Synthesis, Electronic Structure, and Reactivity Studies of a 4-Coordinate Square Planar Germanium(IV) Cation.
Fang, Huayi; Jing, Huize; Zhang, Aixi; Ge, Haonan; Yao, Zhengmin; Brothers, Penelope J.; Fu, Xuefeng; Journal of the American Chemical Society 138 (2016) 7705–7710; doi:10.1021/jacs.6b03547

data_4130439
_publ_section_title
;
 Synthesis, Electronic Structure, and Reactivity Studies of a 4-Coordinate
 Square Planar Germanium(IV) Cation.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7705
_journal_page_last               7710
_journal_paper_doi               10.1021/jacs.6b03547
_journal_volume                  138
_journal_year                    2016
_chemical_formula_sum            'C43 H13 F15 Ge N4'
_chemical_formula_weight         943.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 93.376(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.5561(8)
_cell_length_b                   19.0714(8)
_cell_length_c                   17.2328(8)
_cell_measurement_reflns_used    6916
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.13
_cell_measurement_theta_min      2.37
_cell_volume                     7072.2(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0716
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            60086
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.413
_diffrn_reflns_theta_min         2.368
_exptl_absorpt_coefficient_mu    0.988
_exptl_absorpt_correction_T_max  0.7554
_exptl_absorpt_correction_T_min  0.6286
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2011)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_description       plate
_exptl_crystal_F_000             3728
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.958
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         7241
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+21.2234P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1176
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5716
_reflns_number_total             7241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b03547_si_002.cif
_cod_data_source_block           (TPFC)Ge-C6H5
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4130439
_shelx_estimated_absorpt_t_min   0.812
_shelx_estimated_absorpt_t_max   0.866
_shelxl_version_number           2014/6
_shelx_res_checksum              92378
_shelx_hkl_checksum              5015