#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:12:45 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179958 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/52/7025296.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_7025296
loop_
_publ_author_name
'Pardo, Emilio'
'Dul, Marie-Claire'
'Lescouëzec, Rodrigue'
'Chamoreau, Lise-Marie'
'Journaux, Yves'
'Pasán, Jorge'
'Ruiz-Pérez, Catalina'
'Julve, Miguel'
'Lloret, Francesc'
'Ruiz-García, Rafael'
'Cano, Joan'
_publ_section_title
;
 Variation of the ground spin state in homo- and hetero-octanuclear
 copper(ii) and nickel(ii) double-star complexes with a meso-helicate-type
 metallacryptand core
;
_journal_issue                   20
_journal_name_full               'Dalton Transactions'
_journal_page_first              4786
_journal_paper_doi               10.1039/b926709c
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C84 H150 Cl6 Cu6 N24 Na2 Ni2 O54'
_chemical_formula_weight         3119.58
_chemical_name_systematic
;
?
;
_space_group_IT_number           188
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P -6c 2'
_symmetry_space_group_name_H-M   'P -6 c 2'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   17.426(3)
_cell_length_b                   17.426(3)
_cell_length_c                   31.674(6)
_cell_measurement_temperature    293(2)
_cell_volume                     8330(3)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'MxCube (ESRF, 2006)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 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, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9.6
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Single-axis HUBER diffractometer'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_detector       'ADSC Q210r CCD (binned mode)'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_wavelength     0.72930
_diffrn_reflns_av_R_equivalents  0.0962
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            72097
_diffrn_reflns_theta_full        23.93
_diffrn_reflns_theta_max         23.93
_diffrn_reflns_theta_min         1.91
_diffrn_source                   synchrotron
_diffrn_source_type              'ESRF-CRG BM16'
_exptl_absorpt_coefficient_mu    1.148
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal prisms'
_exptl_crystal_F_000             3216
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.896
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.146
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.12(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         4112
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0970
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2465
_refine_ls_wR_factor_ref         0.2504
_reflns_number_gt                3833
_reflns_number_total             4112
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b926709c.txt
_cod_data_source_block           compound3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
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        8330(2)
_cod_original_sg_symbol_H-M      P-6c2
_cod_database_code               7025296
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, y, -z+1/2'
'-y, -x, -z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'-x+y, y, -z'
'x, x-y, -z'
'x, x-y, z+1/2'
'-y, x-y, z'
'-y, x-y, -z+1/2'
'-x+y, -x, -z+1/2'
'-x+y, -x, 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
C1 C 0.7751(5) 0.5067(4) 0.8870(2) 0.0470(16) Uani 1 1 d .
C2 C 0.8235(4) 0.5020(4) 0.8476(2) 0.0457(15) Uani 1 1 d .
C3 C 0.8158(4) 0.4168(4) 0.7883(2) 0.0408(14) Uani 1 1 d .
C4 C 0.7900(5) 0.4350(5) 0.7500 0.0392(18) Uani 1 2 d S
H4 H 0.7539 0.4602 0.7500 0.047 Uiso 1 2 calc SR
C5 C 0.8729(4) 0.3811(5) 0.7880(2) 0.0497(15) Uani 1 1 d .
H5 H 0.8913 0.3683 0.8132 0.060 Uiso 1 1 calc R
C6 C 0.9011(7) 0.3652(7) 0.7500 0.052(2) Uani 1 2 d S
H6 H 0.9401 0.3434 0.7500 0.062 Uiso 1 2 calc SR
C7 C 0.8442(14) 0.7075(13) 0.8173(9) 0.167(9) Uani 1 1 d .
H15A H 0.8360 0.6566 0.8017 0.251 Uiso 1 1 calc R
H15B H 0.8422 0.7493 0.7982 0.251 Uiso 1 1 calc R
H15C H 0.7980 0.6896 0.8379 0.251 Uiso 1 1 calc R
C8 C 1.0077(16) 0.7807(9) 0.8093(4) 0.150(8) Uani 1 1 d .
H14A H 1.0026 0.7308 0.7940 0.225 Uiso 1 1 calc R
H14B H 1.0626 0.8088 0.8246 0.225 Uiso 1 1 calc R
H14C H 1.0063 0.8222 0.7898 0.225 Uiso 1 1 calc R
C9 C 0.9461(15) 0.8290(9) 0.8636(5) 0.128(6) Uani 1 1 d .
H9A H 0.8913 0.8167 0.8773 0.154 Uiso 1 1 calc R
H9B H 0.9650 0.8796 0.8451 0.154 Uiso 1 1 calc R
C10 C 1.0190(12) 0.8478(8) 0.8973(5) 0.129(7) Uani 1 1 d .
