Linear and T-Shaped Iron(I) Complexes Supported by N-Heterocyclic Carbene Ligands: Synthesis and Structure Characterization.
Ouyang, Zhenwu; Du, Jingzhen; Wang, Lei; Kneebone, Jared L.; Neidig, Michael L.; Deng, Liang; Inorganic chemistry 54 (2015) 8808–8816; doi:10.1021/acs.inorgchem.5b01522

data_4344073
_publ_section_title
;
 Linear and T-Shaped Iron(I) Complexes Supported by N-Heterocyclic Carbene
 Ligands: Synthesis and Structure Characterization.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8808
_journal_page_last               8816
_journal_paper_doi               10.1021/acs.inorgchem.5b01522
_journal_volume                  54
_journal_year                    2015
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C46 H60 Fe N4 O, C24 H20 B, C4 H10 O'
_chemical_formula_sum            'C74 H90 B Fe N4 O2'
_chemical_formula_weight         1134.15
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-06-03
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.873(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.0956(15)
_cell_length_b                   18.1551(19)
_cell_length_c                   13.6087(15)
_cell_measurement_reflns_used    2768
_cell_measurement_temperature    130
_cell_measurement_theta_max      20.39
_cell_measurement_theta_min      2.24
_cell_volume                     3233.8(6)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0656
_diffrn_reflns_av_unetI/netI     0.1586
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32992
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.645
_diffrn_reflns_theta_min         1.497
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.281
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0697 before and 0.0588 after correction.
The Ratio of minimum to maximum transmission is 0.9052.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            purple
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_description       block
_exptl_crystal_F_000             1218
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     753
_refine_ls_number_reflns         19485
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1497
_refine_ls_R_factor_gt           0.0727
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0382P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1427
_reflns_Friedel_coverage         0.944
_reflns_friedel_fraction_full    1.000
_reflns_friedel_fraction_max     0.995
_reflns_number_gt                10606
_reflns_number_total             19485
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01522_si_002.cif
_cod_data_source_block           5+Et2O
_cod_depositor_comments
'Adding full bibliography for 4344069--4344073.cif.'
_cod_database_code               4344073
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.946
_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:
 C3(H3A,H3B), C4(H4A,H4B), C23(H23A,H23B), C24(H24A,H24B), C43(H43A,H43B),
 C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C71(H71A,H71B), C73(H73A,H73B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C16(H16), C18(H18), C27(H27), C29(H29), C36(H36), C38(H38),
 C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C54(H54), C55(H55), C56(H56),
  C57(H57), C58(H58), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64),
 C66(H66), C67(H67), C68(H68), C69(H69), C70(H70)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C72(H72A,H72B,H72C), C74(H74A,H74B,H74C)
;
_shelx_res_checksum              4043
_shelx_hkl_checksum              91176
_olex2_submission_special_instructions 'No special instructions were received'