#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:41:05 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178911 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/40/4114016.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_4114016
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 N12 Ni6 O24 Pr 3+, 3(Cl O4 -)'
_chemical_formula_sum            'C54 H72 Cl3 N12 Ni6 O36 Pr'
_chemical_formula_weight         2064.76
_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 fourier map'
_atom_sites_solution_primary     heavy
_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                   12.4276(12)
_cell_length_b                   12.4276(12)
_cell_length_c                   12.753(2)
_cell_measurement_reflns_used    2752
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.5
_cell_volume                     1705.8(4)
_computing_cell_refinement       'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.624 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)'
_computing_molecular_graphics    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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.051
_diffrn_reflns_av_sigmaI/netI    0.038
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11968
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.546
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS version 2.03 (Bruker, 2001)'
_exptl_crystal_colour            yellow-brown
_exptl_crystal_density_diffrn    2.010
_exptl_crystal_description       column
_exptl_crystal_F_000             1046
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.94
_refine_diff_density_min         -2.02
_refine_diff_density_rms         0.15
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2240
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0450
_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)+(0.075P)²+6.252P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1367
_reflns_number_gt                1730
_reflns_number_total             2744
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0341438si20030113_122949_05.cif
_cod_data_source_block           PRNI6L_complex5
_cod_database_code               4114016
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
Pr1 Pr 0.0000 0.0000 0.5000 0.0243(2) Uani 1 6 d S
Ni2 Ni 0.26572(6) 0.06795(7) 0.66306(6) 0.0248(2) Uani 1 1 d .
N1 N 0.3277(4) 0.1756(4) 0.7882(4) 0.0265(10) Uani 1 1 d .
N2 N 0.3810(4) 0.0018(4) 0.6563(4) 0.0280(10) Uani 1 1 d .
C1 C 0.2835(7) 0.3084(7) 0.9043(6) 0.0473(18) Uani 1 1 d .
H1A H 0.3626 0.3298 0.9380 0.071 Uiso 1 1 calc R
H1B H 0.2157 0.2661 0.9549 0.071 Uiso 1 1 calc R
H1C H 0.2861 0.3843 0.8796 0.071 Uiso 1 1 calc R
C2 C 0.1527(5) 0.1938(5) 0.7415(4) 0.0255(12) Uani 1 1 d .
C3 C 0.2626(5) 0.2254(5) 0.8144(5) 0.0296(12) Uani 1 1 d .
C4 C 0.4378(6) 0.1888(6) 0.8440(5) 0.0311(13) Uani 1 1 d .
H4A H 0.4347 0.2106 0.9182 0.037 Uiso 1 1 calc R
H4B H 0.5139 0.2575 0.8121 0.037 Uiso 1 1 calc R
C5 C 0.4446(6) 0.0714(7) 0.8397(5) 0.0406(15) Uani 1 1 d .
H5A H 0.3632 0.0022 0.8628 0.049 Uiso 1 1 calc R
H5B H 0.5068 0.0790 0.8921 0.049 Uiso 1 1 calc R
C6 C 0.4765(5) 0.0337(6) 0.7369(5) 0.0351(14) Uani 1 1 d .
H6A H 0.5564 0.1028 0.7110 0.042 Uiso 1 1 calc R
H6B H 0.4876 -0.0388 0.7490 0.042 Uiso 1 1 calc R
C7 C 0.3575(5) -0.0761(5) 0.5831(5) 0.0288(12) Uani 1 1 d .
C8 C 0.2496(5) -0.0958(5) 0.5102(4) 0.0249(11) Uani 1 1 d .
C9 C 0.4247(6) -0.1454(6) 0.5641(6) 0.0424(16) Uani 1 1 d .
H9A H 0.5123 -0.0931 0.5835 0.064 Uiso 1 1 calc R
H9B H 0.4188 -0.1673 0.4897 0.064 Uiso 1 1 calc R
H9C H 0.3873 -0.2213 0.6065 0.064 Uiso 1 1 calc R
O1 O 0.1524(4) -0.0868(4) 0.7604(3) 0.0327(9) Uani 1 1 d .
O2 O 0.3900(3) 0.2234(4) 0.5669(3) 0.0270(8) Uani 1 1 d .
O3 O 0.1382(3) 0.1213(3) 0.6639(3) 0.0249(8) Uani 1 1 d .
O4 O 0.1936(3) -0.0378(3) 0.5348(3) 0.0246(8) Uani 1 1 d .
Cl1 Cl 0.3333 -0.3333 0.8921(2) 0.0372(6) Uani 1 3 d SD
O20 O 0.3333 -0.3333 0.7804(7) 0.061(5) Uiso 0.50 3 d SPD
O20' O 0.300(3) -0.401(3) 0.7946(15) 0.062(9) Uiso 0.17 1 d PD
O21 O 0.3665(6) -0.2127(6) 0.9305(5) 0.0706(16) Uiso 1 1 d .
