data_publication_text _publ_contact_author_name 'Jon Zubieta' _publ_contact_author_address ; Department of Chemistry 111 College Place Syracuse University Syracuse, NY 13244 ; data_pmn21a Compound 1 [Cu3(trz)4(H2O)3]F2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H7 Cu1.50 F N6 O1.50' _chemical_formula_weight 277.47 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' '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pmn2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y, z+1/2' '-x, y, z' _cell_length_a 8.9307(6) _cell_length_b 12.8226(9) _cell_length_c 7.9821(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 914.07(11) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 2924 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 28.22 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.016 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 550 _exptl_absorpt_coefficient_mu 3.518 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6205 _exptl_absorpt_correction_T_max 0.7661 _exptl_absorpt_process_details 'SADABS SHELXL-97 (SHELDRICK, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX CCD area detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 9485 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0310 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 28.27 _reflns_number_total 2394 _reflns_number_gt 2315 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0413P)^2^+0.9007P] 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 0.0(4) _refine_ls_number_reflns 2394 _refine_ls_number_parameters 137 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0303 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0777 _refine_ls_wR_factor_gt 0.0763 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _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 0.0000 0.01547(4) 1.00222(6) 0.00615(13) Uani 1 2 d S . . Cu2 Cu 0.0000 0.50764(4) 0.59137(7) 0.00687(13) Uani 1 2 d S . . Cu3 Cu 0.0000 0.25217(4) 0.77156(8) 0.00663(12) Uani 1 2 d S . . F1 F 0.2783(2) 0.75253(15) 0.7884(3) 0.0134(4) Uani 1 1 d . . . O90 O 0.0000 0.1815(3) 1.0961(5) 0.0115(7) Uani 1 2 d S . . O91 O 0.0000 0.3071(3) 0.4881(5) 0.0121(7) Uani 1 2 d S . . O92 O 0.0000 0.6782(3) 0.7188(5) 0.0166(8) Uani 1 2 d S . . N1 N 0.1550(3) 0.0494(2) 0.8312(4) 0.0085(5) Uani 1 1 d . . . N2 N 0.1574(3) 0.1429(2) 0.7478(4) 0.0078(5) Uani 1 1 d . . . N3 N 0.1572(3) 0.3575(2) 0.8159(4) 0.0082(5) Uani 1 1 d . . . N4 N 0.1548(3) 0.4560(2) 0.7501(4) 0.0077(5) Uani 1 1 d . . . N5 N 0.3405(3) 0.4479(2) 0.9321(4) 0.0088(6) Uani 1 1 d . . . N6 N 0.3400(3) 0.0442(2) 0.6475(4) 0.0078(5) Uani 1 1 d . . . C1 C 0.2668(6) 0.5075(3) 0.8218(6) 0.0094(8) Uani 1 1 d . . . H1 H 0.2915 0.5780 0.7978 0.011 Uiso 1 1 calc R . . C2 C 0.2699(4) 0.3551(3) 0.9239(4) 0.0094(6) Uani 1 1 d . . . H2 H 0.2974 0.2955 0.9875 0.011 Uiso 1 1 calc R . . C3 C 0.2640(6) -0.0074(3) 