Core/Shell Oligometallic Template Synthesis of Macrocyclic Hexaoxime
Shigehisa Akine; Shuichi Sunaga; Takanori Taniguchi; Hayato Miyazaki; Tatsuya Nabeshima; Inorganic Chemistry 46 (2007) 2959–2961; doi:10.1021/ic062327s

data_4307837
_publ_contact_author_address
;
1-1-1 Tennodai, Tsukuba, Ibaraki 305-8571, Japan
;
_publ_contact_author_email       nabesima@chem.tsukuba.ac.jp
_publ_contact_author_fax         +81-29-853-4507
_publ_contact_author_name        'Tatsuya Nabeshima'
_publ_contact_author_phone       +81-29-853-4507
_publ_section_title
;
Core/Shell Oligometallic Template Synthesis of Macrocyclic Hexaoxime
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2959
_journal_page_last               2961
_journal_paper_doi               10.1021/ic062327s
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C32 H36 N6 O13'
_chemical_formula_sum            'C32 H36 N6 O13'
_chemical_formula_weight         712.67
_chemical_name_common            'cyclic oxime trimer'
_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                 93.050(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.574(1)
_cell_length_b                   30.384(1)
_cell_length_c                   15.263(1)
_cell_measurement_reflns_used    6626
_cell_measurement_temperature    120
_cell_measurement_theta_max      25.78
_cell_measurement_theta_min      2.41
_cell_volume                     3507.5(5)
_computing_cell_refinement       'DENZO, scalepack'
_computing_data_collection       DENZO
_computing_data_reduction        'DENZO, scalepack'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  ORTEP-3
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'MAC Science DIP-2030'
_diffrn_measurement_method       IP
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.015
_diffrn_reflns_av_sigmaI/netI    0.0172
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29483
_diffrn_reflns_theta_full        25.78
_diffrn_reflns_theta_max         25.78
_diffrn_reflns_theta_min         2.41
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_T_max  0.9843
_exptl_absorpt_correction_T_min  0.8709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   scalepack
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         6626
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0829P)^2^+1.5157P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1455
_reflns_number_gt                5949
_reflns_number_total             6626
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062327ssi20061206_010435_2.cif
_cod_data_source_block           H6L
_cod_database_code               4307837