#------------------------------------------------------------------------------
#$Date: 2019-11-17 10:12:37 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229281 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/78/7047843.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_7047843
loop_
_publ_author_name
'Fernández-Figueiras, Adolfo'
'Lucio-Martínez, Fátima'
'Munín-Cruz, Paula'
'Polo-Ces, Paula'
'Reigosa, Francisco'
'Adams, Harry'
'Pereira, M. Teresa'
'Vila, José M'
_publ_section_title
;
 Palladium iminophosphorane complexes: the pre-cursors to the missing link
 in triphenylphosphane chalcogenide metallacycles.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15801
_journal_page_last               15807
_journal_paper_doi               10.1039/c8dt03062f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C36 H28 Cl2 N0 O2 P2 Pd2'
_chemical_formula_weight         838.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/4
_audit_update_record
;
2018-07-13 deposited with the CCDC.
2018-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 95.459(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   16.503(5)
_cell_length_b                   10.164(5)
_cell_length_c                   19.571(5)
_cell_measurement_reflns_used    1987
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.26
_cell_measurement_theta_min      2.48
_cell_volume                     3268(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXL-2016/4 (Sheldrick, 2016)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0716
_diffrn_reflns_av_unetI/netI     0.0808
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27307
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.543
_exptl_absorpt_coefficient_mu    1.394
_exptl_absorpt_correction_T_max  0.8878
_exptl_absorpt_correction_T_min  0.7696
_exptl_absorpt_correction_type   multi-scans
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_description       plate
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.854
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6677
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0354P)²+0.8254P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0979
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4628
_reflns_number_total             6677
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt03062f2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7047843--7047847.cif.'
_cod_database_code               7047843
_shelx_shelxl_version_number     2016/4
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
C1 C 0.0204(3) 1.1542(4) 0.6582(2) 0.0205(11) Uani 1 1 d . .
C2 C -0.0106(3) 1.2811(4) 0.6478(2) 0.0258(12) Uani 1 1 d . .
H2 H -0.023094 1.311948 0.603311 0.031 Uiso 1 1 calc R U
C3 C -0.0230(3) 1.3613(5) 0.7027(2) 0.0306(13) Uani 1 1 d . .
H3 H -0.043458 1.445774 0.694826 0.037 Uiso 1 1 calc R U
C4 C -0.0055(3) 1.3177(5) 0.7693(2) 0.0299(13) Uani 1 1 d . .
H4 H -0.014881 1.372241 0.805873 0.036 Uiso 1 1 calc R U
C5 C 0.0259(3) 1.1936(5) 0.7814(2) 0.0270(12) Uani 1 1 d . .
H5 H 0.037628 1.163887 0.826224 0.032 Uiso 1 1 calc R U
C6 C 0.0399(3) 1.1127(4) 0.7262(2) 0.0188(11) Uani 1 1 d . .
C7 C 0.0151(3) 0.8389(4) 0.7704(2) 0.0218(11) Uani 1 1 d . .
C8 C -0.0363(3) 0.7640(5) 0.7262(3) 0.0297(13) Uani 1 1 d . .
H8 H -0.032246 0.769047 0.679215 0.036 Uiso 1 1 calc R U
C9 C -0.0931(3) 0.6824(5) 0.7506(3) 0.0394(15) Uani 1 1 d . .
H9 H -0.127921 0.633497 0.720286 0.047 Uiso 1 1 calc R U
C10 C -0.0981(4) 0.6735(5) 0.8201(3) 0.0458(16) Uani 1 1 d . .
H10 H -0.135758 0.616837 0.836835 0.055 Uiso 1 1 calc R U
C11 C -0.0485(4) 0.7468(5) 0.8647(3) 0.0474(17) Uani 1 1 d . .
H11 H -0.053044 0.740659 0.911613 0.057 Uiso 1 1 calc R U
C12 C 0.0091(4) 0.8311(5) 0.8406(3) 0.0343(14) Uani 1 1 d . .
