#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:44:31 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179202 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/37/4313711.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_4313711
loop_
_publ_author_name
'Gerd W. Rabe'
'Mei Zhang-Presse'
'Florian A. Riederer'
'Glenn P. A. Yap'
_publ_section_title
;
 Donor-Functionalized Lanthanide Terphenyl Complexes: Synthesis and
 Structural Characterization of 2,6-Di(o-anisol)phenyl Compounds of
 Ytterbium, Yttrium, and Samarium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3527
_journal_page_last               3533
_journal_paper_doi               10.1021/ic0300161
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C44 H51 O4 Yb'
_chemical_formula_weight         816.89
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 128.0890(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.6759(16)
_cell_length_b                   12.3333(9)
_cell_length_c                   17.6237(12)
_cell_measurement_reflns_used    'reflections from 60 data frames'
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      1.47
_cell_volume                     3879.2(5)
_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      203(2)
_diffrn_measured_fraction_theta_full 0.919
_diffrn_measured_fraction_theta_max 0.919
_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  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0214
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16228
_diffrn_reflns_theta_full        28.63
_diffrn_reflns_theta_max         28.63
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        <1
_diffrn_standards_number         '50 standard frames at start and end'
_exptl_absorpt_coefficient_mu    2.451
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.791271
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing,R., Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.574
_refine_diff_density_min         -1.050
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         4586
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0193
_refine_ls_R_factor_gt           0.0184
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0253P)²+3.7067P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0474
_refine_ls_wR_factor_ref         0.0479
_reflns_number_gt                4446
_reflns_number_total             4586
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0300161_4.cif
_cod_data_source_block           gr2003
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4313711
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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 0.913665(8) 0.7500 0.01845(4) Uani 1 2 d S . .
O1 O 0.42160(7) 0.95611(11) 0.78828(9) 0.0247(3) Uani 1 1 d . . .
O2 O 0.42708(7) 0.84369(12) 0.61559(9) 0.0278(3) Uani 1 1 d . . .
C1 C 0.5000 1.3372(2) 0.7500 0.0413(7) Uani 1 2 d S . .
H1A H 0.5000 1.4134 0.7500 0.050 Uiso 1 2 calc SR . .
C2 C 0.43643(13) 1.28126(17) 0.72157(17) 0.0355(5) Uani 1 1 d . . .
H2A H 0.3937 1.3197 0.7035 0.043 Uiso 1 1 calc R . .
C3 C 0.43525(11) 1.16734(15) 0.71945(14) 0.0257(4) Uani 1 1 d . . .
C4 C 0.5000 1.1066(2) 0.7500 0.0230(5) Uani 1 2 d S . .
C5 C 0.36253(11) 1.11279(17) 0.68104(14) 0.0257(4) Uani 1 1 d . . .
C6 C 0.29361(12) 1.16163(19) 0.60756(16) 0.0348(5) Uani 1 1 d . . .
H6A H 0.2942 1.2287 0.5826 0.042 Uiso 1 1 calc R . .
C7 C 0.22485(13) 1.1150(2) 0.57035(18) 0.0420(5) Uani 1 1 d . . .
H7A H 0.1802 1.1509 0.5218 0.050 Uiso 1 1 calc R . .
C8 C 0.22181(12) 1.0152(2) 0.60470(17) 0.0417(5) Uani 1 1 d . . .
H8A H 0.1754 0.9829 0.5792 0.050 Uiso 1 1 calc R . .
C9 C 0.28850(12) 0.96384(19) 0.67739(16) 0.0338(4) Uani 1 1 d . . .
H9A H 0.2876 0.8965 0.7017 0.041 Uiso 1 1 calc R . .
C10 C 0.35640(10) 1.01292(16) 0.71377(13) 0.0247(4) Uani 1 1 d . . .
C11 C 0.45115(14) 0.9950(2) 0.88399(15) 0.0390(5) Uani 1 1 d . . .
H11A H 0.4100 1.0083 0.8861 0.059 Uiso 1 1 calc R . .
H11B H 0.4787 1.0617 0.8977 0.059 Uiso 1 1 calc R . .
H11C H 0.4843 0.9407 0.9317 0.059 Uiso 1 1 calc R . .
C12 C 0.44301(10) 0.73428(15) 0.51704(14) 0.0263(4) Uani 1 1 d . . .
C13 C 0.41464(12) 0.69968(17) 0.42427(15) 0.0322(4) Uani 1 1 d . . .
H13A H 0.4428 0.6510 0.4170 0.039 Uiso 1 1 calc R . .
