#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:25:15 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179789 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/85/7008509.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_7008509
loop_
_publ_author_name
'Gray, Ian P.'
'Slawin, Alexandra M. Z.'
'Woollins, J. Derek'
_publ_section_title
;
 Synthesis and structure of novel [Ph(RO)PSe2]- complexes.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2188
_journal_page_last               2194
_journal_paper_doi               10.1039/b503793j
_journal_year                    2005
_chemical_formula_sum            'C16 H20 O2 P2 Pb Se4'
_chemical_formula_weight         829.29
_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                110.741(14)
_cell_angle_beta                 97.96(2)
_cell_angle_gamma                100.16(2)
_cell_formula_units_Z            2
_cell_length_a                   6.4975(7)
_cell_length_b                   13.1066(13)
_cell_length_c                   14.502(2)
_cell_measurement_reflns_used    4081
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      25.3491
_cell_measurement_theta_min      2.7121
_cell_volume                     1109.4(3)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2004)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 0.83
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  ccd
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  'confocal optic'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_sigmaI/netI    0.1026
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6681
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.71
_diffrn_standards_decay_%        -
_diffrn_standards_interval_count -
_diffrn_standards_number         -
_exptl_absorpt_coefficient_mu    14.318
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3132
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.482
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.1000
_exptl_crystal_size_mid          0.1000
_exptl_crystal_size_min          0.0100
_refine_diff_density_max         1.938
_refine_diff_density_min         -1.234
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.602
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         3780
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.602
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1025
_reflns_number_gt                3124
_reflns_number_total             3780
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b503793j.txt
_cod_data_source_block           igdw44
_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:

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

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1109.4(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7008509
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.21605(4) 0.05464(2) 0.12720(2) 0.01558(13) Uani 1 1 d . . .
Se1 Se 0.62606(11) 0.20687(6) 0.25059(5) 0.01482(19) Uani 1 1 d . . .
Se2 Se 0.15056(11) 0.13336(7) 0.33463(6) 0.0181(2) Uani 1 1 d . . .
P1 P 0.4952(3) 0.19297(16) 0.37633(14) 0.0125(4) Uani 1 1 d . . .
C1 C 0.5817(12) 0.3242(6) 0.4853(5) 0.0162(17) Uani 1 1 d . . .
C2 C 0.4379(14) 0.3728(8) 0.5374(6) 0.030(2) Uani 1 1 d . . .
H2A H 0.2900 0.3358 0.5173 0.036 Uiso 1 1 calc R . .
C3 C 0.5100(17) 0.4763(8) 0.6196(7) 0.042(3) Uani 1 1 d . . .
H3A H 0.4106 0.5109 0.6539 0.050 Uiso 1 1 calc R . .
C4 C 0.7240(18) 0.5274(8) 0.6504(7) 0.045(3) Uani 1 1 d . . .
H4A H 0.7725 0.5967 0.7074 0.053 Uiso 1 1 calc R . .
C5 C 0.8703(17) 0.4804(9) 0.6005(7) 0.042(3) Uani 1 1 d . . .
H5A H 1.0181 0.5178 0.6220 0.050 Uiso 1 1 calc R . .
C6 C 0.8004(13) 0.3772(7) 0.5179(6) 0.027(2) Uani 1 1 d . . .
H6A H 0.9010 0.3431 0.4842 0.032 Uiso 1 1 calc R . .
O1 O 0.6089(7) 0.1173(4) 0.4213(4) 0.0145(11) Uani 1 1 d . . .
C7 C 0.5825(12) -0.0020(7) 0.3603(6) 0.0226(19) Uani 1 1 d . . .
H7A H 0.6265 -0.0109 0.2957 0.027 Uiso 1 1 calc R . .
H7B H 0.4303 -0.0426 0.3448 0.027 Uiso 1 1 calc R . .
C8 C 0.7175(12) -0.0491(7) 0.4180(6) 0.0222(18) Uani 1 1 d . . .
H8A H 0.7021 -0.1290 0.3777 0.033 Uiso 1 1 calc R . .
H8B H 0.6717 -0.0410 0.4813 0.033 Uiso 1 1 calc R . .
H8C H 0.8678 -0.0085 0.4332 0.033 Uiso 1 1 calc R . .