Cl2 Cl 0.0000 0.0000 1.0000 0.0804(17) Uani 1 6 d SD
O22 O 0.034(3) 0.035(3) 1.106(2) 0.051(9) Uiso 0.17 1 d P
O23 O -0.1163(15) -0.020(2) 1.0467(19) 0.164(9) Uiso 0.50 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'
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'
Cl Cl 0.1484 0.1585 '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'
Pr Pr -0.2180 2.8214 '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 Pr1 O3 180 . 4_556
O3 Pr1 O3 64.17(13) . 2
O3 Pr1 O3 115.83(13) 4_556 2
O3 Pr1 O4 118.37(11) . 3
O3 Pr1 O4 61.63(11) 4_556 3
O3 Pr1 O4 63.07(11) 2 3
O3 Pr1 O4 114.23(11) 6_556 3
O3 Pr1 O4 116.93(11) 5_556 3
O3 Pr1 O4 65.77(11) 3 3
O4 Pr1 O4 117.37(4) 3 2
O4 Pr1 O4 62.63(4) 3 5_556
O4 Pr1 O4 180 2 5_556
N1 Ni2 N2 101.5(2) . .
N1 Ni2 O3 82.87(17) . .
N2 Ni2 O3 175.08(18) . .
N1 Ni2 O4 175.90(17) . .
N2 Ni2 O4 82.64(18) . .
O3 Ni2 O4 93.04(15) . .
N1 Ni2 O1 89.93(18) . .
N2 Ni2 O1 86.52(18) . .
O3 Ni2 O1 91.19(16) . .
O4 Ni2 O1 90.39(16) . .
N1 Ni2 O2 89.45(17) . .
N2 Ni2 O2 90.23(17) . .
O3 Ni2 O2 92.15(15) . .
O4 Ni2 O2 90.48(15) . .
O1 Ni2 O2 176.50(15) . .
C3 N1 C4 126.4(5) . .
C3 N1 Ni2 114.3(4) . .
C4 N1 Ni2 119.3(4) . .
C7 N2 C6 124.6(5) . .
C7 N2 Ni2 114.3(4) . .
C6 N2 Ni2 120.9(4) . .
O1 C2 O3 125.4(5) 2 .
O1 C2 C3 118.4(5) 2 .
O3 C2 C3 116.1(5) . .
N1 C3 C1 127.3(6) . .
N1 C3 C2 114.5(5) . .
C1 C3 C2 118.3(5) . .
N1 C4 C5 111.9(5) . .
C4 C5 C6 118.9(6) . .
N2 C6 C5 113.0(5) . .
N2 C7 C9 125.4(6) . .
N2 C7 C8 114.4(5) . .
C9 C7 C8 120.2(5) . .
O2 C8 O4 124.9(5) 5_556 .
O2 C8 C7 119.0(5) 5_556 .
O4 C8 C7 116.2(5) . .
C2 O1 Ni2 120.3(4) 3 .
C8 O2 Ni2 118.0(3) 6_556 .
C2 O3 Ni2 112.2(3) . .
C2 O3 Pr1 146.0(3) . .
Ni2 O3 Pr1 101.70(14) . .
C8 O4 Ni2 112.4(3) . .
C8 O4 Pr1 147.9(3) . .
Ni2 O4 Pr1 99.48(14) . .
O20 Cl1 O21 110.0(3) . .
O21 Cl1 O21 108.9(3) . 2_545
O21 Cl1 O20' 88.0(15) 2_545 .
O21 Cl1 O20' 99.6(15) 3_655 .
O22 Cl2 O23 102(2) 6_557 3
O22 Cl2 O23 106(2) 5_557 3
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pr1 O3 2.647(4) .
Pr1 O4 2.708(4) .
Ni2 N1 1.975(5) .
Ni2 N2 1.978(5) .
Ni2 O3 2.000(4) .
Ni2 O4 2.007(4) .
Ni2 O1 2.125(4) .
Ni2 O2 2.153(4) .
N1 C3 1.283(7) .
N1 C4 1.478(7) .
N2 C7 1.270(8) .
N2 C6 1.467(7) .
C1 C3 1.475(8) .
C2 O1 1.229(7) 2
C2 O3 1.288(7) .
C2 C3 1.532(8) .
C4 C5 1.504(9) .
C5 C6 1.510(9) .
C7 C9 1.488(8) .
C7 C8 1.547(8) .
C8 O2 1.250(7) 5_556
C8 O4 1.267(7) .
Cl1 O20 1.424(9) .
Cl1 O21 1.428(6) .
Cl1 O20' 1.442(10) .
Cl2 O22 1.42(3) .
Cl2 O23 1.466(10) .
