#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:09:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179233 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/53/4315356.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_4315356
loop_
_publ_author_name
'Emanuele Amadio'
'Gianni Cavinato'
'Alessandro Dolmella'
'Luigi Toniolo'
_publ_section_title
;
 Catalytic Properties of [Pd(COOMe)nX2-n(PPh3)2] (n= 0, 1, 2; X = Cl, NO2,
 ONO2, OAc and OTs) in the Oxidative Carbonylation of MeOH
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3721
_journal_page_last               3729
_journal_paper_doi               10.1021/ic901569w
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C37 H32 Cl2 N2 O6 P2 Pd'
_chemical_formula_weight         839.89
_chemical_name_systematic
;
 cis-bis(nitrato,O)-bis(triphenylphosphine)-palladium(II)
 dichloromethane solvate
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.06(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.975(2)
_cell_length_b                   20.127(3)
_cell_length_c                   15.479(3)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      15.9
_cell_measurement_theta_min      12.8
_cell_volume                     3716.2(11)
_computing_cell_refinement       'FEBO system'
_computing_data_collection       'FEBO system'
_computing_data_reduction        'FEBO system'
_computing_molecular_graphics    'WinGX 1.70.00 (Farrugia, 1999)'
_computing_publication_material  'SHELXTL NT vers.5.10 (Sheldrick, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al. 1999)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Philips PW1100 dffractometer'
_diffrn_measurement_method       'omega-2 theta'
_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  0.0179
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6740
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.31
_diffrn_standards_decay_%        negligible
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.777
_exptl_absorpt_correction_T_max  0.882
_exptl_absorpt_correction_T_min  0.821
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.245
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         6487
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.245
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0523
_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)+(0.0000P)²+12.7950P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1278
_reflns_number_gt                5786
_reflns_number_total             6487
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901569w_si_001_2.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'psi-scans' was replaced
with 'psi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4315356
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
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.45623(3) 0.188807(18) 0.92939(2) 0.03415(12) Uani 1 1 d . . .
P1 P 0.26784(10) 0.17227(6) 0.91684(8) 0.0346(3) Uani 1 1 d . . .
P2 P 0.47360(10) 0.20024(6) 0.78627(8) 0.0338(3) Uani 1 1 d . . .
N1 N 0.5036(4) 0.1383(2) 1.1038(3) 0.0506(11) Uani 1 1 d . . .
O1 O 0.4468(3) 0.18591(17) 1.0634(2) 0.0417(8) Uani 1 1 d . . .
O2 O 0.5401(3) 0.0927(2) 1.0609(3) 0.0612(10) Uani 1 1 d . . .
O3 O 0.5188(5) 0.1430(2) 1.1827(3) 0.0811(15) Uani 1 1 d . . .
N2 N 0.6563(4) 0.2661(3) 0.9601(3) 0.0635(15) Uani 1 1 d . . .
O4 O 0.6301(3) 0.2034(2) 0.9582(2) 0.0552(10) Uani 1 1 d . . .
O5 O 0.5805(4) 0.3076(2) 0.9486(3) 0.0751(13) Uani 1 1 d . . .
O6 O 0.7558(4) 0.2805(3) 0.9738(3) 0.0957(18) Uani 1 1 d . . .
C1 C 0.1913(4) 0.1520(2) 0.8137(3) 0.0381(10) Uani 1 1 d . . .
C2 C 0.1613(4) 0.2020(3) 0.7526(3) 0.0422(11) Uani 1 1 d . . .
H2 H 0.1786 0.2461 0.7657 0.051 Uiso 1 1 calc R . .
C3 C 0.1059(4) 0.1860(3) 0.6728(4) 0.0510(13) Uani 1 1 d . . .
H3 H 0.0864 0.2193 0.6326 0.061 Uiso 1 1 calc R . .
C4 C 0.0799(5) 0.1212(3) 0.6532(4) 0.0618(16) Uani 1 1 d . . .
H4 H 0.0432 0.1107 0.5995 0.074 Uiso 1 1 calc R . .
C5 C 0.1075(6) 0.0715(3) 0.7121(4) 0.0664(17) Uani 1 1 d . . .
H5 H 0.0890 0.0277 0.6983 0.080 Uiso 1 1 calc R . .
C6 C 0.1630(5) 0.0866(3) 0.7925(4) 0.0515(13) Uani 1 1 d . . .
