data_global _publ_contact_author_name 'Brendan Twamley' _publ_contact_author_address ;University Research Office 114 Morrill Hall University of Idaho Moscow ID, 83844-3010 ; _publ_contact_author_email btwamley@uidaho.edu _publ_contact_author_phone '208 885 2847' _publ_contact_author_fax '208 885 2847' loop_ _publ_author_name _publ_author_address 'Gao, Ye' ;Department of Chemistry University of Idaho Moscow ID 83844-2343 ; 'Twamley, Brendan' ;Department of Chemistry University of Idaho Moscow ID 83844-2343 ; "Shreeve, Jean'ne" ;Department of Chemistry University of Idaho Moscow ID 83844-2343 ; data_bt691_compound3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Fec-CH2-triazole-AgNO3 polymer' _chemical_melting_point ? _chemical_formula_moiety 'C16 H16 Ag Fe N6, N O3' _chemical_formula_sum 'C16 H16 Ag Fe N7 O3' _chemical_formula_weight 518.08 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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.2379(11) _cell_length_b 7.6304(4) _cell_length_c 10.6537(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.2920(10) _cell_angle_gamma 90.00 _cell_volume 1743.76(15) _cell_formula_units_Z 4 _cell_measurement_temperature 86(2) _cell_measurement_reflns_used 7935 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 29.88 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.973 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 1.991 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6685 _exptl_absorpt_correction_T_max 0.9427 _exptl_absorpt_process_details 'SADABS; Bruker, 2001' _exptl_special_details ; ? ; _diffrn_ambient_temperature 86(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker/Siemens SMART APEX' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12682 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0220 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 27.50 _reflns_number_total 1987 _reflns_number_gt 1918 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART v. 5.626' _computing_cell_refinement 'Bruker SAINT+ v. 6.45' _computing_data_reduction 'Bruker SAINT+ v. 6.45' _computing_structure_solution 'XS, Bruker SHELXTL v. 6.12' _computing_structure_refinement 'XL, Bruker SHELXTL v. 6.12' _computing_molecular_graphics 'XP, Bruker SHELXTL v. 6.12' _computing_publication_material 'XCIF, Bruker SHELXTL v. 6.12' _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^)+(0.0241P)^2^+8.6309P] 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 1987 _refine_ls_number_parameters 123 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0310 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0659 _refine_ls_wR_factor_gt 0.0651 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.037 _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 Ag1 Ag 0.5000 0.64587(4) 0.2500 0.01831(9) Uani 1 2 d S . . Fe1 Fe 0.24234(19) 1.2536(11) 0.4936(7) 0.0130(6) Uani 0.50 1 d P A -1 C1A C 0.1954(3) 1.0691(8) 0.3625(5) 0.0124(15) Uiso 0.50 1 d PD A -1 H1AA H 0.1523 1.0414 0.3449 0.015 Uiso 0.50 1 calc PR A -1 C2A C 0.2220(3) 1.1975(6) 0.2974(5) 0.0112(10) Uiso 0.50 1 d PD A -1 H2AA H 0.1997 1.2699 0.2282 0.013 Uiso 0.50 1 calc PR A -1 C3A C 0.2867(3) 1.2001(6) 0.3517(5) 0.0115(10) Uiso 0.50 1 d PD A -1 H3AA H 0.3156 1.2741 0.3257 0.014 Uiso 0.50 1 calc PR A -1 C4A C 0.3015(3) 1.0716(8) 0.4532(6) 0.0143(14) Uiso 0.50 1 d PD A -1 C5A C 0.2438(3) 0.9899(13) 0.4575(9) 0.017(4) Uiso 0.50 1 d PD A -1 H5AA H 0.2392 0.8984 0.5147 0.021 Uiso 0.50 1 calc PR A -1 C6A C 0.3652(2) 1.0293(8) 0.5383(5) 0.0178(11) Uiso 0.50 1 d PD A -1 H6AA H 0.3922 1.1341 0.5464 0.021 Uiso 0.50 1 calc PR A -1 H6AB H 0.3620 0.9973 0.6263 0.021 Uiso 0.50 1 calc PR A -1 C8A C 0.4296(3) 0.8876(8) 0.4022(7) 0.0185(16) Uiso 0.50 1 d PD A -1 H8AA H 0.4442 0.9910 0.3701 0.022 Uiso 0.50 1 calc PR A -1 C10A C 0.4127(3) 0.6251(10) 0.4436(7) 0.023(2) Uiso 0.50 1 d PD A -1 H10A H 0.4144 0.5007 0.4446 0.027 Uiso 0.50 1 calc PR A -1 N7A N 0.3935(2) 0.8835(7) 0.4836(5) 0.0181(12) Uiso 0.50 1 d PD A -1 N9A N 0.4421(3) 0.7253(8) 0.3726(7) 0.021(2) Uiso 0.50 1 d PD A -1 N11A N 0.3816(2) 0.7152(8) 0.5105(5) 0.0195(13) Uiso 0.50 1 d PD A -1 C1B C 0.2899(3) 1.4163(8) 0.6370(6) 0.0182(18) Uiso 0.50 1 d PD A -1 H1BA H 0.3338 1.4289 0.6666 0.022 Uiso 0.50 1 calc PR A -1 C2B C 0.2529(3) 1.2973(6) 0.6870(5) 0.0151(11) Uiso 0.50 1 d PD A -1 H2BA H 0.2679 1.2154 0.7552 0.018 Uiso 0.50 1 calc PR A -1 C3B C 0.1906(3) 1.3216(7) 0.6184(5) 0.0160(11) Uiso 0.50 1 d PD A -1 H3BA H 0.1560 1.2599 0.6332 0.019 Uiso 0.50 1 calc PR A -1 C4B C 0.1875(3) 1.4548(8) 0.5223(6) 0.0147(14) Uiso 0.50 1 d PD A -1 C5B C 0.2496(3) 1.5136(11) 0.5348(8) 0.009(3) Uiso 0.50 1 d PD A -1 H5BA H 0.2620 1.6019 0.4839 0.011 Uiso 0.50 1 calc PR A -1 C6B C 0.1308(2) 1.5261(8) 0.4295(5) 0.0199(11) Uiso 0.50 1 d PD A -1 H6BA H 0.1420 1.5753 0.3527 0.024 Uiso 0.50 1 calc PR A -1 H6BB H 0.1004 1.4304 0.3993 0.024 Uiso 0.50 1 calc PR A -1 C8B C 0.0658(3) 1.6431(8) 0.5719(7) 0.0215(17) Uiso 0.50 1 d PD A -1 H8BA H 0.0515 1.5341 0.5958 0.026 Uiso 0.50 1 calc PR A -1 C10B C 0.0844(3) 1.9121(10) 0.5546(7) 0.018(2) Uiso 0.50 1 d PD A -1 H10B H 0.0844 2.0354 0.5672 0.022 Uiso 0.50 1 calc PR A -1 N7B N 0.1022(2) 1.6636(7) 0.4916(5) 0.0194(12) Uiso 0.50 1 d PD A -1 N9B N 0.0529(3) 1.7988(8) 0.6130(6) 0.016(2) Uiso 0.50 1 d PD . -1 N11B N 0.1147(2) 1.8358(8) 0.4793(5) 0.0210(13) Uiso 0.50 1 d PD A -1 N1 N 0.5000 0.2348(4) 0.2500 0.0285(8) Uani 1 2 d S . . O1 O 0.46951(11) 0.3161(3) 0.3139(2) 0.0428(6) Uani 1 1 d . . . O2 O 0.5000 0.0730(4) 0.2500 0.0490(10) Uani 1 2 d S . . 