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_4126495
_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         'C80 H70 As4 Fe2'
_chemical_formula_sum            'C80 H70 As4 Fe2'
_chemical_formula_weight         1442.74
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-08-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.0053(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.03997(19)
_cell_length_b                   31.6780(5)
_cell_length_c                   19.6456(4)
_cell_measurement_reflns_used    18278
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      73.2240
_cell_measurement_theta_min      4.3200
_cell_volume                     6232.9(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      123(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
  1 omega  -20.00   81.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       40.5337  -99.0000  -60.0000 101

  2 omega  -27.00   66.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       40.5337  -57.0000   30.0000 93

  3 omega   17.00  114.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       40.5337   57.0000 -180.0000 97

  4 omega   43.00   69.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.4027  -30.0000  -60.0000 26

  5 omega   43.00   69.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.4027  -30.0000   60.0000 26

  6 omega   19.00  145.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.4027    0.0000  -90.0000 126

  7 omega   48.00  150.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.4027  178.0000    0.0000 102

  8 omega   23.00   79.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.4027  -94.0000    0.0000 56

  9 omega   36.00  111.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.4027 -111.0000  -30.0000 75

 10 omega   28.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.4027  -94.0000   90.0000 81

 11 omega   80.00  158.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.4027   77.0000   90.0000 78

 12 omega   29.00  115.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.4027 -111.0000   60.0000 86

 13 omega   33.00   59.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.4027  -30.0000    0.0000 26

 14 omega   33.00  138.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.4027  -61.0000  120.0000 105

 15 omega   11.00  114.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       40.5337   57.0000    0.0000 103

 16 omega   11.00  114.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       40.5337   57.0000  -90.0000 103

 17 omega   11.00  114.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       40.5337   57.0000   90.0000 103

 18 omega   80.00  158.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.4027   45.0000    0.0000 78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1024638000
_diffrn_orient_matrix_UB_12      -0.0075379000
_diffrn_orient_matrix_UB_13      -0.0535684000
_diffrn_orient_matrix_UB_21      -0.0836286000
_diffrn_orient_matrix_UB_22      0.0275771000
_diffrn_orient_matrix_UB_23      -0.0514736000
_diffrn_orient_matrix_UB_31      0.0783806000
_diffrn_orient_matrix_UB_32      0.0393425000
_diffrn_orient_matrix_UB_33      0.0258073000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            49715
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.559
_diffrn_reflns_theta_min         3.588
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.443
_exptl_absorpt_correction_T_max  0.759
_exptl_absorpt_correction_T_min  0.418
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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            'light brown'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       plate
_exptl_crystal_F_000             2936
_exptl_crystal_recrystallization_method
'layering a dichlormethane solution with hexane'
_exptl_crystal_size_max          0.1961
_exptl_crystal_size_mid          0.1652
_exptl_crystal_size_min          0.0678
_refine_diff_density_max         0.919
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         12353
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0572P)^2^+2.3655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.0999
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11178
_reflns_number_total             12353
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b07354_si_008.cif
_cod_data_source_block           1
_cod_original_cell_volume        6232.95(19)
_cod_database_code               4126495
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         C80H70Fe2As4
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C20(H20A,H20B), C53(H53A,H53B), C46(H46A,H46B), C27(H27A,
 H27B), C34(H34A,H34B), C74(H74A,H74B), C6(H6A,H6B), C67(H67A,H67B), C60(H60A,
 H60B)
2.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C10(H10), C8(H8), C16(H16), C11(H11), C30(H30), C48(H48), C32(H32),
 C9(H9), C26(H26), C36(H36), C12(H12), C79(H79), C65(H65), C66(H66), C40(H40),
 C15(H15), C29(H29), C62(H62), C55(H55), C49(H49), C58(H58), C64(H64), C33(H33),
  C80(H80), C17(H17), C78(H78), C19(H19), C57(H57), C63(H63), C38(H38),
 C59(H59), C25(H25), C37(H37), C24(H24), C52(H52), C77(H77), C23(H23), C39(H39),
  C73(H73), C18(H18), C22(H22), C56(H56), C50(H50), C76(H76), C71(H71),
 C69(H69), C72(H72), C51(H51), C70(H70)
;
_olex2_submission_original_sample_id SM100_3hellbraun
_olex2_submission_special_instructions 'No special instructions were received'