#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:11:22 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180127 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/25/7102512.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_7102512
loop_
_publ_author_name
'Sydora, Orson L'
'Wolczanski, Peter T'
'Lobkovsky, Emil B'
'Rumberger, Evan'
'Hendrickson, David N'
_publ_section_title
;
 First row wheels, [((t)Bu(3)SiS)MX](12)(M = Co, X = Cl; M = Ni, X =
 Br), are common amongst both simpler and more complex aggregates.
;
_journal_issue                   6
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              650
_journal_page_last               651
_journal_paper_doi               10.1039/b311212h
_journal_year                    2004
_chemical_formula_sum            'C24 H54 Br2 Ni2 S2 Si2'
_chemical_formula_weight         740.21
_chemical_name_systematic
;
?
;
_space_group_IT_number           186
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c -2c'
_symmetry_space_group_name_H-M   'P 63 m c'
_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            12
_cell_length_a                   26.128(16)
_cell_length_b                   26.128(16)
_cell_length_c                   24.69(2)
_cell_measurement_temperature    173(2)
_cell_volume                     14597(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.850
_diffrn_measured_fraction_theta_max 0.850
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.1259
_diffrn_reflns_av_sigmaI/netI    0.2481
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9646
_diffrn_reflns_theta_full        22.20
_diffrn_reflns_theta_max         22.20
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    2.559
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.010
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4608
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.984
_refine_diff_density_rms         0.165
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.09(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         3730
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.2261
_refine_ls_R_factor_gt           0.1491
_refine_ls_shift/su_max          1.947
_refine_ls_shift/su_mean         0.171
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3646
_refine_ls_wR_factor_ref         0.4001
_reflns_number_gt                1627
_reflns_number_total             3730
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b311212h.txt
_cod_data_source_block           Ni12_(5)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
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 
;
_cod_original_sg_symbol_H-M      'P6(3)mc '
_cod_database_code               7102512
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, z+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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Br1 Br 0.91275(10) 0.45637(5) 0.83488(12) 0.0892(10) Uani 1 2 d S
