Tetrakis[3-(2-pyridylamino)pyridine-κ<i>N</i>]nickel(II) diperchlorate ethanol disolvate
Wang, Zhi-Min; Acta Crystallographica Section E 64 (2008) m540–; doi:10.1107/S1600536808006569

data_2217849
_publ_section_title
;
 Tetrakis[3-(2-pyridylamino)pyridine-\k<i>N</i>]nickel(II)
 diperchlorate ethanol disolvate
;
_journal_coeditor_code           AT2548
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m540
_journal_paper_doi               10.1107/S1600536808006569
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Ni (C10 H9 N3)4] (Cl O4)2, 2C2 H6 O'
_chemical_formula_moiety         'C40 H36 N12 Ni 2+, 2(Cl O4 -), 2(C2 H6 O)'
_chemical_formula_sum            'C44 H48 Cl2 N12 Ni O10'
_chemical_formula_weight         1034.55
_chemical_name_systematic
;
Tetrakis[3-(2-pyridylamino)pyridine-\kN]nickel(II) bis(perchlorate) ethanol
disolvate
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.891(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.767(4)
_cell_length_b                   10.7067(14)
_cell_length_c                   18.144(2)
_cell_measurement_reflns_used    4315
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      1.63
_cell_volume                     4852.7(11)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0792
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11042
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.63
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.579
_exptl_absorpt_correction_T_max  0.9080
_exptl_absorpt_correction_T_min  0.8364
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.364
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         4315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.084
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0501P)^2^+1.1196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1341
_reflns_number_gt                2875
_reflns_number_total             4315
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            at2548.cif
_cod_data_source_block           I
_cod_original_cell_volume        4852.6(11)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2217849
_cod_database_fobs_code          2217849