#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:41:05 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178911 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/40/4114013.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_4114013
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         'C54 H72 Ba N12 Ni6 O24, C H4 O, 2(Cl O4)'
_chemical_formula_sum            'C55 H76 Ba Cl2 N12 Ni6 O33'
_chemical_formula_weight         1993.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   'geom and circular E-map'
_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            1
_cell_length_a                   12.5041(8)
_cell_length_b                   12.5041(8)
_cell_length_c                   12.8523(11)
_cell_measurement_reflns_used    2916
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      2.45
_cell_volume                     1740.3(2)
_computing_cell_refinement       'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.054 (Bruker, 1998)'
_computing_data_reduction        '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 0.976
_diffrn_measured_fraction_theta_max 0.898
_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  0.043
_diffrn_reflns_av_sigmaI/netI    0.048
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9380
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.72
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.322
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.785
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL XPREP version 5.1 (Bruker, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.902
_exptl_crystal_description       column
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.40
_refine_diff_density_rms         0.09
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2705
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0277
_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)+(0.0313P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0669
_reflns_number_gt                1977
_reflns_number_total             2713
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0341438si20030113_122949_02.cif
_cod_data_source_block           BANICX_complex2
_cod_database_code               4114013
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'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
Ba Ba 0.0000 0.0000 0.5000 0.01587(11) Uani 1 6 d S
Ni Ni 0.26719(3) 0.06946(3) 0.66368(3) 0.02054(11) Uani 1 1 d .
C1 C 0.1553(3) 0.1941(3) 0.7471(2) 0.0223(6) Uani 1 1 d .
C2 C 0.2675(3) 0.2263(3) 0.8185(2) 0.0234(6) Uani 1 1 d .
C3 C 0.2868(3) 0.3060(3) 0.9103(3) 0.0339(8) Uani 1 1 d .
H3A H 0.3653 0.3270 0.9438 0.051 Uiso 1 1 calc R
H3B H 0.2190 0.2618 0.9598 0.051 Uiso 1 1 calc R
H3C H 0.2887 0.3819 0.8879 0.051 Uiso 1 1 calc R
C4 C 0.4414(3) 0.1908(3) 0.8425(2) 0.0277(7) Uani 1 1 d .
H4A H 0.4414 0.2153 0.9157 0.033 Uiso 1 1 calc R
H4B H 0.5164 0.2571 0.8084 0.033 Uiso 1 1 calc R
C5 C 0.4453(3) 0.0715(3) 0.8397(2) 0.0298(7) Uani 1 1 d .
H5A H 0.3634 0.0039 0.8620 0.036 Uiso 1 1 calc R
H5B H 0.5058 0.0779 0.8926 0.036 Uiso 1 1 calc R
C6 C 0.4775(3) 0.0330(3) 0.7378(2) 0.0286(7) Uani 1 1 d .
H6A H 0.5568 0.1014 0.7115 0.034 Uiso 1 1 calc R
H6B H 0.4885 -0.0391 0.7502 0.034 Uiso 1 1 calc R
C7 C 0.4297(3) -0.1434(3) 0.5677(3) 0.0286(7) Uani 1 1 d .
H7A H 0.5184 -0.0857 0.5752 0.043 Uiso 1 1 calc R
H7B H 0.4127 -0.1783 0.4973 0.043 Uiso 1 1 calc R
H7C H 0.4035 -0.2101 0.6187 0.043 Uiso 1 1 calc R
C8 C 0.3604(3) -0.0768(3) 0.5855(2) 0.0213(6) Uani 1 1 d .
C9 C 0.2533(3) -0.0965(3) 0.5123(2) 0.0200(6) Uani 1 1 d .
N1 N 0.3812(2) 0.0007(2) 0.65854(18) 0.0224(5) Uani 1 1 d .
N2 N 0.3315(2) 0.1778(2) 0.78954(18) 0.0213(5) Uani 1 1 d .
O1 O 0.14963(18) -0.08598(18) 0.76868(16) 0.0254(5) Uani 1 1 d .
O2 O 0.39414(18) 0.22782(18) 0.56459(15) 0.0227(4) Uani 1 1 d .
O3 O 0.14440(18) 0.12706(17) 0.66995(15) 0.0214(4) Uani 1 1 d .
O4 O 0.19933(17) -0.03834(17) 0.53741(15) 0.0222(4) Uani 1 1 d .
