#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:33:56 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179335 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/32/4323240.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_4323240
loop_
_publ_author_name
'Felipe Gómez-de la Torre'
'Antonio de la Hoz'
'Félix A. Jalón'
'Blanca R. Manzano'
'Antonio Otero'
'Ana M. Rodríguez'
'M. Carmen Rodríguez-Pérez'
'Áurea Echevarría'
'José Elguero'
_publ_section_title
;
 Synthesis and Characterization of Palladium(II) Complexes with New
 Polydentate Nitrogen Ligands. Dynamic Behavior Involving Pd-N Bond
 Rupture. X-ray Molecular Structure of
 [[Pd(η³-C₄H₇)]₂)(Me-BPzTO)]4-Me-C₆H₄SO₃ [Me-BPzTO =
 4,6-Bis(4-methylpyrazol-1-yl)-1,3,5-triazin-2-olate]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6606
_journal_page_last               6614
_journal_paper_doi               10.1021/ic980307n
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety
'C19 H24 N7 O Pd2 1+, C7 H7 O3 S 1-, C H2 CL2'
_chemical_formula_sum            'C27 H33 Cl2 N7 O4 Pd2 S2'
_chemical_formula_weight         835.36
_chemical_name_systematic        ?
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-A 2y'
_symmetry_space_group_name_H-M   'A 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 99.040(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.7640(10)
_cell_length_b                   16.1890(10)
_cell_length_c                   21.175(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     3305.5(9)
_computing_cell_refinement       'Nonius (control program)'
_computing_data_collection       'Nonius (control program)'
_computing_data_reduction        'XRAY80 (Stewart, 1976)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'four circle diffractometer Nonius-Mach3'
_diffrn_measurement_method       'ω/2\2q 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0669
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            4121
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  90
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.356
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.459
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_description       prism
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.756
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.061
_refine_ls_goodness_of_fit_obs   1.060
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         4121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_restrained_S_obs      1.060
_refine_ls_R_factor_all          0.1014
_refine_ls_R_factor_obs          0.0523
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[σ²(Fo²)+(0.0827P)²+0.5052P] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1757
_refine_ls_wR_factor_obs         0.1328
_reflns_number_observed          2435
_reflns_number_total             4121
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980307n.cif
_cod_data_source_block           bm4
_cod_original_sg_symbol_H-M      'A 2/m'
_cod_database_code               4323240
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x, y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z'
'-x, -y+1/2, -z+1/2'
'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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Pd1 Pd 0.14584(6) 0.19489(3) 0.06037(2) 0.0427(2) Uani 1 d . .
O5 O 0.2044(8) 0.0000 0.0130(3) 0.051(2) Uani 1 d S .
N8 N -0.0593(8) 0.0000 0.1396(3) 0.039(2) Uani 1 d S .
N9 N 0.0826(6) 0.0737(3) 0.0776(3) 0.0396(12) Uani 1 d . .
N10 N -0.0052(6) 0.2148(3) 0.1187(3) 0.0433(13) Uani 1 d . .
N11 N -0.0545(6) 0.1419(3) 0.1397(3) 0.0413(13) Uani 1 d . .
C12 C -0.0078(7) 0.0673(4) 0.1178(3) 0.0362(13) Uani 1 d . .
C13 C 0.1300(10) 0.0000 0.0537(5) 0.041(2) Uani 1 d S .
C14 C -0.1427(7) 0.1554(4) 0.1815(3) 0.0426(15) Uani 1 d . .
H14 H -0.1880 0.1152 0.2019 0.051 Uiso 1 calc . .
C15 C -0.1536(7) 0.2386(4) 0.1883(3) 0.045(2) Uani 1 d . .
C16 C -0.0650(8) 0.2723(4) 0.1484(4) 0.052(2) Uani 1 d . .
H16 H -0.0507 0.3286 0.1437 0.063 Uiso 1 calc . .
C17 C -0.2384(9) 0.2835(5) 0.2310(4) 0.060(2) Uani 1 d . .
H17A H -0.2272 0.3420 0.2264 0.090 Uiso 1 calc . .
H17B H -0.2076 0.2680 0.2747 0.090 Uiso 1 calc . .
