#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:10:08 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180414 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/83/7208300.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_7208300
loop_
_publ_author_name
'Dul, Marie-Claire'
'Lescouëzec, Rodrigue'
'Chamoreau, Lise-Marie'
'Journaux, Yves'
'Carrasco, Rosa'
'Castellano, María'
'Ruiz-García, Rafael'
'Cano, Joan'
'Lloret, Francesc'
'Julve, Miguel'
'Ruiz-Pérez, Catalina'
'Fabelo, Oscar'
'Pardo, Emilio'
_publ_section_title
;
 Self-assembly, metal binding ability, and magnetic properties of
 dinickel(ii) and dicobalt(ii) triple mesocates
;
_journal_issue                   17
_journal_name_full               CrystEngComm
_journal_page_first              5639
_journal_paper_doi               10.1039/c2ce25434d
_journal_volume                  14
_journal_year                    2012
_chemical_formula_sum            'C30 H42 N6 Na8 Ni2 O33'
_chemical_formula_weight         1316.04
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      176
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(15)
_cell_angle_beta                 90.000(18)
_cell_angle_gamma                120.000(19)
_cell_formula_units_Z            2
_cell_length_a                   12.606(3)
_cell_length_b                   12.606(3)
_cell_length_c                   19.668(4)
_cell_measurement_temperature    100(2)
_cell_volume                     2706.7(12)
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_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    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0768
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12800
_diffrn_reflns_theta_full        22.99
_diffrn_reflns_theta_max         22.99
_diffrn_reflns_theta_min         4.55
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.934
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         1284
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.1043
_refine_ls_R_factor_gt           0.0767
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0938P)²+12.4670P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1925
_refine_ls_wR_factor_ref         0.2140
_reflns_number_gt                966
_reflns_number_total             1284
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25434d.txt
_cod_data_source_block           compound_1
_cod_original_cell_volume        2706.8(10)
_cod_database_code               7208300
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, x, z+1/2'
'y, -x+y, z+1/2'
'-x, -y, -z'
'x, y, -z-1/2'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, -x, -z-1/2'
'-y, x-y, -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
Ni1 Ni 0.3333 0.6667 0.57657(7) 0.0407(6) Uani 1 3 d S
O1 O 0.4711(5) 0.6743(5) 0.5129(2) 0.0489(13) Uani 1 1 d .
O2 O 0.6275(5) 0.6406(6) 0.5196(3) 0.0645(16) Uani 1 1 d .
O3 O 0.5227(5) 0.4900(5) 0.6275(2) 0.0594(15) Uani 1 1 d .
N1 N 0.3751(5) 0.5486(5) 0.6266(3) 0.0397(14) Uani 1 1 d .
C1 C 0.5289(7) 0.6272(7) 0.5397(4) 0.0475(18) Uani 1 1 d .
C2 C 0.4700(7) 0.5472(6) 0.6045(4) 0.0446(18) Uani 1 1 d .
C3 C 0.3218(6) 0.4865(6) 0.6888(3) 0.0384(16) Uani 1 1 d .
C4 C 0.2107(7) 0.3803(6) 0.6889(4) 0.0464(18) Uani 1 1 d .
H4 H 0.1728 0.3435 0.6481 0.056 Uiso 1 1 calc R
C6 C 0.3773(9) 0.5368(10) 0.7500 0.041(2) Uani 1 2 d S
H6 H 0.4545 0.6066 0.7500 0.050 Uiso 1 2 calc SR
C5 C 0.1557(11) 0.3287(10) 0.7500 0.057(3) Uani 1 2 d S
H5 H 0.0797 0.2574 0.7500 0.068 Uiso 1 2 calc SR
Na1 Na 0.3117(4) 0.4897(4) 0.43253(17) 0.0771(12) Uani 1 1 d .
Na2 Na 0.8006(15) 0.8268(14) 0.4652(9) 0.124(5) Uani 0.33 1 d P
O1W O 0.3333 0.6667 0.3545(6) 0.089(4) Uani 1 3 d S
O2W O 0.1342(9) 0.3665(11) 0.3675(7) 0.182(6) Uani 1 1 d .
