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_4068178
_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 Mo O2 Si3'
_chemical_formula_sum            'C17 H32 Ge Mo O2 Si3'
_chemical_formula_weight         521.23
_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                 93.0170(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0868(4)
_cell_length_b                   22.4891(10)
_cell_length_c                   11.4638(5)
_cell_measurement_reflns_used    9998
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.12
_cell_measurement_theta_min      2.54
_cell_volume                     2339.43(18)
_computing_cell_refinement       'Bruker SAINT (Bruker AXS, 2011)'
_computing_data_collection       'Bruker APEX2 (Bruker AXS, 2011)'
_computing_data_reduction        'Bruker SAINT (Bruker AXS, 2011)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_diffrn_measurement_method       'fine slicing \f and \w scans'
_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  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0140
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            54504
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.88
_exptl_absorpt_coefficient_mu    1.982
_exptl_absorpt_correction_T_max  0.8576
_exptl_absorpt_correction_T_min  0.3827
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2009)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         5627
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0154
_refine_ls_R_factor_gt           0.0147
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0158P)^2^+1.0229P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0384
_refine_ls_wR_factor_ref         0.0387
_reflns_number_gt                5445
_reflns_number_total             5627
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            om201176n_si_001.cif
_cod_data_source_block           1-Mo
_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 'Empirical'
changed to 'empirical' 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               4068178