#------------------------------------------------------------------------------
#$Date: 2016-03-21 09:18:06 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178621 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/32/4073298.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_4073298
loop_
_publ_author_name
'Chernyshova, Eleonora S.'
'Goddard, Richard'
'Pörschke, Klaus-Richard'
_publ_section_title
;
 Mononuclear NHC−Pd−π-Allyl Complexes Containing Weakly
 Coordinating Ligands
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3236
_journal_paper_doi               10.1021/om0702274
_journal_volume                  26
_journal_year                    2007
_chemical_absolute_configuration ad
_chemical_compound_source        tetrahydrofuran
_chemical_formula_moiety         'C18 H33 N2 O Pd 1+, B F4 1-'
_chemical_formula_sum            'C18 H33 B F4 N2 O Pd'
_chemical_formula_weight         486.67
_chemical_melting_point          ?
_chemical_name_systematic
; 
 (η³-allyl)-(tetrahydrofuran-O)-(1,3-bis(tert-butyl)-
 imidazol-2-ylidine)-palladium(ii) tetrafluoroborate
 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   10.2875(2)
_cell_length_b                   12.6052(3)
_cell_length_c                   16.3796(3)
_cell_measurement_reflns_used    37537
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.14
_cell_measurement_theta_min      2.91
_cell_volume                     2124.04(8)
_computing_cell_refinement       'Denzo / Scalepack (Otwinowski 1997)'
_computing_data_collection       'Collect software (Nonius, 1998)'
_computing_data_reduction        'Denzo / Scalepack (Otwinowski 1997)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD ω-scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         '0.3 mm focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            39642
_diffrn_reflns_theta_full        33.13
_diffrn_reflns_theta_max         33.13
_diffrn_reflns_theta_min         3.18
_diffrn_standards_decay_%        0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.917
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9038
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scalepack, Otwinowski (1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.895
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.019(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         8073
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0211P)²+1.5227P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0604
_reflns_number_gt                7725
_reflns_number_total             8073
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            om0702274si20070309_074405.cif
_cod_data_source_block           9a(BF4)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4073298
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -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_assembly
