#Supplementary Material for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Abrahams, Brendan F.' 'Che, Chi-ming' 'Lee, Gene-Hsiung' 'Peng, Shie-ming' 'Xiong, Ren-Gen' 'You, Xiao-Zeng ' 'Yuan, Rong-Xin' _publ_contact_author_name 'Prof. Ren-Gen Xiong' _publ_contact_author_address ; Prof. Xiao-Zeng You Coordination Chemistry Institue Nanjing University, Nanjing 210093, P. R. China ; _publ_contact_author_email 'xyz@netra.nju.edu.cn' _publ_contact_author_fax '86-25-3317761' _publ_contact_author_phone '86-25-3594724' _publ_requested_journal 'J. Chem.Soc. Dalton Trans.' _publ_section_title ; An Cu(I) coordination polymer employing a nonsteroidal aromatase inhibitor letrozole as building block ; _publ_section_references ; Allen, F.H., Kennard, O., Watson, D.G., Brammer, L., Orpen, A.G. & Taylor, R. (1987). Chem. Soc. Perkin Trans. II, S1-S19. Nardelli, M. (1995). J. Appl. Cryst. 28, 659. Orpen, A.G., Brammer, L., Allen, F.H., Kennard, O., Watson, D.G. & Taylor, R. (1989). J. Chem. Soc. Dalton Trans., S1-S83. Siemens (1996). SMART and SAINT. Area Detector Control and Integration Software. Siemens Analytical X-Ray Systems, Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1996). SADABS. Program for Empirical Absorption Correction of Area Detector Data, University of G\"ottingen, Germany. Sheldrick, G.M. (1997). SHELXTL V5.1 Software Reference Manual, Bruker AXS, Inc., Madison, Wisconsin, USA. Spek, A.L. (1990). Acta Cryst. A46, C-34. ; _publ_section_exptl_refinement ; The data collection covered over a hemisphere of reciprocal space by a combination of three sets of exposures; each set had a different \f angle (0, 88 and 180\%) for the crystal and each exposure of 10s covered 0.3\% in \w. The crystal-to-detector distance was 4 cm and the detector swing angle was -35\%. Coverage of the unique set is over 99% complete. Crystal decay was monitored by repeating fifty initial frames at the end of data collection and analysing the duplicate reflections, and was found to be negligible. ; #=========================================================================== #========================================================================== #== data_1 _database_code_CSD 164957 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H12 B Cl3 Cu F4 N5' _chemical_formula_weight 555.03 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' 'F' 'F' 0.0171 0.0103 '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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 8.9646(3) _cell_length_b 22.8924(9) _cell_length_c 23.9497(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4915.0(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 6867 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 1.260 _exptl_absorpt_correction_type 'empirical used