#------------------------------------------------------------------------------
#$Date: 2019-11-17 10:26:46 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229343 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/73/7047382.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_7047382
loop_
_publ_author_name
'Milocco, Francesca'
'de Vries, Folkert'
'Dall'Anese, Anna'
'Rosar, Vera'
'Zangrando, Ennio'
'Otten, Edwin'
'Milani, Barbara'
_publ_section_title
;
 Palladium alkyl complexes with a formazanate ligand: synthesis, structure
 and reactivity.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14445
_journal_page_last               14451
_journal_paper_doi               10.1039/c8dt03130d
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C41 H35 Cl3 N8 Pd'
_chemical_formula_weight         852.52
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2018-07-31 deposited with the CCDC.
2018-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                98.99(3)
_cell_angle_beta                 90.96(3)
_cell_angle_gamma                99.37(3)
_cell_formula_units_Z            1
_cell_length_a                   8.0390(16)
_cell_length_b                   8.1400(16)
_cell_length_c                   14.734(3)
_cell_measurement_reflns_used    3578
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.76
_cell_measurement_theta_min      2.05
_cell_volume                     938.7(3)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_data_reduction        'XDS - CCP4'
_computing_molecular_graphics    'Ortep3 for Windows'
_computing_publication_material  'Wingx 2013.03 (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'Sir2014 (Burla, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Dectris Pilatus 2M'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  Si111
_diffrn_radiation_source         'Elettra Synchrotron, Trieste (Italy)'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34316
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         1.379
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_T_max  0.847
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       needle
_exptl_crystal_F_000             434
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.283
_refine_diff_density_min         -1.086
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         5601
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0307P)²+0.8368P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0691
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5597
_reflns_number_total             5601
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt03130d2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7047382--7047384.cif.'
_cod_database_code               7047382
_shelx_shelxl_version_number     2018/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pd Pd 0.000000 0.500000 1.000000 0.01013(4) Uani 1 2 d S . P
Cl1 Cl 0.63716(16) 0.56621(15) 0.57701(9) 0.0351(2) Uani 0.5 1 d . . P
Cl2 Cl 0.33628(15) 0.31718(14) 0.57127(10) 0.0498(3) Uani 0.5 1 d . . P
Cl3 Cl 0.3952(2) 0.5149(3) 0.42394(9) 0.0606(4) Uani 0.5 1 d . . P
N1 N 0.00117(15) 0.36893(14) 0.87129(8) 0.01271(19) Uani 1 1 d . . .
N2 N 0.23215(14) 0.60406(14) 0.96786(8) 0.01193(19) Uani 1 1 d . . .
N3 N 0.26081(15) 0.65711(14) 0.89045(8) 0.0132(2) Uani 1 1 d . . .
N4 N 0.05284(15) 0.44402(14) 0.80310(8) 0.0137(2) Uani 1 1 d . . .
C1 C -0.07071(17) 0.19593(16) 0.84453(9) 0.0142(2) Uani 1 1 d . . .
C2 C -0.09656(18) 0.09279(17) 0.91164(9) 0.0148(2) Uani 1 1 d . . .
H2 H -0.066467 0.138101 0.974238 0.018 Uiso 1 1 calc R U .
C3 C -0.16663(19) -0.07709(17) 0.88701(10) 0.0172(2) Uani 1 1 d . . .
H3 H -0.183836 -0.147124 0.933053 0.021 Uiso 1 1 calc R U .
C4 C -0.2113(2) -0.14447(19) 0.79626(11) 0.0252(3) Uani 1 1 d . . .
H4 H -0.259438 -0.260157 0.779753 0.030 Uiso 1 1 calc R U .
C5 C -0.1849(3) -0.0411(2) 0.72935(12) 0.0377(5) Uani 1 1 d . . .
H5 H -0.215225 -0.086881 0.666830 0.045 Uiso 1 1 calc R U .
C6 C -0.1148(3) 0.1280(2) 0.75277(11) 0.0296(4) Uani 1 1 d . . .
H6 H -0.096831 0.197327 0.706440 0.036 Uiso 1 1 calc R U .
C7 C 0.36731(16) 0.65247(16) 1.03505(9) 0.0122(2) Uani 1 1 d . . .
