Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_compound 6 _database_code_CSD 155168 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Gemma Ciruelo' 'Tomás Cuenca' 'Rafael Gómez' 'Pilar Gómez-Sal' 'Avelino Martín' _publ_contact_author_name 'Prof Tomas Cuenca' _publ_contact_author_address ; Prof Tomas Cuenca Departamento de Quimica Inorganica Universidad de Alcala Campus Universitario 28771-Alcala de Henares SPAIN ; _publ_contact_author_email 'pilar.gomez@uah.es' _audit_creation_method SHELXL- _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H22 Cl6 Si2 Zr2' _chemical_formula_weight 641.64 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' 'Si' 'Si' 0.0817 0.0704 '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' 'Zr' 'Zr' -2.9673 0.5597 '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 7.0100(10) _cell_length_b 17.6740(10) _cell_length_c 9.6480(10) _cell_angle_alpha 90.00 _cell_angle_beta 102.56(1) _cell_angle_gamma 90.00 _cell_volume 1166.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prismatic _exptl_crystal_colour Pale yellow _exptl_crystal_size_max 0.20mm _exptl_crystal_size_mid 0.24mm _exptl_crystal_size_min 0.30mm _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.826 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 1.680 _exptl_absorpt_correction_type No _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 Enraf.Nonius CAD4 _diffrn_measurement_method w/2q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200? _diffrn_standards_interval_time ? _diffrn_standards_decay_ none _diffrn_reflns_number 2737 _diffrn_reflns_av_R_equivalents 0.0156 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 26.96 _reflns_number_total 2536 _reflns_number_gt 2009 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0366P)^2^+0.1374P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens located in Fourier map. _refine_ls_hydrogen_treatment isotropic _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2536 _refine_ls_number_parameters 153 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0677 _refine_ls_wR_factor_gt 0.0618 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.047 _refine_ls_shift/su_mean 0.005 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 Zr1 Zr 0.18565(4) 0.012913(15) 0.69377(3) 0.02929(9) Uani 1 d . . . Cl3 Cl 0.18129(9) 0.01258(4) 0.42210(7) 0.03278(15) Uani 1 d . . . Cl2 Cl 0.45735(12) 0.09901(5) 0.71394(9) 0.0489(2) Uani 1 d . . . Cl1 Cl 0.06506(14) 0.07264(5) 0.88109(8) 0.0516(2) Uani 1 d . . . Si1 Si 0.03754(12) -0.17877(4) 0.51217(8) 0.03378(18) Uani 1 d . . . C7 C -0.1697(6) -0.2254(2) 0.5661(5) 0.0552(9) Uani 1 d . . . C1 C 0.1950(4) -0.12747(15) 0.6654(3) 0.0346(6) Uani 1 d . . . C4 C 0.3178(6) -0.07895(19) 0.8882(3) 0.0552(10) Uani 1 d . . . C2 C 0.3887(5) -0.10082(17) 0.6730(4) 0.0422(7) Uani 1 d . . . C5 C 0.1548(6) -0.11288(17) 0.8013(3) 0.0444(7) Uani 1 d . . . C3 C 0.4628(6) -0.07135(19) 0.8097(4) 0.0556(10) Uani 1 d . . . C6 C 0.1898(8) -0.2421(3) 0.4293(6) 0.0630(11) Uani 1 d . . . H1 H 0.043(4) 0.1226(16) 0.598(3) 0.034(8) Uiso 1 d . . . H21 H 0.450(5) -0.1004(18) 0.600(4) 0.045(9) Uiso 1 d . . . H72 H -0.122(6) -0.263(3) 0.624(5) 0.082(14) Uiso 1 d . . . H63 H 0.254(7) -0.271(3) 0.498(5) 0.091(17) Uiso 1 d . . . H51 H 0.043(5) -0.1195(18) 0.825(4) 0.048(10) Uiso 1 d . . . H62 H 0.120(7) -0.264(3) 0.370(5) 0.084(16) Uiso 