#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:37:30 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179730 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/26/7002673.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_7002673
loop_
_publ_author_name
'Ruiz, José'
'Cutillas, Natalia'
'Villa, María Dolores'
'López, Gregorio'
'Espinosa, Arturo'
'Bautista, Delia'
_publ_section_title
;
 N1-Coordination in palladium(II) and platinum(II) complexes with
 9-methylhypoxanthine: crystal structures and theoretical calculations
;
_journal_issue                   43
_journal_name_full               'Dalton Transactions'
_journal_page_first              9637
_journal_page_last               9644
_journal_paper_doi               10.1039/b915427b
_journal_year                    2009
_chemical_formula_sum            'C33 H33 Cl N5 O5 P Pt'
_chemical_formula_weight         841.15
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.609(2)
_cell_angle_beta                 100.862(2)
_cell_angle_gamma                102.408(2)
_cell_formula_units_Z            2
_cell_length_a                   8.8061(4)
_cell_length_b                   9.5922(5)
_cell_length_c                   19.6841(11)
_cell_measurement_reflns_used    7735
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.12
_cell_measurement_theta_min      2.42
_cell_volume                     1582.07(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART APEX'
_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  0.0140
_diffrn_reflns_av_sigmaI/netI    0.0163
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17320
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    4.620
_exptl_absorpt_correction_T_max  0.5072
_exptl_absorpt_correction_T_min  0.3285
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.873
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    'NH free,methyls rigid,others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         6396
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0162
_refine_ls_R_factor_gt           0.0158
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0200P)²+1.3715P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0392
_refine_ls_wR_factor_ref         0.0394
_reflns_number_gt                6301
_reflns_number_total             6396
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b915427b.txt
_cod_data_source_block           md485bs
_cod_database_code               7002673
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -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
Pt1 Pt 0.165833(8) 0.267734(7) 0.728189(4) 0.01155(3) Uani 1 1 d . . .
P1 P 0.10171(6) 0.37279(5) 0.82070(3) 0.01236(10) Uani 1 1 d . . .
O1 O 0.39958(18) 0.56454(17) 0.66524(9) 0.0225(3) Uani 1 1 d . . .
N1 N 0.2801(2) 0.68776(19) 0.58470(10) 0.0166(4) Uani 1 1 d . . .
H01 H 0.368(4) 0.730(3) 0.5829(16) 0.031(8) Uiso 1 1 d . . .
C2 C 0.1507(3) 0.7205(2) 0.54564(11) 0.0179(4) Uani 1 1 d . . .
H2 H 0.1692 0.7930 0.5160 0.022 Uiso 1 1 calc R . .
N3 N 0.0036(2) 0.66008(19) 0.54568(9) 0.0164(4) Uani 1 1 d . . .
C4 C -0.0067(2) 0.5559(2) 0.58854(11) 0.0138(4) Uani 1 1 d . . .
C5 C 0.1158(2) 0.5106(2) 0.62853(11) 0.0137(4) Uani 1 1 d . . .
C6 C 0.2768(3) 0.5832(2) 0.63059(11) 0.0150(4) Uani 1 1 d . . .
N7 N 0.0528(2) 0.39465(18) 0.66075(9) 0.0140(3) Uani 1 1 d . . .
C8 C -0.1032(3) 0.3741(2) 0.64058(11) 0.0160(4) Uani 1 1 d . . .
H8 H -0.1775 0.3007 0.6547 0.019 Uiso 1 1 calc R . .
N9 N -0.1455(2) 0.46923(19) 0.59751(9) 0.0150(4) Uani 1 1 d . . .
C10 C -0.3072(3) 0.4846(3) 0.56945(12) 0.0211(5) Uani 1 1 d . . .
H10A H -0.3763 0.3898 0.5502 0.032 Uiso 1 1 calc R . .
H10B H -0.3044 0.5473 0.5325 0.032 Uiso 1 1 calc R . .
H10C H -0.3489 0.5271 0.6069 0.032 Uiso 1 1 calc R . .
N10 N 0.2411(2) 0.16155(18) 0.64522(9) 0.0126(3) Uani 1 1 d . . .
C11 C 0.2633(2) 0.1269(2) 0.78188(11) 0.0138(4) Uani 1 1 d . . .
