#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:21:28 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179839 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/35/7013527.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_7013527
loop_
_publ_author_name
'Steel, Peter J.'
'Sumby, Christopher J.'
_publ_section_title
;
 Coordination chemistry of di-2-pyridylmethane and related bridging
 ligands with silver(i), copper(ii), palladium(ii) and zinc(ii)
;
_journal_issue                   23
_journal_name_full               'Dalton Transactions'
_journal_page_first              4505
_journal_paper_doi               10.1039/b309479k
_journal_year                    2003
_chemical_formula_sum            'C30 H40 N4 O14 Pd2'
_chemical_formula_weight         893.46
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 125.925(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.644(8)
_cell_length_b                   15.938(6)
_cell_length_c                   14.847(6)
_cell_measurement_reflns_used    4225
_cell_measurement_temperature    168(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.56
_cell_volume                     3764(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      168(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0195
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            12495
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    1.023
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.752192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-38'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3285
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      2.231
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0230
_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)+(0.0381P)²+2.1518P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0634
_reflns_number_gt                2908
_reflns_number_total             3285
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b309479k.txt
_cod_data_source_block           Compound-23
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7013527
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.11233(2) 0.35323(2) 0.71486(3) 0.02429(17) Uani 1 1 d . . .
C1 C 0.0009(3) 0.4866(3) 0.5434(4) 0.0234(10) Uani 1 1 d . . .
N11 N -0.0146(3) 0.3525(2) 0.6063(3) 0.0239(9) Uani 1 1 d . . .
C12 C -0.0542(3) 0.4169(3) 0.5335(3) 0.0241(10) Uani 1 1 d . . .
C13 C -0.1406(3) 0.4180(3) 0.4552(4) 0.0292(11) Uani 1 1 d . . .
H13A H -0.1672 0.4644 0.4062 0.035 Uiso 1 1 calc R . .
C14 C -0.1879(3) 0.3506(3) 0.4490(4) 0.0345(12) Uani 1 1 d . . .
H14A H -0.2472 0.3498 0.3951 0.041 Uiso 1 1 calc R . .
C15 C -0.1473(3) 0.2846(3) 0.5226(4) 0.0315(11) Uani 1 1 d . . .
H15A H -0.1783 0.2377 0.5199 0.038 Uiso 1 1 calc R . .
C16 C -0.0609(3) 0.2876(3) 0.6003(4) 0.0275(11) Uani 1 1 d . . .
H16A H -0.0335 0.2424 0.6511 0.033 Uiso 1 1 calc R . .
N21 N 0.1089(2) 0.4766(2) 0.7423(3) 0.0252(9) Uani 1 1 d . . .
C22 C 0.0548(3) 0.5277(3) 0.6552(4) 0.0247(10) Uani 1 1 d . . .
C23 C 0.0496(3) 0.6127(3) 0.6699(4) 0.0307(11) Uani 1 1 d . . .
H23A H 0.0106 0.6471 0.6084 0.037 Uiso 1 1 calc R . .
C24 C 0.1020(4) 0.6468(3) 0.7755(5) 0.0393(13) Uani 1 1 d . . .
H24A H 0.0995 0.7050 0.7873 0.047 Uiso 1 1 calc R . .
C25 C 0.1580(4) 0.5949(4) 0.8632(4) 0.0400(13) Uani 1 1 d . . .
H25A H 0.1948 0.6173 0.9361 0.048 Uiso 1 1 calc R . .
C26 C 0.1605(3) 0.5104(3) 0.8448(4) 0.0330(11) Uani 1 1 d . . .
H26A H 0.1993 0.4753 0.9057 0.040 Uiso 1 1 calc R . .
O30 O 0.2384(2) 0.3512(2) 0.8261(3) 0.0357(9) Uani 1 1 d . . .
C30 C 0.3751(4) 0.3754(4) 0.8762(6) 0.0603(19) Uani 1 1 d . . .
H30A H 0.4026 0.4030 0.8464 0.090 Uiso 1 1 calc R . .
H30B H 0.3895 0.3156 0.8875 0.090 Uiso 1 1 calc R . .
H30C H 0.3944 0.4011 0.9474 0.090 Uiso 1 1 calc R . .
