#------------------------------------------------------------------------------
#$Date: 2019-11-22 19:14:49 +0200 (Fri, 22 Nov 2019) $
#$Revision: 231292 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/64/4516412.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_4516412
loop_
_publ_author_name
'Zhao, Xiao-Wei'
'Qian, Li-Wen'
'Su, Hu-Chao'
'Mo, Chong-Jiao'
'Que, Chen-Jie'
'Zhu, Qin-Yu'
'Dai, Jie'
_publ_section_title
;
 Co-assembled T4-Cu4In16S35 and Cubic Cu12S8 Clusters: A Crystal Precursor
 for Near-Infrared Absorption Material
;
_journal_issue                   12
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              5749
_journal_paper_doi               10.1021/acs.cgd.5b00960
_journal_volume                  15
_journal_year                    2015
_chemical_formula_sum            'C64 H296 Cu20 In32 N64 S78'
_chemical_formula_weight         9409.63
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   20.0486(4)
_cell_length_b                   20.0486(4)
_cell_length_c                   71.7730(17)
_cell_measurement_reflns_used    14616
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5
_cell_measurement_theta_min      3.2
_cell_volume                     24983.9(9)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0945
_diffrn_reflns_av_unetI/netI     0.0652
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       85
_diffrn_reflns_limit_l_min       -77
_diffrn_reflns_number            37150
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         3.075
_exptl_absorpt_coefficient_mu    3.932
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication '
_exptl_crystal_colour            'clear light red'
_exptl_crystal_density_diffrn    1.875
_exptl_crystal_description       block
_exptl_crystal_F_000             13548
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         3.841
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         9637
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.1148
_refine_ls_R_factor_gt           0.0751
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0010P)²+1600.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1604
_refine_ls_wR_factor_ref         0.1754
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5893
_reflns_number_total             9637
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg5b00960_si_002.cif
_cod_data_source_block           l
_cod_original_cell_volume        24983.9(12)
_cod_database_code               4516412
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.440
_shelx_estimated_absorpt_t_max   0.507
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cu1 Cu 0.45103(13) -0.36858(14) 0.16692(4) 0.0819(7) Uani 1 1 d . . .
Cu2 Cu 0.42384(15) -0.30538(15) 0.13317(3) 0.0848(7) Uani 1 1 d . . .
In1 In 0.96789(6) 0.68956(6) 0.05352(2) 0.0543(3) Uani 1 1 d . . .
In2 In 0.74858(6) 0.55456(5) 0.05226(2) 0.0421(2) Uani 1 1 d . . .
In3 In 0.88877(5) 0.47125(5) 0.05256(2) 0.0427(3) Uani 1 1 d . . .
In4 In 0.86723(5) 0.57452(5) 0.09710(2) 0.0407(2) Uani 1 1 d . . .
Cu3 Cu 0.6667 0.3333 0.05342(4) 0.0358(6) Uani 1 3 d S T P
Cu4 Cu 0.78388(9) 0.35281(8) 0.09639(2) 0.0380(4) Uani 1 1 d . . .
In7 In 0.76579(5) 0.45546(5) 0.14066(2) 0.0368(2) Uani 1 1 d . . .
In8 In 0.6667 0.3333 0.18406(2) 0.0505(4) Uani 1 3 d S T P
S1 S 1.0789(3) 0.8138(3) 0.04247(8) 0.0928(17) Uani 1 1 d . . .
S2 S 0.8503(2) 0.6791(2) 0.04053(6) 0.0573(10) Uani 1 1 d . . .
S3 S 0.9953(2) 0.5929(2) 0.04048(5) 0.0539(10) Uani 1 1 d . . .
S4 S 0.9737(2) 0.7001(2) 0.08744(5) 0.0560(10) Uani 1 1 d . . .
S5 S 0.76652(19) 0.45077(18) 0.03928(4) 0.0385(7) Uani 1 1 d . . .
