#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:32:40 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180226 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/12/7111237.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7111237
loop_
_publ_author_name
'Karmakar, Tapan K.'
'Chandra, Swapan K.'
'Ribas, Joan'
'Mostafa, Golam'
'Lu, Tian H.'
'Ghosh, Barindra K.'
_publ_section_title
;
 Synthesis, structure and magnetism of a new dicubane-like ferromagnetic
 tetranuclear nickel cluster containing versatile azido-only bridges and a
 bis(bidentate) Schiff base blockerElectronic supplementary information
 (ESI) available: a plot of the reduced magnetisation (M/N??) vs. H for 1
 at 2 K. See http://www.rsc.org/suppdata/cc/b2/b205375f/
;
_journal_issue                   20
_journal_name_full               'Chemical Communications'
_journal_page_first              2364
_journal_paper_doi               10.1039/b205375f
_journal_year                    2002
_chemical_formula_moiety         'C52 H44 N32 Ni4, 2(H2 O)'
_chemical_formula_sum            'C52 H48 N32 Ni4 O2'
_chemical_formula_weight         1388.06
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 106.690(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.9364(9)
_cell_length_b                   17.7700(13)
_cell_length_c                   14.4261(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     3176.6(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'ORTEP-3 for windows (Farrugia,1997)'
_computing_publication_material  'Platon99 (Spek,1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18882
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    1.234
_exptl_absorpt_correction_T_max  0.9478
_exptl_absorpt_correction_T_min  0.7764
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         7116
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0869P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1299
_refine_ls_wR_factor_ref         0.1445
_reflns_number_gt                4788
_reflns_number_total             7116
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b205375fsup1.cif
_cod_data_source_block           Ni(II)dicubane
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z 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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7111237
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.54766(3) 0.14510(2) 0.94634(3) 0.03602(14) Uani 1 1 d . . .
Ni2 Ni 0.60976(3) -0.02990(2) 0.98135(3) 0.03608(14) Uani 1 1 d . . .
N1 N 0.4254(2) 0.21023(16) 0.86124(19) 0.0402(6) Uani 1 1 d . . .
N2 N 0.5772(2) 0.13681(16) 0.80909(19) 0.0394(6) Uani 1 1 d . . .
N3 N 0.6819(2) -0.03141(16) 0.87189(19) 0.0393(6) Uani 1 1 d . . .
N4 N 0.7543(2) -0.08360(16) 1.05052(19) 0.0402(6) Uani 1 1 d . . .
N5 N 0.6736(2) 0.07598(17) 1.02336(19) 0.0414(7) Uani 1 1 d . . .
N6 N 0.7650(3) 0.09029(18) 1.0263(2) 0.0495(7) Uani 1 1 d . . .
N7 N 0.8525(3) 0.1049(3) 1.0287(3) 0.0841(13) Uani 1 1 d . . .
N8 N 0.6393(3) 0.23821(19) 0.9996(2) 0.0543(8) Uani 1 1 d . . .
N9 N 0.6144(3) 0.2901(2) 1.0358(2) 0.0660(10) Uani 1 1 d . . .
N10 N 0.5930(6) 0.3445(3) 1.0728(4) 0.122(2) Uani 1 1 d . . .
N11 N 0.4685(2) 0.03564(15) 0.90984(19) 0.0350(6) Uani 1 1 d . . .
N12 N 0.4107(3) 0.0083(2) 0.8279(3) 0.0706(11) Uani 1 1 d . . .
N13 N 0.3581(3) -0.0188(3) 0.7516(3) 0.0762(12) Uani 1 1 d . . .
N14 N 0.4724(2) 0.13234(16) 1.0578(2) 0.0424(7) Uani 1 1 d . . .
N15 N 0.4782(3) 0.1640(2) 1.1293(3) 0.0674(11) Uani 1 1 d . . .
N16 N 0.4843(6) 0.1938(4) 1.2008(4) 0.156(3) Uani 1 1 d . . .
C1 C 0.3596(3) 0.2555(2) 0.8914(3) 0.0492(9) Uani 1 1 d . . .
H1 H 0.3638 0.2559 0.9568 0.059 Uiso 1 1 calc R . .
C2 C 0.2846(3) 0.3021(2) 0.8289(3) 0.0579(10) Uani 1 1 d . . .
