Bis[2,6-bis(1<i>H</i>-benzimidazol-2-yl)pyridine]nickel(II) dipicrate dimethylformamide disolvate
Huang, Xingcai; Kou, Fan; Qi, Baoliang; Meng, Xuan; Wu, Huilu; Acta Crystallographica Section E 66 (2010) m967–; doi:10.1107/S160053681002773X

data_2226992
_publ_section_title
;
 Bis[2,6-bis(1<i>H</i>-benzimidazol-2-yl)pyridine]nickel(II) dipicrate
 dimethylformamide disolvate
;
_journal_coeditor_code           LH5079
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m967
_journal_paper_doi               10.1107/S160053681002773X
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac
'[Ni (C19 H13 N5)2] (C6 H2 N3 O7)2, 2C3 H7 N O'
_chemical_formula_moiety
'C38 H26 N10 Ni 2+, 2(C6 H2 N3 O7 -), 2(C3 H7 N O)'
_chemical_formula_sum            'C56 H44 N18 Ni O16'
_chemical_formula_weight         1283.80
_chemical_name_systematic
;
Bis[2,6-bis(1<i>H</i>-benzimidazol-2-yl)pyridine]nickel(II) dipicrate
dimethylformamide disolvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 93.7750(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.2087(3)
_cell_length_b                   26.5215(5)
_cell_length_c                   14.6989(3)
_cell_measurement_reflns_used    12544
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.01
_cell_volume                     5527.06(19)
_computing_cell_refinement       'RAPID-AUTO Rigaku/MSC (2004)'
_computing_data_collection       'RAPID-AUTO Rigaku/MSC (2004)'
_computing_data_reduction        'RAPID-AUTO Rigaku/MSC (2004)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku R-AXIS Spider'
_diffrn_measurement_method       '\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  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            52251
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.442
_exptl_absorpt_correction_T_max  0.9206
_exptl_absorpt_correction_T_min  0.8569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.598
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     814
_refine_ls_number_reflns         12544
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+2.4350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.1062
_reflns_number_gt                9403
_reflns_number_total             12544
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh5079.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2226992
_cod_database_fobs_code          2226992