#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:43:47 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179125 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/87/4308753.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_4308753
loop_
_publ_author_name
'Anette Yahav'
'Israel Goldberg'
'Arkadi Vigalok'
_publ_section_title
;
Difluoro Complexes of Platinum(II) and -(IV) with Monodentate Phosphine
Ligands: An Exceptional Stability of d6 Octahedral Organometallic Fluorides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1547
_journal_page_last               1553
_journal_paper_doi               10.1021/ic0488177
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C36 H30 F2 P2 Pt'
_chemical_formula_weight         757.63
_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                 116.1981(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7590(2)
_cell_length_b                   33.2970(9)
_cell_length_c                   10.0480(2)
_cell_measurement_reflns_used    5681
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.34
_cell_volume                     2929.64(12)
_computing_cell_refinement       Denzo
_computing_data_collection       'Collect, Nonius B.V.'
_computing_data_reduction        Denzo
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    DIRDIF-96
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean '56 microns'
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '0.9 deg. Phi & Omega 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  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16630
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    4.937
_exptl_absorpt_correction_T_max  0.5247
_exptl_absorpt_correction_T_min  0.4385
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.673
_refine_diff_density_min         -1.435
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6932
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0302P)²+3.2056P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0736
_reflns_number_gt                5681
_reflns_number_total             6932
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0488177si20040826_033003.cif
_cod_data_source_block           ar4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4308753
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
Pt Pt 0.128090(16) 0.108836(4) 0.127851(15) 0.01673(6) Uani 1 1 d . . .
P1 P 0.09520(11) 0.06719(3) 0.28385(10) 0.01508(19) Uani 1 1 d . . .
P2 P 0.01054(11) 0.16272(3) 0.16050(11) 0.0177(2) Uani 1 1 d . . .
F1 F 0.2343(3) 0.06600(7) 0.0691(2) 0.0285(5) Uani 1 1 d . . .
F2 F 0.1691(3) 0.14371(7) -0.0147(3) 0.0314(6) Uani 1 1 d . . .
C1 C 0.1710(4) 0.01730(11) 0.2841(4) 0.0162(8) Uani 1 1 d . . .
C2 C 0.3254(4) 0.01384(12) 0.3203(4) 0.0205(8) Uani 1 1 d . . .
H2 H 0.3867 0.0373 0.3389 0.025 Uiso 1 1 calc R . .
C3 C 0.3902(5) -0.02389(13) 0.3292(4) 0.0246(9) Uani 1 1 d . . .
H3 H 0.4956 -0.0261 0.3533 0.030 Uiso 1 1 calc R . .
C4 C 0.3024(5) -0.05791(13) 0.3033(4) 0.0260(9) Uani 1 1 d . . .
H4 H 0.3476 -0.0836 0.3106 0.031 Uiso 1 1 calc R . .
C5 C 0.1484(5) -0.05498(12) 0.2666(4) 0.0258(9) Uani 1 1 d . . .
H5 H 0.0886 -0.0787 0.2493 0.031 Uiso 1 1 calc R . .
C6 C 0.0808(4) -0.01758(11) 0.2549(4) 0.0201(8) Uani 1 1 d . . .
H6 H -0.0254 -0.0156 0.2275 0.024 Uiso 1 1 calc R . .
C7 C -0.1047(4) 0.05853(11) 0.2401(4) 0.0160(8) Uani 1 1 d . . .
C8 C -0.1625(4) 0.05925(11) 0.3443(4) 0.0168(8) Uani 1 1 d . . .
H8 H -0.0969 0.0649 0.4454 0.020 Uiso 1 1 calc R . .
C9 C -0.3165(4) 0.05176(12) 0.3000(4) 0.0217(8) Uani 1 1 d . . .
H9 H -0.3551 0.0518 0.3718 0.026 Uiso 1 1 calc R . .
C10 C -0.4150(4) 0.04420(13) 0.1524(4) 0.0241(9) Uani 1 1 d . . .
