Nuclearity Control of a Trisaloph Zinc Cluster Complex Dependent on Minute Structural Differences in the Bridging Anions
Masaki Yamamura; Hayato Miyazaki; Masaya Iida; Shigehisa Akine; Tatsuya Nabeshima; Inorganic Chemistry 50 (2011) 5315–5317; doi:10.1021/ic2002833

data_4325396
_publ_contact_author_address
;
Tsukuba, Ibaraki 305-8571, Japan
;
_publ_contact_author_email       akine@chem.tsukuba.ac.jp
_publ_contact_author_fax         +81-29-853-4527
_publ_contact_author_name        'Shigehisa Akine'
_publ_contact_author_phone       +81-29-853-4527
_publ_section_title
;
 Nuclearity Control of a Trisaloph Zinc Cluster Complex Dependent on
 Minute Structural Differences in the Bridging Anions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5315
_journal_page_last               5317
_journal_paper_doi               10.1021/ic2002833
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         C172H230Cl4N12O52Zn12
_chemical_formula_sum            'C172 H230 Cl4 O52 Zn12 n12'
_chemical_formula_weight         4223.92
_chemical_name_common
;
[(C66H72N6O12)Zn6(EtCO2)5(OH)(H2O)]2_(CH2Cl2)2(MeOH)2(H2O)2(C6H14)
;
_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                68.243(11)
_cell_angle_beta                 76.237(12)
_cell_angle_gamma                80.298(14)
_cell_formula_units_Z            1
_cell_length_a                   15.288(6)
_cell_length_b                   17.956(6)
_cell_length_c                   18.488(5)
_cell_measurement_reflns_used    36364
_cell_measurement_temperature    120
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      3.00
_cell_volume                     4560(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    'DIRDIF99 (Beurskens et al., 1999)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.1027
_diffrn_reflns_av_sigmaI/netI    0.1478
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36364
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_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    1.690
_exptl_absorpt_correction_T_max  0.7856
_exptl_absorpt_correction_T_min  0.5512
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Rapid AUTO (Rigaku Corp.)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2190
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.044
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1338
_refine_ls_number_reflns         16163
_refine_ls_number_restraints     368
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.1662
_refine_ls_R_factor_gt           0.0921
_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^)+(0.0718P)^2^+18.5068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2042
_refine_ls_wR_factor_ref         0.2443
_reflns_number_gt                8525
_reflns_number_total             16163
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2002833_si_002.cif
_cod_data_source_block           mh161
_cod_original_formula_sum        'C172 H230 Cl4 n12 O52 Zn12'
_cod_database_code               4325396