#===============================================================================
 data_global
#===============================================================================
_audit_creation_date               2018-06-01

# 1. SUBMISSION DETAILS

_publ_contact_author_name        'Gregory Nocton'
_publ_contact_author_address    
;
LCM, CNRS, Ecole Polytechnique, Université Paris Saclay
F91128 Palaiseau
France
;
_publ_contact_author_email       greg.nocton@polytechnique.edu
_publ_contact_author_phone       330169334402
_publ_contact_author_fax         330169334040

_publ_contact_letter
;
;
#===============================================================================

# TITLE AND AUTHOR LIST

_publ_section_title
;
Lanthanidocenes: Synthesis and Structure of
Linear Sandwich Complexes of Lanthanides
;
# The loop structure below should contain the names  and addresses of all
# authors, in the required order  of publication. Repeat as necessary.


loop_
_publ_author_name
;
[1] Mathieu Xémard
[1] Sébastien Zimmer
[1] Marie Cordier
[1] Violaine Goudy
[1] Louis Ricard
[2] Carine Clavaguéra
[1] Grégory Nocton
;
_publ_author_address
;
[1] LCM, CNRS, Ecole polytechnique, Université Paris-Saclay, 
Route de Saclay, Palaiseau, France
[2] Laboratoire de Chimie Physique, CNRS-Universite_ Paris-Sud,
Universite_ Paris-Saclay, 15 avenue Jean Perrin, 91405 Orsay Cedex,
France
;

#===============================================================================

data_KL1OEt2
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C13 H19 K O'
_chemical_formula_sum
 'C13 H19 K O' 
_chemical_formula_weight          230.38

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'
 'K'  'K'   0.2009   0.2494
 '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'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/n'
_space_group_name_Hall            '-P 2yn'
 
_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.
;
 
loop_
 _space_group_symop_operation_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'
 
_cell_length_a                    7.6540(4)
_cell_length_b                    17.3050(9)
_cell_length_c                    10.5413(6)
_cell_angle_alpha                 90
_cell_angle_beta                  107.269(2)
_cell_angle_gamma                 90
_cell_volume                      1333.28(12)
_cell_formula_units_Z             4
_cell_measurement_temperature     150.0(1)
_cell_measurement_reflns_used     3500
_cell_measurement_theta_min        2.3407
_cell_measurement_theta_max       27.2604
 
_exptl_crystal_description        'plate'
_exptl_crystal_colour             'greenish brown'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.148          
_exptl_crystal_F_000              496
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.240
_exptl_crystal_size_mid           0.200
_exptl_crystal_size_min           0.120
_exptl_absorpt_coefficient_mu     0.373
_shelx_estimated_absorpt_T_min    0.916
_shelx_estimated_absorpt_T_max    0.957
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min    0.6979
_exptl_absorpt_correction_T_max    0.7456
_exptl_absorpt_process_details    'SADABS'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       150(2)
_diffrn_radiation_wavelength      0.71069
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   'Kappa APEX II'
_diffrn_measurement_method        'phi and omega scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             9473
_diffrn_reflns_av_unetI/netI      0.0306
_diffrn_reflns_av_R_equivalents   0.0315
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -21
_diffrn_reflns_limit_k_max        21
_diffrn_reflns_limit_l_min        -13
_diffrn_reflns_limit_l_max        13
_diffrn_reflns_theta_min          2.341
_diffrn_reflns_theta_max          27.487
_diffrn_reflns_theta_full         25.240
_diffrn_measured_fraction_theta_max   0.990
_diffrn_measured_fraction_theta_full  0.998
_diffrn_reflns_Laue_measured_fraction_max    0.990
_diffrn_reflns_Laue_measured_fraction_full   0.998
_diffrn_reflns_point_group_measured_fraction_max   0.990
_diffrn_reflns_point_group_measured_fraction_full  0.998
_reflns_number_total              3027
_reflns_number_gt                 2442
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'Bruker APEX2'
_computing_cell_refinement        'Bruker SAINT'
_computing_data_reduction         'Bruker SAINT'
_computing_structure_solution     'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     'PLATON (Spek, 2009)'
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1006P)²+0.4131P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          3027
_refine_ls_number_parameters      154
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0662
_refine_ls_R_factor_gt            0.0536
_refine_ls_wR_factor_ref          0.1660
_refine_ls_wR_factor_gt           0.1534
_refine_ls_goodness_of_fit_ref    1.051
_refine_ls_restrained_S_all       1.051
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
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
 _atom_site_disorder_assembly
 _atom_site_disorder_group
K1 K 0.52327(6) 0.28503(3) 0.12096(4) 0.0421(2) Uani 1 1 d . . . . .
O1 O 0.61837(19) 0.43435(8) 0.15758(15) 0.0421(4) Uani 1 1 d . . . . .
C1 C 0.4213(7) 0.1411(3) -0.0464(4) 0.0439(15) Uani 0.602(12) 1 d . . P A 1
H1 H 0.3202 0.1534 -0.1210 0.053 Uiso 0.602(12) 1 calc R U P A 1
C1A C 0.5013(13) 0.1110(5) -0.0018(9) 0.065(3) Uani 0.398(12) 1 d . . P A 2
H1A H 0.5603 0.0622 0.0147 0.078 Uiso 0.398(12) 1 calc R U P A 2
C2 C 0.3616(4) 0.11408(16) 0.0546(3) 0.0627(7) Uani 1 1 d . . . . .
H2 H 0.4185 0.0731 0.1120 0.075 Uiso 0.602(12) 1 calc R U P A 1
H2A H 0.3763 0.0706 0.1119 0.075 Uiso 0.398(12) 1 calc R U P A 2
C3 C 0.2096(4) 0.15294(19) 0.0640(3) 0.0671(8) Uani 1 1 d . . . . .
H3 H 0.1525 0.1307 0.1240 0.081 Uiso 1 1 calc R U . . .
C4 C 0.1238(4) 0.22043(19) -0.0006(3) 0.0638(8) Uani 1 1 d . . . . .
H4 H 0.0131 0.2298 0.0201 0.077 Uiso 1 1 calc R U . . .
C5 C 0.1529(4) 0.27826(17) -0.0867(3) 0.0610(8) Uani 1 1 d . . . . .
H5 H 0.0567 0.3150 -0.1025 0.073 Uiso 1 1 calc R U . . .
C6 C 0.2782(4) 0.30118(15) -0.1595(2) 0.0534(6) Uani 1 1 d . . . . .
H6 H 0.2373 0.3485 -0.2042 0.064 Uiso 1 1 calc R U . . .
C7 C 0.4389(4) 0.27785(17) -0.1870(2) 0.0577(7) Uani 1 1 d . . . . .
H7 H 0.4651 0.3121 -0.2493 0.069 Uiso 1 1 calc R U . . .
C8 C 0.5705(5) 0.22102(18) -0.1522(3) 0.0653(8) Uani 1 1 d . . . . .
H8 H 0.6700 0.2275 -0.1878 0.078 Uiso 1 1 calc R U . . .
C9 C 0.5812(4) 0.1560(2) -0.0736(3) 0.0669(8) Uani 1 1 d . . . . .
H9 H 0.6881 0.1252 -0.0423 0.080 Uiso 0.602(12) 1 calc R U P A 1
H9A H 0.6956 0.1325 -0.0675 0.080 Uiso 0.398(12) 1 calc R U P A 2
C10 C 0.8429(3) 0.40891(16) 0.0474(3) 0.0561(6) Uani 1 1 d . . . . .
H10A H 0.9407 0.4326 0.0181 0.082(10) Uiso 1 1 calc R . . . .
H10B H 0.7443 0.3919 -0.0303 0.049(7) Uiso 1 1 calc R . . . .
H10C H 0.8917 0.3643 0.1041 0.066(8) Uiso 1 1 calc R . . . .
C11 C 0.7697(3) 0.46679(13) 0.1240(3) 0.0500(6) Uani 1 1 d . . . . .
H11A H 0.8666 0.4814 0.2059 0.060 Uiso 1 1 calc R U . . .
H11B H 0.7304 0.5139 0.0698 0.060 Uiso 1 1 calc R U . . .
C12 C 0.5459(4) 0.48512(14) 0.2356(3) 0.0542(6) Uani 1 1 d . . . . .
H12A H 0.5072 0.5342 0.1873 0.065 Uiso 1 1 calc R U . . .
H12B H 0.6407 0.4969 0.3203 0.065 Uiso 1 1 calc R U . . .
C13 C 0.3859(4) 0.44722(17) 0.2631(3) 0.0666(7) Uani 1 1 d . . . . .
H13A H 0.3311 0.4828 0.3128 0.075(9) Uiso 1 1 calc R . . . .
H13B H 0.4264 0.4003 0.3155 0.085(10) Uiso 1 1 calc R . . . .
H13C H 0.2949 0.4337 0.1789 0.071(9) Uiso 1 1 calc R . . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
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
K1 O1 2.6811(15) . ?
K1 C6 2.951(2) 4_666 ?
K1 C6 3.007(2) . ?
K1 C1 3.018(3) . ?
K1 C5 3.026(3) . ?
K1 C7 3.118(3) . ?
K1 C5 3.141(2) 4_666 ?
K1 C4 3.148(3) . ?
K1 C9 3.151(3) . ?
K1 C2 3.203(3) . ?
K1 C8 3.205(3) . ?
K1 C3 3.240(3) . ?
O1 C11 1.423(3) . ?
O1 C12 1.424(3) . ?
C1 C2 1.360(5) . ?
C1 C9 1.362(5) . ?
C1 H1 0.9500 . ?
C1A C9 1.352(10) . ?
C1A C2 1.370(9) . ?
C1A H1A 0.9500 . ?
C2 C3 1.373(4) . ?
C2 H2 0.9500 . ?
C2 H2A 0.9500 . ?
C3 C4 1.412(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.413(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.450(4) . ?
C5 K1 3.141(2) 4_565 ?
C5 H5 0.9500 . ?
C6 C7 1.404(4) . ?
C6 K1 2.951(2) 4_565 ?
C6 H6 0.9500 . ?
C7 C8 1.378(4) . ?
C7 K1 3.403(3) 4_565 ?
C7 H7 0.9500 . ?
C8 C9 1.386(5) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C9 H9A 0.9500 . ?
C10 C11 1.496(4) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.491(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
 
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 K1 C6 106.63(6) . 4_666 ?
O1 K1 C6 96.63(6) . . ?
C6 K1 C6 153.15(5) 4_666 . ?
O1 K1 C1 153.08(10) . . ?
C6 K1 C1 92.13(13) 4_666 . ?
C6 K1 C1 61.61(12) . . ?
O1 K1 C5 107.31(7) . . ?
C6 K1 C5 143.81(8) 4_666 . ?
C6 K1 C5 27.81(8) . . ?
C1 K1 C5 61.38(13) . . ?
O1 K1 C7 98.73(6) . . ?
C6 K1 C7 132.89(8) 4_666 . ?
C6 K1 C7 26.42(8) . . ?
C1 K1 C7 54.62(11) . . ?
C5 K1 C7 52.07(8) . . ?
O1 K1 C5 101.63(7) . 4_666 ?
C6 K1 C5 27.31(8) 4_666 4_666 ?
C6 K1 C5 156.94(7) . 4_666 ?
C1 K1 C5 103.72(12) . 4_666 ?
C5 K1 C5 130.66(9) . 4_666 ?
C7 K1 C5 156.18(8) . 4_666 ?
O1 K1 C4 126.17(7) . . ?
C6 K1 C4 118.41(8) 4_666 . ?
C6 K1 C4 52.12(8) . . ?
C1 K1 C4 54.39(11) . . ?
C5 K1 C4 26.36(8) . . ?
C7 K1 C4 71.72(8) . . ?
C5 K1 C4 105.14(8) 4_666 . ?
O1 K1 C9 133.80(7) . . ?
C6 K1 C9 87.95(8) 4_666 . ?
C6 K1 C9 65.99(8) . . ?
C1 K1 C9 25.39(10) . . ?
C5 K1 C9 77.54(7) . . ?
C7 K1 C9 47.15(9) . . ?
C5 K1 C9 109.08(9) 4_666 . ?
C4 K1 C9 77.92(7) . . ?
O1 K1 C2 172.92(7) . . ?
C6 K1 C2 80.03(8) 4_666 . ?
C6 K1 C2 77.49(7) . . ?
C1 K1 C2 25.03(10) . . ?
C5 K1 C2 65.68(8) . . ?
C7 K1 C2 77.80(7) . . ?
C5 K1 C2 83.17(7) 4_666 . ?
C4 K1 C2 46.97(8) . . ?
C9 K1 C2 47.40(8) . . ?
O1 K1 C8 111.37(7) . . ?
C6 K1 C8 107.77(8) 4_666 . ?
C6 K1 C8 49.65(8) . . ?
C1 K1 C8 42.95(10) . . ?
C5 K1 C8 70.60(8) . . ?
C7 K1 C8 25.12(8) . . ?
C5 K1 C8 132.38(9) 4_666 . ?
C4 K1 C8 82.34(8) . . ?
C9 K1 C8 25.16(8) . . ?
C2 K1 C8 67.91(8) . . ?
O1 K1 C3 149.46(7) . . ?
C6 K1 C3 94.00(8) 4_666 . ?
C6 K1 C3 70.84(8) . . ?
C1 K1 C3 42.32(10) . . ?
C5 K1 C3 49.84(9) . . ?
C7 K1 C3 82.30(7) . . ?
C5 K1 C3 86.37(8) 4_666 . ?
C4 K1 C3 25.49(8) . . ?
C9 K1 C3 67.61(8) . . ?
C2 K1 C3 24.60(8) . . ?
C8 K1 C3 82.23(8) . . ?
C11 O1 C12 112.69(17) . . ?
C11 O1 K1 123.41(13) . . ?
C12 O1 K1 122.83(13) . . ?
C2 C1 C9 139.6(5) . . ?
C2 C1 K1 85.12(19) . . ?
C9 C1 K1 82.80(19) . . ?
C2 C1 H1 110.2 . . ?
C9 C1 H1 110.2 . . ?
K1 C1 H1 107.8 . . ?
C9 C1A C2 139.6(8) . . ?
C9 C1A K1 73.3(3) . . ?
C2 C1A K1 75.4(3) . . ?
C9 C1A H1A 110.2 . . ?
C2 C1A H1A 110.2 . . ?
K1 C1A H1A 141.6 . . ?
C1 C2 C3 112.2(4) . . ?
C1A C2 C3 146.9(5) . . ?
C1 C2 K1 69.85(18) . . ?
C1A C2 K1 80.2(3) . . ?
C3 C2 K1 79.20(17) . . ?
C1 C2 H2 123.9 . . ?
C3 C2 H2 123.9 . . ?
K1 C2 H2 118.5 . . ?
C1A C2 H2A 106.6 . . ?
C3 C2 H2A 106.6 . . ?
K1 C2 H2A 128.9 . . ?
C2 C3 C4 130.8(3) . . ?
C2 C3 K1 76.20(15) . . ?
C4 C3 K1 73.65(16) . . ?
C2 C3 H3 114.6 . . ?
C4 C3 H3 114.6 . . ?
K1 C3 H3 128.6 . . ?
C3 C4 C5 139.2(3) . . ?
C3 C4 K1 80.86(16) . . ?
C5 C4 K1 71.97(15) . . ?
C3 C4 H4 110.4 . . ?
C5 C4 H4 110.4 . . ?
K1 C4 H4 132.1 . . ?
C4 C5 C6 142.1(3) . . ?
C4 C5 K1 81.67(16) . . ?
C6 C5 K1 75.38(14) . . ?
C4 C5 K1 108.63(17) . 4_565 ?
C6 C5 K1 69.03(13) . 4_565 ?
K1 C5 K1 132.74(9) . 4_565 ?
C4 C5 H5 108.9 . . ?
C6 C5 H5 108.9 . . ?
K1 C5 H5 127.7 . . ?
K1 C5 H5 93.4 4_565 . ?
C7 C6 C5 142.0(3) . . ?
C7 C6 K1 96.23(15) . 4_565 ?
C5 C6 K1 83.66(14) . 4_565 ?
C7 C6 K1 81.21(15) . . ?
C5 C6 K1 76.81(14) . . ?
K1 C6 K1 142.96(9) 4_565 . ?
C7 C6 H6 109.0 . . ?
C5 C6 H6 109.0 . . ?
K1 C6 H6 90.2 4_565 . ?
K1 C6 H6 125.8 . . ?
C8 C7 C6 140.1(3) . . ?
C8 C7 K1 80.94(16) . . ?
C6 C7 K1 72.37(13) . . ?
C8 C7 K1 114.25(18) . 4_565 ?
C6 C7 K1 59.55(13) . 4_565 ?
K1 C7 K1 120.02(8) . 4_565 ?
C8 C7 H7 110.0 . . ?
C6 C7 H7 110.0 . . ?
K1 C7 H7 132.4 . . ?
K1 C7 H7 98.1 4_565 . ?
C7 C8 C9 130.4(3) . . ?
C7 C8 K1 73.94(15) . . ?
C9 C8 K1 75.27(16) . . ?
C7 C8 H8 114.8 . . ?
C9 C8 H8 114.8 . . ?
K1 C8 H8 129.2 . . ?
C1A C9 C8 147.8(5) . . ?
C1 C9 C8 112.5(4) . . ?
C1A C9 K1 82.5(3) . . ?
C1 C9 K1 71.81(18) . . ?
C8 C9 K1 79.56(16) . . ?
C1 C9 H9 123.7 . . ?
C8 C9 H9 123.7 . . ?
K1 C9 H9 116.4 . . ?
C1A C9 H9A 106.1 . . ?
C8 C9 H9A 106.1 . . ?
K1 C9 H9A 124.3 . . ?
C11 C10 K1 83.81(13) . . ?
C11 C10 H10A 109.5 . . ?
K1 C10 H10A 166.7 . . ?
C11 C10 H10B 109.5 . . ?
K1 C10 H10B 65.6 . . ?
H10A C10 H10B 109.5 . . ?
C11 C10 H10C 109.5 . . ?
K1 C10 H10C 63.1 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O1 C11 C10 109.45(18) . . ?
O1 C11 H11A 109.8 . . ?
C10 C11 H11A 109.8 . . ?
O1 C11 H11B 109.8 . . ?
C10 C11 H11B 109.8 . . ?
H11A C11 H11B 108.2 . . ?
O1 C12 C13 108.9(2) . . ?
O1 C12 H12A 109.9 . . ?
C13 C12 H12A 109.9 . . ?
O1 C12 H12B 109.9 . . ?
C13 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
C12 C13 K1 84.32(14) . . ?
C12 C13 H13A 109.5 . . ?
K1 C13 H13A 165.3 . . ?
C12 C13 H13B 109.5 . . ?
K1 C13 H13B 59.3 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
K1 C13 H13C 69.0 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
 
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
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
C9 C1 C2 C3 141.5(5) . . . . ?
K1 C1 C2 C3 68.6(2) . . . . ?
C9 C1 C2 K1 72.9(5) . . . . ?
C9 C1A C2 C3 12.2(14) . . . . ?
K1 C1A C2 C3 52.2(6) . . . . ?
C9 C1A C2 K1 -40.0(8) . . . . ?
C1 C2 C3 C4 -9.3(4) . . . . ?
C1A C2 C3 C4 1.1(8) . . . . ?
K1 C2 C3 C4 53.5(3) . . . . ?
C1 C2 C3 K1 -62.9(2) . . . . ?
C1A C2 C3 K1 -52.4(7) . . . . ?
C2 C3 C4 C5 -6.2(6) . . . . ?
K1 C3 C4 C5 48.3(3) . . . . ?
C2 C3 C4 K1 -54.5(3) . . . . ?
C3 C4 C5 C6 2.1(6) . . . . ?
K1 C4 C5 C6 52.9(3) . . . . ?
C3 C4 C5 K1 -50.8(4) . . . . ?
C3 C4 C5 K1 81.6(4) . . . 4_565 ?
K1 C4 C5 K1 132.41(12) . . . 4_565 ?
C4 C5 C6 C7 1.7(6) . . . . ?
K1 C5 C6 C7 56.3(3) . . . . ?
K1 C5 C6 C7 -92.0(3) 4_565 . . . ?
C4 C5 C6 K1 93.7(4) . . . 4_565 ?
K1 C5 C6 K1 148.32(7) . . . 4_565 ?
C4 C5 C6 K1 -54.6(3) . . . . ?
K1 C5 C6 K1 -148.32(7) 4_565 . . . ?
C5 C6 C7 C8 -4.6(6) . . . . ?
K1 C6 C7 C8 -92.3(4) 4_565 . . . ?
K1 C6 C7 C8 50.4(4) . . . . ?
C5 C6 C7 K1 -55.0(3) . . . . ?
K1 C6 C7 K1 -142.72(9) 4_565 . . . ?
C5 C6 C7 K1 87.7(3) . . . 4_565 ?
K1 C6 C7 K1 142.72(9) . . . 4_565 ?
C6 C7 C8 C9 5.7(6) . . . . ?
K1 C7 C8 C9 53.7(3) . . . . ?
K1 C7 C8 C9 -65.2(4) 4_565 . . . ?
C6 C7 C8 K1 -48.1(3) . . . . ?
K1 C7 C8 K1 -118.93(13) 4_565 . . . ?
C2 C1A C9 C8 -15.9(14) . . . . ?
K1 C1A C9 C8 -56.4(7) . . . . ?
C2 C1A C9 K1 40.5(9) . . . . ?
C2 C1 C9 C8 -143.6(5) . . . . ?
K1 C1 C9 C8 -70.0(2) . . . . ?
C2 C1 C9 K1 -73.7(5) . . . . ?
C7 C8 C9 C1A 3.9(9) . . . . ?
K1 C8 C9 C1A 57.1(7) . . . . ?
C7 C8 C9 C1 11.9(4) . . . . ?
K1 C8 C9 C1 65.2(2) . . . . ?
C7 C8 C9 K1 -53.2(3) . . . . ?
C12 O1 C11 C10 177.6(2) . . . . ?
K1 O1 C11 C10 9.1(3) . . . . ?
K1 C10 C11 O1 -5.85(16) . . . . ?
C11 O1 C12 C13 178.6(2) . . . . ?
K1 O1 C12 C13 -12.9(3) . . . . ?
O1 C12 C13 K1 8.30(17) . . . . ?
 
