#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:49:53 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179817 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/13/7011395.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_7011395
loop_
_publ_author_name
'Michaele J. Hardie'
'Nino Malic'
'Colin L. Raston'
_publ_section_title
;
 Mineralomimetic host--guest chemistry: the encapsulation of
 [M+⊂[2.2.2]cryptate] (M = Na, K) by saddle shaped Ni(II)
 macrocycles
;
_journal_issue                   3
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              295
_journal_page_last               296
_journal_paper_doi               10.1039/b111197n
_journal_year                    2002
_chemical_formula_sum            'C85 H114 B11 N14 Na Ni3 O6'
_chemical_formula_weight         1745.93
_chemical_name_common
{sodium[2.2.2]cryptate}{carborane}tris{Ni(TMTAA)}
_chemical_name_systematic
; 
{sodium 4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane}
{carbadodecaborane(12)}tris-{5,7,12,14-tetramethyldibenzo[b,i]-1,4,8,11,
tetraazacyclotetrdecinenickel(II)}
;
_space_group_IT_number           161
_symmetry_cell_setting           'trigonal (hexagonal)'
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_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            6
_cell_length_a                   18.0480(1)
_cell_length_b                   18.0480(1)
_cell_length_c                   45.4396(7)
_cell_measurement_temperature    123(2)
_cell_volume                     12818.1(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measurement_device_type  CCD
_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  0.035
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            28096
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    0.722
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5520
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.274(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         6810
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0355P)²+10.0022P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0694
_reflns_number_gt                6347
_reflns_number_total             6810
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b111197n.txt
_cod_data_source_block           c_2:
_cod_original_sg_symbol_H-M      R3c
_cod_database_code               7011395
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'-y, -x, z+1/2'
'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+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'-y+2/3, -x+1/3, z+5/6'
'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+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'
'-y+1/3, -x+2/3, z+7/6'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
B4 B 0.36532(13) 0.63263(13) 1.17121(5) 0.0242(4) Uani 0.92 1 d P . 1
H4 H 0.3864 0.6100 1.1907 0.029 Uiso 1 1 calc R . 1
B3 B 0.39739(16) 0.69814(14) 1.11314(5) 0.0252(5) Uani 0.92 1 d P . 1
H3 H 0.4406 0.7195 1.0935 0.030 Uiso 1 1 calc R . 1
B2 B 0.38501(12) 0.61257(12) 1.13480(5) 0.0216(4) Uani 0.92 1 d P . 1
H2 H 0.4194 0.5767 1.1299 0.026 Uiso 1 1 calc R . 1
B1 B 0.27885(12) 0.56032(13) 1.14875(6) 0.0214(4) Uani 0.92 1 d P . 1
H1 H 0.2427 0.4899 1.1533 0.026 Uiso 1 1 calc R . 1
C22 C 0.71259(11) 0.74766(11) 0.98636(4) 0.0227(3) Uani 1 1 d . . .
H22A H 0.7324 0.7479 0.9663 0.034 Uiso 1 1 calc R . .
H22B H 0.7561 0.7529 1.0004 0.034 Uiso 1 1 calc R . .
H22C H 0.7026 0.7959 0.9889 0.034 Uiso 1 1 calc R . .
C21 C 0.63013(10) 0.66474(10) 0.99181(3) 0.0160(3) Uani 1 1 d . . .
C20 C 0.57296(10) 0.66941(11) 1.01149(4) 0.0184(3) Uani 1 1 d . . .
H20 H 0.5910 0.7238 1.0201 0.022 Uiso 1 1 calc R . .
C19 C 0.44697(11) 0.62711(12) 1.04270(4) 0.0221(3) Uani 1 1 d . . .
H19A H 0.4560 0.6101 1.0623 0.033 Uiso 1 1 calc R . .
H19B H 0.3856 0.5977 1.0383 0.033 Uiso 1 1 calc R . .
H19C H 0.4700 0.6891 1.0423 0.033 Uiso 1 1 calc R . .
C18 C 0.49226(10) 0.60307(10) 1.01990(3) 0.0168(3) Uani 1 1 d . . .
C17 C 0.37916(10) 0.45407(10) 1.01629(4) 0.0165(3) Uani 1 1 d . . .
