#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/20/4322004.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_4322004
loop_
_publ_author_name
'Arno Pfitzner'
'Sara Reiser'
_publ_contact_author
;
         Arno Pfitzner
       Anorganische Chemie
         Universitaet-GH Siegen 
         57068 Siegen
       Germany
;
_publ_contact_author_fax         '049 271 740-2555'
_publ_contact_author_phone       '049 271 740-2726'
_publ_section_title
;
 (CuI)₃P₄Se₄: β-P₄Se₄ Cages between Columns of Copper Iodide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2451
_journal_page_last               2454
_journal_paper_doi               10.1021/ic981042f
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'Cu3 I3 P4 Se4'
_chemical_formula_weight         1011.09
_space_group_IT_number           185
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c -2'
_symmetry_space_group_name_H-M   'P 63 c m'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   19.601(2)
_cell_length_b                   19.601(2)
_cell_length_c                   6.7196(6)
_cell_measurement_temperature    298
_cell_measurement_theta_max      56.3
_cell_measurement_theta_min      4.8
_cell_volume                     2235.8(4)
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_sigmaI/netI    0.0129
_diffrn_reflns_number            1903
_diffrn_reflns_theta_max         28.11
_diffrn_reflns_theta_min         2.40
_exptl_absorpt_coefficient_mu    20.614
_exptl_absorpt_correction_T_max  0.5827
_exptl_absorpt_correction_T_min  0.3546
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    4.504
_exptl_crystal_description       needle
_exptl_crystal_F_000             2652
_exptl_crystal_size_max          .50
_exptl_crystal_size_mid          .03
_exptl_crystal_size_min          .03
_refine_diff_density_max         3.57
_refine_diff_density_min         -3.90
_refine_ls_extinction_coef       0.293472
_refine_ls_extinction_method     'B-C type 1 Gaussian isotropic'
_refine_ls_goodness_of_fit_all   4.55
_refine_ls_goodness_of_fit_obs   4.69
_refine_ls_number_parameters     83
_refine_ls_number_reflns         1903
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_obs          0.0589
_refine_ls_shift/esd_max         0.0005
_refine_ls_shift/esd_mean        0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/(σ²(I)+0.0001I²)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.1450
_refine_ls_wR_factor_obs         0.1449
_reflns_limit_h_max              25
_reflns_limit_h_min              -25
_reflns_limit_k_max              25
_reflns_limit_k_min              -25
_reflns_limit_l_max              8
_reflns_limit_l_min              -8
_reflns_number_observed          1788
_reflns_number_total             37790
_reflns_observed_criterion       I>3\s(I)
_cod_data_source_file            ic981042f.cif
_cod_data_source_block           (CuI)3P4Se4
_cod_original_cell_volume        2235.7(3)
_cod_original_formula_sum        'P4 Cu3 Se4 I3'
_cod_database_code               4322004
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 x-y,x,1/2+z
3 y,x,z
4 -y,x-y,z
5 -x+y,y,1/2+z
6 -x,-y,1/2+z
7 -x,-x+y,z
8 -x+y,-x,z
9 -y,-x,1/2+z
10 y,-x+y,1/2+z
11 x-y,-y,z
12 x,x-y,1/2+z
loop_
_atom_site_label
_atom_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
I1 2 1 0.12944(4) 0.12944(4) 0.70107 0.0158(2)
I2 1 1 0.20185(3) 0.53358(3) 0.0875(1) 0.0240(2)
Cu1 2 1 0.12355(8) 0.12355(8) 0.3135(3) 0.0222(5)
Cu2 1 0.555(6) 0.3360(1) 0.5417(1) 0.1826(4) 0.032(1)
Cu2' 1 0.445(6) 0.3350(1) 0.5413(1) -0.0052(5) 0.024(1)
Se1 2 1 0.29987(6) 0.29987(6) 0.4847(2) 0.0258(4)
Se2 1 1 0.21648(5) 0.32459(5) 0.0507(2) 0.0290(3)
Se3 2 1 0.42058(7) 0.42058(7) -0.1331(2) 0.0265(4)
P1 2 1 0.2327(1) 0.2327(1) 0.2153(6) 0.0189(9)
P2 1 1 0.3382(1) 0.4311(1) 0.0879(5) 0.0261(8)
P3 2 1 0.3978(1) 0.3978(1) 0.3218(5) 0.0196(9)
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
P 0 24 0.102 0.094 International_Tables_Vol_C
Cu 0 18 0.320 1.265 International_Tables_Vol_C
Se 0 24 -0.093 2.226 International_Tables_Vol_C
I 0 18 -0.474 1.812 International_Tables_Vol_C
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_2
_geom_angle_site_symmetry_3
Cu1 I1 Cu1 105.57(7) . . 2_554
Cu1 I1 Cu1 107.91(6) . . 4_555
Cu1 I1 Cu1 105.57(7) 2_554 . .
