Hafnocene-based Bicyclo[2.1.1]hexene Germylenes - Formation, Reactivity and Structural Flexibility.
Dong, Zhaowen; Bedbur, Katja; Schmidtmann, Marc; Müller, Thomas; Journal of the American Chemical Society  (2018) –; doi:10.1021/jacs.7b13536

data_4127176
_publ_section_title
;
 Hafnocene-based Bicyclo[2.1.1]hexene Germylenes - Formation, Reactivity
 and Structural Flexibility.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b13536
_journal_year                    2018
_chemical_formula_structural
'(C7H13N2)2 [GeC4(CH3)2(Si(CH3)3)2Hf(C5H5)(C5H4)] C5H5 *O(C2H5)2'
_chemical_formula_sum            'C45 H74 Ge Hf N4 O Si2'
_chemical_formula_weight         994.34
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                67.6273(15)
_cell_angle_beta                 86.9563(15)
_cell_angle_gamma                74.1423(16)
_cell_formula_units_Z            2
_cell_length_a                   11.6097(4)
_cell_length_b                   13.4515(5)
_cell_length_c                   17.1380(5)
_cell_measurement_reflns_used    9479
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      2.29
_cell_volume                     2376.85(14)
_computing_cell_refinement       'Bruker SAINT V8.34A'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT V8.34A'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            85298
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.034
_diffrn_reflns_theta_min         1.287
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.901
_exptl_absorpt_correction_T_max  0.8626
_exptl_absorpt_correction_T_min  0.5786
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS-2014/5 (Sheldrick)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.060
_refine_diff_density_max         5.712
_refine_diff_density_min         -1.088
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         13912
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+4.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1057
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11199
_reflns_number_total             13912
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b13536_si_003.cif
_cod_data_source_block           dzw77
_cod_original_cell_volume        2376.86(14)
_cod_database_code               4127176
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.568
_shelx_estimated_absorpt_t_max   0.845
_exptl_absorpt_special_details
;
 numerical absorption correction followed by correction based on
 symmetry-related measurements (multi-scan)
;
_shelx_res_checksum              89794
_shelx_hkl_checksum              86786