C14 C 0.34581(13) 0.73600(18) 0.34304(15) 0.0345(4) Uani 1 1 d . . .
H14A H 0.3274 0.7117 0.2814 0.041 Uiso 1 1 calc R . .
C15 C 0.30472(12) 0.80811(18) 0.35349(14) 0.0321(4) Uani 1 1 d . A .
H15A H 0.2585 0.8330 0.2982 0.038 Uiso 1 1 calc R . .
C16 C 0.33008(11) 0.84528(17) 0.44441(14) 0.0279(4) Uani 1 1 d . . .
C17 C 0.40005(10) 0.80784(15) 0.52701(13) 0.0233(3) Uani 1 1 d . A .
C18 C 0.51707(11) 0.69078(17) 0.60575(15) 0.0325(4) Uani 1 1 d . . .
H18A H 0.5372 0.7449 0.6578 0.039 Uiso 1 1 calc R . .
C19 C 0.57613(16) 0.6736(4) 0.5911(2) 0.0709(10) Uani 1 1 d . . .
H19A H 0.5833 0.7405 0.5688 0.106 Uiso 1 1 calc R . .
H19B H 0.5596 0.6171 0.5435 0.106 Uiso 1 1 calc R . .
H19C H 0.6231 0.6522 0.6517 0.106 Uiso 1 1 calc R . .
C20 C 0.50346(19) 0.5864(2) 0.6390(3) 0.0710(11) Uani 1 1 d . . .
H20A H 0.4658 0.5990 0.6478 0.106 Uiso 1 1 calc R . .
H20B H 0.5498 0.5632 0.6996 0.106 Uiso 1 1 calc R . .
H20C H 0.4861 0.5304 0.5908 0.106 Uiso 1 1 calc R . .
C21' C 0.28375(14) 0.9260(2) 0.45294(18) 0.0440(6) Uani 0.47 1 d PD A 2
H21' H 0.3004 0.9221 0.5197 0.053 Uiso 0.47 1 calc PR A 2
C22' C 0.3061(6) 1.0430(8) 0.4388(8) 0.078(4) Uani 0.47 1 d PD A 2
H22A H 0.3602 1.0502 0.4815 0.117 Uiso 0.47 1 calc PR A 2
H22B H 0.2845 1.0986 0.4539 0.117 Uiso 0.47 1 calc PR A 2
H22C H 0.2872 1.0511 0.3725 0.117 Uiso 0.47 1 calc PR A 2
C23' C 0.1996(5) 0.9185(11) 0.3855(9) 0.100(6) Uani 0.47 1 d PD A 2
H23A H 0.1787 0.9754 0.4005 0.151 Uiso 0.47 1 calc PR A 2
H23B H 0.1843 0.8484 0.3929 0.151 Uiso 0.47 1 calc PR A 2
H23C H 0.1815 0.9268 0.3195 0.151 Uiso 0.47 1 calc PR A 2
C21 C 0.28375(14) 0.9260(2) 0.45294(18) 0.0440(6) Uani 0.53 1 d PD A 1
H21 H 0.3101 0.9424 0.5219 0.053 Uiso 0.53 1 calc PR A 1
C22 C 0.2694(6) 1.0303(8) 0.3998(7) 0.081(3) Uani 0.53 1 d PD A 1
H22D H 0.2400 1.0785 0.4082 0.121 Uiso 0.53 1 calc PR A 1
H22E H 0.2422 1.0152 0.3318 0.121 Uiso 0.53 1 calc PR A 1
H22F H 0.3168 1.0646 0.4252 0.121 Uiso 0.53 1 calc PR A 1
C23 C 0.2068(4) 0.8678(8) 0.4106(7) 0.069(3) Uani 0.53 1 d PD A 1
H23D H 0.2165 0.8011 0.4458 0.103 Uiso 0.53 1 calc PR A 1
H23E H 0.1807 0.8514 0.3430 0.103 Uiso 0.53 1 calc PR A 1
H23F H 0.1761 0.9153 0.4172 0.103 Uiso 0.53 1 calc PR A 1
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'
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
_geom_angle_publ_flag
O2 Yb O2 130.55(8) . 2_656 ?
O2 Yb O1 102.32(5) . . ?
O2 Yb O1 88.60(5) 2_656 . ?
O2 Yb O1 88.60(5) . 2_656 ?
O2 Yb O1 102.32(5) 2_656 2_656 ?
O1 Yb O1 153.89(7) . 2_656 ?
