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_7039219
_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
'C54 H60 Fe2 N4 O4, 0.833(C7 H8), 0.167(C6 H14)'
_chemical_formula_sum            'C60.83 H69 Fe2 N4 O4'
_chemical_formula_weight         1031.90
_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
_audit_creation_date             2016-01-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-03-24 deposited with the CCDC.
2016-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.031(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.0413(13)
_cell_length_b                   15.5968(6)
_cell_length_c                   20.4395(7)
_cell_measurement_reflns_used    15934
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      26.3450
_cell_measurement_theta_min      3.3280
_cell_volume                     10745.6(7)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -20.00   32.50   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.3914  -99.0000  -30.0000 70

  2 omega   -8.00   42.25   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.3914   57.0000  120.0000 67

  3 omega  -17.00    8.50   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.3914  -99.0000  120.0000 34

  4 omega  -66.00  -39.00   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.3914  -57.0000  120.0000 36

  5 omega  -20.00   59.50   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -        8.5633   77.0000 -120.0000 106

  6 omega  -64.00   -4.00   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -        8.5633  -38.0000 -150.0000 80

  7 omega  -19.00   46.25   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -        8.5633  -99.0000 -180.0000 87

  8 omega    3.00   28.50   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -        8.5633  -77.0000  150.0000 34

  9 omega  -16.00   30.50   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -        8.5633  -38.0000   30.0000 62

 10 omega   -1.00   28.25   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -        8.5633  -38.0000    0.0000 39

 11 omega    3.00   30.00   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -        8.5633  -19.0000  -60.0000 36

 12 omega  -64.00   30.50   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -        8.5633  -38.0000  -60.0000 126
;
_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      -0.0203244000
_diffrn_orient_matrix_UB_12      -0.0084418000
_diffrn_orient_matrix_UB_13      -0.0109265000
_diffrn_orient_matrix_UB_21      0.0053343000
_diffrn_orient_matrix_UB_22      -0.0375148000
_diffrn_orient_matrix_UB_23      -0.0163074000
_diffrn_orient_matrix_UB_31      -0.0011464000
_diffrn_orient_matrix_UB_32      -0.0242687000
_diffrn_orient_matrix_UB_33      0.0290270000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0987
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            157681
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.351
_diffrn_reflns_theta_max         25.351
_diffrn_reflns_theta_min         2.747
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.990
_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_density_diffrn    1.276
_exptl_crystal_description       plate
_exptl_crystal_F_000             4368
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1311
_refine_ls_number_reflns         19635
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0608
_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^)+(0.0281P)^2^+14.0751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1158
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15942
_reflns_number_total             19635
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01208f2.cif
_cod_data_source_block           Complex1c
_cod_depositor_comments
'Adding full bibliography for 7039213--7039221.cif.'
_cod_original_cell_volume        10745.7(7)
_cod_database_code               7039219
_chemical_oxdiff_formula         'C27 H30 Fe N2 O2'
_chemical_oxdiff_usercomment     '@ 120 K BRML104'
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.769
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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. Restrained distances
 C128-C127 = C127-C126
 1.56 with sigma of 0.02
 C126-C125 = C125-C124
 1.56 with sigma of 0.02
 C123-C124
 1.56 with sigma of 0.02
3. Restrained angles
 C115-C109-C110, C123-C119-C120
 fixed at 120 with sigma of 0.02
 C118-C119-C123
 fixed at 120 with sigma of 0.02
4. Rigid bond restraints
 C116, C117, C119, C120, C121, C118
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(C128) = Uanis(C127) = Uanis(C126) = Uanis(C125) = Uanis(C124) =
Uanis(C123)
6. Others
 Fixed Sof: C123(0.33333) H12A(0.33333) H12B(0.33333) H12C(0.33333)
 C124(0.33333) H12D(0.33333) H12E(0.33333) C125(0.33333) H12F(0.33333)
 H12G(0.33333) C126(0.33333) H12H(0.33333) H12I(0.33333) C127(0.33333)
 H12J(0.33333) H12K(0.33333) C128(0.33333) H12L(0.33333) H12M(0.33333)
 H12N(0.33333) C116(0.66667) C117(0.66667) H117(0.66667) C118(0.66667)
 H118(0.66667) C119(0.66667) H119(0.66667) C120(0.66667) H120(0.66667)
 C121(0.66667) H121(0.66667) C122(0.66667) H12O(0.66667) H12P(0.66667)
 H12Q(0.66667)
7.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C15(H15A,H15B), C16(H16A,H16B), C60(H60A,H60B),
 C61(H61A,H61B), C69(H69A,H69B), C70(H70A,H70B), C124(H12D,H12E), C125(H12F,
 H12G), C126(H12H,H12I), C127(H12J,H12K)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C12(H12), C21(H21), C22(H22), C23(H23), C26(H26), C27(H27), C28(H28),
 C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C39(H39),
  C40(H40), C41(H41), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48),
 C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C57(H57), C66(H66), C75(H75),
  C76(H76), C77(H77), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84),
 C86(H86), C87(H87), C88(H88), C89(H89), C90(H90), C93(H93), C94(H94), C95(H95),
  C98(H98), C99(H99), C100(H100), C101(H101), C102(H102), C104(H104),
 C105(H105), C106(H106), C107(H107), C108(H108), C110(H110), C111(H111),
 C112(H112), C113(H113), C114(H114), C117(H117), C118(H118), C119(H119),
 C120(H120), C121(H121)
7.c Fitted hexagon refined as free rotating group:
 C116(C117,C118,C119,C120,C121)
7.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C55(H55A,H55B,H55C), C59(H59A,H59B,H59C), C62(H62A,H62B,H62C), C63(H63A,H63B,
 H63C), C64(H64A,H64B,H64C), C68(H68A,H68B,H68C), C71(H71A,H71B,H71C), C72(H72A,
 H72B,H72C), C123(H12A,H12B,H12C), C128(H12L,H12M,H12N), C115(H11A,H11B,H11C),
 C122(H12O,H12P,H12Q)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'