#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:01:37 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179737 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/33/7003347.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_7003347
loop_
_publ_author_name
'Singh, Anupam'
'Anandhi, U.'
'Cinellu, Maria Agostina'
'Sharp, Paul R.'
_publ_section_title
;
 Diimine supported group 10 hydroxo, oxo, amido, and imido complexes
;
_journal_issue                   17
_journal_name_full               'Dalton Transactions'
_journal_page_first              2314
_journal_page_last               2327
_journal_paper_doi               10.1039/b715663d
_journal_year                    2008
_chemical_formula_moiety         'C50 H64 N6 Pd2 2+, 2(B F4 1-), 4(C H2 Cl2)'
_chemical_formula_sum            'C54 H72 B2 Cl8 F8 N6 Pd2'
_chemical_formula_weight         1475.20
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 77.461(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.627(4)
_cell_length_b                   24.551(8)
_cell_length_c                   11.490(4)
_cell_measurement_reflns_used    946
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.07
_cell_measurement_theta_min      2.80
_cell_volume                     3201.6(19)
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics
;
L. J. Barbour, X-Seed - Graphical Interface to
SHELX-97 and POV-Ray, 1999
ORTEP (Johnson, 1976), ORTEP 3 for Windows (L. J. Farrugia, 1997)
;
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement
;
SHELXL-97 (Sheldrick, 1997), L. J. Barbour, X-Seed - Graphical Interface to
SHELX-97 and POV-Ray, 1999
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19471
_diffrn_reflns_theta_full        27.17
_diffrn_reflns_theta_max         27.17
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.959
_exptl_absorpt_correction_T_max  0.9102
_exptl_absorpt_correction_T_min  0.6456
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Data were corrected for decay and absorption using the program SADABS
based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995).
;
_exptl_crystal_colour            orange-yellow
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.304
_refine_diff_density_min         -1.272
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         7033
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0412
_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)+(0.0493P)²+5.5886P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1070
_reflns_number_gt                5786
_reflns_number_total             7033
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b715663d.txt
_cod_data_source_block           Pd2(NHtol)2(bpy)2(BF4)2_(12,Ar=tol)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_cell_volume        3201.8(17)
_cod_original_sg_symbol_H-M      'P2(1)/c '
_cod_database_code               7003347
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Pd1 Pd 0.108257(19) 0.034388(9) 0.51337(2) 0.02004(8) Uani 1 1 d . . .
Cl1 Cl -0.47055(11) 0.15508(5) 0.17605(11) 0.0564(3) Uani 1 1 d . . .
F1 F -0.2353(3) 0.21495(14) 0.3952(3) 0.0901(11) Uani 1 1 d . . .
N1 N 0.2529(2) 0.02823(10) 0.5852(2) 0.0213(5) Uani 1 1 d . . .
B1 B -0.2728(4) 0.17232(19) 0.4690(4) 0.0392(10) Uiso 1 1 d . . .
H1 H -0.074(3) 0.0678(17) 0.458(3) 0.034(10) Uiso 1 1 d . . .
Cl2 Cl -0.24388(14) 0.13488(8) 0.01820(19) 0.0991(6) Uani 1 1 d . . .
F2 F -0.3420(3) 0.13800(13) 0.4184(3) 0.0863(11) Uani 1 1 d . . .
N3 N -0.0304(2) 0.03871(10) 0.4292(2) 0.0198(5) Uani 1 1 d . . .
C2 C 0.3229(3) 0.07283(12) 0.5731(3) 0.0210(6) Uani 1 1 d . . .
Cl3 Cl -0.01764(18) 0.26089(7) 0.65753(19) 0.1116(7) Uani 1 1 d . . .
F3 F -0.3402(3) 0.19137(12) 0.5734(2) 0.0700(9) Uani 1 1 d . . .
C3 C 0.4222(3) 0.07458(12) 0.6221(3) 0.0219(6) Uani 1 1 d . . .
H3 H 0.4704 0.1062 0.6121 0.026 Uiso 1 1 calc R . .
Cl4 Cl 0.00574(19) 0.15394(9) 0.74930(18) 0.1146(7) Uani 1 1 d . . .
