Bis[2,6-bis(1-methyl-1<i>H</i>-benzimidazol-2-yl-κ<i>N</i>^3^)pyridine-κ<i>N</i>]zinc dipicrate methanol disolvate
Fan, Xuyang; Yuan, Jingkun; Bai, Ying; Kong, Jin; Wu, Huilu; Acta Crystallographica Section E 68 (2012) m1072–; doi:10.1107/S1600536812031443

data_2235904
_publ_section_title
;
 Bis[2,6-bis(1-methyl-1<i>H</i>-benzimidazol-2-yl-\k<i>N</i>^3^)pyridine-\k<i>N</i>]zinc
 dipicrate methanol disolvate
;
_journal_coeditor_code           LH5492
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1072
_journal_paper_doi               10.1107/S1600536812031443
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Zn (C21 H17 N5)2] (C6 H2 N3 O7)2, 2C H4 O'
_chemical_formula_moiety
'C42 H34 N10 Zn 2+, 2(C6 H2 N3 O7 -), 2(C H4 O)'
_chemical_formula_sum            'C56 H46 N16 O16 Zn'
_chemical_formula_weight         1264.46
_chemical_name_systematic
;
Bis[2,6-bis(1-methyl-1<i>H</i>-benzimidazol-2-yl-\k<i>N</i>^3^)pyridine-
\k<i>N</i>]zinc dipicrate methanol disolvate
;
_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
_cell_angle_alpha                80.8110(10)
_cell_angle_beta                 71.0120(10)
_cell_angle_gamma                88.5380(10)
_cell_formula_units_Z            2
_cell_length_a                   13.2007(3)
_cell_length_b                   13.8024(3)
_cell_length_c                   16.2009(3)
_cell_measurement_reflns_used    10153
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      3.08
_cell_volume                     2754.28(10)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_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      153(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEXII area-detector'
_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  0.0172
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22669
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_T_max  0.852
_exptl_absorpt_correction_T_min  0.816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.513
_refine_ls_extinction_coef       0.0020(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         10148
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+2.8031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1106
_reflns_number_gt                9024
_reflns_number_total             10148
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh5492.cif
_cod_data_source_block           I
_cod_database_code               2235904
_cod_database_fobs_code          2235904