#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:41:05 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178911 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/40/4114014.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_4114014
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_sum            'C54 H72 Cl3 La N12 Ni6 O36'
_chemical_formula_weight         2062.76
_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   'CH3 in delta F, CH2 placed geometrically'
_atom_sites_solution_primary     'Patterson methods'
_atom_sites_solution_secondary   'difference Fourier synthesis'
_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                   12.4549(11)
_cell_length_b                   12.4549(11)
_cell_length_c                   12.736(2)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      16.5
_cell_measurement_theta_min      12.5
_cell_volume                     1711.0(3)
_computing_cell_refinement       'STADI-4 (Stoe & Cie, 1996a)'
_computing_data_collection       'STADI-4 (Stoe & Cie, 1996a)'
_computing_data_reduction        'X-RED (Stoe & Cie, 1996b)'
_computing_molecular_graphics    'SHELXTL/PC (Version 5.03, Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Stoe Stadi-4 four-circle'
_diffrn_measurement_method       omega-theta
_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  0.140
_diffrn_reflns_av_sigmaI/netI    0.021
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2009
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.27
_diffrn_standards_decay_%        '4% random variation'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.450
_exptl_absorpt_correction_T_max  0.839
_exptl_absorpt_correction_T_min  0.700
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            'pale brown'
_exptl_crystal_density_diffrn    2.002
_exptl_crystal_description       column
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.04
_refine_diff_density_min         -1.53
_refine_diff_density_rms         0.19
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    'riding models'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         1988
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0748
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1542P)²+6.4074P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.205
_refine_ls_wR_factor_ref         0.226
_reflns_number_gt                1670
_reflns_number_total             1988
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0341438si20030113_122949_03.cif
_cod_data_source_block           ni6lan_complex3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1542P)^2^+6.4074P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1542P)^2^+6.4074P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4114014
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_calc_flag
_atom_site_refinement_flags
La La 0.0000 0.0000 0.5000 0.0404(4) Uani 1 d S
Ni Ni 0.06667(9) 0.26482(8) 0.66368(7) 0.0416(4) Uani 1 d .
C1 C 0.0698(9) 0.4451(9) 0.8403(7) 0.059(2) Uani 1 d .
H1A H 0.0782 0.5083 0.8919 0.071 Uiso 1 calc R
H1B H 0.0008 0.3644 0.8645 0.071 Uiso 1 calc R
C2A C 0.0323(8) 0.4754(7) 0.7365(6) 0.0509(18) Uani 1 d .
H2A1 H -0.0394 0.4877 0.7480 0.061 Uiso 1 calc R
H2A2 H 0.1017 0.5543 0.7097 0.061 Uiso 1 calc R
N3A N -0.0009(6) 0.3783(6) 0.6566(5) 0.0459(15) Uani 1 d .
C4A C -0.0771(7) 0.3560(7) 0.5839(6) 0.0442(16) Uani 1 d .
C5A C -0.0986(7) 0.2480(7) 0.5117(6) 0.0422(16) Uani 1 d .
O6A O -0.0393(5) 0.1921(5) 0.5360(4) 0.0443(12) Uani 1 d .
O7A O -0.1680(5) 0.2215(5) 0.4335(4) 0.0449(12) Uani 1 d .
C8A C -0.1463(8) 0.4238(8) 0.5624(7) 0.054(2) Uani 1 d .
H8A1 H -0.2101 0.4023 0.6163 0.082 Uiso 1 calc R
H8A2 H -0.1857 0.3999 0.4932 0.082 Uiso 1 calc R
H8A3 H -0.0884 0.5134 0.5638 0.082 Uiso 1 calc R
C2B C 0.1871(8) 0.4381(8) 0.8440(6) 0.0502(18) Uani 1 d .
H2B1 H 0.2554 0.5138 0.8116 0.060 Uiso 1 calc R
H2B2 H 0.2095 0.4355 0.9182 0.060 Uiso 1 calc R
N3B N 0.1744(6) 0.3276(6) 0.7884(5) 0.0452(14) Uani 1 d .
C4B C 0.2252(7) 0.2638(7) 0.8156(6) 0.0448(17) Uani 1 d .
C5B C 0.1937(7) 0.1535(7) 0.7428(6) 0.0454(17) Uani 1 d .
O6B O 0.1214(5) 0.1391(5) 0.6653(4) 0.0438(11) Uani 1 d .
O7B O 0.2378(5) 0.0865(5) 0.7618(4) 0.0492(13) Uani 1 d .
C8B C 0.3085(9) 0.2852(9) 0.9046(7) 0.058(2) Uani 1 d .
