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_4516677
_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         'C34 H27 Fe N3, 2(C2 H3 N)'
_chemical_formula_sum            'C38 H33 Fe N5'
_chemical_formula_weight         615.54
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_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            4
_cell_length_a                   16.9958(7)
_cell_length_b                   10.2025(5)
_cell_length_c                   17.6294(7)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.89
_cell_measurement_theta_min      2.31
_cell_volume                     3056.9(2)
_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 0.997
_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  0.0348
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            37616
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.962
_diffrn_reflns_theta_min         2.306
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.529
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6572
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0764 before and 0.0552 after correction.
The Ratio of minimum to maximum transmission is 0.8810.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.063(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         8801
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+0.4040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0818
_reflns_Friedel_coverage         0.943
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                7780
_reflns_number_total             8801
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs5b01416_si_006.cif
_cod_data_source_block           Compound4b
_cod_database_code               4516677
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.849
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.937(15) 0.063(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C19(H19), C16(H16), C20(H20), C5(H5), C1(H1), C4(H4)
3.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C31(H31), C10(H10), C27(H27), C30(H30), C23(H23), C9(H9), C8(H8),
 C29(H29), C32(H32), C12(H12), C15(H15), C13(H13), C11(H11), C28(H28), C24(H24),
  C14(H14), C25(H25)
3.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              48130
_shelx_hkl_checksum              72047
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'