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_4084540
_publ_section_title
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 Synthesis of Iron P-N-P&#x2032; and P-NH-P&#x2032; Asymmetric
 Hydrogenation Catalysts
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_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6452
_journal_paper_doi               10.1021/om5008083
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C39 H38 Fe N4 P2, 2(B F4)'
_chemical_formula_sum            'C39 H38 B2 F8 Fe N4 P2'
_chemical_formula_weight         854.14
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                110.891(3)
_cell_angle_beta                 92.273(4)
_cell_angle_gamma                90.535(3)
_cell_formula_units_Z            4
_cell_length_a                   10.6495(17)
_cell_length_b                   18.491(3)
_cell_length_c                   21.832(3)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    147(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.57
_cell_volume                     4012.1(11)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      147(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Kappa APEX-DUO CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Bruker Triumph'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_sigmaI/netI    0.0639
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            57026
_diffrn_reflns_theta_full        27.65
_diffrn_reflns_theta_max         27.65
_diffrn_reflns_theta_min         1.00
_exptl_absorpt_coefficient_mu    0.527
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7188
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.822
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1049
_refine_ls_number_reflns         18498
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+2.0820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1115
_reflns_number_gt                12864
_reflns_number_total             18498
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om5008083_si_002.cif
_cod_data_source_block           6a
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 4084538--4084543.cif.
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_cod_original_cell_volume        4012.2(10)
_cod_database_code               4084540