#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:23:38 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180076 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/22/7052240.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_7052240
loop_
_publ_author_name
'Madalan, Augustin M.'
'Avarvari, Narcis'
'Andruh, Marius'
_publ_section_title
;
 Metal complexes as second-sphere ligands
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              521
_journal_paper_doi               10.1039/b517989k
_journal_volume                  30
_journal_year                    2006
_chemical_formula_sum            'C33 H35 Cl Cu N4 O11 Pd'
_chemical_formula_weight         869.04
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 105.49
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.987
_cell_length_b                   36.016
_cell_length_c                   8.417
_cell_measurement_reflns_used    215
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.5
_cell_volume                     3501.828
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       KappaCCD
_computing_data_reduction        'Denzo and Scalepak'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  area_detector
_diffrn_measurement_method       omega-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0766
_diffrn_reflns_av_sigmaI/netI    0.1469
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            19313
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.70
_exptl_absorpt_coefficient_mu    1.263
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.677792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       prism
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         7689
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1762
_refine_ls_R_factor_gt           0.0670
_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)+(0.0566P)²+0.0186P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1481
_reflns_number_gt                3636
_reflns_number_total             7689
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b517989k.txt
_cod_data_source_block           mam107
_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_cell_volume        3501.8
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7052240
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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6992(5) 0.25984(17) 0.4544(7) 0.0648(18) Uani 1 1 d . . .
H1A H 0.6249 0.2647 0.3793 0.097 Uiso 1 1 calc R . .
H1B H 0.7442 0.2822 0.4720 0.097 Uiso 1 1 calc R . .
H1C H 0.6889 0.2513 0.5575 0.097 Uiso 1 1 calc R . .
C2 C 0.8671(5) 0.22183(17) 0.4742(7) 0.0476(15) Uani 1 1 d . . .
C3 C 0.9306(6) 0.24111(19) 0.6108(7) 0.0613(18) Uani 1 1 d . . .
H3 H 0.9017 0.2628 0.6449 0.074 Uiso 1 1 calc R . .
C4 C 1.0404(6) 0.2271(2) 0.6975(8) 0.075(2) Uani 1 1 d . . .
H4 H 1.0826 0.2392 0.7920 0.090 Uiso 1 1 calc R . .
C5 C 1.0842(5) 0.1968(2) 0.6453(8) 0.068(2) Uani 1 1 d . . .
H5 H 1.1576 0.1887 0.7025 0.082 Uiso 1 1 calc R . .
C6 C 1.0222(5) 0.17683(19) 0.5060(7) 0.0529(17) Uani 1 1 d . . .
C7 C 0.9096(5) 0.18939(17) 0.4173(7) 0.0444(15) Uani 1 1 d . . .
C8 C 1.0723(6) 0.1434(2) 0.4667(9) 0.068(2) Uani 1 1 d . . .
H8 H 1.1470 0.1382 0.5299 0.082 Uiso 1 1 calc R . .
C9 C 1.0922(7) 0.0869(2) 0.3244(10) 0.097(3) Uani 1 1 d . . .
H9A H 1.1391 0.0935 0.2509 0.117 Uiso 1 1 calc R . .
H9B H 1.1433 0.0781 0.4272 0.117 Uiso 1 1 calc R . .
C10 C 1.0114(7) 0.0579(2) 0.2505(12) 0.107(3) Uani 1 1 d . . .
H10A H 0.9925 0.0433 0.3367 0.128 Uiso 1 1 calc R . .
H10B H 1.0473 0.0415 0.1871 0.128 Uiso 1 1 calc R . .
C11 C 0.8382(7) 0.05424(19) 0.0249(10) 0.068(2) Uani 1 1 d . . .
H11 H 0.8656 0.0312 0.0029 0.082 Uiso 1 1 calc R . .
C12 C 0.7268(7) 0.06523(18) -0.0738(8) 0.0589(18) Uani 1 1 d . . .
C13 C 0.6688(8) 0.0396(2) -0.1971(10) 0.082(2) Uani 1 1 d . . .
H13 H 0.7054 0.0177 -0.2129 0.099 Uiso 1 1 calc R . .
C14 C 0.5596(9) 0.0471(2) -0.2926(9) 0.087(3) Uani 1 1 d . . .
H14 H 0.5226 0.0302 -0.3732 0.105 Uiso 1 1 calc R . .
C15 C 0.5035(7) 0.0794(2) -0.2707(8) 0.074(2) Uani 1 1 d . . .
H15 H 0.4291 0.0840 -0.3361 0.089 Uiso 1 1 calc R . .
