#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:16:34 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180131 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/29/7102930.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_7102930
loop_
_publ_author_name
'Reithofer, Michael R'
'Galanski, Markus'
'Arion, Vladimir B'
'Keppler, Bernhard K'
_publ_section_title
;
 Unprecedented twofold intramolecular hydroamination in
 diam(m)ine-dicarboxylatodichloridoplatinum(IV) complexes -
 ethane-1,2-diamine vs. ammine ligands.
;
_journal_issue                   9
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1091
_journal_page_last               1093
_journal_paper_doi               10.1039/b715680d
_journal_year                    2008
_chemical_formula_sum            'C14 H26.25 Cl2 N4 O6.13 Pt'
_chemical_formula_weight         614.63
_chemical_name_common
;
(OC-6-54)-Amminedichlorido(2R,2S-imino-kappaN-nis((4-
propylamino)-4-oxobutanoato-2-yl)-kappa$2!O,O')platinum(IV)
;
_chemical_name_systematic
;
(OC-6-54)-Amminedichlorido(2R,2S-imino-kappaN-nis[(4-propylamino)-
4-oxobutanoato-2-yl]-kappa²O,O')platinum(IV)
;
_space_group_IT_number           45
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 -2c'
_symmetry_space_group_name_H-M   'I b a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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            8
_cell_length_a                   22.1412(9)
_cell_length_b                   22.6423(8)
_cell_length_c                   8.5427(3)
_cell_measurement_reflns_used    2282
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.01
_cell_measurement_theta_min      2.90
_cell_volume                     4282.7(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0826
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            61325
_diffrn_reflns_theta_full        28.39
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    6.839
_exptl_absorpt_correction_T_max  0.8753
_exptl_absorpt_correction_T_min  0.1921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    1.906
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2394
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.077
_refine_diff_density_min         -1.770
_refine_diff_density_rms         0.181
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         5339
_refine_ls_number_restraints     213
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0369
_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)+(0.0450P)²+26.6516P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0926
_reflns_number_gt                4259
_reflns_number_total             5339
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b715680d.txt
_cod_data_source_block           MIRE104
_cod_original_sg_symbol_H-M      Iba2
_cod_database_code               7102930
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1, -y+1, z+1/2'
'-x+1, y+1, 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_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 0.845150(10) 0.677872(10) 0.30872(5) 0.01788(8) Uani 1 1 d U . .
Cl1 Cl 0.92836(9) 0.62160(10) 0.2391(3) 0.0293(4) Uani 1 1 d U . .
Cl2 Cl 0.82290(11) 0.69388(11) 0.0495(2) 0.0317(5) Uani 1 1 d U . .
O1 O 0.8974(2) 0.7491(2) 0.3272(11) 0.0271(14) Uani 1 1 d U . .
O2 O 0.9674(3) 0.7853(3) 0.4886(8) 0.0438(18) Uani 1 1 d U . .
O3 O 0.8410(2) 0.7707(3) 0.7076(7) 0.0242(12) Uani 1 1 d U . .
O4 O 0.7955(2) 0.6046(2) 0.3249(11) 0.0323(13) Uani 1 1 d U . .
O5 O 0.7882(5) 0.5249(3) 0.4724(9) 0.066(3) Uani 1 1 d U . .
O6 O 0.7552(3) 0.6613(2) 0.7021(7) 0.0228(12) Uani 1 1 d U . .
N1 N 0.7721(3) 0.7274(3) 0.3643(7) 0.0233(14) Uani 1 1 d U . .
H1A H 0.7707 0.7328 0.4698 0.035 Uiso 1 1 calc R . .
H1B H 0.7380 0.7085 0.3322 0.035 Uiso 1 1 calc R . .
H1C H 0.7747 0.7631 0.3158 0.035 Uiso 1 1 calc R . .
N2 N 0.8627(3) 0.6654(3) 0.5398(8) 0.0178(12) Uani 1 1 d U . .
H2 H 0.8341 0.6863 0.5971 0.021 Uiso 1 1 calc R . .
N3 N 0.9107(3) 0.8019(4) 0.8847(9) 0.0331(17) Uani 1 1 d U . .
H3 H 0.9483 0.7985 0.9161 0.040 Uiso 1 1 calc R . .
N4 N 0.7348(4) 0.5867(4) 0.8678(9) 0.042(2) Uani 1 1 d U . .
H4 H 0.7437 0.5501 0.8939 0.050 Uiso 1 1 calc R . .
C1 C 0.9309(4) 0.7468(4) 0.4539(10) 0.0282(17) Uani 1 1 d U . .
C2 C 0.9229(3) 0.6932(4) 0.5680(10) 0.0263(16) Uani 1 1 d U . .
H2A H 0.9549 0.6634 0.5435 0.032 Uiso 1 1 calc R . .
C3 C 0.9331(4) 0.7153(4) 0.7323(11) 0.0312(19) Uani 1 1 d U . .
H3A H 0.9754 0.7287 0.7425 0.037 Uiso 1 1 calc R . .
H3B H 0.9270 0.6822 0.8065 0.037 Uiso 1 1 calc R . .
