data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year 2009 _journal_volume 11 _journal_page_first 746 loop_ _publ_author_name S.Banerjee N.N.Adrash P.Dastidar _publ_contact_author_name 'Parthasarathi Dastidar' _publ_contact_author_email PARTHOD123@REDIFFMAIL.COM # Attachment 'MOF 1 ANN129A1_FINAL_R1.cif' data_test _database_code_depnum_ccdc_archive 'CCDC 699625' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_absolute_configuration syn _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H40 Cl2 Cu N8 O6' _chemical_formula_weight 863.24 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' 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 TRIGONAL _symmetry_space_group_name_H-M P3(2)21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'y, x, -z' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' _cell_length_a 12.9207(3) _cell_length_b 12.9207(3) _cell_length_c 19.9320(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2881.73(17) _cell_formula_units_Z 3 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCK _exptl_crystal_colour BLUE _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1341 _exptl_absorpt_coefficient_mu 0.768 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7591 _exptl_absorpt_correction_T_max 0.9135 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _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 CCD AREA DETECTOR' _diffrn_measurement_method 'PHI-OMEGA SCAN' _diffrn_detector_area_resol_mean 3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34199 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 32.02 _reflns_number_total 6026 _reflns_number_gt 5364 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER AXS SMART 3' _computing_cell_refinement 'BRUKER AXS SMART 3' _computing_data_reduction 'BRUKER AXS SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER SHELXLTL' _computing_publication_material 'MERCURY 1.4' _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^)+(0.0511P)^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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.007(8) _refine_ls_number_reflns 6026 _refine_ls_number_parameters 266 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0817 _refine_ls_wR_factor_gt 0.0787 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 0.62121(2) 0.0000 1.1667 0.01507(7) Uani 1 2 d S . . Cl1 Cl 0.74236(4) 0.24402(4) 1.139727(19) 0.02142(9) Uani 1 1 d . . . N1 N 0.49621(12) -0.02299(12) 1.09642(6) 0.0154(3) Uani 1 1 d . . . C2 C 0.52791(14) 0.03898(14) 1.03853(7) 0.0164(3) Uani 1 1 d . . . H2 H 0.6069 0.0989 1.0328 0.020 Uiso 1 1 calc R . . C3 C 0.44710(15) 0.01675(14) 0.98713(7) 0.0167(3) Uani 1 1 d . . . C4 C 0.32806(16) -0.07048(15) 0.99715(8) 0.0207(3) Uani 1 1 d . . . H4 H 0.2718 -0.0873 0.9636 0.025 Uiso 1 1 calc R . . C5 C 0.29451(15) -0.13157(16) 1.05710(8) 0.0213(3) Uani 1 1 