#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:30:25 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178568 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/77/4067710.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_4067710
loop_
_publ_author_name
'Crosby, Sarah H.'
'Clarkson, Guy J.'
'Deeth, Robert J.'
'Rourke, Jonathan P.'
_publ_section_title
;
 Platinum(IV) DMSO Complexes: Synthesis, Isomerization, and Agostic
 Intermediates
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1966
_journal_paper_doi               10.1021/om901087m
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C14 H13 Cl F N Pt'
_chemical_formula_weight         444.79
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                   15.3935(3)
_cell_length_b                   7.33660(10)
_cell_length_c                   22.4051(4)
_cell_measurement_reflns_used    8972
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.33
_cell_measurement_theta_min      2.72
_cell_volume                     2530.34(8)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.2833
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'Oxford Diffraction Gemini R'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            15969
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.38
_diffrn_reflns_theta_min         3.08
_diffrn_standards_decay_%        nil
_exptl_absorpt_coefficient_mu    11.293
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.38
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSPACK(CrysAlis, Oxford Diffraction)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.027
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         3203
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0176
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0151P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0305
_refine_ls_wR_factor_ref         0.0317
_reflns_number_gt                2596
_reflns_number_total             3203
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om901087m_si_004.cif
_cod_data_source_block           5c
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               4067710
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, 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
Pt1 Pt 0.440376(6) 0.215636(13) 0.488539(4) 0.01200(4) Uani 1 1 d .
Cl1 Cl 0.51288(4) 0.03280(8) 0.56606(3) 0.01767(14) Uani 1 1 d .
N1 N 0.39291(14) 0.4490(3) 0.52929(9) 0.0128(5) Uani 1 1 d .
C2 C 0.39611(17) 0.4984(3) 0.58815(10) 0.0140(5) Uani 1 1 d .
C3 C 0.36081(18) 0.6625(3) 0.60713(11) 0.0166(6) Uani 1 1 d .
H3A H 0.3642 0.6950 0.6481 0.020 Uiso 1 1 calc R
C4 C 0.32103(18) 0.7786(3) 0.56763(11) 0.0182(6) Uani 1 1 d .
H4A H 0.2968 0.8905 0.5809 0.022 Uiso 1 1 calc R
C5 C 0.31691(17) 0.7300(3) 0.50850(11) 0.0166(6) Uani 1 1 d .
H5A H 0.2889 0.8075 0.4805 0.020 Uiso 1 1 calc R
C6 C 0.35406(16) 0.5666(3) 0.48980(11) 0.0134(5) Uani 1 1 d .
C7 C 0.35331(17) 0.5073(3) 0.42799(11) 0.0142(6) Uani 1 1 d .
C8 C 0.39218(17) 0.3368(3) 0.41737(11) 0.0137(5) Uani 1 1 d .
C9 C 0.39497(19) 0.2729(4) 0.35880(12) 0.0193(6) Uani 1 1 d .
H9A H 0.4217 0.1594 0.3498 0.023 Uiso 1 1 calc R
F10 F 0.36090(12) 0.3114(2) 0.25729(7) 0.0344(4) Uani 1 1 d .
C10 C 0.35866(19) 0.3762(4) 0.31439(11) 0.0220(6) Uani 1 1 d .
C11 C 0.31905(19) 0.5422(3) 0.32367(11) 0.0208(6) Uani 1 1 d .
H11A H 0.2939 0.6086 0.2916 0.025 Uiso 1 1 calc R
C12 C 0.31732(18) 0.6084(3) 0.38157(11) 0.0182(6) Uani 1 1 d .
H12A H 0.2915 0.7233 0.3896 0.022 Uiso 1 1 calc R
C13 C 0.43348(18) 0.3751(4) 0.63460(11) 0.0177(6) Uani 1 1 d .
H13A H 0.4548 0.4488 0.6686 0.021 Uiso 1 1 calc R
H13B H 0.4835 0.3079 0.6176 0.021 Uiso 1 1 calc R
C14 C 0.3651(2) 0.2389(3) 0.65685(12) 0.0229(7) Uani 1 1 d .
H14A H 0.3136 0.3073 0.6709 0.027 Uiso 1 1 calc R
H14B H 0.3466 0.1615 0.6230 0.027 Uiso 1 1 calc R
C15 C 0.3971(2) 0.1171(4) 0.70698(13) 0.0352(8) Uani 1 1 d .
