Metal Activation of a Germylenoid, a New Approach to Metal‒Germanium Triple Bonds: Synthesis and Reactions of the Germylidyne Complexes [Cp(CO)2M≡Ge‒C(SiMe3)3] (M = Mo, W)
Filippou, Alexander C.; Stumpf, Kai W.; Chernov, Oleg; Schnakenburg, Gregor; Organometallics 31 (2012) 748–; doi:10.1021/om201176n

data_4068179
_publ_section_title
;
 Metal Activation of a Germylenoid, a New Approach to Metal--Germanium
 Triple Bonds: Synthesis and Reactions of the Germylidyne Complexes
 [Cp(CO)2M\\tb Ge--C(SiMe3)3] (M = Mo, W)
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              748
_journal_paper_doi               10.1021/om201176n
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C17 H32 Ge O2 Si3 W'
_chemical_formula_sum            'C17 H32 Ge O2 Si3 W'
_chemical_formula_weight         609.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.938(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0559(3)
_cell_length_b                   22.4170(9)
_cell_length_c                   11.5366(3)
_cell_measurement_reflns_used    111
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      60.0
_cell_measurement_theta_min      3.0
_cell_volume                     2338.92(14)
_computing_cell_refinement       'STOE X-AREA (STOE&CIE, 2008)'
_computing_data_collection       'STOE X-AREA (STOE&CIE, 2008)'
_computing_data_reduction        'STOE X-RED (STOE&CIE, 2008)'
_computing_molecular_graphics    'DIAMOND2.1c (Brandenburg, 1999)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      ' 158 frames, detector distance = 100 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14159
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.79
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    6.360
_exptl_absorpt_correction_T_max  0.8380
_exptl_absorpt_correction_T_min  0.3364
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.295
_refine_diff_density_min         -2.323
_refine_diff_density_rms         0.152
_refine_ls_extinction_coef       0.00155(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.939
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         4571
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0449P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0776
_reflns_number_gt                3548
_reflns_number_total             4571
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201176n_si_001.cif
_cod_data_source_block           1-W
_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.

'_exptl_absorpt_correction_type' value 'Multi-Scan'
changed to 'multi-scan' 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_sg_symbol_H-M      'P 21/n'
_cod_database_code               4068179