#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/27/7012721.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_7012721
loop_
_publ_author_name
'Pavlishchuk, Vitaly V.'
'Kolotilov, Sergey V.'
'Addison, Anthony W.'
'Prushan, Michael J.'
'Schollmeyer, Dieter'
'Thompson, Laurence K.'
'Weyhermüller, Thomas'
'Goreshnik, Eugeny A.'
_publ_section_title
;
 Structural, magnetic and related attributes of some oximate-bridged
 tetranuclear nickel(ii) rhombs and a dinuclear congenerElectronic
 supplementary information (ESI) available: mass spectra, \cT vs. T,
 response of magnetic properties, low-lying spin levels and UV-VIS
 data. See http://www.rsc.org/suppdata/dt/b3/b300539a/
;
_journal_issue                   8
_journal_name_full               'Dalton Transactions'
_journal_page_first              1587
_journal_paper_doi               10.1039/b300539a
_journal_year                    2003
_chemical_formula_structural     '[C24 H50 N8 Ni4 O12]2+, 2 (ClO4)-, 0.6 H2O'
_chemical_formula_sum            'C24 H51.2 Cl2 N8 Ni4 O20.6'
_chemical_formula_weight         1087.27
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 111.50(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.7838(6)
_cell_length_b                   20.327(2)
_cell_length_c                   11.1143(9)
_cell_measurement_reflns_used    20067
_cell_measurement_temperature    100(2)
_cell_volume                     2056.6(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       '\391 images at 1 deg. in ω and 120 sec.'
_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  0.0655
_diffrn_reflns_av_sigmaI/netI    0.0589
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20067
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    2.020
_exptl_absorpt_correction_type   'not measured'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_description       'transparent block'
_exptl_crystal_F_000             1124
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.022
_refine_ls_goodness_of_fit_obs   1.066
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         5986
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_restrained_S_obs      1.066
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_obs          0.0379
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0308P)²+1.5692P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0927
_refine_ls_wR_factor_obs         0.0847
_reflns_number_observed          4691
_reflns_number_total             5995
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b300539a.txt
_cod_data_source_block           ST3784
_cod_depositor_comments
;
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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+1.5692P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+1.5692P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C24 H51.20 Cl2 N8 Ni4 O20.60'
_cod_database_code               7012721
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ni1 Ni -0.18364(3) -0.035388(13) 0.22430(3) 0.01394(8) Uani 1 d . .
Ni2 Ni 0.12203(3) 0.025327(13) 0.45594(3) 0.01297(8) Uani 1 d . .
N1 N -0.0472(2) -0.07382(10) 0.1315(2) 0.0209(4) Uani 1 d . .
H1A H 0.0359(2) -0.04993(10) 0.1541(2) 0.025 Uiso 1 calc R .
H1B H -0.0224(2) -0.11549(10) 0.1579(2) 0.025 Uiso 1 calc R .
C2 C -0.1227(3) -0.07262(13) -0.0118(2) 0.0244(5) Uani 1 d . .
H2A H -0.1633(3) -0.11571(13) -0.0422(2) 0.029 Uiso 1 calc R .
H2B H -0.0527(3) -0.06181(13) -0.0518(2) 0.029 Uiso 1 calc R .
C3 C -0.2452(3) -0.02176(12) -0.0495(2) 0.0242(5) Uani 1 d . .
H3A H -0.2030(3) 0.02205(12) -0.0374(2) 0.029 Uiso 1 calc R .
H3B H -0.3058(3) -0.02689(12) -0.1402(2) 0.029 Uiso 1 calc R .
O4 O -0.3332(2) -0.02899(7) 0.0262(2) 0.0182(3) Uani 1 d . .
C5 C -0.4295(3) -0.08644(12) -0.0071(2) 0.0212(5) Uani 1 d . .
H5A H -0.3863(3) -0.12097(12) -0.0419(2) 0.025 Uiso 1 calc R .
H5B H -0.5241(3) -0.07483(12) -0.0717(2) 0.025 Uiso 1 calc R .
C6 C -0.4482(3) -0.10973(12) 0.1145(2) 0.0221(5) Uani 1 d . .
H6A H -0.4992(3) -0.07652(12) 0.1448(2) 0.026 Uiso 1 calc R .
H6B H -0.5063(3) -0.14972(12) 0.0971(2) 0.026 Uiso 1 calc R .
N7 N -0.3011(2) -0.12241(10) 0.2148(2) 0.0200(4) Uani 1 d . .
H7A H -0.2570(2) -0.15652(10) 0.1921(2) 0.024 Uiso 1 calc R .
H7B H -0.3083(2) -0.13132(10) 0.2916(2) 0.024 Uiso 1 calc R .
O11 O 0.2253(2) -0.02277(8) 0.3427(2) 0.0177(3) Uani 1 d . .
C12 C 0.3173(2) -0.06376(11) 0.4089(2) 0.0172(4) Uani 1 d . .
