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_4088479
_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         'C54 H76 Br4 Fe2 N4, 4(C6 H6)'
_chemical_formula_sum            'C78 H100 Br4 Fe2 N4'
_chemical_formula_weight         1524.95
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-01-07
_audit_creation_method
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Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
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_cell_angle_alpha                70.448(7)
_cell_angle_beta                 88.517(5)
_cell_angle_gamma                67.228(5)
_cell_formula_units_Z            1
_cell_length_a                   10.6547(5)
_cell_length_b                   12.2902(8)
_cell_length_c                   16.2704(13)
_cell_measurement_reflns_used    3853
_cell_measurement_temperature    150.02(14)
_cell_measurement_theta_max      26.9200
_cell_measurement_theta_min      3.5580
_cell_volume                     1838.0(2)
_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
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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_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.02(14)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   15.00   43.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4767   77.0000    0.0000 28

  2 omega  -11.00   94.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.4923   77.0000   90.0000 105

  3 omega   11.00   39.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4767   77.0000  120.0000 28

  4 omega  -11.00   94.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.4923   77.0000  -30.0000 105

  5 omega    7.00   40.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4767   77.0000 -120.0000 33

  6 omega  -12.00   86.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.4923   77.0000 -150.0000 98

  7 omega  -46.00  -18.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4767   77.0000  120.0000 28
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0076449000
_diffrn_orient_matrix_UB_12      0.0029080000
_diffrn_orient_matrix_UB_13      -0.0439584000
_diffrn_orient_matrix_UB_21      -0.0059258000
_diffrn_orient_matrix_UB_22      0.0632263000
_diffrn_orient_matrix_UB_23      -0.0154470000
_diffrn_orient_matrix_UB_31      0.0720725000
_diffrn_orient_matrix_UB_32      -0.0215973000
_diffrn_orient_matrix_UB_33      -0.0003247000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0697
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13192
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.358
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.612
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43253
_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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       block
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.081
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         7489
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0547P)^2^+1.6403P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1192
_refine_ls_wR_factor_ref         0.1335
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5586
_reflns_number_total             7489
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00121_si_002.cif
_cod_data_source_block           amji327
_cod_database_code               4088479
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         C54H76N4Fe2Br4
_reflns_odcompleteness_completeness 99.77
_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 Ternary CH refined with riding coordinates:
 C18(H18), C25(H25), C6(H6), C13(H13)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
2.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C10(H10), C22(H22), C11(H11), C21(H21), C9(H9), C33(H33), C28(H28),
 C29(H29), C30(H30), C31(H31), C32(H32), C38(H38), C37(H37), C39(H39), C35(H35),
  C34(H34), C36(H36)
2.d Fitted hexagon refined as free rotating group:
 C33(C28,C29,C30,C31,C32)
2.e Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C8(H8A,H8B,H8C), C15(H15A,H15B,H15C), C20(H20A,H20B,
 H20C), C19(H19A,H19B,H19C), C7(H7A,H7B,H7C), C26(H26A,H26B,H26C), C14(H14A,
 H14B,H14C)
;
_shelx_res_checksum              16262
_shelx_hkl_checksum              15632
_olex2_submission_special_instructions 'No special instructions were received'