Two- and three-coordinate formal iron(i) compounds featuring monodentate aminocarbene ligands
Mo, Zhenbo; Ouyang, Zhenwu; Wang, Lei; Fillman, Kathlyn L.; Neidig, Michael L.; Deng, Liang; Org. Chem. Front. 1 (2014) 1040–; doi:10.1039/C4QO00175C

data_1553021
_publ_section_title
;
 Two- and three-coordinate formal iron(i) compounds featuring monodentate
 aminocarbene ligands
;
_journal_issue                   9
_journal_name_full               'Org. Chem. Front.'
_journal_page_first              1040
_journal_paper_doi               10.1039/C4QO00175C
_journal_volume                  1
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_sum            'C42 H48 Cl Fe N4'
_chemical_formula_weight         700.14
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Hygroscopic, Oxygen-sensitive'
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 100.869(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.723(8)
_cell_length_b                   13.108(9)
_cell_length_c                   13.974(11)
_cell_measurement_reflns_used    3365
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      23.88
_cell_measurement_theta_min      2.48
_cell_volume                     1929(2)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.964
_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_unetI/netI     0.0847
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4576
_diffrn_reflns_point_group_measured_fraction_full 0.522
_diffrn_reflns_point_group_measured_fraction_max 0.503
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.802
_diffrn_reflns_theta_min         1.484
_exptl_absorpt_coefficient_mu    0.493
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.6091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       block
_exptl_crystal_F_000             742
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene and hexane'
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details
; 
No quotients, so Flack parameter determined by classical intensity fit 
;
_refine_ls_abs_structure_Flack   0.13(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         4576
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1044P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1540
_refine_ls_wR_factor_ref         0.1777
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.000
_reflns_Friedel_fraction_max     0.000
_reflns_number_gt                3629
_reflns_number_total             4576
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4qo00175c2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1553021
_shelx_estimated_absorpt_t_min   0.887
_shelx_estimated_absorpt_t_max   0.916
_shelxl_version_number           2013-4
_shelx_res_checksum              70100