#------------------------------------------------------------------------------
#$Date: 2019-11-17 10:44:13 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229408 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/55/7045516.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_7045516
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 I4 P2 Se2'
_chemical_formula_weight         927.86
_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
;
2017-09-13 deposited with the CCDC.
2018-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                105.549(8)
_cell_angle_beta                 98.760(8)
_cell_angle_gamma                98.357(8)
_cell_formula_units_Z            1
_cell_length_a                   7.7755(7)
_cell_length_b                   9.3550(8)
_cell_length_c                   9.4012(9)
_cell_measurement_reflns_used    7113
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.6740
_cell_measurement_theta_min      2.6930
_cell_volume                     638.56(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Siemens 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 0.988
_diffrn_measured_fraction_theta_max 0.931
_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  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            24473
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         31.03
_diffrn_reflns_theta_min         2.30
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    7.852
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.413
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             426
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.137
_refine_ls_extinction_coef       0.00257(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         3805
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0220
_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)+(0.0117P)²+0.1356P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0382
_refine_ls_wR_factor_ref         0.0401
_reflns_number_gt                3313
_reflns_number_total             3805
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt04531j2.cif
_cod_data_source_block           theon
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7045509--7045531.cif.
;
_cod_original_cell_volume        638.56(10)
_cod_database_code               7045516
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
I1 I 0.120010(18) 0.737122(17) 0.529446(16) 0.01147(5) Uani 1 1 d .
I2 I -0.10563(2) 0.796957(19) 0.287462(18) 0.01860(5) Uani 1 1 d .
Se1 Se 0.31957(3) 0.68359(3) 0.77668(3) 0.01312(6) Uani 1 1 d .
P1 P 0.58069(7) 0.68233(7) 0.72333(7) 0.00956(12) Uani 1 1 d .
C01 C 0.5729(3) 0.5717(3) 0.5295(2) 0.0116(5) Uani 1 1 d .
H01A H 0.5544 0.6366 0.4631 0.014 Uiso 1 1 calc R
H01B H 0.6892 0.5420 0.5228 0.014 Uiso 1 1 calc R
C1 C 0.7031(3) 0.6030(3) 0.8554(3) 0.0124(5) Uani 1 1 d .
H1 H 0.6947 0.6629 0.9587 0.015 Uiso 1 1 calc R
C12 C 0.9008(3) 0.6219(3) 0.8502(3) 0.0147(5) Uani 1 1 d .
H12A H 0.9632 0.5882 0.9302 0.022 Uiso 1 1 calc R
H12B H 0.9499 0.7286 0.8652 0.022 Uiso 1 1 calc R
H12C H 0.9157 0.5610 0.7520 0.022 Uiso 1 1 calc R
C11 C 0.6235(3) 0.4382(3) 0.8371(3) 0.0174(5) Uani 1 1 d .
H11A H 0.6475 0.3729 0.7447 0.026 Uiso 1 1 calc R
H11B H 0.4950 0.4267 0.8308 0.026 Uiso 1 1 calc R
H11C H 0.6770 0.4094 0.9240 0.026 Uiso 1 1 calc R
C2 C 0.7047(3) 0.8716(3) 0.7465(3) 0.0132(5) Uani 1 1 d .
H2 H 0.8203 0.8605 0.7149 0.016 Uiso 1 1 calc R
C22 C 0.6066(3) 0.9522(3) 0.6472(3) 0.0198(6) Uani 1 1 d .
H22A H 0.4935 0.9664 0.6774 0.030 Uiso 1 1 calc R
H22B H 0.5840 0.8908 0.5415 0.030 Uiso 1 1 calc R
H22C H 0.6795 1.0511 0.6593 0.030 Uiso 1 1 calc R
C21 C 0.7451(3) 0.9682(3) 0.9114(3) 0.0195(5) Uani 1 1 d .
H21A H 0.8111 1.0689 0.9207 0.029 Uiso 1 1 calc R
H21B H 0.8164 0.9200 0.9729 0.029 Uiso 1 1 calc R
H21C H 0.6336 0.9777 0.9463 0.029 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'
I I -0.4742 1.8119 '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
Se1 I1 I2 175.764(8) .
P1 Se1 I1 104.162(19) .
C01 P1 C1 110.31(11) .
C01 P1 C2 106.23(11) .
C1 P1 C2 107.89(11) .
C01 P1 Se1 112.65(7) .
C1 P1 Se1 106.62(7) .
C2 P1 Se1 113.06(8) .
C01 C01 P1 114.4(2) 2_666
C11 C1 C12 110.8(2) .
C11 C1 P1 113.39(15) .
C12 C1 P1 112.29(16) .
C21 C2 C22 110.0(2) .
C21 C2 P1 111.10(17) .
C22 C2 P1 111.95(16) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 Se1 2.7950(4) .
I1 I2 2.8843(3) .
Se1 P1 2.1652(6) .
P1 C01 1.826(2) .
P1 C1 1.827(2) .
P1 C2 1.829(2) .
C01 C01 1.535(4) 2_666
C1 C11 1.529(3) .
C1 C12 1.531(3) .
C2 C21 1.528(3) .
C2 C22 1.533(3) .
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
I1 Se1 P1 C01 -45.32(9) .
I1 Se1 P1 C1 -166.47(8) .
I1 Se1 P1 C2 75.13(8) .
C1 P1 C01 C01 82.3(2) 2_666
C2 P1 C01 C01 -161.1(2) 2_666
Se1 P1 C01 C01 -36.8(3) 2_666
C01 P1 C1 C11 -58.61(19) .
C2 P1 C1 C11 -174.25(16) .
Se1 P1 C1 C11 64.02(17) .
C01 P1 C1 C12 67.91(19) .
C2 P1 C1 C12 -47.7(2) .
Se1 P1 C1 C12 -169.47(15) .
C01 P1 C2 C21 -171.21(17) .
C1 P1 C2 C21 -52.92(19) .
Se1 P1 C2 C21 64.74(18) .
C01 P1 C2 C22 65.34(19) .
C1 P1 C2 C22 -176.37(16) .
Se1 P1 C2 C22 -58.71(18) .
