# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1659 #============================================================================== data_global #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Dr. Hans-Georg Stammler ; _publ_contact_author_phone '49 521 1066165' _publ_contact_author_fax '49 521 1066146' _publ_contact_author_email georg.stammler@uni-bielefeld.de _publ_requested_journal 'Chem. Comm.' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for deposition To: edwin.constable@unibas.ch Subject: Depositing Crystal Structure Data Dear Madam or Sir, please find enclosed the crystallographic data of C~22~H~30~CrN~2~ (compound2) for deposition in your data file. With kind regards i. A. Beate Neumann ; #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Polymerisation of acrylonitrile with di(organoimido)chromium(VI) complexes ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Siemeling, Ulrich' ; Fakult\"at f. Chemie Universit\"at Bielefeld 33615 Bielefeld Germany ; 'K\"olling, Lars' ; Fakult\"at f. Chemie Universit\"at Bielefeld 33615 Bielefeld Germany ; 'Stammler, Anja' ; Fakult\"at f. Chemie Universit\"at Bielefeld 33615 Bielefeld Germany ; 'Stammler, Hans-Georg' ; Fakult\"at f. Chemie Universit\"at Bielefeld 33615 Bielefeld Germany ; 'Kaminski, Eric' ; Max-Planck-Institut fr Kohlenforschung Kaiser-Wilhelm-Platz 1 45470 Mlheim an der Ruhr Germany ; 'Fink, Gerhard' ; Max-Planck-Institut fr Kohlenforschung Kaiser-Wilhelm-Platz 1 45470 Mlheim an der Ruhr Germany ; #============================================================================== data_compound2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H30 Cr N2' _chemical_formula_weight 374.48 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' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.471(4) _cell_length_b 16.716(10) _cell_length_c 14.781(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.21(3) _cell_angle_gamma 90.00 _cell_volume 2059.9(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 7.9 _exptl_crystal_description plates _exptl_crystal_colour orange _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 0.561 _exptl_absorpt_correction_type 'semi-empirical from psi-scans' _exptl_absorpt_correction_T_min 0.429 _exptl_absorpt_correction_T_max 0.478 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens P2(1) diffractometer' _diffrn_measurement_method 'Wyckoff-scan' _diffrn_refln_scan_width 1.6000 _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3886 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_sigmaI/netI 0.0947 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3627 _reflns_number_gt 2346 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'P3 (1989)' _computing_cell_refinement 'P3 (1989)' _computing_data_reduction 'SHELXTL-PLUS (1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+0.0220P] 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 3627 _refine_ls_number_parameters 230 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1084 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1222 _refine_ls_wR_factor_gt 0.1050 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.82238(7) 0.83074(4) 0.60864(4) 0.01839(18) Uani 1 d . . . N1 N 0.7096(4) 0.84052(18) 0.5077(2) 0.0209(7) Uani 1 d . . . N2 N 0.7669(4) 0.74537(19) 