#------------------------------------------------------------------------------
#$Date: 2016-03-22 13:53:46 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178981 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/04/4120426.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_4120426
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 In5 Rb Se12'
_chemical_formula_sum            'Cd4 In5 Rb Se12'
_chemical_formula_weight         2056.69
_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                   14.8270(5)
_cell_length_b                   14.8270(5)
_cell_length_c                   10.0747(5)
_cell_measurement_reflns_used    2138
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4546
_cell_measurement_theta_min      2.5697
_cell_volume                     1918.09(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 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3823
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    26.634
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8899
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Black-red
_exptl_crystal_density_diffrn    5.342
_exptl_crystal_description       Block
_exptl_crystal_F_000             2646
_exptl_crystal_size_max          0.1200
_exptl_crystal_size_mid          0.1100
_exptl_crystal_size_min          0.0900
_refine_diff_density_max         1.693
_refine_diff_density_min         -1.384
_refine_diff_density_rms         0.390
_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   1.083
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         1692
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0530P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0687
_reflns_number_gt                1661
_reflns_number_total             1692
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4074084_si_002_4.cif
_cod_data_source_block           RbCd4In5Se12
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4120426
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
Rb1 Rb 0.0000 0.0000 0.9105(2) 0.0561(5) Uani 1 3 d S
Cd1 Cd 0.48720(4) 0.20562(4) 0.82469(6) 0.01712(15) Uani 0.4442(4) 1 d P
In1 In 0.48720(4) 0.20562(4) 0.82469(6) 0.01712(15) Uani 0.5558(4) 1 d P
Cd2 Cd 0.02142(5) 0.58824(5) 0.83178(5) 0.01619(19) Uani 0.397(3) 1 d P
In2 In 0.02142(5) 0.58824(5) 0.83178(5) 0.01619(19) Uani 0.603(3) 1 d P
Cd3 Cd 0.30662(5) 0.07500(5) 0.16256(5) 0.01477(15) Uani 0.492(3) 1 d P
In3 In 0.30662(5) 0.07500(5) 0.16256(5) 0.01477(15) Uani 0.508(3) 1 d P
Se1 Se 0.29405(5) 0.08059(6) 0.90389(8) 0.01490(17) Uani 1 1 d .
Se2 Se 0.04802(6) 0.16303(6) 0.23347(8) 0.01484(17) Uani 1 1 d .
Se3 Se 0.37558(6) 0.26634(6) 0.24113(8) 0.01462(17) Uani 1 1 d .
Se4 Se 0.61538(5) 0.15649(6) 0.93742(8) 0.01484(19) 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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 '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 Rb1 Se4 63.02(4) 9_554 8_544
Se4 Rb1 Se4 63.02(4) 9_554 7_444
Se4 Rb1 Se4 63.02(4) 8_544 7_444
Se4 Rb1 Se2 120.009(14) 9_554 1_556
Se4 Rb1 Se2 119.818(17) 8_544 1_556
Se4 Rb1 Se2 176.35(4) 7_444 1_556
Se4 Rb1 Se2 176.35(4) 9_554 3_556
Se4 Rb1 Se2 120.007(14) 8_544 3_556
Se4 Rb1 Se2 119.817(17) 7_444 3_556
Se2 Rb1 Se2 57.06(4) 1_556 3_556
Se4 Rb1 Se2 119.818(17) 9_554 2_556
Se4 Rb1 Se2 176.35(4) 8_544 2_556
Se4 Rb1 Se2 120.008(14) 7_444 2_556
Se2 Rb1 Se2 57.06(4) 1_556 2_556
Se2 Rb1 Se2 57.06(4) 3_556 2_556
Se4 Rb1 Se1 90.27(3) 9_554 3
Se4 Rb1 Se1 119.97(5) 8_544 3
Se4 Rb1 Se1 56.96(2) 7_444 3
Se2 Rb1 Se1 120.09(5) 1_556 3
Se2 Rb1 Se1 89.70(3) 3_556 3
Se2 Rb1 Se1 63.05(2) 2_556 3
Se4 Rb1 Se1 119.97(5) 9_554 .
Se4 Rb1 Se1 56.96(2) 8_544 .
Se4 Rb1 Se1 90.27(3) 7_444 .
Se2 Rb1 Se1 89.70(3) 1_556 .
Se2 Rb1 Se1 63.05(2) 3_556 .
Se2 Rb1 Se1 120.09(5) 2_556 .
Se1 Rb1 Se1 119.971(2) 3 .
