#------------------------------------------------------------------------------
#$Date: 2016-09-07 17:57:18 +0300 (Wed, 07 Sep 2016) $
#$Revision: 186242 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/39/4513920.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_4513920
loop_
_publ_author_name
'Dehury, Niranjan'
'Maity, Niladri'
'Tripathy, Suman Kumar'
'Basset, Jean-Marie'
'Patra, Srikanta'
_publ_section_title
;
 Dinuclear Tetrapyrazolyl Palladium Complexes Exhibiting Facile Tandem
 Transfer Hydrogenation/Suzuki Coupling Reaction of Fluoroarylketone
;
_journal_issue                   8
_journal_name_full               'ACS Catalysis'
_journal_page_first              5535
_journal_paper_doi               10.1021/acscatal.6b01421
_journal_volume                  6
_journal_year                    2016
_chemical_formula_moiety         'C20 H18 Cl4 N8 Pd2'
_chemical_formula_sum            'C20 H18 Cl4 N8 Pd2'
_chemical_formula_weight         725.02
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.281(4)
_cell_angle_beta                 104.335(4)
_cell_angle_gamma                102.182(4)
_cell_formula_units_Z            1
_cell_length_a                   7.6020(10)
_cell_length_b                   8.2980(11)
_cell_length_c                   10.7372(15)
_cell_measurement_reflns_used    2105
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.75
_cell_measurement_theta_min      2.58
_cell_volume                     624.94(15)
_computing_cell_refinement       'Bruker SHELXL'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ortep-3 V2.02 ( Farrugia, 1997)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  Multi-scan
_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  0.0799
_diffrn_reflns_av_sigmaI/netI    0.0889
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15146
_diffrn_reflns_theta_full        28.75
_diffrn_reflns_theta_max         28.75
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    1.893
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.926
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             354
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.657
_refine_diff_density_min         -1.185
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         3210
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1304
_refine_ls_R_factor_gt           0.0748
_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)+(0.1000P)²+0.3557P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1650
_refine_ls_wR_factor_ref         0.1929
_reflns_number_gt                2105
_reflns_number_total             3251
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs6b01421_si_003.cif
_cod_data_source_block           mo_parapzpd2_1_0m_a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/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 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 4513918--4513920.cif.
;
_cod_database_code               4513920
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
Pd1 Pd 0.35572(8) 1.48593(7) 0.26859(6) 0.0362(2) Uani 1 1 d .
Cl1 Cl 0.4517(4) 1.6762(3) 0.1505(2) 0.0591(6) Uani 1 1 d .
Cl2 Cl 0.1687(3) 1.6458(3) 0.3345(3) 0.0622(6) Uani 1 1 d .
N3 N 0.2699(8) 1.3152(7) 0.3726(5) 0.0329(13) Uani 1 1 d .
N4 N 0.2908(9) 1.1559(7) 0.3527(6) 0.0362(14) Uani 1 1 d .
N1 N 0.5326(8) 1.3476(7) 0.2195(6) 0.0339(13) Uani 1 1 d .
N2 N 0.5030(8) 1.1794(7) 0.2195(6) 0.0364(14) Uani 1 1 d .
C9 C 0.1565(10) 1.1258(9) 0.0077(7) 0.0334(16) Uani 1 1 d .
H9 H 0.2612 1.2106 0.0122 0.040 Uiso 1 1 calc R
C8 C 0.1602(9) 1.0434(8) 0.1093(7) 0.0303(15) Uani 1 1 d .
C7 C 0.3285(10) 1.0781(9) 0.2308(7) 0.0337(16) Uani 1 1 d .
H7 H 0.3495 0.9680 0.2419 0.040 Uiso 1 1 calc R
C4 C 0.2115(11) 1.3368(10) 0.4794(7) 0.0421(18) Uani 1 1 d .
H4 H 0.1843 1.4349 0.5155 0.051 Uiso 1 1 calc R
C10 C 0.0017(10) 0.9157(9) 0.1017(7) 0.0385(17) Uani 1 1 d .
H10 H 0.0022 0.8588 0.1696 0.046 Uiso 1 1 calc R
C1 C 0.6936(11) 1.3932(10) 0.1956(8) 0.0452(19) Uani 1 1 d .
