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_4084541
_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         'C46 H44 Fe N4 P2, 2(B F4), 0.5(H2 O)'
_chemical_formula_sum            'C46 H45 B2 F8 Fe N4 O0.5 P2'
_chemical_formula_weight         953.27
_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   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 103.524(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.8424(3)
_cell_length_b                   10.3752(2)
_cell_length_c                   19.0248(4)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    147(2)
_cell_measurement_theta_max      66.41
_cell_measurement_theta_min      2.39
_cell_volume                     2272.71(9)
_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 0.959
_diffrn_measured_fraction_theta_max 0.982
_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  0.0368
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_Laue_measured_fraction_full 0.959
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28140
_diffrn_reflns_point_group_measured_fraction_full 0.914
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.554
_diffrn_reflns_theta_min         3.839
_diffrn_source                   'Bruker ImuS with multi-layer optics''
_exptl_absorpt_coefficient_mu    3.946
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       needle
_exptl_crystal_F_000             982
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
; 
 Flack x determined using 2690 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.034(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         7510
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0485P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0894
_reflns_Friedel_coverage         0.796
_reflns_Friedel_fraction_full    0.862
_reflns_Friedel_fraction_max     0.883
_reflns_number_gt                6820
_reflns_number_total             7510
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5008083_si_002.cif
_cod_data_source_block           6e
_cod_depositor_comments
'Adding full bibliography for 4084538--4084543.cif.'
_cod_original_formula_sum        'C46 H45 B2 F8 Fe N4 O0.50 P2'
_cod_database_code               4084541
_shelx_estimated_absorpt_t_min   0.694
_shelx_estimated_absorpt_t_max   0.925
_shelxl_version_number           2013-3
_shelx_res_checksum              4031
_shelx_hkl_checksum              30978