Photochemical Reaction of Mo(CO)6with Et2SiH2: Spectroscopic Characterization and Crystal Structure of the Bis{(μ-η2-hydridodiethylsilyl)tetracarbonylmolybdenum(I)} Complex [{Mo(μ-η2-H−SiEt2)(CO)4}2]
Stosur, Magdalena; Kochel, Andrzej; Keller, Antoni; Szymańska-Buzar, Teresa; Organometallics 25 (2006) 3791–; doi:10.1021/om060290d

data_4075456
_publ_section_title
;
 Photochemical Reaction of Mo(CO)6with Et2SiH2:&#x00A0; Spectroscopic
 Characterization and Crystal Structure of the
 Bis{(\m-\h2-hydridodiethylsilyl)tetracarbonylmolybdenum(I)} Complex
 [{Mo(\m-\h2-H&#x2212;SiEt2)(CO)4}2]
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3791
_journal_paper_doi               10.1021/om060290d
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C16 H22 Mo2 O8 Si2'
_chemical_formula_weight         590.40
_chemical_name_systematic
;
 bis{(m-h2-hydridodiethylsilyl)tetracarbonyl-molybdenum(I)}
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 120.638(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.1424(8)
_cell_length_b                   10.0636(9)
_cell_length_c                   14.1503(13)
_cell_measurement_reflns_used    2151
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.45
_cell_measurement_theta_min      3.03
_cell_volume                     1120.16(19)
_computing_cell_refinement
'KM4 CCD Software (Oxford Diffraction  Poland Sp,  (1995-2005)'
_computing_data_collection
'KM4 CCD Software (Oxford Diffraction  Poland Sp, (1995-2005)'
_computing_data_reduction
'KM4 CCD Software (Oxford Diffraction  Poland Sp, (1995-2005)'
_computing_molecular_graphics    'ORTEP III Farrugia 1997'
_computing_publication_material  'SHELXL-97 Sheldrick 1997'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  KM4-CCD
_diffrn_measurement_method       '/w scan'
_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  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8669
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.45
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    1.264
_exptl_absorpt_correction_T_max  0.897
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrysAlis 1.171.13, Oxford Diffraction'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.154
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         2628
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0243
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+0.3118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0552
_refine_ls_wR_factor_ref         0.0570
_reflns_number_gt                2316
_reflns_number_total             2628
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060290dsi20060516_075844.cif
_cod_data_source_block           ms01dc
_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_original_cell_volume        1120.16(17)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4075456