0.7677(6) 0.0111(8) Uani 1 1 d . . . H3 H 0.2864 -0.0765 0.8025 0.013 Uiso 1 1 calc R . . C4 C 0.2702(4) 0.1373(2) 0.6408(4) 0.0096(6) Uani 1 1 d . . . H4 H 0.2986 0.1924 0.5679 0.011 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 0.0044(3) 0.0084(2) 0.0057(3) 0.0011(2) 0.000 0.000 Cu2 0.0039(3) 0.0109(3) 0.0058(3) 0.0025(2) 0.000 0.000 Cu3 0.0048(2) 0.0044(2) 0.0108(3) -0.0009(2) 0.000 0.000 F1 0.0128(8) 0.0119(9) 0.0155(11) 0.0000(7) 0.0010(10) -0.0014(8) O90 0.0120(17) 0.0129(16) 0.0097(16) -0.0019(14) 0.000 0.000 O91 0.0141(17) 0.0114(15) 0.0109(17) -0.0022(14) 0.000 0.000 O92 0.0076(17) 0.0169(19) 0.025(2) -0.0048(15) 0.000 0.000 N1 0.0086(14) 0.0089(13) 0.0081(12) 0.0018(11) 0.0002(11) 0.0036(10) N2 0.0080(14) 0.0074(12) 0.0079(13) 0.0016(11) 0.0022(11) 0.0015(10) N3 0.0079(14) 0.0075(12) 0.0093(13) 0.0014(10) -0.0002(10) 0.0008(10) N4 0.0081(13) 0.0087(12) 0.0064(12) 0.0016(11) -0.0016(11) -0.0004(10) N5 0.0075(14) 0.0094(13) 0.0095(14) -0.0011(10) -0.0008(11) 0.0000(10) N6 0.0070(13) 0.0103(13) 0.0062(13) 0.0002(10) 0.0002(10) 0.0006(11) C1 0.009(2) 0.0090(14) 0.0106(18) -0.0006(12) -0.0011(16) -0.0022(12) C2 0.0104(16) 0.0111(15) 0.0067(14) 0.0004(12) 0.0014(12) 0.0024(12) C3 0.011(2) 0.0072(14) 0.0148(16) 0.0028(15) 0.0027(18) 0.0000(11) C4 0.0077(15) 0.0095(15) 0.0115(15) 0.0011(12) 0.0037(13) 0.0002(12) _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 1.993(3) 4 ? Cu1 N1 1.993(3) . ? Cu1 N6 1.993(3) 2 ? Cu1 N6 1.993(3) 3_455 ? Cu1 O90 2.257(3) . ? Cu2 N4 1.989(3) . ? Cu2 N4 1.989(3) 4 ? Cu2 N5 1.992(3) 3_464 ? Cu2 N5 1.992(3) 2_564 ? Cu2 O92 2.412(4) . ? Cu3 N3 1.981(3) . ? Cu3 N3 1.981(3) 4 ? Cu3 N2 1.994(3) 4 ? Cu3 N2 1.994(3) . ? Cu3 O91 2.370(4) . ? N1 C3 1.317(6) . ? N1 N2 1.371(4) . ? N2 C4 1.322(4) . ? N3 C2 1.325(4) . ? N3 N4 1.367(4) . ? N4 C1 1.328(6) . ? N5 C1 1.339(5) . ? N5 C2 1.348(4) . ? N5 Cu2 1.992(3) 2_565 ? N6 C3 1.348(5) . ? N6 C4 1.349(4) . ? N6 Cu1 1.993(3) 2_554 ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 H4 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 N1 Cu1 N1 88.02(17) 4 . ? N1 Cu1 N6 168.74(11) 4 2 ? N1 Cu1 N6 89.11(12) . 2 ? N1 Cu1 N6 89.12(12) 4 3_455 ? N1 Cu1 N6 168.74(11) . 3_455 ? N6 Cu1 N6 91.60(17) 2 3_455 ? N1 Cu1 O90 91.23(11) 4 . ? N1 Cu1 O90 91.23(11) . . ? N6 Cu1 O90 99.71(11) 2 . ? N6 Cu1 O90 99.71(11) 3_455 . ? N4 Cu2 N4 88.06(17) . 4 ? N4 Cu2 N5 177.09(12) . 3_464 ? N4 Cu2 N5 90.28(11) 4 3_464 ? N4 Cu2 N5 90.28(11) . 2_564 ? N4 Cu2 N5 177.09(12) 4 2_564 ? N5 Cu2 N5 91.27(17) 3_464 2_564 ? N4 Cu2 O92 91.91(11) . . ? N4 Cu2 O92 91.91(11) 4 . ? N5 Cu2 O92 90.53(11) 3_464 . ? N5 Cu2 O92 90.53(11) 2_564 . ? N3 Cu3 N3 90.30(16) . 4 ? N3 Cu3 N2 175.07(14) . 