C4 C 0.8916(3) 0.7654(4) 0.7767(10) 0.030(2) Uani 1 1 d U . .
C5 C 0.8742(4) 0.8475(5) 0.9559(12) 0.038(2) Uani 1 1 d U . .
H5A H 0.8421 0.8292 1.0204 0.045 Uiso 1 1 calc R . .
H5B H 0.8546 0.8715 0.8734 0.045 Uiso 1 1 calc R . .
C6 C 0.9132(6) 0.8866(6) 1.0572(18) 0.069(4) Uani 1 1 d U . .
H6A H 0.8869 0.9146 1.1142 0.083 Uiso 1 1 calc R . .
H6B H 0.9339 0.8617 1.1361 0.083 Uiso 1 1 calc R . .
C7 C 0.9590(6) 0.9204(6) 0.971(2) 0.089(5) Uani 1 1 d U . .
H7A H 0.9829 0.9440 1.0447 0.133 Uiso 1 1 calc R . .
H7B H 0.9391 0.9467 0.8960 0.133 Uiso 1 1 calc R . .
H7C H 0.9857 0.8932 0.9146 0.133 Uiso 1 1 calc R . .
C8 C 0.8105(5) 0.5744(4) 0.4494(12) 0.039(2) Uani 1 1 d U . .
C9 C 0.8527(4) 0.5997(4) 0.5688(11) 0.0312(18) Uani 1 1 d U . .
H9 H 0.8925 0.5793 0.5568 0.037 Uiso 1 1 calc R . .
C10 C 0.8305(4) 0.5889(4) 0.7365(11) 0.0324(18) Uani 1 1 d U . .
H10A H 0.8293 0.5459 0.7566 0.039 Uiso 1 1 calc R . .
H10B H 0.8597 0.6067 0.8108 0.039 Uiso 1 1 calc R . .
C11 C 0.7697(4) 0.6142(4) 0.7662(8) 0.0255(17) Uani 1 1 d U . .
C12 C 0.6817(5) 0.6146(5) 0.9391(13) 0.049(3) Uani 1 1 d U . .
H12A H 0.6606 0.6377 0.8574 0.058 Uiso 1 1 calc R . .
H12B H 0.6959 0.6429 1.0196 0.058 Uiso 1 1 calc R . .
C13 C 0.6367(7) 0.5736(6) 1.0142(15) 0.064(3) Uani 1 1 d U . .
H13A H 0.6038 0.5973 1.0616 0.077 Uiso 1 1 calc R . .
H13B H 0.6186 0.5482 0.9324 0.077 Uiso 1 1 calc R . .
C14 C 0.6633(7) 0.5367(7) 1.1331(16) 0.081(5) Uani 1 1 d U . .
H14A H 0.6322 0.5109 1.1777 0.121 Uiso 1 1 calc R . .
H14B H 0.6804 0.5616 1.2159 0.121 Uiso 1 1 calc R . .
H14C H 0.6953 0.5126 1.0865 0.121 Uiso 1 1 calc R . .
O7 O 1.0000(7) 0.5000(7) 0.5557(16) 0.042(8) Uani 0.25 2 d SPR . .
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'
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
O1 Pt1 O4 171.2(4) . . ?
O1 Pt1 N1 89.8(3) . . ?
O4 Pt1 N1 90.2(3) . . ?
O1 Pt1 N2 85.7(3) . . ?
O4 Pt1 N2 85.6(3) . . ?
N1 Pt1 N2 90.1(3) . . ?
O1 Pt1 Cl2 94.2(3) . . ?
O4 Pt1 Cl2 94.6(3) . . ?
N1 Pt1 Cl2 88.13(19) . . ?
N2 Pt1 Cl2 178.25(19) . . ?
O1 Pt1 Cl1 90.23(15) . . ?
O4 Pt1 Cl1 89.93(17) . . ?
N1 Pt1 Cl1 178.69(19) . . ?
N2 Pt1 Cl1 91.18(18) . . ?
Cl2 Pt1 Cl1 90.57(8) . . ?
C1 O1 Pt1 111.2(6) . . ?
C8 O4 Pt1 110.6(6) . . ?
C2 N2 C9 121.0(7) . . ?
C2 N2 Pt1 105.6(5) . . ?
C9 N2 Pt1 105.4(5) . . ?
C4 N3 C5 124.6(8) . . ?
C11 N4 C12 122.7(8) . . ?
O2 C1 O1 123.0(9) . . ?
O2 C1 C2 118.3(8) . . ?
O1 C1 C2 118.7(7) . . ?
N2 C2 C3 115.0(7) . . ?
N2 C2 C1 109.0(6) . . ?
C3 C2 C1 107.8(7) . . ?
C2 C3 C4 113.2(7) . . ?
O3 C4 N3 123.5(8) . . ?
O3 C4 C3 119.4(7) . . ?
N3 C4 C3 117.2(7) . . ?
N3 C5 C6 109.9(8) . . ?
C7 C6 C5 114.4(13) . . ?
O5 C8 O4 120.1(10) . . ?
O5 C8 C9 119.1(10) . . ?
