#------------------------------------------------------------------------------
#$Date: 2019-11-17 10:44:13 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229408 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/55/7045519.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_7045519
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            'C38 H36 Br4 P2 Se2'
_chemical_formula_weight         1032.16
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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
;
2016-07-19 deposited with the CCDC.
2018-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.656(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.2185(2)
_cell_length_b                   6.7500(2)
_cell_length_c                   24.9397(5)
_cell_measurement_reflns_used    16243
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.0660
_cell_measurement_theta_min      3.9300
_cell_volume                     1884.71(8)
_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  SHEXL-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 0.996
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Atlas, Nova'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            36988
_diffrn_reflns_theta_full        75.00
_diffrn_reflns_theta_max         76.34
_diffrn_reflns_theta_min         3.55
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    8.426
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29393
_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            yellow
_exptl_crystal_density_diffrn    1.819
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3942
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0292
_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)+(0.0378P)²+2.3074P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0759
_reflns_number_gt                3634
_reflns_number_total             3942
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt04531j2.cif
_cod_data_source_block           monty
_cod_depositor_comments
'Adding full bibliography for 7045509--7045531.cif.'
_cod_original_cell_volume        1884.72(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7045519
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Br1 Br 0.76987(3) 0.15116(4) 0.360840(12) 0.02401(9) Uani 1 1 d .
Br2 Br 0.64357(3) 0.09797(4) 0.554389(11) 0.02118(9) Uani 1 1 d .
Se1 Se 0.69684(2) 0.13022(4) 0.456195(11) 0.01729(9) Uani 1 1 d .
P1 P 0.65324(5) 0.45497(9) 0.44888(2) 0.01289(13) Uani 1 1 d .
C1 C 0.5640(2) 0.5416(4) 0.50260(10) 0.0143(5) Uani 1 1 d .
H1A H 0.6029 0.5008 0.5376 0.017 Uiso 1 1 calc R
H1B H 0.5608 0.6881 0.5019 0.017 Uiso 1 1 calc R
C11 C 0.7904(2) 0.5918(4) 0.45388(10) 0.0146(5) Uani 1 1 d .
C12 C 0.8385(2) 0.6553(4) 0.50423(11) 0.0172(5) Uani 1 1 d .
H12 H 0.7951 0.6379 0.5354 0.021 Uiso 1 1 calc R
C13 C 0.9506(2) 0.7439(4) 0.50804(11) 0.0202(5) Uani 1 1 d .
H13 H 0.9845 0.7860 0.5420 0.024 Uiso 1 1 calc R
C14 C 1.0131(2) 0.7712(4) 0.46247(12) 0.0210(5) Uani 1 1 d .
H14 H 1.0896 0.8321 0.4655 0.025 Uiso 1 1 calc R
C15 C 0.9652(2) 0.7107(4) 0.41245(12) 0.0206(5) Uani 1 1 d .
H15 H 1.0081 0.7321 0.3813 0.025 Uiso 1 1 calc R
C16 C 0.8541(2) 0.6186(4) 0.40804(11) 0.0184(5) Uani 1 1 d .
H16 H 0.8217 0.5740 0.3740 0.022 Uiso 1 1 calc R
C21 C 0.5688(2) 0.5062(4) 0.38683(10) 0.0149(5) Uani 1 1 d .
C22 C 0.5771(2) 0.6928(4) 0.36328(11) 0.0189(5) Uani 1 1 d .
H22 H 0.6316 0.7884 0.3784 0.023 Uiso 1 1 calc R
C23 C 0.5049(3) 0.7376(5) 0.31751(11) 0.0236(6) Uani 1 1 d .
H23 H 0.5109 0.8635 0.3009 0.028 Uiso 1 1 calc R
C24 C 0.4241(3) 0.5991(5) 0.29606(11) 0.0259(6) Uani 1 1 d .
H24 H 0.3748 0.6306 0.2648 0.031 Uiso 1 1 calc R
C25 C 0.4149(3) 0.4141(5) 0.32006(12) 0.0271(6) Uani 1 1 d .