d . . . H5 H 0.2150 -0.1881 1.0652 0.026 Uiso 1 1 calc R . . C6 C 0.38126(15) -0.10741(15) 1.10515(8) 0.0185(3) Uani 1 1 d . . . H6 H 0.3591 -0.1512 1.1448 0.022 Uiso 1 1 calc R . . C7 C 0.49279(14) 0.08801(14) 0.92383(8) 0.0179(3) Uani 1 1 d . . . O8 O 0.57806(12) 0.19116(11) 0.92468(6) 0.0249(3) Uani 1 1 d . . . N9 N 0.43408(14) 0.03095(13) 0.86797(7) 0.0211(3) Uani 1 1 d . . . H9 H 0.3767 -0.0418 0.8711 0.025 Uiso 1 1 calc R . . C10 C 0.46392(16) 0.08769(16) 0.80237(8) 0.0213(3) Uani 1 1 d . . . H10 H 0.5280 0.1709 0.8070 0.026 Uiso 1 1 calc R . . C11 C 0.50374(19) 0.02229(17) 0.75396(8) 0.0274(4) Uani 1 1 d . . . H11A H 0.4430 -0.0617 0.7541 0.033 Uiso 1 1 calc R . . H11B H 0.5056 0.0524 0.7091 0.033 Uiso 1 1 calc R . . C12 C 0.62204(18) 0.03096(18) 0.76680(8) 0.0280(4) Uani 1 1 d . . . C13 C 0.6323(2) -0.0710(2) 0.76369(12) 0.0438(6) Uani 1 1 d . . . H13 H 0.5638 -0.1452 0.7585 0.053 Uiso 1 1 calc R . . C14 C 0.7414(3) -0.0646(2) 0.76808(13) 0.0511(7) Uani 1 1 d . . . H14 H 0.7458 -0.1341 0.7651 0.061 Uiso 1 1 calc R . . C15 C 0.8446(2) 0.0439(3) 0.77694(11) 0.0449(6) Uani 1 1 d . . . H15 H 0.9181 0.0479 0.7814 0.054 Uiso 1 1 calc R . . C16 C 0.8364(2) 0.1465(2) 0.77904(12) 0.0445(6) Uani 1 1 d . . . H16 H 0.9051 0.2205 0.7841 0.053 Uiso 1 1 calc R . . C17 C 0.7262(2) 0.1396(2) 0.77364(11) 0.0382(5) Uani 1 1 d . . . H17 H 0.7223 0.2095 0.7746 0.046 Uiso 1 1 calc R . . C18 C 0.35279(17) 0.08417(16) 0.77218(8) 0.0236(4) Uani 1 1 d . . . N20 N 0.38172(14) 0.16388(14) 0.72075(7) 0.0246(3) Uani 1 1 d . . . H20 H 0.4566 0.2122 0.7141 0.030 Uiso 1 1 calc R . . C21 C 0.30221(15) 0.17516(15) 0.67773(8) 0.0203(3) Uani 1 1 d . . . C22 C 0.35001(15) 0.23335(14) 0.61703(7) 0.0175(3) Uani 1 1 d . . . H22 H 0.4291 0.2568 0.6071 0.021 Uiso 1 1 calc R . . N23 N 0.28676(12) 0.25680(12) 0.57248(6) 0.0156(2) Uani 1 1 d . . . C24 C 0.17018(15) 0.21590(15) 0.58439(8) 0.0186(3) Uani 1 1 d . . . H24 H 0.1247 0.2280 0.5525 0.022 Uiso 1 1 calc R . . C25 C 0.11646(16) 0.15582(16) 0.64348(9) 0.0226(4) Uani 1 1 d . . . H25 H 0.0357 0.1281 0.6508 0.027 Uiso 1 1 calc R . . C26 C 0.18312(16) 0.13703(16) 0.69166(8) 0.0235(3) Uani 1 1 d . . . H26 H 0.1489 0.0999 0.7322 0.028 Uiso 1 1 calc R . . O27 O 0.37489(12) 0.68746(14) 0.97706(7) 0.0301(3) Uani 1 1 d . . . O19 O 0.25163(12) 0.01458(12) 0.79023(6) 0.0292(3) Uani 1 1 d . . . H27A H 0.329(3) 0.651(2) 1.0155(13) 0.044(7) Uiso 1 1 d . . . H27B H 0.332(3) 0.706(3) 0.9427(15) 0.063(9) Uiso 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 0.01671(10) 0.02219(14) 0.00816(11) -0.00214(10) -0.00107(5) 0.01109(7) Cl1 0.01981(19) 0.02154(19) 0.01888(17) 0.00140(14) -0.00116(15) 0.00730(16) N1 0.0171(6) 0.0185(6) 0.0116(6) -0.0015(5) -0.0002(5) 0.0096(5) C2 0.0179(7) 0.0171(7) 0.0127(6) -0.0003(5) -0.0009(5) 0.0075(6) C3 0.0189(8) 0.0176(7) 0.0138(7) -0.0001(5) -0.0028(6) 0.0094(6) C4 