O4 C8 C9 120.8(8) . . ?
C8 C9 N2 110.7(7) . . ?
C8 C9 C10 112.1(8) . . ?
N2 C9 C10 110.6(7) . . ?
C11 C10 C9 112.9(7) . . ?
O6 C11 N4 123.0(8) . . ?
O6 C11 C10 119.4(8) . . ?
N4 C11 C10 117.5(8) . . ?
N4 C12 C13 116.2(10) . . ?
C14 C13 C12 112.8(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 O1 1.991(5) . ?
Pt1 O4 1.995(5) . ?
Pt1 N1 2.025(6) . ?
Pt1 N2 2.032(7) . ?
Pt1 Cl2 2.298(2) . ?
Pt1 Cl1 2.3177(19) . ?
O1 C1 1.313(12) . ?
O2 C1 1.225(10) . ?
O3 C4 1.273(9) . ?
O4 C8 1.308(13) . ?
O5 C8 1.239(11) . ?
O6 C11 1.240(9) . ?
N2 C2 1.494(10) . ?
N2 C9 1.526(10) . ?
N3 C4 1.309(10) . ?
N3 C5 1.445(11) . ?
N4 C11 1.319(10) . ?
N4 C12 1.467(13) . ?
C1 C2 1.567(13) . ?
C2 C3 1.507(12) . ?
C3 C4 1.507(12) . ?
C5 C6 1.511(15) . ?
C6 C7 1.47(2) . ?
C8 C9 1.497(14) . ?
C9 C10 1.534(13) . ?
C10 C11 1.485(12) . ?
C12 C13 1.506(15) . ?
C13 C14 1.441(19) . ?
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
N1 Pt1 O1 C1 107.5(5) . . . . ?
N2 Pt1 O1 C1 17.4(5) . . . . ?
Cl2 Pt1 O1 C1 -164.3(5) . . . . ?
Cl1 Pt1 O1 C1 -73.8(5) . . . . ?
N1 Pt1 O4 C8 -108.8(6) . . . . ?
N2 Pt1 O4 C8 -18.6(6) . . . . ?
Cl2 Pt1 O4 C8 163.1(6) . . . . ?
Cl1 Pt1 O4 C8 72.5(6) . . . . ?
O1 Pt1 N2 C2 -27.5(5) . . . . ?
O4 Pt1 N2 C2 152.5(5) . . . . ?
N1 Pt1 N2 C2 -117.3(5) . . . . ?
Cl1 Pt1 N2 C2 62.7(4) . . . . ?
O1 Pt1 N2 C9 -156.7(5) . . . . ?
O4 Pt1 N2 C9 23.3(5) . . . . ?
N1 Pt1 N2 C9 113.5(5) . . . . ?
Cl1 Pt1 N2 C9 -66.5(5) . . . . ?
Pt1 O1 C1 O2 178.7(6) . . . . ?
Pt1 O1 C1 C2 -2.6(8) . . . . ?
C9 N2 C2 C3 -88.3(9) . . . . ?
Pt1 N2 C2 C3 152.4(6) . . . . ?
C9 N2 C2 C1 150.6(7) . . . . ?
Pt1 N2 C2 C1 31.3(7) . . . . ?
O2 C1 C2 N2 158.3(7) . . . . ?
O1 C1 C2 N2 -20.5(10) . . . . ?
O2 C1 C2 C3 32.8(10) . . . . ?
O1 C1 C2 C3 -145.9(7) . . . . ?
N2 C2 C3 C4 -64.9(10) . . . . ?
C1 C2 C3 C4 56.9(9) . . . . ?
C5 N3 C4 O3 9.4(15) . . . . ?
C5 N3 C4 C3 -171.6(9) . . . . ?
C2 C3 C4 O3 25.2(12) . . . . ?
C2 C3 C4 N3 -153.9(8) . . . . ?
C4 N3 C5 C6 -171.7(11) . . . . ?
N3 C5 C6 C7 64.7(14) . . . . ?
Pt1 O4 C8 O5 -173.9(8) . . . . ?
Pt1 O4 C8 C9 8.5(11) . . . . ?
O5 C8 C9 N2 -166.1(9) . . . . ?
O4 C8 C9 N2 11.5(12) . . . . ?
O5 C8 C9 C10 -42.0(12) . . . . ?
O4 C8 C9 C10 135.6(9) . . . . ?
C2 N2 C9 C8 -143.7(8) . . . . ?
Pt1 N2 C9 C8 -24.2(8) . . . . ?
C2 N2 C9 C10 91.4(9) . . . . ?
Pt1 N2 C9 C10 -149.2(6) . . . . ?
C8 C9 C10 C11 -58.3(10) . . . . ?
N2 C9 C10 C11 65.8(10) . . . . ?
C12 N4 C11 O6 -13.1(13) . . . . ?
C12 N4 C11 C10 163.0(9) . . . . ?
C9 C10 C11 O6 -35.2(12) . . . . ?
C9 C10 C11 N4 148.6(8) . . . . ?
C11 N4 C12 C13 162.8(10) . . . . ?
N4 C12 C13 C14 56.6(15) . . . . ?