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 Ag1 0.02036(15) 0.01940(15) 0.01969(15) 0.000 0.01327(10) 0.000 Fe1 0.0204(18) 0.0082(6) 0.0127(12) -0.0002(7) 0.0088(16) 0.0006(15) N1 0.0185(16) 0.0177(16) 0.045(2) 0.000 0.0012(15) 0.000 O1 0.0316(12) 0.0458(14) 0.0469(14) -0.0158(12) 0.0033(11) 0.0150(11) O2 0.066(3) 0.0130(15) 0.062(2) 0.000 0.007(2) 0.000 _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 Ag1 N9B 2.144(5) 7_576 ? Ag1 N9B 2.144(5) 8_575 ? Ag1 N9A 2.149(5) . ? Ag1 N9A 2.149(5) 2_655 ? Fe1 C5B 2.028(12) . ? Fe1 C4B 2.032(9) . ? Fe1 C1B 2.034(10) . ? Fe1 C4A 2.036(9) . ? Fe1 C2B 2.038(9) . ? Fe1 C3B 2.041(9) . ? Fe1 C5A 2.051(13) . ? Fe1 C3A 2.052(9) . ? Fe1 C1A 2.063(10) . ? Fe1 C2A 2.064(9) . ? C1A C5A 1.405(7) . ? C1A C2A 1.418(7) . ? C1A H1AA 0.9500 . ? C2A C3A 1.400(7) . ? C2A H2AA 0.9500 . ? C3A C4A 1.433(8) . ? C3A H3AA 0.9500 . ? C4A C5A 1.438(7) . ? C4A C6A 1.501(8) . ? C5A H5AA 0.9500 . ? C6A N7A 1.472(6) . ? C6A H6AA 0.9900 . ? C6A H6AB 0.9900 . ? C8A N9A 1.326(7) . ? C8A N7A 1.329(6) . ? C8A H8AA 0.9500 . ? C10A N11A 1.311(7) . ? C10A N9A 1.358(7) . ? C10A H10A 0.9500 . ? N7A N11A 1.357(7) . ? C1B C2B 1.419(8) . ? C1B C5B 1.422(7) . ? C1B H1BA 0.9500 . ? C2B C3B 1.398(7) . ? C2B H2BA 0.9500 . ? C3B C4B 1.431(7) . ? C3B H3BA 0.9500 . ? C4B C5B 1.424(7) . ? C4B C6B 1.486(8) . ? C5B H5BA 0.9500 . ? C6B N7B 1.471(6) . ? C6B H6BA 0.9900 . ? C6B H6BB 0.9900 . ? C8B N9B 1.324(7) . ? C8B N7B 1.333(6) . ? C8B H8BA 0.9500 . ? C10B N11B 1.312(7) . ? C10B N9B 1.362(7) . ? C10B H10B 0.9500 . ? N7B N11B 1.356(7) . ? N9B Ag1 2.144(5) 7_576 ? N1 O2 1.234(5) . ? N1 O1 1.246(3) 2_655 ? N1 O1 1.246(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 N9B Ag1 N9B 157.3(3) 7_576 8_575 ? N9B Ag1 N9A 6.6(3) 7_576 . ? N9B Ag1 N9A 151.9(2) 8_575 . ? N9B Ag1 N9A 151.9(2) 7_576 2_655 ? N9B Ag1 N9A 6.6(3) 8_575 2_655 ? N9A Ag1 N9A 147.3(3) . 2_655 ? C5B Fe1 C4B 41.1(3) . . ? C5B Fe1 C1B 41.0(3) . . ? C4B Fe1 C1B 68.9(4) . . ? C5B Fe1 C4A 133.9(4) . . ? C4B Fe1 C4A 173.5(5) . . ? C1B Fe1 C4A 109.8(3) . . ? C5B Fe1 C2B 68.9(4) . . ? C4B Fe1 C2B 68.8(3) . . ? C1B Fe1 C2B 40.8(3) . . ? C4A Fe1 C2B 114.6(4) . . ? C5B Fe1 C3B 68.7(3) . . ? C4B Fe1 C3B 41.1(3) . . ? C1B Fe1 C3B 68.0(4) . . ? C4A Fe1 C3B 144.9(5) . . ? C2B Fe1 C3B 40.1(3) . . ? C5B Fe1 C5A 174.7(4) . . ? C4B Fe1 C5A 144.0(4) . . ? C1B Fe1 C5A 135.1(4) . . ? C4A Fe1 C5A 41.2(3) . . ? C2B Fe1 C5A 110.3(5) . . ? C3B Fe1 C5A 114.3(5) . . ? C5B Fe1 C3A 109.1(4) . . ? C4B Fe1 C3A 133.2(5) . . ? C1B Fe1 C3A 114.8(4) . . ? C4A Fe1 C3A 41.0(3) . . ? C2B Fe1 C3A 145.8(3) . . ? C3B Fe1 C3A 173.3(3) . . ? C5A Fe1 C3A 68.4(4) . . ? C5B Fe1 C1A 144.2(4) . . ? C4B Fe1 C1A 113.6(3) . . ? C1B Fe1 C1A 174.2(5) . . ? C4A Fe1 C1A 68.4(3) . . ? C2B Fe1 C1A 134.4(5) . . ? C3B Fe1 C1A 110.1(4) . . ? C5A Fe1 C1A 39.9(3) . . ? C3A Fe1 C1A 67.7(3) . . ? C5B Fe1 C2A 113.9(4) . . ? C4B Fe1 C2A 109.2(3) . . ? C1B Fe1 C2A 144.9(5) . . ? C4A Fe1 C2A 68.0(3) . . ? C2B Fe1 C2A 173.6(4) . . ? C3B Fe1 C2A 134.6(3) . . ? C5A Fe1 C2A 67.4(4) . . ? C3A Fe1 C2A 39.8(2) . . ? C1A Fe1 C2A 40.2(2) . . ? C5A C1A C2A 108.0(6) . . ? C5A C1A Fe1 69.5(5) . . ? C2A C1A Fe1 70.0(4) . . ? C5A C1A H1AA 126.0 . . ? C2A C1A H1AA 126.0 . . ? Fe1 C1A H1AA 126.1 . . ? C3A C2A C1A 108.9(4) . . ? C3A C2A Fe1 69.6(3) . . ? C1A C2A Fe1 69.9(4) . . ? C3A C2A H2AA 125.6 . . ? C1A C2A H2AA 125.6 . . ? Fe1 C2A H2AA 126.5 . . ? C2A C3A C4A 108.0(4) . . ? C2A C3A Fe1 70.6(3) . . ? C4A C3A Fe1 68.9(3) . . ? C2A C3A H3AA 126.0 . . ? C4A C3A H3AA 126.0 . . ? Fe1 C3A H3AA 126.1 . . ? C3A C4A C5A 106.9(5) . . ? C3A C4A C6A 126.6(5) . . ? C5A C4A C6A 126.5(5) . . ? C3A C4A Fe1 70.1(4) . . ? C5A C4A Fe1 69.9(5) . . ? C6A C4A Fe1 125.3(4) . . ? C1A C5A C4A 108.2(5) . . ? C1A C5A Fe1 70.5(5) . . ? C4A C5A Fe1 68.9(5) . . ? C1A C5A H5AA 125.9 . . ? C4A C5A H5AA 125.9 . . ? Fe1 C5A H5AA 126.3 . . ? N7A C6A C4A 110.9(4) . . ? N7A C6A H6AA 109.5 . . ? C4A C6A H6AA 109.5 . . ? N7A C6A H6AB 109.5 . . ? C4A C6A H6AB 109.5 . . ? H6AA C6A H6AB 108.0 . . ? N9A C8A N7A 109.5(6) . . ? N9A C8A H8AA 125.3 . . ? N7A C8A H8AA 125.3 . . ? N11A C10A N9A 114.1(7) . . ? N11A C10A H10A 122.9 . . ? N9A C10A H10A 122.9 . . ? C8A N7A N11A 110.2(4) . . ? C8A N7A C6A 129.4(5) . . ? N11A N7A C6A 120.3(4) . . ? C8A N9A C10A 103.4(5) . . ? C8A N9A Ag1 127.2(5) . . ? C10A N9A Ag1 129.3(5) . . ? C10A N11A N7A 102.7(5) . . ? C2B C1B C5B 108.2(6) . . ? C2B C1B Fe1 69.7(4) . . ? C5B C1B Fe1 69.3(5) . . ? C2B C1B H1BA 125.9 . . ? C5B C1B H1BA 125.9 . . ? Fe1 C1B H1BA 126.6 . . ? C3B C2B C1B 108.1(4) . . ? C3B C2B Fe1 70.1(3) . . ? C1B C2B Fe1 69.5(4) . . ? C3B C2B H2BA 125.9 . . ? C1B C2B H2BA 125.9 . . ? Fe1 C2B H2BA 126.1 . . ? C2B C3B C4B 108.8(4) . . ? C2B C3B Fe1 69.9(3) . . ? C4B C3B Fe1 69.1(4) . . ? C2B C3B H3BA 125.6 . . ? C4B C3B H3BA 125.6 . . ? Fe1 C3B H3BA 127.0 . . ? C5B C4B C3B 107.1(5) . . ? C5B C4B C6B 125.4(5) . . ? C3B C4B C6B 127.4(5) . . ? C5B C4B Fe1 69.3(5) . . ? C3B C4B Fe1 69.8(4) . . ? C6B C4B Fe1 127.9(4) . . ? C1B C5B C4B 107.8(5) . . ? C1B C5B Fe1 69.7(5) . . ? C4B C5B Fe1 69.6(4) . . ? C1B C5B H5BA 126.1 . . ? C4B C5B H5BA 126.1 . . ? Fe1 C5B H5BA 126.1 . . ? N7B C6B C4B 110.7(4) . . ? N7B C6B H6BA 109.5 . . ? C4B C6B H6BA 109.5 . . ? N7B C6B H6BB 109.5 . . ? C4B C6B H6BB 109.5 . . ? H6BA C6B H6BB 108.1 . . ? N9B C8B N7B 109.2(6) . . ? N9B C8B H8BA 125.4 . . ? N7B C8B H8BA 125.4 . . ? N11B C10B N9B 114.0(7) . . ? N11B C10B H10B 123.0 . . ? N9B C10B H10B 123.0 . . ? C8B N7B N11B 110.5(4) . . ? C8B N7B C6B 127.7(6) . . ? N11B N7B C6B 121.6(5) . . ? C8B N9B C10B 103.6(5) . . ? C8B N9B Ag1 127.4(5) . 7_576 ? C10B N9B Ag1 128.8(5) . 7_576 ? C10B N11B N7B 102.7(5) . . ? O2 N1 O1 119.86(19) . 2_655 ? O2 N1 O1 119.86(19) . . ? O1 N1 O1 120.3(4) 2_655 . ? 