data_1LT-BF4 _audit_creation_method SHELXL-97 #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Takayuki Ishida' _publ_contact_author_address ; Department of Applied Physics and Chemistry, The University of Electro-Communications, Chofu, Tokyo 182-8585, Japan ; _publ_contact_author_email ' ishi@pc.uec.ac.jp ' _publ_contact_author_fax ' +81-42-443-5501 ' _publ_contact_author_phone ' +81-42-443-5490 ' _publ_requested_journal ' J. Am. Chem. Soc.' _publ_author_name ; Atsushi Okazawa Daisuke Hashizume Takayuki Ishida ; #============================================================================== data__[Cu(2pyNO-)(2pyNO.)]2(BF4-)2_50K #============================================================================== _chemical_melting_point '447 - 449 K' _chemical_formula_moiety 'C36 H52 Cu2 N8 O4, 2(B F4)' _chemical_formula_sum 'C36 H52 B2 Cu2 F8 N8 O4' _chemical_formula_weight 961.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0010 0.0012 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 6.1.1.4' 'B' 'B' 0.0000 0.0005 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' 'N' 'N' 0.0022 0.0024 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' 'O' 'O' 0.0046 0.0045 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' 'F' 'F' 0.0088 0.0076 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' 'Cu' 'Cu' 0.2770 0.9890 'International Tables Vol C Tables 6.1.1.4 and Sasaki (1989)' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 19.342(1) _cell_length_b 17.360(1) _cell_length_c 12.514(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4201.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 50 _cell_measurement_reflns_used 257087 _cell_measurement_theta_min 1.37 _cell_measurement_theta_max 43.34 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 0.761 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.71262 _exptl_absorpt_correction_T_max 0.77508 _exptl_absorpt_process_details 'MULABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 50 _diffrn_radiation_wavelength 0.61792 _diffrn_radiation_type 'synchrotron' _diffrn_radiation_source 'SPring-8 BL02B1 bending magnet' _diffrn_radiation_monochromator 'Si(111)' _diffrn_measurement_device_type 'MacScience Vacuum Camera' _diffrn_measurement_method '\w-scan' _diffrn_detector_area_resol_mean 10 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 178714 _diffrn_reflns_av_R_equivalents 0.0811 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 43.34 _reflns_number_total 23978 _reflns_number_gt 17579 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'DIP Xpress' _computing_cell_refinement 'DENZO/SCALEPACK' _computing_data_reduction 'DENZO/SCALEPACK' _computing_structure_solution 'SIR-2004' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2sigma(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^)+(0.0470P)^2^+1.8676P] 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 23978 _refine_ls_number_parameters 285 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0667 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1140 _refine_ls_wR_factor_gt 0.0937 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.005 _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 0.559713(5) 0.064289(5) -0.012825(7) 0.00834(2) Uani 1 1 d . . . O1 O 0.52763(3) 0.00562(3) 0.10499(4) 0.00982(7) Uani 1 1 d . . . O2 O 0.58287(3) 0.11220(3) -0.15200(4) 0.01309(8) Uani 1 1 d . . . N1 N 0.50943(3) 0.14533(3) 0.05772(4) 0.00977(7) Uani 1 1 d . . . N2 N 0.50221(3) 0.05063(3) 0.19006(4) 0.00877(7) Uani 1 1 d . . . N3 N 0.63304(3) -0.00495(3) -0.05829(4) 0.00935(7) Uani 1 1 d . . . N4 N 0.63797(3) 0.08258(3) -0.19547(5) 0.01001(7) Uani 1 1 d . . . C1 C 0.48748(3) 0.12543(4) 0.15676(5) 0.00881(8) Uani 1 1 d . . . C2 C 0.44626(4) 0.17668(4) 0.21660(6) 0.01135(9) Uani 1 1 d . . . H2 H 0.4307 0.1630 0.2861 0.014 Uiso 1 1 calc R . . C3 C 0.42885(4) 0.24695(4) 0.17265(6) 0.01333(10) Uani 1 1 d . . . H3 H 0.4016 0.2823 0.2125 0.016 Uiso 1 1 calc R . . C4 C 0.45110(4) 0.26654(4) 0.06947(7) 0.01455(11) Uani 1 1 d . . . H4 H 0.4392 0.3147 0.0384 0.017 Uiso 1 1 calc R . . C5 C 0.49072(4) 0.21394(4) 0.01478(6) 0.01289(10) Uani 1 1 d . . . H5 H 0.5055 0.2261 -0.0556 0.015 Uiso 1 1 calc R . . C6 C 0.54592(3) 0.03733(4) 0.28827(5) 0.01024(8) Uani 1 1 d . . . C7 C 0.61819(4) 0.07066(5) 0.27161(8) 0.01724(12) Uani 1 1 d . . . H7A H 0.6386 0.0486 0.2068 0.026 Uiso 1 1 calc R . . H7B H 0.6473 0.0580 0.3333 0.026 Uiso 1 1 calc R . . H7C H 0.6151 0.1267 0.2640 0.026 Uiso 1 1 calc R . . C8 C 0.55043(4) -0.04968(5) 0.30549(6) 0.01388(10) Uani 1 1 d . . . H8A H 0.5037 -0.0710 0.3125 0.021 Uiso 1 1 calc R . . H8B H 0.5768 -0.0603 0.3708 0.021 Uiso 1 1 calc R . . H8C H 0.5737 -0.0735 0.2443 0.021 Uiso 1 1 calc R . . C9 C 0.51223(5) 0.07393(5) 0.38654(6) 0.01621(12) Uani 1 1 d . . . H9A H 0.5154 0.1301 0.3813 0.024 Uiso 1 1 calc R . . H9B H 0.5362 0.0565 0.4512 0.024 Uiso 1 1 calc R . . H9C H 0.4635 0.0586 0.3901 0.024 Uiso 1 1 calc R . . C10 C 0.65755(3) 0.00984(4) -0.15744(5) 0.00986(8) Uani 1 1 d . . . C11 C 0.69657(4) -0.04380(4) -0.21441(6) 0.01269(10) Uani 1 1 d . . . H11 H 0.7117 -0.0334 -0.2852 0.015 Uiso 1 1 calc R . . C12 C 0.71255(4) -0.11298(4) -0.16412(6) 0.01325(10) Uani 1 1 d . . . H12 H 0.7393 -0.1506 -0.2005 0.016 Uiso 1 1 calc R . . C13 C 0.68941(4) -0.12740(4) -0.06038(6) 0.01289(10) Uani 1 1 d . . . H13 H 0.7015 -0.1736 -0.0243 0.015 Uiso 1 1 calc R . . C14 C 0.64819(4) -0.07230(4) -0.01133(6) 0.01128(9) Uani 1 1 d . . . H14 H 0.6301 -0.0826 0.0578 0.014 Uiso 1 1 calc R . . C15 C 0.67481(4) 0.12979(4) -0.27963(5) 0.01100(9) Uani 1 1 d . . . C16 C 0.65595(5) 0.21409(5) -0.25948(7) 0.01665(12) Uani 1 1 d . . . H16A H 0.6061 0.2211 -0.2690 0.025 Uiso 1 1 calc R . . H16B H 0.6809 0.2470 -0.3102 0.025 Uiso 1 1 calc R . . H16C H 0.6688 0.2282 -0.1863 0.025 Uiso 1 1 calc R . . C17 C 