Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_name 'Prof. Judith A. K. Howard' _journal_name_full 'J.Chem.Soc.,Dalton Trans.' _journal_coden_Cambridge 0186 _publ_contact_author ; Prof. Judith A. K. Howard Department of Chemistry Durham University DURHAM DH1 3LE UK ; _publ_contact_author_phone '+44 191 3744647' _publ_contact_author_fax '+44 191 3844737' _publ_contact_author_email J.A.K.Howard@durham.ac.uk #====================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and Structure of a Series of Tungsten (II) and Tungsten (VI) Diynyl and Diyndiyl Complexes ; loop_ _publ_author_name 'Rachel L. Roberts' 'Horst Puschmann' 'Judith A.K. Howard' 'John H. Yamamoto' 'Arthur J. Carty' ; P.J.Low ; #============================================ data_01srv144Compound1 _database_code_CSD 196749 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ;(1,2,3,4,5-pentamethyl cyclopentadienyl)(tricarbonyl)tungsten(buta-1,3-diynyl) ; _chemical_melting_point ? _chemical_formula_moiety 'C17 H16 O3 W' _chemical_formula_sum 'C17 H16 O3 W' _chemical_formula_weight 452.15 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 19.1104(5) _cell_length_b 10.8040(3) _cell_length_c 7.4292(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1533.90(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7101 _cell_measurement_theta_min 2.166 _cell_measurement_theta_max 27.463 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.958 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 7.537 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.308 _exptl_absorpt_correction_T_max 0.323 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998)' _exptl_special_details ; The data collection nominally covered full sphere of reciprocal space, by a combination of 5 sets of \w scans; each set at different \f and/or 2\q angles and each scan (20 sec exposure) covering 0.3\% in \w. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 120(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 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 16022 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.50 _reflns_number_total 1853 _reflns_number_gt 1587 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART version 5.060 (Bruker, 1999)' _computing_cell_refinement 'SMART version 5.060 (Bruker, 1999)' _computing_data_reduction 'SAINT version 6.02A (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL version 5.10 (Bruker, 1997)' _computing_publication_material 'SHELXTL version 5.10 (Bruker, 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0110P)^2^+3.9836P] 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 1853 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0300 _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_ref 0.0446 _refine_ls_wR_factor_gt 0.0427 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.001 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.402011(10) 0.2500 0.75942(2) 0.01522(6) Uani 1 2 d S . . O21 O 0.42472(15) -0.0019(3) 0.5536(4) 0.0325(7) Uani 1 1 d . . . O22 O 0.5668(2) 0.2500 0.7217(6) 0.0318(9) Uani 1 2 d S . . C1 C 0.3246(3) 0.2500 0.5507(7) 0.0217(11) Uani 1 2 d S . . C2 C 0.2783(3) 0.2500 0.4480(7) 0.0197(11) Uani 1 2 d S . . C3 C 0.2186(3) 0.2500 0.3336(7) 0.0238(12) Uani 1 2 d S . . C4 C 0.1673(3) 0.2500 0.2377(9) 0.0290(12) Uani 1 2 d S . . H4 H 0.123(3) 0.2500 0.154(9) 0.035 Uiso 1 2 d S . . C01 C 0.4146(3) 0.2500 1.0772(7) 0.0182(10) Uani 1 2 d S . . C02 C 0.37497(19) 0.1424(3) 1.0264(5) 0.0166(7) Uani 1 1 d . . . C03 C 0.31121(18) 0.1827(3) 0.9443(5) 0.0166(7) Uani 1 1 d . . . C11 C 0.4818(3) 0.2500 1.1793(8) 0.0225(12) Uani 1 2 d S . . H11A H 0.468(3) 0.2500 1.303(8) 0.022(15) Uiso 1 2 d S . . H11B H 0.510(2) 0.182(4) 1.155(6) 0.032(12) Uiso 1 1 d . . . C12 C 0.3930(2) 0.0117(4) 1.0746(5) 0.0217(8) Uani 1 1 d . . . H12A H 0.379(2) -0.007(4) 1.183(6) 0.033 Uiso 1 1 d . . . H12B H 0.444(2) 0.002(4) 1.086(6) 0.033 Uiso 1 1 d . . . H12C H 0.372(2) -0.044(4) 0.991(6) 0.033 Uiso 1 1 d . . . C13 C 0.2519(2) 0.1013(4) 0.8859(6) 0.0234(8) Uani 1 1 d . . . H13A H 0.264(2) 0.029(4) 0.840(6) 0.035 Uiso 1 1 d . . . H13B H 0.220(2) 0.143(4) 0.808(6) 0.035 Uiso 1 1 d . . . H13C H 0.223(2) 0.085(4) 0.980(6) 0.035 Uiso 1 1 d . . . C21 C 0.41845(19) 0.0916(4) 0.6234(5) 0.0206(8) Uani 1 1 d . . . C22 C 0.5075(2) 0.2500 0.7385(7) 0.0154(9) Uani 1 2 d S . . 