#------------------------------------------------------------------------------
#$Date: 2019-11-17 05:51:32 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228229 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/19/7121959.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_7121959
loop_
_publ_author_name
'Wolf, Benjamin M.'
'Stuhl, Christoph'
'Anwander, Reiner'
_publ_section_title
;
 Synthesis of homometallic divalent lanthanide organoimides from benzyl
 complexes.
;
_journal_issue                   64
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8826
_journal_page_last               8829
_journal_paper_doi               10.1039/c8cc05234d
_journal_volume                  54
_journal_year                    2018
_chemical_formula_sum            'C34 H54 O4 Yb'
_chemical_formula_weight         699.81
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-06-28 deposited with the CCDC.
2018-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.14(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.536(8)
_cell_length_b                   16.441(16)
_cell_length_c                   20.897(16)
_cell_measurement_reflns_used    180
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.41
_cell_measurement_theta_min      2.612
_cell_volume                     3257(5)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection       'Bruker Apex3'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'XT, VERSION 2014/5'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Smart Apex III Duo'
_diffrn_measurement_method       omega/phi-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            35996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         1.960
_diffrn_source                   Imus-tube
_exptl_absorpt_coefficient_mu    2.905
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6071
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       rod
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.205
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.068
_refine_diff_density_max         1.497
_refine_diff_density_min         -1.522
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         4038
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0210
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0280P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0495
_refine_ls_wR_factor_ref         0.0502
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3775
_reflns_number_total             4038
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8cc05234d2.cif
_cod_data_source_block           1-Yb_thp_mo_YbBn2_THP_0m
_cod_depositor_comments
'Adding full bibliography for 7121956--7121961.cif.'
_cod_database_code               7121959
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.587
_shelx_estimated_absorpt_t_max   0.827
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C1 C 0.2997(2) 0.40872(15) 0.24147(10) 0.0264(5) Uani 1 1 d . . .
H1A H 0.2133 0.4334 0.2191 0.032 Uiso 1 1 calc R U .
H1B H 0.3279 0.3636 0.2142 0.032 Uiso 1 1 calc R U .
C2 C 0.2655(2) 0.37511(13) 0.30147(10) 0.0219(4) Uani 1 1 d . . .
C3 C 0.1463(2) 0.40099(14) 0.33156(11) 0.0259(5) Uani 1 1 d . . .
H3 H 0.0811 0.4376 0.3093 0.031 Uiso 1 1 calc R U .
C4 C 0.1221(3) 0.37455(15) 0.39232(11) 0.0304(5) Uani 1 1 d . . .
H4 H 0.0417 0.3939 0.4109 0.037 Uiso 1 1 calc R U .
C5 C 0.2133(3) 0.31998(15) 0.42699(11) 0.0319(5) Uani 1 1 d . . .
H5 H 0.1975 0.3032 0.4691 0.038 Uiso 1 1 calc R U .
C6 C 0.3272(2) 0.29126(14) 0.39814(11) 0.0292(5) Uani 1 1 d . . .
H6 H 0.3894 0.2532 0.4204 0.035 Uiso 1 1 calc R U .
C7 C 0.3524(2) 0.31693(14) 0.33729(11) 0.0254(5) Uani 1 1 d . . .
H7 H 0.4308 0.2949 0.3187 0.030 Uiso 1 1 calc R U .
C8 C 0.1984(2) 0.62766(16) 0.27965(11) 0.0303(5) Uani 1 1 d . . .
H8A H 0.1656 0.5784 0.2552 0.036 Uiso 1 1 calc R U .
H8B H 0.1555 0.6756 0.2565 0.036 Uiso 1 1 calc R U .
C9 C 0.1506(2) 0.62395(16) 0.34643(12) 0.0336(5) Uani 1 1 d . . .
H9A H 0.1868 0.5735 0.3682 0.040 Uiso 1 1 calc R U .
H9B H 0.0463 0.6225 0.3430 0.040 Uiso 1 1 calc R U .
C10 C 0.2041(2) 0.69739(16) 0.38618(12) 0.0324(5) Uani 1 1 d . . .
H10A H 0.1810 0.6910 0.4310 0.039 Uiso 1 1 calc R U .
H10B H 0.1571 0.7473 0.3681 0.039 Uiso 1 1 calc R U .
C11 C 0.3637(2) 0.70538(16) 0.38574(11) 0.0311(5) Uani 1 1 d . . .
H11A H 0.3965 0.7565 0.4075 0.037 Uiso 1 1 calc R U .
H11B H 0.4115 0.6594 0.4097 0.037 Uiso 1 1 calc R U .