H12 H 0.043032 0.881210 0.871116 0.041 Uiso 1 1 calc R U
C13 C 0.1771(3) 0.9576(5) 0.7857(2) 0.0241(11) Uani 1 1 d . .
C14 C 0.2092(4) 0.8462(5) 0.8199(3) 0.0359(14) Uani 1 1 d . .
H14 H 0.179358 0.768459 0.818825 0.043 Uiso 1 1 calc R U
C15 C 0.2857(4) 0.8519(6) 0.8553(3) 0.0420(16) Uani 1 1 d . .
H15 H 0.307406 0.777846 0.878179 0.050 Uiso 1 1 calc R U
C16 C 0.3299(4) 0.9675(6) 0.8566(3) 0.0442(16) Uani 1 1 d . .
H16 H 0.381933 0.970092 0.879512 0.053 Uiso 1 1 calc R U
C17 C 0.2981(4) 1.0776(6) 0.8249(3) 0.0416(15) Uani 1 1 d . .
H17 H 0.327777 1.155577 0.827143 0.050 Uiso 1 1 calc R U
C18 C 0.2214(3) 1.0736(5) 0.7891(2) 0.0316(13) Uani 1 1 d . .
H18 H 0.199726 1.148825 0.767392 0.038 Uiso 1 1 calc R U
C19 C 0.7068(3) 0.5578(4) 0.5354(2) 0.0239(12) Uani 1 1 d . .
C20 C 0.7487(4) 0.4417(5) 0.5217(2) 0.0336(14) Uani 1 1 d . .
H20 H 0.719796 0.365142 0.509887 0.040 Uiso 1 1 calc R U
C21 C 0.8330(4) 0.4412(5) 0.5260(3) 0.0405(15) Uani 1 1 d . .
H21 H 0.859500 0.363341 0.516725 0.049 Uiso 1 1 calc R U
C22 C 0.8797(4) 0.5522(5) 0.5434(3) 0.0384(15) Uani 1 1 d . .
H22 H 0.936168 0.549493 0.545001 0.046 Uiso 1 1 calc R U
C23 C 0.8393(3) 0.6681(5) 0.5586(2) 0.0315(13) Uani 1 1 d . .
H23 H 0.868804 0.743824 0.570954 0.038 Uiso 1 1 calc R U
C24 C 0.7548(3) 0.6692(4) 0.5550(2) 0.0253(12) Uani 1 1 d . .
C25 C 0.7391(3) 0.8905(4) 0.6495(2) 0.0216(11) Uani 1 1 d . .
C26 C 0.7163(3) 0.8536(4) 0.7131(2) 0.0284(13) Uani 1 1 d . .
H26 H 0.676979 0.788634 0.715561 0.034 Uiso 1 1 calc R U
C27 C 0.7506(3) 0.9113(5) 0.7726(3) 0.0331(13) Uani 1 1 d . .
H27 H 0.734357 0.885952 0.814902 0.040 Uiso 1 1 calc R U
C28 C 0.8094(3) 1.0072(5) 0.7688(3) 0.0329(13) Uani 1 1 d . .
H28 H 0.834201 1.044733 0.808815 0.039 Uiso 1 1 calc R U
C29 C 0.8312(3) 1.0470(5) 0.7058(3) 0.0346(14) Uani 1 1 d . .
H29 H 0.869480 1.113617 0.703556 0.042 Uiso 1 1 calc R U
C30 C 0.7968(3) 0.9893(5) 0.6460(3) 0.0293(13) Uani 1 1 d . .
H30 H 0.812176 1.016432 0.603719 0.035 Uiso 1 1 calc R U
C31 C 0.6844(3) 0.9172(5) 0.5042(2) 0.0252(12) Uani 1 1 d . .
C32 C 0.7490(4) 0.9532(6) 0.4680(3) 0.0456(16) Uani 1 1 d . .
H32 H 0.800045 0.916651 0.479978 0.055 Uiso 1 1 calc R U
C33 C 0.7390(4) 1.0433(6) 0.4140(3) 0.0516(18) Uani 1 1 d . .
