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_7121932
_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         'C36 H45 N6 O6 Yb, 7(H2 O)'
_chemical_formula_sum            'C36 H59 N6 O13 Yb'
_chemical_formula_weight         956.93
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-02-19
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.02.02 svn.r3481 for OlexSys, GUI svn.r5470)
;
_audit_update_record
;
2018-06-13 deposited with the CCDC.
2018-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                106.9911(15)
_cell_angle_beta                 90.0945(17)
_cell_angle_gamma                94.4990(17)
_cell_formula_units_Z            2
_cell_length_a                   8.0215(3)
_cell_length_b                   14.8835(6)
_cell_length_c                   17.6485(7)
_cell_measurement_reflns_used    9627
_cell_measurement_temperature    120
_cell_measurement_theta_max      33.28
_cell_measurement_theta_min      2.77
_cell_volume                     2008.17(14)
_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 2016/6 multi-CPU version (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_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 0.900
_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  0.0407
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            55290
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        32.500
_diffrn_reflns_theta_max         35.701
_diffrn_reflns_theta_min         2.414
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.399
_exptl_absorpt_correction_T_max  0.5986
_exptl_absorpt_correction_T_min  0.4216
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
; SADABS-2016/2 (Krause et al, 2015) was used for absorption correction, 
 by numerical inegration based on crystal face-indexing followed by 
 semi-empirical correction based on Laue equivalents and multiple scans. 
 wR2(int) was 0.1486 before and 0.0583 after correction. The Ratio of 
 minimum to maximum transmission is 0.7043. The \l/2 correction factor 
 is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_description       lathe
_exptl_crystal_F_000             982
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol/water'
_exptl_crystal_size_max          0.608
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.072
_refine_diff_density_max         1.095
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         16744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0241P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0536
_refine_ls_wR_factor_ref         0.0554
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14376
_reflns_number_total             16744
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04995e2.cif
_cod_data_source_block           YbL2_18srv061
_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               7121932
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.846
_shelx_estimated_absorpt_t_min   0.323
_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 H(H) groups, All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C28B) = Uanis(C28A)
Uanis(C15B) = Uanis(C15A)
Uanis(C14B) = Uanis(C14A)
Uanis(C13A) = Uanis(C13B)
3. Others
 Uiso(H39A)=Uiso(H39B)=Uiso(H39C)=FVAR(1)
 Uiso(H40A)=Uiso(H40B)=Uiso(H40C)=FVAR(2)
 Sof(C28B)=Sof(H28B)=Sof(C29B)=Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(C30B)=
 Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(3)
 Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30A)=
 Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(3)
 Uiso(H19A)=Uiso(H19B)=Uiso(H19C)=FVAR(4)
 Uiso(H20A)=Uiso(H20B)=Uiso(H20C)=Uiso(H20D)=Uiso(H20E)=Uiso(H20F)=FVAR(5)
 Fixed Sof: C13A(0.9) H13A(0.9) C14A(0.9) C15A(0.9) H15A(0.9) C13B(0.1)
 H13B(0.1) C14B(0.1) C15B(0.1) H15B(0.1) C18A(0.9) H18A(0.9) C19A(0.9)
 H19A(0.9) H19B(0.9) H19C(0.9) C18B(0.1) H18B(0.1) C19B(0.1) H19D(0.1)
 H19E(0.1) H19F(0.1) H20A(0.9) H20B(0.9) H20C(0.9) H20D(0.1) H20E(0.1)
 H20F(0.1) H2W(0.5) H2WB(0.5) H3WA(0.5) H3WB(0.5) H4W(0.5) H4WB(0.5) H5W(0.5)
 H5WB(0.5)
4.a Riding coordinates:
 C19B(H19D,H19E,H19F), C20(H20A,H20B,H20C), C20(H20D,H20E,H20F), C29A(H29A,
 H29B,H29C), C30A(H30A,H30B,H30C), C29B(H29D,H29E,H29F), O1W(H1WA,H1WB),
 O2W(H2WA,H2W,H2WB), O3W(H3W,H3WA,H3WB), O4W(H4WA,H4W,H4WB), O5W(H5W,H5WA,H5WB),
  O6W(H6WA,H6WB), O7W(H7WA,H7WB)
4.b Rotating group:
 C19A(H19A,H19B,H19C)
4.c Ternary CH refined with riding coordinates:
 C18A(H18A), C18B(H18B), C28A(H28A), C28B(H28B), C38(H38)
4.d 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.e Me refined with riding coordinates:
 C30B(H30D,H30E,H30F)
4.f Aromatic/amide H refined with riding coordinates:
 C13A(H13A), C15A(H15A), C13B(H13B), C15B(H15B), C23(H23), C25(H25), C33(H33),
 C35(H35)
4.g Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              22229