0.64809(5) 0.10479(6) -0.38965(6) 0.01791(13) Uani 1 1 d . . . H17A H 0.6585 0.0501 -0.4009 0.027 Uiso 1 1 calc R . . H17B H 0.6707 0.1355 -0.4453 0.027 Uiso 1 1 calc R . . H17C H 0.5980 0.1127 -0.3931 0.027 Uiso 1 1 calc R . . C18 C 0.75340(4) 0.11928(5) -0.26986(6) 0.01486(11) Uani 1 1 d . . . H18A H 0.7668 0.1213 -0.1944 0.022 Uiso 1 1 calc R . . H18B H 0.7770 0.1606 -0.3090 0.022 Uiso 1 1 calc R . . H18C H 0.7667 0.0693 -0.3000 0.022 Uiso 1 1 calc R . . F1 F 0.72856(3) 0.12122(4) 0.09388(5) 0.02372(12) Uani 1 1 d . . . F2 F 0.76261(7) 0.19984(5) -0.04105(6) 0.0456(3) Uani 1 1 d . . . F3 F 0.83256(5) 0.10210(5) 0.01531(10) 0.0462(3) Uani 1 1 d . . . F4 F 0.81607(3) 0.20785(4) 0.11934(5) 0.02159(11) Uani 1 1 d . . . B1 B 0.78475(6) 0.15746(5) 0.04646(7) 0.01672(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01017(3) 0.00773(3) 0.00711(3) 0.00079(2) 0.00274(2) 0.00162(2) O1 0.01377(17) 0.00849(15) 0.00719(14) -0.00004(12) 0.00257(13) 0.00137(13) O2 0.0145(2) 0.01293(19) 0.01186(17) 0.00275(15) 0.00584(15) 0.00453(16) N1 0.01232(19) 0.00795(17) 0.00904(16) 0.00060(13) 0.00234(14) 0.00171(15) N2 0.01029(17) 0.00927(17) 0.00675(15) -0.00024(13) 0.00040(13) 0.00088(14) N3 0.00953(17) 0.00985(17) 0.00868(16) -0.00008(13) 0.00066(13) 0.00116(14) N4 0.01065(18) 0.01006(17) 0.00932(17) 0.00009(14) 0.00378(14) -0.00023(15) C1 0.00963(19) 0.00858(18) 0.00822(17) -0.00020(14) 0.00074(14) 0.00049(16) C2 0.0121(2) 0.0114(2) 0.0106(2) -0.00155(17) 0.00231(17) 0.00135(18) C3 0.0139(2) 0.0108(2) 0.0153(2) -0.00211(18) 0.00267(19) 0.00238(19) C4 0.0175(3) 0.0098(2) 0.0164(3) 0.00110(19) 0.0032(2) 0.0032(2) C5 0.0165(3) 0.0096(2) 0.0125(2) 0.00227(18) 0.0032(2) 0.00238(19) C6 0.00957(19) 0.0121(2) 0.00903(18) 0.00087(16) -0.00106(15) -0.00112(17) C7 0.0112(2) 0.0190(3) 0.0215(3) 0.0033(2) -0.0021(2) -0.0037(2) C8 0.0163(3) 0.0127(2) 0.0127(2) 0.00367(19) -0.00276(19) -0.0004(2) C9 0.0191(3) 0.0206(3) 0.0089(2) -0.0024(2) -0.0016(2) 0.0025(2) C10 0.00925(19) 0.0103(2) 0.01006(19) -0.00105(16) 0.00196(15) 0.00024(16) C11 0.0125(2) 0.0121(2) 0.0134(2) -0.00228(18) 0.00404(18) 0.00067(19) C12 0.0115(2) 0.0118(2) 0.0165(3) -0.00352(19) 0.00155(19) 0.00152(19) C13 0.0127(2) 0.0113(2) 0.0147(2) -0.00125(18) -0.00137(19) 0.00272(19) C14 0.0115(2) 0.0115(2) 0.01078(19) 0.00047(17) -0.00057(17) 0.00234(17) C15 0.0108(2) 0.0137(2) 0.00847(18) 0.00019(16) 0.00187(16) -0.00274(18) C16 0.0181(3) 0.0132(3) 0.0187(3) 0.0029(2) 0.0040(2) -0.0014(2) C17 0.0169(3) 0.0274(4) 0.0093(2) -0.0015(2) 0.0005(2) -0.0059(3) C18 0.0111(2) 0.0196(3) 0.0138(2) 0.0006(2) 0.00237(19) -0.0029(2) F1 0.0174(2) 0.0325(3) 0.0212(2) 0.0054(2) 0.00126(19) -0.0018(2) F2 0.0946(8) 0.0210(3) 0.0214(3) 0.0107(2) -0.0285(4) -0.0229(4) F3 0.0420(5) 0.0200(3) 0.0767(7) -0.0107(4) 0.0398(5) -0.0005(3) F4 0.0228(3) 0.0262(3) 0.0158(2) -0.00171(19) -0.00438(18) 0.0005(2) B1 0.0254(4) 0.0130(3) 0.0117(3) 0.0015(2) 0.0041(3) 