Bis(η^5^-indenyl)tetrakis(μ-iodo)dimolybdenum(<i>Mo</i>—<i>Mo</i>)
Falvello, L. R.; Mattamana, S. P.; Poli, R.; Acta Crystallographica Section C 51 (1995) 569–571; doi:10.1107/S010827019400870X

data_2003335
_publ_section_title
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 Bis(\h^5^-indenyl)tetrakis(\m-iodo)dimolybdenum(<i>Mo</i>---<i>Mo</i>)
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_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              569
_journal_page_last               571
_journal_paper_doi               10.1107/S010827019400870X
_journal_volume                  51
_journal_year                    1995
_chemical_compound_source
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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.
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_chemical_formula_structural     '(C9 H7) Mo I4 Mo (C9 H7)'
_chemical_formula_sum            'C18 H14 I4 Mo2'
_chemical_formula_weight         929.77
_chemical_name_systematic
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 Bis(\h^5^-indenyl)tetrakis(\m~2~-iodo)dimolybdenum
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_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_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(13)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1988a)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1988b)'
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1991)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS-90 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291(2)
_diffrn_measurement_device       'Stoe-Siemens AED 4-circle diffractometer'
_diffrn_measurement_method       '\w-2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0743
_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_reflns_theta_min         2.48
_diffrn_standards_decay_%        15.6
_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_description       'poorly formed block'
_exptl_crystal_F_000             418
_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_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_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1356
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.022
_refine_ls_restrained_S_obs      1.065
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_obs          0.0467
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+0.0000P] wh'
_refine_ls_weighting_scheme      calc
_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)
_cod_data_source_file            fg1020.cif
_cod_data_source_block           xsmall
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+0.0000P] wh' was changed to 'calc'.
New tag '_refine_ls_weighting_details' was created. The value of the
new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+0.0000P] wh'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        515.5(12)
_cod_database_code               2003335