#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/11/7051157.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_7051157
loop_
_publ_author_name
'Marek Necas'
'Mark R. St J. Foreman'
'Jaromír Marek'
'J. Derek Woollins'
'Josef Novosad'
_publ_section_title
;
 New mixed-donor unsymmetrical P--N--P ligands and their palladium(II)
 complexes
;
_journal_issue                   10
_journal_name_full               'New J. Chem.'
_journal_page_first              1256
_journal_page_last               1263
_journal_paper_doi               10.1039/b103501k
_journal_volume                  25
_journal_year                    2001
_chemical_formula_moiety         Ph2P(Se)-NH-P(S)(OPh)2
_chemical_formula_sum            'C24 H21 N O2 P2 S Se'
_chemical_formula_weight         528.38
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           15
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 108.97(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.236(5)
_cell_length_b                   9.654(2)
_cell_length_c                   22.026(4)
_cell_measurement_temperature    293(2)
_cell_volume                     4672.5(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.416
_diffrn_measured_fraction_theta_max 0.416
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2880
_diffrn_reflns_theta_full        22.67
_diffrn_reflns_theta_max         22.67
_diffrn_reflns_theta_min         3.37
_exptl_absorpt_coefficient_mu    1.855
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.980
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         2789
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0768P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.1014
_reflns_number_gt                2268
_reflns_number_total             2789
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b103501k.txt
_cod_data_source_block           5.cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0768P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0768P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4672.5(16)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7051157
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Se Se 0.270825(16) 0.76585(4) 0.202641(17) 0.02262(19) Uani 1 d . . .
P2 P 0.36178(4) 0.75354(8) 0.25921(4) 0.0141(3) Uani 1 d . . .
S S 0.47369(4) 0.53359(8) 0.14809(4) 0.0182(3) Uani 1 d . . .
P1 P 0.40396(4) 0.63102(8) 0.15410(4) 0.0132(3) Uani 1 d . . .
O2 O 0.39504(10) 0.7858(2) 0.12871(11) 0.0152(5) Uani 1 d . . .
O1 O 0.34087(10) 0.5680(2) 0.11226(10) 0.0163(5) Uani 1 d . . .
N N 0.40442(14) 0.6517(3) 0.22752(15) 0.0155(7) Uani 1 d . . .
H0 H 0.4307(16) 0.619(4) 0.2508(17) 0.004(10) Uiso 1 d . . .
C16 C 0.40633(18) 0.5220(4) 0.44979(19) 0.0304(10) Uani 1 d . . .
H16 H 0.4176 0.4724 0.4881 0.036 Uiso 1 calc R . .
C22 C 0.4588(2) 1.1694(4) 0.3101(2) 0.0370(11) Uani 1 d . . .
H22 H 0.4785 1.2540 0.3213 0.044 Uiso 1 calc R . .
C21 C 0.49191(18) 1.0480(4) 0.32158(18) 0.0278(9) Uani 1 d . . .
H21 H 0.5339 1.0504 0.3409 0.033 Uiso 1 calc R . .
C1 C 0.32567(16) 0.4250(3) 0.11077(16) 0.0167(8) Uani 1 d . . .
C13 C 0.37698(15) 0.6674(3) 0.33573(16) 0.0163(8) Uani 1 d . . .
C17 C 0.37711(19) 0.4566(4) 0.39249(19) 0.0307(10) Uani 1 d . . .
H17 H 0.3672 0.3632 0.3922 0.037 Uiso 1 calc R . .
C18 C 0.36245(17) 0.5293(4) 0.33557(18) 0.0243(9) Uani 1 d . . .
H18 H 0.3427 0.4848 0.2970 0.029 Uiso 1 calc R . .
C19 C 0.39985(16) 0.9191(3) 0.27644(16) 0.0169(8) Uani 1 d . . .
C23 C 0.3966(2) 1.1652(4) 0.2821(2) 0.0364(11) Uani 1 d . . .
H23 H 0.3743 1.2471 0.2743 0.044 Uiso 1 calc R . .
C20 C 0.46229(16) 0.9230(4) 0.30420(17) 0.0217(9) Uani 1 d . . .
H20 H 0.4845 0.8411 0.3112 0.026 Uiso 1 calc R . .
C6 C 0.3416(2) 0.3406(4) 0.0698(2) 0.0384(11) Uani 1 d . . .
H6 H 0.3647 0.3742 0.0455 0.046 Uiso 1 calc R . .
C15 C 0.41872(17) 0.6616(4) 0.44998(18) 0.0275(10) Uani 1 d . . .
H15 H 0.4375 0.7065 0.4887 0.033 Uiso 1 calc R . .
C5 C 0.3230(2) 0.2036(5) 0.0646(2) 0.0517(14) Uani 1 d . . .
H5 H 0.3338 0.1440 0.0369 0.062 Uiso 1 calc R . .
C14 C 0.40367(17) 0.7353(4) 0.39351(18) 0.0198(9) Uani 1 d . . .
H14 H 0.4113 0.8299 0.3941 0.024 Uiso 1 calc R . .
C3 C 0.27266(18) 0.2435(4) 0.1407(2) 0.0243(9) Uani 1 d . . .
H3 H 0.2489 0.2109 0.1644 0.029 Uiso 1 calc R . .
C4 C 0.2886(2) 0.1561(4) 0.1003(2) 0.0348(10) Uani 1 d . . .
H4 H 0.2761 0.0641 0.0970 0.042 Uiso 1 calc R . .