Br2 Br 0.85442(6) 0.51236(7) 0.94880(7) 0.0793(7) Uani 1 1 d .
Br3 Br 0.78113(5) 0.56226(10) 0.84284(10) 0.0911(11) Uani 1 2 d S
Ni4 Ni 0.94532(7) 0.53520(10) 0.90224(8) 0.0833(10) Uani 1 1 d .
Ni5 Ni 0.86466(8) 0.60119(9) 0.90504(10) 0.0770(9) Uani 1 1 d .
S2 S 0.8242(2) 0.6485(4) 0.9499(3) 0.111(3) Uani 1 2 d S
S1 S 0.95574(19) 0.6264(2) 0.8759(2) 0.100(2) Uani 1 1 d .
Si1 Si 1.0017(2) 0.6761(3) 0.8009(2) 0.126(4) Uani 1 1 d D
C9 C 1.0760(4) 0.6798(4) 0.8012(5) 0.199(13) Uiso 1 1 d D
C12 C 1.1002(6) 0.7213(5) 0.7540(4) 0.101(7) Uiso 1 1 d D
H12A H 1.1404 0.7296 0.7461 0.152 Uiso 1 1 calc R
H12B H 1.1011 0.7583 0.7628 0.152 Uiso 1 1 calc R
H12C H 1.0751 0.7032 0.7222 0.152 Uiso 1 1 calc R
C11 C 1.0749(6) 0.6211(4) 0.7869(6) 0.105(7) Uiso 1 1 d D
H11A H 1.1152 0.6275 0.7883 0.158 Uiso 1 1 calc R
H11B H 1.0589 0.6084 0.7503 0.158 Uiso 1 1 calc R
H11C H 1.0500 0.5904 0.8130 0.158 Uiso 1 1 calc R
C10 C 1.1195(6) 0.7089(6) 0.8477(4) 0.123(7) Uiso 1 1 d D
H10A H 1.1550 0.7061 0.8409 0.185 Uiso 1 1 calc R
H10B H 1.1011 0.6887 0.8817 0.185 Uiso 1 1 calc R
H10C H 1.1304 0.7506 0.8503 0.185 Uiso 1 1 calc R
C5 C 1.0063(4) 0.7529(3) 0.8125(5) 0.098(7) Uiso 1 1 d D
C8 C 1.0290(6) 0.8077(6) 0.7727(5) 0.185(12) Uiso 1 1 d D
H8A H 1.0252 0.8393 0.7904 0.277 Uiso 1 1 calc R
H8B H 1.0052 0.7955 0.7396 0.277 Uiso 1 1 calc R
H8C H 1.0705 0.8222 0.7636 0.277 Uiso 1 1 calc R
C7 C 1.0502(5) 0.7698(6) 0.8588(5) 0.138(8) Uiso 1 1 d D
H7A H 1.0606 0.8092 0.8723 0.207 Uiso 1 1 calc R
H7B H 1.0859 0.7704 0.8458 0.207 Uiso 1 1 calc R
H7C H 1.0324 0.7409 0.8881 0.207 Uiso 1 1 calc R
C6 C 0.9505(4) 0.7503(6) 0.8372(6) 0.112(7) Uiso 1 1 d D
H6A H 0.9572 0.7905 0.8413 0.168 Uiso 1 1 calc R
H6B H 0.9423 0.7310 0.8727 0.168 Uiso 1 1 calc R
H6C H 0.9166 0.7277 0.8131 0.168 Uiso 1 1 calc R
C1 C 0.9504(4) 0.6369(4) 0.7416(4) 0.064(5) Uiso 1 1 d D
C4 C 0.9802(6) 0.6562(7) 0.6851(4) 0.221(14) Uiso 1 1 d D
H4A H 0.9514 0.6331 0.6569 0.331 Uiso 1 1 calc R
H4B H 1.0137 0.6493 0.6831 0.331 Uiso 1 1 calc R
H4C H 0.9942 0.6983 0.6796 0.331 Uiso 1 1 calc R
C3 C 0.9036(3) 0.6581(4) 0.7403(6) 0.088(6) Uiso 1 1 d D
H3A H 0.8759 0.6386 0.7104 0.133 Uiso 1 1 calc R
H3B H 0.9239 0.7010 0.7351 0.133 Uiso 1 1 calc R
H3C H 0.8818 0.6480 0.7746 0.133 Uiso 1 1 calc R
C2 C 0.9159(5) 0.5694(4) 0.7432(6) 0.076(5) Uiso 1 1 d D
H2A H 0.8921 0.5542 0.7103 0.114 Uiso 1 1 calc R
H2B H 0.8899 0.5561 0.7750 0.114 Uiso 1 1 calc R
H2C H 0.9436 0.5545 0.7454 0.114 Uiso 1 1 calc R
S3 S 1.0001(2) 0.50007(12) 0.9376(3) 0.104(3) Uani 1 2 d S
Si3 Si 1.0375(3) 0.51877(16) 1.0237(3) 0.116(4) Uani 1 2 d SD
C34 C 1.0839(4) 0.4811(4) 1.0271(5) 0.121(8) Uiso 1 1 d D
Si2 Si 0.84128(13) 0.6826(3) 1.0345(2) 0.089(3) Uani 1 2 d SD
C24 C 0.7989(4) 0.7232(4) 1.0320(5) 0.165(10) Uiso 1 1 d D
C20 C 0.8065(3) 0.6130(6) 1.0803(4) 0.147(13) Uiso 1 2 d SD
C36 C 1.1177(5) 0.4942(5) 1.0831(4) 0.044(4) Uiso 1 1 d D
H36A H 1.1416 0.4749 1.0838 0.066 Uiso 1 1 calc R
H36B H 1.0890 0.4789 1.1128 0.066 Uiso 1 1 calc R
