#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:43:47 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179125 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/87/4308754.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_4308754
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            'C48 H40 F2 P2 Pt'
_chemical_formula_weight         911.83
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 102.0220(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.5030(3)
_cell_length_b                   9.85000(10)
_cell_length_c                   19.2560(3)
_cell_measurement_reflns_used    4288
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.86
_cell_measurement_theta_min      2.45
_cell_volume                     3803.55(9)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. Phi 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  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14018
_diffrn_reflns_theta_full        27.86
_diffrn_reflns_theta_max         27.86
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    3.817
_exptl_absorpt_correction_T_max  0.5982
_exptl_absorpt_correction_T_min  0.5156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.359
_refine_diff_density_min         -1.436
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         4509
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0230
_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)+(0.0311P)²+6.4988P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0578
_refine_ls_wR_factor_ref         0.0588
_reflns_number_gt                4288
_reflns_number_total             4509
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0488177si20040826_033018.cif
_cod_data_source_block           ar3
_cod_database_code               4308754
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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 0.5000 0.391788(12) 0.2500 0.01353(5) Uani 1 2 d S . .
P1 P 0.40650(3) 0.40983(6) 0.15331(3) 0.01397(13) Uani 1 1 d . . .
F1 F 0.44658(7) 0.53953(15) 0.29261(7) 0.0183(3) Uani 1 1 d . . .
C1 C 0.44950(12) 0.2523(3) 0.29675(13) 0.0160(5) Uani 1 1 d . . .
C2 C 0.43000(13) 0.2872(3) 0.36013(13) 0.0199(5) Uani 1 1 d . . .
H2 H 0.4438 0.3716 0.3823 0.024 Uiso 1 1 calc R . .
C3 C 0.39051(13) 0.1994(3) 0.39101(14) 0.0246(6) Uani 1 1 d . . .
H3 H 0.3779 0.2244 0.4340 0.030 Uiso 1 1 calc R . .
C4 C 0.36974(14) 0.0762(3) 0.35921(16) 0.0278(6) Uani 1 1 d . . .
H4 H 0.3420 0.0177 0.3795 0.033 Uiso 1 1 calc R . .
C5 C 0.38987(14) 0.0395(3) 0.29759(15) 0.0256(6) Uani 1 1 d . . .
H5 H 0.3768 -0.0460 0.2763 0.031 Uiso 1 1 calc R . .
C6 C 0.42889(14) 0.1258(3) 0.26660(14) 0.0199(5) Uani 1 1 d . . .
H6 H 0.4419 0.0988 0.2241 0.024 Uiso 1 1 calc R . .
C7 C 0.32928(12) 0.3348(2) 0.16779(13) 0.0174(5) Uani 1 1 d . . .
C8 C 0.28995(13) 0.2476(3) 0.11910(16) 0.0259(6) Uani 1 1 d . . .
H8 H 0.3031 0.2248 0.0761 0.031 Uiso 1 1 calc R . .
C9 C 0.23152(15) 0.1942(3) 0.13366(19) 0.0350(7) Uani 1 1 d . . .
H9 H 0.2049 0.1347 0.1005 0.042 Uiso 1 1 calc R . .
C10 C 0.21182(14) 0.2272(3) 0.19612(18) 0.0336(7) Uani 1 1 d . . .
H10 H 0.1722 0.1891 0.2062 0.040 Uiso 1 1 calc R . .
C11 C 0.24979(14) 0.3154(3) 0.24376(16) 0.0293(6) Uani 1 1 d . . .
H11 H 0.2358 0.3388 0.2863 0.035 Uiso 1 1 calc R . .
C12 C 0.30853(14) 0.3704(3) 0.23004(15) 0.0217(5) Uani 1 1 d . . .
H12 H 0.3343 0.4318 0.2628 0.026 Uiso 1 1 calc R . .
C13 C 0.41890(12) 0.3367(3) 0.07067(12) 0.0164(5) Uani 1 1 d . . .
C14 C 0.42555(12) 0.1957(3) 0.06691(13) 0.0195(5) Uani 1 1 d . . .
H14 H 0.4229 0.1413 0.1070 0.023 Uiso 1 1 calc R . .
C15 C 0.43604(14) 0.1345(3) 0.00530(15) 0.0222(5) Uani 1 1 d . . .
H15 H 0.4391 0.0385 0.0027 0.027 Uiso 1 1 calc R . .
C16 C 0.44197(14) 0.2140(3) -0.05242(14) 0.0246(6) Uani 1 1 d . . .
H16 H 0.4497 0.1723 -0.0945 0.030 Uiso 1 1 calc R . .
C17 C 0.43667(14) 0.3538(3) -0.04917(14) 0.0243(5) Uani 1 1 d . . .
H17 H 0.4411 0.4077 -0.0888 0.029 Uiso 1 1 calc R . .
C18 C 0.42481(13) 0.4159(3) 0.01219(14) 0.0193(5) Uani 1 1 d . . .
H18 H 0.4208 0.5118 0.0141 0.023 Uiso 1 1 calc R . .
C19 C 0.38358(13) 0.5876(3) 0.13392(14) 0.0177(5) Uani 1 1 d . . .
C20 C 0.31763(15) 0.6195(3) 0.10226(16) 0.0242(6) Uani 1 1 d . . .