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 W1 0.01541(10) 0.01615(10) 0.01410(10) 0.000 0.00102(9) 0.000 O21 0.0299(16) 0.0260(16) 0.0416(17) -0.0088(14) 0.0036(13) -0.0003(13) O22 0.0189(19) 0.027(2) 0.049(3) 0.000 0.0036(19) 0.000 C1 0.027(3) 0.011(3) 0.027(3) 0.000 0.009(2) 0.000 C2 0.031(3) 0.013(2) 0.015(2) 0.000 0.006(2) 0.000 C3 0.030(3) 0.017(3) 0.024(3) 0.000 0.003(2) 0.000 C4 0.025(3) 0.029(3) 0.033(3) 0.000 0.001(3) 0.000 C01 0.019(3) 0.018(2) 0.017(2) 0.000 0.0046(19) 0.000 C02 0.0171(17) 0.0163(17) 0.0165(16) -0.0013(14) 0.0053(14) 0.0003(14) C03 0.0174(18) 0.0150(17) 0.0173(16) -0.0005(14) 0.0044(13) -0.0014(14) C11 0.020(3) 0.028(3) 0.020(3) 0.000 0.000(2) 0.000 C12 0.022(2) 0.0184(18) 0.0252(19) 0.0037(15) 0.0030(16) 0.0013(16) C13 0.017(2) 0.021(2) 0.032(2) -0.0023(17) 0.0015(16) -0.0037(16) C21 0.0150(19) 0.026(2) 0.0206(17) -0.0033(15) 0.0029(13) -0.0013(15) C22 0.015(2) 0.0106(19) 0.021(2) 0.000 0.001(2) 0.000 _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 W1 C21 2.012(4) . ? W1 C21 2.012(4) 7_565 ? W1 C22 2.023(5) . ? W1 C1 2.143(6) . yes W1 C03 2.329(3) 7_565 ? W1 C03 2.329(3) . ? W1 C02 2.357(3) 7_565 ? W1 C02 2.357(3) . ? W1 C01 2.373(5) . ? O21 C21 1.141(5) . ? O22 C22 1.140(6) . ? C1 C2 1.169(8) . yes C2 C3 1.422(8) . yes C3 C4 1.212(8) . yes C01 C02 1.438(5) . ? C01 C02 1.438(5) 7_565 ? C01 C11 1.492(7) . ? C02 C03 1.431(5) . ? C02 C12 1.496(5) . ? C03 C03 1.453(7) 7_565 ? C03 C13 1.500(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 C21 W1 C21 116.5(2) . 7_565 yes C21 W1 C22 78.79(12) . . yes C21 W1 C22 78.79(12) 7_565 . ? C21 W1 C1 75.20(12) . . yes C21 W1 C1 75.20(12) 7_565 . yes C22 W1 C1 129.3(2) . . ? C21 W1 C03 132.67(13) . 7_565 ? C21 W1 C03 98.46(13) 7_565 7_565 ? C22 W1 C03 142.02(15) . 7_565 ? C1 W1 C03 84.95(16) . 7_565 ? C21 W1 C03 98.46(13) . . ? C21 W1 C03 132.67(13) 7_565 . ? C22 W1 C03 142.02(15) . . ? C1 W1 C03 84.95(16) . . ? C03 W1 C03 36.36(17) 7_565 . ? C21 W1 C02 151.24(14) . 7_565 ? C21 W1 C02 92.14(13) 7_565 7_565 ? C22 W1 C02 106.46(15) . 7_565 ? C1 W1 C02 117.22(15) . 7_565 ? C03 W1 C02 35.56(12) 7_565 7_565 ? C03 W1 C02 59.62(12) . 7_565 ? C21 W1 C02 92.14(13) . . ? C21 W1 C02 151.24(14) 7_565 . ? C22 W1 C02 106.46(15) . . ? C1 W1 C02 117.22(15) . . ? C03 W1 C02 59.62(12) 7_565 . ? C03 W1 C02 35.56(12) . . ? C02 W1 C02 59.13(17) 7_565 . ? C21 W1 C01 118.94(11) . . ? C21 W1 C01 118.94(11) 7_565 . ? C22 W1 C01 88.61(19) . . ? C1 W1 C01 142.13(19) . . ? C03 W1 C01 59.25(14) 7_565 . ? C03 W1 C01 59.25(14) . . ? C02 W1 C01 35.39(11) 7_565 . ? C02 W1 C01 35.39(11) . . ? C2 C1 W1 174.5(5) . . yes C1 C2 C3 175.9(6) . . yes C4 C3 C2 179.4(6) . . yes C02 C01 C02 108.0(4) . 7_565 ? C02 C01 C11 125.9(2) . . ? C02 C01 C11 125.9(2) 7_565 . ? C02 C01 W1 71.7(2) . . ? C02 C01 W1 71.7(2) 7_565 . ? C11 C01 W1 126.4(4) . . ? C03 C02 C01 108.3(3) . . ? C03 C02 C12 125.9(3) . . ? C01 C02 C12 125.4(3) . . ? C03 C02 W1 71.17(19) . . ? C01 C02 W1 72.9(2) . . ? C12 C02 W1 128.0(2) . . ? C02 C03 C03 107.7(2) . 7_565 ? C02 C03 C13 126.0(3) . . ? C03 C03 C13 125.9(2) 7_565 . ? C02 C03 W1 73.27(19) . . ? C03 C03 W1 71.82(8) 7_565 . ? C13 C03 W1 125.2(2) . . ? O21 C21 W1 175.5(3) . . ? O22 C22 W1 178.1(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.978 _refine_diff_density_min -1.418 _refine_diff_density_rms 0.122 #===END data_02srv001Compound2 _database_code_CSD 196751 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; bis((1,2,3,4,5-pentamethyl cyclopentadienyl)(tricarbonyl)tungsten) buta-1,3-diyn-1,4-diyl ; _chemical_melting_point ? _chemical_formula_moiety 'C30 H30 O6 W2, 2(C H2 Cl2)' _chemical_formula_sum 'C32 H34 Cl4 O6 W2' _chemical_formula_weight 1024.09 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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' _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 6.6947(7) _cell_length_b 11.4966(11) _cell_length_c 11.6466(11) _cell_angle_alpha 88.999(2) _cell_angle_beta 84.614(2) _cell_angle_gamma 84.981(2) _cell_volume 888.98(15) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5539 _cell_measurement_theta_min 2.489 _cell_measurement_theta_max 38.257 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas Not_measured _exptl_crystal_density_diffrn 1.913 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 490 _exptl_absorpt_coefficient_mu 6.805 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6958 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998)' _exptl_special_details ; The data collection nominally covered full sphere of reciprocal Space, by a combination of 5 sets of \w scans each set at different \f and/or 2\q angles and each scan (20s exposure) covering 0.3\% in \w. Crystal to detector distance 4.85 cm. ; _diffrn_ambient_temperature 120(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 'Bruker SMART CCD 6K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 10090 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 28.53 _reflns_number_total 4448 _reflns_number_gt 4388 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0000P)^2^+9.0986P] 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 4448 _refine_ls_number_parameters 176 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0943 _refine_ls_wR_factor_gt 0.0923 _refine_ls_goodness_of_fit_ref 1.199 _refine_ls_restrained_S_all 1.199 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.59271(5) 