4 ? N3 Cu3 N2 89.81(10) 4 4 ? N3 Cu3 N2 89.81(10) . . ? N3 Cu3 N2 175.07(14) 4 . ? N2 Cu3 N2 89.65(16) 4 . ? N3 Cu3 O91 88.14(10) . . ? N3 Cu3 O91 88.14(10) 4 . ? N2 Cu3 O91 96.78(10) 4 . ? N2 Cu3 O91 96.78(10) . . ? C3 N1 N2 106.6(3) . . ? C3 N1 Cu1 131.0(3) . . ? N2 N1 Cu1 122.3(2) . . ? C4 N2 N1 106.2(3) . . ? C4 N2 Cu3 129.5(2) . . ? N1 N2 Cu3 123.8(2) . . ? C2 N3 N4 106.5(3) . . ? C2 N3 Cu3 129.6(2) . . ? N4 N3 Cu3 123.4(2) . . ? C1 N4 N3 106.4(3) . . ? C1 N4 Cu2 129.2(2) . . ? N3 N4 Cu2 124.3(2) . . ? C1 N5 C2 104.0(3) . . ? C1 N5 Cu2 127.4(3) . 2_565 ? C2 N5 Cu2 128.2(2) . 2_565 ? C3 N6 C4 103.3(3) . . ? C3 N6 Cu1 125.9(3) . 2_554 ? C4 N6 Cu1 130.4(2) . 2_554 ? N4 C1 N5 111.7(3) . . ? N4 C1 H1 124.2 . . ? N5 C1 H1 124.2 . . ? N3 C2 N5 111.5(3) . . ? N3 C2 H2 124.3 . . ? N5 C2 H2 124.3 . . ? N1 C3 N6 112.0(3) . . ? N1 C3 H3 124.0 . . ? N6 C3 H3 124.0 . . ? N2 C4 N6 112.0(3) . . ? N2 C4 H4 124.0 . . ? N6 C4 H4 124.0 . . ? 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 C3 -121.4(4) 4 . . . ? N6 Cu1 N1 C3 47.7(4) 2 . . . ? N6 Cu1 N1 C3 -46.1(8) 3_455 . . . ? O90 Cu1 N1 C3 147.4(4) . . . . ? N1 Cu1 N1 N2 54.2(3) 4 . . . ? N6 Cu1 N1 N2 -136.7(3) 2 . . . ? N6 Cu1 N1 N2 129.5(5) 3_455 . . . ? O90 Cu1 N1 N2 -37.0(3) . . . . ? C3 N1 N2 C4 -1.2(4) . . . . ? Cu1 N1 N2 C4 -177.7(2) . . . . ? C3 N1 N2 Cu3 171.6(3) . . . . ? Cu1 N1 N2 Cu3 -4.9(4) . . . . ? N3 Cu3 N2 C4 -60.0(3) . . . . ? N3 Cu3 N2 C4 -151.3(13) 4 . . . ? N2 Cu3 N2 C4 124.9(3) 4 . . . ? O91 Cu3 N2 C4 28.1(3) . . . . ? N3 Cu3 N2 N1 129.0(3) . . . . ? N3 Cu3 N2 N1 37.6(16) 4 . . . ? N2 Cu3 N2 N1 -46.1(3) 4 . . . ? O91 Cu3 N2 N1 -142.9(3) . . . . ? N3 Cu3 N3 C2 124.4(3) 4 . . . ? N2 Cu3 N3 C2 33.0(16) 4 . . . ? N2 Cu3 N3 C2 -50.7(3) . . . . ? O91 Cu3 N3 C2 -147.5(3) . . . . ? N3 Cu3 N3 N4 -46.4(3) 4 . . . ? N2 Cu3 N3 N4 -137.8(14) 4 . . . ? N2 Cu3 N3 N4 138.5(3) . . . . ? O91 Cu3 N3 N4 41.7(3) . . . . ? C2 N3 N4 C1 0.2(4) . . . . ? Cu3 N3 N4 C1 172.9(3) . . . . ? C2 N3 N4 Cu2 -175.8(2) . . . . ? Cu3 N3 N4 Cu2 -3.1(4) . . . . ? N4 Cu2 N4 C1 -124.3(3) 4 . . . ? N5 Cu2 N4 C1 -180(97) 3_464 . . . ? N5 Cu2 N4 C1 58.1(4) 2_564 . . . ? O92 Cu2 N4 C1 -32.4(4) . . . . ? N4 Cu2 N4 N3 50.8(3) 4 . . . ? N5 Cu2 N4 N3 -4(3) 3_464 . . . ? N5 Cu2 N4 N3 -126.8(3) 2_564 . . . ? O92 Cu2 N4 N3 142.7(3) . . . . ? N3 N4 C1 N5 -0.8(5) . . . . ? Cu2 N4 C1 N5 175.0(2) . . . . ? C2 N5 C1 N4 0.9(5) . . . . ? Cu2 N5 C1 N4 -172.1(2) 2_565 . . . ? N4 N3 C2 N5 0.3(4) . . . . ? Cu3 N3 C2 N5 -171.7(2) . . . . ? C1 N5 C2 N3 -0.8(4) . . . . ? Cu2 N5 C2 N3 172.2(2) 2_565 . . . ? N2 N1 C3 N6 0.8(5) . . . . ? Cu1 N1 C3 N6 176.9(3) . . . . ? C4 N6 C3 N1 0.0(5) . . . . ? Cu1 N6 C3 N1 -173.6(3) 2_554 . . . ? N1 N2 C4 N6 1.2(4) . . . . ? Cu3 N2 C4 N6 -171.0(2) . . . . ? C3 N6 C4 N2 -0.8(4) . . . . ? Cu1 N6 C4 N2 172.4(2) 2_554 . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.094 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.117 loop_ _publ_author_name _publ_author_address 'Wayne Ouellette' ;Department of Chemistry 111 College Place Syracuse University Syracuse, NY 13244 ;