#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/09/7050912.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_7050912
loop_
_publ_author_name
'Durran, Sean E.'
'Elsegood, Mark R. J.'
'Smith, Martin B.'
_publ_section_title
;
 New complexes of functionalised ligands bearing P/N/Se or P2Se donor
 sets
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1402
_journal_paper_doi               10.1039/b204005k
_journal_volume                  26
_journal_year                    2002
_chemical_formula_sum            'C36 H36 Cl5 N P2 Pd Se'
_chemical_formula_weight         907.21
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_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                 102.898(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.6694(10)
_cell_length_b                   11.6913(8)
_cell_length_c                   22.9159(16)
_cell_measurement_reflns_used    7241
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.17
_cell_measurement_theta_min      2.25
_cell_volume                     3831.0(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0538
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            29211
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.894
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_correction_T_min  0.752
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.800
_refine_diff_density_min         -1.245
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         7530
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0508P)²+34.5612P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1554
_reflns_number_gt                5274
_reflns_number_total             7530
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b204005k.txt
_cod_data_source_block           3c.CHCl3
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7050912
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.36628(3) -0.00250(4) 0.20937(2) 0.01642(13) Uani 1 1 d . . .
Cl1 Cl 0.34827(12) -0.11115(14) 0.12083(7) 0.0266(4) Uani 1 1 d . . .
Cl2 Cl 0.36180(12) -0.17221(14) 0.26520(7) 0.0238(4) Uani 1 1 d . . .
P1 P 0.34319(11) 0.15720(14) 0.15354(7) 0.0166(3) Uani 1 1 d . . .
P2 P 0.38855(11) 0.09733(14) 0.29486(7) 0.0167(3) Uani 1 1 d . . .
C1 C 0.3859(5) 0.2927(5) 0.1892(3) 0.0179(13) Uani 1 1 d . . .
H1A H 0.4550 0.2937 0.1970 0.021 Uiso 1 1 calc R . .
H1B H 0.3622 0.3562 0.1614 0.021 Uiso 1 1 calc R . .
C2 C 0.4191(5) 0.2499(5) 0.2938(3) 0.0203(14) Uani 1 1 d . . .
H2A H 0.4163 0.2848 0.3327 0.024 Uiso 1 1 calc R . .
H2B H 0.4840 0.2572 0.2885 0.024 Uiso 1 1 calc R . .
N1 N 0.3565(4) 0.3114(4) 0.2461(2) 0.0174(11) Uani 1 1 d . . .
C3 C 0.3560(5) 0.4351(5) 0.2593(3) 0.0226(14) Uani 1 1 d . . .
H3A H 0.3219 0.4758 0.2231 0.027 Uiso 1 1 calc R . .
H3B H 0.4212 0.4635 0.2687 0.027 Uiso 1 1 calc R . .
C4 C 0.3104(5) 0.4633(6) 0.3116(3) 0.0247(15) Uani 1 1 d . . .
H4A H 0.3482 0.4286 0.3486 0.030 Uiso 1 1 calc R . .
H4B H 0.3113 0.5472 0.3173 0.030 Uiso 1 1 calc R . .
C5 C 0.2104(5) 0.4211(7) 0.3026(3) 0.0326(17) Uani 1 1 d . . .
H5A H 0.2079 0.3397 0.2906 0.039 Uiso 1 1 calc R . .
H5B H 0.1705 0.4648 0.2696 0.039 Uiso 1 1 calc R . .
Se1 Se 0.15909(6) 0.43626(7) 0.37457(4) 0.0382(2) Uani 1 1 d . . .
C6 C 0.1893(5) 0.5921(6) 0.3961(3) 0.0288(16) Uani 1 1 d . . .
C7 C 0.2185(5) 0.6170(6) 0.4562(3) 0.0297(16) Uani 1 1 d . . .
H7 H 0.2259 0.5572 0.4850 0.036 Uiso 1 1 calc R . .
C8 C 0.2373(5) 0.7299(7) 0.4748(3) 0.0325(17) Uani 1 1 d . . .