C16 C 0.34355(11) 0.43807(12) 1.04455(4) 0.0227(3) Uani 1 1 d . . .
H16 H 0.3714 0.4790 1.0597 0.027 Uiso 1 1 calc R . .
C15 C 0.26803(12) 0.36299(13) 1.05053(4) 0.0272(4) Uani 1 1 d . . .
H15 H 0.2429 0.3538 1.0695 0.033 Uiso 1 1 calc R . .
C14 C 0.22922(11) 0.30135(12) 1.02889(4) 0.0257(4) Uani 1 1 d . . .
H14 H 0.1774 0.2500 1.0331 0.031 Uiso 1 1 calc R . .
C13 C 0.26548(11) 0.31409(11) 1.00111(4) 0.0222(3) Uani 1 1 d . . .
H13 H 0.2400 0.2701 0.9867 0.027 Uiso 1 1 calc R . .
C12 C 0.33912(10) 0.39091(10) 0.99408(4) 0.0168(3) Uani 1 1 d . . .
C11 C 0.25648(11) 0.31959(11) 0.93604(4) 0.0227(3) Uani 1 1 d . . .
H11A H 0.2236 0.3343 0.9496 0.034 Uiso 1 1 calc R . .
H11B H 0.2430 0.2606 0.9397 0.034 Uiso 1 1 calc R . .
H11C H 0.2415 0.3248 0.9157 0.034 Uiso 1 1 calc R . .
C10 C 0.35139(10) 0.37997(10) 0.94085(4) 0.0169(3) Uani 1 1 d . . .
C9 C 0.40151(10) 0.40035(10) 0.91558(4) 0.0187(3) Uani 1 1 d . . .
H9 H 0.3716 0.3816 0.8974 0.022 Uiso 1 1 calc R . .
C8 C 0.52862(11) 0.45537(11) 0.88348(4) 0.0230(4) Uani 1 1 d . . .
H8A H 0.5338 0.4051 0.8788 0.034 Uiso 1 1 calc R . .
H8B H 0.5853 0.5068 0.8829 0.034 Uiso 1 1 calc R . .
H8C H 0.4912 0.4607 0.8690 0.034 Uiso 1 1 calc R . .
C7 C 0.49086(11) 0.44525(10) 0.91388(3) 0.0166(3) Uani 1 1 d . . .
C6 C 0.62873(10) 0.51705(10) 0.93843(3) 0.0161(3) Uani 1 1 d . . .
C5 C 0.67703(11) 0.49083(11) 0.92204(4) 0.0204(3) Uani 1 1 d . . .
H5 H 0.6498 0.4458 0.9081 0.024 Uiso 1 1 calc R . .
C4 C 0.76527(11) 0.53084(12) 0.92613(4) 0.0227(4) Uani 1 1 d . . .
H4A H 0.7985 0.5147 0.9144 0.027 Uiso 1 1 calc R . .
C3 C 0.80483(11) 0.59419(13) 0.94733(4) 0.0228(4) Uani 1 1 d . . .
H3A H 0.8650 0.6214 0.9500 0.027 Uiso 1 1 calc R . .
C2 C 0.75667(11) 0.61807(11) 0.96474(4) 0.0208(3) Uani 1 1 d . . .
H2A H 0.7836 0.6599 0.9797 0.025 Uiso 1 1 calc R . .
C1 C 0.66881(10) 0.58050(10) 0.96011(4) 0.0153(3) Uani 1 1 d . . .
N4 N 0.45696(9) 0.52581(9) 1.00719(3) 0.0153(3) Uani 1 1 d . . .
N3 N 0.38514(8) 0.41296(8) 0.96722(3) 0.0155(3) Uani 1 1 d . . .
N2 N 0.53888(9) 0.48011(9) 0.93792(3) 0.0153(3) Uani 1 1 d . . .
N1 N 0.61014(8) 0.59280(9) 0.97723(3) 0.0148(3) Uani 1 1 d . . .
Ni1 Ni 0.498017(12) 0.501826(13) 0.972830(7) 0.01253(5) Uani 1 1 d . . .
C28 C 0.41989(12) 0.72817(12) 0.96847(4) 0.0232(4) Uani 1 1 d . . .
