One-Pot, Template Syntheses of a New Class of Metallomacrocycles with a Tetraoxime Cyclic Skeleton
Shohei Tashiro; Ai Minoda; Mihoko Yamada; Mitsuhiko Shionoya; Inorganic Chemistry 48 (2009) 10093–10101; doi:10.1021/ic900993j

data_4303447
_publ_contact_author_address
;
Department of Chemistry
The University of Tokyo
Graduate School of Science
7-3-1, Hongo
Bunkyo-ku
Tokyo
113-0033
;
_publ_contact_author_email       ' shionoya@chem.s.u-tokyo.ac.jp '
_publ_contact_author_fax         ' 81-3-5841-8061 '
_publ_contact_author_name        ' Prof Mitsuhiko Shionoya '
_publ_contact_author_phone       ' 81-3-5841-8061 '
_publ_section_title
;
One-Pot, Template Syntheses of a New Class of Metallomacrocycles with a
Tetraoxime Cyclic Skeleton
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10093
_journal_page_last               10101
_journal_paper_doi               10.1021/ic900993j
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C16 H26 Fe N6 O4, 2(Cl O4) '
_chemical_formula_sum            'C16 H26 Cl2 Fe N6 O12'
_chemical_formula_weight         621.17
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 101.9473(19)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   15.1943(7)
_cell_length_b                   9.6651(4)
_cell_length_c                   17.3481(11)
_cell_measurement_reflns_used    10841
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     2492.5(2)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku & RAC 2007)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'CrystalStructure (Rigaku & RAC 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Burla, 1994)'
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.084
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23746
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.890
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.671
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1280.00
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.57
_refine_diff_density_min         -0.63
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5712
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0502P)^2^+0.3001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1208
_reflns_number_gt                3626
_reflns_number_total             5712
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic900993j_si_002_5.cif
_cod_data_source_block           '_Fetetraoxime'
_cod_original_formula_sum        'C16 H26 Cl2 Fe N6 O12 '
_cod_database_code               4303447