C10 C 0.0000 0.0000 1.0290(19) 0.070(9) Uani 0.50 3 d SP
O5 O 0.011(2) -0.087(2) 1.0372(18) 0.108(9) Uani 0.17 1 d P
Cl1 Cl 0.3333 -0.3333 0.89498(11) 0.0334(3) Uani 1 3 d SD
O6 O 0.3333 -0.3333 0.7866(4) 0.101(2) Uani 1 3 d SD
O7 O 0.2131(2) -0.4182(2) 0.9327(2) 0.0619(8) Uani 1 1 d 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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ba Ba -0.3244 2.2819 '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
O3 Ba O3 180.0 . 4_556
O3 Ba O3 64.47(6) . 2
O3 Ba O3 115.53(6) . 5_556
O3 Ba O4 117.36(5) . 5_556
O3 Ba O4 62.64(5) 4_556 5_556
O3 Ba O4 114.64(5) 2 5_556
O3 Ba O4 65.36(5) 5_556 5_556
O3 Ba O4 61.89(6) 3 5_556
O3 Ba O4 118.11(6) . 3
O4 Ba O4 62.88(2) 5_556 3
O4 Ba O4 180.0 5_556 2
O4 Ba O4 117.12(2) 3 2
O3 Ni N1 176.33(9) . .
O3 Ni N2 81.08(9) . .
N1 Ni N2 100.70(10) . .
O3 Ni O4 97.57(8) . .
N1 Ni O4 80.65(9) . .
N2 Ni O4 178.64(9) . .
O3 Ni O1 89.96(8) . .
N1 Ni O1 86.90(9) . .
N2 Ni O1 88.12(8) . .
O4 Ni O1 91.78(8) . .
O3 Ni O2 92.14(8) . .
N1 Ni O2 91.09(9) . .
N2 Ni O2 89.65(8) . .
O4 Ni O2 90.51(8) . .
O1 Ni O2 176.67(7) . .
O1 C1 O3 125.9(3) 2 .
O1 C1 C2 119.3(3) 2 .
O3 C1 C2 114.9(3) . .
N2 C2 C3 128.4(3) . .
N2 C2 C1 113.9(3) . .
C3 C2 C1 117.7(3) . .
N2 C4 C5 111.6(2) . .
C4 C5 C6 118.4(3) . .
N1 C6 C5 111.9(2) . .
N1 C8 C7 125.6(3) . .
N1 C8 C9 113.4(2) . .
C7 C8 C9 121.0(3) . .
O2 C9 O4 125.7(3) 5_556 .
O2 C9 C8 119.2(2) 5_556 .
O4 C9 C8 115.0(2) . .
C8 N1 C6 122.9(3) . .
C8 N1 Ni 115.59(19) . .
C6 N1 Ni 121.42(19) . .
C2 N2 C4 125.9(3) . .
C2 N2 Ni 114.9(2) . .
C4 N2 Ni 119.16(19) . .
C1 O1 Ni 119.69(18) 3 .
C9 O2 Ni 118.10(18) 6_556 .
C1 O3 Ni 115.11(18) . .
C1 O3 Ba 145.43(18) . .
Ni O3 Ba 99.17(7) . .
C9 O4 Ni 115.30(18) . .
C9 O4 Ba 146.62(18) . .
Ni O4 Ba 97.89(7) . .
O6 Cl1 O7 109.91(14) . .
O7 Cl1 O7 109.03(14) . 2_545
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ba O3 2.7725(19) .
Ba O4 2.8050(19) .
Ni O3 1.9971(19) .
Ni N1 2.000(2) .
Ni N2 2.002(2) .
Ni O4 2.0067(19) .
Ni O1 2.214(2) .
Ni O2 2.218(2) .
C1 O1 1.244(3) 2
C1 O3 1.261(3) .
C1 C2 1.552(4) .
C2 N2 1.277(4) .
C2 C3 1.485(4) .
C4 N2 1.467(4) .
C4 C5 1.518(4) .
C5 C6 1.519(4) .
C6 N1 1.471(4) .
C7 C8 1.489(4) .
C8 N1 1.280(4) .
C8 C9 1.553(4) .
C9 O2 1.250(3) 5_556
C9 O4 1.257(3) .
O1 C1 1.244(3) 3
O2 C9 1.250(3) 6_556
C10 O5 1.44(3) 5_557
Cl1 O6 1.393(5) .
Cl1 O7 1.423(2) .
