#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:28:59 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179972 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/66/7026610.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_7026610
loop_
_publ_author_name
'Kou, Hui-Zhong'
'An, Guang-Yu'
'Ji, Cong-Min'
'Wang, Bing-Wu'
'Cui, Ai-Li'
_publ_section_title
;
 Ferromagnetic coupling in oximato-bridged multi-decker Ni(II) clusters.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9604
_journal_page_last               9610
_journal_paper_doi               10.1039/c0dt00528b
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C44 H52 Cl2 N22 Ni4 O12'
_chemical_formula_weight         1386.82
_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                90.84(3)
_cell_angle_beta                 103.82(3)
_cell_angle_gamma                105.62(3)
_cell_formula_units_Z            1
_cell_length_a                   10.306(2)
_cell_length_b                   11.476(2)
_cell_length_c                   12.802(3)
_cell_measurement_reflns_used    3672
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      3.18
_cell_volume                     1410.9(6)
_computing_cell_refinement       'crystalstructure 3.6.0 (Rigaku, 2004)'
_computing_data_collection       'crystalstructure 3.6.0 (Rigaku, 2004)'
_computing_data_reduction        'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XP (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.77
_diffrn_measured_fraction_theta_full 0.883
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       'ω 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  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6619
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.18
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.488
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR; Higashi, 1995'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.050
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         4388
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0759P)²+0.5024P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1160
_reflns_number_gt                3672
_reflns_number_total             4388
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00528b.txt
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1410.9(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7026610
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
Ni1 Ni 0.94705(4) 0.32815(3) 0.02658(3) 0.02925(15) Uani 1 1 d .
Ni2 Ni 0.88618(4) 0.44748(4) 0.24545(3) 0.03232(15) Uani 1 1 d .
Cl1 Cl 0.76378(13) 0.81534(10) 0.47347(8) 0.0609(3) Uani 1 1 d .
N6 N 0.8290(3) 0.0981(3) 0.3070(2) 0.0447(7) Uani 1 1 d .
H6A H 0.8384 0.0602 0.2521 0.054 Uiso 1 1 calc R
H6B H 0.8117 0.0595 0.3614 0.054 Uiso 1 1 calc R
O2 O 0.8886(3) 0.2236(2) 0.14406(18) 0.0387(5) Uani 1 1 d .
N1 N 0.9371(3) 0.1788(2) -0.0730(2) 0.0329(6) Uani 1 1 d .
C1 C 0.9775(3) 0.2051(3) -0.1645(3) 0.0331(7) Uani 1 1 d .
N2 N 1.0101(3) 0.4068(2) -0.1018(2) 0.0325(6) Uani 1 1 d .
N5 N 0.8676(3) 0.2824(2) 0.2275(2) 0.0338(6) Uani 1 1 d .
N9 N 1.1576(3) 0.3511(3) 0.1074(2) 0.0407(7) Uani 1 1 d .
N7 N 0.7352(3) 0.3009(3) -0.0535(2) 0.0396(7) Uani 1 1 d .
N4 N 0.8325(3) 0.4069(3) 0.3746(2) 0.0388(7) Uani 1 1 d .
C6 C 1.0290(3) 0.3372(3) -0.1759(3) 0.0330(7) Uani 1 1 d .
C12 C 0.8414(3) 0.2190(3) 0.3079(3) 0.0359(7) Uani 1 1 d .
C7 C 0.8177(4) 0.2887(3) 0.3934(3) 0.0387(8) Uani 1 1 d .
C5 C 0.8802(4) 0.0634(3) -0.0586(3) 0.0379(8) Uani 1 1 d .
H5A H 0.8517 0.0453 0.0044 0.045 Uiso 1 1 calc R
C11 C 0.8103(5) 0.4802(4) 0.4472(3) 0.0526(10) Uani 1 1 d .
H11A H 0.8200 0.5614 0.4348 0.063 Uiso 1 1 calc R
C2 C 0.9639(4) 0.1149(3) -0.2436(3) 0.0420(8) Uani 1 1 d .
H2A H 0.9934 0.1345 -0.3060 0.050 Uiso 1 1 calc R
C18 C 1.3476(5) 0.3647(4) 0.2386(4) 0.0637(12) Uani 1 1 d .
