#------------------------------------------------------------------------------
#$Date: 2018-08-07 19:40:34 +0300 (Tue, 07 Aug 2018) $
#$Revision: 209451 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/20/45/2204509.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_2204509
loop_
_publ_author_name
'Jaska, Cory A.'
'Lough, Alan J.'
'Manners, Ian'
_publ_section_title
;Bis(μ-phenylphosphido-κ²P:P)bis{[1,2-(dicyclohexylphosphino)ethane-κ²P,P']platinum(I)}
 dichloride bis(dichloromethane) hexane solvate
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1653
_journal_page_last               m1655
_journal_paper_doi               10.1107/S1600536804025309
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac
'[Pt2 (C6 H6 P)2 (C26 H48 P2)2] Cl2, 2C H2 Cl2, C6 H14'
_chemical_formula_moiety
'C64 H108 P6 Pt2 2+, 2Cl -, 2C H2 Cl2, C6 H14'
_chemical_formula_sum            'C72 H126 Cl6 P6 Pt2'
_chemical_formula_weight         1780.43
_chemical_name_systematic
;
Bis(μ-phenylphosphido-κ²P:P)bis{[1,2-(dicyclohexylphosphino)ethane-
κ²P,P']platinum(I)} dichloride bis(dichloromethane) hexane solvate
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 111.348(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   25.2590(9)
_cell_length_b                   13.9810(5)
_cell_length_c                   12.3080(5)
_cell_measurement_reflns_used    14701
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     4048.3(3)
_computing_cell_refinement       'DENZO--SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2003)'
_computing_data_reduction        DENZO--SMN
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      150.0(10)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius KapppaCCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offsets'
_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  0.0610
_diffrn_reflns_av_sigmaI/netI    0.0567
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14701
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.67
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.806
_exptl_absorpt_correction_T_max  0.683
_exptl_absorpt_correction_T_min  0.636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1812
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.255
_refine_diff_density_min         -1.384
_refine_ls_extinction_coef       0.00110(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         4810
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0362
_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)+(0.0435P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0874
_reflns_number_gt                4223
_reflns_number_total             4810
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb6109.cif
_cod_data_source_block           I
_cod_depositor_comments
;
 Removing duplicate rows from the ATOM_TYPE loop.

 Antanas Vaitkus,
 2018-08-07
;
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               2204509
_cod_database_fobs_code          2204509
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
loop_
_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
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Pt1 0.0000 0.131118(14) 0.5000 0.02304(10) Uani d S 1 . . Pt
P1 0.06391(5) 0.25169(7) 0.51287(9) 0.0262(2) Uani d . 1 . . P
H1P 0.114(3) 0.0000 0.535(5) 0.035(17) Uiso d S 1 . . H
P2 0.06166(6) 0.0000 0.55508(12) 0.0243(3) Uani d S 1 . . P