H25 H 0.3589 0.3202 0.3053 0.032 Uiso 1 1 calc R
C26 C 0.4870(2) 0.3660(4) 0.36542(11) 0.0204(5) Uani 1 1 d .
H26 H 0.4810 0.2395 0.3818 0.024 Uiso 1 1 calc R
C91 C 0.7924(3) -0.0583(5) 0.74648(13) 0.0273(6) Uani 1 1 d .
H91 H 0.7499 0.0233 0.7697 0.033 Uiso 1 1 calc R
C92 C 0.8096(3) 0.0048(5) 0.69479(13) 0.0262(6) Uani 1 1 d .
H92 H 0.7793 0.1292 0.6824 0.031 Uiso 1 1 calc R
C93 C 0.8721(3) -0.1168(5) 0.66113(14) 0.0318(7) Uani 1 1 d .
H93 H 0.8832 -0.0762 0.6253 0.038 Uiso 1 1 calc R
C94 C 0.9180(3) -0.2956(5) 0.67955(16) 0.0362(8) Uani 1 1 d .
H94 H 0.9621 -0.3761 0.6567 0.043 Uiso 1 1 calc R
C95 C 0.8997(3) -0.3585(5) 0.73146(15) 0.0316(7) Uani 1 1 d .
H95 H 0.9303 -0.4824 0.7441 0.038 Uiso 1 1 calc R
C96 C 0.8366(3) -0.2389(5) 0.76456(12) 0.0284(6) Uani 1 1 d .
H96 H 0.8234 -0.2812 0.8000 0.034 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'
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 Br2 95.58(2) .
P1 Se1 Br1 87.240(19) .
Br2 Se1 Br1 174.626(15) .
C11 P1 C21 111.34(12) .
C11 P1 C1 107.06(12) .
C21 P1 C1 106.75(11) .
C11 P1 Se1 108.37(8) .
C21 P1 Se1 110.95(9) .
C1 P1 Se1 112.34(9) .
C1 C1 P1 112.0(2) 3_666
C16 C11 C12 120.4(2) .
C16 C11 P1 119.4(2) .
C12 C11 P1 120.0(2) .
C13 C12 C11 119.2(3) .
C14 C13 C12 120.3(3) .
C13 C14 C15 120.7(2) .
C14 C15 C16 119.8(3) .
C15 C16 C11 119.7(3) .
C22 C21 C26 120.6(2) .
C22 C21 P1 119.4(2) .
C26 C21 P1 119.7(2) .
C23 C22 C21 119.4(3) .
C24 C23 C22 120.2(3) .
C23 C24 C25 120.3(3) .
C26 C25 C24 120.4(3) .
C25 C26 C21 119.1(3) .
C96 C91 C92 120.5(3) .
C91 C92 C93 119.0(3) .
C94 C93 C92 120.4(3) .
C93 C94 C95 120.2(3) .
C96 C95 C94 119.3(3) .
C91 C96 C95 120.5(3) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 Se1 2.5681(4) .
Br2 Se1 2.5668(4) .
Se1 P1 2.2509(7) .
P1 C11 1.792(3) .
P1 C21 1.796(3) .
P1 C1 1.819(2) .
C1 C1 1.540(5) 3_666
C11 C16 1.398(4) .
C11 C12 1.402(4) .
C12 C13 1.390(4) .
C13 C14 1.385(4) .
C14 C15 1.388(4) .
C15 C16 1.390(4) .
C21 C22 1.395(4) .
C21 C26 1.401(4) .
C22 C23 1.391(4) .
C23 C24 1.385(4) .
C24 C25 1.391(5) .
C25 C26 1.387(4) .
C91 C96 1.381(5) .
C91 C92 1.383(4) .
C92 C93 1.395(5) .
C93 C94 1.379(5) .
C94 C95 1.390(5) .
C95 C96 1.382(5) .
