# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1895 data_global # 1. SUBMISSION DETAILS _publ_contact_author_name 'R. Poli' _publ_requested_journal ' Dalton trans' _publ_section_title ; Synthesis, characterisation, and olecular and electronic structure of CpMoCl2(R1CCR2) (R1,R2 = Ph,Et,Me) : a new Class of Half-Sandwich 17-electron Molybdenum(III) Organometallics ; _publ_author_name ; Erwan le Grognec, Rinaldo Poli*, Philippe Richard ; _publ_author_address ; L.S.E.O. faculte des sciences, 6 Bd Gabriel 21000 Dijon, FRANCE ; _publ_contact_author_address # Address of author for correspondence ; L.S.E.O. faculte des sciences, 6 Bd Gabriel 21000 Dijon, FRANCE ; _publ_contact_author_email 'poli@satie.u-bourgogne.fr' _publ_contact_author_fax '+33-0380396098' _publ_contact_author_phone '+33-0380396881' data_p22 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C17 H26 Cl2 Mo' _chemical_formula_weight 397.22 _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 'Mo' 'Mo' -1.6832 0.6857 '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' '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' _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 7.4272(4) _cell_length_b 8.5344(3) _cell_length_c 13.7739(6) _cell_angle_alpha 89.929(3) _cell_angle_beta 79.954(3) _cell_angle_gamma 86.459(2) _cell_volume 858.0(5) _cell_measurement_reflns_used 9031 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _cell_formula_units_Z 2 _cell_measurement_temperature 110 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.118 _exptl_crystal_size_mid 0.062 _exptl_crystal_size_min 0.050 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method ? _exptl_crystal_F_000 408 _exptl_absorpt_coefficient_mu 1.065 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'KappaCCD' _diffrn_measurement_method 'KappaCCD' _diffrn_reflns_number 10243 _diffrn_reflns_av_R_equivalents 0.04 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 27.52 _reflns_number_total 3924 _reflns_number_gt 3546 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_cell_refinement 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997) ' _computing_molecular_graphics ORTEP3 _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 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^)+(0.0000P)^2^+1.2687P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3924 _refine_ls_number_parameters 185 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_all 0.0716 _refine_ls_wR_factor_ref 0.0673 _refine_ls_goodness_of_fit_all 1.098 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.098 _refine_ls_restrained_S_obs 1.088 _refine_ls_shift/su_max -0.002 _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 Mo Mo 0.70559(3) 0.74692(2) 0.846830(15) 0.01407(7) Uani 1 d . . Cl1 Cl 0.36900(8) 0.78861(7) 0.87717(5) 0.01995(14) Uani 1 d . . Cl2 Cl 0.62586(9) 0.50489(7) 0.76769(5) 0.02057(14) Uani 1 d . . C1 C 0.6569(4) 0.6670(3) 1.0119(2) 0.0214(6) Uani 1 d . . H1 H 0.5423(4) 0.6418(3) 1.0450(2) 0.028 Uiso 1 calc R . C2 C 0.7916(4) 0.5609(3) 0.9602(2) 0.0209(5) Uani 1 d . . H2 H 0.7814(4) 0.4535(3) 0.9536(2) 0.027 Uiso 1 calc R . C3 C 0.9454(4) 0.6444(3) 0.9198(2) 0.0211(5) Uani 1 d . . H3 H 1.0531(4) 0.6025(3) 0.8814(2) 0.027 Uiso 1 calc R . C4 C 0.9049(4) 0.8041(3) 0.9488(2) 0.0203(5) Uani 1 d . . H4 H 0.9830(4) 0.8851(3) 0.9335(2) 0.026 Uiso 1 calc R . C5 C 0.7247(4) 0.8193(3) 1.0052(2) 0.0210(5) Uani 1 d . . H5 H 0.6631(4) 0.9115(3) 1.0325(2) 0.027 Uiso 1 calc R . C6 C 0.7455(3) 0.9653(3) 0.8182(2) 0.0165(5) Uani 1 d . . C7 C 0.6948(4) 0.9340(3) 0.7244(2) 0.0182(5) Uani 1 d . . C8 C 0.7919(4) 0.8054(3) 0.6717(2) 0.0193(5) Uani 1 d . . C9 C 0.9402(4) 0.7307(3) 0.7130(2) 0.0201(5) Uani 1 d . . C10 C 0.7955(4) 1.1190(3) 0.8527(2) 0.0206(5) Uani 1 d . . H10A H 0.7933(4) 1.1155(3) 0.9233(2) 0.027 Uiso 1 calc R . H10B H 0.7059(4) 1.2005(3) 0.8400(2) 0.027 Uiso 1 calc R . C12 C 0.5372(4) 1.0318(3) 0.6938(2) 0.0263(6) Uani 1 d . . H12A H 0.4679(4) 1.0874(3) 0.7510(2) 0.034 Uiso 1 calc R . H12B H 0.4561(4) 0.9630(3) 0.6690(2) 0.034 Uiso 1 calc R . C14 C 0.7331(4) 0.7430(4) 0.5800(2) 0.0274(6) Uani 1 d . . H14A H 0.6102(4) 0.7857(4) 0.5767(2) 0.036 Uiso 1 calc R . H14B H 0.7303(4) 0.6296(4) 0.5839(2) 0.036 Uiso 1 calc R . C16 C 1.0459(4) 0.5815(3) 0.6700(2) 0.0281(6) Uani 1 d . . H16A H 0.9834(4) 0.5376(3) 0.6211(2) 0.036 Uiso 1 calc R . H16B H 1.0489(4) 0.5051(3) 0.7220(2) 0.036 Uiso 1 calc R . C11 C 0.9870(4) 1.1592(3) 0.8004(2) 0.0264(6) Uani 1 d . . H11A H 1.0156(4) 1.2588(3) 0.8240(2) 0.034 Uiso 1 calc R . H11B H 0.9888(4) 1.1644(3) 0.7306(2) 0.034 Uiso 1 calc R . H11C H 1.0761(4) 1.0795(3) 0.8138(2) 0.034 Uiso 1 calc R . C15 C 0.8633(4) 0.7866(3) 0.4866(2) 0.0265(6) Uani 1 d . . H15A H 0.8224(4) 0.7455(3) 0.4299(2) 0.034 Uiso 1 calc R . H15B H 0.9846(4) 0.7429(3) 0.4892(2) 0.034 Uiso 1 calc R . H15C H 0.8646(4) 0.8988(3) 0.4821(2) 0.034 Uiso 1 calc R . C13 C 0.6033(4) 1.1503(3) 0.6145(2) 0.0287(6) Uani 1 d . . H13A H 0.4997(4) 1.2098(3) 0.5972(2) 0.037 Uiso 1 calc R . H13B H 0.6700(4) 1.0957(3) 0.5572(2) 0.037 Uiso 1 calc R . H13C H 0.6818(4) 1.2200(3) 0.6391(2) 0.037 Uiso 1 calc R . C17 C 1.2407(4) 0.6122(4) 0.6224(2) 0.0302(7) Uani 