C8 C 0.36629(17) 0.56264(17) 1.10841(9) 0.0149(2) Uani 1 1 d . . .
H8 H 0.279798 0.469029 1.110892 0.018 Uiso 1 1 calc R U .
C9 C 0.49212(19) 0.61043(19) 1.17789(10) 0.0182(3) Uani 1 1 d . . .
H9 H 0.491353 0.549334 1.227840 0.022 Uiso 1 1 calc R U .
C10 C 0.61883(19) 0.7471(2) 1.17448(10) 0.0196(3) Uani 1 1 d . . .
H10 H 0.703553 0.780845 1.222521 0.024 Uiso 1 1 calc R U .
C11 C 0.62113(18) 0.83453(19) 1.10026(10) 0.0189(3) Uani 1 1 d . . .
H11 H 0.708694 0.927101 1.097560 0.023 Uiso 1 1 calc R U .
C12 C 0.49688(17) 0.78782(17) 1.03025(10) 0.0156(2) Uani 1 1 d . . .
H12 H 0.499782 0.847213 0.979530 0.019 Uiso 1 1 calc R U .
C13 C 0.15669(17) 0.59334(17) 0.81597(9) 0.0136(2) Uani 1 1 d . . .
C14 C 0.18354(19) 0.67674(19) 0.73395(9) 0.0171(2) Uani 1 1 d . . .
C15 C 0.3198(2) 0.8047(2) 0.72992(10) 0.0220(3) Uani 1 1 d . . .
H15 H 0.400006 0.838251 0.780206 0.026 Uiso 1 1 calc R U .
C16 C 0.3393(3) 0.8840(3) 0.65260(13) 0.0347(4) Uani 1 1 d . . .
H16 H 0.432399 0.971629 0.650970 0.042 Uiso 1 1 calc R U .
C17 C 0.2239(3) 0.8364(4) 0.57745(15) 0.0482(6) Uani 1 1 d . U .
C18 C 0.0883(3) 0.7094(4) 0.58193(13) 0.0427(6) Uani 1 1 d . . .
H18 H 0.008323 0.675812 0.531562 0.051 Uiso 1 1 calc R U .
C19 C 0.0675(2) 0.6303(3) 0.65883(11) 0.0272(3) Uani 1 1 d . . .
H19 H -0.026558 0.543693 0.660500 0.033 Uiso 1 1 calc R U .
C20 C 0.2457(4) 0.9195(6) 0.4927(2) 0.0954(16) Uani 1 1 d . U .
H20A H 0.293201 0.845915 0.444411 0.143 Uiso 1 1 calc R U .
H20B H 0.322162 1.027611 0.507700 0.143 Uiso 1 1 calc R U .
H20C H 0.135748 0.938775 0.470824 0.143 Uiso 1 1 calc R U .
C21 C 0.4235(5) 0.5132(5) 0.5423(2) 0.0267(6) Uani 0.5 1 d . . P
H21 H 0.363055 0.600555 0.576114 0.032 Uiso 0.5 1 calc R U P
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
N2 Pd N2 180.0 . 2_567
N2 Pd N1 82.04(6) . .
N2 Pd N1 97.96(6) 2_567 .
N2 Pd N1 97.97(6) . 2_567
N2 Pd N1 82.03(6) 2_567 2_567
N1 Pd N1 180.0 . 2_567
Cl3 Cl1 C21 65.7(2) 2_666 .
Cl3 Cl1 C21 75.2(2) 2_666 2_666
C21 Cl1 C21 60.1(2) . 2_666
C21 Cl2 Cl3 42.66(13) . 2_666
Cl1 Cl3 C21 91.9(3) 2_666 2_666
Cl1 Cl3 C21 83.3(2) 2_666 .
C21 Cl3 C21 63.9(2) 2_666 .
Cl1 Cl3 Cl2 137.9(3) 2_666 2_666
C21 Cl3 Cl2 48.21(15) 2_666 2_666
C21 Cl3 Cl2 88.42(15) . 2_666
N4 N1 C1 113.74(11) . .
N4 N1 Pd 121.08(9) . .
C1 N1 Pd 124.77(9) . .
