#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/78/2217813.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2217813
loop_
_publ_author_name
'Gunay, Ahmet'
'Brennessel, William W.'
'Jones, William D.'
_publ_section_title
;
 A second polymorph of
 [1,2-bis(di-tert-butylphosphino)ethane]dichloridoplatinum(II)
;
_journal_coeditor_code           PV2062
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m454
_journal_paper_doi               10.1107/S1600536808000603
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Pt Cl2 (C18 H40 P2)]'
_chemical_formula_moiety         'C18 H40 Cl2 P2 Pt'
_chemical_formula_sum            'C18 H40 Cl2 P2 Pt'
_chemical_formula_weight         584.43
_chemical_name_systematic
;
[1,2-bis(di-tert-butylphosphino)ethane]dichloridoplatinum(II)
;
_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                 109.2870(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0981(10)
_cell_length_b                   15.3242(13)
_cell_length_c                   14.5413(13)
_cell_measurement_reflns_used    4040
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.85
_cell_measurement_theta_min      2.97
_cell_volume                     2334.2(4)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al.,  1999)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_diffrn_measurement_method       'area detector, ω scans per φ'
_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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20415
_diffrn_reflns_theta_full        32.03
_diffrn_reflns_theta_max         32.03
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    6.376
_exptl_absorpt_correction_T_max  0.5995
_exptl_absorpt_correction_T_min  0.3420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.107
_refine_diff_density_min         -0.806
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         8022
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0291
_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)+(0.0232P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0598
_reflns_number_gt                6312
_reflns_number_total             8022
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            pv2062.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2217813
_cod_database_fobs_code          2217813
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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Pt Pt1 0.268368(10) 0.706474(7) 0.781256(8) 0.01505(3) Uani d . 1
Cl Cl1 0.17379(7) 0.80168(5) 0.86681(6) 0.02422(16) Uani d . 1
Cl Cl2 0.44219(8) 0.80401(5) 0.81687(6) 0.02415(16) Uani d . 1
P P1 0.09956(7) 0.61552(5) 0.74524(5) 0.01603(14) Uani d . 1
P P2 0.36188(7) 0.61746(5) 0.70173(6) 0.01776(15) Uani d . 1
C C1 0.0577(3) 0.5718(2) 0.8529(2) 0.0227(6) Uani d . 1
C C2 -0.0053(4) 0.4814(2) 0.8323(3) 0.0323(8) Uani d . 1
H H2A -0.0253 0.4613 0.8896 0.048 Uiso calc R 1
H H2B 0.0533 0.4400 0.8177 0.048 Uiso calc R 1
H H2C -0.0842 0.4851 0.7763 0.048 Uiso calc R 1
C C3 -0.0326(3) 0.6333(2) 0.8823(3) 0.0287(7) Uani d . 1
H H3A -0.0520 0.6085 0.9380 0.043 Uiso calc R 1
H H3B -0.1120 0.6402 0.8273 0.043 Uiso calc R 1
