Iron(II) Complexes Containing Chiral Unsymmetrical PNP′ Pincer Ligands: Synthesis and Application in Asymmetric Hydrogenations
Zirakzadeh, Afrooz; Kirchner, Karl; Roller, Alexander; Stöger, Berthold; Widhalm, Michael; Morris, Robert H.; Organometallics 35 (2016) 3781–; doi:10.1021/acs.organomet.6b00711

data_4089108
_publ_section_title
;
 Iron(II) Complexes Containing Chiral Unsymmetrical PNP&#x2032; Pincer
 Ligands: Synthesis and Application in Asymmetric Hydrogenations
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              3781
_journal_paper_doi               10.1021/acs.organomet.6b00711
_journal_volume                  35
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C44 H51 Br2 Fe2 N P2, 3(C4 H8 O)'
_chemical_formula_sum            'C56 H75 Br2 Fe2 N O3 P2'
_chemical_formula_weight         1143.63
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-16
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5793(3)
_cell_length_b                   19.0106(5)
_cell_length_c                   29.2941(9)
_cell_measurement_reflns_used    9506
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      78.814
_cell_measurement_theta_min      2.771
_cell_volume                     5334.7(3)
_computing_cell_refinement       'APEX2 v2013.6-2'
_computing_data_collection       'APEX2 v2013.6-2'
_computing_data_reduction        'APEX2 v2013.6-2'
_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      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            72550
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.343
_diffrn_reflns_theta_min         2.771
_diffrn_source                   'INCOATEC microfocus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.013
_exptl_absorpt_correction_T_max  0.7542
_exptl_absorpt_correction_T_min  0.5444
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0750 before and 0.0597 after correction.
The Ratio of minimum to maximum transmission is 0.7218.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       needle
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.029
_exptl_crystal_size_min          0.027
_refine_diff_density_max         1.272
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Flack x determined using 4589 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.0093(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         11463
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+10.9804P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1088
_reflns_Friedel_coverage         0.798
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                10939
_reflns_number_total             11463
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00711_si_002.cif
_cod_data_source_block           cu_afzi1031a_p212121
_cod_database_code               4089108
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.833
_shelx_estimated_absorpt_t_min   0.329
_shelx_res_checksum              8363
_shelx_hkl_checksum              29175