#------------------------------------------------------------------------------
#$Date: 2016-03-22 14:10:13 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178986 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/09/4120985.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_4120985
loop_
_publ_author_name
'Sibo Lin'
'David E. Herbert'
'Alexandra Velian'
'Michael W. Day'
'Theodor Agapie'
_publ_section_title
;
 Dipalladium(I) Terphenyl Diphosphine Complexes as Models for Two-Site
 Adsorption and Activation of Organic Molecules
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15830
_journal_page_last               15840
_journal_paper_doi               10.1021/ja406696k
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C35 H46 B2 F8 P2 Pd2 S'
_chemical_formula_weight         947.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.950(4)
_cell_length_b                   15.271(3)
_cell_length_c                   13.363(3)
_cell_measurement_reflns_used    29607
_cell_measurement_temperature    100
_cell_volume                     3663.0(14)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'BluIce (SSRL, 2001)'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'pixel array detector'
_diffrn_detector_area_resol_mean 5.814
_diffrn_detector_type            'DECTIRS PILATUS 6M'
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device       'single φ axis'
_diffrn_measurement_device_details
;
         custom air bearing single axis goniometer
;
_diffrn_measurement_device_type  'SSRL single-axis microdiffractometer'
_diffrn_measurement_method       'fine sliced shutterless φ scans'
_diffrn_radiation_collimation    'K-B focussing mirrors'
_diffrn_radiation_monochromator  'liquid nitrogen-cooled double Si(111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.72930
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0136
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29607
_diffrn_reflns_theta_full        31.37
_diffrn_reflns_theta_max         31.37
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.193
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_description       prism
_exptl_crystal_F_000             1904
_refine_diff_density_max         2.842
_refine_diff_density_min         -1.971
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         5551
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0422P)²+5.9760P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0883
_reflns_number_gt                5465
_reflns_number_total             5551
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja406696k_08.cif
_cod_data_source_block           sl5062a
_cod_original_cell_volume        3663.0(13)
_cod_database_code               4120985
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, 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_group
Pd1 Pd 0.673052(9) 0.661338(10) 0.736066(11) 0.02129(6) Uani 1 1 d . .
P1 P 0.66168(3) 0.51124(3) 0.74303(4) 0.01672(9) Uani 1 1 d . .
F7 F 0.55053(11) 0.2500 0.75615(15) 0.0303(4) Uani 1 2 d S .
F6 F 0.48386(12) 0.2500 0.90161(15) 0.0354(4) Uani 1 2 d S .
C8 C 0.63441(9) 0.65585(11) 0.88949(14) 0.0161(3) Uani 1 1 d . .
F4 F 0.44245(13) 0.32524(15) 0.76717(15) 0.0602(6) Uani 1 1 d . .
C1 C 0.61089(10) 0.40827(12) 0.90694(15) 0.0212(3) Uani 1 1 d . .
H1 H 0.6122 0.3593 0.8655 0.025 Uiso 1 1 calc R .
C9 C 0.69968(10) 0.70428(12) 0.91374(15) 0.0200(3) Uani 1 1 d . .
H9 H 0.7400 0.6740 0.9490 0.024 Uiso 1 1 calc R .
C6 C 0.59142(11) 0.39961(13) 1.00700(15) 0.0226(4) Uani 1 1 d . .
H6 H 0.5802 0.3446 1.0329 0.027 Uiso 1 1 calc R .
C3 C 0.62296(9) 0.56507(12) 0.92980(13) 0.0168(3) Uani 1 1 d . .
C10 C 0.59684(10) 0.45327(13) 0.65991(14) 0.0217(3) Uani 1 1 d . .
H10 H 0.5891 0.3943 0.6869 0.026 Uiso 1 1 calc R .
C4 C 0.60314(10) 0.55584(13) 1.03037(14) 0.0203(3) Uani 1 1 d . .
H4 H 0.5997 0.6048 1.0715 0.024 Uiso 1 1 calc R .
C2 C 0.62849(9) 0.49114(12) 0.86872(13) 0.0177(3) Uani 1 1 d . .
C7 C 0.57160(9) 0.70463(12) 0.85363(13) 0.0173(3) Uani 1 1 d . .
H7 H 0.5236 0.6744 0.8483 0.021 Uiso 1 1 calc R .
C13 C 0.75288(11) 0.45716(14) 0.73206(15) 0.0238(4) Uani 1 1 d . .
H13 H 0.7724 0.4707 0.6653 0.029 Uiso 1 1 calc R .
C14 C 0.75048(14) 0.35768(17) 0.7415(2) 0.0375(5) Uani 1 1 d . .
H14A H 0.7353 0.3420 0.8079 0.056 Uiso 1 1 calc R .
H14B H 0.7991 0.3341 0.7284 0.056 Uiso 1 1 calc R .
