Nickel(II) Complexes with Tetra- and Pentadentate Aminopyridine Ligands: Synthesis, Structure, Electrochemistry, and Reduction to Nickel(I) Species
Sergey V. Kryatov; B. Sharmila Mohanraj; Vladislav V. Tarasov; Olga P. Kryatova; Elena V. Rybak-Akimova; Bharathi Nuthakki; James F. Rusling; Richard J. Staples; Alexander Y. Nazarenko; Inorganic Chemistry 41 (2002) 923–930; doi:10.1021/ic010397n

data_4317538
_publ_section_title
;
 Nickel(II) Complexes with Tetra- and Pentadentate Aminopyridine Ligands:
 Synthesis, Structure, Electrochemistry, and Reduction to Nickel(I)
 Species
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              923
_journal_page_last               930
_journal_paper_doi               10.1021/ic010397n
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         Ni(C24N5H31)(ClO4)2
_chemical_formula_sum            'C24 H31 Cl2 N5 Ni O8'
_chemical_formula_weight         647.15
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 118.80(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   40.638(19)
_cell_length_b                   7.6872(7)
_cell_length_c                   40.183(13)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      11
_cell_volume                     11000(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.462
_diffrn_measured_fraction_theta_max 0.462
_diffrn_measurement_device_type  'Rigaku AFC5S'
_diffrn_measurement_method       omega
_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  0.056
_diffrn_reflns_av_sigmaI/netI    0.0557
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            10701
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.98
_diffrn_standards_decay_%        <0.3%
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.957
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5376
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.932
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         9743
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1079
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0781P)^2^+35.3269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1415
_refine_ls_wR_factor_ref         0.1688
_reflns_number_gt                5848
_reflns_number_total             9743
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010397n_1.cif
_cod_data_source_block           al17n
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0781P)^2^+35.3269P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0781P)^2^+35.3269P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        11000(6)
_cod_database_code               4317538