#------------------------------------------------------------------------------
#$Date: 2016-03-21 08:33:43 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178608 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/19/4071983.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_4071983
loop_
_publ_author_name
'Deacon, Glen B.'
'Forsyth, Craig M.'
'Jaroschik, Florian'
'Junk, Peter C.'
'Kay, Danielle L.'
'Maschmeyer, Thomas'
'Masters, Anthony F.'
'Wang, Jun'
'Field, Leslie D.'
_publ_section_title
;
 Accessing Decaphenylmetallocenes of Ytterbium, Calcium, and Barium by
 Desolvation of Solvent-Separated Ion Pairs: Overcoming Adverse Solubility
 Properties#
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4772
_journal_paper_doi               10.1021/om800501z
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C70 H50 Yb'
_chemical_formula_sum            'C70 H50 Yb'
_chemical_formula_weight         1064.14
_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                 95.586(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.3460(2)
_cell_length_b                   13.4649(3)
_cell_length_c                   18.1324(4)
_cell_measurement_temperature    123(2)
_cell_volume                     2513.99(9)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    X-Seed
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KAPPA CCD'
_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  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0397
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32280
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.81
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.904
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SORTAV
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         5769
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0302
_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)+(0.0374P)²+0.0383P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0647
_refine_ls_wR_factor_ref         0.0741
_reflns_number_gt                3947
_reflns_number_total             5769
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800501z_si_003.cif
_cod_data_source_block           ybph5gab
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4071983
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
Yb1 Yb 0.0000 0.5000 0.0000 0.04277(8) Uani 1 2 d S
C1 C -0.2288(2) 0.58038(16) 0.02473(12) 0.0226(5) Uani 1 1 d .
C2 C -0.2549(2) 0.47834(15) 0.00678(13) 0.0234(5) Uani 1 1 d .
C3 C -0.1927(2) 0.41897(16) 0.06540(13) 0.0246(5) Uani 1 1 d .
C4 C -0.1284(2) 0.48491(15) 0.11912(13) 0.0237(5) Uani 1 1 d .
C5 C -0.1506(2) 0.58386(16) 0.09416(12) 0.0223(5) Uani 1 1 d .
C11 C -0.27764(19) 0.66957(16) -0.01639(12) 0.0236(5) Uani 1 1 d .
C12 C -0.2681(2) 0.68243(18) -0.09200(12) 0.0274(5) Uani 1 1 d .
H12 H -0.2347 0.6302 -0.1198 0.033 Uiso 1 1 calc R
C13 C -0.3069(2) 0.77047(19) -0.12702(13) 0.0350(6) Uani 1 1 d .
H13 H -0.2993 0.7784 -0.1785 0.042 Uiso 1 1 calc R
C14 C -0.3566(2) 0.84693(19) -0.08728(14) 0.0394(6) Uani 1 1 d .
H14 H -0.3823 0.9075 -0.1113 0.047 Uiso 1 1 calc R
C15 C -0.3685(2) 0.83473(18) -0.01236(14) 0.0367(6) Uani 1 1 d .
H15 H -0.4024 0.8870 0.0152 0.044 Uiso 1 1 calc R
C16 C -0.3312(2) 0.74655(16) 0.02212(13) 0.0281(5) Uani 1 1 d .
H16 H -0.3423 0.7381 0.0731 0.034 Uiso 1 1 calc R
C21 C -0.3315(2) 0.44285(16) -0.06154(12) 0.0234(5) Uani 1 1 d .
C22 C -0.2866(2) 0.36661(18) -0.10454(13) 0.0314(5) Uani 1 1 d .
H22 H -0.2070 0.3343 -0.0887 0.038 Uiso 1 1 calc R
C23 C -0.3563(2) 0.33728(18) -0.17012(13) 0.0385(6) Uani 1 1 d .
H23 H -0.3227 0.2870 -0.1996 0.046 Uiso 1 1 calc R
C24 C -0.4748(2) 0.38090(19) -0.19289(13) 0.0398(6) Uani 1 1 d .
