data_2003627 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 1270 _journal_page_last 1271 _publ_section_title ; (3-Chloro-1,2-propanediolato-O,O')bis(2,3-dimethyl-2,3-butanediolato-O,O') tungsten(VI) ; _chemical_formula_moiety 'C15 H29 Cl1 O6 W1' _chemical_formula_sum 'C15 H29 Cl1 O6 W1' _chemical_formula_structural '[W(C~3~H~5~ClO~2~)(C~6~H~12~O~2~)~2~]' _chemical_formula_weight 524.68 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _symmetry_space_group_name_H-M 'P -1' _cell_length_a 9.315(3) _cell_length_b 12.995(5) _cell_length_c 8.913(3) _cell_angle_alpha 105.63(3) _cell_angle_beta 104.29(3) _cell_angle_gamma 69.98(3) _cell_volume 961.9(6) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.812 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 4.7 _cell_measurement_theta_max 8.8 _exptl_absorpt_coefficient_mu 6.168 _cell_measurement_temperature 293(2) _exptl_crystal_description 'bright prisms' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_colour 'colourless' _chemical_compound_source ? _diffrn_measurement_device 'Rigaku AFC-5S' _diffrn_measurement_method \w/-2\q _exptl_absorpt_correction_type 'empirical via \y scans' _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 1.00 _diffrn_reflns_number 3614 _reflns_number_total 3383 _reflns_number_observed 2628 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.8 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0466 _refine_ls_wR_factor_obs 0.1091 _refine_ls_wR_factor_all 0.1225 _refine_ls_goodness_of_fit_obs 1.076 _refine_ls_goodness_of_fit_all 1.056 _refine_ls_number_reflns 3383 _refine_ls_number_parameters 208 _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(F~o~^2^) + (0.0534P)^2^] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_shift/esd_max 0.000 _refine_diff_density_max 1.117 _refine_diff_density_min -1.548 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0033 0.001 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.000 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0106 0.006 'Cl' 'Cl' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.1484 0.1 'W' 'W' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' -0.8490 6.87 ; TEXSAN (Molecular Structure Corporation, 1989) ; ; TEXSAN (Molecular Structure Corporation, 1989) ; ; TEXSAN (Molecular Structure Corporation, 1989) ; loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv W1 1 0.08068(5) 0.27828(4) 0.12315(6) 0.0332(2) Cl1 1 -0.4299(4) 0.5992(3) 0.1666(5) 0.0744(11) O1 1 -0.0950(8) 0.2970(6) 0.2167(9) 0.040(2) O2 1 0.0194(8) 0.4375(7) 0.2056(9) 0.043(2) O3 1 -0.0015(9) 0.3083(6) -0.0824(9) 0.040(2) O4 1 0.0651(8) 0.1372(7) 0.0035(8) 0.040(2) O5 1 0.2140(8) 0.2111(6) 0.2915(8) 0.036(2) O6 1 0.2757(8) 0.2879(6) 0.1072(9) 0.040(2) C1 1 -0.1522(13) 0.4023(9) 0.3185(13) 0.042(3) H1A 1 -0.0957(13) 0.4023(9) 0.4256(13) 0.051 H1B 1 -0.2614(13) 0.4177(9) 0.3197(13) 0.051 C2 1 -0.1273(13) 0.4875(10) 0.2512(14) 0.045(3) H2 1 -0.1257(13) 0.5548(10) 0.3334(14) 0.054 C3 1 -0.2459(15) 0.5189(11) 0.1094(15) 0.053(3) H3A 1 -0.2561(15) 0.4516(11) 0.0331(15) 0.064 H3B 1 -0.2117(15) 0.5622(11) 0.0597(15) 