#------------------------------------------------------------------------------
#$Date: 2019-11-28 14:07:15 +0100 (jue 28 de nov de 2019) $
#$Revision: 244008 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/27/7702763.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_7702763
loop_
_publ_author_name
'Zhang, Qian-Feng'
'Song, Yinling'
'Wong, Wai-Yeung'
'Leung, Wa-Hung'
'Xin, Xinquan'
_publ_section_title
;
 Syntheses, molecular structures and optical nonlinearities of
 heteroselenometallic W--Se--Pd compounds containing bidentate phosphine
 ligands
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1963
_journal_paper_doi               10.1039/b110583n
_journal_year                    2002
_chemical_formula_sum            'C56 H58 N2 O2 P4 Pd4 Se8 W2'
_chemical_formula_weight         2340.04
_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_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
_cell_angle_alpha                90.00
_cell_angle_beta                 98.7260(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.55250(10)
_cell_length_b                   15.1794(2)
_cell_length_c                   21.2565(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.44
_cell_measurement_theta_min      1.66
_cell_volume                     3365.47(6)
_computing_cell_refinement       'SAINT (Siemens, 1996b)'
_computing_data_collection       'SMART (Siemens, 1996a)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and PARST (Nardelli, 1995)'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type
;
Siemens SMART CCD area detector diffractometer
;
_diffrn_measurement_method       'ω scan'
_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  0.0933
_diffrn_reflns_av_sigmaI/netI    0.1231
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22144
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    8.911
_exptl_absorpt_correction_T_max  0.524
_exptl_absorpt_correction_T_min  0.242
_exptl_absorpt_correction_type   'empirical using SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.392
_refine_diff_density_min         -1.738
_refine_diff_density_rms         0.294
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         8263
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.1252
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0421P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1261
_reflns_number_gt                4569
_reflns_number_total             8263
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b110583n.txt
_cod_data_source_block           W-Pd-Se-dppm_cluster
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21 /c'
_cod_database_code               7702763
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
W1 W 0.03577(4) 0.78875(3) 0.054942(18) 0.03206(12) Uani 1 1 d .
Pd1 Pd -0.01995(7) 0.96108(5) 0.10744(3) 0.03023(18) Uani 1 1 d .
Pd2 Pd 0.11341(7) 0.89448(5) -0.04922(3) 0.03181(19) Uani 1 1 d .
Se1 Se -0.08532(9) 0.90664(7) -0.00202(4) 0.0332(2) Uani 1 1 d .
Se2 Se 0.09653(11) 0.83218(7) 0.16073(5) 0.0409(3) Uani 1 1 d .
Se3 Se 0.21922(11) 0.76556(7) 0.00742(5) 0.0433(3) Uani 1 1 d .
Se4 Se -0.08522(15) 0.66461(9) 0.05033(7) 0.0716(4) Uani 1 1 d .
P1 P 0.2485(3) 0.89754(19) -0.12285(12) 0.0378(6) Uani 1 1 d .
P2 P -0.0116(3) 1.03479(17) 0.20157(11) 0.0329(6) Uani 1 1 d .
C1 C 0.3514(10) 0.9921(7) -0.1294(5) 0.042(3) Uani 1 1 d .
C2 C 0.3767(11) 1.0548(9) -0.0806(6) 0.061(3) Uani 1 1 d .
H2A H 0.3334 1.0513 -0.0457 0.073 Uiso 1 1 calc R
C3 C 0.4633(14) 1.1208(11) -0.0834(8) 0.091(5) Uani 1 1 d .
H3A H 0.4795 1.1614 -0.0503 0.109 Uiso 1 1 calc R
C4 C 0.5265(13) 1.1272(10) -0.1348(8) 0.077(4) Uani 1 1 d .
H4A H 0.5862 1.1718 -0.1367 0.092 Uiso 1 1 calc R
C5 C 0.5014(12) 1.0682(9) -0.1827(6) 0.065(4) Uani 1 1 d .