_atom_site_disorder_group
C1 C 0.0730(2) 0.59738(19) 1.01945(14) 0.0287(4) Uani 1 1 d . A 1
H1A H 0.0700 0.5769 1.0765 0.034 Uiso 1 1 calc R A 1
H1B H 0.1048 0.6690 1.0110 0.034 Uiso 1 1 calc R A 1
C2A C -0.0355(3) 0.5651(3) 0.9699(3) 0.0298(9) Uani 0.629(7) 1 d P A 1
H2A H -0.1050 0.5244 0.9962 0.036 Uiso 0.629(7) 1 calc PR A 1
C2B C 0.0284(5) 0.6287(4) 0.9377(4) 0.0279(14) Uani 0.371(7) 1 d P A 2
C3 C -0.0330(3) 0.5672(3) 0.8914(2) 0.0521(9) Uani 1 1 d . A 1
H3A H -0.0176 0.6356 0.8661 0.062 Uiso 1 1 calc R A 1
H3B H -0.0977 0.5247 0.8633 0.062 Uiso 1 1 calc R A 1
C4 C 0.30018(17) 0.44356(15) 1.00592(10) 0.0150(3) Uani 1 1 d . A 1
C5 C 0.49650(17) 0.45901(14) 1.06763(12) 0.0202(3) Uani 1 1 d . A 1
H5 H 0.5803 0.4821 1.0795 0.024 Uiso 1 1 calc R A 1
C6 C 0.4280(2) 0.38559(17) 1.10902(12) 0.0214(4) Uani 1 1 d . A 1
H6 H 0.4557 0.3483 1.1548 0.026 Uiso 1 1 calc R A 1
C7 C 0.46371(16) 0.57084(14) 0.93970(12) 0.0170(3) Uani 1 1 d . A 1
C8 C 0.45379(19) 0.5163(2) 0.85615(11) 0.0243(4) Uani 1 1 d . A 1
H8A H 0.5058 0.4531 0.8562 0.036 Uiso 1 1 calc R A 1
H8B H 0.4845 0.5637 0.8145 0.036 Uiso 1 1 calc R A 1
H8C H 0.3648 0.4981 0.8454 0.036 Uiso 1 1 calc R A 1
C9 C 0.60585(19) 0.59921(18) 0.95594(13) 0.0251(4) Uani 1 1 d . A 1
H9A H 0.6576 0.5358 0.9552 0.038 Uiso 1 1 calc R A 1
H9B H 0.6132 0.6327 1.0084 0.038 Uiso 1 1 calc R A 1
H9C H 0.6361 0.6469 0.9144 0.038 Uiso 1 1 calc R A 1
C10 C 0.38203(18) 0.67131(15) 0.94101(15) 0.0251(4) Uani 1 1 d . A 1
H10A H 0.2927 0.6536 0.9308 0.038 Uiso 1 1 calc R A 1
H10B H 0.4124 0.7191 0.8996 0.038 Uiso 1 1 calc R A 1
H10C H 0.3894 0.7046 0.9935 0.038 Uiso 1 1 calc R A 1
C11 C 0.2114(2) 0.29583(17) 1.10020(12) 0.0223(4) Uani 1 1 d . A 1
C12 C 0.0909(3) 0.2901(2) 1.04779(16) 0.0415(6) Uani 1 1 d . A 1
H12A H 0.1149 0.2717 0.9929 0.062 Uiso 1 1 calc R A 1
H12B H 0.0481 0.3577 1.0479 0.062 Uiso 1 1 calc R A 1
H12C H 0.0332 0.2371 1.0692 0.062 Uiso 1 1 calc R A 1
C13 C 0.2783(3) 0.1871(2) 1.0983(2) 0.0475(7) Uani 1 1 d . A 1
H13A H 0.3552 0.1892 1.1314 0.071 Uiso 1 1 calc R A 1
H13B H 0.3015 0.1699 1.0431 0.071 Uiso 1 1 calc R A 1
H13C H 0.2199 0.1342 1.1191 0.071 Uiso 1 1 calc R A 1
C14 C 0.1737(3) 0.3244(3) 1.18739(17) 0.0492(8) Uani 1 1 d . A 1
H14A H 0.2503 0.3276 1.2207 0.074 Uiso 1 1 calc R A 1
H14B H 0.1157 0.2715 1.2086 0.074 Uiso 1 1 calc R A 1
H14C H 0.1312 0.3922 1.1878 0.074 Uiso 1 1 calc R A 1
C15 C 0.1233(3) 0.4015(2) 0.75561(12) 0.0334(5) Uani 1 1 d . A 1
H15A H 0.1616 0.4696 0.7421 0.040 Uiso 1 1 calc R A 1
H15B H 0.0296 0.4070 0.7507 0.040 Uiso 1 1 calc R A 1
C16 C 0.1748(3) 0.3164(3) 0.70034(16) 0.0475(7) Uani 1 1 d . A 1
H16A H 0.1980 0.3451 0.6474 0.057 Uiso 1 1 calc R A 1
H16B H 0.1114 0.2603 0.6929 0.057 Uiso 1 1 calc R A 1
C17 C 0.2947(3) 0.2757(2) 0.74535(15) 0.0385(6) Uani 1 1 d . A 1
