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_7121442
_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         'C30 H31 F2 Ge N7, 2(C F3 O3 S)'
_chemical_formula_sum            'C32 H33 F8 Ge N7 O6 S2'
_chemical_formula_weight         900.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                90
_cell_angle_beta                 106.697(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2065(6)
_cell_length_b                   18.0706(8)
_cell_length_c                   14.8299(8)
_cell_measurement_reflns_used    9285
_cell_measurement_temperature    170
_cell_measurement_theta_max      26.948
_cell_measurement_theta_min      2.854
_cell_volume                     3646.6(3)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0950
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            103933
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.162
_diffrn_reflns_theta_min         2.854
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.050
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0690 before and 0.0609 after correction. The Ratio of minimum to maximum transmission is 0.9142. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_description       prism
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.798
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         8058
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0410P)^2^+6.0496P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1097
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6192
_reflns_number_total             8058
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc01799a2.cif
_cod_data_source_block           asrs11057_p21n
_cod_depositor_comments
'Adding full bibliography for 7121441--7121443.cif.'
_cod_database_code               7121442
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.854
_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.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C1(H1A,H1B), C2(H2A,H2B), C29(H29A,H29B), C25(H25A,H25B)
2.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C20(H20), C23(H23), C11(H11), C14(H14), C8(H8), C10(H10), C16(H16),
 C9(H9), C22(H22), C21(H21), C15(H15)
2.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              7283
_olex2_submission_special_instructions 'No special instructions were received'