Triferrocenes Built on a C3-Symmetric Ligand Platform: Entry to Redox-Activepseudo-Triphenylenes via Chelation-Driven Stereoselection of Triple Schiff Bases
Young-Kwan Lim; Scott Wallace; John C. Bollinger; Xufang Chen; Dongwhan Lee; Inorganic Chemistry 46 (2007) 1694–1703; doi:10.1021/ic062029v

data_4307530
_publ_section_title
;
Triferrocenes Built on a C3-Symmetric Ligand Platform: Entry to
Redox-Activepseudo-Triphenylenes via Chelation-Driven Stereoselection of
Triple Schiff Bases
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1694
_journal_page_last               1703
_journal_paper_doi               10.1021/ic062029v
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety
'C39 H30 B3 F6 Fe3 N3 O3, 1.75(C H3 N O2), 0.25 (C H2 Cl2)'
_chemical_formula_sum            'C41 H35.75 B3 Cl0.5 F6 Fe3 N4.75 O6.5'
_chemical_formula_weight         1030.70
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.915(13)
_cell_angle_beta                 99.125(11)
_cell_angle_gamma                106.223(16)
_cell_formula_units_Z            2
_cell_length_a                   10.447(3)
_cell_length_b                   10.885(2)
_cell_length_c                   18.647(4)
_cell_measurement_reflns_used    975
_cell_measurement_temperature    129(2)
_cell_measurement_theta_max      30.12
_cell_measurement_theta_min      2.37
_cell_volume                     1996.0(8)
_computing_cell_refinement       'SAINT 6.45A (Bruker, 2003)'
_computing_data_collection       'SMART 5.630 (Bruker, 2003)'
_computing_data_reduction        'SAINT 6.45A (Bruker, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      129(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
'   0.30 degree frames measured for   5.17 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            45630
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        0.
_diffrn_standards_interval_time  313
_diffrn_standards_number         146
_exptl_absorpt_coefficient_mu    1.196
_exptl_absorpt_correction_T_max  0.9250
_exptl_absorpt_correction_T_min  0.5120
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
'Face-indexed absorption correction via Bruker XPREP 2005/1'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1045
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.907
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         9180
_refine_ls_number_restraints     261
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
   [\s^2^(Fo^2^)+2Fo^2^+(0.04Fo^2^)^2^]^-1^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.0983
_reflns_number_gt                7136
_reflns_number_total             9180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic062029vsi20061203_112702.cif
_cod_data_source_block           05404
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 'Gaussian' changed to
'gaussian' 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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1996.0(7)
_cod_original_formula_sum        'C41 H35.75 B3 Cl0.50 F6 Fe3 N4.75 O6.50'
_cod_database_code               4307530