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_7719469
_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         'C29 H53 Ge Mn O P4'
_chemical_formula_sum            'C29 H53 Ge Mn O P4'
_chemical_formula_weight         669.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-07-10
_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                 95.39(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.771(3)
_cell_length_b                   9.163(2)
_cell_length_c                   19.523(6)
_cell_measurement_reflns_used    5162
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.86
_cell_measurement_theta_min      2.46
_cell_volume                     3343.1(14)
_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 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
472 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  0.0365
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            42422
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.642
_diffrn_reflns_theta_min         2.096
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.488
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0413 before and 0.0335 after correction.
The Ratio of minimum to maximum transmission is 0.8493.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.649
_refine_diff_density_min         -1.398
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         9368
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0318P)^2^+3.7498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8137
_reflns_number_total             9368
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01701g3.cif
_cod_data_source_block           MnHGenBu_OCHPh2
_cod_depositor_comments
'Adding full bibliography for 7719468--7719476.cif.'
_cod_original_cell_volume        3343.0(14)
_cod_original_sg_symbol_H-M      P2/n
_cod_database_code               7719469
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.707
_shelx_estimated_absorpt_t_min   0.587
_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. Restrained distances
 C3-C4 \\sim C3A-C4A
 with sigma of 0.005
 C3-C2 \\sim C2-C3A
 with sigma of 0.005
 C17-C12 \\sim C12-C17A \\sim C12-C13 \\sim C12-C13A
 with sigma of 0.005
 C16A-C17A \\sim C16-C17 \\sim C14-C13 \\sim C14A-C13A
 with sigma of 0.005
 C15A-C16A \\sim C15-C16 \\sim C15-C14 \\sim C14A-C15A
 with sigma of 0.005
 C5-C12 \\sim C5-C6
 with sigma of 0.005
3. Restrained planarity
 C12, C13, C14, C15, C16, C17
 with sigma of 0.1
 C12, C13A, C14A, C15A, C16A, C17A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C4) = Uanis(C4A)
Uanis(C15) = Uanis(C15A)
Uanis(C13A) = Uanis(C16A)
Uanis(C13) = Uanis(C16)
Uanis(C14A) = Uanis(C17A)
Uanis(C14) = Uanis(C17)
5. Others
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=1-FVAR(1)
 Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=FVAR(1)
 Sof(H5B)=Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15A)=
 Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=1-FVAR(2)
 Sof(H5A)=Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=
 Sof(H16)=Sof(C17)=Sof(H17)=FVAR(2)
 Fixed Sof: H2AA(0.5) H2AB(0.5) H2BC(0.5) H2BD(0.5)
6.a Ternary CH refined with riding coordinates:
 C5(H5A), C5(H5B)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2AA,H2AB), C2(H2BC,H2BD), C3(H3A,H3B), C3A(H3AA,H3AB),
 C20(H20A,H20B), C21(H21A,H21B), C26(H26A,H26B), C27(H27A,H27B)
6.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C13A(H13A), C14(H14),
 C14A(H14A), C15(H15), C15A(H15A), C16(H16), C16A(H16A), C17(H17), C17A(H17A)
6.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C4A(H4AA,H4AB,H4AC), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,
 H25B,H25C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              24011
_olex2_submission_special_instructions 'No special instructions were received'