O3W O -0.127(8) -0.064(5) 0.341(5) 0.22(4) Uani 0.17 1 d P
O4W O 0.600(2) 0.476(2) 0.7500 0.237(13) Uani 1 2 d S
O5W O 0.1541(18) 0.351(2) 0.2500 0.212(9) Uani 1 2 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Na Na 0.0362 0.0249 '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
N1 Ni1 N1 99.09(19) 3_665 4_565
N1 Ni1 N1 99.09(19) 3_665 .
N1 Ni1 N1 99.09(19) 4_565 .
N1 Ni1 O1 79.3(2) 3_665 3_665
N1 Ni1 O1 93.7(2) 4_565 3_665
N1 Ni1 O1 167.2(2) . 3_665
N1 Ni1 O1 167.2(2) 3_665 4_565
N1 Ni1 O1 79.3(2) 4_565 4_565
N1 Ni1 O1 93.7(2) . 4_565
O1 Ni1 O1 88.16(19) 3_665 4_565
N1 Ni1 O1 93.7(2) 3_665 .
N1 Ni1 O1 167.2(2) 4_565 .
N1 Ni1 O1 79.3(2) . .
O1 Ni1 O1 88.16(19) 3_665 .
O1 Ni1 O1 88.16(19) 4_565 .
N1 Ni1 Na1 117.70(17) 3_665 4_565
N1 Ni1 Na1 83.89(16) 4_565 4_565
N1 Ni1 Na1 142.27(17) . 4_565
O1 Ni1 Na1 38.63(15) 3_665 4_565
O1 Ni1 Na1 49.63(15) 4_565 4_565
O1 Ni1 Na1 89.74(15) . 4_565
N1 Ni1 Na1 83.89(16) 3_665 3_665
N1 Ni1 Na1 142.27(17) 4_565 3_665
N1 Ni1 Na1 117.70(17) . 3_665
O1 Ni1 Na1 49.63(15) 3_665 3_665
O1 Ni1 Na1 89.74(15) 4_565 3_665
O1 Ni1 Na1 38.63(15) . 3_665
Na1 Ni1 Na1 62.26(11) 4_565 3_665
N1 Ni1 Na1 142.27(17) 3_665 .
N1 Ni1 Na1 117.70(17) 4_565 .
N1 Ni1 Na1 83.89(16) . .
O1 Ni1 Na1 89.74(15) 3_665 .
O1 Ni1 Na1 38.63(15) 4_565 .
O1 Ni1 Na1 49.63(15) . .
Na1 Ni1 Na1 62.26(11) 4_565 .
Na1 Ni1 Na1 62.26(11) 3_665 .
C1 O1 Ni1 112.7(4) . .
C1 O1 Na1 136.6(5) . 3_665
Ni1 O1 Na1 106.5(2) . 3_665
C1 O1 Na1 101.3(4) . .
Ni1 O1 Na1 93.90(19) . .
Na1 O1 Na1 93.6(2) 3_665 .
C1 O2 Na1 116.0(5) . 7_666
C1 O2 Na2 127.6(7) . .
Na1 O2 Na2 113.1(5) 7_666 .
C2 O3 Na1 116.9(5) . 7_666
C2 N1 C3 118.1(6) . .
C2 N1 Ni1 115.2(5) . .
C3 N1 Ni1 125.8(4) . .
O2 C1 O1 125.5(7) . .
O2 C1 C2 118.1(7) . .
O1 C1 C2 116.4(6) . .
O2 C1 Na1 42.9(4) . 7_666
O1 C1 Na1 165.4(5) . 7_666
C2 C1 Na1 76.1(4) . 7_666
N1 C2 O3 129.5(7) . .
N1 C2 C1 114.5(6) . .
O3 C2 C1 116.0(7) . .
N1 C2 Na1 170.8(5) . 7_666
O3 C2 Na1 41.4(4) . 7_666
C1 C2 Na1 74.6(4) . 7_666
C4 C3 C6 119.0(7) . .
C4 C3 N1 120.5(6) . .
C6 C3 N1 120.3(7) . .
C3 C4 C5 119.3(7) . .
C3 C6 C3 121.8(10) . 8_557
C4 C5 C4 121.5(10) 8_557 .
O3 Na1 O1 159.0(3) 7_666 4_565
O3 Na1 O2 71.7(2) 7_666 7_666
O1 Na1 O2 108.3(2) 4_565 7_666
O3 Na1 O2W 107.7(4) 7_666 .