H8B1 H 0.3239 0.3603 0.9421 0.086 Uiso 1 calc R
H8B2 H 0.3871 0.2954 0.8787 0.086 Uiso 1 calc R
H8B3 H 0.2699 0.2141 0.9524 0.086 Uiso 1 calc R
Cl1 Cl -0.3333 0.3333 0.8931(3) 0.0553(9) Uani 1 d SDU
O1 O -0.4205(8) 0.2125(7) 0.9302(7) 0.090(2) Uani 1 d DU
O2 O -0.3333 0.3333 0.7867(9) 0.155(9) Uani 1 d SDU
Cl2 Cl 0.0000 0.0000 1.0000 0.096(2) Uani 1 d SDU
O3 O 0.0000 0.0000 0.8956(14) 0.129(13) Uani 0.50 d SPDU
O4 O -0.017(3) -0.109(2) 1.045(3) 0.199(16) Uani 0.50 d PDU
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'
La La -0.2871 2.4523 '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
_geom_angle_publ_flag
O6B La O6B 180.0 4_556 . ?
O6B La O6B 64.13(18) 4_556 6_556 ?
O6B La O6B 115.87(18) . 6_556 ?
O6B La O6A 118.02(16) 4_556 5_556 ?
O6B La O6A 61.98(16) . 5_556 y
O6B La O6A 62.75(15) 6_556 5_556 ?
O6B La O6A 65.58(16) 5_556 5_556 ?
O6B La O6A 117.25(15) 3 5_556 ?
O6B La O6A 114.42(16) 2 5_556 ?
O6A La O6A 117.19(6) 5_556 6_556 ?
O6A La O6A 62.81(6) 2 6_556 y
O6A La O6A 180.0 4_556 . ?
N3B Ni N3A 101.7(3) . . y
N3B Ni O6B 82.6(2) . . y
N3A Ni O6B 175.1(2) . . y
N3B Ni O6A 176.0(2) . . y
N3A Ni O6A 82.3(2) . . y
O6B Ni O6A 93.4(2) . . y
N3B Ni O7B 89.8(2) . 2 y
N3A Ni O7B 86.6(2) . 2 y
O6B Ni O7B 91.0(2) . 2 y
O6A Ni O7B 90.4(2) . 2 y
N3B Ni O7A 89.5(2) . 5_556 y
N3A Ni O7A 90.4(2) . 5_556 y
O6B Ni O7A 92.1(2) . 5_556 y
O6A Ni O7A 90.5(2) . 5_556 y
O7B Ni O7A 176.7(2) 2 5_556 y
C2B C1 C2A 118.1(8) . . ?
N3A C2A C1 113.2(7) . . ?
C4A N3A C2A 124.3(7) . . ?
C4A N3A Ni 114.9(5) . . ?
C2A N3A Ni 120.7(5) . . ?
N3A C4A C8A 126.4(7) . . ?
N3A C4A C5A 114.6(7) . . ?
C8A C4A C5A 119.0(7) . . ?
O7A C5A O6A 124.0(7) . . ?
O7A C5A C4A 120.1(7) . . ?
O6A C5A C4A 115.8(7) . . ?
C5A O6A Ni 112.3(5) . . ?
C5A O6A La 147.9(5) . . ?
Ni O6A La 99.7(2) . . ?
C5A O7A Ni 118.8(5) . 6_556 ?
N3B C2B C1 112.5(7) . . ?
C4B N3B C2B 126.0(7) . . ?
C4B N3B Ni 114.8(5) . . ?
C2B N3B Ni 119.2(5) . . ?
N3B C4B C8B 128.1(7) . . ?
N3B C4B C5B 113.9(7) . . ?
C8B C4B C5B 118.0(7) . . ?
O7B C5B O6B 125.0(7) . . ?
O7B C5B C4B 119.1(7) . . ?
O6B C5B C4B 115.9(7) . . ?
C5B O6B Ni 112.8(5) . . ?
C5B O6B La 145.8(5) . . ?
Ni O6B La 101.3(2) . . ?
C5B O7B Ni 120.8(5) . 3 ?
O2 Cl1 O1 109.3(4) . . ?
O1 Cl1 O1 109.6(4) 2_565 . ?
O3 Cl2 O4 114.3(15) . . ?
O4 Cl2 O4 104.2(18) 2 . ?
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
La O6B 2.665(5) . y
La O6A 2.710(5) . ?
Ni N3B 1.972(7) . y
Ni N3A 1.976(6) . y
Ni O6B 1.997(5) . y
Ni O6A 2.002(5) . y
Ni O7B 2.122(6) 2 y
Ni O7A 2.160(5) 5_556 y
C1 C2B 1.508(12) . ?
C1 C2A 1.511(13) . ?
C2A N3A 1.473(10) . ?
N3A C4A 1.254(10) . ?
C4A C8A 1.503(11) . ?
C4A C5A 1.538(10) . ?
C5A O7A 1.250(9) . ?
C5A O6A 1.281(9) . ?
C2B N3B 1.484(10) . ?
N3B C4B 1.286(10) . ?
C4B C8B 1.468(11) . ?
C4B C5B 1.536(11) . ?
C5B O7B 1.232(10) . ?
C5B O6B 1.286(10) . ?
Cl1 O2 1.355(12) . ?
Cl1 O1 1.425(7) . ?
Cl2 O3 1.330(18) . ?
Cl2 O4 1.385(16) . ?
