#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:37:47 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179757 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/53/7005363.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7005363
loop_
_publ_author_name
'Lee, Way-Zen'
'Tseng, Huan-Sheng'
'Kuo, Ting-Shen'
_publ_section_title
;
 Ligand-controlled nuclearity in nickel bis(benzimidazolyl) complexes.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2563
_journal_page_last               2570
_journal_paper_doi               10.1039/b701367a
_journal_year                    2007
_chemical_formula_moiety         'C43 H51 Cl N10 Ni2 O7'
_chemical_formula_sum            'C43 H51 Cl N10 Ni2 O7'
_chemical_formula_weight         972.81
_chemical_name_systematic
;
?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 128.4430(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.0019(3)
_cell_length_b                   21.3390(5)
_cell_length_c                   15.9920(4)
_cell_measurement_reflns_used    27760
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.037
_cell_volume                     5346.1(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'HKL Denzo and Scalepack (O & M 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0544
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21655
_diffrn_reflns_theta_full        25.38
_diffrn_reflns_theta_max         25.38
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    0.806
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.6896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         5039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0469
_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/[σ²(Fo²)+(0.0779P)²+6.8897P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1370
_refine_ls_wR_factor_ref         0.1424
_reflns_number_gt                4221
_reflns_number_total             5039
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b701367a.txt
_cod_data_source_block           complex_5
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7005363
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.04612(19) 0.24406(14) 0.2276(2) 0.0362(6) Uani 1 1 d . . .
C2 C -0.0445(2) 0.30893(14) 0.2219(3) 0.0435(7) Uani 1 1 d . . .
H2 H -0.0290 0.3285 0.1843 0.052 Uiso 1 1 calc R . .
C3 C -0.0671(3) 0.34314(17) 0.2745(3) 0.0561(9) Uani 1 1 d . . .
H3 H -0.0670 0.3867 0.2720 0.067 Uiso 1 1 calc R . .
C4 C -0.0902(3) 0.31330(18) 0.3315(3) 0.0618(10) Uani 1 1 d . . .
H4 H -0.1046 0.3378 0.3663 0.074 Uiso 1 1 calc R . .
C5 C -0.0922(2) 0.24947(18) 0.3376(3) 0.0549(9) Uani 1 1 d . . .
H5 H -0.1082 0.2301 0.3748 0.066 Uiso 1 1 calc R . .
C6 C -0.0691(2) 0.21486(16) 0.2854(2) 0.0407(7) Uani 1 1 d . . .
C7 C -0.0735(3) 0.10175(18) 0.3314(3) 0.0603(10) Uani 1 1 d . . .
H7A H -0.0933 0.1202 0.3672 0.090 Uiso 1 1 calc R . .
H7B H -0.0208 0.0801 0.3825 0.090 Uiso 1 1 calc R . .
H7C H -0.1154 0.0727 0.2785 0.090 Uiso 1 1 calc R . .
C8 C -0.0321(2) 0.14397(14) 0.2218(2) 0.0383(7) Uani 1 1 d . . .
C9 C -0.0111(2) 0.08343(15) 0.1968(3) 0.0465(8) Uani 1 1 d . . .
H9A H 0.0146 0.0552 0.2571 0.056 Uiso 1 1 calc R . .
H9B H -0.0629 0.0641 0.1357 0.056 Uiso 1 1 calc R . .
C10 C 0.1387(2) 0.08267(14) 0.2635(3) 0.0464(8) Uani 1 1 d . . .
H10A H 0.1654 0.0596 0.2389 0.056 Uiso 1 1 calc R . .
H10B H 0.1427 0.0574 0.3169 0.056 Uiso 1 1 calc R . .
C11 C 0.1847(2) 0.14299(13) 0.3123(2) 0.0359(6) Uani 1 1 d . . .
C12 C 0.3146(2) 0.09950(17) 0.4857(3) 0.0535(9) Uani 1 1 d . . .
H12A H 0.3659 0.1172 0.5483 0.080 Uiso 1 1 calc R . .
H12B H 0.3289 0.0701 0.4536 0.080 Uiso 1 1 calc R . .
H12C H 0.2837 0.0784 0.5052 0.080 Uiso 1 1 calc R . .
C13 C 0.28038(19) 0.21292(15) 0.4242(2) 0.0356(6) Uani 1 1 d . . .
C14 C 0.3488(2) 0.24680(17) 0.5091(2) 0.0444(8) Uani 1 1 d . . .
H14 H 0.3944 0.2272 0.5711 0.053 Uiso 1 1 calc R . .
C15 C 0.3460(2) 0.31033(17) 0.4971(3) 0.0479(8) Uani 1 1 d . . .
H15 H 0.3908 0.3343 0.5529 0.057 Uiso 1 1 calc R . .
C16 C 0.2787(2) 0.34077(15) 0.4046(2) 0.0430(7) Uani 1 1 d . . .
