#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:29:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179181 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/29/4312951.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_4312951
loop_
_publ_author_name
'Brandy A. Harper'
'D. Andrew Knight'
'Clifford George'
'Susan L. Brandow'
'Walter J. Dressick'
'Charles S. Dalcey'
'Terence L. Schull'
_publ_section_title
;
 Coordination Chemistry of the Water-Soluble Ligand TPPTP and Formation of
 a [Mo(CO)5(m-TPPTP)] Monolayer on an Alumina Surface
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              516
_journal_page_last               524
_journal_paper_doi               10.1021/ic025862a
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C18 H16 O11 P4'
_chemical_formula_weight         532.19
_chemical_name_systematic
;

  ?

;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.177(6)
_cell_angle_beta                 105.885(6)
_cell_angle_gamma                108.784(5)
_cell_formula_units_Z            2
_cell_length_a                   8.3501(6)
_cell_length_b                   10.1907(6)
_cell_length_c                   14.6529(14)
_cell_measurement_reflns_used    29
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.19
_cell_volume                     1117.50(16)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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      213(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2θ/ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0146
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            3123
_diffrn_reflns_theta_full        57.49
_diffrn_reflns_theta_max         57.49
_diffrn_reflns_theta_min         3.19
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.668
_exptl_absorpt_correction_T_max  0.8126
_exptl_absorpt_correction_T_min  0.3840
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         2884
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0441
_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)+(0.0730P)²+2.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1295
_reflns_number_gt                2641
_reflns_number_total             2884
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025862a-2_s2.cif
_cod_data_source_block           mtpptp
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1117.50(15)
_cod_database_code               4312951
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
P2 P 0.47900(11) 0.82220(9) 0.56936(6) 0.0173(3) Uani 1 1 d . . .
P1 P 1.19194(12) 1.06459(10) 0.75372(7) 0.0218(3) Uani 1 1 d . . .
P1' P 0.17744(11) 0.71809(9) 0.17086(6) 0.0184(3) Uani 1 1 d D . .
P1" P 0.37314(13) 0.75617(10) 0.91813(7) 0.0230(3) Uani 1 1 d D . .
O1 O 1.1690(3) 1.2099(3) 0.76354(19) 0.0296(7) Uani 1 1 d . . .
O2 O 1.3670(3) 1.0759(3) 0.7425(2) 0.0360(7) Uani 1 1 d . . .
O3 O 1.1563(4) 1.0061(3) 0.84399(19) 0.0340(7) Uani 1 1 d . . .
O1' O 0.2277(4) 0.6181(3) 0.11267(19) 0.0258(7) Uani 0.918(3) 1 d PD A 1
O2' O -0.0084(3) 0.7186(3) 0.12148(19) 0.0266(7) Uani 0.918(3) 1 d PD A 1
O3' O 0.3092(3) 0.8723(3) 0.1869(2) 0.0254(7) Uani 0.918(3) 1 d PD A 1
O3'A O 0.357(2) 0.748(3) 0.153(2) 0.025 Uiso 0.082(3) 1 d PD A 2
O2'A O 0.110(4) 0.840(2) 0.174(2) 0.025 Uiso 0.082(3) 1 d PD A 2
O1'A O 0.046(3) 0.591(2) 0.0934(17) 0.025 Uiso 0.082(3) 1 d PD A 2
O1" O 0.3861(5) 0.6536(3) 0.9892(2) 0.0494(9) Uani 1 1 d D B 1
O2" O 0.1944(3) 0.7751(3) 0.8917(2) 0.0310(7) Uani 1 1 d D B 1
O3" O 0.5243(4) 0.8994(3) 0.9577(2) 0.0401(8) Uani 1 1 d D B 1
C1 C 0.7014(5) 0.8396(4) 0.5633(3) 0.0182(8) Uani 1 1 d . . .
C2 C 0.8418(5) 0.9276(4) 0.6432(3) 0.0199(8) Uani 1 1 d . . .
H2A H 0.8160 0.9710 0.6933 0.024 Uiso 1 1 calc R . .
C3 C 1.0186(5) 0.9518(4) 0.6497(3) 0.0198(8) Uani 1 1 d . . .
C4 C 1.0556(5) 0.8871(4) 0.5752(3) 0.0222(8) Uani 1 1 d . . .
H4A H 1.1745 0.9019 0.5790 0.027 Uiso 1 1 calc R . .
