#------------------------------------------------------------------------------
#$Date: 2016-03-22 13:53:46 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178981 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/04/4120427.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_4120427
loop_
_publ_author_name
'Hua Lin'
'Ling Chen'
'Liu-Jiang Zhou'
'Li-Ming Wu'
_publ_section_title
;
 Functionalization Based on the Substitutional Flexibility: Strong Middle
 IR Nonlinear Optical Selenides AXII4XIII5Se12
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12914
_journal_page_last               12921
_journal_paper_doi               10.1021/ja4074084
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'Cd4 Cs In5 Se12'
_chemical_formula_sum            'Cd4 Cs In5 Se12'
_chemical_formula_weight         2104.13
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_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                   14.864(5)
_cell_length_b                   14.864(5)
_cell_length_c                   10.102(5)
_cell_measurement_reflns_used    2174
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4584
_cell_measurement_theta_min      2.5629
_cell_volume                     1932.9(13)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_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      293(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  Saturn724+
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3528
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    25.946
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8324
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Black-red
_exptl_crystal_density_diffrn    5.423
_exptl_crystal_description       Block
_exptl_crystal_F_000             2700
_exptl_crystal_size_max          0.1200
_exptl_crystal_size_mid          0.1100
_exptl_crystal_size_min          0.1100
_refine_diff_density_max         3.433
_refine_diff_density_min         -0.986
_refine_diff_density_rms         0.309
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         1392
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0417P)²+10.6925P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0641
_reflns_number_gt                1370
_reflns_number_total             1392
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4074084_si_002_5.cif
_cod_data_source_block           CsCd4In5Se12
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4120427
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'
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
Cs1 Cs 0.0000 0.0000 0.99953(13) 0.0350(3) Uani 1 3 d S
Cd1 Cd 0.20547(4) 0.48722(5) 0.08565(7) 0.02008(19) Uani 0.4422(4) 1 d P
In1 In 0.20547(4) 0.48722(5) 0.08565(7) 0.02008(19) Uani 0.5578(4) 1 d P
Cd2 Cd 0.58808(6) 0.02159(7) 0.07917(5) 0.0195(3) Uani 0.456(3) 1 d P
In2 In 0.58808(6) 0.02159(7) 0.07917(5) 0.0195(3) Uani 0.544(3) 1 d P
Cd3 Cd 0.35979(6) 0.10132(5) 0.08084(6) 0.01799(19) Uani 0.435(3) 1 d P
In3 In 0.35979(6) 0.10132(5) 0.08084(6) 0.01799(19) Uani 0.565(3) 1 d P
Se1 Se 0.08080(7) 0.29513(6) 0.00553(9) 0.01763(19) Uani 1 1 d .
Se2 Se 0.55108(6) 0.16940(7) 0.00945(8) 0.0180(2) Uani 1 1 d .
Se3 Se 0.29228(8) 0.22486(9) 0.00244(10) 0.0176(2) Uani 1 1 d .
Se4 Se 0.38433(6) 0.54063(7) 0.97456(8) 0.0176(2) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cd Cd -0.8075 1.2024 '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'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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