H16 H 0.2799 0.3841 0.4000 0.052 Uiso 1 1 calc R . .
C17 C 0.2101(2) 0.30743(13) 0.3196(3) 0.0392(7) Uani 1 1 d . . .
H17 H 0.1649 0.3275 0.2580 0.047 Uiso 1 1 calc R . .
C18 C 0.21163(19) 0.24249(13) 0.3303(2) 0.0338(6) Uani 1 1 d . . .
C19 C -0.1540(3) 0.1665(3) -0.0657(4) 0.0854(15) Uani 1 1 d . . .
C20 C -0.1914(4) 0.2230(3) -0.0757(4) 0.1027(18) Uani 1 1 d . . .
H20A H -0.1518 0.2563 -0.0563 0.154 Uiso 1 1 calc R . .
H20B H -0.2066 0.2236 -0.0294 0.154 Uiso 1 1 calc R . .
H20C H -0.2417 0.2285 -0.1482 0.154 Uiso 1 1 calc R . .
C21 C 0.0000 0.30881(17) 0.0000 0.0331(9) Uani 1 2 d S . .
C22 C 0.0000 0.3799(2) 0.0000 0.0566(13) Uani 1 2 d S . .
H22A H 0.0194 0.3949 0.0684 0.085 Uiso 0.50 1 calc PR . .
H22B H -0.0568 0.3949 -0.0544 0.085 Uiso 0.50 1 calc PR . .
H22C H 0.0374 0.3949 -0.0140 0.085 Uiso 0.50 1 calc PR . .
C23 C 0.2871(6) 0.0000 0.7517(6) 0.102(2) Uani 1 2 d S . .
H23A H 0.2855 0.0424 0.7704 0.153 Uiso 0.50 1 calc PR . .
H23B H 0.3318 -0.0225 0.8145 0.153 Uiso 0.50 1 calc PR . .
H23C H 0.2333 -0.0199 0.7209 0.153 Uiso 0.50 1 calc PR . .
Cl1 Cl 0.12818(8) 0.0000 0.46290(9) 0.0501(3) Uani 1 2 d S . .
N1 N -0.02348(16) 0.19758(11) 0.18856(19) 0.0360(6) Uani 1 1 d . . .
N2 N -0.05981(16) 0.15120(12) 0.2795(2) 0.0406(6) Uani 1 1 d . . .
N3 N 0.04851(17) 0.09399(11) 0.17327(19) 0.0409(6) Uani 1 1 d . . .
H3' H 0.0336 0.0679 0.1191 0.049 Uiso 1 1 calc R . .
N4 N 0.26123(16) 0.14971(12) 0.40902(19) 0.0386(6) Uani 1 1 d . . .
N5 N 0.15247(16) 0.19686(10) 0.26151(19) 0.0350(6) Uani 1 1 d . . .
Ni1 Ni 0.03361(2) 0.190054(16) 0.11825(3) 0.03282(15) Uani 1 1 d . . .
O1 O -0.07957(15) 0.16528(11) -0.03354(16) 0.0437(5) Uani 1 1 d . . .
O2 O -0.1937(3) 0.1136(3) -0.0867(5) 0.172(2) Uani 1 1 d . . .
O3 O 0.02410(13) 0.28236(9) 0.08495(15) 0.0359(5) Uani 1 1 d . . .
O4 O 0.3022(3) 0.0000 0.6791(4) 0.1018(16) Uani 1 2 d S . .
H4' H 0.3528 0.0077 0.7098 0.153 Uiso 0.50 1 calc PR . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 130.9(3) . . ?
N1 C1 C6 108.0(3) . . ?
C2 C1 C6 120.9(3) . . ?
C3 C2 C1 117.2(3) . . ?
C3 C2 H2 121.4 . . ?
C1 C2 H2 121.4 . . ?
C2 C3 C4 121.2(3) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C5 C4 C3 122.2(3) . . ?
C5 C4 H4 118.9 . . ?
C3 C4 H4 118.9 . . ?
C4 C5 C6 116.8(3) . . ?
C4 C5 H5 121.6 . . ?
C6 C5 H5 121.6 . . ?
N2 C6 C5 132.2(3) . . ?
N2 C6 C1 106.1(3) . . ?
C5 C6 C1 121.7(3) . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 N2 112.9(3) . . ?
N1 C8 C9 121.0(3) . . ?
N2 C8 C9 126.1(3) . . ?
N3 C9 C8 110.2(2) . . ?
N3 C9 H9A 109.6 . . ?
C8 C9 H9A 109.6 . . ?
N3 C9 H9B 109.6 . . ?
C8 C9 H9B 109.6 . . ?
H9A C9 H9B 108.1 . . ?
N3 C10 C11 110.7(2) . . ?
N3 C10 H10A 109.5 . . ?
C11 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
N5 C11 N4 112.7(3) . . ?
