#------------------------------------------------------------------------------
#$Date: 2016-11-08 22:12:01 +0200 (Tue, 08 Nov 2016) $
#$Revision: 188255 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/57/7055783.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_7055783
loop_
_publ_author_name
'Yang, Jin'
_publ_section_title
;
 Mono- and dinuclear palladium(ii) complexes containing both
 N-heterocyclic carbenes and tetrazole ligands as catalysts for Hiyama
 coupling
;
_journal_issue                   11
_journal_name_full               'New J. Chem.'
_journal_page_first              9739
_journal_paper_doi               10.1039/C6NJ02320G
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C28 H38 Cl2 N6 Pd'
_chemical_formula_sum            'C28 H38 Cl2 N6 Pd'
_chemical_formula_weight         635.94
_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
_audit_update_record
;
2016-07-21 deposited with the CCDC.
2016-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.0270(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3005(5)
_cell_length_b                   16.0897(6)
_cell_length_c                   12.2535(4)
_cell_measurement_reflns_used    9449
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.5356
_cell_measurement_theta_min      2.9518
_cell_volume                     3012.36(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       'ω scans'
_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  0.0264
_diffrn_reflns_av_unetI/netI     0.0137
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            43968
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    0.821
_exptl_absorpt_correction_T_max  0.9224
_exptl_absorpt_correction_T_min  0.8799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         5250
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0448P)²+3.2271P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0761
_reflns_number_gt                4753
_reflns_number_total             5250
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6nj02320g2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 7055783--7055788.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7055783
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 0.712288(11) 0.898026(10) 0.171430(13) 0.02728(8) Uani 1 1 d .
Cl1 Cl 0.82879(5) 0.87953(4) 0.06456(6) 0.04863(17) Uani 1 1 d .
Cl2 Cl 0.59638(4) 0.91355(4) 0.28298(5) 0.04060(15) Uani 1 1 d .
N1 N 0.81418(12) 1.01944(12) 0.31301(14) 0.0289(4) Uani 1 1 d .
N2 N 0.77547(12) 1.07149(11) 0.15613(14) 0.0277(4) Uani 1 1 d .
N3 N 0.66032(14) 0.78785(13) 0.10648(18) 0.0401(5) Uani 1 1 d .
N4 N 0.61345(19) 0.73069(16) 0.1586(2) 0.0674(8) Uani 1 1 d .
N5 N 0.5898(2) 0.67206(19) 0.0916(3) 0.0831(10) Uani 1 1 d .
N6 N 0.62171(17) 0.69130(16) -0.0040(2) 0.0603(7) Uani 1 1 d .
H6 H 0.6149 0.6624 -0.0629 0.072 Uiso 1 1 calc R
C1 C 0.76676(13) 1.00313(13) 0.21910(17) 0.0259(4) Uani 1 1 d .
C2 C 0.85398(17) 1.09670(15) 0.3073(2) 0.0375(6) Uani 1 1 d .
H2 H 0.8910 1.1210 0.3608 0.045 Uiso 1 1 calc R
C3 C 0.82896(17) 1.12961(16) 0.2101(2) 0.0372(5) Uani 1 1 d .
H3 H 0.8445 1.1815 0.1839 0.045 Uiso 1 1 calc R
C4 C 0.81141(15) 0.97354(14) 0.41481(17) 0.0307(5) Uani 1 1 d .
C5 C 0.75665(16) 1.00510(15) 0.49358(19) 0.0361(5) Uani 1 1 d .
C6 C 0.7589(2) 0.96415(19) 0.5935(2) 0.0488(7) Uani 1 1 d .
H6A H 0.7242 0.9836 0.6482 0.059 Uiso 1 1 calc R
C7 C 0.8109(2) 0.89573(18) 0.6136(2) 0.0538(8) Uani 1 1 d .
H7 H 0.8113 0.8698 0.6815 0.065 Uiso 1 1 calc R
C8 C 0.86220(19) 0.86541(18) 0.5344(2) 0.0475(6) Uani 1 1 d .
H8 H 0.8960 0.8182 0.5487 0.057 Uiso 1 1 calc R
C9 C 0.86455(17) 0.90413(15) 0.4328(2) 0.0360(5) Uani 1 1 d .
C10 C 0.69792(18) 1.08036(18) 0.4734(2) 0.0444(6) Uani 1 1 d .