H17C H -0.3344 0.2692 0.2192 0.090 Uiso 1 calc . .
C18 C 0.3056(8) 0.1850(5) 0.0037(4) 0.056(2) Uani 1 d . .
H18A H 0.3741 0.1420 0.0155 0.067 Uiso 1 calc . .
H18B H 0.2781 0.1908 -0.0421 0.067 Uiso 1 calc . .
C19 C 0.3235(8) 0.2594(5) 0.0398(4) 0.056(2) Uani 1 d . .
C20 C 0.2082(10) 0.3121(4) 0.0316(4) 0.064(2) Uani 1 d . .
H20A H 0.1727 0.3287 -0.0120 0.077 Uiso 1 calc . .
H20B H 0.2092 0.3566 0.0623 0.077 Uiso 1 calc . .
C21 C 0.4427(10) 0.2725(7) 0.0947(5) 0.088(3) Uani 1 d . .
H21A H 0.5113 0.2303 0.0935 0.132 Uiso 1 calc . .
H21B H 0.4081 0.2698 0.1346 0.132 Uiso 1 calc . .
H21C H 0.4838 0.3258 0.0905 0.132 Uiso 1 calc . .
S4 S 0.7836(3) 0.0000 0.33471(14) 0.0577(7) Uani 1 d S .
O6 O 0.7352(9) 0.0000 0.3950(4) 0.075(2) Uani 1 d S .
O7 O 0.7476(8) 0.0739(6) 0.3008(4) 0.138(4) Uani 1 d . .
C22 C 0.9672(11) 0.0000 0.3529(5) 0.047(2) Uani 1 d S .
C23 C 1.0307(12) 0.0000 0.4153(5) 0.053(3) Uani 1 d S .
H23 H 0.9774 0.0000 0.4480 0.064 Uiso 1 calc S .
C24 C 1.1736(16) 0.0000 0.4299(7) 0.081(4) Uani 1 d S .
H24 H 1.2166 0.0000 0.4723 0.098 Uiso 1 calc S .
C25 C 1.2538(14) 0.0000 0.3804(8) 0.077(4) Uani 1 d S .
C26 C 1.1873(14) 0.0000 0.3192(7) 0.067(3) Uani 1 d S .
H26 H 1.2391 0.0000 0.2859 0.081 Uiso 1 calc S .
C27 C 1.0470(13) 0.0000 0.3054(5) 0.057(3) Uani 1 d S .
H27 H 1.0043 0.0000 0.2630 0.068 Uiso 1 calc S .
C28 C 1.4137(18) 0.0000 0.3985(12) 0.139(9) Uani 1 d S .
H28A H 1.4383 0.0000 0.4443 0.208 Uiso 1 calc S .
H28B H 1.4509 0.0484 0.3813 0.208 Uiso 0.50 calc P .
H28C H 1.4509 -0.0484 0.3813 0.208 Uiso 0.50 calc P .
C29 C 0.4829(21) 0.0000 -0.1749(9) 0.120(6) Uiso 1 d S .
Cl2 Cl 0.4226(5) 0.0000 -0.1006(2) 0.091(2) Uani 0.796(9) d SP 1
Cl21 Cl 0.6278(23) 0.0430(25) -0.1773(15) 0.077(12) Uani 0.102(4) d P 2
Cl3 Cl 0.5791(10) 0.0818(6) -0.1840(5) 0.114(3) Uani 0.50 d P .
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'
Cl Cl 0.1484 0.1585 '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'
S S 0.1246 0.1234 '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
N10 Pd1 N9 77.8(2) . . ?
N10 Pd1 C19 135.9(3) . . ?
N9 Pd1 C19 139.8(3) . . ?
N10 Pd1 C18 175.0(3) . . ?
N9 Pd1 C18 106.8(3) . . ?
C19 Pd1 C18 39.1(3) . . ?
N10 Pd1 C20 107.1(3) . . ?
N9 Pd1 C20 173.1(3) . . ?
C19 Pd1 C20 38.6(3) . . ?
C18 Pd1 C20 68.5(3) . . ?
C12 N8 C12 112.0(7) . 6 ?
