Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemsitry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Guo Dong' ; Coordination Chemistry Institute and State Key Laboratory of Coordination Chemistry, Nanjing University,Nanjing,210093, People's Republic of China ; 'Mo Hong' ; Coordination Chemistry Institute and State Key Laboratory of Coordination Chemistry, Nanjing University,Nanjing,210093, People's Republic of China ; 'Duan Chun-ying' ; Coordination Chemistry Institute and State Key Laboratory of Coordination Chemistry, Nanjing University,Nanjing,210093, People's Republic of China ; 'Lu Feng' ; Coordination Chemistry Institute and State Key Laboratory of Coordination Chemistry, Nanjing University,Nanjing,210093, People's Republic of China ; _publ_contact_author_name 'Dr. Duan Chun-ying' _publ_contact_author_address ; Coordination Chemistry Institute The State Key Laboratory of Coordinaiton Chemistry Nanjing University , Nanjing 210093 P. R. China ; _publ_contact_author_email duancy@nju.edu.cn _publ_contact_author_fax '00 86 25 331 7761' _publ_contact_author_phone '00 86 25 359 7006' _publ_requested_journal 'Dalton Trans.' _publ_requested_category 'No. B201604B' #======================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Novel ferrocene-based mixed-metal coordination polymers ; data_NaZn3L2(OH)3(H2O) _database_code_CSD 179761 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C12H8O4Fe)2NaZn3(OH)3(H2O)' _chemical_formula_sum 'C24 H21 Fe2 Na O12 Zn3' _chemical_formula_weight 832.21 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 '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/m ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 28.719(8) _cell_length_b 3.3292(9) _cell_length_c 6.2718(17) _cell_angle_alpha 90.00 _cell_angle_beta 97.517(4) _cell_angle_gamma 90.00 _cell_volume 594.5(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 571 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 24.76 _exptl_crystal_description block _exptl_crystal_colour darkness _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 414 _exptl_absorpt_coefficient_mu 4.265 _exptl_absorpt_correction_type empricial _exptl_absorpt_correction_T_min 0.4874 _exptl_absorpt_correction_T_max 0.6683 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 1867 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0704 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 27.95 _reflns_number_total 801 _reflns_number_gt 600 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.1213P)^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_number_reflns 801 _refine_ls_number_parameters 69 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1907 _refine_ls_wR_factor_gt 0.1812 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 Zn1 Zn 0.5000 0.5000 0.5000 0.0364(6) Uani 1 4 d S . . Zn2 Zn 0.5000 1.0000 1.0000 0.0164(5) Uani 0.50 4 d SP . . Na1 Na 0.5000 