1 d . . . H71 H -0.265(7) -0.252(3) 0.480(5) 0.091(14) Uiso 1 d . . . H61 H 0.290(8) -0.217(3) 0.403(6) 0.11(2) Uiso 1 d . . . H41 H 0.327(5) -0.065(2) 0.994(4) 0.063(11) Uiso 1 d . . . H73 H -0.247(8) -0.192(3) 0.599(6) 0.109(19) Uiso 1 d . . . H31 H 0.584(6) -0.050(2) 0.841(4) 0.064(11) Uiso 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 Zr1 0.03502(15) 0.02684(14) 0.02276(13) -0.00140(10) -0.00087(9) -0.00009(11) Cl3 0.0333(3) 0.0362(3) 0.0284(3) 0.0005(3) 0.0057(2) -0.0015(3) Cl2 0.0428(4) 0.0469(4) 0.0511(4) -0.0034(4) -0.0027(3) -0.0124(3) Cl1 0.0731(6) 0.0521(5) 0.0310(4) -0.0075(3) 0.0144(4) 0.0036(4) Si1 0.0435(4) 0.0262(4) 0.0304(4) -0.0009(3) 0.0053(3) -0.0012(3) C7 0.065(2) 0.040(2) 0.062(2) 0.0057(17) 0.016(2) -0.0090(18) C1 0.0455(16) 0.0251(12) 0.0292(13) 0.0030(10) -0.0007(12) 0.0051(12) C4 0.087(3) 0.0394(17) 0.0281(15) 0.0036(13) -0.0115(17) 0.0072(17) C2 0.0402(16) 0.0375(16) 0.0433(17) 0.0005(13) -0.0033(14) 0.0094(13) C5 0.067(2) 0.0346(16) 0.0300(15) 0.0074(12) 0.0077(15) 0.0051(15) C3 0.057(2) 0.0393(17) 0.055(2) 0.0009(15) -0.0227(18) 0.0086(16) C6 0.067(3) 0.055(2) 0.068(3) -0.022(2) 0.018(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 Zr1 Cl1 2.3999(8) . ? Zr1 Cl2 2.4124(8) . ? Zr1 C5 2.483(3) . ? Zr1 C2 2.496(3) . ? Zr1 C1 2.499(3) . ? Zr1 C4 2.501(3) . ? Zr1 C3 2.510(3) . ? Zr1 Cl3 2.6112(8) 3_556 ? Zr1 Cl3 2.6146(7) . ? Cl3 Zr1 2.6113(8) 3_556 ? Si1 C7 1.841(4) . ? Si1 C6 1.845(4) . ? Si1 C1 1.875(3) . ? C1 C2 1.424(4) . ? C1 C5 1.423(4) . ? C4 C5 1.397(5) . ? C4 C3 1.400(6) . ? C2 C3 1.408(5) . ? 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 Cl1 Zr1 Cl2 93.61(3) . . ? Cl1 Zr1 C5 90.13(8) . . ? Cl2 Zr1 C5 132.09(9) . . ? Cl1 Zr1 C2 135.64(8) . . ? Cl2 Zr1 C2 93.47(8) . . ? C5 Zr1 C2 54.23(12) . . ? Cl1 Zr1 C1 122.77(7) . . ? Cl2 Zr1 C1 126.59(7) . . ? C5 Zr1 C1 33.21(9) . . ? C2 Zr1 C1 33.13(10) . . ? Cl1 Zr1 C4 81.64(9) . . ? Cl2 Zr1 C4 101.06(10) . . ? C5 Zr1 C4 32.55(11) . . ? C2 Zr1 C4 54.04(12) . . ? C1 Zr1 C4 54.78(10) . . ? Cl1 Zr1 C3 106.90(10) . . ? Cl2 Zr1 C3 79.47(10) . . ? C5 Zr1 C3 53.97(13) . . ? C2 Zr1 C3 32.67(11) . . ? C1 Zr1 C3 54.79(10) . . ? C4 Zr1 C3 32.44(13) . . ? Cl1 Zr1 Cl3 85.57(3) . 3_556 ? Cl2 Zr1 Cl3 146.13(3) . 3_556 ? C5 Zr1 Cl3 81.78(9) . 3_556 ? C2 Zr1 Cl3 110.64(7) . 3_556 ? C1 Zr1 Cl3 80.13(7) . 3_556 ? C4 Zr1 Cl3 112.25(10) . 3_556 ? C3 Zr1 Cl3 133.11(9) . 3_556 ? Cl1 Zr1 Cl3 145.76(3) . . ? Cl2 Zr1 Cl3 85.37(3) . . ? C5 Zr1 Cl3 115.70(7) . . ? C2 Zr1 Cl3 78.48(8) . . ? C1 Zr1 Cl3 83.26(6) . . ? C4 Zr1 Cl3 132.21(9) . . ? C3 Zr1 Cl3 106.54(10) . . ? Cl3 Zr1 Cl3 76.98(2) 3_556 . ? Zr1 Cl3 Zr1 103.02(2) 3_556 . ? C7 Si1 C6 114.6(2) . . ? C7 Si1 C1 111.05(16) . . ? C6 Si1 C1 109.77(19) . . ? C2 C1 C5 105.7(3) . . ? C2 C1 Si1 126.3(2) . . ? C5 C1 Si1 127.8(2) . . ? C2 C1 Zr1 73.34(17) . . ? C5 C1 Zr1 72.78(16) . . ? Si1 C1 Zr1 122.79(12) . . ? C5 C4 C3 108.2(3) . . ? C5 C4 Zr1 72.99(17) . . ? C3 C4 Zr1 74.12(18) . . ? C3 C2 C1 108.9(3) . . ? C3 C2 Zr1 74.20(19) . . ? C1 C2 Zr1 73.53(17) . . ? C4 C5 C1 109.3(3) . . ? C4 C5 Zr1 74.46(19) . . ? C1 C5 Zr1 74.02(16) . . ? C4 C3 C2 107.9(3) . . ? C4 C3 Zr1 73.4(2) . . ? C2 C3 Zr1 73.14(18) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 26.96 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.482 _refine_diff_density_min -0.423 _refine_diff_density_rms 0.087 #===END