Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_VG0105 _database_code_CSD 186199 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Gibson, Vernon C.' ; O'Reilly, Rachel K. ; 'Reed, Warren' 'Wass, Duncan F.' _publ_contact_author_name 'Prof Vernon C Gibson' _publ_contact_author_address ; Chemistry Imperial College Exhibition Road London SW72AY UNITED KINGDOM ; _publ_contact_author_email 'V.GIBSON@IC.AC.UK' _publ_section_title ; Four coordinate iron complexes bearing [N,N] chelate ligands: catalysts for Atom Transfer Radical Polymerisation (ATRP) and Catalytic Chain Transfer (CCT) Polymerisation. ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C14 H24 N2 Cl2 Fe' _chemical_formula_weight 347.10 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M I2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 13.028(3) _cell_length_b 6.768(2) _cell_length_c 20.069(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.501(14) _cell_angle_gamma 90.00 _cell_volume 1734.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 49 _cell_measurement_theta_min 11.15 _cell_measurement_theta_max 27.69 _exptl_crystal_description 'platy needles' _exptl_crystal_colour 'Pink/magenta dichroic' _exptl_crystal_size_max 1.00 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method ? _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 9.712 _exptl_absorpt_correction_type 'Lamina [1 0 0]' _exptl_absorpt_correction_T_min 0.1554 _exptl_absorpt_correction_T_max 0.7776 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1221 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.50 _diffrn_reflns_theta_max 59.92 _reflns_number_total 1186 _reflns_number_observed 981 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 57 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1063P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1129 _refine_ls_number_parameters 87 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0660 _refine_ls_R_factor_obs 0.0519 _refine_ls_wR_factor_all 0.1555 _refine_ls_wR_factor_obs 0.1383 _refine_ls_goodness_of_fit_all 1.073 _refine_ls_goodness_of_fit_obs 1.099 _refine_ls_restrained_S_all 1.122 _refine_ls_restrained_S_obs 1.099 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe Fe 0.7500 0.20663(14) 0.5000 0.0482(4) Uani 1 d S . Cl Cl 0.87457(11) 0.3713(2) 0.57087(8) 0.0776(5) Uani 1 d . . C1 C 0.7184(4) -0.1983(8) 0.5273(3) 0.0592(12) Uani 1 d . . H1A H 0.6972(4) -0.3164(8) 0.5441(3) 0.071 Uiso 1 calc R . N1 N 0.6949(2) -0.0374(5) 0.5495(2) 0.0466(8) Uani 1 d . . C2 C 0.6355(3) -0.0344(7) 0.6052(2) 0.0495(10) Uani 1 d . . H2A H 0.5984(3) -0.1602(7) 0.6056(2) 0.059 Uiso 1 calc R . C3 C 0.7123(3) -0.0098(9) 0.6721(3) 0.0616(13) Uani 1 d . . H3A H 0.7518(3) 0.1114(9) 0.6711(3) 0.074 Uiso 1 calc R . H3B H 0.7614(3) -0.1192(9) 0.6784(3) 0.074 Uiso 1 calc R . C4 C 0.6554(4) -0.0029(11) 0.7312(3) 0.075(2) Uani 1 d . . H4A H 0.6216(4) -0.1291(11) 0.7348(3) 0.090 Uiso 1 calc R . H4B H 0.7058(4) 0.0186(11) 0.7732(3) 0.090 Uiso 1 calc R . C5 C 0.5736(5) 0.1599(11) 0.7225(3) 0.076(2) Uani 1 d . . H5A H 0.6079(5) 0.2877(11) 0.7250(3) 0.091 Uiso 1 calc R . H5B H 0.5347(5) 0.1526(11) 0.7589(3) 0.091 Uiso 1 calc R . C6 C 0.4987(4) 0.1385(9) 0.6541(3) 0.0659(14) Uani 1 d . . H6A H 0.4501(4) 0.2488(9) 0.6477(3) 0.079 Uiso 1 calc R . H6B H 0.4583(4) 0.0180(9) 0.6541(3) 0.079 Uiso 1 calc R . C7 C 0.5569(4) 0.1323(9) 0.5954(3) 0.0610(12) Uani 1 d . . H7A H 0.5072(4) 0.1139(9) 0.5529(3) 0.073 Uiso 1 calc R . H7B H 0.5928(4) 0.2569(9) 0.5929(3) 0.073 Uiso 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 Fe 0.0502(5) 0.0355(5) 0.0612(5) 0.000 0.0160(4) 0.000 Cl 0.0760(8) 0.0643(9) 0.0860(9) -0.0091(6) 0.0009(7) -0.0134(6) C1 0.066(3) 0.043(3) 0.076(3) -0.003(2) 0.032(3) -0.002(2) N1 0.038(2) 0.044(2) 0.059(2) -0.001(2) 0.013(2) 0.0017(14) C2 0.042(2) 0.049(2) 0.061(2) 0.002(2) 0.018(2) -0.007(2) C3 0.046(2) 0.078(4) 0.063(3) 0.011(2) 0.014(2) 0.010(2) C4 0.063(3) 0.111(5) 0.055(3) 0.014(3) 0.020(2) 0.013(3) C5 0.068(3) 0.097(5) 0.066(3) -0.001(3) 0.023(3) 0.006(3) C6 0.049(2) 0.077(4) 0.075(3) -0.002(3) 0.022(2) 0.015(2) C7 0.046(2) 0.078(3) 0.061(3) 0.001(2) 0.016(2) 0.016(2) _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 Fe N1 2.125(4) 2_656 ? Fe N1 2.125(4) . ? Fe Cl 2.2311(15) . ? Fe Cl 2.2311(15) 2_656 ? C1 N1 1.239(6) . ? C1 C1 1.495(9) 2_656 ? N1 C2 1.480(5) . ? C2 C7 1.510(7) . ? C2 C3 1.515(7) . ? C3 C4 1.521(7) . ? C4 C5 1.518(9) . ? C5 C6 1.524(8) . ? C6 C7 1.525(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe N1 78.0(2) 2_656 . ? N1 Fe Cl 114.57(10) 2_656 . ? N1 Fe Cl 111.13(11) . . ? N1 Fe Cl 111.13(11) 2_656 2_656 ? N1 Fe Cl 114.57(10) . 2_656 ? Cl Fe Cl 120.08(10) . 2_656 ? N1 C1 C1 118.4(3) . 2_656 ? C1 N1 C2 119.2(4) . . ? C1 N1 Fe 112.6(3) . . ? C2 N1 Fe 128.2(3) . . ? N1 C2 C7 110.7(4) . . ? N1 C2 C3 108.5(3) . . ? C7 C2 C3 110.2(4) . . ? C2 C3 C4 110.8(4) . . ? C5 C4 C3 111.9(5) . . ? C4 C5 C6 110.1(5) . . ? C5 C6 C7 111.7(4) . . ? C2 C7 C6 110.4(4) . . ? _refine_diff_density_max 0.348 _refine_diff_density_min -0.354 _refine_diff_density_rms 0.075