#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:15:42 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179834 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/30/7013079.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_7013079
loop_
_publ_author_name
'Robin B. Bedford'
'Catherine S. J. Cazin'
'Simon J. Coles'
'Thomas Gelbrich'
'Michael B. Hursthouse'
'Véronique J. M. Scordia'
_publ_section_title
;
 Phosphine and arsine adducts of N-donor palladacycles as catalysts in
 the Suzuki coupling of aryl bromides
;
_journal_issue                   17
_journal_name_full               'Dalton Trans.'
_journal_page_first              3350
_journal_page_last               3356
_journal_paper_doi               10.1039/B304053D
_journal_year                    2003
_chemical_formula_sum            'C30 H20 F6 N2 O4 Pd2'
_chemical_formula_weight         799.28
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                68.0360(15)
_cell_angle_beta                 85.2730(15)
_cell_angle_gamma                88.4090(9)
_cell_formula_units_Z            2
_cell_length_a                   9.6340(2)
_cell_length_b                   11.3047(3)
_cell_length_c                   14.3380(3)
_cell_measurement_temperature    150(2)
_cell_volume                     1443.27(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0904
_diffrn_reflns_av_sigmaI/netI    0.0645
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17171
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    1.324
_exptl_absorpt_correction_T_max  0.6921
_exptl_absorpt_correction_T_min  0.5573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.839
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.059
_refine_diff_density_min         -1.401
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       0.0061(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         5041
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.319
_refine_ls_shift/su_mean         0.020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0796P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1147
_reflns_number_gt                4225
_reflns_number_total             5041
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            B304053D.txt
_cod_data_source_block           6c
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7013079
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.61034(3) 0.38332(3) 0.19185(2) 0.02628(14) Uani 1 1 d . . .
Pd2 Pd 0.58747(3) 0.10316(3) 0.31592(2) 0.02629(14) Uani 1 1 d . . .
O2 O 0.4091(3) 0.1155(3) 0.2436(2) 0.0328(6) Uani 1 1 d . . .
N1 N 0.7542(3) 0.3634(3) 0.0871(2) 0.0254(7) Uani 1 1 d . . .
O4 O 0.4851(3) 0.4069(3) 0.3063(2) 0.0372(7) Uani 1 1 d . . .
O3 O 0.4763(3) 0.1983(3) 0.4053(2) 0.0375(7) Uani 1 1 d . . .
O1 O 0.4279(3) 0.3222(3) 0.1418(2) 0.0337(7) Uani 1 1 d . . .
N2 N 0.7726(3) 0.0780(3) 0.3775(2) 0.0281(7) Uani 1 1 d . . .
F3 F 0.1287(3) 0.1935(3) 0.1965(2) 0.0578(8) Uani 1 1 d DU . .
F2 F 0.2391(3) 0.0963(3) 0.1111(3) 0.0705(10) Uani 1 1 d DU . .
F1 F 0.2158(3) 0.2987(3) 0.0475(2) 0.0574(8) Uani 1 1 d DU . .
C16 C 0.6820(4) 0.0029(4) 0.2442(3) 0.0283(9) Uani 1 1 d . . .
C1 C 0.7717(4) 0.4520(4) 0.2282(3) 0.0299(9) Uani 1 1 d . . .
C9 C 0.6232(5) 0.3593(4) -0.0494(3) 0.0347(9) Uani 1 1 d . . .
H9 H 0.5656 0.4254 -0.0423 0.042 Uiso 1 1 calc R . .
C7 C 0.8788(4) 0.3909(4) 0.0974(3) 0.0280(9) Uani 1 1 d . . .
H7 H 0.9559 0.3774 0.0567 0.034 Uiso 1 1 calc R . .
C14 C 0.3734(4) 0.2162(4) 0.1763(3) 0.0254(8) Uani 1 1 d . . .
C15 C 0.2382(4) 0.2016(4) 0.1313(3) 0.0378(10) Uani 1 1 d . . .
C22 C 0.8660(4) 0.0215(4) 0.3395(3) 0.0326(9) Uani 1 1 d . . .
H22 H 0.9585 0.0103 0.3594 0.039 Uiso 1 1 calc R . .
C5 C 1.0231(5) 0.4845(4) 0.1908(3) 0.0383(10) Uani 1 1 d . . .
