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_4516674
_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         'C44 H56 Fe Li N2 O Si2'
_chemical_formula_sum            'C44 H56 Fe Li N2 O Si2'
_chemical_formula_weight         747.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 103.752(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3913(5)
_cell_length_b                   26.6073(12)
_cell_length_c                   13.8664(7)
_cell_measurement_reflns_used    2790
_cell_measurement_temperature    102(1)
_cell_measurement_theta_max      27.5550
_cell_measurement_theta_min      3.0470
_cell_volume                     4082.3(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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      102(1)
_diffrn_detector_area_resol_mean 16.0839
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -14.00   20.00   1.0000   27.9500
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -99.0000   30.0000 34

  2 omega  -47.00   44.00   1.0000   27.9500
omega____ theta____ kappa____ phi______ frames
    -       22.2592  -57.0000 -150.0000 91

  3 omega   38.00   74.00   1.0000   27.9500
omega____ theta____ kappa____ phi______ frames
    -       22.2592  179.0000 -180.0000 36

  4 omega    1.00   91.00   1.0000   27.9500
omega____ theta____ kappa____ phi______ frames
    -       22.2592   57.0000    0.0000 90
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0006739000
_diffrn_orient_matrix_UB_12      -0.0241402000
_diffrn_orient_matrix_UB_13      -0.0218058000
_diffrn_orient_matrix_UB_21      -0.0159723000
_diffrn_orient_matrix_UB_22      0.0110258000
_diffrn_orient_matrix_UB_23      -0.0479264000
_diffrn_orient_matrix_UB_31      0.0620815000
_diffrn_orient_matrix_UB_32      0.0025316000
_diffrn_orient_matrix_UB_33      0.0003469000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_unetI/netI     0.0827
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17142
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.943
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.463
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90377
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       needle
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         7217
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0703
_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^)+(0.0391P)^2^+2.9054P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1311
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5628
_reflns_number_total             7217
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs5b01416_si_004.cif
_cod_data_source_block           Compound3
_cod_database_code               4516674
_chemical_oxdiff_formula         C40H40N2FeSi2
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C5(H5), C4(H4), C1(H1), C32(H32), C31(H31), C16(H16), C19(H19), C20(H20)
2.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C37(H37A,H37B), C43(H43A,H43B), C42(H42A,H42B)
2.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C14(H14), C12(H12), C8(H8), C11(H11), C10(H10), C9(H9), C13(H13),
 C25(H25), C26(H26), C23(H23), C24(H24), C27(H27), C30(H30), C29(H29), C28(H28)
2.d Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C35(H35A,H35B,H35C), C34(H34A,H34B,H34C), C39(H39A,H39B,
 H39C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C44(H44A,H44B,H44C), C41(H41A,
 H41B,H41C)
;
_shelx_res_checksum              57863
_shelx_hkl_checksum              9451
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'