#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:26:56 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179970 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/64/7026423.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_7026423
loop_
_publ_author_name
'Zhang, Qian'
'He, Lisi'
'Liu, Jun-Min'
'Wang, Wei'
'Zhang, Jianyong'
'Su, Cheng-Yong'
_publ_section_title
;
 Pd2L2 metallacycles as molecular containers for small molecules.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11171
_journal_page_last               11179
_journal_paper_doi               10.1039/c0dt00406e
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C66 H76 Cl10 N10 Pd2'
_chemical_formula_weight         1576.67
_chemical_name_systematic
;
?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 122.780(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.6272(10)
_cell_length_b                   16.7990(10)
_cell_length_c                   14.8756(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      5
_cell_volume                     3703.5(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       'ω scan'
_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  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4433
_diffrn_reflns_theta_full        26.11
_diffrn_reflns_theta_max         26.11
_diffrn_reflns_theta_min         2.32
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 800
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.891
_exptl_absorpt_correction_T_max  0.8079
_exptl_absorpt_correction_T_min  0.7059
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   PSI-scan
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.152
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    geom
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         3770
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0730
_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)+(0.0910P)²+38.4236P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1801
_refine_ls_wR_factor_ref         0.2148
_reflns_number_gt                2795
_reflns_number_total             3770
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00406e.txt
_cod_data_source_block           4
_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 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'PSI-scan'
changed to 'psi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        3703.5(4)
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               7026423
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd -0.56045(5) -0.5000 1.25023(6) 0.0463(3) Uani 1 2 d S . .
N1 N -0.5617(4) -0.6195(3) 1.2501(4) 0.0475(13) Uani 1 1 d . . .
N2 N -0.5555(4) -0.7427(3) 1.2070(4) 0.0487(13) Uani 1 1 d . . .
C1 C -0.5446(5) -0.6660(3) 1.1927(5) 0.0486(16) Uani 1 1 d . . .
H1A H -0.5271 -0.6479 1.1475 0.058 Uiso 1 1 calc R . .
C2 C -0.5835(4) -0.6672(3) 1.3084(5) 0.0403(13) Uani 1 1 d . . .
C3 C -0.6058(4) -0.6508(4) 1.3826(5) 0.0449(14) Uani 1 1 d . . .
H3A H -0.6086 -0.5986 1.4013 0.054 Uiso 1 1 calc R . .
C4 C -0.6237(4) -0.7128(4) 1.4276(5) 0.0484(15) Uani 1 1 d . . .
C5 C -0.6209(5) -0.7923(4) 1.3988(5) 0.0525(16) Uani 1 1 d . . .
C6 C -0.5980(5) -0.8099(4) 1.3263(5) 0.0504(16) Uani 1 1 d . . .
H6A H -0.5948 -0.8622 1.3080 0.061 Uiso 1 1 calc R . .
C7 C -0.5796(4) -0.7460(4) 1.2817(5) 0.0409(13) Uani 1 1 d . . .
C8 C -0.6439(7) -0.8600(6) 1.4463(7) 0.082(3) Uani 1 1 d . . .
H8A H -0.6594 -0.8392 1.4945 0.122 Uiso 1 1 calc R . .
H8B H -0.5928 -0.8947 1.4846 0.122 Uiso 1 1 calc R . .
H8C H -0.6942 -0.8892 1.3902 0.122 Uiso 1 1 calc R . .
C9 C -0.6485(5) -0.6938(6) 1.5086(6) 0.068(2) Uani 1 1 d . . .
H9A H -0.6455 -0.6373 1.5199 0.103 Uiso 1 1 calc R . .
H9B H -0.6070 -0.7200 1.5750 0.103 Uiso 1 1 calc R . .
H9C H -0.7087 -0.7122 1.4820 0.103 Uiso 1 1 calc R . .
C10 C -0.5426(7) -0.8143(4) 1.1599(7) 0.071(2) Uani 1 1 d . . .
H10A H -0.5971 -0.8462 1.1274 0.086 Uiso 1 1 calc R . .
H10B H -0.4940 -0.8456 1.2166 0.086 Uiso 1 1 calc R . .