O1 Na1 O2W 92.5(3) 4_565 .
O2 Na1 O2W 107.0(4) 7_666 .
O3 Na1 O1W 84.3(2) 7_666 .
O1 Na1 O1W 92.2(2) 4_565 .
O2 Na1 O1W 155.6(2) 7_666 .
O2W Na1 O1W 84.4(4) . .
O3 Na1 O1 87.8(2) 7_666 .
O1 Na1 O1 71.2(2) 4_565 .
O2 Na1 O1 90.3(2) 7_666 .
O2W Na1 O1 159.5(3) . .
O1W Na1 O1 83.8(2) . .
O3 Na1 C1 51.0(2) 7_666 7_666
O1 Na1 C1 125.6(2) 4_565 7_666
O2 Na1 C1 21.12(18) 7_666 7_666
O2W Na1 C1 114.3(3) . 7_666
O1W Na1 C1 134.4(2) . 7_666
O1 Na1 C1 85.77(19) . 7_666
O3 Na1 C2 21.68(19) 7_666 7_666
O1 Na1 C2 149.6(2) 4_565 7_666
O2 Na1 C2 50.2(2) 7_666 7_666
O2W Na1 C2 113.3(3) . 7_666
O1W Na1 C2 105.6(2) . 7_666
O1 Na1 C2 86.14(19) . 7_666
C1 Na1 C2 29.3(2) 7_666 7_666
O3 Na1 Ni1 124.2(2) 7_666 .
O1 Na1 Ni1 34.83(13) 4_565 .
O2 Na1 Ni1 99.91(17) 7_666 .
O2W Na1 Ni1 126.8(3) . .
O1W Na1 Ni1 89.4(2) . .
O1 Na1 Ni1 36.47(11) . .
C1 Na1 Ni1 107.32(16) 7_666 .
C2 Na1 Ni1 119.30(17) 7_666 .
O3 Na1 Na1 79.0(2) 7_666 3_665
O1 Na1 Na1 83.88(15) 4_565 3_665
O2 Na1 Na1 122.0(2) 7_666 3_665
O2W Na1 Na1 129.4(4) . 3_665
O1W Na1 Na1 45.56(16) . 3_665
O1 Na1 Na1 38.95(14) . 3_665
C1 Na1 Na1 108.2(2) 7_666 3_665
C2 Na1 Na1 91.2(2) 7_666 3_665
Ni1 Na1 Na1 58.87(5) . 3_665
O3 Na1 Na1 128.93(19) 7_666 4_565
O1 Na1 Na1 47.49(16) 4_565 4_565
O2 Na1 Na1 155.57(15) 7_666 4_565
O2W Na1 Na1 80.8(3) . 4_565
O1W Na1 Na1 45.56(15) . 4_565
O1 Na1 Na1 78.95(13) . 4_565
C1 Na1 Na1 164.66(19) 7_666 4_565
C2 Na1 Na1 148.4(2) 7_666 4_565
Ni1 Na1 Na1 58.87(5) . 4_565
Na1 Na1 Na1 60.000(2) 3_665 4_565
O3 Na1 Na2 125.6(3) 7_666 4_565
O1 Na1 Na2 72.7(3) 4_565 4_565
O2 Na1 Na2 74.4(3) 7_666 4_565
O2W Na1 Na2 46.2(5) . 4_565
O1W Na1 Na2 125.8(3) . 4_565
O1 Na1 Na2 133.7(3) . 4_565
C1 Na1 Na2 92.3(3) 7_666 4_565
C2 Na1 Na2 113.1(3) 7_666 4_565
Ni1 Na1 Na2 102.5(3) . 4_565
Na1 Na1 Na2 155.2(3) 3_665 4_565
Na1 Na1 Na2 97.1(3) 4_565 4_565
O2 Na2 O2W 81.4(5) . 3_665
O2 Na2 O3W 140(2) . 1_665
O2W Na2 O3W 61(2) 3_665 1_665
O2 Na2 Na2 92.7(9) . 10_656
O2W Na2 Na2 153.3(8) 3_665 10_656
O3W Na2 Na2 114.9(18) 1_665 10_656
O2 Na2 Na2 107.2(9) . 9_566
O2W Na2 Na2 109.4(7) 3_665 9_566