H2 H 0.2406 0.3337 0.8524 0.069 Uiso 1 1 calc R . .
C3 C 0.2772(3) 0.3006(2) 0.7332(3) 0.0614(11) Uani 1 1 d . . .
H3 H 0.2263 0.3302 0.6900 0.074 Uiso 1 1 calc R . .
C4 C 0.3457(3) 0.2545(2) 0.6998(3) 0.0554(10) Uani 1 1 d . . .
H4 H 0.3416 0.2532 0.6344 0.066 Uiso 1 1 calc R . .
C5 C 0.4198(3) 0.21088(19) 0.7655(2) 0.0421(8) Uani 1 1 d . . .
C6 C 0.5025(3) 0.16447(19) 0.7394(2) 0.0411(8) Uani 1 1 d . . .
C7 C 0.4913(3) 0.1532(2) 0.6341(2) 0.0472(9) Uani 1 1 d . . .
C8 C 0.5612(4) 0.1872(3) 0.5909(3) 0.0718(13) Uani 1 1 d . . .
H8 H 0.6133 0.2207 0.6257 0.086 Uiso 1 1 calc R . .
C9 C 0.5533(5) 0.1712(3) 0.4951(4) 0.0937(18) Uani 1 1 d . . .
H9 H 0.6017 0.1930 0.4662 0.112 Uiso 1 1 calc R . .
C10 C 0.4753(6) 0.1237(3) 0.4426(3) 0.101(2) Uani 1 1 d . . .
H10 H 0.4703 0.1138 0.3781 0.121 Uiso 1 1 calc R . .
C11 C 0.4063(6) 0.0916(4) 0.4838(4) 0.113(2) Uani 1 1 d . . .
H11 H 0.3537 0.0587 0.4486 0.136 Uiso 1 1 calc R . .
C12 C 0.4135(5) 0.1078(3) 0.5805(3) 0.0830(15) Uani 1 1 d . . .
H12 H 0.3635 0.0868 0.6082 0.100 Uiso 1 1 calc R . .
C13 C 0.6644(3) 0.0918(2) 0.7890(2) 0.0451(8) Uani 1 1 d . . .
H13A H 0.7302 0.0995 0.8411 0.054 Uiso 1 1 calc R . .
H13B H 0.6770 0.1101 0.7298 0.054 Uiso 1 1 calc R . .
C14 C 0.6403(3) 0.0072(2) 0.7785(2) 0.0434(8) Uani 1 1 d . . .
H14A H 0.5630 -0.0005 0.7542 0.052 Uiso 1 1 calc R . .
H14B H 0.6734 -0.0141 0.7320 0.052 Uiso 1 1 calc R . .
C15 C 0.7721(3) -0.06748(19) 0.8913(2) 0.0389(7) Uani 1 1 d . . .
C16 C 0.8340(3) -0.0805(2) 0.8204(3) 0.0480(9) Uani 1 1 d . . .
C17 C 0.9182(4) -0.0344(3) 0.8164(3) 0.0759(14) Uani 1 1 d . . .
H17 H 0.9393 0.0053 0.8598 0.091 Uiso 1 1 calc R . .
C18 C 0.9716(4) -0.0478(4) 0.7465(4) 0.0982(19) Uani 1 1 d . . .
H18 H 1.0282 -0.0168 0.7428 0.118 Uiso 1 1 calc R . .
C19 C 0.9400(5) -0.1076(4) 0.6826(4) 0.0870(17) Uani 1 1 d . . .
H19 H 0.9751 -0.1161 0.6357 0.104 Uiso 1 1 calc R . .
C20 C 0.8597(5) -0.1530(3) 0.6878(3) 0.0813(16) Uani 1 1 d . . .
H20 H 0.8404 -0.1935 0.6455 0.098 Uiso 1 1 calc R . .
C21 C 0.8055(4) -0.1401(3) 0.7554(3) 0.0674(12) Uani 1 1 d . . .
H21 H 0.7489 -0.1717 0.7578 0.081 Uiso 1 1 calc R . .
C22 C 0.8155(3) -0.09701(19) 0.9918(2) 0.0410(8) Uani 1 1 d . . .
C23 C 0.9150(3) -0.1318(2) 1.0226(3) 0.0538(10) Uani 1 1 d . . .