H8 H 0.2550 0.7471 0.5163 0.039 Uiso 1 1 calc R . .
C9 C 0.2301(5) 0.8165(6) 0.4332(4) 0.0339(18) Uani 1 1 d . . .
H9 H 0.2438 0.8931 0.4461 0.041 Uiso 1 1 calc R . .
C10 C 0.2029(6) 0.7915(6) 0.3724(4) 0.0377(19) Uani 1 1 d . . .
H10 H 0.1996 0.8507 0.3436 0.045 Uiso 1 1 calc R . .
C11 C 0.1804(6) 0.6797(6) 0.3540(3) 0.0330(17) Uani 1 1 d . . .
H11 H 0.1590 0.6630 0.3126 0.040 Uiso 1 1 calc R . .
C12 C 0.2189(4) 0.1785(6) 0.1245(3) 0.0218(14) Uani 1 1 d . . .
C13 C 0.1613(5) 0.0878(7) 0.1022(4) 0.042(2) Uani 1 1 d . . .
H13 H 0.1874 0.0137 0.1012 0.051 Uiso 1 1 calc R . .
C14 C 0.0665(6) 0.1031(8) 0.0813(5) 0.053(3) Uani 1 1 d . . .
H14 H 0.0282 0.0395 0.0660 0.063 Uiso 1 1 calc R . .
C15 C 0.0272(6) 0.2072(9) 0.0825(5) 0.063(3) Uani 1 1 d . . .
H15 H -0.0378 0.2181 0.0663 0.076 Uiso 1 1 calc R . .
C16 C 0.0823(7) 0.2966(10) 0.1072(8) 0.112(6) Uani 1 1 d . . .
H16 H 0.0548 0.3690 0.1109 0.134 Uiso 1 1 calc R . .
C17 C 0.1773(7) 0.2830(9) 0.1269(6) 0.080(4) Uani 1 1 d . . .
H17 H 0.2147 0.3471 0.1426 0.096 Uiso 1 1 calc R . .
C18 C 0.4000(4) 0.1533(5) 0.0916(3) 0.0189(13) Uani 1 1 d . . .
C19 C 0.3512(5) 0.1522(6) 0.0321(3) 0.0253(15) Uani 1 1 d . . .
H19 H 0.2848 0.1554 0.0225 0.030 Uiso 1 1 calc R . .
C20 C 0.4004(6) 0.1462(6) -0.0132(3) 0.0333(18) Uani 1 1 d . . .
H20 H 0.3672 0.1447 -0.0539 0.040 Uiso 1 1 calc R . .
C21 C 0.4961(6) 0.1426(6) 0.0000(4) 0.0349(18) Uani 1 1 d . . .
H21 H 0.5288 0.1398 -0.0314 0.042 Uiso 1 1 calc R . .
C22 C 0.5452(5) 0.1431(6) 0.0592(4) 0.0319(17) Uani 1 1 d . . .
H22 H 0.6116 0.1399 0.0684 0.038 Uiso 1 1 calc R . .
C23 C 0.4977(5) 0.1483(6) 0.1047(3) 0.0245(15) Uani 1 1 d . . .
H23 H 0.5315 0.1485 0.1452 0.029 Uiso 1 1 calc R . .
C24 C 0.2815(5) 0.0993(5) 0.3225(3) 0.0204(14) Uani 1 1 d . . .
C25 C 0.1966(5) 0.0775(6) 0.2833(3) 0.0287(16) Uani 1 1 d . . .
H25 H 0.1953 0.0564 0.2430 0.034 Uiso 1 1 calc R . .
C26 C 0.1138(5) 0.0865(7) 0.3026(4) 0.041(2) Uani 1 1 d . . .
H26 H 0.0557 0.0715 0.2756 0.049 Uiso 1 1 calc R . .
C27 C 0.1157(6) 0.1175(7) 0.3611(4) 0.040(2) Uani 1 1 d . . .
H27 H 0.0590 0.1236 0.3744 0.048 Uiso 1 1 calc R . .