Se4 Cs1 Se4 62.80(4) 4_445 5
Se4 Cs1 Se4 62.80(4) 4_445 6_455
Se4 Cs1 Se4 62.80(4) 5 6_455
Se4 Cs1 Se2 176.58(3) 4_445 9
Se4 Cs1 Se2 120.09(3) 5 9
Se4 Cs1 Se2 119.81(3) 6_455 9
Se4 Cs1 Se2 119.81(3) 4_445 7_445
Se4 Cs1 Se2 176.58(3) 5 7_445
Se4 Cs1 Se2 120.09(3) 6_455 7_445
Se2 Cs1 Se2 57.23(4) 9 7_445
Se4 Cs1 Se2 120.09(3) 4_445 8_545
Se4 Cs1 Se2 119.81(3) 5 8_545
Se4 Cs1 Se2 176.58(3) 6_455 8_545
Se2 Cs1 Se2 57.23(4) 9 8_545
Se2 Cs1 Se2 57.23(4) 7_445 8_545
Se4 Cs1 Se1 90.26(2) 4_445 2_556
Se4 Cs1 Se1 120.00(3) 5 2_556
Se4 Cs1 Se1 57.21(2) 6_455 2_556
Se2 Cs1 Se1 89.61(2) 9 2_556
Se2 Cs1 Se1 62.88(2) 7_445 2_556
Se2 Cs1 Se1 120.08(3) 8_545 2_556
Se4 Cs1 Se1 120.00(3) 4_445 1_556
Se4 Cs1 Se1 57.21(2) 5 1_556
Se4 Cs1 Se1 90.26(2) 6_455 1_556
Se2 Cs1 Se1 62.88(2) 9 1_556
Se2 Cs1 Se1 120.08(3) 7_445 1_556
Se2 Cs1 Se1 89.61(2) 8_545 1_556
Se1 Cs1 Se1 119.976(1) 2_556 1_556
Se4 Cs1 Se1 57.22(2) 4_445 3_556
Se4 Cs1 Se1 90.26(2) 5 3_556
Se4 Cs1 Se1 120.00(3) 6_455 3_556
Se2 Cs1 Se1 120.08(3) 9 3_556
Se2 Cs1 Se1 89.61(2) 7_445 3_556
Se2 Cs1 Se1 62.88(2) 8_545 3_556
Se1 Cs1 Se1 119.976(1) 2_556 3_556
Se1 Cs1 Se1 119.976(1) 1_556 3_556
Se4 Cs1 Se3 90.28(2) 4_445 1_556
Se4 Cs1 Se3 57.84(2) 5 1_556
Se4 Cs1 Se3 120.63(3) 6_455 1_556
Se2 Cs1 Se3 90.03(2) 9 1_556
Se2 Cs1 Se3 119.21(3) 7_445 1_556
Se2 Cs1 Se3 61.98(3) 8_545 1_556
Se1 Cs1 Se3 177.06(2) 2_556 1_556
Se1 Cs1 Se3 57.36(2) 1_556 1_556
Se1 Cs1 Se3 62.63(2) 3_556 1_556
Se4 Cs1 Se3 57.84(2) 4_445 3_556
Se4 Cs1 Se3 120.63(3) 5 3_556
Se4 Cs1 Se3 90.28(2) 6_455 3_556
Se2 Cs1 Se3 119.21(3) 9 3_556
Se2 Cs1 Se3 61.98(3) 7_445 3_556
Se2 Cs1 Se3 90.03(2) 8_545 3_556
Se1 Cs1 Se3 62.63(2) 2_556 3_556
Se1 Cs1 Se3 177.06(2) 1_556 3_556
Se1 Cs1 Se3 57.36(2) 3_556 3_556
Se3 Cs1 Se3 119.994(1) 1_556 3_556
Se4 Cs1 Se3 120.63(3) 4_445 2_556
Se4 Cs1 Se3 90.27(2) 5 2_556
Se4 Cs1 Se3 57.84(2) 6_455 2_556
Se2 Cs1 Se3 61.98(2) 9 2_556
Se2 Cs1 Se3 90.03(2) 7_445 2_556
Se2 Cs1 Se3 119.21(3) 8_545 2_556
Se1 Cs1 Se3 57.36(2) 2_556 2_556
Se1 Cs1 Se3 62.63(2) 1_556 2_556
Se1 Cs1 Se3 177.06(2) 3_556 2_556
Se3 Cs1 Se3 119.994(1) 1_556 2_556
Se3 Cs1 Se3 119.994(1) 3_556 2_556
Se2 Cd1 Se4 113.33(4) 4_455 3_564
Se2 Cd1 Se4 112.65(4) 4_455 1_554
Se4 Cd1 Se4 101.95(5) 3_564 1_554
Se2 Cd1 Se1 112.46(4) 4_455 .
Se4 Cd1 Se1 110.94(4) 3_564 .
Se4 Cd1 Se1 104.73(5) 1_554 .
Se4 Cd2 Se3 119.54(4) 2_654 6
Se4 Cd2 Se2 112.93(4) 2_654 .
Se3 Cd2 Se2 101.73(4) 6 .
Se4 Cd2 Se3 106.86(4) 2_654 2_655
Se3 Cd2 Se3 105.34(4) 6 2_655
Se2 Cd2 Se3 110.04(4) . 2_655
Se1 Cd3 Se2 120.25(4) 3 .
Se1 Cd3 Se1 112.08(4) 3 5
Se2 Cd3 Se1 103.43(4) . 5
Se1 Cd3 Se3 103.39(4) 3 .
Se2 Cd3 Se3 111.81(4) . .
Se1 Cd3 Se3 105.11(4) 5 .
In3 Se1 Cd3 0.000(12) 2 2
In3 Se1 In3 103.87(4) 2 9_554
Cd3 Se1 In3 103.87(4) 2 9_554
In3 Se1 Cd3 103.87(4) 2 9_554
Cd3 Se1 Cd3 103.87(4) 2 9_554
In3 Se1 Cd3 0.00(3) 9_554 9_554
In3 Se1 Cd1 103.42(4) 2 .
Cd3 Se1 Cd1 103.42(4) 2 .
In3 Se1 Cd1 105.21(4) 9_554 .
Cd3 Se1 Cd1 105.21(4) 9_554 .
In3 Se1 Cs1 93.77(3) 2 1_554
Cd3 Se1 Cs1 93.77(3) 2 1_554
In3 Se1 Cs1 93.29(4) 9_554 1_554
Cd3 Se1 Cs1 93.29(4) 9_554 1_554
Cd1 Se1 Cs1 150.61(4) . 1_554
Cd3 Se2 In1 103.16(4) . 7_544
Cd3 Se2 Cd1 103.16(4) . 7_544
In1 Se2 Cd1 0.00(3) 7_544 7_544
Cd3 Se2 Cd2 104.30(4) . .
In1 Se2 Cd2 103.24(3) 7_544 .
