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_4089107
_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_sum            'C38 H43 Br2 Fe2 N P2'
_chemical_formula_weight         847.19
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                100.365(2)
_cell_angle_beta                 95.972(2)
_cell_angle_gamma                107.632(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5717(6)
_cell_length_b                   13.1857(8)
_cell_length_c                   15.5566(9)
_cell_measurement_reflns_used    9796
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.6
_cell_measurement_theta_min      2.3
_cell_volume                     1814.11(19)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker KAPPA APEX II CCD'
_diffrn_measurement_method       '\w- and \f-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            66074
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.112
_diffrn_reflns_theta_min         2.265
_exptl_absorpt_coefficient_mu    3.118
_exptl_absorpt_correction_T_max  0.65
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_description       plate
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Flack x determined using 7936 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.006(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         21121
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.893
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0280
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0494
_refine_ls_wR_factor_ref         0.0519
_reflns_Friedel_coverage         0.986
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                18382
_reflns_number_total             21121
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00711_si_002.cif
_cod_data_source_block           I
_cod_database_code               4089107
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.417
_shelx_estimated_absorpt_t_max   0.811
_shelx_res_checksum              45945
_shelx_hkl_checksum              9939