1 d . . H17A H 1.3035(4) 0.5156(4) 0.5961(2) 0.039 Uiso 1 calc R . H17B H 1.3037(4) 0.6539(4) 0.6709(2) 0.039 Uiso 1 calc R . H17C H 1.2382(4) 0.6864(4) 0.5701(2) 0.039 Uiso 1 calc R . H9 H 1.0232(43) 0.7969(35) 0.7392(22) 0.023(8) 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 Mo 0.01445(12) 0.01519(11) 0.01219(12) 0.00245(8) -0.00090(8) -0.00205(8) Cl1 0.0145(3) 0.0243(3) 0.0202(3) 0.0006(2) -0.0002(2) -0.0021(2) Cl2 0.0244(3) 0.0174(3) 0.0197(3) 0.0003(2) -0.0020(3) -0.0052(2) C1 0.0224(14) 0.0290(14) 0.0135(12) 0.0102(10) -0.0037(10) -0.0062(11) C2 0.0245(14) 0.0193(12) 0.0213(13) 0.0080(10) -0.0100(11) -0.0037(10) C3 0.0171(13) 0.0264(13) 0.0203(13) 0.0063(11) -0.0058(10) 0.0014(10) C4 0.0216(13) 0.0240(13) 0.0181(13) 0.0068(10) -0.0088(11) -0.0067(11) C5 0.0271(14) 0.0268(13) 0.0101(12) 0.0010(10) -0.0052(10) -0.0038(11) C6 0.0150(12) 0.0186(12) 0.0149(12) 0.0036(9) -0.0008(9) 0.0008(9) C7 0.0202(13) 0.0188(12) 0.0156(12) 0.0073(10) -0.0019(10) -0.0059(10) C8 0.0224(13) 0.0223(12) 0.0129(12) 0.0044(10) 0.0007(10) -0.0093(10) C9 0.0217(14) 0.0196(12) 0.0165(13) 0.0009(10) 0.0047(10) -0.0043(11) C10 0.0255(14) 0.0175(12) 0.0173(13) 0.0008(10) 0.0004(11) -0.0012(10) C12 0.0242(14) 0.0310(15) 0.0239(14) 0.0083(12) -0.0062(12) 0.0006(12) C14 0.033(2) 0.034(2) 0.0149(13) -0.0010(11) -0.0016(12) -0.0117(13) C16 0.031(2) 0.0219(13) 0.0264(15) -0.0034(11) 0.0066(12) 0.0014(12) C11 0.029(2) 0.0259(14) 0.0239(14) 0.0025(11) -0.0014(12) -0.0100(12) C15 0.031(2) 0.0315(15) 0.0165(13) 0.0032(11) -0.0020(11) -0.0057(12) C13 0.039(2) 0.0247(14) 0.0221(14) 0.0051(11) -0.0060(13) 0.0045(12) C17 0.0230(15) 0.0306(15) 0.034(2) -0.0016(13) 0.0017(12) 0.0026(12) _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 Mo C6 1.934(2) . ? Mo C4 2.284(3) . ? Mo C5 2.298(2) . ? Mo C9 2.303(3) . ? Mo C3 2.319(3) . ? Mo C7 2.329(2) . ? Mo C1 2.346(2) . ? Mo C2 2.363(2) . ? Mo C8 2.444(2) . ? Mo Cl1 2.4652(7) . ? Mo Cl2 2.4874(6) . ? C1 C2 1.404(4) . ? C1 C5 1.420(4) . ? C2 C3 1.414(4) . ? C3 C4 1.420(4) . ? C4 C5 1.425(4) . ? C6 C7 1.438(4) . ? C6 C10 1.486(4) . ? C7 C8 1.404(4) . ? C7 C12 1.515(4) . ? C8 C9 1.440(4) . ? C8 C14 1.514(4) . ? C9 C16 1.518(4) . ? C10 C11 1.537(4) . ? C12 C13 1.526(4) . ? C14 C15 1.529(4) . ? C16 C17 1.519(4) . ? 