H36C H 1.1435 0.5370 1.0874 0.066 Uiso 1 1 calc R
C21 C 0.8170(3) 0.6340(6) 1.1421(4) 0.151(13) Uiso 1 2 d SD
H21A H 0.7993(5) 0.5986(9) 1.1633(6) 0.226 Uiso 1 2 d SD
H21B H 0.8591(6) 0.646(2) 1.1478(9) 0.226 Uiso 1 1 d D
C25 C 0.7385(4) 0.7076(7) 1.0133(7) 0.239(15) Uiso 1 1 d D
H25A H 0.7317 0.7406 1.0208 0.358 Uiso 1 1 calc R
H25B H 0.7089 0.6723 1.0325 0.358 Uiso 1 1 calc R
H25C H 0.7351 0.6998 0.9742 0.358 Uiso 1 1 calc R
C35 C 1.0661(7) 0.4159(4) 1.0159(6) 0.110(8) Uiso 1 1 d D
H35A H 1.1002 0.4106 1.0218 0.165 Uiso 1 1 calc R
H35B H 1.0527 0.4060 0.9783 0.165 Uiso 1 1 calc R
H35C H 1.0340 0.3900 1.0404 0.165 Uiso 1 1 calc R
C42 C 0.9664(4) 0.48319(19) 1.0663(5) 0.109(10) Uiso 1 2 d SD
C37 C 1.1367(6) 0.5170(6) 0.9844(5) 0.153(9) Uiso 1 1 d D
H37A H 1.1632 0.5005 0.9842 0.229 Uiso 1 1 calc R
H37B H 1.1589 0.5587 0.9949 0.229 Uiso 1 1 calc R
H37C H 1.1201 0.5136 0.9481 0.229 Uiso 1 1 calc R
C22 C 0.8548(4) 0.5903(4) 1.0749(7) 0.158(10) Uiso 1 1 d D
H22A H 0.8419 0.5548 1.0970 0.237 Uiso 1 1 calc R
H22B H 0.8935 0.6215 1.0875 0.237 Uiso 1 1 calc R
H22C H 0.8578 0.5812 1.0369 0.237 Uiso 1 1 calc R
C26 C 0.8107(7) 0.7653(6) 1.0837(5) 0.40(2) Uiso 1 1 d D
H26A H 0.7867 0.7844 1.0805 0.601 Uiso 1 1 calc R
H26B H 0.8526 0.7955 1.0851 0.601 Uiso 1 1 calc R
H26C H 0.7998 0.7415 1.1168 0.601 Uiso 1 1 calc R
C43 C 0.9608(5) 0.5356(5) 1.0939(6) 0.163(10) Uiso 1 1 d D
H43A H 0.9252 0.5189 1.1165 0.245 Uiso 1 1 calc R
H43B H 0.9581 0.5606 1.0657 0.245 Uiso 1 1 calc R
H43C H 0.9956 0.5595 1.1165 0.245 Uiso 1 1 calc R
C27 C 0.8409(6) 0.7764(6) 0.9861(5) 0.246(16) Uiso 1 1 d D
H27A H 0.8241 0.8021 0.9801 0.369 Uiso 1 1 calc R
H27B H 0.8416 0.7578 0.9518 0.369 Uiso 1 1 calc R
H27C H 0.8813 0.8000 1.0000 0.369 Uiso 1 1 calc R
C44 C 0.9072(5) 0.4536(2) 1.0323(6) 0.36(3) Uiso 1 2 d SD
H44A H 0.8750(6) 0.4375(3) 1.0586(11) 0.540 Uiso 1 2 d SD
H44B H 0.9071(8) 0.4839(8) 1.0105(9) 0.540 Uiso 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'
Si Si 0.0817 0.0704 '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'
Br Br -0.2901 2.4595 '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
Ni4 Br1 Ni4 83.86(16) . 9
Ni4 Br2 Ni5 85.89(10) . .
Ni5 Br3 Ni5 86.79(15) . 8_655
S3 Ni4 S1 138.84(17) . .
S3 Ni4 Br2 117.6(2) . .
S1 Ni4 Br2 89.06(16) . .
S3 Ni4 Br1 86.84(18) . .
S1 Ni4 Br1 118.71(17) . .
Br2 Ni4 Br1 103.25(10) . .
S1 Ni5 S2 135.1(3) . .
S1 Ni5 Br3 121.11(18) . .
S2 Ni5 Br3 88.37(17) . .
S1 Ni5 Br2 90.96(19) . .
S2 Ni5 Br2 116.1(2) . .
Br3 Ni5 Br2 103.40(10) . .
Si2 S2 Ni5 128.3(2) . 8_655
Si2 S2 Ni5 128.3(2) . .
Ni5 S2 Ni5 94.7(3) 8_655 .
Si1 S1 Ni5 128.2(3) . .
Si1 S1 Ni4 125.1(3) . .
Ni5 S1 Ni4 92.60(18) . .
C9 Si1 C1 117.3(6) . .
C9 Si1 C5 114.1(5) . .
C1 Si1 C5 109.1(6) . .
C9 Si1 S1 105.4(5) . .
C1 Si1 S1 107.2(4) . .
C5 Si1 S1 102.3(4) . .
C12 C9 C10 106.5(8) . .
C12 C9 C11 109.2(11) . .
C10 C9 C11 107.6(11) . .
C12 C9 Si1 94.9(9) . .
C10 C9 Si1 121.2(10) . .
C11 C9 Si1 115.7(7) . .
C7 C5 C6 106.0(10) . .
