#------------------------------------------------------------------------------ #$Date: 2009-11-14 13:09:05 +0000 (Sat, 14 Nov 2009) $ #$Revision: 846 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003335.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_2003335 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 569 _journal_page_last 571 _publ_section_title ; Bis(\h^5^-indenyl)tetrakis(\m~2~-iodo)dimolybdenum ; _chemical_formula_sum 'C18 H14 I4 Mo2' _chemical_formula_structural '(C9 H7) Mo I4 Mo (C9 H7)' _chemical_formula_weight 929.77 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _symmetry_space_group_name_H-M 'P -1' _cell_length_a 8.155(13) _cell_length_b 8.546(8) _cell_length_c 8.681(11) _cell_angle_alpha 102.47(9) _cell_angle_beta 117.42(11) _cell_angle_gamma 93.41(11) _cell_volume 515.5(12) _cell_formula_units_Z 1 _exptl_crystal_density_diffrn 2.995 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 16 _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 14.8 _exptl_absorpt_coefficient_mu 7.204 _cell_measurement_temperature 291(2) _exptl_crystal_description 'poorly formed block' _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.25 _exptl_crystal_colour black _chemical_compound_source ; The title compound was prepared in a two-stage synthetic procedure. In the first step, MoI~3~(thf)~3~ and sodium indenyl, NaC~9~H~7~, were reacted in THF to yield Na[(C~9~H~7~)MoI~3~]. The latter was further reacted with tetraphenylphosphonium iodide, PPh~4~I, in a mixture of THF and dichloromethane to give PPh~4~[(C~9~H~7~)MoI~3~]. From a dichloromethane solution of this compound, crystals of the title compound were obtained by cooling to 253 K. ; _diffrn_measurement_device 'Stoe-Siemens AED 4-circle diffractometer' _diffrn_measurement_method '\w-2\q scans' _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.610 _exptl_absorpt_correction_T_max 1.000 _diffrn_reflns_number 1443 _reflns_number_total 1356 _reflns_number_observed 994 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0242 _diffrn_reflns_theta_max 22.49 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 9 _diffrn_standards_number 1 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 180 _diffrn_standards_decay_% 15.6 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0467 _refine_ls_wR_factor_obs 0.1010 _refine_ls_wR_factor_all 0.1148 _refine_ls_goodness_of_fit_obs 1.063 _refine_ls_goodness_of_fit_all 1.020 _refine_ls_number_reflns 1356 _refine_ls_number_parameters 109 _refine_ls_hydrogen_treatment ; H atoms treated as riding atoms, C-H 0.93\%A ; _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+0.0000P] wh' _refine_ls_shift/esd_max 0.000 _refine_diff_density_max 1.108 _refine_diff_density_min -1.039 _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 'Mo' 'Mo' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' -1.6832 0. 'I' 'I' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' -0.4742 1.81 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 Mo1 1 -0.0410(2) 0.1060(2) 0.1130(2) 0.0273(4) I1 1 -0.27753(15) 0.03909(14) -0.26087(15) 0.0443(4) I2 1 -0.19230(15) -0.22821(13) 0.00659(15) 0.0390(4) C1 1 -0.180(2) 0.316(2) 0.154(2) 0.046(5) H1 1 -0.240(2) 0.360(2) 0.057(2) 0.056 C2 1 -0.257(2) 0.183(2) 0.178(2) 0.041(4) H2 1 -0.381(2) 0.127(2) 0.105(2) 0.050 C3 1 -0.119(3) 0.145(2) 0.335(2) 0.051(5) H3 1 -0.131(3) 0.058(2) 0.380(2) 0.061 C4 1 0.044(2) 0.271(2) 0.407(2) 0.042(4) C5 1 0.221(3) 0.298(2) 0.572(2) 0.053(5) H5 1 0.249(3) 0.227(2) 0.644(2) 0.064 C6 1 0.345(3) 0.435(3) 0.614(3) 0.068(6) H6 1 0.459(3) 0.459(3) 0.721(3) 0.082 C7 1 0.309(3) 0.542(2) 0.501(3) 0.050(5) H7 1 0.399(3) 0.634(2) 0.537(3) 0.060 C8 1 0.148(2) 0.513(2) 0.346(2) 0.039(4) H8 1 0.129(2) 0.580(2) 0.271(2) 0.047 C9 1 0.007(2) 0.378(2) 0.297(2) 0.040(4) 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 Mo1 0.0240(7) 0.0042(6) 0.0084(6) 0.0219(8) 0.0010(6) 0.0278(8) I1 0.0355(6) 0.0108(5) 0.0001(5) 0.0422(7) 0.0090(5) 0.0341(7) I2 0.0409(6) -0.0003(5) 0.0179(5) 0.0292(6) 0.0041(5) 0.0407(7) C1 0.046(11) 0.022(9) 0.015(9) 0.053(12) 0.001(9) 0.031(10) C2 0.030(6) 0.008(5) 0.027(5) 0.047(7) -0.002(5) 0.049(7) C3 0.062(12) 0.003(10) 0.028(10) 0.050(12) -0.006(9) 0.036(11) C4 0.054(11) -0.009(8) 0.026(9) 0.031(10) 0.000(8) 0.039(11) C5 0.064(13) -0.002(10) 0.020(10) 0.050(12) -0.003(9) 0.033(11) C6 0.052(13) 0.009(12) 0.029(11) 0.074(16) -0.014(12) 0.062(15) C7 0.044(11) -0.012(9) 0.032(11) 0.038(11) -0.007(10) 0.061(14) C8 0.043(10) -0.005(8) 0.013(9) 0.020(9) 0.000(8) 0.041(10) C9 0.033(9) 0.005(8) 0.012(8) 0.035(10) -0.010(8) 0.036(10)