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_7121443
_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 H33 Ge N7, 2(C F3 O3 S)'
_chemical_formula_sum            'C32 H33 F6 Ge N7 O6 S2'
_chemical_formula_weight         862.40
_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'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 96.184(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7605(7)
_cell_length_b                   11.2818(5)
_cell_length_c                   21.5537(10)
_cell_measurement_reflns_used    9071
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      33.218
_cell_measurement_theta_min      2.776
_cell_volume                     3568.3(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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.9968
_diffrn_measured_fraction_theta_max 0.9968
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            116595
_diffrn_reflns_theta_full        33.2629
_diffrn_reflns_theta_max         33.26
_diffrn_reflns_theta_min         2.78
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.062
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.7103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0438 before and 0.0406 after correction. The Ratio of minimum to maximum transmission is 0.9515. The \l/2 correction factor is Not present.'
_exptl_crystal_density_diffrn    1.6051
_exptl_crystal_description       block
_exptl_crystal_F_000             1762.6963
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.9328
_refine_diff_density_min         -1.0728
_refine_diff_density_rms         0.0916
_refine_ls_d_res_high            0.6479
_refine_ls_d_res_low             7.3373
_refine_ls_goodness_of_fit_ref   1.0506
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    54
_refine_ls_number_parameters     490
_refine_ls_number_reflns         13707
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0506
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+2.2381P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0864
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              22
_reflns_limit_h_min              -22
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              33
_reflns_limit_l_min              0
_reflns_number_gt                11594
_reflns_number_total             13707
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8cc01799a2.cif
_cod_data_source_block           ASRS11052_P21c
_cod_depositor_comments
'Adding full bibliography for 7121441--7121443.cif.'
_cod_database_code               7121443
_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:
 C1(H1a,H1b), C3(H3a,H3b), C2(H2a,H2b), C27(H27a,H27b), C29(H29a,H29b),
 C25(H25a,H25b)
2.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C23(H23), C11(H11), C21(H21), C17(H17), C22(H22), C14(H14), C8(H8),
 C10(H10), C16(H16), C15(H15), C9(H9)
2.c Idealised Me refined as rotating group:
 C28(H28a,H28b,H28c), C30(H30a,H30b,H30c), C26(H26a,H26b,H26c)
;
_olex2_submission_special_instructions 'No special instructions were received'