#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:05:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179092 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/54/4305435.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_4305435
loop_
_publ_author_name
'Jiyong Yao'
'Daniel M. Wells'
'George H. Chan'
'Hui-Yi Zeng'
'Donald E. Ellis'
'Richard P. Van Duyne'
'James A. Ibers'
_publ_contact_author_address
;
        Department of Chemistry
        Northwestern University
        2145 Sheridan Road
        Evanston, IL 60208-3113, USA
;
_publ_contact_author_email       ibers@chem.northwestern.edu
_publ_contact_author_fax         '+1 847 491 2976'
_publ_contact_author_name        'James A. Ibers'
_publ_contact_author_phone       '+1 847 491 5449'
_publ_section_title
;
Syntheses, Structures, Physical Properties, and Electronic Properties of
Some AMUQ3 Compounds (A = Alkali Metal, M = Cu or Ag, Q = S or Se)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6873
_journal_page_last               6879
_journal_paper_doi               10.1021/ic800424t
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'Cu Rb S3 U'
_chemical_formula_weight         483.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   none
_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                   3.9885(4)
_cell_length_b                   14.3991(16)
_cell_length_c                   10.2961(12)
_cell_measurement_temperature    153(2)
_cell_volume                     591.31(11)
_computing_cell_refinement       'SMART Version 5.054 (Bruker, 2000)'
_computing_data_collection       'SMART Version 5.054 (Bruker, 2000)'
_computing_data_reduction        'Saint-Plus Version 6.45a (Bruker, 2003)'
_computing_molecular_graphics    'CrystalMaker, 2005'
_computing_publication_material  'SHELXTL (Sheldrick, 2003)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2003)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2003)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       '0.3°ω 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  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3505
_diffrn_reflns_theta_full        28.62
_diffrn_reflns_theta_max         28.62
_diffrn_reflns_theta_min         2.83
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    40.030
_exptl_absorpt_correction_T_max  0.66997
_exptl_absorpt_correction_T_min  0.07654
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   face-indexed
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    5.428
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.026
_exptl_crystal_size_min          0.010
_refine_diff_density_max         3.939
_refine_diff_density_min         -1.935
_refine_diff_density_rms         0.461
_refine_ls_extinction_coef       0.00006(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.494
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     24
_refine_ls_number_reflns         449
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.494
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0300P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0618
_refine_ls_wR_factor_ref         0.0635
_reflns_number_gt                421
_reflns_number_total             449
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800424t-file012_1.cif
_cod_data_source_block           RbCuUS3
_cod_database_code               4305435
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Rb Rb 0.0000 0.74197(7) 0.2500 0.0115(3) Uani 1 4 d S . .
U U 0.0000 0.0000 0.0000 0.00522(19) Uani 1 4 d S . .
Cu Cu 0.0000 0.46497(9) 0.2500 0.0100(3) Uani 1 4 d S . .
S1 S 0.0000 0.05852(17) 0.2500 0.0060(5) Uani 1 4 d S . .
S2 S 0.0000 0.37889(11) 0.05901(18) 0.0077(4) Uani 1 2 d S . .
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'
Cu Cu 0.3201 1.2651 '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'
U U -9.6767 9.6646 '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
_geom_angle_publ_flag
S1 Rb S1 74.10(6) 5_455 5 ?
S1 Rb S2 144.12(3) 5_455 14_556 ?
S1 Rb S2 96.23(3) 5 14_556 ?
S1 Rb S2 96.23(3) 5_455 14_456 ?
S1 Rb S2 144.12(3) 5 14_456 ?
S2 Rb S2 71.22(4) 14_556 14_456 ?
S1 Rb S2 144.12(3) 5_455 5 ?
S1 Rb S2 96.23(3) 5 5 ?
S2 Rb S2 70.08(6) 14_556 5 ?
S2 Rb S2 109.71(6) 14_456 5 ?
S1 Rb S2 96.23(3) 5_455 5_455 ?
S1 Rb S2 144.12(3) 5 5_455 ?
S2 Rb S2 109.71(6) 14_556 5_455 ?
S2 Rb S2 70.08(6) 14_456 5_455 ?
S2 Rb S2 71.22(4) 5 5_455 ?
S1 Rb S2 67.48(3) 5_455 9_565 ?
S1 Rb S2 67.48(3) 5 9_565 ?
S2 Rb S2 141.26(3) 14_556 9_565 ?
S2 Rb S2 141.26(3) 14_456 9_565 ?
S2 Rb S2 76.85(4) 5 9_565 ?
S2 Rb S2 76.85(4) 5_455 9_565 ?
S1 Rb S2 67.48(3) 5_455 2_565 ?
S1 Rb S2 67.48(3) 5 2_565 ?