C12 C 0.3080(3) 0.1247(2) 0.85381(11) 0.0168(4) Uani 1 1 d . . .
H12 H 0.2940 0.1997 0.8848 0.020 Uiso 1 1 calc R . .
C13 C 0.3726(3) 0.0156(2) 0.88129(12) 0.0182(4) Uani 1 1 d . . .
H13 H 0.3990 0.0158 0.9304 0.022 Uiso 1 1 calc R . .
C14 C 0.3985(3) -0.0930(2) 0.83738(12) 0.0177(4) Uani 1 1 d . . .
H14 H 0.4429 -0.1672 0.8561 0.021 Uiso 1 1 calc R . .
C15 C 0.3588(3) -0.0924(2) 0.76584(12) 0.0173(4) Uani 1 1 d . . .
H15 H 0.3790 -0.1649 0.7353 0.021 Uiso 1 1 calc R . .
C16 C 0.2897(2) 0.0142(2) 0.73859(11) 0.0143(4) Uani 1 1 d . . .
C17 C 0.2345(3) 0.0111(2) 0.66154(11) 0.0152(4) Uani 1 1 d . . .
H17A H 0.3036 -0.0325 0.6364 0.018 Uiso 1 1 calc R . .
H17B H 0.1242 -0.0478 0.6463 0.018 Uiso 1 1 calc R . .
C18 C 0.4104(3) 0.2311(2) 0.64591(12) 0.0192(4) Uani 1 1 d . . .
H18A H 0.4438 0.1848 0.6069 0.029 Uiso 1 1 calc R . .
H18B H 0.4780 0.2207 0.6899 0.029 Uiso 1 1 calc R . .
H18C H 0.4206 0.3335 0.6414 0.029 Uiso 1 1 calc R . .
C19 C 0.1452(3) 0.1558(2) 0.57419(11) 0.0206(5) Uani 1 1 d . . .
H19A H 0.1825 0.0965 0.5410 0.031 Uiso 1 1 calc R . .
H19B H 0.1565 0.2534 0.5611 0.031 Uiso 1 1 calc R . .
H19C H 0.0330 0.1137 0.5735 0.031 Uiso 1 1 calc R . .
C21 C -0.0309(2) 0.4922(2) 0.79931(11) 0.0143(4) Uani 1 1 d . . .
C22 C -0.1957(3) 0.4459(2) 0.79029(11) 0.0174(4) Uani 1 1 d . . .
H22 H -0.2414 0.3541 0.8018 0.021 Uiso 1 1 calc R . .
C23 C -0.2928(3) 0.5348(3) 0.76435(12) 0.0194(4) Uani 1 1 d . . .
H23 H -0.4050 0.5025 0.7576 0.023 Uiso 1 1 calc R . .
C24 C -0.2280(3) 0.6694(2) 0.74826(12) 0.0203(5) Uani 1 1 d . . .
H24 H -0.2956 0.7289 0.7304 0.024 Uiso 1 1 calc R . .
C25 C -0.0638(3) 0.7176(2) 0.75820(12) 0.0218(5) Uani 1 1 d . . .
H25 H -0.0188 0.8107 0.7480 0.026 Uiso 1 1 calc R . .
C26 C 0.0345(3) 0.6289(2) 0.78317(12) 0.0181(4) Uani 1 1 d . . .
H26 H 0.1466 0.6613 0.7893 0.022 Uiso 1 1 calc R . .
C31 C -0.0020(3) 0.2450(2) 0.86982(12) 0.0169(4) Uani 1 1 d . . .
C32 C -0.1046(3) 0.1197(2) 0.83186(13) 0.0218(5) Uani 1 1 d . . .
H32 H -0.1153 0.1031 0.7828 0.026 Uiso 1 1 calc R . .
C33 C -0.1910(3) 0.0194(3) 0.86573(15) 0.0288(6) Uani 1 1 d . . .
H33 H -0.2625 -0.0646 0.8396 0.035 Uiso 1 1 calc R . .
C34 C -0.1732(3) 0.0416(3) 0.93741(15) 0.0298(6) Uani 1 1 d . . .
H34 H -0.2322 -0.0274 0.9604 0.036 Uiso 1 1 calc R . .
C35 C -0.0698(3) 0.1640(3) 0.97577(13) 0.0261(5) Uani 1 1 d . . .
