#------------------------------------------------------------------------------
#$Date: 2019-11-17 10:44:13 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229408 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/55/7045509.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_7045509
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            'C14 H32 Br6 Cl2 P2 Se'
_chemical_formula_weight         891.66
_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
;
2016-07-19 deposited with the CCDC.
2018-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.973(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1753(2)
_cell_length_b                   19.4723(4)
_cell_length_c                   14.0281(2)
_cell_measurement_reflns_used    30087
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.3060
_cell_measurement_theta_min      2.2830
_cell_volume                     2752.61(9)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_sigmaI/netI    0.0225
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            164062
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         2.28
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.385
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74504
_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    2.152
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.3000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_refine_diff_density_max         1.708
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         7717
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0253
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0170P)²+3.7050P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0457
_refine_ls_wR_factor_ref         0.0476
_reflns_number_gt                6755
_reflns_number_total             7717
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt04531j2.cif
_cod_data_source_block           noel
_cod_depositor_comments
'Adding full bibliography for 7045509--7045531.cif.'
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7045509
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 0.21806(2) 0.670849(11) 0.566675(16) 0.00978(5) Uani 1 1 d .
Br1 Br 0.51268(2) 0.568441(13) 0.606673(18) 0.01759(5) Uani 1 1 d .
Br2 Br 0.57763(2) 0.742873(12) 0.557578(18) 0.01508(5) Uani 1 1 d .
Br3 Br 0.17748(3) 0.537968(12) 0.547069(17) 0.01631(5) Uani 1 1 d .
Br4 Br 0.25527(3) 0.679571(12) 0.390469(17) 0.01577(5) Uani 1 1 d .
Br5 Br 0.26187(3) 0.798577(12) 0.593617(18) 0.01678(5) Uani 1 1 d .
Br6 Br 0.17526(3) 0.656578(12) 0.744918(16) 0.01620(5) Uani 1 1 d .
P1 P 0.71202(6) 0.58436(3) 0.67638(4) 0.01034(11) Uani 1 1 d .
P2 P 0.76411(6) 0.70168(3) 0.52644(4) 0.00952(11) Uani 1 1 d .
C01 C 0.8111(2) 0.62247(11) 0.59244(16) 0.0100(4) Uani 1 1 d .
H01A H 0.8215 0.5869 0.5436 0.012 Uiso 1 1 calc R
H01B H 0.9005 0.6304 0.6286 0.012 Uiso 1 1 calc R
C1 C 0.7744(2) 0.49782(11) 0.70184(17) 0.0127(4) Uani 1 1 d .
H1 H 0.7475 0.4705 0.6420 0.015 Uiso 1 1 calc R
C2 C 0.7120(2) 0.64241(12) 0.77825(17) 0.0133(5) Uani 1 1 d .
H2 H 0.7093 0.6901 0.7517 0.016 Uiso 1 1 calc R
C3 C 0.8902(2) 0.76567(12) 0.56168(17) 0.0122(4) Uani 1 1 d .
H3 H 0.9771 0.7463 0.5489 0.015 Uiso 1 1 calc R
C4 C 0.7465(2) 0.68371(12) 0.39893(16) 0.0140(5) Uani 1 1 d .
H4 H 0.7198 0.7274 0.3642 0.017 Uiso 1 1 calc R
C11 C 0.7054(3) 0.46459(13) 0.78052(19) 0.0202(5) Uani 1 1 d .
H11A H 0.7298 0.4159 0.7865 0.030 Uiso 1 1 calc R
H11B H 0.6090 0.4687 0.7635 0.030 Uiso 1 1 calc R
H11C H 0.7332 0.4879 0.8420 0.030 Uiso 1 1 calc R
C12 C 0.9246(3) 0.49269(13) 0.72318(19) 0.0186(5) Uani 1 1 d .
H12A H 0.9555 0.5162 0.7839 0.028 Uiso 1 1 calc R
H12B H 0.9645 0.5143 0.6710 0.028 Uiso 1 1 calc R
H12C H 0.9508 0.4443 0.7284 0.028 Uiso 1 1 calc R
C21 C 0.5921(3) 0.63506(14) 0.8314(2) 0.0241(6) Uani 1 1 d .
H21A H 0.5904 0.5887 0.8583 0.036 Uiso 1 1 calc R
H21B H 0.5108 0.6429 0.7866 0.036 Uiso 1 1 calc R
H21C H 0.5980 0.6688 0.8836 0.036 Uiso 1 1 calc R
C22 C 0.8438(3) 0.63563(13) 0.84616(17) 0.0168(5) Uani 1 1 d .