C12 C 0.4020(2) 0.70565(14) 0.31709(12) 0.0284(5) Uani 1 1 d . . .
H12A H 0.3605 0.7543 0.2944 0.034 Uiso 1 1 calc R U .
H12B H 0.5057 0.7089 0.3176 0.034 Uiso 1 1 calc R U .
C13 C 0.4640(3) 0.48556(14) 0.08919(11) 0.0266(5) Uani 1 1 d . . .
H13A H 0.5440 0.4536 0.1102 0.032 Uiso 1 1 calc R U .
H13B H 0.4992 0.5185 0.0546 0.032 Uiso 1 1 calc R U .
C14 C 0.3495(3) 0.42823(15) 0.06021(11) 0.0315(5) Uani 1 1 d . . .
H14A H 0.3185 0.3928 0.0943 0.038 Uiso 1 1 calc R U .
H14B H 0.3876 0.3931 0.0277 0.038 Uiso 1 1 calc R U .
C15 C 0.2242(3) 0.47634(15) 0.02873(12) 0.0315(5) Uani 1 1 d . . .
H15A H 0.1463 0.4387 0.0140 0.038 Uiso 1 1 calc R U .
H15B H 0.2518 0.5059 -0.0092 0.038 Uiso 1 1 calc R U .
C16 C 0.1744(2) 0.53707(16) 0.07723(12) 0.0315(5) Uani 1 1 d . . .
H16A H 0.1008 0.5728 0.0552 0.038 Uiso 1 1 calc R U .
H16B H 0.1324 0.5072 0.1116 0.038 Uiso 1 1 calc R U .
C17 C 0.2966(2) 0.58846(14) 0.10678(10) 0.0251(4) Uani 1 1 d . . .
H17A H 0.3315 0.6229 0.0730 0.030 Uiso 1 1 calc R U .
H17B H 0.2633 0.6249 0.1397 0.030 Uiso 1 1 calc R U .
O1 O 0.35087(15) 0.63305(10) 0.28277(8) 0.0262(3) Uani 1 1 d . . .
O2 O 0.41017(16) 0.53881(10) 0.13595(7) 0.0222(3) Uani 1 1 d . . .
Yb1 Yb 0.5000 0.51829(2) 0.2500 0.01739(5) Uani 1 2 d S T P
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
C2 C1 Yb1 115.89(14) . .
C2 C1 H1A 108.3 . .
Yb1 C1 H1A 108.3 . .
C2 C1 H1B 108.3 . .
Yb1 C1 H1B 108.3 . .
H1A C1 H1B 107.4 . .
C3 C2 C7 114.6(2) . .
C3 C2 C1 122.5(2) . .
C7 C2 C1 122.8(2) . .
C4 C3 C2 122.1(2) . .
C4 C3 H3 119.0 . .
C2 C3 H3 119.0 . .
C3 C4 C5 121.4(2) . .
C3 C4 H4 119.3 . .
C5 C4 H4 119.3 . .
C6 C5 C4 117.9(2) . .
C6 C5 H5 121.0 . .
C4 C5 H5 121.0 . .
C5 C6 C7 121.3(2) . .
C5 C6 H6 119.4 . .
C7 C6 H6 119.4 . .
C6 C7 C2 122.6(2) . .
C6 C7 H7 118.7 . .
C2 C7 H7 118.7 . .
O1 C8 C9 111.06(18) . .
O1 C8 H8A 109.4 . .
C9 C8 H8A 109.4 . .
O1 C8 H8B 109.4 . .
C9 C8 H8B 109.4 . .
H8A C8 H8B 108.0 . .
C8 C9 C10 110.8(2) . .
C8 C9 H9A 109.5 . .
C10 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
C10 C9 H9B 109.5 . .
H9A C9 H9B 108.1 . .
C9 C10 C11 109.9(2) . .
C9 C10 H10A 109.7 . .
C11 C10 H10A 109.7 . .
C9 C10 H10B 109.7 . .
C11 C10 H10B 109.7 . .
H10A C10 H10B 108.2 . .
C12 C11 C10 110.24(19) . .
C12 C11 H11A 109.6 . .
C10 C11 H11A 109.6 . .
C12 C11 H11B 109.6 . .
C10 C11 H11B 109.6 . .
H11A C11 H11B 108.1 . .
O1 C12 C11 111.30(19) . .
O1 C12 H12A 109.4 . .
C11 C12 H12A 109.4 . .
O1 C12 H12B 109.4 . .
C11 C12 H12B 109.4 . .
H12A C12 H12B 108.0 . .
O2 C13 C14 110.7(2) . .
O2 C13 H13A 109.5 . .
