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_4130438
_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 H24 F15 Ge N4 O2, C24 B F20'
_chemical_formula_sum            'C69 H24 B F35 Ge N4 O2'
_chemical_formula_weight         1689.32
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-11-24
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                94.292(5)
_cell_angle_beta                 95.582(4)
_cell_angle_gamma                98.626(4)
_cell_formula_units_Z            2
_cell_length_a                   13.1675(5)
_cell_length_b                   15.2199(9)
_cell_length_c                   19.0967(11)
_cell_measurement_reflns_used    3349
_cell_measurement_temperature    180.01(10)
_cell_measurement_theta_max      64.1980
_cell_measurement_theta_min      3.3820
_cell_volume                     3750.3(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      180.01(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0708
_diffrn_reflns_av_unetI/netI     0.1113
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21654
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.750
_diffrn_reflns_theta_min         3.416
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.769
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88337
_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            red
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       Block
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.029
_refine_diff_density_max         0.850
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1046
_refine_ls_number_reflns         13911
_refine_ls_number_restraints     148
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.1197
_refine_ls_R_factor_gt           0.0710
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0632P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1620
_refine_ls_wR_factor_ref         0.1975
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7716
_reflns_number_total             13911
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b03547_si_006.cif
_cod_data_source_block           '[(TPFC)Ge(THF)2][B(C6F5)4]'
_cod_database_code               4130438
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C68-C67 = C69-C68 = C67-C66
 1.54 with sigma of 0.01
 O2-C66 = O2-C69
 1.43 with sigma of 0.01
 O2-C69A = O2-C66A
 1.43 with sigma of 0.01
 C69A-C68A = C68A-C67A = C67A-C66A
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C68 \\sim C66 \\sim C67 \\sim C69 \\sim C69A \\sim C67A \\sim C66A \\sim C68A:
within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C68) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C69)
\\sim Ueq, Uanis(C69A) \\sim Ueq, Uanis(C68A) \\sim Ueq, Uanis(C67A) \\sim Ueq,
Uanis(C66A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C69A)=Sof(H69C)=Sof(H69D)=Sof(C68A)=Sof(H68C)=Sof(H68D)=Sof(C67A)=
 Sof(H67C)=Sof(H67D)=Sof(C66A)=Sof(H66C)=Sof(H66D)=1-FVAR(1)
 Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(C67)=Sof(H67A)=
 Sof(H67B)=Sof(C69)=Sof(H69A)=Sof(H69B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B), C68(H68A,
 H68B), C66(H66A,H66B), C67(H67A,H67B), C69(H69A,H69B), C69A(H69C,H69D),
 C68A(H68C,H68D), C67A(H67C,H67D), C66A(H66C,H66D)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C8(H8), C12(H12), C13(H13), C16(H16), C17(H17)
;
_shelx_res_checksum              55596
_shelx_hkl_checksum              34372
_shelx_fab_checksum              22965