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_4303449
_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         'C12 H20 N4 O4 Pd, 2(B F4) '
_chemical_formula_sum            'C12 H20 B2 F8 N4 O4 Pd'
_chemical_formula_weight         564.32
_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'
_cell_angle_alpha                90.0000
_cell_angle_beta                 101.131(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   6.5039(6)
_cell_length_b                   14.0356(10)
_cell_length_c                   11.1689(8)
_cell_measurement_reflns_used    7184
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.2
_cell_volume                     1000.39(14)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.035
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9389
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    1.029
_exptl_absorpt_correction_T_max  0.857
_exptl_absorpt_correction_T_min  0.658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.873
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             560.00
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.75
_refine_diff_density_min         -0.66
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2283
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0150P)^2^+1.6371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0676
_reflns_number_gt                2023
_reflns_number_total             2283
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic900993j_si_002_7.cif
_cod_data_source_block           '_Pdtetraoxime'
_cod_original_cell_volume        1000.38(14)
_cod_original_formula_sum        'C12 H20 B2 F8 N4 O4 Pd '
_cod_database_code               4303449