Neutral and Cationic Paramagnetic Amino-amidinate Iron(II) Complexes:19F NMR Evidence for Interactions with Weakly Coordinating Anions
Sciarone, Timo J. J.; Nijhuis, Christian A.; Meetsma, Auke; Hessen, Bart; Organometallics 27 (2008) 2058–; doi:10.1021/om701155b

data_4070964
_publ_section_title
;
 Neutral and Cationic Paramagnetic Amino-amidinate Iron(II) Complexes:19F
 NMR Evidence for Interactions with Weakly Coordinating Anions
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2058
_journal_paper_doi               10.1021/om701155b
_journal_volume                  27
_journal_year                    2008
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C26 H32 Cl Fe N3 O3, 2(C4H8O)'
_chemical_formula_sum            'C34 H48 Cl Fe N3 O5'
_chemical_formula_weight         670.07
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   direct
_cell_angle_alpha                90
_cell_angle_beta                 96.305(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4467(8)
_cell_length_b                   20.014(2)
_cell_length_c                   18.161(2)
_cell_measurement_reflns_used    5621
_cell_measurement_temperature    105
_cell_measurement_theta_max      23.74
_cell_measurement_theta_min      2.33
_cell_volume                     3412.9(6)
_computing_cell_refinement       'SAINT, Bruker Version 6.02A, 2000'
_computing_data_collection       'SMART, Bruker Version 5.168, 2000'
_computing_data_reduction        'XPREP, Bruker Version 5.1/NT, 2000'
_computing_molecular_graphics
;
 PLUTO  (Meetsma, 2001) 
 PLATON (Spek, 1994)
;
_computing_publication_material
;
 PLATON (Spek, 1990)
 SHELXL (Sheldrick, 1997)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
 DIRDIF-99 (Beurskens et al., 1999)
;
_diffrn_ambient_temperature      105(2)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type
;
  Bruker Smart Apex 
;
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_detector
;
 CCD area-detector
;
_diffrn_radiation_monochromator  'parallel mounted graphite'
_diffrn_radiation_source         'fine focus sealed Siemens Mo tube '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_sigmaI/netI    0.0846
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31758
_diffrn_reflns_reduction_process
;
 Intensity data were corrected for Lorentz and polarization
  effects, decay and absorption and reduced to F~o~^2^
  using SAINT (Bruker, 2000) and SADABS (Sheldrick, 2001)

 Intensity data were corrected for Lorentz and polarization effects,
  scale variation, for absorption and reduced to F~o~^2^
;
_diffrn_reflns_theta_full        29.73
_diffrn_reflns_theta_max         29.73
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_T_max  0.9733
_exptl_absorpt_correction_T_min  0.8990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, Bruker, 2000)'
_exptl_crystal_colour            '  bright-yellow'
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       '  platelet'
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         9004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0628
_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^)+(0.0945P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1601
_refine_ls_wR_factor_ref         0.1737
_reflns_number_gt                5499
_reflns_number_total             9004
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om701155b-file005.cif
_cod_data_source_block           c26h32cl
_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.

'_exptl_absorpt_correction_type' value 'Multi-Scan'
changed to 'multi-scan' 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_sg_symbol_H-M      'P 21/n'
_cod_database_code               4070964