H18A H 1.4061 0.3631 0.3059 0.076 Uiso 1 1 calc R
C13 C 0.6287(4) 0.2315(4) -0.0260(3) 0.0495(9) Uani 1 1 d .
H13A H 0.6340 0.1946 0.0385 0.059 Uiso 1 1 calc R
N8 N 0.5103(3) 0.2198(3) -0.1019(3) 0.0596(10) Uani 1 1 d .
C19 C 1.2061(4) 0.3408(4) 0.2144(3) 0.0538(10) Uani 1 1 d .
H19A H 1.1515 0.3207 0.2633 0.065 Uiso 1 1 calc R
C4 C 0.8621(4) -0.0307(3) -0.1345(3) 0.0439(8) Uani 1 1 d .
H4A H 0.8211 -0.1106 -0.1231 0.053 Uiso 1 1 calc R
C3 C 0.9057(4) -0.0043(3) -0.2270(3) 0.0462(9) Uani 1 1 d .
H3B H 0.8960 -0.0664 -0.2782 0.055 Uiso 1 1 calc R
C14 C 0.6817(4) 0.3360(4) -0.1535(3) 0.0549(10) Uani 1 1 d .
H14A H 0.7337 0.3869 -0.1937 0.066 Uiso 1 1 calc R
C17 C 1.2682(4) 0.3816(4) 0.0693(4) 0.0617(12) Uani 1 1 d .
H17A H 1.2676 0.3954 -0.0022 0.074 Uiso 1 1 calc R
C15 C 0.5449(5) 0.2861(5) -0.1840(4) 0.0674(13) Uani 1 1 d .
H15A H 0.4846 0.2947 -0.2484 0.081 Uiso 1 1 calc R
C10 C 0.7734(6) 0.4384(4) 0.5394(4) 0.0680(14) Uani 1 1 d .
H10A H 0.7588 0.4910 0.5886 0.082 Uiso 1 1 calc R
C9 C 0.7584(6) 0.3190(4) 0.5581(4) 0.0685(13) Uani 1 1 d .
H9A H 0.7323 0.2896 0.6196 0.082 Uiso 1 1 calc R
N10 N 1.3844(4) 0.3900(4) 0.1503(5) 0.0810(13) Uani 1 1 d .
C16 C 0.3709(5) 0.1447(6) -0.0982(5) 0.093(2) Uani 1 1 d .
H16A H 0.3772 0.1071 -0.0314 0.140 Uiso 1 1 calc R
H16B H 0.3356 0.0830 -0.1574 0.140 Uiso 1 1 calc R
H16C H 0.3091 0.1950 -0.1033 0.140 Uiso 1 1 calc R
O6 O 0.7755(5) 0.7894(5) 0.3699(3) 0.1050(15) Uani 1 1 d .
O5 O 0.8361(6) 0.7616(4) 0.5541(3) 0.1179(17) Uani 1 1 d .
C22 C 0.5241(6) -0.0642(6) -0.2517(6) 0.0838(16) Uani 1 1 d .
O4 O 0.7867(9) 0.9374(5) 0.4996(4) 0.167(3) Uani 1 1 d .
C8 C 0.7822(5) 0.2427(4) 0.4855(3) 0.0567(11) Uani 1 1 d .
H8A H 0.7746 0.1618 0.4980 0.068 Uiso 1 1 calc R
C20 C 1.5267(6) 0.4253(9) 0.1432(7) 0.133(3) Uani 1 1 d .
H20A H 1.5872 0.4249 0.2129 0.200 Uiso 1 1 calc R
H20B H 1.5486 0.5054 0.1190 0.200 Uiso 1 1 calc R
H20C H 1.5392 0.3690 0.0928 0.200 Uiso 1 1 calc R
O3 O 0.6208(7) 0.7633(9) 0.4697(6) 0.210(4) Uani 1 1 d .
C21 C 0.5509(7) 0.0073(7) -0.3418(6) 0.108(2) Uani 1 1 d .
N11 N 0.5056(6) -0.1184(8) -0.1822(6) 0.137(3) Uani 1 1 d .
N3 N 1.0851(3) 0.3862(3) -0.2544(2) 0.0408(7) Uani 1 1 d .
