#------------------------------------------------------------------------------
#$Date: 2023-02-23 09:57:30 +0200 (Thu, 23 Feb 2023) $
#$Revision: 281099 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/85/1568519.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1568519
loop_
_publ_author_name
'Hauser, Adrian'
'Münzfeld, Luca'
'Schlittenhardt, Sören'
'Köppe, Ralf'
'Uhlmann, Cedric'
'Rauska, Ulf-Christian'
'Ruben, Mario'
'Roesky, Peter W.'
_publ_section_title
;
 Molecular cyclo-P3 complexes of the rare-earth elements via a one-pot
 reaction and selective reduction
;
_journal_issue                   8
_journal_name_full               'Chemical Science'
_journal_page_first              2149
_journal_page_last               2158
_journal_paper_doi               10.1039/D2SC06730G
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C110 H156 N4 O6 P4 Yb2, C4 H8 O'
_chemical_formula_sum            'C114 H164 N4 O7 P4 Yb2'
_chemical_formula_weight         2172.44
_space_group_crystal_system      orthorhombic
_space_group_IT_number           50
_space_group_name_Hall           '-P 2ab 2b'
_space_group_name_H-M_alt        'P b a n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-07-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-12-02 deposited with the CCDC.	2023-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   32.1927(9)
_cell_length_b                   12.2887(4)
_cell_length_c                   14.1317(6)
_cell_measurement_reflns_used    24165
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.59
_cell_measurement_theta_min      2.88
_cell_volume                     5590.6(3)
_computing_cell_refinement       'X-Area Recipe 1.33.0.0 (STOE, 2015)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)'
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_details      '840 frames, detector distance = 100 mm'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32524
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.760
_diffrn_reflns_theta_min         2.903
_diffrn_source                   Axo_Mo
_diffrn_source_current           0.830
_diffrn_source_power             0.050
_diffrn_source_voltage           60
_exptl_absorpt_coefficient_mu    1.773
_exptl_absorpt_correction_T_max  0.8333
_exptl_absorpt_correction_T_min  0.3003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            'clear brownish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2264
_exptl_crystal_size_max          0.133
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.048
_refine_diff_density_max         2.592
_refine_diff_density_min         -1.371
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.918
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         6352
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      0.915
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0769P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1175
_reflns_d_resolution_high        0.763
_reflns_d_resolution_low         8.911
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              39
_reflns_limit_h_min              -41
_reflns_limit_k_max              6
_reflns_limit_k_min              -16
_reflns_limit_l_max              18
_reflns_limit_l_min              -17
_reflns_number_gt                3731
_reflns_number_total             6352
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2sc06730g3.cif
_cod_data_source_block           ah138-e2
_cod_original_sg_symbol_H-M      'P b a n'
_cod_database_code               1568519
_shelx_shelxl_version_number     2018/3
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O3-C29 = O3-C32
 1.44 with sigma of 0.02
 C29-C30
 1.53 with sigma of 0.02
 O3-C30 = C30-C32
 2.38 with sigma of 0.04
 O3-C29 \\sim O3-C32
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O3 \\sim C29 \\sim C30 \\sim C32: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C29 \\sim C32 \\sim O3 \\sim C31 \\sim C30: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.0002 within 2A
4. Rigid body (RIGU) restrains