0.0208(8) 0.0232(8) 0.0167(7) -0.0009(6) -0.0054(6) 0.0100(7) C5 0.0166(8) 0.0222(8) 0.0198(7) 0.0011(6) -0.0005(6) 0.0057(7) C6 0.0206(8) 0.0201(8) 0.0145(7) 0.0009(6) 0.0014(6) 0.0099(7) C7 0.0197(8) 0.0194(8) 0.0142(7) 0.0003(6) -0.0036(6) 0.0094(7) O8 0.0253(7) 0.0218(6) 0.0182(5) 0.0009(5) -0.0048(5) 0.0047(5) N9 0.0257(8) 0.0183(7) 0.0137(6) 0.0037(5) -0.0047(5) 0.0067(6) C10 0.0252(8) 0.0199(8) 0.0131(7) 0.0034(6) -0.0047(6) 0.0071(7) C11 0.0401(11) 0.0245(9) 0.0138(7) -0.0030(6) -0.0060(7) 0.0132(8) C12 0.0392(11) 0.0296(10) 0.0155(7) -0.0005(6) 0.0015(7) 0.0174(9) C13 0.0541(14) 0.0292(11) 0.0493(13) 0.0035(9) 0.0110(11) 0.0218(11) C14 0.0659(18) 0.0463(14) 0.0587(15) 0.0167(12) 0.0219(12) 0.0412(14) C15 0.0502(14) 0.0666(17) 0.0337(10) 0.0042(11) 0.0096(10) 0.0411(14) C16 0.0370(12) 0.0457(13) 0.0468(13) -0.0138(11) -0.0035(10) 0.0177(11) C17 0.0401(12) 0.0331(11) 0.0428(11) -0.0090(9) -0.0091(9) 0.0193(10) C18 0.0273(9) 0.0220(9) 0.0154(7) 0.0027(6) -0.0057(6) 0.0078(8) N20 0.0204(7) 0.0281(8) 0.0185(6) 0.0098(6) -0.0027(6) 0.0069(6) C21 0.0215(8) 0.0215(8) 0.0152(7) 0.0023(6) -0.0031(6) 0.0086(7) C22 0.0181(8) 0.0203(8) 0.0144(6) 0.0015(6) -0.0010(6) 0.0100(7) N23 0.0182(6) 0.0178(6) 0.0115(5) 0.0007(5) -0.0008(5) 0.0095(5) C24 0.0182(8) 0.0213(8) 0.0170(7) 0.0018(6) -0.0005(6) 0.0104(7) C25 0.0192(8) 0.0249(9) 0.0224(8) 0.0038(6) 0.0016(6) 0.0100(7) C26 0.0237(9) 0.0271(9) 0.0163(7) 0.0065(6) 0.0030(6) 0.0102(8) O27 0.0240(7) 0.0417(8) 0.0267(6) 0.0049(6) 0.0035(5) 0.0181(6) O19 0.0241(7) 0.0258(7) 0.0237(6) 0.0096(5) -0.0030(5) 0.0019(5) _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 N23 2.0276(13) 2_655 ? Cu1 N23 2.0276(13) 6_656 ? Cu1 N1 2.0438(13) 5_557 ? Cu1 N1 2.0438(13) . ? N1 C6 1.344(2) . ? N1 C2 1.3463(19) . ? C2 C3 1.386(2) . ? C2 H2 0.9300 . ? C3 C4 1.394(3) . ? C3 C7 1.498(2) . ? C4 C5 1.377(2) . ? C4 H4 0.9300 . ? C5 C6 1.386(2) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 O8 1.234(2) . ? C7 N9 1.341(2) . ? N9 C10 1.454(2) . ? N9 H9 0.8600 . ? C10 C11 1.531(3) . ? C10 C18 1.536(2) . ? C10 H10 0.9800 . ? C11 C12 1.498(3) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C17 1.383(3) . ? C12 C13 1.390(3) . ? C13 C14 1.372(4) . ? C13 H13 0.9300 . ? C14 C15 1.380(4) . ? C14 H14 0.9300 . ? C15 C16 1.382(4) . ? C15 H15 0.9300 . ? C16 C17 1.385(3) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 O19 1.213(2) . ? C18 N20 1.366(2) . ? N20 C21 1.401(2) . ? N20 H20 0.8600 . ? C21 C26 1.389(2) . ? C21 C22 1.395(2) . ? C22 N23 1.340(2) . ? C22 H22 0.9300 . ? N23 C24 1.345(2) . ? N23 Cu1 2.0276(13) 3_664 ? C24 C25 1.390(2) . ? C24 H24 0.9300 . ? C25 C26 1.390(2) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? O27 H27A 0.94(3) . ? O27 H27B 0.98(3) . ? 