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#$Date: 2016-03-23 00:54:11 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179134 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/96/4309600.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_4309600
loop_
_publ_author_name
'Catelijne H. M. Amijs'
'Alexsandro Berger'
'Fouad Soulimani'
'Tom Visser'
'Gerard P. M. van Klink'
'Martin Lutz'
'Anthony L. Spek'
'Gerard van Koten'
_publ_contact_author_address
; Bijvoet Center for Biomolecular Research
  Dep. Crystal and Structural Chemistry
  Utrecht University
  Padualaan 8
  3584 CH Utrecht
  The Netherlands
;
_publ_contact_author_email       m.lutz@chem.uu.nl
_publ_contact_author_fax         '[+31] 30 2533940'
_publ_contact_author_name        'Martin Lutz'
_publ_contact_author_phone       '[+31] 30 2533902'
_publ_section_title
;
Neutral Pyridyl-Functionalized C,N-ortho-Chelated Aminoaryl Platinum(II)
Corner Building Blocks for Application in Coordination Reactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6567
_journal_page_last               6578
_journal_paper_doi               10.1021/ic050697v
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C12 H19 N3 O3 Pt'
_chemical_formula_sum            'C12 H19 N3 O3 Pt'
_chemical_formula_weight         448.39
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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            4
_cell_length_a                   10.5554(4)
_cell_length_b                   12.5362(4)
_cell_length_c                   10.8290(2)
_cell_measurement_reflns_used    224
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.12
_cell_measurement_theta_min      3.86
_cell_volume                     1432.94(8)
_computing_cell_refinement       Dirax
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'EvalCCD, ABST'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-99 (Beurskens et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11035
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    9.800
_exptl_absorpt_correction_T_max  0.55
_exptl_absorpt_correction_T_min  0.19
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.078
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.702
_refine_diff_density_min         -1.313
_refine_diff_density_rms         0.207
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.013(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         3247
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0214
_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)+(0.0259P)²+0.2339P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0443
_refine_ls_wR_factor_ref         0.0464
_reflns_number_gt                2935
_reflns_number_total             3247
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic050697vsi20050504_091400_3.cif
_cod_data_source_block           s3363a
_cod_database_code               4309600
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'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
Pt1 Pt 0.079298(11) 0.180629(9) 0.49571(3) 0.01620(5) Uani 1 1 d . . .
O1 O 0.0668(3) 0.0083(3) 0.4714(3) 0.0263(10) Uani 1 1 d . . .
O2 O 0.1897(4) -0.0101(3) 0.6305(4) 0.0457(11) Uani 1 1 d . . .
O3 O 0.1388(4) -0.1478(3) 0.5215(4) 0.0407(12) Uani 1 1 d . . .
N1 N -0.0193(4) 0.2043(3) 0.6607(3) 0.0174(8) Uani 1 1 d . . .
N2 N 0.1821(4) 0.2037(3) 0.3333(3) 0.0208(8) Uani 1 1 d . . .
N3 N 0.1338(4) -0.0513(3) 0.5436(4) 0.0246(8) Uani 1 1 d . . .
C1 C 0.0820(3) 0.3340(3) 0.4972(14) 0.0178(7) Uani 1 1 d . . .
C2 C 0.0024(4) 0.3871(3) 0.5797(4) 0.0199(9) Uani 1 1 d . . .
C3 C 0.0040(5) 0.4984(4) 0.5797(5) 0.0255(10) Uani 1 1 d . . .
H3 H -0.0494 0.5374 0.6340 0.031 Uiso 1 1 calc R . .
C4 C 0.0846(4) 0.5509(3) 0.4994(12) 0.0293(9) Uani 1 1 d . . .
H4 H 0.0860 0.6267 0.5000 0.035 Uiso 1 1 calc R . .
C5 C 0.1637(5) 0.4966(4) 0.4176(4) 0.0295(11) Uani 1 1 d . . .
H5 H 0.2176 0.5350 0.3631 0.035 Uiso 1 1 calc R . .
C6 C 0.1629(4) 0.3858(4) 0.4165(4) 0.0208(9) Uani 1 1 d . . .
C7 C -0.0832(4) 0.3133(3) 0.6514(5) 0.0220(10) Uani 1 1 d . . .
H7A H -0.1658 0.3065 0.6089 0.026 Uiso 1 1 calc R . .
H7B H -0.0984 0.3425 0.7351 0.026 Uiso 1 1 calc R . .
