#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:41:47 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178663 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/74/4077476.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_4077476
loop_
_publ_author_name
'Clegg, William'
'Izod, Keith'
'Liddle, Stephen T.'
'O'Shaughness, Paul'
'Sheffield, Joanne M.'
_publ_section_title
;
 Synthesis and Structural Characterization of the First Lanthanide(II)
 Cuboidal Cluster. Unexpected C−O Activation by an Unchanged
 Ytterbium(II) Center
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2090
_journal_paper_doi               10.1021/om000057u
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C38 H72 O4 P2 Si4 Yb'
_chemical_formula_weight         940.30
_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                 118.11(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.546(5)
_cell_length_b                   18.212(4)
_cell_length_c                   12.838(8)
_cell_measurement_reflns_used    14608
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.17
_cell_measurement_theta_min      1.87
_cell_volume                     2587(2)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_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  0.0595
_diffrn_reflns_av_sigmaI/netI    0.0696
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12527
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.992
_exptl_absorpt_correction_T_max  0.8133
_exptl_absorpt_correction_T_min  0.4347
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         5.075
_refine_diff_density_min         -3.359
_refine_diff_density_rms         0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4295
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0693
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1306P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1822
_refine_ls_wR_factor_ref         0.1892
_reflns_number_gt                2895
_reflns_number_total             4295
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000057u.cif
_cod_data_source_block           ki45
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4077476
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Yb Yb 0.5000 0.5000 0.5000 0.0304(2) Uani 1 2 d S . .
P P 0.5518(2) 0.59185(13) 0.3381(2) 0.0323(6) Uani 1 1 d . . .
Si2 Si 0.7050(3) 0.49815(14) 0.2506(3) 0.0508(8) Uani 1 1 d . . .
Si1 Si 0.6893(2) 0.68137(13) 0.2317(2) 0.0365(6) Uani 1 1 d . . .
O1 O 0.3784(6) 0.6156(3) 0.4355(6) 0.0406(16) Uani 1 1 d . . .
C1 C 0.6129(8) 0.5877(5) 0.2248(8) 0.035(2) Uani 1 1 d . . .
H1 H 0.5413 0.5839 0.1446 0.042 Uiso 1 1 calc R . .
C2 C 0.7239(11) 0.6916(7) 0.1022(10) 0.066(3) Uani 1 1 d . . .
H2A H 0.7895 0.6581 0.1132 0.099 Uiso 1 1 calc R . .
H2B H 0.7485 0.7423 0.0990 0.099 Uiso 1 1 calc R . .
H2C H 0.6516 0.6797 0.0283 0.099 Uiso 1 1 calc R . .
C3 C 0.5904(10) 0.7643(5) 0.2217(10) 0.054(3) Uani 1 1 d . . .
H3A H 0.5173 0.7641 0.1449 0.081 Uiso 1 1 calc R . .
H3B H 0.6357 0.8097 0.2301 0.081 Uiso 1 1 calc R . .
H3C H 0.5677 0.7614 0.2849 0.081 Uiso 1 1 calc R . .
C4 C 0.8417(9) 0.6883(6) 0.3806(10) 0.053(3) Uani 1 1 d . . .
H4A H 0.8251 0.6824 0.4475 0.079 Uiso 1 1 calc R . .
H4B H 0.8788 0.7364 0.3854 0.079 Uiso 1 1 calc R . .
H4C H 0.8970 0.6495 0.3830 0.079 Uiso 1 1 calc R . .
C5 C 0.5957(12) 0.4162(6) 0.1863(13) 0.070(4) Uani 1 1 d . . .
H5A H 0.5425 0.4243 0.1019 0.106 Uiso 1 1 calc R . .
H5B H 0.5469 0.4117 0.2272 0.106 Uiso 1 1 calc R . .
H5C H 0.6422 0.3710 0.1972 0.106 Uiso 1 1 calc R . .
C6 C 0.8144(12) 0.4801(7) 0.4146(12) 0.065(4) Uani 1 1 d . . .
H6A H 0.8614 0.4356 0.4219 0.098 Uiso 1 1 calc R . .
H6B H 0.7683 0.4735 0.4578 0.098 Uiso 1 1 calc R . .
H6C H 0.8693 0.5219 0.4475 0.098 Uiso 1 1 calc R . .
C7 C 0.7986(16) 0.5011(6) 0.1667(19) 0.085(6) Uani 1 1 d . . .
H7A H 0.7439 0.5037 0.0816 0.128 Uiso 1 1 calc R . .
H7B H 0.8483 0.4567 0.1845 0.128 Uiso 1 1 calc R . .