H5A H 0.5433 1.0729 -0.2181 0.078 Uiso 1 1 calc R
C6 C 0.4154(11) 1.0021(9) -0.1798(5) 0.059(3) Uani 1 1 d .
H6A H 0.3998 0.9625 -0.2135 0.071 Uiso 1 1 calc R
C7 C 0.3629(13) 0.8067(8) -0.1219(5) 0.055(3) Uani 1 1 d .
C8 C 0.4804(13) 0.8134(10) -0.0845(8) 0.083(5) Uani 1 1 d .
H8A H 0.5017 0.8644 -0.0611 0.100 Uiso 1 1 calc R
C9 C 0.5697(17) 0.7431(15) -0.0813(11) 0.117(7) Uani 1 1 d .
H9A H 0.6509 0.7490 -0.0576 0.141 Uiso 1 1 calc R
C10 C 0.536(2) 0.6680(16) -0.1127(11) 0.129(10) Uani 1 1 d .
H10A H 0.5929 0.6210 -0.1086 0.155 Uiso 1 1 calc R
C11 C 0.421(2) 0.6586(12) -0.1503(8) 0.122(8) Uani 1 1 d .
H11A H 0.4018 0.6073 -0.1736 0.146 Uiso 1 1 calc R
C12 C 0.3297(17) 0.7293(10) -0.1535(6) 0.089(5) Uani 1 1 d .
H12A H 0.2483 0.7226 -0.1769 0.107 Uiso 1 1 calc R
C13 C -0.0258(10) 0.9640(6) 0.2704(4) 0.035(2) Uani 1 1 d .
C14 C 0.0720(16) 0.9579(10) 0.3206(6) 0.093(5) Uani 1 1 d .
H14A H 0.1477 0.9895 0.3212 0.111 Uiso 1 1 calc R
C15 C 0.052(2) 0.9006(12) 0.3723(7) 0.147(10) Uani 1 1 d .
H15A H 0.1128 0.8991 0.4090 0.176 Uiso 1 1 calc R
C16 C -0.057(2) 0.8475(9) 0.3677(7) 0.096(6) Uani 1 1 d .
H16A H -0.0666 0.8062 0.3990 0.116 Uiso 1 1 calc R
C17 C -0.1430(15) 0.8578(9) 0.3186(7) 0.076(4) Uani 1 1 d .
H17A H -0.2189 0.8263 0.3175 0.091 Uiso 1 1 calc R
C18 C -0.1328(12) 0.9094(9) 0.2692(6) 0.068(4) Uani 1 1 d .
H18A H -0.1968 0.9094 0.2339 0.081 Uiso 1 1 calc R
C19 C 0.1321(10) 1.0988(7) 0.2265(5) 0.039(2) Uani 1 1 d .
C20 C 0.2344(12) 1.0930(8) 0.1962(6) 0.059(3) Uani 1 1 d .
H20A H 0.2301 1.0570 0.1605 0.071 Uiso 1 1 calc R
C21 C 0.3477(13) 1.1400(10) 0.2167(7) 0.078(4) Uani 1 1 d .
H21A H 0.4187 1.1344 0.1959 0.094 Uiso 1 1 calc R
C22 C 0.3510(15) 1.1951(10) 0.2692(7) 0.082(5) Uani 1 1 d .
H22A H 0.4259 1.2258 0.2839 0.098 Uiso 1 1 calc R
C23 C 0.2459(14) 1.2055(10) 0.2999(7) 0.082(5) Uani 1 1 d .
H23A H 0.2476 1.2435 0.3343 0.099 Uiso 1 1 calc R
C24 C 0.1372(12) 1.1564(8) 0.2771(5) 0.056(3) Uani 1 1 d .
H24A H 0.0648 1.1627 0.2968 0.067 Uiso 1 1 calc R
C25 C -0.1480(9) 1.1127(6) 0.2008(5) 0.037(2) Uani 1 1 d .