H14C H 0.7156 0.3344 0.6940 0.056 Uiso 1 1 calc R .
C5 C 0.58860(10) 0.47270(13) 1.06848(14) 0.0221(3) Uani 1 1 d . .
H5 H 0.5769 0.4661 1.1359 0.027 Uiso 1 1 calc R .
C11 C 0.62703(13) 0.44419(19) 0.55376(17) 0.0356(5) Uani 1 1 d . .
H11A H 0.6322 0.5012 0.5243 0.053 Uiso 1 1 calc R .
H11B H 0.5932 0.4097 0.5145 0.053 Uiso 1 1 calc R .
H11C H 0.6748 0.4159 0.5557 0.053 Uiso 1 1 calc R .
C12 C 0.52195(12) 0.5007(2) 0.66062(18) 0.0380(5) Uani 1 1 d . .
H12A H 0.5026 0.5019 0.7276 0.057 Uiso 1 1 calc R .
H12B H 0.4876 0.4704 0.6177 0.057 Uiso 1 1 calc R .
H12C H 0.5285 0.5595 0.6370 0.057 Uiso 1 1 calc R .
C15 C 0.80687(12) 0.49628(17) 0.80780(19) 0.0329(5) Uani 1 1 d . .
H15A H 0.8116 0.5581 0.7961 0.049 Uiso 1 1 calc R .
H15B H 0.8547 0.4689 0.8008 0.049 Uiso 1 1 calc R .
H15C H 0.7883 0.4865 0.8743 0.049 Uiso 1 1 calc R .
F3 F 0.63565(12) 0.2500 0.38989(19) 0.0509(6) Uani 1 2 d S .
S1 S 0.71222(12) 0.82109(10) 0.57479(15) 0.0233(3) Uani 0.50 1 d P -1
C17 C 0.7186(5) 0.6501(5) 0.5800(7) 0.0278(15) Uani 0.50 1 d P -1
H17 H 0.7483 0.5988 0.5614 0.033 Uiso 0.50 1 calc PR -1
C18 C 0.7547(2) 0.7261(3) 0.6176(3) 0.0266(8) Uani 0.50 1 d P -1
H18 H 0.8086 0.7253 0.6294 0.032 Uiso 0.50 1 calc PR -1
C19 C 0.6543(3) 0.6761(3) 0.5171(3) 0.0288(8) Uani 0.50 1 d P -1
H19 H 0.6243 0.6352 0.4848 0.035 Uiso 0.50 1 calc PR -1
C20 C 0.5802(3) 0.8093(3) 0.4586(4) 0.0347(10) Uani 0.50 1 d P -1
H20A H 0.5502 0.8392 0.5073 0.052 Uiso 0.50 1 calc PR -1
H20B H 0.5502 0.7675 0.4233 0.052 Uiso 0.50 1 calc PR -1
H20C H 0.6002 0.8510 0.4121 0.052 Uiso 0.50 1 calc PR -1
C21 C 0.6422(2) 0.7633(5) 0.5099(3) 0.024(2) Uani 0.50 1 d P -1
B2 B 0.58478(18) 0.2500 0.3132(3) 0.0254(6) Uani 1 2 d S .
F1 F 0.59469(14) 0.32225(14) 0.25230(17) 0.0620(6) Uani 1 1 d . .
F2 F 0.51296(12) 0.2500 0.34872(19) 0.0556(7) Uani 1 2 d S .
B1 B 0.47900(19) 0.2500 0.7981(3) 0.0275(6) Uani 1 2 d S .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0037 0.0017 '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'
B B 0.0016 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0190 0.0109 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1089 0.1019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1294 0.1310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9286 1.0622 '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
C8 Pd1 C17 172.86(17) . .
C8 Pd1 S1 175.42(6) . 8_575
C17 Pd1 S1 11.62(15) . 8_575
C8 Pd1 P1 83.96(5) . .
C17 Pd1 P1 89.64(18) . .
S1 Pd1 P1 100.51(4) 8_575 .
C8 Pd1 C18 147.71(11) . .
C17 Pd1 C18 35.7(2) . .
S1 Pd1 C18 29.66(12) 8_575 .
P1 Pd1 C18 119.75(9) . .
C8 Pd1 C7 34.94(6) . .
C17 Pd1 C7 150.5(2) . .
S1 Pd1 C7 142.03(6) 8_575 .
P1 Pd1 C7 100.00(4) . .
C18 Pd1 C7 139.53(10) . .
C8 Pd1 C9 34.46(6) . .
C17 Pd1 C9 146.0(3) . .
S1 Pd1 C9 143.51(7) 8_575 .
P1 Pd1 C9 103.81(4) . .
C18 Pd1 C9 113.87(11) . .
C7 Pd1 C9 58.25(6) . .
