#------------------------------------------------------------------------------ #$Date: 2008-01-13 23:15:36 +0100 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003379.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_2003379 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 571 _journal_page_last 573 _publ_section_title ; Bis(triphenylphosphine)iminium Tetrachlorooxomolybdenum(V) at 150 K ; _chemical_formula_moiety '[C36 H30 N P2]^+^[Cl4 Mo O]^-^' _chemical_formula_sum 'C36 H30 Cl4 Mo N O P2' _chemical_formula_analytical ; Found: C 54.26, H 4.02, Cl 18.10, Mo 11.95, N 1.69%, Calc: C 53.95, H 4.91, Cl 17.7, Mo 11.97, N 1.75 %. ; _chemical_formula_weight 792.29 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' '-x, -y, z+1/2' _symmetry_space_group_name_H-M 'P n a 21' _cell_length_a 21.470(6) _cell_length_b 16.765(2) _cell_length_c 9.6155(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3461.0(12) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'MoK\a' _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 44 _cell_measurement_theta_min 15 _cell_measurement_theta_max 16 _exptl_absorpt_coefficient_mu 0.811 _cell_measurement_temperature 150.0(2) _exptl_crystal_description Lath _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.19 _exptl_crystal_colour Green _diffrn_measurement_device 'Stoe Stadi-4 four-circle' _diffrn_measurement_method ; \w-\q scans with on-line profile analysis (Clegg, 1981) ; _exptl_absorpt_correction_type ; \y scans (North, Phillips & Mathews, 1968) ; _exptl_absorpt_correction_T_min 0.547 _exptl_absorpt_correction_T_max 0.621 _diffrn_reflns_number 3137 _reflns_number_total 2743 _reflns_number_observed 2416 _reflns_observed_criterion >4sigma(F) _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_theta_max 22.52 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 10 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 'not significant' _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0422 _refine_ls_wR_factor_obs 0.0780 _refine_ls_wR_factor_all 0.0872 _refine_ls_goodness_of_fit_obs 1.049 _refine_ls_goodness_of_fit_all 1.082 _refine_ls_number_reflns 2739 _refine_ls_number_parameters 407 _refine_ls_hydrogen_treatment ? _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(F~o~^2^) + 16.8557P] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_shift/esd_max -0.001 _refine_diff_density_max 0.487 _refine_diff_density_min -0.607 _refine_ls_extinction_method SHELXL93 _refine_ls_extinction_coef 0.00059(13) 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 'Cl' 'Cl' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.1484 0.1 'Mo' 'Mo' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' -1.6832 0. 