F4 F -0.1778(2) 0.14193(10) 0.4928(2) 0.0530(6) Uani 1 1 d . . .
C4 C 0.4516(3) 0.03007(13) 0.6862(3) 0.0227(6) Uani 1 1 d . . .
C5 C 0.3819(3) -0.01608(13) 0.6904(3) 0.0264(7) Uani 1 1 d . . .
H5 H 0.4012 -0.0481 0.7285 0.032 Uiso 1 1 calc R . .
C6 C 0.2846(3) -0.01564(13) 0.6397(3) 0.0270(7) Uani 1 1 d . . .
H6 H 0.2383 -0.0478 0.6436 0.032 Uiso 1 1 calc R . .
C7 C 0.5503(3) 0.03293(13) 0.7555(3) 0.0252(6) Uani 1 1 d . . .
C8 C 0.6465(4) 0.07268(19) 0.6996(4) 0.0498(11) Uani 1 1 d . . .
H8A H 0.7092 0.0722 0.7445 0.075 Uiso 1 1 calc R . .
H8B H 0.6134 0.1095 0.7015 0.075 Uiso 1 1 calc R . .
H8C H 0.6790 0.0621 0.6168 0.075 Uiso 1 1 calc R . .
C9 C 0.6045(4) -0.02254(16) 0.7646(4) 0.0458(10) Uani 1 1 d . . .
H9A H 0.6341 -0.0373 0.6844 0.069 Uiso 1 1 calc R . .
H9B H 0.5448 -0.0471 0.8097 0.069 Uiso 1 1 calc R . .
H9C H 0.6698 -0.0191 0.8055 0.069 Uiso 1 1 calc R . .
N2 N 0.1815(2) 0.10922(10) 0.4710(2) 0.0214(5) Uani 1 1 d . . .
C10 C 0.4939(4) 0.0539(2) 0.8808(4) 0.0544(12) Uani 1 1 d . . .
H10A H 0.4353 0.0275 0.9210 0.082 Uiso 1 1 calc R . .
H10B H 0.4555 0.0889 0.8745 0.082 Uiso 1 1 calc R . .
H10C H 0.5550 0.0585 0.9269 0.082 Uiso 1 1 calc R . .
C12 C 0.2833(3) 0.11876(12) 0.5073(3) 0.0213(6) Uani 1 1 d . . .
C13 C 0.3417(3) 0.16827(13) 0.4863(3) 0.0229(6) Uani 1 1 d . . .
H13 H 0.4141 0.1733 0.5104 0.028 Uiso 1 1 calc R . .
C14 C 0.2952(3) 0.21084(13) 0.4299(3) 0.0244(6) Uani 1 1 d . . .
C15 C 0.1889(3) 0.20028(13) 0.3974(3) 0.0293(7) Uani 1 1 d . . .
H15 H 0.1527 0.2280 0.3602 0.035 Uiso 1 1 calc R . .
C16 C 0.1353(3) 0.15005(13) 0.4184(3) 0.0285(7) Uani 1 1 d . . .
H16 H 0.0630 0.1441 0.3948 0.034 Uiso 1 1 calc R . .
C17 C 0.3529(3) 0.26719(13) 0.4096(3) 0.0278(7) Uani 1 1 d . . .
C18 C 0.4810(3) 0.26590(15) 0.4225(4) 0.0353(8) Uani 1 1 d . . .
H18A H 0.4838 0.2553 0.5041 0.053 Uiso 1 1 calc R . .
H18B H 0.5161 0.3021 0.4054 0.053 Uiso 1 1 calc R . .
H18C H 0.5253 0.2394 0.3663 0.053 Uiso 1 1 calc R . .
C19 C 0.2819(3) 0.30582(14) 0.5038(4) 0.0389(9) Uani 1 1 d . . .
H19A H 0.2022 0.3101 0.4898 0.058 Uiso 1 1 calc R . .
H19B H 0.3209 0.3414 0.4981 0.058 Uiso 1 1 calc R . .
H19C H 0.2774 0.2906 0.5835 0.058 Uiso 1 1 calc R . .
