#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:12:50 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180065 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/11/7051159.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_7051159
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         iPr2P(S)-NH-P(S)(OPh)2
_chemical_formula_sum            'C18 H25 N O2 P2 S2'
_chemical_formula_weight         413.45
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_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
_cell_angle_alpha                97.97(3)
_cell_angle_beta                 104.38(3)
_cell_angle_gamma                92.35(3)
_cell_formula_units_Z            2
_cell_length_a                   8.494(2)
_cell_length_b                   9.173(2)
_cell_length_c                   13.751(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1024.6(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_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  0.0163
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3764
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         3.69
_exptl_absorpt_coefficient_mu    0.428
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             436
_refine_diff_density_max         1.128
_refine_diff_density_min         -0.933
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         3602
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0771
_refine_ls_shift/su_max          1.306
_refine_ls_shift/su_mean         0.019
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0745P)²+3.1152P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1908
_refine_ls_wR_factor_ref         0.2127
_reflns_number_gt                2585
_reflns_number_total             3602
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b103501k.txt
_cod_data_source_block           7.cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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^)+(0.0745P)^2^+3.1152P] 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^)+(0.0745P)^2^+3.1152P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7051159
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.32126(16) 0.66449(17) 0.58888(11) 0.0529(4) Uani 1 d . . .
P2 P 0.64334(17) 0.73491(18) 0.75645(10) 0.0544(5) Uani 1 d . . .
S1 S 0.2961(2) 0.6248(2) 0.44314(13) 0.0821(6) Uani 1 d . . .
S2 S 0.5567(2) 0.8442(2) 0.85402(13) 0.0846(7) Uani 1 d . . .
N1 N 0.5147(6) 0.6485(6) 0.6535(4) 0.0480(12) Uani 1 d . . .
O2 O 0.7596(5) 0.6127(5) 0.7950(3) 0.0796(15) Uani 1 d . . .
O1 O 0.7631(4) 0.8251(5) 0.7106(3) 0.0626(12) Uani 1 d . . .
C31 C 0.1946(7) 0.5359(8) 0.6295(5) 0.0649(17) Uani 1 d . . .
C32 C 0.2321(15) 0.3859(9) 0.5998(10) 0.108(3) Uani 1 d . . .
C6 C 0.9940(7) 0.9190(8) 0.8516(4) 0.0595(15) Uani 1 d . . .
C4 C 1.1131(9) 1.1627(10) 0.8602(6) 0.084(2) Uani 1 d . . .
C33 C 0.1914(9) 0.5732(8) 0.7384(6) 0.0664(17) Uani 1 d . . .
C3 C 0.9947(11) 1.1813(12) 0.7770(7) 0.111(3) Uani 1 d . . .
C1 C 0.8791(6) 0.9386(7) 0.7666(4) 0.0598(16) Uani 1 d . . .
C23 C 0.0925(13) 0.8633(12) 0.5749(8) 0.151(5) Uani 1 d . . .
H23A H 0.0261 0.7894 0.5928 0.227 Uiso 1 d R . .
H23B H 0.0758 0.8497 0.5025 0.227 Uiso 1 d R . .
H23C H 0.0629 0.9595 0.5978 0.227 Uiso 1 d R . .
C5 C 1.1103(8) 1.0349(10) 0.8980(5) 0.074(2) Uani 1 d . . .
C22 C 0.3843(14) 0.9633(10) 0.5957(8) 0.139(4) Uani 1 d . . .
H22A H 0.4951 0.9562 0.6322 0.208 Uiso 1 d R . .
H22B H 0.3532 1.0611 0.6126 0.208 Uiso 1 d R . .
H22C H 0.3749 0.9429 0.5240 0.208 Uiso 1 d R . .
C21 C 0.2718(10) 0.8485(8) 0.6249(6) 0.093(2) Uani 1 d . . .
H21 H 0.2879 0.8668 0.6988 0.111 Uiso 1 d R . .