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 C1A H1AA N11B 0.95 2.42 3.019(9) 121.1 1_545 C8A H8AA O2 0.95 2.10 2.902(6) 141.2 1_565 C8A H8AA O2 0.95 2.10 2.902(6) 141.2 2_665 C10A H10A O1 0.95 2.51 3.161(7) 125.3 . C10B H10B O1 0.95 2.26 2.930(7) 126.5 7_576 C8B H8BA O2 0.95 2.38 3.151(7) 138.0 7_566 C8B H8BA O2 0.95 2.38 3.151(7) 138.0 8_466 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.637 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.091 #===END data_bt698_compound4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Fec-CH2-triazole-CdCl2)n polymer' _chemical_melting_point ? _chemical_formula_moiety 'C32 H32 Cd Cl2 Fe2 N12' _chemical_formula_sum 'C32 H32 Cd Cl2 Fe2 N12' _chemical_formula_weight 879.70 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.0577(3) _cell_length_b 8.5381(4) _cell_length_c 15.1071(6) _cell_angle_alpha 98.342(1) _cell_angle_beta 92.997(1) _cell_angle_gamma 112.781(1) _cell_volume 824.56(6) _cell_formula_units_Z 1 _cell_measurement_temperature 86(2) _cell_measurement_reflns_used 7780 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 30.00 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.772 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 442 _exptl_absorpt_coefficient_mu 1.715 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7147 _exptl_absorpt_correction_T_max 0.9041 _exptl_absorpt_process_details 'SADABS; Bruker, 2001' _exptl_special_details ; ? ; _diffrn_ambient_temperature 86(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker/Siemens SMART APEX' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12320 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3769 _reflns_number_gt 3442 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART v. 5.626' _computing_cell_refinement 'Bruker SAINT+ v. 6.45' _computing_data_reduction 'Bruker SAINT+ v. 6.45' _computing_structure_solution 'XS, Bruker SHELXTL v. 6.12' _computing_structure_refinement 'XL, Bruker SHELXTL v. 6.12' _computing_molecular_graphics 'XP, Bruker SHELXTL v. 6.12' _computing_publication_material 'XCIF, Bruker SHELXTL v. 6.12' _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^)+(0.0317P)^2^+0.5802P] 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 3769 _refine_ls_number_parameters 223 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0327 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0664 _refine_ls_wR_factor_gt 0.0648 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 Cl1 Cl 1.36121(8) 0.19445(7) 0.45834(4) 0.01412(12) Uani 1 1 d . . . C1 C 0.8036(4) 0.5183(3) 0.85357(16) 0.0148(5) Uani 1 1 d . . . H1 H 0.7332 0.4001 0.8578 0.018 Uiso 1 1 calc R . . C2 C 0.9207(4) 0.6544(3) 0.92580(16) 0.0177(5) Uani 1 1 d . . . H2 H 0.9428 0.6430 0.9867 0.021 Uiso 1 1 calc R . . C3 C 0.9991(4) 0.8110(3) 0.89110(16) 0.0174(5) Uani 1 1 d . . . H3 H 1.0816 0.9224 0.9247 0.021 Uiso 1 1 calc R . . C4 C 0.9320(4) 0.7709(3) 0.79758(16) 0.0142(5) Uani 1 1 d . . . H4 H 0.9631 0.8511 0.7575 0.017 Uiso 1 1 calc R . . C5 C 0.8102(3) 0.5901(3) 0.77354(15) 0.0121(4) Uani 1 1 d . . . C6 C 0.7112(4) 0.4983(3) 0.68036(16) 0.0135(5) Uani 1 1 d . . . H6A H 0.5759 0.4046 0.6837 0.016 Uiso 1 1 calc R . . H6B H 0.6860 0.5803 0.6462 0.016 Uiso 1 1 calc R . . C9 C 1.1020(4) 0.4146(3) 0.57488(15) 0.0122(4) Uani 1 1 d . . . H9 H 1.2358 0.4467 0.5557 0.015 Uiso 1 1 calc R . . C11 C 0.7974(4) 0.2615(3) 0.59554(15) 0.0129(4) Uani 1 1 d . . . H11 H 0.6689 0.1677 0.5958 0.015 Uiso 1 1 calc R . . C12 C 0.3916(4) 0.6541(3) 0.81205(17) 0.0155(5) Uani 1 1 d . . . H12 H 0.3279 0.5900 0.7539 0.019 Uiso 1 1 calc R . . C13 C 0.3816(4) 0.5861(3) 0.89355(18) 0.0189(5) Uani 1 1 d . . . H13 H 0.3104 0.4687 0.8990 0.023 Uiso 1 1 calc R . . C14 C 0.4963(4) 0.7245(4) 0.96476(17) 0.0206(5) Uani 1 1 d . . . H14 H 0.5155 0.7159 1.0263 0.025 Uiso 1 1 calc R . . C15 C 0.5775(4) 0.8783(3) 0.92829(16) 0.0172(5) Uani 1 1 d . . . H15 H 0.6597 0.9904 0.9612 0.021 Uiso 1 1 calc R . . C16 C 0.5141(4) 0.8350(3) 0.83349(15) 0.0132(5) Uani 1 1 d . . . C17 C 0.5782(4) 0.9570(3) 0.76825(16) 0.0149(5) Uani 1 1 d . . . H17A H 0.6969 1.0631 0.7981 0.018 Uiso 1 1 calc R . . H17B H 0.6262 0.9030 0.7166 0.018 Uiso 1 1 calc R . . C20 C 0.2252(4) 1.1410(3) 0.72328(15) 0.0137(5) Uani 1 1 d . . . H20 H 0.1613 1.2200 0.7362 0.016 Uiso 1 1 calc R . . C22 C 0.2997(3) 0.9444(3) 0.65393(15) 0.0118(4) Uani 1 1 d . . . H22 H 0.3049 0.8545 0.6103 0.014 Uiso 1 1 calc R . . Fe1 Fe 0.68225(5) 0.70128(4) 0.86820(2) 0.01088(9) Uani 1 1 d . . . Cd1 Cd 1.0000 0.0000 0.5000 0.00948(7) Uani 1 2 d S . . N7 N 0.8429(3) 0.4247(2) 0.63260(13) 0.0112(4) Uani 1 1 d . . . N8 N 1.0398(3) 0.5264(3) 0.61994(13) 0.0142(4) Uani 1 1 d . . . N10 N 0.9580(3) 0.2490(2) 0.55824(13) 0.0124(4) Uani 1 1 d . . . N18 N 0.4135(3) 1.0056(2) 0.73387(13) 0.0120(4) Uani 1 1 d . . . N19 N 0.3666(3) 1.1329(2) 0.78080(13) 0.0150(4) Uani 1 1 d . . . N21 N 0.1776(3) 1.0278(2) 0.64411(13) 0.0128(4) 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 Cl1 0.0123(3) 0.0153(3) 0.0160(3) 0.0039(2) 0.0044(2) 0.0062(2) C1 0.0150(11) 0.0162(12) 0.0190(12) 0.0070(9) 0.0056(9) 0.0107(10) C2 0.0172(12) 0.0291(14) 0.0125(11) 0.0039(10) 0.0015(9) 0.0152(11) C3 0.0112(11) 0.0218(12) 0.0177(12) -0.0030(10) 0.0005(9) 0.0075(10) C4 0.0122(11) 0.0172(12) 0.0160(11) 0.0040(9) 0.0048(9) 0.0081(9) C5 0.0119(11) 0.0151(11) 0.0131(11) 0.0037(9) 0.0043(9) 0.0087(9) C6 0.0130(11) 0.0138(11) 0.0160(11) 0.0004(9) 0.0041(9) 0.0083(9) C9 0.0128(11) 0.0130(11) 0.0108(11) 0.0022(8) 0.0002(8) 0.0053(9) C11 0.0134(11) 0.0121(11) 0.0140(11) 0.0021(9) 0.0017(9) 0.0062(9) C12 0.0101(11) 0.0187(12) 0.0189(12) 0.0039(9) 0.0010(9) 0.0070(9) C13 0.0141(12) 0.0227(13) 0.0265(13) 0.0135(11) 0.0107(10) 0.0104(10) C14 0.0232(13) 0.0386(15) 0.0140(12) 0.0118(11) 0.0107(10) 0.0239(12) C15 