Exquisite sensitivity of the ligand field to solvation and donor polarisability in coordinatively saturated lanthanide complexes.
Mason, Kevin; Harnden, Alice C.; Patrick, Connor W.; Poh, Adeline W. J.; Batsanov, Andrei S.; Suturina, Elizaveta A.; Vonci, Michele; McInnes, Eric J. L.; Chilton, Nicholas F.; Parker, David; Chemical communications (Cambridge, England) 54 (2018) 8486–8489; doi:10.1039/c8cc04995e

data_7121934
_publ_section_title
;
 Exquisite sensitivity of the ligand field to solvation and donor
 polarisability in coordinatively saturated lanthanide complexes.
;
_journal_issue                   61
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8486
_journal_page_last               8489
_journal_paper_doi               10.1039/c8cc04995e
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C30 H33 N6 O9 Yb, 4(C H4 O)'
_chemical_formula_sum            'C34 H49 N6 O13 Yb'
_chemical_formula_weight         922.83
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-06-11
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-13 deposited with the CCDC.
2018-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                95.4509(16)
_cell_angle_beta                 93.4986(15)
_cell_angle_gamma                96.4015(15)
_cell_formula_units_Z            2
_cell_length_a                   7.8898(3)
_cell_length_b                   14.8884(6)
_cell_length_c                   15.9436(7)
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.91
_cell_measurement_theta_min      2.57
_cell_volume                     1847.88(13)
_computing_cell_refinement       'SAINT v8.38A (Bruker, 2017)'
_computing_data_collection       'APEX3 v.2016.1-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'Bruker PHOTON 100 CMOS'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '3-circle area detector diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40729
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         2.573
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.604
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8373
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;   
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.0799 before and 0.0396 after correction. 
The Ratio of minimum to maximum transmission is 0.8373. 
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_description       needle
_exptl_crystal_F_000             938
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Et2O, methanol'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         10767
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0259P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0540
_refine_ls_wR_factor_ref         0.0560
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8888
_reflns_number_total             10767
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04995e2.cif
_cod_data_source_block           YbL4_18srv138
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7121932--7121939.cif.
;
_cod_database_code               7121934
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.903
_shelx_estimated_absorpt_t_min   0.637
_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 O(H) groups
2. Restrained distances
 O5S-C5S
 1.4 with sigma of 0.02
3. Others
 Uiso(H18A)=Uiso(H18B)=Uiso(H18C)=FVAR(1)
 Uiso(H28A)=Uiso(H28B)=Uiso(H28C)=FVAR(2)
 Uiso(H38A)=Uiso(H38B)=Uiso(H38C)=FVAR(3)
 Uiso(H4SA)=Uiso(H4SB)=Uiso(H4SC)=Uiso(H5SA)=Uiso(H5SB)=Uiso(H5SC)=FVAR(4)
 Uiso(H3SA)=Uiso(H3SB)=Uiso(H3SC)=FVAR(5)
 Uiso(H1SA)=Uiso(H1SB)=Uiso(H1SC)=FVAR(6)
 Uiso(H2SA)=Uiso(H2SB)=Uiso(H2SC)=FVAR(7)
 Fixed Sof: O4S(0.85) H4S(0.85) C4S(0.85) H4SA(0.85) H4SB(0.85) H4SC(0.85)
 O5S(0.15) H5S(0.15) C5S(0.15) H5SA(0.15) H5SB(0.15) H5SC(0.15)
4.a Riding coordinates:
 C4S(H4SA,H4SB,H4SC), C5S(H5SA,H5SB,H5SC)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B), C9(H9A,H9B),
 C11(H11A,H11B), C21(H21A,H21B), C31(H31A,H31B)
4.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C15(H15), C23(H23), C25(H25), C33(H33), C35(H35)
4.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C28(H28A,H28B,H28C), C38(H38A,H38B,H38C), C3S(H3SA,H3SB,
 H3SC), C1S(H1SA,H1SB,H1SC), C2S(H2SA,H2SB,H2SC)
4.e Idealised tetrahedral OH refined as rotating group:
 O4S(H4S), O3S(H3S), O1S(H1S), O2S(H2S), O5S(H5S)
;
_shelx_res_checksum              86929