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#$Date: 2016-03-24 02:46:15 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179595 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/59/4505936.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_4505936
loop_
_publ_author_name
'Carrión, M. Carmen'
'Durá, Gema'
'Jalón, Félix A.'
'Manzano, Blanca R.'
'Rodríguez, Ana M.'
_publ_section_title
;
 Polynuclear Complexes Containing Ditopic Bispyrazolylmethane Ligands.
 Influence of Metal Geometry and Supramolecular Interactions
;
_journal_issue                   4
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1952
_journal_paper_doi               10.1021/cg201677s
_journal_volume                  12
_journal_year                    2012
_chemical_formula_moiety         'C32 H38 Cl6 N10 Pd3, 2(C3 H6 O)'
_chemical_formula_sum            'C38 H50 Cl6 N10 O2 Pd3'
_chemical_formula_weight         1210.78
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.508(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.1235(9)
_cell_length_b                   15.5263(16)
_cell_length_c                   17.465(2)
_cell_measurement_reflns_used    5885
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      26.269
_cell_measurement_theta_min      2.365
_cell_volume                     2440.0(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      230(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega and phi 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  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16892
_diffrn_reflns_theta_full        26.44
_diffrn_reflns_theta_max         26.44
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    1.465
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9353
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4993
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0507P)²+0.3704P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0986
_reflns_number_gt                4322
_reflns_number_total             4993
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg201677s_si_002.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4505936
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Pd1 Pd 0.43321(2) 0.465041(15) 0.843761(15) 0.02611(10) Uani 1 1 d .
Pd2 Pd 0.0000 0.5000 0.5000 0.03223(12) Uani 1 2 d S
Cl1 Cl 0.21409(10) 0.48997(6) 0.88567(6) 0.0436(2) Uani 1 1 d .
Cl2 Cl 0.44463(10) 0.60637(6) 0.80914(7) 0.0474(3) Uani 1 1 d .
Cl3 Cl 0.17495(11) 0.52430(7) 0.42178(6) 0.0520(3) Uani 1 1 d .
N1 N 0.6292(3) 0.43745(18) 0.80887(16) 0.0272(6) Uani 1 1 d .
N2 N 0.6348(3) 0.36725(17) 0.76147(15) 0.0262(6) Uani 1 1 d .
N3 N 0.4202(3) 0.33578(17) 0.86244(16) 0.0286(6) Uani 1 1 d .
N4 N 0.4507(3) 0.28142(17) 0.80500(15) 0.0258(6) Uani 1 1 d .
N5 N 0.1601(3) 0.44503(18) 0.58046(16) 0.0331(7) Uani 1 1 d .
O1 O 0.5068(4) 0.2420(3) 0.57260(19) 0.0772(11) Uani 1 1 d .
C1 C 0.7765(3) 0.3505(2) 0.75281(19) 0.0312(7) Uani 1 1 d .
C2 C 0.8624(4) 0.4111(2) 0.7942(2) 0.0362(8) Uani 1 1 d .
H2 H 0.9650 0.4164 0.7986 0.043 Uiso 1 1 calc R
C3 C 0.7688(4) 0.4640(2) 0.8291(2) 0.0312(8) Uani 1 1 d .
C4 C 0.8148(4) 0.2766(3) 0.7053(2) 0.0474(10) Uani 1 1 d .
H4A H 0.7852 0.2237 0.7269 0.071 Uiso 1 1 calc R
H4B H 0.9200 0.2759 0.7056 0.071 Uiso 1 1 calc R
H4C H 0.7636 0.2826 0.6530 0.071 Uiso 1 1 calc R
C5 C 0.8091(4) 0.5371(2) 0.8842(2) 0.0407(9) Uani 1 1 d .
H5A H 0.7379 0.5827 0.8722 0.061 Uiso 1 1 calc R
H5B H 0.9063 0.5580 0.8795 0.061 Uiso 1 1 calc R
H5C H 0.8089 0.5177 0.9364 0.061 Uiso 1 1 calc R
C6 C 0.4407(4) 0.1980(2) 0.8262(2) 0.0333(8) Uani 1 1 d .
C7 C 0.4026(4) 0.2002(2) 0.8989(2) 0.0437(9) Uani 1 1 d .
H7 H 0.3871 0.1525 0.9288 0.052 Uiso 1 1 calc R
C8 C 0.3911(4) 0.2856(2) 0.9202(2) 0.0370(8) Uani 1 1 d .
C9 C 0.4687(5) 0.1254(2) 0.7752(2) 0.0483(10) Uani 1 1 d .
H9A H 0.3976 0.1272 0.7282 0.072 Uiso 1 1 calc R
H9B H 0.4595 0.0719 0.8015 0.072 Uiso 1 1 calc R
H9C H 0.5672 0.1303 0.7631 0.072 Uiso 1 1 calc R
C10 C 0.3606(6) 0.3213(3) 0.9955(2) 0.0603(12) Uani 1 1 d .
H10A H 0.3975 0.3792 1.0017 0.090 Uiso 1 1 calc R
H10B H 0.4093 0.2864 1.0375 0.090 Uiso 1 1 calc R
H10C H 0.2554 0.3212 0.9956 0.090 Uiso 1 1 calc R
C11 C 0.5012(3) 0.3170(2) 0.73756(18) 0.0261(7) Uani 1 1 d .
H11 H 0.5287 0.2684 0.7071 0.031 Uiso 1 1 calc R
C12 C 0.3805(3) 0.3668(2) 0.68551(18) 0.0260(7) Uani 1 1 d .
