#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2012590.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2012590
loop_
_publ_author_name
'Kato, Masako'
'Ogawa, Yuki'
'Kozakai, Mikiko'
'Sugimoto, Yukihiro'
_publ_section_title
;
Bis(8-quinolinolato-N,O)platinum(II) and its synthetic
intermediate, 8-hydroxyquinolinium
dichloro(8-quinolinolato-N,O)platinate(II) tetrahydrate
;
_journal_issue 3
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first m147
_journal_page_last m149
_journal_volume 58
_journal_year 2002
_chemical_formula_iupac '[Pt (C9 H6 N O)2]'
_chemical_formula_moiety 'C18 H12 N2 O2 Pt'
_chemical_formula_sum 'C18 H12 N2 O2 Pt'
_chemical_formula_weight 483.39
_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'
_cell_angle_alpha 90
_cell_angle_beta 106.430(10)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 11.349(2)
_cell_length_b 4.704(2)
_cell_length_c 13.7310(10)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 294.2
_cell_measurement_theta_max 15.0
_cell_measurement_theta_min 14.6
_cell_volume 703.1(3)
_computing_cell_refinement 'Rigaku/AFC Diffractometer Control Software'
_computing_data_collection
'Rigaku/AFC Diffractometer Control Software (Rigaku, 1995)'
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 2000)'
_computing_molecular_graphics 'ORTEPII (Johnson, 1976)'
_computing_publication_material TEXSAN
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_diffrn_measured_fraction_theta_full 1.0
_diffrn_measured_fraction_theta_max 1.0
_diffrn_measurement_device_type 'Rigaku AFC-7R'
_diffrn_measurement_method \w/2\q
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength .7107
_diffrn_reflns_av_R_equivalents .015
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 0
_diffrn_reflns_limit_k_min -6
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 1685
_diffrn_reflns_theta_full 27.49
_diffrn_reflns_theta_max 27.49
_diffrn_reflns_theta_min 2.06
_diffrn_standards_decay_% 1.65
_diffrn_standards_interval_count 150
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 9.951
_exptl_absorpt_correction_T_max .822
_exptl_absorpt_correction_T_min .397
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details '(de Meulenaer & Tompa, 1965)'
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 2.283
_exptl_crystal_density_meas 'not measured'
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 456.00
_exptl_crystal_size_max .21
_exptl_crystal_size_mid .10
_exptl_crystal_size_min .02
_refine_diff_density_max .83
_refine_diff_density_min -.43
_refine_ls_extinction_coef .0006
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref .971
_refine_ls_hydrogen_treatment constr
_refine_ls_number_parameters 107
_refine_ls_number_reflns 1607
_refine_ls_R_factor_gt .018
_refine_ls_shift/su_max .005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.0181P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref .045
_reflns_number_gt 1053
_reflns_number_total 1607
_reflns_threshold_expression I>2\s(I)
_[local]_cod_data_source_file oa1121.cif
_[local]_cod_data_source_block I
_cod_original_cell_volume 703.0(3)
_cod_database_code 2012590
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2+y,1/2-z
-x,-y,-z
1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Pt1 .0000 .0000 .0000 .02828(9) Uani d S 1.00 Pt
O1 -.1716(3) .1457(7) -.0629(2) .0351(7) Uani d . 1.00 O
N1 -.0042(3) .2755(8) .1092(3) .0303(8) Uani d . 1.00 N
C1 .0835(4) .3380(10) .1928(3) .0350(10) Uani d . 1.00 C
C2 .0646(4) .5360(10) .2631(3) .0430(10) Uani d . 1.00 C
C3 -.0448(4) .6720(10) .2469(3) .0400(10) Uani d . 1.00 C
C4 -.1410(4) .6150(10) .1570(3) .0330(10) Uani d . 1.00 C
C5 -.2580(4) .7420(10) .1312(4) .0410(10) Uani d . 1.00 C
C6 -.3420(4) .6680(10) .0424(4) .0430(10) Uani d . 1.00 C
C7 -.3170(4) .4650(10) -.0246(4) .0410(10) Uani d . 1.00 C
C8 -.2039(4) .3350(10) -.0036(3) .0316(10) Uani d . 1.00 C
C9 -.1157(4) .4122(9) .0897(3) .0293(10) Uani d . 1.00 C
H1 .1620 .2457 .2057 .0349 Uiso calc . 1.00 H
H2 .1303 .5832 .3239 .0427 Uiso calc . 1.00 H
