Hexadentate Hydroxypyridonate Iron Chelators Based on TREN-Me-3,2-HOPO: Variation of Cap Size1
Jide Xu; Brendon O'Sulliva; Kenneth N. Raymond; Inorganic Chemistry 41 (2002) 6731–6742; doi:10.1021/ic025610+

data_4327539
_publ_contact_author
;
Kenneth N. Raymond
Department of Chemistry
University of California
Berkeley, CA  94720-1460
;
_publ_contact_author_email       raymond@socrates.berkeley.edu
_publ_contact_author_fax         510-486-5283
_publ_contact_author_phone       510-642-7219
_publ_section_title
;
 Hexadentate Hydroxypyridonate Iron Chelators Based on TREN-Me-3,2-HOPO:
 Variation of Cap Size1
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6731
_journal_page_last               6742
_journal_paper_doi               10.1021/ic025610+
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety
;
Fe (C29 H34 N7 O0), (C H4 O)3.5 
;
_chemical_formula_sum            'C32.5 H51 Fe N7 O12.5'
_chemical_formula_weight         749.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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                 101.15
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.5294(3)
_cell_length_b                   19.7831(4)
_cell_length_c                   27.2439(4)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      23.25
_cell_measurement_theta_min      3.00
_cell_volume                     7154.3(2)
_computing_cell_refinement
; 
SMART (Siemens, 1995) SAINT (Siemens, 1995) 
;
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction
; 
SAINT (Siemens, 1995) XPREP (Siemens, 1995) 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device       '3 circle diffractometer'
_diffrn_measurement_method       'omega scans with profile analysis'
_diffrn_radiation_detector       'CCD area detector'
_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  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            13870
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_T_max  0.840
_exptl_absorpt_correction_T_min  0.735
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red_black
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_description       cube
_exptl_crystal_F_000             3368
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         4866
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0735
_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^)+(0.0534P)^2^+29.0302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1616
_refine_ls_wR_factor_ref         0.1688
_reflns_number_gt                4231
_reflns_number_total             4866
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0256102B-2_s1_2.cif
_cod_data_source_block           FeTR332-Me-3,2-HOPO
_cod_original_formula_sum        'C32.50 H51 Fe N7 O12.50'
_cod_database_code               4327539