C2 C 0.8772(10) 1.0693(11) 0.7294(6) 0.111(4) Uani 1 d . . .
C7 C 0.700(3) 0.520(2) 0.8534(18) 0.057(6) Uani 0.534(9) d P A 1
C8 C 0.6302(16) 0.399(3) 0.8182(14) 0.084(8) Uani 0.534(9) d P A 1
H8 H 0.5901 0.3767 0.7480 0.100 Uiso 0.534(9) calc PR A 1
C9 C 0.605(2) 0.287(2) 0.8792(17) 0.090(7) Uani 0.534(9) d P A 1
H9 H 0.5243 0.2100 0.8588 0.107 Uiso 0.534(9) calc PR A 1
C10 C 0.7286(17) 0.3141(14) 0.9791(9) 0.067(4) Uani 0.534(9) d P A 1
H10 H 0.7207 0.2513 1.0256 0.080 Uiso 0.534(9) calc PR A 1
C11 C 0.8544(16) 0.4253(12) 1.0085(8) 0.064(3) Uani 0.534(9) d P A 1
H11 H 0.9313 0.4311 1.0705 0.077 Uiso 0.534(9) calc PR A 1
C12 C 0.8644(14) 0.5267(12) 0.9452(7) 0.057(3) Uani 0.534(9) d P A 1
H12 H 0.9552 0.5920 0.9539 0.068 Uiso 0.534(9) calc PR A 1
C7A C 0.746(4) 0.490(4) 0.847(2) 0.065(9) Uani 0.466(9) d P A 2
C8A C 0.713(3) 0.374(2) 0.8158(12) 0.068(4) Uani 0.466(9) d P A 2
H8A H 0.7146 0.3472 0.7482 0.081 Uiso 0.466(9) calc PR A 2
C9A C 0.672(2) 0.263(2) 0.8629(15) 0.069(5) Uani 0.466(9) d P A 2
H9A H 0.7030 0.1698 0.8421 0.083 Uiso 0.466(9) calc PR A 2
C10A C 0.5938(17) 0.2708(14) 0.9337(11) 0.049(3) Uani 0.466(9) d P A 2
H10A H 0.5637 0.1887 0.9596 0.058 Uiso 0.466(9) calc PR A 2
C11A C 0.5603(16) 0.4102(12) 0.9663(9) 0.056(3) Uani 0.466(9) d P A 2
H11A H 0.5052 0.4242 1.0171 0.067 Uiso 0.466(9) calc PR A 2
C12A C 0.6048(15) 0.5320(13) 0.9270(8) 0.051(3) Uani 0.466(9) d P A 2
H12A H 0.5674 0.6248 0.9397 0.062 Uiso 0.466(9) calc PR A 2
H6 H 0.991(7) 0.835(6) 0.872(4) 0.050(16) Uiso 1 d . . .
H32A H 0.163(11) 0.308(10) 0.621(6) 0.12(3) Uiso 1 d . . .
H5 H 1.174(8) 1.012(7) 0.950(5) 0.08(2) Uiso 1 d . . .
H33B H 0.104(9) 0.516(8) 0.745(5) 0.08(2) Uiso 1 d . . .
H33C H 0.158(9) 0.678(9) 0.753(5) 0.09(2) Uiso 1 d . . .
H32B H 0.243(15) 0.360(13) 0.523(11) 0.19(5) Uiso 1 d . . .
H32C H 0.311(4) 0.362(4) 0.648(3) 0.000(9) Uiso 1 d . . .
H1 H 0.552(6) 0.605(6) 0.625(4) 0.029(17) Uiso 1 d . . .
H33A H 0.303(8) 0.569(7) 0.780(5) 0.071(19) Uiso 1 d . . .
H3 H 0.994(11) 1.283(10) 0.751(7) 0.12(3) Uiso 1 d . . .
H4 H 1.194(9) 1.239(8) 0.892(6) 0.10(2) Uiso 1 d . . .