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 C6 Mo C4 77.62(10) . . ? C6 Mo C5 83.94(10) . . ? C4 Mo C5 36.22(10) . . ? C6 Mo C9 77.52(10) . . ? C4 Mo C9 90.95(10) . . ? C5 Mo C9 126.92(10) . . ? C6 Mo C3 107.88(10) . . ? C4 Mo C3 35.91(9) . . ? C5 Mo C3 60.00(10) . . ? C9 Mo C3 79.24(10) . . ? C6 Mo C7 38.02(10) . . ? C4 Mo C7 112.31(9) . . ? C5 Mo C7 121.07(9) . . ? C9 Mo C7 63.06(9) . . ? C3 Mo C7 131.65(9) . . ? C6 Mo C1 118.71(10) . . ? C4 Mo C1 59.13(9) . . ? C5 Mo C1 35.58(9) . . ? C9 Mo C1 137.58(10) . . ? C3 Mo C1 58.77(10) . . ? C7 Mo C1 152.48(9) . . ? C6 Mo C2 136.19(10) . . ? C4 Mo C2 58.79(9) . . ? C5 Mo C2 58.91(9) . . ? C9 Mo C2 105.44(10) . . ? C3 Mo C2 35.14(9) . . ? C7 Mo C2 166.53(10) . . ? C1 Mo C2 34.68(9) . . ? C6 Mo C8 65.26(9) . . ? C4 Mo C8 117.71(9) . . ? C5 Mo C8 145.86(9) . . ? C9 Mo C8 35.16(9) . . ? C3 Mo C8 114.30(9) . . ? C7 Mo C8 34.11(9) . . ? C1 Mo C8 172.38(9) . . ? C2 Mo C8 137.82(9) . . ? C6 Mo Cl1 93.97(8) . . ? C4 Mo Cl1 128.26(7) . . ? C5 Mo Cl1 92.57(7) . . ? C9 Mo Cl1 137.51(7) . . ? C3 Mo Cl1 141.56(7) . . ? C7 Mo Cl1 84.55(7) . . ? C1 Mo Cl1 83.12(7) . . ? C2 Mo Cl1 108.88(7) . . ? C8 Mo Cl1 103.42(7) . . ? C6 Mo Cl2 140.61(8) . . ? C4 Mo Cl2 135.49(7) . . ? C5 Mo Cl2 134.93(7) . . ? C9 Mo Cl2 80.85(7) . . ? C3 Mo Cl2 99.80(7) . . ? C7 Mo Cl2 102.64(7) . . ? C1 Mo Cl2 99.42(7) . . ? C2 Mo Cl2 81.28(7) . . ? C8 Mo Cl2 78.12(6) . . ? Cl1 Mo Cl2 80.36(2) . . ? C2 C1 C5 108.6(2) . . ? C2 C1 Mo 73.32(15) . . ? C5 C1 Mo 70.38(14) . . ? C1 C2 C3 108.7(2) . . ? C1 C2 Mo 72.00(14) . . ? C3 C2 Mo 70.75(14) . . ? C2 C3 C4 107.3(2) . . ? C2 C3 Mo 74.11(15) . . ? C4 C3 Mo 70.71(14) . . ? C3 C4 C5 108.5(2) . . ? C3 C4 Mo 73.38(15) . . ? C5 C4 Mo 72.43(14) . . ? C1 C5 C4 106.9(2) . . ? C1 C5 Mo 74.03(15) . . ? C4 C5 Mo 71.35(14) . . ? C7 C6 C10 126.1(2) . . ? C7 C6 Mo 86.0(2) . . ? C10 C6 Mo 147.9(2) . . ? C8 C7 C6 115.2(2) . . ? C8 C7 C12 125.8(2) . . ? C6 C7 C12 118.9(2) . . ? C8 C7 Mo 77.43(14) . . ? C6 C7 Mo 55.94(13) . . ? C12 C7 Mo 132.1(2) . . ? C7 C8 C9 116.8(2) . . ? C7 C8 C14 120.8(2) . . ? C9 C8 C14 122.3(2) . . ? C7 C8 Mo 68.46(14) . . ? C9 C8 Mo 67.06(14) . . ? C14 C8 Mo 132.7(2) . . ? C8 C9 C16 122.9(2) . . ? C8 C9 Mo 77.79(15) . . ? C16 C9 Mo 126.2(2) . . ? C6 C10 C11 111.3(2) . . ? C7 C12 C13 112.0(2) . . ? C8 C14 C15 111.5(2) . . ? C9 C16 C17 111.7(2) . . ? _refine_diff_density_max 0.498 _refine_diff_density_min -0.841 _refine_diff_density_rms 0.095 #==END data_poli17ap _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C19 H15 Cl2 Mo' _chemical_formula_weight 410.15 _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' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 18.958(6) _cell_length_b 12.485(1) _cell_length_c 7.187(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1701.