O3W Na2 Na2 97.4(14) 1_665 9_566
Na2 Na2 Na2 97.2(8) 10_656 9_566
O2 Na2 Na1 70.6(4) . 3_665
O2W Na2 Na1 39.7(3) 3_665 3_665
O3W Na2 Na1 86.1(17) 1_665 3_665
Na2 Na2 Na1 158.8(9) 10_656 3_665
Na2 Na2 Na1 76.4(5) 9_566 3_665
O2 Na2 Na1 32.0(3) . 7_666
O2W Na2 Na1 104.2(5) 3_665 7_666
O3W Na2 Na1 143.9(14) 1_665 7_666
Na2 Na2 Na1 62.5(6) 10_656 7_666
Na2 Na2 Na1 118.8(8) 9_566 7_666
Na1 Na2 Na1 102.5(3) 3_665 7_666
O2 Na2 Na2 148.6(6) . 4_675
O2W Na2 Na2 108.6(6) 3_665 4_675
O3W Na2 Na2 63.6(17) 1_665 4_675
Na2 Na2 Na2 90.000(7) 10_656 4_675
Na2 Na2 Na2 41.4(4) 9_566 4_675
Na1 Na2 Na2 97.6(6) 3_665 4_675
Na1 Na2 Na2 146.3(3) 7_666 4_675
O2 Na2 Na2 133.4(7) . 3_765
O2W Na2 Na2 133.8(4) 3_665 3_765
O3W Na2 Na2 75.6(18) 1_665 3_765
Na2 Na2 Na2 41.4(4) 10_656 3_765
Na2 Na2 Na2 90.000(6) 9_566 3_765
Na1 Na2 Na2 155.7(5) 3_665 3_765
Na1 Na2 Na2 101.7(6) 7_666 3_765
Na2 Na2 Na2 60.000(4) 4_675 3_765
Na1 O1W Na1 88.9(3) 4_565 3_665
Na1 O1W Na1 88.9(3) 4_565 .
Na1 O1W Na1 88.9(3) 3_665 .
Na1 O2W Na2 94.0(6) . 4_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 2.060(6) 3_665
Ni1 N1 2.060(6) 4_565
Ni1 N1 2.060(6) .
Ni1 O1 2.104(5) 3_665
Ni1 O1 2.104(5) 4_565
Ni1 O1 2.104(5) .
Ni1 Na1 3.531(4) 4_565
Ni1 Na1 3.531(4) 3_665
Ni1 Na1 3.531(4) .
O1 C1 1.263(9) .
O1 Na1 2.300(6) 3_665
O1 Na1 2.697(6) .
O2 C1 1.233(9) .
O2 Na1 2.330(7) 7_666
O2 Na2 2.508(16) .
O3 C2 1.283(9) .
O3 Na1 2.299(6) 7_666
N1 C2 1.281(9) .
N1 C3 1.427(8) .
C1 C2 1.563(11) .
C1 Na1 3.077(9) 7_666
C2 Na1 3.098(9) 7_666
C3 C4 1.370(10) .
C3 C6 1.377(9) .
C4 C5 1.377(9) .
C6 C3 1.377(8) 8_557
C5 C4 1.377(9) 8_557
Na1 O3 2.299(6) 7_666
Na1 O1 2.300(6) 4_565
Na1 O2 2.330(7) 7_666
Na1 O2W 2.362(9) .
Na1 O1W 2.608(8) .
Na1 C1 3.077(9) 7_666
Na1 C2 3.098(9) 7_666
Na1 Na1 3.651(7) 3_665
Na1 Na1 3.651(7) 4_565
Na1 Na2 3.686(19) 4_565
Na2 O2W 2.67(2) 3_665
Na2 O3W 2.73(8) 1_665
Na2 Na2 2.73(2) 10_656
Na2 Na2 2.73(2) 9_566
Na2 Na1 3.686(19) 3_665
Na2 Na1 4.039(16) 7_666
Na2 Na2 4.10(3) 4_675
Na2 Na2 4.10(3) 3_765
O1W Na1 2.608(8) 4_565
O1W Na1 2.608(8) 3_665
O2W Na2 2.67(2) 4_565
O3W Na2 2.73(8) 1_445
