#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/10/1101085.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_1101085
loop_
_publ_author_name
'Mohammad Abul Haj'
'Miguel Quirós'
'Juan M. Salas'
_publ_section_title
;
 Solution and solid state coexistence of head--head and head--tail
 isomers in dimeric Pd(II) and Pt(II) complexes of the type
 [M2(a--a)2(µ-L-N3N4)2]2+ with a bridging triazolopyrimidine
 ligand and chelating bidentate diamines
;
_journal_issue                   24
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              4740
_journal_page_last               4745
_journal_paper_doi               10.1039/b207263g
_journal_year                    2002
_chemical_formula_sum            'C26 H29 Cl3 N16 O19 Pd2'
_chemical_formula_weight         1188.80
_space_group_IT_number           59
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2a'
_symmetry_space_group_name_H-M   'P m m n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_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            2
_cell_length_a                   11.1799(14)
_cell_length_b                   18.9400(18)
_cell_length_c                   9.6374(8)
_cell_measurement_reflns_used    46
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.5
_cell_measurement_theta_min      12.5
_cell_volume                     2040.7(4)
_computing_cell_refinement       'STADI4 (STOE, 1996)'
_computing_data_collection       'STADI4 (STOE, 1996)'
_computing_data_reduction        'X-RED  (STOE, 1996)'
_computing_molecular_graphics    'SHELXTL PLUS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'STOE STADI4 4-circle-diffractometer'
_diffrn_measurement_method
; Scan width (omega) = 1.05 - 1.25, scan ratio 2theta:omega = 1.00
I(Net) and sigma(I) calculated according to Blessing (1987)
;
_diffrn_radiation_collimation    '0.8 mm'
_diffrn_radiation_detector       'NaI(Tl) scintillation counter'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_polarisn_norm  90
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3193
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        3.7
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.176
_exptl_absorpt_correction_T_max  0.6505
_exptl_absorpt_correction_T_min  0.5388
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.858
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         3193
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.1404
_refine_ls_R_factor_gt           0.0821
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0600P)²+10.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1705
_refine_ls_wR_factor_ref         0.2107
_reflns_number_gt                1900
_reflns_number_total             3193
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207263g.txt
_cod_data_source_block           compound6
_cod_original_sg_symbol_H-M      'P m m n'
_cod_database_code               1101085
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z'
'x+1/2, -y, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z'
'-x-1/2, y, 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
Pd Pd 0.39204(8) 0.2500 0.53000(8) 0.0569(3) Uani 1 2 d S . .
N1 N 0.3916(10) 0.4104(9) 0.8390(17) 0.075(4) Uiso 0.50 1 d PD A -1
C2 C 0.4428(11) 0.3648(11) 0.752(2) 0.069(7) Uiso 0.50 1 d PD A -1
H2 H 0.5283 0.3619 0.7445 0.082 Uiso 0.50 1 d PR A -1
N3 N 0.3718(10) 0.3220(7) 0.6749(14) 0.051(3) Uiso 0.50 1 d PD A -1
C3A C 0.2635(9) 0.3451(5) 0.7167(9) 0.046(2) Uiso 0.50 1 d PD A -1
N4 N 0.1558(10) 0.3287(7) 0.6722(14) 0.048(3) Uiso 0.50 1 d PD . -1
C5 C 0.0559(15) 0.3528(14) 0.738(3) 0.082(8) Uiso 0.50 1 d PD A -1
H5 H -0.0215 0.3345 0.7138 0.098 Uiso 0.50 1 d PR A -1
C6 C 0.0682(14) 0.4025(10) 0.840(2) 0.073(5) Uiso 0.50 1 d PD A -1
H6 H -0.0031 0.4187 0.8855 0.088 Uiso 0.50 1 d PR A -1
C7 C 0.1767(10) 0.4309(8) 0.8837(16) 0.080(5) Uiso 0.50 1 d PD A -1
O7 O 0.2073(10) 0.4767(6) 0.9664(12) 0.096(4) Uiso 0.50 1 d PD A -1
N8 N 0.2726(9) 0.3958(5) 0.8183(9) 0.058(3) Uiso 0.50 1 d PD A -1
N1P N 0.4419(6) 0.3179(4) 0.3814(6) 0.0691(17) Uani 1 1 d . A .
