#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:41:20 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179257 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/77/4317703.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_4317703
loop_
_publ_author_name
'Gerd W. Rabe'
'Christian D. Bérubé'
'Glenn P. A. Yap'
'Kin-Chung Lam'
'Thomas E. Concolino'
'Arnold L. Rheingold'
_publ_section_title
;
 Synthesis and Structural Characterization of 2,6-Dimesitylphenyl
 Complexes of Scandium, Ytterbium, and Yttrium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1446
_journal_page_last               1453
_journal_paper_doi               10.1021/ic0109492
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C32 H41 Cl2 O2 Yb'
_chemical_formula_weight         701.59
_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                 101.749(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2447(7)
_cell_length_b                   15.5683(12)
_cell_length_c                   20.0979(14)
_cell_measurement_temperature    173(2)
_cell_volume                     3138.3(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0586
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26167
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    3.176
_exptl_absorpt_correction_T_max  0.5692
_exptl_absorpt_correction_T_min  0.4492
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1412
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.705
_refine_diff_density_min         -1.867
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         6152
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0432
_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)+(0.0440P)²+8.4638P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1076
_reflns_number_gt                4889
_reflns_number_total             6152
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0109492_2.cif
_cod_data_source_block           rab23
_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.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' 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_original_cell_volume        3138.3(5)
_cod_database_code               4317703
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
Yb1 Yb 0.51688(3) 0.341132(17) 0.166567(12) 0.03085(10) Uani 1 1 d . . .
Cl1 Cl 0.42849(17) 0.48461(11) 0.12099(8) 0.0448(4) Uani 1 1 d . . .
Cl2 Cl 0.64723(17) 0.21131(11) 0.21877(8) 0.0451(4) Uani 1 1 d . . .
O1 O 0.6628(4) 0.3493(3) 0.0959(2) 0.0420(11) Uani 1 1 d . . .
O2 O 0.6117(5) 0.4124(3) 0.2640(2) 0.0441(11) Uani 1 1 d . A .
C1 C 0.3132(6) 0.2659(4) 0.1393(3) 0.0300(13) Uani 1 1 d . . .
C2 C 0.2383(6) 0.2502(4) 0.1887(3) 0.0311(13) Uani 1 1 d . . .
C3 C 0.1285(6) 0.1954(4) 0.1777(3) 0.0383(14) Uani 1 1 d . . .
H3A H 0.0805 0.1859 0.2128 0.046 Uiso 1 1 calc R . .
C4 C 0.0894(7) 0.1547(4) 0.1152(3) 0.0447(16) Uani 1 1 d . . .
H4A H 0.0162 0.1160 0.1077 0.054 Uiso 1 1 calc R . .
C5 C 0.1584(7) 0.1713(4) 0.0640(3) 0.0393(15) Uani 1 1 d . . .
H5A H 0.1302 0.1452 0.0207 0.047 Uiso 1 1 calc R . .
C6 C 0.2679(6) 0.2254(4) 0.0752(3) 0.0295(12) Uani 1 1 d . . .
C7 C 0.2724(6) 0.2968(4) 0.2561(3) 0.0295(12) Uani 1 1 d . . .
C8 C 0.3436(7) 0.2554(4) 0.3143(3) 0.0374(14) Uani 1 1 d . . .
C9 C 0.3673(7) 0.2989(5) 0.3763(3) 0.0441(16) Uani 1 1 d . . .
H9A H 0.4165 0.2708 0.4155 0.053 Uiso 1 1 calc R . .
C10 C 0.3223(6) 0.3807(4) 0.3828(3) 0.0395(15) Uani 1 1 d . . .
C11 C 0.2515(6) 0.4207(4) 0.3246(3) 0.0368(14) Uani 1 1 d . . .
H11A H 0.2203 0.4777 0.3279 0.044 Uiso 1 1 calc R . .