 O3, C29, C30, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, C32, C31, C30, C29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.0001
5. Others
 Fixed Sof: O3(0.25) C29(0.25) H29A(0.25) H29B(0.25) C30(0.25) H30A(0.25)
 H30B(0.25) C32(0.25) H32A(0.25) H32B(0.25) C31(0.25) H31A(0.25) H31B(0.25)
6.a Ternary CH refined with riding coordinates:
 C19(H19), C22(H22)
6.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C27(H27A,H27B), C26(H26A,H26B), C25(H25A,H25B), C29(H29A,
 H29B), C30(H30A,H30B), C32(H32A,H32B), C31(H31A,H31B)
6.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C15(H15), C2(H2), C17(H17), C16(H16)
6.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C12(H12A,H12B,
 H12C), C24(H24A,H24B,H24C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C8(H8A,H8B,
 H8C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in mineral oil'
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '100.0 mm'
_stoe_detector_pixelsize_x       '0.075 mm'
_stoe_detector_pixelsize_y       '0.075 mm'
_stoe_detector_size_x            '8.0 cm'
_stoe_detector_size_y            '7.7 cm'
_stoe_evaluation_integration_a   10.1
_stoe_evaluation_integration_b   -0.1
_stoe_evaluation_integration_ems 0.014
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_completeness 94.4
_stoe_evaluation_lana_dxs_max_order 1
_stoe_evaluation_lana_dys_max_order 1
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 55.6
_stoe_evaluation_lana_max_2theta_desired 55.6
_stoe_evaluation_lana_mean_redundancy 4.1
_stoe_evaluation_lana_number_refls_after_or 25903
_stoe_evaluation_lana_number_refls_outliers 3130
_stoe_evaluation_lana_number_refls_total 29033
_stoe_evaluation_lana_number_refls_unique 6258
_stoe_evaluation_lana_number_refls_written 25903
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group mmm
_stoe_evaluation_lana_table
;
#----------------------------------------------------------------------------
2Theta           6.9   12.7   18.5   24.3   30.1   35.9   41.7   47.5   53.3
#----------------------------------------------------------------------------
<Resolution>    5.01   3.02   2.16   1.68   1.37   1.14   1.00   0.88   0.81
N(total)          84    821   2120   3502   3762   4659   5485   5654   2946
<Redundancy>     2.1    5.2    6.7    6.9    5.1    4.6    4.2    3.5    2.3
Complet. [%%]    82.1   98.4  100.0  100.0  100.0   99.7  100.0   99.7   77.4
<I/sigma>       64.2   45.3   31.4   18.6   11.7    7.2    4.9    2.9    1.9
R(int)         0.027  0.016  0.018  0.023  0.028  0.051  0.063  0.094  0.126
#----------------------------------------------------------------------------
;
_stoe_measurement_identifier     AH138-e2
_stoe_measurement_max_exposure_per_frame '20.0 s'
_stoe_measurement_mean_exposure_per_frame '20.0 s'
_stoe_measurement_min_exposure_per_frame '20.0 s'
_stoe_measurement_total_exposure_time '3.8 h'
_stoe_measurement_total_frame_number 675
_stoe_measurement_total_run_number 5
_stoe_measurement_tube_power     '49.8 W'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y, -z'
'x, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x-1/2, -y, z'
'-x, y-1/2, z'
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 0.66936(2) 0.250000 0.500000 0.02566(9) Uani 1 2 d S T P . .
P1 P 0.750000 0.250000 0.39092(11) 0.0316(3) Uani 1 2 d S T P . .
P2 P 0.750000 0.37269(12) 0.500000 0.0322(3) Uani 1 2 d S T P . .
O1 O 0.59804(10) 0.250000 0.500000 0.0254(8) Uani 1 2 d S T P . .
O2 O 0.65364(8) 0.0771(2) 0.42276(19) 0.0319(6) Uani 1 1 d . . . . .
N1 N 0.64467(9) 0.3292(3) 0.3645(2) 0.0284(7) Uani 1 1 d . . . . .
C28 C 0.68150(12) 0.0004(3) 0.3750(3) 0.0342(10) Uani 1 1 d . . . . .
H28A H 0.697261 -0.043181 0.421704 0.041 Uiso 1 1 calc R U . . .
H28B H 0.701411 0.039535 0.333843 0.041 Uiso 1 1 calc R U . . .
C13 C 0.66661(10) 0.3743(3) 0.2833(3) 0.0303(9) Uani 1 1 d . . . . .
C14 C 0.67317(12) 0.3110(4) 0.2019(3) 0.0323(10) Uani 1 1 d . . . . .
C23 C 0.70606(13) 0.6370(3) 0.3876(3) 0.0422(11) Uani 1 1 d . . . . .
H23A H 0.731098 0.594728 0.401903 0.063 Uiso 1 1 calc R U . . .