sadabs' _exptl_absorpt_correction_T_min 0.7792 _exptl_absorpt_correction_T_max 0.8621 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 44209 _diffrn_reflns_av_R_equivalents 0.0805 _diffrn_reflns_av_sigmaI/netI 0.0683 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5644 _reflns_number_gt 3092 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1691P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0055(9) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5644 _refine_ls_number_parameters 307 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1380 _refine_ls_R_factor_gt 0.0822 _refine_ls_wR_factor_ref 0.2814 _refine_ls_wR_factor_gt 0.2535 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.007 _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 0.00278(8) 0.22061(3) 0.42177(3) 0.0229(3) Uani 1 1 d . . . N1 N -0.1553(6) 0.27283(19) 0.45839(18) 0.0242(11) Uani 1 1 d . . . N2 N -0.3467(5) 0.2928(2) 0.51556(19) 0.0244(11) Uani 1 1 d . . . N3 N -0.2193(5) 0.32541(18) 0.44464(17) 0.0201(10) Uani 1 1 d . . . N4 N -0.4027(6) 0.2492(2) 0.1448(2) 0.0300(12) Uani 1 1 d . . . N5 N -0.4005(7) 0.6436(2) 0.4164(2) 0.0334(13) Uani 1 1 d . . . C1 C -0.2358(7) 0.2556(3) 0.5010(2) 0.0277(13) Uani 1 1 d . . . H1A H -0.2178 0.2199 0.5201 0.033 Uiso 1 1 calc R . . C2 C -0.3337(6) 0.3357(3) 0.4790(2) 0.0242(12) Uani 1 1 d . . . H2A H -0.3965 0.3691 0.4774 0.029 Uiso 1 1 calc R . . C3 C -0.1640(7) 0.3594(2) 0.3964(2) 0.0215(12) Uani 1 1 d . . . H3A H -0.0525 0.3592 0.3979 0.026 Uiso 1 1 calc R . . C4 C -0.2118(6) 0.3305(2) 0.3411(2) 0.0208(12) Uani 1 1 d . . . C5 C -0.3145(7) 0.2861(3) 0.3386(2) 0.0311(14) Uani 1 1 d . . . H5A H -0.3547 0.2701 0.3720 0.037 Uiso 1 1 calc R . . C6 C -0.3590(8) 0.2647(3) 0.2869(3) 0.0352(15) Uani 1 1 d . . . H6A H -0.4305 0.2341 0.2849 0.042 Uiso 1 1 calc R . . C7 C -0.2996(7) 0.2877(3) 0.2386(2) 0.0289(14) Uani 1 1 d . . . C8 C -0.1955(8) 0.3322(3) 0.2408(2) 0.0317(14) Uani 1 1 d . . . H8A H -0.1553 0.3478 0.2073 0.038 Uiso 1 1 calc R . . C9 C -0.1498(7) 0.3540(3) 0.2918(2) 0.0310(14) Uani 1 1 d . . . H9A H -0.0778 0.3844 0.2937 0.037 Uiso 1 1 calc R . . C10 C -0.2155(6) 0.4224(2) 0.4007(2) 0.0205(12) Uani 1 1 d . . . C11 C -0.3464(7) 0.4403(3) 0.3763(3) 0.0352(15) Uani 1 1 d . . . H11A H -0.4049 0.4134 0.3556 0.042 Uiso 1 1 calc R . . C12 C -0.3935(8) 0.4981(3) 0.3819(3) 0.0376(16) Uani 1 1 d . . . H12A H -0.4839 0.5107 0.3651 0.045 Uiso 1 1 calc R . . C13 C -0.3081(7) 0.5365(2) 0.4120(2) 0.0271(13) Uani 1 1 d . . . C14 C -0.1794(8) 0.5198(3) 0.4368(3) 0.0372(16) Uani 1 1 d . . . H14A H -0.1224 0.5470 0.4578 0.045 Uiso 1 1 calc R . . C15 C -0.1308(8) 0.4618(3) 0.4314(3) 0.0365(16) Uani 1 1 d . . . H15A H -0.0406 0.4496 0.4486 0.044 Uiso 1 1 calc R . . C16 C -0.3542(7) 0.2664(3) 0.1858(3) 0.0314(14) Uani 1 1 d . . . C17 C -0.3576(8) 