Se11 Se 0.01866(11) 0.22114(7) 0.09608(6) 0.0175(2) Uani 1 1 d . . .
Se12 Se 0.30871(11) 0.07672(6) -0.07849(6) 0.0171(2) Uani 1 1 d . . .
P11 P 0.1881(3) 0.22458(17) -0.02257(15) 0.0154(4) Uani 1 1 d . . .
C11 C 0.0163(13) 0.2423(8) -0.1208(6) 0.025(2) Uani 1 1 d . . .
C12 C 0.0501(19) 0.2116(10) -0.2159(7) 0.050(3) Uani 1 1 d . B .
H12A H 0.1593 0.1732 -0.2326 0.061 Uiso 1 1 calc R . .
C13 C -0.0711(18) 0.2348(9) -0.2897(8) 0.046(3) Uani 1 1 d . . .
H13A H -0.0388 0.2145 -0.3548 0.055 Uiso 1 1 calc R A 1
C14 C -0.2277(15) 0.2837(10) -0.2718(8) 0.049(3) Uani 1 1 d . B 1
H14A H -0.2791 0.3222 -0.3111 0.059 Uiso 1 1 calc R B 1
C15A C -0.309(3) 0.2763(16) -0.1966(14) 0.030(4) Uiso 0.50 1 d P B 1
H15A H -0.4496 0.2864 -0.1934 0.036 Uiso 0.50 1 calc PR B 1
C16A C -0.189(2) 0.2530(13) -0.1180(11) 0.016(3) Uiso 0.50 1 d P B 1
H16A H -0.2516 0.2451 -0.0648 0.019 Uiso 0.50 1 calc PR B 1
C15B C -0.226(3) 0.3560(18) -0.1585(15) 0.038(5) Uiso 0.50 1 d P B 2
C16B C -0.100(3) 0.3320(15) -0.0891(13) 0.028(4) Uiso 0.50 1 d P B 2
O11 O 0.3664(8) 0.3391(5) 0.0142(4) 0.0249(13) Uani 1 1 d . . .
C17 C 0.5451(12) 0.3689(7) 0.0982(7) 0.0250(19) Uani 1 1 d . B .
H17A H 0.6314 0.3123 0.0822 0.030 Uiso 1 1 calc R . .
H17B H 0.4914 0.3702 0.1591 0.030 Uiso 1 1 calc R . .
C18 C 0.680(2) 0.4814(10) 0.1179(9) 0.069(4) Uani 1 1 d . . .
H18A H 0.8007 0.5019 0.1749 0.103 Uiso 1 1 calc R B .
H18B H 0.5939 0.5372 0.1342 0.103 Uiso 1 1 calc R . .
H18C H 0.7341 0.4795 0.0577 0.103 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'
O O 0.0106 0.0060 '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'
Pb Pb -3.3944 10.1111 '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
Se11 Pb1 Se1 97.05(3) . . ?
Se11 Pb1 Se2 88.73(3) . . ?
Se1 Pb1 Se2 75.22(3) . . ?
Se11 Pb1 Se12 71.63(3) . . ?
Se1 Pb1 Se12 93.82(3) . . ?
Se2 Pb1 Se12 156.37(2) . . ?
P1 Se1 Pb1 84.42(5) . . ?
P1 Se2 Pb1 84.32(6) . . ?
O1 P1 C1 98.8(3) . . ?
O1 P1 Se2 112.8(2) . . ?
C1 P1 Se2 112.0(2) . . ?
O1 P1 Se1 110.2(2) . . ?
C1 P1 Se1 111.0(3) . . ?
Se2 P1 Se1 111.50(9) . . ?
C2 C1 C6 119.5(7) . . ?
C2 C1 P1 121.7(6) . . ?
C6 C1 P1 118.8(6) . . ?
C1 C2 C3 120.1(8) . . ?
C1 C2 H2A 119.9 . . ?
C3 C2 H2A 119.9 . . ?
C4 C3 C2 119.7(9) . . ?
C4 C3 H3A 120.1 . . ?
C2 C3 H3A 120.1 . . ?
C3 C4 C5 121.2(9) . . ?
C3 C4 H4A 119.4 . . ?
C5 C4 H4A 119.4 . . ?
C4 C5 C6 119.6(9) . . ?
C4 C5 H5A 120.2 . . ?
C6 C5 H5A 120.2 . . ?