H35 H -0.0563 0.1779 1.0251 0.031 Uiso 1 1 calc R . .
C36 C 0.0144(3) 0.2667(2) 0.94213(12) 0.0198(4) Uani 1 1 d . . .
H36 H 0.0833 0.3518 0.9684 0.024 Uiso 1 1 calc R . .
C41 C 0.2716(2) 0.4911(2) 0.88101(11) 0.0142(4) Uani 1 1 d . . .
C42 C 0.4246(3) 0.4907(2) 0.87212(11) 0.0162(4) Uani 1 1 d . . .
H42 H 0.4393 0.4263 0.8360 0.019 Uiso 1 1 calc R . .
C43 C 0.5562(3) 0.5840(2) 0.91579(11) 0.0183(4) Uani 1 1 d . . .
H43 H 0.6603 0.5840 0.9091 0.022 Uiso 1 1 calc R . .
C44 C 0.5351(3) 0.6765(2) 0.96884(11) 0.0179(4) Uani 1 1 d . . .
H44 H 0.6251 0.7391 0.9990 0.021 Uiso 1 1 calc R . .
C45 C 0.3833(3) 0.6788(2) 0.97843(11) 0.0182(4) Uani 1 1 d . . .
H45 H 0.3695 0.7425 1.0151 0.022 Uiso 1 1 calc R . .
C46 C 0.2520(3) 0.5875(2) 0.93424(11) 0.0168(4) Uani 1 1 d . . .
H46 H 0.1480 0.5903 0.9401 0.020 Uiso 1 1 calc R . .
Cl1 Cl 0.68658(6) 0.93790(6) 0.59991(3) 0.02063(11) Uani 1 1 d . . .
O2 O 0.5762(2) 0.8213(2) 0.55214(10) 0.0366(5) Uani 1 1 d . . .
O3 O 0.8321(2) 0.8960(2) 0.62230(12) 0.0425(5) Uani 1 1 d . . .
O4 O 0.7147(2) 1.06295(19) 0.56438(11) 0.0365(4) Uani 1 1 d . . .
O5 O 0.6184(3) 0.9661(2) 0.65851(11) 0.0428(5) Uani 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'
P P 0.1023 0.0942 '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'
Pt Pt -1.7033 8.3905 '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
C11 Pt1 N7 172.66(7) . . ?
C11 Pt1 N10 81.46(8) . . ?
N7 Pt1 N10 92.67(7) . . ?
C11 Pt1 P1 94.34(6) . . ?
N7 Pt1 P1 91.64(5) . . ?
N10 Pt1 P1 175.46(5) . . ?
C31 P1 C21 104.24(10) . . ?
C31 P1 C41 108.15(10) . . ?
C21 P1 C41 102.56(10) . . ?
C31 P1 Pt1 113.30(7) . . ?
C21 P1 Pt1 114.09(7) . . ?
C41 P1 Pt1 113.53(7) . . ?
C2 N1 C6 125.74(19) . . ?
N3 C2 N1 125.1(2) . . ?
C2 N3 C4 111.70(18) . . ?
N3 C4 N9 125.41(19) . . ?
N3 C4 C5 128.1(2) . . ?
N9 C4 C5 106.38(18) . . ?
C4 C5 N7 109.40(18) . . ?
C4 C5 C6 119.32(19) . . ?
N7 C5 C6 131.27(19) . . ?
O1 C6 N1 121.1(2) . . ?
O1 C6 C5 129.0(2) . . ?
N1 C6 C5 109.89(18) . . ?
C8 N7 C5 104.97(17) . . ?
C8 N7 Pt1 123.97(14) . . ?
C5 N7 Pt1 131.05(14) . . ?
N7 C8 N9 112.62(19) . . ?
C8 N9 C4 106.61(17) . . ?
C8 N9 C10 127.29(19) . . ?
C4 N9 C10 125.98(18) . . ?
C19 N10 C18 108.64(17) . . ?
C19 N10 C17 108.65(16) . . ?
C18 N10 C17 107.75(16) . . ?
C19 N10 Pt1 116.12(13) . . ?
C18 N10 Pt1 109.44(13) . . ?
C17 N10 Pt1 105.93(12) . . ?
C12 C11 C16 116.37(19) . . ?
C12 C11 Pt1 130.45(16) . . ?
C16 C11 Pt1 113.18(15) . . ?
