Bis[1,3-bis(1-benzyl-1<i>H</i>-benzimidazol-2-yl)-2-oxapropane]nickel(II) dipicrate–dimethylformamide–ethanol (1/2/0.25)
Wu, Huilu; Yun, Ruirui; Li, Ke; Wang, Kaitong; Huang, Xingcai; Acta Crystallographica Section E 65 (2009) m751–m752; doi:10.1107/S1600536809021163

data_2222391
_publ_section_title
;
 Bis[1,3-bis(1-benzyl-1<i>H</i>-benzimidazol-2-yl)-2-oxapropane]nickel(II)
 dipicrate--dimethylformamide--ethanol (1/2/0.25)
;
_journal_coeditor_code           LH2826
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m751
_journal_page_last               m752
_journal_paper_doi               10.1107/S1600536809021163
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac
'[Ni (C30 H26 N4 O)2] (C6 H2 N3 O7)2, 2C3 H7 N O, 0.25C2 H6 O'
_chemical_formula_moiety
'C60 H52 N8 Ni O2 2+, 2(C6 H2 N3 O7 -), 2(C3 H7 N O), 0.25(C2 H6 O)'
_chemical_formula_sum            'C78.5 H71.5 N16 Ni O18.25'
_chemical_formula_weight         1589.73
_chemical_name_systematic
;
Bis[1,3-bis(1-benzyl-1<i>H</i>-benzimidazol-2-yl)-2-oxapropane]nickel(II)
dipicrate--dimethylformamide--ethanol (1/2/0.25)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 107.5130(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.6265(4)
_cell_length_b                   18.1735(5)
_cell_length_c                   26.6287(8)
_cell_measurement_reflns_used    7422
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.25
_cell_measurement_theta_min      3.08
_cell_volume                     7673.2(4)
_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    '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 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER'
_diffrn_measurement_method       '\f and \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  0.1003
_diffrn_reflns_av_sigmaI/netI    0.0864
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            57512
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         3.08
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.335
_exptl_absorpt_correction_T_max  0.9641
_exptl_absorpt_correction_T_min  0.9484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3314
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.473
_refine_diff_density_min         -0.703
_refine_ls_extinction_coef       0.0065(7)
_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   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1031
_refine_ls_number_reflns         13620
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.1604
_refine_ls_R_factor_gt           0.0931
_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^)+(0.159P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2411
_refine_ls_wR_factor_ref         0.2896
_reflns_number_gt                7422
_reflns_number_total             13620
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh2826.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C78.50 H71.50 N16 Ni O18.25'
_cod_database_code               2222391
_cod_database_fobs_code          2222391