#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:20:14 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179785 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/81/7008161.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_7008161
loop_
_publ_author_name
'Baber, R. Angharad'
'Clarke, Matthew L.'
'Heslop, Katie M.'
'Marr, Andrew C.'
'Orpen, A. Guy'
'Pringle, Paul G.'
'Ward, Andrew'
'Zambrano-Williams, Damaris E'
_publ_section_title
;
 Phenylphosphatrioxa-adamantanes: bulky, robust, electron-poor ligands
 that give very efficient rhodium(I) hydroformylation catalysts.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1079
_journal_page_last               1085
_journal_paper_doi               10.1039/b418259f
_journal_year                    2005
_chemical_formula_moiety         'C32 H42 Cl2 O6 P2 Pd, 2(C H2 Cl2)'
_chemical_formula_sum            'C34 H46 Cl6 O6 P2 Pd'
_chemical_formula_weight         931.75
_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                90.03(3)
_cell_angle_beta                 103.56(3)
_cell_angle_gamma                108.26(3)
_cell_formula_units_Z            1
_cell_length_a                   7.6097(15)
_cell_length_b                   10.758(2)
_cell_length_c                   12.984(3)
_cell_measurement_reflns_used    3501
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.3
_cell_measurement_theta_min      2.672
_cell_volume                     978.1(4)
_computing_cell_refinement       'SAINT (Bruker-AXS, 2001)'
_computing_data_collection       'SMART (Bruker-AXS, 2001)'
_computing_data_reduction        'SHELXTL (Bruker-AXS, 2001)'
_computing_molecular_graphics    'SHELXTL (Bruker-AXS, 2001)'
_computing_publication_material  'SHELXTL (Bruker-AXS, 2001)'
_computing_structure_refinement  'SHELXTL (Bruker-AXS, 2001)'
_computing_structure_solution    'SHELXTL (Bruker-AXS, 2001)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'ω scans'
_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  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11262
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    1.008
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.895
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         4471
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0334
_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)+(0.0424P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0814
_reflns_number_gt                3883
_reflns_number_total             4471
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b418259f.txt
_cod_data_source_block           meso-2a.2CH2Cl2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7008161
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
Pd1 Pd 0.0000 0.0000 0.0000 0.00905(8) Uani 1 2 d S . .
P1 P -0.12623(9) 0.10193(6) -0.14477(5) 0.01016(14) Uani 1 1 d . . .
O1 O -0.3114(2) -0.09487(16) -0.30258(13) 0.0119(3) Uani 1 1 d . . .
O2 O -0.2161(3) 0.02988(17) -0.44042(13) 0.0145(4) Uani 1 1 d . . .
O3 O -0.0473(2) 0.21788(16) -0.32342(13) 0.0131(4) Uani 1 1 d . . .
C1 C -0.1803(3) 0.2446(2) -0.10386(19) 0.0123(5) Uani 1 1 d . . .
C2 C -0.1358(4) 0.3645(2) -0.1499(2) 0.0148(5) Uani 1 1 d . . .
H2A H -0.0716 0.3757 -0.2037 0.018 Uiso 1 1 calc R . .
C3 C -0.1878(4) 0.4668(2) -0.1151(2) 0.0172(5) Uani 1 1 d . . .
H3A H -0.1566 0.5468 -0.1451 0.021 Uiso 1 1 calc R . .
C4 C -0.2859(4) 0.4505(3) -0.0360(2) 0.0174(5) Uani 1 1 d . . .
H4A H -0.3219 0.5190 -0.0138 0.021 Uiso 1 1 calc R . .
C5 C -0.3301(4) 0.3321(3) 0.0101(2) 0.0169(5) Uani 1 1 d . . .
H5A H -0.3967 0.3210 0.0628 0.020 Uiso 1 1 calc R . .
C6 C -0.2754(4) 0.2305(2) -0.0224(2) 0.0153(5) Uani 1 1 d . . .
H6A H -0.3021 0.1522 0.0102 0.018 Uiso 1 1 calc R . .
C7 C 0.0298(3) 0.1476(2) -0.24012(19) 0.0126(5) Uani 1 1 d . . .
C8 C 0.0273(3) 0.0170(2) -0.28872(19) 0.0133(5) Uani 1 1 d . . .