H20 H 0.2853 0.5494 0.0915 0.029 Uiso 1 1 calc R . .
C21 C 0.29918(15) 0.7538(3) 0.08653(15) 0.0282(6) Uani 1 1 d . . .
H21 H 0.2542 0.7751 0.0655 0.034 Uiso 1 1 calc R . .
C22 C 0.34587(16) 0.8561(3) 0.10135(16) 0.0287(6) Uani 1 1 d . . .
H22 H 0.3334 0.9476 0.0899 0.034 Uiso 1 1 calc R . .
C23 C 0.41140(15) 0.8245(3) 0.13313(16) 0.0278(6) Uani 1 1 d . . .
H23 H 0.4435 0.8951 0.1436 0.033 Uiso 1 1 calc R . .
C24 C 0.43067(13) 0.6913(3) 0.14982(14) 0.0225(5) Uani 1 1 d . . .
H24 H 0.4755 0.6710 0.1719 0.027 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
C1 Pt C1 95.30(14) 2_655 . ?
C1 Pt F1 86.56(9) 2_655 2_655 ?
C1 Pt F1 176.94(7) . 2_655 ?
C1 Pt F1 176.95(7) 2_655 . ?
C1 Pt F1 86.56(9) . . ?
F1 Pt F1 91.70(8) 2_655 . ?
C1 Pt P1 96.03(7) 2_655 . ?
C1 Pt P1 89.73(7) . . ?
F1 Pt P1 92.49(4) 2_655 . ?
F1 Pt P1 81.53(4) . . ?
C1 Pt P1 89.73(7) 2_655 2_655 ?
C1 Pt P1 96.03(7) . 2_655 ?
F1 Pt P1 81.53(4) 2_655 2_655 ?
F1 Pt P1 92.49(4) . 2_655 ?
P1 Pt P1 171.45(3) . 2_655 ?
C13 P1 C7 104.99(11) . . ?
C13 P1 C19 106.15(12) . . ?
C7 P1 C19 103.00(12) . . ?
C13 P1 Pt 114.76(8) . . ?
C7 P1 Pt 115.70(8) . . ?
C19 P1 Pt 111.15(9) . . ?
C6 C1 C2 117.5(2) . . ?
C6 C1 Pt 123.57(19) . . ?
C2 C1 Pt 118.79(18) . . ?
C3 C2 C1 120.9(2) . . ?
C3 C2 H2 119.6 . . ?
C1 C2 H2 119.6 . . ?
C4 C3 C2 120.4(3) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C5 C4 C3 119.3(3) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C4 C5 C6 120.7(3) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C1 121.2(3) . . ?
C5 C6 H6 119.4 . . ?
C1 C6 H6 119.4 . . ?
C8 C7 C12 119.6(2) . . ?
C8 C7 P1 123.1(2) . . ?
C12 C7 P1 117.3(2) . . ?
C9 C8 C7 119.9(3) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C10 C9 C8 120.4(3) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C11 C10 C9 119.9(3) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C10 C11 C12 120.6(3) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C11 C12 C7 119.6(3) . . ?
C11 C12 H12 120.2 . . ?
C7 C12 H12 120.2 . . ?
C18 C13 C14 119.2(2) . . ?
C18 C13 P1 122.54(19) . . ?
C14 C13 P1 118.24(18) . . ?
C15 C14 C13 120.7(2) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C16 C15 C14 119.7(3) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C17 C16 C15 120.4(2) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C16 C17 C18 120.2(3) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C13 C18 C17 119.9(2) . . ?
C13 C18 H18 120.1 . . ?
C17 C18 H18 120.1 . . ?
C24 C19 C20 119.6(2) . . ?
C24 C19 P1 121.3(2) . . ?
C20 C19 P1 119.2(2) . . ?
C21 C20 C19 120.2(3) . . ?
C21 C20 H20 119.9 . . ?
C19 C20 H20 119.9 . . ?
C22 C21 C20 120.3(3) . . ?
C22 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C21 C22 C23 119.5(3) . . ?
C21 C22 H22 120.2 . . ?
C23 C22 H22 120.2 . . ?
C24 C23 C22 121.1(3) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
C23 C24 C19 119.4(3) . . ?
C23 C24 H24 120.3 . . ?
C19 C24 H24 120.3 . . ?
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
Pt C1 2.039(2) 2_655 ?
Pt C1 2.039(2) . ?
Pt F1 2.0892(14) 2_655 ?
Pt F1 2.0892(14) . ?
Pt P1 2.3846(6) . ?
Pt P1 2.3847(7) 2_655 ?
P1 C13 1.812(2) . ?
P1 C7 1.820(3) . ?
P1 C19 1.831(3) . ?
C1 C6 1.402(4) . ?
C1 C2 1.404(3) . ?
C2 C3 1.399(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.385(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.383(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.385(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.397(4) . ?
C7 C12 1.398(4) . ?
C8 C9 1.389(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.385(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.380(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.395(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C18 1.396(4) . ?
C13 C14 1.399(3) . ?
C14 C15 1.387(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.386(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.384(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.396(4) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C24 1.395(4) . ?
C19 C20 1.398(4) . ?
C20 C21 1.392(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.378(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.391(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.388(4) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