C11 C -0.5207(4) -0.7967(3) 1.0760(5) 0.0421(14) Uani 1 1 d . . .
C12 C -0.4315(4) -0.7934(4) 1.1080(5) 0.0454(14) Uani 1 1 d . . .
C13 C -0.5896(4) -0.7937(4) 0.9706(5) 0.0471(15) Uani 1 1 d . . .
C14 C -0.3560(7) -0.7899(7) 1.2253(6) 0.099(3) Uani 1 1 d . . .
H14A H -0.3812 -0.7896 1.2685 0.149 Uiso 1 1 calc R . .
H14B H -0.3212 -0.7424 1.2386 0.149 Uiso 1 1 calc R . .
H14C H -0.3177 -0.8356 1.2430 0.149 Uiso 1 1 calc R . .
C15 C -0.6861(6) -0.7926(7) 0.9370(9) 0.092(3) Uani 1 1 d . . .
H15A H -0.6896 -0.7941 0.9991 0.138 Uiso 1 1 calc R . .
H15B H -0.7165 -0.8380 0.8928 0.138 Uiso 1 1 calc R . .
H15C H -0.7142 -0.7448 0.8973 0.138 Uiso 1 1 calc R . .
Cl1 Cl -0.4102(2) -0.5000 1.3107(3) 0.0794(9) Uani 1 2 d S . .
Cl2 Cl -0.7106(2) -0.5000 1.1877(4) 0.0909(11) Uani 1 2 d S . .
N3 N -0.0468(16) -0.5000 1.692(2) 0.126(8) Uani 0.60 2 d SPDU A 1
C17 C -0.1197(15) -0.5000 1.654(2) 0.089(6) Uani 0.60 2 d SPDU A 1
C18 C -0.2166(15) -0.5000 1.607(2) 0.098(7) Uani 0.60 2 d SPDU A 1
H18A H -0.2353 -0.5518 1.6149 0.147 Uiso 0.50 1 calc PR A 1
H18B H -0.2473 -0.4869 1.5325 0.147 Uiso 0.50 1 calc PR A 1
H18C H -0.2312 -0.4613 1.6429 0.147 Uiso 0.50 1 calc PR A 1
N3' N -0.016(4) -0.5000 1.822(3) 0.182(15) Uani 0.40 2 d SPDU B 2
C17' C 0.006(4) -0.5000 1.907(3) 0.165(13) Uani 0.40 2 d SPDU B 2
C18' C 0.0000 -0.5000 2.0000 0.137(11) Uani 0.80 4 d SPDU . 2
C16 C -0.292(2) -0.5000 1.054(5) 0.176(12) Uani 0.50 2 d SPDU . 1
H16A H -0.3122 -0.5000 0.9785 0.211 Uiso 0.50 2 calc SPR . 1
Cl3 Cl -0.3234(9) -0.4124(7) 1.0974(12) 0.194(5) Uani 0.50 1 d PDU . 1
Cl4 Cl -0.1703(10) -0.5000 1.1480(13) 0.161(5) Uani 0.50 2 d SPDU . 1
C16' C -0.346(3) -0.5000 1.135(4) 0.146(10) Uani 0.50 2 d SPU . 2
H16B H -0.3407 -0.5000 1.2043 0.175 Uiso 0.50 2 calc SPR . 2
Cl3' Cl -0.3981(11) -0.4164(8) 1.0704(12) 0.203(5) Uani 0.50 1 d PU . 2
Cl4' Cl -0.2388(17) -0.5000 1.157(2) 0.236(7) Uani 0.50 2 d SPU . 2
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Pd1 N1 178.8(3) 6_545 .
N1 Pd1 Cl2 89.43(16) 6_545 .
N1 Pd1 Cl2 89.43(16) . .
N1 Pd1 Cl1 90.58(16) 6_545 .
N1 Pd1 Cl1 90.58(16) . .
Cl2 Pd1 Cl1 179.26(15) . .
C1 N1 C2 107.7(5) . .
C1 N1 Pd1 126.3(4) . .
C2 N1 Pd1 125.9(4) . .
C1 N2 C7 107.4(5) . .
C1 N2 C10 129.8(5) . .
C7 N2 C10 122.8(5) . .
N1 C1 N2 111.6(5) . .