1.0000 1.0000 0.0164(5) Uani 0.50 4 d SP . . Fe1 Fe 0.32985(7) 1.0000 0.8151(4) 0.0194(6) Uani 0.50 2 d SP . . C6 C 0.3537(3) 0.5000 0.9878(14) 0.0255(17) Uani 1 2 d S . . H6A H 0.3734 0.5000 1.1238 0.031 Uiso 1 2 d SR . . C2 C 0.3693(3) 0.5000 0.7808(13) 0.0238(17) Uani 1 2 d S . . O2 O 0.44991(19) 0.5000 0.9151(10) 0.0361(15) Uani 1 2 d S . . O1 O 0.42867(18) 0.5000 0.5573(10) 0.0308(14) Uani 1 2 d S . . C1 C 0.4196(3) 0.5000 0.7436(13) 0.0242(17) Uani 1 2 d S . . C4 C 0.2893(3) 0.5000 0.7351(15) 0.0298(19) Uani 1 2 d S . . H4A H 0.2573 0.5000 0.6684 0.036 Uiso 1 2 d SR . . C5 C 0.3043(3) 0.5000 0.9554(15) 0.0284(19) Uani 1 2 d S . . H5A H 0.2842 0.5000 1.0662 0.034 Uiso 1 2 d SR . . C3 C 0.3294(3) 0.5000 0.6236(14) 0.0278(18) Uani 1 2 d S . . H3A H 0.3294 0.5000 0.4706 0.033 Uiso 1 2 d SR . . O1W O 0.52045(18) 1.0000 0.7152(8) 0.0280(14) 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 Zn1 0.0274(9) 0.0585(11) 0.0243(8) 0.000 0.0068(6) 0.000 Zn2 0.0133(9) 0.0284(11) 0.0077(9) 0.000 0.0015(6) 0.000 Na1 0.0133(9) 0.0284(11) 0.0077(9) 0.000 0.0015(6) 0.000 Fe1 0.0121(10) 0.0183(11) 0.0281(12) 0.000 0.0044(9) 0.000 C6 0.019(4) 0.025(4) 0.032(4) 0.000 0.003(3) 0.000 C2 0.022(4) 0.019(4) 0.030(4) 0.000 0.004(3) 0.000 O2 0.016(3) 0.054(4) 0.038(4) 0.000 0.004(3) 0.000 O1 0.015(3) 0.040(4) 0.038(3) 0.000 0.008(2) 0.000 C1 0.022(4) 0.021(4) 0.031(4) 0.000 0.007(3) 0.000 C4 0.018(4) 0.025(4) 0.046(5) 0.000 0.003(4) 0.000 C5 0.021(4) 0.025(4) 0.041(5) 0.000 0.012(4) 0.000 C3 0.020(4) 0.027(4) 0.036(5) 0.000 0.006(3) 0.000 O1W 0.018(3) 0.051(4) 0.015(3) 0.000 0.002(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 Zn1 O1 2.126(5) 5_666 ? Zn1 O1 2.126(5) . ? Zn1 O1W 2.175(3) . ? Zn1 O1W 2.175(3) 5_666 ? Zn1 O1W 2.175(3) 1_545 ? Zn1 O1W 2.175(3) 5_676 ? Zn1 Na1 3.5503(8) 1_544 ? Zn1 Na1 3.5503(8) 1_545 ? Zn1 Na1 3.5503(8) 1_554 ? Zn2 O1W 1.952(5) . ? Zn2 O1W 1.952(5) 5_677 ? Zn2 O2 2.219(4) 5_677 ? Zn2 O2 2.219(4) . ? Zn2 O2 2.219(4) 5_667 ? Zn2 O2 2.219(4) 1_565 ? Zn2 Na1 3.3292(9) 1_565 ? Zn2 Na1 3.3292(9) 1_545 ? Fe1 C2 2.041(5) 1_565 ? Fe1 C2 2.041(5) . ? Fe1 C3 2.052(5) . ? Fe1 C3 2.052(5) 1_565 ? Fe1 C6 2.054(5) 1_565 ? Fe1 C6 2.054(5) . ? Fe1 C4 2.055(5) . ? Fe1 C4 2.055(5) 1_565 ? Fe1 C5 2.062(5) . ? Fe1 C5 2.062(5) 1_565 ? C6 C5 1.407(10) . ? C6 C2 1.428(12) . ? C6 Fe1 2.054(5) 1_545 ? C2 C3 1.412(11) . ? C2 C1 1.492(10) . ? C2 Fe1 2.041(5) 1_545 ? O2 C1 1.292(10) . ? O2 Na1 2.219(4) 1_545 ? O2 Zn2 2.219(4) 1_545 ? O1 C1 1.230(10) . ? C1 Na1 3.117(7) 1_545 ? C4 C5 1.393(13) . ? C4 C3 1.422(11) . ? C4 Fe1 2.055(5) 1_545 ? C5 Fe1 2.062(5) 1_545 ? C3 Fe1 2.052(5) 1_545 ? O1W Zn1 2.175(3) 1_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O1 180.00(5) 5_666 . ? O1 Zn1 O1W 85.23(17) 5_666 . ? O1 Zn1 O1W 94.77(17) . . ? O1 Zn1 O1W 94.77(17) 5_666 5_666 ? O1 Zn1 O1W 85.23(17) . 5_666 ? O1W Zn1 O1W 180.0(3) . 5_666 ? O1 Zn1 O1W 85.23(17) 5_666 1_545 ? O1 Zn1 O1W 94.77(17) . 