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_7043072
_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         '(C31 H55 Fe Ge N O Si3), 0.5 (C7H8)'
_chemical_formula_sum            'C34.5 H59 Fe Ge N O Si3'
_chemical_formula_weight         716.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_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                 109.345(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.8319(14)
_cell_length_b                   12.2428(5)
_cell_length_c                   20.4141(9)
_cell_measurement_reflns_used    5516
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.11
_cell_volume                     7742.3(6)
_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      140(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1133
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            55443
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         1.964
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    1.269
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Higashi, 1999)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       block
_exptl_crystal_F_000             3048
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.160
_refine_diff_density_max         2.026
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         8863
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0753
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+57.6127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1393
_refine_ls_wR_factor_ref         0.1484
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6985
_reflns_number_total             8863
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01159h2.cif
_cod_data_source_block           tara3b
_cod_original_cell_volume        7742.2(6)
_cod_original_formula_sum        'C34.50 H59 Fe Ge N O Si3'
_cod_database_code               7043072
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.776
_shelx_estimated_absorpt_t_max   0.823
_shelx_res_checksum              46856