Temperature-dependent NIR-CPL spectra of chiral Yb(III) complexes.
Sickinger, Annika; Grasser, Maxime; Baguenard, Bruno; Bensalah-Ledoux, Amina; Guy, Laure; Bui, Anh Thy; Guyot, Yannick; Dorcet, Vincent; Pointillart, Fabrice; Cador, Olivier; Guy, Stéphan; Maury, Olivier; Le Guennic, Boris; Riobé, François; Physical chemistry chemical physics : PCCP 26 (2024) 15776–15783; doi:10.1039/d4cp01286k

data_7248667
_publ_section_title
;
 Temperature-dependent NIR-CPL spectra of chiral Yb(III) complexes.
;
_journal_issue                   21
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              15776
_journal_page_last               15783
_journal_paper_doi               10.1039/d4cp01286k
_journal_volume                  26
_journal_year                    2024
_chemical_absolute_configuration rm/ad/rmad/syn/unk/.
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C153 H168 N12 O6 Yb, 3(C F3 O3 S)'
_chemical_formula_sum            'C156 H168 F9 N12 O15 S3 Yb'
_chemical_formula_weight         2891.23
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_update_record
;
2024-02-13 deposited with the CCDC.	2024-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.181(4)
_cell_length_b                   26.777(6)
_cell_length_c                   31.548(7)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.1939
_cell_measurement_theta_min      2.1963
_cell_measurement_wavelength     0.710730
_cell_volume                     18738(7)
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2020)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 CMOS-PHOTON70
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_orient_matrix_UB_11      -0.0064273
_diffrn_orient_matrix_UB_12      0.0020232
_diffrn_orient_matrix_UB_13      0.0313267
_diffrn_orient_matrix_UB_21      -0.0237057
_diffrn_orient_matrix_UB_22      -0.0317469
_diffrn_orient_matrix_UB_23      -0.0009272
_diffrn_orient_matrix_UB_31      0.0378058
_diffrn_orient_matrix_UB_32      -0.0195626
_diffrn_orient_matrix_UB_33      0.0047444
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0776
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            248701
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.544
_diffrn_reflns_theta_min         1.890
_diffrn_source_current           1.00
_diffrn_source_power             50.0
_diffrn_source_voltage           50.00
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.025
_exptl_crystal_description       prism
_exptl_crystal_F_000             6028
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.190
_refine_diff_density_max         2.436
_refine_diff_density_min         -0.986
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
Flack x determined using 12401 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.008(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1760
_refine_ls_number_reflns         42946
_refine_ls_number_restraints     511
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0640P)^2^+14.6682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1354
_reflns_Friedel_coverage         0.878
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                31838
_reflns_number_total             42946
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d4cp01286k3.cif
_cod_data_source_block           ATB99
_cod_depositor_comments
'Adding full bibliography for 7248667--7248668.cif.'
_cod_database_code               7248667
_shelx_res_checksum              4331
_shelx_fab_checksum              822