C12 N9 C13 117.2(6) . . ?
C12 N9 Pd1 115.3(4) . . ?
C13 N9 Pd1 127.4(5) . . ?
C16 N10 N11 104.4(5) . . ?
C16 N10 Pd1 143.2(5) . . ?
N11 N10 Pd1 112.0(4) . . ?
C14 N11 N10 111.5(5) . . ?
C14 N11 C12 129.5(6) . . ?
N10 N11 C12 119.0(5) . . ?
N9 C12 N8 128.5(6) . . ?
N9 C12 N11 115.6(5) . . ?
N8 C12 N11 115.9(5) . . ?
O5 C13 N9 121.7(4) . . ?
O5 C13 N9 121.7(4) . 6 ?
N9 C13 N9 116.6(8) . 6 ?
N11 C14 C15 107.5(6) . . ?
C14 C15 C16 104.7(6) . . ?
C14 C15 C17 127.0(7) . . ?
C16 C15 C17 128.2(7) . . ?
N10 C16 C15 111.9(6) . . ?
C19 C18 Pd1 70.8(4) . . ?
C20 C19 C18 114.9(8) . . ?
C20 C19 C21 120.8(8) . . ?
C18 C19 C21 122.8(8) . . ?
C20 C19 Pd1 70.1(4) . . ?
C18 C19 Pd1 70.1(4) . . ?
C21 C19 Pd1 117.4(6) . . ?
C19 C20 Pd1 71.3(4) . . ?
O7 S4 O7 116.0(9) . 6 ?
O7 S4 O6 111.3(4) . . ?
O7 S4 O6 111.3(4) 6 . ?
O7 S4 C22 105.9(4) . . ?
O7 S4 C22 105.9(4) 6 . ?
O6 S4 C22 105.7(5) . . ?
C27 C22 C23 119.1(11) . . ?
C27 C22 S4 120.9(9) . . ?
C23 C22 S4 120.0(8) . . ?
C24 C23 C22 120.3(11) . . ?
C23 C24 C25 119.7(12) . . ?
C26 C25 C24 118.4(13) . . ?
C26 C25 C28 123.4(16) . . ?
C24 C25 C28 118.3(16) . . ?
C25 C26 C27 121.4(12) . . ?
C22 C27 C26 121.1(12) . . ?
Cl21 C29 Cl21 52.1(27) . 6 ?
Cl21 C29 Cl3 79.7(17) . 6 ?
Cl21 C29 Cl3 28.0(12) 6 6 ?
Cl21 C29 Cl3 28.0(12) . . ?
Cl21 C29 Cl3 79.7(17) 6 . ?
Cl3 C29 Cl3 106.6(13) 6 . ?
Cl3 C29 Cl2 112.3(9) 6 . ?
Cl3 C29 Cl2 112.3(9) . . ?
Cl3 Cl21 Cl21 142.9(29) . 6 ?
Cl3 Cl21 C29 80.7(22) . . ?
Cl21 Cl21 C29 63.9(13) 6 . ?
Cl3 Cl21 Cl3 129.7(33) . 6 ?
Cl21 Cl21 Cl3 13.2(6) 6 6 ?
C29 Cl21 Cl3 51.6(13) . 6 ?
Cl21 Cl3 C29 71.2(28) . . ?
Cl21 Cl3 Cl21 23.9(26) . 6 ?
C29 Cl3 Cl21 48.7(9) . 6 ?
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 N10 2.092(5) . ?
Pd1 N9 2.106(5) . ?
Pd1 C19 2.129(7) . ?
Pd1 C18 2.119(7) . ?
Pd1 C20 2.113(7) . ?
O5 C13 1.212(11) . ?
N8 C12 1.314(7) . ?
N8 C12 1.314(7) 6 ?
N9 C12 1.323(8) . ?
N9 C13 1.402(7) . ?
N10 C16 1.311(8) . ?
N10 N11 1.376(7) . ?
N11 C14 1.345(8) . ?
N11 C12 1.396(8) . ?
C13 N9 1.402(7) 6 ?
C14 C15 1.360(9) . ?
C15 C16 1.411(9) . ?
C15 C17 1.506(10) . ?
C18 C19 1.423(10) . ?