0.0203(12) 0.0236(13) 0.0130(11) -0.0009(9) 0.0018(9) 0.0160(11) C16 0.0135(11) 0.0172(11) 0.0131(11) 0.0027(9) 0.0022(9) 0.0106(9) C17 0.0130(11) 0.0185(12) 0.0159(12) 0.0054(9) 0.0010(9) 0.0084(10) C20 0.0158(11) 0.0108(11) 0.0153(11) 0.0039(9) 0.0026(9) 0.0057(9) C22 0.0119(11) 0.0118(11) 0.0127(11) 0.0042(8) 0.0029(8) 0.0047(9) Fe1 0.01109(17) 0.01415(17) 0.00978(16) 0.00257(13) 0.00261(12) 0.00728(13) Cd1 0.01082(12) 0.00972(12) 0.00920(12) 0.00101(8) 0.00116(8) 0.00574(9) N7 0.0112(9) 0.0106(9) 0.0122(9) 0.0018(7) 0.0021(7) 0.0046(7) N8 0.0129(10) 0.0153(10) 0.0139(10) 0.0030(8) 0.0034(8) 0.0048(8) N10 0.0135(9) 0.0117(9) 0.0127(9) 0.0019(7) 0.0018(7) 0.0058(8) N18 0.0126(9) 0.0125(9) 0.0118(9) 0.0028(7) 0.0015(7) 0.0058(8) N19 0.0174(10) 0.0117(9) 0.0157(10) 0.0020(8) 0.0029(8) 0.0056(8) N21 0.0123(9) 0.0125(9) 0.0139(10) 0.0041(8) 0.0028(8) 0.0044(8) _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 Cl1 Cd1 2.6162(5) . ? C1 C2 1.421(3) . ? C1 C5 1.428(3) . ? C1 Fe1 2.044(2) . ? C1 H1 0.9500 . ? C2 C3 1.424(4) . ? C2 Fe1 2.054(2) . ? C2 H2 0.9500 . ? C3 C4 1.415(3) . ? C3 Fe1 2.049(2) . ? C3 H3 0.9500 . ? C4 C5 1.425(3) . ? C4 Fe1 2.042(2) . ? C4 H4 0.9500 . ? C5 C6 1.496(3) . ? C5 Fe1 2.041(2) . ? C6 N7 1.473(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C9 N8 1.317(3) . ? C9 N10 1.361(3) . ? C9 H9 0.9500 . ? C11 N10 1.325(3) . ? C11 N7 1.329(3) . ? C11 H11 0.9500 . ? C12 C16 1.425(3) . ? C12 C13 1.429(3) . ? C12 Fe1 2.042(2) . ? C12 H12 0.9500 . ? C13 C14 1.417(4) . ? C13 Fe1 2.048(2) . ? C13 H13 0.9500 . ? C14 C15 1.420(4) . ? C14 Fe1 2.051(2) . ? C14 H14 0.9500 . ? C15 C16 1.428(3) . ? C15 Fe1 2.047(2) . ? C15 H15 0.9500 . ? C16 C17 1.497(3) . ? C16 Fe1 2.036(2) . ? C17 N18 1.472(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C20 N19 1.318(3) . ? C20 N21 1.360(3) . ? C20 H20 0.9500 . ? C22 N21 1.328(3) . ? C22 N18 1.329(3) . ? C22 H22 0.9500 . ? Cd1 N10 2.3138(19) . ? Cd1 N10 2.3138(19) 2_756 ? Cd1 N21 2.3876(19) 1_645 ? Cd1 N21 2.3876(19) 2_666 ? Cd1 Cl1 2.6162(5) 2_756 ? N7 N8 1.365(3) . ? N18 N19 1.368(3) . ? N21 Cd1 2.3876(19) 1_465 ? 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 C2 C1 C5 108.0(2) . . ? C2 C1 Fe1 70.06(13) . . ? C5 C1 Fe1 69.42(13) . . ? C2 C1 H1 126.0 . . ? C5 C1 H1 126.0 . . ? Fe1 C1 H1 126.1 . . ? C1 C2 C3 108.2(2) . . ? C1 C2 Fe1 69.36(13) . . ? C3 C2 Fe1 69.53(14) . . ? C1 C2 H2 125.9 . . ? C3 C2 H2 125.9 . . ? Fe1 C2 H2 126.8 . . ? C4 C3 C2 107.8(2) . . ? C4 C3 Fe1 69.47(14) . . ? C2 C3 Fe1 69.85(14) . . ? C4 C3 H3 126.1 . . ? C2 C3 H3 126.1 . . ? Fe1 C3 H3 126.1 . . ? C3 C4 C5 108.7(2) . . ? C3 C4 Fe1 70.06(14) . . ? C5 C4 Fe1 69.56(13) . . ? C3 C4 H4 125.7 . . ? C5 C4 H4 125.7 . . ? Fe1 C4 H4 126.3 . . ? C4 C5 C1 107.4(2) . . ? C4 C5 C6 124.6(2) . . ? C1 C5 C6 128.0(2) . . ? C4 C5 Fe1 69.60(13) . . ? C1 C5 Fe1 69.66(13) . . ? C6 C5 Fe1 126.16(16) . . ? N7 C6 C5 111.37(18) . . ? N7 C6 H6A 109.4 . . ? C5 C6 H6A 109.4 . . ? N7 C6 H6B 109.4 . . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? N8 C9 N10 114.2(2) . . ? N8 C9 H9 122.9 . . ? N10 C9 H9 122.9 . . ? N10 C11 N7 109.9(2) . . ? N10 C11 H11 125.0 . . ? N7 C11 H11 125.0 . . ? C16 C12 C13 107.9(2) . . ? C16 C12 Fe1 69.33(13) . . ? C13 C12 Fe1 69.80(14) . . ? C16 C12 H12 126.1 . . ? C13 C12 H12 126.1 . . ? Fe1 C12 H12 126.4 . . ? C14 C13 C12 108.0(2) . . ? C14 C13 Fe1 69.90(14) . . ? C12 C13 Fe1 69.30(13) . . ? C14 C13 H13 126.0 . . ? C12 C13 H13 126.0 . . ? Fe1 C13 H13 126.4 . . ? C13 C14 C15 108.2(2) . . ? C13 C14 Fe1 69.66(14) . . ? C15 C14 Fe1 69.59(13) . . ? C13 C14 H14 125.9 . . ? C15 C14 H14 125.9 . . ? Fe1 C14 H14 126.4 . . ? C14 C15 C16 108.1(2) . . ? C14 C15 Fe1 69.88(14) . . ? C16 C15 Fe1 69.10(13) . . ? C14 C15 H15 125.9 . . ? C16 C15 H15 125.9 . . ? Fe1 C15 H15 126.6 . . ? C12 C16 C15 107.7(2) . . ? C12 C16 C17 126.6(2) . . ? C15 C16 C17 125.6(2) . . ? C12 C16 Fe1 69.76(13) . . ? C15 C16 Fe1 69.97(13) . . ? C17 C16 Fe1 122.59(16) . . ? N18 C17 C16 114.25(19) . . ? N18 C17 H17A 108.7 . . ? C16 C17 H17A 108.7 . . ? N18 C17 H17B 108.7 . . ? C16 C17 H17B 108.7 . . ? H17A C17 H17B 107.6 . . ? N19 C20 N21 114.9(2) . . ? N19 C20 H20 122.5 . . ? N21 C20 H20 122.5 . . ? N21 C22 N18 109.9(2) . . ? N21 C22 H22 125.1 . . ? N18 C22 H22 125.1 . . ? C16 Fe1 C5 121.00(9) . . ? C16 Fe1 C4 106.15(9) . . ? C5 Fe1 C4 40.84(9) . . ? C16 Fe1 C12 40.90(9) . . ? C5 Fe1 C12 106.50(10) . . ? C4 Fe1 C12 122.33(10) . . ? C16 Fe1 C1 157.80(10) . . ? C5 Fe1 C1 40.92(9) . . ? C4 Fe1 C1 68.47(9) . . ? C12 Fe1 C1 122.42(10) . . ? C16 Fe1 C13 68.79(10) . . ? C5 Fe1 C13 123.30(10) . . ? C4 Fe1 C13 159.36(11) . . ? C12 Fe1 C13 40.90(10) . . ? C1 Fe1 C13 108.23(10) . . ? C16 Fe1 C15 40.93(9) . . ? C5 Fe1 C15 157.46(10) . . ? C4 Fe1 C15 121.83(10) . . ? C12 Fe1 C15 68.58(10) . . ? C1 Fe1 C15 160.21(10) . . ? C13 Fe1 C15 68.27(10) . . ? C16 Fe1 C3 122.26(10) . . ? C5 Fe1 C3 68.65(9) . . ? C4 Fe1 C3 40.46(9) . . ? C12 Fe1 C3 158.50(10) . . ? C1 Fe1 C3 68.50(10) . . ? C13 Fe1 C3 159.11(10) . . ? C15 Fe1 C3 107.42(10) . . ? C16 Fe1 C14 68.67(9) . . ? C5 Fe1 C14 160.08(11) . . ? C4 Fe1 C14 158.19(11) . . ? C12 Fe1 C14 68.49(10) . . ? C1 Fe1 C14 124.24(10) . . ? C13 Fe1 C14 40.45(11) . . ? C15 Fe1 C14 40.53(10) . . ? C3 Fe1 C14 123.09(11) . . ? C16 Fe1 C2 159.33(11) . . ? C5 Fe1 C2 68.52(9) . . ? C4 Fe1 C2 68.11(10) . . ? C12 Fe1 C2 158.99(10) . . ? C1 Fe1 C2 40.57(10) . . ? C13 Fe1 C2 123.53(10) . . ? C15 Fe1 C2 123.85(10) . . ? C3 Fe1 C2 40.62(10) . . ? C14 Fe1 C2 108.84(10) . . ? N10 Cd1 N10 180.0 . 2_756 ? N10 Cd1 N21 86.69(7) . 1_645 ? N10 Cd1 N21 93.31(7) 2_756 1_645 ? N10 Cd1 N21 93.31(7) . 2_666 ? N10 Cd1 N21 86.69(7) 2_756 2_666 ? N21 Cd1 N21 180.000(1) 1_645 2_666 ? N10 Cd1 Cl1 91.59(5) . 