O2 Yb C4 114.72(4) . . ?
O2 Yb C4 114.72(4) 2_656 . ?
O1 Yb C4 76.94(3) . . ?
O1 Yb C4 76.94(3) 2_656 . ?
O2 Yb C10 86.21(5) . . ?
O2 Yb C10 113.01(5) 2_656 . ?
O1 Yb C10 24.41(5) . . ?
O1 Yb C10 137.33(5) 2_656 . ?
C4 Yb C10 67.16(4) . . ?
O2 Yb C10 113.01(5) . 2_656 ?
O2 Yb C10 86.21(5) 2_656 2_656 ?
O1 Yb C10 137.33(5) . 2_656 ?
O1 Yb C10 24.41(5) 2_656 2_656 ?
C4 Yb C10 67.16(4) . 2_656 ?
C10 Yb C10 134.32(7) . 2_656 ?
C10 O1 C11 112.43(14) . . ?
C10 O1 Yb 113.04(10) . . ?
C11 O1 Yb 121.54(12) . . ?
C17 O2 Yb 159.04(12) . . ?
C2 C1 C2 120.2(3) . 2_656 ?
C1 C2 C3 120.4(2) . . ?
C2 C3 C4 121.15(19) . . ?
C2 C3 C5 117.24(18) . . ?
C4 C3 C5 121.58(18) . . ?
C3 C4 C3 116.6(2) . 2_656 ?
C3 C4 Yb 121.72(12) . . ?
C3 C4 Yb 121.72(12) 2_656 . ?
C10 C5 C6 114.72(19) . . ?
C10 C5 C3 124.62(17) . . ?
C6 C5 C3 120.66(19) . . ?
C7 C6 C5 122.8(2) . . ?
C6 C7 C8 120.2(2) . . ?
C7 C8 C9 119.0(2) . . ?
C10 C9 C8 119.5(2) . . ?
C9 C10 C5 123.75(18) . . ?
C9 C10 O1 115.99(17) . . ?
C5 C10 O1 120.26(17) . . ?
C9 C10 Yb 129.51(14) . . ?
C5 C10 Yb 94.14(12) . . ?
O1 C10 Yb 42.55(7) . . ?
C13 C12 C17 118.82(18) . . ?
C13 C12 C18 120.79(18) . . ?
C17 C12 C18 120.35(17) . . ?
C14 C13 C12 121.23(19) . . ?
C15 C14 C13 119.49(18) . . ?
C14 C15 C16 121.85(19) . . ?
C15 C16 C17 118.53(18) . . ?
C15 C16 C21' 120.33(19) . . ?
C17 C16 C21' 121.12(18) . . ?
O2 C17 C16 120.22(17) . . ?
O2 C17 C12 119.68(16) . . ?
C16 C17 C12 120.08(16) . . ?
C12 C18 C20 109.7(2) . . ?
C12 C18 C19 113.8(2) . . ?
C20 C18 C19 110.8(3) . . ?
C23' C21' C16 119.9(6) . . ?
C23' C21' C22' 107.6(6) . . ?
C16 C21' C22' 105.7(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Yb O2 2.0634(13) . ?
Yb O2 2.0634(13) 2_656 ?
Yb O1 2.3172(13) . ?
Yb O1 2.3172(13) 2_656 ?
Yb C4 2.379(3) . ?
Yb C10 3.1535(18) . ?
Yb C10 3.1535(18) 2_656 ?
O1 C10 1.416(2) . ?
O1 C11 1.459(2) . ?
O2 C17 1.352(2) . ?
C1 C2 1.383(3) . ?
C1 C2 1.383(3) 2_656 ?
C2 C3 1.405(3) . ?
C3 C4 1.425(2) . ?
C3 C5 1.501(3) . ?
C4 C3 1.425(2) 2_656 ?
C5 C10 1.403(3) . ?
C5 C6 1.409(3) . ?
C6 C7 1.390(3) . ?
C7 C8 1.392(4) . ?
C8 C9 1.392(3) . ?
C9 C10 1.389(3) . ?
C12 C13 1.404(3) . ?
C12 C17 1.419(3) . ?
C12 C18 1.521(3) . ?
C13 C14 1.389(3) . ?
C14 C15 1.380(3) . ?
C15 C16 1.404(3) . ?
C16 C17 1.414(3) . ?
C16 C21' 1.521(3) . ?
C18 C20 1.523(4) . ?
C18 C19 1.527(3) . ?
C21' C23' 1.505(9) . ?
C21' C22' 1.598(9) . ?