1_545 ? O1W Zn1 O1W 99.9(2) . 1_545 ? O1W Zn1 O1W 80.1(2) 5_666 1_545 ? O1 Zn1 O1W 94.77(17) 5_666 5_676 ? O1 Zn1 O1W 85.23(17) . 5_676 ? O1W Zn1 O1W 80.1(2) . 5_676 ? O1W Zn1 O1W 99.9(2) 5_666 5_676 ? O1W Zn1 O1W 180.0(3) 1_545 5_676 ? O1 Zn1 Na1 74.90(14) 5_666 1_544 ? O1 Zn1 Na1 105.10(15) . 1_544 ? O1W Zn1 Na1 151.13(12) . 1_544 ? O1W Zn1 Na1 28.87(12) 5_666 1_544 ? O1W Zn1 Na1 99.09(11) 1_545 1_544 ? O1W Zn1 Na1 80.91(11) 5_676 1_544 ? O1 Zn1 Na1 105.10(14) 5_666 1_545 ? O1 Zn1 Na1 74.90(14) . 1_545 ? O1W Zn1 Na1 80.91(11) . 1_545 ? O1W Zn1 Na1 99.09(11) 5_666 1_545 ? O1W Zn1 Na1 28.87(12) 1_545 1_545 ? O1W Zn1 Na1 151.13(12) 5_676 1_545 ? Na1 Zn1 Na1 124.079(18) 1_544 1_545 ? O1 Zn1 Na1 74.90(14) 5_666 1_554 ? O1 Zn1 Na1 105.10(14) . 1_554 ? O1W Zn1 Na1 99.09(11) . 1_554 ? O1W Zn1 Na1 80.91(11) 5_666 1_554 ? O1W Zn1 Na1 151.13(12) 1_545 1_554 ? O1W Zn1 Na1 28.87(12) 5_676 1_554 ? Na1 Zn1 Na1 55.921(18) 1_544 1_554 ? Na1 Zn1 Na1 180.0 1_545 1_554 ? O1W Zn2 O1W 180.0(3) . 5_677 ? O1W Zn2 O2 87.5(2) . 5_677 ? O1W Zn2 O2 92.5(2) 5_677 5_677 ? O1W Zn2 O2 92.5(2) . . ? O1W Zn2 O2 87.5(2) 5_677 . ? O2 Zn2 O2 180.0(2) 5_677 . ? O1W Zn2 O2 87.5(2) . 5_667 ? O1W Zn2 O2 92.5(2) 5_677 5_667 ? O2 Zn2 O2 97.2(2) 5_677 5_667 ? O2 Zn2 O2 82.8(2) . 5_667 ? O1W Zn2 O2 92.5(2) . 1_565 ? O1W Zn2 O2 87.5(2) 5_677 1_565 ? O2 Zn2 O2 82.8(2) 5_677 1_565 ? O2 Zn2 O2 97.2(2) . 1_565 ? O2 Zn2 O2 180.0(2) 5_667 1_565 ? O1W Zn2 Na1 90.000(1) . 1_565 ? O1W Zn2 Na1 90.000(1) 5_677 1_565 ? O2 Zn2 Na1 41.39(11) 5_677 1_565 ? O2 Zn2 Na1 138.61(11) . 1_565 ? O2 Zn2 Na1 138.61(11) 5_667 1_565 ? O2 Zn2 Na1 41.39(11) 1_565 1_565 ? O1W Zn2 Na1 90.000(1) . 1_545 ? O1W Zn2 Na1 90.000(1) 5_677 1_545 ? O2 Zn2 Na1 138.61(11) 5_677 1_545 ? O2 Zn2 Na1 41.39(11) . 1_545 ? O2 Zn2 Na1 41.39(11) 5_667 1_545 ? O2 Zn2 Na1 138.61(11) 1_565 1_545 ? Na1 Zn2 Na1 180.0 1_565 1_545 ? C2 Fe1 C2 109.3(4) 1_565 . ? C2 Fe1 C3 124.1(3) 1_565 . ? C2 Fe1 C3 40.4(3) . . ? C2 Fe1 C3 40.4(3) 1_565 1_565 ? C2 Fe1 C3 124.1(3) . 1_565 ? C3 Fe1 C3 108.5(4) . 1_565 ? C2 Fe1 C6 40.8(3) 1_565 1_565 ? C2 Fe1 C6 124.4(3) . 1_565 ? C3 Fe1 C6 160.4(3) . 1_565 ? C3 Fe1 C6 68.1(3) 1_565 1_565 ? C2 Fe1 C6 124.4(3) 1_565 . ? C2 Fe1 C6 40.8(3) . . ? C3 Fe1 C6 68.1(3) . . ? C3 Fe1 C6 160.4(3) 1_565 . ? C6 Fe1 C6 108.3(4) 1_565 . ? C2 Fe1 C4 159.9(4) 1_565 . ? C2 Fe1 C4 67.6(3) . . ? C3 Fe1 C4 40.5(3) . . ? C3 Fe1 C4 123.6(3) 1_565 . ? C6 Fe1 C4 157.6(3) 1_565 . ? C6 Fe1 C4 67.2(3) . . ? C2 Fe1 C4 67.6(3) 1_565 1_565 ? C2 Fe1 C4 159.9(4) . 1_565 ? C3 Fe1 C4 123.6(3) . 1_565 ? C3 Fe1 C4 40.5(3) 1_565 1_565 ? C6 Fe1 C4 67.2(3) 1_565 1_565 ? C6 Fe1 C4 157.6(3) . 1_565 ? C4 Fe1 C4 108.2(4) . 1_565 ? C2 Fe1 C5 159.5(4) 1_565 . ? C2 Fe1 C5 67.7(3) . . ? C3 Fe1 C5 67.6(3) . . ? C3 Fe1 C5 158.3(3) 1_565 . ? C6 Fe1 C5 122.8(3) 1_565 . ? C6 Fe1 C5 40.0(3) . . ? C4 Fe1 C5 39.5(3) . . ? C4 Fe1 C5 122.4(3) 1_565 . ? C2 Fe1 C5 67.7(3) 1_565 1_565 ? C2 Fe1 C5 159.5(4) . 