H23B H 0.698886 0.682482 0.442109 0.063 Uiso 1 1 calc R U . . .
H23C H 0.711234 0.683420 0.332417 0.063 Uiso 1 1 calc R U . . .
C6 C 0.57559(12) 0.2935(3) 0.4231(3) 0.0285(9) Uani 1 1 d . . . . .
C19 C 0.66259(13) 0.1888(4) 0.1974(3) 0.0360(10) Uani 1 1 d . . . . .
H19 H 0.656349 0.163505 0.263093 0.043 Uiso 1 1 calc R U . . .
C21 C 0.62353(13) 0.1671(4) 0.1352(3) 0.0442(11) Uani 1 1 d . . . . .
H21A H 0.599434 0.203739 0.163151 0.066 Uiso 1 1 calc R U . . .
H21B H 0.618279 0.088674 0.132013 0.066 Uiso 1 1 calc R U . . .
H21C H 0.628300 0.195381 0.071242 0.066 Uiso 1 1 calc R U . . .
C5 C 0.53263(12) 0.2965(3) 0.4206(3) 0.0307(9) Uani 1 1 d . . . . .
C4 C 0.51419(12) 0.3429(3) 0.3408(3) 0.0354(10) Uani 1 1 d . . . . .
H4 H 0.484757 0.344667 0.336371 0.042 Uiso 1 1 calc R U . . .
C15 C 0.69029(13) 0.3581(4) 0.1218(3) 0.0390(11) Uani 1 1 d . . . . .
H15 H 0.695005 0.314961 0.067093 0.047 Uiso 1 1 calc R U . . .
C3 C 0.53782(12) 0.3868(3) 0.2677(3) 0.0342(10) Uani 1 1 d . . . . .
C18 C 0.67840(11) 0.4850(3) 0.2835(3) 0.0315(9) Uani 1 1 d . . . . .
C2 C 0.58086(12) 0.3821(3) 0.2743(3) 0.0327(9) Uani 1 1 d . . . . .
H2 H 0.597024 0.411623 0.224229 0.039 Uiso 1 1 calc R U . . .
C1 C 0.60137(11) 0.3356(3) 0.3519(3) 0.0295(9) Uani 1 1 d . . . . .
C20 C 0.69965(14) 0.1238(4) 0.1608(3) 0.0439(11) Uani 1 1 d . . . . .
H20A H 0.705472 0.144583 0.095211 0.066 Uiso 1 1 calc R U . . .
H20B H 0.693264 0.045912 0.163685 0.066 Uiso 1 1 calc R U . . .
H20C H 0.724027 0.139209 0.200167 0.066 Uiso 1 1 calc R U . . .
C22 C 0.67024(11) 0.5597(4) 0.3661(3) 0.0358(11) Uani 1 1 d . . . . .
H22 H 0.666102 0.512971 0.423267 0.043 Uiso 1 1 calc R U . . .
C27 C 0.65306(13) -0.0723(4) 0.3163(3) 0.0392(10) Uani 1 1 d . . . . .
H27A H 0.665843 -0.144208 0.304210 0.047 Uiso 1 1 calc R U . . .
H27B H 0.645712 -0.037782 0.255222 0.047 Uiso 1 1 calc R U . . .
C17 C 0.69562(12) 0.5297(3) 0.2018(3) 0.0376(10) Uani 1 1 d . . . . .
H17 H 0.704045 0.603759 0.201627 0.045 Uiso 1 1 calc R U . . .
C16 C 0.70062(13) 0.4677(4) 0.1208(3) 0.0438(11) Uani 1 1 d . . . . .
H16 H 0.711096 0.500111 0.064640 0.053 Uiso 1 1 calc R U . . .
C11 C 0.50628(16) 0.250000 0.500000 0.0274(11) Uani 1 2 d S T P . .
C26 C 0.61511(12) -0.0817(3) 0.3818(3) 0.0393(11) Uani 1 1 d . . . . .
H26A H 0.590000 -0.103827 0.346226 0.047 Uiso 1 1 calc R U . . .
H26B H 0.620150 -0.134240 0.433590 0.047 Uiso 1 1 calc R U . . .