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 N23 Cu1 N23 94.02(8) 2_655 6_656 ? N23 Cu1 N1 88.88(5) 2_655 5_557 ? N23 Cu1 N1 176.57(6) 6_656 5_557 ? N23 Cu1 N1 176.57(6) 2_655 . ? N23 Cu1 N1 88.88(5) 6_656 . ? N1 Cu1 N1 88.29(7) 5_557 . ? C6 N1 C2 118.54(14) . . ? C6 N1 Cu1 120.11(11) . . ? C2 N1 Cu1 121.16(11) . . ? N1 C2 C3 122.44(15) . . ? N1 C2 H2 118.8 . . ? C3 C2 H2 118.8 . . ? C2 C3 C4 118.29(14) . . ? C2 C3 C7 118.06(14) . . ? C4 C3 C7 123.64(14) . . ? C5 C4 C3 119.45(15) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 118.89(16) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? N1 C6 C5 122.30(15) . . ? N1 C6 H6 118.8 . . ? C5 C6 H6 118.8 . . ? O8 C7 N9 124.00(15) . . ? O8 C7 C3 121.13(14) . . ? N9 C7 C3 114.86(14) . . ? C7 N9 C10 122.34(14) . . ? C7 N9 H9 118.8 . . ? C10 N9 H9 118.8 . . ? N9 C10 C11 111.48(14) . . ? N9 C10 C18 109.21(14) . . ? C11 C10 C18 107.69(14) . . ? N9 C10 H10 109.5 . . ? C11 C10 H10 109.5 . . ? C18 C10 H10 109.5 . . ? C12 C11 C10 117.58(15) . . ? C12 C11 H11A 107.9 . . ? C10 C11 H11A 107.9 . . ? C12 C11 H11B 107.9 . . ? C10 C11 H11B 107.9 . . ? H11A C11 H11B 107.2 . . ? C17 C12 C13 117.4(2) . . ? C17 C12 C11 122.13(19) . . ? C13 C12 C11 119.93(19) . . ? C14 C13 C12 121.4(2) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C13 C14 C15 120.7(2) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C14 C15 C16 118.6(2) . . ? C14 C15 H15 120.7 . . ? C16 C15 H15 120.7 . . ? C15 C16 C17 120.4(3) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C12 C17 C16 121.3(2) . . ? C12 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? O19 C18 N20 124.65(17) . . ? O19 C18 C10 123.41(15) . . ? N20 C18 C10 111.85(15) . . ? C18 N20 C21 126.83(16) . . ? C18 N20 H20 116.6 . . ? C21 N20 H20 116.6 . . ? C26 C21 C22 118.56(15) . . ? C26 C21 N20 125.51(15) . . ? C22 C21 N20 115.90(15) . . ? N23 C22 C21 122.73(15) . . ? N23 C22 H22 118.6 . . ? C21 C22 H22 118.6 . . ? C22 N23 C24 118.95(13) . . ? C22 N23 Cu1 117.45(11) . 3_664 ? C24 N23 Cu1 122.51(11) . 3_664 ? N23 C24 C25 121.16(15) . . ? N23 C24 H24 119.4 . . ? C25 C24 H24 119.4 . . ? C26 C25 C24 120.19(16) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C21 C26 C25 118.24(15) . . ? C21 C26 H26 120.9 . . ? C25 C26 H26 120.9 . . ? H27A O27 H27B 114(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N9 H9 Cl1 0.86 2.45 3.2865(15) 165.8 4_547 N20 H20 O27 0.86 1.96 2.815(2) 173.6 6_656 O27 H27A O8 0.94(3) 1.95(3) 2.8486(19) 159(2) 4_557 O27 H27B Cl1 0.98(3) 2.18(3) 3.1592(15) 175(2) 4_557 _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 32.02 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.526 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.070 data_sb0387c _database_code_depnum_ccdc_archive 'CCDC 699626' #TrackingRef 'sb0387c_FINAL.