H3A H 1.1052 0.3460 -0.3026 0.049 Uiso 1 1 calc R
O1 O 1.0567(2) 0.52821(19) -0.12158(18) 0.0364(5) Uani 1 1 d .
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'
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'
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'
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
O2 Ni1 N2 170.28(10) . .
O2 Ni1 O1 85.83(9) . 2_765
N2 Ni1 O1 103.76(10) . 2_765
O2 Ni1 N1 93.24(10) . .
N2 Ni1 N1 77.27(10) . .
O1 Ni1 N1 176.36(10) 2_765 .
O2 Ni1 N9 89.22(11) . .
N2 Ni1 N9 89.24(12) . .
O1 Ni1 N9 90.05(11) 2_765 .
N1 Ni1 N9 93.45(11) . .
O2 Ni1 N7 89.76(12) . .
N2 Ni1 N7 91.62(12) . .
O1 Ni1 N7 90.74(11) 2_765 .
N1 Ni1 N7 85.73(11) . .
N9 Ni1 N7 178.66(11) . .
O1 Ni2 N3 84.20(11) 2_765 2_765
O1 Ni2 N5 90.79(11) 2_765 .
N3 Ni2 N5 174.73(11) 2_765 .
O1 Ni2 N4 173.96(12) 2_765 .
N3 Ni2 N4 101.35(12) 2_765 .
N5 Ni2 N4 83.59(12) . .
O4 Cl1 O5 112.3(3) . .
O4 Cl1 O6 113.4(3) . .
O5 Cl1 O6 115.1(3) . .
O4 Cl1 O3 104.2(5) . .
O5 Cl1 O3 105.5(4) . .
O6 Cl1 O3 105.0(4) . .
C12 N6 H6A 120.0 . .
C12 N6 H6B 120.0 . .
H6A N6 H6B 120.0 . .
N5 O2 Ni1 115.99(18) . .
C5 N1 C1 119.0(3) . .
C5 N1 Ni1 125.1(2) . .
C1 N1 Ni1 115.4(2) . .
N1 C1 C2 121.9(3) . .
N1 C1 C6 114.4(3) . .
C2 C1 C6 123.6(3) . .
C6 N2 O1 109.5(3) . .
C6 N2 Ni1 118.3(2) . .
O1 N2 Ni1 131.54(19) . .
C12 N5 O2 116.9(3) . .
C12 N5 Ni2 116.3(2) . .
O2 N5 Ni2 126.5(2) . .
C17 N9 C19 105.4(4) . .
C17 N9 Ni1 129.1(3) . .
C19 N9 Ni1 125.5(3) . .
C13 N7 C14 105.3(3) . .
C13 N7 Ni1 126.4(3) . .
C14 N7 Ni1 127.6(3) . .
C11 N4 C7 118.5(3) . .
C11 N4 Ni2 128.1(3) . .
C7 N4 Ni2 113.4(2) . .
N2 C6 N3 120.4(3) . .
N2 C6 C1 113.8(3) . .
N3 C6 C1 125.8(3) . .
N5 C12 N6 122.7(3) . .
N5 C12 C7 113.3(3) . .
N6 C12 C7 123.9(3) . .
N4 C7 C8 121.8(3) . .
N4 C7 C12 113.0(3) . .
C8 C7 C12 125.2(3) . .
N1 C5 C4 122.1(3) . .
N1 C5 H5A 118.9 . .
C4 C5 H5A 118.9 . .
N4 C11 C10 121.9(4) . .
N4 C11 H11A 119.1 . .
C10 C11 H11A 119.1 . .
C3 C2 C1 118.3(3) . .
C3 C2 H2A 120.9 . .
C1 C2 H2A 120.9 . .
N10 C18 C19 106.8(4) . .
N10 C18 H18A 126.6 . .
C19 C18 H18A 126.6 . .
N7 C13 N8 111.6(4) . .
N7 C13 H13A 124.2 . .
N8 C13 H13A 124.2 . .
C13 N8 C15 107.0(3) . .
C13 N8 C16 125.8(4) . .
C15 N8 C16 127.2(4) . .
N9 C19 C18 109.3(4) . .
N9 C19 H19A 125.4 . .
C18 C19 H19A 125.4 . .
C3 C4 C5 119.0(3) . .
C3 C4 H4A 120.5 . .
