# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1608 data_global # 1. SUBMISSION DETAILS _publ_contact_author ; Prof. Dr. Helmut Fischer Universit\"at Konstanz Fakult\"at f\"ur Chemie Fach M727 D-78457 Konstanz Bundesrepublik Deutschland ; _publ_contact_author_phone 07531-88-2783 _publ_contact_author_fax 07531-88-3136 _publ_contact_author_email hfischer@dg6.chemie.uni-konstanz.de _publ_requested_journal 'J. Chem. Soc., Chemical Communications' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission (1 compound) for structural data deposition. We are awaiting a notice about the assigned CSD number. ; # 2. TITLE AND AUTHOR LIST _publ_section_title ; Novel hepta-coordinated molybdenum(II) and tungsten(II) carbene complexes by oxidative decarbonylation of Mo(0) and W(0) carbene complexes ; loop_ _publ_author_name _publ_author_address 'Fischer, Helmut' ; Universit\"at Konstanz Fakult\"at f\"ur Chemie Fach M727 D-78457 Konstanz Bundesrepublik Deutschland ; 'J\"ager, Monika' ; Universit\"at Konstanz Fakult\"at f\"ur Chemie Fach M727 D-78457 Konstanz Bundesrepublik Deutschland ; 'Stumpf, R\"udiger' ; Universit\"at Konstanz Fakult\"at f\"ur Chemie Fach M727 D-78457 Konstanz Bundesrepublik Deutschland ; 'Troll, Carsten' ; Universit\"at Konstanz Fakult\"at f\"ur Chemie Fach M727 D-78457 Konstanz Bundesrepublik Deutschland ; 'Fischer, Helmut' ; Universit\"at Konstanz Fakult\"at f\"ur Chemie Fach M727 D-78457 Konstanz Bundesrepublik Deutschland ; #----------------------------------------------------------------------- data_RSC _audit_creation_date 10-03-00 _audit_creation_method 'CIFEX (AG Fischer, 1994)' _chemical_name_systematic ; Tricarbonyl(dicloro){O,C-[methoxy(o-methoxyphenyl)carbene]}tungsten ; _chemical_formula_moiety 'C13 H12 Cl4 O5 W' _chemical_formula_sum 'C13 H12 Cl4 O5 W' _chemical_formula_weight 573.9 _chemical_melting_point '80 (decomp)' _computing_data_collection 'Siemens P3/V software 1989' _computing_structure_solution 'Siemens SHELXTL PLUS (VMS) 1990' _computing_structure_refinement 'Siemens SHELXTL PLUS (VMS) 1990' _cell_length_a 9.567(6) _cell_length_b 11.994(6) _cell_length_c 15.986(5) _cell_angle_alpha 90 _cell_angle_beta 100.57(4) _cell_angle_gamma 90 _cell_volume 1803.3(15) _cell_formula_units_Z 4 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, 1/2+y, 1/2-z' '-x, -y, -z' 'x, 1/2-y, 1/2+z' _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 2.114 _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 7.160 _exptl_absorpt_correction_type 'Semi-empirical' _exptl_absorpt_correction_T_min 0.1318 _exptl_absorpt_correction_T_max 0.1963 _diffrn_special_details ; Scan speed variable; 2.00 to 29.30\% per min in \w. \w scan range 0.70\%. Background measurement: Stationary crystal and stationary counter at beginning and end of scan, each for 25.0% of total scan time. ; _diffrn_ambient_temperature 300 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine focus X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens R3m/V diffractometer' _diffrn_measurement_method wyckoff _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4391 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.0 _diffrn_reflns_theta_max 27.0 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.002 