H8A H 1.0753 0.8658 0.8835 0.155 Uiso 1 1 calc R
H8B H 1.0264 0.8949 0.9161 0.155 Uiso 1 1 calc R
C11 C 0.9218(11) 0.7512(7) 0.9547(4) 0.142(7) Uani 1 1 d .
H11A H 0.9046 0.6970 0.9696 0.213 Uiso 1 1 calc R
H11B H 0.8708 0.7481 0.9414 0.213 Uiso 1 1 calc R
H11C H 0.9470 0.7999 0.9742 0.213 Uiso 1 1 calc R
C12 C 1.0684(10) 0.7670(11) 0.9412(5) 0.146(8) Uani 1 1 d .
H7A H 1.0818 0.7997 0.9675 0.176 Uiso 1 1 calc R
H7B H 1.1191 0.7982 0.9227 0.176 Uiso 1 1 calc R
C13 C 1.0542(10) 0.6765(12) 0.9500(4) 0.148(7) Uani 1 1 d .
H10A H 1.1096 0.6801 0.9580 0.178 Uiso 1 1 calc R
H10B H 1.0122 0.6490 0.9729 0.178 Uiso 1 1 calc R
C14 C 1.0920(11) 0.6385(13) 0.8838(5) 0.135(6) Uani 1 1 d .
H13A H 1.1215 0.6985 0.8738 0.203 Uiso 1 1 calc R
H13B H 1.0693 0.5986 0.8603 0.203 Uiso 1 1 calc R
H13C H 1.1332 0.6279 0.8992 0.203 Uiso 1 1 calc R
C15 C 0.9741(10) 0.5348(10) 0.9257(5) 0.121(5) Uani 1 1 d .
H16A H 0.9259 0.5258 0.9437 0.181 Uiso 1 1 calc R
H16B H 1.0142 0.5228 0.9411 0.181 Uiso 1 1 calc R
H16C H 0.9513 0.4956 0.9019 0.181 Uiso 1 1 calc R
Cu1 Cu 0.94262(6) 0.66471(6) 0.88038(3) 0.0646(4) Uani 1 1 d .
N1 N 0.7808(3) 0.4284(3) 0.82627(15) 0.0399(12) Uani 1 1 d .
N2 N 0.9332(7) 0.7503(6) 0.8392(3) 0.087(2) Uani 1 1 d .
N3 N 0.9899(7) 0.7650(6) 0.9213(3) 0.106(4) Uani 1 1 d .
N4 N 1.0196(6) 0.6242(7) 0.9113(3) 0.100(3) Uani 1 1 d .
Ni1 Ni 0.6667 0.3333 0.85534(4) 0.0387(4) Uani 1 3 d S
O1 O 0.7038(3) 0.4402(3) 0.89691(15) 0.0490(11) Uani 1 1 d .
O2 O 0.8983(3) 0.5698(3) 0.83797(17) 0.0619(13) Uani 1 1 d .
O1W O 0.6059(3) 0.2118(5) 1.0000 0.0625(19) Uani 1 2 d S
O3 O 0.8139(4) 0.5787(3) 0.90754(18) 0.0661(15) Uani 1 1 d .
O4 O 1.2315(15) 0.9148(18) 0.8605(8) 0.227(7) Uani 0.67 1 d PD
O3W O 0.4292(4) 0.1197(5) 0.9701(2) 0.098(2) Uani 1 1 d .
O5 O 1.3064(18) 0.8525(15) 0.8828(8) 0.227(7) Uani 0.67 1 d PD
O2W O 0.9964(8) 0.6042(8) 0.7500 0.134(5) Uani 1 2 d S
O6 O 1.3764(16) 1.0048(19) 0.8727(10) 0.227(7) Uani 0.67 1 d PD
O7 O 1.2919(16) 0.9432(17) 0.9285(6) 0.227(7) Uani 0.67 1 d PD
O8 O 1.0761(11) 0.9922(12) 0.7500 0.173(11) Uani 0.80 2 d SP
O9 O 1.0000 1.0000 0.7932(6) 0.24(2) Uani 0.80 3 d SPD
O10 O 1.0447(4) 1.0893(8) 1.0000 0.25(2) Uani 0.80 2 d SPD
O11 O 1.0000 1.0000 1.0433(6) 0.60(9) Uani 0.80 3 d SPD
Na1 Na 0.6667 0.3333 0.95171(14) 0.0561(11) Uani 1 3 d S
Cl1 Cl 1.0000 1.0000 1.0000 0.0724(13) Uani 1 6 d SD
Cl2 Cl 1.0000 1.0000 0.7500 0.0798(15) Uani 1 6 d SD
Cl3 Cl 1.3027(3) 0.9331(4) 0.8868(3) 0.139(2) Uani 0.67 1 d PD
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'
Cu Cu 0.3201 1.2651 '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'
Na Na 0.0362 0.0249 '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'
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
O1 C1 O3 125.7(7) . .
