An Iron Germylene Complex Having Fe-H and Ge-H Bonds: Synthesis, Structure and Reactivity
Dhungana, Tara Prasad; Hashimoto, Hisako; Tobita, Hiromi; Dalton Trans.  (2017) –; doi:10.1039/C7DT01159H

data_7043073
_publ_section_title
;
 An Iron Germylene Complex Having Fe-H and Ge-H Bonds: Synthesis,
 Structure and Reactivity
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01159H
_journal_year                    2017
_chemical_formula_moiety         '(C28 H49 Fe Ge N O2 Si3), 1(C7H8)'
_chemical_formula_sum            'C35 H57 Fe Ge N O2 Si3'
_chemical_formula_weight         736.52
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-05-18 deposited with the CCDC.
2017-05-22 downloaded from the CCDC.
;
_cell_angle_alpha                77.427(2)
_cell_angle_beta                 86.298(3)
_cell_angle_gamma                80.826(2)
_cell_formula_units_Z            2
_cell_length_a                   8.6833(7)
_cell_length_b                   12.7710(10)
_cell_length_c                   17.5545(9)
_cell_measurement_reflns_used    36054
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.19
_cell_volume                     1874.8(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver.1.11'
_computing_molecular_graphics    'ORTEP III'
_computing_publication_material  'Yadokari-XG 2009'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26076
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.230
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    1.315
_exptl_absorpt_correction_T_max  0.7690
_exptl_absorpt_correction_T_min  0.7116
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Higashi, 1999)'
_exptl_crystal_colour            brawn
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_description       block
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_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.350
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.085
_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     459
_refine_ls_number_reflns         8525
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0425P)^2^+1.3738P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.0970
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7525
_reflns_number_total             8525
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01159h2.cif
_cod_data_source_block           tara6a
_cod_database_code               7043073
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.621
_shelx_estimated_absorpt_t_max   0.656
_shelx_res_checksum              18534