H28A H 0.4231 0.7188 0.9898 0.028 Uiso 1 1 calc R . .
H28B H 0.4298 0.7869 0.9659 0.028 Uiso 1 1 calc R . .
C27 C 0.48988(12) 0.72121(13) 0.95284(4) 0.0258(4) Uani 1 1 d . . .
H27A H 0.5457 0.7593 0.9623 0.031 Uiso 1 1 calc R . .
H27B H 0.4787 0.6617 0.9539 0.031 Uiso 1 1 calc R . .
C26 C 0.55169(12) 0.73334(13) 0.90588(5) 0.0312(4) Uani 1 1 d . . .
H26A H 0.6008 0.7438 0.9184 0.037 Uiso 1 1 calc R . .
H26B H 0.5736 0.7753 0.8896 0.037 Uiso 1 1 calc R . .
C25 C 0.51096(13) 0.64429(13) 0.89351(5) 0.0331(4) Uani 1 1 d . . .
H25A H 0.5542 0.6375 0.8823 0.040 Uiso 1 1 calc R . .
H25B H 0.4906 0.6025 0.9099 0.040 Uiso 1 1 calc R . .
C24 C 0.46765(14) 0.66326(16) 0.84610(4) 0.0378(5) Uani 1 1 d . . .
H24A H 0.5051 0.6439 0.8372 0.045 Uiso 1 1 calc R . .
H24B H 0.5001 0.7265 0.8474 0.045 Uiso 1 1 calc R . .
C23 C 0.38833(16) 0.63417(16) 0.82756(5) 0.0399(5) Uani 1 1 d . . .
H23A H 0.4056 0.6540 0.8071 0.048 Uiso 1 1 calc R . .
H23B H 0.3553 0.5709 0.8273 0.048 Uiso 1 1 calc R . .
N6 N 0.3333 0.6667 0.95782(6) 0.0189(5) Uani 1 3 d S . .
N5 N 0.3333 0.6667 0.83851(7) 0.0317(7) Uani 1 3 d S . .
O2 O 0.49180(9) 0.74545(8) 0.92290(3) 0.0254(3) Uani 1 1 d . . .
O1 O 0.44083(9) 0.62694(9) 0.87473(3) 0.0308(3) Uani 1 1 d . . .
Na1 Na 0.3333 0.6667 0.89775(3) 0.0218(3) Uani 1 3 d S . .
C4A C 0.36532(13) 0.63263(13) 1.17121(5) 0.0242(4) Uani 0.08 1 d P . 2
C1A C 0.27885(12) 0.56032(13) 1.14875(6) 0.0214(4) Uani 0.08 1 d P . 2
C2A C 0.38501(12) 0.61257(12) 1.13480(5) 0.0216(4) Uani 0.08 1 d P . 2
C3A C 0.39739(16) 0.69814(14) 1.11314(5) 0.0252(5) Uani 0.08 1 d P . 2
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'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
B4 B2 1.767(3) . ?
B4 B1 1.773(3) . ?
B4 B1 1.779(3) 2_665 ?
B4 B4 1.788(4) 3_565 ?
B4 B4 1.788(4) 2_665 ?
B3 B3 1.734(4) 3_565 ?
B3 B3 1.734(4) 2_665 ?
B3 B2 1.744(3) 2_665 ?
B3 B1 1.748(3) 2_665 ?
B3 B2 1.749(3) . ?
B2 B3 1.744(3) 3_565 ?
B2 B1 1.774(3) 2_665 ?
B2 B1 1.776(3) . ?
B1 B3 1.748(3) 3_565 ?
B1 B2 1.774(3) 3_565 ?
B1 B4 1.779(3) 3_565 ?
C22 C21 1.513(2) . ?
C21 N1 1.336(2) . ?
C21 C20 1.400(2) . ?
C20 C18 1.399(2) . ?
C19 C18 1.512(2) . ?
C18 N4 1.340(2) . ?
C17 C16 1.400(2) . ?
C17 N4 1.415(2) . ?
C17 C12 1.420(2) . ?
C16 C15 1.386(3) . ?
C15 C14 1.384(3) . ?
C14 C13 1.387(3) . ?
