#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:41:05 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178911 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/40/4114018.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_4114018
loop_
_publ_author_name
'Xiang Lin'
'Dan M. J. Doble'
'Alexander J. Blake'
'Andrew Harrison'
'Claire Wilson'
'Martin Schröder'
_publ_section_title
;
 Cationic Assembly of Metal Complex Aggregates: Structural Diversity,
 Solution Stability, and Magnetic Properties
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9476
_journal_page_last               9483
_journal_paper_doi               10.1021/ja0341438
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety
'2(C83 H117 N18 Na5 Ni9 O40), 2(C H4 O), 4(B F4)'
_chemical_formula_sum            'C85 H125 B2 F8 N18 Na5 Ni9 O42'
_chemical_formula_weight         2887.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           163
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2c'
_symmetry_space_group_name_H-M   'P -3 1 c'
_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                   16.9608(10)
_cell_length_b                   16.9608(10)
_cell_length_c                   24.7593(14)
_cell_measurement_reflns_used    15061
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.6
_cell_measurement_theta_min      2.4
_cell_volume                     6168.2(6)
_computing_cell_refinement       'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.054 (Bruker, 1998)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-97; PLATON (Spek, 2002)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area detector'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_av_sigmaI/netI    0.031
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            33443
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.65
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.456
_exptl_absorpt_correction_T_max  0.694
_exptl_absorpt_correction_T_min  0.556
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS version 2.03 (Bruker, 2001)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             2972
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.84
_refine_diff_density_min         -1.21
_refine_diff_density_rms         0.14
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.234
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         4985
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.234
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0731
_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)+(0.041P)²+54.99P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1751
_refine_ls_wR_factor_ref         0.2065
_reflns_number_gt                3681
_reflns_number_total             5254
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0341438si20030113_122949_07.cif
_cod_data_source_block           NINACL_complex7
_cod_original_cell_volume        6168.2(10)
_cod_database_code               4114018
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -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 0.22819(5) 0.46307(5) 0.40598(3) 0.0268(2) Uani 1 1 d .
Ni2 Ni 0.03623(7) 0.51811(4) 0.2500 0.0299(3) Uani 1 2 d S
Na1 Na 0.3333 0.6667 0.34180(17) 0.0338(10) Uani 1 3 d S
Na2 Na 0.25238(12) 0.5048(2) 0.2500 0.0308(8) Uani 1 2 d S
O0 O 0.3333 0.6667 0.2500 0.0128(16) Uani 1 6 d S
O1 O 0.2879(3) 0.3993(3) 0.3657(2) 0.0395(12) Uani 1 1 d .
O2 O 0.0285(3) 0.4229(3) 0.30477(19) 0.0372(11) Uani 1 1 d .
O3 O 0.1718(3) 0.4798(3) 0.33578(17) 0.0289(9) Uani 1 1 d .
O4 O 0.1224(3) 0.6300(3) 0.29742(17) 0.0302(10) Uani 1 1 d .
O5 O 0.1638(3) 0.5178(3) 0.45259(17) 0.0301(9) Uani 1 1 d .
O6 O 0.1660(3) 0.3319(7) 0.2500 0.075(3) Uani 1 2 d S
O7 O 0.3504(3) 0.5776(3) 0.40659(17) 0.0277(9) Uani 1 1 d .
N1 N 0.2796(4) 0.4446(4) 0.4760(2) 0.0311(12) Uani 1 1 d .
N2 N -0.0576(4) 0.5320(4) 0.2947(2) 0.0341(12) Uani 1 1 d .
N3 N 0.1110(4) 0.3426(4) 0.4053(2) 0.0333(12) Uani 1 1 d .
C1 C -0.0784(6) 0.6194(7) 0.3670(4) 0.060(3) Uani 1 1 d .
H1A H -0.1350 0.5642 0.3771 0.090 Uiso 1 1 calc R
H1B H -0.0930 0.6622 0.3493 0.090 Uiso 1 1 calc R
H1C H -0.0422 0.6478 0.3995 0.090 Uiso 1 1 calc R
C2 C -0.0252(5) 0.5950(5) 0.3292(3) 0.0345(15) Uani 1 1 d .
C3 C 0.0795(4) 0.6508(5) 0.3308(3) 0.0308(13) Uani 1 1 d .
C4 C -0.1569(5) 0.4744(6) 0.2872(3) 0.050(2) Uani 1 1 d .
C5 C -0.1824(8) 0.3824(10) 0.2715(6) 0.042(3) Uani 0.50 1 d P
C6 C 0.0882(5) 0.4206(4) 0.3329(2) 0.0312(14) Uani 1 1 d .
C7 C 0.0559(5) 0.3346(5) 0.3681(3) 0.0361(15) Uani 1 1 d .
C8 C -0.0345(6) 0.2529(6) 0.3540(3) 0.062(3) Uani 1 1 d .