C20 C 0.3500(4) 0.28818(16) 0.2845(4) 0.0431(10) Uani 1 1 d . . .
H20A H 0.3904 0.2622 0.2247 0.065 Uiso 1 1 calc R . .
H20B H 0.3898 0.3236 0.2716 0.065 Uiso 1 1 calc R . .
H20C H 0.2680 0.2922 0.2773 0.065 Uiso 1 1 calc R . .
C21 C 0.0092(3) 0.04192(12) 0.3022(3) 0.0216(6) Uani 1 1 d . . .
C22 C 0.0793(3) 0.00016(14) 0.2411(3) 0.0280(7) Uani 1 1 d . . .
H22 H 0.0975 -0.0307 0.2837 0.034 Uiso 1 1 calc R . .
C23 C 0.1221(3) 0.00343(15) 0.1191(3) 0.0333(8) Uani 1 1 d . . .
H23 H 0.1696 -0.0254 0.0794 0.040 Uiso 1 1 calc R . .
C24 C 0.0975(3) 0.04774(16) 0.0529(3) 0.0323(8) Uani 1 1 d . . .
C25 C 0.0254(3) 0.08849(15) 0.1136(3) 0.0320(7) Uani 1 1 d . . .
H25 H 0.0061 0.1189 0.0704 0.038 Uiso 1 1 calc R . .
C26 C -0.0192(3) 0.08570(13) 0.2360(3) 0.0270(7) Uani 1 1 d . . .
H26 H -0.0693 0.1138 0.2749 0.032 Uiso 1 1 calc R . .
C27 C 0.1470(4) 0.0513(2) -0.0794(3) 0.0467(10) Uani 1 1 d . . .
H27A H 0.2235 0.0698 -0.0940 0.070 Uiso 1 1 calc R . .
H27B H 0.0926 0.0718 -0.1170 0.070 Uiso 1 1 calc R . .
H27C H 0.1571 0.0145 -0.1131 0.070 Uiso 1 1 calc R . .
C1S C -0.3247(4) 0.17788(17) 0.1275(4) 0.0493(10) Uani 1 1 d . . .
H1S1 H -0.3251 0.2152 0.0948 0.059 Uiso 1 1 calc R . .
H1S2 H -0.2862 0.1794 0.1963 0.059 Uiso 1 1 calc R . .
C2S C -0.0930(4) 0.20349(19) 0.7206(5) 0.0557(11) Uani 1 1 d . . .
H2S1 H -0.1398 0.1885 0.6657 0.067 Uiso 1 1 calc R . .
H2S2 H -0.1480 0.2136 0.7960 0.067 Uiso 1 1 calc R . .
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'
B B 0.0013 0.0007 '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'
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'
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
N1 Pd1 N2 79.89(10) . . ?
N1 Pd1 N3 98.64(10) . 3_556 ?
N2 Pd1 N3 175.11(10) . 3_556 ?
N1 Pd1 N3 175.83(10) . . ?
N2 Pd1 N3 99.85(10) . . ?
N3 Pd1 N3 81.96(10) 3_556 . ?
N1 Pd1 Pd1 139.49(7) . 3_556 ?
N2 Pd1 Pd1 140.61(7) . 3_556 ?
N3 Pd1 Pd1 41.01(7) 3_556 3_556 ?
N3 Pd1 Pd1 40.96(7) . 3_556 ?
C6 N1 C2 118.7(3) . . ?
C6 N1 Pd1 125.9(2) . . ?
C2 N1 Pd1 115.46(19) . . ?
F1 B1 F3 109.3(4) . . ?
F1 B1 F2 110.2(4) . . ?
F3 B1 F2 107.6(4) . . ?
F1 B1 F4 111.8(4) . . ?
F3 B1 F4 109.6(3) . . ?
F2 B1 F4 108.2(4) . . ?
C21 N3 Pd1 113.38(18) . 3_556 ?
C21 N3 Pd1 111.70(18) . . ?
Pd1 N3 Pd1 98.04(10) 3_556 . ?
N1 C2 C3 121.1(3) . . ?