C16 C 0.5570(6) 0.1048(2) -0.1526(7) 0.0604(18) Uani 1 1 d . . .
C17 C 0.6710(6) 0.09848(19) -0.0519(7) 0.0519(16) Uani 1 1 d . . .
C18 C 0.3911(6) 0.1443(2) -0.1948(8) 0.085(2) Uani 1 1 d . . .
H18A H 0.3706 0.1683 -0.1618 0.128 Uiso 1 1 calc R . .
H18B H 0.3443 0.1257 -0.1623 0.128 Uiso 1 1 calc R . .
H18C H 0.3781 0.1438 -0.3124 0.128 Uiso 1 1 calc R . .
C19 C 0.7200(5) 0.16488(17) 0.6585(7) 0.0499(15) Uani 1 1 d . . .
H19 H 0.6833 0.1869 0.6729 0.060 Uiso 1 1 calc R . .
C20 C 0.8276(5) 0.15746(19) 0.7596(7) 0.0538(17) Uani 1 1 d . . .
H20 H 0.8629 0.1740 0.8428 0.065 Uiso 1 1 calc R . .
C21 C 0.8822(6) 0.1257(2) 0.7369(8) 0.0621(19) Uani 1 1 d . . .
H21 H 0.9560 0.1205 0.8032 0.074 Uiso 1 1 calc R . .
C22 C 0.8290(5) 0.10149(18) 0.6180(8) 0.0514(16) Uani 1 1 d . . .
H22 H 0.8658 0.0795 0.6036 0.062 Uiso 1 1 calc R . .
C23 C 0.7199(5) 0.10944(16) 0.5177(7) 0.0439(15) Uani 1 1 d . . .
C24 C 0.6505(5) 0.08509(15) 0.3889(7) 0.0415(14) Uani 1 1 d . . .
C25 C 0.6864(6) 0.05054(17) 0.3503(8) 0.0563(17) Uani 1 1 d . . .
H25 H 0.7595 0.0417 0.4043 0.068 Uiso 1 1 calc R . .
C26 C 0.6122(7) 0.02939(18) 0.2303(9) 0.0677(19) Uani 1 1 d . . .
H26 H 0.6349 0.0061 0.2033 0.081 Uiso 1 1 calc R . .
C27 C 0.5055(7) 0.04295(17) 0.1519(8) 0.0630(19) Uani 1 1 d . . .
H27 H 0.4542 0.0290 0.0716 0.076 Uiso 1 1 calc R . .
C28 C 0.4753(5) 0.07785(17) 0.1944(7) 0.0531(16) Uani 1 1 d . . .
H28 H 0.4029 0.0873 0.1403 0.064 Uiso 1 1 calc R . .
C29 C 0.1690(5) 0.16770(19) 0.0990(7) 0.071(2) Uani 1 1 d . . .
H29A H 0.1771 0.1476 0.0282 0.106 Uiso 1 1 calc R . .
H29B H 0.1538 0.1903 0.0361 0.106 Uiso 1 1 calc R . .
H29C H 0.1058 0.1626 0.1459 0.106 Uiso 1 1 calc R . .
C30 C 0.2785(5) 0.17183(18) 0.2343(7) 0.0491(16) Uani 1 1 d . . .
C31 C 0.2891(5) 0.19954(18) 0.3485(8) 0.0598(17) Uani 1 1 d . . .
H31 H 0.2225 0.2131 0.3451 0.072 Uiso 1 1 calc R . .
C32 C 0.3881(5) 0.20973(16) 0.4689(7) 0.0498(16) Uani 1 1 d . . .
C33 C 0.3862(6) 0.24173(19) 0.5781(8) 0.084(2) Uani 1 1 d . . .
H33A H 0.4617 0.2451 0.6521 0.126 Uiso 1 1 calc R . .
H33B H 0.3312 0.2372 0.6404 0.126 Uiso 1 1 calc R . .
H33C H 0.3644 0.2637 0.5127 0.126 Uiso 1 1 calc R . .
N1 N 1.0275(4) 0.11968(16) 0.3556(7) 0.0574(14) Uani 1 1 d . . .
N2 N 0.9041(5) 0.07354(15) 0.1416(7) 0.0640(15) Uani 1 1 d . . .
N3 N 0.6662(4) 0.14142(13) 0.5399(5) 0.0418(12) Uani 1 1 d . . .
N4 N 0.5453(4) 0.09844(12) 0.3092(5) 0.0440(12) Uani 1 1 d . . .
