#------------------------------------------------------------------------------
#$Date: 2016-03-21 09:22:05 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178622 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/33/4073300.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_4073300
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_compound_source        toluene
_chemical_formula_moiety         'C14 H25 B F4 N2 Pd'
_chemical_formula_sum            'C14 H25 B F4 N2 Pd'
_chemical_formula_weight         414.57
_chemical_melting_point          ?
_chemical_name_systematic
; 
 (η³-allyl)-(tetrafluoroborato-F)-(1,3-bis(tert-butyl)-
 imidazol-2-ylidine)-palladium(ii)
 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                103.688(2)
_cell_angle_beta                 90.954(2)
_cell_angle_gamma                97.222(2)
_cell_formula_units_Z            2
_cell_length_a                   8.5926(5)
_cell_length_b                   9.9062(5)
_cell_length_c                   10.5937(5)
_cell_measurement_reflns_used    73734
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.14
_cell_measurement_theta_min      2.91
_cell_volume                     868.17(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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24774
_diffrn_reflns_theta_full        33.07
_diffrn_reflns_theta_max         33.07
_diffrn_reflns_theta_min         4.25
_diffrn_standards_decay_%        0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.103
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.80332
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scalepack, Otwinowski (1997)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.004
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         6538
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0277P)²+1.1423P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0900
_reflns_number_gt                5695
_reflns_number_total             6538
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            om0702274si20070309_074405.cif
_cod_data_source_block           12a
_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               4073300
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
C1 C 0.3666(3) 0.0124(3) 0.2887(3) 0.0330(6) Uani 1 1 d . A 1
H1A H 0.4104 0.0374 0.3774 0.040 Uiso 1 1 calc R A 1
H1B H 0.4445 -0.0078 0.2241 0.040 Uiso 1 1 calc R A 1
C2A C 0.2505(6) 0.0909(5) 0.2606(6) 0.0279(10) Uani 0.50 1 d P A 1
H2A H 0.2536 0.1251 0.1810 0.033 Uiso 0.50 1 calc PR A 1
C2B C 0.2631(8) 0.0747(6) 0.3792(8) 0.0472(17) Uani 0.50 1 d P B 2
C3 C 0.1212(4) 0.0995(3) 0.3344(4) 0.0412(7) Uani 1 1 d . A 1
H3A H 0.0317 0.1321 0.2996 0.049 Uiso 1 1 calc R A 1
H3B H 0.1403 0.1352 0.4276 0.049 Uiso 1 1 calc R A 1
C4 C 0.2288(2) -0.3114(2) 0.1817(2) 0.0178(4) Uani 1 1 d . A 1
C5 C 0.3096(3) -0.5221(2) 0.1657(2) 0.0232(4) Uani 1 1 d . A 1
H5 H 0.3404 -0.6000 0.1889 0.028 Uiso 1 1 calc R A 1
C6 C 0.3008(3) -0.5019(2) 0.0449(2) 0.0249(4) Uani 1 1 d . A 1
H6 H 0.3244 -0.5632 -0.0312 0.030 Uiso 1 1 calc R A 1
C7 C 0.2654(3) -0.3837(2) 0.3943(2) 0.0190(4) Uani 1 1 d . A 1
C8 C 0.1143(4) -0.3299(3) 0.4453(3) 0.0341(6) Uani 1 1 d . A 1
H8A H 0.0258 -0.3966 0.4059 0.051 Uiso 1 1 calc R A 1
H8B H 0.1067 -0.2419 0.4240 0.051 Uiso 1 1 calc R A 1