H8A H -0.0457 0.2019 0.3776 0.093 Uiso 1 1 calc R
H8B H -0.0336 0.2360 0.3163 0.093 Uiso 1 1 calc R
H8C H -0.0830 0.2677 0.3590 0.093 Uiso 1 1 calc R
C9 C 0.0981(6) 0.2720(5) 0.4443(3) 0.0441(18) Uani 1 1 d .
H9A H 0.1344 0.2438 0.4331 0.053 Uiso 1 1 calc R
H9B H 0.0332 0.2239 0.4451 0.053 Uiso 1 1 calc R
C10 C 0.1277(5) 0.3134(5) 0.5005(3) 0.0425(17) Uani 1 1 d .
H10A H 0.0988 0.2636 0.5273 0.051 Uiso 1 1 calc R
H10B H 0.1033 0.3548 0.5067 0.051 Uiso 1 1 calc R
C11 C 0.2299(5) 0.3663(5) 0.5119(3) 0.0422(17) Uani 1 1 d .
H11A H 0.2398 0.3878 0.5498 0.051 Uiso 1 1 calc R
H11B H 0.2548 0.3248 0.5078 0.051 Uiso 1 1 calc R
C12 C 0.1829(4) 0.5989(4) 0.4453(2) 0.0267(12) Uani 1 1 d .
C13 C 0.1473(4) 0.6401(4) 0.4874(3) 0.0311(14) Uani 1 1 d .
C14 C 0.0982(5) 0.5869(5) 0.5362(3) 0.0392(16) Uani 1 1 d .
H14A H 0.0391 0.5837 0.5388 0.059 Uiso 1 1 calc R
H14B H 0.1344 0.6168 0.5685 0.059 Uiso 1 1 calc R
H14C H 0.0890 0.5252 0.5335 0.059 Uiso 1 1 calc R
C15 C 0.169(2) 0.257(2) 0.2756(14) 0.077(9) Uiso 0.33 1 d P
B1 B -0.6667 -0.3333 0.5888(6) 0.044(3) Uani 1 3 d S
F1 F -0.6667 -0.3333 0.5330(3) 0.061(2) Uani 1 3 d S
F2 F -0.7147(4) -0.2927(4) 0.6073(2) 0.0725(17) Uani 1 1 d .
C100 C 0.051(4) -0.009(5) 0.505(2) 0.071(17) Uiso 0.17 1 d PD
O100 O 0.087(2) 0.0538(19) 0.4612(11) 0.038(7) Uiso 0.17 1 d PD
C101 C 0.141(4) 0.151(4) 0.326(2) 0.055(13) Uiso 0.17 1 d P
O101 O 0.208(3) 0.195(3) 0.2840(17) 0.071(11) Uiso 0.17 1 d P
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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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'
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
O7 Ni1 N3 175.5(2) . .
O7 Ni1 N1 80.1(2) . .
N3 Ni1 N1 97.6(2) . .
O7 Ni1 O3 101.38(17) . .
N3 Ni1 O3 80.9(2) . .
N1 Ni1 O3 178.19(19) . .
O7 Ni1 O1 88.38(19) . .
N3 Ni1 O1 87.6(2) . .
N1 Ni1 O1 88.4(2) . .
O3 Ni1 O1 92.70(19) . .
O7 Ni1 O5 94.66(17) . .
N3 Ni1 O5 89.18(19) . .
N1 Ni1 O5 87.53(19) . .
O3 Ni1 O5 91.31(17) . .
O1 Ni1 O5 174.41(18) . .
N2 Ni2 N2 95.3(3) 6_565 .
N2 Ni2 O2 86.6(2) 6_565 .
N2 Ni2 O2 89.2(2) . .
O2 Ni2 O2 173.7(3) . 6_565
N2 Ni2 O4 79.78(19) 6_565 6_565
N2 Ni2 O4 174.9(2) . 6_565
O2 Ni2 O4 89.07(18) . 6_565
O2 Ni2 O4 94.79(18) . .
O2 Ni2 O4 89.07(18) 6_565 .
O4 Ni2 O4 105.2(2) 6_565 .
O0 Na1 O7 133.79(13) . .
O7 Na1 O7 77.4(2) 2_665 .
O7 Na1 O3 139.1(2) . 3_565
O0 Na1 O3 87.13(11) . .
O7 Na1 O3 70.05(14) 3_565 .
O7 Na1 O3 71.92(14) . .
O3 Na1 O3 119.75(2) . 2_665
O0 Na2 O4 94.31(14) . 2_665
O4 Na2 O4 171.4(3) 2_665 6_565
O0 Na2 O3 98.62(13) . 5
O4 Na2 O3 90.02(14) 2_665 5
O4 Na2 O3 88.69(14) 6_565 5
O3 Na2 O3 162.8(3) 5 .
O0 Na2 O6 180.00(19) . .
O4 Na2 O6 85.69(14) 2_665 .
O3 Na2 O6 81.38(13) . .