C25 C 0.61111(11) 0.0331(3) 0.4191(3) 0.0378(10) Uani 1 1 d . . . . .
H25A H 0.593504 0.077483 0.376614 0.045 Uiso 1 1 calc R U . . .
H25B H 0.598495 0.032834 0.483035 0.045 Uiso 1 1 calc R U . . .
C7 C 0.51818(13) 0.4399(4) 0.1795(3) 0.0423(11) Uani 1 1 d . . . . .
C12 C 0.47852(13) 0.1580(4) 0.4588(3) 0.0473(12) Uani 1 1 d . . . . .
H12A H 0.460640 0.187931 0.409065 0.071 Uiso 1 1 calc R U . . .
H12B H 0.461243 0.127324 0.509289 0.071 Uiso 1 1 calc R U . . .
H12C H 0.496159 0.100745 0.432067 0.071 Uiso 1 1 calc R U . . .
C24 C 0.63006(13) 0.6244(4) 0.3509(3) 0.0444(12) Uani 1 1 d . . . . .
H24A H 0.625793 0.674080 0.404293 0.067 Uiso 1 1 calc R U . . .
H24B H 0.606534 0.574006 0.346616 0.067 Uiso 1 1 calc R U . . .
H24C H 0.632158 0.666390 0.292180 0.067 Uiso 1 1 calc R U . . .
C9 C 0.53184(17) 0.3801(5) 0.0920(3) 0.0719(17) Uani 1 1 d . . . . .
H9A H 0.562231 0.380968 0.088023 0.108 Uiso 1 1 calc R U . . .
H9B H 0.520109 0.415609 0.035970 0.108 Uiso 1 1 calc R U . . .
H9C H 0.522082 0.304595 0.095002 0.108 Uiso 1 1 calc R U . . .
C10 C 0.53243(17) 0.5588(4) 0.1724(4) 0.0707(17) Uani 1 1 d . . . . .
H10A H 0.523933 0.598290 0.229421 0.106 Uiso 1 1 calc R U . . .
H10B H 0.519709 0.592773 0.116688 0.106 Uiso 1 1 calc R U . . .
H10C H 0.562740 0.561334 0.166363 0.106 Uiso 1 1 calc R U . . .
C8 C 0.47102(15) 0.4426(6) 0.1838(4) 0.087(2) Uani 1 1 d . . . . .
H8A H 0.460415 0.368550 0.192888 0.131 Uiso 1 1 calc R U . . .
H8B H 0.460070 0.472307 0.124456 0.131 Uiso 1 1 calc R U . . .
H8C H 0.462152 0.488543 0.236716 0.131 Uiso 1 1 calc R U . . .
O3 O 0.6749(6) 0.6996(14) -0.0758(14) 0.100(3) Uani 0.25 1 d D U P A -1
C29 C 0.6875(8) 0.758(3) 0.009(3) 0.095(3) Uani 0.25 1 d D U P A -1
H29A H 0.705688 0.820122 -0.008308 0.113 Uiso 0.25 1 calc R U P A -1
H29B H 0.703425 0.709211 0.051363 0.113 Uiso 0.25 1 calc R U P A -1
C30 C 0.6493(9) 0.800(2) 0.060(2) 0.103(4) Uani 0.25 1 d D U P A -1
H30A H 0.652050 0.795257 0.129878 0.124 Uiso 0.25 1 calc R U P A -1
H30B H 0.642070 0.875299 0.041613 0.124 Uiso 0.25 1 calc R U P A -1
C32 C 0.6340(7) 0.661(2) -0.046(2) 0.102(4) Uani 0.25 1 d D U P A -1
H32A H 0.614388 0.664620 -0.099528 0.123 Uiso 0.25 1 calc R U P A -1
H32B H 0.635988 0.584551 -0.024573 0.123 Uiso 0.25 1 calc R U P A -1
C31 C 0.6205(11) 0.7221(19) 0.024(3) 0.107(4) Uani 0.25 1 d . U P A -1
H31A H 0.611811 0.673901 0.076231 0.128 Uiso 0.25 1 calc R U P A -1
H31B H 0.595502 0.761509 0.001626 0.128 Uiso 0.25 1 calc R U P A -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -1 0 0.0540
1 1 0 0.0640
-4 3 0 0.0640
-1 0 0 0.0610
0 0 1 0.0430
0 0 -1 0.0120
5 -3 0 0.0500
1 0 0 0.0620
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
P1 Yb1 P1 61.40(5) 3_656 . ?
