Novel Iron Porphyrin-Alkanethiolate Complex with Intramolecular NH...S Hydrogen Bond: Synthesis, Spectroscopy, and Reactivity
Noriyuki Suzuki; Tsunehiko Higuchi; Yasuteru Urano; Kazuya Kikuchi; Hidehiro Uekusa; Yuji Ohashi; Takeshi Uchida; Teizo Kitagawa; Tetsuo Nagano; Journal of the American Chemical Society 121 (1999) 11571–11572; doi:10.1021/ja992511v

data_4116639
_publ_contact_author_address
; Faculty of Pharmaceutical Sciences
University of Tokyo
7-3-1 Hongo, Bunkyo-ku
Tokyo 113-0033, JAPAN
;
_publ_contact_author_email       higuchi@mol.f.u-tokyo.ac.jp
_publ_contact_author_fax         81(35684)2395
_publ_contact_author_name        'Professor Tsunehiko Higuchi'
_publ_contact_author_phone       '81(33812)2111 ext. 4852'
_publ_section_title
;
 Novel Iron Porphyrin-Alkanethiolate Complex with Intramolecular NH...S
 Hydrogen Bond: Synthesis, Spectroscopy, and Reactivity
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11571
_journal_page_last               11572
_journal_paper_doi               10.1021/ja992511v
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C70 H66 Fe N9 O6 S'
_chemical_formula_weight         1217.23
_chemical_name_common            o-NHAcSR
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 101.6502(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.387(2)
_cell_length_b                   17.4364(10)
_cell_length_c                   13.8016(12)
_cell_measurement_reflns_used    22631
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      3.06
_cell_volume                     6219.2(8)
_computing_cell_refinement       'RAPID AUTO (T.Higashi, 1998)'
_computing_data_collection       'RAPID AUTO (T.Higashi, 1998)'
_computing_data_reduction        'RAPID AUTO (T.Higashi, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 100
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'RIGAKU R-RAXIS RAPID'
_diffrn_measurement_method       'oscillation photograph'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1305
_diffrn_reflns_av_sigmaI/netI    0.2013
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            63723
_diffrn_reflns_theta_full        68.25
_diffrn_reflns_theta_max         68.25
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    2.745
_exptl_absorpt_correction_T_max  0.9471
_exptl_absorpt_correction_T_min  0.4930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR, T.Higashi (1998)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       needle
_exptl_crystal_F_000             2556
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.698
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         10849
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.703
_refine_ls_R_factor_all          0.2092
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0692P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1364
_reflns_number_gt                3057
_reflns_number_total             10849
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja992511v.cif
_cod_data_source_block           yakucu
_cod_original_cell_volume        6219.3(8)
_cod_database_code               4116639