#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/05/7110585.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_7110585
loop_
_publ_author_name
'Clendenning, Scott B.'
'Hitchcock, Peter B.'
'Nixon, John F.'
_publ_section_title
;
 First η1-ligated 2,4,6-tri-tert-butyl-1,3,5-triphosphabenzene complexes
 and the remarkable trihydration reaction of trans-[PtCl2(PMe3)(P3C3But3)]
 to cis-[PtCl(PMe3)(P3O3C3H5But3)], containing the novel
 CH(But)PH(O)C(But)PH(O)CH(But)P(O) ring system
;
_journal_issue                   15
_journal_name_full               'Chemical Communications'
_journal_page_first              1377
_journal_paper_doi               10.1039/a903745d
_journal_year                    1999
_chemical_formula_sum            'C20.5 H46 Cl6 O3 P4 Pt'
_chemical_formula_weight         872.24
_chemical_name_common            '[PtCl(PMe3)(C15H32O3P3)].2.5(CH2Cl2)'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           64
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.508(9)
_cell_length_b                   15.924(9)
_cell_length_c                   29.018(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     6704(6)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_molecular_graphics    'CAMERON (Watkin and Pearce,1993)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_method       ω--2θ
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0561
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2428
_diffrn_reflns_theta_full        22.94
_diffrn_reflns_theta_max         22.94
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.877
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.37
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3464
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.651
_refine_diff_density_min         -5.303
_refine_diff_density_rms         0.334
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         2428
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0921
_refine_ls_R_factor_gt           0.0746
_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)+(0.1200P)²+238.8816P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1957
_refine_ls_wR_factor_ref         0.2088
_reflns_number_gt                1951
_reflns_number_total             2428
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            903745dsup1.cif
_cod_data_source_block           mar299
_cod_original_sg_symbol_H-M      Cmca
_cod_original_formula_sum        'C20.50 H46 Cl6 O3 P4 Pt'
_cod_database_code               7110585
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, -z'
'x, -y+1/2, z+1/2'
'x, y+1/2, -z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, -z'
'x+1/2, -y+1, z+1/2'
'x+1/2, y+1, -z+1/2'
'-x, -y, -z'
'-x, y, z'
'-x, y-1/2, -z-1/2'
'-x, -y-1/2, z-1/2'
'-x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, z'
'-x+1/2, y, -z-1/2'
'-x+1/2, -y, 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
Pt Pt 0.0000 0.05688(5) 0.66683(3) 0.0168(4) Uani 1 2 d S
Cl1 Cl 0.0000 -0.0460(3) 0.72803(19) 0.0280(13) Uani 1 2 d S
Cl2 Cl 0.2500 0.3138(4) 0.7500 0.061(2) Uani 1 2 d S
Cl3 Cl 0.1996(9) 0.4350(7) 0.6773(4) 0.056(3) Uani 0.50 1 d P
Cl4 Cl 0.5000 0.0355(6) 0.6188(3) 0.071(2) Uani 1 2 d S
Cl5 Cl 0.6577(8) -0.0658(7) 0.6496(5) 0.056(3) Uani 0.50 1 d P
Cl6 Cl 0.5000 0.0898(10) 0.4890(6) 0.156(6) Uani 1 2 d S
P1 P 0.0000 0.1536(3) 0.6116(2) 0.0219(13) Uani 1 2 d S
P2 P 0.1030(3) 0.0066(2) 0.58085(14) 0.0255(9) Uani 1 1 d .
H2 H 0.1534 -0.0036 0.6037 0.031 Uiso 1 1 calc R
P3 P 0.0000 0.1478(4) 0.7272(2) 0.0269(14) Uani 1 2 d S
O1 O 0.0000 0.2454(9) 0.6192(5) 0.026(3) Uani 1 2 d S
O2 O 0.1335(9) -0.0359(7) 0.5362(4) 0.044(3) Uani 1 1 d .
H2A H 0.115(18) 0.0000 0.5000 0.05(7) Uiso 1 2 d S
C1 C 0.0954(10) 0.1199(9) 0.5739(5) 0.024(4) Uani 1 1 d .