Cd1 Se2 Cd2 103.24(3) 7_544 .
Cd3 Se2 Cs1 93.72(3) . 4_554
In1 Se2 Cs1 151.04(4) 7_544 4_554
Cd1 Se2 Cs1 151.04(4) 7_544 4_554
Cd2 Se2 Cs1 94.98(3) . 4_554
In2 Se3 Cd2 0.000(2) 8_544 8_544
In2 Se3 Cd3 105.19(4) 8_544 .
Cd2 Se3 Cd3 105.19(4) 8_544 .
In2 Se3 In2 103.44(5) 8_544 3_665
Cd2 Se3 In2 103.44(5) 8_544 3_665
Cd3 Se3 In2 105.64(4) . 3_665
In2 Se3 Cd2 103.44(5) 8_544 3_665
Cd2 Se3 Cd2 103.44(5) 8_544 3_665
Cd3 Se3 Cd2 105.64(4) . 3_665
In2 Se3 Cd2 0.00(4) 3_665 3_665
In2 Se3 Cs1 94.70(4) 8_544 1_554
Cd2 Se3 Cs1 94.70(4) 8_544 1_554
Cd3 Se3 Cs1 93.10(4) . 1_554
In2 Se3 Cs1 149.16(3) 3_665 1_554
Cd2 Se3 Cs1 149.16(3) 3_665 1_554
In2 Se4 Cd2 0.00(3) 3_666 3_666
In2 Se4 In1 103.74(4) 3_666 2_666
Cd2 Se4 In1 103.74(4) 3_666 2_666
In2 Se4 Cd1 103.74(4) 3_666 2_666
Cd2 Se4 Cd1 103.74(4) 3_666 2_666
In1 Se4 Cd1 0.00(3) 2_666 2_666
In2 Se4 Cd1 102.71(4) 3_666 1_556
Cd2 Se4 Cd1 102.71(4) 3_666 1_556
In1 Se4 Cd1 103.91(4) 2_666 1_556
Cd1 Se4 Cd1 103.91(4) 2_666 1_556
In2 Se4 In1 102.71(4) 3_666 1_556
Cd2 Se4 In1 102.71(4) 3_666 1_556
In1 Se4 In1 103.91(4) 2_666 1_556
Cd1 Se4 In1 103.91(4) 2_666 1_556
Cd1 Se4 In1 0.000(15) 1_556 1_556
In2 Se4 Cs1 151.06(3) 3_666 7_554
Cd2 Se4 Cs1 151.06(3) 3_666 7_554
In1 Se4 Cs1 94.42(4) 2_666 7_554
Cd1 Se4 Cs1 94.42(4) 2_666 7_554
Cd1 Se4 Cs1 94.38(4) 1_556 7_554
In1 Se4 Cs1 94.38(4) 1_556 7_554
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cs1 Se4 3.8999(19) 4_445
Cs1 Se4 3.8999(19) 5
Cs1 Se4 3.8999(19) 6_455
Cs1 Se2 3.9214(19) 9
Cs1 Se2 3.9214(19) 7_445
Cs1 Se2 3.9214(19) 8_545
Cs1 Se1 3.9270(16) 2_556
Cs1 Se1 3.9270(16) 1_556
Cs1 Se1 3.9270(16) 3_556
Cs1 Se3 3.9402(17) 1_556
Cs1 Se3 3.9402(17) 3_556
Cs1 Se3 3.9402(17) 2_556
Cd1 Se2 2.6063(17) 4_455
Cd1 Se4 2.6142(12) 3_564
Cd1 Se4 2.6167(12) 1_554
Cd1 Se1 2.6364(13) .
Cd2 Se4 2.5903(14) 2_654
Cd2 Se3 2.6045(18) 6
Cd2 Se2 2.6142(13) .
Cd2 Se3 2.6271(13) 2_655
Cd3 Se1 2.5939(13) 3
Cd3 Se2 2.5983(13) .
Cd3 Se1 2.6169(17) 5
Cd3 Se3 2.6170(12) .
Se1 In3 2.5939(12) 2
Se1 Cd3 2.5939(12) 2
Se1 In3 2.6169(17) 9_554
Se1 Cd3 2.6169(17) 9_554
Se1 Cs1 3.9270(16) 1_554
Se2 In1 2.6063(17) 7_544
Se2 Cd1 2.6063(17) 7_544
Se2 Cs1 3.9214(19) 4_554
Se3 In2 2.6045(18) 8_544
Se3 Cd2 2.6045(18) 8_544
Se3 In2 2.6271(13) 3_665
Se3 Cd2 2.6271(13) 3_665
Se3 Cs1 3.9402(17) 1_554
Se4 In2 2.5903(14) 3_666
Se4 Cd2 2.5903(14) 3_666
Se4 In1 2.6142(12) 2_666
Se4 Cd1 2.6142(12) 2_666
Se4 Cd1 2.6167(12) 1_556
Se4 In1 2.6167(12) 1_556
Se4 Cs1 3.8999(19) 7_554