H33 H 0.782753 1.067188 0.389954 0.062 Uiso 1 1 calc R U
C34 C 0.6646(4) 1.0945(6) 0.3976(3) 0.0553(18) Uani 1 1 d . .
H34 H 0.656702 1.151803 0.360502 0.066 Uiso 1 1 calc R U
C35 C 0.5995(4) 1.0646(6) 0.4343(3) 0.0554(18) Uani 1 1 d . .
H35 H 0.549196 1.104253 0.423273 0.066 Uiso 1 1 calc R U
C36 C 0.6100(4) 0.9753(5) 0.4875(3) 0.0402(15) Uani 1 1 d . .
H36 H 0.566341 0.954265 0.512257 0.048 Uiso 1 1 calc R U
O1 O 0.0927(2) 0.9093(3) 0.66033(14) 0.0236(8) Uani 1 1 d . .
O2 O 0.6122(2) 0.7502(3) 0.58944(15) 0.0232(8) Uani 1 1 d . .
P1 P 0.08205(8) 0.95140(12) 0.73340(6) 0.0207(3) Uani 1 1 d . .
P2 P 0.69391(9) 0.80612(12) 0.57526(6) 0.0239(3) Uani 1 1 d . .
CL1 Cl -0.03743(11) 1.14759(13) 0.50073(6) 0.0501(5) Uani 1 1 d . .
CL2 Cl 0.55968(9) 0.39428(12) 0.46737(6) 0.0338(3) Uani 1 1 d . .
PD1 Pd 0.03090(3) 1.02332(4) 0.58601(2) 0.02449(12) Uani 1 1 d . .
PD2 Pd 0.58853(3) 0.57906(4) 0.53349(2) 0.02554(12) 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'
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'
Cl Cl 0.1484 0.1585 '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
C2 C1 C6 117.6(4) . .
C2 C1 PD1 125.3(3) . .
C6 C1 PD1 116.9(3) . .
C3 C2 C1 120.8(4) . .
C2 C3 C4 120.8(4) . .
C5 C4 C3 120.0(4) . .
C4 C5 C6 119.6(4) . .
C5 C6 C1 121.1(4) . .
C5 C6 P1 125.0(3) . .
C1 C6 P1 113.8(3) . .
C8 C7 C12 119.4(5) . .
C8 C7 P1 117.7(4) . .
C12 C7 P1 122.8(4) . .
C9 C8 C7 121.0(5) . .
C8 C9 C10 119.5(5) . .
C11 C10 C9 120.7(5) . .
C10 C11 C12 120.5(5) . .
C7 C12 C11 119.0(5) . .
C18 C13 C14 119.6(5) . .
C18 C13 P1 119.2(4) . .
C14 C13 P1 121.2(4) . .
C15 C14 C13 119.6(5) . .
C14 C15 C16 120.0(5) . .
C17 C16 C15 120.7(6) . .
C16 C17 C18 120.0(6) . .
C13 C18 C17 120.1(5) . .
C20 C19 C24 116.8(5) . .
C20 C19 PD2 126.5(4) . .
C24 C19 PD2 116.6(3) . .
C21 C20 C19 120.0(5) . .
C20 C21 C22 122.8(5) . .
C21 C22 C23 118.1(5) . .
C24 C23 C22 119.4(5) . .
C23 C24 C19 122.7(4) . .
C23 C24 P2 125.4(4) . .
C19 C24 P2 111.9(4) . .
C26 C25 C30 119.0(4) . .
C26 C25 P2 118.2(4) . .
C30 C25 P2 122.8(4) . .
C27 C26 C25 121.3(5) . .
C26 C27 C28 119.3(5) . .
C29 C28 C27 120.0(5) . .
C28 C29 C30 120.8(5) . .
C29 C30 C25 119.5(5) . .
C36 C31 C32 118.7(5) . .
C36 C31 P2 117.8(4) . .
C32 C31 P2 123.3(4) . .
C31 C32 C33 121.3(5) . .
