#------------------------------------------------------------------------------ #$Date: 2012-02-24 19:13:23 +0200 (Fri, 24 Feb 2012) $ #$Revision: 34330 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/06/41/4064129.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4064129 loop_ _publ_author_name 'Tran Huy, Ngoc Hoa' 'Lu, Yunpeng' 'Mathey, Fran\,cois' _publ_section_title ; Oligomerization of Terminal Phosphinidene Complexes ; _journal_issue 6 _journal_name_full Organometallics _journal_page_first 1734 _journal_volume 30 _journal_year 2011 _chemical_formula_moiety 'C25 H12 N2 O15 P2 W3' _chemical_formula_sum 'C25 H12 N2 O15 P2 W3' _chemical_formula_weight 1193.86 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 92.847(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 11.8633(5) _cell_length_b 21.0617(8) _cell_length_c 12.6050(5) _cell_measurement_reflns_used 6080 _cell_measurement_temperature 103(2) _cell_measurement_theta_max 30.47 _cell_measurement_theta_min 3.01 _cell_volume 3145.6(2) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 103(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 43554 _diffrn_reflns_theta_full 28.00 _diffrn_reflns_theta_max 28.00 _diffrn_reflns_theta_min 1.88 _exptl_absorpt_coefficient_mu 11.119 _exptl_absorpt_correction_T_max 0.6647 _exptl_absorpt_correction_T_min 0.4027 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour brown _exptl_crystal_density_diffrn 2.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2192 _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _refine_diff_density_max 5.427 _refine_diff_density_min -2.631 _refine_diff_density_rms 0.501 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.188 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 426 _refine_ls_number_reflns 7603 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.188 _refine_ls_R_factor_all 0.0503 _refine_ls_R_factor_gt 0.0366 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0602P)^2^+28.1653P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0954 _refine_ls_wR_factor_ref 0.1203 _reflns_number_gt 6407 _reflns_number_total 7603 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file om101144n_si_003.cif _[local]_cod_data_source_block mat33 _[local]_cod_cif_authors_sg_H-M P2(1)/n _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 4064129 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' 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 