0.0009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 O1 1.8963(5) . ? Cu1 N1 1.9246(6) . ? Cu1 N3 1.9442(6) . ? Cu1 O2 1.9813(6) . ? Cu1 O1 2.3785(6) 5_655 ? O1 N2 1.4091(7) . ? O1 Cu1 2.3786(6) 5_655 ? O2 N4 1.3024(8) . ? N1 C1 1.3550(8) . ? N1 C5 1.3559(9) . ? N2 C1 1.3931(9) . ? N2 C6 1.5095(9) . ? N3 C14 1.3410(9) . ? N3 C10 1.3529(8) . ? N4 C10 1.4016(9) . ? N4 C15 1.5129(9) . ? C1 C2 1.4100(9) . ? C2 C3 1.3799(11) . ? C2 H2 0.9500 . ? C3 C4 1.4028(11) . ? C3 H3 0.9500 . ? C4 C5 1.3746(10) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.5270(10) . ? C6 C8 1.5282(11) . ? C6 C9 1.5300(10) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.3946(9) . ? C11 C12 1.3907(11) . ? C11 H11 0.9500 . ? C12 C13 1.3959(11) . ? C12 H12 0.9500 . ? C13 C14 1.3884(10) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.5291(11) . ? C15 C17 1.5333(10) . ? C15 C18 1.5359(10) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? F1 B1 1.3889(12) . ? F2 B1 1.3870(12) . ? F3 B1 1.3896(13) . ? F4 B1 1.4014(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 O1 Cu1 N1 82.57(2) . . ? O1 Cu1 N3 97.71(2) . . ? N1 Cu1 N3 162.70(3) . . ? O1 Cu1 O2 169.37(3) . . ? N1 Cu1 O2 102.16(2) . . ? N3 Cu1 O2 80.64(2) . . ? O1 Cu1 O1 82.56(2) . 5_655 ? N1 Cu1 O1 103.68(2) . 5_655 ? N3 Cu1 O1 93.49(2) . 5_655 ? O2 Cu1 O1 87.05(2) . 5_655 ? N2 O1 Cu1 113.81(4) . . ? N2 O1 Cu1 113.66(4) . 5_655 ? Cu1 O1 Cu1 97.44(2) . 5_655 ? N4 O2 Cu1 112.73(4) . . ? C1 N1 C5 120.19(6) . . ? C1 N1 Cu1 113.05(4) . . ? C5 N1 Cu1 126.53(5) . . ? C1 N2 O1 111.24(5) . . ? C1 N2 C6 120.04(5) . . ? O1 N2 C6 109.56(5) . . ? C14 N3 C10 119.39(6) . . ? C14 N3 Cu1 124.76(5) . . ? C10 N3 Cu1 114.00(5) . . ? O2 N4 C10 115.78(5) . . ? O2 N4 C15 117.53(6) . . ? C10 N4 C15 126.67(6) . . ? N1 C1 N2 116.56(5) . . ? N1 C1 C2 120.14(6) . . ? N2 C1 C2 123.02(6) . . ? C3 C2 C1 118.96(6) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 120.42(7) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 117.92(7) . . ? C5 C4 H4 121.0 . . ? C3 C4 H4 121.0 . . ? N1 C5 C4 122.35(7) . . ? N1 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? N2 C6 C7 110.09(6) . . ? N2 C6 C8 107.33(5) . . ? C7 C6 C8 109.97(6) . . ? N2 C6 C9 110.63(6) . . ? C7 C6 C9 110.02(7) . . ? C8 C6 C9 108.75(6) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N3 C10 C11 122.13(6) . . ? N3 C10 N4 112.81(6) . . ? C11 C10 N4 125.04(6) . . ? C12 C11 C10 117.74(7) . . ? C12 C11 H11 121.1 . . ? C10 C11 H11 121.1 . . ? C11 C12 C13 120.30(6) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 118.15(7) . . ? C14 C13 H13 120.9 . . ? C12 C13 H13 120.9 . . ? N3 C14 C13 122.17(7) . . ? N3 C14 H14 118.9 . . ? C13 C14 H14 118.9 . . ? N4 C15 C16 106.94(6) . . ? N4 C15 C17 108.24(6) . . ? C16 C15 C17 109.79(7) . . ? N4 C15 C18 110.26(6) . . ? C16 C15 C18 109.68(6) . . ? C17 C15 C18 111.80(6) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? F2 B1 F1 109.64(10) . . ? F2 B1 F3 110.54(10) . . ? F1 B1 F3 109.10(8) . . ? F2 B1 F4 108.44(8) . . ? F1 B1 F4 110.06(7) . . ? F3 B1 F4 109.06(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cu1 O1 N2 -15.08(4) . . . . ? N3 Cu1 O1 N2 147.46(4) . . . . ? O2 Cu1 O1 N2 -132.23(12) . . . . ? O1 Cu1 O1 N2 -120.00(5) 5_655 . . . ? N1 Cu1 O1 Cu1 104.92(2) . . . 