Na1 O0 Na1 180.0 . 4_665
Na1 O0 Na2 90.0 . 3_565
Na2 O0 Na2 120.0 3_565 .
C3 O1 Ni1 130.7(4) 2_665 .
C6 O2 Ni2 131.1(4) . .
C6 O3 Ni1 110.5(4) . .
C6 O3 Na2 113.4(4) . .
Ni1 O3 Na2 119.76(19) . .
C6 O3 Na1 156.4(4) . .
Ni1 O3 Na1 82.06(15) . .
Na2 O3 Na1 73.89(15) . .
C3 O4 Ni2 112.6(4) . .
C3 O4 Na2 120.2(4) . 3_565
Ni2 O4 Na2 114.44(18) . 3_565
C12 O5 Ni1 119.9(4) . .
C15 O6 C15 81(3) 5 .
C15 O6 Na2 139.6(14) 5 .
C15 O6 Na2 139.6(14) . .
C12 O7 Ni1 114.8(4) 2_665 .
C12 O7 Na1 140.8(4) 2_665 .
Ni1 O7 Na1 102.74(18) . .
C13 N1 C11 120.9(6) 2_665 .
C13 N1 Ni1 115.1(4) 2_665 .
C11 N1 Ni1 124.0(5) . .
C2 N2 C4 121.1(6) . .
C2 N2 Ni2 115.4(4) . .
C4 N2 Ni2 123.5(4) . .
C7 N3 C9 126.1(6) . .
C7 N3 Ni1 114.5(5) . .
C9 N3 Ni1 119.4(5) . .
N2 C2 C1 126.3(6) . .
N2 C2 C3 114.7(6) . .
C1 C2 C3 119.0(6) . .
O1 C3 O4 128.0(6) 3_565 .
O1 C3 C2 114.5(6) 3_565 .
O4 C3 C2 117.4(5) . .
C5 C4 N2 112.0(8) . .
C5 C4 C5 54.8(11) . 6_565
N2 C4 C5 112.3(7) . 6_565
C4 C5 C4 116.9(10) . 6_565
O2 C6 O3 127.8(6) . .
O2 C6 C7 115.7(6) . .
O3 C6 C7 116.5(6) . .
N3 C7 C8 128.5(7) . .
N3 C7 C6 114.4(6) . .
C8 C7 C6 117.1(7) . .
N3 C9 C10 110.1(6) . .
C9 C10 C11 117.0(6) . .
N1 C11 C10 113.0(6) . .
O7 C12 O5 126.6(6) 3_565 .
O7 C12 C13 116.3(5) 3_565 .
O5 C12 C13 117.0(5) . .
N1 C13 C14 126.2(6) 3_565 .
N1 C13 C12 113.6(6) 3_565 .
C14 C13 C12 120.2(6) . .
F1 B1 F2 109.4(7) . .
F2 B1 F2 109.5(7) . 3_445
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 2.035(6) .
Ni1 N3 2.016(6) .
Ni1 O1 2.071(5) .
Ni1 O3 2.071(4) .
Ni1 O5 2.098(4) .
Ni1 O7 2.011(4) .
Ni2 N2 2.047(5) 6_565
Ni2 N2 2.047(5) .
Ni2 O2 2.062(5) .
Ni2 O2 2.062(5) 6_565
Ni2 O4 2.084(4) 6_565
Ni2 O4 2.084(4) .
Na1 O0 2.273(4) .
Na1 O7 2.318(5) .
Na1 O3 2.982(4) .
Na1 Na2 3.290(4) .
Na2 O0 2.378(4) .
Na2 O4 2.413(4) 2_665
Na2 O3 2.445(4) .
Na2 O6 2.538(11) .
Na2 Na2 4.119(6) 3_565
O1 C3 1.248(8) 2_665
O2 C6 1.246(8) .
O3 C6 1.265(8) .
O4 C3 1.262(7) .
O5 C12 1.259(7) .
O6 C15 1.45(4) 5
O6 C15 1.45(4) .
O7 C12 1.256(7) 2_665
N1 C13 1.270(9) 2_665
N1 C11 1.465(8) .
N2 C2 1.261(9) .
N2 C4 1.475(8) .
N3 C7 1.270(9) .
N3 C9 1.468(9) .
C1 C2 1.495(10) .
C2 C3 1.540(9) .
C3 O1 1.248(8) 3_565
C4 C5 1.448(17) .
C4 C5 1.567(17) 6_565
C5 C4 1.567(17) 6_565
C6 C7 1.545(9) .
C7 C8 1.506(10) .
C9 C10 1.527(11) .
C10 C11 1.527(11) .
C12 O7 1.256(7) 3_565
C12 C13 1.537(8) .
C13 N1 1.270(9) 3_565
C13 C14 1.488(9) .
C15 O101 1.51(5) .
F1 B1 1.380(17) .
F2 B1 1.384(7) .
C100 O100 1.421(10) .
C101 O101 1.44(7) .
