Low-Valent Iron Mono-Diazadiene Compounds: Electronic Structure and Catalytic Application
Lichtenberg, Crispin; Adelhardt, Mario; Gianetti, Thomas L.; Meyer, Karsten; de Bruin, Bas; Grützmacher, Hansjörg; ACS Catalysis 5 (2015) 6230–; doi:10.1021/acscatal.5b01416

data_4516678
_publ_section_title
;
 Low-Valent Iron Mono-Diazadiene Compounds: Electronic Structure and
 Catalytic Application
;
_journal_issue                   10
_journal_name_full               'ACS Catalysis'
_journal_page_first              6230
_journal_paper_doi               10.1021/acscatal.5b01416
_journal_volume                  5
_journal_year                    2015
_chemical_formula_moiety
'8(C36 H32 Fe N2 O), 4(C20 H40 F6 Na O5 P), 0.17(O4)'
_chemical_formula_sum            'C368 H416 F24 Fe8 N16 Na4 O28.7 P4'
_chemical_formula_weight         6640.98
_space_group_crystal_system      tetragonal
_space_group_IT_number           128
_space_group_name_Hall           '-P 4 2n'
_space_group_name_H-M_alt        'P 4/m n c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-16
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   17.2377(5)
_cell_length_b                   17.2377(5)
_cell_length_c                   27.3182(8)
_cell_measurement_reflns_used    9798
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      2.24
_cell_volume                     8117.3(4)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            69422
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.519
_diffrn_reflns_theta_min         1.397
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.456
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6977
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1286 before and 0.0442 after correction.
The Ratio of minimum to maximum transmission is 0.9356.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       block
_exptl_crystal_F_000             3494
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         2.201
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5272
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0650P)^2^+9.9070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1429
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4024
_reflns_number_total             5272
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs5b01416_si_005.cif
_cod_data_source_block           Compound4a
_cod_original_cell_volume        8117.3(5)
_cod_original_formula_sum        'C368 H416 F24 Fe8 N16 Na4 O28.70 P4'
_cod_database_code               4516678
_shelx_estimated_absorpt_t_max   0.804
_shelx_estimated_absorpt_t_min   0.804
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C28) = Uanis(C27) = Uanis(C26) = Uanis(C25)
3. Rigid body (RIGU) restrains
 O2A, C21A, C22A, C23A, C24A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C22A)=Sof(H22C)=Sof(H22D)=Sof(C23A)=Sof(H23C)=Sof(H23D)=Sof(C21A)=
 Sof(H21C)=Sof(H21D)=Sof(O2A)=Sof(C24A)=Sof(H24C)=Sof(H24D)=1-FVAR(1)
 Sof(O2)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C22)=
 Sof(H22A)=Sof(H22B)=Sof(C21)=Sof(H21A)=Sof(H21B)=FVAR(1)
 Fixed Sof: C20(0.5) H20A(0.5) H20B(0.5) C18(0.5) H18A(0.5) H18B(0.5) C17(0.5)
 H17A(0.5) H17B(0.5) C19(0.5) H19A(0.5) H19B(0.5) O3(0.25) C25(0.25) H25A(0.25)
 H25B(0.25) C26(0.25) H26A(0.25) H26B(0.25) C27(0.25) H27A(0.25) H27B(0.25)
 C28(0.25) H28A(0.25) H28B(0.25)
5.a Free rotating group:
 O3(C25,C26,C27,C28,O4)
5.b Ternary CH refined with riding coordinates:
 C5(H5), C4(H4), C1(H1)
5.c Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C18(H18A,H18B), C17(H17A,H17B), C23(H23A,H23B), C24(H24A,
 H24B), C22(H22A,H22B), C21(H21A,H21B), C19(H19A,H19B), C25(H25A,H25B),
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C22A(H22C,H22D), C23A(H23C,
 H23D), C21A(H21C,H21D), C24A(H24C,H24D)
5.d Aromatic/amide H refined with riding coordinates:
 C16(H16), C12(H12), C15(H15), C11(H11), C13(H13), C9(H9), C14(H14), C8(H8),
 C10(H10)
;
_shelx_res_checksum              69235
_shelx_hkl_checksum              79470
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'