5_655 ? N3 Cu1 O1 Cu1 -92.53(2) . . . 5_655 ? O2 Cu1 O1 Cu1 -12.23(13) . . . 5_655 ? O1 Cu1 O1 Cu1 0.0 5_655 . . 5_655 ? O1 Cu1 O2 N4 -90.22(14) . . . . ? N1 Cu1 O2 N4 154.28(5) . . . . ? N3 Cu1 O2 N4 -8.33(5) . . . . ? O1 Cu1 O2 N4 -102.36(5) 5_655 . . . ? O1 Cu1 N1 C1 9.45(5) . . . . ? N3 Cu1 N1 C1 -82.62(10) . . . . ? O2 Cu1 N1 C1 179.79(5) . . . . ? O1 Cu1 N1 C1 89.89(5) 5_655 . . . ? O1 Cu1 N1 C5 -164.98(7) . . . . ? N3 Cu1 N1 C5 102.95(10) . . . . ? O2 Cu1 N1 C5 5.36(7) . . . . ? O1 Cu1 N1 C5 -84.54(7) 5_655 . . . ? Cu1 O1 N2 C1 17.68(7) . . . . ? Cu1 O1 N2 C1 -92.68(5) 5_655 . . . ? Cu1 O1 N2 C6 -117.40(5) . . . . ? Cu1 O1 N2 C6 132.24(4) 5_655 . . . ? O1 Cu1 N3 C14 0.79(6) . . . . ? N1 Cu1 N3 C14 90.55(10) . . . . ? O2 Cu1 N3 C14 -168.59(6) . . . . ? O1 Cu1 N3 C14 -82.16(6) 5_655 . . . ? O1 Cu1 N3 C10 165.16(5) . . . . ? N1 Cu1 N3 C10 -105.08(9) . . . . ? O2 Cu1 N3 C10 -4.22(5) . . . . ? O1 Cu1 N3 C10 82.21(5) 5_655 . . . ? Cu1 O2 N4 C10 19.33(8) . . . . ? Cu1 O2 N4 C15 -159.73(5) . . . . ? C5 N1 C1 N2 172.79(6) . . . . ? Cu1 N1 C1 N2 -2.03(8) . . . . ? C5 N1 C1 C2 -1.35(10) . . . . ? Cu1 N1 C1 C2 -176.17(5) . . . . ? O1 N2 C1 N1 -10.01(8) . . . . ? C6 N2 C1 N1 119.76(7) . . . . ? O1 N2 C1 C2 163.95(6) . . . . ? C6 N2 C1 C2 -66.28(9) . . . . ? N1 C1 C2 C3 0.00(10) . . . . ? N2 C1 C2 C3 -173.75(7) . . . . ? C1 C2 C3 C4 0.85(11) . . . . ? C2 C3 C4 C5 -0.37(12) . . . . ? C1 N1 C5 C4 1.89(12) . . . . ? Cu1 N1 C5 C4 175.96(6) . . . . ? C3 C4 C5 N1 -1.01(13) . . . . ? C1 N2 C6 C7 -62.23(8) . . . . ? O1 N2 C6 C7 68.28(7) . . . . ? C1 N2 C6 C8 178.09(6) . . . . ? O1 N2 C6 C8 -51.40(7) . . . . ? C1 N2 C6 C9 59.59(8) . . . . ? O1 N2 C6 C9 -169.91(6) . . . . ? C14 N3 C10 C11 2.03(10) . . . . ? Cu1 N3 C10 C11 -163.25(6) . . . . ? C14 N3 C10 N4 -179.47(6) . . . . ? Cu1 N3 C10 N4 15.25(7) . . . . ? O2 N4 C10 N3 -23.07(9) . . . . ? C15 N4 C10 N3 155.89(6) . . . . ? O2 N4 C10 C11 155.38(7) . . . . ? C15 N4 C10 C11 -25.66(11) . . . . ? N3 C10 C11 C12 -2.78(11) . . . . ? N4 C10 C11 C12 178.91(7) . . . . ? C10 C11 C12 C13 0.47(11) . . . . ? C11 C12 C13 C14 2.42(11) . . . . ? C10 N3 C14 C13 1.10(11) . . . . ? Cu1 N3 C14 C13 164.69(6) . . . . ? C12 C13 C14 N3 -3.28(11) . . . . ? O2 N4 C15 C16 23.71(8) . . . . ? C10 N4 C15 C16 -155.23(7) . . . . ? O2 N4 C15 C17 -94.52(8) . . . . ? C10 N4 C15 C17 86.54(9) . . . . ? O2 N4 C15 C18 142.90(7) . . . . ? C10 N4 C15 C18 -36.04(9) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 43.34 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.473 _refine_diff_density_min -1.300 _refine_diff_density_rms 0.109