#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:56:31 +0100 (vie 25 de mar de 2016) $
#$Revision: 179871 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/67/7016727.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_7016727
loop_
_publ_author_name
'Escuer, Albert'
'Vlahopoulou, Gina'
'Mautner, Franz A.'
_publ_section_title
;
 Use of 6-methylpyridine-2-carbaldehydeoxime in nickel(ii) carboxylate
 chemistry: synthetic, structural and magnetic properties of penta and
 hexanuclear complexes.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10109
_journal_page_last               10116
_journal_paper_doi               10.1039/c1dt10657k
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C54 H60 N12 Ni6 O18, 6(C H4 O), H2 O'
_chemical_formula_sum            'C60 H86 N12 Ni6 O25'
_chemical_formula_weight         1727.55
_chemical_name_common            (Ni6(6-mpko)6(ac)6)(MeOH)6.H2O
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   18.0582(8)
_cell_length_b                   18.0582(8)
_cell_length_c                   18.8851(9)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.69
_cell_volume                     5333.3(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXTL/PC
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker PII CCD'
_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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0113
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            45816
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    1.643
_exptl_absorpt_correction_T_max  0.6916
_exptl_absorpt_correction_T_min  0.4777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2694
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.354
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.090
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         2682
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.202
_refine_ls_restrained_S_obs      1.106
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0306
_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)+(0.0394P)²+25.1442P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0956
_reflns_number_gt                2464
_reflns_number_total             2724
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10657k.txt
_cod_data_source_block           TZ368B
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
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        5333.3(5)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7016727
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.83079(2) 0.86602(2) 0.049820(14) 0.01551(10) Uani 1 1 d .
O1 O 0.94189(9) 0.85589(10) 0.05076(8) 0.0177(3) Uani 1 1 d .
O2 O 0.76486(10) 0.74643(10) 0.01058(9) 0.0221(3) Uani 1 1 d .
O3 O 0.71401(10) 0.86076(11) 0.04734(9) 0.0233(3) Uani 1 1 d .
O4 O 0.5951(2) 0.7465(2) 0.1402(2) 0.0727(9) Uani 1 1 d .
H4A H 0.6322 0.7765 0.1100 0.109 Uiso 1 1 calc R
O5 O 1.0000 1.0000 0.4344(11) 0.133(5) Uani 0.50 3 d S
H11 H 1.0000 1.0000 0.3909 0.186 Uiso 0.50 3 d S
H12 H 0.9494 0.9857 0.4471 0.186 Uiso 0.166667 1 d P
N1 N 0.81148(12) 0.83794(12) 0.16180(10) 0.0184(4) Uani 1 1 d .
N2 N 0.88509(11) 0.98628(11) 0.09011(10) 0.0166(4) Uani 1 1 d .
C1 C 0.78190(15) 0.76435(15) 0.19864(13) 0.0224(5) Uani 1 1 d .
C2 C 0.7894(2) 0.7643(2) 0.27246(13) 0.0281(5) Uani 1 1 d .
H2 H 0.7686 0.7118 0.29720 0.034 Uiso 1 1 calc R
C3 C 0.8269(2) 0.8403(2) 0.30916(13) 0.0311(5) Uani 1 1 d .
H3 H 0.8331 0.8409 0.35914 0.037 Uiso 1 1 calc R
C4 C 0.8555(2) 0.9162(2) 0.27194(13) 0.0269(5) Uani 1 1 d .
H4 H 0.8805 0.9695 0.29601 0.032 Uiso 1 1 calc R
C5 C 0.84695(14) 0.91236(14) 0.19866(12) 0.0204(4) Uani 1 1 d .
C6 C 0.88018(14) 0.99137(14) 0.15742(12) 0.0191(4) Uani 1 1 d .
H6 H 0.89753 1.04465 0.17988 0.023 Uiso 1 1 calc R
C7 C 0.7410(2) 0.6814(2) 0.15897(14) 0.0296(5) Uani 1 1 d .
H7A H 0.6927 0.6763 0.1313 0.044 Uiso 1 1 calc R
H7B H 0.7204 0.6339 0.1926 0.044 Uiso 1 1 calc R
H7C H 0.7830 0.6800 0.1271 0.044 Uiso 1 1 calc R
C8 C 0.69608(15) 0.9142(2) 0.02120(12) 0.0225(5) Uani 1 1 d .
C9 C 0.6050(2) 0.8962(2) 0.0299(2) 0.0333(6) Uani 1 1 d .
H9A H 0.6006 0.9231 0.0735 0.050 Uiso 1 1 calc R
H9B H 0.5660 0.8343 0.0324 0.050 Uiso 1 1 calc R
H9C H 0.5897 0.9197 -0.0107 0.050 Uiso 1 1 calc R
C10 C 0.5972(4) 0.7991(4) 0.1964(3) 0.091(2) Uani 1 1 d .