C19 C20 1.402(12) . ?
C19 C21 1.526(13) . ?
S4 O7 1.411(7) . ?
S4 O7 1.411(7) 6 ?
S4 O6 1.430(9) . ?
S4 C22 1.773(11) . ?
C22 C27 1.365(14) . ?
C22 C23 1.368(14) . ?
C23 C24 1.38(2) . ?
C24 C25 1.40(2) . ?
C25 C26 1.36(2) . ?
C25 C28 1.55(2) . ?
C26 C27 1.35(2) . ?
C29 Cl21 1.58(3) . ?
C29 Cl21 1.58(3) 6 ?
C29 Cl3 1.652(14) 6 ?
C29 Cl3 1.652(14) . ?
C29 Cl2 1.76(2) . ?
Cl21 Cl3 0.79(3) . ?
Cl21 Cl21 1.39(8) 6 ?
Cl21 Cl3 2.08(4) 6 ?
Cl3 Cl21 2.08(4) 6 ?
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_site_symmetry_2
_geom_contact_distance
_geom_contact_publ_flag
O5 Pd1 6_555 3.3865(28) ?
O5 N8 5_555 3.3188(96) ?
O5 N8 2_555 3.3188(96) ?
O5 N9 5_555 3.3568(82) ?
O5 N9 2_555 3.3568(82) ?
O5 N9 6_555 2.2847(87) ?
O5 C12 5_555 3.2971(84) ?
O5 C12 2_555 3.2971(84) ?
O5 C12 6_555 3.4420(99) ?
O5 C13 5_555 3.34(1) ?
O5 C13 2_555 3.34(1) ?
O5 C18 6_555 3.1693(81) ?
O5 H18A 6_555 2.8296(44) ?
O5 H18B 6_555 3.4179(33) ?
N8 O5 5_555 3.318(96) ?
N8 O5 2_555 3.318(96) ?
N8 N9 6_555 2.3749(90) ?
N8 N11 6_555 2.2972(53) ?
N8 C12 6_555 1.3143(76) ?
N8 C14 6_555 2.8292(79) ?
N8 H14 6_555 2.7053(58) ?
N8 H27 1_455 2.5875(70) ?
N8 H27 6_455 2.5875(70) ?
N9 O5 5_555 3.356(82) ?
N9 O5 2_555 3.356(82) ?
N9 N9 2_555 3.425(71) ?
N9 N9 6_555 2.3856(73) ?
N9 C12 6_555 2.6359(81) ?
N9 C13 5_555 3.413(98) ?
N9 C13 2_555 3.413(98) ?
N9 Cl21 2_655 3.29(2) ?
N10 H17B 7_555 2.8319(53) ?
N10 H18B 2_555 2.919(55) ?
N10 H20A 2_555 3.164(52) ?
N11 C12 6_555 3.4580(79) ?
N11 H17B 7_555 3.2409(50) ?
N11 H18B 2_555 2.8721(50) ?
N11 H27 1_455 3.4554(53) ?
N11 H27 6_455 3.4554(53) ?
C12 O5 5_555 3.2971(84) ?
C12 O5 2_555 3.2971(84) ?
C12 N9 6_555 2.6359(81) ?
C12 N11 6_555 3.4580(79) ?
C12 C12 6_555 2.1790(82) ?
C12 H18B 2_555 3.4926(59) ?
C12 H27 1_455 3.2461(60) ?
C12 H27 6_455 3.2461(60) ?
C13 Pd1 6_555 3.1609(08) ?
C13 O5 5_555 3.34(1) ?
C13 O5 2_555 3.34(1) ?
C13 N9 5_555 3.4132(98) ?
C13 N9 2_555 3.4132(98) ?
C13 N9 6_555 1.4022(77) ?
C13 C12 6_555 2.32(1) ?
C13 C13 5_555 3.13(1) ?
C13 C13 2_555 3.13(1) ?
C13 H18A 6_555 3.4967(79) ?
C13 Cl21 5_655 3.3135(79) ?
C13 Cl21 2_655 3.31(2) ?
C14 H18B 2_555 3.0910(63) ?
C14 O7 1_455 3.18(1) ?