O1 C1 C2 118.5(6) . .
O3 C1 C2 115.8(6) . .
O2 C2 N1 126.8(6) . .
O2 C2 C1 118.5(6) . .
N1 C2 C1 114.6(6) . .
C4 C3 N1 120.1(6) . .
C4 C3 C5 118.3(6) . .
N1 C3 C5 121.4(6) . .
C3 C4 C3 122.4(8) . 2_556
C6 C5 C3 119.7(6) . .
C5 C6 C5 121.5(9) . 2_556
N2 C9 C10 106.2(13) . .
N3 C10 C9 107.4(11) . .
N3 C12 C13 112.8(10) . .
N4 C13 C12 107.5(13) . .
O2 Cu1 N3 177.4(3) . .
O2 Cu1 N2 92.1(3) . .
N3 Cu1 N2 85.6(4) . .
O2 Cu1 N4 94.9(4) . .
N3 Cu1 N4 86.4(5) . .
N2 Cu1 N4 149.2(4) . .
O2 Cu1 O3 81.56(19) . .
N3 Cu1 O3 100.4(3) . .
N2 Cu1 O3 109.0(3) . .
N4 Cu1 O3 101.7(3) . .
C2 N1 C3 120.5(5) . .
C2 N1 Ni1 113.9(4) . .
C3 N1 Ni1 125.4(4) . .
C8 N2 C9 107.6(11) . .
C8 N2 C7 112.5(15) . .
C9 N2 C7 109.7(13) . .
C8 N2 Cu1 107.1(9) . .
C9 N2 Cu1 108.0(8) . .
C7 N2 Cu1 111.7(9) . .
C10 N3 C12 109.4(12) . .
C10 N3 C11 111.9(11) . .
C12 N3 C11 110.1(11) . .
C10 N3 Cu1 108.1(7) . .
C12 N3 Cu1 105.6(9) . .
C11 N3 Cu1 111.5(6) . .
C15 N4 C14 110.0(13) . .
C15 N4 C13 104.1(11) . .
C14 N4 C13 110.1(12) . .
C15 N4 Cu1 115.3(8) . .
C14 N4 Cu1 108.5(9) . .
C13 N4 Cu1 108.7(12) . .
N1 Ni1 N1 101.59(17) 12_665 .
N1 Ni1 N1 101.59(17) 12_665 9_655
N1 Ni1 N1 101.59(17) . 9_655
N1 Ni1 O1 79.73(18) 12_665 12_665
N1 Ni1 O1 93.0(2) . 12_665
N1 Ni1 O1 164.6(2) 9_655 12_665
N1 Ni1 O1 164.64(19) 12_665 .
N1 Ni1 O1 79.73(18) . .
N1 Ni1 O1 93.0(2) 9_655 .
O1 Ni1 O1 84.92(19) 12_665 .
N1 Ni1 O1 93.0(2) 12_665 9_655
N1 Ni1 O1 164.64(19) . 9_655
N1 Ni1 O1 79.73(18) 9_655 9_655
O1 Ni1 O1 84.92(19) 12_665 9_655
O1 Ni1 O1 84.92(19) . 9_655
N1 Ni1 Na1 116.52(13) 12_665 .
N1 Ni1 Na1 116.52(14) . .
N1 Ni1 Na1 116.52(13) 9_655 .
O1 Ni1 Na1 51.21(13) 12_665 .
O1 Ni1 Na1 51.21(13) . .
O1 Ni1 Na1 51.21(13) 9_655 .
C1 O1 Ni1 112.9(4) . .
C1 O1 Na1 131.7(4) . .
Ni1 O1 Na1 85.44(19) . .
C2 O2 Cu1 113.8(4) . .
Na1 O1W Na1 79.6(3) 3_667 .
C1 O3 Cu1 109.7(5) . .
O1 Na1 O1 72.9(2) 12_665 9_655
O1 Na1 O1 72.9(2) 12_665 .
O1 Na1 O1 72.9(2) 9_655 .
O1 Na1 O1W 97.28(15) 12_665 3_667
O1 Na1 O1W 170.01(18) 9_655 3_667
O1 Na1 O1W 106.59(15) . 3_667
O1 Na1 O1W 106.59(15) 12_665 .
O1 Na1 O1W 97.28(16) 9_655 .
O1 Na1 O1W 170.01(18) . .
O1W Na1 O1W 83.4(2) 3_667 .
