#------------------------------------------------------------------------------
#$Date: 2019-11-28 15:07:15 +0200 (Thu, 28 Nov 2019) $
#$Revision: 244008 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/27/7702765.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_7702765
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            'C28 H28 Cl2 P2 Pd Se4 W'
_chemical_formula_weight         1103.43
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/m 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                 91.4810(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.0512(6)
_cell_length_b                   14.8092(9)
_cell_length_c                   10.8528(7)
_cell_measurement_temperature    293(2)
_cell_volume                     1614.90(17)
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Smart CCD'
_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  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7972
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    8.906
_exptl_crystal_colour            deep-red
_exptl_crystal_density_diffrn    2.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.892
_refine_diff_density_min         -2.370
_refine_diff_density_rms         0.248
_refine_ls_extinction_coef       0.0006(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2949
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1145P)²+3.1731P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1517
_refine_ls_wR_factor_ref         0.1549
_reflns_number_gt                2698
_reflns_number_total             2949
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b110583n.txt
_cod_data_source_block           W-Se-Pd-dppp_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      P2(1)/m
_cod_database_code               7702765
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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
C1 C 0.6192(7) 0.0390(5) 0.7043(6) 0.0328(15) Uani 1 1 d .
C2 C 0.7286(8) 0.0486(6) 0.6314(8) 0.0457(18) Uani 1 1 d .
H2 H 0.7421 0.1024 0.5893 0.055 Uiso 1 1 calc R
C3 C 0.8179(9) -0.0214(8) 0.6207(9) 0.058(2) Uani 1 1 d .
H3 H 0.8911 -0.0146 0.5709 0.070 Uiso 1 1 calc R
C4 C 0.8002(10) -0.1008(7) 0.6825(9) 0.062(3) Uani 1 1 d .
H4 H 0.8622 -0.1471 0.6765 0.075 Uiso 1 1 calc R
C5 C 0.6919(10) -0.1114(6) 0.7524(10) 0.061(3) Uani 1 1 d .
H5 H 0.6787 -0.1659 0.7928 0.074 Uiso 1 1 calc R
C6 C 0.5994(8) -0.0417(5) 0.7649(7) 0.0425(18) Uani 1 1 d .
H6 H 0.5254 -0.0496 0.8134 0.051 Uiso 1 1 calc R
C7 C 0.3510(7) 0.0888(5) 0.7755(7) 0.0338(15) Uani 1 1 d .
C8 C 0.2913(9) 0.1225(6) 0.8804(8) 0.048(2) Uani 1 1 d .
H8 H 0.3341 0.1667 0.9275 0.057 Uiso 1 1 calc R
C9 C 0.1690(9) 0.0905(7) 0.9147(10) 0.062(3) Uani 1 1 d .
H9 H 0.1296 0.1135 0.9847 0.075 Uiso 1 1 calc R
C10 C 0.1064(10) 0.0267(8) 0.8482(10) 0.066(3) Uani 1 1 d .
H10 H 0.0234 0.0065 0.8724 0.079 Uiso 1 1 calc R
C11 C 0.1626(9) -0.0107(7) 0.7424(9) 0.056(2) Uani 1 1 d .
H11 H 0.1195 -0.0559 0.6973 0.067 Uiso 1 1 calc R
C12 C 0.2835(8) 0.0223(6) 0.7088(8) 0.0469(19) Uani 1 1 d .
H12 H 0.3221 -0.0008 0.6384 0.056 Uiso 1 1 calc R
C13 C 0.4684(9) 0.1647(5) 0.5608(6) 0.0401(17) Uani 1 1 d .
H13A H 0.5513 0.1722 0.5181 0.048 Uiso 1 1 calc R
H13B H 0.4205 0.1150 0.5220 0.048 Uiso 1 1 calc R
C14 C 0.3864(12) 0.2500 0.5445(11) 0.041(2) Uani 1 2 d S
H14A H 0.3449 0.2500 0.4628 0.050 Uiso 1 2 calc SR
H14B H 0.3161 0.2500 0.6041 0.050 Uiso 1 2 calc SR
C15 C 0.981(3) 0.7500 0.354(3) 0.129(9) Uiso 1 2 d S
H15A H 0.9248 0.6972 0.3455 0.155 Uiso 0.50 1 calc PR
H15B H 0.9248 0.8028 0.3455 0.155 Uiso 0.50 1 calc PR
Cl1 Cl 1.0863(10) 0.7500 0.2432(10) 0.173(3) Uiso 1 2 d S
Cl2 Cl 1.0520(10) 0.7500 0.5028(10) 0.175(3) Uiso 1 2 d S
P1 P 0.50687(18) 0.13485(11) 0.72252(16) 0.0295(4) Uani 1 1 d .
