#------------------------------------------------------------------------------
#$Date: 2016-03-21 08:33:43 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178608 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/19/4071982.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_4071982
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 Ba'
_chemical_formula_sum            'C70 H50 Ba'
_chemical_formula_weight         1028.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 128.559(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.0103(4)
_cell_length_b                   13.7274(4)
_cell_length_c                   17.9609(4)
_cell_measurement_temperature    123(2)
_cell_volume                     2508.37(14)
_computing_cell_refinement       'Bruker Apex2 v2.0'
_computing_data_collection       'Bruker Apex2 v2.0'
_computing_data_reduction        'Bruker Apex2 v2.0'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker X8 Apex 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  0.0661
_diffrn_reflns_av_sigmaI/netI    0.0496
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_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            32867
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.836
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       acicular
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         5765
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0320P)²+1.3867P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0740
_refine_ls_wR_factor_ref         0.0836
_reflns_number_gt                4110
_reflns_number_total             5765
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800501z_si_002.cif
_cod_data_source_block           new
_cod_original_cell_volume        2508.37(12)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4071982
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Ba1 Ba 0.5000 0.5000 0.0000 0.03760(9) Uani 1 2 d S
C1 C 0.5968(2) 0.63034(15) 0.15912(15) 0.0165(5) Uani 1 1 d .
C2 C 0.5757(2) 0.69321(15) 0.08765(15) 0.0166(5) Uani 1 1 d .
C3 C 0.4378(2) 0.70201(15) 0.01561(15) 0.0162(5) Uani 1 1 d .
C4 C 0.3735(2) 0.64396(16) 0.04094(15) 0.0170(5) Uani 1 1 d .
C5 C 0.4725(2) 0.60015(15) 0.13046(15) 0.0165(5) Uani 1 1 d .
C11 C 0.7278(2) 0.59885(17) 0.24435(16) 0.0189(5) Uani 1 1 d .
C12 C 0.7569(2) 0.50024(19) 0.26874(16) 0.0248(5) Uani 1 1 d .
H12 H 0.6898 0.4529 0.2319 0.030 Uiso 1 1 calc R
C13 C 0.8814(3) 0.4708(2) 0.3454(2) 0.0362(7) Uani 1 1 d .
H13 H 0.8994 0.4035 0.3608 0.043 Uiso 1 1 calc R
C14 C 0.9804(3) 0.5390(2) 0.39994(19) 0.0365(7) Uani 1 1 d .
H14 H 1.0664 0.5186 0.4523 0.044 Uiso 1 1 calc R
C15 C 0.9535(3) 0.6363(2) 0.37779(18) 0.0303(6) Uani 1 1 d .
H15 H 1.0207 0.6834 0.4154 0.036 Uiso 1 1 calc R
C16 C 0.8287(2) 0.66572(18) 0.30083(16) 0.0230(5) Uani 1 1 d .
H16 H 0.8115 0.7331 0.2862 0.028 Uiso 1 1 calc R
C21 C 0.6767(2) 0.73202(17) 0.08175(16) 0.0200(5) Uani 1 1 d .
C22 C 0.7765(3) 0.67236(19) 0.09933(17) 0.0258(6) Uani 1 1 d .
H22 H 0.7858 0.6082 0.1227 0.031 Uiso 1 1 calc R
C23 C 0.8623(3) 0.7045(2) 0.08347(19) 0.0371(7) Uani 1 1 d .
H23 H 0.9300 0.6628 0.0963 0.045 Uiso 1 1 calc R
C24 C 0.8489(3) 0.7972(3) 0.0490(2) 0.0448(8) Uani 1 1 d .
H24 H 0.9045 0.8185 0.0348 0.054 Uiso 1 1 calc R
C25 C 0.7549(3) 0.8586(2) 0.0351(2) 0.0421(8) Uani 1 1 d .
H25 H 0.7486 0.9235 0.0141 0.051 Uiso 1 1 calc R
C26 C 0.6695(3) 0.82720(19) 0.05138(18) 0.0293(6) Uani 1 1 d .
H26 H 0.6054 0.8707 0.0418 0.035 Uiso 1 1 calc R
C31 C 0.3696(2) 0.75952(16) -0.07333(16) 0.0183(5) Uani 1 1 d .
C32 C 0.3965(2) 0.74558(17) -0.13646(16) 0.0211(5) Uani 1 1 d .
H32 H 0.4630 0.7008 -0.1209 0.025 Uiso 1 1 calc R
C33 C 0.3277(3) 0.79614(19) -0.22146(17) 0.0281(6) Uani 1 1 d .