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.24 _cell_measurement_theta_max 18.32 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method none _exptl_crystal_F_000 820 _exptl_absorpt_coefficient_mu 1.078 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 0.98 _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 'Enraf Nonius CAD4' _diffrn_measurement_method omega-scans _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 7200 _diffrn_standards_decay_% 3 _diffrn_reflns_number 1860 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0160 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 26.30 _reflns_number_total 1860 _reflns_number_gt 1764 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 EXPRESS' _computing_cell_refinement 'SET4 (de Boer & Duisenberg, 1984)' _computing_data_reduction 'XCAD4 (Harms, 1996)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP3 _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 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-factors 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^)+(0.0326P)^2^+0.2117P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(5) _refine_ls_number_reflns 1860 _refine_ls_number_parameters 199 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0231 _refine_ls_R_factor_gt 0.0198 _refine_ls_wR_factor_all 0.0526 _refine_ls_wR_factor_ref 0.0512 _refine_ls_goodness_of_fit_all 1.072 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.072 _refine_ls_restrained_S_obs 1.074 _refine_ls_shift/su_max -0.002 _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 Mo1 Mo 0.781947(10) 0.58261(2) 0.73650(5) 0.03549(8) Uani 1 d . . Cl1 Cl 0.79460(5) 0.43956(7) 0.9518(2) 0.0574(2) Uani 1 d . . Cl2 Cl 0.76732(5) 0.70208(7) 0.98987(14) 0.0543(2) Uani 1 d . . C1 C 0.6997(2) 0.4850(3) 0.5672(7) 0.0705(12) Uani 1 d . . H1 H 0.6960(2) 0.4114(3) 0.5836(7) 0.092 Uiso 1 calc R . C2 C 0.7442(2) 0.5384(4) 0.4381(6) 0.0782(13) Uani 1 d . . H2 H 0.7752(2) 0.5063(4) 0.3548(6) 0.102 Uiso 1 calc R . C3 C 0.7324(2) 0.6502(4) 0.4600(6) 0.0664(11) Uani 1 d . . H3 H 0.7542(2) 0.7045(4) 0.3928(6) 0.086 Uiso 1 calc R . C4 C 0.6836(2) 0.6637(3) 0.5963(6) 0.0644(10) Uani 1 d . . H4 H 0.6667(2) 0.7295(3) 0.6373(6) 0.084 Uiso 1 calc R . C5 C 0.6624(2) 0.5641(3) 0.6659(7) 0.0635(10) Uani 1 d . . H5 H 0.6297(2) 0.5524(3) 0.7601(7) 0.083 Uiso 1 calc R . C6 C 0.87175(15) 0.6543(2) 0.6443(4) 0.0385(6) Uani 1 d . . C7 C 0.8801(2) 0.5508(2) 0.6415(5) 0.0407(6) Uani 1 d . . C8 C 0.9292(2) 0.4631(2) 0.6092(5) 0.0439(7) Uani 1 d . . C9 C 0.9030(2) 0.3619(2) 0.5616(6) 0.0600(9) Uani 1 d . . H9 H 0.8547(2) 0.3500(2) 0.5540(6) 0.078 Uiso 1 calc R . C10 C 0.9504(2) 0.2795(3) 0.5258(7) 