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_4516676
_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         'C50 H39 Fe N2 P, C6 H14'
_chemical_formula_sum            'C56 H53 Fe N2 P'
_chemical_formula_weight         840.82
_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
_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                 93.471(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7305(15)
_cell_length_b                   14.4122(7)
_cell_length_c                   17.4229(8)
_cell_measurement_reflns_used    5424
_cell_measurement_temperature    106.2(2)
_cell_measurement_theta_max      27.0350
_cell_measurement_theta_min      3.0630
_cell_volume                     4193.4(5)
_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)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      106.2(2)
_diffrn_detector_area_resol_mean 16.0839
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.873
_diffrn_measurement_details
;
  1 omega  -14.00   22.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9802  -99.0000 -180.0000 36

  2 omega  -50.00   80.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490    0.0000   90.0000 130

  3 omega    6.00   63.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490   57.0000  120.0000 57

  4 omega  -39.00   41.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9802   57.0000    0.0000 80
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0265339000
_diffrn_orient_matrix_UB_12      0.0366729000
_diffrn_orient_matrix_UB_13      0.0110789000
_diffrn_orient_matrix_UB_21      0.0330032000
_diffrn_orient_matrix_UB_22      -0.0276187000
_diffrn_orient_matrix_UB_23      -0.0097150000
_diffrn_orient_matrix_UB_31      -0.0034676000
_diffrn_orient_matrix_UB_32      0.0176610000
_diffrn_orient_matrix_UB_33      -0.0380385000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_unetI/netI     0.1068
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.873
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26124
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.873
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.100
_diffrn_reflns_theta_min         2.819
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.440
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98022
_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 brown'
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       plate
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.993
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         9822
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.1173
_refine_ls_R_factor_gt           0.0785
_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^)+(0.0484P)^2^+7.1965P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.1723
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6981
_reflns_number_total             9822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs5b01416_si_007.cif
_cod_data_source_block           Compound4c
_cod_database_code               4516676
_chemical_oxdiff_formula         Fe1N2C40H404P1
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Restrained distances
 C55-C54
 1.54 with sigma of 0.01
3. Rigid body (RIGU) restrains
 C56, C55, C54, C53, C52, C51
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 C20(H20), C19(H19), C5(H5), C16(H16), C4(H4), C1(H1)
4.b Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B), C52(H52A,H52B), C55(H55A,H55B), C54(H54A,H54B)
4.c Aromatic/amide H refined with riding coordinates:
 C27(H27), C29(H29), C30(H30), C50(H50), C28(H28), C37(H37), C38(H38),
 C43(H43), C46(H46), C34(H34), C23(H23), C31(H31), C8(H8), C26(H26), C32(H32),
 C44(H44), C24(H24), C9(H9), C12(H12), C42(H42), C10(H10), C48(H48), C36(H36),
 C40(H40), C25(H25), C35(H35), C49(H49), C13(H13), C41(H41), C11(H11), C14(H14),
  C15(H15), C47(H47)
4.d Idealised Me refined as rotating group:
 C56(H56A,H56B,H56C), C51(H51A,H51B,H51C)
;
_shelx_res_checksum              15834
_shelx_hkl_checksum              34240
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'