_refine_diff_density_max    0.591
_refine_diff_density_min   -0.264
_refine_diff_density_rms    0.072



# ===END

 
data_1
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C18 H18 Yb'
_chemical_formula_sum
 'C18 H18 Yb' 
_chemical_formula_weight          407.36

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'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/n'
_space_group_name_Hall            '-P 2yn'
 
_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.
;
 
loop_
 _space_group_symop_operation_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'
 
_cell_length_a                    7.3832(5)
_cell_length_b                    8.9146(6)
_cell_length_c                    11.0651(8)
_cell_angle_alpha                 90
_cell_angle_beta                  99.998(2)
_cell_angle_gamma                 90
_cell_volume                      717.23(9)
_cell_formula_units_Z             2
_cell_measurement_temperature     150.0(1)
_cell_measurement_reflns_used     9992
_cell_measurement_theta_min        2.9522
_cell_measurement_theta_max       29.9982
 
_exptl_crystal_description        'block'
_exptl_crystal_colour             'yellow'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.886          
_exptl_crystal_F_000              392
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.220
_exptl_crystal_size_mid           0.060
_exptl_crystal_size_min           0.060
_exptl_absorpt_coefficient_mu     6.502
_shelx_estimated_absorpt_T_min    0.509
_shelx_estimated_absorpt_T_max    0.624
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min    0.5157
_exptl_absorpt_correction_T_max    0.7467
_exptl_absorpt_process_details    'SADABS'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       150(2)
_diffrn_radiation_wavelength      0.71069
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   'Kappa APEX II'
_diffrn_measurement_method        'phi and omega scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_av_unetI/netI      0.0224
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -4
_diffrn_reflns_limit_l_max        17
_diffrn_reflns_theta_min          3.616
_diffrn_reflns_theta_max          33.845
_diffrn_reflns_theta_full         25.240
_diffrn_reflns_number             31319
_diffrn_measured_fraction_theta_max   0.997
_diffrn_measured_fraction_theta_full  0.998
_diffrn_reflns_Laue_measured_fraction_max    0.997
_diffrn_reflns_Laue_measured_fraction_full   0.998
_diffrn_reflns_point_group_measured_fraction_max   0.997
_diffrn_reflns_point_group_measured_fraction_full  0.998
_reflns_number_total              2886
_reflns_number_gt                 2100
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'Bruker APEX2'
_computing_cell_refinement        'Bruker SAINT'
_computing_data_reduction         'Bruker SAINT'
_computing_structure_solution     'SHELXT(Sheldrick,2014)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     'PLATON (Spek, 2009)'
_computing_publication_material   ?
_refine_special_details
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0179P)²+7.3443P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          2886
_refine_ls_number_parameters      170
_refine_ls_number_restraints      108
_refine_ls_R_factor_all           0.0550
_refine_ls_R_factor_gt            0.0401
_refine_ls_wR_factor_ref          0.1182
_refine_ls_wR_factor_gt           0.1127
_refine_ls_goodness_of_fit_ref    1.368
_refine_ls_restrained_S_all       1.351
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
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
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Yb1 Yb 0.0000 0.0000 0.0000 0.02118(10) Uani 1 2 d S . P . .
C1 C 0.143(3) 0.009(3) 0.2491(15) 0.039(3) Uani 0.5 1 d . U P A 1
H1 H 0.1702 -0.0599 0.3150 0.047 Uiso 0.5 1 calc R U P A 1
C2 C 0.291(3) 0.019(3) 0.192(2) 0.043(4) Uani 0.5 1 d . U P A 1
H2 H 0.3822 -0.0502 0.2281 0.052 Uiso 0.5 1 calc R U P A 1
C3 C 0.355(3) 0.096(3) 0.099(2) 0.039(4) Uani 0.5 1 d . U P A 1
H3 H 0.4783 0.0691 0.0967 0.047 Uiso 0.5 1 calc R U P A 1
C4 C 0.291(3) 0.203(3) 0.007(2) 0.033(3) Uani 0.5 1 d . U P A 1
H4 H 0.3818 0.2219 -0.0422 0.040 Uiso 0.5 1 calc R U P A 1
C5 C 0.140(3) 0.285(2) -0.0322(15) 0.025(3) Uani 0.5 1 d . U P A 1
H5 H 0.1550 0.3427 -0.1020 0.030 Uiso 0.5 1 calc R U P A 1
C6 C -0.029(2) 0.3100(17) -0.0008(15) 0.024(3) Uani 0.5 1 d . U P A 1
H6 H -0.0870 0.3868 -0.0535 0.029 Uiso 0.5 1 calc R U P A 1
C7 C -0.152(2) 0.269(2) 0.0770(15) 0.024(2) Uani 0.5 1 d . U P A 1
H7 H -0.2651 0.3218 0.0571 0.029 Uiso 0.5 1 calc R U P A 1
C8 C -0.153(3) 0.171(2) 0.1768(16) 0.030(3) Uani 0.5 1 d . U P A 1
H8 H -0.2664 0.1773 0.2066 0.035 Uiso 0.5 1 calc R U P A 1
C9 C -0.033(4) 0.064(3) 0.2454(16) 0.038(4) Uani 0.5 1 d . U P A 1
H9 H -0.0907 0.0178 0.3062 0.045 Uiso 0.5 1 calc R U P A 1
C10 C -0.222(3) 0.027(3) -0.2316(15) 0.040(4) Uani 0.5 1 d . U P A 2
H10 H -0.2768 0.1097 -0.2782 0.048 Uiso 0.5 1 calc R U P A 2
C11 C -0.340(2) -0.032(2) -0.1561(17) 0.030(3) Uani 0.5 1 d . U P A 2
H11 H -0.4579 0.0141 -0.1758 0.037 Uiso 0.5 1 calc R U P A 2
C12 C -0.341(3) -0.138(3) -0.0602(19) 0.033(3) Uani 0.5 1 d . U P A 2
H12 H -0.4573 -0.1355 -0.0347 0.040 Uiso 0.5 1 calc R U P A 2
C13 C -0.234(4) -0.239(3) 0.007(2) 0.037(4) Uani 0.5 1 d . U P A 2
H13 H -0.2975 -0.2805 0.0664 0.044 Uiso 0.5 1 calc R U P A 2
C14 C -0.066(3) -0.302(2) 0.018(2) 0.044(4) Uani 0.5 1 d . U P A 2
H14 H -0.0519 -0.3763 0.0809 0.053 Uiso 0.5 1 calc R U P A 2
C15 C 0.092(3) -0.293(2) -0.034(2) 0.037(4) Uani 0.5 1 d . U P A 2
H15 H 0.1856 -0.3572 0.0076 0.045 Uiso 0.5 1 calc R U P A 2
C16 C 0.154(3) -0.214(3) -0.131(3) 0.045(4) Uani 0.5 1 d . U P A 2
H16 H 0.2705 -0.2521 -0.1416 0.054 Uiso 0.5 1 calc R U P A 2
C17 C 0.099(3) -0.099(3) -0.218(2) 0.044(4) Uani 0.5 1 d . U P A 2
H17 H 0.1933 -0.0795 -0.2644 0.052 Uiso 0.5 1 calc R U P A 2
C18 C -0.055(3) -0.002(3) -0.2554(12) 0.034(3) Uani 0.5 1 d . U P A 2
H18 H -0.0300 0.0630 -0.3185 0.041 Uiso 0.5 1 calc R U P A 2
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
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 C15 2.74(2) 3 ?
Yb1 C15 2.74(2) . ?
Yb1 C13 2.75(2) . ?
Yb1 C13 2.75(2) 3 ?
Yb1 C2 2.753(18) . ?
Yb1 C2 2.753(18) 3 ?
Yb1 C14 2.75(2) . ?
Yb1 C14 2.75(2) 3 ?
Yb1 C16 2.76(2) 3 ?
Yb1 C16 2.76(2) . ?
Yb1 C6 2.772(15) . ?
Yb1 C6 2.772(15) 3 ?
Yb1 C12 2.77(2) . ?
Yb1 C12 2.77(2) 3 ?
Yb1 C1 2.777(16) 3 ?
Yb1 C1 2.777(16) . ?
Yb1 C17 2.78(2) 3 ?
Yb1 C17 2.78(2) . ?
Yb1 C18 2.785(13) 3 ?
Yb1 C18 2.785(13) . ?
Yb1 C5 2.789(16) . ?
Yb1 C5 2.789(16) 3 ?
Yb1 C3 2.79(2) 3 ?
Yb1 C3 2.79(2) . ?
Yb1 C4 2.797(19) . ?
Yb1 C4 2.797(19) 3 ?
Yb1 C10 2.803(16) 3 ?
Yb1 C10 2.803(16) . ?
Yb1 C11 2.806(16) . ?
Yb1 C11 2.806(16) 3 ?
Yb1 C9 2.828(18) . ?
Yb1 C9 2.828(18) 3 ?
Yb1 C7 2.841(15) . ?
Yb1 C7 2.841(15) 3 ?
Yb1 C8 2.863(16) 3 ?
Yb1 C8 2.863(16) . ?
C1 C2 1.36(3) . ?
C1 C9 1.39(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.38(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.42(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.33(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.38(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.40(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.41(2) . ?
C7 H7 0.9500 . ?
C8 C9 1.42(3) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C18 1.33(3) . ?
C10 C11 1.41(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.42(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.34(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.34(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.39(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.43(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.42(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.43(3) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
 
