#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/54/4335475.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_4335475
loop_
_publ_author_name
'Verena Pichler'
'Simone Göschl'
'Samuel M. Meier'
'Alexander Roller'
'Michael A. Jakupec'
'Markus Galanski'
'Bernhard K. Keppler'
_publ_section_title
;
 Bulky N(,N)-(Di)alkylethane-1,2-diamineplatinum(II) Compounds as
 Precursors for Generating Unsymmetrically Substituted Platinum(IV)
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8151
_journal_page_last               8162
_journal_paper_doi               10.1021/ic400816g
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C22 H26 Cl2 N2 O4 Pt'
_chemical_formula_sum            'C22 H26 Cl2 N2 O4 Pt'
_chemical_formula_weight         648.44
_chemical_name_systematic
; 
(OC-6-54)-Dichlorido(N,N-dimethylethane-1,2-diamine)hydroxido[(2E)-3-
phenylprop-2-enoato]platinum(IV) 
;
_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                65.149(4)
_cell_angle_beta                 72.991(4)
_cell_angle_gamma                85.489(4)
_cell_formula_units_Z            2
_cell_length_a                   7.8654(6)
_cell_length_b                   12.8074(11)
_cell_length_c                   13.3055(12)
_cell_measurement_reflns_used    3424
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.86
_cell_measurement_theta_min      2.71
_cell_volume                     1161.51(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0942
_diffrn_reflns_av_sigmaI/netI    0.0761
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25532
_diffrn_reflns_theta_full        25.30
_diffrn_reflns_theta_max         25.30
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    6.301
_exptl_absorpt_correction_T_max  0.8335
_exptl_absorpt_correction_T_min  0.5714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.854
_exptl_crystal_description       plate
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.364
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4133
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0321P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0716
_reflns_number_gt                3323
_reflns_number_total             4133
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400816g_si_002.cif
_cod_data_source_block           vepi219
_cod_original_cell_volume        1161.51(17)
_cod_original_sg_symbol_Hall     P-1
_cod_database_code               4335475
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
Pt1 Pt 0.12194(3) 0.23722(2) 0.24129(2) 0.01970(10) Uani 1 1 d .
Cl1 Cl 0.3635(2) 0.35782(14) 0.19312(13) 0.0266(4) Uani 1 1 d .
Cl2 Cl 0.2863(2) 0.07320(14) 0.30029(13) 0.0290(4) Uani 1 1 d .
O1 O 0.2045(5) 0.2348(4) 0.0838(3) 0.0258(11) Uani 1 1 d .
O2 O 0.1466(7) 0.4154(4) -0.0295(4) 0.0359(12) Uani 1 1 d .
O3 O 0.0445(6) 0.2162(4) 0.4078(3) 0.0253(11) Uani 1 1 d .
O4 O -0.0067(6) 0.4009(4) 0.3846(4) 0.0332(12) Uani 1 1 d .
N1 N -0.0270(6) 0.3779(4) 0.1938(4) 0.0237(13) Uani 1 1 d .
H1A H -0.0125 0.4252 0.2273 0.028 Uiso 1 1 calc R
H1B H 0.0094 0.4189 0.1148 0.028 Uiso 1 1 calc R
N2 N -0.1124(7) 0.1414(4) 0.2749(4) 0.0238(13) Uani 1 1 d .
C1 C 0.2007(8) 0.3201(6) -0.0150(5) 0.0239(16) Uani 1 1 d .
C2 C 0.2693(9) 0.2831(6) -0.1115(6) 0.0301(17) Uani 1 1 d .
H2 H 0.3170 0.2092 -0.0947 0.036 Uiso 1 1 calc R
C3 C 0.2671(9) 0.3476(6) -0.2187(6) 0.0315(17) Uani 1 1 d .
H3 H 0.2227 0.4221 -0.2332 0.038 Uiso 1 1 calc R
C4 C 0.3260(9) 0.3174(6) -0.3193(5) 0.0264(16) Uani 1 1 d .
C5 C 0.3146(9) 0.3973(6) -0.4262(6) 0.0303(17) Uani 1 1 d .
H5 H 0.2769 0.4722 -0.4351 0.036 Uiso 1 1 calc R
C6 C 0.3575(9) 0.3696(6) -0.5210(6) 0.0346(18) Uani 1 1 d .