N3 N2 C7 115.11(11) . .
N3 N2 Pd 122.32(9) . .
C7 N2 Pd 121.55(9) . .
N2 N3 C13 120.38(12) . .
N1 N4 C13 121.90(12) . .
C2 C1 C6 119.54(13) . .
C2 C1 N1 119.00(12) . .
C6 C1 N1 121.46(13) . .
C1 C2 C3 119.99(13) . .
C1 C2 H2 120.0 . .
C3 C2 H2 120.0 . .
C4 C3 C2 120.58(13) . .
C4 C3 H3 119.7 . .
C2 C3 H3 119.7 . .
C3 C4 C5 119.27(14) . .
C3 C4 H4 120.4 . .
C5 C4 H4 120.4 . .
C6 C5 C4 120.80(15) . .
C6 C5 H5 119.6 . .
C4 C5 H5 119.6 . .
C5 C6 C1 119.82(15) . .
C5 C6 H6 120.1 . .
C1 C6 H6 120.1 . .
C8 C7 C12 120.06(13) . .
C8 C7 N2 117.96(12) . .
C12 C7 N2 121.97(12) . .
C9 C8 C7 119.89(13) . .
C9 C8 H8 120.1 . .
C7 C8 H8 120.1 . .
C10 C9 C8 120.23(13) . .
C10 C9 H9 119.9 . .
C8 C9 H9 119.9 . .
C9 C10 C11 119.68(14) . .
C9 C10 H10 120.2 . .
C11 C10 H10 120.2 . .
C12 C11 C10 120.71(14) . .
C12 C11 H11 119.6 . .
C10 C11 H11 119.6 . .
C11 C12 C7 119.39(13) . .
C11 C12 H12 120.3 . .
C7 C12 H12 120.3 . .
N4 C13 N3 125.76(12) . .
N4 C13 C14 115.90(12) . .
N3 C13 C14 117.09(12) . .
C15 C14 C19 118.44(14) . .
C15 C14 C13 121.75(13) . .
C19 C14 C13 119.78(14) . .
C14 C15 C16 120.40(16) . .
C14 C15 H15 119.8 . .
C16 C15 H15 119.8 . .
C15 C16 C17 121.00(17) . .
C15 C16 H16 119.5 . .
C17 C16 H16 119.5 . .
C18 C17 C16 118.36(16) . .
C18 C17 C20 120.3(2) . .
C16 C17 C20 121.4(2) . .
C17 C18 C19 121.03(18) . .
C17 C18 H18 119.5 . .
C19 C18 H18 119.5 . .
C18 C19 C14 120.77(17) . .
C18 C19 H19 119.6 . .
C14 C19 H19 119.6 . .
C17 C20 H20A 109.5 . .
C17 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
C17 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
Cl1 C21 Cl2 110.7(2) . .
Cl1 C21 Cl3 110.9(2) . .
Cl2 C21 Cl3 111.3(2) . .
Cl1 C21 H21 107.9 . .
Cl2 C21 H21 107.9 . .
Cl3 C21 H21 107.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd N2 2.0162(13) .
Pd N2 2.0162(13) 2_567
Pd N1 2.0265(13) .
Pd N1 2.0265(13) 2_567
Cl1 Cl3 0.667(2) 2_666
Cl1 C21 1.749(4) .
Cl1 C21 1.805(4) 2_666
Cl2 C21 1.755(4) .
Cl2 Cl3 2.353(2) 2_666
Cl3 C21 1.595(4) 2_666
Cl3 C21 1.757(4) .
N1 N4 1.2956(16) .
N1 C1 1.4235(17) .
N2 N3 1.2925(15) .
N2 C7 1.4208(18) .
N3 C13 1.3507(18) .
N4 C13 1.3426(18) .
C1 C2 1.3910(18) .
C1 C6 1.395(2) .
C2 C3 1.3943(19) .
C2 H2 0.9500 .
C3 C4 1.381(2) .
C3 H3 0.9500 .
C4 C5 1.390(2) .
C4 H4 0.9500 .
C5 C6 1.387(2) .
C5 H5 0.9500 .
C6 H6 0.9500 .
C7 C8 1.3958(18) .