H10 H -0.5207 0.0396 0.1223 0.029 Uiso 1 1 calc R . .
C11 C -0.3557(4) 0.04344(13) 0.0494(4) 0.0240(9) Uani 1 1 d . . .
H11 H -0.4216 0.0379 -0.0517 0.029 Uiso 1 1 calc R . .
C12 C -0.2028(4) 0.05060(12) 0.0916(4) 0.0210(8) Uani 1 1 d . . .
H12 H -0.1643 0.0501 0.0197 0.025 Uiso 1 1 calc R . .
C13 C 0.1941(4) 0.08131(11) 0.4793(4) 0.0173(8) Uani 1 1 d . . .
C14 C 0.2704(4) 0.11771(12) 0.5218(4) 0.0230(9) Uani 1 1 d . . .
H14 H 0.2790 0.1345 0.4494 0.028 Uiso 1 1 calc R . .
C15 C 0.3343(5) 0.12981(14) 0.6693(4) 0.0323(10) Uani 1 1 d . . .
H15 H 0.3851 0.1550 0.6970 0.039 Uiso 1 1 calc R . .
C16 C 0.3242(5) 0.10528(15) 0.7764(5) 0.0345(11) Uani 1 1 d . . .
H16 H 0.3640 0.1140 0.8765 0.041 Uiso 1 1 calc R . .
C17 C 0.2559(5) 0.06810(15) 0.7363(4) 0.0312(10) Uani 1 1 d . . .
H17 H 0.2525 0.0508 0.8100 0.037 Uiso 1 1 calc R . .
C18 C 0.1920(4) 0.05566(13) 0.5897(4) 0.0221(9) Uani 1 1 d . . .
H18 H 0.1468 0.0298 0.5637 0.026 Uiso 1 1 calc R . .
C19 C 0.1428(4) 0.20358(12) 0.2541(4) 0.0196(8) Uani 1 1 d . . .
C20 C 0.2857(4) 0.20359(13) 0.2549(4) 0.0245(9) Uani 1 1 d . . .
H20 H 0.3164 0.1813 0.2152 0.029 Uiso 1 1 calc R . .
C21 C 0.3834(5) 0.23594(14) 0.3134(5) 0.0311(10) Uani 1 1 d . . .
H21 H 0.4808 0.2357 0.3135 0.037 Uiso 1 1 calc R . .
C22 C 0.3410(5) 0.26862(14) 0.3717(4) 0.0346(11) Uani 1 1 d . . .
H22 H 0.4094 0.2905 0.4127 0.042 Uiso 1 1 calc R . .
C23 C 0.1974(5) 0.26933(13) 0.3701(5) 0.0329(10) Uani 1 1 d . . .
H23 H 0.1666 0.2919 0.4082 0.039 Uiso 1 1 calc R . .
C24 C 0.0997(5) 0.23672(13) 0.3121(5) 0.0297(10) Uani 1 1 d . . .
H24 H 0.0023 0.2370 0.3121 0.036 Uiso 1 1 calc R . .
C25 C -0.1189(4) 0.15942(11) 0.2483(4) 0.0199(8) Uani 1 1 d . . .
C26 C -0.0685(5) 0.16399(13) 0.4003(4) 0.0253(9) Uani 1 1 d . . .
H26 H 0.0361 0.1697 0.4616 0.030 Uiso 1 1 calc R . .
C27 C -0.1666(5) 0.16043(13) 0.4632(5) 0.0263(9) Uani 1 1 d . . .
H27 H -0.1296 0.1630 0.5676 0.032 Uiso 1 1 calc R . .
C28 C -0.3198(5) 0.15302(13) 0.3751(5) 0.0291(10) Uani 1 1 d . . .
H28 H -0.3878 0.1510 0.4193 0.035 Uiso 1 1 calc R . .
C29 C -0.3750(5) 0.14850(12) 0.2238(5) 0.0266(9) Uani 1 1 d . . .
H29 H -0.4802 0.1432 0.1638 0.032 Uiso 1 1 calc R . .
