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_7718858
_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
'0.54(C16 H43 Ge1 Mn P4), 0.40(C16 H45 Ge1 Mn P4), 0.06(C16 H45 Ge1 Mn P4)'
_chemical_formula_sum            'C16 H43.92 Ge Mn P4'
_chemical_formula_weight         487.84
_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             2025-04-24
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7221)
;
_audit_update_record
;
2025-05-01 deposited with the CCDC.	2025-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                88.987(10)
_cell_angle_beta                 75.985(19)
_cell_angle_gamma                75.957(14)
_cell_formula_units_Z            2
_cell_length_a                   9.159(3)
_cell_length_b                   9.8098(18)
_cell_length_c                   14.115(3)
_cell_measurement_reflns_used    4028
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.03
_cell_measurement_theta_min      2.36
_cell_volume                     1192.5(5)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
456 frames, detector distance = 100.0 mm
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0755
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20812
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.660
_diffrn_reflns_theta_min         2.142
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.055
_exptl_absorpt_correction_T_max  0.492870
_exptl_absorpt_correction_T_min  0.395938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0392 before and 0.0202 after correction.
 The Ratio of minimum to maximum transmission is 0.81.

Final HKLF 4 output contains 24934 reflections, Rint = 0.0156
 (9228 with I > 3sig(I), Rint = 0.0099)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       block
_exptl_crystal_F_000             514
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.45
_refine_diff_density_max         2.869
_refine_diff_density_min         -1.160
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         20812
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0206P)^2^+0.3064P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1322
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13591
_reflns_number_total             20812
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01025j3.cif
_cod_data_source_block           MnGeHEt2_H2_trans
_cod_depositor_comments
'Adding full bibliography for 7718858--7718867.cif.'
_cod_original_cell_volume        1192.6(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7718858
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.458
_shelx_estimated_absorpt_t_min   0.372
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9513(2)
 0.0487(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All Ge(H) groups
3. Restrained distances
 Ge2-Mn1 \\sim Mn1-Ge3
 with sigma of 0.002
 C1-Ge1 \\sim Ge1-C3
 with sigma of 0.002
 C3A-Ge2 \\sim Ge2-C1A \\sim Ge3-C3B \\sim Ge3-C1B
 with sigma of 0.002
 C3-C4 \\sim C3A-C4A \\sim C3B-C4B \\sim C1B-C2B \\sim C1-C2 \\sim C1A-C2A
 with sigma of 0.002
4. Uiso/Uaniso restraints and constraints
Uanis(Ge2) = Uanis(Ge1)
Uanis(Ge1) = Uanis(Ge2) = Uanis(Ge3)
Uanis(C1) = Uanis(C1A)
Uanis(C2) = Uanis(C2A)
Uanis(C3) = Uanis(C3B)
Uanis(C4) = Uanis(C4B)
Uanis(C1B) = Uanis(C1)
Uanis(C2) = Uanis(C2B)
5. Others
 1*[Sof(Ge1)+Sof(C1)+Sof(H1A)+Sof(H1B)+Sof(C2)+Sof(H2A)+Sof(H2B)+Sof(H2C)+
 Sof(C3)+Sof(H3A)+Sof(H3B)+Sof(C4)+Sof(H4A)+Sof(H4B)+Sof(H4C)]+1*[Sof(H2)+
 Sof(Ge2)+Sof(H3)+Sof(C1A)+Sof(H1AA)+Sof(H1AB)+Sof(C2A)+Sof(H2AA)+Sof(H2AB)+
 Sof(H2AC)+Sof(C3A)+Sof(H3AA)+Sof(H3AB)+Sof(C4A)+Sof(H4AA)+Sof(H4AB)+Sof(H4AC)]+
 1*[Sof(Ge3)+Sof(C1B)+Sof(H1BA)+Sof(H1BB)+Sof(C2B)+Sof(H2BA)+Sof(H2BB)+
 Sof(H2BC)+Sof(C3B)+Sof(H3BA)+Sof(H3BB)+Sof(C4B)+Sof(H4BA)+Sof(H4BB)+Sof(H4BC)]=
 1 with esd of 0.000001
 Sof(Ge1)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=
 Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=FVAR(1)
 Sof(H2)=Sof(Ge2)=Sof(H3)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2AA)=
 Sof(H2AB)=Sof(H2AC)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=
 Sof(H4AC)=FVAR(2)
 Sof(Ge3)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(H2BC)=
 Sof(C3B)=Sof(H3BA)=Sof(H3BB)=Sof(C4B)=Sof(H4BA)=Sof(H4BB)=Sof(H4BC)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C13(H13A,H13B), C14(H14A,H14B), C1(H1A,H1B), C3(H3A,
 H3B), C1A(H1AA,H1AB), C3A(H3AA,H3AB), C1B(H1BA,H1BB), C3B(H3BA,H3BB)
6.b Me refined with riding coordinates:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C2A(H2AA,H2AB,H2AC), C4A(H4AA,H4AB,H4AC),
 C2B(H2BA,H2BB,H2BC), C4B(H4BA,H4BB,H4BC)
6.c Idealised Me refined as rotating group:
 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)
;
_shelx_res_checksum              23089
_shelx_hkl_checksum              94036
_olex2_submission_special_instructions 'No special instructions were received'