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_4088384
_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_sum            'C57 H80 B Cl Fe N6'
_chemical_formula_weight         951.38
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90.3820(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4567(8)
_cell_length_b                   18.2217(11)
_cell_length_c                   21.8734(12)
_cell_measurement_reflns_used    8512
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      27.14
_cell_measurement_theta_min      2.24
_cell_volume                     5363.3(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            54136
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.677
_diffrn_reflns_theta_min         1.862
_exptl_absorpt_coefficient_mu    0.373
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         16487
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+0.4307P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1244
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10813
_reflns_number_total             16487
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00047_si_002.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4088384
_shelx_estimated_absorpt_t_min   0.881
_shelx_estimated_absorpt_t_max   0.913
_shelxl_version_number           2014-3
_shelx_res_checksum              8360
_shelx_hkl_checksum              39666