Chalcogens as Terminal Ligands to Iron: Synthesis and Structure of Complexes with FeIII-S and FeIII-Se Motifs
Peter L. Larsen; Rajeev Gupta; Douglas R. Powell; Andrew S. Borovik; Journal of the American Chemical Society 126 (2004) 6522–6523; doi:10.1021/ja049118w

data_4112612
_publ_contact_author
; 
   Prof. Andrew S. Borovik 
   Department of Chemistry 
   University of Kansas 
   Rm 2010 Malott Hall
   1251 Wescoe Hall Dr. 
   Lawrence, KS  66045-7582  USA 
;
_publ_contact_author_email       aborovik@ku.edu
_publ_contact_author_fax         1(785)8645396
_publ_contact_author_phone       1(785)8644067
_publ_section_title
;
 Chalcogens as Terminal Ligands to Iron: Synthesis and Structure of
 Complexes with FeIII-S and FeIII-Se Motifs
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6522
_journal_page_last               6523
_journal_paper_doi               10.1021/ja049118w
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         '2(C8 H20 N) 1+, (C21 H42 Fe N7 O3 Se) 2-'
_chemical_formula_sum            'C37 H82 Fe N9 O3 Se'
_chemical_formula_weight         835.93
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 94.027(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.110(2)
_cell_length_b                   19.850(2)
_cell_length_c                   11.8266(16)
_cell_measurement_reflns_used    6649
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.64
_cell_measurement_theta_min      2.21
_cell_volume                     4475.1(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\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  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            27721
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        -0.18
_diffrn_standards_number         182
_exptl_absorpt_coefficient_mu    1.193
_exptl_absorpt_correction_T_max  0.7546
_exptl_absorpt_correction_T_min  0.7086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sheldrick, 2000'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             1804
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.101
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         8793
_refine_ls_number_restraints     1013
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0830
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1400P)^2^+13.6000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2370
_refine_ls_wR_factor_ref         0.2594
_reflns_number_gt                6182
_reflns_number_total             8793
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja049118wsi20040414_055935_2.cif
_cod_data_source_block           compound_FeIIIH3buea(Se)
_cod_database_code               4112612