#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/74/4317422.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_4317422
loop_
_publ_author_name
'Jennifer A. Aitken'
'Michel Evain'
'Lykourgos Iordanidis'
'Mercouri G. Kanatzidis'
_publ_section_title
;
 NaCeP2Se6, Cu0.4Ce1.2P2Se6, Ce4(P2Se6)3, and the Incommensurately
 Modulated AgCeP2Se6: New Selenophosphates Featuring the Ethane-Like
 [P2Se6]4- Anion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              180
_journal_page_last               191
_journal_paper_doi               10.1021/ic010618p
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'Ce1.2 Cu0.4 P2 Se6'
_chemical_formula_weight         729.26
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 111.269(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0409(14)
_cell_length_b                   7.6418(8)
_cell_length_c                   11.6999(13)
_cell_measurement_reflns_used    1566
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.12
_cell_measurement_theta_min      3.23
_cell_volume                     1003.23(19)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_publication_material  'ORTEP and Crystal-maker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'omega scan'
_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  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5033
_diffrn_reflns_theta_full        27.12
_diffrn_reflns_theta_max         27.12
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    28.258
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.694397
_exptl_absorpt_correction_type   'empirical SADABS'
_exptl_crystal_colour            plate
_exptl_crystal_density_diffrn    4.828
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       yellow
_exptl_crystal_F_000             1261
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.160
_refine_diff_density_min         -1.675
_refine_diff_density_rms         0.399
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         2150
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0430
_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)+(0.0530P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1022
_reflns_number_gt                1586
_reflns_number_total             2150
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010618p_2.cif
_cod_data_source_block           Cu0.4Ce1.2P2Se6
_cod_original_formula_sum        'Ce1.20 Cu0.40 P2 Se6'
_cod_database_code               4317422
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Ce1 Ce 0.34521(6) 0.10723(8) 0.59066(5) 0.01718(18) Uani 1 1 d . . .
Se1 Se 0.07631(11) -0.00855(14) 0.33234(10) 0.0211(3) Uani 1 1 d . . .
Se2 Se 0.11195(11) 0.20214(15) 0.05700(9) 0.0198(3) Uani 1 1 d . . .
Se3 Se 0.79822(11) 0.20691(15) 0.37616(10) 0.0244(3) Uani 1 1 d . . .
Se4 Se 0.30382(11) 0.17902(14) 0.85441(9) 0.0181(3) Uani 1 1 d . . .
Se5 Se 0.44748(10) 0.02295(14) 0.18031(9) 0.0162(3) Uani 1 1 d . . .
Se6 Se 0.59711(10) 0.19570(13) 0.56492(9) 0.0158(3) Uani 1 1 d . . .
P1 P 0.1898(2) 0.1141(3) 0.2457(2) 0.0125(6) Uani 1 1 d . . .
P2 P 0.6834(3) 0.0995(3) 0.7531(2) 0.0118(5) Uani 1 1 d . . .
Ce2 Ce 0.8563(3) 0.1145(5) 0.1148(3) 0.0285(10) Uani 0.1984(17) 1 d P . .
Cu1 Cu 0.9350(4) 0.2224(5) 0.2860(4) 0.0382(15) Uani 0.405(5) 1 d P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
P P 0.1023 0.0942 '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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 '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
Se2 Ce1 Se3 81.72(4) 4_566 3_656 ?
Se2 Ce1 Se5 132.84(3) 4_566 3_656 ?
Se3 Ce1 Se5 87.31(3) 3_656 3_656 ?
Se2 Ce1 Se4 77.91(3) 4_566 4_565 ?
Se3 Ce1 Se4 127.73(4) 3_656 4_565 ?
Se5 Ce1 Se4 139.72(4) 3_656 4_565 ?
Se2 Ce1 Se5 80.99(3) 4_566 4_566 ?
Se3 Ce1 Se5 147.37(4) 3_656 4_566 ?
Se5 Ce1 Se5 84.47(2) 3_656 4_566 ?
