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_7043069
_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_sum            'C31 H56 Fe Ge O2 Si3'
_chemical_formula_weight         673.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 91.6874(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9028(5)
_cell_length_b                   25.0183(11)
_cell_length_c                   15.9058(6)
_cell_measurement_reflns_used    25779
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      1.28
_cell_volume                     3541.2(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver.1.11'
_computing_molecular_graphics    'ORTEP III'
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_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1224
_diffrn_reflns_av_unetI/netI     0.0797
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32577
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.429
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    1.384
_exptl_absorpt_correction_T_max  0.8859
_exptl_absorpt_correction_T_min  0.8578
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Higashi, 1999)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       block
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_exptl_crystal_size_max          0.190
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_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         8120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0635
_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^)+(0.0221P)^2^+6.5474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1108
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6730
_reflns_number_total             8120
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01159h2.cif
_cod_data_source_block           tara5a
_cod_database_code               7043069
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.779
_shelx_estimated_absorpt_t_max   0.809
_shelx_res_checksum              83555