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_7032874
_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         'C58 H50 Fe N6 P4, 2(Cl)'
_chemical_formula_sum            'C58 H50 Cl2 Fe N6 P4'
_chemical_formula_weight         1081.67
_chemical_name_common
'5b.solv  [Fe(k3-P,N,P-PNP-Ph)2](Cl)2.solv   1610'
_chemical_name_systematic
; 
5b.solv  --  [Fe(k^3^-P,N,P-PNP-Ph)~2~](Cl)~2~.solv
;
_space_group_IT_number           122
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1224(2)
_cell_length_b                   15.1224(2)
_cell_length_c                   30.8856(6)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.43
_cell_measurement_theta_min      2.32
_cell_volume                     7063.13(19)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31615
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    0.414
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'program SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.017
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.35
_platon_squeeze_details
;
The title structure was obtained from methanol / diethyl ether. It is
a solvate with disordered solvent molecules. This solvent was SQUEEZED
with program PLATON. 
According to PLATON, the solvent accessible volume is 2562 A^3^ per unit
cell (36% of the unit cell volume) with an electron count of 305. It is 
estimated that there are at least 16 methanol molecules per unit cell
or 4 molecules per Fe complex, which may be O-H...Cl hydrogen bonded to the
the cloride anions. The solvent cavity forms a 3-dimensional infinte
structure between the Fe(PNP-Ph)2 complexes and the Cl anions. 
The highest solvent denity peaks identified by procedure SQUEEZE were:
C101 0.261 0.923 0.182 !       3.62 eA-3
C102 0.301 0.904 0.211 !       2.73 eA-3
C103 0.796 0.145 0.421 !       2.17 eA-3
C104 0.264 0.056 0.387 !       2.02 eA-3
C105 1.000 1.002 0.414 !       0.99 eA-3
C106 0.547 0.803 0.193 !       0.99 eA-3
C107 1.000 0.995 0.437 !       0.79 eA-3
;
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 2345 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.020(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         5139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0259
_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^)+(0.0450P)^2^+2.1416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0707
_reflns_number_gt                4943
_reflns_number_total             5139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02866j2.cif
_cod_data_source_block           5b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 7032871--7032878.cif.
;
_cod_original_sg_symbol_Hall     'I -4 2bw '
_cod_database_code               7032874