Synthesis, Structure, and Physical Properties for a Series of Monomeric Iron(III) Hydroxo Complexes with Varying Hydrogen-Bond Networks
Jhumpa Mukherjee; Robie L. Lucas; Matthew K. Zart; Douglas R. Powell; Victor W. Day; A. S. Borovik; Inorganic Chemistry 47 (2008) 5780–5786; doi:10.1021/ic800048e

data_4305235
_publ_contact_author
; 
   Prof. Andrew S. Borovik 
   Department of Chemistry -- University of California, Irvine
   1102 Natural Sciences II 
   Irvine, CA 92697-2025  USA 
;
_publ_contact_author_email       aborovik@uci.edu
_publ_contact_author_fax         1(949)8248571
_publ_contact_author_phone       1(949)8241510
_publ_section_title
;
Synthesis, Structure, and Physical Properties for a Series of Monomeric
Iron(III) Hydroxo Complexes with Varying Hydrogen-Bond Networks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5780
_journal_page_last               5786
_journal_paper_doi               10.1021/ic800048e
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'K 1+, (C17 H33 Fe N5 O4) 1-, (C4 H9 N O)1.5'
_chemical_formula_sum            'C23 H46.5 Fe K N6.5 O5.5'
_chemical_formula_weight         597.12
_chemical_name_common            K[FeIIIH1iPr(OH)].1.5Et2O
_chemical_name_systematic
; 
 Potassium {[(N'-tert-butylureayl)-N-ethyl]-bis
 (N''-isopropylcarbamoylmethyl)-aminato(hydroxo)ferrate(III)} 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 107.612(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.175(3)
_cell_length_b                   9.8523(12)
_cell_length_c                   26.326(3)
_cell_measurement_reflns_used    6342
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.29
_cell_volume                     6223.6(13)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            19294
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        0.18
_diffrn_standards_number         465
_exptl_absorpt_coefficient_mu    0.661
_exptl_absorpt_correction_T_max  0.9309
_exptl_absorpt_correction_T_min  0.8017
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sheldrick, 2000'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2552
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         6080
_refine_ls_number_restraints     230
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0300
_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^)+(0.0480P)^2^+5.8000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0831
_reflns_number_gt                5609
_reflns_number_total             6080
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800048e-file006_2.cif
_cod_data_source_block           asb
_cod_original_formula_sum        'C23 H46.50 Fe K N6.50 O5.50'
_cod_database_code               4305235