Bivalent, Trivalent, and Tetravalent Nickel Complexes with a Common Tridentate Deprotonated Pyridine Bis-Amide Ligand. Molecular Structures of Nickel(II) and Nickel(IV) and Redox Activity
Apurba Kumar Patra; Rabindranath Mukherjee; Inorganic Chemistry 38 (1999) 1388–1393; doi:10.1021/ic980672e

data_4321857
_publ_contact_author
;
     Prof. R. N. Mukherjee
     Indian Institute of Technology Kanpur
     Department of Chemistry
     208 016
     Kanpur
     India
;
_publ_contact_author_email       rnm@iitk.ernet.in
_publ_section_title
;
 Bivalent, Trivalent, and Tetravalent Nickel Complexes with a Common
 Tridentate Deprotonated Pyridine Bis-Amide Ligand. Molecular Structures
 of Nickel(II) and Nickel(IV) and Redox Activity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1388
_journal_page_last               1393
_journal_paper_doi               10.1021/ic980672e
_journal_volume                  38
_journal_year                    1999
_chemical_formula_analytical     'C54 H68 N8 O5 Ni'
_chemical_formula_moiety         'Ni C38 N6 O4 H26 2-, C16 N2 H40 2+,O H2'
_chemical_formula_structural
'(Ni(C19 N3 O2 H13)(C19 N3 O2 H13)) ((N C8 H20)(N C8 H20))(O H2))'
_chemical_formula_sum            'C54 H68 N8 Ni O5'
_chemical_formula_weight         966.69
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
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_audit_creation_date             98-00-08
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_cell_angle_alpha                90.00(1)
_cell_angle_beta                 90.00(2)
_cell_angle_gamma                90.00(2)
_cell_formula_units_Z            4
_cell_length_a                   10.175(2)
_cell_length_b                   20.834(3)
_cell_length_c                   23.765(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      28
_cell_measurement_theta_min      16
_cell_volume                     5037.8(15)
_diffrn_ambient_temperature      293
_diffrn_attenuator_code          13.364
_diffrn_measurement_device       CAD4mach
_diffrn_measurement_method       theta-2theta
_diffrn_radiation_detector       'proportional counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed xray_tube'
_diffrn_radiation_type           'Mo K- alpha'
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_diffrn_reflns_reduction_process No_monochr_Lp_applied
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        0.69
_diffrn_standards_interval_time  3600
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_exptl_absorpt_coefficient_mu    0.44
_exptl_absorpt_correction_T_max  0.8229
_exptl_absorpt_correction_T_min  0.8221
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            yellowish_brown
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_meas      1.281
_exptl_crystal_density_method    flotation
_exptl_crystal_description       'Block shaped'
_exptl_crystal_F_000             2063.58
_exptl_crystal_preparation
'Ethyl acetate diffusion to acetonitrile solution'
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_refine_diff_density_max         .961
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_refine_ls_abs_structure_details none
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_refine_ls_extinction_expression no
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.99
_refine_ls_hydrogen_treatment    no
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     308
_refine_ls_number_reflns         1509
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .212
_refine_ls_R_factor_obs          .069
_refine_ls_shift/esd_mean        0
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         .058
_refine_ls_wR_factor_obs         .044
_reflns_d_resolution_high        .842
_reflns_d_resolution_low         11.883
_reflns_limit_h_max              12
_reflns_limit_h_min              0
_reflns_limit_k_max              24
_reflns_limit_k_min              0
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_reflns_limit_l_min              0
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_reflns_number_total             4422
_reflns_observed_criterion       refl_observed_if_Inet_>_.000_sigma(Inet)
_cod_data_source_file            ic980672e_1.cif
_cod_data_source_block           C54H68N8O5Ni
_cod_original_cell_volume        5038(1)
_cod_original_sg_symbol_Hall     -P_2ab_2ac
_cod_original_formula_sum        'C54 H68 N8 O5 Ni'
_cod_database_code               4321857