Kinetically Controlled Formation of Octahedraltrans-Dicarbonyl Iron(II) PNP Pincer Complexes: The Decisive Role of Spin-State Changes§
Benito-Garagorri, David; Alves, Luis Gonçalo; Veiros, Luis F.; Standfest-Hauser, Christina M.; Tanaka, Shinji; Mereiter, Kurt; Kirchner, Karl; Organometallics 29 (2010) 4932–; doi:10.1021/om1001638

data_4065853
_publ_section_title
;
 Kinetically Controlled Formation of Octahedraltrans-Dicarbonyl Iron(II)
 PNP Pincer Complexes: The Decisive Role of Spin-State Changes&#x00A7;
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              4932
_journal_paper_doi               10.1021/om1001638
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C19 H33 Cl Fe N3 O2 P2, B F4'
_chemical_formula_sum            'C19 H33 B Cl F4 Fe N3 O2 P2'
_chemical_formula_weight         575.53
_chemical_name_common            '1195 trans-[Fe(PNP-iPr)(CO)2Cl]BF4'
_chemical_name_systematic
; 
(N,N'-bis(di-isopropylphosphino)-2,6-diaminopyridine)-
-trans-bis(carbonyl)-chloro-iron(II) tetrafluoroborate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.434(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0019(15)
_cell_length_b                   29.868(6)
_cell_length_c                   11.398(2)
_cell_measurement_reflns_used    6624
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      23.54
_cell_measurement_theta_min      2.32
_cell_volume                     2599.0(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT, SADABS, XPREP'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart APEX CCD 3-axis'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0507
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            36817
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.32
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.856
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'program SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
Flack H D (1983), Acta Cryst. A39, 876-881.

The structure has space group P2(1), but is pseudocentric with a 
pseudcentre at x,y,z = 0.731, 0.250, 0.305. A refinement using
TWIN and BASF of program SHELXL97 was carried out indicating
that the crystal behaves like a racemic twin with twin
components roughly in 1:1 proprotion. 
;
_refine_ls_abs_structure_Flack   0.515(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         11305
_refine_ls_number_restraints     276
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0717P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1238
_reflns_number_gt                9004
_reflns_number_total             11305
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1001638_si_001.cif
_cod_data_source_block           5a-1195
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2599.1(8)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4065853