#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:20:51 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178946 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/75/4117539.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_4117539
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         'C40 Cd13 In22 N4 S52'
_chemical_formula_sum            'C40 Cd13 In22 N4 S52'
_chemical_formula_weight         6190.80
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           141
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4bd 2'
_symmetry_space_group_name_H-M   'I 41/a m d :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            4
_cell_length_a                   28.0877(4)
_cell_length_b                   28.0877(4)
_cell_length_c                   26.7025(4)
_cell_measurement_temperature    150(2)
_cell_volume                     21066.1(5)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1078
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            40812
_diffrn_reflns_theta_full        20.00
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         1.05
_exptl_absorpt_coefficient_mu    4.166
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.952
_exptl_crystal_description       'elongated square bipyramid'
_exptl_crystal_F_000             11208
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.114
_refine_diff_density_min         -6.611
_refine_diff_density_rms         0.642
_refine_ls_extinction_coef       0.00021(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2601
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.2824
_refine_ls_R_factor_gt           0.1946
_refine_ls_shift/su_max          0.500
_refine_ls_shift/su_mean         0.102
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+20000.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4616
_refine_ls_wR_factor_ref         0.6185
_reflns_number_gt                1236
_reflns_number_total             2601
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210039u_si_002_6.cif
_cod_data_source_block           ISC-9-No-SQ
_cod_original_sg_symbol_H-M      'I 41/a m d'
_cod_database_code               4117539
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+1/4, x+3/4, z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-x+1/2, y, -z+1/2'
'x, -y, -z'
'y+1/4, x+3/4, -z+1/4'
'-y+1/4, -x+1/4, -z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+3/4, x+5/4, z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-x+1, y+1/2, -z+1'
'x+1/2, -y+1/2, -z+1/2'
'y+3/4, x+5/4, -z+3/4'
'-y+3/4, -x+3/4, -z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-1/4, -x-3/4, -z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'x-1/2, -y, z-1/2'
'-x, y, z'
'-y-1/4, -x-3/4, z-1/4'
'y-1/4, x-1/4, z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y+1/4, -x-1/4, -z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'x, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'
'-y+1/4, -x-1/4, z+1/4'
'y+1/4, x+1/4, z-1/4'
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
N1 N 0.164(6) 0.2500 0.860(6) 0.20(6) Uiso 1 2 d S
Cd1 Cd 0.5000 0.2500 1.1250 0.168(11) Uani 1 8 d S
Cd2 Cd 0.4298(2) 0.3202(2) 1.02153(18) 0.081(2) Uani 1 1 d .
Cd3 Cd 0.3593(3) 0.2500 1.1252(3) 0.084(3) Uani 1 2 d S
In1 In 0.5000 0.2500 0.9147(4) 0.085(4) Uani 1 4 d S
In2 In 0.3598(3) 0.2500 0.9133(3) 0.109(4) Uani 1 2 d S
In3 In 0.3576(2) 0.3924(2) 1.1250 0.092(3) Uani 1 2 d S
In4 In 0.2874(3) 0.3219(3) 1.0207(2) 0.115(3) Uani 1 1 d .
In5 In 0.2239(5) 0.2500 0.9192(5) 0.175(6) Uani 1 2 d S
S1 S 0.4309(7) 0.2500 1.0745(7) 0.049(6) Uani 1 2 d S
S2 S 0.5000 0.3233(9) 0.9667(7) 0.058(6) Uani 1 2 d S
S3 S 0.4296(6) 0.3935(6) 1.0708(6) 0.063(5) Uani 1 1 d .
S4 S 0.3593(6) 0.3233(7) 0.9668(6) 0.075(6) Uani 1 1 d .
S5 S 0.2858(9) 0.2500 1.0750(9) 0.079(8) Uani 1 2 d S
S6 S 0.4302(10) 0.2500 0.8604(9) 0.097(10) Uani 1 2 d S
S7 S 0.2900(13) 0.2500 0.8610(12) 0.150(18) Uani 1 2 d S
S8 S 0.2160(9) 0.3209(13) 0.9684(10) 0.148(12) Uani 1 1 d .
S9 S 0.2861(7) 0.3937(9) 1.0727(8) 0.100(7) Uani 1 1 d .
C1 C 0.5000 0.390(3) 0.917(3) 0.037(18) Uiso 1 2 d S
C2 C 0.4288(18) 0.4620(19) 1.0212(18) 0.042(14) Uiso 1 1 d .
C3 C 0.430(3) 0.320(3) 0.812(3) 0.09(2) Uiso 1 1 d .
C4 C 0.360(3) 0.400(3) 0.908(3) 0.11(3) Uiso 1 1 d .
C5 C 0.176(9) 0.2500 1.134(9) 0.24(10) Uiso 1 2 d S
C6 C 0.215(3) 0.394(3) 1.128(3) 0.10(3) 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
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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'
C C 0.0033 0.0016 '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
S1 Cd1 S1 109.0(5) . 27_567
S1 Cd1 S1 109.0(5) . 20_658
S1 Cd1 S1 110.4(10) 27_567 20_658
S1 Cd1 S1 110.4(10) . 10_554
S1 Cd1 S1 109.0(5) 27_567 10_554
S1 Cd1 S1 109.0(5) 20_658 10_554
S1 Cd2 S3 111.8(5) . .