H5 H 1.1068 0.4769 0.1536 0.046 Uiso 1 1 calc R . .
C8 C 0.7297(4) 0.3094(4) 0.0136(3) 0.0264(8) Uani 1 1 d . . .
C10 C 0.6021(5) 0.3106(4) -0.1233(3) 0.0425(11) Uani 1 1 d . . .
H10 H 0.5306 0.3446 -0.1678 0.051 Uiso 1 1 calc R . .
C29 C 0.4507(4) 0.3130(4) 0.3836(3) 0.0322(9) Uani 1 1 d . A .
C6 C 0.8969(4) 0.4425(4) 0.1725(3) 0.0312(9) Uani 1 1 d . . .
C13 C 0.8116(4) 0.2106(4) 0.0058(3) 0.0336(9) Uani 1 1 d . . .
H13 H 0.8834 0.1763 0.0498 0.040 Uiso 1 1 calc R . .
C28 C 0.7128(5) 0.1018(4) 0.5355(3) 0.0438(11) Uani 1 1 d . . .
H28 H 0.6353 0.0471 0.5453 0.053 Uiso 1 1 calc R . .
C20 C 0.9024(5) -0.0949(4) 0.2199(3) 0.0429(11) Uani 1 1 d . . .
H20 H 0.9970 -0.1124 0.2340 0.051 Uiso 1 1 calc R . .
C23 C 0.8038(4) 0.1281(4) 0.4517(3) 0.0311(9) Uani 1 1 d . . .
C11 C 0.6850(5) 0.2129(4) -0.1318(3) 0.0424(11) Uani 1 1 d . . .
H11 H 0.6710 0.1807 -0.1827 0.051 Uiso 1 1 calc R . .
C26 C 0.8456(6) 0.2354(4) 0.5913(4) 0.0507(13) Uani 1 1 d . . .
H26 H 0.8587 0.2735 0.6388 0.061 Uiso 1 1 calc R . .
C17 C 0.6250(5) -0.0432(4) 0.1790(3) 0.0354(9) Uani 1 1 d . . .
H17 H 0.5308 -0.0255 0.1635 0.042 Uiso 1 1 calc R . .
C18 C 0.7074(5) -0.1162(4) 0.1359(3) 0.0404(11) Uani 1 1 d . . .
H18 H 0.6674 -0.1500 0.0928 0.048 Uiso 1 1 calc R . .
C12 C 0.7874(5) 0.1623(4) -0.0673(3) 0.0384(10) Uani 1 1 d . . .
H12 H 0.8422 0.0937 -0.0727 0.046 Uiso 1 1 calc R . .
C21 C 0.8223(4) -0.0235(4) 0.2653(3) 0.0336(9) Uani 1 1 d . . .
C3 C 0.9034(5) 0.5483(4) 0.3171(3) 0.0443(12) Uani 1 1 d . . .
H3 H 0.9058 0.5862 0.3660 0.053 Uiso 1 1 calc R . .
C27 C 0.7338(6) 0.1553(5) 0.6062(3) 0.0504(13) Uani 1 1 d . . .
H27 H 0.6711 0.1367 0.6646 0.060 Uiso 1 1 calc R . .
C2 C 0.7772(5) 0.5053(4) 0.3016(3) 0.0366(10) Uani 1 1 d . . .
H2 H 0.6948 0.5120 0.3406 0.044 Uiso 1 1 calc R . .
C4 C 1.0249(5) 0.5375(4) 0.2638(4) 0.0457(12) Uani 1 1 d . . .
H4 H 1.1103 0.5663 0.2769 0.055 Uiso 1 1 calc R . .
C24 C 0.9189(5) 0.2063(4) 0.4368(4) 0.0410(11) Uani 1 1 d . . .
H24 H 0.9833 0.2228 0.3795 0.049 Uiso 1 1 calc R . .
C30 C 0.3679(6) 0.3448(5) 0.4680(4) 0.0509(13) Uani 1 1 d . . .
C25 C 0.9378(6) 0.2603(5) 0.5084(4) 0.0504(13) Uani 1 1 d . . .
H25 H 1.0153 0.3147 0.4993 0.060 Uiso 1 1 calc R . .
C19 C 0.8451(5) -0.1401(5) 0.1548(4) 0.0450(12) Uani 1 1 d . . .
