Bis(dimethylmalonato-κ^2^<i>O</i>,<i>O</i>')bis[4-(4-pyridylamino-κ<i>N</i>^4^)pyridinium]nickel(II) hexahydrate
Farnum, Gregory A.; LaDuca, Robert L.; Acta Crystallographica Section E 64 (2008) m1603–; doi:10.1107/S160053680803835X

data_2220305
_publ_section_title
;Bis(dimethylmalonato-\k^2^<i>O</i>,<i>O</i>')bis[4-(4-pyridylamino-\k<i>N</i>^4^)pyridinium]nickel(II)
 hexahydrate
;
_journal_coeditor_code           PK2132
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1603
_journal_paper_doi               10.1107/S160053680803835X
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Ni (C5 H6 O4)2 (C10 H10 N3)2] , 6H2 O'
_chemical_formula_moiety         'C30 H32 N6 Ni O8 , 6H2 O'
_chemical_formula_sum            'C30 H44 N6 Ni O14'
_chemical_formula_weight         771.42
_chemical_name_systematic
;
Bis(dimethylmalonato-\k^2^<i>O</i>,<i>O</i>')bis[4-(4-pyridylamino-
\k<i>N</i>^4^)pyridinium]nickel(II) hexahydrate
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.96(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.428(4)
_cell_length_b                   8.0473(16)
_cell_length_c                   23.731(5)
_cell_measurement_reflns_used    49338
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.09
_cell_measurement_theta_min      1.73
_cell_volume                     3485.3(13)
_computing_cell_refinement       'SMART (Bruker, 2006)'
_computing_data_collection       'SMART (Bruker, 2006)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2006)'
_computing_molecular_graphics    'Crystal Maker (Palmer, 2007)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Bruker SMART 1K'
_diffrn_measurement_method       \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  0.0785
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            49338
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.09
_diffrn_reflns_theta_min         1.73
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_correction_T_min  0.833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(TWINABS; Sheldrick, 2007)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.843
_refine_diff_density_min         -0.605
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         3998
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0996P)^2^+4.676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1517
_refine_ls_wR_factor_ref         0.1630
_reflns_number_gt                3222
_reflns_number_total             3998
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pk2132.cif
_cod_data_source_block           I
_cod_original_cell_volume        3485.4(12)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2220305
_cod_database_fobs_code          2220305