#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:01:19 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179947 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/42/7024214.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_7024214
loop_
_publ_author_name
'Crociani, Bruno'
'Antonaroli, Simonetta'
'Burattini, Marcello'
'Paoli, Paola'
'Rossi, Patrizia'
_publ_section_title
;
 Palladium complexes with a tridentate PNO ligand. Synthesis of eta1-allyl
 complexes and cross-coupling reactions promoted by boron compounds.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3665
_journal_page_last               3672
_journal_paper_doi               10.1039/b913130b
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C28 H24 N O P Pd'
_chemical_formula_weight         527.85
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.043(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.8186(3)
_cell_length_b                   18.2721(5)
_cell_length_c                   12.9970(4)
_cell_measurement_temperature    173
_cell_volume                     2280.43(12)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
;
_computing_molecular_graphics    'ORTEP-3 (Farruggia, 1997)'
_computing_publication_material  'PARST97 (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 16.4547
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'Xcalibur3 4 circles diffractometer'
_diffrn_measurement_method       'intensity from ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_sigmaI/netI    0.0943
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16704
_diffrn_reflns_theta_full        32.49
_diffrn_reflns_theta_max         32.49
_diffrn_reflns_theta_min         3.67
_exptl_absorpt_coefficient_mu    0.905
_exptl_absorpt_correction_T_max  0.709
_exptl_absorpt_correction_T_min  0.636
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
;
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.829
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         7446
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.829
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0367
_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)+(0.0214P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0591
_refine_ls_wR_factor_ref         0.0655
_reflns_number_gt                4554
_reflns_number_total             7446
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b913130b.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7024214
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
Pd1 Pd 0.686535(17) -0.035785(11) 0.276418(14) 0.02061(5) Uani 1 1 d
P1 P 0.72070(6) 0.07577(4) 0.22760(4) 0.01957(13) Uani 1 1 d
O1 O 0.65983(16) -0.13949(10) 0.33402(13) 0.0281(4) Uani 1 1 d
N1 N 0.51066(18) -0.01381(12) 0.33806(14) 0.0219(4) Uani 1 1 d
C1 C 0.5718(2) 0.13483(14) 0.23225(17) 0.0222(5) Uani 1 1 d
C2 C 0.5653(2) 0.20279(16) 0.18321(19) 0.0287(6) Uani 1 1 d
C3 C 0.4573(3) 0.25154(17) 0.1833(2) 0.0323(6) Uani 1 1 d
C4 C 0.3513(3) 0.23274(17) 0.2342(2) 0.0346(7) Uani 1 1 d
C5 C 0.3555(3) 0.16590(17) 0.2817(2) 0.0325(7) Uani 1 1 d
C6 C 0.4617(2) 0.11479(15) 0.28216(17) 0.0243(5) Uani 1 1 d
C7 C 0.4414(2) 0.04545(16) 0.33302(18) 0.0280(6) Uani 1 1 d
C8 C 0.4704(2) -0.07813(15) 0.38641(17) 0.0247(5) Uani 1 1 d
C9 C 0.3558(3) -0.08235(18) 0.4346(2) 0.0330(7) Uani 1 1 d
C10 C 0.3245(3) -0.1470(2) 0.4788(2) 0.0399(8) Uani 1 1 d
C11 C 0.4071(3) -0.2076(2) 0.4761(2) 0.0402(8) Uani 1 1 d
C12 C 0.5194(3) -0.20522(18) 0.4285(2) 0.0340(7) Uani 1 1 d
C13 C 0.5531(2) -0.14039(16) 0.38119(17) 0.0266(6) Uani 1 1 d
C14 C 0.8474(3) -0.07301(16) 0.2103(2) 0.0271(6) Uani 1 1 d
C15 C 0.7742(3) -0.11987(18) 0.1250(3) 0.0350(7) Uani 1 1 d
C16 C 0.7498(3) -0.1052(2) 0.0235(3) 0.0433(8) Uani 1 1 d
C17 C 0.7423(2) 0.08777(13) 0.09330(17) 0.0196(5) Uani 1 1 d
C18 C 0.6254(2) 0.07883(15) 0.01253(18) 0.0244(5) Uani 1 1 d