C31 C 0.2806(3) 0.3853(3) 0.7947(5) 0.0380(13) Uani 1 1 d . . .
O31 O 0.2488(2) 0.4240(3) 0.7071(3) 0.0516(11) Uani 1 1 d . . .
O40 O 0.1181(2) 0.2279(2) 0.6966(3) 0.0339(8) Uani 1 1 d . . .
O41 O 0.0841(3) 0.2455(2) 0.5260(3) 0.0543(12) Uani 1 1 d . . .
C40 C 0.1210(5) 0.1074(4) 0.6052(6) 0.0615(19) Uani 1 1 d . . .
H40A H 0.1111 0.0920 0.5345 0.092 Uiso 1 1 calc R . .
H40B H 0.0822 0.0761 0.6139 0.092 Uiso 1 1 calc R . .
H40C H 0.1791 0.0936 0.6667 0.092 Uiso 1 1 calc R . .
C41 C 0.1064(3) 0.2013(3) 0.6060(4) 0.0373(12) Uani 1 1 d . . .
O50 O 0.0765(4) 0.1683(3) 0.3511(5) 0.0687(14) Uani 1 1 d D . .
H50A H 0.083(6) 0.188(6) 0.406(5) 0.103 Uiso 1 1 d D . .
H50B H 0.029(3) 0.154(6) 0.316(8) 0.103 Uiso 1 1 d D . .
O60 O 0.0849(3) 0.1138(3) 0.8132(4) 0.0508(11) Uani 1 1 d D . .
H60A H 0.094(5) 0.145(4) 0.777(6) 0.076 Uiso 1 1 d D . .
H60B H 0.109(5) 0.068(3) 0.832(6) 0.076 Uiso 1 1 d D . .
O70 O 0.3248(3) 0.4691(3) 0.6062(4) 0.0502(11) Uani 1 1 d D . .
H70A H 0.306(5) 0.458(5) 0.641(6) 0.075 Uiso 1 1 d D . .
H70B H 0.361(4) 0.435(4) 0.633(6) 0.075 Uiso 1 1 d D . .
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
_geom_angle_publ_flag
O30 Pd1 N21 91.20(15) . . ?
O30 Pd1 N11 178.14(14) . . ?
N21 Pd1 N11 89.70(15) . . ?
O30 Pd1 O40 87.45(14) . . ?
N21 Pd1 O40 176.61(13) . . ?
N11 Pd1 O40 91.57(14) . . ?
C1 C1 C12 122.2(5) 5_566 . ?
C1 C1 C22 122.0(5) 5_566 . ?
C12 C1 C22 115.7(4) . . ?
C16 N11 C12 118.6(4) . . ?
C16 N11 Pd1 121.8(3) . . ?
C12 N11 Pd1 119.5(3) . . ?
N11 C12 C13 121.7(4) . . ?
N11 C12 C1 116.1(4) . . ?
C13 C12 C1 122.2(4) . . ?
C12 C13 C14 119.3(5) . . ?
C15 C14 C13 118.9(5) . . ?
C16 C15 C14 119.2(5) . . ?
N11 C16 C15 122.2(4) . . ?
C26 N21 C22 118.9(4) . . ?
C26 N21 Pd1 121.7(3) . . ?
C22 N21 Pd1 119.4(3) . . ?
N21 C22 C23 121.6(4) . . ?
N21 C22 C1 116.2(4) . . ?
C23 C22 C1 122.2(4) . . ?
C24 C23 C22 119.2(5) . . ?
C25 C24 C23 118.9(5) . . ?
C26 C25 C24 119.9(5) . . ?
N21 C26 C25 121.5(5) . . ?
C31 O30 Pd1 116.1(3) . . ?
O31 C31 O30 124.1(5) . . ?
O31 C31 C30 121.4(5) . . ?
O30 C31 C30 114.5(5) . . ?
C41 O40 Pd1 118.1(3) . . ?
O41 C41 O40 124.4(5) . . ?
O41 C41 C40 121.4(5) . . ?
O40 C41 C40 114.2(5) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 O30 2.016(4) . ?
Pd1 N21 2.017(4) . ?
Pd1 N11 2.024(4) . ?
Pd1 O40 2.028(4) . ?
C1 C1 1.339(9) 5_566 ?
C1 C12 1.497(7) . ?