C5 C 0.9185(5) 0.8010(4) 0.4953(3) 0.0230(8) Uani 1 1 d . . .
H5A H 0.9447 0.7586 0.4448 0.028 Uiso 1 1 calc R . .
C6 C 0.7422(5) 0.7772(4) 0.4897(3) 0.0218(8) Uani 1 1 d . . .
H6A H 0.6497 0.7182 0.4355 0.026 Uiso 1 1 calc R . .
C1' C 0.3243(4) 0.7000(4) 0.4588(2) 0.0163(8) Uani 1 1 d . A .
C2' C 0.3141(4) 0.7480(4) 0.3718(2) 0.0180(8) Uani 1 1 d . . .
H2'A H 0.3932 0.8373 0.3710 0.022 Uiso 1 1 calc R A .
C3' C 0.1877(4) 0.6658(4) 0.2850(3) 0.0189(8) Uani 1 1 d . A .
C4' C 0.0673(5) 0.5355(4) 0.2879(3) 0.0268(9) Uani 1 1 d . . .
H4'A H -0.0196 0.4798 0.2307 0.032 Uiso 1 1 calc R A .
C5' C 0.0747(5) 0.4880(4) 0.3738(3) 0.0286(9) Uani 1 1 d . A .
H5'A H -0.0070 0.4001 0.3751 0.034 Uiso 1 1 calc R . .
C6' C 0.2027(5) 0.5696(4) 0.4589(3) 0.0242(9) Uani 1 1 d . . .
H6'A H 0.2069 0.5361 0.5173 0.029 Uiso 1 1 calc R A .
C1" C 0.4670(4) 0.7127(4) 0.6624(2) 0.0170(8) Uani 1 1 d . B .
C2" C 0.4224(4) 0.7585(4) 0.7406(2) 0.0188(8) Uani 1 1 d . . .
H2"A H 0.3965 0.8416 0.7424 0.023 Uiso 1 1 calc R B .
C3" C 0.4155(5) 0.6833(4) 0.8167(3) 0.0198(8) Uani 1 1 d . B .
C4" C 0.4478(5) 0.5583(4) 0.8123(3) 0.0263(9) Uani 1 1 d . . .
H4"A H 0.4397 0.5056 0.8620 0.032 Uiso 1 1 calc R B .
C5" C 0.4920(5) 0.5108(4) 0.7350(3) 0.0281(9) Uani 1 1 d . B .
H5"A H 0.5135 0.4258 0.7323 0.034 Uiso 1 1 calc R . .
C6" C 0.5047(5) 0.5877(4) 0.6618(3) 0.0248(9) Uani 1 1 d . . .
H6"A H 0.5390 0.5562 0.6109 0.030 Uiso 1 1 calc R B .
O1S O 0.0951(4) 0.3461(3) 0.0620(2) 0.0418(8) Uani 1 1 d D . .
H1SA H -0.012(4) 0.309(5) 0.082(3) 0.050 Uiso 1 1 d D . .
H1SB H 0.068(6) 0.332(5) -0.0089(9) 0.050 Uiso 1 1 d D . .
O2S O 0.8477(8) 0.9595(5) 0.9381(4) 0.1010(17) Uani 1 1 d D . .
H2SA H 0.872(10) 0.882(6) 0.969(5) 0.121 Uiso 1 1 d D . .
H2SB H 0.858(11) 1.035(6) 0.900(5) 0.121 Uiso 1 1 d D . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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
_geom_angle_publ_flag
C1" P2 C1 99.48(15) . . ?
C1" P2 C1' 103.18(16) . . ?
C1 P2 C1' 104.66(15) . . ?
O2 P1 O3 115.50(17) . . ?
O2 P1 O1 112.22(16) . . ?
O3 P1 O1 104.02(15) . . ?
O2 P1 C3 108.84(16) . . ?
O3 P1 C3 107.69(16) . . ?
O1 P1 C3 108.24(15) . . ?
O1' P1' O2'A 148.2(12) . . ?
O1' P1' O2' 112.51(16) . . ?
O2'A P1' O2' 51.6(11) . . ?
O1' P1' O1'A 54.5(11) . . ?
O2'A P1' O1'A 112.4(16) . . ?
O2' P1' O1'A 61.7(11) . . ?
O1' P1' O3'A 53.6(11) . . ?
O2'A P1' O3'A 117.0(16) . . ?
O2' P1' O3'A 139.7(11) . . ?
