#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:36:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179853 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/49/7014996.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_7014996
loop_
_publ_author_name
'Crosby, Sarah H.'
'Deeth, Robert J.'
'Clarkson, Guy J.'
'Rourke, Jonathan P.'
_publ_section_title
;
 Platinum(IV) centres with agostic interactions from either sp²
 or sp³ C-H bonds.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1227
_journal_page_last               1229
_journal_paper_doi               10.1039/c0dt01428a
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C15 H15 Cl3 F N Pt'
_chemical_formula_weight         529.72
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 111.7518(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0861(2)
_cell_length_b                   8.07835(10)
_cell_length_c                   15.9059(3)
_cell_measurement_reflns_used    11638
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.75
_cell_measurement_theta_min      3.02
_cell_volume                     1561.75(5)
_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 0.990
_diffrn_measured_fraction_theta_max 0.927
_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  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18193
_diffrn_reflns_theta_full        29.50
_diffrn_reflns_theta_max         30.82
_diffrn_reflns_theta_min         3.03
_diffrn_standards_decay_%        nil
_exptl_absorpt_coefficient_mu    9.499
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.42
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSPACK(CrysAlis, Oxford Diffraction)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.400
_refine_diff_density_min         -1.780
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         4551
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0204
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0207P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0420
_refine_ls_wR_factor_ref         0.0428
_reflns_number_gt                3917
_reflns_number_total             4551
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0DT01428A.TXT
_cod_data_source_block           sc14
_cod_original_cell_volume        1561.75(4)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7014996
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.229160(8) 0.563377(12) 0.415608(6) 0.01009(4) Uani 1 1 d . . .
N1 N 0.21776(18) 0.7518(3) 0.32817(14) 0.0099(4) Uani 1 1 d . . .
Cl1 Cl 0.24001(6) 0.34887(8) 0.51348(4) 0.01704(14) Uani 1 1 d . . .
Cl2 Cl 0.07393(5) 0.66141(8) 0.43649(4) 0.01446(13) Uani 1 1 d . . .
C2 C 0.1641(2) 0.7436(3) 0.23670(17) 0.0116(5) Uani 1 1 d . . .
Cl3 Cl 0.38087(6) 0.46633(8) 0.39059(5) 0.01678(14) Uani 1 1 d . . .
C3 C 0.1653(2) 0.8813(3) 0.18565(18) 0.0151(6) Uani 1 1 d . . .
H3A H 0.1302 0.8769 0.1216 0.018 Uiso 1 1 calc R . .
C4 C 0.2172(2) 1.0263(3) 0.22676(19) 0.0157(6) Uani 1 1 d . . .
H4A H 0.2169 1.1207 0.1911 0.019 Uiso 1 1 calc R . .
C5 C 0.2691(2) 1.0325(3) 0.31962(19) 0.0149(6) Uani 1 1 d . . .
H5A H 0.3037 1.1314 0.3486 0.018 Uiso 1 1 calc R . .
C6 C 0.2699(2) 0.8927(3) 0.36981(18) 0.0128(5) Uani 1 1 d . . .
C7 C 0.3275(2) 0.8766(3) 0.46789(18) 0.0126(5) Uani 1 1 d . . .
C8 C 0.3894(2) 1.0035(4) 0.52401(19) 0.0151(6) Uani 1 1 d . . .
H8A H 0.3932 1.1090 0.4989 0.018 Uiso 1 1 calc R . .
C9 C 0.4450(2) 0.9764(4) 0.61559(19) 0.0172(6) Uani 1 1 d . . .
H9A H 0.4856 1.0625 0.6542 0.021 Uiso 1 1 calc R . .
F10 F 0.49603(14) 0.7931(2) 0.73880(10) 0.0262(4) Uani 1 1 d . . .
C10 C 0.4398(2) 0.8207(4) 0.64904(18) 0.0177(6) Uani 1 1 d . . .
C11 C 0.3797(2) 0.6911(4) 0.59802(18) 0.0153(6) Uani 1 1 d . . .
H11A H 0.3770 0.5859 0.6238 0.018 Uiso 1 1 calc R . .
C12 C 0.3237(2) 0.7234(3) 0.50704(18) 0.0125(5) Uani 1 1 d . . .
C13 C 0.1080(2) 0.5831(3) 0.18995(17) 0.0117(5) Uani 1 1 d . . .
C14 C -0.0062(2) 0.6261(4) 0.11820(19) 0.0168(6) Uani 1 1 d . . .
H14A H 0.0028 0.7020 0.0734 0.025 Uiso 1 1 calc R . .
H14B H -0.0514 0.6789 0.1478 0.025 Uiso 1 1 calc R . .
H14C H -0.0424 0.5245 0.0879 0.025 Uiso 1 1 calc R . .
C15 C 0.1804(2) 0.5044(4) 0.14307(19) 0.0152(6) Uani 1 1 d . . .
H15A H 0.1926 0.5848 0.1016 0.023 Uiso 1 1 calc R . .
H15B H 0.1433 0.4065 0.1089 0.023 Uiso 1 1 calc R . .
H15C H 0.2513 0.4718 0.1889 0.023 Uiso 1 1 calc R . .