H33 H 0.3459 0.7853 -0.2645 0.034 Uiso 1 1 calc R
C34 C 0.2325(3) 0.8624(2) -0.24379(19) 0.0354(7) Uani 1 1 d .
H34 H 0.1857 0.8975 -0.3020 0.043 Uiso 1 1 calc R
C35 C 0.2050(3) 0.8779(2) -0.18195(19) 0.0329(6) Uani 1 1 d .
H35 H 0.1392 0.9233 -0.1976 0.039 Uiso 1 1 calc R
C36 C 0.2735(3) 0.82717(17) -0.09738(17) 0.0233(5) Uani 1 1 d .
H36 H 0.2548 0.8386 -0.0547 0.028 Uiso 1 1 calc R
C41 C 0.2303(2) 0.62671(16) -0.01947(16) 0.0175(5) Uani 1 1 d .
C42 C 0.1555(2) 0.61101(16) -0.11732(16) 0.0215(5) Uani 1 1 d .
H42 H 0.1979 0.6119 -0.1453 0.026 Uiso 1 1 calc R
C43 C 0.0215(3) 0.59420(18) -0.17471(18) 0.0273(6) Uani 1 1 d .
H43 H -0.0268 0.5847 -0.2412 0.033 Uiso 1 1 calc R
C44 C -0.0421(3) 0.59123(18) -0.13590(19) 0.0297(6) Uani 1 1 d .
H44 H -0.1339 0.5789 -0.1750 0.036 Uiso 1 1 calc R
C45 C 0.0293(3) 0.60635(18) -0.0394(2) 0.0294(6) Uani 1 1 d .
H45 H -0.0137 0.6046 -0.0119 0.035 Uiso 1 1 calc R
C46 C 0.1632(3) 0.62400(17) 0.01765(18) 0.0236(5) Uani 1 1 d .
H46 H 0.2104 0.6345 0.0839 0.028 Uiso 1 1 calc R
C51 C 0.4541(2) 0.52614(15) 0.18106(16) 0.0171(5) Uani 1 1 d .
C52 C 0.3768(3) 0.44370(17) 0.13412(17) 0.0230(5) Uani 1 1 d .
H52 H 0.3274 0.4387 0.0671 0.028 Uiso 1 1 calc R
C53 C 0.3703(3) 0.36895(19) 0.18292(19) 0.0297(6) Uani 1 1 d .
H53 H 0.3182 0.3129 0.1498 0.036 Uiso 1 1 calc R
C54 C 0.4399(3) 0.3766(2) 0.2797(2) 0.0369(7) Uani 1 1 d .
H54 H 0.4373 0.3252 0.3139 0.044 Uiso 1 1 calc R
C55 C 0.5134(3) 0.4585(2) 0.32702(19) 0.0350(7) Uani 1 1 d .
H55 H 0.5595 0.4642 0.3936 0.042 Uiso 1 1 calc R
C56 C 0.5209(3) 0.53292(18) 0.27860(17) 0.0247(6) Uani 1 1 d .
H56 H 0.5721 0.5891 0.3123 0.030 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'
Ba Ba -0.3244 2.2819 '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
C1 Ba1 C1 180.00(7) 3_665 .
C1 Ba1 C2 151.73(6) 3_665 .
C1 Ba1 C2 28.27(6) . .
C1 Ba1 C2 28.27(6) 3_665 3_665
C1 Ba1 C2 151.73(6) . 3_665
C2 Ba1 C2 180.0 . 3_665
C1 Ba1 C5 28.15(6) 3_665 3_665
C1 Ba1 C5 151.85(6) . 3_665
C2 Ba1 C5 133.57(6) . 3_665
C2 Ba1 C5 46.43(6) 3_665 3_665
C1 Ba1 C5 151.85(6) 3_665 .
C1 Ba1 C5 28.15(6) . .
C2 Ba1 C5 46.43(6) . .
C2 Ba1 C5 133.57(6) 3_665 .
C5 Ba1 C5 180.00(9) 3_665 .
C1 Ba1 C4 133.72(6) 3_665 .
C1 Ba1 C4 46.28(6) . .
C2 Ba1 C4 46.34(6) . .
C2 Ba1 C4 133.66(6) 3_665 .
C5 Ba1 C4 151.94(6) 3_665 .
C5 Ba1 C4 28.06(6) . .
