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_7039217
_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         'C32 H48 Fe2 N4 O4'
_chemical_formula_sum            'C32 H48 Fe2 N4 O4'
_chemical_formula_weight         664.44
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-02-17
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Olex2 1.2
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_audit_update_record
;
2016-03-23 deposited with the CCDC.
2016-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                84.382(3)
_cell_angle_beta                 72.596(4)
_cell_angle_gamma                86.906(3)
_cell_formula_units_Z            1
_cell_length_a                   7.8337(3)
_cell_length_b                   10.2379(3)
_cell_length_c                   10.7448(4)
_cell_measurement_reflns_used    17846
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      30.7190
_cell_measurement_theta_min      3.3530
_cell_volume                     818.06(5)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_reduction
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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)'
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Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
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_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_details
;
  1 omega  -12.00   85.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912   57.0000   60.0000 97

  2 omega  -17.00   88.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912   77.0000 -180.0000 105

  3 omega   -8.00   87.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912   38.0000  -60.0000 95

  4 omega  -56.00   41.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912  -57.0000  -90.0000 97

  5 omega  -73.00  -27.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.3975  132.0000  131.3605 46

  6 omega  -90.00  -44.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.3975  161.0000   26.0000 46

  7 omega   35.00  101.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912  178.0000  -90.0000 66

  8 omega   -8.00   87.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912   38.0000   30.0000 95

  9 omega   34.00  100.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912 -178.0000   60.0000 66

 10 omega    0.00   68.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912 -123.0000  112.6844 68

 11 omega  -72.00  -27.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.3975  130.0000 -120.9467 45

 12 omega  -73.00  -27.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.3975  132.0000  -59.3551 46

 13 omega  -89.00  -39.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.3975  155.0000  169.8001 50

 14 omega    6.00   73.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912 -130.0000 -103.1869 67

 15 omega  -20.00   54.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912  -99.0000    0.0000 74

 16 omega   -5.00   65.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912 -117.0000  148.0000 70

 17 omega  -73.00  -27.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.3975  132.0000   90.5802 46

 18 omega   35.00  101.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912  178.0000   90.0000 66

 19 omega   35.00  101.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912  178.0000  150.0000 66

 20 omega  -72.00  -10.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912    0.0000 -180.0000 62

 21 omega   35.00  101.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912  178.0000 -120.0000 66
;
_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      -0.0429125000
_diffrn_orient_matrix_UB_12      0.0067715000
_diffrn_orient_matrix_UB_13      0.0673374000
_diffrn_orient_matrix_UB_21      0.0079178000
_diffrn_orient_matrix_UB_22      -0.0688605000
_diffrn_orient_matrix_UB_23      0.0137759000
_diffrn_orient_matrix_UB_31      0.0842964000
_diffrn_orient_matrix_UB_32      0.0078763000
_diffrn_orient_matrix_UB_33      0.0098672000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            35409
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.142
_diffrn_reflns_theta_min         2.862
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.927
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_correction_T_min  0.709
_exptl_absorpt_correction_type   gaussian
_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)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       plate
_exptl_crystal_F_000             352
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.6512
_exptl_crystal_size_mid          0.1049
_exptl_crystal_size_min          0.1016
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         4970
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0235P)^2^+0.4478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0723
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4603
_reflns_number_total             4970
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01208f2.cif
_cod_data_source_block           Complex1b
_cod_depositor_comments
'Adding full bibliography for 7039213--7039221.cif.'
_cod_original_cell_volume        818.06(6)
_cod_database_code               7039217
_chemical_oxdiff_formula         'C16 H24 Fe N2 O2'
_chemical_oxdiff_usercomment     '@ 120 K BRML51'
_reflns_odcompleteness_completeness 99.85
_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.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C6(H6A,H6B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C15(H15), C14(H14), C13(H13), C16(H16), C12(H12)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method Hexane