H17A H 0.3150 0.2033 0.7298 0.046 Uiso 1 1 calc R A 1
H17B H 0.3697 0.3204 0.7351 0.046 Uiso 1 1 calc R A 1
C18 C 0.2518(2) 0.28216(17) 0.83396(14) 0.0256(4) Uani 1 1 d . A 1
H18A H 0.2107 0.2164 0.8508 0.031 Uiso 1 1 calc R A 1
H18B H 0.3257 0.2956 0.8693 0.031 Uiso 1 1 calc R A 1
B1 B 0.7123(2) 0.4479(2) 0.68209(16) 0.0290(5) Uani 1 1 d . B 1
F1 F 0.80136(16) 0.36892(15) 0.66249(11) 0.0462(4) Uani 1 1 d . B 1
F2 F 0.69957(15) 0.51729(16) 0.61575(10) 0.0473(4) Uani 1 1 d . B 1
F3 F 0.59253(15) 0.40238(14) 0.69995(9) 0.0380(3) Uani 1 1 d . B 1
F4 F 0.75724(18) 0.50501(16) 0.74816(11) 0.0547(5) Uani 1 1 d . B 1
N1 N 0.41837(14) 0.49379(13) 1.00386(8) 0.0152(3) Uani 1 1 d . A 1
N2 N 0.30862(15) 0.37601(12) 1.07070(10) 0.0172(3) Uani 1 1 d . A 1
O1 O 0.15982(14) 0.36954(12) 0.83786(8) 0.0233(3) Uani 1 1 d . A 1
Pd1 Pd 0.138332(12) 0.482885(11) 0.937872(8) 0.01535(3) Uani 1 1 d . A 1
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'
F F 0.0171 0.0103 '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'
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_publ_flag
C2A C1 Pd1 72.04(16) y
C3 C2A C1 122.9(4) y
C3 C2A Pd1 75.4(2) y
C1 C2A Pd1 68.01(16) y
C2A C3 Pd1 70.1(2) y
N2 C4 N1 104.54(14) y
N2 C4 Pd1 128.44(13) y
N1 C4 Pd1 126.23(12) y
C6 C5 N1 107.02(16) y
C5 C6 N2 107.22(16) y
N1 C7 C10 110.89(15) y
N1 C7 C9 109.02(15) y
C10 C7 C9 109.36(16) y
N1 C7 C8 108.25(15) y
C10 C7 C8 110.42(17) y
C9 C7 C8 108.87(16) y
N2 C11 C12 113.34(17) y
N2 C11 C14 108.20(18) y
C12 C11 C14 109.6(2) y
N2 C11 C13 107.24(18) y
C12 C11 C13 108.3(2) y
C14 C11 C13 110.2(2) y
O1 C15 C16 105.6(2) y
C15 C16 C17 103.6(2) y
C18 C17 C16 102.0(2) y
O1 C18 C17 105.78(19) y
F4 B1 F1 109.5(2) y
F4 B1 F3 110.3(2) y
F1 B1 F3 109.6(2) y
F4 B1 F2 108.3(2) y
F1 B1 F2 109.2(2) y
F3 B1 F2 109.7(2) y
C4 N1 C5 110.42(14) y
C4 N1 C7 126.15(14) y
C5 N1 C7 123.33(14) y
C4 N2 C6 110.79(15) y
C4 N2 C11 128.94(16) y
C6 N2 C11 120.23(16) y
C18 O1 C15 109.71(16) y
C18 O1 Pd1 126.46(12) y
C15 O1 Pd1 119.13(13) y
C4 Pd1 C1 94.62(8) y
C4 Pd1 C2A 131.35(12) y
C1 Pd1 C2A 39.94(12) y
C4 Pd1 O1 99.57(6) y
C1 Pd1 O1 165.64(7) y
C2A Pd1 O1 125.93(11) y
C4 Pd1 C3 162.11(9) y
C1 Pd1 C3 68.11(10) y
C2A Pd1 C3 34.54(13) y
O1 Pd1 C3 97.91(9) y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2A 1.439(4) y
C1 Pd1 2.079(2) y
C2A C3 1.286(5) y
C2A Pd1 2.132(3) y
C3 Pd1 2.194(3) y
C4 N2 1.363(2) y
C4 N1 1.371(2) y
C4 Pd1 2.0640(18) y
C5 C6 1.347(3) y
C5 N1 1.389(2) y
C6 N2 1.384(2) y
C7 N1 1.505(2) y
C7 C10 1.520(3) y
C7 C9 1.529(3) y
C7 C8 1.535(3) y
C11 N2 1.501(2) y
C11 C12 1.510(3) y
C11 C14 1.523(3) y
C11 C13 1.533(4) y
C15 O1 1.455(2) y
C15 C16 1.501(4) y
C16 C17 1.525(4) y
C17 C18 1.519(3) y
C18 O1 1.453(3) y
B1 F4 1.379(3) y
B1 F1 1.391(3) y
B1 F3 1.391(3) y
B1 F2 1.401(3) y
O1 Pd1 2.1850(14) y
