Modulation of Multimetal Complexation Behavior of Tetraoxime Ligand by Covalent Transformation of Olefinic Functionalities
Shigehisa Akine; Satoko Kagiyama; Tatsuya Nabeshima; Inorganic Chemistry 49 (2010) 2141–2152; doi:10.1021/ic9019926

data_4314978
_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
;
 Modulation of Multimetal Complexation Behavior of Tetraoxime Ligand by
 Covalent Transformation of Olefinic Functionalities
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2141
_journal_page_last               2152
_journal_paper_doi               10.1021/ic9019926
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         C34.50H34BaN4O14.50Zn2
_chemical_formula_sum            'C34.5 H34 Ba N4 O14.5 Zn2'
_chemical_formula_weight         1004.74
_chemical_name_common            '[cis-LZn2Ba(OAc)2]_0.5MeOH'
_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                103.5402(16)
_cell_angle_beta                 107.7635(15)
_cell_angle_gamma                102.6695(17)
_cell_formula_units_Z            2
_cell_length_a                   10.5880(6)
_cell_length_b                   13.0232(7)
_cell_length_c                   15.2344(8)
_cell_measurement_reflns_used    17676
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      3.02
_cell_volume                     1846.52(18)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0493
_diffrn_reflns_av_sigmaI/netI    0.0563
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17676
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.02
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.419
_exptl_absorpt_correction_T_max  0.6433
_exptl_absorpt_correction_T_min  0.5306
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Rapid AUTO (Rigaku Corp.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.807
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1002
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.969
_refine_diff_density_min         -1.067
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         8040
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0569P)^2^+3.2031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1105
_reflns_number_gt                6985
_reflns_number_total             8040
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9019926_si_001_14.cif
_cod_data_source_block           cis-LZn2Ba
_cod_original_cell_volume        1846.52(17)
_cod_original_formula_sum        'C34.50 H34 Ba N4 O14.50 Zn2'
_cod_database_code               4314978