C2P C 0.4282(10) 0.3887(6) 0.3823(9) 0.090(3) Uani 1 1 d . . .
H2P H 0.3881 0.4104 0.4553 0.107 Uiso 1 1 d R A .
C3P C 0.4739(12) 0.4284(6) 0.2738(11) 0.118(4) Uani 1 1 d . A .
H3P H 0.4626 0.4770 0.2700 0.142 Uiso 1 1 d R . .
C4P C 0.5375(14) 0.3919(9) 0.1737(12) 0.144(6) Uani 1 1 d . . .
H4P H 0.5733 0.4180 0.1034 0.173 Uiso 1 1 d R A .
N5P N 0.5492(9) 0.3229(6) 0.1714(8) 0.109(3) Uani 1 1 d . A .
C6P C 0.4992(8) 0.2887(5) 0.2758(7) 0.081(3) Uani 1 1 d . . .
Cl1 Cl 0.2500 0.2500 0.0583(4) 0.0679(10) Uani 1 4 d S . .
O1Q O 0.3519(10) 0.2500 -0.0262(9) 0.096(3) Uani 1 2 d S . .
O2Q O 0.2500 0.1891(6) 0.1438(11) 0.126(4) Uani 1 2 d S . .
Cl2 Cl 0.2500 0.56295(19) 0.5095(4) 0.0891(10) Uani 1 2 d S . .
O3Q O 0.3488(9) 0.5628(5) 0.4235(9) 0.147(3) Uani 1 1 d . . .
O4Q O 0.2500 0.5034(6) 0.5949(11) 0.123(4) Uani 1 2 d S . .
O5Q O 0.2500 0.6234(7) 0.5939(15) 0.170(6) Uani 1 2 d S . .
O1W O 0.2500 0.5837(5) 0.1318(10) 0.118(4) Uani 1 2 d S . .
O2W O 0.1676(12) 0.7096(6) 0.0628(10) 0.086(3) Uani 0.50 1 d P . -1
O3W O 0.684(3) 0.2500 0.578(3) 0.170(11) Uiso 0.50 2 d SP . .
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
_geom_angle_publ_flag
N3 Pd N3 87.9(9) . 7_565 ?
N3 Pd N1P 170.2(4) . 7_565 ?
N3 Pd N1P 95.4(5) 7_565 7_565 ?
N3 Pd N1P 95.4(5) . . ?
N3 Pd N1P 170.2(4) 7_565 . ?
N1P Pd N1P 79.9(4) 7_565 . ?
N3 Pd N4 8.7(6) . 8_655 ?
N3 Pd N4 90.0(3) 7_565 8_655 ?
N1P Pd N4 174.5(5) 7_565 8_655 ?
N1P Pd N4 94.7(5) . 8_655 ?
N3 Pd N4 90.0(3) . 2 ?
N3 Pd N4 8.7(6) 7_565 2 ?
N1P Pd N4 94.7(5) 7_565 2 ?
N1P Pd N4 174.5(5) . 2 ?
N4 Pd N4 90.8(9) 8_655 2 ?
N3 Pd Pd 83.4(3) . 2 ?
N3 Pd Pd 83.4(3) 7_565 2 ?
N1P Pd Pd 106.2(2) 7_565 2 ?
N1P Pd Pd 106.2(2) . 2 ?
N4 Pd Pd 75.2(3) 8_655 2 ?
N4 Pd Pd 75.2(3) 2 2 ?
C2 N1 N8 101.2(11) . . ?
N1 C2 N3 118.7(10) . . ?
C3A N3 C2 99.6(7) . . ?
C3A N3 Pd 122.8(8) . . ?
C2 N3 Pd 137.5(8) . . ?
N4 C3A N3 130.4(8) . . ?
N4 C3A N8 117.6(10) . . ?
N3 C3A N8 111.9(8) . . ?
C3A N4 C5 121.4(12) . . ?
