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_4321170
_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 N12 Ni O7'
_chemical_formula_weight         823.50
_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             'Fri Jul  2 10:17:51 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                   14.198(2)
_cell_length_b                   22.422(2)
_cell_length_c                   12.019(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293.2
_cell_measurement_theta_max      15.5
_cell_measurement_theta_min      11.2
_cell_volume                     3826.2(9)
_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      -0.00494
_diffrn_orient_matrix_UB_12      0.02807
_diffrn_orient_matrix_UB_13      0.06439
_diffrn_orient_matrix_UB_21      -0.00884
_diffrn_orient_matrix_UB_22      0.03408
_diffrn_orient_matrix_UB_23      -0.05265
_diffrn_orient_matrix_UB_31      -0.06970
_diffrn_orient_matrix_UB_32      -0.00631
_diffrn_orient_matrix_UB_33      0.00212
_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  0.000
_diffrn_reflns_av_sigmaI/netI    0.086
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3779
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.43
_diffrn_standards_decay_%        -5.14
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_correction_T_min  0.851
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1720.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.30
_refine_diff_density_min         -0.29
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     515
_refine_ls_number_reflns         2597
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.1270
_refine_ls_shift/su_mean         0.0160
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/\s^2^(Fo) + 0.00020|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0455
_refine_ls_wR_factor_ref         0.0429
_reflns_number_gt                2803
_reflns_number_total             3779
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ic9909025_1.cif
_cod_data_source_block           '[NiH3L(Ph)](NO3)2(1)'
_cod_original_cell_volume        3826.4(6)
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C37 H40 N12 O7 Ni '
_cod_database_code               4321170