#------------------------------------------------------------------------------
#$Date: 2016-03-21 14:17:58 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178713 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/24/4082495.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_4082495
loop_
_publ_author_name
'Lister, Julia M.'
'Carreira, Monica'
'Haddow, Mairi F.'
'Hamilton, Alex'
'McMullin, Claire L.'
'Orpen, A. Guy'
'Pringle, Paul G.'
'Stennett, Tom E.'
_publ_section_title
;
 Unexpectedly High Barriers to M--P Rotation in Tertiary Phobane
 Complexes: PhobPR Behavior That Is Commensurate withtBu2PR
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              702
_journal_paper_doi               10.1021/om400980e
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C24 H46 Cl2 P2 Pt'
_chemical_formula_sum            'C24 H46 Cl2 P2 Pt'
_chemical_formula_weight         662.54
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.787(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.1637(6)
_cell_length_b                   7.8841(6)
_cell_length_c                   20.4032(17)
_cell_measurement_reflns_used    5423
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.48
_cell_measurement_theta_min      2.74
_cell_volume                     1311.67(18)
_computing_cell_refinement       'Apex II (Bruker-AXS, 2007)'
_computing_data_collection       'Apex II (Bruker-AXS, 2007)'
_computing_data_reduction
; 
 SAINT v7.34A (Bruker-AXS, 2007) & XPREP v2005/4 (Bruker-AXS, 2005) 
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.896
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0652
_diffrn_reflns_av_sigmaI/netI    0.0726
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            23807
_diffrn_reflns_theta_full        34.51
_diffrn_reflns_theta_max         34.51
_diffrn_reflns_theta_min         4.61
_exptl_absorpt_coefficient_mu    5.684
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_correction_T_min  0.4676
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs - bruker 2008'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.261
_refine_diff_density_min         -1.975
_refine_diff_density_rms         0.231
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.236
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         4981
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.236
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0034P)²+15.1361P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1166
_reflns_number_gt                3501
_reflns_number_total             4981
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400980e_si_002.cif
_cod_data_source_block           2a
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4082495
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Pt1 Pt 0.0000 0.5000 0.0000 0.01491(8) Uani 1 2 d S . .
P1 P 0.1980(2) 0.3055(2) 0.03355(9) 0.0166(3) Uani 1 1 d . . .
Cl1 Cl -0.1989(2) 0.2922(2) 0.00684(10) 0.0253(4) Uani 1 1 d . . .
C1 C 0.1496(8) 0.1359(9) 0.0910(4) 0.0237(14) Uani 1 1 d . C .
H1 H 0.0829 0.0477 0.0668 0.028 Uiso 1 1 calc R . .
C2 C 0.3188(9) 0.0599(9) 0.1110(4) 0.0275(16) Uani 1 1 d . . .
H2A H 0.3428 -0.0354 0.0814 0.033 Uiso 1 1 calc R . .
H2B H 0.3174 0.0151 0.1563 0.033 Uiso 1 1 calc R . .
C3 C 0.4554(9) 0.1974(10) 0.1073(4) 0.0294(16) Uani 1 1 d . . .
H3A H 0.5085 0.2144 0.1515 0.035 Uiso 1 1 calc R . .
H3B H 0.5401 0.1577 0.0778 0.035 Uiso 1 1 calc R . .
C11 C 0.2831(9) 0.1640(9) -0.1610(4) 0.0251(15) Uani 1 1 d . . .
H11A H 0.2638 0.0407 -0.1564 0.030 Uiso 1 1 calc R . .
H11B H 0.4031 0.1823 -0.1612 0.030 Uiso 1 1 calc R . .
C4 C 0.3835(8) 0.3683(9) 0.0816(4) 0.0243(15) Uani 1 1 d D C .
H4 H 0.443(9) 0.411(10) 0.046(3) 0.029 Uiso 1 1 d D . .
C9 C 0.2781(10) 0.1918(10) -0.0365(4) 0.0304(16) Uani 1 1 d . . .
H9A H 0.3993 0.2000 -0.0339 0.036 Uiso 1 1 calc R . .
H9B H 0.2490 0.0704 -0.0329 0.036 Uiso 1 1 calc R . .
C5 C 0.3534(10) 0.4974(15) 0.1360(4) 0.0419(18) Uani 1 1 d . . .
H5A H 0.4423 0.4835 0.1704 0.050 Uiso 1 1 calc R A 1
H5B H 0.3655 0.6121 0.1172 0.050 Uiso 1 1 calc R A 1
C10 C 0.2166(11) 0.2552(10) -0.1022(4) 0.0329(18) Uani 1 1 d . . .
H10A H 0.2444 0.3770 -0.1054 0.039 Uiso 1 1 calc R . .
H10B H 0.0955 0.2458 -0.1048 0.039 Uiso 1 1 calc R . .
C8 C 0.0541(10) 0.1970(12) 0.1501(4) 0.0365(19) Uani 1 1 d . . .
