#------------------------------------------------------------------------------
#$Date: 2019-11-17 10:44:13 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229408 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/55/7045525.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_7045525
loop_
_publ_author_name
'Upmann, Daniel'
'Jones, Peter G.'
_publ_section_title
;
 Bromination and iodination of diphosphane dichalcogenides.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2748
_journal_page_last               2758
_journal_paper_doi               10.1039/c7dt04531j
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C52 H48 Br24 P4 Se3'
_chemical_formula_weight         2951.50
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-07-19 deposited with the CCDC.
2018-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.356(4)
_cell_angle_beta                 101.185(4)
_cell_angle_gamma                105.297(4)
_cell_formula_units_Z            1
_cell_length_a                   8.5395(4)
_cell_length_b                   11.2623(7)
_cell_length_c                   21.3286(8)
_cell_measurement_reflns_used    11169
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.9050
_cell_measurement_theta_min      2.5120
_cell_volume                     1937.44(17)
_computing_cell_refinement
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) 
(compiled Aug 13 2014,18:06:01) 
;
_computing_data_collection
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) 
(compiled Aug 13 2014,18:06:01) 
;
_computing_data_reduction
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) 
(compiled Aug 13 2014,18:06:01) 
;
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford diffraction Xcalibur, Eos'
_diffrn_measurement_method       ω-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0969
_diffrn_reflns_av_sigmaI/netI    0.0586
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            101158
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         2.17
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    13.915
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) 
(compiled Aug 13 2014,18:06:01) 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1362
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.045
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         10436
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0207P)²+2.9343P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0698
_reflns_number_gt                7858
_reflns_number_total             10436
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt04531j2.cif
_cod_data_source_block           jim
_cod_depositor_comments
'Adding full bibliography for 7045509--7045531.cif.'
_cod_database_code               7045525
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Br1 Br 0.92363(6) 0.87831(5) 0.61926(2) 0.01919(11) Uani 1 1 d .
Br2 Br 0.39402(5) 0.38855(4) 0.63984(2) 0.01306(10) Uani 1 1 d .
Br3 Br 0.01669(6) 0.28953(4) 0.54255(2) 0.01481(10) Uani 1 1 d .
Br4 Br 0.29885(5) 0.53896(4) 0.48211(2) 0.01336(10) Uani 1 1 d .
Br5 Br 0.11275(5) 0.60350(4) 0.61374(2) 0.01265(10) Uani 1 1 d .
Br6 Br 0.64495(6) 0.89051(5) 1.02452(2) 0.01993(11) Uani 1 1 d .
Br7 Br 0.65509(6) 0.88874(5) 1.15483(2) 0.01804(11) Uani 1 1 d .
Br8 Br 0.67288(6) 0.89627(5) 1.26849(2) 0.02391(12) Uani 1 1 d .
Br9 Br 0.27049(7) 0.63421(5) 1.04291(2) 0.02357(12) Uani 1 1 d .
Br10 Br 0.00014(6) 0.82628(5) 1.01278(2) 0.01720(11) Uani 1 1 d .
Br11 Br 0.21255(6) 0.76324(5) 0.88383(2) 0.01657(10) Uani 1 1 d .
Br12 Br 0.15057(6) 0.69650(5) 0.76989(2) 0.02221(12) Uani 1 1 d .
Se1 Se 0.0000 0.5000 0.5000 0.00945(13) Uani 1 2 d S
Se2 Se 0.27757(6) 0.83337(5) 1.01020(2) 0.01440(10) Uani 1 1 d .
P1 P 0.69536(15) 0.84817(11) 0.65264(5) 0.0122(2) Uani 1 1 d .
P2 P 0.61225(14) 0.47583(11) 0.71052(5) 0.0111(2) Uani 1 1 d .
C01 C 0.5954(5) 0.6846(4) 0.6423(2) 0.0132(9) Uani 1 1 d .
H01A H 0.4947 0.6659 0.6609 0.016 Uiso 1 1 calc R
H01B H 0.5612 0.6592 0.5960 0.016 Uiso 1 1 calc R
C02 C 0.7150(5) 0.6120(4) 0.6753(2) 0.0135(9) Uani 1 1 d .
H02A H 0.7999 0.6666 0.7091 0.016 Uiso 1 1 calc R
H02B H 0.7728 0.5876 0.6434 0.016 Uiso 1 1 calc R
C11 C 0.5722(6) 0.9367(4) 0.6102(2) 0.0130(9) Uani 1 1 d .
C12 C 0.6412(6) 1.0647(5) 0.6136(2) 0.0199(11) Uani 1 1 d .