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
C15 Yb1 C15 180.0 3 . ?
C15 Yb1 C13 124.3(8) 3 . ?
C15 Yb1 C13 55.7(8) . . ?
C15 Yb1 C13 55.7(8) 3 3 ?
C15 Yb1 C13 124.3(8) . 3 ?
C13 Yb1 C13 180.0(6) . 3 ?
C2 Yb1 C2 180.0 . 3 ?
C15 Yb1 C14 150.6(7) 3 . ?
C15 Yb1 C14 29.4(7) . . ?
C13 Yb1 C14 28.2(7) . . ?
C13 Yb1 C14 151.8(7) 3 . ?
C15 Yb1 C14 29.4(7) 3 3 ?
C15 Yb1 C14 150.6(7) . 3 ?
C13 Yb1 C14 151.8(7) . 3 ?
C13 Yb1 C14 28.2(7) 3 3 ?
C14 Yb1 C14 180.0 . 3 ?
C15 Yb1 C16 30.1(7) 3 3 ?
C15 Yb1 C16 149.9(7) . 3 ?
C13 Yb1 C16 101.8(8) . 3 ?
C13 Yb1 C16 78.2(8) 3 3 ?
C14 Yb1 C16 123.0(8) . 3 ?
C14 Yb1 C16 57.0(8) 3 3 ?
C15 Yb1 C16 149.9(7) 3 . ?
C15 Yb1 C16 30.1(7) . . ?
C13 Yb1 C16 78.2(8) . . ?
C13 Yb1 C16 101.8(8) 3 . ?
C14 Yb1 C16 57.0(8) . . ?
C14 Yb1 C16 123.0(8) 3 . ?
C16 Yb1 C16 180.0 3 . ?
C2 Yb1 C6 89.4(6) . . ?
C2 Yb1 C6 90.6(6) 3 . ?
C2 Yb1 C6 90.6(6) . 3 ?
C2 Yb1 C6 89.4(6) 3 3 ?
C6 Yb1 C6 180.0 . 3 ?
C15 Yb1 C12 102.6(6) 3 . ?
C15 Yb1 C12 77.4(6) . . ?
C13 Yb1 C12 28.0(6) . . ?
C13 Yb1 C12 152.0(6) 3 . ?
C14 Yb1 C12 54.5(7) . . ?
C14 Yb1 C12 125.5(7) 3 . ?
C16 Yb1 C12 89.6(6) 3 . ?
C16 Yb1 C12 90.4(6) . . ?
C15 Yb1 C12 77.4(6) 3 3 ?
C15 Yb1 C12 102.6(6) . 3 ?
C13 Yb1 C12 152.0(6) . 3 ?
C13 Yb1 C12 28.0(6) 3 3 ?
C14 Yb1 C12 125.5(7) . 3 ?
C14 Yb1 C12 54.5(7) 3 3 ?
C16 Yb1 C12 90.4(6) 3 3 ?
C16 Yb1 C12 89.6(6) . 3 ?
C12 Yb1 C12 180.0 . 3 ?
C2 Yb1 C1 151.6(7) . 3 ?
C2 Yb1 C1 28.4(7) 3 3 ?
C6 Yb1 C1 90.6(6) . 3 ?
C6 Yb1 C1 89.4(6) 3 3 ?
C2 Yb1 C1 28.4(7) . . ?
C2 Yb1 C1 151.6(7) 3 . ?
C6 Yb1 C1 89.4(6) . . ?
C6 Yb1 C1 90.6(6) 3 . ?
C1 Yb1 C1 180.0 3 . ?
C15 Yb1 C17 58.1(8) 3 3 ?
C15 Yb1 C17 121.9(8) . 3 ?
C13 Yb1 C17 87.7(7) . 3 ?
C13 Yb1 C17 92.3(7) 3 3 ?
C14 Yb1 C17 99.8(8) . 3 ?
C14 Yb1 C17 80.2(8) 3 3 ?
C16 Yb1 C17 29.6(8) 3 3 ?
C16 Yb1 C17 150.4(8) . 3 ?
C12 Yb1 C17 89.0(6) . 3 ?
C12 Yb1 C17 91.0(6) 3 3 ?
C15 Yb1 C17 121.9(8) 3 . ?
C15 Yb1 C17 58.1(8) . . ?
C13 Yb1 C17 92.3(7) . . ?
C13 Yb1 C17 87.7(7) 3 . ?
C14 Yb1 C17 80.2(8) . . ?
C14 Yb1 C17 99.8(8) 3 . ?
C16 Yb1 C17 150.4(8) 3 . ?
C16 Yb1 C17 29.6(8) . . ?
C12 Yb1 C17 91.0(6) . . ?
C12 Yb1 C17 89.0(6) 3 . ?
C17 Yb1 C17 180.0 3 . ?
C15 Yb1 C18 81.5(8) 3 3 ?
C15 Yb1 C18 98.5(8) . 3 ?
C13 Yb1 C18 87.7(6) . 3 ?
C13 Yb1 C18 92.3(6) 3 3 ?
C14 Yb1 C18 85.9(8) . 3 ?
C14 Yb1 C18 94.1(8) 3 3 ?
C16 Yb1 C18 57.5(8) 3 3 ?
C16 Yb1 C18 122.5(8) . 3 ?
C12 Yb1 C18 102.3(6) . 3 ?
C12 Yb1 C18 77.7(6) 3 3 ?
C17 Yb1 C18 29.9(7) 3 3 ?
C17 Yb1 C18 150.1(7) . 3 ?
C15 Yb1 C18 98.5(8) 3 . ?
C15 Yb1 C18 81.5(8) . . ?
C13 Yb1 C18 92.3(6) . . ?
C13 Yb1 C18 87.7(6) 3 . ?
C14 Yb1 C18 94.1(8) . . ?
C14 Yb1 C18 85.9(8) 3 . ?
C16 Yb1 C18 122.5(8) 3 . ?
C16 Yb1 C18 57.5(8) . . ?
C12 Yb1 C18 77.7(6) . . ?
C12 Yb1 C18 102.3(6) 3 . ?
C17 Yb1 C18 150.1(7) 3 . ?
C17 Yb1 C18 29.9(7) . . ?
C18 Yb1 C18 180.0 3 . ?
C2 Yb1 C5 77.5(7) . . ?
C2 Yb1 C5 102.5(7) 3 . ?
C6 Yb1 C5 28.6(5) . . ?
C6 Yb1 C5 151.4(5) 3 . ?
C1 Yb1 C5 89.2(6) 3 . ?
C1 Yb1 C5 90.8(6) . . ?
C2 Yb1 C5 102.5(7) . 3 ?
C2 Yb1 C5 77.5(7) 3 3 ?
C6 Yb1 C5 151.4(5) . 3 ?
C6 Yb1 C5 28.6(5) 3 3 ?
C1 Yb1 C5 90.8(6) 3 3 ?
C1 Yb1 C5 89.2(6) . 3 ?
C5 Yb1 C5 180.0 . 3 ?
C2 Yb1 C3 151.2(7) . 3 ?
C2 Yb1 C3 28.8(7) 3 3 ?
C6 Yb1 C3 103.7(6) . 3 ?
C6 Yb1 C3 76.3(6) 3 3 ?
C1 Yb1 C3 55.3(7) 3 3 ?
C1 Yb1 C3 124.7(7) . 3 ?
C5 Yb1 C3 124.9(7) . 3 ?
C5 Yb1 C3 55.1(7) 3 3 ?
C2 Yb1 C3 28.8(7) . . ?
C2 Yb1 C3 151.2(7) 3 . ?
C6 Yb1 C3 76.3(6) . . ?
C6 Yb1 C3 103.7(6) 3 . ?
C1 Yb1 C3 124.7(7) 3 . ?
C1 Yb1 C3 55.3(7) . . ?
C5 Yb1 C3 55.1(7) . . ?
C5 Yb1 C3 124.9(7) 3 . ?
C3 Yb1 C3 180.0 3 . ?
C2 Yb1 C4 56.4(8) . . ?
C2 Yb1 C4 123.6(8) 3 . ?
C6 Yb1 C4 54.1(6) . . ?
C6 Yb1 C4 125.9(6) 3 . ?
C1 Yb1 C4 101.8(7) 3 . ?
C1 Yb1 C4 78.2(7) . . ?
C5 Yb1 C4 27.6(6) . . ?
C5 Yb1 C4 152.4(6) 3 . ?
C3 Yb1 C4 150.6(7) 3 . ?
C3 Yb1 C4 29.4(7) . . ?
C2 Yb1 C4 123.6(8) . 3 ?
C2 Yb1 C4 56.4(8) 3 3 ?
C6 Yb1 C4 125.9(6) . 3 ?
C6 Yb1 C4 54.1(6) 3 3 ?
C1 Yb1 C4 78.2(7) 3 3 ?
C1 Yb1 C4 101.8(7) . 3 ?
C5 Yb1 C4 152.4(6) . 3 ?
C5 Yb1 C4 27.6(6) 3 3 ?
C3 Yb1 C4 29.4(7) 3 3 ?
C3 Yb1 C4 150.6(7) . 3 ?
C4 Yb1 C4 180.0 . 3 ?
C15 Yb1 C10 94.4(6) 3 3 ?
C15 Yb1 C10 85.6(6) . 3 ?
C13 Yb1 C10 100.3(7) . 3 ?
C13 Yb1 C10 79.7(7) 3 3 ?
C14 Yb1 C10 86.2(7) . 3 ?
C14 Yb1 C10 93.8(7) 3 3 ?
C16 Yb1 C10 78.9(7) 3 3 ?
C16 Yb1 C10 101.1(7) . 3 ?
C12 Yb1 C10 123.0(6) . 3 ?
C12 Yb1 C10 57.0(6) 3 3 ?
C17 Yb1 C10 55.6(7) 3 3 ?
C17 Yb1 C10 124.4(7) . 3 ?
C18 Yb1 C10 27.5(5) 3 3 ?
C18 Yb1 C10 152.5(5) . 3 ?
C15 Yb1 C10 85.6(6) 3 . ?
C15 Yb1 C10 94.4(6) . . ?
C13 Yb1 C10 79.7(7) . . ?
C13 Yb1 C10 100.3(7) 3 . ?
C14 Yb1 C10 93.8(7) . . ?
C14 Yb1 C10 86.2(7) 3 . ?
C16 Yb1 C10 101.1(7) 3 . ?
C16 Yb1 C10 78.9(7) . . ?
C12 Yb1 C10 57.0(6) . . ?
C12 Yb1 C10 123.0(6) 3 . ?
C17 Yb1 C10 124.4(7) 3 . ?
C17 Yb1 C10 55.6(7) . . ?
C18 Yb1 C10 152.5(5) 3 . ?
C18 Yb1 C10 27.5(5) . . ?
C10 Yb1 C10 180.0(9) 3 . ?
C15 Yb1 C11 87.9(5) 3 . ?
C15 Yb1 C11 92.1(5) . . ?
C13 Yb1 C11 55.9(6) . . ?
C13 Yb1 C11 124.1(6) 3 . ?
C14 Yb1 C11 78.1(6) . . ?
C14 Yb1 C11 101.9(6) 3 . ?
C16 Yb1 C11 89.3(6) 3 . ?
C16 Yb1 C11 90.7(6) . . ?
C12 Yb1 C11 29.5(6) . . ?
C12 Yb1 C11 150.5(6) 3 . ?
C17 Yb1 C11 102.8(6) 3 . ?
C17 Yb1 C11 77.2(6) . . ?
C18 Yb1 C11 125.7(5) 3 . ?
C18 Yb1 C11 54.3(5) . . ?
C10 Yb1 C11 150.9(5) 3 . ?
C10 Yb1 C11 29.1(5) . . ?
C15 Yb1 C11 92.1(5) 3 3 ?
C15 Yb1 C11 87.9(5) . 3 ?
C13 Yb1 C11 124.1(6) . 3 ?
C13 Yb1 C11 55.9(6) 3 3 ?
C14 Yb1 C11 101.9(6) . 3 ?
C14 Yb1 C11 78.1(6) 3 3 ?
C16 Yb1 C11 90.7(6) 3 3 ?
C16 Yb1 C11 89.3(6) . 3 ?
C12 Yb1 C11 150.5(6) . 3 ?
C12 Yb1 C11 29.5(6) 3 3 ?
C17 Yb1 C11 77.2(6) 3 3 ?
C17 Yb1 C11 102.8(6) . 3 ?
C18 Yb1 C11 54.3(5) 3 3 ?
C18 Yb1 C11 125.7(5) . 3 ?
C10 Yb1 C11 29.1(5) 3 3 ?
C10 Yb1 C11 150.9(5) . 3 ?
C11 Yb1 C11 180.0 . 3 ?
C2 Yb1 C9 55.4(7) . . ?
C2 Yb1 C9 124.6(7) 3 . ?
C6 Yb1 C9 77.3(6) . . ?
C6 Yb1 C9 102.7(6) 3 . ?
C1 Yb1 C9 151.3(7) 3 . ?
C1 Yb1 C9 28.7(7) . . ?
C5 Yb1 C9 92.0(5) . . ?
C5 Yb1 C9 88.0(5) 3 . ?
C3 Yb1 C9 102.0(7) 3 . ?
C3 Yb1 C9 78.0(7) . . ?
C4 Yb1 C9 92.1(6) . . ?
C4 Yb1 C9 87.9(6) 3 . ?
C2 Yb1 C9 124.6(7) . 3 ?
C2 Yb1 C9 55.4(7) 3 3 ?
C6 Yb1 C9 102.7(6) . 3 ?
C6 Yb1 C9 77.3(6) 3 3 ?
C1 Yb1 C9 28.7(7) 3 3 ?
C1 Yb1 C9 151.3(7) . 3 ?
C5 Yb1 C9 88.0(5) . 3 ?
C5 Yb1 C9 92.0(5) 3 3 ?
C3 Yb1 C9 78.0(7) 3 3 ?
C3 Yb1 C9 102.0(7) . 3 ?
C4 Yb1 C9 87.9(6) . 3 ?
C4 Yb1 C9 92.1(6) 3 3 ?
C9 Yb1 C9 180.0 . 3 ?
C2 Yb1 C7 90.7(6) . . ?
C2 Yb1 C7 89.3(6) 3 . ?
C6 Yb1 C7 28.9(4) . . ?
C6 Yb1 C7 151.1(4) 3 . ?
C1 Yb1 C7 102.8(6) 3 . ?
C1 Yb1 C7 77.2(6) . . ?
C5 Yb1 C7 56.3(6) . . ?
C5 Yb1 C7 123.7(6) 3 . ?
C3 Yb1 C7 89.1(6) 3 . ?
C3 Yb1 C7 90.9(6) . . ?
C4 Yb1 C7 77.7(5) . . ?
C4 Yb1 C7 102.3(5) 3 . ?
C9 Yb1 C7 55.6(6) . . ?
C9 Yb1 C7 124.4(6) 3 . ?
C2 Yb1 C7 89.3(6) . 3 ?
C2 Yb1 C7 90.7(6) 3 3 ?
C6 Yb1 C7 151.1(4) . 3 ?
C6 Yb1 C7 28.9(4) 3 3 ?
C1 Yb1 C7 77.2(6) 3 3 ?
C1 Yb1 C7 102.8(6) . 3 ?
C5 Yb1 C7 123.7(6) . 3 ?
C5 Yb1 C7 56.3(6) 3 3 ?
C3 Yb1 C7 90.9(6) 3 3 ?
C3 Yb1 C7 89.1(6) . 3 ?
C4 Yb1 C7 102.3(5) . 3 ?
C4 Yb1 C7 77.7(5) 3 3 ?
C9 Yb1 C7 124.4(6) . 3 ?
C9 Yb1 C7 55.6(6) 3 3 ?
C7 Yb1 C7 180.0(6) . 3 ?
C2 Yb1 C8 102.2(6) . 3 ?
C2 Yb1 C8 77.8(6) 3 3 ?
C6 Yb1 C8 124.6(5) . 3 ?
C6 Yb1 C8 55.4(5) 3 3 ?
C1 Yb1 C8 55.5(7) 3 3 ?
C1 Yb1 C8 124.5(7) . 3 ?
C5 Yb1 C8 101.3(5) . 3 ?
C5 Yb1 C8 78.7(5) 3 3 ?
C3 Yb1 C8 91.3(6) 3 3 ?
C3 Yb1 C8 88.7(6) . 3 ?
C4 Yb1 C8 88.2(5) . 3 ?
C4 Yb1 C8 91.8(5) 3 3 ?
C9 Yb1 C8 151.0(6) . 3 ?
C9 Yb1 C8 29.0(6) 3 3 ?
C7 Yb1 C8 151.4(5) . 3 ?
C7 Yb1 C8 28.6(5) 3 3 ?
C2 Yb1 C8 77.8(6) . . ?
C2 Yb1 C8 102.2(6) 3 . ?
C6 Yb1 C8 55.4(5) . . ?
C6 Yb1 C8 124.6(5) 3 . ?
C1 Yb1 C8 124.5(7) 3 . ?
C1 Yb1 C8 55.5(7) . . ?
C5 Yb1 C8 78.7(5) . . ?
C5 Yb1 C8 101.3(5) 3 . ?
C3 Yb1 C8 88.7(6) 3 . ?
C3 Yb1 C8 91.3(6) . . ?
C4 Yb1 C8 91.8(5) . . ?
C4 Yb1 C8 88.2(5) 3 . ?
C9 Yb1 C8 29.0(6) . . ?
C9 Yb1 C8 151.0(6) 3 . ?
C7 Yb1 C8 28.6(5) . . ?
C7 Yb1 C8 151.4(5) 3 . ?
C8 Yb1 C8 180.0 3 . ?
C2 C1 C9 142(2) . . ?
C2 C1 Yb1 74.8(10) . . ?
C9 C1 Yb1 77.7(10) . . ?
C2 C1 H1 108.8 . . ?
C9 C1 H1 108.8 . . ?
Yb1 C1 H1 137.4 . . ?
C1 C2 C3 142(2) . . ?
C1 C2 Yb1 76.8(11) . . ?
C3 C2 Yb1 77.1(11) . . ?
C1 C2 H2 109.2 . . ?
C3 C2 H2 109.2 . . ?
Yb1 C2 H2 133.2 . . ?
C2 C3 C4 139(2) . . ?
C2 C3 Yb1 74.0(11) . . ?
C4 C3 Yb1 75.5(10) . . ?
C2 C3 H3 110.5 . . ?
C4 C3 H3 110.5 . . ?
Yb1 C3 H3 138.7 . . ?
C5 C4 C3 139.0(19) . . ?
C5 C4 Yb1 75.8(10) . . ?
C3 C4 Yb1 75.1(12) . . ?
C5 C4 H4 110.5 . . ?
C3 C4 H4 110.5 . . ?
Yb1 C4 H4 135.8 . . ?
C4 C5 C6 138.6(17) . . ?
C4 C5 Yb1 76.5(11) . . ?
C6 C5 Yb1 75.0(9) . . ?
C4 C5 H5 110.7 . . ?
C6 C5 H5 110.7 . . ?
Yb1 C5 H5 134.0 . . ?
C5 C6 C7 145.7(17) . . ?
C5 C6 Yb1 76.4(10) . . ?
C7 C6 Yb1 78.2(9) . . ?
C5 C6 H6 107.1 . . ?
C7 C6 H6 107.1 . . ?
Yb1 C6 H6 138.2 . . ?
C6 C7 C8 137.3(16) . . ?
C6 C7 Yb1 72.8(8) . . ?
C8 C7 Yb1 76.5(10) . . ?
C6 C7 H7 111.3 . . ?
C8 C7 H7 111.3 . . ?
Yb1 C7 H7 136.5 . . ?
C7 C8 C9 137.9(17) . . ?
C7 C8 Yb1 74.8(9) . . ?
C9 C8 Yb1 74.2(10) . . ?
C7 C8 H8 111.0 . . ?
C9 C8 H8 111.0 . . ?
Yb1 C8 H8 138.2 . . ?
C1 C9 C8 138.3(18) . . ?
C1 C9 Yb1 73.6(10) . . ?
C8 C9 Yb1 76.9(9) . . ?
C1 C9 H9 110.9 . . ?
C8 C9 H9 110.9 . . ?
Yb1 C9 H9 135.6 . . ?
C18 C10 C11 137(2) . . ?
C18 C10 Yb1 75.5(9) . . ?
C11 C10 Yb1 75.6(9) . . ?
C18 C10 H10 111.3 . . ?
C11 C10 H10 111.3 . . ?
Yb1 C10 H10 133.5 . . ?
C10 C11 C12 140.5(18) . . ?
C10 C11 Yb1 75.3(9) . . ?
C12 C11 Yb1 74.0(10) . . ?
C10 C11 H11 109.8 . . ?
C12 C11 H11 109.8 . . ?
Yb1 C11 H11 141.4 . . ?
C13 C12 C11 141.7(19) . . ?
C13 C12 Yb1 75.0(12) . . ?
C11 C12 Yb1 76.5(10) . . ?
C13 C12 H12 109.1 . . ?
C11 C12 H12 109.1 . . ?
Yb1 C12 H12 138.6 . . ?
C12 C13 C14 141(2) . . ?
C12 C13 Yb1 76.9(12) . . ?
C14 C13 Yb1 76.0(12) . . ?
C12 C13 H13 109.3 . . ?
C14 C13 H13 109.3 . . ?
Yb1 C13 H13 135.1 . . ?
C13 C14 C15 140(2) . . ?
C13 C14 Yb1 75.8(12) . . ?
C15 C14 Yb1 74.8(13) . . ?
C13 C14 H14 110.2 . . ?
C15 C14 H14 110.2 . . ?
Yb1 C14 H14 137.2 . . ?
C14 C15 C16 138(2) . . ?
C14 C15 Yb1 75.8(12) . . ?
C16 C15 Yb1 75.7(12) . . ?
C14 C15 H15 111.0 . . ?
C16 C15 H15 111.0 . . ?
Yb1 C15 H15 133.3 . . ?
C17 C16 C15 141(2) . . ?
C17 C16 Yb1 75.9(13) . . ?
C15 C16 Yb1 74.2(12) . . ?
C17 C16 H16 109.5 . . ?
C15 C16 H16 109.5 . . ?
Yb1 C16 H16 140.7 . . ?
C16 C17 C18 139(2) . . ?
C16 C17 Yb1 74.5(13) . . ?
C18 C17 Yb1 75.3(10) . . ?
C16 C17 H17 110.6 . . ?
C18 C17 H17 110.6 . . ?
Yb1 C17 H17 138.0 . . ?
C10 C18 C17 141(2) . . ?
C10 C18 Yb1 77.0(9) . . ?
C17 C18 Yb1 74.8(11) . . ?
C10 C18 H18 109.5 . . ?
C17 C18 H18 109.5 . . ?
Yb1 C18 H18 136.8 . . ?
 
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
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
C9 C1 C2 C3 4(6) . . . . ?
Yb1 C1 C2 C3 48(3) . . . . ?
C9 C1 C2 Yb1 -45(3) . . . . ?
C1 C2 C3 C4 -5(5) . . . . ?
Yb1 C2 C3 C4 43(3) . . . . ?
C1 C2 C3 Yb1 -48(3) . . . . ?
C2 C3 C4 C5 3(4) . . . . ?
Yb1 C3 C4 C5 46(2) . . . . ?
C2 C3 C4 Yb1 -43(3) . . . . ?
C3 C4 C5 C6 2(4) . . . . ?
Yb1 C4 C5 C6 48(2) . . . . ?
C3 C4 C5 Yb1 -46(2) . . . . ?
C4 C5 C6 C7 -5(4) . . . . ?
Yb1 C5 C6 C7 43(2) . . . . ?
C4 C5 C6 Yb1 -48(2) . . . . ?
C5 C6 C7 C8 3(4) . . . . ?
Yb1 C6 C7 C8 46.0(19) . . . . ?
C5 C6 C7 Yb1 -43(2) . . . . ?
C6 C7 C8 C9 -1(3) . . . . ?
Yb1 C7 C8 C9 44(2) . . . . ?
C6 C7 C8 Yb1 -45.0(18) . . . . ?
C2 C1 C9 C8 -3(5) . . . . ?
Yb1 C1 C9 C8 -47(2) . . . . ?
C2 C1 C9 Yb1 44(3) . . . . ?
C7 C8 C9 C1 2(4) . . . . ?
Yb1 C8 C9 C1 46(2) . . . . ?
C7 C8 C9 Yb1 -44(2) . . . . ?
C18 C10 C11 C12 8(4) . . . . ?
Yb1 C10 C11 C12 -40(2) . . . . ?
C18 C10 C11 Yb1 48(2) . . . . ?
C10 C11 C12 C13 -2(4) . . . . ?
Yb1 C11 C12 C13 -43(3) . . . . ?
C10 C11 C12 Yb1 40(2) . . . . ?
C11 C12 C13 C14 -3(5) . . . . ?
Yb1 C12 C13 C14 -46(3) . . . . ?
C11 C12 C13 Yb1 43(3) . . . . ?
C12 C13 C14 C15 2(5) . . . . ?
Yb1 C13 C14 C15 -45(3) . . . . ?
C12 C13 C14 Yb1 47(3) . . . . ?
C13 C14 C15 C16 -4(5) . . . . ?
Yb1 C14 C15 C16 -49(2) . . . . ?
C13 C14 C15 Yb1 45(3) . . . . ?
C14 C15 C16 C17 8(5) . . . . ?
Yb1 C15 C16 C17 -41(3) . . . . ?
C14 C15 C16 Yb1 49(2) . . . . ?
C15 C16 C17 C18 -3(5) . . . . ?
Yb1 C16 C17 C18 -44(3) . . . . ?
C15 C16 C17 Yb1 41(3) . . . . ?
C11 C10 C18 C17 -4(4) . . . . ?
Yb1 C10 C18 C17 45(3) . . . . ?
C11 C10 C18 Yb1 -49(2) . . . . ?
C16 C17 C18 C10 -1(5) . . . . ?
Yb1 C17 C18 C10 -45(3) . . . . ?
C16 C17 C18 Yb1 44(3) . . . . ?
 