0.0730(12) Uani 1 d . . H10 H 0.9333(2) 0.2127(3) 0.4902(7) 0.095 Uiso 1 calc R . C11 C 1.0214(2) 0.2947(3) 0.5420(7) 0.0710(12) Uani 1 d . . H11 H 1.0523(2) 0.2387(3) 0.5172(7) 0.092 Uiso 1 calc R . C12 C 1.0472(2) 0.3930(3) 0.5949(6) 0.0645(10) Uani 1 d . . H12 H 1.0955(2) 0.4025(3) 0.6103(6) 0.084 Uiso 1 calc R . C13 C 1.0017(2) 0.4780(3) 0.6254(5) 0.0503(8) Uani 1 d . . H13 H 1.0196(2) 0.5450(3) 0.6567(5) 0.065 Uiso 1 calc R . C14 C 0.90438(15) 0.7569(2) 0.6035(5) 0.0402(6) Uani 1 d . . C15 C 0.8715(2) 0.8519(2) 0.6547(5) 0.0483(7) Uani 1 d . . H15 H 0.8275(2) 0.8499(2) 0.7118(5) 0.063 Uiso 1 calc R . C16 C 0.9036(2) 0.9496(3) 0.6215(6) 0.0606(10) Uani 1 d . . H16 H 0.8815(2) 1.0126(3) 0.6585(6) 0.079 Uiso 1 calc R . C17 C 0.9680(2) 0.9538(3) 0.5340(7) 0.0613(9) Uani 1 d . . H17 H 0.9896(2) 1.0195(3) 0.5121(7) 0.080 Uiso 1 calc R . C18 C 1.0006(2) 0.8605(3) 0.4790(6) 0.0575(9) Uani 1 d . . H18 H 1.0438(2) 0.8637(3) 0.4179(6) 0.075 Uiso 1 calc R . C19 C 0.96979(15) 0.7617(2) 0.5135(6) 0.0474(7) Uani 1 d . . H19 H 0.99245(15) 0.6991(2) 0.4771(6) 0.062 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 Mo1 0.03681(13) 0.03399(12) 0.03566(13) -0.00121(13) 0.00262(14) -0.00175(7) Cl1 0.0692(5) 0.0435(4) 0.0596(6) 0.0137(4) 0.0072(5) -0.0031(4) Cl2 0.0693(5) 0.0505(4) 0.0430(4) -0.0093(4) 0.0064(4) 0.0105(4) C1 0.075(2) 0.050(2) 0.086(3) -0.006(2) -0.034(3) -0.013(2) C2 0.057(2) 0.133(4) 0.045(2) -0.031(3) -0.011(2) 0.003(3) C3 0.074(2) 0.074(3) 0.052(3) 0.010(2) -0.019(2) -0.011(2) C4 0.063(2) 0.062(2) 0.068(3) 0.000(2) -0.019(2) 0.013(2) C5 0.041(2) 0.083(3) 0.067(2) 0.003(2) -0.003(2) -0.010(2) C6 0.0393(14) 0.0389(14) 0.0371(15) -0.0025(12) 0.0007(13) -0.0003(11) C7 0.0414(15) 0.0375(13) 0.043(2) -0.0051(13) 0.0059(13) -0.0039(12) C8 0.049(2) 0.0377(14) 0.045(2) -0.0017(14) 0.0101(14) 0.0025(13) C9 0.065(2) 0.040(2) 0.074(3) -0.009(2) 0.003(2) 0.0004(15) C10 0.094(3) 0.043(2) 0.082(3) -0.015(2) 0.008(3) 0.013(2) C11 0.086(3) 0.066(2) 0.061(3) 0.005(2) 0.020(2) 0.032(2) C12 0.056(2) 0.078(2) 0.060(2) 0.017(2) 0.018(2) 0.020(2) C13 0.050(2) 0.053(2) 0.049(2) 0.005(2) 0.011(2) 0.0024(15) C14 0.0429(14) 0.0397(13) 0.0380(14) 0.0008(13) -0.0027(13) -0.0062(12) C15 0.051(2) 0.0411(15) 0.053(2) 0.0027(14) 0.003(2) -0.0001(12) C16 0.073(2) 0.0378(15) 0.071(3) -0.001(2) 0.001(2) 0.001(2) C17 0.067(2) 0.043(2) 0.074(3) 0.010(2) -0.005(2) -0.014(2) C18 0.045(2) 0.060(2) 0.068(2) 0.010(2) 0.004(2) -0.0128(13) C19 0.046(2) 0.044(2) 0.052(2) 0.0030(15) 0.0040(14) -0.0020(13) _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 Mo1 C7 