H8C H 0.1152 -0.3173 0.5380 0.051 Uiso 1 1 calc R A 1
C9 C 0.2751(4) -0.5237(3) 0.4282(3) 0.0299(5) Uani 1 1 d . A 1
H9A H 0.1847 -0.5889 0.3904 0.045 Uiso 1 1 calc R A 1
H9B H 0.2781 -0.5106 0.5210 0.045 Uiso 1 1 calc R A 1
H9C H 0.3686 -0.5598 0.3945 0.045 Uiso 1 1 calc R A 1
C10 C 0.4089(3) -0.2804(3) 0.4549(3) 0.0325(6) Uani 1 1 d . A 1
H10A H 0.5025 -0.3167 0.4215 0.049 Uiso 1 1 calc R A 1
H10B H 0.4114 -0.2674 0.5477 0.049 Uiso 1 1 calc R A 1
H10C H 0.4033 -0.1921 0.4336 0.049 Uiso 1 1 calc R A 1
C11 C 0.2332(3) -0.3087(3) -0.0582(2) 0.0281(5) Uani 1 1 d . A 1
C12 C 0.0832(4) -0.2392(5) -0.0499(4) 0.0503(9) Uani 1 1 d . A 1
H12A H -0.0060 -0.3082 -0.0505 0.075 Uiso 1 1 calc R A 1
H12B H 0.0735 -0.1988 -0.1231 0.075 Uiso 1 1 calc R A 1
H12C H 0.0882 -0.1670 0.0291 0.075 Uiso 1 1 calc R A 1
C13 C 0.2267(6) -0.4241(4) -0.1838(3) 0.0616(12) Uani 1 1 d . A 1
H13A H 0.1370 -0.4928 -0.1852 0.092 Uiso 1 1 calc R A 1
H13B H 0.3206 -0.4679 -0.1878 0.092 Uiso 1 1 calc R A 1
H13C H 0.2184 -0.3838 -0.2573 0.092 Uiso 1 1 calc R A 1
C14 C 0.3765(4) -0.1999(3) -0.0570(3) 0.0378(6) Uani 1 1 d . A 1
H14A H 0.4699 -0.2446 -0.0629 0.057 Uiso 1 1 calc R A 1
H14B H 0.3824 -0.1282 0.0223 0.057 Uiso 1 1 calc R A 1
H14C H 0.3671 -0.1588 -0.1298 0.057 Uiso 1 1 calc R A 1
B1 B -0.2354(4) -0.1449(3) 0.2278(4) 0.0404(8) Uani 1 1 d . A 1
F1 F -0.09962(18) -0.21248(16) 0.23858(18) 0.0337(4) Uani 1 1 d . A 1
F2 F -0.2479(3) -0.0492(3) 0.3409(4) 0.1147(16) Uani 1 1 d . A 1
F3 F -0.2152(3) -0.0832(4) 0.1257(4) 0.1143(15) Uani 1 1 d . A 1
F4 F -0.36486(19) -0.24445(19) 0.20385(18) 0.0374(4) Uani 1 1 d . A 1
N1 N 0.2641(2) -0.40529(18) 0.24921(17) 0.0170(3) Uani 1 1 d . A 1
N2 N 0.2501(2) -0.3729(2) 0.05495(18) 0.0206(4) Uani 1 1 d . A 1
Pd1 Pd 0.15345(2) -0.119027(17) 0.254074(19) 0.02175(6) 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'
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 72.1(2) y
C3 C2A C1 118.8(4) y
C3 C2A Pd1 73.8(2) y
C1 C2A Pd1 68.8(2) y
C2A C3 Pd1 69.2(2) y
N1 C4 N2 105.04(18) y
N1 C4 Pd1 127.74(16) y
N2 C4 Pd1 127.20(16) y
C6 C5 N1 107.1(2) y
C5 C6 N2 107.2(2) y
N1 C7 C8 109.81(18) y
N1 C7 C9 108.84(18) y
C8 C7 C9 108.8(2) y
N1 C7 C10 109.07(19) y
C8 C7 C10 111.1(2) y
C9 C7 C10 109.3(2) y
N2 C11 C14 108.9(2) y
N2 C11 C12 110.2(2) y
C14 C11 C12 110.1(3) y
N2 C11 C13 108.6(2) y
C14 C11 C13 109.0(3) y
C12 C11 C13 110.0(3) y
F2 B1 F3 111.7(4) y
F2 B1 F4 110.3(3) y
F3 B1 F4 110.3(3) y
F2 B1 F1 108.9(3) y
F3 B1 F1 107.0(3) y
F4 B1 F1 108.5(2) y
B1 F1 Pd1 128.04(17) y
C4 N1 C5 110.35(18) y
C4 N1 C7 125.70(17) y
C5 N1 C7 123.82(18) y
C4 N2 C6 110.27(19) y
C4 N2 C11 126.0(2) y
C6 N2 C11 123.6(2) y
C4 Pd1 C1 101.01(10) y
C4 Pd1 C2A 133.53(16) y
C1 Pd1 C2A 39.09(16) y
C4 Pd1 C3 169.13(10) y
C1 Pd1 C3 68.13(12) y
C2A Pd1 C3 37.02(18) y
C4 Pd1 F1 92.87(7) y
C1 Pd1 F1 166.09(9) y
C2A Pd1 F1 128.78(15) y
C3 Pd1 F1 97.99(9) y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2A 1.408(6) y
C1 Pd1 2.082(3) y
C2A C3 1.369(7) y
C2A Pd1 2.126(5) y
C3 Pd1 2.185(3) y
C4 N1 1.359(3) y
C4 N2 1.363(3) y
C4 Pd1 2.067(2) y
C5 C6 1.344(3) y
C5 N1 1.384(3) y
C6 N2 1.383(3) y
C7 N1 1.501(3) y
C7 C8 1.524(3) y
C7 C9 1.524(3) y
C7 C10 1.525(3) y
C11 N2 1.497(3) y
C11 C14 1.528(4) y
C11 C12 1.530(4) y
C11 C13 1.530(4) y
B1 F2 1.356(5) y
B1 F3 1.366(5) y
B1 F4 1.367(4) y
B1 F1 1.432(3) y
F1 Pd1 2.2411(15) y
