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_4130437
_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         'C45 H17 F15 Ge N4'
_chemical_formula_sum            'C45 H17 F15 Ge N4'
_chemical_formula_weight         971.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-05-26
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.695(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.4990(19)
_cell_length_b                   35.608(7)
_cell_length_c                   26.043(6)
_cell_measurement_reflns_used    24148
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4824
_cell_measurement_theta_min      1.5781
_cell_volume                     7810(3)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2013)'
_computing_structure_solution
;
'SHELXS (Sheldrick, 2013)'
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device
;
Saturn724 (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0017
_diffrn_orient_matrix_UB_12      0.0024
_diffrn_orient_matrix_UB_13      0.1187
_diffrn_orient_matrix_UB_21      -0.0005
_diffrn_orient_matrix_UB_22      -0.0281
_diffrn_orient_matrix_UB_23      0.0006
_diffrn_orient_matrix_UB_31      0.0383
_diffrn_orient_matrix_UB_32      -0.0006
_diffrn_orient_matrix_UB_33      0.0058
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0680
_diffrn_reflns_av_unetI/netI     0.0733
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            55268
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.511
_diffrn_reflns_theta_min         1.678
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           30.0000
_diffrn_source_power             1.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.897
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8115
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_description       plate
_exptl_crystal_F_000             3856
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1299
_refine_ls_number_reflns         17576
_refine_ls_number_restraints     372
_refine_ls_restrained_S_all      1.192
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.0910
_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^)+(0.0186P)^2^+19.7421P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1465
_refine_ls_wR_factor_ref         0.1575
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14090
_reflns_number_total             17576
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b03547_si_003.cif
_cod_data_source_block           (TPFC)Ge-CH2CH2C6H5
_cod_database_code               4130437
_shelxl_version_number           2013-4
_diffrn_number_total             17891
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C41-C40 = C42-C41 = C45-C40 = C45-C44 = C44-C43 = C43-C42
 1.42 with sigma of 0.01
 C41B-C40B = C42B-C41B = C43B-C42B = C43A-C42A = C42A-C41A = C45B-C40B = C41A-
 C40A = C45A-C40A = C45A-C44A = C45B-C44B = C44A-C43A = C44B-C43B
 1.39 with sigma of 0.01
 C41C-C40C = C42C-C41C = C43C-C42C = C44C-C43C = C45C-C44C = C45C-C40C
 1.39 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C39C
\\sim C40C \\sim C41C \\sim C42C \\sim C43C \\sim C44C \\sim C45C: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C39A) \\sim Ueq, Uanis(C40A) \\sim Ueq, Uanis(C41A) \\sim Ueq,
Uanis(C42A) \\sim Ueq, Uanis(C43A) \\sim Ueq, Uanis(C44A) \\sim Ueq,
Uanis(C45A) \\sim Ueq, Uanis(C39B) \\sim Ueq, Uanis(C40B) \\sim Ueq,
Uanis(C45B) \\sim Ueq, Uanis(C44B) \\sim Ueq, Uanis(C43B) \\sim Ueq,
Uanis(C42B) \\sim Ueq, Uanis(C41B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42)
\\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq,
Uanis(C39C) \\sim Ueq, Uanis(C40C) \\sim Ueq, Uanis(C41C) \\sim Ueq,
Uanis(C42C) \\sim Ueq, Uanis(C43C) \\sim Ueq, Uanis(C44C) \\sim Ueq,
Uanis(C45C) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H38C)=Sof(H38D)=Sof(C39B)=Sof(H39C)=Sof(H39D)=Sof(C40B)=Sof(C45B)=
 Sof(H45B)=Sof(C44B)=Sof(H44B)=Sof(C43B)=Sof(H43B)=Sof(C42B)=Sof(H42B)=
 Sof(C41B)=Sof(H41B)=1-FVAR(1)
 Sof(H38A)=Sof(H38B)=Sof(C39A)=Sof(H39A)=Sof(H39B)=Sof(C40A)=Sof(C41A)=
 Sof(H41A)=Sof(C42A)=Sof(H42A)=Sof(C43A)=Sof(H43A)=Sof(C44A)=Sof(H44A)=
 Sof(C45A)=Sof(H45A)=FVAR(1)
 Sof(H38G)=Sof(H38H)=Sof(C39C)=Sof(H39G)=Sof(H39H)=Sof(C40C)=Sof(C41C)=
 Sof(H41C)=Sof(C42C)=Sof(H42C)=Sof(C43C)=Sof(H43C)=Sof(C44C)=Sof(H44C)=
 Sof(C45C)=Sof(H45C)=1-FVAR(2)
 Sof(H38E)=Sof(H38F)=Sof(C39)=Sof(H39E)=Sof(H39F)=Sof(C40)=Sof(C41)=Sof(H41)=
 Sof(C42)=Sof(H42)=Sof(C43)=Sof(H43)=Sof(C44)=Sof(H44)=Sof(C45)=Sof(H45)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C38A(H38A,H38B), C38A(H38C,H38D), C39A(H39A,H39B), C38(H38E,H38F), C38(H38G,
 H38H), C39(H39E,H39F), C39B(H39C,H39D), C39C(H39G,H39H)
5.b Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C3A(H3A), C7A(H7A), C8A(H8A), C12A(H12A), C13A(H13A), C17A(H17A),
 C18A(H18A), C41A(H41A), C42A(H42A), C43A(H43A), C44A(H44A), C45A(H45A), C2(H2),
  C3(H3), C7(H7), C8(H8), C12(H12), C13(H13), C17(H17), C18(H18), C41(H41),
 C42(H42), C43(H43), C44(H44), C45(H45), C45B(H45B), C44B(H44B), C43B(H43B),
 C42B(H42B), C41B(H41B), C41C(H41C), C42C(H42C), C43C(H43C), C44C(H44C),
 C45C(H45C)
;
_shelx_res_checksum              29324
_shelx_hkl_checksum              92618