C8 C 0.0714(6) 0.2070(7) 0.7659(8) 0.0258(17) Uani 1 1 d . . .
H8A H 0.0244 0.2137 0.8435 0.039 Uiso 1 1 calc R . .
H8B H 0.1284 0.2682 0.7564 0.039 Uiso 1 1 calc R . .
H8C H 0.1211 0.1410 0.7669 0.039 Uiso 1 1 calc R . .
C9 C -0.1176(5) 0.1226(4) 0.6865(5) 0.0249(10) Uani 1 1 d . . .
H9A H -0.0777 0.0523 0.6930 0.037 Uiso 1 1 calc R . .
H9B H -0.1797 0.1220 0.6192 0.037 Uiso 1 1 calc R . .
H9C H -0.1604 0.1397 0.7643 0.037 Uiso 1 1 calc R . .
C10 C 0.2467(5) 0.3120(3) 0.3435(4) 0.0248(10) Uani 1 1 d . . .
H10A H 0.3296 0.3042 0.3852 0.030 Uiso 1 1 calc R . .
H10B H 0.2615 0.3418 0.2600 0.030 Uiso 1 1 calc R . .
C11 C 0.0939(6) 0.2038(7) 0.2280(9) 0.0280(18) Uani 1 1 d . . .
H11A H 0.1415 0.2143 0.1513 0.042 Uiso 1 1 calc R . .
H11B H 0.0325 0.2617 0.2381 0.042 Uiso 1 1 calc R . .
H11C H 0.0491 0.1353 0.2247 0.042 Uiso 1 1 calc R . .
C12 C 0.2808(4) 0.1205(4) 0.3107(4) 0.0269(10) Uani 1 1 d . . .
H12A H 0.2412 0.0498 0.3109 0.040 Uiso 1 1 calc R . .
H12B H 0.3449 0.1240 0.3760 0.040 Uiso 1 1 calc R . .
H12C H 0.3210 0.1333 0.2305 0.040 Uiso 1 1 calc R . .
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'
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
C1 Pt1 N2 82.0(4) . . ?
C1 Pt1 N1 81.9(4) . . ?
N2 Pt1 N1 163.82(14) . . ?
C1 Pt1 O1 173.0(4) . . ?
N2 Pt1 O1 93.84(13) . . ?
N1 Pt1 O1 102.33(13) . . ?
N3 O1 Pt1 117.9(3) . . ?
C9 N1 C8 108.8(4) . . ?
C9 N1 C7 108.7(3) . . ?
C8 N1 C7 108.3(5) . . ?
C9 N1 Pt1 114.3(3) . . ?
C8 N1 Pt1 109.7(4) . . ?
C7 N1 Pt1 106.9(3) . . ?
C11 N2 C12 108.4(4) . . ?
C11 N2 C10 109.8(5) . . ?
C12 N2 C10 108.7(4) . . ?
C11 N2 Pt1 108.9(4) . . ?
C12 N2 Pt1 113.8(3) . . ?
C10 N2 Pt1 107.2(3) . . ?
O2 N3 O3 122.8(4) . . ?
O2 N3 O1 118.9(4) . . ?
O3 N3 O1 118.3(4) . . ?
C6 C1 C2 123.5(3) . . ?
C6 C1 Pt1 118.2(6) . . ?
C2 C1 Pt1 118.3(6) . . ?
C3 C2 C1 118.0(5) . . ?
C3 C2 C7 128.3(4) . . ?
C1 C2 C7 113.4(4) . . ?
C4 C3 C2 118.9(5) . . ?
C4 C3 H3 120.6 . . ?
C2 C3 H3 120.6 . . ?
C3 C4 C5 122.4(4) . . ?
C3 C4 H4 118.8 . . ?
C5 C4 H4 118.8 . . ?
C6 C5 C4 119.3(5) . . ?
C6 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?
C1 C6 C5 117.9(5) . . ?
C1 C6 C10 114.0(4) . . ?
C5 C6 C10 128.0(4) . . ?
C2 C7 N1 108.6(3) . . ?
C2 C7 H7A 110.0 . . ?
N1 C7 H7A 110.0 . . ?
C2 C7 H7B 110.0 . . ?
N1 C7 H7B 110.0 . . ?
H7A C7 H7B 108.4 . . ?
N1 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C10 N2 108.9(4) . . ?
C6 C10 H10A 109.9 . . ?
N2 C10 H10A 109.9 . . ?
