C(4) H(4) 2.725 ? . . C(5) Cu(2) 2.8429(18) ? . . C(5) F(4) 3.109(8) ? . 7_667 C(5) F(6) 3.263(8) ? . 7_667 C(5) F(7) 3.45(2) ? . 7_667 C(5) F(8) 3.00(2) ? . 7_667 C(5) N(2) 2.391(3) ? . . C(5) N(3) 1.353(3) ? . . C(5) N(4) 2.722(4) ? . . C(5) C(3) 2.524(4) ? . . C(5) C(7) 2.360(3) ? . . C(5) C(8) 2.292(4) ? . . C(5) H(3) 2.720 ? . . C(5) H(4) 2.027 ? . . C(5) H(5) 3.202 ? . . C(5) H(6) 3.126 ? . . C(6) F(1) 3.164(2) ? . 7_657 C(6) F(2) 3.229(3) ? . 7_657 C(6) F(6) 3.298(8) ? . 7_667 C(6) F(8) 3.50(2) ? . 7_667 C(6) N(3) 2.381(2) ? . . C(6) N(4) 2.377(4) ? . . C(6) C(3) 3.018(4) ? . . C(6) C(4) 2.525(3) ? . . C(6) C(8) 2.678(4) ? . . C(6) H(3) 2.757 ? . . C(6) H(5) 2.004 ? . . C(6) H(8) 2.989 ? . 7_667 C(7) Cu(1) 2.960(3) ? . 4_565 C(7) F(1) 3.287(3) ? . 7_657 C(7) F(3) 2.939(8) ? . 4_565 C(7) F(6) 3.190(6) ? . 7_667 C(7) F(9) 3.11(2) ? . 4_565 C(7) N(3) 2.718(2) ? . . C(7) N(4) 1.344(3) ? . . C(7) C(5) 2.360(3) ? . . C(7) C(8) 2.288(2) ? . . C(7) H(4) 2.023 ? . . C(7) H(6) 3.121 ? . . C(7) H(8) 3.516 ? . 7_667 C(8) Cu(1) 2.887(3) ? . 4_565 C(8) Cu(2) 3.009(2) ? . . C(8) F(1) 3.215(2) ? . 2_656 C(8) F(5) 3.038(6) ? . 5_445 C(8) F(6) 3.124(5) ? . 7_667 C(8) F(7) 3.099(16) ? . 7_667 C(8) F(10) 3.359(18) ? . 5_445 C(8) N(3) 1.329(4) ? . . C(8) N(4) 1.337(2) ? . . C(8) C(5) 2.292(4) ? . . C(8) C(6) 2.678(4) ? . . C(8) C(7) 2.288(2) ? . . C(8) H(5) 3.131 ? . . C(9) Cu(1) 2.017(4) ? . . C(9) F(2) 3.557(6) ? . 1_565 C(9) F(2) 3.415(6) ? . 2_666 C(9) F(3) 3.478(10) ? . . C(9) F(9) 3.27(3) ? . . C(9) N(1) 3.255(3) ? . . C(9) H(4) 3.528 ? . 7_667 C(9) H(9) 2.002 ? . . C(9) H(10) 2.002 ? . . C(9) H(10) 3.089 ? . 3_676 C(10) Cu(1) 2.013(2) ? . . C(10) F(2) 3.289(6) ? . 4_564 C(10) F(3) 3.379(7) ? . . C(10) F(9) 3.10(2) ? . . C(10) N(4) 3.299(4) ? . 4_564 C(10) H(3) 3.419 ? . 6_656 C(10) H(7) 2.003 ? . . C(10) H(7) 3.511 ? . 3_676 C(10) H(8) 2.003 ? . . C(10) H(10) 2.868 ? . 3_676 B(1) F(1) 1.371(3) ? . . B(1) F(1) 1.371(3) ? . 2_656 B(1) F(2) 1.404(2) ? . . B(1) F(2) 1.404(2) ? . 2_656 B(1) H(4) 2.931 ? . 