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_7718860
_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         'C33 H52 Ge Mn N P4, 0.5(C7 H8)'
_chemical_formula_sum            'C36.5 H56 Ge Mn N P4'
_chemical_formula_weight         760.23
_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             2024-08-12
_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                93.122(18)
_cell_angle_beta                 98.196(19)
_cell_angle_gamma                101.38(3)
_cell_formula_units_Z            4
_cell_length_a                   10.896(4)
_cell_length_b                   15.146(4)
_cell_length_c                   23.533(7)
_cell_measurement_reflns_used    2720
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.035
_cell_measurement_theta_min      2.321
_cell_volume                     3755(2)
_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 0.994
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
440 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  0.0474
_diffrn_reflns_av_unetI/netI     0.0978
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            44723
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.622
_diffrn_reflns_theta_min         1.694
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.333
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6265
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0402 before and 0.0343 after correction.
The Ratio of minimum to maximum transmission is 0.8399.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       block
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.408
_refine_diff_density_min         -1.020
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     804
_refine_ls_number_reflns         20889
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0473P)^2^+2.3581P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1493
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14995
_reflns_number_total             20889
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01025j3.cif
_cod_data_source_block           MnGeHPh2_CNXyl_cis
_cod_depositor_comments
'Adding full bibliography for 7718858--7718867.cif.'
_cod_original_formula_sum        'C36.50 H56 Ge Mn N P4'
_cod_database_code               7718860
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.878
_shelx_estimated_absorpt_t_min   0.555
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All Ge(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C30B-C31B \\sim C30A-C31A
 with sigma of 0.002
 C30A-P3A \\sim P3A-C30B \\sim C31B-P4A \\sim P4A-C31A
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C30A) = Uanis(C31A)
Uanis(C30B) = Uanis(C31B)
Uanis(C37) = Uanis(C40)
Uanis(C36) = Uanis(C39)
4. Others
 Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(C31A)=Sof(H31C)=Sof(H31D)=1-FVAR(1)
 Sof(C30B)=Sof(H30A)=Sof(H30B)=Sof(C31B)=Sof(H31A)=Sof(H31B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C24(H24C,H24D), C25(H25C,H25D), C30(H30E,H30F), C31(H31E,H31F), C24A(H24A,
 H24B), C25A(H25A,H25B), C30B(H30A,H30B), C30A(H30C,H30D), C31B(H31A,H31B),
 C31A(H31C,H31D)
5.b Me refined with riding coordinates:
 C9(H9A,H9B,H9C), C8A(H8AA,H8AB,H8AC)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15),
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C4A(H4A), C5A(H5A), C6A(H6A),
  C11A(H11A), C12A(H12A), C13A(H13A), C14A(H14A), C15A(H15A), C17A(H17A),
 C18A(H18A), C19A(H19A), C20A(H20A), C21A(H21A), C36(H36), C37(H37), C38(H38),
 C39(H39), C40(H40)
5.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C22(H22D,H22E,H22F), C23(H23D,H23E,H23F), C26(H26D,H26E,
 H26F), C27(H27D,H27E,H27F), C28(H28D,H28E,H28F), C29(H29D,H29E,H29F), C32(H32D,
 H32E,H32F), C33(H33D,H33E,H33F), C9A(H9AA,H9AB,H9AC), C22A(H22A,H22B,H22C),
 C23A(H23A,H23B,H23C), C26A(H26A,H26B,H26C), C27A(H27A,H27B,H27C), C28A(H28A,
 H28B,H28C), C29A(H29A,H29B,H29C), C32A(H32A,H32B,H32C), C33A(H33A,H33B,H33C),
 C34(H34A,H34B,H34C)
;
_shelx_res_checksum              74827
_shelx_hkl_checksum              8912
_olex2_submission_special_instructions 'No special instructions were received'