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_7714122
_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 H66 Ge Mn2 P8'
_chemical_formula_sum            'C24 H66 Ge Mn2 P8'
_chemical_formula_weight         784.99
_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                 101.283(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.673(2)
_cell_length_b                   17.979(7)
_cell_length_c                   11.970(3)
_cell_measurement_reflns_used    3852
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.372
_cell_measurement_theta_min      2.265
_cell_volume                     3729.9(18)
_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_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
456 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  0.0346
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            46413
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.563
_diffrn_reflns_theta_min         1.632
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.825
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6689
_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 0.0258 after correction.
The Ratio of minimum to maximum transmission is 0.8968.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       block
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.00048(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         10386
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0321
_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^)+3.7772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0751
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9090
_reflns_number_total             10386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02437g3.cif
_cod_data_source_block           Mn2Ge
_cod_original_cell_volume        3729.7(18)
_cod_database_code               7714122
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.658
_shelx_estimated_absorpt_t_min   0.529
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C9(H9A,H9B), C4(H4A,H4B), C10(H10A,H10B), C21(H21A,H21B),
 C15(H15A,H15B), C22(H22A,H22B), C16(H16A,H16B)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C12(H12A,H12B,H12C), C8(H8A,H8B,H8C),
 C18(H18A,H18B,H18C), C23(H23A,H23B,H23C), C19(H19A,H19B,H19C), C11(H11A,H11B,
 H11C), C24(H24A,H24B,H24C), C1(H1A,H1B,H1C), C14(H14A,H14B,H14C), C7(H7A,H7B,
 H7C), C17(H17A,H17B,H17C), C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C6(H6A,
 H6B,H6C)
;
_shelx_res_checksum              44095
_olex2_submission_special_instructions 'No special instructions were received'