C14 H27 1_455 3.2540(67) ?
C14 H27 6_455 3.2540(67) ?
H14 S4 1_455 3.4223(26) ?
H14 S4 6_455 3.4223(26) ?
H14 O7 1_455 2.3758(93) ?
H14 C27 1_455 3.4597(93) ?
H14 C27 6_455 3.4597(93) ?
H14 H27 1_455 2.8132(02) ?
H14 H27 6_455 2.8132(02) ?
H14 C29 5_555 3.40(1) ?
H14 C29 2_555 3.40(1) ?
H14 Cl2 5_555 3.4335(37) ?
H14 Cl2 2_555 3.4335(37) ?
C15 H17B 7_555 3.4921(70) ?
C15 H18B 2_555 3.2361(63) ?
C16 H17B 7_555 2.9664(74) ?
C16 H18B 2_555 3.1089(71) ?
C16 H20A 2_555 3.0546(71) ?
H16 H17B 7_555 3.2281(03) ?
H16 H20A 2_555 2.8571(06) ?
H16 O7 7_655 3.3966(78) ?
H16 C22 7_655 2.8891(31) ?
H16 C22 4_655 2.8891(31) ?
H16 C23 7_655 3.0614(44) ?
H16 C23 4_655 3.0614(44) ?
H16 C24 7_655 3.3134(75) ?
H16 C24 4_655 3.3134(75) ?
H16 C25 7_655 3.4012(78) ?
H16 C25 4_655 3.4012(78) ?
H16 C26 7_655 3.2277(75) ?
H16 C26 4_655 3.2277(75) ?
H16 C27 7_655 2.9736(41) ?
H16 C27 4_655 2.9736(41) ?
H16 H27 7_655 3.3944(03) ?
H16 H27 4_655 3.3944(03) ?
C17 Cl3 8_455 3.4899(32) ?
H17A C25 7_655 3.3966(16) ?
H17A C25 4_655 3.39(1) ?
H17A C26 7_655 2.7829(59) ?
H17A C26 4_655 2.7829(59) ?
H17A H26 7_655 2.5720(02) ?
H17A H26 4_655 2.5720(02) ?
H17A C27 7_655 3.2354(81) ?
H17A C27 4_655 3.2354(81) ?
H17A H27 7_655 3.3435(02) ?
H17A H27 4_655 3.3435(02) ?
H17A H28B 7_655 3.3989(04) ?
H17A H28C 4_655 3.3989(04) ?
H17A Cl21 8_455 3.2460(42) ?
H17A Cl3 8_455 3.1351(01) ?
H17B N10 7_555 2.8319(53) ?
H17B N11 7_555 3.2409(50) ?
H17B C15 7_555 3.4921(70) ?
H17B C16 7_555 2.9664(74) ?
H17B H16 7_555 3.2281(03) ?
H17B H21B 7_555 3.0124(04) ?
H17B O7 1_455 3.2315(94) ?
H17B Cl3 8_455 3.4049(95) ?
H17C C21 1_455 3.14(1) ?
H17C H21A 1_455 2.9126(06) ?
H17C H21B 1_455 2.8479(04) ?
H17C H21B 7_555 3.3457(07) ?
H17C H21C 1_455 3.1462(06) ?
H17C Cl3 8_455 3.3588(96) ?
C18 H18A 2_655 3.2904(83) ?
C18 H21A 2_655 3.0212(86) ?
H18A C18 2_655 3.2904(83) ?
H18A H18A 2_655 2.6428(03) ?
H18A H18B 2_655 3.4449(03) ?
H18A H21A 2_655 3.0726(05) ?
H18A Cl2 5_655 3.3683(32) ?
H18A Cl2 2_655 3.3683(32) ?
H18B N10 2_555 2.9192(55) ?
H18B N11 2_555 2.8721(50) ?
H18B C12 2_555 3.4926(59) ?
H18B C14 2_555 3.0910(63) ?
H18B C15 2_555 3.2361(63) ?
H18B C16 2_555 3.1089(71) ?
H18B H18A 2_655 3.4449(03) ?
H18B C21 2_655 3.3725(09) ?
H18B H21A 2_655 2.5541(03) ?
