Bis[bis(1-ethylbenzimidazol-2-ylmethyl) ether]cobalt(II) dipicrate dimethylformamide disolvate
Wu, Huilu; Yun, Ruirui; Sun, Tao; Li, Ke; Meng, Xuan; Acta Crystallographica Section E 65 (2009) m1196–m1197; doi:10.1107/S1600536809035934

data_2223471
_publ_section_title
;
 Bis[bis(1-ethylbenzimidazol-2-ylmethyl) ether]cobalt(II) dipicrate
 dimethylformamide disolvate
;
_journal_coeditor_code           LH2889
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1196
_journal_page_last               m1197
_journal_paper_doi               10.1107/S1600536809035934
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac
'[Co (C20 H22 N4 O)2] (C6 H2 N3 O7)2, 2C3 H7 N O'
_chemical_formula_moiety
'C40 H44 Co N8 O2 2+, 2(C6 H2 N3 O7 -), 2(C3 H7 N O)'
_chemical_formula_sum            'C58 H62 Co N16 O18'
_chemical_formula_weight         1330.17
_chemical_name_systematic
;
Bis[bis(1-ethylbenzimidazol-2-ylmethyl) ether]cobalt(II)
dipicrate dimethylformamide 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                110.6640(10)
_cell_angle_beta                 96.4700(10)
_cell_angle_gamma                99.6120(10)
_cell_formula_units_Z            2
_cell_length_a                   13.8799(4)
_cell_length_b                   14.6525(4)
_cell_length_c                   16.5701(3)
_cell_measurement_reflns_used    7749
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      3.00
_cell_volume                     3054.62(14)
_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) and PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku R-AXIS Spider'
_diffrn_measurement_method       '\f and \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  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24337
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.368
_exptl_absorpt_correction_T_max  0.9503
_exptl_absorpt_correction_T_min  0.8729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1386
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.980
_refine_diff_density_min         -0.895
_refine_ls_extinction_coef       0.0022(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   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     858
_refine_ls_number_reflns         11225
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.10
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0663P)^2^+2.0559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1360
_reflns_number_gt                8833
_reflns_number_total             11225
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh2889.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 'Triclinic' changed to 'triclinic'
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_cell_volume        3054.62(13)
_cod_database_code               2223471
_cod_database_fobs_code          2223471