W1 W 0.28357(3) 0.080358(16) 0.52610(3) 0.01712(10) Uani 1 1 d . W2 W 0.19355(3) 0.139744(16) 1.02188(3) 0.01807(10) Uani 1 1 d . W3 W 0.22767(3) 0.253688(14) 0.72170(2) 0.01152(9) Uani 1 1 d . C1 C 0.0555(9) 0.1131(4) 0.7156(8) 0.026(2) Uani 1 1 d . C2 C -0.0451(9) 0.1454(5) 0.6875(9) 0.030(2) Uani 1 1 d . H2 H -0.0505 0.1886 0.6660 0.036 Uiso 1 1 calc R C3 C -0.1363(8) 0.1038(5) 0.6964(7) 0.025(2) Uani 1 1 d . H3 H -0.2139 0.1135 0.6828 0.030 Uiso 1 1 calc R C4 C -0.0933(8) 0.0481(5) 0.7274(8) 0.026(2) Uani 1 1 d . H4 H -0.1364 0.0109 0.7384 0.031 Uiso 1 1 calc R C5 C 0.0935(9) -0.0016(5) 0.7702(8) 0.027(2) Uani 1 1 d . H5A H 0.0615 -0.0249 0.8290 0.040 Uiso 1 1 calc R H5B H 0.1691 0.0137 0.7923 0.040 Uiso 1 1 calc R H5C H 0.0986 -0.0299 0.7089 0.040 Uiso 1 1 calc R C6 C 0.1165(8) 0.0689(4) 0.4820(8) 0.0230(19) Uani 1 1 d . C7 C 0.2935(9) -0.0104(4) 0.5870(7) 0.024(2) Uani 1 1 d . C8 C 0.4510(10) 0.0916(5) 0.5696(8) 0.029(2) Uani 1 1 d . C9 C 0.2791(8) 0.1644(4) 0.4424(7) 0.0192(17) Uani 1 1 d . C10 C 0.3269(8) 0.0446(4) 0.3867(8) 0.0232(19) Uani 1 1 d . C11 C 0.4309(9) 0.1425(4) 0.8266(9) 0.029(2) Uani 1 1 d . C12 C 0.5174(8) 0.1859(5) 0.8242(8) 0.027(2) Uani 1 1 d . H12 H 0.5094 0.2302 0.8122 0.032 Uiso 1 1 calc R C13 C 0.6207(9) 0.1527(5) 0.8428(8) 0.029(2) Uani 1 1 d . H13 H 0.6944 0.1705 0.8464 0.035 Uiso 1 1 calc R C14 C 0.5932(8) 0.0906(5) 0.8545(8) 0.025(2) Uani 1 1 d . H14 H 0.6461 0.0573 0.8672 0.030 Uiso 1 1 calc R C15 C 0.4237(9) 0.0222(5) 0.8534(9) 0.029(2) Uani 1 1 d . H15A H 0.4786 -0.0120 0.8450 0.043 Uiso 1 1 calc R H15B H 0.3636 0.0189 0.7975 0.043 Uiso 1 1 calc R H15C H 0.3911 0.0185 0.9231 0.043 Uiso 1 1 calc R C16 C 0.1891(9) 0.0434(5) 1.0184(7) 0.027(2) Uani 1 1 d . C17 C 0.0275(10) 0.1405(4) 0.9676(8) 0.029(2) Uani 1 1 d . C18 C 0.1941(8) 0.2361(4) 1.0479(7) 0.0214(18) Uani 1 1 d . C19 C 0.3564(9) 0.1368(5) 1.0831(9) 0.029(2) Uani 1 1 d . C20 C 0.1369(9) 0.1333(5) 1.1668(7) 0.024(2) Uani 1 1 d . C21 C 0.0869(8) 0.2692(5) 0.8084(7) 0.0217(19) Uani 1 1 d . C22 C 0.1250(8) 0.2419(4) 0.5881(7) 0.0219(19) Uani 1 1 d . C23 C 0.3705(8) 0.2458(4) 0.6369(7) 0.0199(18) Uani 1 1 d . C24 C 0.3226(8) 0.2935(4) 0.8477(7) 0.0216(18) Uani 1 1 d . C25 C 0.2200(8) 0.3459(4) 0.6714(7) 0.0187(17) Uani 1 1 d . N1 N 0.0219(7) 0.0518(4) 0.7414(6) 0.0202(16) Uani 1 1 d . N2 N 0.4794(7) 0.0829(4) 0.8456(6) 0.0222(16) Uani 1 1 d . O1 O 0.0223(7) 0.0633(3) 0.4579(6) 