S2 Rb S2 76.85(4) 14_556 2_565 ?
S2 Rb S2 76.85(4) 14_456 2_565 ?
S2 Rb S2 141.26(3) 5 2_565 ?
S2 Rb S2 141.26(3) 5_455 2_565 ?
S2 Rb S2 122.64(6) 9_565 2_565 ?
S1 Rb Cu 174.79(3) 5_455 5 ?
S1 Rb Cu 111.10(3) 5 5 ?
S2 Rb Cu 37.23(3) 14_556 5 ?
S2 Rb Cu 79.53(3) 14_456 5 ?
S2 Rb Cu 37.23(3) 5 5 ?
S2 Rb Cu 79.53(3) 5_455 5 ?
S2 Rb Cu 114.06(2) 9_565 5 ?
S2 Rb Cu 114.06(2) 2_565 5 ?
S1 Rb Cu 111.10(3) 5_455 5_455 ?
S1 Rb Cu 174.79(3) 5 5_455 ?
S2 Rb Cu 79.53(3) 14_556 5_455 ?
S2 Rb Cu 37.23(3) 14_456 5_455 ?
S2 Rb Cu 79.53(3) 5 5_455 ?
S2 Rb Cu 37.23(3) 5_455 5_455 ?
S2 Rb Cu 114.06(2) 9_565 5_455 ?
S2 Rb Cu 114.06(2) 2_565 5_455 ?
Cu Rb Cu 63.69(3) 5 5_455 ?
S1 Rb Rb 127.05(3) 5_455 1_655 ?
S1 Rb Rb 52.95(3) 5 1_655 ?
S2 Rb Rb 54.390(19) 14_556 1_655 ?
S2 Rb Rb 125.609(19) 14_456 1_655 ?
S2 Rb Rb 54.390(19) 5 1_655 ?
S2 Rb Rb 125.609(19) 5_455 1_655 ?
S2 Rb Rb 90.0 9_565 1_655 ?
S2 Rb Rb 90.0 2_565 1_655 ?
Cu Rb Rb 58.156(14) 5 1_655 ?
Cu Rb Rb 121.843(14) 5_455 1_655 ?
S1 Rb Rb 52.95(3) 5_455 1_455 ?
S1 Rb Rb 127.05(3) 5 1_455 ?
S2 Rb Rb 125.609(19) 14_556 1_455 ?
S2 Rb Rb 54.390(19) 14_456 1_455 ?
S2 Rb Rb 125.609(19) 5 1_455 ?
S2 Rb Rb 54.390(19) 5_455 1_455 ?
S2 Rb Rb 90.0 9_565 1_455 ?
S2 Rb Rb 90.0 2_565 1_455 ?
Cu Rb Rb 121.843(14) 5 1_455 ?
Cu Rb Rb 58.156(14) 5_455 1_455 ?
Rb Rb Rb 180.0 1_655 1_455 ?
S1 U S1 180.000(1) . 9 ?
S1 U S2 90.73(5) . 13 ?
S1 U S2 89.27(5) 9 13 ?
S1 U S2 89.27(5) . 5_445 ?
S1 U S2 90.73(5) 9 5_445 ?
S2 U S2 180.00(5) 13 5_445 ?
S1 U S2 90.73(5) . 13_455 ?
S1 U S2 89.27(5) 9 13_455 ?
S2 U S2 94.40(5) 13 13_455 ?
S2 U S2 85.60(5) 5_445 13_455 ?
S1 U S2 89.27(5) . 5_545 ?
S1 U S2 90.73(5) 9 5_545 ?
S2 U S2 85.60(5) 13 5_545 ?
S2 U S2 94.40(5) 5_445 5_545 ?
S2 U S2 180.00(5) 13_455 5_545 ?
S1 U Cu 134.01(3) . 13_455 ?
S1 U Cu 45.99(3) 9 13_455 ?
S2 U Cu 99.86(4) 13 13_455 ?
S2 U Cu 80.14(4) 5_445 13_455 ?
S2 U Cu 44.20(4) 13_455 13_455 ?
S2 U Cu 135.80(4) 5_545 13_455 ?
S1 U Cu 45.99(3) . 5_545 ?
S1 U Cu 134.01(3) 9 5_545 ?
S2 U Cu 80.14(4) 13 5_545 ?
S2 U Cu 99.86(4) 5_445 5_545 ?
S2 U Cu 135.80(4) 13_455 5_545 ?
S2 U Cu 44.20(4) 5_545 5_545 ?
Cu U Cu 180.00(5) 13_455 5_545 ?
S1 U Cu 134.01(3) . 13 ?
S1 U Cu 45.99(3) 9 13 ?
S2 U Cu 44.20(4) 13 13 ?
