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_4088476
_publ_section_title
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 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 Cl2 Fe N2, C3.5'
_chemical_formula_sum            'C32.5 H42 Cl2 Fe N2'
_chemical_formula_weight         587.43
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.52(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.155(2)
_cell_length_b                   19.056(4)
_cell_length_c                   15.342(3)
_cell_measurement_reflns_used    4209
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.0610
_cell_measurement_theta_min      3.0180
_cell_volume                     3240.2(11)
_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
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0774
_diffrn_reflns_av_unetI/netI     0.1231
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17089
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.029
_exptl_absorpt_coefficient_mu    0.652
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       block
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5688
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.1497
_refine_ls_R_factor_gt           0.0802
_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^)+(0.0288P)^2^+11.4214P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1486
_refine_ls_wR_factor_ref         0.1864
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3356
_reflns_number_total             5688
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00121_si_002.cif
_cod_data_source_block           amji85_refinalise
_cod_original_formula_sum        'C32.50 H42 Cl2 Fe N2'
_cod_database_code               4088476
_shelxl_version_number           2013-2
_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. Others
 Fixed Sof: C4AA(0.5) C3AA(0.5) C5AA(0.5)
3.a Ternary CH refined with riding coordinates:
 C27(H27), C20(H20), C8(H8), C15(H15)
3.b Secondary CH2 refined with riding coordinates:
 C5(H5a,H5b), C3(H3a,H3b), C4(H4a,H4b), C2(H2a,H2b)
3.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C13(H13), C25(H25), C11(H11), C12(H12), C23(H23)
3.d Idealised Me refined as rotating group:
 C28(H28a,H28b,H28c), C22(H22a,H22b,H22c), C29(H29a,H29b,H29c), C17(H17a,H17b,
 H17c), C9(H9a,H9b,H9c), C21(H21a,H21b,H21c), C10(H10a,H10b,H10c), C16(H16a,
 H16b,H16c)
;
_shelx_res_checksum              79716
_shelx_hkl_checksum              15149
_olex2_submission_special_instructions 'No special instructions were received'