C1 Ba1 C4 46.28(6) 3_665 3_665
C1 Ba1 C4 133.72(6) . 3_665
C2 Ba1 C4 133.66(6) . 3_665
C2 Ba1 C4 46.34(6) 3_665 3_665
C5 Ba1 C4 28.06(6) 3_665 3_665
C5 Ba1 C4 151.94(6) . 3_665
C4 Ba1 C4 180.00(9) . 3_665
C1 Ba1 C3 134.01(6) 3_665 .
C1 Ba1 C3 45.99(6) . .
C2 Ba1 C3 27.95(6) . .
C2 Ba1 C3 152.05(6) 3_665 .
C5 Ba1 C3 134.08(6) 3_665 .
C5 Ba1 C3 45.92(6) . .
C4 Ba1 C3 27.88(6) . .
C4 Ba1 C3 152.12(6) 3_665 .
C1 Ba1 C3 45.99(6) 3_665 3_665
C1 Ba1 C3 134.01(6) . 3_665
C2 Ba1 C3 152.05(6) . 3_665
C2 Ba1 C3 27.95(6) 3_665 3_665
C5 Ba1 C3 45.92(6) 3_665 3_665
C5 Ba1 C3 134.08(6) . 3_665
C4 Ba1 C3 152.12(6) . 3_665
C4 Ba1 C3 27.88(6) 3_665 3_665
C3 Ba1 C3 180.0 . 3_665
C5 C1 C2 108.3(2) . .
C5 C1 C11 127.4(2) . .
C2 C1 C11 124.1(2) . .
C5 C1 Ba1 76.50(12) . .
C2 C1 Ba1 76.41(12) . .
C11 C1 Ba1 110.56(14) . .
C3 C2 C1 107.3(2) . .
C3 C2 C21 125.3(2) . .
C1 C2 C21 127.0(2) . .
C3 C2 Ba1 77.06(12) . .
C1 C2 Ba1 75.33(12) . .
C21 C2 Ba1 107.70(14) . .
C2 C3 C4 108.82(19) . .
C2 C3 C31 126.6(2) . .
C4 C3 C31 124.6(2) . .
C2 C3 Ba1 74.99(12) . .
C4 C3 Ba1 75.77(12) . .
C31 C3 Ba1 114.45(14) . .
C3 C4 C5 107.5(2) . .
C3 C4 C41 125.4(2) . .
C5 C4 C41 126.9(2) . .
C3 C4 Ba1 76.34(13) . .
C5 C4 Ba1 75.25(13) . .
C41 C4 Ba1 110.74(14) . .
C1 C5 C4 108.09(19) . .
C1 C5 C51 124.2(2) . .
C4 C5 C51 127.3(2) . .
C1 C5 Ba1 75.35(12) . .
C4 C5 Ba1 76.69(12) . .
C51 C5 Ba1 108.49(13) . .
C16 C11 C12 117.5(2) . .
C16 C11 C1 121.2(2) . .
C12 C11 C1 121.3(2) . .
C13 C12 C11 121.1(2) . .
C13 C12 H12 119.5 . .
C11 C12 H12 119.5 . .
C12 C13 C14 120.2(3) . .
C12 C13 H13 119.9 . .
C14 C13 H13 119.9 . .
C15 C14 C13 119.6(3) . .
C15 C14 H14 120.2 . .
C13 C14 H14 120.2 . .
C14 C15 C16 120.1(3) . .
C14 C15 H15 120.0 . .
C16 C15 H15 120.0 . .
C15 C16 C11 121.5(2) . .
C15 C16 H16 119.2 . .
C11 C16 H16 119.2 . .
C22 C21 C26 117.7(2) . .
C22 C21 C2 121.0(2) . .
C26 C21 C2 121.2(2) . .
C23 C22 C21 121.5(3) . .
C23 C22 H22 119.3 . .
C21 C22 H22 119.3 . .
C24 C23 C22 119.6(3) . .
C24 C23 H23 120.2 . .
C22 C23 H23 120.2 . .
C25 C24 C23 119.8(3) . .
C25 C24 H24 120.1 . .
C23 C24 H24 120.1 . .
C24 C25 C26 120.8(3) . .
C24 C25 H25 119.6 . .
C26 C25 H25 119.6 . .
C25 C26 C21 120.5(3) . .
C25 C26 H26 119.7 . .
C21 C26 H26 119.7 . .
C32 C31 C36 118.2(2) . .
C32 C31 C3 121.3(2) . .
C36 C31 C3 120.6(2) . .
C33 C32 C31 120.8(2) . .
C33 C32 H32 119.6 . .
C31 C32 H32 119.6 . .
C34 C33 C32 119.9(2) . .
C34 C33 H33 120.0 . .
C32 C33 H33 120.0 . .
