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_4088480
_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         'C31 H46 Br2 Fe N2 O'
_chemical_formula_sum            'C31 H46 Br2 Fe N2 O'
_chemical_formula_weight         678.37
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-05-03
_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_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.5289(4)
_cell_length_b                   18.4203(6)
_cell_length_c                   22.0688(6)
_cell_measurement_reflns_used    5540
_cell_measurement_temperature    150.02(10)
_cell_measurement_theta_max      27.8910
_cell_measurement_theta_min      3.8820
_cell_volume                     6312.7(3)
_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      150.02(10)
_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  -51.00   59.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -19.0000  -60.0000 110

  2 omega   19.00   57.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -99.0000   90.0000 38
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0134211000
_diffrn_orient_matrix_UB_12      -0.0271352000
_diffrn_orient_matrix_UB_13      -0.0207175000
_diffrn_orient_matrix_UB_21      0.0002307000
_diffrn_orient_matrix_UB_22      -0.0260538000
_diffrn_orient_matrix_UB_23      0.0237091000
_diffrn_orient_matrix_UB_31      -0.0436527000
_diffrn_orient_matrix_UB_32      0.0082275000
_diffrn_orient_matrix_UB_33      0.0064740000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15419
_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         25.024
_diffrn_reflns_theta_min         3.394
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.035
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
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    1.428
_exptl_crystal_description       block
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         5552
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0307
_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^)+(0.0219P)^2^+5.5250P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0677
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4572
_reflns_number_total             5552
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00121_si_002.cif
_cod_data_source_block           amji293
_cod_database_code               4088480
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         C54H42N4Fe2Br4
_reflns_odcompleteness_completeness 99.63
_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), C13(H13), C6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C29(H29A,H29B), C28(H28A,H28B), C31(H31A,H31B),
 C30(H30A,H30B)
2.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C23(H23), C9(H9), C10(H10), C22(H22), C11(H11)
2.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C7(H7A,H7B,
 H7C), C15(H15A,H15B,H15C), C14(H14A,H14B,H14C), C8(H8A,H8B,H8C), C27(H27A,H27B,
 H27C)
;
_shelx_res_checksum              88118
_shelx_hkl_checksum              83715
_olex2_submission_special_instructions 'No special instructions were received'