#------------------------------------------------------------------------------
#$Date: 2019-11-17 10:44:13 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229408 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/55/7045515.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_7045515
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 Br4 P2 Se2'
_chemical_formula_weight         739.90
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                90.00
_cell_angle_beta                 107.253(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.2568(5)
_cell_length_b                   9.4204(3)
_cell_length_c                   15.9393(6)
_cell_measurement_reflns_used    14377
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.5910
_cell_measurement_theta_min      2.5040
_cell_volume                     2331.20(14)
_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 0.998
_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  0.0693
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            87552
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.53
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    10.161
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66876
_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            yellow
_exptl_crystal_density_diffrn    2.108
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.205
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         3402
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.205
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0323
_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)+(0.0176P)²+4.7085P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0517
_refine_ls_wR_factor_ref         0.0531
_reflns_number_gt                3114
_reflns_number_total             3402
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt04531j2.cif
_cod_data_source_block           tywin
_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        2331.19(14)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7045515
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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 0.372188(15) 0.69862(3) 0.721251(16) 0.01050(6) Uani 1 1 d .
Br1 Br 0.447854(16) 0.83931(3) 0.627671(18) 0.01826(7) Uani 1 1 d .
Br2 Br 0.313258(17) 0.55640(3) 0.830495(16) 0.01424(6) Uani 1 1 d .
P1 P 0.29365(4) 0.57556(6) 0.60299(4) 0.00812(12) Uani 1 1 d .
C01 C 0.26976(16) 0.6761(2) 0.50033(15) 0.0093(5) Uani 1 1 d .
H1A H 0.3240 0.6867 0.4846 0.011 Uiso 1 1 calc R
H1B H 0.2299 0.6189 0.4535 0.011 Uiso 1 1 calc R
C1 C 0.35673(16) 0.4223(3) 0.58772(17) 0.0117(5) Uani 1 1 d .
H2 H 0.3231 0.3733 0.5326 0.014 Uiso 1 1 calc R
C11 C 0.36962(17) 0.3161(3) 0.66298(18) 0.0163(5) Uani 1 1 d .
H3A H 0.4028 0.2346 0.6525 0.024 Uiso 1 1 calc R
H3B H 0.3134 0.2837 0.6663 0.024 Uiso 1 1 calc R
H3C H 0.4010 0.3619 0.7184 0.024 Uiso 1 1 calc R
C12 C 0.44372(18) 0.4640(3) 0.5766(2) 0.0206(6) Uani 1 1 d .
H4A H 0.4786 0.5115 0.6300 0.031 Uiso 1 1 calc R
H4B H 0.4346 0.5287 0.5265 0.031 Uiso 1 1 calc R
H4C H 0.4737 0.3787 0.5661 0.031 Uiso 1 1 calc R
C2 C 0.19376(15) 0.5091(3) 0.61948(17) 0.0110(5) Uani 1 1 d .
H5 H 0.2106 0.4550 0.6760 0.013 Uiso 1 1 calc R
C21 C 0.13265(17) 0.6274(3) 0.62981(18) 0.0166(5) Uani 1 1 d .
H6A H 0.1014 0.6651 0.5718 0.025 Uiso 1 1 calc R
H6B H 0.1661 0.7037 0.6661 0.025 Uiso 1 1 calc R
H6C H 0.0915 0.5890 0.6581 0.025 Uiso 1 1 calc R
C22 C 0.14955(17) 0.4026(3) 0.54700(17) 0.0147(5) Uani 1 1 d .
H7A H 0.0956 0.3700 0.5561 0.022 Uiso 1 1 calc R
H7B H 0.1877 0.3213 0.5492 0.022 Uiso 1 1 calc R
H7C H 0.1372 0.4488 0.4895 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 0.0033 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
P1 Se1 Br1 91.705(18) .
P1 Se1 Br2 93.740(18) .
Br1 Se1 Br2 173.137(13) .
C1 P1 C01 105.57(11) .
C1 P1 C2 107.78(12) .
C01 P1 C2 110.09(12) .
C1 P1 Se1 108.41(9) .
C01 P1 Se1 113.46(8) .
C2 P1 Se1 111.21(8) .
C01 C01 P1 117.0(2) 7_566
C11 C1 C12 110.1(2) .
C11 C1 P1 111.35(17) .
C12 C1 P1 112.77(18) .
C21 C2 C22 112.4(2) .
C21 C2 P1 113.39(17) .
C22 C2 P1 110.61(17) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Se1 P1 2.2583(7) .
Se1 Br1 2.5657(4) .
Se1 Br2 2.5951(4) .
P1 C1 1.829(2) .
P1 C01 1.830(2) .
P1 C2 1.831(2) .
C01 C01 1.531(5) 7_566
C1 C11 1.528(3) .
C1 C12 1.528(4) .
C2 C21 1.534(4) .
C2 C22 1.538(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
Br1 Se1 P1 C1 86.17(9) .
Br2 Se1 P1 C1 -89.65(9) .
Br1 Se1 P1 C01 -30.76(9) .
Br2 Se1 P1 C01 153.42(9) .
Br1 Se1 P1 C2 -155.51(9) .
Br2 Se1 P1 C2 28.67(9) .
C1 P1 C01 C01 -170.1(2) 7_566
C2 P1 C01 C01 73.9(3) 7_566
Se1 P1 C01 C01 -51.5(3) 7_566
C01 P1 C1 C11 -171.18(18) .
C2 P1 C1 C11 -53.5(2) .
Se1 P1 C1 C11 66.93(19) .
C01 P1 C1 C12 64.5(2) .
C2 P1 C1 C12 -177.89(19) .
Se1 P1 C1 C12 -57.4(2) .
C1 P1 C2 C21 -177.84(18) .
C01 P1 C2 C21 -63.2(2) .
Se1 P1 C2 C21 63.46(19) .
C1 P1 C2 C22 -50.5(2) .
C01 P1 C2 C22 64.2(2) .
Se1 P1 C2 C22 -169.21(14) .