2_756 ? N10 Cd1 Cl1 88.41(5) 2_756 2_756 ? N21 Cd1 Cl1 93.92(5) 1_645 2_756 ? N21 Cd1 Cl1 86.08(5) 2_666 2_756 ? N10 Cd1 Cl1 88.41(5) . . ? N10 Cd1 Cl1 91.59(5) 2_756 . ? N21 Cd1 Cl1 86.08(5) 1_645 . ? N21 Cd1 Cl1 93.92(5) 2_666 . ? Cl1 Cd1 Cl1 180.0 2_756 . ? C11 N7 N8 110.03(18) . . ? C11 N7 C6 128.67(19) . . ? N8 N7 C6 121.30(18) . . ? C9 N8 N7 102.54(18) . . ? C11 N10 C9 103.31(19) . . ? C11 N10 Cd1 127.74(16) . . ? C9 N10 Cd1 128.28(15) . . ? C22 N18 N19 110.39(18) . . ? C22 N18 C17 127.0(2) . . ? N19 N18 C17 122.54(19) . . ? C20 N19 N18 101.85(18) . . ? C22 N21 C20 102.95(19) . . ? C22 N21 Cd1 120.56(15) . 1_465 ? C20 N21 Cd1 134.90(15) . 1_465 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.886 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.092 #===END data_bt700_compoun5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(Fec-CH2-triazole)ZnCl2)n' _chemical_melting_point ? _chemical_formula_moiety 'C16 H16 Cl2 Fe N6 Zn' _chemical_formula_sum 'C16 H16 Cl2 Fe N6 Zn' _chemical_formula_weight 484.47 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3608(4) _cell_length_b 11.1924(6) _cell_length_c 12.0129(6) _cell_angle_alpha 71.008(1) _cell_angle_beta 75.759(1) _cell_angle_gamma 84.464(1) _cell_volume 906.91(8) _cell_formula_units_Z 2 _cell_measurement_temperature 86(2) _cell_measurement_reflns_used 5299 _cell_measurement_theta_min 2.85 _cell_measurement_theta_max 30.00 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.774 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 2.430 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.392 _exptl_absorpt_correction_T_max 0.712 _exptl_absorpt_process_details 'SADABS; Bruker, 2001' _exptl_special_details ; ? ; _diffrn_ambient_temperature 86(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker/Siemens SMART APEX' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13387 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4180 _reflns_number_gt 3999 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART v. 5.626' _computing_cell_refinement 'Bruker SAINT+ v. 6.45' _computing_data_reduction 'Bruker SAINT+ v. 6.45' _computing_structure_solution 'XS, Bruker SHELXTL v. 6.12' _computing_structure_refinement 'XL, Bruker SHELXTL v. 6.12' _computing_molecular_graphics 'XP, Bruker SHELXTL v. 6.12' _computing_publication_material 'XCIF, Bruker SHELXTL v. 6.12' _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^)+(0.0278P)^2^+0.5217P] 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 4180 _refine_ls_number_parameters 238 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0221 _refine_ls_R_factor_gt 0.0211 _refine_ls_wR_factor_ref 0.0545 _refine_ls_wR_factor_gt 0.0539 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 C1 C 0.5199(2) -0.15866(14) 0.44726(14) 0.0150(3) Uani 1 1 d . . . H1 H 0.4279 -0.1884 0.4199 0.018 Uiso 1 1 calc R . . C2 C 0.5358(2) -0.19106(14) 0.56958(14) 0.0179(3) Uani 1 1 d . . . H2 H 0.4554 -0.2455 0.6382 0.021 Uiso 1 1 calc R . . C3 C 0.6937(2) -0.12723(15) 0.57067(14) 0.0177(3) Uani 1 1 d . . . H3 H 0.7378 -0.1325 0.6401 0.021 Uiso 1 1 calc R . . C4 C 0.7738(2) -0.05428(15) 0.44954(14) 0.0149(3) Uani 1 1 d . . . H4 H 0.8799 -0.0019 0.4241 0.018 Uiso 1 1 calc R . . C5 C 0.6667(2) -0.07368(14) 0.37318(13) 0.0125(3) Uani 1 1 d . . . C6 C 0.7176(2) -0.01970(14) 0.23774(13) 0.0134(3) Uani 1 1 d . . . H6A H 0.7907 0.0579 0.2149 0.016 Uiso 1 1 calc R . . H6B H 0.7990 -0.0814 0.2043 0.016 Uiso 1 1 calc R . . C9 C 0.3207(2) -0.01714(14) 0.12563(14) 0.0152(3) Uani 1 1 d . . . H9 H 0.2273 -0.0558 0.1073 0.018 Uiso 1 1 calc R . . C11 C 0.4757(2) 0.12332(14) 0.14287(13) 0.0122(3) Uani 1 1 d . . . H11 H 0.5193 0.2012 0.1412 0.015 Uiso 1 1 calc R . . C13 C 0.3049(2) 0.51352(14) -0.05896(13) 0.0127(3) Uani 1 1 d . . . H13 H 0.2074 0.5511 -0.0124 0.015 Uiso 1 1 calc R . . C16 C 0.4637(2) 0.37698(14) -0.13248(13) 0.0133(3) Uani 1 1 d . . . H16 H 0.5067 0.3014 -0.1511 0.016 Uiso 1 1 calc R . . C17 C 0.7384(2) 0.51553(14) -0.26266(13) 0.0144(3) Uani 1 1 d . . . H17A H 0.8363 0.4838 -0.2160 0.017 Uiso 1 1 calc R . . H17B H 0.7504 0.6084 -0.2982 0.017 Uiso 1 1 calc R . . C18 C 0.7703(2) 0.45822(14) -0.36201(13) 0.0121(3) Uani 1 1 d . . . C19 C 0.7151(2) 0.51244(14) -0.47436(14) 0.0138(3) Uani 1 1 d . . . H19 H 0.6420 0.5875 -0.4960 0.017 Uiso 1 1 calc R . . C20 C 0.7891(2) 0.43399(15) -0.54803(14) 0.0158(3) Uani 1 1 d . . . H20 H 0.7742 0.4478 -0.6276 0.019 Uiso 1 1 calc R . . C21 C 0.8896(2) 0.33113(14) -0.48172(14) 0.0162(3) Uani 1 1 d . . . H21 H 0.9537 0.2648 -0.5096 0.019 Uiso 1 1 calc R . . C22 C 0.8771(2) 0.34531(14) -0.36652(14) 0.0145(3) Uani 1 1 d . . . H22 H 0.9302 0.2897 -0.3037 0.017 Uiso 1 1 calc R . . Cl1 Cl -0.03074(5) 0.27828(3) 0.22593(3) 0.01528(8) Uani 1 1 d . . . Cl2 Cl -0.05183(5) 0.21100(4) -0.05162(3) 0.01636(8) Uani 1 1 d . . . Fe1 Fe 0.5000 0.0000 0.5000 0.01076(7) Uani 1 2 d S . . Fe2 Fe 1.0000 0.5000 -0.5000 0.00972(7) Uani 1 2 d S . . N7 N 0.55467(17) 0.01109(11) 0.18331(11) 0.0115(2) Uani 1 1 d . . . N8 N 0.45683(19) -0.08115(12) 0.17320(12) 0.0151(3) Uani 1 1 d . . . N10 N 0.32556(17) 0.11007(12) 0.10479(11) 0.0125(2) Uani 1 1 d . . . N12 N 0.30462(17) 0.39011(12) -0.05423(11) 0.0120(2) Uani 1 1 d . . . N14 N 0.45203(17) 0.57578(12) -0.13376(11) 0.0129(2) Uani 1 1 d . . . N15 N 0.55196(17) 0.48628(12) -0.17994(11) 0.0119(2) Uani 1 1 d . . . Zn1 Zn 0.13343(2) 0.247550(15) 0.055439(14) 0.01048(5) 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 C1 0.0159(7) 0.0112(7) 0.0159(7) -0.0040(6) -0.0010(6) 0.0008(5) C2 0.0219(8) 0.0121(7) 0.0149(7) -0.0014(6) -0.0009(6) 0.0041(6) C3 0.0182(7) 0.0203(8) 0.0141(7) -0.0061(6) -0.0054(6) 0.0096(6) C4 0.0113(7) 