#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/88/1518838.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_1518838
loop_
_publ_author_name
'Xu, Long'
'Solowey, Douglas P.'
'Vicic, David A.'
_publ_section_title
;
 Stepwise Conversion of a Platinum Dimethyl Complex to a
 Perfluorometallacyclobutane Derivative
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3474
_journal_paper_doi               10.1021/acs.organomet.5b00045
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C11 H12 F4 O2 Pt'
_chemical_formula_weight         447.30
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                102.145(6)
_cell_angle_beta                 93.505(5)
_cell_angle_gamma                100.070(5)
_cell_formula_units_Z            2
_cell_length_a                   6.3410(14)
_cell_length_b                   8.327(2)
_cell_length_c                   11.491(3)
_cell_measurement_temperature    142(2)
_cell_volume                     581.0(2)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      142(2)
_diffrn_measured_fraction_theta_full 0.841
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 0.841
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1772
_diffrn_reflns_point_group_measured_fraction_full 0.841
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.783
_diffrn_reflns_theta_min         3.280
_exptl_absorpt_coefficient_mu    12.119
_exptl_absorpt_correction_T_max  0.744970
_exptl_absorpt_correction_T_min  0.411412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.557
_exptl_crystal_description       needle
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_refine_diff_density_max         3.148
_refine_diff_density_min         -1.354
_refine_diff_density_rms         0.331
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         1772
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0822P)²+7.0581P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1280
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1685
_reflns_number_total             1772
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            om5b00045_si_001.cif
_cod_data_source_block           Compound13
_cod_depositor_comments
'Adding full bibliography for 1518835--1518839.cif.'
_cod_database_code               1518838
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.138
_shelx_estimated_absorpt_t_max   0.888
_shelxl_version_number           2014/6
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Pt1 Pt 0.28815(9) 0.54056(8) 0.76117(5) 0.0283(3) Uani 1 1 d . .
O1 O -0.078(2) 0.1587(15) 0.8667(11) 0.044(3) Uani 1 1 d . .
O2 O 0.1312(19) 0.4075(18) 0.8720(11) 0.047(3) Uani 1 1 d . .
F1 F 0.1132(16) 0.3426(14) 0.5232(9) 0.047(3) Uani 1 1 d . .
F2 F 0.3039(16) 0.2197(13) 0.6266(11) 0.050(3) Uani 1 1 d . .
F3 F -0.1961(16) 0.3322(14) 0.6627(10) 0.048(3) Uani 1 1 d . .
F4 F -0.1024(19) 0.0860(14) 0.6248(10) 0.051(3) Uani 1 1 d . .
C1 C 0.161(3) 0.327(2) 0.6308(18) 0.043(5) Uani 1 1 d . .
C2 C -0.034(2) 0.2474(19) 0.6841(14) 0.027(3) Uani 1 1 d . .
C3 C 0.006(3) 0.270(3) 0.8202(17) 0.040(4) Uani 1 1 d . .
C4 C 0.730(3) 0.720(2) 0.8763(14) 0.039(4) Uani 1 1 d . .
H4A H 0.8273 0.8197 0.9273 0.046 Uiso 1 1 calc R U
H4B H 0.7857 0.6204 0.8880 0.046 Uiso 1 1 calc R U
C5 C 0.504(3) 0.711(2) 0.9212(14) 0.040(4) Uani 1 1 d . .
H5A H 0.4890 0.6762 0.9990 0.048 Uiso 1 1 calc R U
C6 C 0.354(3) 0.800(2) 0.8898(16) 0.041(4) Uani 1 1 d . .
H6A H 0.2438 0.8166 0.9478 0.050 Uiso 1 1 calc R U
C7 C 0.391(3) 0.930(2) 0.8193(17) 0.045(5) Uani 1 1 d . .
H7A H 0.5455 0.9834 0.8337 0.054 Uiso 1 1 calc R U
H7B H 0.3070 1.0166 0.8488 0.054 Uiso 1 1 calc R U
C8 C 0.332(3) 0.866(2) 0.6846(18) 0.038(4) Uani 1 1 d . .
H8A H 0.1786 0.8688 0.6659 0.046 Uiso 1 1 calc R U
H8B H 0.4184 0.9429 0.6430 0.046 Uiso 1 1 calc R U
C9 C 0.366(3) 0.6941(19) 0.6361(14) 0.027(3) Uani 1 1 d . .
H9A H 0.2933 0.6437 0.5536 0.033 Uiso 1 1 calc R U
C10 C 0.547(3) 0.628(2) 0.6627(14) 0.031(4) Uani 1 1 d . .