0.74894(3) 0.72516(3) 0.01340(8) Uani 1 1 d . . . O21 O 0.3211(11) 0.5782(7) 0.8688(7) 0.0348(16) Uani 1 1 d . . . O22 O 0.2859(10) 0.9298(7) 0.8625(7) 0.039(2) Uani 1 1 d . . . O23 O 0.3961(12) 0.8868(7) 0.5231(7) 0.0367(17) Uani 1 1 d . . . C1 C 0.5426(11) 0.6191(7) 0.6056(7) 0.0183(14) Uani 1 1 d . . . C2 C 0.5145(10) 0.5428(6) 0.5381(7) 0.0177(15) Uani 1 1 d . . . C01 C 0.8814(11) 0.8498(7) 0.7135(7) 0.0154(7) Uani 1 1 d . . . C02 C 0.9308(11) 0.7449(7) 0.6451(7) 0.0154(7) Uani 1 1 d . . . C03 C 0.9137(11) 0.6475(7) 0.7274(7) 0.0154(7) Uani 1 1 d . . . C04 C 0.8584(11) 0.6918(7) 0.8409(7) 0.0154(7) Uani 1 1 d . . . C05 C 0.8370(10) 0.8175(6) 0.8300(7) 0.0154(7) Uani 1 1 d . . . C11 C 0.8975(13) 0.9736(7) 0.6679(8) 0.0237(17) Uani 1 1 d . . . H11A H 1.0350 0.9952 0.6723 0.036 Uiso 1 1 calc R . . H11B H 0.8026 1.0275 0.7146 0.036 Uiso 1 1 calc R . . H11C H 0.8653 0.9779 0.5875 0.036 Uiso 1 1 calc R . . C12 C 0.9971(13) 0.7327(8) 0.5225(7) 0.0215(16) Uani 1 1 d . . . H12A H 1.1439 0.7330 0.5111 0.032 Uiso 1 1 calc R . . H12B H 0.9345 0.7979 0.4795 0.032 Uiso 1 1 calc R . . H12C H 0.9573 0.6589 0.4947 0.032 Uiso 1 1 calc R . . C13 C 0.9706(14) 0.5234(7) 0.6953(9) 0.0248(18) Uani 1 1 d . . . H13A H 1.1139 0.5040 0.7040 0.037 Uiso 1 1 calc R . . H13B H 0.9451 0.5119 0.6149 0.037 Uiso 1 1 calc R . . H13C H 0.8902 0.4725 0.7457 0.037 Uiso 1 1 calc R . . C14 C 0.8375(14) 0.6244(9) 0.9508(8) 0.0271(19) Uani 1 1 d . . . H14A H 0.9689 0.6120 0.9819 0.041 Uiso 1 1 calc R . . H14B H 0.7881 0.5487 0.9365 0.041 Uiso 1 1 calc R . . H14C H 0.7418 0.6681 1.0065 0.041 Uiso 1 1 calc R . . C15 C 0.7962(12) 0.9006(8) 0.9312(8) 0.0238(16) Uani 1 1 d . . . H15A H 0.9239 0.9162 0.9601 0.036 Uiso 1 1 calc R . . H15B H 0.7107 0.8653 0.9927 0.036 Uiso 1 1 calc R . . H15C H 0.7275 0.9741 0.9059 0.036 Uiso 1 1 calc R . . C21 C 0.4110(13) 0.6446(8) 0.8148(7) 0.0211(16) Uani 1 1 d . . . C22 C 0.3988(13) 0.8656(8) 0.8127(8) 0.0270(19) Uani 1 1 d . . . C23 C 0.4644(13) 0.8358(7) 0.6002(8) 0.0221(17) Uani 1 1 d . . . C1S C 0.468(3) 0.7066(13) 0.2706(13) 0.061(4) Uani 1 1 d . . . H1SA H 0.3848 0.7317 0.3422 0.073 Uiso 1 1 calc R . . H1SB H 0.5051 0.6217 0.2772 0.073 Uiso 1 1 calc R . . Cl1 Cl 0.3234(5) 0.7326(3) 0.1532(3) 0.0553(8) Uani 1 1 d . . . Cl2 Cl 0.6854(7) 0.7800(5) 0.2575(3) 0.0712(12) Uani 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 W1 0.01195(12) 0.01338(14) 0.01476(14) -0.00506(8) 0.00020(9) -0.00104(9) O21 0.031(4) 0.041(4) 0.034(4) 0.007(3) 0.000(3) -0.013(3) O22 0.025(3) 0.043(4) 0.049(5) -0.027(4) 0.001(3) 0.004(3) O23 0.037(4) 0.032(4) 0.043(4) 0.009(3) -0.018(3) -0.005(3) C1 0.017(3) 0.017(4) 0.021(4) 0.000(3) -0.003(3) -0.001(3) C2 0.014(3) 0.018(4) 0.021(4) -0.002(3) 0.000(3) -0.001(3) C01 0.0122(14) 0.0153(17) 0.0195(17) -0.0074(13) -0.0030(12) -0.0020(12) C02 0.0122(14) 0.0153(17) 0.0195(17) -0.0074(13) -0.0030(12) -0.0020(12) C03 0.0122(14) 0.0153(17) 0.0195(17) -0.0074(13) -0.0030(12) -0.0020(12) C04 0.0122(14) 0.0153(17) 0.0195(17) -0.0074(13) -0.0030(12) -0.0020(12) C05 0.0122(14) 0.0153(17) 0.0195(17) -0.0074(13) -0.0030(12) -0.0020(12) C11 0.025(4) 0.012(4) 0.034(5) 0.003(3) -0.002(3) -0.005(3) C12 0.022(4) 0.028(4) 0.015(4) -0.009(3) 0.001(3) -0.005(3) C13 0.021(4) 0.014(4) 0.039(5) -0.006(3) -0.004(4) 0.000(3) C14 0.027(4) 0.030(5) 0.023(4) 0.014(4) 0.000(3) -0.002(4) C15 0.025(4) 0.026(4) 0.021(4) -0.013(3) 0.001(3) -0.003(3) C21 0.017(4) 0.026(4) 0.020(4) -0.006(3) 0.004(3) -0.007(3) C22 0.022(4) 0.027(4) 0.032(5) -0.014(4) 0.000(3) 0.000(3) C23 0.019(4) 0.014(4) 0.034(5) -0.004(3) -0.002(3) -0.005(3) C1S 0.092(12) 0.046(8) 0.044(8) 0.005(6) 0.008(7) -0.013(7) Cl1 0.0535(18) 0.0522(18) 0.060(2) -0.0024(15) -0.0012(15) -0.0061(15) Cl2 0.075(2) 0.104(3) 0.0388(18) 0.0019(19) -0.0093(17) -0.028(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 W1 C23 1.971(9) . ? W1 C21 1.995(8) . ? W1 C22 2.005(8) . ? W1 C1 2.127(7) . yes W1 C05 2.328(7) . ? W1 C01 2.331(7) . ? W1 C03 2.356(8) . ? W1 C02 2.363(8) . ? W1 C04 2.372(8) . ? O21 C21 1.154(11) . ? O22 C22 1.135(11) . ? O23 C23 1.171(12) . ? C1 C2 1.226(10) . yes C2 C2 1.376(14) 2_666 yes C01 C05 1.411(11) . ? C01 C02 1.454(10) . ? C01 C11 1.520(11) . ? C02 C12 1.460(11) . ? C02 C03 1.466(11) . ? C03 C04 1.429(11) . ? C03 C13 1.489(11) . ? C04 C05 1.444(10) . ? C04 C14 1.487(11) . ? C05 C15 1.520(9) . ? C1S Cl2 1.741(17) . ? C1S Cl1 1.752(16) . ? 