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_4344069
_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 ad
_chemical_formula_moiety         'C54 H68 Br Fe N4'
_chemical_formula_sum            'C54 H68 Br Fe N4'
_chemical_formula_weight         908.88
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-09-24
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.158(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8860(8)
_cell_length_b                   24.2337(19)
_cell_length_c                   18.0401(14)
_cell_measurement_reflns_used    8404
_cell_measurement_temperature    130
_cell_measurement_theta_max      26.13
_cell_measurement_theta_min      2.34
_cell_volume                     4759.1(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  'XH (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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  0.0573
_diffrn_reflns_av_unetI/netI     0.1222
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            48657
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         30.73
_diffrn_reflns_theta_min         1.68
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.196
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0834 before and 0.0520 after correction.
The Ratio of minimum to maximum transmission is 0.7354.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1924
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.241
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.008(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1097
_refine_ls_number_reflns         24299
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.1101
_reflns_number_gt                15435
_reflns_number_total             24299
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01522_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4344069--4344073.cif.'
_cod_database_code               4344069
_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. Restrained distances
 C6-C7 = C7-C8 = C8-C9
 1.52 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C6 \\sim C7 \\sim C8 \\sim C9: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
C29 \\sim C30: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
C79 \\sim C80: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
Uanis(C8) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C30) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C80) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C17(H17A,H17B), C19(H19A,
 H19B), C27(H27A,H27B), C29(H29A,H29B), C32(H32A,H32B), C33(H33A,H33B),
 C34(H34A,H34B), C35(H35A,H35B), C43(H43A,H43B), C45(H45A,H45B), C53(H53A,H53B),
  C55(H55A,H55B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,
 H61B), C69(H69A,H69B), C71(H71A,H71B), C79(H79A,H79B), C81(H81A,H81B),
 C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B), C87(H87A,H87B), C95(H95A,H95B),
  C97(H97A,H97B), C105(H10A,H10B), C107(H10F,H10G)
4.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C23(H23), C24(H24), C25(H25), C39(H39),
 C40(H40), C41(H41), C49(H49), C50(H50), C51(H51), C65(H65), C66(H66), C67(H67),
  C75(H75), C76(H76), C77(H77), C91(H91), C92(H92), C93(H93), C101(H101),
 C102(H102), C103(H103)
4.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C28(H28A,H28B,H28C), C30(H30A,H30B,
 H30C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C54(H54A,H54B,H54C), C56(H56A,
 H56B,H56C), C70(H70A,H70B,H70C), C72(H72A,H72B,H72C), C80(H80A,H80B,H80C),
 C82(H82A,H82B,H82C), C96(H96A,H96B,H96C), C98(H98A,H98B,H98C), C106(H10C,H10D,
 H10E), C108(H10H,H10I,H10J)
;
_olex2_submission_special_instructions 'No special instructions were received'