C12 C 0.2251(6) 0.3801(4) 0.2620(3) 0.0337(13) Uani 1 1 d . . .
C13 C 0.3862(8) 0.1624(4) 0.3121(3) 0.0520(19) Uani 1 1 d . . .
H13A H 0.3630 0.1412 0.2653 0.078 Uiso 1 1 calc R . .
H13B H 0.3404 0.1277 0.3410 0.078 Uiso 1 1 calc R . .
H13C H 0.4828 0.1580 0.3287 0.078 Uiso 1 1 calc R . .
C14 C 0.3442(8) 0.4262(5) 0.4511(3) 0.056(2) Uani 1 1 d . . .
H14A H 0.3960 0.3890 0.4862 0.084 Uiso 1 1 calc R . .
H14B H 0.2578 0.4390 0.4626 0.084 Uiso 1 1 calc R . .
H14C H 0.3930 0.4798 0.4486 0.084 Uiso 1 1 calc R . .
C15 C 0.1395(7) 0.4250(4) 0.2014(3) 0.0448(16) Uani 1 1 d . . .
H15A H 0.1156 0.4824 0.2149 0.067 Uiso 1 1 calc R . .
H15B H 0.0582 0.3915 0.1853 0.067 Uiso 1 1 calc R . .
H15C H 0.1894 0.4300 0.1648 0.067 Uiso 1 1 calc R . .
C16 C 0.3362(6) 0.2418(4) 0.0167(3) 0.0311(13) Uani 1 1 d . . .
C17 C 0.2896(6) 0.3094(4) -0.0291(3) 0.0329(13) Uani 1 1 d . . .
C18 C 0.3451(6) 0.3186(4) -0.0860(3) 0.0350(14) Uani 1 1 d . . .
H18A H 0.3138 0.3635 -0.1172 0.042 Uiso 1 1 calc R . .
C19 C 0.4449(6) 0.2647(4) -0.0992(3) 0.0360(14) Uani 1 1 d . . .
C20 C 0.4898(6) 0.1998(4) -0.0535(3) 0.0360(14) Uani 1 1 d . . .
H20A H 0.5595 0.1633 -0.0614 0.043 Uiso 1 1 calc R . .
C21 C 0.4354(6) 0.1861(4) 0.0043(3) 0.0340(13) Uani 1 1 d . . .
C22 C 0.1813(6) 0.3681(4) -0.0173(3) 0.0386(15) Uani 1 1 d . . .
H22A H 0.1624 0.4106 -0.0540 0.058 Uiso 1 1 calc R . .
H22B H 0.2097 0.3976 0.0263 0.058 Uiso 1 1 calc R . .
H22C H 0.1006 0.3346 -0.0166 0.058 Uiso 1 1 calc R . .
C23 C 0.5004(7) 0.2785(5) -0.1629(3) 0.0479(18) Uani 1 1 d . . .
H23A H 0.5695 0.2355 -0.1647 0.072 Uiso 1 1 calc R . .
H23B H 0.5390 0.3361 -0.1620 0.072 Uiso 1 1 calc R . .
H23C H 0.4285 0.2726 -0.2030 0.072 Uiso 1 1 calc R . .
C24 C 0.4828(7) 0.1107(4) 0.0503(3) 0.0420(16) Uani 1 1 d . . .
H24A H 0.4357 0.1101 0.0881 0.063 Uiso 1 1 calc R . .
H24B H 0.5789 0.1159 0.0681 0.063 Uiso 1 1 calc R . .
H24C H 0.4646 0.0572 0.0244 0.063 Uiso 1 1 calc R . .
C25 C 0.7907(9) 0.3049(9) 0.1049(6) 0.110(5) Uani 1 1 d . . .
H25A H 0.7776 0.2427 0.0955 0.132 Uiso 1 1 calc R . .
H25B H 0.8425 0.3125 0.1518 0.132 Uiso 1 1 calc R . .
