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_1568515
_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         'C55 H78 N2 O3 Yb'
_chemical_formula_sum            'C55 H78 N2 O3 Yb'
_chemical_formula_weight         988.23
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-16
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_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            8
_cell_length_a                   18.5124(14)
_cell_length_b                   15.2519(11)
_cell_length_c                   35.298(3)
_cell_measurement_reflns_used    19986
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.09
_cell_measurement_theta_min      2.20
_cell_volume                     9966.4(13)
_computing_cell_refinement
;
X-Area Recipe 1.34.0.0 (STOE, 2019)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.154.0 (STOE, 2019)
;
_computing_data_reduction
;
X-Area Integrate 1.77.0.0 (STOE, 2019)
X-Area LANA 1.77.1.0 (STOE, 2019)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.88, Darmstadt 2019
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_details
;
 297 frames, detector distance = 80 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0671
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            31881
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.520
_diffrn_reflns_theta_min         2.200
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.920
_exptl_absorpt_correction_T_max  0.9463
_exptl_absorpt_correction_T_min  0.5260
_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, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             4128
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.033
_refine_diff_density_max         2.449
_refine_diff_density_min         -1.739
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         12120
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0647
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0380P)^2^+91.7915P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1330
_refine_ls_wR_factor_ref         0.1534
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7910
_reflns_number_total             12120
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06730g3.cif
_cod_data_source_block           ahucr_11_sv
_cod_original_cell_volume        9966.5(13)
_cod_database_code               1568515
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.802
_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
 C33A-C35A \\sim C34A-C33A
 with sigma of 0.01
 C34B-C33B \\sim C35B-C33B
 with sigma of 0.01
 C29-C33B \\sim C30-C25
 with sigma of 0.01
 C30-C25 \\sim C33A-C29
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C35B \\sim C33B \\sim C34B: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
C35A \\sim C33A \\sim C34A: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
C33B \\sim C29: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
4. Others
 Fixed Sof: C33B(0.5) H33B(0.5) C34B(0.5) H34A(0.5) H34B(0.5) H34C(0.5)
 C35B(0.5) H35A(0.5) H35B(0.5) H35C(0.5) C35A(0.5) H35D(0.5) H35E(0.5)
 H35F(0.5) C33A(0.5) H33A(0.5) C34A(0.5) H34D(0.5) H34E(0.5) H34F(0.5)
5.a Ternary CH refined with riding coordinates:
 C42(H42), C45(H45), C30(H30), C33B(H33B), C33A(H33A)
5.b Secondary CH2 refined with riding coordinates:
 C48(H48A,H48B), C50(H50A,H50B), C55(H55A,H55B), C51(H51A,H51B), C49(H49A,
 H49B), C53(H53A,H53B), C52(H52A,H52B), C54(H54A,H54B)
5.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C40(H40), C38(H38), C11(H11), C3(H3), C5(H5), C39(H39), C28(H28),
 C26(H26), C27(H27)
5.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C15(H15A,H15B,H15C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C21(H21A,H21B,H21C), C19(H19A,H19B,H19C), C18(H18A,
 H18B,H18C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C32(H32A,H32B,H32C),
 C47(H47A,H47B,H47C), C31(H31A,H31B,H31C), C34B(H34A,H34B,H34C), C46(H46A,H46B,
 H46C), C35B(H35A,H35B,H35C), C35A(H35D,H35E,H35F), C34A(H34D,H34E,H34F)
;
_shelx_res_checksum              27097
_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'