'N' 'N' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0061 0.003 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0106 0.006 'P' 'P' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.1023 0.094 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881 _refine_ls_abs_structure_Flack -0.06(7) ; SIR92 (Altomare, Cascarano, Giacovazzo & Guagliardi, 1993) ; 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 Mo 1 0.32011(3) 0.88378(5) 0.75802(10) 0.0268(2) O 1 0.2755(3) 0.8043(4) 0.7710(10) 0.044(2) Cl1 1 0.29822(13) 0.9470(2) 0.5466(4) 0.0485(8) Cl2 1 0.25780(12) 0.9821(2) 0.8632(4) 0.0493(8) Cl3 1 0.38362(11) 0.8934(2) 0.9531(3) 0.0384(7) Cl4 1 0.40793(11) 0.8305(2) 0.6450(3) 0.0409(7) N 1 0.0690(3) 0.8135(4) 1.0281(9) 0.024(2) P1 1 0.04379(10) 0.87878(14) 0.9243(3) 0.0188(6) P2 1 0.10041(10) 0.72870(15) 1.0434(3) 0.0221(6) C1 1 -0.0386(4) 0.8890(5) 0.9480(10) 0.021(2) C2 1 -0.0747(4) 0.8207(5) 0.9599(11) 0.026(2) H2 1 -0.0566(4) 0.7696(5) 0.9465(11) 0.031 C3 1 -0.1377(4) 0.8277(6) 0.9917(11) 0.031(3) H3 1 -0.1623(4) 0.7809(6) 1.0014(11) 0.037 C4 1 -0.1651(4) 0.9008(6) 1.0092(11) 0.032(3) H4 1 -0.2081(4) 0.9046(6) 1.0311(11) 0.038 C5 1 -0.1298(4) 0.9687(6) 0.9949(11) 0.029(3) H5 1 -0.1487(4) 1.0196(6) 1.0056(11) 0.035 C6 1 -0.0669(4) 0.9635(5) 0.9653(11) 0.024(2) H6 1 -0.0428(4) 1.0108(5) 0.9565(11) 0.028 C7 1 0.0795(4) 0.9733(5) 0.9599(10) 0.021(2) C8 1 0.1033(4) 0.9872(6) 1.0935(11) 0.029(3) H8 1 0.1006(4) 0.9473(6) 1.1633(11) 0.035 C9 1 0.1308(4) 1.0605(6) 1.1219(12) 0.028(2) H9 1 0.1476(4) 1.0708(6) 1.2115(12) 0.034 C10 1 0.1337(4) 1.1185(6) 1.0201(12) 0.029(3) H10 1 0.1522(4) 1.1686(6) 1.0406(12) 0.035 C11 1 0.1102(4) 1.1046(6) 0.8895(11) 0.029(2) H11 1 0.1125(4) 1.1448(6) 0.8201(11) 0.034 C12 1 0.0830(4) 1.0317(6) 0.8594(11) 0.031(3) H12 1 0.0668(4) 1.0219(6) 0.7691(11) 0.037 C13 1 0.0611(4) 0.8551(5) 0.7448(12) 0.025(2) C14 1 0.0140(4) 0.8375(5) 0.6520(11) 0.025(2) H14 1 -0.0285(4) 0.8426(5) 0.6778(11) 0.030 C15 1 0.0309(4) 0.8116(5) 0.5183(11) 0.027(3) H15 1 -0.0007(4) 0.7979(5) 0.4532(11) 0.033 C16 1 0.0914(5) 0.8060(6) 0.4809(12) 0.036(3) H16 1 0.1020(5) 0.7896(6) 0.3893(12) 0.043 C17 1 0.1385(4) 0.8239(6) 0.5752(11) 0.030(3) H17 1 0.1809(4) 0.8185(6) 0.5487(11) 0.036 C18 1 0.1234(4) 0.8497(6) 0.7080(10) 0.025(2) H18 1 0.1552(4) 0.8633(6) 0.7726(10) 0.029 C19 1 0.0492(4) 0.6651(5) 1.1388(11) 0.021(2) C20 1 0.0005(4) 0.6971(6) 1.2127(10) 0.027(2) H20 1 -0.0063(4) 0.7531(6) 1.2102(10) 0.033 C21 1 -0.0386(4) 0.6497(6) 1.2901(12) 0.035(3) H21 1 -0.0732(4) 0.6726(6) 1.3369(12) 0.042 C22 1 -0.0276(5) 0.5687(7) 1.2997(12) 0.042(3) H22 1 -0.0536(5) 0.5360(7) 1.3560(12) 0.050 C23 1 0.0213(4) 0.5357(5) 1.2269(13) 0.039(3) H23 1 0.0289(4) 0.4800(5) 1.2335(13) 0.047 C24 1 0.0595(4) 0.5821(5) 1.1448(12) 0.028(2) H24 1 0.0924(4) 0.5585(5) 1.0929(12) 0.034 C25 1 0.1192(4) 0.6778(5) 0.8821(11) 0.021(2) C26 1 0.0708(4) 0.6572(5) 0.7913(11) 0.027(3) H26 1 0.0288(4) 0.6692(5) 0.8151(11) 0.032 C27 1 0.0841(5) 0.6198(5) 0.6681(12) 0.033(3) H27 1 0.0514(5) 0.6067(5) 0.6055(12) 0.039 C28 1 0.1443(5) 0.6012(6) 0.6354(13) 0.040(3) H28 1 0.1532(5) 0.5755(6) 0.5496(13) 0.048 C29 1 0.1921(4) 0.6192(6) 0.7249(12) 0.040(3) H29 1 0.2336(4) 0.6044(6) 0.7023(12) 0.048 C30 1 0.1798(5) 0.6592(6) 0.8485(12) 0.032(3) H30 1 0.2129(5) 0.6735(6) 0.9093(12) 0.038 C31 1 0.1706(4) 0.7421(5) 1.1409(11) 0.026(2) C32 1 0.1904(4) 0.6840(6) 1.2373(12) 0.032(3) H32 1 0.1690(4) 0.6348(6) 1.2472(12) 0.038 C33 1 0.2422(4) 0.7015(7) 1.3168(11) 