C26 C 0.8599(10) 0.3462(10) 0.0548(6) 0.122(6) Uani 1 1 d . . .
H26A H 0.9123 0.3964 0.0753 0.147 Uiso 1 1 calc R . .
H26B H 0.9207 0.3049 0.0391 0.147 Uiso 1 1 calc R . .
C27 C 0.7590(9) 0.3717(7) 0.0007(4) 0.079(3) Uani 1 1 d . . .
H27A H 0.7313 0.3233 -0.0310 0.094 Uiso 1 1 calc R . .
H27B H 0.7895 0.4196 -0.0247 0.094 Uiso 1 1 calc R . .
C28 C 0.6467(7) 0.3997(5) 0.0327(3) 0.0501(18) Uani 1 1 d . . .
H28A H 0.6523 0.4620 0.0427 0.060 Uiso 1 1 calc R . .
H28B H 0.5597 0.3873 0.0024 0.060 Uiso 1 1 calc R . .
C29 C 0.6044(12) 0.5037(6) 0.2773(5) 0.100(4) Uani 1 1 d . A .
H29A H 0.5136 0.5199 0.2826 0.120 Uiso 1 1 calc R . .
H29B H 0.6276 0.5377 0.2397 0.120 Uiso 1 1 calc R . .
C30 C 0.7051(11) 0.5188(6) 0.3431(5) 0.086(3) Uani 1 1 d . . .
C31 C 0.6953(16) 0.4471(8) 0.3786(6) 0.087(5) Uani 0.75 1 d P A 1
H31A H 0.6170 0.4502 0.4005 0.104 Uiso 0.75 1 calc PR A 1
H31B H 0.7764 0.4389 0.4144 0.104 Uiso 0.75 1 calc PR A 1
C31' C 0.807(3) 0.4701(19) 0.3371(15) 0.048(7) Uiso 0.25 1 d P A 2
H31C H 0.8783 0.4674 0.3784 0.058 Uiso 0.25 1 calc PR A 2
H31D H 0.8432 0.4816 0.2960 0.058 Uiso 0.25 1 calc PR A 2
C32 C 0.6795(14) 0.3742(7) 0.3276(5) 0.115(5) Uani 1 1 d . . .
H32A H 0.7675 0.3511 0.3235 0.138 Uiso 1 1 calc R A 1
H32B H 0.6256 0.3271 0.3413 0.138 Uiso 1 1 calc R 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'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.0060 '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
O1 Yb1 O2 106.87(17) . . ?
O1 Yb1 C1 123.21(17) . . ?
O2 Yb1 C1 129.87(18) . . ?
O1 Yb1 Cl1 87.50(12) . . ?
O2 Yb1 Cl1 86.55(11) . . ?
C1 Yb1 Cl1 96.93(14) . . ?
O1 Yb1 Cl2 86.84(12) . . ?
O2 Yb1 Cl2 86.33(11) . . ?
C1 Yb1 Cl2 93.84(14) . . ?
Cl1 Yb1 Cl2 169.22(6) . . ?
C25 O1 C28 107.5(5) . . ?
C25 O1 Yb1 125.8(4) . . ?
C28 O1 Yb1 126.7(4) . . ?
C32 O2 C29 105.8(6) . . ?
C32 O2 Yb1 126.8(5) . . ?
C29 O2 Yb1 127.1(4) . . ?
C2 C1 C6 116.2(5) . . ?
C2 C1 Yb1 120.7(4) . . ?
C6 C1 Yb1 122.7(4) . . ?
C3 C2 C1 122.5(5) . . ?
C3 C2 C7 117.9(5) . . ?
C1 C2 C7 119.5(5) . . ?
C4 C3 C2 119.8(6) . . ?
C5 C4 C3 119.3(6) . . ?
C6 C5 C4 120.7(5) . . ?
C5 C6 C1 121.4(5) . . ?
C5 C6 C16 117.7(5) . . ?