C13 C12 C11 122.0(2) . . ?
C14 C13 C12 120.3(2) . . ?
C13 C14 C15 119.3(2) . . ?
C14 C15 C16 120.2(2) . . ?
C15 C16 C11 121.8(2) . . ?
C15 C16 C17 121.28(19) . . ?
C11 C16 C17 116.86(18) . . ?
N10 C17 C16 109.03(16) . . ?
C22 C21 C26 119.3(2) . . ?
C22 C21 P1 122.17(16) . . ?
C26 C21 P1 118.00(16) . . ?
C23 C22 C21 119.7(2) . . ?
C24 C23 C22 120.8(2) . . ?
C23 C24 C25 119.9(2) . . ?
C24 C25 C26 119.8(2) . . ?
C25 C26 C21 120.4(2) . . ?
C36 C31 C32 119.2(2) . . ?
C36 C31 P1 123.70(17) . . ?
C32 C31 P1 117.08(17) . . ?
C33 C32 C31 120.2(2) . . ?
C34 C33 C32 120.1(2) . . ?
C33 C34 C35 120.3(2) . . ?
C34 C35 C36 120.0(2) . . ?
C35 C36 C31 120.2(2) . . ?
C42 C41 C46 119.05(19) . . ?
C42 C41 P1 119.28(16) . . ?
C46 C41 P1 121.60(16) . . ?
C41 C42 C43 120.5(2) . . ?
C44 C43 C42 119.8(2) . . ?
C43 C44 C45 120.6(2) . . ?
C46 C45 C44 119.6(2) . . ?
C45 C46 C41 120.4(2) . . ?
O3 Cl1 O5 109.99(13) . . ?
O3 Cl1 O4 109.94(12) . . ?
O5 Cl1 O4 110.52(13) . . ?
O3 Cl1 O2 108.91(13) . . ?
O5 Cl1 O2 108.63(13) . . ?
O4 Cl1 O2 108.81(12) . . ?
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
Pt1 C11 2.016(2) . ?
Pt1 N7 2.1253(18) . ?
Pt1 N10 2.1390(17) . ?
Pt1 P1 2.2333(5) . ?
P1 C31 1.820(2) . ?
P1 C21 1.822(2) . ?
P1 C41 1.822(2) . ?
O1 C6 1.221(3) . ?
N1 C2 1.361(3) . ?
N1 C6 1.402(3) . ?
C2 N3 1.300(3) . ?
N3 C4 1.358(3) . ?
C4 N9 1.373(3) . ?
C4 C5 1.382(3) . ?
C5 N7 1.388(3) . ?
C5 C6 1.431(3) . ?
N7 C8 1.323(3) . ?
C8 N9 1.357(3) . ?
N9 C10 1.471(3) . ?
N10 C19 1.481(3) . ?
N10 C18 1.494(3) . ?
N10 C17 1.494(3) . ?
C11 C12 1.400(3) . ?
C11 C16 1.409(3) . ?
C12 C13 1.393(3) . ?
C13 C14 1.384(3) . ?
C14 C15 1.386(3) . ?
C15 C16 1.391(3) . ?
C16 C17 1.499(3) . ?
C21 C22 1.396(3) . ?
C21 C26 1.402(3) . ?
C22 C23 1.392(3) . ?
C23 C24 1.382(3) . ?
C24 C25 1.391(3) . ?
C25 C26 1.392(3) . ?
C31 C36 1.397(3) . ?
C31 C32 1.398(3) . ?
C32 C33 1.388(3) . ?
C33 C34 1.384(4) . ?
C34 C35 1.384(4) . ?
C35 C36 1.390(3) . ?
C41 C42 1.391(3) . ?
C41 C46 1.402(3) . ?
C42 C43 1.392(3) . ?
C43 C44 1.382(3) . ?
C44 C45 1.389(3) . ?
C45 C46 1.387(3) . ?
Cl1 O3 1.4265(19) . ?
Cl1 O5 1.430(2) . ?
Cl1 O4 1.4359(18) . ?
Cl1 O2 1.4490(19) . ?
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
N1 H01 O2 0.80(3) 2.08(3) 2.859(3) 166(3) .
C2 H2 O4 0.95 2.41 3.323(3) 160.8 2_676
C17 H17B O3 0.99 2.46 3.394(3) 157.9 1_445