P2 Yb1 P1 41.97(2) . . ?
P2 Yb1 P1 41.97(2) 2_655 3_656 ?
P2 Yb1 P1 41.97(2) 2_655 . ?
P2 Yb1 P1 41.97(2) . 3_656 ?
P2 Yb1 P2 60.29(5) 2_655 . ?
O1 Yb1 P1 149.30(3) . 3_656 ?
O1 Yb1 P1 149.30(3) . . ?
O1 Yb1 P2 149.85(3) . . ?
O1 Yb1 P2 149.85(3) . 2_655 ?
O1 Yb1 O2 78.04(6) . . ?
O1 Yb1 O2 78.04(6) . 4_556 ?
O2 Yb1 P1 87.13(6) 4_556 3_656 ?
O2 Yb1 P1 113.98(6) . 3_656 ?
O2 Yb1 P1 87.13(6) . . ?
O2 Yb1 P1 113.98(6) 4_556 . ?
O2 Yb1 P2 75.06(6) 4_556 . ?
O2 Yb1 P2 128.04(6) . . ?
O2 Yb1 P2 75.06(6) . 2_655 ?
O2 Yb1 P2 128.04(6) 4_556 2_655 ?
O2 Yb1 O2 156.07(12) 4_556 . ?
N1 Yb1 P1 82.61(8) 4_556 3_656 ?
N1 Yb1 P1 82.61(8) . . ?
N1 Yb1 P1 136.49(8) 4_556 . ?
N1 Yb1 P1 136.49(8) . 3_656 ?
N1 Yb1 P2 120.89(8) 4_556 . ?
N1 Yb1 P2 94.97(8) 4_556 2_655 ?
N1 Yb1 P2 94.97(8) . . ?
N1 Yb1 P2 120.89(8) . 2_655 ?
N1 Yb1 O1 69.70(7) 4_556 . ?
N1 Yb1 O1 69.70(7) . . ?
N1 Yb1 O2 85.64(10) . . ?
N1 Yb1 O2 85.64(10) 4_556 4_556 ?
N1 Yb1 O2 86.11(10) . 4_556 ?
N1 Yb1 O2 86.11(10) 4_556 . ?
N1 Yb1 N1 139.40(15) . 4_556 ?
Yb1 P1 Yb1 118.60(5) . 2_655 ?
P2 P1 Yb1 68.59(3) . . ?
P2 P1 Yb1 68.59(3) 2_655 . ?
P2 P1 Yb1 68.59(3) 2_655 2_655 ?
P2 P1 Yb1 68.59(3) . 2_655 ?
P2 P1 P2 88.73(8) 2_655 . ?
Yb1 P2 Yb1 119.71(5) . 2_655 ?
P1 P2 Yb1 69.44(3) 3_656 2_655 ?
P1 P2 Yb1 69.44(3) 3_656 . ?
P1 P2 Yb1 69.44(3) . 2_655 ?
P1 P2 Yb1 69.44(3) . . ?
P1 P2 P1 91.27(8) 3_656 . ?
C6 O1 Yb1 120.82(19) 4_556 . ?
C6 O1 Yb1 120.82(19) . . ?
C6 O1 C6 118.4(4) 4_556 . ?
C28 O2 Yb1 129.7(2) . . ?
C28 O2 C25 108.5(3) . . ?
C25 O2 Yb1 121.9(2) . . ?
C13 N1 Yb1 130.7(2) . . ?
C1 N1 Yb1 118.2(2) . . ?
C1 N1 C13 111.1(3) . . ?
O2 C28 H28A 110.7 . . ?
O2 C28 H28B 110.7 . . ?