C1 C6 C16 120.9(5) . . ?
C12 C7 C8 119.1(5) . . ?
C12 C7 C2 120.0(5) . . ?
C8 C7 C2 120.8(5) . . ?
C9 C8 C7 119.2(6) . . ?
C9 C8 C13 119.4(6) . . ?
C7 C8 C13 121.3(5) . . ?
C10 C9 C8 122.4(6) . . ?
C9 C10 C11 117.6(6) . . ?
C9 C10 C14 121.9(6) . . ?
C11 C10 C14 120.5(6) . . ?
C12 C11 C10 122.1(6) . . ?
C11 C12 C7 119.6(5) . . ?
C11 C12 C15 119.5(6) . . ?
C7 C12 C15 120.8(5) . . ?
C21 C16 C17 120.5(5) . . ?
C21 C16 C6 120.3(5) . . ?
C17 C16 C6 118.9(5) . . ?
C18 C17 C16 118.2(6) . . ?
C18 C17 C22 120.7(6) . . ?
C16 C17 C22 121.0(5) . . ?
C17 C18 C19 122.4(6) . . ?
C20 C19 C18 118.4(5) . . ?
C20 C19 C23 122.2(6) . . ?
C18 C19 C23 119.4(6) . . ?
C19 C20 C21 121.8(6) . . ?
C16 C21 C20 118.7(6) . . ?
C16 C21 C24 121.9(5) . . ?
C20 C21 C24 119.4(6) . . ?
O1 C25 C26 104.5(7) . . ?
C27 C26 C25 105.7(9) . . ?
C26 C27 C28 105.1(7) . . ?
O1 C28 C27 104.8(6) . . ?
O2 C29 C30 105.1(7) . . ?
C31' C30 C31 73.4(15) . . ?
C31' C30 C29 104.0(15) . . ?
C31 C30 C29 102.9(9) . . ?
C30 C31 C32 105.8(10) . . ?
C30 C31' C32 85.7(16) . . ?
O2 C32 C31 104.8(8) . . ?
O2 C32 C31' 87.9(11) . . ?
C31 C32 C31' 52.3(11) . . ?
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
Yb1 O1 2.266(4) . ?
Yb1 O2 2.288(4) . ?
Yb1 C1 2.358(6) . ?
Yb1 Cl1 2.5121(16) . ?
Yb1 Cl2 2.5295(16) . ?
O1 C25 1.459(10) . ?
O1 C28 1.473(8) . ?
O2 C32 1.452(9) . ?
O2 C29 1.452(9) . ?
C1 C2 1.395(8) . ?
C1 C6 1.424(7) . ?
C2 C3 1.394(9) . ?
C2 C7 1.512(8) . ?
C3 C4 1.391(9) . ?
C4 C5 1.387(9) . ?
C5 C6 1.385(8) . ?
C6 C16 1.507(8) . ?
C7 C12 1.397(9) . ?
C7 C8 1.402(8) . ?
C8 C9 1.397(9) . ?
C8 C13 1.516(9) . ?
C9 C10 1.369(9) . ?
C10 C11 1.392(9) . ?
C10 C14 1.520(8) . ?
C11 C12 1.385(8) . ?
C12 C15 1.519(8) . ?
C16 C21 1.396(8) . ?
C16 C17 1.416(9) . ?
C17 C18 1.386(8) . ?
C17 C22 1.492(9) . ?
C18 C19 1.389(9) . ?
C19 C20 1.380(9) . ?
C19 C23 1.518(8) . ?
C20 C21 1.403(8) . ?
C21 C24 1.512(9) . ?
C25 C26 1.491(12) . ?
C26 C27 1.396(13) . ?
C27 C28 1.493(10) . ?
C29 C30 1.520(11) . ?
C30 C31' 1.31(3) . ?
C30 C31 1.341(16) . ?
C31 C32 1.516(13) . ?
C31' C32 1.97(3) . ?