S6 S 0.9119(2) 0.3716(2) 0.03999(5) 0.0470(8) Uani 1 1 d . . .
S7 S 0.74338(18) 0.55817(17) 0.08648(4) 0.0377(7) Uani 1 1 d . . .
S8 S 0.89344(18) 0.47250(18) 0.08685(4) 0.0384(7) Uani 1 1 d . . .
S9 S 0.86893(19) 0.58263(18) 0.13109(4) 0.0409(8) Uani 1 1 d . . .
S10 S 0.6667 0.3333 0.08584(10) 0.0596(17) Uani 1 3 d S T P
S11 S 0.79623(17) 0.35738(17) 0.12976(4) 0.0338(7) Uani 1 1 d . . .
S12 S 0.7681(2) 0.4611(2) 0.17494(5) 0.0487(9) Uani 1 1 d . . .
S13 S 0.6667 0.3333 0.21844(10) 0.088(3) Uani 1 3 d S T P
S14 S 0.5266(3) -0.2743(4) 0.14886(10) 0.1025(19) Uani 1 1 d . . .
S15 S 0.3333 -0.3333 0.11322(13) 0.108(3) Uani 1 3 d S T P
N1 N 0.9875(11) 0.5196(12) 0.1524(3) 0.111(6) Uani 1 1 d . . .
N2 N 0.9332(16) 0.679(2) 0.1779(5) 0.30(3) Uani 1 1 d . . .
N3 N 0.5515(11) 0.1110(13) -0.0054(2) 0.109(6) Uani 1 1 d . . .
N4 N 0.4472(16) 0.1832(15) -0.0025(3) 0.151(10) Uani 1 1 d . . .
N5 N 0.6206(14) 0.5100(14) 0.1734(3) 0.132(8) Uani 1 1 d . . .
N6 N 1.1131(10) 0.4219(10) -0.0028(2) 0.088(5) Uani 1 1 d . . .
C1 C 1.0145(15) 0.4973(19) 0.1364(4) 0.128(10) Uani 1 1 d . . .
C2 C 1.0657(17) 0.571(3) 0.1231(6) 0.24(2) Uani 1 1 d . . .
C3 C 0.939(2) 0.644(2) 0.2013(5) 0.159(12) Uani 1 1 d . U .
C4 C 0.8567(17) 0.6094(15) 0.2091(4) 0.122(9) Uani 1 1 d . . .
C5 C 0.5712(19) 0.193(2) -0.0123(5) 0.193(18) Uani 1 1 d . . .
C6 C 0.4974(19) 0.1983(16) -0.0168(3) 0.121(9) Uani 1 1 d . . .
C7 C 1.0496(17) 0.341(2) 0.0093(3) 0.174(13) Uani 1 1 d . U .
C8 C 0.605(4) 0.540(5) 0.1951(10) 0.31(3) Uiso 1 1 d . . .
C9 C 0.586(4) 0.481(5) 0.2071(11) 0.33(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
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'
Cu Cu 0.3201 1.2651 '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'
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
S14 Cu1 S14 169.5(3) 14 .
S14 Cu1 Cu1 50.11(19) 14 14
S14 Cu1 Cu1 136.6(2) . 14
S14 Cu1 Cu1 138.5(2) 14 15_445
S14 Cu1 Cu1 49.35(19) . 15_445
Cu1 Cu1 Cu1 119.982(6) 14 15_445
S14 Cu1 Cu2 48.09(18) 14 14
S14 Cu1 Cu2 139.7(2) . 14
Cu1 Cu1 Cu2 61.90(10) 14 14
Cu1 Cu1 Cu2 90.60(11) 15_445 14
S14 Cu1 Cu2 139.3(2) 14 .
S14 Cu1 Cu2 47.36(18) . .
Cu1 Cu1 Cu2 89.52(11) 14 .
Cu1 Cu1 Cu2 60.58(10) 15_445 .
