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_4126493
_publ_section_title
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 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         '(C80 H70 As5 Fe2), (B F4), (C H2 Cl2)0.5'
_chemical_formula_structural     '[(C40 H35 Fe)2 As5](B F4)*0.5(C H2 Cl2)'
_chemical_formula_sum            'C80.5 H71 As5 B Cl F4 Fe2'
_chemical_formula_weight         1646.93
_space_group_crystal_system      orthorhombic
_space_group_IT_number           30
_space_group_name_Hall           'P 2 -2bc'
_space_group_name_H-M_alt        'P n c 2'
_symmetry_space_group_name_Hall  'P 2 -2bc'
_symmetry_space_group_name_H-M   'P n c 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.10717(18)
_cell_length_b                   22.29586(14)
_cell_length_c                   19.62199(12)
_cell_measurement_reflns_used    73472
_cell_measurement_temperature    122.8(7)
_cell_measurement_theta_max      66.4390
_cell_measurement_theta_min      4.0990
_cell_volume                     13609.05(14)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      122.8(7)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            127713
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.700
_diffrn_reflns_theta_max         66.700
_diffrn_reflns_theta_min         3.320
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.916
_exptl_absorpt_correction_T_max  0.478
_exptl_absorpt_correction_T_min  0.151
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
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CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_description       'trucnacted prism'
_exptl_crystal_F_000             6632
_exptl_crystal_size_max          0.347
_exptl_crystal_size_mid          0.298
_exptl_crystal_size_min          0.127
_refine_diff_density_max         0.814
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.477(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1725
_refine_ls_number_reflns         23841
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0238
_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^)+(0.0407P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0589
_reflns_Friedel_coverage         0.937
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                22300
_reflns_number_total             23841
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b07354_si_009.cif
_cod_data_source_block           4
_cod_original_formula_sum        'C80.50 H71 As5 B Cl F4 Fe2'
_cod_database_code               4126493
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.473
_shelx_estimated_absorpt_t_min   0.197
_shelx_res_checksum              98465
_shelx_hkl_checksum              27637
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.300
_oxdiff_exptl_absorpt_empirical_full_min 0.875