C3A N4 Pd 127.9(9) . 2 ?
C5 N4 Pd 109.4(9) . 2 ?
N4 C5 C6 118.8(17) . . ?
C5 C6 C7 124.8(18) . . ?
O7 C7 C6 135.5(12) . . ?
O7 C7 N8 114.3(11) . . ?
C6 C7 N8 110.2(12) . . ?
N1 N8 C3A 108.4(11) . . ?
N1 N8 C7 125.2(11) . . ?
C3A N8 C7 126.3(10) . . ?
C6P N1P C2P 118.4(8) . . ?
C6P N1P Pd 114.6(6) . . ?
C2P N1P Pd 127.0(6) . . ?
N1P C2P C3P 119.5(10) . . ?
C4P C3P C2P 116.4(12) . . ?
N5P C4P C3P 124.1(11) . . ?
C4P N5P C6P 115.6(10) . . ?
N5P C6P N1P 125.9(10) . . ?
N5P C6P C6P 119.3(6) . 7_565 ?
N1P C6P C6P 114.7(5) . 7_565 ?
O1Q Cl1 O1Q 108.9(9) 2 . ?
O1Q Cl1 O2Q 109.8(3) 2 2 ?
O1Q Cl1 O2Q 109.8(3) . 2 ?
O1Q Cl1 O2Q 109.8(3) 2 . ?
O1Q Cl1 O2Q 109.8(3) . . ?
O2Q Cl1 O2Q 108.9(11) 2 . ?
O3Q Cl2 O3Q 106.2(9) . 8_655 ?
O3Q Cl2 O4Q 110.6(5) . . ?
O3Q Cl2 O4Q 110.6(5) 8_655 . ?
O3Q Cl2 O5Q 110.5(6) . . ?
O3Q Cl2 O5Q 110.5(6) 8_655 . ?
O4Q Cl2 O5Q 108.5(8) . . ?
O7 O1W O2W 118.8(5) 1_554 . ?
O2W O2W O1W 108.0(7) 2_565 . ?
O2W O2W N5P 121.7(4) 2_565 4_465 ?
O1W O2W N5P 100.1(5) . 4_465 ?
O3W O3W O5Q 75.8(5) 2_655 5_666 ?
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
Pd N3 1.964(10) . ?
Pd N3 1.964(10) 7_565 ?
Pd N1P 2.004(6) 7_565 ?
Pd N1P 2.004(6) . ?
Pd N4 2.095(11) 8_655 ?
Pd N4 2.095(11) 2 ?
Pd Pd 3.1760(17) 2 ?
N1 C2 1.333(5) . ?
N1 N8 1.373(5) . ?
C2 N3 1.357(5) . ?
N3 C3A 1.349(5) . ?
C3A N4 1.315(5) . ?
C3A N8 1.375(5) . ?
N4 C5 1.362(5) . ?
N4 Pd 2.095(11) 2 ?
C5 C6 1.368(5) . ?
C6 C7 1.393(5) . ?
C7 O7 1.227(5) . ?
C7 N8 1.410(5) . ?
N1P C6P 1.323(10) . ?
N1P C2P 1.350(11) . ?
C2P C3P 1.385(12) . ?
C3P C4P 1.384(18) . ?
C4P N5P 1.314(16) . ?
N5P C6P 1.321(10) . ?
C6P C6P 1.466(19) 7_565 ?
Cl1 O1Q 1.400(9) 2 ?
Cl1 O1Q 1.400(9) . ?
Cl1 O2Q 1.417(10) 2 ?
Cl1 O2Q 1.417(10) . ?
Cl2 O3Q 1.381(9) . ?
Cl2 O3Q 1.381(9) 8_655 ?
Cl2 O4Q 1.397(10) . ?
Cl2 O5Q 1.404(12) . ?
O1W O7 2.622(15) 1_554 ?
O1W O2W 2.641(15) . ?
O2W O2W 2.39(3) 2_565 ?
O2W N5P 2.688(13) 4_465 ?
O3W O3W 1.47(6) 2_655 ?
O3W O5Q 3.01(2) 5_666 ?