Cu2 Cu1 Cu2 122.62(12) 14 .
S14 Cu2 S15 170.0(3) . .
S14 Cu2 Cu2 137.8(2) . 2_545
S15 Cu2 Cu2 49.68(15) . 2_545
S14 Cu2 Cu2 137.3(2) . 3_655
S15 Cu2 Cu2 49.68(15) . 3_655
Cu2 Cu2 Cu2 60.0 2_545 3_655
S14 Cu2 Cu1 47.81(18) . 15_445
S15 Cu2 Cu1 139.64(18) . 15_445
Cu2 Cu2 Cu1 90.16(10) 2_545 15_445
Cu2 Cu2 Cu1 118.89(7) 3_655 15_445
S14 Cu2 Cu1 47.80(18) . .
S15 Cu2 Cu1 139.22(17) . .
Cu2 Cu2 Cu1 118.49(7) 2_545 .
Cu2 Cu2 Cu1 89.72(10) 3_655 .
Cu1 Cu2 Cu1 57.52(6) 15_445 .
S4 In1 S2 112.97(15) . .
S4 In1 S3 115.44(14) . .
S2 In1 S3 111.99(14) . .
S4 In1 S1 104.48(16) . .
S2 In1 S1 107.70(17) . .
S3 In1 S1 103.15(17) . .
S6 In2 S2 105.34(13) 2_655 .
S6 In2 S7 108.03(12) 2_655 .
S2 In2 S7 109.80(13) . .
S6 In2 S5 108.44(12) 2_655 .
S2 In2 S5 109.38(13) . .
S7 In2 S5 115.36(11) . .
S6 In3 S3 104.81(12) . .
S6 In3 S8 110.88(12) . .
S3 In3 S8 109.42(12) . .
S6 In3 S5 107.51(12) . .
S3 In3 S5 109.06(12) . .
S8 In3 S5 114.68(11) . .
S9 In4 S4 103.79(12) . .
S9 In4 S7 107.35(11) . .
S4 In4 S7 110.64(13) . .
S9 In4 S8 110.59(12) . .
S4 In4 S8 109.28(13) . .
S7 In4 S8 114.64(11) . .
S10 Cu3 S5 114.77(10) . 3_665
S10 Cu3 S5 114.77(10) . 2_655
S5 Cu3 S5 103.70(11) 3_665 2_655
S10 Cu3 S5 114.77(10) . .
S5 Cu3 S5 103.69(11) 3_665 .
S5 Cu3 S5 103.69(11) 2_655 .
S10 Cu4 S8 114.83(13) . .
S10 Cu4 S11 114.2(2) . .
S8 Cu4 S11 102.73(12) . .
S10 Cu4 S7 114.52(13) . 3_665
S8 Cu4 S7 104.03(12) . 3_665
S11 Cu4 S7 105.18(12) . 3_665
S9 In7 S11 108.76(11) . 2_655
S9 In7 S11 109.02(11) . .
S11 In7 S11 115.22(14) 2_655 .
S9 In7 S12 104.24(12) . .
S11 In7 S12 108.63(12) 2_655 .
S11 In7 S12 110.39(12) . .
S12 In8 S12 113.04(7) . 3_665
S12 In8 S12 113.04(7) . 2_655
S12 In8 S12 113.04(7) 3_665 2_655
S12 In8 S13 105.61(8) . .
S12 In8 S13 105.61(8) 3_665 .
S12 In8 S13 105.61(8) 2_655 .
In1 S2 In2 103.39(14) . .
In1 S3 In3 102.89(13) . .
In1 S4 In4 102.36(14) . .
Cu3 S5 In2 105.29(12) . .
Cu3 S5 In3 105.64(12) . .
In2 S5 In3 105.42(12) . .
In3 S6 In2 104.30(12) . 3_665
Cu4 S7 In4 105.70(12) 2_655 .
Cu4 S7 In2 106.67(12) 2_655 .
