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_7718866
_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         'C16 H43 Ge Mn N2 P4'
_chemical_formula_sum            'C16 H43 Ge Mn N2 P4'
_chemical_formula_weight         514.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 90.674(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.295(3)
_cell_length_b                   16.194(4)
_cell_length_c                   16.278(4)
_cell_measurement_reflns_used    4787
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.277
_cell_measurement_theta_min      2.502
_cell_volume                     2450.0(12)
_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 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
424 frames, detector distance = 90.0 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  0.0232
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30837
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.618
_diffrn_reflns_theta_min         2.503
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.006
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6556
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0484 before and 0.0263 after correction.
The Ratio of minimum to maximum transmission is 0.8787.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.201
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         7531
_refine_ls_number_restraints     409
_refine_ls_restrained_S_all      1.416
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0337
_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^)+3.0402P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0878
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6855
_reflns_number_total             7531
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01025j3.cif
_cod_data_source_block           MnGeHEt2_N2_cis
_cod_depositor_comments
'Adding full bibliography for 7718858--7718867.cif.'
_cod_original_cell_volume        2450.1(11)
_cod_database_code               7718866
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.634
_shelx_estimated_absorpt_t_min   0.501
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P1-C5 \\sim P1-C6 \\sim P1-C5A \\sim P1-C6A \\sim P2-C9 \\sim P2-C10 \\sim
P2A-C9A \\sim P2A-C10A \\sim P3-
 C12 \\sim P3-C11 \\sim P3A-C12A \\sim P3A-C11A \\sim P4-C15 \\sim P4-C16 \\sim
P4-C15A \\sim P4-C16A
 with sigma of 0.002
 P1-C7 \\sim P2-C8 \\sim P3-C13 \\sim P4-C14 \\sim P1-C7A \\sim P2A-C8A \\sim
P3A-C13A \\sim P4-C14A
 with sigma of 0.005
 C7-C8 \\sim C13-C14 \\sim C7A-C8A \\sim C13A-C14A
 with sigma of 0.005
 P2-Mn1 \\sim Mn1-P3A
 with sigma of 0.002
 P2A-Mn1 \\sim Mn1-P3
 with sigma of 0.002
 C15-C16 \\sim C11-C12 \\sim C5-C6 \\sim C14-C15 \\sim C5A-C6A \\sim C10A-C9A
\\sim C12A-C11A \\sim C15A-
 C16A
 with sigma of 0.005
 C7-C5 \\sim C7-C6 \\sim C8-C9 \\sim C8-C10 \\sim C13-C11 \\sim C13-C12 \\sim
C14-C15 \\sim C14-C16 \\sim C7A-
 C5A \\sim C7A-C6A \\sim C8A-C9A \\sim C8A-C10A \\sim C13A-C11A \\sim C13A-C12A
\\sim C14A-C15A \\sim C14A-
 C16A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(P3) = Uanis(P2A)
Uanis(P2) = Uanis(P3A)
Uanis(C6A) = Uanis(C7)
Uanis(C9) = Uanis(C12A)
Uanis(C14A) = Uanis(C15)
Uanis(C16A) = Uanis(C16)
Uanis(C14) = Uanis(C15A)
Uanis(C9A) = Uanis(C12)
Uanis(C7A) = Uanis(C6)
Uanis(C5A) = Uanis(C5)
Uanis(C7) = Uanis(C6A)
4. Others
 Sof(P2A)=Sof(P3A)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C6A)=Sof(H6AA)=
 Sof(H6AB)=Sof(H6AC)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=
 Sof(C11A)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C12A)=Sof(H12D)=Sof(H12E)=
 Sof(H12F)=Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(C14A)=Sof(H14C)=Sof(H14D)=
 Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16A)=Sof(H16D)=Sof(H16E)=
 Sof(H16F)=1-FVAR(1)
 Sof(P2)=Sof(P3)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=Sof(H6A)=Sof(H6B)=
 Sof(H6C)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C9)=Sof(H9A)=
 Sof(H9B)=Sof(H9C)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C11)=Sof(H11A)=
 Sof(H11B)=Sof(H11C)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C13)=Sof(H13A)=
 Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C7(H7A,H7B), C8(H8A,H8B), C13(H13A,H13B), C14(H14A,
 H14B), C7A(H7AA,H7AB), C8A(H8AA,H8AB), C13A(H13C,H13D), C14A(H14C,H14D)
5.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C5A(H5AA,H5AB,H5AC), C6A(H6AA,H6AB,
 H6AC), C9A(H9AA,H9AB,H9AC), C10A(H10D,H10E,H10F), C11A(H11D,H11E,H11F),
 C12A(H12D,H12E,H12F), C15A(H15D,H15E,H15F), C16A(H16D,H16E,H16F)
;
_shelx_res_checksum              54361
_shelx_hkl_checksum              20243
_olex2_submission_special_instructions 'No special instructions were received'