0.037(3) H33 1 0.2559(4) 0.6633(7) 1.3832(11) 0.044 C34 1 0.2749(4) 0.7719(6) 1.3040(12) 0.037(3) H34 1 0.3099(4) 0.7825(6) 1.3616(12) 0.044 C35 1 0.2560(4) 0.8259(6) 1.2077(12) 0.032(3) H35 1 0.2789(4) 0.8739(6) 1.1964(12) 0.038 C36 1 0.2041(4) 0.8124(6) 1.1254(11) 0.029(2) H36 1 0.1916(4) 0.8509(6) 1.0587(11) 0.034 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 Mo 0.0223(4) -0.0009(4) -0.0007(5) 0.0248(4) -0.0028(6) 0.0334(5) O 0.035(3) -0.009(3) -0.004(5) 0.026(3) -0.007(5) 0.071(6) Cl1 0.049(2) 0.0017(13) -0.015(2) 0.049(2) 0.007(2) 0.047(2) Cl2 0.0359(14) 0.0083(13) 0.006(2) 0.045(2) -0.007(2) 0.067(2) Cl3 0.0411(14) 0.0006(13) -0.0047(13) 0.044(2) -0.0020(15) 0.030(2) Cl4 0.0340(14) 0.0081(12) 0.0026(14) 0.048(2) -0.009(2) 0.041(2) N 0.034(5) 0.003(4) 0.001(4) 0.018(4) -0.001(4) 0.020(5) P1 0.0164(11) 0.0007(10) -0.0007(11) 0.0223(14) 0.0012(13) 0.0178(14) P2 0.0200(12) 0.0010(10) -0.0015(13) 0.0279(13) 0.0024(13) 0.0182(13) C1 0.022(5) -0.001(4) 0.006(5) 0.022(5) 0.005(5) 0.017(5) C2 0.019(5) 0.004(4) 0.001(5) 0.022(5) -0.003(5) 0.035(7) C3 0.024(5) -0.010(5) 0.004(5) 0.037(6) -0.003(6) 0.032(7) C4 0.023(5) 0.006(5) 0.006(5) 0.049(7) -0.010(6) 0.024(6) C5 0.029(5) 0.008(4) -0.003(5) 0.027(6) -0.022(5) 0.031(6) C6 0.021(5) 0.001(4) -0.002(5) 0.024(5) 0.001(5) 0.026(6) C7 0.017(5) -0.004(4) 0.004(5) 0.024(5) 0.001(5) 0.021(6) C8 0.022(5) -0.002(5) 0.000(5) 0.039(6) 0.000(5) 0.027(6) C9 0.025(5) -0.003(4) 0.002(5) 0.032(6) -0.005(6) 0.029(6) C10 0.019(5) -0.003(4) 0.007(5) 0.023(6) -0.010(6) 0.045(7) C11 0.021(5) -0.002(5) 0.007(5) 0.028(6) 0.002(5) 0.037(7) C12 0.021(5) -0.005(5) 0.004(5) 0.040(6) 0.000(6) 0.030(6) C13 0.026(5) -0.007(4) 0.004(6) 0.030(5) 0.008(6) 0.019(6) C14 0.026(5) -0.003(4) -0.009(5) 0.023(5) -0.011(5) 0.025(6) C15 0.031(6) 0.006(4) -0.005(5) 0.023(5) -0.009(5) 0.028(7) C16 0.050(7) 0.003(6) 0.000(6) 0.040(7) -0.011(6) 0.017(6) C17 0.020(5) -0.003(5) 0.019(5) 0.037(6) 0.005(6) 0.034(7) C18 0.026(5) -0.004(4) 0.008(4) 0.033(5) -0.002(4) 0.015(5) C19 0.028(5) -0.001(4) -0.008(5) 0.019(5) 0.002(5) 0.017(5) C20 0.024(5) -0.002(5) -0.004(5) 0.035(5) -0.002(5) 0.022(6) C21 0.022(5) 0.002(5) 0.002(5) 0.043(6) 0.001(6) 0.040(8) C22 0.037(6) -0.012(5) 0.005(6) 0.052(7) 0.014(6) 0.036(8) C23 0.043(6) -0.009(5) -0.002(6) 0.020(5) 0.004(6) 0.054(9) C24 0.027(5) -0.006(4) -0.013(5) 0.021(5) 0.004(5) 0.036(6) C25 0.022(5) -0.003(4) 0.012(5) 0.020(5) 0.006(5) 0.021(6) C26 0.027(5) -0.005(4) 0.007(5) 0.018(5) -0.002(5) 0.035(8) C27 0.040(6) -0.011(5) -0.005(6) 0.019(5) 0.001(6) 0.039(7) C28 0.046(6) -0.012(5) 0.010(6) 0.040(7) -0.016(6) 0.035(7) C29 0.029(5) 0.012(5) 0.019(6) 0.050(7) -0.008(7) 0.041(9) C30 0.021(5) 0.002(5) -0.006(5) 0.035(6) 0.004(6) 0.040(7) C31 0.019(5) 0.002(4) 0.007(5) 0.025(5) -0.007(5) 0.034(6) C32 0.023(5) -0.001(4) -0.003(6) 0.039(5) 0.010(6) 0.035(7) C33 0.023(5) 0.008(5) -0.007(5) 0.056(7) 0.000(6) 0.032(6) C34 0.017(5) 0.012(5) -0.003(5) 0.049(7) -0.015(6) 0.043(8) C35 0.030(5) -0.004(4) 0.000(5) 0.024(5) 0.000(5) 0.042(7) C36 0.017(5) 0.006(4) 0.001(5) 0.041(6) 0.009(6) 0.028(6)