Se4 Rb1 Se1 56.96(2) 9_554 2
Se4 Rb1 Se1 90.27(3) 8_544 2
Se4 Rb1 Se1 119.97(5) 7_444 2
Se2 Rb1 Se1 63.05(2) 1_556 2
Se2 Rb1 Se1 120.09(5) 3_556 2
Se2 Rb1 Se1 89.70(3) 2_556 2
Se1 Rb1 Se1 119.971(2) 3 2
Se1 Rb1 Se1 119.971(2) . 2
Se4 Rb1 Se3 57.79(2) 9_554 7_445
Se4 Rb1 Se3 120.80(5) 8_544 7_445
Se4 Rb1 Se3 90.25(3) 7_444 7_445
Se2 Rb1 Se3 89.97(3) 1_556 7_445
Se2 Rb1 Se3 119.12(5) 3_556 7_445
Se2 Rb1 Se3 62.05(2) 2_556 7_445
Se1 Rb1 Se3 62.682(19) 3 7_445
Se1 Rb1 Se3 176.98(4) . 7_445
Se1 Rb1 Se3 57.313(18) 2 7_445
Se4 Rb1 Se3 90.25(3) 9_554 9
Se4 Rb1 Se3 57.79(2) 8_544 9
Se4 Rb1 Se3 120.80(5) 7_444 9
Se2 Rb1 Se3 62.05(2) 1_556 9
Se2 Rb1 Se3 89.97(3) 3_556 9
Se2 Rb1 Se3 119.12(5) 2_556 9
Se1 Rb1 Se3 176.98(4) 3 9
Se1 Rb1 Se3 57.311(18) . 9
Se1 Rb1 Se3 62.684(19) 2 9
Se3 Rb1 Se3 119.997(1) 7_445 9
Se4 Rb1 Se3 120.80(5) 9_554 8_545
Se4 Rb1 Se3 90.25(3) 8_544 8_545
Se4 Rb1 Se3 57.79(2) 7_444 8_545
Se2 Rb1 Se3 119.12(5) 1_556 8_545
Se2 Rb1 Se3 62.05(2) 3_556 8_545
Se2 Rb1 Se3 89.97(3) 2_556 8_545
Se1 Rb1 Se3 57.313(18) 3 8_545
Se1 Rb1 Se3 62.683(18) . 8_545
Se1 Rb1 Se3 176.98(4) 2 8_545
Se3 Rb1 Se3 119.995(1) 7_445 8_545
Se3 Rb1 Se3 119.994(1) 9 8_545
Se2 Cd1 Se4 113.50(3) 5 .
Se2 Cd1 Se4 112.89(3) 5 3_665
Se4 Cd1 Se4 101.44(4) . 3_665
Se2 Cd1 Se1 112.42(3) 5 .
Se4 Cd1 Se1 110.99(3) . .
Se4 Cd1 Se1 104.78(4) 3_665 .
Se4 Cd2 Se3 120.04(4) 2 4_455
Se4 Cd2 Se2 113.02(3) 2 8
Se3 Cd2 Se2 100.99(3) 4_455 8
Se4 Cd2 Se3 106.96(3) 2 8
Se3 Cd2 Se3 105.17(3) 4_455 8
Se2 Cd2 Se3 110.25(3) 8 8
Se1 Cd3 Se2 120.79(4) 6_554 3
Se1 Cd3 Se3 102.77(3) 6_554 .
Se2 Cd3 Se3 112.13(3) 3 .
Se1 Cd3 Se1 112.07(3) 6_554 1_554
Se2 Cd3 Se1 103.08(3) 3 1_554
Se3 Cd3 Se1 105.24(3) . 1_554
In3 Se1 Cd3 0.0 8_545 8_545
In3 Se1 In3 103.68(3) 8_545 1_556
Cd3 Se1 In3 103.68(3) 8_545 1_556
In3 Se1 Cd3 103.68(3) 8_545 1_556
Cd3 Se1 Cd3 103.68(3) 8_545 1_556
In3 Se1 Cd3 0.00(3) 1_556 1_556
In3 Se1 Cd1 103.23(3) 8_545 .
Cd3 Se1 Cd1 103.23(3) 8_545 .
In3 Se1 Cd1 104.70(3) 1_556 .
Cd3 Se1 Cd1 104.70(3) 1_556 .
In3 Se1 Rb1 94.08(3) 8_545 .
Cd3 Se1 Rb1 94.08(3) 8_545 .
In3 Se1 Rb1 93.42(4) 1_556 .
Cd3 Se1 Rb1 93.42(4) 1_556 .
Cd1 Se1 Rb1 150.92(4) . .
