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_7714119
_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         'C24 H43 Ge Mn P4'
_chemical_formula_sum            'C24 H43 Ge Mn P4'
_chemical_formula_weight         582.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-06
_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                 103.094(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9001(17)
_cell_length_b                   14.3514(16)
_cell_length_c                   12.5626(12)
_cell_measurement_reflns_used    4359
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.11
_cell_measurement_theta_min      2.356
_cell_volume                     2792.1(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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
440 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  0.0334
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32261
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.511
_diffrn_reflns_theta_min         1.935
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.768
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6452
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0436 before and 0.0311 after correction.
The Ratio of minimum to maximum transmission is 0.8650.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_description       block
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.948
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         7772
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0247
_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^)+0.9107P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0664
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6931
_reflns_number_total             7772
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02437g3.cif
_cod_data_source_block           MnHGePh2
_cod_database_code               7714119
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.777
_shelx_estimated_absorpt_t_min   0.619
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C15(H15A,H15B), C16(H16A,H16B), C22(H22A,H22B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C6(H6), C2(H2), C11(H11), C8(H8), C10(H10), C9(H9), C5(H5), C4(H4),
 C3(H3)
2.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C20(H20A,H20B,H20C), C19(H19A,H19B,
 H19C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C14(H14A,H14B,H14C), C13(H13A,
 H13B,H13C)
;
_shelx_res_checksum              17451
_olex2_submission_special_instructions 'No special instructions were received'