_refine_diff_density_max    2.034
_refine_diff_density_min   -1.512
_refine_diff_density_rms    0.160



# ===END

 
data_2
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C18 H18 Sm'
_chemical_formula_sum
 'C18 H18 Sm' 
_chemical_formula_weight          384.67

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'
 'Sm'  'Sm'  -0.1638   3.4418
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/n'
_space_group_name_Hall            '-P 2yn'
 
_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.
;
 
loop_
 _space_group_symop_operation_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'
 
_cell_length_a                    7.3082(4)
_cell_length_b                    9.0727(5)
_cell_length_c                    11.3296(6)
_cell_angle_alpha                 90
_cell_angle_beta                  99.968(2)
_cell_angle_gamma                 90
_cell_volume                      739.87(7)
_cell_formula_units_Z             2
_cell_measurement_temperature     150.0(1)
_cell_measurement_reflns_used     9911
_cell_measurement_theta_min        2.8930
_cell_measurement_theta_max       27.9489
 
_exptl_crystal_description        'block'
_exptl_crystal_colour             'orange'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.727          
_exptl_crystal_F_000              376
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.120
_exptl_crystal_size_mid           0.100
_exptl_crystal_size_min           0.080
_exptl_absorpt_coefficient_mu     3.952
_shelx_estimated_absorpt_T_min    0.648
_shelx_estimated_absorpt_T_max    0.743
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min    0.6699
_exptl_absorpt_correction_T_max    0.7467
_exptl_absorpt_process_details    'SADABS'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       150(2)
_diffrn_radiation_wavelength      0.71069
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   'Kappa APEX II'
_diffrn_measurement_method        'phi and omega scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             34494
_diffrn_reflns_av_unetI/netI      0.0241
_diffrn_reflns_av_R_equivalents   0.0522
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_k_max        14
_diffrn_reflns_limit_l_min        -17
_diffrn_reflns_limit_l_max        17
_diffrn_reflns_theta_min          3.613
_diffrn_reflns_theta_max          33.940
_diffrn_reflns_theta_full         25.240
_diffrn_measured_fraction_theta_max   0.999
_diffrn_measured_fraction_theta_full  0.999
_diffrn_reflns_Laue_measured_fraction_max    0.999
_diffrn_reflns_Laue_measured_fraction_full   0.999
_diffrn_reflns_point_group_measured_fraction_max   0.999
_diffrn_reflns_point_group_measured_fraction_full  0.999
_reflns_number_total              3007
_reflns_number_gt                 1906
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'Bruker APEX2'
_computing_cell_refinement        'Bruker SAINT'
_computing_data_reduction         'Bruker SAINT'
_computing_structure_solution     'SHELXT(Sheldrick,2014)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     'PLATON (Spek, 2009)'
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0374P)²+0.2370P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          3007
_refine_ls_number_parameters      169
_refine_ls_number_restraints      108
_refine_ls_R_factor_all           0.0411
_refine_ls_R_factor_gt            0.0197
_refine_ls_wR_factor_ref          0.0645
_refine_ls_wR_factor_gt           0.0537
_refine_ls_goodness_of_fit_ref    0.990
_refine_ls_restrained_S_all       1.020
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
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
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Sm1 Sm 0.0000 0.0000 0.0000 0.01849(5) Uani 1 2 d S . P . .
C1 C 0.3156(15) -0.0256(10) 0.1916(9) 0.038(2) Uani 0.5 1 d . U P A -1
H1 H 0.4132 0.0373 0.2280 0.046 Uiso 0.5 1 calc R U P A -1
C2 C 0.3709(13) -0.1026(11) 0.0988(9) 0.0315(18) Uani 0.5 1 d . U P A -1
H2 H 0.4931 -0.0748 0.0900 0.038 Uiso 0.5 1 calc R U P A -1
C3 C 0.3029(11) -0.2060(12) 0.0167(10) 0.0297(17) Uani 0.5 1 d . U P A -1
H3 H 0.3953 -0.2285 -0.0302 0.036 Uiso 0.5 1 calc R U P A -1
C4 C 0.1524(12) -0.2876(10) -0.0220(8) 0.0278(16) Uani 0.5 1 d . U P A -1
H4 H 0.1726 -0.3462 -0.0881 0.033 Uiso 0.5 1 calc R U P A -1
C5 C -0.0290(9) -0.3155(7) 0.0034(5) 0.0179(12) Uani 0.5 1 d . U P A -1
H5 H -0.0939 -0.3820 -0.0538 0.021 Uiso 0.5 1 calc R U P A -1
C6 C -0.1429(10) -0.2741(8) 0.0883(6) 0.0229(11) Uani 0.5 1 d . U P A -1
H6 H -0.2563 -0.3277 0.0746 0.027 Uiso 0.5 1 calc R U P A -1
C7 C -0.1378(9) -0.1805(9) 0.1836(7) 0.0236(12) Uani 0.5 1 d . U P A -1
H7 H -0.2481 -0.1912 0.2165 0.028 Uiso 0.5 1 calc R U P A -1
C8 C -0.0235(15) -0.0745(9) 0.2482(6) 0.0317(15) Uani 0.5 1 d . U P A -1
H8 H -0.0826 -0.0322 0.3085 0.038 Uiso 0.5 1 calc R U P A -1
C9 C 0.1590(18) -0.0096(9) 0.2508(7) 0.0372(16) Uani 0.5 1 d . U P A -1
H9 H 0.1808 0.0662 0.3094 0.045 Uiso 0.5 1 calc R U P A -1
C10 C 0.3505(12) -0.0408(12) 0.1566(9) 0.0337(18) Uani 0.5 1 d . U P A -2
H10 H 0.4658 0.0097 0.1744 0.040 Uiso 0.5 1 calc R U P A -2
C11 C 0.3557(12) -0.1383(11) 0.0664(8) 0.0287(16) Uani 0.5 1 d . U P A -2
H11 H 0.4755 -0.1345 0.0448 0.034 Uiso 0.5 1 calc R U P A -2
C12 C 0.2541(14) -0.2375(11) -0.0029(8) 0.0306(18) Uani 0.5 1 d . U P A -2
H12 H 0.3225 -0.2745 -0.0606 0.037 Uiso 0.5 1 calc R U P A -2
C13 C 0.0834(13) -0.3033(8) -0.0179(8) 0.0315(18) Uani 0.5 1 d . U P A -2
H13 H 0.0684 -0.3703 -0.0833 0.038 Uiso 0.5 1 calc R U P A -2
C14 C -0.0842(13) -0.3002(9) 0.0381(11) 0.042(2) Uani 0.5 1 d . U P A -2
H14 H -0.1745 -0.3679 -0.0002 0.051 Uiso 0.5 1 calc R U P A -2
C15 C -0.1464(11) -0.2292(11) 0.1278(11) 0.0440(19) Uani 0.5 1 d . U P A -2
H15 H -0.2648 -0.2676 0.1354 0.053 Uiso 0.5 1 calc R U P A -2
C16 C -0.0993(12) -0.1221(12) 0.2112(9) 0.0398(17) Uani 0.5 1 d . U P A -2
H16 H -0.1983 -0.1076 0.2545 0.048 Uiso 0.5 1 calc R U P A -2
C17 C 0.0477(16) -0.0252(9) 0.2550(6) 0.0358(16) Uani 0.5 1 d . U P A -2
H17 H 0.0170 0.0341 0.3179 0.043 Uiso 0.5 1 calc R U P A -2
C18 C 0.2298(15) 0.0103(9) 0.2327(7) 0.0339(15) Uani 0.5 1 d . U P A -2
H18 H 0.2837 0.0890 0.2821 0.041 Uiso 0.5 1 calc R U P A -2
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
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
Sm1 C13 2.833(8) . ?
Sm1 C14 2.841(7) . ?
Sm1 C16 2.843(7) . ?
Sm1 C15 2.846(8) . ?
Sm1 C12 2.849(9) . ?
Sm1 C17 2.859(7) . ?
Sm1 C4 2.865(8) . ?
Sm1 C11 2.867(9) . ?
Sm1 C5 2.871(6) . ?
Sm1 C18 2.872(7) . ?
Sm1 C10 2.876(9) . ?
Sm1 C3 2.878(10) . ?
Sm1 C9 2.879(7) . ?
Sm1 C1 2.890(8) . ?
Sm1 C2 2.901(10) . ?
Sm1 C8 2.926(6) . ?
Sm1 C6 2.939(7) . ?
Sm1 C7 2.958(6) . ?
C1 C2 1.379(13) . ?
C1 C9 1.431(16) . ?
C1 H1 0.9500 . ?
C2 C3 1.354(10) . ?
C2 H2 0.9500 . ?
C3 C4 1.336(10) . ?
C3 H3 0.9500 . ?
C4 C5 1.427(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.427(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.369(8) . ?
C6 H6 0.9500 . ?
C7 C8 1.395(10) . ?
C7 H7 0.9500 . ?
C8 C9 1.454(15) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.357(11) . ?
C10 C18 1.414(14) . ?
C10 H10 0.9500 . ?
C11 C12 1.332(9) . ?
C11 H11 0.9500 . ?
C12 C13 1.367(11) . ?
C12 H12 0.9500 . ?
C13 C14 1.474(18) . ?
C13 H13 0.9500 . ?
C14 C15 1.347(14) . ?
C14 H14 0.9500 . ?
C15 C16 1.358(12) . ?
C15 H15 0.9500 . ?
C16 C17 1.410(12) . ?
C16 H16 0.9500 . ?
C17 C18 1.434(14) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
 
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
C13 Sm1 C14 30.1(4) . . ?
C13 Sm1 C16 76.8(3) . . ?
C14 Sm1 C16 53.5(3) . . ?
C13 Sm1 C15 55.4(3) . . ?
C14 Sm1 C15 27.4(3) . . ?
C16 Sm1 C15 27.6(2) . . ?
C13 Sm1 C12 27.8(2) . . ?
C14 Sm1 C12 55.6(3) . . ?
C16 Sm1 C12 88.7(3) . . ?
C15 Sm1 C12 75.9(3) . . ?
C13 Sm1 C17 90.3(2) . . ?
C14 Sm1 C17 76.2(3) . . ?
C16 Sm1 C17 28.6(2) . . ?
C15 Sm1 C17 54.4(3) . . ?
C12 Sm1 C17 89.2(2) . . ?
C13 Sm1 C11 52.9(2) . . ?
C14 Sm1 C11 75.6(3) . . ?
C16 Sm1 C11 87.7(2) . . ?
C15 Sm1 C11 87.1(3) . . ?
C12 Sm1 C11 26.96(19) . . ?
C17 Sm1 C11 75.7(2) . . ?
C4 Sm1 C5 28.81(19) . . ?
C13 Sm1 C18 89.9(2) . . ?
C14 Sm1 C18 90.0(3) . . ?
C16 Sm1 C18 55.5(3) . . ?
C15 Sm1 C18 76.6(3) . . ?
C12 Sm1 C18 75.9(3) . . ?
C17 Sm1 C18 29.0(3) . . ?
C11 Sm1 C18 54.1(3) . . ?
C13 Sm1 C10 74.9(3) . . ?
C14 Sm1 C10 88.6(3) . . ?
C16 Sm1 C10 76.1(3) . . ?
C15 Sm1 C10 88.0(3) . . ?
C12 Sm1 C10 52.9(2) . . ?
C17 Sm1 C10 55.0(3) . . ?
C11 Sm1 C10 27.3(2) . . ?
C18 Sm1 C10 28.5(3) . . ?
C4 Sm1 C3 26.9(2) . . ?
C5 Sm1 C3 53.8(2) . . ?
C4 Sm1 C9 87.8(3) . . ?
C5 Sm1 C9 88.6(2) . . ?
C3 Sm1 C9 75.0(3) . . ?
C4 Sm1 C1 73.8(3) . . ?
C5 Sm1 C1 87.8(2) . . ?
C3 Sm1 C1 52.7(3) . . ?
C9 Sm1 C1 28.7(3) . . ?
C4 Sm1 C2 52.4(2) . . ?
C5 Sm1 C2 75.0(2) . . ?
C3 Sm1 C2 27.1(2) . . ?
C9 Sm1 C2 54.5(3) . . ?
C1 Sm1 C2 27.6(3) . . ?
C4 Sm1 C8 87.8(2) . . ?
C5 Sm1 C8 74.93(18) . . ?
C3 Sm1 C8 87.7(3) . . ?
C9 Sm1 C8 29.0(3) . . ?
C1 Sm1 C8 55.4(3) . . ?
C2 Sm1 C8 76.2(3) . . ?
C4 Sm1 C6 54.9(2) . . ?
C5 Sm1 C6 28.40(16) . . ?
C3 Sm1 C6 75.1(2) . . ?
C9 Sm1 C6 75.2(2) . . ?
C1 Sm1 C6 87.7(2) . . ?
C2 Sm1 C6 87.7(2) . . ?
C8 Sm1 C6 52.7(2) . . ?
C4 Sm1 C7 75.0(2) . . ?
C5 Sm1 C7 53.39(17) . . ?
C3 Sm1 C7 86.9(2) . . ?
C9 Sm1 C7 54.4(3) . . ?
C1 Sm1 C7 75.6(3) . . ?
C2 Sm1 C7 87.7(2) . . ?
C8 Sm1 C7 27.42(19) . . ?
C6 Sm1 C7 26.85(16) . . ?
C2 C1 C9 140.6(8) . . ?
C2 C1 Sm1 76.7(5) . . ?
C9 C1 Sm1 75.2(5) . . ?
C2 C1 H1 109.7 . . ?
C9 C1 H1 109.7 . . ?
Sm1 C1 H1 136.0 . . ?
C3 C2 C1 138.9(8) . . ?
C3 C2 Sm1 75.5(5) . . ?
C1 C2 Sm1 75.8(5) . . ?
C3 C2 H2 110.5 . . ?
C1 C2 H2 110.5 . . ?
Sm1 C2 H2 135.0 . . ?
C4 C3 C2 142.5(8) . . ?
C4 C3 Sm1 76.0(5) . . ?
C2 C3 Sm1 77.4(6) . . ?
C4 C3 H3 108.8 . . ?
C2 C3 H3 108.8 . . ?
Sm1 C3 H3 135.7 . . ?
C3 C4 C5 140.6(8) . . ?
C3 C4 Sm1 77.1(5) . . ?
C5 C4 Sm1 75.8(4) . . ?
C3 C4 H4 109.7 . . ?
C5 C4 H4 109.7 . . ?
Sm1 C4 H4 134.0 . . ?
C6 C5 C4 139.5(7) . . ?
C6 C5 Sm1 78.5(4) . . ?
C4 C5 Sm1 75.4(5) . . ?
C6 C5 H5 110.3 . . ?
C4 C5 H5 110.3 . . ?
Sm1 C5 H5 130.8 . . ?
C7 C6 C5 139.1(7) . . ?
C7 C6 Sm1 77.3(4) . . ?
C5 C6 Sm1 73.1(4) . . ?
C7 C6 H6 110.5 . . ?
C5 C6 H6 110.5 . . ?
Sm1 C6 H6 136.7 . . ?
C6 C7 C8 140.7(7) . . ?
C6 C7 Sm1 75.8(4) . . ?
C8 C7 Sm1 75.0(4) . . ?
C6 C7 H7 109.7 . . ?
C8 C7 H7 109.7 . . ?
Sm1 C7 H7 138.4 . . ?
C7 C8 C9 138.9(7) . . ?
C7 C8 Sm1 77.5(4) . . ?
C9 C8 Sm1 73.7(4) . . ?
C7 C8 H8 110.5 . . ?
C9 C8 H8 110.5 . . ?
Sm1 C8 H8 135.0 . . ?
C1 C9 C8 139.0(7) . . ?
C1 C9 Sm1 76.1(4) . . ?
C8 C9 Sm1 77.3(4) . . ?
C1 C9 H9 110.5 . . ?
C8 C9 H9 110.5 . . ?
Sm1 C9 H9 131.2 . . ?
C11 C10 C18 140.8(9) . . ?
C11 C10 Sm1 76.0(5) . . ?
C18 C10 Sm1 75.6(4) . . ?
C11 C10 H10 109.6 . . ?
C18 C10 H10 109.6 . . ?
Sm1 C10 H10 137.0 . . ?
C12 C11 C10 143.0(8) . . ?
C12 C11 Sm1 75.7(5) . . ?
C10 C11 Sm1 76.7(5) . . ?
C12 C11 H11 108.5 . . ?
C10 C11 H11 108.5 . . ?
Sm1 C11 H11 138.7 . . ?
C11 C12 C13 140.5(8) . . ?
C11 C12 Sm1 77.3(5) . . ?
C13 C12 Sm1 75.4(5) . . ?
C11 C12 H12 109.8 . . ?
C13 C12 H12 109.8 . . ?
Sm1 C12 H12 134.2 . . ?
C12 C13 C14 138.3(8) . . ?
C12 C13 Sm1 76.7(5) . . ?
C14 C13 Sm1 75.3(5) . . ?
C12 C13 H13 110.8 . . ?
C14 C13 H13 110.8 . . ?
Sm1 C13 H13 132.9 . . ?
C15 C14 C13 138.4(8) . . ?
C15 C14 Sm1 76.5(5) . . ?
C13 C14 Sm1 74.6(4) . . ?
C15 C14 H14 110.8 . . ?
C13 C14 H14 110.8 . . ?
Sm1 C14 H14 134.6 . . ?
C14 C15 C16 142.1(8) . . ?
C14 C15 Sm1 76.1(5) . . ?
C16 C15 Sm1 76.1(4) . . ?
C14 C15 H15 108.9 . . ?
C16 C15 H15 108.9 . . ?
Sm1 C15 H15 137.9 . . ?
C15 C16 C17 141.0(7) . . ?
C15 C16 Sm1 76.3(5) . . ?
C17 C16 Sm1 76.3(4) . . ?
C15 C16 H16 109.5 . . ?
C17 C16 H16 109.5 . . ?
Sm1 C16 H16 135.1 . . ?
C16 C17 C18 138.7(7) . . ?
C16 C17 Sm1 75.1(4) . . ?
C18 C17 Sm1 76.0(4) . . ?
C16 C17 H17 110.6 . . ?
C18 C17 H17 110.6 . . ?
Sm1 C17 H17 135.2 . . ?
C10 C18 C17 136.9(8) . . ?
C10 C18 Sm1 75.9(5) . . ?
C17 C18 Sm1 75.0(4) . . ?
C10 C18 H18 111.6 . . ?
C17 C18 H18 111.6 . . ?
Sm1 C18 H18 133.1 . . ?
 
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
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
C9 C1 C2 C3 -1(2) . . . . ?
Sm1 C1 C2 C3 -46.9(12) . . . . ?
C9 C1 C2 Sm1 45.5(11) . . . . ?
C1 C2 C3 C4 1(2) . . . . ?
Sm1 C2 C3 C4 -45.7(13) . . . . ?
C1 C2 C3 Sm1 46.9(12) . . . . ?
C2 C3 C4 C5 -2(2) . . . . ?
Sm1 C3 C4 C5 -47.6(11) . . . . ?
C2 C3 C4 Sm1 46.0(13) . . . . ?
C3 C4 C5 C6 -3.5(18) . . . . ?
Sm1 C4 C5 C6 -51.4(9) . . . . ?
C3 C4 C5 Sm1 47.9(11) . . . . ?
C4 C5 C6 C7 4.9(16) . . . . ?
Sm1 C5 C6 C7 -45.6(9) . . . . ?
C4 C5 C6 Sm1 50.5(9) . . . . ?
C5 C6 C7 C8 1.3(16) . . . . ?
Sm1 C6 C7 C8 -43.2(9) . . . . ?
C5 C6 C7 Sm1 44.5(9) . . . . ?
C6 C7 C8 C9 -2.9(17) . . . . ?
Sm1 C7 C8 C9 -46.3(9) . . . . ?
C6 C7 C8 Sm1 43.4(9) . . . . ?
C2 C1 C9 C8 4.9(19) . . . . ?
Sm1 C1 C9 C8 50.9(10) . . . . ?
C2 C1 C9 Sm1 -45.9(11) . . . . ?
C7 C8 C9 C1 -3.1(17) . . . . ?
Sm1 C8 C9 C1 -50.5(10) . . . . ?
C7 C8 C9 Sm1 47.4(9) . . . . ?
C18 C10 C11 C12 2(2) . . . . ?
Sm1 C10 C11 C12 -42.7(13) . . . . ?
C18 C10 C11 Sm1 44.6(11) . . . . ?
C10 C11 C12 C13 -4(2) . . . . ?
Sm1 C11 C12 C13 -47.3(11) . . . . ?
C10 C11 C12 Sm1 42.9(13) . . . . ?
C11 C12 C13 C14 -1.0(19) . . . . ?
Sm1 C12 C13 C14 -48.8(9) . . . . ?
C11 C12 C13 Sm1 47.8(12) . . . . ?
C12 C13 C14 C15 1.7(17) . . . . ?
Sm1 C13 C14 C15 -47.6(10) . . . . ?
C12 C13 C14 Sm1 49.2(10) . . . . ?
C13 C14 C15 C16 3.4(19) . . . . ?
Sm1 C14 C15 C16 -43.7(11) . . . . ?
C13 C14 C15 Sm1 47.1(10) . . . . ?
C14 C15 C16 C17 -2.9(19) . . . . ?
Sm1 C15 C16 C17 -46.6(10) . . . . ?
C14 C15 C16 Sm1 43.7(11) . . . . ?
C15 C16 C17 C18 -0.3(17) . . . . ?
Sm1 C16 C17 C18 -46.9(9) . . . . ?
C15 C16 C17 Sm1 46.6(10) . . . . ?
C11 C10 C18 C17 4.1(19) . . . . ?
Sm1 C10 C18 C17 48.9(9) . . . . ?
C11 C10 C18 Sm1 -44.7(12) . . . . ?
C16 C17 C18 C10 -2.5(16) . . . . ?
Sm1 C17 C18 C10 -49.1(9) . . . . ?
C16 C17 C18 Sm1 46.6(9) . . . . ?
 