Se4 Ce1 Se5 74.75(3) 4_565 4_566 ?
Se2 Ce1 Se6 130.92(3) 4_566 3_656 ?
Se3 Ce1 Se6 75.63(3) 3_656 3_656 ?
Se5 Ce1 Se6 89.23(3) 3_656 3_656 ?
Se4 Ce1 Se6 82.55(3) 4_565 3_656 ?
Se5 Ce1 Se6 135.58(4) 4_566 3_656 ?
Se2 Ce1 Se6 137.58(3) 4_566 . ?
Se3 Ce1 Se6 140.21(4) 3_656 . ?
Se5 Ce1 Se6 69.96(3) 3_656 . ?
Se4 Ce1 Se6 70.00(3) 4_565 . ?
Se5 Ce1 Se6 64.55(3) 4_566 . ?
Se6 Ce1 Se6 71.98(3) 3_656 . ?
Se2 Ce1 Se4 66.65(3) 4_566 . ?
Se3 Ce1 Se4 74.46(3) 3_656 . ?
Se5 Ce1 Se4 66.21(3) 3_656 . ?
Se4 Ce1 Se4 135.12(3) 4_565 . ?
Se5 Ce1 Se4 73.32(3) 4_566 . ?
Se6 Ce1 Se4 141.78(3) 3_656 . ?
Se6 Ce1 Se4 120.76(3) . . ?
Se2 Ce1 Se1 60.75(3) 4_566 . ?
Se3 Ce1 Se1 62.81(3) 3_656 . ?
Se5 Ce1 Se1 146.68(3) 3_656 . ?
Se4 Ce1 Se1 65.20(3) 4_565 . ?
Se5 Ce1 Se1 128.61(3) 4_566 . ?
Se6 Ce1 Se1 70.18(3) 3_656 . ?
Se6 Ce1 Se1 123.75(3) . . ?
Se4 Ce1 Se1 114.82(3) . . ?
P1 Se1 Cu1 95.30(12) . 1_455 ?
P1 Se1 Cu1 90.78(12) . 2_645 ?
Cu1 Se1 Cu1 127.26(7) 1_455 2_645 ?
P1 Se1 Ce2 109.87(11) . 2_645 ?
Cu1 Se1 Ce2 151.65(14) 1_455 2_645 ?
Cu1 Se1 Ce2 42.82(12) 2_645 2_645 ?
P1 Se1 Ce2 88.91(10) . 1_455 ?
Cu1 Se1 Ce2 41.75(13) 1_455 1_455 ?
Cu1 Se1 Ce2 86.25(13) 2_645 1_455 ?
Ce2 Se1 Ce2 123.46(10) 2_645 1_455 ?
P1 Se1 Ce1 76.34(8) . . ?
Cu1 Se1 Ce1 110.88(12) 1_455 . ?
Cu1 Se1 Ce1 121.43(12) 2_645 . ?
Ce2 Se1 Ce1 88.26(8) 2_645 . ?
Ce2 Se1 Ce1 148.17(8) 1_455 . ?
P1 Se2 Ce1 88.79(8) . 4_565 ?
P1 Se2 Ce2 107.07(10) . 3_655 ?
Ce1 Se2 Ce2 97.21(8) 4_565 3_655 ?
P1 Se2 Ce2 80.05(10) . 1_455 ?
Ce1 Se2 Ce2 155.53(7) 4_565 1_455 ?
Ce2 Se2 Ce2 106.84(8) 3_655 1_455 ?
P2 Se3 Cu1 92.95(13) 4_565 . ?
P2 Se3 Ce2 100.79(10) 4_565 4_566 ?
Cu1 Se3 Ce2 117.03(15) . 4_566 ?
P2 Se3 Ce1 111.39(9) 4_565 3_656 ?
Cu1 Se3 Ce1 129.83(11) . 3_656 ?
Ce2 Se3 Ce1 101.15(8) 4_566 3_656 ?