C28 C 0.1995(6) 0.1394(7) 0.3999(4) 0.0365(19) Uani 1 1 d . . .
H28 H 0.2005 0.1604 0.4401 0.044 Uiso 1 1 calc R . .
C29 C 0.2821(5) 0.1312(6) 0.3813(3) 0.0278(16) Uani 1 1 d . . .
H29 H 0.3397 0.1473 0.4085 0.033 Uiso 1 1 calc R . .
C30 C 0.4817(4) 0.0452(5) 0.3551(3) 0.0193(13) Uani 1 1 d . . .
C31 C 0.5724(5) 0.0886(6) 0.3618(3) 0.0225(14) Uani 1 1 d . . .
H31 H 0.5853 0.1434 0.3341 0.027 Uiso 1 1 calc R . .
C32 C 0.6437(5) 0.0518(6) 0.4087(3) 0.0306(17) Uani 1 1 d . . .
H32 H 0.7053 0.0806 0.4126 0.037 Uiso 1 1 calc R . .
C33 C 0.6252(6) -0.0262(6) 0.4495(3) 0.0328(18) Uani 1 1 d . . .
H33 H 0.6737 -0.0496 0.4821 0.039 Uiso 1 1 calc R . .
C34 C 0.5353(5) -0.0709(6) 0.4431(3) 0.0282(16) Uani 1 1 d . . .
H34 H 0.5229 -0.1249 0.4713 0.034 Uiso 1 1 calc R . .
C35 C 0.4638(5) -0.0367(6) 0.3958(3) 0.0239(15) Uani 1 1 d . . .
H35 H 0.4031 -0.0688 0.3909 0.029 Uiso 1 1 calc R . .
C36 C 0.1457(7) 0.7565(9) 0.1551(5) 0.057(3) Uani 1 1 d . . .
H36 H 0.2099 0.7893 0.1603 0.069 Uiso 1 1 calc R . .
Cl3 Cl 0.0861(2) 0.7780(3) 0.08045(13) 0.0740(8) Uani 1 1 d . . .
Cl4 Cl 0.1561(2) 0.6119(3) 0.17152(15) 0.0779(9) Uani 1 1 d . . .
Cl5 Cl 0.0884(2) 0.8280(3) 0.20334(14) 0.0726(8) Uani 1 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'
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'
Cl Cl 0.1484 0.1585 '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'
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
P2 Pd1 P1 92.24(6) . . ?
P2 Pd1 Cl1 177.83(7) . . ?
P1 Pd1 Cl1 89.09(6) . . ?
P2 Pd1 Cl2 88.87(6) . . ?
P1 Pd1 Cl2 169.99(6) . . ?
Cl1 Pd1 Cl2 90.13(6) . . ?
C18 P1 C12 108.6(3) . . ?
C18 P1 C1 101.6(3) . . ?
C12 P1 C1 105.2(3) . . ?
C18 P1 Pd1 113.0(2) . . ?
C12 P1 Pd1 109.6(2) . . ?
C1 P1 Pd1 118.2(2) . . ?
C30 P2 C24 107.5(3) . . ?
C30 P2 C2 101.0(3) . . ?
C24 P2 C2 102.9(3) . . ?
C30 P2 Pd1 115.3(2) . . ?
C24 P2 Pd1 110.0(2) . . ?
C2 P2 Pd1 118.8(2) . . ?
N1 C1 P1 112.6(4) . . ?
N1 C2 P2 112.0(4) . . ?
C2 N1 C3 111.2(5) . . ?
C2 N1 C1 109.4(5) . . ?
C3 N1 C1 109.9(5) . . ?
N1 C3 C4 113.2(5) . . ?
C5 C4 C3 113.7(6) . . ?
C4 C5 Se1 113.4(5) . . ?
C6 Se1 C5 101.0(3) . . ?
C7 C6 C11 119.8(7) . . ?
C7 C6 Se1 117.4(5) . . ?
C11 C6 Se1 122.8(6) . . ?
C6 C7 C8 120.0(7) . . ?
C9 C8 C7 120.3(7) . . ?