_refine_diff_density_max    0.726
_refine_diff_density_min   -0.946
_refine_diff_density_rms    0.102



# ===END

 
data_3
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C25 H41 O4 Yb, C9 H9'
_chemical_formula_sum
 'C34 H50 O4 Yb' 
_chemical_formula_weight          695.78

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'
 
_space_group_crystal_system       orthorhombic
_space_group_IT_number            31
_space_group_name_H-M_alt         'P m n 21'
_space_group_name_Hall            'P 2ac -2'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 '-x, y, z'
 'x+1/2, -y, z+1/2'
 
_cell_length_a                    13.5501(4)
_cell_length_b                    12.9804(4)
_cell_length_c                    8.9048(3)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      1566.23(9)
_cell_formula_units_Z             2
_cell_measurement_temperature     150.0(1)
_cell_measurement_reflns_used     8331
_cell_measurement_theta_min        2.7371
_cell_measurement_theta_max       27.5268
 
_exptl_crystal_description        'block'
_exptl_crystal_colour             'orange'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.475          
_exptl_crystal_F_000              712
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.220
_exptl_crystal_size_mid           0.160
_exptl_crystal_size_min           0.080
_exptl_absorpt_coefficient_mu     3.020
_shelx_estimated_absorpt_T_min    0.556
_shelx_estimated_absorpt_T_max    0.794
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min    0.6300
_exptl_absorpt_correction_T_max    0.7456
_exptl_absorpt_process_details    'SADABS'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       150(2)
_diffrn_radiation_wavelength      0.71069
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   'Kappa APEX II'
_diffrn_measurement_method        'phi and omega scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             10729
_diffrn_reflns_av_unetI/netI      0.0361
_diffrn_reflns_av_R_equivalents   0.0314
_diffrn_reflns_limit_h_min        -13
_diffrn_reflns_limit_h_max        17
_diffrn_reflns_limit_k_min        -16
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -11
_diffrn_reflns_limit_l_max        11
_diffrn_reflns_theta_min          3.139
_diffrn_reflns_theta_max          27.534
_diffrn_reflns_theta_full         25.240
_diffrn_measured_fraction_theta_max   0.994
_diffrn_measured_fraction_theta_full  0.997
_diffrn_reflns_Laue_measured_fraction_max    0.994
_diffrn_reflns_Laue_measured_fraction_full   0.997
_diffrn_reflns_point_group_measured_fraction_max   0.996
_diffrn_reflns_point_group_measured_fraction_full  0.998
_reflns_number_total              3733
_reflns_number_gt                 3642
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.884
_reflns_Friedel_fraction_max      0.998
_reflns_Friedel_fraction_full     0.999
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'Bruker APEX2'
_computing_cell_refinement        'Bruker SAINT'
_computing_data_reduction         'Bruker SAINT'
_computing_structure_solution     'SHELXT(Sheldrick,2014)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     'PLATON (Spek, 2009)'
_computing_publication_material   ?
_refine_special_details
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0246P)²+0.0344P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack    -0.023(15)
_chemical_absolute_configuration  ?
_refine_ls_number_reflns          3733
_refine_ls_number_parameters      191
_refine_ls_number_restraints      21
_refine_ls_R_factor_all           0.0209
_refine_ls_R_factor_gt            0.0203
_refine_ls_wR_factor_ref          0.0518
_refine_ls_wR_factor_gt           0.0516
_refine_ls_goodness_of_fit_ref    1.062
_refine_ls_restrained_S_all       1.070
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
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
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Yb1 Yb 0.0000 0.32982(2) 0.45305(6) 0.02165(7) Uani 1 2 d S T P B .
O1 O 0.1459(2) 0.2861(2) 0.3080(3) 0.0281(6) Uani 1 1 d . . . . .
O2 O 0.0000 0.1438(3) 0.4515(13) 0.0300(7) Uani 1 2 d S T P B .
O3 O 0.0000 0.4551(3) 0.2419(5) 0.0284(9) Uani 1 2 d S T P B .
C1 C 0.1340(4) 0.2380(5) 0.1610(5) 0.0419(12) Uani 1 1 d . . . . .
H1A H 0.0875 0.2779 0.0979 0.050 Uiso 1 1 calc R U . . .
H1B H 0.1091 0.1667 0.1711 0.050 Uiso 1 1 calc R U . . .
C2 C 0.2367(4) 0.2389(6) 0.0933(7) 0.0593(15) Uani 1 1 d . . . . .
H2A H 0.2460 0.1801 0.0238 0.071 Uiso 1 1 calc R U . . .
H2B H 0.2493 0.3039 0.0384 0.071 Uiso 1 1 calc R U . . .
C3 C 0.3024(4) 0.2296(5) 0.2262(7) 0.0529(14) Uani 1 1 d . . . . .
H3A H 0.3693 0.2564 0.2041 0.064 Uiso 1 1 calc R U . . .
H3B H 0.3077 0.1571 0.2598 0.064 Uiso 1 1 calc R U . . .
C4 C 0.2508(3) 0.2954(4) 0.3429(6) 0.0355(9) Uani 1 1 d . . . . .
H4A H 0.2647 0.2697 0.4454 0.043 Uiso 1 1 calc R U . . .
H4B H 0.2725 0.3680 0.3357 0.043 Uiso 1 1 calc R U . . .
C5 C 0.0845(3) 0.0761(3) 0.4652(10) 0.0434(11) Uani 1 1 d . . . . .
H5A H 0.1429 0.1149 0.5008 0.052 Uiso 1 1 calc R U . B .
H5B H 0.1004 0.0443 0.3670 0.052 Uiso 1 1 calc R U . . .
C6 C 0.0561(5) -0.0041(4) 0.5758(6) 0.0485(13) Uani 1 1 d . . . . .
H6A H 0.0820 0.0130 0.6768 0.058 Uiso 1 1 calc R U . . .
H6B H 0.0820 -0.0723 0.5455 0.058 Uiso 1 1 calc R U . . .
C7 C -0.0844(4) 0.5115(4) 0.1920(6) 0.0425(11) Uani 1 1 d . . . . .
H7A H -0.1013 0.5664 0.2648 0.051 Uiso 1 1 calc R U . B .
H7B H -0.1420 0.4652 0.1807 0.051 Uiso 1 1 calc R U . . .
C8 C -0.0563(4) 0.5575(4) 0.0430(5) 0.0421(11) Uani 1 1 d . . . . .
H8A H -0.0823 0.6285 0.0334 0.050 Uiso 1 1 calc R U . . .
H8B H -0.0823 0.5153 -0.0408 0.050 Uiso 1 1 calc R U . . .
C9 C 0.0491(6) 0.5171(5) 0.5946(9) 0.081(3) Uani 1 1 d . . . . .
H9 H 0.0673 0.5842 0.5621 0.098 Uiso 1 1 calc R U . . .
C10 C 0.1358(5) 0.4673(5) 0.6187(7) 0.0565(16) Uani 1 1 d . . . . .
H10 H 0.1917 0.5046 0.5845 0.068 Uiso 1 1 calc R U . . .
C11 C 0.1592(4) 0.3740(5) 0.6824(6) 0.0509(14) Uani 1 1 d . . . . .
H11 H 0.2278 0.3592 0.6855 0.061 Uiso 1 1 calc R U . . .
C12 C 0.0991(3) 0.2975(5) 0.7432(6) 0.0462(11) Uani 1 1 d D U . . .
H12 H 0.1377 0.2429 0.7831 0.055 Uiso 1 1 calc R U . A 1
C13A C 0.0000 0.2781(12) 0.7624(15) 0.042(2) Uani 0.5 2 d DS TU P B 1
H13A H 0.0000 0.2175 0.8222 0.050 Uiso 0.5 2 calc R U P B 1
C13B C 0.0000 0.3304(11) 0.7670(18) 0.045(2) Uani 0.5 2 d DS TU P B 2
H13B H 0.0000 0.3959 0.8145 0.053 Uiso 0.5 2 calc R U P B 2
C14 C 0.3693(5) 0.0545(5) 0.5711(8) 0.0671(19) Uani 1 1 d . . . . .
H14 H 0.3097 0.0281 0.5301 0.081 Uiso 1 1 calc R U . . .
C15 C 0.3480(5) 0.1288(6) 0.6749(9) 0.0661(18) Uani 1 1 d . . . . .
H15 H 0.2790 0.1385 0.6879 0.079 Uiso 1 1 calc R U . . .
C16 C 0.4033(7) 0.1931(6) 0.7654(10) 0.073(2) Uani 1 1 d . . . . .
H16 H 0.3597 0.2353 0.8219 0.087 Uiso 1 1 calc R U . . .
C17 C 0.5000 0.2184(8) 0.8040(12) 0.088(4) Uani 1 2 d S T P . .
H17 H 0.5000 0.2691 0.8810 0.106 Uiso 1 2 calc R U P . .
C18 C 0.4497(5) 0.0048(5) 0.5054(6) 0.0592(16) Uani 1 1 d . . . . .
H18 H 0.4265 -0.0465 0.4379 0.071 Uiso 1 1 calc R U . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
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 O2 2.415(3) . ?
Yb1 O1 2.429(3) 3 ?
Yb1 O1 2.429(3) . ?
Yb1 O3 2.485(4) . ?
Yb1 C13B 2.796(16) . ?
Yb1 C9 2.818(6) . ?
Yb1 C9 2.818(6) 3 ?
Yb1 C13A 2.836(14) . ?
Yb1 C12 2.942(5) 3 ?
Yb1 C12 2.942(5) . ?
Yb1 C10 2.957(5) 3 ?
Yb1 C10 2.957(5) . ?
O1 C1 1.459(5) . ?
O1 C4 1.460(5) . ?
O2 C5 1.448(5) 3 ?
O2 C5 1.448(5) . ?
O3 C7 1.429(5) 3 ?
O3 C7 1.429(5) . ?
C1 C2 1.517(8) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.486(9) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.516(7) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.484(8) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C6 1.520(12) 3 ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.503(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C8 1.527(10) 3 ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C9 1.330(17) 3 ?
C9 C10 1.358(10) . ?
C9 H9 0.9500 . ?
C10 C11 1.375(9) . ?
C10 H10 0.9500 . ?
C11 C12 1.393(9) . ?
C11 H11 0.9500 . ?
C12 C13A 1.377(5) . ?
C12 C13B 1.425(5) . ?
C12 H12 0.9500 . ?
C13A C12 1.377(5) 3 ?
C13A H13A 0.9500 . ?
C13B C12 1.425(5) 3 ?
C13B H13B 0.9500 . ?
C14 C15 1.367(11) . ?
C14 C18 1.395(10) . ?
C14 H14 0.9500 . ?
C15 C16 1.381(13) . ?
C15 H15 0.9500 . ?
C16 C17 1.393(11) . ?
C16 H16 0.9500 . ?
C17 C16 1.393(11) 3_655 ?
C17 H17 0.9500 . ?
C18 C18 1.364(15) 3_655 ?
C18 H18 0.9500 . ?
 
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 Yb1 O1 76.31(17) . 3 ?
O2 Yb1 O1 76.31(17) . . ?
O1 Yb1 O1 108.97(14) 3 . ?
O2 Yb1 O3 130.5(3) . . ?
O1 Yb1 O3 75.55(9) 3 . ?
O1 Yb1 O3 75.55(9) . . ?
O2 Yb1 C13B 90.5(4) . . ?
O1 Yb1 C13B 122.17(11) 3 . ?
O1 Yb1 C13B 122.17(11) . . ?
O3 Yb1 C13B 139.0(3) . . ?
O2 Yb1 C9 149.9(3) . . ?
O1 Yb1 C9 129.16(16) 3 . ?
O1 Yb1 C9 104.3(2) . . ?
O3 Yb1 C9 76.9(2) . . ?
C13B Yb1 C9 63.3(3) . . ?
O2 Yb1 C9 149.9(3) . 3 ?
O1 Yb1 C9 104.3(2) 3 3 ?
O1 Yb1 C9 129.16(16) . 3 ?
O3 Yb1 C9 76.9(2) . 3 ?
C13B Yb1 C9 63.3(3) . 3 ?
C9 Yb1 C9 27.3(3) . 3 ?
O2 Yb1 C13A 76.6(4) . . ?
O1 Yb1 C13A 117.48(14) 3 . ?
O1 Yb1 C13A 117.48(14) . . ?
O3 Yb1 C13A 152.9(3) . . ?
C9 Yb1 C13A 76.7(4) . . ?
C9 Yb1 C13A 76.7(4) 3 . ?
O2 Yb1 C12 82.1(3) . 3 ?
O1 Yb1 C12 93.58(11) 3 3 ?
O1 Yb1 C12 143.65(12) . 3 ?
O3 Yb1 C12 139.25(14) . 3 ?
C13B Yb1 C12 28.60(10) . 3 ?
C9 Yb1 C12 80.7(2) . 3 ?
C9 Yb1 C12 67.8(2) 3 3 ?
C13A Yb1 C12 27.49(9) . 3 ?
O2 Yb1 C12 82.1(3) . . ?
O1 Yb1 C12 143.65(12) 3 . ?
O1 Yb1 C12 93.58(11) . . ?
O3 Yb1 C12 139.25(14) . . ?
C13B Yb1 C12 28.60(10) . . ?
C9 Yb1 C12 67.8(2) . . ?
C9 Yb1 C12 80.7(2) 3 . ?
C13A Yb1 C12 27.49(9) . . ?
C12 Yb1 C12 54.31(16) 3 . ?
O2 Yb1 C10 127.3(2) . 3 ?
O1 Yb1 C10 84.25(14) 3 3 ?
O1 Yb1 C10 155.87(15) . 3 ?
O3 Yb1 C10 89.00(16) . 3 ?
C13B Yb1 C10 60.0(2) . 3 ?
C9 Yb1 C10 53.4(2) . 3 ?
C9 Yb1 C10 27.06(19) 3 3 ?
C13A Yb1 C10 70.0(3) . 3 ?
C12 Yb1 C10 50.50(18) 3 3 ?
C12 Yb1 C10 86.09(16) . 3 ?
O2 Yb1 C10 127.3(2) . . ?
O1 Yb1 C10 155.87(15) 3 . ?
O1 Yb1 C10 84.25(14) . . ?
O3 Yb1 C10 89.00(16) . . ?
C13B Yb1 C10 60.0(2) . . ?
C9 Yb1 C10 27.06(19) . . ?
C9 Yb1 C10 53.4(2) 3 . ?
C13A Yb1 C10 70.0(3) . . ?
C12 Yb1 C10 86.09(16) 3 . ?
C12 Yb1 C10 50.50(18) . . ?
C10 Yb1 C10 76.9(2) 3 . ?
C1 O1 C4 109.5(3) . . ?
C1 O1 Yb1 119.2(3) . . ?
C4 O1 Yb1 131.3(3) . . ?
C5 O2 C5 104.5(5) 3 . ?
C5 O2 Yb1 127.3(2) 3 . ?
C5 O2 Yb1 127.3(2) . . ?
C7 O3 C7 106.3(5) 3 . ?
C7 O3 Yb1 124.8(2) 3 . ?
C7 O3 Yb1 124.8(2) . . ?
O1 C1 C2 104.6(4) . . ?
O1 C1 H1A 110.8 . . ?
C2 C1 H1A 110.8 . . ?
O1 C1 H1B 110.8 . . ?
C2 C1 H1B 110.8 . . ?
H1A C1 H1B 108.9 . . ?
C3 C2 C1 103.4(5) . . ?
C3 C2 H2A 111.1 . . ?
C1 C2 H2A 111.1 . . ?
C3 C2 H2B 111.1 . . ?
C1 C2 H2B 111.1 . . ?
H2A C2 H2B 109.0 . . ?
C2 C3 C4 102.9(4) . . ?
C2 C3 H3A 111.2 . . ?
C4 C3 H3A 111.2 . . ?
C2 C3 H3B 111.2 . . ?
C4 C3 H3B 111.2 . . ?
H3A C3 H3B 109.1 . . ?
O1 C4 C3 104.9(4) . . ?
O1 C4 H4A 110.8 . . ?
C3 C4 H4A 110.8 . . ?
O1 C4 H4B 110.8 . . ?
C3 C4 H4B 110.8 . . ?
H4A C4 H4B 108.8 . . ?
O2 C5 C6 106.1(6) . . ?
O2 C5 H5A 110.5 . . ?
C6 C5 H5A 110.5 . . ?
O2 C5 H5B 110.5 . . ?
C6 C5 H5B 110.5 . . ?
H5A C5 H5B 108.7 . . ?
C5 C6 C6 105.0(3) . 3 ?
C5 C6 H6A 110.7 . . ?
C6 C6 H6A 110.7 3 . ?
C5 C6 H6B 110.7 . . ?
C6 C6 H6B 110.7 3 . ?
H6A C6 H6B 108.8 . . ?
O3 C7 C8 106.0(4) . . ?
O3 C7 H7A 110.5 . . ?
C8 C7 H7A 110.5 . . ?
O3 C7 H7B 110.5 . . ?
C8 C7 H7B 110.5 . . ?
H7A C7 H7B 108.7 . . ?
C7 C8 C8 104.7(3) . 3 ?
C7 C8 H8A 110.8 . . ?
C8 C8 H8A 110.8 3 . ?
C7 C8 H8B 110.8 . . ?
C8 C8 H8B 110.8 3 . ?
H8A C8 H8B 108.9 . . ?
C9 C9 C10 149.9(5) 3 . ?
C9 C9 Yb1 76.35(17) 3 . ?
C10 C9 Yb1 82.2(3) . . ?
C9 C9 H9 105.0 3 . ?
C10 C9 H9 105.0 . . ?
Yb1 C9 H9 135.7 . . ?
C9 C10 C11 133.2(7) . . ?
C9 C10 Yb1 70.7(3) . . ?
C11 C10 Yb1 79.5(3) . . ?
C9 C10 H10 113.4 . . ?
C11 C10 H10 113.4 . . ?
Yb1 C10 H10 130.1 . . ?
C10 C11 C12 130.8(5) . . ?
C10 C11 Yb1 74.0(3) . . ?
C12 C11 Yb1 73.2(3) . . ?
C10 C11 H11 114.6 . . ?
C12 C11 H11 114.6 . . ?
Yb1 C11 H11 132.8 . . ?
C13A C12 C11 138.5(8) . . ?
C11 C12 C13B 113.3(7) . . ?
C13A C12 Yb1 71.9(6) . . ?
C11 C12 Yb1 79.9(3) . . ?
C13B C12 Yb1 70.0(7) . . ?
C13A C12 H12 110.8 . . ?
C11 C12 H12 110.8 . . ?
Yb1 C12 H12 133.3 . . ?
C12 C13A C12 154.4(13) 3 . ?
C12 C13A Yb1 80.6(6) 3 . ?
C12 C13A Yb1 80.6(6) . . ?
C12 C13A H13A 102.8 3 . ?
C12 C13A H13A 102.8 . . ?
Yb1 C13A H13A 137.8 . . ?
C12 C13B C12 141.0(10) 3 . ?
C12 C13B Yb1 81.4(7) 3 . ?
C12 C13B Yb1 81.4(7) . . ?
C12 C13B H13B 109.5 3 . ?
C12 C13B H13B 109.5 . . ?
Yb1 C13B H13B 116.6 . . ?
C15 C14 C18 140.8(7) . . ?
C15 C14 H14 109.6 . . ?
C18 C14 H14 109.6 . . ?
C14 C15 C16 134.9(7) . . ?
C14 C15 H15 112.5 . . ?
C16 C15 H15 112.5 . . ?
C15 C16 C17 142.8(8) . . ?
C15 C16 H16 108.6 . . ?
C17 C16 H16 108.6 . . ?
C16 C17 C16 140.1(11) 3_655 . ?
C16 C17 H17 109.9 3_655 . ?
C16 C17 H17 109.9 . . ?
C18 C18 C14 141.3(4) 3_655 . ?
C18 C18 H18 109.3 3_655 . ?
C14 C18 H18 109.3 . . ?
 