H6 H 0.1813 0.0528 0.8323 0.062 Uiso 1 1 calc R . .
C7 C 0.1991(4) 0.2467(2) 0.9539(3) 0.0412(11) Uani 1 1 d . . .
C8 C 0.2606(5) 0.2924(3) 1.0054(4) 0.0508(13) Uani 1 1 d . . .
H8 H 0.3363 0.2850 1.0210 0.061 Uiso 1 1 calc R . .
C9 C 0.2098(6) 0.3487(3) 1.0336(4) 0.0646(16) Uani 1 1 d . . .
H9 H 0.2512 0.3791 1.0685 0.078 Uiso 1 1 calc R . .
C10 C 0.0982(6) 0.3602(3) 1.0105(5) 0.0687(18) Uani 1 1 d . . .
H10 H 0.0647 0.3988 1.0288 0.082 Uiso 1 1 calc R . .
C11 C 0.0360(5) 0.3152(3) 0.9610(5) 0.0648(17) Uani 1 1 d . . .
H11 H -0.0399 0.3229 0.9464 0.078 Uiso 1 1 calc R . .
C12 C 0.0858(4) 0.2582(3) 0.9324(4) 0.0533(14) Uani 1 1 d . . .
H12 H 0.0433 0.2275 0.8988 0.064 Uiso 1 1 calc R . .
C13 C 0.2341(4) 0.1038(3) 0.9882(3) 0.0423(11) Uani 1 1 d . . .
C14 C 0.2973(5) 0.0462(3) 0.9906(3) 0.0478(12) Uani 1 1 d . . .
H14 H 0.3605 0.0438 0.9599 0.057 Uiso 1 1 calc R . .
C15 C 0.2672(6) -0.0080(3) 1.0385(4) 0.0625(16) Uani 1 1 d . . .
H15 H 0.3093 -0.0469 1.0394 0.075 Uiso 1 1 calc R . .
C16 C 0.1749(7) -0.0040(4) 1.0844(5) 0.085(2) Uani 1 1 d . . .
H16 H 0.1544 -0.0404 1.1165 0.102 Uiso 1 1 calc R . .
C17 C 0.1117(7) 0.0535(4) 1.0837(6) 0.095(3) Uani 1 1 d . . .
H17 H 0.0491 0.0558 1.1151 0.114 Uiso 1 1 calc R . .
C18 C 0.1422(5) 0.1079(3) 1.0358(4) 0.0681(18) Uani 1 1 d . . .
H18 H 0.1007 0.1470 1.0357 0.082 Uiso 1 1 calc R . .
C19 C 0.4302(4) 0.1247(2) 0.7283(3) 0.0408(11) Uani 1 1 d . . .
C20 C 0.4589(5) 0.0654(3) 0.7715(4) 0.0604(15) Uani 1 1 d . . .
H20 H 0.4935 0.0664 0.8278 0.072 Uiso 1 1 calc R . .
C21 C 0.4356(7) 0.0044(3) 0.7301(6) 0.084(2) Uani 1 1 d . . .
H21 H 0.4553 -0.0351 0.7586 0.100 Uiso 1 1 calc R . .
C22 C 0.3841(7) 0.0032(4) 0.6481(6) 0.091(3) Uani 1 1 d . . .
H22 H 0.3706 -0.0373 0.6201 0.109 Uiso 1 1 calc R . .
C23 C 0.3525(6) 0.0606(4) 0.6068(5) 0.080(2) Uani 1 1 d . . .
H23 H 0.3156 0.0591 0.5514 0.096 Uiso 1 1 calc R . .
C24 C 0.3748(5) 0.1214(3) 0.6466(4) 0.0529(13) Uani 1 1 d . . .
H24 H 0.3521 0.1603 0.6179 0.064 Uiso 1 1 calc R . .
C25 C 0.6203(4) 0.2125(3) 0.7655(3) 0.0379(10) Uani 1 1 d . . .
C26 C 0.6956(5) 0.1601(3) 0.7723(4) 0.0637(16) Uani 1 1 d . . .
H26 H 0.6716 0.1177 0.7855 0.076 Uiso 1 1 calc R . .
C27 C 0.8068(5) 0.1714(4) 0.7594(5) 0.076(2) Uani 1 1 d . . .
