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_7718862
_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 Mn N2 P4 Si'
_chemical_formula_sum            'C24 H43 Mn N2 P4 Si'
_chemical_formula_weight         566.51
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-04-24
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7217)
;
_audit_update_record
;
2025-05-01 deposited with the CCDC.	2025-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.91(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.300(6)
_cell_length_b                   16.285(9)
_cell_length_c                   17.635(12)
_cell_measurement_reflns_used    7013
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      25.21
_cell_measurement_theta_min      2.42
_cell_volume                     2845(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Dual Source D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0770
_diffrn_reflns_av_unetI/netI     0.0937
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31909
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.739
_diffrn_reflns_theta_min         2.425
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.747
_exptl_absorpt_correction_T_max  0.8622
_exptl_absorpt_correction_T_min  0.7513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0958 before and 0.0734 after correction.
The Ratio of minimum to maximum transmission is 0.8714.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.009
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details
;
 Flack x determined using 2080 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.046(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         7794
_refine_ls_number_restraints     194
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_gt           0.0585
_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^)+(0.0497P)^2^+9.1517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1464
_reflns_Friedel_coverage         0.930
_reflns_Friedel_fraction_full    0.960
_reflns_Friedel_fraction_max     0.926
_reflns_number_gt                5386
_reflns_number_total             7794
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01025j3.cif
_cod_data_source_block           MnSiHPh2_N2_trans
_cod_depositor_comments
'Adding full bibliography for 7718858--7718867.cif.'
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               7718862
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.896
_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
 Si1-C1 \\sim Si1A-C1A \\sim Si1-C7 \\sim Si1A-C7A
 with sigma of 0.005
 C1-C2 \\sim C6-C1 \\sim C1A-C2A \\sim C6A-C1A \\sim C7-C8 \\sim C12-C7 \\sim
C7A-C8A \\sim C12A-C7A
 with sigma of 0.005
 C2-C3 \\sim C5-C6 \\sim C2A-C3A \\sim C5A-C6A \\sim C8-C9 \\sim C11-C12 \\sim
C8A-C9A \\sim C11A-C12A
 with sigma of 0.005
 C3-C4 \\sim C4-C5 \\sim C3A-C4A \\sim C4A-C5A \\sim C9-C10 \\sim C10-C11 \\sim
C9A-C10A \\sim C10A-C11A
 with sigma of 0.005
 P1-C13 \\sim P1-C14 \\sim P2-C17 \\sim P2-C18 \\sim P2-C17A \\sim P2-C18A
\\sim P3-C19 \\sim P3-C20 \\sim P4-
 C23 \\sim P4-C24 \\sim P4-C23A \\sim P4-C24A
 with sigma of 0.005
 C13-C14 \\sim C17-C18 \\sim C17A-C18A \\sim C19-C20 \\sim C23-C24 \\sim
C23A-C24A
 with sigma of 0.005
 P1-C15 \\sim P2-C16 \\sim P2-C16A \\sim P3-C21 \\sim P4-C22 \\sim P4-C22A
 with sigma of 0.005
 C15-C16 \\sim C15-C16A \\sim C21-C22 \\sim C21-C22A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(Si1) = Uanis(Si1A)
Uanis(C22A) = Uanis(C22)
Uanis(C23) = Uanis(C24A)
Uanis(C24) = Uanis(C23A)
Uanis(C18A) = Uanis(C18)
Uanis(C17) = Uanis(C17A)
Uanis(C16A) = Uanis(C16)
Uanis(C1) = Uanis(C4)
Uanis(C6) = Uanis(C3)
Uanis(C5) = Uanis(C2)
Uanis(C7) = Uanis(C10)
Uanis(C8) = Uanis(C11)
Uanis(C9) = Uanis(C12)
Uanis(C1A) = Uanis(C4A)
Uanis(C6A) = Uanis(C3A)
Uanis(C5A) = Uanis(C2A)
Uanis(C7A) = Uanis(C10A)
Uanis(C8A) = Uanis(C11A)
Uanis(C9A) = Uanis(C12A)
4. Others
 Sof(Si1A)=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)=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(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(Si1)=Sof(H1)=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)=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(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), C15(H15C,H15D), C16(H16A,H16B), C16A(H16C,H16D), C21(H21A,
 H21B), C21(H21C,H21D), C22(H22A,H22B), C22A(H22C,H22D)
5.b Me refined with riding coordinates:
 C20(H20A,H20B,H20C)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C2A(H2A), C3(H3), C3A(H3A), C4(H4), C4A(H4A), C5(H5), C5A(H5A),
 C6(H6), C6A(H6A), C8(H8), C8A(H8A), C9(H9), C9A(H9A), C10(H10), C10A(H10A),
 C11(H11), C11A(H11A), C12(H12), C12A(H12A)
5.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C17A(H17D,H17E,
 H17F), C18(H18A,H18B,H18C), C18A(H18D,H18E,H18F), C19(H19A,H19B,H19C),
 C23(H23A,H23B,H23C), C23A(H23D,H23E,H23F), C24(H24A,H24B,H24C), C24A(H24D,H24E,
 H24F)
;
_shelx_res_checksum              78340
_shelx_hkl_checksum              92178
_olex2_submission_special_instructions 'No special instructions were received'