#------------------------------------------------------------------------------
#$Date: 2016-03-21 13:06:47 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178691 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/02/4080277.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_4080277
loop_
_publ_author_name
'Sobaczynski, Adam P.'
'Bauer, Tobias'
'Kempe, Rhett'
_publ_section_title
;
 Heterometallic Hydride Complexes of Rare-Earth Metals and Ruthenium
 through C--H Bond Activation
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1363
_journal_paper_doi               10.1021/om301039g
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C50 H82 O2 P4 Ru2 Y2'
_chemical_formula_weight         1219.00
_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                 113.074(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.7450(7)
_cell_length_b                   25.8100(19)
_cell_length_c                   11.9330(9)
_cell_measurement_reflns_used    10067
_cell_measurement_temperature    133(2)
_cell_volume                     2761.3(4)
_computing_cell_refinement       X-AREA-STOE
_computing_data_collection       X-AREA-STOE
_computing_data_reduction        X-AREA-STOE
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  STOE-IPDSII
_diffrn_measurement_method       Omega-Scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0841
_diffrn_reflns_av_sigmaI/netI    0.2018
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9116
_diffrn_reflns_theta_full        24.59
_diffrn_reflns_theta_max         24.59
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    2.768
_exptl_absorpt_correction_T_max  0.7421
_exptl_absorpt_correction_T_min  0.5025
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.613
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         4627
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.613
_refine_ls_R_factor_all          0.1306
_refine_ls_R_factor_gt           0.0394
_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)+(0.0135P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0843
_reflns_number_gt                1808
_reflns_number_total             4627
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            om301039g_si_003.cif
_cod_data_source_block           t323mpma
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4080277
#BEGIN Tags that were not found in dictionaries:
_cell_measurement_2theta_min     3.16
_cell_measurement_2theta_max     49.83
#END Tags that were not found in dictionaries
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
C1 C 0.7211(9) -0.0231(3) 0.3061(7) 0.053(2) Uani 1 1 d .
H1 H 0.7641 -0.0440 0.2628 0.063 Uiso 1 1 calc R
C2 C 0.5689(9) -0.0113(3) 0.2627(8) 0.056(2) Uani 1 1 d .
H2 H 0.4941 -0.0215 0.1868 0.068 Uiso 1 1 calc R
C3 C 0.5484(10) 0.0185(4) 0.3532(9) 0.067(3) Uani 1 1 d .
H3 H 0.4565 0.0322 0.3502 0.080 Uiso 1 1 calc R
C4 C 0.6864(9) 0.0243(3) 0.4478(8) 0.054(2) Uani 1 1 d .
H4 H 0.7013 0.0424 0.5209 0.065 Uiso 1 1 calc R
C5 C 0.8060(9) -0.0003(3) 0.4237(7) 0.047(2) Uani 1 1 d .
C6 C 0.8051(10) 0.1439(3) 0.1215(9) 0.068(3) Uani 1 1 d .
H6A H 0.8582 0.1681 0.1890 0.082 Uiso 1 1 calc R
H6B H 0.8425 0.1495 0.0564 0.082 Uiso 1 1 calc R
C7 C 0.6392(11) 0.1550(4) 0.0724(8) 0.077(3) Uani 1 1 d .
H7A H 0.5934 0.1448 -0.0145 0.092 Uiso 1 1 calc R
H7B H 0.6233 0.1926 0.0777 0.092 Uiso 1 1 calc R
C8 C 1.0383(8) 0.0730(4) 0.2623(7) 0.064(2) Uani 1 1 d .
H8A H 1.0930 0.1043 0.2552 0.076 Uiso 1 1 calc R
H8B H 1.0831 0.0416 0.2429 0.076 Uiso 1 1 calc R
C9 C 0.8022(10) 0.0415(3) 0.0370(8) 0.071(3) Uani 1 1 d .
H9A H 0.8706 0.0522 -0.0008 0.106 Uiso 1 1 calc R
H9B H 0.6992 0.0485 -0.0191 0.106 Uiso 1 1 calc R
H9C H 0.8143 0.0043 0.0552 0.106 Uiso 1 1 calc R
C10 C 0.3780(9) 0.0947(4) 0.0378(9) 0.084(3) Uani 1 1 d .