0.0330(17) Uani 1 1 d . O2 O 0.3025(7) -0.0614(3) 0.6135(6) 0.0375(18) Uani 1 1 d . O3 O 0.5450(7) 0.0962(4) 0.5908(7) 0.0361(18) Uani 1 1 d . O4 O 0.2758(6) 0.2074(3) 0.3897(6) 0.0273(15) Uani 1 1 d . O5 O 0.3497(6) 0.0274(4) 0.3054(5) 0.0310(16) Uani 1 1 d . O6 O 0.1842(7) -0.0108(3) 1.0225(6) 0.0356(18) Uani 1 1 d . O7 O -0.0674(7) 0.1405(4) 0.9472(7) 0.042(2) Uani 1 1 d . O8 O 0.1959(6) 0.2882(3) 1.0698(6) 0.0335(17) Uani 1 1 d . O9 O 0.4483(8) 0.1344(4) 1.1185(8) 0.050(2) Uani 1 1 d . O10 O 0.0989(8) 0.1308(4) 1.2485(6) 0.040(2) Uani 1 1 d . O11 O 0.0111(7) 0.2812(4) 0.8550(6) 0.0385(19) Uani 1 1 d . O12 O 0.0665(7) 0.2369(4) 0.5146(6) 0.0350(17) Uani 1 1 d . O13 O 0.4480(6) 0.2433(3) 0.5899(6) 0.0304(16) Uani 1 1 d . O14 O 0.3711(6) 0.3202(4) 0.9130(6) 0.0361(18) Uani 1 1 d . O15 O 0.2172(7) 0.3967(3) 0.6422(6) 0.0300(16) Uani 1 1 d . P1 P 0.2014(2) 0.13189(11) 0.68876(19) 0.0227(5) Uani 1 1 d . P2 P 0.2798(2) 0.15613(12) 0.8414(2) 0.0232(5) 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 0.0291(2) 0.01082(16) 0.01151(16) -0.00089(12) 0.00151(13) 0.00210(13) W2 0.0306(2) 0.01310(17) 0.01053(16) 0.00077(12) 0.00063(13) 0.00073(13) W3 0.01533(16) 0.00752(15) 0.01159(16) 0.00058(11) -0.00069(11) 0.00077(11) C1 0.029(5) 0.018(4) 0.031(5) 0.003(4) -0.004(4) -0.005(4) C2 0.029(5) 0.024(5) 0.036(6) 0.008(4) -0.003(4) -0.001(4) C3 0.021(5) 0.033(5) 0.019(4) 0.003(4) -0.001(4) 0.001(4) C4 0.020(5) 0.035(5) 0.024(5) -0.004(4) 0.002(4) -0.009(4) C5 0.030(5) 0.022(5) 0.027(5) 0.001(4) -0.007(4) -0.004(4) C6 0.025(5) 0.016(4) 0.028(5) 0.005(4) 0.010(4) 0.000(4) C7 0.038(6) 0.017(4) 0.018(4) -0.001(3) 0.003(4) 0.003(4) C8 0.046(7) 0.018(4) 0.023(5) 0.000(4) -0.003(4) 0.002(4) C9 0.021(4) 0.018(4) 0.018(4) 0.001(3) 0.000(3) -0.003(3) C10 0.028(5) 0.018(4) 0.023(5) 0.001(4) 0.001(4) 0.002(4) C11 0.026(5) 0.018(5) 0.043(6) 0.004(4) -0.003(4) 0.006(4) C12 0.020(5) 0.024(5) 0.035(5) 0.004(4) -0.003(4) 0.004(4) C13 0.022(5) 0.033(5) 0.032(5) -0.011(4) 0.002(4) -0.001(4) C14 0.022(5) 0.027(5) 0.026(5) -0.010(4) -0.006(4) 0.010(4) C15 0.029(5) 0.019(4) 0.038(6) 0.005(4) 0.001(4) 0.001(4) C16 0.043(6) 0.020(5) 0.019(4) 0.000(4) 0.008(4) -0.007(4) C17 0.046(7) 0.019(5) 0.021(5) -0.004(4) -0.002(4) -0.004(4) C18 0.023(5) 0.022(5) 0.019(4) -0.002(4) 0.003(4) 0.000(4) C19 0.023(5) 0.026(5) 0.037(6) 0.006(4) -0.001(4) -0.002(4) C20 0.029(5) 0.028(5) 0.015(4) 0.001(4) -0.005(4) -0.003(4) C21 0.022(5) 0.026(5) 