Three- and Four-Coordinate Homoleptic Iron(I)‒NHC Complexes: Synthesis and Characterization
Ouyang, Zhenwu; Meng, Yinshan; Cheng, Jun; Xiao, Jie; Gao, Song; Deng, Liang; Organometallics 35 (2016) 1361–; doi:10.1021/acs.organomet.6b00047

data_4088382
_publ_section_title
;
 Three- and Four-Coordinate Homoleptic Iron(I)--NHC Complexes: Synthesis
 and Characterization
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              1361
_journal_paper_doi               10.1021/acs.organomet.6b00047
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C36 H64 Fe N8, C24 H20 B'
_chemical_formula_sum            'C60 H84 B Fe N8'
_chemical_formula_weight         984.01
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-01-19
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                98.120(3)
_cell_angle_beta                 97.916(3)
_cell_angle_gamma                90.190(3)
_cell_formula_units_Z            2
_cell_length_a                   12.036(2)
_cell_length_b                   12.076(2)
_cell_length_c                   19.667(4)
_cell_measurement_reflns_used    5557
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      26.880
_cell_measurement_theta_min      2.44
_cell_volume                     2802.2(9)
_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      140.15
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.983
_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  0.0432
_diffrn_reflns_av_unetI/netI     0.0728
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19382
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.056
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.314
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2008/4 (Bruker,2010) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0706 before and 0.0547 after correction.
 The Ratio of minimum to maximum transmission is 0.84.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 21384 reflections, Rint = 0.0851
 (5522 with I > 3sig(I), Rint = 0.0740)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_description       block
_exptl_crystal_F_000             1062
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.573
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         10807
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0780
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1240P)^2^+3.7871P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2124
_refine_ls_wR_factor_ref         0.2278
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8229
_reflns_number_total             10807
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00047_si_002.cif
_cod_data_source_block           2
_cod_original_cell_volume        2802.1(9)
_cod_database_code               4088382
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.898
_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:
 C9(H9A,H9B), C11(H11A,H11B), C17(H17A,H17B), C19(H19A,H19B), C25(H25A,H25B),
 C27(H27A,H27B), C33(H33A,H33B), C35(H35A,H35B)
2.b Aromatic/amide H refined with riding coordinates:
 C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C45(H45),
 C46(H46), C47(H47), C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54),
  C56(H56), C57(H57), C58(H58), C59(H59), C60(H60)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C20(H20A,H20B,
 H20C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C28(H28A,
 H28B,H28C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C),
 C36(H36A,H36B,H36C)
;
_shelx_res_checksum              37781
_shelx_hkl_checksum              23669
_olex2_submission_special_instructions 'No special instructions were received'