C8 C9 C10 119.9(7) . . ?
C11 C10 C9 119.8(7) . . ?
C10 C11 C6 120.1(7) . . ?
C17 C12 C13 117.2(7) . . ?
C17 C12 P1 121.8(6) . . ?
C13 C12 P1 120.9(6) . . ?
C14 C13 C12 121.1(8) . . ?
C15 C14 C13 120.9(8) . . ?
C14 C15 C16 118.8(8) . . ?
C15 C16 C17 120.8(10) . . ?
C12 C17 C16 121.1(9) . . ?
C19 C18 C23 119.3(6) . . ?
C19 C18 P1 123.0(5) . . ?
C23 C18 P1 117.6(5) . . ?
C18 C19 C20 119.5(7) . . ?
C21 C20 C19 120.8(7) . . ?
C20 C21 C22 120.0(7) . . ?
C23 C22 C21 120.0(7) . . ?
C22 C23 C18 120.4(7) . . ?
C25 C24 C29 119.2(6) . . ?
C25 C24 P2 119.4(5) . . ?
C29 C24 P2 121.3(5) . . ?
C24 C25 C26 120.2(7) . . ?
C27 C26 C25 120.0(8) . . ?
C28 C27 C26 119.9(7) . . ?
C27 C28 C29 120.7(8) . . ?
C28 C29 C24 120.1(7) . . ?
C31 C30 C35 119.3(6) . . ?
C31 C30 P2 119.8(5) . . ?
C35 C30 P2 120.9(5) . . ?
C32 C31 C30 120.3(7) . . ?
C33 C32 C31 120.1(7) . . ?
C32 C33 C34 120.1(7) . . ?
C35 C34 C33 120.3(7) . . ?
C34 C35 C30 119.7(7) . . ?
Cl4 C36 Cl5 111.2(6) . . ?
Cl4 C36 Cl3 110.6(6) . . ?
Cl5 C36 Cl3 110.1(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
Pd1 P2 2.2409(17) . ?
Pd1 P1 2.2459(17) . ?
Pd1 Cl1 2.3580(17) . ?
Pd1 Cl2 2.3697(16) . ?
P1 C18 1.801(7) . ?
P1 C12 1.813(6) . ?
P1 C1 1.827(6) . ?
P2 C30 1.818(7) . ?
P2 C24 1.820(6) . ?
P2 C2 1.840(6) . ?
C1 N1 1.478(8) . ?
C2 N1 1.452(8) . ?
N1 C3 1.478(8) . ?
C3 C4 1.533(9) . ?
C4 C5 1.518(10) . ?
C5 Se1 1.967(7) . ?
Se1 C6 1.914(7) . ?
C6 C7 1.381(10) . ?
C6 C11 1.393(10) . ?
C7 C8 1.395(11) . ?
C8 C9 1.379(11) . ?
C9 C10 1.393(11) . ?
C10 C11 1.391(11) . ?
C12 C17 1.373(11) . ?
C12 C13 1.381(10) . ?
C13 C14 1.377(11) . ?
C14 C15 1.349(14) . ?
C15 C16 1.365(15) . ?
C16 C17 1.374(13) . ?
C18 C19 1.390(9) . ?
C18 C23 1.397(9) . ?
C19 C20 1.394(10) . ?
C20 C21 1.368(11) . ?
C21 C22 1.388(11) . ?
C22 C23 1.378(10) . ?
C24 C25 1.387(10) . ?
C24 C29 1.396(10) . ?
C25 C26 1.387(10) . ?
C26 C27 1.384(12) . ?
C27 C28 1.371(12) . ?
C28 C29 1.375(10) . ?
C30 C31 1.400(9) . ?
C30 C35 1.401(9) . ?
C31 C32 1.390(9) . ?
C32 C33 1.377(11) . ?
C33 C34 1.396(11) . ?
C34 C35 1.388(10) . ?
C36 Cl4 1.732(10) . ?
C36 Cl5 1.744(11) . ?
C36 Cl3 1.756(11) . ?