In4 S7 In2 105.00(12) . .
Cu4 S8 In3 105.28(13) . .
Cu4 S8 In4 106.00(12) . .
In3 S8 In4 106.51(12) . .
In4 S9 In7 103.56(12) . .
Cu4 S10 Cu4 109.79(17) 3_665 2_655
Cu4 S10 Cu4 109.79(17) 3_665 .
Cu4 S10 Cu4 109.79(17) 2_655 .
Cu4 S10 Cu3 109.15(18) 3_665 .
Cu4 S10 Cu3 109.15(18) 2_655 .
Cu4 S10 Cu3 109.15(18) . .
Cu4 S11 In7 104.97(12) . 3_665
Cu4 S11 In7 106.57(12) . .
In7 S11 In7 105.33(12) 3_665 .
In8 S12 In7 103.52(13) . .
Cu1 S14 Cu2 84.1(2) 15_445 .
Cu1 S14 Cu1 80.5(2) 15_445 .
Cu2 S14 Cu1 84.8(2) . .
Cu2 S15 Cu2 80.6(3) 2_545 3_655
Cu2 S15 Cu2 80.6(3) 2_545 .
Cu2 S15 Cu2 80.6(3) 3_655 .
N1 C1 C2 111(3) . .
C4 C3 N2 105(2) . .
C6 C5 N3 113(2) . .
N4 C6 C5 116(2) . .
C9 C8 N5 107(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 S14 2.139(7) 14
Cu1 S14 2.164(7) .
Cu1 Cu1 2.781(2) 14
Cu1 Cu1 2.781(2) 15_445
Cu1 Cu2 2.872(4) 14
Cu1 Cu2 2.909(4) .
Cu2 S14 2.149(7) .
Cu2 S15 2.154(7) .
Cu2 Cu2 2.787(4) 2_545
Cu2 Cu2 2.787(4) 3_655
Cu2 Cu1 2.872(4) 15_445
In1 S4 2.441(4) .
In1 S2 2.445(4) .
In1 S3 2.448(4) .
In1 S1 2.499(4) .
In2 S6 2.444(4) 2_655
In2 S2 2.452(4) .
In2 S7 2.461(3) .
In2 S5 2.465(3) .
In3 S6 2.439(4) .
In3 S3 2.460(4) .
In3 S8 2.462(3) .
In3 S5 2.465(3) .
In4 S9 2.444(3) .
In4 S4 2.450(4) .
In4 S7 2.458(3) .
In4 S8 2.465(3) .
Cu3 S10 2.327(8) .
Cu3 S5 2.422(3) 3_665
Cu3 S5 2.422(3) 2_655
Cu3 S5 2.422(3) .
Cu4 S10 2.309(3) .
Cu4 S8 2.404(3) .
Cu4 S11 2.405(3) .
Cu4 S7 2.409(3) 3_665
In7 S9 2.445(3) .
In7 S11 2.449(3) 2_655
In7 S11 2.460(3) .
In7 S12 2.463(3) .
In8 S12 2.433(4) .
In8 S12 2.433(4) 3_665
In8 S12 2.433(4) 2_655
In8 S13 2.467(7) .
S6 In2 2.444(4) 3_665
S7 Cu4 2.409(3) 2_655
S10 Cu4 2.309(3) 3_665
S10 Cu4 2.309(3) 2_655
S11 In7 2.449(3) 3_665
S14 Cu1 2.139(7) 15_445
S15 Cu2 2.154(7) 2_545
S15 Cu2 2.154(7) 3_655
N1 C1 1.43(3) .
N2 C3 1.84(5) .
N3 C5 1.57(4) .
N4 C6 1.37(3) .
N5 C8 1.75(7) .
N6 C7 1.71(3) .
C1 C2 1.63(5) .
C3 C4 1.54(4) .
C5 C6 1.57(4) .
C8 C9 1.36(8) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
N3 C5 C6 N4 60(4)
