Chiral Iron(II) NPPN Complexes: Synthesis and Application in the Asymmetric Strecker Reaction of Azomethine Imines
Huber, Raffael; Bigler, Raphael; Mezzetti, Antonio; Organometallics 34 (2015) 3374–; doi:10.1021/acs.organomet.5b00357

data_4086170
_publ_section_title
;
 Chiral Iron(II) NPPN Complexes: Synthesis and Application in the
 Asymmetric Strecker Reaction of Azomethine Imines
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3374
_journal_paper_doi               10.1021/acs.organomet.5b00357
_journal_volume                  34
_journal_year                    2015
_chemical_absolute_configuration rmad
_chemical_formula_sum            'C50 H65.39 B2 F8 Fe N4 O0.7 P2'
_chemical_formula_weight         1025.02
_chemical_melting_point          ?
_chemical_name_common            '[Fe(CNtBu)2(NPPN)](BF4)2 &#x00FA; 0.70 H2O'
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_hydrogens   mixed
_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                   10.9540(4)
_cell_length_b                   10.9540(4)
_cell_length_c                   41.6585(19)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.74
_cell_measurement_theta_min      2.37
_cell_volume                     4998.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXL-2013 (Sheldrick, 2013)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            48759
_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         29.397
_diffrn_reflns_theta_min         1.922
_exptl_absorpt_coefficient_mu    0.436
_exptl_absorpt_correction_T_max  0.9977
_exptl_absorpt_correction_T_min  0.8689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0788 before and 0.0586 after correction.
The Ratio of minimum to maximum transmission is 0.8709.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2148
_exptl_crystal_size_max          0.438
_exptl_crystal_size_mid          0.342
_exptl_crystal_size_min          0.137
_refine_diff_density_max         0.771
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Flack x determined using 2388 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.002(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6887
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0371P)^2^+3.4931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0948
_reflns_Friedel_coverage         0.702
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6192
_reflns_number_total             6887
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00357_si_004.cif
_cod_data_source_block           new5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 
;
_cod_original_cell_volume        4998.6(4)
_cod_original_formula_sum        'C50 H65.39 B2 F8 Fe N4 O0.70 P2'
_cod_database_code               4086170
_shelx_estimated_absorpt_t_min   0.832
_shelx_estimated_absorpt_t_max   0.943
_shelxl_version_number           2013-4
_shelx_res_checksum              56114
_shelx_hkl_checksum              41752