0.5971(3) 0.4156(3) 0.0334(15) Uani 1 1 d . . . B1 B 0.2761(12) 0.3897(4) 0.4202(3) 0.047(2) Uani 1 1 d . . . F1 F 0.1621(4) 0.37070(18) 0.45615(17) 0.0472(11) Uani 1 1 d . . . F2 F 0.3712(5) 0.3459(2) 0.40737(19) 0.0544(12) Uani 1 1 d . . . F3 F 0.3472(9) 0.4351(3) 0.4453(3) 0.141(4) Uani 1 1 d . . . F4 F 0.2025(8) 0.4066(3) 0.3709(2) 0.115(3) Uani 1 1 d . . . Cl1 Cl -0.7871(9) 0.5609(3) 0.4011(3) 0.234(3) Uiso 1 1 d D . . C18 C -0.8287(19) 0.6304(8) 0.3760(6) 0.156(11) Uani 0.70 1 d PD A 1 H18A H -0.7417 0.6563 0.3846 0.188 Uiso 0.70 1 calc PR A 1 Cl2 Cl -0.9828(7) 0.6587(3) 0.4105(4) 0.171(4) Uani 0.70 1 d PD A 1 Cl3 Cl -0.8501(13) 0.6287(4) 0.3034(4) 0.247(5) Uani 0.70 1 d PD A 1 C18' C -0.842(4) 0.5303(9) 0.3382(10) 0.15(2) Uiso 0.30 1 d PD A 2 H18B H -0.8477 0.4877 0.3473 0.180 Uiso 0.30 1 calc PR A 2 Cl2' Cl -0.734(4) 0.5312(15) 0.2775(12) 0.38(3) Uani 0.30 1 d PD A 2 Cl3' Cl -0.996(2) 0.5402(13) 0.2920(13) 0.262(13) Uani 0.30 1 d PD A 2 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 0.0303(5) 0.0204(4) 0.0181(4) 0.0018(2) 0.0003(3) -0.0009(3) N1 0.034(3) 0.019(2) 0.019(2) 0.0024(18) 0.002(2) 0.003(2) N2 0.030(3) 0.022(2) 0.021(2) 0.0027(18) 0.001(2) 0.001(2) N3 0.030(3) 0.017(2) 0.014(2) 0.0004(17) -0.0036(19) 0.003(2) N4 0.037(3) 0.029(3) 0.025(2) -0.004(2) -0.005(2) 0.004(2) N5 0.043(3) 0.019(3) 0.038(3) -0.004(2) -0.003(2) 0.006(2) C1 0.035(4) 0.022(3) 0.025(3) 0.004(2) 0.004(3) 0.002(3) C2 0.025(3) 0.028(3) 0.020(3) 0.000(2) -0.002(2) 0.003(3) C3 0.027(3) 0.019(3) 0.018(3) 0.001(2) -0.001(2) 0.003(2) C4 0.024(3) 0.022(3) 0.016(2) -0.001(2) -0.002(2) 0.003(2) C5 0.045(4) 0.031(3) 0.017(3) 0.001(2) -0.001(3) -0.013(3) C6 0.044(4) 0.031(3) 0.031(3) -0.006(3) -0.004(3) -0.013(3) C7 0.036(3) 0.032(3) 0.019(3) -0.006(2) -0.005(2) 0.009(3) C8 0.041(4) 0.036(3) 0.018(3) 0.001(2) 0.000(2) 0.006(3) C9 0.043(4) 0.031(3) 0.019(3) 0.003(2) -0.003(3) -0.004(3) C10 0.026(3) 0.018(3) 0.018(2) 0.002(2) 0.003(2) 0.003(2) C11 0.033(4) 0.025(3) 0.048(4) -0.006(3) -0.009(3) 0.002(3) C12 0.029(4) 0.027(3) 0.057(4) 0.000(3) -0.003(3) 0.005(3) C13 0.036(4) 0.015(3) 0.030(3) 0.000(2) 0.003(3) 0.001(3) C14 0.049(4) 0.020(3) 0.042(4) -0.010(3) -0.013(3) 0.002(3) C15 0.047(4) 0.028(3) 0.035(3) -0.003(3) -0.016(3) 0.006(3) C16 0.037(4) 0.027(3) 0.030(3) -0.004(3) 0.000(3) 0.006(3) C17 0.039(4) 0.026(3) 0.035(3) -0.003(3) 0.003(3) -0.003(3) B1 0.066(6) 0.039(5) 0.036(4) 0.001(3) 0.000(4) -0.003(5) F1 0.040(2) 0.046(2) 0.055(3) 0.0102(19) -0.0001(19) -0.002(2) F2 0.040(3) 0.053(3) 0.070(3) 0.002(2) 0.004(2) 0.007(2) F3 0.149(6) 0.114(5) 0.161(6) -0.092(5) 0.101(5) -0.097(5) F4 0.164(6) 0.136(5) 0.045(3) 0.042(3) 0.028(3) 0.096(5) C18 0.111(16) 0.20(2) 0.16(2) 0.109(19) -0.070(16) -0.042(17) Cl2 0.121(5) 0.086(4) 0.307(12) 0.003(5) -0.010(5) 0.002(3) Cl3 