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_7121935
_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         'C39 H51 N6 O6 Yb, 5(H2 O), C H4 O'
_chemical_formula_sum            'C40 H65 N6 O12 Yb'
_chemical_formula_weight         995.02
_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             2018-06-11
_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                86.530(2)
_cell_angle_beta                 86.957(2)
_cell_angle_gamma                74.094(2)
_cell_formula_units_Z            2
_cell_length_a                   7.6574(3)
_cell_length_b                   13.1494(5)
_cell_length_c                   22.7470(9)
_cell_measurement_reflns_used    9598
_cell_measurement_temperature    160
_cell_measurement_theta_max      30.75
_cell_measurement_theta_min      2.35
_cell_volume                     2197.08(15)
_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 multi-CPU (Sheldrick, 2015a)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      160
_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 0.898
_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  0.0339
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            60349
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        32.500
_diffrn_reflns_theta_max         35.782
_diffrn_reflns_theta_min         2.470
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.195
_exptl_absorpt_correction_T_max  0.8218
_exptl_absorpt_correction_T_min  0.5907
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
 wR2(int) was 0.1157 before and 0.0418 after correction. 
 The Ratio of minimum to maximum transmission is 0.7188. 
 The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_description       blade
_exptl_crystal_F_000             1026
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol/water'
_exptl_crystal_size_max          0.392
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.116
_refine_diff_density_max         1.974
_refine_diff_density_min         -2.086
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       0.00041(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         18394
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+1.7520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0619
_refine_ls_wR_factor_ref         0.0640
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15744
_reflns_number_total             18394
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04995e2.cif
_cod_data_source_block           YbL3_18srv194
_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               7121935
_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 O(H,H) groups, All O(H,H,H) groups
2. Others
 Uiso(H18A)=Uiso(H18B)=Uiso(H18C)=FVAR(1)
 Uiso(H19A)=Uiso(H19B)=Uiso(H19C)=FVAR(2)
 Uiso(H20A)=Uiso(H20B)=FVAR(3)
 Uiso(H20C)=Uiso(H28A)=Uiso(H28B)=Uiso(H28C)=FVAR(4)
 Uiso(H29A)=Uiso(H29B)=Uiso(H29C)=FVAR(5)
 Uiso(H30A)=Uiso(H30B)=Uiso(H30C)=FVAR(6)
 Uiso(H38A)=Uiso(H38B)=Uiso(H38C)=FVAR(7)
 Uiso(H39A)=Uiso(H39B)=Uiso(H39C)=FVAR(8)
 Uiso(H40A)=Uiso(H40B)=Uiso(H40C)=FVAR(9)
 Uiso(H10A)=Uiso(H10B)=Uiso(H10C)=FVAR(10)
 Fixed Sof: H3W(0.5) H3W1(0.5)
3.a Riding coordinates:
 O1W(H1W1,H1W2), O2(H2), O3W(H3W,H3W1,H3W2), O4W(H4W1,H4W2), O5W(H5W1,H5W2),
 O6W(H6W1,H6W2)
3.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)
3.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C23(H23), C24(H24), C33(H33), C34(H34)
3.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C), C40(H40A,H40B,H40C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              35151