#------------------------------------------------------------------------------
#$Date: 2018-09-05 00:22:48 +0300 (Wed, 05 Sep 2018) $
#$Revision: 210434 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/10/38/7103828.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_7103828
loop_
_publ_author_name
'Amoroso, Angelo J.'
'Chung, Simon S. M.'
'Spencer, Douglas J. E.'
'Danks, Jonathan P.'
'Glenny, Mark W.'
'Blake, Alexander J.'
'Cooke, Paul A.'
'Wilson, Claire'
'Schröder, Martin'
_publ_section_title
;
 Pinwheel motifs: formation of unusual homo- and hetero-nuclear
 aggregates via bridging thiolates
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   16
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2020
_journal_page_last               2021
_journal_paper_doi               10.1039/b303851c
_journal_year                    2003
_chemical_absolute_configuration ad
_chemical_formula_sum            'C34 H65 B4 F16 N9 Ni6 S8'
_chemical_formula_weight         1555.93
_space_group_IT_number           211
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'I 4 2 3'
_symmetry_space_group_name_H-M   'I 4 3 2'
_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                90.00
_cell_formula_units_Z            12
_cell_length_a                   25.796(5)
_cell_length_b                   25.796(5)
_cell_length_c                   25.796(5)
_cell_measurement_reflns_used    34
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      13.5
_cell_measurement_theta_min      10
_cell_volume                     17166(6)
_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 (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      220(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.094
_diffrn_reflns_av_sigmaI/netI    0.108
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            4060
_diffrn_reflns_theta_full        22.54
_diffrn_reflns_theta_max         22.54
_diffrn_reflns_theta_min         2.74
_diffrn_standards_decay_%        'random variation +/-2.4'
_diffrn_standards_interval_time  '60 min'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.316
_exptl_absorpt_correction_T_max  0.697
_exptl_absorpt_correction_T_min  0.588
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       tablet
_exptl_crystal_F_000             9504
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.95
_refine_diff_density_min         -0.47
_refine_diff_density_rms         0.11
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.13
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         1899
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.15
_refine_ls_R_factor_all          0.103
_refine_ls_R_factor_gt           0.066
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0126P)²+262.3P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.113
_refine_ls_wR_factor_ref         0.129
_reflns_number_gt                1422
_reflns_number_total             1899
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303851c.txt
_cod_data_source_block           ni3pzs
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0126P)^2^+262.3P] 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^)+(0.0126P)^2^+262.3P] 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               7103828
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'x+1/2, z+1/2, -y+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'x+1/2, -z+1/2, y+1/2'
'z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni -0.42355(6) -0.15408(6) -0.60226(6) 0.0248(4) Uani 1 d . . .
Ni2 Ni -0.5000 -0.20259(13) -0.5000 0.0211(8) Uani 1 d S . .
Ni3 Ni -0.5000 -0.08537(12) -0.5000 0.0213(8) Uani 1 d S . .
N1 N -0.3576(4) -0.1238(4) -0.6200(4) 0.027(3) Uani 1 d U . .
C2 C -0.3521(6) -0.1316(5) -0.6772(5) 0.041(4) Uani 1 d U . .
H2A H -0.3154 -0.1313 -0.6871 0.049 Uiso 1 calc R . .
H2B H -0.3700 -0.1039 -0.6961 0.049 Uiso 1 calc R . .
C3 C -0.3766(6) -0.1841(5) -0.6896(5) 0.035(3) Uani 1 d U . .
H3A H -0.4074 -0.1795 -0.7112 0.042 Uiso 1 calc R . .
H3B H -0.3518 -0.2060 -0.7083 0.042 Uiso 1 calc R . .
N4 N -0.3906(4) -0.2081(5) -0.6405(4) 0.036(3) Uani 1 d U . .
C5 C -0.3419(5) -0.2164(5) -0.6099(6) 0.035(3) Uani 1 d U . .
H5A H -0.3162 -0.2352 -0.6306 0.042 Uiso 1 calc R . .
H5B H -0.3493 -0.2366 -0.5785 0.042 Uiso 1 calc R . .
