#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:20:51 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178946 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/75/4117535.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_4117535
loop_
_publ_author_name
'Tao Wu'
'Xianhui Bu'
'Puhong Liao'
'Le Wang'
'Shou-Tian Zheng'
'Richard Ma'
'Pingyun Feng'
_publ_section_title
;
 Superbase Route to Supertetrahedral Chalcogenide Clusters
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3619
_journal_page_last               3622
_journal_paper_doi               10.1021/ja210039u
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C21 H27 Ga10 N9 O3 S16'
_chemical_formula_sum            'C21 H27 Ga10 N9 O3 S16'
_chemical_formula_weight         1663.68
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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            6
_cell_length_a                   21.70730(10)
_cell_length_b                   21.70730(10)
_cell_length_c                   28.5686(3)
_cell_measurement_temperature    150(2)
_cell_volume                     11658.19(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       'Omega Scan'
_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  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            34402
_diffrn_reflns_theta_full        22.49
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    3.862
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       block
_exptl_crystal_F_000             4836
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.923
_refine_diff_density_min         -1.289
_refine_diff_density_rms         0.236
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         3382
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0892
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1694P)²+503.4629P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2905
_refine_ls_wR_factor_ref         0.3203
_reflns_number_gt                2610
_reflns_number_total             3382
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210039u_si_002_2.cif
_cod_data_source_block           ISC-2
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4117535
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Ga1 Ga 0.89844(7) 0.90073(7) 0.14464(5) 0.0470(6) Uani 1 1 d .
Ga2 Ga 0.89994(9) 1.00119(9) 0.25287(6) 0.0606(6) Uani 1 1 d .
Ga3 Ga 1.0000 1.0000 0.34728(12) 0.0925(12) Uani 1 3 d S
Ga4 Ga 0.99407(8) 0.81370(8) 0.15046(6) 0.0550(6) Uani 1 1 d .
N1 N 0.9908(7) 0.7245(5) 0.1255(5) 0.124(3) Uani 1 1 d GD
C1 C 0.9421(7) 0.6595(6) 0.1452(5) 0.124(3) Uani 1 1 d GD
H1A H 0.9111 0.6576 0.1693 0.149 Uiso 1 1 calc R
C2 C 0.9388(7) 0.5973(5) 0.1295(6) 0.124(3) Uani 1 1 d GD
H2A H 0.9056 0.5529 0.1430 0.149 Uiso 1 1 calc R
C3 C 0.9842(7) 0.6001(5) 0.0942(5) 0.124(3) Uani 1 1 d GD
C4 C 1.0329(7) 0.6651(6) 0.0746(5) 0.124(3) Uani 1 1 d GD
C5 C 1.0362(7) 0.7273(5) 0.0902(5) 0.124(3) Uani 1 1 d GD
H5A H 1.0695 0.7717 0.0767 0.149 Uiso 1 1 calc R
C6 C 0.9813(11) 0.5325(9) 0.0795(9) 0.124(3) Uani 1 1 d D
H6A H 0.9436 0.4925 0.0968 0.186 Uiso 1 1 calc R
H6B H 1.0271 0.5357 0.0860 0.186 Uiso 1 1 calc R
H6C H 0.9713 0.5252 0.0458 0.186 Uiso 1 1 calc R
C7 C 1.0806(11) 0.6701(11) 0.0346(8) 0.124(3) Uani 1 1 d D
H7A H 1.1114 0.7201 0.0260 0.186 Uiso 1 1 calc R
H7B H 1.0514 0.6438 0.0076 0.186 Uiso 1 1 calc R
H7C H 1.1098 0.6496 0.0442 0.186 Uiso 1 1 calc R
S1 S 0.8979(3) 0.9976(3) 0.33072(16) 0.0903(16) Uani 1 1 d .
S2 S 0.89352(19) 0.80088(18) 0.11925(13) 0.0545(9) Uani 1 1 d .
S3 S 1.0000 1.0000 0.11748(19) 0.0439(13) Uani 1 3 d S
S4 S 0.80212(19) 0.90325(19) 0.11979(14) 0.0568(10) Uani 1 1 d .
S5 S 0.89814(19) 0.89984(19) 0.22611(13) 0.0546(10) Uani 1 1 d .
