#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:37:47 +0100 (vie 25 de mar de 2016) $
#$Revision: 179757 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/53/7005365.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_7005365
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         'C40 H54 Cl4 N10 Ni2 O4'
_chemical_formula_sum            'C40 H54 Cl4 N10 Ni2 O4'
_chemical_formula_weight         998.15
_chemical_name_systematic
;
?
;
_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                113.6570(10)
_cell_angle_beta                 99.9230(10)
_cell_angle_gamma                100.4470(10)
_cell_formula_units_Z            1
_cell_length_a                   8.4850(2)
_cell_length_b                   11.8690(3)
_cell_length_c                   12.9820(4)
_cell_measurement_reflns_used    23359
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.037
_cell_volume                     1133.25(5)
_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-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0572
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17699
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    1.118
_exptl_absorpt_correction_T_max  0.8003
_exptl_absorpt_correction_T_min  0.7273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.165
_refine_ls_extinction_coef       0.024(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0502
_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)+(0.0854P)²+0.6869P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1376
_refine_ls_wR_factor_ref         0.1467
_reflns_number_gt                3328
_reflns_number_total             4000
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b701367a.txt
_cod_data_source_block           complex_1
_cod_database_code               7005365
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Ni1 Ni 0.53111(5) 0.15566(4) 0.11005(4) 0.0353(2) Uani 1 1 d . . .
Cl1 Cl 0.82600(11) 0.20240(9) 0.14692(8) 0.0481(3) Uani 1 1 d . . .
Cl2 Cl 0.49395(11) 0.05793(8) -0.10239(7) 0.0402(3) Uani 1 1 d . . .
O1 O 0.1728(6) 0.7951(5) 0.1390(6) 0.1136(16) Uani 1 1 d . . .
H1 H 0.2327 0.8306 0.1113 0.170 Uiso 1 1 calc R . .
O2 O 0.8459(8) 0.0312(6) 0.3226(7) 0.168(3) Uani 1 1 d . . .
H2' H 0.7798 0.0378 0.2726 0.252 Uiso 1 1 calc R . .
N1 N 0.4970(4) 0.3216(3) 0.1093(2) 0.0387(7) Uani 1 1 d . . .
N2 N 0.3200(4) 0.4306(3) 0.0817(3) 0.0489(8) Uani 1 1 d . . .
N3 N 0.2630(4) 0.1088(3) 0.0693(3) 0.0398(7) Uani 1 1 d . . .
H3' H 0.233(6) 0.035(4) 0.017(4) 0.055(13) Uiso 1 1 d . . .
N4 N 0.3364(4) 0.2581(3) 0.3913(3) 0.0489(8) Uani 1 1 d . . .
N5 N 0.5066(4) 0.2239(3) 0.2771(2) 0.0378(7) Uani 1 1 d . . .
C1 C 0.5858(5) 0.4483(4) 0.1501(3) 0.0457(9) Uani 1 1 d . . .
C2 C 0.7552(6) 0.5088(4) 0.2050(4) 0.0562(11) Uani 1 1 d . . .
H2 H 0.8287 0.4604 0.2182 0.067 Uiso 1 1 d R . .
C3 C 0.8088(7) 0.6392(5) 0.2391(4) 0.0712(14) Uani 1 1 d . . .
H3 H 0.9239 0.6853 0.2775 0.085 Uiso 1 1 d R . .
C4 C 0.6962(9) 0.7068(5) 0.2160(4) 0.0760(16) Uani 1 1 d . . .
H4 H 0.7372 0.7970 0.2402 0.091 Uiso 1 1 d R . .
C5 C 0.5315(8) 0.6470(5) 0.1626(4) 0.0696(14) Uani 1 1 d . . .
H5 H 0.4544 0.6917 0.1464 0.084 Uiso 1 1 d R . .
C6 C 0.4747(6) 0.5169(4) 0.1314(3) 0.0517(10) Uani 1 1 d . . .
C7 C 0.1623(6) 0.4587(5) 0.0500(4) 0.0662(13) Uani 1 1 d . . .
H7A H 0.1854 0.5475 0.0670 0.079 Uiso 1 1 d R . .
H7B H 0.0902 0.4413 0.0945 0.079 Uiso 1 1 d R . .
H7C H 0.1090 0.4067 -0.0319 0.079 Uiso 1 1 d R . .
C8 C 0.3406(5) 0.3154(4) 0.0708(3) 0.0425(9) Uani 1 1 d . . .
C9 C 0.2055(5) 0.1925(4) 0.0213(4) 0.0480(10) Uani 1 1 d . . .
H9A H 0.1802 0.1511 -0.0624 0.058 Uiso 1 1 d R . .
H9B H 0.1071 0.2092 0.0441 0.058 Uiso 1 1 d R . .
C10 C 0.2104(5) 0.1171(4) 0.1740(4) 0.0471(9) Uani 1 1 d . . .
H10A H 0.1184 0.1538 0.1775 0.057 Uiso 1 1 d R . .