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
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
C4 O1 C1 C2 -11.6(6) . . . . ?
Yb1 O1 C1 C2 170.6(3) . . . . ?
O1 C1 C2 C3 31.2(6) . . . . ?
C1 C2 C3 C4 -38.3(6) . . . . ?
C1 O1 C4 C3 -12.1(5) . . . . ?
Yb1 O1 C4 C3 165.3(3) . . . . ?
C2 C3 C4 O1 31.4(6) . . . . ?
C5 O2 C5 C6 -35.7(11) 3 . . . ?
Yb1 O2 C5 C6 133.9(7) . . . . ?
O2 C5 C6 C6 21.7(6) . . . 3 ?
C7 O3 C7 C8 34.8(7) 3 . . . ?
Yb1 O3 C7 C8 -167.2(3) . . . . ?
O3 C7 C8 C8 -20.7(4) . . . 3 ?
C9 C9 C10 C11 -9.0(12) 3 . . . ?
Yb1 C9 C10 C11 -53.7(7) . . . . ?
C9 C9 C10 Yb1 44.7(6) 3 . . . ?
C9 C10 C11 C12 0.9(11) . . . . ?
Yb1 C10 C11 C12 -49.8(6) . . . . ?
C9 C10 C11 Yb1 50.7(6) . . . . ?
C10 C11 C12 C13A 2.7(13) . . . . ?
Yb1 C11 C12 C13A -47.4(10) . . . . ?
C10 C11 C12 C13B -12.8(10) . . . . ?
Yb1 C11 C12 C13B -62.9(7) . . . . ?
C10 C11 C12 Yb1 50.1(6) . . . . ?
C11 C12 C13A C12 7(3) . . . 3 ?
Yb1 C12 C13A C12 -43(3) . . . 3 ?
C11 C12 C13A Yb1 49.6(10) . . . . ?
C11 C12 C13B C12 133.6(19) . . . 3 ?
Yb1 C12 C13B C12 65(2) . . . 3 ?
C11 C12 C13B Yb1 68.8(5) . . . . ?
C18 C14 C15 C16 1.4(14) . . . . ?
C14 C15 C16 C17 -1.0(17) . . . . ?
C15 C16 C17 C16 3(2) . . . 3_655 ?
C15 C14 C18 C18 -2.6(12) . . . 3_655 ?
 
_refine_diff_density_max    0.965
_refine_diff_density_min   -0.375
_refine_diff_density_rms    0.073



# ===END
 
data_4
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C14 H21 N7 Yb, 2(C9 H9)'
_chemical_formula_sum
 'C32 H39 N7 Yb' 
_chemical_formula_weight          694.74

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'
 'N'  'N'   0.0061   0.0033
 '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'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/c'
_space_group_name_Hall            '-P 2ybc'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    21.525(3)
_cell_length_b                    22.637(3)
_cell_length_c                    14.4941(19)
_cell_angle_alpha                 90
_cell_angle_beta                  106.479(4)
_cell_angle_gamma                 90
_cell_volume                      6772.3(16)
_cell_formula_units_Z             8
_cell_measurement_temperature     150.0(1)
_cell_measurement_reflns_used     9883
_cell_measurement_theta_min        2.2826
_cell_measurement_theta_max       25.1988
 
_exptl_crystal_description        'block'
_exptl_crystal_colour             'orange'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.363          
_exptl_crystal_F_000              2800
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.180
_exptl_crystal_size_mid           0.120
_exptl_crystal_size_min           0.080
_exptl_absorpt_coefficient_mu     2.791
_shelx_estimated_absorpt_T_min    0.633
_shelx_estimated_absorpt_T_max    0.808
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min    0.6284
_exptl_absorpt_correction_T_max    0.7382
_exptl_absorpt_process_details    'SADABS'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       150(2)
_diffrn_radiation_wavelength      0.71069
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   'Kappa APEX II'
_diffrn_measurement_method        'phi and omega scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             133810
_diffrn_reflns_av_unetI/netI      0.0642
_diffrn_reflns_av_R_equivalents   0.1111
_diffrn_reflns_limit_h_min        -28
_diffrn_reflns_limit_h_max        27
_diffrn_reflns_limit_k_min        -29
_diffrn_reflns_limit_k_max        29
_diffrn_reflns_limit_l_min        -18
_diffrn_reflns_limit_l_max        18
_diffrn_reflns_theta_min          0.986
_diffrn_reflns_theta_max          27.608
_diffrn_reflns_theta_full         25.240
_diffrn_measured_fraction_theta_max   0.995
_diffrn_measured_fraction_theta_full  0.998
_diffrn_reflns_Laue_measured_fraction_max    0.995
_diffrn_reflns_Laue_measured_fraction_full   0.998
_diffrn_reflns_point_group_measured_fraction_max   0.995
_diffrn_reflns_point_group_measured_fraction_full  0.998
_reflns_number_total              15624
_reflns_number_gt                 12938
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'Bruker APEX2'
_computing_cell_refinement        'Bruker SAINT'
_computing_data_reduction         'Bruker SAINT'
_computing_structure_solution     'SHELXT(Sheldrick,2014)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     'PLATON (Spek, 2009)'
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0414P)²+152.7528P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          15624
_refine_ls_number_parameters      735
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0938
_refine_ls_R_factor_gt            0.0786
_refine_ls_wR_factor_ref          0.2000
_refine_ls_wR_factor_gt           0.1925
_refine_ls_goodness_of_fit_ref    1.170
_refine_ls_restrained_S_all       1.170
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
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
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Yb1 Yb 0.12136(2) 0.58000(2) 0.18655(3) 0.02323(11) Uani 1 1 d . . . . .
N1 N 0.1087(5) 0.5120(5) 0.0407(7) 0.042(2) Uani 1 1 d . . . . .
N2 N 0.1194(5) 0.6527(4) 0.0509(6) 0.035(2) Uani 1 1 d . . . . .
N3 N 0.0390(5) 0.6566(4) 0.1947(8) 0.041(2) Uani 1 1 d . . . . .
N4 N 0.2107(5) 0.6511(4) 0.2601(7) 0.039(2) Uani 1 1 d . . . . .
N5 N 0.1413(5) 0.5716(5) 0.3642(6) 0.041(2) Uani 1 1 d . . . . .
N6 N 0.0353(5) 0.5064(4) 0.1947(7) 0.034(2) Uani 1 1 d . . . . .
N7 N 0.2163(5) 0.5090(4) 0.2259(7) 0.039(2) Uani 1 1 d . . . . .
C1 C 0.1131(6) 0.4730(5) -0.0061(7) 0.032(2) Uani 1 1 d . . . . .
C2 C 0.1199(6) 0.4231(5) -0.0647(9) 0.037(3) Uani 1 1 d . . . . .
H2A H 0.1654 0.4190 -0.0638 0.056 Uiso 1 1 calc R U . . .
H2B H 0.0932 0.4294 -0.1310 0.056 Uiso 1 1 calc R U . . .
H2C H 0.1058 0.3870 -0.0390 0.056 Uiso 1 1 calc R U . . .
C3 C 0.1216(5) 0.6889(5) 0.0000(7) 0.028(2) Uani 1 1 d . . . . .
C4 C 0.1236(6) 0.7366(6) -0.0668(8) 0.039(3) Uani 1 1 d . . . . .
H4A H 0.1302 0.7200 -0.1258 0.059 Uiso 1 1 calc R U . . .
H4B H 0.1594 0.7635 -0.0370 0.059 Uiso 1 1 calc R U . . .
H4C H 0.0827 0.7585 -0.0826 0.059 Uiso 1 1 calc R U . . .
C5 C 0.0072(5) 0.6976(5) 0.1935(7) 0.030(2) Uani 1 1 d . . . . .
C6 C -0.0315(6) 0.7508(5) 0.1901(9) 0.039(3) Uani 1 1 d . . . . .
H6A H -0.0118 0.7836 0.1642 0.058 Uiso 1 1 calc R U . . .
H6B H -0.0331 0.7607 0.2552 0.058 Uiso 1 1 calc R U . . .
H6C H -0.0755 0.7439 0.1487 0.058 Uiso 1 1 calc R U . . .
C7 C 0.2510(5) 0.6822(4) 0.3007(7) 0.027(2) Uani 1 1 d . . . . .
C8 C 0.3015(5) 0.7220(5) 0.3542(7) 0.032(2) Uani 1 1 d . . . . .
H8A H 0.2850 0.7455 0.3990 0.048 Uiso 1 1 calc R U . . .
H8B H 0.3145 0.7484 0.3093 0.048 Uiso 1 1 calc R U . . .
H8C H 0.3391 0.6989 0.3904 0.048 Uiso 1 1 calc R U . . .
C9 C 0.1670(5) 0.5737(5) 0.4454(7) 0.031(2) Uani 1 1 d . . . . .
C10 C 0.2014(5) 0.5724(5) 0.5474(8) 0.035(2) Uani 1 1 d . . . . .
H10A H 0.1888 0.5371 0.5767 0.053 Uiso 1 1 calc R U . . .
H10B H 0.1904 0.6077 0.5786 0.053 Uiso 1 1 calc R U . . .
H10C H 0.2482 0.5716 0.5556 0.053 Uiso 1 1 calc R U . . .
C11 C 0.0015(5) 0.4668(4) 0.1929(7) 0.026(2) Uani 1 1 d . . . . .
C12 C -0.0400(5) 0.4159(5) 0.1882(8) 0.029(2) Uani 1 1 d . . . . .
H12A H -0.0382 0.3908 0.1339 0.044 Uiso 1 1 calc R U . . .
H12B H -0.0847 0.4291 0.1794 0.044 Uiso 1 1 calc R U . . .
H12C H -0.0253 0.3933 0.2481 0.044 Uiso 1 1 calc R U . . .
C13 C 0.2530(5) 0.4723(5) 0.2294(8) 0.031(2) Uani 1 1 d . . . . .
C14 C 0.2990(6) 0.4246(5) 0.2349(9) 0.036(3) Uani 1 1 d . . . . .
H14A H 0.2989 0.3986 0.2889 0.055 Uiso 1 1 calc R U . . .
H14B H 0.3425 0.4411 0.2446 0.055 Uiso 1 1 calc R U . . .
H14C H 0.2867 0.4020 0.1748 0.055 Uiso 1 1 calc R U . . .
Yb2 Yb 0.36367(2) 0.09941(2) 0.10788(3) 0.02083(11) Uani 1 1 d . . . . .
N8 N 0.3997(6) 0.0265(5) 0.0018(8) 0.052(3) Uani 1 1 d . . . . .
N9 N 0.3672(4) 0.1614(4) -0.0352(6) 0.0287(19) Uani 1 1 d . . . . .
N10 N 0.2494(5) 0.0751(4) 0.0106(7) 0.039(2) Uani 1 1 d . . . . .
N11 N 0.3001(5) 0.1896(4) 0.1173(7) 0.039(2) Uani 1 1 d . . . . .
N12 N 0.4735(5) 0.1460(5) 0.1607(7) 0.039(2) Uani 1 1 d . . . . .
N13 N 0.3957(5) 0.1093(5) 0.2902(7) 0.043(2) Uani 1 1 d . . . . .
N14 N 0.3525(5) 0.0014(4) 0.1810(7) 0.038(2) Uani 1 1 d . . . . .
C15 C 0.3998(8) -0.0096(6) -0.0491(10) 0.052(4) Uani 1 1 d . . . . .
C16 C 0.3976(11) -0.0583(7) -0.1181(12) 0.087(7) Uani 1 1 d . . . . .
H16A H 0.3563 -0.0793 -0.1299 0.131 Uiso 1 1 calc R U . . .
H16B H 0.4334 -0.0857 -0.0913 0.131 Uiso 1 1 calc R U . . .
H16C H 0.4017 -0.0420 -0.1788 0.131 Uiso 1 1 calc R U . . .
C17 C 0.3715(5) 0.1946(5) -0.0923(7) 0.025(2) Uani 1 1 d . . . . .
C18 C 0.3758(5) 0.2370(5) -0.1652(8) 0.037(3) Uani 1 1 d . . . . .
H18A H 0.3344 0.2578 -0.1887 0.055 Uiso 1 1 calc R U . . .
H18B H 0.3856 0.2163 -0.2188 0.055 Uiso 1 1 calc R U . . .
H18C H 0.4103 0.2655 -0.1373 0.055 Uiso 1 1 calc R U . . .
C19 C 0.1943(5) 0.0761(5) -0.0155(8) 0.032(2) Uani 1 1 d . . . . .
C20 C 0.1247(5) 0.0768(6) -0.0471(9) 0.041(3) Uani 1 1 d . . . . .
H20A H 0.1092 0.1168 -0.0406 0.061 Uiso 1 1 calc R U . . .
H20B H 0.1078 0.0495 -0.0076 0.061 Uiso 1 1 calc R U . . .
H20C H 0.1097 0.0645 -0.1146 0.061 Uiso 1 1 calc R U . . .
C21 C 0.2638(5) 0.2269(5) 0.1043(7) 0.027(2) Uani 1 1 d . . . . .
C22 C 0.2168(6) 0.2744(5) 0.0869(8) 0.036(2) Uani 1 1 d . . . . .
H22A H 0.2309 0.3063 0.0517 0.054 Uiso 1 1 calc R U . . .
H22B H 0.2132 0.2896 0.1485 0.054 Uiso 1 1 calc R U . . .
H22C H 0.1746 0.2596 0.0488 0.054 Uiso 1 1 calc R U . . .
C23 C 0.5096(5) 0.1809(5) 0.1991(7) 0.028(2) Uani 1 1 d . . . . .
C24 C 0.5551(5) 0.2254(5) 0.2491(8) 0.034(2) Uani 1 1 d . . . . .
H24A H 0.5667 0.2510 0.2021 0.051 Uiso 1 1 calc R U . . .
H24B H 0.5941 0.2061 0.2895 0.051 Uiso 1 1 calc R U . . .
H24C H 0.5352 0.2491 0.2897 0.051 Uiso 1 1 calc R U . . .
C25 C 0.4235(5) 0.0943(4) 0.3650(7) 0.025(2) Uani 1 1 d . . . . .
C26 C 0.4589(5) 0.0724(5) 0.4590(7) 0.031(2) Uani 1 1 d . . . . .
H26A H 0.5035 0.0631 0.4595 0.046 Uiso 1 1 calc R U . . .
H26B H 0.4378 0.0367 0.4737 0.046 Uiso 1 1 calc R U . . .
H26C H 0.4595 0.1027 0.5076 0.046 Uiso 1 1 calc R U . . .
C27 C 0.3612(5) -0.0341(5) 0.2386(7) 0.029(2) Uani 1 1 d . . . . .
C28 C 0.3735(6) -0.0767(5) 0.3166(8) 0.038(3) Uani 1 1 d . . . . .
H28A H 0.4164 -0.0943 0.3260 0.058 Uiso 1 1 calc R U . . .
H28B H 0.3404 -0.1078 0.3006 0.058 Uiso 1 1 calc R U . . .
H28C H 0.3718 -0.0568 0.3759 0.058 Uiso 1 1 calc R U . . .
C29 C 0.3382(5) 0.0003(5) 0.5467(8) 0.035(2) Uani 1 1 d . . . . .
H29 H 0.3133 -0.0341 0.5240 0.042 Uiso 1 1 calc R U . . .
C30 C 0.3086(6) 0.0506(6) 0.4959(8) 0.039(3) Uani 1 1 d . . . . .
H30 H 0.2714 0.0391 0.4460 0.047 Uiso 1 1 calc R U . . .
C31 C 0.3157(5) 0.1115(5) 0.4946(8) 0.037(3) Uani 1 1 d . . . . .
H31 H 0.2820 0.1283 0.4443 0.045 Uiso 1 1 calc R U . . .
C32 C 0.3574(6) 0.1561(5) 0.5445(7) 0.033(2) Uani 1 1 d . . . . .
H32 H 0.3459 0.1931 0.5135 0.039 Uiso 1 1 calc R U . . .
C33 C 0.4104(5) 0.1626(4) 0.6255(7) 0.029(2) Uani 1 1 d . . . . .
H33 H 0.4211 0.2032 0.6361 0.035 Uiso 1 1 calc R U . . .
C34 C 0.4525(5) 0.1285(5) 0.6957(8) 0.035(2) Uani 1 1 d . . . . .
H34 H 0.4802 0.1533 0.7426 0.042 Uiso 1 1 calc R U . . .
C35 C 0.4670(5) 0.0694(5) 0.7191(7) 0.032(2) Uani 1 1 d . . . . .
H35 H 0.5035 0.0669 0.7742 0.039 Uiso 1 1 calc R U . . .
C36 C 0.4455(5) 0.0132(5) 0.6883(7) 0.029(2) Uani 1 1 d . . . . .
H36 H 0.4748 -0.0157 0.7235 0.035 Uiso 1 1 calc R U . . .
C37 C 0.3938(6) -0.0140(4) 0.6212(8) 0.032(2) Uani 1 1 d . . . . .
H37 H 0.3975 -0.0557 0.6283 0.038 Uiso 1 1 calc R U . . .
C38 C 0.6983(6) 0.2841(8) 0.3956(9) 0.053(4) Uani 1 1 d . . . . .
H38 H 0.7326 0.2985 0.3727 0.064 Uiso 1 1 calc R U . . .
C39 C 0.6547(7) 0.3301(6) 0.3985(9) 0.048(4) Uani 1 1 d . . . . .
H39 H 0.6695 0.3656 0.3769 0.058 Uiso 1 1 calc R U . . .
C40 C 0.5988(8) 0.3411(5) 0.4216(9) 0.055(4) Uani 1 1 d . . . . .
H40 H 0.5865 0.3813 0.4094 0.065 Uiso 1 1 calc R U . . .
C41 C 0.5546(6) 0.3115(7) 0.4574(9) 0.050(4) Uani 1 1 d . . . . .
H41 H 0.5206 0.3374 0.4604 0.060 Uiso 1 1 calc R U . . .
C42 C 0.5441(6) 0.2567(8) 0.4899(8) 0.052(4) Uani 1 1 d . . . . .
H42 H 0.5062 0.2568 0.5112 0.062 Uiso 1 1 calc R U . . .
C43 C 0.5725(9) 0.2010(8) 0.5012(8) 0.064(5) Uani 1 1 d . . . . .
H43 H 0.5479 0.1755 0.5294 0.077 Uiso 1 1 calc R U . . .
C44 C 0.6226(11) 0.1700(6) 0.4862(9) 0.069(6) Uani 1 1 d . . . . .
H44 H 0.6210 0.1299 0.5046 0.082 Uiso 1 1 calc R U . . .
C45 C 0.6768(9) 0.1799(6) 0.4511(9) 0.057(4) Uani 1 1 d . . . . .
H45 H 0.7001 0.1441 0.4526 0.068 Uiso 1 1 calc R U . . .
C46 C 0.7063(5) 0.2246(9) 0.4158(9) 0.058(5) Uani 1 1 d . . . . .
H46 H 0.7436 0.2102 0.4005 0.069 Uiso 1 1 calc R U . . .
C47 C 0.0544(6) 0.2586(7) 0.0761(8) 0.048(3) Uani 1 1 d . . . . .
H47 H 0.0187 0.2553 0.0199 0.058 Uiso 1 1 calc R U . . .
C48 C 0.0676(6) 0.3184(6) 0.1007(8) 0.043(3) Uani 1 1 d . . . . .
H48 H 0.0399 0.3433 0.0541 0.051 Uiso 1 1 calc R U . . .
C49 C 0.1087(6) 0.3514(5) 0.1717(10) 0.040(3) Uani 1 1 d . . . . .
H49 H 0.1023 0.3922 0.1567 0.048 Uiso 1 1 calc R U . . .
C50 C 0.1569(6) 0.3446(5) 0.2591(10) 0.042(3) Uani 1 1 d . . . . .
H50 H 0.1690 0.3822 0.2877 0.050 Uiso 1 1 calc R U . . .
C51 C 0.1926(6) 0.3012(6) 0.3172(9) 0.042(3) Uani 1 1 d . . . . .
H51 H 0.2201 0.3178 0.3744 0.051 Uiso 1 1 calc R U . . .
C52 C 0.2003(6) 0.2393(7) 0.3169(8) 0.046(3) Uani 1 1 d . . . . .
H52 H 0.2347 0.2275 0.3708 0.055 Uiso 1 1 calc R U . . .
C53 C 0.1743(7) 0.1915(6) 0.2644(11) 0.051(3) Uani 1 1 d . . . . .
H53 H 0.1962 0.1566 0.2924 0.061 Uiso 1 1 calc R U . . .
C54 C 0.1257(7) 0.1782(6) 0.1828(12) 0.055(4) Uani 1 1 d . . . . .
H54 H 0.1251 0.1366 0.1737 0.066 Uiso 1 1 calc R U . . .
C55 C 0.0779(6) 0.2025(6) 0.1097(10) 0.051(4) Uani 1 1 d . . . . .
H55 H 0.0534 0.1725 0.0697 0.061 Uiso 1 1 calc R U . . .
C56 C 0.0487(6) 0.5860(7) 0.5741(8) 0.046(3) Uani 1 1 d . . . . .
H56 H 0.0125 0.5850 0.5184 0.056 Uiso 1 1 calc R U . . .
C57 C 0.0704(6) 0.6427(6) 0.5917(9) 0.047(3) Uani 1 1 d . . . . .
H57 H 0.0449 0.6682 0.5436 0.056 Uiso 1 1 calc R U . . .
C58 C 0.1176(6) 0.6751(5) 0.6567(9) 0.041(3) Uani 1 1 d . . . . .
H58 H 0.1131 0.7160 0.6411 0.049 Uiso 1 1 calc R U . . .
C59 C 0.1696(6) 0.6660(5) 0.7381(9) 0.040(3) Uani 1 1 d . . . . .
H59 H 0.1886 0.7028 0.7622 0.048 Uiso 1 1 calc R U . . .
C60 C 0.2025(6) 0.6205(6) 0.7949(8) 0.043(3) Uani 1 1 d . . . . .
H60 H 0.2343 0.6362 0.8487 0.052 Uiso 1 1 calc R U . . .
C61 C 0.2039(6) 0.5598(7) 0.7988(10) 0.052(4) Uani 1 1 d . . . . .
H61 H 0.2409 0.5471 0.8478 0.062 Uiso 1 1 calc R U . . .
C62 C 0.1682(8) 0.5106(7) 0.7535(11) 0.059(4) Uani 1 1 d . . . . .
H62 H 0.1893 0.4748 0.7788 0.070 Uiso 1 1 calc R U . . .
C63 C 0.1097(8) 0.4992(5) 0.6809(11) 0.052(4) Uani 1 1 d . . . . .
H63 H 0.0997 0.4583 0.6794 0.062 Uiso 1 1 calc R U . . .
C64 C 0.0621(6) 0.5292(7) 0.6109(10) 0.052(4) Uani 1 1 d . . . . .
H64 H 0.0288 0.5028 0.5786 0.063 Uiso 1 1 calc R U . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
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 N5 2.495(9) . ?
Yb1 N4 2.503(10) . ?
Yb1 N3 2.507(10) . ?
Yb1 N6 2.519(9) . ?
Yb1 N7 2.533(10) . ?
Yb1 N2 2.555(9) . ?
Yb1 N1 2.566(10) . ?
N1 C1 1.135(14) . ?
N2 C3 1.114(14) . ?
N3 C5 1.150(14) . ?
N4 C7 1.141(13) . ?
N5 C9 1.150(14) . ?
N6 C11 1.149(13) . ?
N7 C13 1.139(14) . ?
C1 C2 1.445(15) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.460(15) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.457(15) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.455(13) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.454(14) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.448(14) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.452(15) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
Yb2 N11 2.482(10) . ?
Yb2 N14 2.501(9) . ?
Yb2 N12 2.502(9) . ?
Yb2 N9 2.523(8) . ?
Yb2 N10 2.524(10) . ?
Yb2 N8 2.524(10) . ?
Yb2 N13 2.544(10) . ?
N8 C15 1.101(16) . ?
N9 C17 1.141(13) . ?
N10 C19 1.138(14) . ?
N11 C21 1.130(14) . ?
N12 C23 1.137(14) . ?
N13 C25 1.133(14) . ?
N14 C27 1.134(13) . ?
C15 C16 1.479(19) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.449(14) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.437(15) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.449(14) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.447(15) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.447(14) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.453(14) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C37 1.403(16) . ?
C29 C30 1.409(17) . ?
C29 H29 0.9500 . ?
C30 C31 1.387(17) . ?
C30 H30 0.9500 . ?
C31 C32 1.407(17) . ?
C31 H31 0.9500 . ?
C32 C33 1.393(15) . ?
C32 H32 0.9500 . ?
C33 C34 1.388(16) . ?
C33 H33 0.9500 . ?
C34 C35 1.393(16) . ?
C34 H34 0.9500 . ?
C35 C36 1.385(15) . ?
C35 H35 0.9500 . ?
C36 C37 1.395(15) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 C46 1.38(2) . ?
C38 C39 1.41(2) . ?
C38 H38 0.9500 . ?
C39 C40 1.36(2) . ?
C39 H39 0.9500 . ?
C40 C41 1.38(2) . ?
C40 H40 0.9500 . ?
C41 C42 1.37(2) . ?
C41 H41 0.9500 . ?
C42 C43 1.39(2) . ?
C42 H42 0.9500 . ?
C43 C44 1.36(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.41(3) . ?
C44 H44 0.9500 . ?
C45 C46 1.37(2) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C47 C55 1.40(2) . ?
C47 C48 1.41(2) . ?
C47 H47 0.9500 . ?
C48 C49 1.373(19) . ?
C48 H48 0.9500 . ?
C49 C50 1.400(19) . ?
C49 H49 0.9500 . ?
C50 C51 1.377(19) . ?
C50 H50 0.9500 . ?
C51 C52 1.41(2) . ?
C51 H51 0.9500 . ?
C52 C53 1.35(2) . ?
C52 H52 0.9500 . ?
C53 C54 1.37(2) . ?
C53 H53 0.9500 . ?
C54 C55 1.37(2) . ?
C54 H54 0.9500 . ?
C55 H55 0.9500 . ?
C56 C57 1.37(2) . ?
C56 C64 1.39(2) . ?
C56 H56 0.9500 . ?
C57 C58 1.383(19) . ?
C57 H57 0.9500 . ?
C58 C59 1.393(18) . ?
C58 H58 0.9500 . ?
C59 C60 1.381(19) . ?
C59 H59 0.9500 . ?
C60 C61 1.37(2) . ?
C60 H60 0.9500 . ?
C61 C62 1.41(2) . ?
C61 H61 0.9500 . ?
C62 C63 1.42(2) . ?
C62 H62 0.9500 . ?
C63 C64 1.40(2) . ?
C63 H63 0.9500 . ?
C64 H64 0.9500 . ?
 