C13 C 0.2398(4) 0.3314(2) 0.6680(2) 0.0363(8) Uani 1 1 d .
H13 H 0.2177 0.2805 0.6917 0.044 Uiso 1 1 calc R
C14 C 0.1330(4) 0.3716(2) 0.6155(2) 0.0398(9) Uani 1 1 d .
H14 H 0.0390 0.3470 0.6039 0.048 Uiso 1 1 calc R
C15 C 0.2965(4) 0.4794(2) 0.5970(2) 0.0368(8) Uani 1 1 d .
H15 H 0.3162 0.5302 0.5724 0.044 Uiso 1 1 calc R
C16 C 0.4079(4) 0.4424(2) 0.6489(2) 0.0345(8) Uani 1 1 d .
H16 H 0.5012 0.4681 0.6594 0.041 Uiso 1 1 calc R
C21 C 0.2961(7) 0.1977(4) 0.4878(4) 0.111(2) Uani 1 1 d .
H21A H 0.2750 0.1670 0.5325 0.167 Uiso 1 1 calc R
H21B H 0.3096 0.1573 0.4480 0.167 Uiso 1 1 calc R
H21C H 0.2146 0.2353 0.4690 0.167 Uiso 1 1 calc R
C22 C 0.4323(5) 0.2487(3) 0.5094(3) 0.0594(12) Uani 1 1 d .
C23 C 0.4673(8) 0.3097(5) 0.4515(5) 0.135(3) Uani 1 1 d .
H23A H 0.5425 0.3490 0.4754 0.203 Uiso 1 1 calc R
H23B H 0.3795 0.3413 0.4304 0.203 Uiso 1 1 calc R
H23C H 0.5031 0.2789 0.4106 0.203 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'
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
N1 Pd1 N3 85.27(11) . .
N1 Pd1 Cl1 177.35(8) . .
N3 Pd1 Cl1 92.21(8) . .
N1 Pd1 Cl2 92.43(8) . .
N3 Pd1 Cl2 173.92(8) . .
Cl1 Pd1 Cl2 90.15(4) . .
N5 Pd2 N5 180.000(1) . 3_566
N5 Pd2 Cl3 89.41(9) . .
N5 Pd2 Cl3 90.59(9) 3_566 .
N5 Pd2 Cl3 90.59(9) . 3_566
N5 Pd2 Cl3 89.41(9) 3_566 3_566
Cl3 Pd2 Cl3 180.0 . 3_566
C3 N1 N2 106.1(2) . .
C3 N1 Pd1 135.1(2) . .
N2 N1 Pd1 118.11(19) . .
C1 N2 N1 110.6(3) . .
C1 N2 C11 129.7(3) . .
N1 N2 C11 119.1(2) . .
C8 N3 N4 106.4(3) . .
C8 N3 Pd1 136.0(2) . .
N4 N3 Pd1 117.6(2) . .
C6 N4 N3 110.9(3) . .
C6 N4 C11 129.4(3) . .
N3 N4 C11 119.4(3) . .
C14 N5 C15 118.4(3) . .
C14 N5 Pd2 120.5(2) . .
C15 N5 Pd2 121.0(2) . .
N2 C1 C2 106.6(3) . .
N2 C1 C4 121.8(3) . .
C2 C1 C4 131.6(3) . .
C1 C2 C3 107.5(3) . .
N1 C3 C2 109.2(3) . .
N1 C3 C5 122.0(3) . .
C2 C3 C5 128.7(3) . .
N4 C6 C7 105.6(3) . .
N4 C6 C9 122.4(3) . .
C7 C6 C9 132.0(3) . .
C6 C7 C8 108.3(3) . .
N3 C8 C7 108.8(3) . .
N3 C8 C10 122.5(3) . .
C7 C8 C10 128.6(3) . .
N4 C11 N2 109.7(2) . .
N4 C11 C12 112.7(2) . .
N2 C11 C12 113.0(3) . .
C16 C12 C13 118.0(3) . .
C16 C12 C11 122.8(3) . .
C13 C12 C11 119.0(3) . .
C14 C13 C12 119.8(3) . .
N5 C14 C13 122.0(3) . .
N5 C15 C16 122.4(3) . .
C15 C16 C12 119.4(3) . .
O1 C22 C23 122.5(5) . .
O1 C22 C21 121.0(5) . .
C23 C22 C21 116.4(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 N1 2.028(3) .
Pd1 N3 2.040(3) .
Pd1 Cl1 2.2727(9) .
Pd1 Cl2 2.2830(10) .
Pd2 N5 2.039(3) .
Pd2 N5 2.039(3) 3_566
Pd2 Cl3 2.2971(11) .
Pd2 Cl3 2.2971(11) 3_566
N1 C3 1.331(4) .
N1 N2 1.375(4) .
N2 C1 1.351(4) .
N2 C11 1.450(4) .
N3 C8 1.335(4) .
N3 N4 1.374(4) .
N4 C6 1.355(4) .
N4 C11 1.444(4) .
N5 C14 1.336(4) .
N5 C15 1.341(4) .
O1 C22 1.201(5) .
C1 C2 1.355(5) .
C1 C4 1.490(5) .
C2 C3 1.396(5) .
C3 C5 1.494(5) .
C6 C7 1.370(5) .
C6 C9 1.484(5) .
C7 C8 1.386(5) .
C8 C10 1.495(5) .
C11 C12 1.519(4) .
C12 C16 1.379(5) .
C12 C13 1.383(4) .
C13 C14 1.373(5) .
C15 C16 1.372(5) .
C21 C22 1.470(7) .
C22 C23 1.459(8) .
