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_4307836
_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         C43H55N6O27.50Zn6
_chemical_formula_sum            'C43 H55 N6 O27.5 Zn6'
_chemical_formula_weight         1488.15
_chemical_name_common
;
[(C30H24N6O12Zn6)(CH3CO2)5(OH)](MeOH)3(H2O)1.5
;
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                101.521(10)
_cell_angle_beta                 99.117(12)
_cell_angle_gamma                96.200(10)
_cell_formula_units_Z            4
_cell_length_a                   14.503(5)
_cell_length_b                   18.608(5)
_cell_length_c                   21.841(6)
_cell_measurement_reflns_used    44115
_cell_measurement_temperature    120
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      3.00
_cell_volume                     5643(3)
_computing_cell_refinement       'Rapid AUTO (Rigaku Corp.)'
_computing_data_collection       'Rapid AUTO (Rigaku Corp.)'
_computing_data_reduction        'Rapid AUTO (Rigaku Corp.)'
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku R-AXIS Rapid'
_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  0.1277
_diffrn_reflns_av_sigmaI/netI    0.1807
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            44115
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.601
_exptl_absorpt_correction_T_max  0.6963
_exptl_absorpt_correction_T_min  0.5091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Rapid AUTO (Rigaku Corp.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3020
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.100
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1570
_refine_ls_number_reflns         19828
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1252
_refine_ls_R_factor_gt           0.0804
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0791P)^2^+12.3788P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1976
_refine_ls_wR_factor_ref         0.2244
_reflns_number_gt                12163
_reflns_number_total             19828
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062327ssi20061206_010435_1.cif
_cod_data_source_block           LZn6
_cod_original_formula_sum        'C43 H55 N6 O27.50 Zn6'
_cod_database_code               4307836