#------------------------------------------------------------------------------
#$Date: 2019-11-17 10:44:13 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229408 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/55/7045511.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_7045511
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            'C50 H46 Br6 O4 P4 Se2'
_chemical_formula_weight         1472.13
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-07-27 deposited with the CCDC.
2018-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.676(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.0635(3)
_cell_length_b                   9.5315(2)
_cell_length_c                   20.8476(5)
_cell_measurement_reflns_used    19818
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.2620
_cell_measurement_theta_min      3.9410
_cell_volume                     2595.65(10)
_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 10.3543
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Atlas, Nova'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0682
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            51628
_diffrn_reflns_theta_full        75.00
_diffrn_reflns_theta_max         76.46
_diffrn_reflns_theta_min         3.97
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    8.712
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59630
_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            'pale yellow'
_exptl_crystal_density_diffrn    1.884
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.949
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         5421
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0263
_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)+(0.0255P)²+2.4300P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0617
_reflns_number_gt                4616
_reflns_number_total             5421
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt04531j2.cif
_cod_data_source_block           roy
_cod_depositor_comments
'Adding full bibliography for 7045509--7045531.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7045511
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
Se1 Se 0.59667(2) 0.07875(3) 0.431137(14) 0.01651(7) Uani 1 1 d .
Br1 Br 0.62136(2) -0.02239(3) 0.554405(14) 0.01951(7) Uani 1 1 d .
Br2 Br 0.77894(2) 0.11486(3) 0.425512(15) 0.02179(8) Uani 1 1 d .
Br3 Br 0.57078(2) 0.15715(3) 0.319637(14) 0.02165(7) Uani 1 1 d .
P1 P 0.07889(5) 0.27750(7) 0.40215(3) 0.01488(14) Uani 1 1 d .
P2 P 0.20202(5) 0.44075(7) 0.50632(3) 0.01475(14) Uani 1 1 d .
O1 O -0.01680(15) 0.3672(2) 0.40768(10) 0.0202(4) Uani 1 1 d .
O2 O 0.11847(15) 0.5516(2) 0.50408(10) 0.0188(4) Uani 1 1 d .
H01 H 0.069(5) 0.589(6) 0.543(3) 0.09(2) Uiso 1 1 d .
C01 C 0.1557(2) 0.2750(3) 0.47469(13) 0.0161(5) Uani 1 1 d .
H01A H 0.2159 0.2145 0.4669 0.019 Uiso 1 1 calc R
H01B H 0.1150 0.2292 0.5085 0.019 Uiso 1 1 calc R
C11 C 0.0478(2) 0.0969(3) 0.38530(14) 0.0164(5) Uani 1 1 d .
C12 C 0.0729(2) -0.0138(3) 0.42693(14) 0.0201(6) Uani 1 1 d .
H12 H 0.1086 0.0041 0.4661 0.024 Uiso 1 1 calc R
C13 C 0.0449(2) -0.1503(3) 0.41027(16) 0.0247(6) Uani 1 1 d .
H13 H 0.0617 -0.2259 0.4382 0.030 Uiso 1 1 calc R
C14 C -0.0074(2) -0.1763(3) 0.35314(16) 0.0251(7) Uani 1 1 d .
H14 H -0.0271 -0.2695 0.3424 0.030 Uiso 1 1 calc R
C15 C -0.0311(2) -0.0665(3) 0.31154(16) 0.0249(6) Uani 1 1 d .
H15 H -0.0662 -0.0848 0.2722 0.030 Uiso 1 1 calc R
C16 C -0.0036(2) 0.0690(3) 0.32752(15) 0.0213(6) Uani 1 1 d .
H16 H -0.0198 0.1438 0.2991 0.026 Uiso 1 1 calc R
C21 C 0.1519(2) 0.3400(3) 0.33625(13) 0.0169(5) Uani 1 1 d .
C22 C 0.1050(2) 0.4263(3) 0.29058(14) 0.0193(6) Uani 1 1 d .
H22 H 0.0368 0.4582 0.2965 0.023 Uiso 1 1 calc R
C23 C 0.1589(2) 0.4654(3) 0.23619(15) 0.0246(6) Uani 1 1 d .
H23 H 0.1271 0.5229 0.2045 0.029 Uiso 1 1 calc R
C24 C 0.2589(2) 0.4206(3) 0.22822(15) 0.0253(7) Uani 1 1 d .
H24 H 0.2957 0.4479 0.1912 0.030 Uiso 1 1 calc R
C25 C 0.3055(2) 0.3360(3) 0.27415(15) 0.0235(6) Uani 1 1 d .
H25 H 0.3744 0.3071 0.2687 0.028 Uiso 1 1 calc R
C26 C 0.2523(2) 0.2932(3) 0.32803(14) 0.0199(6) Uani 1 1 d .
H26 H 0.2836 0.2330 0.3588 0.024 Uiso 1 1 calc R
C31 C 0.3075(2) 0.4948(3) 0.45880(14) 0.0174(6) Uani 1 1 d .
C32 C 0.3003(3) 0.6174(3) 0.42247(17) 0.0277(7) Uani 1 1 d .
H32 H 0.2413 0.6753 0.4248 0.033 Uiso 1 1 calc R
C33 C 0.3811(3) 0.6537(4) 0.38267(18) 0.0337(8) Uani 1 1 d .
H33 H 0.3770 0.7363 0.3573 0.040 Uiso 1 1 calc R
C34 C 0.4671(3) 0.5697(3) 0.38013(16) 0.0278(7) Uani 1 1 d .
