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_7043070
_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 H55 Fe Ge N O S Si3'
_chemical_formula_weight         702.53
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-05-11 deposited with the CCDC.
2017-05-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.6371(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8979(6)
_cell_length_b                   16.6926(6)
_cell_length_c                   17.0382(7)
_cell_measurement_reflns_used    62621
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      1.22
_cell_volume                     3635.8(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_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 0.994
_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  0.0846
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
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_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            54145
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.452
_diffrn_reflns_theta_min         1.593
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    1.405
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_exptl_absorpt_correction_T_min  0.6855
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Higashi, 1999)'
_exptl_crystal_colour            red
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_exptl_crystal_description       block
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_refine_diff_density_max         0.627
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         8270
_refine_ls_number_restraints     0
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_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1287
_refine_ls_wR_factor_ref         0.1367
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7095
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_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01159h2.cif
_cod_data_source_block           tara7a
_cod_database_code               7043070
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.596
_shelx_estimated_absorpt_t_max   0.703
_shelx_res_checksum              90324