H23 H 0.9559 -0.1400 0.9800 0.065 Uiso 1 1 calc R . .
C24 C 0.9529(3) -0.1542(2) 1.1189(3) 0.0619(11) Uani 1 1 d . . .
H24 H 1.0193 -0.1782 1.1414 0.074 Uiso 1 1 calc R . .
C25 C 0.8913(3) -0.1405(2) 1.1798(3) 0.0612(11) Uani 1 1 d . . .
H25 H 0.9153 -0.1546 1.2445 0.073 Uiso 1 1 calc R . .
C26 C 0.7917(3) -0.1050(2) 1.1427(3) 0.0498(9) Uani 1 1 d . . .
H26 H 0.7496 -0.0958 1.1841 0.060 Uiso 1 1 calc R . .
O1W1 O 0.6540(9) 0.5031(5) 1.0809(9) 0.153(4) Uani 0.50 1 d P A 1
H1W1 H 0.6814 0.4593 1.0765 0.183 Uiso 0.50 1 d P B 1
H2W1 H 0.6755 0.5124 1.1439 0.183 Uiso 0.50 1 d P C 1
O1W2 O 0.6252(15) 0.6019(10) 0.9289(13) 0.125(6) Uani 0.25 1 d P D 2
H1W2 H 0.6167 0.5584 0.9017 0.150 Uiso 0.25 1 d P E 2
H2W2 H 0.5762 0.6025 0.9612 0.150 Uiso 0.25 1 d P F 2
O1W3 O 0.3296(11) 0.3181(16) 1.1604(19) 0.186(12) Uani 0.25 1 d P G 3
H1W3 H 0.3614 0.2758 1.1608 0.223 Uiso 0.25 1 d P H 3
H2W3 H 0.2853 0.3109 1.1952 0.223 Uiso 0.25 1 d P I 3
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'
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
N8 Ni1 N1 91.84(13) . .
N8 Ni1 N5 89.80(12) . .
N1 Ni1 N5 175.79(10) . .
N8 Ni1 N14 98.30(12) . .
N1 Ni1 N14 94.07(11) . .
N5 Ni1 N14 89.53(11) . .
N8 Ni1 N2 99.53(12) . .
N1 Ni1 N2 78.24(11) . .
N5 Ni1 N2 97.67(11) . .
N14 Ni1 N2 160.77(12) . .
N8 Ni1 N11 170.34(12) . .
N1 Ni1 N11 97.48(11) . .
N5 Ni1 N11 81.07(11) . .
N14 Ni1 N11 78.60(10) . .
N2 Ni1 N11 84.90(10) . .
N3 Ni2 N5 90.33(11) . .
N3 Ni2 N4 79.52(11) . .
N5 Ni2 N4 92.77(11) . .
N3 Ni2 N11 176.07(11) . 3_657
N5 Ni2 N11 93.59(11) . 3_657
N4 Ni2 N11 100.32(10) . 3_657
N3 Ni2 N14 95.09(11) . 3_657
N5 Ni2 N14 172.92(11) . 3_657
N4 Ni2 N14 92.69(11) . 3_657
N11 Ni2 N14 80.99(11) 3_657 3_657
N3 Ni2 N11 98.55(10) . .
N5 Ni2 N11 82.05(11) . .
N4 Ni2 N11 174.49(11) . .
N11 Ni2 N11 81.96(10) 3_657 .
N14 Ni2 N11 92.62(11) 3_657 .
C1 N1 C5 118.2(3) . .
C1 N1 Ni1 126.8(2) . .
C5 N1 Ni1 114.7(2) . .
C6 N2 C13 120.1(3) . .
C6 N2 Ni1 114.1(2) . .
C13 N2 Ni1 124.8(2) . .
C15 N3 C14 120.1(3) . .
C15 N3 Ni2 115.0(2) . .
C14 N3 Ni2 124.8(2) . .
C26 N4 C22 118.1(3) . .
C26 N4 Ni2 128.8(2) . .
C22 N4 Ni2 113.1(2) . .
N6 N5 Ni2 120.6(2) . .
N6 N5 Ni1 120.3(2) . .
Ni2 N5 Ni1 101.18(12) . .
N7 N6 N5 179.2(5) . .
N9 N8 Ni1 127.5(3) . .
N8 N9 N10 177.2(6) . .
