From imine to amine: an unexpected left turn. Cis-β iron(ii) PNNP′ precatalysts for the asymmetric transfer hydrogenation of acetophenone
Demmans, Karl Z.; Seo, Chris S. G.; Lough, Alan J.; Morris, Robert H.; Chem. Sci.  (2017) –; doi:10.1039/C7SC02558K

data_1546751
_publ_section_title
;
 From imine to amine: an unexpected left turn. Cis-\b iron(ii)
 PNNP&#x2032; precatalysts for the asymmetric transfer hydrogenation of
 acetophenone
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC02558K
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C39 H42 Br Fe N2 O P2, C24 H20 B, C4 H8 O'
_chemical_formula_sum            'C67 H70 B Br Fe N2 O2 P2'
_chemical_formula_weight         1143.76
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-05-23 deposited with the CCDC.
2017-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9864(4)
_cell_length_b                   12.9194(4)
_cell_length_c                   40.2053(14)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.63
_cell_measurement_theta_min      2.20
_cell_volume                     5706.6(3)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker Kappa APEX-DUO CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1096
_diffrn_reflns_av_unetI/netI     0.0764
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            111385
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.391
_diffrn_reflns_theta_max         67.391
_diffrn_reflns_theta_min         2.198
_diffrn_source                   'Bruker ImuS with multi-layer optics'
_exptl_absorpt_coefficient_mu    3.829
_exptl_absorpt_correction_T_max  0.7344
_exptl_absorpt_correction_T_min  0.5700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       needle
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.017(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     700
_refine_ls_number_reflns         10120
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+3.1449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1211
_reflns_Friedel_coverage         0.789
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                9076
_reflns_number_total             10120
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc02558k2.cif
_cod_data_source_block           6a
_cod_database_code               1546751
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.597
_shelx_estimated_absorpt_t_max   0.963
_shelx_res_checksum              70599