#------------------------------------------------------------------------------
#$Date: 2016-03-21 13:58:25 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178708 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/19/4081937.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_4081937
loop_
_publ_author_name
'Kluge, Tim'
'Bette, Martin'
'Rüffer, Tobias'
'Bruhn, Clemens'
'Wagner, Christoph'
'Ströhl, Dieter'
'Schmidt, Jürgen'
'Steinborn, Dirk'
_publ_section_title
;
 Activation of Acetyl Ligands through Hydrogen Bonds: A New Way to
 Platinum(II) Complexes Bearing Protonated Iminoacetyl Ligands
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              7090
_journal_paper_doi               10.1021/om400812w
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C13 H17 N3 O2 Pt'
_chemical_formula_sum            'C13 H17 N3 O2 Pt'
_chemical_formula_weight         442.39
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   5.3000(3)
_cell_length_b                   10.4320(7)
_cell_length_c                   25.1210(18)
_cell_measurement_reflns_used    5127
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.72
_cell_measurement_theta_min      3.12
_cell_volume                     1388.93(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'area detector'
_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  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            5565
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    10.104
_exptl_absorpt_correction_T_max  0.7854
_exptl_absorpt_correction_T_min  0.5254
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(IPDS Software; Stoe & Cie, 1999)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.116
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.478
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.018
_refine_diff_density_max         1.186
_refine_diff_density_min         -1.612
_refine_diff_density_rms         0.187
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_coef       0.0053(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         3003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0355
_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)+(0.0684P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1098
_reflns_number_gt                2540
_reflns_number_total             3003
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400812w_si_003.cif
_cod_data_source_block           c:\i2t0652
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               4081937
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -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
C1 C 0.146(2) -0.1525(12) 0.1371(4) 0.039(2) Uani 1 1 d .
C2 C 0.147(2) -0.2626(9) 0.1730(5) 0.042(3) Uani 1 1 d .
H1 H 0.0588 -0.3345 0.1561 0.050 Uiso 1 1 calc R
H3 H 0.0613 -0.2398 0.2062 0.050 Uiso 1 1 calc R
H2 H 0.3216 -0.2874 0.1807 0.050 Uiso 1 1 calc R
C3 C 0.493(2) -0.0608(11) 0.2156(4) 0.039(2) Uani 1 1 d .
C4 C 0.366(2) 0.0040(15) 0.2608(4) 0.052(3) Uani 1 1 d .
H5 H 0.4523 -0.0183 0.2940 0.062 Uiso 1 1 calc R
H4 H 0.1899 -0.0240 0.2626 0.062 Uiso 1 1 calc R
H6 H 0.3724 0.0970 0.2555 0.062 Uiso 1 1 calc R
C5 C 0.629(2) 0.2209(12) 0.0956(4) 0.040(2) Uani 1 1 d .
C6 C 0.794(2) 0.3233(10) 0.0877(4) 0.038(2) Uani 1 1 d .
H7 H 0.7780 0.3753 0.0569 0.046 Uiso 1 1 calc R
C7 C 0.976(2) 0.3489(11) 0.1240(5) 0.044(3) Uani 1 1 d .
H8 H 1.0853 0.4199 0.1190 0.052 Uiso 1 1 calc R
C8 C 1.002(2) 0.2713(11) 0.1686(5) 0.040(2) Uani 1 1 d .
H9 H 1.1312 0.2871 0.1941 0.048 Uiso 1 1 calc R
C9 C 0.836(2) 0.1707(12) 0.1750(4) 0.039(2) Uani 1 1 d .
H10 H 0.8525 0.1152 0.2048 0.047 Uiso 1 1 calc R
C10 C 0.428(2) 0.1883(12) 0.0584(4) 0.040(2) Uani 1 1 d .
H11 H 0.3936 0.2396 0.0279 0.048 Uiso 1 1 calc R
C11 C -0.201(2) -0.2414(11) 0.0847(5) 0.043(3) Uani 1 1 d .
H12 H -0.3452 -0.1984 0.0670 0.052 Uiso 1 1 calc R
H13 H -0.2646 -0.2790 0.1183 0.052 Uiso 1 1 calc R
C12 C -0.113(3) -0.3452(11) 0.0504(5) 0.051(3) Uani 1 1 d .
H14 H -0.2396 -0.3974 0.0345 0.061 Uiso 1 1 calc R
C13 C 0.128(3) -0.3749(11) 0.0388(5) 0.053(3) Uani 1 1 d .
H16 H 0.2616 -0.3259 0.0536 0.064 Uiso 1 1 calc R
H15 H 0.1642 -0.4449 0.0159 0.064 Uiso 1 1 calc R
N1 N 0.2971(18) 0.0860(8) 0.0688(3) 0.0347(18) Uani 1 1 d .
N2 N 0.6513(17) 0.1505(10) 0.1395(3) 0.0374(19) Uani 1 1 d .
N3 N -0.0133(18) -0.1457(9) 0.0975(4) 0.038(2) Uani 1 1 d .
H17 H -0.0054 -0.0775 0.0769 0.046 Uiso 1 1 calc R
O1 O 0.1085(13) 0.0548(7) 0.0377(3) 0.0402(17) Uani 1 1 d .
O2 O 0.6529(19) -0.1398(10) 0.2246(4) 0.065(3) Uani 1 1 d .
