#------------------------------------------------------------------------------
#$Date: 2019-11-26 01:29:14 +0200 (Tue, 26 Nov 2019) $
#$Revision: 242279 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/22/4132282.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_4132282
loop_
_publ_author_name
'Joshi, Hemant'
'Kharel, Sugam'
'Ehnbom, Andreas'
'Skopek, Katrin'
'Hess, Gisela D.'
'Fiedler, Tobias'
'Hampel, Frank'
'Bhuvanesh, Nattamai'
'Gladysz, John A.'
_publ_section_title
;
 Three-Fold Intramolecular Ring Closing Alkene Metatheses of Square Planar
 Complexes with cis Phosphorus Donor Ligands P(X(CH₂)
 ₘCH═CH₂)₃ (X = -, m = 5-10; X =
 O, m = 3-5): Syntheses, Structures, and Thermal Properties of Macrocyclic
 Dibridgehead Diphosphorus Complexes.
;
_journal_issue                   27
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8463
_journal_page_last               8478
_journal_paper_doi               10.1021/jacs.8b02846
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C30 H60 Cl2 O6 P2 Pt'
_chemical_formula_weight         844.71
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   27.3660(7)
_cell_length_b                   27.3660(7)
_cell_length_c                   26.3180(8)
_cell_measurement_reflns_used    2894
_cell_measurement_temperature    173(2)
_cell_volume                     17068.9(8)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'SHELXTL NT'
_computing_publication_material  'SHELXTL NT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.789
_diffrn_measured_fraction_theta_max 0.789
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotaing anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1292
_diffrn_reflns_av_sigmaI/netI    0.0986
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            6654
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    3.960
_exptl_absorpt_correction_T_max  0.4376
_exptl_absorpt_correction_T_min  0.3378
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Scalepack
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7740
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.752
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2664
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1032
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.063
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0965P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1546
_refine_ls_wR_factor_ref         0.1813
_reflns_number_gt                1801
_reflns_number_total             2664
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8b02846_si_009.cif
_cod_data_source_block           ks01
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Trigonal' was changed to
'trigonal' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      R-3c
_cod_database_code               4132282
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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
Pt1 Pt 0.3333 0.30416(2) -0.0833 0.0375(3) Uani 1 2 d S
P1 P 0.32075(13) 0.35440(13) -0.02451(12) 0.0368(7) Uani 1 1 d .
Cl1 Cl 0.33233(15) 0.24156(14) -0.02157(16) 0.0568(9) Uani 1 1 d .
O11 O 0.2862(4) 0.3809(4) -0.0481(4) 0.0422(19) Uani 1 1 d .
C11 C 0.2775(6) 0.4215(6) -0.0199(6) 0.053(3) Uani 1 1 d .
H11A H 0.3136 0.4574 -0.0165 0.063 Uiso 1 1 calc R
H11B H 0.2633 0.4069 0.0146 0.063 Uiso 1 1 calc R
C12 C 0.2350(6) 0.4312(6) -0.0484(6) 0.052(3) Uani 1 1 d .
H12A H 0.2468 0.4396 -0.0843 0.062 Uiso 1 1 calc R
H12B H 0.1979 0.3960 -0.0476 0.062 Uiso 1 1 calc R
C13 C 0.2282(9) 0.4782(8) -0.0273(8) 0.081(6) Uani 1 1 d D
H13A H 0.2143 0.4683 0.0081 0.097 Uiso 1 1 calc R
H13B H 0.1985 0.4801 -0.0471 0.097 Uiso 1 1 calc R
C14 C 0.2782(10) 0.5348(9) -0.0267(11) 0.146(16) Uani 1 1 d D
H14A H 0.3059 0.5360 -0.0018 0.176 Uiso 1 1 calc R
H14B H 0.2673 0.5628 -0.0164 0.176 Uiso 1 1 calc R
C15 C 0.3040(11) 0.5489(12) -0.0779(16) 0.27(4) Uani 1 1 d D
H15A H 0.2882 0.5126 -0.0964 0.326 Uiso 1 1 calc R
H15B H 0.2886 0.5707 -0.0947 0.326 Uiso 1 1 calc R
O21 O 0.2875(4) 0.3213(4) 0.0243(4) 0.046(2) Uani 1 1 d .