H H3C 0.0083 0.6903 0.9002 0.043 Uiso calc R 1
C C4 0.1821(3) 0.5634(2) 0.9392(2) 0.0308(8) Uani d . 1
H H4A 0.1632 0.5409 0.9960 0.046 Uiso calc R 1
H H4B 0.2227 0.6208 0.9547 0.046 Uiso calc R 1
H H4C 0.2400 0.5231 0.9221 0.046 Uiso calc R 1
C C5 -0.0478(3) 0.6578(2) 0.6491(2) 0.0232(7) Uani d . 1
C C6 -0.1592(3) 0.5927(2) 0.6247(3) 0.0302(8) Uani d . 1
H H6A -0.2334 0.6177 0.5744 0.045 Uiso calc R 1
H H6B -0.1812 0.5807 0.6834 0.045 Uiso calc R 1
H H6C -0.1342 0.5383 0.6006 0.045 Uiso calc R 1
C C7 -0.0919(3) 0.7459(2) 0.6749(3) 0.0316(8) Uani d . 1
H H7A -0.1686 0.7645 0.6224 0.047 Uiso calc R 1
H H7B -0.0240 0.7891 0.6833 0.047 Uiso calc R 1
H H7C -0.1113 0.7406 0.7357 0.047 Uiso calc R 1
C C8 -0.0127(3) 0.6711(3) 0.5569(3) 0.0388(9) Uani d . 1
H H8A -0.0871 0.6932 0.5046 0.058 Uiso calc R 1
H H8B 0.0143 0.6154 0.5370 0.058 Uiso calc R 1
H H8C 0.0573 0.7133 0.5700 0.058 Uiso calc R 1
C C9 0.5007(3) 0.5527(2) 0.7849(2) 0.0246(7) Uani d . 1
C C10 0.5670(4) 0.4957(2) 0.7285(3) 0.0349(9) Uani d . 1
H H10A 0.6377 0.4637 0.7747 0.052 Uiso calc R 1
H H10B 0.5999 0.5329 0.6874 0.052 Uiso calc R 1
H H10C 0.5053 0.4541 0.6874 0.052 Uiso calc R 1
C C11 0.5985(3) 0.6126(2) 0.8564(3) 0.0340(8) Uani d . 1
H H11A 0.6690 0.5774 0.8984 0.051 Uiso calc R 1
H H11B 0.5573 0.6440 0.8967 0.051 Uiso calc R 1
H H11C 0.6317 0.6546 0.8199 0.051 Uiso calc R 1
C C12 0.4469(3) 0.4907(2) 0.8451(3) 0.0298(8) Uani d . 1
H H12A 0.5166 0.4561 0.8890 0.045 Uiso calc R 1
H H12B 0.3840 0.4516 0.8011 0.045 Uiso calc R 1
H H12C 0.4058 0.5249 0.8834 0.045 Uiso calc R 1
C C13 0.4076(3) 0.6704(2) 0.5996(2) 0.0241(7) Uani d . 1
C C14 0.5394(3) 0.7143(2) 0.6356(3) 0.0292(7) Uani d . 1
H H14A 0.5579 0.7404 0.5802 0.044 Uiso calc R 1
H H14B 0.6046 0.6707 0.6667 0.044 Uiso calc R 1
H H14C 0.5396 0.7600 0.6829 0.044 Uiso calc R 1
C C15 0.4083(4) 0.6035(2) 0.5199(3) 0.0374(9) Uani d . 1
H H15A 0.4322 0.6329 0.4687 0.056 Uiso calc R 1
H H15B 0.3230 0.5780 0.4919 0.056 Uiso calc R 1
H H15C 0.4702 0.5572 0.5489 0.056 Uiso calc R 1
C C16 0.3071(3) 0.7402(2) 0.5518(3) 0.0286(7) Uani d . 1
H H16A 0.3286 0.7684 0.4988 0.043 Uiso calc R 1
H H16B 0.3055 0.7839 0.6006 0.043 Uiso calc R 1
H H16C 0.2229 0.7126 0.5256 0.043 Uiso calc R 1
C C31 0.1465(3) 0.5180(2) 0.6924(2) 0.0216(6) Uani d . 1
H H31A 0.1853 0.4755 0.7452 0.026 Uiso calc R 1
H H31B 0.0690 0.4908 0.6465 0.026 Uiso calc R 1
C C32 0.2411(3) 0.5363(2) 0.6385(2) 0.0211(6) Uani d . 1
H H32A 0.1938 0.5577 0.5721 0.025 Uiso calc R 1
H H32B 0.2842 0.4813 0.6320 0.025 Uiso calc R 1
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_publ_flag
P2 Pt1 P1 89.70(3) y
P2 Pt1 Cl2 90.82(3) y
P1 Pt1 Cl2 178.77(3) y
P2 Pt1 Cl1 178.84(3) y
P1 Pt1 Cl1 91.39(3) y
Cl2 Pt1 Cl1 88.09(3) y
C31 P1 C5 105.46(15) ?
C31 P1 C1 103.85(14) ?
C5 P1 C1 110.23(14) ?
C31 P1 Pt1 105.77(10) ?
C5 P1 Pt1 114.31(11) ?
C1 P1 Pt1 115.98(11) ?
C32 P2 C9 105.70(15) ?
C32 P2 C13 103.69(14) ?
C9 P2 C13 110.56(15) ?
C32 P2 Pt1 106.44(10) ?
C9 P2 Pt1 113.88(11) ?
C13 P2 Pt1 115.45(11) ?
C4 C1 C3 108.6(3) ?
C4 C1 C2 108.2(3) ?
C3 C1 C2 108.1(3) ?
C4 C1 P1 107.8(2) ?
C3 C1 P1 111.9(2) ?
C2 C1 P1 112.1(2) ?
C1 C2 H2A 109.5 ?
C1 C2 H2B 109.5 ?