H1 H 0.0763 0.1312 0.5414 0.029 Uiso 1 1 calc R
C2 C 0.0000 -0.0311(12) 0.6067(8) 0.020(5) Uani 1 2 d S
C3 C 0.1923(11) 0.1656(11) 0.5820(6) 0.033(4) Uani 1 1 d .
C4 C 0.2169(11) 0.1720(12) 0.6337(6) 0.039(4) Uani 1 1 d .
H4A H 0.1672 0.2009 0.6501 0.059 Uiso 1 1 calc R
H4B H 0.2744 0.2037 0.6372 0.059 Uiso 1 1 calc R
H4C H 0.2249 0.1155 0.6464 0.059 Uiso 1 1 calc R
C5 C 0.1818(14) 0.2554(12) 0.5609(7) 0.049(5) Uani 1 1 d .
H5A H 0.1319 0.2853 0.5767 0.073 Uiso 1 1 calc R
H5B H 0.1673 0.2508 0.5280 0.073 Uiso 1 1 calc R
H5C H 0.2396 0.2865 0.5648 0.073 Uiso 1 1 calc R
C6 C 0.2704(11) 0.1196(13) 0.5562(6) 0.043(5) Uani 1 1 d .
H6A H 0.2773 0.0628 0.5688 0.064 Uiso 1 1 calc R
H6B H 0.3282 0.1506 0.5601 0.064 Uiso 1 1 calc R
H6C H 0.2551 0.1161 0.5233 0.064 Uiso 1 1 calc R
C7 C 0.0000 -0.1306(14) 0.6115(9) 0.035(6) Uani 1 2 d S
C8 C -0.0861(12) -0.1589(10) 0.6398(6) 0.036(4) Uani 1 1 d .
H8A H -0.1423 -0.1427 0.6234 0.055 Uiso 1 1 calc R
H8B H -0.0851 -0.1317 0.6701 0.055 Uiso 1 1 calc R
H8C H -0.0849 -0.2200 0.6438 0.055 Uiso 1 1 calc R
C9 C 0.0000 -0.1786(15) 0.5655(9) 0.065(11) Uani 1 2 d S
H9A H 0.0541 -0.1622 0.5474 0.098 Uiso 0.50 1 calc PR
H9B H -0.0561 -0.1649 0.5482 0.098 Uiso 0.50 1 calc PR
H9C H 0.0020 -0.2391 0.5715 0.098 Uiso 1 2 calc SR
C10 C 0.0000 0.2590(14) 0.7204(8) 0.038(6) Uani 1 2 d S
H10A H -0.0518 0.2756 0.7007 0.057 Uiso 0.50 1 calc PR
H10B H 0.0580 0.2767 0.7060 0.057 Uiso 0.50 1 calc PR
H10C H -0.0062 0.2858 0.7506 0.057 Uiso 0.50 1 calc PR
C11 C 0.0997(14) 0.1333(10) 0.7644(6) 0.044(5) Uani 1 1 d .
H11A H 0.1077 0.0734 0.7709 0.066 Uiso 1 1 calc R
H11B H 0.0903 0.1638 0.7933 0.066 Uiso 1 1 calc R
H11C H 0.1549 0.1548 0.7489 0.066 Uiso 1 1 calc R
C12 C 0.241(4) 0.421(2) 0.7309(15) 0.067(17) Uani 0.50 1 d P
H12A H 0.2013 0.4521 0.7527 0.081 Uiso 0.50 1 calc PR
H12B H 0.3034 0.4469 0.7324 0.081 Uiso 0.50 1 calc PR
C13 C 0.535(2) -0.0578(19) 0.6457(13) 0.039(9) Uiso 0.50 1 d P
H13A H 0.5106 -0.1063 0.6281 0.047 Uiso 0.50 1 calc PR
H13B H 0.5080 -0.0602 0.6771 0.047 Uiso 0.50 1 calc PR
C14 C 0.561(5) 0.0000 0.5000 0.08(2) Uiso 0.50 2 d SP
H14A H 0.6013 -0.0109 0.4732 0.095 Uiso 0.25 1 calc PR
H14B H 0.6013 0.0109 0.5268 0.095 Uiso 0.25 1 calc PR
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'
O O 0.0106 0.0060 '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 Pt C2 82.6(6) . .