H3 -.0603 .8029 .2965 .0397 Uiso calc . 1.00 H
H4 -.2772 .8820 .1769 .0412 Uiso calc . 1.00 H
H5 -.4212 .7566 .0246 .0428 Uiso calc . 1.00 H
H6 -.3794 .4211 -.0863 .0408 Uiso calc . 1.00 H
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Pt1 .02730(10) .02680(10) .03090(10) .00010(10) .00834(8) .0000(2)
O1 .0270(10) .037(2) .038(2) .001(2) .0020(10) -.003(2)
N1 .030(2) .028(2) .033(2) .001(2) .0090(10) .003(2)
C1 .031(2) .034(3) .039(2) .004(2) .008(2) .002(2)
C2 .042(2) .047(4) .037(2) -.007(3) .008(2) -.008(2)
C3 .047(3) .037(3) .036(2) -.003(2) .013(2) -.010(2)
C4 .038(2) .030(2) .035(2) -.002(2) .016(2) .002(2)
C5 .043(3) .040(3) .046(3) .002(2) .022(2) -.001(2)
C6 .034(2) .044(3) .051(3) .012(2) .014(2) .006(3)
C7 .033(2) .039(3) .046(2) -.003(2) .005(2) .000(2)
C8 .031(2) .029(2) .037(2) .000(2) .013(2) .002(2)
C9 .035(2) .025(2) .031(2) -.002(2) .014(2) .007(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pt Pt -1.703 8.390
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
C C .003 .002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N .006 .003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O .011 .006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H .000 .000
;International Tables for Crystallography
(1992, Vol. C, Table 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_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Pt1 N1 . 82.80(10) yes
O1 Pt1 N1 3_555 97.20(10) yes
Pt1 O1 C8 . 111.5(2) no
Pt1 N1 C1 . 128.7(3) no
Pt1 N1 C9 . 111.9(2) no
C1 N1 C9 . 119.3(4) no
N1 C1 C2 . 121.5(4) no
N1 C1 H1 . 119.4 no
C2 C1 H1 . 119.1 no
C1 C2 C3 . 120.7(4) no
C1 C2 H2 . 120.9 no
C3 C2 H2 . 118.3 no
C2 C3 C4 . 119.6(5) no
C2 C3 H3 . 121.5 no
C4 C3 H3 . 118.8 no
C3 C4 C5 . 125.2(5) no
C3 C4 C9 . 116.6(4) no
C5 C4 C9 . 118.2(4) no
C4 C5 C6 . 119.2(5) no
C4 C5 H4 . 119.3 no
C6 C5 H4 . 121.5 no
C5 C6 C7 . 122.6(4) no
C5 C6 H5 . 118.9 no
C7 C6 H5 . 118.4 no
C6 C7 C8 . 120.8(4) no
C6 C7 H6 . 119.2 no
C8 C7 H6 . 119.9 no
O1 C8 C7 . 125.0(4) no
O1 C8 C9 . 118.4(4) no
C7 C8 C9 . 116.6(4) no
N1 C9 C4 . 122.2(3) no
N1 C9 C8 . 115.3(4) no
C4 C9 C8 . 122.5(4) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Pt1 O1 2.014(3) yes
Pt1 N1 1.992(4) yes
O1 C8 1.325(6) no
N1 C1 1.322(5) no
N1 C9 1.377(6) no
C1 C2 1.401(7) no
C1 H1 .961 no
C2 C3 1.359(7) no
C2 H2 .974 no
C3 C4 1.423(6) no
C3 H3 .971 no
C4 C5 1.408(6) no
C4 C9 1.413(7) no
C5 C6 1.363(6) no
C5 H4 .977 no
C6 C7 1.407(8) no
C6 H5 .959 no
C7 C8 1.379(6) no
C7 H6 .961 no
C8 C9 1.432(5) no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
Pt1 C9 3.435(4) 1_545
Pt1 C9 3.435(4) 3_565
Pt1 C4 3.527(5) 1_545
Pt1 C4 3.527(5) 3_565
O1 C1 3.330(6) 3_565
O1 C2 3.369(5) 4_454
O1 C6 3.531(6) 1_545
O1 N1 3.537(5) 3_565
N1 C3 3.513(6) 1_545
C5 C8 3.496(7) 1_565
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Pt1 O1 C8 C7 . . . -177.9(4) no
Pt1 O1 C8 C9 . . . 2.2(5) no
Pt1 O1 C8 C7 3_555 3_555 3_555 177.9(4) no
Pt1 O1 C8 C9 3_555 3_555 3_555 -2.2(5) no
Pt1 N1 C1 C2 . . . -179.0(4) no
Pt1 N1 C9 C4 . . . 179.2(4) no
Pt1 N1 C9 C8 . . . -.9(5) no
Pt1 N1 C1 C2 3_555 3_555 3_555 179.0(4) no
Pt1 N1 C9 C4 3_555 3_555 3_555 -179.2(4) no
Pt1 N1 C9 C8 3_555 3_555 3_555 .9(5) no
O1 Pt1 N1 C1 . . . -178.1(4) no
O1 Pt1 N1 C9 . . . 1.6(3) no
O1 Pt1 N1 C1 . 3_555 3_555 -1.9(4) no
O1 Pt1 N1 C9 . 3_555 3_555 178.4(3) no
O1 C8 C7 C6 . . . -178.8(5) no
O1 C8 C9 N1 . . . -.9(6) no
O1 C8 C9 C4 . . . 179.0(4) no
N1 Pt1 O1 C8 . . . -2.1(3) no
N1 Pt1 O1 C8 . 3_555 3_555 -177.9(3) no
N1 C1 C2 C3 . . . -.6(8) no
N1 C9 C4 C3 . . . .1(7) no
N1 C9 C4 C5 . . . -179.4(4) no
N1 C9 C8 C7 . . . 179.1(4) no
C1 N1 C9 C4 . . . -1.2(7) no
C1 N1 C9 C8 . . . 178.8(4) no
C1 C2 C3 C4 . . . -.6(8) no
C2 C1 N1 C9 . . . 1.4(7) no
C2 C3 C4 C5 . . . -179.8(5) no
C2 C3 C4 C9 . . . .8(7) no
C3 C4 C5 C6 . . . -180.0(5) no
C3 C4 C9 C8 . . . -179.9(4) no
C4 C5 C6 C7 . . . .7(8) no
C4 C9 C8 C7 . . . -.9(7) no
C5 C4 C9 C8 . . . .6(7) no
C5 C6 C7 C8 . . . -1.0(8) no
C6 C5 C4 C9 . . . -.5(7) no
C6 C7 C8 C9 . . . 1.1(7) no
C6 C7 C8 C9 . . . 1.1(7) no