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 C23 W1 C21 113.3(4) . . yes C23 W1 C22 77.8(4) . . yes C21 W1 C22 78.6(4) . . yes C23 W1 C1 75.1(3) . . yes C21 W1 C1 75.5(3) . . ? C22 W1 C1 130.6(3) . . ? C23 W1 C05 125.0(3) . . ? C21 W1 C05 114.2(3) . . ? C22 W1 C05 85.9(3) . . ? C1 W1 C05 143.2(3) . . ? C23 W1 C01 96.4(3) . . ? C21 W1 C01 148.8(3) . . ? C22 W1 C01 99.6(3) . . ? C1 W1 C01 123.7(3) . . ? C05 W1 C01 35.3(3) . . ? C23 W1 C03 130.9(3) . . ? C21 W1 C03 103.6(3) . . ? C22 W1 C03 142.8(3) . . ? C1 W1 C03 84.5(3) . . ? C05 W1 C03 58.9(2) . . ? C01 W1 C03 59.4(3) . . ? C23 W1 C02 98.4(3) . . ? C21 W1 C02 139.0(3) . . ? C22 W1 C02 135.4(3) . . ? C1 W1 C02 89.2(3) . . ? C05 W1 C02 59.7(3) . . ? C01 W1 C02 36.1(2) . . ? C03 W1 C02 36.2(3) . . ? C23 W1 C04 155.4(3) . . ? C21 W1 C04 91.3(3) . . ? C22 W1 C04 108.5(3) . . ? C1 W1 C04 113.3(3) . . ? C05 W1 C04 35.8(3) . . ? C01 W1 C04 59.4(3) . . ? C03 W1 C04 35.2(3) . . ? C02 W1 C04 60.0(3) . . ? C2 C1 W1 178.9(8) . . yes C1 C2 C2 179.3(10) . 2_666 yes C05 C01 C02 109.1(7) . . ? C05 C01 C11 125.8(7) . . ? C02 C01 C11 124.8(7) . . ? C05 C01 W1 72.3(4) . . ? C02 C01 W1 73.1(4) . . ? C11 C01 W1 125.8(6) . . ? C01 C02 C12 129.8(8) . . ? C01 C02 C03 105.3(7) . . ? C12 C02 C03 124.9(8) . . ? C01 C02 W1 70.8(4) . . ? C12 C02 W1 124.9(6) . . ? C03 C02 W1 71.6(5) . . ? C04 C03 C02 109.6(7) . . ? C04 C03 C13 126.8(8) . . ? C02 C03 C13 123.1(8) . . ? C04 C03 W1 73.0(4) . . ? C02 C03 W1 72.1(5) . . ? C13 C03 W1 126.7(5) . . ? C03 C04 C05 106.6(7) . . ? C03 C04 C14 127.7(8) . . ? C05 C04 C14 125.6(7) . . ? C03 C04 W1 71.8(4) . . ? C05 C04 W1 70.5(4) . . ? C14 C04 W1 125.3(6) . . ? C01 C05 C04 109.4(6) . . ? C01 C05 C15 125.9(7) . . ? C04 C05 C15 124.4(8) . . ? C01 C05 W1 72.5(4) . . ? C04 C05 W1 73.8(4) . . ? C15 C05 W1 125.4(5) . . ? O21 C21 W1 173.9(8) . . ? O22 C22 W1 178.4(8) . . ? O23 C23 W1 177.1(8) . . ? Cl2 C1S Cl1 112.7(8) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.53 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 2.416 _refine_diff_density_min -2.950 _refine_diff_density_rms 0.208 #===END data_01srv159Compound3 _database_code_CSD 196750 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ;(1,2,3,4,5-pentamethyl cyclopentadienyl)(oxo- peroxo)tungsten(buta-1,3-diynyl) ; _chemical_melting_point ? _chemical_formula_moiety 'C14 H16 O3 W' _chemical_formula_sum 'C14 H16 O3 W' _chemical_formula_weight 416.12 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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 7.7790(3) _cell_length_b 13.8399(5) _cell_length_c 12.7350(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.2000(10) _cell_angle_gamma 90.00 _cell_volume 1357.04(9) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5031 _cell_measurement_theta_min 3.027 _cell_measurement_theta_max 28.477 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.037 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 8.509 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.296 _exptl_absorpt_correction_T_max 0.551 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 15600 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 28.48 _reflns_number_total 3424 _reflns_number_gt 3112 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART version 5.060 (Bruker, 1999)' _computing_cell_refinement 'SMART version 5.060 (Bruker, 1999)' _computing_data_reduction 'SAINT version 6.02A (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL version 5.10 (Bruker, 1997)' _computing_publication_material 'SHELXTL version 5.10 (Bruker, 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0148P)^2^+3.9895P] 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 3424 _refine_ls_number_parameters 167 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0277 _refine_ls_R_factor_gt 0.0233 _refine_ls_wR_factor_ref 0.0506 _refine_ls_wR_factor_gt 0.0493 _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_restrained_S_all 1.146 _refine_ls_shift/su_max 0.002 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.867293(18) 0.207952(10) 0.629470(11) 0.01432(5) Uani 1 1 d . . . O1 O 0.8639(4) 0.3009(2) 0.7193(2) 0.0264(6) Uani 1 1 d . . . O2 O 1.0642(5) 0.2250(2) 0.5548(3) 0.0366(8) Uani 1 1 d . . . O3 O 0.9067(5) 0.2705(3) 0.4996(3) 0.0361(8) Uani 1 1 d . . . C1 C 1.0396(5) 0.1158(3) 0.7228(3) 0.0193(7) Uani 1 1 d . . . C2 C 1.1365(5) 0.0640(3) 0.7812(3) 0.0188(7) Uani 1 1 d . . . C3 C 1.2404(5) 0.0027(3) 0.8492(3) 0.0209(8) Uani 1 1 d . . . C4 C 1.3295(6) -0.0507(3) 0.9061(4) 0.0269(9) Uani 1 1 d . . . H4 H 1.386(7) -0.085(4) 0.938(4) 0.033(15) Uiso 1 1 d . . . C01 C 0.5727(5) 0.1809(3) 0.6624(3) 0.0172(7) Uani 1 1 d . . . C02 C 0.6659(5) 0.0949(3) 0.6900(3) 0.0160(7) Uani 1 1 d . . . C03 C 0.7157(5) 0.0533(3) 0.5934(3) 0.0156(7) Uani 1 1 d . . . C04 C 0.6583(5) 0.1156(3) 0.5083(3) 0.0161(7) Uani 1 1 d . . . C05 C 0.5772(5) 0.1980(3) 0.5516(3) 0.0164(7) Uani 1 1 d . . . C11 C 0.4886(5) 0.2452(3) 0.7346(3) 0.0241(9) Uani 1 1 d . . . H11A H 0.3701 0.2226 0.7379 0.036 Uiso 1 1 calc R . . H11B H 0.4848 0.3115 0.7073 0.036 Uiso 1 1 calc R . . H11C H 0.5557 0.2436 0.8058 0.036 Uiso 1 1 calc R . . C12 C 0.6908(5) 0.0470(3) 0.7967(3) 0.0246(8) Uani 1 1 d . . . H12A H 0.5919 0.0045 0.8026 0.037 Uiso 1 1 calc R . . H12B H 0.6987 0.0965 0.8523 0.037 Uiso 1 1 calc R . . H12C H 0.7980 0.0089 0.8050 0.037 Uiso 