1_565 ? C3 Fe1 C5 158.3(3) . 1_565 ? C3 Fe1 C5 67.6(3) 1_565 1_565 ? C6 Fe1 C5 40.0(3) 1_565 1_565 ? C6 Fe1 C5 122.8(3) . 1_565 ? C4 Fe1 C5 122.4(3) . 1_565 ? C4 Fe1 C5 39.5(3) 1_565 1_565 ? C5 Fe1 C5 107.7(4) . 1_565 ? C5 C6 C2 107.4(8) . . ? C5 C6 Fe1 70.3(3) . 1_545 ? C2 C6 Fe1 69.1(3) . 1_545 ? C5 C6 Fe1 70.3(3) . . ? C2 C6 Fe1 69.1(3) . . ? Fe1 C6 Fe1 108.3(4) 1_545 . ? C3 C2 C6 108.1(7) . . ? C3 C2 C1 127.3(7) . . ? C6 C2 C1 124.6(7) . . ? C3 C2 Fe1 70.2(3) . 1_545 ? C6 C2 Fe1 70.1(3) . 1_545 ? C1 C2 Fe1 125.36(18) . 1_545 ? C3 C2 Fe1 70.2(3) . . ? C6 C2 Fe1 70.1(3) . . ? C1 C2 Fe1 125.36(18) . . ? Fe1 C2 Fe1 109.3(4) 1_545 . ? C1 O2 Zn2 123.0(3) . . ? C1 O2 Na1 123.0(3) . 1_545 ? Zn2 O2 Na1 97.2(2) . 1_545 ? C1 O2 Zn2 123.0(3) . 1_545 ? Zn2 O2 Zn2 97.2(2) . 1_545 ? Na1 O2 Zn2 0.0 1_545 1_545 ? C1 O1 Zn1 119.3(5) . . ? O1 C1 O2 126.0(7) . . ? O1 C1 C2 118.5(7) . . ? O2 C1 C2 115.5(7) . . ? O1 C1 Na1 104.8(4) . 1_545 ? O2 C1 Na1 36.65(17) . 1_545 ? C2 C1 Na1 125.9(4) . 1_545 ? C5 C4 C3 108.8(7) . . ? C5 C4 Fe1 70.5(3) . . ? C3 C4 Fe1 69.6(3) . . ? C5 C4 Fe1 70.5(3) . 1_545 ? C3 C4 Fe1 69.6(3) . 1_545 ? Fe1 C4 Fe1 108.2(4) . 1_545 ? C4 C5 C6 108.5(8) . . ? C4 C5 Fe1 70.0(3) . 1_545 ? C6 C5 Fe1 69.7(3) . 1_545 ? C4 C5 Fe1 70.0(3) . . ? C6 C5 Fe1 69.7(3) . . ? Fe1 C5 Fe1 107.7(4) 1_545 . ? C2 C3 C4 107.0(7) . . ? C2 C3 Fe1 69.4(3) . . ? C4 C3 Fe1 69.9(3) . . ? C2 C3 Fe1 69.4(3) . 1_545 ? C4 C3 Fe1 69.9(3) . 1_545 ? Fe1 C3 Fe1 108.5(4) . 1_545 ? Zn2 O1W Zn1 118.60(16) . . ? Zn2 O1W Zn1 118.60(16) . 1_565 ? Zn1 O1W Zn1 99.9(2) . 1_565 ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 27.95 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.919 _refine_diff_density_min -0.800 _refine_diff_density_rms 0.178 #################################################### data_CdL(DMF)2(H2O) _database_code_CSD 179762 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C12H8O4Fe)Cd (C3H7NO)2 (H2O)' _chemical_formula_sum 'C18 H24 Cd Fe N2 O7' _chemical_formula_weight 548.64 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' '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' 'Cd' 'Cd' -0.8075 1.2024 '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' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.9152(11) _cell_length_b 10.2854(19) _cell_length_c 17.189(3) _cell_angle_alpha 88.915(3) _cell_angle_beta 89.652(3) _cell_angle_gamma 85.133(4) _cell_volume 1041.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1944 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 25.22 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.749 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 1.758 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4781 _exptl_absorpt_correction_T_max 0.7195 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 6580 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0909 