H10 H 0.6931 1.0902 0.3944 0.053 Uiso 1 1 calc R
C11 C 0.7378(2) 1.15845(19) 0.5275(3) 0.0592(8) Uani 1 1 d .
H11A H 0.7423 1.1510 0.6053 0.089 Uiso 1 1 calc R
H11B H 0.7010 1.2054 0.5098 0.089 Uiso 1 1 calc R
H11C H 0.7949 1.1679 0.5012 0.089 Uiso 1 1 calc R
C12 C 0.6058(2) 1.0657(2) 0.5111(3) 0.0668(9) Uani 1 1 d .
H12A H 0.6081 1.0578 0.5888 0.100 Uiso 1 1 calc R
H12B H 0.5814 1.0170 0.4758 0.100 Uiso 1 1 calc R
H12C H 0.5697 1.1129 0.4923 0.100 Uiso 1 1 calc R
C13 C 0.92521(18) 0.87090(17) 0.3492(2) 0.0439(6) Uani 1 1 d .
H13 H 0.9165 0.9043 0.2826 0.053 Uiso 1 1 calc R
C14 C 1.0204(2) 0.8800(3) 0.3905(3) 0.0685(9) Uani 1 1 d .
H14A H 1.0332 0.9377 0.4041 0.103 Uiso 1 1 calc R
H14B H 1.0579 0.8592 0.3365 0.103 Uiso 1 1 calc R
H14C H 1.0301 0.8491 0.4571 0.103 Uiso 1 1 calc R
C15 C 0.9040(3) 0.7802(2) 0.3200(3) 0.0711(10) Uani 1 1 d .
H15A H 0.9134 0.7460 0.3838 0.107 Uiso 1 1 calc R
H15B H 0.9413 0.7617 0.2643 0.107 Uiso 1 1 calc R
H15C H 0.8440 0.7759 0.2936 0.107 Uiso 1 1 calc R
C16 C 0.73007(16) 1.08680(14) 0.05123(18) 0.0310(5) Uani 1 1 d .
C17 C 0.64031(17) 1.10421(13) 0.0498(2) 0.0353(5) Uani 1 1 d .
C18 C 0.5986(2) 1.11975(18) -0.0527(2) 0.0496(7) Uani 1 1 d .
H18 H 0.5390 1.1315 -0.0574 0.060 Uiso 1 1 calc R
C19 C 0.6441(2) 1.1180(2) -0.1463(2) 0.0564(8) Uani 1 1 d .
H19 H 0.6146 1.1267 -0.2136 0.068 Uiso 1 1 calc R
C20 C 0.7321(2) 1.10357(18) -0.1415(2) 0.0526(8) Uani 1 1 d .
H20 H 0.7618 1.1046 -0.2057 0.063 Uiso 1 1 calc R
C21 C 0.77885(18) 1.08719(16) -0.0422(2) 0.0387(6) Uani 1 1 d .
C22 C 0.59066(18) 1.11180(16) 0.1529(2) 0.0422(6) Uani 1 1 d .
H22 H 0.6191 1.0746 0.2072 0.051 Uiso 1 1 calc R
C23 C 0.5977(3) 1.1995(2) 0.1992(3) 0.0724(10) Uani 1 1 d .
H23A H 0.6583 1.2134 0.2134 0.109 Uiso 1 1 calc R
H23B H 0.5678 1.2023 0.2660 0.109 Uiso 1 1 calc R
H23C H 0.5716 1.2380 0.1474 0.109 Uiso 1 1 calc R
C24 C 0.4949(2) 1.0853(2) 0.1394(3) 0.0665(9) Uani 1 1 d .
H24A H 0.4628 1.1255 0.0954 0.100 Uiso 1 1 calc R
H24B H 0.4706 1.0819 0.2099 0.100 Uiso 1 1 calc R
H24C H 0.4911 1.0320 0.1044 0.100 Uiso 1 1 calc R
C25 C 0.87685(19) 1.0760(2) -0.0407(2) 0.0496(7) Uani 1 1 d .
H25 H 0.8961 1.0539 0.0311 0.059 Uiso 1 1 calc R
C26 C 0.9215(2) 1.1601(2) -0.0547(3) 0.0721(10) Uani 1 1 d .
H26A H 0.9020 1.1840 -0.1235 0.108 Uiso 1 1 calc R
H26B H 0.9838 1.1524 -0.0530 0.108 Uiso 1 1 calc R
H26C H 0.9068 1.1965 0.0036 0.108 Uiso 1 1 calc R
C27 C 0.9065(3) 1.0148(2) -0.1280(3) 0.0707(10) Uani 1 1 d .
