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_4065856
_publ_section_title
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 Kinetically Controlled Formation of Octahedraltrans-Dicarbonyl Iron(II)
 PNP Pincer Complexes: The Decisive Role of Spin-State Changes&#x00A7;
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_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         'C32 H60 Fe N6 P2, 2(B F4), 3(C H3 N O2)'
_chemical_formula_sum            'C35 H69 B2 F8 Fe N9 O6 P2'
_chemical_formula_weight         1003.40
_chemical_name_common            '1259 [Fe(PNP-iPr)(CN-tBu)3](BF4)2.(CH3NO2)3'
_chemical_name_systematic
; 
(N,N'-bis(di-isopropylphosphino)-2,6-diaminopyridine)-
tris(tert-butylnitrile)-iron(II) bis(tetrafluoroborate) 
tris(nitromethane) solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 104.110(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3009(6)
_cell_length_b                   43.262(2)
_cell_length_c                   10.4947(5)
_cell_measurement_reflns_used    8243
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.01
_cell_measurement_theta_min      2.21
_cell_volume                     4976.1(4)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       60
_diffrn_reflns_limit_k_min       -59
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            67536
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.446
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'program SADABS'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         14359
_refine_ls_number_restraints     164
_refine_ls_restrained_S_all      1.196
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0691
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0541P)^2^+8.4601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1580
_refine_ls_wR_factor_ref         0.1606
_reflns_number_gt                13169
_reflns_number_total             14359
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1001638_si_001.cif
_cod_data_source_block           7.(CH3NO2)3-1259
_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        4976.0(4)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4065856