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_4516679
_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         'C32 H24 Cl2 Fe N2'
_chemical_formula_sum            'C32 H24 Cl2 Fe N2'
_chemical_formula_weight         563.28
_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'
_atom_sites_solution_hydrogens   geom
_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                 99.058(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.5314(5)
_cell_length_b                   9.7274(2)
_cell_length_c                   13.9300(4)
_cell_measurement_reflns_used    8616
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.05
_cell_measurement_theta_min      2.34
_cell_volume                     2613.55(11)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.967
_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  0.0619
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34180
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.132
_diffrn_reflns_theta_min         2.112
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.806
_exptl_absorpt_correction_T_max  0.8622
_exptl_absorpt_correction_T_min  0.7186
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1051 before and 0.0564 after correction.
The Ratio of minimum to maximum transmission is 0.8334.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       needle
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.082
_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     334
_refine_ls_number_reflns         7452
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0465P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0982
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5389
_reflns_number_total             7452
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs5b01416_si_003.cif
_cod_data_source_block           Compound1a
_cod_database_code               4516679
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.661
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C16(H16)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C11(H11), C15(H15), C8(H8), C10(H10), C12(H12), C9(H9),
 C14(H14), C13(H13), C19(H19), C20(H20), C23(H23), C30(H30), C25(H25), C24(H24),
  C26(H26), C27(H27), C29(H29), C28(H28), C31(H31), C32(H32)
;
_shelx_res_checksum              39852
_shelx_hkl_checksum              12396
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'