Pt Pt 0.38960(5) -0.00320(4) 0.142652(12) 0.03210(16) 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'
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
N3 C1 C2 121.1(11)
N3 C1 Pt 114.9(8)
C2 C1 Pt 124.0(8)
C1 C2 H1 109.5
C1 C2 H3 109.5
H1 C2 H3 109.5
C1 C2 H2 109.5
H1 C2 H2 109.5
H3 C2 H2 109.5
O2 C3 C4 119.3(10)
O2 C3 Pt 124.6(9)
C4 C3 Pt 116.0(8)
C3 C4 H5 109.5
C3 C4 H4 109.5
H5 C4 H4 109.5
C3 C4 H6 109.5
H5 C4 H6 109.5
H4 C4 H6 109.5
N2 C5 C6 119.1(10)
N2 C5 C10 117.8(10)
C6 C5 C10 123.0(10)
C7 C6 C5 120.1(10)
C7 C6 H7 120.0
C5 C6 H7 120.0
C6 C7 C8 120.0(11)
C6 C7 H8 120.0
C8 C7 H8 120.0
C9 C8 C7 118.1(11)
C9 C8 H9 120.9
C7 C8 H9 120.9
N2 C9 C8 120.6(11)
N2 C9 H10 119.7
C8 C9 H10 119.7
N1 C10 C5 116.8(10)
N1 C10 H11 121.6
C5 C10 H11 121.6
N3 C11 C12 115.0(10)
N3 C11 H12 108.5
C12 C11 H12 108.5
N3 C11 H13 108.5
C12 C11 H13 108.5
H12 C11 H13 107.5
C13 C12 C11 126.9(11)
C13 C12 H14 116.5
C11 C12 H14 116.5
C12 C13 H16 120.0
C12 C13 H15 120.0
H16 C13 H15 120.0
C10 N1 O1 119.2(8)
C10 N1 Pt 114.4(7)
O1 N1 Pt 126.0(7)
C5 N2 C9 121.9(10)
C5 N2 Pt 113.0(7)
C9 N2 Pt 124.8(8)
C1 N3 C11 125.2(10)
C1 N3 H17 117.4
C11 N3 H17 117.4
C3 Pt C1 90.4(4)
C3 Pt N2 94.7(4)
C1 Pt N2 173.8(4)
C3 Pt N1 171.4(4)
C1 Pt N1 97.4(4)
N2 Pt N1 77.7(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N3 1.308(14)
C1 C2 1.459(15)
C1 Pt 2.029(12)
C2 H1 0.9800
C2 H3 0.9800
C2 H2 0.9800
C3 O2 1.203(14)
C3 C4 1.481(16)
C3 Pt 2.006(10)
C4 H5 0.9800
C4 H4 0.9800
C4 H6 0.9800
C5 N2 1.329(14)
C5 C6 1.392(16)
C5 C10 1.460(14)
C6 C7 1.353(16)
C6 H7 0.9500
C7 C8 1.390(16)
C7 H8 0.9500
C8 C9 1.379(16)
C8 H9 0.9500
C9 N2 1.341(13)
C9 H10 0.9500
C10 N1 1.300(14)
C10 H11 0.9500
C11 N3 1.446(14)
C11 C12 1.461(17)
C11 H12 0.9900
C11 H13 0.9900
C12 C13 1.347(18)
C12 H14 0.9500
C13 H16 0.9500
C13 H15 0.9500
N1 O1 1.311(11)
N1 Pt 2.131(8)
N2 Pt 2.122(9)
N3 H17 0.8800
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
N3 H17 O1 0.88 1.80 2.655(12) 163.1
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
N2 C5 C6 C7 1.2(18)
C10 C5 C6 C7 179.5(11)
C5 C6 C7 C8 1.3(18)
C6 C7 C8 C9 -1.2(18)
C7 C8 C9 N2 -1.3(18)
N2 C5 C10 N1 -5.5(16)
C6 C5 C10 N1 176.1(11)
N3 C11 C12 C13 14.6(18)
C5 C10 N1 O1 177.8(9)
C5 C10 N1 Pt 4.9(13)
C6 C5 N2 C9 -3.8(17)
C10 C5 N2 C9 177.7(10)
C6 C5 N2 Pt -178.5(9)
C10 C5 N2 Pt 3.0(13)
C8 C9 N2 C5 3.9(18)
C8 C9 N2 Pt 178.0(9)
C2 C1 N3 C11 0.4(18)
Pt C1 N3 C11 178.7(9)
C12 C11 N3 C1 -86.9(14)
O2 C3 Pt C1 85.2(11)
C4 C3 Pt C1 -97.1(9)
O2 C3 Pt N2 -91.3(11)
C4 C3 Pt N2 86.5(9)
N3 C1 Pt C3 167.8(9)
C2 C1 Pt C3 -13.9(10)
N3 C1 Pt N1 -8.5(9)
C2 C1 Pt N1 169.7(10)
C5 N2 Pt C3 -176.2(8)
C9 N2 Pt C3 9.4(10)
C5 N2 Pt N1 -0.4(8)
C9 N2 Pt N1 -174.9(10)
C10 N1 Pt C1 -178.7(8)
O1 N1 Pt C1 9.1(9)
C10 N1 Pt N2 -2.6(8)
O1 N1 Pt N2 -174.8(9)
