#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:01:37 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179737 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/33/7003346.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_7003346
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         'C48 H60 N6 Pd2 2+, 2(B F4 1-), 4(C4 H8 O)'
_chemical_formula_sum            'C64 H92 B2 F8 N6 O4 Pd2'
_chemical_formula_weight         1395.86
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.2730(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.4761(8)
_cell_length_b                   11.1520(5)
_cell_length_c                   18.0618(8)
_cell_measurement_reflns_used    7740
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.06
_cell_measurement_theta_min      2.31
_cell_volume                     3322.8(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0457
_diffrn_reflns_av_sigmaI/netI    0.0532
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23148
_diffrn_reflns_theta_full        27.13
_diffrn_reflns_theta_max         27.13
_diffrn_reflns_theta_min         1.41
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_T_max  0.9700
_exptl_absorpt_correction_T_min  0.8618
_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            YELLOW
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         7335
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0380
_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)+(0.0431P)²+2.3700P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.0968
_reflns_number_gt                5355
_reflns_number_total             7335
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b715663d.txt
_cod_data_source_block           Pd2(NHPh)2(bpy)2(BF4)2_(12,Ar=Ph)
_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_sg_symbol_H-M      'P2(1)/n '
_cod_database_code               7003346
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
Pd1 Pd 0.451127(13) 0.02220(2) 0.412065(12) 0.01900(8) Uani 1 1 d . . .
F1 F 0.60453(12) 0.2816(2) 0.45299(13) 0.0510(6) Uani 1 1 d . . .
O1 O 0.72464(18) 0.1184(3) 0.2208(2) 0.0672(9) Uani 1 1 d . . .
N1 N 0.33611(15) 0.0075(2) 0.33736(14) 0.0229(6) Uani 1 1 d . . .
C6 C 0.27474(19) -0.0457(3) 0.35294(18) 0.0294(8) Uani 1 1 d . . .
H6 H 0.2842 -0.0779 0.4039 0.035 Uiso 1 1 calc R . .
B1 B 0.6836(3) 0.3241(4) 0.4693(2) 0.0367(10) Uani 1 1 d . . .
F2 F 0.72785(13) 0.2816(2) 0.54448(12) 0.0520(6) Uani 1 1 d . . .
O2 O 0.0970(3) 0.3182(4) 0.2691(3) 0.1152(16) Uani 1 1 d . . .
N2 N 0.46571(14) 0.0852(2) 0.31124(13) 0.0221(5) Uani 1 1 d . . .
C5 C 0.19834(19) -0.0560(3) 0.29861(18) 0.0285(7) Uani 1 1 d . . .
H5 H 0.1570 -0.0965 0.3122 0.034 Uiso 1 1 calc R . .
F3 F 0.68456(18) 0.4457(2) 0.46904(18) 0.0756(8) Uani 1 1 d . . .
N3 N 0.56858(15) 0.0258(3) 0.48599(14) 0.0204(5) Uani 1 1 d . . .
C4 C 0.18134(17) -0.0075(3) 0.22415(17) 0.0233(7) Uani 1 1 d . . .
F4 F 0.71626(16) 0.2763(2) 0.41608(13) 0.0596(7) Uani 1 1 d . . .
C3 C 0.24612(18) 0.0463(3) 0.20763(17) 0.0237(7) Uani 1 1 d . . .
H3 H 0.2377 0.0802 0.1573 0.028 Uiso 1 1 calc R . .
C2 C 0.32247(18) 0.0507(3) 0.26368(17) 0.0213(7) Uani 1 1 d . . .
C7 C 0.39550(17) 0.0965(3) 0.24906(17) 0.0221(7) Uani 1 1 d . . .
C8 C 0.39551(18) 0.1400(3) 0.17732(17) 0.0247(7) Uani 1 1 d . . .
H8 H 0.3456 0.1481 0.1356 0.030 Uiso 1 1 calc R . .
C9 C 0.46780(18) 0.1723(3) 0.16545(17) 0.0252(7) Uani 1 1 d . . .
C10 C 0.53831(19) 0.1606(3) 0.22952(18) 0.0280(7) Uani 1 1 d . . .
H10 H 0.5891 0.1814 0.2245 0.034 Uiso 1 1 calc R . .
