Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Martyn Coles' 'Sarah C. Cole' 'Peter B. Hitchcock' _publ_contact_author_name 'Dr Martyn Coles' _publ_contact_author_address ; Department of Chemistry University of Sussex Falmer Brighton BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email M.P.COLES@SUSSEX.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Dimesitylzinc: A strictly 2-coordinate, homoleptic diarylzinc compound ; data_oct2202 _database_code_CSD 217302 _audit_creation_date 2002-10-25T14:09:49-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common dimesitylzinc _chemical_formula_moiety 'C18 H22 Zn1' _chemical_formula_sum 'C18 H22 Zn' _chemical_formula_weight 303.73 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_Int_Tables_number 14 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 4.9926(2) _cell_length_b 10.1948(3) _cell_length_c 15.1331(5) _cell_angle_alpha 90 _cell_angle_beta 96.618(1) _cell_angle_gamma 90 _cell_volume 765.12(5) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2860 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 320 _exptl_special_details ; The compound crystallises as very long needles. When cut, the needles splinter and fragment lengthwise. It was impossible to obtain a clean short fragment and for the data collection a rather long piece , clear in the middle and frayed at the ends , was used. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.589 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.4598 _exptl_absorpt_correction_T_max 0.6674 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_unetI/netI 0.0336 _diffrn_reflns_number 4275 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.973 _diffrn_measured_fraction_theta_max 0.973 _reflns_number_total 1303 _reflns_number_gt 1154 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0497P)^2^+0.1916P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refined _refine_ls_extinction_method none _refine_ls_number_reflns 1303 _refine_ls_number_parameters 132 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0343 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0856 _refine_ls_wR_factor_gt 0.082 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.271 _refine_diff_density_min -0.469 _refine_diff_density_rms 0.052 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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 Zn Zn 0 0 0 0.04088(19) Uani 1 2 d S . . C1 C 0.2625(4) 0.12303(18) -0.03694(13) 0.0387(4) Uani 1 1 d . . . C2 C 0.3296(4) 0.1258(2) -0.12449(14) 0.0418(5) Uani 1 1 d . . . C3 C 0.5193(5) 0.2144(2) -0.14886(15) 0.0471(5) Uani 1 1 d . . . H3 H 0.558(4) 0.216(2) -0.2092(17) 0.051(6) Uiso 1 1 d . . . C4 C 0.6461(4) 0.3034(2) -0.08906(15) 0.0469(5) Uani 1 1 d . . . C5 C 0.5786(5) 0.3019(2) -0.00259(15) 0.0475(5) Uani 1 1 d . . . H5 H 0.650(5) 0.357(2) 0.0357(16) 0.049(7) Uiso 1 1 d . . . C6 C 0.3908(4) 0.2135(2) 0.02397(13) 0.0420(5) Uani 1 1 d . . . C7 C 0.1880(6) 0.0349(3) -0.19388(18) 0.0535(6) Uani 1 1 d . . . H7C H 0.197(6) -0.054(3) -0.176(2) 0.068(9) Uiso 1 1 d . . . H7B H 0.007(7) 0.054(3) -0.207(2) 0.078(9) Uiso 1 1 d . . . H7A H 0.254(7) 0.047(4) -0.248(3) 0.083(9) Uiso 1 1 d . . . C8 C 0.8507(5) 0.3998(3) -0.1163(2) 0.0613(7) Uani 1 1 d . . . H8C H 1.021(8) 0.374(3) -0.101(2) 0.101(11) Uiso 1 1 d . . . H8B H 0.827(12) 0.483(4) -0.089(4) 0.14(2) Uiso 1 1 d . . . H8A H 0.806(10) 0.423(5) -0.178(4) 0.157(18) Uiso 1 1 d . . . C9 C 0.3185(6) 0.2187(3) 0.11780(16) 0.0552(6) Uani 1 1 d . . . H9C H 0.432(6) 0.271(3) 0.153(2) 0.077(9) Uiso 1 1 d . . . H9B H 0.322(6) 0.139(3) 0.144(2) 0.069(8) Uiso 1 1 d . . . H9A H 0.152(6) 0.260(3) 0.1186(17) 0.065(8) Uiso 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 Zn 0.0520(3) 0.0380(3) 0.0338(3) 0.00053(11) 0.01014(17) -0.00164(12) C1 0.0432(10) 0.0358(10) 0.0376(10) 0.0043(8) 0.0065(8) 0.0065(8) C2 0.0446(11) 0.0409(10) 0.0408(11) 0.0025(9) 0.0089(9) 0.0095(9) C3 0.0478(12) 0.0546(13) 0.0411(12) 0.0081(10) 0.0137(9) 0.0112(10) C4 0.0392(11) 0.0481(12) 0.0537(13) 0.0133(10) 0.0066(9) 0.0067(9) C5 0.0465(11) 0.0435(13) 0.0511(14) 0.0021(10) 0.0001(9) -0.0005(11) C6 0.0460(11) 0.0407(11) 0.0394(11) 0.0046(9) 0.0051(9) 0.0062(9) C7 0.0617(16) 0.0599(15) 0.0408(14) -0.0060(12) 0.0148(12) 0.0001(14) C8 0.0497(14) 0.0614(16) 0.0736(18) 0.0208(14) 0.0104(12) -0.0024(12) C9 0.0713(18) 0.0552(15) 0.0390(13) -0.0019(11) 0.0065(11) -0.0075(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Zn C1 1.9422(19) 3 ? Zn C1 1.9422(19) . ? C1 C2 1.404(3) . ? C1 C6 1.405(3) . ? C2 C3 1.389(3) . ? C2 C7 1.513(4) . ? C3 C4 1.383(3) . ? C4 C5 1.388(3) . ? C4 C8 1.508(3) . ? C5 C6 1.393(3) . ? C6 C9 1.506(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 C1 Zn C1 180.00(13) 3 . ? C2 C1 C6 117.75(18) . . ? C2 C1 Zn 121.80(15) . . ? C6 C1 Zn 120.45(15) . . ? C3 C2 C1 120.5(2) . . ? C3 C2 C7 119.5(2) . . ? C1 C2 C7 120.0(2) . . ? C4 C3 C2 121.9(2) . . ? C3 C4 C5 117.8(2) . . ? C3 C4 C8 121.5(2) . . ? C5 C4 C8 120.7(2) . . ? C4 C5 C6 121.6(2) . . ? C5 C6 C1 120.43(19) . . ? C5 C6 C9 119.5(2) . . ? C1 C6 C9 120.1(2) . . ? #===END