In3 Se2 Cd3 0.000(13) 2 2
In3 Se2 Cd1 102.95(3) 2 9_554
Cd3 Se2 Cd1 102.95(3) 2 9_554
In3 Se2 In1 102.95(3) 2 9_554
Cd3 Se2 In1 102.95(3) 2 9_554
Cd1 Se2 In1 0.00(3) 9_554 9_554
In3 Se2 Cd2 104.20(3) 2 6_454
Cd3 Se2 Cd2 104.20(3) 2 6_454
Cd1 Se2 Cd2 102.67(3) 9_554 6_454
In1 Se2 Cd2 102.67(3) 9_554 6_454
In3 Se2 In2 104.20(3) 2 6_454
Cd3 Se2 In2 104.20(3) 2 6_454
Cd1 Se2 In2 102.67(3) 9_554 6_454
In1 Se2 In2 102.67(3) 9_554 6_454
Cd2 Se2 In2 0.00(6) 6_454 6_454
In3 Se2 Rb1 93.84(3) 2 1_554
Cd3 Se2 Rb1 93.84(3) 2 1_554
Cd1 Se2 Rb1 151.38(4) 9_554 1_554
In1 Se2 Rb1 151.38(4) 9_554 1_554
Cd2 Se2 Rb1 95.31(3) 6_454 1_554
In2 Se2 Rb1 95.31(3) 6_454 1_554
In2 Se3 Cd2 0.00(3) 7_544 7_544
In2 Se3 Cd3 105.16(3) 7_544 .
Cd2 Se3 Cd3 105.16(3) 7_544 .
In2 Se3 In2 102.86(3) 7_544 6_454
Cd2 Se3 In2 102.86(3) 7_544 6_454
Cd3 Se3 In2 105.20(3) . 6_454
In2 Se3 Cd2 102.86(3) 7_544 6_454
Cd2 Se3 Cd2 102.86(3) 7_544 6_454
Cd3 Se3 Cd2 105.20(3) . 6_454
In2 Se3 Cd2 0.000(12) 6_454 6_454
In2 Se3 Rb1 95.12(4) 7_544 4_554
Cd2 Se3 Rb1 95.12(4) 7_544 4_554
Cd3 Se3 Rb1 93.49(3) . 4_554
In2 Se3 Rb1 149.39(3) 6_454 4_554
Cd2 Se3 Rb1 149.39(3) 6_454 4_554
In2 Se4 Cd2 0.000(17) 3 3
In2 Se4 Cd1 103.59(3) 3 .
Cd2 Se4 Cd1 103.59(3) 3 .
In2 Se4 Cd1 102.15(3) 3 2_655
Cd2 Se4 Cd1 102.15(3) 3 2_655
Cd1 Se4 Cd1 103.60(3) . 2_655
In2 Se4 In1 102.15(3) 3 2_655
Cd2 Se4 In1 102.15(3) 3 2_655
Cd1 Se4 In1 103.60(3) . 2_655
Cd1 Se4 In1 0.00(3) 2_655 2_655
In2 Se4 Rb1 151.37(3) 3 4
Cd2 Se4 Rb1 151.37(3) 3 4
Cd1 Se4 Rb1 94.69(3) . 4
Cd1 Se4 Rb1 94.58(3) 2_655 4
In1 Se4 Rb1 94.58(3) 2_655 4
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rb1 Se4 3.872(2) 9_554
Rb1 Se4 3.872(2) 8_544
Rb1 Se4 3.872(2) 7_444
Rb1 Se2 3.901(2) 1_556
Rb1 Se2 3.901(2) 3_556
Rb1 Se2 3.901(2) 2_556
Rb1 Se1 3.9027(7) 3
Rb1 Se1 3.9027(7) .
Rb1 Se1 3.9027(7) 2
Rb1 Se3 3.9150(8) 7_445
Rb1 Se3 3.9150(8) 9
Rb1 Se3 3.9151(8) 8_545
Cd1 Se2 2.6075(10) 5
Cd1 Se4 2.6110(8) .
Cd1 Se4 2.6174(9) 3_665
Cd1 Se1 2.6393(8) .
Cd2 Se4 2.5904(9) 2
Cd2 Se3 2.6061(11) 4_455
Cd2 Se2 2.6151(8) 8
Cd2 Se3 2.6279(8) 8
Cd3 Se1 2.5924(9) 6_554
Cd3 Se2 2.5937(9) 3
Cd3 Se3 2.6116(9) .
Cd3 Se1 2.6170(11) 1_554
Se1 In3 2.5925(9) 8_545
Se1 Cd3 2.5925(9) 8_545
Se1 In3 2.6170(11) 1_556
Se1 Cd3 2.6170(11) 1_556
Se2 In3 2.5937(9) 2
Se2 Cd3 2.5937(9) 2
Se2 Cd1 2.6075(10) 9_554
Se2 In1 2.6075(10) 9_554
Se2 Cd2 2.6151(8) 6_454
Se2 In2 2.6151(8) 6_454
Se2 Rb1 3.901(2) 1_554
Se3 In2 2.6061(11) 7_544
Se3 Cd2 2.6061(11) 7_544
Se3 In2 2.6280(8) 6_454
Se3 Cd2 2.6280(8) 6_454
Se3 Rb1 3.9150(8) 4_554
Se4 In2 2.5904(9) 3
Se4 Cd2 2.5904(9) 3
Se4 Cd1 2.6174(9) 2_655
Se4 In1 2.6174(9) 2_655
Se4 Rb1 3.872(2) 4