1 1 calc R . . C13 C 0.7999(5) -0.0434(3) 0.5860(4) 0.0248(8) Uani 1 1 d . . . H13A H 0.7101 -0.0931 0.5711 0.037 Uiso 1 1 calc R . . H13B H 0.8730 -0.0580 0.6534 0.037 Uiso 1 1 calc R . . H13C H 0.8718 -0.0423 0.5288 0.037 Uiso 1 1 calc R . . C14 C 0.6804(5) 0.1024(3) 0.3945(3) 0.0228(8) Uani 1 1 d . . . H14A H 0.5841 0.0636 0.3586 0.034 Uiso 1 1 calc R . . H14B H 0.7905 0.0692 0.3902 0.034 Uiso 1 1 calc R . . H14C H 0.6810 0.1657 0.3601 0.034 Uiso 1 1 calc R . . C15 C 0.4925(6) 0.2809(3) 0.4879(3) 0.0256(8) Uani 1 1 d . . . H15A H 0.3716 0.2644 0.4613 0.038 Uiso 1 1 calc R . . H15B H 0.5551 0.2940 0.4278 0.038 Uiso 1 1 calc R . . H15C H 0.4954 0.3385 0.5329 0.038 Uiso 1 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 W1 0.01440(7) 0.01310(7) 0.01564(7) -0.00098(6) 0.00271(5) -0.00232(6) O1 0.0317(16) 0.0189(14) 0.0272(14) -0.0058(12) 0.0000(12) -0.0012(12) O2 0.0383(19) 0.0345(18) 0.0410(19) 0.0001(15) 0.0190(16) -0.0038(15) O3 0.0406(19) 0.0426(19) 0.0249(15) 0.0022(14) 0.0044(14) -0.0156(16) C1 0.0179(17) 0.0192(18) 0.0209(17) -0.0052(15) 0.0031(14) -0.0020(15) C2 0.0149(17) 0.0194(18) 0.0223(18) -0.0044(15) 0.0031(15) -0.0027(14) C3 0.0181(18) 0.0224(19) 0.0222(18) -0.0028(16) 0.0037(15) -0.0020(15) C4 0.025(2) 0.029(2) 0.026(2) 0.0039(19) 0.0022(18) 0.0047(19) C01 0.0157(17) 0.0179(17) 0.0182(17) -0.0042(14) 0.0036(14) -0.0036(14) C02 0.0156(17) 0.0165(17) 0.0159(16) -0.0001(13) 0.0025(14) -0.0054(13) C03 0.0124(16) 0.0145(16) 0.0195(17) -0.0036(14) 0.0015(13) -0.0034(13) C04 0.0134(16) 0.0179(17) 0.0165(16) -0.0038(14) 0.0002(13) -0.0025(14) C05 0.0155(16) 0.0162(16) 0.0171(16) -0.0008(14) 0.0014(13) 0.0009(14) C11 0.023(2) 0.027(2) 0.025(2) -0.0077(16) 0.0096(17) -0.0009(16) C12 0.024(2) 0.028(2) 0.0210(19) 0.0084(17) 0.0028(16) -0.0058(17) C13 0.0199(19) 0.0153(18) 0.038(2) -0.0032(17) 0.0015(17) 0.0008(15) C14 0.0232(19) 0.030(2) 0.0156(17) -0.0056(15) 0.0047(15) -0.0018(16) C15 0.025(2) 0.023(2) 0.027(2) 0.0037(17) 0.0002(16) 0.0056(17) _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 W1 O1 1.724(3) . yes W1 O2 1.929(3) . yes W1 O3 1.929(3) . yes W1 C1 2.093(4) . yes W1 C05 2.336(4) . ? W1 C01 2.417(4) . ? W1 C02 2.417(3) . ? W1 C04 2.438(4) . ? W1 C03 2.456(4) . ? O2 O3 1.465(5) . yes C1 C2 1.215(5) . yes C2 C3 1.387(6) . yes C3 C4 1.187(6) . yes C01 C02 1.412(5) . ? C01 C05 1.436(5) . ? C01 C11 1.495(5) . ? C02 C03 1.459(5) . ? C02 C12 1.499(5) . ? C03 C04 1.407(5) . ? C03 C13 1.499(5) . ? C04 C05 1.450(5) . ? C04 C14 1.495(5) . ? C05 C15 1.502(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 O1 W1 O2 108.92(15) . . yes O1 W1 O3 104.66(15) . . yes O2 W1 O3 44.64(15) . . yes O1 W1 C1 98.48(14) . . yes O2 W1 C1 82.25(15) . . ? O3 W1 C1 126.37(15) . . ? O1 W1 C05 102.73(13) . . ? O2 W1 C05 125.79(14) . . ? O3 W1 C05 85.66(14) . . ? C1 W1 C05 134.97(14) . . ? O1 W1 C01 84.03(13) . . ? O2 W1 C01 160.67(14) . . ? O3 W1 C01 119.25(14) . . ? C1 W1 C01 110.68(14) . . ? C05 W1 C01 35.13(12) . . ? O1 W1 C02 101.54(13) . . ? O2 W1 C02 146.35(13) . . ? O3 W1 C02 138.86(13) . . ? C1 W1 C02 79.39(14) . . ? C05 W1 C02 57.75(13) . . ? C01 W1 C02 33.97(12) . . ? O1 W1 C04 137.68(13) . . ? O2 W1 C04 104.87(14) . . ? O3 W1 C04 82.28(13) . . ? C1 W1 C04 110.79(14) . . ? C05 W1 C04 35.29(12) . . ? C01 W1 C04 57.69(12) . . ? C02 W1 C04 57.20(12) . . ? O1 W1 C03 136.24(13) . . ? O2 W1 C03 114.09(13) . . ? O3 W1 C03 111.19(13) . . ? C1 W1 C03 80.01(13) . . ? C05 W1 C03 57.32(12) . . ? C01 W1 C03 57.00(12) . . ? C02 W1 C03 34.84(12) . . ? C04 W1 C03 33.42(12) . . ? O3 O2 W1 67.69(18) . . yes O2 O3 W1 67.68(18) . . yes C2 C1 W1 176.9(3) . . yes C1 C2 C3 177.3(4) . . yes C4 C3 C2 178.9(5) . . yes C02 C01 C05 107.4(3) . . ? C02 C01 C11 127.1(4) . . ? C05 C01 C11 125.4(4) . . ? C02 C01 W1 73.0(2) . . ? C05 C01 W1 69.4(2) . . ? C11 C01 W1 121.6(3) . . ? C01 C02 C03 108.2(3) . . ? C01 C02 C12 126.4(3) . . ? C03 C02 C12 125.1(3) . . ? C01 C02 W1 73.0(2) . . ? C03 C02 W1 74.0(2) . . ? C12 C02 W1 124.7(3) . . ? C04 C03 C02 108.3(3) . . ? C04 C03 C13 126.3(3) . . ? C02 C03 C13 125.2(3) . . ? C04 C03 W1 72.6(2) . . ? C02 C03 W1 71.13(19) . . ? C13 C03 W1 126.0(2) . . ? C03 C04 C05 107.3(3) . . ? C03 C04 C14 127.2(3) . . ? C05 C04 C14 125.5(3) . . ? C03 C04 W1 74.0(2) . . ? C05 C04 W1 68.5(2) . . ? C14 C04 W1 121.3(2) . . ? C01 C05 C04 108.5(3) . . ? C01 C05 C15 125.9(3) . . ? C04 C05 C15 125.2(3) . . ? C01 C05 W1 75.5(2) . . ? C04 C05 W1 76.2(2) . . ? C15 C05 W1 120.5(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.171 _refine_diff_density_min -1.500 _refine_diff_density_rms 0.134 #===END data_02srv059Compound4 _database_code_CSD 196753 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ;(1,2,3,4,5-pentamethyl cyclopentadienyl)(dioxo)tungsten(buta- 1,3-diynyl) ; _chemical_melting_point ? _chemical_formula_moiety 'C14 H16 O2 W' _chemical_formula_sum 'C14 H16 O2 