#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:55:39 +0100 (vie 25 de mar de 2016) $
#$Revision: 179906 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/02/7020234.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_7020234
loop_
_publ_author_name
'Alhanash, Fatma B.'
'Barnes, Nicholas A.'
'Brisdon, Alan K.'
'Godfrey, Stephen M.'
'Pritchard, Robin G.'
_publ_section_title
;
 Formation of M4Se4 cuboids (M = As, Sb, Bi) via secondary
 pnictogen-chalcogen interactions in the co-crystals
 MX3·Se=P(p-FC6)H4)3 (M = As, X = Br; M = Sb, X = Cl; M = Bi, X =
 Cl, Br).
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10211
_journal_page_last               10218
_journal_paper_doi               10.1039/c2dt31010d
_journal_volume                  41
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C18 H12 Bi1 Br3 F3 P1 Se1'
_chemical_formula_sum            'C18 H12 Bi Br3 F3 P Se'
_chemical_formula_weight         843.89
_chemical_name_systematic
;
?
;
_space_group_IT_number           197
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      197
_symmetry_space_group_name_Hall  'I 2 2 3'
_symmetry_space_group_name_H-M   'I 2 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2012-04-26T08:25:03-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.3328(8)
_cell_length_b                   16.3328(8)
_cell_length_c                   16.3328(8)
_cell_measurement_reflns_used    1304
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_measurement_wavelength     0.71073
_cell_volume                     4356.9(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.21492E-2
_diffrn_orient_matrix_UB_12      -0.573283E-1
_diffrn_orient_matrix_UB_13      -0.213889E-1
_diffrn_orient_matrix_UB_21      0.218383E-1
_diffrn_orient_matrix_UB_22      0.19274E-1
_diffrn_orient_matrix_UB_23      -0.53854E-1
_diffrn_orient_matrix_UB_31      0.571594E-1
_diffrn_orient_matrix_UB_32      -0.95193E-2
_diffrn_orient_matrix_UB_33      0.197712E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.082
_diffrn_reflns_av_unetI/netI     0.0769
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2034
_diffrn_reflns_reduction_process
;
Scaled and merged with Sortav
R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.06
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    15.367
_exptl_absorpt_correction_T_max  0.3087
_exptl_absorpt_correction_T_min  0.26
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Blessing, R. H. (1995) Acta Cryst., A51, 33-38.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3072
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.697
_refine_diff_density_min         -1.158
_refine_diff_density_rms         0.198
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.057(19)
_refine_ls_extinction_coef       0.00025(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         1491
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0353P)²+52.4074P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1062
_reflns_number_gt                1302
_reflns_number_total             1491
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c2dt31010d.txt
_cod_data_source_block           rob6
_cod_database_code               7020234
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z'
'-x, y, -z'
'z, x, y'
'y, z, x'
'-z, -x, y'
'-y, z, -x'
'z, -x, -y'
'-y, -z, x'
'-z, x, -y'
'y, -z, -x'
'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+1/2'
'-x+1/2, y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-y+1/2, -z+1/2, x+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+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
C1 C 0.2726(7) 0.1395(6) 0.8459(7) 0.026(2) Uani 1 1 d .
C2 C 0.3223(8) 0.1324(8) 0.7789(8) 0.037(3) Uani 1 1 d .
H2 H 0.3001 0.139 0.7255 0.044 Uiso 1 1 calc R
C3 C 0.4047(7) 0.1158(9) 0.7886(8) 0.038(3) Uani 1 1 d .
H3 H 0.44 0.1131 0.7424 0.045 Uiso 1 1 calc R
C4 C 0.4344(7) 0.1033(8) 0.8648(8) 0.035(3) Uani 1 1 d .
C5 C 0.3860(8) 0.1098(8) 0.9336(7) 0.033(3) Uani 1 1 d .
H5 H 0.4091 0.1016 0.9863 0.04 Uiso 1 1 calc R
C6 C 0.3036(8) 0.1283(8) 0.9255(7) 0.035(3) Uani 1 1 d .
H6 H 0.2692 0.1331 0.9722 0.042 Uiso 1 1 calc R
F1 F 0.5153(4) 0.0897(5) 0.8761(5) 0.047(2) Uani 1 1 d .
P1 P 0.16510(18) 0.16510(18) 0.83490(18) 0.0255(11) Uani 1 3 d S
Se1 Se 0.08773(7) 0.08773(7) 0.91227(7) 0.0242(4) Uani 1 3 d S
Br1 Br 0.14584(8) 0.26932(8) 1.07836(8) 0.0320(3) Uani 1 1 d .