7_657 B(1) H(4) 2.931 ? . 8_454 B(1) H(6) 3.428 ? . . B(1) H(6) 3.428 ? . 2_656 B(1) H(7) 3.292 ? . 1_545 B(1) H(7) 3.292 ? . 2_646 B(1) H(8) 3.457 ? . 1_545 B(1) H(8) 3.457 ? . 2_646 B(1) H(10) 3.520 ? . 3_666 B(1) H(10) 3.520 ? . 4_565 B(2) H(1) 2.999 ? . . B(2) H(2) 3.091 ? . 8_565 B(2) H(5) 3.482 ? . 4_564 H(1) F(3) 2.432 ? . . H(1) F(4) 2.634 ? . . H(1) F(8) 2.500 ? . . H(1) F(9) 2.759 ? . . H(1) F(10) 2.912 ? . . H(1) C(2) 3.130 ? . . H(1) C(3) 2.000 ? . . H(1) C(4) 3.201 ? . . H(1) B(2) 2.999 ? . . H(1) H(3) 2.308 ? . . H(1) H(5) 3.328 ? . 4_564 H(1) H(9) 3.015 ? . 6_646 H(2) Cu(1) 2.919 ? . . H(2) Cu(2) 3.134 ? . . H(2) F(4) 2.701 ? . 8_464 H(2) F(5) 2.428 ? . 8_464 H(2) F(6) 3.281 ? . 6_646 H(2) F(7) 3.030 ? . 6_646 H(2) F(7) 3.263 ? . 8_464 H(2) F(8) 3.254 ? . 8_464 H(2) F(10) 2.380 ? . 8_464 H(2) N(1) 1.951 ? . . H(2) N(2) 1.944 ? . . H(2) C(1) 3.120 ? . . H(2) C(4) 3.126 ? . . H(2) B(2) 3.091 ? . 8_464 H(2) H(6) 3.574 ? . 4_564 H(2) H(7) 3.518 ? . . H(3) F(2) 2.365 ? . 7_657 H(3) F(8) 3.491 ? . 7_667 H(3) N(1) 3.212 ? . . H(3) N(2) 3.219 ? . . H(3) C(1) 2.019 ? . . H(3) C(4) 2.026 ? . . H(3) C(5) 2.720 ? . . H(3) C(6) 2.757 ? . . H(3) C(10) 3.419 ? . 6_646 H(3) H(1) 2.308 ? . . H(3) H(4) 2.248 ? . . H(3) H(8) 3.119 ? . 7_667 H(3) H(9) 2.699 ? . 6_646 H(3) H(10) 3.485 ? . 6_646 H(4) F(1) 2.505 ? . 7_657 H(4) F(2) 2.301 ? . 7_657 H(4) N(3) 3.222 ? . . H(4) N(4) 3.216 ? . . H(4) C(3) 2.769 ? . . H(4) C(4) 2.725 ? . . H(4) C(5) 2.027 ? . . H(4) C(7) 2.023 ? . . H(4) C(9) 3.528 ? . 7_667 H(4) B(1) 2.931 ? . 7_657 H(4) H(3) 2.248 ? . . H(4) H(5) 2.314 ? . . H(4) H(8) 2.620 ? . 7_667 H(5) Cu(1) 3.038 ? . 4_565 H(5) F(1) 2.732 ? . 7_657 H(5) F(3) 2.266 ? . 4_565 H(5) F(9) 2.483 ? . 4_565 H(5) F(10) 3.317 ? . 4_565 H(5) N(4) 1.973 ? . . H(5) C(5) 3.202 ? . . H(5) C(6) 2.004 ? . . H(5) C(8) 3.131 ? . . H(5) B(2) 3.482 ? . 4_565 H(5) H(1) 3.328 ? . 4_565 H(5) H(4) 2.314 ? . . H(5) H(8) 3.530 ? . 7_667 H(6) Cu(1) 2.894 ? . 4_565 H(6) Cu(2) 3.085 ? . . H(6) F(1) 3.552 ? . . H(6) F(1) 2.584 ? . 