H2 H 0.787(10) 1.081(9) 0.679(7) 0.11(3) Uiso 1 d . . .
H31 H 0.090(9) 0.547(7) 0.588(5) 0.08(2) Uiso 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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 '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
N1 P1 C21 107.8(3) . . ?
N1 P1 C31 106.5(3) . . ?
C21 P1 C31 109.4(4) . . ?
N1 P1 S1 111.2(2) . . ?
C21 P1 S1 110.2(3) . . ?
C31 P1 S1 111.7(2) . . ?
O2 P2 O1 98.8(2) . . ?
O2 P2 N1 104.1(3) . . ?
O1 P2 N1 101.7(2) . . ?
O2 P2 S2 116.2(2) . . ?
O1 P2 S2 116.0(2) . . ?
N1 P2 S2 117.5(2) . . ?
P2 N1 P1 136.5(4) . . ?
C7 O2 C7 20.2(11) . . ?
C7 O2 P2 115.2(10) . . ?
C7 O2 P2 134.8(10) . . ?
C1 O1 P2 124.7(3) . . ?
C32 C31 C33 114.9(8) . . ?
C32 C31 P1 110.0(5) . . ?
C33 C31 P1 114.0(5) . . ?
C1 C6 C5 118.0(7) . . ?
C5 C4 C3 119.2(7) . . ?
C4 C3 C2 120.5(8) . . ?
C6 C1 C2 120.9(6) . . ?
C6 C1 O1 122.2(6) . . ?
C2 C1 O1 116.8(5) . . ?
C4 C5 C6 121.8(7) . . ?
C23 C21 C22 111.2(7) . . ?
C23 C21 P1 109.3(7) . . ?
C22 C21 P1 110.9(7) . . ?
C1 C2 C3 119.6(7) . . ?
C8 C7 O2 123.2(19) . . ?
C8 C7 C12 116.9(15) . . ?
O2 C7 C12 98.2(16) . . ?
C7 C8 C9 124(2) . . ?
C8 C9 C10 110.2(17) . . ?
C11 C10 C9 125.2(11) . . ?
C12 C11 C10 119.5(11) . . ?
C11 C12 C7 112.5(13) . . ?
C8 C7 O2 129(2) . . ?
C8 C7 C12 104(2) . . ?
O2 C7 C12 108.3(15) . . ?
C7 C8 C9 128.2(19) . . ?
C10 C9 C8 127.7(19) . . ?
C9 C10 C11 114.1(14) . . ?
C10 C11 C12 122.7(12) . . ?
C11 C12 C7 112.5(14) . . ?
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
P1 N1 1.686(5) . ?
P1 C21 1.789(7) . ?
P1 C31 1.800(6) . ?
P1 S1 1.942(2) . ?
P2 O2 1.584(4) . ?
P2 O1 1.585(3) . ?
P2 N1 1.636(5) . ?
P2 S2 1.877(3) . ?
O2 C7 1.41(2) . ?
O2 C7 1.43(3) . ?
O1 C1 1.401(6) . ?
C31 C32 1.451(11) . ?
C31 C33 1.496(9) . ?
C6 C1 1.362(7) . ?
C6 C5 1.388(9) . ?
C4 C5 1.349(11) . ?
C4 C3 1.358(11) . ?
C3 C2 1.373(10) . ?
C1 C2 1.366(10) . ?
C23 C21 1.528(11) . ?
C22 C21 1.552(12) . ?
C7 C8 1.21(3) . ?
C7 C12 1.63(3) . ?
C8 C9 1.45(2) . ?
C9 C10 1.49(3) . ?
C10 C11 1.389(18) . ?
C11 C12 1.373(14) . ?
C7 C8 1.09(4) . ?
C7 C12 1.83(2) . ?
C8 C9 1.36(2) . ?
C9 C10 1.30(2) . ?
C10 C11 1.360(17) . ?
C11 C12 1.385(15) . ?