C8 Pd1 Pd1 92.22(5) . 8_575
C17 Pd1 Pd1 94.39(18) . 8_575
S1 Pd1 Pd1 83.25(4) 8_575 8_575
P1 Pd1 Pd1 174.409(13) . 8_575
C18 Pd1 Pd1 65.39(9) . 8_575
C7 Pd1 Pd1 74.63(4) . 8_575
C9 Pd1 Pd1 74.85(4) . 8_575
C2 P1 C10 105.74(9) . .
C2 P1 C13 106.92(9) . .
C10 P1 C13 107.42(9) . .
C2 P1 Pd1 103.63(6) . .
C10 P1 Pd1 120.77(7) . .
C13 P1 Pd1 111.39(7) . .
C9 C8 C7 116.97(15) . .
C9 C8 C3 120.73(16) . .
C7 C8 C3 119.47(15) . .
C9 C8 Pd1 86.09(12) . .
C7 C8 Pd1 85.14(11) . .
C3 C8 Pd1 114.78(12) . .
C6 C1 C2 119.60(18) . .
C9 C9 C8 121.32(10) 8_575 .
C9 C9 Pd1 105.15(4) 8_575 .
C8 C9 Pd1 59.46(10) . .
C5 C6 C1 120.20(18) . .
C2 C3 C4 119.91(17) . .
C2 C3 C8 121.80(16) . .
C4 C3 C8 118.23(16) . .
C11 C10 C12 111.21(18) . .
C11 C10 P1 112.41(14) . .
C12 C10 P1 109.00(15) . .
C5 C4 C3 119.43(18) . .
C3 C2 C1 120.08(17) . .
C3 C2 P1 115.41(13) . .
C1 C2 P1 124.49(14) . .
C7 C7 C8 121.30(10) 8_575 .
C7 C7 Pd1 105.37(4) 8_575 .
C8 C7 Pd1 59.92(10) . .
C15 C13 C14 110.73(19) . .
C15 C13 P1 109.70(15) . .
C14 C13 P1 114.55(16) . .
C6 C5 C4 120.69(17) . .
C18 S1 C21 93.3(3) . .
C18 S1 Pd1 85.56(15) . 8_575
C21 S1 Pd1 107.70(15) . 8_575
C18 C17 C19 109.7(5) . .
C18 C17 Pd1 77.0(4) . .
C19 C17 Pd1 102.9(5) . .
C17 C18 S1 111.4(4) . .
C17 C18 Pd1 67.3(4) . .
S1 C18 Pd1 107.2(2) . .
C21 C19 C17 115.4(5) . .
C19 C21 C20 128.2(5) . .
C19 C21 S1 110.1(4) . .
C20 C21 S1 121.7(5) . .
F3 B2 F2 111.5(3) . .
F3 B2 F1 110.73(19) . 8_565
F2 B2 F1 108.9(2) . 8_565
F3 B2 F1 110.73(19) . .
F2 B2 F1 108.9(2) . .
F1 B2 F1 105.9(3) 8_565 .
F6 B1 F4 109.13(19) . 8_565
F6 B1 F4 109.13(19) . .
F4 B1 F4 112.0(3) 8_565 .
F6 B1 F7 110.0(3) . .
F4 B1 F7 108.31(19) 8_565 .
F4 B1 F7 108.3(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 C8 2.1660(19) .
Pd1 C17 2.247(9) .
Pd1 S1 2.283(2) 8_575
Pd1 P1 2.3031(7) .
Pd1 C18 2.373(4) .
Pd1 C7 2.4942(18) .
Pd1 C9 2.509(2) .
Pd1 Pd1 2.7079(6) 8_575
P1 C2 1.8083(19) .
P1 C10 1.8363(19) .
P1 C13 1.840(2) .
F7 B1 1.401(4) .
F6 B1 1.385(4) .
C8 C9 1.423(2) .
C8 C7 1.434(2) .
C8 C3 1.501(2) .
F4 B1 1.386(3) .
C1 C6 1.388(3) .
C1 C2 1.401(3) .
C9 C9 1.396(4) 8_575
C6 C5 1.387(3) .
C3 C2 1.397(2) .
C3 C4 1.397(2) .
C10 C11 1.525(3) .
C10 C12 1.527(3) .
C4 C5 1.393(3) .
C7 C7 1.386(4) 8_575
C13 C15 1.523(3) .
C13 C14 1.525(4) .
F3 B2 1.372(4) .
S1 C18 1.736(4) .
S1 C21 1.763(5) .
S1 Pd1 2.283(2) 8_575
C17 C18 1.421(10) .
C17 C19 1.481(10) .
C19 C21 1.354(7) .
C20 C21 1.484(7) .
B2 F2 1.374(4) .
B2 F1 1.383(3) 8_565
B2 F1 1.383(3) .
B1 F4 1.386(3) 8_565