0.339(14) 0.169(7) 0.235(10) -0.054(7) -0.090(10) -0.017(8) Cl2' 0.48(6) 0.38(4) 0.30(3) 0.05(3) -0.27(4) -0.07(4) Cl3' 0.18(2) 0.29(3) 0.31(3) 0.12(3) 0.03(2) -0.044(18) _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 N4 1.921(5) 6_656 ? Cu1 N5 1.992(5) 8 ? Cu1 N2 2.041(5) 4_556 ? Cu1 N1 2.051(5) . ? N1 C1 1.311(7) . ? N1 N3 1.374(6) . ? N2 C2 1.322(7) . ? N2 C1 1.355(7) . ? N2 Cu1 2.041(5) 4_456 ? N3 C2 1.336(7) . ? N3 C3 1.478(7) . ? N4 C16 1.144(7) . ? N4 Cu1 1.921(5) 6_556 ? N5 C17 1.131(8) . ? N5 Cu1 1.992(5) 8_565 ? C3 C10 1.518(7) . ? C3 C4 1.541(7) . ? C4 C5 1.373(8) . ? C4 C9 1.411(8) . ? C5 C6 1.391(8) . ? C6 C7 1.379(9) . ? C7 C8 1.382(9) . ? C7 C16 1.441(8) . ? C8 C9 1.382(8) . ? C10 C11 1.373(8) . ? C10 C15 1.390(8) . ? C11 C12 1.394(9) . ? C12 C13 1.371(9) . ? C13 C14 1.354(9) . ? C13 C17 1.458(9) . ? C14 C15 1.401(8) . ? B1 F2 1.351(10) . ? B1 F3 1.359(10) . ? B1 F4 1.406(10) . ? B1 F1 1.405(10) . ? Cl1 C18 1.743(14) . ? Cl1 C18' 1.731(18) . ? C18 Cl3 1.750(15) . ? C18 Cl2 1.736(15) . ? C18' Cl2' 1.75(2) . ? C18' Cl3' 1.781(18) . ? Cl2' Cl3' 2.38(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cu1 N5 116.9(2) 6_656 8 ? N4 Cu1 N2 111.7(2) 6_656 4_556 ? N5 Cu1 N2 102.6(2) 8 4_556 ? N4 Cu1 N1 117.46(19) 6_656 . ? N5 Cu1 N1 103.0(2) 8 . ? N2 Cu1 N1 103.27(18) 4_556 . ? C1 N1 N3 102.8(5) . . ? C1 N1 Cu1 122.5(4) . . ? N3 N1 Cu1 134.2(3) . . ? C2 N2 C1 103.5(5) . . ? C2 N2 Cu1 131.1(4) . 4_456 ? C1 N2 Cu1 125.4(4) . 4_456 ? C2 N3 N1 109.1(4) . . ? C2 N3 C3 130.3(5) . . ? N1 N3 C3 120.5(4) . . ? C16 N4 Cu1 176.1(5) . 6_556 ? C17 N5 Cu1 171.9(6) . 8_565 ? N1 C1 N2 114.5(5) . . ? N2 C2 N3 110.1(5) . . ? N3 C3 C10 110.2(4) . . ? N3 C3 C4 110.6(4) . . ? C10 C3 C4 112.4(4) . . ? C5 C4 C9 120.7(5) . . ? C5 C4 C3 122.7(5) . . ? C9 C4 C3 116.5(5) . . ? C4 C5 C6 119.5(5) . . ? C7 C6 C5 120.1(6) . . ? C6 C7 C8 120.7(5) . . ? C6 C7 C16 118.3(6) . . ? C8 C7 C16 120.9(5) . . ? C9 C8 C7 120.1(6) . . ? C8 C9 C4 119.0(6) . . ? C11 C10 C15 119.8(5) . . ? C11 C10 C3 121.0(5) . . ? C15 C10 C3 119.1(5) . . ? C10 C11 C12 120.1(6) . . ? C13 C12 C11 119.3(6) . . ? C14 C13 C12 121.6(6) . . ? C14 C13 C17 120.2(6) . . ? C12 C13 C17 118.2(6) . . ? C13 C14 C15 119.5(6) . . ? C10 C15 C14 119.6(6) . . ? N4 C16 C7 177.5(7) . . ? N5 C17 C13 176.7(7) . . ? F2 B1 F3 111.8(9) . . ? F2 B1 F4 108.0(6) . . ? F3 B1 F4 112.4(8) . . ? F2 B1 F1 111.6(7) . . ? F3 B1 F1 107.8(6) . . ? F4 B1 F1 105.0(8) . . ? C18 Cl1 C18' 90.5(11) . . ? Cl1 C18 Cl3 110.2(11) . . ? Cl1 C18 Cl2 110.3(9) . . ? Cl3 C18 Cl2 113.2(10) . . ? Cl1 C18' Cl2' 124(2) . . ? Cl1 C18' Cl3' 135(3) . . ? Cl2' C18' Cl3' 84.7(16) . . ? C18' Cl2' Cl3' 48.3(10) . . ? C18' Cl3' Cl2' 47.1(9) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.454 _refine_diff_density_min -1.475 _refine_diff_density_rms 0.195