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_4084539
_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         'C53 H48 Br Fe N2 O P2, B F4, C4 H10 O'
_chemical_formula_sum            'C57 H58 B Br F4 Fe N2 O2 P2'
_chemical_formula_weight         1087.56
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.4589(7)
_cell_length_b                   17.3014(6)
_cell_length_c                   14.5749(6)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    147(2)
_cell_measurement_theta_max      27.33
_cell_measurement_theta_min      2.35
_cell_volume                     5159.0(3)
_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 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            45277
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.514
_diffrn_reflns_theta_min         1.541
_diffrn_source
'sealed tube with Bruker Triumph monochromator'
_exptl_absorpt_coefficient_mu    1.188
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            bronze
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       needle
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
; 
 Flack x determined using 2337 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.021(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         5943
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+9.6286P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1034
_reflns_Friedel_coverage         0.817
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                5526
_reflns_number_total             5943
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5008083_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4084538--4084543.cif.'
_cod_database_code               4084539
_shelx_estimated_absorpt_t_min   0.748
_shelx_estimated_absorpt_t_max   0.880
_shelxl_version_number           2013-4
_shelx_res_checksum              80255
_shelx_hkl_checksum              76416