S2 U Cu 135.80(4) 5_445 13 ?
S2 U Cu 99.86(4) 13_455 13 ?
S2 U Cu 80.14(4) 5_545 13 ?
Cu U Cu 74.491(10) 13_455 13 ?
Cu U Cu 105.509(10) 5_545 13 ?
S1 U Cu 45.99(3) . 5_445 ?
S1 U Cu 134.01(3) 9 5_445 ?
S2 U Cu 135.80(4) 13 5_445 ?
S2 U Cu 44.20(4) 5_445 5_445 ?
S2 U Cu 80.14(4) 13_455 5_445 ?
S2 U Cu 99.86(4) 5_545 5_445 ?
Cu U Cu 105.509(10) 13_455 5_445 ?
Cu U Cu 74.491(10) 5_545 5_445 ?
Cu U Cu 180.00(5) 13 5_445 ?
S1 U U 90.0 . 1_655 ?
S1 U U 90.0 9 1_655 ?
S2 U U 42.80(3) 13 1_655 ?
S2 U U 137.20(3) 5_445 1_655 ?
S2 U U 137.20(3) 13_455 1_655 ?
S2 U U 42.80(3) 5_545 1_655 ?
Cu U U 127.246(5) 13_455 1_655 ?
Cu U U 52.754(5) 5_545 1_655 ?
Cu U U 52.754(5) 13 1_655 ?
Cu U U 127.246(5) 5_445 1_655 ?
S1 U U 90.0 . 1_455 ?
S1 U U 90.0 9 1_455 ?
S2 U U 137.20(3) 13 1_455 ?
S2 U U 42.80(3) 5_445 1_455 ?
S2 U U 42.80(3) 13_455 1_455 ?
S2 U U 137.20(3) 5_545 1_455 ?
Cu U U 52.754(5) 13_455 1_455 ?
Cu U U 127.246(5) 5_545 1_455 ?
Cu U U 127.246(5) 13 1_455 ?
Cu U U 52.754(5) 5_445 1_455 ?
U U U 180.0 1_655 1_455 ?
S2 Cu S2 115.56(11) . 10_556 ?
S2 Cu S1 107.37(3) . 5 ?
S2 Cu S1 107.37(3) 10_556 5 ?
S2 Cu S1 107.37(3) . 5_455 ?
S2 Cu S1 107.37(3) 10_556 5_455 ?
S1 Cu S1 111.92(11) 5 5_455 ?
S2 Cu U 137.95(3) . 6 ?
S2 Cu U 54.60(3) 10_556 6 ?
S1 Cu U 54.040(15) 5 6 ?
S1 Cu U 114.57(4) 5_455 6 ?
S2 Cu U 54.60(3) . 5_455 ?
S2 Cu U 137.95(3) 10_556 5_455 ?
S1 Cu U 114.57(4) 5 5_455 ?
S1 Cu U 54.040(15) 5_455 5_455 ?
U Cu U 162.39(5) 6 5_455 ?
S2 Cu U 137.95(3) . 6_455 ?
S2 Cu U 54.60(3) 10_556 6_455 ?
S1 Cu U 114.57(4) 5 6_455 ?
S1 Cu U 54.040(15) 5_455 6_455 ?
U Cu U 74.491(10) 6 6_455 ?
U Cu U 102.739(12) 5_455 6_455 ?
S2 Cu U 54.60(3) . 5 ?
S2 Cu U 137.95(3) 10_556 5 ?
S1 Cu U 54.040(15) 5 5 ?
S1 Cu U 114.57(4) 5_455 5 ?
U Cu U 102.739(13) 6 5 ?
U Cu U 74.491(10) 5_455 5 ?
U Cu U 162.39(5) 6_455 5 ?
S2 Cu Rb 63.07(4) . 5_445 ?
S2 Cu Rb 63.07(4) 10_556 5_445 ?
S1 Cu Rb 155.88(6) 5 5_445 ?
S1 Cu Rb 92.20(5) 5_455 5_445 ?
U Cu Rb 116.70(3) 6 5_445 ?
U Cu Rb 79.090(16) 5_455 5_445 ?
U Cu Rb 79.090(16) 6_455 5_445 ?
U Cu Rb 116.70(3) 5 5_445 ?
S2 Cu Rb 63.07(4) . 5_545 ?
S2 Cu Rb 63.07(4) 10_556 5_545 ?
S1 Cu Rb 92.20(5) 5 5_545 ?
S1 Cu Rb 155.88(6) 5_455 5_545 ?
U Cu Rb 79.090(16) 6 5_545 ?
U Cu Rb 116.70(3) 5_455 5_545 ?
U Cu Rb 116.70(3) 6_455 5_545 ?
U Cu Rb 79.090(16) 5 5_545 ?