H8A H 0.0203 0.0966 0.1752 0.044 Uiso 1 1 calc R B 1
H8B H -0.0469 0.2553 0.1333 0.044 Uiso 1 1 calc R B 1
C12 C 0.2047(12) 0.2241(12) -0.2262(5) 0.044(2) Uani 1 1 d . . .
H12A H 0.0863 0.2034 -0.2268 0.065 Uiso 1 1 calc R . .
H12B H 0.2524 0.1619 -0.2622 0.065 Uiso 1 1 calc R . .
H12C H 0.2250 0.3458 -0.2314 0.065 Uiso 1 1 calc R . .
C6A C 0.1918(18) 0.493(2) 0.1696(6) 0.044(5) Uani 0.64(2) 1 d P C 1
H6A1 H 0.1943 0.5798 0.2047 0.053 Uiso 0.64(2) 1 calc PR C 1
H6A2 H 0.1023 0.5234 0.1372 0.053 Uiso 0.64(2) 1 calc PR C 1
C7A C 0.1543(19) 0.323(2) 0.1990(7) 0.042(4) Uani 0.64(2) 1 d P C 1
H7A1 H 0.0902 0.3411 0.2384 0.050 Uiso 0.64(2) 1 calc PR C 1
H7A2 H 0.2589 0.2679 0.2135 0.050 Uiso 0.64(2) 1 calc PR C 1
C6B C 0.262(4) 0.411(3) 0.1950(12) 0.037(7) Uani 0.36(2) 1 d P C 2
H6B1 H 0.3184 0.3043 0.2076 0.045 Uiso 0.36(2) 1 calc PR C 2
H6B2 H 0.2683 0.4878 0.2334 0.045 Uiso 0.36(2) 1 calc PR C 2
C7B C 0.081(4) 0.372(3) 0.1770(14) 0.037(7) Uani 0.36(2) 1 d P C 2
H7B1 H 0.0164 0.3857 0.2166 0.044 Uiso 0.36(2) 1 calc PR C 2
H7B2 H 0.0388 0.4559 0.1441 0.044 Uiso 0.36(2) 1 calc PR C 2
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'
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
P1 Pt1 P1 180.0 . 3_565
P1 Pt1 Cl1 90.29(6) . 3_565
P1 Pt1 Cl1 89.71(6) 3_565 3_565
P1 Pt1 Cl1 89.71(6) . .
P1 Pt1 Cl1 90.29(6) 3_565 .
Cl1 Pt1 Cl1 180.0 3_565 .
C4 P1 C1 93.1(3) . .
C4 P1 C9 103.4(4) . .
C1 P1 C9 103.8(4) . .
C4 P1 Pt1 121.9(2) . .
C1 P1 Pt1 120.3(2) . .
C9 P1 Pt1 111.4(2) . .
C2 C1 C8 113.2(6) . .
C2 C1 P1 103.6(5) . .
C8 C1 P1 113.8(5) . .
C2 C1 H1 108.7 . .
C8 C1 H1 108.7 . .
P1 C1 H1 108.7 . .
C1 C2 C3 110.5(6) . .
C1 C2 H2A 109.6 . .
C3 C2 H2A 109.6 . .
C1 C2 H2B 109.6 . .
C3 C2 H2B 109.6 . .
H2A C2 H2B 108.1 . .
C4 C3 C2 111.1(5) . .
C4 C3 H3A 109.4 . .
C2 C3 H3A 109.4 . .
C4 C3 H3B 109.4 . .
C2 C3 H3B 109.4 . .
H3A C3 H3B 108.0 . .
C10 C11 C12 113.0(6) . .
C10 C11 H11A 109.0 . .
C12 C11 H11A 109.0 . .
C10 C11 H11B 109.0 . .
C12 C11 H11B 109.0 . .
H11A C11 H11B 107.8 . .
C5 C4 C3 113.7(7) . .
C5 C4 P1 114.2(5) . .
C3 C4 P1 103.6(5) . .
C5 C4 H4 115(5) . .
C3 C4 H4 111(5) . .
P1 C4 H4 98(5) . .
C10 C9 P1 114.8(5) . .
C10 C9 H9A 108.6 . .
P1 C9 H9A 108.6 . .
C10 C9 H9B 108.6 . .
P1 C9 H9B 108.6 . .
H9A C9 H9B 107.6 . .
C6A C5 C4 119.0(9) . .
C4 C5 C6B 111.1(11) . .
C6A C5 H5A 107.6 . .
C4 C5 H5A 107.6 . .
C6B C5 H5A 77.0 . .
C6A C5 H5B 107.6 . .
C4 C5 H5B 107.6 . .
C6B C5 H5B 137.8 . .
H5A C5 H5B 107.0 . .
C9 C10 C11 115.6(6) . .
C9 C10 H10A 108.4 . .
C11 C10 H10A 108.4 . .
C9 C10 H10B 108.4 . .
C11 C10 H10B 108.4 . .
H10A C10 H10B 107.4 . .
C7B C8 C1 120.3(12) . .
C1 C8 C7A 114.7(8) . .
