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_1568518
_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 Sm2, C7 H8'
_chemical_formula_sum            'C117 H164 N4 O6 P4 Sm2'
_chemical_formula_weight         2147.09
_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
_audit_creation_date             2022-05-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_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                   32.7745(7)
_cell_length_b                   12.3366(3)
_cell_length_c                   14.1237(5)
_cell_measurement_reflns_used    93980
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.38
_cell_measurement_theta_min      2.28
_cell_volume                     5710.6(3)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details
;
 2413 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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            109804
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.583
_diffrn_reflns_theta_min         2.278
_exptl_absorpt_coefficient_mu    1.126
_exptl_absorpt_correction_T_max  0.9085
_exptl_absorpt_correction_T_min  0.1486
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2252
_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.055
_refine_diff_density_max         1.101
_refine_diff_density_min         -1.543
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         7708
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0725P)^2^+22.9841P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1387
_refine_ls_wR_factor_ref         0.1729
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4824
_reflns_number_total             7708
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06730g3.cif
_cod_data_source_block           ah123_2
_cod_original_sg_symbol_H-M      'P b a n'
_cod_database_code               1568518
_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. Uiso/Uaniso restraints and constraints
C34 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C35 \\sim C29: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: C35(0.25) H35A(0.25) H35B(0.25) H35C(0.25) C29(0.25) C30(0.25)
 H30(0.25) C31(0.25) H31(0.25) C32(0.25) H32(0.25) C33(0.25) H33(0.25)
 C34(0.25) H34(0.25)
4.a Free rotating group:
 C35(C29,C30,C31,C32,C33,C34)
4.b Ternary CH refined with riding coordinates:
 C19(H19), C22(H22)
4.c Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C27(H27A,H27B), C25(H25A,H25B), C26(H26A,H26B)
4.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C17(H17), C15(H15), C16(H16), C30(H30), C31(H31), C32(H32),
 C33(H33), C34(H34)
4.e Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C21(H21A,H21B,
 H21C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C11(H11A,
 H11B,H11C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              13863
_olex2_submission_special_instructions 'No special instructions were received'