Cu1 I1 Cu1 105.57(5) 2_554 . 4_555
Cu1 I1 Cu1 107.91(6) 4_555 . .
Cu1 I1 Cu1 105.57(5) 4_555 . 2_554
Cu2 I2 Cu2 104.0(1) . . 5_554
Cu2 I2 Cu2 110.13(9) . . 8_565
Cu2 I2 Cu2' 27.8(1) . . .
Cu2 I2 Cu2' 75.6(1) . . 5_555
Cu2 I2 Cu2' 117.31(9) . . 8_565
Cu2 I2 Cu2 104.0(1) 5_554 . .
Cu2 I2 Cu2 101.64(9) 5_554 . 8_565
Cu2 I2 Cu2' 76.2(1) 5_554 . .
Cu2 I2 Cu2' 174.36(7) 5_554 . 5_555
Cu2 I2 Cu2' 73.6(1) 5_554 . 8_565
Cu2 I2 Cu2 110.13(9) 8_565 . .
Cu2 I2 Cu2 101.64(9) 8_565 . 5_554
Cu2 I2 Cu2' 117.71(9) 8_565 . .
Cu2 I2 Cu2' 73.5(1) 8_565 . 5_555
Cu2 I2 Cu2' 28.1(1) 8_565 . 8_565
Cu2' I2 Cu2' 103.4(1) . . 5_555
Cu2' I2 Cu2' 110.3(1) . . 8_565
Cu2' I2 Cu2' 103.4(1) 5_555 . .
Cu2' I2 Cu2' 101.5(1) 5_555 . 8_565
Cu2' I2 Cu2' 110.3(1) 8_565 . .
Cu2' I2 Cu2' 101.5(1) 8_565 . 5_555
I1 Cu1 I1 115.78(6) . . 3_555
I1 Cu1 I1 108.10(7) . . 5_555
I1 Cu1 P1 109.8(1) . . .
I1 Cu1 I1 115.78(6) 3_555 . .
I1 Cu1 I1 108.10(7) 3_555 . 5_555
I1 Cu1 P1 109.8(1) 3_555 . .
I1 Cu1 I1 108.10(7) 5_555 . .
I1 Cu1 I1 108.10(7) 5_555 . 3_555
I1 Cu1 P1 104.6(1) 5_555 . .
I2 Cu2 I2 118.3(1) . . 4_665
I2 Cu2 I2 103.8(1) . . 5_555
I2 Cu2 Cu2' 75.1(2) . . .
I2 Cu2 P2 111.5(1) . . .
I2 Cu2 I2 118.3(1) 4_665 . .
I2 Cu2 I2 106.77(9) 4_665 . 5_555
I2 Cu2 Cu2' 76.4(1) 4_665 . .
I2 Cu2 P2 111.3(1) 4_665 . .
I2 Cu2 I2 103.8(1) 5_555 . .
I2 Cu2 I2 106.77(9) 5_555 . 4_665
I2 Cu2 Cu2' 176.7(2) 5_555 . .
I2 Cu2 P2 103.8(1) 5_555 . .
Cu2' Cu2 P2 73.9(2) . . .