0.6467(2) 0.0203(7) Uani 1 d . . . C1 C 0.8960(5) 0.9493(2) 0.7004(3) 0.0209(9) Uani 1 d . . . C2 C 1.0090(5) 0.9232(2) 0.7769(3) 0.0284(10) Uani 1 d . . . H2 H 0.9745 0.8907 0.8224 0.034 Uiso 1 calc R . . C3 C 1.1671(6) 0.9441(3) 0.7862(3) 0.0397(12) Uani 1 d . . . H3 H 1.2407 0.9263 0.8384 0.048 Uiso 1 calc R . . C4 C 1.2220(5) 0.9909(3) 0.7205(3) 0.0397(12) Uani 1 d . . . H4 H 1.3325 1.0044 0.7274 0.048 Uiso 1 calc R . . C5 C 1.1145(5) 1.0178(2) 0.6450(3) 0.0340(11) Uani 1 d . . . H5 H 1.1506 1.0506 0.6003 0.041 Uiso 1 calc R . . C6 C 0.9541(5) 0.9966(2) 0.6347(3) 0.0260(10) Uani 1 d . . . H6 H 0.8817 1.0145 0.5820 0.031 Uiso 1 calc R . . C7 C 0.7314(5) 0.9187(2) 0.6835(3) 0.0270(10) Uani 1 d . . . H7A H 0.6521 0.9546 0.6465 0.032 Uiso 1 calc R . . H7B H 0.6932 0.8991 0.7390 0.032 Uiso 1 calc R . . C8 C 1.0707(4) 0.7386(2) 0.5299(3) 0.0228(9) Uani 1 d . . . C9 C 1.1265(4) 0.6657(3) 0.5685(3) 0.0291(9) Uani 1 d . . . H9 H 1.1572 0.6619 0.6333 0.035 Uiso 1 calc R . . C10 C 1.1387(5) 0.5984(3) 0.5152(3) 0.0334(11) Uani 1 d . . . H10 H 1.1773 0.5497 0.5440 0.040 Uiso 1 calc R . . C11 C 1.0953(5) 0.6018(3) 0.4206(3) 0.0352(11) Uani 1 d . . . H11 H 1.1027 0.5557 0.3840 0.042 Uiso 1 calc R . . C12 C 1.0405(5) 0.6743(3) 0.3804(3) 0.0316(10) Uani 1 d . . . H12 H 1.0102 0.6778 0.3155 0.038 Uiso 1 calc R . . C13 C 1.0298(4) 0.7407(2) 0.4336(3) 0.0245(9) Uani 1 d . . . H13 H 0.9935 0.7896 0.4044 0.029 Uiso 1 calc R . . C14 C 1.0549(5) 0.8104(2) 0.5858(3) 0.0293(10) Uani 1 d . . . H14A H 1.0908 0.8577 0.5545 0.035 Uiso 1 calc R . . H14B H 1.1272 0.8047 0.6459 0.035 Uiso 1 calc R . . C15 C 0.6087(5) 0.7884(2) 0.3529(3) 0.0270(10) Uani 1 d . . . H15A H 0.6638 0.8324 0.3276 0.040 Uiso 1 calc R . . H15B H 0.5107 0.7747 0.3098 0.040 Uiso 1 calc R . . H15C H 0.6795 0.7416 0.3625 0.040 Uiso 1 calc R . . C16 C 0.4515(5) 0.8869(3) 0.4300(3) 0.0388(12) Uani 1 d . . . H16A H 0.4311 0.9058 0.4896 0.058 Uiso 1 calc R . . H16B H 0.3500 0.8711 0.3914 0.058 Uiso 1 calc R . . H16C H 0.5012 0.9298 0.3996 0.058 Uiso 1 calc R . . C17 C 0.5653(5) 0.8142(2) 0.4448(3) 0.0252(10) Uani 1 d . . . C18 C 0.4838(5) 0.7463(2) 0.4909(3) 0.0280(10) Uani 1 d . . . H18A H 0.4419 0.7694 0.5436 0.034 Uiso 1 calc R . . H18B H 0.3906 0.7269 0.4462 0.034 Uiso 1 calc R . . C19 C 0.5886(4) 0.6737(2) 0.5259(2) 0.0237(8) Uani 1 d . . . H19A H 0.6747 0.6693 0.4888 0.028 Uiso 1 calc R . . H19B H 0.5215 0.6250 0.5141 0.028 Uiso 1 calc R . . C20 C 0.6671(4) 0.6740(2) 0.6282(2) 0.0220(8) Uani 1 d . . . C21 C 0.5426(5) 0.6742(3) 0.6928(3) 0.0313(10) Uani 1 d . . . H21A H 0.5983 0.6755 0.7569 0.047 Uiso 1 calc R . . H21B H 0.4768 0.6257 0.6824 0.047 Uiso 1 calc R . . H21C H 0.4737 0.7214 0.6803 0.047 Uiso 1 calc R . . C22 C 0.7720(5) 0.5993(2) 0.6486(3) 0.0295(10) Uani 1 d . . . H22A H 0.8504 0.5977 0.6072 0.044 Uiso 1 calc R . . H22B H 0.7042 0.5514 0.6392 0.044 Uiso 1 calc R . . H22C H 0.8284 0.6010 0.7125 0.044 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 Cr1 0.0183(3) 0.0171(3) 0.0196(3) -0.0023(3) 0.0028(2) -0.0014(3) N1 0.0228(17) 0.0164(18) 0.0239(17) 0.0015(14) 0.0052(14) -0.0012(15) N2 0.0211(17) 0.0221(18) 0.0173(17) -0.0015(14) 0.0026(14) -0.0020(15) C1 0.033(2) 0.0108(19) 0.019(2) -0.0068(16) 0.0048(18) -0.0010(18) C2 0.044(3) 0.019(2) 0.022(2) -0.0031(18) 0.006(2) -0.001(2) C3 