0.016(4) 0.006(4) -0.003(4) 0.003(4) C22 0.031(5) 0.018(4) 0.017(4) 0.001(3) 0.003(4) -0.001(4) C23 0.023(5) 0.014(4) 0.022(4) -0.002(3) 0.001(4) -0.006(3) C24 0.022(5) 0.022(4) 0.020(4) -0.001(4) 0.002(4) -0.003(4) C25 0.019(4) 0.015(4) 0.022(4) -0.005(3) -0.001(3) -0.002(3) N1 0.025(4) 0.018(4) 0.017(4) -0.001(3) 0.000(3) -0.002(3) N2 0.025(4) 0.018(4) 0.024(4) 0.000(3) -0.002(3) 0.003(3) O1 0.032(4) 0.024(4) 0.043(4) 0.003(3) 0.004(3) -0.001(3) O2 0.055(5) 0.019(4) 0.038(4) 0.003(3) 0.006(4) 0.007(3) O3 0.029(4) 0.035(4) 0.044(5) -0.002(4) -0.009(3) 0.005(3) O4 0.030(4) 0.022(3) 0.030(4) 0.008(3) -0.001(3) -0.003(3) O5 0.044(4) 0.032(4) 0.018(3) -0.008(3) 0.008(3) 0.005(3) O6 0.059(5) 0.013(3) 0.035(4) 0.002(3) 0.003(4) 0.007(3) O7 0.035(5) 0.042(5) 0.047(5) 0.001(4) -0.016(4) -0.006(4) O8 0.035(4) 0.019(3) 0.047(5) -0.012(3) 0.005(3) -0.001(3) O9 0.039(5) 0.046(5) 0.063(6) 0.014(5) -0.007(4) -0.004(4) O10 0.059(6) 0.047(5) 0.015(3) 0.001(3) 0.006(3) -0.014(4) O11 0.032(4) 0.057(5) 0.027(4) 0.007(4) 0.010(3) 0.018(4) O12 0.038(4) 0.042(4) 0.024(4) 0.000(3) -0.012(3) 0.003(4) O13 0.027(4) 0.035(4) 0.030(4) -0.005(3) 0.011(3) -0.009(3) O14 0.025(4) 0.050(5) 0.033(4) -0.011(4) -0.006(3) -0.002(3) O15 0.045(5) 0.010(3) 0.034(4) 0.003(3) -0.005(3) -0.001(3) P1 0.0288(13) 0.0183(11) 0.0207(11) 0.0002(9) -0.0008(10) 0.0001(9) P2 0.0287(13) 0.0200(11) 0.0206(11) -0.0001(9) -0.0015(10) 0.0030(10) 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' N N 0.0061 0.0033 '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' P P 0.1023 0.0942 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C10 W1 C6 90.3(4) C10 W1 C8 89.5(4) C6 W1 C8 179.7(4) C10 W1 C9 82.8(4) C6 W1 C9 87.8(4) C8 W1 C9 92.2(4) C10 W1 C7 88.0(4) C6 W1 C7 91.6(4) C8 W1 C7 88.3(4) C9 W1 C7 170.8(4) C10 W1 P1 171.4(3) C6 W1 P1 82.2(3) C8 W1 P1 98.0(3) C9 W1 P1 92.6(3) C7 W1 P1 96.4(3) C20 W2 C16 86.6(4) C20 W2 C19 90.4(4) C16 W2 C19 90.1(4) C20 W2 C17 86.8(4) C16 W2 C17 88.7(4) C19 W2 C17 177.0(4) C20 W2 C18 85.4(4) C16 W2 C18 171.9(4) C19 W2 C18 88.5(4) C17 W2 C18 92.3(4) C20 W2 P2 174.6(3) C16 W2 P2 97.3(3) C19 W2 P2 85.8(3) C17 W2 P2 97.0(3) C18 W2 P2 90.6(3) C22 W3 C25 81.0(4) C22 W3 C23 92.0(4) C25 W3 C23 86.6(3) C22 W3 C21 89.5(4) C25 W3 C21 89.4(4) C23 W3 C21 175.4(4) C22 W3 C24 163.2(4) C25 W3 C24 82.4(4) C23 W3 C24 90.0(4) C21 W3 C24 87.3(4) C22 W3 P2 119.7(3) C25 W3 P2 159.2(3) C23 W3 P2 93.4(3) C21 W3 P2 89.6(3) C24 