Synthesis of Iron P-N-P′ and P-NH-P′ Asymmetric Hydrogenation Catalysts
Sonnenberg, Jessica F.; Lough, Alan J.; Morris, Robert H.; Organometallics 33 (2014) 6452–; doi:10.1021/om5008083

data_4084543
_publ_section_title
;
 Synthesis of Iron P-N-P&#x2032; and P-NH-P&#x2032; Asymmetric
 Hydrogenation Catalysts
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6452
_journal_paper_doi               10.1021/om5008083
_journal_volume                  33
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C36 H35 Br2 Fe N P2'
_chemical_formula_sum            'C36 H35 Br2 Fe N P2'
_chemical_formula_weight         759.26
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 94.945(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2404(4)
_cell_length_b                   14.3315(4)
_cell_length_c                   23.1281(8)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    147(2)
_cell_measurement_theta_max      65.81
_cell_measurement_theta_min      3.84
_cell_volume                     3381.7(2)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      147(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker Kpaa 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  0.139
_diffrn_reflns_av_unetI/netI     0.090
_diffrn_reflns_Laue_measured_fraction_full 0.950
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            40740
_diffrn_reflns_point_group_measured_fraction_full 0.769
_diffrn_reflns_point_group_measured_fraction_max 0.787
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.665
_diffrn_reflns_theta_min         1.917
_diffrn_source                   'Bruker ImuS'
_exptl_absorpt_coefficient_mu    7.427
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.5035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       needle
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details
;
 Flack x determined using 2766 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.065(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     762
_refine_ls_number_reflns         20691
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0458
_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^)+0.9503P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1111
_reflns_Friedel_coverage         0.550
_reflns_Friedel_fraction_full    0.571
_reflns_Friedel_fraction_max     0.585
_reflns_number_gt                19353
_reflns_number_total             20691
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5008083_si_002.cif
_cod_data_source_block           FePPh2C6H4CHNCHiPrCH2PPh2Br2
_cod_depositor_comments
'Adding full bibliography for 4084538--4084543.cif.'
_cod_database_code               4084543
_shelx_estimated_absorpt_t_min   0.588
_shelx_estimated_absorpt_t_max   0.808
_shelxl_version_number           2013-2