C13 C 0.3644(2) -0.06402(11) 0.5486(2) 0.0169(4) Uani 1 d . .
N14 N 0.2919(2) -0.02161(9) 0.5917(2) 0.0151(4) Uani 1 d . .
O15 O 0.3312(2) -0.01341(8) 0.71616(15) 0.0188(3) Uani 1 d . .
C16 C 0.3804(3) -0.11294(13) 0.3433(2) 0.0257(5) Uani 1 d . .
H16A H 0.3624(18) -0.15658(13) 0.3671(14) 0.038 Uiso 1 calc R .
H16B H 0.4843(4) -0.1060(6) 0.3696(14) 0.038 Uiso 1 calc R .
H16C H 0.3349(15) -0.1078(6) 0.2513(3) 0.038 Uiso 1 calc R .
C17 C 0.4799(3) -0.10861(13) 0.6357(2) 0.0275(6) Uani 1 d . .
H17A H 0.5733(5) -0.0867(4) 0.6641(15) 0.041 Uiso 1 calc R .
H17B H 0.4850(15) -0.1479(4) 0.5895(6) 0.041 Uiso 1 calc R .
H17C H 0.4557(11) -0.1199(8) 0.7094(10) 0.041 Uiso 1 calc R .
O21 O 0.2365(2) 0.11535(7) 0.48883(15) 0.0170(3) Uani 1 d . .
C22 C 0.1733(2) 0.15750(11) 0.4052(2) 0.0164(4) Uani 1 d . .
C23 C 0.0395(2) 0.14091(10) 0.2973(2) 0.0167(4) Uani 1 d . .
N24 N -0.0009(2) 0.07969(9) 0.3006(2) 0.0148(4) Uani 1 d . .
O25 O -0.1132(2) 0.05737(8) 0.20336(15) 0.0186(3) Uani 1 d . .
C26 C 0.2373(3) 0.22463(11) 0.4147(2) 0.0225(5) Uani 1 d . .
H26A H 0.1724(10) 0.2560(2) 0.4304(18) 0.034 Uiso 1 calc R .
H26B H 0.2497(19) 0.2353(4) 0.3352(7) 0.034 Uiso 1 calc R .
H26C H 0.3309(10) 0.2259(3) 0.4846(12) 0.034 Uiso 1 calc R .
C27 C -0.0436(3) 0.18762(12) 0.1919(2) 0.0267(6) Uani 1 d . .
H27A H 0.0041(12) 0.1908(7) 0.1304(10) 0.040 Uiso 1 calc R .
H27B H -0.0461(18) 0.2302(3) 0.2283(3) 0.040 Uiso 1 calc R .
H27C H -0.1421(7) 0.1718(5) 0.1493(12) 0.040 Uiso 1 calc R .
O30 O -0.0347(2) -0.04686(8) 0.40814(15) 0.0143(3) Uani 1 d . .
H30 H -0.0030(29) -0.0820(14) 0.4148(26) 0.017 Uiso 1 d . .
Cl1X Cl 0.1000(4) -0.23528(13) 0.4277(5) 0.0327(8) Uani 0.299(4) d P 2
O41X O 0.1298(10) -0.2384(4) 0.5610(8) 0.050(2) Uani 0.299(4) d P 2
O45X O -0.1146(12) -0.2194(6) 0.1050(12) 0.084(4) Uiso 0.299(4) d P 2
Cl1 Cl 0.0591(2) -0.23053(5) 0.3559(2) 0.0307(4) Uani 0.701(4) d P 1
O41 O -0.0134(4) -0.2137(2) 0.2219(3) 0.0518(10) Uani 0.701(4) d P 1
O44 O 0.1873(3) -0.27233(10) 0.3751(3) 0.0514(7) Uani 1 d . .
O43 O 0.1084(3) -0.17023(11) 0.4163(3) 0.0619(8) Uani 1 d . .
O42 O -0.0435(3) -0.26397(13) 0.3901(3) 0.0710(9) Uani 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
_geom_angle_publ_flag
O30 Ni1 O25 94.16(6) . . ?
O30 Ni1 O15 93.48(6) . 3_556 ?
O25 Ni1 O15 84.11(7) . 3_556 ?
O30 Ni1 N7 97.54(7) . . ?
O25 Ni1 N7 166.88(7) . . ?
O15 Ni1 N7 89.24(8) 3_556 . ?
O30 Ni1 N1 95.70(7) . . ?
O25 Ni1 N1 89.20(7) . . ?
O15 Ni1 N1 169.00(7) 3_556 . ?
N7 Ni1 N1 95.53(8) . . ?
O30 Ni1 O4 175.92(6) . . ?
O25 Ni1 O4 87.65(6) . . ?
O15 Ni1 O4 90.33(6) 3_556 . ?
N7 Ni1 O4 81.07(7) . . ?
N1 Ni1 O4 80.65(7) . . ?
N14 Ni2 N24 163.13(8) . . ?
N14 Ni2 O30 90.08(7) . 3_556 ?
N24 Ni2 O30 103.59(7) . 3_556 ?