P2 Se3 Ce2 80.62(9) 4_565 . ?
Cu1 Se3 Ce2 34.86(13) . . ?
Ce2 Se3 Ce2 151.39(12) 4_566 . ?
Ce1 Se3 Ce2 104.89(7) 3_656 . ?
P1 Se4 Ce2 108.08(11) 4_566 3_656 ?
P1 Se4 Ce1 90.09(7) 4_566 4_566 ?
Ce2 Se4 Ce1 100.71(7) 3_656 4_566 ?
P1 Se4 Ce1 81.57(7) 4_566 . ?
Ce2 Se4 Ce1 107.41(7) 3_656 . ?
Ce1 Se4 Ce1 151.87(4) 4_566 . ?
P2 Se5 Ce1 90.74(8) 3_656 3_656 ?
P2 Se5 Ce1 105.00(8) 3_656 4_565 ?
Ce1 Se5 Ce1 132.98(4) 3_656 4_565 ?
P2 Se6 Ce1 102.06(8) . 3_656 ?
P2 Se6 Ce1 87.42(8) . . ?
Ce1 Se6 Ce1 108.02(3) 3_656 . ?
P2 Se6 Ce2 84.06(10) . 4_566 ?
Ce1 Se6 Ce2 91.85(7) 3_656 4_566 ?
Ce1 Se6 Ce2 159.64(7) . 4_566 ?
Se2 P1 Se4 108.52(12) . 4_565 ?
Se2 P1 Se1 119.52(13) . . ?
Se4 P1 Se1 114.10(11) 4_565 . ?
Se2 P1 P2 106.00(12) . 3_656 ?
Se4 P1 P2 104.05(14) 4_565 3_656 ?
Se1 P1 P2 103.01(13) . 3_656 ?
Se3 P2 Se6 113.12(12) 4_566 . ?
Se3 P2 Se5 114.79(11) 4_566 3_656 ?
Se6 P2 Se5 111.00(13) . 3_656 ?
Se3 P2 P1 102.95(14) 4_566 3_656 ?
Se6 P2 P1 108.98(13) . 3_656 ?
Se5 P2 P1 105.21(13) 3_656 3_656 ?
Cu1 Ce2 Se3 127.14(19) . 4_565 ?
Cu1 Ce2 Se1 54.38(14) . 2_655 ?
Se3 Ce2 Se1 72.81(9) 4_565 2_655 ?
Cu1 Ce2 Se4 105.47(17) . 3_656 ?
Se3 Ce2 Se4 120.40(13) 4_565 3_656 ?
Se1 Ce2 Se4 144.55(13) 2_655 3_656 ?
Cu1 Ce2 Se1 50.37(14) . 1_655 ?
Se3 Ce2 Se1 139.44(14) 4_565 1_655 ?
Se1 Ce2 Se1 92.04(10) 2_655 1_655 ?
Se4 Ce2 Se1 93.94(10) 3_656 1_655 ?
Cu1 Ce2 Se2 141.7(2) . 3_655 ?
Se3 Ce2 Se2 78.49(8) 4_565 3_655 ?
Se1 Ce2 Se2 139.34(13) 2_655 3_655 ?
Se4 Ce2 Se2 75.42(8) 3_656 3_655 ?
Se1 Ce2 Se2 91.43(10) 1_655 3_655 ?
Cu1 Ce2 Se6 93.90(17) . 4_565 ?
Se3 Ce2 Se6 75.23(9) 4_565 4_565 ?
Se1 Ce2 Se6 77.38(9) 2_655 4_565 ?
Se4 Ce2 Se6 75.34(9) 3_656 4_565 ?
Se1 Ce2 Se6 139.10(12) 1_655 4_565 ?
Se2 Ce2 Se6 122.24(12) 3_655 4_565 ?
Cu1 Ce2 Se2 89.11(17) . 1_655 ?
Se3 Ce2 Se2 69.34(8) 4_565 1_655 ?
Se1 Ce2 Se2 70.10(8) 2_655 1_655 ?