C30 C -0.2750(5) 0.15183(12) 0.1602(4) 0.0225(8) Uani 1 1 d . . .
H30 H -0.3124 0.1489 0.0560 0.027 Uiso 1 1 calc R . .
C31 C -0.1176(4) 0.18317(11) -0.0209(4) 0.0200(8) Uani 1 1 d . . .
C32 C -0.1967(5) 0.15625(13) -0.1344(4) 0.0264(9) Uani 1 1 d . . .
H32 H -0.1753 0.1283 -0.1195 0.032 Uiso 1 1 calc R . .
C33 C -0.3077(5) 0.17011(14) -0.2707(4) 0.0314(10) Uani 1 1 d . . .
H33 H -0.3641 0.1516 -0.3475 0.038 Uiso 1 1 calc R . .
C34 C -0.3350(5) 0.21074(14) -0.2931(5) 0.0304(10) Uani 1 1 d . . .
H34 H -0.4096 0.2201 -0.3863 0.036 Uiso 1 1 calc R . .
C35 C -0.2565(5) 0.23762(13) -0.1835(5) 0.0298(10) Uani 1 1 d . . .
H35 H -0.2759 0.2656 -0.2007 0.036 Uiso 1 1 calc R . .
C36 C -0.1473(4) 0.22404(12) -0.0455(5) 0.0238(9) Uani 1 1 d . . .
H36 H -0.0934 0.2427 0.0314 0.029 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'
P P 0.1023 0.0942 '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'
F F 0.0171 0.0103 '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
F1 Pt F2 84.81(9) . . ?
F1 Pt P1 91.05(7) . . ?
F2 Pt P1 175.74(7) . . ?
F1 Pt P2 169.92(7) . . ?
F2 Pt P2 85.27(7) . . ?
P1 Pt P2 98.89(3) . . ?
C1 P1 C7 104.31(17) . . ?
C1 P1 C13 102.26(16) . . ?
C7 P1 C13 107.52(16) . . ?
C1 P1 Pt 112.72(12) . . ?
C7 P1 Pt 113.66(12) . . ?
C13 P1 Pt 115.21(13) . . ?
C19 P2 C31 104.66(18) . . ?
C19 P2 C25 106.09(18) . . ?
C31 P2 C25 100.87(17) . . ?
C19 P2 Pt 112.51(13) . . ?
C31 P2 Pt 108.85(12) . . ?
C25 P2 Pt 122.03(13) . . ?
C2 C1 C6 119.5(4) . . ?
C2 C1 P1 118.0(3) . . ?
C6 C1 P1 122.5(3) . . ?
C1 C2 C3 120.1(4) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 H2 120.0 . . ?
C4 C3 C2 120.3(4) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 120.4(4) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C4 C5 C6 120.3(4) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C1 119.5(4) . . ?
C5 C6 H6 120.3 . . ?
C1 C6 H6 120.3 . . ?
C8 C7 C12 119.5(3) . . ?
C8 C7 P1 124.2(3) . . ?
C12 C7 P1 116.3(3) . . ?
C9 C8 C7 119.8(3) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C8 C9 C10 121.1(4) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 H9 119.5 . . ?
C9 C10 C11 118.6(4) . . ?
C9 C10 H10 120.7 . . ?
C11 C10 H10 120.7 . . ?
C12 C11 C10 121.1(4) . . ?
C12 C11 H11 119.4 . . ?
C10 C11 H11 119.4 . . ?
C11 C12 C7 119.9(3) . . ?
C11 C12 H12 120.0 . . ?
C7 C12 H12 120.0 . . ?
C14 C13 C18 118.7(3) . . ?
C14 C13 P1 120.8(3) . . ?
C18 C13 P1 120.5(3) . . ?
C13 C14 C15 120.6(4) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
C14 C15 C16 120.3(4) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C17 C16 C15 119.5(4) . . ?
C17 C16 H16 120.3 . . ?
C15 C16 H16 120.3 . . ?
C16 C17 C18 120.8(4) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
C17 C18 C13 120.0(4) . . ?