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
N5 Yb1 N4 73.9(3) . . ?
N5 Yb1 N3 85.5(4) . . ?
N4 Yb1 N3 90.2(4) . . ?
N5 Yb1 N6 79.3(3) . . ?
N4 Yb1 N6 153.1(3) . . ?
N3 Yb1 N6 85.2(3) . . ?
N5 Yb1 N7 80.1(3) . . ?
N4 Yb1 N7 80.7(3) . . ?
N3 Yb1 N7 164.6(3) . . ?
N6 Yb1 N7 97.3(3) . . ?
N5 Yb1 N2 143.5(3) . . ?
N4 Yb1 N2 75.9(3) . . ?
N3 Yb1 N2 74.5(3) . . ?
N6 Yb1 N2 127.6(3) . . ?
N7 Yb1 N2 114.7(3) . . ?
N5 Yb1 N1 138.7(3) . . ?
N4 Yb1 N1 128.7(3) . . ?
N3 Yb1 N1 122.9(3) . . ?
N6 Yb1 N1 74.6(3) . . ?
N7 Yb1 N1 72.3(3) . . ?
N2 Yb1 N1 77.1(3) . . ?
C1 N1 Yb1 162.3(9) . . ?
C3 N2 Yb1 171.9(9) . . ?
C5 N3 Yb1 169.4(9) . . ?
C7 N4 Yb1 174.5(9) . . ?
C9 N5 Yb1 160.9(9) . . ?
C11 N6 Yb1 169.5(9) . . ?
C13 N7 Yb1 168.1(9) . . ?
N1 C1 C2 179.0(14) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 C3 C4 179.3(12) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N3 C5 C6 177.8(12) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N4 C7 C8 178.6(12) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N5 C9 C10 176.2(13) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N6 C11 C12 178.0(11) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N7 C13 C14 178.7(13) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N11 Yb2 N14 125.9(3) . . ?
N11 Yb2 N12 97.1(3) . . ?
N14 Yb2 N12 116.2(3) . . ?
N11 Yb2 N9 74.5(3) . . ?
N14 Yb2 N9 150.6(3) . . ?
N12 Yb2 N9 76.8(3) . . ?
N11 Yb2 N10 75.2(3) . . ?
N14 Yb2 N10 81.2(3) . . ?
N12 Yb2 N10 161.6(3) . . ?
N9 Yb2 N10 85.0(3) . . ?
N11 Yb2 N8 147.2(4) . . ?
N14 Yb2 N8 76.2(3) . . ?
N12 Yb2 N8 92.0(4) . . ?
N9 Yb2 N8 77.1(3) . . ?
N10 Yb2 N8 86.4(4) . . ?
N11 Yb2 N13 82.1(3) . . ?
N14 Yb2 N13 70.6(3) . . ?
N12 Yb2 N13 72.0(3) . . ?
N9 Yb2 N13 137.9(3) . . ?
N10 Yb2 N13 122.2(4) . . ?
N8 Yb2 N13 130.6(4) . . ?
C15 N8 Yb2 162.4(13) . . ?
C17 N9 Yb2 172.0(8) . . ?
C19 N10 Yb2 160.1(10) . . ?
C21 N11 Yb2 166.3(9) . . ?
C23 N12 Yb2 153.9(9) . . ?
C25 N13 Yb2 151.9(9) . . ?
C27 N14 Yb2 157.5(9) . . ?
N8 C15 C16 178.1(19) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N9 C17 C18 178.9(11) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N10 C19 C20 179.0(13) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N11 C21 C22 179.5(13) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N12 C23 C24 179.2(12) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N13 C25 C26 177.5(11) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N14 C27 C28 176.6(12) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C37 C29 C30 138.6(10) . . ?
C37 C29 H29 110.7 . . ?
C30 C29 H29 110.7 . . ?
C31 C30 C29 140.8(11) . . ?
C31 C30 H30 109.6 . . ?
C29 C30 H30 109.6 . . ?
C30 C31 C32 139.7(10) . . ?
C30 C31 H31 110.2 . . ?
C32 C31 H31 110.2 . . ?
C33 C32 C31 139.4(10) . . ?
C33 C32 H32 110.3 . . ?
C31 C32 H32 110.3 . . ?
C34 C33 C32 140.1(10) . . ?
C34 C33 H33 109.9 . . ?
C32 C33 H33 109.9 . . ?
C33 C34 C35 139.9(10) . . ?
C33 C34 H34 110.0 . . ?
C35 C34 H34 110.0 . . ?
C36 C35 C34 140.7(10) . . ?
C36 C35 H35 109.7 . . ?
C34 C35 H35 109.7 . . ?
C35 C36 C37 139.2(10) . . ?
C35 C36 H36 110.4 . . ?
C37 C36 H36 110.4 . . ?
C36 C37 C29 140.6(10) . . ?
C36 C37 H37 109.7 . . ?
C29 C37 H37 109.7 . . ?
C46 C38 C39 139.3(12) . . ?
C46 C38 H38 110.3 . . ?
C39 C38 H38 110.3 . . ?
C40 C39 C38 141.8(12) . . ?
C40 C39 H39 109.1 . . ?
C38 C39 H39 109.1 . . ?
C39 C40 C41 139.0(12) . . ?
C39 C40 H40 110.5 . . ?
C41 C40 H40 110.5 . . ?
C42 C41 C40 140.4(12) . . ?
C42 C41 H41 109.8 . . ?
C40 C41 H41 109.8 . . ?
C41 C42 C43 138.7(12) . . ?
C41 C42 H42 110.6 . . ?
C43 C42 H42 110.6 . . ?
C44 C43 C42 142.5(13) . . ?
C44 C43 H43 108.7 . . ?
C42 C43 H43 108.7 . . ?
C43 C44 C45 138.6(13) . . ?
C43 C44 H44 110.7 . . ?
C45 C44 H44 110.7 . . ?
C46 C45 C44 140.2(12) . . ?
C46 C45 H45 109.9 . . ?
C44 C45 H45 109.9 . . ?
C45 C46 C38 139.3(12) . . ?
C45 C46 H46 110.3 . . ?
C38 C46 H46 110.3 . . ?
C55 C47 C48 139.0(11) . . ?
C55 C47 H47 110.5 . . ?
C48 C47 H47 110.5 . . ?
C49 C48 C47 139.0(11) . . ?
C49 C48 H48 110.5 . . ?
C47 C48 H48 110.5 . . ?
C48 C49 C50 140.6(11) . . ?
C48 C49 H49 109.7 . . ?
C50 C49 H49 109.7 . . ?
C51 C50 C49 140.7(11) . . ?
C51 C50 H50 109.7 . . ?
C49 C50 H50 109.7 . . ?
C50 C51 C52 138.8(11) . . ?
C50 C51 H51 110.6 . . ?
C52 C51 H51 110.6 . . ?
C53 C52 C51 140.2(12) . . ?
C53 C52 H52 109.9 . . ?
C51 C52 H52 109.9 . . ?
C52 C53 C54 139.0(13) . . ?
C52 C53 H53 110.5 . . ?
C54 C53 H53 110.5 . . ?
C55 C54 C53 143.3(13) . . ?
C55 C54 H54 108.3 . . ?
C53 C54 H54 108.3 . . ?
C54 C55 C47 138.9(12) . . ?
C54 C55 H55 110.5 . . ?
C47 C55 H55 110.5 . . ?
C57 C56 C64 140.8(11) . . ?
C57 C56 H56 109.6 . . ?
C64 C56 H56 109.6 . . ?
C56 C57 C58 140.5(11) . . ?
C56 C57 H57 109.7 . . ?
C58 C57 H57 109.7 . . ?
C57 C58 C59 139.2(11) . . ?
C57 C58 H58 110.4 . . ?
C59 C58 H58 110.4 . . ?
C60 C59 C58 140.3(11) . . ?
C60 C59 H59 109.9 . . ?
C58 C59 H59 109.9 . . ?
C61 C60 C59 140.4(11) . . ?
C61 C60 H60 109.8 . . ?
C59 C60 H60 109.8 . . ?
C60 C61 C62 140.4(12) . . ?
C60 C61 H61 109.8 . . ?
C62 C61 H61 109.8 . . ?
C61 C62 C63 138.0(12) . . ?
C61 C62 H62 111.0 . . ?
C63 C62 H62 111.0 . . ?
C64 C63 C62 139.9(12) . . ?
C64 C63 H63 110.1 . . ?
C62 C63 H63 110.1 . . ?
C56 C64 C63 139.4(12) . . ?
C56 C64 H64 110.3 . . ?
C63 C64 H64 110.3 . . ?
 
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
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
C37 C29 C30 C31 -4(3) . . . . ?
C29 C30 C31 C32 0(3) . . . . ?
C30 C31 C32 C33 -6(3) . . . . ?
C31 C32 C33 C34 6(3) . . . . ?
C32 C33 C34 C35 6(3) . . . . ?
C33 C34 C35 C36 -4(3) . . . . ?
C34 C35 C36 C37 -7(3) . . . . ?
C35 C36 C37 C29 4(3) . . . . ?
C30 C29 C37 C36 7(3) . . . . ?
C46 C38 C39 C40 0(3) . . . . ?
C38 C39 C40 C41 2(3) . . . . ?
C39 C40 C41 C42 2(3) . . . . ?
C40 C41 C42 C43 -3(3) . . . . ?
C41 C42 C43 C44 -2(3) . . . . ?
C42 C43 C44 C45 2(3) . . . . ?
C43 C44 C45 C46 1(3) . . . . ?
C44 C45 C46 C38 0(3) . . . . ?
C39 C38 C46 C45 -2(3) . . . . ?
C55 C47 C48 C49 -3(3) . . . . ?
C47 C48 C49 C50 -4(3) . . . . ?
C48 C49 C50 C51 7(3) . . . . ?
C49 C50 C51 C52 2(3) . . . . ?
C50 C51 C52 C53 -6(3) . . . . ?
C51 C52 C53 C54 0(3) . . . . ?
C52 C53 C54 C55 1(4) . . . . ?
C53 C54 C55 C47 4(4) . . . . ?
C48 C47 C55 C54 0(3) . . . . ?
C64 C56 C57 C58 -1(3) . . . . ?
C56 C57 C58 C59 3(3) . . . . ?
C57 C58 C59 C60 2(3) . . . . ?
C58 C59 C60 C61 5(3) . . . . ?
C59 C60 C61 C62 -10(3) . . . . ?
C60 C61 C62 C63 -3(3) . . . . ?
C61 C62 C63 C64 10(3) . . . . ?
C57 C56 C64 C63 -9(3) . . . . ?
C62 C63 C64 C56 3(3) . . . . ?
 
