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_7039215
_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         'C17 H31 Fe N3 O Si2'
_chemical_formula_sum            'C17 H31 Fe N3 O Si2'
_chemical_formula_weight         405.48
_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             2015-02-19
_audit_creation_method
;
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
_cell_angle_beta                 103.421(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8709(5)
_cell_length_b                   16.3660(5)
_cell_length_c                   8.6899(3)
_cell_measurement_reflns_used    11441
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      28.1380
_cell_measurement_theta_min      3.3560
_cell_volume                     2195.50(13)
_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
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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)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_details
;
  1 omega  -20.00   30.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.4310  -99.0000 -180.0000 50

  2 omega  -12.00   83.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.5247   38.0000   60.0000 95

  3 omega  -12.00   83.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.5247   38.0000 -180.0000 95

  4 omega  -62.00   33.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.5247  -38.0000   30.0000 95

  5 omega  -20.00   50.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.5247  -99.0000  -60.0000 70

  6 omega  -16.00   81.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.5247   57.0000 -120.0000 97

  7 omega  -62.00   -9.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.5247  -38.0000   90.0000 53

  8 omega   13.00   79.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.5247 -146.0000 -113.4498 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      0.0237757000
_diffrn_orient_matrix_UB_12      0.0352618000
_diffrn_orient_matrix_UB_13      0.0317230000
_diffrn_orient_matrix_UB_21      -0.0308984000
_diffrn_orient_matrix_UB_22      0.0250397000
_diffrn_orient_matrix_UB_23      -0.0508693000
_diffrn_orient_matrix_UB_31      -0.0243322000
_diffrn_orient_matrix_UB_32      0.0025962000
_diffrn_orient_matrix_UB_33      0.0587394000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            38643
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.665
_diffrn_reflns_theta_min         2.712
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_T_max  0.977
_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            'intense green'
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       plate
_exptl_crystal_F_000             864
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.4586
_exptl_crystal_size_mid          0.1651
_exptl_crystal_size_min          0.109
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         5793
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0257P)^2^+1.7038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.0915
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4655
_reflns_number_total             5793
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01208f2.cif
_cod_data_source_block           Complex3a
_cod_depositor_comments
'Adding full bibliography for 7039213--7039221.cif.'
_cod_original_cell_volume        2195.50(12)
_cod_database_code               7039215
_chemical_oxdiff_formula         'C17 H31 Fe N3 O Si2'
_chemical_oxdiff_usercomment     '@ 120 K BRML60'
_reflns_odcompleteness_completeness 99.79
_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), C9(H9), 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)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method Hexane