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H30 Cl2 Cu N8 O5' _chemical_formula_weight 693.04 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' 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z' '-x, -y, z' 'y, -x, z' _cell_length_a 13.266(4) _cell_length_b 13.266(4) _cell_length_c 5.3885(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 948.3(5) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 357 _exptl_absorpt_coefficient_mu 0.759 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8630 _exptl_absorpt_correction_T_max 0.9559 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _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 Apex II' _diffrn_measurement_method 'Omega scan' _diffrn_detector_area_resol_mean 3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7648 _diffrn_reflns_av_R_equivalents 0.0541 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 23.26 _reflns_number_total 1333 _reflns_number_gt 1268 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Mercury 2.3' _computing_publication_material Shelxl-97 _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^)+(0.2800P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(5) _refine_ls_number_reflns 1333 _refine_ls_number_parameters 99 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1103 _refine_ls_R_factor_gt 0.1075 _refine_ls_wR_factor_ref 0.3056 _refine_ls_wR_factor_gt 0.2980 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.004 _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 1.0000 1.0000 0.3360 0.0198(8) Uani 1 4 d S . . Cl1 Cl 1.0000 1.0000 -0.1329(12) 0.0264(14) Uani 1 4 d S . . N1 N 0.9253(5) 0.8658(5) 0.3617(18) 0.0248(19) Uani 1 1 d . . . C2 C 0.8488(8) 0.8420(8) 0.212(2) 0.035(2) Uani 1 1 d . . . H2 H 0.8310 0.8872 0.0873 0.042 Uiso 1 1 calc R . . C3 C 0.7945(9) 0.7529(11) 0.234(3) 0.053(3) Uani 1 1 d . . . H3 H 0.7392 0.7407 0.1324 0.063 Uiso 1 1 calc R . . C4 C 0.8238(12) 0.6828(11) 0.409(3) 0.070(5) Uani 1 1 d . . . H4 H 0.7905 0.6214 0.4229 0.084 Uiso 1 1 calc R . . C5 C 0.9025(12) 0.7057(9) 0.559(2) 0.052(4) Uani 1 1 d . . . C6 C 0.9531(8) 0.8002(7) 0.526(2) 0.028(3) Uani 1 1 d . . . H6 H 1.0081 0.8150 0.6270 0.034 Uiso 1 1 calc R . . N7 N 0.9635(16) 0.6361(15) 0.768(4) 0.040(5) Uiso 0.25 1 d P . . C7 C 0.9635(16) 0.6361(15) 0.768(4) 0.040(5) Uiso 0.25 1 d PD . . O8 O 1.0424(17) 0.6684(17) 0.875(5) 0.074(6) Uiso 0.50 1 d PD . . N9 N 0.9258(10) 0.5490(10) 0.818(5) 0.033(3) Uiso 0.50 1 d P . . C10 C 1.0113(13) 0.6187(11) 0.798(4) 0.024(4) Uiso 0.50 1 d PD . . O11 O 1.0821(11) 0.6736(10) 0.780(3) 0.041(4) Uiso 0.50 1 d PD . . C12 C 1.0000 0.5000 1.012(8) 0.077(13) Uiso 0.50 2 d SPD . . C13 C 1.0850(18) 0.548(2) 1.188(5) 0.053(6) Uiso 0.50 1 d PD . . O14 O 0.758(3) 0.468(3) 0.773(8) 0.071(11) Uiso 0.25 1 d P . . Cl2A Cl 0.641(3) 0.466(3) 0.372(8) 0.069(9) Uiso 0.10 1 d P . . Cl2B Cl 0.643(2) 0.460(2) 0.191(6) 0.074(7) Uiso 0.15 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0197(9) 0.0197(9) 0.0200(13) 0.000 0.000 0.000 Cl1 0.0273(14) 0.0273(14) 0.024(4) 