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_7121933
_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_absolute_configuration ad
_chemical_formula_moiety         'C27 H27 N6 O6 Yb, 3(H2 O)'
_chemical_formula_sum            'C27 H33 N6 O9 Yb'
_chemical_formula_weight         758.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-06-13
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-19 deposited with the CCDC.
2018-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.3301(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.9466(3)
_cell_length_b                   11.7823(5)
_cell_length_c                   14.7072(6)
_cell_measurement_reflns_used    9868
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.30
_cell_measurement_theta_min      2.23
_cell_volume                     1358.81(10)
_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      120
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'Bruker PHOTON 100 CMOS'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0423
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36972
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.725
_diffrn_reflns_theta_min         2.226
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.509
_exptl_absorpt_correction_T_max  0.9913
_exptl_absorpt_correction_T_min  0.5421
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
; SADABS-2016/2 (Krause et al, 2015) was used for absorption correction. 
 wR2(int) was 0.1170 before and 0.0401 after correction. The Ratio of minimum  
 to maximum transmission is 0.5469. The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.854
_exptl_crystal_description       lathe
_exptl_crystal_F_000             758
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: water/methanol'
_exptl_crystal_size_max          0.305
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.017
_refine_diff_density_max         0.892
_refine_diff_density_min         -0.925
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details
;
 Flack x determined using 4177 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons et at., 2004, 2013). 
 x = -0.016(6) by classical fit to all intensities. 
 Hooft parameter y = -0.004(3).
;
_refine_ls_abs_structure_Flack   -0.017(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         10726
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0191P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0443
_refine_ls_wR_factor_ref         0.0460
_reflns_Friedel_coverage         0.972
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.974
_reflns_number_gt                9393
_reflns_number_total             10726
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04995e2.cif
_cod_data_source_block           18srv253
_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               7121933
_ccdc_comments
'isomorphous with IMAYEC (Tb), OHIPAW (Eu), OHIPEA (Gd), OHIPIE (Lu)'
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.414
_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
2. Uiso/Uaniso restraints and constraints
Uanis(O3W') = Uanis(O3W)
3. Others
 Fixed Sof: O3W'(0.2) O3W(0.8)
4.a Riding coordinates:
 O3W(H3WA,H3WB), O1W(H1WA,H1WB), O2W(H2WA,H2WB)
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), C14(H14), C15(H15), C23(H23), C24(H24), C25(H25), C33(H33),
 C34(H34), C35(H35)
;
_shelx_res_checksum              5033
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'