Manganese germylene hydride complexes: reactivity with carbon dioxide, benzophenone, and diisopropylcarbodiimide.
Price, Jeffrey S.; Emslie, David J. H.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 14821–14837; doi:10.1039/d5dt01701g

data_7719474
_publ_section_title
;
 Manganese germylene hydride complexes: reactivity with carbon dioxide,
 benzophenone, and diisopropylcarbodiimide.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14821
_journal_page_last               14837
_journal_paper_doi               10.1039/d5dt01701g
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C23 H48 Ge Mn N P4'
_chemical_formula_sum            'C23 H48 Ge Mn N P4'
_chemical_formula_weight         590.03
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-08-12
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-07-16 deposited with the CCDC.	2025-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                89.364(19)
_cell_angle_beta                 74.516(18)
_cell_angle_gamma                89.79(2)
_cell_formula_units_Z            4
_cell_length_a                   12.406(5)
_cell_length_b                   14.090(6)
_cell_length_c                   17.415(7)
_cell_measurement_reflns_used    2287
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.566
_cell_measurement_theta_min      2.307
_cell_volume                     2933(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
432 frames, detector distance = 100.0 mm
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0875
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33576
_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         29.130
_diffrn_reflns_theta_min         1.703
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.685
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0535 before and 0.0366 after correction.
The Ratio of minimum to maximum transmission is 0.7874.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.853
_refine_diff_density_min         -1.053
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         15716
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0319P)^2^+9.0666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1358
_refine_ls_wR_factor_ref         0.1457
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12659
_reflns_number_total             15716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01701g3.cif
_cod_data_source_block           MnGeH2Ph_CNtBu_cis
_cod_depositor_comments
'Adding full bibliography for 7719468--7719476.cif.'
_cod_database_code               7719474
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.678
_shelx_estimated_absorpt_t_min   0.552
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9594(7)
 0.0406(7)
2. 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
3. Restrained distances
 H1A-Ge1 \\sim Ge1-H1B \\sim H1AB-Ge1A \\sim Ge1A-H1AA
 with sigma of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C20(H20A,H20B), C21(H21A,H21B), C14A(H14C,
 H14D), C15A(H15C,H15D), C20A(H20C,H20D), C21A(H21C,H21D)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C2A(H2A), C3A(H3A), C4A(H4A),
 C5A(H5A), C6A(H6A)
4.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,
 H18B,H18C), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C),
 C9A(H9AA,H9AB,H9AC), C10A(H10D,H10E,H10F), C11A(H11D,H11E,H11F), C12A(H12D,
 H12E,H12F), C13A(H13D,H13E,H13F), C16A(H16D,H16E,H16F), C17A(H17D,H17E,H17F),
 C18A(H18D,H18E,H18F), C19A(H19D,H19E,H19F), C22A(H22D,H22E,H22F), C23A(H23D,
 H23E,H23F)
;
_shelx_res_checksum              9244
_olex2_submission_special_instructions 'No special instructions were received'