Se4 Ce2 Se2 144.11(12) 3_656 1_655 ?
Se1 Ce2 Se2 70.13(8) 1_655 1_655 ?
Se2 Ce2 Se2 73.16(8) 3_655 1_655 ?
Se6 Ce2 Se2 137.31(11) 4_565 1_655 ?
Cu1 Ce2 Se3 38.97(14) . . ?
Se3 Ce2 Se3 133.52(12) 4_565 . ?
Se1 Ce2 Se3 75.33(8) 2_655 . ?
Se4 Ce2 Se3 72.95(8) 3_656 . ?
Se1 Ce2 Se3 73.74(8) 1_655 . ?
Se2 Ce2 Se3 143.78(12) 3_655 . ?
Se6 Ce2 Se3 65.37(7) 4_565 . ?
Se2 Ce2 Se3 128.08(11) 1_655 . ?
Ce2 Cu1 Se3 106.2(2) . . ?
Ce2 Cu1 Se1 87.89(18) . 1_655 ?
Se3 Cu1 Se1 115.99(16) . 1_655 ?
Ce2 Cu1 Se1 82.80(17) . 2_655 ?
Se3 Cu1 Se1 114.00(16) . 2_655 ?
Se1 Cu1 Se1 129.80(18) 1_655 2_655 ?
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
Ce1 Se2 3.0599(14) 4_566 ?
Ce1 Se3 3.0631(13) 3_656 ?
Ce1 Se5 3.0900(13) 3_656 ?
Ce1 Se4 3.0916(12) 4_565 ?
Ce1 Se5 3.1091(12) 4_566 ?
Ce1 Se6 3.1736(12) 3_656 ?
Ce1 Se6 3.2265(14) . ?
Ce1 Se4 3.3448(12) . ?
Ce1 Se1 3.6471(14) . ?
Se1 P1 2.186(3) . ?
Se1 Cu1 2.374(4) 1_455 ?
Se1 Cu1 2.455(4) 2_645 ?
Se1 Ce2 2.996(4) 2_645 ?
Se1 Ce2 3.080(4) 1_455 ?
Se2 P1 2.169(3) . ?
Se2 Ce1 3.0600(14) 4_565 ?
Se2 Ce2 3.255(4) 3_655 ?
Se2 Ce2 3.448(4) 1_455 ?
Se3 P2 2.175(3) 4_565 ?
Se3 Cu1 2.258(4) . ?
Se3 Ce2 2.955(4) 4_566 ?
Se3 Ce1 3.0631(13) 3_656 ?
Se3 Ce2 3.448(4) . ?
Se4 P1 2.176(3) 4_566 ?
Se4 Ce2 3.063(4) 3_656 ?
Se4 Ce1 3.0915(12) 4_566 ?
Se5 P2 2.204(3) 3_656 ?
Se5 Ce1 3.0900(13) 3_656 ?
Se5 Ce1 3.1091(12) 4_565 ?
Se6 P2 2.193(3) . ?
Se6 Ce1 3.1736(12) 3_656 ?
Se6 Ce2 3.296(4) 4_566 ?
P1 Se4 2.176(3) 4_565 ?
P1 P2 2.231(4) 3_656 ?
P2 Se3 2.175(3) 4_566 ?
P2 Se5 2.204(3) 3_656 ?
P2 P1 2.231(4) 3_656 ?
Ce2 Cu1 2.052(6) . ?
Ce2 Se3 2.955(4) 4_565 ?
Ce2 Se1 2.996(4) 2_655 ?
Ce2 Se4 3.063(4) 3_656 ?
Ce2 Se1 3.080(4) 1_655 ?
Ce2 Se2 3.255(4) 3_655 ?
Ce2 Se6 3.296(4) 4_565 ?
Ce2 Se2 3.448(4) 1_655 ?
Cu1 Se1 2.374(4) 1_655 ?
Cu1 Se1 2.455(4) 2_655 ?