C5 C6 C1 119.7(8) . . ?
C5 C6 H6A 120.2 . . ?
C1 C6 H6A 120.2 . . ?
C7 O1 P1 120.3(5) . . ?
O1 C7 C8 108.6(6) . . ?
O1 C7 H7A 110.0 . . ?
C8 C7 H7A 110.0 . . ?
O1 C7 H7B 110.0 . . ?
C8 C7 H7B 110.0 . . ?
H7A C7 H7B 108.3 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
P11 Se11 Pb1 91.38(6) . . ?
P11 Se12 Pb1 82.35(6) . . ?
O11 P11 C11 98.7(4) . . ?
O11 P11 Se12 113.7(2) . . ?
C11 P11 Se12 112.3(3) . . ?
O11 P11 Se11 110.8(2) . . ?
C11 P11 Se11 109.7(3) . . ?
Se12 P11 Se11 111.08(10) . . ?
C12 C11 C16A 111.8(10) . . ?
C12 C11 C16B 116.4(10) . . ?
C16A C11 C16B 40.8(9) . . ?
C12 C11 P11 121.8(7) . . ?
C16A C11 P11 123.5(9) . . ?
C16B C11 P11 116.9(9) . . ?
C11 C12 C13 121.7(9) . . ?
C11 C12 H12A 119.2 . . ?
C13 C12 H12A 119.2 . . ?
C14 C13 C12 121.7(10) . . ?
C14 C13 H13A 119.2 . . ?
C12 C13 H13A 119.2 . . ?
C15A C14 C13 115.7(13) . . ?
C15A C14 H14A 122.1 . . ?
C13 C14 H14A 122.1 . . ?
C14 C15A C16A 120.9(15) . . ?
C14 C15A H15A 119.6 . . ?
C16A C15A H15A 119.6 . . ?
C11 C16A C15A 119.6(14) . . ?
C11 C16A H16A 120.2 . . ?
C15A C16A H16A 120.2 . . ?
C15B C16B C11 121.4(15) . . ?
C17 O11 P11 121.1(6) . . ?
O11 C17 C18 109.3(8) . . ?
O11 C17 H17A 109.8 . . ?
C18 C17 H17A 109.8 . . ?
O11 C17 H17B 109.8 . . ?
C18 C17 H17B 109.8 . . ?
H17A C17 H17B 108.3 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
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
Pb1 Se11 2.8522(9) . ?
Pb1 Se1 2.9249(12) . ?
Pb1 Se2 2.9335(9) . ?
Pb1 Se12 3.2235(10) . ?
Se1 P1 2.166(2) . ?
Se2 P1 2.160(2) . ?
P1 O1 1.593(5) . ?
P1 C1 1.805(7) . ?
C1 C2 1.383(11) . ?
C1 C6 1.399(11) . ?
C2 C3 1.399(12) . ?
C2 H2A 0.9500 . ?
C3 C4 1.367(14) . ?
C3 H3A 0.9500 . ?
C4 C5 1.374(14) . ?
C4 H4A 0.9500 . ?
C5 C6 1.399(12) . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9500 . ?
O1 C7 1.463(9) . ?
C7 C8 1.486(12) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
Se11 P11 2.176(2) . ?
Se12 P11 2.151(2) . ?
P11 O11 1.591(6) . ?
P11 C11 1.793(9) . ?
C11 C12 1.354(13) . ?
C11 C16A 1.369(16) . ?
C11 C16B 1.479(18) . ?
C12 C13 1.394(14) . ?
C12 H12A 0.9500 . ?
C13 C14 1.303(14) . ?
C13 H13A 0.9500 . ?
C14 C15A 1.30(2) . ?
C14 H14A 0.9500 . ?
C15A C16A 1.45(2) . ?
C15A H15A 0.9500 . ?
C16A H16A 0.9500 . ?
C15B C16B 1.37(3) . ?
O11 C17 1.448(10) . ?
C17 C18 1.483(13) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
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_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Se11 Pb1 Se1 P1 100.24(6) . . . . ?
Se2 Pb1 Se1 P1 13.43(6) . . . . ?
Se12 Pb1 Se1 P1 172.18(6) . . . . ?
Se11 Pb1 Se2 P1 -111.11(6) . . . . ?
