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_4327538
_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 (C30 H36 N7 O0), C3 H7 N O, C4 H10 O
;
_chemical_formula_sum            'C37 H53 Fe N8 O11'
_chemical_formula_weight         841.74
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                86.8570(10)
_cell_angle_beta                 88.4140(10)
_cell_angle_gamma                70.1240(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4891(2)
_cell_length_b                   12.3583(2)
_cell_length_c                   15.0473(2)
_cell_measurement_reflns_used    5353
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      23.26
_cell_measurement_theta_min      3.00
_cell_volume                     2006.12(6)
_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      163(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_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  0.0209
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8320
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.806
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red_black
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       plate
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.0019(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         5581
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0483P)^2^+2.9755P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1210
_reflns_number_gt                4801
_reflns_number_total             5581
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0256102B-2_s1_1.cif
_cod_data_source_block           FeTRPN-Me-3,2-HOPO
_cod_original_cell_volume        2006.12(5)
_cod_database_code               4327538