C17 C18 H18 120.0 . . ?
C13 C18 H18 120.0 . . ?
C20 C19 C24 118.9(4) . . ?
C20 C19 P2 118.8(3) . . ?
C24 C19 P2 122.0(3) . . ?
C21 C20 C19 120.2(4) . . ?
C21 C20 H20 119.9 . . ?
C19 C20 H20 119.9 . . ?
C20 C21 C22 120.9(4) . . ?
C20 C21 H21 119.6 . . ?
C22 C21 H21 119.6 . . ?
C21 C22 C23 119.7(4) . . ?
C21 C22 H22 120.1 . . ?
C23 C22 H22 120.1 . . ?
C24 C23 C22 119.4(4) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
C23 C24 C19 120.9(4) . . ?
C23 C24 H24 119.5 . . ?
C19 C24 H24 119.5 . . ?
C26 C25 C30 118.0(4) . . ?
C26 C25 P2 122.5(3) . . ?
C30 C25 P2 119.5(3) . . ?
C27 C26 C25 121.2(4) . . ?
C27 C26 H26 119.4 . . ?
C25 C26 H26 119.4 . . ?
C26 C27 C28 120.0(4) . . ?
C26 C27 H27 120.0 . . ?
C28 C27 H27 120.0 . . ?
C27 C28 C29 120.7(4) . . ?
C27 C28 H28 119.6 . . ?
C29 C28 H28 119.6 . . ?
C28 C29 C30 119.2(4) . . ?
C28 C29 H29 120.4 . . ?
C30 C29 H29 120.4 . . ?
C29 C30 C25 120.8(4) . . ?
C29 C30 H30 119.6 . . ?
C25 C30 H30 119.6 . . ?
C36 C31 C32 119.4(4) . . ?
C36 C31 P2 122.6(3) . . ?
C32 C31 P2 117.8(3) . . ?
C31 C32 C33 120.1(4) . . ?
C31 C32 H32 119.9 . . ?
C33 C32 H32 119.9 . . ?
C34 C33 C32 119.7(4) . . ?
C34 C33 H33 120.2 . . ?
C32 C33 H33 120.2 . . ?
C35 C34 C33 120.9(4) . . ?
C35 C34 H34 119.6 . . ?
C33 C34 H34 119.6 . . ?
C34 C35 C36 120.0(4) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C31 C36 C35 120.0(4) . . ?
C31 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
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
Pt F1 1.999(2) . ?
Pt F2 2.016(2) . ?
Pt P1 2.2198(9) . ?
Pt P2 2.2304(10) . ?
P1 C1 1.818(4) . ?
P1 C7 1.824(4) . ?
P1 C13 1.826(4) . ?
P2 C19 1.825(4) . ?
P2 C31 1.827(4) . ?
P2 C25 1.836(4) . ?
C1 C2 1.390(5) . ?
C1 C6 1.407(5) . ?
C2 C3 1.392(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.374(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.390(5) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.392(5) . ?
C7 C12 1.397(5) . ?
C8 C9 1.388(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.389(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.391(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.380(5) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.388(5) . ?
C13 C18 1.407(5) . ?
C14 C15 1.391(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.388(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.379(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.385(6) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.391(5) . ?
C19 C24 1.397(5) . ?
C20 C21 1.386(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.383(7) . ?
C21 H21 0.9500 . ?
C22 C23 1.394(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.392(6) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.391(5) . ?
C25 C30 1.406(5) . ?
C26 C27 1.366(5) . ?
C26 H26 0.9500 . ?
C27 C28 1.383(6) . ?
C27 H27 0.9500 . ?
C28 C29 1.379(6) . ?
C28 H28 0.9500 . ?
C29 C30 1.387(5) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C36 1.390(5) . ?
C31 C32 1.386(6) . ?
C32 C33 1.397(6) . ?
C32 H32 0.9500 . ?
C33 C34 1.378(6) . ?
C33 H33 0.9500 . ?
C34 C35 1.363(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.399(6) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