H10A H 0.3102 0.0819 0.0742 0.125 Uiso 1 1 calc R
H10B H 0.4035 0.0664 -0.0052 0.125 Uiso 1 1 calc R
H10C H 0.3291 0.1226 -0.0199 0.125 Uiso 1 1 calc R
C11 C 0.4731(10) 0.1708(3) 0.2216(9) 0.079(3) Uani 1 1 d .
H11A H 0.3996 0.1909 0.1555 0.118 Uiso 1 1 calc R
H11B H 0.5543 0.1936 0.2717 0.118 Uiso 1 1 calc R
H11C H 0.4250 0.1555 0.2721 0.118 Uiso 1 1 calc R
C12 C 1.4718(9) 0.2210(3) 0.5818(8) 0.055(2) Uani 1 1 d .
H12A H 1.5056 0.2156 0.5154 0.082 Uiso 1 1 calc R
H12B H 1.5524 0.2120 0.6596 0.082 Uiso 1 1 calc R
H12C H 1.4441 0.2574 0.5833 0.082 Uiso 1 1 calc R
C13 C 1.3893(8) 0.1304(3) 0.5535(8) 0.055(2) Uani 1 1 d .
H13A H 1.3035 0.1069 0.5288 0.083 Uiso 1 1 calc R
H13B H 1.4631 0.1197 0.6332 0.083 Uiso 1 1 calc R
H13C H 1.4345 0.1290 0.4932 0.083 Uiso 1 1 calc R
C14 C 0.9580(9) 0.0886(3) 0.7533(8) 0.060(2) Uani 1 1 d .
H14A H 0.8672 0.0747 0.7585 0.090 Uiso 1 1 calc R
H14B H 1.0445 0.0793 0.8269 0.090 Uiso 1 1 calc R
H14C H 0.9699 0.0741 0.6817 0.090 Uiso 1 1 calc R
C15 C 1.2137(9) 0.2031(3) 0.4387(7) 0.053(2) Uani 1 1 d .
H15A H 1.1233 0.1828 0.4238 0.080 Uiso 1 1 calc R
H15B H 1.2483 0.1968 0.3730 0.080 Uiso 1 1 calc R
H15C H 1.1917 0.2400 0.4413 0.080 Uiso 1 1 calc R
C16 C 0.9001(9) 0.1659(3) 0.8450(8) 0.065(3) Uani 1 1 d .
H16A H 0.8904 0.2037 0.8441 0.098 Uiso 1 1 calc R
H16B H 0.9764 0.1549 0.9233 0.098 Uiso 1 1 calc R
H16C H 0.8044 0.1500 0.8339 0.098 Uiso 1 1 calc R
C17 C 0.8209(8) 0.1641(3) 0.6216(7) 0.056(2) Uani 1 1 d .
H17A H 0.8038 0.2016 0.6208 0.083 Uiso 1 1 calc R
H17B H 0.7294 0.1457 0.6129 0.083 Uiso 1 1 calc R
H17C H 0.8492 0.1549 0.5538 0.083 Uiso 1 1 calc R
C18 C 0.9459(9) 0.1489(3) 0.7416(7) 0.048(2) Uani 1 1 d .
C19 C 1.0937(9) 0.1730(3) 0.7506(8) 0.046(2) Uani 1 1 d .
C20 C 1.1724(10) 0.2066(3) 0.8477(7) 0.050(2) Uani 1 1 d .
H20 H 1.1369 0.2122 0.9104 0.060 Uiso 1 1 calc R
C21 C 1.3012(9) 0.2317(3) 0.8533(8) 0.051(2) Uani 1 1 d .
H21 H 1.3533 0.2542 0.9192 0.061 Uiso 1 1 calc R
C22 C 1.3519(9) 0.2237(3) 0.7640(7) 0.045(2) Uani 1 1 d .
H22 H 1.4400 0.2412 0.7692 0.054 Uiso 1 1 calc R
C23 C 1.2804(9) 0.1908(3) 0.6638(7) 0.042(2) Uani 1 1 d .
