#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:28:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179846 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/42/7014243.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_7014243
loop_
_publ_author_name
'Higham, Lee J.'
'Whittlesey, Michael K.'
'Wood, Paul T.'
_publ_section_title
;
 Water-soluble hydroxyalkylated phosphines: examples of their differing
 behaviour toward ruthenium and rhodium.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4202
_journal_page_last               4208
_journal_paper_doi               10.1039/b411701h
_journal_year                    2004
_chemical_formula_sum            'C30 H40 Cl2 O6 P4 Ru'
_chemical_formula_weight         792.48
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                99.87(2)
_cell_angle_beta                 105.120(10)
_cell_angle_gamma                109.15(2)
_cell_formula_units_Z            1
_cell_length_a                   9.283(2)
_cell_length_b                   10.008(6)
_cell_length_c                   10.5680(10)
_cell_measurement_reflns_used    37
_cell_measurement_temperature    293(2)
_cell_volume                     859.1(6)
_computing_cell_refinement       'Denzo (Otwinowski, 1987)'
_computing_data_collection       'Rigaku Control software'
_computing_data_reduction        'Scalepack (Otwinowski, 1987)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0825
_diffrn_reflns_av_sigmaI/netI    0.1017
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5570
_diffrn_reflns_theta_max         25.59
_diffrn_reflns_theta_min         2.47
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.838
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_description       block
_exptl_crystal_F_000             398
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       0.0480(77)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.010
_refine_ls_goodness_of_fit_obs   1.073
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         2959
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_restrained_S_obs      1.073
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_obs          0.0641
_refine_ls_shift/esd_max         -0.006
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1188P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2084
_refine_ls_wR_factor_obs         0.1666
_reflns_number_observed          2003
_reflns_number_total             2962
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b411701h.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1188P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1188P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7014243
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ru1 Ru 0.0000 0.0000 0.0000 0.0541(4) Uani 1 d S .
Cl1 Cl -0.0571(2) 0.1220(2) 0.1906(2) 0.0709(5) Uani 1 d . .
P1 P -0.1243(2) 0.1086(2) -0.1516(2) 0.0676(5) Uani 1 d . .
H1 H -0.2465(100) 0.0289(101) -0.2988(87) 0.100(26) Uiso 1 d . .
C1 C -0.0172(9) 0.2323(9) -0.2389(7) 0.069(2) Uani 1 d . .
C2 C 0.0153(10) 0.3796(9) -0.2096(9) 0.083(2) Uani 1 d . .
H2 H -0.0154(10) 0.4223(9) -0.1413(9) 0.100 Uiso 1 calc R .
C3 C 0.0948(13) 0.4683(11) -0.2811(11) 0.105(3) Uani 1 d . .
H3 H 0.1160(13) 0.5685(11) -0.2598(11) 0.126 Uiso 1 calc R .
C4 C 0.1394(15) 0.4081(13) -0.3796(11) 0.114(3) Uani 1 d . .
H4 H 0.1932(15) 0.4658(13) -0.4265(11) 0.137 Uiso 1 calc R .
C5 C 0.1040(14) 0.2590(15) -0.4100(11) 0.117(3) Uani 1 d . .
H5 H 0.1336(14) 0.2160(15) -0.4789(11) 0.140 Uiso 1 calc R .
C6 C 0.0261(11) 0.1722(10) -0.3410(9) 0.090(2) Uani 1 d . .
H6 H 0.0028(11) 0.0717(10) -0.3643(9) 0.108 Uiso 1 calc R .
C7 C -0.2402(11) 0.2064(12) -0.0829(11) 0.099(3) Uani 1 d . .
H7A H -0.2998(11) 0.1477(12) -0.0350(11) 0.118 Uiso 1 calc R .
H7B H -0.1644(11) 0.2998(12) -0.0174(11) 0.118 Uiso 1 calc R .
O1 O -0.3484(10) 0.2323(10) -0.1845(8) 0.123(2) Uani 1 d . .
P2 P -0.2505(2) -0.2091(2) -0.0790(2) 0.0617(5) Uani 1 d . .
C11 C -0.4068(9) -0.2311(8) -0.2378(8) 0.071(2) Uani 1 d . .
C12 C -0.3979(11) -0.2877(11) -0.3638(8) 0.091(3) Uani 1 d . .
H12 H -0.3185(11) -0.3238(11) -0.3684(8) 0.110 Uiso 1 calc R .
C13 C -0.5085(14) -0.2901(14) -0.4832(9) 0.111(3) Uani 1 d . .
H13 H -0.4991(14) -0.3251(14) -0.5668(9) 0.134 Uiso 1 calc R .
C14 C -0.6294(12) -0.2427(14) -0.4810(10) 0.110(3) Uani 1 d . .
H14 H -0.7028(12) -0.2462(14) -0.5617(10) 0.132 Uiso 1 calc R .
C15 C -0.6410(11) -0.1897(12) -0.3572(10) 0.097(3) Uani 1 d . .
H15 H -0.7225(11) -0.1560(12) -0.3540(10) 0.116 Uiso 1 calc R .
