#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:56:22 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178674 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/85/4078584.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_4078584
loop_
_publ_author_name
'Guo, Shuai'
'Huynh, Han Vinh'
_publ_section_title
;
 Dipalladium Complexes with Triazolidin-Diylidene Bridges and Their
 Catalytic Activities
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              4565
_journal_paper_doi               10.1021/om3003625
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C30 H42 N4 O4 Pd'
_chemical_formula_weight         629.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.9882(9)
_cell_length_b                   9.9514(5)
_cell_length_c                   18.5623(10)
_cell_measurement_reflns_used    2168
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      22.51
_cell_measurement_theta_min      2.50
_cell_volume                     3138.1(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0681
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20932
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    0.630
_exptl_absorpt_correction_T_max  0.9283
_exptl_absorpt_correction_T_min  0.8051
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2001)'
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3595
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0465
_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)+(0.0348P)²+2.7885P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1062
_reflns_number_gt                2371
_reflns_number_total             3595
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3003625_si_002.cif
_cod_data_source_block           b234a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'Not Measured' 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_original_sg_symbol_H-M      Pbca
_cod_database_code               4078584
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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 0.0000 0.5000 0.5000 0.02394(11) Uani 1 2 d S
O1 O -0.03078(15) 0.6946(2) 0.49055(11) 0.0319(5) Uani 1 1 d .
O2 O -0.0862(2) 0.6764(3) 0.38268(17) 0.0718(10) Uani 1 1 d .
N1 N 0.13267(15) 0.5947(3) 0.40159(14) 0.0267(6) Uani 1 1 d .
N2 N 0.06780(14) 0.4295(3) 0.35371(13) 0.0230(6) Uani 1 1 d .
C1 C 0.07079(18) 0.5112(3) 0.41195(17) 0.0244(7) Uani 1 1 d .
C2 C 0.17032(17) 0.5658(3) 0.33668(17) 0.0255(7) Uani 1 1 d .
C3 C 0.23554(19) 0.6215(3) 0.30213(19) 0.0348(8) Uani 1 1 d .
H3 H 0.2630 0.6942 0.3224 0.042 Uiso 1 1 calc R
C4 C 0.25829(19) 0.5667(4) 0.23751(19) 0.0384(9) Uani 1 1 d .
H4 H 0.3024 0.6016 0.2133 0.046 Uiso 1 1 calc R
C5 C 0.2169(2) 0.4602(4) 0.2075(2) 0.0389(9) Uani 1 1 d .
H5 H 0.2343 0.4244 0.1634 0.047 Uiso 1 1 calc R
C6 C 0.15110(19) 0.4044(3) 0.24005(17) 0.0308(8) Uani 1 1 d .
H6 H 0.1232 0.3330 0.2189 0.037 Uiso 1 1 calc R
C7 C 0.12867(18) 0.4598(3) 0.30551(17) 0.0234(7) Uani 1 1 d .
C8 C 0.1549(2) 0.7010(3) 0.45348(19) 0.0349(8) Uani 1 1 d .
H8 H 0.1143 0.7018 0.4917 0.042 Uiso 1 1 calc R
C9 C 0.2324(3) 0.6684(5) 0.4892(2) 0.0666(14) Uani 1 1 d .
H9A H 0.2285 0.5820 0.5132 0.100 Uiso 1 1 calc R
H9B H 0.2449 0.7374 0.5243 0.100 Uiso 1 1 calc R
H9C H 0.2736 0.6647 0.4530 0.100 Uiso 1 1 calc R
C10 C 0.1539(2) 0.8388(4) 0.4182(2) 0.0523(11) Uani 1 1 d .
H10A H 0.1962 0.8445 0.3832 0.078 Uiso 1 1 calc R
H10B H 0.1611 0.9075 0.4547 0.078 Uiso 1 1 calc R
H10C H 0.1038 0.8523 0.3942 0.078 Uiso 1 1 calc R
C11 C 0.00455(18) 0.3295(3) 0.34275(18) 0.0280(7) Uani 1 1 d .