H7C H 0.8510 0.5445 0.1914 0.128 Uiso 1 1 calc R . .
C8 C 0.3924(8) 0.6249(5) 0.2496(9) 0.037(2) Uani 1 1 d . . .
C9 C 0.3289(8) 0.6423(5) 0.1246(9) 0.042(2) Uani 1 1 d . . .
H9 H 0.3729 0.6430 0.0813 0.050 Uiso 1 1 calc R . .
C10 C 0.2044(10) 0.6584(6) 0.0653(11) 0.058(3) Uani 1 1 d . . .
H10 H 0.1659 0.6669 -0.0175 0.070 Uiso 1 1 calc R . .
C11 C 0.1361(8) 0.6621(5) 0.1259(9) 0.047(3) Uani 1 1 d . . .
H11 H 0.0521 0.6728 0.0845 0.057 Uiso 1 1 calc R . .
C12 C 0.1941(9) 0.6497(5) 0.2502(10) 0.045(3) Uani 1 1 d . . .
C13 C 0.1208(9) 0.6535(6) 0.3173(11) 0.060(3) Uani 1 1 d . . .
H13A H 0.1135 0.6041 0.3438 0.089 Uiso 1 1 calc R . .
H13B H 0.0401 0.6729 0.2651 0.089 Uiso 1 1 calc R . .
H13C H 0.1618 0.6858 0.3859 0.089 Uiso 1 1 calc R . .
C14 C 0.3195(8) 0.6312(5) 0.3073(8) 0.034(2) Uani 1 1 d . . .
C15 C 0.4343(11) 0.6833(6) 0.5048(10) 0.056(3) Uani 1 1 d . . .
H15A H 0.5018 0.6985 0.4914 0.084 Uiso 1 1 calc R . .
H15B H 0.4640 0.6733 0.5890 0.084 Uiso 1 1 calc R . .
H15C H 0.3738 0.7225 0.4795 0.084 Uiso 1 1 calc R . .
O2 O 0.6757(6) 0.5633(4) 0.6701(6) 0.0526(19) Uani 1 1 d DU . .
C16 C 0.7796(11) 0.6013(9) 0.6658(10) 0.084(4) Uani 1 1 d DU A .
H16A H 0.7575 0.6523 0.6371 0.101 Uiso 0.56(2) 1 calc PR A 1
H16B H 0.8034 0.5749 0.6126 0.101 Uiso 0.56(2) 1 calc PR A 1
H16C H 0.8341 0.5652 0.6577 0.101 Uiso 0.44(2) 1 calc PR A 2
H16D H 0.7502 0.6359 0.5985 0.101 Uiso 0.44(2) 1 calc PR A 2
C17 C 0.8810(17) 0.6007(19) 0.7905(16) 0.087(8) Uani 0.56(2) 1 d PDU A 1
H17A H 0.9507 0.5728 0.7947 0.105 Uiso 0.56(2) 1 calc PR A 1
H17B H 0.9078 0.6515 0.8177 0.105 Uiso 0.56(2) 1 calc PR A 1
C18 C 0.8353(16) 0.5656(14) 0.8655(14) 0.069(6) Uani 0.56(2) 1 d PDU A 1
H18A H 0.8658 0.5914 0.9422 0.082 Uiso 0.56(2) 1 calc PR A 1
H18B H 0.8604 0.5135 0.8805 0.082 Uiso 0.56(2) 1 calc PR A 1
C19 C 0.6985(17) 0.5720(16) 0.7950(13) 0.063(6) Uani 0.56(2) 1 d PDU A 1
H19A H 0.6580 0.5327 0.8168 0.075 Uiso 0.56(2) 1 calc PR A 1
H19B H 0.6702 0.6203 0.8073 0.075 Uiso 0.56(2) 1 calc PR A 1
C17X C 0.844(3) 0.6418(18) 0.781(2) 0.068(7) Uani 0.44(2) 1 d PDU A 2
H17C H 0.9306 0.6286 0.8218 0.082 Uiso 0.44(2) 1 calc PR A 2
H17D H 0.8365 0.6955 0.7673 0.082 Uiso 0.44(2) 1 calc PR A 2
C18X C 0.785(3) 0.6192(14) 0.8522(19) 0.061(6) Uani 0.44(2) 1 d PDU A 2
H18C H 0.7239 0.6560 0.8463 0.074 Uiso 0.44(2) 1 calc PR A 2
H18D H 0.8449 0.6132 0.9363 0.074 Uiso 0.44(2) 1 calc PR A 2
C19X C 0.724(3) 0.5463(14) 0.7993(14) 0.058(7) Uani 0.44(2) 1 d PDU A 2
H19C H 0.7834 0.5055 0.8248 0.069 Uiso 0.44(2) 1 calc PR A 2
H19D H 0.6589 0.5346 0.8190 0.069 Uiso 0.44(2) 1 calc PR A 2
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'
Si Si 0.0817 0.0704 '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'
Yb Yb -0.3850 5.5486 '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
O1 Yb O1 180.000(1) . 3_666
O1 Yb O2 87.2(2) . 3_666
O1 Yb O2 92.8(2) 3_666 3_666
O1 Yb O2 92.8(2) . .