O2 C28 C27 105.1(3) . . ?
H28A C28 H28B 108.8 . . ?
C27 C28 H28A 110.7 . . ?
C27 C28 H28B 110.7 . . ?
C14 C13 N1 120.4(4) . . ?
C14 C13 C18 119.7(4) . . ?
C18 C13 N1 119.7(4) . . ?
C13 C14 C19 122.7(4) . . ?
C15 C14 C13 119.8(4) . . ?
C15 C14 C19 117.5(4) . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
C5 C6 O1 122.8(4) . . ?
C5 C6 C1 124.3(4) . . ?
C1 C6 O1 112.9(3) . . ?
C14 C19 H19 108.0 . . ?
C14 C19 C21 111.6(4) . . ?
C21 C19 H19 108.0 . . ?
C20 C19 C14 110.6(3) . . ?
C20 C19 H19 108.0 . . ?
C20 C19 C21 110.6(4) . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C6 C5 C4 117.2(4) . . ?
C6 C5 C11 122.0(4) . . ?
C4 C5 C11 120.9(3) . . ?
C5 C4 H4 119.1 . . ?
C3 C4 C5 121.7(4) . . ?
C3 C4 H4 119.1 . . ?
C14 C15 H15 119.7 . . ?
C14 C15 C16 120.7(4) . . ?
C16 C15 H15 119.7 . . ?
C4 C3 C7 122.7(3) . . ?
C2 C3 C4 118.6(4) . . ?
C2 C3 C7 118.7(4) . . ?
C13 C18 C22 122.8(4) . . ?
C17 C18 C13 119.0(4) . . ?
C17 C18 C22 118.1(4) . . ?
C3 C2 H2 118.7 . . ?
C3 C2 C1 122.6(4) . . ?
C1 C2 H2 118.7 . . ?
C6 C1 N1 118.3(3) . . ?
C2 C1 N1 126.0(4) . . ?
C2 C1 C6 115.6(3) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C23 C22 H22 107.4 . . ?
C23 C22 C24 110.1(4) . . ?
C18 C22 C23 113.7(3) . . ?
C18 C22 H22 107.4 . . ?
C18 C22 C24 110.7(4) . . ?
C24 C22 H22 107.4 . . ?
C28 C27 H27A 111.5 . . ?
C28 C27 H27B 111.5 . . ?
C28 C27 C26 101.2(3) . . ?
H27A C27 H27B 109.4 . . ?
C26 C27 H27A 111.5 . . ?
C26 C27 H27B 111.5 . . ?
C18 C17 H17 119.5 . . ?
C16 C17 C18 121.0(4) . . ?
C16 C17 H17 119.5 . . ?
C15 C16 H16 120.1 . . ?
C17 C16 C15 119.9(4) . . ?
C17 C16 H16 120.1 . . ?
C5 C11 C5 112.1(4) . 4_556 ?
C5 C11 C12 108.5(2) 4_556 4_556 ?
C5 C11 C12 108.9(2) 4_556 . ?
C5 C11 C12 108.9(2) . 4_556 ?
C5 C11 C12 108.5(2) . . ?
C12 C11 C12 109.8(5) 4_556 . ?
C27 C26 H26A 111.4 . . ?
C27 C26 H26B 111.4 . . ?
H26A C26 H26B 109.2 . . ?
C25 C26 C27 102.0(3) . . ?
C25 C26 H26A 111.4 . . ?
C25 C26 H26B 111.4 . . ?
O2 C25 C26 106.0(3) . . ?
O2 C25 H25A 110.5 . . ?
O2 C25 H25B 110.5 . . ?
C26 C25 H25A 110.5 . . ?
C26 C25 H25B 110.5 . . ?
H25A C25 H25B 108.7 . . ?
C9 C7 C3 109.7(4) . . ?
C9 C7 C10 108.9(4) . . ?
C9 C7 C8 109.6(4) . . ?
C10 C7 C3 109.5(4) . . ?
C8 C7 C3 112.8(4) . . ?
C8 C7 C10 106.3(4) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C29 O3 C32 100(2) . . ?
