Redox flexibility in a germanium hydride manifold: hydrogen shuttling <i>via</i> oxidative addition and reductive elimination.
Caise, Alexa; Hicks, Jamie; Heilmann, Andreas; Aldridge, Simon; Chemical communications (Cambridge, England) 59 (2023) 7251–7254; doi:10.1039/d3cc01411h

data_7131656
_publ_section_title
;
 Redox flexibility in a germanium hydride manifold: hydrogen shuttling
 <i>via</i> oxidative addition and reductive elimination.
;
_journal_issue                   47
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7251
_journal_page_last               7254
_journal_paper_doi               10.1039/d3cc01411h
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C30 H42 Ge N2 O'
_chemical_formula_sum            'C30 H42 Ge N2 O'
_chemical_formula_weight         519.24
_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             2023-02-15
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-16 deposited with the CCDC.	2023-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                102.491(3)
_cell_angle_beta                 100.285(3)
_cell_angle_gamma                93.091(4)
_cell_formula_units_Z            2
_cell_length_a                   8.2011(3)
_cell_length_b                   10.5814(6)
_cell_length_c                   16.5784(5)
_cell_measurement_reflns_used    8407
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      75.9920
_cell_measurement_theta_min      5.4860
_cell_volume                     1375.61(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector_area_resol_mean 10.4102
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13167
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.498
_diffrn_reflns_theta_min         4.300
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.681
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96121
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_description       block
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         5678
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+0.3289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0744
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5403
_reflns_number_total             5678
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01411h2.cif
_cod_data_source_block           compound-3
_cod_depositor_comments
'Adding full bibliography for 7131655--7131658.cif.'
_cod_database_code               7131656
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.877
_shelx_estimated_absorpt_t_min   0.719
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
N1 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
N1A \\sim C9A \\sim C10A \\sim C11A \\sim C12A \\sim C13A \\sim C14A: within 2A
with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
3. Others
 Sof(H7BC)=Sof(H7BD)=Sof(N1A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10D)=Sof(H10E)=
 Sof(H10F)=Sof(C11A)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C12A)=Sof(H12A)=
 Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C14A)=Sof(H14D)=Sof(H14E)=
 Sof(H14F)=1-FVAR(1)
 Sof(H7AA)=Sof(H7AB)=Sof(N1)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10A)=Sof(H10B)=
 Sof(H10C)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12)=Sof(H12)=Sof(C13)=
 Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C15(H15), C18(H18), C9(H9), C12(H12), C9A(H9A), C12A(H12A)
4.b Secondary CH2 refined with riding coordinates:
 C7(H7AA,H7AB), C7(H7BC,H7BD), C8(H8A,H8B)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27),
 C28(H28), C29(H29)
4.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,
 H14B,H14C), C10A(H10D,H10E,H10F), C11A(H11D,H11E,H11F), C13A(H13D,H13E,H13F),
 C14A(H14D,H14E,H14F)
;
_shelx_res_checksum              60348
_shelx_hkl_checksum              35116
_olex2_submission_special_instructions 'No special instructions were received'