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 28.37 _reflns_number_total 4679 _reflns_number_gt 3336 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0620P)^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_number_reflns 4679 _refine_ls_number_parameters 266 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0847 _refine_ls_R_factor_gt 0.0609 _refine_ls_wR_factor_ref 0.1408 _refine_ls_wR_factor_gt 0.1332 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 Cd1 Cd 0.18752(7) -0.52383(4) 0.24187(3) 0.03379(16) Uani 1 1 d . . . Fe1 Fe 0.50574(14) -0.03540(8) 0.26717(5) 0.0323(2) Uani 1 1 d . . . O1W O -0.1887(7) -0.4914(4) 0.2069(3) 0.0469(11) Uani 1 1 d . . . H1WA H -0.2719 -0.4515 0.2408 0.056 Uiso 1 1 d R . . H1WB H -0.2219 -0.5690 0.1995 0.056 Uiso 1 1 d R . . O1 O 0.4625(7) -0.3969(4) 0.3021(3) 0.0470(11) Uani 1 1 d . . . O2 O 0.1152(7) -0.3074(4) 0.2816(3) 0.0462(11) Uani 1 1 d . . . O3 O 0.1765(7) 0.2636(4) 0.1922(3) 0.0458(11) Uani 1 1 d . . . O4 O 0.5043(7) 0.3247(4) 0.2304(3) 0.0424(10) Uani 1 1 d . . . O5 O 0.0803(8) -0.6067(5) 0.3624(3) 0.0533(12) Uani 1 1 d . . . O6 O 0.2728(9) -0.4389(5) 0.1187(3) 0.0605(14) Uani 1 1 d . . . N1 N -0.1837(9) -0.6626(6) 0.4492(3) 0.0467(14) Uani 1 1 d . . . N2 N 0.1858(13) -0.2980(7) 0.0209(3) 0.0659(19) Uani 1 1 d . . . C1 C 0.3155(11) -0.3012(6) 0.3042(3) 0.0357(14) Uani 1 1 d . . . C2 C 0.3810(10) -0.1742(6) 0.3344(3) 0.0356(14) Uani 1 1 d . . . C3 C 0.5981(11) -0.1489(6) 0.3609(3) 0.0402(15) Uani 1 1 d . . . H3A H 0.7316 -0.2119 0.3649 0.048 Uiso 1 1 calc R . . C4 C 0.5865(12) -0.0153(6) 0.3810(4) 0.0458(16) Uani 1 1 d . . . H4A H 0.7122 0.0309 0.4004 0.055 Uiso 1 1 calc R . . C5 C 0.3645(12) 0.0394(7) 0.3676(4) 0.0470(17) Uani 1 1 d . . . H5A H 0.3096 0.1308 0.3754 0.056 Uiso 1 1 calc R . . C6 C 0.2358(11) -0.0575(6) 0.3386(3) 0.0387(14) Uani 1 1 d . . . H6A H 0.0754 -0.0465 0.3239 0.046 Uiso 1 1 calc R . . C7 C 0.3847(11) 0.0017(6) 0.1584(3) 0.0399(15) Uani 1 1 d . . . H7A H 0.2256 0.0033 0.1425 0.048 Uiso 1 1 calc R . . C8 C 0.5452(11) -0.1075(6) 0.1576(4) 0.0415(15) Uani 1 1 d . . . H8A H 0.5156 -0.1957 0.1421 0.050 Uiso 1 1 calc R . . C9 C 0.7540(12) -0.0701(6) 0.1859(4) 0.0454(16) Uani 1 1 d . . . H9A H 0.8940 -0.1272 0.1927 0.054 Uiso 1 1 calc R . . C10 C 0.7253(11) 0.0646(6) 0.2021(4) 0.0388(14) Uani 1 1 d . . . H10A H 0.8417 0.1172 0.2223 0.047 Uiso 1 1 calc R . . C11 C 0.4953(10) 0.1097(6) 0.1857(3) 0.0325(13) Uani 1 1 d . . . C12 C 0.3837(11) 0.2407(6) 0.2037(3) 0.0356(14) Uani 1 1 d . . . C13 C -0.1180(12) -0.6198(7) 0.3807(4) 0.0474(17) Uani 1 1 d . . . H13A H -0.2293 -0.5979 0.3436 0.057 Uiso 1 1 calc R . . C14 C -0.4229(12) -0.6744(8) 0.4676(5) 0.064(2) Uani 1 1 d . . . H14A H -0.5153 -0.6373 0.4258 0.097 Uiso 1 1 calc R . . H14B H -0.4622 -0.6287 0.5147 0.097 Uiso 1 1 calc R . . H14C H -0.4481 -0.7649 0.4746 0.097 Uiso 1 1 calc R . . C15 C -0.0238(15) -0.7010(11) 0.5086(5) 0.095(4) Uani 