H18B H21C 2_655 3.4608(02) ?
C19 H21A 2_655 3.4955(87) ?
C20 O6 7_655 3.4209(83) ?
C20 O6 4_655 3.4209(83) ?
C20 H24 3_454 3.2957(73) ?
C20 H24 8_454 3.2957(73) ?
H20A N10 2_555 3.1648(52) ?
H20A C16 2_555 3.0546(71) ?
H20A H16 2_555 2.8571(06) ?
H20A H20A 2_555 3.4878(04) ?
H20A C23 3_454 3.3643(55) ?
H20A C23 8_454 3.3643(55) ?
H20A H23 3_454 3.3972(02) ?
H20A H23 8_454 3.3972(02) ?
H20A C24 3_454 3.0355(59) ?
H20A C24 8_454 3.0355(59) ?
H20A H24 3_454 2.8343(02) ?
H20A H24 8_454 2.8343(02) ?
H20B S4 7_655 3.1775(21) ?
H20B S4 4_655 3.1775(21) ?
H20B O6 7_655 2.5190(32) ?
H20B O6 4_655 2.5190(32) ?
H20B O7 7_655 3.0751(91) ?
H20B C23 7_655 3.3836(84) ?
H20B C23 4_655 3.3836(84) ?
H20B H23 7_655 2.9377(02) ?
H20B H23 4_655 2.9377(02) ?
H20B H24 3_454 3.0117(03) ?
H20B H24 8_454 3.0117(03) ?
C21 H17C 1_655 3.1439(00) ?
C21 H18B 2_655 3.37(1) ?
C21 H28B 7_755 3.09(1) ?
C21 H28C 4_755 3.09(1) ?
H21A H17C 1_655 2.9126(06) ?
H21A C18 2_655 3.0212(86) ?
H21A H18A 2_655 3.0726(05) ?
H21A H18B 2_655 2.5541(03) ?
H21A C19 2_655 3.4955(87) ?
H21A Cl3 2_655 3.2804(96) ?
H21B H17B 7_555 3.0124(04) ?
H21B H17C 1_655 2.8479(04) ?
H21B H17C 7_555 3.3457(07) ?
H21B O7 7_655 3.3515(92) ?
H21B H28B 7_755 3.2886(02) ?
H21B H28C 4_755 3.2886(02) ?
H21B Cl3 2_655 3.2139(91) ?
H21C H17C 1_655 3.1462(06) ?
H21C H18B 2_655 3.4608(02) ?
H21C C28 7_755 2.9903(58) ?
H21C C28 4_755 2.9903(58) ?
H21C H28A 7_755 3.0420(02) ?
H21C H28A 4_755 3.0420(02) ?
H21C H28B 7_755 2.1894(01) ?
H21C H28C 4_755 2.1894(01) ?
S4 H14 1_655 3.4223(26) ?
S4 H14 6_655 3.4223(26) ?
S4 H20B 7_655 3.1775(21) ?
S4 H20B 4_645 3.1775(21) ?
S4 O7 6_555 1.4113(92) ?
O6 C20 7_655 3.4209(83) ?
O6 C20 4_645 3.4209(83) ?
O6 H20B 7_655 2.5190(32) ?
O6 H20B 4_645 2.5190(32) ?
O6 O7 6_555 2.34(1) ?
O6 H24 5_756 2.7746(88) ?
O6 H24 2_756 2.7746(88) ?
O6 C28 1_455 3.15(2) ?
O6 C28 6_455 3.15(2) ?
O6 H28A 1_455 3.2311(91) ?
O6 H28A 6_455 3.2311(91) ?
O6 H28B 1_455 2.8544(82) ?
O6 H28B 6_455 2.8544(82) ?
O6 H28C 1_455 2.8544(82) ?
O6 H28C 6_455 2.8544(82) ?
O7 C14 1_655 3.18(1) ?
O7 H14 1_655 2.3758(93) ?
O7 H16 7_655 3.3966(78) ?
O7 H17B 1_655 3.2315(94) ?
O7 H20B 7_655 3.0751(91) ?
O7 H21B 7_655 3.3515(92) ?
O7 O7 6_555 2.39(1) ?
