data_2003335
_publ_section_title
;
 Bis(\h^5^-indenyl)tetrakis(\m~2~-iodo)dimolybdenum
;
_journal_name_full               'Acta Crystallographica C'
_journal_page_first              569
_journal_page_last               571
_journal_volume                  51
_journal_year                    1995
_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.
;
_chemical_formula_structural     '(C9 H7) Mo I4 Mo (C9 H7)'
_chemical_formula_sum            'C18 H14 I4 Mo2'
_chemical_formula_weight         929.77
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                102.47(9)
_cell_angle_beta                 117.42(11)
_cell_angle_gamma                93.41(11)
_cell_formula_units_Z            1
_cell_length_a                   8.155(13)
_cell_length_b                   8.546(8)
_cell_length_c                   8.681(11)
_cell_measurement_reflns_used    16
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      14.8
_cell_measurement_theta_min      10.0
_cell_volume                     515.5(12)
_diffrn_measurement_device       'Stoe-Siemens AED 4-circle diffractometer'
_diffrn_measurement_method       '\w-2\q scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            1443
_diffrn_reflns_theta_max         22.49
_diffrn_standards_decay_%        15.6
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  180
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    7.204
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.610
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.995
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_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_thermal_history   'cooling to 253 K'
_refine_diff_density_max         1.108
_refine_diff_density_min         -1.039
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.020
_refine_ls_goodness_of_fit_obs   1.063
_refine_ls_hydrogen_treatment    ' H atoms treated as riding atoms, C-H 0.93\%A'
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1356
_refine_ls_R_factor_obs          0.0467
_refine_ls_shift/esd_max         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+0.0000P] wh'
_refine_ls_wR_factor_all         0.1148
_refine_ls_wR_factor_obs         0.1010
_reflns_number_observed          994
_reflns_number_total             1356
_reflns_observed_criterion       >2sigma(I)
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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)
