Aqua(dimethylformamide){tris[(1-methyl-1<i>H</i>-benzimidazol-2-yl)methyl]amine}nickel(II) dipicrate
Li, Ke; Sun, Tao; Yang, Yang; Jia, Beibei; Wu, Huilu; Acta Crystallographica Section E 66 (2010) m1025–; doi:10.1107/S1600536810029181

data_2226997
_publ_section_title
;
 Aqua(dimethylformamide){tris[(1-methyl-1<i>H</i>-benzimidazol-2-yl)methyl]amine}nickel(II)
 dipicrate
;
_journal_coeditor_code           LH5085
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1025
_journal_paper_doi               10.1107/S1600536810029181
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac
'[Ni (C27 H27 N7) (C3 H7 N O) (H2 O)] (C6 H2 N3 O7)2'
_chemical_formula_moiety         'C30 H36 N8 Ni O2 2+, 2(C6 H2 N3 O7 -)'
_chemical_formula_sum            'C42 H40 N14 Ni O16'
_chemical_formula_weight         1055.57
_chemical_name_systematic
;
Aqua(dimethylformamide){tris[(1-methyl-1<i>H</i>-benzimidazol-2-
yl)methyl]amine}nickel(II) dipicrate
;
_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                108.5830(10)
_cell_angle_beta                 95.7030(10)
_cell_angle_gamma                99.5060(10)
_cell_formula_units_Z            2
_cell_length_a                   12.0768(3)
_cell_length_b                   13.2619(4)
_cell_length_c                   15.3544(4)
_cell_measurement_reflns_used    8420
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.2386
_cell_measurement_theta_min      2.4172
_cell_volume                     2268.37(11)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'APEX2 (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics
'SHElXTL (Sheldrick, 2008) and 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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_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  0.0405
_diffrn_reflns_av_sigmaI/netI    0.0556
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18738
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    0.518
_exptl_absorpt_correction_T_max  0.9452
_exptl_absorpt_correction_T_min  0.8815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.006
_refine_diff_density_min         -1.237
_refine_ls_extinction_coef       0.0026(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         8420
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0452P)^2^+5.4011P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1592
_reflns_number_gt                5743
_reflns_number_total             8420
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh5085.cif
_cod_data_source_block           I
_cod_original_cell_volume        2268.36(11)
_cod_database_code               2226997
_cod_database_fobs_code          2226997