C7 C5 C8 108.4(8) . .
C6 C5 C8 101.6(10) . .
C7 C5 Si1 93.3(9) . .
C6 C5 Si1 115.8(7) . .
C8 C5 Si1 129.3(9) . .
C2 C1 C4 108.0(10) . .
C2 C1 C3 107.0(8) . .
C4 C1 C3 102.6(11) . .
C2 C1 Si1 116.9(8) . .
C4 C1 Si1 114.4(6) . .
C3 C1 Si1 106.8(8) . .
Ni4 S3 Ni4 94.3(3) . 9
Ni4 S3 Si3 124.8(2) . .
Ni4 S3 Si3 124.7(2) 9 .
C34 Si3 C34 113.0(6) . 9
C34 Si3 C42 115.9(4) . .
C34 Si3 C42 115.8(4) 9 .
C34 Si3 S3 104.2(4) . .
C34 Si3 S3 104.1(4) 9 .
C42 Si3 S3 101.5(5) . .
C35 C34 C37 102.8(11) . .
C35 C34 C36 102.9(10) . .
C37 C34 C36 102.8(8) . .
C35 C34 Si3 129.8(9) . .
C37 C34 Si3 104.5(9) . .
C36 C34 Si3 110.9(9) . .
C24 Si2 C24 121.4(6) 8_655 .
C24 Si2 C20 114.6(4) 8_655 .
C24 Si2 C20 114.5(4) . .
C24 Si2 S2 98.0(4) 8_655 .
C24 Si2 S2 98.0(4) . .
C20 Si2 S2 105.5(5) . .
C24 Si2 C27 38.0(4) 8_655 8_655
C24 Si2 C27 90.0(5) . 8_655
C20 Si2 C27 152.4(3) . 8_655
S2 Si2 C27 81.9(4) . 8_655
C25 C24 C26 104.2(12) . .
C25 C24 C27 100.2(10) . .
C26 C24 C27 98.3(8) . .
C25 C24 Si2 134.3(10) . .
C26 C24 Si2 113.3(10) . .
C27 C24 Si2 99.3(8) . .
C21 C20 C22 99.8(7) . 8_655
C21 C20 C22 99.8(7) . .
C22 C20 C22 142.3(11) 8_655 .
C21 C20 Si2 108.4(9) . .
C22 C20 Si2 102.0(6) 8_655 .
C22 C20 Si2 101.9(6) . .
C44 C42 C43 99.2(6) . .
C44 C42 C43 99.2(6) . 9
C43 C42 C43 128.7(14) . 9
C44 C42 Si3 114.7(9) . .
C43 C42 Si3 107.4(5) . .
C43 C42 Si3 107.4(5) 9 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 Ni4 2.445(3) .
Br1 Ni4 2.446(3) 9
Br2 Ni4 2.429(3) .
Br2 Ni5 2.450(3) .
Br3 Ni5 2.436(3) .
Br3 Ni5 2.436(3) 8_655
Ni4 S3 2.229(5) .
Ni4 S1 2.350(7) .
Ni5 S1 2.247(6) .
Ni5 S2 2.277(6) .
S2 Si2 2.225(10) .
S2 Ni5 2.275(6) 8_655
S1 Si1 2.235(7) .
Si1 C9 1.893(12) .
Si1 C1 1.902(10) .
Si1 C5 1.971(12) .
C9 C12 1.500(15) .
C9 C10 1.524(15) .
C9 C11 1.563(16) .
C5 C7 1.521(15) .
C5 C6 1.550(15) .
C5 C8 1.587(15) .
C1 C2 1.528(11) .
C1 C4 1.555(14) .
C1 C3 1.578(15) .
S3 Ni4 2.230(5) 9
S3 Si3 2.287(10) .
Si3 C34 1.907(13) .
Si3 C34 1.909(13) 9
Si3 C42 1.924(13) .
C34 C35 1.549(15) .
C34 C37 1.612(15) .
C34 C36 1.583(14) .
Si2 C24 1.879(13) 8_655
Si2 C24 1.877(13) .
Si2 C20 1.937(13) .
Si2 C27 2.731(16) 8_655
C24 C25 1.494(15) .
C24 C26 1.610(16) .
C24 C27 1.703(15) .
C20 C21 1.599(14) .
C20 C22 1.646(13) 8_655
C20 C22 1.649(13) .
C42 C44 1.580(15) .
C42 C43 1.601(14) .
C42 C43 1.600(14) 9
