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_7718863
_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      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 105.80(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.333(2)
_cell_length_b                   16.308(3)
_cell_length_c                   17.760(4)
_cell_measurement_reflns_used    488
_cell_measurement_temperature    100
_cell_measurement_theta_max      19.92
_cell_measurement_theta_min      2.34
_cell_volume                     2879.7(11)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_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_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
 204 frames, detector distance = 115 mm
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1929
_diffrn_reflns_av_unetI/netI     0.2176
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9837
_diffrn_reflns_point_group_measured_fraction_full 0.924
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.399
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.720
_exptl_absorpt_correction_T_max  0.9516
_exptl_absorpt_correction_T_min  0.8416
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 'X-SHAPE version 2.05 and X-RED32 version 1.10,
STOE & Cie GmbH: Darmstadt, Germany, 2004.'
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.08(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.872
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         5401
_refine_ls_number_restraints     710
_refine_ls_restrained_S_all      0.822
_refine_ls_R_factor_all          0.1865
_refine_ls_R_factor_gt           0.0852
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1080P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1881
_refine_ls_wR_factor_ref         0.2392
_reflns_Friedel_coverage         0.835
_reflns_Friedel_fraction_full    0.849
_reflns_Friedel_fraction_max     0.837
_reflns_number_gt                2199
_reflns_number_total             5401
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01025j3.cif
_cod_data_source_block           MnGeHPh2_N2_trans
_cod_depositor_comments
'Adding full bibliography for 7718858--7718867.cif.'
_cod_original_cell_volume        2879.9(11)
_cod_database_code               7718863
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.725
_shelx_estimated_absorpt_t_min   0.480
_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
 Ge1-C1 \\sim Ge1-C7 \\sim Ge1A-C7A \\sim Ge1A-C1A
 with sigma of 0.02
 Mn1-Ge1A \\sim Mn1-Ge1
 with sigma of 0.005
 C7A-C8A \\sim C8A-C9A \\sim C9A-C10A \\sim C10A-C11A \\sim C11A-C12A \\sim
C12A-C7A \\sim C7-C8 \\sim C8-
 C9 \\sim C9-C10 \\sim C10-C11 \\sim C11-C12 \\sim C12-C7 \\sim C1-C2 \\sim
C2-C3 \\sim C3-C4 \\sim C4-C5 \\sim C5-
 C6 \\sim C6-C1 \\sim C1A-C2A \\sim C2A-C3A \\sim C3A-C4A \\sim C4A-C5A \\sim
C5A-C6A \\sim C6A-C1A
 with sigma of 0.005
 C7-C10 \\sim C8-C11 \\sim C9-C12 \\sim C7A-C10A \\sim C8A-C11A \\sim C9A-C12A
\\sim C1-C4 \\sim C2-C5 
 C3-C6 \\sim C1A-C4A \\sim C2A-C5A \\sim C3A-C6A
 with sigma of 0.005
3. Restrained planarity
 C7A, C8A, C9A, C10A, C11A, C12A
 with sigma of 0.1
 C7, C8, C9, C10, C11, C12
 with sigma of 0.1
 C1A, C2A, C3A, C4A, C5A, C6A
 with sigma of 0.1
 C1, C2, C3, C4, C5, C6
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(Ge1A) = Uanis(Ge1)
Uanis(C7A) = Uanis(C7)
Uanis(C8A) = Uanis(C8)
Uanis(C9A) = Uanis(C9)
Uanis(C10A) = Uanis(C10)
Uanis(C11A) = Uanis(C11)
Uanis(C12A) = Uanis(C12)
Uanis(C1) = Uanis(C1A)
Uanis(C2A) = Uanis(C2)
Uanis(C3A) = Uanis(C3)
Uanis(C4A) = Uanis(C4)
Uanis(C5A) = Uanis(C5)
Uanis(C6A) = Uanis(C6)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(Ge1A)=Sof(C1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=
 Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=
 Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=1-FVAR(1)
 Sof(Ge1)=Sof(C1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=
 Sof(H5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9)=Sof(C10)=
 Sof(H10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C21(H21A,H21B), C22(H22A,H22B)
7.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), C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C6A(H6A), C8A(H8A), C9A(H9A),
  C10A(H10A), C11A(H11A), C12A(H12A)
7.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C)
;
_shelx_res_checksum              90932
_shelx_hkl_checksum              68878
_olex2_submission_special_instructions 'No special instructions were received'