H27 H 0.8573 0.1362 0.7637 0.091 Uiso 1 1 calc R . .
C28 C 0.8436(5) 0.2335(4) 0.7405(4) 0.0708(19) Uani 1 1 d . . .
H28 H 0.9188 0.2405 0.7328 0.085 Uiso 1 1 calc R . .
C29 C 0.7697(5) 0.2851(4) 0.7328(5) 0.0680(17) Uani 1 1 d . . .
H29 H 0.7943 0.3272 0.7189 0.082 Uiso 1 1 calc R . .
C30 C 0.6588(4) 0.2747(3) 0.7457(4) 0.0537(14) Uani 1 1 d . . .
H30 H 0.6091 0.3103 0.7411 0.064 Uiso 1 1 calc R . .
C31 C 0.4053(4) 0.2739(2) 0.7388(3) 0.0386(11) Uani 1 1 d . . .
C32 C 0.3685(4) 0.3212(3) 0.7948(4) 0.0505(13) Uani 1 1 d . . .
H32 H 0.3791 0.3147 0.8544 0.061 Uiso 1 1 calc R . .
C33 C 0.3158(5) 0.3785(3) 0.7616(5) 0.0707(19) Uani 1 1 d . . .
H33 H 0.2914 0.4104 0.7991 0.085 Uiso 1 1 calc R . .
C34 C 0.2996(6) 0.3880(3) 0.6732(6) 0.079(2) Uani 1 1 d . . .
H34 H 0.2612 0.4253 0.6511 0.095 Uiso 1 1 calc R . .
C35 C 0.3401(6) 0.3426(3) 0.6178(5) 0.076(2) Uani 1 1 d . . .
H35 H 0.3311 0.3499 0.5583 0.092 Uiso 1 1 calc R . .
C36 C 0.3941(5) 0.2860(3) 0.6502(4) 0.0556(14) Uani 1 1 d . . .
H36 H 0.4231 0.2559 0.6124 0.067 Uiso 1 1 calc R . .
C37 C 0.1796(11) 0.0610(6) 0.3608(8) 0.153(5) Uani 1 1 d . . .
H37A H 0.1337 0.0634 0.3060 0.183 Uiso 1 1 calc R . .
H37B H 0.1904 0.1059 0.3827 0.183 Uiso 1 1 calc R . .
Cl1 Cl 0.1096(3) 0.01464(16) 0.4342(3) 0.1504(12) Uani 1 1 d . . .
Cl2 Cl 0.3069(4) 0.0276(2) 0.3436(3) 0.1948(19) 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'
Pd Pd -0.9988 1.0072 '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
_geom_angle_publ_flag
O1 Pd O4 86.16(14) . . ?
O1 Pd P2 175.21(10) . . ?
O4 Pd P2 91.05(11) . . ?
O1 Pd P1 86.60(10) . . ?
O4 Pd P1 172.75(11) . . ?
P2 Pd P1 96.19(5) . . ?
C1 P1 C7 104.7(2) . . ?
C1 P1 C13 103.9(2) . . ?
C7 P1 C13 107.3(2) . . ?
C1 P1 Pd 121.90(16) . . ?
C7 P1 Pd 108.96(17) . . ?
C13 P1 Pd 109.19(16) . . ?
C31 P2 C19 112.6(2) . . ?
C31 P2 C25 102.9(2) . . ?
C19 P2 C25 105.2(2) . . ?
C31 P2 Pd 113.78(17) . . ?
C19 P2 Pd 110.64(17) . . ?
C25 P2 Pd 111.09(15) . . ?
O3 N1 O2 124.6(5) . . ?
O3 N1 O1 116.6(5) . . ?
O2 N1 O1 118.8(4) . . ?
N1 O1 Pd 115.2(3) . . ?
O6 N2 O5 123.8(6) . . ?
O6 N2 O4 117.5(6) . . ?
O5 N2 O4 118.7(5) . . ?
N2 O4 Pd 111.8(3) . . ?
C6 C1 C2 118.5(5) . . ?
C6 C1 P1 120.9(4) . . ?
C2 C1 P1 120.6(4) . . ?
C3 C2 C1 120.4(5) . . ?
C4 C3 C2 120.0(5) . . ?
C3 C4 C5 120.7(5) . . ?
C4 C5 C6 120.2(6) . . ?