N12 N11 Ni2 112.8(2) . 3_657
N12 N11 Ni2 114.8(2) . .
Ni2 N11 Ni2 98.04(10) 3_657 .
N12 N11 Ni1 131.2(2) . .
Ni2 N11 Ni1 98.96(11) 3_657 .
Ni2 N11 Ni1 95.23(11) . .
N13 N12 N11 178.4(4) . .
N15 N14 Ni2 123.9(2) . 3_657
N15 N14 Ni1 134.2(3) . .
Ni2 N14 Ni1 101.32(12) 3_657 .
N16 N15 N14 178.6(6) . .
N1 C1 C2 122.7(3) . .
C3 C2 C1 118.6(4) . .
C2 C3 C4 120.0(4) . .
C5 C4 C3 118.7(4) . .
N1 C5 C4 121.8(3) . .
N1 C5 C6 114.9(3) . .
C4 C5 C6 123.3(3) . .
N2 C6 C5 116.9(3) . .
N2 C6 C7 125.3(3) . .
C5 C6 C7 117.7(3) . .
C12 C7 C8 118.9(4) . .
C12 C7 C6 120.1(4) . .
C8 C7 C6 121.1(4) . .
C7 C8 C9 119.5(5) . .
C10 C9 C8 120.7(5) . .
C11 C10 C9 119.9(5) . .
C10 C11 C12 119.6(6) . .
C7 C12 C11 121.3(5) . .
N2 C13 C14 113.9(3) . .
N3 C14 C13 110.9(3) . .
N3 C15 C16 124.1(3) . .
N3 C15 C22 116.8(3) . .
C16 C15 C22 119.2(3) . .
C17 C16 C21 118.9(4) . .
C17 C16 C15 121.6(4) . .
C21 C16 C15 119.4(4) . .
C16 C17 C18 119.3(5) . .
C19 C18 C17 119.8(5) . .
C20 C19 C18 120.8(4) . .
C19 C20 C21 120.2(5) . .
C20 C21 C16 121.0(5) . .
N4 C22 C23 122.8(3) . .
N4 C22 C15 115.3(3) . .
C23 C22 C15 121.7(3) . .
C22 C23 C24 118.6(4) . .
C25 C24 C23 119.2(4) . .
C24 C25 C26 118.6(4) . .
N4 C26 C25 122.8(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N8 2.052(3) .
Ni1 N1 2.057(3) .
Ni1 N5 2.087(3) .
Ni1 N14 2.117(3) .
Ni1 N2 2.127(3) .
Ni1 N11 2.191(3) .
Ni2 N3 2.053(3) .
Ni2 N5 2.074(3) .
Ni2 N4 2.081(3) .
Ni2 N11 2.101(2) 3_657
Ni2 N14 2.102(3) 3_657
Ni2 N11 2.162(3) .
N1 C1 1.332(4) .
N1 C5 1.362(4) .
N2 C6 1.276(4) .
N2 C13 1.477(4) .
N3 C15 1.290(4) .
N3 C14 1.469(4) .
N4 C26 1.334(4) .
N4 C22 1.337(4) .
N5 N6 1.199(4) .
N6 N7 1.151(5) .
N8 N9 1.150(5) .
N9 N10 1.176(6) .
N11 N12 1.297(5) .
N11 Ni2 2.101(2) 3_657
N12 N13 1.216(5) .
N14 N15 1.159(4) .
N14 Ni2 2.102(3) 3_657
N15 N16 1.142(5) .
C1 C2 1.391(5) .
C2 C3 1.356(6) .
C3 C4 1.390(6) .
C4 C5 1.377(5) .
C5 C6 1.483(5) .
C6 C7 1.497(4) .
C7 C12 1.348(6) .
C7 C8 1.377(6) .
C8 C9 1.387(6) .
C9 C10 1.366(8) .
C10 C11 1.336(8) .
C11 C12 1.400(7) .
C13 C14 1.534(5) .
C15 C16 1.486(5) .
C15 C22 1.491(5) .
C16 C17 1.379(6) .
C16 C21 1.392(6) .
C17 C18 1.397(6) .
C18 C19 1.390(8) .
C19 C20 1.334(8) .
C20 C21 1.375(6) .
C22 C23 1.381(5) .
C23 C24 1.391(5) .
C24 C25 1.367(6) .
C25 C26 1.397(5) .