O1'A P1' O3'A 105.4(16) . . ?
O1' P1' O3' 111.06(16) . . ?
O2'A P1' O3' 60.1(11) . . ?
O2' P1' O3' 106.76(15) . . ?
O1'A P1' O3' 143.7(12) . . ?
O3'A P1' O3' 59.5(11) . . ?
O1' P1' C3' 107.91(16) . . ?
O2'A P1' C3' 103.8(12) . . ?
O2' P1' C3' 109.68(16) . . ?
O1'A P1' C3' 107.4(12) . . ?
O3'A P1' C3' 110.7(11) . . ?
O3' P1' C3' 108.88(16) . . ?
O2" P1" O3" 110.17(16) . . ?
O2" P1" O1" 112.30(18) . . ?
O3" P1" O1" 111.3(2) . . ?
O2" P1" C3" 112.72(16) . . ?
O3" P1" C3" 105.18(17) . . ?
O1" P1" C3" 104.84(17) . . ?
C6 C1 C2 118.5(3) . . ?
C6 C1 P2 127.3(3) . . ?
C2 C1 P2 114.2(3) . . ?
C3 C2 C1 121.3(3) . . ?
C4 C3 C2 118.9(3) . . ?
C4 C3 P1 121.9(3) . . ?
C2 C3 P1 119.2(3) . . ?
C5 C4 C3 120.5(3) . . ?
C4 C5 C6 120.1(3) . . ?
C1 C6 C5 120.6(3) . . ?
C6' C1' C2' 118.5(3) . . ?
C6' C1' P2 123.2(3) . . ?
C2' C1' P2 117.8(3) . . ?
C1' C2' C3' 121.3(3) . . ?
C4' C3' C2' 118.6(3) . . ?
C4' C3' P1' 118.4(3) . . ?
C2' C3' P1' 123.0(3) . . ?
C5' C4' C3' 120.5(3) . . ?
C4' C5' C6' 120.2(4) . . ?
C1' C6' C5' 120.9(3) . . ?
C2" C1" C6" 117.8(3) . . ?
C2" C1" P2 117.6(3) . . ?
C6" C1" P2 124.6(3) . . ?
C1" C2" C3" 121.5(3) . . ?
C4" C3" C2" 119.2(3) . . ?
C4" C3" P1" 122.3(3) . . ?
C2" C3" P1" 118.5(3) . . ?
C5" C4" C3" 120.2(4) . . ?
C6" C5" C4" 120.3(3) . . ?
C5" C6" C1" 121.0(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P2 C1" 1.827(4) . ?
P2 C1 1.835(4) . ?
P2 C1' 1.835(3) . ?
P1 O2 1.484(3) . ?
P1 O3 1.552(3) . ?
P1 O1 1.554(3) . ?
P1 C3 1.790(4) . ?
P1' O1' 1.512(3) . ?
P1' O2'A 1.522(11) . ?
P1' O2' 1.524(3) . ?
P1' O1'A 1.534(11) . ?
P1' O3'A 1.535(11) . ?
P1' O3' 1.558(3) . ?
P1' C3' 1.780(4) . ?
P1" O2" 1.514(3) . ?
P1" O3" 1.533(3) . ?
P1" O1" 1.536(3) . ?
P1" C3" 1.784(4) . ?
C1 C6 1.388(5) . ?
C1 C2 1.402(5) . ?
C2 C3 1.391(5) . ?
C3 C4 1.391(5) . ?
C4 C5 1.386(5) . ?
C5 C6 1.391(5) . ?
C1' C6' 1.389(5) . ?
C1' C2' 1.389(5) . ?
C2' C3' 1.405(5) . ?
C3' C4' 1.396(5) . ?
C4' C5' 1.374(6) . ?
C5' C6' 1.391(5) . ?
C1" C2" 1.391(5) . ?
C1" C6" 1.407(5) . ?
C2" C3" 1.402(5) . ?
C3" C4" 1.385(5) . ?
C4" C5" 1.386(6) . ?
C5" C6" 1.380(6) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1S H1SA O2" 0.985(10) 1.653(13) 2.632(4) 172(4) 2_566
O1S H1SB O2' 0.991(10) 1.580(14) 2.561(4) 170(5) 2_565
O1S H1SB O1'A 0.991(10) 1.74(5) 2.49(3) 130(4) 2_565
O2S H2SB O2'A 0.980(11) 1.74(3) 2.72(3) 173(7) 2_676
O2S H2SB O3' 0.980(11) 2.12(5) 2.931(6) 139(6) 2_676
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1" P2 C1 C6 108.2(3) . . . . ?