C24 C 1.1498(9) 0.1648(3) 0.6599(7) 0.040(2) Uani 1 1 d .
C25 C 1.3368(8) 0.1867(3) 0.5618(7) 0.045(2) Uani 1 1 d .
O1 O 1.0822(5) 0.1301(2) 0.5706(4) 0.0449(14) Uani 1 1 d .
Y1 Y 1.01511(8) 0.06722(4) 0.45473(7) 0.0465(2) Uani 1 1 d .
Ru1 Ru 0.70202(7) 0.06134(3) 0.28577(6) 0.0487(2) Uani 1 1 d .
P1 P 0.5477(3) 0.11957(9) 0.1574(2) 0.0599(7) Uani 1 1 d .
P2 P 0.8435(3) 0.07741(9) 0.1765(2) 0.0550(7) Uani 1 1 d .
H1RU H 0.776(5) 0.1023(19) 0.371(4) 0.007(13) Uiso 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'
Y Y -2.7962 3.5667 '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'
P P 0.1023 0.0942 '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
C2 C1 C5 113.0(8) . .
C2 C1 Ru1 73.2(5) . .
C5 C1 Ru1 72.1(5) . .
C1 C2 C3 106.5(8) . .
C1 C2 Ru1 70.0(5) . .
C3 C2 Ru1 72.3(5) . .
C4 C3 C2 107.5(8) . .
C4 C3 Ru1 70.6(5) . .
C2 C3 Ru1 71.3(5) . .
C3 C4 C5 113.0(8) . .
C3 C4 Ru1 73.3(5) . .
C5 C4 Ru1 71.3(5) . .
C1 C5 C4 99.9(7) . .
C1 C5 Ru1 69.7(5) . .
C4 C5 Ru1 70.5(5) . .
C1 C5 Y1 106.7(5) . 3_756
C4 C5 Y1 128.6(6) . 3_756
Ru1 C5 Y1 160.4(4) . 3_756
C1 C5 Y1 122.1(5) . .
C4 C5 Y1 109.0(6) . .
Ru1 C5 Y1 74.4(2) . .
Y1 C5 Y1 93.0(3) 3_756 .
C7 C6 P2 110.7(6) . .
C6 C7 P1 111.6(6) . .
P2 C8 Y1 94.3(3) . .
C17 C18 C16 107.8(7) . .
C17 C18 C19 110.1(7) . .
C16 C18 C19 112.9(7) . .
C17 C18 C14 110.2(7) . .
C16 C18 C14 104.5(7) . .
C19 C18 C14 111.2(7) . .
C24 C19 C20 118.4(8) . .
C24 C19 C18 121.5(7) . .
C20 C19 C18 120.0(8) . .
C21 C20 C19 121.1(8) . .
C22 C21 C20 119.5(8) . .
C21 C22 C23 123.2(8) . .
C22 C23 C24 116.8(7) . .
C22 C23 C25 120.5(7) . .
C24 C23 C25 122.6(7) . .
O1 C24 C19 119.4(7) . .
O1 C24 C23 119.6(7) . .
C19 C24 C23 121.0(7) . .
C23 C25 C12 113.2(7) . .
C23 C25 C15 110.6(6) . .
C12 C25 C15 106.8(7) . .
C23 C25 C13 110.3(6) . .
C12 C25 C13 105.5(6) . .
C15 C25 C13 110.2(7) . .
C24 O1 Y1 168.1(5) . .
O1 Y1 C8 117.9(3) . .
O1 Y1 C5 101.0(2) . 3_756
C8 Y1 C5 107.1(3) . 3_756
O1 Y1 C5 130.4(2) . .
C8 Y1 C5 105.6(3) . .
C5 Y1 C5 87.0(3) 3_756 .
O1 Y1 Ru1 118.20(14) . .
C8 Y1 Ru1 78.92(18) . .
C5 Y1 Ru1 132.12(19) 3_756 .
C5 Y1 Ru1 47.07(18) . .
O1 Y1 P2 123.28(15) . .
C8 Y1 P2 34.92(18) . .
C5 Y1 P2 130.5(2) 3_756 .
C5 Y1 P2 80.77(19) . .
