Oxidation of a germanium(ii) dication to access cationic germanium(iv) fluorides.
Suter, Riccardo; Swidan, Ala'aeddeen; Macdonald, Charles L. B.; Burford, Neil; Chemical communications (Cambridge, England) 54 (2018) 4140–4143; doi:10.1039/c8cc01799a

data_7121441
_publ_section_title
;
 Oxidation of a germanium(ii) dication to access cationic germanium(iv)
 fluorides.
;
_journal_issue                   33
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4140
_journal_page_last               4143
_journal_paper_doi               10.1039/c8cc01799a
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C31 H33 F4 Ge N7 O3 S, 2(C F3 O3 S), C2 H3 N'
_chemical_formula_sum            'C35 H36 F10 Ge N8 O9 S3'
_chemical_formula_weight         1071.49
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-11-22 deposited with the CCDC.
2018-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                84.79(14)
_cell_angle_beta                 80.30(13)
_cell_angle_gamma                88.99(12)
_cell_formula_units_Z            2
_cell_length_a                   11.55(3)
_cell_length_b                   14.24(3)
_cell_length_c                   14.38(3)
_cell_measurement_reflns_used    6387
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      24.137
_cell_measurement_theta_min      2.890
_cell_volume                     2322(9)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.968
_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  0.0893
_diffrn_reflns_av_unetI/netI     0.0814
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            31482
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.442
_diffrn_reflns_theta_min         2.872
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.892
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6154
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0730 before and 0.0624 after correction. The Ratio of minimum to maximum transmission is 0.8258. The \l/2 correction factor is Not present.'
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_description       prism
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.277
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     672
_refine_ls_number_reflns         8328
_refine_ls_number_restraints     254
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.1631
_refine_ls_R_factor_gt           0.0972
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1256P)^2^+26.6558P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2478
_refine_ls_wR_factor_ref         0.3124
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5228
_reflns_number_total             8328
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc01799a2.cif
_cod_data_source_block           asrs11111_p-1
_cod_depositor_comments
'Adding full bibliography for 7121441--7121443.cif.'
_cod_original_cell_volume        2323(9)
_cod_database_code               7121441
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.776
_shelx_estimated_absorpt_t_min   0.722
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C33'-S3'
 1.824 with sigma of 0.02
 C33-S3
 1.824 with sigma of 0.02
 C33'-F9' \\sim C33'-F7' \\sim C33'-F13
 with sigma of 0.02
 F9'-F7' \\sim F7'-F13 \\sim F13-F9'
 with sigma of 0.04
 S3'-F9' \\sim S3'-F7' \\sim S3'-F13
 with sigma of 0.04
 S3'-O7' \\sim S3'-O9' \\sim S3'-O8'
 with sigma of 0.02
 O7'-O9' \\sim O9'-O8' \\sim O7'-O8'
 with sigma of 0.04
 C33'-O7' \\sim C33'-O9' \\sim C33'-O8'
 with sigma of 0.04
 C33-F8' \\sim C33-F7 \\sim C33-F9
 with sigma of 0.02
 F8'-F7 \\sim F7-F9 \\sim F9-F8'
 with sigma of 0.04
 S3-F8' \\sim S3-F7 \\sim S3-F9
 with sigma of 0.04
 S3-O7 \\sim S3-O8 \\sim S3-O9
 with sigma of 0.02
 O7-O8 \\sim O8-O9 \\sim O7-O9
 with sigma of 0.04
 C33-O7 \\sim C33-O8 \\sim C33-O9
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C33' \\sim F9' \\sim F7' \\sim F13 \\sim S3' \\sim O7' \\sim O9' \\sim O8':
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C33 \\sim F8' \\sim F7 \\sim F9 \\sim S3 \\sim O7 \\sim O8 \\sim O9: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08
C33' \\sim C33: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
S3' \\sim S3: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
O7' \\sim O7: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
F9' \\sim F8': within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C33', F9', F7', F13, S3', O7', O9', O8'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C33, F8', F7, F9, S3, O7, O8, O9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C33)=Sof(F8')=Sof(F7)=Sof(F9)=Sof(O7)=Sof(O8)=Sof(O9)=1-FVAR(1)
 Sof(C33')=Sof(F9')=Sof(F7')=Sof(F13)=Sof(O7')=Sof(O9')=Sof(O8')=FVAR(1)
 Fixed Sof: S3(0.28) S3'(0.72)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C29(H29A,H29B), C3(H3A,H3B), C2(H2A,H2B), C25(H25A,H25B),
 C27(H27A,H27B)
6.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C20(H20), C17(H17), C16(H16), C10(H10), C15(H15), C23(H23),
 C21(H21), C22(H22), C14(H14), C8(H8), C9(H9)
6.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C30(H30A,H30B,H30C), C28(H28A,H28B,H28C), C35(H35A,H35B,
 H35C)
;
_shelx_res_checksum              79817
_shelx_fab_checksum              12926
_olex2_submission_special_instructions 'No special instructions were received'