Thermal reactions of an overcrowded germacyclopropabenzene with group 6 metal hexacarbonyl complexes [M(CO)6](M = Cr, Mo, and W): a novel mode of CO insertion leading to the formation of cyclic germoxycarbene metal complexes.
Tajima, Tomoyuki; Sasaki, Takayo; Sasamori, Takahiro; Takeda, Nobuhiro; Tokitoh, Norihiro; Chemical communications (Cambridge, England)  (2004) 402–403; doi:10.1039/b314010e

data_7102470
_publ_section_title
;
 Thermal reactions of an overcrowded germacyclopropabenzene with group
 6 metal hexacarbonyl complexes [M(CO)6](M = Cr, Mo, and W): a novel
 mode of CO insertion leading to the formation of cyclic germoxycarbene
 metal complexes.
;
_journal_issue                   4
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              402
_journal_page_last               403
_journal_paper_doi               10.1039/b314010e
_journal_year                    2004
_chemical_formula_moiety         'C51 H80 Ge O6 Si6 Cr'
_chemical_formula_sum            'C51 H80 Cr Ge O6 Si6'
_chemical_formula_weight         1082.28
_chemical_name_common            'Cr complex'
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.335(4)
_cell_angle_beta                 71.540(3)
_cell_angle_gamma                84.6841(17)
_cell_formula_units_Z            2
_cell_length_a                   11.8841(16)
_cell_length_b                   13.7144(8)
_cell_length_c                   19.8020(9)
_cell_measurement_temperature    103(2)
_cell_volume                     2985.9(5)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'RIGAKU/MSC Meacury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0521
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28396
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    0.847
_exptl_absorpt_correction_T_max  0.8488
_exptl_absorpt_correction_T_min  0.7851
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisum
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.048
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         10452
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0671P)^2^+1.1906P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1187
_reflns_number_gt                7940
_reflns_number_total             10452
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b314010e.txt
_cod_data_source_block           Cr(CO)6
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7102470