0.042(3) 0.032(3) 0.038(3) -0.007(2) -0.010(2) 0.004(2) C4 0.029(3) 0.033(3) 0.056(3) -0.011(2) 0.006(2) -0.010(2) C5 0.046(3) 0.018(2) 0.040(3) -0.004(2) 0.014(2) -0.007(2) C6 0.040(3) 0.014(2) 0.024(2) -0.0028(18) 0.0058(19) -0.0018(19) C7 0.036(2) 0.021(2) 0.027(2) -0.0031(18) 0.0133(19) 0.005(2) C8 0.0102(18) 0.029(2) 0.030(2) -0.0040(19) 0.0068(17) -0.0013(18) C9 0.023(2) 0.039(3) 0.027(2) 0.003(2) 0.0095(17) 0.003(2) C10 0.031(2) 0.024(2) 0.048(3) 0.010(2) 0.016(2) 0.011(2) C11 0.036(3) 0.025(2) 0.048(3) -0.012(2) 0.015(2) 0.002(2) C12 0.032(2) 0.036(2) 0.029(2) -0.005(2) 0.0100(19) 0.008(2) C13 0.021(2) 0.021(2) 0.033(2) 0.0041(19) 0.0087(18) 0.0072(18) C14 0.020(2) 0.032(3) 0.037(3) -0.0109(19) 0.0090(19) -0.0041(18) C15 0.032(2) 0.025(2) 0.023(2) -0.0021(18) -0.0001(19) -0.0040(19) C16 0.035(3) 0.039(3) 0.039(3) 0.005(2) -0.003(2) 0.012(2) C17 0.023(2) 0.028(3) 0.022(2) 0.0009(18) -0.0037(17) -0.0005(18) C18 0.018(2) 0.033(2) 0.031(2) 0.003(2) -0.0001(18) -0.0053(19) C19 0.026(2) 0.022(2) 0.022(2) -0.0022(19) 0.0019(16) -0.007(2) C20 0.024(2) 0.0176(19) 0.025(2) -0.0013(19) 0.0041(16) -0.0024(19) C21 0.033(2) 0.033(2) 0.030(2) 0.007(2) 0.0105(19) -0.002(2) C22 0.034(2) 0.018(2) 0.037(3) 0.005(2) 0.010(2) 0.000(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 Cr1 N1 1.631(3) . Y Cr1 N2 1.633(3) . Y Cr1 C7 2.070(4) . Y Cr1 C14 2.085(4) . Y Cr1 C1 2.420(4) . Y N1 C17 1.466(5) . Y N2 C20 1.459(5) . Y C1 C6 1.408(5) . Y C1 C2 1.415(5) . Y C1 C7 1.464(5) . Y C2 C3 1.368(6) . Y C3 C4 1.389(6) . Y C4 C5 1.385(6) . Y C5 C6 1.386(6) . Y C8 C9 1.393(6) . Y C8 C13 1.404(5) . Y C8 C14 1.476(5) . Y C9 C10 1.386(6) . Y C10 C11 1.383(6) . Y C11 C12 1.393(6) . Y C12 C13 1.373(5) . Y C15 C17 1.531(5) . Y C16 C17 1.542(5) . Y C17 C18 1.548(5) . Y C18 C19 1.538(6) . Y C19 C20 1.540(5) . Y C20 C22 1.532(5) . Y C20 C21 1.543(5) . Y 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 Cr1 N2 104.19(16) . . Y N1 Cr1 C7 101.82(16) . . Y N2 Cr1 C7 106.26(17) . . Y N1 Cr1 C14 106.56(16) . . Y N2 Cr1 C14 104.52(17) . . Y C7 Cr1 C14 130.89(16) . . Y N1 Cr1 C1 118.78(15) . . Y N2 Cr1 C1 125.73(15) . . Y C7 Cr1 C1 37.03(14) . . Y C14 Cr1 C1 93.87(15) . . Y C17 N1 Cr1 146.8(3) . . Y C20 N2 Cr1 147.3(3) . . Y C6 C1 C2 117.1(4) . . Y C6 C1 C7 121.2(4) . . Y C2 C1 C7 121.2(4) . . Y C6 C1 Cr1 99.2(2) . . Y C2 C1 Cr1 105.4(2) . . Y C7 C1 Cr1 58.36(19) . . Y C3 C2 C1 120.9(4) . . Y C2 C3 C4 121.1(4) . . Y C5 C4 C3 119.5(4) . . Y C4 C5 C6 119.8(4) . . Y C5 C6 C1 121.6(4) . . Y C1 C7 Cr1 84.6(2) . . Y C9 C8 C13 116.2(4) . . Y C9 C8 C14 122.7(4) . . Y C13 C8 C14 121.1(4) . . Y C10 C9 C8 122.1(4) . . Y C11 C10 C9 120.5(4) . . Y C10 C11 C12 118.4(4) . . Y C13 C12 C11 120.7(4) . . Y C12 C13 C8 122.0(4) . . Y C8 C14 Cr1 113.9(3) . . Y N1 C17 C15 110.1(3) . . Y N1 C17 C16 106.4(3) . . Y C15 C17 C16 109.8(3) . . Y N1 C17 C18 109.1(3) . . Y C15 C17 C18 112.4(3) . . Y C16 C17 C18 108.9(3) . . Y C19 C18 C17 116.8(3) . . Y C18 C19 C20 116.7(3) . . Y N2 C20 C22 109.4(3) . . Y N2 C20 C19 108.8(3) . . Y C22 C20 C19 109.0(3) . . Y N2 C20 C21 108.6(3) . . Y C22 C20 C21 108.4(3) . . Y C19 C20 C21 112.6(3) . . Y _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.358 _refine_diff_density_min -0.285 _refine_diff_density_rms 0.070 # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./