H22A H 0.8512 0.6730 0.8934 0.025 Uiso 1 1 calc R
H22B H 0.9180 0.6382 0.8086 0.025 Uiso 1 1 calc R
H22C H 0.8461 0.5914 0.8797 0.025 Uiso 1 1 calc R
C31 C 0.8641(3) 0.83052(13) 0.50073(19) 0.0189(5) Uani 1 1 d .
H31A H 0.7813 0.8519 0.5139 0.028 Uiso 1 1 calc R
H31B H 0.8564 0.8184 0.4324 0.028 Uiso 1 1 calc R
H31C H 0.9377 0.8628 0.5168 0.028 Uiso 1 1 calc R
C32 C 0.9024(3) 0.78188(13) 0.66950(17) 0.0162(5) Uani 1 1 d .
H32A H 0.9714 0.8166 0.6861 0.024 Uiso 1 1 calc R
H32B H 0.9261 0.7400 0.7066 0.024 Uiso 1 1 calc R
H32C H 0.8174 0.7994 0.6847 0.024 Uiso 1 1 calc R
C41 C 0.8815(3) 0.66212(14) 0.37105(18) 0.0199(5) Uani 1 1 d .
H41A H 0.9079 0.6178 0.4009 0.030 Uiso 1 1 calc R
H41B H 0.9483 0.6969 0.3936 0.030 Uiso 1 1 calc R
H41C H 0.8743 0.6579 0.3009 0.030 Uiso 1 1 calc R
C42 C 0.6375(3) 0.63058(13) 0.36825(18) 0.0199(5) Uani 1 1 d .
H42A H 0.6276 0.6244 0.2983 0.030 Uiso 1 1 calc R
H42B H 0.5534 0.6467 0.3869 0.030 Uiso 1 1 calc R
H42C H 0.6619 0.5867 0.4000 0.030 Uiso 1 1 calc R
C99 C 0.2296(3) 0.48380(14) 0.8540(2) 0.0204(5) Uani 1 1 d .
H99A H 0.1963 0.4383 0.8300 0.024 Uiso 1 1 calc R
H99B H 0.2121 0.5170 0.8003 0.024 Uiso 1 1 calc R
Cl98 Cl 0.40143(7) 0.47882(4) 0.89206(7) 0.0407(2) Uani 1 1 d .
Cl99 Cl 0.14416(8) 0.50981(4) 0.94911(5) 0.03061(16) Uani 1 1 d .
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'
Cl Cl 0.1484 0.1585 '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
Br5 Se1 Br4 91.849(10)
Br5 Se1 Br6 90.620(10)
Br4 Se1 Br6 177.447(12)
Br5 Se1 Br3 177.386(13)
Br4 Se1 Br3 90.368(10)
Br6 Se1 Br3 87.180(10)
C01 P1 C1 107.25(11)
C01 P1 C2 108.43(11)
C1 P1 C2 117.31(11)
C01 P1 Br1 109.80(8)
C1 P1 Br1 103.74(8)
C2 P1 Br1 110.11(8)
C4 P2 C3 111.92(11)
C4 P2 C01 108.72(11)
C3 P2 C01 108.48(11)
C4 P2 Br2 107.63(8)
C3 P2 Br2 107.40(8)
C01 P2 Br2 112.74(8)
P1 C01 P2 122.99(13)
C12 C1 C11 112.3(2)
C12 C1 P1 114.44(17)
C11 C1 P1 110.52(17)
C21 C2 C22 112.2(2)
C21 C2 P1 114.40(17)
C22 C2 P1 109.73(16)
C31 C3 C32 111.47(19)
C31 C3 P2 110.78(17)
C32 C3 P2 111.63(16)
C42 C4 C41 112.4(2)
C42 C4 P2 112.14(17)
C41 C4 P2 109.59(17)
Cl98 C99 Cl99 111.05(15)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Se1 Br5 2.5457(3)
Se1 Br4 2.5577(3)
Se1 Br6 2.6117(3)
Se1 Br3 2.6286(3)
Br1 P1 2.1486(7)
Br2 P2 2.1597(6)
P1 C01 1.812(2)
P1 C1 1.819(2)
P1 C2 1.822(2)
P2 C4 1.807(2)
P2 C3 1.808(2)
P2 C01 1.828(2)
C1 C12 1.520(3)
C1 C11 1.531(3)
C2 C21 1.523(3)
C2 C22 1.539(3)
C3 C31 1.528(3)
C3 C32 1.533(3)
C4 C42 1.534(3)
C4 C41 1.538(3)
C99 Cl98 1.759(3)
C99 Cl99 1.765(3)