0.0183(7) 0.0152(7) -0.0062(6) -0.0036(6) 0.0040(6) C5 0.0116(7) 0.0118(6) 0.0132(7) -0.0041(5) -0.0020(5) 0.0027(5) C6 0.0106(7) 0.0162(7) 0.0123(7) -0.0040(6) -0.0017(5) 0.0008(5) C9 0.0172(7) 0.0136(7) 0.0163(7) -0.0060(6) -0.0040(6) -0.0027(6) C11 0.0138(7) 0.0117(6) 0.0096(6) -0.0031(5) -0.0002(5) -0.0010(5) C13 0.0127(7) 0.0131(7) 0.0121(7) -0.0044(5) -0.0027(5) 0.0013(5) C16 0.0138(7) 0.0123(7) 0.0133(7) -0.0050(5) -0.0001(5) -0.0023(5) C17 0.0123(7) 0.0163(7) 0.0138(7) -0.0051(6) 0.0015(6) -0.0055(5) C18 0.0090(6) 0.0135(7) 0.0121(7) -0.0036(5) 0.0016(5) -0.0039(5) C19 0.0088(6) 0.0163(7) 0.0159(7) -0.0050(6) -0.0015(5) -0.0013(5) C20 0.0120(7) 0.0217(8) 0.0157(7) -0.0088(6) -0.0010(6) -0.0046(6) C21 0.0127(7) 0.0139(7) 0.0218(8) -0.0089(6) 0.0024(6) -0.0042(6) C22 0.0137(7) 0.0110(7) 0.0154(7) -0.0016(5) 0.0003(5) -0.0028(5) Cl1 0.01379(17) 0.02034(18) 0.01283(17) -0.00797(14) -0.00112(13) -0.00073(13) Cl2 0.01698(17) 0.01948(18) 0.01521(17) -0.00679(14) -0.00523(13) -0.00369(14) Fe1 0.01041(14) 0.01036(14) 0.01021(14) -0.00224(11) -0.00201(11) 0.00169(10) Fe2 0.00814(13) 0.01040(14) 0.00992(14) -0.00321(11) -0.00036(10) -0.00112(10) N7 0.0121(6) 0.0114(6) 0.0111(6) -0.0041(5) -0.0016(5) -0.0013(4) N8 0.0181(6) 0.0123(6) 0.0168(6) -0.0059(5) -0.0045(5) -0.0023(5) N10 0.0132(6) 0.0126(6) 0.0113(6) -0.0037(5) -0.0021(5) -0.0005(5) N12 0.0119(6) 0.0123(6) 0.0112(6) -0.0035(5) -0.0016(5) -0.0007(5) N14 0.0133(6) 0.0123(6) 0.0131(6) -0.0055(5) -0.0018(5) 0.0014(5) N15 0.0127(6) 0.0124(6) 0.0107(6) -0.0052(5) -0.0003(5) -0.0007(5) Zn1 0.00989(9) 0.01130(9) 0.00967(9) -0.00273(6) -0.00134(6) -0.00162(6) _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 C1 C2 1.426(2) . ? C1 C5 1.428(2) . ? C1 Fe1 2.0525(15) . ? C1 H1 0.9500 . ? C2 C3 1.427(2) . ? C2 Fe1 2.0438(15) . ? C2 H2 0.9500 . ? C3 C4 1.424(2) . ? C3 Fe1 2.0490(15) . ? C3 H3 0.9500 . ? C4 C5 1.424(2) . ? C4 Fe1 2.0493(15) . ? C4 H4 0.9500 . ? C5 C6 1.502(2) . ? C5 Fe1 2.0517(14) . ? C6 N7 1.4644(18) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C9 N8 1.311(2) . ? C9 N10 1.3654(19) . ? C9 H9 0.9500 . ? C11 N7 1.3237(19) . ? C11 N10 1.3334(19) . ? C11 H11 0.9500 . ? C13 N14 1.3136(19) . ? C13 N12 1.3640(19) . ? C13 H13 0.9500 . ? C16 N15 1.3268(19) . ? C16 N12 1.3387(19) . ? C16 H16 0.9500 . ? C17 N15 1.4771(18) . ? C17 C18 1.491(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.430(2) . ? C18 C22 1.432(2) . ? C18 Fe2 2.0237(14) . ? C19 C20 1.424(2) . ? C19 Fe2 2.0411(14) . ? C19 H19 0.9500 . ? C20 C21 1.427(2) . ? C20 Fe2 2.0560(15) . ? C20 H20 0.9500 . ? C21 C22 1.423(2) . ? C21 Fe2 2.0540(15) . ? C21 H21 0.9500 . ? C22 Fe2 2.0417(15) . ? C22 H22 0.9500 . ? Cl1 Zn1 2.2212(4) . ? Cl2 Zn1 2.2347(4) . ? Fe1 C2 2.0437(15) 2_656 ? Fe1 C3 2.0490(15) 2_656 ? Fe1 C4 2.0493(15) 2_656 ? Fe1 C5 2.0517(14) 2_656 ? Fe1 C1 2.0525(15) 2_656 ? Fe2 C18 2.0237(14) 2_764 ? Fe2 C19 2.0411(14) 2_764 ? Fe2 C22 2.0417(15) 2_764 ? Fe2 C21 2.0540(15) 2_764 ? Fe2 C20 2.0560(15) 2_764 ? N7 N8 1.3665(17) . ? N10 Zn1 2.0293(13) . ? N12 Zn1 2.0180(12) . ? N14 N15 1.3679(17) . ? 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 C2 C1 C5 107.98(14) . . ? C2 C1 Fe1 69.30(9) . . ? C5 C1 Fe1 69.62(8) . . ? C2 C1 H1 126.0 . . ? C5 C1 H1 126.0 . . ? Fe1 C1 H1 126.6 . . ? C1 C2 C3 107.86(14) . . ? C1 C2 Fe1 69.95(9) . . ? C3 C2 Fe1 69.79(9) . . ? C1 C2 H2 126.1 . . ? C3 C2 H2 126.1 . . ? Fe1 C2 H2 125.8 . . ? C4 C3 C2 108.13(14) . . ? C4 C3 Fe1 69.67(8) . . ? C2 C3 Fe1 69.40(9) . . ? C4 C3 H3 125.9 . . ? C2 C3 H3 125.9 . . ? Fe1 C3 H3 126.6 . . ? C3 C4 C5 108.01(14) . . ? C3 C4 Fe1 69.65(9) . . ? C5 C4 Fe1 69.78(8) . . ? C3 C4 H4 126.0 . . ? C5 C4 H4 126.0 . . ? Fe1 C4 H4 126.1 . . ? C4 C5 C1 108.02(13) . . ? C4 C5 C6 123.40(13) . . ? C1 C5 C6 128.38(13) . . ? C4 C5 Fe1 69.59(8) . . ? C1 C5 Fe1 69.67(8) . . ? C6 C5 Fe1 130.16(10) . . ? N7 C6 C5 113.41(12) . . ? N7 C6 H6A 108.9 . . ? C5 C6 H6A 108.9 . . ? N7 C6 H6B 108.9 . . ? C5 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? N8 C9 N10 113.91(13) . . ? N8 C9 H9 123.0 . . ? N10 C9 H9 123.0 . . ? N7 C11 N10 109.41(13) . . ? N7 C11 H11 125.3 . . ? N10 C11 H11 125.3 . . ? N14 C13 N12 113.96(13) . . ? N14 C13 H13 123.0 . . ? N12 C13 H13 123.0 . . ? N15 C16 N12 109.20(13) . . ? N15 C16 H16 125.4 . . ? N12 C16 H16 125.4 . . ? N15 C17 C18 112.44(12) . . ? N15 C17 H17A 109.1 . . ? C18 C17 H17A 109.1 . . ? N15 C17 H17B 109.1 . . ? C18 C17 H17B 109.1 . . ? H17A C17 H17B 107.8 . . ? C19 C18 C22 107.89(13) . . ? C19 C18 C17 126.00(14) . . ? C22 C18 C17 125.86(14) . . ? C19 C18 Fe2 70.06(8) . . ? C22 C18 Fe2 70.06(8) . . ? C17 C18 Fe2 120.99(10) . . ? C20 C19 C18 107.88(13) . . ? C20 C19 Fe2 70.23(8) . . ? C18 C19 Fe2 68.76(8) . . ? C20 C19 H19 126.1 . . ? C18 C19 H19 126.1 . . ? Fe2 C19 H19 126.5 . . ? C19 C20 C21 108.24(13) . . ? C19 C20 Fe2 69.10(8) . . ? C21 C20 Fe2 69.61(9) . . ? C19 C20 H20 125.9 . . ? C21 C20 H20 125.9 . . ? Fe2 C20 H20 127.0 . . ? C22 C21 C20 108.05(13) . . ? C22 C21 Fe2 69.20(8) . . ? C20 C21 Fe2 69.76(8) . . ? C22 C21 H21 126.0 . . ? C20 C21 H21 126.0 . . ? Fe2 C21 H21 126.6 . . ? C21 C22 C18 107.94(13) . . ? C21 C22 Fe2 70.13(9) . . ? C18 C22 Fe2 68.70(8) . . ? C21 C22 H22 126.0 . . ? C18 C22 H22 126.0 . . ? Fe2 C22 H22 126.7 . . ? C2 Fe1 C2 180.00(10) 2_656 . ? C2 Fe1 C3 40.81(7) 2_656 2_656 ? C2 Fe1 C3 139.19(7) . 2_656 ? C2 Fe1 C3 139.19(7) 2_656 . ? C2 Fe1 C3 40.81(7) . . ? C3 Fe1 C3 180.00(9) 2_656 . ? C2 Fe1 C4 111.33(6) 2_656 . ? C2 Fe1 C4 68.67(6) . . ? C3 Fe1 C4 139.32(6) 2_656 . ? C3 Fe1 C4 40.68(6) . . ? C2 Fe1 C4 68.67(6) 2_656 2_656 ? C2 Fe1 C4 111.33(6) . 2_656 ? C3 Fe1 C4 40.68(6) 2_656 2_656 ? C3 Fe1 C4 139.32(6) . 2_656 ? C4 Fe1 C4 180.00(9) . 