H12 H 0.7523 1.0995 0.6357 0.024 Uiso 1 1 calc R
C13 C 0.5485(6) 1.1398(4) 0.5852(2) 0.0200(11) Uani 1 1 d .
H13 H 0.5958 1.2265 0.5870 0.024 Uiso 1 1 calc R
C14 C 0.3865(6) 1.0893(5) 0.5541(2) 0.0192(11) Uani 1 1 d .
H14 H 0.3223 1.1418 0.5350 0.023 Uiso 1 1 calc R
C15 C 0.3168(6) 0.9637(4) 0.5502(2) 0.0183(10) Uani 1 1 d .
H15 H 0.2051 0.9302 0.5287 0.022 Uiso 1 1 calc R
C16 C 0.4091(6) 0.8863(4) 0.5776(2) 0.0176(10) Uani 1 1 d .
H16 H 0.3618 0.7996 0.5743 0.021 Uiso 1 1 calc R
C21 C 0.7385(5) 0.8904(4) 0.7360(2) 0.0108(9) Uani 1 1 d .
C22 C 0.8936(5) 0.9157(4) 0.7754(2) 0.0128(9) Uani 1 1 d .
H22 H 0.9889 0.9181 0.7582 0.015 Uiso 1 1 calc R
C23 C 0.9075(6) 0.9375(4) 0.8405(2) 0.0142(10) Uani 1 1 d .
H23 H 1.0137 0.9563 0.8680 0.017 Uiso 1 1 calc R
C24 C 0.7695(6) 0.9323(4) 0.8657(2) 0.0164(10) Uani 1 1 d .
H24 H 0.7809 0.9461 0.9105 0.020 Uiso 1 1 calc R
C25 C 0.6131(6) 0.9068(4) 0.8259(2) 0.0165(10) Uani 1 1 d .
H25 H 0.5184 0.9035 0.8437 0.020 Uiso 1 1 calc R
C26 C 0.5958(6) 0.8863(5) 0.7608(2) 0.0164(10) Uani 1 1 d .
H26 H 0.4899 0.8698 0.7332 0.020 Uiso 1 1 calc R
C31 C 0.7478(5) 0.3796(4) 0.7306(2) 0.0120(9) Uani 1 1 d .
C32 C 0.7431(6) 0.3177(5) 0.7869(2) 0.0176(10) Uani 1 1 d .
H32 H 0.6662 0.3248 0.8126 0.021 Uiso 1 1 calc R
C33 C 0.8514(6) 0.2458(5) 0.8053(2) 0.0190(11) Uani 1 1 d .
H33 H 0.8480 0.2022 0.8432 0.023 Uiso 1 1 calc R
C34 C 0.9643(6) 0.2382(4) 0.7680(2) 0.0169(10) Uani 1 1 d .
H34 H 1.0411 0.1912 0.7812 0.020 Uiso 1 1 calc R
C35 C 0.9668(6) 0.2981(4) 0.7117(2) 0.0162(10) Uani 1 1 d .
H35 H 1.0439 0.2907 0.6862 0.019 Uiso 1 1 calc R
C36 C 0.8589(5) 0.3682(4) 0.6924(2) 0.0116(9) Uani 1 1 d .
H36 H 0.8599 0.4085 0.6534 0.014 Uiso 1 1 calc R
C41 C 0.5523(6) 0.5161(4) 0.7817(2) 0.0137(10) Uani 1 1 d .
C42 C 0.6744(6) 0.5940(5) 0.8280(2) 0.0215(11) Uani 1 1 d .
H42 H 0.7816 0.6300 0.8196 0.026 Uiso 1 1 calc R
C43 C 0.6374(7) 0.6187(5) 0.8869(2) 0.0287(13) Uani 1 1 d .
H43 H 0.7184 0.6734 0.9185 0.034 Uiso 1 1 calc R
C44 C 0.4827(7) 0.5631(5) 0.8989(2) 0.0277(13) Uani 1 1 d .
H44 H 0.4585 0.5782 0.9394 0.033 Uiso 1 1 calc R
C45 C 0.3627(7) 0.4860(6) 0.8528(3) 0.0301(13) Uani 1 1 d .
H45 H 0.2561 0.4493 0.8615 0.036 Uiso 1 1 calc R
C46 C 0.3963(6) 0.4619(5) 0.7947(2) 0.0233(12) Uani 1 1 d .
H46 H 0.3134 0.4083 0.7632 0.028 Uiso 1 1 calc R
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 0.0000 0.0000 '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'
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'
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
Br8 Br7 Br6 177.39(3) . .
Br12 Br11 Se2 179.03(3) . .
Br3 Se1 Br3 180.000(19) . 2_566
Br3 Se1 Br5 90.632(15) . .
Br3 Se1 Br5 89.368(15) 2_566 .