H10A H 0.6513 0.8212 0.2221 0.137 Uiso 1 1 calc R
H10B H 0.5494 0.7655 0.2287 0.137 Uiso 1 1 calc R
H10C H 0.5923 0.8469 0.1774 0.137 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'
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'
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 173.87(7) . .
O2 Ni1 O1 89.97(6) . 11_565
N2 Ni1 O1 90.50(7) . 11_565
O2 Ni1 O3 84.24(7) . .
N2 Ni1 O3 89.64(7) . .
O1 Ni1 O3 90.19(6) 11_565 .
O2 Ni1 O1 89.31(6) . .
N2 Ni1 O1 96.79(7) . .
O1 Ni1 O1 91.47(7) 11_565 .
O3 Ni1 O1 173.34(6) . .
O2 Ni1 N1 99.72(7) . .
N2 Ni1 N1 79.59(7) . .
O1 Ni1 N1 169.99(7) 11_565 .
O3 Ni1 N1 88.29(7) . .
O1 Ni1 N1 91.16(6) . .
N2 O1 Ni1 113.31(12) 2_765 12_655
N2 O1 Ni1 129.61(12) 2_765 .
Ni1 O1 Ni1 108.60(7) 12_655 .
C8 O2 Ni1 136.8(2) 12_655 .
C8 O3 Ni1 128.4(2) . .
C10 O4 H4A 109.5 . .
H11 O5 H12 106 . .
C1 N1 C5 118.0(2) . .
C1 N1 Ni1 132.3(2) . .
C5 N1 Ni1 109.19(14) . .
C6 N2 O1 118.9(2) . 3_675
C6 N2 Ni1 115.77(15) . .
O1 N2 Ni1 124.60(13) 3_675 .
N1 C1 C2 121.5(2) . .
N1 C1 C7 118.7(2) . .
C2 C1 C7 119.8(2) . .
C3 C2 C1 120.0(2) . .
C3 C2 H2 119.99 . .
C1 C2 H2 119.99 . .
C2 C3 C4 118.9(2) . .
C2 C3 H3 120.54 . .
C4 C3 H3 120.54 . .
C3 C4 C5 118.5(2) . .
C3 C4 H4 120.7 . .
C5 C4 H4 120.73 . .
N1 C5 C4 123.1(2) . .
N1 C5 C6 116.9(2) . .
C4 C5 C6 120.0(2) . .
N2 C6 C5 117.8(2) . .
N2 C6 H6 121.08 . .
C5 C6 H6 121.08 . .
C1 C7 H7A 109.47 . .
C1 C7 H7B 109.47 . .
H7A C7 H7B 109.5 . .
C1 C7 H7C 109.47 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
O2 C8 O3 126.3(2) 11_565 .
O2 C8 C9 116.3(2) 11_565 .
O3 C8 C9 117.3(2) . .
C8 C9 H9A 109.47 . .
C8 C9 H9B 109.47 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.47 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
O4 C10 H10A 109.5 . .
O4 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
O4 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O2 2.015(2) .
Ni1 N2 2.031(2) .
Ni1 O1 2.042(2) 11_565
Ni1 O3 2.063(2) .
Ni1 O1 2.104(2) .
Ni1 N1 2.162(2) .
O1 N2 1.353(2) 2_765
O1 Ni1 2.042(2) 12_655
O2 C8 1.249(3) 12_655
O3 C8 1.262(3) .
O4 C10 1.412(6) .
O4 H4A 0.84 .
O5 H11 0.82 .
O5 H12 0.85 .
N1 C1 1.351(3) .
N1 C5 1.356(3) .
N2 C6 1.281(3) .
N2 O1 1.353(2) 3_675
C1 C2 1.401(3) .
C1 C7 1.497(3) .
C2 C3 1.376(4) .
C2 H2 0.95 .
C3 C4 1.389(4) .
C3 H3 0.95 .
C4 C5 1.390(3) .
C4 H4 0.95 .
C5 C6 1.465(3) .
C6 H6 0.95 .
C7 H7A 0.98 .
C7 H7B 0.98 .
C7 H7C 0.98 .
C8 O2 1.249(3) 11_565
C8 C9 1.517(3) .
C9 H9A 0.98 .
C9 H9B 0.98 .
C9 H9C 0.98 .
C10 H10A 0.98 .
C10 H10B 0.98 .
C10 H10C 0.98 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
C5 N1 C1 C2 -1.7(3) .
C5 N1 C1 C7 178.8(2) .
N1 C1 C2 C3 0.6(4) .
C7 C1 C2 C3 -180.0(2) .
C1 C2 C3 C4 1.1(4) .
C2 C3 C4 C5 -1.5(4) .
C1 N1 C5 C4 1.3(3) .
C1 N1 C5 C6 178.7(2) .
C3 C4 C5 N1 0.3(4) .
C3 C4 C5 C6 -177.1(2) .
O1 N2 C6 C5 178.7(2) 3_675
N1 C5 C6 N2 -10.0(3) .
C4 C5 C6 N2 167.6(2) .