H10A H 0.5807 0.5405 0.5962 0.037 Uiso 1 1 calc R U
C11 C 0.744(3) 0.731(2) 0.7496(17) 0.038(4) Uani 1 1 d . .
H11A H 0.8747 0.6912 0.7224 0.046 Uiso 1 1 calc R U
H11B H 0.7597 0.8496 0.7449 0.046 Uiso 1 1 calc R U
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'
O O 0.0106 0.0060 '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'
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
O2 Pt1 C1 83.2(7)
O2 Pt1 C9 164.3(6)
C1 Pt1 C9 94.5(7)
O2 Pt1 C10 157.6(6)
C1 Pt1 C10 95.2(7)
C9 Pt1 C10 38.0(6)
O2 Pt1 C5 90.3(6)
C1 Pt1 C5 159.1(7)
C9 Pt1 C5 96.9(7)
C10 Pt1 C5 83.3(7)
O2 Pt1 C6 97.9(6)
C1 Pt1 C6 165.6(7)
C9 Pt1 C6 80.5(7)
C10 Pt1 C6 89.1(7)
C5 Pt1 C6 35.1(7)
C3 O2 Pt1 115.8(11)
F1 C1 F2 108.5(16)
F1 C1 C2 112.3(15)
F2 C1 C2 106.0(14)
F1 C1 Pt1 118.4(12)
F2 C1 Pt1 107.7(12)
C2 C1 Pt1 103.1(12)
F4 C2 F3 106.7(12)
F4 C2 C1 110.2(14)
F3 C2 C1 106.1(13)
F4 C2 C3 113.8(14)
F3 C2 C3 107.2(13)
C1 C2 C3 112.4(13)
O1 C3 O2 127.4(17)
O1 C3 C2 118.8(16)
O2 C3 C2 113.8(15)
C11 C4 C5 116.4(14)
C11 C4 H4A 108.2
C5 C4 H4A 108.2
C11 C4 H4B 108.2
C5 C4 H4B 108.2
H4A C4 H4B 107.3
C6 C5 C4 124.2(17)
C6 C5 Pt1 73.5(10)
C4 C5 Pt1 102.4(10)
C6 C5 H5A 115.6
C4 C5 H5A 115.6
Pt1 C5 H5A 115.6
C5 C6 C7 125.5(16)
C5 C6 Pt1 71.4(10)
C7 C6 Pt1 108.8(11)
C5 C6 H6A 114.2
C7 C6 H6A 114.2
Pt1 C6 H6A 114.2
C6 C7 C8 114.9(14)
C6 C7 H7A 108.5
C8 C7 H7A 108.5
C6 C7 H7B 108.5
C8 C7 H7B 108.5
H7A C7 H7B 107.5
C9 C8 C7 114.8(14)
C9 C8 H8A 108.6
C7 C8 H8A 108.6
C9 C8 H8B 108.6
C7 C8 H8B 108.6
H8A C8 H8B 107.5
C10 C9 C8 126.7(15)
C10 C9 Pt1 71.6(9)
C8 C9 Pt1 110.1(11)
C10 C9 H9A 113.5
C8 C9 H9A 113.5
Pt1 C9 H9A 113.5
C9 C10 C11 122.9(15)
C9 C10 Pt1 70.4(9)
C11 C10 Pt1 110.5(11)
C9 C10 H10A 114.9
C11 C10 H10A 114.9
Pt1 C10 H10A 114.9
C4 C11 C10 114.5(13)
C4 C11 H11A 108.6
C10 C11 H11A 108.6
C4 C11 H11B 108.6
C10 C11 H11B 108.6
H11A C11 H11B 107.6
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pt1 O2 2.050(12)
Pt1 C1 2.07(2)
Pt1 C9 2.141(15)
Pt1 C10 2.156(15)
Pt1 C5 2.274(16)
Pt1 C6 2.301(17)
O1 C3 1.23(2)
O2 C3 1.27(2)
F1 C1 1.29(2)
F2 C1 1.37(2)
F3 C2 1.385(19)
F4 C2 1.354(18)
C1 C2 1.52(3)
C2 C3 1.54(2)
C4 C11 1.48(2)
C4 C5 1.55(2)
C4 H4A 0.9900
C4 H4B 0.9900
C5 C6 1.38(3)
C5 H5A 1.0000
C6 C7 1.47(3)
C6 H6A 1.0000
C7 C8 1.53(3)
C7 H7A 0.9900
C7 H7B 0.9900
C8 C9 1.48(2)
C8 H8A 0.9900
C8 H8B 0.9900
C9 C10 1.40(2)
C9 H9A 1.0000
C10 C11 1.55(2)
C10 H10A 1.0000
C11 H11A 0.9900
C11 H11B 0.9900