O7 C29 5_655 3.42(1) ?
O7 C29 2_655 3.42(1) ?
C22 H16 7_655 2.8891(31) ?
C22 H16 4_645 2.8891(31) ?
C22 O7 6_555 2.55(1) ?
C23 H16 7_655 3.0614(44) ?
C23 H16 4_645 3.0614(44) ?
C23 H20A 3_645 3.3643(55) ?
C23 H20A 8_655 3.3643(55) ?
C23 H20B 7_655 3.3836(84) ?
C23 H20B 4_645 3.3836(84) ?
C23 H23 5_756 2.90(1) ?
C23 H23 2_756 2.90(1) ?
H23 H20A 3_645 3.3972(02) ?
H23 H20A 8_655 3.3972(02) ?
H23 H20B 7_655 2.9377(02) ?
H23 H20B 4_645 2.9377(02) ?
H23 C23 5_756 2.90(1) ?
H23 C23 2_756 2.90(1) ?
H23 H23 5_756 2.1765(05) ?
H23 H23 2_756 2.1765(05) ?
H23 C24 5_756 3.17(1) ?
H23 C24 2_756 3.17(1) ?
H23 H24 5_756 2.7268(04) ?
H23 H24 2_756 2.7268(04) ?
C24 H16 7_655 3.3134(75) ?
C24 H16 4_645 3.3134(75) ?
C24 H20A 3_645 3.0355(59) ?
C24 H20A 8_655 3.0355(59) ?
C24 H23 5_756 3.17(1) ?
C24 H23 2_756 3.17(1) ?
C24 H28B 6_555 3.14(1) ?
C24 H28C 6_555 3.14(1) ?
H24 C20 3_645 3.2957(73) ?
H24 C20 8_655 3.2957(73) ?
H24 H20A 3_645 2.8343(02) ?
H24 H20A 8_655 2.8343(02) ?
H24 H20B 3_645 3.0117(03) ?
H24 H20B 8_655 3.0117(03) ?
H24 O6 5_756 2.7746(88) ?
H24 O6 2_756 2.7746(88) ?
H24 H23 5_756 2.7268(04) ?
H24 H23 2_756 2.7268(04) ?
H24 H28B 6_555 3.3094(04) ?
H24 H28C 6_555 3.3094(04) ?
C25 H16 7_655 3.4012(78) ?
C25 H16 4_645 3.4012(78) ?
C25 H17A 7_655 3.39(1) ?
C25 H17A 4_645 3.39(1) ?
C25 H28B 6_555 2.07(1) ?
C25 H28C 6_555 2.07(1) ?
C26 H16 7_655 3.2277(75) ?
C26 H16 4_645 3.2277(75) ?
C26 H17A 7_655 2.7829(59) ?
C26 H17A 4_645 2.7829(59) ?
C26 H28B 6_555 2.81(1) ?
C26 H28C 6_555 2.81(1) ?
H26 H17A 7_655 2.5720(02) ?
H26 H17A 4_645 2.5720(02) ?
H26 H28B 6_555 2.7685(04) ?
H26 H28C 6_555 2.7685(04) ?
H26 Cl21 5_755 2.89(3) ?
H26 Cl21 2_755 2.89(3) ?
H26 Cl3 5_755 3.28(1) ?
H26 Cl3 2_755 3.28(1) ?
C27 H14 1_655 3.4597(93) ?
C27 H14 6_655 3.4597(93) ?
C27 H16 7_655 2.9736(41) ?
C27 H16 4_645 2.9736(41) ?
C27 H17A 7_655 3.2354(81) ?
C27 H17A 4_645 3.2354(81) ?
C27 O7 6_555 3.14(1) ?
H27 N8 1_655 2.5875(70) ?
H27 N8 6_655 2.5875(70) ?
H27 N11 1_655 3.4554(53) ?
H27 N11 6_655 3.4554(53) ?
H27 C12 1_655 3.2461(60) ?
H27 C12 6_655 3.2461(60) ?
H27 C14 1_655 3.2540(67) ?
H27 C14 6_655 3.2540(67) ?
H27 H14 1_655 2.8132(02) ?
H27 H14 6_655 2.8132(02) ?