C24 C 0.36734(18) 1.0409(4) 0.26572(18) 0.0254(9) Uani 1 d . . .
H24 H 0.3252 1.0387 0.2472 0.030 Uiso 1 calc R . .
C2 C 0.29130(16) 0.3800(4) 0.14674(17) 0.0201(8) Uani 1 d . . .
H2 H 0.2808 0.4396 0.1746 0.024 Uiso 1 calc R . .
C12 C 0.32300(16) 0.8372(3) 0.02569(17) 0.0186(8) Uani 1 d . . .
H12 H 0.2914 0.8212 0.0420 0.022 Uiso 1 calc R . .
C7 C 0.38247(15) 0.8200(3) 0.06391(16) 0.0140(8) Uani 1 d . . .
C9 C 0.41660(18) 0.8852(4) -0.02195(18) 0.0276(10) Uani 1 d . . .
H9 H 0.4482 0.9024 -0.0382 0.033 Uiso 1 calc R . .
C8 C 0.42982(17) 0.8419(4) 0.04050(17) 0.0240(9) Uani 1 d . . .
H8 H 0.4699 0.8279 0.0664 0.029 Uiso 1 calc R . .
C11 C 0.31106(18) 0.8779(3) -0.03621(17) 0.0240(9) Uani 1 d . . .
H11 H 0.2709 0.8890 -0.0625 0.029 Uiso 1 calc R . .
C10 C 0.35793(18) 0.9031(4) -0.06043(18) 0.0254(9) Uani 1 d . . .
H10 H 0.3495 0.9320 -0.1027 0.030 Uiso 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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 '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'
O O 0.0106 0.0060 '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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N P2 C19 106.70(15) . . ?
N P2 C13 98.82(15) . . ?
C19 P2 C13 106.10(16) . . ?
N P2 Se 113.70(12) . . ?
C19 P2 Se 114.11(12) . . ?
C13 P2 Se 115.94(12) . . ?
O1 P1 O2 99.65(13) . . ?
O1 P1 N 109.42(14) . . ?
O2 P1 N 101.14(14) . . ?
O1 P1 S 114.61(10) . . ?
O2 P1 S 117.08(10) . . ?
N P1 S 113.37(12) . . ?
C7 O2 P1 122.8(2) . . ?
C1 O1 P1 124.4(2) . . ?
P1 N P2 131.6(2) . . ?
C17 C16 C15 119.5(4) . . ?
C23 C22 C21 120.0(4) . . ?
C22 C21 C20 119.6(4) . . ?
C6 C1 C2 122.3(3) . . ?
C6 C1 O1 118.6(3) . . ?
C2 C1 O1 118.9(3) . . ?
C18 C13 C14 119.8(3) . . ?
C18 C13 P2 118.0(3) . . ?
C14 C13 P2 122.1(3) . . ?
C16 C17 C18 120.1(4) . . ?
C13 C18 C17 120.2(4) . . ?
C24 C19 C20 119.5(3) . . ?
C24 C19 P2 121.1(3) . . ?
C20 C19 P2 119.4(3) . . ?
C24 C23 C22 120.2(4) . . ?
C19 C20 C21 120.3(3) . . ?
C1 C6 C5 118.9(4) . . ?
C14 C15 C16 120.8(4) . . ?
C4 C5 C6 119.8(4) . . ?
C15 C14 C13 119.4(3) . . ?
C4 C3 C2 120.8(4) . . ?
C3 C4 C5 120.0(4) . . ?
C23 C24 C19 120.4(4) . . ?
C1 C2 C3 118.2(3) . . ?
C11 C12 C7 119.1(3) . . ?
C12 C7 C8 121.3(3) . . ?
C12 C7 O2 119.2(3) . . ?
C8 C7 O2 119.4(3) . . ?
C10 C9 C8 121.0(4) . . ?
C9 C8 C7 118.5(3) . . ?
C12 C11 C10 120.6(4) . . ?
C9 C10 C11 119.5(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Se P2 2.0787(12) . ?
P2 N 1.699(3) . ?
P2 C19 1.806(3) . ?
P2 C13 1.808(3) . ?
S P1 1.9148(12) . ?
P1 O1 1.578(2) . ?
P1 O2 1.586(2) . ?
P1 N 1.626(3) . ?
O2 C7 1.400(4) . ?
O1 C1 1.423(4) . ?
C16 C17 1.377(6) . ?
C16 C15 1.378(6) . ?
C22 C23 1.375(6) . ?
C22 C21 1.380(6) . ?
C21 C20 1.380(5) . ?
C1 C6 1.354(5) . ?
C1 C2 1.366(5) . ?
C13 C18 1.375(5) . ?
C13 C14 1.386(5) . ?
C17 C18 1.380(5) . ?
C19 C24 1.376(5) . ?
C19 C20 1.380(5) . ?
C23 C24 1.369(5) . ?
C6 C5 1.385(6) . ?
C15 C14 1.376(5) . ?
C5 C4 1.372(6) . ?
C3 C4 1.361(5) . ?
C3 C2 1.379(5) . ?
C12 C11 1.358(5) . ?
C12 C7 1.375(5) . ?
C7 C8 1.375(5) . ?
C9 C10 1.362(5) . ?
C9 C8 1.373(5) . ?
C11 C10 1.381(5) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N H0 S 0.73(4) 2.71(4) 3.432(4) 170(3) 2_655
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30652865