C11 C 0.53502(18) 0.1189(3) 0.30066(17) 0.0248(7) Uani 1 1 d . . .
H11 H 0.5840 0.1139 0.3438 0.030 Uiso 1 1 calc R . .
C12 C 0.09813(18) -0.0183(3) 0.16142(18) 0.0281(7) Uani 1 1 d . . .
C13 C 0.03295(19) -0.0561(4) 0.1968(2) 0.0396(9) Uani 1 1 d . . .
H13A H 0.0465 -0.1352 0.2213 0.059 Uiso 1 1 calc R . .
H13B H -0.0199 -0.0598 0.1552 0.059 Uiso 1 1 calc R . .
H13C H 0.0307 0.0026 0.2364 0.059 Uiso 1 1 calc R . .
C14 C 0.1039(2) -0.1144(4) 0.1024(2) 0.0454(10) Uani 1 1 d . . .
H14A H 0.1433 -0.0891 0.0775 0.068 Uiso 1 1 calc R . .
H14B H 0.0506 -0.1249 0.0622 0.068 Uiso 1 1 calc R . .
H14C H 0.1213 -0.1906 0.1299 0.068 Uiso 1 1 calc R . .
C15 C 0.0730(2) 0.1029(4) 0.1192(2) 0.0420(9) Uani 1 1 d . . .
H15A H 0.0745 0.1653 0.1579 0.063 Uiso 1 1 calc R . .
H15B H 0.0179 0.0966 0.0817 0.063 Uiso 1 1 calc R . .
H15C H 0.1105 0.1238 0.0912 0.063 Uiso 1 1 calc R . .
C16 C 0.46675(19) 0.2173(3) 0.08513(18) 0.0316(8) Uani 1 1 d . . .
C18 C 0.4237(2) 0.1249(4) 0.0225(2) 0.0414(9) Uani 1 1 d . . .
H18A H 0.4523 0.0481 0.0346 0.062 Uiso 1 1 calc R . .
H18B H 0.4234 0.1530 -0.0290 0.062 Uiso 1 1 calc R . .
H18C H 0.3678 0.1145 0.0218 0.062 Uiso 1 1 calc R . .
C17 C 0.5525(2) 0.2383(5) 0.0823(2) 0.0539(12) Uani 1 1 d . . .
H17A H 0.5799 0.2991 0.1212 0.081 Uiso 1 1 calc R . .
H17B H 0.5492 0.2662 0.0299 0.081 Uiso 1 1 calc R . .
H17C H 0.5832 0.1632 0.0940 0.081 Uiso 1 1 calc R . .
C19 C 0.4204(2) 0.3362(4) 0.0668(2) 0.0463(10) Uani 1 1 d . . .
H19A H 0.3657 0.3249 0.0692 0.069 Uiso 1 1 calc R . .
H19B H 0.4169 0.3630 0.0142 0.069 Uiso 1 1 calc R . .
H19C H 0.4490 0.3967 0.1054 0.069 Uiso 1 1 calc R . .
C20 C 0.62053(17) -0.0553(3) 0.46389(16) 0.0227(7) Uani 1 1 d . . .
C21 C 0.5999(2) -0.1759(3) 0.45322(18) 0.0287(7) Uani 1 1 d . . .
H21 H 0.5517 -0.2033 0.4612 0.034 Uiso 1 1 calc R . .
C22 C 0.6485(2) -0.2565(3) 0.4311(2) 0.0383(9) Uani 1 1 d . . .
H22 H 0.6337 -0.3387 0.4240 0.046 Uiso 1 1 calc R . .
C23 C 0.7189(2) -0.2173(4) 0.4193(2) 0.0438(10) Uani 1 1 d . . .
H23 H 0.7523 -0.2724 0.4040 0.053 Uiso 1 1 calc R . .
C24 C 0.7402(2) -0.0976(4) 0.4298(2) 0.0393(9) Uani 1 1 d . . .
H24 H 0.7884 -0.0706 0.4217 0.047 Uiso 1 1 calc R . .
C25 C 0.69146(19) -0.0163(3) 0.45211(18) 0.0302(7) Uani 1 1 d . . .
H25 H 0.7065 0.0659 0.4593 0.036 Uiso 1 1 calc R . .
C26 C 0.7997(3) 0.1425(5) 0.2801(3) 0.0731(14) Uani 1 1 d . . .