H27 H16 7_655 3.3944(03) ?
H27 H16 4_645 3.3944(03) ?
H27 H17A 7_655 3.3435(02) ?
H27 H17A 4_645 3.3435(02) ?
H27 O7 6_555 2.9984(84) ?
C28 H21C 7_755 2.9903(58) ?
C28 H21C 2_745 2.9903(58) ?
C28 O6 1_655 3.1518(04) ?
C28 O6 6_655 3.15(2) ?
C28 H28B 6_555 0.96(1) ?
C28 H28C 6_555 0.96(1) ?
H28A H21C 7_755 3.0420(02) ?
H28A H21C 2_745 3.0420(02) ?
H28A O6 1_655 3.2311(91) ?
H28A O6 6_655 3.2311(91) ?
H28A H28B 6_555 1.5677(03) ?
H28A H28C 6_555 1.5677(03) ?
H28B H17A 7_655 3.3989(04) ?
H28B C21 7_755 3.0936(13) ?
H28B H21B 7_755 3.2886(02) ?
H28B H21C 7_755 2.1894(01) ?
H28B O6 1_655 2.8544(82) ?
H28B O6 6_655 2.8544(82) ?
H28B H28B 6_555 1.5677(01) ?
H28C H17A 4_645 3.3989(4) ?
H28C C21 2_745 3.09(1) ?
H28C H21B 2_745 3.2886(02) ?
H28C H21C 2_745 2.1894(01) ?
H28C O6 1_655 2.8544(82) ?
H28C O6 6_655 2.8544(82) ?
H28C H28C 6_555 1.5677(01) ?
C29 H14 5_555 3.40(1) ?
C29 H14 2_555 3.40(1) ?
C29 O7 5_655 3.42(1) ?
C29 O7 2_655 3.42(1) ?
C29 Cl21 6_555 1.58(3) ?
C29 Cl3 6_555 1.65(1) ?
Cl2 H14 5_555 3.4335(37) ?
Cl2 H14 2_555 3.4335(37) ?
Cl2 H18A 5_655 3.3683(32) ?
Cl2 H18A 6_555 3.4533(38) ?
Cl2 H18A 2_655 3.3683(32) ?
Cl2 Cl21 6_555 2.8562(98) ?
Cl2 Cl3 6_555 2.83(1) ?
Cl21 N9 2_655 3.28(2) ?
Cl21 C13 5_655 3.31(2) ?
Cl21 C13 2_655 3.31(2) ?
Cl21 H17A 8_656 3.24(3) ?
Cl21 H26 5_755 2.89(3) ?
Cl21 H26 2_755 2.89(3) ?
Cl21 Cl21 6_555 1.39(5) ?
Cl21 Cl3 6_555 2.07(4) ?
Cl3 C17 8_656 3.48(1) ?
Cl3 H17A 8_656 3.13(1) ?
Cl3 H17B 8_656 3.4049(95) ?
Cl3 H17C 8_656 3.3588(96) ?
Cl3 H21A 2_655 3.2804(96) ?
Cl3 H21B 2_655 3.2139(91) ?
Cl3 H26 5_755 3.28(1) ?
Cl3 H26 2_755 3.28(1) ?
Cl3 Cl21 6_555 2.07(4) ?
Cl3 Cl3 6_555 2.64(1) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C14 H14 N8 0.930(7) 2.829(8) 2.705(6) 87.96(4) . ?
C18 H18A O5 0.970(8) 3.169(8) 2.830(4) 101.53(46) . ?
C23 H23 O6 0.930(11) 2.850(14) 2.453(8) 105.75(72) . ?
C27 H27 O7 0.930(11) 3.146(14) 2.998(8) 90.45(17) . ?
C14 H14 O7 0.930(7) 3.182(12) 2.376(9) 144.88(46) 1_455 ?
C20 H20B O6 0.970(8) 3.421(08) 2.519(3) 154.62(43) 7_655 ?
C24 H24 O6 0.930(14) 3.675(17) 2.775(9) 163.23(90) 5_756 ?
C27 H27 N8 0.930(11) 3.501(13) 2.587(7) 167.45(70) 1_655 ?
