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_4344070
_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         'C46 H60 Br Fe N4'
_chemical_formula_sum            'C46 H60 Br Fe N4'
_chemical_formula_weight         804.74
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-11-03
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.585(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4572(7)
_cell_length_b                   23.2863(15)
_cell_length_c                   17.1202(12)
_cell_measurement_reflns_used    4559
_cell_measurement_temperature    130
_cell_measurement_theta_max      24.53
_cell_measurement_theta_min      2.33
_cell_volume                     4132.5(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.0783
_diffrn_reflns_av_unetI/netI     0.0928
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41572
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.596
_diffrn_reflns_theta_min         1.485
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.368
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1164 before and 0.0497 after correction. The Ratio of minimum to maximum transmission is 0.7480. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       block
_exptl_crystal_F_000             1700
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.038
_refine_diff_density_min         -1.282
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         12643
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1107
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+1.5233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1335
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7756
_reflns_number_total             12643
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01522_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 4344069--4344073.cif.'
_cod_database_code               4344070
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.646
_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. Rigid bond restraints
 C23, C24
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
C23 \\sim C24: within 1.7A with sigma of 0.001 and sigma for terminal atoms of
0.002
C21 \\sim C22: within 1.7A with sigma of 0.005 and sigma for terminal atoms of
0.01
Uanis(C22) \\sim Ueq, Uanis(C24) \\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:
 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              69089
_shelx_hkl_checksum              19821
_olex2_submission_special_instructions 'No special instructions were received'