C16 C 0.0864(3) 0.4547(4) 0.25242(19) 0.0159(6) Uani 1 1 d . . .
H16A H 0.159(3) 0.406(4) 0.299(2) 0.024 Uiso 1 1 d . . .
H16B H 0.049(3) 0.358(4) 0.209(2) 0.024 Uiso 1 1 d . . .
H16C H 0.037(3) 0.501(4) 0.275(2) 0.024 Uiso 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'
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
_geom_angle_publ_flag
C12 Pt1 N1 83.21(10) . . ?
C12 Pt1 Cl1 97.41(8) . . ?
N1 Pt1 Cl1 179.30(7) . . ?
C12 Pt1 Cl3 90.30(8) . . ?
N1 Pt1 Cl3 89.20(6) . . ?
Cl1 Pt1 Cl3 91.12(2) . . ?
C12 Pt1 Cl2 90.78(8) . . ?
N1 Pt1 Cl2 89.79(6) . . ?
Cl1 Pt1 Cl2 89.88(2) . . ?
Cl3 Pt1 Cl2 178.42(2) . . ?
C12 Pt1 H16A 164.0(9) . . ?
N1 Pt1 H16A 87.3(8) . . ?
Cl1 Pt1 H16A 92.2(8) . . ?
Cl3 Pt1 H16A 76.7(9) . . ?
Cl2 Pt1 H16A 102.1(9) . . ?
C2 N1 C6 121.7(2) . . ?
C2 N1 Pt1 124.98(17) . . ?
C6 N1 Pt1 113.34(17) . . ?
N1 C2 C3 118.4(2) . . ?
N1 C2 C13 121.4(2) . . ?
C3 C2 C13 120.1(2) . . ?
C2 C3 C4 120.8(2) . . ?
C2 C3 H3A 119.6 . . ?
C4 C3 H3A 119.6 . . ?
C5 C4 C3 119.7(3) . . ?
C5 C4 H4A 120.2 . . ?
C3 C4 H4A 120.2 . . ?
C4 C5 C6 119.0(3) . . ?
C4 C5 H5A 120.5 . . ?
C6 C5 H5A 120.5 . . ?
N1 C6 C5 120.4(2) . . ?
N1 C6 C7 114.2(2) . . ?
C5 C6 C7 125.4(3) . . ?
C12 C7 C8 118.2(2) . . ?
C12 C7 C6 117.7(2) . . ?
C8 C7 C6 124.1(3) . . ?
C9 C8 C7 120.6(3) . . ?
C9 C8 H8A 119.7 . . ?
C7 C8 H8A 119.7 . . ?
C10 C9 C8 118.0(3) . . ?
C10 C9 H9A 121.0 . . ?
C8 C9 H9A 121.0 . . ?
F10 C10 C9 118.1(2) . . ?
F10 C10 C11 117.5(3) . . ?
C9 C10 C11 124.4(3) . . ?
C10 C11 C12 115.9(3) . . ?
C10 C11 H11A 122.0 . . ?
C12 C11 H11A 122.0 . . ?
C11 C12 C7 122.8(3) . . ?
C11 C12 Pt1 125.8(2) . . ?
C7 C12 Pt1 111.38(19) . . ?
C16 C13 C2 115.2(2) . . ?
C16 C13 C15 109.1(2) . . ?
C2 C13 C15 108.1(2) . . ?
C16 C13 C14 105.7(2) . . ?
C2 C13 C14 109.0(2) . . ?
C15 C13 C14 109.5(2) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 112.2(18) . . ?
C13 C16 H16B 103.6(17) . . ?
H16A C16 H16B 105(2) . . ?
C13 C16 H16C 107(2) . . ?
H16A C16 H16C 118(3) . . ?
H16B C16 H16C 110(3) . . ?
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 C12 1.996(3) . ?
Pt1 N1 2.029(2) . ?
Pt1 Cl1 2.2984(6) . ?
Pt1 Cl3 2.3021(7) . ?
Pt1 Cl2 2.3161(6) . ?
Pt1 H16A 2.16(3) . ?
N1 C2 1.363(3) . ?
N1 C6 1.366(3) . ?
C2 C3 1.381(4) . ?
C2 C13 1.539(4) . ?
C3 C4 1.389(4) . ?
C3 H3A 0.9500 . ?
C4 C5 1.379(4) . ?
C4 H4A 0.9500 . ?
C5 C6 1.380(4) . ?
C5 H5A 0.9500 . ?
C6 C7 1.465(4) . ?
C7 C12 1.394(4) . ?
C7 C8 1.403(4) . ?
C8 C9 1.383(4) . ?
C8 H8A 0.9500 . ?
C9 C10 1.377(4) . ?
C9 H9A 0.9500 . ?
F10 C10 1.361(3) . ?
C10 C11 1.379(4) . ?
C11 C12 1.383(4) . ?
C11 H11A 0.9500 . ?
C13 C16 1.533(4) . ?
C13 C15 1.544(4) . ?
C13 C14 1.546(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 1.04(3) . ?
C16 H16B 1.03(3) . ?
C16 H16C 0.93(3) . ?
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 Cl2 0.95 2.78 3.707(3) 167.0 4_575
C9 H9A F10 0.95 2.47 3.344(3) 152.3 2_656