O3 C29 H29A 109.8 . . ?
O3 C29 H29B 109.8 . . ?
O3 C29 C30 109.4(18) . . ?
H29A C29 H29B 108.2 . . ?
C30 C29 H29A 109.8 . . ?
C30 C29 H29B 109.8 . . ?
C29 C30 H30A 112.3 . . ?
C29 C30 H30B 112.3 . . ?
H30A C30 H30B 109.9 . . ?
C31 C30 C29 97(2) . . ?
C31 C30 H30A 112.3 . . ?
C31 C30 H30B 112.3 . . ?
O3 C32 H32A 109.8 . . ?
O3 C32 H32B 109.8 . . ?
H32A C32 H32B 108.2 . . ?
C31 C32 O3 109(2) . . ?
C31 C32 H32A 109.8 . . ?
C31 C32 H32B 109.8 . . ?
C30 C31 H31A 108.3 . . ?
C30 C31 H31B 108.3 . . ?
C32 C31 C30 116(3) . . ?
C32 C31 H31A 108.3 . . ?
C32 C31 H31B 108.3 . . ?
H31A C31 H31B 107.4 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Yb1 P1 3.0192(8) . ?
Yb1 P1 3.0192(8) 3_656 ?
Yb1 P2 3.0021(8) 2_655 ?
Yb1 P2 3.0021(8) . ?
Yb1 O1 2.296(3) . ?
Yb1 O2 2.442(3) . ?
Yb1 O2 2.442(3) 4_556 ?
Yb1 N1 2.290(3) 4_556 ?
Yb1 N1 2.290(3) . ?
P1 P2 2.1562(15) . ?
P1 P2 2.1562(15) 2_655 ?
O1 C6 1.411(4) . ?
O1 C6 1.411(4) 4_556 ?
O2 C28 1.466(4) . ?
O2 C25 1.473(4) . ?
N1 C13 1.457(5) . ?
N1 C1 1.408(4) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C27 1.524(6) . ?
C13 C14 1.405(6) . ?
C13 C18 1.412(5) . ?
C14 C19 1.541(6) . ?
C14 C15 1.385(6) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C23 C22 1.524(5) . ?
C6 C5 1.384(5) . ?
C6 C1 1.403(5) . ?
C19 H19 1.0000 . ?
C19 C21 1.557(5) . ?
C19 C20 1.525(6) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C5 C4 1.395(5) . ?
C5 C11 1.519(5) . ?
C4 H4 0.9500 . ?
C4 C3 1.392(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.387(6) . ?
C3 C2 1.390(5) . ?
C3 C7 1.542(5) . ?
C18 C22 1.508(6) . ?
C18 C17 1.394(5) . ?
C2 H2 0.9500 . ?
C2 C1 1.402(5) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C22 H22 1.0000 . ?
C22 C24 1.533(5) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C26 1.537(6) . ?
C17 H17 0.9500 . ?
C17 C16 1.384(6) . ?
C16 H16 0.9500 . ?
C11 C12 1.554(5) 4_556 ?
C11 C12 1.554(5) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C25 1.511(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C7 C9 1.505(6) . ?
C7 C10 1.535(7) . ?
C7 C8 1.520(6) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
O3 C29 1.459(16) . ?
O3 C32 1.460(15) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.517(19) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.43(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C31 1.31(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
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
Yb1 O1 C6 C5 -179.1(3) . . . . ?
Yb1 O1 C6 C1 -0.9(4) . . . . ?
Yb1 O2 C28 C27 -163.2(2) . . . . ?
Yb1 O2 C25 C26 -170.4(2) . . . . ?
Yb1 N1 C13 C14 95.9(4) . . . . ?
Yb1 N1 C13 C18 -89.2(4) . . . . ?
Yb1 N1 C1 C6 0.2(5) . . . . ?
Yb1 N1 C1 C2 179.3(3) . . . . ?
O1 C6 C5 C4 179.2(3) . . . . ?
O1 C6 C5 C11 -1.7(6) . . . . ?
O1 C6 C1 N1 0.4(5) . . . . ?