C5 C4 H4A 120.5 . .
C4 C3 C2 119.7(3) . .
C4 C3 H3B 120.1 . .
C2 C3 H3B 120.1 . .
C15 C14 N7 109.9(4) . .
C15 C14 H14A 125.0 . .
N7 C14 H14A 125.0 . .
N9 C17 N10 109.7(5) . .
N9 C17 H17A 125.1 . .
N10 C17 H17A 125.1 . .
C14 C15 N8 106.2(4) . .
C14 C15 H15A 126.9 . .
N8 C15 H15A 126.9 . .
C9 C10 C11 119.5(4) . .
C9 C10 H10A 120.3 . .
C11 C10 H10A 120.3 . .
C10 C9 C8 119.6(4) . .
C10 C9 H9A 120.2 . .
C8 C9 H9A 120.2 . .
C18 N10 C17 108.8(4) . .
C18 N10 C20 123.9(5) . .
C17 N10 C20 127.3(6) . .
N8 C16 H16A 109.5 . .
N8 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
N8 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
N11 C22 C21 179.1(7) . .
C9 C8 C7 118.7(4) . .
C9 C8 H8A 120.6 . .
C7 C8 H8A 120.6 . .
N10 C20 H20A 109.5 . .
N10 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
N10 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
C6 N3 Ni2 110.6(2) . 2_765
C6 N3 H3A 124.7 . .
Ni2 N3 H3A 124.7 2_765 .
N2 O1 Ni2 114.87(17) . 2_765
N2 O1 Ni1 124.35(18) . 2_765
Ni2 O1 Ni1 120.69(11) 2_765 2_765
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O2 2.040(2) .
Ni1 N2 2.044(3) .
Ni1 O1 2.048(2) 2_765
Ni1 N1 2.086(3) .
Ni1 N9 2.112(3) .
Ni1 N7 2.114(3) .
Ni2 O1 1.819(2) 2_765
Ni2 N3 1.848(3) 2_765
Ni2 N5 1.857(3) .
Ni2 N4 1.891(3) .
Cl1 O4 1.379(5) .
Cl1 O5 1.379(4) .
Cl1 O6 1.395(3) .
Cl1 O3 1.422(6) .
N6 C12 1.358(5) .
N6 H6A 0.8600 .
N6 H6B 0.8600 .
O2 N5 1.346(3) .
N1 C5 1.331(4) .
N1 C1 1.347(4) .
C1 C2 1.393(4) .
C1 C6 1.487(5) .
N2 C6 1.313(4) .
N2 O1 1.395(3) .
N5 C12 1.307(4) .
N9 C17 1.310(5) .
N9 C19 1.359(5) .
N7 C13 1.298(5) .
N7 C14 1.379(5) .
N4 C11 1.344(5) .
N4 C7 1.355(5) .
C6 N3 1.335(4) .
C12 C7 1.451(5) .
C7 C8 1.388(5) .
C5 C4 1.385(5) .
C5 H5A 0.9300 .
C11 C10 1.380(6) .
C11 H11A 0.9300 .
C2 C3 1.380(5) .
C2 H2A 0.9300 .
C18 N10 1.289(7) .
C18 C19 1.365(6) .
C18 H18A 0.9300 .
C13 N8 1.339(5) .
C13 H13A 0.9300 .
N8 C15 1.366(6) .
N8 C16 1.476(6) .
C19 H19A 0.9300 .
C4 C3 1.374(5) .
C4 H4A 0.9300 .
C3 H3B 0.9300 .
C14 C15 1.328(6) .
C14 H14A 0.9300 .
C17 N10 1.364(6) .
C17 H17A 0.9300 .
C15 H15A 0.9300 .
C10 C9 1.368(7) .
C10 H10A 0.9300 .
C9 C8 1.375(6) .
C9 H9A 0.9300 .
N10 C20 1.438(7) .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
C22 N11 1.117(8) .
C22 C21 1.463(9) .
C8 H8A 0.9300 .
C20 H20A 0.9600 .
C20 H20B 0.9600 .
C20 H20C 0.9600 .
N3 Ni2 1.848(3) 2_765
N3 H3A 0.8600 .
O1 Ni2 1.819(2) 2_765
O1 Ni1 2.048(2) 2_765