O1 O 0.7580(3) 0.23202(11) 0.3862(4) 0.0527(10) Uani 1 1 d . . .
O2 O 0.8420(3) 0.17326(10) 0.2870(4) 0.0462(10) Uani 1 1 d . . .
O1W O 0.5865(5) 0.17996(16) 0.1887(7) 0.0514(12) Uani 1 1 d . . .
O3 O 0.5092(4) 0.13721(14) -0.1182(5) 0.0666(13) Uani 1 1 d . . .
O4 O 0.7136(3) 0.12467(11) 0.0566(4) 0.0492(10) Uani 1 1 d . . .
O5 O 0.3584(3) 0.14896(12) 0.2317(5) 0.0588(11) Uani 1 1 d . . .
O6 O 0.4847(3) 0.19302(11) 0.4938(4) 0.0551(11) Uani 1 1 d . . .
O7 O 0.2201(7) 0.0404(2) 0.9535(11) 0.209(4) Uani 1 1 d . . .
O8 O 0.1459(6) 0.08849(17) 0.7882(11) 0.183(4) Uani 1 1 d . . .
O9 O 0.0368(6) 0.03983(18) 0.8005(13) 0.209(4) Uani 1 1 d . . .
O10 O 0.1844(11) 0.0353(3) 0.6996(12) 0.282(6) Uani 1 1 d . . .
Pd1 Pd 0.87139(4) 0.122864(13) 0.20871(5) 0.04750(18) Uani 1 1 d . . .
Cu2 Cu 0.51329(6) 0.149695(19) 0.37644(8) 0.0454(2) Uani 1 1 d . . .
Cl3 Cl 0.14672(17) 0.05152(6) 0.8162(3) 0.0792(6) Uani 1 1 d . . .
H1W H 0.649(5) 0.1860(15) 0.233(6) 0.04(2) Uiso 1 1 d . . .
H2W H 0.593(8) 0.165(2) 0.139(10) 0.12(5) Uiso 1 1 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'
Cu Cu 0.3201 1.2651 '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'
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
O1 C2 C3 123.3(6) . . ?
O1 C2 C7 114.7(5) . . ?
C3 C2 C7 122.1(6) . . ?
C2 C3 C4 118.6(7) . . ?
C5 C4 C3 120.9(7) . . ?
C4 C5 C6 121.7(7) . . ?
C5 C6 C8 117.7(6) . . ?
C5 C6 C7 119.2(6) . . ?
C8 C6 C7 123.0(6) . . ?
O2 C7 C2 116.9(5) . . ?
O2 C7 C6 125.6(6) . . ?
C2 C7 C6 117.4(6) . . ?
N1 C8 C6 128.0(6) . . ?
C10 C9 N1 109.4(7) . . ?
C9 C10 N2 111.3(6) . . ?
N2 C11 C12 125.6(6) . . ?
C17 C12 C13 119.4(7) . . ?
C17 C12 C11 124.3(6) . . ?
C13 C12 C11 116.3(7) . . ?
C14 C13 C12 120.3(8) . . ?
C13 C14 C15 120.8(7) . . ?
C16 C15 C14 120.5(8) . . ?
O3 C16 C15 125.5(7) . . ?
O3 C16 C17 113.7(6) . . ?
C15 C16 C17 120.8(7) . . ?
O4 C17 C12 126.2(6) . . ?
O4 C17 C16 115.5(6) . . ?
C12 C17 C16 118.2(6) . . ?
N3 C19 C20 121.9(6) . . ?
C21 C20 C19 119.1(6) . . ?
C22 C21 C20 119.9(6) . . ?
C21 C22 C23 120.0(6) . . ?
N3 C23 C22 119.9(6) . . ?
N3 C23 C24 114.4(5) . . ?
C22 C23 C24 125.7(6) . . ?
N4 C24 C25 120.8(6) . . ?
N4 C24 C23 115.1(5) . . ?
C25 C24 C23 124.1(6) . . ?
C26 C25 C24 119.1(6) . . ?
C27 C26 C25 119.6(6) . . ?
C26 C27 C28 118.5(6) . . ?
N4 C28 C27 122.6(6) . . ?
O5 C30 C31 123.9(5) . . ?
O5 C30 C29 115.8(6) . . ?
C31 C30 C29 120.3(6) . . ?
C30 C31 C32 127.3(6) . . ?
O6 C32 C31 124.0(5) . . ?
O6 C32 C33 115.5(6) . . ?
C31 C32 C33 120.5(6) . . ?
C8 N1 C9 121.9(6) . . ?