H26A H 0.7921 0.1474 0.3319 0.088 Uiso 1 1 calc R . .
H26B H 0.8219 0.2199 0.2696 0.088 Uiso 1 1 calc R . .
C27 C 0.8556(3) 0.0445(4) 0.2795(4) 0.0794(17) Uani 1 1 d . . .
H27A H 0.8897 0.0234 0.3336 0.095 Uiso 1 1 calc R . .
H27B H 0.8914 0.0673 0.2492 0.095 Uiso 1 1 calc R . .
C28 C 0.8022(4) -0.0575(5) 0.2415(3) 0.0817(17) Uani 1 1 d . . .
H28A H 0.7955 -0.1135 0.2815 0.098 Uiso 1 1 calc R . .
H28B H 0.8253 -0.1020 0.2064 0.098 Uiso 1 1 calc R . .
C29 C 0.7230(4) -0.0018(4) 0.1958(4) 0.094(2) Uani 1 1 d . . .
H29A H 0.7151 -0.0049 0.1390 0.113 Uiso 1 1 calc R . .
H29B H 0.6779 -0.0456 0.2054 0.113 Uiso 1 1 calc R . .
C30 C 0.0187(4) 0.3054(6) 0.2777(4) 0.100(2) Uani 1 1 d . . .
H30A H -0.0138 0.3789 0.2594 0.120 Uiso 1 1 calc R . .
H30B H -0.0106 0.2369 0.2461 0.120 Uiso 1 1 calc R . .
C31 C 0.0295(4) 0.2869(9) 0.3535(3) 0.127(3) Uani 1 1 d . . .
H31A H -0.0087 0.2252 0.3596 0.153 Uiso 1 1 calc R . .
H31B H 0.0201 0.3620 0.3785 0.153 Uiso 1 1 calc R . .
C32 C 0.1139(5) 0.2462(13) 0.3901(4) 0.237(7) Uani 1 1 d . . .
H32A H 0.1370 0.2822 0.4430 0.285 Uiso 1 1 calc R . .
H32B H 0.1151 0.1579 0.3960 0.285 Uiso 1 1 calc R . .
C33 C 0.1599(4) 0.2796(6) 0.3442(4) 0.098(2) Uani 1 1 d . . .
H33A H 0.1921 0.2113 0.3354 0.118 Uiso 1 1 calc R . .
H33B H 0.1970 0.3465 0.3685 0.118 Uiso 1 1 calc R . .
H1 H 0.5843(19) 0.093(3) 0.4872(18) 0.019(9) 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'
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'
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
N1 Pd1 N2 79.77(9) . . ?
N1 Pd1 N3 176.29(11) . . ?
N2 Pd1 N3 100.45(10) . . ?
N1 Pd1 N3 98.81(10) . 3_656 ?
N2 Pd1 N3 174.58(11) . 3_656 ?
N3 Pd1 N3 81.31(11) . 3_656 ?
N1 Pd1 Pd1 139.27(7) . 3_656 ?
N2 Pd1 Pd1 140.94(7) . 3_656 ?
N3 Pd1 Pd1 40.73(7) . 3_656 ?
N3 Pd1 Pd1 40.58(7) 3_656 3_656 ?
C29 O1 C26 109.7(4) . . ?
C6 N1 C2 118.1(3) . . ?
C6 N1 Pd1 125.9(2) . . ?
C2 N1 Pd1 115.98(19) . . ?
N1 C6 C5 123.0(3) . . ?
F3 B1 F4 112.1(3) . . ?
F3 B1 F1 110.6(3) . . ?
F4 B1 F1 109.3(3) . . ?
F3 B1 F2 109.7(3) . . ?
F4 B1 F2 108.7(3) . . ?
F1 B1 F2 106.2(3) . . ?
C30 O2 C33 108.3(5) . . ?
C11 N2 C7 117.7(2) . . ?
C11 N2 Pd1 127.4(2) . . ?
C7 N2 Pd1 114.89(19) . . ?
C6 C5 C4 120.4(3) . . ?
C20 N3 Pd1 113.49(19) . . ?
C20 N3 Pd1 113.3(2) . 3_656 ?
Pd1 N3 Pd1 98.69(11) . 3_656 ?