H24 H -0.5232 0.3598 -0.2373 0.048 Uiso 1 1 calc R
C25 C -0.5218(2) 0.4552(2) -0.15062(13) 0.0318(6) Uani 1 1 d .
H25 H -0.6034 0.4848 -0.1657 0.038 Uiso 1 1 calc R
C26 C -0.4508(2) 0.48694(14) -0.08626(12) 0.0240(5) Uani 1 1 d .
H26 H -0.4834 0.5395 -0.0584 0.029 Uiso 1 1 calc R
C31 C -0.1890(2) 0.30883(16) 0.07010(12) 0.0252(5) Uani 1 1 d .
C32 C -0.0719(2) 0.25946(17) 0.09098(12) 0.0275(5) Uani 1 1 d .
H32 H 0.0049 0.2975 0.1023 0.033 Uiso 1 1 calc R
C33 C -0.0648(2) 0.15719(18) 0.09551(13) 0.0358(6) Uani 1 1 d .
H33 H 0.0163 0.1257 0.1091 0.043 Uiso 1 1 calc R
C34 C -0.1754(3) 0.10082(19) 0.08030(15) 0.0451(7) Uani 1 1 d .
H34 H -0.1714 0.0305 0.0835 0.054 Uiso 1 1 calc R
C35 C -0.2923(2) 0.14801(18) 0.06033(16) 0.0459(7) Uani 1 1 d .
H35 H -0.3688 0.1095 0.0498 0.055 Uiso 1 1 calc R
C36 C -0.2995(2) 0.25062(17) 0.05543(14) 0.0337(6) Uani 1 1 d .
H36 H -0.3809 0.2815 0.0419 0.040 Uiso 1 1 calc R
C41 C -0.0555(2) 0.45638(17) 0.19037(12) 0.0255(5) Uani 1 1 d .
C42 C 0.0729(2) 0.48681(15) 0.20771(14) 0.0295(5) Uani 1 1 d .
H42 H 0.1144 0.5252 0.1730 0.035 Uiso 1 1 calc R
C43 C 0.1405(3) 0.4618(2) 0.27486(16) 0.0456(8) Uani 1 1 d .
H43 H 0.2282 0.4821 0.2856 0.055 Uiso 1 1 calc R
C44 C 0.0808(4) 0.4078(2) 0.32567(16) 0.0669(11) Uani 1 1 d .
H44 H 0.1268 0.3912 0.3719 0.080 Uiso 1 1 calc R
C45 C -0.0445(4) 0.3778(2) 0.30993(15) 0.0662(10) Uani 1 1 d .
H45 H -0.0853 0.3405 0.3456 0.079 Uiso 1 1 calc R
C46 C -0.1137(3) 0.40096(18) 0.24249(13) 0.0427(7) Uani 1 1 d .
H46 H -0.2007 0.3788 0.2322 0.051 Uiso 1 1 calc R
C51 C -0.10134(19) 0.67453(16) 0.13385(12) 0.0230(5) Uani 1 1 d .
C52 C -0.0394(2) 0.74923(16) 0.09704(13) 0.0270(5) Uani 1 1 d .
H52 H -0.0298 0.7418 0.0458 0.032 Uiso 1 1 calc R
C53 C 0.0083(2) 0.83375(18) 0.13360(14) 0.0348(6) Uani 1 1 d .
H53 H 0.0506 0.8833 0.1075 0.042 Uiso 1 1 calc R
C54 C -0.0055(2) 0.84611(19) 0.20814(14) 0.0377(6) Uani 1 1 d .
H54 H 0.0276 0.9038 0.2335 0.045 Uiso 1 1 calc R
C55 C -0.0680(2) 0.77354(18) 0.24528(13) 0.0347(6) Uani 1 1 d .
H55 H -0.0787 0.7820 0.2963 0.042 Uiso 1 1 calc R
C56 C -0.1152(2) 0.68885(17) 0.20892(12) 0.0280(5) Uani 1 1 d .
