#------------------------------------------------------------------------------
#$Date: 2019-11-23 13:31:58 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233453 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/88/4348874.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_4348874
loop_
_publ_author_name
'Yue, Cheng-Yang'
'Lei, Xiao-Wu'
'Han, Yong-Fang'
'Lu, Xin-Xiu'
'Tian, Ya-Wei'
'Xu, Jing'
'Liu, Xiao-Fan'
'Xu, Xin'
_publ_section_title
;
 Transition-Metal-Complex Cationic Dyes Photosensitive to Two Types of 2D
 Layered Silver Bromides with Visible-Light-Driven Photocatalytic
 Properties.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              12193
_journal_page_last               12203
_journal_paper_doi               10.1021/acs.inorgchem.6b01770
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         C60N12H48Co2KAg6Br11
_chemical_formula_sum            'C60 H48 Ag6 Br11 Co2 K N12'
_chemical_formula_weight         2620.29
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_cell_setting           trigonal
_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            3
_cell_length_a                   14.1784(14)
_cell_length_b                   14.1784(14)
_cell_length_c                   30.746(3)
_cell_measurement_reflns_used    5994
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.87
_cell_volume                     5352.7(9)
_computing_cell_refinement       'APEX2 Software Suite (Bruker,2005)'
_computing_data_collection       'APEX2 Software Suite (Bruker,2005)'
_computing_data_reduction        'APEX2 Software Suite (Bruker,2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART 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  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            20590
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    8.328
_exptl_absorpt_correction_T_max  0.6809
_exptl_absorpt_correction_T_min  0.5555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3696
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.643
_refine_diff_density_min         -0.940
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         2718
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0205P)²+28.9623P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0691
_reflns_number_gt                2153
_reflns_number_total             2718
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01770_si_003.cif
_cod_data_source_block           C60N12H48Co2KAg6Br11
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4348874
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
K1 K 1.0000 0.0000 0.0000 0.098(3) Uani 1 6 d SPU
Ag1 Ag 0.90986(3) 0.05231(3) 0.130445(12) 0.05541(12) Uani 1 1 d .
Co1 Co 1.0000 0.0000 0.37745(2) 0.02335(17) Uani 1 3 d S
Br3 Br 1.0000 0.0000 0.20280(2) 0.04350(18) Uani 1 3 d S
Br2 Br 1.08116(4) 0.20771(5) 0.083479(18) 0.06346(16) Uani 1 1 d U
Br1 Br 0.8333 0.1667 0.1667 0.0843(3) Uani 1 2 d S
N1 N 0.8560(2) -0.0497(2) 0.41294(9) 0.0316(7) Uani 1 1 d .
N2 N 0.9765(2) 0.1119(3) 0.34233(9) 0.0325(7) Uani 1 1 d .
C6 C 0.7896(3) -0.1939(3) 0.36081(12) 0.0347(8) Uani 1 1 d .
C5 C 0.7717(3) -0.1465(3) 0.40054(12) 0.0344(8) Uani 1 1 d .
C10 C 0.9230(3) 0.0926(4) 0.30446(13) 0.0447(10) Uani 1 1 d .
H10 H 0.8956 0.0244 0.2917 0.054 Uiso 1 1 calc .
C7 C 0.7109(4) -0.2892(4) 0.34189(16) 0.0539(12) Uani 1 1 d .
H7 H 0.6435 -0.3302 0.3553 0.065 Uiso 1 1 calc .
C1 C 0.8410(3) 0.0023(4) 0.44614(13) 0.0429(9) Uani 1 1 d .
H1 H 0.8989 0.0693 0.4547 0.051 Uiso 1 1 calc .
C2 C 0.7438(4) -0.0389(4) 0.46835(14) 0.0520(11) Uani 1 1 d .
H2 H 0.7354 0.0008 0.4906 0.062 Uiso 1 1 calc .
C3 C 0.6606(4) -0.1386(5) 0.45699(16) 0.0582(13) Uani 1 1 d .
H3 H 0.5950 -0.1692 0.4721 0.070 Uiso 1 1 calc .
C8 C 0.7320(5) -0.3234(4) 0.30339(18) 0.0668(15) Uani 1 1 d .
H8 H 0.6793 -0.3879 0.2906 0.080 Uiso 1 1 calc .
C4 C 0.6739(3) -0.1938(4) 0.42321(15) 0.0523(11) Uani 1 1 d .
H4 H 0.6177 -0.2625 0.4155 0.063 Uiso 1 1 calc .
C9 C 0.9068(4) 0.1688(4) 0.28380(15) 0.0568(13) Uani 1 1 d .
H9 H 0.8711 0.1536 0.2572 0.068 Uiso 1 1 calc .
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'
K K 0.2009 0.2494 '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'
Co Co 0.3494 0.9721 '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'
Ag Ag -0.8971 1.1015 '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
Br2 K1 Br2 180.0 . 10_755
Br2 K1 Br2 104.409(13) . 12_545
Br2 K1 Br2 75.591(13) 10_755 12_545
Br2 K1 Br2 75.591(13) . 3_765
Br2 K1 Br2 104.409(13) 10_755 3_765
Br2 K1 Br2 180.00(2) 12_545 3_765
Br2 K1 Br2 75.591(13) . 2_645
Br2 K1 Br2 104.409(13) 10_755 2_645
Br2 K1 Br2 104.409(13) 12_545 2_645
Br2 K1 Br2 75.591(13) 3_765 2_645
Br2 K1 Br2 104.409(13) . 11_665
Br2 K1 Br2 75.591(13) 10_755 11_665
Br2 K1 Br2 75.591(13) 12_545 11_665
Br2 K1 Br2 104.409(13) 3_765 11_665
Br2 K1 Br2 180.000(12) 2_645 11_665
Br1 Ag1 Br2 124.576(19) . 2_645
Br1 Ag1 Br2 101.678(17) . .
