Mono- and Dinuclear Neutral and Cationic Iron(II) Compounds Supported by an Amidinato-diolefin Ligand: Characterization and Catalytic Application
Lichtenberg, Crispin; Adelhardt, Mario; Wörle, Michael; Büttner, Torsten; Meyer, Karsten; Grützmacher, Hansjörg; Organometallics 34 (2015) 3079–; doi:10.1021/acs.organomet.5b00395

data_4085916
_publ_section_title
;
 Mono- and Dinuclear Neutral and Cationic Iron(II) Compounds Supported by
 an Amidinato-diolefin Ligand: Characterization and Catalytic Application
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3079
_journal_paper_doi               10.1021/acs.organomet.5b00395
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C37 H28 N2'
_chemical_formula_sum            'C37 H28 N2'
_chemical_formula_weight         500.61
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-09-19
_audit_creation_method
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Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.833(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8479(8)
_cell_length_b                   17.9934(12)
_cell_length_c                   14.5763(10)
_cell_measurement_reflns_used    3921
_cell_measurement_temperature    104(3)
_cell_measurement_theta_max      30.4090
_cell_measurement_theta_min      3.6880
_cell_volume                     2708.5(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
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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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)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      104(3)
_diffrn_detector_area_resol_mean 16.0839
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_details
;
  1 omega  -46.00   48.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.1029   77.0000   90.0000 94

  2 omega  -66.00  -37.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.1029 -179.0000  -90.0000 29

  3 omega  -14.00   20.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.1029  -99.0000 -120.0000 34

  4 omega  -25.00   13.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.1029  -99.0000  -30.0000 38

  5 omega   41.00   77.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.5717   57.0000 -120.0000 36
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0214398000
_diffrn_orient_matrix_UB_12      0.0217055000
_diffrn_orient_matrix_UB_13      0.0328585000
_diffrn_orient_matrix_UB_21      -0.0541451000
_diffrn_orient_matrix_UB_22      -0.0238038000
_diffrn_orient_matrix_UB_23      -0.0068498000
_diffrn_orient_matrix_UB_31      0.0364060000
_diffrn_orient_matrix_UB_32      -0.0226760000
_diffrn_orient_matrix_UB_33      0.0385731000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13456
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.452
_diffrn_reflns_theta_min         3.003
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71730
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         7342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_gt           0.0685
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1719
_refine_ls_wR_factor_ref         0.1898
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5603
_reflns_number_total             7342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00395_si_003.cif
_cod_data_source_block           Compound_1
_cod_depositor_comments
'Adding full bibliography for 4085916--4085926.cif.'
_cod_database_code               4085916
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         N2C40H40
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1A), C16(H16)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C11(H11), C4(H4), C5(H5), C19(H19), C10(H10), C26(H26), C30(H30),
 C9(H9), C37(H37), C23(H23), C15(H15), C33(H33), C20(H20), C12(H12), C36(H36),
 C14(H14), C25(H25), C27(H27), C35(H35), C29(H29), C13(H13), C24(H24), C34(H34),
  C28(H28)
;
_shelx_res_checksum              92565
_shelx_hkl_checksum              25492
_olex2_submission_special_instructions 'No special instructions were received'