#------------------------------------------------------------------------------
#$Date: 2016-03-21 14:58:37 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178732 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/43/4084368.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_4084368
loop_
_publ_author_name
'Guo, Tongxun'
'Dechert, Sebastian'
'Meyer, Franc'
_publ_section_title
;
 Dinuclear Palladium Complexes of Pyrazole-Bridged Bis(NHC) Ligands: A
 Delicate Balance between Normal and Abnormal Carbene Coordination
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5145
_journal_paper_doi               10.1021/om500351j
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C26 H30 N12 Pd2 2+, 2(F6 P -), 2(C3 H6 O)'
_chemical_formula_sum            'C32 H42 F12 N12 O2 P2 Pd2'
_chemical_formula_weight         1129.52
_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                 99.781(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.1354(2)
_cell_length_b                   11.0444(4)
_cell_length_c                   23.5739(6)
_cell_measurement_reflns_used    25821
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.64
_cell_measurement_theta_min      1.75
_cell_volume                     2087.34(11)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       ω
_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  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            25821
_diffrn_reflns_theta_full        25.64
_diffrn_reflns_theta_max         25.64
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    1.040
_exptl_absorpt_correction_T_max  0.8577
_exptl_absorpt_correction_T_min  0.6383
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         3934
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0309
_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)+(0.0399P)²+3.2005P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0782
_reflns_number_gt                3760
_reflns_number_total             3934
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500351j_si_002.cif
_cod_data_source_block           LMe2Pd2PF62-togu1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4084368--4084374.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4084368
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
Pd1 Pd 0.80708(3) 0.61530(2) 0.471235(11) 0.02535(9) Uani 1 1 d .
N1 N 0.8542(4) 0.4376(3) 0.44711(12) 0.0272(6) Uani 1 1 d .
N2 N 0.9801(4) 0.3579(2) 0.46775(13) 0.0266(6) Uani 1 1 d .
N3 N 0.5197(4) 0.5165(3) 0.39117(13) 0.0329(7) Uani 1 1 d .
N4 N 0.4314(4) 0.6329(3) 0.45226(13) 0.0319(7) Uani 1 1 d .
N5 N 1.1774(4) 0.1313(3) 0.48762(13) 0.0319(7) Uani 1 1 d .
N6 N 1.3013(4) 0.1365(3) 0.57524(13) 0.0320(7) Uani 1 1 d .
C1 C 0.8481(5) 0.2884(3) 0.38326(16) 0.0327(8) Uani 1 1 d .
H1 H 0.8167 0.2392 0.3501 0.039 Uiso 1 1 calc R
C2 C 0.7754(5) 0.3952(3) 0.39613(15) 0.0306(7) Uani 1 1 d .
C3 C 0.9753(5) 0.2681(3) 0.42829(15) 0.0301(8) Uani 1 1 d .
C4 C 0.6370(5) 0.4605(3) 0.35838(16) 0.0348(9) Uani 1 1 d .
H4A H 0.6851 0.5239 0.3365 0.042 Uiso 1 1 calc R
H4B H 0.5760 0.4026 0.3303 0.042 Uiso 1 1 calc R
C5 C 0.5724(5) 0.5923(3) 0.43511(16) 0.0303(8) Uani 1 1 d .
C6 C 0.3486(5) 0.5083(4) 0.38100(18) 0.0404(9) Uani 1 1 d .
H6 H 0.2823 0.4603 0.3524 0.048 Uiso 1 1 calc R
C7 C 0.2931(5) 0.5810(4) 0.41915(19) 0.0402(9) Uani 1 1 d .
H7 H 0.1800 0.5943 0.4227 0.048 Uiso 1 1 calc R
C8 C 0.4232(5) 0.7213(4) 0.49765(18) 0.0386(9) Uani 1 1 d .
H8A H 0.5045 0.6999 0.5318 0.058 Uiso 1 1 calc R
H8B H 0.3108 0.7213 0.5074 0.058 Uiso 1 1 calc R
H8C H 0.4489 0.8020 0.4842 0.058 Uiso 1 1 calc R
C9 C 1.1051(5) 0.1706(4) 0.43005(16) 0.0356(9) Uani 1 1 d .
H9A H 1.0540 0.0998 0.4081 0.043 Uiso 1 1 calc R
H9B H 1.1957 0.2008 0.4105 0.043 Uiso 1 1 calc R
C10 C 1.2304(4) 0.2075(3) 0.53101(16) 0.0300(7) Uani 1 1 d .
C11 C 1.2137(5) 0.0128(3) 0.50390(19) 0.0380(9) Uani 1 1 d .
H11 H 1.1883 -0.0573 0.4808 0.046 Uiso 1 1 calc R
C12 C 1.2913(5) 0.0162(3) 0.55846(19) 0.0378(9) Uani 1 1 d .
H12 H 1.3322 -0.0514 0.5815 0.045 Uiso 1 1 calc R
C13 C 1.3754(6) 0.1770(4) 0.63309(17) 0.0406(9) Uani 1 1 d .
H13A H 1.4869 0.2100 0.6324 0.061 Uiso 1 1 calc R
H13B H 1.3841 0.1082 0.6597 0.061 Uiso 1 1 calc R
H13C H 1.3050 0.2398 0.6459 0.061 Uiso 1 1 calc R
P1 P 0.63202(15) 0.65740(10) 0.20230(5) 0.0406(3) Uani 1 1 d .
F1 F 0.5661(5) 0.7678(3) 0.23522(12) 0.0727(10) Uani 1 1 d .
F2 F 0.4906(6) 0.5752(4) 0.2183(2) 0.1059(16) Uani 1 1 d .