H8A H 0.1234 0.0335 -0.3291 0.016 Uiso 1 1 calc R . .
H8B H 0.0581 -0.0376 -0.2324 0.016 Uiso 1 1 calc R . .
C9 C -0.1686(4) -0.0552(2) -0.36145(19) 0.0135(5) Uani 1 1 d . . .
C10 C -0.2272(4) 0.1462(2) -0.39261(19) 0.0140(5) Uani 1 1 d . . .
C11 C -0.3472(3) 0.0102(2) -0.25117(19) 0.0114(5) Uani 1 1 d . . .
C12 C -0.3856(4) 0.1056(2) -0.33426(19) 0.0127(5) Uani 1 1 d . . .
H12A H -0.5070 0.0640 -0.3849 0.015 Uiso 1 1 calc R . .
H12B H -0.3935 0.1829 -0.2996 0.015 Uiso 1 1 calc R . .
C26 C -0.5167(3) -0.0525(2) -0.2053(2) 0.0145(5) Uani 1 1 d . . .
H26A H -0.6256 -0.0978 -0.2617 0.022 Uiso 1 1 calc R . .
H26B H -0.5446 0.0142 -0.1693 0.022 Uiso 1 1 calc R . .
H26C H -0.4874 -0.1138 -0.1559 0.022 Uiso 1 1 calc R . .
C27 C -0.2630(4) 0.2346(3) -0.4799(2) 0.0184(6) Uani 1 1 d . . .
H27A H -0.1598 0.2564 -0.5143 0.028 Uiso 1 1 calc R . .
H27B H -0.2714 0.3135 -0.4499 0.028 Uiso 1 1 calc R . .
H27C H -0.3806 0.1900 -0.5309 0.028 Uiso 1 1 calc R . .
C29 C 0.2308(3) 0.2358(2) -0.1879(2) 0.0158(5) Uani 1 1 d . . .
H29A H 0.3041 0.2562 -0.2402 0.024 Uiso 1 1 calc R . .
H29B H 0.2899 0.1915 -0.1330 0.024 Uiso 1 1 calc R . .
H29C H 0.2255 0.3156 -0.1575 0.024 Uiso 1 1 calc R . .
C31 C -0.1736(4) -0.1779(3) -0.4196(2) 0.0178(5) Uani 1 1 d . . .
H31A H -0.0816 -0.1557 -0.4617 0.027 Uiso 1 1 calc R . .
H31B H -0.2988 -0.2184 -0.4650 0.027 Uiso 1 1 calc R . .
H31C H -0.1435 -0.2379 -0.3691 0.027 Uiso 1 1 calc R . .
C98 C 0.5708(5) -0.5829(3) 0.2777(3) 0.0375(8) Uani 1 1 d . . .
H98A H 0.5325 -0.5489 0.2099 0.045 Uiso 1 1 calc R . .
H98B H 0.4895 -0.6732 0.2749 0.045 Uiso 1 1 calc R . .
Cl1 Cl 0.18298(9) 0.20643(6) 0.07596(5) 0.01610(14) Uani 1 1 d . . .
Cl96 Cl 0.53962(18) -0.48955(9) 0.37921(8) 0.0574(3) Uani 1 1 d . . .
Cl97 Cl 0.81103(13) -0.57839(9) 0.29900(7) 0.0446(2) 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'
Pd Pd -0.9988 1.0072 '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
Cl1 Pd1 Cl1 180.00(4) . 2 ?
Cl1 Pd1 P1 87.10(4) . . ?
Cl1 Pd1 P1 92.90(4) 2 . ?
Cl1 Pd1 P1 92.90(4) . 2 ?
Cl1 Pd1 P1 87.10(4) 2 2 ?
P1 Pd1 P1 180.00(3) . 2 ?
C1 P1 C7 110.04(11) . . ?
C1 P1 C11 103.42(11) . . ?
C7 P1 C11 94.02(11) . . ?
C1 P1 Pd1 112.42(8) . . ?
C7 P1 Pd1 112.98(8) . . ?
C11 P1 Pd1 122.19(8) . . ?
C9 O1 C11 115.62(18) . . ?
C10 O2 C9 111.08(18) . . ?
C10 O3 C7 116.13(18) . . ?
