C-H Activation of Cycloalkenes by Dimetallynes (M = Ge, Sn) under Ambient Conditions
Owen T. Summerscales; James C. Fettinger; Philip P. Power; Journal of the American Chemical Society 133 (2011) 11960–11963; doi:10.1021/ja205816d

data_4106542
_publ_section_title
;
 C-H Activation of Cycloalkenes by Dimetallynes (M = Ge, Sn) under Ambient
 Conditions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11960
_journal_page_last               11963
_journal_paper_doi               10.1021/ja205816d
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C42 H54 Ge'
_chemical_formula_sum            'C42 H54 Ge'
_chemical_formula_weight         631.44
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 95.87
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.8497(12)
_cell_length_b                   25.8968(11)
_cell_length_c                   17.0594(7)
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      2.43
_cell_volume                     6965.4(7)
_computing_cell_refinement       'SAINT (7.68A) (Bruker, 2009)'
_computing_data_collection       'Apex2 (2010-11.3) (Bruker, 2010)'
_computing_data_reduction        'SAINT (7.68A) (Bruker, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\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  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29533
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    0.907
_exptl_absorpt_correction_T_max  0.8775
_exptl_absorpt_correction_T_min  0.8662
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS 2008/2 (Sheldrick, 2008)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       Block
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         7988
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0278P)^2^+7.4731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0740
_refine_ls_wR_factor_ref         0.0790
_reflns_number_gt                6494
_reflns_number_total             7988
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja205816d_si_002.cif
_cod_data_source_block           ots34fmi
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4106542