C14 C13 H13A 109.5 . .
O2 C13 H13B 109.5 . .
C14 C13 H13B 109.5 . .
H13A C13 H13B 108.1 . .
C13 C14 C15 110.3(2) . .
C13 C14 H14A 109.6 . .
C15 C14 H14A 109.6 . .
C13 C14 H14B 109.6 . .
C15 C14 H14B 109.6 . .
H14A C14 H14B 108.1 . .
C14 C15 C16 109.7(2) . .
C14 C15 H15A 109.7 . .
C16 C15 H15A 109.7 . .
C14 C15 H15B 109.7 . .
C16 C15 H15B 109.7 . .
H15A C15 H15B 108.2 . .
C17 C16 C15 110.7(2) . .
C17 C16 H16A 109.5 . .
C15 C16 H16A 109.5 . .
C17 C16 H16B 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 108.1 . .
O2 C17 C16 111.6(2) . .
O2 C17 H17A 109.3 . .
C16 C17 H17A 109.3 . .
O2 C17 H17B 109.3 . .
C16 C17 H17B 109.3 . .
H17A C17 H17B 108.0 . .
C12 O1 C8 110.77(17) . .
C12 O1 Yb1 125.84(13) . .
C8 O1 Yb1 122.53(14) . .
C17 O2 C13 111.26(16) . .
C17 O2 Yb1 130.89(13) . .
C13 O2 Yb1 117.26(13) . .
O2 Yb1 O2 164.28(8) . 2_655
O2 Yb1 O1 90.72(6) . .
O2 Yb1 O1 77.37(6) 2_655 .
O2 Yb1 O1 77.36(6) . 2_655
O2 Yb1 O1 90.72(6) 2_655 2_655
O1 Yb1 O1 82.10(10) . 2_655
O2 Yb1 C1 109.58(6) . 2_655
O2 Yb1 C1 81.55(6) 2_655 2_655
O1 Yb1 C1 158.80(6) . 2_655
O1 Yb1 C1 96.07(9) 2_655 2_655
O2 Yb1 C1 81.55(6) . .
O2 Yb1 C1 109.59(6) 2_655 .
O1 Yb1 C1 96.07(9) . .
O1 Yb1 C1 158.79(6) 2_655 .
C1 Yb1 C1 93.02(13) 2_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.439(3) .
C1 Yb1 2.617(3) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 C3 1.422(3) .
C2 C7 1.424(3) .
C3 C4 1.385(3) .
C3 H3 0.9500 .
C4 C5 1.397(3) .
C4 H4 0.9500 .
C5 C6 1.380(4) .
C5 H5 0.9500 .
C6 C7 1.385(3) .
C6 H6 0.9500 .
C7 H7 0.9500 .
C8 O1 1.452(3) .
C8 C9 1.515(4) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 C10 1.522(4) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 C11 1.529(3) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 C12 1.517(3) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 O1 1.450(3) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 O2 1.446(3) .
C13 C14 1.518(3) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 C15 1.523(3) .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 C16 1.534(4) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C16 C17 1.516(3) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 O2 1.439(3) .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
O1 Yb1 2.502(2) .
O2 Yb1 2.468(2) .
Yb1 O2 2.468(2) 2_655
Yb1 O1 2.502(2) 2_655
Yb1 C1 2.617(3) 2_655
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
Yb1 C1 C2 C3 100.8(2)
Yb1 C1 C2 C7 -75.5(2)
C7 C2 C3 C4 3.3(3)
C1 C2 C3 C4 -173.2(2)
C2 C3 C4 C5 -0.8(4)
C3 C4 C5 C6 -1.6(4)
C4 C5 C6 C7 1.4(4)
C5 C6 C7 C2 1.3(3)
C3 C2 C7 C6 -3.5(3)
C1 C2 C7 C6 173.0(2)
O1 C8 C9 C10 57.0(3)
C8 C9 C10 C11 -53.2(3)
C9 C10 C11 C12 53.0(3)
C10 C11 C12 O1 -57.0(3)
O2 C13 C14 C15 58.1(3)
C13 C14 C15 C16 -53.6(3)
C14 C15 C16 C17 52.3(3)
C15 C16 C17 O2 -55.6(3)
C11 C12 O1 C8 60.6(2)
C11 C12 O1 Yb1 -108.92(18)
C9 C8 O1 C12 -60.3(2)
C9 C8 O1 Yb1 109.62(19)
C16 C17 O2 C13 60.1(2)
C16 C17 O2 Yb1 -110.72(18)
C14 C13 O2 C17 -61.1(2)
C14 C13 O2 Yb1 111.07(17)
