Transfer Reagent for Bonding Isomers of Iron Complexes.
Schmidt, Monika; Seitz, Andreas E.; Eckhardt, Maria; Balázs, Gábor; Peresypkina, Eugenia V.; Virovets, Alexander V.; Riedlberger, Felix; Bodensteiner, Michael; Zolnhofer, Eva M.; Meyer, Karsten; Scheer, Manfred; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b07354

data_4126496
_publ_section_title
;
 Transfer Reagent for Bonding Isomers of Iron Complexes.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b07354
_journal_year                    2017
_chemical_formula_moiety         'C34 H58 As4 Fe2'
_chemical_formula_structural     'Cp(t-Bu)3 Fe As4 Fe Cp(t-Bu)3'
_chemical_formula_sum            'C136 H232 As16 Fe8'
_chemical_formula_weight         3512.72
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 102.137(2)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   14.5980(2)
_cell_length_b                   13.8302(2)
_cell_length_c                   18.4082(3)
_cell_measurement_reflns_used    17066
_cell_measurement_temperature    123.0(2)
_cell_measurement_theta_max      73.0367
_cell_measurement_theta_min      3.0939
_cell_volume                     3633.42(10)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.61 (release 04-03-2010 CrysAlis171 .NET)
(compiled Mar  4 2010,15:49:12)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.61 (release 04-03-2010 CrysAlis171 .NET)
(compiled Mar  4 2010,15:49:12)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.61 (release 04-03-2010 CrysAlis171 .NET)
(compiled Mar  4 2010,15:49:12)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123.0(2)
_diffrn_detector_area_resol_mean 10.5431
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24572
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        70.000
_diffrn_reflns_theta_max         73.186
_diffrn_reflns_theta_min         3.525
_exptl_absorpt_coefficient_mu    10.600
_exptl_absorpt_correction_T_max  0.501
_exptl_absorpt_correction_T_min  0.135
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.61 (release 04-03-2010 CrysAlis171 .NET)
(compiled Mar  4 2010,15:49:12)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_description       'thick plate'
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.3970
_exptl_crystal_size_mid          0.2929
_exptl_crystal_size_min          0.0741
_refine_diff_density_max         1.248
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         7159
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0875P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1119
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6437
_reflns_number_total             7159
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b07354_si_006.cif
_cod_data_source_block           2a
_cod_database_code               4126496
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.102
_shelx_estimated_absorpt_t_max   0.507
_shelx_res_checksum              95791
_shelx_hkl_checksum              14107