C21 C 0.2356(6) 0.2676(5) 0.0234(7) 0.060(4) Uani 1 1 d .
H21A H 0.2381 0.2424 0.0489 0.072 Uiso 1 1 calc R
H21B H 0.2314 0.2501 -0.0104 0.072 Uiso 1 1 calc R
C22 C 0.1849(7) 0.2720(6) 0.0340(7) 0.057(3) Uani 1 1 d .
H22A H 0.1809 0.2952 0.0072 0.069 Uiso 1 1 calc R
H22B H 0.1899 0.2914 0.0669 0.069 Uiso 1 1 calc R
C23 C 0.1311(7) 0.2144(7) 0.0359(7) 0.065(4) Uani 1 1 d .
H23A H 0.1359 0.1902 0.0611 0.078 Uiso 1 1 calc R
H23B H 0.0993 0.2193 0.0473 0.078 Uiso 1 1 calc R
C24 C 0.1168(7) 0.1850(7) -0.0160(7) 0.066(5) Uani 1 1 d .
H24A H 0.0845 0.1461 -0.0123 0.080 Uiso 1 1 calc R
H24B H 0.1495 0.1825 -0.0286 0.080 Uiso 1 1 calc R
C25 C 0.1009(7) 0.2193(8) -0.0565(7) 0.063(4) Uani 1 1 d .
H25A H 0.0681 0.2216 -0.0435 0.075 Uiso 1 1 calc R
H25B H 0.1331 0.2583 -0.0594 0.075 Uiso 1 1 calc R
C26 C 0.0864(6) 0.1922(8) -0.1100(8) 0.066(4) Uani 1 1 d .
H26A H 0.0606 0.1510 -0.1065 0.079 Uiso 1 1 calc R
H26B H 0.0663 0.2078 -0.1294 0.079 Uiso 1 1 calc R
C27 C 0.1387(6) 0.2025(7) -0.1398(7) 0.064(4) Uani 1 1 d .
H27A H 0.1266 0.1803 -0.1716 0.076 Uiso 1 1 calc R
H27B H 0.1599 0.1888 -0.1195 0.076 Uiso 1 1 calc R
C28 C 0.1782(6) 0.2656(6) -0.1530(5) 0.051(3) Uani 1 1 d .
H28A H 0.1555 0.2821 -0.1656 0.061 Uiso 1 1 calc R
H28B H 0.1983 0.2864 -0.1220 0.061 Uiso 1 1 calc R
C29 C 0.2208(6) 0.2719(6) -0.1931(6) 0.051(3) Uani 1 1 d .
H29A H 0.2435 0.2555 -0.1802 0.062 Uiso 1 1 calc R
H29B H 0.2005 0.2504 -0.2238 0.062 Uiso 1 1 calc R
C30 C 0.2600(6) 0.3328(6) -0.2077(5) 0.050(3) Uani 1 1 d .
H30A H 0.2857 0.3341 -0.2348 0.060 Uiso 1 1 calc R
H30B H 0.2373 0.3487 -0.2216 0.060 Uiso 1 1 calc R
O30 O 0.2931(3) 0.3672(4) -0.1661(4) 0.0414(19) Uani 1 1 d .
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'
O O 0.0106 0.0060 '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 91.07(16) . 12_554
P1 Pt1 Cl1 172.70(12) . 12_554
P1 Pt1 Cl1 91.17(13) 12_554 12_554
P1 Pt1 Cl1 91.17(13) . .
P1 Pt1 Cl1 172.71(12) 12_554 .
Cl1 Pt1 Cl1 87.5(2) 12_554 .
O11 P1 O21 106.2(5) . .