H19 H 0.9004 -0.1875 0.1231 0.054 Uiso 1 1 calc R . .
F4A F 0.3017(18) 0.2540(13) 0.5370(8) 0.069(4) Uani 0.50 1 d PDU A 1
F5A F 0.285(4) 0.440(3) 0.433(2) 0.083(7) Uani 0.50 1 d PDU A 1
F6A F 0.4634(19) 0.3876(17) 0.5146(11) 0.099(6) Uani 0.50 1 d PDU A 1
F4B F 0.259(2) 0.2598(19) 0.4999(12) 0.111(6) Uani 0.50 1 d PDU A 2
F5B F 0.306(4) 0.454(3) 0.437(2) 0.076(7) Uani 0.50 1 d PDU A 2
F6B F 0.4336(17) 0.3254(19) 0.5464(12) 0.112(7) Uani 0.50 1 d PDU A 2
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'
F F 0.0171 0.0103 '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
C1 Pd1 N1 81.19(15) . . ?
C1 Pd1 O4 92.04(14) . . ?
N1 Pd1 O4 173.01(13) . . ?
C1 Pd1 O1 175.26(13) . . ?
N1 Pd1 O1 98.26(12) . . ?
O4 Pd1 O1 88.64(11) . . ?
C1 Pd1 Pd2 108.95(11) . . ?
N1 Pd1 Pd2 94.94(9) . . ?
O4 Pd1 Pd2 85.60(8) . . ?
O1 Pd1 Pd2 75.78(8) . . ?
C16 Pd2 N2 80.89(15) . . ?
C16 Pd2 O2 92.07(14) . . ?
N2 Pd2 O2 172.97(12) . . ?
C16 Pd2 O3 174.94(13) . . ?
N2 Pd2 O3 99.13(12) . . ?
O2 Pd2 O3 87.86(12) . . ?
C16 Pd2 Pd1 110.98(11) . . ?
N2 Pd2 Pd1 98.86(9) . . ?
O2 Pd2 Pd1 83.77(8) . . ?
O3 Pd2 Pd1 74.04(8) . . ?
C14 O2 Pd2 122.2(3) . . ?
C7 N1 C8 119.7(3) . . ?
C7 N1 Pd1 114.0(3) . . ?
C8 N1 Pd1 125.9(2) . . ?
C29 O4 Pd1 120.0(3) . . ?
C29 O3 Pd2 129.7(3) . . ?
C14 O1 Pd1 127.3(3) . . ?
C22 N2 C23 121.5(3) . . ?
C22 N2 Pd2 114.9(3) . . ?
C23 N2 Pd2 123.3(3) . . ?
C17 C16 C21 119.3(4) . . ?
C17 C16 Pd2 127.0(3) . . ?
C21 C16 Pd2 113.6(3) . . ?
C2 C1 C6 118.4(4) . . ?
C2 C1 Pd1 128.2(3) . . ?
C6 C1 Pd1 113.4(3) . . ?
C8 C9 C10 118.9(4) . . ?
N1 C7 C6 117.2(4) . . ?
O1 C14 O2 130.6(4) . . ?
O1 C14 C15 116.4(4) . . ?
O2 C14 C15 113.0(3) . . ?
F1 C15 F2 107.8(4) . . ?
F1 C15 F3 107.1(4) . . ?
F2 C15 F3 107.0(4) . . ?
F1 C15 C14 112.8(4) . . ?
F2 C15 C14 111.5(4) . . ?
F3 C15 C14 110.4(4) . . ?
N2 C22 C21 116.3(4) . . ?
C4 C5 C6 119.4(4) . . ?
C13 C8 C9 121.0(4) . . ?
C13 C8 N1 120.4(4) . . ?
C9 C8 N1 118.6(3) . . ?
C11 C10 C9 120.0(4) . . ?
O3 C29 O4 130.3(4) . . ?
O3 C29 C30 114.7(4) . . ?
O4 C29 C30 114.9(4) . . ?
C5 C6 C1 120.8(4) . . ?
C5 C6 C7 125.4(4) . . ?
C1 C6 C7 113.8(4) . . ?
C8 C13 C12 119.1(4) . . ?
C23 C28 C27 119.9(4) . . ?
