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_7719472
_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      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-07-12
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-07-16 deposited with the CCDC.	2025-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.847(7)
_cell_length_b                   14.761(6)
_cell_length_c                   10.530(4)
_cell_measurement_reflns_used    725
_cell_measurement_temperature    100
_cell_measurement_theta_max      19.37
_cell_measurement_theta_min      2.61
_cell_volume                     2929(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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
430 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  0.0996
_diffrn_reflns_av_unetI/netI     0.0984
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            27778
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         1.752
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.687
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5447
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0714 before and 0.0617 after correction.
The Ratio of minimum to maximum transmission is 0.7304.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       plate
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Flack x determined using 2037 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         6716
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0425
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0959
_reflns_Friedel_coverage         0.896
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                5263
_reflns_number_total             6716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01701g3.cif
_cod_data_source_block           MnGeH2Ph_CNtBu_trans
_cod_depositor_comments
'Adding full bibliography for 7719468--7719476.cif.'
_cod_original_cell_volume        2929.5(19)
_cod_database_code               7719472
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.920
_shelx_estimated_absorpt_t_min   0.552
_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. Restrained distances
 C2-C5 \\sim C2A-C5A \\sim C2-C3 \\sim C2A-C3A \\sim C2-C4 \\sim C2A-C4A
 with sigma of 0.0002
 C5-C3 \\sim C3-C4 \\sim C4-C5 \\sim C5A-C3A \\sim C3A-C4A \\sim C4A-C5A
 with sigma of 0.0002
 C1-N1 \\sim C1-N1A
 with sigma of 0.005
 N1-C2 \\sim N1A-C2A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.05
Uanis(C4A) = Uanis(C5)
Uanis(C5A) = Uanis(C3)
Uanis(C4) = Uanis(C3A)
Uanis(C2) = Uanis(C2A)
Uanis(N1) = Uanis(N1A)
4. Others
 Fixed Sof: N1(0.5) N1A(0.5) C2(0.5) C2A(0.5) C3(0.5) H3A(0.5) H3B(0.5)
 H3C(0.5) C3A(0.5) H3AA(0.5) H3AB(0.5) H3AC(0.5) C4(0.5) H4A(0.5) H4B(0.5)
 H4C(0.5) C4A(0.5) H4AA(0.5) H4AB(0.5) H4AC(0.5) C5(0.5) H5A(0.5) H5B(0.5)
 H5C(0.5) C5A(0.5) H5AA(0.5) H5AB(0.5) H5AC(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C20(H20A,H20B), C21(H21A,H21B)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11)
5.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C3A(H3AA,H3AB,H3AC), C4(H4A,H4B,H4C), C4A(H4AA,H4AB,H4AC),
 C5(H5A,H5B,H5C), C5A(H5AA,H5AB,H5AC), 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)
;
_shelx_res_checksum              99474
_olex2_submission_special_instructions 'No special instructions were received'