H2A C2 H2B 109.5 ?
C1 C2 H2C 109.5 ?
H2A C2 H2C 109.5 ?
H2B C2 H2C 109.5 ?
C1 C3 H3A 109.5 ?
C1 C3 H3B 109.5 ?
H3A C3 H3B 109.5 ?
C1 C3 H3C 109.5 ?
H3A C3 H3C 109.5 ?
H3B C3 H3C 109.5 ?
C1 C4 H4A 109.5 ?
C1 C4 H4B 109.5 ?
H4A C4 H4B 109.5 ?
C1 C4 H4C 109.5 ?
H4A C4 H4C 109.5 ?
H4B C4 H4C 109.5 ?
C7 C5 C8 107.0(3) ?
C7 C5 C6 109.4(3) ?
C8 C5 C6 107.7(3) ?
C7 C5 P1 113.1(2) ?
C8 C5 P1 106.7(2) ?
C6 C5 P1 112.6(2) ?
C5 C6 H6A 109.5 ?
C5 C6 H6B 109.5 ?
H6A C6 H6B 109.5 ?
C5 C6 H6C 109.5 ?
H6A C6 H6C 109.5 ?
H6B C6 H6C 109.5 ?
C5 C7 H7A 109.5 ?
C5 C7 H7B 109.5 ?
H7A C7 H7B 109.5 ?
C5 C7 H7C 109.5 ?
H7A C7 H7C 109.5 ?
H7B C7 H7C 109.5 ?
C5 C8 H8A 109.5 ?
C5 C8 H8B 109.5 ?
H8A C8 H8B 109.5 ?
C5 C8 H8C 109.5 ?
H8A C8 H8C 109.5 ?
H8B C8 H8C 109.5 ?
C11 C9 C10 110.2(3) ?
C11 C9 C12 107.7(3) ?
C10 C9 C12 107.1(3) ?
C11 C9 P2 111.3(2) ?
C10 C9 P2 112.8(2) ?
C12 C9 P2 107.4(2) ?
C9 C10 H10A 109.5 ?
C9 C10 H10B 109.5 ?
H10A C10 H10B 109.5 ?
C9 C10 H10C 109.5 ?
H10A C10 H10C 109.5 ?
H10B C10 H10C 109.5 ?
C9 C11 H11A 109.5 ?
C9 C11 H11B 109.5 ?
H11A C11 H11B 109.5 ?
C9 C11 H11C 109.5 ?
H11A C11 H11C 109.5 ?
H11B C11 H11C 109.5 ?
C9 C12 H12A 109.5 ?
C9 C12 H12B 109.5 ?
H12A C12 H12B 109.5 ?
C9 C12 H12C 109.5 ?
H12A C12 H12C 109.5 ?
H12B C12 H12C 109.5 ?
C16 C13 C14 108.5(3) ?
C16 C13 C15 107.8(3) ?
C14 C13 C15 107.8(3) ?
C16 C13 P2 107.9(2) ?
C14 C13 P2 113.0(2) ?
C15 C13 P2 111.7(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 109.5 ?
C13 C16 H16B 109.5 ?
H16A C16 H16B 109.5 ?
C13 C16 H16C 109.5 ?
H16A C16 H16C 109.5 ?
H16B C16 H16C 109.5 ?
C32 C31 P1 113.8(2) ?
C32 C31 H31A 108.8 ?
P1 C31 H31A 108.8 ?
C32 C31 H31B 108.8 ?
P1 C31 H31B 108.8 ?
H31A C31 H31B 107.7 ?
C31 C32 P2 112.3(2) ?
C31 C32 H32A 109.2 ?
P2 C32 H32A 109.2 ?
C31 C32 H32B 109.2 ?
P2 C32 H32B 109.2 ?
H32A C32 H32B 107.9 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Pt1 P2 2.2513(8) y
Pt1 P1 2.2536(8) y
Pt1 Cl2 2.3588(8) y
Pt1 Cl1 2.3750(8) y
P1 C31 1.833(3) ?
P1 C5 1.881(3) ?
P1 C1 1.897(3) ?
P2 C32 1.837(3) ?
P2 C9 1.895(3) ?
P2 C13 1.903(3) ?
C1 C4 1.534(5) ?
C1 C3 1.535(4) ?
C1 C2 1.537(5) ?
C2 H2A 0.9800 ?
C2 H2B 0.9800 ?
