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_7039213
_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         'C15 H35 Fe N3 O Si2'
_chemical_formula_sum            'C15 H35 Fe N3 O Si2'
_chemical_formula_weight         385.49
_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     iterative
_audit_creation_date             2014-12-12
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_audit_update_record
;
2016-03-23 deposited with the CCDC.
2016-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 127.970(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3546(6)
_cell_length_b                   15.0837(4)
_cell_length_c                   17.2714(10)
_cell_measurement_reflns_used    12899
_cell_measurement_temperature    119.97(18)
_cell_measurement_theta_max      30.2490
_cell_measurement_theta_min      3.6620
_cell_volume                     2126.6(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, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.97(18)
_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 0.948
_diffrn_measurement_details
;
  1 omega  -86.00    9.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2412  -38.0000   90.0000 95

  2 omega  -20.00   27.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2412  -99.0000 -150.0000 47

  3 omega  -40.00   57.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2412   57.0000 -150.0000 97

  4 omega  -56.00   41.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       14.3350  -57.0000  -30.0000 97

  5 omega   35.00  101.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       14.3350  178.0000  -30.0000 66

  6 omega  -20.00   54.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       14.3350  -99.0000  -30.0000 74

  7 omega  -12.00   84.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       14.3350   57.0000  120.0000 96

  8 omega  -20.00   22.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2412  -99.0000  -60.0000 42

  9 omega  -36.00   59.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2412   38.0000  120.0000 95
;
_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      -0.0520534000
_diffrn_orient_matrix_UB_12      -0.0285563000
_diffrn_orient_matrix_UB_13      -0.0406167000
_diffrn_orient_matrix_UB_21      -0.0302345000
_diffrn_orient_matrix_UB_22      -0.0182804000
_diffrn_orient_matrix_UB_23      0.0238858000
_diffrn_orient_matrix_UB_31      -0.0626296000
_diffrn_orient_matrix_UB_32      0.0325911000
_diffrn_orient_matrix_UB_33      -0.0222054000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            44800
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.076
_diffrn_reflns_theta_min         2.837
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.827
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.950
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.3657
_exptl_crystal_size_mid          0.2421
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         6463
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0302P)^2^+0.7753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0826
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5349
_reflns_number_total             6463
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01208f2.cif
_cod_data_source_block           Complex1a
_cod_depositor_comments
'Adding full bibliography for 7039213--7039221.cif.'
_cod_database_code               7039213
_chemical_oxdiff_formula         'C15 H35 Fe N3 O Si2'
_chemical_oxdiff_usercomment     '@ 120 K BRML25'
_reflns_odcompleteness_completeness 99.80
_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:
 C6(H6A,H6B), C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C8(H8A,H8B,H8C), C5(H5A,H5B,H5C), C9(H9A,H9B,H9C),
 C1(H1A,H1B,H1C), C12(H12A,H12B,H12C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C),
  C11(H11A,H11B,H11C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              11239
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method Hexane