#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:02:04 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178882 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/11/4111183.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_4111183
loop_
_publ_author_name
'Nathaniel K. Szymczak'
'Lev N. Zakharov'
'David R. Tyler'
_publ_section_title
;
 Solution Chemistry of a Water-Soluble η2-H2 Ruthenium Complex: Evidence
 for Coordinated H2 Acting as a Hydrogen Bond Donor
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15830
_journal_page_last               15835
_journal_paper_doi               10.1021/ja065532f
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C36 H80 Cl2 O8 P4 Ru'
_chemical_formula_sum            'C36 H80 Cl2 O8 P4 Ru'
_chemical_formula_weight         936.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.108(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.6618(18)
_cell_length_b                   10.2967(15)
_cell_length_c                   18.735(3)
_cell_measurement_reflns_used    4830
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.28
_cell_volume                     2321.6(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      273(2)
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18726
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.853
_refine_diff_density_min         -1.566
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         5433
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0611
_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)+(0.0727P)²+6.1473P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1482
_refine_ls_wR_factor_ref         0.1602
_reflns_number_gt                4252
_reflns_number_total             5433
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja065532fsi20060925_072421.cif
_cod_data_source_block           nks2
_cod_database_code               4111183
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, 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
Ru1 Ru 0.0000 0.5000 0.0000 0.02338(14) Uani 1 2 d S
Cl1 Cl 0.18546(8) 0.41082(10) 0.05724(6) 0.0337(3) Uani 1 1 d .
P1 P 0.03257(9) 0.63574(10) 0.10465(6) 0.0277(2) Uani 1 1 d .
P2 P 0.07385(9) 0.67494(10) -0.04888(6) 0.0275(2) Uani 1 1 d .
O1 O 0.0700(3) 0.5515(4) 0.3515(2) 0.0518(9) Uani 1 1 d D
O2 O -0.1869(5) 0.8753(6) 0.2115(4) 0.1035(19) Uani 1 1 d D
O3 O 0.4501(3) 0.7222(5) -0.0218(2) 0.0585(11) Uani 1 1 d D
O4 O 0.0056(4) 0.8698(5) -0.2728(2) 0.0674(12) Uani 1 1 d D
C1 C 0.1352(4) 0.7570(4) 0.0971(3) 0.0398(11) Uani 1 1 d .
H1A H 0.1409 0.8260 0.1333 0.048 Uiso 1 1 calc R
H1B H 0.2077 0.7169 0.1071 0.048 Uiso 1 1 calc R
C2 C 0.0964(4) 0.8118(4) 0.0175(3) 0.0400(11) Uani 1 1 d .
H2A H 0.1522 0.8702 0.0099 0.048 Uiso 1 1 calc R
H2B H 0.0279 0.8602 0.0094 0.048 Uiso 1 1 calc R
C3 C 0.0932(4) 0.5712(4) 0.1996(2) 0.0326(9) Uani 1 1 d .
H3A H 0.0383 0.5156 0.2104 0.039 Uiso 1 1 calc R
H3B H 0.1556 0.5165 0.1996 0.039 Uiso 1 1 calc R
C4 C 0.1336(4) 0.6676(4) 0.2640(3) 0.0390(11) Uani 1 1 d .
H4A H 0.1966 0.7154 0.2583 0.047 Uiso 1 1 calc R
H4B H 0.0749 0.7295 0.2617 0.047 Uiso 1 1 calc R
C5 C 0.1674(4) 0.6017(5) 0.3394(3) 0.0455(12) Uani 1 1 d D
H5A H 0.2193 0.5319 0.3404 0.055 Uiso 1 1 calc R
H5B H 0.2033 0.6634 0.3786 0.055 Uiso 1 1 calc R
C6 C 0.0944(8) 0.4791(7) 0.4194(4) 0.084(2) Uani 1 1 d D
H6A H 0.0265 0.4469 0.4254 0.126 Uiso 1 1 calc R
H6B H 0.1312 0.5341 0.4610 0.126 Uiso 1 1 calc R
H6C H 0.1419 0.4074 0.4174 0.126 Uiso 1 1 calc R
C7 C -0.0774(4) 0.7453(4) 0.1140(3) 0.0389(11) Uani 1 1 d .
H7A H -0.0418 0.8198 0.1434 0.047 Uiso 1 1 calc R
H7B H -0.1183 0.7768 0.0643 0.047 Uiso 1 1 calc R
C8 C -0.1599(5) 0.6913(5) 0.1491(3) 0.0508(13) Uani 1 1 d D
H8A H -0.1186 0.6510 0.1964 0.061 Uiso 1 1 calc R
H8B H -0.2012 0.6230 0.1167 0.061 Uiso 1 1 calc R
C9 C -0.2495(8) 0.7915(8) 0.1657(5) 0.119(4) Uani 1 1 d D
H9A H -0.2942 0.8332 0.1198 0.143 Uiso 1 1 calc R
H9B H -0.2981 0.7470 0.1887 0.143 Uiso 1 1 calc R
C10 C -0.2782(12) 0.9568(11) 0.2230(6) 0.184(8) Uani 1 1 d D
H10A H -0.2466 1.0267 0.2568 0.276 Uiso 1 1 calc R
H10B H -0.3239 0.9044 0.2439 0.276 Uiso 1 1 calc R
H10C H -0.3225 0.9917 0.1756 0.276 Uiso 1 1 calc R
C11 C 0.2116(4) 0.6510(5) -0.0586(3) 0.0373(10) Uani 1 1 d .
H11A H 0.2629 0.6362 -0.0087 0.045 Uiso 1 1 calc R
H11B H 0.2092 0.5714 -0.0868 0.045 Uiso 1 1 calc R
C12 C 0.2621(4) 0.7561(5) -0.0955(3) 0.0418(11) Uani 1 1 d .