I2 Cu2' I2 118.7(1) . . 4_665
I2 Cu2' I2 103.9(1) . . 5_554
I2 Cu2' Cu2 77.0(2) . . .
I2 Cu2' P2 112.3(1) . . .
I2 Cu2' I2 118.7(1) 4_665 . .
I2 Cu2' I2 106.0(1) 4_665 . 5_554
I2 Cu2' Cu2 75.5(1) 4_665 . .
I2 Cu2' P2 110.9(1) 4_665 . .
I2 Cu2' I2 103.9(1) 5_554 . .
I2 Cu2' I2 106.0(1) 5_554 . 4_665
I2 Cu2' Cu2 177.3(2) 5_554 . .
I2 Cu2' P2 103.4(1) 5_554 . .
Cu2 Cu2' P2 73.9(2) . . .
P1 Se1 P3 96.3(1) . . .
P1 Se2 P2 100.2(1) . . .
P2 Se3 P2 87.6(1) . . 3_555
P2 Se3 P2 87.6(1) 3_555 . .
Cu1 P1 Se1 108.9(2) . . .
Cu1 P1 Se2 117.1(1) . . .
Cu1 P1 Se2 117.1(1) . . 3_555
Se1 P1 Se2 101.7(1) . . .
Se1 P1 Se2 101.7(1) . . 3_555
Se2 P1 Se2 108.1(2) . . 3_555
Se2 P1 Se2 108.1(2) 3_555 . .
Cu2 P2 Cu2' 32.1(1) . . .
Cu2 P2 Se2 113.3(1) . . .
Cu2 P2 Se3 128.2(1) . . .
Cu2 P2 P3 109.9(2) . . .
Cu2' P2 Se2 109.1(1) . . .
Cu2' P2 Se3 105.3(1) . . .
Cu2' P2 P3 137.2(2) . . .
Se2 P2 Se3 108.2(1) . . .
Se2 P2 P3 105.8(1) . . .
Se3 P2 P3 86.2(1) . . .
Se1 P3 P2 104.3(1) . . .
Se1 P3 P2 104.3(1) . . 3_555
P2 P3 P2 89.4(2) . . 3_555
P2 P3 P2 89.4(2) 3_555 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
I1 Cu1 2.594(2) . .
I1 Cu1 2.607(2) . 2_554
I1 Cu1 2.594(1) . 4_555
I2 Cu2 2.633(3) . .
I2 Cu2 2.724(3) . 5_554
I2 Cu2 2.599(3) . 8_565
I2 Cu2' 2.612(3) . .
I2 Cu2' 2.740(4) . 5_555
I2 Cu2' 2.609(4) . 8_565
Cu1 I1 2.594(2) . .
Cu1 I1 2.594(2) . 3_555
Cu1 I1 2.607(2) . 5_555
Cu1 P1 2.239(2) . .
Cu2 I2 2.633(3) . .
Cu2 I2 2.599(2) . 4_665
Cu2 I2 2.724(3) . 5_555
Cu2 Cu2' 1.262(5) . .
Cu2 P2 2.280(4) . .
Cu2' I2 2.612(3) . .
Cu2' I2 2.609(2) . 4_665
Cu2' I2 2.740(4) . 5_554
Cu2' Cu2 1.262(5) . .
Cu2' P2 2.280(4) . .
Se1 P1 2.238(4) . .
Se1 P3 2.210(3) . .
Se2 P1 2.267(4) . .
Se2 P2 2.264(2) . .
Se3 P2 2.278(3) . .
Se3 P2 2.278(3) . 3_555
P1 Cu1 2.239(2) . .
P1 Se1 2.238(4) . .
P1 Se2 2.267(4) . .
P1 Se2 2.267(4) . 3_555
P2 Cu2 2.280(4) . .
P2 Cu2' 2.280(4) . .
P2 Se2 2.264(2) . .
P2 Se3 2.278(3) . .
P2 P3 2.241(5) . .
P3 Se1 2.210(3) . .
P3 P2 2.241(5) . .
P3 P2 2.241(5) . 3_555