C35 C34 C33 120.2(2) . .
C35 C34 H34 119.9 . .
C33 C34 H34 119.9 . .
C36 C35 C34 119.8(3) . .
C36 C35 H35 120.1 . .
C34 C35 H35 120.1 . .
C35 C36 C31 121.1(2) . .
C35 C36 H36 119.4 . .
C31 C36 H36 119.4 . .
C46 C41 C42 116.5(2) . .
C46 C41 C4 122.2(2) . .
C42 C41 C4 121.3(2) . .
C43 C42 C41 121.9(2) . .
C43 C42 H42 119.0 . .
C41 C42 H42 119.0 . .
C44 C43 C42 120.3(2) . .
C44 C43 H43 119.9 . .
C42 C43 H43 119.9 . .
C43 C44 C45 119.1(2) . .
C43 C44 H44 120.4 . .
C45 C44 H44 120.4 . .
C44 C45 C46 120.4(2) . .
C44 C45 H45 119.8 . .
C46 C45 H45 119.8 . .
C45 C46 C41 121.8(2) . .
C45 C46 H46 119.1 . .
C41 C46 H46 119.1 . .
C56 C51 C52 117.7(2) . .
C56 C51 C5 121.0(2) . .
C52 C51 C5 121.2(2) . .
C53 C52 C51 121.6(2) . .
C53 C52 H52 119.2 . .
C51 C52 H52 119.2 . .
C54 C53 C52 119.4(2) . .
C54 C53 H53 120.3 . .
C52 C53 H53 120.3 . .
C53 C54 C55 120.0(2) . .
C53 C54 H54 120.0 . .
C55 C54 H54 120.0 . .
C54 C55 C56 120.6(2) . .
C54 C55 H55 119.7 . .
C56 C55 H55 119.7 . .
C55 C56 C51 120.6(2) . .
C55 C56 H56 119.7 . .
C51 C56 H56 119.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ba1 C1 2.910(2) 3_665
Ba1 C1 2.910(2) .
Ba1 C2 2.924(2) .
Ba1 C2 2.924(2) 3_665
Ba1 C5 2.925(2) 3_665
Ba1 C5 2.925(2) .
Ba1 C4 2.943(2) .
Ba1 C4 2.943(2) 3_665
Ba1 C3 2.951(2) .
Ba1 C3 2.951(2) 3_665
C1 C5 1.419(3) .
C1 C2 1.425(3) .
C1 C11 1.477(3) .
C2 C3 1.419(3) .
C2 C21 1.481(3) .
C3 C4 1.420(3) .
C3 C31 1.482(3) .
C4 C5 1.423(3) .
C4 C41 1.478(3) .
C5 C51 1.479(3) .
C11 C16 1.391(3) .
C11 C12 1.400(3) .
C12 C13 1.380(4) .
C12 H12 0.9500 .
C13 C14 1.386(4) .
C13 H13 0.9500 .
C14 C15 1.376(4) .
C14 H14 0.9500 .
C15 C16 1.382(4) .
C15 H15 0.9500 .
C16 H16 0.9500 .
C21 C22 1.394(4) .
C21 C26 1.396(3) .
C22 C23 1.385(4) .
C22 H22 0.9500 .
C23 C24 1.378(4) .
C23 H23 0.9500 .
C24 C25 1.375(5) .
C24 H24 0.9500 .
C25 C26 1.383(4) .
C25 H25 0.9500 .
C26 H26 0.9500 .
C31 C32 1.393(3) .
C31 C36 1.393(3) .
C32 C33 1.382(3) .
C32 H32 0.9500 .
C33 C34 1.380(4) .
C33 H33 0.9500 .
C34 C35 1.379(4) .
C34 H34 0.9500 .
C35 C36 1.378(3) .
C35 H35 0.9500 .
C36 H36 0.9500 .
C41 C46 1.391(3) .
C41 C42 1.396(3) .
C42 C43 1.384(3) .
C42 H42 0.9500 .
C43 C44 1.375(4) .
C43 H43 0.9500 .
C44 C45 1.380(4) .
C44 H44 0.9500 .
C45 C46 1.385(4) .
C45 H45 0.9500 .
C46 H46 0.9500 .
C51 C56 1.391(3) .
C51 C52 1.395(3) .
C52 C53 1.386(3) .
C52 H52 0.9500 .
C53 C54 1.374(4) .
C53 H53 0.9500 .
C54 C55 1.375(4) .
C54 H54 0.9500 .
C55 C56 1.383(4) .
C55 H55 0.9500 .
C56 H56 0.9500 .