H56 H -0.1576 0.6397 0.2354 0.034 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'
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
C3 Yb1 C3 180.0 3_565 .
C3 Yb1 C4 31.35(7) 3_565 3_565
C3 Yb1 C4 148.65(7) . 3_565
C3 Yb1 C4 148.65(7) 3_565 .
C3 Yb1 C4 31.35(7) . .
C4 Yb1 C4 180.0 3_565 .
C3 Yb1 C2 148.78(7) 3_565 .
C3 Yb1 C2 31.22(7) . .
C4 Yb1 C2 128.45(7) 3_565 .
C4 Yb1 C2 51.55(7) . .
C3 Yb1 C2 31.22(7) 3_565 3_565
C3 Yb1 C2 148.78(7) . 3_565
C4 Yb1 C2 51.55(7) 3_565 3_565
C4 Yb1 C2 128.45(7) . 3_565
C2 Yb1 C2 180.00(9) . 3_565
C3 Yb1 C5 51.49(7) 3_565 3_565
C3 Yb1 C5 128.51(7) . 3_565
C4 Yb1 C5 30.91(6) 3_565 3_565
C4 Yb1 C5 149.09(6) . 3_565
C2 Yb1 C5 128.61(6) . 3_565
C2 Yb1 C5 51.39(6) 3_565 3_565
C3 Yb1 C5 128.51(7) 3_565 .
C3 Yb1 C5 51.49(7) . .
C4 Yb1 C5 149.09(6) 3_565 .
C4 Yb1 C5 30.91(6) . .
C2 Yb1 C5 51.39(6) . .
C2 Yb1 C5 128.61(6) 3_565 .
C5 Yb1 C5 180.0 3_565 .
C3 Yb1 C1 51.43(7) 3_565 3_565
C3 Yb1 C1 128.57(7) . 3_565
C4 Yb1 C1 51.23(7) 3_565 3_565
C4 Yb1 C1 128.77(7) . 3_565
C2 Yb1 C1 148.95(6) . 3_565
C2 Yb1 C1 31.05(6) 3_565 3_565
C5 Yb1 C1 30.98(6) 3_565 3_565
C5 Yb1 C1 149.02(6) . 3_565
C3 Yb1 C1 128.57(7) 3_565 .
C3 Yb1 C1 51.43(7) . .
C4 Yb1 C1 128.77(7) 3_565 .
C4 Yb1 C1 51.23(7) . .
C2 Yb1 C1 31.05(6) . .
C2 Yb1 C1 148.95(6) 3_565 .
C5 Yb1 C1 149.02(6) 3_565 .
C5 Yb1 C1 30.98(6) . .
C1 Yb1 C1 180.0 3_565 .
C5 C1 C2 108.05(18) . .
C5 C1 C11 123.68(19) . .
C2 C1 C11 128.18(18) . .
C5 C1 Yb1 74.17(12) . .
C2 C1 Yb1 74.01(12) . .
C11 C1 Yb1 120.55(14) . .
C1 C2 C3 107.81(18) . .
C1 C2 C21 124.94(19) . .
C3 C2 C21 127.2(2) . .
C1 C2 Yb1 74.94(12) . .
C3 C2 Yb1 73.76(12) . .
C21 C2 Yb1 116.54(15) . .
C2 C3 C4 107.70(19) . .
C2 C3 C31 127.4(2) . .
C4 C3 C31 124.9(2) . .
C2 C3 Yb1 75.02(13) . .
C4 C3 Yb1 74.32(13) . .
C31 C3 Yb1 114.83(15) . .
C5 C4 C3 108.36(19) . .
C5 C4 C41 125.1(2) . .
C3 C4 C41 126.53(19) . .
C5 C4 Yb1 75.32(12) . .
C3 C4 Yb1 74.33(13) . .
C41 C4 Yb1 118.50(15) . .