O11 P1 O30 102.6(5) . 12_554
O21 P1 O30 101.7(5) . 12_554
O11 P1 Pt1 109.0(4) . .
O21 P1 Pt1 116.0(4) . .
O30 P1 Pt1 119.7(4) 12_554 .
C11 O11 P1 121.1(9) . .
O11 C11 C12 108.4(11) . .
C13 C12 C11 113.8(13) . .
C12 C13 C14 117.4(17) . .
C13 C14 C15 110(2) . .
C15 C15 C14 126(4) 12_554 .
C21 O21 P1 124.3(10) . .
O21 C21 C22 113.7(12) . .
C21 C22 C23 112.6(12) . .
C24 C23 C22 111.8(15) . .
C23 C24 C25 110.8(14) . .
C26 C25 C24 113.6(15) . .
C27 C26 C25 112.7(13) . .
C26 C27 C28 112.8(14) . .
C29 C28 C27 110.6(13) . .
C30 C29 C28 112.5(12) . .
O30 C30 C29 113.4(12) . .
C30 O30 P1 125.6(8) . 12_554
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 P1 2.209(3) .
Pt1 P1 2.209(3) 12_554
Pt1 Cl1 2.352(3) 12_554
Pt1 Cl1 2.352(3) .
P1 O11 1.577(9) .
P1 O21 1.573(10) .
P1 O30 1.580(9) 12_554
O11 C11 1.451(15) .
C11 C12 1.52(2) .
C12 C13 1.50(2) .
C13 C14 1.47(3) .
C14 C15 1.48(3) .
C15 C15 1.42(6) 12_554
O21 C21 1.445(15) .
C21 C22 1.48(2) .
C22 C23 1.53(2) .
C23 C24 1.53(3) .
C24 C25 1.62(2) .
C25 C26 1.55(3) .
C26 C27 1.53(2) .
C27 C28 1.55(2) .
C28 C29 1.518(18) .
C29 C30 1.51(2) .
C30 O30 1.432(17) .
O30 P1 1.580(8) 12_554
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
_geom_torsion_site_symmetry_4
P1 Pt1 P1 O11 38.1(4) 12_554 .
Cl1 Pt1 P1 O11 -69.8(11) 12_554 .
Cl1 Pt1 P1 O11 -148.8(4) . .
P1 Pt1 P1 O21 158.0(4) 12_554 .
Cl1 Pt1 P1 O21 50.1(12) 12_554 .
Cl1 Pt1 P1 O21 -29.0(4) . .
P1 Pt1 P1 O30 -79.4(4) 12_554 12_554
Cl1 Pt1 P1 O30 172.7(10) 12_554 12_554
Cl1 Pt1 P1 O30 93.6(4) . 12_554
O21 P1 O11 C11 61.7(11) . .
O30 P1 O11 C11 -44.7(11) 12_554 .
Pt1 P1 O11 C11 -172.6(9) . .
P1 O11 C11 C12 -170.4(9) . .
O11 C11 C12 C13 -171.8(15) . .
C11 C12 C13 C14 61(2) . .
C12 C13 C14 C15 52(3) . .
C13 C14 C15 C15 -140.9(13) . 12_554
O11 P1 O21 C21 74.8(10) . .
O30 P1 O21 C21 -178.2(10) 12_554 .
Pt1 P1 O21 C21 -46.5(11) . .
P1 O21 C21 C22 -103.5(15) . .
O21 C21 C22 C23 -176.6(14) . .
C21 C22 C23 C24 -66.0(19) . .
C22 C23 C24 C25 -66.1(18) . .
C23 C24 C25 C26 179.6(14) . .
C24 C25 C26 C27 -75.7(18) . .
C25 C26 C27 C28 -65.8(19) . .
C26 C27 C28 C29 -165.7(14) . .
C27 C28 C29 C30 179.4(12) . .
C28 C29 C30 O30 60.9(16) . .
C29 C30 O30 P1 75.3(14) . 12_554