0.000 0.000 0.000 N1 0.023(4) 0.020(3) 0.032(6) 0.005(4) -0.002(4) -0.007(3) C2 0.035(5) 0.033(5) 0.036(5) -0.002(4) -0.001(5) -0.003(4) C3 0.038(6) 0.064(8) 0.056(8) -0.008(6) 0.002(5) -0.014(6) C4 0.074(9) 0.046(8) 0.089(13) -0.009(7) 0.031(8) -0.019(7) C5 0.085(10) 0.023(6) 0.047(10) 0.012(4) 0.027(6) -0.001(6) C6 0.032(5) 0.013(5) 0.040(6) -0.009(4) 0.009(4) -0.007(4) _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 N1 2.043(7) 3_775 ? Cu1 N1 2.043(7) 4_575 ? Cu1 N1 2.043(7) . ? Cu1 N1 2.043(7) 2_755 ? Cu1 Cl1 2.527(6) . ? N1 C6 1.296(14) . ? N1 C2 1.334(14) . ? C2 C3 1.390(18) . ? C3 C4 1.38(2) . ? C4 C5 1.36(2) . ? C5 C6 1.432(16) . ? C5 N7 1.66(3) . ? N7 C10 0.694(19) . ? N7 O8 1.272(18) . ? N7 N9 1.29(3) . ? N7 O11 1.65(2) . ? O8 O11 0.74(2) . ? O8 C10 0.88(2) . ? N9 C10 1.47(2) . ? N9 C12 1.58(3) . ? C10 O11 1.193(17) . ? C10 C12 1.96(3) . ? C12 N9 1.58(3) 3_765 ? C12 C13 1.607(19) 3_765 ? C12 C13 1.607(19) . ? C12 C10 1.96(3) 3_765 ? Cl2A Cl2B 0.98(5) . ? 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 89.74(4) 3_775 4_575 ? N1 Cu1 N1 172.2(6) 3_775 . ? N1 Cu1 N1 89.74(4) 4_575 . ? N1 Cu1 N1 89.74(4) 3_775 2_755 ? N1 Cu1 N1 172.2(6) 4_575 2_755 ? N1 Cu1 N1 89.74(4) . 2_755 ? N1 Cu1 Cl1 93.9(3) 3_775 . ? N1 Cu1 Cl1 93.9(3) 4_575 . ? N1 Cu1 Cl1 93.9(3) . . ? N1 Cu1 Cl1 93.9(3) 2_755 . ? C6 N1 C2 118.2(8) . . ? C6 N1 Cu1 119.6(7) . . ? C2 N1 Cu1 122.2(7) . . ? N1 C2 C3 122.9(11) . . ? C4 C3 C2 119.1(12) . . ? C5 C4 C3 118.3(12) . . ? C4 C5 C6 118.8(12) . . ? C4 C5 N7 130.8(12) . . ? C6 C5 N7 110.0(12) . . ? N1 C6 C5 122.6(10) . . ? C10 N7 O8 41.6(19) . . ? C10 N7 N9 90(2) . . ? O8 N7 N9 122(2) . . ? C10 N7 O11 38.7(17) . . ? O8 N7 O11 25.2(12) . . ? N9 N7 O11 129.1(18) . . ? C10 N7 C5 142(3) . . ? O8 N7 C5 121.4(18) . . ? N9 N7 C5 116.8(16) . . ? O11 N7 C5 108.9(13) . . ? O11 O8 C10 94(3) . . ? O11 O8 N7 108(3) . . ? C10 O8 N7 31.4(14) . . ? N7 N9 C10 28.2(9) . . ? N7 N9 C12 105.5(14) . . ? C10 N9 C12 80.0(11) . . ? N7 C10 O8 107(3) . . ? N7 C10 O11 120(2) . . ? O8 C10 O11 38.1(17) . . ? N7 C10 N9 61(2) . . ? O8 C10 N9 143(3) . . ? O11 C10 N9 178.4(18) . . ? N7 C10 C12 110(2) . . ? O8 C10 C12 111(3) . . ? O11 C10 C12 126.7(16) . . ? N9 C10 C12 52.5(10) . . ? O8 O11 C10 48(2) . . ? O8 O11 N7 47.2(18) . . ? C10 O11 N7 21.3(10) . . ? N9 C12 N9 97(3) . 3_765 ? N9 C12 C13 96.8(11) . 3_765 ? N9 C12 C13 131.8(11) 3_765 3_765 ? N9 C12 C13 131.8(11) . . ? N9 C12 C13 96.8(11) 3_765 . ? C13 C12 C13 108(3) 3_765 . ? N9 C12 C10 83.8(18) . 3_765 ? N9 C12 C10 47.5(10) 3_765 3_765 ? C13 C12 C10 88.6(11) 3_765 3_765 ? C13 C12 C10 136.2(10) . 3_765 ? N9 C12 C10 47.5(10) . . ? N9 C12 C10 83.8(18) 3_765 . ? C13 C12 C10 136.2(10) 3_765 . ? C13 C12 C10 88.6(11) . . ? C10 C12 C10 108(2) 3_765 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.687 _refine_diff_density_min -0.622 _refine_diff_density_rms 0.216