H25A H -0.1971 1.0982 0.2344 0.044 Uiso 1 1 calc R
H25B H -0.1166 1.1726 0.2073 0.044 Uiso 1 1 calc R
N1 N 0.3361(13) 0.5642(8) 0.0846(6) 0.076(3) Uani 1 1 d .
O1 O 0.3337(11) 0.6177(9) 0.1828(5) 0.115(4) Uani 1 1 d .
C26 C 0.4680(18) 0.5901(13) 0.0844(11) 0.139(8) Uani 1 1 d .
H26A H 0.4946 0.5720 0.0452 0.208 Uiso 1 1 calc R
H26B H 0.5217 0.5624 0.1194 0.208 Uiso 1 1 calc R
H26C H 0.4753 0.6529 0.0885 0.208 Uiso 1 1 calc R
C27 C 0.269(2) 0.5244(10) 0.0274(9) 0.144(9) Uani 1 1 d .
H27A H 0.3264 0.5166 -0.0029 0.217 Uiso 1 1 calc R
H27B H 0.1992 0.5620 0.0096 0.217 Uiso 1 1 calc R
H27C H 0.2351 0.4682 0.0375 0.217 Uiso 1 1 calc R
C28 C 0.2822(17) 0.5839(11) 0.1360(9) 0.088(5) Uani 1 1 d .
H28B H 0.1961 0.5695 0.1346 0.105 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'
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'
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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
Se4 W1 Se2 110.25(5) . .
Se4 W1 Se3 110.66(5) . .
Se2 W1 Se3 109.47(4) . .
Se4 W1 Se1 110.01(5) . .
Se2 W1 Se1 108.68(4) . .
Se3 W1 Se1 107.71(4) . .
Se4 W1 Pd1 127.72(5) . .
Se2 W1 Pd1 54.91(3) . .
Se3 W1 Pd1 121.58(3) . .
Se1 W1 Pd1 53.81(3) . .
Se4 W1 Pd2 129.62(4) . .
Se2 W1 Pd2 120.12(3) . .
Se3 W1 Pd2 54.28(3) . .
Se1 W1 Pd2 53.60(3) . .
Pd1 W1 Pd2 83.97(2) . .
P2 Pd1 Se1 163.56(8) . .
P2 Pd1 Se2 92.04(7) . .
Se1 Pd1 Se2 102.35(4) . .
P2 Pd1 Pd2 88.03(7) . 3_575
Se1 Pd1 Pd2 78.73(3) . 3_575
Se2 Pd1 Pd2 172.49(5) . 3_575
P2 Pd1 W1 141.82(7) . .
Se1 Pd1 W1 52.19(3) . .
Se2 Pd1 W1 50.19(3) . .
Pd2 Pd1 W1 130.15(3) 3_575 .
P1 Pd2 Se1 160.11(8) . .
P1 Pd2 Se3 93.87(8) . .
Se1 Pd2 Se3 102.13(4) . .
P1 Pd2 Pd1 83.61(7) . 3_575
Se1 Pd2 Pd1 81.25(4) . 3_575
Se3 Pd2 Pd1 175.03(5) . 3_575
P1 Pd2 W1 143.43(7) . .
Se1 Pd2 W1 52.04(3) . .
Se3 Pd2 W1 50.24(3) . .
Pd1 Pd2 W1 132.74(3) 3_575 .
W1 Se1 Pd2 74.36(3) . .
W1 Se1 Pd1 74.00(3) . .
Pd2 Se1 Pd1 106.00(4) . .
W1 Se2 Pd1 74.91(3) . .
W1 Se3 Pd2 75.49(4) . .
C1 P1 C7 101.2(5) . .
C1 P1 C25 105.6(5) . 3_575
C7 P1 C25 103.7(5) . 3_575
C1 P1 Pd2 120.9(4) . .
C7 P1 Pd2 117.3(3) . .
