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_4086171
_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            'C48 H64 F12 Fe N4 P2 Sb2 Si2'
_chemical_formula_weight         1342.50
_chemical_melting_point          ?
_chemical_name_common            '[Fe(CNSi Me3)2(NPPN)](SbF6)2'
_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   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                   11.2303(5)
_cell_length_b                   11.2303(5)
_cell_length_c                   44.950(3)
_cell_measurement_reflns_used    9705
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      26.26
_cell_measurement_theta_min      2.27
_cell_volume                     5669.1(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SAINT'
_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      101(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0989
_diffrn_reflns_av_unetI/netI     0.0733
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       68
_diffrn_reflns_limit_l_min       -68
_diffrn_reflns_number            151478
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.953
_diffrn_reflns_theta_min         2.266
_exptl_absorpt_coefficient_mu    1.373
_exptl_absorpt_correction_T_max  0.9359
_exptl_absorpt_correction_T_min  0.7992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0914 before and 0.0781 after correction.
The Ratio of minimum to maximum transmission is 0.8539.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.180
_refine_diff_density_max         2.318
_refine_diff_density_min         -1.060
_refine_diff_density_rms         0.150
_refine_ls_abs_structure_details
;
 Flack x determined using 2631 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.001(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         10280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.1143
_refine_ls_R_factor_gt           0.0744
_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^)+(0.0624P)^2^+23.1338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1609
_refine_ls_wR_factor_ref         0.1738
_reflns_Friedel_coverage         0.714
_reflns_friedel_fraction_full    1.000
_reflns_friedel_fraction_max     0.950
_reflns_number_gt                7692
_reflns_number_total             10280
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00357_si_005.cif
_cod_data_source_block           iso
_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        5669.2(6)
_cod_database_code               4086171
_shelx_estimated_absorpt_t_min   0.717
_shelx_estimated_absorpt_t_max   0.790
_shelxl_version_number           2013-4
_shelx_res_checksum              26407
_shelx_hkl_checksum              36605