H6 H 0.3478 0.4246 -0.5938 0.041 Uiso 1 1 calc R
C7 C 0.4146(9) 0.2607(7) -0.5078(6) 0.0336(18) Uani 1 1 d .
H7 H 0.4394 0.2397 -0.5710 0.040 Uiso 1 1 calc R
C8 C 0.4354(9) 0.1831(6) -0.4039(6) 0.0338(18) Uani 1 1 d .
H8 H 0.4795 0.1098 -0.3963 0.041 Uiso 1 1 calc R
C9 C 0.3923(9) 0.2110(6) -0.3098(6) 0.0335(18) Uani 1 1 d .
H9 H 0.4083 0.1570 -0.2383 0.040 Uiso 1 1 calc R
C10 C -0.0112(9) 0.2967(6) 0.4454(5) 0.0254(16) Uani 1 1 d .
C11 C -0.0855(8) 0.2464(6) 0.5739(5) 0.0265(16) Uani 1 1 d .
H11 H -0.1034 0.1651 0.6150 0.032 Uiso 1 1 calc R
C12 C -0.1274(8) 0.3110(6) 0.6327(5) 0.0269(16) Uani 1 1 d .
H12 H -0.1055 0.3918 0.5890 0.032 Uiso 1 1 calc R
C13 C -0.2040(9) 0.2709(6) 0.7583(5) 0.0276(16) Uani 1 1 d .
C14 C -0.2388(8) 0.3516(6) 0.8065(5) 0.0282(16) Uani 1 1 d .
H14 H -0.2084 0.4309 0.7577 0.034 Uiso 1 1 calc R
C15 C -0.3164(9) 0.3181(7) 0.9235(6) 0.0343(18) Uani 1 1 d .
H15 H -0.3378 0.3742 0.9545 0.041 Uiso 1 1 calc R
C16 C -0.3628(9) 0.2041(6) 0.9954(6) 0.0292(17) Uani 1 1 d .
H16 H -0.4198 0.1816 1.0755 0.035 Uiso 1 1 calc R
C17 C -0.3262(9) 0.1215(6) 0.9508(6) 0.0337(18) Uani 1 1 d .
H17 H -0.3508 0.0420 1.0011 0.040 Uiso 1 1 calc R
C18 C -0.2537(9) 0.1554(6) 0.8329(5) 0.0327(18) Uani 1 1 d .
H18 H -0.2374 0.0992 0.8022 0.039 Uiso 1 1 calc R
C19 C -0.2137(9) 0.3392(6) 0.2316(7) 0.041(2) Uani 1 1 d .
H19A H -0.2664 0.3257 0.3136 0.050 Uiso 1 1 calc R
H19B H -0.2801 0.3996 0.1849 0.050 Uiso 1 1 calc R
C20 C -0.2293(9) 0.2343(7) 0.2189(7) 0.046(2) Uani 1 1 d .
H20A H -0.1971 0.2518 0.1355 0.056 Uiso 1 1 calc R
H20B H -0.3550 0.2044 0.2537 0.056 Uiso 1 1 calc R
C21 C -0.2009(11) 0.0747(7) 0.3997(6) 0.047(2) Uani 1 1 d .
H21A H -0.2221 0.1262 0.4392 0.070 Uiso 1 1 calc R
H21B H -0.1243 0.0137 0.4330 0.070 Uiso 1 1 calc R
H21C H -0.3147 0.0402 0.4095 0.070 Uiso 1 1 calc R
C22 C -0.0836(10) 0.0619(6) 0.2178(6) 0.040(2) Uani 1 1 d .
