Photochemical Reaction of Mo(CO)6with Et2GeH2: NMR and DFT Studies of Reaction Products; Crystal Structure of a Novel Complex [{Mo(μ-η2-H−GeEt2)(CO)4}2]
Zyder, Magdalena; Kochel, Andrzej; Handzlik, Jarosław; Szymańska-Buzar, Teresa; Organometallics 28 (2009) 5857–; doi:10.1021/om900299k

data_4069610
_publ_section_title
;
 Photochemical Reaction of Mo(CO)6with Et2GeH2: NMR and DFT Studies of
 Reaction Products; Crystal Structure of a Novel Complex
 [{Mo(\m-\h2-H&#x2212;GeEt2)(CO)4}2]
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              5857
_journal_paper_doi               10.1021/om900299k
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C16 H22 Ge2 Mo2 O8'
_chemical_formula_weight         679,44
_chemical_name_systematic
;
 Bis{(u-n2-hydridodiethylgermyl)tetracarbonylmolybdenum(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                 120.82(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.183(2)
_cell_length_b                   10.109(2)
_cell_length_c                   14.233(2)
_cell_measurement_reflns_used    2310
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.66
_cell_measurement_theta_min      2.99
_cell_volume                     1134.7(4)
_computing_cell_refinement
'KM4CCD Software, (Oxford Diffraction Poland Sp, 1995-2003'
_computing_data_collection
'KM4CCD Software, (Oxford Diffraction Poland Sp, 1995-2003'
_computing_data_reduction
'KM4CCD Software, (Oxford Diffraction Poland Sp, 1995-2003'
_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 0.999
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  KM4-CCD
_diffrn_measurement_method       /w
_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  0.0190
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9687
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.66
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    3.740
_exptl_absorpt_correction_T_max  0.678
_exptl_absorpt_correction_T_min  0.645
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'CrysAlis RED 1.171.30. Oxford Diffraction'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.989
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         2769
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0185
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0426
_refine_ls_wR_factor_ref         0.0441
_reflns_number_gt                2438
_reflns_number_total             2769
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900299k_si_002.cif
_cod_data_source_block           yelo
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4069610