H10B H 0.1764 0.0331 0.1694 0.057 Uiso 1 1 d R . .
C11 C 0.3508(4) 0.2006(3) 0.2810(3) 0.0408(8) Uani 1 1 d . . .
C12 C 0.1840(7) 0.2527(6) 0.4289(5) 0.0750(15) Uani 1 1 d . . .
H12A H 0.2120 0.3023 0.5122 0.090 Uiso 1 1 d R . .
H12B H 0.1290 0.1654 0.4081 0.090 Uiso 1 1 d R . .
H12C H 0.1113 0.2869 0.3918 0.090 Uiso 1 1 d R . .
C13 C 0.4955(5) 0.3254(4) 0.4635(4) 0.0497(10) Uani 1 1 d . . .
C14 C 0.5549(7) 0.4029(5) 0.5834(4) 0.0695(13) Uani 1 1 d . . .
H14 H 0.4793 0.4169 0.6314 0.083 Uiso 1 1 d R . .
C15 C 0.7255(8) 0.4566(5) 0.6269(4) 0.0798(16) Uani 1 1 d . . .
H15 H 0.7703 0.5142 0.7086 0.096 Uiso 1 1 d R . .
C16 C 0.8322(7) 0.4323(5) 0.5562(4) 0.0680(13) Uani 1 1 d . . .
H16 H 0.9496 0.4685 0.5933 0.082 Uiso 1 1 d R . .
C17 C 0.7726(5) 0.3558(4) 0.4368(4) 0.0519(10) Uani 1 1 d . . .
H17 H 0.8441 0.3406 0.3857 0.062 Uiso 1 1 d R . .
C18 C 0.6022(5) 0.3024(3) 0.3909(3) 0.0407(8) Uani 1 1 d . . .
C19 C 0.2339(10) 0.8578(8) 0.2641(8) 0.116(3) Uani 1 1 d . . .
H19A H 0.3330 0.9259 0.2873 0.174 Uiso 1 1 calc R . .
H19B H 0.2591 0.7972 0.2913 0.174 Uiso 1 1 calc R . .
H19C H 0.1506 0.8922 0.2973 0.174 Uiso 1 1 calc R . .
C20 C 0.7722(18) 0.0429(9) 0.4237(10) 0.195(6) Uani 1 1 d . . .
H20A H 0.8536 0.0433 0.4853 0.292 Uiso 1 1 calc R . .
H20B H 0.6760 -0.0284 0.3976 0.292 Uiso 1 1 calc R . .
H20C H 0.7405 0.1211 0.4522 0.292 Uiso 1 1 calc R . .
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'
Ni Ni 0.3393 1.1124 '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'
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 Ni1 N5 87.96(11) . . ?
N1 Ni1 N3 80.39(12) . . ?
N5 Ni1 N3 81.22(12) . . ?
N1 Ni1 Cl1 100.04(9) . . ?
N5 Ni1 Cl1 101.06(8) . . ?
N3 Ni1 Cl1 177.69(9) . . ?
N1 Ni1 Cl2 90.89(8) . . ?
N5 Ni1 Cl2 167.51(8) . . ?
N3 Ni1 Cl2 86.33(9) . . ?
Cl1 Ni1 Cl2 91.39(3) . . ?
N1 Ni1 Cl2 167.57(9) . 2_655 ?
N5 Ni1 Cl2 89.72(9) . 2_655 ?
N3 Ni1 Cl2 87.18(9) . 2_655 ?
Cl1 Ni1 Cl2 92.39(3) . 2_655 ?
Cl2 Ni1 Cl2 88.73(3) . 2_655 ?
Ni1 Cl2 Ni1 91.27(3) . 2_655 ?
C19 O1 H1 109.5 . . ?
C20 O2 H2' 109.5 . . ?
C8 N1 C1 106.0(3) . . ?
C8 N1 Ni1 113.7(3) . . ?
C1 N1 Ni1 139.7(3) . . ?
C8 N2 C6 106.9(3) . . ?
C8 N2 C7 126.9(4) . . ?
C6 N2 C7 126.2(4) . . ?
C10 N3 C9 114.2(3) . . ?
C10 N3 Ni1 109.4(2) . . ?
C9 N3 Ni1 108.9(2) . . ?
C10 N3 H3' 112(3) . . ?
C9 N3 H3' 109(3) . . ?
Ni1 N3 H3' 103(3) . . ?
C11 N4 C13 106.9(3) . . ?
C11 N4 C12 127.5(4) . . ?
C13 N4 C12 125.6(4) . . ?
C11 N5 C18 106.4(3) . . ?
C11 N5 Ni1 113.3(2) . . ?
C18 N5 Ni1 139.7(2) . . ?
N1 C1 C2 130.0(4) . . ?
N1 C1 C6 108.7(4) . . ?
C2 C1 C6 121.3(4) . . ?
C3 C2 C1 117.1(5) . . ?
C3 C2 H2 122.9 . . ?