H22A H -0.0248 0.1044 0.1351 0.061 Uiso 1 1 calc R
H22B H -0.1986 0.0282 0.2284 0.061 Uiso 1 1 calc R
H22C H -0.0085 0.0005 0.2521 0.061 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'
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'
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
O3 Pt1 O1 172.13(17)
O3 Pt1 N1 91.82(18)
O1 Pt1 N1 95.25(18)
O3 Pt1 N2 89.01(17)
O1 Pt1 N2 88.19(18)
N1 Pt1 N2 85.1(2)
O3 Pt1 Cl1 93.08(12)
O1 Pt1 Cl1 90.44(13)
N1 Pt1 Cl1 89.25(14)
N2 Pt1 Cl1 174.04(15)
O3 Pt1 Cl2 87.04(13)
O1 Pt1 Cl2 85.81(13)
N1 Pt1 Cl2 178.43(14)
N2 Pt1 Cl2 93.79(15)
Cl1 Pt1 Cl2 91.90(6)
C1 O1 Pt1 126.5(4)
C10 O3 Pt1 126.5(4)
C19 N1 Pt1 108.8(4)
C19 N1 H1A 109.9
Pt1 N1 H1A 109.9
C19 N1 H1B 109.9
Pt1 N1 H1B 109.9
H1A N1 H1B 108.3
C22 N2 C21 108.2(5)
C22 N2 C20 107.2(5)
C21 N2 C20 111.2(6)
C22 N2 Pt1 113.7(4)
C21 N2 Pt1 113.6(4)
C20 N2 Pt1 102.7(4)
O2 C1 O1 127.0(6)
O2 C1 C2 122.8(6)
O1 C1 C2 110.2(6)
C3 C2 C1 123.5(7)
C3 C2 H2 118.2
C1 C2 H2 118.2
C2 C3 C4 127.6(7)
C2 C3 H3 116.2
C4 C3 H3 116.2
C5 C4 C9 118.6(6)
C5 C4 C3 119.4(6)
C9 C4 C3 122.1(6)
C4 C5 C6 121.1(6)
C4 C5 H5 119.5
C6 C5 H5 119.5
C7 C6 C5 119.1(6)
C7 C6 H6 120.4
C5 C6 H6 120.4
C8 C7 C6 120.2(6)
C8 C7 H7 119.9
C6 C7 H7 119.9
C7 C8 C9 120.3(7)
C7 C8 H8 119.8
C9 C8 H8 119.8
C8 C9 C4 120.5(7)
C8 C9 H9 119.8
C4 C9 H9 119.8
O4 C10 O3 125.8(6)
O4 C10 C11 122.7(6)
O3 C10 C11 111.5(6)
C12 C11 C10 122.4(6)
C12 C11 H11 118.8
C10 C11 H11 118.8
C11 C12 C13 126.9(6)
C11 C12 H12 116.5
C13 C12 H12 116.5
C14 C13 C18 117.5(6)
C14 C13 C12 119.3(6)
C18 C13 C12 123.1(6)
C15 C14 C13 121.2(6)
C15 C14 H14 119.4
C13 C14 H14 119.4
C14 C15 C16 120.3(6)
C14 C15 H15 119.9
C16 C15 H15 119.9
C15 C16 C17 119.9(6)
C15 C16 H16 120.0
C17 C16 H16 120.0
C18 C17 C16 119.8(7)
C18 C17 H17 120.1
C16 C17 H17 120.1
C17 C18 C13 121.1(7)
C17 C18 H18 119.4
C13 C18 H18 119.4
C20 C19 N1 110.2(6)
C20 C19 H19A 109.6
N1 C19 H19A 109.6
C20 C19 H19B 109.6
N1 C19 H19B 109.6
H19A C19 H19B 108.1
C19 C20 N2 113.3(6)
C19 C20 H20A 108.9
N2 C20 H20A 108.9
C19 C20 H20B 108.9
N2 C20 H20B 108.9
H20A C20 H20B 107.7
N2 C21 H21A 109.5
N2 C21 H21B 109.5
H21A C21 H21B 109.5
N2 C21 H21C 109.5
H21A C21 H21C 109.5
H21B C21 H21C 109.5
N2 C22 H22A 109.5
N2 C22 H22B 109.5
H22A C22 H22B 109.5
N2 C22 H22C 109.5
H22A C22 H22C 109.5
H22B C22 H22C 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pt1 O3 2.021(4)