Se1 Pb1 Se2 P1 -13.48(6) . . . . ?
Se12 Pb1 Se2 P1 -77.95(8) . . . . ?
Pb1 Se2 P1 O1 -105.5(2) . . . . ?
Pb1 Se2 P1 C1 144.1(3) . . . . ?
Pb1 Se2 P1 Se1 19.09(8) . . . . ?
Pb1 Se1 P1 O1 106.9(2) . . . . ?
Pb1 Se1 P1 C1 -144.7(3) . . . . ?
Pb1 Se1 P1 Se2 -19.14(8) . . . . ?
O1 P1 C1 C2 -114.6(7) . . . . ?
Se2 P1 C1 C2 4.4(8) . . . . ?
Se1 P1 C1 C2 129.7(7) . . . . ?
O1 P1 C1 C6 64.8(7) . . . . ?
Se2 P1 C1 C6 -176.2(6) . . . . ?
Se1 P1 C1 C6 -50.9(7) . . . . ?
C6 C1 C2 C3 2.6(14) . . . . ?
P1 C1 C2 C3 -178.1(8) . . . . ?
C1 C2 C3 C4 -2.2(15) . . . . ?
C2 C3 C4 C5 1.6(16) . . . . ?
C3 C4 C5 C6 -1.4(16) . . . . ?
C4 C5 C6 C1 1.7(15) . . . . ?
C2 C1 C6 C5 -2.3(13) . . . . ?
P1 C1 C6 C5 178.3(7) . . . . ?
C1 P1 O1 C7 178.7(5) . . . . ?
Se2 P1 O1 C7 60.2(5) . . . . ?
Se1 P1 O1 C7 -65.0(5) . . . . ?
P1 O1 C7 C8 176.0(5) . . . . ?
Se1 Pb1 Se11 P11 79.94(6) . . . . ?
Se2 Pb1 Se11 P11 154.88(6) . . . . ?
Se12 Pb1 Se11 P11 -11.76(5) . . . . ?
Se11 Pb1 Se12 P11 12.00(5) . . . . ?
Se1 Pb1 Se12 P11 -84.17(6) . . . . ?
Se2 Pb1 Se12 P11 -23.18(8) . . . . ?
Pb1 Se12 P11 O11 109.7(3) . . . . ?
Pb1 Se12 P11 C11 -139.3(3) . . . . ?
Pb1 Se12 P11 Se11 -16.09(7) . . . . ?
Pb1 Se11 P11 O11 -109.3(3) . . . . ?
Pb1 Se11 P11 C11 142.9(3) . . . . ?
Pb1 Se11 P11 Se12 18.09(8) . . . . ?
O11 P11 C11 C12 86.0(9) . . . . ?
Se12 P11 C11 C12 -34.1(10) . . . . ?
Se11 P11 C11 C12 -158.1(9) . . . . ?
O11 P11 C11 C16A -115.2(10) . . . . ?
Se12 P11 C11 C16A 124.7(10) . . . . ?
Se11 P11 C11 C16A 0.6(11) . . . . ?
O11 P11 C11 C16B -68.1(10) . . . . ?
Se12 P11 C11 C16B 171.7(9) . . . . ?
Se11 P11 C11 C16B 47.7(10) . . . . ?
C16A C11 C12 C13 25.0(17) . . . . ?
C16B C11 C12 C13 -19.7(18) . . . . ?
P11 C11 C12 C13 -174.0(9) . . . . ?
C11 C12 C13 C14 -2.5(19) . . . . ?
C12 C13 C14 C15A -21.6(19) . . . . ?
C13 C14 C15A C16A 21(2) . . . . ?
C12 C11 C16A C15A -24.5(18) . . . . ?
C16B C11 C16A C15A 81.2(19) . . . . ?
P11 C11 C16A C15A 174.9(11) . . . . ?
C14 C15A C16A C11 2(2) . . . . ?
C12 C11 C16B C15B 21(2) . . . . ?
C16A C11 C16B C15B -72.3(19) . . . . ?
P11 C11 C16B C15B 176.7(14) . . . . ?
C11 P11 O11 C17 177.7(6) . . . . ?
Se12 P11 O11 C17 -63.2(6) . . . . ?
Se11 P11 O11 C17 62.7(6) . . . . ?
P11 O11 C17 C18 -177.8(7) . . . . ?