Bi1 Bi 0.11493(3) 0.11493(3) 1.11493(3) 0.0265(2) Uani 1 3 d S
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.033(6) 0.016(5) 0.029(6) 0.001(4) 0.001(5) 0.000(4)
C2 0.030(6) 0.050(8) 0.031(6) 0.011(6) 0.005(5) -0.004(6)
C3 0.029(6) 0.048(7) 0.036(7) 0.015(6) 0.006(5) -0.002(6)
C4 0.024(6) 0.034(7) 0.048(8) 0.011(6) -0.009(5) 0.006(5)
C5 0.037(6) 0.035(6) 0.028(6) -0.006(5) -0.004(5) 0.010(7)
C6 0.033(6) 0.043(8) 0.029(6) -0.014(6) -0.001(5) 0.016(6)
F1 0.013(3) 0.063(5) 0.064(5) -0.012(5) 0.000(3) 0.006(3)
P1 0.0255(11) 0.0255(11) 0.0255(11) 0.0011(12) 0.0011(12) -0.0011(12)
Se1 0.0242(4) 0.0242(4) 0.0242(4) 0.0006(4) 0.0006(4) -0.0006(4)
Br1 0.0382(7) 0.0273(6) 0.0304(6) -0.0006(5) -0.0020(5) -0.0030(5)
Bi1 0.0265(2) 0.0265(2) 0.0265(2) -0.00115(18) -0.00115(18) -0.00115(18)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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
C2 C1 C6 121.0(12) . .
C2 C1 P1 120.9(10) . .
C6 C1 P1 118.0(9) . .
C1 C2 C3 120.1(12) . .
C1 C2 H2 120 . .
C3 C2 H2 120 . .
C4 C3 C2 119.0(12) . .
C4 C3 H3 120.5 . .
C2 C3 H3 120.5 . .
C3 C4 F1 120.0(12) . .
C3 C4 C5 122.3(11) . .
F1 C4 C5 117.5(11) . .
C4 C5 C6 119.8(11) . .
C4 C5 H5 120.1 . .
C6 C5 H5 120.1 . .
C5 C6 C1 117.7(11) . .
C5 C6 H6 121.1 . .
C1 C6 H6 121.1 . .
C1 P1 C1 107.2(4) 11_656 12_566
C1 P1 C1 107.2(4) 11_656 .
C1 P1 C1 107.2(4) 12_566 .
C1 P1 Se1 111.6(4) 11_656 .
C1 P1 Se1 111.6(4) 12_566 .
C1 P1 Se1 111.6(4) . .
Br1 Bi1 Br1 94.40(4) . 6_546
Br1 Bi1 Br1 94.40(4) . 5_456
Br1 Bi1 Br1 94.40(4) 6_546 5_456
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.368(16) .
C1 C6 1.407(17) .
C1 P1 1.814(12) .
C2 C3 1.383(18) .
C2 H2 0.95 .
C3 C4 1.351(17) .
C3 H3 0.95 .
C4 F1 1.354(13) .
C4 C5 1.376(18) .
C5 C6 1.386(17) .
C5 H5 0.95 .
C6 H6 0.95 .
P1 C1 1.814(12) 11_656
P1 C1 1.814(12) 12_566
P1 Se1 2.189(5) .
Br1 Bi1 2.6400(13) .
Bi1 Br1 2.6400(13) 6_546
Bi1 Br1 2.6400(13) 5_456
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_4
C6 C1 C2 C3 -1(2) .
P1 C1 C2 C3 177.7(11) .
C1 C2 C3 C4 3(2) .
C2 C3 C4 F1 -177.8(12) .
C2 C3 C4 C5 -3(2) .
C3 C4 C5 C6 1(2) .
F1 C4 C5 C6 176.4(12) .
C4 C5 C6 C1 0(2) .
C2 C1 C6 C5 0.0(19) .
P1 C1 C6 C5 -179.2(10) .
C2 C1 P1 C1 -102.2(8) 11_656
C6 C1 P1 C1 77.0(12) 11_656
C2 C1 P1 C1 12.7(12) 12_566
C6 C1 P1 C1 -168.1(9) 12_566
C2 C1 P1 Se1 135.2(9) .
C6 C1 P1 Se1 -45.5(10) .