C19 C20 C21 120.4(4) . . ?
C28 C23 C24 120.9(4) . . ?
C28 C23 N2 117.9(4) . . ?
C24 C23 N2 121.2(4) . . ?
C12 C11 C10 120.4(4) . . ?
C25 C26 C27 120.3(4) . . ?
C16 C17 C18 119.4(4) . . ?
C19 C18 C17 121.4(4) . . ?
C11 C12 C13 120.5(4) . . ?
C20 C21 C16 119.9(4) . . ?
C20 C21 C22 126.0(4) . . ?
C16 C21 C22 113.9(4) . . ?
C4 C3 C2 121.8(4) . . ?
C26 C27 C28 119.9(5) . . ?
C3 C2 C1 119.6(4) . . ?
C3 C4 C5 119.9(4) . . ?
C23 C24 C25 118.4(4) . . ?
F4A C30 F5B 116.3(19) . . ?
F4A C30 F6B 75.8(10) . . ?
F5B C30 F6B 113.0(16) . . ?
F4A C30 F5A 109.1(19) . . ?
F5B C30 F5A 12(3) . . ?
F6B C30 F5A 122.5(17) . . ?
F4A C30 F4B 29.7(9) . . ?
F5B C30 F4B 103(2) . . ?
F6B C30 F4B 105.4(10) . . ?
F5A C30 F4B 92(2) . . ?
F4A C30 F6A 106.5(10) . . ?
F5B C30 F6A 92.1(19) . . ?
F6B C30 F6A 31.7(11) . . ?
F5A C30 F6A 104.2(18) . . ?
F4B C30 F6A 135.5(9) . . ?
F4A C30 C29 117.2(7) . . ?
F5B C30 C29 114.2(13) . . ?
F6B C30 C29 114.9(8) . . ?
F5A C30 C29 112.4(14) . . ?
F4B C30 C29 105.0(8) . . ?
F6A C30 C29 106.5(8) . . ?
C26 C25 C24 120.6(5) . . ?
C18 C19 C20 119.5(4) . . ?
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 C1 1.948(4) . ?
Pd1 N1 2.029(3) . ?
Pd1 O4 2.050(3) . ?
Pd1 O1 2.175(3) . ?
Pd1 Pd2 3.0005(4) . ?
Pd2 C16 1.957(4) . ?
Pd2 N2 2.021(3) . ?
Pd2 O2 2.055(3) . ?
Pd2 O3 2.165(3) . ?
O2 C14 1.248(5) . ?
N1 C7 1.282(5) . ?
N1 C8 1.439(5) . ?
O4 C29 1.243(5) . ?
O3 C29 1.238(5) . ?
O1 C14 1.226(5) . ?
N2 C22 1.289(5) . ?
N2 C23 1.434(5) . ?
F3 C15 1.332(5) . ?
F2 C15 1.326(5) . ?
F1 C15 1.318(5) . ?
C16 C17 1.384(6) . ?
C16 C21 1.409(6) . ?
C1 C2 1.400(6) . ?
C1 C6 1.415(6) . ?
C9 C8 1.388(6) . ?
C9 C10 1.394(6) . ?
C7 C6 1.427(5) . ?
C14 C15 1.540(6) . ?
C22 C21 1.435(6) . ?
C5 C4 1.389(6) . ?
C5 C6 1.396(6) . ?
C8 C13 1.383(6) . ?
C10 C11 1.382(7) . ?
C29 C30 1.542(6) . ?
C13 C12 1.388(6) . ?
C28 C23 1.369(6) . ?
C28 C27 1.390(6) . ?
C20 C19 1.377(7) . ?
C20 C21 1.394(6) . ?
C23 C24 1.389(6) . ?
C11 C12 1.370(7) . ?
C26 C25 1.366(7) . ?
C26 C27 1.378(7) . ?
C17 C18 1.398(6) . ?
C18 C19 1.375(7) . ?
C3 C4 1.373(7) . ?
C3 C2 1.387(6) . ?
C24 C25 1.402(7) . ?
C30 F4A 1.270(15) . ?
C30 F5B 1.30(3) . ?
C30 F6B 1.279(18) . ?
C30 F5A 1.29(3) . ?
C30 F4B 1.37(2) . ?
C30 F6A 1.376(18) . ?
