Iron piano-stool complexes containing NHC ligands outfitted with pendent arms: synthesis, characterization, and screening for catalytic transfer hydrogenation
Das, Parthapratim; Elder, Thomas J.; Brennessel, William W.; Chmely, Stephen C.; RSC Adv.  (2016) –; doi:10.1039/C6RA20764B

data_7226521
_publ_section_title
;
 Iron piano-stool complexes containing NHC ligands outfitted with pendent
 arms: synthesis, characterization, and screening for catalytic transfer
 hydrogenation
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA20764B
_journal_year                    2016
_chemical_formula_moiety         'C13 H15 Fe N2 O3, C H2 Cl2, I'
_chemical_formula_sum            'C14 H17 Cl2 Fe I N2 O3'
_chemical_formula_weight         514.95
_chemical_name_common            utksc01
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-12-08 deposited with the CCDC.
2016-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   29.269(4)
_cell_length_b                   38.689(5)
_cell_length_c                   6.4704(9)
_cell_measurement_reflns_used    3743
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      37.60
_cell_measurement_theta_min      2.52
_cell_volume                     7327.0(17)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR2011 (Burla et al., 2012)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       67
_diffrn_reflns_limit_k_min       -67
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            68174
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        37.785
_diffrn_reflns_theta_max         38.624
_diffrn_reflns_theta_min         1.745
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.814
_exptl_absorpt_correction_T_max  0.4404
_exptl_absorpt_correction_T_min  0.2751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2012)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_description       needle
_exptl_crystal_F_000             4032
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.279
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.140
_refine_ls_abs_structure_details
; 
 Flack x determined using 3830 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   -0.006(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         9897
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0473P)^2^+4.4020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0817
_reflns_Friedel_coverage         0.840
_reflns_Friedel_fraction_full    0.967
_reflns_Friedel_fraction_max     0.930
_reflns_number_gt                9001
_reflns_number_total             9897
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra20764b2.cif
_cod_data_source_block           utksc01
_cod_database_code               7226521
_shelx_estimated_absorpt_t_min   0.334
_shelx_estimated_absorpt_t_max   0.631
_shelxl_version_number           2013-4
_shelx_res_checksum              26522