C25 P1 Pd2 106.5(3) 3_575 .
C19 P2 C13 104.3(5) . .
C19 P2 C25 105.9(5) . .
C13 P2 C25 102.9(5) . .
C19 P2 Pd1 116.0(3) . .
C13 P2 Pd1 114.4(3) . .
C25 P2 Pd1 112.1(3) . .
C6 C1 C2 116.5(11) . .
C6 C1 P1 121.5(10) . .
C2 C1 P1 121.9(8) . .
C3 C2 C1 121.3(12) . .
C2 C3 C4 119.9(15) . .
C5 C4 C3 119.5(14) . .
C4 C5 C6 120.6(12) . .
C1 C6 C5 122.2(13) . .
C8 C7 C12 119.3(12) . .
C8 C7 P1 119.2(11) . .
C12 C7 P1 121.4(11) . .
C7 C8 C9 120.6(17) . .
C10 C9 C8 119(2) . .
C9 C10 C11 122.1(19) . .
C10 C11 C12 118.9(18) . .
C7 C12 C11 119.7(16) . .
C14 C13 C18 119.0(11) . .
C14 C13 P2 121.1(10) . .
C18 C13 P2 119.7(8) . .
C13 C14 C15 117.2(15) . .
C16 C15 C14 120.5(13) . .
C17 C16 C15 117.4(13) . .
C16 C17 C18 125.5(15) . .
C17 C18 C13 119.9(12) . .
C20 C19 C24 118.4(11) . .
C20 C19 P2 121.5(8) . .
C24 C19 P2 120.0(9) . .
C19 C20 C21 121.8(12) . .
C22 C21 C20 118.2(13) . .
C23 C22 C21 121.6(13) . .
C22 C23 C24 117.0(13) . .
C19 C24 C23 122.9(12) . .
P1 C25 P2 107.2(5) 3_575 .
C28 N1 C27 124.2(17) . .
C28 N1 C26 118.0(15) . .
C27 N1 C26 117.6(16) . .
O1 C28 N1 126.0(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 Se4 2.2699(14) .
W1 Se2 2.3376(10) .
W1 Se3 2.3420(12) .
W1 Se1 2.4149(10) .
W1 Pd1 2.9382(8) .
W1 Pd2 2.9496(8) .
Pd1 P2 2.283(3) .
Pd1 Se1 2.4668(11) .
Pd1 Se2 2.4899(12) .
Pd1 Pd2 2.6346(10) 3_575
Pd2 P1 2.272(3) .
Pd2 Se1 2.4652(12) .
Pd2 Se3 2.4735(12) .
Pd2 Pd1 2.6346(10) 3_575
P1 C1 1.818(11) .
P1 C7 1.831(12) .
P1 C25 1.832(10) 3_575
P2 C19 1.811(11) .
P2 C13 1.840(9) .
P2 C25 1.861(9) .
C1 C6 1.359(14) .
C1 C2 1.403(15) .
C2 C3 1.364(17) .
C3 C4 1.367(19) .
C4 C5 1.353(18) .
C5 C6 1.361(16) .
C7 C8 1.371(17) .
C7 C12 1.372(18) .
C8 C9 1.42(2) .
C9 C10 1.34(3) .
C10 C11 1.35(3) .
C11 C12 1.44(2) .
C13 C14 1.370(15) .
C13 C18 1.398(15) .
C14 C15 1.44(2) .
C15 C16 1.40(2) .
C16 C17 1.287(19) .
C17 C18 1.327(16) .
C19 C20 1.342(15) .
C19 C24 1.380(14) .
C20 C21 1.404(16) .
C21 C22 1.390(18) .
C22 C23 1.38(2) .
C23 C24 1.391(16) .
C25 P1 1.832(10) 3_575
N1 C28 1.340(19) .
N1 C27 1.446(18) .
N1 C26 1.45(2) .
O1 C28 1.176(18) .