C7B C8 H8A 125.9 . .
C1 C8 H8A 108.6 . .
C7A C8 H8A 108.6 . .
C7B C8 H8B 78.6 . .
C1 C8 H8B 108.6 . .
C7A C8 H8B 108.6 . .
H8A C8 H8B 107.6 . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C7A C6A C5 113.5(11) . .
C7A C6A H6A1 108.9 . .
C5 C6A H6A1 108.9 . .
C7A C6A H6A2 108.9 . .
C5 C6A H6A2 108.9 . .
H6A1 C6A H6A2 107.7 . .
C6A C7A C8 114.2(11) . .
C6A C7A H7A1 108.7 . .
C8 C7A H7A1 108.7 . .
C6A C7A H7A2 108.7 . .
C8 C7A H7A2 108.7 . .
H7A1 C7A H7A2 107.6 . .
C7B C6B C5 112.7(19) . .
C7B C6B H6B1 109.0 . .
C5 C6B H6B1 109.0 . .
C7B C6B H6B2 109.0 . .
C5 C6B H6B2 109.0 . .
H6B1 C6B H6B2 107.8 . .
C8 C7B C6B 113(2) . .
C8 C7B H7B1 109.0 . .
C6B C7B H7B1 109.0 . .
C8 C7B H7B2 109.0 . .
C6B C7B H7B2 109.0 . .
H7B1 C7B H7B2 107.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 P1 2.3079(16) .
Pt1 P1 2.3079(16) 3_565
Pt1 Cl1 2.3155(16) 3_565
Pt1 Cl1 2.3155(16) .
P1 C4 1.832(7) .
P1 C1 1.834(7) .
P1 C9 1.835(8) .
C1 C2 1.543(9) .
C1 C8 1.544(11) .
C1 H1 1.0000 .
C2 C3 1.559(11) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.551(10) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C11 C10 1.521(10) .
C11 C12 1.523(11) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C4 C5 1.535(12) .
C4 H4 0.95(2) .
C9 C10 1.494(11) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C5 C6A 1.516(17) .
C5 C6B 1.60(3) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C8 C7B 1.50(3) .
C8 C7A 1.604(19) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C6A C7A 1.51(3) .
C6A H6A1 0.9900 .
C6A H6A2 0.9900 .
C7A H7A1 0.9900 .
C7A H7A2 0.9900 .
C6B C7B 1.54(4) .
C6B H6B1 0.9900 .
C6B H6B2 0.9900 .
C7B H7B1 0.9900 .
C7B H7B2 0.9900 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
Cl1 Pt1 P1 C4 31.3(3) 3_565
Cl1 Pt1 P1 C4 -148.7(3) .
Cl1 Pt1 P1 C1 147.1(3) 3_565
Cl1 Pt1 P1 C1 -32.9(3) .
Cl1 Pt1 P1 C9 -91.2(3) 3_565
Cl1 Pt1 P1 C9 88.8(3) .
C4 P1 C1 C2 -38.9(5) .
C9 P1 C1 C2 65.7(6) .
Pt1 P1 C1 C2 -168.9(4) .
C4 P1 C1 C8 84.5(6) .
C9 P1 C1 C8 -170.9(6) .
Pt1 P1 C1 C8 -45.6(6) .
C8 C1 C2 C3 -94.8(8) .
P1 C1 C2 C3 29.0(7) .
C1 C2 C3 C4 -2.6(9) .
C2 C3 C4 C5 99.5(8) .
C2 C3 C4 P1 -25.0(8) .
C1 P1 C4 C5 -87.0(6) .
C9 P1 C4 C5 168.1(6) .
Pt1 P1 C4 C5 41.9(7) .
C1 P1 C4 C3 37.3(5) .
C9 P1 C4 C3 -67.7(6) .
Pt1 P1 C4 C3 166.2(4) .
C4 P1 C9 C10 -126.5(6) .
C1 P1 C9 C10 136.9(6) .
Pt1 P1 C9 C10 6.1(7) .
C3 C4 C5 C6A -86.8(11) .
P1 C4 C5 C6A 31.8(12) .
C3 C4 C5 C6B -46.8(13) .
P1 C4 C5 C6B 71.8(13) .
P1 C9 C10 C11 179.3(6) .
C12 C11 C10 C9 175.0(8) .
C2 C1 C8 C7B 86.4(16) .
P1 C1 C8 C7B -31.5(16) .
C2 C1 C8 C7A 52.2(11) .
P1 C1 C8 C7A -65.8(10) .
C4 C5 C6A C7A 55.7(13) .
C6B C5 C6A C7A -31.2(17) .
C5 C6A C7A C8 -89.9(13) .
C7B C8 C7A C6A -41(2) .
C1 C8 C7A C6A 66.9(13) .
C6A C5 C6B C7B 38.1(17) .
C4 C5 C6B C7B -72.6(19) .
C1 C8 C7B C6B -54(2) .
C7A C8 C7B C6B 33.8(19) .
C5 C6B C7B C8 92(2) .