Br3 Se1 Br5 89.368(15) . 2_566
Br3 Se1 Br5 90.632(15) 2_566 2_566
Br5 Se1 Br5 180.0 . 2_566
Br3 Se1 Br4 89.049(15) . .
Br3 Se1 Br4 90.951(15) 2_566 .
Br5 Se1 Br4 89.886(14) . .
Br5 Se1 Br4 90.114(14) 2_566 .
Br3 Se1 Br4 90.951(15) . 2_566
Br3 Se1 Br4 89.049(15) 2_566 2_566
Br5 Se1 Br4 90.114(14) . 2_566
Br5 Se1 Br4 89.886(14) 2_566 2_566
Br4 Se1 Br4 180.0 . 2_566
Br9 Se2 Br10 97.48(3) . .
Br9 Se2 Br11 93.67(2) . .
Br10 Se2 Br11 94.56(2) . .
C11 P1 C21 109.9(2) . .
C11 P1 C01 112.7(2) . .
C21 P1 C01 107.5(2) . .
C11 P1 Br1 109.77(16) . .
C21 P1 Br1 109.67(15) . .
C01 P1 Br1 107.24(16) . .
C31 P2 C41 108.5(2) . .
C31 P2 C02 110.0(2) . .
C41 P2 C02 110.7(2) . .
C31 P2 Br2 112.75(15) . .
C41 P2 Br2 109.39(16) . .
C02 P2 Br2 105.44(15) . .
C02 C01 P1 110.1(3) . .
C01 C02 P2 113.1(3) . .
C16 C11 C12 119.6(4) . .
C16 C11 P1 123.3(4) . .
C12 C11 P1 117.0(4) . .
C13 C12 C11 120.1(5) . .
C12 C13 C14 119.9(5) . .
C15 C14 C13 120.8(4) . .
C14 C15 C16 120.2(4) . .
C15 C16 C11 119.4(4) . .
C22 C21 C26 121.3(4) . .
C22 C21 P1 124.8(3) . .
C26 C21 P1 113.7(3) . .
C21 C22 C23 118.8(4) . .
C24 C23 C22 120.8(4) . .
C23 C24 C25 120.4(4) . .
C26 C25 C24 120.0(4) . .
C25 C26 C21 118.7(4) . .
C36 C31 C32 120.5(4) . .
C36 C31 P2 121.5(3) . .
C32 C31 P2 118.0(3) . .
C33 C32 C31 119.6(4) . .
C34 C33 C32 119.4(4) . .
C35 C34 C33 120.8(4) . .
C36 C35 C34 120.6(4) . .
C35 C36 C31 119.2(4) . .
C46 C41 C42 120.1(4) . .
C46 C41 P2 122.3(4) . .
C42 C41 P2 117.2(4) . .
C41 C42 C43 119.2(5) . .
C44 C43 C42 119.6(5) . .
C45 C44 C43 120.8(5) . .
C46 C45 C44 120.3(5) . .
C45 C46 C41 119.9(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 P1 2.1481(13) .
Br2 P2 2.1534(12) .
Br3 Se1 2.5724(5) .
Br4 Se1 2.5768(4) .
Br5 Se1 2.5764(4) .
Br6 Br7 2.7641(7) .
Br7 Br8 2.3990(7) .
Br9 Se2 2.3421(7) .
Br10 Se2 2.3607(6) .
Br11 Br12 2.4535(7) .
Br11 Se2 2.7126(6) .
Se1 Br3 2.5724(5) 2_566
Se1 Br5 2.5764(4) 2_566
Se1 Br4 2.5768(4) 2_566
P1 C11 1.765(5) .
P1 C21 1.779(4) .
P1 C01 1.807(5) .
P2 C31 1.782(5) .
P2 C41 1.785(4) .
P2 C02 1.802(5) .
C01 C02 1.542(6) .
C11 C16 1.396(6) .
C11 C12 1.401(6) .
C12 C13 1.373(6) .
C13 C14 1.379(7) .
C14 C15 1.377(7) .
C15 C16 1.383(6) .
C21 C22 1.381(6) .
C21 C26 1.410(6) .
C22 C23 1.385(6) .
C23 C24 1.375(6) .
C24 C25 1.393(6) .
C25 C26 1.379(6) .
C31 C36 1.394(6) .
C31 C32 1.395(6) .
C32 C33 1.387(6) .
C33 C34 1.383(6) .
C34 C35 1.381(6) .
C35 C36 1.372(6) .
C41 C46 1.393(7) .
C41 C42 1.393(6) .
C42 C43 1.397(7) .
C43 C44 1.378(8) .
C44 C45 1.378(8) .
C45 C46 1.367(7) .