W' _chemical_formula_weight 400.12 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.5473(11) _cell_length_b 12.6869(11) _cell_length_c 17.0809(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2719.0(4) _cell_formula_units_Z 8 _cell_measurement_temperature 393(2) _cell_measurement_reflns_used 6073 _cell_measurement_theta_min 2.576 _cell_measurement_theta_max 34.815 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.955 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 8.484 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6701 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998)' _exptl_special_details ; The data collection nominally covered full sphere of reciprocal space, by a combination of 3 sets of \w scans; each set at different \f and/or 2\q angles and each scan (XX sec exposure) covering 0.3\% in \w. Crystal to detector distance 4.85 cm. ; _diffrn_ambient_temperature 120(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 'Bruker SMART CCD 6K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 28375 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 27.00 _reflns_number_total 2964 _reflns_number_gt 2563 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SMART version 5.625 (Bruker, 2001)' _computing_data_reduction 'SAINT version 6.02A (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL version 6.12 (Bruker, 2001)' _computing_publication_material 'SHELXTL version 6.12 (Bruker, 2001)' _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^)+(0.0000P)^2^+6.6022P] 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 2964 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0273 _refine_ls_R_factor_gt 0.0212 _refine_ls_wR_factor_ref 0.0650 _refine_ls_wR_factor_gt 0.0580 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.002 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.145827(11) 0.170157(12) 0.620554(8) 0.02198(7) Uani 1 1 d . . . O1 O 0.1173(3) 0.0457(2) 0.65713(18) 0.0390(7) Uani 1 1 d . . . O2 O 0.2573(2) 0.2170(3) 0.66823(18) 0.0426(8) Uani 1 1 d . . . C1 C 0.2046(3) 0.1397(3) 0.5088(2) 0.0251(8) Uani 1 1 d . . . C2 C 0.2434(3) 0.1171(3) 0.4467(2) 0.0241(7) Uani 1 1 d . . . C3 C 0.2870(3) 0.0877(3) 0.3759(2) 0.0246(8) Uani 1 1 d . . . C4 C 0.3224(3) 0.0574(3) 0.3147(3) 0.0316(9) Uani 1 1 d . . . H4 H 0.344(5) 0.032(5) 0.267(4) 0.065(19) Uiso 1 1 d . . . C01 C -0.0431(3) 0.2026(3) 0.6297(2) 0.0222(7) Uani 1 1 d . . . C02 C -0.0202(3) 0.2209(3) 0.5509(2) 0.0216(7) Uani 1 1 d . . . C03 C 0.0512(3) 0.3101(3) 0.5465(2) 0.0225(7) Uani 1 1 d . . . C04 C 0.0717(3) 0.3463(3) 0.6231(2) 0.0227(8) Uani 1 1 d . . . C05 C 0.0184(3) 0.2753(3) 0.6761(2) 0.0214(7) Uani 1 1 d . . . C11 C -0.1174(4) 0.1204(4) 0.6618(3) 0.0381(10) Uani 1 1 d . . . H11A H -0.1795 0.1157 0.6291 0.057 Uiso 1 1 calc R . . H11B H -0.1384 0.1395 0.7139 0.057 Uiso 1 1 calc R . . H11C H -0.0819 0.0534 0.6628 0.057 Uiso 1 1 calc R . . C12 C -0.0638(4) 0.1631(3) 0.4813(2) 0.0328(9) Uani 1 1 d . . . H12A H -0.0963 0.0985 0.4982 0.049 Uiso 1 1 calc R . . H12B H -0.0070 0.1476 0.4455 0.049 Uiso 1 1 calc R . . H12C H -0.1161 0.2062 0.4556 0.049 Uiso 1 1 calc R . . C13 C 0.0880(4) 0.3613(4) 0.4721(2) 0.0351(9) Uani 1 1 d . . . H13A H 0.0333 0.4075 0.4529 0.053 Uiso 1 1 calc R . . H13B H 0.1027 0.3080 0.4337 0.053 Uiso 1 1 calc R . . H13C H 0.1515 0.4012 0.4821 0.053 Uiso 1 1 calc R . . C14 C 0.1396(4) 0.4373(4) 0.6469(3) 0.0430(11) Uani 1 1 d . . . H14A H 0.1817 0.4181 0.6916 0.064 Uiso 1 1 calc R . . H14B H 0.0950 0.4962 0.6600 0.064 Uiso 1 1 calc R . . H14C H 0.1858 0.4563 0.6044 0.064 Uiso 1 1 calc R . . C15 C 0.0165(4) 0.2836(4) 0.7643(2) 0.0338(9) Uani 1 1 d . . . H15A H 0.0801 0.3180 0.7820 0.051 Uiso 1 1 calc R . . H15B H 0.0127 0.2142 0.7866 0.051 Uiso 1 1 calc R . . H15C H -0.0447 0.3237 0.7803 0.051 Uiso 1 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 W1 0.01987(10) 0.03137(11) 0.01470(10) 0.00240(5) -0.00043(5) 0.00648(5) O1 0.0509(18) 0.0371(17) 0.0290(16) 0.0106(13) 0.0102(14) 0.0218(15) O2 0.0246(15) 0.074(2) 0.0294(15) -0.0104(15) -0.0069(12) 0.0080(15) C1 0.0248(18) 0.0283(18) 0.0221(18) 0.0018(15) -0.0006(14) 0.0039(16) C2 0.0244(18) 0.0239(18) 0.0241(18) 0.0015(15) 0.0001(15) 0.0000(15) C3 0.0264(19) 0.0250(18) 0.0226(19) -0.0014(14) 0.0018(14) -0.0037(15) C4 0.029(2) 0.036(2) 0.029(2) -0.0064(17) 0.0038(17) -0.0090(18) C01 0.0168(17) 0.0266(18) 0.0233(18) 0.0022(14) 0.0019(13) 0.0000(14) C02 0.0230(17) 0.0225(18) 0.0193(17) 0.0001(13) -0.0053(14) 0.0027(15) C03 0.0249(18) 0.0248(17) 0.0178(17) 0.0028(13) -0.0019(14) 0.0040(15) C04 0.0231(18) 0.0222(17) 0.0229(19) -0.0002(13) -0.0008(14) -0.0008(14) C05 0.0194(16) 0.0257(18) 0.0191(17) 0.0003(14) -0.0009(13) 0.0023(15) C11 0.032(2) 0.038(2) 0.044(3) 0.002(2) 0.0088(19) -0.0091(19) C12 0.031(2) 0.038(2) 0.030(2) -0.0108(17) -0.0108(18) 0.0000(17) C13 0.046(3) 0.034(2) 0.026(2) 0.0111(17) 0.0027(18) 0.003(2) C14 