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_4516675
_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         'C35 H33 Fe N2 O3 P'
_chemical_formula_sum            'C35 H33 Fe N2 O3 P'
_chemical_formula_weight         616.45
_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                 112.094(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1400(9)
_cell_length_b                   13.3999(9)
_cell_length_c                   16.5218(10)
_cell_measurement_reflns_used    9823
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      31.10
_cell_measurement_theta_min      2.84
_cell_volume                     2900.6(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.899
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            50454
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.529
_diffrn_reflns_theta_min         2.223
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6954
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0464 before and 0.0430 after correction.
The Ratio of minimum to maximum transmission is 0.9319.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.730
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         8707
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0387
_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          0.1220
_refine_ls_wR_factor_ref         0.1352
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7023
_reflns_number_total             8707
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs5b01416_si_008.cif
_cod_data_source_block           Compound4d
_cod_database_code               4516675
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.809
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C19(H19), C16(H16), C1(H1), C4(H4), C20(H20), C5(H5)
2.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C23(H23), C31(H31), C12(H12), C11(H11), C27(H27), C15(H15),
 C28(H28), C24(H24), C26(H26), C13(H13), C8(H8), C29(H29), C9(H9), C25(H25),
 C30(H30), C14(H14), C10(H10)
2.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              59445
_shelx_hkl_checksum              7405
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'