Pt1 O1 2.018(4)
Pt1 N1 2.040(5)
Pt1 N2 2.124(5)
Pt1 Cl1 2.3072(16)
Pt1 Cl2 2.3413(16)
O1 C1 1.316(7)
O2 C1 1.216(7)
O3 C10 1.319(7)
O4 C10 1.232(7)
N1 C19 1.459(8)
N1 H1A 0.9200
N1 H1B 0.9200
N2 C22 1.476(8)
N2 C21 1.482(8)
N2 C20 1.516(9)
C1 C2 1.492(9)
C2 C3 1.319(9)
C2 H2 0.9500
C3 C4 1.483(9)
C3 H3 0.9500
C4 C5 1.384(9)
C4 C9 1.388(9)
C5 C6 1.392(9)
C5 H5 0.9500
C6 C7 1.385(9)
C6 H6 0.9500
C7 C8 1.370(9)
C7 H7 0.9500
C8 C9 1.385(9)
C8 H8 0.9500
C9 H9 0.9500
C10 C11 1.494(8)
C11 C12 1.324(8)
C11 H11 0.9500
C12 C13 1.469(8)
C12 H12 0.9500
C13 C14 1.403(9)
C13 C18 1.399(9)
C14 C15 1.380(9)
C14 H14 0.9500
C15 C16 1.374(9)
C15 H15 0.9500
C16 C17 1.391(9)
C16 H16 0.9500
C17 C18 1.385(9)
C17 H17 0.9500
C18 H18 0.9500
C19 C20 1.442(10)
C19 H19A 0.9900
C19 H19B 0.9900
C20 H20A 0.9900
C20 H20B 0.9900
C21 H21A 0.9800
C21 H21B 0.9800
C21 H21C 0.9800
C22 H22A 0.9800
C22 H22B 0.9800
C22 H22C 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
N1 Pt1 O1 C1 17.8(5)
N2 Pt1 O1 C1 102.7(5)
Cl1 Pt1 O1 C1 -71.5(5)
Cl2 Pt1 O1 C1 -163.3(5)
N1 Pt1 O3 C10 -24.7(5)
N2 Pt1 O3 C10 -109.8(5)
Cl1 Pt1 O3 C10 64.7(5)
Cl2 Pt1 O3 C10 156.4(5)
O3 Pt1 N1 C19 -76.2(4)
O1 Pt1 N1 C19 100.4(4)
N2 Pt1 N1 C19 12.7(4)
Cl1 Pt1 N1 C19 -169.2(4)
O3 Pt1 N2 C22 -140.3(4)
O1 Pt1 N2 C22 32.3(4)
N1 Pt1 N2 C22 127.7(5)
Cl2 Pt1 N2 C22 -53.4(4)
O3 Pt1 N2 C21 -16.1(5)
O1 Pt1 N2 C21 156.6(5)
N1 Pt1 N2 C21 -108.0(5)
Cl2 Pt1 N2 C21 70.9(5)
O3 Pt1 N2 C20 104.2(4)
O1 Pt1 N2 C20 -83.2(4)
N1 Pt1 N2 C20 12.3(4)
Cl2 Pt1 N2 C20 -168.9(4)
Pt1 O1 C1 O2 -0.3(10)
Pt1 O1 C1 C2 -178.6(4)
O2 C1 C2 C3 -4.2(10)
O1 C1 C2 C3 174.2(6)
C1 C2 C3 C4 -177.7(6)
C2 C3 C4 C5 -179.6(7)
C2 C3 C4 C9 0.5(11)
C9 C4 C5 C6 4.1(10)
C3 C4 C5 C6 -175.8(6)
C4 C5 C6 C7 -0.8(10)
C5 C6 C7 C8 -2.7(10)
C6 C7 C8 C9 2.8(10)
C7 C8 C9 C4 0.6(10)
C5 C4 C9 C8 -4.0(10)
C3 C4 C9 C8 175.9(6)
Pt1 O3 C10 O4 -8.6(9)
Pt1 O3 C10 C11 170.5(4)
O4 C10 C11 C12 -10.2(11)
O3 C10 C11 C12 170.7(6)
C10 C11 C12 C13 178.8(6)
C11 C12 C13 C14 179.4(7)
C11 C12 C13 C18 -4.1(11)
C18 C13 C14 C15 1.1(10)
C12 C13 C14 C15 177.8(6)
C13 C14 C15 C16 -0.6(11)
C14 C15 C16 C17 2.1(10)
C15 C16 C17 C18 -4.2(10)
C16 C17 C18 C13 4.8(10)
C14 C13 C18 C17 -3.2(10)
C12 C13 C18 C17 -179.8(6)
Pt1 N1 C19 C20 -37.2(7)
N1 C19 C20 N2 51.8(9)
C22 N2 C20 C19 -157.4(6)
C21 N2 C20 C19 84.6(7)
Pt1 N2 C20 C19 -37.3(7)