N14 Ni2 O30 100.82(7) . . ?
N24 Ni2 O30 90.88(7) . . ?
O30 Ni2 O30 82.45(7) 3_556 . ?
N14 Ni2 O21 92.34(7) . . ?
N24 Ni2 O21 77.68(7) . . ?
O30 Ni2 O21 91.46(6) 3_556 . ?
O30 Ni2 O21 165.46(6) . . ?
N14 Ni2 O11 77.63(7) . . ?
N24 Ni2 O11 90.50(7) . . ?
O30 Ni2 O11 163.79(6) 3_556 . ?
O30 Ni2 O11 89.44(6) . . ?
O21 Ni2 O11 99.48(6) . . ?
C2 N1 Ni1 111.14(14) . . ?
N1 C2 C3 109.8(2) . . ?
O4 C3 C2 110.8(2) . . ?
C3 O4 C5 114.1(2) . . ?
C3 O4 Ni1 106.31(13) . . ?
C5 O4 Ni1 110.12(13) . . ?
O4 C5 C6 107.7(2) . . ?
N7 C6 C5 109.0(2) . . ?
C6 N7 Ni1 104.75(14) . . ?
C12 O11 Ni2 110.80(15) . . ?
O11 C12 C13 120.8(2) . . ?
O11 C12 C16 119.7(2) . . ?
C13 C12 C16 119.5(2) . . ?
N14 C13 C12 112.7(2) . . ?
N14 C13 C17 122.9(2) . . ?
C12 C13 C17 124.4(2) . . ?
O15 N14 C13 118.8(2) . . ?
O15 N14 Ni2 124.89(14) . . ?
C13 N14 Ni2 116.27(15) . . ?
N14 O15 Ni1 115.82(12) . 3_556 ?
C22 O21 Ni2 112.34(14) . . ?
O21 C22 C23 120.3(2) . . ?
O21 C22 C26 119.7(2) . . ?
C23 C22 C26 119.9(2) . . ?
N24 C23 C22 112.8(2) . . ?
N24 C23 C27 122.8(2) . . ?
C22 C23 C27 124.4(2) . . ?
O25 N24 C23 118.5(2) . . ?
O25 N24 Ni2 124.74(13) . . ?
C23 N24 Ni2 116.71(14) . . ?
N24 O25 Ni1 116.17(12) . . ?
Ni2 O30 Ni1 112.22(7) 3_556 . ?
Ni2 O30 Ni2 97.55(7) 3_556 . ?
Ni1 O30 Ni2 111.70(7) . . ?
O43 Cl1X O41X 98.5(4) . . ?
O43 Cl1X O44 114.9(3) . . ?
O41X Cl1X O44 119.3(5) . . ?
O43 Cl1X O42 117.6(3) . . ?
O41X Cl1X O42 95.3(4) . . ?
O44 Cl1X O42 109.7(3) . . ?
O42 Cl1 O43 117.3(2) . . ?
O42 Cl1 O41 105.8(2) . . ?
O43 Cl1 O41 104.0(2) . . ?
O42 Cl1 O44 110.2(2) . . ?
O43 Cl1 O44 108.2(2) . . ?
O41 Cl1 O44 111.2(2) . . ?
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 O30 2.0421(15) . ?
Ni1 O25 2.050(2) . ?
Ni1 O15 2.051(2) 3_556 ?
Ni1 N7 2.091(2) . ?
Ni1 N1 2.113(2) . ?
Ni1 O4 2.155(2) . ?
Ni2 N14 2.028(2) . ?
Ni2 N24 2.032(2) . ?
Ni2 O30 2.037(2) 3_556 ?
Ni2 O30 2.047(2) . ?
Ni2 O21 2.106(2) . ?
Ni2 O11 2.120(2) . ?
N1 C2 1.490(3) . ?
C2 C3 1.520(4) . ?
C3 O4 1.415(3) . ?
O4 C5 1.461(3) . ?
C5 C6 1.505(3) . ?
C6 N7 1.485(3) . ?
O11 C12 1.249(3) . ?
C12 C13 1.449(3) . ?
C12 C16 1.497(3) . ?
C13 N14 1.313(3) . ?
C13 C17 1.494(3) . ?
N14 O15 1.303(2) . ?
O15 Ni1 2.051(2) 3_556 ?
O21 C22 1.249(3) . ?
C22 C23 1.454(3) . ?
C22 C26 1.489(3) . ?
C23 N24 1.310(3) . ?
C23 C27 1.495(3) . ?
N24 O25 1.308(2) . ?
O30 Ni2 2.037(2) 3_556 ?
Cl1X O43 1.334(3) . ?
Cl1X O41X 1.402(10) . ?
Cl1X O44 1.415(3) . ?
Cl1X O42 1.434(4) . ?
Cl1 O42 1.376(3) . ?
Cl1 O43 1.396(3) . ?
Cl1 O41 1.436(4) . ?
Cl1 O44 1.464(2) . ?
