Synthesis, Characterization, and Spontaneous Resolution of Chiral Nickel(II) Complexes with the Tripod Ligand Tris[2-(((2-phenylimidazol-4-yl)methylidene)amino)ethyl]amine
Ikuko Katsuki; Naohide Matsumoto; Masaaki Kojima; Inorganic Chemistry 39 (2000) 3350–3354; doi:10.1021/ic9909025

data_4321171
_publ_contact_author_address
;
Department of Chemistry, Faculty of Science, Kumamoto University, Kurokami
2-39-1, Kumamoto 860-8555, Japan
;
_publ_contact_author_email       ' naohide@aster.sci.kumamoto-u.ac.jp '
_publ_contact_author_fax         ' +81-96-342-3390'
_publ_contact_author_name        ' Naohide Matsumoto'
_publ_contact_author_phone       ' +81-96-342-3390'
_publ_section_title
;
 Synthesis, Characterization, and Spontaneous Resolution of Chiral
 Nickel(II) Complexes with the Tripod Ligand
 Tris[2-(((2-phenylimidazol-4-yl)methylidene)amino)ethyl]amine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3350
_journal_page_last               3354
_journal_paper_doi               10.1021/ic9909025
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C37 H40 Cl2 N10 Ni O9'
_chemical_formula_weight         898.39
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_date             'Wed Jan 27 16:09:53 1999'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.206(2)
_cell_length_b                   22.735(3)
_cell_length_c                   12.696(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293.2
_cell_measurement_theta_max      11.7
_cell_measurement_theta_min      10.1
_cell_volume                     4100.5(13)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      293.2
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.00153
_diffrn_orient_matrix_UB_12      0.03892
_diffrn_orient_matrix_UB_13      -0.03667
_diffrn_orient_matrix_UB_21      -0.01806
_diffrn_orient_matrix_UB_22      -0.02001
_diffrn_orient_matrix_UB_23      -0.06717
_diffrn_orient_matrix_UB_31      -0.06802
_diffrn_orient_matrix_UB_32      0.00444
_diffrn_orient_matrix_UB_33      0.01865
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.192
_diffrn_reflns_av_sigmaI/netI    0.093
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4033
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.43
_diffrn_standards_decay_%        -1.00
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.670
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.931
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1864.00
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.71
_refine_diff_density_min         -1.04
_refine_ls_abs_structure_Flack   0.10(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.460
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     533
_refine_ls_number_reflns         2931
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0697
_refine_ls_shift/su_max          5.3140
_refine_ls_shift/su_mean         0.2680
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0435
_refine_ls_wR_factor_ref         0.0435
_reflns_number_gt                2931
_reflns_number_total             4029
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ic9909025_2.cif
_cod_data_source_block           '[Ni(H3L)](ClO4)2(2)'
_cod_original_cell_volume        4100.5(10)
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C37 H40 Cl2 N10 O9 Ni '
_cod_database_code               4321171