C6 C1 C2 119.0(2) . . ?
C6 C1 P1 116.83(18) . . ?
C2 C1 P1 124.11(19) . . ?
C3 C2 C1 119.9(2) . . ?
C3 C2 H2A 120.1 . . ?
C1 C2 H2A 120.1 . . ?
C4 C3 C2 120.5(2) . . ?
C4 C3 H3A 119.8 . . ?
C2 C3 H3A 119.8 . . ?
C5 C4 C3 120.0(2) . . ?
C5 C4 H4A 120.0 . . ?
C3 C4 H4A 120.0 . . ?
C6 C5 C4 120.0(2) . . ?
C6 C5 H5A 120.0 . . ?
C4 C5 H5A 120.0 . . ?
C5 C6 C1 120.6(2) . . ?
C5 C6 H6A 119.7 . . ?
C1 C6 H6A 119.7 . . ?
O3 C7 C29 106.47(19) . . ?
O3 C7 C8 108.9(2) . . ?
C29 C7 C8 112.3(2) . . ?
O3 C7 P1 110.77(16) . . ?
C29 C7 P1 112.99(17) . . ?
C8 C7 P1 105.43(16) . . ?
C9 C8 C7 110.8(2) . . ?
C9 C8 H8A 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
O1 C9 O2 110.43(19) . . ?
O1 C9 C31 106.5(2) . . ?
O2 C9 C31 107.0(2) . . ?
O1 C9 C8 111.27(19) . . ?
O2 C9 C8 108.59(19) . . ?
C31 C9 C8 112.9(2) . . ?
O3 C10 O2 110.3(2) . . ?
O3 C10 C27 105.6(2) . . ?
O2 C10 C27 107.7(2) . . ?
O3 C10 C12 112.11(19) . . ?
O2 C10 C12 108.1(2) . . ?
C27 C10 C12 113.0(2) . . ?
O1 C11 C26 106.67(19) . . ?
O1 C11 C12 108.18(19) . . ?
C26 C11 C12 112.6(2) . . ?
O1 C11 P1 109.11(16) . . ?
C26 C11 P1 112.05(17) . . ?
C12 C11 P1 108.09(16) . . ?
C10 C12 C11 110.59(19) . . ?
C10 C12 H12A 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
C11 C26 H26A 109.5 . . ?
C11 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C11 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C10 C27 H27A 109.5 . . ?
C10 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C10 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C7 C29 H29A 109.5 . . ?
C7 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C7 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C9 C31 H31A 109.5 . . ?
C9 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C9 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
Cl96 C98 Cl97 111.54(19) . . ?
Cl96 C98 H98A 109.3 . . ?
Cl97 C98 H98A 109.3 . . ?
Cl96 C98 H98B 109.3 . . ?
Cl97 C98 H98B 109.3 . . ?
H98A C98 H98B 108.0 . . ?
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
Pd1 Cl1 2.2934(11) . ?
Pd1 Cl1 2.2934(11) 2 ?
Pd1 P1 2.3395(9) . ?
Pd1 P1 2.3395(9) 2 ?
P1 C1 1.818(3) . ?
P1 C7 1.873(3) . ?
P1 C11 1.892(3) . ?
O1 C9 1.430(3) . ?
O1 C11 1.440(3) . ?
O2 C10 1.432(3) . ?
O2 C9 1.433(3) . ?
O3 C10 1.427(3) . ?
O3 C7 1.438(3) . ?
C1 C6 1.398(3) . ?
C1 C2 1.400(3) . ?
C2 C3 1.388(4) . ?
C2 H2A 0.9300 . ?
C3 C4 1.386(4) . ?
C3 H3A 0.9300 . ?
C4 C5 1.385(4) . ?
C4 H4A 0.9300 . ?
C5 C6 1.383(4) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
C7 C29 1.518(3) . ?
C7 C8 1.533(3) . ?
C8 C9 1.527(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C31 1.506(4) . ?
C10 C27 1.510(3) . ?
C10 C12 1.522(3) . ?
C11 C26 1.513(3) . ?
C11 C12 1.531(3) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C98 Cl96 1.760(4) . ?
C98 Cl97 1.768(4) . ?
C98 H98A 0.9700 . ?
C98 H98B 0.9700 . ?