1 1 d . . . H15A H 0.1259 -0.6856 0.4908 0.143 Uiso 1 1 calc R . . H15B H -0.0298 -0.7922 0.5206 0.143 Uiso 1 1 calc R . . H15C H -0.0597 -0.6512 0.5544 0.143 Uiso 1 1 calc R . . C16 C 0.1474(14) -0.3572(7) 0.0862(4) 0.0562(19) Uani 1 1 d . . . H16A H 0.0092 -0.3343 0.1105 0.067 Uiso 1 1 calc R . . C17 C 0.396(2) -0.3226(12) -0.0177(6) 0.149(6) Uani 1 1 d . . . H17A H 0.5002 -0.3735 0.0159 0.224 Uiso 1 1 calc R . . H17B H 0.4571 -0.2413 -0.0307 0.224 Uiso 1 1 calc R . . H17C H 0.3750 -0.3697 -0.0644 0.224 Uiso 1 1 calc R . . C18 C 0.034(2) -0.1972(13) -0.0132(6) 0.125(5) Uani 1 1 d . . . H18A H -0.0993 -0.1839 0.0186 0.188 Uiso 1 1 calc R . . H18B H -0.0074 -0.2223 -0.0644 0.188 Uiso 1 1 calc R . . H18C H 0.1082 -0.1177 -0.0169 0.188 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 Cd1 0.0300(3) 0.0296(3) 0.0413(3) 0.00652(18) 0.00279(18) -0.00180(17) Fe1 0.0321(5) 0.0260(5) 0.0385(5) 0.0012(4) 0.0019(4) -0.0018(3) O1W 0.030(2) 0.043(3) 0.069(3) -0.012(2) 0.005(2) -0.011(2) O1 0.039(3) 0.032(2) 0.069(3) 0.003(2) 0.003(2) 0.001(2) O2 0.038(3) 0.036(3) 0.064(3) -0.005(2) -0.003(2) -0.003(2) O3 0.036(3) 0.039(3) 0.062(3) -0.002(2) -0.010(2) 0.005(2) O4 0.044(3) 0.025(2) 0.060(3) 0.0004(19) 0.004(2) -0.0071(19) O5 0.041(3) 0.073(3) 0.045(3) 0.015(2) 0.007(2) -0.006(2) O6 0.061(3) 0.061(3) 0.055(3) 0.021(3) 0.018(3) 0.012(3) N1 0.035(3) 0.066(4) 0.039(3) 0.009(3) 0.002(2) -0.009(3) N2 0.087(5) 0.067(4) 0.042(4) 0.017(3) 0.007(4) -0.002(4) C1 0.042(4) 0.023(3) 0.041(3) 0.006(3) 0.007(3) -0.001(3) C2 0.034(3) 0.033(3) 0.039(3) 0.005(3) 0.005(3) -0.001(3) C3 0.038(4) 0.042(4) 0.039(4) 0.005(3) -0.005(3) 0.000(3) C4 0.050(4) 0.046(4) 0.042(4) -0.008(3) -0.004(3) -0.008(3) C5 0.056(5) 0.039(4) 0.046(4) -0.008(3) 0.008(3) -0.002(3) C6 0.036(3) 0.039(4) 0.041(4) -0.002(3) 0.006(3) 0.000(3) C7 0.037(4) 0.043(4) 0.039(4) 0.001(3) 0.002(3) -0.007(3) C8 0.050(4) 0.033(3) 0.041(4) -0.004(3) 0.006(3) -0.002(3) C9 0.047(4) 0.031(3) 0.057(4) 0.003(3) 0.016(3) 0.005(3) C10 0.038(4) 0.035(3) 0.044(4) -0.001(3) 0.004(3) -0.007(3) C11 0.032(3) 0.035(3) 0.030(3) 0.009(2) 0.003(2) -0.004(3) C12 0.046(4) 0.030(3) 0.031(3) 0.006(2) 0.003(3) -0.007(3) C13 0.046(4) 0.058(4) 0.038(4) 0.007(3) -0.007(3) -0.006(3) C14 0.040(4) 0.086(6) 0.068(5) 0.008(4) 0.010(4) -0.015(4) C15 0.053(5) 0.171(11) 0.060(6) 0.047(6) 0.002(4) -0.014(6) C16 0.061(5) 0.057(5) 0.049(4) 0.009(4) 0.008(4) -0.005(4) C17 0.214(16) 0.118(10) 0.102(9) 0.046(7) 0.095(10) 0.046(10) C18 0.124(11) 0.166(13) 0.081(7) 0.054(7) -0.010(7) 0.009(9) _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 Cd1 O1W 2.304(4) . ? Cd1 O5 2.330(4) . ? Cd1 O4 2.343(4) 1_545 ? Cd1 O2 2.344(4) . ? Cd1 O6 2.343(4) . ? Cd1 O3 2.368(4) 1_545 ? Cd1 O1 2.420(5) . ? Cd1 C12 2.686(6) 1_545 ? Cd1 C1 2.713(6) . ? Fe1 C2 2.007(6) . ? Fe1 C3 2.022(6) . ? Fe1 C11 2.025(5) . ? Fe1 C4 2.035(6) . ? Fe1 C7 2.024(6) . ? Fe1 C9 2.035(6) . ? Fe1 C6 