C5 C4 C3 116.4(3) . . ?
C5 C4 C12 122.4(3) . . ?
C3 C4 C12 121.1(3) . . ?
C2 C3 C4 120.8(3) . . ?
N1 C2 C3 121.2(3) . . ?
N1 C2 C7 114.5(2) . . ?
C3 C2 C7 124.3(3) . . ?
N2 C7 C8 121.6(3) . . ?
N2 C7 C2 114.5(2) . . ?
C8 C7 C2 123.8(3) . . ?
C7 C8 C9 120.9(3) . . ?
C10 C9 C8 116.5(3) . . ?
C10 C9 C16 123.4(3) . . ?
C8 C9 C16 120.1(3) . . ?
C11 C10 C9 120.4(3) . . ?
N2 C11 C10 122.8(3) . . ?
C4 C12 C13 111.6(3) . . ?
C4 C12 C14 107.8(3) . . ?
C13 C12 C14 108.9(3) . . ?
C4 C12 C15 110.1(3) . . ?
C13 C12 C15 108.4(3) . . ?
C14 C12 C15 109.9(3) . . ?
C9 C16 C19 109.2(3) . . ?
C9 C16 C18 109.2(3) . . ?
C19 C16 C18 109.1(3) . . ?
C9 C16 C17 112.1(3) . . ?
C19 C16 C17 108.2(3) . . ?
C18 C16 C17 109.0(3) . . ?
C21 C20 C25 119.0(3) . . ?
C21 C20 N3 119.4(3) . . ?
C25 C20 N3 121.6(3) . . ?
C22 C21 C20 120.9(3) . . ?
C21 C22 C23 120.0(4) . . ?
C24 C23 C22 119.7(3) . . ?
C23 C24 C25 120.4(3) . . ?
C24 C25 C20 120.0(3) . . ?
O1 C26 C27 107.8(4) . . ?
C26 C27 C28 104.8(4) . . ?
C27 C28 C29 105.3(4) . . ?
O1 C29 C28 107.5(5) . . ?
C31 C30 O2 108.0(6) . . ?
C30 C31 C32 106.9(5) . . ?
C33 C32 C31 110.0(6) . . ?
C32 C33 O2 102.8(5) . . ?
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 2.024(2) . ?
Pd1 N2 2.045(2) . ?
Pd1 N3 2.047(2) . ?
Pd1 N3 2.053(2) 3_656 ?
Pd1 Pd1 3.1099(4) 3_656 ?
F1 B1 1.397(5) . ?
O1 C29 1.412(5) . ?
O1 C26 1.418(5) . ?
N1 C6 1.334(4) . ?
N1 C2 1.361(4) . ?
C6 C5 1.376(4) . ?
B1 F3 1.356(5) . ?
B1 F4 1.377(5) . ?
B1 F2 1.406(5) . ?
O2 C30 1.434(7) . ?
O2 C33 1.500(7) . ?
N2 C11 1.341(4) . ?
N2 C7 1.369(4) . ?
C5 C4 1.388(4) . ?
N3 C20 1.428(4) . ?
N3 Pd1 2.053(2) 3_656 ?
C4 C3 1.397(4) . ?
C4 C12 1.525(4) . ?
C3 C2 1.384(4) . ?
C2 C7 1.477(4) . ?
C7 C8 1.384(4) . ?
C8 C9 1.397(4) . ?
C9 C10 1.390(4) . ?
C9 C16 1.529(4) . ?
C10 C11 1.386(4) . ?
C12 C13 1.538(4) . ?
C12 C14 1.538(5) . ?
C12 C15 1.543(5) . ?
C16 C19 1.531(5) . ?
C16 C18 1.532(5) . ?
C16 C17 1.534(4) . ?
C20 C21 1.389(5) . ?
C20 C25 1.395(4) . ?
C21 C22 1.384(5) . ?
C22 C23 1.387(5) . ?
C23 C24 1.382(6) . ?
C24 C25 1.391(5) . ?
C26 C27 1.468(6) . ?
C27 C28 1.487(7) . ?
C28 C29 1.493(8) . ?
C30 C31 1.335(8) . ?
C31 C32 1.474(9) . ?
C32 C33 1.384(9) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H1 F1 0.80(3) 2.25(3) 3.022(4) 163(3) .