H11 H -0.0299 0.3331 0.3857 0.034 Uiso 1 1 calc R
C12 C 0.0372(2) 0.1883(3) 0.3384(2) 0.0460(10) Uani 1 1 d .
H12A H 0.0677 0.1786 0.2945 0.069 Uiso 1 1 calc R
H12B H -0.0059 0.1243 0.3381 0.069 Uiso 1 1 calc R
H12C H 0.0707 0.1715 0.3797 0.069 Uiso 1 1 calc R
C13 C -0.0459(2) 0.3672(4) 0.2782(2) 0.0488(10) Uani 1 1 d .
H13A H -0.0631 0.4597 0.2829 0.073 Uiso 1 1 calc R
H13B H -0.0915 0.3087 0.2761 0.073 Uiso 1 1 calc R
H13C H -0.0153 0.3572 0.2344 0.073 Uiso 1 1 calc R
C14 C -0.06484(19) 0.7413(3) 0.43497(18) 0.0292(7) Uani 1 1 d .
C15 C -0.0748(2) 0.8918(3) 0.4372(2) 0.0393(9) Uani 1 1 d .
H15A H -0.0390 0.9332 0.4030 0.059 Uiso 1 1 calc R
H15B H -0.0631 0.9242 0.4853 0.059 Uiso 1 1 calc R
H15C H -0.1286 0.9148 0.4247 0.059 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'
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
O1 Pd1 O1 180.00(12) . 5_566
O1 Pd1 C1 88.23(10) . 5_566
O1 Pd1 C1 91.77(10) 5_566 5_566
O1 Pd1 C1 91.77(10) . .
O1 Pd1 C1 88.23(10) 5_566 .
C1 Pd1 C1 180.0 5_566 .
C14 O1 Pd1 122.8(2) . .
C1 N1 C2 110.6(3) . .
C1 N1 C8 123.0(3) . .
C2 N1 C8 126.4(3) . .
C1 N2 C7 110.7(3) . .
C1 N2 C11 122.8(3) . .
C7 N2 C11 126.4(2) . .
N2 C1 N1 106.5(3) . .
N2 C1 Pd1 126.0(2) . .
N1 C1 Pd1 127.4(2) . .
N1 C2 C3 132.8(3) . .
N1 C2 C7 106.4(3) . .
C3 C2 C7 120.8(3) . .
C4 C3 C2 117.8(3) . .
C3 C4 C5 120.7(3) . .
C6 C5 C4 122.7(3) . .
C5 C6 C7 116.3(3) . .
C6 C7 C2 121.6(3) . .
C6 C7 N2 132.6(3) . .
C2 C7 N2 105.8(3) . .
N1 C8 C9 110.8(3) . .
N1 C8 C10 111.2(3) . .
C9 C8 C10 113.2(3) . .
N2 C11 C12 111.5(3) . .
N2 C11 C13 110.6(3) . .
C12 C11 C13 113.2(3) . .
O2 C14 O1 125.9(3) . .
O2 C14 C15 120.9(3) . .
O1 C14 C15 113.1(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 O1 2.013(2) .
Pd1 O1 2.013(2) 5_566
Pd1 C1 2.032(3) 5_566
Pd1 C1 2.032(3) .
O1 C14 1.271(4) .
O2 C14 1.221(4) .
N1 C1 1.354(4) .
N1 C2 1.394(4) .
N1 C8 1.480(4) .
N2 C1 1.354(4) .
N2 C7 1.400(4) .
N2 C11 1.479(4) .
C2 C3 1.395(4) .
C2 C7 1.396(4) .
C3 C4 1.373(5) .
C4 C5 1.388(5) .
C5 C6 1.387(5) .
C6 C7 1.388(4) .
C8 C9 1.510(5) .
C8 C10 1.519(5) .
C11 C12 1.512(5) .
C11 C13 1.520(5) .
C14 C15 1.507(4) .