2.034(6) . ? Fe1 C10 2.040(6) . ? Fe1 C8 2.042(6) . ? Fe1 C5 2.048(7) . ? O1W H1WA 0.8501 . ? O1W H1WB 0.8500 . ? O1 C1 1.258(7) . ? O2 C1 1.256(7) . ? O3 C12 1.245(7) . ? O3 Cd1 2.368(4) 1_565 ? O4 C12 1.261(7) . ? O4 Cd1 2.343(4) 1_565 ? O5 C13 1.230(8) . ? O6 C16 1.204(8) . ? N1 C13 1.317(8) . ? N1 C15 1.424(9) . ? N1 C14 1.463(8) . ? N2 C16 1.296(8) . ? N2 C17 1.414(12) . ? N2 C18 1.431(12) . ? C1 C2 1.497(8) . ? C2 C3 1.411(8) . ? C2 C6 1.418(8) . ? C3 C4 1.419(9) . ? C3 H3A 0.9800 . ? C4 C5 1.403(9) . ? C4 H4A 0.9800 . ? C5 C6 1.405(9) . ? C5 H5A 0.9800 . ? C6 H6A 0.9800 . ? C7 C8 1.408(9) . ? C7 C11 1.425(8) . ? C7 H7A 0.9800 . ? C8 C9 1.417(9) . ? C8 H8A 0.9800 . ? C9 C10 1.414(9) . ? C9 H9A 0.9800 . ? C10 C11 1.428(8) . ? C10 H10A 0.9800 . ? C11 C12 1.487(9) . ? C12 Cd1 2.686(6) 1_565 ? C13 H13A 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9300 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? 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 O1W Cd1 O5 89.76(16) . . ? O1W Cd1 O4 141.29(16) . 1_545 ? O5 Cd1 O4 93.72(16) . 1_545 ? O1W Cd1 O2 81.24(15) . . ? O5 Cd1 O2 92.45(17) . . ? O4 Cd1 O2 136.94(15) 1_545 . ? O1W Cd1 O6 86.87(17) . . ? O5 Cd1 O6 176.62(17) . . ? O4 Cd1 O6 88.87(16) 1_545 . ? O2 Cd1 O6 87.11(17) . . ? O1W Cd1 O3 86.08(15) . 1_545 ? O5 Cd1 O3 88.04(17) . 1_545 ? O4 Cd1 O3 55.59(14) 1_545 1_545 ? O2 Cd1 O3 167.31(14) . 1_545 ? O6 Cd1 O3 91.65(17) . 1_545 ? O1W Cd1 O1 136.39(15) . . ? O5 Cd1 O1 91.39(16) . . ? O4 Cd1 O1 82.12(15) 1_545 . ? O2 Cd1 O1 55.15(15) . . ? O6 Cd1 O1 91.10(17) . . ? O3 Cd1 O1 137.53(15) 1_545 . ? O1W Cd1 C12 113.60(17) . 1_545 ? O5 Cd1 C12 90.48(17) . 1_545 ? O4 Cd1 C12 27.99(16) 1_545 1_545 ? O2 Cd1 C12 164.90(17) . 1_545 ? O6 Cd1 C12 90.81(17) . 1_545 ? O3 Cd1 C12 27.61(16) 1_545 1_545 ? O1 Cd1 C12 109.99(17) . 1_545 ? O1W Cd1 C1 108.78(17) . . ? O5 Cd1 C1 92.85(18) . . ? O4 Cd1 C1 109.53(17) 1_545 . ? O2 Cd1 C1 27.54(16) . . ? O6 Cd1 C1 88.31(18) . . ? O3 Cd1 C1 165.11(17) 1_545 . ? O1 Cd1 C1 27.62(16) . . ? C12 Cd1 C1 137.50(19) 1_545 . ? C2 Fe1 C3 41.0(2) . . ? C2 Fe1 C11 156.1(2) . . ? C3 Fe1 C11 161.7(2) . . ? C2 Fe1 C4 68.6(3) . . ? C3 Fe1 C4 40.9(2) . . ? C11 Fe1 C4 124.9(3) . . ? C2 Fe1 C7 120.4(3) . . ? C3 Fe1 C7 155.4(3) . . ? C11 Fe1 C7 41.2(2) . . ? C4 Fe1 C7 162.4(3) . . ? C2 Fe1 C9 124.3(2) . . ? C3 Fe1 C9 106.4(3) . . ? C11 Fe1 C9 69.0(2) . . ? C4 Fe1 C9 120.4(3) . . ? C7 Fe1 C9 68.9(3) . . ? C2 Fe1 C6 41.1(2) . . ? C3 Fe1 C6 69.0(3) . . ? C11 Fe1 C6 120.8(2) . . ? C4 Fe1 C6 68.2(3) . . ? C7 Fe1 C6 107.6(3) . . ? C9 Fe1 C6 162.0(3) . . ? C2 Fe1 C10 161.2(2) . . ? C3 Fe1 C10 124.1(3) . . ? C11 Fe1 C10 41.1(2) . . ? C4 Fe1 C10 107.5(3) . . ? C7 Fe1 C10 69.0(2) . . ? C9 Fe1 C10 40.6(2) . . ? C6 Fe1 C10 156.2(2) . . ? C2 Fe1 C8 107.4(3) . . ? C3 Fe1 C8 120.3(3) . . ? C11 Fe1 C8 68.5(2) . . ? C4 Fe1 C8 155.8(3) . . ? C7 Fe1 C8 40.5(2) . . ? C9 Fe1 C8 40.7(3) . . ? C6 Fe1 C8 125.4(3) . . ? C10 Fe1 C8 68.2(2) . . ? C2 Fe1 C5 68.2(3) . . ? C3 Fe1 C5 68.3(3) . . ? C11 Fe1 C5 108.2(3) . . ? C4 Fe1 C5 40.2(3) . . ? C7 Fe1 C5 125.8(3) . . ? C9 Fe1 C5 155.8(3) . . ? C6 Fe1 C5 40.3(2) . . ? C10 Fe1 C5 121.4(3) . . ? C8 Fe1 C5 162.5(3) . . ? Cd1 O1W H1WA 113.6 . . ? Cd1 O1W H1WB 101.9 . . ? H1WA O1W H1WB 113.6 . . ? C1 O1 Cd1 89.3(4) . . ? C1 O2 Cd1 92.8(4) . . ? C12 O3 Cd1 90.6(4) . 