H12A H 0.2147 0.7695 -0.1467 0.050 Uiso 1 1 calc R
H12B H 0.2658 0.8371 -0.0684 0.050 Uiso 1 1 calc R
C13 C 0.3773(4) 0.7189(6) -0.0960(3) 0.0479(13) Uani 1 1 d D
H13A H 0.3762 0.6324 -0.1167 0.057 Uiso 1 1 calc R
H13B H 0.4025 0.7792 -0.1271 0.057 Uiso 1 1 calc R
C14 C 0.5579(4) 0.6766(8) -0.0171(4) 0.071(2) Uani 1 1 d D
H14A H 0.6049 0.6804 0.0341 0.106 Uiso 1 1 calc R
H14B H 0.5886 0.7300 -0.0477 0.106 Uiso 1 1 calc R
H14C H 0.5531 0.5884 -0.0345 0.106 Uiso 1 1 calc R
C15 C -0.0086(4) 0.7443(4) -0.1390(3) 0.0356(10) Uani 1 1 d .
H15A H 0.0135 0.7015 -0.1782 0.043 Uiso 1 1 calc R
H15B H -0.0858 0.7221 -0.1467 0.043 Uiso 1 1 calc R
C16 C -0.0023(5) 0.8909(4) -0.1502(3) 0.0432(12) Uani 1 1 d .
H16A H -0.0399 0.9357 -0.1194 0.052 Uiso 1 1 calc R
H16B H 0.0748 0.9181 -0.1339 0.052 Uiso 1 1 calc R
C17 C -0.0553(4) 0.9283(5) -0.2314(3) 0.0454(12) Uani 1 1 d D
H17A H -0.1318 0.8989 -0.2489 0.054 Uiso 1 1 calc R
H17B H -0.0545 1.0220 -0.2370 0.054 Uiso 1 1 calc R
C18 C -0.0357(6) 0.8988(10) -0.3492(4) 0.090(3) Uani 1 1 d D
H18A H 0.0089 0.8563 -0.3753 0.135 Uiso 1 1 calc R
H18B H -0.0333 0.9910 -0.3561 0.135 Uiso 1 1 calc R
H18C H -0.1110 0.8691 -0.3687 0.135 Uiso 1 1 calc R
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
P1 Ru1 P1 180.0 . 3_565
P1 Ru1 P2 83.13(4) . .
P1 Ru1 P2 96.87(4) 3_565 .
P1 Ru1 P2 96.87(4) . 3_565
P1 Ru1 P2 83.13(4) 3_565 3_565
P2 Ru1 P2 180.0 . 3_565
P1 Ru1 Cl1 92.20(4) . 3_565
P1 Ru1 Cl1 87.80(4) 3_565 3_565
P2 Ru1 Cl1 89.16(4) . 3_565
P2 Ru1 Cl1 90.84(4) 3_565 3_565
P1 Ru1 Cl1 87.80(4) . .
P1 Ru1 Cl1 92.20(4) 3_565 .
P2 Ru1 Cl1 90.84(4) . .
P2 Ru1 Cl1 89.16(4) 3_565 .
Cl1 Ru1 Cl1 180.0 3_565 .
C3 P1 C1 103.2(2) . .
C3 P1 C7 103.4(2) . .
C1 P1 C7 99.5(2) . .
C3 P1 Ru1 120.64(14) . .
C1 P1 Ru1 106.63(16) . .
C7 P1 Ru1 120.30(16) . .
C11 P2 C15 104.5(2) . .
C11 P2 C2 102.6(2) . .
C15 P2 C2 104.4(2) . .
C11 P2 Ru1 116.40(15) . .
C15 P2 Ru1 118.53(15) . .
C2 P2 Ru1 108.77(16) . .
C5 O1 C6 112.1(5) . .
C9 O2 C10 97.4(8) . .
C13 O3 C14 112.0(5) . .
C17 O4 C18 112.5(5) . .
C2 C1 P1 107.8(3) . .
C1 C2 P2 108.2(3) . .
C4 C3 P1 118.0(3) . .
C5 C4 C3 112.1(4) . .
O1 C5 C4 107.8(4) . .
C8 C7 P1 117.6(3) . .
C7 C8 C9 117.9(6) . .
O2 C9 C8 103.2(7) . .
C12 C11 P2 119.8(3) . .
C13 C12 C11 111.4(4) . .
O3 C13 C12 108.9(4) . .
C16 C15 P2 118.2(3) . .
C17 C16 C15 111.4(4) . .
O4 C17 C16 107.6(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 P1 2.3377(11) .
Ru1 P1 2.3377(11) 3_565
Ru1 P2 2.3430(11) .
Ru1 P2 2.3430(11) 3_565
Ru1 Cl1 2.4376(10) 3_565
Ru1 Cl1 2.4376(10) .
P1 C3 1.830(4) .
P1 C1 1.839(5) .
P1 C7 1.842(5) .
P2 C11 1.826(5) .
P2 C15 1.831(5) .
P2 C2 1.842(5) .
O1 C5 1.419(6) .
O1 C6 1.423(6) .
O2 C9 1.299(8) .
O2 C10 1.497(9) .
O3 C13 1.410(6) .
O3 C14 1.420(6) .
O4 C17 1.390(6) .
O4 C18 1.394(7) .
C1 C2 1.527(7) .
C3 C4 1.523(6) .
C4 C5 1.505(7) .
C7 C8 1.504(7) .
C8 C9 1.633(9) .
C11 C12 1.527(6) .
C12 C13 1.511(7) .
C15 C16 1.530(6) .
C16 C17 1.510(7) .