Pd1 Pd 0.58682(8) 0.2500 0.84559(7) 0.0288(3) Uani 1 2 d S
Se1 Se 0.66407(9) 0.12328(5) 0.97816(7) 0.0448(3) Uani 1 1 d .
Se2 Se 0.63112(15) 0.2500 1.27901(12) 0.0599(4) Uani 1 2 d S
Se3 Se 0.95481(13) 0.2500 1.12581(14) 0.0589(4) Uani 1 2 d S
W1 W 0.73095(4) 0.2500 1.09428(3) 0.0336(2) Uani 1 2 d S
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'
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'
Cl Cl 0.1484 0.1585 '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
C2 C1 C6 119.3(7) . .
C2 C1 P1 119.1(6) . .
C6 C1 P1 121.6(6) . .
C3 C2 C1 120.1(8) . .
C2 C3 C4 120.8(9) . .
C5 C4 C3 119.5(8) . .
C4 C5 C6 121.0(9) . .
C1 C6 C5 119.2(8) . .
C8 C7 C12 117.7(7) . .
C8 C7 P1 121.2(6) . .
C12 C7 P1 121.0(6) . .
C9 C8 C7 120.3(9) . .
C10 C9 C8 120.5(10) . .
C9 C10 C11 121.7(9) . .
C12 C11 C10 117.1(9) . .
C11 C12 C7 122.6(8) . .
C14 C13 P1 114.3(6) . .
C13 C14 C13 112.8(10) 4_565 .
Cl1 C15 Cl2 115.4(16) . .
C7 P1 C1 106.5(3) . .
C7 P1 C13 103.3(4) . .
C1 P1 C13 101.5(3) . .
C7 P1 Pd1 112.7(2) . .
C1 P1 Pd1 115.5(2) . .
C13 P1 Pd1 115.9(2) . .
P1 Pd1 P1 95.80(9) . 4_565
P1 Pd1 Se1 177.74(6) . 4_565
P1 Pd1 Se1 82.82(5) 4_565 4_565
P1 Pd1 Se1 82.82(5) . .
P1 Pd1 Se1 177.74(6) 4_565 .
Se1 Pd1 Se1 98.49(4) 4_565 .
P1 Pd1 W1 132.03(4) . .
P1 Pd1 W1 132.03(4) 4_565 .
Se1 Pd1 W1 49.25(2) 4_565 .
Se1 Pd1 W1 49.25(2) . .
W1 Se1 Pd1 77.73(3) . .
Se2 W1 Se3 109.09(6) . .
Se2 W1 Se1 110.35(3) . .
Se3 W1 Se1 110.49(3) . .
Se2 W1 Se1 110.35(3) . 4_565
Se3 W1 Se1 110.49(3) . 4_565
Se1 W1 Se1 106.05(4) . 4_565
Se2 W1 Pd1 125.16(5) . .
Se3 W1 Pd1 125.75(4) . .
Se1 W1 Pd1 53.024(19) . .
Se1 W1 Pd1 53.023(19) 4_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.378(11) .
C1 C6 1.381(11) .
C1 P1 1.828(7) .
C2 C3 1.379(12) .
C3 C4 1.366(16) .
C4 C5 1.352(15) .
C5 C6 1.398(12) .
C7 C8 1.393(11) .
C7 C12 1.390(11) .
C7 P1 1.815(7) .
C8 C9 1.377(12) .
C9 C10 1.336(16) .
C10 C11 1.406(15) .
C11 C12 1.368(12) .
C13 C14 1.515(10) .
C13 P1 1.842(7) .
C14 C13 1.515(10) 4_565
C15 Cl1 1.62(3) .
C15 Cl2 1.74(3) .
P1 Pd1 2.2982(17) .
Pd1 P1 2.2982(17) 4_565
Pd1 Se1 2.4773(9) 4_565
Pd1 Se1 2.4773(9) .
Pd1 W1 3.0302(8) .
Se1 W1 2.3491(8) .
Se2 W1 2.2650(13) .
Se3 W1 2.2671(14) .
W1 Se1 2.3492(8) 4_565