N5 C11 C10 121.6(3) . . ?
N4 C11 C10 125.8(3) . . ?
N4 C12 H12A 109.5 . . ?
N4 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N4 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 C14 132.6(3) . . ?
N4 C13 C18 105.7(2) . . ?
C14 C13 C18 121.7(3) . . ?
C15 C14 C13 116.8(3) . . ?
C15 C14 H14 121.6 . . ?
C13 C14 H14 121.6 . . ?
C14 C15 C16 122.6(3) . . ?
C14 C15 H15 118.7 . . ?
C16 C15 H15 118.7 . . ?
C17 C16 C15 121.1(3) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C16 C17 C18 117.2(3) . . ?
C16 C17 H17 121.4 . . ?
C18 C17 H17 121.4 . . ?
N5 C18 C17 130.9(3) . . ?
N5 C18 C13 108.4(3) . . ?
C17 C18 C13 120.6(3) . . ?
O1 C19 O2 118.3(6) . . ?
O1 C19 C20 119.6(5) . . ?
O2 C19 C20 122.1(6) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O3 C21 O3 126.7(4) 2 . ?
O3 C21 C22 116.67(18) 2 . ?
O3 C21 C22 116.67(18) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O4 C23 H23A 109.5 . . ?
O4 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
O4 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C8 N1 C1 106.1(2) . . ?
C8 N1 Ni1 114.3(2) . . ?
C1 N1 Ni1 138.74(19) . . ?
C8 N2 C6 106.8(2) . . ?
C8 N2 C7 127.2(3) . . ?
C6 N2 C7 125.9(3) . . ?
C10 N3 C9 114.7(2) . . ?
C10 N3 Ni1 109.13(18) . . ?
C9 N3 Ni1 108.54(18) . . ?
C10 N3 H3' 108.1 . . ?
C9 N3 H3' 108.1 . . ?
Ni1 N3 H3' 108.1 . . ?
C11 N4 C13 107.4(2) . . ?
C11 N4 C12 126.7(3) . . ?
C13 N4 C12 125.9(3) . . ?
C11 N5 C18 105.8(2) . . ?
C11 N5 Ni1 114.3(2) . . ?
C18 N5 Ni1 139.69(19) . . ?
O3 Ni1 N5 94.57(8) . . ?
O3 Ni1 N1 94.31(8) . . ?
N5 Ni1 N1 92.07(10) . . ?
O3 Ni1 O1 94.77(8) . . ?
N5 Ni1 O1 167.87(9) . . ?
N1 Ni1 O1 94.91(9) . . ?
O3 Ni1 O1 94.69(8) . 2 ?
N5 Ni1 O1 94.00(9) . 2 ?
N1 Ni1 O1 168.70(9) . 2 ?
O1 Ni1 O1 77.54(10) . 2 ?
O3 Ni1 N3 172.92(8) . . ?
N5 Ni1 N3 80.90(9) . . ?
N1 Ni1 N3 80.50(9) . . ?
O1 Ni1 N3 90.48(9) . . ?
O1 Ni1 N3 91.07(9) 2 . ?
C19 O1 Ni1 128.7(3) . . ?
C19 O1 Ni1 128.1(3) . 2 ?
Ni1 O1 Ni1 95.23(9) . 2 ?
C21 O3 Ni1 129.3(2) . . ?
C23 O4 H4' 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.389(4) . ?
C1 C2 1.389(4) . ?
C1 C6 1.407(4) . ?
C2 C3 1.384(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.406(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.368(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.392(4) . ?
C5 H5 0.9300 . ?
C6 N2 1.382(4) . ?
C7 N2 1.471(4) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 N1 1.317(4) . ?
C8 N2 1.348(4) . ?
C8 C9 1.489(4) . ?
C9 N3 1.473(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N3 1.469(4) . ?
C10 C11 1.490(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N5 1.321(4) . ?
C11 N4 1.346(4) . ?
C12 N4 1.471(4) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 N4 1.382(4) . ?
C13 C14 1.389(4) . ?
C13 C18 1.406(4) . ?
C14 C15 1.365(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.396(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.385(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.394(4) . ?
C17 H17 0.9300 . ?
C18 N5 1.393(4) . ?
C19 O1 1.237(5) . ?
C19 O2 1.297(7) . ?
C19 C20 1.374(8) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 O3 1.258(3) 2 ?
C21 O3 1.258(3) . ?
C21 C22 1.517(6) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 O4 1.369(8) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
N1 Ni1 2.047(2) . ?
N3 Ni1 2.177(2) . ?
N3 H3' 0.9100 . ?
N5 Ni1 2.037(2) . ?
Ni1 O3 2.018(2) . ?
Ni1 O1 2.113(2) . ?
Ni1 O1 2.123(2) 2 ?
O1 Ni1 2.123(2) 2 ?
O4 H4' 0.8200 . ?
