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_1546750
_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         'C47 H40 Br Fe N2 O P2, C24 H20 B'
_chemical_formula_sum            'C71 H60 B Br Fe N2 O P2'
_chemical_formula_weight         1165.72
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_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                110.941(5)
_cell_angle_beta                 97.709(6)
_cell_angle_gamma                101.330(5)
_cell_formula_units_Z            2
_cell_length_a                   11.301(2)
_cell_length_b                   14.448(3)
_cell_length_c                   19.278(4)
_cell_measurement_reflns_used    8113
_cell_measurement_temperature    151(2)
_cell_measurement_theta_max      22.63
_cell_measurement_theta_min      2.31
_cell_volume                     2809.8(10)
_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      151(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Kappa APEX-DUO CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1305
_diffrn_reflns_av_unetI/netI     0.1647
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            92778
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.617
_diffrn_reflns_theta_min         1.536
_diffrn_source
'sealed tube with Bruker Triumph monochromator'
_exptl_absorpt_coefficient_mu    1.085
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       Block
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
; 
 Flack x determined using 5061 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.000(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.939
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1423
_refine_ls_number_reflns         25756
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.1340
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0071P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0715
_refine_ls_wR_factor_ref         0.0881
_reflns_Friedel_coverage         0.986
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                14715
_reflns_number_total             25756
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc02558k2.cif
_cod_data_source_block           5d
_cod_original_cell_volume        2809.8(9)
_cod_database_code               1546750
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.881
_shelx_estimated_absorpt_t_max   0.899
_shelx_res_checksum              70414