H1 H 0.7480 1.5019 0.1895 0.054 Uiso 1 1 calc R
C6 C 0.2496(12) 1.0796(11) 0.4474(8) 0.047(2) Uani 1 1 d .
H6 H 0.2556 0.9710 0.4557 0.057 Uiso 1 1 calc R
C3 C 0.6481(11) 1.1250(11) 0.1956(8) 0.047(2) Uani 1 1 d .
H3 H 0.6610 1.0153 0.1902 0.056 Uiso 1 1 calc R
C5 C 0.1971(13) 1.1928(11) 0.5290(8) 0.054(2) Uani 1 1 d .
H5 H 0.1593 1.1759 0.6030 0.065 Uiso 1 1 calc R
C2 C 0.7727(12) 1.2582(12) 0.1807(10) 0.058(2) Uani 1 1 d .
H2 H 0.8871 1.2588 0.1639 0.069 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'
Cl Cl 0.1484 0.1585 '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
N3 Pd1 N1 89.5(2) . .
N3 Pd1 Cl1 179.60(16) . .
N1 Pd1 Cl1 90.21(18) . .
N3 Pd1 Cl2 89.68(17) . .
N1 Pd1 Cl2 177.00(17) . .
Cl1 Pd1 Cl2 90.59(9) . .
C4 N3 N4 106.2(6) . .
C4 N3 Pd1 130.1(5) . .
N4 N3 Pd1 123.1(4) . .
C6 N4 N3 110.6(6) . .
C6 N4 C7 127.5(6) . .
N3 N4 C7 121.4(5) . .
C1 N1 N2 106.2(6) . .
C1 N1 Pd1 131.3(5) . .
N2 N1 Pd1 122.2(5) . .
C3 N2 N1 109.5(6) . .
C3 N2 C7 127.5(6) . .
N1 N2 C7 122.7(5) . .
C8 C9 C10 121.0(7) . 2_575
C8 C9 H9 119.5 . .
C10 C9 H9 119.5 2_575 .
C9 C8 C10 119.1(7) . .
C9 C8 C7 124.4(6) . .
C10 C8 C7 116.5(6) . .
N2 C7 N4 109.7(5) . .
N2 C7 C8 114.3(6) . .
N4 C7 C8 112.1(6) . .
N2 C7 H7 106.8 . .
N4 C7 H7 106.8 . .
C8 C7 H7 106.8 . .
N3 C4 C5 110.2(7) . .
N3 C4 H4 124.9 . .
C5 C4 H4 124.9 . .
C9 C10 C8 119.9(7) 2_575 .
C9 C10 H10 120.1 2_575 .
C8 C10 H10 120.1 . .
N1 C1 C2 110.9(7) . .
N1 C1 H1 124.5 . .
C2 C1 H1 124.5 . .
N4 C6 C5 106.9(7) . .
N4 C6 H6 126.6 . .
C5 C6 H6 126.6 . .
N2 C3 C2 107.9(7) . .
N2 C3 H3 126.1 . .
C2 C3 H3 126.1 . .
C6 C5 C4 106.2(7) . .
C6 C5 H5 126.9 . .
C4 C5 H5 126.9 . .
C3 C2 C1 105.4(7) . .
C3 C2 H2 127.3 . .
C1 C2 H2 127.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 N3 2.040(6) .
Pd1 N1 2.052(6) .
Pd1 Cl1 2.291(2) .
Pd1 Cl2 2.296(2) .
N3 C4 1.328(9) .
N3 N4 1.354(8) .
N4 C6 1.347(10) .
N4 C7 1.484(9) .
N1 C1 1.303(9) .
N1 N2 1.366(8) .
N2 C3 1.342(9) .
N2 C7 1.457(9) .
C9 C8 1.375(10) .
C9 C10 1.393(10) 2_575
C9 H9 0.9300 .
C8 C10 1.402(10) .
C8 C7 1.523(9) .
C7 H7 0.9800 .
C4 C5 1.380(12) .
C4 H4 0.9300 .
C10 C9 1.393(10) 2_575
C10 H10 0.9300 .
C1 C2 1.385(11) .
C1 H1 0.9300 .
C6 C5 1.369(12) .
C6 H6 0.9300 .
C3 C2 1.354(12) .
C3 H3 0.9300 .
C5 H5 0.9300 .
C2 H2 0.9300 .