0.064 C4 1 -0.1392(16) 0.2649(13) -0.3443(15) 0.066(4) H4A 1 -0.2346(16) 0.2854(13) -0.3052(15) 0.079 H4B 1 -0.1409(16) 0.2082(13) -0.4389(15) 0.079 H4C 1 -0.1277(16) 0.3294(13) -0.3674(15) 0.079 C5 1 -0.0031(14) 0.2200(12) -0.2192(14) 0.050(3) C6 1 -0.0268(12) 0.1275(10) -0.1516(13) 0.039(3) C7 1 0.0334(17) 0.0085(11) -0.2459(15) 0.057(3) H7A 1 0.1388(17) -0.0053(11) -0.2566(15) 0.069 H7B 1 -0.0296(17) 0.0006(11) -0.3488(15) 0.069 H7C 1 0.0287(17) -0.0443(11) -0.1913(15) 0.069 C8 1 0.1499(16) 0.1863(13) -0.2731(16) 0.063(4) H8A 1 0.2320(16) 0.1586(13) -0.1914(16) 0.076 H8B 1 0.1645(16) 0.2500(13) -0.2955(16) 0.076 H8C 1 0.1512(16) 0.1287(13) -0.3670(16) 0.076 C9 1 -0.1927(13) 0.1484(12) -0.1354(14) 0.051(3) H9A 1 -0.2311(13) 0.2228(12) -0.0765(14) 0.061 H9B 1 -0.1970(13) 0.0953(12) -0.0810(14) 0.061 H9C 1 -0.2554(13) 0.1403(12) -0.2386(14) 0.061 C10 1 0.4576(16) 0.1717(12) 0.4707(14) 0.058(3) H10A 1 0.4297(16) 0.2450(12) 0.5362(14) 0.069 H10B 1 0.5681(16) 0.1448(12) 0.4766(14) 0.069 H10C 1 0.4241(16) 0.1218(12) 0.5068(14) 0.069 C11 1 0.3803(13) 0.1772(9) 0.3013(13) 0.040(3) C12 1 0.4044(12) 0.2698(10) 0.2351(14) 0.043(3) C13 1 0.5530(14) 0.2321(13) 0.1689(17) 0.064(4) H13A 1 0.5586(14) 0.1632(13) 0.0930(17) 0.077 H13B 1 0.6401(14) 0.2210(13) 0.2532(17) 0.077 H13C 1 0.5545(14) 0.2883(13) 0.1184(17) 0.077 C14 1 0.4257(15) 0.0604(11) 0.1991(16) 0.058(4) H14A 1 0.3771(15) 0.0630(11) 0.0913(16) 0.069 H14B 1 0.3922(15) 0.0108(11) 0.2360(16) 0.069 H14C 1 0.5363(15) 0.0338(11) 0.2057(16) 0.069 C15 1 0.3942(16) 0.3772(11) 0.3536(16) 0.060(4) H15A 1 0.2997(16) 0.4005(11) 0.3950(16) 0.072 H15B 1 0.3955(16) 0.4337(11) 0.3036(16) 0.072 H15C 1 0.4810(16) 0.3664(11) 0.4383(16) 0.072 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 W1 0.0323(2) -0.0101(2) 0.0046(2) 0.0335(3) 0.0084(2) 0.0345(2) Cl1 0.051(2) 0.007(2) 0.005(2) 0.072(3) -0.004(2) 0.066(2) O1 0.042(4) -0.013(3) 0.006(3) 0.034(4) 0.013(4) 0.047(5) O2 0.038(4) -0.020(4) 0.000(3) 0.051(5) 0.007(4) 0.042(4) O3 0.051(5) -0.011(3) 0.006(4) 0.030(4) 0.018(4) 0.044(4) O4 0.039(4) -0.021(4) -0.008(3) 0.051(5) 0.018(4) 0.034(4) O5 0.036(4) -0.011(3) 0.002(3) 0.038(4) 0.010(3) 0.034(4) O6 0.040(4) -0.017(3) 0.014(4) 0.037(4) 0.007(4) 0.050(5) C1 0.046(6) -0.009(5) 0.006(5) 0.043(7) 0.004(5) 0.033(6) C2 0.043(6) -0.008(5) 0.011(5) 0.040(7) 0.007(6) 0.049(7) C3 0.059(8) 0.008(6) 0.015(6) 0.039(7) 0.006(6) 0.046(7) C4 0.068(9) -0.023(8) -0.016(7) 0.082(11) 0.035(8) 0.048(8) C5 0.047(7) -0.024(6) -0.001(5) 0.067(9) 0.018(6) 0.041(7) C6 0.040(6) -0.011(5) 0.003(5) 0.041(7) 0.010(5) 0.036(6) C7 0.080(10) -0.016(7) 0.014(7) 0.046(8) 0.005(6) 0.043(7) C8 0.078(10) -0.036(8) 0.022(7) 0.078(11) 0.008(7) 0.048(8) C9 0.036(6) -0.023(6) -0.008(5) 0.068(9) 0.010(6) 0.046(7) C10 0.063(8) -0.010(7) 0.009(6) 0.062(9) 0.008(6) 0.041(7) C11 0.042(6) -0.012(5) 0.009(5) 0.029(6) -0.002(5) 0.045(7) C12 0.027(5) -0.017(5) 0.006(5) 0.054(8) -0.002(6) 0.045(7) C13 0.037(7) -0.017(7) 0.013(7) 0.076(10) 0.009(8) 0.077(10) C14 0.049(7) -0.013(6) 0.005(7) 0.043(8) -0.001(7) 0.070(9) C15 0.061(8) -0.018(6) 0.002(7) 0.041(8) -0.001(7) 0.068(9)