C6 C -0.3210(5) -0.1609(5) -0.5950(6) 0.035(3) Uani 1 d U . .
H6A H -0.3208 -0.1563 -0.5573 0.042 Uiso 1 calc R . .
H6B H -0.2857 -0.1559 -0.6081 0.042 Uiso 1 calc R . .
C11 C -0.3494(6) -0.0703(5) -0.6019(6) 0.044(4) Uani 1 d U . .
H11A H -0.3614 -0.0458 -0.6283 0.053 Uiso 1 calc R . .
H11B H -0.3124 -0.0643 -0.5958 0.053 Uiso 1 calc R . .
C12 C -0.3792(5) -0.0619(5) -0.5522(5) 0.031(3) Uani 1 d U . .
H12A H -0.3781 -0.0253 -0.5420 0.037 Uiso 1 calc R . .
H12B H -0.3646 -0.0829 -0.5241 0.037 Uiso 1 calc R . .
S1 S -0.44538(13) -0.08163(13) -0.56599(13) 0.0275(8) Uani 1 d . . .
C41 C -0.4212(6) -0.2568(5) -0.6460(5) 0.039(3) Uani 1 d U . .
H41A H -0.4428 -0.2549 -0.6771 0.046 Uiso 1 calc R . .
H41B H -0.3976 -0.2864 -0.6496 0.046 Uiso 1 calc R . .
C42 C -0.4542(5) -0.2642(6) -0.6001(5) 0.036(4) Uani 1 d U . .
H42A H -0.4327 -0.2741 -0.5704 0.043 Uiso 1 calc R . .
H42B H -0.4791 -0.2921 -0.6066 0.043 Uiso 1 calc R . .
S4 S -0.48892(13) -0.20402(14) -0.58559(13) 0.0278(9) Uani 1 d . . .
B1 B -0.7500 -0.2500 -0.7500 0.044(12) Uani 1 d SD . .
F10 F -0.7851(5) -0.2149(5) -0.7851(5) 0.048(8) Uani 0.50 d SPD . .
F11 F -0.7140(3) -0.2140(3) -0.7500 0.066(4) Uani 1 d SD . .
B2 B -0.5000 -0.2202(8) -0.7798(8) 0.057(8) Uani 1 d SD . .
F20 F -0.5138(5) -0.2306(7) -0.8288(5) 0.141(6) Uani 1 d D . .
F21 F -0.5398(6) -0.2296(5) -0.7508(6) 0.189(9) Uani 1 d D . .
B3 B -0.4090(18) -0.4090(18) -0.5910(18) 0.03(3) Uiso 0.25 d SPD A 1
F30 F -0.3733(13) -0.4422(13) -0.6041(13) 0.055(10) Uiso 0.25 d PD A 1
F31 F -0.4389(17) -0.4389(17) -0.5611(17) 0.28(15) Uiso 0.25 d SPD A 1
C1A C -0.4341(12) -0.4341(12) -0.5659(12) 0.18(9) Uiso 0.75 d SPDU B 2
C2A C -0.4020(11) -0.4020(11) -0.5980(11) 0.12(3) Uiso 0.75 d SPDU B 2
N1A N -0.3771(10) -0.3771(10) -0.6229(10) 0.096(13) Uiso 0.75 d SPDU B 2
B4 B -0.2500 0.0290(14) -0.5290(14) 0.051(16) Uiso 0.50 d SPD . .
F40 F -0.2141(11) 0.0525(12) -0.5535(13) 0.151(12) Uiso 0.50 d PD . .
F41 F -0.2430(19) -0.0201(11) -0.5388(12) 0.163(13) Uiso 0.50 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'
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
_geom_angle_publ_flag
N4 Ni1 N1 77.3(5) . . y
N4 Ni1 S1 166.0(4) . . y
N1 Ni1 S1 89.0(3) . . y
N4 Ni1 S4 90.9(4) . . y
N1 Ni1 S4 167.4(3) . . y
S1 Ni1 S4 103.02(15) . . y
S4 Ni2 S4 178.1(3) 21_554 23_455 ?
S4 Ni2 S4 89.984(4) 21_554 . ?