Rb Cu Rb 63.69(3) 5_445 5_545 ?
S2 Cu Rb 122.22(5) . . ?
S2 Cu Rb 122.22(5) 10_556 . ?
S1 Cu Rb 55.96(6) 5 . ?
S1 Cu Rb 55.96(6) 5_455 . ?
U Cu Rb 81.19(2) 6 . ?
U Cu Rb 81.19(2) 5_455 . ?
U Cu Rb 81.19(2) 6_455 . ?
U Cu Rb 81.19(2) 5 . ?
Rb Cu Rb 148.156(14) 5_445 . ?
Rb Cu Rb 148.156(14) 5_545 . ?
Cu S1 Cu 111.92(11) 5_445 5_545 ?
Cu S1 U 79.97(4) 5_445 . ?
Cu S1 U 79.97(4) 5_545 . ?
Cu S1 U 79.97(4) 5_445 2 ?
Cu S1 U 79.97(4) 5_545 2 ?
U S1 U 143.74(10) . 2 ?
Cu S1 Rb 161.09(8) 5_445 5_545 ?
Cu S1 Rb 86.99(4) 5_545 5_545 ?
U S1 Rb 104.38(3) . 5_545 ?
U S1 Rb 104.38(3) 2 5_545 ?
Cu S1 Rb 86.99(4) 5_445 5_445 ?
Cu S1 Rb 161.09(8) 5_545 5_445 ?
U S1 Rb 104.38(3) . 5_445 ?
U S1 Rb 104.38(3) 2 5_445 ?
Rb S1 Rb 74.10(6) 5_545 5_445 ?
Cu S2 U 81.20(5) . 5 ?
Cu S2 U 81.20(5) . 5_455 ?
U S2 U 94.40(5) 5 5_455 ?
Cu S2 Rb 79.70(5) . 5_445 ?
U S2 Rb 157.65(6) 5 5_445 ?
U S2 Rb 94.04(2) 5_455 5_445 ?
Cu S2 Rb 79.70(5) . 5_545 ?
U S2 Rb 94.04(2) 5 5_545 ?
U S2 Rb 157.65(6) 5_455 5_545 ?
Rb S2 Rb 71.22(4) 5_445 5_545 ?
Cu S2 Rb 176.46(8) . 9_565 ?
U S2 Rb 96.42(5) 5 9_565 ?
U S2 Rb 96.42(5) 5_455 9_565 ?
Rb S2 Rb 103.15(4) 5_445 9_565 ?
Rb S2 Rb 103.15(4) 5_545 9_565 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rb S1 3.310(2) 5_455 ?
Rb S1 3.310(2) 5 ?
Rb S2 3.4251(16) 14_556 ?
Rb S2 3.4251(15) 14_456 ?
Rb S2 3.4251(16) 5 ?
Rb S2 3.4251(15) 5_455 ?
Rb S2 3.6264(19) 9_565 ?
Rb S2 3.6264(19) 2_565 ?
Rb Cu 3.7798(14) 5 ?
Rb Cu 3.7798(14) 5_455 ?
Rb Rb 3.9885(4) 1_655 ?
Rb Rb 3.9885(4) 1_455 ?
U S1 2.7085(8) . ?
U S1 2.7085(8) 9 ?
U S2 2.7179(12) 13 ?
U S2 2.7179(12) 5_445 ?
U S2 2.7179(12) 13_455 ?
U S2 2.7179(12) 5_545 ?
U Cu 3.2950(3) 13_455 ?
U Cu 3.2950(3) 5_545 ?
U Cu 3.2950(3) 13 ?
U Cu 3.2950(3) 5_445 ?
U U 3.9885(4) 1_655 ?
U U 3.9885(4) 1_455 ?
Cu S2 2.3244(19) . ?
Cu S2 2.3245(19) 10_556 ?
Cu S1 2.4066(16) 5 ?
Cu S1 2.4066(16) 5_455 ?
Cu U 3.2950(3) 6 ?
Cu U 3.2950(3) 5_455 ?
Cu U 3.2950(3) 6_455 ?
Cu U 3.2950(3) 5 ?
Cu Rb 3.7798(14) 5_445 ?
Cu Rb 3.7798(14) 5_545 ?
S1 Cu 2.4066(16) 5_445 ?
S1 Cu 2.4066(16) 5_545 ?
S1 U 2.7085(8) 2 ?
S1 Rb 3.310(2) 5_545 ?
S1 Rb 3.310(2) 5_445 ?
S2 U 2.7179(12) 5 ?
S2 U 2.7179(12) 5_455 ?
S2 Rb 3.4250(15) 5_445 ?
S2 Rb 3.4250(15) 5_545 ?
S2 Rb 3.6265(19) 9_565 ?
