Molecular cyclo-P3 complexes of the rare-earth elements via a one-pot reaction and selective reduction
Hauser, Adrian; Münzfeld, Luca; Schlittenhardt, Sören; Köppe, Ralf; Uhlmann, Cedric; Rauska, Ulf-Christian; Ruben, Mario; Roesky, Peter W.; Chemical Science 14 (2023) 2149–2158; doi:10.1039/D2SC06730G

data_1568519
_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, \w 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(\m~2~-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/[\s^2^(Fo^2^)+(0.0769P)^2^] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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
_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)
;
_shelx_res_checksum              39966
_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'