S4 Ni2 S4 89.984(5) 23_455 . ?
S4 Ni2 S4 89.984(4) 21_554 3_454 ?
S4 Ni2 S4 89.984(5) 23_455 3_454 ?
S4 Ni2 S4 178.1(3) . 3_454 ?
S1 Ni3 S1 175.0(2) 23_455 21_554 ?
S1 Ni3 S1 89.891(10) 23_455 . ?
S1 Ni3 S1 89.891(10) 21_554 . ?
S1 Ni3 S1 89.891(11) 23_455 3_454 ?
S1 Ni3 S1 89.891(11) 21_554 3_454 ?
S1 Ni3 S1 175.0(2) . 3_454 ?
C11 N1 C6 112.0(11) . . y
C11 N1 C2 115.2(11) . . ?
C6 N1 C2 106.3(11) . . ?
C11 N1 Ni1 115.5(8) . . ?
C6 N1 Ni1 101.3(8) . . ?
C2 N1 Ni1 105.2(8) . . y
N1 C2 C3 106.7(11) . . ?
N4 C3 C2 107.3(11) . . ?
C3 N4 C41 114.1(10) . . ?
C3 N4 C5 108.2(11) . . ?
C41 N4 C5 111.9(11) . . ?
C3 N4 Ni1 104.4(9) . . y
C41 N4 Ni1 115.4(9) . . ?
C5 N4 Ni1 101.8(8) . . y
N4 C5 C6 106.6(10) . . ?
N1 C6 C5 105.1(10) . . ?
N1 C11 C12 109.4(11) . . ?
C11 C12 S1 105.8(9) . . ?
C12 S1 Ni1 94.7(4) . . ?
C12 S1 Ni3 117.4(4) . . y
Ni1 S1 Ni3 117.43(18) . . y
C42 C41 N4 109.9(11) . . ?
C41 C42 S4 109.9(11) . . ?
C42 S4 Ni1 94.7(4) . . y
C42 S4 Ni2 106.3(5) . . ?
Ni1 S4 Ni2 106.68(16) . . y
F21 B2 F21 115(3) 19_444 . ?
F21 B2 F20 107.4(10) 19_444 19_444 ?
F21 B2 F20 105.7(8) . 19_444 ?
F21 B2 F20 107.3(10) . . ?
F30 B3 F30 117(2) 11_544 . ?
F30 B3 F31 100(4) . . ?
N1A C2A C1A 180(4) . . ?
F40 B4 F41 105(2) . . ?
F40 B4 F41 119(2) 43_444 . ?
F40 B4 F41 119(2) . 43_444 ?
F40 B4 F41 105(2) 43_444 43_444 ?
F41 B4 F41 113(5) . 43_444 ?
F40 B4 F41 118(2) . 4_554 ?
F40 B4 F41 127(2) 43_444 4_554 ?
F40 B4 F41 127(2) . 42_454 ?
F40 B4 F41 118(2) 43_444 42_454 ?
F41 F41 B4 115(5) 42_454 . ?
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
Ni1 N4 1.909(12) . y
Ni1 N1 1.928(10) . y
Ni1 S1 2.165(4) . y
Ni1 S4 2.165(4) . y
Ni2 S4 2.227(3) . y
Ni3 S1 2.212(3) . y
N1 C11 1.471(16) . y
N1 C6 1.493(16) . y
N1 C2 1.495(15) . y
C2 C3 1.529(18) . y
C3 N4 1.454(17) . ?
N4 C41 1.490(17) . ?
N4 C5 1.499(16) . ?
C5 C6 1.577(18) . ?
C11 C12 1.510(18) . ?
C12 S1 1.816(13) . ?
C41 C42 1.469(18) . ?
C42 S4 1.830(14) . ?
B1 F11 1.314(12) . ?
B1 F10 1.57(2) . ?
B2 F21 1.294(17) . ?
B2 F20 1.341(17) . ?
B3 F30 1.30(3) . ?
B3 F31 1.33(5) . ?
C1A C2A 1.44(2) . ?
C2A N1A 1.11(2) . ?
B4 F40 1.27(3) . ?
B4 F41 1.30(3) . ?