H15A H 0.3495 0.0384 0.7205 0.053 Uiso 1 1 calc R
H15B H 0.4172 0.1926 0.7403 0.053 Uiso 1 1 calc R
H15C H 0.4452 0.0416 0.6925 0.053 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'
F F 0.0171 0.0103 '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
C8 Pt1 N1 81.45(9) . .
C8 Pt1 Cl1 92.55(7) . 5_656
N1 Pt1 Cl1 173.99(6) . 5_656
C8 Pt1 Cl1 170.84(7) . .
N1 Pt1 Cl1 107.40(6) . .
Cl1 Pt1 Cl1 78.61(2) 5_656 .
Pt1 Cl1 Pt1 101.39(2) 5_656 .
C2 N1 C6 118.1(2) . .
C2 N1 Pt1 129.05(16) . .
C6 N1 Pt1 112.86(15) . .
N1 C2 C3 120.7(2) . .
N1 C2 C13 121.7(2) . .
C3 C2 C13 117.5(2) . .
C4 C3 C2 121.0(2) . .
C4 C3 H3A 119.5 . .
C2 C3 H3A 119.5 . .
C3 C4 C5 118.8(2) . .
C3 C4 H4A 120.6 . .
C5 C4 H4A 120.6 . .
C4 C5 C6 119.6(2) . .
C4 C5 H5A 120.2 . .
C6 C5 H5A 120.2 . .
N1 C6 C5 121.7(2) . .
N1 C6 C7 115.5(2) . .
C5 C6 C7 122.8(2) . .
C12 C7 C8 121.1(2) . .
C12 C7 C6 123.8(2) . .
C8 C7 C6 115.1(2) . .
C9 C8 C7 118.1(2) . .
C9 C8 Pt1 126.8(2) . .
C7 C8 Pt1 115.10(17) . .
C10 C9 C8 119.0(2) . .
C10 C9 H9A 120.5 . .
C8 C9 H9A 120.5 . .
F10 C10 C9 118.5(2) . .
F10 C10 C11 117.4(2) . .
C9 C10 C11 124.1(2) . .
C10 C11 C12 117.4(2) . .
C10 C11 H11A 121.3 . .
C12 C11 H11A 121.3 . .
C11 C12 C7 120.3(2) . .
C11 C12 H12A 119.8 . .
C7 C12 H12A 119.8 . .
C2 C13 C14 110.9(2) . .
C2 C13 H13A 109.5 . .
C14 C13 H13A 109.5 . .
C2 C13 H13B 109.5 . .
C14 C13 H13B 109.5 . .
H13A C13 H13B 108.1 . .
C15 C14 C13 113.7(3) . .
C15 C14 H14A 108.8 . .
C13 C14 H14A 108.8 . .
C15 C14 H14B 108.8 . .
C13 C14 H14B 108.8 . .
H14A C14 H14B 107.7 . .
C14 C15 H15A 109.5 . .
C14 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C14 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 C8 1.970(2) .
Pt1 N1 2.0737(19) .
Pt1 Cl1 2.3100(6) 5_656
Pt1 Cl1 2.4620(6) .
Cl1 Pt1 2.3100(6) 5_656
N1 C2 1.368(3) .
N1 C6 1.373(3) .
C2 C3 1.388(3) .
C2 C13 1.494(3) .
C3 C4 1.372(4) .
C3 H3A 0.9500 .
C4 C5 1.373(3) .
C4 H4A 0.9500 .
C5 C6 1.393(3) .
C5 H5A 0.9500 .
C6 C7 1.452(3) .
C7 C12 1.392(3) .
C7 C8 1.407(3) .
C8 C9 1.394(3) .
C9 C10 1.370(4) .
C9 H9A 0.9500 .
F10 C10 1.365(3) .
C10 C11 1.377(4) .
C11 C12 1.385(3) .
C11 H11A 0.9500 .
C12 H12A 0.9500 .
C13 C14 1.534(4) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 C15 1.517(4) .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
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
_geom_hbond_site_symmetry_A
C3 H3A F10 0.95 2.45 3.370(3) 163.7 7_566