O1 C6 C1 C2 -178.7(3) . . . . ?
O2 C28 C27 C26 -36.1(4) . . . . ?
N1 C13 C14 C19 -7.4(5) . . . . ?
N1 C13 C14 C15 173.5(3) . . . . ?
N1 C13 C18 C22 1.6(5) . . . . ?
N1 C13 C18 C17 -173.7(3) . . . . ?
C28 O2 C25 C26 9.1(4) . . . . ?
C28 C27 C26 C25 40.9(4) . . . . ?
C13 N1 C1 C6 178.8(4) . . . . ?
C13 N1 C1 C2 -2.2(5) . . . . ?
C13 C14 C19 C21 107.6(4) . . . . ?
C13 C14 C19 C20 -128.9(4) . . . . ?
C13 C14 C15 C16 -0.8(6) . . . . ?
C13 C18 C22 C23 139.6(4) . . . . ?
C13 C18 C22 C24 -95.9(4) . . . . ?
C13 C18 C17 C16 1.0(6) . . . . ?
C14 C13 C18 C22 176.5(3) . . . . ?
C14 C13 C18 C17 1.3(5) . . . . ?
C14 C15 C16 C17 3.0(7) . . . . ?
C6 O1 C6 C5 0.9(3) 4_556 . . . ?
C6 O1 C6 C1 179.1(4) 4_556 . . . ?
C6 C5 C4 C3 -1.4(6) . . . . ?
C6 C5 C11 C5 0.8(3) . . . 4_556 ?
C6 C5 C11 C12 -119.5(5) . . . . ?
C6 C5 C11 C12 120.9(4) . . . 4_556 ?
C19 C14 C15 C16 -179.9(4) . . . . ?
C5 C6 C1 N1 178.6(4) . . . . ?
C5 C6 C1 C2 -0.5(6) . . . . ?
C5 C4 C3 C2 1.1(6) . . . . ?
C5 C4 C3 C7 -179.1(4) . . . . ?
C4 C5 C11 C5 179.9(4) . . . 4_556 ?
C4 C5 C11 C12 -60.0(5) . . . 4_556 ?
C4 C5 C11 C12 59.5(5) . . . . ?
C4 C3 C2 C1 -0.4(6) . . . . ?
C4 C3 C7 C9 -120.2(5) . . . . ?
C4 C3 C7 C10 120.3(5) . . . . ?
C4 C3 C7 C8 2.2(6) . . . . ?
C15 C14 C19 C21 -73.2(5) . . . . ?
C15 C14 C19 C20 50.3(5) . . . . ?
C3 C2 C1 N1 -179.0(4) . . . . ?
C3 C2 C1 C6 0.1(6) . . . . ?
C18 C13 C14 C19 177.7(3) . . . . ?
C18 C13 C14 C15 -1.4(6) . . . . ?
C18 C17 C16 C15 -3.2(6) . . . . ?
C2 C3 C7 C9 59.6(5) . . . . ?
C2 C3 C7 C10 -59.9(5) . . . . ?
C2 C3 C7 C8 -178.0(4) . . . . ?
C1 N1 C13 C14 -82.4(4) . . . . ?
C1 N1 C13 C18 92.5(4) . . . . ?
C1 C6 C5 C4 1.2(7) . . . . ?
C1 C6 C5 C11 -179.8(3) . . . . ?
C22 C18 C17 C16 -174.5(4) . . . . ?
C27 C26 C25 O2 -31.4(4) . . . . ?
C17 C18 C22 C23 -45.1(5) . . . . ?
C17 C18 C22 C24 79.4(5) . . . . ?
C11 C5 C4 C3 179.5(3) . . . . ?
C25 O2 C28 C27 17.3(4) . . . . ?
C7 C3 C2 C1 179.8(4) . . . . ?
O3 C29 C30 C31 24(4) . . . . ?
O3 C32 C31 C30 -7(3) . . . . ?
C29 O3 C32 C31 22(3) . . . . ?
C29 C30 C31 C32 -11(3) . . . . ?
C32 O3 C29 C30 -28(3) . . . . ?