S1 Cd2 S2 111.4(7) . .
S3 Cd2 S2 107.0(7) . .
S1 Cd2 S4 112.6(7) . .
S3 Cd2 S4 106.7(6) . .
S2 Cd2 S4 106.9(6) . .
S1 Cd3 S3 110.9(5) . 16_556
S1 Cd3 S3 110.9(5) . 20_658
S3 Cd3 S3 107.7(8) 16_556 20_658
S1 Cd3 S5 113.0(8) . .
S3 Cd3 S5 107.1(6) 16_556 .
S3 Cd3 S5 107.1(6) 20_658 .
S6 In1 S6 107.0(13) . 10_554
S6 In1 S2 109.4(4) . .
S6 In1 S2 109.4(4) 10_554 .
S6 In1 S2 109.4(4) . 10_554
S6 In1 S2 109.4(4) 10_554 10_554
S2 In1 S2 112.0(11) . 10_554
S7 In2 S6 109.0(11) . .
S7 In2 S4 109.0(6) . 29
S6 In2 S4 109.6(6) . 29
S7 In2 S4 109.0(6) . .
S6 In2 S4 109.6(6) . .
S4 In2 S4 110.6(9) 29 .
S9 In3 S9 107.5(11) 16_556 .
S9 In3 S3 109.5(7) 16_556 .
S9 In3 S3 109.6(6) . .
S9 In3 S3 109.6(6) 16_556 16_556
S9 In3 S3 109.5(7) . 16_556
S3 In3 S3 111.1(8) . 16_556
S8 In4 S9 108.7(9) . .
S8 In4 S4 109.7(8) . .
S9 In4 S4 109.2(8) . .
S8 In4 S5 107.9(10) . .
S9 In4 S5 109.7(7) . .
S4 In4 S5 111.5(8) . .
N1 In5 S8 108(2) . 29
N1 In5 S8 108(2) . .
S8 In5 S8 112.4(16) 29 .
N1 In5 S7 97(4) . .
S8 In5 S7 115.1(9) 29 .
S8 In5 S7 115.1(9) . .
Cd1 S1 Cd3 111.3(8) . .
Cd1 S1 Cd2 110.0(6) . .
Cd3 S1 Cd2 108.4(6) . .
Cd1 S1 Cd2 110.0(6) . 29
Cd3 S1 Cd2 108.4(6) . 29
Cd2 S1 Cd2 108.7(8) . 29
C1 S2 Cd2 111.7(11) . .
C1 S2 Cd2 111.7(11) . 22_655
Cd2 S2 Cd2 106.8(8) . 22_655
C1 S2 In1 111.1(19) . .
Cd2 S2 In1 107.7(7) . .
Cd2 S2 In1 107.7(7) 22_655 .
Cd2 S3 Cd3 106.7(7) . 27_567
Cd2 S3 In3 107.7(7) . .
Cd3 S3 In3 108.3(6) 27_567 .
Cd2 S4 In4 108.0(6) . .
Cd2 S4 In2 107.7(7) . .
In4 S4 In2 108.8(8) . .
Cd3 S5 In4 107.6(7) . .
Cd3 S5 In4 107.6(7) . 29
In4 S5 In4 108.6(10) . 29
In2 S6 In1 107.9(10) . .
In2 S7 In5 104.6(13) . .
In5 S8 In4 104.2(11) . .
In3 S9 In4 107.4(8) . .
C5 C1 S2 172(10) 11_544 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 In5 2.31(16) .
Cd1 S1 2.36(2) .
Cd1 S1 2.36(2) 27_567
Cd1 S1 2.36(2) 20_658
Cd1 S1 2.36(2) 10_554
Cd2 S1 2.427(13) .
Cd2 S3 2.444(18) .
Cd2 S2 2.457(13) .
Cd2 S4 2.463(17) .
Cd3 S1 2.42(2) .
Cd3 S3 2.448(16) 16_556
Cd3 S3 2.448(16) 20_658
Cd3 S5 2.46(2) .
In1 S6 2.44(3) .
In1 S6 2.44(3) 10_554
In1 S2 2.48(2) .
In1 S2 2.48(2) 10_554
In2 S7 2.41(3) .
In2 S6 2.43(3) .
In2 S4 2.51(2) 29
In2 S4 2.51(2) .
In3 S9 2.45(2) 16_556
In3 S9 2.45(2) .
In3 S3 2.487(17) .
In3 S3 2.487(17) 16_556
In4 S8 2.45(2) .
In4 S9 2.45(2) .
In4 S4 2.479(19) .
In4 S5 2.488(16) .
In5 S8 2.40(3) 29
In5 S8 2.40(3) .
In5 S7 2.42(4) .
S1 Cd2 2.427(13) 29
S2 C1 2.30(8) .
S2 Cd2 2.457(13) 22_655
S3 Cd3 2.448(16) 27_567
S5 In4 2.488(16) 29
C1 C5 1.3(2) 11_544
C4 C6 1.98(12) 11_544
C5 C1 1.3(2) 12_454
C6 C4 1.98(13) 12_454