C19 C 0.6362(3) 0.08130(16) -0.09117(19) 0.0308(6) Uani 1 1 d
C20 C 0.7647(3) 0.09267(17) -0.1161(2) 0.0350(7) Uani 1 1 d
C21 C 0.8807(3) 0.10125(18) -0.0380(2) 0.0346(7) Uani 1 1 d
C22 C 0.8707(2) 0.09886(16) 0.06712(19) 0.0280(6) Uani 1 1 d
C23 C 0.8721(2) 0.11981(15) 0.31089(17) 0.0215(5) Uani 1 1 d
C24 C 0.9586(3) 0.07762(17) 0.3856(2) 0.0303(6) Uani 1 1 d
C25 C 1.0707(3) 0.10870(19) 0.4539(2) 0.0344(7) Uani 1 1 d
C26 C 1.0975(3) 0.18238(19) 0.4474(2) 0.0352(7) Uani 1 1 d
C27 C 1.0132(3) 0.22435(18) 0.3725(3) 0.0394(7) Uani 1 1 d
C28 C 0.9005(3) 0.19365(16) 0.3039(2) 0.0295(6) Uani 1 1 d
H2 H 0.637(2) 0.2144(14) 0.1458(17) 0.025(6) Uiso 1 1 d
H3 H 0.458(2) 0.2951(15) 0.1495(18) 0.025(7) Uiso 1 1 d
H4 H 0.277(2) 0.2654(14) 0.2343(16) 0.021(6) Uiso 1 1 d
H5 H 0.280(2) 0.1485(14) 0.3121(17) 0.025(6) Uiso 1 1 d
H7 H 0.360(2) 0.0479(14) 0.3659(17) 0.028(6) Uiso 1 1 d
H9 H 0.302(2) -0.0450(14) 0.4336(18) 0.021(7) Uiso 1 1 d
H10 H 0.250(2) -0.1466(15) 0.5049(18) 0.029(7) Uiso 1 1 d
H11 H 0.391(2) -0.2485(16) 0.5065(19) 0.037(8) Uiso 1 1 d
H12 H 0.572(2) -0.2447(16) 0.432(2) 0.036(8) Uiso 1 1 d
H14A H 0.9141(18) -0.0335(12) 0.1820(14) 0.005(5) Uiso 1 1 d
H14B H 0.894(3) -0.0973(17) 0.264(2) 0.040(8) Uiso 1 1 d
H15 H 0.744(3) -0.1606(17) 0.145(2) 0.047(9) Uiso 1 1 d
H16B H 0.705(3) -0.1348(19) -0.019(2) 0.056(11) Uiso 1 1 d
H16A H 0.780(3) -0.0622(18) -0.003(2) 0.048(10) Uiso 1 1 d
H18 H 0.538(2) 0.0750(13) 0.0286(16) 0.017(6) Uiso 1 1 d
H19 H 0.558(2) 0.0767(14) -0.1466(17) 0.020(6) Uiso 1 1 d
H20 H 0.771(2) 0.0912(16) -0.185(2) 0.038(7) Uiso 1 1 d
H21 H 0.963(2) 0.1081(16) -0.0542(19) 0.038(8) Uiso 1 1 d
H22 H 0.950(2) 0.1036(14) 0.1194(17) 0.021(6) Uiso 1 1 d
H24 H 0.940(3) 0.0330(15) 0.390(2) 0.028(7) Uiso 1 1 d
H25 H 1.125(2) 0.0854(15) 0.4982(18) 0.024(7) Uiso 1 1 d
H26 H 1.173(3) 0.2036(16) 0.492(2) 0.042(8) Uiso 1 1 d
H27 H 1.033(2) 0.2685(15) 0.3654(19) 0.021(7) Uiso 1 1 d
H28 H 0.840(2) 0.2243(15) 0.2517(18) 0.033(7) Uiso 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'
O O 0.0106 0.0060 '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'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C14 Pd1 O1 90.84(9)
C14 Pd1 N1 171.33(10)
O1 Pd1 N1 81.97(7)
C14 Pd1 P1 90.53(8)
O1 Pd1 P1 175.83(5)
N1 Pd1 P1 96.98(6)
C17 P1 C1 102.41(10)
C17 P1 C23 105.78(10)
C1 P1 C23 106.09(11)
C17 P1 Pd1 116.65(8)
C1 P1 Pd1 111.67(8)
C23 P1 Pd1 113.17(9)
C13 O1 Pd1 110.58(16)
C7 N1 C8 122.0(2)
C7 N1 Pd1 128.26(17)
C8 N1 Pd1 109.75(15)
C2 C1 C6 118.2(2)
C2 C1 P1 118.18(17)
C6 C1 P1 123.6(2)
C3 C2 C1 122.4(2)
C2 C3 C4 119.5(3)
C5 C4 C3 118.8(3)
C4 C5 C6 123.5(2)
C5 C6 C1 117.6(2)
C5 C6 C7 114.1(2)
C1 C6 C7 128.2(2)
N1 C7 C6 129.7(2)
C9 C8 C13 120.2(3)
C9 C8 N1 124.4(3)
C13 C8 N1 115.37(19)
C10 C9 C8 120.3(3)
C11 C10 C9 119.8(3)
C12 C11 C10 121.2(3)
C11 C12 C13 120.6(3)
O1 C13 C12 119.8(3)
O1 C13 C8 122.3(2)
C12 C13 C8 117.9(2)
C15 C14 Pd1 102.18(16)
C16 C15 C14 126.7(3)
C22 C17 C18 118.7(2)
C22 C17 P1 123.21(17)
C18 C17 P1 117.86(16)
C19 C18 C17 121.0(2)
C18 C19 C20 119.7(2)
C21 C20 C19 120.3(2)
C20 C21 C22 120.4(2)
C17 C22 C21 120.0(2)
C24 C23 C28 119.1(2)
C24 C23 P1 118.3(2)
C28 C23 P1 122.60(19)
C25 C24 C23 120.7(3)
C26 C25 C24 119.9(3)
C27 C26 C25 119.6(3)
C26 C27 C28 120.8(3)
C23 C28 C27 119.8(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pd1 C14 2.065(2)
Pd1 O1 2.0741(17)
Pd1 N1 2.0887(17)
Pd1 P1 2.1814(7)
P1 C17 1.815(2)
P1 C1 1.829(2)
P1 C23 1.833(2)
O1 C13 1.320(3)
N1 C7 1.273(3)
N1 C8 1.427(3)
C1 C2 1.391(4)
C1 C6 1.419(3)
C2 C3 1.385(4)
C3 C4 1.387(4)
C4 C5 1.365(4)
C5 C6 1.399(3)
C6 C7 1.462(4)
C8 C9 1.400(3)
C8 C13 1.408(4)
C9 C10 1.376(4)
C10 C11 1.376(4)
C11 C12 1.373(4)
C12 C13 1.406(4)
C14 C15 1.465(4)
C15 C16 1.317(4)
C17 C22 1.388(3)
C17 C18 1.394(3)
C18 C19 1.374(3)
C19 C20 1.382(3)
C20 C21 1.367(4)
C21 C22 1.391(3)
C23 C24 1.384(4)
C23 C28 1.385(4)
C24 C25 1.383(4)
C25 C26 1.378(4)
C26 C27 1.373(4)
C27 C28 1.386(4)