O1 Yb O2 87.2(2) 3_666 .
O2 Yb O2 180.000(1) 3_666 .
O1 Yb P 113.91(15) . 3_666
O1 Yb P 66.09(15) 3_666 3_666
O2 Yb P 87.63(16) 3_666 3_666
O2 Yb P 92.37(16) . 3_666
O1 Yb P 66.09(15) . .
O1 Yb P 113.91(15) 3_666 .
O2 Yb P 92.37(16) 3_666 .
O2 Yb P 87.63(16) . .
P Yb P1 180.0 3_666 .
C8 P C1 104.1(4) . .
C8 P Yb 94.7(3) . .
C1 P Yb 142.9(3) . .
C6 Si2 C7 107.9(8) . .
C6 Si2 C5 109.4(6) . .
C7 Si2 C5 106.2(6) . .
C6 Si2 C1 113.1(5) . .
C7 Si2 C1 110.6(5) . .
C5 Si2 C1 109.4(5) . .
C2 Si1 C3 105.6(5) . .
C2 Si1 C1 110.8(5) . .
C3 Si1 C1 113.6(4) . .
C2 Si1 C4 108.8(5) . .
C3 Si1 C4 108.4(5) . .
C1 Si1 C4 109.5(4) . .
C14 O1 C15 110.8(7) . .
C14 O1 Yb 115.8(5) . .
C15 O1 Yb 117.2(6) . .
P C1 Si2 108.6(5) . .
P C1 Si1 107.0(5) . .
Si2 C1 Si1 119.4(5) . .
C14 C8 C9 113.9(8) . .
C14 C8 P 118.2(7) . .
C9 C8 P 127.9(7) . .
C10 C9 C8 122.3(10) . .
C11 C10 C9 121.4(10) . .
C10 C11 C12 119.3(9) . .
C14 C12 C11 118.0(9) . .
C14 C12 C13 122.1(10) . .
C11 C12 C13 119.8(9) . .
C8 C14 C12 124.9(9) . .
C8 C14 O1 117.2(7) . .
C12 C14 O1 117.9(8) . .
C19 O2 C16 105.1(10) . .
C19 O2 C19X 21.4(17) . .
C16 O2 C19X 103.1(12) . .
C19 O2 Yb 128.3(8) . .
C16 O2 Yb 126.6(6) . .
C19X O2 Yb 126.3(9) . .
C17X C16 O2 105.3(10) . .
C17X C16 C17 33.2(16) . .
O2 C16 C17 105.8(10) . .
C18 C17 C16 107.6(11) . .
C17 C18 C19 104.7(12) . .
O2 C19 C18 102.8(12) . .
C18X C17X C16 106.2(11) . .
C17X C18X C19X 104.7(14) . .
O2 C19X C18X 99.8(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Yb O1 2.502(6) .
Yb O1 2.502(6) 3_666
Yb O2 2.535(7) 3_666
Yb O2 2.535(7) .
Yb P 2.969(3) 3_666
Yb P 2.969(3) .
P C8 1.873(10) .
P C1 1.939(9) .
Si2 C6 1.923(14) .
Si2 C7 1.932(12) .
Si2 C5 1.930(11) .
Si2 C1 1.935(10) .
Si1 C2 1.915(11) .
Si1 C3 1.920(10) .
Si1 C1 1.938(9) .
Si1 C4 1.970(11) .
O1 C14 1.479(11) .
O1 C15 1.487(11) .
C8 C14 1.427(13) .
C8 C9 1.451(13) .
C9 C10 1.409(14) .
C10 C11 1.405(15) .
C11 C12 1.426(14) .
C12 C14 1.428(12) .
C12 C13 1.529(14) .
O2 C19 1.498(15) .
O2 C16 1.499(11) .
O2 C19X 1.504(15) .
C16 C17X 1.500(18) .
C16 C17 1.504(17) .
C17 C18 1.48(2) .
C18 C19 1.521(19) .
C17X C18X 1.48(2) .
C18X C19X 1.520(19) .