0.049(3) 0.042(3) 0.038(3) -0.007(2) -0.004(2) -0.014(2) C15 0.039(2) 0.045(3) 0.0175(19) -0.0016(16) 0.0025(16) 0.010(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 W1 O2 1.724(3) . yes W1 O1 1.735(3) . yes W1 C1 2.082(4) . yes W1 C05 2.288(4) . ? W1 C01 2.411(4) . ? W1 C04 2.421(4) . ? W1 C03 2.483(4) . ? W1 C02 2.484(3) . ? C1 C2 1.202(5) . yes C2 C3 1.379(5) . yes C3 C4 1.200(6) . yes C01 C02 1.396(5) . ? C01 C05 1.442(5) . ? C01 C11 1.503(6) . ? C02 C03 1.446(5) . ? C02 C12 1.500(5) . ? C03 C04 1.410(5) . ? C03 C13 1.500(5) . ? C04 C05 1.441(5) . ? C04 C14 1.492(6) . ? C05 C15 1.510(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 O2 W1 O1 108.09(17) . . yes O2 W1 C1 102.12(15) . . ? O1 W1 C1 103.53(15) . . yes O2 W1 C05 99.78(14) . . ? O1 W1 C05 103.72(14) . . ? C1 W1 C05 137.37(14) . . ? O2 W1 C01 135.11(14) . . ? O1 W1 C01 85.94(14) . . ? C1 W1 C01 116.03(13) . . ? C05 W1 C01 35.61(13) . . ? O2 W1 C04 89.15(15) . . ? O1 W1 C04 138.94(14) . . ? C1 W1 C04 108.92(14) . . ? C05 W1 C04 35.48(13) . . ? C01 W1 C04 57.56(13) . . ? O2 W1 C03 112.47(15) . . ? O1 W1 C03 137.36(14) . . ? C1 W1 C03 80.53(13) . . ? C05 W1 C03 57.30(12) . . ? C01 W1 C03 55.98(12) . . ? C04 W1 C03 33.39(12) . . ? O2 W1 C02 144.84(15) . . ? O1 W1 C02 103.61(14) . . ? C1 W1 C02 84.59(13) . . ? C05 W1 C02 57.44(12) . . ? C01 W1 C02 33.09(12) . . ? C04 W1 C02 56.45(12) . . ? C03 W1 C02 33.85(12) . . ? C2 C1 W1 175.4(3) . . yes C1 C2 C3 178.0(4) . . yes C4 C3 C2 176.8(4) . . yes C02 C01 C05 108.3(3) . . ? C02 C01 C11 126.5(4) . . ? C05 C01 C11 125.2(4) . . ? C02 C01 W1 76.3(2) . . ? C05 C01 W1 67.55(19) . . ? C11 C01 W1 121.0(3) . . ? C01 C02 C03 107.9(3) . . ? C01 C02 C12 127.4(4) . . ? C03 C02 C12 124.6(3) . . ? C01 C02 W1 70.6(2) . . ? C03 C02 W1 73.0(2) . . ? C12 C02 W1 124.0(3) . . ? C04 C03 C02 108.7(3) . . ? C04 C03 C13 126.1(4) . . ? C02 C03 C13 125.0(3) . . ? C04 C03 W1 70.9(2) . . ? C02 C03 W1 73.1(2) . . ? C13 C03 W1 126.4(3) . . ? C03 C04 C05 107.2(3) . . ? C03 C04 C14 127.5(4) . . ? C05 C04 C14 125.3(4) . . ? C03 C04 W1 75.7(2) . . ? C05 C04 W1 67.2(2) . . ? C14 C04 W1 120.0(3) . . ? C04 C05 C01 107.6(3) . . ? C04 C05 C15 126.2(3) . . ? C01 C05 C15 125.8(3) . . ? C04 C05 W1 77.3(2) . . ? C01 C05 W1 76.8(2) . . ? C15 C05 W1 117.7(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.686 _refine_diff_density_min -1.841 _refine_diff_density_rms 0.113 #===END data_02srv044Compound6 _database_code_CSD 196752 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; bis((1,2,3,4,5-pentamethyl cyclopentadienyl)(dioxo)tungsten) buta-1,3-diyn-1,4-diyl ; _chemical_melting_point ? _chemical_formula_moiety 'C24 H30 O4 W2' _chemical_formula_sum 'C24 H30 O4 W2' _chemical_formula_weight 750.18 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.6091(5) _cell_length_b 12.1041(4) _cell_length_c 15.4689(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2360.89(15) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 6342 _cell_measurement_theta_min 2.634 _cell_measurement_theta_max 29.993 _exptl_crystal_description block _exptl_crystal_colour light_yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas "not measured'" _exptl_crystal_density_diffrn 2.111 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 9.763 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4462 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998)' _exptl_special_details ; The data collection nominally covered full sphere of reciprocal Space, by a combination of 3 sets of \w scans each set at different \f and/or 2\q angles and each scan (8s exposure) covering 0.3\% in \w. Crystal to detector distance 4.85 cm. ; _diffrn_ambient_temperature 120(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 'Bruker SMART CCD 6K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 16192 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 30.01 _reflns_number_total 3396 _reflns_number_gt 2872 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SMART version 5.625 (Bruker, 2001)' _computing_data_reduction 'SAINT version 6.02A (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL version 6.12 (Bruker, 2001)' _computing_publication_material 'SHELXTL version 6.12 (Bruker, 2001)' _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^)+(0.0192P)^2^+5.9062P] 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 3396 _refine_ls_number_parameters 141 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0320 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0624 _refine_ls_wR_factor_gt 0.0586 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.003 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.115022(11) 0.760533(11) 0.148762(8) 0.01295(5) Uani 1 1 d . . . O1 O 0.2480(2) 0.7647(2) 0.1205(2) 0.0263(6) Uani 1 1 d . . . C1 C 0.0519(3) 0.8838(3) 0.0714(2) 0.0192(7) Uani 1 1 d . . . C2 C 0.0184(3) 0.9578(3) 0.0256(2) 0.0193(7) Uani 