N1 C2 C12 114.9(3) . . ?
C3 C2 C12 124.0(3) . . ?
C2 C3 C4 120.5(3) . . ?
C5 C4 C3 116.6(3) . . ?
C5 C4 C7 121.1(3) . . ?
C3 C4 C7 122.2(3) . . ?
C6 C5 C4 120.3(3) . . ?
N1 C6 C5 122.5(3) . . ?
C9 C7 C8 109.2(3) . . ?
C9 C7 C4 111.4(3) . . ?
C8 C7 C4 112.1(3) . . ?
C9 C7 C10 109.6(3) . . ?
C8 C7 C10 107.9(3) . . ?
C4 C7 C10 106.7(3) . . ?
C16 N2 C12 118.0(3) . . ?
C16 N2 Pd1 126.4(2) . . ?
C12 N2 Pd1 115.40(19) . . ?
N2 C12 C13 121.6(3) . . ?
N2 C12 C2 114.4(3) . . ?
C13 C12 C2 124.0(3) . . ?
C12 C13 C14 120.8(3) . . ?
C15 C14 C13 116.1(3) . . ?
C15 C14 C17 120.8(3) . . ?
C13 C14 C17 123.0(3) . . ?
C16 C15 C14 120.9(3) . . ?
N2 C16 C15 122.5(3) . . ?
C18 C17 C14 111.7(3) . . ?
C18 C17 C20 108.5(3) . . ?
C14 C17 C20 110.3(3) . . ?
C18 C17 C19 109.3(3) . . ?
C14 C17 C19 107.4(3) . . ?
C20 C17 C19 109.5(3) . . ?
C26 C21 C22 118.1(3) . . ?
C26 C21 N3 122.3(3) . . ?
C22 C21 N3 119.6(3) . . ?
C23 C22 C21 120.5(3) . . ?
C22 C23 C24 121.8(3) . . ?
C25 C24 C23 117.5(3) . . ?
C25 C24 C27 121.4(3) . . ?
C23 C24 C27 121.1(4) . . ?
C26 C25 C24 121.5(3) . . ?
C25 C26 C21 120.5(3) . . ?
Cl2 C1S Cl1 111.5(2) . . ?
Cl3 C2S Cl4 110.5(3) . . ?
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 N1 2.034(3) . ?
Pd1 N2 2.039(3) . ?
Pd1 N3 2.053(3) 3_556 ?
Pd1 N3 2.055(2) . ?
Pd1 Pd1 3.1015(8) 3_556 ?
Cl1 C1S 1.758(5) . ?
F1 B1 1.358(5) . ?
N1 C6 1.337(4) . ?
N1 C2 1.353(4) . ?
B1 F3 1.365(5) . ?
B1 F2 1.378(5) . ?
B1 F4 1.407(5) . ?
Cl2 C1S 1.750(5) . ?
N3 C21 1.434(4) . ?
N3 Pd1 2.053(3) 3_556 ?
C2 C3 1.390(4) . ?
C2 C12 1.485(4) . ?
Cl3 C2S 1.733(5) . ?
C3 C4 1.401(4) . ?
Cl4 C2S 1.752(5) . ?
C4 C5 1.388(4) . ?
C4 C7 1.534(4) . ?
C5 C6 1.381(4) . ?
C7 C9 1.514(5) . ?
C7 C8 1.518(5) . ?
C7 C10 1.536(5) . ?
N2 C16 1.341(4) . ?
N2 C12 1.358(4) . ?
C12 C13 1.387(4) . ?
C13 C14 1.398(4) . ?
C14 C15 1.391(4) . ?
C14 C17 1.533(4) . ?
C15 C16 1.379(5) . ?
C17 C18 1.529(5) . ?
C17 C20 1.535(5) . ?
C17 C19 1.537(5) . ?
C21 C26 1.397(4) . ?
C21 C22 1.399(4) . ?
C22 C23 1.385(5) . ?
C23 C24 1.392(5) . ?
C24 C25 1.392(5) . ?
C24 C27 1.506(5) . ?
C25 C26 1.391(5) . ?