Ru1 Y1 P2 44.37(5) . .
O1 Y1 Y1 125.82(14) . 3_756
C8 Y1 Y1 112.8(2) . 3_756
C5 Y1 Y1 44.76(18) 3_756 3_756
C5 Y1 Y1 42.28(18) . 3_756
Ru1 Y1 Y1 88.37(3) . 3_756
P2 Y1 Y1 108.90(5) . 3_756
C1 Ru1 C4 60.4(3) . .
C1 Ru1 C5 38.2(3) . .
C4 Ru1 C5 38.1(3) . .
C1 Ru1 C2 36.8(3) . .
C4 Ru1 C2 60.7(3) . .
C5 Ru1 C2 64.3(3) . .
C1 Ru1 C3 60.7(3) . .
C4 Ru1 C3 36.1(3) . .
C5 Ru1 C3 63.8(3) . .
C2 Ru1 C3 36.5(3) . .
C1 Ru1 P1 138.1(2) . .
C4 Ru1 P1 128.8(2) . .
C5 Ru1 P1 165.8(2) . .
C2 Ru1 P1 106.0(2) . .
C3 Ru1 P1 102.2(2) . .
C1 Ru1 P2 101.6(2) . .
C4 Ru1 P2 147.4(2) . .
C5 Ru1 P2 110.6(2) . .
C2 Ru1 P2 122.3(3) . .
C3 Ru1 P2 158.8(3) . .
P1 Ru1 P2 83.20(9) . .
C1 Ru1 Y1 87.4(2) . .
C4 Ru1 Y1 80.3(2) . .
C5 Ru1 Y1 58.6(2) . .
C2 Ru1 Y1 121.7(2) . .
C3 Ru1 Y1 116.1(2) . .
P1 Ru1 Y1 132.24(7) . .
P2 Ru1 Y1 71.54(6) . .
C11 P1 C10 101.3(5) . .
C11 P1 C7 103.5(4) . .
C10 P1 C7 103.3(5) . .
C11 P1 Ru1 118.1(3) . .
C10 P1 Ru1 117.2(3) . .
C7 P1 Ru1 111.6(3) . .
C8 P2 C9 107.5(4) . .
C8 P2 C6 106.9(5) . .
C9 P2 C6 102.2(4) . .
C8 P2 Ru1 114.2(3) . .
C9 P2 Ru1 117.9(3) . .
C6 P2 Ru1 107.0(3) . .
C8 P2 Y1 50.8(2) . .
C9 P2 Y1 141.1(3) . .
C6 P2 Y1 114.5(3) . .
Ru1 P2 Y1 64.09(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.400(10) .
C1 C5 1.446(11) .
C1 Ru1 2.194(8) .
C2 C3 1.403(12) .
C2 Ru1 2.236(8) .
C3 C4 1.384(10) .
C3 Ru1 2.249(9) .
C4 C5 1.451(11) .
C4 Ru1 2.215(9) .
C5 Ru1 2.226(8) .
C5 Y1 2.479(8) 3_756
C5 Y1 2.595(8) .
C6 C7 1.515(11) .
C6 P2 1.823(9) .
C7 P1 1.835(10) .
C8 P2 1.773(8) .
C8 Y1 2.399(7) .
C9 P2 1.808(9) .
C10 P1 1.826(8) .
C11 P1 1.816(9) .
C12 C25 1.525(10) .
C13 C25 1.557(10) .
C14 C18 1.563(11) .
C15 C25 1.548(10) .
C16 C18 1.532(11) .
C17 C18 1.524(10) .
C18 C19 1.534(11) .
C19 C24 1.407(11) .
C19 C20 1.409(11) .
C20 C21 1.391(11) .
C21 C22 1.354(11) .
C22 C23 1.409(10) .
C23 C24 1.424(10) .
C23 C25 1.523(10) .
C24 O1 1.348(8) .
O1 Y1 2.066(5) .
Y1 C5 2.479(8) 3_756
Y1 Ru1 2.9283(10) .
Y1 P2 3.088(2) .
Y1 Y1 3.6803(19) 3_756
Ru1 P1 2.250(2) .
Ru1 P2 2.276(2) .
