Iron(II) complexes featuring κ3- and κ2-bound PNP pincer ligands‒the significance of sterics.
Glatz, Mathias; Bichler, Bernhard; Mastalir, Matthias; Stöger, Berthold; Weil, Matthias; Mereiter, Kurt; Pittenauer, Ernst; Allmaier, Günter; Veiros, Luis F.; Kirchner, Karl; Dalton transactions (Cambridge, England : 2003) 44 (2015) 281–294; doi:10.1039/c4dt02866j

data_7032876
_publ_section_title
;
 Iron(II) complexes featuring \k3- and \k2-bound PNP pincer ligands--the
 significance of sterics.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              281
_journal_page_last               294
_journal_paper_doi               10.1039/c4dt02866j
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C18 H34 Fe N6 P4, 2(C F3 O3 S), 2(C3 H6 O)'
_chemical_formula_sum            'C26 H46 F6 Fe N6 O8 P4 S2'
_chemical_formula_weight         928.54
_chemical_name_common
'5d.2(Me2CO)   [Fe(k3-P,N,P-PNP-Me)2](CF3SO3)2.(Me2CO)2'
_chemical_name_systematic
; 
5d.2(Me2CO)  --  [Fe(k^3^-P,N,P-PNP-Me)~2~](CF~3~SO~3~)~2~.(Me~2~CO)~2~ 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 98.886(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6764(17)
_cell_length_b                   18.291(2)
_cell_length_c                   16.390(2)
_cell_measurement_reflns_used    6729
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.986
_cell_measurement_theta_min      2.272
_cell_volume                     4050.8(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\w- and \f-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  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33718
_diffrn_reflns_theta_full        32.00
_diffrn_reflns_theta_max         32.00
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'program SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.198
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         6952
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0695P)^2^+8.9523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1277
_reflns_number_gt                6060
_reflns_number_total             6952
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02866j2.cif
_cod_data_source_block           5d
_cod_depositor_comments
'Adding full bibliography for 7032871--7032878.cif.'
_cod_original_cell_volume        4051.0(9)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7032876