W3 P2 76.8(3) C22 W3 P1 71.9(3) C25 W3 P1 151.6(3) C23 W3 P1 86.2(2) C21 W3 P1 98.4(3) C24 W3 P1 125.0(3) P2 W3 P1 48.79(8) N1 C1 C2 105.0(8) N1 C1 P1 121.9(7) C2 C1 P1 130.6(8) C3 C2 C1 109.0(9) C3 C2 H2 125.5 C1 C2 H2 125.5 C4 C3 C2 106.8(9) C4 C3 H3 126.6 C2 C3 H3 126.6 C3 C4 N1 110.7(9) C3 C4 H4 124.7 N1 C4 H4 124.7 N1 C5 H5A 109.5 N1 C5 H5B 109.5 H5A C5 H5B 109.5 N1 C5 H5C 109.5 H5A C5 H5C 109.5 H5B C5 H5C 109.5 O1 C6 W1 179.1(9) O2 C7 W1 174.8(8) O3 C8 W1 177.4(9) O4 C9 W1 174.6(8) O5 C10 W1 176.3(8) C12 C11 N2 107.4(9) C12 C11 P2 129.3(7) N2 C11 P2 121.3(7) C11 C12 C13 108.0(9) C11 C12 H12 126.0 C13 C12 H12 126.0 C14 C13 C12 106.4(9) C14 C13 H13 126.8 C12 C13 H13 126.8 C13 C14 N2 110.4(8) C13 C14 H14 124.8 N2 C14 H14 124.8 N2 C15 H15A 109.5 N2 C15 H15B 109.5 H15A C15 H15B 109.5 N2 C15 H15C 109.5 H15A C15 H15C 109.5 H15B C15 H15C 109.5 O6 C16 W2 175.8(8) O7 C17 W2 173.5(9) O8 C18 W2 175.1(9) O9 C19 W2 179.1(10) O10 C20 W2 176.4(9) O11 C21 W3 176.2(9) O12 C22 W3 178.1(9) O13 C23 W3 178.0(8) O14 C24 W3 173.9(9) O15 C25 W3 178.7(9) C4 N1 C1 108.5(8) C4 N1 C5 123.9(8) C1 N1 C5 127.4(8) C14 N2 C11 107.8(8) C14 N2 C15 123.8(8) C11 N2 C15 128.4(8) C1 P1 P2 104.9(4) C1 P1 W1 117.4(3) P2 P1 W1 130.63(14) C1 P1 W3 106.9(3) P2 P1 W3 65.37(9) W1 P1 W3 119.78(10) C11 P2 P1 104.7(4) C11 P2 W2 120.3(4) P1 P2 W2 125.88(13) C11 P2 W3 105.7(3) P1 P2 W3 65.84(9) W2 P2 W3 121.74(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance W1 C10 2.002(9) W1 C6 2.046(10) W1 C8 2.048(12) W1 C9 2.059(9) W1 C7 2.061(9) W1 P1 2.556(2) W2 C20 1.982(9) W2 C16 2.031(10) W2 C19 2.045(11) W2 C17 2.054(12) W2 C18 2.056(9) W2 P2 2.564(3) W3 C22 2.043(10) W3 C25 2.044(9) W3 C23 2.055(9) W3 C21 2.067(10) W3 C24 2.077(9) W3 P2 2.605(2) W3 P1 2.615(2) C1 N1 1.395(12) C1 C2 1.404(14) C1 P1 1.823(11) C2 C3 1.402(14) C2 H2 0.9500 C3 C4 1.331(14) C3 H3 0.9500 C4 N1 1.371(12) C4 H4 0.9500 C5 N1 1.445(12) C5 H5A 0.9800 C5 H5B 0.9800 C5 H5C 0.9800 C6 O1 1.149(12) C7 O2 1.129(12) C8 O3 1.137(13) C9 O4 1.124(11) C10 O5 1.132(11) C11 C12 1.375(14) C11 N2 1.397(12) C11 P2 1.834(11) C12 C13 1.419(14) C12 H12 0.9500 C13 C14 1.358(14) C13 H13 0.9500 C14 N2 1.359(12) C14 H14 0.9500 C15 N2 1.444(12) C15 H15A 0.9800 C15 H15B 0.9800 C15 H15C 0.9800 C16 O6 1.145(12) C17 O7 1.142(14) C18 O8 1.132(12) C19 O9 1.159(13) C20 O10 1.146(12) C21 O11 1.126(12) C22 O12 1.135(12) C23 O13 1.119(12) C24 O14 1.131(12) C25 O15 1.131(11) P1 P2 2.156(4)