0.002 'International Tables Vol IV Table 2.3.1' 'H' 'H' 0.000 0.000 'International Tables Vol IV Table 2.3.1' 'Cl' 'Cl' 0.132 0.159 'International Tables Vol IV Table 2.3.1' 'O' 'O' 0.008 0.006 'International Tables Vol IV Table 2.3.1' 'W' 'W' -1.421 6.872 'International Tables Vol IV Table 2.3.1' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_special_details ; Refinement uses F of all reflections obeying the _reflns_observed_criterion. Minimized quantity: \Sw(F~o~-F~c~)^2^. All residuals are based on F. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/(\s^2^(F) + 0.00030 F^2^)' _refine_ls_hydrogen_treatment 'riding with fixed isotropic U' _refine_ls_number_reflns 2782 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.058 _refine_ls_R_factor_obs 0.034 _refine_ls_wR_factor_all 0.041 _refine_ls_wR_factor_obs 0.037 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.168 _refine_ls_shift/esd_max 0.0008 _refine_ls_shift/esd_mean 0.0002 _refine_diff_density_min -1.089 _refine_diff_density_max 1.229 _reflns_limit_h_min 0 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 15 _reflns_limit_l_min -20 _reflns_limit_l_max 20 _reflns_number_total 3949 _reflns_number_observed 2782 _reflns_observed_criterion 'reflns observed if F > 4.0 \s(F)' 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 W1 W 0.2507(1) 0.2430(1) 0.0939(1) 0.027(1) Uani 1 d . Cl1 Cl 0.3071(3) 0.1987(2) 0.2481(1) 0.043(1) Uani 1 d . Cl2 Cl 0.1208(2) 0.4053(2) 0.1379(1) 0.039(1) Uani 1 d . C1 C 0.3311(10) 0.0882(6) 0.0954(5) 0.041(3) Uani 1 d . O1 O 0.3750(8) 0.0000(4) 0.0968(4) 0.057(2) Uani 1 d . C2 C 0.0771(9) 0.1491(6) 0.0742(6) 0.045(3) Uani 1 d . O2 O -0.0221(7) 0.0962(5) 0.0624(5) 0.068(3) Uani 1 d . C3 C 0.1421(8) 0.2950(6) -0.0185(5) 0.034(2) Uani 1 d . O3 O 0.0755(6) 0.3234(5) -0.0815(4) 0.052(2) Uani 1 d . C4 C 0.3776(8) 0.2255(5) -0.0020(5) 0.028(2) Uani 1 d . O4 O 0.3667(6) 0.1626(4) -0.0700(3) 0.035(2) Uani 1 d . C31 C 0.2531(8) 0.0839(6) -0.0981(5) 0.042(3) Uani 1 d . C5 C 0.5038(7) 0.2948(6) 0.0068(4) 0.028(2) Uani 1 d . C6 C 0.5974(8) 0.2924(6) -0.0518(5) 0.035(2) Uani 1 d . C7 C 0.7166(8) 0.3574(6) -0.0383(5) 0.041(3) Uani 1 d . C8 C 0.7434(8) 0.4293(6) 0.0305(5) 0.039(3) Uani 1 d . C9 C 0.6520(8) 0.4348(6) 0.0888(5) 0.035(2) Uani 1 d . C10 C 0.5338(7) 0.3674(5) 0.0753(4) 0.028(2) Uani 1 d . O5 O 0.4350(5) 0.3625(4) 0.1285(3) 0.032(2) Uani 1 d . C11 C 0.4621(9) 0.4331(7) 0.2043(5) 0.045(3) Uani 1 d . C100 C -0.1245(10) 0.2574(8) 0.2363(6) 0.059(3) Uani 1 d . Cl11 Cl -0.1322(3) 0.3683(2) 0.3048(2) 0.074(1) Uani 1 d . Cl12 Cl -0.2832(3) 0.1794(2) 0.2208(2) 0.076(1) Uani 1 d . H31A H 0.2674(8) 0.0480(6) -0.1495(5) 0.080(0) Uiso 1 calc R H31B H 0.2517(8) 0.0287(6) -0.0547(5) 0.080(0) Uiso 1 calc R H31C H 0.1642(8) 0.1232(6) -0.1084(5) 0.080(0) Uiso 1 calc R H6A H 0.5779(8) 0.2445(6) -0.1006(5) 0.080(0) Uiso 1 calc R H7A H 0.7825(8) 0.3537(6) -0.0768(5) 0.080(0) Uiso 1 calc R H8A H 0.8258(8) 0.4765(6) 0.0384(5) 0.080(0) Uiso 1 calc R H9A H 0.6716(8) 0.4830(6) 0.1376(5) 0.080(0) Uiso 1 calc R H11A H 0.5471(9) 0.4753(7) 0.2035(5) 0.080(0) Uiso 1 calc R H11B H 0.3836(9) 0.4831(7) 0.2037(5) 0.080(0) Uiso 1 calc R H11C H 0.4743(9) 0.3881(7) 0.2548(5) 0.080(0) Uiso 1 calc