Octaakis(4-aminopyridine)-1κ^4^<i>N</i>^1^,2κ^4^<i>N</i>^1^-aqua-2κ<i>O</i>-μ-carbonato-1:2κ^3^<i>O</i>,<i>O</i>':<i>O</i>''-dinickel(II) dichloride pentahydrate
Fun, Hoong-Kun; Sinthiya, A; Jebas, Samuel Robinson; Ravindran Durai Nayagam, B.; Alfred Cecil Raj, S.; Acta Crystallographica Section E 64 (2008) m1436–m1437; doi:10.1107/S1600536808033321

data_2219758
_publ_section_title
;Octaakis(4-aminopyridine)-1\k^4^<i>N</i>^1^,2\k^4^<i>N</i>^1^-aqua-2\k<i>O</i>-\m-carbonato-1:2\k^3^<i>O</i>,<i>O</i>':<i>O</i>''-dinickel(II)
 dichloride pentahydrate
;
_journal_coeditor_code           AT2653
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1436
_journal_page_last               m1437
_journal_paper_doi               10.1107/S1600536808033321
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Ni2 (C O3) (C5 H6 N2)8 (H2 O)] Cl2, 5H2 O'
_chemical_formula_moiety         'C41 H50 N16 Ni2 O4 2+, 2(Cl -), 5(H2 O)'
_chemical_formula_sum            'C41 H60 Cl2 N16 Ni2 O9'
_chemical_formula_weight         1109.37
_chemical_name_systematic
'Octaakis(4-aminopyridine)-1\k^4^N^1^,2\k^4^N^1^-aqua-2\kO-\m-carbonato-1:2\k^3^O,O':O''-dinickel(II) dichloride pentahydrate'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.7970(10)
_cell_angle_beta                 68.7480(10)
_cell_angle_gamma                75.1910(10)
_cell_formula_units_Z            2
_cell_length_a                   12.8877(3)
_cell_length_b                   14.7920(3)
_cell_length_c                   15.0510(3)
_cell_measurement_reflns_used    8874
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.91
_cell_measurement_theta_min      2.49
_cell_volume                     2583.59(10)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2003)
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD 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  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0521
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            42253
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.74
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.899
_exptl_absorpt_correction_T_max  0.8337
_exptl_absorpt_correction_T_min  0.5599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.73
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.221
_refine_diff_density_min         -1.940
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         13659
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0645
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0775P)^2^+7.7222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1656
_refine_ls_wR_factor_ref         0.1795
_reflns_number_gt                10282
_reflns_number_total             13659
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            at2653.cif
_cod_data_source_block           I
_cod_original_cell_volume        2583.59(9)
_cod_database_code               2219758
_cod_database_fobs_code          2219758