Reactions of a hydrido(hydrogermylene)tungsten complex with some heterocumulenes: hydrogermylation and thermal rearrangement
Hashimoto, Hisako; Fukuda, Tetsuya; Tobita, Hiromi; New Journal of Chemistry 34 (2010) 1723–; doi:10.1039/c0nj00137f

data_7053534
_publ_section_title
;
 Reactions of a hydrido(hydrogermylene)tungsten complex with some
 heterocumulenes: hydrogermylation and thermal rearrangement
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1723
_journal_paper_doi               10.1039/c0nj00137f
_journal_volume                  34
_journal_year                    2010
_chemical_formula_moiety         'C29 H49 Ge N O3 Si3 W, C6 D6'
_chemical_formula_sum            'C35 H49 D6 Ge N O3 Si3 W'
_chemical_formula_weight         884.53
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 99.9596(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.8560(3)
_cell_length_b                   13.7380(5)
_cell_length_c                   15.9500(7)
_cell_measurement_reflns_used    8545
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      1.30
_cell_volume                     1911.29(13)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_molecular_graphics    ORTEP
_computing_publication_material
'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18067
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    3.920
_exptl_absorpt_correction_T_max  0.6098
_exptl_absorpt_correction_T_min  0.4658
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'NUMABS (Higashi, 1999)'
_exptl_crystal_colour            'reddish orange'
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.671
_refine_diff_density_min         -1.873
_refine_diff_density_rms         0.242
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.016(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         8545
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0525P)^2^+1.2974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0824
_reflns_number_gt                8291
_reflns_number_total             8545
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0nj00137f.txt
_cod_data_source_block           PhNCO
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7053534