C1 C2 H2 120.0 . . ?
C2 C3 C4 121.1(5) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 118.6 . . ?
C5 C4 C3 121.4(5) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.1 . . ?
C4 C5 C6 118.3(5) . . ?
C4 C5 H5 122.0 . . ?
C6 C5 H5 119.7 . . ?
N2 C6 C5 133.2(4) . . ?
N2 C6 C1 106.0(4) . . ?
C5 C6 C1 120.8(5) . . ?
N2 C7 H7A 108.7 . . ?
N2 C7 H7B 109.8 . . ?
H7A C7 H7B 109.5 . . ?
N2 C7 H7C 109.8 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 N2 112.4(4) . . ?
N1 C8 C9 121.5(3) . . ?
N2 C8 C9 126.1(3) . . ?
N3 C9 C8 108.4(3) . . ?
N3 C9 H9A 110.0 . . ?
C8 C9 H9A 110.4 . . ?
N3 C9 H9B 108.7 . . ?
C8 C9 H9B 109.9 . . ?
H9A C9 H9B 109.5 . . ?
N3 C10 C11 109.8(3) . . ?
N3 C10 H10A 108.5 . . ?
C11 C10 H10A 109.3 . . ?
N3 C10 H10B 109.9 . . ?
C11 C10 H10B 109.8 . . ?
H10A C10 H10B 109.5 . . ?
N5 C11 N4 112.3(3) . . ?
N5 C11 C10 122.0(3) . . ?
N4 C11 C10 125.7(3) . . ?
N4 C12 H12A 109.0 . . ?
N4 C12 H12B 109.4 . . ?
H12A C12 H12B 109.5 . . ?
N4 C12 H12C 109.9 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 C14 132.0(4) . . ?
N4 C13 C18 106.0(3) . . ?
C14 C13 C18 121.9(4) . . ?
C15 C14 C13 116.3(4) . . ?
C15 C14 H14 123.3 . . ?
C13 C14 H14 120.4 . . ?
C14 C15 C16 122.1(4) . . ?
C14 C15 H15 118.5 . . ?
C16 C15 H15 119.3 . . ?
C17 C16 C15 121.4(5) . . ?
C17 C16 H16 121.1 . . ?
C15 C16 H16 117.5 . . ?
C18 C17 C16 117.5(4) . . ?
C18 C17 H17 119.8 . . ?
C16 C17 H17 122.7 . . ?
C17 C18 N5 130.9(3) . . ?
C17 C18 C13 120.7(4) . . ?
N5 C18 C13 108.4(3) . . ?
O1 C19 H19A 109.5 . . ?
O1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O2 C20 H20A 109.5 . . ?
O2 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O2 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 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
Ni1 N1 2.046(3) . ?
Ni1 N5 2.051(3) . ?
Ni1 N3 2.157(3) . ?
Ni1 Cl1 2.3809(9) . ?
Ni1 Cl2 2.4600(10) . ?
Ni1 Cl2 2.4651(10) 2_655 ?
Cl2 Ni1 2.4650(10) 2_655 ?
O1 C19 1.435(9) . ?
O1 H1 0.8200 . ?
O2 C20 1.517(13) . ?
O2 H2' 0.8200 . ?
N1 C8 1.312(5) . ?
N1 C1 1.386(5) . ?
N2 C8 1.365(5) . ?
N2 C6 1.371(6) . ?
N2 C7 1.467(5) . ?
N3 C10 1.475(5) . ?
N3 C9 1.477(5) . ?
N3 H3' 0.82(5) . ?
N4 C11 1.355(5) . ?
N4 C13 1.383(6) . ?
N4 C12 1.458(5) . ?
N5 C11 1.315(5) . ?
N5 C18 1.385(5) . ?
C1 C2 1.397(6) . ?
C1 C6 1.404(6) . ?
C2 C3 1.387(6) . ?
C2 H2 0.9594 . ?
C3 C4 1.421(8) . ?
C3 H3 0.9598 . ?
C4 C5 1.359(8) . ?
C4 H4 0.9608 . ?
C5 C6 1.393(7) . ?
C5 H5 0.9601 . ?
C7 H7A 0.9599 . ?
C7 H7B 0.9604 . ?
C7 H7C 0.9604 . ?
C8 C9 1.497(6) . ?
C9 H9A 0.9597 . ?
C9 H9B 0.9603 . ?
C10 C11 1.492(5) . ?
C10 H10A 0.9596 . ?
C10 H10B 0.9606 . ?
C12 H12A 0.9603 . ?
C12 H12B 0.9597 . ?
C12 H12C 0.9605 . ?
C13 C14 1.391(6) . ?
C13 C18 1.399(5) . ?
C14 C15 1.384(8) . ?
C14 H14 0.9595 . ?
C15 C16 1.384(7) . ?
C15 H15 0.9601 . ?
C16 C17 1.384(6) . ?
C16 H16 0.9603 . ?
C17 C18 1.384(6) . ?
C17 H17 0.9607 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