C1 0.0327(2) 0.3683(3) 0.5233(4) 0.0317(10) Uani d . 1 . . C
H1A 0.0469 0.3886 0.6061 0.038 Uiso calc R 1 . . H
H1B 0.0457 0.4160 0.4791 0.038 Uiso calc R 1 . . H
C2 0.07685(19) 0.2521(3) 0.3735(4) 0.0310(9) Uani d . 1 . . C
H2A 0.0992 0.3108 0.3721 0.037 Uiso calc R 1 . . H
C3 0.0203(2) 0.2579(3) 0.2720(4) 0.0349(10) Uani d . 1 . . C
H3A 0.0001 0.3169 0.2788 0.042 Uiso calc R 1 . . H
H3B -0.0036 0.2025 0.2746 0.042 Uiso calc R 1 . . H
C4 0.0294(2) 0.2582(4) 0.1558(4) 0.0460(12) Uani d . 1 . . C
H4A -0.0080 0.2587 0.0909 0.055 Uiso calc R 1 . . H
H4B 0.0499 0.3172 0.1500 0.055 Uiso calc R 1 . . H
C5 0.0629(2) 0.1721(4) 0.1437(4) 0.0473(12) Uani d . 1 . . C
H5A 0.0695 0.1762 0.0693 0.057 Uiso calc R 1 . . H
H5B 0.0408 0.1132 0.1418 0.057 Uiso calc R 1 . . H
C6 0.1196(2) 0.1669(4) 0.2449(4) 0.0458(12) Uani d . 1 . . C
H6A 0.1431 0.2230 0.2424 0.055 Uiso calc R 1 . . H
H6B 0.1402 0.1085 0.2375 0.055 Uiso calc R 1 . . H
C7 0.1109(2) 0.1653(4) 0.3618(4) 0.0386(10) Uani d . 1 . . C
H7A 0.0905 0.1061 0.3674 0.046 Uiso calc R 1 . . H
H7B 0.1483 0.1650 0.4265 0.046 Uiso calc R 1 . . H
C8 0.13461(18) 0.2549(3) 0.6302(4) 0.0332(10) Uani d . 1 . . C
H8A 0.1553 0.1957 0.6231 0.040 Uiso calc R 1 . . H
C9 0.1312(2) 0.2546(3) 0.7519(4) 0.0383(11) Uani d . 1 . . C
H9A 0.1111 0.1962 0.7617 0.046 Uiso calc R 1 . . H
H9B 0.1092 0.3108 0.7604 0.046 Uiso calc R 1 . . H
C10 0.1910(2) 0.2574(4) 0.8465(5) 0.0544(15) Uani d . 1 . . C
H10A 0.1880 0.2592 0.9244 0.065 Uiso calc R 1 . . H
H10B 0.2120 0.1986 0.8417 0.065 Uiso calc R 1 . . H
C11 0.2235(3) 0.3442(4) 0.8314(5) 0.0640(18) Uani d . 1 . . C
H11A 0.2040 0.4030 0.8416 0.077 Uiso calc R 1 . . H
H11B 0.2622 0.3438 0.8918 0.077 Uiso calc R 1 . . H
C12 0.2275(2) 0.3447(4) 0.7122(6) 0.0613(16) Uani d . 1 . . C
H12A 0.2501 0.2889 0.7050 0.074 Uiso calc R 1 . . H
H12B 0.2475 0.4034 0.7033 0.074 Uiso calc R 1 . . H
C13 0.1690(2) 0.3410(4) 0.6151(5) 0.0491(13) Uani d . 1 . . C
H13A 0.1736 0.3365 0.5387 0.059 Uiso calc R 1 . . H
H13B 0.1481 0.4007 0.6158 0.059 Uiso calc R 1 . . H
C14 0.0938(2) 0.0000 0.7138(5) 0.0278(12) Uani d S 1 . . C
C15 0.0598(3) 0.0000 0.7821(5) 0.0323(13) Uani d S 1 . . C
H15A 0.0196 0.0000 0.7446 0.039 Uiso calc SR 1 . . H
C16 0.0831(3) 0.0000 0.9013(6) 0.0447(17) Uani d S 1 . . C
H16A 0.0593 0.0000 0.9457 0.054 Uiso calc SR 1 . . H
C17 0.1423(3) 0.0000 0.9578(6) 0.0480(18) Uani d S 1 . . C
H17A 0.1586 0.0000 1.0406 0.058 Uiso calc SR 1 . . H
C18 0.1769(3) 0.0000 0.8933(6) 0.0467(18) Uani d S 1 . . C
H18A 0.2170 0.0000 0.9317 0.056 Uiso calc SR 1 . . H
C19 0.1528(3) 0.0000 0.7708(5) 0.0354(14) Uani d S 1 . . C
H19A 0.1768 0.0000 0.7266 0.043 Uiso calc SR 1 . . H
Cl1 0.0629(2) 0.5000 0.2809(4) 0.0558(9) Uani d SP 0.60 A 1 Cl
Cl1a 0.0897(3) 0.5000 0.3404(5) 0.0470(12) Uani d SP 0.40 B 2 Cl
Cl2 0.26019(10) 0.10394(19) 0.6145(2) 0.1069(7) Uani d D 1 . . Cl
C1S 0.2690(9) 0.0000 0.5444(15) 0.068(5) Uiso d SPD 0.50 . 1 C
H1S1 0.3076 0.0000 0.5409 0.082 Uiso calc SPR 0.50 . 1 H
H1S2 0.2411 0.0000 0.4633 0.082 Uiso calc SPR 0.50 . 1 H
C1Sa 0.2986(7) 0.0000 0.615(3) 0.115(9) Uiso d SPD 0.50 . 2 C
H1S3 0.3095 0.0000 0.5455 0.138 Uiso calc SPR 0.50 . 2 H
H1S4 0.3339 0.0000 0.6850 0.138 Uiso calc SPR 0.50 . 2 H
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'
Cl Cl 0.1484 0.1585 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
P1 Pt1 P1 2_556 . 85.70(6) y
P1 Pt1 P2 2_556 5_556 100.24(4) ?
