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_4327541
_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_structural
;
(Fe C27 H30 N7 O9), (C H Cl2)0.5, (C4 H10 O)0.375
;
_chemical_formula_sum            'C29 H34.25 Cl Fe N7 O9.375'
_chemical_formula_weight         722.20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.600(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.478(3)
_cell_length_b                   12.3531(13)
_cell_length_c                   27.360(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    157(2)
_cell_measurement_theta_max      23.26
_cell_measurement_theta_min      3
_cell_volume                     6918.5(15)
_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      157(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_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  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            24558
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_T_max  0.9284
_exptl_absorpt_correction_T_min  0.8626
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red_black
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       plate
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     849
_refine_ls_number_reflns         9508
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0653
_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^)+(0.0293P)^2^+12.0630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1374
_reflns_number_gt                7334
_reflns_number_total             9711
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0256102B-2_s1_4.cif
_cod_data_source_block           FeTREN-Me-3,2-HOPO
_cod_original_cell_volume        6918.6(15)
_cod_database_code               4327541