Three-Coordinate Iron(II) Expanded Ring N-Heterocyclic Carbene Complexes
Dunsford, Jay J.; Evans, David J.; Pugh, Thomas; Shah, Sachin N.; Chilton, Nicholas F.; Ingleson, Michael J.; Organometallics 35 (2016) 1098–; doi:10.1021/acs.organomet.6b00121

data_4088474
_publ_section_title
;
 Three-Coordinate Iron(II) Expanded Ring N-Heterocyclic Carbene Complexes
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1098
_journal_paper_doi               10.1021/acs.organomet.6b00121
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C29 H42 Br2 Fe N2'
_chemical_formula_sum            'C29 H42 Br2 Fe N2'
_chemical_formula_weight         634.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-02-10
_audit_creation_method
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Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
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_cell_length_b                   24.9246(3)
_cell_length_c                   12.43441(14)
_cell_measurement_reflns_used    27891
_cell_measurement_temperature    100
_cell_measurement_theta_max      74.4050
_cell_measurement_theta_min      1.7710
_cell_volume                     2909.65(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega   76.21  263.71   1.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0000   73.8672  -40.7898 125

  2 phi    -12.35  311.55   1.4995    5.0000
omega____ theta____ kappa____ phi______ frames
-166.2204   55.0000   73.8672     -     216

  3 omega   81.71  269.21   1.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   73.8672   39.2094 125

  4 phi   -203.50  147.35   1.4994    5.0000
omega____ theta____ kappa____ phi______ frames
 128.6396   75.5000   73.8672     -     234

  5 omega   97.82  264.32   1.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   73.8672 -115.7903 111

  6 omega   62.71  145.21   1.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000   73.8672    9.2088 55

  7 omega  -15.50  145.00   1.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0000   73.8672   94.2102 107

  8 omega  167.21  269.21   1.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   73.8672   -5.7905 68

  9 omega  -40.72   67.28   1.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -65.0000   73.8672  -45.7903 72

 10 omega   75.15  187.65   1.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       75.0000   73.8672 -170.7912 75

 11 omega   93.69  267.69   1.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   73.8672   54.2088 116

 12 phi   -188.59  115.78   1.4994    5.0000
omega____ theta____ kappa____ phi______ frames
 -67.4004  -69.5000   73.8672     -     203

 13 phi      1.65  322.55   1.4995    8.0000
omega____ theta____ kappa____ phi______ frames
 170.4096  110.0000   73.8672     -     214

 14 phi    -25.79  332.56   1.4994    8.0000
omega____ theta____ kappa____ phi______ frames
 128.3596  110.0000   73.8672     -     239

 15 phi    -20.19  332.13   1.4992    5.0000
omega____ theta____ kappa____ phi______ frames
  56.1396   10.0000   73.8672     -     235

 16 phi    -25.79  334.02   1.4992    8.0000
omega____ theta____ kappa____ phi______ frames
-140.7903  111.0000   73.8672     -     240
;
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
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_diffrn_orient_matrix_UB_13      -0.1053887000
_diffrn_orient_matrix_UB_21      0.0282324000
_diffrn_orient_matrix_UB_22      -0.0593837000
_diffrn_orient_matrix_UB_23      -0.0247308000
_diffrn_orient_matrix_UB_31      -0.1497333000
_diffrn_orient_matrix_UB_32      -0.0044711000
_diffrn_orient_matrix_UB_33      -0.0616272000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0108
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            35861
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.595
_diffrn_reflns_theta_min         3.547
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.503
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         5080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0204
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0247P)^2^+2.2840P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0503
_refine_ls_wR_factor_ref         0.0506
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4958
_reflns_number_total             5080
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00121_si_002.cif
_cod_data_source_block           xmji75
_cod_original_cell_volume        2909.64(6)
_cod_database_code               4088474
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 96.17
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.41
_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 Ternary CH refined with riding coordinates:
 C8(H8), C15(H15), C20(H20), C27(H27)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B)
2.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C23(H23), C24(H24), C25(H25)
2.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C)
;
_shelx_res_checksum              16671
_shelx_hkl_checksum              9273
_olex2_submission_special_instructions 'No special instructions were received'