P1 Pt1 P2 . 5_556 166.11(4) n
P1 Pt1 P2 2_556 . 166.11(4) y
P1 Pt1 P2 . . 100.24(4) y
P2 Pt1 P2 2_556 . 76.87(6) y
C1 P1 C8 . . 104.0(2) ?
C1 P1 C2 . . 106.6(2) ?
C8 P1 C2 . . 106.1(2) ?
C1 P1 Pt1 . . 110.29(14) ?
C8 P1 Pt1 . . 121.83(15) ?
C2 P1 Pt1 . . 107.08(14) ?
H1P P2 C14 . . 96(2) ?
H1P P2 Pt1 . 5_556 120.6(10) ?
C14 P2 Pt1 . 5_556 107.49(12) ?
H1P P2 Pt1 . . 120.6(10) ?
C14 P2 Pt1 . . 107.49(12) ?
Pt1 P2 Pt1 5_556 . 103.13(6) y
C1 C1 P1 2_556 . 113.85(17) ?
C1 C1 H1A 2_556 . 108.8 ?
P1 C1 H1A . . 108.8 ?
C1 C1 H1B 2_556 . 108.8 ?
P1 C1 H1B . . 108.8 ?
H1A C1 H1B . . 107.7 ?
C3 C2 C7 . . 111.0(4) ?
C3 C2 P1 . . 109.3(3) ?
C7 C2 P1 . . 112.3(3) ?
C3 C2 H2A . . 108.1 ?
C7 C2 H2A . . 108.1 ?
P1 C2 H2A . . 108.1 ?
C2 C3 C4 . . 110.7(4) ?
C2 C3 H3A . . 109.5 ?
C4 C3 H3A . . 109.5 ?
C2 C3 H3B . . 109.5 ?
C4 C3 H3B . . 109.5 ?
H3A C3 H3B . . 108.1 ?
C5 C4 C3 . . 111.7(4) ?
C5 C4 H4A . . 109.3 ?
C3 C4 H4A . . 109.3 ?
C5 C4 H4B . . 109.3 ?
C3 C4 H4B . . 109.3 ?
H4A C4 H4B . . 107.9 ?
C4 C5 C6 . . 110.6(4) ?
C4 C5 H5A . . 109.5 ?
C6 C5 H5A . . 109.5 ?
C4 C5 H5B . . 109.5 ?
C6 C5 H5B . . 109.5 ?
H5A C5 H5B . . 108.1 ?
C5 C6 C7 . . 110.8(4) ?
C5 C6 H6A . . 109.5 ?
C7 C6 H6A . . 109.5 ?
C5 C6 H6B . . 109.5 ?
C7 C6 H6B . . 109.5 ?
H6A C6 H6B . . 108.1 ?
C2 C7 C6 . . 110.8(4) ?
C2 C7 H7A . . 109.5 ?
C6 C7 H7A . . 109.5 ?
C2 C7 H7B . . 109.5 ?
C6 C7 H7B . . 109.5 ?
H7A C7 H7B . . 108.1 ?
C9 C8 C13 . . 110.9(4) ?
C9 C8 P1 . . 112.5(3) ?
C13 C8 P1 . . 110.7(3) ?
C9 C8 H8A . . 107.5 ?
C13 C8 H8A . . 107.5 ?
P1 C8 H8A . . 107.5 ?
C8 C9 C10 . . 110.5(4) ?
C8 C9 H9A . . 109.5 ?
C10 C9 H9A . . 109.5 ?
C8 C9 H9B . . 109.5 ?
C10 C9 H9B . . 109.5 ?
H9A C9 H9B . . 108.1 ?
C11 C10 C9 . . 110.8(4) ?
C11 C10 H10A . . 109.5 ?
C9 C10 H10A . . 109.5 ?
C11 C10 H10B . . 109.5 ?
C9 C10 H10B . . 109.5 ?
H10A C10 H10B . . 108.1 ?
C12 C11 C10 . . 110.8(5) ?
C12 C11 H11A . . 109.5 ?
C10 C11 H11A . . 109.5 ?
C12 C11 H11B . . 109.5 ?
C10 C11 H11B . . 109.5 ?
H11A C11 H11B . . 108.1 ?
C11 C12 C13 . . 112.0(5) ?
C11 C12 H12A . . 109.2 ?
C13 C12 H12A . . 109.2 ?
C11 C12 H12B . . 109.2 ?
C13 C12 H12B . . 109.2 ?
H12A C12 H12B . . 107.9 ?