1_565 ? C12 O4 Cd1 91.3(4) . 1_565 ? C13 O5 Cd1 123.4(4) . . ? C16 O6 Cd1 121.8(5) . . ? C13 N1 C15 121.3(6) . . ? C13 N1 C14 121.9(6) . . ? C15 N1 C14 116.8(6) . . ? C16 N2 C17 120.2(8) . . ? C16 N2 C18 124.1(8) . . ? C17 N2 C18 115.5(8) . . ? O2 C1 O1 122.7(6) . . ? O2 C1 C2 118.4(5) . . ? O1 C1 C2 118.9(6) . . ? O2 C1 Cd1 59.7(3) . . ? O1 C1 Cd1 63.1(3) . . ? C2 C1 Cd1 176.7(4) . . ? C3 C2 C6 108.6(5) . . ? C3 C2 C1 126.1(6) . . ? C6 C2 C1 125.3(6) . . ? C3 C2 Fe1 70.1(3) . . ? C6 C2 Fe1 70.5(3) . . ? C1 C2 Fe1 123.6(4) . . ? C2 C3 C4 107.2(6) . . ? C2 C3 Fe1 68.9(3) . . ? C4 C3 Fe1 70.0(3) . . ? C2 C3 H3A 126.4 . . ? C4 C3 H3A 126.4 . . ? Fe1 C3 H3A 126.4 . . ? C5 C4 C3 108.2(6) . . ? C5 C4 Fe1 70.4(4) . . ? C3 C4 Fe1 69.1(3) . . ? C5 C4 H4A 125.9 . . ? C3 C4 H4A 125.9 . . ? Fe1 C4 H4A 125.9 . . ? C4 C5 C6 108.7(6) . . ? C4 C5 Fe1 69.4(4) . . ? C6 C5 Fe1 69.3(4) . . ? C4 C5 H5A 125.6 . . ? C6 C5 H5A 125.6 . . ? Fe1 C5 H5A 125.6 . . ? C5 C6 C2 107.3(6) . . ? C5 C6 Fe1 70.4(4) . . ? C2 C6 Fe1 68.4(3) . . ? C5 C6 H6A 126.3 . . ? C2 C6 H6A 126.3 . . ? Fe1 C6 H6A 126.3 . . ? C8 C7 C11 107.8(6) . . ? C8 C7 Fe1 70.4(4) . . ? C11 C7 Fe1 69.4(3) . . ? C8 C7 H7A 126.1 . . ? C11 C7 H7A 126.1 . . ? Fe1 C7 H7A 126.1 . . ? C7 C8 C9 108.7(6) . . ? C7 C8 Fe1 69.0(4) . . ? C9 C8 Fe1 69.4(4) . . ? C7 C8 H8A 125.6 . . ? C9 C8 H8A 125.6 . . ? Fe1 C8 H8A 125.6 . . ? C8 C9 C10 107.9(6) . . ? C8 C9 Fe1 69.9(4) . . ? C10 C9 Fe1 69.9(4) . . ? C8 C9 H9A 126.1 . . ? C10 C9 H9A 126.1 . . ? Fe1 C9 H9A 126.1 . . ? C9 C10 C11 107.9(6) . . ? C9 C10 Fe1 69.5(3) . . ? C11 C10 Fe1 68.9(3) . . ? C9 C10 H10A 126.0 . . ? C11 C10 H10A 126.0 . . ? Fe1 C10 H10A 126.0 . . ? C7 C11 C10 107.6(5) . . ? C7 C11 C12 125.9(5) . . ? C10 C11 C12 126.0(5) . . ? C7 C11 Fe1 69.4(3) . . ? C10 C11 Fe1 70.0(3) . . ? C12 C11 Fe1 120.0(4) . . ? O3 C12 O4 122.5(6) . . ? O3 C12 C11 119.3(5) . . ? O4 C12 C11 118.2(6) . . ? O3 C12 Cd1 61.8(3) . 1_565 ? O4 C12 Cd1 60.7(3) . 1_565 ? C11 C12 Cd1 177.8(4) . 1_565 ? O5 C13 N1 124.6(6) . . ? O5 C13 H13A 117.7 . . ? N1 C13 H13A 117.7 . . ? N1 C14 H14A 109.5 . . ? N1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 H15A 109.5 . . ? N1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O6 C16 N2 126.5(8) . . ? O6 C16 H16A 116.7 . . ? N2 C16 H16A 116.7 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.899 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 0.899 _refine_diff_density_max '2.168 (1.95/%A from Cd(1) )' _refine_diff_density_min -0.694 _refine_diff_density_rms 0.166