Manganese germylene complexes: reactivity with dihydrogen, isonitriles, and dinitrogen.
Price, Jeffrey S.; Emslie, David J. H.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 9949–9968; doi:10.1039/d5dt01025j

data_7718867
_publ_section_title
;
 Manganese germylene complexes: reactivity with dihydrogen, isonitriles,
 and dinitrogen.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9949
_journal_page_last               9968
_journal_paper_doi               10.1039/d5dt01025j
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C24 H43 Ge Mn N2 P4'
_chemical_formula_sum            'C24 H43 Ge Mn N2 P4'
_chemical_formula_weight         611.01
_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             2024-08-07
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-05-01 deposited with the CCDC.	2025-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                71.401(12)
_cell_angle_beta                 83.524(16)
_cell_angle_gamma                77.39(2)
_cell_formula_units_Z            2
_cell_length_a                   9.636(2)
_cell_length_b                   10.981(3)
_cell_length_c                   14.658(3)
_cell_measurement_reflns_used    2443
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.30
_cell_measurement_theta_min      2.56
_cell_volume                     1433.0(6)
_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
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
422 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  0.0219
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16604
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.618
_diffrn_reflns_theta_min         1.995
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.728
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0375 before and 0.0225 after correction.
The Ratio of minimum to maximum transmission is 0.8608.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_description       block
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.990
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         7994
_refine_ls_number_restraints     311
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0376
_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^)+1.7262P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0945
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6864
_reflns_number_total             7994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01025j3.cif
_cod_data_source_block           MnGeHPh2_N2_cis
_cod_depositor_comments
'Adding full bibliography for 7718858--7718867.cif.'
_cod_database_code               7718867
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.724
_shelx_estimated_absorpt_t_min   0.545
_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
 Mn1-P2 \\sim Mn1-P2A \\sim Mn1-P4 \\sim Mn1-P4A
 with sigma of 0.005
 Mn1-P3 \\sim Mn1-P3A
 with sigma of 0.005
 Mn1-P2 \\sim Mn1-P2A
 with sigma of 0.005
 P1-C13 \\sim P1-C14 \\sim P2-C17 \\sim P2-C18 \\sim P3-C19 \\sim P3-C20 \\sim
P4-C23 \\sim P4-C24 \\sim P1A-
 C13A \\sim P1A-C14A \\sim P2A-C17A \\sim P2A-C18A \\sim P3A-C19A \\sim
P3A-C20A \\sim P4A-C23A \\sim P4A-
 C24A
 with sigma of 0.005
 P1-C15 \\sim P2-C16 \\sim P3-C21 \\sim P4-C22 \\sim P1A-C15A \\sim P2A-C16A
\\sim P3A-C21A \\sim P4A-C22A
 with sigma of 0.005
 C15-C16 \\sim C21-C22 \\sim C15A-C16A \\sim C21A-C22A
 with sigma of 0.005
 C13-C14 \\sim C17-C18 \\sim C19-C20 \\sim C23-C24 \\sim C13A-C14A \\sim
C17A-C18A \\sim C19A-C20A 
 C23A-C24A
 with sigma of 0.01
 C15-C13 \\sim C15-C14 \\sim C16-C17 \\sim C16-C18 \\sim C21-C19 \\sim C21-C20
\\sim C22-C23 \\sim C22-C24
 \\sim C15A-C13A \\sim C15A-C14A \\sim C16A-C17A \\sim C16A-C18A \\sim
C21A-C19A \\sim C21A-C20A \\sim C22A-
 C23A \\sim C22A-C24A
 with sigma of 0.01
 P1-P2 \\sim P1A-P2A
 with sigma of 0.01
 P3-P4 \\sim P3A-P4A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(P3) = Uanis(P3A)
Uanis(P4) = Uanis(P4A)
Uanis(P1A) = Uanis(P1)
Uanis(P2) = Uanis(P2A)
Uanis(C23) = Uanis(C18A)
Uanis(C16A) = Uanis(C24)
Uanis(C17A) = Uanis(C22)
Uanis(C21) = Uanis(C21A)
Uanis(C19) = Uanis(C19A)
Uanis(C20) = Uanis(C20A)
Uanis(C18) = Uanis(C22A)
Uanis(C17) = Uanis(C23A)
Uanis(C16) = Uanis(C24A)
Uanis(C15) = Uanis(C15A)
Uanis(C14A) = Uanis(C13)
Uanis(C14) = Uanis(C13A)
4. Others
 Sof(P1A)=Sof(P2A)=Sof(P3A)=Sof(P4A)=Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=
 Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C15A)=Sof(H15C)=Sof(H15D)=
 Sof(C16A)=Sof(H16C)=Sof(H16D)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=
 Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19A)=Sof(H19D)=Sof(H19E)=
 Sof(H19F)=Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C21A)=Sof(H21C)=
 Sof(H21D)=Sof(C22A)=Sof(H22C)=Sof(H22D)=Sof(C23A)=Sof(H23D)=Sof(H23E)=
 Sof(H23F)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(1)
 Sof(P1)=Sof(P2)=Sof(P3)=Sof(P4)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(C16)=
 Sof(H16A)=Sof(H16B)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18A)=
 Sof(H18B)=Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C20)=Sof(H20A)=
 Sof(H20B)=Sof(H20C)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=
 FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C15A(H15C,H15D), C16(H16A,H16B), C16A(H16C,H16D), C21(H21A,
 H21B), C21A(H21C,H21D), C22(H22A,H22B), C22A(H22C,H22D)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12)
5.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C13A(H13D,H13E,H13F), C14(H14A,H14B,H14C), C14A(H14D,
 H14E,H14F), C17(H17A,H17B,H17C), C17A(H17D,H17E,H17F), C18(H18A,H18B,H18C),
 C18A(H18D,H18E,H18F), C19(H19A,H19B,H19C), C19A(H19D,H19E,H19F), C20(H20A,H20B,
 H20C), C20A(H20D,H20E,H20F), C23(H23A,H23B,H23C), C23A(H23D,H23E,H23F),
 C24(H24A,H24B,H24C), C24A(H24D,H24E,H24F)
;
_shelx_res_checksum              94263
_shelx_hkl_checksum              22533
_olex2_submission_special_instructions 'No special instructions were received'