2_656 ? C2 Fe1 C5 111.38(6) 2_656 . ? C2 Fe1 C5 68.62(6) . . ? C3 Fe1 C5 111.62(6) 2_656 . ? C3 Fe1 C5 68.38(6) . . ? C4 Fe1 C5 40.63(6) . . ? C4 Fe1 C5 139.37(6) 2_656 . ? C2 Fe1 C5 68.62(6) 2_656 2_656 ? C2 Fe1 C5 111.38(6) . 2_656 ? C3 Fe1 C5 68.38(6) 2_656 2_656 ? C3 Fe1 C5 111.62(6) . 2_656 ? C4 Fe1 C5 139.37(6) . 2_656 ? C4 Fe1 C5 40.63(6) 2_656 2_656 ? C5 Fe1 C5 180.00(6) . 2_656 ? C2 Fe1 C1 40.75(6) 2_656 2_656 ? C2 Fe1 C1 139.25(6) . 2_656 ? C3 Fe1 C1 68.42(6) 2_656 2_656 ? C3 Fe1 C1 111.58(6) . 2_656 ? C4 Fe1 C1 111.54(6) . 2_656 ? C4 Fe1 C1 68.46(6) 2_656 2_656 ? C5 Fe1 C1 139.29(6) . 2_656 ? C5 Fe1 C1 40.71(6) 2_656 2_656 ? C2 Fe1 C1 139.25(6) 2_656 . ? C2 Fe1 C1 40.75(6) . . ? C3 Fe1 C1 111.58(6) 2_656 . ? C3 Fe1 C1 68.42(6) . . ? C4 Fe1 C1 68.46(6) . . ? C4 Fe1 C1 111.54(6) 2_656 . ? C5 Fe1 C1 40.71(6) . . ? C5 Fe1 C1 139.29(6) 2_656 . ? C1 Fe1 C1 180.0 2_656 . ? C18 Fe2 C18 180.00(8) 2_764 . ? C18 Fe2 C19 41.18(6) 2_764 2_764 ? C18 Fe2 C19 138.82(6) . 2_764 ? C18 Fe2 C19 138.82(6) 2_764 . ? C18 Fe2 C19 41.18(6) . . ? C19 Fe2 C19 180.000(15) 2_764 . ? C18 Fe2 C22 41.24(6) 2_764 2_764 ? C18 Fe2 C22 138.76(6) . 2_764 ? C19 Fe2 C22 69.03(6) 2_764 2_764 ? C19 Fe2 C22 110.97(6) . 2_764 ? C18 Fe2 C22 138.76(6) 2_764 . ? C18 Fe2 C22 41.24(6) . . ? C19 Fe2 C22 110.97(6) 2_764 . ? C19 Fe2 C22 69.03(6) . . ? C22 Fe2 C22 180.00(9) 2_764 . ? C18 Fe2 C21 68.98(6) 2_764 2_764 ? C18 Fe2 C21 111.02(6) . 2_764 ? C19 Fe2 C21 68.67(6) 2_764 2_764 ? C19 Fe2 C21 111.33(6) . 2_764 ? C22 Fe2 C21 40.67(6) 2_764 2_764 ? C22 Fe2 C21 139.33(6) . 2_764 ? C18 Fe2 C21 111.02(6) 2_764 . ? C18 Fe2 C21 68.98(6) . . ? C19 Fe2 C21 111.33(6) 2_764 . ? C19 Fe2 C21 68.67(6) . . ? C22 Fe2 C21 139.33(6) 2_764 . ? C22 Fe2 C21 40.67(6) . . ? C21 Fe2 C21 180.0 2_764 . ? C18 Fe2 C20 68.86(6) 2_764 2_764 ? C18 Fe2 C20 111.14(6) . 2_764 ? C19 Fe2 C20 40.67(6) 2_764 2_764 ? C19 Fe2 C20 139.33(6) . 2_764 ? C22 Fe2 C20 68.51(6) 2_764 2_764 ? C22 Fe2 C20 111.49(6) . 2_764 ? C21 Fe2 C20 40.63(6) 2_764 2_764 ? C21 Fe2 C20 139.37(6) . 2_764 ? C18 Fe2 C20 111.14(6) 2_764 . ? C18 Fe2 C20 68.86(6) . . ? C19 Fe2 C20 139.33(6) 2_764 . ? C19 Fe2 C20 40.67(6) . . ? C22 Fe2 C20 111.49(6) 2_764 . ? C22 Fe2 C20 68.51(6) . . ? C21 Fe2 C20 139.37(6) 2_764 . ? C21 Fe2 C20 40.63(6) . . ? C20 Fe2 C20 180.000(1) 2_764 . ? C11 N7 N8 110.44(12) . . ? C11 N7 C6 128.17(13) . . ? N8 N7 C6 121.34(12) . . ? C9 N8 N7 102.77(12) . . ? C11 N10 C9 103.47(12) . . ? C11 N10 Zn1 125.79(10) . . ? C9 N10 Zn1 130.02(10) . . ? C16 N12 C13 103.56(12) . . ? C16 N12 Zn1 124.91(10) . . ? C13 N12 Zn1 131.10(10) . . ? C13 N14 N15 102.82(12) . . ? C16 N15 N14 110.46(12) . . ? C16 N15 C17 128.99(13) . . ? N14 N15 C17 120.35(12) . . ? N12 Zn1 N10 100.28(5) . . ? N12 Zn1 Cl1 114.71(4) . . ? N10 Zn1 Cl1 105.71(4) . . ? N12 Zn1 Cl2 107.89(4) . . ? N10 Zn1 Cl2 116.11(4) . . ? Cl1 Zn1 Cl2 111.831(15) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.386 _refine_diff_density_min -0.264 _refine_diff_density_rms 0.064 #===END data_bt709_compound6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Fec-CH2-Me-imidazole-ZnCl2)n _chemical_melting_point ? _chemical_formula_moiety 'C20 H22 Cl2 Fe N4 Zn' _chemical_formula_sum 'C20 H22 Cl2 Fe N4 Zn' _chemical_formula_weight 510.54 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.902(1) _cell_length_b 11.6328(8) _cell_length_c 13.340(1) _cell_angle_alpha 90.00 _cell_angle_beta 117.339(1) _cell_angle_gamma 90.00 _cell_volume 2054.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 86(2) _cell_measurement_reflns_used 5112 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 27.52 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.651 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 2.147 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6612 _exptl_absorpt_correction_T_max 0.9583 _exptl_absorpt_process_details 'SADABS; Bruker, 2001' _exptl_special_details ; ? ; _diffrn_ambient_temperature 86(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker/Siemens SMART APEX' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13577 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 27.53 _reflns_number_total 2368 _reflns_number_gt 1936 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART v. 5.626' _computing_cell_refinement 'Bruker SAINT+ v. 6.45' _computing_data_reduction 'Bruker SAINT+ v. 6.45' _computing_structure_solution 'XS, Bruker SHELXTL v. 6.12' _computing_structure_refinement 'XL, Bruker SHELXTL v. 6.12' _computing_molecular_graphics 'XP, Bruker SHELXTL v. 6.12' _computing_publication_material 'XCIF, Bruker SHELXTL v. 6.12' _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^+1.1296P] 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 2368 _refine_ls_number_parameters 130 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0828 _refine_ls_wR_factor_gt 0.0780 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _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 C1 C 0.8758(2) 0.6556(2) 0.0307(2) 0.0183(6) Uani 1 1 d . . . H1 H 0.8997 0.6369 -0.0221 0.022 Uiso 1 1 calc R . . C2 C 0.9032(2) 0.7541(2) 0.1022(2) 0.0206(6) Uani 1 1 d . . . H2 H 0.9483 0.8130 0.1047 0.025 Uiso 1 1 calc R . . C3 C 0.8518(2) 0.7491(2) 0.1687(2) 0.0192(6) Uani 1 1 d . . . H3 H 0.8564 0.8041 0.2236 0.023 Uiso 1 1 calc R . . C4 C 0.7922(2) 0.6479(2) 0.1393(2) 0.0181(6) Uani 1 1 d . . . H4 H 0.7503 0.6229 0.1715 0.022 Uiso 1 1 calc R . . C5 C 0.80584(19) 0.5901(2) 0.0531(2) 0.0152(5) Uani 1 1 d . . . C6 C 0.7525(2) 0.4823(2) -0.0061(2) 0.0192(6) Uani 1 1 d . . . H6A H 0.6959 0.4673 0.0116 0.023 Uiso 1 1 calc R . . H6B H 0.7236 0.4938 -0.0886 0.023 Uiso 1 1 calc R . . C8 C 0.85766(19) 0.3241(2) 0.1257(2) 0.0154(6) Uani 1 1 d . . . C10 C 0.9136(2) 0.2407(2) 0.0193(2) 0.0181(6) Uani 1 1 d . . . H10 H 0.9484 0.1889 -0.0058 0.022 Uiso 1 1 calc R . . C11 C 0.8551(2) 0.3291(2) -0.0411(2) 0.0200(6) Uani 1 1 d . . . H11 H 0.8412 0.3510 -0.1154 0.024 Uiso 1 1 calc R . . C12 C 0.8405(2) 0.3561(2) 0.2228(2) 0.0209(6) Uani 1 1 d . . . H12A H 0.8539 0.2896 0.2728 0.031 Uiso 1 1 calc R . . H12B H 0.7702 0.3807 0.1955 0.031 Uiso 1 1 calc R . . H12C H 0.8859 0.4192 0.2645 0.031 Uiso 1 1 calc R . . Cl1 Cl 1.08622(5) 0.02576(6) 0.18031(6) 0.01920(16) Uani 1 1 d . . . Fe1 Fe 0.7500 0.7500 0.0000 0.01285(14) Uani 1 2 d S . . N7 N 0.81963(16) 0.38135(18) 0.02659(19) 0.0164(5) Uani 1 1 d . . . N9 N 0.91478(16) 0.23737(18) 0.12317(19) 0.0148(5) Uani 1 1 d . . . Zn1 Zn 1.0000 0.12882(3) 0.2500 0.01327(13) Uani 1 2 d S . . 