Iron(ii) β-ketiminate complexes as mediators of controlled radical polymerisation.
Lake, Benjamin R. M.; Shaver, Michael P.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 15840–15849; doi:10.1039/c6dt01208f

data_7039218
_publ_section_title
;
 Iron(ii) \b-ketiminate complexes as mediators of controlled radical
 polymerisation.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15840
_journal_page_last               15849
_journal_paper_doi               10.1039/c6dt01208f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         '2(C18 H20 Fe N2 O2)'
_chemical_formula_sum            'C36 H40 Fe2 N4 O4'
_chemical_formula_weight         704.42
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-21
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-03-23 deposited with the CCDC.
2016-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 119.539(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2528(4)
_cell_length_b                   18.5226(6)
_cell_length_c                   24.7956(13)
_cell_measurement_reflns_used    8947
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      75.6810
_cell_measurement_theta_min      4.7240
_cell_volume                     3297.7(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
  1 omega  -50.00   29.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000 -180.0000 79

  2 omega -122.00   -6.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -19.0000 -180.0000 116

  3 omega -116.00  -21.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -38.0000 -120.0000 95

  4 omega  -50.00   29.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000    0.0000 79

  5 omega   65.00  120.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1686  168.0000  171.0000 55

  6 omega   23.00   98.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1686 -125.0000 -150.0000 75

  7 omega   23.00   98.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1686 -125.0000  -30.0000 75

  8 omega   36.00   91.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000   60.0000 55

  9 omega   30.00  109.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  120.0000 79

 10 omega   94.00  178.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000    0.0000 84

 11 omega   39.00  121.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  120.0000 82

 12 omega   40.00   99.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000 -180.0000 59

 13 omega   30.00  109.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -30.0000 79

 14 omega   40.00   99.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  150.0000 59

 15 omega   30.00  109.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -180.0000 79

 16 omega   30.00  109.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -60.0000 79

 17 omega   41.00  139.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000  -60.0000 98

 18 omega   37.00  117.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -115.0000  -62.0000 80

 19 omega   94.00  178.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000  -30.0000 84

 20 omega   41.00  139.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000   60.0000 98

 21 omega   87.00  178.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000  -30.0000 91

 22 omega   87.00  178.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000  -90.0000 91

 23 omega   36.00   91.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  -30.0000 55

 24 omega   31.00  156.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -15.0000  -60.0000 125

 25 omega   87.00  178.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000 -150.0000 91

 26 omega   39.00  121.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   90.0000 82

 27 omega   39.00  113.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   60.0000 74

 28 omega   66.00   93.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  150.0000 27

 29 omega   45.00   98.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  -60.0000 53

 30 omega   92.00  121.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000    0.0000 29

 31 omega   84.00  109.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -150.0000 25

 32 omega   42.00  120.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -180.0000 78

 33 omega   72.00  121.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  150.0000 49

 34 omega  126.00  159.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000  -60.0000 33

 35 omega   89.00  168.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000  -60.0000 79
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0669363000
_diffrn_orient_matrix_UB_12      0.0236352000
_diffrn_orient_matrix_UB_13      0.1367496000
_diffrn_orient_matrix_UB_21      -0.0220829000
_diffrn_orient_matrix_UB_22      0.0785509000
_diffrn_orient_matrix_UB_23      -0.0118729000
_diffrn_orient_matrix_UB_31      -0.0113595000
_diffrn_orient_matrix_UB_32      -0.0138244000
_diffrn_orient_matrix_UB_33      0.1648464000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1062
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            53543
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.889
_diffrn_reflns_theta_min         3.145
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.420
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_description       plate
_exptl_crystal_F_000             1472
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.1677
_exptl_crystal_size_mid          0.1112
_exptl_crystal_size_min          0.0678
_refine_diff_density_max         0.689
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.200
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         6864
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.202
_refine_ls_R_factor_all          0.1020
_refine_ls_R_factor_gt           0.0861
_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^)+(0.0273P)^2^+13.7296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1848
_refine_ls_wR_factor_ref         0.1922
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5515
_reflns_number_total             6864
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01208f2.cif
_cod_data_source_block           Complex3b
_cod_depositor_comments
'Adding full bibliography for 7039213--7039221.cif.'
_cod_database_code               7039218
_chemical_oxdiff_formula         'C18 H20 Fe N2 O2'
_chemical_oxdiff_usercomment     '@ 120 K BRML246'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C22B-C23
 1.5 with sigma of 0.02
3. Restrained planarity
 C30B, C31B, C32B, C33B, C34B, C35B, C36B
 with sigma of 0.1
4. Others
 Fixed Sof: Fe2A(0.75) Fe2B(0.25) O3A(0.75) O3B(0.25) O4A(0.75) O4B(0.25)
 N3A(0.75) N3B(0.25) N4A(0.75) N4B(0.25) C25B(0.25) C26B(0.25) H26B(0.25)
 C27B(0.25) H27B(0.25) C28B(0.25) H28B(0.25) C29B(0.25) H29B(0.25) C19A(0.75)
 H19A(0.75) H19B(0.75) H19C(0.75) C19B(0.25) H19D(0.25) H19E(0.25) H19F(0.25)
 C20A(0.75) C20B(0.25) C21A(0.75) H21A(0.75) C21B(0.25) H21B(0.25) C22A(0.75)
 C22B(0.25) H23A(0.75) H23B(0.75) H23C(0.75) H23D(0.25) H23E(0.25) H23F(0.25)
 C24A(0.75) H24A(0.75) H24B(0.75) C24B(0.25) H24C(0.25) H24D(0.25) C25A(0.75)
 C26A(0.75) H26A(0.75) C27A(0.75) H27A(0.75) C28A(0.75) H28A(0.75) C29A(0.75)
 H29A(0.75) C30A(0.75) H30A(0.75) H30B(0.75) C30B(0.25) H30C(0.25) H30D(0.25)
 C31A(0.75) C32A(0.75) H32A(0.75) C33A(0.75) H33A(0.75) C34A(0.75) H34A(0.75)
 C35A(0.75) H35A(0.75) C35B(0.25) H35B(0.25) C36B(0.25) H36B(0.25) C31B(0.25)
 C32B(0.25) H32B(0.25) C33B(0.25) H33B(0.25) C34B(0.25) H34B(0.25) C36A(0.75)
 H36A(0.75)
5.a Secondary CH2 refined with riding coordinates:
 C24A(H24A,H24B), C24B(H24C,H24D), C30A(H30A,H30B), C30B(H30C,H30D), C6(H6A,
 H6B), C12(H12A,H12B)
5.b Me refined with riding coordinates:
 C23(H23A,H23B,H23C), C23(H23D,H23E,H23F)
5.c Aromatic/amide H refined with riding coordinates:
 C26B(H26B), C27B(H27B), C28B(H28B), C29B(H29B), C21A(H21A), C21B(H21B),
 C26A(H26A), C27A(H27A), C28A(H28A), C29A(H29A), C32A(H32A), C33A(H33A),
 C34A(H34A), C35A(H35A), C35B(H35B), C36B(H36B), C32B(H32B), C33B(H33B),
 C34B(H34B), C36A(H36A), C3(H3), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18)
5.d Fitted hexagon refined as free rotating group:
 N4B(C25B,C26B,C27B,C28B,C29B), C35B(C36B,C31B,C32B,C33B,C34B)
5.e Idealised Me refined as rotating group:
 C19A(H19A,H19B,H19C), C19B(H19D,H19E,H19F), C1(H1A,H1B,H1C), C5(H5A,H5B,H5C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method Toluene/Hexane