H34 H 0.5213 0.5943 0.3523 0.033 Uiso 1 1 calc R
C35 C 0.4753(2) 0.4498(3) 0.41760(15) 0.0219(6) Uani 1 1 d .
H35 H 0.5354 0.3938 0.4162 0.026 Uiso 1 1 calc R
C36 C 0.3952(2) 0.4123(3) 0.45718(14) 0.0201(6) Uani 1 1 d .
H36 H 0.4003 0.3305 0.4831 0.024 Uiso 1 1 calc R
C41 C 0.2415(2) 0.3983(3) 0.58666(13) 0.0162(5) Uani 1 1 d .
C42 C 0.2350(2) 0.5019(3) 0.63425(14) 0.0198(6) Uani 1 1 d .
H42 H 0.2150 0.5948 0.6234 0.024 Uiso 1 1 calc R
C43 C 0.2583(2) 0.4672(3) 0.69707(15) 0.0227(6) Uani 1 1 d .
H43 H 0.2523 0.5362 0.7297 0.027 Uiso 1 1 calc R
C44 C 0.2905(2) 0.3324(3) 0.71323(14) 0.0209(6) Uani 1 1 d .
H44 H 0.3052 0.3094 0.7567 0.025 Uiso 1 1 calc R
C45 C 0.3011(2) 0.2316(3) 0.66569(14) 0.0212(6) Uani 1 1 d .
H45 H 0.3249 0.1403 0.6764 0.025 Uiso 1 1 calc R
C46 C 0.2767(2) 0.2646(3) 0.60253(14) 0.0187(6) Uani 1 1 d .
H46 H 0.2841 0.1958 0.5700 0.022 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 0.0181 0.0091 '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 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.7943 1.1372 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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_3
Br2 Se1 Br3 92.035(14) .
Br2 Se1 Br1 89.458(13) .
Br3 Se1 Br1 177.035(16) .
Br2 Se1 Br1 176.024(16) 3_656
Br3 Se1 Br1 91.721(13) 3_656
Br1 Se1 Br1 86.732(12) 3_656
Se1 Br1 Se1 93.268(12) 3_656
O1 P1 C21 108.58(13) .
O1 P1 C11 111.62(13) .
C21 P1 C11 106.85(13) .
O1 P1 C01 113.17(12) .
C21 P1 C01 110.64(13) .
C11 P1 C01 105.79(13) .
O2 P2 C31 109.97(13) .
O2 P2 C41 112.58(12) .
C31 P2 C41 111.67(13) .
O2 P2 C01 111.00(13) .
C31 P2 C01 107.86(13) .
C41 P2 C01 103.53(13) .
P1 C01 P2 118.21(15) .
C16 C11 C12 119.8(3) .
C16 C11 P1 117.0(2) .
C12 C11 P1 123.2(2) .
C13 C12 C11 119.3(3) .
C14 C13 C12 120.4(3) .
C13 C14 C15 120.2(3) .
C16 C15 C14 119.8(3) .
C15 C16 C11 120.5(3) .
C22 C21 C26 120.7(3) .
C22 C21 P1 119.2(2) .
C26 C21 P1 119.9(2) .
C23 C22 C21 119.4(3) .
C24 C23 C22 120.1(3) .
C23 C24 C25 120.2(3) .
C24 C25 C26 120.6(3) .
C25 C26 C21 119.0(3) .
C36 C31 C32 120.7(3) .
C36 C31 P2 119.5(2) .
C32 C31 P2 119.8(2) .
C33 C32 C31 119.0(3) .
C34 C33 C32 120.1(3) .
C33 C34 C35 120.9(3) .
C36 C35 C34 119.6(3) .
C35 C36 C31 119.7(3) .
C46 C41 C42 119.9(3) .
C46 C41 P2 121.3(2) .
C42 C41 P2 118.9(2) .
C43 C42 C41 119.1(3) .
C42 C43 C44 120.9(3) .
C45 C44 C43 119.9(3) .
C46 C45 C44 119.8(3) .
C45 C46 C41 120.3(3) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Se1 Br2 2.4099(4) .
Se1 Br3 2.4612(4) .
Se1 Br1 2.7600(4) .
Se1 Br1 2.9176(4) 3_656
Br1 Se1 2.9176(4) 3_656
P1 O1 1.520(2) .
P1 C21 1.784(3) .
P1 C11 1.803(3) .
P1 C01 1.805(3) .
P2 O2 1.519(2) .
P2 C31 1.782(3) .
P2 C41 1.793(3) .
P2 C01 1.813(3) .
C11 C16 1.398(4) .
C11 C12 1.402(4) .
C12 C13 1.394(4) .
C13 C14 1.388(5) .
C14 C15 1.392(5) .
C15 C16 1.380(4) .
C21 C22 1.395(4) .
C21 C26 1.397(4) .
C22 C23 1.393(4) .
C23 C24 1.386(5) .
C24 C25 1.387(4) .
C25 C26 1.390(4) .
C31 C36 1.391(4) .
C31 C32 1.395(4) .
C32 C33 1.394(5) .
C33 C34 1.380(5) .
C34 C35 1.387(5) .
C35 C36 1.387(4) .
C41 C46 1.393(4) .
C41 C42 1.404(4) .
C42 C43 1.381(4) .
C43 C44 1.392(4) .
C44 C45 1.388(4) .
C45 C46 1.387(4) .