C8 N1 Pd1 124.8(5) . . ?
C9 N1 Pd1 113.3(5) . . ?
C11 N2 C10 121.5(6) . . ?
C11 N2 Pd1 126.0(5) . . ?
C10 N2 Pd1 112.3(5) . . ?
C19 N3 C23 119.2(5) . . ?
C19 N3 Cu2 126.3(4) . . ?
C23 N3 Cu2 114.4(4) . . ?
C28 N4 C24 119.3(5) . . ?
C28 N4 Cu2 126.3(4) . . ?
C24 N4 Cu2 114.4(4) . . ?
C2 O1 C1 118.2(4) . . ?
C7 O2 Pd1 123.7(4) . . ?
C16 O3 C18 118.9(6) . . ?
C17 O4 Pd1 123.4(4) . . ?
C30 O5 Cu2 125.7(4) . . ?
C32 O6 Cu2 125.3(4) . . ?
N2 Pd1 N1 84.0(3) . . ?
N2 Pd1 O4 94.3(2) . . ?
N1 Pd1 O4 178.3(2) . . ?
N2 Pd1 O2 177.7(2) . . ?
N1 Pd1 O2 93.9(2) . . ?
O4 Pd1 O2 87.76(15) . . ?
O6 Cu2 O5 93.56(17) . . ?
O6 Cu2 N4 165.45(17) . . ?
O5 Cu2 N4 91.93(19) . . ?
O6 Cu2 N3 91.36(18) . . ?
O5 Cu2 N3 169.55(18) . . ?
N4 Cu2 N3 81.2(2) . . ?
O6 Cu2 O1W 97.0(2) . . ?
O5 Cu2 O1W 93.01(19) . . ?
N4 Cu2 O1W 96.1(2) . . ?
N3 Cu2 O1W 95.54(18) . . ?
O7 Cl3 O10 103.8(6) . . ?
O7 Cl3 O8 115.1(5) . . ?
O10 Cl3 O8 107.1(6) . . ?
O7 Cl3 O9 113.3(6) . . ?
O10 Cl3 O9 107.8(7) . . ?
O8 Cl3 O9 109.1(4) . . ?
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
C1 O1 1.431(6) . ?
C2 O1 1.370(6) . ?
C2 C3 1.384(7) . ?
C2 C7 1.409(8) . ?
C3 C4 1.416(9) . ?
C4 C5 1.336(9) . ?
C5 C6 1.407(8) . ?
C6 C8 1.424(9) . ?
C6 C7 1.430(8) . ?
C7 O2 1.312(6) . ?
C8 N1 1.274(8) . ?
C9 C10 1.448(9) . ?
C9 N1 1.474(8) . ?
C10 N2 1.478(8) . ?
C11 N2 1.288(8) . ?
C11 C12 1.427(9) . ?
C12 C17 1.407(8) . ?
C12 C13 1.423(9) . ?
C13 C14 1.368(10) . ?
C14 C15 1.379(10) . ?
C15 C16 1.378(8) . ?
C16 O3 1.365(8) . ?
C16 C17 1.421(8) . ?
C17 O4 1.317(6) . ?
C18 O3 1.413(7) . ?
C19 N3 1.336(7) . ?
C19 C20 1.369(7) . ?
C20 C21 1.357(8) . ?
C21 C22 1.351(8) . ?
C22 C23 1.384(7) . ?
C23 N3 1.356(7) . ?
C23 C24 1.468(8) . ?
C24 N4 1.348(7) . ?
C24 C25 1.383(7) . ?
C25 C26 1.382(8) . ?
C26 C27 1.363(9) . ?
C27 C28 1.382(7) . ?
C28 N4 1.324(6) . ?
C29 C30 1.499(7) . ?
C30 O5 1.268(6) . ?
C30 C31 1.368(8) . ?
C31 C32 1.388(8) . ?
C32 O6 1.272(6) . ?
C32 C33 1.479(8) . ?
N1 Pd1 1.951(5) . ?
N2 Pd1 1.936(6) . ?
N3 Cu2 1.998(4) . ?
N4 Cu2 1.998(4) . ?
O2 Pd1 1.994(4) . ?
O1W Cu2 2.279(5) . ?
O4 Pd1 1.982(4) . ?
O5 Cu2 1.930(4) . ?
O6 Cu2 1.926(4) . ?
O7 Cl3 1.313(7) . ?
O8 Cl3 1.352(6) . ?
O9 Cl3 1.355(7) . ?
O10 Cl3 1.321(9) . ?