C6 C10 H10B 109.9 . . ?
N2 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 H12A 109.5 . . ?
N2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
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 C1 1.923(3) . ?
Pt1 N2 2.087(4) . ?
Pt1 N1 2.089(4) . ?
Pt1 O1 2.180(3) . ?
O1 N3 1.292(5) . ?
O2 N3 1.226(5) . ?
O3 N3 1.234(5) . ?
N1 C9 1.484(6) . ?
N1 C8 1.488(8) . ?
N1 C7 1.528(5) . ?
N2 C11 1.471(9) . ?
N2 C12 1.494(6) . ?
N2 C10 1.524(5) . ?
C1 C6 1.384(11) . ?
C1 C2 1.396(11) . ?
C2 C3 1.395(6) . ?
C2 C7 1.508(6) . ?
C3 C4 1.383(11) . ?
C3 H3 0.9500 . ?
C4 C5 1.395(10) . ?
C4 H4 0.9500 . ?
C5 C6 1.389(7) . ?
C5 H5 0.9500 . ?
C6 C10 1.504(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Pt1 O1 N3 108.1(3) . . . . ?
N1 Pt1 O1 N3 -72.3(3) . . . . ?
C1 Pt1 N1 C9 147.0(4) . . . . ?
N2 Pt1 N1 C9 151.1(5) . . . . ?
O1 Pt1 N1 C9 -27.4(3) . . . . ?
C1 Pt1 N1 C8 -90.5(5) . . . . ?
N2 Pt1 N1 C8 -86.4(7) . . . . ?
O1 Pt1 N1 C8 95.1(4) . . . . ?
C1 Pt1 N1 C7 26.7(3) . . . . ?
N2 Pt1 N1 C7 30.8(6) . . . . ?
O1 Pt1 N1 C7 -147.7(2) . . . . ?
C1 Pt1 N2 C11 -93.7(5) . . . . ?
N1 Pt1 N2 C11 -97.9(7) . . . . ?
O1 Pt1 N2 C11 80.7(4) . . . . ?
C1 Pt1 N2 C12 145.3(4) . . . . ?
N1 Pt1 N2 C12 141.1(5) . . . . ?
O1 Pt1 N2 C12 -40.3(3) . . . . ?
C1 Pt1 N2 C10 25.0(3) . . . . ?
N1 Pt1 N2 C10 20.9(6) . . . . ?
O1 Pt1 N2 C10 -160.6(3) . . . . ?
Pt1 O1 N3 O2 8.0(5) . . . . ?
Pt1 O1 N3 O3 -171.8(3) . . . . ?
N2 Pt1 C1 C6 -12.4(7) . . . . ?
N1 Pt1 C1 C6 166.5(7) . . . . ?
N2 Pt1 C1 C2 167.8(7) . . . . ?
N1 Pt1 C1 C2 -13.4(7) . . . . ?
C6 C1 C2 C3 0.7(12) . . . . ?
Pt1 C1 C2 C3 -179.5(5) . . . . ?
C6 C1 C2 C7 176.0(7) . . . . ?
Pt1 C1 C2 C7 -4.2(9) . . . . ?
C1 C2 C3 C4 -0.6(9) . . . . ?
C7 C2 C3 C4 -175.1(6) . . . . ?
C2 C3 C4 C5 0.5(11) . . . . ?
C3 C4 C5 C6 -0.4(11) . . . . ?
C2 C1 C6 C5 -0.6(11) . . . . ?
Pt1 C1 C6 C5 179.6(5) . . . . ?
C2 C1 C6 C10 175.5(7) . . . . ?
Pt1 C1 C6 C10 -4.3(9) . . . . ?
C4 C5 C6 C1 0.5(9) . . . . ?
C4 C5 C6 C10 -175.0(6) . . . . ?
C3 C2 C7 N1 -158.6(5) . . . . ?
C1 C2 C7 N1 26.7(7) . . . . ?
C9 N1 C7 C2 -158.7(4) . . . . ?
C8 N1 C7 C2 83.3(5) . . . . ?
Pt1 N1 C7 C2 -34.9(4) . . . . ?
C1 C6 C10 N2 25.6(7) . . . . ?
C5 C6 C10 N2 -158.8(4) . . . . ?
C11 N2 C10 C6 85.2(5) . . . . ?
C12 N2 C10 C6 -156.4(4) . . . . ?
Pt1 N2 C10 C6 -32.9(4) . . . . ?
