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_7039216
_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         'C18 H33 Fe N3 O2 Si2'
_chemical_formula_sum            'C18 H33 Fe N3 O2 Si2'
_chemical_formula_weight         435.50
_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     direct
_audit_creation_date             2015-06-24
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;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-03-23 deposited with the CCDC.
2016-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.425(4)
_cell_angle_beta                 100.153(5)
_cell_angle_gamma                97.601(5)
_cell_formula_units_Z            2
_cell_length_a                   8.8657(6)
_cell_length_b                   10.8724(6)
_cell_length_c                   12.2568(5)
_cell_measurement_reflns_used    9506
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      30.3150
_cell_measurement_theta_min      3.3770
_cell_volume                     1152.16(11)
_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)
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_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    '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 0.916
_diffrn_measurement_details
;
  1 omega  -40.00   57.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.0850   57.0000  -30.0000 97

  2 omega  -20.00   27.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.0850  -99.0000  -30.0000 47

  3 omega  -86.00    9.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.0850  -38.0000   30.0000 95

  4 omega  -83.00   14.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.0850  -57.0000 -180.0000 97

  5 omega -100.00   74.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.0850    0.0000 -180.0000 174

  6 omega   35.00  101.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6475  178.0000 -150.0000 66

  7 omega  -20.00   51.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6475  -99.0000   90.0000 71

  8 omega   34.00  100.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6475 -178.0000  -30.0000 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      0.0119947000
_diffrn_orient_matrix_UB_12      0.0625347000
_diffrn_orient_matrix_UB_13      0.0200417000
_diffrn_orient_matrix_UB_21      0.0121020000
_diffrn_orient_matrix_UB_22      -0.0204283000
_diffrn_orient_matrix_UB_23      0.0552970000
_diffrn_orient_matrix_UB_31      0.0802477000
_diffrn_orient_matrix_UB_32      0.0028690000
_diffrn_orient_matrix_UB_33      -0.0005818000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24682
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.030
_diffrn_reflns_theta_min         2.814
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.774
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.905
_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_density_diffrn    1.255
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.4065
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.1573
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         6749
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0448P)^2^+0.3264P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1088
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5501
_reflns_number_total             6749
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01208f2.cif
_cod_data_source_block           Complex4a
_cod_depositor_comments
'Adding full bibliography for 7039213--7039221.cif.'
_cod_database_code               7039216
_chemical_oxdiff_formula         'C18 H33 Fe N3 O2 Si2'
_chemical_oxdiff_usercomment     '@ 120 K BRML123'
_reflns_odcompleteness_completeness 99.87
_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)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C10(H10), C11(H11)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method Hexane