Br2 Ag1 Br2 111.24(3) 2_645 .
Br1 Ag1 Br3 102.066(16) . .
Br2 Ag1 Br3 108.992(17) 2_645 .
Br2 Ag1 Br3 106.811(18) . .
Br1 Ag1 Ag1 150.981(13) . 2_645
Br2 Ag1 Ag1 56.584(16) 2_645 2_645
Br2 Ag1 Ag1 103.929(15) . 2_645
Br3 Ag1 Ag1 57.374(9) . 2_645
Br1 Ag1 Ag1 129.546(18) . 3_765
Br2 Ag1 Ag1 105.873(16) 2_645 3_765
Br2 Ag1 Ag1 54.191(16) . 3_765
Br3 Ag1 Ag1 57.374(9) . 3_765
Ag1 Ag1 Ag1 60.0 2_645 3_765
N2 Co1 N2 95.48(11) . 2_645
N2 Co1 N2 95.49(11) . 3_765
N2 Co1 N2 95.49(11) 2_645 3_765
N2 Co1 N1 78.18(12) . 3_765
N2 Co1 N1 171.02(12) 2_645 3_765
N2 Co1 N1 91.48(12) 3_765 3_765
N2 Co1 N1 171.02(12) . 2_645
N2 Co1 N1 91.48(12) 2_645 2_645
N2 Co1 N1 78.17(12) 3_765 2_645
N1 Co1 N1 95.49(11) 3_765 2_645
N2 Co1 N1 91.48(12) . .
N2 Co1 N1 78.18(12) 2_645 .
N2 Co1 N1 171.02(12) 3_765 .
N1 Co1 N1 95.49(11) 3_765 .
N1 Co1 N1 95.49(11) 2_645 .
Ag1 Br3 Ag1 65.249(19) 2_645 3_765
Ag1 Br3 Ag1 65.248(19) 2_645 .
Ag1 Br3 Ag1 65.249(19) 3_765 .
Ag1 Br2 Ag1 69.23(2) 3_765 .
Ag1 Br2 K1 86.894(18) 3_765 .
Ag1 Br2 K1 85.770(18) . .
Ag1 Br1 Ag1 180.0 . 13_655
C1 N1 C5 118.3(3) . .
C1 N1 Co1 127.4(3) . .
C5 N1 Co1 114.3(2) . .
C10 N2 C6 118.8(3) . 3_765
C10 N2 Co1 125.8(3) . .
C6 N2 Co1 115.4(2) 3_765 .
N2 C6 C7 120.6(4) 2_645 .
N2 C6 C5 115.5(3) 2_645 .
C7 C6 C5 123.8(4) . .
N1 C5 C4 120.8(4) . .
N1 C5 C6 115.6(3) . .
C4 C5 C6 123.6(4) . .
N2 C10 C9 122.9(4) . .
N2 C10 H10 118.5 . .
C9 C10 H10 118.5 . .
C8 C7 C6 120.0(4) . .
C8 C7 H7 120.0 . .
C6 C7 H7 120.0 . .
N1 C1 C2 123.1(4) . .
N1 C1 H1 118.5 . .
C2 C1 H1 118.5 . .
C3 C2 C1 118.5(4) . .
C3 C2 H2 120.8 . .
C1 C2 H2 120.8 . .
C2 C3 C4 119.6(4) . .
C2 C3 H3 120.2 . .
C4 C3 H3 120.2 . .
C7 C8 C9 119.5(4) . 2_645
C7 C8 H8 120.3 . .
C9 C8 H8 120.3 2_645 .
C3 C4 C5 119.7(4) . .
C3 C4 H4 120.2 . .
C5 C4 H4 120.2 . .
C10 C9 C8 118.2(4) . 3_765
C10 C9 H9 120.9 . .
C8 C9 H9 120.9 3_765 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K1 Br2 3.6326(7) .
K1 Br2 3.6327(7) 10_755
K1 Br2 3.6327(7) 12_545
K1 Br2 3.6327(7) 3_765
K1 Br2 3.6327(7) 2_645
K1 Br2 3.6327(7) 11_665
Ag1 Br1 2.6087(4) .
Ag1 Br2 2.6585(6) 2_645
Ag1 Br2 2.7363(6) .
Ag1 Br3 2.8427(7) .
Ag1 Ag1 3.0651(7) 2_645
Ag1 Ag1 3.0651(7) 3_765
Co1 N2 2.079(3) .
Co1 N2 2.079(3) 2_645
Co1 N2 2.079(3) 3_765
Co1 N1 2.102(3) 3_765
Co1 N1 2.102(3) 2_645
Co1 N1 2.102(3) .
Br3 Ag1 2.8426(7) 2_645
Br3 Ag1 2.8426(7) 3_765
Br2 Ag1 2.6586(6) 3_765
Br1 Ag1 2.6088(4) 13_655
N1 C1 1.337(5) .
N1 C5 1.348(5) .
N2 C10 1.341(5) .
N2 C6 1.343(5) 3_765
C6 N2 1.343(5) 2_645
C6 C7 1.379(6) .
C6 C5 1.475(5) .
C5 C4 1.389(6) .
C10 C9 1.368(6) .
C10 H10 0.9300 .
C7 C8 1.368(7) .
C7 H7 0.9300 .
C1 C2 1.380(6) .
C1 H1 0.9300 .
C2 C3 1.358(7) .
C2 H2 0.9300 .
C3 C4 1.369(7) .
C3 H3 0.9300 .
C8 C9 1.369(7) 2_645
C8 H8 0.9300 .
C4 H4 0.9300 .
C9 C8 1.369(7) 3_765
C9 H9 0.9300 .