C34 C33 C32 118.2(6) . .
C33 C34 C35 121.9(6) . .
C34 C35 C36 119.3(6) . .
C31 C36 C35 120.4(5) . .
P1 O1 PD1 114.45(17) . .
P2 O2 PD2 110.14(17) . .
O1 P1 C6 105.31(19) . .
O1 P1 C7 109.4(2) . .
C6 P1 C7 111.6(2) . .
O1 P1 C13 112.0(2) . .
C6 P1 C13 109.1(2) . .
C7 P1 C13 109.4(2) . .
O2 P2 C24 106.2(2) . .
O2 P2 C31 111.5(2) . .
C24 P2 C31 109.3(2) . .
O2 P2 C25 110.0(2) . .
C24 P2 C25 110.8(2) . .
C31 P2 C25 109.2(2) . .
O2 P2 PD2 41.14(11) . .
C24 P2 PD2 70.03(18) . .
C31 P2 PD2 105.77(17) . .
C25 P2 PD2 141.99(16) . .
PD1 CL1 PD1 93.60(5) . 3_576
PD2 CL2 PD2 93.80(5) . 3_666
C1 PD1 O1 86.79(16) . .
C1 PD1 CL1 94.58(14) . .
O1 PD1 CL1 178.61(9) . .
C1 PD1 CL1 176.40(14) . 3_576
O1 PD1 CL1 92.26(9) . 3_576
CL1 PD1 CL1 86.40(5) . 3_576
C19 PD2 O2 86.89(16) . .
C19 PD2 CL2 94.17(13) . .
O2 PD2 CL2 177.49(9) . .
C19 PD2 CL2 179.31(12) . 3_666
O2 PD2 CL2 92.76(10) . 3_666
CL2 PD2 CL2 86.20(5) . 3_666
C19 PD2 P2 61.50(13) . .
O2 PD2 P2 28.72(9) . .
CL2 PD2 P2 151.13(5) . .
CL2 PD2 P2 118.30(4) 3_666 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.396(6) .
C1 C6 1.404(6) .
C1 PD1 1.960(4) .
C2 C3 1.380(6) .
C3 C4 1.380(6) .
C4 C5 1.375(6) .
C5 C6 1.395(6) .
C6 P1 1.781(5) .
C7 C8 1.381(6) .
C7 C12 1.389(6) .
C7 P1 1.790(5) .
C8 C9 1.371(7) .
C9 C10 1.374(8) .
C10 C11 1.360(8) .
C11 C12 1.395(7) .
C13 C18 1.385(7) .
C13 C14 1.394(7) .
C13 P1 1.791(5) .
C14 C15 1.382(7) .
C15 C16 1.383(8) .
C16 C17 1.361(8) .
C17 C18 1.387(7) .
C19 C20 1.406(7) .
C19 C24 1.414(7) .
C19 PD2 1.961(5) .
C20 C21 1.386(8) .
C21 C22 1.390(8) .
C22 C23 1.399(7) .
C23 C24 1.390(7) .
C24 P2 1.783(5) .
C25 C26 1.386(6) .
C25 C30 1.390(7) .
C25 P2 1.787(5) .
C26 C27 1.377(6) .
C27 C28 1.382(7) .
C28 C29 1.378(7) .
C29 C30 1.383(7) .
C31 C36 1.373(7) .
C31 C32 1.384(7) .
C31 P2 1.787(5) .
C32 C33 1.397(7) .
C33 C34 1.345(8) .
C34 C35 1.382(8) .
C35 C36 1.380(7) .
O1 P1 1.519(3) .
O1 PD1 2.053(3) .
O2 P2 1.514(3) .
O2 PD2 2.073(3) .
P2 PD2 2.9577(17) .
CL1 PD1 2.3008(14) .
CL1 PD1 2.4384(14) 3_576
CL2 PD2 2.3047(14) .
CL2 PD2 2.4593(17) 3_666
PD1 CL1 2.4383(14) 3_576
PD2 CL2 2.4594(17) 3_666