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 0.0134(13) 0.0183(14) 0.0224(15) 0.0012(11) 0.0076(12) 0.0018(10) C2 0.0123(13) 0.0156(13) 0.0253(16) 0.0031(11) 0.0011(12) -0.0006(10) C3 0.0185(14) 0.0149(13) 0.0151(14) 0.0001(10) -0.0001(11) 0.0023(10) C4 0.0186(13) 0.0155(13) 0.0162(14) 0.0042(11) 0.0045(11) 0.0023(10) C5 0.0140(12) 0.0113(12) 0.0144(13) 0.0027(10) 0.0015(11) 0.0032(10) C6 0.0202(14) 0.0111(13) 0.0183(14) 0.0030(10) 0.0019(12) 0.0021(10) C8 0.0139(12) 0.0123(12) 0.0158(14) 0.0010(10) 0.0030(11) -0.0004(10) C10 0.0176(13) 0.0159(13) 0.0205(15) -0.0019(11) 0.0086(12) -0.0016(10) C11 0.0232(14) 0.0188(14) 0.0150(14) -0.0010(11) 0.0062(12) -0.0036(11) C12 0.0219(14) 0.0186(14) 0.0209(15) 0.0023(11) 0.0089(12) 0.0040(11) Cl1 0.0200(3) 0.0158(3) 0.0228(4) 0.0006(3) 0.0106(3) 0.0032(2) Fe1 0.0110(3) 0.0093(3) 0.0144(3) 0.0010(2) 0.0025(2) -0.00039(19) N7 0.0183(11) 0.0112(11) 0.0150(12) -0.0002(8) 0.0036(10) -0.0002(8) N9 0.0131(11) 0.0127(11) 0.0155(12) -0.0001(9) 0.0040(9) 0.0003(8) Zn1 0.0116(2) 0.0093(2) 0.0153(2) 0.000 0.00307(17) 0.000 _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 C1 C2 1.424(4) . ? C1 C5 1.429(4) . ? C1 Fe1 2.045(3) . ? C1 H1 0.9500 . ? C2 C3 1.416(4) . ? C2 Fe1 2.053(3) . ? C2 H2 0.9500 . ? C3 C4 1.417(4) . ? C3 Fe1 2.057(3) . ? C3 H3 0.9500 . ? C4 C5 1.426(4) . ? C4 Fe1 2.046(3) . ? C4 H4 0.9500 . ? C5 C6 1.501(4) . ? C5 Fe1 2.028(3) . ? C6 N7 1.473(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C8 N9 1.330(3) . ? C8 N7 1.352(3) . ? C8 C12 1.478(4) . ? C10 C11 1.350(4) . ? C10 N9 1.378(4) . ? C10 H10 0.9500 . ? C11 N7 1.379(4) . ? C11 H11 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? Cl1 Zn1 2.2471(7) . ? Fe1 C5 2.028(3) 7_665 ? Fe1 C1 2.045(3) 7_665 ? Fe1 C4 2.046(3) 7_665 ? Fe1 C2 2.053(3) 7_665 ? Fe1 C3 2.057(3) 7_665 ? N9 Zn1 2.024(2) . ? Zn1 N9 2.024(2) 2_755 ? Zn1 Cl1 2.2471(7) 2_755 ? 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 C2 C1 C5 107.6(3) . . ? C2 C1 Fe1 69.96(15) . . ? C5 C1 Fe1 68.80(15) . . ? C2 C1 H1 126.2 . . ? C5 C1 H1 126.2 . . ? Fe1 C1 H1 126.6 . . ? C3 C2 C1 108.4(2) . . ? C3 C2 Fe1 70.00(15) . . ? C1 C2 Fe1 69.37(15) . . ? C3 C2 H2 125.8 . . ? C1 C2 H2 125.8 . . ? Fe1 C2 H2 126.4 . . ? C2 C3 C4 108.1(2) . . ? C2 C3 Fe1 69.70(16) . . ? C4 C3 Fe1 69.37(15) . . ? C2 C3 H3 125.9 . . ? C4 C3 H3 125.9 . . ? Fe1 C3 H3 126.6 . . ? C3 C4 C5 108.2(3) . . ? C3 C4 Fe1 70.21(16) . . ? C5 C4 Fe1 68.83(15) . . ? C3 C4 H4 125.9 . . ? C5 C4 H4 125.9 . . ? Fe1 C4 H4 126.6 . . ? C4 C5 C1 107.8(2) . . ? C4 C5 C6 125.5(3) . . ? C1 C5 C6 126.7(3) . . ? C4 C5 Fe1 70.21(15) . . ? C1 C5 Fe1 70.12(15) . . ? C6 C5 Fe1 123.35(18) . . ? N7 C6 C5 112.7(2) . . ? N7 C6 H6A 109.0 . . ? C5 C6 H6A 109.0 . . ? N7 C6 H6B 109.0 . . ? C5 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? N9 C8 N7 109.5(2) . . ? N9 C8 C12 125.7(2) . . ? N7 C8 C12 124.7(2) . . ? C11 C10 N9 109.2(2) . . ? C11 C10 H10 125.4 . . ? N9 C10 H10 125.4 . . ? C10 C11 N7 106.3(3) . . ? C10 C11 H11 126.8 . . ? N7 C11 H11 126.8 . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C5 Fe1 C5 180.0 7_665 . ? C5 Fe1 C1 41.08(11) 7_665 7_665 ? C5 Fe1 C1 138.92(11) . 7_665 ? C5 Fe1 C1 138.92(11) 7_665 . ? C5 Fe1 C1 41.08(11) . . ? C1 Fe1 C1 180.0 7_665 . ? C5 Fe1 C4 139.03(11) 7_665 . ? C5 Fe1 C4 40.97(11) . . ? C1 Fe1 C4 111.38(11) 7_665 . ? C1 Fe1 C4 68.62(11) . . ? C5 Fe1 C4 40.97(11) 7_665 7_665 ? C5 Fe1 C4 139.03(11) . 7_665 ? C1 Fe1 C4 68.62(11) 7_665 7_665 ? C1 Fe1 C4 111.38(11) . 7_665 ? C4 Fe1 C4 180.00(12) . 7_665 ? C5 Fe1 C2 68.68(10) 7_665 7_665 ? C5 Fe1 C2 111.32(10) . 7_665 ? C1 Fe1 C2 40.67(11) 7_665 7_665 ? C1 Fe1 C2 139.33(11) . 7_665 ? C4 Fe1 C2 111.94(11) . 7_665 ? C4 Fe1 C2 68.06(11) 7_665 7_665 ? C5 Fe1 C2 111.32(10) 7_665 . ? C5 Fe1 C2 68.68(10) . . ? C1 Fe1 C2 139.33(11) 7_665 . ? C1 Fe1 C2 40.67(11) . . ? C4 Fe1 C2 68.06(11) . . ? C4 Fe1 C2 111.94(11) 7_665 . ? C2 Fe1 C2 180.00(15) 7_665 . ? C5 Fe1 C3 111.39(10) 7_665 . ? C5 Fe1 C3 68.61(10) . . ? C1 Fe1 C3 111.68(11) 7_665 . ? C1 Fe1 C3 68.32(11) . . ? C4 Fe1 C3 40.42(10) . . ? C4 Fe1 C3 139.58(10) 7_665 . ? C2 Fe1 C3 139.70(12) 7_665 . ? C2 Fe1 C3 40.30(12) . . ? C5 Fe1 C3 68.61(10) 7_665 7_665 ? C5 Fe1 C3 111.39(10) . 7_665 ? C1 Fe1 C3 68.32(11) 7_665 7_665 ? C1 Fe1 C3 111.68(11) . 7_665 ? C4 Fe1 C3 139.58(10) . 7_665 ? C4 Fe1 C3 40.42(10) 7_665 7_665 ? C2 Fe1 C3 40.30(12) 7_665 7_665 ? C2 Fe1 C3 139.70(12) . 7_665 ? C3 Fe1 C3 180.0 . 7_665 ? C8 N7 C11 108.0(2) . . ? C8 N7 C6 127.2(2) . . ? C11 N7 C6 124.8(2) . . ? C8 N9 C10 107.0(2) . . ? C8 N9 Zn1 127.93(19) . . ? C10 N9 Zn1 124.83(18) . . ? N9 Zn1 N9 102.80(12) 2_755 . ? N9 Zn1 Cl1 104.21(7) 2_755 2_755 ? N9 Zn1 Cl1 114.85(6) . 2_755 ? N9 Zn1 Cl1 114.85(6) 2_755 . ? N9 Zn1 Cl1 104.21(7) . . ? Cl1 Zn1 Cl1 115.51(4) 2_755 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.843 _refine_diff_density_min -0.543 _refine_diff_density_rms 0.101