2_656 H(6) F(5) 2.392 ? . 5_445 H(6) F(6) 3.596 ? . 7_667 H(6) F(7) 3.410 ? . 7_667 H(6) F(10) 2.592 ? . 5_445 H(6) N(3) 1.941 ? . . H(6) N(4) 1.949 ? . . H(6) C(5) 3.126 ? . . H(6) C(7) 3.121 ? . . H(6) B(1) 3.428 ? . . H(6) H(2) 3.574 ? . 4_565 H(6) H(10) 3.379 ? . 4_565 H(7) Cu(1) 2.601 ? . . H(7) F(1) 3.437 ? . 1_565 H(7) F(2) 3.210 ? . 1_565 H(7) F(2) 2.668 ? . 2_666 H(7) N(1) 3.529 ? . . H(7) C(10) 2.003 ? . . H(7) C(10) 3.511 ? . 3_676 H(7) B(1) 3.292 ? . 1_565 H(7) H(2) 3.518 ? . . H(7) H(8) 1.624 ? . . H(7) H(9) 2.766 ? . . H(7) H(9) 3.551 ? . 3_676 H(7) H(10) 2.240 ? . . H(7) H(10) 2.734 ? . 3_676 H(8) Cu(1) 2.601 ? . . H(8) F(1) 3.208 ? . 1_565 H(8) F(2) 3.060 ? . 1_565 H(8) F(2) 3.489 ? . 2_666 H(8) F(3) 3.371 ? . . H(8) F(6) 3.257 ? . . H(8) F(8) 3.082 ? . . H(8) F(9) 3.134 ? . . H(8) N(1) 3.589 ? . . H(8) C(6) 2.989 ? . 7_667 H(8) C(7) 3.516 ? . 7_667 H(8) C(10) 2.003 ? . . H(8) B(1) 3.457 ? . 1_565 H(8) H(3) 3.119 ? . 7_667 H(8) H(4) 2.620 ? . 7_667 H(8) H(5) 3.530 ? . 7_667 H(8) H(7) 1.624 ? . . H(8) H(9) 2.240 ? . . H(8) H(10) 2.766 ? . . H(8) H(10) 3.551 ? . 3_676 H(9) Cu(1) 2.596 ? . . H(9) F(2) 3.210 ? . 4_564 H(9) F(3) 3.203 ? . . H(9) F(6) 3.113 ? . . H(9) F(9) 2.851 ? . . H(9) C(1) 3.043 ? . 6_656 H(9) C(3) 2.865 ? . 6_656 H(9) C(9) 2.002 ? . . H(9) H(1) 3.015 ? . 6_656 H(9) H(3) 2.699 ? . 6_656 H(9) H(7) 2.766 ? . . H(9) H(7) 3.551 ? . 3_676 H(9) H(8) 2.240 ? . . H(9) H(10) 1.623 ? . . H(9) H(10) 3.233 ? . 3_676 H(10) Cu(1) 2.596 ? . . H(10) F(1) 3.153 ? . 3_666 H(10) F(2) 2.754 ? . 4_564 H(10) N(4) 3.555 ? . 4_564 H(10) C(9) 2.002 ? . . H(10) C(9) 3.089 ? . 3_676 H(10) C(10) 2.868 ? . 3_676 H(10) B(1) 3.520 ? . 3_666 H(10) H(3) 3.485 ? . 6_656 H(10) H(6) 3.379 ? . 4_564 H(10) H(7) 2.240 ? . . H(10) H(7) 2.734 ? . 3_676 H(10) H(8) 2.766 ? . . H(10) H(8) 3.551 ? . 3_676 H(10) H(9) 1.623 ? . . H(10) H(9) 3.233 ? . 3_676 H(10) H(10) 2.306 ? . 3_676 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.436 _refine_diff_density_min -0.351 _refine_diff_density_rms 0.072