P1 Pt P3 96.6(2) . .
C2 Pt P3 179.2(6) . .
P1 Pt Cl1 178.84(19) . .
C2 Pt Cl1 98.6(6) . .
P3 Pt Cl1 82.3(2) . .
C12 Cl2 C12 37(3) 15_557 .
Cl5 Cl3 C12 162(2) 5_455 .
C13 Cl4 C13 33(2) 10_655 .
Cl3 Cl5 C13 130.5(17) 5_545 .
C14 Cl6 C14 62(4) 10_655 .
O1 P1 C1 112.1(6) . 10
O1 P1 C1 112.1(6) . .
C1 P1 C1 97.3(9) 10 .
O1 P1 Pt 125.2(6) . .
C1 P1 Pt 103.1(5) 10 .
C1 P1 Pt 103.1(5) . .
O2 P2 C2 116.8(9) . .
O2 P2 C1 111.3(7) . .
C2 P2 C1 109.3(8) . .
C10 P3 C11 101.1(7) . 10
C10 P3 C11 101.1(7) . .
C11 P3 C11 105.3(13) 10 .
C10 P3 Pt 123.2(8) . .
C11 P3 Pt 112.1(6) 10 .
C11 P3 Pt 112.1(6) . .
C3 C1 P2 112.4(11) . .
C3 C1 P1 116.1(10) . .
P2 C1 P1 105.6(7) . .
C7 C2 P2 112.0(8) . 10
C7 C2 P2 112.0(8) . .
P2 C2 P2 114.6(12) 10 .
C7 C2 Pt 123.7(16) . .
P2 C2 Pt 96.7(7) 10 .
P2 C2 Pt 96.7(7) . .
C6 C3 C4 109.4(14) . .
C6 C3 C5 108.4(14) . .
C4 C3 C5 110.0(14) . .
C6 C3 C1 110.9(13) . .
C4 C3 C1 112.1(12) . .
C5 C3 C1 105.9(13) . .
C9 C7 C8 108.3(13) . .
C9 C7 C8 108.3(13) . 10
C8 C7 C8 106.2(19) . 10
C9 C7 C2 114.7(19) . .
C8 C7 C2 109.5(13) . .
C8 C7 C2 109.5(13) 10 .
Cl3 C12 Cl2 116(2) . .
Cl4 C13 Cl5 112.0(18) . .
Cl6 C14 Cl6 118(4) 9_656 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt P1 2.224(6) .
Pt C2 2.24(2) .
Pt P3 2.273(6) .
Pt Cl1 2.416(5) .
Cl2 C12 1.80(4) 15_557
Cl2 C12 1.80(4) .
Cl3 Cl5 1.008(15) 5_455
Cl3 C12 1.68(5) .
Cl4 C13 1.75(3) 10_655
Cl4 C13 1.75(3) .
Cl5 Cl3 1.008(15) 5_545
Cl5 C13 1.79(4) .
Cl6 C14 1.71(4) 10_655
Cl6 C14 1.71(4) .
P1 O1 1.479(15) .
P1 C1 1.843(16) 10
P1 C1 1.843(16) .
P2 O2 1.528(12) .
P2 C2 1.777(12) .
P2 C1 1.818(15) .
P3 C10 1.78(2) .
P3 C11 1.819(18) 10
P3 C11 1.819(18) .
C1 C3 1.601(19) .
C2 C7 1.59(3) .
C2 P2 1.777(12) 10
C3 C6 1.54(2) .
C3 C4 1.54(2) .
C3 C5 1.56(2) .
C7 C9 1.54(3) .
C7 C8 1.56(2) .
C7 C8 1.56(2) 10
C14 Cl6 1.71(4) 9_656