R H10A H -0.0471(10) 0.2097(8) 0.2605(6) 0.080(0) Uiso 1 calc R H10B H -0.1066(10) 0.2843(8) 0.1827(6) 0.080(0) 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 W1 0.026(1) 0.027(1) 0.030(1) -0.003(1) 0.011(1) -0.001(1) Cl1 0.061(1) 0.043(1) 0.028(1) 0.004(1) 0.012(1) 0.003(1) Cl2 0.033(1) 0.038(1) 0.048(1) 0.002(1) 0.014(1) -0.005(1) C1 0.060(6) 0.040(4) 0.025(4) -0.002(4) 0.015(4) -0.002(3) O1 0.084(5) 0.035(3) 0.059(4) 0.020(3) 0.028(4) 0.011(3) C2 0.046(5) 0.033(4) 0.061(6) -0.007(4) 0.027(5) -0.008(4) O2 0.047(4) 0.064(4) 0.100(6) -0.028(3) 0.031(4) -0.016(4) C3 0.033(4) 0.033(3) 0.038(4) -0.004(3) 0.011(3) -0.012(3) O3 0.045(4) 0.052(3) 0.053(4) 0.003(3) -0.009(3) -0.002(3) C4 0.026(4) 0.029(3) 0.029(4) -0.001(3) 0.007(3) 0.002(3) O4 0.040(3) 0.036(3) 0.031(3) -0.013(2) 0.014(2) -0.009(2) C31 0.046(5) 0.040(4) 0.042(4) -0.015(4) 0.014(4) -0.009(4) C5 0.026(3) 0.030(3) 0.028(3) 0.001(3) 0.008(3) 0.002(3) C6 0.041(4) 0.036(4) 0.033(4) -0.001(3) 0.014(3) 0.001(3) C7 0.037(5) 0.048(4) 0.042(5) -0.004(4) 0.020(4) 0.004(4) C8 0.033(4) 0.038(4) 0.046(5) -0.019(3) 0.004(4) 0.001(4) C9 0.032(4) 0.034(4) 0.040(4) -0.003(3) 0.006(3) 0.000(3) C10 0.023(3) 0.031(3) 0.033(4) -0.001(3) 0.008(3) 0.004(3) O5 0.029(3) 0.033(2) 0.033(3) -0.003(2) 0.006(2) -0.013(2) C11 0.044(5) 0.052(5) 0.039(5) -0.005(4) 0.008(4) -0.020(4) C100 0.059(5) 0.071(6) 0.046(5) 0.018(6) 0.006(4) -0.009(5) Cl11 0.059(2) 0.079(2) 0.077(2) 0.016(1) -0.004(1) -0.027(1) Cl12 0.099(2) 0.055(1) 0.078(2) -0.012(1) 0.023(2) 0.008(1) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 Cl1 2.483(2) . . ? W1 Cl2 2.480(2) . . ? W1 C1 2.008(8) . . ? W1 C2 1.983(8) . . ? W1 C3 2.003(7) . . ? W1 C4 2.133(8) . . ? W1 O5 2.261(5) . . ? C1 O1 1.137(10) . . ? C2 O2 1.129(11) . . ? C3 O3 1.140(9) . . ? C4 O4 1.312(8) . . ? C4 C5 1.452(10) . . ? O4 C31 1.447(9) . . ? C5 C6 1.410(11) . . ? C5 C10 1.388(9) . . ? C6 C7 1.365(11) . . ? C7 C8 1.384(11) . . ? C8 C9 1.392(12) . . ? C9 C10 1.375(10) . . ? C10 O5 1.383(9) . . ? O5 C11 1.461(9) . . ? C100 Cl11 1.733(10) . . ? C100 Cl12 1.761(10) . . ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 W1 Cl2 85.1(1) . . . ? Cl1 W1 C1 77.1(2) . . . ? Cl2 W1 C1 158.9(3) . . . ? Cl1 W1 C2 93.4(3) . . . ? Cl2 W1 C2 92.4(3) . . . ? C1 W1 C2 77.6(3) . . . ? Cl1 W1 C3 160.0(2) . . . ? Cl2 W1 C3 78.8(2) . . . ? C1 W1 C3 115.7(3) . . . ? C2 W1 C3 75.7(3) . . . ? Cl1 W1 C4 130.1(2) . . . ? Cl2 W1 C4 131.5(2) . . . ? C1 W1 C4 69.5(3) . . . ? C2 W1 C4 113.6(3) . . . ? C3 W1 C4 69.9(3) . . . ? Cl1 W1 O5 82.8(1) . . . ? Cl2 W1 O5 80.9(1) . . . ? C1 W1 O5 107.7(3) . . . ? C2 W1 O5 172.6(3) . . . ? C3 W1 O5 106.0(2) . . . ? C4 W1 O5 73.6(2) . . . ? W1 C1 O1 179.0(8) . . . ? W1 C2 O2 179.5(6) . . . ? W1 C3 O3 177.3(7) . . . ? W1 C4 O4 133.1(5) . . . ? W1 C4 C5 116.5(5) . . . ? O4 C4 C5 110.4(6) . . . ? C4 O4 C31 124.9(6) . . . ? C4 C5 C6 122.8(6) . . . ? C4 C5 C10 118.9(7) . . . ? C6 C5 C10 118.2(6) . . . ? C5 C6 C7 119.8(7) . . . ? C6 C7 C8 120.6(8) . . . ? C7 C8 C9 121.0(7) . . . ? C8 C9 C10 117.8(7) . . . ? C5 C10 C9 122.5(7) . . . ? C5 C10 O5 113.1(6) . . . ? C9 C10 O5 124.3(6) . . . ? W1 O5 C10 117.8(4) . . . ? W1 O5 C11 125.6(5) . . . ? C10 O5 C11 116.6(5) . . . ? Cl11 C100 Cl12 111.2(6) . . . ?