C1 C6 C5 120.3(5) . . ?
C12 C7 C8 119.0(5) . . ?
C12 C7 P1 121.4(4) . . ?
C8 C7 P1 119.6(4) . . ?
C9 C8 C7 120.1(6) . . ?
C10 C9 C8 120.3(6) . . ?
C11 C10 C9 120.4(5) . . ?
C10 C11 C12 120.0(6) . . ?
C11 C12 C7 120.1(6) . . ?
C18 C13 C14 119.7(5) . . ?
C18 C13 P1 120.4(4) . . ?
C14 C13 P1 119.8(4) . . ?
C15 C14 C13 120.5(5) . . ?
C16 C15 C14 119.5(6) . . ?
C15 C16 C17 120.8(7) . . ?
C16 C17 C18 119.7(7) . . ?
C13 C18 C17 119.9(6) . . ?
C24 C19 C20 118.5(5) . . ?
C24 C19 P2 126.0(4) . . ?
C20 C19 P2 115.5(4) . . ?
C19 C20 C21 119.9(7) . . ?
C22 C21 C20 119.9(7) . . ?
C23 C22 C21 120.5(6) . . ?
C22 C23 C24 120.5(7) . . ?
C19 C24 C23 120.7(6) . . ?
C30 C25 C26 118.7(5) . . ?
C30 C25 P2 120.4(4) . . ?
C26 C25 P2 120.8(4) . . ?
C27 C26 C25 119.5(6) . . ?
C28 C27 C26 121.0(6) . . ?
C29 C28 C27 119.8(6) . . ?
C28 C29 C30 120.0(6) . . ?
C29 C30 C25 121.0(6) . . ?
C32 C31 C36 119.3(5) . . ?
C32 C31 P2 117.7(4) . . ?
C36 C31 P2 122.9(4) . . ?
C31 C32 C33 119.9(6) . . ?
C34 C33 C32 120.1(6) . . ?
C35 C34 C33 120.1(6) . . ?
C34 C35 C36 120.2(7) . . ?
C35 C36 C31 120.3(6) . . ?
Cl2 C37 Cl1 112.2(6) . . ?
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
Pd O1 2.088(3) . ?
Pd O4 2.111(4) . ?
Pd P2 2.2551(13) . ?
Pd P1 2.2717(13) . ?
P1 C1 1.817(5) . ?
P1 C7 1.826(5) . ?
P1 C13 1.833(5) . ?
P2 C31 1.817(5) . ?
P2 C19 1.818(5) . ?
P2 C25 1.831(5) . ?
N1 O3 1.222(6) . ?
N1 O2 1.235(6) . ?
N1 O1 1.303(5) . ?
N2 O6 1.226(6) . ?
N2 O5 1.235(7) . ?
N2 O4 1.301(7) . ?
C1 C6 1.390(7) . ?
C1 C2 1.406(7) . ?
C2 C3 1.388(7) . ?
C3 C4 1.367(8) . ?
C4 C5 1.375(9) . ?
C5 C6 1.392(8) . ?
C7 C12 1.386(7) . ?
C7 C8 1.387(7) . ?
C8 C9 1.374(8) . ?
C9 C10 1.372(9) . ?
C10 C11 1.363(10) . ?
C11 C12 1.384(8) . ?
C13 C18 1.379(8) . ?
C13 C14 1.385(7) . ?
C14 C15 1.384(8) . ?
C15 C16 1.369(9) . ?
C16 C17 1.382(10) . ?
C17 C18 1.389(9) . ?
C19 C24 1.377(7) . ?
C19 C20 1.396(7) . ?
C20 C21 1.401(9) . ?
C21 C22 1.362(12) . ?
C22 C23 1.358(12) . ?
C23 C24 1.385(8) . ?
C25 C30 1.379(7) . ?
C25 C26 1.385(8) . ?
C26 C27 1.382(8) . ?
C27 C28 1.365(10) . ?
C28 C29 1.362(9) . ?
C29 C30 1.377(8) . ?
C31 C32 1.386(7) . ?
C31 C36 1.388(7) . ?
C32 C33 1.390(8) . ?
C33 C34 1.379(10) . ?
C34 C35 1.371(11) . ?
C35 C36 1.382(9) . ?
C37 Cl2 1.707(11) . ?
C37 Cl1 1.742(11) . ?
