An intramolecular phosphine-oxide stabilized germanium(iv) di-cation with enhanced Lewis acidity and catalytic applications
Kumari, Akanksha; Peddi, Balakrishna; Yildiz, Cem. B.; Majumdar, Moumita; Chemical Communications 61 (2025) 6506–6509; doi:10.1039/D5CC00250H

data_7134361
_publ_section_title
;
 An intramolecular phosphine-oxide stabilized germanium(iv) di-cation with
 enhanced Lewis acidity and catalytic applications
;
_journal_issue                   35
_journal_name_full               'Chemical Communications'
_journal_page_first              6506
_journal_page_last               6509
_journal_paper_doi               10.1039/D5CC00250H
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C36 H44 F Ge O2 P2, C F3 O3 S, 2(C4 H8 O)'
_chemical_formula_sum            'C45 H60 F4 Ge O7 P2 S'
_chemical_formula_weight         955.52
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2025-01-13
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-01-13 deposited with the CCDC.	2025-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                73.204(3)
_cell_angle_beta                 72.985(3)
_cell_angle_gamma                81.658(3)
_cell_formula_units_Z            2
_cell_length_a                   12.3052(13)
_cell_length_b                   12.8654(14)
_cell_length_c                   15.2505(16)
_cell_measurement_reflns_used    9030
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      2.21
_cell_volume                     2205.3(4)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0594
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            53849
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.148
_diffrn_reflns_theta_max         25.148
_diffrn_reflns_theta_min         1.942
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.882
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1031 before and 0.0649 after correction.
The Ratio of minimum to maximum transmission is 0.9075.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         7874
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0289P)^2^+3.9104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0943
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6367
_reflns_number_total             7874
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc00250h2.cif
_cod_data_source_block           new
_cod_depositor_comments
'Adding full bibliography for 7134358--7134361.cif.'
_cod_database_code               7134361
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.933
_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 Ternary CH refined with riding coordinates:
 C35(H35), C28(H28), C31(H31), C25(H25)
2.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C13(H13A,H13B), C1(H1A,H1B), C10(H10A,H10B), C44(H44A,H44B),
 C45(H45A,H45B), C40(H40A,H40B), C43(H43A,H43B), C42(H42A,H42B), C38(H38A,H38B),
  C39(H39A,H39B), C41(H41A,H41B)
2.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C15(H15), C4(H4), C19(H19), C20(H20), C7(H7), C3(H3), C8(H8)
2.d Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C29(H29A,H29B,H29C), C27(H27A,H27B,H27C), C32(H32A,H32B,
 H32C), C34(H34A,H34B,H34C), C33(H33A,H33B,H33C), C30(H30A,H30B,H30C), C26(H26A,
 H26B,H26C)
;
_shelx_res_checksum              20011
_shelx_hkl_checksum              26788
_olex2_exptl_crystal_mounting_method 150K
_olex2_submission_special_instructions 'No special instructions were received'