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_4130436
_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_moiety         'C43 H14 F15 Ge N4, C24 B F20'
_chemical_formula_sum            'C67 H14 B F35 Ge N4'
_chemical_formula_weight         1623.22
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.166(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.836(3)
_cell_length_b                   10.6607(6)
_cell_length_c                   29.1236(19)
_cell_measurement_reflns_used    4422
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      70.0610
_cell_measurement_theta_min      3.5810
_cell_volume                     7537.8(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0646
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            22346
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.24
_diffrn_reflns_theta_min         3.64
_exptl_absorpt_coefficient_mu    1.719
_exptl_absorpt_correction_T_max  0.9039
_exptl_absorpt_correction_T_min  0.7250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'purple block'
_exptl_crystal_F_000             3184
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
;
_refine_diff_density_max         1.982
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     853
_refine_ls_number_reflns         13589
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.1310
_refine_ls_R_factor_gt           0.1020
_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^)+(0.1600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2715
_refine_ls_wR_factor_ref         0.2984
_reflns_number_gt                8525
_reflns_number_total             13589
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b03547_si_007.cif
_cod_data_source_block           5
_cod_original_cell_volume        7537.9(11)
_cod_original_sg_symbol_H-M      'P 2(1)/n'
_cod_database_code               4130436