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_4070963
_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         'C46 H64 Fe N6'
_chemical_formula_sum            'C46 H64 Fe N6'
_chemical_formula_weight         756.90
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   direct
_audit_creation_date             '2004-04-20  09:15:15'
_audit_creation_method
;
 PLATON <TABLE ACC> option 
 SHELXL97-2 & Manual Editing 
;
_audit_update_record
;
 ?
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.6967(8)
_cell_length_b                   18.5086(9)
_cell_length_c                   25.923(1)
_cell_measurement_reflns_used    7696
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      27.31
_cell_measurement_theta_min      2.24
_cell_volume                     8490.8(7)
_computing_cell_refinement       'SAINTPLUS, Version 6.02A, (Bruker, 2000)'
_computing_data_collection       'SMART, Version 5.624, (Bruker, 2001)'
_computing_data_reduction        'XPREP, Version 5.1/NT, (Bruker, 2000)'
_computing_molecular_graphics
;
 PLUTO (Meetsma, 2003) 
 PLATON (Spek, 1994)
;
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
 DIRDIF-99 (Beurskens et al., 1999)
;
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0527
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            71048
_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)
;
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.394
_exptl_absorpt_correction_T_max  0.9361
_exptl_absorpt_correction_T_min  0.9001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Sheldrick, Bruker, 2001))'
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     734
_refine_ls_number_reflns         9731
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+4.7606P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1094
_reflns_number_gt                7759
_reflns_number_total             9731
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om701155b-file004.cif
_cod_data_source_block           global
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_cell_volume        8490.9(7)
_cod_database_code               4070963
_vrn_publ_code_void_volume       149.4
_vrn_publ_code_frame_time_sec    10.0
_vrn_publ_code_meas_time_hour    8.3