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_7131658
_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         'C20 H37 Ge N2, B C24 F20, 0.5(C6 H14)'
_chemical_formula_sum            'C47 H44 B F20 Ge N2'
_chemical_formula_weight         1100.24
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.1855(2)
_cell_length_b                   22.2471(3)
_cell_length_c                   22.8462(3)
_cell_measurement_reflns_used    18763
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      75.7200
_cell_measurement_theta_min      3.6370
_cell_volume                     9243.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_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_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -116.00 -23.00   1.00   10.00    --  -42.66 -19.00 120.00   93
  2  \w      3.00  29.00   1.00   10.00    --  -42.66  18.00  68.00   26
  3  \w     79.00 119.00   1.00   10.00    --   42.66 178.00-150.00   40
  4  \w     41.00  66.00   1.00   40.00    --  111.00 -45.00 -90.00   25
  5  \w     37.00 104.00   1.00   40.00    --  111.00 -95.00 150.00   67
  6  \w     83.00 109.00   1.00   40.00    --  111.00-113.00  77.00   26
  7  \w     60.00  87.00   1.00   40.00    --  111.00 -61.00 120.00   27
  8  \w     45.00  82.00   1.00   40.00    --  111.00 -61.00 150.00   37
  9  \w     43.00  70.00   1.00   40.00    --  111.00 -45.00  60.00   27
 10  \w    134.00 176.00   1.00   40.00    --  111.00  77.00-150.00   42
 11  \w     40.00  70.00   1.00   40.00    --  111.00 -45.00   0.00   30
 12  \w     85.00 178.00   1.00   40.00    --  111.00  15.00   0.00   93
 13  \w     41.00  72.00   1.00   40.00    --  111.00 -45.00-120.00   31
 14  \w     52.00  77.00   1.00   40.00    --  111.00 -61.00  30.00   25
 15  \w    -88.00 -42.00   1.00   10.00    --  -42.66 178.00-180.00   46
 16  \w   -125.00 -99.00   1.00   10.00    --  -42.66 178.00-180.00   26
 17  \w     89.00 119.00   1.00   10.00    --   42.66 178.00  90.00   30
 18  \w     42.00  72.00   1.00   40.00    --  111.00 -45.00-180.00   30
 19  \w     41.00  69.00   1.00   40.00    --  111.00 -45.00 -60.00   28
 20  \w     78.00 112.00   1.00   40.00    --  111.00-125.00  60.00   34
 21  \w    101.00 126.00   1.00   40.00    --  111.00 -77.00-150.00   25
 22  \w     77.00 103.00   1.00   40.00    --  111.00  15.00-150.00   26
 23  \w    147.00 172.00   1.00   40.00    --  111.00  15.00-150.00   25
 24  \w     39.00 112.00   1.00   40.00    --  111.00-125.00 -60.00   73
 25  \w     61.00  88.00   1.00   40.00    --  111.00 -61.00-120.00   27
 26  \w     42.00  68.00   1.00   40.00    --  111.00-125.00  60.00   26
 27  \w    118.00 166.00   1.00   40.00    --  111.00  61.00 -90.00   48
 28  \w     81.00 108.00   1.00   40.00    --  111.00-104.00-157.17   27
 29  \w    -37.00   7.00   1.00   10.00    --  -42.66  57.00  30.00   44
 30  \w     -4.00  36.00   1.00   10.00    --  -42.66  19.00 120.00   40
 31  \w    -11.00  18.00   1.00   10.00    --  -42.66  38.00 -30.00   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_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  0.0469
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            64509
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.666
_diffrn_reflns_theta_min         3.688
_exptl_absorpt_coefficient_mu    1.973
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.81a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_description       block
_exptl_crystal_F_000             4456
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         9607
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+3.2299P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0815
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7547
_reflns_number_total             9607
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01411h2.cif
_cod_data_source_block           compound-5
_cod_depositor_comments
'Adding full bibliography for 7131655--7131658.cif.'
_cod_database_code               7131658
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.827
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All Ge(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12), C15(H15), C18(H18)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C46(H46A,H46B), C47(H47A,H47B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5)
2.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,
 H20B,H20C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              74822
_shelx_hkl_checksum              71445
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;