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_4088477
_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         'C27 H38 Br2 Fe N2 O'
_chemical_formula_sum            'C27 H38 Br2 Fe N2 O'
_chemical_formula_weight         622.26
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-03-13
_audit_creation_method
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Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                78.655(4)
_cell_angle_beta                 80.812(4)
_cell_angle_gamma                80.569(4)
_cell_formula_units_Z            2
_cell_length_a                   8.4392(4)
_cell_length_b                   12.4618(5)
_cell_length_c                   13.7286(6)
_cell_measurement_reflns_used    5374
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      28.6620
_cell_measurement_theta_min      3.8830
_cell_volume                     1384.28(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.852
_diffrn_measurement_details
;
  1 omega   38.00   70.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601   57.0000    0.0000 32

  2 omega  -10.00   81.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601   77.0000   60.0000 91

  3 omega  -46.00   40.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -57.0000 -180.0000 86

  4 omega  -19.00   40.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -99.0000  150.0000 59

  5 omega  -51.00   45.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -77.0000  -60.0000 96

  6 omega   36.00   61.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -99.0000 -150.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0367089000
_diffrn_orient_matrix_UB_12      0.0541191000
_diffrn_orient_matrix_UB_13      0.0060595000
_diffrn_orient_matrix_UB_21      -0.0558062000
_diffrn_orient_matrix_UB_22      -0.0015061000
_diffrn_orient_matrix_UB_23      -0.0330901000
_diffrn_orient_matrix_UB_31      -0.0540868000
_diffrn_orient_matrix_UB_32      -0.0224330000
_diffrn_orient_matrix_UB_33      0.0411604000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.852
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11179
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.852
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.029
_diffrn_reflns_theta_min         3.366
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.452
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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    1.493
_exptl_crystal_description       block
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         6298
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0306P)^2^+0.6809P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0730
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5379
_reflns_number_total             6298
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00121_si_002.cif
_cod_data_source_block           amji282
_cod_original_cell_volume        1384.29(11)
_cod_database_code               4088477
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         C46H61N4Fe2Br4
_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:
 C2(H2a,H2b), C3(H3a,H3b), C4(H4a,H4b), C5(H5a,H5b), C24(H24a,H24b), C25(H25a,
 H25b), C26(H26a,H26b), C27(H27a,H27b)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C12(H12), C18(H18), C21(H21)
2.c Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C11(H11a,H11b,H11c), C14(H14a,H14b,H14c), C17(H17a,H17b,
 H17c), C20(H20a,H20b,H20c), C23(H23a,H23b,H23c)
;
_shelx_res_checksum              71121
_shelx_hkl_checksum              70530
_olex2_date_sample_data_collection 2015-03-12
_olex2_submission_special_instructions 'No special instructions were received'