Reactions of [(dmpe)<sub>2</sub>MnH(C<sub>2</sub>H<sub>4</sub>)] with hydrogermanes to form germylene, germyl, hydrogermane, and germanide complexes.
Price, Jeffrey S.; Vargas-Baca, Ignacio; Emslie, David J. H.; Britten, James F.; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt02437g

data_7714120
_publ_section_title
;
 Reactions of [(dmpe)<sub>2</sub>MnH(C<sub>2</sub>H<sub>4</sub>)] with
 hydrogermanes to form germylene, germyl, hydrogermane, and germanide
 complexes.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt02437g
_journal_year                    2023
_chemical_formula_moiety         'C32 H84 Ge2 Mn2 O P8'
_chemical_formula_sum            'C32 H84 Ge2 Mn2 O P8'
_chemical_formula_weight         987.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-23
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-07-25 deposited with the CCDC.	2023-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.100(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   26.777(18)
_cell_length_b                   9.568(3)
_cell_length_c                   9.796(5)
_cell_measurement_reflns_used    605
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      20.326
_cell_measurement_theta_min      2.276
_cell_volume                     2372(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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
436 frames, detector distance = 100 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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.1121
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6567
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.545
_diffrn_reflns_theta_min         2.200
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.069
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5183
_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 0.0564 before and 0.0305 after correction.
 
For component 2:
 wR2(int) was 0.0610 before and 0.0345 after correction.
 The Ratio of minimum to maximum transmission is 0.61.

Final HKLF 4 output contains 20564 reflections, Rint = 0.0874
 (3408 with I > 3sig(I), Rint = 0.0584)
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       plate
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.223
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.17(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         6567
_refine_ls_number_restraints     157
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.1031
_refine_ls_R_factor_gt           0.0604
_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^)+(0.0936P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1562
_reflns_Friedel_coverage         0.874
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                3895
_reflns_number_total             6567
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02437g3.cif
_cod_data_source_block           MnGenBuO
_cod_database_code               7714120
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.820
_shelx_estimated_absorpt_t_min   0.576
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.83(2)
 0.17(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
3. Restrained distances
 C7A-C8 \\sim C7-C8A \\sim C14A-C13A \\sim C14-C13
 with sigma of 0.002
 C6A-C7A \\sim C7A-C5A
 with sigma of 0.002
 C6-C7 \\sim C7-C5
 with sigma of 0.002
 C9-C8 \\sim C8-C10
 with sigma of 0.002
 C10A-C8A \\sim C8A-C9A
 with sigma of 0.002
 C7A-C8A \\sim C7-C8
 with sigma of 0.002
 C6-P1 \\sim P1-C5A \\sim C6A-P1 \\sim P1-C5 \\sim C10-P2 \\sim P2-C9A \\sim
C10A-P2 \\sim P2-C9 \\sim C11A-P3
 \\sim P3-C12 \\sim C12A-P3 \\sim P3-C11 \\sim C16-P4 \\sim P4-C15A \\sim
C16A-P4 \\sim P4-C15
 with sigma of 0.002
 C8A-P2 \\sim P2-C8 \\sim C7-P1 \\sim P1-C7A \\sim C13-P3 \\sim P3-C13A \\sim
P4-C14 \\sim P4-C14A
 with sigma of 0.002
 C12A-C13A \\sim C13A-C11A
 with sigma of 0.002
 C12-C13 \\sim C13-C11
 with sigma of 0.002
4. Uiso/Uaniso restraints and constraints
Uanis(C14A) = Uanis(C14)
Uanis(C15A) = Uanis(C16) = Uanis(C15) = Uanis(C16A)
Uanis(C5) = Uanis(C6A)
Uanis(C6) = Uanis(C5A)
Uanis(C6A) = Uanis(C5) = Uanis(C5A) = Uanis(C6)
Uanis(C8) = Uanis(C8A) = Uanis(C7) = Uanis(C7A)
Uanis(C9) = Uanis(C10A) = Uanis(C10) = Uanis(C9A)
Uanis(C13) = Uanis(C13A)
Uanis(C12A) = Uanis(C11) = Uanis(C11A) = Uanis(C12)
5. Others
 Sof(C11A)=Sof(H11F)=Sof(H11D)=Sof(H11E)=Sof(C12A)=Sof(H12D)=Sof(H12E)=
 Sof(H12F)=Sof(C13A)=Sof(H13D)=Sof(H13C)=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(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12)=Sof(H12C)=Sof(H12A)=Sof(H12B)=
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14B)=Sof(H14A)=Sof(C15)=Sof(H15A)=
 Sof(H15B)=Sof(H15C)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(1)
 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(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(2)
 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(H10A)=Sof(H10B)=Sof(H10C)=FVAR(2)
 Fixed Uiso: H1(0.01)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C7(H7A,H7B), C8(H8A,H8B), C13(H13A,
 H13B), C14(H14B,H14A), C7A(H7AA,H7AB), C8A(H8AA,H8AB), C13A(H13D,H13C),
 C14A(H14C,H14D)
6.b Me refined with riding coordinates:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C10(H10D,
 H10E,H10F), C11(H11A,H11B,H11C), C12(H12C,H12A,H12B), C15(H15A,H15B,H15C),
 C16(H16A,H16B,H16C), C5A(H5AA,H5AB,H5AC), C6A(H6AA,H6AB,H6AC), C9A(H9AA,H9AB,
 H9AC), C10A(H10A,H10B,H10C), C11A(H11F,H11D,H11E), C12A(H12D,H12E,H12F),
 C15A(H15D,H15E,H15F), C16A(H16D,H16E,H16F)
;
_shelx_res_checksum              26784
_olex2_submission_special_instructions 'No special instructions were received'