N1 C1 H1A 124.2 . .
N2 C1 H1A 124.2 . .
N1 C2 C3 133.0(6) . .
N1 C2 C7 107.4(5) . .
C3 C2 C7 119.6(5) . .
C4 C3 C2 118.7(6) . .
C4 C3 H3A 120.7 . .
C2 C3 H3A 120.7 . .
C3 C4 C5 121.2(6) . .
C3 C4 C9 118.0(7) . .
C5 C4 C9 120.7(6) . .
C6 C5 C4 121.1(6) . .
C6 C5 C8 118.3(7) . .
C4 C5 C8 120.6(6) . .
C5 C6 C7 116.9(6) . .
C5 C6 H6A 121.6 . .
C7 C6 H6A 121.6 . .
N2 C7 C6 131.7(6) . .
N2 C7 C2 105.8(5) . .
C6 C7 C2 122.5(5) . .
C5 C8 H8A 109.5 . .
C5 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C5 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C4 C9 H9A 109.5 . .
C4 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C4 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
N2 C10 C11 113.9(5) . .
N2 C10 H10A 108.8 . .
C11 C10 H10A 108.8 . .
N2 C10 H10B 108.8 . .
C11 C10 H10B 108.8 . .
H10A C10 H10B 107.7 . .
C13 C11 C12 122.3(6) . .
C13 C11 C10 119.0(7) . .
C12 C11 C10 118.3(6) . .
C11 C12 C13 118.6(6) . 2_457
C11 C12 C14 121.8(7) . .
C13 C12 C14 119.6(7) 2_457 .
C11 C13 C12 118.9(6) . 2_457
C11 C13 C15 121.9(7) . .
C12 C13 C15 119.2(7) 2_457 .
C12 C14 H14A 109.5 . .
C12 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C12 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C13 C15 H15A 109.5 . .
C13 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C13 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
N3 C17 C18 178(3) . .
N3' C17' C18' 160(7) . .
C17' C18' C17' 180.00(5) . 5_549
Cl3 C16 Cl3 109(3) . 6_545
Cl3 C16 Cl4 101(2) . .
Cl3 C16 Cl4 101(2) 6_545 .
Cl3 C16 H16A 114.9 . .
Cl3 C16 H16A 114.9 6_545 .
Cl4 C16 H16A 114.9 . .
Cl3' C16' Cl3' 115(3) 6_545 .
Cl3' C16' Cl4' 108.0(18) 6_545 .
Cl3' C16' Cl4' 108.0(18) . .
Cl3' C16' H16B 108.6 6_545 .
Cl3' C16' H16B 108.6 . .
Cl4' C16' H16B 108.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 N1 2.008(5) 6_545
Pd1 N1 2.008(5) .
Pd1 Cl2 2.282(3) .
Pd1 Cl1 2.290(3) .
N1 C1 1.306(7) .
N1 C2 1.378(7) .
N2 C1 1.336(8) .
N2 C7 1.389(7) .
N2 C10 1.471(8) .
C1 H1A 0.9300 .
C2 C3 1.385(8) .
C2 C7 1.395(8) .
C3 C4 1.365(9) .
C3 H3A 0.9300 .
C4 C5 1.410(10) .
C4 C9 1.522(9) .
C5 C6 1.373(9) .
C5 C8 1.506(10) .
C6 C7 1.389(8) .
C6 H6A 0.9300 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C10 C11 1.522(8) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C11 C13 1.368(9) .
C11 C12 1.374(9) .
C12 C13 1.406(9) 2_457
C12 C14 1.519(10) .
C13 C12 1.406(9) 2_457
C13 C15 1.491(10) .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
N3 C17 1.088(17) .
C17 C18 1.455(17) .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
N3' C17' 1.11(2) .
C17' C18' 1.44(3) .
C18' C17' 1.44(3) 5_549
C16 Cl3 1.81(3) .
C16 Cl3 1.81(3) 6_545
C16 Cl4 1.82(3) .
C16 H16A 0.9800 .
C16' Cl3' 1.67(3) 6_545
C16' Cl3' 1.67(3) .
C16' Cl4' 1.74(5) .
C16' H16B 0.9800 .