C1 C22 1.497(6) . ?
N11 C16 1.346(6) . ?
N11 C12 1.357(6) . ?
C12 C13 1.385(6) . ?
C13 C14 1.388(7) . ?
C14 C15 1.384(7) . ?
C15 C16 1.383(7) . ?
N21 C26 1.351(6) . ?
N21 C22 1.361(6) . ?
C22 C23 1.386(7) . ?
C23 C24 1.385(7) . ?
C24 C25 1.383(8) . ?
C25 C26 1.380(8) . ?
O30 C31 1.285(7) . ?
C30 C31 1.517(8) . ?
C31 O31 1.229(7) . ?
O40 C41 1.296(6) . ?
O41 C41 1.221(6) . ?
C40 C41 1.525(8) . ?
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
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O30 Pd1 N11 C16 -23(5) . . . . ?
N21 Pd1 N11 C16 -141.3(4) . . . . ?
O40 Pd1 N11 C16 35.6(4) . . . . ?
O30 Pd1 N11 C12 161(4) . . . . ?
N21 Pd1 N11 C12 42.1(3) . . . . ?
O40 Pd1 N11 C12 -141.1(3) . . . . ?
C16 N11 C12 C13 1.1(7) . . . . ?
Pd1 N11 C12 C13 177.8(3) . . . . ?
C16 N11 C12 C1 -179.2(4) . . . . ?
Pd1 N11 C12 C1 -2.5(5) . . . . ?
C1 C1 C12 N11 126.5(6) 5_566 . . . ?
C22 C1 C12 N11 -56.7(5) . . . . ?
C1 C1 C12 C13 -53.8(8) 5_566 . . . ?
C22 C1 C12 C13 123.0(5) . . . . ?
N11 C12 C13 C14 -1.5(7) . . . . ?
C1 C12 C13 C14 178.8(4) . . . . ?
C12 C13 C14 C15 0.9(7) . . . . ?
C13 C14 C15 C16 0.1(7) . . . . ?
C12 N11 C16 C15 0.0(7) . . . . ?
Pd1 N11 C16 C15 -176.7(4) . . . . ?
C14 C15 C16 N11 -0.6(7) . . . . ?
O30 Pd1 N21 C26 -37.4(4) . . . . ?
N11 Pd1 N21 C26 141.0(4) . . . . ?
O40 Pd1 N21 C26 29(3) . . . . ?
O30 Pd1 N21 C22 141.0(4) . . . . ?
N11 Pd1 N21 C22 -40.6(4) . . . . ?
O40 Pd1 N21 C22 -153(2) . . . . ?
C26 N21 C22 C23 -2.1(7) . . . . ?
Pd1 N21 C22 C23 179.5(4) . . . . ?
C26 N21 C22 C1 178.6(4) . . . . ?
Pd1 N21 C22 C1 0.1(5) . . . . ?
C1 C1 C22 N21 -125.0(6) 5_566 . . . ?
C12 C1 C22 N21 58.2(6) . . . . ?
C1 C1 C22 C23 55.7(8) 5_566 . . . ?
C12 C1 C22 C23 -121.1(5) . . . . ?
N21 C22 C23 C24 1.4(8) . . . . ?
C1 C22 C23 C24 -179.3(5) . . . . ?
C22 C23 C24 C25 0.0(8) . . . . ?
C23 C24 C25 C26 -0.6(9) . . . . ?
C22 N21 C26 C25 1.5(7) . . . . ?
Pd1 N21 C26 C25 179.9(4) . . . . ?
C24 C25 C26 N21 -0.1(9) . . . . ?
N21 Pd1 O30 C31 -74.3(4) . . . . ?
N11 Pd1 O30 C31 167(4) . . . . ?
O40 Pd1 O30 C31 108.9(4) . . . . ?
Pd1 O30 C31 O31 6.3(8) . . . . ?
Pd1 O30 C31 C30 -174.5(4) . . . . ?
O30 Pd1 O40 C41 -106.5(4) . . . . ?
N21 Pd1 O40 C41 -173(2) . . . . ?
N11 Pd1 O40 C41 75.1(4) . . . . ?
Pd1 O40 C41 O41 -7.4(8) . . . . ?
Pd1 O40 C41 C40 173.9(4) . . . . ?