C16 C -0.5316(10) -0.1855(10) -0.2351(9) 0.080(2) Uani 1 d . .
H16 H -0.5431(10) -0.1519(10) -0.1521(9) 0.096 Uiso 1 calc R .
C17 C -0.2312(11) -0.3890(10) -0.1253(10) 0.092(2) Uani 1 d . .
H17A H -0.1864(11) -0.3915(10) -0.1986(10) 0.110 Uiso 1 calc R .
H17B H -0.1564(11) -0.3980(10) -0.0471(10) 0.110 Uiso 1 calc R .
O2 O -0.3833(9) -0.5106(8) -0.1678(9) 0.126(3) Uani 1 d . .
C18 C -0.3671(10) -0.2449(10) 0.0378(9) 0.080(2) Uani 1 d . .
H18 H -0.3006(10) -0.2691(10) 0.1116(9) 0.096 Uiso 1 calc R .
O3 O -0.3872(9) -0.1212(10) 0.1011(8) 0.079(2) Uani 0.67 d P .
O13 O -0.5136(22) -0.3565(22) -0.0094(18) 0.091(5) Uani 0.33 d P .
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'
Ru Ru -1.2594 0.8363 '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
P1 Ru1 P1 180.0 2 . ?
P1 Ru1 P2 91.45(7) 2 . ?
P1 Ru1 P2 88.55(7) . . ?
P1 Ru1 P2 88.55(7) 2 2 ?
P1 Ru1 P2 91.45(7) . 2 ?
P2 Ru1 P2 180.0 . 2 ?
P1 Ru1 Cl1 87.09(7) 2 . ?
P1 Ru1 Cl1 92.91(7) . . ?
P2 Ru1 Cl1 94.26(7) . . ?
P2 Ru1 Cl1 85.74(7) 2 . ?
P1 Ru1 Cl1 92.92(7) 2 2 ?
P1 Ru1 Cl1 87.08(7) . 2 ?
P2 Ru1 Cl1 85.74(7) . 2 ?
P2 Ru1 Cl1 94.26(7) 2 2 ?
Cl1 Ru1 Cl1 180.0 . 2 ?
H1 P1 C1 82.5(34) . . ?
H1 P1 C7 99.2(31) . . ?
C1 P1 C7 104.3(4) . . ?
H1 P1 Ru1 126.5(34) . . ?
C1 P1 Ru1 124.1(2) . . ?
C7 P1 Ru1 114.1(3) . . ?
C6 C1 C2 118.2(8) . . ?
C6 C1 P1 118.2(6) . . ?
C2 C1 P1 123.5(6) . . ?
C1 C2 C3 121.1(9) . . ?
C4 C3 C2 120.0(9) . . ?
C3 C4 C5 118.6(9) . . ?
C6 C5 C4 121.6(10) . . ?
C1 C6 C5 120.5(9) . . ?
O1 C7 P1 112.7(7) . . ?
C11 P2 C18 102.5(4) . . ?
C11 P2 C17 98.9(4) . . ?
C18 P2 C17 100.3(4) . . ?
C11 P2 Ru1 118.8(3) . . ?
C18 P2 Ru1 118.8(3) . . ?
C17 P2 Ru1 114.2(3) . . ?
C16 C11 C12 118.5(7) . . ?
C16 C11 P2 120.9(6) . . ?
C12 C11 P2 120.5(6) . . ?
C11 C12 C13 119.8(8) . . ?
C14 C13 C12 121.9(9) . . ?
C13 C14 C15 118.6(8) . . ?
C14 C15 C16 121.0(9) . . ?
C11 C16 C15 120.2(8) . . ?
O2 C17 P2 112.0(6) . . ?
O13 C18 O3 106.5(11) . . ?
O13 C18 P2 119.0(9) . . ?
O3 C18 P2 113.5(6) . . ?
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
Ru1 P1 2.352(2) 2 ?
Ru1 P1 2.352(2) . ?
Ru1 P2 2.383(2) . ?
Ru1 P2 2.383(2) 2 ?
Ru1 Cl1 2.443(2) . ?
Ru1 Cl1 2.443(2) 2 ?
P1 H1 1.55(8) . ?
P1 C1 1.853(8) . ?
P1 C7 1.871(9) . ?
C1 C6 1.360(11) . ?
C1 C2 1.365(11) . ?
C2 C3 1.413(12) . ?
C3 C4 1.339(15) . ?
C4 C5 1.38(2) . ?
C5 C6 1.375(13) . ?
C7 O1 1.390(11) . ?
P2 C11 1.834(8) . ?
P2 C18 1.849(8) . ?
P2 C17 1.863(9) . ?
C11 C16 1.382(11) . ?
C11 C12 1.389(11) . ?
C12 C13 1.394(13) . ?
C13 C14 1.358(14) . ?
C14 C15 1.370(14) . ?
C15 C16 1.402(12) . ?
C17 O2 1.426(11) . ?
C18 O13 1.34(2) . ?
C18 O3 1.395(12) . ?
