[μ-2,3,5,6-Tetrakis(2-pyridyl)pyrazine-κ^6^<i>N</i>^6^,<i>N</i>^1^,<i>N</i>^2^:<i>N</i>^3^,<i>N</i>^4^,<i>N</i>^5^]bis[diaqua(dihydrogen <i>m</i>-phenylenediphosphonato-κ<i>O</i>)nickel(II)] dihydrate
DeBurgomaster, Paul; Zubieta, Jon; Acta Crystallographica Section E 66 (2010) m1424–m1425; doi:10.1107/S1600536810041279

data_2227896
_publ_section_title
;
 [\m-2,3,5,6-Tetrakis(2-pyridyl)pyrazine-\k^6^<i>N</i>^6^,<i>N</i>^1^,<i>N</i>^2^:<i>N</i>^3^,<i>N</i>^4^,<i>N</i>^5^]bis[diaqua(dihydrogen
 <i>m</i>-phenylenediphosphonato-\k<i>O</i>)nickel(II)] dihydrate
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1424
_journal_page_last               m1425
_journal_paper_doi               10.1107/S1600536810041279
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac
'[Ni2 (C6 H6 O6 P2)2 (C24 H16 N6) (H2 O)4] , 2H2 O'
_chemical_formula_moiety         'C36 H36 N6 Ni2 O16 P4, 2(H2 O)'
_chemical_formula_sum            'C36 H40 N6 Ni2 O18 P4'
_chemical_formula_weight         1086.04
_chemical_name_systematic
;
[\m-2,3,5,6-Tetrakis(2-pyridyl)pyrazine-
\k^6^<i>N</i>^6^,<i>N</i>^1^,<i>N</i>^2^:<i>N</i>^3^,<i>N</i>^4^,<i>N</i>^5^]
bis[diaqua(dihydrogen
<i>m</i>-phenylenediphosphonato-\k<i>O</i>)nickel(II)] dihydrate
;
_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                85.386(2)
_cell_angle_beta                 81.7070(10)
_cell_angle_gamma                69.3640(10)
_cell_formula_units_Z            1
_cell_length_a                   7.9702(6)
_cell_length_b                   10.0785(8)
_cell_length_c                   14.0960(12)
_cell_measurement_reflns_used    3874
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.75
_cell_volume                     1048.03(15)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 1999)'
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10484
_diffrn_reflns_theta_full        28.08
_diffrn_reflns_theta_max         28.08
_diffrn_reflns_theta_min         2.75
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.138
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_correction_T_min  0.804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_meas      1.724(2)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       block
_exptl_crystal_F_000             558
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.909
_refine_diff_density_min         -0.797
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.322
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         5044
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.322
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0660
_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^)+(0.0262P)^2^+4.5072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1316
_refine_ls_wR_factor_ref         0.1327
_reflns_number_gt                4821
_reflns_number_total             5044
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            pk2273.cif
_cod_data_source_block           I
_cod_database_code               2227896
_cod_database_fobs_code          2227896