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_4344072
_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_formula_moiety         'C32 H12 B F24, C46 H60 Fe N4'
_chemical_formula_sum            'C78 H72 B F24 Fe N4'
_chemical_formula_weight         1588.05
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-10-31
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                79.488(3)
_cell_angle_beta                 84.243(3)
_cell_angle_gamma                89.168(3)
_cell_formula_units_Z            2
_cell_length_a                   12.520(2)
_cell_length_b                   15.717(3)
_cell_length_c                   19.186(3)
_cell_measurement_reflns_used    4058
_cell_measurement_temperature    130
_cell_measurement_theta_max      22.38
_cell_measurement_theta_min      2.33
_cell_volume                     3693.2(11)
_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)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 0.995
_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  0.0591
_diffrn_reflns_av_unetI/netI     0.1454
_diffrn_reflns_laue_measured_fraction_full 0.995
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            37428
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.085
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.312
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1096 before and 0.0507 after correction.
The Ratio of minimum to maximum transmission is 0.5496.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            Orange
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       block
_exptl_crystal_F_000             1630
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.938
_refine_diff_density_min         -1.109
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     981
_refine_ls_number_reflns         14454
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1543
_refine_ls_R_factor_gt           0.0920
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1920P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2481
_refine_ls_wR_factor_ref         0.2852
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8031
_reflns_number_total             14454
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01522_si_002.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 4344069--4344073.cif.'
_cod_original_cell_volume        3693.1(10)
_cod_database_code               4344072
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.935
_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
 C33-C34
 1.52 with sigma of 0.01
 C13-C14
 1.52 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C33 \\sim C34: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
C6 \\sim C13 \\sim C14: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
C70 \\sim F16 \\sim F17 \\sim F18: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C34) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C14) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F16) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(F13) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C11(H11A,H11B), C13(H13A,H13B), C21(H21A,H21B),
 C23(H23A,H23B), C25(H25A,H25B), C26(H26A,H26B), C33(H33A,H33B), C35(H35A,H35B),
  C43(H43A,H43B), C45(H45A,H45B)
4.b Aromatic/amide H refined with riding coordinates:
 C48(H48), C50(H50), C52(H52), C56(H56), C58(H58), C60(H60), C64(H64),
 C66(H66), C68(H68), C72(H72), C74(H74), C76(H76), C7(H7), C8(H8), C9(H9),
 C17(H17), C18(H18), C19(H19), C29(H29), C30(H30), C31(H31), C39(H39), C40(H40),
  C41(H41)
4.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C44(H44A,H44B,H44C), C46(H46A,
 H46B,H46C)
;
_shelx_res_checksum              5142
_shelx_hkl_checksum              49276
_olex2_submission_special_instructions 'No special instructions were received'