C1' P2 C1 C6 1.8(4) . . . . ?
C1" P2 C1 C2 -72.3(3) . . . . ?
C1' P2 C1 C2 -178.7(3) . . . . ?
C6 C1 C2 C3 -0.5(5) . . . . ?
P2 C1 C2 C3 180.0(3) . . . . ?
C1 C2 C3 C4 0.0(5) . . . . ?
C1 C2 C3 P1 -179.7(3) . . . . ?
O2 P1 C3 C4 1.5(4) . . . . ?
O3 P1 C3 C4 -124.4(3) . . . . ?
O1 P1 C3 C4 123.7(3) . . . . ?
O2 P1 C3 C2 -178.7(3) . . . . ?
O3 P1 C3 C2 55.4(3) . . . . ?
O1 P1 C3 C2 -56.5(3) . . . . ?
C2 C3 C4 C5 0.6(5) . . . . ?
P1 C3 C4 C5 -179.6(3) . . . . ?
C3 C4 C5 C6 -0.8(5) . . . . ?
C2 C1 C6 C5 0.3(5) . . . . ?
P2 C1 C6 C5 179.7(3) . . . . ?
C4 C5 C6 C1 0.4(5) . . . . ?
C1" P2 C1' C6' 13.8(3) . . . . ?
C1 P2 C1' C6' 117.4(3) . . . . ?
C1" P2 C1' C2' -174.4(3) . . . . ?
C1 P2 C1' C2' -70.7(3) . . . . ?
C6' C1' C2' C3' -1.9(5) . . . . ?
P2 C1' C2' C3' -174.2(3) . . . . ?
C1' C2' C3' C4' 2.1(5) . . . . ?
C1' C2' C3' P1' -176.3(3) . . . . ?
O1' P1' C3' C4' -65.5(3) . . . . ?
O2'A P1' C3' C4' 111.1(12) . . . . ?
O2' P1' C3' C4' 57.4(3) . . . . ?
O1'A P1' C3' C4' -8.1(12) . . . . ?
O3'A P1' C3' C4' -122.6(12) . . . . ?
O3' P1' C3' C4' 173.8(3) . . . . ?
O1' P1' C3' C2' 112.9(3) . . . . ?
O2'A P1' C3' C2' -70.4(12) . . . . ?
O2' P1' C3' C2' -124.2(3) . . . . ?
O1'A P1' C3' C2' 170.4(12) . . . . ?
O3'A P1' C3' C2' 55.9(12) . . . . ?
O3' P1' C3' C2' -7.7(3) . . . . ?
C2' C3' C4' C5' -1.2(5) . . . . ?
P1' C3' C4' C5' 177.4(3) . . . . ?
C3' C4' C5' C6' 0.0(6) . . . . ?
C2' C1' C6' C5' 0.7(5) . . . . ?
P2 C1' C6' C5' 172.5(3) . . . . ?
C4' C5' C6' C1' 0.2(6) . . . . ?
C1 P2 C1" C2" 128.0(3) . . . . ?
C1' P2 C1" C2" -124.4(3) . . . . ?
C1 P2 C1" C6" -50.0(3) . . . . ?
C1' P2 C1" C6" 57.6(3) . . . . ?
C6" C1" C2" C3" 0.1(5) . . . . ?
P2 C1" C2" C3" -178.0(3) . . . . ?
C1" C2" C3" C4" -2.2(5) . . . . ?
C1" C2" C3" P1" 175.5(3) . . . . ?
O2" P1" C3" C4" -121.4(3) . . . . ?
O3" P1" C3" C4" 118.6(3) . . . . ?
O1" P1" C3" C4" 1.1(4) . . . . ?
O2" P1" C3" C2" 61.0(3) . . . . ?
O3" P1" C3" C2" -59.1(3) . . . . ?
O1" P1" C3" C2" -176.6(3) . . . . ?
C2" C3" C4" C5" 2.0(5) . . . . ?
P1" C3" C4" C5" -175.6(3) . . . . ?
C3" C4" C5" C6" 0.2(6) . . . . ?
C4" C5" C6" C1" -2.3(6) . . . . ?
C2" C1" C6" C5" 2.1(5) . . . . ?
P2 C1" C6" C5" -179.9(3) . . . . ?
