Bis(silylenyl)-substituted ferrocene-stabilized 6-arene iron(0) complexes: synthesis, structure and catalytic application
Driess, Matthias; Luecke, Marcel Philip; Porwal, Digvijay; Kostenko, Arseni; Zhou, Yupeng; Yao, Shenglai; Keck, Matthias; Limberg, Christian; Oestreich, Martin; Dalton Trans.  (2017) –; doi:10.1039/C7DT03301J

data_7044253
_publ_section_title
;
 Bis(silylenyl)-substituted ferrocene-stabilized 6-arene iron(0)
 complexes: synthesis, structure and catalytic application
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03301J
_journal_year                    2017
_chemical_formula_sum            'C47 H62 Br2 Fe N4 Ni Si2'
_chemical_formula_weight         1013.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc1m3f49
_audit_creation_method           'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_audit_update_record
;
2016-07-13 deposited with the CCDC.
2017-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.0990(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.2617(4)
_cell_length_b                   8.97920(10)
_cell_length_c                   17.6242(2)
_cell_measurement_reflns_used    10685
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.9810
_cell_measurement_theta_min      4.5210
_cell_volume                     4627.59(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30160
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         67.50
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    5.814
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10506
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.281
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         8339
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+3.8691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.1023
_reflns_number_gt                7004
_reflns_number_total             8339
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt03301j2.cif
_cod_data_source_block           SiFcSiNiBr2
_cod_original_sg_symbol_H-M      p21/c
_cod_database_code               7044253