H27A H 0.8802 0.9615 -0.1171 0.106 Uiso 1 1 calc R
H27B H 0.9690 1.0095 -0.1221 0.106 Uiso 1 1 calc R
H27C H 0.8887 1.0354 -0.1993 0.106 Uiso 1 1 calc R
C28 C 0.66518(18) 0.76140(17) 0.0057(2) 0.0480(6) Uani 1 1 d .
H28 H 0.6944 0.7878 -0.0493 0.058 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
C1 Pd1 N3 174.42(8)
C1 Pd1 Cl1 87.18(6)
N3 Pd1 Cl1 87.93(6)
C1 Pd1 Cl2 93.33(6)
N3 Pd1 Cl2 91.64(6)
Cl1 Pd1 Cl2 178.22(3)
C1 N1 C2 110.37(18)
C1 N1 C4 126.39(18)
C2 N1 C4 122.10(18)
C1 N2 C3 110.44(18)
C1 N2 C16 125.90(18)
C3 N2 C16 123.45(19)
C28 N3 N4 106.4(2)
C28 N3 Pd1 126.59(19)
N4 N3 Pd1 126.96(17)
N5 N4 N3 109.6(3)
N4 N5 N6 106.7(2)
C28 N6 N5 109.2(2)
N1 C1 N2 105.23(18)
N1 C1 Pd1 128.38(16)
N2 C1 Pd1 125.73(15)
C3 C2 N1 107.0(2)
C2 C3 N2 106.9(2)
C9 C4 C5 123.0(2)
C9 C4 N1 120.1(2)
C5 C4 N1 116.8(2)
C6 C5 C4 116.5(2)
C6 C5 C10 120.5(2)
C4 C5 C10 123.0(2)
C7 C6 C5 121.7(3)
C8 C7 C6 120.4(3)
C7 C8 C9 121.1(3)
C8 C9 C4 117.2(2)
C8 C9 C13 119.4(2)
C4 C9 C13 123.3(2)
C5 C10 C11 111.4(2)
C5 C10 C12 112.1(3)
C11 C10 C12 110.5(2)
C14 C13 C9 110.5(2)
C14 C13 C15 110.9(3)
C9 C13 C15 111.4(3)
C17 C16 C21 123.6(2)
C17 C16 N2 117.9(2)
C21 C16 N2 118.4(2)
C16 C17 C18 116.5(2)
C16 C17 C22 122.8(2)
C18 C17 C22 120.6(3)
C19 C18 C17 121.3(3)
C20 C19 C18 120.7(3)
C19 C20 C21 121.8(3)
C16 C21 C20 116.1(3)
C16 C21 C25 124.1(2)
C20 C21 C25 119.6(2)
C17 C22 C23 110.9(2)
C17 C22 C24 114.1(3)
C23 C22 C24 110.4(3)
C21 C25 C26 110.0(3)
C21 C25 C27 113.4(3)
C26 C25 C27 109.7(3)
N6 C28 N3 108.1(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pd1 C1 1.961(2)
Pd1 N3 2.084(2)
Pd1 Cl1 2.2864(7)
Pd1 Cl2 2.3091(6)
N1 C1 1.353(3)
N1 C2 1.388(3)
N1 C4 1.452(3)
N2 C1 1.354(3)
N2 C3 1.387(3)
N2 C16 1.450(3)
N3 C28 1.313(3)
N3 N4 1.348(3)
N4 N5 1.290(4)
N5 N6 1.330(4)
N6 C28 1.312(4)
C2 C3 1.341(3)
C4 C9 1.392(3)
C4 C5 1.406(3)
C5 C6 1.389(4)
C5 C10 1.520(4)
C6 C7 1.374(4)
C7 C8 1.370(4)
C8 C9 1.394(4)
C9 C13 1.516(4)
C10 C11 1.532(4)
C10 C12 1.525(4)
C13 C14 1.524(4)
C13 C15 1.534(4)
C16 C17 1.401(4)
C16 C21 1.400(4)
C17 C18 1.401(4)
C17 C22 1.512(4)
C18 C19 1.373(5)
C19 C20 1.364(5)
C20 C21 1.403(4)
C21 C25 1.510(4)
C22 C23 1.522(4)
C22 C24 1.526(4)
C25 C26 1.530(5)
C25 C27 1.539(4)