O1 Na1 O1W 170.01(18) 12_665 7_557
O1 Na1 O1W 106.59(15) 9_655 7_557
O1 Na1 O1W 97.28(15) . 7_557
O1W Na1 O1W 83.4(2) 3_667 7_557
O1W Na1 O1W 83.4(2) . 7_557
O1 Na1 Ni1 43.35(14) 12_665 .
O1 Na1 Ni1 43.35(14) 9_655 .
O1 Na1 Ni1 43.35(14) . .
O1W Na1 Ni1 129.82(14) 3_667 .
O1W Na1 Ni1 129.82(14) . .
O1W Na1 Ni1 129.82(14) 7_557 .
O1 Na1 Na1 136.65(14) 12_665 3_667
O1 Na1 Na1 136.65(14) 9_655 3_667
O1 Na1 Na1 136.65(14) . 3_667
O1W Na1 Na1 50.18(14) 3_667 3_667
O1W Na1 Na1 50.18(14) . 3_667
O1W Na1 Na1 50.18(14) 7_557 3_667
Ni1 Na1 Na1 180.000(1) . 3_667
O10 Cl1 O10 119.999(9) 7_567 .
O10 Cl1 O10 120.000(5) 7_567 3_777
O10 Cl1 O10 120.001(5) . 3_777
O10 Cl1 O11 90.000(1) 7_567 3_777
O10 Cl1 O11 90.000(6) . 3_777
O10 Cl1 O11 90.000(6) 3_777 3_777
O10 Cl1 O11 90.000(1) 7_567 .
O10 Cl1 O11 90.000(6) . .
O10 Cl1 O11 90.000(6) 3_777 .
O11 Cl1 O11 180.00(2) 3_777 .
O9 Cl2 O9 180.000(16) . 2_556
O9 Cl2 O8 90.000(11) . .
O9 Cl2 O8 90.000(11) 2_556 .
O9 Cl2 O8 90.000(18) . 11_676
O9 Cl2 O8 90.000(18) 2_556 11_676
O8 Cl2 O8 120.000(8) . 11_676
O9 Cl2 O8 90.000(8) . 9_765
O9 Cl2 O8 90.000(8) 2_556 9_765
O8 Cl2 O8 120.000(9) . 9_765
O8 Cl2 O8 120.000(10) 11_676 9_765
O6 Cl3 O7 109.4(19) . .
O6 Cl3 O4 110.1(19) . .
O7 Cl3 O4 116.4(14) . .
O6 Cl3 O5 113(2) . .
O7 Cl3 O5 106.7(13) . .
O4 Cl3 O5 101.2(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.243(9) .
C1 O3 1.267(9) .
C1 C2 1.531(10) .
C2 O2 1.284(9) .
C2 N1 1.304(9) .
C3 C4 1.385(8) .
C3 N1 1.408(8) .
C3 C5 1.413(10) .
C4 C3 1.385(8) 2_556
C5 C6 1.379(9) .
C6 C5 1.379(9) 2_556
C7 N2 1.51(2) .
C8 N2 1.48(2) .
C9 N2 1.490(15) .
C9 C10 1.56(3) .
C10 N3 1.479(19) .
C11 N3 1.516(15) .
C12 N3 1.49(2) .
C12 C13 1.50(3) .
C13 N4 1.465(17) .
C14 N4 1.447(18) .
C15 N4 1.423(18) .
Cu1 O2 1.965(5) .
Cu1 N3 1.993(8) .
Cu1 N2 2.049(9) .
Cu1 N4 2.050(11) .
Cu1 O3 2.158(6) .
N1 Ni1 2.062(5) .
Ni1 N1 2.062(5) 12_665
Ni1 N1 2.062(5) 9_655
Ni1 O1 2.102(5) 12_665
Ni1 O1 2.102(5) .
Ni1 O1 2.102(5) 9_655
Ni1 Na1 3.052(5) .
O1 Na1 2.387(6) .
O1W Na1 2.389(7) 3_667
O1W Na1 2.389(7) .
O4 Cl3 1.392(15) .
O5 Cl3 1.443(16) .
O6 Cl3 1.344(16) .
O7 Cl3 1.358(16) .
O8 Cl2 1.400(16) .
O9 Cl2 1.367(18) .
O10 Cl1 1.348(12) .
O11 Cl1 1.373(19) .
Na1 O1 2.387(6) 12_665
Na1 O1 2.387(6) 9_655
Na1 O1W 2.389(7) 3_667
Na1 O1W 2.389(7) 7_557
Na1 Na1 3.059(9) 3_667
Cl1 O10 1.348(12) 7_567
Cl1 O10 1.348(12) 3_777
Cl1 O11 1.373(19) 3_777
Cl2 O9 1.367(18) 2_556
Cl2 O8 1.400(16) 11_676
Cl2 O8 1.400(16) 9_765