F3 F 0.5196(5) 0.6993(3) 0.14371(13) 0.0799(11) Uani 1 1 d .
F4 F 0.7763(5) 0.7416(3) 0.18627(12) 0.0760(10) Uani 1 1 d .
F5 F 0.7539(4) 0.6227(3) 0.26008(12) 0.0710(9) Uani 1 1 d .
F6 F 0.6971(4) 0.5499(3) 0.16772(14) 0.0638(8) Uani 1 1 d .
O1 O 1.0641(5) 0.8595(4) 0.37798(16) 0.0684(11) Uani 1 1 d .
C14 C 1.1396(7) 0.7910(5) 0.2902(2) 0.0543(12) Uani 1 1 d .
H14A H 1.2036 0.7300 0.3149 0.081 Uiso 1 1 calc R
H14B H 1.2158 0.8412 0.2723 0.081 Uiso 1 1 calc R
H14C H 1.0602 0.7506 0.2602 0.081 Uiso 1 1 calc R
C15 C 1.0463(6) 0.8694(4) 0.3259(2) 0.0497(11) Uani 1 1 d .
C16 C 0.9293(7) 0.9599(5) 0.2935(3) 0.0608(14) Uani 1 1 d .
H16A H 0.8368 0.9174 0.2696 0.091 Uiso 1 1 calc R
H16B H 0.9890 1.0088 0.2689 0.091 Uiso 1 1 calc R
H16C H 0.8854 1.0127 0.3208 0.091 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'
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'
P P 0.1023 0.0942 '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
C5 Pd1 C10 89.02(15) . 3_766
C5 Pd1 N2 161.96(14) . 3_766
C10 Pd1 N2 89.08(13) 3_766 3_766
C5 Pd1 N1 88.29(13) . .
C10 Pd1 N1 162.23(14) 3_766 .
N2 Pd1 N1 98.75(11) 3_766 .
C2 N1 N2 107.8(3) . .
C2 N1 Pd1 119.1(2) . .
N2 N1 Pd1 131.5(2) . .
C3 N2 N1 107.0(3) . .
C3 N2 Pd1 120.2(2) . 3_766
N1 N2 Pd1 129.6(2) . 3_766
C5 N3 C6 110.9(4) . .
C5 N3 C4 121.3(3) . .
C6 N3 C4 127.7(3) . .
C5 N4 C7 110.1(3) . .
C5 N4 C8 125.9(3) . .
C7 N4 C8 124.0(3) . .
C10 N5 C11 110.9(3) . .
C10 N5 C9 123.7(3) . .
C11 N5 C9 125.2(3) . .
C10 N6 C12 109.8(3) . .
C10 N6 C13 126.5(3) . .
C12 N6 C13 123.6(3) . .
C3 C1 C2 105.4(3) . .
N1 C2 C1 109.7(3) . .
N1 C2 C4 124.0(3) . .
C1 C2 C4 126.1(3) . .
N2 C3 C1 110.0(3) . .
N2 C3 C9 124.5(3) . .
C1 C3 C9 125.0(3) . .
N3 C4 C2 112.4(3) . .
N3 C5 N4 105.1(3) . .
N3 C5 Pd1 124.9(3) . .
N4 C5 Pd1 129.4(3) . .
C7 C6 N3 106.9(4) . .
C6 C7 N4 107.1(4) . .
N5 C9 C3 114.2(3) . .
N5 C10 N6 105.4(3) . .
N5 C10 Pd1 124.9(3) . 3_766
N6 C10 Pd1 129.6(3) . 3_766
C12 C11 N5 106.6(3) . .
C11 C12 N6 107.3(3) . .
F2 P1 F6 90.8(2) . .
F2 P1 F1 90.2(2) . .
F6 P1 F1 178.20(18) . .
F2 P1 F5 91.7(2) . .
F6 P1 F5 92.66(18) . .
F1 P1 F5 88.81(17) . .
F2 P1 F3 92.3(3) . .
F6 P1 F3 87.94(17) . .
F1 P1 F3 90.52(16) . .
F5 P1 F3 175.9(2) . .
F2 P1 F4 179.7(2) . .
F6 P1 F4 89.51(19) . .
F1 P1 F4 89.5(2) . .
F5 P1 F4 88.09(19) . .
F3 P1 F4 87.8(2) . .
O1 C15 C16 122.1(5) . .
O1 C15 C14 122.0(5) . .
C16 C15 C14 116.0(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 C5 1.970(4) .
Pd1 C10 1.980(4) 3_766
Pd1 N2 2.076(3) 3_766
Pd1 N1 2.096(3) .
N1 C2 1.346(5) .
N1 N2 1.376(4) .
N2 C3 1.356(5) .
N2 Pd1 2.076(3) 3_766
N3 C5 1.344(5) .
N3 C6 1.375(6) .
N3 C4 1.464(5) .
N4 C5 1.356(5) .
N4 C7 1.380(5) .
N4 C8 1.458(5) .
N5 C10 1.338(5) .
N5 C11 1.382(5) .
N5 C9 1.451(5) .
N6 C10 1.353(5) .
N6 C12 1.385(5) .
N6 C13 1.464(5) .
C1 C3 1.369(5) .
C1 C2 1.376(5) .
C2 C4 1.496(5) .
C3 C9 1.504(5) .
C6 C7 1.339(6) .
C10 Pd1 1.980(4) 3_766
C11 C12 1.334(6) .
P1 F2 1.561(4) .
P1 F6 1.582(3) .
P1 F1 1.586(3) .
P1 F5 1.589(3) .
P1 F3 1.590(3) .
P1 F4 1.593(3) .
O1 C15 1.217(6) .
C14 C15 1.499(7) .
C15 C16 1.497(7) .