S6 S 0.8054(2) 1.0071(2) 0.22829(15) 0.0681(11) Uani 1 1 d .
O1 O 1.0000 1.0000 0.4241(11) 0.156(12) Uani 1 3 d S
O2 O 0.0000 0.0000 0.0000 0.24(3) Uiso 1 6 d S
O3 O 0.851(3) 0.581(3) 1.0106(19) 0.21(2) Uiso 0.50 1 d P
N2 N 0.8912(18) 0.6910(18) 1.0170(12) 0.204(13) Uiso 1 1 d .
N3 N 0.892(2) 0.983(2) 0.0028(15) 0.241(17) Uiso 1 1 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 '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'
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
S4 Ga1 S2 109.20(14) . .
S4 Ga1 S3 109.76(13) . .
S2 Ga1 S3 110.81(13) . .
S4 Ga1 S5 108.62(14) . .
S2 Ga1 S5 108.52(14) . .
S3 Ga1 S5 109.90(16) . .
S1 Ga2 S6 108.29(18) . .
S1 Ga2 S5 107.86(18) . .
S6 Ga2 S5 111.86(16) . .
S1 Ga2 S5 110.75(18) . 3_675
S6 Ga2 S5 108.11(16) . 3_675
S5 Ga2 S5 109.97(17) . 3_675
O1 Ga3 S1 102.19(14) . 3_675
O1 Ga3 S1 102.19(14) . 2_765
S1 Ga3 S1 115.66(10) 3_675 2_765
O1 Ga3 S1 102.20(14) . .
S1 Ga3 S1 115.66(9) 3_675 .
S1 Ga3 S1 115.66(10) 2_765 .
N1 Ga4 S2 100.0(5) . .
N1 Ga4 S4 101.2(3) . 2_765
S2 Ga4 S4 116.82(16) . 2_765
N1 Ga4 S6 102.3(5) . 2_765
S2 Ga4 S6 115.91(16) . 2_765
S4 Ga4 S6 116.24(17) 2_765 2_765
C1 N1 C5 120.0 . .
C1 N1 Ga4 118.1(6) . .
C5 N1 Ga4 121.8(6) . .
C2 C1 N1 120.0 . .
C1 C2 C3 120.0 . .
C4 C3 C2 120.0 . .
C4 C3 C6 121.2(11) . .
C2 C3 C6 118.7(12) . .
C5 C4 C3 120.0 . .
C5 C4 C7 118.2(11) . .
C3 C4 C7 121.7(11) . .
C4 C5 N1 120.0 . .
Ga2 S1 Ga3 102.0(2) . .
Ga1 S2 Ga4 100.31(15) . .
Ga1 S3 Ga1 109.35(13) 3_675 2_765
Ga1 S3 Ga1 109.35(13) 3_675 .
Ga1 S3 Ga1 109.35(13) 2_765 .
Ga1 S4 Ga4 101.80(15) . 3_675
Ga2 S5 Ga2 109.39(17) . 2_765
Ga2 S5 Ga1 108.92(15) . .
Ga2 S5 Ga1 109.28(15) 2_765 .
Ga2 S6 Ga4 100.05(16) . 3_675
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ga1 S4 2.234(4) .
Ga1 S2 2.237(4) .
Ga1 S3 2.314(2) .
Ga1 S5 2.328(4) .
Ga2 S1 2.225(5) .
Ga2 S6 2.234(5) .
Ga2 S5 2.311(4) .
Ga2 S5 2.326(4) 3_675
Ga3 O1 2.20(3) .
Ga3 S1 2.241(6) 3_675
Ga3 S1 2.241(5) 2_765
Ga3 S1 2.241(5) .
Ga4 N1 2.031(8) .
Ga4 S2 2.243(4) .
Ga4 S4 2.244(4) 2_765
Ga4 S6 2.247(4) 2_765
N1 C1 1.3900 .
N1 C5 1.3900 .
C1 C2 1.3900 .
C2 C3 1.3900 .
C3 C4 1.3900 .
C3 C6 1.496(15) .
C4 C5 1.3900 .
C4 C7 1.507(15) .
S3 Ga1 2.314(2) 3_675
S3 Ga1 2.314(2) 2_765
S4 Ga4 2.244(4) 3_675
S5 Ga2 2.326(4) 2_765
S6 Ga4 2.247(4) 3_675