C12 C13 C8 . . 111.2(4) ?
C12 C13 H13A . . 109.4 ?
C8 C13 H13A . . 109.4 ?
C12 C13 H13B . . 109.4 ?
C8 C13 H13B . . 109.4 ?
H13A C13 H13B . . 108.0 ?
C19 C14 C15 . . 118.2(5) ?
C19 C14 P2 . . 121.1(5) ?
C15 C14 P2 . . 120.7(4) ?
C16 C15 C14 . . 121.5(6) ?
C16 C15 H15A . . 119.2 ?
C14 C15 H15A . . 119.2 ?
C15 C16 C17 . . 119.9(7) ?
C15 C16 H16A . . 120.0 ?
C17 C16 H16A . . 120.0 ?
C18 C17 C16 . . 120.0(6) ?
C18 C17 H17A . . 120.0 ?
C16 C17 H17A . . 120.0 ?
C17 C18 C19 . . 120.1(7) ?
C17 C18 H18A . . 120.0 ?
C19 C18 H18A . . 120.0 ?
C14 C19 C18 . . 120.3(6) ?
C14 C19 H19A . . 119.8 ?
C18 C19 H19A . . 119.8 ?
Cl2 C1S Cl2 . 6 112.7(8) ?
Cl2 C1S H1S1 . . 109.0 ?
Cl2 C1S H1S1 6 . 109.0 ?
Cl2 C1S H1S2 . . 109.0 ?
Cl2 C1S H1S2 6 . 109.0 ?
H1S1 C1S H1S2 . . 107.8 ?
Cl2 C1Sa Cl2 6 . 112.7(8) ?
Cl2 C1Sa H1S3 6 . 109.0 ?
Cl2 C1Sa H1S3 . . 109.0 ?
Cl2 C1Sa H1S4 6 . 109.1 ?
Cl2 C1Sa H1S4 . . 109.1 ?
H1S3 C1Sa H1S4 . . 107.8 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pt1 P1 2_556 2.2993(11) ?
Pt1 P1 . 2.2993(11) y
Pt1 P2 5_556 2.3403(9) ?
Pt1 P2 . 2.3403(9) y
P1 C1 . 1.836(4) ?
P1 C8 . 1.843(4) ?
P1 C2 . 1.859(4) ?
H1P P2 . 1.43(6) y
P2 C14 . 1.822(6) ?
P2 Pt1 5_556 2.3403(9) ?
C1 C1 2_556 1.537(9) ?
C1 H1A . 0.9900 ?
C1 H1B . 0.9900 ?
C2 C3 . 1.520(6) ?
C2 C7 . 1.525(6) ?
C2 H2A . 1.0000 ?
C3 C4 . 1.529(6) ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C4 C5 . 1.510(7) ?
C4 H4A . 0.9900 ?
C4 H4B . 0.9900 ?
C5 C6 . 1.521(7) ?
C5 H5A . 0.9900 ?
C5 H5B . 0.9900 ?
C6 C7 . 1.533(6) ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C8 C9 . 1.532(6) ?
C8 C13 . 1.536(6) ?
C8 H8A . 1.0000 ?
C9 C10 . 1.536(6) ?
C9 H9A . 0.9900 ?
C9 H9B . 0.9900 ?
C10 C11 . 1.514(8) ?
C10 H10A . 0.9900 ?
C10 H10B . 0.9900 ?
C11 C12 . 1.506(10) ?
C11 H11A . 0.9900 ?
C11 H11B . 0.9900 ?
C12 C13 . 1.525(7) ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
C13 H13A . 0.9900 ?
C13 H13B . 0.9900 ?
C14 C19 . 1.397(8) ?
C14 C15 . 1.405(8) ?
C15 C16 . 1.367(9) ?
C15 H15A . 0.9500 ?
C16 C17 . 1.400(10) ?
C16 H16A . 0.9500 ?
C17 C18 . 1.376(11) ?
C17 H17A . 0.9500 ?
C18 C19 . 1.405(9) ?
C18 H18A . 0.9500 ?
C19 H19A . 0.9500 ?
Cl2 C1S . 1.746(8) ?
Cl2 C1Sa . 1.746(8) ?
C1S Cl2 6 1.746(8) ?
C1S H1S1 . 0.9900 ?
C1S H1S2 . 0.9900 ?
C1Sa Cl2 6 1.746(8) ?
C1Sa H1S3 . 0.9900 ?
C1Sa H1S4 . 0.9900 ?