C7 C12 1.3989(19) .
C8 C9 1.391(2) .
C8 H8 0.9500 .
C9 C10 1.389(2) .
C9 H9 0.9500 .
C10 C11 1.394(2) .
C10 H10 0.9500 .
C11 C12 1.388(2) .
C11 H11 0.9500 .
C12 H12 0.9500 .
C13 C14 1.4782(18) .
C14 C15 1.393(2) .
C14 C19 1.399(2) .
C15 C16 1.393(2) .
C15 H15 0.9500 .
C16 C17 1.397(3) .
C16 H16 0.9500 .
C17 C18 1.385(3) .
C17 C20 1.510(3) .
C18 C19 1.387(2) .
C18 H18 0.9500 .
C19 H19 0.9500 .
C20 H20A 0.9800 .
C20 H20B 0.9800 .
C20 H20C 0.9800 .
C21 H21 1.0000 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
C7 N2 N3 C13 167.14(11) .
Pd N2 N3 C13 -24.22(16) .
C1 N1 N4 C13 -164.70(12) .
Pd N1 N4 C13 22.37(17) .
N4 N1 C1 C2 166.01(12) .
Pd N1 C1 C2 -21.36(17) .
N4 N1 C1 C6 -13.7(2) .
Pd N1 C1 C6 158.95(14) .
C6 C1 C2 C3 -0.2(2) .
N1 C1 C2 C3 -179.93(13) .
C1 C2 C3 C4 -0.1(2) .
C2 C3 C4 C5 0.3(3) .
C3 C4 C5 C6 -0.1(3) .
C4 C5 C6 C1 -0.3(4) .
C2 C1 C6 C5 0.4(3) .
N1 C1 C6 C5 -179.87(19) .
N3 N2 C7 C8 -161.83(12) .
Pd N2 C7 C8 29.43(15) .
N3 N2 C7 C12 19.50(18) .
Pd N2 C7 C12 -149.24(10) .
C12 C7 C8 C9 1.5(2) .
N2 C7 C8 C9 -177.18(12) .
C7 C8 C9 C10 -0.1(2) .
C8 C9 C10 C11 -1.1(2) .
C9 C10 C11 C12 0.8(2) .
C10 C11 C12 C7 0.6(2) .
C8 C7 C12 C11 -1.8(2) .
N2 C7 C12 C11 176.84(12) .
N1 N4 C13 N3 22.5(2) .
N1 N4 C13 C14 -170.65(12) .
N2 N3 C13 N4 -21.7(2) .
N2 N3 C13 C14 171.60(12) .
N4 C13 C14 C15 -161.91(14) .
N3 C13 C14 C15 6.1(2) .
N4 C13 C14 C19 19.9(2) .
N3 C13 C14 C19 -172.14(14) .
C19 C14 C15 C16 0.0(3) .
C13 C14 C15 C16 -178.31(16) .
C14 C15 C16 C17 -0.4(3) .
C15 C16 C17 C18 0.6(4) .
C15 C16 C17 C20 -178.9(3) .
C16 C17 C18 C19 -0.3(4) .
C20 C17 C18 C19 179.2(3) .
C17 C18 C19 C14 -0.2(4) .
C15 C14 C19 C18 0.4(3) .
C13 C14 C19 C18 178.65(18) .
Cl3 Cl1 C21 Cl2 16.0(2) 2_666
C21 Cl1 C21 Cl2 102.4(3) 2_666
Cl3 Cl1 C21 Cl3 -108.0(3) 2_666
C21 Cl1 C21 Cl3 -21.69(11) 2_666
Cl3 Cl2 C21 Cl1 -6.04(9) 2_666
Cl3 Cl2 C21 Cl3 117.8(3) 2_666
Cl1 Cl3 C21 Cl1 119.2(3) 2_666
C21 Cl3 C21 Cl1 23.81(12) 2_666
Cl2 Cl3 C21 Cl1 -19.40(19) 2_666
Cl1 Cl3 C21 Cl2 -4.5(3) 2_666
C21 Cl3 C21 Cl2 -99.9(3) 2_666
Cl2 Cl3 C21 Cl2 -143.15(18) 2_666