_refine_diff_density_max    7.790
_refine_diff_density_min   -3.020
_refine_diff_density_rms    0.232


 

# ===END

 
data_6
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C18 H18 Tm'
_chemical_formula_sum
 'C18 H18 Tm' 
_chemical_formula_weight          403.25

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'
 'Tm'  'Tm'  -0.3139   5.2483
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/n'
_space_group_name_Hall            '-P 2yn'
 
_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.
;
 
loop_
 _space_group_symop_operation_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'
 
_cell_length_a                    7.3412(5)
_cell_length_b                    8.8404(5)
_cell_length_c                    11.1729(7)
_cell_angle_alpha                 90
_cell_angle_beta                  100.906(2)
_cell_angle_gamma                 90
_cell_volume                      712.02(8)
_cell_formula_units_Z             2
_cell_measurement_temperature     150.0(1)
_cell_measurement_reflns_used     8647
_cell_measurement_theta_min        2.9584
_cell_measurement_theta_max       28.5901
 
_exptl_crystal_description        'block'
_exptl_crystal_colour             'dark brown'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.881          
_exptl_crystal_F_000              390
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.100
_exptl_crystal_size_mid           0.060
_exptl_crystal_size_min           0.040
_exptl_absorpt_coefficient_mu     6.213
_shelx_estimated_absorpt_T_min    0.523
_shelx_estimated_absorpt_T_max    0.636
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min    0.6361
_exptl_absorpt_correction_T_max    0.7464
_exptl_absorpt_process_details    'SADABS'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       150(2)
_diffrn_radiation_wavelength      0.71069
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   'Kappa APEX II'
_diffrn_measurement_method        'phi and omega scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             29740
_diffrn_reflns_av_unetI/netI      0.0224
_diffrn_reflns_av_R_equivalents   0.0500
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -17
_diffrn_reflns_limit_l_max        17
_diffrn_reflns_theta_min          3.647
_diffrn_reflns_theta_max          32.891
_diffrn_reflns_theta_full         25.240
_diffrn_measured_fraction_theta_max   0.997
_diffrn_measured_fraction_theta_full  0.998
_diffrn_reflns_Laue_measured_fraction_max    0.997
_diffrn_reflns_Laue_measured_fraction_full   0.998
_diffrn_reflns_point_group_measured_fraction_max   0.997
_diffrn_reflns_point_group_measured_fraction_full  0.998
_reflns_number_total              2652
_reflns_number_gt                 1750
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'Bruker APEX2'
_computing_cell_refinement        'Bruker SAINT'
_computing_data_reduction         'Bruker SAINT'
_computing_structure_solution     'SHELXT(Sheldrick,2014)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     'PLATON (Spek, 2009)'
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0361P)²+0.7790P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          2652
_refine_ls_number_parameters      169
_refine_ls_number_restraints      108
_refine_ls_R_factor_all           0.0396
_refine_ls_R_factor_gt            0.0219
_refine_ls_wR_factor_ref          0.0647
_refine_ls_wR_factor_gt           0.0560
_refine_ls_goodness_of_fit_ref    0.988
_refine_ls_restrained_S_all       1.008
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
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
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Tm1 Tm 0.0000 0.0000 0.0000 0.02104(6) Uani 1 2 d S . P . .
C1 C 0.147(3) -0.0049(11) 0.2464(8) 0.0430(19) Uani 0.5 1 d . U P A 1
H1 H 0.1665 -0.0846 0.3044 0.052 Uiso 0.5 1 calc R U P A 1
C2 C 0.303(2) 0.0122(13) 0.1906(12) 0.043(2) Uani 0.5 1 d . U P A 1
H2 H 0.4009 -0.0517 0.2291 0.051 Uiso 0.5 1 calc R U P A 1
C3 C 0.3577(14) 0.0912(14) 0.0992(12) 0.038(2) Uani 0.5 1 d . U P A 1
H3 H 0.4801 0.0623 0.0929 0.045 Uiso 0.5 1 calc R U P A 1
C4 C 0.2966(13) 0.1953(14) 0.0161(11) 0.033(2) Uani 0.5 1 d . U P A 1
H4 H 0.3912 0.2167 -0.0288 0.040 Uiso 0.5 1 calc R U P A 1
C5 C 0.1468(16) 0.2817(10) -0.0273(8) 0.0247(17) Uani 0.5 1 d . U P A 1
H5 H 0.1675 0.3396 -0.0951 0.030 Uiso 0.5 1 calc R U P A 1
C6 C -0.0347(11) 0.3126(8) -0.0019(6) 0.0196(15) Uani 0.5 1 d . U P A 1
H6 H -0.0958 0.3862 -0.0572 0.023 Uiso 0.5 1 calc R U P A 1
C7 C -0.1516(11) 0.2676(10) 0.0802(8) 0.0244(14) Uani 0.5 1 d . U P A 1
H7 H -0.2670 0.3193 0.0628 0.029 Uiso 0.5 1 calc R U P A 1
C8 C -0.1453(14) 0.1714(13) 0.1769(8) 0.0292(17) Uani 0.5 1 d . U P A 1
H8 H -0.2543 0.1842 0.2101 0.035 Uiso 0.5 1 calc R U P A 1
C9 C -0.037(2) 0.0639(12) 0.2415(8) 0.036(2) Uani 0.5 1 d . U P A 1
H9 H -0.0972 0.0202 0.3012 0.043 Uiso 0.5 1 calc R U P A 1
C10 C -0.2281(14) 0.0224(8) -0.2279(7) 0.0250(15) Uani 0.5 1 d . U P A 2
H10 H -0.2836 0.1054 -0.2753 0.030 Uiso 0.5 1 calc R U P A 2
C11 C -0.3432(10) -0.0337(11) -0.1524(10) 0.0242(17) Uani 0.5 1 d . U P A 2
H11 H -0.4597 0.0162 -0.1709 0.029 Uiso 0.5 1 calc R U P A 2
C12 C -0.3463(14) -0.1352(13) -0.0613(9) 0.0271(17) Uani 0.5 1 d . U P A 2
H12 H -0.4652 -0.1328 -0.0395 0.032 Uiso 0.5 1 calc R U P A 2
C13 C -0.2420(18) -0.2363(12) 0.0078(8) 0.032(2) Uani 0.5 1 d . U P A 2
H13 H -0.3082 -0.2775 0.0655 0.039 Uiso 0.5 1 calc R U P A 2
C14 C -0.0630(19) -0.3027(9) 0.0231(9) 0.035(2) Uani 0.5 1 d . U P A 2
H14 H -0.0417 -0.3712 0.0898 0.042 Uiso 0.5 1 calc R U P A 2
C15 C 0.0971(14) -0.2933(9) -0.0370(12) 0.038(2) Uani 0.5 1 d . U P A 2
H15 H 0.1903 -0.3621 0.0000 0.046 Uiso 0.5 1 calc R U P A 2
C16 C 0.1564(11) -0.2161(12) -0.1305(13) 0.037(2) Uani 0.5 1 d . U P A 2
H16 H 0.2738 -0.2538 -0.1406 0.045 Uiso 0.5 1 calc R U P A 2
C17 C 0.1017(12) -0.1054(15) -0.2115(11) 0.0351(19) Uani 0.5 1 d . U P A 2
H17 H 0.1981 -0.0839 -0.2549 0.042 Uiso 0.5 1 calc R U P A 2
C18 C -0.0492(15) -0.0116(12) -0.2531(6) 0.0285(14) Uani 0.5 1 d . U P A 2
H18 H -0.0257 0.0488 -0.3189 0.034 Uiso 0.5 1 calc R U P A 2
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
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
Tm1 C14 2.736(8) . ?
Tm1 C14 2.736(8) 3 ?
Tm1 C15 2.741(8) . ?
Tm1 C15 2.741(8) 3 ?
Tm1 C5 2.753(7) 3 ?
Tm1 C5 2.754(7) . ?
Tm1 C13 2.755(9) 3 ?
Tm1 C13 2.755(9) . ?
Tm1 C4 2.757(9) . ?
Tm1 C4 2.757(9) 3 ?
Tm1 C1 2.760(8) . ?
Tm1 C1 2.760(8) 3 ?
C1 C2 1.41(2) . ?
C1 C9 1.47(2) . ?
C1 H1 0.9500 . ?
C2 C3 1.358(18) . ?
C2 H2 0.9500 . ?
C3 C4 1.323(14) . ?
C3 H3 0.9500 . ?
C4 C5 1.352(13) . ?
C4 H4 0.9500 . ?
C5 C6 1.440(12) . ?
C5 H5 0.9500 . ?
C6 C7 1.426(10) . ?
C6 H6 0.9500 . ?
C7 C8 1.369(11) . ?
C7 H7 0.9500 . ?
C8 C9 1.357(13) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.393(12) . ?
C10 C18 1.426(13) . ?
C10 H10 0.9500 . ?
C11 C12 1.361(12) . ?
C11 H11 0.9500 . ?
C12 C13 1.325(12) . ?
C12 H12 0.9500 . ?
C13 C14 1.420(15) . ?
C13 H13 0.9500 . ?
C14 C15 1.46(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.386(16) . ?
C15 H15 0.9500 . ?
C16 C17 1.342(14) . ?
C16 H16 0.9500 . ?
C17 C18 1.392(13) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
 
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
C14 Tm1 C14 180.0 . 3 ?
C14 Tm1 C15 31.0(5) . . ?
C14 Tm1 C15 149.0(5) 3 . ?
C14 Tm1 C15 149.0(5) . 3 ?
C14 Tm1 C15 31.0(5) 3 3 ?
C15 Tm1 C15 180.0 . 3 ?
C5 Tm1 C5 180.0 3 . ?
C14 Tm1 C13 150.0(3) . 3 ?
C14 Tm1 C13 30.0(3) 3 3 ?
C15 Tm1 C13 121.7(4) . 3 ?
C15 Tm1 C13 58.3(4) 3 3 ?
C14 Tm1 C13 30.0(3) . . ?
C14 Tm1 C13 150.0(3) 3 . ?
C15 Tm1 C13 58.3(4) . . ?
C15 Tm1 C13 121.7(4) 3 . ?
C13 Tm1 C13 180.0 3 . ?
C5 Tm1 C4 151.6(3) 3 . ?
C5 Tm1 C4 28.4(3) . . ?
C5 Tm1 C4 28.4(3) 3 3 ?
C5 Tm1 C4 151.6(3) . 3 ?
C4 Tm1 C4 180.0 . 3 ?
C5 Tm1 C1 87.9(3) 3 . ?
C5 Tm1 C1 92.1(3) . . ?
C4 Tm1 C1 77.9(4) . . ?
C4 Tm1 C1 102.1(4) 3 . ?
C5 Tm1 C1 92.1(3) 3 3 ?
C5 Tm1 C1 87.9(3) . 3 ?
C4 Tm1 C1 102.1(4) . 3 ?
C4 Tm1 C1 77.9(4) 3 3 ?
C1 Tm1 C1 180.0 . 3 ?
C2 C1 C9 139.0(9) . . ?
C2 C1 Tm1 75.8(5) . . ?
C9 C1 Tm1 76.9(5) . . ?
C2 C1 H1 110.5 . . ?
C9 C1 H1 110.5 . . ?
Tm1 C1 H1 132.2 . . ?
C3 C2 C1 139.9(9) . . ?
C3 C2 Tm1 75.6(6) . . ?
C1 C2 Tm1 74.6(6) . . ?
C3 C2 H2 110.0 . . ?
C1 C2 H2 110.0 . . ?
Tm1 C2 H2 138.7 . . ?
C4 C3 C2 140.9(10) . . ?
C4 C3 Tm1 75.6(5) . . ?
C2 C3 Tm1 76.1(6) . . ?
C4 C3 H3 109.6 . . ?
C2 C3 H3 109.6 . . ?
Tm1 C3 H3 136.9 . . ?
C3 C4 C5 142.2(9) . . ?
C3 C4 Tm1 76.7(6) . . ?
C5 C4 Tm1 75.6(5) . . ?
C3 C4 H4 108.9 . . ?
C5 C4 H4 108.9 . . ?
Tm1 C4 H4 137.5 . . ?
C4 C5 C6 139.2(8) . . ?
C4 C5 Tm1 76.0(5) . . ?
C6 C5 Tm1 75.7(4) . . ?
C4 C5 H5 110.4 . . ?
C6 C5 H5 110.4 . . ?
Tm1 C5 H5 134.5 . . ?
C7 C6 C5 140.0(8) . . ?
C7 C6 Tm1 77.5(4) . . ?
C5 C6 Tm1 74.1(5) . . ?
C7 C6 H6 110.0 . . ?
C5 C6 H6 110.0 . . ?
Tm1 C6 H6 135.9 . . ?
C8 C7 C6 138.3(8) . . ?
C8 C7 Tm1 76.9(5) . . ?
C6 C7 Tm1 73.1(4) . . ?
C8 C7 H7 110.9 . . ?
C6 C7 H7 110.9 . . ?
Tm1 C7 H7 136.5 . . ?
C9 C8 C7 141.6(9) . . ?
C9 C8 Tm1 74.8(5) . . ?
C7 C8 Tm1 75.2(5) . . ?
C9 C8 H8 109.2 . . ?
C7 C8 H8 109.2 . . ?
Tm1 C8 H8 141.9 . . ?
C8 C9 C1 138.7(9) . . ?
C8 C9 Tm1 77.5(5) . . ?
C1 C9 Tm1 72.5(5) . . ?
C8 C9 H9 110.7 . . ?
C1 C9 H9 110.7 . . ?
Tm1 C9 H9 137.1 . . ?
C11 C10 C18 137.0(8) . . ?
C11 C10 Tm1 75.5(4) . . ?
C18 C10 Tm1 75.4(4) . . ?
C11 C10 H10 111.5 . . ?
C18 C10 H10 111.5 . . ?
Tm1 C10 H10 133.3 . . ?
C12 C11 C10 141.8(8) . . ?
C12 C11 Tm1 75.7(5) . . ?
C10 C11 Tm1 75.5(4) . . ?
C12 C11 H11 109.1 . . ?
C10 C11 H11 109.1 . . ?
Tm1 C11 H11 139.4 . . ?
C13 C12 C11 142.3(9) . . ?
C13 C12 Tm1 75.3(5) . . ?
C11 C12 Tm1 75.9(5) . . ?
C13 C12 H12 108.9 . . ?
C11 C12 H12 108.9 . . ?
Tm1 C12 H12 140.4 . . ?
C12 C13 C14 140.2(9) . . ?
C12 C13 Tm1 77.0(5) . . ?
C14 C13 Tm1 74.3(5) . . ?
C12 C13 H13 109.9 . . ?
C14 C13 H13 109.9 . . ?
Tm1 C13 H13 136.7 . . ?
C13 C14 C15 136.7(8) . . ?
C13 C14 Tm1 75.7(5) . . ?
C15 C14 Tm1 74.7(5) . . ?
C13 C14 H14 111.7 . . ?
C15 C14 H14 111.7 . . ?
Tm1 C14 H14 133.7 . . ?
C16 C15 C14 140.3(8) . . ?
C16 C15 Tm1 77.0(5) . . ?
C14 C15 Tm1 74.3(5) . . ?
C16 C15 H15 109.9 . . ?
C14 C15 H15 109.9 . . ?
Tm1 C15 H15 136.6 . . ?
C17 C16 C15 140.4(8) . . ?
C17 C16 Tm1 75.6(5) . . ?
C15 C16 Tm1 73.9(5) . . ?
C17 C16 H16 109.8 . . ?
C15 C16 H16 109.8 . . ?
Tm1 C16 H16 141.0 . . ?
C16 C17 C18 141.1(9) . . ?
C16 C17 Tm1 76.4(6) . . ?
C18 C17 Tm1 76.0(4) . . ?
C16 C17 H17 109.5 . . ?
C18 C17 H17 109.5 . . ?
Tm1 C17 H17 135.6 . . ?
C17 C18 C10 139.9(8) . . ?
C17 C18 Tm1 75.0(5) . . ?
C10 C18 Tm1 74.9(4) . . ?
C17 C18 H18 110.1 . . ?
C10 C18 H18 110.1 . . ?
Tm1 C18 H18 139.3 . . ?
 
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
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
C9 C1 C2 C3 -7(2) . . . . ?
Tm1 C1 C2 C3 43.2(13) . . . . ?
C9 C1 C2 Tm1 -49.8(12) . . . . ?
C1 C2 C3 C4 2(2) . . . . ?
Tm1 C2 C3 C4 44.7(14) . . . . ?
C1 C2 C3 Tm1 -42.9(13) . . . . ?
C2 C3 C4 C5 -1(2) . . . . ?
Tm1 C3 C4 C5 43.9(13) . . . . ?
C2 C3 C4 Tm1 -44.9(14) . . . . ?
C3 C4 C5 C6 3(2) . . . . ?
Tm1 C4 C5 C6 47.4(10) . . . . ?
C3 C4 C5 Tm1 -44.2(13) . . . . ?
C4 C5 C6 C7 -1.1(18) . . . . ?
Tm1 C5 C6 C7 46.3(10) . . . . ?
C4 C5 C6 Tm1 -47.4(10) . . . . ?
C5 C6 C7 C8 0.5(18) . . . . ?
Tm1 C6 C7 C8 45.9(10) . . . . ?
C5 C6 C7 Tm1 -45.4(10) . . . . ?
C6 C7 C8 C9 -5(2) . . . . ?
Tm1 C7 C8 C9 39.7(12) . . . . ?
C6 C7 C8 Tm1 -44.8(10) . . . . ?
C7 C8 C9 C1 4(2) . . . . ?
Tm1 C8 C9 C1 44.1(11) . . . . ?
C7 C8 C9 Tm1 -39.8(12) . . . . ?
C2 C1 C9 C8 4(2) . . . . ?
Tm1 C1 C9 C8 -45.4(12) . . . . ?
C2 C1 C9 Tm1 49.5(12) . . . . ?
C18 C10 C11 C12 6.4(18) . . . . ?
Tm1 C10 C11 C12 -42.3(11) . . . . ?
C18 C10 C11 Tm1 48.7(9) . . . . ?
C10 C11 C12 C13 1(2) . . . . ?
Tm1 C11 C12 C13 -41.1(13) . . . . ?
C10 C11 C12 Tm1 42.2(11) . . . . ?
C11 C12 C13 C14 -3(2) . . . . ?
Tm1 C12 C13 C14 -44.7(12) . . . . ?
C11 C12 C13 Tm1 41.2(13) . . . . ?
C12 C13 C14 C15 -3(2) . . . . ?
Tm1 C13 C14 C15 -48.2(10) . . . . ?
C12 C13 C14 Tm1 45.4(12) . . . . ?
C13 C14 C15 C16 3.0(19) . . . . ?
Tm1 C14 C15 C16 -45.4(11) . . . . ?
C13 C14 C15 Tm1 48.5(10) . . . . ?
C14 C15 C16 C17 4(2) . . . . ?
Tm1 C15 C16 C17 -40.9(12) . . . . ?
C14 C15 C16 Tm1 44.8(11) . . . . ?
C15 C16 C17 C18 -5(2) . . . . ?
Tm1 C16 C17 C18 -46.0(12) . . . . ?
C15 C16 C17 Tm1 40.5(12) . . . . ?
C16 C17 C18 C10 4(2) . . . . ?
Tm1 C17 C18 C10 -42.5(10) . . . . ?
C16 C17 C18 Tm1 46.1(12) . . . . ?
C11 C10 C18 C17 -6.2(17) . . . . ?
Tm1 C10 C18 C17 42.5(10) . . . . ?
C11 C10 C18 Tm1 -48.7(9) . . . . ?
 
_refine_diff_density_max    0.993
_refine_diff_density_min   -0.477
_refine_diff_density_rms    0.121



# ===END of CIF