1 1 d . . . C01 C 0.1064(3) 0.5837(3) 0.0763(2) 0.0158(6) Uani 1 1 d . . . C02 C 0.0222(3) 0.6442(3) 0.0412(2) 0.0159(6) Uani 1 1 d . . . C03 C -0.0536(3) 0.6680(3) 0.1105(2) 0.0169(7) Uani 1 1 d . . . C04 C -0.0135(3) 0.6213(3) 0.1875(2) 0.0161(6) Uani 1 1 d . . . C05 C 0.0874(3) 0.5732(3) 0.1682(2) 0.0168(7) Uani 1 1 d . . . C11 C 0.2000(3) 0.5390(3) 0.0291(3) 0.0263(8) Uani 1 1 d . . . H11A H 0.1935 0.5557 -0.0314 0.039 Uiso 1 1 calc R . . H11B H 0.2032 0.4603 0.0367 0.039 Uiso 1 1 calc R . . H11C H 0.2636 0.5720 0.0514 0.039 Uiso 1 1 calc R . . C12 C 0.0084(3) 0.6751(3) -0.0520(2) 0.0247(8) Uani 1 1 d . . . H12A H 0.0692 0.7162 -0.0712 0.037 Uiso 1 1 calc R . . H12B H -0.0541 0.7196 -0.0583 0.037 Uiso 1 1 calc R . . H12C H 0.0014 0.6093 -0.0862 0.037 Uiso 1 1 calc R . . C13 C -0.1575(3) 0.7272(3) 0.1006(3) 0.0258(8) Uani 1 1 d . . . H13A H -0.2133 0.6741 0.0930 0.039 Uiso 1 1 calc R . . H13B H -0.1545 0.7748 0.0511 0.039 Uiso 1 1 calc R . . H13C H -0.1712 0.7704 0.1514 0.039 Uiso 1 1 calc R . . C14 C -0.0643(3) 0.6212(3) 0.2743(2) 0.0255(8) Uani 1 1 d . . . H14A H -0.1204 0.6748 0.2754 0.038 Uiso 1 1 calc R . . H14B H -0.0124 0.6397 0.3174 0.038 Uiso 1 1 calc R . . H14C H -0.0928 0.5492 0.2861 0.038 Uiso 1 1 calc R . . C15 C 0.1526(3) 0.5047(3) 0.2300(3) 0.0269(8) Uani 1 1 d . . . H15A H 0.1532 0.5393 0.2858 0.040 Uiso 1 1 calc R . . H15B H 0.2238 0.4988 0.2087 0.040 Uiso 1 1 calc R . . H15C H 0.1221 0.4322 0.2347 0.040 Uiso 1 1 calc R . . O2 O 0.1021(3) 0.8150(3) 0.25115(18) 0.0321(7) Uani 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 W1 0.01562(8) 0.00948(8) 0.01376(8) 0.00216(4) -0.00269(4) -0.00132(4) O1 0.0173(13) 0.0192(14) 0.0422(16) 0.0081(12) -0.0029(12) -0.0043(10) C1 0.0222(18) 0.0093(15) 0.0260(18) 0.0019(12) -0.0026(14) -0.0007(12) C2 0.0201(17) 0.0120(16) 0.0258(18) -0.0003(13) -0.0039(14) -0.0030(13) C01 0.0194(17) 0.0096(15) 0.0182(16) -0.0002(11) 0.0035(13) -0.0009(12) C02 0.0209(17) 0.0085(14) 0.0183(15) 0.0024(11) 0.0009(13) -0.0032(12) C03 0.0171(17) 0.0140(16) 0.0198(16) -0.0016(12) 0.0000(13) -0.0025(12) C04 0.0203(16) 0.0123(16) 0.0157(15) 0.0002(12) 0.0017(13) -0.0027(12) C05 0.0218(17) 0.0095(15) 0.0192(16) 0.0025(12) -0.0012(13) 0.0008(12) C11 0.025(2) 0.0194(19) 0.034(2) -0.0034(15) 0.0100(16) 0.0018(15) C12 0.036(2) 0.0223(19) 0.0156(16) 0.0023(14) -0.0033(15) -0.0076(16) C13 0.0162(18) 0.024(2) 0.037(2) 0.0017(15) -0.0020(15) 0.0031(15) C14 0.032(2) 0.024(2) 0.0205(17) 0.0011(14) 0.0084(15) -0.0054(16) C15 0.030(2) 0.0176(18) 0.034(2) 0.0099(15) -0.0072(17) 0.0025(15) O2 0.0543(19) 0.0242(15) 0.0178(13) -0.0016(11) -0.0026(12) -0.0101(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 W1 O2 1.723(3) . yes W1 O1 1.733(3) . yes W1 C1 2.072(4) . yes W1 C05 2.313(3) . ? W1 C04 2.414(3) . ? W1 C01 2.418(3) . ? W1 C03 2.475(4) . ? W1 C02 2.474(3) . ? C1 C2 1.217(5) . yes C2 C2 1.375(7) 5_575 yes C01 C02 1.399(5) . ? C01 C05 1.447(5) . ? C01 C11 1.491(5) . ? C02 C03 1.465(5) . ? C02 C12 1.499(5) . ? C03 C04 1.413(5) . ? C03 C13 1.501(5) . ? C04 C05 1.430(5) . ? C04 C14 1.487(5) . ? C05 C15 1.509(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 O2 W1 O1 108.17(16) . . yes O2 W1 C1 102.67(15) . . yes O1 W1 C1 101.85(14) . . yes O2 W1 C05 103.95(13) . . ? O1 W1 C05 101.94(13) . . ? C1 W1 C05 136.29(13) . . ? O2 W1 C04 88.58(13) . . ? O1 W1 C04 137.07(12) . . ? C1 W1 C04 112.86(13) . . ? C05 W1 C04 35.14(12) . . ? O2 W1 C01 139.47(13) . . ? O1 W1 C01 87.30(13) . . ? C1 W1 C01 110.62(13) . . ? C05 W1 C01 35.52(11) . . ? C04 W1 C01 57.77(11) . . ? O2 W1 C03 108.14(13) . . ? O1 W1 C03 141.64(13) . . ? C1 W1 C03 81.81(13) . . ? C05 W1 C03 57.20(12) . . ? C04 W1 C03 33.57(11) . . ? C01 W1 C03 56.63(12) . . ? O2 W1 C02 142.28(13) . . ? O1 W1 C02 107.75(13) . . ? C1 W1 C02 80.75(12) . . ? C05 W1 C02 57.22(11) . . ? C04 W1 C02 56.79(11) . . ? C01 W1 C02 33.22(11) . . ? C03 W1 C02 34.44(11) . . ? C2 C1 W1 177.6(3) . . yes C1 C2 C2 179.3(5) . 5_575 yes C02 C01 C05 107.6(3) . . ? C02 C01 C11 126.9(3) . . ? C05 C01 C11 125.5(3) . . ? C02 C01 W1 75.6(2) . . ? C05 C01 W1 68.28(19) . . ? C11 C01 W1 120.9(2) . . ? C01 C02 C03 108.2(3) . . ? C01 C02 C12 126.3(3) . . ? C03 C02 C12 125.4(3) . . ? C01 C02 W1 71.2(2) . . ? C03 C02 W1 72.78(19) . . ? C12 C02 W1 124.0(2) . . ? C04 C03 C02 107.8(3) . . ? C04 C03 C13 126.1(3) . . ? C02 C03 C13 126.0(3) . . ? C04 C03 W1 70.9(2) . . ? C02 C03 W1 72.78(19) . . ? C13 C03 W1 124.0(3) . . ? C03 C04 C05 107.8(3) . . ? C03 C04 C14 127.4(3) . . ? C05 C04 C14 124.9(3) . . ? C03 C04 W1 75.6(2) . . ? C05 C04 W1 68.60(19) . . ? C14 C04 W1 120.9(2) . . ? C04 C05 C01 108.5(3) . . ? C04 C05 C15 125.1(3) . . ? C01 C05 C15 125.5(3) . . ? C04 C05 W1 76.3(2) . . ? C01 C05 W1 76.2(2) . . ? C15 C05 W1 122.7(3) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.732 _refine_diff_density_min -2.310 _refine_diff_density_rms 0.185