2.021(3) . ? Mo1 C6 2.034(3) . ? Mo1 C1 2.322(4) . ? Mo1 C2 2.328(4) . ? Mo1 C5 2.334(4) . ? Mo1 C4 2.349(4) . ? Mo1 C3 2.355(4) . ? Mo1 Cl2 2.3702(9) . ? Mo1 Cl1 2.3750(9) . ? C1 C5 1.407(6) . ? C1 C2 1.420(7) . ? C2 C3 1.422(6) . ? C3 C4 1.358(6) . ? C4 C5 1.399(5) . ? C6 C7 1.303(4) . ? C6 C14 1.452(4) . ? C7 C8 1.455(4) . ? C8 C13 1.394(5) . ? C8 C9 1.400(4) . ? C9 C10 1.389(5) . ? C10 C11 1.366(6) . ? C11 C12 1.375(6) . ? C12 C13 1.384(5) . ? C14 C15 1.390(4) . ? C14 C19 1.400(4) . ? C15 C16 1.383(4) . ? C16 C17 1.375(5) . ? C17 C18 1.376(5) . ? C18 C19 1.386(4) . ? 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 C7 Mo1 C6 37.47(11) . . ? C7 Mo1 C1 109.7(2) . . ? C6 Mo1 C1 128.5(2) . . ? C7 Mo1 C2 85.72(15) . . ? C6 Mo1 C2 93.5(2) . . ? C1 Mo1 C2 35.6(2) . . ? C7 Mo1 C5 143.2(2) . . ? C6 Mo1 C5 141.75(14) . . ? C1 Mo1 C5 35.2(2) . . ? C2 Mo1 C5 58.5(2) . . ? C7 Mo1 C4 132.1(2) . . ? C6 Mo1 C4 109.57(15) . . ? C1 Mo1 C4 57.9(2) . . ? C2 Mo1 C4 57.5(2) . . ? C5 Mo1 C4 34.75(14) . . ? C7 Mo1 C3 98.8(2) . . ? C6 Mo1 C3 84.35(14) . . ? C1 Mo1 C3 58.53(15) . . ? C2 Mo1 C3 35.4(2) . . ? C5 Mo1 C3 57.6(2) . . ? C4 Mo1 C3 33.6(2) . . ? C7 Mo1 Cl2 119.41(9) . . ? C6 Mo1 Cl2 94.08(9) . . ? C1 Mo1 Cl2 130.84(13) . . ? C2 Mo1 Cl2 145.20(13) . . ? C5 Mo1 Cl2 96.64(12) . . ? C4 Mo1 Cl2 88.02(11) . . ? C3 Mo1 Cl2 112.10(12) . . ? C7 Mo1 Cl1 88.81(10) . . ? C6 Mo1 Cl1 117.29(9) . . ? C1 Mo1 Cl1 90.83(12) . . ? C2 Mo1 Cl1 116.93(15) . . ? C5 Mo1 Cl1 99.52(11) . . ? C4 Mo1 Cl1 133.14(12) . . ? C3 Mo1 Cl1 149.26(11) . . ? Cl2 Mo1 Cl1 89.12(4) . . ? C5 C1 C2 107.4(4) . . ? C5 C1 Mo1 72.9(2) . . ? C2 C1 Mo1 72.4(2) . . ? C1 C2 C3 107.1(4) . . ? C1 C2 Mo1 72.0(2) . . ? C3 C2 Mo1 73.4(2) . . ? C4 C3 C2 108.0(4) . . ? C4 C3 Mo1 73.0(2) . . ? C2 C3 Mo1 71.3(2) . . ? C3 C4 C5 110.1(4) . . ? C3 C4 Mo1 73.4(2) . . ? C5 C4 Mo1 72.0(2) . . ? C4 C5 C1 107.4(4) . . ? C4 C5 Mo1 73.2(2) . . ? C1 C5 Mo1 72.0(2) . . ? C7 C6 C14 145.1(3) . . ? C7 C6 Mo1 70.7(2) . . ? C14 C6 Mo1 144.1(2) . . ? C6 C7 C8 145.8(3) . . ? C6 C7 Mo1 71.8(2) . . ? C8 C7 Mo1 142.2(2) . . ? C13 C8 C9 119.4(3) . . ? C13 C8 C7 121.1(3) . . ? C9 C8 C7 119.5(3) . . ? C10 C9 C8 119.0(3) . . ? C11 C10 C9 121.2(4) . . ? C10 C11 C12 119.9(3) . . ? C11 C12 C13 120.5(4) . . ? C12 C13 C8 119.9(3) . . ? C15 C14 C19 118.9(3) . . ? C15 C14 C6 120.5(3) . . ? C19 C14 C6 120.6(3) . . ? C16 C15 C14 120.6(3) . . ? C17 C16 C15 120.2(3) . . ? C16 C17 C18 119.8(3) . . ? C17 C18 C19 120.8(3) . . ? C18 C19 C14 119.6(3) . . ? _refine_diff_density_max 0.256 _refine_diff_density_min -0.217 _refine_diff_density_rms 0.056