C2 H2C 0.9800 ?
C3 H3A 0.9800 ?
C3 H3B 0.9800 ?
C3 H3C 0.9800 ?
C4 H4A 0.9800 ?
C4 H4B 0.9800 ?
C4 H4C 0.9800 ?
C5 C7 1.525(5) ?
C5 C8 1.528(5) ?
C5 C6 1.536(4) ?
C6 H6A 0.9800 ?
C6 H6B 0.9800 ?
C6 H6C 0.9800 ?
C7 H7A 0.9800 ?
C7 H7B 0.9800 ?
C7 H7C 0.9800 ?
C8 H8A 0.9800 ?
C8 H8B 0.9800 ?
C8 H8C 0.9800 ?
C9 C11 1.535(5) ?
C9 C10 1.542(5) ?
C9 C12 1.540(5) ?
C10 H10A 0.9800 ?
C10 H10B 0.9800 ?
C10 H10C 0.9800 ?
C11 H11A 0.9800 ?
C11 H11B 0.9800 ?
C11 H11C 0.9800 ?
C12 H12A 0.9800 ?
C12 H12B 0.9800 ?
C12 H12C 0.9800 ?
C13 C16 1.536(5) ?
C13 C14 1.536(5) ?
C13 C15 1.549(5) ?
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 0.9800 ?
C16 H16B 0.9800 ?
C16 H16C 0.9800 ?
C31 C32 1.529(4) ?
C31 H31A 0.9900 ?
C31 H31B 0.9900 ?
C32 H32A 0.9900 ?
C32 H32B 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
P2 Pt1 P1 C31 8.74(11)
Cl1 Pt1 P1 C31 -170.88(11)
P2 Pt1 P1 C5 -106.82(12)
Cl1 Pt1 P1 C5 73.55(12)
P2 Pt1 P1 C1 123.22(11)
Cl1 Pt1 P1 C1 -56.40(11)
P1 Pt1 P2 C32 9.20(11)
Cl2 Pt1 P2 C32 -169.68(11)
P1 Pt1 P2 C9 -106.85(12)
Cl2 Pt1 P2 C9 74.27(12)
P1 Pt1 P2 C13 123.65(12)
Cl2 Pt1 P2 C13 -55.24(12)
C31 P1 C1 C4 83.6(2)
C5 P1 C1 C4 -163.8(2)
Pt1 P1 C1 C4 -31.9(3)
C31 P1 C1 C3 -157.1(2)
C5 P1 C1 C3 -44.5(3)
Pt1 P1 C1 C3 87.4(2)
C31 P1 C1 C2 -35.4(3)
C5 P1 C1 C2 77.2(3)
Pt1 P1 C1 C2 -151.0(2)
C31 P1 C5 C7 -172.7(2)
C1 P1 C5 C7 75.7(3)
Pt1 P1 C5 C7 -57.0(3)
C31 P1 C5 C8 -55.3(3)
C1 P1 C5 C8 -166.8(2)
Pt1 P1 C5 C8 60.4(3)
C31 P1 C5 C6 62.6(3)
C1 P1 C5 C6 -48.9(3)
Pt1 P1 C5 C6 178.4(2)
C32 P2 C9 C11 -169.3(2)
C13 P2 C9 C11 79.1(3)
Pt1 P2 C9 C11 -52.8(3)
C32 P2 C9 C10 66.3(3)
C13 P2 C9 C10 -45.3(3)
Pt1 P2 C9 C10 -177.3(2)
C32 P2 C9 C12 -51.6(2)
C13 P2 C9 C12 -163.2(2)
Pt1 P2 C9 C12 64.9(2)
C32 P2 C13 C16 81.9(2)
C9 P2 C13 C16 -165.2(2)
Pt1 P2 C13 C16 -34.1(3)
C32 P2 C13 C14 -158.1(2)
C9 P2 C13 C14 -45.2(3)
Pt1 P2 C13 C14 85.9(2)
C32 P2 C13 C15 -36.4(3)
C9 P2 C13 C15 76.5(3)
Pt1 P2 C13 C15 -152.4(2)
C5 P1 C31 C32 91.5(2)
C1 P1 C31 C32 -152.5(2)
Pt1 P1 C31 C32 -30.0(2)
P1 C31 C32 P2 39.6(3)
C9 P2 C32 C31 91.6(2)
C13 P2 C32 C31 -152.0(2)
Pt1 P2 C32 C31 -29.8(2)