C4 C5 C1 108.09(18) . .
C4 C5 C51 125.54(19) . .
C1 C5 C51 126.38(19) . .
C4 C5 Yb1 73.77(12) . .
C1 C5 Yb1 74.85(12) . .
C51 C5 Yb1 117.63(14) . .
C12 C11 C16 118.0(2) . .
C12 C11 C1 122.9(2) . .
C16 C11 C1 119.01(19) . .
C13 C12 C11 120.8(2) . .
C14 C13 C12 120.2(2) . .
C13 C14 C15 119.7(2) . .
C16 C15 C14 119.9(2) . .
C15 C16 C11 121.3(2) . .
C22 C21 C26 117.6(2) . .
C22 C21 C2 121.6(2) . .
C26 C21 C2 120.8(2) . .
C23 C22 C21 121.0(2) . .
C24 C23 C22 120.4(2) . .
C25 C24 C23 119.5(2) . .
C24 C25 C26 120.4(2) . .
C25 C26 C21 121.1(2) . .
C36 C31 C32 117.2(2) . .
C36 C31 C3 122.4(2) . .
C32 C31 C3 120.4(2) . .
C33 C32 C31 121.9(2) . .
C34 C33 C32 119.9(2) . .
C33 C34 C35 119.2(2) . .
C34 C35 C36 121.0(2) . .
C35 C36 C31 120.8(2) . .
C46 C41 C42 118.1(2) . .
C46 C41 C4 121.1(2) . .
C42 C41 C4 120.8(2) . .
C43 C42 C41 121.0(3) . .
C44 C43 C42 119.9(3) . .
C45 C44 C43 120.0(2) . .
C44 C45 C46 121.1(3) . .
C41 C46 C45 120.0(3) . .
C56 C51 C52 117.5(2) . .
C56 C51 C5 121.6(2) . .
C52 C51 C5 120.89(19) . .
C53 C52 C51 121.5(2) . .
C54 C53 C52 120.1(2) . .
C55 C54 C53 119.3(2) . .
C56 C55 C54 120.7(2) . .
C55 C56 C51 120.9(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Yb1 C3 2.652(2) 3_565
Yb1 C3 2.652(2) .
Yb1 C4 2.652(2) 3_565
Yb1 C4 2.652(2) .
Yb1 C2 2.668(2) .
Yb1 C2 2.668(2) 3_565
Yb1 C5 2.672(2) 3_565
Yb1 C5 2.672(2) .
Yb1 C1 2.680(2) 3_565
Yb1 C1 2.680(2) .
C1 C5 1.429(3) .
C1 C2 1.432(3) .
C1 C11 1.476(3) .
C2 C3 1.432(3) .
C2 C21 1.483(3) .
C3 C4 1.433(3) .
C3 C31 1.486(3) .
C4 C5 1.419(3) .
C4 C41 1.482(3) .
C5 C51 1.482(3) .
C11 C12 1.395(3) .
C11 C16 1.395(3) .
C12 C13 1.385(3) .
C13 C14 1.384(3) .
C14 C15 1.386(3) .
C15 C16 1.379(3) .
C21 C22 1.396(3) .
C21 C26 1.403(3) .
C22 C23 1.387(3) .
C23 C24 1.385(3) .
C24 C25 1.377(3) .
C25 C26 1.385(3) .
C31 C36 1.390(3) .
C31 C32 1.401(3) .
C32 C33 1.381(3) .
C33 C34 1.379(3) .
C34 C35 1.383(3) .
C35 C36 1.386(3) .
C41 C46 1.387(3) .
C41 C42 1.397(3) .
C42 C43 1.386(4) .
C43 C44 1.367(4) .
C44 C45 1.361(4) .
C45 C46 1.391(4) .
C51 C56 1.396(3) .
C51 C52 1.397(3) .
C52 C53 1.384(3) .
C53 C54 1.383(3) .
C54 C55 1.383(3) .
C55 C56 1.382(3) .
